# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guofu Zi' _publ_contact_author_email ZIGUOFU@HOTMAIL.COM _publ_section_title ; Lanthanide and group 4 metal complexes with new chiral biaryl-based NNO-donor ligands ; loop_ _publ_author_name 'Guofu Zi.' 'Hai-Bin Song.' 'Qiuwen Wang.' 'Li Xiang.' # Attachment 'compound_2H.cif' data_2H _database_code_depnum_ccdc_archive 'CCDC 687843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 N2 O2' _chemical_formula_sum 'C28 H34 N2 O2' _chemical_formula_weight 430.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.3062(14) _cell_length_b 8.1494(10) _cell_length_c 13.4427(16) _cell_angle_alpha 90.00 _cell_angle_beta 115.782(8) _cell_angle_gamma 90.00 _cell_volume 1213.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2413 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9768 _exptl_absorpt_correction_T_max 0.9869 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9175 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2302 _reflns_number_gt 2072 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'None, Friedel Pairs merged' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2302 _refine_ls_number_parameters 335 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1703 _refine_ls_wR_factor_gt 0.1572 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.4174(3) 0.5605(4) 0.7630(3) 0.0409(8) Uani 1 1 d . . . O2 O 0.7971(4) 0.6431(5) 0.9352(3) 0.0579(10) Uani 1 1 d . . . H2 H 0.723(6) 0.652(9) 0.885(5) 0.087 Uiso 1 1 d . . . N1 N 0.6144(3) 0.9226(4) 0.9497(3) 0.0354(8) Uani 1 1 d . . . N2 N 0.8684(3) 0.8891(5) 1.0983(3) 0.0427(9) Uani 1 1 d . . . H2A H 0.852(5) 0.811(7) 1.046(4) 0.051 Uiso 1 1 d . . . C1 C 0.5114(4) 0.7938(5) 0.7321(3) 0.0313(10) Uani 1 1 d . . . C2 C 0.4964(4) 0.6221(5) 0.7248(3) 0.0338(10) Uani 1 1 d . . . C3 C 0.5581(4) 0.5258(6) 0.6814(4) 0.0404(11) Uani 1 1 d . . . H3 H 0.5473 0.4102 0.6762 0.048 Uiso 1 1 calc R . . C4 C 0.6360(4) 0.6015(6) 0.6458(4) 0.0429(11) Uani 1 1 d . . . H4 H 0.6785 0.5353 0.6164 0.052 Uiso 1 1 calc R . . C5 C 0.6541(4) 0.7699(6) 0.6515(4) 0.0381(11) Uani 1 1 d . A . C6 C 0.5902(4) 0.8679(5) 0.6952(3) 0.0313(9) Uani 1 1 d . A . C7 C 0.6057(4) 1.0521(5) 0.7022(4) 0.0350(10) Uani 1 1 d D . . H7A H 0.5390 1.1011 0.6411 0.042 Uiso 0.612(14) 1 d PR A 1 H7B H 0.6036 1.0900 0.7690 0.042 Uiso 0.612(14) 1 d PR A 1 H7C H 0.5276 1.1016 0.6789 0.042 Uiso 0.388(14) 1 d PR A 2 H7D H 0.6534 1.0822 0.7780 0.042 Uiso 0.388(14) 1 d PR A 2 C8 C 0.7232(7) 1.1111(9) 0.6992(8) 0.038(2) Uani 0.612(14) 1 d PD A 1 H8A H 0.7214 1.2318 0.6906 0.045 Uiso 0.612(14) 1 calc PR A 1 H8B H 0.7933 1.0821 0.7692 0.045 Uiso 0.612(14) 1 calc PR A 1 C9 C 0.7353(10) 1.0292(9) 0.6020(9) 0.039(3) Uani 0.612(14) 1 d PD A 1 H9A H 0.6646 1.0579 0.5324 0.047 Uiso 0.612(14) 1 calc PR A 1 H9B H 0.8085 1.0711 0.5974 0.047 Uiso 0.612(14) 1 calc PR A 1 C8' C 0.6651(13) 1.1232(11) 0.6319(13) 0.042(4) Uani 0.388(14) 1 d PD A 2 H8'A H 0.6065 1.1223 0.5530 0.051 Uiso 0.388(14) 1 calc PR A 2 H8'B H 0.6894 1.2383 0.6539 0.051 Uiso 0.388(14) 1 calc PR A 2 C9' C 0.7761(10) 1.0215(13) 0.6480(15) 0.045(5) Uani 0.388(14) 1 d PD A 2 H9'A H 0.8140 1.0692 0.6030 0.054 Uiso 0.388(14) 1 calc PR A 2 H9'B H 0.8357 1.0265 0.7265 0.054 Uiso 0.388(14) 1 calc PR A 2 C10 C 0.7437(5) 0.8436(5) 0.6150(5) 0.0514(13) Uani 1 1 d D . . H10A H 0.8237 0.8149 0.6680 0.062 Uiso 0.612(14) 1 d PR A 1 H10B H 0.7310 0.7957 0.5455 0.062 Uiso 0.612(14) 1 d PR A 1 H10C H 0.8165 0.7799 0.6465 0.062 Uiso 0.388(14) 1 d PR A 2 H10D H 0.7117 0.8347 0.5361 0.062 Uiso 0.388(14) 1 d PR A 2 C11 C 0.4368(4) 0.8927(5) 0.7739(4) 0.0315(9) Uani 1 1 d . . . C12 C 0.4884(4) 0.9504(5) 0.8828(4) 0.0326(9) Uani 1 1 d . . . C13 C 0.4150(4) 1.0321(5) 0.9227(4) 0.0371(10) Uani 1 1 d . . . H13 H 0.4482 1.0694 0.9971 0.045 Uiso 1 1 calc R . . C14 C 0.2950(4) 1.0583(6) 0.8541(4) 0.0423(11) Uani 1 1 d . . . H14 H 0.2462 1.1124 0.8826 0.051 Uiso 1 1 calc R . . C15 C 0.2431(4) 1.0082(5) 0.7449(4) 0.0381(10) Uani 1 1 d . B . C16 C 0.3134(4) 0.9198(5) 0.7041(4) 0.0354(10) Uani 1 1 d . B . C17 C 0.2594(4) 0.8539(6) 0.5875(4) 0.0417(11) Uani 1 1 d D . . H17A H 0.3155 0.8708 0.5565 0.050 Uiso 0.626(14) 1 d PR B 1 H17B H 0.2479 0.7377 0.5902 0.050 Uiso 0.626(14) 1 d PR B 1 H17C H 0.2873 0.9183 0.5435 0.050 Uiso 0.374(14) 1 d PR B 2 H17D H 0.2869 0.7433 0.5888 0.050 Uiso 0.374(14) 1 d PR B 2 C18 C 0.1390(7) 0.9294(14) 0.5111(6) 0.054(3) Uani 0.626(14) 1 d PD B 1 H18A H 0.1006 0.8625 0.4430 0.065 Uiso 0.626(14) 1 calc PR B 1 H18B H 0.1522 1.0412 0.4897 0.065 Uiso 0.626(14) 1 calc PR B 1 C19 C 0.0550(6) 0.9381(13) 0.5685(6) 0.052(3) Uani 0.626(14) 1 d PD B 1 H19A H 0.0413 0.8261 0.5892 0.062 Uiso 0.626(14) 1 calc PR B 1 H19B H -0.0239 0.9840 0.5168 0.062 Uiso 0.626(14) 1 calc PR B 1 C18' C 0.1204(8) 0.8550(17) 0.5316(11) 0.047(4) Uani 0.374(14) 1 d PD B 2 H18C H 0.0895 0.7672 0.5633 0.056 Uiso 0.374(14) 1 calc PR B 2 H18D H 0.0905 0.8341 0.4514 0.056 Uiso 0.374(14) 1 calc PR B 2 C19' C 0.0745(11) 1.0233(17) 0.5499(8) 0.055(5) Uani 0.374(14) 1 d PD B 2 H19C H 0.1101 1.1119 0.5231 0.066 Uiso 0.374(14) 1 calc PR B 2 H19D H -0.0144 1.0287 0.5080 0.066 Uiso 0.374(14) 1 calc PR B 2 C20 C 0.1104(4) 1.0460(6) 0.6724(4) 0.0478(12) Uani 1 1 d D . . H20A H 0.0658 1.0300 0.7150 0.057 Uiso 0.626(14) 1 d PR B 1 H20B H 0.1027 1.1592 0.6507 0.057 Uiso 0.626(14) 1 d PR B 1 H20C H 0.0615 0.9763 0.6940 0.057 Uiso 0.374(14) 1 d PR B 2 H20D H 0.0946 1.1576 0.6849 0.057 Uiso 0.374(14) 1 d PR B 2 C21 C 0.3913(5) 0.3887(6) 0.7499(5) 0.0592(15) Uani 1 1 d . . . H21A H 0.4639 0.3266 0.7965 0.089 Uiso 1 1 calc R . . H21B H 0.3654 0.3580 0.6724 0.089 Uiso 1 1 calc R . . H21C H 0.3267 0.3639 0.7716 0.089 Uiso 1 1 calc R . . C22 C 0.6717(4) 1.0311(6) 1.0239(4) 0.0401(10) Uani 1 1 d . . . H22 H 0.6293 1.1262 1.0282 0.048 Uiso 1 1 calc R . . C23 C 0.7955(4) 1.0154(6) 1.0997(4) 0.0414(11) Uani 1 1 d . . . C24 C 0.8643(5) 1.1139(7) 1.1900(5) 0.0621(15) Uani 1 1 d . . . H24 H 0.8375 1.2111 1.2115 0.074 Uiso 1 1 calc R . . C25 C 0.9785(5) 1.0459(9) 1.2431(5) 0.0716(18) Uani 1 1 d . . . H25 H 1.0437 1.0878 1.3073 0.086 Uiso 1 1 calc R . . C26 C 0.9801(5) 0.9049(8) 1.1852(5) 0.0601(15) Uani 1 1 d . . . H26 H 1.0467 0.8329 1.2028 0.072 Uiso 1 1 calc R . . C27 C 0.8151(5) 0.4711(8) 0.9449(5) 0.0649(16) Uani 1 1 d . . . H27A H 0.8091 0.4249 0.8746 0.078 Uiso 1 1 calc R . . H27B H 0.7529 0.4184 0.9623 0.078 Uiso 1 1 calc R . . C28 C 0.9386(6) 0.4397(9) 1.0362(5) 0.0732(18) Uani 1 1 d . . . H28A H 0.9438 0.4868 1.1052 0.110 Uiso 1 1 calc R . . H28B H 0.9995 0.4906 1.0176 0.110 Uiso 1 1 calc R . . H28C H 0.9529 0.3211 1.0454 0.110 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0530(18) 0.0245(15) 0.0551(19) -0.0027(14) 0.0326(16) -0.0023(13) O2 0.053(2) 0.063(3) 0.052(2) -0.0046(19) 0.0186(18) 0.007(2) N1 0.044(2) 0.032(2) 0.037(2) -0.0028(16) 0.0230(17) -0.0056(16) N2 0.039(2) 0.042(2) 0.048(2) 0.0012(19) 0.0204(19) -0.0061(18) C1 0.034(2) 0.027(2) 0.034(2) 0.0024(17) 0.016(2) 0.0035(17) C2 0.040(2) 0.026(2) 0.039(2) 0.0010(18) 0.019(2) 0.0009(18) C3 0.051(3) 0.026(2) 0.045(3) -0.003(2) 0.022(2) 0.002(2) C4 0.057(3) 0.035(3) 0.047(3) -0.002(2) 0.033(2) 0.009(2) C5 0.049(3) 0.030(2) 0.044(3) 0.000(2) 0.029(2) 0.0067(19) C6 0.036(2) 0.025(2) 0.034(2) 0.0031(17) 0.0173(19) 0.0039(17) C7 0.040(2) 0.029(2) 0.045(2) 0.0012(19) 0.026(2) 0.0004(18) C8 0.028(4) 0.034(4) 0.054(6) 0.010(4) 0.020(4) 0.006(3) C9 0.035(5) 0.040(5) 0.050(7) 0.003(4) 0.026(5) -0.006(4) C8' 0.040(8) 0.034(7) 0.057(10) 0.011(7) 0.025(8) 0.009(6) C9' 0.034(9) 0.050(9) 0.048(11) 0.005(7) 0.015(8) 0.011(7) C10 0.060(3) 0.045(3) 0.066(4) 0.005(3) 0.043(3) 0.009(2) C11 0.039(2) 0.025(2) 0.039(2) 0.0036(18) 0.025(2) 0.0008(17) C12 0.040(2) 0.025(2) 0.040(2) 0.0011(18) 0.025(2) -0.0013(18) C13 0.053(3) 0.032(2) 0.035(2) -0.0057(19) 0.028(2) -0.004(2) C14 0.053(3) 0.036(2) 0.052(3) 0.003(2) 0.036(2) 0.008(2) C15 0.040(2) 0.033(2) 0.047(3) 0.006(2) 0.024(2) 0.0040(19) C16 0.044(2) 0.028(2) 0.043(3) 0.0019(19) 0.028(2) 0.0009(18) C17 0.044(2) 0.041(3) 0.040(3) -0.001(2) 0.019(2) -0.001(2) C18 0.061(6) 0.042(6) 0.053(6) 0.004(5) 0.018(5) 0.004(5) C19 0.038(5) 0.072(7) 0.046(5) 0.021(5) 0.018(4) 0.010(4) C18' 0.049(9) 0.041(9) 0.033(8) 0.005(7) 0.002(6) 0.013(7) C19' 0.047(8) 0.074(12) 0.057(10) 0.031(9) 0.034(7) 0.011(8) C20 0.043(2) 0.044(3) 0.058(3) 0.007(2) 0.025(2) 0.009(2) C21 0.086(4) 0.026(2) 0.089(4) -0.003(2) 0.060(4) -0.012(2) C22 0.043(2) 0.034(2) 0.044(3) -0.004(2) 0.020(2) -0.005(2) C23 0.047(3) 0.033(2) 0.046(3) -0.003(2) 0.022(2) -0.009(2) C24 0.073(4) 0.046(3) 0.061(3) -0.013(3) 0.023(3) -0.018(3) C25 0.056(3) 0.071(4) 0.063(4) 0.000(3) 0.002(3) -0.029(3) C26 0.043(3) 0.072(4) 0.060(3) 0.012(3) 0.017(3) -0.007(3) C27 0.074(4) 0.067(4) 0.065(4) -0.013(3) 0.042(3) 0.002(3) C28 0.087(5) 0.076(5) 0.066(4) 0.007(3) 0.043(4) 0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.376(5) . ? O1 C21 1.430(6) . ? O2 C27 1.417(8) . ? O2 H2 0.87(7) . ? N1 C22 1.290(6) . ? N1 C12 1.432(5) . ? N2 C26 1.369(7) . ? N2 C23 1.371(6) . ? N2 H2A 0.90(6) . ? C1 C6 1.404(5) . ? C1 C2 1.409(6) . ? C1 C11 1.502(5) . ? C2 C3 1.385(6) . ? C3 C4 1.388(6) . ? C3 H3 0.9500 . ? C4 C5 1.387(7) . ? C4 H4 0.9500 . ? C5 C6 1.414(6) . ? C5 C10 1.513(6) . ? C6 C7 1.511(6) . ? C7 C8' 1.538(9) . ? C7 C8 1.541(7) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9601 . ? C7 H7D 0.9599 . ? C8 C9 1.531(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.520(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C8' C9' 1.530(9) . ? C8' H8'A 0.9900 . ? C8' H8'B 0.9900 . ? C9' C10 1.517(10) . ? C9' H9'A 0.9900 . ? C9' H9'B 0.9900 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C10 H10D 0.9600 . ? C11 C12 1.400(6) . ? C11 C16 1.412(6) . ? C12 C13 1.403(5) . ? C13 C14 1.376(6) . ? C13 H13 0.9500 . ? C14 C15 1.383(7) . ? C14 H14 0.9500 . ? C15 C16 1.408(6) . ? C15 C20 1.525(6) . ? C16 C17 1.509(6) . ? C17 C18 1.519(8) . ? C17 C18' 1.541(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9601 . ? C17 H17D 0.9600 . ? C18 C19 1.536(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.537(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C18' C19' 1.542(10) . ? C18' H18C 0.9900 . ? C18' H18D 0.9900 . ? C19' C20 1.519(9) . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C20 H20D 0.9600 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.422(6) . ? C22 H22 0.9500 . ? C23 C24 1.393(7) . ? C24 C25 1.385(9) . ? C24 H24 0.9500 . ? C25 C26 1.393(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.503(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 C21 117.9(3) . . ? C27 O2 H2 103(5) . . ? C22 N1 C12 117.1(4) . . ? C26 N2 C23 109.8(5) . . ? C26 N2 H2A 122(3) . . ? C23 N2 H2A 128(3) . . ? C6 C1 C2 119.5(4) . . ? C6 C1 C11 122.1(4) . . ? C2 C1 C11 118.4(3) . . ? O1 C2 C3 123.8(4) . . ? O1 C2 C1 115.4(4) . . ? C3 C2 C1 120.8(4) . . ? C2 C3 C4 118.7(4) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 122.6(4) . . ? C5 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C4 C5 C6 118.4(4) . . ? C4 C5 C10 119.8(4) . . ? C6 C5 C10 121.7(4) . . ? C1 C6 C5 119.9(4) . . ? C1 C6 C7 119.5(3) . . ? C5 C6 C7 120.6(4) . . ? C6 C7 C8' 114.6(5) . . ? C6 C7 C8 113.7(4) . . ? C8' C7 C8 33.2(5) . . ? C6 C7 H7A 108.8 . . ? C8' C7 H7A 77.0 . . ? C8 C7 H7A 108.1 . . ? C6 C7 H7B 108.9 . . ? C8' C7 H7B 131.8 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 107.8 . . ? C6 C7 H7C 108.4 . . ? C8' C7 H7C 108.5 . . ? C8 C7 H7C 132.6 . . ? H7A C7 H7C 35.3 . . ? H7B C7 H7C 75.0 . . ? C6 C7 H7D 108.8 . . ? C8' C7 H7D 108.7 . . ? C8 C7 H7D 78.5 . . ? H7A C7 H7D 134.6 . . ? H7B C7 H7D 34.8 . . ? H7C C7 H7D 107.6 . . ? C9 C8 C7 109.1(6) . . ? C9 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? C9 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C10 C9 C8 111.3(6) . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9' C8' C7 110.1(8) . . ? C9' C8' H8'A 109.6 . . ? C7 C8' H8'A 109.6 . . ? C9' C8' H8'B 109.6 . . ? C7 C8' H8'B 109.6 . . ? H8'A C8' H8'B 108.2 . . ? C10 C9' C8' 111.8(8) . . ? C10 C9' H9'A 109.3 . . ? C8' C9' H9'A 109.3 . . ? C10 C9' H9'B 109.3 . . ? C8' C9' H9'B 109.3 . . ? H9'A C9' H9'B 107.9 . . ? C5 C10 C9' 114.8(5) . . ? C5 C10 C9 114.1(4) . . ? C9' C10 C9 23.0(6) . . ? C5 C10 H10A 108.5 . . ? C9' C10 H10A 87.8 . . ? C9 C10 H10A 108.9 . . ? C5 C10 H10B 108.8 . . ? C9' C10 H10B 125.7 . . ? C9 C10 H10B 108.6 . . ? H10A C10 H10B 107.7 . . ? C5 C10 H10C 108.3 . . ? C9' C10 H10C 108.2 . . ? C9 C10 H10C 126.3 . . ? H10A C10 H10C 23.3 . . ? H10B C10 H10C 86.2 . . ? C5 C10 H10D 108.8 . . ? C9' C10 H10D 109.0 . . ? C9 C10 H10D 88.5 . . ? H10A C10 H10D 126.7 . . ? H10B C10 H10D 23.1 . . ? H10C C10 H10D 107.6 . . ? C12 C11 C16 120.7(3) . . ? C12 C11 C1 119.9(4) . . ? C16 C11 C1 119.4(4) . . ? C11 C12 C13 118.9(4) . . ? C11 C12 N1 118.6(3) . . ? C13 C12 N1 122.4(4) . . ? C14 C13 C12 120.0(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 122.0(4) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C14 C15 C16 119.1(4) . . ? C14 C15 C20 119.3(4) . . ? C16 C15 C20 121.5(4) . . ? C15 C16 C11 119.1(4) . . ? C15 C16 C17 121.3(4) . . ? C11 C16 C17 119.7(3) . . ? C16 C17 C18 114.7(4) . . ? C16 C17 C18' 113.5(5) . . ? C18 C17 C18' 28.1(5) . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17A 108.8 . . ? C18' C17 H17A 130.0 . . ? C16 C17 H17B 108.5 . . ? C18 C17 H17B 108.0 . . ? C18' C17 H17B 82.8 . . ? H17A C17 H17B 107.7 . . ? C16 C17 H17C 109.4 . . ? C18 C17 H17C 82.3 . . ? C18' C17 H17C 108.3 . . ? H17A C17 H17C 30.1 . . ? H17B C17 H17C 131.3 . . ? C16 C17 H17D 108.8 . . ? C18 C17 H17D 128.7 . . ? C18' C17 H17D 108.8 . . ? H17A C17 H17D 80.1 . . ? H17B C17 H17D 29.6 . . ? H17C C17 H17D 107.8 . . ? C17 C18 C19 110.5(6) . . ? C17 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? C17 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? C18 C19 C20 110.7(6) . . ? C18 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C17 C18' C19' 109.5(8) . . ? C17 C18' H18C 109.8 . . ? C19' C18' H18C 109.8 . . ? C17 C18' H18D 109.8 . . ? C19' C18' H18D 109.8 . . ? H18C C18' H18D 108.2 . . ? C20 C19' C18' 109.1(8) . . ? C20 C19' H19C 109.9 . . ? C18' C19' H19C 109.9 . . ? C20 C19' H19D 109.9 . . ? C18' C19' H19D 109.9 . . ? H19C C19' H19D 108.3 . . ? C19' C20 C15 113.2(5) . . ? C19' C20 C19 30.7(5) . . ? C15 C20 C19 113.2(4) . . ? C19' C20 H20A 131.2 . . ? C15 C20 H20A 108.8 . . ? C19 C20 H20A 108.8 . . ? C19' C20 H20B 81.0 . . ? C15 C20 H20B 109.0 . . ? C19 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C19' C20 H20C 109.3 . . ? C15 C20 H20C 109.0 . . ? C19 C20 H20C 81.2 . . ? H20A C20 H20C 30.9 . . ? H20B C20 H20C 132.0 . . ? C19' C20 H20D 108.6 . . ? C15 C20 H20D 108.8 . . ? C19 C20 H20D 131.1 . . ? H20A C20 H20D 79.2 . . ? H20B C20 H20D 30.9 . . ? H20C C20 H20D 107.8 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C23 123.2(4) . . ? N1 C22 H22 118.4 . . ? C23 C22 H22 118.4 . . ? N2 C23 C24 106.9(4) . . ? N2 C23 C22 124.1(4) . . ? C24 C23 C22 128.9(5) . . ? C25 C24 C23 108.4(6) . . ? C25 C24 H24 125.8 . . ? C23 C24 H24 125.8 . . ? C24 C25 C26 107.4(5) . . ? C24 C25 H25 126.3 . . ? C26 C25 H25 126.3 . . ? N2 C26 C25 107.5(5) . . ? N2 C26 H26 126.2 . . ? C25 C26 H26 126.2 . . ? O2 C27 C28 107.8(5) . . ? O2 C27 H27A 110.2 . . ? C28 C27 H27A 110.2 . . ? O2 C27 H27B 110.2 . . ? C28 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 O1 C2 C3 -4.7(7) . . . . ? C21 O1 C2 C1 175.2(4) . . . . ? C6 C1 C2 O1 179.9(4) . . . . ? C11 C1 C2 O1 -3.3(6) . . . . ? C6 C1 C2 C3 -0.2(6) . . . . ? C11 C1 C2 C3 176.6(4) . . . . ? O1 C2 C3 C4 -179.7(4) . . . . ? C1 C2 C3 C4 0.4(6) . . . . ? C2 C3 C4 C5 -0.2(7) . . . . ? C3 C4 C5 C6 -0.2(7) . . . . ? C3 C4 C5 C10 177.8(4) . . . . ? C2 C1 C6 C5 -0.3(6) . . . . ? C11 C1 C6 C5 -176.9(4) . . . . ? C2 C1 C6 C7 179.6(4) . . . . ? C11 C1 C6 C7 2.9(6) . . . . ? C4 C5 C6 C1 0.4(7) . . . . ? C10 C5 C6 C1 -177.6(4) . . . . ? C4 C5 C6 C7 -179.4(4) . . . . ? C10 C5 C6 C7 2.6(7) . . . . ? C1 C6 C7 C8' -164.0(7) . . . . ? C5 C6 C7 C8' 15.8(9) . . . . ? C1 C6 C7 C8 159.5(5) . . . . ? C5 C6 C7 C8 -20.7(7) . . . . ? C6 C7 C8 C9 49.5(9) . . . . ? C8' C7 C8 C9 -49.7(7) . . . . ? C7 C8 C9 C10 -62.0(10) . . . . ? C6 C7 C8' C9' -46.1(14) . . . . ? C8 C7 C8' C9' 50.1(9) . . . . ? C7 C8' C9' C10 59.5(17) . . . . ? C4 C5 C10 C9' -167.2(8) . . . . ? C6 C5 C10 C9' 10.8(9) . . . . ? C4 C5 C10 C9 167.5(6) . . . . ? C6 C5 C10 C9 -14.6(8) . . . . ? C8' C9' C10 C5 -42.0(15) . . . . ? C8' C9' C10 C9 51.7(10) . . . . ? C8 C9 C10 C5 44.4(10) . . . . ? C8 C9 C10 C9' -52.6(11) . . . . ? C6 C1 C11 C12 -81.5(5) . . . . ? C2 C1 C11 C12 101.8(5) . . . . ? C6 C1 C11 C16 101.4(5) . . . . ? C2 C1 C11 C16 -75.3(5) . . . . ? C16 C11 C12 C13 1.6(6) . . . . ? C1 C11 C12 C13 -175.4(4) . . . . ? C16 C11 C12 N1 -178.8(4) . . . . ? C1 C11 C12 N1 4.2(5) . . . . ? C22 N1 C12 C11 148.7(4) . . . . ? C22 N1 C12 C13 -31.7(5) . . . . ? C11 C12 C13 C14 -1.7(6) . . . . ? N1 C12 C13 C14 178.7(4) . . . . ? C12 C13 C14 C15 -0.9(7) . . . . ? C13 C14 C15 C16 3.5(7) . . . . ? C13 C14 C15 C20 -178.0(4) . . . . ? C14 C15 C16 C11 -3.5(6) . . . . ? C20 C15 C16 C11 178.1(4) . . . . ? C14 C15 C16 C17 176.4(4) . . . . ? C20 C15 C16 C17 -2.0(6) . . . . ? C12 C11 C16 C15 1.0(6) . . . . ? C1 C11 C16 C15 178.0(4) . . . . ? C12 C11 C16 C17 -179.0(4) . . . . ? C1 C11 C16 C17 -1.9(6) . . . . ? C15 C16 C17 C18 16.6(7) . . . . ? C11 C16 C17 C18 -163.4(6) . . . . ? C15 C16 C17 C18' -14.2(9) . . . . ? C11 C16 C17 C18' 165.8(7) . . . . ? C16 C17 C18 C19 -45.7(10) . . . . ? C18' C17 C18 C19 48.4(9) . . . . ? C17 C18 C19 C20 61.1(11) . . . . ? C16 C17 C18' C19' 47.1(13) . . . . ? C18 C17 C18' C19' -51.7(9) . . . . ? C17 C18' C19' C20 -65.1(15) . . . . ? C18' C19' C20 C15 48.9(13) . . . . ? C18' C19' C20 C19 -47.8(8) . . . . ? C14 C15 C20 C19' 165.5(7) . . . . ? C16 C15 C20 C19' -16.1(9) . . . . ? C14 C15 C20 C19 -161.1(6) . . . . ? C16 C15 C20 C19 17.3(7) . . . . ? C18 C19 C20 C19' 50.5(8) . . . . ? C18 C19 C20 C15 -46.3(9) . . . . ? C12 N1 C22 C23 176.8(4) . . . . ? C26 N2 C23 C24 0.3(5) . . . . ? C26 N2 C23 C22 -176.8(4) . . . . ? N1 C22 C23 N2 3.7(7) . . . . ? N1 C22 C23 C24 -172.8(5) . . . . ? N2 C23 C24 C25 -0.3(6) . . . . ? C22 C23 C24 C25 176.7(5) . . . . ? C23 C24 C25 C26 0.1(6) . . . . ? C23 N2 C26 C25 -0.3(5) . . . . ? C24 C25 C26 N2 0.1(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O2 0.90(6) 1.92(6) 2.814(6) 172(5) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.194 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.053 # Attachment 'compound_3H.cif' data_3H _database_code_depnum_ccdc_archive 'CCDC 687844' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 N2 O' _chemical_formula_sum 'C20 H20 N2 O' _chemical_formula_weight 304.38 _chemical_absolute_configuration rm loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.9931(8) _cell_length_b 18.730(2) _cell_length_c 11.5194(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.603(2) _cell_angle_gamma 90.00 _cell_volume 1700.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 4835 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9912 _exptl_absorpt_correction_T_max 0.9985 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20292 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.86 _reflns_number_total 4158 _reflns_number_gt 3868 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.1551P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'None, Friedel pairs merged' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4158 _refine_ls_number_parameters 429 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.9478(2) 0.13241(8) 0.52725(15) 0.0356(4) Uani 1 1 d . . . O2 O 0.0458(2) 0.33878(8) 0.07441(13) 0.0357(4) Uani 1 1 d . . . N1 N 0.6424(2) 0.28385(10) 0.40807(14) 0.0280(4) Uani 1 1 d . . . N2 N 0.5070(2) 0.28160(11) 0.15568(14) 0.0289(4) Uani 1 1 d . . . H2 H 0.488(3) 0.3236(16) 0.185(2) 0.040(7) Uiso 1 1 d . . . N3 N 0.4130(2) 0.43719(10) 0.16976(14) 0.0264(4) Uani 1 1 d . . . N4 N 0.5242(2) 0.43793(11) 0.42810(15) 0.0286(4) Uani 1 1 d . . . H4A H 0.542(3) 0.3922(16) 0.407(2) 0.036(7) Uiso 1 1 d . . . C1 C 0.9997(3) 0.25323(11) 0.50000(19) 0.0278(4) Uani 1 1 d . . . C2 C 1.0338(3) 0.18230(11) 0.4727(2) 0.0303(4) Uani 1 1 d . . . C3 C 1.1443(3) 0.16588(13) 0.3956(2) 0.0385(5) Uani 1 1 d . . . H3 H 1.1650 0.1176 0.3772 0.046 Uiso 1 1 calc R . . C4 C 1.2235(3) 0.22070(15) 0.3463(3) 0.0460(6) Uani 1 1 d . . . H4 H 1.2974 0.2100 0.2920 0.055 Uiso 1 1 calc R . . C5 C 1.1969(3) 0.29077(14) 0.3747(2) 0.0425(6) Uani 1 1 d . . . H5 H 1.2548 0.3278 0.3412 0.051 Uiso 1 1 calc R . . C6 C 1.0864(3) 0.30798(12) 0.4516(2) 0.0349(5) Uani 1 1 d . . . C7 C 1.0598(4) 0.38417(12) 0.4835(2) 0.0447(6) Uani 1 1 d . . . H7A H 1.1282 0.4153 0.4416 0.067 Uiso 1 1 calc R . . H7B H 1.0943 0.3905 0.5686 0.067 Uiso 1 1 calc R . . H7C H 0.9396 0.3965 0.4612 0.067 Uiso 1 1 calc R . . C8 C 0.8737(3) 0.26739(11) 0.57881(18) 0.0302(4) Uani 1 1 d . . . C9 C 0.7017(3) 0.27719(12) 0.53221(16) 0.0305(4) Uani 1 1 d . . . C10 C 0.5813(3) 0.28475(15) 0.6059(2) 0.0423(6) Uani 1 1 d . . . H10 H 0.4649 0.2908 0.5732 0.051 Uiso 1 1 calc R . . C11 C 0.6310(4) 0.28337(15) 0.7268(2) 0.0499(7) Uani 1 1 d . . . H11 H 0.5489 0.2874 0.7773 0.060 Uiso 1 1 calc R . . C12 C 0.8007(4) 0.27613(15) 0.77370(19) 0.0495(7) Uani 1 1 d . . . H12 H 0.8345 0.2767 0.8568 0.059 Uiso 1 1 calc R . . C13 C 0.9234(3) 0.26803(12) 0.70184(19) 0.0391(5) Uani 1 1 d . . . C14 C 1.1084(4) 0.25949(15) 0.7548(2) 0.0534(7) Uani 1 1 d . . . H14A H 1.1203 0.2587 0.8408 0.080 Uiso 1 1 calc R . . H14B H 1.1733 0.2996 0.7306 0.080 Uiso 1 1 calc R . . H14C H 1.1515 0.2147 0.7272 0.080 Uiso 1 1 calc R . . C15 C 0.9777(4) 0.05939(12) 0.5040(3) 0.0467(6) Uani 1 1 d . . . H15A H 0.9409 0.0496 0.4200 0.070 Uiso 1 1 calc R . . H15B H 0.9138 0.0292 0.5505 0.070 Uiso 1 1 calc R . . H15C H 1.0992 0.0490 0.5254 0.070 Uiso 1 1 calc R . . C16 C 0.6529(2) 0.22893(12) 0.34359(17) 0.0274(4) Uani 1 1 d . . . H16 H 0.7064 0.1874 0.3799 0.033 Uiso 1 1 calc R . . C17 C 0.5885(3) 0.22630(12) 0.21963(17) 0.0278(4) Uani 1 1 d . . . C18 C 0.5839(3) 0.16798(13) 0.1451(2) 0.0354(5) Uani 1 1 d . . . H18 H 0.6314 0.1222 0.1652 0.042 Uiso 1 1 calc R . . C19 C 0.4959(4) 0.18909(14) 0.0342(2) 0.0426(6) Uani 1 1 d . . . H19 H 0.4729 0.1602 -0.0344 0.051 Uiso 1 1 calc R . . C20 C 0.4497(3) 0.25923(13) 0.04363(18) 0.0370(5) Uani 1 1 d . . . H20 H 0.3881 0.2874 -0.0177 0.044 Uiso 1 1 calc R . . C21 C 0.0596(2) 0.46373(11) 0.07193(16) 0.0246(4) Uani 1 1 d . . . C22 C -0.0089(3) 0.40196(12) 0.11464(17) 0.0278(4) Uani 1 1 d . . . C23 C -0.1238(3) 0.40694(14) 0.19293(18) 0.0366(5) Uani 1 1 d . . . H23 H -0.1695 0.3650 0.2220 0.044 Uiso 1 1 calc R . . C24 C -0.1704(3) 0.47334(16) 0.2275(2) 0.0413(6) Uani 1 1 d . . . H24 H -0.2460 0.4770 0.2827 0.050 Uiso 1 1 calc R . . C25 C -0.1096(3) 0.53412(15) 0.1837(2) 0.0404(5) Uani 1 1 d . . . H25 H -0.1455 0.5794 0.2075 0.048 Uiso 1 1 calc R . . C26 C 0.0052(3) 0.53045(12) 0.10408(19) 0.0323(5) Uani 1 1 d . . . C27 C 0.0670(4) 0.59835(13) 0.0566(2) 0.0481(6) Uani 1 1 d . . . H27A H -0.0227 0.6184 -0.0029 0.072 Uiso 1 1 calc R . . H27B H 0.1673 0.5883 0.0207 0.072 Uiso 1 1 calc R . . H27C H 0.0966 0.6327 0.1209 0.072 Uiso 1 1 calc R . . C28 C 0.1915(2) 0.45664(10) -0.00524(16) 0.0237(4) Uani 1 1 d . . . C29 C 0.3623(3) 0.44623(11) 0.04561(16) 0.0257(4) Uani 1 1 d . . . C30 C 0.4878(3) 0.44157(13) -0.02519(18) 0.0328(5) Uani 1 1 d . . . H30 H 0.6027 0.4339 0.0096 0.039 Uiso 1 1 calc R . . C31 C 0.4441(3) 0.44822(12) -0.14601(19) 0.0340(5) Uani 1 1 d . . . H31 H 0.5296 0.4464 -0.1942 0.041 Uiso 1 1 calc R . . C32 C 0.2755(3) 0.45752(12) -0.19704(17) 0.0324(4) Uani 1 1 d . . . H32 H 0.2467 0.4615 -0.2802 0.039 Uiso 1 1 calc R . . C33 C 0.1486(3) 0.46112(11) -0.12863(17) 0.0274(4) Uani 1 1 d . . . C34 C -0.0347(3) 0.46923(15) -0.18507(18) 0.0378(5) Uani 1 1 d . . . H34A H -0.0445 0.4644 -0.2707 0.057 Uiso 1 1 calc R . . H34B H -0.0759 0.5164 -0.1661 0.057 Uiso 1 1 calc R . . H34C H -0.1028 0.4321 -0.1551 0.057 Uiso 1 1 calc R . . C35 C -0.0451(4) 0.27608(14) 0.0977(2) 0.0504(7) Uani 1 1 d . . . H35A H -0.0397 0.2707 0.1829 0.076 Uiso 1 1 calc R . . H35B H 0.0060 0.2342 0.0665 0.076 Uiso 1 1 calc R . . H35C H -0.1638 0.2804 0.0597 0.076 Uiso 1 1 calc R . . C36 C 0.3990(2) 0.49159(12) 0.23462(17) 0.0286(4) Uani 1 1 d . . . H36 H 0.3516 0.5338 0.1970 0.034 Uiso 1 1 calc R . . C37 C 0.4501(3) 0.49341(12) 0.36055(17) 0.0287(4) Uani 1 1 d . . . C38 C 0.4426(3) 0.55143(13) 0.43448(19) 0.0358(5) Uani 1 1 d . . . H38 H 0.3986 0.5974 0.4118 0.043 Uiso 1 1 calc R . . C39 C 0.5122(3) 0.52949(14) 0.54941(19) 0.0383(5) Uani 1 1 d . . . H39 H 0.5228 0.5577 0.6188 0.046 Uiso 1 1 calc R . . C40 C 0.5616(3) 0.45987(14) 0.54240(17) 0.0339(5) Uani 1 1 d . . . H40 H 0.6135 0.4314 0.6067 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0416(9) 0.0206(7) 0.0459(9) 0.0007(6) 0.0111(7) -0.0002(6) O2 0.0507(10) 0.0257(7) 0.0308(8) 0.0007(6) 0.0074(7) -0.0080(7) N1 0.0261(8) 0.0368(9) 0.0210(8) 0.0019(7) 0.0034(6) 0.0051(7) N2 0.0309(9) 0.0348(10) 0.0204(8) 0.0000(7) 0.0030(6) 0.0010(8) N3 0.0245(8) 0.0363(9) 0.0190(7) 0.0013(7) 0.0053(6) 0.0017(7) N4 0.0288(9) 0.0369(10) 0.0204(8) -0.0018(7) 0.0053(6) -0.0017(7) C1 0.0272(9) 0.0247(10) 0.0277(9) -0.0006(8) -0.0069(8) -0.0001(8) C2 0.0267(10) 0.0251(10) 0.0373(11) 0.0012(8) 0.0007(8) 0.0003(8) C3 0.0288(11) 0.0302(11) 0.0572(15) -0.0041(10) 0.0094(10) 0.0039(9) C4 0.0293(11) 0.0461(14) 0.0649(16) 0.0006(13) 0.0147(11) -0.0012(10) C5 0.0293(11) 0.0393(13) 0.0574(15) 0.0060(11) 0.0030(10) -0.0095(10) C6 0.0329(11) 0.0258(10) 0.0407(12) 0.0012(9) -0.0092(9) -0.0046(8) C7 0.0636(17) 0.0222(11) 0.0422(13) 0.0019(9) -0.0089(12) -0.0054(10) C8 0.0398(11) 0.0228(10) 0.0251(9) 0.0004(7) -0.0026(8) 0.0044(8) C9 0.0414(11) 0.0297(10) 0.0198(9) 0.0028(8) 0.0034(8) 0.0093(9) C10 0.0494(14) 0.0514(14) 0.0278(11) 0.0078(10) 0.0116(10) 0.0192(12) C11 0.0778(19) 0.0499(15) 0.0250(11) 0.0069(10) 0.0174(12) 0.0224(14) C12 0.086(2) 0.0413(13) 0.0190(10) 0.0016(9) 0.0015(11) 0.0122(13) C13 0.0581(14) 0.0289(11) 0.0253(10) 0.0006(8) -0.0076(9) 0.0042(10) C14 0.0621(16) 0.0494(15) 0.0377(12) 0.0047(11) -0.0237(12) -0.0041(13) C15 0.0597(16) 0.0204(10) 0.0619(16) 0.0002(10) 0.0156(13) 0.0009(10) C16 0.0239(9) 0.0350(11) 0.0236(9) 0.0029(8) 0.0048(7) 0.0030(8) C17 0.0239(9) 0.0364(11) 0.0236(9) 0.0006(8) 0.0053(7) 0.0002(8) C18 0.0410(12) 0.0352(12) 0.0305(11) -0.0010(9) 0.0076(9) 0.0021(9) C19 0.0547(15) 0.0434(13) 0.0274(11) -0.0087(10) 0.0007(11) 0.0009(11) C20 0.0434(12) 0.0442(13) 0.0213(10) -0.0012(9) -0.0005(9) 0.0000(10) C21 0.0249(9) 0.0253(9) 0.0232(8) 0.0024(8) 0.0023(7) 0.0008(8) C22 0.0282(10) 0.0327(10) 0.0206(9) 0.0009(8) -0.0014(7) -0.0048(8) C23 0.0309(11) 0.0527(14) 0.0254(10) 0.0021(10) 0.0024(8) -0.0148(10) C24 0.0248(10) 0.0693(17) 0.0305(11) -0.0074(11) 0.0065(8) -0.0006(11) C25 0.0367(12) 0.0492(14) 0.0357(12) -0.0042(10) 0.0073(10) 0.0135(11) C26 0.0318(11) 0.0329(11) 0.0314(11) 0.0014(9) 0.0032(9) 0.0061(9) C27 0.0705(18) 0.0261(11) 0.0484(14) 0.0047(10) 0.0123(13) 0.0061(12) C28 0.0276(9) 0.0214(9) 0.0221(8) 0.0006(7) 0.0039(7) 0.0001(7) C29 0.0295(9) 0.0289(10) 0.0193(8) 0.0022(7) 0.0056(7) 0.0023(8) C30 0.0296(10) 0.0449(12) 0.0240(10) 0.0009(9) 0.0045(8) 0.0042(9) C31 0.0374(11) 0.0423(13) 0.0249(10) -0.0003(9) 0.0126(8) 0.0026(9) C32 0.0409(11) 0.0361(12) 0.0197(8) 0.0017(8) 0.0037(8) -0.0022(9) C33 0.0319(10) 0.0259(10) 0.0235(9) 0.0028(8) 0.0018(7) -0.0009(8) C34 0.0350(11) 0.0490(13) 0.0270(10) 0.0057(10) -0.0020(8) -0.0015(11) C35 0.086(2) 0.0351(13) 0.0283(11) 0.0016(10) 0.0044(12) -0.0244(13) C36 0.0259(9) 0.0376(11) 0.0234(10) 0.0022(8) 0.0076(8) 0.0012(8) C37 0.0268(10) 0.0373(11) 0.0228(10) -0.0005(8) 0.0068(8) 0.0014(8) C38 0.0382(12) 0.0414(12) 0.0286(10) -0.0044(9) 0.0077(9) 0.0001(10) C39 0.0422(12) 0.0485(14) 0.0257(10) -0.0093(10) 0.0098(9) -0.0075(11) C40 0.0336(10) 0.0478(13) 0.0201(9) -0.0033(9) 0.0037(8) -0.0060(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.373(3) . ? O1 C15 1.422(3) . ? O2 C22 1.369(3) . ? O2 C35 1.430(3) . ? N1 C16 1.280(3) . ? N1 C9 1.435(2) . ? N2 C20 1.362(3) . ? N2 C17 1.371(3) . ? N2 H2 0.88(3) . ? N3 C36 1.279(3) . ? N3 C29 1.430(2) . ? N4 C40 1.364(3) . ? N4 C37 1.372(3) . ? N4 H4A 0.91(3) . ? C1 C2 1.402(3) . ? C1 C6 1.404(3) . ? C1 C8 1.488(3) . ? C2 C3 1.387(3) . ? C3 C4 1.378(4) . ? C3 H3 0.9500 . ? C4 C5 1.378(4) . ? C4 H4 0.9500 . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C6 C7 1.497(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.402(3) . ? C8 C13 1.407(3) . ? C9 C10 1.393(3) . ? C10 C11 1.383(3) . ? C10 H10 0.9500 . ? C11 C12 1.380(4) . ? C11 H11 0.9500 . ? C12 C13 1.393(4) . ? C12 H12 0.9500 . ? C13 C14 1.511(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.436(3) . ? C16 H16 0.9500 . ? C17 C18 1.386(3) . ? C18 C19 1.409(3) . ? C18 H18 0.9500 . ? C19 C20 1.374(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.393(3) . ? C21 C22 1.403(3) . ? C21 C28 1.495(3) . ? C22 C23 1.394(3) . ? C23 C24 1.376(4) . ? C23 H23 0.9500 . ? C24 C25 1.367(4) . ? C24 H24 0.9500 . ? C25 C26 1.403(3) . ? C25 H25 0.9500 . ? C26 C27 1.500(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.406(3) . ? C28 C33 1.408(2) . ? C29 C30 1.397(3) . ? C30 C31 1.383(3) . ? C30 H30 0.9500 . ? C31 C32 1.388(3) . ? C31 H31 0.9500 . ? C32 C33 1.386(3) . ? C32 H32 0.9500 . ? C33 C34 1.508(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.440(3) . ? C36 H36 0.9500 . ? C37 C38 1.388(3) . ? C38 C39 1.409(3) . ? C38 H38 0.9500 . ? C39 C40 1.369(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 C15 117.12(19) . . ? C22 O2 C35 116.47(18) . . ? C16 N1 C9 117.76(18) . . ? C20 N2 C17 109.4(2) . . ? C20 N2 H2 125.9(18) . . ? C17 N2 H2 124.5(18) . . ? C36 N3 C29 116.88(18) . . ? C40 N4 C37 108.88(19) . . ? C40 N4 H4A 121.7(16) . . ? C37 N4 H4A 129.3(16) . . ? C2 C1 C6 118.4(2) . . ? C2 C1 C8 118.82(19) . . ? C6 C1 C8 122.75(19) . . ? O1 C2 C3 124.2(2) . . ? O1 C2 C1 114.3(2) . . ? C3 C2 C1 121.4(2) . . ? C4 C3 C2 119.0(2) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.8(2) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 120.8(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 119.5(2) . . ? C5 C6 C7 120.6(2) . . ? C1 C6 C7 120.0(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 118.6(2) . . ? C9 C8 C1 120.67(17) . . ? C13 C8 C1 120.7(2) . . ? C10 C9 C8 120.86(19) . . ? C10 C9 N1 116.85(19) . . ? C8 C9 N1 122.20(18) . . ? C11 C10 C9 120.0(2) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 119.6(2) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 121.4(2) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C8 119.4(2) . . ? C12 C13 C14 120.7(2) . . ? C8 C13 C14 119.9(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C15 H15A 109.5 . . ? O1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 123.89(19) . . ? N1 C16 H16 118.1 . . ? C17 C16 H16 118.1 . . ? N2 C17 C18 107.56(18) . . ? N2 C17 C16 124.60(19) . . ? C18 C17 C16 127.7(2) . . ? C17 C18 C19 107.3(2) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? C20 C19 C18 107.2(2) . . ? C20 C19 H19 126.4 . . ? C18 C19 H19 126.4 . . ? N2 C20 C19 108.5(2) . . ? N2 C20 H20 125.8 . . ? C19 C20 H20 125.8 . . ? C26 C21 C22 119.29(18) . . ? C26 C21 C28 121.34(18) . . ? C22 C21 C28 119.36(18) . . ? O2 C22 C23 124.0(2) . . ? O2 C22 C21 115.40(17) . . ? C23 C22 C21 120.6(2) . . ? C24 C23 C22 119.1(2) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C25 C24 C23 121.1(2) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 120.8(2) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C21 C26 C25 119.0(2) . . ? C21 C26 C27 121.8(2) . . ? C25 C26 C27 119.2(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 119.03(17) . . ? C29 C28 C21 119.79(16) . . ? C33 C28 C21 121.18(17) . . ? C30 C29 C28 120.46(17) . . ? C30 C29 N3 117.71(17) . . ? C28 C29 N3 121.78(17) . . ? C31 C30 C29 119.76(19) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 120.12(19) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 121.07(18) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C28 119.51(18) . . ? C32 C33 C34 120.68(17) . . ? C28 C33 C34 119.80(18) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O2 C35 H35A 109.5 . . ? O2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 C37 124.7(2) . . ? N3 C36 H36 117.6 . . ? C37 C36 H36 117.6 . . ? N4 C37 C38 107.69(18) . . ? N4 C37 C36 125.19(19) . . ? C38 C37 C36 127.0(2) . . ? C37 C38 C39 107.3(2) . . ? C37 C38 H38 126.3 . . ? C39 C38 H38 126.3 . . ? C40 C39 C38 107.2(2) . . ? C40 C39 H39 126.4 . . ? C38 C39 H39 126.4 . . ? N4 C40 C39 109.0(2) . . ? N4 C40 H40 125.5 . . ? C39 C40 H40 125.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 O1 C2 C3 1.2(3) . . . . ? C15 O1 C2 C1 -179.5(2) . . . . ? C6 C1 C2 O1 177.76(18) . . . . ? C8 C1 C2 O1 -2.2(3) . . . . ? C6 C1 C2 C3 -2.9(3) . . . . ? C8 C1 C2 C3 177.1(2) . . . . ? O1 C2 C3 C4 -179.9(2) . . . . ? C1 C2 C3 C4 0.8(3) . . . . ? C2 C3 C4 C5 1.4(4) . . . . ? C3 C4 C5 C6 -1.5(4) . . . . ? C4 C5 C6 C1 -0.6(3) . . . . ? C4 C5 C6 C7 179.1(2) . . . . ? C2 C1 C6 C5 2.8(3) . . . . ? C8 C1 C6 C5 -177.2(2) . . . . ? C2 C1 C6 C7 -177.0(2) . . . . ? C8 C1 C6 C7 3.0(3) . . . . ? C2 C1 C8 C9 -90.5(2) . . . . ? C6 C1 C8 C9 89.5(3) . . . . ? C2 C1 C8 C13 86.6(2) . . . . ? C6 C1 C8 C13 -93.4(3) . . . . ? C13 C8 C9 C10 -2.4(3) . . . . ? C1 C8 C9 C10 174.8(2) . . . . ? C13 C8 C9 N1 174.1(2) . . . . ? C1 C8 C9 N1 -8.7(3) . . . . ? C16 N1 C9 C10 -115.8(2) . . . . ? C16 N1 C9 C8 67.5(3) . . . . ? C8 C9 C10 C11 0.7(4) . . . . ? N1 C9 C10 C11 -176.0(2) . . . . ? C9 C10 C11 C12 1.5(4) . . . . ? C10 C11 C12 C13 -1.9(4) . . . . ? C11 C12 C13 C8 0.2(4) . . . . ? C11 C12 C13 C14 -179.4(2) . . . . ? C9 C8 C13 C12 1.9(3) . . . . ? C1 C8 C13 C12 -175.2(2) . . . . ? C9 C8 C13 C14 -178.5(2) . . . . ? C1 C8 C13 C14 4.4(3) . . . . ? C9 N1 C16 C17 175.74(19) . . . . ? C20 N2 C17 C18 0.8(2) . . . . ? C20 N2 C17 C16 -174.7(2) . . . . ? N1 C16 C17 N2 -0.7(3) . . . . ? N1 C16 C17 C18 -175.2(2) . . . . ? N2 C17 C18 C19 -0.5(3) . . . . ? C16 C17 C18 C19 174.7(2) . . . . ? C17 C18 C19 C20 0.1(3) . . . . ? C17 N2 C20 C19 -0.7(3) . . . . ? C18 C19 C20 N2 0.4(3) . . . . ? C35 O2 C22 C23 11.9(3) . . . . ? C35 O2 C22 C21 -168.28(19) . . . . ? C26 C21 C22 O2 177.13(18) . . . . ? C28 C21 C22 O2 -4.0(3) . . . . ? C26 C21 C22 C23 -3.1(3) . . . . ? C28 C21 C22 C23 175.77(17) . . . . ? O2 C22 C23 C24 -179.88(19) . . . . ? C21 C22 C23 C24 0.4(3) . . . . ? C22 C23 C24 C25 1.9(3) . . . . ? C23 C24 C25 C26 -1.4(3) . . . . ? C22 C21 C26 C25 3.5(3) . . . . ? C28 C21 C26 C25 -175.30(19) . . . . ? C22 C21 C26 C27 -176.9(2) . . . . ? C28 C21 C26 C27 4.3(3) . . . . ? C24 C25 C26 C21 -1.3(3) . . . . ? C24 C25 C26 C27 179.1(2) . . . . ? C26 C21 C28 C29 96.1(2) . . . . ? C22 C21 C28 C29 -82.7(2) . . . . ? C26 C21 C28 C33 -83.0(2) . . . . ? C22 C21 C28 C33 98.1(2) . . . . ? C33 C28 C29 C30 1.0(3) . . . . ? C21 C28 C29 C30 -178.14(19) . . . . ? C33 C28 C29 N3 -176.41(18) . . . . ? C21 C28 C29 N3 4.4(3) . . . . ? C36 N3 C29 C30 114.0(2) . . . . ? C36 N3 C29 C28 -68.5(3) . . . . ? C28 C29 C30 C31 0.9(3) . . . . ? N3 C29 C30 C31 178.4(2) . . . . ? C29 C30 C31 C32 -1.8(4) . . . . ? C30 C31 C32 C33 0.7(3) . . . . ? C31 C32 C33 C28 1.2(3) . . . . ? C31 C32 C33 C34 -178.3(2) . . . . ? C29 C28 C33 C32 -2.1(3) . . . . ? C21 C28 C33 C32 177.09(19) . . . . ? C29 C28 C33 C34 177.5(2) . . . . ? C21 C28 C33 C34 -3.4(3) . . . . ? C29 N3 C36 C37 -177.35(18) . . . . ? C40 N4 C37 C38 0.5(2) . . . . ? C40 N4 C37 C36 177.42(19) . . . . ? N3 C36 C37 N4 1.6(3) . . . . ? N3 C36 C37 C38 177.9(2) . . . . ? N4 C37 C38 C39 -0.8(2) . . . . ? C36 C37 C38 C39 -177.6(2) . . . . ? C37 C38 C39 C40 0.7(3) . . . . ? C37 N4 C40 C39 -0.1(2) . . . . ? C38 C39 C40 N4 -0.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.197 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.039 # Attachment 'compound_5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 687845' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C85 H65 N6 O3 Y' _chemical_formula_sum 'C85 H65 N6 O3 Y' _chemical_formula_weight 1307.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 13.782(6) _cell_length_b 15.196(7) _cell_length_c 36.501(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7644(6) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11020 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 0.813 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9088 _exptl_absorpt_correction_T_max 0.9529 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57829 _diffrn_reflns_av_R_equivalents 0.1690 _diffrn_reflns_av_sigmaI/netI 0.1366 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13497 _reflns_number_gt 9737 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1955P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.116(13) _refine_ls_number_reflns 13497 _refine_ls_number_parameters 846 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.1792 _refine_ls_R_factor_gt 0.1453 _refine_ls_wR_factor_ref 0.3650 _refine_ls_wR_factor_gt 0.3392 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.166 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.27012(7) 0.55736(8) 0.88256(3) 0.0452(3) Uani 1 1 d . . . N1 N 0.3219(7) 0.5074(7) 0.8203(3) 0.052(2) Uani 1 1 d U . . N2 N 0.2332(7) 0.6677(7) 0.8377(2) 0.055(2) Uani 1 1 d . . . N3 N 0.0865(6) 0.5549(6) 0.8933(2) 0.039(2) Uani 1 1 d . . . N4 N 0.2336(6) 0.5260(6) 0.9445(2) 0.045(2) Uani 1 1 d . . . N5 N 0.3550(6) 0.6797(5) 0.9120(3) 0.043(2) Uani 1 1 d . . . N6 N 0.4322(7) 0.5155(5) 0.8990(3) 0.047(2) Uani 1 1 d U . . O1 O 0.2438(5) 0.3931(5) 0.8823(2) 0.0543(19) Uani 1 1 d . . . O2 O -0.1612(5) 0.5253(5) 0.9417(2) 0.055(2) Uani 1 1 d . . . O3 O 0.5215(5) 0.8364(6) 0.9670(2) 0.055(2) Uani 1 1 d . . . C1 C 0.2251(9) 0.3384(6) 0.8218(3) 0.049(3) Uani 1 1 d . . . C2 C 0.1843(9) 0.3566(9) 0.8545(4) 0.064(4) Uani 1 1 d . . . C3 C 0.0833(8) 0.3466(8) 0.8605(4) 0.056(3) Uani 1 1 d . . . H3A H 0.0560 0.3627 0.8834 0.067 Uiso 1 1 calc R . . C4 C 0.0253(8) 0.3143(8) 0.8336(4) 0.066(4) Uani 1 1 d . . . H4A H -0.0410 0.3021 0.8387 0.080 Uiso 1 1 calc R . . C5 C 0.0626(8) 0.2986(9) 0.7982(3) 0.054(3) Uani 1 1 d . . . C6 C 0.1630(8) 0.3116(8) 0.7905(3) 0.050(3) Uani 1 1 d . . . C7 C 0.1982(9) 0.2910(8) 0.7543(3) 0.061(4) Uani 1 1 d . . . H7A H 0.2658 0.2932 0.7493 0.073 Uiso 1 1 calc R . . C8 C 0.1373(10) 0.2694(8) 0.7283(3) 0.056(3) Uani 1 1 d . . . H8A H 0.1628 0.2609 0.7044 0.068 Uiso 1 1 calc R . . C9 C 0.0366(9) 0.2577(9) 0.7331(4) 0.065(4) Uani 1 1 d . . . H9A H -0.0048 0.2417 0.7134 0.078 Uiso 1 1 calc R . . C10 C 0.0008(9) 0.2711(9) 0.7691(4) 0.066(4) Uani 1 1 d . . . H10A H -0.0661 0.2615 0.7739 0.080 Uiso 1 1 calc R . . C11 C 0.3326(9) 0.3499(8) 0.8160(3) 0.051(3) Uani 1 1 d . . . C12 C 0.3772(9) 0.4278(8) 0.8132(3) 0.054(3) Uani 1 1 d . . . C13 C 0.4798(9) 0.4394(12) 0.8060(3) 0.073(4) Uani 1 1 d . . . H13A H 0.5110 0.4952 0.8051 0.087 Uiso 1 1 calc R . . C14 C 0.5308(10) 0.3548(12) 0.8001(4) 0.080(5) Uani 1 1 d . . . H14A H 0.5980 0.3579 0.7944 0.096 Uiso 1 1 calc R . . C15 C 0.4924(10) 0.2762(8) 0.8020(3) 0.056(3) Uani 1 1 d U . . C16 C 0.3859(9) 0.2679(10) 0.8104(3) 0.062(3) Uani 1 1 d . . . C17 C 0.3526(11) 0.1805(12) 0.8136(4) 0.083(5) Uani 1 1 d . . . H17A H 0.2865 0.1734 0.8204 0.100 Uiso 1 1 calc R . . C18 C 0.4013(13) 0.1087(10) 0.8084(4) 0.084(5) Uani 1 1 d . . . H18A H 0.3703 0.0528 0.8088 0.100 Uiso 1 1 calc R . . C19 C 0.5067(12) 0.1164(11) 0.8016(4) 0.084(4) Uani 1 1 d U . . H19A H 0.5458 0.0650 0.8000 0.100 Uiso 1 1 calc R . . C20 C 0.5492(15) 0.2007(13) 0.7976(5) 0.099(5) Uani 1 1 d U . . H20A H 0.6163 0.2060 0.7920 0.119 Uiso 1 1 calc R . . C21 C 0.2614(10) 0.3292(8) 0.9120(4) 0.065(3) Uani 1 1 d . . . H21A H 0.2445 0.2700 0.9035 0.098 Uiso 1 1 calc R . . H21B H 0.2214 0.3445 0.9333 0.098 Uiso 1 1 calc R . . H21C H 0.3301 0.3307 0.9190 0.098 Uiso 1 1 calc R . . C22 C 0.3150(9) 0.5637(9) 0.7972(4) 0.062(3) Uani 1 1 d . . . H22A H 0.3419 0.5519 0.7738 0.074 Uiso 1 1 calc R . . C23 C 0.2708(9) 0.6441(7) 0.8026(3) 0.052(3) Uani 1 1 d . . . C24 C 0.2460(10) 0.7144(11) 0.7800(4) 0.082(4) Uani 1 1 d . . . H24A H 0.2601 0.7164 0.7545 0.098 Uiso 1 1 calc R . . C25 C 0.1979(9) 0.7824(10) 0.7989(3) 0.064(3) Uani 1 1 d U . . H25A H 0.1755 0.8373 0.7897 0.077 Uiso 1 1 calc R . . C26 C 0.1910(8) 0.7484(8) 0.8357(4) 0.056(3) Uani 1 1 d . . . H26A H 0.1612 0.7781 0.8556 0.067 Uiso 1 1 calc R . . C27 C -0.0998(7) 0.6509(10) 0.9125(3) 0.061(4) Uani 1 1 d . . . C28 C -0.1427(8) 0.6128(7) 0.9456(3) 0.044(3) Uani 1 1 d U . . C29 C -0.1614(7) 0.6602(10) 0.9757(3) 0.052(3) Uani 1 1 d . . . H29A H -0.1854 0.6323 0.9972 0.063 Uiso 1 1 calc R . . C30 C -0.1451(7) 0.7523(10) 0.9753(3) 0.056(4) Uani 1 1 d . . . H30A H -0.1609 0.7861 0.9964 0.067 Uiso 1 1 calc R . . C31 C -0.1054(7) 0.7953(9) 0.9439(3) 0.050(3) Uani 1 1 d . . . C32 C -0.0842(8) 0.7467(8) 0.9125(3) 0.047(3) Uani 1 1 d . . . C33 C -0.0475(7) 0.7854(8) 0.8813(3) 0.049(3) Uani 1 1 d . . . H33A H -0.0299 0.7499 0.8610 0.058 Uiso 1 1 calc R . . C34 C -0.0362(8) 0.8759(9) 0.8795(4) 0.061(3) Uani 1 1 d . . . H34A H -0.0134 0.9027 0.8576 0.073 Uiso 1 1 calc R . . C35 C -0.0594(8) 0.9298(11) 0.9114(4) 0.073(4) Uani 1 1 d . . . H35A H -0.0513 0.9919 0.9109 0.088 Uiso 1 1 calc R . . C36 C -0.0932(8) 0.8877(9) 0.9420(4) 0.062(3) Uani 1 1 d . . . H36A H -0.1091 0.9220 0.9630 0.075 Uiso 1 1 calc R . . C37 C -0.0829(7) 0.6003(8) 0.8771(3) 0.051(3) Uani 1 1 d . . . C38 C 0.0085(7) 0.5646(8) 0.8680(3) 0.044(2) Uani 1 1 d . . . C39 C 0.0218(8) 0.5392(6) 0.8318(3) 0.043(3) Uani 1 1 d U . . H39A H 0.0848 0.5203 0.8248 0.051 Uiso 1 1 calc R . . C40 C -0.0487(9) 0.5393(11) 0.8056(3) 0.074(4) Uani 1 1 d . . . H40A H -0.0333 0.5228 0.7811 0.088 Uiso 1 1 calc R . . C41 C -0.1445(8) 0.5639(9) 0.8148(3) 0.060(3) Uani 1 1 d . . . C42 C -0.1627(9) 0.5985(10) 0.8503(3) 0.063(4) Uani 1 1 d . . . C43 C -0.2572(8) 0.6289(7) 0.8596(3) 0.050(3) Uani 1 1 d . . . H43A H -0.2695 0.6491 0.8838 0.061 Uiso 1 1 calc R . . C44 C -0.3293(8) 0.6298(9) 0.8350(4) 0.063(4) Uani 1 1 d . . . H44A H -0.3915 0.6515 0.8415 0.076 Uiso 1 1 calc R . . C45 C -0.3121(10) 0.5983(11) 0.7993(4) 0.081(5) Uani 1 1 d . . . H45A H -0.3629 0.5999 0.7817 0.097 Uiso 1 1 calc R . . C46 C -0.2234(9) 0.5655(10) 0.7897(4) 0.066(3) Uani 1 1 d . . . H46A H -0.2142 0.5432 0.7656 0.080 Uiso 1 1 calc R . . C47 C -0.1925(9) 0.4795(10) 0.9736(4) 0.071(4) Uani 1 1 d . . . H47A H -0.2044 0.4176 0.9675 0.106 Uiso 1 1 calc R . . H47B H -0.2524 0.5062 0.9828 0.106 Uiso 1 1 calc R . . H47C H -0.1421 0.4831 0.9925 0.106 Uiso 1 1 calc R . . C48 C 0.0673(8) 0.5243(8) 0.9243(3) 0.053(3) Uani 1 1 d . . . H48A H 0.0011 0.5120 0.9295 0.063 Uiso 1 1 calc R . . C49 C 0.1347(8) 0.5064(8) 0.9520(4) 0.054(3) Uani 1 1 d . . . C50 C 0.1256(10) 0.4746(10) 0.9886(3) 0.069(4) Uani 1 1 d . . . H50A H 0.0678 0.4570 1.0007 0.083 Uiso 1 1 calc R . . C51 C 0.2228(8) 0.4747(7) 1.0032(3) 0.050(3) Uani 1 1 d . . . H51A H 0.2414 0.4568 1.0271 0.059 Uiso 1 1 calc R . . C52 C 0.2830(9) 0.5049(7) 0.9765(4) 0.054(3) Uani 1 1 d . . . H52A H 0.3512 0.5110 0.9794 0.065 Uiso 1 1 calc R . . C53 C 0.4818(7) 0.8456(7) 0.9027(4) 0.046(3) Uani 1 1 d . . . C54 C 0.5532(7) 0.8431(7) 0.9318(4) 0.050(3) Uani 1 1 d . . . C55 C 0.6519(7) 0.8509(7) 0.9200(4) 0.055(3) Uani 1 1 d . . . H55A H 0.7020 0.8505 0.9378 0.066 Uiso 1 1 calc R . . C56 C 0.6770(7) 0.8591(8) 0.8828(3) 0.053(3) Uani 1 1 d . . . H56A H 0.7434 0.8640 0.8760 0.064 Uiso 1 1 calc R . . C57 C 0.6075(8) 0.8601(8) 0.8567(3) 0.053(3) Uani 1 1 d . . . C58 C 0.5064(8) 0.8512(10) 0.8660(3) 0.059(3) Uani 1 1 d . . . C59 C 0.4350(9) 0.8474(9) 0.8374(3) 0.059(3) Uani 1 1 d . . . H59A H 0.3687 0.8370 0.8430 0.071 Uiso 1 1 calc R . . C60 C 0.4639(9) 0.8588(9) 0.8025(4) 0.066(4) Uani 1 1 d . . . H60A H 0.4155 0.8649 0.7842 0.079 Uiso 1 1 calc R . . C61 C 0.5614(9) 0.8623(8) 0.7917(4) 0.059(3) Uani 1 1 d U . . H61A H 0.5785 0.8631 0.7665 0.071 Uiso 1 1 calc R . . C62 C 0.6319(9) 0.8645(10) 0.8185(4) 0.075(4) Uani 1 1 d . . . H62A H 0.6981 0.8690 0.8115 0.090 Uiso 1 1 calc R . . C63 C 0.3721(7) 0.8445(8) 0.9156(3) 0.043(3) Uani 1 1 d . . . C64 C 0.3199(7) 0.7661(8) 0.9192(3) 0.046(3) Uani 1 1 d . . . C65 C 0.2170(7) 0.7765(7) 0.9298(3) 0.042(3) Uani 1 1 d . . . H65A H 0.1770 0.7256 0.9310 0.050 Uiso 1 1 calc R . . C66 C 0.1799(8) 0.8515(9) 0.9373(3) 0.055(3) Uani 1 1 d . . . H66A H 0.1148 0.8527 0.9459 0.066 Uiso 1 1 calc R . . C67 C 0.2293(9) 0.9334(9) 0.9338(3) 0.056(3) Uani 1 1 d . . . C68 C 0.3291(7) 0.9259(7) 0.9228(3) 0.040(2) Uani 1 1 d . . . C69 C 0.3811(8) 1.0067(9) 0.9185(3) 0.059(3) Uani 1 1 d . . . H69A H 0.4476 1.0052 0.9117 0.071 Uiso 1 1 calc R . . C70 C 0.3371(8) 1.0854(8) 0.9240(3) 0.049(3) Uani 1 1 d . . . H70A H 0.3716 1.1383 0.9194 0.059 Uiso 1 1 calc R . . C71 C 0.2385(10) 1.0893(9) 0.9368(3) 0.064(4) Uani 1 1 d . . . H71A H 0.2104 1.1445 0.9429 0.076 Uiso 1 1 calc R . . C72 C 0.1857(9) 1.0149(7) 0.9402(3) 0.049(3) Uani 1 1 d . . . H72A H 0.1192 1.0180 0.9469 0.058 Uiso 1 1 calc R . . C73 C 0.5905(7) 0.8063(7) 0.9929(3) 0.044(3) Uani 1 1 d . . . H73A H 0.5603 0.8031 1.0172 0.066 Uiso 1 1 calc R . . H73B H 0.6455 0.8471 0.9937 0.066 Uiso 1 1 calc R . . H73C H 0.6135 0.7477 0.9857 0.066 Uiso 1 1 calc R . . C74 C 0.4367(9) 0.6584(9) 0.9267(3) 0.056(3) Uani 1 1 d . . . H74A H 0.4698 0.7006 0.9413 0.067 Uiso 1 1 calc R . . C75 C 0.4778(9) 0.5764(9) 0.9219(3) 0.059(3) Uani 1 1 d . . . C76 C 0.5667(9) 0.5347(11) 0.9352(4) 0.077(5) Uani 1 1 d . . . H76A H 0.6135 0.5619 0.9506 0.093 Uiso 1 1 calc R . . C77 C 0.5721(8) 0.4503(9) 0.9221(4) 0.065(3) Uani 1 1 d . . . H77A H 0.6215 0.4080 0.9264 0.078 Uiso 1 1 calc R . . C78 C 0.4874(9) 0.4406(8) 0.9009(3) 0.055(3) Uani 1 1 d . . . H78A H 0.4702 0.3873 0.8890 0.066 Uiso 1 1 calc R . . C79 C -0.1215(17) 0.0283(16) 0.7832(6) 0.132(7) Uani 1 1 d U . . H79A H -0.1774 0.0382 0.7993 0.198 Uiso 1 1 calc R . . H79B H -0.1241 -0.0317 0.7734 0.198 Uiso 1 1 calc R . . H79C H -0.1229 0.0706 0.7630 0.198 Uiso 1 1 calc R . . C80 C -0.0269(10) 0.0404(10) 0.8054(4) 0.130(7) Uani 1 1 d GU . . C81 C -0.0272(10) 0.0943(9) 0.8361(4) 0.111(6) Uani 1 1 d GU . . H81 H -0.0843 0.1256 0.8426 0.133 Uiso 1 1 calc R . . C82 C 0.0561(12) 0.1024(9) 0.8573(3) 0.156(9) Uani 1 1 d GU . . H82 H 0.0559 0.1392 0.8784 0.187 Uiso 1 1 calc R . . C83 C 0.1396(10) 0.0565(11) 0.8478(4) 0.129(7) Uani 1 1 d GU . . H83 H 0.1965 0.0620 0.8623 0.155 Uiso 1 1 calc R . . C84 C 0.1399(10) 0.0026(10) 0.8171(4) 0.129(7) Uani 1 1 d GU . . H84 H 0.1970 -0.0288 0.8106 0.155 Uiso 1 1 calc R . . C85 C 0.0566(12) -0.0055(9) 0.7958(3) 0.123(7) Uani 1 1 d GU . . H85 H 0.0568 -0.0424 0.7748 0.148 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0290(5) 0.0590(7) 0.0475(5) -0.0039(5) 0.0006(5) 0.0001(5) N1 0.046(5) 0.042(5) 0.069(6) 0.003(5) -0.004(4) -0.023(4) N2 0.035(5) 0.076(7) 0.055(6) 0.016(5) -0.009(5) -0.016(5) N3 0.039(5) 0.031(4) 0.048(5) 0.011(4) -0.003(4) 0.008(4) N4 0.032(4) 0.067(6) 0.036(4) -0.006(4) -0.001(4) 0.000(4) N5 0.018(4) 0.029(5) 0.081(6) 0.003(4) -0.010(4) 0.000(3) N6 0.054(5) 0.015(4) 0.071(5) -0.005(4) 0.005(4) 0.009(4) O1 0.050(5) 0.067(5) 0.046(4) -0.001(4) 0.003(4) -0.017(4) O2 0.042(4) 0.069(6) 0.054(5) 0.009(4) 0.015(4) 0.000(4) O3 0.035(4) 0.087(6) 0.044(4) -0.001(4) 0.000(3) -0.006(4) C1 0.044(6) 0.015(5) 0.089(8) 0.011(5) 0.034(7) 0.002(5) C2 0.041(7) 0.065(8) 0.086(10) 0.017(7) -0.006(7) 0.021(6) C3 0.027(6) 0.067(8) 0.073(8) -0.015(6) 0.006(6) 0.011(5) C4 0.027(6) 0.049(7) 0.123(12) -0.023(7) 0.005(7) 0.001(5) C5 0.034(6) 0.070(8) 0.057(7) -0.006(6) 0.010(5) -0.007(6) C6 0.042(6) 0.046(7) 0.061(7) 0.003(6) -0.013(5) -0.019(5) C7 0.044(7) 0.075(9) 0.064(8) -0.042(7) 0.005(6) -0.021(6) C8 0.075(9) 0.050(7) 0.044(6) -0.017(5) 0.005(6) -0.021(6) C9 0.035(6) 0.083(10) 0.078(9) -0.009(7) -0.018(6) 0.000(6) C10 0.039(7) 0.081(9) 0.080(9) -0.033(7) 0.017(6) 0.004(6) C11 0.046(7) 0.055(8) 0.052(7) 0.000(6) -0.005(5) -0.006(6) C12 0.059(7) 0.058(8) 0.045(6) 0.008(6) 0.006(5) -0.008(6) C13 0.052(8) 0.104(11) 0.062(8) -0.016(8) 0.004(6) 0.000(8) C14 0.047(8) 0.128(14) 0.064(9) 0.001(8) 0.020(7) 0.027(9) C15 0.065(7) 0.036(6) 0.066(6) 0.000(5) 0.007(5) -0.017(5) C16 0.051(7) 0.073(10) 0.063(8) -0.003(7) 0.028(6) -0.013(7) C17 0.053(8) 0.115(14) 0.082(10) 0.003(10) -0.004(7) 0.035(9) C18 0.094(12) 0.050(9) 0.107(12) -0.006(8) 0.002(10) -0.015(8) C19 0.076(8) 0.089(8) 0.086(8) -0.005(7) 0.005(6) 0.026(7) C20 0.097(9) 0.106(9) 0.095(8) -0.010(7) 0.007(7) 0.010(8) C21 0.046(7) 0.063(8) 0.086(9) 0.016(7) -0.008(7) -0.003(6) C22 0.045(7) 0.040(7) 0.100(10) -0.020(8) 0.007(7) -0.006(6) C23 0.048(6) 0.054(7) 0.054(7) 0.008(5) -0.021(6) -0.038(6) C24 0.053(9) 0.096(11) 0.096(10) 0.021(9) 0.012(7) -0.010(8) C25 0.045(6) 0.089(7) 0.059(6) 0.031(6) -0.013(5) 0.008(6) C26 0.029(6) 0.056(8) 0.082(9) -0.022(6) -0.019(6) 0.003(5) C27 0.023(5) 0.117(12) 0.042(6) 0.032(7) -0.013(5) 0.016(6) C28 0.038(5) 0.027(5) 0.066(6) 0.008(5) -0.010(5) -0.002(4) C29 0.023(5) 0.099(11) 0.036(6) -0.015(6) -0.002(4) -0.013(6) C30 0.012(5) 0.112(12) 0.043(6) -0.018(7) -0.008(4) 0.012(6) C31 0.019(5) 0.082(10) 0.050(7) -0.001(6) -0.006(5) 0.007(5) C32 0.035(6) 0.051(7) 0.056(7) 0.011(6) -0.020(5) -0.004(5) C33 0.029(5) 0.058(7) 0.059(7) 0.005(6) -0.003(5) 0.021(5) C34 0.035(6) 0.096(11) 0.051(7) 0.016(7) -0.009(6) 0.004(6) C35 0.023(6) 0.108(11) 0.088(10) 0.016(9) -0.011(6) 0.008(7) C36 0.034(6) 0.064(9) 0.088(10) -0.004(7) 0.003(6) 0.025(6) C37 0.034(6) 0.072(8) 0.047(7) 0.026(6) -0.014(5) 0.005(5) C38 0.037(6) 0.056(7) 0.041(5) -0.005(5) 0.016(4) 0.009(5) C39 0.039(5) 0.018(5) 0.071(6) 0.014(4) -0.003(5) 0.002(4) C40 0.042(7) 0.129(13) 0.050(7) 0.001(8) -0.007(6) 0.010(8) C41 0.044(7) 0.064(8) 0.072(8) -0.010(7) -0.011(6) -0.017(6) C42 0.043(7) 0.106(11) 0.040(7) 0.020(6) 0.000(5) -0.011(7) C43 0.042(7) 0.054(7) 0.055(6) 0.013(5) -0.010(5) 0.010(5) C44 0.022(6) 0.081(9) 0.086(10) -0.017(7) -0.008(6) -0.019(6) C45 0.044(8) 0.104(12) 0.095(11) 0.029(9) -0.013(8) -0.050(8) C46 0.034(6) 0.089(9) 0.076(8) -0.009(7) -0.001(6) -0.019(7) C47 0.037(6) 0.088(10) 0.087(10) 0.014(8) -0.011(7) 0.013(7) C48 0.031(6) 0.076(9) 0.051(7) 0.016(6) -0.016(5) 0.007(6) C49 0.035(6) 0.046(7) 0.082(9) -0.018(6) -0.004(6) 0.003(5) C50 0.051(8) 0.106(11) 0.050(7) 0.016(7) 0.003(6) -0.017(7) C51 0.045(6) 0.058(7) 0.046(6) -0.001(5) -0.001(5) 0.017(6) C52 0.041(6) 0.035(6) 0.086(9) -0.010(6) 0.004(6) -0.005(5) C53 0.021(5) 0.028(6) 0.087(9) -0.006(5) -0.002(5) 0.006(4) C54 0.024(5) 0.032(6) 0.092(9) -0.011(6) -0.003(5) -0.009(5) C55 0.019(5) 0.042(7) 0.104(10) 0.006(6) -0.019(6) 0.016(5) C56 0.025(5) 0.077(8) 0.057(7) 0.003(6) 0.000(6) -0.011(5) C57 0.028(6) 0.068(8) 0.064(8) 0.015(6) -0.004(5) 0.000(5) C58 0.029(6) 0.099(10) 0.050(7) -0.003(6) 0.009(5) 0.003(6) C59 0.040(7) 0.085(9) 0.052(7) -0.010(6) -0.003(5) -0.004(6) C60 0.047(7) 0.086(10) 0.063(8) 0.003(7) -0.023(6) 0.007(7) C61 0.041(6) 0.070(7) 0.066(6) 0.007(5) 0.008(5) -0.018(5) C62 0.023(6) 0.107(12) 0.095(11) 0.025(9) 0.004(6) 0.021(7) C63 0.021(5) 0.069(8) 0.039(6) 0.017(5) 0.002(4) 0.001(5) C64 0.021(5) 0.078(8) 0.039(6) -0.007(5) -0.012(4) -0.023(5) C65 0.021(5) 0.029(5) 0.076(7) 0.005(5) -0.012(5) 0.003(5) C66 0.023(5) 0.082(9) 0.060(7) 0.025(6) -0.001(5) 0.028(6) C67 0.043(6) 0.073(9) 0.050(6) 0.018(6) -0.010(5) -0.033(7) C68 0.025(5) 0.046(7) 0.051(6) -0.005(5) -0.007(4) 0.001(5) C69 0.029(6) 0.098(11) 0.049(7) 0.001(7) 0.000(5) 0.018(7) C70 0.039(6) 0.057(8) 0.051(7) -0.008(5) 0.002(5) 0.004(5) C71 0.058(8) 0.081(9) 0.052(7) 0.005(6) -0.001(6) 0.028(7) C72 0.048(7) 0.034(6) 0.064(8) -0.003(5) 0.001(6) -0.004(6) C73 0.024(5) 0.047(7) 0.061(7) 0.017(5) -0.003(5) 0.000(5) C74 0.042(7) 0.072(9) 0.054(7) -0.006(6) 0.018(6) 0.005(6) C75 0.044(7) 0.063(9) 0.069(8) -0.014(7) 0.013(6) -0.015(6) C76 0.029(6) 0.117(14) 0.086(9) 0.031(9) -0.016(6) 0.028(7) C77 0.037(6) 0.034(7) 0.124(11) 0.005(7) 0.001(7) 0.001(6) C78 0.079(9) 0.035(6) 0.051(6) 0.003(6) -0.002(6) -0.026(7) C79 0.128(11) 0.149(11) 0.119(10) -0.009(8) -0.015(8) -0.005(9) C80 0.131(11) 0.138(11) 0.122(10) 0.020(8) -0.015(8) -0.005(9) C81 0.120(10) 0.107(9) 0.105(9) 0.014(8) -0.010(8) -0.011(8) C82 0.160(12) 0.153(12) 0.156(12) 0.011(9) -0.005(9) 0.003(9) C83 0.126(10) 0.135(10) 0.127(10) 0.005(9) -0.001(8) -0.009(9) C84 0.123(11) 0.137(11) 0.126(10) -0.001(8) 0.004(8) -0.006(8) C85 0.120(10) 0.135(10) 0.114(10) 0.000(8) -0.014(8) -0.008(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N4 2.365(8) . ? Y1 N6 2.399(9) . ? Y1 N2 2.399(9) . ? Y1 N5 2.445(9) . ? Y1 N1 2.501(10) . ? Y1 O1 2.523(8) . ? Y1 N3 2.561(8) . ? N1 C22 1.203(17) . ? N1 C12 1.453(16) . ? N2 C26 1.359(15) . ? N2 C23 1.427(16) . ? N3 C48 1.252(13) . ? N3 C38 1.424(13) . ? N4 C52 1.388(15) . ? N4 C49 1.422(14) . ? N5 C74 1.289(15) . ? N5 C64 1.422(15) . ? N6 C78 1.370(15) . ? N6 C75 1.395(15) . ? O1 C2 1.417(16) . ? O1 C21 1.474(14) . ? O2 C28 1.361(13) . ? O2 C47 1.425(16) . ? O3 C54 1.361(14) . ? O3 C73 1.417(12) . ? C1 C2 1.348(18) . ? C1 C6 1.485(17) . ? C1 C11 1.507(16) . ? C2 C3 1.417(17) . ? C3 C4 1.358(17) . ? C3 H3A 0.9500 . ? C4 C5 1.412(18) . ? C4 H4A 0.9500 . ? C5 C10 1.423(17) . ? C5 C6 1.425(16) . ? C6 C7 1.442(17) . ? C7 C8 1.310(16) . ? C7 H7A 0.9500 . ? C8 C9 1.410(18) . ? C8 H8A 0.9500 . ? C9 C10 1.417(18) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.337(17) . ? C11 C16 1.460(19) . ? C12 C13 1.449(18) . ? C13 C14 1.48(2) . ? C13 H13A 0.9500 . ? C14 C15 1.31(2) . ? C14 H14A 0.9500 . ? C15 C20 1.40(2) . ? C15 C16 1.505(18) . ? C16 C17 1.41(2) . ? C17 C18 1.30(2) . ? C17 H17A 0.9500 . ? C18 C19 1.48(2) . ? C18 H18A 0.9500 . ? C19 C20 1.42(2) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.380(18) . ? C22 H22A 0.9500 . ? C23 C24 1.392(19) . ? C24 C25 1.41(2) . ? C24 H24A 0.9500 . ? C25 C26 1.441(18) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.465(16) . ? C27 C32 1.472(18) . ? C27 C37 1.519(18) . ? C28 C29 1.340(16) . ? C29 C30 1.418(18) . ? C29 H29A 0.9500 . ? C30 C31 1.429(17) . ? C30 H30A 0.9500 . ? C31 C32 1.394(17) . ? C31 C36 1.417(19) . ? C32 C33 1.377(16) . ? C33 C34 1.386(17) . ? C33 H33A 0.9500 . ? C34 C35 1.46(2) . ? C34 H34A 0.9500 . ? C35 C36 1.370(19) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.411(15) . ? C37 C42 1.472(15) . ? C38 C39 1.388(15) . ? C39 C40 1.365(16) . ? C39 H39A 0.9500 . ? C40 C41 1.413(18) . ? C40 H40A 0.9500 . ? C41 C46 1.422(17) . ? C41 C42 1.422(18) . ? C42 C43 1.423(17) . ? C43 C44 1.339(16) . ? C43 H43A 0.9500 . ? C44 C45 1.41(2) . ? C44 H44A 0.9500 . ? C45 C46 1.37(2) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.401(16) . ? C48 H48A 0.9500 . ? C49 C50 1.424(18) . ? C50 C51 1.442(18) . ? C50 H50A 0.9500 . ? C51 C52 1.361(16) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? C53 C58 1.381(16) . ? C53 C54 1.449(16) . ? C53 C63 1.585(14) . ? C54 C55 1.432(16) . ? C55 C56 1.406(18) . ? C55 H55A 0.9500 . ? C56 C57 1.351(16) . ? C56 H56A 0.9500 . ? C57 C62 1.437(18) . ? C57 C58 1.441(16) . ? C58 C59 1.436(17) . ? C59 C60 1.346(18) . ? C59 H59A 0.9500 . ? C60 C61 1.401(18) . ? C60 H60A 0.9500 . ? C61 C62 1.380(18) . ? C61 H61A 0.9500 . ? C62 H62A 0.9500 . ? C63 C68 1.396(15) . ? C63 C64 1.398(15) . ? C64 C65 1.478(14) . ? C65 C66 1.280(15) . ? C65 H65A 0.9500 . ? C66 C67 1.425(17) . ? C66 H66A 0.9500 . ? C67 C72 1.397(17) . ? C67 C68 1.438(16) . ? C68 C69 1.430(17) . ? C69 C70 1.356(16) . ? C69 H69A 0.9500 . ? C70 C71 1.438(18) . ? C70 H70A 0.9500 . ? C71 C72 1.350(18) . ? C71 H71A 0.9500 . ? C72 H72A 0.9500 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C75 1.381(17) . ? C74 H74A 0.9500 . ? C75 C76 1.463(17) . ? C76 C77 1.37(2) . ? C76 H76A 0.9500 . ? C77 C78 1.407(17) . ? C77 H77A 0.9500 . ? C78 H78A 0.9500 . ? C79 C80 1.54(2) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C81 1.3900 . ? C80 C85 1.3900 . ? C81 C82 1.3900 . ? C81 H81 0.9500 . ? C82 C83 1.3900 . ? C82 H82 0.9500 . ? C83 C84 1.3900 . ? C83 H83 0.9500 . ? C84 C85 1.3900 . ? C84 H84 0.9500 . ? C85 H85 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Y1 N6 84.6(3) . . ? N4 Y1 N2 138.5(3) . . ? N6 Y1 N2 123.6(3) . . ? N4 Y1 N5 80.5(3) . . ? N6 Y1 N5 69.3(3) . . ? N2 Y1 N5 82.5(3) . . ? N4 Y1 N1 150.3(3) . . ? N6 Y1 N1 83.2(3) . . ? N2 Y1 N1 69.6(4) . . ? N5 Y1 N1 119.6(3) . . ? N4 Y1 O1 76.9(3) . . ? N6 Y1 O1 82.6(3) . . ? N2 Y1 O1 131.2(3) . . ? N5 Y1 O1 145.4(3) . . ? N1 Y1 O1 74.8(3) . . ? N4 Y1 N3 68.9(3) . . ? N6 Y1 N3 151.4(3) . . ? N2 Y1 N3 84.6(3) . . ? N5 Y1 N3 114.6(3) . . ? N1 Y1 N3 114.6(3) . . ? O1 Y1 N3 81.0(3) . . ? C22 N1 C12 120.6(11) . . ? C22 N1 Y1 113.4(9) . . ? C12 N1 Y1 124.3(7) . . ? C26 N2 C23 109.5(9) . . ? C26 N2 Y1 139.3(8) . . ? C23 N2 Y1 111.2(8) . . ? C48 N3 C38 117.6(9) . . ? C48 N3 Y1 110.7(7) . . ? C38 N3 Y1 130.2(6) . . ? C52 N4 C49 105.1(9) . . ? C52 N4 Y1 138.2(7) . . ? C49 N4 Y1 115.5(7) . . ? C74 N5 C64 116.9(9) . . ? C74 N5 Y1 114.2(8) . . ? C64 N5 Y1 128.3(6) . . ? C78 N6 C75 105.7(10) . . ? C78 N6 Y1 138.6(7) . . ? C75 N6 Y1 113.2(7) . . ? C2 O1 C21 111.3(9) . . ? C2 O1 Y1 118.2(7) . . ? C21 O1 Y1 128.7(7) . . ? C28 O2 C47 116.6(10) . . ? C54 O3 C73 115.9(8) . . ? C2 C1 C6 119.8(11) . . ? C2 C1 C11 120.7(12) . . ? C6 C1 C11 119.4(10) . . ? C1 C2 C3 121.5(13) . . ? C1 C2 O1 118.2(11) . . ? C3 C2 O1 120.0(12) . . ? C4 C3 C2 120.5(12) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 120.5(11) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C4 C5 C10 120.9(10) . . ? C4 C5 C6 120.6(11) . . ? C10 C5 C6 118.4(10) . . ? C5 C6 C7 118.4(10) . . ? C5 C6 C1 116.6(10) . . ? C7 C6 C1 124.8(10) . . ? C8 C7 C6 120.2(11) . . ? C8 C7 H7A 119.9 . . ? C6 C7 H7A 119.9 . . ? C7 C8 C9 124.9(12) . . ? C7 C8 H8A 117.5 . . ? C9 C8 H8A 117.5 . . ? C8 C9 C10 116.1(11) . . ? C8 C9 H9A 121.9 . . ? C10 C9 H9A 121.9 . . ? C9 C10 C5 121.6(11) . . ? C9 C10 H10A 119.2 . . ? C5 C10 H10A 119.2 . . ? C12 C11 C16 120.9(11) . . ? C12 C11 C1 124.4(11) . . ? C16 C11 C1 114.5(10) . . ? C11 C12 C13 124.8(13) . . ? C11 C12 N1 118.8(11) . . ? C13 C12 N1 116.3(11) . . ? C12 C13 C14 112.5(14) . . ? C12 C13 H13A 123.8 . . ? C14 C13 H13A 123.8 . . ? C15 C14 C13 126.4(13) . . ? C15 C14 H14A 116.8 . . ? C13 C14 H14A 116.8 . . ? C14 C15 C20 121.1(14) . . ? C14 C15 C16 118.8(12) . . ? C20 C15 C16 120.1(13) . . ? C17 C16 C11 129.0(11) . . ? C17 C16 C15 114.4(12) . . ? C11 C16 C15 116.6(11) . . ? C18 C17 C16 127.8(15) . . ? C18 C17 H17A 116.1 . . ? C16 C17 H17A 116.1 . . ? C17 C18 C19 117.8(15) . . ? C17 C18 H18A 121.1 . . ? C19 C18 H18A 121.1 . . ? C20 C19 C18 119.7(15) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C15 C20 C19 119.9(17) . . ? C15 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C23 124.5(13) . . ? N1 C22 H22A 117.7 . . ? C23 C22 H22A 117.7 . . ? C22 C23 C24 134.8(13) . . ? C22 C23 N2 120.6(11) . . ? C24 C23 N2 104.5(12) . . ? C23 C24 C25 112.8(13) . . ? C23 C24 H24A 123.6 . . ? C25 C24 H24A 123.6 . . ? C24 C25 C26 102.9(12) . . ? C24 C25 H25A 128.5 . . ? C26 C25 H25A 128.5 . . ? N2 C26 C25 110.2(11) . . ? N2 C26 H26A 124.9 . . ? C25 C26 H26A 124.9 . . ? C28 C27 C32 116.7(11) . . ? C28 C27 C37 124.2(12) . . ? C32 C27 C37 118.6(10) . . ? C29 C28 O2 125.1(11) . . ? C29 C28 C27 122.9(11) . . ? O2 C28 C27 112.0(11) . . ? C28 C29 C30 119.4(11) . . ? C28 C29 H29A 120.3 . . ? C30 C29 H29A 120.3 . . ? C29 C30 C31 121.4(11) . . ? C29 C30 H30A 119.3 . . ? C31 C30 H30A 119.3 . . ? C32 C31 C36 117.4(11) . . ? C32 C31 C30 119.9(12) . . ? C36 C31 C30 122.5(12) . . ? C33 C32 C31 122.1(11) . . ? C33 C32 C27 118.3(11) . . ? C31 C32 C27 119.6(11) . . ? C32 C33 C34 120.3(12) . . ? C32 C33 H33A 119.9 . . ? C34 C33 H33A 119.9 . . ? C33 C34 C35 119.7(12) . . ? C33 C34 H34A 120.1 . . ? C35 C34 H34A 120.1 . . ? C36 C35 C34 117.6(14) . . ? C36 C35 H35A 121.2 . . ? C34 C35 H35A 121.2 . . ? C35 C36 C31 122.9(13) . . ? C35 C36 H36A 118.6 . . ? C31 C36 H36A 118.6 . . ? C38 C37 C42 120.2(11) . . ? C38 C37 C27 122.1(9) . . ? C42 C37 C27 117.3(10) . . ? C39 C38 C37 116.6(10) . . ? C39 C38 N3 119.2(9) . . ? C37 C38 N3 124.2(9) . . ? C40 C39 C38 125.1(11) . . ? C40 C39 H39A 117.5 . . ? C38 C39 H39A 117.5 . . ? C39 C40 C41 119.8(12) . . ? C39 C40 H40A 120.1 . . ? C41 C40 H40A 120.1 . . ? C40 C41 C46 124.5(12) . . ? C40 C41 C42 118.7(11) . . ? C46 C41 C42 116.5(12) . . ? C41 C42 C43 119.9(11) . . ? C41 C42 C37 118.7(11) . . ? C43 C42 C37 121.3(11) . . ? C44 C43 C42 121.5(12) . . ? C44 C43 H43A 119.3 . . ? C42 C43 H43A 119.3 . . ? C43 C44 C45 119.5(12) . . ? C43 C44 H44A 120.2 . . ? C45 C44 H44A 120.2 . . ? C46 C45 C44 120.8(13) . . ? C46 C45 H45A 119.6 . . ? C44 C45 H45A 119.6 . . ? C45 C46 C41 121.7(13) . . ? C45 C46 H46A 119.2 . . ? C41 C46 H46A 119.2 . . ? O2 C47 H47A 109.5 . . ? O2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N3 C48 C49 125.8(11) . . ? N3 C48 H48A 117.1 . . ? C49 C48 H48A 117.1 . . ? C48 C49 N4 117.2(11) . . ? C48 C49 C50 133.1(12) . . ? N4 C49 C50 109.7(10) . . ? C49 C50 C51 105.3(11) . . ? C49 C50 H50A 127.3 . . ? C51 C50 H50A 127.3 . . ? C52 C51 C50 107.6(10) . . ? C52 C51 H51A 126.2 . . ? C50 C51 H51A 126.2 . . ? C51 C52 N4 112.4(10) . . ? C51 C52 H52A 123.8 . . ? N4 C52 H52A 123.8 . . ? C58 C53 C54 123.1(10) . . ? C58 C53 C63 121.6(10) . . ? C54 C53 C63 115.3(10) . . ? O3 C54 C55 126.6(10) . . ? O3 C54 C53 118.5(9) . . ? C55 C54 C53 114.9(11) . . ? C56 C55 C54 122.2(10) . . ? C56 C55 H55A 118.9 . . ? C54 C55 H55A 118.9 . . ? C57 C56 C55 120.4(10) . . ? C57 C56 H56A 119.8 . . ? C55 C56 H56A 119.8 . . ? C56 C57 C62 121.3(11) . . ? C56 C57 C58 121.2(11) . . ? C62 C57 C58 117.4(10) . . ? C53 C58 C59 122.2(10) . . ? C53 C58 C57 118.1(11) . . ? C59 C58 C57 119.6(11) . . ? C60 C59 C58 118.7(11) . . ? C60 C59 H59A 120.6 . . ? C58 C59 H59A 120.6 . . ? C59 C60 C61 123.8(12) . . ? C59 C60 H60A 118.1 . . ? C61 C60 H60A 118.1 . . ? C62 C61 C60 118.4(12) . . ? C62 C61 H61A 120.8 . . ? C60 C61 H61A 120.8 . . ? C61 C62 C57 121.6(11) . . ? C61 C62 H62A 119.2 . . ? C57 C62 H62A 119.2 . . ? C68 C63 C64 121.3(9) . . ? C68 C63 C53 116.8(9) . . ? C64 C63 C53 121.9(10) . . ? C63 C64 N5 126.5(9) . . ? C63 C64 C65 115.3(11) . . ? N5 C64 C65 118.2(9) . . ? C66 C65 C64 122.3(11) . . ? C66 C65 H65A 118.8 . . ? C64 C65 H65A 118.8 . . ? C65 C66 C67 124.6(11) . . ? C65 C66 H66A 117.7 . . ? C67 C66 H66A 117.7 . . ? C72 C67 C66 123.6(11) . . ? C72 C67 C68 121.9(10) . . ? C66 C67 C68 114.4(12) . . ? C63 C68 C69 121.9(9) . . ? C63 C68 C67 121.9(10) . . ? C69 C68 C67 116.2(10) . . ? C70 C69 C68 121.1(10) . . ? C70 C69 H69A 119.4 . . ? C68 C69 H69A 119.4 . . ? C69 C70 C71 120.5(12) . . ? C69 C70 H70A 119.8 . . ? C71 C70 H70A 119.8 . . ? C72 C71 C70 120.3(12) . . ? C72 C71 H71A 119.8 . . ? C70 C71 H71A 119.8 . . ? C71 C72 C67 119.7(11) . . ? C71 C72 H72A 120.2 . . ? C67 C72 H72A 120.2 . . ? O3 C73 H73A 109.5 . . ? O3 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? O3 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N5 C74 C75 122.2(12) . . ? N5 C74 H74A 118.9 . . ? C75 C74 H74A 118.9 . . ? C74 C75 N6 119.3(11) . . ? C74 C75 C76 133.8(13) . . ? N6 C75 C76 106.8(12) . . ? C77 C76 C75 109.5(13) . . ? C77 C76 H76A 125.3 . . ? C75 C76 H76A 125.3 . . ? C76 C77 C78 104.1(11) . . ? C76 C77 H77A 127.9 . . ? C78 C77 H77A 127.9 . . ? N6 C78 C77 113.7(10) . . ? N6 C78 H78A 123.2 . . ? C77 C78 H78A 123.2 . . ? C80 C79 H79A 109.5 . . ? C80 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C80 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C81 C80 C85 120.0 . . ? C81 C80 C79 119.3(14) . . ? C85 C80 C79 120.6(14) . . ? C80 C81 C82 120.0 . . ? C80 C81 H81 120.0 . . ? C82 C81 H81 120.0 . . ? C83 C82 C81 120.0 . . ? C83 C82 H82 120.0 . . ? C81 C82 H82 120.0 . . ? C84 C83 C82 120.0 . . ? C84 C83 H83 120.0 . . ? C82 C83 H83 120.0 . . ? C83 C84 C85 120.0 . . ? C83 C84 H84 120.0 . . ? C85 C84 H84 120.0 . . ? C84 C85 C80 120.0 . . ? C84 C85 H85 120.0 . . ? C80 C85 H85 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Y1 N1 C22 171.6(8) . . . . ? N6 Y1 N1 C22 -122.1(9) . . . . ? N2 Y1 N1 C22 7.7(8) . . . . ? N5 Y1 N1 C22 -60.6(9) . . . . ? O1 Y1 N1 C22 153.7(9) . . . . ? N3 Y1 N1 C22 81.3(9) . . . . ? N4 Y1 N1 C12 -23.1(12) . . . . ? N6 Y1 N1 C12 43.2(8) . . . . ? N2 Y1 N1 C12 172.9(9) . . . . ? N5 Y1 N1 C12 104.7(8) . . . . ? O1 Y1 N1 C12 -41.0(8) . . . . ? N3 Y1 N1 C12 -113.5(8) . . . . ? N4 Y1 N2 C26 10.2(14) . . . . ? N6 Y1 N2 C26 -115.3(11) . . . . ? N5 Y1 N2 C26 -56.3(11) . . . . ? N1 Y1 N2 C26 178.2(12) . . . . ? O1 Y1 N2 C26 132.5(10) . . . . ? N3 Y1 N2 C26 59.4(11) . . . . ? N4 Y1 N2 C23 -173.8(6) . . . . ? N6 Y1 N2 C23 60.8(8) . . . . ? N5 Y1 N2 C23 119.8(7) . . . . ? N1 Y1 N2 C23 -5.7(6) . . . . ? O1 Y1 N2 C23 -51.4(8) . . . . ? N3 Y1 N2 C23 -124.5(7) . . . . ? N4 Y1 N3 C48 -10.9(8) . . . . ? N6 Y1 N3 C48 12.4(11) . . . . ? N2 Y1 N3 C48 -158.4(8) . . . . ? N5 Y1 N3 C48 -79.2(8) . . . . ? N1 Y1 N3 C48 137.0(8) . . . . ? O1 Y1 N3 C48 68.4(8) . . . . ? N4 Y1 N3 C38 -176.3(10) . . . . ? N6 Y1 N3 C38 -153.0(8) . . . . ? N2 Y1 N3 C38 36.2(9) . . . . ? N5 Y1 N3 C38 115.4(9) . . . . ? N1 Y1 N3 C38 -28.4(10) . . . . ? O1 Y1 N3 C38 -97.0(9) . . . . ? N6 Y1 N4 C52 7.6(10) . . . . ? N2 Y1 N4 C52 -129.4(10) . . . . ? N5 Y1 N4 C52 -62.3(10) . . . . ? N1 Y1 N4 C52 73.6(12) . . . . ? O1 Y1 N4 C52 91.3(10) . . . . ? N3 Y1 N4 C52 176.6(11) . . . . ? N6 Y1 N4 C49 -157.5(8) . . . . ? N2 Y1 N4 C49 65.5(9) . . . . ? N5 Y1 N4 C49 132.7(8) . . . . ? N1 Y1 N4 C49 -91.5(9) . . . . ? O1 Y1 N4 C49 -73.8(7) . . . . ? N3 Y1 N4 C49 11.6(7) . . . . ? N4 Y1 N5 C74 77.5(8) . . . . ? N6 Y1 N5 C74 -10.2(8) . . . . ? N2 Y1 N5 C74 -140.5(8) . . . . ? N1 Y1 N5 C74 -79.1(9) . . . . ? O1 Y1 N5 C74 27.8(10) . . . . ? N3 Y1 N5 C74 139.0(7) . . . . ? N4 Y1 N5 C64 -92.9(9) . . . . ? N6 Y1 N5 C64 179.3(10) . . . . ? N2 Y1 N5 C64 49.0(9) . . . . ? N1 Y1 N5 C64 110.5(9) . . . . ? O1 Y1 N5 C64 -142.6(8) . . . . ? N3 Y1 N5 C64 -31.4(10) . . . . ? N4 Y1 N6 C78 87.7(11) . . . . ? N2 Y1 N6 C78 -125.1(11) . . . . ? N5 Y1 N6 C78 169.6(12) . . . . ? N1 Y1 N6 C78 -65.2(11) . . . . ? O1 Y1 N6 C78 10.3(11) . . . . ? N3 Y1 N6 C78 65.9(14) . . . . ? N4 Y1 N6 C75 -70.6(8) . . . . ? N2 Y1 N6 C75 76.6(9) . . . . ? N5 Y1 N6 C75 11.3(7) . . . . ? N1 Y1 N6 C75 136.6(8) . . . . ? O1 Y1 N6 C75 -148.0(8) . . . . ? N3 Y1 N6 C75 -92.4(9) . . . . ? N4 Y1 O1 C2 133.4(8) . . . . ? N6 Y1 O1 C2 -140.5(8) . . . . ? N2 Y1 O1 C2 -11.5(9) . . . . ? N5 Y1 O1 C2 -176.0(8) . . . . ? N1 Y1 O1 C2 -55.6(8) . . . . ? N3 Y1 O1 C2 63.1(8) . . . . ? N4 Y1 O1 C21 -30.0(9) . . . . ? N6 Y1 O1 C21 56.1(9) . . . . ? N2 Y1 O1 C21 -174.9(9) . . . . ? N5 Y1 O1 C21 20.6(11) . . . . ? N1 Y1 O1 C21 141.0(9) . . . . ? N3 Y1 O1 C21 -100.3(9) . . . . ? C6 C1 C2 C3 3.2(17) . . . . ? C11 C1 C2 C3 179.7(12) . . . . ? C6 C1 C2 O1 -171.8(9) . . . . ? C11 C1 C2 O1 4.7(16) . . . . ? C21 O1 C2 C1 -109.5(12) . . . . ? Y1 O1 C2 C1 84.3(11) . . . . ? C21 O1 C2 C3 75.4(14) . . . . ? Y1 O1 C2 C3 -90.8(12) . . . . ? C1 C2 C3 C4 3(2) . . . . ? O1 C2 C3 C4 178.0(11) . . . . ? C2 C3 C4 C5 -7(2) . . . . ? C3 C4 C5 C10 -175.2(13) . . . . ? C3 C4 C5 C6 4(2) . . . . ? C4 C5 C6 C7 177.4(12) . . . . ? C10 C5 C6 C7 -3.7(19) . . . . ? C4 C5 C6 C1 2.4(17) . . . . ? C10 C5 C6 C1 -178.7(11) . . . . ? C2 C1 C6 C5 -5.8(16) . . . . ? C11 C1 C6 C5 177.7(11) . . . . ? C2 C1 C6 C7 179.6(12) . . . . ? C11 C1 C6 C7 3.1(17) . . . . ? C5 C6 C7 C8 6.6(19) . . . . ? C1 C6 C7 C8 -178.9(11) . . . . ? C6 C7 C8 C9 -5(2) . . . . ? C7 C8 C9 C10 0(2) . . . . ? C8 C9 C10 C5 3(2) . . . . ? C4 C5 C10 C9 178.0(13) . . . . ? C6 C5 C10 C9 -1(2) . . . . ? C2 C1 C11 C12 -72.6(16) . . . . ? C6 C1 C11 C12 103.9(14) . . . . ? C2 C1 C11 C16 112.3(12) . . . . ? C6 C1 C11 C16 -71.2(14) . . . . ? C16 C11 C12 C13 -2.3(19) . . . . ? C1 C11 C12 C13 -177.1(12) . . . . ? C16 C11 C12 N1 -177.9(11) . . . . ? C1 C11 C12 N1 7.3(18) . . . . ? C22 N1 C12 C11 -122.1(13) . . . . ? Y1 N1 C12 C11 73.7(12) . . . . ? C22 N1 C12 C13 62.0(15) . . . . ? Y1 N1 C12 C13 -102.2(10) . . . . ? C11 C12 C13 C14 2.8(18) . . . . ? N1 C12 C13 C14 178.4(10) . . . . ? C12 C13 C14 C15 -2(2) . . . . ? C13 C14 C15 C20 -176.9(14) . . . . ? C13 C14 C15 C16 1(2) . . . . ? C12 C11 C16 C17 177.2(13) . . . . ? C1 C11 C16 C17 -7(2) . . . . ? C12 C11 C16 C15 0.8(18) . . . . ? C1 C11 C16 C15 176.1(11) . . . . ? C14 C15 C16 C17 -177.0(13) . . . . ? C20 C15 C16 C17 0.7(19) . . . . ? C14 C15 C16 C11 -0.1(19) . . . . ? C20 C15 C16 C11 177.6(13) . . . . ? C11 C16 C17 C18 179.7(15) . . . . ? C15 C16 C17 C18 -4(2) . . . . ? C16 C17 C18 C19 6(3) . . . . ? C17 C18 C19 C20 -6(2) . . . . ? C14 C15 C20 C19 176.8(14) . . . . ? C16 C15 C20 C19 -1(2) . . . . ? C18 C19 C20 C15 3(2) . . . . ? C12 N1 C22 C23 -174.5(10) . . . . ? Y1 N1 C22 C23 -8.7(15) . . . . ? N1 C22 C23 C24 -172.6(14) . . . . ? N1 C22 C23 N2 3.2(18) . . . . ? C26 N2 C23 C22 -178.3(10) . . . . ? Y1 N2 C23 C22 4.5(12) . . . . ? C26 N2 C23 C24 -1.3(12) . . . . ? Y1 N2 C23 C24 -178.6(8) . . . . ? C22 C23 C24 C25 178.2(13) . . . . ? N2 C23 C24 C25 1.9(14) . . . . ? C23 C24 C25 C26 -1.7(15) . . . . ? C23 N2 C26 C25 0.3(13) . . . . ? Y1 N2 C26 C25 176.4(9) . . . . ? C24 C25 C26 N2 0.8(14) . . . . ? C47 O2 C28 C29 -7.4(15) . . . . ? C47 O2 C28 C27 173.0(9) . . . . ? C32 C27 C28 C29 -4.4(15) . . . . ? C37 C27 C28 C29 -176.4(10) . . . . ? C32 C27 C28 O2 175.2(9) . . . . ? C37 C27 C28 O2 3.2(14) . . . . ? O2 C28 C29 C30 -175.5(10) . . . . ? C27 C28 C29 C30 4.1(16) . . . . ? C28 C29 C30 C31 -2.6(15) . . . . ? C29 C30 C31 C32 1.6(15) . . . . ? C29 C30 C31 C36 176.6(10) . . . . ? C36 C31 C32 C33 3.6(15) . . . . ? C30 C31 C32 C33 178.8(9) . . . . ? C36 C31 C32 C27 -177.3(9) . . . . ? C30 C31 C32 C27 -2.1(14) . . . . ? C28 C27 C32 C33 -177.5(9) . . . . ? C37 C27 C32 C33 -5.1(14) . . . . ? C28 C27 C32 C31 3.3(14) . . . . ? C37 C27 C32 C31 175.8(9) . . . . ? C31 C32 C33 C34 -4.1(16) . . . . ? C27 C32 C33 C34 176.8(9) . . . . ? C32 C33 C34 C35 2.6(15) . . . . ? C33 C34 C35 C36 -0.9(15) . . . . ? C34 C35 C36 C31 0.5(17) . . . . ? C32 C31 C36 C35 -1.8(16) . . . . ? C30 C31 C36 C35 -176.9(10) . . . . ? C28 C27 C37 C38 -98.5(13) . . . . ? C32 C27 C37 C38 89.7(13) . . . . ? C28 C27 C37 C42 88.5(13) . . . . ? C32 C27 C37 C42 -83.3(13) . . . . ? C42 C37 C38 C39 8.1(17) . . . . ? C27 C37 C38 C39 -164.7(10) . . . . ? C42 C37 C38 N3 -173.0(11) . . . . ? C27 C37 C38 N3 14.2(18) . . . . ? C48 N3 C38 C39 -136.2(11) . . . . ? Y1 N3 C38 C39 28.4(15) . . . . ? C48 N3 C38 C37 45.0(16) . . . . ? Y1 N3 C38 C37 -150.5(9) . . . . ? C37 C38 C39 C40 -5.9(18) . . . . ? N3 C38 C39 C40 175.2(12) . . . . ? C38 C39 C40 C41 -2(2) . . . . ? C39 C40 C41 C46 -179.5(13) . . . . ? C39 C40 C41 C42 8(2) . . . . ? C40 C41 C42 C43 176.1(13) . . . . ? C46 C41 C42 C43 2.6(19) . . . . ? C40 C41 C42 C37 -5(2) . . . . ? C46 C41 C42 C37 -178.5(12) . . . . ? C38 C37 C42 C41 -2.9(18) . . . . ? C27 C37 C42 C41 170.3(12) . . . . ? C38 C37 C42 C43 176.0(12) . . . . ? C27 C37 C42 C43 -10.9(18) . . . . ? C41 C42 C43 C44 -3.2(19) . . . . ? C37 C42 C43 C44 177.9(12) . . . . ? C42 C43 C44 C45 1.3(19) . . . . ? C43 C44 C45 C46 1(2) . . . . ? C44 C45 C46 C41 -2(2) . . . . ? C40 C41 C46 C45 -173.3(15) . . . . ? C42 C41 C46 C45 0(2) . . . . ? C38 N3 C48 C49 177.0(11) . . . . ? Y1 N3 C48 C49 9.6(15) . . . . ? N3 C48 C49 N4 0.9(19) . . . . ? N3 C48 C49 C50 177.9(14) . . . . ? C52 N4 C49 C48 178.2(10) . . . . ? Y1 N4 C49 C48 -12.1(13) . . . . ? C52 N4 C49 C50 0.5(13) . . . . ? Y1 N4 C49 C50 170.3(8) . . . . ? C48 C49 C50 C51 -177.5(13) . . . . ? N4 C49 C50 C51 -0.4(14) . . . . ? C49 C50 C51 C52 0.1(14) . . . . ? C50 C51 C52 N4 0.2(14) . . . . ? C49 N4 C52 C51 -0.4(12) . . . . ? Y1 N4 C52 C51 -166.5(8) . . . . ? C73 O3 C54 C55 -21.7(15) . . . . ? C73 O3 C54 C53 160.5(9) . . . . ? C58 C53 C54 O3 -179.2(11) . . . . ? C63 C53 C54 O3 2.6(14) . . . . ? C58 C53 C54 C55 2.8(16) . . . . ? C63 C53 C54 C55 -175.5(9) . . . . ? O3 C54 C55 C56 -178.7(11) . . . . ? C53 C54 C55 C56 -0.9(15) . . . . ? C54 C55 C56 C57 0.2(18) . . . . ? C55 C56 C57 C62 -177.2(12) . . . . ? C55 C56 C57 C58 -1.2(19) . . . . ? C54 C53 C58 C59 175.5(11) . . . . ? C63 C53 C58 C59 -6(2) . . . . ? C54 C53 C58 C57 -3.8(19) . . . . ? C63 C53 C58 C57 174.3(11) . . . . ? C56 C57 C58 C53 3(2) . . . . ? C62 C57 C58 C53 179.1(13) . . . . ? C56 C57 C58 C59 -176.4(13) . . . . ? C62 C57 C58 C59 0(2) . . . . ? C53 C58 C59 C60 175.9(13) . . . . ? C57 C58 C59 C60 -5(2) . . . . ? C58 C59 C60 C61 9(2) . . . . ? C59 C60 C61 C62 -8(2) . . . . ? C60 C61 C62 C57 2(2) . . . . ? C56 C57 C62 C61 177.6(13) . . . . ? C58 C57 C62 C61 1(2) . . . . ? C58 C53 C63 C68 -89.6(14) . . . . ? C54 C53 C63 C68 88.7(12) . . . . ? C58 C53 C63 C64 89.3(14) . . . . ? C54 C53 C63 C64 -92.5(12) . . . . ? C68 C63 C64 N5 178.6(10) . . . . ? C53 C63 C64 N5 -0.2(16) . . . . ? C68 C63 C64 C65 1.7(15) . . . . ? C53 C63 C64 C65 -177.1(10) . . . . ? C74 N5 C64 C63 49.5(15) . . . . ? Y1 N5 C64 C63 -140.3(9) . . . . ? C74 N5 C64 C65 -133.7(10) . . . . ? Y1 N5 C64 C65 36.5(13) . . . . ? C63 C64 C65 C66 -4.0(15) . . . . ? N5 C64 C65 C66 178.8(11) . . . . ? C64 C65 C66 C67 5.1(18) . . . . ? C65 C66 C67 C72 176.2(12) . . . . ? C65 C66 C67 C68 -3.5(16) . . . . ? C64 C63 C68 C69 -178.6(10) . . . . ? C53 C63 C68 C69 0.2(15) . . . . ? C64 C63 C68 C67 -0.5(16) . . . . ? C53 C63 C68 C67 178.4(9) . . . . ? C72 C67 C68 C63 -178.6(10) . . . . ? C66 C67 C68 C63 1.1(14) . . . . ? C72 C67 C68 C69 -0.4(15) . . . . ? C66 C67 C68 C69 179.3(10) . . . . ? C63 C68 C69 C70 177.1(11) . . . . ? C67 C68 C69 C70 -1.1(16) . . . . ? C68 C69 C70 C71 4.3(17) . . . . ? C69 C70 C71 C72 -6.2(17) . . . . ? C70 C71 C72 C67 4.6(18) . . . . ? C66 C67 C72 C71 178.9(11) . . . . ? C68 C67 C72 C71 -1.4(17) . . . . ? C64 N5 C74 C75 179.6(11) . . . . ? Y1 N5 C74 C75 8.0(14) . . . . ? N5 C74 C75 N6 3.1(18) . . . . ? N5 C74 C75 C76 -179.1(13) . . . . ? C78 N6 C75 C74 -177.8(11) . . . . ? Y1 N6 C75 C74 -12.5(13) . . . . ? C78 N6 C75 C76 3.9(13) . . . . ? Y1 N6 C75 C76 169.1(8) . . . . ? C74 C75 C76 C77 179.5(14) . . . . ? N6 C75 C76 C77 -2.5(15) . . . . ? C75 C76 C77 C78 0.1(15) . . . . ? C75 N6 C78 C77 -4.1(13) . . . . ? Y1 N6 C78 C77 -163.4(9) . . . . ? C76 C77 C78 N6 2.5(15) . . . . ? C85 C80 C81 C82 0.0 . . . . ? C79 C80 C81 C82 176.8(16) . . . . ? C80 C81 C82 C83 0.0 . . . . ? C81 C82 C83 C84 0.0 . . . . ? C82 C83 C84 C85 0.0 . . . . ? C83 C84 C85 C80 0.0 . . . . ? C81 C80 C85 C84 0.0 . . . . ? C79 C80 C85 C84 -176.7(16) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.022 0.250 0.000 698.5 85.0 2 -0.066 0.750 0.500 698.6 85.8 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.824 _refine_diff_density_min -1.142 _refine_diff_density_rms 0.126 # Attachment 'compound_6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 687846' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H73 N6 O3 Yb' _chemical_formula_sum 'C92 H73 N6 O3 Yb' _chemical_formula_weight 1483.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 13.6374(12) _cell_length_b 15.0903(14) _cell_length_c 36.529(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7517.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 14684 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3044 _exptl_absorpt_coefficient_mu 1.299 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8390 _exptl_absorpt_correction_T_max 0.8810 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61210 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.99 _reflns_number_total 14721 _reflns_number_gt 13841 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+6.7053P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(10) _refine_ls_number_reflns 14721 _refine_ls_number_parameters 923 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1544 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.203 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.72967(2) 0.56081(2) 0.616925(8) 0.03063(9) Uani 1 1 d . . . N1 N 0.6747(5) 0.5130(5) 0.67732(16) 0.0354(15) Uani 1 1 d . . . N2 N 0.7701(5) 0.6698(4) 0.66021(15) 0.0324(13) Uani 1 1 d . . . N3 N 0.9111(4) 0.5591(5) 0.60728(13) 0.0314(13) Uani 1 1 d . . . N4 N 0.7647(5) 0.5276(4) 0.55562(15) 0.0364(14) Uani 1 1 d . . . N5 N 0.6486(4) 0.6847(4) 0.58777(16) 0.0313(13) Uani 1 1 d . . . N6 N 0.5709(5) 0.5172(5) 0.60067(18) 0.0410(16) Uani 1 1 d . . . O1 O 0.7560(4) 0.3997(3) 0.61886(13) 0.0366(11) Uani 1 1 d . . . O2 O 1.1599(4) 0.5273(4) 0.55775(14) 0.0400(13) Uani 1 1 d . . . O3 O 0.4822(4) 0.8446(4) 0.53417(14) 0.0394(13) Uani 1 1 d . . . C1 C 0.7712(7) 0.3450(5) 0.68014(19) 0.0358(16) Uani 1 1 d . . . C2 C 0.8147(6) 0.3632(4) 0.6467(2) 0.0319(16) Uani 1 1 d . . . C3 C 0.9156(6) 0.3498(5) 0.6408(2) 0.042(2) Uani 1 1 d . . . H3 H 0.9433 0.3613 0.6174 0.051 Uiso 1 1 calc R . . C4 C 0.9741(6) 0.3201(6) 0.6689(2) 0.043(2) Uani 1 1 d . . . H4 H 1.0419 0.3104 0.6646 0.052 Uiso 1 1 calc R . . C5 C 0.9344(6) 0.3037(6) 0.7041(2) 0.042(2) Uani 1 1 d . . . C6 C 0.8325(6) 0.3160(6) 0.71021(19) 0.0363(17) Uani 1 1 d . . . C7 C 0.7951(6) 0.3011(6) 0.7457(2) 0.043(2) Uani 1 1 d . . . H7 H 0.7271 0.3098 0.7502 0.052 Uiso 1 1 calc R . . C8 C 0.8531(7) 0.2750(6) 0.7735(2) 0.050(2) Uani 1 1 d . . . H8 H 0.8251 0.2652 0.7970 0.060 Uiso 1 1 calc R . . C9 C 0.9554(7) 0.2616(6) 0.7684(2) 0.048(2) Uani 1 1 d . . . H9 H 0.9956 0.2421 0.7880 0.057 Uiso 1 1 calc R . . C10 C 0.9948(7) 0.2774(6) 0.7343(3) 0.048(2) Uani 1 1 d . . . H10 H 1.0634 0.2708 0.7308 0.058 Uiso 1 1 calc R . . C11 C 0.6621(6) 0.3545(6) 0.6853(2) 0.0391(19) Uani 1 1 d . . . C12 C 0.6187(5) 0.4372(6) 0.68554(19) 0.0385(17) Uani 1 1 d . . . C13 C 0.5168(6) 0.4467(7) 0.6925(2) 0.047(2) Uani 1 1 d . . . H13 H 0.4875 0.5038 0.6929 0.056 Uiso 1 1 calc R . . C14 C 0.4606(7) 0.3718(7) 0.6988(3) 0.053(2) Uani 1 1 d . . . H14 H 0.3929 0.3785 0.7042 0.064 Uiso 1 1 calc R . . C15 C 0.5008(8) 0.2864(7) 0.6973(3) 0.059(3) Uani 1 1 d . . . C16 C 0.6017(7) 0.2763(6) 0.6903(2) 0.045(2) Uani 1 1 d . . . C17 C 0.6419(8) 0.1873(7) 0.6879(2) 0.056(2) Uani 1 1 d . . . H17 H 0.7101 0.1801 0.6834 0.067 Uiso 1 1 calc R . . C18 C 0.5848(9) 0.1139(7) 0.6920(3) 0.070(3) Uani 1 1 d . . . H18 H 0.6129 0.0565 0.6899 0.083 Uiso 1 1 calc R . . C19 C 0.4837(11) 0.1234(8) 0.6992(4) 0.087(4) Uani 1 1 d . . . H19 H 0.4435 0.0725 0.7022 0.105 Uiso 1 1 calc R . . C20 C 0.4423(9) 0.2094(10) 0.7021(3) 0.082(4) Uani 1 1 d . . . H20 H 0.3743 0.2156 0.7072 0.098 Uiso 1 1 calc R . . C21 C 0.7381(9) 0.3357(5) 0.5893(2) 0.055(2) Uani 1 1 d . . . H21A H 0.8006 0.3191 0.5781 0.083 Uiso 1 1 calc R . . H21B H 0.6954 0.3626 0.5708 0.083 Uiso 1 1 calc R . . H21C H 0.7064 0.2828 0.5994 0.083 Uiso 1 1 calc R . . C22 C 0.6850(6) 0.5742(6) 0.7025(2) 0.0412(19) Uani 1 1 d . . . H22 H 0.6579 0.5646 0.7261 0.049 Uiso 1 1 calc R . . C23 C 0.7348(7) 0.6530(5) 0.69543(18) 0.0356(16) Uani 1 1 d . . . C24 C 0.7607(8) 0.7242(7) 0.7186(2) 0.059(3) Uani 1 1 d . . . H24 H 0.7460 0.7296 0.7439 0.071 Uiso 1 1 calc R . . C25 C 0.8117(7) 0.7849(7) 0.6973(2) 0.050(2) Uani 1 1 d . . . H25 H 0.8391 0.8396 0.7051 0.060 Uiso 1 1 calc R . . C26 C 0.8144(6) 0.7487(6) 0.6620(2) 0.043(2) Uani 1 1 d . . . H26 H 0.8444 0.7770 0.6416 0.052 Uiso 1 1 calc R . . C27 C 1.1000(5) 0.6551(5) 0.58746(19) 0.0326(16) Uani 1 1 d . . . C28 C 1.1415(6) 0.6167(6) 0.5560(2) 0.0342(17) Uani 1 1 d . . . C29 C 1.1624(5) 0.6693(6) 0.52471(17) 0.0346(18) Uani 1 1 d . . . H29 H 1.1884 0.6418 0.5034 0.042 Uiso 1 1 calc R . . C30 C 1.1459(5) 0.7576(5) 0.5247(2) 0.0340(17) Uani 1 1 d . . . H30 H 1.1595 0.7912 0.5033 0.041 Uiso 1 1 calc R . . C31 C 1.1080(5) 0.8010(6) 0.5566(2) 0.0357(17) Uani 1 1 d . . . C32 C 1.0847(5) 0.7488(5) 0.58770(18) 0.0284(15) Uani 1 1 d . . . C33 C 1.0508(5) 0.7934(5) 0.6192(2) 0.0337(15) Uani 1 1 d . . . H33 H 1.0346 0.7598 0.6404 0.040 Uiso 1 1 calc R . . C34 C 1.0405(5) 0.8849(5) 0.6203(2) 0.0372(17) Uani 1 1 d . . . H34 H 1.0176 0.9134 0.6418 0.045 Uiso 1 1 calc R . . C35 C 1.0646(5) 0.9357(6) 0.5885(2) 0.0407(17) Uani 1 1 d . . . H35 H 1.0588 0.9984 0.5891 0.049 Uiso 1 1 calc R . . C36 C 1.0957(6) 0.8952(6) 0.5574(2) 0.0379(18) Uani 1 1 d . . . H36 H 1.1093 0.9294 0.5362 0.045 Uiso 1 1 calc R . . C37 C 1.0826(5) 0.6049(5) 0.62205(19) 0.0299(15) Uani 1 1 d . . . C38 C 0.9913(5) 0.5700(5) 0.63191(17) 0.0305(15) Uani 1 1 d . . . C39 C 0.9748(6) 0.5448(5) 0.66875(19) 0.0343(18) Uani 1 1 d . . . H39 H 0.9112 0.5267 0.6763 0.041 Uiso 1 1 calc R . . C40 C 1.0506(6) 0.5462(7) 0.6938(2) 0.048(2) Uani 1 1 d . . . H40 H 1.0380 0.5288 0.7184 0.057 Uiso 1 1 calc R . . C41 C 1.1456(5) 0.5726(6) 0.68404(19) 0.0363(17) Uani 1 1 d . . . C42 C 1.1624(5) 0.6051(5) 0.6483(2) 0.0343(17) Uani 1 1 d . . . C43 C 1.2567(5) 0.6356(5) 0.6396(2) 0.0354(17) Uani 1 1 d . . . H43 H 1.2693 0.6570 0.6156 0.042 Uiso 1 1 calc R . . C44 C 1.3316(6) 0.6354(6) 0.6648(2) 0.045(2) Uani 1 1 d . . . H44 H 1.3948 0.6564 0.6582 0.055 Uiso 1 1 calc R . . C45 C 1.3145(7) 0.6040(7) 0.7005(2) 0.052(2) Uani 1 1 d . . . H45 H 1.3658 0.6055 0.7181 0.063 Uiso 1 1 calc R . . C46 C 1.2245(7) 0.5712(6) 0.70994(19) 0.047(2) Uani 1 1 d . . . H46 H 1.2143 0.5474 0.7337 0.057 Uiso 1 1 calc R . . C47 C 1.1927(6) 0.4825(6) 0.5250(2) 0.044(2) Uani 1 1 d . . . H47A H 1.1424 0.4878 0.5059 0.065 Uiso 1 1 calc R . . H47B H 1.2041 0.4198 0.5304 0.065 Uiso 1 1 calc R . . H47C H 1.2538 0.5096 0.5163 0.065 Uiso 1 1 calc R . . C48 C 0.9332(6) 0.5248(5) 0.5758(2) 0.0312(16) Uani 1 1 d . . . H48 H 0.9999 0.5115 0.5707 0.037 Uiso 1 1 calc R . . C49 C 0.8617(6) 0.5062(6) 0.5487(2) 0.0360(17) Uani 1 1 d . . . C50 C 0.8722(7) 0.4686(6) 0.5139(2) 0.047(2) Uani 1 1 d . . . H50 H 0.9313 0.4495 0.5026 0.056 Uiso 1 1 calc R . . C51 C 0.7777(8) 0.4651(6) 0.4992(2) 0.054(2) Uani 1 1 d . . . H51 H 0.7594 0.4423 0.4759 0.065 Uiso 1 1 calc R . . C52 C 0.7147(7) 0.5023(6) 0.5258(2) 0.047(2) Uani 1 1 d . . . H52 H 0.6458 0.5085 0.5230 0.056 Uiso 1 1 calc R . . C53 C 0.5271(5) 0.8489(6) 0.5963(2) 0.0353(18) Uani 1 1 d . . . C54 C 0.4522(6) 0.8515(6) 0.5704(2) 0.0393(19) Uani 1 1 d . . . C55 C 0.3543(6) 0.8597(6) 0.5800(2) 0.045(2) Uani 1 1 d . . . H55 H 0.3051 0.8593 0.5616 0.054 Uiso 1 1 calc R . . C56 C 0.3280(6) 0.8686(6) 0.6164(2) 0.0452(19) Uani 1 1 d . . . H56 H 0.2610 0.8755 0.6228 0.054 Uiso 1 1 calc R . . C57 C 0.4005(6) 0.8674(6) 0.6440(2) 0.0387(18) Uani 1 1 d . . . C58 C 0.5020(6) 0.8563(5) 0.6333(2) 0.0322(16) Uani 1 1 d . . . C59 C 0.5734(6) 0.8545(6) 0.6617(2) 0.0415(19) Uani 1 1 d . . . H59 H 0.6409 0.8476 0.6558 0.050 Uiso 1 1 calc R . . C60 C 0.5442(7) 0.8627(6) 0.6980(2) 0.049(2) Uani 1 1 d . . . H60 H 0.5929 0.8617 0.7166 0.059 Uiso 1 1 calc R . . C61 C 0.4470(7) 0.8724(7) 0.7081(2) 0.049(2) Uani 1 1 d . . . H61 H 0.4296 0.8760 0.7332 0.059 Uiso 1 1 calc R . . C62 C 0.3758(6) 0.8766(6) 0.6815(2) 0.045(2) Uani 1 1 d . . . H62 H 0.3093 0.8858 0.6884 0.054 Uiso 1 1 calc R . . C63 C 0.6328(5) 0.8480(5) 0.58420(19) 0.0292(15) Uani 1 1 d . . . C64 C 0.6861(6) 0.7711(5) 0.5800(2) 0.0338(17) Uani 1 1 d . . . C65 C 0.7859(6) 0.7760(5) 0.56919(19) 0.0327(18) Uani 1 1 d . . . H65 H 0.8229 0.7228 0.5674 0.039 Uiso 1 1 calc R . . C66 C 0.8301(5) 0.8541(5) 0.5612(2) 0.0347(17) Uani 1 1 d . . . H66 H 0.8964 0.8547 0.5533 0.042 Uiso 1 1 calc R . . C67 C 0.7787(5) 0.9335(5) 0.56474(17) 0.0328(14) Uani 1 1 d . . . C68 C 0.6787(5) 0.9309(5) 0.57673(18) 0.0305(15) Uani 1 1 d . . . C69 C 0.6265(7) 1.0119(6) 0.5802(2) 0.042(2) Uani 1 1 d . . . H69 H 0.5602 1.0113 0.5882 0.051 Uiso 1 1 calc R . . C70 C 0.6715(7) 1.0922(6) 0.5720(3) 0.052(3) Uani 1 1 d . . . H70 H 0.6356 1.1458 0.5745 0.063 Uiso 1 1 calc R . . C71 C 0.7676(9) 1.0949(6) 0.5603(3) 0.055(2) Uani 1 1 d . . . H71 H 0.7974 1.1501 0.5547 0.066 Uiso 1 1 calc R . . C72 C 0.8206(7) 1.0176(6) 0.5568(2) 0.043(2) Uani 1 1 d . . . H72 H 0.8869 1.0205 0.5489 0.052 Uiso 1 1 calc R . . C73 C 0.4112(6) 0.8125(7) 0.5081(2) 0.045(2) Uani 1 1 d . . . H73A H 0.3842 0.7560 0.5167 0.068 Uiso 1 1 calc R . . H73B H 0.4429 0.8039 0.4843 0.068 Uiso 1 1 calc R . . H73C H 0.3581 0.8559 0.5056 0.068 Uiso 1 1 calc R . . C74 C 0.5634(6) 0.6633(5) 0.5729(2) 0.0357(17) Uani 1 1 d . . . H74 H 0.5300 0.7052 0.5580 0.043 Uiso 1 1 calc R . . C75 C 0.5215(6) 0.5791(6) 0.5789(2) 0.0412(19) Uani 1 1 d . . . C76 C 0.4361(7) 0.5437(8) 0.5643(3) 0.068(3) Uani 1 1 d . . . H76 H 0.3913 0.5717 0.5480 0.081 Uiso 1 1 calc R . . C77 C 0.4302(9) 0.4592(7) 0.5784(3) 0.075(4) Uani 1 1 d . . . H77 H 0.3788 0.4180 0.5740 0.090 Uiso 1 1 calc R . . C78 C 0.5128(7) 0.4446(7) 0.6002(3) 0.059(3) Uani 1 1 d . . . H78 H 0.5263 0.3910 0.6129 0.071 Uiso 1 1 calc R . . C79 C 1.1266(11) 0.0354(11) 0.7155(4) 0.110(5) Uani 1 1 d U . . H79A H 1.1278 0.0739 0.7371 0.165 Uiso 1 1 calc R . . H79B H 1.1786 0.0534 0.6985 0.165 Uiso 1 1 calc R . . H79C H 1.1372 -0.0261 0.7230 0.165 Uiso 1 1 calc R . . C80 C 1.0282(12) 0.0434(10) 0.6967(4) 0.096(4) Uani 1 1 d U . . C81 C 1.0336(11) 0.0989(8) 0.6642(3) 0.078(3) Uani 1 1 d U . . H81 H 1.0926 0.1277 0.6572 0.093 Uiso 1 1 calc R . . C82 C 0.9475(14) 0.1076(12) 0.6437(5) 0.119(5) Uani 1 1 d U . . H82 H 0.9484 0.1435 0.6224 0.143 Uiso 1 1 calc R . . C83 C 0.8652(11) 0.0680(10) 0.6530(4) 0.086(4) Uani 1 1 d U . . H83 H 0.8081 0.0781 0.6387 0.104 Uiso 1 1 calc R . . C84 C 0.8598(12) 0.0161(10) 0.6808(4) 0.094(4) Uani 1 1 d U . . H84 H 0.8000 -0.0130 0.6868 0.113 Uiso 1 1 calc R . . C85 C 0.9509(11) 0.0023(9) 0.7041(3) 0.083(4) Uani 1 1 d U . . H85 H 0.9493 -0.0375 0.7242 0.099 Uiso 1 1 calc R . . C86 C 0.843(2) 0.3808(17) 0.3974(7) 0.234(13) Uani 1 1 d DU . . H86A H 0.8551 0.3925 0.4234 0.351 Uiso 1 1 calc R . . H86B H 0.8110 0.4325 0.3863 0.351 Uiso 1 1 calc R . . H86C H 0.9049 0.3690 0.3849 0.351 Uiso 1 1 calc R . . C87 C 0.7770(15) 0.3018(12) 0.3938(6) 0.155(9) Uani 1 1 d DU . . C88 C 0.6971(11) 0.3104(14) 0.4142(4) 0.118(6) Uani 1 1 d . . . H88 H 0.6795 0.3632 0.4268 0.141 Uiso 1 1 calc R . . C89 C 0.6361(11) 0.2240(15) 0.4150(4) 0.120(7) Uani 1 1 d . . . H89 H 0.5777 0.2185 0.4290 0.144 Uiso 1 1 calc R . . C90 C 0.6740(12) 0.1520(11) 0.3930(4) 0.095(5) Uani 1 1 d . . . H90 H 0.6424 0.0960 0.3923 0.114 Uiso 1 1 calc R . . C91 C 0.7524(13) 0.1671(18) 0.3745(4) 0.150(9) Uani 1 1 d . . . H91 H 0.7684 0.1232 0.3568 0.180 Uiso 1 1 calc R . . C92 C 0.8131(16) 0.2336(12) 0.3763(7) 0.145(8) Uani 1 1 d . . . H92 H 0.8771 0.2326 0.3661 0.173 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02849(15) 0.03677(16) 0.02663(13) 0.00195(13) -0.00172(12) -0.00074(14) N1 0.032(4) 0.047(4) 0.028(3) 0.006(3) 0.008(3) 0.010(3) N2 0.024(3) 0.037(3) 0.036(3) -0.013(2) -0.004(3) -0.002(3) N3 0.033(3) 0.041(3) 0.020(2) 0.003(3) 0.002(2) -0.001(3) N4 0.037(3) 0.047(4) 0.026(3) -0.001(2) -0.001(3) -0.003(3) N5 0.030(3) 0.030(3) 0.034(3) 0.004(3) -0.002(2) 0.004(3) N6 0.033(4) 0.049(4) 0.040(3) 0.007(3) -0.001(3) -0.014(3) O1 0.037(3) 0.036(3) 0.037(2) -0.001(2) -0.002(2) 0.002(2) O2 0.033(3) 0.051(4) 0.035(3) -0.004(2) 0.003(2) 0.008(3) O3 0.025(3) 0.064(4) 0.029(3) -0.004(2) -0.005(2) -0.004(3) C1 0.035(4) 0.038(4) 0.034(3) 0.001(3) 0.006(4) -0.003(4) C2 0.036(4) 0.020(3) 0.040(4) 0.005(3) -0.002(3) 0.002(3) C3 0.040(5) 0.036(5) 0.051(5) 0.007(4) 0.016(4) -0.003(4) C4 0.030(4) 0.034(4) 0.065(5) 0.009(4) 0.010(4) 0.010(4) C5 0.045(5) 0.033(5) 0.049(5) 0.011(4) 0.010(4) 0.001(4) C6 0.037(4) 0.043(5) 0.030(4) 0.003(3) 0.003(3) 0.004(4) C7 0.041(5) 0.051(5) 0.037(4) 0.013(3) 0.008(3) -0.006(4) C8 0.060(6) 0.054(6) 0.036(4) 0.015(4) 0.005(4) 0.006(5) C9 0.042(5) 0.054(6) 0.047(5) 0.015(4) -0.006(4) 0.004(4) C10 0.036(5) 0.049(5) 0.059(5) 0.006(4) 0.003(4) 0.002(4) C11 0.040(5) 0.045(5) 0.032(4) 0.006(3) -0.002(3) -0.005(4) C12 0.029(4) 0.052(5) 0.034(3) 0.006(4) -0.001(3) 0.003(4) C13 0.038(4) 0.063(6) 0.039(4) 0.017(4) 0.007(3) 0.011(5) C14 0.032(5) 0.076(7) 0.052(5) 0.009(5) 0.010(4) 0.003(5) C15 0.051(6) 0.066(7) 0.059(6) 0.006(5) 0.011(5) -0.013(5) C16 0.045(5) 0.048(5) 0.042(4) 0.008(4) 0.008(4) 0.000(4) C17 0.071(7) 0.048(6) 0.050(5) 0.003(4) 0.005(5) -0.017(5) C18 0.075(8) 0.050(6) 0.083(8) 0.008(5) 0.031(6) -0.017(6) C19 0.122(12) 0.050(7) 0.089(9) 0.020(6) 0.013(8) -0.030(7) C20 0.057(7) 0.122(12) 0.067(7) -0.008(7) 0.021(6) -0.040(7) C21 0.089(7) 0.031(4) 0.045(4) -0.003(3) -0.005(5) -0.019(5) C22 0.032(4) 0.061(6) 0.031(4) 0.000(4) -0.001(3) 0.014(4) C23 0.037(4) 0.041(4) 0.029(3) -0.006(3) -0.005(3) 0.007(4) C24 0.053(6) 0.084(7) 0.040(4) -0.020(4) -0.008(4) 0.003(5) C25 0.037(4) 0.064(6) 0.048(5) -0.024(4) -0.002(4) -0.006(4) C26 0.028(4) 0.062(6) 0.039(4) -0.010(4) -0.012(3) -0.003(4) C27 0.024(4) 0.045(5) 0.028(3) -0.003(3) 0.003(3) 0.001(3) C28 0.034(4) 0.040(5) 0.028(3) -0.004(3) 0.004(3) -0.001(3) C29 0.033(4) 0.054(5) 0.017(3) -0.004(3) 0.006(3) -0.007(4) C30 0.024(4) 0.046(5) 0.032(4) 0.001(3) -0.001(3) -0.005(3) C31 0.025(4) 0.046(5) 0.036(4) 0.005(3) 0.000(3) -0.001(3) C32 0.020(3) 0.039(4) 0.026(3) -0.004(3) 0.004(3) -0.005(3) C33 0.025(3) 0.048(4) 0.028(3) -0.006(3) -0.001(3) -0.001(3) C34 0.031(4) 0.039(4) 0.041(4) -0.010(4) 0.001(4) -0.004(3) C35 0.033(4) 0.047(5) 0.041(4) 0.005(4) -0.007(3) 0.001(4) C36 0.027(4) 0.048(5) 0.038(4) 0.003(3) 0.008(3) 0.001(4) C37 0.031(4) 0.029(4) 0.030(4) -0.005(3) -0.005(3) 0.001(3) C38 0.031(4) 0.037(4) 0.024(3) 0.001(3) 0.002(3) 0.003(3) C39 0.030(4) 0.045(5) 0.028(3) 0.006(3) -0.001(3) 0.002(4) C40 0.046(5) 0.065(7) 0.033(4) 0.000(4) -0.003(3) -0.004(5) C41 0.031(4) 0.049(5) 0.029(3) -0.001(4) 0.001(3) 0.004(4) C42 0.027(4) 0.043(4) 0.033(4) -0.008(3) 0.000(3) 0.006(3) C43 0.023(4) 0.039(4) 0.044(4) -0.006(3) -0.002(3) 0.007(3) C44 0.026(4) 0.059(6) 0.052(5) -0.003(4) -0.004(4) 0.013(4) C45 0.038(5) 0.080(7) 0.040(4) -0.006(4) -0.015(4) 0.008(5) C46 0.049(5) 0.062(5) 0.031(3) -0.003(4) -0.012(4) 0.014(5) C47 0.032(4) 0.053(5) 0.046(4) -0.016(4) 0.006(4) 0.006(4) C48 0.025(4) 0.031(4) 0.037(4) 0.002(3) 0.002(3) 0.000(3) C49 0.035(4) 0.042(5) 0.031(4) -0.001(3) 0.002(3) -0.001(4) C50 0.053(5) 0.054(6) 0.034(4) -0.017(4) 0.006(4) -0.007(4) C51 0.060(6) 0.072(6) 0.030(4) -0.006(4) -0.001(4) -0.003(5) C52 0.047(6) 0.064(6) 0.029(4) 0.003(3) -0.007(4) -0.004(4) C53 0.023(4) 0.049(5) 0.034(4) -0.003(3) -0.007(3) -0.002(3) C54 0.026(4) 0.052(5) 0.039(4) -0.005(4) 0.004(3) 0.007(4) C55 0.026(4) 0.062(6) 0.046(5) -0.002(4) -0.003(3) 0.007(4) C56 0.028(4) 0.062(5) 0.046(4) -0.001(4) 0.007(4) -0.002(4) C57 0.029(4) 0.044(5) 0.044(4) 0.001(4) 0.003(3) 0.004(3) C58 0.034(4) 0.025(4) 0.037(4) -0.001(3) 0.001(3) -0.001(3) C59 0.035(4) 0.057(6) 0.032(4) -0.005(3) 0.001(3) 0.001(4) C60 0.051(6) 0.062(6) 0.034(4) 0.000(4) -0.007(4) 0.009(5) C61 0.038(5) 0.076(7) 0.033(4) -0.001(4) 0.008(4) -0.002(5) C62 0.034(4) 0.056(6) 0.043(4) 0.001(4) 0.004(4) -0.003(4) C63 0.022(4) 0.034(4) 0.032(4) -0.005(3) 0.000(3) -0.002(3) C64 0.032(4) 0.039(4) 0.030(4) -0.001(3) -0.003(3) 0.002(3) C65 0.028(5) 0.037(4) 0.033(3) 0.001(3) -0.006(3) 0.006(3) C66 0.021(4) 0.048(5) 0.035(4) -0.007(3) 0.001(3) -0.002(3) C67 0.026(3) 0.044(4) 0.028(3) 0.004(3) 0.000(3) -0.004(4) C68 0.029(4) 0.031(4) 0.032(3) -0.006(3) -0.007(3) 0.000(3) C69 0.042(5) 0.041(5) 0.045(5) -0.010(4) -0.002(4) -0.001(4) C70 0.040(5) 0.040(5) 0.076(7) -0.011(4) -0.017(5) 0.012(4) C71 0.059(6) 0.042(5) 0.063(5) -0.006(4) -0.013(5) -0.011(5) C72 0.033(4) 0.050(5) 0.047(5) -0.001(4) -0.012(4) -0.009(4) C73 0.033(4) 0.066(6) 0.036(4) -0.001(4) -0.010(3) -0.003(4) C74 0.028(4) 0.039(5) 0.040(4) 0.000(3) -0.004(3) 0.004(3) C75 0.036(4) 0.040(5) 0.048(4) 0.001(4) -0.008(3) -0.004(4) C76 0.045(6) 0.071(8) 0.087(7) 0.012(6) -0.029(5) -0.015(5) C77 0.071(7) 0.056(7) 0.099(9) 0.014(6) -0.033(6) -0.025(6) C78 0.055(6) 0.051(6) 0.070(6) 0.017(5) -0.012(5) -0.033(5) C79 0.114(8) 0.110(9) 0.107(8) -0.021(7) -0.049(7) 0.030(7) C80 0.114(8) 0.091(8) 0.085(7) -0.049(6) 0.019(6) 0.003(7) C81 0.105(7) 0.061(6) 0.067(6) -0.014(5) -0.019(6) 0.021(6) C82 0.133(9) 0.111(9) 0.113(9) -0.004(7) 0.012(8) 0.008(8) C83 0.096(7) 0.081(7) 0.081(6) -0.005(6) 0.010(6) 0.015(7) C84 0.097(8) 0.100(8) 0.086(7) -0.013(6) 0.001(7) -0.001(7) C85 0.110(8) 0.078(7) 0.061(6) -0.011(5) 0.007(6) 0.007(6) C86 0.244(16) 0.228(16) 0.230(16) -0.005(10) 0.011(10) -0.021(10) C87 0.157(17) 0.097(12) 0.21(2) -0.038(12) 0.116(16) -0.047(12) C88 0.085(11) 0.164(16) 0.103(11) -0.052(11) -0.018(9) 0.000(11) C89 0.065(9) 0.22(2) 0.080(10) 0.001(12) -0.025(8) 0.015(12) C90 0.098(11) 0.101(11) 0.085(10) 0.038(8) -0.037(8) -0.017(9) C91 0.095(14) 0.28(3) 0.076(10) 0.039(13) -0.009(9) -0.039(16) C92 0.134(16) 0.096(12) 0.20(2) -0.021(14) 0.046(17) -0.025(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N6 2.340(7) . ? Yb1 N4 2.344(6) . ? Yb1 N2 2.347(5) . ? Yb1 N5 2.419(6) . ? Yb1 N1 2.439(6) . ? Yb1 O1 2.459(5) . ? Yb1 N3 2.500(6) . ? Yb1 C75 3.172(8) . ? Yb1 C74 3.182(8) . ? Yb1 C49 3.184(8) . ? Yb1 C23 3.188(7) . ? Yb1 C22 3.190(7) . ? N1 C22 1.310(11) . ? N1 C12 1.408(11) . ? N2 C26 1.337(10) . ? N2 C23 1.397(9) . ? N3 C48 1.297(9) . ? N3 C38 1.426(9) . ? N4 C52 1.340(10) . ? N4 C49 1.384(11) . ? N5 C74 1.323(9) . ? N5 C64 1.429(10) . ? N6 C78 1.352(11) . ? N6 C75 1.399(11) . ? O1 C2 1.407(8) . ? O1 C21 1.467(9) . ? O2 C28 1.374(10) . ? O2 C47 1.446(9) . ? O3 C54 1.390(9) . ? O3 C73 1.442(9) . ? C1 C2 1.385(10) . ? C1 C6 1.448(11) . ? C1 C11 1.507(12) . ? C2 C3 1.407(11) . ? C3 C4 1.373(12) . ? C3 H3 0.9500 . ? C4 C5 1.418(11) . ? C4 H4 0.9500 . ? C5 C6 1.420(11) . ? C5 C10 1.434(12) . ? C6 C7 1.413(10) . ? C7 C8 1.345(11) . ? C7 H7 0.9500 . ? C8 C9 1.422(13) . ? C8 H8 0.9500 . ? C9 C10 1.376(12) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.381(12) . ? C11 C16 1.451(12) . ? C12 C13 1.420(10) . ? C13 C14 1.384(14) . ? C13 H13 0.9500 . ? C14 C15 1.402(15) . ? C14 H14 0.9500 . ? C15 C16 1.408(13) . ? C15 C20 1.420(15) . ? C16 C17 1.454(14) . ? C17 C18 1.362(14) . ? C17 H17 0.9500 . ? C18 C19 1.411(18) . ? C18 H18 0.9500 . ? C19 C20 1.419(19) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.394(12) . ? C22 H22 0.9500 . ? C23 C24 1.412(11) . ? C24 C25 1.387(14) . ? C24 H24 0.9500 . ? C25 C26 1.402(11) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.407(10) . ? C27 C32 1.428(11) . ? C27 C37 1.493(10) . ? C28 C29 1.419(10) . ? C29 C30 1.351(11) . ? C29 H29 0.9500 . ? C30 C31 1.435(11) . ? C30 H30 0.9500 . ? C31 C32 1.418(10) . ? C31 C36 1.432(12) . ? C32 C33 1.413(10) . ? C33 C34 1.388(11) . ? C33 H33 0.9500 . ? C34 C35 1.429(11) . ? C34 H34 0.9500 . ? C35 C36 1.356(11) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.399(10) . ? C37 C42 1.449(10) . ? C38 C39 1.417(9) . ? C39 C40 1.381(11) . ? C39 H39 0.9500 . ? C40 C41 1.403(11) . ? C40 H40 0.9500 . ? C41 C42 1.414(10) . ? C41 C46 1.433(10) . ? C42 C43 1.402(11) . ? C43 C44 1.375(11) . ? C43 H43 0.9500 . ? C44 C45 1.405(13) . ? C44 H44 0.9500 . ? C45 C46 1.368(13) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.417(10) . ? C48 H48 0.9500 . ? C49 C50 1.400(10) . ? C50 C51 1.397(13) . ? C50 H50 0.9500 . ? C51 C52 1.415(12) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.393(10) . ? C53 C58 1.400(10) . ? C53 C63 1.507(10) . ? C54 C55 1.386(11) . ? C55 C56 1.383(12) . ? C55 H55 0.9500 . ? C56 C57 1.413(12) . ? C56 H56 0.9500 . ? C57 C62 1.418(11) . ? C57 C58 1.448(11) . ? C58 C59 1.421(11) . ? C59 C60 1.392(11) . ? C59 H59 0.9500 . ? C60 C61 1.383(13) . ? C60 H60 0.9500 . ? C61 C62 1.375(12) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C64 1.378(11) . ? C63 C68 1.425(11) . ? C64 C65 1.420(11) . ? C65 C66 1.355(11) . ? C65 H65 0.9500 . ? C66 C67 1.396(11) . ? C66 H66 0.9500 . ? C67 C72 1.420(11) . ? C67 C68 1.432(10) . ? C68 C69 1.422(11) . ? C69 C70 1.390(13) . ? C69 H69 0.9500 . ? C70 C71 1.380(15) . ? C70 H70 0.9500 . ? C71 C72 1.378(13) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C75 1.411(11) . ? C74 H74 0.9500 . ? C75 C76 1.389(12) . ? C76 C77 1.377(15) . ? C76 H76 0.9500 . ? C77 C78 1.398(14) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C80 1.51(2) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C85 1.252(19) . ? C80 C81 1.457(19) . ? C81 C82 1.40(2) . ? C81 H81 0.9500 . ? C82 C83 1.32(2) . ? C82 H82 0.9500 . ? C83 C84 1.285(19) . ? C83 H83 0.9500 . ? C84 C85 1.520(19) . ? C84 H84 0.9500 . ? C85 H85 0.9500 . ? C86 C87 1.497(10) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C92 1.31(2) . ? C87 C88 1.33(2) . ? C88 C89 1.55(3) . ? C88 H88 0.9500 . ? C89 C90 1.45(2) . ? C89 H89 0.9500 . ? C90 C91 1.29(2) . ? C90 H90 0.9500 . ? C91 C92 1.30(2) . ? C91 H91 0.9500 . ? C92 H92 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Yb1 N4 83.5(2) . . ? N6 Yb1 N2 125.8(2) . . ? N4 Yb1 N2 138.2(2) . . ? N6 Yb1 N5 71.5(2) . . ? N4 Yb1 N5 80.7(2) . . ? N2 Yb1 N5 82.1(2) . . ? N6 Yb1 N1 82.1(2) . . ? N4 Yb1 N1 149.7(2) . . ? N2 Yb1 N1 70.7(2) . . ? N5 Yb1 N1 119.1(2) . . ? N6 Yb1 O1 82.2(2) . . ? N4 Yb1 O1 77.65(19) . . ? N2 Yb1 O1 129.75(19) . . ? N5 Yb1 O1 147.51(18) . . ? N1 Yb1 O1 74.1(2) . . ? N6 Yb1 N3 151.3(2) . . ? N4 Yb1 N3 70.2(2) . . ? N2 Yb1 N3 82.5(2) . . ? N5 Yb1 N3 113.5(2) . . ? N1 Yb1 N3 115.36(19) . . ? O1 Yb1 N3 81.3(2) . . ? N6 Yb1 C75 23.8(2) . . ? N4 Yb1 C75 77.5(2) . . ? N2 Yb1 C75 116.4(2) . . ? N5 Yb1 C75 48.0(2) . . ? N1 Yb1 C75 98.5(2) . . ? O1 Yb1 C75 103.24(19) . . ? N3 Yb1 C75 145.60(19) . . ? N6 Yb1 C74 49.4(2) . . ? N4 Yb1 C74 76.5(2) . . ? N2 Yb1 C74 99.6(2) . . ? N5 Yb1 C74 22.5(2) . . ? N1 Yb1 C74 112.5(2) . . ? O1 Yb1 C74 126.82(18) . . ? N3 Yb1 C74 129.7(2) . . ? C75 Yb1 C74 25.7(2) . . ? N6 Yb1 C49 104.6(2) . . ? N4 Yb1 C49 23.3(2) . . ? N2 Yb1 C49 125.2(2) . . ? N5 Yb1 C49 96.5(2) . . ? N1 Yb1 C49 143.6(2) . . ? O1 Yb1 C49 71.59(19) . . ? N3 Yb1 C49 47.70(18) . . ? C75 Yb1 C49 100.7(2) . . ? C74 Yb1 C49 97.6(2) . . ? N6 Yb1 C23 111.8(2) . . ? N4 Yb1 C23 161.5(2) . . ? N2 Yb1 C23 23.5(2) . . ? N5 Yb1 C23 93.9(2) . . ? N1 Yb1 C23 47.3(2) . . ? O1 Yb1 C23 113.73(18) . . ? N3 Yb1 C23 96.3(2) . . ? C75 Yb1 C23 112.1(2) . . ? C74 Yb1 C23 105.0(2) . . ? C49 Yb1 C23 143.6(2) . . ? N6 Yb1 C22 95.2(2) . . ? N4 Yb1 C22 171.2(2) . . ? N2 Yb1 C22 48.8(2) . . ? N5 Yb1 C22 107.2(2) . . ? N1 Yb1 C22 22.2(2) . . ? O1 Yb1 C22 93.6(2) . . ? N3 Yb1 C22 109.13(18) . . ? C75 Yb1 C22 104.6(2) . . ? C74 Yb1 C22 109.18(19) . . ? C49 Yb1 C22 153.0(2) . . ? C23 Yb1 C22 25.2(2) . . ? C22 N1 C12 118.8(7) . . ? C22 N1 Yb1 113.1(5) . . ? C12 N1 Yb1 126.9(5) . . ? C26 N2 C23 105.9(6) . . ? C26 N2 Yb1 139.7(5) . . ? C23 N2 Yb1 114.4(5) . . ? C48 N3 C38 115.3(6) . . ? C48 N3 Yb1 111.0(5) . . ? C38 N3 Yb1 132.0(4) . . ? C52 N4 C49 105.8(7) . . ? C52 N4 Yb1 137.1(6) . . ? C49 N4 Yb1 114.8(5) . . ? C74 N5 C64 117.1(6) . . ? C74 N5 Yb1 113.3(5) . . ? C64 N5 Yb1 128.9(5) . . ? C78 N6 C75 104.6(7) . . ? C78 N6 Yb1 140.6(6) . . ? C75 N6 Yb1 113.7(5) . . ? C2 O1 C21 111.6(6) . . ? C2 O1 Yb1 119.4(4) . . ? C21 O1 Yb1 127.2(5) . . ? C28 O2 C47 118.4(6) . . ? C54 O3 C73 117.1(6) . . ? C2 C1 C6 118.8(8) . . ? C2 C1 C11 121.0(7) . . ? C6 C1 C11 120.2(7) . . ? C1 C2 O1 118.1(7) . . ? C1 C2 C3 121.6(7) . . ? O1 C2 C3 120.2(7) . . ? C4 C3 C2 120.1(7) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.8(8) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 119.5(8) . . ? C4 C5 C10 122.0(8) . . ? C6 C5 C10 118.5(7) . . ? C7 C6 C5 118.5(7) . . ? C7 C6 C1 122.5(7) . . ? C5 C6 C1 119.0(7) . . ? C8 C7 C6 121.9(8) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 C9 121.2(8) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 118.5(8) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C9 C10 C5 121.4(8) . . ? C9 C10 H10 119.3 . . ? C5 C10 H10 119.3 . . ? C12 C11 C16 119.4(8) . . ? C12 C11 C1 120.7(7) . . ? C16 C11 C1 120.0(8) . . ? C11 C12 N1 120.0(7) . . ? C11 C12 C13 120.8(9) . . ? N1 C12 C13 119.2(8) . . ? C14 C13 C12 119.3(9) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 121.9(9) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C14 C15 C16 119.2(9) . . ? C14 C15 C20 121.9(11) . . ? C16 C15 C20 118.9(11) . . ? C15 C16 C11 119.4(9) . . ? C15 C16 C17 118.7(9) . . ? C11 C16 C17 122.0(8) . . ? C18 C17 C16 121.9(10) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C17 C18 C19 119.8(11) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 119.6(10) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C15 121.1(11) . . ? C19 C20 H20 119.5 . . ? C15 C20 H20 119.5 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C23 121.6(7) . . ? N1 C22 Yb1 44.7(4) . . ? C23 C22 Yb1 77.3(4) . . ? N1 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? Yb1 C22 H22 162.6 . . ? C22 C23 N2 119.5(6) . . ? C22 C23 C24 131.4(8) . . ? N2 C23 C24 109.1(7) . . ? C22 C23 Yb1 77.4(4) . . ? N2 C23 Yb1 42.1(3) . . ? C24 C23 Yb1 151.2(6) . . ? C25 C24 C23 107.0(7) . . ? C25 C24 H24 126.5 . . ? C23 C24 H24 126.5 . . ? C24 C25 C26 105.8(8) . . ? C24 C25 H25 127.1 . . ? C26 C25 H25 127.1 . . ? N2 C26 C25 112.3(8) . . ? N2 C26 H26 123.9 . . ? C25 C26 H26 123.9 . . ? C28 C27 C32 118.1(7) . . ? C28 C27 C37 123.1(7) . . ? C32 C27 C37 118.3(6) . . ? O2 C28 C27 116.1(7) . . ? O2 C28 C29 123.4(7) . . ? C27 C28 C29 120.6(7) . . ? C30 C29 C28 121.2(7) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 120.6(7) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C32 C31 C36 120.6(7) . . ? C32 C31 C30 118.6(7) . . ? C36 C31 C30 120.9(7) . . ? C33 C32 C31 117.5(7) . . ? C33 C32 C27 121.6(7) . . ? C31 C32 C27 120.8(6) . . ? C34 C33 C32 121.9(7) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C33 C34 C35 119.3(8) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C36 C35 C34 120.6(8) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C31 120.1(8) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C38 C37 C42 119.9(6) . . ? C38 C37 C27 123.4(6) . . ? C42 C37 C27 116.0(6) . . ? C37 C38 C39 119.2(6) . . ? C37 C38 N3 124.3(6) . . ? C39 C38 N3 116.5(6) . . ? C40 C39 C38 120.5(7) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C41 121.8(7) . . ? C39 C40 H40 119.1 . . ? C41 C40 H40 119.1 . . ? C40 C41 C42 118.9(7) . . ? C40 C41 C46 121.4(7) . . ? C42 C41 C46 119.6(7) . . ? C43 C42 C41 118.0(7) . . ? C43 C42 C37 122.8(7) . . ? C41 C42 C37 119.2(7) . . ? C44 C43 C42 122.0(8) . . ? C44 C43 H43 119.0 . . ? C42 C43 H43 119.0 . . ? C43 C44 C45 119.9(8) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.3(8) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C41 120.1(7) . . ? C45 C46 H46 119.9 . . ? C41 C46 H46 119.9 . . ? O2 C47 H47A 109.5 . . ? O2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N3 C48 C49 122.6(7) . . ? N3 C48 Yb1 46.8(4) . . ? C49 C48 Yb1 76.4(4) . . ? N3 C48 H48 118.7 . . ? C49 C48 H48 118.7 . . ? Yb1 C48 H48 163.3 . . ? N4 C49 C50 111.0(7) . . ? N4 C49 C48 118.9(7) . . ? C50 C49 C48 130.1(8) . . ? N4 C49 Yb1 41.9(3) . . ? C50 C49 Yb1 150.9(6) . . ? C48 C49 Yb1 77.9(4) . . ? C51 C50 C49 105.7(8) . . ? C51 C50 H50 127.2 . . ? C49 C50 H50 127.2 . . ? C50 C51 C52 106.3(7) . . ? C50 C51 H51 126.9 . . ? C52 C51 H51 126.9 . . ? N4 C52 C51 111.3(8) . . ? N4 C52 H52 124.4 . . ? C51 C52 H52 124.4 . . ? C54 C53 C58 118.3(7) . . ? C54 C53 C63 120.2(7) . . ? C58 C53 C63 121.2(7) . . ? O3 C54 C53 115.3(7) . . ? O3 C54 C55 122.1(7) . . ? C53 C54 C55 122.6(7) . . ? C56 C55 C54 120.0(8) . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C57 120.3(7) . . ? C55 C56 H56 119.8 . . ? C57 C56 H56 119.8 . . ? C62 C57 C56 121.5(7) . . ? C62 C57 C58 120.0(7) . . ? C56 C57 C58 118.5(7) . . ? C53 C58 C59 122.3(7) . . ? C53 C58 C57 120.3(7) . . ? C59 C58 C57 117.4(7) . . ? C60 C59 C58 119.8(8) . . ? C60 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C61 C60 C59 122.5(8) . . ? C61 C60 H60 118.8 . . ? C59 C60 H60 118.8 . . ? C62 C61 C60 119.6(8) . . ? C62 C61 H61 120.2 . . ? C60 C61 H61 120.2 . . ? C61 C62 C57 120.6(8) . . ? C61 C62 H62 119.7 . . ? C57 C62 H62 119.7 . . ? C64 C63 C68 119.1(7) . . ? C64 C63 C53 122.9(7) . . ? C68 C63 C53 118.0(7) . . ? C63 C64 C65 119.5(7) . . ? C63 C64 N5 123.9(7) . . ? C65 C64 N5 116.5(7) . . ? C66 C65 C64 122.1(7) . . ? C66 C65 H65 118.9 . . ? C64 C65 H65 118.9 . . ? C65 C66 C67 120.3(7) . . ? C65 C66 H66 119.9 . . ? C67 C66 H66 119.9 . . ? C66 C67 C72 123.1(7) . . ? C66 C67 C68 118.8(7) . . ? C72 C67 C68 118.0(8) . . ? C69 C68 C63 121.2(7) . . ? C69 C68 C67 118.7(8) . . ? C63 C68 C67 120.1(7) . . ? C70 C69 C68 120.7(8) . . ? C70 C69 H69 119.7 . . ? C68 C69 H69 119.7 . . ? C71 C70 C69 120.7(9) . . ? C71 C70 H70 119.6 . . ? C69 C70 H70 119.6 . . ? C70 C71 C72 120.1(9) . . ? C70 C71 H71 119.9 . . ? C72 C71 H71 119.9 . . ? C71 C72 C67 121.7(8) . . ? C71 C72 H72 119.1 . . ? C67 C72 H72 119.1 . . ? O3 C73 H73A 109.5 . . ? O3 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? O3 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N5 C74 C75 120.7(7) . . ? N5 C74 Yb1 44.3(4) . . ? C75 C74 Yb1 76.8(5) . . ? N5 C74 H74 119.7 . . ? C75 C74 H74 119.7 . . ? Yb1 C74 H74 162.6 . . ? C76 C75 N6 111.4(8) . . ? C76 C75 C74 128.7(8) . . ? N6 C75 C74 119.7(7) . . ? C76 C75 Yb1 152.3(7) . . ? N6 C75 Yb1 42.5(4) . . ? C74 C75 Yb1 77.6(4) . . ? C77 C76 C75 105.1(9) . . ? C77 C76 H76 127.4 . . ? C75 C76 H76 127.4 . . ? C76 C77 C78 108.2(9) . . ? C76 C77 H77 125.9 . . ? C78 C77 H77 125.9 . . ? N6 C78 C77 110.6(9) . . ? N6 C78 H78 124.7 . . ? C77 C78 H78 124.7 . . ? C80 C79 H79A 109.5 . . ? C80 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C80 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C85 C80 C81 120.1(16) . . ? C85 C80 C79 127.7(17) . . ? C81 C80 C79 111.8(14) . . ? C82 C81 C80 116.6(15) . . ? C82 C81 H81 121.7 . . ? C80 C81 H81 121.7 . . ? C81 C82 C83 122.4(17) . . ? C81 C82 H82 118.8 . . ? C83 C82 H82 118.8 . . ? C84 C83 C82 122.0(17) . . ? C84 C83 H83 119.0 . . ? C82 C83 H83 119.0 . . ? C83 C84 C85 118.5(15) . . ? C83 C84 H84 120.7 . . ? C85 C84 H84 120.7 . . ? C80 C85 C84 120.1(15) . . ? C80 C85 H85 120.0 . . ? C84 C85 H85 120.0 . . ? C87 C86 H86A 109.5 . . ? C87 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C87 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C92 C87 C88 131.3(18) . . ? C92 C87 C86 116(2) . . ? C88 C87 C86 111.4(19) . . ? C87 C88 C89 111.7(16) . . ? C87 C88 H88 124.1 . . ? C89 C88 H88 124.1 . . ? C90 C89 C88 115.4(14) . . ? C90 C89 H89 122.3 . . ? C88 C89 H89 122.3 . . ? C91 C90 C89 117.3(18) . . ? C91 C90 H90 121.4 . . ? C89 C90 H90 121.4 . . ? C90 C91 C92 129(2) . . ? C90 C91 H91 115.3 . . ? C92 C91 H91 115.3 . . ? C87 C92 C91 113(2) . . ? C87 C92 H92 123.4 . . ? C91 C92 H92 123.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Yb1 N1 C22 -125.5(6) . . . . ? N4 Yb1 N1 C22 172.2(5) . . . . ? N2 Yb1 N1 C22 6.9(5) . . . . ? N5 Yb1 N1 C22 -61.9(6) . . . . ? O1 Yb1 N1 C22 150.4(6) . . . . ? N3 Yb1 N1 C22 78.3(6) . . . . ? C75 Yb1 N1 C22 -108.2(5) . . . . ? C74 Yb1 N1 C22 -85.8(6) . . . . ? C49 Yb1 N1 C22 130.6(5) . . . . ? C23 Yb1 N1 C22 4.1(5) . . . . ? N6 Yb1 N1 C12 41.4(6) . . . . ? N4 Yb1 N1 C12 -20.8(9) . . . . ? N2 Yb1 N1 C12 173.9(6) . . . . ? N5 Yb1 N1 C12 105.0(6) . . . . ? O1 Yb1 N1 C12 -42.7(6) . . . . ? N3 Yb1 N1 C12 -114.7(6) . . . . ? C75 Yb1 N1 C12 58.8(6) . . . . ? C74 Yb1 N1 C12 81.2(6) . . . . ? C49 Yb1 N1 C12 -62.5(7) . . . . ? C23 Yb1 N1 C12 171.1(7) . . . . ? C22 Yb1 N1 C12 167.0(10) . . . . ? N6 Yb1 N2 C26 -116.6(8) . . . . ? N4 Yb1 N2 C26 10.0(10) . . . . ? N5 Yb1 N2 C26 -56.4(8) . . . . ? N1 Yb1 N2 C26 179.0(9) . . . . ? O1 Yb1 N2 C26 130.9(8) . . . . ? N3 Yb1 N2 C26 58.8(8) . . . . ? C75 Yb1 N2 C26 -91.0(9) . . . . ? C74 Yb1 N2 C26 -70.4(9) . . . . ? C49 Yb1 N2 C26 36.1(9) . . . . ? C23 Yb1 N2 C26 -175.9(12) . . . . ? C22 Yb1 N2 C26 -177.6(10) . . . . ? N6 Yb1 N2 C23 59.3(6) . . . . ? N4 Yb1 N2 C23 -174.1(5) . . . . ? N5 Yb1 N2 C23 119.6(6) . . . . ? N1 Yb1 N2 C23 -5.1(5) . . . . ? O1 Yb1 N2 C23 -53.2(6) . . . . ? N3 Yb1 N2 C23 -125.3(6) . . . . ? C75 Yb1 N2 C23 84.9(6) . . . . ? C74 Yb1 N2 C23 105.5(5) . . . . ? C49 Yb1 N2 C23 -148.0(5) . . . . ? C22 Yb1 N2 C23 -1.6(5) . . . . ? N6 Yb1 N3 C48 12.2(8) . . . . ? N4 Yb1 N3 C48 -12.1(5) . . . . ? N2 Yb1 N3 C48 -160.0(6) . . . . ? N5 Yb1 N3 C48 -82.0(6) . . . . ? N1 Yb1 N3 C48 135.5(5) . . . . ? O1 Yb1 N3 C48 67.8(5) . . . . ? C75 Yb1 N3 C48 -33.0(7) . . . . ? C74 Yb1 N3 C48 -63.6(6) . . . . ? C49 Yb1 N3 C48 -5.2(5) . . . . ? C23 Yb1 N3 C48 -179.1(5) . . . . ? C22 Yb1 N3 C48 158.6(5) . . . . ? N6 Yb1 N3 C38 -152.2(6) . . . . ? N4 Yb1 N3 C38 -176.6(7) . . . . ? N2 Yb1 N3 C38 35.6(7) . . . . ? N5 Yb1 N3 C38 113.5(7) . . . . ? N1 Yb1 N3 C38 -28.9(7) . . . . ? O1 Yb1 N3 C38 -96.7(7) . . . . ? C75 Yb1 N3 C38 162.5(6) . . . . ? C74 Yb1 N3 C38 131.9(6) . . . . ? C49 Yb1 N3 C38 -169.6(8) . . . . ? C23 Yb1 N3 C38 16.4(7) . . . . ? C22 Yb1 N3 C38 -5.9(7) . . . . ? N6 Yb1 N4 C52 4.3(8) . . . . ? N2 Yb1 N4 C52 -134.8(8) . . . . ? N5 Yb1 N4 C52 -68.0(8) . . . . ? N1 Yb1 N4 C52 66.2(10) . . . . ? O1 Yb1 N4 C52 87.7(8) . . . . ? N3 Yb1 N4 C52 172.8(9) . . . . ? C75 Yb1 N4 C52 -19.1(8) . . . . ? C74 Yb1 N4 C52 -45.5(8) . . . . ? C49 Yb1 N4 C52 159.6(11) . . . . ? C23 Yb1 N4 C52 -142.3(8) . . . . ? C22 Yb1 N4 C52 85.7(18) . . . . ? N6 Yb1 N4 C49 -155.4(6) . . . . ? N2 Yb1 N4 C49 65.5(7) . . . . ? N5 Yb1 N4 C49 132.4(6) . . . . ? N1 Yb1 N4 C49 -93.5(7) . . . . ? O1 Yb1 N4 C49 -72.0(5) . . . . ? N3 Yb1 N4 C49 13.1(5) . . . . ? C75 Yb1 N4 C49 -178.8(6) . . . . ? C74 Yb1 N4 C49 154.9(6) . . . . ? C23 Yb1 N4 C49 58.0(10) . . . . ? C22 Yb1 N4 C49 -74.0(16) . . . . ? N6 Yb1 N5 C74 -9.0(5) . . . . ? N4 Yb1 N5 C74 77.1(5) . . . . ? N2 Yb1 N5 C74 -141.1(5) . . . . ? N1 Yb1 N5 C74 -78.4(6) . . . . ? O1 Yb1 N5 C74 28.5(7) . . . . ? N3 Yb1 N5 C74 140.6(5) . . . . ? C75 Yb1 N5 C74 -4.4(5) . . . . ? C49 Yb1 N5 C74 94.2(5) . . . . ? C23 Yb1 N5 C74 -120.7(5) . . . . ? C22 Yb1 N5 C74 -98.8(5) . . . . ? N6 Yb1 N5 C64 -178.8(6) . . . . ? N4 Yb1 N5 C64 -92.6(6) . . . . ? N2 Yb1 N5 C64 49.2(6) . . . . ? N1 Yb1 N5 C64 111.9(6) . . . . ? O1 Yb1 N5 C64 -141.2(5) . . . . ? N3 Yb1 N5 C64 -29.1(6) . . . . ? C75 Yb1 N5 C64 -174.1(7) . . . . ? C74 Yb1 N5 C64 -169.7(9) . . . . ? C49 Yb1 N5 C64 -75.6(6) . . . . ? C23 Yb1 N5 C64 69.5(6) . . . . ? C22 Yb1 N5 C64 91.5(6) . . . . ? N4 Yb1 N6 C78 92.0(10) . . . . ? N2 Yb1 N6 C78 -120.5(10) . . . . ? N5 Yb1 N6 C78 174.3(10) . . . . ? N1 Yb1 N6 C78 -61.3(10) . . . . ? O1 Yb1 N6 C78 13.6(10) . . . . ? N3 Yb1 N6 C78 69.0(11) . . . . ? C75 Yb1 N6 C78 165.7(13) . . . . ? C74 Yb1 N6 C78 169.8(11) . . . . ? C49 Yb1 N6 C78 82.2(10) . . . . ? C23 Yb1 N6 C78 -98.9(10) . . . . ? C22 Yb1 N6 C78 -79.3(10) . . . . ? N4 Yb1 N6 C75 -73.7(6) . . . . ? N2 Yb1 N6 C75 73.8(6) . . . . ? N5 Yb1 N6 C75 8.7(5) . . . . ? N1 Yb1 N6 C75 133.0(6) . . . . ? O1 Yb1 N6 C75 -152.0(6) . . . . ? N3 Yb1 N6 C75 -96.7(7) . . . . ? C74 Yb1 N6 C75 4.1(5) . . . . ? C49 Yb1 N6 C75 -83.5(6) . . . . ? C23 Yb1 N6 C75 95.5(6) . . . . ? C22 Yb1 N6 C75 115.1(6) . . . . ? N6 Yb1 O1 C2 -140.6(5) . . . . ? N4 Yb1 O1 C2 134.4(5) . . . . ? N2 Yb1 O1 C2 -9.7(6) . . . . ? N5 Yb1 O1 C2 -176.3(5) . . . . ? N1 Yb1 O1 C2 -56.7(5) . . . . ? N3 Yb1 O1 C2 62.9(5) . . . . ? C75 Yb1 O1 C2 -151.8(5) . . . . ? C74 Yb1 O1 C2 -163.2(5) . . . . ? C49 Yb1 O1 C2 111.1(5) . . . . ? C23 Yb1 O1 C2 -30.2(5) . . . . ? C22 Yb1 O1 C2 -45.9(5) . . . . ? N6 Yb1 O1 C21 55.8(7) . . . . ? N4 Yb1 O1 C21 -29.1(7) . . . . ? N2 Yb1 O1 C21 -173.3(7) . . . . ? N5 Yb1 O1 C21 20.1(8) . . . . ? N1 Yb1 O1 C21 139.8(7) . . . . ? N3 Yb1 O1 C21 -100.6(7) . . . . ? C75 Yb1 O1 C21 44.6(7) . . . . ? C74 Yb1 O1 C21 33.3(7) . . . . ? C49 Yb1 O1 C21 -52.4(7) . . . . ? C23 Yb1 O1 C21 166.3(7) . . . . ? C22 Yb1 O1 C21 150.6(7) . . . . ? C6 C1 C2 O1 -173.8(6) . . . . ? C11 C1 C2 O1 6.6(11) . . . . ? C6 C1 C2 C3 3.4(11) . . . . ? C11 C1 C2 C3 -176.3(8) . . . . ? C21 O1 C2 C1 -109.4(8) . . . . ? Yb1 O1 C2 C1 84.6(7) . . . . ? C21 O1 C2 C3 73.4(9) . . . . ? Yb1 O1 C2 C3 -92.6(7) . . . . ? C1 C2 C3 C4 -1.7(12) . . . . ? O1 C2 C3 C4 175.4(7) . . . . ? C2 C3 C4 C5 -0.9(13) . . . . ? C3 C4 C5 C6 1.6(14) . . . . ? C3 C4 C5 C10 -176.4(9) . . . . ? C4 C5 C6 C7 -178.7(8) . . . . ? C10 C5 C6 C7 -0.6(13) . . . . ? C4 C5 C6 C1 0.2(13) . . . . ? C10 C5 C6 C1 178.3(8) . . . . ? C2 C1 C6 C7 176.2(8) . . . . ? C11 C1 C6 C7 -4.2(12) . . . . ? C2 C1 C6 C5 -2.6(12) . . . . ? C11 C1 C6 C5 177.1(8) . . . . ? C5 C6 C7 C8 -0.6(13) . . . . ? C1 C6 C7 C8 -179.4(8) . . . . ? C6 C7 C8 C9 0.4(14) . . . . ? C7 C8 C9 C10 1.1(15) . . . . ? C8 C9 C10 C5 -2.3(14) . . . . ? C4 C5 C10 C9 -179.9(9) . . . . ? C6 C5 C10 C9 2.0(14) . . . . ? C2 C1 C11 C12 -70.0(10) . . . . ? C6 C1 C11 C12 110.4(9) . . . . ? C2 C1 C11 C16 110.3(9) . . . . ? C6 C1 C11 C16 -69.3(10) . . . . ? C16 C11 C12 N1 -174.0(7) . . . . ? C1 C11 C12 N1 6.3(11) . . . . ? C16 C11 C12 C13 3.4(11) . . . . ? C1 C11 C12 C13 -176.3(7) . . . . ? C22 N1 C12 C11 -117.9(8) . . . . ? Yb1 N1 C12 C11 75.8(8) . . . . ? C22 N1 C12 C13 64.7(9) . . . . ? Yb1 N1 C12 C13 -101.6(7) . . . . ? C11 C12 C13 C14 -0.6(12) . . . . ? N1 C12 C13 C14 176.7(7) . . . . ? C12 C13 C14 C15 -2.0(14) . . . . ? C13 C14 C15 C16 1.7(15) . . . . ? C13 C14 C15 C20 -177.0(10) . . . . ? C14 C15 C16 C11 1.1(14) . . . . ? C20 C15 C16 C11 179.9(9) . . . . ? C14 C15 C16 C17 -178.4(9) . . . . ? C20 C15 C16 C17 0.3(14) . . . . ? C12 C11 C16 C15 -3.6(12) . . . . ? C1 C11 C16 C15 176.1(8) . . . . ? C12 C11 C16 C17 175.9(8) . . . . ? C1 C11 C16 C17 -4.4(12) . . . . ? C15 C16 C17 C18 0.7(14) . . . . ? C11 C16 C17 C18 -178.9(9) . . . . ? C16 C17 C18 C19 -1.0(17) . . . . ? C17 C18 C19 C20 0.3(19) . . . . ? C18 C19 C20 C15 0.6(19) . . . . ? C14 C15 C20 C19 177.8(11) . . . . ? C16 C15 C20 C19 -0.9(17) . . . . ? C12 N1 C22 C23 -176.3(7) . . . . ? Yb1 N1 C22 C23 -8.2(9) . . . . ? C12 N1 C22 Yb1 -168.1(9) . . . . ? N6 Yb1 C22 N1 54.0(6) . . . . ? N4 Yb1 C22 N1 -26.5(17) . . . . ? N2 Yb1 C22 N1 -171.3(6) . . . . ? N5 Yb1 C22 N1 126.2(5) . . . . ? O1 Yb1 C22 N1 -28.4(5) . . . . ? N3 Yb1 C22 N1 -110.5(5) . . . . ? C75 Yb1 C22 N1 76.2(6) . . . . ? C74 Yb1 C22 N1 102.7(5) . . . . ? C49 Yb1 C22 N1 -83.3(7) . . . . ? C23 Yb1 C22 N1 -172.9(8) . . . . ? N6 Yb1 C22 C23 -133.1(5) . . . . ? N4 Yb1 C22 C23 146.4(14) . . . . ? N2 Yb1 C22 C23 1.5(4) . . . . ? N5 Yb1 C22 C23 -60.9(5) . . . . ? N1 Yb1 C22 C23 172.9(8) . . . . ? O1 Yb1 C22 C23 144.4(5) . . . . ? N3 Yb1 C22 C23 62.4(5) . . . . ? C75 Yb1 C22 C23 -110.9(5) . . . . ? C74 Yb1 C22 C23 -84.5(5) . . . . ? C49 Yb1 C22 C23 89.6(7) . . . . ? N1 C22 C23 N2 3.6(12) . . . . ? Yb1 C22 C23 N2 -2.2(6) . . . . ? N1 C22 C23 C24 -174.8(9) . . . . ? Yb1 C22 C23 C24 179.3(10) . . . . ? N1 C22 C23 Yb1 5.9(7) . . . . ? C26 N2 C23 C22 -179.5(7) . . . . ? Yb1 N2 C23 C22 3.3(9) . . . . ? C26 N2 C23 C24 -0.7(9) . . . . ? Yb1 N2 C23 C24 -178.0(6) . . . . ? C26 N2 C23 Yb1 177.3(8) . . . . ? N6 Yb1 C23 C22 51.5(5) . . . . ? N4 Yb1 C23 C22 -164.6(7) . . . . ? N2 Yb1 C23 C22 -177.1(8) . . . . ? N5 Yb1 C23 C22 123.2(5) . . . . ? N1 Yb1 C23 C22 -3.6(4) . . . . ? O1 Yb1 C23 C22 -39.4(5) . . . . ? N3 Yb1 C23 C22 -122.6(5) . . . . ? C75 Yb1 C23 C22 77.3(5) . . . . ? C74 Yb1 C23 C22 103.3(5) . . . . ? C49 Yb1 C23 C22 -130.2(5) . . . . ? N6 Yb1 C23 N2 -131.4(5) . . . . ? N4 Yb1 C23 N2 12.5(10) . . . . ? N5 Yb1 C23 N2 -59.7(6) . . . . ? N1 Yb1 C23 N2 173.4(7) . . . . ? O1 Yb1 C23 N2 137.7(5) . . . . ? N3 Yb1 C23 N2 54.5(6) . . . . ? C75 Yb1 C23 N2 -105.6(6) . . . . ? C74 Yb1 C23 N2 -79.6(6) . . . . ? C49 Yb1 C23 N2 46.9(7) . . . . ? C22 Yb1 C23 N2 177.1(8) . . . . ? N6 Yb1 C23 C24 -127.4(13) . . . . ? N4 Yb1 C23 C24 16.5(17) . . . . ? N2 Yb1 C23 C24 4.0(11) . . . . ? N5 Yb1 C23 C24 -55.8(13) . . . . ? N1 Yb1 C23 C24 177.4(14) . . . . ? O1 Yb1 C23 C24 141.7(13) . . . . ? N3 Yb1 C23 C24 58.4(13) . . . . ? C75 Yb1 C23 C24 -101.7(13) . . . . ? C74 Yb1 C23 C24 -75.6(13) . . . . ? C49 Yb1 C23 C24 50.8(14) . . . . ? C22 Yb1 C23 C24 -178.9(16) . . . . ? C22 C23 C24 C25 178.8(9) . . . . ? N2 C23 C24 C25 0.2(11) . . . . ? Yb1 C23 C24 C25 -2.6(17) . . . . ? C23 C24 C25 C26 0.4(11) . . . . ? C23 N2 C26 C25 1.0(10) . . . . ? Yb1 N2 C26 C25 177.1(6) . . . . ? C24 C25 C26 N2 -0.9(11) . . . . ? C47 O2 C28 C27 173.5(7) . . . . ? C47 O2 C28 C29 -6.6(11) . . . . ? C32 C27 C28 O2 176.5(7) . . . . ? C37 C27 C28 O2 4.1(11) . . . . ? C32 C27 C28 C29 -3.4(11) . . . . ? C37 C27 C28 C29 -175.7(7) . . . . ? O2 C28 C29 C30 -177.8(7) . . . . ? C27 C28 C29 C30 2.0(12) . . . . ? C28 C29 C30 C31 0.9(11) . . . . ? C29 C30 C31 C32 -2.4(11) . . . . ? C29 C30 C31 C36 176.4(7) . . . . ? C36 C31 C32 C33 -0.9(10) . . . . ? C30 C31 C32 C33 177.8(6) . . . . ? C36 C31 C32 C27 -177.9(7) . . . . ? C30 C31 C32 C27 0.9(11) . . . . ? C28 C27 C32 C33 -174.8(7) . . . . ? C37 C27 C32 C33 -2.2(10) . . . . ? C28 C27 C32 C31 1.9(11) . . . . ? C37 C27 C32 C31 174.6(6) . . . . ? C31 C32 C33 C34 -0.1(10) . . . . ? C27 C32 C33 C34 176.7(7) . . . . ? C32 C33 C34 C35 0.1(11) . . . . ? C33 C34 C35 C36 1.1(11) . . . . ? C34 C35 C36 C31 -2.2(12) . . . . ? C32 C31 C36 C35 2.2(11) . . . . ? C30 C31 C36 C35 -176.6(7) . . . . ? C28 C27 C37 C38 -99.3(9) . . . . ? C32 C27 C37 C38 88.4(9) . . . . ? C28 C27 C37 C42 90.0(9) . . . . ? C32 C27 C37 C42 -82.3(9) . . . . ? C42 C37 C38 C39 7.2(11) . . . . ? C27 C37 C38 C39 -163.1(7) . . . . ? C42 C37 C38 N3 -173.9(7) . . . . ? C27 C37 C38 N3 15.7(12) . . . . ? C48 N3 C38 C37 45.2(11) . . . . ? Yb1 N3 C38 C37 -150.9(6) . . . . ? C48 N3 C38 C39 -136.0(8) . . . . ? Yb1 N3 C38 C39 28.0(10) . . . . ? C37 C38 C39 C40 -6.4(12) . . . . ? N3 C38 C39 C40 174.7(8) . . . . ? C38 C39 C40 C41 0.3(14) . . . . ? C39 C40 C41 C42 4.9(14) . . . . ? C39 C40 C41 C46 -177.9(9) . . . . ? C40 C41 C42 C43 176.7(8) . . . . ? C46 C41 C42 C43 -0.5(12) . . . . ? C40 C41 C42 C37 -3.9(12) . . . . ? C46 C41 C42 C37 178.9(7) . . . . ? C38 C37 C42 C43 177.2(7) . . . . ? C27 C37 C42 C43 -11.7(10) . . . . ? C38 C37 C42 C41 -2.1(11) . . . . ? C27 C37 C42 C41 168.9(7) . . . . ? C41 C42 C43 C44 -0.6(12) . . . . ? C37 C42 C43 C44 180.0(7) . . . . ? C42 C43 C44 C45 0.0(13) . . . . ? C43 C44 C45 C46 1.9(14) . . . . ? C44 C45 C46 C41 -3.0(14) . . . . ? C40 C41 C46 C45 -174.8(9) . . . . ? C42 C41 C46 C45 2.3(13) . . . . ? C38 N3 C48 C49 177.5(7) . . . . ? Yb1 N3 C48 C49 10.2(9) . . . . ? C38 N3 C48 Yb1 167.3(8) . . . . ? N6 Yb1 C48 N3 -172.4(5) . . . . ? N4 Yb1 C48 N3 164.7(6) . . . . ? N2 Yb1 C48 N3 20.4(6) . . . . ? N5 Yb1 C48 N3 106.5(5) . . . . ? N1 Yb1 C48 N3 -55.5(6) . . . . ? O1 Yb1 C48 N3 -107.5(5) . . . . ? C75 Yb1 C48 N3 157.7(5) . . . . ? C74 Yb1 C48 N3 129.0(5) . . . . ? C49 Yb1 C48 N3 171.2(8) . . . . ? C23 Yb1 C48 N3 1.0(6) . . . . ? C22 Yb1 C48 N3 -26.6(6) . . . . ? N6 Yb1 C48 C49 16.4(6) . . . . ? N4 Yb1 C48 C49 -6.4(4) . . . . ? N2 Yb1 C48 C49 -150.7(5) . . . . ? N5 Yb1 C48 C49 -64.7(5) . . . . ? N1 Yb1 C48 C49 133.3(5) . . . . ? O1 Yb1 C48 C49 81.3(5) . . . . ? N3 Yb1 C48 C49 -171.2(8) . . . . ? C75 Yb1 C48 C49 -13.5(5) . . . . ? C74 Yb1 C48 C49 -42.2(5) . . . . ? C23 Yb1 C48 C49 -170.1(4) . . . . ? C22 Yb1 C48 C49 162.3(4) . . . . ? C52 N4 C49 C50 1.0(9) . . . . ? Yb1 N4 C49 C50 166.8(6) . . . . ? C52 N4 C49 C48 -179.5(7) . . . . ? Yb1 N4 C49 C48 -13.8(9) . . . . ? C52 N4 C49 Yb1 -165.8(8) . . . . ? N3 C48 C49 N4 1.7(12) . . . . ? Yb1 C48 C49 N4 9.4(6) . . . . ? N3 C48 C49 C50 -179.0(9) . . . . ? Yb1 C48 C49 C50 -171.3(10) . . . . ? N3 C48 C49 Yb1 -7.6(7) . . . . ? N6 Yb1 C49 N4 25.3(6) . . . . ? N2 Yb1 C49 N4 -132.1(5) . . . . ? N5 Yb1 C49 N4 -47.2(6) . . . . ? N1 Yb1 C49 N4 121.8(6) . . . . ? O1 Yb1 C49 N4 101.8(6) . . . . ? N3 Yb1 C49 N4 -163.2(7) . . . . ? C75 Yb1 C49 N4 1.2(6) . . . . ? C74 Yb1 C49 N4 -24.6(6) . . . . ? C23 Yb1 C49 N4 -153.0(5) . . . . ? C22 Yb1 C49 N4 161.1(6) . . . . ? N6 Yb1 C49 C50 -0.7(13) . . . . ? N4 Yb1 C49 C50 -26.0(11) . . . . ? N2 Yb1 C49 C50 -158.1(12) . . . . ? N5 Yb1 C49 C50 -73.2(13) . . . . ? N1 Yb1 C49 C50 95.8(13) . . . . ? O1 Yb1 C49 C50 75.7(13) . . . . ? N3 Yb1 C49 C50 170.8(14) . . . . ? C75 Yb1 C49 C50 -24.8(13) . . . . ? C74 Yb1 C49 C50 -50.6(13) . . . . ? C23 Yb1 C49 C50 -179.0(11) . . . . ? C22 Yb1 C49 C50 135.1(12) . . . . ? N6 Yb1 C49 C48 -167.0(5) . . . . ? N4 Yb1 C49 C48 167.7(8) . . . . ? N2 Yb1 C49 C48 35.6(5) . . . . ? N5 Yb1 C49 C48 120.5(5) . . . . ? N1 Yb1 C49 C48 -70.5(6) . . . . ? O1 Yb1 C49 C48 -90.5(5) . . . . ? N3 Yb1 C49 C48 4.5(4) . . . . ? C75 Yb1 C49 C48 168.9(4) . . . . ? C74 Yb1 C49 C48 143.1(4) . . . . ? C23 Yb1 C49 C48 14.7(6) . . . . ? C22 Yb1 C49 C48 -31.2(8) . . . . ? N4 C49 C50 C51 -1.2(10) . . . . ? C48 C49 C50 C51 179.5(9) . . . . ? Yb1 C49 C50 C51 17.1(16) . . . . ? C49 C50 C51 C52 0.9(10) . . . . ? C49 N4 C52 C51 -0.5(9) . . . . ? Yb1 N4 C52 C51 -161.3(6) . . . . ? C50 C51 C52 N4 -0.2(10) . . . . ? C73 O3 C54 C53 156.2(8) . . . . ? C73 O3 C54 C55 -23.2(12) . . . . ? C58 C53 C54 O3 179.4(7) . . . . ? C63 C53 C54 O3 6.0(12) . . . . ? C58 C53 C54 C55 -1.1(14) . . . . ? C63 C53 C54 C55 -174.6(8) . . . . ? O3 C54 C55 C56 -178.4(8) . . . . ? C53 C54 C55 C56 2.2(14) . . . . ? C54 C55 C56 C57 -1.4(14) . . . . ? C55 C56 C57 C62 179.8(9) . . . . ? C55 C56 C57 C58 -0.3(13) . . . . ? C54 C53 C58 C59 -179.9(8) . . . . ? C63 C53 C58 C59 -6.5(13) . . . . ? C54 C53 C58 C57 -0.6(13) . . . . ? C63 C53 C58 C57 172.8(7) . . . . ? C62 C57 C58 C53 -178.8(8) . . . . ? C56 C57 C58 C53 1.3(12) . . . . ? C62 C57 C58 C59 0.5(12) . . . . ? C56 C57 C58 C59 -179.4(8) . . . . ? C53 C58 C59 C60 179.6(8) . . . . ? C57 C58 C59 C60 0.3(12) . . . . ? C58 C59 C60 C61 0.4(15) . . . . ? C59 C60 C61 C62 -1.9(15) . . . . ? C60 C61 C62 C57 2.7(15) . . . . ? C56 C57 C62 C61 177.8(9) . . . . ? C58 C57 C62 C61 -2.0(13) . . . . ? C54 C53 C63 C64 -95.0(10) . . . . ? C58 C53 C63 C64 91.7(10) . . . . ? C54 C53 C63 C68 84.8(10) . . . . ? C58 C53 C63 C68 -88.4(10) . . . . ? C68 C63 C64 C65 1.3(10) . . . . ? C53 C63 C64 C65 -178.8(7) . . . . ? C68 C63 C64 N5 178.1(6) . . . . ? C53 C63 C64 N5 -2.1(11) . . . . ? C74 N5 C64 C63 50.8(10) . . . . ? Yb1 N5 C64 C63 -139.8(6) . . . . ? C74 N5 C64 C65 -132.4(7) . . . . ? Yb1 N5 C64 C65 37.0(9) . . . . ? C63 C64 C65 C66 -2.8(11) . . . . ? N5 C64 C65 C66 -179.8(7) . . . . ? C64 C65 C66 C67 2.2(11) . . . . ? C65 C66 C67 C72 -180.0(7) . . . . ? C65 C66 C67 C68 -0.2(10) . . . . ? C64 C63 C68 C69 179.3(7) . . . . ? C53 C63 C68 C69 -0.6(10) . . . . ? C64 C63 C68 C67 0.6(10) . . . . ? C53 C63 C68 C67 -179.3(6) . . . . ? C66 C67 C68 C69 -179.9(7) . . . . ? C72 C67 C68 C69 -0.1(9) . . . . ? C66 C67 C68 C63 -1.2(9) . . . . ? C72 C67 C68 C63 178.6(7) . . . . ? C63 C68 C69 C70 -178.5(8) . . . . ? C67 C68 C69 C70 0.2(11) . . . . ? C68 C69 C70 C71 0.1(14) . . . . ? C69 C70 C71 C72 -0.4(14) . . . . ? C70 C71 C72 C67 0.5(13) . . . . ? C66 C67 C72 C71 179.6(8) . . . . ? C68 C67 C72 C71 -0.2(11) . . . . ? C64 N5 C74 C75 179.5(7) . . . . ? Yb1 N5 C74 C75 8.5(9) . . . . ? C64 N5 C74 Yb1 171.0(8) . . . . ? N6 Yb1 C74 N5 168.7(6) . . . . ? N4 Yb1 C74 N5 -98.4(5) . . . . ? N2 Yb1 C74 N5 39.1(5) . . . . ? N1 Yb1 C74 N5 112.1(5) . . . . ? O1 Yb1 C74 N5 -161.3(5) . . . . ? N3 Yb1 C74 N5 -49.1(6) . . . . ? C75 Yb1 C74 N5 172.5(8) . . . . ? C49 Yb1 C74 N5 -88.6(5) . . . . ? C23 Yb1 C74 N5 62.6(5) . . . . ? C22 Yb1 C74 N5 88.6(5) . . . . ? N6 Yb1 C74 C75 -3.8(5) . . . . ? N4 Yb1 C74 C75 89.1(5) . . . . ? N2 Yb1 C74 C75 -133.4(5) . . . . ? N5 Yb1 C74 C75 -172.5(8) . . . . ? N1 Yb1 C74 C75 -60.4(5) . . . . ? O1 Yb1 C74 C75 26.2(5) . . . . ? N3 Yb1 C74 C75 138.3(5) . . . . ? C49 Yb1 C74 C75 98.8(5) . . . . ? C23 Yb1 C74 C75 -109.9(5) . . . . ? C22 Yb1 C74 C75 -83.9(5) . . . . ? C78 N6 C75 C76 -2.1(11) . . . . ? Yb1 N6 C75 C76 168.6(7) . . . . ? C78 N6 C75 C74 -178.8(8) . . . . ? Yb1 N6 C75 C74 -8.2(10) . . . . ? C78 N6 C75 Yb1 -170.7(9) . . . . ? N5 C74 C75 C76 -176.5(10) . . . . ? Yb1 C74 C75 C76 -170.5(11) . . . . ? N5 C74 C75 N6 -0.4(12) . . . . ? Yb1 C74 C75 N6 5.6(7) . . . . ? N5 C74 C75 Yb1 -6.1(7) . . . . ? N6 Yb1 C75 C76 -23.4(14) . . . . ? N4 Yb1 C75 C76 79.0(16) . . . . ? N2 Yb1 C75 C76 -143.1(15) . . . . ? N5 Yb1 C75 C76 167.7(17) . . . . ? N1 Yb1 C75 C76 -70.5(16) . . . . ? O1 Yb1 C75 C76 5.1(16) . . . . ? N3 Yb1 C75 C76 99.1(16) . . . . ? C74 Yb1 C75 C76 163.8(18) . . . . ? C49 Yb1 C75 C76 78.5(16) . . . . ? C23 Yb1 C75 C76 -117.7(15) . . . . ? C22 Yb1 C75 C76 -92.2(16) . . . . ? N4 Yb1 C75 N6 102.4(6) . . . . ? N2 Yb1 C75 N6 -119.7(6) . . . . ? N5 Yb1 C75 N6 -168.9(7) . . . . ? N1 Yb1 C75 N6 -47.1(6) . . . . ? O1 Yb1 C75 N6 28.5(6) . . . . ? N3 Yb1 C75 N6 122.5(6) . . . . ? C74 Yb1 C75 N6 -172.8(9) . . . . ? C49 Yb1 C75 N6 101.9(6) . . . . ? C23 Yb1 C75 N6 -94.3(6) . . . . ? C22 Yb1 C75 N6 -68.8(6) . . . . ? N6 Yb1 C75 C74 172.8(9) . . . . ? N4 Yb1 C75 C74 -84.8(5) . . . . ? N2 Yb1 C75 C74 53.1(5) . . . . ? N5 Yb1 C75 C74 3.8(4) . . . . ? N1 Yb1 C75 C74 125.7(5) . . . . ? O1 Yb1 C75 C74 -158.7(4) . . . . ? N3 Yb1 C75 C74 -64.8(6) . . . . ? C49 Yb1 C75 C74 -85.3(5) . . . . ? C23 Yb1 C75 C74 78.5(5) . . . . ? C22 Yb1 C75 C74 103.9(5) . . . . ? N6 C75 C76 C77 2.3(13) . . . . ? C74 C75 C76 C77 178.7(10) . . . . ? Yb1 C75 C76 C77 19(2) . . . . ? C75 C76 C77 C78 -1.6(15) . . . . ? C75 N6 C78 C77 1.0(12) . . . . ? Yb1 N6 C78 C77 -165.5(8) . . . . ? C76 C77 C78 N6 0.4(15) . . . . ? C85 C80 C81 C82 4.1(19) . . . . ? C79 C80 C81 C82 177.3(12) . . . . ? C80 C81 C82 C83 0(2) . . . . ? C81 C82 C83 C84 -2(3) . . . . ? C82 C83 C84 C85 1(2) . . . . ? C81 C80 C85 C84 -5.1(19) . . . . ? C79 C80 C85 C84 -177.1(12) . . . . ? C83 C84 C85 C80 2(2) . . . . ? C92 C87 C88 C89 -3(4) . . . . ? C86 C87 C88 C89 -171.8(19) . . . . ? C87 C88 C89 C90 -2(2) . . . . ? C88 C89 C90 C91 -1.5(19) . . . . ? C89 C90 C91 C92 12(3) . . . . ? C88 C87 C92 C91 12(4) . . . . ? C86 C87 C92 C91 179(2) . . . . ? C90 C91 C92 C87 -16(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.166 _refine_diff_density_min -1.260 _refine_diff_density_rms 0.152 # Attachment 'compound_7.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 687847' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H81 N6 O3 Sm' _chemical_formula_sum 'C78 H81 N6 O3 Sm' _chemical_formula_weight 1300.84 _chemical_absolute_configuratiom rm loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 14.048(2) _cell_length_b 15.095(2) _cell_length_c 36.137(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7663(2) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 18305 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2708 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8415 _exptl_absorpt_correction_T_max 0.8810 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 59268 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.88 _reflns_number_total 18043 _reflns_number_gt 17232 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+0.1859P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.022(7) _refine_ls_number_reflns 18043 _refine_ls_number_parameters 800 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.224452(11) 0.558906(10) 0.384190(4) 0.02218(4) Uani 1 1 d . . . N1 N 0.1865(2) 0.5090(2) 0.31910(7) 0.0300(6) Uani 1 1 d . . . N2 N 0.2658(2) 0.6712(2) 0.33815(7) 0.0300(6) Uani 1 1 d . . . N3 N 0.40556(19) 0.5461(2) 0.39344(7) 0.0302(6) Uani 1 1 d . . . N4 N 0.2651(2) 0.53159(17) 0.44883(7) 0.0249(5) Uani 1 1 d . . . N5 N 0.13514(18) 0.67943(19) 0.41597(7) 0.0251(5) Uani 1 1 d . . . N6 N 0.0613(2) 0.5134(2) 0.39833(8) 0.0303(6) Uani 1 1 d . . . O1 O 0.23419(17) 0.38919(13) 0.38754(5) 0.0288(5) Uani 1 1 d . . . O2 O 0.6480(2) 0.5235(3) 0.43993(8) 0.0589(10) Uani 1 1 d . . . O3 O -0.02406(16) 0.84009(16) 0.46963(6) 0.0284(5) Uani 1 1 d . . . C1 C 0.2660(3) 0.3350(2) 0.32684(9) 0.0307(7) Uani 1 1 d . . . C2 C 0.2959(3) 0.3472(2) 0.36356(9) 0.0335(8) Uani 1 1 d . . . C3 C 0.3864(3) 0.3217(3) 0.37444(11) 0.0455(10) Uani 1 1 d . . . H3 H 0.4054 0.3267 0.3996 0.055 Uiso 1 1 calc R . . C4 C 0.4480(3) 0.2892(3) 0.34850(14) 0.0601(14) Uani 1 1 d . . . H4 H 0.5096 0.2707 0.3561 0.072 Uiso 1 1 calc R . . C5 C 0.4232(3) 0.2823(4) 0.31113(14) 0.0612(15) Uani 1 1 d . . . C6 C 0.3312(3) 0.3068(3) 0.30021(11) 0.0427(10) Uani 1 1 d . . . C7 C 0.3003(3) 0.3024(4) 0.25982(10) 0.0537(12) Uani 1 1 d . . . H7A H 0.2682 0.3586 0.2532 0.064 Uiso 1 1 calc R . . H7B H 0.2534 0.2539 0.2569 0.064 Uiso 1 1 calc R . . C8 C 0.3827(4) 0.2868(5) 0.23310(15) 0.087(2) Uani 1 1 d . . . H8A H 0.3568 0.2665 0.2091 0.105 Uiso 1 1 calc R . . H8B H 0.4160 0.3438 0.2288 0.105 Uiso 1 1 calc R . . C9 C 0.4519(4) 0.2214(5) 0.24652(17) 0.106(3) Uani 1 1 d . . . H9A H 0.5023 0.2129 0.2277 0.127 Uiso 1 1 calc R . . H9B H 0.4196 0.1638 0.2503 0.127 Uiso 1 1 calc R . . C10 C 0.4976(3) 0.2514(5) 0.28321(17) 0.095(2) Uani 1 1 d . . . H10A H 0.5342 0.2016 0.2939 0.114 Uiso 1 1 calc R . . H10B H 0.5426 0.3004 0.2782 0.114 Uiso 1 1 calc R . . C11 C 0.1631(2) 0.3490(2) 0.31675(8) 0.0292(7) Uani 1 1 d . . . C12 C 0.1288(2) 0.4335(3) 0.31101(8) 0.0296(7) Uani 1 1 d . . . C13 C 0.0335(2) 0.4455(3) 0.29995(8) 0.0342(7) Uani 1 1 d . . . H13 H 0.0095 0.5034 0.2955 0.041 Uiso 1 1 calc R . . C14 C -0.0246(3) 0.3728(3) 0.29555(9) 0.0365(9) Uani 1 1 d . . . H14 H -0.0887 0.3812 0.2880 0.044 Uiso 1 1 calc R . . C15 C 0.0085(3) 0.2876(3) 0.30186(9) 0.0332(8) Uani 1 1 d . A . C16 C 0.1035(2) 0.2758(3) 0.31269(8) 0.0299(7) Uani 1 1 d . . . C17 C 0.1416(3) 0.1842(3) 0.32043(10) 0.0408(9) Uani 1 1 d . A . H17A H 0.1919 0.1709 0.3020 0.049 Uiso 1 1 calc R . . H17B H 0.1720 0.1846 0.3451 0.049 Uiso 1 1 calc R . . C18 C 0.0707(4) 0.1119(4) 0.31952(19) 0.086(2) Uani 1 1 d D . . H18A H 0.0823 0.0750 0.3407 0.104 Uiso 0.396(7) 1 d PR A 1 H18B H 0.0855 0.0769 0.2981 0.104 Uiso 0.396(7) 1 d PR A 1 H18C H 0.0422 0.1053 0.3435 0.104 Uiso 0.604(7) 1 d PR A 2 H18D H 0.1034 0.0577 0.3138 0.104 Uiso 0.604(7) 1 d PR A 2 C19 C -0.0321(6) 0.1265(6) 0.3181(3) 0.0525(16) Uani 0.396(7) 1 d PD A 1 H19A H -0.0570 0.1315 0.3436 0.063 Uiso 0.396(7) 1 calc PR A 1 H19B H -0.0629 0.0746 0.3063 0.063 Uiso 0.396(7) 1 calc PR A 1 C19' C -0.0068(5) 0.1251(4) 0.2918(2) 0.0525(16) Uani 0.604(7) 1 d PD A 2 H19C H -0.0529 0.0758 0.2939 0.063 Uiso 0.604(7) 1 calc PR A 2 H19D H 0.0211 0.1226 0.2666 0.063 Uiso 0.604(7) 1 calc PR A 2 C20 C -0.0588(3) 0.2112(3) 0.29622(11) 0.0433(9) Uani 1 1 d D . . H20A H -0.0593 0.1962 0.2704 0.052 Uiso 0.396(7) 1 d PR A 1 H20B H -0.1220 0.2298 0.3028 0.052 Uiso 0.396(7) 1 d PR A 1 H20C H -0.0970 0.2223 0.2747 0.052 Uiso 0.604(7) 1 d PR A 2 H20D H -0.1008 0.2067 0.3171 0.052 Uiso 0.604(7) 1 d PR A 2 C21 C 0.2118(3) 0.3388(2) 0.42029(9) 0.0378(8) Uani 1 1 d . . . H21A H 0.1870 0.2806 0.4131 0.057 Uiso 1 1 calc R . . H21B H 0.1637 0.3704 0.4348 0.057 Uiso 1 1 calc R . . H21C H 0.2695 0.3311 0.4352 0.057 Uiso 1 1 calc R . . C22 C 0.1990(2) 0.5690(3) 0.29378(8) 0.0344(8) Uani 1 1 d . . . H22 H 0.1774 0.5576 0.2693 0.041 Uiso 1 1 calc R . . C23 C 0.2437(2) 0.6505(3) 0.30154(9) 0.0340(8) Uani 1 1 d . . . C24 C 0.2708(3) 0.7210(3) 0.27844(9) 0.0439(9) Uani 1 1 d . . . H24 H 0.2640 0.7234 0.2523 0.053 Uiso 1 1 calc R . . C25 C 0.3088(3) 0.7854(3) 0.30048(11) 0.0427(9) Uani 1 1 d . . . H25 H 0.3337 0.8408 0.2926 0.051 Uiso 1 1 calc R . . C26 C 0.3040(2) 0.7540(2) 0.33674(10) 0.0357(8) Uani 1 1 d . . . H26 H 0.3248 0.7864 0.3578 0.043 Uiso 1 1 calc R . . C27 C 0.5915(3) 0.6460(4) 0.40877(9) 0.0513(13) Uani 1 1 d . . . C28 C 0.6295(3) 0.6137(4) 0.44123(11) 0.0528(12) Uani 1 1 d . . . C29 C 0.6502(3) 0.6695(4) 0.47136(10) 0.0573(14) Uani 1 1 d . . . H29 H 0.6753 0.6466 0.4938 0.069 Uiso 1 1 calc R . . C30 C 0.6326(3) 0.7598(4) 0.46692(13) 0.0600(13) Uani 1 1 d . . . H30 H 0.6461 0.7988 0.4869 0.072 Uiso 1 1 calc R . . C31 C 0.5977(3) 0.7932(4) 0.43575(13) 0.0605(14) Uani 1 1 d . . . C32 C 0.5753(3) 0.7360(4) 0.40588(11) 0.0521(12) Uani 1 1 d . . . C33 C 0.5407(3) 0.7727(3) 0.37030(12) 0.0555(12) Uani 1 1 d . . . H33A H 0.4876 0.7353 0.3613 0.067 Uiso 1 1 calc R . . H33B H 0.5927 0.7690 0.3519 0.067 Uiso 1 1 calc R . . C34 C 0.5063(3) 0.8691(4) 0.37244(16) 0.0671(15) Uani 1 1 d . . . H34A H 0.4999 0.8931 0.3471 0.081 Uiso 1 1 calc R . . H34B H 0.4427 0.8707 0.3842 0.081 Uiso 1 1 calc R . . C35 C 0.5738(4) 0.9275(4) 0.39428(18) 0.0838(19) Uani 1 1 d . . . H35A H 0.6365 0.9296 0.3818 0.101 Uiso 1 1 calc R . . H35B H 0.5483 0.9886 0.3955 0.101 Uiso 1 1 calc R . . C36 C 0.5853(3) 0.8913(4) 0.43275(16) 0.0690(16) Uani 1 1 d . . . H36A H 0.6412 0.9202 0.4443 0.083 Uiso 1 1 calc R . . H36B H 0.5286 0.9084 0.4474 0.083 Uiso 1 1 calc R . . C37 C 0.5723(2) 0.5840(3) 0.37522(8) 0.0393(9) Uani 1 1 d . . . C38 C 0.4819(2) 0.5494(3) 0.36711(8) 0.0322(7) Uani 1 1 d . . . C39 C 0.4637(3) 0.5131(3) 0.33216(9) 0.0386(9) Uani 1 1 d . . . H39 H 0.4013 0.4944 0.3258 0.046 Uiso 1 1 calc R . . C40 C 0.5372(3) 0.5047(3) 0.30692(10) 0.0437(10) Uani 1 1 d . . . H40 H 0.5244 0.4800 0.2832 0.052 Uiso 1 1 calc R . . C41 C 0.6295(3) 0.5317(3) 0.31551(10) 0.0409(10) Uani 1 1 d . . . C42 C 0.6472(2) 0.5737(3) 0.34936(10) 0.0448(10) Uani 1 1 d . . . C43 C 0.7462(3) 0.6091(4) 0.35919(11) 0.0539(12) Uani 1 1 d . . . H43A H 0.7460 0.6745 0.3571 0.065 Uiso 1 1 calc R . . H43B H 0.7607 0.5938 0.3852 0.065 Uiso 1 1 calc R . . C44 C 0.8237(3) 0.5719(4) 0.33449(11) 0.0531(12) Uani 1 1 d . . . H44A H 0.8373 0.5100 0.3418 0.064 Uiso 1 1 calc R . . H44B H 0.8826 0.6069 0.3379 0.064 Uiso 1 1 calc R . . C45 C 0.7948(3) 0.5742(4) 0.29382(11) 0.0586(13) Uani 1 1 d . . . H45A H 0.7792 0.6358 0.2866 0.070 Uiso 1 1 calc R . . H45B H 0.8486 0.5538 0.2783 0.070 Uiso 1 1 calc R . . C46 C 0.7093(3) 0.5153(4) 0.28730(11) 0.0570(12) Uani 1 1 d . . . H46A H 0.7295 0.4526 0.2888 0.068 Uiso 1 1 calc R . . H46B H 0.6845 0.5261 0.2621 0.068 Uiso 1 1 calc R . . C47 C 0.6754(4) 0.4804(5) 0.47441(14) 0.086(2) Uani 1 1 d . . . H47A H 0.7300 0.5114 0.4852 0.129 Uiso 1 1 calc R . . H47B H 0.6927 0.4186 0.4694 0.129 Uiso 1 1 calc R . . H47C H 0.6218 0.4821 0.4918 0.129 Uiso 1 1 calc R . . C48 C 0.4265(2) 0.5128(2) 0.42567(9) 0.0304(7) Uani 1 1 d . . . H48 H 0.4900 0.4943 0.4302 0.036 Uiso 1 1 calc R . . C49 C 0.3589(2) 0.5032(2) 0.45411(8) 0.0271(7) Uani 1 1 d . . . C50 C 0.3688(3) 0.4677(2) 0.48978(9) 0.0341(8) Uani 1 1 d . . . H50 H 0.4252 0.4439 0.5004 0.041 Uiso 1 1 calc R . . C51 C 0.2800(3) 0.4740(2) 0.50655(8) 0.0359(7) Uani 1 1 d . . . H51 H 0.2638 0.4548 0.5308 0.043 Uiso 1 1 calc R . . C52 C 0.2199(3) 0.5138(2) 0.48116(8) 0.0306(7) Uani 1 1 d . . . H52 H 0.1549 0.5270 0.4858 0.037 Uiso 1 1 calc R . . C53 C 0.0174(2) 0.8398(2) 0.40651(8) 0.0237(6) Uani 1 1 d . . . C54 C -0.0546(2) 0.8392(2) 0.43328(8) 0.0267(7) Uani 1 1 d . . . C55 C -0.1495(2) 0.8350(3) 0.42310(9) 0.0368(8) Uani 1 1 d . . . H55 H -0.1983 0.8341 0.4413 0.044 Uiso 1 1 calc R . . C56 C -0.1714(2) 0.8321(3) 0.38588(10) 0.0421(8) Uani 1 1 d . . . H56 H -0.2364 0.8286 0.3787 0.051 Uiso 1 1 calc R . . C57 C -0.1022(2) 0.8340(3) 0.35847(9) 0.0364(8) Uani 1 1 d . . . C58 C -0.0069(2) 0.8371(2) 0.36887(9) 0.0292(7) Uani 1 1 d . . . C59 C 0.0729(2) 0.8350(3) 0.34041(8) 0.0305(7) Uani 1 1 d . . . H59A H 0.1065 0.7775 0.3422 0.037 Uiso 1 1 calc R . . H59B H 0.1192 0.8823 0.3462 0.037 Uiso 1 1 calc R . . C60 C 0.0375(3) 0.8474(3) 0.30075(9) 0.0382(9) Uani 1 1 d . . . H60A H 0.0244 0.9109 0.2963 0.046 Uiso 1 1 calc R . . H60B H 0.0878 0.8285 0.2833 0.046 Uiso 1 1 calc R . . C61 C -0.0515(3) 0.7945(4) 0.29362(10) 0.0500(11) Uani 1 1 d . . . H61A H -0.0394 0.7311 0.2988 0.060 Uiso 1 1 calc R . . H61B H -0.0703 0.8004 0.2673 0.060 Uiso 1 1 calc R . . C62 C -0.1307(3) 0.8277(4) 0.31812(9) 0.0484(10) Uani 1 1 d . . . H62A H -0.1860 0.7874 0.3159 0.058 Uiso 1 1 calc R . . H62B H -0.1509 0.8870 0.3094 0.058 Uiso 1 1 calc R . . C63 C 0.1197(2) 0.8419(2) 0.41853(8) 0.0222(6) Uani 1 1 d . . . C64 C 0.1717(2) 0.7649(2) 0.42376(8) 0.0214(6) Uani 1 1 d . . . C65 C 0.2662(3) 0.7694(2) 0.43518(8) 0.0264(7) Uani 1 1 d . . . H65 H 0.3009 0.7164 0.4395 0.032 Uiso 1 1 calc R . . C66 C 0.3099(2) 0.8508(2) 0.44035(9) 0.0316(8) Uani 1 1 d . . . H66 H 0.3742 0.8529 0.4484 0.038 Uiso 1 1 calc R . . C67 C 0.2610(2) 0.9293(2) 0.43394(8) 0.0287(7) Uani 1 1 d . . . C68 C 0.1633(2) 0.9257(2) 0.42398(8) 0.0253(7) Uani 1 1 d . . . C69 C 0.1072(3) 1.0088(2) 0.41778(10) 0.0337(8) Uani 1 1 d . . . H69A H 0.0514 1.0081 0.4346 0.040 Uiso 1 1 calc R . . H69B H 0.0828 1.0083 0.3921 0.040 Uiso 1 1 calc R . . C70 C 0.1609(3) 1.0935(3) 0.42384(16) 0.0602(13) Uani 1 1 d . . . H70A H 0.1302 1.1413 0.4093 0.072 Uiso 1 1 calc R . . H70B H 0.1568 1.1099 0.4503 0.072 Uiso 1 1 calc R . . C71 C 0.2602(4) 1.0878(3) 0.41334(16) 0.0653(14) Uani 1 1 d . . . H71A H 0.2911 1.1460 0.4173 0.078 Uiso 1 1 calc R . . H71B H 0.2649 1.0731 0.3867 0.078 Uiso 1 1 calc R . . C72 C 0.3122(3) 1.0169(3) 0.43604(11) 0.0397(9) Uani 1 1 d . . . H72A H 0.3779 1.0099 0.4265 0.048 Uiso 1 1 calc R . . H72B H 0.3162 1.0362 0.4622 0.048 Uiso 1 1 calc R . . C73 C -0.0907(2) 0.8118(3) 0.49672(8) 0.0322(7) Uani 1 1 d . . . H73A H -0.1433 0.8544 0.4980 0.048 Uiso 1 1 calc R . . H73B H -0.0592 0.8082 0.5209 0.048 Uiso 1 1 calc R . . H73C H -0.1156 0.7534 0.4899 0.048 Uiso 1 1 calc R . . C74 C 0.0542(2) 0.6548(2) 0.43020(8) 0.0288(7) Uani 1 1 d . . . H74 H 0.0216 0.6938 0.4465 0.035 Uiso 1 1 calc R . . C75 C 0.0135(2) 0.5714(2) 0.42198(8) 0.0286(7) Uani 1 1 d . . . C76 C -0.0721(3) 0.5352(3) 0.43478(11) 0.0402(9) Uani 1 1 d . . . H76 H -0.1160 0.5613 0.4515 0.048 Uiso 1 1 calc R . . C77 C -0.0793(3) 0.4530(3) 0.41785(11) 0.0439(9) Uani 1 1 d . . . H77 H -0.1303 0.4122 0.4203 0.053 Uiso 1 1 calc R . . C78 C 0.0033(2) 0.4415(3) 0.39628(9) 0.0347(7) Uani 1 1 d . . . H78 H 0.0168 0.3900 0.3821 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02095(7) 0.02231(7) 0.02327(6) -0.00185(6) -0.00048(6) 0.00118(7) N1 0.0300(15) 0.0329(16) 0.0270(12) -0.0034(11) -0.0019(11) 0.0009(13) N2 0.0236(13) 0.0370(16) 0.0296(12) -0.0004(11) 0.0008(11) 0.0017(14) N3 0.0226(13) 0.0408(18) 0.0271(12) -0.0036(11) 0.0015(10) 0.0006(13) N4 0.0248(13) 0.0234(13) 0.0265(11) -0.0031(9) 0.0022(11) 0.0006(11) N5 0.0213(13) 0.0255(14) 0.0286(12) 0.0024(11) 0.0007(10) 0.0021(11) N6 0.0309(15) 0.0258(16) 0.0341(13) 0.0017(11) -0.0002(12) -0.0027(13) O1 0.0373(12) 0.0221(11) 0.0269(9) -0.0018(8) -0.0044(10) 0.0070(10) O2 0.0285(15) 0.109(3) 0.0391(15) 0.0112(16) -0.0037(12) -0.0115(17) O3 0.0228(11) 0.0352(14) 0.0273(10) 0.0005(9) 0.0049(9) 0.0011(10) C1 0.0243(16) 0.0330(18) 0.0347(15) -0.0135(13) -0.0036(14) 0.0012(16) C2 0.036(2) 0.0251(17) 0.0400(17) -0.0098(13) -0.0119(14) 0.0050(14) C3 0.035(2) 0.044(2) 0.058(2) -0.0232(18) -0.0220(17) 0.0149(18) C4 0.034(2) 0.065(3) 0.081(3) -0.039(3) -0.021(2) 0.019(2) C5 0.027(2) 0.080(4) 0.077(3) -0.052(3) -0.003(2) 0.007(2) C6 0.0236(18) 0.056(3) 0.049(2) -0.0246(18) -0.0022(16) -0.0067(18) C7 0.032(2) 0.089(4) 0.0398(19) -0.030(2) 0.0082(15) -0.011(2) C8 0.049(3) 0.148(6) 0.065(3) -0.052(4) 0.022(3) -0.022(4) C9 0.042(3) 0.174(7) 0.102(4) -0.100(5) 0.012(3) 0.000(4) C10 0.028(2) 0.146(6) 0.110(4) -0.082(4) 0.005(3) 0.010(3) C11 0.0246(17) 0.039(2) 0.0240(14) -0.0076(13) -0.0024(12) 0.0021(15) C12 0.0274(16) 0.038(2) 0.0234(13) -0.0023(14) -0.0013(11) -0.0051(16) C13 0.0277(16) 0.043(2) 0.0318(14) -0.0054(16) -0.0048(12) 0.0034(18) C14 0.0244(17) 0.056(3) 0.0286(16) -0.0092(15) -0.0053(13) -0.0005(17) C15 0.0288(18) 0.044(2) 0.0274(15) -0.0091(14) 0.0016(13) -0.0016(16) C16 0.0295(18) 0.038(2) 0.0221(14) -0.0080(13) -0.0015(13) 0.0003(15) C17 0.048(2) 0.031(2) 0.0436(19) -0.0130(16) -0.0044(16) -0.0010(18) C18 0.081(4) 0.044(3) 0.135(5) 0.026(3) -0.055(4) -0.023(3) C19 0.052(4) 0.051(4) 0.054(3) -0.007(3) -0.001(3) -0.024(3) C19' 0.052(4) 0.051(4) 0.054(3) -0.007(3) -0.001(3) -0.024(3) C20 0.039(2) 0.049(3) 0.0415(19) -0.0083(17) -0.0050(17) -0.0073(19) C21 0.050(2) 0.0230(17) 0.0407(17) 0.0050(13) -0.0019(17) -0.0014(18) C22 0.0300(17) 0.048(2) 0.0254(13) -0.0024(15) -0.0015(11) 0.0024(16) C23 0.0287(19) 0.045(2) 0.0283(15) 0.0012(14) 0.0008(13) 0.0004(15) C24 0.0371(19) 0.062(3) 0.0330(16) 0.0157(16) 0.0047(17) -0.004(2) C25 0.036(2) 0.043(2) 0.049(2) 0.0103(17) 0.0021(16) -0.0068(18) C26 0.0296(19) 0.031(2) 0.0465(19) -0.0011(15) 0.0015(14) -0.0065(15) C27 0.0203(18) 0.113(4) 0.0210(15) 0.0024(19) 0.0019(13) -0.011(2) C28 0.034(2) 0.087(4) 0.038(2) -0.001(2) 0.0042(17) -0.010(2) C29 0.029(2) 0.116(5) 0.0269(17) -0.001(2) -0.0010(14) -0.029(3) C30 0.044(3) 0.085(4) 0.050(2) -0.017(2) 0.012(2) -0.016(3) C31 0.029(2) 0.099(4) 0.053(2) -0.020(3) 0.0045(19) -0.018(2) C32 0.028(2) 0.081(4) 0.047(2) -0.020(2) 0.0140(17) -0.015(2) C33 0.033(2) 0.074(3) 0.060(2) -0.026(2) 0.0113(19) -0.007(2) C34 0.039(2) 0.072(4) 0.090(4) -0.027(3) 0.010(2) -0.012(2) C35 0.044(3) 0.090(5) 0.117(5) -0.046(4) 0.011(3) -0.011(3) C36 0.031(2) 0.075(4) 0.101(4) -0.040(3) 0.006(2) -0.011(2) C37 0.0242(16) 0.069(3) 0.0252(15) 0.0058(15) 0.0004(12) 0.0007(17) C38 0.0210(15) 0.048(2) 0.0276(14) 0.0014(15) 0.0032(12) 0.0061(16) C39 0.0293(19) 0.055(3) 0.0316(16) -0.0075(16) 0.0016(14) 0.0027(18) C40 0.040(2) 0.064(3) 0.0278(16) 0.0006(17) 0.0053(15) 0.006(2) C41 0.033(2) 0.056(3) 0.0331(17) 0.0096(16) 0.0082(15) 0.0156(18) C42 0.0264(17) 0.076(3) 0.0318(16) 0.0141(19) 0.0044(14) 0.0054(19) C43 0.027(2) 0.092(4) 0.0423(19) 0.012(2) 0.0057(15) -0.001(2) C44 0.0270(18) 0.080(4) 0.052(2) 0.018(2) 0.0096(17) 0.007(2) C45 0.035(2) 0.093(4) 0.048(2) 0.016(2) 0.0193(17) 0.012(2) C46 0.049(3) 0.084(3) 0.0370(18) 0.0087(19) 0.0149(18) 0.022(2) C47 0.051(3) 0.152(6) 0.055(3) 0.035(3) -0.013(2) -0.021(4) C48 0.0251(17) 0.035(2) 0.0308(15) -0.0048(14) 0.0003(13) -0.0009(15) C49 0.0300(17) 0.0261(17) 0.0252(14) -0.0020(12) 0.0002(12) 0.0002(14) C50 0.0299(18) 0.039(2) 0.0335(16) 0.0021(14) -0.0078(14) 0.0014(15) C51 0.044(2) 0.0369(18) 0.0270(14) 0.0031(12) 0.0050(16) -0.0038(18) C52 0.0312(17) 0.0324(18) 0.0283(14) -0.0026(12) 0.0060(15) -0.0001(17) C53 0.0202(15) 0.0211(16) 0.0298(14) 0.0030(12) 0.0007(12) 0.0019(13) C54 0.0211(15) 0.0304(19) 0.0287(14) -0.0032(13) 0.0000(12) 0.0028(14) C55 0.0202(16) 0.058(3) 0.0320(16) -0.0092(16) 0.0010(13) 0.0046(16) C56 0.0213(16) 0.067(3) 0.0381(16) -0.0001(19) 0.0007(16) 0.0021(17) C57 0.0261(17) 0.053(2) 0.0301(15) 0.0004(15) -0.0036(13) 0.0017(17) C58 0.0218(16) 0.035(2) 0.0310(15) -0.0001(13) 0.0014(12) 0.0009(15) C59 0.0258(16) 0.038(2) 0.0281(15) 0.0017(13) -0.0001(13) 0.0026(15) C60 0.040(2) 0.047(2) 0.0273(16) 0.0039(15) 0.0011(15) 0.0001(18) C61 0.039(2) 0.086(4) 0.0245(16) -0.0034(18) -0.0008(15) -0.006(2) C62 0.0312(19) 0.083(3) 0.0308(17) 0.0005(19) -0.0045(15) 0.001(2) C63 0.0199(15) 0.0247(17) 0.0220(13) -0.0022(11) 0.0018(11) 0.0038(13) C64 0.0240(16) 0.0203(16) 0.0200(13) 0.0007(11) 0.0029(12) -0.0003(13) C65 0.0228(16) 0.0256(16) 0.0307(14) 0.0023(11) -0.0014(14) 0.0055(14) C66 0.0193(16) 0.036(2) 0.0394(17) 0.0031(14) -0.0023(13) 0.0023(14) C67 0.0241(16) 0.0276(18) 0.0344(14) 0.0020(12) -0.0003(12) -0.0041(14) C68 0.0252(15) 0.0247(18) 0.0259(13) 0.0022(11) 0.0015(12) 0.0033(13) C69 0.041(2) 0.0244(19) 0.0362(17) 0.0044(14) -0.0006(15) 0.0013(16) C70 0.054(3) 0.025(2) 0.102(4) 0.009(2) -0.021(3) 0.004(2) C71 0.056(3) 0.035(2) 0.105(4) 0.001(2) -0.003(3) -0.007(2) C72 0.0317(19) 0.033(2) 0.055(2) 0.0036(17) -0.0027(17) -0.0035(16) C73 0.0278(17) 0.040(2) 0.0285(15) 0.0020(14) 0.0078(13) 0.0038(15) C74 0.0283(17) 0.0301(19) 0.0280(14) 0.0030(12) 0.0032(13) 0.0026(14) C75 0.0267(16) 0.0277(19) 0.0315(14) 0.0025(13) 0.0005(12) -0.0001(14) C76 0.0281(18) 0.045(3) 0.048(2) 0.0032(17) 0.0043(16) -0.0016(16) C77 0.0311(19) 0.039(2) 0.062(2) 0.0127(19) -0.0038(17) -0.0142(18) C78 0.0343(17) 0.0313(18) 0.0384(15) -0.0003(15) -0.0056(13) -0.0094(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N4 2.440(2) . ? Sm1 N2 2.445(3) . ? Sm1 N6 2.447(3) . ? Sm1 N5 2.491(3) . ? Sm1 N1 2.527(3) . ? Sm1 O1 2.568(2) . ? Sm1 N3 2.573(3) . ? N1 C22 1.299(4) . ? N1 C12 1.430(5) . ? N2 C26 1.361(5) . ? N2 C23 1.395(4) . ? N3 C48 1.302(4) . ? N3 C38 1.434(4) . ? N4 C52 1.356(4) . ? N4 C49 1.399(4) . ? N5 C74 1.302(4) . ? N5 C64 1.417(4) . ? N6 C78 1.359(5) . ? N6 C75 1.395(4) . ? O1 C2 1.380(4) . ? O1 C21 1.442(4) . ? O2 C28 1.387(6) . ? O2 C47 1.457(5) . ? O3 C54 1.382(4) . ? O3 C73 1.420(4) . ? C1 C6 1.395(5) . ? C1 C2 1.404(4) . ? C1 C11 1.506(5) . ? C2 C3 1.385(5) . ? C3 C4 1.367(6) . ? C3 H3 0.9500 . ? C4 C5 1.399(6) . ? C4 H4 0.9500 . ? C5 C6 1.401(6) . ? C5 C10 1.526(6) . ? C6 C7 1.524(5) . ? C7 C8 1.526(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.469(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.542(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.378(5) . ? C11 C16 1.394(5) . ? C12 C13 1.409(4) . ? C13 C14 1.376(5) . ? C13 H13 0.9500 . ? C14 C15 1.386(6) . ? C14 H14 0.9500 . ? C15 C16 1.403(5) . ? C15 C20 1.505(5) . ? C16 C17 1.508(5) . ? C17 C18 1.479(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.462(8) . ? C18 C19' 1.494(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9602 . ? C18 H18C 0.9600 . ? C18 H18D 0.9600 . ? C19 C20 1.550(8) . ? C19 H18C 1.4271 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 H20D 1.5481 . ? C19' C20 1.501(7) . ? C19' H18B 1.5033 . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C19' H20A 1.5137 . ? C20 H20A 0.9600 . ? C20 H20B 0.9601 . ? C20 H20C 0.9600 . ? C20 H20D 0.9600 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.410(5) . ? C22 H22 0.9500 . ? C23 C24 1.405(5) . ? C24 C25 1.365(6) . ? C24 H24 0.9500 . ? C25 C26 1.395(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.378(6) . ? C27 C32 1.381(7) . ? C27 C37 1.555(6) . ? C28 C29 1.407(6) . ? C29 C30 1.394(8) . ? C29 H29 0.9500 . ? C30 C31 1.328(7) . ? C30 H30 0.9500 . ? C31 C32 1.417(6) . ? C31 C36 1.495(8) . ? C32 C33 1.482(7) . ? C33 C34 1.536(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.516(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.502(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.404(5) . ? C37 C42 1.416(5) . ? C38 C39 1.400(5) . ? C39 C40 1.383(5) . ? C39 H39 0.9500 . ? C40 C41 1.395(6) . ? C40 H40 0.9500 . ? C41 C42 1.400(6) . ? C41 C46 1.535(5) . ? C42 C43 1.532(5) . ? C43 C44 1.515(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.525(6) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.512(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.407(4) . ? C48 H48 0.9500 . ? C49 C50 1.403(4) . ? C50 C51 1.390(5) . ? C50 H50 0.9500 . ? C51 C52 1.384(5) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.400(4) . ? C53 C58 1.403(4) . ? C53 C63 1.502(4) . ? C54 C55 1.384(5) . ? C55 C56 1.381(5) . ? C55 H55 0.9500 . ? C56 C57 1.388(5) . ? C56 H56 0.9500 . ? C57 C58 1.391(5) . ? C57 C62 1.515(5) . ? C58 C59 1.522(4) . ? C59 C60 1.528(4) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.506(6) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.508(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.385(4) . ? C63 C68 1.419(4) . ? C64 C65 1.392(4) . ? C65 C66 1.386(5) . ? C65 H65 0.9500 . ? C66 C67 1.389(5) . ? C66 H66 0.9500 . ? C67 C68 1.420(4) . ? C67 C72 1.508(5) . ? C68 C69 1.497(5) . ? C69 C70 1.501(6) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.448(7) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.533(6) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C75 1.414(5) . ? C74 H74 0.9500 . ? C75 C76 1.400(5) . ? C76 C77 1.386(6) . ? C76 H76 0.9500 . ? C77 C78 1.408(5) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Sm1 N2 135.48(9) . . ? N4 Sm1 N6 88.38(9) . . ? N2 Sm1 N6 124.01(9) . . ? N4 Sm1 N5 78.45(8) . . ? N2 Sm1 N5 85.81(9) . . ? N6 Sm1 N5 68.71(9) . . ? N4 Sm1 N1 152.90(9) . . ? N2 Sm1 N1 67.88(9) . . ? N6 Sm1 N1 85.02(9) . . ? N5 Sm1 N1 122.75(9) . . ? N4 Sm1 O1 76.93(7) . . ? N2 Sm1 O1 135.31(8) . . ? N6 Sm1 O1 76.12(9) . . ? N5 Sm1 O1 137.20(8) . . ? N1 Sm1 O1 75.98(8) . . ? N4 Sm1 N3 68.39(9) . . ? N2 Sm1 N3 84.57(9) . . ? N6 Sm1 N3 151.41(10) . . ? N5 Sm1 N3 119.53(9) . . ? N1 Sm1 N3 107.88(9) . . ? O1 Sm1 N3 82.33(9) . . ? C22 N1 C12 119.2(3) . . ? C22 N1 Sm1 114.8(2) . . ? C12 N1 Sm1 123.22(19) . . ? C26 N2 C23 104.9(3) . . ? C26 N2 Sm1 139.1(2) . . ? C23 N2 Sm1 115.9(2) . . ? C48 N3 C38 116.0(3) . . ? C48 N3 Sm1 111.6(2) . . ? C38 N3 Sm1 130.57(19) . . ? C52 N4 C49 105.2(3) . . ? C52 N4 Sm1 138.5(2) . . ? C49 N4 Sm1 113.75(18) . . ? C74 N5 C64 119.9(3) . . ? C74 N5 Sm1 114.4(2) . . ? C64 N5 Sm1 125.1(2) . . ? C78 N6 C75 104.3(3) . . ? C78 N6 Sm1 140.7(2) . . ? C75 N6 Sm1 113.7(2) . . ? C2 O1 C21 114.2(3) . . ? C2 O1 Sm1 117.53(19) . . ? C21 O1 Sm1 123.60(18) . . ? C28 O2 C47 117.3(4) . . ? C54 O3 C73 116.6(3) . . ? C6 C1 C2 119.7(3) . . ? C6 C1 C11 120.4(3) . . ? C2 C1 C11 119.9(3) . . ? O1 C2 C3 121.7(3) . . ? O1 C2 C1 117.7(3) . . ? C3 C2 C1 120.5(3) . . ? C4 C3 C2 119.1(4) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 122.1(4) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C4 C5 C6 118.8(4) . . ? C4 C5 C10 119.4(4) . . ? C6 C5 C10 121.8(4) . . ? C1 C6 C5 119.5(4) . . ? C1 C6 C7 119.1(3) . . ? C5 C6 C7 121.4(3) . . ? C6 C7 C8 113.4(4) . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C7 113.4(5) . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C8 C9 C10 111.2(5) . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C5 C10 C9 111.9(4) . . ? C5 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? C5 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C16 120.5(3) . . ? C12 C11 C1 120.1(3) . . ? C16 C11 C1 119.4(3) . . ? C11 C12 C13 119.6(3) . . ? C11 C12 N1 120.6(3) . . ? C13 C12 N1 119.6(4) . . ? C14 C13 C12 119.6(4) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 121.5(3) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C14 C15 C16 118.9(3) . . ? C14 C15 C20 118.6(3) . . ? C16 C15 C20 122.6(4) . . ? C11 C16 C15 120.0(3) . . ? C11 C16 C17 119.6(3) . . ? C15 C16 C17 120.4(3) . . ? C18 C17 C16 115.7(4) . . ? C18 C17 H17A 108.4 . . ? C16 C17 H17A 108.4 . . ? C18 C17 H17B 108.4 . . ? C16 C17 H17B 108.4 . . ? H17A C17 H17B 107.4 . . ? C19 C18 C17 123.7(6) . . ? C19 C18 C19' 40.2(5) . . ? C17 C18 C19' 114.0(5) . . ? C19 C18 H18A 106.4 . . ? C17 C18 H18A 107.2 . . ? C19' C18 H18A 137.4 . . ? C19 C18 H18B 105.5 . . ? C17 C18 H18B 106.2 . . ? C19' C18 H18B 71.9 . . ? H18A C18 H18B 106.8 . . ? C19 C18 H18C 68.6 . . ? C17 C18 H18C 109.7 . . ? C19' C18 H18C 108.5 . . ? H18A C18 H18C 44.8 . . ? H18B C18 H18C 139.6 . . ? C19 C18 H18D 126.4 . . ? C17 C18 H18D 108.2 . . ? C19' C18 H18D 108.5 . . ? H18A C18 H18D 66.2 . . ? H18B C18 H18D 41.9 . . ? H18C C18 H18D 107.8 . . ? C18 C19 C20 112.4(6) . . ? C18 C19 H18C 38.8 . . ? C20 C19 H18C 133.7 . . ? C18 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? H18C C19 H19A 71.1 . . ? C18 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H18C C19 H19B 114.8 . . ? H19A C19 H19B 107.8 . . ? C18 C19 H20D 137.2 . . ? C20 C19 H20D 36.1 . . ? H18C C19 H20D 130.2 . . ? H19A C19 H20D 75.1 . . ? H19B C19 H20D 109.6 . . ? C18 C19' C20 113.5(5) . . ? C18 C19' H18B 37.4 . . ? C20 C19' H18B 145.4 . . ? C18 C19' H19C 108.9 . . ? C20 C19' H19C 108.9 . . ? H18B C19' H19C 100.9 . . ? C18 C19' H19D 108.9 . . ? C20 C19' H19D 108.9 . . ? H18B C19' H19D 77.3 . . ? H19C C19' H19D 107.7 . . ? C18 C19' H20A 142.4 . . ? C20 C19' H20A 37.1 . . ? H18B C19' H20A 147.2 . . ? H19C C19' H20A 104.7 . . ? H19D C19' H20A 75.6 . . ? C19' C20 C15 111.8(4) . . ? C19' C20 C19 38.9(5) . . ? C15 C20 C19 114.3(5) . . ? C19' C20 H20A 72.2 . . ? C15 C20 H20A 108.5 . . ? C19 C20 H20A 107.6 . . ? C19' C20 H20B 136.9 . . ? C15 C20 H20B 108.8 . . ? C19 C20 H20B 109.8 . . ? H20A C20 H20B 107.6 . . ? C19' C20 H20C 109.7 . . ? C15 C20 H20C 109.1 . . ? C19 C20 H20C 133.9 . . ? H20A C20 H20C 41.4 . . ? H20B C20 H20C 68.5 . . ? C19' C20 H20D 108.8 . . ? C15 C20 H20D 109.5 . . ? C19 C20 H20D 71.9 . . ? H20A C20 H20D 138.0 . . ? H20B C20 H20D 42.2 . . ? H20C C20 H20D 107.9 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C23 121.9(3) . . ? N1 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? N2 C23 C24 109.5(3) . . ? N2 C23 C22 118.9(3) . . ? C24 C23 C22 131.6(3) . . ? C25 C24 C23 107.3(3) . . ? C25 C24 H24 126.3 . . ? C23 C24 H24 126.3 . . ? C24 C25 C26 106.7(3) . . ? C24 C25 H25 126.6 . . ? C26 C25 H25 126.6 . . ? N2 C26 C25 111.4(3) . . ? N2 C26 H26 124.3 . . ? C25 C26 H26 124.3 . . ? C28 C27 C32 118.4(5) . . ? C28 C27 C37 121.2(5) . . ? C32 C27 C37 120.3(4) . . ? C27 C28 O2 113.0(4) . . ? C27 C28 C29 121.8(6) . . ? O2 C28 C29 125.1(5) . . ? C30 C29 C28 117.3(4) . . ? C30 C29 H29 121.3 . . ? C28 C29 H29 121.3 . . ? C31 C30 C29 122.3(5) . . ? C31 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C30 C31 C32 119.7(6) . . ? C30 C31 C36 118.7(5) . . ? C32 C31 C36 121.5(5) . . ? C27 C32 C31 120.4(5) . . ? C27 C32 C33 119.1(4) . . ? C31 C32 C33 120.4(5) . . ? C32 C33 C34 114.5(4) . . ? C32 C33 H33A 108.6 . . ? C34 C33 H33A 108.6 . . ? C32 C33 H33B 108.6 . . ? C34 C33 H33B 108.6 . . ? H33A C33 H33B 107.6 . . ? C35 C34 C33 112.4(5) . . ? C35 C34 H34A 109.1 . . ? C33 C34 H34A 109.1 . . ? C35 C34 H34B 109.1 . . ? C33 C34 H34B 109.1 . . ? H34A C34 H34B 107.9 . . ? C36 C35 C34 109.7(5) . . ? C36 C35 H35A 109.7 . . ? C34 C35 H35A 109.7 . . ? C36 C35 H35B 109.7 . . ? C34 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C31 C36 C35 116.1(4) . . ? C31 C36 H36A 108.3 . . ? C35 C36 H36A 108.3 . . ? C31 C36 H36B 108.3 . . ? C35 C36 H36B 108.3 . . ? H36A C36 H36B 107.4 . . ? C38 C37 C42 119.5(3) . . ? C38 C37 C27 122.9(3) . . ? C42 C37 C27 116.9(3) . . ? C39 C38 C37 119.9(3) . . ? C39 C38 N3 116.7(3) . . ? C37 C38 N3 123.4(3) . . ? C40 C39 C38 119.7(4) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 121.4(4) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C40 C41 C42 119.4(3) . . ? C40 C41 C46 119.0(4) . . ? C42 C41 C46 121.6(4) . . ? C41 C42 C37 119.7(3) . . ? C41 C42 C43 121.4(3) . . ? C37 C42 C43 118.9(3) . . ? C44 C43 C42 112.7(4) . . ? C44 C43 H43A 109.0 . . ? C42 C43 H43A 109.0 . . ? C44 C43 H43B 109.0 . . ? C42 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C43 C44 C45 111.6(3) . . ? C43 C44 H44A 109.3 . . ? C45 C44 H44A 109.3 . . ? C43 C44 H44B 109.3 . . ? C45 C44 H44B 109.3 . . ? H44A C44 H44B 108.0 . . ? C46 C45 C44 110.4(3) . . ? C46 C45 H45A 109.6 . . ? C44 C45 H45A 109.6 . . ? C46 C45 H45B 109.6 . . ? C44 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? C45 C46 C41 112.4(4) . . ? C45 C46 H46A 109.1 . . ? C41 C46 H46A 109.1 . . ? C45 C46 H46B 109.1 . . ? C41 C46 H46B 109.1 . . ? H46A C46 H46B 107.8 . . ? O2 C47 H47A 109.5 . . ? O2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N3 C48 C49 122.8(3) . . ? N3 C48 H48 118.6 . . ? C49 C48 H48 118.6 . . ? N4 C49 C50 109.6(3) . . ? N4 C49 C48 120.3(3) . . ? C50 C49 C48 130.1(3) . . ? C51 C50 C49 106.6(3) . . ? C51 C50 H50 126.7 . . ? C49 C50 H50 126.7 . . ? C52 C51 C50 106.8(3) . . ? C52 C51 H51 126.6 . . ? C50 C51 H51 126.6 . . ? N4 C52 C51 111.8(3) . . ? N4 C52 H52 124.1 . . ? C51 C52 H52 124.1 . . ? C54 C53 C58 119.6(3) . . ? C54 C53 C63 119.5(3) . . ? C58 C53 C63 121.0(3) . . ? O3 C54 C55 123.5(3) . . ? O3 C54 C53 115.6(3) . . ? C55 C54 C53 120.8(3) . . ? C56 C55 C54 118.4(3) . . ? C56 C55 H55 120.8 . . ? C54 C55 H55 120.8 . . ? C55 C56 C57 122.5(3) . . ? C55 C56 H56 118.7 . . ? C57 C56 H56 118.7 . . ? C56 C57 C58 118.8(3) . . ? C56 C57 C62 120.0(3) . . ? C58 C57 C62 121.1(3) . . ? C57 C58 C53 119.8(3) . . ? C57 C58 C59 121.7(3) . . ? C53 C58 C59 118.4(3) . . ? C58 C59 C60 113.0(3) . . ? C58 C59 H59A 109.0 . . ? C60 C59 H59A 109.0 . . ? C58 C59 H59B 109.0 . . ? C60 C59 H59B 109.0 . . ? H59A C59 H59B 107.8 . . ? C61 C60 C59 111.5(3) . . ? C61 C60 H60A 109.3 . . ? C59 C60 H60A 109.3 . . ? C61 C60 H60B 109.3 . . ? C59 C60 H60B 109.3 . . ? H60A C60 H60B 108.0 . . ? C60 C61 C62 109.6(4) . . ? C60 C61 H61A 109.7 . . ? C62 C61 H61A 109.7 . . ? C60 C61 H61B 109.7 . . ? C62 C61 H61B 109.7 . . ? H61A C61 H61B 108.2 . . ? C61 C62 C57 113.0(3) . . ? C61 C62 H62A 109.0 . . ? C57 C62 H62A 109.0 . . ? C61 C62 H62B 109.0 . . ? C57 C62 H62B 109.0 . . ? H62A C62 H62B 107.8 . . ? C64 C63 C68 120.1(3) . . ? C64 C63 C53 121.7(3) . . ? C68 C63 C53 118.1(3) . . ? C63 C64 C65 120.2(3) . . ? C63 C64 N5 123.1(3) . . ? C65 C64 N5 116.6(3) . . ? C66 C65 C64 120.3(3) . . ? C66 C65 H65 119.8 . . ? C64 C65 H65 119.8 . . ? C65 C66 C67 121.0(3) . . ? C65 C66 H66 119.5 . . ? C67 C66 H66 119.5 . . ? C66 C67 C68 119.2(3) . . ? C66 C67 C72 120.3(3) . . ? C68 C67 C72 120.5(3) . . ? C63 C68 C67 119.0(3) . . ? C63 C68 C69 119.9(3) . . ? C67 C68 C69 121.0(3) . . ? C68 C69 C70 115.3(3) . . ? C68 C69 H69A 108.5 . . ? C70 C69 H69A 108.5 . . ? C68 C69 H69B 108.5 . . ? C70 C69 H69B 108.5 . . ? H69A C69 H69B 107.5 . . ? C71 C70 C69 113.3(4) . . ? C71 C70 H70A 108.9 . . ? C69 C70 H70A 108.9 . . ? C71 C70 H70B 108.9 . . ? C69 C70 H70B 108.9 . . ? H70A C70 H70B 107.7 . . ? C70 C71 C72 111.1(4) . . ? C70 C71 H71A 109.4 . . ? C72 C71 H71A 109.4 . . ? C70 C71 H71B 109.4 . . ? C72 C71 H71B 109.4 . . ? H71A C71 H71B 108.0 . . ? C67 C72 C71 111.0(3) . . ? C67 C72 H72A 109.4 . . ? C71 C72 H72A 109.4 . . ? C67 C72 H72B 109.4 . . ? C71 C72 H72B 109.4 . . ? H72A C72 H72B 108.0 . . ? O3 C73 H73A 109.5 . . ? O3 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? O3 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N5 C74 C75 121.6(3) . . ? N5 C74 H74 119.2 . . ? C75 C74 H74 119.2 . . ? N6 C75 C76 111.7(3) . . ? N6 C75 C74 119.6(3) . . ? C76 C75 C74 128.7(3) . . ? C77 C76 C75 105.4(3) . . ? C77 C76 H76 127.3 . . ? C75 C76 H76 127.3 . . ? C76 C77 C78 107.2(3) . . ? C76 C77 H77 126.4 . . ? C78 C77 H77 126.4 . . ? N6 C78 C77 111.4(4) . . ? N6 C78 H78 124.3 . . ? C77 C78 H78 124.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Sm1 N1 C22 -159.5(2) . . . . ? N2 Sm1 N1 C22 -5.9(2) . . . . ? N6 Sm1 N1 C22 124.0(2) . . . . ? N5 Sm1 N1 C22 63.3(3) . . . . ? O1 Sm1 N1 C22 -159.1(3) . . . . ? N3 Sm1 N1 C22 -82.1(3) . . . . ? N4 Sm1 N1 C12 39.5(4) . . . . ? N2 Sm1 N1 C12 -167.0(3) . . . . ? N6 Sm1 N1 C12 -37.1(3) . . . . ? N5 Sm1 N1 C12 -97.8(3) . . . . ? O1 Sm1 N1 C12 39.8(2) . . . . ? N3 Sm1 N1 C12 116.8(3) . . . . ? N4 Sm1 N2 C26 -16.6(4) . . . . ? N6 Sm1 N2 C26 113.0(3) . . . . ? N5 Sm1 N2 C26 52.3(4) . . . . ? N1 Sm1 N2 C26 -179.8(4) . . . . ? O1 Sm1 N2 C26 -141.3(3) . . . . ? N3 Sm1 N2 C26 -68.0(4) . . . . ? N4 Sm1 N2 C23 165.6(2) . . . . ? N6 Sm1 N2 C23 -64.8(3) . . . . ? N5 Sm1 N2 C23 -125.5(2) . . . . ? N1 Sm1 N2 C23 2.5(2) . . . . ? O1 Sm1 N2 C23 40.9(3) . . . . ? N3 Sm1 N2 C23 114.3(2) . . . . ? N4 Sm1 N3 C48 14.0(2) . . . . ? N2 Sm1 N3 C48 157.9(2) . . . . ? N6 Sm1 N3 C48 -23.8(4) . . . . ? N5 Sm1 N3 C48 75.8(3) . . . . ? N1 Sm1 N3 C48 -137.5(2) . . . . ? O1 Sm1 N3 C48 -65.0(2) . . . . ? N4 Sm1 N3 C38 177.5(3) . . . . ? N2 Sm1 N3 C38 -38.6(3) . . . . ? N6 Sm1 N3 C38 139.7(3) . . . . ? N5 Sm1 N3 C38 -120.7(3) . . . . ? N1 Sm1 N3 C38 26.1(3) . . . . ? O1 Sm1 N3 C38 98.6(3) . . . . ? N2 Sm1 N4 C52 130.3(3) . . . . ? N6 Sm1 N4 C52 -10.0(3) . . . . ? N5 Sm1 N4 C52 58.6(3) . . . . ? N1 Sm1 N4 C52 -85.7(4) . . . . ? O1 Sm1 N4 C52 -86.1(3) . . . . ? N3 Sm1 N4 C52 -172.9(3) . . . . ? N2 Sm1 N4 C49 -71.3(2) . . . . ? N6 Sm1 N4 C49 148.4(2) . . . . ? N5 Sm1 N4 C49 -143.0(2) . . . . ? N1 Sm1 N4 C49 72.7(3) . . . . ? O1 Sm1 N4 C49 72.3(2) . . . . ? N3 Sm1 N4 C49 -14.5(2) . . . . ? N4 Sm1 N5 C74 -81.0(2) . . . . ? N2 Sm1 N5 C74 140.8(2) . . . . ? N6 Sm1 N5 C74 11.8(2) . . . . ? N1 Sm1 N5 C74 80.6(2) . . . . ? O1 Sm1 N5 C74 -25.1(3) . . . . ? N3 Sm1 N5 C74 -137.8(2) . . . . ? N4 Sm1 N5 C64 89.6(2) . . . . ? N2 Sm1 N5 C64 -48.5(2) . . . . ? N6 Sm1 N5 C64 -177.6(2) . . . . ? N1 Sm1 N5 C64 -108.8(2) . . . . ? O1 Sm1 N5 C64 145.5(2) . . . . ? N3 Sm1 N5 C64 32.8(3) . . . . ? N4 Sm1 N6 C78 -97.2(4) . . . . ? N2 Sm1 N6 C78 115.6(3) . . . . ? N5 Sm1 N6 C78 -175.4(4) . . . . ? N1 Sm1 N6 C78 56.5(3) . . . . ? O1 Sm1 N6 C78 -20.2(3) . . . . ? N3 Sm1 N6 C78 -62.4(4) . . . . ? N4 Sm1 N6 C75 67.1(2) . . . . ? N2 Sm1 N6 C75 -80.2(2) . . . . ? N5 Sm1 N6 C75 -11.2(2) . . . . ? N1 Sm1 N6 C75 -139.2(2) . . . . ? O1 Sm1 N6 C75 144.0(2) . . . . ? N3 Sm1 N6 C75 101.8(3) . . . . ? N4 Sm1 O1 C2 -123.8(2) . . . . ? N2 Sm1 O1 C2 19.9(3) . . . . ? N6 Sm1 O1 C2 144.6(2) . . . . ? N5 Sm1 O1 C2 179.75(19) . . . . ? N1 Sm1 O1 C2 56.3(2) . . . . ? N3 Sm1 O1 C2 -54.3(2) . . . . ? N4 Sm1 O1 C21 30.5(3) . . . . ? N2 Sm1 O1 C21 174.2(2) . . . . ? N6 Sm1 O1 C21 -61.1(3) . . . . ? N5 Sm1 O1 C21 -25.9(3) . . . . ? N1 Sm1 O1 C21 -149.3(3) . . . . ? N3 Sm1 O1 C21 100.0(3) . . . . ? C21 O1 C2 C3 -59.4(5) . . . . ? Sm1 O1 C2 C3 97.3(4) . . . . ? C21 O1 C2 C1 123.9(3) . . . . ? Sm1 O1 C2 C1 -79.4(3) . . . . ? C6 C1 C2 O1 169.2(3) . . . . ? C11 C1 C2 O1 -13.2(5) . . . . ? C6 C1 C2 C3 -7.5(6) . . . . ? C11 C1 C2 C3 170.1(4) . . . . ? O1 C2 C3 C4 -172.9(4) . . . . ? C1 C2 C3 C4 3.7(6) . . . . ? C2 C3 C4 C5 1.2(8) . . . . ? C3 C4 C5 C6 -2.1(8) . . . . ? C3 C4 C5 C10 175.8(5) . . . . ? C2 C1 C6 C5 6.5(6) . . . . ? C11 C1 C6 C5 -171.1(4) . . . . ? C2 C1 C6 C7 -174.2(4) . . . . ? C11 C1 C6 C7 8.3(6) . . . . ? C4 C5 C6 C1 -1.8(7) . . . . ? C10 C5 C6 C1 -179.7(5) . . . . ? C4 C5 C6 C7 178.9(5) . . . . ? C10 C5 C6 C7 1.0(8) . . . . ? C1 C6 C7 C8 169.6(5) . . . . ? C5 C6 C7 C8 -11.1(7) . . . . ? C6 C7 C8 C9 41.3(7) . . . . ? C7 C8 C9 C10 -60.8(7) . . . . ? C4 C5 C10 C9 163.0(6) . . . . ? C6 C5 C10 C9 -19.1(9) . . . . ? C8 C9 C10 C5 48.3(8) . . . . ? C6 C1 C11 C12 -101.9(4) . . . . ? C2 C1 C11 C12 80.5(4) . . . . ? C6 C1 C11 C16 77.0(5) . . . . ? C2 C1 C11 C16 -100.6(4) . . . . ? C16 C11 C12 C13 -1.8(5) . . . . ? C1 C11 C12 C13 177.1(3) . . . . ? C16 C11 C12 N1 173.0(3) . . . . ? C1 C11 C12 N1 -8.1(4) . . . . ? C22 N1 C12 C11 127.3(3) . . . . ? Sm1 N1 C12 C11 -72.5(3) . . . . ? C22 N1 C12 C13 -57.9(4) . . . . ? Sm1 N1 C12 C13 102.3(3) . . . . ? C11 C12 C13 C14 1.0(5) . . . . ? N1 C12 C13 C14 -173.9(3) . . . . ? C12 C13 C14 C15 0.1(5) . . . . ? C13 C14 C15 C16 -0.5(5) . . . . ? C13 C14 C15 C20 -179.5(3) . . . . ? C12 C11 C16 C15 1.5(5) . . . . ? C1 C11 C16 C15 -177.5(3) . . . . ? C12 C11 C16 C17 -177.8(3) . . . . ? C1 C11 C16 C17 3.3(5) . . . . ? C14 C15 C16 C11 -0.3(5) . . . . ? C20 C15 C16 C11 178.7(3) . . . . ? C14 C15 C16 C17 179.0(3) . . . . ? C20 C15 C16 C17 -2.0(5) . . . . ? C11 C16 C17 C18 173.3(4) . . . . ? C15 C16 C17 C18 -6.0(5) . . . . ? C16 C17 C18 C19 -10.9(9) . . . . ? C16 C17 C18 C19' 34.0(7) . . . . ? C17 C18 C19 C20 32.7(11) . . . . ? C19' C18 C19 C20 -55.5(6) . . . . ? C19 C18 C19' C20 59.1(7) . . . . ? C17 C18 C19' C20 -55.3(8) . . . . ? C18 C19' C20 C15 45.7(7) . . . . ? C18 C19' C20 C19 -56.4(6) . . . . ? C14 C15 C20 C19' 161.2(4) . . . . ? C16 C15 C20 C19' -17.9(5) . . . . ? C14 C15 C20 C19 -156.5(5) . . . . ? C16 C15 C20 C19 24.5(7) . . . . ? C18 C19 C20 C19' 57.5(7) . . . . ? C18 C19 C20 C15 -37.7(9) . . . . ? C12 N1 C22 C23 171.0(3) . . . . ? Sm1 N1 C22 C23 9.1(4) . . . . ? C26 N2 C23 C24 1.1(4) . . . . ? Sm1 N2 C23 C24 179.6(2) . . . . ? C26 N2 C23 C22 -177.6(3) . . . . ? Sm1 N2 C23 C22 0.9(4) . . . . ? N1 C22 C23 N2 -7.1(5) . . . . ? N1 C22 C23 C24 174.5(4) . . . . ? N2 C23 C24 C25 -0.5(5) . . . . ? C22 C23 C24 C25 178.1(4) . . . . ? C23 C24 C25 C26 -0.4(5) . . . . ? C23 N2 C26 C25 -1.4(4) . . . . ? Sm1 N2 C26 C25 -179.3(3) . . . . ? C24 C25 C26 N2 1.1(5) . . . . ? C32 C27 C28 O2 -176.1(4) . . . . ? C37 C27 C28 O2 0.4(5) . . . . ? C32 C27 C28 C29 1.2(6) . . . . ? C37 C27 C28 C29 177.8(3) . . . . ? C47 O2 C28 C27 -171.4(4) . . . . ? C47 O2 C28 C29 11.4(6) . . . . ? C27 C28 C29 C30 -1.3(6) . . . . ? O2 C28 C29 C30 175.7(4) . . . . ? C28 C29 C30 C31 0.0(6) . . . . ? C29 C30 C31 C32 1.2(7) . . . . ? C29 C30 C31 C36 -177.2(4) . . . . ? C28 C27 C32 C31 0.0(6) . . . . ? C37 C27 C32 C31 -176.6(3) . . . . ? C28 C27 C32 C33 175.9(4) . . . . ? C37 C27 C32 C33 -0.7(6) . . . . ? C30 C31 C32 C27 -1.2(6) . . . . ? C36 C31 C32 C27 177.1(4) . . . . ? C30 C31 C32 C33 -177.0(4) . . . . ? C36 C31 C32 C33 1.3(6) . . . . ? C27 C32 C33 C34 168.3(4) . . . . ? C31 C32 C33 C34 -15.9(5) . . . . ? C32 C33 C34 C35 44.8(6) . . . . ? C33 C34 C35 C36 -58.1(6) . . . . ? C30 C31 C36 C35 162.5(4) . . . . ? C32 C31 C36 C35 -15.9(6) . . . . ? C34 C35 C36 C31 43.5(6) . . . . ? C28 C27 C37 C38 99.2(5) . . . . ? C32 C27 C37 C38 -84.3(5) . . . . ? C28 C27 C37 C42 -90.0(5) . . . . ? C32 C27 C37 C42 86.4(5) . . . . ? C42 C37 C38 C39 -6.6(6) . . . . ? C27 C37 C38 C39 163.9(4) . . . . ? C42 C37 C38 N3 171.4(4) . . . . ? C27 C37 C38 N3 -18.1(6) . . . . ? C48 N3 C38 C39 128.5(4) . . . . ? Sm1 N3 C38 C39 -34.4(5) . . . . ? C48 N3 C38 C37 -49.5(5) . . . . ? Sm1 N3 C38 C37 147.6(3) . . . . ? C37 C38 C39 C40 5.5(6) . . . . ? N3 C38 C39 C40 -172.5(4) . . . . ? C38 C39 C40 C41 0.0(7) . . . . ? C39 C40 C41 C42 -4.4(6) . . . . ? C39 C40 C41 C46 176.2(4) . . . . ? C40 C41 C42 C37 3.3(6) . . . . ? C46 C41 C42 C37 -177.3(4) . . . . ? C40 C41 C42 C43 -176.6(4) . . . . ? C46 C41 C42 C43 2.7(6) . . . . ? C38 C37 C42 C41 2.1(6) . . . . ? C27 C37 C42 C41 -169.0(4) . . . . ? C38 C37 C42 C43 -177.9(4) . . . . ? C27 C37 C42 C43 11.0(6) . . . . ? C41 C42 C43 C44 -15.9(6) . . . . ? C37 C42 C43 C44 164.1(4) . . . . ? C42 C43 C44 C45 45.6(6) . . . . ? C43 C44 C45 C46 -63.5(6) . . . . ? C44 C45 C46 C41 48.4(5) . . . . ? C40 C41 C46 C45 160.0(4) . . . . ? C42 C41 C46 C45 -19.4(6) . . . . ? C38 N3 C48 C49 -178.5(3) . . . . ? Sm1 N3 C48 C49 -12.3(4) . . . . ? C52 N4 C49 C50 0.5(4) . . . . ? Sm1 N4 C49 C50 -164.9(2) . . . . ? C52 N4 C49 C48 -179.4(3) . . . . ? Sm1 N4 C49 C48 15.3(4) . . . . ? N3 C48 C49 N4 -1.4(5) . . . . ? N3 C48 C49 C50 178.8(4) . . . . ? N4 C49 C50 C51 0.2(4) . . . . ? C48 C49 C50 C51 -180.0(4) . . . . ? C49 C50 C51 C52 -0.8(4) . . . . ? C49 N4 C52 C51 -1.0(4) . . . . ? Sm1 N4 C52 C51 158.5(2) . . . . ? C50 C51 C52 N4 1.2(4) . . . . ? C73 O3 C54 C55 17.1(5) . . . . ? C73 O3 C54 C53 -160.8(3) . . . . ? C58 C53 C54 O3 178.7(3) . . . . ? C63 C53 C54 O3 -0.3(5) . . . . ? C58 C53 C54 C55 0.7(6) . . . . ? C63 C53 C54 C55 -178.3(3) . . . . ? O3 C54 C55 C56 -178.3(4) . . . . ? C53 C54 C55 C56 -0.5(6) . . . . ? C54 C55 C56 C57 -0.5(6) . . . . ? C55 C56 C57 C58 1.3(6) . . . . ? C55 C56 C57 C62 178.1(4) . . . . ? C56 C57 C58 C53 -1.1(6) . . . . ? C62 C57 C58 C53 -177.8(4) . . . . ? C56 C57 C58 C59 177.1(4) . . . . ? C62 C57 C58 C59 0.3(6) . . . . ? C54 C53 C58 C57 0.1(6) . . . . ? C63 C53 C58 C57 179.1(3) . . . . ? C54 C53 C58 C59 -178.1(3) . . . . ? C63 C53 C58 C59 0.9(5) . . . . ? C57 C58 C59 C60 11.2(5) . . . . ? C53 C58 C59 C60 -170.6(3) . . . . ? C58 C59 C60 C61 -42.8(5) . . . . ? C59 C60 C61 C62 63.4(5) . . . . ? C60 C61 C62 C57 -50.7(5) . . . . ? C56 C57 C62 C61 -157.0(4) . . . . ? C58 C57 C62 C61 19.8(6) . . . . ? C54 C53 C63 C64 91.7(4) . . . . ? C58 C53 C63 C64 -87.3(4) . . . . ? C54 C53 C63 C68 -89.3(4) . . . . ? C58 C53 C63 C68 91.8(4) . . . . ? C68 C63 C64 C65 1.4(4) . . . . ? C53 C63 C64 C65 -179.5(3) . . . . ? C68 C63 C64 N5 -174.8(3) . . . . ? C53 C63 C64 N5 4.2(4) . . . . ? C74 N5 C64 C63 -52.8(4) . . . . ? Sm1 N5 C64 C63 137.0(2) . . . . ? C74 N5 C64 C65 130.8(3) . . . . ? Sm1 N5 C64 C65 -39.4(3) . . . . ? C63 C64 C65 C66 -1.9(4) . . . . ? N5 C64 C65 C66 174.6(3) . . . . ? C64 C65 C66 C67 -0.6(5) . . . . ? C65 C66 C67 C68 3.6(5) . . . . ? C65 C66 C67 C72 -174.0(3) . . . . ? C64 C63 C68 C67 1.5(4) . . . . ? C53 C63 C68 C67 -177.6(3) . . . . ? C64 C63 C68 C69 179.2(3) . . . . ? C53 C63 C68 C69 0.1(4) . . . . ? C66 C67 C68 C63 -4.0(4) . . . . ? C72 C67 C68 C63 173.6(3) . . . . ? C66 C67 C68 C69 178.4(3) . . . . ? C72 C67 C68 C69 -4.1(4) . . . . ? C63 C68 C69 C70 -179.1(3) . . . . ? C67 C68 C69 C70 -1.5(5) . . . . ? C68 C69 C70 C71 34.3(6) . . . . ? C69 C70 C71 C72 -60.7(6) . . . . ? C66 C67 C72 C71 156.5(4) . . . . ? C68 C67 C72 C71 -21.0(5) . . . . ? C70 C71 C72 C67 53.1(5) . . . . ? C64 N5 C74 C75 177.5(3) . . . . ? Sm1 N5 C74 C75 -11.3(4) . . . . ? C78 N6 C75 C76 0.9(4) . . . . ? Sm1 N6 C75 C76 -168.9(2) . . . . ? C78 N6 C75 C74 -179.6(3) . . . . ? Sm1 N6 C75 C74 10.7(4) . . . . ? N5 C74 C75 N6 0.5(5) . . . . ? N5 C74 C75 C76 -179.9(3) . . . . ? N6 C75 C76 C77 -1.6(4) . . . . ? C74 C75 C76 C77 178.9(3) . . . . ? C75 C76 C77 C78 1.6(4) . . . . ? C75 N6 C78 C77 0.2(4) . . . . ? Sm1 N6 C78 C77 165.3(3) . . . . ? C76 C77 C78 N6 -1.2(4) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.052 0.750 0.000 904.3 88.1 2 -0.103 0.250 0.500 904.2 87.5 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.629 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.070 # Attachment 'compound_8.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 687848' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H84 N5 O2 Si2 Y' _chemical_formula_sum 'C70 H84 N5 O2 Si2 Y' _chemical_formula_weight 1172.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 11.787(3) _cell_length_b 13.395(3) _cell_length_c 40.333(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6368(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 15160 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.8 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 1.001 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8098 _exptl_absorpt_correction_T_max 0.8562 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 57268 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0848 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.83 _reflns_number_total 15076 _reflns_number_gt 13701 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0108P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.011(3) _refine_ls_number_reflns 15076 _refine_ls_number_parameters 766 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.84920(2) 0.92394(2) 0.363217(6) 0.01702(6) Uani 1 1 d . . . Si1 Si 0.92686(8) 0.77572(7) 0.29803(2) 0.0246(2) Uani 1 1 d . . . Si2 Si 1.11792(7) 0.84359(6) 0.34154(2) 0.02308(19) Uani 1 1 d . . . N1 N 0.86514(19) 1.08611(17) 0.39096(5) 0.0188(5) Uani 1 1 d . . . N2 N 0.93660(19) 0.90406(17) 0.41584(5) 0.0212(5) Uani 1 1 d . . . N3 N 0.7297(2) 0.78403(17) 0.38252(5) 0.0185(5) Uani 1 1 d . . . N4 N 0.6546(2) 0.96501(16) 0.35629(5) 0.0216(5) Uani 1 1 d . . . N5 N 0.97571(19) 0.83992(17) 0.33195(5) 0.0198(5) Uani 1 1 d . . . O1 O 0.85102(17) 1.04700(13) 0.31655(4) 0.0199(4) Uani 1 1 d . . . O2 O 0.49874(17) 0.56822(18) 0.41045(5) 0.0358(5) Uani 1 1 d . . . C1 C 0.8503(3) 1.2259(2) 0.35255(6) 0.0196(6) Uani 1 1 d . . . C2 C 0.8106(2) 1.1768(2) 0.38066(6) 0.0185(6) Uani 1 1 d . . . C3 C 0.7159(3) 1.2118(2) 0.39717(7) 0.0240(7) Uani 1 1 d . . . H3 H 0.6890 1.1783 0.4164 0.029 Uiso 1 1 calc R . . C4 C 0.6606(3) 1.2956(2) 0.38558(7) 0.0252(6) Uani 1 1 d . . . H4 H 0.5963 1.3199 0.3973 0.030 Uiso 1 1 calc R . . C5 C 0.6963(2) 1.3452(2) 0.35733(7) 0.0228(6) Uani 1 1 d . . . C6 C 0.7920(2) 1.3103(2) 0.34036(7) 0.0214(6) Uani 1 1 d . . . C7 C 0.8310(3) 1.3601(2) 0.30836(6) 0.0264(7) Uani 1 1 d . . . H7A H 0.9003 1.3995 0.3129 0.032 Uiso 1 1 calc R . . H7B H 0.8510 1.3077 0.2921 0.032 Uiso 1 1 calc R . . C8 C 0.7417(2) 1.4282(2) 0.29331(7) 0.0290(7) Uani 1 1 d . . . H8A H 0.7762 1.4684 0.2753 0.035 Uiso 1 1 calc R . . H8B H 0.6802 1.3874 0.2835 0.035 Uiso 1 1 calc R . . C9 C 0.6928(3) 1.4971(2) 0.31947(7) 0.0286(7) Uani 1 1 d . . . H9A H 0.6399 1.5451 0.3090 0.034 Uiso 1 1 calc R . . H9B H 0.7546 1.5354 0.3302 0.034 Uiso 1 1 calc R . . C10 C 0.6301(2) 1.4356(2) 0.34544(7) 0.0302(7) Uani 1 1 d . . . H10A H 0.6129 1.4788 0.3647 0.036 Uiso 1 1 calc R . . H10B H 0.5570 1.4129 0.3360 0.036 Uiso 1 1 calc R . . C11 C 0.9553(2) 1.1900(2) 0.33549(6) 0.0183(6) Uani 1 1 d . . . C12 C 0.9510(2) 1.1045(2) 0.31601(7) 0.0194(6) Uani 1 1 d . . . C13 C 1.0424(2) 1.0724(2) 0.29731(6) 0.0226(6) Uani 1 1 d . . . H13 H 1.0364 1.0151 0.2835 0.027 Uiso 1 1 calc R . . C14 C 1.1420(3) 1.1252(2) 0.29914(6) 0.0232(6) Uani 1 1 d . . . H14 H 1.2050 1.1044 0.2862 0.028 Uiso 1 1 calc R . . C15 C 1.1528(3) 1.2092(2) 0.31970(6) 0.0211(6) Uani 1 1 d . . . C16 C 1.0594(2) 1.2415(2) 0.33786(7) 0.0198(6) Uani 1 1 d . . . C17 C 1.0693(2) 1.3286(2) 0.36168(8) 0.0271(7) Uani 1 1 d . . . H17A H 1.0721 1.3025 0.3846 0.033 Uiso 1 1 calc R . . H17B H 1.0007 1.3708 0.3597 0.033 Uiso 1 1 calc R . . C18 C 1.1736(3) 1.3926(2) 0.35553(9) 0.0379(9) Uani 1 1 d . . . H18A H 1.1619 1.4334 0.3353 0.045 Uiso 1 1 calc R . . H18B H 1.1847 1.4387 0.3745 0.045 Uiso 1 1 calc R . . C19 C 1.2783(3) 1.3288(3) 0.35126(9) 0.0418(9) Uani 1 1 d . . . H19A H 1.2894 1.2866 0.3712 0.050 Uiso 1 1 calc R . . H19B H 1.3459 1.3719 0.3486 0.050 Uiso 1 1 calc R . . C20 C 1.2645(3) 1.2631(2) 0.32083(8) 0.0286(7) Uani 1 1 d . . . H20A H 1.2717 1.3050 0.3007 0.034 Uiso 1 1 calc R . . H20B H 1.3266 1.2133 0.3204 0.034 Uiso 1 1 calc R . . C21 C 0.9026(2) 1.0813(2) 0.42114(6) 0.0233(6) Uani 1 1 d . . . H21 H 0.9016 1.1395 0.4346 0.028 Uiso 1 1 calc R . . C22 C 0.9449(3) 0.9911(2) 0.43433(7) 0.0231(7) Uani 1 1 d . . . C23 C 0.9980(3) 0.9720(3) 0.46450(8) 0.0338(8) Uani 1 1 d . . . H23 H 1.0128 1.0189 0.4816 0.041 Uiso 1 1 calc R . . C24 C 1.0250(3) 0.8715(3) 0.46470(8) 0.0346(8) Uani 1 1 d . . . H24 H 1.0632 0.8361 0.4818 0.042 Uiso 1 1 calc R . . C25 C 0.9851(3) 0.8325(2) 0.43483(7) 0.0265(7) Uani 1 1 d . . . H25 H 0.9912 0.7643 0.4286 0.032 Uiso 1 1 calc R . . C26 C 0.7788(3) 1.0649(3) 0.28812(7) 0.0312(8) Uani 1 1 d . . . H26A H 0.7531 1.1345 0.2883 0.047 Uiso 1 1 calc R . . H26B H 0.7130 1.0204 0.2891 0.047 Uiso 1 1 calc R . . H26C H 0.8216 1.0521 0.2677 0.047 Uiso 1 1 calc R . . C27 C 0.7066(2) 0.6477(2) 0.42430(6) 0.0204(6) Uani 1 1 d . . . C28 C 0.7647(2) 0.6928(2) 0.39772(7) 0.0188(6) Uani 1 1 d . . . C29 C 0.8647(3) 0.6497(2) 0.38613(6) 0.0228(6) Uani 1 1 d . . . H29 H 0.9062 0.6814 0.3689 0.027 Uiso 1 1 calc R . . C30 C 0.9040(2) 0.5618(2) 0.39942(7) 0.0241(7) Uani 1 1 d . . . H30 H 0.9716 0.5330 0.3909 0.029 Uiso 1 1 calc R . . C31 C 0.8472(3) 0.5142(2) 0.42502(6) 0.0221(6) Uani 1 1 d . . . C32 C 0.7490(2) 0.5577(2) 0.43778(6) 0.0220(7) Uani 1 1 d . . . C33 C 0.6885(3) 0.5096(2) 0.46699(7) 0.0279(7) Uani 1 1 d . . . H33A H 0.6057 0.5189 0.4644 0.034 Uiso 1 1 calc R . . H33B H 0.7119 0.5438 0.4876 0.034 Uiso 1 1 calc R . . C34 C 0.7139(3) 0.3978(2) 0.47027(7) 0.0317(8) Uani 1 1 d . . . H34A H 0.6818 0.3726 0.4914 0.038 Uiso 1 1 calc R . . H34B H 0.6771 0.3613 0.4518 0.038 Uiso 1 1 calc R . . C35 C 0.8393(3) 0.3781(2) 0.46960(7) 0.0349(8) Uani 1 1 d . . . H35A H 0.8531 0.3056 0.4722 0.042 Uiso 1 1 calc R . . H35B H 0.8759 0.4128 0.4884 0.042 Uiso 1 1 calc R . . C36 C 0.8920(3) 0.4142(2) 0.43714(7) 0.0297(7) Uani 1 1 d . . . H36A H 0.9751 0.4195 0.4402 0.036 Uiso 1 1 calc R . . H36B H 0.8779 0.3634 0.4198 0.036 Uiso 1 1 calc R . . C37 C 0.5996(3) 0.6936(2) 0.43823(7) 0.0229(7) Uani 1 1 d . . . C38 C 0.4943(3) 0.6523(2) 0.42990(7) 0.0263(7) Uani 1 1 d . . . C39 C 0.3939(3) 0.6970(3) 0.43978(8) 0.0350(8) Uani 1 1 d . . . H39 H 0.3228 0.6692 0.4337 0.042 Uiso 1 1 calc R . . C40 C 0.3992(3) 0.7825(3) 0.45862(9) 0.0438(10) Uani 1 1 d . A . H40 H 0.3305 0.8142 0.4650 0.053 Uiso 1 1 calc R . . C41 C 0.5013(3) 0.8240(2) 0.46865(9) 0.0412(9) Uani 1 1 d D . . C42 C 0.6039(3) 0.7795(2) 0.45839(7) 0.0264(7) Uani 1 1 d D A . C43 C 0.7182(6) 0.8152(7) 0.4703(2) 0.029(2) Uani 0.632(6) 1 d PDU A 1 H43A H 0.7636 0.8398 0.4513 0.035 Uiso 0.632(6) 1 calc PR A 1 H43B H 0.7599 0.7597 0.4809 0.035 Uiso 0.632(6) 1 calc PR A 1 C44 C 0.6986(8) 0.9003(7) 0.4954(2) 0.038(2) Uani 0.632(6) 1 d PDU A 1 H44A H 0.6786 0.8702 0.5171 0.046 Uiso 0.632(6) 1 calc PR A 1 H44B H 0.7709 0.9368 0.4984 0.046 Uiso 0.632(6) 1 calc PR A 1 C45 C 0.6056(4) 0.9763(4) 0.48610(15) 0.0473(19) Uani 0.632(6) 1 d PDU A 1 H45A H 0.6051 1.0320 0.5022 0.057 Uiso 0.632(6) 1 calc PR A 1 H45B H 0.6207 1.0040 0.4638 0.057 Uiso 0.632(6) 1 calc PR A 1 C46 C 0.4903(6) 0.9228(5) 0.48640(19) 0.0404(18) Uani 0.632(6) 1 d PDU A 1 H46A H 0.4655 0.9115 0.5096 0.048 Uiso 0.632(6) 1 calc PR A 1 H46B H 0.4326 0.9646 0.4752 0.048 Uiso 0.632(6) 1 calc PR A 1 C43' C 0.7127(10) 0.8320(11) 0.4654(4) 0.020(4) Uani 0.368(6) 1 d PDU A 2 H43C H 0.7394 0.8594 0.4440 0.024 Uiso 0.368(6) 1 calc PR A 2 H43D H 0.7679 0.7798 0.4719 0.024 Uiso 0.368(6) 1 calc PR A 2 C44' C 0.7246(13) 0.9167(13) 0.4911(4) 0.036(4) Uani 0.368(6) 1 d PDU A 2 H44C H 0.7996 0.9125 0.5020 0.043 Uiso 0.368(6) 1 calc PR A 2 H44D H 0.7194 0.9822 0.4798 0.043 Uiso 0.368(6) 1 calc PR A 2 C45' C 0.6302(7) 0.9082(7) 0.5172(2) 0.038(3) Uani 0.368(6) 1 d PDU A 2 H45C H 0.6295 0.9675 0.5318 0.045 Uiso 0.368(6) 1 calc PR A 2 H45D H 0.6407 0.8477 0.5310 0.045 Uiso 0.368(6) 1 calc PR A 2 C46' C 0.5188(10) 0.9015(8) 0.4970(3) 0.043(4) Uani 0.368(6) 1 d PDU A 2 H46C H 0.5060 0.9682 0.4871 0.052 Uiso 0.368(6) 1 calc PR A 2 H46D H 0.4568 0.8906 0.5132 0.052 Uiso 0.368(6) 1 calc PR A 2 C47 C 0.6226(2) 0.7970(2) 0.37616(6) 0.0234(7) Uani 1 1 d . . . H47 H 0.5713 0.7434 0.3800 0.028 Uiso 1 1 calc R . . C48 C 0.5800(2) 0.8881(2) 0.36373(7) 0.0230(6) Uani 1 1 d . . . C49 C 0.4688(2) 0.9195(3) 0.35974(8) 0.0362(8) Uani 1 1 d . . . H49 H 0.4025 0.8805 0.3631 0.043 Uiso 1 1 calc R . . C50 C 0.4727(3) 1.0188(2) 0.34995(8) 0.0344(8) Uani 1 1 d . . . H50 H 0.4100 1.0614 0.3455 0.041 Uiso 1 1 calc R . . C51 C 0.5872(3) 1.0433(2) 0.34800(7) 0.0263(7) Uani 1 1 d . . . H51 H 0.6149 1.1070 0.3416 0.032 Uiso 1 1 calc R . . C52 C 0.3937(3) 0.5207(3) 0.40298(9) 0.0470(10) Uani 1 1 d . . . H52A H 0.3543 0.5039 0.4237 0.070 Uiso 1 1 calc R . . H52B H 0.4081 0.4594 0.3903 0.070 Uiso 1 1 calc R . . H52C H 0.3463 0.5658 0.3898 0.070 Uiso 1 1 calc R . . C53 C 0.9594(3) 0.8364(2) 0.25698(7) 0.0335(8) Uani 1 1 d . . . H53A H 0.9137 0.8971 0.2546 0.050 Uiso 1 1 calc R . . H53B H 0.9413 0.7900 0.2390 0.050 Uiso 1 1 calc R . . H53C H 1.0401 0.8538 0.2561 0.050 Uiso 1 1 calc R . . C54 C 0.7677(3) 0.7678(2) 0.29908(7) 0.0313(8) Uani 1 1 d . . . H54A H 0.7443 0.7212 0.3165 0.047 Uiso 1 1 calc R . . H54B H 0.7398 0.7440 0.2776 0.047 Uiso 1 1 calc R . . H54C H 0.7360 0.8340 0.3037 0.047 Uiso 1 1 calc R . . C55 C 0.9826(3) 0.6443(2) 0.29541(8) 0.0365(8) Uani 1 1 d . . . H55A H 1.0645 0.6459 0.2912 0.055 Uiso 1 1 calc R . . H55B H 0.9444 0.6090 0.2773 0.055 Uiso 1 1 calc R . . H55C H 0.9680 0.6096 0.3164 0.055 Uiso 1 1 calc R . . C56 C 1.2137(3) 0.8515(2) 0.30441(7) 0.0296(7) Uani 1 1 d . . . H56A H 1.2015 0.7931 0.2902 0.044 Uiso 1 1 calc R . . H56B H 1.2930 0.8530 0.3117 0.044 Uiso 1 1 calc R . . H56C H 1.1967 0.9124 0.2919 0.044 Uiso 1 1 calc R . . C57 C 1.1677(3) 0.7289(2) 0.36442(8) 0.0316(7) Uani 1 1 d . . . H57A H 1.1244 0.7218 0.3850 0.047 Uiso 1 1 calc R . . H57B H 1.2485 0.7356 0.3696 0.047 Uiso 1 1 calc R . . H57C H 1.1559 0.6699 0.3505 0.047 Uiso 1 1 calc R . . C58 C 1.1515(3) 0.9544(2) 0.36882(6) 0.0276(7) Uani 1 1 d . . . H58A H 1.1010 1.0100 0.3631 0.041 Uiso 1 1 calc R . . H58B H 1.2305 0.9747 0.3653 0.041 Uiso 1 1 calc R . . H58C H 1.1404 0.9361 0.3921 0.041 Uiso 1 1 calc R . . C59 C 0.1125(4) 0.4741(4) 0.78890(13) 0.0737(16) Uani 1 1 d . . . H59 H 0.1591 0.5115 0.8036 0.088 Uiso 1 1 calc R . . C60 C 0.0600(4) 0.5204(4) 0.76437(14) 0.0733(15) Uani 1 1 d . . . H60 H 0.0683 0.5906 0.7620 0.088 Uiso 1 1 calc R . . C61 C -0.0056(4) 0.4691(6) 0.74251(12) 0.089(2) Uani 1 1 d . . . H61 H -0.0420 0.5024 0.7246 0.107 Uiso 1 1 calc R . . C62 C -0.0183(4) 0.3659(5) 0.74695(14) 0.087(2) Uani 1 1 d . . . H62 H -0.0645 0.3282 0.7322 0.104 Uiso 1 1 calc R . . C63 C 0.0363(4) 0.3201(4) 0.77264(15) 0.0838(18) Uani 1 1 d . . . H63 H 0.0288 0.2501 0.7759 0.101 Uiso 1 1 calc R . . C64 C 0.1017(4) 0.3755(4) 0.79356(13) 0.0762(16) Uani 1 1 d . . . H64 H 0.1397 0.3442 0.8115 0.091 Uiso 1 1 calc R . . C65 C 0.1977(4) 0.2493(5) 0.44968(13) 0.0763(16) Uani 1 1 d . . . H65 H 0.1200 0.2658 0.4527 0.092 Uiso 1 1 calc R . . C66 C 0.2812(7) 0.3127(4) 0.46119(13) 0.0842(18) Uani 1 1 d . . . H66 H 0.2622 0.3733 0.4721 0.101 Uiso 1 1 calc R . . C67 C 0.3912(6) 0.2859(5) 0.45651(15) 0.094(2) Uani 1 1 d . . . H67 H 0.4495 0.3292 0.4641 0.113 Uiso 1 1 calc R . . C68 C 0.4202(5) 0.1990(6) 0.44136(17) 0.110(3) Uani 1 1 d . . . H68 H 0.4974 0.1805 0.4386 0.132 Uiso 1 1 calc R . . C69 C 0.3335(7) 0.1386(5) 0.43018(12) 0.097(2) Uani 1 1 d . . . H69 H 0.3509 0.0774 0.4194 0.116 Uiso 1 1 calc R . . C70 C 0.2262(6) 0.1653(5) 0.43440(12) 0.0793(17) Uani 1 1 d . . . H70 H 0.1679 0.1230 0.4262 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.01655(13) 0.01902(13) 0.01548(10) 0.00116(11) -0.00013(11) -0.00067(13) Si1 0.0280(5) 0.0253(5) 0.0206(4) -0.0032(4) 0.0037(4) -0.0042(4) Si2 0.0204(5) 0.0242(5) 0.0246(4) 0.0010(3) 0.0020(3) 0.0020(4) N1 0.0179(13) 0.0208(12) 0.0176(10) 0.0029(9) -0.0001(9) -0.0012(11) N2 0.0212(13) 0.0233(14) 0.0190(11) 0.0040(10) -0.0030(9) -0.0015(11) N3 0.0222(14) 0.0177(13) 0.0157(11) 0.0028(9) 0.0028(10) -0.0014(11) N4 0.0180(12) 0.0227(12) 0.0241(12) 0.0043(9) 0.0006(11) 0.0015(11) N5 0.0157(13) 0.0234(14) 0.0203(11) 0.0002(10) 0.0028(9) 0.0023(11) O1 0.0181(10) 0.0228(10) 0.0188(9) 0.0030(7) -0.0012(9) -0.0027(9) O2 0.0222(12) 0.0469(15) 0.0383(12) -0.0137(12) 0.0025(10) -0.0073(12) C1 0.0180(15) 0.0224(15) 0.0184(12) -0.0025(10) 0.0003(12) -0.0010(14) C2 0.0188(16) 0.0184(15) 0.0182(13) -0.0022(11) -0.0005(11) 0.0003(12) C3 0.0249(17) 0.0291(18) 0.0181(13) 0.0007(12) 0.0033(12) -0.0009(14) C4 0.0203(16) 0.0290(16) 0.0262(14) -0.0027(12) 0.0055(13) 0.0041(15) C5 0.0235(16) 0.0219(16) 0.0231(15) -0.0009(12) -0.0004(12) 0.0025(13) C6 0.0189(15) 0.0209(16) 0.0242(14) -0.0005(12) 0.0002(12) 0.0008(13) C7 0.0277(19) 0.0272(17) 0.0243(14) 0.0060(12) 0.0052(13) 0.0030(14) C8 0.0302(18) 0.0298(18) 0.0270(15) 0.0081(15) -0.0004(13) 0.0030(16) C9 0.0302(19) 0.0247(17) 0.0310(16) 0.0017(13) -0.0035(13) 0.0042(14) C10 0.0286(19) 0.0312(18) 0.0308(15) 0.0005(14) 0.0013(13) 0.0120(16) C11 0.0198(15) 0.0183(15) 0.0167(13) 0.0059(11) 0.0011(11) -0.0011(12) C12 0.0158(15) 0.0210(16) 0.0213(14) 0.0038(11) -0.0013(11) -0.0010(12) C13 0.0248(16) 0.0223(15) 0.0206(13) 0.0019(13) 0.0015(11) 0.0003(15) C14 0.0205(16) 0.0251(16) 0.0240(13) 0.0036(11) 0.0029(13) 0.0046(14) C15 0.0198(15) 0.0215(15) 0.0220(13) 0.0044(11) 0.0013(13) -0.0026(14) C16 0.0183(16) 0.0207(16) 0.0205(14) 0.0015(11) 0.0012(12) -0.0002(12) C17 0.0253(17) 0.0259(16) 0.0301(15) -0.0039(14) 0.0019(15) -0.0024(13) C18 0.026(2) 0.0347(19) 0.053(2) -0.0151(15) 0.0041(15) -0.0073(15) C19 0.025(2) 0.054(2) 0.047(2) -0.0095(18) 0.0019(16) -0.0117(18) C20 0.0211(18) 0.0288(19) 0.0361(17) -0.0017(14) 0.0031(14) -0.0010(14) C21 0.0275(16) 0.0219(16) 0.0206(13) -0.0019(13) -0.0015(11) -0.0025(15) C22 0.0296(18) 0.0219(16) 0.0177(13) 0.0002(12) -0.0047(12) -0.0025(14) C23 0.046(2) 0.0298(19) 0.0255(16) -0.0012(14) -0.0159(15) -0.0022(17) C24 0.039(2) 0.036(2) 0.0291(17) 0.0073(15) -0.0162(15) -0.0003(17) C25 0.0286(18) 0.0207(17) 0.0304(16) 0.0044(13) -0.0031(13) 0.0026(14) C26 0.0274(18) 0.042(2) 0.0237(15) 0.0074(15) -0.0065(12) -0.0027(17) C27 0.0205(16) 0.0212(16) 0.0194(13) -0.0003(12) 0.0012(11) -0.0044(13) C28 0.0194(16) 0.0155(15) 0.0217(14) -0.0019(11) -0.0023(11) 0.0005(12) C29 0.0231(17) 0.0244(15) 0.0210(13) -0.0010(12) 0.0043(12) -0.0025(14) C30 0.0221(16) 0.0207(17) 0.0294(15) -0.0064(13) 0.0009(12) 0.0021(13) C31 0.0242(16) 0.0179(14) 0.0242(13) -0.0011(11) -0.0052(14) 0.0008(14) C32 0.0267(16) 0.0229(18) 0.0164(13) 0.0012(11) 0.0013(11) -0.0024(13) C33 0.033(2) 0.0274(17) 0.0236(15) 0.0045(13) 0.0033(13) -0.0012(14) C34 0.047(2) 0.0271(19) 0.0208(15) 0.0036(13) 0.0061(14) -0.0034(15) C35 0.054(2) 0.0218(16) 0.0288(15) 0.0027(12) -0.0080(17) 0.0031(17) C36 0.0323(18) 0.0233(17) 0.0333(16) -0.0012(14) -0.0046(13) 0.0029(15) C37 0.0263(17) 0.0235(16) 0.0189(14) 0.0044(12) 0.0045(12) 0.0028(13) C38 0.0291(18) 0.0287(18) 0.0210(14) 0.0034(13) 0.0052(13) 0.0010(15) C39 0.0244(19) 0.043(2) 0.0373(18) 0.0076(16) 0.0067(15) 0.0025(16) C40 0.030(2) 0.039(2) 0.063(2) 0.0052(19) 0.0217(18) 0.0045(18) C41 0.046(2) 0.0256(19) 0.053(2) -0.0051(16) 0.0242(19) 0.0021(17) C42 0.0293(18) 0.0261(17) 0.0236(15) 0.0008(13) 0.0081(13) 0.0021(14) C43 0.046(4) 0.021(4) 0.021(4) 0.001(3) 0.006(3) -0.001(3) C44 0.039(5) 0.038(5) 0.037(4) -0.016(3) 0.001(3) -0.009(4) C45 0.050(4) 0.036(3) 0.056(4) -0.024(3) 0.001(3) 0.006(3) C46 0.033(4) 0.028(3) 0.060(4) -0.007(3) 0.010(3) 0.011(3) C43' 0.020(4) 0.019(4) 0.020(4) 0.0004(10) 0.0005(10) -0.0003(10) C44' 0.038(7) 0.033(7) 0.037(6) -0.011(5) 0.018(5) -0.008(6) C45' 0.040(6) 0.039(5) 0.035(4) -0.014(4) 0.009(4) -0.006(4) C46' 0.042(7) 0.026(6) 0.062(7) -0.001(5) 0.017(5) 0.014(5) C47 0.0237(18) 0.0255(16) 0.0209(13) 0.0029(12) -0.0001(12) -0.0079(13) C48 0.0193(15) 0.0259(16) 0.0237(14) 0.0065(13) -0.0016(13) -0.0024(12) C49 0.0152(15) 0.048(2) 0.0452(19) 0.015(2) -0.0013(14) -0.0044(17) C50 0.0205(18) 0.037(2) 0.046(2) 0.0160(16) -0.0013(14) 0.0086(15) C51 0.0254(18) 0.0230(17) 0.0305(16) 0.0029(13) -0.0003(13) 0.0026(13) C52 0.032(2) 0.054(3) 0.055(2) -0.0113(19) -0.0033(18) -0.0165(19) C53 0.040(2) 0.039(2) 0.0215(15) -0.0063(14) 0.0022(14) -0.0101(17) C54 0.035(2) 0.034(2) 0.0240(16) -0.0018(14) -0.0011(14) -0.0067(16) C55 0.047(2) 0.0292(19) 0.0333(17) -0.0060(15) 0.0095(16) -0.0025(17) C56 0.0266(18) 0.0265(18) 0.0356(17) -0.0006(14) 0.0047(14) 0.0043(15) C57 0.0248(18) 0.0330(17) 0.0370(16) 0.0023(15) 0.0024(16) 0.0030(14) C58 0.0202(15) 0.0330(17) 0.0296(15) 0.0021(12) -0.0018(14) -0.0008(14) C59 0.041(3) 0.084(4) 0.096(4) -0.051(3) 0.005(3) 0.006(3) C60 0.058(4) 0.068(4) 0.094(4) 0.001(3) 0.033(3) 0.008(3) C61 0.048(3) 0.178(7) 0.040(3) 0.009(4) 0.019(2) 0.036(4) C62 0.035(3) 0.142(6) 0.082(4) -0.071(4) -0.001(3) -0.011(4) C63 0.063(4) 0.057(3) 0.131(5) -0.039(3) -0.011(4) 0.006(3) C64 0.056(3) 0.084(4) 0.089(4) -0.028(3) -0.021(3) 0.030(3) C65 0.060(4) 0.105(5) 0.063(3) 0.045(3) 0.007(3) 0.014(3) C66 0.141(6) 0.044(3) 0.068(3) 0.020(3) 0.022(4) 0.017(4) C67 0.094(5) 0.098(5) 0.091(5) 0.046(4) -0.024(4) -0.050(4) C68 0.057(4) 0.158(7) 0.115(6) 0.090(5) 0.040(4) 0.024(4) C69 0.142(6) 0.094(5) 0.055(3) 0.014(3) 0.043(4) 0.021(5) C70 0.096(5) 0.093(5) 0.049(3) 0.015(3) -0.009(3) -0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N5 2.254(2) . ? Y1 N2 2.374(2) . ? Y1 N4 2.375(3) . ? Y1 N1 2.451(2) . ? Y1 N3 2.470(2) . ? Y1 O1 2.5022(17) . ? Y1 Si1 3.4192(10) . ? Si1 N5 1.715(2) . ? Si1 C54 1.880(3) . ? Si1 C55 1.882(3) . ? Si1 C53 1.884(3) . ? Si2 N5 1.721(2) . ? Si2 C56 1.878(3) . ? Si2 C57 1.885(3) . ? Si2 C58 1.890(3) . ? N1 C21 1.296(3) . ? N1 C2 1.436(3) . ? N2 C25 1.354(3) . ? N2 C22 1.387(3) . ? N3 C47 1.301(4) . ? N3 C28 1.428(3) . ? N4 C51 1.357(3) . ? N4 C48 1.387(3) . ? O1 C12 1.407(3) . ? O1 C26 1.448(3) . ? O2 C38 1.374(4) . ? O2 C52 1.425(4) . ? C1 C2 1.392(3) . ? C1 C6 1.411(4) . ? C1 C11 1.496(4) . ? C2 C3 1.382(4) . ? C3 C4 1.380(4) . ? C3 H3 0.9500 . ? C4 C5 1.384(4) . ? C4 H4 0.9500 . ? C5 C6 1.400(4) . ? C5 C10 1.519(4) . ? C6 C7 1.523(4) . ? C7 C8 1.519(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.516(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.524(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.390(4) . ? C11 C16 1.411(4) . ? C12 C13 1.384(4) . ? C13 C14 1.372(4) . ? C13 H13 0.9500 . ? C14 C15 1.404(4) . ? C14 H14 0.9500 . ? C15 C16 1.392(4) . ? C15 C20 1.502(4) . ? C16 C17 1.515(4) . ? C17 C18 1.520(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.512(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.519(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.411(4) . ? C21 H21 0.9500 . ? C22 C23 1.392(4) . ? C23 C24 1.384(4) . ? C23 H23 0.9500 . ? C24 C25 1.395(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.408(4) . ? C27 C32 1.415(4) . ? C27 C37 1.511(4) . ? C28 C29 1.394(4) . ? C29 C30 1.375(4) . ? C29 H29 0.9500 . ? C30 C31 1.386(4) . ? C30 H30 0.9500 . ? C31 C32 1.394(4) . ? C31 C36 1.521(4) . ? C32 C33 1.520(4) . ? C33 C34 1.533(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.501(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.527(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.399(4) . ? C37 C42 1.410(4) . ? C38 C39 1.385(4) . ? C39 C40 1.376(5) . ? C39 H39 0.9500 . ? C40 C41 1.386(5) . ? C40 H40 0.9500 . ? C41 C42 1.411(4) . ? C41 C46 1.510(6) . ? C41 C46' 1.557(8) . ? C42 C43' 1.490(9) . ? C42 C43 1.508(6) . ? C43 C44 1.543(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.542(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.536(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C43' C44' 1.543(9) . ? C43' H43C 0.9900 . ? C43' H43D 0.9900 . ? C44' C45' 1.537(9) . ? C44' H44C 0.9900 . ? C44' H44D 0.9900 . ? C45' C46' 1.548(8) . ? C45' H45C 0.9900 . ? C45' H45D 0.9900 . ? C46' H46C 0.9900 . ? C46' H46D 0.9900 . ? C47 C48 1.412(4) . ? C47 H47 0.9500 . ? C48 C49 1.386(4) . ? C49 C50 1.389(4) . ? C49 H49 0.9500 . ? C50 C51 1.391(4) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.322(6) . ? C59 C64 1.339(6) . ? C59 H59 0.9500 . ? C60 C61 1.359(7) . ? C60 H60 0.9500 . ? C61 C62 1.402(7) . ? C61 H61 0.9500 . ? C62 C63 1.366(7) . ? C62 H62 0.9500 . ? C63 C64 1.363(6) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C70 1.326(7) . ? C65 C66 1.380(7) . ? C65 H65 0.9500 . ? C66 C67 1.358(7) . ? C66 H66 0.9500 . ? C67 C68 1.358(8) . ? C67 H67 0.9500 . ? C68 C69 1.379(8) . ? C68 H68 0.9500 . ? C69 C70 1.326(8) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Y1 N2 99.04(8) . . ? N5 Y1 N4 133.53(8) . . ? N2 Y1 N4 123.37(8) . . ? N5 Y1 N1 130.34(8) . . ? N2 Y1 N1 70.00(8) . . ? N4 Y1 N1 85.55(7) . . ? N5 Y1 N3 100.06(8) . . ? N2 Y1 N3 83.13(8) . . ? N4 Y1 N3 70.27(8) . . ? N1 Y1 N3 124.91(7) . . ? N5 Y1 O1 84.39(7) . . ? N2 Y1 O1 137.96(7) . . ? N4 Y1 O1 76.54(7) . . ? N1 Y1 O1 76.05(6) . . ? N3 Y1 O1 137.89(7) . . ? N5 Y1 Si1 26.21(6) . . ? N2 Y1 Si1 120.40(6) . . ? N4 Y1 Si1 107.62(5) . . ? N1 Y1 Si1 147.69(5) . . ? N3 Y1 Si1 87.39(6) . . ? O1 Y1 Si1 78.57(5) . . ? N5 Si1 C54 110.22(13) . . ? N5 Si1 C55 113.36(14) . . ? C54 Si1 C55 107.27(16) . . ? N5 Si1 C53 114.59(13) . . ? C54 Si1 C53 104.32(15) . . ? C55 Si1 C53 106.45(15) . . ? N5 Si1 Y1 35.47(8) . . ? C54 Si1 Y1 75.43(10) . . ? C55 Si1 Y1 132.83(10) . . ? C53 Si1 Y1 118.66(11) . . ? N5 Si2 C56 114.08(13) . . ? N5 Si2 C57 112.93(13) . . ? C56 Si2 C57 104.43(14) . . ? N5 Si2 C58 110.93(13) . . ? C56 Si2 C58 107.11(14) . . ? C57 Si2 C58 106.84(13) . . ? C21 N1 C2 117.8(2) . . ? C21 N1 Y1 114.3(2) . . ? C2 N1 Y1 125.70(16) . . ? C25 N2 C22 105.1(2) . . ? C25 N2 Y1 140.2(2) . . ? C22 N2 Y1 114.64(17) . . ? C47 N3 C28 118.6(2) . . ? C47 N3 Y1 112.98(19) . . ? C28 N3 Y1 128.33(18) . . ? C51 N4 C48 104.8(2) . . ? C51 N4 Y1 140.6(2) . . ? C48 N4 Y1 114.49(17) . . ? Si1 N5 Si2 121.36(13) . . ? Si1 N5 Y1 118.32(12) . . ? Si2 N5 Y1 120.29(12) . . ? C12 O1 C26 112.9(2) . . ? C12 O1 Y1 112.28(15) . . ? C26 O1 Y1 134.43(17) . . ? C38 O2 C52 117.0(2) . . ? C2 C1 C6 120.0(3) . . ? C2 C1 C11 120.0(3) . . ? C6 C1 C11 120.0(2) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 N1 120.6(2) . . ? C1 C2 N1 119.1(2) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 121.7(3) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C4 C5 C6 119.2(3) . . ? C4 C5 C10 119.1(3) . . ? C6 C5 C10 121.7(3) . . ? C5 C6 C1 119.3(3) . . ? C5 C6 C7 120.8(3) . . ? C1 C6 C7 119.9(3) . . ? C8 C7 C6 113.1(2) . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C7 110.5(2) . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 109.5(2) . . ? C8 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? C8 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C5 C10 C9 113.5(2) . . ? C5 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? C5 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C16 118.2(3) . . ? C12 C11 C1 119.7(3) . . ? C16 C11 C1 122.1(2) . . ? C13 C12 C11 122.4(3) . . ? C13 C12 O1 119.3(2) . . ? C11 C12 O1 118.2(2) . . ? C14 C13 C12 118.4(3) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 121.5(3) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C16 C15 C14 119.3(3) . . ? C16 C15 C20 121.8(3) . . ? C14 C15 C20 118.9(3) . . ? C15 C16 C11 120.0(3) . . ? C15 C16 C17 120.8(3) . . ? C11 C16 C17 119.1(2) . . ? C16 C17 C18 113.2(3) . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.8 . . ? C19 C18 C17 111.1(3) . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? C19 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C20 109.4(3) . . ? C18 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? C18 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? C15 C20 C19 113.4(3) . . ? C15 C20 H20A 108.9 . . ? C19 C20 H20A 108.9 . . ? C15 C20 H20B 108.9 . . ? C19 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? N1 C21 C22 121.1(3) . . ? N1 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? N2 C22 C23 110.3(3) . . ? N2 C22 C21 119.5(2) . . ? C23 C22 C21 130.2(3) . . ? C24 C23 C22 106.7(3) . . ? C24 C23 H23 126.7 . . ? C22 C23 H23 126.7 . . ? C23 C24 C25 106.4(3) . . ? C23 C24 H24 126.8 . . ? C25 C24 H24 126.8 . . ? N2 C25 C24 111.5(3) . . ? N2 C25 H25 124.3 . . ? C24 C25 H25 124.3 . . ? O1 C26 H26A 109.5 . . ? O1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 119.1(3) . . ? C28 C27 C37 121.0(3) . . ? C32 C27 C37 119.9(2) . . ? C29 C28 C27 119.3(3) . . ? C29 C28 N3 117.0(2) . . ? C27 C28 N3 123.6(3) . . ? C30 C29 C28 120.6(3) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 121.5(3) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C30 C31 C32 119.0(3) . . ? C30 C31 C36 118.5(3) . . ? C32 C31 C36 122.5(3) . . ? C31 C32 C27 120.5(3) . . ? C31 C32 C33 119.9(3) . . ? C27 C32 C33 119.6(3) . . ? C32 C33 C34 112.9(2) . . ? C32 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? C32 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C35 C34 C33 111.2(3) . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? C33 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C34 C35 C36 111.1(3) . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C31 C36 C35 114.4(3) . . ? C31 C36 H36A 108.7 . . ? C35 C36 H36A 108.7 . . ? C31 C36 H36B 108.7 . . ? C35 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C38 C37 C42 119.5(3) . . ? C38 C37 C27 119.4(3) . . ? C42 C37 C27 121.1(3) . . ? O2 C38 C39 123.4(3) . . ? O2 C38 C37 115.3(3) . . ? C39 C38 C37 121.2(3) . . ? C40 C39 C38 118.7(3) . . ? C40 C39 H39 120.7 . . ? C38 C39 H39 120.7 . . ? C39 C40 C41 122.4(3) . . ? C39 C40 H40 118.8 . . ? C41 C40 H40 118.8 . . ? C40 C41 C42 119.3(3) . . ? C40 C41 C46 114.6(4) . . ? C42 C41 C46 125.7(4) . . ? C40 C41 C46' 126.6(5) . . ? C42 C41 C46' 112.6(5) . . ? C46 C41 C46' 23.0(5) . . ? C37 C42 C41 118.9(3) . . ? C37 C42 C43' 121.7(7) . . ? C41 C42 C43' 118.9(7) . . ? C37 C42 C43 118.3(4) . . ? C41 C42 C43 122.6(4) . . ? C43' C42 C43 11.7(9) . . ? C42 C43 C44 108.0(7) . . ? C42 C43 H43A 110.1 . . ? C44 C43 H43A 110.1 . . ? C42 C43 H43B 110.1 . . ? C44 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? C45 C44 C43 115.7(7) . . ? C45 C44 H44A 108.4 . . ? C43 C44 H44A 108.4 . . ? C45 C44 H44B 108.4 . . ? C43 C44 H44B 108.4 . . ? H44A C44 H44B 107.4 . . ? C46 C45 C44 108.6(6) . . ? C46 C45 H45A 110.0 . . ? C44 C45 H45A 110.0 . . ? C46 C45 H45B 110.0 . . ? C44 C45 H45B 110.0 . . ? H45A C45 H45B 108.4 . . ? C41 C46 C45 109.2(5) . . ? C41 C46 H46A 109.8 . . ? C45 C46 H46A 109.8 . . ? C41 C46 H46B 109.8 . . ? C45 C46 H46B 109.8 . . ? H46A C46 H46B 108.3 . . ? C42 C43' C44' 123.6(13) . . ? C42 C43' H43C 106.4 . . ? C44' C43' H43C 106.4 . . ? C42 C43' H43D 106.4 . . ? C44' C43' H43D 106.4 . . ? H43C C43' H43D 106.5 . . ? C45' C44' C43' 109.8(12) . . ? C45' C44' H44C 109.7 . . ? C43' C44' H44C 109.7 . . ? C45' C44' H44D 109.7 . . ? C43' C44' H44D 109.7 . . ? H44C C44' H44D 108.2 . . ? C44' C45' C46' 104.9(10) . . ? C44' C45' H45C 110.8 . . ? C46' C45' H45C 110.8 . . ? C44' C45' H45D 110.8 . . ? C46' C45' H45D 110.8 . . ? H45C C45' H45D 108.8 . . ? C45' C46' C41 122.5(8) . . ? C45' C46' H46C 106.7 . . ? C41 C46' H46C 106.7 . . ? C45' C46' H46D 106.7 . . ? C41 C46' H46D 106.7 . . ? H46C C46' H46D 106.6 . . ? N3 C47 C48 122.0(3) . . ? N3 C47 H47 119.0 . . ? C48 C47 H47 119.0 . . ? C49 C48 N4 110.4(3) . . ? C49 C48 C47 129.7(3) . . ? N4 C48 C47 119.6(2) . . ? C48 C49 C50 107.0(3) . . ? C48 C49 H49 126.5 . . ? C50 C49 H49 126.5 . . ? C49 C50 C51 105.9(3) . . ? C49 C50 H50 127.1 . . ? C51 C50 H50 127.1 . . ? N4 C51 C50 111.9(3) . . ? N4 C51 H51 124.1 . . ? C50 C51 H51 124.1 . . ? O2 C52 H52A 109.5 . . ? O2 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O2 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si1 C53 H53A 109.5 . . ? Si1 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si1 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? Si1 C54 H54A 109.5 . . ? Si1 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? Si1 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Si1 C55 H55A 109.5 . . ? Si1 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? Si1 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? Si2 C56 H56A 109.5 . . ? Si2 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? Si2 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? Si2 C57 H57A 109.5 . . ? Si2 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? Si2 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? Si2 C58 H58A 109.5 . . ? Si2 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? Si2 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 C64 121.5(5) . . ? C60 C59 H59 119.2 . . ? C64 C59 H59 119.2 . . ? C59 C60 C61 121.0(5) . . ? C59 C60 H60 119.5 . . ? C61 C60 H60 119.5 . . ? C60 C61 C62 118.4(5) . . ? C60 C61 H61 120.8 . . ? C62 C61 H61 120.8 . . ? C63 C62 C61 119.3(5) . . ? C63 C62 H62 120.3 . . ? C61 C62 H62 120.3 . . ? C64 C63 C62 119.4(5) . . ? C64 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? C59 C64 C63 120.3(5) . . ? C59 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C70 C65 C66 119.9(5) . . ? C70 C65 H65 120.1 . . ? C66 C65 H65 120.1 . . ? C67 C66 C65 118.1(5) . . ? C67 C66 H66 120.9 . . ? C65 C66 H66 120.9 . . ? C66 C67 C68 121.9(6) . . ? C66 C67 H67 119.0 . . ? C68 C67 H67 119.0 . . ? C67 C68 C69 117.6(6) . . ? C67 C68 H68 121.2 . . ? C69 C68 H68 121.2 . . ? C70 C69 C68 120.4(6) . . ? C70 C69 H69 119.8 . . ? C68 C69 H69 119.8 . . ? C65 C70 C69 122.0(6) . . ? C65 C70 H70 119.0 . . ? C69 C70 H70 119.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Y1 Si1 N5 -38.78(15) . . . . ? N4 Y1 Si1 N5 172.41(15) . . . . ? N1 Y1 Si1 N5 61.93(17) . . . . ? N3 Y1 Si1 N5 -119.25(15) . . . . ? O1 Y1 Si1 N5 100.67(14) . . . . ? N5 Y1 Si1 C54 168.54(18) . . . . ? N2 Y1 Si1 C54 129.76(13) . . . . ? N4 Y1 Si1 C54 -19.05(12) . . . . ? N1 Y1 Si1 C54 -129.53(14) . . . . ? N3 Y1 Si1 C54 49.29(12) . . . . ? O1 Y1 Si1 C54 -90.79(12) . . . . ? N5 Y1 Si1 C55 68.3(2) . . . . ? N2 Y1 Si1 C55 29.55(17) . . . . ? N4 Y1 Si1 C55 -119.26(16) . . . . ? N1 Y1 Si1 C55 130.26(18) . . . . ? N3 Y1 Si1 C55 -50.92(16) . . . . ? O1 Y1 Si1 C55 169.00(16) . . . . ? N5 Y1 Si1 C53 -92.87(18) . . . . ? N2 Y1 Si1 C53 -131.65(14) . . . . ? N4 Y1 Si1 C53 79.54(13) . . . . ? N1 Y1 Si1 C53 -30.94(16) . . . . ? N3 Y1 Si1 C53 147.88(13) . . . . ? O1 Y1 Si1 C53 7.80(13) . . . . ? N5 Y1 N1 C21 -90.8(2) . . . . ? N2 Y1 N1 C21 -5.92(19) . . . . ? N4 Y1 N1 C21 122.1(2) . . . . ? N3 Y1 N1 C21 59.9(2) . . . . ? O1 Y1 N1 C21 -160.7(2) . . . . ? Si1 Y1 N1 C21 -121.51(18) . . . . ? N5 Y1 N1 C2 106.8(2) . . . . ? N2 Y1 N1 C2 -168.4(2) . . . . ? N4 Y1 N1 C2 -40.4(2) . . . . ? N3 Y1 N1 C2 -102.5(2) . . . . ? O1 Y1 N1 C2 36.85(19) . . . . ? Si1 Y1 N1 C2 76.0(2) . . . . ? N5 Y1 N2 C25 -46.2(3) . . . . ? N4 Y1 N2 C25 113.8(3) . . . . ? N1 Y1 N2 C25 -176.0(3) . . . . ? N3 Y1 N2 C25 52.9(3) . . . . ? O1 Y1 N2 C25 -137.9(3) . . . . ? Si1 Y1 N2 C25 -30.0(3) . . . . ? N5 Y1 N2 C22 132.7(2) . . . . ? N4 Y1 N2 C22 -67.3(2) . . . . ? N1 Y1 N2 C22 2.91(19) . . . . ? N3 Y1 N2 C22 -128.2(2) . . . . ? O1 Y1 N2 C22 41.0(2) . . . . ? Si1 Y1 N2 C22 148.93(18) . . . . ? N5 Y1 N3 C47 -125.8(2) . . . . ? N2 Y1 N3 C47 136.2(2) . . . . ? N4 Y1 N3 C47 6.98(19) . . . . ? N1 Y1 N3 C47 76.4(2) . . . . ? O1 Y1 N3 C47 -33.0(2) . . . . ? Si1 Y1 N3 C47 -102.78(19) . . . . ? N5 Y1 N3 C28 51.0(2) . . . . ? N2 Y1 N3 C28 -47.0(2) . . . . ? N4 Y1 N3 C28 -176.2(2) . . . . ? N1 Y1 N3 C28 -106.8(2) . . . . ? O1 Y1 N3 C28 143.76(19) . . . . ? Si1 Y1 N3 C28 74.0(2) . . . . ? N5 Y1 N4 C51 -102.9(3) . . . . ? N2 Y1 N4 C51 104.8(3) . . . . ? N1 Y1 N4 C51 42.4(3) . . . . ? N3 Y1 N4 C51 172.0(3) . . . . ? O1 Y1 N4 C51 -34.3(3) . . . . ? Si1 Y1 N4 C51 -107.5(3) . . . . ? N5 Y1 N4 C48 79.9(2) . . . . ? N2 Y1 N4 C48 -72.4(2) . . . . ? N1 Y1 N4 C48 -134.88(19) . . . . ? N3 Y1 N4 C48 -5.26(18) . . . . ? O1 Y1 N4 C48 148.4(2) . . . . ? Si1 Y1 N4 C48 75.26(19) . . . . ? C54 Si1 N5 Si2 169.91(16) . . . . ? C55 Si1 N5 Si2 49.7(2) . . . . ? C53 Si1 N5 Si2 -72.8(2) . . . . ? Y1 Si1 N5 Si2 -178.3(2) . . . . ? C54 Si1 N5 Y1 -11.82(19) . . . . ? C55 Si1 N5 Y1 -132.07(14) . . . . ? C53 Si1 N5 Y1 105.47(16) . . . . ? C56 Si2 N5 Si1 37.5(2) . . . . ? C57 Si2 N5 Si1 -81.49(19) . . . . ? C58 Si2 N5 Si1 158.60(15) . . . . ? C56 Si2 N5 Y1 -140.69(14) . . . . ? C57 Si2 N5 Y1 100.28(16) . . . . ? C58 Si2 N5 Y1 -19.63(17) . . . . ? N2 Y1 N5 Si1 146.84(13) . . . . ? N4 Y1 N5 Si1 -10.00(19) . . . . ? N1 Y1 N5 Si1 -141.78(11) . . . . ? N3 Y1 N5 Si1 62.28(14) . . . . ? O1 Y1 N5 Si1 -75.43(13) . . . . ? N2 Y1 N5 Si2 -34.87(15) . . . . ? N4 Y1 N5 Si2 168.28(11) . . . . ? N1 Y1 N5 Si2 36.50(18) . . . . ? N3 Y1 N5 Si2 -119.44(13) . . . . ? O1 Y1 N5 Si2 102.86(14) . . . . ? Si1 Y1 N5 Si2 178.3(2) . . . . ? N5 Y1 O1 C12 -74.11(17) . . . . ? N2 Y1 O1 C12 23.2(2) . . . . ? N4 Y1 O1 C12 148.58(17) . . . . ? N1 Y1 O1 C12 59.88(16) . . . . ? N3 Y1 O1 C12 -172.92(16) . . . . ? Si1 Y1 O1 C12 -99.96(16) . . . . ? N5 Y1 O1 C26 97.8(2) . . . . ? N2 Y1 O1 C26 -164.9(2) . . . . ? N4 Y1 O1 C26 -39.5(2) . . . . ? N1 Y1 O1 C26 -128.2(2) . . . . ? N3 Y1 O1 C26 -1.0(3) . . . . ? Si1 Y1 O1 C26 72.0(2) . . . . ? C6 C1 C2 C3 -1.6(4) . . . . ? C11 C1 C2 C3 177.8(3) . . . . ? C6 C1 C2 N1 174.5(2) . . . . ? C11 C1 C2 N1 -6.1(4) . . . . ? C21 N1 C2 C3 -58.5(4) . . . . ? Y1 N1 C2 C3 103.4(3) . . . . ? C21 N1 C2 C1 125.4(3) . . . . ? Y1 N1 C2 C1 -72.7(3) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? N1 C2 C3 C4 -175.9(3) . . . . ? C2 C3 C4 C5 1.1(5) . . . . ? C3 C4 C5 C6 -1.0(4) . . . . ? C3 C4 C5 C10 178.6(3) . . . . ? C4 C5 C6 C1 -0.4(4) . . . . ? C10 C5 C6 C1 180.0(3) . . . . ? C4 C5 C6 C7 177.3(3) . . . . ? C10 C5 C6 C7 -2.3(4) . . . . ? C2 C1 C6 C5 1.7(4) . . . . ? C11 C1 C6 C5 -177.7(3) . . . . ? C2 C1 C6 C7 -176.1(3) . . . . ? C11 C1 C6 C7 4.6(4) . . . . ? C5 C6 C7 C8 -14.9(4) . . . . ? C1 C6 C7 C8 162.8(3) . . . . ? C6 C7 C8 C9 48.0(4) . . . . ? C7 C8 C9 C10 -64.5(3) . . . . ? C4 C5 C10 C9 166.3(3) . . . . ? C6 C5 C10 C9 -14.1(4) . . . . ? C8 C9 C10 C5 46.5(3) . . . . ? C2 C1 C11 C12 75.4(3) . . . . ? C6 C1 C11 C12 -105.2(3) . . . . ? C2 C1 C11 C16 -106.0(3) . . . . ? C6 C1 C11 C16 73.3(4) . . . . ? C16 C11 C12 C13 -4.4(4) . . . . ? C1 C11 C12 C13 174.2(2) . . . . ? C16 C11 C12 O1 173.1(2) . . . . ? C1 C11 C12 O1 -8.3(4) . . . . ? C26 O1 C12 C13 -81.9(3) . . . . ? Y1 O1 C12 C13 91.8(2) . . . . ? C26 O1 C12 C11 100.5(3) . . . . ? Y1 O1 C12 C11 -85.7(2) . . . . ? C11 C12 C13 C14 2.4(4) . . . . ? O1 C12 C13 C14 -175.0(2) . . . . ? C12 C13 C14 C15 0.8(4) . . . . ? C13 C14 C15 C16 -2.0(4) . . . . ? C13 C14 C15 C20 179.4(3) . . . . ? C14 C15 C16 C11 0.0(4) . . . . ? C20 C15 C16 C11 178.5(3) . . . . ? C14 C15 C16 C17 176.8(3) . . . . ? C20 C15 C16 C17 -4.7(4) . . . . ? C12 C11 C16 C15 3.1(4) . . . . ? C1 C11 C16 C15 -175.5(2) . . . . ? C12 C11 C16 C17 -173.8(2) . . . . ? C1 C11 C16 C17 7.7(4) . . . . ? C15 C16 C17 C18 17.8(4) . . . . ? C11 C16 C17 C18 -165.4(3) . . . . ? C16 C17 C18 C19 -46.9(4) . . . . ? C17 C18 C19 C20 62.9(4) . . . . ? C16 C15 C20 C19 20.5(4) . . . . ? C14 C15 C20 C19 -161.0(3) . . . . ? C18 C19 C20 C15 -48.7(4) . . . . ? C2 N1 C21 C22 172.4(3) . . . . ? Y1 N1 C21 C22 8.5(3) . . . . ? C25 N2 C22 C23 -0.2(4) . . . . ? Y1 N2 C22 C23 -179.4(2) . . . . ? C25 N2 C22 C21 179.3(3) . . . . ? Y1 N2 C22 C21 0.0(3) . . . . ? N1 C21 C22 N2 -6.0(4) . . . . ? N1 C21 C22 C23 173.3(3) . . . . ? N2 C22 C23 C24 0.9(4) . . . . ? C21 C22 C23 C24 -178.5(3) . . . . ? C22 C23 C24 C25 -1.2(4) . . . . ? C22 N2 C25 C24 -0.6(4) . . . . ? Y1 N2 C25 C24 178.4(2) . . . . ? C23 C24 C25 N2 1.2(4) . . . . ? C32 C27 C28 C29 -2.3(4) . . . . ? C37 C27 C28 C29 178.3(3) . . . . ? C32 C27 C28 N3 -179.4(2) . . . . ? C37 C27 C28 N3 1.2(4) . . . . ? C47 N3 C28 C29 139.3(3) . . . . ? Y1 N3 C28 C29 -37.3(3) . . . . ? C47 N3 C28 C27 -43.5(4) . . . . ? Y1 N3 C28 C27 139.9(2) . . . . ? C27 C28 C29 C30 2.9(4) . . . . ? N3 C28 C29 C30 -179.9(2) . . . . ? C28 C29 C30 C31 -1.2(4) . . . . ? C29 C30 C31 C32 -0.9(4) . . . . ? C29 C30 C31 C36 176.6(3) . . . . ? C30 C31 C32 C27 1.4(4) . . . . ? C36 C31 C32 C27 -176.0(3) . . . . ? C30 C31 C32 C33 -176.9(3) . . . . ? C36 C31 C32 C33 5.7(4) . . . . ? C28 C27 C32 C31 0.2(4) . . . . ? C37 C27 C32 C31 179.6(3) . . . . ? C28 C27 C32 C33 178.6(3) . . . . ? C37 C27 C32 C33 -2.1(4) . . . . ? C31 C32 C33 C34 -23.6(4) . . . . ? C27 C32 C33 C34 158.1(3) . . . . ? C32 C33 C34 C35 50.9(3) . . . . ? C33 C34 C35 C36 -60.1(3) . . . . ? C30 C31 C36 C35 168.2(3) . . . . ? C32 C31 C36 C35 -14.4(4) . . . . ? C34 C35 C36 C31 41.2(4) . . . . ? C28 C27 C37 C38 102.8(3) . . . . ? C32 C27 C37 C38 -76.5(4) . . . . ? C28 C27 C37 C42 -74.7(4) . . . . ? C32 C27 C37 C42 106.0(3) . . . . ? C52 O2 C38 C39 -6.1(4) . . . . ? C52 O2 C38 C37 176.5(3) . . . . ? C42 C37 C38 O2 -179.4(3) . . . . ? C27 C37 C38 O2 3.1(4) . . . . ? C42 C37 C38 C39 3.1(4) . . . . ? C27 C37 C38 C39 -174.4(3) . . . . ? O2 C38 C39 C40 -178.5(3) . . . . ? C37 C38 C39 C40 -1.2(5) . . . . ? C38 C39 C40 C41 -1.5(5) . . . . ? C39 C40 C41 C42 2.2(6) . . . . ? C39 C40 C41 C46 174.5(4) . . . . ? C39 C40 C41 C46' -162.6(7) . . . . ? C38 C37 C42 C41 -2.4(4) . . . . ? C27 C37 C42 C41 175.1(3) . . . . ? C38 C37 C42 C43' -174.2(8) . . . . ? C27 C37 C42 C43' 3.3(8) . . . . ? C38 C37 C42 C43 172.9(5) . . . . ? C27 C37 C42 C43 -9.6(6) . . . . ? C40 C41 C42 C37 -0.2(5) . . . . ? C46 C41 C42 C37 -171.6(5) . . . . ? C46' C41 C42 C37 166.6(6) . . . . ? C40 C41 C42 C43' 171.9(8) . . . . ? C46 C41 C42 C43' 0.4(10) . . . . ? C46' C41 C42 C43' -21.4(10) . . . . ? C40 C41 C42 C43 -175.3(6) . . . . ? C46 C41 C42 C43 13.3(8) . . . . ? C46' C41 C42 C43 -8.5(8) . . . . ? C37 C42 C43 C44 -172.4(5) . . . . ? C41 C42 C43 C44 2.8(9) . . . . ? C43' C42 C43 C44 78(5) . . . . ? C42 C43 C44 C45 -42.0(10) . . . . ? C43 C44 C45 C46 66.2(9) . . . . ? C40 C41 C46 C45 -161.8(4) . . . . ? C42 C41 C46 C45 10.0(8) . . . . ? C46' C41 C46 C45 71.2(17) . . . . ? C44 C45 C46 C41 -45.4(7) . . . . ? C37 C42 C43' C44' -171.1(12) . . . . ? C41 C42 C43' C44' 17.1(17) . . . . ? C43 C42 C43' C44' -95(5) . . . . ? C42 C43' C44' C45' 24(2) . . . . ? C43' C44' C45' C46' -52.0(15) . . . . ? C44' C45' C46' C41 52.5(14) . . . . ? C40 C41 C46' C45' 151.1(8) . . . . ? C42 C41 C46' C45' -14.4(13) . . . . ? C46 C41 C46' C45' -144(3) . . . . ? C28 N3 C47 C48 174.6(2) . . . . ? Y1 N3 C47 C48 -8.2(3) . . . . ? C51 N4 C48 C49 0.4(3) . . . . ? Y1 N4 C48 C49 178.6(2) . . . . ? C51 N4 C48 C47 -174.7(3) . . . . ? Y1 N4 C48 C47 3.5(3) . . . . ? N3 C47 C48 C49 -170.5(3) . . . . ? N3 C47 C48 N4 3.5(4) . . . . ? N4 C48 C49 C50 -0.8(4) . . . . ? C47 C48 C49 C50 173.7(3) . . . . ? C48 C49 C50 C51 0.8(4) . . . . ? C48 N4 C51 C50 0.1(3) . . . . ? Y1 N4 C51 C50 -177.3(2) . . . . ? C49 C50 C51 N4 -0.5(4) . . . . ? C64 C59 C60 C61 -1.2(8) . . . . ? C59 C60 C61 C62 1.3(7) . . . . ? C60 C61 C62 C63 -0.8(8) . . . . ? C61 C62 C63 C64 0.3(8) . . . . ? C60 C59 C64 C63 0.7(8) . . . . ? C62 C63 C64 C59 -0.2(8) . . . . ? C70 C65 C66 C67 -0.4(7) . . . . ? C65 C66 C67 C68 -0.8(8) . . . . ? C66 C67 C68 C69 1.1(9) . . . . ? C67 C68 C69 C70 -0.3(8) . . . . ? C66 C65 C70 C69 1.2(8) . . . . ? C68 C69 C70 C65 -0.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.259 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.057 # Attachment 'compound_9.cif' data_9 _database_code_depnum_ccdc_archive 'CCDC 687849' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H84 N5 O2 Si2 Yb' _chemical_formula_sum 'C70 H84 N5 O2 Si2 Yb' _chemical_formula_weight 1256.64 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 11.7812(5) _cell_length_b 13.4201(4) _cell_length_c 40.2693(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6366.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 12999 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2612 _exptl_absorpt_coefficient_mu 1.554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7067 _exptl_absorpt_correction_T_max 0.7891 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 53730 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.91 _reflns_number_total 14944 _reflns_number_gt 14095 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(8) _refine_ls_number_reflns 14944 _refine_ls_number_parameters 715 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1404 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.651213(19) 0.075760(18) 0.863290(5) 0.01684(7) Uani 1 1 d . . . Si1 Si 0.57385(14) 0.22252(14) 0.79852(4) 0.0234(4) Uani 1 1 d . . . Si2 Si 0.38305(14) 0.15408(13) 0.84206(4) 0.0222(3) Uani 1 1 d . . . N1 N 0.6371(4) -0.0826(4) 0.89072(10) 0.0211(9) Uani 1 1 d . . . N2 N 0.5636(4) 0.0957(4) 0.91489(11) 0.0236(11) Uani 1 1 d . . . N3 N 0.7683(4) 0.2144(4) 0.88240(10) 0.0182(9) Uani 1 1 d . . . N4 N 0.8416(4) 0.0344(4) 0.85606(10) 0.0208(9) Uani 1 1 d . . . N5 N 0.5228(4) 0.1569(4) 0.83255(11) 0.0203(10) Uani 1 1 d . . . O1 O 0.6493(3) -0.0462(3) 0.81677(8) 0.0196(7) Uani 1 1 d . . . O2 O 1.0022(4) 0.4296(4) 0.91025(10) 0.0358(11) Uani 1 1 d . . . C1 C 0.5431(5) -0.1882(4) 0.83503(12) 0.0208(11) Uani 1 1 d . . . C2 C 0.5490(5) -0.1040(4) 0.81614(13) 0.0212(12) Uani 1 1 d . . . C3 C 0.4552(5) -0.0728(5) 0.79733(12) 0.0203(10) Uani 1 1 d . . . H3 H 0.4595 -0.0148 0.7839 0.024 Uiso 1 1 calc R . . C4 C 0.3588(5) -0.1269(5) 0.79879(13) 0.0254(12) Uani 1 1 d . . . H4 H 0.2967 -0.1084 0.7850 0.030 Uiso 1 1 calc R . . C5 C 0.3469(5) -0.2086(4) 0.81967(12) 0.0207(11) Uani 1 1 d . . . C6 C 0.4389(5) -0.2416(4) 0.83814(13) 0.0192(11) Uani 1 1 d . . . C7 C 0.4324(5) -0.3299(5) 0.86213(16) 0.0295(13) Uani 1 1 d . . . H7A H 0.5016 -0.3711 0.8598 0.035 Uiso 1 1 calc R . . H7B H 0.4296 -0.3047 0.8852 0.035 Uiso 1 1 calc R . . C8 C 0.3294(6) -0.3937(5) 0.85568(19) 0.0400(18) Uani 1 1 d . . . H8A H 0.3188 -0.4400 0.8746 0.048 Uiso 1 1 calc R . . H8B H 0.3427 -0.4342 0.8355 0.048 Uiso 1 1 calc R . . C9 C 0.2192(6) -0.3315(6) 0.85094(18) 0.0373(17) Uani 1 1 d . . . H9A H 0.1535 -0.3765 0.8476 0.045 Uiso 1 1 calc R . . H9B H 0.2047 -0.2905 0.8709 0.045 Uiso 1 1 calc R . . C10 C 0.2339(5) -0.2647(5) 0.82084(15) 0.0276(13) Uani 1 1 d . . . H10A H 0.1713 -0.2155 0.8205 0.033 Uiso 1 1 calc R . . H10B H 0.2271 -0.3060 0.8006 0.033 Uiso 1 1 calc R . . C11 C 0.6527(5) -0.2257(4) 0.85302(13) 0.0192(11) Uani 1 1 d . . . C12 C 0.6914(5) -0.1758(4) 0.88047(13) 0.0169(11) Uani 1 1 d . . . C13 C 0.7848(5) -0.2098(5) 0.89714(13) 0.0241(13) Uani 1 1 d . . . H13 H 0.8127 -0.1758 0.9161 0.029 Uiso 1 1 calc R . . C14 C 0.8378(5) -0.2956(5) 0.88546(13) 0.0234(12) Uani 1 1 d . . . H14 H 0.9001 -0.3213 0.8977 0.028 Uiso 1 1 calc R . . C15 C 0.8049(5) -0.3455(5) 0.85702(14) 0.0233(12) Uani 1 1 d . . . C16 C 0.7101(5) -0.3094(5) 0.84004(14) 0.0216(12) Uani 1 1 d . . . C17 C 0.6711(6) -0.3585(5) 0.80837(14) 0.0278(14) Uani 1 1 d . . . H17A H 0.6513 -0.3061 0.7921 0.033 Uiso 1 1 calc R . . H17B H 0.6015 -0.3973 0.8130 0.033 Uiso 1 1 calc R . . C18 C 0.7589(5) -0.4271(5) 0.79308(13) 0.0267(12) Uani 1 1 d . . . H18A H 0.8216 -0.3872 0.7835 0.032 Uiso 1 1 calc R . . H18B H 0.7239 -0.4666 0.7750 0.032 Uiso 1 1 calc R . . C19 C 0.8052(6) -0.4965(5) 0.81973(15) 0.0294(14) Uani 1 1 d . . . H19A H 0.8576 -0.5456 0.8097 0.035 Uiso 1 1 calc R . . H19B H 0.7422 -0.5332 0.8304 0.035 Uiso 1 1 calc R . . C20 C 0.8683(5) -0.4336(5) 0.84553(14) 0.0295(13) Uani 1 1 d . . . H20A H 0.8859 -0.4761 0.8650 0.035 Uiso 1 1 calc R . . H20B H 0.9412 -0.4113 0.8359 0.035 Uiso 1 1 calc R . . C21 C 0.7197(5) -0.0640(6) 0.78821(14) 0.0292(14) Uani 1 1 d . . . H21A H 0.7375 -0.1352 0.7867 0.044 Uiso 1 1 calc R . . H21B H 0.7902 -0.0259 0.7903 0.044 Uiso 1 1 calc R . . H21C H 0.6793 -0.0432 0.7681 0.044 Uiso 1 1 calc R . . C22 C 0.5993(5) -0.0795(5) 0.92083(12) 0.0220(11) Uani 1 1 d . . . H22 H 0.6016 -0.1377 0.9343 0.026 Uiso 1 1 calc R . . C23 C 0.5545(6) 0.0100(4) 0.93385(13) 0.0241(12) Uani 1 1 d . . . C24 C 0.4968(6) 0.0300(5) 0.96382(15) 0.0324(15) Uani 1 1 d . . . H24 H 0.4775 -0.0165 0.9807 0.039 Uiso 1 1 calc R . . C25 C 0.4744(6) 0.1308(5) 0.96352(15) 0.0316(15) Uani 1 1 d . . . H25 H 0.4396 0.1678 0.9809 0.038 Uiso 1 1 calc R . . C26 C 0.5113(5) 0.1685(5) 0.93366(14) 0.0263(13) Uani 1 1 d . . . H26 H 0.5020 0.2358 0.9268 0.032 Uiso 1 1 calc R . . C27 C 0.8987(5) 0.3042(5) 0.93801(13) 0.0237(12) Uani 1 1 d . . . C28 C 1.0056(5) 0.3457(5) 0.92969(13) 0.0215(12) Uani 1 1 d . . . C29 C 1.1048(5) 0.2978(6) 0.94006(16) 0.0347(16) Uani 1 1 d . . . H29 H 1.1763 0.3246 0.9338 0.042 Uiso 1 1 calc R . . C30 C 1.1013(5) 0.2147(6) 0.9587(2) 0.0431(19) Uani 1 1 d . A . H30 H 1.1702 0.1831 0.9649 0.052 Uiso 1 1 calc R . . C31 C 0.9962(7) 0.1734(5) 0.9692(2) 0.048(2) Uani 1 1 d D . . C32 C 0.8944(5) 0.2189(5) 0.95857(13) 0.0259(13) Uani 1 1 d . A . C33 C 0.7826(6) 0.1765(5) 0.96857(15) 0.0352(16) Uani 1 1 d D . . H33A H 0.7460 0.1457 0.9499 0.042 Uiso 0.546(11) 1 d PR A 1 H33B H 0.7345 0.2288 0.9767 0.042 Uiso 0.546(11) 1 d PR A 1 H33C H 0.7409 0.1623 0.9486 0.042 Uiso 0.454(11) 1 d PR A 2 H33D H 0.7423 0.2282 0.9801 0.042 Uiso 0.454(11) 1 d PR A 2 C34 C 0.8034(11) 0.0993(10) 0.9960(3) 0.034(3) Uani 0.546(11) 1 d PD A 1 H34A H 0.8291 0.1336 1.0164 0.041 Uiso 0.546(11) 1 calc PR A 1 H34B H 0.7314 0.0644 1.0011 0.041 Uiso 0.546(11) 1 calc PR A 1 C35 C 0.8924(9) 0.0236(7) 0.9854(4) 0.046(4) Uani 0.546(11) 1 d PD A 1 H35A H 0.8737 -0.0024 0.9630 0.055 Uiso 0.546(11) 1 calc PR A 1 H35B H 0.8931 -0.0331 1.0011 0.055 Uiso 0.546(11) 1 calc PR A 1 C36 C 1.0097(9) 0.0732(8) 0.9847(3) 0.039(3) Uani 0.546(11) 1 d PDU A 1 H36A H 1.0397 0.0799 1.0075 0.047 Uiso 0.546(11) 1 calc PR A 1 H36B H 1.0634 0.0323 0.9716 0.047 Uiso 0.546(11) 1 calc PR A 1 C34' C 0.7777(12) 0.0828(11) 0.9906(4) 0.034(3) Uani 0.454(11) 1 d PD A 2 H34C H 0.7889 0.0223 0.9770 0.041 Uiso 0.454(11) 1 calc PR A 2 H34D H 0.7029 0.0782 1.0017 0.041 Uiso 0.454(11) 1 calc PR A 2 C35' C 0.8731(10) 0.0918(11) 1.0167(3) 0.038(4) Uani 0.454(11) 1 d PD A 2 H35C H 0.8721 0.0338 1.0319 0.045 Uiso 0.454(11) 1 calc PR A 2 H35D H 0.8633 0.1532 1.0300 0.045 Uiso 0.454(11) 1 calc PR A 2 C36' C 0.9867(10) 0.0956(11) 0.9970(3) 0.039(3) Uani 0.454(11) 1 d PDU A 2 H36C H 1.0489 0.1078 1.0130 0.047 Uiso 0.454(11) 1 calc PR A 2 H36D H 0.9997 0.0290 0.9871 0.047 Uiso 0.454(11) 1 calc PR A 2 C37 C 0.7911(5) 0.3512(4) 0.92411(13) 0.0202(11) Uani 1 1 d . . . C38 C 0.7336(5) 0.3061(4) 0.89774(13) 0.0172(11) Uani 1 1 d . . . C39 C 0.6348(5) 0.3485(4) 0.88555(13) 0.0207(11) Uani 1 1 d . . . H39 H 0.5940 0.3172 0.8681 0.025 Uiso 1 1 calc R . . C40 C 0.5959(5) 0.4378(5) 0.89924(13) 0.0213(12) Uani 1 1 d . . . H40 H 0.5284 0.4673 0.8909 0.026 Uiso 1 1 calc R . . C41 C 0.6544(6) 0.4843(4) 0.92495(13) 0.0251(12) Uani 1 1 d . . . C42 C 0.7512(5) 0.4407(5) 0.93758(13) 0.0241(13) Uani 1 1 d . . . C43 C 0.8111(6) 0.4898(5) 0.96671(14) 0.0268(13) Uani 1 1 d . . . H43A H 0.8940 0.4800 0.9642 0.032 Uiso 1 1 calc R . . H43B H 0.7874 0.4561 0.9874 0.032 Uiso 1 1 calc R . . C44 C 0.7872(6) 0.6010(5) 0.97001(15) 0.0325(15) Uani 1 1 d . . . H44A H 0.8194 0.6256 0.9912 0.039 Uiso 1 1 calc R . . H44B H 0.8250 0.6371 0.9516 0.039 Uiso 1 1 calc R . . C45 C 0.6640(7) 0.6221(5) 0.96919(14) 0.0339(15) Uani 1 1 d . . . H45A H 0.6520 0.6947 0.9719 0.041 Uiso 1 1 calc R . . H45B H 0.6272 0.5883 0.9882 0.041 Uiso 1 1 calc R . . C46 C 0.6070(5) 0.5878(5) 0.93698(14) 0.0271(13) Uani 1 1 d . . . H46A H 0.6199 0.6383 0.9195 0.033 Uiso 1 1 calc R . . H46B H 0.5241 0.5823 0.9406 0.033 Uiso 1 1 calc R . . C47 C 1.1050(6) 0.4762(7) 0.90265(19) 0.047(2) Uani 1 1 d . . . H47A H 1.1489 0.4860 0.9231 0.070 Uiso 1 1 calc R . . H47B H 1.0900 0.5410 0.8923 0.070 Uiso 1 1 calc R . . H47C H 1.1483 0.4344 0.8872 0.070 Uiso 1 1 calc R . . C48 C 0.8738(5) 0.2002(5) 0.87614(13) 0.0238(13) Uani 1 1 d . . . H48 H 0.9254 0.2531 0.8805 0.029 Uiso 1 1 calc R . . C49 C 0.9168(5) 0.1117(4) 0.86334(14) 0.0222(11) Uani 1 1 d . . . C50 C 1.0340(5) 0.0774(5) 0.86035(14) 0.0257(12) Uani 1 1 d . . . H50 H 1.1017 0.1133 0.8649 0.031 Uiso 1 1 calc R . . C51 C 1.0232(5) -0.0189(5) 0.84935(15) 0.0274(13) Uani 1 1 d . . . H51 H 1.0845 -0.0617 0.8437 0.033 Uiso 1 1 calc R . . C52 C 0.9119(6) -0.0437(5) 0.84772(15) 0.0289(14) Uani 1 1 d . . . H52 H 0.8852 -0.1079 0.8415 0.035 Uiso 1 1 calc R . . C53 C 0.7341(5) 0.2328(5) 0.79919(14) 0.0286(14) Uani 1 1 d . . . H53A H 0.7564 0.2921 0.8118 0.043 Uiso 1 1 calc R . . H53B H 0.7626 0.2384 0.7764 0.043 Uiso 1 1 calc R . . H53C H 0.7664 0.1733 0.8097 0.043 Uiso 1 1 calc R . . C54 C 0.5401(6) 0.1625(5) 0.75728(14) 0.0313(14) Uani 1 1 d . . . H54A H 0.5907 0.1056 0.7537 0.047 Uiso 1 1 calc R . . H54B H 0.5509 0.2112 0.7394 0.047 Uiso 1 1 calc R . . H54C H 0.4611 0.1396 0.7573 0.047 Uiso 1 1 calc R . . C55 C 0.5164(7) 0.3540(6) 0.79615(17) 0.0398(18) Uani 1 1 d . . . H55A H 0.4339 0.3518 0.7933 0.060 Uiso 1 1 calc R . . H55B H 0.5508 0.3886 0.7772 0.060 Uiso 1 1 calc R . . H55C H 0.5348 0.3896 0.8167 0.060 Uiso 1 1 calc R . . C56 C 0.3503(5) 0.0418(5) 0.86913(14) 0.0264(12) Uani 1 1 d . . . H56A H 0.4016 -0.0130 0.8633 0.040 Uiso 1 1 calc R . . H56B H 0.2716 0.0209 0.8655 0.040 Uiso 1 1 calc R . . H56C H 0.3608 0.0596 0.8925 0.040 Uiso 1 1 calc R . . C57 C 0.2872(5) 0.1484(5) 0.80437(14) 0.0293(14) Uani 1 1 d . . . H57A H 0.2985 0.2082 0.7908 0.044 Uiso 1 1 calc R . . H57B H 0.2079 0.1450 0.8116 0.044 Uiso 1 1 calc R . . H57C H 0.3056 0.0891 0.7912 0.044 Uiso 1 1 calc R . . C58 C 0.3342(5) 0.2694(5) 0.86437(16) 0.0294(13) Uani 1 1 d . . . H58A H 0.3810 0.2797 0.8842 0.044 Uiso 1 1 calc R . . H58B H 0.2546 0.2614 0.8709 0.044 Uiso 1 1 calc R . . H58C H 0.3414 0.3270 0.8496 0.044 Uiso 1 1 calc R . . C59 C 0.0996(4) 0.3709(3) 0.79546(11) 0.088(4) Uani 1 1 d G . . H59 H 0.1354 0.3388 0.8137 0.105 Uiso 1 1 calc R . . C60 C 0.0335(5) 0.3160(4) 0.77351(11) 0.074(3) Uani 1 1 d G . . H60 H 0.0241 0.2463 0.7767 0.088 Uiso 1 1 calc R . . C61 C -0.0190(3) 0.3629(4) 0.74684(10) 0.067(3) Uani 1 1 d G . . H61 H -0.0642 0.3254 0.7318 0.080 Uiso 1 1 calc R . . C62 C -0.0053(4) 0.4648(4) 0.74214(9) 0.090(5) Uani 1 1 d G . . H62 H -0.0411 0.4969 0.7239 0.108 Uiso 1 1 calc R . . C63 C 0.0608(4) 0.5198(4) 0.76409(8) 0.075(3) Uani 1 1 d G . . H63 H 0.0702 0.5894 0.7609 0.089 Uiso 1 1 calc R . . C64 C 0.1133(3) 0.4728(4) 0.79076(8) 0.062(3) Uani 1 1 d G . . H64 H 0.1585 0.5103 0.8058 0.075 Uiso 1 1 calc R . . C65 C 0.3031(5) 0.7471(5) 0.95082(11) 0.075(3) Uani 1 1 d GU . . H65 H 0.3800 0.7283 0.9541 0.090 Uiso 1 1 calc R . . C66 C 0.2161(5) 0.6858(4) 0.96214(9) 0.083(3) Uani 1 1 d GU . . H66 H 0.2336 0.6252 0.9732 0.100 Uiso 1 1 calc R . . C67 C 0.1036(5) 0.7133(5) 0.95729(9) 0.079(3) Uani 1 1 d GU . . H67 H 0.0442 0.6714 0.9650 0.095 Uiso 1 1 calc R . . C68 C 0.0780(5) 0.8020(5) 0.94112(11) 0.086(3) Uani 1 1 d GU . . H68 H 0.0011 0.8208 0.9378 0.103 Uiso 1 1 calc R . . C69 C 0.1649(6) 0.8632(4) 0.92980(11) 0.091(4) Uani 1 1 d GU . . H69 H 0.1474 0.9239 0.9187 0.109 Uiso 1 1 calc R . . C70 C 0.2775(5) 0.8358(4) 0.93465(11) 0.079(3) Uani 1 1 d GU . . H70 H 0.3369 0.8776 0.9269 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01602(11) 0.01794(13) 0.01657(10) -0.00118(9) 0.00041(9) -0.00050(10) Si1 0.0262(9) 0.0226(9) 0.0215(7) 0.0034(6) -0.0021(6) -0.0039(7) Si2 0.0187(8) 0.0235(9) 0.0245(7) -0.0012(6) -0.0021(6) 0.0016(7) N1 0.023(2) 0.019(2) 0.0210(19) -0.0010(18) -0.0004(17) -0.003(2) N2 0.024(2) 0.024(3) 0.022(2) -0.0019(19) 0.0022(18) 0.000(2) N3 0.020(2) 0.017(3) 0.0175(19) -0.0015(17) -0.0016(17) -0.009(2) N4 0.012(2) 0.024(3) 0.026(2) -0.0021(18) 0.0038(17) 0.003(2) N5 0.024(3) 0.018(3) 0.019(2) -0.0019(17) -0.0051(18) -0.003(2) O1 0.0169(18) 0.021(2) 0.0211(16) -0.0013(14) 0.0067(15) 0.0001(17) O2 0.024(2) 0.048(3) 0.035(2) 0.010(2) -0.0070(17) -0.016(2) C1 0.021(3) 0.024(3) 0.018(2) -0.003(2) 0.001(2) -0.003(2) C2 0.026(3) 0.018(3) 0.020(2) -0.0042(19) 0.000(2) 0.004(2) C3 0.024(3) 0.014(3) 0.023(2) -0.003(2) -0.003(2) 0.007(3) C4 0.020(3) 0.032(3) 0.024(2) -0.002(2) -0.005(2) -0.001(3) C5 0.017(2) 0.018(3) 0.027(2) -0.008(2) 0.000(2) 0.001(3) C6 0.021(3) 0.014(3) 0.022(2) -0.006(2) -0.001(2) -0.005(2) C7 0.028(3) 0.031(4) 0.030(3) 0.009(3) -0.006(3) -0.010(3) C8 0.035(4) 0.031(4) 0.054(4) 0.013(3) -0.013(3) -0.008(3) C9 0.024(3) 0.046(5) 0.042(3) 0.008(3) 0.000(3) 0.009(3) C10 0.020(3) 0.027(4) 0.036(3) 0.000(3) 0.000(2) 0.002(3) C11 0.020(3) 0.007(2) 0.031(3) 0.0014(19) 0.002(2) 0.009(3) C12 0.014(2) 0.015(3) 0.022(2) -0.002(2) 0.0006(19) 0.000(2) C13 0.028(3) 0.024(3) 0.020(2) 0.002(2) 0.000(2) -0.005(3) C14 0.016(3) 0.027(3) 0.027(2) 0.003(2) -0.004(2) 0.007(3) C15 0.016(3) 0.022(3) 0.031(3) 0.003(2) 0.000(2) -0.002(2) C16 0.013(3) 0.026(3) 0.026(3) -0.003(2) 0.001(2) 0.000(2) C17 0.032(4) 0.027(3) 0.024(3) -0.007(2) -0.009(2) 0.013(3) C18 0.032(3) 0.020(3) 0.029(3) -0.007(3) 0.003(2) 0.005(3) C19 0.028(3) 0.028(4) 0.033(3) -0.005(3) -0.002(2) 0.009(3) C20 0.021(3) 0.034(4) 0.034(3) -0.003(3) -0.002(2) 0.010(3) C21 0.022(3) 0.038(4) 0.027(3) -0.005(3) 0.008(2) -0.002(3) C22 0.027(3) 0.019(3) 0.020(2) -0.003(2) -0.002(2) 0.001(3) C23 0.032(3) 0.017(3) 0.022(2) -0.001(2) 0.003(2) 0.004(3) C24 0.039(4) 0.031(4) 0.027(3) 0.004(3) 0.013(3) -0.004(3) C25 0.031(4) 0.032(4) 0.032(3) -0.003(3) 0.013(3) -0.003(3) C26 0.031(3) 0.023(3) 0.025(3) -0.007(2) 0.002(2) 0.002(3) C27 0.023(3) 0.028(3) 0.020(2) -0.005(2) -0.006(2) 0.002(3) C28 0.017(3) 0.028(3) 0.019(2) -0.002(2) -0.005(2) 0.000(2) C29 0.010(3) 0.053(5) 0.041(3) -0.010(3) -0.011(2) -0.001(3) C30 0.012(3) 0.037(4) 0.081(5) -0.004(4) -0.020(3) 0.005(3) C31 0.048(5) 0.035(5) 0.063(5) 0.007(4) -0.035(4) -0.008(4) C32 0.032(3) 0.022(3) 0.024(3) -0.004(2) -0.007(2) -0.001(3) C33 0.038(4) 0.037(4) 0.031(3) 0.005(3) -0.012(3) -0.010(3) C34 0.047(7) 0.027(6) 0.029(5) 0.008(5) -0.011(5) -0.001(5) C35 0.033(7) 0.035(8) 0.069(9) 0.038(7) 0.002(6) 0.009(6) C36 0.042(5) 0.027(5) 0.047(5) -0.014(4) -0.012(4) 0.021(4) C34' 0.047(7) 0.027(6) 0.029(5) 0.008(5) -0.011(5) -0.001(5) C35' 0.043(9) 0.023(9) 0.048(8) 0.012(6) -0.013(7) 0.001(7) C36' 0.042(5) 0.027(5) 0.047(5) -0.014(4) -0.012(4) 0.021(4) C37 0.021(3) 0.021(3) 0.018(2) 0.001(2) -0.001(2) -0.003(2) C38 0.018(3) 0.011(3) 0.023(2) 0.0018(19) 0.001(2) -0.001(2) C39 0.020(3) 0.017(3) 0.025(2) -0.002(2) -0.003(2) 0.001(2) C40 0.015(3) 0.017(3) 0.032(3) 0.004(2) -0.002(2) -0.004(2) C41 0.032(3) 0.016(3) 0.027(2) 0.004(2) 0.004(3) 0.014(3) C42 0.029(3) 0.025(4) 0.019(2) -0.002(2) -0.001(2) -0.001(3) C43 0.032(3) 0.022(3) 0.026(3) -0.005(2) -0.007(2) 0.002(3) C44 0.043(4) 0.030(4) 0.025(3) -0.005(2) -0.002(3) 0.001(3) C45 0.058(5) 0.016(3) 0.028(3) -0.002(2) 0.003(3) -0.002(3) C46 0.031(3) 0.018(3) 0.033(3) 0.004(2) 0.002(2) 0.000(3) C47 0.019(3) 0.069(6) 0.052(4) 0.000(4) 0.002(3) -0.010(4) C48 0.025(3) 0.023(3) 0.024(2) -0.004(2) 0.000(2) -0.002(2) C49 0.023(3) 0.019(3) 0.024(2) -0.005(2) 0.003(2) -0.001(2) C50 0.020(3) 0.027(3) 0.030(3) -0.012(3) 0.008(2) 0.000(3) C51 0.011(3) 0.031(4) 0.040(3) -0.008(3) 0.000(2) 0.010(2) C52 0.031(3) 0.024(3) 0.032(3) -0.006(2) 0.006(3) 0.001(3) C53 0.024(3) 0.037(4) 0.025(3) -0.001(3) -0.004(2) -0.016(3) C54 0.035(4) 0.039(4) 0.020(3) 0.007(2) -0.006(2) -0.009(3) C55 0.049(4) 0.040(4) 0.031(3) 0.009(3) -0.013(3) -0.004(4) C56 0.016(3) 0.030(3) 0.032(3) 0.003(2) 0.003(2) -0.007(3) C57 0.027(3) 0.033(4) 0.028(3) 0.000(3) -0.004(2) 0.007(3) C58 0.024(3) 0.024(3) 0.041(3) -0.003(3) -0.002(3) 0.007(3) C59 0.039(5) 0.129(11) 0.095(8) -0.036(8) -0.021(5) 0.032(7) C60 0.045(5) 0.059(7) 0.117(9) -0.032(6) -0.003(5) 0.004(5) C61 0.039(5) 0.088(8) 0.074(6) -0.036(6) -0.001(4) -0.011(5) C62 0.037(5) 0.186(15) 0.046(5) 0.011(7) 0.017(4) 0.037(7) C63 0.055(6) 0.065(7) 0.104(8) 0.013(6) 0.049(6) 0.012(5) C64 0.035(4) 0.053(6) 0.099(7) -0.049(5) -0.002(4) 0.010(4) C65 0.082(6) 0.080(6) 0.063(5) -0.034(5) -0.009(4) 0.007(5) C66 0.107(7) 0.072(6) 0.071(6) -0.018(5) -0.010(5) 0.007(6) C67 0.059(5) 0.092(7) 0.088(6) -0.038(5) 0.010(5) -0.040(5) C68 0.054(5) 0.115(8) 0.088(6) -0.046(6) -0.019(5) -0.002(6) C69 0.132(8) 0.075(6) 0.065(5) -0.016(5) -0.015(6) 0.007(7) C70 0.101(7) 0.091(7) 0.046(4) 0.002(5) 0.015(5) 0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N5 2.237(5) . ? Yb1 N4 2.329(5) . ? Yb1 N2 2.336(4) . ? Yb1 N1 2.401(5) . ? Yb1 N3 2.441(5) . ? Yb1 O1 2.488(3) . ? Si1 N5 1.737(5) . ? Si1 C54 1.888(6) . ? Si1 C55 1.892(8) . ? Si1 C53 1.893(6) . ? Si2 N5 1.691(5) . ? Si2 C58 1.879(6) . ? Si2 C57 1.893(6) . ? Si2 C56 1.899(6) . ? N1 C22 1.292(7) . ? N1 C12 1.465(7) . ? N2 C26 1.381(7) . ? N2 C23 1.384(7) . ? N3 C48 1.283(8) . ? N3 C38 1.436(7) . ? N4 C52 1.378(8) . ? N4 C49 1.395(7) . ? O1 C2 1.413(7) . ? O1 C21 1.438(6) . ? O2 C28 1.371(8) . ? O2 C47 1.398(8) . ? C1 C2 1.364(8) . ? C1 C6 1.427(8) . ? C1 C11 1.564(8) . ? C2 C3 1.403(7) . ? C3 C4 1.350(8) . ? C3 H3 0.9500 . ? C4 C5 1.389(8) . ? C4 H4 0.9500 . ? C5 C6 1.387(8) . ? C5 C10 1.531(8) . ? C6 C7 1.531(8) . ? C7 C8 1.507(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.556(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.517(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.370(7) . ? C11 C16 1.412(8) . ? C12 C13 1.366(8) . ? C13 C14 1.392(9) . ? C13 H13 0.9500 . ? C14 C15 1.383(8) . ? C14 H14 0.9500 . ? C15 C16 1.396(8) . ? C15 C20 1.473(9) . ? C16 C17 1.507(8) . ? C17 C18 1.516(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.522(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.531(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.413(8) . ? C22 H22 0.9500 . ? C23 C24 1.411(8) . ? C24 C25 1.380(10) . ? C24 H24 0.9500 . ? C25 C26 1.374(8) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.414(9) . ? C27 C28 1.417(8) . ? C27 C37 1.523(8) . ? C28 C29 1.398(8) . ? C29 C30 1.344(11) . ? C29 H29 0.9500 . ? C30 C31 1.421(11) . ? C30 H30 0.9500 . ? C31 C32 1.411(9) . ? C31 C36 1.491(9) . ? C31 C36' 1.536(9) . ? C32 C33 1.491(9) . ? C33 C34 1.535(9) . ? C33 C34' 1.540(9) . ? C33 H33A 0.9601 . ? C33 H33B 0.9599 . ? C33 H33C 0.9601 . ? C33 H33D 0.9599 . ? C34 C35 1.522(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.533(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C34' C35' 1.544(9) . ? C34' H34C 0.9900 . ? C34' H34D 0.9900 . ? C35' C36' 1.556(9) . ? C35' H35C 0.9900 . ? C35' H35D 0.9900 . ? C36' H36C 0.9900 . ? C36' H36D 0.9900 . ? C37 C38 1.396(7) . ? C37 C42 1.399(8) . ? C38 C39 1.385(8) . ? C39 C40 1.397(8) . ? C39 H39 0.9500 . ? C40 C41 1.391(8) . ? C40 H40 0.9500 . ? C41 C42 1.380(8) . ? C41 C46 1.572(8) . ? C42 C43 1.519(8) . ? C43 C44 1.525(9) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.480(10) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.531(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.391(8) . ? C48 H48 0.9500 . ? C49 C50 1.460(8) . ? C50 C51 1.372(9) . ? C50 H50 0.9500 . ? C51 C52 1.354(9) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.3900 . ? C59 C64 1.3900 . ? C59 H59 0.9500 . ? C60 C61 1.3900 . ? C60 H60 0.9500 . ? C61 C62 1.3900 . ? C61 H61 0.9500 . ? C62 C63 1.3900 . ? C62 H62 0.9500 . ? C63 C64 1.3900 . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C66 1.3900 . ? C65 C70 1.3900 . ? C65 H65 0.9500 . ? C66 C67 1.3900 . ? C66 H66 0.9500 . ? C67 C68 1.3899 . ? C67 H67 0.9500 . ? C68 C69 1.3900 . ? C68 H68 0.9500 . ? C69 C70 1.3901 . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Yb1 N4 134.25(16) . . ? N5 Yb1 N2 97.92(17) . . ? N4 Yb1 N2 124.35(16) . . ? N5 Yb1 N1 129.67(17) . . ? N4 Yb1 N1 85.03(16) . . ? N2 Yb1 N1 70.21(16) . . ? N5 Yb1 N3 100.70(17) . . ? N4 Yb1 N3 71.14(17) . . ? N2 Yb1 N3 83.22(16) . . ? N1 Yb1 N3 124.67(15) . . ? N5 Yb1 O1 84.10(15) . . ? N4 Yb1 O1 75.99(15) . . ? N2 Yb1 O1 137.83(15) . . ? N1 Yb1 O1 76.31(13) . . ? N3 Yb1 O1 138.10(14) . . ? N5 Si1 C54 113.9(3) . . ? N5 Si1 C55 112.9(3) . . ? C54 Si1 C55 106.1(3) . . ? N5 Si1 C53 111.8(3) . . ? C54 Si1 C53 104.7(3) . . ? C55 Si1 C53 106.8(3) . . ? N5 Si2 C58 112.9(3) . . ? N5 Si2 C57 113.6(3) . . ? C58 Si2 C57 103.5(3) . . ? N5 Si2 C56 110.2(3) . . ? C58 Si2 C56 108.4(3) . . ? C57 Si2 C56 107.9(3) . . ? C22 N1 C12 116.3(5) . . ? C22 N1 Yb1 115.3(4) . . ? C12 N1 Yb1 126.6(3) . . ? C26 N2 C23 104.6(5) . . ? C26 N2 Yb1 140.0(4) . . ? C23 N2 Yb1 115.5(4) . . ? C48 N3 C38 119.2(5) . . ? C48 N3 Yb1 111.9(4) . . ? C38 N3 Yb1 128.9(3) . . ? C52 N4 C49 103.6(5) . . ? C52 N4 Yb1 142.3(4) . . ? C49 N4 Yb1 114.1(3) . . ? Si2 N5 Si1 121.8(3) . . ? Si2 N5 Yb1 121.5(2) . . ? Si1 N5 Yb1 116.7(2) . . ? C2 O1 C21 112.1(4) . . ? C2 O1 Yb1 112.5(3) . . ? C21 O1 Yb1 134.9(4) . . ? C28 O2 C47 117.8(5) . . ? C2 C1 C6 120.6(5) . . ? C2 C1 C11 118.8(5) . . ? C6 C1 C11 120.6(5) . . ? C1 C2 C3 120.5(6) . . ? C1 C2 O1 119.1(5) . . ? C3 C2 O1 120.3(5) . . ? C4 C3 C2 118.6(6) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 122.4(5) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C6 C5 C4 119.9(5) . . ? C6 C5 C10 120.4(5) . . ? C4 C5 C10 119.6(5) . . ? C5 C6 C1 117.7(5) . . ? C5 C6 C7 123.1(5) . . ? C1 C6 C7 119.2(5) . . ? C8 C7 C6 111.8(5) . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 112.8(6) . . ? C7 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C8 108.6(5) . . ? C10 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? C10 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.3 . . ? C9 C10 C5 114.5(5) . . ? C9 C10 H10A 108.6 . . ? C5 C10 H10A 108.6 . . ? C9 C10 H10B 108.6 . . ? C5 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? C12 C11 C16 121.9(5) . . ? C12 C11 C1 119.4(5) . . ? C16 C11 C1 118.7(5) . . ? C13 C12 C11 120.1(5) . . ? C13 C12 N1 119.9(5) . . ? C11 C12 N1 119.9(5) . . ? C12 C13 C14 118.1(5) . . ? C12 C13 H13 120.9 . . ? C14 C13 H13 120.9 . . ? C15 C14 C13 123.7(5) . . ? C15 C14 H14 118.1 . . ? C13 C14 H14 118.1 . . ? C14 C15 C16 117.5(6) . . ? C14 C15 C20 120.5(5) . . ? C16 C15 C20 122.0(5) . . ? C15 C16 C11 118.6(5) . . ? C15 C16 C17 120.4(5) . . ? C11 C16 C17 121.0(5) . . ? C16 C17 C18 113.7(5) . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C17 C18 C19 109.3(5) . . ? C17 C18 H18A 109.8 . . ? C19 C18 H18A 109.8 . . ? C17 C18 H18B 109.8 . . ? C19 C18 H18B 109.8 . . ? H18A C18 H18B 108.3 . . ? C18 C19 C20 108.3(5) . . ? C18 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? C18 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? C15 C20 C19 114.2(5) . . ? C15 C20 H20A 108.7 . . ? C19 C20 H20A 108.7 . . ? C15 C20 H20B 108.7 . . ? C19 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C23 120.3(6) . . ? N1 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? N2 C23 C24 110.6(5) . . ? N2 C23 C22 118.2(5) . . ? C24 C23 C22 131.2(6) . . ? C25 C24 C23 105.7(6) . . ? C25 C24 H24 127.1 . . ? C23 C24 H24 127.1 . . ? C26 C25 C24 107.9(6) . . ? C26 C25 H25 126.0 . . ? C24 C25 H25 126.0 . . ? C25 C26 N2 111.1(6) . . ? C25 C26 H26 124.5 . . ? N2 C26 H26 124.5 . . ? C32 C27 C28 119.3(5) . . ? C32 C27 C37 121.4(5) . . ? C28 C27 C37 119.4(5) . . ? O2 C28 C29 124.9(6) . . ? O2 C28 C27 115.6(5) . . ? C29 C28 C27 119.4(6) . . ? C30 C29 C28 121.5(6) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C29 C30 C31 121.1(6) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 118.8(6) . . ? C32 C31 C36 127.4(7) . . ? C30 C31 C36 112.5(7) . . ? C32 C31 C36' 116.9(8) . . ? C30 C31 C36' 123.1(7) . . ? C36 C31 C36' 24.4(6) . . ? C31 C32 C27 119.8(6) . . ? C31 C32 C33 120.3(6) . . ? C27 C32 C33 119.9(5) . . ? C32 C33 C34 108.2(7) . . ? C32 C33 C34' 120.0(7) . . ? C34 C33 C34' 16.2(10) . . ? C32 C33 H33A 110.5 . . ? C34 C33 H33A 110.1 . . ? C34' C33 H33A 94.7 . . ? C32 C33 H33B 109.6 . . ? C34 C33 H33B 109.9 . . ? C34' C33 H33B 112.2 . . ? H33A C33 H33B 108.5 . . ? C32 C33 H33C 107.6 . . ? C34 C33 H33C 123.3 . . ? C34' C33 H33C 107.5 . . ? H33A C33 H33C 14.2 . . ? H33B C33 H33C 97.4 . . ? C32 C33 H33D 107.0 . . ? C34 C33 H33D 102.7 . . ? C34' C33 H33D 107.1 . . ? H33A C33 H33D 117.8 . . ? H33B C33 H33D 9.7 . . ? H33C C33 H33D 107.0 . . ? C35 C34 C33 110.9(8) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.0 . . ? C34 C35 C36 109.7(8) . . ? C34 C35 H35A 109.7 . . ? C36 C35 H35A 109.7 . . ? C34 C35 H35B 109.7 . . ? C36 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C31 C36 C35 107.6(7) . . ? C31 C36 H36A 110.2 . . ? C35 C36 H36A 110.2 . . ? C31 C36 H36B 110.2 . . ? C35 C36 H36B 110.2 . . ? H36A C36 H36B 108.5 . . ? C33 C34' C35' 107.5(8) . . ? C33 C34' H34C 110.2 . . ? C35' C34' H34C 110.2 . . ? C33 C34' H34D 110.2 . . ? C35' C34' H34D 110.2 . . ? H34C C34' H34D 108.5 . . ? C34' C35' C36' 106.4(8) . . ? C34' C35' H35C 110.5 . . ? C36' C35' H35C 110.5 . . ? C34' C35' H35D 110.5 . . ? C36' C35' H35D 110.5 . . ? H35C C35' H35D 108.6 . . ? C31 C36' C35' 117.2(9) . . ? C31 C36' H36C 108.0 . . ? C35' C36' H36C 108.0 . . ? C31 C36' H36D 108.0 . . ? C35' C36' H36D 108.0 . . ? H36C C36' H36D 107.3 . . ? C38 C37 C42 120.2(5) . . ? C38 C37 C27 120.3(5) . . ? C42 C37 C27 119.5(5) . . ? C39 C38 C37 119.9(5) . . ? C39 C38 N3 116.0(5) . . ? C37 C38 N3 124.0(5) . . ? C38 C39 C40 119.2(5) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? C41 C40 C39 121.1(5) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C42 C41 C40 119.5(5) . . ? C42 C41 C46 123.7(6) . . ? C40 C41 C46 116.7(5) . . ? C41 C42 C37 119.9(5) . . ? C41 C42 C43 119.0(5) . . ? C37 C42 C43 121.1(5) . . ? C42 C43 C44 114.0(5) . . ? C42 C43 H43A 108.8 . . ? C44 C43 H43A 108.8 . . ? C42 C43 H43B 108.8 . . ? C44 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? C45 C44 C43 111.5(6) . . ? C45 C44 H44A 109.3 . . ? C43 C44 H44A 109.3 . . ? C45 C44 H44B 109.3 . . ? C43 C44 H44B 109.3 . . ? H44A C44 H44B 108.0 . . ? C44 C45 C46 113.1(5) . . ? C44 C45 H45A 109.0 . . ? C46 C45 H45A 109.0 . . ? C44 C45 H45B 109.0 . . ? C46 C45 H45B 109.0 . . ? H45A C45 H45B 107.8 . . ? C45 C46 C41 111.8(5) . . ? C45 C46 H46A 109.3 . . ? C41 C46 H46A 109.3 . . ? C45 C46 H46B 109.3 . . ? C41 C46 H46B 109.3 . . ? H46A C46 H46B 107.9 . . ? O2 C47 H47A 109.5 . . ? O2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N3 C48 C49 123.6(6) . . ? N3 C48 H48 118.2 . . ? C49 C48 H48 118.2 . . ? C48 C49 N4 118.8(5) . . ? C48 C49 C50 130.1(5) . . ? N4 C49 C50 110.4(5) . . ? C51 C50 C49 103.6(5) . . ? C51 C50 H50 128.2 . . ? C49 C50 H50 128.2 . . ? C52 C51 C50 109.7(5) . . ? C52 C51 H51 125.2 . . ? C50 C51 H51 125.2 . . ? C51 C52 N4 112.5(6) . . ? C51 C52 H52 123.7 . . ? N4 C52 H52 123.7 . . ? Si1 C53 H53A 109.5 . . ? Si1 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si1 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? Si1 C54 H54A 109.5 . . ? Si1 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? Si1 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Si1 C55 H55A 109.5 . . ? Si1 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? Si1 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? Si2 C56 H56A 109.5 . . ? Si2 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? Si2 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? Si2 C57 H57A 109.5 . . ? Si2 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? Si2 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? Si2 C58 H58A 109.5 . . ? Si2 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? Si2 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 C64 120.0 . . ? C60 C59 H59 120.0 . . ? C64 C59 H59 120.0 . . ? C59 C60 C61 120.0 . . ? C59 C60 H60 120.0 . . ? C61 C60 H60 120.0 . . ? C62 C61 C60 120.0 . . ? C62 C61 H61 120.0 . . ? C60 C61 H61 120.0 . . ? C63 C62 C61 120.0 . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C63 C64 C59 120.0 . . ? C63 C64 H64 120.0 . . ? C59 C64 H64 120.0 . . ? C66 C65 C70 120.0 . . ? C66 C65 H65 120.0 . . ? C70 C65 H65 120.0 . . ? C67 C66 C65 120.0 . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C68 C67 C66 120.0 . . ? C68 C67 H67 120.0 . . ? C66 C67 H67 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C68 C69 C70 120.0 . . ? C68 C69 H69 120.0 . . ? C70 C69 H69 120.0 . . ? C65 C70 C69 120.0 . . ? C65 C70 H70 120.0 . . ? C69 C70 H70 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Yb1 N1 C22 -89.8(4) . . . . ? N4 Yb1 N1 C22 123.3(4) . . . . ? N2 Yb1 N1 C22 -6.0(4) . . . . ? N3 Yb1 N1 C22 60.3(4) . . . . ? O1 Yb1 N1 C22 -160.0(4) . . . . ? N5 Yb1 N1 C12 106.4(4) . . . . ? N4 Yb1 N1 C12 -40.5(4) . . . . ? N2 Yb1 N1 C12 -169.8(4) . . . . ? N3 Yb1 N1 C12 -103.5(4) . . . . ? O1 Yb1 N1 C12 36.2(4) . . . . ? N5 Yb1 N2 C26 -45.3(6) . . . . ? N4 Yb1 N2 C26 116.3(6) . . . . ? N1 Yb1 N2 C26 -174.7(7) . . . . ? N3 Yb1 N2 C26 54.7(6) . . . . ? O1 Yb1 N2 C26 -135.2(6) . . . . ? N5 Yb1 N2 C23 131.9(4) . . . . ? N4 Yb1 N2 C23 -66.5(5) . . . . ? N1 Yb1 N2 C23 2.5(4) . . . . ? N3 Yb1 N2 C23 -128.1(4) . . . . ? O1 Yb1 N2 C23 42.0(5) . . . . ? N5 Yb1 N3 C48 -127.1(4) . . . . ? N4 Yb1 N3 C48 6.2(4) . . . . ? N2 Yb1 N3 C48 136.1(4) . . . . ? N1 Yb1 N3 C48 75.9(4) . . . . ? O1 Yb1 N3 C48 -34.0(5) . . . . ? N5 Yb1 N3 C38 50.4(4) . . . . ? N4 Yb1 N3 C38 -176.3(4) . . . . ? N2 Yb1 N3 C38 -46.5(4) . . . . ? N1 Yb1 N3 C38 -106.7(4) . . . . ? O1 Yb1 N3 C38 143.5(4) . . . . ? N5 Yb1 N4 C52 -101.8(6) . . . . ? N2 Yb1 N4 C52 104.2(6) . . . . ? N1 Yb1 N4 C52 42.3(6) . . . . ? N3 Yb1 N4 C52 171.5(6) . . . . ? O1 Yb1 N4 C52 -34.8(6) . . . . ? N5 Yb1 N4 C49 81.1(4) . . . . ? N2 Yb1 N4 C49 -72.9(4) . . . . ? N1 Yb1 N4 C49 -134.8(4) . . . . ? N3 Yb1 N4 C49 -5.5(4) . . . . ? O1 Yb1 N4 C49 148.1(4) . . . . ? C58 Si2 N5 Si1 -79.8(4) . . . . ? C57 Si2 N5 Si1 37.7(4) . . . . ? C56 Si2 N5 Si1 158.8(3) . . . . ? C58 Si2 N5 Yb1 100.3(3) . . . . ? C57 Si2 N5 Yb1 -142.3(3) . . . . ? C56 Si2 N5 Yb1 -21.1(4) . . . . ? C54 Si1 N5 Si2 -72.9(4) . . . . ? C55 Si1 N5 Si2 48.2(4) . . . . ? C53 Si1 N5 Si2 168.7(3) . . . . ? C54 Si1 N5 Yb1 107.1(3) . . . . ? C55 Si1 N5 Yb1 -131.8(3) . . . . ? C53 Si1 N5 Yb1 -11.3(4) . . . . ? N4 Yb1 N5 Si2 167.6(2) . . . . ? N2 Yb1 N5 Si2 -33.9(3) . . . . ? N1 Yb1 N5 Si2 36.9(4) . . . . ? N3 Yb1 N5 Si2 -118.4(3) . . . . ? O1 Yb1 N5 Si2 103.7(3) . . . . ? N4 Yb1 N5 Si1 -12.4(4) . . . . ? N2 Yb1 N5 Si1 146.2(3) . . . . ? N1 Yb1 N5 Si1 -143.0(2) . . . . ? N3 Yb1 N5 Si1 61.6(3) . . . . ? O1 Yb1 N5 Si1 -76.3(3) . . . . ? N5 Yb1 O1 C2 -73.0(3) . . . . ? N4 Yb1 O1 C2 148.6(3) . . . . ? N2 Yb1 O1 C2 22.3(4) . . . . ? N1 Yb1 O1 C2 60.3(3) . . . . ? N3 Yb1 O1 C2 -172.4(3) . . . . ? N5 Yb1 O1 C21 98.2(5) . . . . ? N4 Yb1 O1 C21 -40.3(5) . . . . ? N2 Yb1 O1 C21 -166.5(5) . . . . ? N1 Yb1 O1 C21 -128.5(5) . . . . ? N3 Yb1 O1 C21 -1.2(6) . . . . ? C6 C1 C2 C3 -5.1(8) . . . . ? C11 C1 C2 C3 174.5(5) . . . . ? C6 C1 C2 O1 172.4(5) . . . . ? C11 C1 C2 O1 -8.0(7) . . . . ? C21 O1 C2 C1 101.0(6) . . . . ? Yb1 O1 C2 C1 -85.7(5) . . . . ? C21 O1 C2 C3 -81.5(6) . . . . ? Yb1 O1 C2 C3 91.8(5) . . . . ? C1 C2 C3 C4 1.1(8) . . . . ? O1 C2 C3 C4 -176.4(5) . . . . ? C2 C3 C4 C5 3.9(8) . . . . ? C3 C4 C5 C6 -4.8(8) . . . . ? C3 C4 C5 C10 178.2(5) . . . . ? C4 C5 C6 C1 0.7(8) . . . . ? C10 C5 C6 C1 177.7(5) . . . . ? C4 C5 C6 C7 178.9(5) . . . . ? C10 C5 C6 C7 -4.0(8) . . . . ? C2 C1 C6 C5 4.1(8) . . . . ? C11 C1 C6 C5 -175.4(5) . . . . ? C2 C1 C6 C7 -174.2(5) . . . . ? C11 C1 C6 C7 6.3(8) . . . . ? C5 C6 C7 C8 17.2(8) . . . . ? C1 C6 C7 C8 -164.5(6) . . . . ? C6 C7 C8 C9 -45.9(8) . . . . ? C7 C8 C9 C10 61.7(8) . . . . ? C8 C9 C10 C5 -46.7(8) . . . . ? C6 C5 C10 C9 20.0(8) . . . . ? C4 C5 C10 C9 -163.0(6) . . . . ? C2 C1 C11 C12 74.1(7) . . . . ? C6 C1 C11 C12 -106.3(6) . . . . ? C2 C1 C11 C16 -104.9(6) . . . . ? C6 C1 C11 C16 74.7(7) . . . . ? C16 C11 C12 C13 -3.4(9) . . . . ? C1 C11 C12 C13 177.7(5) . . . . ? C16 C11 C12 N1 172.8(5) . . . . ? C1 C11 C12 N1 -6.2(8) . . . . ? C22 N1 C12 C13 -59.6(7) . . . . ? Yb1 N1 C12 C13 104.0(5) . . . . ? C22 N1 C12 C11 124.2(6) . . . . ? Yb1 N1 C12 C11 -72.1(6) . . . . ? C11 C12 C13 C14 -0.3(8) . . . . ? N1 C12 C13 C14 -176.4(5) . . . . ? C12 C13 C14 C15 3.4(9) . . . . ? C13 C14 C15 C16 -2.8(9) . . . . ? C13 C14 C15 C20 177.5(6) . . . . ? C14 C15 C16 C11 -0.9(8) . . . . ? C20 C15 C16 C11 178.8(6) . . . . ? C14 C15 C16 C17 178.4(6) . . . . ? C20 C15 C16 C17 -1.9(9) . . . . ? C12 C11 C16 C15 4.0(9) . . . . ? C1 C11 C16 C15 -177.1(5) . . . . ? C12 C11 C16 C17 -175.4(6) . . . . ? C1 C11 C16 C17 3.6(8) . . . . ? C15 C16 C17 C18 -15.5(8) . . . . ? C11 C16 C17 C18 163.8(6) . . . . ? C16 C17 C18 C19 48.7(7) . . . . ? C17 C18 C19 C20 -64.7(7) . . . . ? C14 C15 C20 C19 164.5(6) . . . . ? C16 C15 C20 C19 -15.2(9) . . . . ? C18 C19 C20 C15 47.9(7) . . . . ? C12 N1 C22 C23 174.5(5) . . . . ? Yb1 N1 C22 C23 9.0(7) . . . . ? C26 N2 C23 C24 0.3(7) . . . . ? Yb1 N2 C23 C24 -177.9(4) . . . . ? C26 N2 C23 C22 178.9(5) . . . . ? Yb1 N2 C23 C22 0.8(7) . . . . ? N1 C22 C23 N2 -6.8(9) . . . . ? N1 C22 C23 C24 171.6(7) . . . . ? N2 C23 C24 C25 -2.3(8) . . . . ? C22 C23 C24 C25 179.3(7) . . . . ? C23 C24 C25 C26 3.4(8) . . . . ? C24 C25 C26 N2 -3.4(8) . . . . ? C23 N2 C26 C25 1.9(7) . . . . ? Yb1 N2 C26 C25 179.3(5) . . . . ? C47 O2 C28 C29 -6.1(9) . . . . ? C47 O2 C28 C27 177.0(6) . . . . ? C32 C27 C28 O2 -178.7(5) . . . . ? C37 C27 C28 O2 2.5(8) . . . . ? C32 C27 C28 C29 4.3(8) . . . . ? C37 C27 C28 C29 -174.5(5) . . . . ? O2 C28 C29 C30 -178.8(6) . . . . ? C27 C28 C29 C30 -2.1(10) . . . . ? C28 C29 C30 C31 -1.4(11) . . . . ? C29 C30 C31 C32 2.6(12) . . . . ? C29 C30 C31 C36 170.6(9) . . . . ? C29 C30 C31 C36' -164.4(10) . . . . ? C30 C31 C32 C27 -0.3(11) . . . . ? C36 C31 C32 C27 -166.3(9) . . . . ? C36' C31 C32 C27 167.5(8) . . . . ? C30 C31 C32 C33 178.9(7) . . . . ? C36 C31 C32 C33 12.8(13) . . . . ? C36' C31 C32 C33 -13.3(12) . . . . ? C28 C27 C32 C31 -3.1(9) . . . . ? C37 C27 C32 C31 175.7(6) . . . . ? C28 C27 C32 C33 177.8(5) . . . . ? C37 C27 C32 C33 -3.4(8) . . . . ? C31 C32 C33 C34 12.2(10) . . . . ? C27 C32 C33 C34 -168.7(8) . . . . ? C31 C32 C33 C34' 0.1(13) . . . . ? C27 C32 C33 C34' 179.2(10) . . . . ? C32 C33 C34 C35 -52.3(12) . . . . ? C34' C33 C34 C35 87(4) . . . . ? C33 C34 C35 C36 71.2(13) . . . . ? C32 C31 C36 C35 3.4(15) . . . . ? C30 C31 C36 C35 -163.4(9) . . . . ? C36' C31 C36 C35 75.6(18) . . . . ? C34 C35 C36 C31 -42.7(13) . . . . ? C32 C33 C34' C35' 39.2(16) . . . . ? C34 C33 C34' C35' -6(3) . . . . ? C33 C34' C35' C36' -61.5(15) . . . . ? C32 C31 C36' C35' -14.2(16) . . . . ? C30 C31 C36' C35' 153.0(10) . . . . ? C36 C31 C36' C35' -136(2) . . . . ? C34' C35' C36' C31 52.6(15) . . . . ? C32 C27 C37 C38 -75.5(7) . . . . ? C28 C27 C37 C38 103.3(7) . . . . ? C32 C27 C37 C42 105.6(7) . . . . ? C28 C27 C37 C42 -75.6(7) . . . . ? C42 C37 C38 C39 -2.0(8) . . . . ? C27 C37 C38 C39 179.1(5) . . . . ? C42 C37 C38 N3 -180.0(5) . . . . ? C27 C37 C38 N3 1.1(8) . . . . ? C48 N3 C38 C39 139.0(6) . . . . ? Yb1 N3 C38 C39 -38.3(7) . . . . ? C48 N3 C38 C37 -43.0(8) . . . . ? Yb1 N3 C38 C37 139.7(5) . . . . ? C37 C38 C39 C40 2.0(8) . . . . ? N3 C38 C39 C40 -179.9(5) . . . . ? C38 C39 C40 C41 -0.3(8) . . . . ? C39 C40 C41 C42 -1.2(9) . . . . ? C39 C40 C41 C46 176.4(5) . . . . ? C40 C41 C42 C37 1.1(9) . . . . ? C46 C41 C42 C37 -176.3(5) . . . . ? C40 C41 C42 C43 -177.2(6) . . . . ? C46 C41 C42 C43 5.4(9) . . . . ? C38 C37 C42 C41 0.5(9) . . . . ? C27 C37 C42 C41 179.4(5) . . . . ? C38 C37 C42 C43 178.8(5) . . . . ? C27 C37 C42 C43 -2.3(8) . . . . ? C41 C42 C43 C44 -23.5(8) . . . . ? C37 C42 C43 C44 158.2(6) . . . . ? C42 C43 C44 C45 50.7(7) . . . . ? C43 C44 C45 C46 -59.8(7) . . . . ? C44 C45 C46 C41 39.9(7) . . . . ? C42 C41 C46 C45 -13.1(8) . . . . ? C40 C41 C46 C45 169.4(5) . . . . ? C38 N3 C48 C49 175.7(5) . . . . ? Yb1 N3 C48 C49 -6.6(7) . . . . ? N3 C48 C49 N4 1.6(9) . . . . ? N3 C48 C49 C50 -167.9(6) . . . . ? C52 N4 C49 C48 -173.5(5) . . . . ? Yb1 N4 C49 C48 4.7(7) . . . . ? C52 N4 C49 C50 -2.0(6) . . . . ? Yb1 N4 C49 C50 176.1(4) . . . . ? C48 C49 C50 C51 173.6(6) . . . . ? N4 C49 C50 C51 3.4(7) . . . . ? C49 C50 C51 C52 -3.5(7) . . . . ? C50 C51 C52 N4 2.5(8) . . . . ? C49 N4 C52 C51 -0.2(7) . . . . ? Yb1 N4 C52 C51 -177.4(4) . . . . ? C64 C59 C60 C61 0.0 . . . . ? C59 C60 C61 C62 0.0 . . . . ? C60 C61 C62 C63 0.0 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C59 0.0 . . . . ? C60 C59 C64 C63 0.0 . . . . ? C70 C65 C66 C67 0.0 . . . . ? C65 C66 C67 C68 0.0 . . . . ? C66 C67 C68 C69 0.0 . . . . ? C67 C68 C69 C70 0.0 . . . . ? C66 C65 C70 C69 0.0 . . . . ? C68 C69 C70 C65 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.203 _refine_diff_density_min -1.641 _refine_diff_density_rms 0.166 # Attachment 'compound_10.cif' data_10 _database_code_depnum_ccdc_archive 'CCDC 687850' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61.25 H56 N6 O2 Ti' _chemical_formula_sum 'C61.25 H56 N6 O2 Ti' _chemical_formula_weight 956.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.2184(17) _cell_length_b 19.767(2) _cell_length_c 19.104(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.488(2) _cell_angle_gamma 90.00 _cell_volume 5683.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5629 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 22.65 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2014 _exptl_absorpt_coefficient_mu 0.196 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.788925 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24624 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.02 _reflns_number_total 18458 _reflns_number_gt 11141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1541P)^2^+0.0744P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_number_reflns 18458 _refine_ls_number_parameters 1325 _refine_ls_number_restraints 136 _refine_ls_R_factor_all 0.1366 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2612 _refine_ls_wR_factor_gt 0.2108 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.19735(8) 0.65215(6) 0.55928(6) 0.0453(3) Uani 1 1 d . . . Ti2 Ti 0.67087(8) 0.75960(7) 0.95740(7) 0.0494(3) Uani 1 1 d . . . O1 O 0.1115(4) 0.3798(3) 0.6720(3) 0.0798(17) Uani 1 1 d . . . O2 O 0.1971(4) 0.8584(3) 0.3375(3) 0.0705(15) Uani 1 1 d . . . O3 O 0.6975(4) 0.5143(3) 1.1384(4) 0.0790(17) Uani 1 1 d . . . O4 O 0.5767(4) 0.9283(4) 0.6973(3) 0.0818(18) Uani 1 1 d . . . N1 N 0.2377(4) 0.5670(3) 0.4966(3) 0.0509(15) Uani 1 1 d . . . N2 N 0.1386(4) 0.5627(3) 0.6038(3) 0.0471(14) Uani 1 1 d . . . N3 N 0.0801(4) 0.6495(3) 0.4771(3) 0.0498(13) Uani 1 1 d . . . N4 N 0.2328(4) 0.7180(3) 0.4738(3) 0.0471(14) Uani 1 1 d . . . N5 N 0.3123(4) 0.6513(3) 0.6166(3) 0.0517(14) Uani 1 1 d . . . N6 N 0.1440(4) 0.7199(3) 0.6097(4) 0.0579(16) Uani 1 1 d . . . N7 N 0.6680(4) 0.6651(3) 0.8962(3) 0.0599(16) Uani 1 1 d . . . N8 N 0.6541(4) 0.6808(3) 1.0352(3) 0.0505(14) Uani 1 1 d . . . N9 N 0.5274(4) 0.7564(3) 0.9215(3) 0.0527(14) Uani 1 1 d . . . N10 N 0.6539(4) 0.8095(3) 0.8533(3) 0.0504(14) Uani 1 1 d . . . N11 N 0.7984(4) 0.7587(4) 0.9735(3) 0.0592(15) Uani 1 1 d . . . N12 N 0.6526(4) 0.8368(3) 1.0150(3) 0.0555(16) Uani 1 1 d . . . C1 C 0.2795(5) 0.5520(5) 0.4415(4) 0.060(2) Uani 1 1 d . . . H1A H 0.3087 0.5838 0.4173 0.073 Uiso 1 1 calc R . . C2 C 0.2743(6) 0.4850(5) 0.4249(5) 0.075(2) Uani 1 1 d . . . H2A H 0.2985 0.4638 0.3887 0.090 Uiso 1 1 calc R . . C3 C 0.2271(6) 0.4550(4) 0.4714(5) 0.068(2) Uani 1 1 d . . . H3A H 0.2137 0.4092 0.4737 0.082 Uiso 1 1 calc R . . C4 C 0.2023(5) 0.5064(4) 0.5150(4) 0.0537(18) Uani 1 1 d . . . C5 C 0.1520(4) 0.5062(4) 0.5709(4) 0.0487(17) Uani 1 1 d . . . H5A H 0.1281 0.4659 0.5847 0.058 Uiso 1 1 calc R . . C6 C 0.0867(4) 0.5574(3) 0.6593(4) 0.0431(15) Uani 1 1 d . . . C7 C 0.0107(5) 0.6002(4) 0.6568(4) 0.0562(19) Uani 1 1 d . . . H7A H -0.0027 0.6302 0.6193 0.067 Uiso 1 1 calc R . . C8 C -0.0425(5) 0.5980(4) 0.7077(5) 0.064(2) Uani 1 1 d . . . H8A H -0.0921 0.6260 0.7041 0.077 Uiso 1 1 calc R . . C9 C -0.0238(4) 0.5538(4) 0.7661(4) 0.0567(19) Uani 1 1 d . . . C10 C -0.0798(6) 0.5498(5) 0.8194(5) 0.079(3) Uani 1 1 d . . . H10A H -0.1305 0.5765 0.8161 0.095 Uiso 1 1 calc R . . C11 C -0.0593(7) 0.5065(6) 0.8758(6) 0.104(4) Uani 1 1 d . . . H11A H -0.0955 0.5049 0.9109 0.124 Uiso 1 1 calc R . . C12 C 0.0155(7) 0.4650(6) 0.8806(5) 0.095(3) Uani 1 1 d . . . H12A H 0.0287 0.4358 0.9188 0.113 Uiso 1 1 calc R . . C13 C 0.0690(5) 0.4672(5) 0.8297(5) 0.072(2) Uani 1 1 d . . . H13A H 0.1189 0.4395 0.8338 0.087 Uiso 1 1 calc R . . C14 C 0.0505(5) 0.5111(4) 0.7701(4) 0.0513(17) Uani 1 1 d . . . C15 C 0.1082(5) 0.5132(3) 0.7167(4) 0.0457(16) Uani 1 1 d . . . C16 C 0.1905(4) 0.4712(4) 0.7254(4) 0.0472(17) Uani 1 1 d . . . C17 C 0.2709(5) 0.5014(4) 0.7592(4) 0.0553(19) Uani 1 1 d . . . C18 C 0.2753(5) 0.5682(4) 0.7863(4) 0.059(2) Uani 1 1 d . . . H18A H 0.2237 0.5940 0.7820 0.071 Uiso 1 1 calc R . . C19 C 0.3522(6) 0.5954(6) 0.8183(5) 0.080(3) Uani 1 1 d . . . H19A H 0.3518 0.6392 0.8360 0.096 Uiso 1 1 calc R . . C20 C 0.4306(7) 0.5606(7) 0.8253(5) 0.091(3) Uani 1 1 d . . . H20A H 0.4833 0.5807 0.8461 0.110 Uiso 1 1 calc R . . C21 C 0.4293(6) 0.4954(6) 0.8009(5) 0.085(3) Uani 1 1 d . . . H21A H 0.4819 0.4707 0.8074 0.102 Uiso 1 1 calc R . . C22 C 0.3520(5) 0.4645(5) 0.7666(4) 0.062(2) Uani 1 1 d . . . C23 C 0.3486(6) 0.3973(5) 0.7414(5) 0.071(2) Uani 1 1 d . . . H23A H 0.4008 0.3721 0.7464 0.086 Uiso 1 1 calc R . . C24 C 0.2721(7) 0.3682(5) 0.7103(5) 0.080(3) Uani 1 1 d . . . H24A H 0.2721 0.3238 0.6944 0.096 Uiso 1 1 calc R . . C25 C 0.1919(5) 0.4061(4) 0.7022(4) 0.0551(19) Uani 1 1 d . . . C26 C 0.1106(9) 0.3158(5) 0.6347(7) 0.113(4) Uani 1 1 d . . . H26A H 0.0504 0.3033 0.6174 0.170 Uiso 1 1 calc R . . H26B H 0.1377 0.2816 0.6665 0.170 Uiso 1 1 calc R . . H26C H 0.1433 0.3203 0.5957 0.170 Uiso 1 1 calc R . . C27 C 0.0013(5) 0.6198(4) 0.4620(5) 0.062(2) Uani 1 1 d . . . H27A H -0.0248 0.5938 0.4939 0.075 Uiso 1 1 calc R . . C28 C -0.0380(5) 0.6324(4) 0.3919(5) 0.069(2) Uani 1 1 d . . . H28A H -0.0927 0.6168 0.3697 0.082 Uiso 1 1 calc R . . C29 C 0.0223(5) 0.6732(4) 0.3625(4) 0.062(2) Uani 1 1 d . . . H29A H 0.0157 0.6904 0.3167 0.074 Uiso 1 1 calc R . . C30 C 0.0947(4) 0.6828(4) 0.4161(4) 0.0494(17) Uani 1 1 d . . . C31 C 0.1741(5) 0.7185(4) 0.4182(4) 0.0539(18) Uani 1 1 d . . . H31A H 0.1847 0.7429 0.3787 0.065 Uiso 1 1 calc R . . C32 C 0.3123(4) 0.7551(4) 0.4708(3) 0.0479(16) Uani 1 1 d . . . C33 C 0.3947(5) 0.7181(4) 0.4809(4) 0.0569(19) Uani 1 1 d . . . H33A H 0.3948 0.6723 0.4920 0.068 Uiso 1 1 calc R . . C34 C 0.4739(5) 0.7504(5) 0.4741(4) 0.062(2) Uani 1 1 d . . . H34A H 0.5266 0.7259 0.4812 0.075 Uiso 1 1 calc R . . C35 C 0.4760(5) 0.8171(5) 0.4572(4) 0.060(2) Uani 1 1 d . . . C36 C 0.5551(5) 0.8497(6) 0.4459(5) 0.077(3) Uani 1 1 d . . . H36A H 0.6075 0.8249 0.4503 0.093 Uiso 1 1 calc R . . C37 C 0.5572(7) 0.9161(7) 0.4288(7) 0.103(4) Uani 1 1 d . . . H37A H 0.6102 0.9363 0.4213 0.123 Uiso 1 1 calc R . . C38 C 0.4794(8) 0.9535(6) 0.4228(7) 0.108(4) Uani 1 1 d . . . H38A H 0.4809 0.9989 0.4100 0.130 Uiso 1 1 calc R . . C39 C 0.3989(6) 0.9255(5) 0.4353(6) 0.085(3) Uani 1 1 d . . . H39A H 0.3486 0.9524 0.4338 0.102 Uiso 1 1 calc R . . C40 C 0.3950(5) 0.8569(4) 0.4499(4) 0.0557(19) Uani 1 1 d . . . C41 C 0.3125(4) 0.8231(4) 0.4587(4) 0.0474(17) Uani 1 1 d . . . C42 C 0.2321(4) 0.8667(4) 0.4603(4) 0.0498(18) Uani 1 1 d . . . C43 C 0.2161(5) 0.8934(3) 0.5252(4) 0.0517(18) Uani 1 1 d . . . C44 C 0.2723(5) 0.8814(4) 0.5897(5) 0.066(2) Uani 1 1 d . . . H44A H 0.3228 0.8550 0.5895 0.079 Uiso 1 1 calc R . . C45 C 0.2549(7) 0.9073(5) 0.6520(5) 0.083(3) Uani 1 1 d . . . H45A H 0.2936 0.8987 0.6935 0.099 Uiso 1 1 calc R . . C46 C 0.1809(8) 0.9459(5) 0.6543(7) 0.090(3) Uani 1 1 d . . . H46A H 0.1704 0.9637 0.6974 0.108 Uiso 1 1 calc R . . C47 C 0.1231(7) 0.9586(5) 0.5959(6) 0.080(3) Uani 1 1 d . . . H47A H 0.0718 0.9834 0.5988 0.097 Uiso 1 1 calc R . . C48 C 0.1406(6) 0.9341(4) 0.5292(5) 0.067(2) Uani 1 1 d . . . C49 C 0.0826(6) 0.9460(5) 0.4657(6) 0.083(3) Uani 1 1 d . . . H49A H 0.0303 0.9698 0.4676 0.099 Uiso 1 1 calc R . . C50 C 0.1002(6) 0.9241(5) 0.4027(6) 0.075(3) Uani 1 1 d . . . H50A H 0.0625 0.9351 0.3614 0.090 Uiso 1 1 calc R . . C51 C 0.1764(5) 0.8844(4) 0.3997(5) 0.060(2) Uani 1 1 d . . . C52 C 0.1452(8) 0.8774(8) 0.2729(6) 0.116(4) Uani 1 1 d . . . H52A H 0.1682 0.8560 0.2343 0.174 Uiso 1 1 calc R . . H52B H 0.1474 0.9256 0.2676 0.174 Uiso 1 1 calc R . . H52C H 0.0848 0.8635 0.2731 0.174 Uiso 1 1 calc R . . C53 C 0.3733(6) 0.5948(5) 0.6242(5) 0.074(2) Uani 1 1 d . . . H53A H 0.4261 0.6072 0.6555 0.111 Uiso 1 1 calc R . . H53B H 0.3884 0.5830 0.5787 0.111 Uiso 1 1 calc R . . H53C H 0.3458 0.5568 0.6435 0.111 Uiso 1 1 calc R . . C54 C 0.3563(6) 0.7114(5) 0.6525(4) 0.070(2) Uani 1 1 d . . . H54A H 0.4131 0.6987 0.6777 0.105 Uiso 1 1 calc R . . H54B H 0.3200 0.7294 0.6851 0.105 Uiso 1 1 calc R . . H54C H 0.3642 0.7452 0.6178 0.105 Uiso 1 1 calc R . . C55 C 0.1586(7) 0.7288(5) 0.6876(5) 0.085(3) Uani 1 1 d . . . H55A H 0.1241 0.7664 0.7000 0.128 Uiso 1 1 calc R . . H55B H 0.2205 0.7372 0.7035 0.128 Uiso 1 1 calc R . . H55C H 0.1407 0.6885 0.7097 0.128 Uiso 1 1 calc R . . C56 C 0.0738(6) 0.7658(5) 0.5804(6) 0.080(3) Uani 1 1 d . . . H56A H 0.0583 0.7945 0.6173 0.121 Uiso 1 1 calc R . . H56B H 0.0226 0.7403 0.5602 0.121 Uiso 1 1 calc R . . H56C H 0.0939 0.7931 0.5443 0.121 Uiso 1 1 calc R . . C57 C 0.6752(5) 0.6404(5) 0.8316(4) 0.072(2) Uani 1 1 d . . . H57A H 0.6801 0.6667 0.7920 0.086 Uiso 1 1 calc R . . C58 C 0.6741(6) 0.5684(5) 0.8324(6) 0.084(3) Uani 1 1 d . . . H58A H 0.6778 0.5398 0.7943 0.100 Uiso 1 1 calc R . . C59 C 0.6668(6) 0.5499(5) 0.8981(5) 0.073(2) Uani 1 1 d . . . H59A H 0.6655 0.5057 0.9145 0.088 Uiso 1 1 calc R . . C60 C 0.6614(5) 0.6079(4) 0.9380(5) 0.064(2) Uani 1 1 d . . . C61 C 0.6521(5) 0.6194(4) 1.0091(4) 0.059(2) Uani 1 1 d . . . H61A H 0.6444 0.5828 1.0382 0.071 Uiso 1 1 calc R . . C62 C 0.6443(5) 0.6852(4) 1.1086(4) 0.0501(17) Uani 1 1 d . . . C63 C 0.5757(5) 0.7282(4) 1.1262(4) 0.0528(18) Uani 1 1 d . . . H63A H 0.5429 0.7541 1.0909 0.063 Uiso 1 1 calc R . . C64 C 0.5576(5) 0.7320(4) 1.1928(5) 0.063(2) Uani 1 1 d . . . H64A H 0.5110 0.7592 1.2024 0.076 Uiso 1 1 calc R . . C65 C 0.6075(5) 0.6960(4) 1.2484(4) 0.0580(19) Uani 1 1 d . . . C66 C 0.5887(7) 0.6967(6) 1.3183(5) 0.089(3) Uani 1 1 d . . . H66A H 0.5434 0.7245 1.3294 0.107 Uiso 1 1 calc R . . C67 C 0.6351(7) 0.6580(8) 1.3705(5) 0.119(5) Uani 1 1 d . . . H67A H 0.6208 0.6589 1.4162 0.142 Uiso 1 1 calc R . . C68 C 0.7053(7) 0.6165(7) 1.3541(5) 0.110(4) Uani 1 1 d . . . H68A H 0.7373 0.5897 1.3889 0.132 Uiso 1 1 calc R . . C69 C 0.7251(6) 0.6159(5) 1.2883(5) 0.082(3) Uani 1 1 d . . . H69A H 0.7717 0.5886 1.2788 0.098 Uiso 1 1 calc R . . C70 C 0.6793(4) 0.6546(5) 1.2326(4) 0.0574(18) Uani 1 1 d . . . C71 C 0.6982(4) 0.6524(4) 1.1620(4) 0.0498(16) Uani 1 1 d . . . C72 C 0.7796(5) 0.6131(4) 1.1488(4) 0.0580(19) Uani 1 1 d . . . C73 C 0.8648(5) 0.6490(5) 1.1546(4) 0.0601(19) Uani 1 1 d . . . C74 C 0.8725(6) 0.7183(5) 1.1702(5) 0.074(2) Uani 1 1 d . . . H74A H 0.8225 0.7427 1.1778 0.088 Uiso 1 1 calc R . . C75 C 0.9527(6) 0.7505(6) 1.1746(5) 0.085(3) Uani 1 1 d . . . H75A H 0.9560 0.7966 1.1842 0.102 Uiso 1 1 calc R . . C76 C 1.0285(7) 0.7159(8) 1.1650(6) 0.094(3) Uani 1 1 d . . . H76A H 1.0824 0.7387 1.1682 0.112 Uiso 1 1 calc R . . C77 C 1.0243(5) 0.6504(8) 1.1513(5) 0.092(3) Uani 1 1 d . . . H77A H 1.0762 0.6275 1.1456 0.111 Uiso 1 1 calc R . . C78 C 0.9418(6) 0.6134(6) 1.1449(5) 0.073(2) Uani 1 1 d . . . C79 C 0.9341(7) 0.5440(7) 1.1322(6) 0.098(3) Uani 1 1 d . . . H79A H 0.9848 0.5196 1.1263 0.118 Uiso 1 1 calc R . . C80 C 0.8543(7) 0.5102(6) 1.1280(6) 0.095(3) Uani 1 1 d . . . H80A H 0.8513 0.4641 1.1181 0.113 Uiso 1 1 calc R . . C81 C 0.7796(6) 0.5448(4) 1.1383(5) 0.065(2) Uani 1 1 d . . . C82 C 0.6906(8) 0.4462(6) 1.1219(7) 0.114(4) Uani 1 1 d . . . H82A H 0.6309 0.4312 1.1235 0.171 Uiso 1 1 calc R . . H82B H 0.7309 0.4210 1.1555 0.171 Uiso 1 1 calc R . . H82C H 0.7051 0.4392 1.0752 0.171 Uiso 1 1 calc R . . C83 C 0.4499(5) 0.7411(4) 0.9439(4) 0.059(2) Uani 1 1 d . . . H83A H 0.4456 0.7206 0.9871 0.070 Uiso 1 1 calc R . . C84 C 0.3780(5) 0.7594(4) 0.8956(4) 0.064(2) Uani 1 1 d . . . H84A H 0.3184 0.7535 0.9000 0.076 Uiso 1 1 calc R . . C85 C 0.4117(5) 0.7886(4) 0.8389(5) 0.067(2) Uani 1 1 d . . . H85A H 0.3794 0.8059 0.7977 0.081 Uiso 1 1 calc R . . C86 C 0.5029(5) 0.7864(4) 0.8563(4) 0.0546(19) Uani 1 1 d . . . C87 C 0.5726(5) 0.8127(4) 0.8231(4) 0.0549(18) Uani 1 1 d . . . H87A H 0.5595 0.8328 0.7788 0.066 Uiso 1 1 calc R . . C88 C 0.7223(4) 0.8392(4) 0.8186(4) 0.0500(18) Uani 1 1 d . . . C89 C 0.7943(5) 0.7960(5) 0.8056(4) 0.069(2) Uani 1 1 d . . . H89A H 0.7948 0.7509 0.8195 0.083 Uiso 1 1 calc R . . C90 C 0.8605(6) 0.8201(6) 0.7736(5) 0.079(3) Uani 1 1 d . . . H90A H 0.9051 0.7909 0.7638 0.095 Uiso 1 1 calc R . . C91 C 0.8636(6) 0.8887(6) 0.7546(5) 0.077(3) Uani 1 1 d . . . C92 C 0.9371(7) 0.9140(8) 0.7227(6) 0.104(4) Uani 1 1 d . . . H92A H 0.9828 0.8856 0.7136 0.125 Uiso 1 1 calc R . . C93 C 0.9370(8) 0.9828(8) 0.7060(6) 0.105(4) Uani 1 1 d . . . H93A H 0.9827 0.9998 0.6837 0.126 Uiso 1 1 calc R . . C94 C 0.8715(7) 1.0269(6) 0.7213(5) 0.089(3) Uani 1 1 d . . . H94A H 0.8748 1.0730 0.7123 0.106 Uiso 1 1 calc R . . C95 C 0.8018(6) 1.0004(5) 0.7499(4) 0.072(2) Uani 1 1 d . . . H95A H 0.7564 1.0293 0.7585 0.087 Uiso 1 1 calc R . . C96 C 0.7955(4) 0.9321(4) 0.7668(4) 0.0542(19) Uani 1 1 d . . . C97 C 0.7214(5) 0.9061(4) 0.7991(4) 0.057(2) Uani 1 1 d . . . C98 C 0.6496(4) 0.9533(4) 0.8102(4) 0.0505(18) Uani 1 1 d . . . C99 C 0.6568(5) 0.9926(4) 0.8735(4) 0.0538(18) Uani 1 1 d . . . C100 C 0.7339(7) 0.9896(4) 0.9259(4) 0.072(2) Uani 1 1 d . . . H10B H 0.7813 0.9618 0.9191 0.086 Uiso 1 1 calc R . . C101 C 0.7380(8) 1.0277(6) 0.9861(5) 0.094(3) Uani 1 1 d . . . H10C H 0.7882 1.0250 1.0203 0.113 Uiso 1 1 calc R . . C102 C 0.6664(10) 1.0715(6) 0.9978(7) 0.107(4) Uani 1 1 d . . . H10D H 0.6693 1.0968 1.0391 0.128 Uiso 1 1 calc R . . C103 C 0.5959(9) 1.0750(5) 0.9478(7) 0.097(3) Uani 1 1 d . . . H10E H 0.5497 1.1037 0.9550 0.116 Uiso 1 1 calc R . . C104 C 0.5874(6) 1.0379(5) 0.8852(5) 0.074(2) Uani 1 1 d . . . C105 C 0.5157(7) 1.0455(6) 0.8332(7) 0.089(3) Uani 1 1 d . . . H10F H 0.4712 1.0759 0.8404 0.107 Uiso 1 1 calc R . . C106 C 0.5074(6) 1.0096(6) 0.7706(6) 0.085(3) Uani 1 1 d . . . H10G H 0.4573 1.0143 0.7367 0.102 Uiso 1 1 calc R . . C107 C 0.5781(6) 0.9646(5) 0.7595(5) 0.068(2) Uani 1 1 d . . . C108 C 0.5113(7) 0.9436(8) 0.6390(5) 0.127(5) Uani 1 1 d . . . H10H H 0.5203 0.9158 0.5994 0.190 Uiso 1 1 calc R . . H10I H 0.5158 0.9904 0.6267 0.190 Uiso 1 1 calc R . . H10J H 0.4534 0.9349 0.6513 0.190 Uiso 1 1 calc R . . C109 C 0.8574(5) 0.6993(5) 0.9694(5) 0.082(3) Uani 1 1 d . . . H10K H 0.9184 0.7133 0.9801 0.123 Uiso 1 1 calc R . . H10L H 0.8468 0.6806 0.9225 0.123 Uiso 1 1 calc R . . H10M H 0.8453 0.6657 1.0029 0.123 Uiso 1 1 calc R . . C110 C 0.8552(6) 0.8213(5) 0.9827(5) 0.077(3) Uani 1 1 d . . . H11B H 0.9167 0.8086 0.9901 0.116 Uiso 1 1 calc R . . H11C H 0.8420 0.8464 1.0229 0.116 Uiso 1 1 calc R . . H11D H 0.8431 0.8488 0.9410 0.116 Uiso 1 1 calc R . . C111 C 0.7108(7) 0.8534(5) 1.0809(5) 0.081(3) Uani 1 1 d . . . H11E H 0.6899 0.8939 1.1008 0.121 Uiso 1 1 calc R . . H11F H 0.7703 0.8604 1.0712 0.121 Uiso 1 1 calc R . . H11G H 0.7104 0.8169 1.1139 0.121 Uiso 1 1 calc R . . C112 C 0.5764(6) 0.8819(4) 1.0064(5) 0.071(2) Uani 1 1 d . . . H11H H 0.5848 0.9163 1.0423 0.106 Uiso 1 1 calc R . . H11I H 0.5237 0.8565 1.0106 0.106 Uiso 1 1 calc R . . H11J H 0.5704 0.9028 0.9605 0.106 Uiso 1 1 calc R . . C113 C 0.3152(15) 0.6647(6) 0.2541(9) 0.114(7) Uani 0.50 1 d PDU . . H11K H 0.3372 0.6674 0.3038 0.170 Uiso 0.50 1 calc PR . . H11L H 0.3473 0.6304 0.2329 0.170 Uiso 0.50 1 calc PR . . H11M H 0.2532 0.6534 0.2476 0.170 Uiso 0.50 1 calc PR . . C114 C 0.3276(6) 0.7312(4) 0.2201(5) 0.059(4) Uani 0.50 1 d PGDU . . C115 C 0.3505(6) 0.7874(5) 0.2627(4) 0.062(4) Uani 0.50 1 d PGDU . . H115 H 0.3545 0.7838 0.3116 0.075 Uiso 0.50 1 calc PR . . C116 C 0.3675(7) 0.8490(4) 0.2322(7) 0.081(5) Uani 0.50 1 d PGU . . H116 H 0.3828 0.8865 0.2607 0.097 Uiso 0.50 1 calc PR . . C117 C 0.3616(8) 0.8544(5) 0.1591(7) 0.098(6) Uani 0.50 1 d PGU . . H117 H 0.3729 0.8956 0.1387 0.117 Uiso 0.50 1 calc PR . . C118 C 0.3387(7) 0.7982(6) 0.1165(4) 0.087(5) Uani 0.50 1 d PGU . . H118 H 0.3347 0.8018 0.0676 0.104 Uiso 0.50 1 calc PR . . C119 C 0.3217(6) 0.7366(5) 0.1470(5) 0.061(4) Uani 0.50 1 d PGDU . . H119 H 0.3064 0.6991 0.1185 0.073 Uiso 0.50 1 calc PR . . C120 C 0.6428(17) 0.7886(9) 0.6344(16) 0.156(11) Uani 0.50 1 d PDU . . H12B H 0.6765 0.8286 0.6282 0.234 Uiso 0.50 1 calc PR . . H12C H 0.6355 0.7843 0.6833 0.234 Uiso 0.50 1 calc PR . . H12D H 0.5855 0.7918 0.6059 0.234 Uiso 0.50 1 calc PR . . C121 C 0.6906(8) 0.7282(6) 0.6126(7) 0.089(6) Uani 0.50 1 d PGDU . . C122 C 0.7616(9) 0.7361(7) 0.5752(8) 0.125(8) Uani 0.50 1 d PGDU . . H122 H 0.7831 0.7792 0.5677 0.150 Uiso 0.50 1 calc PR . . C123 C 0.8006(9) 0.6797(10) 0.5490(7) 0.111(7) Uani 0.50 1 d PGU . . H123 H 0.8481 0.6850 0.5240 0.133 Uiso 0.50 1 calc PR . . C124 C 0.7686(11) 0.6154(8) 0.5603(8) 0.117(8) Uani 0.50 1 d PGU . . H124 H 0.7946 0.5777 0.5428 0.140 Uiso 0.50 1 calc PR . . C125 C 0.6975(11) 0.6075(6) 0.5977(9) 0.175(13) Uani 0.50 1 d PGU . . H125 H 0.6760 0.5644 0.6052 0.210 Uiso 0.50 1 calc PR . . C126 C 0.6585(8) 0.6639(8) 0.6238(7) 0.088(5) Uani 0.50 1 d PGDU . . H126 H 0.6110 0.6586 0.6488 0.105 Uiso 0.50 1 calc PR . . C127 C 0.8915(14) 0.1544(7) 0.0906(10) 0.110(7) Uani 0.50 1 d PDU . . H12E H 0.8343 0.1436 0.1030 0.165 Uiso 0.50 1 calc PR . . H12F H 0.9367 0.1448 0.1299 0.165 Uiso 0.50 1 calc PR . . H12G H 0.9016 0.1277 0.0505 0.165 Uiso 0.50 1 calc PR . . C128 C 0.8943(9) 0.2271(6) 0.0724(6) 0.144(10) Uani 0.50 1 d PGDU . . C129 C 0.8765(8) 0.2468(6) 0.0019(5) 0.067(4) Uani 0.50 1 d PGDU . . H129 H 0.8590 0.2148 -0.0331 0.081 Uiso 0.50 1 calc PR . . C130 C 0.8849(9) 0.3143(7) -0.0164(6) 0.131(9) Uani 0.50 1 d PGU . . H130 H 0.8730 0.3275 -0.0636 0.157 Uiso 0.50 1 calc PR . . C131 C 0.9111(10) 0.3621(5) 0.0358(8) 0.104(7) Uani 0.50 1 d PGU . . H131 H 0.9167 0.4073 0.0236 0.125 Uiso 0.50 1 calc PR . . C132 C 0.9289(9) 0.3425(6) 0.1064(7) 0.111(7) Uani 0.50 1 d PGU . . H132 H 0.9464 0.3745 0.1413 0.133 Uiso 0.50 1 calc PR . . C133 C 0.9205(8) 0.2750(7) 0.1246(5) 0.084(5) Uani 0.50 1 d PGDU . . H133 H 0.9325 0.2618 0.1718 0.101 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0468(6) 0.0408(7) 0.0490(7) 0.0029(6) 0.0095(5) 0.0047(6) Ti2 0.0484(7) 0.0474(7) 0.0529(8) -0.0004(6) 0.0095(5) 0.0011(6) O1 0.099(5) 0.047(4) 0.094(4) -0.002(3) 0.015(4) -0.014(3) O2 0.068(3) 0.077(4) 0.065(4) 0.005(3) 0.003(3) 0.009(3) O3 0.084(4) 0.048(4) 0.106(5) -0.003(3) 0.020(4) -0.007(3) O4 0.078(4) 0.107(5) 0.058(4) 0.000(3) 0.003(3) -0.016(4) N1 0.061(4) 0.046(4) 0.047(3) 0.003(3) 0.014(3) -0.002(3) N2 0.046(3) 0.044(4) 0.053(3) 0.006(3) 0.013(3) 0.008(3) N3 0.049(3) 0.047(3) 0.053(3) 0.010(3) 0.008(2) 0.003(3) N4 0.040(3) 0.049(4) 0.052(3) 0.007(3) 0.004(3) 0.003(3) N5 0.054(3) 0.045(3) 0.056(3) 0.004(3) 0.011(3) 0.006(3) N6 0.066(4) 0.043(4) 0.068(4) 0.002(3) 0.020(3) -0.001(3) N7 0.059(4) 0.061(5) 0.060(4) -0.009(3) 0.009(3) -0.002(3) N8 0.055(3) 0.043(4) 0.055(4) 0.000(3) 0.013(3) 0.001(3) N9 0.056(3) 0.050(3) 0.055(3) -0.002(3) 0.015(3) -0.002(3) N10 0.050(3) 0.054(4) 0.048(3) -0.002(3) 0.010(3) 0.002(3) N11 0.044(3) 0.072(4) 0.061(4) 0.004(4) 0.009(3) 0.008(3) N12 0.068(4) 0.051(4) 0.050(4) 0.002(3) 0.017(3) -0.001(3) C1 0.062(5) 0.073(6) 0.051(4) -0.004(4) 0.026(4) 0.013(4) C2 0.089(6) 0.070(7) 0.070(6) -0.006(5) 0.027(5) 0.020(5) C3 0.085(6) 0.043(5) 0.076(6) -0.009(4) 0.009(5) 0.016(4) C4 0.066(5) 0.038(4) 0.056(4) 0.003(3) 0.005(4) 0.008(3) C5 0.046(4) 0.046(4) 0.054(4) 0.000(3) 0.007(3) 0.000(3) C6 0.042(3) 0.038(4) 0.050(4) 0.000(3) 0.011(3) 0.001(3) C7 0.045(4) 0.059(5) 0.064(5) 0.009(4) 0.007(3) 0.008(3) C8 0.044(4) 0.068(6) 0.083(6) -0.002(5) 0.018(4) 0.007(4) C9 0.040(4) 0.070(5) 0.061(5) 0.003(4) 0.013(3) 0.000(4) C10 0.066(5) 0.099(7) 0.082(6) 0.004(6) 0.039(5) 0.017(5) C11 0.100(8) 0.122(9) 0.102(8) 0.015(7) 0.060(7) 0.016(7) C12 0.099(7) 0.121(9) 0.074(6) 0.027(6) 0.046(5) 0.020(7) C13 0.059(5) 0.082(6) 0.081(6) 0.016(5) 0.027(4) 0.013(4) C14 0.052(4) 0.049(4) 0.055(4) 0.004(4) 0.015(3) -0.003(3) C15 0.055(4) 0.032(4) 0.052(4) -0.002(3) 0.011(3) -0.003(3) C16 0.043(4) 0.043(4) 0.057(4) 0.012(3) 0.012(3) 0.004(3) C17 0.063(5) 0.061(5) 0.041(4) 0.009(4) 0.005(3) 0.007(4) C18 0.066(5) 0.054(5) 0.056(5) -0.002(4) 0.006(4) 0.003(4) C19 0.081(7) 0.093(7) 0.062(5) -0.007(5) -0.001(5) -0.019(6) C20 0.078(7) 0.113(9) 0.075(6) 0.002(6) -0.017(5) -0.023(6) C21 0.053(5) 0.115(9) 0.081(6) 0.033(6) -0.007(4) 0.015(5) C22 0.048(4) 0.076(6) 0.060(5) 0.022(4) 0.007(4) 0.010(4) C23 0.056(5) 0.072(7) 0.086(6) 0.010(5) 0.007(4) 0.023(5) C24 0.115(8) 0.057(6) 0.077(6) 0.022(5) 0.045(6) 0.033(6) C25 0.065(5) 0.039(5) 0.062(5) 0.013(4) 0.013(4) 0.000(4) C26 0.162(11) 0.050(6) 0.124(9) -0.019(6) 0.008(8) -0.024(7) C27 0.057(5) 0.059(5) 0.070(5) 0.001(4) 0.007(4) -0.003(4) C28 0.052(4) 0.066(6) 0.080(6) 0.000(4) -0.015(4) -0.004(4) C29 0.070(5) 0.064(5) 0.048(4) 0.000(4) 0.001(4) 0.002(4) C30 0.047(4) 0.039(4) 0.059(4) 0.002(3) 0.001(3) 0.000(3) C31 0.058(4) 0.049(5) 0.056(4) 0.003(4) 0.013(4) 0.004(4) C32 0.047(4) 0.052(5) 0.046(4) 0.006(4) 0.011(3) 0.004(4) C33 0.054(4) 0.050(5) 0.068(5) 0.006(4) 0.014(4) 0.014(4) C34 0.041(4) 0.078(6) 0.069(5) 0.004(5) 0.014(3) 0.013(4) C35 0.049(4) 0.075(6) 0.062(5) 0.003(4) 0.022(3) -0.002(4) C36 0.046(5) 0.093(8) 0.095(7) 0.001(5) 0.017(4) -0.013(5) C37 0.058(6) 0.119(10) 0.135(10) 0.017(8) 0.023(6) -0.026(6) C38 0.095(8) 0.079(8) 0.152(11) 0.024(7) 0.025(7) -0.023(6) C39 0.053(5) 0.054(6) 0.150(9) 0.025(6) 0.019(5) -0.011(4) C40 0.050(4) 0.058(5) 0.062(5) 0.004(4) 0.018(3) -0.004(4) C41 0.048(4) 0.041(4) 0.053(4) 0.005(3) 0.006(3) 0.003(3) C42 0.038(4) 0.039(4) 0.074(5) 0.007(4) 0.013(3) -0.002(3) C43 0.052(4) 0.033(4) 0.073(5) -0.004(4) 0.018(4) -0.003(3) C44 0.054(5) 0.065(6) 0.078(6) 0.001(5) 0.011(4) 0.005(4) C45 0.090(7) 0.073(6) 0.083(7) -0.014(5) 0.006(5) 0.004(5) C46 0.107(8) 0.062(6) 0.108(9) -0.015(6) 0.044(7) 0.004(6) C47 0.081(6) 0.063(6) 0.103(8) -0.015(6) 0.032(6) 0.018(5) C48 0.069(5) 0.037(4) 0.097(7) 0.005(4) 0.016(5) 0.010(4) C49 0.064(5) 0.073(6) 0.110(8) -0.004(6) 0.009(5) 0.022(5) C50 0.067(5) 0.061(6) 0.091(7) 0.008(5) -0.013(5) 0.019(4) C51 0.047(4) 0.057(5) 0.076(6) 0.003(4) 0.010(4) 0.001(4) C52 0.103(8) 0.164(12) 0.074(7) 0.011(7) -0.009(6) 0.029(8) C53 0.082(6) 0.076(6) 0.061(5) -0.001(4) -0.002(4) 0.019(5) C54 0.065(5) 0.078(6) 0.062(5) -0.007(4) -0.002(4) -0.006(4) C55 0.104(7) 0.074(6) 0.085(7) -0.030(5) 0.038(5) -0.012(5) C56 0.069(5) 0.056(5) 0.124(8) -0.007(5) 0.036(5) 0.006(5) C57 0.068(5) 0.090(7) 0.059(5) -0.022(5) 0.016(4) -0.009(5) C58 0.074(6) 0.085(8) 0.094(8) -0.043(6) 0.019(5) -0.004(5) C59 0.088(6) 0.047(5) 0.086(7) -0.018(5) 0.014(5) 0.010(4) C60 0.067(5) 0.050(5) 0.076(6) -0.010(4) 0.009(4) 0.001(4) C61 0.058(5) 0.053(5) 0.064(5) -0.004(4) 0.002(4) 0.005(4) C62 0.054(4) 0.042(4) 0.055(4) 0.000(3) 0.012(3) 0.000(3) C63 0.054(4) 0.053(5) 0.052(4) 0.008(3) 0.009(3) 0.005(4) C64 0.053(4) 0.061(5) 0.077(6) -0.003(4) 0.015(4) 0.005(4) C65 0.054(4) 0.062(5) 0.059(5) -0.009(4) 0.012(4) -0.006(4) C66 0.083(6) 0.125(9) 0.065(6) -0.006(6) 0.029(5) 0.018(6) C67 0.107(8) 0.193(13) 0.056(6) -0.007(7) 0.012(5) 0.066(9) C68 0.098(7) 0.173(12) 0.059(6) 0.021(7) 0.014(5) 0.052(8) C69 0.073(6) 0.114(8) 0.059(5) 0.013(5) 0.015(4) 0.023(5) C70 0.047(4) 0.071(5) 0.054(4) 0.001(4) 0.008(3) -0.001(4) C71 0.047(4) 0.044(4) 0.059(4) -0.003(4) 0.010(3) 0.006(3) C72 0.060(5) 0.054(5) 0.062(5) 0.010(4) 0.014(4) 0.015(4) C73 0.051(4) 0.069(6) 0.060(5) 0.010(4) 0.011(3) 0.011(4) C74 0.064(5) 0.085(7) 0.069(6) 0.016(5) 0.001(4) -0.003(5) C75 0.070(6) 0.102(8) 0.080(6) 0.017(6) 0.001(5) -0.022(6) C76 0.069(7) 0.121(10) 0.089(7) 0.024(7) 0.005(5) -0.018(7) C77 0.044(5) 0.141(11) 0.096(7) 0.029(8) 0.025(4) 0.003(6) C78 0.064(5) 0.090(7) 0.066(5) 0.021(5) 0.008(4) 0.016(5) C79 0.076(7) 0.104(9) 0.122(9) 0.016(7) 0.037(6) 0.036(7) C80 0.098(8) 0.076(7) 0.111(8) -0.005(6) 0.022(6) 0.018(6) C81 0.067(5) 0.051(5) 0.077(6) 0.005(4) 0.011(4) 0.011(4) C82 0.130(10) 0.065(8) 0.151(12) -0.007(7) 0.033(8) -0.006(7) C83 0.055(4) 0.050(5) 0.074(5) -0.001(4) 0.018(4) -0.013(3) C84 0.046(4) 0.059(5) 0.087(6) -0.004(5) 0.015(4) -0.011(4) C85 0.062(5) 0.061(5) 0.073(6) 0.007(4) -0.009(4) 0.004(4) C86 0.057(4) 0.056(5) 0.051(4) -0.004(4) 0.007(3) -0.002(4) C87 0.060(5) 0.054(5) 0.051(4) 0.001(4) 0.010(3) 0.002(4) C88 0.047(4) 0.065(5) 0.039(4) 0.001(3) 0.012(3) 0.000(4) C89 0.065(5) 0.075(6) 0.072(5) -0.006(5) 0.025(4) 0.016(4) C90 0.065(5) 0.104(8) 0.074(6) -0.007(5) 0.032(5) 0.014(5) C91 0.069(6) 0.100(8) 0.066(6) -0.004(5) 0.028(4) -0.011(5) C92 0.064(6) 0.153(12) 0.106(8) -0.001(8) 0.047(6) -0.004(7) C93 0.086(7) 0.137(11) 0.101(8) 0.016(8) 0.041(6) -0.037(8) C94 0.087(7) 0.104(8) 0.078(6) 0.011(6) 0.025(5) -0.029(6) C95 0.068(5) 0.089(7) 0.064(5) 0.003(5) 0.022(4) -0.015(5) C96 0.042(4) 0.070(5) 0.053(4) -0.003(4) 0.015(3) -0.011(4) C97 0.066(5) 0.067(6) 0.040(4) 0.002(4) 0.015(3) -0.008(4) C98 0.042(4) 0.058(5) 0.052(4) 0.007(4) 0.009(3) -0.003(3) C99 0.062(5) 0.044(5) 0.059(5) 0.002(4) 0.020(4) -0.002(4) C100 0.105(7) 0.055(5) 0.055(5) -0.004(4) 0.010(5) -0.010(5) C101 0.119(8) 0.094(8) 0.067(6) -0.002(6) 0.007(6) -0.019(7) C102 0.152(12) 0.081(8) 0.101(9) -0.035(7) 0.065(9) -0.009(8) C103 0.117(9) 0.060(6) 0.121(10) -0.016(6) 0.047(8) 0.003(6) C104 0.083(6) 0.063(6) 0.085(6) 0.000(5) 0.041(5) 0.002(5) C105 0.088(7) 0.078(7) 0.109(9) 0.017(6) 0.038(7) 0.016(6) C106 0.059(5) 0.092(7) 0.106(8) 0.034(6) 0.018(5) 0.009(5) C107 0.067(5) 0.075(6) 0.065(5) 0.005(5) 0.020(4) -0.010(5) C108 0.094(8) 0.211(15) 0.066(6) 0.003(8) -0.018(6) -0.008(9) C109 0.052(5) 0.095(7) 0.098(7) 0.003(6) 0.008(5) 0.019(5) C110 0.069(5) 0.077(6) 0.087(6) -0.002(5) 0.016(5) -0.013(5) C111 0.106(7) 0.073(6) 0.062(5) -0.013(5) 0.011(5) -0.018(5) C112 0.079(6) 0.054(5) 0.084(6) -0.011(4) 0.028(5) 0.006(4) C113 0.096(10) 0.115(11) 0.135(11) 0.010(9) 0.034(8) 0.006(8) C114 0.037(6) 0.059(7) 0.086(8) 0.000(7) 0.028(6) 0.008(6) C115 0.041(6) 0.081(8) 0.071(7) -0.034(7) 0.030(6) 0.014(6) C116 0.063(8) 0.081(9) 0.103(9) -0.009(8) 0.023(7) 0.025(7) C117 0.088(9) 0.080(9) 0.124(10) 0.029(8) 0.014(8) 0.015(8) C118 0.067(8) 0.113(10) 0.073(8) 0.010(8) -0.011(7) 0.024(8) C119 0.037(6) 0.077(8) 0.067(7) -0.025(7) -0.001(6) -0.001(6) C120 0.168(14) 0.164(14) 0.134(13) -0.009(9) 0.012(9) 0.002(10) C121 0.089(9) 0.103(10) 0.065(8) 0.003(7) -0.027(7) 0.018(8) C122 0.121(11) 0.141(12) 0.107(11) 0.030(9) 0.000(8) 0.002(9) C123 0.105(10) 0.121(11) 0.100(10) 0.014(8) -0.004(8) 0.022(9) C124 0.110(10) 0.132(11) 0.101(10) -0.011(9) -0.010(8) 0.009(9) C125 0.177(15) 0.176(16) 0.165(15) -0.009(10) -0.002(10) -0.007(10) C126 0.078(8) 0.093(9) 0.084(9) 0.003(8) -0.014(7) -0.006(8) C127 0.087(9) 0.119(10) 0.125(11) 0.013(9) 0.020(8) -0.010(8) C128 0.095(11) 0.166(13) 0.175(13) 0.004(10) 0.037(9) 0.016(9) C129 0.060(7) 0.092(9) 0.053(7) 0.016(7) 0.020(6) 0.000(7) C130 0.098(11) 0.151(12) 0.145(12) -0.028(9) 0.027(9) 0.002(9) C131 0.089(9) 0.115(10) 0.115(10) -0.001(8) 0.043(8) 0.019(8) C132 0.110(10) 0.132(11) 0.094(10) -0.006(8) 0.030(8) 0.035(9) C133 0.061(7) 0.109(10) 0.083(8) -0.035(8) 0.013(7) 0.007(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N6 1.900(6) . ? Ti1 N5 1.922(6) . ? Ti1 N3 2.196(6) . ? Ti1 N1 2.204(6) . ? Ti1 N2 2.208(6) . ? Ti1 N4 2.217(6) . ? Ti2 N11 1.920(6) . ? Ti2 N12 1.926(6) . ? Ti2 N9 2.191(6) . ? Ti2 N8 2.194(6) . ? Ti2 N10 2.200(6) . ? Ti2 N7 2.201(6) . ? O1 C25 1.377(10) . ? O1 C26 1.449(11) . ? O2 C51 1.373(10) . ? O2 C52 1.413(11) . ? O3 C81 1.388(10) . ? O3 C82 1.383(12) . ? O4 C107 1.385(10) . ? O4 C108 1.413(11) . ? N1 C1 1.342(9) . ? N1 C4 1.381(9) . ? N2 C5 1.311(9) . ? N2 C6 1.416(8) . ? N3 C27 1.328(9) . ? N3 C30 1.386(9) . ? N4 C31 1.283(9) . ? N4 C32 1.422(9) . ? N5 C53 1.445(10) . ? N5 C54 1.482(10) . ? N6 C56 1.450(11) . ? N6 C55 1.483(12) . ? N7 C57 1.346(10) . ? N7 C60 1.395(11) . ? N8 C61 1.310(9) . ? N8 C62 1.435(9) . ? N9 C83 1.347(9) . ? N9 C86 1.379(9) . ? N10 C87 1.288(9) . ? N10 C88 1.439(9) . ? N11 C109 1.488(10) . ? N11 C110 1.504(11) . ? N12 C112 1.453(10) . ? N12 C111 1.466(11) . ? C1 C2 1.362(12) . ? C1 H1A 0.9300 . ? C2 C3 1.359(12) . ? C2 H2A 0.9300 . ? C3 C4 1.401(10) . ? C3 H3A 0.9300 . ? C4 C5 1.402(10) . ? C5 H5A 0.9300 . ? C6 C15 1.403(9) . ? C6 C7 1.428(9) . ? C7 C8 1.354(10) . ? C7 H7A 0.9300 . ? C8 C9 1.413(11) . ? C8 H8A 0.9300 . ? C9 C14 1.404(10) . ? C9 C10 1.423(11) . ? C10 C11 1.375(14) . ? C10 H10A 0.9300 . ? C11 C12 1.394(14) . ? C11 H11A 0.9300 . ? C12 C13 1.359(12) . ? C12 H12A 0.9300 . ? C13 C14 1.425(11) . ? C13 H13A 0.9300 . ? C14 C15 1.441(9) . ? C15 C16 1.493(9) . ? C16 C25 1.362(10) . ? C16 C17 1.428(10) . ? C17 C18 1.415(11) . ? C17 C22 1.423(10) . ? C18 C19 1.349(12) . ? C18 H18A 0.9300 . ? C19 C20 1.366(14) . ? C19 H19A 0.9300 . ? C20 C21 1.371(15) . ? C20 H20A 0.9300 . ? C21 C22 1.399(13) . ? C21 H21A 0.9300 . ? C22 C23 1.411(12) . ? C23 C24 1.355(14) . ? C23 H23A 0.9300 . ? C24 C25 1.420(12) . ? C24 H24A 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.405(11) . ? C27 H27A 0.9300 . ? C28 C29 1.400(11) . ? C28 H28A 0.9300 . ? C29 C30 1.402(10) . ? C29 H29A 0.9300 . ? C30 C31 1.395(10) . ? C31 H31A 0.9300 . ? C32 C41 1.363(10) . ? C32 C33 1.441(9) . ? C33 C34 1.387(11) . ? C33 H33A 0.9300 . ? C34 C35 1.358(12) . ? C34 H34A 0.9300 . ? C35 C36 1.410(11) . ? C35 C40 1.451(11) . ? C36 C37 1.353(15) . ? C36 H36A 0.9300 . ? C37 C38 1.386(15) . ? C37 H37A 0.9300 . ? C38 C39 1.398(13) . ? C38 H38A 0.9300 . ? C39 C40 1.387(12) . ? C39 H39A 0.9300 . ? C40 C41 1.454(10) . ? C41 C42 1.502(10) . ? C42 C51 1.375(11) . ? C42 C43 1.402(10) . ? C43 C48 1.413(11) . ? C43 C44 1.413(11) . ? C44 C45 1.357(12) . ? C44 H44A 0.9300 . ? C45 C46 1.367(13) . ? C45 H45A 0.9300 . ? C46 C47 1.340(14) . ? C46 H46A 0.9300 . ? C47 C48 1.425(13) . ? C47 H47A 0.9300 . ? C48 C49 1.409(13) . ? C49 C50 1.343(13) . ? C49 H49A 0.9300 . ? C50 C51 1.407(11) . ? C50 H50A 0.9300 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.424(14) . ? C57 H57A 0.9300 . ? C58 C59 1.327(14) . ? C58 H58A 0.9300 . ? C59 C60 1.386(11) . ? C59 H59A 0.9300 . ? C60 C61 1.405(12) . ? C61 H61A 0.9300 . ? C62 C71 1.373(10) . ? C62 C63 1.424(10) . ? C63 C64 1.344(11) . ? C63 H63A 0.9300 . ? C64 C65 1.404(11) . ? C64 H64A 0.9300 . ? C65 C66 1.407(11) . ? C65 C70 1.432(11) . ? C66 C67 1.367(14) . ? C66 H66A 0.9300 . ? C67 C68 1.419(14) . ? C67 H67A 0.9300 . ? C68 C69 1.334(13) . ? C68 H68A 0.9300 . ? C69 C70 1.410(12) . ? C69 H69A 0.9300 . ? C70 C71 1.420(10) . ? C71 C72 1.515(10) . ? C72 C81 1.365(11) . ? C72 C73 1.468(11) . ? C73 C78 1.403(11) . ? C73 C74 1.404(13) . ? C74 C75 1.367(12) . ? C74 H74A 0.9300 . ? C75 C76 1.375(15) . ? C75 H75A 0.9300 . ? C76 C77 1.321(16) . ? C76 H76A 0.9300 . ? C77 C78 1.443(14) . ? C77 H77A 0.9300 . ? C78 C79 1.394(15) . ? C79 C80 1.379(15) . ? C79 H79A 0.9300 . ? C80 C81 1.365(12) . ? C80 H80A 0.9300 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 C84 1.371(11) . ? C83 H83A 0.9300 . ? C84 C85 1.390(11) . ? C84 H84A 0.9300 . ? C85 C86 1.379(10) . ? C85 H85A 0.9300 . ? C86 C87 1.413(10) . ? C87 H87A 0.9300 . ? C88 C97 1.372(11) . ? C88 C89 1.440(10) . ? C89 C90 1.340(12) . ? C89 H89A 0.9300 . ? C90 C91 1.407(14) . ? C90 H90A 0.9300 . ? C91 C96 1.391(12) . ? C91 C92 1.440(13) . ? C92 C93 1.398(17) . ? C92 H92A 0.9300 . ? C93 C94 1.387(16) . ? C93 H93A 0.9300 . ? C94 C95 1.367(12) . ? C94 H94A 0.9300 . ? C95 C96 1.396(12) . ? C95 H95A 0.9300 . ? C96 C97 1.458(10) . ? C97 C98 1.475(11) . ? C98 C107 1.364(11) . ? C98 C99 1.428(10) . ? C99 C100 1.427(11) . ? C99 C104 1.426(11) . ? C100 C101 1.370(13) . ? C100 H10B 0.9300 . ? C101 C102 1.435(16) . ? C101 H10C 0.9300 . ? C102 C103 1.329(17) . ? C102 H10D 0.9300 . ? C103 C104 1.392(15) . ? C103 H10E 0.9300 . ? C104 C105 1.371(14) . ? C105 C106 1.381(15) . ? C105 H10F 0.9300 . ? C106 C107 1.436(13) . ? C106 H10G 0.9300 . ? C108 H10H 0.9600 . ? C108 H10I 0.9600 . ? C108 H10J 0.9600 . ? C109 H10K 0.9600 . ? C109 H10L 0.9600 . ? C109 H10M 0.9600 . ? C110 H11B 0.9600 . ? C110 H11C 0.9600 . ? C110 H11D 0.9600 . ? C111 H11E 0.9600 . ? C111 H11F 0.9600 . ? C111 H11G 0.9600 . ? C112 H11H 0.9600 . ? C112 H11I 0.9600 . ? C112 H11J 0.9600 . ? C113 C114 1.492(6) . ? C113 H11K 0.9600 . ? C113 H11L 0.9600 . ? C113 H11M 0.9600 . ? C114 C115 1.3900 . ? C114 C119 1.3900 . ? C115 C116 1.3900 . ? C115 H115 0.9300 . ? C116 C117 1.3900 . ? C116 H116 0.9300 . ? C117 C118 1.3900 . ? C117 H117 0.9300 . ? C118 C119 1.3900 . ? C118 H118 0.9300 . ? C119 H119 0.9300 . ? C120 C121 1.489(6) . ? C120 H12B 0.9600 . ? C120 H12C 0.9600 . ? C120 H12D 0.9600 . ? C121 C122 1.3900 . ? C121 C126 1.3900 . ? C122 C123 1.3900 . ? C122 H122 0.9300 . ? C123 C124 1.3900 . ? C123 H123 0.9300 . ? C124 C125 1.3900 . ? C124 H124 0.9300 . ? C125 C126 1.3900 . ? C125 H125 0.9300 . ? C126 H126 0.9300 . ? C127 C128 1.480(6) . ? C127 H12E 0.9600 . ? C127 H12F 0.9600 . ? C127 H12G 0.9600 . ? C128 C129 1.3900 . ? C128 C133 1.3900 . ? C129 C130 1.3900 . ? C129 H129 0.9300 . ? C130 C131 1.3900 . ? C130 H130 0.9300 . ? C131 C132 1.3900 . ? C131 H131 0.9300 . ? C132 C133 1.3900 . ? C132 H132 0.9300 . ? C133 H133 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ti1 N5 98.0(3) . . ? N6 Ti1 N3 90.9(3) . . ? N5 Ti1 N3 169.2(2) . . ? N6 Ti1 N1 170.9(3) . . ? N5 Ti1 N1 90.0(2) . . ? N3 Ti1 N1 81.7(2) . . ? N6 Ti1 N2 98.2(2) . . ? N5 Ti1 N2 99.2(2) . . ? N3 Ti1 N2 85.6(2) . . ? N1 Ti1 N2 76.0(2) . . ? N6 Ti1 N4 97.3(2) . . ? N5 Ti1 N4 97.2(2) . . ? N3 Ti1 N4 75.4(2) . . ? N1 Ti1 N4 86.0(2) . . ? N2 Ti1 N4 155.6(2) . . ? N11 Ti2 N12 98.2(3) . . ? N11 Ti2 N9 170.8(2) . . ? N12 Ti2 N9 88.9(3) . . ? N11 Ti2 N8 95.8(3) . . ? N12 Ti2 N8 97.8(2) . . ? N9 Ti2 N8 88.9(2) . . ? N11 Ti2 N10 97.5(2) . . ? N12 Ti2 N10 98.8(2) . . ? N9 Ti2 N10 75.6(2) . . ? N8 Ti2 N10 157.0(2) . . ? N11 Ti2 N7 91.0(3) . . ? N12 Ti2 N7 169.5(3) . . ? N9 Ti2 N7 82.4(2) . . ? N8 Ti2 N7 76.2(3) . . ? N10 Ti2 N7 84.8(2) . . ? C25 O1 C26 118.6(8) . . ? C51 O2 C52 119.0(7) . . ? C81 O3 C82 117.4(8) . . ? C107 O4 C108 119.0(9) . . ? C1 N1 C4 104.8(6) . . ? C1 N1 Ti1 142.9(5) . . ? C4 N1 Ti1 112.0(5) . . ? C5 N2 C6 116.2(6) . . ? C5 N2 Ti1 113.3(5) . . ? C6 N2 Ti1 130.5(4) . . ? C27 N3 C30 106.2(6) . . ? C27 N3 Ti1 141.1(5) . . ? C30 N3 Ti1 112.1(4) . . ? C31 N4 C32 117.1(6) . . ? C31 N4 Ti1 113.5(5) . . ? C32 N4 Ti1 129.3(4) . . ? C53 N5 C54 109.5(6) . . ? C53 N5 Ti1 125.6(5) . . ? C54 N5 Ti1 124.6(5) . . ? C56 N6 C55 107.8(7) . . ? C56 N6 Ti1 126.3(6) . . ? C55 N6 Ti1 125.5(6) . . ? C57 N7 C60 104.7(7) . . ? C57 N7 Ti2 142.8(6) . . ? C60 N7 Ti2 112.4(5) . . ? C61 N8 C62 115.4(6) . . ? C61 N8 Ti2 113.5(5) . . ? C62 N8 Ti2 131.1(5) . . ? C83 N9 C86 104.5(6) . . ? C83 N9 Ti2 141.8(5) . . ? C86 N9 Ti2 113.2(5) . . ? C87 N10 C88 119.1(6) . . ? C87 N10 Ti2 113.8(5) . . ? C88 N10 Ti2 127.1(4) . . ? C109 N11 C110 108.3(6) . . ? C109 N11 Ti2 127.1(6) . . ? C110 N11 Ti2 124.1(5) . . ? C112 N12 C111 109.3(7) . . ? C112 N12 Ti2 127.0(5) . . ? C111 N12 Ti2 123.3(6) . . ? N1 C1 C2 112.3(8) . . ? N1 C1 H1A 123.8 . . ? C2 C1 H1A 123.8 . . ? C3 C2 C1 106.9(8) . . ? C3 C2 H2A 126.5 . . ? C1 C2 H2A 126.5 . . ? C2 C3 C4 106.7(8) . . ? C2 C3 H3A 126.7 . . ? C4 C3 H3A 126.7 . . ? N1 C4 C5 118.2(7) . . ? N1 C4 C3 109.2(7) . . ? C5 C4 C3 132.6(7) . . ? N2 C5 C4 120.3(7) . . ? N2 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C15 C6 N2 122.7(6) . . ? C15 C6 C7 119.3(6) . . ? N2 C6 C7 118.0(6) . . ? C8 C7 C6 121.7(7) . . ? C8 C7 H7A 119.2 . . ? C6 C7 H7A 119.2 . . ? C7 C8 C9 121.0(7) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C14 C9 C8 118.8(7) . . ? C14 C9 C10 119.3(7) . . ? C8 C9 C10 121.8(7) . . ? C11 C10 C9 120.3(8) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 120.4(9) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 120.2(9) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 121.5(8) . . ? C12 C13 H13A 119.3 . . ? C14 C13 H13A 119.3 . . ? C9 C14 C13 118.2(7) . . ? C9 C14 C15 120.9(6) . . ? C13 C14 C15 120.9(7) . . ? C6 C15 C14 118.4(6) . . ? C6 C15 C16 121.9(6) . . ? C14 C15 C16 119.7(6) . . ? C25 C16 C17 119.3(7) . . ? C25 C16 C15 122.9(7) . . ? C17 C16 C15 117.8(6) . . ? C18 C17 C22 116.7(7) . . ? C18 C17 C16 123.2(7) . . ? C22 C17 C16 120.1(7) . . ? C19 C18 C17 121.9(8) . . ? C19 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? C18 C19 C20 122.1(10) . . ? C18 C19 H19A 119.0 . . ? C20 C19 H19A 119.0 . . ? C19 C20 C21 118.1(9) . . ? C19 C20 H20A 121.0 . . ? C21 C20 H20A 121.0 . . ? C20 C21 C22 122.6(9) . . ? C20 C21 H21A 118.7 . . ? C22 C21 H21A 118.7 . . ? C21 C22 C23 123.8(8) . . ? C21 C22 C17 118.6(9) . . ? C23 C22 C17 117.5(7) . . ? C24 C23 C22 122.3(8) . . ? C24 C23 H23A 118.8 . . ? C22 C23 H23A 118.8 . . ? C23 C24 C25 119.5(9) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C16 C25 O1 116.0(7) . . ? C16 C25 C24 121.1(8) . . ? O1 C25 C24 122.9(8) . . ? O1 C26 H26A 109.5 . . ? O1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 C28 111.9(7) . . ? N3 C27 H27A 124.1 . . ? C28 C27 H27A 124.1 . . ? C29 C28 C27 105.8(7) . . ? C29 C28 H28A 127.1 . . ? C27 C28 H28A 127.1 . . ? C28 C29 C30 106.0(7) . . ? C28 C29 H29A 127.0 . . ? C30 C29 H29A 127.0 . . ? N3 C30 C31 117.5(6) . . ? N3 C30 C29 110.1(6) . . ? C31 C30 C29 132.4(7) . . ? N4 C31 C30 121.0(7) . . ? N4 C31 H31A 119.5 . . ? C30 C31 H31A 119.5 . . ? C41 C32 N4 122.6(6) . . ? C41 C32 C33 120.0(7) . . ? N4 C32 C33 117.5(7) . . ? C34 C33 C32 120.3(7) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C35 C34 C33 121.4(7) . . ? C35 C34 H34A 119.3 . . ? C33 C34 H34A 119.3 . . ? C34 C35 C36 122.1(8) . . ? C34 C35 C40 119.9(7) . . ? C36 C35 C40 117.9(8) . . ? C37 C36 C35 122.2(9) . . ? C37 C36 H36A 118.9 . . ? C35 C36 H36A 118.9 . . ? C36 C37 C38 119.1(9) . . ? C36 C37 H37A 120.4 . . ? C38 C37 H37A 120.4 . . ? C37 C38 C39 122.2(10) . . ? C37 C38 H38A 118.9 . . ? C39 C38 H38A 118.9 . . ? C40 C39 C38 119.1(9) . . ? C40 C39 H39A 120.4 . . ? C38 C39 H39A 120.4 . . ? C39 C40 C35 119.3(7) . . ? C39 C40 C41 122.4(7) . . ? C35 C40 C41 118.4(7) . . ? C32 C41 C40 119.8(6) . . ? C32 C41 C42 122.6(6) . . ? C40 C41 C42 117.4(6) . . ? C51 C42 C43 118.8(7) . . ? C51 C42 C41 122.2(7) . . ? C43 C42 C41 118.9(7) . . ? C42 C43 C48 120.7(8) . . ? C42 C43 C44 123.1(7) . . ? C48 C43 C44 116.2(8) . . ? C45 C44 C43 122.0(8) . . ? C45 C44 H44A 119.0 . . ? C43 C44 H44A 119.0 . . ? C44 C45 C46 120.5(10) . . ? C44 C45 H45A 119.8 . . ? C46 C45 H45A 119.8 . . ? C47 C46 C45 121.4(10) . . ? C47 C46 H46A 119.3 . . ? C45 C46 H46A 119.3 . . ? C46 C47 C48 119.7(9) . . ? C46 C47 H47A 120.2 . . ? C48 C47 H47A 120.2 . . ? C43 C48 C49 117.4(8) . . ? C43 C48 C47 120.2(8) . . ? C49 C48 C47 122.4(8) . . ? C50 C49 C48 122.3(8) . . ? C50 C49 H49A 118.8 . . ? C48 C49 H49A 118.8 . . ? C49 C50 C51 119.4(8) . . ? C49 C50 H50A 120.3 . . ? C51 C50 H50A 120.3 . . ? O2 C51 C42 116.2(7) . . ? O2 C51 C50 122.7(8) . . ? C42 C51 C50 121.1(8) . . ? O2 C52 H52A 109.5 . . ? O2 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O2 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N5 C53 H53A 109.5 . . ? N5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N5 C54 H54A 109.5 . . ? N5 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N5 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N6 C55 H55A 109.5 . . ? N6 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N6 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N6 C56 H56A 109.5 . . ? N6 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N6 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N7 C57 C58 110.5(9) . . ? N7 C57 H57A 124.8 . . ? C58 C57 H57A 124.8 . . ? C59 C58 C57 106.7(8) . . ? C59 C58 H58A 126.7 . . ? C57 C58 H58A 126.7 . . ? C58 C59 C60 108.2(9) . . ? C58 C59 H59A 125.9 . . ? C60 C59 H59A 125.9 . . ? N7 C60 C59 109.9(8) . . ? N7 C60 C61 116.6(7) . . ? C59 C60 C61 133.5(9) . . ? N8 C61 C60 121.2(8) . . ? N8 C61 H61A 119.4 . . ? C60 C61 H61A 119.4 . . ? C71 C62 C63 119.0(7) . . ? C71 C62 N8 124.1(6) . . ? C63 C62 N8 116.9(6) . . ? C64 C63 C62 121.1(7) . . ? C64 C63 H63A 119.5 . . ? C62 C63 H63A 119.5 . . ? C63 C64 C65 121.7(7) . . ? C63 C64 H64A 119.2 . . ? C65 C64 H64A 119.2 . . ? C64 C65 C66 123.4(8) . . ? C64 C65 C70 118.3(7) . . ? C66 C65 C70 118.3(8) . . ? C67 C66 C65 122.1(9) . . ? C67 C66 H66A 118.9 . . ? C65 C66 H66A 118.9 . . ? C66 C67 C68 119.1(9) . . ? C66 C67 H67A 120.4 . . ? C68 C67 H67A 120.4 . . ? C69 C68 C67 119.7(10) . . ? C69 C68 H68A 120.2 . . ? C67 C68 H68A 120.2 . . ? C68 C69 C70 123.4(9) . . ? C68 C69 H69A 118.3 . . ? C70 C69 H69A 118.3 . . ? C69 C70 C71 123.6(7) . . ? C69 C70 C65 117.3(7) . . ? C71 C70 C65 119.1(7) . . ? C62 C71 C70 120.5(6) . . ? C62 C71 C72 122.1(6) . . ? C70 C71 C72 117.4(6) . . ? C81 C72 C73 118.0(7) . . ? C81 C72 C71 123.4(7) . . ? C73 C72 C71 118.3(7) . . ? C78 C73 C74 118.2(8) . . ? C78 C73 C72 119.6(9) . . ? C74 C73 C72 122.2(7) . . ? C75 C74 C73 120.8(9) . . ? C75 C74 H74A 119.6 . . ? C73 C74 H74A 119.6 . . ? C74 C75 C76 121.3(11) . . ? C74 C75 H75A 119.3 . . ? C76 C75 H75A 119.3 . . ? C77 C76 C75 119.8(10) . . ? C77 C76 H76A 120.1 . . ? C75 C76 H76A 120.1 . . ? C76 C77 C78 122.0(10) . . ? C76 C77 H77A 119.0 . . ? C78 C77 H77A 119.0 . . ? C79 C78 C73 117.8(9) . . ? C79 C78 C77 124.3(10) . . ? C73 C78 C77 117.9(10) . . ? C80 C79 C78 122.5(9) . . ? C80 C79 H79A 118.8 . . ? C78 C79 H79A 118.8 . . ? C81 C80 C79 119.6(10) . . ? C81 C80 H80A 120.2 . . ? C79 C80 H80A 120.2 . . ? C80 C81 C72 122.3(9) . . ? C80 C81 O3 123.5(9) . . ? C72 C81 O3 114.2(7) . . ? O3 C82 H82A 109.5 . . ? O3 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? O3 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N9 C83 C84 112.1(7) . . ? N9 C83 H83A 124.0 . . ? C84 C83 H83A 124.0 . . ? C83 C84 C85 106.5(7) . . ? C83 C84 H84A 126.7 . . ? C85 C84 H84A 126.7 . . ? C86 C85 C84 105.9(7) . . ? C86 C85 H85A 127.1 . . ? C84 C85 H85A 127.1 . . ? C85 C86 N9 111.0(7) . . ? C85 C86 C87 132.5(8) . . ? N9 C86 C87 116.3(6) . . ? N10 C87 C86 121.1(7) . . ? N10 C87 H87A 119.5 . . ? C86 C87 H87A 119.5 . . ? C97 C88 N10 122.6(6) . . ? C97 C88 C89 120.2(7) . . ? N10 C88 C89 117.2(7) . . ? C90 C89 C88 120.7(9) . . ? C90 C89 H89A 119.7 . . ? C88 C89 H89A 119.7 . . ? C89 C90 C91 121.1(8) . . ? C89 C90 H90A 119.5 . . ? C91 C90 H90A 119.5 . . ? C96 C91 C90 119.8(8) . . ? C96 C91 C92 120.1(10) . . ? C90 C91 C92 120.1(10) . . ? C93 C92 C91 117.4(11) . . ? C93 C92 H92A 121.3 . . ? C91 C92 H92A 121.3 . . ? C94 C93 C92 122.7(9) . . ? C94 C93 H93A 118.7 . . ? C92 C93 H93A 118.7 . . ? C95 C94 C93 117.9(10) . . ? C95 C94 H94A 121.1 . . ? C93 C94 H94A 121.1 . . ? C94 C95 C96 123.2(10) . . ? C94 C95 H95A 118.4 . . ? C96 C95 H95A 118.4 . . ? C91 C96 C95 118.7(7) . . ? C91 C96 C97 119.8(8) . . ? C95 C96 C97 121.5(7) . . ? C88 C97 C96 118.4(7) . . ? C88 C97 C98 123.3(7) . . ? C96 C97 C98 118.3(7) . . ? C107 C98 C99 117.8(7) . . ? C107 C98 C97 122.1(7) . . ? C99 C98 C97 119.9(6) . . ? C100 C99 C104 117.9(8) . . ? C100 C99 C98 121.6(7) . . ? C104 C99 C98 120.6(8) . . ? C101 C100 C99 119.8(9) . . ? C101 C100 H10B 120.1 . . ? C99 C100 H10B 120.1 . . ? C100 C101 C102 121.4(11) . . ? C100 C101 H10C 119.3 . . ? C102 C101 H10C 119.3 . . ? C103 C102 C101 118.1(10) . . ? C103 C102 H10D 121.0 . . ? C101 C102 H10D 121.0 . . ? C102 C103 C104 123.6(11) . . ? C102 C103 H10E 118.2 . . ? C104 C103 H10E 118.2 . . ? C105 C104 C103 121.8(10) . . ? C105 C104 C99 118.9(9) . . ? C103 C104 C99 119.2(10) . . ? C104 C105 C106 122.1(10) . . ? C104 C105 H10F 118.9 . . ? C106 C105 H10F 118.9 . . ? C105 C106 C107 118.2(9) . . ? C105 C106 H10G 120.9 . . ? C107 C106 H10G 120.9 . . ? C98 C107 O4 115.7(8) . . ? C98 C107 C106 122.2(9) . . ? O4 C107 C106 122.1(9) . . ? O4 C108 H10H 109.5 . . ? O4 C108 H10I 109.5 . . ? H10H C108 H10I 109.5 . . ? O4 C108 H10J 109.5 . . ? H10H C108 H10J 109.5 . . ? H10I C108 H10J 109.5 . . ? N11 C109 H10K 109.5 . . ? N11 C109 H10L 109.5 . . ? H10K C109 H10L 109.5 . . ? N11 C109 H10M 109.5 . . ? H10K C109 H10M 109.5 . . ? H10L C109 H10M 109.5 . . ? N11 C110 H11B 109.5 . . ? N11 C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? N11 C110 H11D 109.5 . . ? H11B C110 H11D 109.5 . . ? H11C C110 H11D 109.5 . . ? N12 C111 H11E 109.5 . . ? N12 C111 H11F 109.5 . . ? H11E C111 H11F 109.5 . . ? N12 C111 H11G 109.5 . . ? H11E C111 H11G 109.5 . . ? H11F C111 H11G 109.5 . . ? N12 C112 H11H 109.5 . . ? N12 C112 H11I 109.5 . . ? H11H C112 H11I 109.5 . . ? N12 C112 H11J 109.5 . . ? H11H C112 H11J 109.5 . . ? H11I C112 H11J 109.5 . . ? C114 C113 H11K 109.5 . . ? C114 C113 H11L 109.5 . . ? H11K C113 H11L 109.5 . . ? C114 C113 H11M 109.5 . . ? H11K C113 H11M 109.5 . . ? H11L C113 H11M 109.5 . . ? C115 C114 C119 120.0 . . ? C115 C114 C113 119.1(5) . . ? C119 C114 C113 120.8(5) . . ? C116 C115 C114 120.0 . . ? C116 C115 H115 120.0 . . ? C114 C115 H115 120.0 . . ? C117 C116 C115 120.0 . . ? C117 C116 H116 120.0 . . ? C115 C116 H116 120.0 . . ? C116 C117 C118 120.0 . . ? C116 C117 H117 120.0 . . ? C118 C117 H117 120.0 . . ? C119 C118 C117 120.0 . . ? C119 C118 H118 120.0 . . ? C117 C118 H118 120.0 . . ? C118 C119 C114 120.0 . . ? C118 C119 H119 120.0 . . ? C114 C119 H119 120.0 . . ? C121 C120 H12B 109.5 . . ? C121 C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C121 C120 H12D 109.5 . . ? H12B C120 H12D 109.5 . . ? H12C C120 H12D 109.5 . . ? C122 C121 C126 120.0 . . ? C122 C121 C120 120.2(6) . . ? C126 C121 C120 119.5(6) . . ? C121 C122 C123 120.0 . . ? C121 C122 H122 120.0 . . ? C123 C122 H122 120.0 . . ? C124 C123 C122 120.0 . . ? C124 C123 H123 120.0 . . ? C122 C123 H123 120.0 . . ? C123 C124 C125 120.0 . . ? C123 C124 H124 120.0 . . ? C125 C124 H124 120.0 . . ? C126 C125 C124 120.0 . . ? C126 C125 H125 120.0 . . ? C124 C125 H125 120.0 . . ? C125 C126 C121 120.0 . . ? C125 C126 H126 120.0 . . ? C121 C126 H126 120.0 . . ? C128 C127 H12E 109.5 . . ? C128 C127 H12F 109.5 . . ? H12E C127 H12F 109.5 . . ? C128 C127 H12G 109.5 . . ? H12E C127 H12G 109.5 . . ? H12F C127 H12G 109.5 . . ? C129 C128 C133 120.0 . . ? C129 C128 C127 119.4(5) . . ? C133 C128 C127 120.5(5) . . ? C128 C129 C130 120.0 . . ? C128 C129 H129 120.0 . . ? C130 C129 H129 120.0 . . ? C129 C130 C131 120.0 . . ? C129 C130 H130 120.0 . . ? C131 C130 H130 120.0 . . ? C132 C131 C130 120.0 . . ? C132 C131 H131 120.0 . . ? C130 C131 H131 120.0 . . ? C133 C132 C131 120.0 . . ? C133 C132 H132 120.0 . . ? C131 C132 H132 120.0 . . ? C132 C133 C128 120.0 . . ? C132 C133 H133 120.0 . . ? C128 C133 H133 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ti1 N1 C1 124.1(16) . . . . ? N5 Ti1 N1 C1 -85.1(9) . . . . ? N3 Ti1 N1 C1 87.9(9) . . . . ? N2 Ti1 N1 C1 175.4(9) . . . . ? N4 Ti1 N1 C1 12.1(8) . . . . ? N6 Ti1 N1 C4 -48.0(18) . . . . ? N5 Ti1 N1 C4 102.7(5) . . . . ? N3 Ti1 N1 C4 -84.3(5) . . . . ? N2 Ti1 N1 C4 3.2(5) . . . . ? N4 Ti1 N1 C4 -160.1(5) . . . . ? N6 Ti1 N2 C5 170.0(5) . . . . ? N5 Ti1 N2 C5 -90.5(5) . . . . ? N3 Ti1 N2 C5 79.7(5) . . . . ? N1 Ti1 N2 C5 -2.9(5) . . . . ? N4 Ti1 N2 C5 41.0(8) . . . . ? N6 Ti1 N2 C6 -7.3(6) . . . . ? N5 Ti1 N2 C6 92.2(6) . . . . ? N3 Ti1 N2 C6 -97.5(6) . . . . ? N1 Ti1 N2 C6 179.9(6) . . . . ? N4 Ti1 N2 C6 -136.2(6) . . . . ? N6 Ti1 N3 C27 -87.3(9) . . . . ? N5 Ti1 N3 C27 127.7(13) . . . . ? N1 Ti1 N3 C27 87.4(8) . . . . ? N2 Ti1 N3 C27 10.9(8) . . . . ? N4 Ti1 N3 C27 175.4(9) . . . . ? N6 Ti1 N3 C30 103.7(5) . . . . ? N5 Ti1 N3 C30 -41.4(16) . . . . ? N1 Ti1 N3 C30 -81.7(5) . . . . ? N2 Ti1 N3 C30 -158.2(5) . . . . ? N4 Ti1 N3 C30 6.4(5) . . . . ? N6 Ti1 N4 C31 -94.2(5) . . . . ? N5 Ti1 N4 C31 166.8(5) . . . . ? N3 Ti1 N4 C31 -5.2(5) . . . . ? N1 Ti1 N4 C31 77.3(5) . . . . ? N2 Ti1 N4 C31 34.9(8) . . . . ? N6 Ti1 N4 C32 90.4(6) . . . . ? N5 Ti1 N4 C32 -8.6(6) . . . . ? N3 Ti1 N4 C32 179.4(6) . . . . ? N1 Ti1 N4 C32 -98.1(6) . . . . ? N2 Ti1 N4 C32 -140.5(6) . . . . ? N6 Ti1 N5 C53 154.8(6) . . . . ? N3 Ti1 N5 C53 -60.5(16) . . . . ? N1 Ti1 N5 C53 -20.8(6) . . . . ? N2 Ti1 N5 C53 55.1(6) . . . . ? N4 Ti1 N5 C53 -106.7(6) . . . . ? N6 Ti1 N5 C54 -33.4(6) . . . . ? N3 Ti1 N5 C54 111.3(14) . . . . ? N1 Ti1 N5 C54 151.1(6) . . . . ? N2 Ti1 N5 C54 -133.1(6) . . . . ? N4 Ti1 N5 C54 65.1(6) . . . . ? N5 Ti1 N6 C56 151.3(6) . . . . ? N3 Ti1 N6 C56 -22.5(6) . . . . ? N1 Ti1 N6 C56 -58.3(19) . . . . ? N2 Ti1 N6 C56 -108.1(6) . . . . ? N4 Ti1 N6 C56 53.0(7) . . . . ? N5 Ti1 N6 C55 -37.5(7) . . . . ? N3 Ti1 N6 C55 148.8(7) . . . . ? N1 Ti1 N6 C55 113.0(17) . . . . ? N2 Ti1 N6 C55 63.1(7) . . . . ? N4 Ti1 N6 C55 -135.8(6) . . . . ? N11 Ti2 N7 C57 -81.7(9) . . . . ? N12 Ti2 N7 C57 126.6(15) . . . . ? N9 Ti2 N7 C57 91.8(9) . . . . ? N8 Ti2 N7 C57 -177.4(9) . . . . ? N10 Ti2 N7 C57 15.7(9) . . . . ? N11 Ti2 N7 C60 93.1(5) . . . . ? N12 Ti2 N7 C60 -58.5(16) . . . . ? N9 Ti2 N7 C60 -93.3(5) . . . . ? N8 Ti2 N7 C60 -2.6(5) . . . . ? N10 Ti2 N7 C60 -169.5(5) . . . . ? N11 Ti2 N8 C61 -88.6(6) . . . . ? N12 Ti2 N8 C61 172.2(5) . . . . ? N9 Ti2 N8 C61 83.5(5) . . . . ? N10 Ti2 N8 C61 36.4(9) . . . . ? N7 Ti2 N8 C61 1.0(5) . . . . ? N11 Ti2 N8 C62 91.9(6) . . . . ? N12 Ti2 N8 C62 -7.2(6) . . . . ? N9 Ti2 N8 C62 -96.0(6) . . . . ? N10 Ti2 N8 C62 -143.1(6) . . . . ? N7 Ti2 N8 C62 -178.4(6) . . . . ? N11 Ti2 N9 C83 147.4(16) . . . . ? N12 Ti2 N9 C83 -71.5(9) . . . . ? N8 Ti2 N9 C83 26.2(8) . . . . ? N10 Ti2 N9 C83 -170.9(9) . . . . ? N7 Ti2 N9 C83 102.5(9) . . . . ? N11 Ti2 N9 C86 -42(2) . . . . ? N12 Ti2 N9 C86 98.8(5) . . . . ? N8 Ti2 N9 C86 -163.5(5) . . . . ? N10 Ti2 N9 C86 -0.6(5) . . . . ? N7 Ti2 N9 C86 -87.2(5) . . . . ? N11 Ti2 N10 C87 174.0(5) . . . . ? N12 Ti2 N10 C87 -86.5(5) . . . . ? N9 Ti2 N10 C87 0.1(5) . . . . ? N8 Ti2 N10 C87 49.2(8) . . . . ? N7 Ti2 N10 C87 83.6(5) . . . . ? N11 Ti2 N10 C88 -7.9(6) . . . . ? N12 Ti2 N10 C88 91.6(6) . . . . ? N9 Ti2 N10 C88 178.2(6) . . . . ? N8 Ti2 N10 C88 -132.7(6) . . . . ? N7 Ti2 N10 C88 -98.3(6) . . . . ? N12 Ti2 N11 C109 153.9(7) . . . . ? N9 Ti2 N11 C109 -65(2) . . . . ? N8 Ti2 N11 C109 55.1(7) . . . . ? N10 Ti2 N11 C109 -106.0(7) . . . . ? N7 Ti2 N11 C109 -21.1(7) . . . . ? N12 Ti2 N11 C110 -35.2(6) . . . . ? N9 Ti2 N11 C110 105.5(18) . . . . ? N8 Ti2 N11 C110 -133.9(6) . . . . ? N10 Ti2 N11 C110 64.9(6) . . . . ? N7 Ti2 N11 C110 149.8(6) . . . . ? N11 Ti2 N12 C112 153.8(6) . . . . ? N9 Ti2 N12 C112 -20.4(6) . . . . ? N8 Ti2 N12 C112 -109.2(6) . . . . ? N10 Ti2 N12 C112 54.8(7) . . . . ? N7 Ti2 N12 C112 -54.9(17) . . . . ? N11 Ti2 N12 C111 -34.4(7) . . . . ? N9 Ti2 N12 C111 151.4(6) . . . . ? N8 Ti2 N12 C111 62.6(7) . . . . ? N10 Ti2 N12 C111 -133.4(6) . . . . ? N7 Ti2 N12 C111 116.9(15) . . . . ? C4 N1 C1 C2 -1.4(9) . . . . ? Ti1 N1 C1 C2 -173.9(7) . . . . ? N1 C1 C2 C3 0.0(11) . . . . ? C1 C2 C3 C4 1.4(10) . . . . ? C1 N1 C4 C5 -178.5(6) . . . . ? Ti1 N1 C4 C5 -3.3(8) . . . . ? C1 N1 C4 C3 2.3(8) . . . . ? Ti1 N1 C4 C3 177.4(5) . . . . ? C2 C3 C4 N1 -2.4(9) . . . . ? C2 C3 C4 C5 178.5(8) . . . . ? C6 N2 C5 C4 179.8(6) . . . . ? Ti1 N2 C5 C4 2.1(8) . . . . ? N1 C4 C5 N2 0.9(10) . . . . ? C3 C4 C5 N2 179.9(8) . . . . ? C5 N2 C6 C15 55.4(9) . . . . ? Ti1 N2 C6 C15 -127.4(6) . . . . ? C5 N2 C6 C7 -125.8(7) . . . . ? Ti1 N2 C6 C7 51.4(8) . . . . ? C15 C6 C7 C8 -1.5(11) . . . . ? N2 C6 C7 C8 179.7(7) . . . . ? C6 C7 C8 C9 1.0(12) . . . . ? C7 C8 C9 C14 -1.1(12) . . . . ? C7 C8 C9 C10 -178.7(8) . . . . ? C14 C9 C10 C11 2.7(14) . . . . ? C8 C9 C10 C11 -179.6(10) . . . . ? C9 C10 C11 C12 -1.4(18) . . . . ? C10 C11 C12 C13 0.3(19) . . . . ? C11 C12 C13 C14 -0.4(17) . . . . ? C8 C9 C14 C13 179.5(8) . . . . ? C10 C9 C14 C13 -2.9(12) . . . . ? C8 C9 C14 C15 1.7(11) . . . . ? C10 C9 C14 C15 179.3(7) . . . . ? C12 C13 C14 C9 1.8(13) . . . . ? C12 C13 C14 C15 179.6(9) . . . . ? N2 C6 C15 C14 -179.2(6) . . . . ? C7 C6 C15 C14 2.0(10) . . . . ? N2 C6 C15 C16 3.6(10) . . . . ? C7 C6 C15 C16 -175.2(7) . . . . ? C9 C14 C15 C6 -2.1(10) . . . . ? C13 C14 C15 C6 -179.9(7) . . . . ? C9 C14 C15 C16 175.1(7) . . . . ? C13 C14 C15 C16 -2.6(11) . . . . ? C6 C15 C16 C25 -94.9(9) . . . . ? C14 C15 C16 C25 87.9(9) . . . . ? C6 C15 C16 C17 84.8(9) . . . . ? C14 C15 C16 C17 -92.4(8) . . . . ? C25 C16 C17 C18 -178.5(7) . . . . ? C15 C16 C17 C18 1.7(10) . . . . ? C25 C16 C17 C22 1.9(10) . . . . ? C15 C16 C17 C22 -177.8(7) . . . . ? C22 C17 C18 C19 -0.7(11) . . . . ? C16 C17 C18 C19 179.8(8) . . . . ? C17 C18 C19 C20 1.1(13) . . . . ? C18 C19 C20 C21 -2.1(15) . . . . ? C19 C20 C21 C22 2.9(15) . . . . ? C20 C21 C22 C23 -179.5(10) . . . . ? C20 C21 C22 C17 -2.5(13) . . . . ? C18 C17 C22 C21 1.3(11) . . . . ? C16 C17 C22 C21 -179.1(7) . . . . ? C18 C17 C22 C23 178.5(7) . . . . ? C16 C17 C22 C23 -2.0(11) . . . . ? C21 C22 C23 C24 177.9(9) . . . . ? C17 C22 C23 C24 0.9(13) . . . . ? C22 C23 C24 C25 0.2(14) . . . . ? C17 C16 C25 O1 178.2(6) . . . . ? C15 C16 C25 O1 -2.2(10) . . . . ? C17 C16 C25 C24 -0.8(11) . . . . ? C15 C16 C25 C24 178.9(7) . . . . ? C26 O1 C25 C16 168.8(8) . . . . ? C26 O1 C25 C24 -12.3(12) . . . . ? C23 C24 C25 C16 -0.3(12) . . . . ? C23 C24 C25 O1 -179.1(8) . . . . ? C30 N3 C27 C28 -0.1(9) . . . . ? Ti1 N3 C27 C28 -169.6(6) . . . . ? N3 C27 C28 C29 -0.1(10) . . . . ? C27 C28 C29 C30 0.2(9) . . . . ? C27 N3 C30 C31 180.0(7) . . . . ? Ti1 N3 C30 C31 -7.2(8) . . . . ? C27 N3 C30 C29 0.3(8) . . . . ? Ti1 N3 C30 C29 173.1(5) . . . . ? C28 C29 C30 N3 -0.3(9) . . . . ? C28 C29 C30 C31 -180.0(8) . . . . ? C32 N4 C31 C30 179.2(7) . . . . ? Ti1 N4 C31 C30 3.2(9) . . . . ? N3 C30 C31 N4 2.8(10) . . . . ? C29 C30 C31 N4 -177.6(8) . . . . ? C31 N4 C32 C41 60.2(9) . . . . ? Ti1 N4 C32 C41 -124.6(6) . . . . ? C31 N4 C32 C33 -119.6(7) . . . . ? Ti1 N4 C32 C33 55.7(9) . . . . ? C41 C32 C33 C34 -3.9(11) . . . . ? N4 C32 C33 C34 175.8(7) . . . . ? C32 C33 C34 C35 -0.7(12) . . . . ? C33 C34 C35 C36 -176.1(8) . . . . ? C33 C34 C35 C40 3.5(12) . . . . ? C34 C35 C36 C37 179.7(10) . . . . ? C40 C35 C36 C37 0.1(14) . . . . ? C35 C36 C37 C38 0.5(18) . . . . ? C36 C37 C38 C39 1(2) . . . . ? C37 C38 C39 C40 -4.2(18) . . . . ? C38 C39 C40 C35 4.7(14) . . . . ? C38 C39 C40 C41 -175.7(9) . . . . ? C34 C35 C40 C39 177.6(9) . . . . ? C36 C35 C40 C39 -2.8(12) . . . . ? C34 C35 C40 C41 -2.0(11) . . . . ? C36 C35 C40 C41 177.6(8) . . . . ? N4 C32 C41 C40 -174.4(6) . . . . ? C33 C32 C41 C40 5.4(10) . . . . ? N4 C32 C41 C42 11.1(11) . . . . ? C33 C32 C41 C42 -169.1(7) . . . . ? C39 C40 C41 C32 178.0(8) . . . . ? C35 C40 C41 C32 -2.5(11) . . . . ? C39 C40 C41 C42 -7.3(12) . . . . ? C35 C40 C41 C42 172.3(7) . . . . ? C32 C41 C42 C51 -97.2(9) . . . . ? C40 C41 C42 C51 88.2(9) . . . . ? C32 C41 C42 C43 86.6(9) . . . . ? C40 C41 C42 C43 -88.0(8) . . . . ? C51 C42 C43 C48 4.4(10) . . . . ? C41 C42 C43 C48 -179.3(7) . . . . ? C51 C42 C43 C44 -176.2(7) . . . . ? C41 C42 C43 C44 0.1(10) . . . . ? C42 C43 C44 C45 -179.3(8) . . . . ? C48 C43 C44 C45 0.1(12) . . . . ? C43 C44 C45 C46 0.5(14) . . . . ? C44 C45 C46 C47 0.8(16) . . . . ? C45 C46 C47 C48 -2.7(16) . . . . ? C42 C43 C48 C49 0.3(11) . . . . ? C44 C43 C48 C49 -179.0(8) . . . . ? C42 C43 C48 C47 177.4(7) . . . . ? C44 C43 C48 C47 -2.0(11) . . . . ? C46 C47 C48 C43 3.3(14) . . . . ? C46 C47 C48 C49 -179.8(10) . . . . ? C43 C48 C49 C50 -4.6(14) . . . . ? C47 C48 C49 C50 178.4(9) . . . . ? C48 C49 C50 C51 3.9(15) . . . . ? C52 O2 C51 C42 -176.8(9) . . . . ? C52 O2 C51 C50 6.5(13) . . . . ? C43 C42 C51 O2 177.9(6) . . . . ? C41 C42 C51 O2 1.8(10) . . . . ? C43 C42 C51 C50 -5.3(11) . . . . ? C41 C42 C51 C50 178.5(7) . . . . ? C49 C50 C51 O2 177.8(8) . . . . ? C49 C50 C51 C42 1.2(13) . . . . ? C60 N7 C57 C58 -0.6(9) . . . . ? Ti2 N7 C57 C58 174.5(6) . . . . ? N7 C57 C58 C59 -0.4(10) . . . . ? C57 C58 C59 C60 1.2(10) . . . . ? C57 N7 C60 C59 1.4(9) . . . . ? Ti2 N7 C60 C59 -175.4(6) . . . . ? C57 N7 C60 C61 -179.3(7) . . . . ? Ti2 N7 C60 C61 3.9(9) . . . . ? C58 C59 C60 N7 -1.7(10) . . . . ? C58 C59 C60 C61 179.2(9) . . . . ? C62 N8 C61 C60 -179.6(7) . . . . ? Ti2 N8 C61 C60 0.8(9) . . . . ? N7 C60 C61 N8 -3.3(11) . . . . ? C59 C60 C61 N8 175.8(9) . . . . ? C61 N8 C62 C71 56.1(10) . . . . ? Ti2 N8 C62 C71 -124.5(7) . . . . ? C61 N8 C62 C63 -125.8(7) . . . . ? Ti2 N8 C62 C63 53.6(9) . . . . ? C71 C62 C63 C64 -6.4(11) . . . . ? N8 C62 C63 C64 175.4(7) . . . . ? C62 C63 C64 C65 2.4(12) . . . . ? C63 C64 C65 C66 -177.7(9) . . . . ? C63 C64 C65 C70 0.3(12) . . . . ? C64 C65 C66 C67 176.0(11) . . . . ? C70 C65 C66 C67 -1.9(16) . . . . ? C65 C66 C67 C68 1(2) . . . . ? C66 C67 C68 C69 0(2) . . . . ? C67 C68 C69 C70 -0.5(19) . . . . ? C68 C69 C70 C71 -177.7(10) . . . . ? C68 C69 C70 C65 -0.4(15) . . . . ? C64 C65 C70 C69 -176.5(8) . . . . ? C66 C65 C70 C69 1.6(12) . . . . ? C64 C65 C70 C71 0.9(11) . . . . ? C66 C65 C70 C71 179.0(8) . . . . ? C63 C62 C71 C70 7.5(11) . . . . ? N8 C62 C71 C70 -174.4(7) . . . . ? C63 C62 C71 C72 -172.1(7) . . . . ? N8 C62 C71 C72 6.0(12) . . . . ? C69 C70 C71 C62 172.3(8) . . . . ? C65 C70 C71 C62 -4.9(11) . . . . ? C69 C70 C71 C72 -8.1(12) . . . . ? C65 C70 C71 C72 174.7(7) . . . . ? C62 C71 C72 C81 -96.4(10) . . . . ? C70 C71 C72 C81 84.0(10) . . . . ? C62 C71 C72 C73 89.9(9) . . . . ? C70 C71 C72 C73 -89.7(9) . . . . ? C81 C72 C73 C78 3.9(11) . . . . ? C71 C72 C73 C78 177.9(7) . . . . ? C81 C72 C73 C74 -175.5(8) . . . . ? C71 C72 C73 C74 -1.4(11) . . . . ? C78 C73 C74 C75 1.3(12) . . . . ? C72 C73 C74 C75 -179.4(8) . . . . ? C73 C74 C75 C76 -1.1(14) . . . . ? C74 C75 C76 C77 0.0(16) . . . . ? C75 C76 C77 C78 0.9(16) . . . . ? C74 C73 C78 C79 177.5(9) . . . . ? C72 C73 C78 C79 -1.9(12) . . . . ? C74 C73 C78 C77 -0.4(12) . . . . ? C72 C73 C78 C77 -179.7(8) . . . . ? C76 C77 C78 C79 -178.4(11) . . . . ? C76 C77 C78 C73 -0.7(14) . . . . ? C73 C78 C79 C80 0.8(16) . . . . ? C77 C78 C79 C80 178.5(10) . . . . ? C78 C79 C80 C81 -1.7(17) . . . . ? C79 C80 C81 C72 3.9(16) . . . . ? C79 C80 C81 O3 -176.9(9) . . . . ? C73 C72 C81 C80 -5.0(13) . . . . ? C71 C72 C81 C80 -178.7(8) . . . . ? C73 C72 C81 O3 175.8(7) . . . . ? C71 C72 C81 O3 2.1(12) . . . . ? C82 O3 C81 C80 -4.9(14) . . . . ? C82 O3 C81 C72 174.4(9) . . . . ? C86 N9 C83 C84 0.7(9) . . . . ? Ti2 N9 C83 C84 171.4(6) . . . . ? N9 C83 C84 C85 -0.3(10) . . . . ? C83 C84 C85 C86 -0.2(9) . . . . ? C84 C85 C86 N9 0.6(9) . . . . ? C84 C85 C86 C87 -174.2(8) . . . . ? C83 N9 C86 C85 -0.8(9) . . . . ? Ti2 N9 C86 C85 -174.6(5) . . . . ? C83 N9 C86 C87 174.9(7) . . . . ? Ti2 N9 C86 C87 1.1(8) . . . . ? C88 N10 C87 C86 -177.8(7) . . . . ? Ti2 N10 C87 C86 0.5(9) . . . . ? C85 C86 C87 N10 173.4(8) . . . . ? N9 C86 C87 N10 -1.1(11) . . . . ? C87 N10 C88 C97 57.0(9) . . . . ? Ti2 N10 C88 C97 -121.0(7) . . . . ? C87 N10 C88 C89 -124.1(8) . . . . ? Ti2 N10 C88 C89 57.9(8) . . . . ? C97 C88 C89 C90 -0.9(12) . . . . ? N10 C88 C89 C90 -179.8(8) . . . . ? C88 C89 C90 C91 2.7(14) . . . . ? C89 C90 C91 C96 -2.2(14) . . . . ? C89 C90 C91 C92 177.7(9) . . . . ? C96 C91 C92 C93 0.8(15) . . . . ? C90 C91 C92 C93 -179.1(10) . . . . ? C91 C92 C93 C94 2.4(18) . . . . ? C92 C93 C94 C95 -4.1(17) . . . . ? C93 C94 C95 C96 2.6(15) . . . . ? C90 C91 C96 C95 177.7(8) . . . . ? C92 C91 C96 C95 -2.2(13) . . . . ? C90 C91 C96 C97 -0.1(13) . . . . ? C92 C91 C96 C97 -180.0(8) . . . . ? C94 C95 C96 C91 0.5(13) . . . . ? C94 C95 C96 C97 178.2(8) . . . . ? N10 C88 C97 C96 177.5(6) . . . . ? C89 C88 C97 C96 -1.4(10) . . . . ? N10 C88 C97 C98 -1.7(11) . . . . ? C89 C88 C97 C98 179.5(7) . . . . ? C91 C96 C97 C88 1.9(11) . . . . ? C95 C96 C97 C88 -175.9(7) . . . . ? C91 C96 C97 C98 -178.9(7) . . . . ? C95 C96 C97 C98 3.3(11) . . . . ? C88 C97 C98 C107 -92.7(9) . . . . ? C96 C97 C98 C107 88.2(9) . . . . ? C88 C97 C98 C99 91.9(9) . . . . ? C96 C97 C98 C99 -87.2(8) . . . . ? C107 C98 C99 C100 -173.0(7) . . . . ? C97 C98 C99 C100 2.6(11) . . . . ? C107 C98 C99 C104 5.1(11) . . . . ? C97 C98 C99 C104 -179.3(7) . . . . ? C104 C99 C100 C101 2.3(12) . . . . ? C98 C99 C100 C101 -179.5(8) . . . . ? C99 C100 C101 C102 -0.7(14) . . . . ? C100 C101 C102 C103 -0.8(17) . . . . ? C101 C102 C103 C104 0.7(18) . . . . ? C102 C103 C104 C105 -176.5(11) . . . . ? C102 C103 C104 C99 1.0(16) . . . . ? C100 C99 C104 C105 175.1(8) . . . . ? C98 C99 C104 C105 -3.1(12) . . . . ? C100 C99 C104 C103 -2.5(12) . . . . ? C98 C99 C104 C103 179.3(8) . . . . ? C103 C104 C105 C106 179.2(10) . . . . ? C99 C104 C105 C106 1.7(14) . . . . ? C104 C105 C106 C107 -2.1(15) . . . . ? C99 C98 C107 O4 176.3(7) . . . . ? C97 C98 C107 O4 0.8(11) . . . . ? C99 C98 C107 C106 -5.7(11) . . . . ? C97 C98 C107 C106 178.8(8) . . . . ? C108 O4 C107 C98 -171.7(9) . . . . ? C108 O4 C107 C106 10.2(13) . . . . ? C105 C106 C107 C98 4.3(13) . . . . ? C105 C106 C107 O4 -177.8(8) . . . . ? C119 C114 C115 C116 0.0 . . . . ? C113 C114 C115 C116 176.2(12) . . . . ? C114 C115 C116 C117 0.0 . . . . ? C115 C116 C117 C118 0.0 . . . . ? C116 C117 C118 C119 0.0 . . . . ? C117 C118 C119 C114 0.0 . . . . ? C115 C114 C119 C118 0.0 . . . . ? C113 C114 C119 C118 -176.1(13) . . . . ? C126 C121 C122 C123 0.0 . . . . ? C120 C121 C122 C123 -173.9(18) . . . . ? C121 C122 C123 C124 0.0 . . . . ? C122 C123 C124 C125 0.0 . . . . ? C123 C124 C125 C126 0.0 . . . . ? C124 C125 C126 C121 0.0 . . . . ? C122 C121 C126 C125 0.0 . . . . ? C120 C121 C126 C125 173.9(18) . . . . ? C133 C128 C129 C130 0.0 . . . . ? C127 C128 C129 C130 -175.6(15) . . . . ? C128 C129 C130 C131 0.0 . . . . ? C129 C130 C131 C132 0.0 . . . . ? C130 C131 C132 C133 0.0 . . . . ? C131 C132 C133 C128 0.0 . . . . ? C129 C128 C133 C132 0.0 . . . . ? C127 C128 C133 C132 175.5(15) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.005 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.091 # Attachment 'compound_11.cif' data_11 _database_code_depnum_ccdc_archive 'CCDC 687851' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C63 H58 N6 O2 Zr' _chemical_formula_sum 'C63 H58 N6 O2 Zr' _chemical_formula_weight 1022.37 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 12.9851(4) _cell_length_b 19.0596(5) _cell_length_c 21.8018(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5395.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11456 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 0.253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9654 _exptl_absorpt_correction_T_max 0.9751 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51031 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.88 _reflns_number_total 12808 _reflns_number_gt 11007 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.0290P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0038(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), 5766 Friedel Pairs, Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 12808 _refine_ls_number_parameters 696 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.277531(19) 0.269501(14) 0.854941(12) 0.02690(8) Uani 1 1 d . . . O1 O 0.51476(15) 0.47675(12) 1.00814(10) 0.0402(5) Uani 1 1 d . . . O2 O 0.2290(2) -0.02419(11) 0.72752(10) 0.0472(6) Uani 1 1 d . . . N1 N 0.34868(17) 0.34068(12) 0.92995(11) 0.0272(5) Uani 1 1 d . . . N2 N 0.45527(16) 0.26087(12) 0.84800(11) 0.0300(5) Uani 1 1 d . . . N3 N 0.27600(18) 0.16484(12) 0.79782(10) 0.0271(5) Uani 1 1 d . . . N4 N 0.31086(17) 0.17696(13) 0.92176(11) 0.0287(6) Uani 1 1 d . . . N5 N 0.2784(2) 0.33482(13) 0.77999(11) 0.0384(6) Uani 1 1 d . . . N6 N 0.12829(18) 0.28267(15) 0.88663(12) 0.0387(6) Uani 1 1 d . . . C1 C 0.3167(2) 0.46097(16) 0.96647(13) 0.0288(6) Uani 1 1 d . . . C2 C 0.2949(2) 0.39002(15) 0.96834(12) 0.0266(6) Uani 1 1 d . . . C3 C 0.2140(2) 0.36437(16) 1.00645(13) 0.0329(6) Uani 1 1 d . . . H3 H 0.1993 0.3156 1.0072 0.039 Uiso 1 1 calc R . . C4 C 0.1571(2) 0.40931(18) 1.04214(13) 0.0343(7) Uani 1 1 d . . . H4 H 0.1040 0.3910 1.0675 0.041 Uiso 1 1 calc R . . C5 C 0.1760(2) 0.48173(18) 1.04186(13) 0.0328(7) Uani 1 1 d . . . C6 C 0.2565(2) 0.50818(16) 1.00355(14) 0.0325(7) Uani 1 1 d . . . C7 C 0.2752(3) 0.58201(17) 1.00303(16) 0.0477(8) Uani 1 1 d . . . H7 H 0.3276 0.6005 0.9773 0.057 Uiso 1 1 calc R . . C8 C 0.2185(3) 0.62667(19) 1.03905(18) 0.0599(10) Uani 1 1 d . . . H8 H 0.2319 0.6757 1.0382 0.072 Uiso 1 1 calc R . . C9 C 0.1405(3) 0.5999(2) 1.07724(18) 0.0575(11) Uani 1 1 d . . . H9 H 0.1015 0.6312 1.1020 0.069 Uiso 1 1 calc R . . C10 C 0.1198(3) 0.5297(2) 1.07938(15) 0.0458(9) Uani 1 1 d . . . H10 H 0.0677 0.5126 1.1061 0.055 Uiso 1 1 calc R . . C11 C 0.3997(2) 0.49040(15) 0.92616(14) 0.0308(7) Uani 1 1 d . . . C12 C 0.5001(2) 0.49556(15) 0.94769(16) 0.0345(7) Uani 1 1 d . . . C13 C 0.5821(2) 0.51791(16) 0.90972(18) 0.0435(9) Uani 1 1 d . . . H13 H 0.6505 0.5190 0.9250 0.052 Uiso 1 1 calc R . . C14 C 0.5618(2) 0.53794(16) 0.85080(19) 0.0465(9) Uani 1 1 d . . . H14 H 0.6171 0.5522 0.8252 0.056 Uiso 1 1 calc R . . C15 C 0.4603(3) 0.53793(16) 0.82691(16) 0.0404(8) Uani 1 1 d . . . C16 C 0.3774(2) 0.51408(14) 0.86566(14) 0.0326(7) Uani 1 1 d . . . C17 C 0.2746(3) 0.51665(14) 0.84146(13) 0.0355(7) Uani 1 1 d . . . H17 H 0.2188 0.5007 0.8660 0.043 Uiso 1 1 calc R . . C18 C 0.2556(3) 0.54159(16) 0.78378(15) 0.0433(8) Uani 1 1 d . . . H18 H 0.1871 0.5432 0.7686 0.052 Uiso 1 1 calc R . . C19 C 0.3384(3) 0.56503(18) 0.74661(17) 0.0507(10) Uani 1 1 d . . . H19 H 0.3245 0.5831 0.7068 0.061 Uiso 1 1 calc R . . C20 C 0.4374(3) 0.56212(17) 0.76697(18) 0.0509(10) Uani 1 1 d . . . H20 H 0.4918 0.5765 0.7407 0.061 Uiso 1 1 calc R . . C21 C 0.6186(2) 0.47064(19) 1.03044(18) 0.0478(9) Uani 1 1 d . . . H21A H 0.6570 0.4379 1.0044 0.072 Uiso 1 1 calc R . . H21B H 0.6176 0.4531 1.0727 0.072 Uiso 1 1 calc R . . H21C H 0.6519 0.5168 1.0294 0.072 Uiso 1 1 calc R . . C22 C 0.4496(2) 0.33745(14) 0.93540(14) 0.0274(6) Uani 1 1 d . . . H22 H 0.4832 0.3628 0.9671 0.033 Uiso 1 1 calc R . . C23 C 0.5078(2) 0.29653(15) 0.89431(14) 0.0305(7) Uani 1 1 d . . . C24 C 0.6155(2) 0.28740(16) 0.88710(15) 0.0366(7) Uani 1 1 d . . . H24 H 0.6685 0.3057 0.9125 0.044 Uiso 1 1 calc R . . C25 C 0.6274(2) 0.24582(15) 0.83484(15) 0.0392(8) Uani 1 1 d . . . H25 H 0.6907 0.2308 0.8175 0.047 Uiso 1 1 calc R . . C26 C 0.5289(2) 0.23035(17) 0.81281(14) 0.0353(7) Uani 1 1 d . . . H26 H 0.5153 0.2022 0.7778 0.042 Uiso 1 1 calc R . . C27 C 0.1772(2) 0.11261(16) 0.71219(14) 0.0306(7) Uani 1 1 d . . . C28 C 0.2529(2) 0.15857(15) 0.73381(13) 0.0286(6) Uani 1 1 d . . . C29 C 0.3100(2) 0.20024(15) 0.69271(14) 0.0306(7) Uani 1 1 d . . . H29 H 0.3624 0.2302 0.7081 0.037 Uiso 1 1 calc R . . C30 C 0.2912(2) 0.19817(15) 0.63089(13) 0.0344(7) Uani 1 1 d . . . H30 H 0.3321 0.2256 0.6039 0.041 Uiso 1 1 calc R . . C31 C 0.2108(3) 0.15533(15) 0.60673(13) 0.0349(7) Uani 1 1 d . . . C32 C 0.1538(2) 0.11203(15) 0.64748(14) 0.0330(6) Uani 1 1 d . . . C33 C 0.0728(3) 0.07031(18) 0.62327(15) 0.0408(8) Uani 1 1 d . . . H33 H 0.0346 0.0406 0.6499 0.049 Uiso 1 1 calc R . . C34 C 0.0486(3) 0.07218(19) 0.56187(16) 0.0480(9) Uani 1 1 d . . . H34 H -0.0070 0.0450 0.5465 0.058 Uiso 1 1 calc R . . C35 C 0.1066(3) 0.11454(19) 0.52179(16) 0.0501(9) Uani 1 1 d . . . H35 H 0.0906 0.1149 0.4793 0.060 Uiso 1 1 calc R . . C36 C 0.1858(3) 0.15530(18) 0.54334(15) 0.0442(9) Uani 1 1 d . . . H36 H 0.2241 0.1836 0.5157 0.053 Uiso 1 1 calc R . . C37 C 0.1156(2) 0.06655(18) 0.75376(14) 0.0341(7) Uani 1 1 d . . . C38 C 0.1409(2) -0.00403(18) 0.75860(15) 0.0385(8) Uani 1 1 d . . . C39 C 0.0825(3) -0.0496(2) 0.79620(17) 0.0510(10) Uani 1 1 d . . . H39 H 0.0998 -0.0980 0.7988 0.061 Uiso 1 1 calc R . . C40 C 0.0014(3) -0.0236(2) 0.82856(17) 0.0576(11) Uani 1 1 d . . . H40 H -0.0364 -0.0545 0.8543 0.069 Uiso 1 1 calc R . . C41 C -0.0286(2) 0.0468(2) 0.82545(16) 0.0490(10) Uani 1 1 d . . . C42 C 0.0281(2) 0.09260(19) 0.78567(14) 0.0381(8) Uani 1 1 d . . . C43 C -0.0069(2) 0.1631(2) 0.77821(16) 0.0436(8) Uani 1 1 d . . . H43 H 0.0289 0.1936 0.7512 0.052 Uiso 1 1 calc R . . C44 C -0.0917(2) 0.1876(2) 0.80952(16) 0.0521(10) Uani 1 1 d . . . H44 H -0.1154 0.2342 0.8031 0.063 Uiso 1 1 calc R . . C45 C -0.1435(3) 0.1431(3) 0.85131(18) 0.0640(12) Uani 1 1 d . . . H45 H -0.2000 0.1607 0.8744 0.077 Uiso 1 1 calc R . . C46 C -0.1131(2) 0.0754(3) 0.85871(18) 0.0671(13) Uani 1 1 d . . . H46 H -0.1492 0.0464 0.8868 0.081 Uiso 1 1 calc R . . C47 C 0.2460(4) -0.09688(18) 0.7171(2) 0.0705(13) Uani 1 1 d . . . H47A H 0.2596 -0.1203 0.7563 0.106 Uiso 1 1 calc R . . H47B H 0.3054 -0.1029 0.6898 0.106 Uiso 1 1 calc R . . H47C H 0.1848 -0.1176 0.6980 0.106 Uiso 1 1 calc R . . C48 C 0.3014(2) 0.10829(15) 0.82934(14) 0.0282(6) Uani 1 1 d . . . H48 H 0.3054 0.0642 0.8091 0.034 Uiso 1 1 calc R . . C49 C 0.3226(2) 0.11255(15) 0.89270(13) 0.0279(6) Uani 1 1 d . . . C50 C 0.3583(2) 0.06220(16) 0.93474(14) 0.0328(7) Uani 1 1 d . . . H50 H 0.3721 0.0142 0.9264 0.039 Uiso 1 1 calc R . . C51 C 0.3697(2) 0.09621(16) 0.99112(15) 0.0353(7) Uani 1 1 d . . . H51 H 0.3925 0.0763 1.0287 0.042 Uiso 1 1 calc R . . C52 C 0.3405(2) 0.16617(17) 0.98050(14) 0.0350(7) Uani 1 1 d . . . H52 H 0.3414 0.2017 1.0110 0.042 Uiso 1 1 calc R . . C53 C 0.3674(3) 0.37139(18) 0.75361(16) 0.0494(9) Uani 1 1 d . . . H53A H 0.3886 0.3478 0.7157 0.074 Uiso 1 1 calc R . . H53B H 0.4245 0.3707 0.7830 0.074 Uiso 1 1 calc R . . H53C H 0.3486 0.4201 0.7445 0.074 Uiso 1 1 calc R . . C54 C 0.1874(3) 0.34534(19) 0.73987(16) 0.0504(10) Uani 1 1 d . . . H54A H 0.1711 0.3955 0.7377 0.076 Uiso 1 1 calc R . . H54B H 0.1284 0.3198 0.7568 0.076 Uiso 1 1 calc R . . H54C H 0.2027 0.3277 0.6986 0.076 Uiso 1 1 calc R . . C55 C 0.0677(3) 0.34699(19) 0.87681(16) 0.0476(9) Uani 1 1 d . . . H55A H 0.0043 0.3354 0.8546 0.071 Uiso 1 1 calc R . . H55B H 0.1083 0.3805 0.8527 0.071 Uiso 1 1 calc R . . H55C H 0.0503 0.3679 0.9165 0.071 Uiso 1 1 calc R . . C56 C 0.0733(2) 0.2361(2) 0.92878(15) 0.0480(8) Uani 1 1 d . . . H56A H 0.0664 0.2590 0.9688 0.072 Uiso 1 1 calc R . . H56B H 0.1118 0.1922 0.9335 0.072 Uiso 1 1 calc R . . H56C H 0.0047 0.2259 0.9123 0.072 Uiso 1 1 calc R . . C57 C 0.2838(3) 0.7846(3) 0.8677(2) 0.0631(19) Uani 0.681(6) 1 d PGDU A 1 C58 C 0.2168(4) 0.8331(2) 0.8937(2) 0.055(3) Uani 0.681(6) 1 d PGD A 1 H58A H 0.2390 0.8799 0.9008 0.065 Uiso 0.681(6) 1 calc PR A 1 C59 C 0.1172(3) 0.8131(2) 0.9094(2) 0.069(2) Uani 0.681(6) 1 d PGU A 1 H59A H 0.0714 0.8462 0.9271 0.083 Uiso 0.681(6) 1 calc PR A 1 C60 C 0.0847(3) 0.7446(3) 0.8990(3) 0.074(2) Uani 0.681(6) 1 d PGU A 1 H60A H 0.0167 0.7310 0.9097 0.089 Uiso 0.681(6) 1 calc PR A 1 C61 C 0.1517(4) 0.6961(2) 0.8731(3) 0.097(3) Uani 0.681(6) 1 d PG A 1 H61A H 0.1295 0.6493 0.8660 0.117 Uiso 0.681(6) 1 calc PR A 1 C62 C 0.2513(3) 0.7161(2) 0.8574(3) 0.067(2) Uani 0.681(6) 1 d PGD A 1 H62A H 0.2971 0.6830 0.8397 0.081 Uiso 0.681(6) 1 calc PR A 1 C63 C 0.3939(5) 0.8030(5) 0.8513(5) 0.098(3) Uani 0.681(6) 1 d PDU A 1 H63A H 0.4065 0.8526 0.8604 0.147 Uiso 0.681(6) 1 calc PR A 1 H63B H 0.4052 0.7944 0.8075 0.147 Uiso 0.681(6) 1 calc PR A 1 H63C H 0.4412 0.7739 0.8754 0.147 Uiso 0.681(6) 1 calc PR A 1 C64 C 0.1776(7) 0.7829(6) 0.8955(5) 0.083(6) Uani 0.319(6) 1 d PGD A 2 C65 C 0.2182(9) 0.7188(4) 0.8772(5) 0.078(6) Uani 0.319(6) 1 d PGD A 2 H65A H 0.1786 0.6772 0.8814 0.094 Uiso 0.319(6) 1 calc PR A 2 C66 C 0.3169(10) 0.7156(5) 0.8526(6) 0.101(7) Uani 0.319(6) 1 d PG A 2 H66A H 0.3447 0.6718 0.8400 0.121 Uiso 0.319(6) 1 calc PR A 2 C67 C 0.3748(8) 0.7765(6) 0.8463(6) 0.080(4) Uani 0.319(6) 1 d PGU A 2 H67A H 0.4422 0.7744 0.8295 0.096 Uiso 0.319(6) 1 calc PR A 2 C68 C 0.3341(9) 0.8406(5) 0.8647(6) 0.081(5) Uani 0.319(6) 1 d PG A 2 H68A H 0.3737 0.8823 0.8604 0.097 Uiso 0.319(6) 1 calc PR A 2 C69 C 0.2355(9) 0.8438(4) 0.8893(5) 0.064(6) Uani 0.319(6) 1 d PGD A 2 H69A H 0.2077 0.8876 0.9018 0.077 Uiso 0.319(6) 1 calc PR A 2 C70 C 0.0688(11) 0.7881(9) 0.9213(10) 0.104(6) Uani 0.319(6) 1 d PDU A 2 H70A H 0.0370 0.7414 0.9214 0.156 Uiso 0.319(6) 1 calc PR A 2 H70B H 0.0278 0.8198 0.8957 0.156 Uiso 0.319(6) 1 calc PR A 2 H70C H 0.0716 0.8063 0.9633 0.156 Uiso 0.319(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02524(12) 0.02950(13) 0.02597(14) 0.00247(13) 0.00290(12) 0.00447(12) O1 0.0258(11) 0.0510(14) 0.0439(14) -0.0064(11) -0.0039(10) 0.0039(10) O2 0.0544(14) 0.0321(11) 0.0552(14) -0.0033(10) 0.0053(13) -0.0010(12) N1 0.0238(12) 0.0307(13) 0.0272(13) 0.0013(11) 0.0041(10) 0.0043(10) N2 0.0264(11) 0.0313(12) 0.0324(13) 0.0012(12) 0.0067(10) 0.0059(10) N3 0.0249(11) 0.0328(12) 0.0237(12) 0.0012(10) 0.0043(11) 0.0023(11) N4 0.0263(13) 0.0339(13) 0.0259(13) 0.0039(11) 0.0009(10) -0.0002(10) N5 0.0501(15) 0.0341(13) 0.0309(14) 0.0047(11) 0.0075(14) 0.0125(14) N6 0.0280(12) 0.0512(18) 0.0369(15) 0.0005(13) 0.0000(11) 0.0045(12) C1 0.0231(13) 0.0383(16) 0.0251(15) -0.0012(13) 0.0005(12) 0.0043(12) C2 0.0241(14) 0.0326(14) 0.0232(14) 0.0001(12) 0.0025(11) 0.0029(12) C3 0.0271(14) 0.0422(16) 0.0292(16) 0.0054(13) -0.0006(14) -0.0004(14) C4 0.0189(13) 0.062(2) 0.0224(16) 0.0028(15) 0.0010(12) 0.0010(14) C5 0.0252(14) 0.051(2) 0.0216(15) -0.0044(14) -0.0023(12) 0.0069(14) C6 0.0252(14) 0.0421(17) 0.0304(16) -0.0064(13) -0.0005(12) 0.0082(12) C7 0.0499(19) 0.0430(18) 0.050(2) -0.0094(16) 0.0120(19) 0.0060(18) C8 0.065(2) 0.046(2) 0.069(3) -0.0214(19) 0.017(2) 0.008(2) C9 0.049(2) 0.067(3) 0.056(3) -0.031(2) 0.0060(19) 0.023(2) C10 0.0334(17) 0.076(3) 0.0283(18) -0.0103(17) -0.0005(14) 0.0146(18) C11 0.0301(15) 0.0266(15) 0.0358(17) -0.0004(13) 0.0098(13) 0.0050(12) C12 0.0291(15) 0.0295(15) 0.045(2) -0.0016(14) 0.0023(14) 0.0026(12) C13 0.0311(17) 0.0328(17) 0.067(3) -0.0042(17) 0.0099(17) -0.0037(14) C14 0.0388(17) 0.0354(17) 0.065(3) 0.0069(19) 0.0212(19) -0.0005(14) C15 0.049(2) 0.0251(16) 0.047(2) 0.0079(14) 0.0177(16) 0.0048(14) C16 0.0389(16) 0.0241(14) 0.0348(19) -0.0003(12) 0.0068(14) 0.0048(12) C17 0.0403(16) 0.0320(15) 0.0343(17) 0.0014(12) 0.0075(16) 0.0051(14) C18 0.049(2) 0.0385(17) 0.0427(19) 0.0069(15) 0.0043(16) 0.0138(15) C19 0.077(3) 0.0380(19) 0.037(2) 0.0131(16) 0.0163(19) 0.0163(18) C20 0.057(2) 0.0351(18) 0.061(3) 0.0165(17) 0.023(2) 0.0067(17) C21 0.0259(16) 0.053(2) 0.065(2) -0.0096(19) -0.0108(16) 0.0058(15) C22 0.0263(14) 0.0277(14) 0.0284(16) 0.0070(13) 0.0032(12) 0.0021(11) C23 0.0269(14) 0.0322(15) 0.0325(17) 0.0039(13) 0.0036(13) 0.0052(12) C24 0.0275(14) 0.0383(18) 0.0441(19) 0.0082(14) -0.0001(14) 0.0057(13) C25 0.0283(15) 0.0392(18) 0.050(2) 0.0052(14) 0.0138(14) 0.0118(13) C26 0.0354(15) 0.0340(15) 0.0365(17) -0.0024(16) 0.0073(13) 0.0084(15) C27 0.0275(14) 0.0348(16) 0.0296(17) 0.0022(13) 0.0047(13) 0.0026(12) C28 0.0289(15) 0.0316(14) 0.0253(15) 0.0008(12) 0.0041(11) 0.0069(11) C29 0.0326(15) 0.0295(15) 0.0297(16) -0.0030(13) 0.0073(12) 0.0023(12) C30 0.0386(16) 0.0328(15) 0.0320(17) 0.0029(12) 0.0114(14) 0.0032(13) C31 0.0412(17) 0.0364(16) 0.0270(16) -0.0001(13) 0.0067(14) 0.0090(14) C32 0.0339(15) 0.0363(15) 0.0289(15) 0.0012(15) 0.0006(14) 0.0044(12) C33 0.0414(18) 0.0472(19) 0.0339(19) -0.0007(15) -0.0029(14) -0.0010(15) C34 0.058(2) 0.048(2) 0.037(2) -0.0066(17) -0.0087(17) -0.0032(18) C35 0.070(3) 0.051(2) 0.0285(18) -0.0035(16) -0.0056(18) 0.0047(19) C36 0.064(2) 0.0396(18) 0.0288(18) 0.0022(15) 0.0049(16) 0.0076(16) C37 0.0259(15) 0.0497(19) 0.0266(16) 0.0034(14) -0.0028(13) -0.0054(14) C38 0.0348(17) 0.0449(19) 0.0360(18) 0.0034(15) -0.0050(15) -0.0095(15) C39 0.046(2) 0.058(2) 0.049(2) 0.0161(18) -0.0102(18) -0.0184(18) C40 0.0353(19) 0.089(3) 0.049(2) 0.032(2) -0.0084(17) -0.020(2) C41 0.0272(16) 0.083(3) 0.037(2) 0.0237(19) -0.0088(14) -0.0052(17) C42 0.0232(14) 0.063(2) 0.0276(17) 0.0076(16) -0.0039(13) -0.0028(14) C43 0.0246(15) 0.069(2) 0.0375(19) 0.0032(18) 0.0060(14) 0.0057(16) C44 0.0269(16) 0.091(3) 0.038(2) 0.001(2) 0.0019(15) 0.0121(18) C45 0.0301(17) 0.121(4) 0.040(2) 0.018(3) 0.0069(18) 0.016(2) C46 0.0228(15) 0.137(4) 0.042(2) 0.038(3) 0.0059(17) -0.002(2) C47 0.101(4) 0.037(2) 0.074(3) -0.0022(19) 0.012(3) 0.003(2) C48 0.0204(14) 0.0298(15) 0.0343(16) 0.0016(13) 0.0035(11) -0.0021(11) C49 0.0205(13) 0.0308(15) 0.0323(17) 0.0042(13) -0.0005(12) -0.0008(12) C50 0.0237(14) 0.0329(16) 0.0420(19) 0.0111(14) -0.0054(13) 0.0012(12) C51 0.0286(15) 0.0428(18) 0.0344(18) 0.0138(14) -0.0067(14) -0.0032(14) C52 0.0311(15) 0.0390(17) 0.0349(18) 0.0024(14) -0.0041(14) -0.0060(13) C53 0.071(2) 0.0352(18) 0.042(2) 0.0058(16) 0.0156(19) 0.0117(18) C54 0.063(2) 0.053(2) 0.036(2) 0.0072(17) 0.0000(17) 0.0236(18) C55 0.0343(17) 0.065(2) 0.043(2) -0.0034(18) 0.0002(15) 0.0186(17) C56 0.0294(15) 0.071(2) 0.044(2) 0.004(2) 0.0036(14) -0.0069(17) C57 0.062(3) 0.091(5) 0.036(3) -0.006(3) -0.010(3) -0.020(4) C58 0.061(5) 0.050(4) 0.053(6) -0.009(4) -0.007(4) -0.002(4) C59 0.068(5) 0.083(5) 0.058(4) 0.019(4) -0.013(4) 0.008(4) C60 0.063(4) 0.078(5) 0.080(5) 0.018(4) 0.004(4) -0.018(4) C61 0.061(5) 0.072(5) 0.159(9) 0.013(5) 0.024(5) -0.013(4) C62 0.070(5) 0.065(5) 0.066(5) -0.019(4) 0.015(5) -0.003(4) C63 0.080(5) 0.139(8) 0.075(5) -0.020(6) 0.002(5) -0.038(5) C64 0.096(13) 0.089(14) 0.064(10) 0.016(10) -0.039(10) 0.015(10) C65 0.142(18) 0.050(9) 0.044(8) 0.003(6) 0.052(10) 0.016(11) C66 0.111(14) 0.054(10) 0.138(16) -0.022(12) 0.049(15) -0.004(10) C67 0.080(7) 0.113(9) 0.047(7) -0.015(7) -0.006(6) -0.005(8) C68 0.103(13) 0.071(10) 0.069(11) -0.038(9) -0.026(10) 0.010(9) C69 0.090(14) 0.075(12) 0.028(10) 0.004(9) -0.002(9) 0.024(11) C70 0.117(11) 0.100(12) 0.095(11) 0.017(10) 0.006(10) -0.008(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N5 2.054(2) . ? Zr1 N6 2.073(2) . ? Zr1 N1 2.317(2) . ? Zr1 N2 2.319(2) . ? Zr1 N4 2.328(2) . ? Zr1 N3 2.352(2) . ? O1 C12 1.379(4) . ? O1 C21 1.438(4) . ? O2 C38 1.383(4) . ? O2 C47 1.421(4) . ? N1 C22 1.317(3) . ? N1 C2 1.440(3) . ? N2 C26 1.357(3) . ? N2 C23 1.395(4) . ? N3 C48 1.320(3) . ? N3 C28 1.432(3) . ? N4 C52 1.353(4) . ? N4 C49 1.390(4) . ? N5 C53 1.467(5) . ? N5 C54 1.484(4) . ? N6 C56 1.464(4) . ? N6 C55 1.472(4) . ? C1 C2 1.382(4) . ? C1 C6 1.440(4) . ? C1 C11 1.500(4) . ? C2 C3 1.425(4) . ? C3 C4 1.373(4) . ? C3 H3 0.9500 . ? C4 C5 1.402(5) . ? C4 H4 0.9500 . ? C5 C10 1.426(4) . ? C5 C6 1.430(4) . ? C6 C7 1.428(4) . ? C7 C8 1.372(4) . ? C7 H7 0.9500 . ? C8 C9 1.407(5) . ? C8 H8 0.9500 . ? C9 C10 1.366(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.389(4) . ? C11 C16 1.424(4) . ? C12 C13 1.414(4) . ? C13 C14 1.366(5) . ? C13 H13 0.9500 . ? C14 C15 1.418(5) . ? C14 H14 0.9500 . ? C15 C20 1.417(5) . ? C15 C16 1.441(4) . ? C16 C17 1.436(4) . ? C17 C18 1.367(4) . ? C17 H17 0.9500 . ? C18 C19 1.418(5) . ? C18 H18 0.9500 . ? C19 C20 1.362(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.408(4) . ? C22 H22 0.9500 . ? C23 C24 1.417(4) . ? C24 C25 1.396(4) . ? C24 H24 0.9500 . ? C25 C26 1.397(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.399(4) . ? C27 C32 1.443(4) . ? C27 C37 1.494(4) . ? C28 C29 1.408(4) . ? C29 C30 1.370(4) . ? C29 H29 0.9500 . ? C30 C31 1.426(4) . ? C30 H30 0.9500 . ? C31 C36 1.420(4) . ? C31 C32 1.421(4) . ? C32 C33 1.421(4) . ? C33 C34 1.375(4) . ? C33 H33 0.9500 . ? C34 C35 1.407(5) . ? C34 H34 0.9500 . ? C35 C36 1.372(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.389(4) . ? C37 C42 1.422(4) . ? C38 C39 1.415(4) . ? C39 C40 1.362(5) . ? C39 H39 0.9500 . ? C40 C41 1.399(6) . ? C40 H40 0.9500 . ? C41 C46 1.423(5) . ? C41 C42 1.434(4) . ? C42 C43 1.428(5) . ? C43 C44 1.377(4) . ? C43 H43 0.9500 . ? C44 C45 1.414(5) . ? C44 H44 0.9500 . ? C45 C46 1.358(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.411(4) . ? C48 H48 0.9500 . ? C49 C50 1.406(4) . ? C50 C51 1.398(4) . ? C50 H50 0.9500 . ? C51 C52 1.406(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.3900 . ? C57 C62 1.3900 . ? C57 C63 1.515(7) . ? C58 C59 1.3900 . ? C58 H58A 0.9500 . ? C59 C60 1.3900 . ? C59 H59A 0.9500 . ? C60 C61 1.3900 . ? C60 H60A 0.9500 . ? C61 C62 1.3900 . ? C61 H61A 0.9500 . ? C62 H62A 0.9500 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.3900 . ? C64 C69 1.3900 . ? C64 C70 1.523(8) . ? C65 C66 1.3900 . ? C65 H65A 0.9500 . ? C66 C67 1.3900 . ? C66 H66A 0.9500 . ? C67 C68 1.3900 . ? C67 H67A 0.9500 . ? C68 C69 1.3900 . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Zr1 N6 101.36(11) . . ? N5 Zr1 N1 101.79(10) . . ? N6 Zr1 N1 93.82(9) . . ? N5 Zr1 N2 89.17(10) . . ? N6 Zr1 N2 163.95(10) . . ? N1 Zr1 N2 71.99(8) . . ? N5 Zr1 N4 162.89(9) . . ? N6 Zr1 N4 93.27(9) . . ? N1 Zr1 N4 85.86(8) . . ? N2 Zr1 N4 78.58(8) . . ? N5 Zr1 N3 95.33(9) . . ? N6 Zr1 N3 105.74(10) . . ? N1 Zr1 N3 150.90(8) . . ? N2 Zr1 N3 85.05(8) . . ? N4 Zr1 N3 71.96(8) . . ? C12 O1 C21 118.2(3) . . ? C38 O2 C47 118.6(3) . . ? C22 N1 C2 117.4(2) . . ? C22 N1 Zr1 115.65(19) . . ? C2 N1 Zr1 126.82(17) . . ? C26 N2 C23 105.9(2) . . ? C26 N2 Zr1 140.2(2) . . ? C23 N2 Zr1 113.88(17) . . ? C48 N3 C28 119.4(2) . . ? C48 N3 Zr1 114.51(18) . . ? C28 N3 Zr1 126.04(17) . . ? C52 N4 C49 105.4(2) . . ? C52 N4 Zr1 139.5(2) . . ? C49 N4 Zr1 113.85(18) . . ? C53 N5 C54 109.4(2) . . ? C53 N5 Zr1 127.2(2) . . ? C54 N5 Zr1 123.1(2) . . ? C56 N6 C55 109.6(3) . . ? C56 N6 Zr1 126.3(2) . . ? C55 N6 Zr1 123.5(2) . . ? C2 C1 C6 118.9(3) . . ? C2 C1 C11 122.0(2) . . ? C6 C1 C11 119.0(3) . . ? C1 C2 C3 120.2(3) . . ? C1 C2 N1 121.5(2) . . ? C3 C2 N1 118.2(2) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 121.2(3) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C10 122.6(3) . . ? C4 C5 C6 118.5(3) . . ? C10 C5 C6 118.9(3) . . ? C7 C6 C5 118.4(3) . . ? C7 C6 C1 121.3(3) . . ? C5 C6 C1 120.3(3) . . ? C8 C7 C6 121.0(3) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 120.0(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 121.1(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C5 120.5(3) . . ? C9 C10 H10 119.7 . . ? C5 C10 H10 119.7 . . ? C12 C11 C16 118.8(3) . . ? C12 C11 C1 120.2(3) . . ? C16 C11 C1 121.0(3) . . ? O1 C12 C11 115.7(3) . . ? O1 C12 C13 122.3(3) . . ? C11 C12 C13 122.0(3) . . ? C14 C13 C12 119.4(3) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 121.7(3) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C20 C15 C14 122.2(3) . . ? C20 C15 C16 119.1(3) . . ? C14 C15 C16 118.6(3) . . ? C11 C16 C17 122.7(3) . . ? C11 C16 C15 119.4(3) . . ? C17 C16 C15 117.9(3) . . ? C18 C17 C16 121.2(3) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 119.9(3) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 121.1(3) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C15 120.8(3) . . ? C19 C20 H20 119.6 . . ? C15 C20 H20 119.6 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C23 120.2(3) . . ? N1 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? N2 C23 C22 117.9(2) . . ? N2 C23 C24 110.0(3) . . ? C22 C23 C24 131.9(3) . . ? C25 C24 C23 105.6(3) . . ? C25 C24 H24 127.2 . . ? C23 C24 H24 127.2 . . ? C24 C25 C26 107.4(3) . . ? C24 C25 H25 126.3 . . ? C26 C25 H25 126.3 . . ? N2 C26 C25 111.1(3) . . ? N2 C26 H26 124.5 . . ? C25 C26 H26 124.5 . . ? C28 C27 C32 118.8(3) . . ? C28 C27 C37 122.7(3) . . ? C32 C27 C37 118.4(3) . . ? C27 C28 C29 120.6(3) . . ? C27 C28 N3 121.9(3) . . ? C29 C28 N3 117.5(3) . . ? C30 C29 C28 121.0(3) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 120.7(3) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C36 C31 C32 119.3(3) . . ? C36 C31 C30 121.8(3) . . ? C32 C31 C30 118.9(3) . . ? C33 C32 C31 118.6(3) . . ? C33 C32 C27 121.5(3) . . ? C31 C32 C27 119.8(3) . . ? C34 C33 C32 121.1(3) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 119.8(3) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 120.9(3) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C31 120.4(3) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C38 C37 C42 119.3(3) . . ? C38 C37 C27 119.3(3) . . ? C42 C37 C27 121.3(3) . . ? O2 C38 C37 115.3(3) . . ? O2 C38 C39 123.8(3) . . ? C37 C38 C39 120.8(3) . . ? C40 C39 C38 119.4(4) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C39 C40 C41 122.7(3) . . ? C39 C40 H40 118.7 . . ? C41 C40 H40 118.7 . . ? C40 C41 C46 123.9(4) . . ? C40 C41 C42 118.0(3) . . ? C46 C41 C42 118.1(4) . . ? C37 C42 C43 121.8(3) . . ? C37 C42 C41 119.6(3) . . ? C43 C42 C41 118.5(3) . . ? C44 C43 C42 121.1(3) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 119.8(4) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C46 C45 C44 120.5(3) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C41 121.8(4) . . ? C45 C46 H46 119.1 . . ? C41 C46 H46 119.1 . . ? O2 C47 H47A 109.5 . . ? O2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N3 C48 C49 120.8(3) . . ? N3 C48 H48 119.6 . . ? C49 C48 H48 119.6 . . ? N4 C49 C50 110.0(3) . . ? N4 C49 C48 118.4(3) . . ? C50 C49 C48 131.6(3) . . ? C51 C50 C49 107.0(3) . . ? C51 C50 H50 126.5 . . ? C49 C50 H50 126.5 . . ? C50 C51 C52 105.4(3) . . ? C50 C51 H51 127.3 . . ? C52 C51 H51 127.3 . . ? N4 C52 C51 112.1(3) . . ? N4 C52 H52 123.9 . . ? C51 C52 H52 123.9 . . ? N5 C53 H53A 109.5 . . ? N5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N5 C54 H54A 109.5 . . ? N5 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N5 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N6 C55 H55A 109.5 . . ? N6 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N6 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N6 C56 H56A 109.5 . . ? N6 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N6 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C62 120.0 . . ? C58 C57 C63 122.2(4) . . ? C62 C57 C63 117.8(4) . . ? C57 C58 C59 120.0 . . ? C57 C58 H58A 120.0 . . ? C59 C58 H58A 120.0 . . ? C58 C59 C60 120.0 . . ? C58 C59 H59A 120.0 . . ? C60 C59 H59A 120.0 . . ? C61 C60 C59 120.0 . . ? C61 C60 H60A 120.0 . . ? C59 C60 H60A 120.0 . . ? C62 C61 C60 120.0 . . ? C62 C61 H61A 120.0 . . ? C60 C61 H61A 120.0 . . ? C61 C62 C57 120.0 . . ? C61 C62 H62A 120.0 . . ? C57 C62 H62A 120.0 . . ? C57 C63 H63A 109.5 . . ? C57 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C57 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 C69 120.0 . . ? C65 C64 C70 121.0(7) . . ? C69 C64 C70 119.0(7) . . ? C66 C65 C64 120.0 . . ? C66 C65 H65A 120.0 . . ? C64 C65 H65A 120.0 . . ? C67 C66 C65 120.0 . . ? C67 C66 H66A 120.0 . . ? C65 C66 H66A 120.0 . . ? C68 C67 C66 120.0 . . ? C68 C67 H67A 120.0 . . ? C66 C67 H67A 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H68A 120.0 . . ? C69 C68 H68A 120.0 . . ? C68 C69 C64 120.0 . . ? C68 C69 H69A 120.0 . . ? C64 C69 H69A 120.0 . . ? C64 C70 H70A 109.5 . . ? C64 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C64 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Zr1 N1 C22 -90.4(2) . . . . ? N6 Zr1 N1 C22 167.2(2) . . . . ? N2 Zr1 N1 C22 -5.18(19) . . . . ? N4 Zr1 N1 C22 74.2(2) . . . . ? N3 Zr1 N1 C22 34.4(3) . . . . ? N5 Zr1 N1 C2 86.1(2) . . . . ? N6 Zr1 N1 C2 -16.3(2) . . . . ? N2 Zr1 N1 C2 171.3(2) . . . . ? N4 Zr1 N1 C2 -109.4(2) . . . . ? N3 Zr1 N1 C2 -149.1(2) . . . . ? N5 Zr1 N2 C26 -73.4(3) . . . . ? N6 Zr1 N2 C26 155.2(4) . . . . ? N1 Zr1 N2 C26 -176.1(3) . . . . ? N4 Zr1 N2 C26 94.6(3) . . . . ? N3 Zr1 N2 C26 22.0(3) . . . . ? N5 Zr1 N2 C23 108.07(19) . . . . ? N6 Zr1 N2 C23 -23.4(4) . . . . ? N1 Zr1 N2 C23 5.38(18) . . . . ? N4 Zr1 N2 C23 -83.95(19) . . . . ? N3 Zr1 N2 C23 -156.51(19) . . . . ? N5 Zr1 N3 C48 163.6(2) . . . . ? N6 Zr1 N3 C48 -93.0(2) . . . . ? N1 Zr1 N3 C48 37.4(3) . . . . ? N2 Zr1 N3 C48 74.9(2) . . . . ? N4 Zr1 N3 C48 -4.72(18) . . . . ? N5 Zr1 N3 C28 -14.9(2) . . . . ? N6 Zr1 N3 C28 88.5(2) . . . . ? N1 Zr1 N3 C28 -141.1(2) . . . . ? N2 Zr1 N3 C28 -103.6(2) . . . . ? N4 Zr1 N3 C28 176.8(2) . . . . ? N5 Zr1 N4 C52 127.7(4) . . . . ? N6 Zr1 N4 C52 -83.4(3) . . . . ? N1 Zr1 N4 C52 10.2(3) . . . . ? N2 Zr1 N4 C52 82.7(3) . . . . ? N3 Zr1 N4 C52 171.1(3) . . . . ? N5 Zr1 N4 C49 -37.2(4) . . . . ? N6 Zr1 N4 C49 111.75(18) . . . . ? N1 Zr1 N4 C49 -154.64(18) . . . . ? N2 Zr1 N4 C49 -82.20(18) . . . . ? N3 Zr1 N4 C49 6.26(17) . . . . ? N6 Zr1 N5 C53 152.1(2) . . . . ? N1 Zr1 N5 C53 55.7(3) . . . . ? N2 Zr1 N5 C53 -15.7(2) . . . . ? N4 Zr1 N5 C53 -59.6(5) . . . . ? N3 Zr1 N5 C53 -100.6(2) . . . . ? N6 Zr1 N5 C54 -35.1(2) . . . . ? N1 Zr1 N5 C54 -131.5(2) . . . . ? N2 Zr1 N5 C54 157.1(2) . . . . ? N4 Zr1 N5 C54 113.2(4) . . . . ? N3 Zr1 N5 C54 72.2(2) . . . . ? N5 Zr1 N6 C56 162.4(3) . . . . ? N1 Zr1 N6 C56 -94.8(3) . . . . ? N2 Zr1 N6 C56 -67.5(5) . . . . ? N4 Zr1 N6 C56 -8.7(3) . . . . ? N3 Zr1 N6 C56 63.4(3) . . . . ? N5 Zr1 N6 C55 -27.4(3) . . . . ? N1 Zr1 N6 C55 75.5(2) . . . . ? N2 Zr1 N6 C55 102.8(4) . . . . ? N4 Zr1 N6 C55 161.5(2) . . . . ? N3 Zr1 N6 C55 -126.3(2) . . . . ? C6 C1 C2 C3 0.0(4) . . . . ? C11 C1 C2 C3 -178.8(3) . . . . ? C6 C1 C2 N1 176.7(2) . . . . ? C11 C1 C2 N1 -2.1(4) . . . . ? C22 N1 C2 C1 58.4(4) . . . . ? Zr1 N1 C2 C1 -118.0(3) . . . . ? C22 N1 C2 C3 -124.8(3) . . . . ? Zr1 N1 C2 C3 58.7(3) . . . . ? C1 C2 C3 C4 -0.5(4) . . . . ? N1 C2 C3 C4 -177.3(3) . . . . ? C2 C3 C4 C5 0.6(4) . . . . ? C3 C4 C5 C10 -178.6(3) . . . . ? C3 C4 C5 C6 -0.2(4) . . . . ? C4 C5 C6 C7 179.6(3) . . . . ? C10 C5 C6 C7 -2.0(4) . . . . ? C4 C5 C6 C1 -0.3(4) . . . . ? C10 C5 C6 C1 178.2(3) . . . . ? C2 C1 C6 C7 -179.5(3) . . . . ? C11 C1 C6 C7 -0.6(4) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? C11 C1 C6 C5 179.2(3) . . . . ? C5 C6 C7 C8 1.0(5) . . . . ? C1 C6 C7 C8 -179.1(3) . . . . ? C6 C7 C8 C9 -0.1(6) . . . . ? C7 C8 C9 C10 0.2(6) . . . . ? C8 C9 C10 C5 -1.2(6) . . . . ? C4 C5 C10 C9 -179.6(3) . . . . ? C6 C5 C10 C9 2.1(5) . . . . ? C2 C1 C11 C12 -88.8(4) . . . . ? C6 C1 C11 C12 92.4(3) . . . . ? C2 C1 C11 C16 91.8(4) . . . . ? C6 C1 C11 C16 -87.1(3) . . . . ? C21 O1 C12 C11 170.7(3) . . . . ? C21 O1 C12 C13 -8.7(4) . . . . ? C16 C11 C12 O1 175.2(2) . . . . ? C1 C11 C12 O1 -4.3(4) . . . . ? C16 C11 C12 C13 -5.5(4) . . . . ? C1 C11 C12 C13 175.1(3) . . . . ? O1 C12 C13 C14 -177.9(3) . . . . ? C11 C12 C13 C14 2.8(5) . . . . ? C12 C13 C14 C15 1.0(5) . . . . ? C13 C14 C15 C20 176.5(3) . . . . ? C13 C14 C15 C16 -1.9(5) . . . . ? C12 C11 C16 C17 -174.3(3) . . . . ? C1 C11 C16 C17 5.1(4) . . . . ? C12 C11 C16 C15 4.4(4) . . . . ? C1 C11 C16 C15 -176.1(3) . . . . ? C20 C15 C16 C11 -179.3(3) . . . . ? C14 C15 C16 C11 -0.9(4) . . . . ? C20 C15 C16 C17 -0.5(4) . . . . ? C14 C15 C16 C17 177.9(3) . . . . ? C11 C16 C17 C18 178.1(3) . . . . ? C15 C16 C17 C18 -0.7(4) . . . . ? C16 C17 C18 C19 0.4(5) . . . . ? C17 C18 C19 C20 1.1(5) . . . . ? C18 C19 C20 C15 -2.4(5) . . . . ? C14 C15 C20 C19 -176.4(3) . . . . ? C16 C15 C20 C19 2.0(5) . . . . ? C2 N1 C22 C23 -172.5(2) . . . . ? Zr1 N1 C22 C23 4.4(3) . . . . ? C26 N2 C23 C22 175.6(3) . . . . ? Zr1 N2 C23 C22 -5.4(3) . . . . ? C26 N2 C23 C24 -0.1(3) . . . . ? Zr1 N2 C23 C24 178.97(19) . . . . ? N1 C22 C23 N2 0.7(4) . . . . ? N1 C22 C23 C24 175.3(3) . . . . ? N2 C23 C24 C25 0.6(3) . . . . ? C22 C23 C24 C25 -174.3(3) . . . . ? C23 C24 C25 C26 -0.8(3) . . . . ? C23 N2 C26 C25 -0.5(3) . . . . ? Zr1 N2 C26 C25 -179.1(2) . . . . ? C24 C25 C26 N2 0.9(4) . . . . ? C32 C27 C28 C29 -4.1(4) . . . . ? C37 C27 C28 C29 179.0(3) . . . . ? C32 C27 C28 N3 176.4(2) . . . . ? C37 C27 C28 N3 -0.4(4) . . . . ? C48 N3 C28 C27 55.4(4) . . . . ? Zr1 N3 C28 C27 -126.1(2) . . . . ? C48 N3 C28 C29 -124.1(3) . . . . ? Zr1 N3 C28 C29 54.4(3) . . . . ? C27 C28 C29 C30 1.7(4) . . . . ? N3 C28 C29 C30 -178.8(3) . . . . ? C28 C29 C30 C31 2.0(4) . . . . ? C29 C30 C31 C36 176.3(3) . . . . ? C29 C30 C31 C32 -3.1(4) . . . . ? C36 C31 C32 C33 -0.4(4) . . . . ? C30 C31 C32 C33 179.0(3) . . . . ? C36 C31 C32 C27 -178.8(3) . . . . ? C30 C31 C32 C27 0.6(4) . . . . ? C28 C27 C32 C33 -175.4(3) . . . . ? C37 C27 C32 C33 1.6(4) . . . . ? C28 C27 C32 C31 2.9(4) . . . . ? C37 C27 C32 C31 179.9(3) . . . . ? C31 C32 C33 C34 -0.8(5) . . . . ? C27 C32 C33 C34 177.5(3) . . . . ? C32 C33 C34 C35 1.7(5) . . . . ? C33 C34 C35 C36 -1.3(6) . . . . ? C34 C35 C36 C31 0.1(5) . . . . ? C32 C31 C36 C35 0.8(5) . . . . ? C30 C31 C36 C35 -178.6(3) . . . . ? C28 C27 C37 C38 -101.9(3) . . . . ? C32 C27 C37 C38 81.3(4) . . . . ? C28 C27 C37 C42 81.8(4) . . . . ? C32 C27 C37 C42 -95.0(3) . . . . ? C47 O2 C38 C37 -164.3(3) . . . . ? C47 O2 C38 C39 19.5(5) . . . . ? C42 C37 C38 O2 -178.1(3) . . . . ? C27 C37 C38 O2 5.5(4) . . . . ? C42 C37 C38 C39 -1.8(5) . . . . ? C27 C37 C38 C39 -178.2(3) . . . . ? O2 C38 C39 C40 175.1(3) . . . . ? C37 C38 C39 C40 -0.8(5) . . . . ? C38 C39 C40 C41 1.3(5) . . . . ? C39 C40 C41 C46 180.0(4) . . . . ? C39 C40 C41 C42 1.0(5) . . . . ? C38 C37 C42 C43 -174.4(3) . . . . ? C27 C37 C42 C43 1.9(5) . . . . ? C38 C37 C42 C41 4.1(4) . . . . ? C27 C37 C42 C41 -179.6(3) . . . . ? C40 C41 C42 C37 -3.6(5) . . . . ? C46 C41 C42 C37 177.3(3) . . . . ? C40 C41 C42 C43 174.9(3) . . . . ? C46 C41 C42 C43 -4.1(5) . . . . ? C37 C42 C43 C44 -179.9(3) . . . . ? C41 C42 C43 C44 1.6(5) . . . . ? C42 C43 C44 C45 2.0(5) . . . . ? C43 C44 C45 C46 -3.0(6) . . . . ? C44 C45 C46 C41 0.4(6) . . . . ? C40 C41 C46 C45 -175.7(4) . . . . ? C42 C41 C46 C45 3.2(6) . . . . ? C28 N3 C48 C49 -178.8(2) . . . . ? Zr1 N3 C48 C49 2.6(3) . . . . ? C52 N4 C49 C50 0.9(3) . . . . ? Zr1 N4 C49 C50 170.71(18) . . . . ? C52 N4 C49 C48 -177.3(2) . . . . ? Zr1 N4 C49 C48 -7.5(3) . . . . ? N3 C48 C49 N4 3.3(4) . . . . ? N3 C48 C49 C50 -174.4(3) . . . . ? N4 C49 C50 C51 -0.4(3) . . . . ? C48 C49 C50 C51 177.5(3) . . . . ? C49 C50 C51 C52 -0.2(3) . . . . ? C49 N4 C52 C51 -1.0(3) . . . . ? Zr1 N4 C52 C51 -166.6(2) . . . . ? C50 C51 C52 N4 0.7(3) . . . . ? C62 C57 C58 C59 0.0 . . . . ? C63 C57 C58 C59 -178.4(7) . . . . ? C57 C58 C59 C60 0.0 . . . . ? C58 C59 C60 C61 0.0 . . . . ? C59 C60 C61 C62 0.0 . . . . ? C60 C61 C62 C57 0.0 . . . . ? C58 C57 C62 C61 0.0 . . . . ? C63 C57 C62 C61 178.5(6) . . . . ? C69 C64 C65 C66 0.0 . . . . ? C70 C64 C65 C66 178.6(14) . . . . ? C64 C65 C66 C67 0.0 . . . . ? C65 C66 C67 C68 0.0 . . . . ? C66 C67 C68 C69 0.0 . . . . ? C67 C68 C69 C64 0.0 . . . . ? C65 C64 C69 C68 0.0 . . . . ? C70 C64 C69 C68 -178.6(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.362 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.053 # Attachment 'compound_13.cif' data_13 _database_code_depnum_ccdc_archive 'CCDC 687852' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H66 N6 O2 Zr' _chemical_formula_sum 'C56 H66 N6 O2 Zr' _chemical_formula_weight 946.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 13.0138(5) _cell_length_b 19.3136(8) _cell_length_c 22.3245(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5611.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11193 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9629 _exptl_absorpt_correction_T_max 0.9720 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 50262 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.11 _reflns_number_total 12379 _reflns_number_gt 11752 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+2.4170P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 12379 _refine_ls_number_parameters 611 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.280602(19) 0.771980(14) 0.641544(11) 0.02085(7) Uani 1 1 d . . . N1 N 0.2779(2) 0.66787(12) 0.69669(10) 0.0226(5) Uani 1 1 d . . . N2 N 0.30437(18) 0.68147(13) 0.57551(11) 0.0256(6) Uani 1 1 d . . . N3 N 0.34707(18) 0.84152(12) 0.56699(10) 0.0209(5) Uani 1 1 d . . . N4 N 0.45772(17) 0.76021(12) 0.64335(11) 0.0252(5) Uani 1 1 d . . . N5 N 0.2933(2) 0.83770(14) 0.71413(11) 0.0319(6) Uani 1 1 d . . . N6 N 0.12978(19) 0.79024(14) 0.61602(11) 0.0296(6) Uani 1 1 d . . . O1 O 0.2589(2) 0.47934(13) 0.77427(13) 0.0474(7) Uani 1 1 d . . . O2 O 0.51264(16) 0.97111(12) 0.48334(9) 0.0284(5) Uani 1 1 d . . . C1 C 0.1346(2) 0.55942(17) 0.74389(14) 0.0283(7) Uani 1 1 d . . . C2 C 0.1675(3) 0.49096(19) 0.74424(16) 0.0377(8) Uani 1 1 d . . . C3 C 0.1137(3) 0.4397(2) 0.71447(19) 0.0475(9) Uani 1 1 d . . . H3 H 0.1375 0.3932 0.7142 0.057 Uiso 1 1 calc R . . C4 C 0.0232(3) 0.4585(2) 0.68477(17) 0.0437(9) Uani 1 1 d . . . H4 H -0.0151 0.4236 0.6648 0.052 Uiso 1 1 calc R . . C5 C -0.0126(2) 0.52580(19) 0.68343(14) 0.0329(7) Uani 1 1 d . . . C6 C 0.0436(2) 0.57758(18) 0.71344(13) 0.0280(7) Uani 1 1 d . . . C7 C 0.0101(2) 0.65180(18) 0.71372(15) 0.0319(7) Uani 1 1 d . . . H7A H 0.0590 0.6792 0.6894 0.038 Uiso 1 1 calc R . . H7B H 0.0132 0.6695 0.7553 0.038 Uiso 1 1 calc R . . C8 C -0.0989(2) 0.6634(2) 0.68922(15) 0.0355(8) Uani 1 1 d . . . H8A H -0.1497 0.6521 0.7208 0.043 Uiso 1 1 calc R . . H8B H -0.1075 0.7128 0.6785 0.043 Uiso 1 1 calc R . . C9 C -0.1193(3) 0.6187(2) 0.63431(16) 0.0427(9) Uani 1 1 d . . . H9A H -0.1890 0.6285 0.6187 0.051 Uiso 1 1 calc R . . H9B H -0.0691 0.6302 0.6025 0.051 Uiso 1 1 calc R . . C10 C -0.1107(3) 0.5423(2) 0.64991(15) 0.0393(8) Uani 1 1 d . . . H10A H -0.1703 0.5288 0.6748 0.047 Uiso 1 1 calc R . . H10B H -0.1130 0.5147 0.6126 0.047 Uiso 1 1 calc R . . C11 C 0.1892(2) 0.61099(16) 0.78264(14) 0.0252(6) Uani 1 1 d . . . C12 C 0.2590(2) 0.65989(16) 0.75979(13) 0.0251(6) Uani 1 1 d . . . C13 C 0.3105(2) 0.70342(16) 0.79935(13) 0.0266(6) Uani 1 1 d . . . H13 H 0.3598 0.7354 0.7844 0.032 Uiso 1 1 calc R . . C14 C 0.2906(2) 0.70057(15) 0.86015(14) 0.0300(6) Uani 1 1 d . . . H14 H 0.3270 0.7305 0.8864 0.036 Uiso 1 1 calc R . . C15 C 0.2182(3) 0.65461(16) 0.88385(13) 0.0288(6) Uani 1 1 d . . . C16 C 0.1676(2) 0.60955(16) 0.84481(13) 0.0284(7) Uani 1 1 d . . . C17 C 0.0880(3) 0.55860(19) 0.86849(15) 0.0370(8) Uani 1 1 d . . . H17A H 0.1191 0.5119 0.8702 0.044 Uiso 1 1 calc R . . H17B H 0.0295 0.5567 0.8402 0.044 Uiso 1 1 calc R . . C18 C 0.0478(3) 0.5778(2) 0.93077(16) 0.0442(9) Uani 1 1 d . . . H18A H 0.0027 0.6189 0.9277 0.053 Uiso 1 1 calc R . . H18B H 0.0066 0.5391 0.9470 0.053 Uiso 1 1 calc R . . C19 C 0.1359(3) 0.5935(2) 0.97301(16) 0.0445(9) Uani 1 1 d . . . H19A H 0.1814 0.5525 0.9760 0.053 Uiso 1 1 calc R . . H19B H 0.1086 0.6036 1.0135 0.053 Uiso 1 1 calc R . . C20 C 0.1978(3) 0.6555(2) 0.95050(15) 0.0421(9) Uani 1 1 d . . . H20A H 0.1601 0.6985 0.9606 0.051 Uiso 1 1 calc R . . H20B H 0.2644 0.6568 0.9719 0.051 Uiso 1 1 calc R . . C21 C 0.2890(5) 0.4091(2) 0.7852(3) 0.092(2) Uani 1 1 d . . . H21A H 0.2321 0.3841 0.8041 0.138 Uiso 1 1 calc R . . H21B H 0.3489 0.4084 0.8118 0.138 Uiso 1 1 calc R . . H21C H 0.3067 0.3868 0.7471 0.138 Uiso 1 1 calc R . . C22 C 0.3038(2) 0.61317(16) 0.66553(13) 0.0247(6) Uani 1 1 d . . . H22 H 0.3112 0.5698 0.6851 0.030 Uiso 1 1 calc R . . C23 C 0.3211(2) 0.61795(17) 0.60306(13) 0.0255(6) Uani 1 1 d . . . C24 C 0.3581(2) 0.56981(17) 0.56191(14) 0.0305(7) Uani 1 1 d . . . H24 H 0.3743 0.5227 0.5695 0.037 Uiso 1 1 calc R . . C25 C 0.3666(2) 0.60443(19) 0.50754(15) 0.0346(7) Uani 1 1 d . . . H25 H 0.3906 0.5858 0.4707 0.042 Uiso 1 1 calc R . . C26 C 0.3328(2) 0.67218(18) 0.51782(13) 0.0291(7) Uani 1 1 d . . . H26 H 0.3301 0.7072 0.4880 0.035 Uiso 1 1 calc R . . C27 C 0.4011(2) 0.99038(15) 0.56458(12) 0.0211(6) Uani 1 1 d . . . C28 C 0.5010(2) 0.99432(16) 0.54173(12) 0.0237(6) Uani 1 1 d . . . C29 C 0.5814(2) 1.01968(16) 0.57655(14) 0.0287(7) Uani 1 1 d . . . H29 H 0.6497 1.0201 0.5615 0.034 Uiso 1 1 calc R . . C30 C 0.5598(2) 1.04429(16) 0.63366(15) 0.0309(7) Uani 1 1 d . . . H30 H 0.6143 1.0612 0.6579 0.037 Uiso 1 1 calc R . . C31 C 0.4602(2) 1.04479(16) 0.65618(13) 0.0277(7) Uani 1 1 d . . . C32 C 0.3801(2) 1.01637(15) 0.62192(13) 0.0242(6) Uani 1 1 d . . . C33 C 0.2720(2) 1.01483(15) 0.64606(13) 0.0279(6) Uani 1 1 d . . . H33A H 0.2584 0.9685 0.6633 0.034 Uiso 1 1 calc R . . H33B H 0.2233 1.0220 0.6125 0.034 Uiso 1 1 calc R . . C34 C 0.2520(3) 1.0695(2) 0.69385(16) 0.0444(9) Uani 1 1 d . . . H34A H 0.2497 1.1157 0.6748 0.053 Uiso 1 1 calc R . . H34B H 0.1842 1.0607 0.7125 0.053 Uiso 1 1 calc R . . C35 C 0.3332(3) 1.0691(2) 0.74142(15) 0.0422(9) Uani 1 1 d . . . H35A H 0.3300 1.0246 0.7633 0.051 Uiso 1 1 calc R . . H35B H 0.3187 1.1066 0.7704 0.051 Uiso 1 1 calc R . . C36 C 0.4408(3) 1.0787(2) 0.71659(15) 0.0391(8) Uani 1 1 d . . . H36A H 0.4905 1.0597 0.7458 0.047 Uiso 1 1 calc R . . H36B H 0.4545 1.1289 0.7128 0.047 Uiso 1 1 calc R . . C37 C 0.3169(2) 0.95992(16) 0.52700(13) 0.0227(6) Uani 1 1 d . . . C38 C 0.2926(2) 0.88936(15) 0.52904(12) 0.0213(5) Uani 1 1 d . . . C39 C 0.2102(2) 0.86389(16) 0.49506(12) 0.0249(6) Uani 1 1 d . . . H39 H 0.1929 0.8162 0.4967 0.030 Uiso 1 1 calc R . . C40 C 0.1542(2) 0.90845(17) 0.45904(13) 0.0273(7) Uani 1 1 d . . . H40 H 0.0988 0.8906 0.4360 0.033 Uiso 1 1 calc R . . C41 C 0.1771(2) 0.97884(17) 0.45575(13) 0.0261(6) Uani 1 1 d . A . C42 C 0.2591(2) 1.00421(16) 0.48960(12) 0.0232(6) Uani 1 1 d . A . C43 C 0.2886(3) 1.08061(16) 0.48765(14) 0.0327(7) Uani 1 1 d D . . H43A H 0.3621 1.0841 0.4865 0.039 Uiso 0.620(11) 1 d PR A 1 H43B H 0.2654 1.1027 0.5237 0.039 Uiso 0.620(11) 1 d PR A 1 H43C H 0.3482 1.0863 0.4628 0.039 Uiso 0.380(11) 1 d PR A 2 H43D H 0.3056 1.0962 0.5273 0.039 Uiso 0.380(11) 1 d PR A 2 C44 C 0.2444(4) 1.1198(3) 0.4331(3) 0.0385(18) Uani 0.620(11) 1 d PDU A 1 H44A H 0.2530 1.1703 0.4388 0.046 Uiso 0.620(11) 1 calc PR A 1 H44B H 0.2819 1.1061 0.3963 0.046 Uiso 0.620(11) 1 calc PR A 1 C45 C 0.1309(5) 1.1023(3) 0.4265(3) 0.0394(18) Uani 0.620(11) 1 d PDU A 1 H45A H 0.1016 1.1291 0.3929 0.047 Uiso 0.620(11) 1 calc PR A 1 H45B H 0.0941 1.1158 0.4635 0.047 Uiso 0.620(11) 1 calc PR A 1 C44' C 0.2001(8) 1.1257(5) 0.4623(5) 0.040(3) Uani 0.380(11) 1 d PDU A 2 H44C H 0.1427 1.1275 0.4913 0.047 Uiso 0.380(11) 1 calc PR A 2 H44D H 0.2247 1.1735 0.4554 0.047 Uiso 0.380(11) 1 calc PR A 2 C45' C 0.1631(10) 1.0943(5) 0.4035(5) 0.044(3) Uani 0.380(11) 1 d PDU A 2 H45C H 0.1124 1.1255 0.3845 0.053 Uiso 0.380(11) 1 calc PR A 2 H45D H 0.2219 1.0888 0.3758 0.053 Uiso 0.380(11) 1 calc PR A 2 C46 C 0.1148(3) 1.02519(18) 0.41510(15) 0.0368(8) Uani 1 1 d D . . H46A H 0.0432 1.0149 0.4205 0.044 Uiso 0.620(11) 1 d PR A 1 H46B H 0.1321 1.0147 0.3743 0.044 Uiso 0.620(11) 1 d PR A 1 H46C H 0.0483 1.0325 0.4327 0.044 Uiso 0.380(11) 1 d PR A 2 H46D H 0.1049 1.0020 0.3775 0.044 Uiso 0.380(11) 1 d PR A 2 C47 C 0.6147(2) 0.9680(2) 0.46018(15) 0.0365(8) Uani 1 1 d . . . H47A H 0.6436 1.0148 0.4583 0.055 Uiso 1 1 calc R . . H47B H 0.6134 0.9479 0.4199 0.055 Uiso 1 1 calc R . . H47C H 0.6572 0.9391 0.4864 0.055 Uiso 1 1 calc R . . C48 C 0.4478(2) 0.83814(15) 0.56014(12) 0.0216(6) Uani 1 1 d . . . H48 H 0.4801 0.8640 0.5292 0.026 Uiso 1 1 calc R . . C49 C 0.5073(2) 0.79662(16) 0.59834(13) 0.0233(6) Uani 1 1 d . . . C50 C 0.6143(2) 0.78583(16) 0.60197(14) 0.0276(6) Uani 1 1 d . . . H50 H 0.6656 0.8051 0.5766 0.033 Uiso 1 1 calc R . . C51 C 0.6297(2) 0.74129(16) 0.65018(15) 0.0330(7) Uani 1 1 d . . . H51 H 0.6937 0.7241 0.6643 0.040 Uiso 1 1 calc R . . C52 C 0.5324(2) 0.72678(19) 0.67387(14) 0.0314(7) Uani 1 1 d . . . H52 H 0.5204 0.6972 0.7071 0.038 Uiso 1 1 calc R . . C53 C 0.2073(3) 0.8506(2) 0.75443(15) 0.0426(9) Uani 1 1 d . . . H53A H 0.2249 0.8346 0.7948 0.064 Uiso 1 1 calc R . . H53B H 0.1465 0.8256 0.7401 0.064 Uiso 1 1 calc R . . H53C H 0.1926 0.9004 0.7555 0.064 Uiso 1 1 calc R . . C54 C 0.3869(3) 0.8704(2) 0.73725(17) 0.0439(9) Uani 1 1 d . . . H54A H 0.3753 0.9202 0.7421 0.066 Uiso 1 1 calc R . . H54B H 0.4435 0.8628 0.7090 0.066 Uiso 1 1 calc R . . H54C H 0.4045 0.8500 0.7761 0.066 Uiso 1 1 calc R . . C55 C 0.0747(3) 0.85564(19) 0.62656(16) 0.0394(8) Uani 1 1 d . . . H55A H 0.0563 0.8766 0.5880 0.059 Uiso 1 1 calc R . . H55B H 0.1191 0.8874 0.6490 0.059 Uiso 1 1 calc R . . H55C H 0.0122 0.8465 0.6497 0.059 Uiso 1 1 calc R . . C56 C 0.0676(3) 0.74678(19) 0.57623(15) 0.0382(8) Uani 1 1 d . . . H56A H -0.0005 0.7398 0.5940 0.057 Uiso 1 1 calc R . . H56B H 0.1014 0.7019 0.5709 0.057 Uiso 1 1 calc R . . H56C H 0.0604 0.7696 0.5373 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02003(12) 0.02256(13) 0.01997(11) 0.00171(11) 0.00055(11) -0.00022(11) N1 0.0230(11) 0.0235(12) 0.0214(11) 0.0030(9) 0.0006(10) -0.0016(11) N2 0.0267(14) 0.0273(13) 0.0230(12) -0.0031(10) -0.0005(10) -0.0010(10) N3 0.0198(11) 0.0228(12) 0.0203(11) 0.0006(9) -0.0008(9) -0.0003(10) N4 0.0221(11) 0.0255(13) 0.0280(11) 0.0048(11) -0.0018(10) -0.0006(9) N5 0.0420(16) 0.0282(14) 0.0256(12) -0.0010(10) -0.0021(12) 0.0075(13) N6 0.0206(12) 0.0369(16) 0.0315(12) 0.0076(11) -0.0008(10) -0.0010(11) O1 0.0421(15) 0.0331(14) 0.0670(17) 0.0005(12) -0.0163(13) 0.0071(11) O2 0.0211(10) 0.0404(13) 0.0238(10) 0.0001(9) 0.0020(8) -0.0018(9) C1 0.0240(15) 0.0319(18) 0.0289(15) 0.0029(13) 0.0009(12) -0.0041(13) C2 0.0330(17) 0.0342(19) 0.0459(19) 0.0009(16) -0.0070(15) -0.0018(15) C3 0.049(2) 0.031(2) 0.062(2) -0.0069(18) -0.0064(19) -0.0006(17) C4 0.043(2) 0.045(2) 0.0429(19) -0.0082(17) -0.0044(17) -0.0148(17) C5 0.0266(15) 0.044(2) 0.0278(15) 0.0014(14) 0.0017(13) -0.0104(14) C6 0.0227(14) 0.0393(19) 0.0219(13) 0.0040(13) 0.0017(11) -0.0055(13) C7 0.0285(16) 0.0378(19) 0.0295(16) 0.0072(14) -0.0057(13) -0.0038(14) C8 0.0255(16) 0.047(2) 0.0336(17) 0.0129(15) 0.0009(13) -0.0039(15) C9 0.0264(15) 0.069(3) 0.0324(17) 0.0078(18) -0.0069(14) -0.0127(16) C10 0.0319(17) 0.058(2) 0.0285(17) -0.0004(16) -0.0036(14) -0.0145(16) C11 0.0225(14) 0.0249(16) 0.0281(14) 0.0041(13) -0.0031(11) -0.0006(11) C12 0.0280(16) 0.0240(15) 0.0233(13) 0.0023(12) -0.0029(11) 0.0010(12) C13 0.0299(15) 0.0222(15) 0.0276(14) 0.0064(12) -0.0044(11) -0.0006(12) C14 0.0376(16) 0.0258(14) 0.0265(13) -0.0018(12) -0.0049(15) 0.0025(13) C15 0.0294(14) 0.0307(16) 0.0264(13) 0.0027(12) -0.0018(14) 0.0059(14) C16 0.0249(14) 0.0302(16) 0.0301(16) 0.0075(13) 0.0042(12) 0.0039(13) C17 0.0331(16) 0.045(2) 0.0329(18) 0.0101(15) 0.0050(14) -0.0048(15) C18 0.042(2) 0.047(2) 0.044(2) 0.0101(17) 0.0125(17) 0.0000(17) C19 0.050(2) 0.052(2) 0.0311(17) 0.0091(16) 0.0089(16) 0.0061(19) C20 0.051(2) 0.045(2) 0.0303(17) -0.0010(15) 0.0083(15) 0.0036(17) C21 0.087(4) 0.034(2) 0.156(6) -0.002(3) -0.062(4) 0.016(3) C22 0.0223(15) 0.0243(15) 0.0274(14) 0.0001(12) -0.0028(11) -0.0012(11) C23 0.0215(13) 0.0270(16) 0.0279(15) -0.0025(12) -0.0016(11) -0.0020(12) C24 0.0228(15) 0.0294(17) 0.0392(17) -0.0059(14) 0.0001(13) 0.0026(13) C25 0.0281(16) 0.043(2) 0.0330(16) -0.0100(15) 0.0044(13) -0.0013(15) C26 0.0259(15) 0.0371(19) 0.0243(14) -0.0022(13) 0.0023(12) -0.0032(14) C27 0.0192(13) 0.0210(14) 0.0232(13) 0.0036(11) -0.0033(11) -0.0028(11) C28 0.0237(14) 0.0254(15) 0.0219(13) 0.0042(12) 0.0001(11) 0.0017(12) C29 0.0219(14) 0.0328(17) 0.0313(15) 0.0022(13) -0.0007(12) -0.0068(13) C30 0.0298(15) 0.0303(16) 0.0325(16) -0.0028(14) -0.0079(13) -0.0055(13) C31 0.0285(15) 0.0260(16) 0.0287(15) -0.0007(12) -0.0041(12) -0.0031(12) C32 0.0240(14) 0.0214(15) 0.0271(14) 0.0000(11) -0.0019(11) 0.0025(11) C33 0.0268(14) 0.0298(15) 0.0271(13) -0.0043(12) 0.0001(14) 0.0002(12) C34 0.0351(19) 0.059(3) 0.0386(19) -0.0179(18) 0.0018(14) 0.0046(17) C35 0.048(2) 0.048(2) 0.0306(17) -0.0146(16) -0.0007(16) 0.0050(18) C36 0.0393(19) 0.043(2) 0.0346(17) -0.0116(16) -0.0020(15) -0.0078(16) C37 0.0190(13) 0.0280(16) 0.0211(13) 0.0036(12) 0.0003(11) 0.0004(11) C38 0.0175(13) 0.0261(14) 0.0203(12) 0.0021(11) -0.0015(11) 0.0010(12) C39 0.0205(13) 0.0309(16) 0.0233(13) 0.0012(11) -0.0039(12) -0.0036(13) C40 0.0187(13) 0.0415(19) 0.0217(13) -0.0008(12) -0.0012(11) -0.0024(13) C41 0.0209(13) 0.0360(18) 0.0213(13) 0.0044(12) 0.0002(11) 0.0044(12) C42 0.0186(13) 0.0266(15) 0.0243(13) 0.0034(12) 0.0000(10) 0.0040(11) C43 0.0347(16) 0.0262(16) 0.0371(16) 0.0082(13) -0.0075(15) 0.0027(14) C44 0.039(3) 0.036(3) 0.040(3) 0.011(3) -0.003(3) 0.006(2) C45 0.039(4) 0.045(4) 0.034(4) 0.017(3) 0.000(3) 0.011(3) C44' 0.042(6) 0.035(5) 0.042(5) 0.011(4) -0.003(4) 0.007(4) C45' 0.044(6) 0.046(6) 0.043(6) 0.020(5) 0.001(5) 0.003(5) C46 0.0263(16) 0.051(2) 0.0334(17) 0.0074(15) -0.0054(14) 0.0072(15) C47 0.0221(15) 0.052(2) 0.0359(17) 0.0014(16) 0.0066(13) 0.0045(15) C48 0.0201(13) 0.0225(14) 0.0223(13) -0.0008(11) 0.0039(11) -0.0003(11) C49 0.0196(13) 0.0254(15) 0.0248(13) 0.0009(11) 0.0026(11) 0.0010(11) C50 0.0234(14) 0.0243(17) 0.0351(15) 0.0026(12) 0.0008(12) 0.0023(12) C51 0.0227(14) 0.0320(17) 0.0443(18) 0.0041(14) -0.0054(13) 0.0057(12) C52 0.0291(15) 0.0307(17) 0.0345(15) 0.0096(15) -0.0025(12) 0.0040(15) C53 0.056(2) 0.044(2) 0.0276(16) -0.0027(14) 0.0067(17) 0.0170(19) C54 0.056(2) 0.033(2) 0.042(2) -0.0049(16) -0.0073(18) -0.0015(17) C55 0.0259(16) 0.048(2) 0.044(2) 0.0088(16) 0.0005(14) 0.0097(15) C56 0.0292(16) 0.049(2) 0.0361(17) 0.0062(15) -0.0034(14) -0.0059(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N5 2.065(3) . ? Zr1 N6 2.074(2) . ? Zr1 N3 2.307(2) . ? Zr1 N2 2.307(2) . ? Zr1 N4 2.316(2) . ? Zr1 N1 2.358(2) . ? N1 C22 1.309(4) . ? N1 C12 1.439(4) . ? N2 C26 1.352(4) . ? N2 C23 1.389(4) . ? N3 C48 1.322(4) . ? N3 C38 1.440(4) . ? N4 C52 1.351(4) . ? N4 C49 1.386(4) . ? N5 C53 1.458(5) . ? N5 C54 1.466(5) . ? N6 C56 1.466(4) . ? N6 C55 1.471(4) . ? O1 C2 1.384(4) . ? O1 C21 1.433(5) . ? O2 C28 1.387(3) . ? O2 C47 1.427(4) . ? C1 C2 1.390(5) . ? C1 C6 1.410(4) . ? C1 C11 1.498(4) . ? C2 C3 1.382(5) . ? C3 C4 1.400(6) . ? C3 H3 0.9500 . ? C4 C5 1.381(5) . ? C4 H4 0.9500 . ? C5 C6 1.409(5) . ? C5 C10 1.514(5) . ? C6 C7 1.498(5) . ? C7 C8 1.536(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.523(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.519(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.406(4) . ? C11 C16 1.417(4) . ? C12 C13 1.392(4) . ? C13 C14 1.383(4) . ? C13 H13 0.9500 . ? C14 C15 1.399(4) . ? C14 H14 0.9500 . ? C15 C16 1.397(4) . ? C15 C20 1.512(4) . ? C16 C17 1.523(4) . ? C17 C18 1.531(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.515(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.529(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.416(4) . ? C22 H22 0.9500 . ? C23 C24 1.393(4) . ? C24 C25 1.390(5) . ? C24 H24 0.9500 . ? C25 C26 1.399(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.399(4) . ? C27 C32 1.402(4) . ? C27 C37 1.500(4) . ? C28 C29 1.393(4) . ? C29 C30 1.389(4) . ? C29 H29 0.9500 . ? C30 C31 1.391(4) . ? C30 H30 0.9500 . ? C31 C32 1.404(4) . ? C31 C36 1.520(4) . ? C32 C33 1.507(4) . ? C33 C34 1.523(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.498(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.517(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.400(4) . ? C37 C42 1.412(4) . ? C38 C39 1.403(4) . ? C39 C40 1.386(4) . ? C39 H39 0.9500 . ? C40 C41 1.394(5) . ? C40 H40 0.9500 . ? C41 C42 1.397(4) . ? C41 C46 1.510(4) . ? C42 C43 1.525(4) . ? C43 C44 1.545(5) . ? C43 C44' 1.551(7) . ? C43 H43A 0.9599 . ? C43 H43B 0.9601 . ? C43 H43C 0.9599 . ? C43 H43D 0.9600 . ? C44 C45 1.522(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.525(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C44' C45' 1.523(9) . ? C44' H44C 0.9900 . ? C44' H44D 0.9900 . ? C45' C46 1.498(8) . ? C45' H45C 0.9900 . ? C45' H45D 0.9900 . ? C46 H46A 0.9599 . ? C46 H46B 0.9601 . ? C46 H46C 0.9599 . ? C46 H46D 0.9600 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.404(4) . ? C48 H48 0.9500 . ? C49 C50 1.410(4) . ? C50 C51 1.392(4) . ? C50 H50 0.9500 . ? C51 C52 1.401(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Zr1 N6 100.76(11) . . ? N5 Zr1 N3 100.27(10) . . ? N6 Zr1 N3 93.30(9) . . ? N5 Zr1 N2 162.99(10) . . ? N6 Zr1 N2 94.60(10) . . ? N3 Zr1 N2 85.98(9) . . ? N5 Zr1 N4 88.12(10) . . ? N6 Zr1 N4 164.39(9) . . ? N3 Zr1 N4 72.34(8) . . ? N2 Zr1 N4 78.66(9) . . ? N5 Zr1 N1 96.64(9) . . ? N6 Zr1 N1 105.92(10) . . ? N3 Zr1 N1 151.49(9) . . ? N2 Zr1 N1 71.91(8) . . ? N4 Zr1 N1 85.53(9) . . ? C22 N1 C12 118.5(2) . . ? C22 N1 Zr1 114.02(18) . . ? C12 N1 Zr1 127.25(19) . . ? C26 N2 C23 105.2(3) . . ? C26 N2 Zr1 138.2(2) . . ? C23 N2 Zr1 114.02(18) . . ? C48 N3 C38 116.9(2) . . ? C48 N3 Zr1 115.25(19) . . ? C38 N3 Zr1 127.85(18) . . ? C52 N4 C49 105.9(2) . . ? C52 N4 Zr1 140.5(2) . . ? C49 N4 Zr1 113.66(18) . . ? C53 N5 C54 110.3(3) . . ? C53 N5 Zr1 121.9(2) . . ? C54 N5 Zr1 127.4(2) . . ? C56 N6 C55 108.7(3) . . ? C56 N6 Zr1 126.3(2) . . ? C55 N6 Zr1 124.2(2) . . ? C2 O1 C21 118.1(3) . . ? C28 O2 C47 117.2(2) . . ? C2 C1 C6 119.9(3) . . ? C2 C1 C11 118.9(3) . . ? C6 C1 C11 120.7(3) . . ? C3 C2 O1 123.5(3) . . ? C3 C2 C1 121.5(3) . . ? O1 C2 C1 114.9(3) . . ? C2 C3 C4 117.9(4) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C5 C4 C3 122.5(3) . . ? C5 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C4 C5 C6 118.9(3) . . ? C4 C5 C10 119.6(3) . . ? C6 C5 C10 121.6(3) . . ? C5 C6 C1 119.3(3) . . ? C5 C6 C7 122.0(3) . . ? C1 C6 C7 118.7(3) . . ? C6 C7 C8 114.0(3) . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 111.4(3) . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 110.7(3) . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C5 C10 C9 112.3(3) . . ? C5 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? C5 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C16 119.8(3) . . ? C12 C11 C1 122.9(3) . . ? C16 C11 C1 117.3(3) . . ? C13 C12 C11 119.1(3) . . ? C13 C12 N1 118.3(3) . . ? C11 C12 N1 122.6(3) . . ? C14 C13 C12 120.6(3) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 121.5(3) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C16 C15 C14 118.5(3) . . ? C16 C15 C20 122.6(3) . . ? C14 C15 C20 118.9(3) . . ? C15 C16 C11 120.3(3) . . ? C15 C16 C17 120.4(3) . . ? C11 C16 C17 119.2(3) . . ? C16 C17 C18 113.0(3) . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? C16 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C19 C18 C17 110.8(3) . . ? C19 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C18 C19 C20 110.5(3) . . ? C18 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? C18 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? C15 C20 C19 114.0(3) . . ? C15 C20 H20A 108.8 . . ? C19 C20 H20A 108.8 . . ? C15 C20 H20B 108.8 . . ? C19 C20 H20B 108.8 . . ? H20A C20 H20B 107.6 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C23 120.8(3) . . ? N1 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? N2 C23 C24 110.6(3) . . ? N2 C23 C22 118.0(3) . . ? C24 C23 C22 131.4(3) . . ? C25 C24 C23 106.4(3) . . ? C25 C24 H24 126.8 . . ? C23 C24 H24 126.8 . . ? C24 C25 C26 106.4(3) . . ? C24 C25 H25 126.8 . . ? C26 C25 H25 126.8 . . ? N2 C26 C25 111.5(3) . . ? N2 C26 H26 124.3 . . ? C25 C26 H26 124.3 . . ? C28 C27 C32 119.7(3) . . ? C28 C27 C37 119.7(3) . . ? C32 C27 C37 120.6(3) . . ? O2 C28 C29 123.8(3) . . ? O2 C28 C27 115.3(2) . . ? C29 C28 C27 120.9(3) . . ? C30 C29 C28 118.7(3) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C29 C30 C31 121.5(3) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C30 C31 C32 119.5(3) . . ? C30 C31 C36 118.6(3) . . ? C32 C31 C36 121.9(3) . . ? C27 C32 C31 119.5(3) . . ? C27 C32 C33 120.1(3) . . ? C31 C32 C33 120.4(3) . . ? C32 C33 C34 113.4(3) . . ? C32 C33 H33A 108.9 . . ? C34 C33 H33A 108.9 . . ? C32 C33 H33B 108.9 . . ? C34 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C35 C34 C33 111.9(3) . . ? C35 C34 H34A 109.2 . . ? C33 C34 H34A 109.2 . . ? C35 C34 H34B 109.2 . . ? C33 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C34 C35 C36 113.0(3) . . ? C34 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? C34 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C35 C36 C31 115.1(3) . . ? C35 C36 H36A 108.5 . . ? C31 C36 H36A 108.5 . . ? C35 C36 H36B 108.5 . . ? C31 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? C38 C37 C42 119.2(3) . . ? C38 C37 C27 121.9(2) . . ? C42 C37 C27 118.8(3) . . ? C37 C38 C39 119.8(3) . . ? C37 C38 N3 122.2(2) . . ? C39 C38 N3 118.0(3) . . ? C40 C39 C38 119.9(3) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C41 121.6(3) . . ? C39 C40 H40 119.2 . . ? C41 C40 H40 119.2 . . ? C40 C41 C42 118.5(3) . . ? C40 C41 C46 119.7(3) . . ? C42 C41 C46 121.8(3) . . ? C41 C42 C37 121.0(3) . . ? C41 C42 C43 121.1(3) . . ? C37 C42 C43 118.0(3) . . ? C42 C43 C44 113.7(3) . . ? C42 C43 C44' 111.5(5) . . ? C44 C43 C44' 32.9(4) . . ? C42 C43 H43A 108.6 . . ? C44 C43 H43A 108.4 . . ? C44' C43 H43A 133.7 . . ? C42 C43 H43B 109.1 . . ? C44 C43 H43B 109.0 . . ? C44' C43 H43B 79.8 . . ? H43A C43 H43B 107.8 . . ? C42 C43 H43C 109.3 . . ? C44 C43 H43C 77.8 . . ? C44' C43 H43C 108.9 . . ? H43A C43 H43C 34.0 . . ? H43B C43 H43C 133.5 . . ? C42 C43 H43D 109.5 . . ? C44 C43 H43D 131.2 . . ? C44' C43 H43D 109.4 . . ? H43A C43 H43D 76.9 . . ? H43B C43 H43D 33.0 . . ? H43C C43 H43D 108.1 . . ? C45 C44 C43 109.1(5) . . ? C45 C44 H44A 109.9 . . ? C43 C44 H44A 109.9 . . ? C45 C44 H44B 109.9 . . ? C43 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? C44 C45 C46 111.5(5) . . ? C44 C45 H45A 109.3 . . ? C46 C45 H45A 109.3 . . ? C44 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 108.0 . . ? C45' C44' C43 109.0(8) . . ? C45' C44' H44C 109.9 . . ? C43 C44' H44C 109.9 . . ? C45' C44' H44D 109.9 . . ? C43 C44' H44D 109.9 . . ? H44C C44' H44D 108.3 . . ? C46 C45' C44' 109.8(8) . . ? C46 C45' H45C 109.7 . . ? C44' C45' H45C 109.7 . . ? C46 C45' H45D 109.7 . . ? C44' C45' H45D 109.7 . . ? H45C C45' H45D 108.2 . . ? C45' C46 C41 114.0(5) . . ? C45' C46 C45 26.0(4) . . ? C41 C46 C45 113.8(3) . . ? C45' C46 H46A 127.8 . . ? C41 C46 H46A 108.8 . . ? C45 C46 H46A 108.3 . . ? C45' C46 H46B 85.8 . . ? C41 C46 H46B 108.6 . . ? C45 C46 H46B 109.4 . . ? H46A C46 H46B 107.7 . . ? C45' C46 H46C 108.6 . . ? C41 C46 H46C 108.9 . . ? C45 C46 H46C 85.0 . . ? H46A C46 H46C 26.5 . . ? H46B C46 H46C 129.0 . . ? C45' C46 H46D 108.8 . . ? C41 C46 H46D 108.7 . . ? C45 C46 H46D 128.4 . . ? H46A C46 H46D 83.3 . . ? H46B C46 H46D 26.3 . . ? H46C C46 H46D 107.7 . . ? O2 C47 H47A 109.5 . . ? O2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N3 C48 C49 120.4(3) . . ? N3 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? N4 C49 C48 118.2(2) . . ? N4 C49 C50 110.1(3) . . ? C48 C49 C50 131.6(3) . . ? C51 C50 C49 106.1(3) . . ? C51 C50 H50 127.0 . . ? C49 C50 H50 127.0 . . ? C50 C51 C52 106.6(3) . . ? C50 C51 H51 126.7 . . ? C52 C51 H51 126.7 . . ? N4 C52 C51 111.3(3) . . ? N4 C52 H52 124.3 . . ? C51 C52 H52 124.3 . . ? N5 C53 H53A 109.5 . . ? N5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N5 C54 H54A 109.5 . . ? N5 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N5 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N6 C55 H55A 109.5 . . ? N6 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N6 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N6 C56 H56A 109.5 . . ? N6 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N6 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Zr1 N1 C22 -158.7(2) . . . . ? N6 Zr1 N1 C22 98.1(2) . . . . ? N3 Zr1 N1 C22 -32.5(3) . . . . ? N2 Zr1 N1 C22 8.4(2) . . . . ? N4 Zr1 N1 C22 -71.1(2) . . . . ? N5 Zr1 N1 C12 16.3(2) . . . . ? N6 Zr1 N1 C12 -86.9(2) . . . . ? N3 Zr1 N1 C12 142.5(2) . . . . ? N2 Zr1 N1 C12 -176.6(3) . . . . ? N4 Zr1 N1 C12 103.9(2) . . . . ? N5 Zr1 N2 C26 -118.9(4) . . . . ? N6 Zr1 N2 C26 86.5(3) . . . . ? N3 Zr1 N2 C26 -6.5(3) . . . . ? N4 Zr1 N2 C26 -79.2(3) . . . . ? N1 Zr1 N2 C26 -168.2(3) . . . . ? N5 Zr1 N2 C23 39.4(5) . . . . ? N6 Zr1 N2 C23 -115.2(2) . . . . ? N3 Zr1 N2 C23 151.8(2) . . . . ? N4 Zr1 N2 C23 79.1(2) . . . . ? N1 Zr1 N2 C23 -9.89(19) . . . . ? N5 Zr1 N3 C48 87.8(2) . . . . ? N6 Zr1 N3 C48 -170.6(2) . . . . ? N2 Zr1 N3 C48 -76.3(2) . . . . ? N4 Zr1 N3 C48 3.1(2) . . . . ? N1 Zr1 N3 C48 -37.6(3) . . . . ? N5 Zr1 N3 C38 -89.8(2) . . . . ? N6 Zr1 N3 C38 11.8(2) . . . . ? N2 Zr1 N3 C38 106.2(2) . . . . ? N4 Zr1 N3 C38 -174.5(2) . . . . ? N1 Zr1 N3 C38 144.8(2) . . . . ? N5 Zr1 N4 C52 77.8(3) . . . . ? N6 Zr1 N4 C52 -157.0(4) . . . . ? N3 Zr1 N4 C52 179.2(4) . . . . ? N2 Zr1 N4 C52 -91.4(3) . . . . ? N1 Zr1 N4 C52 -19.0(3) . . . . ? N5 Zr1 N4 C49 -104.7(2) . . . . ? N6 Zr1 N4 C49 20.5(5) . . . . ? N3 Zr1 N4 C49 -3.34(19) . . . . ? N2 Zr1 N4 C49 86.0(2) . . . . ? N1 Zr1 N4 C49 158.4(2) . . . . ? N6 Zr1 N5 C53 34.8(3) . . . . ? N3 Zr1 N5 C53 130.2(2) . . . . ? N2 Zr1 N5 C53 -119.4(4) . . . . ? N4 Zr1 N5 C53 -158.1(2) . . . . ? N1 Zr1 N5 C53 -72.9(2) . . . . ? N6 Zr1 N5 C54 -153.2(3) . . . . ? N3 Zr1 N5 C54 -57.8(3) . . . . ? N2 Zr1 N5 C54 52.6(5) . . . . ? N4 Zr1 N5 C54 13.9(3) . . . . ? N1 Zr1 N5 C54 99.1(3) . . . . ? N5 Zr1 N6 C56 -164.0(2) . . . . ? N3 Zr1 N6 C56 94.9(2) . . . . ? N2 Zr1 N6 C56 8.7(2) . . . . ? N4 Zr1 N6 C56 72.3(5) . . . . ? N1 Zr1 N6 C56 -63.8(3) . . . . ? N5 Zr1 N6 C55 27.6(3) . . . . ? N3 Zr1 N6 C55 -73.5(2) . . . . ? N2 Zr1 N6 C55 -159.7(2) . . . . ? N4 Zr1 N6 C55 -96.2(4) . . . . ? N1 Zr1 N6 C55 127.8(2) . . . . ? C21 O1 C2 C3 -12.7(6) . . . . ? C21 O1 C2 C1 169.8(4) . . . . ? C6 C1 C2 C3 1.0(5) . . . . ? C11 C1 C2 C3 173.1(3) . . . . ? C6 C1 C2 O1 178.6(3) . . . . ? C11 C1 C2 O1 -9.3(5) . . . . ? O1 C2 C3 C4 -178.7(3) . . . . ? C1 C2 C3 C4 -1.4(6) . . . . ? C2 C3 C4 C5 1.1(6) . . . . ? C3 C4 C5 C6 -0.5(6) . . . . ? C3 C4 C5 C10 179.5(3) . . . . ? C4 C5 C6 C1 0.1(5) . . . . ? C10 C5 C6 C1 -179.9(3) . . . . ? C4 C5 C6 C7 179.6(3) . . . . ? C10 C5 C6 C7 -0.3(5) . . . . ? C2 C1 C6 C5 -0.3(5) . . . . ? C11 C1 C6 C5 -172.2(3) . . . . ? C2 C1 C6 C7 -179.9(3) . . . . ? C11 C1 C6 C7 8.2(4) . . . . ? C5 C6 C7 C8 10.9(4) . . . . ? C1 C6 C7 C8 -169.5(3) . . . . ? C6 C7 C8 C9 -40.8(4) . . . . ? C7 C8 C9 C10 61.2(4) . . . . ? C4 C5 C10 C9 -160.0(3) . . . . ? C6 C5 C10 C9 20.0(4) . . . . ? C8 C9 C10 C5 -49.7(4) . . . . ? C2 C1 C11 C12 104.2(4) . . . . ? C6 C1 C11 C12 -83.8(4) . . . . ? C2 C1 C11 C16 -76.3(4) . . . . ? C6 C1 C11 C16 95.7(4) . . . . ? C16 C11 C12 C13 3.9(4) . . . . ? C1 C11 C12 C13 -176.5(3) . . . . ? C16 C11 C12 N1 -174.7(3) . . . . ? C1 C11 C12 N1 4.8(5) . . . . ? C22 N1 C12 C13 127.8(3) . . . . ? Zr1 N1 C12 C13 -47.0(4) . . . . ? C22 N1 C12 C11 -53.5(4) . . . . ? Zr1 N1 C12 C11 131.7(3) . . . . ? C11 C12 C13 C14 -2.5(4) . . . . ? N1 C12 C13 C14 176.3(3) . . . . ? C12 C13 C14 C15 -0.5(5) . . . . ? C13 C14 C15 C16 1.8(5) . . . . ? C13 C14 C15 C20 -178.2(3) . . . . ? C14 C15 C16 C11 -0.3(4) . . . . ? C20 C15 C16 C11 179.7(3) . . . . ? C14 C15 C16 C17 -180.0(3) . . . . ? C20 C15 C16 C17 0.1(5) . . . . ? C12 C11 C16 C15 -2.6(4) . . . . ? C1 C11 C16 C15 177.9(3) . . . . ? C12 C11 C16 C17 177.1(3) . . . . ? C1 C11 C16 C17 -2.5(4) . . . . ? C15 C16 C17 C18 18.1(4) . . . . ? C11 C16 C17 C18 -161.5(3) . . . . ? C16 C17 C18 C19 -48.9(4) . . . . ? C17 C18 C19 C20 61.9(4) . . . . ? C16 C15 C20 C19 12.7(5) . . . . ? C14 C15 C20 C19 -167.3(3) . . . . ? C18 C19 C20 C15 -43.1(4) . . . . ? C12 N1 C22 C23 178.6(3) . . . . ? Zr1 N1 C22 C23 -6.0(4) . . . . ? C26 N2 C23 C24 -0.9(3) . . . . ? Zr1 N2 C23 C24 -166.1(2) . . . . ? C26 N2 C23 C22 176.1(3) . . . . ? Zr1 N2 C23 C22 10.9(3) . . . . ? N1 C22 C23 N2 -3.3(4) . . . . ? N1 C22 C23 C24 173.0(3) . . . . ? N2 C23 C24 C25 1.1(4) . . . . ? C22 C23 C24 C25 -175.4(3) . . . . ? C23 C24 C25 C26 -0.8(4) . . . . ? C23 N2 C26 C25 0.4(3) . . . . ? Zr1 N2 C26 C25 159.9(2) . . . . ? C24 C25 C26 N2 0.3(4) . . . . ? C47 O2 C28 C29 5.5(4) . . . . ? C47 O2 C28 C27 -174.2(3) . . . . ? C32 C27 C28 O2 -176.2(3) . . . . ? C37 C27 C28 O2 2.3(4) . . . . ? C32 C27 C28 C29 4.1(4) . . . . ? C37 C27 C28 C29 -177.3(3) . . . . ? O2 C28 C29 C30 177.3(3) . . . . ? C27 C28 C29 C30 -3.1(5) . . . . ? C28 C29 C30 C31 -0.7(5) . . . . ? C29 C30 C31 C32 3.5(5) . . . . ? C29 C30 C31 C36 -174.3(3) . . . . ? C28 C27 C32 C31 -1.3(4) . . . . ? C37 C27 C32 C31 -179.8(3) . . . . ? C28 C27 C32 C33 177.7(3) . . . . ? C37 C27 C32 C33 -0.9(4) . . . . ? C30 C31 C32 C27 -2.5(5) . . . . ? C36 C31 C32 C27 175.3(3) . . . . ? C30 C31 C32 C33 178.5(3) . . . . ? C36 C31 C32 C33 -3.7(5) . . . . ? C27 C32 C33 C34 -155.4(3) . . . . ? C31 C32 C33 C34 23.6(4) . . . . ? C32 C33 C34 C35 -49.5(4) . . . . ? C33 C34 C35 C36 56.2(5) . . . . ? C34 C35 C36 C31 -35.8(5) . . . . ? C30 C31 C36 C35 -172.6(3) . . . . ? C32 C31 C36 C35 9.6(5) . . . . ? C28 C27 C37 C38 91.0(4) . . . . ? C32 C27 C37 C38 -90.5(4) . . . . ? C28 C27 C37 C42 -90.6(3) . . . . ? C32 C27 C37 C42 88.0(3) . . . . ? C42 C37 C38 C39 -1.3(4) . . . . ? C27 C37 C38 C39 177.1(3) . . . . ? C42 C37 C38 N3 -178.8(3) . . . . ? C27 C37 C38 N3 -0.4(4) . . . . ? C48 N3 C38 C37 -56.2(4) . . . . ? Zr1 N3 C38 C37 121.4(3) . . . . ? C48 N3 C38 C39 126.3(3) . . . . ? Zr1 N3 C38 C39 -56.1(3) . . . . ? C37 C38 C39 C40 0.9(4) . . . . ? N3 C38 C39 C40 178.4(3) . . . . ? C38 C39 C40 C41 -0.4(4) . . . . ? C39 C40 C41 C42 0.4(4) . . . . ? C39 C40 C41 C46 179.0(3) . . . . ? C40 C41 C42 C37 -0.9(4) . . . . ? C46 C41 C42 C37 -179.5(3) . . . . ? C40 C41 C42 C43 179.6(3) . . . . ? C46 C41 C42 C43 0.9(4) . . . . ? C38 C37 C42 C41 1.3(4) . . . . ? C27 C37 C42 C41 -177.2(3) . . . . ? C38 C37 C42 C43 -179.1(3) . . . . ? C27 C37 C42 C43 2.4(4) . . . . ? C41 C42 C43 C44 -17.7(5) . . . . ? C37 C42 C43 C44 162.7(4) . . . . ? C41 C42 C43 C44' 18.0(6) . . . . ? C37 C42 C43 C44' -161.6(5) . . . . ? C42 C43 C44 C45 47.2(7) . . . . ? C44' C43 C44 C45 -46.2(7) . . . . ? C43 C44 C45 C46 -61.9(8) . . . . ? C42 C43 C44' C45' -50.5(10) . . . . ? C44 C43 C44' C45' 50.3(7) . . . . ? C43 C44' C45' C46 66.0(12) . . . . ? C44' C45' C46 C41 -46.8(11) . . . . ? C44' C45' C46 C45 48.8(9) . . . . ? C40 C41 C46 C45' -165.0(6) . . . . ? C42 C41 C46 C45' 13.6(7) . . . . ? C40 C41 C46 C45 166.5(4) . . . . ? C42 C41 C46 C45 -14.9(5) . . . . ? C44 C45 C46 C45' -50.5(11) . . . . ? C44 C45 C46 C41 45.7(7) . . . . ? C38 N3 C48 C49 175.3(3) . . . . ? Zr1 N3 C48 C49 -2.6(4) . . . . ? C52 N4 C49 C48 -178.3(3) . . . . ? Zr1 N4 C49 C48 3.4(3) . . . . ? C52 N4 C49 C50 -0.7(3) . . . . ? Zr1 N4 C49 C50 -179.0(2) . . . . ? N3 C48 C49 N4 -0.6(4) . . . . ? N3 C48 C49 C50 -177.6(3) . . . . ? N4 C49 C50 C51 0.5(3) . . . . ? C48 C49 C50 C51 177.6(3) . . . . ? C49 C50 C51 C52 0.0(4) . . . . ? C49 N4 C52 C51 0.7(4) . . . . ? Zr1 N4 C52 C51 178.3(2) . . . . ? C50 C51 C52 N4 -0.5(4) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.079 0.250 0.500 500.4 67.1 2 -0.106 0.750 1.000 500.4 66.8 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.430 _refine_diff_density_min -2.326 _refine_diff_density_rms 0.061 # Attachment 'compound_14.cif' data_14 _database_code_depnum_ccdc_archive 'CCDC 687853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H56 N6 O2 Ti' _chemical_formula_sum 'C50 H56 N6 O2 Ti' _chemical_formula_weight 820.91 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 19.454(2) _cell_length_b 19.6057(15) _cell_length_c 24.4069(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.122(4) _cell_angle_gamma 90.00 _cell_volume 9309.1(14) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 21233 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 26.4 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3488 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9473 _exptl_absorpt_correction_T_max 0.9601 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 69902 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0869 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 31863 _reflns_number_gt 28839 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0839P)^2^+3.7239P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_number_reflns 31863 _refine_ls_number_parameters 2100 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.1966 _refine_ls_wR_factor_gt 0.1871 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.22167(7) 0.75576(6) 0.98516(6) 0.0298(3) Uani 1 1 d . . . Ti2 Ti 0.28919(7) 0.05732(6) 0.72792(6) 0.0337(3) Uani 1 1 d . . . Ti3 Ti 0.73170(7) 0.56445(7) 0.76414(6) 0.0343(3) Uani 1 1 d . . . Ti4 Ti 0.78202(7) 0.24765(6) 0.52271(6) 0.0311(3) Uani 1 1 d . . . N1 N 0.1531(3) 0.8341(3) 0.9532(3) 0.0338(15) Uani 1 1 d . . . N2 N 0.2229(3) 0.7392(4) 0.8963(3) 0.0341(15) Uani 1 1 d . . . N3 N 0.3147(3) 0.6878(3) 0.9856(3) 0.0312(15) Uani 1 1 d . . . N4 N 0.3079(4) 0.8233(4) 0.9633(3) 0.0403(17) Uani 1 1 d . . . N5 N 0.2260(3) 0.7892(4) 1.0599(3) 0.0406(17) Uani 1 1 d . . . N6 N 0.1551(3) 0.6851(3) 0.9945(3) 0.0335(15) Uani 1 1 d . . . N7 N 0.1990(4) 0.1242(3) 0.7338(3) 0.0367(16) Uani 1 1 d . . . N8 N 0.2008(3) -0.0098(4) 0.7088(3) 0.0354(16) Uani 1 1 d . . . N9 N 0.3548(3) -0.0255(3) 0.6956(3) 0.0292(14) Uani 1 1 d . . . N10 N 0.2805(3) 0.0701(3) 0.6385(3) 0.0337(15) Uani 1 1 d . . . N11 N 0.2894(4) 0.0273(3) 0.8033(3) 0.0388(17) Uani 1 1 d . . . N12 N 0.3600(4) 0.1282(3) 0.7329(3) 0.0430(17) Uani 1 1 d . . . N13 N 0.6618(3) 0.4856(4) 0.7986(3) 0.0363(16) Uani 1 1 d . . . N14 N 0.7325(4) 0.5852(4) 0.8525(3) 0.0399(17) Uani 1 1 d . . . N15 N 0.8219(4) 0.6324(4) 0.7614(3) 0.0401(17) Uani 1 1 d . . . N16 N 0.8177(4) 0.4976(4) 0.7897(3) 0.0388(17) Uani 1 1 d . . . N17 N 0.7348(3) 0.5274(3) 0.6900(3) 0.0320(15) Uani 1 1 d . . . N18 N 0.6646(4) 0.6350(3) 0.7502(3) 0.0406(17) Uani 1 1 d . . . N19 N 0.8487(3) 0.3256(3) 0.5574(3) 0.0309(15) Uani 1 1 d . . . N20 N 0.7790(3) 0.2299(3) 0.6112(3) 0.0356(16) Uani 1 1 d . . . N21 N 0.6914(3) 0.1793(3) 0.5166(3) 0.0300(14) Uani 1 1 d . . . N22 N 0.6935(3) 0.3127(3) 0.5441(3) 0.0331(15) Uani 1 1 d . . . N23 N 0.7801(4) 0.2824(4) 0.4491(3) 0.0415(17) Uani 1 1 d . . . N24 N 0.8513(3) 0.1791(3) 0.5149(3) 0.0363(16) Uani 1 1 d . . . O1 O 0.0116(3) 0.9116(4) 0.8648(3) 0.0522(17) Uani 1 1 d . . . O2 O 0.4973(3) 0.6094(3) 1.0056(3) 0.0490(16) Uani 1 1 d . . . O3 O 0.0236(3) 0.2060(3) 0.7699(3) 0.0537(17) Uani 1 1 d . . . O4 O 0.4919(3) -0.1046(4) 0.6120(3) 0.0490(16) Uani 1 1 d . . . O5 O 0.5135(3) 0.4106(3) 0.8820(2) 0.0440(15) Uani 1 1 d . . . O6 O 1.0048(3) 0.7097(4) 0.7388(3) 0.0605(18) Uani 1 1 d . . . O7 O 0.9932(3) 0.4070(4) 0.6415(3) 0.0533(17) Uani 1 1 d . . . O8 O 0.5144(3) 0.0996(3) 0.4832(2) 0.0448(15) Uani 1 1 d . . . C1 C 0.0004(4) 0.8372(4) 0.9422(3) 0.0348(18) Uani 1 1 d . . . C2 C -0.0129(5) 0.8525(5) 0.8854(4) 0.045(2) Uani 1 1 d . . . C3 C -0.0473(5) 0.8041(6) 0.8529(4) 0.055(3) Uani 1 1 d . . . H3 H -0.0523 0.8117 0.8147 0.067 Uiso 1 1 calc R . . C4 C -0.0738(4) 0.7456(6) 0.8761(5) 0.058(3) Uani 1 1 d . . . H4 H -0.0991 0.7145 0.8540 0.070 Uiso 1 1 calc R . . C5 C -0.0638(5) 0.7318(5) 0.9319(5) 0.055(3) Uani 1 1 d . . . H5 H -0.0825 0.6911 0.9470 0.066 Uiso 1 1 calc R . . C6 C -0.0271(4) 0.7761(4) 0.9662(4) 0.039(2) Uani 1 1 d . . . C7 C -0.0161(4) 0.7641(5) 1.0269(4) 0.044(2) Uani 1 1 d . . . H7A H 0.0321 0.7521 1.0336 0.067 Uiso 1 1 calc R . . H7B H -0.0457 0.7268 1.0392 0.067 Uiso 1 1 calc R . . H7C H -0.0275 0.8058 1.0472 0.067 Uiso 1 1 calc R . . C8 C 0.0411(4) 0.8896(4) 0.9751(3) 0.0303(17) Uani 1 1 d . . . C9 C 0.1120(4) 0.8866(4) 0.9815(3) 0.0318(18) Uani 1 1 d . . . C10 C 0.1468(5) 0.9309(4) 1.0175(3) 0.038(2) Uani 1 1 d . . . H10 H 0.1947 0.9256 1.0236 0.046 Uiso 1 1 calc R . . C11 C 0.1115(4) 0.9818(4) 1.0437(4) 0.040(2) Uani 1 1 d . . . H11 H 0.1354 1.0134 1.0663 0.048 Uiso 1 1 calc R . . C12 C 0.0394(5) 0.9873(4) 1.0373(4) 0.041(2) Uani 1 1 d . . . H12 H 0.0147 1.0220 1.0560 0.049 Uiso 1 1 calc R . . C13 C 0.0044(4) 0.9406(4) 1.0028(4) 0.040(2) Uani 1 1 d . . . C14 C -0.0762(4) 0.9467(5) 0.9972(4) 0.045(2) Uani 1 1 d . . . H14A H -0.0884 0.9538 0.9586 0.067 Uiso 1 1 calc R . . H14B H -0.0925 0.9854 1.0190 0.067 Uiso 1 1 calc R . . H14C H -0.0978 0.9046 1.0104 0.067 Uiso 1 1 calc R . . C15 C 0.0180(6) 0.9214(8) 0.8073(4) 0.075(4) Uani 1 1 d . . . H15A H 0.0516 0.8890 0.7926 0.112 Uiso 1 1 calc R . . H15B H 0.0334 0.9681 0.8000 0.112 Uiso 1 1 calc R . . H15C H -0.0267 0.9138 0.7897 0.112 Uiso 1 1 calc R . . C16 C 0.1531(4) 0.8427(4) 0.8982(3) 0.0325(17) Uani 1 1 d . . . H16 H 0.1288 0.8790 0.8811 0.039 Uiso 1 1 calc R . . C17 C 0.1919(3) 0.7938(4) 0.8670(3) 0.0333(18) Uani 1 1 d . . . C18 C 0.2040(4) 0.7897(4) 0.8104(3) 0.0369(18) Uani 1 1 d . . . H18 H 0.1891 0.8202 0.7826 0.044 Uiso 1 1 calc R . . C19 C 0.2437(4) 0.7297(5) 0.8044(4) 0.048(2) Uani 1 1 d . . . H19 H 0.2593 0.7108 0.7708 0.058 Uiso 1 1 calc R . . C20 C 0.2559(4) 0.7027(4) 0.8574(4) 0.041(2) Uani 1 1 d . . . H20 H 0.2838 0.6640 0.8647 0.049 Uiso 1 1 calc R . . C21 C 0.4124(5) 0.6398(4) 1.0690(3) 0.0379(19) Uani 1 1 d . . . C22 C 0.4818(5) 0.6459(4) 1.0514(3) 0.044(2) Uani 1 1 d . . . C23 C 0.5284(5) 0.6891(5) 1.0792(4) 0.052(2) Uani 1 1 d . . . H23 H 0.5748 0.6923 1.0672 0.062 Uiso 1 1 calc R . . C24 C 0.5073(5) 0.7251(5) 1.1220(4) 0.051(2) Uani 1 1 d . . . H24 H 0.5388 0.7548 1.1398 0.062 Uiso 1 1 calc R . . C25 C 0.4392(6) 0.7204(5) 1.1419(4) 0.055(3) Uani 1 1 d . . . H25 H 0.4249 0.7463 1.1728 0.066 Uiso 1 1 calc R . . C26 C 0.3932(5) 0.6761(4) 1.1145(3) 0.045(2) Uani 1 1 d . . . C27 C 0.3204(5) 0.6656(5) 1.1371(4) 0.048(2) Uani 1 1 d . . . H27A H 0.2876 0.6921 1.1152 0.072 Uiso 1 1 calc R . . H27B H 0.3187 0.6808 1.1753 0.072 Uiso 1 1 calc R . . H27C H 0.3084 0.6171 1.1352 0.072 Uiso 1 1 calc R . . C28 C 0.3658(4) 0.5914(4) 1.0367(3) 0.0344(19) Uani 1 1 d . . . C29 C 0.3186(4) 0.6176(4) 0.9995(4) 0.037(2) Uani 1 1 d . . . C30 C 0.2732(4) 0.5731(4) 0.9691(4) 0.0354(18) Uani 1 1 d . . . H30 H 0.2423 0.5907 0.9424 0.042 Uiso 1 1 calc R . . C31 C 0.2762(5) 0.5031(4) 0.9804(4) 0.045(2) Uani 1 1 d . . . H31 H 0.2447 0.4734 0.9626 0.054 Uiso 1 1 calc R . . C32 C 0.3242(4) 0.4756(4) 1.0171(4) 0.044(2) Uani 1 1 d . . . H32 H 0.3261 0.4278 1.0230 0.053 Uiso 1 1 calc R . . C33 C 0.3696(4) 0.5193(4) 1.0450(3) 0.0355(18) Uani 1 1 d . . . C34 C 0.4248(5) 0.4912(5) 1.0858(4) 0.061(3) Uani 1 1 d . . . H34A H 0.4708 0.4987 1.0706 0.091 Uiso 1 1 calc R . . H34B H 0.4174 0.4423 1.0915 0.091 Uiso 1 1 calc R . . H34C H 0.4209 0.5152 1.1209 0.091 Uiso 1 1 calc R . . C35 C 0.5692(4) 0.6059(7) 0.9875(5) 0.068(3) Uani 1 1 d . . . H35A H 0.5844 0.6513 0.9758 0.103 Uiso 1 1 calc R . . H35B H 0.5730 0.5741 0.9567 0.103 Uiso 1 1 calc R . . H35C H 0.5982 0.5901 1.0178 0.103 Uiso 1 1 calc R . . C36 C 0.3700(4) 0.7208(4) 0.9701(3) 0.0347(19) Uani 1 1 d . . . H36 H 0.4117 0.6960 0.9670 0.042 Uiso 1 1 calc R . . C37 C 0.3709(4) 0.7891(5) 0.9582(4) 0.042(2) Uani 1 1 d . . . C38 C 0.4219(4) 0.8374(4) 0.9442(3) 0.0339(19) Uani 1 1 d . . . H38 H 0.4694 0.8282 0.9395 0.041 Uiso 1 1 calc R . . C39 C 0.3900(5) 0.9008(4) 0.9385(3) 0.042(2) Uani 1 1 d . . . H39 H 0.4109 0.9425 0.9280 0.050 Uiso 1 1 calc R . . C40 C 0.3203(4) 0.8900(4) 0.9516(3) 0.0353(19) Uani 1 1 d . . . H40 H 0.2864 0.9248 0.9522 0.042 Uiso 1 1 calc R . . C41 C 0.1681(4) 0.7886(4) 1.0978(4) 0.043(2) Uani 1 1 d . . . H41A H 0.1821 0.7668 1.1322 0.064 Uiso 1 1 calc R . . H41B H 0.1299 0.7630 1.0815 0.064 Uiso 1 1 calc R . . H41C H 0.1534 0.8355 1.1051 0.064 Uiso 1 1 calc R . . C42 C 0.2839(5) 0.8262(5) 1.0848(4) 0.043(2) Uani 1 1 d . . . H42A H 0.2727 0.8748 1.0870 0.065 Uiso 1 1 calc R . . H42B H 0.3251 0.8200 1.0623 0.065 Uiso 1 1 calc R . . H42C H 0.2924 0.8084 1.1217 0.065 Uiso 1 1 calc R . . C43 C 0.1490(4) 0.6390(4) 1.0436(4) 0.040(2) Uani 1 1 d . . . H43A H 0.1022 0.6417 1.0582 0.060 Uiso 1 1 calc R . . H43B H 0.1818 0.6534 1.0718 0.060 Uiso 1 1 calc R . . H43C H 0.1589 0.5919 1.0327 0.060 Uiso 1 1 calc R . . C44 C 0.1080(5) 0.6602(4) 0.9514(4) 0.047(2) Uani 1 1 d . . . H44A H 0.1258 0.6175 0.9361 0.071 Uiso 1 1 calc R . . H44B H 0.1044 0.6944 0.9223 0.071 Uiso 1 1 calc R . . H44C H 0.0624 0.6522 0.9673 0.071 Uiso 1 1 calc R . . C45 C 0.1166(5) 0.1770(4) 0.8278(4) 0.047(2) Uani 1 1 d . . . C46 C 0.0462(5) 0.1689(4) 0.8155(4) 0.046(2) Uani 1 1 d . . . C47 C 0.0059(5) 0.1276(4) 0.8465(4) 0.056(3) Uani 1 1 d . . . H47 H -0.0416 0.1236 0.8379 0.068 Uiso 1 1 calc R . . C48 C 0.0325(6) 0.0913(5) 0.8904(4) 0.055(3) Uani 1 1 d . . . H48 H 0.0044 0.0601 0.9100 0.066 Uiso 1 1 calc R . . C49 C 0.1023(6) 0.1011(4) 0.9058(4) 0.057(3) Uani 1 1 d . . . H49 H 0.1203 0.0791 0.9374 0.069 Uiso 1 1 calc R . . C50 C 0.1455(5) 0.1445(4) 0.8732(3) 0.044(2) Uani 1 1 d . . . C51 C 0.2212(5) 0.1558(5) 0.8889(4) 0.057(2) Uani 1 1 d . . . H51A H 0.2506 0.1429 0.8580 0.086 Uiso 1 1 calc R . . H51B H 0.2327 0.1277 0.9208 0.086 Uiso 1 1 calc R . . H51C H 0.2285 0.2040 0.8977 0.086 Uiso 1 1 calc R . . C52 C 0.1589(4) 0.2238(4) 0.7921(3) 0.040(2) Uani 1 1 d . . . C53 C 0.1974(4) 0.1967(4) 0.7475(3) 0.0309(17) Uani 1 1 d . . . C54 C 0.2400(4) 0.2404(4) 0.7178(4) 0.041(2) Uani 1 1 d . . . H54 H 0.2684 0.2218 0.6899 0.049 Uiso 1 1 calc R . . C55 C 0.2424(4) 0.3094(4) 0.7276(4) 0.043(2) Uani 1 1 d . . . H55 H 0.2698 0.3388 0.7058 0.051 Uiso 1 1 calc R . . C56 C 0.2031(5) 0.3346(4) 0.7708(4) 0.049(2) Uani 1 1 d . . . H56 H 0.2043 0.3821 0.7786 0.059 Uiso 1 1 calc R . . C57 C 0.1624(4) 0.2929(4) 0.8025(3) 0.043(2) Uani 1 1 d . . . C58 C 0.1198(5) 0.3231(5) 0.8490(4) 0.056(3) Uani 1 1 d . . . H58A H 0.0712 0.3122 0.8431 0.085 Uiso 1 1 calc R . . H58B H 0.1258 0.3727 0.8497 0.085 Uiso 1 1 calc R . . H58C H 0.1351 0.3037 0.8840 0.085 Uiso 1 1 calc R . . C59 C -0.0492(5) 0.2020(6) 0.7548(5) 0.076(3) Uani 1 1 d . . . H59A H -0.0629 0.1541 0.7517 0.114 Uiso 1 1 calc R . . H59B H -0.0564 0.2249 0.7196 0.114 Uiso 1 1 calc R . . H59C H -0.0769 0.2244 0.7830 0.114 Uiso 1 1 calc R . . C60 C 0.1399(4) 0.0971(4) 0.7211(3) 0.0329(18) Uani 1 1 d . . . H60 H 0.0992 0.1238 0.7202 0.040 Uiso 1 1 calc R . . C61 C 0.1383(4) 0.0251(4) 0.7082(3) 0.0349(19) Uani 1 1 d . . . C62 C 0.0854(4) -0.0162(5) 0.6903(4) 0.041(2) Uani 1 1 d . . . H62 H 0.0390 -0.0030 0.6841 0.050 Uiso 1 1 calc R . . C63 C 0.1129(5) -0.0802(5) 0.6831(4) 0.050(2) Uani 1 1 d . . . H63 H 0.0896 -0.1209 0.6729 0.060 Uiso 1 1 calc R . . C64 C 0.1834(4) -0.0719(4) 0.6943(3) 0.040(2) Uani 1 1 d . . . H64 H 0.2156 -0.1082 0.6916 0.047 Uiso 1 1 calc R . . C65 C 0.5074(4) -0.0297(4) 0.6841(3) 0.0363(19) Uani 1 1 d . . . C66 C 0.5182(5) -0.0422(5) 0.6292(4) 0.049(2) Uani 1 1 d . . . C67 C 0.5566(4) 0.0019(6) 0.5953(4) 0.059(3) Uani 1 1 d . . . H67 H 0.5636 -0.0074 0.5575 0.071 Uiso 1 1 calc R . . C68 C 0.5842(5) 0.0608(6) 0.6207(6) 0.073(4) Uani 1 1 d . . . H68 H 0.6091 0.0926 0.5992 0.088 Uiso 1 1 calc R . . C69 C 0.5757(5) 0.0735(5) 0.6764(4) 0.055(3) Uani 1 1 d . . . H69 H 0.5962 0.1123 0.6932 0.066 Uiso 1 1 calc R . . C70 C 0.5360(5) 0.0274(4) 0.7072(4) 0.047(2) Uani 1 1 d . . . C71 C 0.5288(5) 0.0483(5) 0.7679(4) 0.055(2) Uani 1 1 d . . . H71A H 0.4941 0.0843 0.7712 0.083 Uiso 1 1 calc R . . H71B H 0.5731 0.0652 0.7814 0.083 Uiso 1 1 calc R . . H71C H 0.5147 0.0086 0.7895 0.083 Uiso 1 1 calc R . . C72 C 0.4664(4) -0.0769(4) 0.7192(3) 0.0347(18) Uani 1 1 d . . . C73 C 0.3942(4) -0.0734(4) 0.7256(3) 0.0367(19) Uani 1 1 d . . . C74 C 0.3591(4) -0.1207(4) 0.7605(3) 0.0386(19) Uani 1 1 d . . . H74 H 0.3103 -0.1202 0.7629 0.046 Uiso 1 1 calc R . . C75 C 0.3972(5) -0.1674(4) 0.7909(3) 0.041(2) Uani 1 1 d . . . H75 H 0.3745 -0.1958 0.8167 0.050 Uiso 1 1 calc R . . C76 C 0.4676(5) -0.1730(5) 0.7840(4) 0.046(2) Uani 1 1 d . . . H76 H 0.4919 -0.2079 0.8029 0.055 Uiso 1 1 calc R . . C77 C 0.5034(4) -0.1287(4) 0.7501(3) 0.0342(18) Uani 1 1 d . . . C78 C 0.5814(5) -0.1354(6) 0.7430(5) 0.064(3) Uani 1 1 d . . . H78A H 0.5994 -0.1680 0.7699 0.096 Uiso 1 1 calc R . . H78B H 0.6031 -0.0908 0.7486 0.096 Uiso 1 1 calc R . . H78C H 0.5915 -0.1518 0.7060 0.096 Uiso 1 1 calc R . . C79 C 0.4857(7) -0.1141(6) 0.5536(4) 0.071(3) Uani 1 1 d . . . H79A H 0.4574 -0.0776 0.5381 0.106 Uiso 1 1 calc R . . H79B H 0.4641 -0.1583 0.5461 0.106 Uiso 1 1 calc R . . H79C H 0.5315 -0.1129 0.5369 0.106 Uiso 1 1 calc R . . C80 C 0.3528(4) -0.0289(4) 0.6414(4) 0.0378(19) Uani 1 1 d . . . H80 H 0.3779 -0.0637 0.6231 0.045 Uiso 1 1 calc R . . C81 C 0.3140(4) 0.0184(4) 0.6105(3) 0.0345(18) Uani 1 1 d . . . C82 C 0.3035(4) 0.0283(5) 0.5529(4) 0.045(2) Uani 1 1 d . . . H82 H 0.3217 0.0011 0.5242 0.054 Uiso 1 1 calc R . . C83 C 0.2615(5) 0.0853(4) 0.5469(4) 0.049(2) Uani 1 1 d . . . H83 H 0.2443 0.1037 0.5136 0.059 Uiso 1 1 calc R . . C84 C 0.2498(4) 0.1098(4) 0.5999(3) 0.0359(18) Uani 1 1 d . . . H84 H 0.2236 0.1494 0.6080 0.043 Uiso 1 1 calc R . . C85 C 0.3534(5) 0.0237(5) 0.8379(4) 0.059(3) Uani 1 1 d . . . H85A H 0.3458 0.0483 0.8723 0.088 Uiso 1 1 calc R . . H85B H 0.3917 0.0447 0.8181 0.088 Uiso 1 1 calc R . . H85C H 0.3643 -0.0240 0.8458 0.088 Uiso 1 1 calc R . . C86 C 0.2362(5) -0.0088(5) 0.8328(4) 0.051(2) Uani 1 1 d . . . H86A H 0.2456 -0.0579 0.8316 0.076 Uiso 1 1 calc R . . H86B H 0.1916 0.0004 0.8158 0.076 Uiso 1 1 calc R . . H86C H 0.2356 0.0066 0.8710 0.076 Uiso 1 1 calc R . . C87 C 0.4037(4) 0.1501(5) 0.6867(4) 0.051(2) Uani 1 1 d . . . H87A H 0.3861 0.1931 0.6718 0.077 Uiso 1 1 calc R . . H87B H 0.4029 0.1150 0.6581 0.077 Uiso 1 1 calc R . . H87C H 0.4510 0.1566 0.6996 0.077 Uiso 1 1 calc R . . C88 C 0.3729(5) 0.1724(5) 0.7803(4) 0.053(2) Uani 1 1 d . . . H88A H 0.4198 0.1648 0.7938 0.079 Uiso 1 1 calc R . . H88B H 0.3399 0.1618 0.8093 0.079 Uiso 1 1 calc R . . H88C H 0.3677 0.2203 0.7694 0.079 Uiso 1 1 calc R . . C89 C 0.5095(4) 0.4833(4) 0.8069(4) 0.039(2) Uani 1 1 d . . . C90 C 0.4911(4) 0.4719(4) 0.8618(4) 0.042(2) Uani 1 1 d . . . C91 C 0.4507(4) 0.5210(5) 0.8897(4) 0.047(2) Uani 1 1 d . . . H91 H 0.4377 0.5138 0.9268 0.056 Uiso 1 1 calc R . . C92 C 0.4308(4) 0.5786(5) 0.8629(4) 0.052(2) Uani 1 1 d . . . H92 H 0.4064 0.6124 0.8828 0.062 Uiso 1 1 calc R . . C93 C 0.4444(4) 0.5903(4) 0.8079(4) 0.043(2) Uani 1 1 d . . . H93 H 0.4271 0.6298 0.7900 0.052 Uiso 1 1 calc R . . C94 C 0.4861(4) 0.5403(4) 0.7782(4) 0.048(2) Uani 1 1 d . . . C95 C 0.5012(5) 0.5543(5) 0.7191(3) 0.049(2) Uani 1 1 d . . . H95A H 0.5469 0.5748 0.7158 0.073 Uiso 1 1 calc R . . H95B H 0.4667 0.5858 0.7044 0.073 Uiso 1 1 calc R . . H95C H 0.4998 0.5115 0.6984 0.073 Uiso 1 1 calc R . . C96 C 0.5497(4) 0.4319(4) 0.7746(4) 0.0381(19) Uani 1 1 d . . . C97 C 0.6222(4) 0.4350(4) 0.7707(4) 0.039(2) Uani 1 1 d . . . C98 C 0.6582(4) 0.3863(4) 0.7397(4) 0.0393(19) Uani 1 1 d . . . H98 H 0.7069 0.3882 0.7380 0.047 Uiso 1 1 calc R . . C99 C 0.6232(5) 0.3355(5) 0.7117(4) 0.045(2) Uani 1 1 d . . . H99 H 0.6478 0.3046 0.6891 0.054 Uiso 1 1 calc R . . C100 C 0.5527(4) 0.3298(5) 0.7168(4) 0.044(2) Uani 1 1 d . . . H100 H 0.5290 0.2936 0.6990 0.053 Uiso 1 1 calc R . . C101 C 0.5162(4) 0.3768(4) 0.7479(3) 0.0357(18) Uani 1 1 d . . . C102 C 0.4378(5) 0.3714(5) 0.7522(4) 0.053(3) Uani 1 1 d . . . H10A H 0.4247 0.3666 0.7908 0.080 Uiso 1 1 calc R . . H10B H 0.4219 0.3315 0.7316 0.080 Uiso 1 1 calc R . . H10C H 0.4167 0.4127 0.7370 0.080 Uiso 1 1 calc R . . C103 C 0.5006(7) 0.3980(6) 0.9388(4) 0.077(4) Uani 1 1 d . . . H10D H 0.5106 0.4392 0.9600 0.115 Uiso 1 1 calc R . . H10E H 0.5300 0.3606 0.9516 0.115 Uiso 1 1 calc R . . H10F H 0.4522 0.3854 0.9438 0.115 Uiso 1 1 calc R . . C104 C 0.6607(4) 0.4869(4) 0.8520(3) 0.0319(18) Uani 1 1 d . . . H104 H 0.6340 0.4542 0.8713 0.038 Uiso 1 1 calc R . . C105 C 0.6986(4) 0.5366(5) 0.8820(3) 0.042(2) Uani 1 1 d . . . C106 C 0.7088(5) 0.5483(4) 0.9385(3) 0.046(2) Uani 1 1 d . . . H106 H 0.6904 0.5216 0.9675 0.056 Uiso 1 1 calc R . . C107 C 0.7504(4) 0.6054(4) 0.9445(4) 0.045(2) Uani 1 1 d . . . H107 H 0.7669 0.6248 0.9777 0.054 Uiso 1 1 calc R . . C108 C 0.7624(4) 0.6279(4) 0.8912(3) 0.040(2) Uani 1 1 d . . . H108 H 0.7880 0.6677 0.8823 0.048 Uiso 1 1 calc R . . C109 C 0.9204(5) 0.6766(4) 0.6751(4) 0.050(2) Uani 1 1 d . . . C110 C 0.9885(5) 0.6694(4) 0.6934(4) 0.048(2) Uani 1 1 d . . . C111 C 1.0324(6) 0.6227(5) 0.6705(4) 0.056(3) Uani 1 1 d . . . H111 H 1.0779 0.6172 0.6842 0.067 Uiso 1 1 calc R . . C112 C 1.0075(6) 0.5816(4) 0.6247(5) 0.063(3) Uani 1 1 d . . . H112 H 1.0368 0.5492 0.6077 0.075 Uiso 1 1 calc R . . C113 C 0.9411(7) 0.5902(5) 0.6062(5) 0.067(3) Uani 1 1 d . . . H113 H 0.9245 0.5629 0.5768 0.080 Uiso 1 1 calc R . . C114 C 0.8981(5) 0.6388(4) 0.6302(4) 0.049(2) Uani 1 1 d . . . C115 C 0.8237(6) 0.6476(6) 0.6078(4) 0.073(3) Uani 1 1 d . . . H11A H 0.8161 0.6158 0.5774 0.110 Uiso 1 1 calc R . . H11B H 0.8174 0.6945 0.5947 0.110 Uiso 1 1 calc R . . H11C H 0.7907 0.6382 0.6371 0.110 Uiso 1 1 calc R . . C116 C 0.8727(5) 0.7251(4) 0.7044(4) 0.049(2) Uani 1 1 d . . . C117 C 0.8279(5) 0.7015(4) 0.7473(4) 0.044(2) Uani 1 1 d . . . C118 C 0.7821(5) 0.7484(5) 0.7696(4) 0.050(2) Uani 1 1 d . . . H118 H 0.7470 0.7328 0.7935 0.060 Uiso 1 1 calc R . . C119 C 0.7867(5) 0.8171(5) 0.7577(4) 0.056(3) Uani 1 1 d . . . H119 H 0.7579 0.8484 0.7765 0.067 Uiso 1 1 calc R . . C120 C 0.8324(6) 0.8411(5) 0.7188(4) 0.063(3) Uani 1 1 d . . . H120 H 0.8349 0.8885 0.7107 0.076 Uiso 1 1 calc R . . C121 C 0.8737(6) 0.7958(5) 0.6924(4) 0.063(3) Uani 1 1 d . . . C122 C 0.9251(7) 0.8216(5) 0.6516(5) 0.097(5) Uani 1 1 d . . . H12A H 0.9282 0.8714 0.6543 0.145 Uiso 1 1 calc R . . H12B H 0.9105 0.8089 0.6146 0.145 Uiso 1 1 calc R . . H12C H 0.9702 0.8015 0.6594 0.145 Uiso 1 1 calc R . . C123 C 1.0730(6) 0.7040(7) 0.7602(6) 0.090(4) Uani 1 1 d . . . H12D H 1.0813 0.6569 0.7720 0.135 Uiso 1 1 calc R . . H12E H 1.0783 0.7348 0.7915 0.135 Uiso 1 1 calc R . . H12F H 1.1061 0.7163 0.7317 0.135 Uiso 1 1 calc R . . C124 C 0.8792(4) 0.6030(4) 0.7788(3) 0.0335(18) Uani 1 1 d . . . H124 H 0.9204 0.6288 0.7815 0.040 Uiso 1 1 calc R . . C125 C 0.8792(4) 0.5316(4) 0.7937(3) 0.0344(19) Uani 1 1 d . . . C126 C 0.9319(4) 0.4900(5) 0.8141(3) 0.0385(19) Uani 1 1 d . . . H126 H 0.9780 0.5029 0.8217 0.046 Uiso 1 1 calc R . . C127 C 0.9031(5) 0.4269(4) 0.8206(4) 0.042(2) Uani 1 1 d . . . H127 H 0.9255 0.3864 0.8324 0.050 Uiso 1 1 calc R . . C128 C 0.8315(4) 0.4346(5) 0.8060(3) 0.041(2) Uani 1 1 d . . . H128 H 0.7984 0.3990 0.8078 0.049 Uiso 1 1 calc R . . C129 C 0.7915(5) 0.4870(4) 0.6662(4) 0.043(2) Uani 1 1 d . . . H12G H 0.7808 0.4383 0.6691 0.065 Uiso 1 1 calc R . . H12H H 0.8342 0.4967 0.6861 0.065 Uiso 1 1 calc R . . H12I H 0.7972 0.4993 0.6275 0.065 Uiso 1 1 calc R . . C130 C 0.6760(5) 0.5249(5) 0.6516(4) 0.054(3) Uani 1 1 d . . . H13A H 0.6895 0.5450 0.6164 0.081 Uiso 1 1 calc R . . H13B H 0.6374 0.5506 0.6669 0.081 Uiso 1 1 calc R . . H13C H 0.6622 0.4773 0.6458 0.081 Uiso 1 1 calc R . . C131 C 0.6588(5) 0.6761(5) 0.7008(4) 0.058(3) Uani 1 1 d . . . H13D H 0.6124 0.6712 0.6854 0.086 Uiso 1 1 calc R . . H13E H 0.6927 0.6607 0.6739 0.086 Uiso 1 1 calc R . . H13F H 0.6672 0.7241 0.7097 0.086 Uiso 1 1 calc R . . C132 C 0.6155(5) 0.6617(4) 0.7914(4) 0.047(2) Uani 1 1 d . . . H13G H 0.6305 0.7070 0.8035 0.071 Uiso 1 1 calc R . . H13H H 0.6140 0.6307 0.8229 0.071 Uiso 1 1 calc R . . H13I H 0.5696 0.6650 0.7749 0.071 Uiso 1 1 calc R . . C133 C 1.0031(4) 0.3313(4) 0.5660(4) 0.039(2) Uani 1 1 d . . . C134 C 1.0187(5) 0.3478(5) 0.6217(4) 0.048(2) Uani 1 1 d . . . C135 C 1.0579(5) 0.3017(6) 0.6531(4) 0.057(3) Uani 1 1 d . . . H135 H 1.0678 0.3115 0.6904 0.068 Uiso 1 1 calc R . . C136 C 1.0819(5) 0.2425(6) 0.6300(5) 0.067(3) Uani 1 1 d . . . H136 H 1.1066 0.2110 0.6521 0.081 Uiso 1 1 calc R . . C137 C 1.0709(5) 0.2277(5) 0.5751(5) 0.057(3) Uani 1 1 d . . . H137 H 1.0908 0.1877 0.5599 0.068 Uiso 1 1 calc R . . C138 C 1.0306(4) 0.2710(4) 0.5411(4) 0.0376(19) Uani 1 1 d . . . C139 C 1.0186(5) 0.2568(6) 0.4816(4) 0.059(3) Uani 1 1 d . . . H13J H 0.9700 0.2461 0.4756 0.088 Uiso 1 1 calc R . . H13K H 1.0469 0.2179 0.4702 0.088 Uiso 1 1 calc R . . H13L H 1.0311 0.2970 0.4600 0.088 Uiso 1 1 calc R . . C140 C 0.9613(5) 0.3830(4) 0.5332(4) 0.038(2) Uani 1 1 d . . . C141 C 0.8880(4) 0.3803(4) 0.5276(3) 0.0327(18) Uani 1 1 d . . . C142 C 0.8538(5) 0.4233(4) 0.4937(4) 0.039(2) Uani 1 1 d . . . H142 H 0.8056 0.4182 0.4887 0.047 Uiso 1 1 calc R . . C143 C 0.8889(5) 0.4751(4) 0.4661(4) 0.044(2) Uani 1 1 d . . . H143 H 0.8642 0.5076 0.4450 0.053 Uiso 1 1 calc R . . C144 C 0.9590(5) 0.4787(4) 0.4698(4) 0.042(2) Uani 1 1 d . . . H144 H 0.9829 0.5121 0.4491 0.050 Uiso 1 1 calc R . . C145 C 0.9964(4) 0.4336(4) 0.5038(4) 0.039(2) Uani 1 1 d . . . C146 C 1.0754(5) 0.4404(5) 0.5071(4) 0.051(2) Uani 1 1 d . . . H14D H 1.0899 0.4412 0.5456 0.076 Uiso 1 1 calc R . . H14E H 1.0898 0.4827 0.4891 0.076 Uiso 1 1 calc R . . H14F H 1.0968 0.4014 0.4886 0.076 Uiso 1 1 calc R . . C147 C 0.9935(6) 0.4191(7) 0.6995(4) 0.070(4) Uani 1 1 d . . . H14G H 0.9712 0.3809 0.7183 0.105 Uiso 1 1 calc R . . H14H H 0.9685 0.4613 0.7074 0.105 Uiso 1 1 calc R . . H14I H 1.0410 0.4234 0.7124 0.105 Uiso 1 1 calc R . . C148 C 0.8503(4) 0.3295(4) 0.6116(3) 0.0348(18) Uani 1 1 d . . . H148 H 0.8752 0.3647 0.6296 0.042 Uiso 1 1 calc R . . C149 C 0.8139(4) 0.2800(4) 0.6420(3) 0.0302(17) Uani 1 1 d . . . C150 C 0.8060(4) 0.2716(4) 0.6994(3) 0.0373(19) Uani 1 1 d . . . H150 H 0.8233 0.2995 0.7281 0.045 Uiso 1 1 calc R . . C151 C 0.7658(4) 0.2109(4) 0.7035(4) 0.044(2) Uani 1 1 d . . . H151 H 0.7530 0.1885 0.7364 0.053 Uiso 1 1 calc R . . C152 C 0.7484(4) 0.1903(4) 0.6500(4) 0.044(2) Uani 1 1 d . . . H152 H 0.7189 0.1531 0.6419 0.052 Uiso 1 1 calc R . . C153 C 0.6042(4) 0.1311(4) 0.4249(3) 0.0350(18) Uani 1 1 d . . . C154 C 0.5334(4) 0.1379(4) 0.4397(4) 0.041(2) Uani 1 1 d . . . C155 C 0.4899(4) 0.1834(4) 0.4086(4) 0.042(2) Uani 1 1 d . . . H155 H 0.4426 0.1880 0.4175 0.051 Uiso 1 1 calc R . . C156 C 0.5165(6) 0.2187(5) 0.3673(4) 0.056(3) Uani 1 1 d . . . H156 H 0.4878 0.2497 0.3480 0.067 Uiso 1 1 calc R . . C157 C 0.5847(5) 0.2120(4) 0.3513(4) 0.048(2) Uani 1 1 d . . . H157 H 0.6013 0.2379 0.3212 0.058 Uiso 1 1 calc R . . C158 C 0.6288(4) 0.1679(4) 0.3788(4) 0.0404(19) Uani 1 1 d . . . C159 C 0.7021(5) 0.1574(4) 0.3619(3) 0.052(3) Uani 1 1 d . . . H15D H 0.7315 0.1905 0.3808 0.078 Uiso 1 1 calc R . . H15E H 0.7061 0.1638 0.3222 0.078 Uiso 1 1 calc R . . H15F H 0.7166 0.1111 0.3716 0.078 Uiso 1 1 calc R . . C160 C 0.6478(4) 0.0833(4) 0.4582(3) 0.0339(18) Uani 1 1 d . . . C161 C 0.6919(4) 0.1071(4) 0.5000(4) 0.0367(19) Uani 1 1 d . . . C162 C 0.7351(4) 0.0625(4) 0.5315(3) 0.0373(18) Uani 1 1 d . . . H162 H 0.7630 0.0792 0.5605 0.045 Uiso 1 1 calc R . . C163 C 0.7344(4) -0.0065(4) 0.5175(4) 0.039(2) Uani 1 1 d . . . H163 H 0.7638 -0.0370 0.5366 0.047 Uiso 1 1 calc R . . C164 C 0.6923(5) -0.0314(4) 0.4772(4) 0.049(2) Uani 1 1 d . . . H164 H 0.6925 -0.0789 0.4694 0.058 Uiso 1 1 calc R . . C165 C 0.6486(4) 0.0123(4) 0.4467(4) 0.043(2) Uani 1 1 d . . . C166 C 0.6014(5) -0.0169(5) 0.4017(4) 0.053(2) Uani 1 1 d . . . H16A H 0.5535 -0.0051 0.4098 0.080 Uiso 1 1 calc R . . H16B H 0.6062 -0.0667 0.4005 0.080 Uiso 1 1 calc R . . H16C H 0.6143 0.0024 0.3661 0.080 Uiso 1 1 calc R . . C167 C 0.4426(5) 0.1005(6) 0.4983(5) 0.068(3) Uani 1 1 d . . . H16D H 0.4282 0.1476 0.5053 0.103 Uiso 1 1 calc R . . H16E H 0.4359 0.0731 0.5314 0.103 Uiso 1 1 calc R . . H16F H 0.4150 0.0814 0.4683 0.103 Uiso 1 1 calc R . . C168 C 0.6335(4) 0.2088(4) 0.5311(3) 0.0321(17) Uani 1 1 d . . . H168 H 0.5922 0.1828 0.5311 0.039 Uiso 1 1 calc R . . C169 C 0.6312(4) 0.2765(4) 0.5463(4) 0.039(2) Uani 1 1 d . . . C170 C 0.5776(5) 0.3202(4) 0.5627(4) 0.044(2) Uani 1 1 d . . . H170 H 0.5305 0.3085 0.5670 0.052 Uiso 1 1 calc R . . C171 C 0.6075(5) 0.3847(5) 0.5715(4) 0.042(2) Uani 1 1 d . . . H171 H 0.5841 0.4247 0.5831 0.051 Uiso 1 1 calc R . . C172 C 0.6779(5) 0.3795(4) 0.5601(3) 0.042(2) Uani 1 1 d . . . H172 H 0.7101 0.4157 0.5629 0.050 Uiso 1 1 calc R . . C173 C 0.8396(4) 0.2866(4) 0.4117(3) 0.0397(19) Uani 1 1 d . . . H17A H 0.8275 0.2661 0.3764 0.059 Uiso 1 1 calc R . . H17B H 0.8787 0.2620 0.4277 0.059 Uiso 1 1 calc R . . H17C H 0.8522 0.3346 0.4063 0.059 Uiso 1 1 calc R . . C174 C 0.7223(4) 0.3200(4) 0.4229(3) 0.040(2) Uani 1 1 d . . . H17D H 0.7310 0.3692 0.4251 0.060 Uiso 1 1 calc R . . H17E H 0.6794 0.3092 0.4419 0.060 Uiso 1 1 calc R . . H17F H 0.7186 0.3064 0.3844 0.060 Uiso 1 1 calc R . . C175 C 0.8601(5) 0.1380(4) 0.4641(4) 0.051(2) Uani 1 1 d . . . H17G H 0.9067 0.1445 0.4498 0.076 Uiso 1 1 calc R . . H17H H 0.8266 0.1527 0.4365 0.076 Uiso 1 1 calc R . . H17I H 0.8530 0.0896 0.4725 0.076 Uiso 1 1 calc R . . C176 C 0.8953(4) 0.1523(5) 0.5585(4) 0.044(2) Uani 1 1 d . . . H17J H 0.8773 0.1082 0.5709 0.066 Uiso 1 1 calc R . . H17K H 0.8960 0.1844 0.5893 0.066 Uiso 1 1 calc R . . H17L H 0.9421 0.1462 0.5446 0.066 Uiso 1 1 calc R . . C177 C 0.7859(2) -0.01423(18) 0.85006(16) 0.100(5) Uani 1 1 d G . . H177 H 0.7813 -0.0285 0.8871 0.120 Uiso 1 1 calc R . . C178 C 0.7282(2) -0.00987(17) 0.81653(15) 0.116(6) Uani 1 1 d G . . H178 H 0.6842 -0.0211 0.8306 0.139 Uiso 1 1 calc R . . C179 C 0.7350(2) 0.01097(17) 0.76238(15) 0.124(7) Uani 1 1 d G . . H179 H 0.6956 0.0140 0.7395 0.149 Uiso 1 1 calc R . . C180 C 0.7995(2) 0.02746(17) 0.74175(15) 0.100(4) Uani 1 1 d G . . H180 H 0.8041 0.0417 0.7047 0.120 Uiso 1 1 calc R . . C181 C 0.8571(2) 0.02310(18) 0.77528(16) 0.064(3) Uani 1 1 d G . . H181 H 0.9012 0.0344 0.7612 0.076 Uiso 1 1 calc R . . C182 C 0.8504(2) 0.00226(18) 0.82944(16) 0.084(4) Uani 1 1 d G . . H182 H 0.8898 -0.0007 0.8524 0.101 Uiso 1 1 calc R . . C183 C 0.14397(18) 0.5166(2) 0.76172(15) 0.096(4) Uani 1 1 d G . . H183 H 0.0955 0.5193 0.7657 0.115 Uiso 1 1 calc R . . C184 C 0.18649(19) 0.5261(2) 0.80692(15) 0.101(4) Uani 1 1 d GU . . H184 H 0.1671 0.5354 0.8418 0.121 Uiso 1 1 calc R . . C185 C 0.25742(19) 0.52205(19) 0.80106(14) 0.116(5) Uani 1 1 d GU . . H185 H 0.2865 0.5286 0.8319 0.139 Uiso 1 1 calc R . . C186 C 0.28584(17) 0.50848(18) 0.75000(14) 0.097(4) Uani 1 1 d GU . . H186 H 0.3343 0.5057 0.7460 0.117 Uiso 1 1 calc R . . C187 C 0.24332(17) 0.49895(18) 0.70481(14) 0.092(4) Uani 1 1 d GU . . H187 H 0.2627 0.4897 0.6699 0.111 Uiso 1 1 calc R . . C188 C 0.17238(17) 0.50300(19) 0.71067(15) 0.097(4) Uani 1 1 d GU . . H188 H 0.1433 0.4965 0.6798 0.117 Uiso 1 1 calc R . . C189 C 0.77453(19) 0.79899(17) 0.51085(17) 0.085(4) Uani 1 1 d GU . . H189 H 0.8228 0.8041 0.5150 0.102 Uiso 1 1 calc R . . C190 C 0.74698(18) 0.78251(17) 0.45995(17) 0.154(7) Uani 1 1 d GU . . H190 H 0.7764 0.7764 0.4294 0.185 Uiso 1 1 calc R . . C191 C 0.67632(18) 0.77504(16) 0.45383(16) 0.117(5) Uani 1 1 d GU . . H191 H 0.6575 0.7638 0.4190 0.140 Uiso 1 1 calc R . . C192 C 0.63323(18) 0.78405(15) 0.49860(16) 0.086(3) Uani 1 1 d GU . . H192 H 0.5849 0.7789 0.4944 0.103 Uiso 1 1 calc R . . C193 C 0.66079(19) 0.80052(16) 0.54950(16) 0.108(4) Uani 1 1 d GU . . H193 H 0.6313 0.8067 0.5801 0.129 Uiso 1 1 calc R . . C194 C 0.73144(19) 0.80799(16) 0.55563(17) 0.168(7) Uani 1 1 d GU . . H194 H 0.7503 0.8193 0.5904 0.202 Uiso 1 1 calc R . . C195 C 0.3664(3) 0.2926(2) 0.01995(13) 0.057(2) Uani 1 1 d GU . . H195 H 0.4113 0.2857 0.0057 0.068 Uiso 1 1 calc R . . C196 C 0.3101(3) 0.2936(2) -0.01517(13) 0.097(4) Uani 1 1 d GU . . H196 H 0.3165 0.2874 -0.0534 0.116 Uiso 1 1 calc R . . C197 C 0.2445(3) 0.3037(2) 0.00569(14) 0.103(4) Uani 1 1 d GU . . H197 H 0.2060 0.3044 -0.0183 0.123 Uiso 1 1 calc R . . C198 C 0.2351(2) 0.3128(2) 0.06166(14) 0.102(4) Uani 1 1 d GU . . H198 H 0.1903 0.3197 0.0759 0.122 Uiso 1 1 calc R . . C199 C 0.2915(2) 0.31175(19) 0.09678(14) 0.110(4) Uani 1 1 d GU . . H199 H 0.2851 0.3180 0.1350 0.133 Uiso 1 1 calc R . . C200 C 0.3571(2) 0.3017(2) 0.07593(13) 0.095(4) Uani 1 1 d GU . . H200 H 0.3956 0.3010 0.0999 0.114 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0350(8) 0.0253(7) 0.0291(7) -0.0023(6) 0.0014(6) -0.0004(6) Ti2 0.0471(7) 0.0246(7) 0.0295(7) 0.0008(6) -0.0031(6) 0.0010(6) Ti3 0.0476(8) 0.0253(7) 0.0299(8) -0.0024(6) -0.0052(6) 0.0035(6) Ti4 0.0422(8) 0.0234(7) 0.0277(7) 0.0017(6) 0.0016(6) 0.0008(6) N1 0.035(3) 0.038(4) 0.028(4) -0.002(3) 0.002(3) -0.003(3) N2 0.040(3) 0.037(4) 0.026(3) -0.002(3) 0.005(3) 0.003(3) N3 0.036(3) 0.028(3) 0.030(4) -0.001(3) 0.001(3) 0.001(3) N4 0.054(4) 0.028(4) 0.039(4) 0.002(3) -0.001(3) 0.002(3) N5 0.042(4) 0.045(4) 0.035(4) -0.006(3) -0.008(3) -0.002(3) N6 0.039(3) 0.028(3) 0.034(4) -0.006(3) 0.004(3) -0.004(3) N7 0.051(4) 0.030(3) 0.029(4) -0.001(3) 0.002(3) -0.004(3) N8 0.040(4) 0.039(4) 0.027(4) -0.010(3) 0.004(3) 0.010(3) N9 0.034(3) 0.021(3) 0.033(4) -0.001(3) 0.001(3) 0.004(2) N10 0.041(3) 0.032(3) 0.028(3) -0.008(3) -0.003(3) -0.002(3) N11 0.072(5) 0.018(3) 0.027(4) 0.007(3) -0.001(3) 0.001(3) N12 0.053(4) 0.025(3) 0.051(5) 0.004(3) -0.008(4) 0.008(3) N13 0.024(3) 0.048(4) 0.037(4) -0.016(3) -0.007(3) 0.010(3) N14 0.045(4) 0.038(4) 0.036(4) -0.003(3) -0.012(3) 0.004(3) N15 0.048(4) 0.038(4) 0.034(4) -0.004(3) -0.003(3) -0.004(3) N16 0.050(4) 0.034(4) 0.032(4) 0.006(3) 0.005(3) 0.000(3) N17 0.048(4) 0.013(3) 0.035(4) 0.000(3) 0.002(3) 0.002(3) N18 0.059(4) 0.025(3) 0.038(4) -0.002(3) 0.000(3) 0.004(3) N19 0.042(3) 0.018(3) 0.033(4) 0.003(3) 0.004(3) 0.007(3) N20 0.050(4) 0.029(3) 0.028(3) 0.013(3) 0.001(3) 0.002(3) N21 0.046(4) 0.011(3) 0.033(4) 0.003(2) 0.002(3) 0.002(2) N22 0.046(4) 0.022(3) 0.031(4) 0.003(3) -0.010(3) -0.009(3) N23 0.045(4) 0.049(4) 0.031(4) 0.002(3) -0.006(3) -0.009(3) N24 0.048(4) 0.035(4) 0.026(3) -0.007(3) 0.010(3) 0.012(3) O1 0.045(3) 0.068(4) 0.043(4) 0.015(3) 0.005(3) 0.013(3) O2 0.038(3) 0.046(3) 0.063(4) -0.002(3) -0.003(3) -0.004(3) O3 0.054(4) 0.051(4) 0.056(4) 0.012(3) 0.011(3) 0.005(3) O4 0.058(4) 0.060(4) 0.029(3) -0.003(3) 0.001(3) 0.016(3) O5 0.058(4) 0.051(4) 0.023(3) 0.006(3) 0.006(3) 0.006(3) O6 0.060(4) 0.051(4) 0.071(5) -0.020(3) 0.004(4) -0.014(3) O7 0.063(4) 0.066(4) 0.031(3) -0.008(3) 0.000(3) -0.004(3) O8 0.046(3) 0.047(3) 0.041(3) 0.012(3) 0.005(3) -0.001(3) C1 0.032(4) 0.035(4) 0.037(5) -0.011(3) -0.002(3) -0.002(3) C2 0.052(5) 0.057(6) 0.025(4) -0.005(4) 0.009(4) 0.004(4) C3 0.048(5) 0.077(7) 0.041(5) -0.020(5) 0.005(4) 0.013(5) C4 0.028(4) 0.074(7) 0.071(7) -0.029(6) -0.016(4) 0.005(4) C5 0.041(5) 0.049(5) 0.074(7) -0.019(5) 0.011(5) 0.005(4) C6 0.043(4) 0.036(4) 0.037(5) -0.003(4) 0.017(4) 0.003(3) C7 0.049(5) 0.041(5) 0.043(5) -0.006(4) -0.003(4) -0.011(4) C8 0.054(5) 0.018(4) 0.019(4) 0.000(3) 0.003(3) -0.003(3) C9 0.034(4) 0.022(4) 0.040(5) 0.001(3) 0.006(3) 0.001(3) C10 0.053(5) 0.021(4) 0.040(5) -0.002(3) 0.010(4) -0.004(3) C11 0.045(4) 0.020(4) 0.056(6) -0.007(4) -0.007(4) -0.002(3) C12 0.063(5) 0.019(4) 0.041(5) -0.001(3) -0.007(4) 0.007(3) C13 0.035(4) 0.026(4) 0.059(6) 0.002(4) 0.001(4) 0.001(3) C14 0.039(4) 0.047(5) 0.048(6) -0.011(4) -0.001(4) 0.014(4) C15 0.065(6) 0.133(11) 0.025(5) 0.006(6) 0.010(5) 0.024(7) C16 0.032(4) 0.029(4) 0.036(5) 0.005(3) -0.004(3) -0.003(3) C17 0.019(3) 0.040(4) 0.041(5) 0.003(4) 0.000(3) 0.000(3) C18 0.040(4) 0.043(4) 0.028(4) 0.003(3) 0.005(3) -0.007(3) C19 0.050(5) 0.052(5) 0.043(5) -0.022(4) 0.007(4) -0.003(4) C20 0.045(4) 0.033(4) 0.045(5) -0.005(4) 0.002(4) -0.006(4) C21 0.059(5) 0.036(4) 0.019(4) 0.006(3) -0.005(4) 0.005(4) C22 0.067(6) 0.037(5) 0.029(5) -0.011(4) -0.017(4) 0.001(4) C23 0.055(5) 0.044(5) 0.056(6) 0.008(4) -0.003(5) -0.007(4) C24 0.075(6) 0.046(5) 0.033(5) -0.001(4) -0.017(4) 0.004(4) C25 0.099(8) 0.043(5) 0.023(5) -0.005(4) -0.014(5) 0.013(5) C26 0.070(6) 0.031(4) 0.033(5) 0.001(4) -0.006(4) 0.011(4) C27 0.069(6) 0.039(5) 0.036(5) 0.006(4) 0.001(4) 0.012(4) C28 0.042(4) 0.020(4) 0.042(5) -0.010(3) 0.020(4) 0.001(3) C29 0.044(4) 0.023(4) 0.044(5) -0.012(3) 0.011(4) 0.003(3) C30 0.031(4) 0.028(4) 0.047(5) -0.001(4) 0.001(3) -0.007(3) C31 0.055(5) 0.028(4) 0.053(6) -0.002(4) 0.007(4) 0.008(4) C32 0.055(5) 0.023(4) 0.055(6) 0.001(4) 0.009(4) 0.004(3) C33 0.044(4) 0.028(4) 0.035(4) 0.005(3) 0.006(3) 0.012(3) C34 0.076(7) 0.051(5) 0.055(6) -0.001(5) -0.016(5) 0.015(5) C35 0.032(5) 0.098(9) 0.075(8) -0.005(6) 0.002(5) -0.009(5) C36 0.028(4) 0.039(5) 0.037(5) -0.002(4) 0.007(3) 0.002(3) C37 0.042(4) 0.042(5) 0.040(5) -0.002(4) 0.006(4) 0.003(4) C38 0.031(4) 0.041(4) 0.030(4) 0.017(4) -0.003(3) -0.013(3) C39 0.052(5) 0.036(4) 0.036(5) 0.007(4) 0.002(4) -0.005(4) C40 0.051(5) 0.014(3) 0.041(5) 0.003(3) -0.008(4) -0.003(3) C41 0.058(5) 0.032(4) 0.038(5) 0.003(4) 0.017(4) -0.008(4) C42 0.055(5) 0.038(5) 0.037(5) 0.002(4) -0.009(4) -0.002(4) C43 0.044(4) 0.024(4) 0.052(5) -0.005(3) 0.019(4) -0.003(3) C44 0.052(5) 0.029(4) 0.062(6) -0.014(4) 0.009(4) -0.002(4) C45 0.076(6) 0.024(4) 0.041(5) -0.007(4) 0.005(4) 0.006(4) C46 0.071(6) 0.024(4) 0.043(5) 0.005(4) 0.000(5) 0.013(4) C47 0.073(6) 0.037(5) 0.059(6) 0.009(4) 0.020(5) -0.011(5) C48 0.091(8) 0.032(5) 0.042(6) 0.009(4) 0.009(5) 0.007(5) C49 0.101(8) 0.038(5) 0.032(5) 0.008(4) 0.023(5) 0.012(5) C50 0.067(6) 0.031(4) 0.034(5) -0.008(3) 0.004(4) -0.001(4) C51 0.064(6) 0.052(5) 0.056(6) 0.001(4) -0.010(5) 0.007(5) C52 0.057(5) 0.031(4) 0.032(4) -0.004(3) 0.003(4) 0.010(4) C53 0.043(4) 0.029(4) 0.021(4) 0.004(3) -0.006(3) 0.008(3) C54 0.059(5) 0.022(4) 0.041(5) 0.001(3) -0.008(4) 0.006(4) C55 0.056(5) 0.030(4) 0.042(5) -0.001(4) 0.015(4) 0.002(4) C56 0.073(6) 0.011(3) 0.063(6) -0.005(4) 0.002(5) 0.009(4) C57 0.054(5) 0.029(4) 0.046(5) 0.008(4) 0.007(4) 0.011(4) C58 0.063(6) 0.045(5) 0.061(6) -0.016(4) 0.029(5) 0.014(4) C59 0.071(7) 0.071(7) 0.086(9) 0.034(6) 0.003(6) 0.005(6) C60 0.054(5) 0.029(4) 0.016(4) 0.007(3) 0.004(3) 0.005(4) C61 0.057(5) 0.026(4) 0.022(4) -0.013(3) 0.006(4) -0.015(4) C62 0.039(4) 0.051(5) 0.035(5) 0.001(4) 0.011(4) -0.004(4) C63 0.066(6) 0.036(5) 0.049(6) -0.018(4) 0.016(5) -0.024(4) C64 0.054(5) 0.032(4) 0.032(5) 0.000(3) 0.000(4) -0.009(4) C65 0.052(5) 0.023(4) 0.034(5) 0.003(3) -0.002(4) 0.006(3) C66 0.047(5) 0.051(6) 0.048(6) 0.003(5) 0.004(4) 0.016(4) C67 0.039(5) 0.089(8) 0.050(6) 0.035(6) 0.011(4) 0.012(5) C68 0.046(5) 0.063(7) 0.110(10) 0.044(7) 0.008(6) -0.001(5) C69 0.063(6) 0.039(5) 0.064(7) 0.019(5) 0.004(5) -0.008(4) C70 0.055(5) 0.022(4) 0.064(6) 0.017(4) -0.005(4) 0.010(3) C71 0.084(6) 0.028(4) 0.054(6) -0.010(4) -0.012(5) 0.008(4) C72 0.038(4) 0.040(5) 0.027(4) -0.002(4) -0.005(3) 0.006(3) C73 0.060(5) 0.018(4) 0.032(5) 0.002(3) 0.001(4) 0.002(3) C74 0.050(5) 0.035(4) 0.031(4) -0.008(4) 0.011(4) -0.005(4) C75 0.070(6) 0.030(4) 0.025(4) 0.001(3) 0.003(4) -0.002(4) C76 0.061(5) 0.044(5) 0.032(5) 0.005(4) -0.007(4) 0.020(4) C77 0.059(5) 0.030(4) 0.014(4) -0.001(3) -0.001(3) 0.003(4) C78 0.062(6) 0.058(7) 0.071(8) 0.002(6) -0.003(6) -0.005(5) C79 0.089(8) 0.061(7) 0.062(7) -0.025(6) 0.004(6) 0.014(6) C80 0.039(4) 0.033(4) 0.042(5) -0.002(4) 0.005(4) -0.005(3) C81 0.046(4) 0.025(4) 0.032(4) 0.002(3) -0.003(3) -0.003(3) C82 0.048(5) 0.049(5) 0.037(5) 0.001(4) 0.004(4) -0.001(4) C83 0.076(6) 0.039(5) 0.032(5) -0.002(4) -0.009(4) -0.002(4) C84 0.038(4) 0.042(4) 0.027(4) -0.002(3) -0.006(3) 0.005(3) C85 0.091(7) 0.050(6) 0.035(5) 0.001(4) -0.004(5) 0.023(5) C86 0.059(6) 0.059(6) 0.034(5) 0.003(4) 0.002(4) 0.005(5) C87 0.044(5) 0.041(5) 0.069(6) 0.014(4) 0.000(4) -0.013(4) C88 0.068(6) 0.050(5) 0.040(5) -0.003(4) -0.010(4) -0.014(5) C89 0.040(4) 0.044(5) 0.034(4) -0.005(4) -0.009(3) -0.008(3) C90 0.040(4) 0.035(4) 0.052(6) -0.010(4) 0.006(4) -0.008(3) C91 0.048(5) 0.041(5) 0.050(6) -0.017(4) 0.012(4) 0.002(4) C92 0.045(5) 0.054(6) 0.057(6) -0.020(5) 0.008(4) 0.002(4) C93 0.041(4) 0.038(5) 0.051(5) -0.016(4) -0.001(4) 0.008(3) C94 0.033(4) 0.037(5) 0.075(7) -0.020(4) 0.006(4) 0.008(3) C95 0.066(5) 0.040(5) 0.040(5) 0.011(4) -0.016(4) 0.004(4) C96 0.056(5) 0.023(4) 0.036(5) -0.002(3) 0.000(4) -0.009(3) C97 0.062(5) 0.020(4) 0.036(5) 0.009(3) 0.000(4) -0.010(3) C98 0.048(4) 0.034(4) 0.036(5) -0.001(4) -0.007(4) 0.011(4) C99 0.062(5) 0.046(5) 0.027(4) 0.009(4) 0.009(4) -0.005(4) C100 0.050(5) 0.041(5) 0.040(5) -0.013(4) -0.006(4) -0.001(4) C101 0.045(4) 0.039(4) 0.023(4) 0.005(3) 0.004(3) -0.006(4) C102 0.064(6) 0.032(5) 0.063(7) 0.003(4) -0.002(5) 0.000(4) C103 0.138(11) 0.051(6) 0.041(6) 0.001(5) 0.012(7) -0.006(7) C104 0.033(4) 0.021(4) 0.041(5) 0.011(3) -0.010(3) 0.011(3) C105 0.045(4) 0.048(5) 0.033(5) -0.006(4) -0.005(4) 0.007(4) C106 0.058(5) 0.050(5) 0.032(4) 0.012(4) 0.004(4) 0.002(4) C107 0.050(5) 0.052(5) 0.033(5) -0.017(4) -0.007(4) 0.011(4) C108 0.054(5) 0.030(4) 0.037(5) -0.016(3) -0.009(4) 0.003(3) C109 0.086(7) 0.006(3) 0.058(6) -0.001(3) 0.007(5) -0.013(4) C110 0.060(5) 0.030(4) 0.053(6) 0.002(4) 0.008(4) -0.013(4) C111 0.076(6) 0.036(5) 0.055(6) 0.004(4) 0.021(5) -0.008(4) C112 0.088(8) 0.022(4) 0.079(7) -0.003(4) 0.037(6) -0.012(4) C113 0.121(10) 0.033(5) 0.046(6) -0.008(4) 0.032(7) -0.007(6) C114 0.086(7) 0.030(4) 0.031(5) 0.003(4) 0.001(5) -0.014(4) C115 0.109(10) 0.067(7) 0.044(6) -0.009(5) -0.001(6) 0.002(6) C116 0.078(6) 0.035(5) 0.033(5) 0.004(4) -0.005(4) -0.010(4) C117 0.067(6) 0.020(4) 0.046(5) -0.004(4) -0.007(4) -0.002(4) C118 0.061(5) 0.033(4) 0.055(5) -0.019(4) -0.002(5) 0.005(4) C119 0.063(6) 0.034(5) 0.071(7) -0.024(5) -0.016(5) 0.012(4) C120 0.082(7) 0.042(5) 0.065(7) 0.001(5) -0.007(6) -0.002(5) C121 0.108(8) 0.044(5) 0.036(5) -0.011(4) 0.003(5) 0.006(6) C122 0.173(14) 0.019(5) 0.098(9) 0.002(5) 0.029(9) -0.006(6) C123 0.070(7) 0.094(9) 0.105(10) -0.036(8) -0.031(7) 0.007(7) C124 0.048(4) 0.020(3) 0.032(4) -0.004(3) 0.010(4) -0.007(3) C125 0.048(4) 0.041(5) 0.014(4) 0.004(3) 0.005(3) 0.012(3) C126 0.034(4) 0.052(5) 0.029(4) -0.003(4) -0.011(3) 0.006(4) C127 0.061(5) 0.032(4) 0.033(5) -0.001(4) 0.000(4) 0.008(4) C128 0.036(4) 0.056(6) 0.030(4) 0.005(4) -0.001(3) -0.004(4) C129 0.063(5) 0.027(4) 0.041(5) -0.014(4) 0.014(4) -0.001(4) C130 0.078(7) 0.053(6) 0.031(5) -0.015(4) -0.005(5) -0.007(5) C131 0.068(6) 0.052(6) 0.053(6) 0.020(5) -0.019(5) 0.009(5) C132 0.062(5) 0.035(4) 0.044(5) -0.004(4) -0.003(4) 0.006(4) C133 0.045(4) 0.032(4) 0.041(5) 0.007(4) -0.007(4) -0.001(3) C134 0.050(5) 0.050(5) 0.043(5) 0.009(4) 0.000(4) -0.013(4) C135 0.052(5) 0.068(7) 0.050(6) 0.009(5) 0.002(4) -0.010(5) C136 0.064(6) 0.067(7) 0.072(8) 0.035(6) -0.016(5) -0.018(5) C137 0.051(5) 0.044(5) 0.075(8) 0.009(5) 0.005(5) -0.002(4) C138 0.042(4) 0.023(4) 0.048(5) 0.001(3) 0.002(4) 0.003(3) C139 0.073(6) 0.049(6) 0.055(6) -0.001(5) -0.003(5) 0.015(5) C140 0.061(5) 0.025(4) 0.029(4) -0.015(3) -0.003(4) 0.004(4) C141 0.037(4) 0.030(4) 0.031(4) -0.003(3) 0.007(3) -0.001(3) C142 0.052(5) 0.020(4) 0.046(5) 0.000(3) 0.006(4) -0.003(3) C143 0.068(6) 0.029(4) 0.036(5) 0.005(4) 0.002(4) -0.002(4) C144 0.051(5) 0.018(4) 0.055(6) -0.007(4) 0.001(4) -0.002(3) C145 0.043(4) 0.024(4) 0.050(5) 0.004(4) 0.002(4) -0.001(3) C146 0.066(6) 0.026(4) 0.061(6) 0.006(4) 0.004(5) -0.006(4) C147 0.087(8) 0.105(9) 0.018(5) -0.016(5) -0.001(5) -0.039(7) C148 0.055(5) 0.026(4) 0.023(4) -0.002(3) 0.005(3) -0.007(3) C149 0.035(4) 0.026(4) 0.030(4) 0.003(3) -0.002(3) 0.011(3) C150 0.045(4) 0.043(5) 0.024(4) -0.002(3) 0.010(3) 0.006(4) C151 0.049(5) 0.043(5) 0.040(5) 0.011(4) 0.017(4) 0.006(4) C152 0.038(4) 0.032(4) 0.061(6) 0.008(4) 0.003(4) -0.004(3) C153 0.062(5) 0.029(4) 0.013(4) -0.002(3) -0.004(3) -0.006(4) C154 0.048(5) 0.039(5) 0.036(5) -0.002(4) -0.011(4) -0.005(4) C155 0.054(5) 0.026(4) 0.047(5) -0.007(4) -0.004(4) 0.001(3) C156 0.088(7) 0.028(4) 0.051(6) -0.001(4) -0.037(5) -0.006(5) C157 0.090(7) 0.021(4) 0.033(5) 0.006(3) -0.007(4) -0.024(4) C158 0.053(5) 0.024(4) 0.044(5) 0.001(3) -0.005(4) -0.008(3) C159 0.096(7) 0.034(4) 0.026(4) 0.003(3) 0.012(4) -0.018(4) C160 0.038(4) 0.031(4) 0.033(4) 0.012(3) 0.003(3) 0.000(3) C161 0.047(4) 0.023(4) 0.040(5) 0.003(3) 0.017(4) 0.007(3) C162 0.043(4) 0.036(4) 0.032(4) 0.014(4) 0.004(3) 0.007(3) C163 0.044(4) 0.017(3) 0.055(5) 0.003(3) 0.006(4) 0.004(3) C164 0.059(5) 0.022(4) 0.066(6) -0.002(4) 0.012(5) 0.001(4) C165 0.052(5) 0.024(4) 0.054(6) -0.010(4) -0.003(4) -0.002(3) C166 0.061(6) 0.036(5) 0.063(6) -0.014(4) -0.010(4) -0.004(4) C167 0.055(6) 0.069(7) 0.081(8) 0.007(6) 0.002(6) 0.003(5) C168 0.025(4) 0.039(4) 0.033(4) -0.001(3) 0.001(3) -0.001(3) C169 0.053(5) 0.025(4) 0.038(5) 0.006(3) -0.007(4) -0.003(3) C170 0.058(5) 0.033(4) 0.039(5) -0.021(4) 0.006(4) 0.000(4) C171 0.049(5) 0.036(5) 0.042(5) -0.015(4) 0.000(4) 0.008(4) C172 0.070(6) 0.024(4) 0.032(5) -0.006(3) 0.002(4) 0.004(4) C173 0.056(5) 0.037(4) 0.026(4) 0.002(3) 0.006(4) 0.001(4) C174 0.058(5) 0.036(4) 0.026(4) -0.005(3) 0.006(4) -0.007(4) C175 0.077(6) 0.015(4) 0.060(6) -0.003(4) 0.015(5) -0.006(4) C176 0.049(5) 0.041(5) 0.042(5) 0.003(4) 0.002(4) 0.006(4) C177 0.099(9) 0.062(7) 0.139(12) -0.025(7) 0.060(9) -0.007(6) C178 0.083(9) 0.051(7) 0.213(17) -0.038(9) -0.030(11) 0.005(6) C179 0.077(8) 0.026(5) 0.27(2) -0.006(9) -0.019(11) 0.014(5) C180 0.122(10) 0.037(5) 0.141(12) -0.005(6) -0.043(9) 0.014(6) C181 0.093(7) 0.038(5) 0.060(6) -0.006(5) -0.003(6) 0.002(5) C182 0.062(6) 0.056(6) 0.135(11) -0.013(7) 0.002(7) -0.024(5) C183 0.048(6) 0.053(6) 0.186(14) 0.015(8) -0.013(8) -0.002(5) C184 0.091(7) 0.061(6) 0.152(9) -0.039(6) -0.003(7) -0.007(5) C185 0.107(8) 0.077(7) 0.163(9) -0.019(7) -0.018(7) -0.011(6) C186 0.093(7) 0.060(6) 0.139(9) 0.001(6) 0.018(7) 0.000(5) C187 0.100(7) 0.043(5) 0.133(8) 0.030(5) 0.024(6) 0.008(5) C188 0.090(7) 0.078(6) 0.125(8) 0.030(6) 0.019(6) 0.026(6) C189 0.061(6) 0.066(6) 0.128(8) 0.019(6) 0.003(6) 0.011(5) C190 0.157(10) 0.115(9) 0.190(10) -0.029(8) -0.006(9) 0.027(8) C191 0.104(8) 0.076(7) 0.170(9) -0.033(7) 0.017(7) -0.017(6) C192 0.090(7) 0.072(6) 0.096(7) -0.006(6) 0.007(6) 0.008(5) C193 0.088(7) 0.081(7) 0.154(9) 0.048(7) -0.024(7) 0.002(6) C194 0.171(11) 0.128(9) 0.206(11) 0.053(8) -0.011(9) 0.008(8) C195 0.069(5) 0.031(4) 0.070(6) 0.008(4) 0.011(5) 0.000(4) C196 0.106(8) 0.079(6) 0.106(8) -0.025(6) 0.008(6) 0.004(6) C197 0.093(7) 0.078(7) 0.137(8) -0.019(7) -0.013(7) -0.009(6) C198 0.097(7) 0.069(6) 0.139(8) 0.014(6) 0.031(7) -0.017(6) C199 0.127(8) 0.090(7) 0.114(8) 0.036(6) 0.038(7) -0.002(7) C200 0.090(7) 0.087(7) 0.107(7) 0.028(6) 0.017(6) 0.005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N6 1.911(7) . ? Ti1 N5 1.939(7) . ? Ti1 N1 2.178(7) . ? Ti1 N2 2.192(7) . ? Ti1 N4 2.203(8) . ? Ti1 N3 2.247(6) . ? Ti2 N11 1.933(7) . ? Ti2 N12 1.961(7) . ? Ti2 N7 2.195(7) . ? Ti2 N10 2.204(7) . ? Ti2 N9 2.212(6) . ? Ti2 N8 2.214(7) . ? Ti3 N18 1.931(7) . ? Ti3 N17 1.950(7) . ? Ti3 N14 2.195(7) . ? Ti3 N15 2.204(7) . ? Ti3 N13 2.226(7) . ? Ti3 N16 2.215(7) . ? Ti4 N24 1.912(6) . ? Ti4 N23 1.921(7) . ? Ti4 N19 2.176(7) . ? Ti4 N20 2.190(7) . ? Ti4 N22 2.206(7) . ? Ti4 N21 2.219(6) . ? N1 C16 1.355(10) . ? N1 C9 1.476(10) . ? N2 C20 1.352(10) . ? N2 C17 1.422(10) . ? N3 C36 1.312(10) . ? N3 C29 1.420(10) . ? N4 C40 1.359(10) . ? N4 C37 1.404(11) . ? N5 C42 1.470(11) . ? N5 C41 1.459(11) . ? N6 C44 1.476(11) . ? N6 C43 1.506(10) . ? N7 C60 1.304(11) . ? N7 C53 1.461(10) . ? N8 C64 1.313(11) . ? N8 C61 1.396(11) . ? N9 C80 1.325(11) . ? N9 C73 1.415(10) . ? N10 C84 1.358(10) . ? N10 C81 1.386(10) . ? N11 C86 1.446(11) . ? N11 C85 1.503(12) . ? N12 C88 1.466(11) . ? N12 C87 1.477(11) . ? N13 C104 1.304(10) . ? N13 C97 1.427(10) . ? N14 C105 1.363(11) . ? N14 C108 1.387(10) . ? N15 C124 1.325(11) . ? N15 C117 1.402(11) . ? N16 C128 1.324(11) . ? N16 C125 1.374(11) . ? N17 C130 1.480(11) . ? N17 C129 1.478(10) . ? N18 C131 1.456(11) . ? N18 C132 1.483(11) . ? N19 C148 1.324(10) . ? N19 C141 1.505(10) . ? N20 C152 1.362(10) . ? N20 C149 1.409(10) . ? N21 C168 1.316(10) . ? N21 C161 1.473(10) . ? N22 C169 1.406(10) . ? N22 C172 1.399(10) . ? N23 C174 1.487(11) . ? N23 C173 1.480(10) . ? N24 C176 1.464(11) . ? N24 C175 1.490(10) . ? O1 C2 1.349(12) . ? O1 C15 1.422(11) . ? O2 C22 1.362(11) . ? O2 C35 1.471(10) . ? O3 C46 1.399(11) . ? O3 C59 1.465(12) . ? O4 C66 1.391(13) . ? O4 C79 1.443(12) . ? O5 C90 1.370(11) . ? O5 C103 1.432(11) . ? O6 C110 1.396(12) . ? O6 C123 1.428(12) . ? O7 C134 1.353(12) . ? O7 C147 1.434(11) . ? O8 C154 1.353(11) . ? O8 C167 1.445(11) . ? C1 C6 1.436(12) . ? C1 C2 1.442(12) . ? C1 C8 1.525(11) . ? C2 C3 1.405(14) . ? C3 C4 1.380(16) . ? C3 H3 0.9500 . ? C4 C5 1.403(15) . ? C4 H4 0.9500 . ? C5 C6 1.400(13) . ? C5 H5 0.9500 . ? C6 C7 1.516(12) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.389(11) . ? C8 C13 1.404(11) . ? C9 C10 1.408(12) . ? C10 C11 1.370(11) . ? C10 H10 0.9500 . ? C11 C12 1.414(12) . ? C11 H11 0.9500 . ? C12 C13 1.417(12) . ? C12 H12 0.9500 . ? C13 C14 1.579(11) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.439(11) . ? C16 H16 0.9500 . ? C17 C18 1.402(11) . ? C18 C19 1.415(12) . ? C18 H18 0.9500 . ? C19 C20 1.417(13) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.372(12) . ? C21 C22 1.421(12) . ? C21 C28 1.531(12) . ? C22 C23 1.413(12) . ? C23 C24 1.328(13) . ? C23 H23 0.9500 . ? C24 C25 1.415(14) . ? C24 H24 0.9500 . ? C25 C26 1.415(14) . ? C25 H25 0.9500 . ? C26 C27 1.535(12) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.386(12) . ? C28 C33 1.430(10) . ? C29 C30 1.447(11) . ? C30 C31 1.400(12) . ? C30 H30 0.9500 . ? C31 C32 1.400(13) . ? C31 H31 0.9500 . ? C32 C33 1.406(12) . ? C32 H32 0.9500 . ? C33 C34 1.564(12) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.370(12) . ? C36 H36 0.9500 . ? C37 C38 1.412(11) . ? C38 C39 1.396(12) . ? C38 H38 0.9500 . ? C39 C40 1.410(12) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.397(12) . ? C45 C46 1.410(13) . ? C45 C52 1.508(12) . ? C46 C47 1.359(12) . ? C47 C48 1.387(14) . ? C47 H47 0.9500 . ? C48 C49 1.421(15) . ? C48 H48 0.9500 . ? C49 C50 1.437(12) . ? C49 H49 0.9500 . ? C50 C51 1.537(13) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C57 1.381(11) . ? C52 C53 1.426(11) . ? C53 C54 1.394(12) . ? C54 C55 1.376(11) . ? C54 H54 0.9500 . ? C55 C56 1.395(12) . ? C55 H55 0.9500 . ? C56 C57 1.377(12) . ? C56 H56 0.9500 . ? C57 C58 1.525(11) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.447(11) . ? C60 H60 0.9500 . ? C61 C62 1.379(11) . ? C62 C63 1.377(13) . ? C62 H62 0.9500 . ? C63 C64 1.406(13) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C70 1.372(12) . ? C65 C66 1.378(13) . ? C65 C72 1.493(12) . ? C66 C67 1.412(14) . ? C67 C68 1.416(17) . ? C67 H67 0.9500 . ? C68 C69 1.393(15) . ? C68 H68 0.9500 . ? C69 C70 1.407(12) . ? C69 H69 0.9500 . ? C70 C71 1.541(13) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.417(11) . ? C72 C77 1.455(11) . ? C73 C74 1.433(12) . ? C74 C75 1.390(12) . ? C74 H74 0.9500 . ? C75 C76 1.385(13) . ? C75 H75 0.9500 . ? C76 C77 1.389(12) . ? C76 H76 0.9500 . ? C77 C78 1.533(13) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C81 1.414(12) . ? C80 H80 0.9500 . ? C81 C82 1.434(12) . ? C82 C83 1.391(12) . ? C82 H82 0.9500 . ? C83 C84 1.401(12) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 C94 1.394(13) . ? C89 C90 1.406(13) . ? C89 C96 1.498(12) . ? C90 C91 1.418(12) . ? C91 C92 1.359(14) . ? C91 H91 0.9500 . ? C92 C93 1.388(13) . ? C92 H92 0.9500 . ? C93 C94 1.466(11) . ? C93 H93 0.9500 . ? C94 C95 1.498(13) . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 C101 1.418(12) . ? C96 C97 1.415(12) . ? C97 C98 1.406(12) . ? C98 C99 1.385(13) . ? C98 H98 0.9500 . ? C99 C100 1.383(12) . ? C99 H99 0.9500 . ? C100 C101 1.390(12) . ? C100 H100 0.9500 . ? C101 C102 1.533(12) . ? C102 H10A 0.9800 . ? C102 H10B 0.9800 . ? C102 H10C 0.9800 . ? C103 H10D 0.9800 . ? C103 H10E 0.9800 . ? C103 H10F 0.9800 . ? C104 C105 1.424(11) . ? C104 H104 0.9500 . ? C105 C106 1.412(12) . ? C106 C107 1.388(12) . ? C106 H106 0.9500 . ? C107 C108 1.396(12) . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 C114 1.391(13) . ? C109 C110 1.406(13) . ? C109 C116 1.510(13) . ? C110 C111 1.371(13) . ? C111 C112 1.462(14) . ? C111 H111 0.9500 . ? C112 C113 1.377(16) . ? C112 H112 0.9500 . ? C113 C114 1.398(14) . ? C113 H113 0.9500 . ? C114 C115 1.557(15) . ? C115 H11A 0.9800 . ? C115 H11B 0.9800 . ? C115 H11C 0.9800 . ? C116 C121 1.415(13) . ? C116 C117 1.440(13) . ? C117 C118 1.392(12) . ? C118 C119 1.381(14) . ? C118 H118 0.9500 . ? C119 C120 1.383(14) . ? C119 H119 0.9500 . ? C120 C121 1.362(14) . ? C120 H120 0.9500 . ? C121 C122 1.501(15) . ? C122 H12A 0.9800 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C124 C125 1.445(11) . ? C124 H124 0.9500 . ? C125 C126 1.401(11) . ? C126 C127 1.368(12) . ? C126 H126 0.9500 . ? C127 C128 1.446(12) . ? C127 H127 0.9500 . ? C128 H128 0.9500 . ? C129 H12G 0.9800 . ? C129 H12H 0.9800 . ? C129 H12I 0.9800 . ? C130 H13A 0.9800 . ? C130 H13B 0.9800 . ? C130 H13C 0.9800 . ? C131 H13D 0.9800 . ? C131 H13E 0.9800 . ? C131 H13F 0.9800 . ? C132 H13G 0.9800 . ? C132 H13H 0.9800 . ? C132 H13I 0.9800 . ? C133 C134 1.431(13) . ? C133 C138 1.434(12) . ? C133 C140 1.524(12) . ? C134 C135 1.408(14) . ? C135 C136 1.371(16) . ? C135 H135 0.9500 . ? C136 C137 1.387(15) . ? C136 H136 0.9500 . ? C137 C138 1.422(13) . ? C137 H137 0.9500 . ? C138 C139 1.497(13) . ? C139 H13J 0.9800 . ? C139 H13K 0.9800 . ? C139 H13L 0.9800 . ? C140 C145 1.403(12) . ? C140 C141 1.434(12) . ? C141 C142 1.355(12) . ? C142 C143 1.397(12) . ? C142 H142 0.9500 . ? C143 C144 1.368(13) . ? C143 H143 0.9500 . ? C144 C145 1.413(12) . ? C144 H144 0.9500 . ? C145 C146 1.545(12) . ? C146 H14D 0.9800 . ? C146 H14E 0.9800 . ? C146 H14F 0.9800 . ? C147 H14G 0.9800 . ? C147 H14H 0.9800 . ? C147 H14I 0.9800 . ? C148 C149 1.413(11) . ? C148 H148 0.9500 . ? C149 C150 1.420(11) . ? C150 C151 1.427(11) . ? C150 H150 0.9500 . ? C151 C152 1.406(13) . ? C151 H151 0.9500 . ? C152 H152 0.9500 . ? C153 C158 1.420(11) . ? C153 C154 1.430(12) . ? C153 C160 1.502(11) . ? C154 C155 1.443(12) . ? C155 C156 1.328(13) . ? C155 H155 0.9500 . ? C156 C157 1.389(14) . ? C156 H156 0.9500 . ? C157 C158 1.391(13) . ? C157 H157 0.9500 . ? C158 C159 1.501(13) . ? C159 H15D 0.9800 . ? C159 H15E 0.9800 . ? C159 H15F 0.9800 . ? C160 C161 1.410(12) . ? C160 C165 1.422(11) . ? C161 C162 1.434(11) . ? C162 C163 1.394(12) . ? C162 H162 0.9500 . ? C163 C164 1.369(13) . ? C163 H163 0.9500 . ? C164 C165 1.417(13) . ? C164 H164 0.9500 . ? C165 C166 1.540(12) . ? C166 H16A 0.9800 . ? C166 H16B 0.9800 . ? C166 H16C 0.9800 . ? C167 H16D 0.9800 . ? C167 H16E 0.9800 . ? C167 H16F 0.9800 . ? C168 C169 1.379(11) . ? C168 H168 0.9500 . ? C169 C170 1.409(12) . ? C170 C171 1.407(12) . ? C170 H170 0.9500 . ? C171 C172 1.403(13) . ? C171 H171 0.9500 . ? C172 H172 0.9500 . ? C173 H17A 0.9800 . ? C173 H17B 0.9800 . ? C173 H17C 0.9800 . ? C174 H17D 0.9800 . ? C174 H17E 0.9800 . ? C174 H17F 0.9800 . ? C175 H17G 0.9800 . ? C175 H17H 0.9800 . ? C175 H17I 0.9800 . ? C176 H17J 0.9800 . ? C176 H17K 0.9800 . ? C176 H17L 0.9800 . ? C177 C178 1.3900 . ? C177 C182 1.3900 . ? C177 H177 0.9500 . ? C178 C179 1.3900 . ? C178 H178 0.9500 . ? C179 C180 1.3900 . ? C179 H179 0.9500 . ? C180 C181 1.3900 . ? C180 H180 0.9500 . ? C181 C182 1.3900 . ? C181 H181 0.9500 . ? C182 H182 0.9500 . ? C183 C188 1.3900 . ? C183 C184 1.3900 . ? C183 H183 0.9500 . ? C184 C185 1.3900 . ? C184 H184 0.9500 . ? C185 C186 1.3900 . ? C185 H185 0.9500 . ? C186 C187 1.3900 . ? C186 H186 0.9500 . ? C187 C188 1.3900 . ? C187 H187 0.9500 . ? C188 H188 0.9500 . ? C189 C190 1.3900 . ? C189 C194 1.3900 . ? C189 H189 0.9500 . ? C190 C191 1.3900 . ? C190 H190 0.9500 . ? C191 C192 1.3899 . ? C191 H191 0.9500 . ? C192 C193 1.3900 . ? C192 H192 0.9500 . ? C193 C194 1.3900 . ? C193 H193 0.9500 . ? C194 H194 0.9500 . ? C195 C196 1.3899 . ? C195 C200 1.3901 . ? C195 H195 0.9500 . ? C196 C197 1.3900 . ? C196 H196 0.9500 . ? C197 C198 1.3900 . ? C197 H197 0.9500 . ? C198 C199 1.3900 . ? C198 H198 0.9500 . ? C199 C200 1.3900 . ? C199 H199 0.9500 . ? C200 H200 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ti1 N5 99.3(3) . . ? N6 Ti1 N1 98.0(3) . . ? N5 Ti1 N1 97.1(3) . . ? N6 Ti1 N2 91.1(3) . . ? N5 Ti1 N2 168.3(3) . . ? N1 Ti1 N2 76.0(2) . . ? N6 Ti1 N4 168.9(3) . . ? N5 Ti1 N4 89.6(3) . . ? N1 Ti1 N4 87.4(3) . . ? N2 Ti1 N4 80.8(3) . . ? N6 Ti1 N3 96.6(3) . . ? N5 Ti1 N3 99.4(3) . . ? N1 Ti1 N3 155.9(3) . . ? N2 Ti1 N3 84.6(2) . . ? N4 Ti1 N3 75.2(2) . . ? N11 Ti2 N12 99.0(3) . . ? N11 Ti2 N7 96.9(3) . . ? N12 Ti2 N7 97.7(3) . . ? N11 Ti2 N10 168.0(3) . . ? N12 Ti2 N10 91.9(3) . . ? N7 Ti2 N10 86.4(3) . . ? N11 Ti2 N9 96.6(3) . . ? N12 Ti2 N9 97.8(3) . . ? N7 Ti2 N9 157.5(3) . . ? N10 Ti2 N9 76.9(3) . . ? N11 Ti2 N8 91.1(3) . . ? N12 Ti2 N8 168.5(3) . . ? N7 Ti2 N8 75.4(2) . . ? N10 Ti2 N8 78.6(3) . . ? N9 Ti2 N8 86.4(2) . . ? N18 Ti3 N17 97.3(3) . . ? N18 Ti3 N14 92.5(3) . . ? N17 Ti3 N14 168.5(3) . . ? N18 Ti3 N15 95.7(3) . . ? N17 Ti3 N15 99.9(3) . . ? N14 Ti3 N15 85.0(3) . . ? N18 Ti3 N13 98.7(3) . . ? N17 Ti3 N13 96.4(3) . . ? N14 Ti3 N13 76.1(3) . . ? N15 Ti3 N13 156.7(3) . . ? N18 Ti3 N16 169.6(3) . . ? N17 Ti3 N16 90.9(3) . . ? N14 Ti3 N16 80.1(3) . . ? N15 Ti3 N16 76.4(3) . . ? N13 Ti3 N16 86.8(2) . . ? N24 Ti4 N23 99.7(3) . . ? N24 Ti4 N19 96.5(3) . . ? N23 Ti4 N19 97.2(3) . . ? N24 Ti4 N20 90.4(3) . . ? N23 Ti4 N20 168.1(3) . . ? N19 Ti4 N20 75.2(2) . . ? N24 Ti4 N22 168.6(3) . . ? N23 Ti4 N22 90.1(3) . . ? N19 Ti4 N22 88.1(2) . . ? N20 Ti4 N22 80.6(2) . . ? N24 Ti4 N21 97.4(3) . . ? N23 Ti4 N21 97.9(3) . . ? N19 Ti4 N21 157.4(2) . . ? N20 Ti4 N21 87.0(3) . . ? N22 Ti4 N21 75.2(2) . . ? C16 N1 C9 112.2(7) . . ? C16 N1 Ti1 116.2(5) . . ? C9 N1 Ti1 131.0(5) . . ? C20 N2 C17 104.2(7) . . ? C20 N2 Ti1 141.2(6) . . ? C17 N2 Ti1 112.4(5) . . ? C36 N3 C29 120.2(7) . . ? C36 N3 Ti1 111.5(5) . . ? C29 N3 Ti1 128.3(5) . . ? C40 N4 C37 106.5(7) . . ? C40 N4 Ti1 139.9(6) . . ? C37 N4 Ti1 113.6(5) . . ? C42 N5 C41 109.5(7) . . ? C42 N5 Ti1 126.0(6) . . ? C41 N5 Ti1 124.2(5) . . ? C44 N6 C43 108.6(6) . . ? C44 N6 Ti1 125.1(6) . . ? C43 N6 Ti1 125.8(5) . . ? C60 N7 C53 115.6(7) . . ? C60 N7 Ti2 116.4(5) . . ? C53 N7 Ti2 127.8(5) . . ? C64 N8 C61 103.1(7) . . ? C64 N8 Ti2 143.9(6) . . ? C61 N8 Ti2 112.8(5) . . ? C80 N9 C73 119.8(7) . . ? C80 N9 Ti2 112.2(5) . . ? C73 N9 Ti2 127.9(5) . . ? C84 N10 C81 106.5(6) . . ? C84 N10 Ti2 141.6(5) . . ? C81 N10 Ti2 111.7(5) . . ? C86 N11 C85 106.9(7) . . ? C86 N11 Ti2 128.5(6) . . ? C85 N11 Ti2 123.3(6) . . ? C88 N12 C87 109.5(7) . . ? C88 N12 Ti2 125.9(6) . . ? C87 N12 Ti2 124.3(6) . . ? C104 N13 C97 118.8(7) . . ? C104 N13 Ti3 112.0(5) . . ? C97 N13 Ti3 129.2(5) . . ? C105 N14 C108 105.4(7) . . ? C105 N14 Ti3 112.7(5) . . ? C108 N14 Ti3 141.4(6) . . ? C124 N15 C117 115.4(7) . . ? C124 N15 Ti3 113.4(5) . . ? C117 N15 Ti3 131.2(6) . . ? C128 N16 C125 104.9(7) . . ? C128 N16 Ti3 142.1(6) . . ? C125 N16 Ti3 112.9(5) . . ? C130 N17 C129 108.0(7) . . ? C130 N17 Ti3 125.1(5) . . ? C129 N17 Ti3 126.1(6) . . ? C131 N18 C132 108.5(7) . . ? C131 N18 Ti3 126.4(6) . . ? C132 N18 Ti3 124.8(6) . . ? C148 N19 C141 115.6(7) . . ? C148 N19 Ti4 116.2(5) . . ? C141 N19 Ti4 127.9(5) . . ? C152 N20 C149 103.8(7) . . ? C152 N20 Ti4 142.2(6) . . ? C149 N20 Ti4 113.6(5) . . ? C168 N21 C161 120.2(7) . . ? C168 N21 Ti4 113.4(5) . . ? C161 N21 Ti4 126.4(5) . . ? C169 N22 C172 105.9(7) . . ? C169 N22 Ti4 113.0(5) . . ? C172 N22 Ti4 141.0(6) . . ? C174 N23 C173 107.3(6) . . ? C174 N23 Ti4 126.3(6) . . ? C173 N23 Ti4 125.7(5) . . ? C176 N24 C175 110.0(7) . . ? C176 N24 Ti4 126.3(5) . . ? C175 N24 Ti4 123.1(6) . . ? C2 O1 C15 121.0(9) . . ? C22 O2 C35 118.9(7) . . ? C46 O3 C59 118.3(7) . . ? C66 O4 C79 116.2(8) . . ? C90 O5 C103 116.4(8) . . ? C110 O6 C123 117.1(8) . . ? C134 O7 C147 119.6(9) . . ? C154 O8 C167 117.4(8) . . ? C6 C1 C2 120.0(8) . . ? C6 C1 C8 122.8(7) . . ? C2 C1 C8 117.2(7) . . ? O1 C2 C3 122.5(9) . . ? O1 C2 C1 118.3(8) . . ? C3 C2 C1 119.0(9) . . ? C4 C3 C2 120.6(10) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.4(9) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 122.0(10) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C1 117.7(8) . . ? C5 C6 C7 124.0(8) . . ? C1 C6 C7 118.3(8) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 118.8(7) . . ? C9 C8 C1 123.0(7) . . ? C13 C8 C1 118.0(7) . . ? C8 C9 C10 121.3(7) . . ? C8 C9 N1 121.1(7) . . ? C10 C9 N1 117.5(7) . . ? C11 C10 C9 120.0(8) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.1(8) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 119.5(8) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.3 . . ? C8 C13 C12 120.1(8) . . ? C8 C13 C14 121.2(8) . . ? C12 C13 C14 118.7(8) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.4 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C15 H15A 109.5 . . ? O1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 116.3(7) . . ? N1 C16 H16 121.9 . . ? C17 C16 H16 121.8 . . ? C18 C17 N2 112.4(7) . . ? C18 C17 C16 130.4(8) . . ? N2 C17 C16 117.2(7) . . ? C17 C18 C19 104.1(7) . . ? C17 C18 H18 128.0 . . ? C19 C18 H18 128.0 . . ? C18 C19 C20 107.8(8) . . ? C18 C19 H19 126.1 . . ? C20 C19 H19 126.1 . . ? N2 C20 C19 111.4(8) . . ? N2 C20 H20 124.3 . . ? C19 C20 H20 124.3 . . ? C26 C21 C22 117.5(8) . . ? C26 C21 C28 125.2(8) . . ? C22 C21 C28 117.3(7) . . ? O2 C22 C23 124.4(9) . . ? O2 C22 C21 114.6(7) . . ? C23 C22 C21 121.0(8) . . ? C24 C23 C22 119.7(9) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 121.9(9) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C24 C25 C26 118.0(9) . . ? C24 C25 H25 121.0 . . ? C26 C25 H25 121.0 . . ? C21 C26 C25 121.8(9) . . ? C21 C26 C27 118.3(8) . . ? C25 C26 C27 119.8(8) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 119.5(8) . . ? C29 C28 C21 119.9(7) . . ? C33 C28 C21 120.6(8) . . ? C28 C29 N3 123.4(7) . . ? C28 C29 C30 121.1(7) . . ? N3 C29 C30 115.4(8) . . ? C31 C30 C29 117.6(8) . . ? C31 C30 H30 121.2 . . ? C29 C30 H30 121.2 . . ? C32 C31 C30 122.0(9) . . ? C32 C31 H31 119.0 . . ? C30 C31 H31 119.0 . . ? C31 C32 C33 119.5(8) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C32 C33 C28 120.1(8) . . ? C32 C33 C34 121.6(7) . . ? C28 C33 C34 118.3(8) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O2 C35 H35A 109.5 . . ? O2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O2 C35 H35C 109.4 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 C37 123.7(8) . . ? N3 C36 H36 118.2 . . ? C37 C36 H36 118.1 . . ? C36 C37 N4 115.9(8) . . ? C36 C37 C38 135.6(8) . . ? N4 C37 C38 108.4(8) . . ? C39 C38 C37 108.0(7) . . ? C39 C38 H38 126.0 . . ? C37 C38 H38 126.0 . . ? C38 C39 C40 105.7(7) . . ? C38 C39 H39 127.2 . . ? C40 C39 H39 127.1 . . ? N4 C40 C39 111.3(7) . . ? N4 C40 H40 124.3 . . ? C39 C40 H40 124.3 . . ? N5 C41 H41A 109.5 . . ? N5 C41 H41B 109.4 . . ? H41A C41 H41B 109.5 . . ? N5 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N5 C42 H42A 109.4 . . ? N5 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N5 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N6 C43 H43A 109.5 . . ? N6 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N6 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N6 C44 H44A 109.5 . . ? N6 C44 H44B 109.4 . . ? H44A C44 H44B 109.5 . . ? N6 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 120.4(9) . . ? C50 C45 C52 121.2(8) . . ? C46 C45 C52 118.4(8) . . ? C47 C46 O3 124.9(9) . . ? C47 C46 C45 120.7(9) . . ? O3 C46 C45 114.4(8) . . ? C46 C47 C48 121.4(10) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.2 . . ? C47 C48 C49 119.4(9) . . ? C47 C48 H48 120.3 . . ? C49 C48 H48 120.3 . . ? C48 C49 C50 119.5(9) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.3 . . ? C45 C50 C49 118.4(9) . . ? C45 C50 C51 120.9(8) . . ? C49 C50 C51 120.6(8) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C57 C52 C53 118.6(8) . . ? C57 C52 C45 121.1(7) . . ? C53 C52 C45 120.2(7) . . ? C54 C53 C52 118.8(7) . . ? C54 C53 N7 117.8(7) . . ? C52 C53 N7 123.2(7) . . ? C55 C54 C53 122.3(8) . . ? C55 C54 H54 118.9 . . ? C53 C54 H54 118.9 . . ? C54 C55 C56 117.4(8) . . ? C54 C55 H55 121.3 . . ? C56 C55 H55 121.3 . . ? C57 C56 C55 122.1(7) . . ? C57 C56 H56 119.0 . . ? C55 C56 H56 118.9 . . ? C52 C57 C56 120.5(8) . . ? C52 C57 C58 119.4(8) . . ? C56 C57 C58 120.1(8) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O3 C59 H59A 109.5 . . ? O3 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? O3 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N7 C60 C61 117.9(8) . . ? N7 C60 H60 121.0 . . ? C61 C60 H60 121.1 . . ? C62 C61 N8 111.5(7) . . ? C62 C61 C60 131.1(9) . . ? N8 C61 C60 117.2(7) . . ? C61 C62 C63 106.6(8) . . ? C61 C62 H62 126.7 . . ? C63 C62 H62 126.7 . . ? C62 C63 C64 104.4(8) . . ? C62 C63 H63 127.8 . . ? C64 C63 H63 127.8 . . ? N8 C64 C63 114.3(8) . . ? N8 C64 H64 122.9 . . ? C63 C64 H64 122.9 . . ? C70 C65 C66 118.9(8) . . ? C70 C65 C72 119.1(8) . . ? C66 C65 C72 122.0(8) . . ? C65 C66 O4 113.1(8) . . ? C65 C66 C67 122.9(10) . . ? O4 C66 C67 123.8(9) . . ? C66 C67 C68 116.3(10) . . ? C66 C67 H67 121.8 . . ? C68 C67 H67 121.9 . . ? C69 C68 C67 121.9(9) . . ? C69 C68 H68 119.1 . . ? C67 C68 H68 119.0 . . ? C68 C69 C70 118.2(10) . . ? C68 C69 H69 120.9 . . ? C70 C69 H69 120.9 . . ? C65 C70 C69 121.8(9) . . ? C65 C70 C71 125.1(8) . . ? C69 C70 C71 113.2(8) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C73 C72 C77 117.8(8) . . ? C73 C72 C65 124.5(7) . . ? C77 C72 C65 117.8(7) . . ? C72 C73 N9 120.7(7) . . ? C72 C73 C74 120.6(8) . . ? N9 C73 C74 118.6(7) . . ? C75 C74 C73 119.3(8) . . ? C75 C74 H74 120.4 . . ? C73 C74 H74 120.3 . . ? C74 C75 C76 121.0(8) . . ? C74 C75 H75 119.5 . . ? C76 C75 H75 119.5 . . ? C77 C76 C75 121.3(8) . . ? C77 C76 H76 119.3 . . ? C75 C76 H76 119.4 . . ? C76 C77 C72 119.9(8) . . ? C76 C77 C78 120.8(8) . . ? C72 C77 C78 119.3(8) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? O4 C79 H79A 109.5 . . ? O4 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? O4 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? N9 C80 C81 120.9(8) . . ? N9 C80 H80 119.5 . . ? C81 C80 H80 119.5 . . ? N10 C81 C80 117.9(7) . . ? N10 C81 C82 108.5(7) . . ? C80 C81 C82 133.4(8) . . ? C83 C82 C81 107.1(8) . . ? C83 C82 H82 126.4 . . ? C81 C82 H82 126.4 . . ? C82 C83 C84 105.9(8) . . ? C82 C83 H83 127.0 . . ? C84 C83 H83 127.0 . . ? N10 C84 C83 111.8(7) . . ? N10 C84 H84 124.1 . . ? C83 C84 H84 124.1 . . ? N11 C85 H85A 109.5 . . ? N11 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? N11 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? N11 C86 H86A 109.5 . . ? N11 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? N11 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N12 C87 H87A 109.4 . . ? N12 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? N12 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N12 C88 H88A 109.5 . . ? N12 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? N12 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C94 C89 C90 121.4(8) . . ? C94 C89 C96 116.4(8) . . ? C90 C89 C96 122.0(8) . . ? O5 C90 C89 113.6(8) . . ? O5 C90 C91 126.8(8) . . ? C89 C90 C91 119.6(9) . . ? C92 C91 C90 119.3(9) . . ? C92 C91 H91 120.3 . . ? C90 C91 H91 120.4 . . ? C91 C92 C93 123.3(8) . . ? C91 C92 H92 118.3 . . ? C93 C92 H92 118.4 . . ? C92 C93 C94 118.3(9) . . ? C92 C93 H93 120.8 . . ? C94 C93 H93 120.9 . . ? C89 C94 C93 118.0(9) . . ? C89 C94 C95 124.4(7) . . ? C93 C94 C95 117.6(8) . . ? C94 C95 H95A 109.5 . . ? C94 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C94 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C101 C96 C97 117.3(8) . . ? C101 C96 C89 120.9(7) . . ? C97 C96 C89 121.8(7) . . ? C98 C97 C96 120.3(8) . . ? C98 C97 N13 117.4(7) . . ? C96 C97 N13 122.3(8) . . ? C99 C98 C97 120.6(8) . . ? C99 C98 H98 119.7 . . ? C97 C98 H98 119.6 . . ? C98 C99 C100 120.0(9) . . ? C98 C99 H99 120.0 . . ? C100 C99 H99 120.0 . . ? C101 C100 C99 120.1(8) . . ? C101 C100 H100 119.9 . . ? C99 C100 H100 120.0 . . ? C100 C101 C96 121.5(7) . . ? C100 C101 C102 120.0(8) . . ? C96 C101 C102 118.5(8) . . ? C101 C102 H10A 109.5 . . ? C101 C102 H10B 109.4 . . ? H10A C102 H10B 109.5 . . ? C101 C102 H10C 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? O5 C103 H10D 109.5 . . ? O5 C103 H10E 109.5 . . ? H10D C103 H10E 109.5 . . ? O5 C103 H10F 109.5 . . ? H10D C103 H10F 109.5 . . ? H10E C103 H10F 109.5 . . ? N13 C104 C105 121.1(8) . . ? N13 C104 H104 119.4 . . ? C105 C104 H104 119.4 . . ? N14 C105 C106 109.6(8) . . ? N14 C105 C104 117.3(7) . . ? C106 C105 C104 133.1(8) . . ? C107 C106 C105 108.3(8) . . ? C107 C106 H106 125.8 . . ? C105 C106 H106 125.8 . . ? C106 C107 C108 104.7(7) . . ? C106 C107 H107 127.6 . . ? C108 C107 H107 127.6 . . ? N14 C108 C107 111.9(8) . . ? N14 C108 H108 124.0 . . ? C107 C108 H108 124.1 . . ? C114 C109 C110 119.3(9) . . ? C114 C109 C116 121.2(9) . . ? C110 C109 C116 119.5(8) . . ? C111 C110 O6 124.0(9) . . ? C111 C110 C109 121.7(9) . . ? O6 C110 C109 114.1(8) . . ? C110 C111 C112 118.3(10) . . ? C110 C111 H111 120.8 . . ? C112 C111 H111 120.8 . . ? C113 C112 C111 119.5(9) . . ? C113 C112 H112 120.3 . . ? C111 C112 H112 120.2 . . ? C112 C113 C114 120.5(10) . . ? C112 C113 H113 119.7 . . ? C114 C113 H113 119.7 . . ? C113 C114 C109 120.5(10) . . ? C113 C114 C115 119.0(9) . . ? C109 C114 C115 120.3(9) . . ? C114 C115 H11A 109.5 . . ? C114 C115 H11B 109.5 . . ? H11A C115 H11B 109.5 . . ? C114 C115 H11C 109.5 . . ? H11A C115 H11C 109.5 . . ? H11B C115 H11C 109.5 . . ? C121 C116 C117 118.3(9) . . ? C121 C116 C109 120.6(8) . . ? C117 C116 C109 121.0(8) . . ? C118 C117 N15 119.2(8) . . ? C118 C117 C116 117.4(8) . . ? N15 C117 C116 122.8(8) . . ? C119 C118 C117 121.3(9) . . ? C119 C118 H118 119.3 . . ? C117 C118 H118 119.3 . . ? C118 C119 C120 121.3(9) . . ? C118 C119 H119 119.4 . . ? C120 C119 H119 119.4 . . ? C121 C120 C119 118.8(10) . . ? C121 C120 H120 120.6 . . ? C119 C120 H120 120.6 . . ? C120 C121 C116 122.2(10) . . ? C120 C121 C122 119.2(9) . . ? C116 C121 C122 118.5(9) . . ? C121 C122 H12A 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? O6 C123 H12D 109.4 . . ? O6 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? O6 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? N15 C124 C125 120.1(7) . . ? N15 C124 H124 119.9 . . ? C125 C124 H124 120.0 . . ? N16 C125 C126 112.3(8) . . ? N16 C125 C124 116.9(7) . . ? C126 C125 C124 130.7(8) . . ? C127 C126 C125 105.6(7) . . ? C127 C126 H126 127.2 . . ? C125 C126 H126 127.2 . . ? C126 C127 C128 105.7(8) . . ? C126 C127 H127 127.1 . . ? C128 C127 H127 127.2 . . ? N16 C128 C127 111.5(8) . . ? N16 C128 H128 124.3 . . ? C127 C128 H128 124.2 . . ? N17 C129 H12G 109.5 . . ? N17 C129 H12H 109.5 . . ? H12G C129 H12H 109.5 . . ? N17 C129 H12I 109.5 . . ? H12G C129 H12I 109.5 . . ? H12H C129 H12I 109.5 . . ? N17 C130 H13A 109.5 . . ? N17 C130 H13B 109.5 . . ? H13A C130 H13B 109.5 . . ? N17 C130 H13C 109.5 . . ? H13A C130 H13C 109.5 . . ? H13B C130 H13C 109.5 . . ? N18 C131 H13D 109.5 . . ? N18 C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? N18 C131 H13F 109.5 . . ? H13D C131 H13F 109.5 . . ? H13E C131 H13F 109.5 . . ? N18 C132 H13G 109.4 . . ? N18 C132 H13H 109.5 . . ? H13G C132 H13H 109.5 . . ? N18 C132 H13I 109.5 . . ? H13G C132 H13I 109.5 . . ? H13H C132 H13I 109.5 . . ? C134 C133 C138 120.6(8) . . ? C134 C133 C140 117.5(8) . . ? C138 C133 C140 121.8(8) . . ? O7 C134 C135 123.8(9) . . ? O7 C134 C133 117.1(8) . . ? C135 C134 C133 119.1(9) . . ? C136 C135 C134 120.2(10) . . ? C136 C135 H135 119.9 . . ? C134 C135 H135 119.9 . . ? C135 C136 C137 121.5(10) . . ? C135 C136 H136 119.3 . . ? C137 C136 H136 119.2 . . ? C136 C137 C138 121.4(10) . . ? C136 C137 H137 119.3 . . ? C138 C137 H137 119.3 . . ? C137 C138 C133 116.9(8) . . ? C137 C138 C139 122.7(8) . . ? C133 C138 C139 120.4(7) . . ? C138 C139 H13J 109.5 . . ? C138 C139 H13K 109.5 . . ? H13J C139 H13K 109.5 . . ? C138 C139 H13L 109.5 . . ? H13J C139 H13L 109.5 . . ? H13K C139 H13L 109.5 . . ? C145 C140 C141 117.6(8) . . ? C145 C140 C133 118.6(8) . . ? C141 C140 C133 123.7(8) . . ? C142 C141 C140 121.5(8) . . ? C142 C141 N19 119.3(7) . . ? C140 C141 N19 119.1(7) . . ? C141 C142 C143 120.4(8) . . ? C141 C142 H142 119.8 . . ? C143 C142 H142 119.8 . . ? C144 C143 C142 119.6(9) . . ? C144 C143 H143 120.2 . . ? C142 C143 H143 120.2 . . ? C143 C144 C145 121.3(8) . . ? C143 C144 H144 119.3 . . ? C145 C144 H144 119.4 . . ? C140 C145 C144 119.4(8) . . ? C140 C145 C146 121.4(8) . . ? C144 C145 C146 119.2(8) . . ? C145 C146 H14D 109.5 . . ? C145 C146 H14E 109.5 . . ? H14D C146 H14E 109.5 . . ? C145 C146 H14F 109.4 . . ? H14D C146 H14F 109.5 . . ? H14E C146 H14F 109.5 . . ? O7 C147 H14G 109.5 . . ? O7 C147 H14H 109.5 . . ? H14G C147 H14H 109.5 . . ? O7 C147 H14I 109.5 . . ? H14G C147 H14I 109.5 . . ? H14H C147 H14I 109.5 . . ? N19 C148 C149 118.2(7) . . ? N19 C148 H148 120.9 . . ? C149 C148 H148 120.9 . . ? C148 C149 N20 116.2(7) . . ? C148 C149 C150 130.7(7) . . ? N20 C149 C150 113.1(7) . . ? C149 C150 C151 103.0(7) . . ? C149 C150 H150 128.5 . . ? C151 C150 H150 128.5 . . ? C152 C151 C150 107.8(7) . . ? C152 C151 H151 126.1 . . ? C150 C151 H151 126.1 . . ? N20 C152 C151 112.1(8) . . ? N20 C152 H152 124.0 . . ? C151 C152 H152 123.9 . . ? C158 C153 C154 118.5(8) . . ? C158 C153 C160 123.7(7) . . ? C154 C153 C160 117.7(7) . . ? O8 C154 C153 114.3(7) . . ? O8 C154 C155 126.5(8) . . ? C153 C154 C155 119.3(8) . . ? C156 C155 C154 119.4(9) . . ? C156 C155 H155 120.3 . . ? C154 C155 H155 120.3 . . ? C155 C156 C157 122.6(9) . . ? C155 C156 H156 118.7 . . ? C157 C156 H156 118.7 . . ? C158 C157 C156 120.7(8) . . ? C158 C157 H157 119.7 . . ? C156 C157 H157 119.7 . . ? C157 C158 C153 119.4(8) . . ? C157 C158 C159 122.5(8) . . ? C153 C158 C159 118.1(8) . . ? C158 C159 H15D 109.5 . . ? C158 C159 H15E 109.5 . . ? H15D C159 H15E 109.5 . . ? C158 C159 H15F 109.5 . . ? H15D C159 H15F 109.5 . . ? H15E C159 H15F 109.5 . . ? C161 C160 C165 117.4(7) . . ? C161 C160 C153 121.8(7) . . ? C165 C160 C153 120.7(8) . . ? C160 C161 C162 122.7(7) . . ? C160 C161 N21 120.8(7) . . ? C162 C161 N21 116.3(8) . . ? C163 C162 C161 117.1(8) . . ? C163 C162 H162 121.5 . . ? C161 C162 H162 121.4 . . ? C164 C163 C162 121.8(8) . . ? C164 C163 H163 119.1 . . ? C162 C163 H163 119.1 . . ? C163 C164 C165 121.3(8) . . ? C163 C164 H164 119.4 . . ? C165 C164 H164 119.4 . . ? C164 C165 C160 119.6(8) . . ? C164 C165 C166 120.4(7) . . ? C160 C165 C166 120.0(8) . . ? C165 C166 H16A 109.5 . . ? C165 C166 H16B 109.5 . . ? H16A C166 H16B 109.5 . . ? C165 C166 H16C 109.5 . . ? H16A C166 H16C 109.5 . . ? H16B C166 H16C 109.5 . . ? O8 C167 H16D 109.5 . . ? O8 C167 H16E 109.5 . . ? H16D C167 H16E 109.5 . . ? O8 C167 H16F 109.4 . . ? H16D C167 H16F 109.5 . . ? H16E C167 H16F 109.5 . . ? N21 C168 C169 121.5(8) . . ? N21 C168 H168 119.3 . . ? C169 C168 H168 119.2 . . ? C168 C169 N22 116.6(8) . . ? C168 C169 C170 133.3(8) . . ? N22 C169 C170 110.0(7) . . ? C171 C170 C169 106.5(8) . . ? C171 C170 H170 126.8 . . ? C169 C170 H170 126.7 . . ? C172 C171 C170 107.9(8) . . ? C172 C171 H171 126.0 . . ? C170 C171 H171 126.1 . . ? N22 C172 C171 109.7(8) . . ? N22 C172 H172 125.2 . . ? C171 C172 H172 125.2 . . ? N23 C173 H17A 109.5 . . ? N23 C173 H17B 109.5 . . ? H17A C173 H17B 109.5 . . ? N23 C173 H17C 109.5 . . ? H17A C173 H17C 109.5 . . ? H17B C173 H17C 109.5 . . ? N23 C174 H17D 109.4 . . ? N23 C174 H17E 109.5 . . ? H17D C174 H17E 109.5 . . ? N23 C174 H17F 109.5 . . ? H17D C174 H17F 109.5 . . ? H17E C174 H17F 109.5 . . ? N24 C175 H17G 109.5 . . ? N24 C175 H17H 109.5 . . ? H17G C175 H17H 109.5 . . ? N24 C175 H17I 109.5 . . ? H17G C175 H17I 109.5 . . ? H17H C175 H17I 109.5 . . ? N24 C176 H17J 109.5 . . ? N24 C176 H17K 109.4 . . ? H17J C176 H17K 109.5 . . ? N24 C176 H17L 109.4 . . ? H17J C176 H17L 109.5 . . ? H17K C176 H17L 109.5 . . ? C178 C177 C182 120.0 . . ? C178 C177 H177 120.0 . . ? C182 C177 H177 120.0 . . ? C179 C178 C177 120.0 . . ? C179 C178 H178 120.0 . . ? C177 C178 H178 120.0 . . ? C178 C179 C180 120.0 . . ? C178 C179 H179 120.0 . . ? C180 C179 H179 120.0 . . ? C181 C180 C179 120.0 . . ? C181 C180 H180 120.0 . . ? C179 C180 H180 120.0 . . ? C182 C181 C180 120.0 . . ? C182 C181 H181 120.0 . . ? C180 C181 H181 120.0 . . ? C181 C182 C177 120.0 . . ? C181 C182 H182 120.0 . . ? C177 C182 H182 120.0 . . ? C188 C183 C184 120.0 . . ? C188 C183 H183 120.0 . . ? C184 C183 H183 120.0 . . ? C185 C184 C183 120.0 . . ? C185 C184 H184 120.0 . . ? C183 C184 H184 120.0 . . ? C186 C185 C184 120.0 . . ? C186 C185 H185 120.0 . . ? C184 C185 H185 120.0 . . ? C185 C186 C187 120.0 . . ? C185 C186 H186 120.0 . . ? C187 C186 H186 120.0 . . ? C188 C187 C186 120.0 . . ? C188 C187 H187 120.0 . . ? C186 C187 H187 120.0 . . ? C183 C188 C187 120.0 . . ? C183 C188 H188 120.0 . . ? C187 C188 H188 120.0 . . ? C190 C189 C194 120.0 . . ? C190 C189 H189 120.0 . . ? C194 C189 H189 120.0 . . ? C189 C190 C191 120.0 . . ? C189 C190 H190 120.0 . . ? C191 C190 H190 120.0 . . ? C192 C191 C190 120.0 . . ? C192 C191 H191 120.0 . . ? C190 C191 H191 120.0 . . ? C191 C192 C193 120.0 . . ? C191 C192 H192 120.0 . . ? C193 C192 H192 120.0 . . ? C194 C193 C192 120.0 . . ? C194 C193 H193 120.0 . . ? C192 C193 H193 120.0 . . ? C193 C194 C189 120.0 . . ? C193 C194 H194 120.0 . . ? C189 C194 H194 120.0 . . ? C196 C195 C200 120.0 . . ? C196 C195 H195 120.0 . . ? C200 C195 H195 120.0 . . ? C195 C196 C197 120.0 . . ? C195 C196 H196 120.0 . . ? C197 C196 H196 120.0 . . ? C198 C197 C196 120.0 . . ? C198 C197 H197 120.0 . . ? C196 C197 H197 120.0 . . ? C197 C198 C199 120.0 . . ? C197 C198 H198 120.0 . . ? C199 C198 H198 120.0 . . ? C200 C199 C198 120.0 . . ? C200 C199 H199 120.0 . . ? C198 C199 H199 120.0 . . ? C199 C200 C195 120.0 . . ? C199 C200 H200 120.0 . . ? C195 C200 H200 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ti1 N1 C16 -99.6(6) . . . . ? N5 Ti1 N1 C16 159.9(6) . . . . ? N2 Ti1 N1 C16 -10.5(5) . . . . ? N4 Ti1 N1 C16 70.6(6) . . . . ? N3 Ti1 N1 C16 27.1(10) . . . . ? N6 Ti1 N1 C9 89.3(7) . . . . ? N5 Ti1 N1 C9 -11.2(7) . . . . ? N2 Ti1 N1 C9 178.4(7) . . . . ? N4 Ti1 N1 C9 -100.5(7) . . . . ? N3 Ti1 N1 C9 -144.0(7) . . . . ? N6 Ti1 N2 C20 -90.7(9) . . . . ? N5 Ti1 N2 C20 116.4(15) . . . . ? N1 Ti1 N2 C20 171.3(9) . . . . ? N4 Ti1 N2 C20 81.7(9) . . . . ? N3 Ti1 N2 C20 5.8(9) . . . . ? N6 Ti1 N2 C17 109.7(5) . . . . ? N5 Ti1 N2 C17 -43.2(15) . . . . ? N1 Ti1 N2 C17 11.7(5) . . . . ? N4 Ti1 N2 C17 -78.0(5) . . . . ? N3 Ti1 N2 C17 -153.8(5) . . . . ? N6 Ti1 N3 C36 168.8(6) . . . . ? N5 Ti1 N3 C36 -90.7(6) . . . . ? N1 Ti1 N3 C36 41.8(10) . . . . ? N2 Ti1 N3 C36 78.3(6) . . . . ? N4 Ti1 N3 C36 -3.6(6) . . . . ? N6 Ti1 N3 C29 -10.6(7) . . . . ? N5 Ti1 N3 C29 89.9(7) . . . . ? N1 Ti1 N3 C29 -137.6(7) . . . . ? N2 Ti1 N3 C29 -101.1(7) . . . . ? N4 Ti1 N3 C29 177.0(7) . . . . ? N6 Ti1 N4 C40 138.5(14) . . . . ? N5 Ti1 N4 C40 -78.4(9) . . . . ? N1 Ti1 N4 C40 18.7(9) . . . . ? N2 Ti1 N4 C40 95.0(9) . . . . ? N3 Ti1 N4 C40 -178.2(10) . . . . ? N6 Ti1 N4 C37 -39.7(18) . . . . ? N5 Ti1 N4 C37 103.3(6) . . . . ? N1 Ti1 N4 C37 -159.6(6) . . . . ? N2 Ti1 N4 C37 -83.3(6) . . . . ? N3 Ti1 N4 C37 3.5(6) . . . . ? N6 Ti1 N5 C42 156.5(7) . . . . ? N1 Ti1 N5 C42 -104.1(7) . . . . ? N2 Ti1 N5 C42 -50.9(17) . . . . ? N4 Ti1 N5 C42 -16.7(7) . . . . ? N3 Ti1 N5 C42 58.2(7) . . . . ? N6 Ti1 N5 C41 -31.6(7) . . . . ? N1 Ti1 N5 C41 67.8(7) . . . . ? N2 Ti1 N5 C41 121.0(13) . . . . ? N4 Ti1 N5 C41 155.2(7) . . . . ? N3 Ti1 N5 C41 -129.9(7) . . . . ? N5 Ti1 N6 C44 152.1(6) . . . . ? N1 Ti1 N6 C44 53.5(7) . . . . ? N2 Ti1 N6 C44 -22.5(6) . . . . ? N4 Ti1 N6 C44 -65.4(17) . . . . ? N3 Ti1 N6 C44 -107.2(6) . . . . ? N5 Ti1 N6 C43 -37.3(6) . . . . ? N1 Ti1 N6 C43 -135.9(6) . . . . ? N2 Ti1 N6 C43 148.1(6) . . . . ? N4 Ti1 N6 C43 105.2(15) . . . . ? N3 Ti1 N6 C43 63.4(6) . . . . ? N11 Ti2 N7 C60 -93.2(6) . . . . ? N12 Ti2 N7 C60 166.7(6) . . . . ? N10 Ti2 N7 C60 75.2(6) . . . . ? N9 Ti2 N7 C60 33.3(10) . . . . ? N8 Ti2 N7 C60 -3.9(6) . . . . ? N11 Ti2 N7 C53 90.4(7) . . . . ? N12 Ti2 N7 C53 -9.7(7) . . . . ? N10 Ti2 N7 C53 -101.1(7) . . . . ? N9 Ti2 N7 C53 -143.0(7) . . . . ? N8 Ti2 N7 C53 179.8(7) . . . . ? N11 Ti2 N8 C64 -86.0(10) . . . . ? N12 Ti2 N8 C64 122.6(15) . . . . ? N7 Ti2 N8 C64 177.1(10) . . . . ? N10 Ti2 N8 C64 87.9(10) . . . . ? N9 Ti2 N8 C64 10.5(10) . . . . ? N11 Ti2 N8 C61 99.5(6) . . . . ? N12 Ti2 N8 C61 -51.9(16) . . . . ? N7 Ti2 N8 C61 2.7(5) . . . . ? N10 Ti2 N8 C61 -86.6(6) . . . . ? N9 Ti2 N8 C61 -163.9(6) . . . . ? N11 Ti2 N9 C80 165.8(5) . . . . ? N12 Ti2 N9 C80 -94.1(6) . . . . ? N7 Ti2 N9 C80 39.2(9) . . . . ? N10 Ti2 N9 C80 -4.0(5) . . . . ? N8 Ti2 N9 C80 75.1(5) . . . . ? N11 Ti2 N9 C73 -11.9(7) . . . . ? N12 Ti2 N9 C73 88.2(7) . . . . ? N7 Ti2 N9 C73 -138.5(7) . . . . ? N10 Ti2 N9 C73 178.3(7) . . . . ? N8 Ti2 N9 C73 -102.6(7) . . . . ? N11 Ti2 N10 C84 121.7(15) . . . . ? N12 Ti2 N10 C84 -82.5(9) . . . . ? N7 Ti2 N10 C84 15.1(9) . . . . ? N9 Ti2 N10 C84 179.9(9) . . . . ? N8 Ti2 N10 C84 90.9(9) . . . . ? N11 Ti2 N10 C81 -52.9(15) . . . . ? N12 Ti2 N10 C81 102.8(5) . . . . ? N7 Ti2 N10 C81 -159.6(5) . . . . ? N9 Ti2 N10 C81 5.2(5) . . . . ? N8 Ti2 N10 C81 -83.7(5) . . . . ? N12 Ti2 N11 C86 159.0(7) . . . . ? N7 Ti2 N11 C86 60.0(7) . . . . ? N10 Ti2 N11 C86 -45.5(18) . . . . ? N9 Ti2 N11 C86 -101.9(7) . . . . ? N8 Ti2 N11 C86 -15.4(7) . . . . ? N12 Ti2 N11 C85 -35.9(7) . . . . ? N7 Ti2 N11 C85 -134.8(6) . . . . ? N10 Ti2 N11 C85 119.6(13) . . . . ? N9 Ti2 N11 C85 63.2(6) . . . . ? N8 Ti2 N11 C85 149.7(6) . . . . ? N11 Ti2 N12 C88 -34.0(7) . . . . ? N7 Ti2 N12 C88 64.3(7) . . . . ? N10 Ti2 N12 C88 150.9(7) . . . . ? N9 Ti2 N12 C88 -132.0(7) . . . . ? N8 Ti2 N12 C88 117.0(14) . . . . ? N11 Ti2 N12 C87 153.0(6) . . . . ? N7 Ti2 N12 C87 -108.7(7) . . . . ? N10 Ti2 N12 C87 -22.0(7) . . . . ? N9 Ti2 N12 C87 55.0(7) . . . . ? N8 Ti2 N12 C87 -56.0(16) . . . . ? N18 Ti3 N13 C104 -95.7(5) . . . . ? N17 Ti3 N13 C104 165.9(5) . . . . ? N14 Ti3 N13 C104 -5.3(5) . . . . ? N15 Ti3 N13 C104 31.7(9) . . . . ? N16 Ti3 N13 C104 75.3(5) . . . . ? N18 Ti3 N13 C97 86.6(7) . . . . ? N17 Ti3 N13 C97 -11.8(7) . . . . ? N14 Ti3 N13 C97 177.0(7) . . . . ? N15 Ti3 N13 C97 -146.0(7) . . . . ? N16 Ti3 N13 C97 -102.3(7) . . . . ? N18 Ti3 N14 C105 105.6(6) . . . . ? N17 Ti3 N14 C105 -43.0(16) . . . . ? N15 Ti3 N14 C105 -158.9(6) . . . . ? N13 Ti3 N14 C105 7.3(5) . . . . ? N16 Ti3 N14 C105 -81.8(6) . . . . ? N18 Ti3 N14 C108 -84.0(9) . . . . ? N17 Ti3 N14 C108 127.4(14) . . . . ? N15 Ti3 N14 C108 11.5(9) . . . . ? N13 Ti3 N14 C108 177.7(9) . . . . ? N16 Ti3 N14 C108 88.6(9) . . . . ? N18 Ti3 N15 C124 169.2(6) . . . . ? N17 Ti3 N15 C124 -92.4(6) . . . . ? N14 Ti3 N15 C124 77.1(6) . . . . ? N13 Ti3 N15 C124 41.2(10) . . . . ? N16 Ti3 N15 C124 -3.9(6) . . . . ? N18 Ti3 N15 C117 -7.2(8) . . . . ? N17 Ti3 N15 C117 91.3(8) . . . . ? N14 Ti3 N15 C117 -99.2(8) . . . . ? N13 Ti3 N15 C117 -135.1(8) . . . . ? N16 Ti3 N15 C117 179.8(8) . . . . ? N18 Ti3 N16 C128 136.5(15) . . . . ? N17 Ti3 N16 C128 -81.8(10) . . . . ? N14 Ti3 N16 C128 91.1(10) . . . . ? N15 Ti3 N16 C128 178.3(10) . . . . ? N13 Ti3 N16 C128 14.6(10) . . . . ? N18 Ti3 N16 C125 -38.4(18) . . . . ? N17 Ti3 N16 C125 103.3(6) . . . . ? N14 Ti3 N16 C125 -83.8(6) . . . . ? N15 Ti3 N16 C125 3.4(5) . . . . ? N13 Ti3 N16 C125 -160.3(6) . . . . ? N18 Ti3 N17 C130 -32.8(7) . . . . ? N14 Ti3 N17 C130 115.6(14) . . . . ? N15 Ti3 N17 C130 -129.9(7) . . . . ? N13 Ti3 N17 C130 66.8(7) . . . . ? N16 Ti3 N17 C130 153.7(7) . . . . ? N18 Ti3 N17 C129 158.3(6) . . . . ? N14 Ti3 N17 C129 -53.3(16) . . . . ? N15 Ti3 N17 C129 61.1(6) . . . . ? N13 Ti3 N17 C129 -102.1(6) . . . . ? N16 Ti3 N17 C129 -15.2(6) . . . . ? N17 Ti3 N18 C131 -37.3(8) . . . . ? N14 Ti3 N18 C131 148.7(7) . . . . ? N15 Ti3 N18 C131 63.4(8) . . . . ? N13 Ti3 N18 C131 -135.0(7) . . . . ? N16 Ti3 N18 C131 104.1(16) . . . . ? N17 Ti3 N18 C132 150.5(7) . . . . ? N14 Ti3 N18 C132 -23.6(7) . . . . ? N15 Ti3 N18 C132 -108.8(7) . . . . ? N13 Ti3 N18 C132 52.8(7) . . . . ? N16 Ti3 N18 C132 -68.2(18) . . . . ? N24 Ti4 N19 C148 -94.9(6) . . . . ? N23 Ti4 N19 C148 164.4(6) . . . . ? N20 Ti4 N19 C148 -6.2(6) . . . . ? N22 Ti4 N19 C148 74.6(6) . . . . ? N21 Ti4 N19 C148 32.7(9) . . . . ? N24 Ti4 N19 C141 91.8(6) . . . . ? N23 Ti4 N19 C141 -8.9(6) . . . . ? N20 Ti4 N19 C141 -179.5(6) . . . . ? N22 Ti4 N19 C141 -98.7(6) . . . . ? N21 Ti4 N19 C141 -140.6(7) . . . . ? N24 Ti4 N20 C152 -87.3(9) . . . . ? N23 Ti4 N20 C152 124.6(14) . . . . ? N19 Ti4 N20 C152 176.1(10) . . . . ? N22 Ti4 N20 C152 85.6(9) . . . . ? N21 Ti4 N20 C152 10.1(9) . . . . ? N24 Ti4 N20 C149 102.6(5) . . . . ? N23 Ti4 N20 C149 -45.5(16) . . . . ? N19 Ti4 N20 C149 6.1(5) . . . . ? N22 Ti4 N20 C149 -84.5(5) . . . . ? N21 Ti4 N20 C149 -160.0(5) . . . . ? N24 Ti4 N21 C168 167.4(6) . . . . ? N23 Ti4 N21 C168 -91.7(6) . . . . ? N19 Ti4 N21 C168 39.9(10) . . . . ? N20 Ti4 N21 C168 77.4(6) . . . . ? N22 Ti4 N21 C168 -3.6(6) . . . . ? N24 Ti4 N21 C161 -10.7(7) . . . . ? N23 Ti4 N21 C161 90.2(7) . . . . ? N19 Ti4 N21 C161 -138.2(7) . . . . ? N20 Ti4 N21 C161 -100.8(7) . . . . ? N22 Ti4 N21 C161 178.2(7) . . . . ? N24 Ti4 N22 C169 -46.5(17) . . . . ? N23 Ti4 N22 C169 102.5(6) . . . . ? N19 Ti4 N22 C169 -160.3(6) . . . . ? N20 Ti4 N22 C169 -85.0(6) . . . . ? N21 Ti4 N22 C169 4.3(5) . . . . ? N24 Ti4 N22 C172 127.9(14) . . . . ? N23 Ti4 N22 C172 -83.1(9) . . . . ? N19 Ti4 N22 C172 14.1(9) . . . . ? N20 Ti4 N22 C172 89.4(9) . . . . ? N21 Ti4 N22 C172 178.7(9) . . . . ? N24 Ti4 N23 C174 158.0(7) . . . . ? N19 Ti4 N23 C174 -104.1(7) . . . . ? N20 Ti4 N23 C174 -54.4(17) . . . . ? N22 Ti4 N23 C174 -16.0(7) . . . . ? N21 Ti4 N23 C174 59.1(7) . . . . ? N24 Ti4 N23 C173 -32.7(7) . . . . ? N19 Ti4 N23 C173 65.1(7) . . . . ? N20 Ti4 N23 C173 114.9(14) . . . . ? N22 Ti4 N23 C173 153.2(7) . . . . ? N21 Ti4 N23 C173 -131.7(7) . . . . ? N23 Ti4 N24 C176 154.7(7) . . . . ? N19 Ti4 N24 C176 56.2(7) . . . . ? N20 Ti4 N24 C176 -18.9(7) . . . . ? N22 Ti4 N24 C176 -56.8(18) . . . . ? N21 Ti4 N24 C176 -105.9(7) . . . . ? N23 Ti4 N24 C175 -35.1(7) . . . . ? N19 Ti4 N24 C175 -133.5(6) . . . . ? N20 Ti4 N24 C175 151.3(6) . . . . ? N22 Ti4 N24 C175 113.4(14) . . . . ? N21 Ti4 N24 C175 64.3(6) . . . . ? C15 O1 C2 C3 -14.5(13) . . . . ? C15 O1 C2 C1 161.9(8) . . . . ? C6 C1 C2 O1 177.6(7) . . . . ? C8 C1 C2 O1 0.4(11) . . . . ? C6 C1 C2 C3 -5.9(12) . . . . ? C8 C1 C2 C3 176.9(7) . . . . ? O1 C2 C3 C4 -177.5(8) . . . . ? C1 C2 C3 C4 6.2(13) . . . . ? C2 C3 C4 C5 -3.4(13) . . . . ? C3 C4 C5 C6 0.2(13) . . . . ? C4 C5 C6 C1 0.1(12) . . . . ? C4 C5 C6 C7 178.8(8) . . . . ? C2 C1 C6 C5 2.8(11) . . . . ? C8 C1 C6 C5 179.8(7) . . . . ? C2 C1 C6 C7 -176.0(7) . . . . ? C8 C1 C6 C7 1.1(11) . . . . ? C6 C1 C8 C9 89.5(10) . . . . ? C2 C1 C8 C9 -93.4(10) . . . . ? C6 C1 C8 C13 -86.3(10) . . . . ? C2 C1 C8 C13 90.8(9) . . . . ? C13 C8 C9 C10 3.6(12) . . . . ? C1 C8 C9 C10 -172.1(7) . . . . ? C13 C8 C9 N1 -179.9(7) . . . . ? C1 C8 C9 N1 4.3(12) . . . . ? C16 N1 C9 C8 66.9(9) . . . . ? Ti1 N1 C9 C8 -121.7(8) . . . . ? C16 N1 C9 C10 -116.5(8) . . . . ? Ti1 N1 C9 C10 54.9(10) . . . . ? C8 C9 C10 C11 -5.1(12) . . . . ? N1 C9 C10 C11 178.3(7) . . . . ? C9 C10 C11 C12 3.8(13) . . . . ? C10 C11 C12 C13 -1.1(13) . . . . ? C9 C8 C13 C12 -0.9(13) . . . . ? C1 C8 C13 C12 175.1(8) . . . . ? C9 C8 C13 C14 -180.0(8) . . . . ? C1 C8 C13 C14 -4.0(12) . . . . ? C11 C12 C13 C8 -0.4(13) . . . . ? C11 C12 C13 C14 178.8(8) . . . . ? C9 N1 C16 C17 -179.9(6) . . . . ? Ti1 N1 C16 C17 7.3(8) . . . . ? C20 N2 C17 C18 1.7(8) . . . . ? Ti1 N2 C17 C18 168.7(5) . . . . ? C20 N2 C17 C16 -179.2(7) . . . . ? Ti1 N2 C17 C16 -12.2(8) . . . . ? N1 C16 C17 C18 -177.6(8) . . . . ? N1 C16 C17 N2 3.5(10) . . . . ? N2 C17 C18 C19 0.6(9) . . . . ? C16 C17 C18 C19 -178.3(8) . . . . ? C17 C18 C19 C20 -2.7(9) . . . . ? C17 N2 C20 C19 -3.5(9) . . . . ? Ti1 N2 C20 C19 -164.1(7) . . . . ? C18 C19 C20 N2 4.0(10) . . . . ? C35 O2 C22 C23 9.3(13) . . . . ? C35 O2 C22 C21 -173.2(8) . . . . ? C26 C21 C22 O2 -179.1(7) . . . . ? C28 C21 C22 O2 2.8(11) . . . . ? C26 C21 C22 C23 -1.5(12) . . . . ? C28 C21 C22 C23 -179.6(8) . . . . ? O2 C22 C23 C24 176.7(8) . . . . ? C21 C22 C23 C24 -0.7(14) . . . . ? C22 C23 C24 C25 1.6(14) . . . . ? C23 C24 C25 C26 -0.4(14) . . . . ? C22 C21 C26 C25 2.7(12) . . . . ? C28 C21 C26 C25 -179.4(8) . . . . ? C22 C21 C26 C27 -174.9(8) . . . . ? C28 C21 C26 C27 3.1(12) . . . . ? C24 C25 C26 C21 -1.9(13) . . . . ? C24 C25 C26 C27 175.7(8) . . . . ? C26 C21 C28 C29 79.3(10) . . . . ? C22 C21 C28 C29 -102.7(9) . . . . ? C26 C21 C28 C33 -99.7(10) . . . . ? C22 C21 C28 C33 78.2(10) . . . . ? C33 C28 C29 N3 -175.2(7) . . . . ? C21 C28 C29 N3 5.8(11) . . . . ? C33 C28 C29 C30 0.0(11) . . . . ? C21 C28 C29 C30 -179.0(7) . . . . ? C36 N3 C29 C28 51.6(11) . . . . ? Ti1 N3 C29 C28 -129.1(7) . . . . ? C36 N3 C29 C30 -123.9(8) . . . . ? Ti1 N3 C29 C30 55.5(9) . . . . ? C28 C29 C30 C31 3.0(12) . . . . ? N3 C29 C30 C31 178.6(7) . . . . ? C29 C30 C31 C32 -4.1(13) . . . . ? C30 C31 C32 C33 2.1(13) . . . . ? C31 C32 C33 C28 1.1(12) . . . . ? C31 C32 C33 C34 -179.1(8) . . . . ? C29 C28 C33 C32 -2.1(12) . . . . ? C21 C28 C33 C32 176.9(7) . . . . ? C29 C28 C33 C34 178.1(7) . . . . ? C21 C28 C33 C34 -2.9(11) . . . . ? C29 N3 C36 C37 -177.2(8) . . . . ? Ti1 N3 C36 C37 3.4(11) . . . . ? N3 C36 C37 N4 -0.2(14) . . . . ? N3 C36 C37 C38 175.5(9) . . . . ? C40 N4 C37 C36 178.0(8) . . . . ? Ti1 N4 C37 C36 -3.1(10) . . . . ? C40 N4 C37 C38 1.2(10) . . . . ? Ti1 N4 C37 C38 180.0(6) . . . . ? C36 C37 C38 C39 -178.3(11) . . . . ? N4 C37 C38 C39 -2.3(10) . . . . ? C37 C38 C39 C40 2.5(10) . . . . ? C37 N4 C40 C39 0.4(10) . . . . ? Ti1 N4 C40 C39 -177.9(7) . . . . ? C38 C39 C40 N4 -1.8(10) . . . . ? C59 O3 C46 C47 1.7(14) . . . . ? C59 O3 C46 C45 -178.6(9) . . . . ? C50 C45 C46 C47 -2.2(13) . . . . ? C52 C45 C46 C47 -179.7(8) . . . . ? C50 C45 C46 O3 178.1(7) . . . . ? C52 C45 C46 O3 0.5(11) . . . . ? O3 C46 C47 C48 178.5(9) . . . . ? C45 C46 C47 C48 -1.2(14) . . . . ? C46 C47 C48 C49 4.7(15) . . . . ? C47 C48 C49 C50 -4.7(14) . . . . ? C46 C45 C50 C49 2.0(12) . . . . ? C52 C45 C50 C49 179.5(7) . . . . ? C46 C45 C50 C51 -176.7(8) . . . . ? C52 C45 C50 C51 0.7(12) . . . . ? C48 C49 C50 C45 1.4(12) . . . . ? C48 C49 C50 C51 -179.8(8) . . . . ? C50 C45 C52 C57 -91.2(11) . . . . ? C46 C45 C52 C57 86.3(11) . . . . ? C50 C45 C52 C53 87.3(10) . . . . ? C46 C45 C52 C53 -95.2(10) . . . . ? C57 C52 C53 C54 3.4(12) . . . . ? C45 C52 C53 C54 -175.2(8) . . . . ? C57 C52 C53 N7 178.2(8) . . . . ? C45 C52 C53 N7 -0.4(12) . . . . ? C60 N7 C53 C54 -124.3(8) . . . . ? Ti2 N7 C53 C54 52.1(10) . . . . ? C60 N7 C53 C52 60.8(10) . . . . ? Ti2 N7 C53 C52 -122.8(8) . . . . ? C52 C53 C54 C55 -4.8(13) . . . . ? N7 C53 C54 C55 -179.9(8) . . . . ? C53 C54 C55 C56 3.5(14) . . . . ? C54 C55 C56 C57 -0.8(14) . . . . ? C53 C52 C57 C56 -0.8(14) . . . . ? C45 C52 C57 C56 177.8(8) . . . . ? C53 C52 C57 C58 178.1(8) . . . . ? C45 C52 C57 C58 -3.3(13) . . . . ? C55 C56 C57 C52 -0.5(15) . . . . ? C55 C56 C57 C58 -179.4(9) . . . . ? C53 N7 C60 C61 -178.8(7) . . . . ? Ti2 N7 C60 C61 4.4(10) . . . . ? C64 N8 C61 C62 -3.4(9) . . . . ? Ti2 N8 C61 C62 173.2(6) . . . . ? C64 N8 C61 C60 -178.1(7) . . . . ? Ti2 N8 C61 C60 -1.5(9) . . . . ? N7 C60 C61 C62 -175.4(8) . . . . ? N7 C60 C61 N8 -1.9(11) . . . . ? N8 C61 C62 C63 4.5(10) . . . . ? C60 C61 C62 C63 178.3(9) . . . . ? C61 C62 C63 C64 -3.6(10) . . . . ? C61 N8 C64 C63 1.0(10) . . . . ? Ti2 N8 C64 C63 -173.7(7) . . . . ? C62 C63 C64 N8 1.7(11) . . . . ? C70 C65 C66 O4 174.5(7) . . . . ? C72 C65 C66 O4 -4.8(11) . . . . ? C70 C65 C66 C67 -1.0(13) . . . . ? C72 C65 C66 C67 179.8(8) . . . . ? C79 O4 C66 C65 165.2(8) . . . . ? C79 O4 C66 C67 -19.4(12) . . . . ? C65 C66 C67 C68 -0.1(13) . . . . ? O4 C66 C67 C68 -175.0(8) . . . . ? C66 C67 C68 C69 1.9(14) . . . . ? C67 C68 C69 C70 -2.7(15) . . . . ? C66 C65 C70 C69 0.1(13) . . . . ? C72 C65 C70 C69 179.4(8) . . . . ? C66 C65 C70 C71 -179.8(8) . . . . ? C72 C65 C70 C71 -0.5(13) . . . . ? C68 C69 C70 C65 1.7(14) . . . . ? C68 C69 C70 C71 -178.4(9) . . . . ? C70 C65 C72 C73 93.2(11) . . . . ? C66 C65 C72 C73 -87.5(11) . . . . ? C70 C65 C72 C77 -84.8(10) . . . . ? C66 C65 C72 C77 94.5(10) . . . . ? C77 C72 C73 N9 -178.3(7) . . . . ? C65 C72 C73 N9 3.7(13) . . . . ? C77 C72 C73 C74 -1.6(12) . . . . ? C65 C72 C73 C74 -179.6(8) . . . . ? C80 N9 C73 C72 62.8(10) . . . . ? Ti2 N9 C73 C72 -119.6(7) . . . . ? C80 N9 C73 C74 -113.9(9) . . . . ? Ti2 N9 C73 C74 63.6(9) . . . . ? C72 C73 C74 C75 4.2(12) . . . . ? N9 C73 C74 C75 -179.0(7) . . . . ? C73 C74 C75 C76 -6.1(13) . . . . ? C74 C75 C76 C77 5.4(14) . . . . ? C75 C76 C77 C72 -2.7(13) . . . . ? C75 C76 C77 C78 179.9(9) . . . . ? C73 C72 C77 C76 0.8(12) . . . . ? C65 C72 C77 C76 178.9(8) . . . . ? C73 C72 C77 C78 178.3(8) . . . . ? C65 C72 C77 C78 -3.6(12) . . . . ? C73 N9 C80 C81 -179.9(7) . . . . ? Ti2 N9 C80 C81 2.2(9) . . . . ? C84 N10 C81 C80 177.5(7) . . . . ? Ti2 N10 C81 C80 -6.0(9) . . . . ? C84 N10 C81 C82 0.8(9) . . . . ? Ti2 N10 C81 C82 177.3(5) . . . . ? N9 C80 C81 N10 2.7(11) . . . . ? N9 C80 C81 C82 178.4(9) . . . . ? N10 C81 C82 C83 -1.8(10) . . . . ? C80 C81 C82 C83 -177.8(9) . . . . ? C81 C82 C83 C84 2.1(10) . . . . ? C81 N10 C84 C83 0.6(9) . . . . ? Ti2 N10 C84 C83 -174.2(7) . . . . ? C82 C83 C84 N10 -1.7(10) . . . . ? C103 O5 C90 C89 175.8(8) . . . . ? C103 O5 C90 C91 -6.7(13) . . . . ? C94 C89 C90 O5 174.5(7) . . . . ? C96 C89 C90 O5 0.3(11) . . . . ? C94 C89 C90 C91 -3.3(12) . . . . ? C96 C89 C90 C91 -177.5(8) . . . . ? O5 C90 C91 C92 -177.8(8) . . . . ? C89 C90 C91 C92 -0.4(13) . . . . ? C90 C91 C92 C93 4.1(14) . . . . ? C91 C92 C93 C94 -4.2(13) . . . . ? C90 C89 C94 C93 3.2(12) . . . . ? C96 C89 C94 C93 177.7(7) . . . . ? C90 C89 C94 C95 -177.4(8) . . . . ? C96 C89 C94 C95 -2.9(12) . . . . ? C92 C93 C94 C89 0.4(12) . . . . ? C92 C93 C94 C95 -179.1(8) . . . . ? C94 C89 C96 C101 -90.2(10) . . . . ? C90 C89 C96 C101 84.3(11) . . . . ? C94 C89 C96 C97 91.7(10) . . . . ? C90 C89 C96 C97 -93.8(10) . . . . ? C101 C96 C97 C98 2.3(12) . . . . ? C89 C96 C97 C98 -179.6(8) . . . . ? C101 C96 C97 N13 -176.0(7) . . . . ? C89 C96 C97 N13 2.2(13) . . . . ? C104 N13 C97 C98 -115.8(8) . . . . ? Ti3 N13 C97 C98 61.7(10) . . . . ? C104 N13 C97 C96 62.5(11) . . . . ? Ti3 N13 C97 C96 -120.0(8) . . . . ? C96 C97 C98 C99 1.3(13) . . . . ? N13 C97 C98 C99 179.7(8) . . . . ? C97 C98 C99 C100 -4.0(13) . . . . ? C98 C99 C100 C101 3.0(14) . . . . ? C99 C100 C101 C96 0.7(14) . . . . ? C99 C100 C101 C102 178.4(8) . . . . ? C97 C96 C101 C100 -3.3(13) . . . . ? C89 C96 C101 C100 178.5(8) . . . . ? C97 C96 C101 C102 179.0(8) . . . . ? C89 C96 C101 C102 0.8(12) . . . . ? C97 N13 C104 C105 -179.4(7) . . . . ? Ti3 N13 C104 C105 2.6(9) . . . . ? C108 N14 C105 C106 -1.4(9) . . . . ? Ti3 N14 C105 C106 172.4(6) . . . . ? C108 N14 C105 C104 177.6(7) . . . . ? Ti3 N14 C105 C104 -8.6(9) . . . . ? N13 C104 C105 N14 4.1(11) . . . . ? N13 C104 C105 C106 -177.2(9) . . . . ? N14 C105 C106 C107 -0.3(10) . . . . ? C104 C105 C106 C107 -179.1(8) . . . . ? C105 C106 C107 C108 1.8(10) . . . . ? C105 N14 C108 C107 2.6(9) . . . . ? Ti3 N14 C108 C107 -168.2(7) . . . . ? C106 C107 C108 N14 -2.7(10) . . . . ? C123 O6 C110 C111 3.8(14) . . . . ? C123 O6 C110 C109 179.0(10) . . . . ? C114 C109 C110 C111 -4.5(13) . . . . ? C116 C109 C110 C111 175.5(8) . . . . ? C114 C109 C110 O6 -179.8(7) . . . . ? C116 C109 C110 O6 0.2(12) . . . . ? O6 C110 C111 C112 177.1(8) . . . . ? C109 C110 C111 C112 2.3(13) . . . . ? C110 C111 C112 C113 -0.6(13) . . . . ? C111 C112 C113 C114 1.3(14) . . . . ? C112 C113 C114 C109 -3.6(14) . . . . ? C112 C113 C114 C115 179.4(9) . . . . ? C110 C109 C114 C113 5.1(13) . . . . ? C116 C109 C114 C113 -175.0(8) . . . . ? C110 C109 C114 C115 -177.9(9) . . . . ? C116 C109 C114 C115 2.1(12) . . . . ? C114 C109 C116 C121 -97.6(11) . . . . ? C110 C109 C116 C121 82.3(12) . . . . ? C114 C109 C116 C117 85.8(11) . . . . ? C110 C109 C116 C117 -94.2(11) . . . . ? C124 N15 C117 C118 -128.7(9) . . . . ? Ti3 N15 C117 C118 47.6(12) . . . . ? C124 N15 C117 C116 60.9(12) . . . . ? Ti3 N15 C117 C116 -122.8(9) . . . . ? C121 C116 C117 C118 7.8(13) . . . . ? C109 C116 C117 C118 -175.6(9) . . . . ? C121 C116 C117 N15 178.4(9) . . . . ? C109 C116 C117 N15 -5.0(14) . . . . ? N15 C117 C118 C119 178.9(9) . . . . ? C116 C117 C118 C119 -10.2(14) . . . . ? C117 C118 C119 C120 6.7(16) . . . . ? C118 C119 C120 C121 -0.4(16) . . . . ? C119 C120 C121 C116 -1.7(17) . . . . ? C119 C120 C121 C122 -177.9(11) . . . . ? C117 C116 C121 C120 -2.0(16) . . . . ? C109 C116 C121 C120 -178.6(10) . . . . ? C117 C116 C121 C122 174.1(10) . . . . ? C109 C116 C121 C122 -2.5(16) . . . . ? C117 N15 C124 C125 -179.1(7) . . . . ? Ti3 N15 C124 C125 4.0(10) . . . . ? C128 N16 C125 C126 -1.5(9) . . . . ? Ti3 N16 C125 C126 175.2(5) . . . . ? C128 N16 C125 C124 -179.3(7) . . . . ? Ti3 N16 C125 C124 -2.5(9) . . . . ? N15 C124 C125 N16 -1.0(12) . . . . ? N15 C124 C125 C126 -178.3(8) . . . . ? N16 C125 C126 C127 2.8(10) . . . . ? C124 C125 C126 C127 -179.8(8) . . . . ? C125 C126 C127 C128 -2.8(9) . . . . ? C125 N16 C128 C127 -0.3(9) . . . . ? Ti3 N16 C128 C127 -175.5(7) . . . . ? C126 C127 C128 N16 2.1(10) . . . . ? C147 O7 C134 C135 -12.6(13) . . . . ? C147 O7 C134 C133 165.9(8) . . . . ? C138 C133 C134 O7 177.3(7) . . . . ? C140 C133 C134 O7 2.1(12) . . . . ? C138 C133 C134 C135 -4.0(13) . . . . ? C140 C133 C134 C135 -179.2(8) . . . . ? O7 C134 C135 C136 179.9(9) . . . . ? C133 C134 C135 C136 1.4(14) . . . . ? C134 C135 C136 C137 2.6(15) . . . . ? C135 C136 C137 C138 -4.0(15) . . . . ? C136 C137 C138 C133 1.3(13) . . . . ? C136 C137 C138 C139 179.2(9) . . . . ? C134 C133 C138 C137 2.7(12) . . . . ? C140 C133 C138 C137 177.7(8) . . . . ? C134 C133 C138 C139 -175.2(8) . . . . ? C140 C133 C138 C139 -0.2(12) . . . . ? C134 C133 C140 C145 90.3(10) . . . . ? C138 C133 C140 C145 -84.9(10) . . . . ? C134 C133 C140 C141 -94.2(10) . . . . ? C138 C133 C140 C141 90.7(11) . . . . ? C145 C140 C141 C142 2.2(12) . . . . ? C133 C140 C141 C142 -173.4(8) . . . . ? C145 C140 C141 N19 178.5(7) . . . . ? C133 C140 C141 N19 2.9(12) . . . . ? C148 N19 C141 C142 -118.2(9) . . . . ? Ti4 N19 C141 C142 55.1(9) . . . . ? C148 N19 C141 C140 65.4(9) . . . . ? Ti4 N19 C141 C140 -121.3(7) . . . . ? C140 C141 C142 C143 -4.6(13) . . . . ? N19 C141 C142 C143 179.1(7) . . . . ? C141 C142 C143 C144 5.5(13) . . . . ? C142 C143 C144 C145 -4.1(14) . . . . ? C141 C140 C145 C144 -0.8(12) . . . . ? C133 C140 C145 C144 175.1(8) . . . . ? C141 C140 C145 C146 -179.7(8) . . . . ? C133 C140 C145 C146 -3.9(12) . . . . ? C143 C144 C145 C140 1.8(14) . . . . ? C143 C144 C145 C146 -179.3(9) . . . . ? C141 N19 C148 C149 179.4(7) . . . . ? Ti4 N19 C148 C149 5.3(9) . . . . ? N19 C148 C149 N20 0.3(10) . . . . ? N19 C148 C149 C150 -179.6(7) . . . . ? C152 N20 C149 C148 -179.3(7) . . . . ? Ti4 N20 C149 C148 -5.6(8) . . . . ? C152 N20 C149 C150 0.6(8) . . . . ? Ti4 N20 C149 C150 174.3(5) . . . . ? C148 C149 C150 C151 -177.9(8) . . . . ? N20 C149 C150 C151 2.2(8) . . . . ? C149 C150 C151 C152 -4.1(9) . . . . ? C149 N20 C152 C151 -3.4(9) . . . . ? Ti4 N20 C152 C151 -173.9(7) . . . . ? C150 C151 C152 N20 4.9(10) . . . . ? C167 O8 C154 C153 -176.2(8) . . . . ? C167 O8 C154 C155 4.3(13) . . . . ? C158 C153 C154 O8 178.3(7) . . . . ? C160 C153 C154 O8 0.4(11) . . . . ? C158 C153 C154 C155 -2.1(12) . . . . ? C160 C153 C154 C155 -180.0(7) . . . . ? O8 C154 C155 C156 178.7(8) . . . . ? C153 C154 C155 C156 -0.8(12) . . . . ? C154 C155 C156 C157 2.3(13) . . . . ? C155 C156 C157 C158 -0.9(14) . . . . ? C156 C157 C158 C153 -2.1(12) . . . . ? C156 C157 C158 C159 178.0(8) . . . . ? C154 C153 C158 C157 3.5(12) . . . . ? C160 C153 C158 C157 -178.7(8) . . . . ? C154 C153 C158 C159 -176.6(7) . . . . ? C160 C153 C158 C159 1.2(12) . . . . ? C158 C153 C160 C161 82.5(10) . . . . ? C154 C153 C160 C161 -99.7(9) . . . . ? C158 C153 C160 C165 -94.3(10) . . . . ? C154 C153 C160 C165 83.5(10) . . . . ? C165 C160 C161 C162 -1.8(12) . . . . ? C153 C160 C161 C162 -178.7(7) . . . . ? C165 C160 C161 N21 -176.5(7) . . . . ? C153 C160 C161 N21 6.6(11) . . . . ? C168 N21 C161 C160 53.9(11) . . . . ? Ti4 N21 C161 C160 -128.1(7) . . . . ? C168 N21 C161 C162 -121.2(8) . . . . ? Ti4 N21 C161 C162 56.8(9) . . . . ? C160 C161 C162 C163 2.8(12) . . . . ? N21 C161 C162 C163 177.8(7) . . . . ? C161 C162 C163 C164 -2.6(12) . . . . ? C162 C163 C164 C165 1.5(14) . . . . ? C163 C164 C165 C160 -0.4(14) . . . . ? C163 C164 C165 C166 -179.6(8) . . . . ? C161 C160 C165 C164 0.5(12) . . . . ? C153 C160 C165 C164 177.4(8) . . . . ? C161 C160 C165 C166 179.7(8) . . . . ? C153 C160 C165 C166 -3.4(13) . . . . ? C161 N21 C168 C169 -179.3(8) . . . . ? Ti4 N21 C168 C169 2.5(10) . . . . ? N21 C168 C169 N22 1.5(13) . . . . ? N21 C168 C169 C170 179.2(9) . . . . ? C172 N22 C169 C168 179.0(8) . . . . ? Ti4 N22 C169 C168 -4.7(9) . . . . ? C172 N22 C169 C170 0.8(9) . . . . ? Ti4 N22 C169 C170 177.1(6) . . . . ? C168 C169 C170 C171 -178.5(10) . . . . ? N22 C169 C170 C171 -0.7(10) . . . . ? C169 C170 C171 C172 0.3(11) . . . . ? C169 N22 C172 C171 -0.6(9) . . . . ? Ti4 N22 C172 C171 -175.2(7) . . . . ? C170 C171 C172 N22 0.1(11) . . . . ? C182 C177 C178 C179 0.0 . . . . ? C177 C178 C179 C180 0.0 . . . . ? C178 C179 C180 C181 0.0 . . . . ? C179 C180 C181 C182 0.0 . . . . ? C180 C181 C182 C177 0.0 . . . . ? C178 C177 C182 C181 0.0 . . . . ? C188 C183 C184 C185 0.0 . . . . ? C183 C184 C185 C186 0.0 . . . . ? C184 C185 C186 C187 0.0 . . . . ? C185 C186 C187 C188 0.0 . . . . ? C184 C183 C188 C187 0.0 . . . . ? C186 C187 C188 C183 0.0 . . . . ? C194 C189 C190 C191 0.0 . . . . ? C189 C190 C191 C192 0.0 . . . . ? C190 C191 C192 C193 0.0 . . . . ? C191 C192 C193 C194 0.0 . . . . ? C192 C193 C194 C189 0.0 . . . . ? C190 C189 C194 C193 0.0 . . . . ? C200 C195 C196 C197 0.0 . . . . ? C195 C196 C197 C198 0.0 . . . . ? C196 C197 C198 C199 0.0 . . . . ? C197 C198 C199 C200 0.0 . . . . ? C198 C199 C200 C195 0.0 . . . . ? C196 C195 C200 C199 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.475 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.063 # Attachment 'compound_15.cif' data_15 _database_code_depnum_ccdc_archive 'CCDC 687854' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H56 N6 O2 Zr' _chemical_formula_sum 'C50 H56 N6 O2 Zr' _chemical_formula_weight 864.23 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 11.6280(9) _cell_length_b 19.8068(15) _cell_length_c 20.0566(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4619.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 14108 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9457 _exptl_absorpt_correction_T_max 0.9615 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 55738 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.87 _reflns_number_total 10997 _reflns_number_gt 10575 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+1.8239P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 10997 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.469779(17) 0.408058(9) 0.473529(10) 0.02285(5) Uani 1 1 d . . . O1 O 0.51538(18) 0.55412(9) 0.74026(8) 0.0424(4) Uani 1 1 d . . . O2 O 0.23118(15) 0.25183(10) 0.25535(9) 0.0426(4) Uani 1 1 d . . . N1 N 0.46338(18) 0.47721(8) 0.56613(9) 0.0260(4) Uani 1 1 d . . . N2 N 0.42003(17) 0.34199(9) 0.56483(10) 0.0257(4) Uani 1 1 d . . . N3 N 0.39734(16) 0.32544(9) 0.40415(9) 0.0244(4) Uani 1 1 d . . . N4 N 0.27241(15) 0.42019(9) 0.47156(10) 0.0271(4) Uani 1 1 d . . . N5 N 0.49104(18) 0.48563(9) 0.40600(10) 0.0318(4) Uani 1 1 d . . . N6 N 0.63590(16) 0.37078(9) 0.47992(10) 0.0290(4) Uani 1 1 d . . . C1 C 0.6439(2) 0.52634(11) 0.65566(13) 0.0313(5) Uani 1 1 d . . . C2 C 0.6099(2) 0.51667(12) 0.72187(13) 0.0352(5) Uani 1 1 d . . . C3 C 0.6650(3) 0.47124(13) 0.76298(14) 0.0439(6) Uani 1 1 d . . . H3 H 0.6404 0.4652 0.8078 0.053 Uiso 1 1 calc R . . C4 C 0.7569(3) 0.43442(14) 0.73810(17) 0.0485(7) Uani 1 1 d . . . H4 H 0.7940 0.4020 0.7656 0.058 Uiso 1 1 calc R . . C5 C 0.7946(2) 0.44460(13) 0.67364(16) 0.0452(7) Uani 1 1 d . . . H5 H 0.8586 0.4197 0.6574 0.054 Uiso 1 1 calc R . . C6 C 0.7397(2) 0.49119(13) 0.63199(14) 0.0365(5) Uani 1 1 d . . . C7 C 0.7840(2) 0.50201(16) 0.56222(16) 0.0488(7) Uani 1 1 d . . . H7A H 0.7462 0.4702 0.5318 0.073 Uiso 1 1 calc R . . H7B H 0.8672 0.4945 0.5613 0.073 Uiso 1 1 calc R . . H7C H 0.7672 0.5483 0.5481 0.073 Uiso 1 1 calc R . . C8 C 0.4906(2) 0.54783(10) 0.56869(11) 0.0274(5) Uani 1 1 d . . . C9 C 0.5761(2) 0.57297(10) 0.61130(12) 0.0290(5) Uani 1 1 d . . . C10 C 0.43098(19) 0.59044(11) 0.52595(12) 0.0317(4) Uani 1 1 d . . . H10 H 0.3742 0.5726 0.4968 0.038 Uiso 1 1 calc R . . C11 C 0.4543(2) 0.65902(11) 0.52581(14) 0.0392(5) Uani 1 1 d . . . H11 H 0.4138 0.6883 0.4965 0.047 Uiso 1 1 calc R . . C12 C 0.5366(3) 0.68469(11) 0.56837(14) 0.0427(6) Uani 1 1 d . . . H12 H 0.5515 0.7319 0.5684 0.051 Uiso 1 1 calc R . . C13 C 0.5983(2) 0.64308(12) 0.61124(13) 0.0371(5) Uani 1 1 d . . . C14 C 0.6881(3) 0.67166(14) 0.65770(17) 0.0539(8) Uani 1 1 d . . . H14A H 0.6927 0.7207 0.6517 0.081 Uiso 1 1 calc R . . H14B H 0.7629 0.6513 0.6477 0.081 Uiso 1 1 calc R . . H14C H 0.6669 0.6615 0.7039 0.081 Uiso 1 1 calc R . . C15 C 0.4716(4) 0.5445(2) 0.80522(16) 0.0882(15) Uani 1 1 d . . . H15A H 0.5326 0.5528 0.8379 0.132 Uiso 1 1 calc R . . H15B H 0.4438 0.4980 0.8099 0.132 Uiso 1 1 calc R . . H15C H 0.4079 0.5759 0.8130 0.132 Uiso 1 1 calc R . . C16 C 0.43375(19) 0.44757(11) 0.62188(12) 0.0264(5) Uani 1 1 d . . . H16 H 0.4282 0.4734 0.6617 0.032 Uiso 1 1 calc R . . C17 C 0.4101(2) 0.37796(11) 0.62365(11) 0.0267(4) Uani 1 1 d . . . C18 C 0.3791(2) 0.33528(13) 0.67614(12) 0.0335(5) Uani 1 1 d . . . H18 H 0.3669 0.3476 0.7214 0.040 Uiso 1 1 calc R . . C19 C 0.3697(2) 0.27144(13) 0.64865(12) 0.0358(5) Uani 1 1 d . . . H19 H 0.3501 0.2310 0.6715 0.043 Uiso 1 1 calc R . . C20 C 0.3946(2) 0.27779(11) 0.58093(12) 0.0303(5) Uani 1 1 d . . . H20 H 0.3937 0.2414 0.5501 0.036 Uiso 1 1 calc R . . C21 C 0.3918(2) 0.32258(12) 0.25600(11) 0.0288(5) Uani 1 1 d . . . C22 C 0.2792(2) 0.31137(13) 0.23416(12) 0.0355(5) Uani 1 1 d . . . C23 C 0.2238(3) 0.35789(17) 0.19288(14) 0.0476(7) Uani 1 1 d . . . H23 H 0.1470 0.3503 0.1786 0.057 Uiso 1 1 calc R . . C24 C 0.2828(3) 0.41508(16) 0.17325(13) 0.0496(7) Uani 1 1 d . . . H24 H 0.2456 0.4470 0.1452 0.060 Uiso 1 1 calc R . . C25 C 0.3938(3) 0.42687(14) 0.19336(13) 0.0432(6) Uani 1 1 d . . . H25 H 0.4327 0.4665 0.1790 0.052 Uiso 1 1 calc R . . C26 C 0.4499(2) 0.38052(12) 0.23516(11) 0.0323(5) Uani 1 1 d . . . C27 C 0.5705(2) 0.39486(13) 0.25763(14) 0.0383(6) Uani 1 1 d . . . H27A H 0.6145 0.3527 0.2587 0.057 Uiso 1 1 calc R . . H27B H 0.5689 0.4148 0.3024 0.057 Uiso 1 1 calc R . . H27C H 0.6069 0.4265 0.2266 0.057 Uiso 1 1 calc R . . C28 C 0.45294(19) 0.27024(11) 0.29748(11) 0.0259(4) Uani 1 1 d . . . C29 C 0.4590(2) 0.27448(10) 0.36702(11) 0.0259(4) Uani 1 1 d . . . C30 C 0.5250(2) 0.22857(10) 0.40303(11) 0.0295(4) Uani 1 1 d . . . H30 H 0.5306 0.2326 0.4501 0.035 Uiso 1 1 calc R . . C31 C 0.5825(2) 0.17711(12) 0.37041(13) 0.0363(5) Uani 1 1 d . . . H31 H 0.6282 0.1461 0.3950 0.044 Uiso 1 1 calc R . . C32 C 0.5732(2) 0.17094(12) 0.30209(14) 0.0363(5) Uani 1 1 d . . . H32 H 0.6105 0.1345 0.2801 0.044 Uiso 1 1 calc R . . C33 C 0.5102(2) 0.21724(11) 0.26507(12) 0.0316(5) Uani 1 1 d . . . C34 C 0.5046(3) 0.21101(14) 0.18970(13) 0.0442(7) Uani 1 1 d . . . H34A H 0.5491 0.1716 0.1754 0.066 Uiso 1 1 calc R . . H34B H 0.5367 0.2518 0.1692 0.066 Uiso 1 1 calc R . . H34C H 0.4243 0.2056 0.1758 0.066 Uiso 1 1 calc R . . C35 C 0.1129(3) 0.2411(2) 0.2412(2) 0.0737(11) Uani 1 1 d . . . H35A H 0.1020 0.2379 0.1929 0.111 Uiso 1 1 calc R . . H35B H 0.0677 0.2789 0.2587 0.111 Uiso 1 1 calc R . . H35C H 0.0875 0.1990 0.2623 0.111 Uiso 1 1 calc R . . C36 C 0.2848(2) 0.32292(11) 0.40039(11) 0.0269(4) Uani 1 1 d . . . H36 H 0.2488 0.2892 0.3739 0.032 Uiso 1 1 calc R . . C37 C 0.2174(2) 0.36984(11) 0.43527(11) 0.0271(5) Uani 1 1 d . . . C38 C 0.0976(2) 0.37593(13) 0.44139(12) 0.0333(5) Uani 1 1 d . . . H38 H 0.0409 0.3476 0.4219 0.040 Uiso 1 1 calc R . . C39 C 0.0790(2) 0.43174(13) 0.48184(14) 0.0380(6) Uani 1 1 d . . . H39 H 0.0065 0.4493 0.4951 0.046 Uiso 1 1 calc R . . C40 C 0.1865(2) 0.45715(12) 0.49929(12) 0.0337(5) Uani 1 1 d . . . H40 H 0.1982 0.4954 0.5270 0.040 Uiso 1 1 calc R . . C41 C 0.4032(3) 0.51091(13) 0.36039(13) 0.0416(6) Uani 1 1 d . . . H41A H 0.4346 0.5129 0.3151 0.062 Uiso 1 1 calc R . . H41B H 0.3792 0.5562 0.3744 0.062 Uiso 1 1 calc R . . H41C H 0.3366 0.4806 0.3611 0.062 Uiso 1 1 calc R . . C42 C 0.5917(2) 0.52863(12) 0.40270(14) 0.0402(6) Uani 1 1 d . . . H42A H 0.5698 0.5752 0.4133 0.060 Uiso 1 1 calc R . . H42B H 0.6242 0.5269 0.3577 0.060 Uiso 1 1 calc R . . H42C H 0.6491 0.5129 0.4349 0.060 Uiso 1 1 calc R . . C43 C 0.7158(2) 0.37480(14) 0.42407(14) 0.0379(6) Uani 1 1 d . . . H43A H 0.7266 0.3297 0.4049 0.057 Uiso 1 1 calc R . . H43B H 0.7900 0.3921 0.4398 0.057 Uiso 1 1 calc R . . H43C H 0.6847 0.4052 0.3900 0.057 Uiso 1 1 calc R . . C44 C 0.6857(2) 0.32834(13) 0.53178(14) 0.0373(5) Uani 1 1 d . . . H44A H 0.7621 0.3454 0.5436 0.056 Uiso 1 1 calc R . . H44B H 0.6924 0.2819 0.5154 0.056 Uiso 1 1 calc R . . H44C H 0.6360 0.3291 0.5713 0.056 Uiso 1 1 calc R . . C45 C 0.4937(6) 0.84438(19) 0.4673(2) 0.0926(17) Uani 1 1 d . . . H45 H 0.4893 0.8348 0.4210 0.111 Uiso 1 1 calc R . . C46 C 0.5948(7) 0.8617(2) 0.4954(2) 0.110(2) Uani 1 1 d . . . H46 H 0.6612 0.8654 0.4680 0.131 Uiso 1 1 calc R . . C47 C 0.6046(6) 0.8743(2) 0.5639(3) 0.0991(17) Uani 1 1 d . . . H47 H 0.6765 0.8852 0.5836 0.119 Uiso 1 1 calc R . . C48 C 0.5063(6) 0.87017(18) 0.6011(2) 0.0916(17) Uani 1 1 d . . . H48 H 0.5113 0.8780 0.6477 0.110 Uiso 1 1 calc R . . C49 C 0.4031(6) 0.8555(2) 0.5747(3) 0.1004(17) Uani 1 1 d . . . H49 H 0.3363 0.8552 0.6020 0.120 Uiso 1 1 calc R . . C50 C 0.3952(7) 0.8408(2) 0.5075(3) 0.124(2) Uani 1 1 d . . . H50 H 0.3233 0.8282 0.4886 0.149 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02673(9) 0.01784(8) 0.02398(9) 0.00122(8) 0.00198(9) 0.00153(8) O1 0.0564(12) 0.0432(10) 0.0277(8) -0.0025(7) 0.0007(8) 0.0146(9) O2 0.0331(9) 0.0533(11) 0.0414(10) -0.0108(9) 0.0000(8) -0.0092(8) N1 0.0301(9) 0.0200(8) 0.0279(9) -0.0001(7) 0.0009(9) 0.0014(8) N2 0.0286(9) 0.0217(9) 0.0270(10) 0.0035(7) 0.0013(8) 0.0007(7) N3 0.0271(9) 0.0213(8) 0.0248(9) 0.0013(7) 0.0024(7) 0.0007(7) N4 0.0269(8) 0.0272(9) 0.0272(9) 0.0041(8) 0.0028(8) 0.0044(7) N5 0.0428(12) 0.0218(8) 0.0307(10) 0.0037(7) 0.0077(8) 0.0014(8) N6 0.0283(9) 0.0256(9) 0.0332(10) -0.0005(8) 0.0004(9) 0.0051(7) C1 0.0356(12) 0.0207(10) 0.0378(13) -0.0043(9) -0.0067(10) 0.0004(9) C2 0.0423(13) 0.0271(11) 0.0363(13) -0.0042(10) -0.0073(11) 0.0042(10) C3 0.0569(17) 0.0354(13) 0.0395(15) 0.0015(11) -0.0157(13) -0.0005(12) C4 0.0548(17) 0.0291(12) 0.0616(19) -0.0042(12) -0.0261(15) 0.0056(12) C5 0.0374(13) 0.0300(13) 0.068(2) -0.0165(13) -0.0184(13) 0.0049(10) C6 0.0317(12) 0.0293(12) 0.0486(15) -0.0103(11) -0.0065(11) -0.0027(10) C7 0.0363(14) 0.0482(16) 0.0620(19) -0.0148(14) 0.0066(13) 0.0009(12) C8 0.0351(12) 0.0207(9) 0.0263(10) -0.0008(8) 0.0056(9) 0.0042(8) C9 0.0381(12) 0.0184(10) 0.0307(12) -0.0020(8) 0.0042(10) 0.0017(8) C10 0.0425(11) 0.0231(9) 0.0295(10) 0.0005(11) -0.0003(10) 0.0061(9) C11 0.0569(15) 0.0229(10) 0.0377(12) 0.0048(10) -0.0009(14) 0.0065(10) C12 0.0608(16) 0.0176(9) 0.0496(15) 0.0024(10) 0.0008(15) -0.0027(12) C13 0.0466(14) 0.0221(11) 0.0425(14) -0.0049(10) 0.0016(12) -0.0032(10) C14 0.067(2) 0.0264(13) 0.069(2) -0.0084(13) -0.0179(17) -0.0065(13) C15 0.106(3) 0.124(4) 0.0352(16) 0.0140(19) 0.022(2) 0.060(3) C16 0.0273(11) 0.0252(10) 0.0268(11) -0.0019(9) 0.0020(8) 0.0021(8) C17 0.0268(10) 0.0279(10) 0.0253(11) 0.0017(9) 0.0001(9) -0.0004(9) C18 0.0376(13) 0.0363(13) 0.0265(12) 0.0062(10) -0.0012(10) -0.0113(10) C19 0.0416(13) 0.0314(12) 0.0344(13) 0.0121(10) -0.0037(11) -0.0120(10) C20 0.0308(11) 0.0232(10) 0.0371(13) 0.0034(9) -0.0026(10) -0.0035(9) C21 0.0324(11) 0.0307(11) 0.0233(11) -0.0029(9) 0.0008(9) 0.0037(9) C22 0.0343(12) 0.0421(14) 0.0299(12) -0.0080(10) 0.0008(10) 0.0031(11) C23 0.0431(15) 0.0659(19) 0.0338(14) -0.0114(13) -0.0089(12) 0.0179(14) C24 0.0671(19) 0.0477(17) 0.0340(13) 0.0005(13) -0.0050(13) 0.0227(15) C25 0.0621(18) 0.0389(14) 0.0287(12) 0.0031(10) 0.0047(12) 0.0111(12) C26 0.0441(14) 0.0286(10) 0.0243(11) -0.0003(9) 0.0064(10) 0.0043(10) C27 0.0411(13) 0.0313(13) 0.0423(14) 0.0037(10) 0.0075(11) -0.0056(10) C28 0.0259(10) 0.0235(9) 0.0284(11) -0.0007(8) 0.0013(9) -0.0020(8) C29 0.0263(10) 0.0195(9) 0.0319(11) -0.0014(8) 0.0025(9) -0.0017(9) C30 0.0357(11) 0.0240(9) 0.0289(11) 0.0021(8) 0.0019(10) 0.0011(10) C31 0.0406(13) 0.0227(10) 0.0456(15) 0.0043(10) 0.0037(11) 0.0056(10) C32 0.0382(12) 0.0231(11) 0.0475(15) -0.0051(10) 0.0079(11) 0.0047(9) C33 0.0339(12) 0.0252(10) 0.0356(12) -0.0042(9) 0.0043(10) -0.0033(9) C34 0.0589(19) 0.0375(13) 0.0362(13) -0.0115(11) 0.0079(12) 0.0058(12) C35 0.0328(15) 0.079(3) 0.109(3) -0.029(2) -0.0059(18) -0.0130(16) C36 0.0317(11) 0.0240(10) 0.0251(11) 0.0049(8) -0.0003(9) -0.0033(9) C37 0.0287(11) 0.0271(11) 0.0256(11) 0.0046(9) 0.0019(9) 0.0010(9) C38 0.0267(11) 0.0397(13) 0.0334(12) 0.0060(10) 0.0027(10) -0.0009(10) C39 0.0281(10) 0.0454(13) 0.0406(14) 0.0061(11) 0.0084(11) 0.0098(10) C40 0.0385(13) 0.0288(11) 0.0337(12) 0.0028(9) 0.0069(10) 0.0091(10) C41 0.0574(17) 0.0319(12) 0.0354(14) 0.0112(10) 0.0017(12) 0.0050(12) C42 0.0483(15) 0.0274(12) 0.0449(15) 0.0061(10) 0.0137(13) -0.0036(11) C43 0.0345(12) 0.0399(13) 0.0393(14) 0.0002(11) 0.0078(11) 0.0095(11) C44 0.0337(11) 0.0368(12) 0.0414(14) 0.0033(12) -0.0058(12) 0.0031(9) C45 0.172(6) 0.047(2) 0.058(2) 0.0117(18) 0.008(3) 0.001(3) C46 0.208(7) 0.057(3) 0.064(3) 0.009(2) 0.014(3) -0.049(3) C47 0.152(5) 0.053(2) 0.093(3) -0.005(2) 0.013(3) -0.054(3) C48 0.162(6) 0.0356(17) 0.078(3) -0.0047(17) 0.033(3) -0.001(2) C49 0.140(5) 0.066(3) 0.095(4) 0.001(3) -0.010(4) 0.039(3) C50 0.178(6) 0.058(3) 0.137(5) 0.027(3) -0.039(5) 0.047(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N5 2.0631(18) . ? Zr1 N6 2.0719(18) . ? Zr1 N3 2.3073(19) . ? Zr1 N4 2.3079(17) . ? Zr1 N1 2.3089(17) . ? Zr1 N2 2.3239(19) . ? O1 C2 1.377(3) . ? O1 C15 1.412(4) . ? O2 C22 1.372(3) . ? O2 C35 1.420(3) . ? N1 C16 1.309(3) . ? N1 C8 1.435(3) . ? N2 C20 1.345(3) . ? N2 C17 1.383(3) . ? N3 C36 1.312(3) . ? N3 C29 1.445(3) . ? N4 C40 1.358(3) . ? N4 C37 1.391(3) . ? N5 C42 1.449(3) . ? N5 C41 1.460(3) . ? N6 C44 1.457(3) . ? N6 C43 1.458(3) . ? C1 C6 1.396(4) . ? C1 C2 1.399(4) . ? C1 C9 1.505(3) . ? C2 C3 1.378(4) . ? C3 C4 1.386(4) . ? C3 H3 0.9500 . ? C4 C5 1.380(5) . ? C4 H4 0.9500 . ? C5 C6 1.399(4) . ? C5 H5 0.9500 . ? C6 C7 1.506(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.389(3) . ? C8 C9 1.402(3) . ? C9 C13 1.412(3) . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 C12 1.379(4) . ? C11 H11 0.9500 . ? C12 C13 1.390(4) . ? C12 H12 0.9500 . ? C13 C14 1.510(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.406(3) . ? C16 H16 0.9500 . ? C17 C18 1.398(3) . ? C18 C19 1.384(4) . ? C18 H18 0.9500 . ? C19 C20 1.394(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.396(3) . ? C21 C22 1.399(3) . ? C21 C28 1.507(3) . ? C22 C23 1.396(4) . ? C23 C24 1.381(5) . ? C23 H23 0.9500 . ? C24 C25 1.372(4) . ? C24 H24 0.9500 . ? C25 C26 1.405(4) . ? C25 H25 0.9500 . ? C26 C27 1.500(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.399(3) . ? C28 C33 1.403(3) . ? C29 C30 1.392(3) . ? C30 C31 1.383(3) . ? C30 H30 0.9500 . ? C31 C32 1.380(4) . ? C31 H31 0.9500 . ? C32 C33 1.389(4) . ? C32 H32 0.9500 . ? C33 C34 1.518(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.403(3) . ? C36 H36 0.9500 . ? C37 C38 1.403(3) . ? C38 C39 1.388(4) . ? C38 H38 0.9500 . ? C39 C40 1.392(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.348(8) . ? C45 C50 1.403(8) . ? C45 H45 0.9500 . ? C46 C47 1.400(6) . ? C46 H46 0.9500 . ? C47 C48 1.367(7) . ? C47 H47 0.9500 . ? C48 C49 1.344(8) . ? C48 H48 0.9500 . ? C49 C50 1.382(8) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Zr1 N6 101.20(8) . . ? N5 Zr1 N3 100.14(7) . . ? N6 Zr1 N3 97.18(7) . . ? N5 Zr1 N4 91.74(7) . . ? N6 Zr1 N4 164.85(7) . . ? N3 Zr1 N4 72.57(7) . . ? N5 Zr1 N1 95.17(7) . . ? N6 Zr1 N1 101.05(8) . . ? N3 Zr1 N1 153.39(7) . . ? N4 Zr1 N1 85.41(7) . . ? N5 Zr1 N2 165.13(7) . . ? N6 Zr1 N2 89.01(7) . . ? N3 Zr1 N2 89.14(7) . . ? N4 Zr1 N2 79.90(7) . . ? N1 Zr1 N2 72.07(6) . . ? C2 O1 C15 117.6(2) . . ? C22 O2 C35 117.5(3) . . ? C16 N1 C8 117.68(18) . . ? C16 N1 Zr1 115.44(14) . . ? C8 N1 Zr1 126.86(14) . . ? C20 N2 C17 105.30(19) . . ? C20 N2 Zr1 140.93(17) . . ? C17 N2 Zr1 113.76(14) . . ? C36 N3 C29 116.02(19) . . ? C36 N3 Zr1 115.20(15) . . ? C29 N3 Zr1 128.71(14) . . ? C40 N4 C37 105.22(19) . . ? C40 N4 Zr1 141.34(17) . . ? C37 N4 Zr1 113.07(14) . . ? C42 N5 C41 109.6(2) . . ? C42 N5 Zr1 124.37(17) . . ? C41 N5 Zr1 125.65(17) . . ? C44 N6 C43 109.07(19) . . ? C44 N6 Zr1 128.32(16) . . ? C43 N6 Zr1 121.83(16) . . ? C6 C1 C2 118.7(2) . . ? C6 C1 C9 121.5(2) . . ? C2 C1 C9 119.8(2) . . ? O1 C2 C3 124.2(2) . . ? O1 C2 C1 114.0(2) . . ? C3 C2 C1 121.7(3) . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.7(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 119.3(3) . . ? C1 C6 C7 121.2(2) . . ? C5 C6 C7 119.5(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 C9 121.0(2) . . ? C10 C8 N1 117.4(2) . . ? C9 C8 N1 121.63(19) . . ? C8 C9 C13 118.5(2) . . ? C8 C9 C1 120.90(19) . . ? C13 C9 C1 120.6(2) . . ? C11 C10 C8 120.0(2) . . ? C11 C10 H10 120.0 . . ? C8 C10 H10 120.0 . . ? C12 C11 C10 119.8(2) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 121.5(2) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C9 119.3(2) . . ? C12 C13 C14 121.1(2) . . ? C9 C13 C14 119.6(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C15 H15A 109.5 . . ? O1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 120.8(2) . . ? N1 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? N2 C17 C18 110.6(2) . . ? N2 C17 C16 117.9(2) . . ? C18 C17 C16 131.5(2) . . ? C19 C18 C17 105.8(2) . . ? C19 C18 H18 127.1 . . ? C17 C18 H18 127.1 . . ? C18 C19 C20 106.8(2) . . ? C18 C19 H19 126.6 . . ? C20 C19 H19 126.6 . . ? N2 C20 C19 111.4(2) . . ? N2 C20 H20 124.3 . . ? C19 C20 H20 124.3 . . ? C26 C21 C22 119.3(2) . . ? C26 C21 C28 120.2(2) . . ? C22 C21 C28 120.3(2) . . ? O2 C22 C23 124.3(3) . . ? O2 C22 C21 114.9(2) . . ? C23 C22 C21 120.9(3) . . ? C24 C23 C22 118.8(3) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C25 C24 C23 121.5(3) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 120.1(3) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 119.4(2) . . ? C21 C26 C27 121.2(2) . . ? C25 C26 C27 119.4(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 118.9(2) . . ? C29 C28 C21 122.19(19) . . ? C33 C28 C21 118.9(2) . . ? C30 C29 C28 120.4(2) . . ? C30 C29 N3 117.55(19) . . ? C28 C29 N3 122.07(19) . . ? C31 C30 C29 120.2(2) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C30 119.8(2) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 120.9(2) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C32 C33 C28 119.8(2) . . ? C32 C33 C34 120.1(2) . . ? C28 C33 C34 120.1(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O2 C35 H35A 109.5 . . ? O2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 C37 120.2(2) . . ? N3 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? N4 C37 C36 118.6(2) . . ? N4 C37 C38 110.4(2) . . ? C36 C37 C38 130.9(2) . . ? C39 C38 C37 105.9(2) . . ? C39 C38 H38 127.0 . . ? C37 C38 H38 127.0 . . ? C38 C39 C40 107.1(2) . . ? C38 C39 H39 126.4 . . ? C40 C39 H39 126.4 . . ? N4 C40 C39 111.3(2) . . ? N4 C40 H40 124.4 . . ? C39 C40 H40 124.4 . . ? N5 C41 H41A 109.5 . . ? N5 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N5 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N5 C42 H42A 109.5 . . ? N5 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N5 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N6 C43 H43A 109.5 . . ? N6 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N6 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N6 C44 H44A 109.5 . . ? N6 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N6 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 119.0(5) . . ? C46 C45 H45 120.5 . . ? C50 C45 H45 120.5 . . ? C45 C46 C47 121.8(6) . . ? C45 C46 H46 119.1 . . ? C47 C46 H46 119.1 . . ? C48 C47 C46 117.1(6) . . ? C48 C47 H47 121.4 . . ? C46 C47 H47 121.4 . . ? C49 C48 C47 123.1(5) . . ? C49 C48 H48 118.5 . . ? C47 C48 H48 118.5 . . ? C48 C49 C50 119.3(7) . . ? C48 C49 H49 120.4 . . ? C50 C49 H49 120.4 . . ? C49 C50 C45 119.7(7) . . ? C49 C50 H50 120.2 . . ? C45 C50 H50 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Zr1 N1 C16 170.71(17) . . . . ? N6 Zr1 N1 C16 -86.79(17) . . . . ? N3 Zr1 N1 C16 45.6(2) . . . . ? N4 Zr1 N1 C16 79.37(17) . . . . ? N2 Zr1 N1 C16 -1.48(17) . . . . ? N5 Zr1 N1 C8 -10.73(19) . . . . ? N6 Zr1 N1 C8 91.77(19) . . . . ? N3 Zr1 N1 C8 -135.86(18) . . . . ? N4 Zr1 N1 C8 -102.07(19) . . . . ? N2 Zr1 N1 C8 177.1(2) . . . . ? N5 Zr1 N2 C20 148.4(3) . . . . ? N6 Zr1 N2 C20 -77.8(3) . . . . ? N3 Zr1 N2 C20 19.4(3) . . . . ? N4 Zr1 N2 C20 91.8(3) . . . . ? N1 Zr1 N2 C20 -179.7(3) . . . . ? N5 Zr1 N2 C17 -30.2(4) . . . . ? N6 Zr1 N2 C17 103.62(16) . . . . ? N3 Zr1 N2 C17 -159.19(16) . . . . ? N4 Zr1 N2 C17 -86.74(16) . . . . ? N1 Zr1 N2 C17 1.67(15) . . . . ? N5 Zr1 N3 C36 -92.26(16) . . . . ? N6 Zr1 N3 C36 164.94(16) . . . . ? N4 Zr1 N3 C36 -3.62(15) . . . . ? N1 Zr1 N3 C36 31.9(2) . . . . ? N2 Zr1 N3 C36 76.05(16) . . . . ? N5 Zr1 N3 C29 90.93(17) . . . . ? N6 Zr1 N3 C29 -11.87(18) . . . . ? N4 Zr1 N3 C29 179.57(18) . . . . ? N1 Zr1 N3 C29 -144.91(16) . . . . ? N2 Zr1 N3 C29 -100.76(17) . . . . ? N5 Zr1 N4 C40 -83.7(2) . . . . ? N6 Zr1 N4 C40 127.4(3) . . . . ? N3 Zr1 N4 C40 176.2(3) . . . . ? N1 Zr1 N4 C40 11.3(2) . . . . ? N2 Zr1 N4 C40 83.9(2) . . . . ? N5 Zr1 N4 C37 104.72(15) . . . . ? N6 Zr1 N4 C37 -44.2(4) . . . . ? N3 Zr1 N4 C37 4.64(14) . . . . ? N1 Zr1 N4 C37 -160.23(15) . . . . ? N2 Zr1 N4 C37 -87.65(15) . . . . ? N6 Zr1 N5 C42 -36.6(2) . . . . ? N3 Zr1 N5 C42 -136.04(18) . . . . ? N4 Zr1 N5 C42 151.35(19) . . . . ? N1 Zr1 N5 C42 65.81(19) . . . . ? N2 Zr1 N5 C42 96.1(3) . . . . ? N6 Zr1 N5 C41 151.46(19) . . . . ? N3 Zr1 N5 C41 52.0(2) . . . . ? N4 Zr1 N5 C41 -20.6(2) . . . . ? N1 Zr1 N5 C41 -106.2(2) . . . . ? N2 Zr1 N5 C41 -75.9(4) . . . . ? N5 Zr1 N6 C44 161.57(19) . . . . ? N3 Zr1 N6 C44 -96.6(2) . . . . ? N4 Zr1 N6 C44 -50.2(4) . . . . ? N1 Zr1 N6 C44 64.0(2) . . . . ? N2 Zr1 N6 C44 -7.55(19) . . . . ? N5 Zr1 N6 C43 -29.69(19) . . . . ? N3 Zr1 N6 C43 72.18(18) . . . . ? N4 Zr1 N6 C43 118.6(3) . . . . ? N1 Zr1 N6 C43 -127.30(18) . . . . ? N2 Zr1 N6 C43 161.19(18) . . . . ? C15 O1 C2 C3 -0.8(4) . . . . ? C15 O1 C2 C1 176.5(3) . . . . ? C6 C1 C2 O1 179.4(2) . . . . ? C9 C1 C2 O1 -1.6(3) . . . . ? C6 C1 C2 C3 -3.1(4) . . . . ? C9 C1 C2 C3 175.8(2) . . . . ? O1 C2 C3 C4 177.5(2) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C2 C3 C4 C5 1.9(4) . . . . ? C3 C4 C5 C6 -1.2(4) . . . . ? C2 C1 C6 C5 3.7(3) . . . . ? C9 C1 C6 C5 -175.2(2) . . . . ? C2 C1 C6 C7 -177.0(2) . . . . ? C9 C1 C6 C7 4.1(4) . . . . ? C4 C5 C6 C1 -1.6(4) . . . . ? C4 C5 C6 C7 179.1(2) . . . . ? C16 N1 C8 C10 -125.3(2) . . . . ? Zr1 N1 C8 C10 56.1(3) . . . . ? C16 N1 C8 C9 56.3(3) . . . . ? Zr1 N1 C8 C9 -122.2(2) . . . . ? C10 C8 C9 C13 1.7(3) . . . . ? N1 C8 C9 C13 -179.9(2) . . . . ? C10 C8 C9 C1 -177.6(2) . . . . ? N1 C8 C9 C1 0.7(3) . . . . ? C6 C1 C9 C8 83.2(3) . . . . ? C2 C1 C9 C8 -95.7(3) . . . . ? C6 C1 C9 C13 -96.2(3) . . . . ? C2 C1 C9 C13 84.9(3) . . . . ? C9 C8 C10 C11 -1.1(4) . . . . ? N1 C8 C10 C11 -179.5(2) . . . . ? C8 C10 C11 C12 -0.2(4) . . . . ? C10 C11 C12 C13 0.8(4) . . . . ? C11 C12 C13 C9 -0.1(4) . . . . ? C11 C12 C13 C14 -179.9(3) . . . . ? C8 C9 C13 C12 -1.2(4) . . . . ? C1 C9 C13 C12 178.2(2) . . . . ? C8 C9 C13 C14 178.7(3) . . . . ? C1 C9 C13 C14 -2.0(4) . . . . ? C8 N1 C16 C17 -177.6(2) . . . . ? Zr1 N1 C16 C17 1.1(3) . . . . ? C20 N2 C17 C18 0.4(3) . . . . ? Zr1 N2 C17 C18 179.45(16) . . . . ? C20 N2 C17 C16 179.2(2) . . . . ? Zr1 N2 C17 C16 -1.8(3) . . . . ? N1 C16 C17 N2 0.5(3) . . . . ? N1 C16 C17 C18 178.9(2) . . . . ? N2 C17 C18 C19 0.0(3) . . . . ? C16 C17 C18 C19 -178.6(3) . . . . ? C17 C18 C19 C20 -0.3(3) . . . . ? C17 N2 C20 C19 -0.6(3) . . . . ? Zr1 N2 C20 C19 -179.26(19) . . . . ? C18 C19 C20 N2 0.6(3) . . . . ? C35 O2 C22 C23 -8.2(4) . . . . ? C35 O2 C22 C21 173.0(3) . . . . ? C26 C21 C22 O2 177.7(2) . . . . ? C28 C21 C22 O2 2.1(3) . . . . ? C26 C21 C22 C23 -1.1(4) . . . . ? C28 C21 C22 C23 -176.7(2) . . . . ? O2 C22 C23 C24 -178.0(2) . . . . ? C21 C22 C23 C24 0.7(4) . . . . ? C22 C23 C24 C25 0.0(4) . . . . ? C23 C24 C25 C26 -0.4(4) . . . . ? C22 C21 C26 C25 0.8(3) . . . . ? C28 C21 C26 C25 176.4(2) . . . . ? C22 C21 C26 C27 179.6(2) . . . . ? C28 C21 C26 C27 -4.8(3) . . . . ? C24 C25 C26 C21 -0.1(4) . . . . ? C24 C25 C26 C27 -178.9(2) . . . . ? C26 C21 C28 C29 86.6(3) . . . . ? C22 C21 C28 C29 -97.8(3) . . . . ? C26 C21 C28 C33 -90.3(3) . . . . ? C22 C21 C28 C33 85.2(3) . . . . ? C33 C28 C29 C30 2.9(3) . . . . ? C21 C28 C29 C30 -174.1(2) . . . . ? C33 C28 C29 N3 -176.6(2) . . . . ? C21 C28 C29 N3 6.4(3) . . . . ? C36 N3 C29 C30 -116.2(2) . . . . ? Zr1 N3 C29 C30 60.5(3) . . . . ? C36 N3 C29 C28 63.3(3) . . . . ? Zr1 N3 C29 C28 -119.9(2) . . . . ? C28 C29 C30 C31 -1.9(4) . . . . ? N3 C29 C30 C31 177.6(2) . . . . ? C29 C30 C31 C32 -0.7(4) . . . . ? C30 C31 C32 C33 2.4(4) . . . . ? C31 C32 C33 C28 -1.4(4) . . . . ? C31 C32 C33 C34 177.8(2) . . . . ? C29 C28 C33 C32 -1.2(3) . . . . ? C21 C28 C33 C32 175.9(2) . . . . ? C29 C28 C33 C34 179.6(2) . . . . ? C21 C28 C33 C34 -3.4(3) . . . . ? C29 N3 C36 C37 179.34(19) . . . . ? Zr1 N3 C36 C37 2.1(3) . . . . ? C40 N4 C37 C36 180.0(2) . . . . ? Zr1 N4 C37 C36 -5.5(2) . . . . ? C40 N4 C37 C38 -0.5(3) . . . . ? Zr1 N4 C37 C38 174.09(15) . . . . ? N3 C36 C37 N4 2.4(3) . . . . ? N3 C36 C37 C38 -177.1(2) . . . . ? N4 C37 C38 C39 0.6(3) . . . . ? C36 C37 C38 C39 -179.9(2) . . . . ? C37 C38 C39 C40 -0.5(3) . . . . ? C37 N4 C40 C39 0.1(3) . . . . ? Zr1 N4 C40 C39 -171.82(19) . . . . ? C38 C39 C40 N4 0.2(3) . . . . ? C50 C45 C46 C47 1.8(7) . . . . ? C45 C46 C47 C48 -1.8(7) . . . . ? C46 C47 C48 C49 -0.7(7) . . . . ? C47 C48 C49 C50 3.0(7) . . . . ? C48 C49 C50 C45 -2.9(7) . . . . ? C46 C45 C50 C49 0.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.622 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.051 # Attachment 'compound_16.cif' data_16 _database_code_depnum_ccdc_archive 'CCDC 687855' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H86 N10 O2 Zr3' _chemical_formula_sum 'C76 H86 N10 O2 Zr3' _chemical_formula_weight 1445.21 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 13.8984(4) _cell_length_b 18.2349(5) _cell_length_c 26.8816(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6812.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 15564 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.505 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8970 _exptl_absorpt_correction_T_max 0.9236 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64426 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.88 _reflns_number_total 16248 _reflns_number_gt 14957 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+3.2024P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 16248 _refine_ls_number_parameters 835 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.20454(3) 0.533485(17) 0.755585(12) 0.02335(8) Uani 1 1 d . . . Zr2 Zr 0.24507(2) 0.555099(16) 0.634710(12) 0.01996(7) Uani 1 1 d . . . Zr3 Zr 0.28665(3) 0.592313(17) 0.515710(13) 0.02388(8) Uani 1 1 d . . . O1 O 0.32032(16) 0.50498(12) 0.69923(8) 0.0211(5) Uani 1 1 d . . . O2 O 0.20008(16) 0.51082(11) 0.56141(8) 0.0206(5) Uani 1 1 d . . . N1 N 0.37839(19) 0.54137(14) 0.59516(10) 0.0192(6) Uani 1 1 d . . . N2 N 0.3890(2) 0.51213(15) 0.48736(11) 0.0223(6) Uani 1 1 d . . . N3 N 0.1371(2) 0.48509(15) 0.66619(10) 0.0199(6) Uani 1 1 d . . . N4 N 0.1604(2) 0.41985(15) 0.76394(10) 0.0232(6) Uani 1 1 d . . . N5 N 0.2271(2) 0.63122(15) 0.70001(11) 0.0258(7) Uani 1 1 d . . . N6 N 0.3009(2) 0.55060(16) 0.81213(11) 0.0296(7) Uani 1 1 d . . . N7 N 0.0842(2) 0.56979(16) 0.79218(11) 0.0281(7) Uani 1 1 d . . . N8 N 0.2141(2) 0.64982(14) 0.58425(11) 0.0273(7) Uani 1 1 d . . . N9 N 0.1824(2) 0.59637(18) 0.46184(11) 0.0335(8) Uani 1 1 d . . . N10 N 0.3703(3) 0.67768(17) 0.48964(13) 0.0395(9) Uani 1 1 d . . . C1 C 0.4831(2) 0.47366(19) 0.67808(13) 0.0211(7) Uani 1 1 d . . . C2 C 0.3953(2) 0.45504(19) 0.69806(12) 0.0224(7) Uani 1 1 d . . . C3 C 0.3788(3) 0.38327(19) 0.71810(14) 0.0259(8) Uani 1 1 d . . . H3 H 0.3207 0.3727 0.7353 0.031 Uiso 1 1 calc R . . C4 C 0.4473(3) 0.3300(2) 0.71221(14) 0.0297(9) Uani 1 1 d . . . H4 H 0.4363 0.2827 0.7259 0.036 Uiso 1 1 calc R . . C5 C 0.5335(3) 0.3436(2) 0.68648(14) 0.0266(8) Uani 1 1 d . . . C6 C 0.5539(3) 0.4168(2) 0.67019(13) 0.0253(8) Uani 1 1 d . . . C7 C 0.6381(3) 0.4289(2) 0.64231(15) 0.0335(9) Uani 1 1 d . . . H7 H 0.6534 0.4774 0.6322 0.040 Uiso 1 1 calc R . . C8 C 0.6988(3) 0.3727(2) 0.62936(17) 0.0453(11) Uani 1 1 d . . . H8 H 0.7537 0.3822 0.6093 0.054 Uiso 1 1 calc R . . C9 C 0.6793(3) 0.3006(2) 0.64610(18) 0.0457(12) Uani 1 1 d . . . H9 H 0.7218 0.2617 0.6377 0.055 Uiso 1 1 calc R . . C10 C 0.5997(3) 0.2870(2) 0.67423(16) 0.0381(10) Uani 1 1 d . . . H10 H 0.5882 0.2386 0.6859 0.046 Uiso 1 1 calc R . . C11 C 0.5030(2) 0.55011(19) 0.66125(13) 0.0225(7) Uani 1 1 d . . . C12 C 0.4541(2) 0.58061(18) 0.62124(13) 0.0223(7) Uani 1 1 d . . . C13 C 0.4761(3) 0.6531(2) 0.60564(15) 0.0294(8) Uani 1 1 d . . . H13 H 0.4442 0.6731 0.5775 0.035 Uiso 1 1 calc R . . C14 C 0.5431(3) 0.6947(2) 0.63077(16) 0.0359(10) Uani 1 1 d . . . H14 H 0.5553 0.7435 0.6202 0.043 Uiso 1 1 calc R . . C15 C 0.5935(3) 0.6663(2) 0.67154(15) 0.0310(9) Uani 1 1 d . . . C16 C 0.5734(2) 0.5931(2) 0.68748(13) 0.0247(8) Uani 1 1 d . . . C17 C 0.6242(3) 0.5657(2) 0.72903(14) 0.0319(9) Uani 1 1 d . . . H17 H 0.6112 0.5174 0.7405 0.038 Uiso 1 1 calc R . . C18 C 0.6923(3) 0.6075(2) 0.75317(15) 0.0399(10) Uani 1 1 d . . . H18 H 0.7255 0.5880 0.7811 0.048 Uiso 1 1 calc R . . C19 C 0.7131(3) 0.6791(2) 0.73656(16) 0.0426(11) Uani 1 1 d . . . H19 H 0.7607 0.7075 0.7530 0.051 Uiso 1 1 calc R . . C20 C 0.6650(3) 0.7075(2) 0.69700(16) 0.0374(10) Uani 1 1 d . . . H20 H 0.6795 0.7558 0.6861 0.045 Uiso 1 1 calc R . . C21 C 0.4125(2) 0.46951(18) 0.57353(13) 0.0223(7) Uani 1 1 d . . . H21A H 0.4641 0.4491 0.5948 0.027 Uiso 1 1 calc R . . H21B H 0.3585 0.4341 0.5732 0.027 Uiso 1 1 calc R . . C22 C 0.4496(2) 0.47938(18) 0.52185(13) 0.0219(7) Uani 1 1 d . . . C23 C 0.5351(2) 0.45917(18) 0.50001(13) 0.0243(8) Uani 1 1 d . . . H23 H 0.5885 0.4367 0.5159 0.029 Uiso 1 1 calc R . . C24 C 0.5278(3) 0.4786(2) 0.44919(14) 0.0288(8) Uani 1 1 d . . . H24 H 0.5753 0.4711 0.4243 0.035 Uiso 1 1 calc R . . C25 C 0.4389(3) 0.5102(2) 0.44267(14) 0.0296(9) Uani 1 1 d . . . H25 H 0.4150 0.5283 0.4119 0.035 Uiso 1 1 calc R . . C26 C 0.0701(2) 0.42581(18) 0.56964(12) 0.0201(7) Uani 1 1 d . . . C27 C 0.1583(2) 0.44483(18) 0.54982(12) 0.0208(7) Uani 1 1 d . . . C28 C 0.2070(3) 0.39680(17) 0.51611(13) 0.0246(7) Uani 1 1 d . . . H28 H 0.2656 0.4121 0.5012 0.030 Uiso 1 1 calc R . . C29 C 0.1704(3) 0.32946(19) 0.50525(13) 0.0278(8) Uani 1 1 d . . . H29 H 0.2036 0.2984 0.4827 0.033 Uiso 1 1 calc R . . C30 C 0.0826(3) 0.30485(18) 0.52725(13) 0.0238(8) Uani 1 1 d . . . C31 C 0.0327(2) 0.35253(18) 0.56012(13) 0.0213(7) Uani 1 1 d . . . C32 C -0.0520(3) 0.32603(19) 0.58309(13) 0.0247(8) Uani 1 1 d . . . H32 H -0.0855 0.3564 0.6060 0.030 Uiso 1 1 calc R . . C33 C -0.0867(3) 0.2572(2) 0.57283(14) 0.0285(8) Uani 1 1 d . . . H33 H -0.1440 0.2407 0.5885 0.034 Uiso 1 1 calc R . . C34 C -0.0384(3) 0.2110(2) 0.53954(15) 0.0328(9) Uani 1 1 d . . . H34 H -0.0637 0.1638 0.5322 0.039 Uiso 1 1 calc R . . C35 C 0.0455(3) 0.23394(19) 0.51754(15) 0.0317(9) Uani 1 1 d . . . H35 H 0.0790 0.2020 0.4956 0.038 Uiso 1 1 calc R . . C36 C 0.0125(2) 0.47875(18) 0.59979(13) 0.0211(7) Uani 1 1 d . . . C37 C 0.0440(2) 0.50502(17) 0.64598(13) 0.0206(7) Uani 1 1 d . . . C38 C -0.0136(2) 0.5548(2) 0.67286(14) 0.0247(8) Uani 1 1 d . . . H38 H 0.0078 0.5716 0.7044 0.030 Uiso 1 1 calc R . . C39 C -0.0996(3) 0.57959(19) 0.65466(14) 0.0281(8) Uani 1 1 d . . . H39 H -0.1369 0.6128 0.6738 0.034 Uiso 1 1 calc R . . C40 C -0.1336(2) 0.55646(19) 0.60781(13) 0.0241(8) Uani 1 1 d . . . C41 C -0.0776(2) 0.50448(18) 0.58030(13) 0.0220(7) Uani 1 1 d . . . C42 C -0.1153(3) 0.48123(19) 0.53321(13) 0.0249(8) Uani 1 1 d . . . H42 H -0.0797 0.4472 0.5138 0.030 Uiso 1 1 calc R . . C43 C -0.2013(3) 0.50699(19) 0.51566(14) 0.0288(8) Uani 1 1 d . . . H43 H -0.2246 0.4901 0.4845 0.035 Uiso 1 1 calc R . . C44 C -0.2558(3) 0.55790(19) 0.54296(14) 0.0309(8) Uani 1 1 d . . . H44 H -0.3155 0.5751 0.5303 0.037 Uiso 1 1 calc R . . C45 C -0.2225(2) 0.58255(18) 0.58778(14) 0.0270(8) Uani 1 1 d . . . H45 H -0.2590 0.6176 0.6059 0.032 Uiso 1 1 calc R . . C46 C 0.1501(2) 0.40430(18) 0.67258(12) 0.0215(7) Uani 1 1 d . . . H46A H 0.2177 0.3913 0.6651 0.026 Uiso 1 1 calc R . . H46B H 0.1084 0.3782 0.6485 0.026 Uiso 1 1 calc R . . C47 C 0.1260(2) 0.37943(19) 0.72425(13) 0.0229(8) Uani 1 1 d . . . C48 C 0.0798(3) 0.3178(2) 0.74144(15) 0.0325(9) Uani 1 1 d . . . H48 H 0.0493 0.2811 0.7218 0.039 Uiso 1 1 calc R . . C49 C 0.0863(3) 0.3194(2) 0.79405(15) 0.0342(9) Uani 1 1 d . . . H49 H 0.0615 0.2838 0.8165 0.041 Uiso 1 1 calc R . . C50 C 0.1348(3) 0.3818(2) 0.80641(14) 0.0284(8) Uani 1 1 d . . . H50 H 0.1491 0.3969 0.8394 0.034 Uiso 1 1 calc R . . C51 C 0.3156(3) 0.6709(2) 0.71676(15) 0.0339(9) Uani 1 1 d . . . H51A H 0.3269 0.7132 0.6951 0.051 Uiso 1 1 calc R . . H51B H 0.3710 0.6377 0.7151 0.051 Uiso 1 1 calc R . . H51C H 0.3069 0.6878 0.7511 0.051 Uiso 1 1 calc R . . C52 C 0.1468(3) 0.6862(2) 0.70112(16) 0.0363(10) Uani 1 1 d . . . H52A H 0.1319 0.6987 0.7357 0.054 Uiso 1 1 calc R . . H52B H 0.0897 0.6652 0.6852 0.054 Uiso 1 1 calc R . . H52C H 0.1665 0.7305 0.6832 0.054 Uiso 1 1 calc R . . C53 C 0.4066(3) 0.5500(2) 0.80727(15) 0.0389(10) Uani 1 1 d . . . H53A H 0.4324 0.5976 0.8178 0.058 Uiso 1 1 calc R . . H53B H 0.4241 0.5409 0.7725 0.058 Uiso 1 1 calc R . . H53C H 0.4334 0.5112 0.8283 0.058 Uiso 1 1 calc R . . C54 C 0.2756(3) 0.5664(2) 0.86482(14) 0.0409(10) Uani 1 1 d . . . H54A H 0.3077 0.5309 0.8866 0.061 Uiso 1 1 calc R . . H54B H 0.2058 0.5626 0.8691 0.061 Uiso 1 1 calc R . . H54C H 0.2967 0.6161 0.8734 0.061 Uiso 1 1 calc R . . C55 C 0.0810(3) 0.6395(2) 0.81838(16) 0.0394(10) Uani 1 1 d . . . H55A H 0.0328 0.6714 0.8029 0.059 Uiso 1 1 calc R . . H55B H 0.1442 0.6631 0.8167 0.059 Uiso 1 1 calc R . . H55C H 0.0637 0.6311 0.8533 0.059 Uiso 1 1 calc R . . C56 C -0.0076(3) 0.5317(2) 0.79876(15) 0.0373(10) Uani 1 1 d . . . H56A H -0.0190 0.5233 0.8343 0.056 Uiso 1 1 calc R . . H56B H -0.0056 0.4846 0.7813 0.056 Uiso 1 1 calc R . . H56C H -0.0597 0.5619 0.7851 0.056 Uiso 1 1 calc R . . C57 C 0.1095(3) 0.6609(2) 0.57166(15) 0.0334(9) Uani 1 1 d . . . H57A H 0.0778 0.6876 0.5987 0.050 Uiso 1 1 calc R . . H57B H 0.0784 0.6131 0.5673 0.050 Uiso 1 1 calc R . . H57C H 0.1042 0.6892 0.5408 0.050 Uiso 1 1 calc R . . C58 C 0.2527(3) 0.72437(19) 0.59365(16) 0.0416(10) Uani 1 1 d . . . H58A H 0.2577 0.7511 0.5621 0.062 Uiso 1 1 calc R . . H58B H 0.3165 0.7206 0.6089 0.062 Uiso 1 1 calc R . . H58C H 0.2093 0.7508 0.6161 0.062 Uiso 1 1 calc R . . C59 C 0.0830(3) 0.5691(2) 0.46411(15) 0.0399(11) Uani 1 1 d . . . H59A H 0.0383 0.6104 0.4613 0.060 Uiso 1 1 calc R . . H59B H 0.0726 0.5439 0.4959 0.060 Uiso 1 1 calc R . . H59C H 0.0719 0.5348 0.4366 0.060 Uiso 1 1 calc R . . C60 C 0.1991(3) 0.6307(3) 0.41292(15) 0.0496(12) Uani 1 1 d . . . H60A H 0.1831 0.5957 0.3865 0.074 Uiso 1 1 calc R . . H60B H 0.2669 0.6449 0.4101 0.074 Uiso 1 1 calc R . . H60C H 0.1584 0.6743 0.4097 0.074 Uiso 1 1 calc R . . C61 C 0.3333(4) 0.7491(2) 0.47450(18) 0.0612(16) Uani 1 1 d . . . H61A H 0.3616 0.7874 0.4955 0.092 Uiso 1 1 calc R . . H61B H 0.2632 0.7498 0.4782 0.092 Uiso 1 1 calc R . . H61C H 0.3503 0.7583 0.4397 0.092 Uiso 1 1 calc R . . C62 C 0.4751(3) 0.6751(2) 0.48154(17) 0.0470(12) Uani 1 1 d . . . H62A H 0.4888 0.6803 0.4460 0.070 Uiso 1 1 calc R . . H62B H 0.5003 0.6280 0.4934 0.070 Uiso 1 1 calc R . . H62C H 0.5059 0.7152 0.4999 0.070 Uiso 1 1 calc R . . C63 C 0.1606(3) 0.1854(3) 0.63286(18) 0.0504(12) Uani 1 1 d . . . H63A H 0.1193 0.1521 0.6138 0.076 Uiso 1 1 calc R . . H63B H 0.1395 0.2361 0.6276 0.076 Uiso 1 1 calc R . . H63C H 0.1561 0.1733 0.6683 0.076 Uiso 1 1 calc R . . C64 C 0.2621(3) 0.1771(2) 0.61600(14) 0.0364(10) Uani 1 1 d . . . C65 C 0.3039(3) 0.1077(2) 0.61118(14) 0.0386(10) Uani 1 1 d . . . H65 H 0.2665 0.0653 0.6182 0.046 Uiso 1 1 calc R . . C66 C 0.3984(3) 0.0997(3) 0.59647(16) 0.0466(11) Uani 1 1 d . . . H66 H 0.4251 0.0520 0.5931 0.056 Uiso 1 1 calc R . . C67 C 0.4540(4) 0.1601(3) 0.58673(17) 0.0552(13) Uani 1 1 d . . . H67 H 0.5194 0.1544 0.5773 0.066 Uiso 1 1 calc R . . C68 C 0.4140(4) 0.2299(3) 0.59081(18) 0.0547(13) Uani 1 1 d . . . H68 H 0.4519 0.2718 0.5835 0.066 Uiso 1 1 calc R . . C69 C 0.3198(3) 0.2382(2) 0.60537(16) 0.0432(11) Uani 1 1 d . . . H69 H 0.2934 0.2861 0.6083 0.052 Uiso 1 1 calc R . . C70 C 0.6903(4) 0.6099(3) 0.25479(19) 0.0699(16) Uani 1 1 d . . . H70A H 0.7233 0.6447 0.2329 0.105 Uiso 1 1 calc R . . H70B H 0.6236 0.6257 0.2597 0.105 Uiso 1 1 calc R . . H70C H 0.6909 0.5611 0.2395 0.105 Uiso 1 1 calc R . . C71 C 0.7413(4) 0.6070(2) 0.30442(16) 0.0448(11) Uani 1 1 d . . . C72 C 0.6859(3) 0.5976(2) 0.34819(17) 0.0439(11) Uani 1 1 d . . . H72 H 0.6178 0.5941 0.3462 0.053 Uiso 1 1 calc R . . C73 C 0.7316(3) 0.5935(2) 0.39413(17) 0.0446(11) Uani 1 1 d . . . H73 H 0.6951 0.5870 0.4237 0.054 Uiso 1 1 calc R . . C74 C 0.8299(4) 0.5991(2) 0.39639(19) 0.0490(12) Uani 1 1 d . . . H74 H 0.8613 0.5958 0.4277 0.059 Uiso 1 1 calc R . . C75 C 0.8841(4) 0.6094(2) 0.3538(2) 0.0604(14) Uani 1 1 d . . . H75 H 0.9521 0.6139 0.3559 0.073 Uiso 1 1 calc R . . C76 C 0.8397(4) 0.6131(2) 0.3092(2) 0.0560(14) Uani 1 1 d . . . H76 H 0.8775 0.6202 0.2801 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02550(17) 0.02402(16) 0.02052(18) -0.00286(13) 0.00239(15) -0.00177(14) Zr2 0.02251(16) 0.01738(14) 0.02000(16) 0.00019(13) 0.00140(14) -0.00027(13) Zr3 0.02639(17) 0.02169(15) 0.02357(18) 0.00607(14) 0.00325(15) 0.00265(14) O1 0.0211(12) 0.0242(12) 0.0179(12) -0.0010(10) -0.0003(10) 0.0018(10) O2 0.0229(12) 0.0180(11) 0.0208(12) 0.0002(9) 0.0027(11) -0.0016(10) N1 0.0205(14) 0.0160(13) 0.0210(15) -0.0005(12) 0.0028(12) 0.0005(11) N2 0.0217(15) 0.0248(15) 0.0204(16) 0.0048(12) 0.0009(13) 0.0023(12) N3 0.0206(14) 0.0180(14) 0.0211(16) 0.0004(11) 0.0020(12) -0.0004(11) N4 0.0287(16) 0.0249(15) 0.0161(15) -0.0027(12) 0.0022(13) -0.0046(12) N5 0.0275(18) 0.0230(14) 0.0268(17) -0.0055(12) 0.0044(13) 0.0009(12) N6 0.0324(17) 0.0323(16) 0.0240(16) -0.0017(13) -0.0011(14) -0.0044(15) N7 0.0304(18) 0.0307(17) 0.0231(17) -0.0068(13) 0.0008(14) 0.0003(13) N8 0.0302(16) 0.0188(13) 0.0330(18) 0.0038(12) 0.0027(15) 0.0026(13) N9 0.0319(18) 0.0425(19) 0.0261(17) 0.0077(15) 0.0021(14) 0.0108(15) N10 0.051(2) 0.0280(17) 0.040(2) 0.0111(16) 0.0102(18) -0.0039(16) C1 0.0200(17) 0.0266(17) 0.0167(18) 0.0039(15) -0.0005(14) -0.0007(14) C2 0.0263(18) 0.0256(18) 0.0154(17) 0.0005(14) -0.0015(14) 0.0002(15) C3 0.0247(19) 0.0266(18) 0.026(2) 0.0067(16) -0.0001(16) -0.0044(15) C4 0.032(2) 0.0256(18) 0.032(2) 0.0119(16) -0.0028(17) -0.0029(16) C5 0.0195(19) 0.032(2) 0.029(2) 0.0058(16) 0.0001(16) 0.0018(15) C6 0.0229(18) 0.0308(19) 0.022(2) 0.0057(15) -0.0019(15) -0.0017(15) C7 0.0249(19) 0.036(2) 0.040(2) 0.0110(18) 0.0043(18) 0.0007(15) C8 0.030(2) 0.041(2) 0.064(3) 0.011(2) 0.011(2) 0.0102(19) C9 0.029(2) 0.041(2) 0.068(3) 0.011(2) 0.009(2) 0.0135(18) C10 0.033(2) 0.032(2) 0.049(3) 0.0136(19) 0.000(2) 0.0095(18) C11 0.0200(17) 0.0231(18) 0.024(2) 0.0005(15) 0.0052(14) -0.0039(14) C12 0.0237(18) 0.0226(17) 0.0207(19) -0.0002(14) 0.0050(14) -0.0024(14) C13 0.032(2) 0.0252(18) 0.031(2) 0.0035(16) 0.0034(18) -0.0028(16) C14 0.041(2) 0.0216(18) 0.046(3) -0.0029(18) 0.003(2) -0.0078(16) C15 0.027(2) 0.031(2) 0.036(2) -0.0088(17) 0.0057(18) -0.0050(16) C16 0.0186(17) 0.0305(19) 0.025(2) -0.0056(16) 0.0062(15) -0.0022(15) C17 0.026(2) 0.037(2) 0.032(2) -0.0052(17) 0.0006(17) -0.0074(17) C18 0.030(2) 0.055(3) 0.034(2) -0.014(2) 0.0002(19) -0.0066(19) C19 0.028(2) 0.048(2) 0.052(3) -0.028(2) 0.001(2) -0.006(2) C20 0.031(2) 0.034(2) 0.046(3) -0.0125(19) 0.010(2) -0.0064(18) C21 0.0242(18) 0.0172(16) 0.0254(19) 0.0004(15) -0.0016(15) 0.0001(14) C22 0.0242(17) 0.0193(16) 0.0221(19) 0.0007(14) -0.0006(15) -0.0042(13) C23 0.0199(17) 0.0247(18) 0.028(2) -0.0053(15) -0.0019(14) -0.0005(14) C24 0.028(2) 0.0302(19) 0.028(2) -0.0020(16) 0.0070(17) -0.0002(16) C25 0.031(2) 0.035(2) 0.022(2) 0.0043(16) 0.0040(17) 0.0006(17) C26 0.0220(17) 0.0234(17) 0.0148(17) -0.0015(13) -0.0019(14) 0.0029(13) C27 0.0215(17) 0.0206(16) 0.0202(18) 0.0017(14) -0.0003(14) 0.0006(14) C28 0.0219(16) 0.0281(17) 0.0239(18) -0.0017(15) 0.0026(16) -0.0008(15) C29 0.030(2) 0.0272(18) 0.026(2) -0.0067(15) 0.0042(16) 0.0025(15) C30 0.0240(18) 0.0223(17) 0.025(2) -0.0046(15) 0.0005(15) 0.0002(14) C31 0.0215(18) 0.0232(17) 0.0192(19) 0.0019(14) -0.0013(15) 0.0028(14) C32 0.0237(18) 0.0255(18) 0.025(2) 0.0032(15) 0.0020(15) 0.0056(15) C33 0.0247(19) 0.0282(19) 0.033(2) 0.0011(16) 0.0020(17) -0.0053(15) C34 0.038(2) 0.0224(18) 0.038(2) -0.0045(17) -0.0007(19) -0.0015(16) C35 0.033(2) 0.0265(19) 0.036(2) -0.0063(17) -0.0004(19) 0.0002(16) C36 0.0185(16) 0.0207(16) 0.0242(19) -0.0013(14) 0.0035(14) 0.0006(13) C37 0.0215(17) 0.0171(15) 0.023(2) 0.0015(14) 0.0040(14) -0.0006(13) C38 0.0251(18) 0.0241(17) 0.025(2) -0.0012(16) 0.0029(15) -0.0017(15) C39 0.0264(19) 0.0245(18) 0.033(2) 0.0002(16) 0.0067(17) 0.0046(15) C40 0.0209(17) 0.0231(17) 0.028(2) 0.0031(15) 0.0037(15) -0.0001(15) C41 0.0232(18) 0.0218(17) 0.0209(19) 0.0025(14) 0.0033(15) -0.0005(14) C42 0.0241(18) 0.0249(18) 0.026(2) 0.0009(15) 0.0012(15) 0.0012(14) C43 0.0269(18) 0.0312(18) 0.028(2) 0.0027(16) -0.0040(18) -0.0002(16) C44 0.0218(18) 0.0294(18) 0.041(2) 0.0120(17) -0.0037(17) 0.0015(17) C45 0.0190(18) 0.0247(17) 0.037(2) 0.0041(15) 0.0083(16) 0.0035(14) C46 0.0219(17) 0.0208(16) 0.0218(19) -0.0005(14) -0.0010(14) 0.0002(14) C47 0.0218(18) 0.0229(17) 0.024(2) 0.0015(15) 0.0012(15) 0.0004(14) C48 0.041(2) 0.0267(19) 0.030(2) -0.0021(17) 0.0014(19) -0.0072(17) C49 0.043(2) 0.029(2) 0.030(2) 0.0070(17) 0.0081(19) -0.0035(18) C50 0.033(2) 0.034(2) 0.0189(19) 0.0020(16) 0.0061(16) 0.0036(17) C51 0.038(2) 0.0288(19) 0.035(2) -0.0064(17) 0.0028(19) -0.0060(17) C52 0.042(2) 0.0241(19) 0.043(3) -0.0038(18) 0.006(2) 0.0071(17) C53 0.037(2) 0.046(3) 0.033(2) -0.007(2) -0.0054(19) -0.004(2) C54 0.043(3) 0.057(3) 0.023(2) 0.0014(19) -0.0057(19) -0.002(2) C55 0.044(3) 0.040(2) 0.034(2) -0.0066(19) 0.008(2) 0.007(2) C56 0.034(2) 0.050(3) 0.027(2) -0.005(2) 0.0034(18) 0.000(2) C57 0.039(2) 0.027(2) 0.034(2) 0.0053(17) 0.0038(19) 0.0118(17) C58 0.055(3) 0.0238(18) 0.046(3) -0.0013(17) 0.013(2) -0.0007(19) C59 0.030(2) 0.060(3) 0.029(2) 0.007(2) -0.0008(18) 0.011(2) C60 0.050(3) 0.066(3) 0.033(2) 0.018(2) -0.003(2) 0.012(3) C61 0.107(4) 0.025(2) 0.052(3) 0.017(2) 0.022(3) 0.008(2) C62 0.055(3) 0.043(2) 0.043(3) 0.001(2) 0.009(2) -0.022(2) C63 0.045(3) 0.059(3) 0.048(3) -0.006(2) 0.000(2) 0.004(2) C64 0.046(3) 0.040(2) 0.024(2) -0.0029(17) -0.0021(18) -0.001(2) C65 0.052(3) 0.030(2) 0.034(2) 0.0015(17) 0.000(2) -0.002(2) C66 0.049(3) 0.055(3) 0.035(3) -0.008(2) 0.000(2) 0.012(2) C67 0.040(3) 0.087(4) 0.039(3) -0.001(3) -0.002(2) 0.005(3) C68 0.062(3) 0.059(3) 0.043(3) 0.005(2) 0.002(3) -0.023(3) C69 0.054(3) 0.038(2) 0.038(3) 0.0011(19) 0.002(2) -0.005(2) C70 0.096(4) 0.055(3) 0.060(4) -0.003(3) 0.007(4) -0.002(3) C71 0.074(4) 0.028(2) 0.033(2) -0.0011(17) -0.001(2) 0.001(2) C72 0.049(3) 0.031(2) 0.052(3) -0.004(2) -0.001(2) -0.0078(19) C73 0.062(3) 0.031(2) 0.041(3) 0.0008(19) 0.003(2) -0.006(2) C74 0.064(3) 0.029(2) 0.054(3) 0.000(2) 0.003(3) -0.001(2) C75 0.073(4) 0.036(3) 0.072(4) -0.006(3) 0.008(3) 0.001(2) C76 0.067(4) 0.038(3) 0.063(4) 0.001(2) 0.021(3) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N6 2.050(3) . ? Zr1 N7 2.050(3) . ? Zr1 N4 2.173(3) . ? Zr1 O1 2.270(2) . ? Zr1 N5 2.346(3) . ? Zr1 N3 2.726(3) . ? Zr1 Zr2 3.3212(5) . ? Zr2 N3 2.145(3) . ? Zr2 N1 2.151(3) . ? Zr2 O2 2.219(2) . ? Zr2 O1 2.222(2) . ? Zr2 N8 2.238(3) . ? Zr2 N5 2.252(3) . ? Zr2 Zr3 3.3208(5) . ? Zr3 N9 2.050(3) . ? Zr3 N10 2.065(3) . ? Zr3 N2 2.178(3) . ? Zr3 O2 2.273(2) . ? Zr3 N8 2.347(3) . ? Zr3 N1 2.655(3) . ? O1 C2 1.384(4) . ? O2 C27 1.372(4) . ? N1 C12 1.453(4) . ? N1 C21 1.510(4) . ? N2 C22 1.387(4) . ? N2 C25 1.388(4) . ? N3 C37 1.449(4) . ? N3 C46 1.494(4) . ? N4 C47 1.382(4) . ? N4 C50 1.382(4) . ? N5 C51 1.497(4) . ? N5 C52 1.499(4) . ? N6 C53 1.475(5) . ? N6 C54 1.487(5) . ? N7 C55 1.454(5) . ? N7 C56 1.463(5) . ? N8 C58 1.483(4) . ? N8 C57 1.507(5) . ? N9 C59 1.469(5) . ? N9 C60 1.475(5) . ? N10 C61 1.459(5) . ? N10 C62 1.473(5) . ? C1 C2 1.375(5) . ? C1 C6 1.445(5) . ? C1 C11 1.491(5) . ? C2 C3 1.434(5) . ? C3 C4 1.370(5) . ? C3 H3 0.9500 . ? C4 C5 1.405(5) . ? C4 H4 0.9500 . ? C5 C10 1.421(5) . ? C5 C6 1.433(5) . ? C6 C7 1.408(5) . ? C7 C8 1.372(5) . ? C7 H7 0.9500 . ? C8 C9 1.416(5) . ? C8 H8 0.9500 . ? C9 C10 1.364(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.388(5) . ? C11 C16 1.439(5) . ? C12 C13 1.419(5) . ? C13 C14 1.378(5) . ? C13 H13 0.9500 . ? C14 C15 1.400(6) . ? C14 H14 0.9500 . ? C15 C20 1.422(5) . ? C15 C16 1.428(5) . ? C16 C17 1.413(5) . ? C17 C18 1.378(5) . ? C17 H17 0.9500 . ? C18 C19 1.410(6) . ? C18 H18 0.9500 . ? C19 C20 1.358(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.493(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.376(5) . ? C23 C24 1.415(5) . ? C23 H23 0.9500 . ? C24 C25 1.375(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.381(5) . ? C26 C31 1.456(5) . ? C26 C36 1.493(4) . ? C27 C28 1.431(5) . ? C28 C29 1.361(5) . ? C28 H28 0.9500 . ? C29 C30 1.428(5) . ? C29 H29 0.9500 . ? C30 C35 1.416(5) . ? C30 C31 1.421(5) . ? C31 C32 1.414(5) . ? C32 C33 1.373(5) . ? C32 H32 0.9500 . ? C33 C34 1.400(5) . ? C33 H33 0.9500 . ? C34 C35 1.373(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.401(5) . ? C36 C41 1.436(5) . ? C37 C38 1.410(5) . ? C38 C39 1.368(5) . ? C38 H38 0.9500 . ? C39 C40 1.410(5) . ? C39 H39 0.9500 . ? C40 C45 1.428(5) . ? C40 C41 1.432(5) . ? C41 C42 1.434(5) . ? C42 C43 1.368(5) . ? C42 H42 0.9500 . ? C43 C44 1.405(5) . ? C43 H43 0.9500 . ? C44 C45 1.367(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.499(5) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.375(5) . ? C48 C49 1.418(5) . ? C48 H48 0.9500 . ? C49 C50 1.364(5) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.490(6) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.399(5) . ? C64 C69 1.401(6) . ? C65 C66 1.379(6) . ? C65 H65 0.9500 . ? C66 C67 1.370(7) . ? C66 H66 0.9500 . ? C67 C68 1.393(7) . ? C67 H67 0.9500 . ? C68 C69 1.375(7) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 C71 1.511(7) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C76 1.378(7) . ? C71 C72 1.416(6) . ? C72 C73 1.391(6) . ? C72 H72 0.9500 . ? C73 C74 1.372(6) . ? C73 H73 0.9500 . ? C74 C75 1.384(7) . ? C74 H74 0.9500 . ? C75 C76 1.350(7) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Zr1 N7 97.36(12) . . ? N6 Zr1 N4 104.66(11) . . ? N7 Zr1 N4 91.60(11) . . ? N6 Zr1 O1 93.82(11) . . ? N7 Zr1 O1 166.48(10) . . ? N4 Zr1 O1 92.91(9) . . ? N6 Zr1 N5 105.63(11) . . ? N7 Zr1 N5 99.73(11) . . ? N4 Zr1 N5 145.88(10) . . ? O1 Zr1 N5 69.79(9) . . ? N6 Zr1 N3 158.08(11) . . ? N7 Zr1 N3 104.28(11) . . ? N4 Zr1 N3 71.65(9) . . ? O1 Zr1 N3 65.27(8) . . ? N5 Zr1 N3 74.37(9) . . ? N6 Zr1 Zr2 126.63(9) . . ? N7 Zr1 Zr2 124.71(9) . . ? N4 Zr1 Zr2 105.20(7) . . ? O1 Zr1 Zr2 41.77(6) . . ? N5 Zr1 Zr2 42.64(7) . . ? N3 Zr1 Zr2 40.04(6) . . ? N3 Zr2 N1 136.78(10) . . ? N3 Zr2 O2 86.37(9) . . ? N1 Zr2 O2 76.20(9) . . ? N3 Zr2 O1 77.09(10) . . ? N1 Zr2 O1 86.12(9) . . ? O2 Zr2 O1 132.53(8) . . ? N3 Zr2 N8 124.34(11) . . ? N1 Zr2 N8 87.46(11) . . ? O2 Zr2 N8 71.85(9) . . ? O1 Zr2 N8 151.77(10) . . ? N3 Zr2 N5 88.94(11) . . ? N1 Zr2 N5 123.56(11) . . ? O2 Zr2 N5 152.26(9) . . ? O1 Zr2 N5 72.39(9) . . ? N8 Zr2 N5 88.59(10) . . ? N3 Zr2 Zr3 128.58(8) . . ? N1 Zr2 Zr3 52.97(7) . . ? O2 Zr2 Zr3 42.95(6) . . ? O1 Zr2 Zr3 138.94(6) . . ? N8 Zr2 Zr3 44.91(7) . . ? N5 Zr2 Zr3 130.11(7) . . ? N3 Zr2 Zr1 54.87(8) . . ? N1 Zr2 Zr1 128.01(7) . . ? O2 Zr2 Zr1 141.05(6) . . ? O1 Zr2 Zr1 42.89(6) . . ? N8 Zr2 Zr1 130.70(8) . . ? N5 Zr2 Zr1 44.90(7) . . ? Zr3 Zr2 Zr1 175.008(13) . . ? N9 Zr3 N10 97.52(14) . . ? N9 Zr3 N2 103.82(12) . . ? N10 Zr3 N2 91.12(12) . . ? N9 Zr3 O2 91.79(11) . . ? N10 Zr3 O2 166.96(12) . . ? N2 Zr3 O2 95.51(9) . . ? N9 Zr3 N8 103.58(12) . . ? N10 Zr3 N8 99.86(12) . . ? N2 Zr3 N8 148.77(10) . . ? O2 Zr3 N8 68.93(9) . . ? N9 Zr3 N1 156.97(11) . . ? N10 Zr3 N1 105.45(12) . . ? N2 Zr3 N1 74.50(9) . . ? O2 Zr3 N1 65.84(8) . . ? N8 Zr3 N1 74.40(9) . . ? N9 Zr3 Zr2 124.40(9) . . ? N10 Zr3 Zr2 125.37(10) . . ? N2 Zr3 Zr2 108.28(8) . . ? O2 Zr3 Zr2 41.71(6) . . ? N8 Zr3 Zr2 42.31(7) . . ? N1 Zr3 Zr2 40.29(6) . . ? C2 O1 Zr2 127.4(2) . . ? C2 O1 Zr1 134.4(2) . . ? Zr2 O1 Zr1 95.34(8) . . ? C27 O2 Zr2 129.79(19) . . ? C27 O2 Zr3 132.4(2) . . ? Zr2 O2 Zr3 95.33(8) . . ? C12 N1 C21 112.7(3) . . ? C12 N1 Zr2 109.17(19) . . ? C21 N1 Zr2 124.2(2) . . ? C12 N1 Zr3 124.3(2) . . ? C21 N1 Zr3 98.30(19) . . ? Zr2 N1 Zr3 86.74(9) . . ? C22 N2 C25 105.3(3) . . ? C22 N2 Zr3 116.8(2) . . ? C25 N2 Zr3 130.3(2) . . ? C37 N3 C46 113.5(3) . . ? C37 N3 Zr2 109.12(19) . . ? C46 N3 Zr2 123.2(2) . . ? C37 N3 Zr1 123.8(2) . . ? C46 N3 Zr1 100.14(19) . . ? Zr2 N3 Zr1 85.09(9) . . ? C47 N4 C50 106.3(3) . . ? C47 N4 Zr1 121.8(2) . . ? C50 N4 Zr1 129.5(2) . . ? C51 N5 C52 106.4(3) . . ? C51 N5 Zr2 116.2(2) . . ? C52 N5 Zr2 120.7(2) . . ? C51 N5 Zr1 106.6(2) . . ? C52 N5 Zr1 113.3(2) . . ? Zr2 N5 Zr1 92.46(10) . . ? C53 N6 C54 108.7(3) . . ? C53 N6 Zr1 125.7(2) . . ? C54 N6 Zr1 125.5(2) . . ? C55 N7 C56 109.2(3) . . ? C55 N7 Zr1 122.7(3) . . ? C56 N7 Zr1 128.1(2) . . ? C58 N8 C57 105.3(3) . . ? C58 N8 Zr2 122.3(2) . . ? C57 N8 Zr2 115.1(2) . . ? C58 N8 Zr3 112.8(2) . . ? C57 N8 Zr3 107.3(2) . . ? Zr2 N8 Zr3 92.78(10) . . ? C59 N9 C60 109.2(3) . . ? C59 N9 Zr3 128.5(2) . . ? C60 N9 Zr3 122.3(3) . . ? C61 N10 C62 109.6(4) . . ? C61 N10 Zr3 124.7(3) . . ? C62 N10 Zr3 125.6(3) . . ? C2 C1 C6 119.0(3) . . ? C2 C1 C11 120.9(3) . . ? C6 C1 C11 120.0(3) . . ? C1 C2 O1 120.9(3) . . ? C1 C2 C3 121.0(3) . . ? O1 C2 C3 118.1(3) . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 121.6(3) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C4 C5 C10 122.5(3) . . ? C4 C5 C6 118.9(3) . . ? C10 C5 C6 118.5(3) . . ? C7 C6 C5 118.3(3) . . ? C7 C6 C1 122.1(3) . . ? C5 C6 C1 119.2(3) . . ? C8 C7 C6 122.0(4) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C9 119.7(4) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C5 121.5(4) . . ? C9 C10 H10 119.3 . . ? C5 C10 H10 119.3 . . ? C12 C11 C16 119.6(3) . . ? C12 C11 C1 121.3(3) . . ? C16 C11 C1 119.1(3) . . ? C11 C12 C13 119.8(3) . . ? C11 C12 N1 122.0(3) . . ? C13 C12 N1 118.1(3) . . ? C14 C13 C12 120.9(4) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 121.2(4) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C20 122.1(4) . . ? C14 C15 C16 118.9(3) . . ? C20 C15 C16 119.0(4) . . ? C17 C16 C15 118.0(3) . . ? C17 C16 C11 122.3(3) . . ? C15 C16 C11 119.7(3) . . ? C18 C17 C16 121.3(4) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 120.3(4) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 120.0(4) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C15 121.3(4) . . ? C19 C20 H20 119.4 . . ? C15 C20 H20 119.4 . . ? C22 C21 N1 111.2(3) . . ? C22 C21 H21A 109.4 . . ? N1 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? N1 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C23 C22 N2 110.8(3) . . ? C23 C22 C21 131.5(3) . . ? N2 C22 C21 117.7(3) . . ? C22 C23 C24 106.4(3) . . ? C22 C23 H23 126.8 . . ? C24 C23 H23 126.8 . . ? C25 C24 C23 107.0(3) . . ? C25 C24 H24 126.5 . . ? C23 C24 H24 126.5 . . ? C24 C25 N2 110.4(3) . . ? C24 C25 H25 124.8 . . ? N2 C25 H25 124.8 . . ? C27 C26 C31 118.7(3) . . ? C27 C26 C36 121.5(3) . . ? C31 C26 C36 119.8(3) . . ? O2 C27 C26 120.6(3) . . ? O2 C27 C28 118.7(3) . . ? C26 C27 C28 120.7(3) . . ? C29 C28 C27 120.7(3) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 121.0(3) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C35 C30 C31 119.7(3) . . ? C35 C30 C29 121.4(3) . . ? C31 C30 C29 118.9(3) . . ? C32 C31 C30 118.0(3) . . ? C32 C31 C26 122.3(3) . . ? C30 C31 C26 119.7(3) . . ? C33 C32 C31 121.1(3) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C34 120.7(4) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C35 C34 C33 120.0(4) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C30 120.5(4) . . ? C34 C35 H35 119.7 . . ? C30 C35 H35 119.7 . . ? C37 C36 C41 119.0(3) . . ? C37 C36 C26 122.3(3) . . ? C41 C36 C26 118.7(3) . . ? C36 C37 C38 119.8(3) . . ? C36 C37 N3 121.7(3) . . ? C38 C37 N3 118.5(3) . . ? C39 C38 C37 121.7(4) . . ? C39 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? C38 C39 C40 120.9(3) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C39 C40 C45 121.8(3) . . ? C39 C40 C41 118.5(3) . . ? C45 C40 C41 119.7(3) . . ? C40 C41 C42 117.0(3) . . ? C40 C41 C36 120.1(3) . . ? C42 C41 C36 122.9(3) . . ? C43 C42 C41 121.4(3) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C42 C43 C44 121.2(4) . . ? C42 C43 H43 119.4 . . ? C44 C43 H43 119.4 . . ? C45 C44 C43 119.7(3) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C40 121.0(3) . . ? C44 C45 H45 119.5 . . ? C40 C45 H45 119.5 . . ? N3 C46 C47 112.2(3) . . ? N3 C46 H46A 109.2 . . ? C47 C46 H46A 109.2 . . ? N3 C46 H46B 109.2 . . ? C47 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? C48 C47 N4 109.8(3) . . ? C48 C47 C46 131.5(3) . . ? N4 C47 C46 118.5(3) . . ? C47 C48 C49 106.7(3) . . ? C47 C48 H48 126.6 . . ? C49 C48 H48 126.6 . . ? C50 C49 C48 107.0(3) . . ? C50 C49 H49 126.5 . . ? C48 C49 H49 126.5 . . ? C49 C50 N4 110.1(3) . . ? C49 C50 H50 124.9 . . ? N4 C50 H50 124.9 . . ? N5 C51 H51A 109.5 . . ? N5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N5 C52 H52A 109.5 . . ? N5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N6 C53 H53A 109.5 . . ? N6 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N6 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N6 C54 H54A 109.5 . . ? N6 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N6 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N7 C55 H55A 109.5 . . ? N7 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N7 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N7 C56 H56A 109.5 . . ? N7 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N7 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N8 C57 H57A 109.5 . . ? N8 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N8 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N8 C58 H58A 109.5 . . ? N8 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? N8 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N9 C59 H59A 109.5 . . ? N9 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? N9 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N9 C60 H60A 109.5 . . ? N9 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N9 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N10 C61 H61A 109.5 . . ? N10 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N10 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N10 C62 H62A 109.5 . . ? N10 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N10 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 H63A 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C64 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 C69 117.6(4) . . ? C65 C64 C63 120.8(4) . . ? C69 C64 C63 121.6(4) . . ? C66 C65 C64 121.1(4) . . ? C66 C65 H65 119.4 . . ? C64 C65 H65 119.4 . . ? C67 C66 C65 120.5(4) . . ? C67 C66 H66 119.8 . . ? C65 C66 H66 119.8 . . ? C66 C67 C68 119.6(5) . . ? C66 C67 H67 120.2 . . ? C68 C67 H67 120.2 . . ? C69 C68 C67 120.3(5) . . ? C69 C68 H68 119.9 . . ? C67 C68 H68 119.9 . . ? C68 C69 C64 120.9(4) . . ? C68 C69 H69 119.5 . . ? C64 C69 H69 119.5 . . ? C71 C70 H70A 109.5 . . ? C71 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C71 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C76 C71 C72 118.2(5) . . ? C76 C71 C70 123.0(5) . . ? C72 C71 C70 118.9(5) . . ? C73 C72 C71 119.7(4) . . ? C73 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C74 C73 C72 119.4(5) . . ? C74 C73 H73 120.3 . . ? C72 C73 H73 120.3 . . ? C73 C74 C75 121.0(5) . . ? C73 C74 H74 119.5 . . ? C75 C74 H74 119.5 . . ? C76 C75 C74 119.5(5) . . ? C76 C75 H75 120.2 . . ? C74 C75 H75 120.2 . . ? C75 C76 C71 122.2(5) . . ? C75 C76 H76 118.9 . . ? C71 C76 H76 118.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Zr1 Zr2 N3 155.80(14) . . . . ? N7 Zr1 Zr2 N3 -69.04(14) . . . . ? N4 Zr1 Zr2 N3 33.87(12) . . . . ? O1 Zr1 Zr2 N3 110.86(12) . . . . ? N5 Zr1 Zr2 N3 -132.37(14) . . . . ? N6 Zr1 Zr2 N1 30.27(14) . . . . ? N7 Zr1 Zr2 N1 165.44(14) . . . . ? N4 Zr1 Zr2 N1 -91.65(12) . . . . ? O1 Zr1 Zr2 N1 -14.67(12) . . . . ? N5 Zr1 Zr2 N1 102.10(14) . . . . ? N3 Zr1 Zr2 N1 -125.53(13) . . . . ? N6 Zr1 Zr2 O2 149.32(14) . . . . ? N7 Zr1 Zr2 O2 -75.52(14) . . . . ? N4 Zr1 Zr2 O2 27.39(12) . . . . ? O1 Zr1 Zr2 O2 104.37(13) . . . . ? N5 Zr1 Zr2 O2 -138.86(14) . . . . ? N3 Zr1 Zr2 O2 -6.48(13) . . . . ? N6 Zr1 Zr2 O1 44.94(14) . . . . ? N7 Zr1 Zr2 O1 -179.89(14) . . . . ? N4 Zr1 Zr2 O1 -76.98(12) . . . . ? N5 Zr1 Zr2 O1 116.77(14) . . . . ? N3 Zr1 Zr2 O1 -110.86(13) . . . . ? N6 Zr1 Zr2 N8 -96.46(16) . . . . ? N7 Zr1 Zr2 N8 38.70(15) . . . . ? N4 Zr1 Zr2 N8 141.61(13) . . . . ? O1 Zr1 Zr2 N8 -141.40(14) . . . . ? N5 Zr1 Zr2 N8 -24.64(15) . . . . ? N3 Zr1 Zr2 N8 107.74(14) . . . . ? N6 Zr1 Zr2 N5 -71.83(15) . . . . ? N7 Zr1 Zr2 N5 63.34(15) . . . . ? N4 Zr1 Zr2 N5 166.25(14) . . . . ? O1 Zr1 Zr2 N5 -116.77(14) . . . . ? N3 Zr1 Zr2 N5 132.37(14) . . . . ? N6 Zr1 Zr2 Zr3 -69.1(2) . . . . ? N7 Zr1 Zr2 Zr3 66.0(2) . . . . ? N4 Zr1 Zr2 Zr3 168.93(18) . . . . ? O1 Zr1 Zr2 Zr3 -114.09(19) . . . . ? N5 Zr1 Zr2 Zr3 2.7(2) . . . . ? N3 Zr1 Zr2 Zr3 135.06(19) . . . . ? N3 Zr2 Zr3 N9 32.05(15) . . . . ? N1 Zr2 Zr3 N9 156.52(14) . . . . ? O2 Zr2 Zr3 N9 44.68(14) . . . . ? O1 Zr2 Zr3 N9 150.78(14) . . . . ? N8 Zr2 Zr3 N9 -70.78(16) . . . . ? N5 Zr2 Zr3 N9 -97.83(15) . . . . ? Zr1 Zr2 Zr3 N9 -100.3(2) . . . . ? N3 Zr2 Zr3 N10 164.92(15) . . . . ? N1 Zr2 Zr3 N10 -70.60(15) . . . . ? O2 Zr2 Zr3 N10 177.56(15) . . . . ? O1 Zr2 Zr3 N10 -76.34(15) . . . . ? N8 Zr2 Zr3 N10 62.10(17) . . . . ? N5 Zr2 Zr3 N10 35.05(16) . . . . ? Zr1 Zr2 Zr3 N10 32.6(2) . . . . ? N3 Zr2 Zr3 N2 -90.02(12) . . . . ? N1 Zr2 Zr3 N2 34.45(12) . . . . ? O2 Zr2 Zr3 N2 -77.38(12) . . . . ? O1 Zr2 Zr3 N2 28.71(12) . . . . ? N8 Zr2 Zr3 N2 167.16(14) . . . . ? N5 Zr2 Zr3 N2 140.11(13) . . . . ? Zr1 Zr2 Zr3 N2 137.63(18) . . . . ? N3 Zr2 Zr3 O2 -12.64(13) . . . . ? N1 Zr2 Zr3 O2 111.84(12) . . . . ? O1 Zr2 Zr3 O2 106.10(13) . . . . ? N8 Zr2 Zr3 O2 -115.46(14) . . . . ? N5 Zr2 Zr3 O2 -142.51(13) . . . . ? Zr1 Zr2 Zr3 O2 -144.98(19) . . . . ? N3 Zr2 Zr3 N8 102.82(15) . . . . ? N1 Zr2 Zr3 N8 -132.71(14) . . . . ? O2 Zr2 Zr3 N8 115.46(14) . . . . ? O1 Zr2 Zr3 N8 -138.44(15) . . . . ? N5 Zr2 Zr3 N8 -27.05(15) . . . . ? Zr1 Zr2 Zr3 N8 -29.5(2) . . . . ? N3 Zr2 Zr3 N1 -124.47(13) . . . . ? O2 Zr2 Zr3 N1 -111.84(12) . . . . ? O1 Zr2 Zr3 N1 -5.74(12) . . . . ? N8 Zr2 Zr3 N1 132.71(14) . . . . ? N5 Zr2 Zr3 N1 105.65(13) . . . . ? Zr1 Zr2 Zr3 N1 103.18(19) . . . . ? N3 Zr2 O1 C2 111.2(3) . . . . ? N1 Zr2 O1 C2 -28.7(3) . . . . ? O2 Zr2 O1 C2 38.6(3) . . . . ? N8 Zr2 O1 C2 -106.0(3) . . . . ? N5 Zr2 O1 C2 -155.8(3) . . . . ? Zr3 Zr2 O1 C2 -24.1(3) . . . . ? Zr1 Zr2 O1 C2 162.8(3) . . . . ? N3 Zr2 O1 Zr1 -51.63(9) . . . . ? N1 Zr2 O1 Zr1 168.46(10) . . . . ? O2 Zr2 O1 Zr1 -124.27(10) . . . . ? N8 Zr2 O1 Zr1 91.2(2) . . . . ? N5 Zr2 O1 Zr1 41.39(9) . . . . ? Zr3 Zr2 O1 Zr1 173.05(2) . . . . ? N6 Zr1 O1 C2 53.8(3) . . . . ? N7 Zr1 O1 C2 -160.5(4) . . . . ? N4 Zr1 O1 C2 -51.1(3) . . . . ? N5 Zr1 O1 C2 159.0(3) . . . . ? N3 Zr1 O1 C2 -119.4(3) . . . . ? Zr2 Zr1 O1 C2 -160.8(3) . . . . ? N6 Zr1 O1 Zr2 -145.38(10) . . . . ? N7 Zr1 O1 Zr2 0.4(5) . . . . ? N4 Zr1 O1 Zr2 109.70(10) . . . . ? N5 Zr1 O1 Zr2 -40.13(9) . . . . ? N3 Zr1 O1 Zr2 41.45(8) . . . . ? N3 Zr2 O2 C27 -26.2(3) . . . . ? N1 Zr2 O2 C27 114.0(3) . . . . ? O1 Zr2 O2 C27 42.6(3) . . . . ? N8 Zr2 O2 C27 -154.2(3) . . . . ? N5 Zr2 O2 C27 -106.9(3) . . . . ? Zr3 Zr2 O2 C27 163.7(3) . . . . ? Zr1 Zr2 O2 C27 -20.9(3) . . . . ? N3 Zr2 O2 Zr3 170.13(10) . . . . ? N1 Zr2 O2 Zr3 -49.73(9) . . . . ? O1 Zr2 O2 Zr3 -121.09(10) . . . . ? N8 Zr2 O2 Zr3 42.13(10) . . . . ? N5 Zr2 O2 Zr3 89.4(2) . . . . ? Zr1 Zr2 O2 Zr3 175.44(2) . . . . ? N9 Zr3 O2 C27 52.5(3) . . . . ? N10 Zr3 O2 C27 -171.9(5) . . . . ? N2 Zr3 O2 C27 -51.6(3) . . . . ? N8 Zr3 O2 C27 156.3(3) . . . . ? N1 Zr3 O2 C27 -121.9(3) . . . . ? Zr2 Zr3 O2 C27 -163.0(3) . . . . ? N9 Zr3 O2 Zr2 -144.51(11) . . . . ? N10 Zr3 O2 Zr2 -8.9(5) . . . . ? N2 Zr3 O2 Zr2 111.42(10) . . . . ? N8 Zr3 O2 Zr2 -40.64(9) . . . . ? N1 Zr3 O2 Zr2 41.14(8) . . . . ? N3 Zr2 N1 C12 -125.0(2) . . . . ? O2 Zr2 N1 C12 165.9(2) . . . . ? O1 Zr2 N1 C12 -58.5(2) . . . . ? N8 Zr2 N1 C12 94.0(2) . . . . ? N5 Zr2 N1 C12 7.4(2) . . . . ? Zr3 Zr2 N1 C12 125.3(2) . . . . ? Zr1 Zr2 N1 C12 -48.5(2) . . . . ? N3 Zr2 N1 C21 11.9(3) . . . . ? O2 Zr2 N1 C21 -57.2(2) . . . . ? O1 Zr2 N1 C21 78.4(2) . . . . ? N8 Zr2 N1 C21 -129.1(3) . . . . ? N5 Zr2 N1 C21 144.3(2) . . . . ? Zr3 Zr2 N1 C21 -97.8(3) . . . . ? Zr1 Zr2 N1 C21 88.3(2) . . . . ? N3 Zr2 N1 Zr3 109.75(14) . . . . ? O2 Zr2 N1 Zr3 40.64(7) . . . . ? O1 Zr2 N1 Zr3 176.23(8) . . . . ? N8 Zr2 N1 Zr3 -31.29(9) . . . . ? N5 Zr2 N1 Zr3 -117.91(10) . . . . ? Zr1 Zr2 N1 Zr3 -173.826(18) . . . . ? N9 Zr3 N1 C12 -168.2(3) . . . . ? N10 Zr3 N1 C12 16.0(3) . . . . ? N2 Zr3 N1 C12 102.8(2) . . . . ? O2 Zr3 N1 C12 -153.7(3) . . . . ? N8 Zr3 N1 C12 -80.2(2) . . . . ? Zr2 Zr3 N1 C12 -111.1(3) . . . . ? N9 Zr3 N1 C21 66.9(3) . . . . ? N10 Zr3 N1 C21 -108.9(2) . . . . ? N2 Zr3 N1 C21 -22.05(18) . . . . ? O2 Zr3 N1 C21 81.46(18) . . . . ? N8 Zr3 N1 C21 155.0(2) . . . . ? Zr2 Zr3 N1 C21 124.1(2) . . . . ? N9 Zr3 N1 Zr2 -57.2(3) . . . . ? N10 Zr3 N1 Zr2 127.06(12) . . . . ? N2 Zr3 N1 Zr2 -146.12(11) . . . . ? O2 Zr3 N1 Zr2 -42.61(8) . . . . ? N8 Zr3 N1 Zr2 30.90(9) . . . . ? N9 Zr3 N2 C22 -159.0(2) . . . . ? N10 Zr3 N2 C22 103.0(2) . . . . ? O2 Zr3 N2 C22 -65.7(2) . . . . ? N8 Zr3 N2 C22 -8.2(4) . . . . ? N1 Zr3 N2 C22 -2.7(2) . . . . ? Zr2 Zr3 N2 C22 -25.0(2) . . . . ? N9 Zr3 N2 C25 56.2(3) . . . . ? N10 Zr3 N2 C25 -41.8(3) . . . . ? O2 Zr3 N2 C25 149.5(3) . . . . ? N8 Zr3 N2 C25 -153.1(3) . . . . ? N1 Zr3 N2 C25 -147.5(3) . . . . ? Zr2 Zr3 N2 C25 -169.8(3) . . . . ? N1 Zr2 N3 C37 -125.3(2) . . . . ? O2 Zr2 N3 C37 -59.9(2) . . . . ? O1 Zr2 N3 C37 164.9(2) . . . . ? N8 Zr2 N3 C37 5.1(3) . . . . ? N5 Zr2 N3 C37 92.7(2) . . . . ? Zr3 Zr2 N3 C37 -51.3(2) . . . . ? Zr1 Zr2 N3 C37 124.1(2) . . . . ? N1 Zr2 N3 C46 11.6(3) . . . . ? O2 Zr2 N3 C46 77.0(2) . . . . ? O1 Zr2 N3 C46 -58.2(2) . . . . ? N8 Zr2 N3 C46 142.1(2) . . . . ? N5 Zr2 N3 C46 -130.3(3) . . . . ? Zr3 Zr2 N3 C46 85.6(3) . . . . ? Zr1 Zr2 N3 C46 -98.9(3) . . . . ? N1 Zr2 N3 Zr1 110.54(13) . . . . ? O2 Zr2 N3 Zr1 175.92(8) . . . . ? O1 Zr2 N3 Zr1 40.73(7) . . . . ? N8 Zr2 N3 Zr1 -119.00(11) . . . . ? N5 Zr2 N3 Zr1 -31.44(9) . . . . ? Zr3 Zr2 N3 Zr1 -175.490(19) . . . . ? N6 Zr1 N3 C37 -171.5(3) . . . . ? N7 Zr1 N3 C37 17.9(3) . . . . ? N4 Zr1 N3 C37 104.8(2) . . . . ? O1 Zr1 N3 C37 -153.0(3) . . . . ? N5 Zr1 N3 C37 -78.4(2) . . . . ? Zr2 Zr1 N3 C37 -109.8(2) . . . . ? N6 Zr1 N3 C46 61.1(3) . . . . ? N7 Zr1 N3 C46 -109.5(2) . . . . ? N4 Zr1 N3 C46 -22.63(19) . . . . ? O1 Zr1 N3 C46 79.6(2) . . . . ? N5 Zr1 N3 C46 154.2(2) . . . . ? Zr2 Zr1 N3 C46 122.8(2) . . . . ? N6 Zr1 N3 Zr2 -61.8(3) . . . . ? N7 Zr1 N3 Zr2 127.62(11) . . . . ? N4 Zr1 N3 Zr2 -145.48(12) . . . . ? O1 Zr1 N3 Zr2 -43.26(8) . . . . ? N5 Zr1 N3 Zr2 31.31(9) . . . . ? N6 Zr1 N4 C47 -155.2(3) . . . . ? N7 Zr1 N4 C47 106.8(3) . . . . ? O1 Zr1 N4 C47 -60.4(3) . . . . ? N5 Zr1 N4 C47 -3.2(4) . . . . ? N3 Zr1 N4 C47 2.3(2) . . . . ? Zr2 Zr1 N4 C47 -19.9(3) . . . . ? N6 Zr1 N4 C50 44.8(3) . . . . ? N7 Zr1 N4 C50 -53.2(3) . . . . ? O1 Zr1 N4 C50 139.5(3) . . . . ? N5 Zr1 N4 C50 -163.3(3) . . . . ? N3 Zr1 N4 C50 -157.7(3) . . . . ? Zr2 Zr1 N4 C50 -179.9(3) . . . . ? N3 Zr2 N5 C51 147.0(2) . . . . ? N1 Zr2 N5 C51 -2.6(3) . . . . ? O2 Zr2 N5 C51 -132.9(2) . . . . ? O1 Zr2 N5 C51 70.2(2) . . . . ? N8 Zr2 N5 C51 -88.6(3) . . . . ? Zr3 Zr2 N5 C51 -69.9(3) . . . . ? Zr1 Zr2 N5 C51 109.8(3) . . . . ? N3 Zr2 N5 C52 -81.9(3) . . . . ? N1 Zr2 N5 C52 128.5(3) . . . . ? O2 Zr2 N5 C52 -1.8(4) . . . . ? O1 Zr2 N5 C52 -158.7(3) . . . . ? N8 Zr2 N5 C52 42.5(3) . . . . ? Zr3 Zr2 N5 C52 61.2(3) . . . . ? Zr1 Zr2 N5 C52 -119.1(3) . . . . ? N3 Zr2 N5 Zr1 37.18(11) . . . . ? N1 Zr2 N5 Zr1 -112.41(11) . . . . ? O2 Zr2 N5 Zr1 117.31(17) . . . . ? O1 Zr2 N5 Zr1 -39.61(9) . . . . ? N8 Zr2 N5 Zr1 161.57(11) . . . . ? Zr3 Zr2 N5 Zr1 -179.70(2) . . . . ? N6 Zr1 N5 C51 9.4(2) . . . . ? N7 Zr1 N5 C51 109.9(2) . . . . ? N4 Zr1 N5 C51 -142.4(2) . . . . ? O1 Zr1 N5 C51 -78.9(2) . . . . ? N3 Zr1 N5 C51 -147.8(2) . . . . ? Zr2 Zr1 N5 C51 -118.3(2) . . . . ? N6 Zr1 N5 C52 -107.3(2) . . . . ? N7 Zr1 N5 C52 -6.8(3) . . . . ? N4 Zr1 N5 C52 100.9(3) . . . . ? O1 Zr1 N5 C52 164.4(3) . . . . ? N3 Zr1 N5 C52 95.5(2) . . . . ? Zr2 Zr1 N5 C52 125.1(3) . . . . ? N6 Zr1 N5 Zr2 127.65(12) . . . . ? N7 Zr1 N5 Zr2 -131.81(11) . . . . ? N4 Zr1 N5 Zr2 -24.1(2) . . . . ? O1 Zr1 N5 Zr2 39.33(9) . . . . ? N3 Zr1 N5 Zr2 -29.57(9) . . . . ? N7 Zr1 N6 C53 -166.4(3) . . . . ? N4 Zr1 N6 C53 100.0(3) . . . . ? O1 Zr1 N6 C53 5.9(3) . . . . ? N5 Zr1 N6 C53 -64.1(3) . . . . ? N3 Zr1 N6 C53 22.8(5) . . . . ? Zr2 Zr1 N6 C53 -22.2(4) . . . . ? N7 Zr1 N6 C54 13.0(3) . . . . ? N4 Zr1 N6 C54 -80.6(3) . . . . ? O1 Zr1 N6 C54 -174.7(3) . . . . ? N5 Zr1 N6 C54 115.3(3) . . . . ? N3 Zr1 N6 C54 -157.9(3) . . . . ? Zr2 Zr1 N6 C54 157.2(2) . . . . ? N6 Zr1 N7 C55 49.6(3) . . . . ? N4 Zr1 N7 C55 154.6(3) . . . . ? O1 Zr1 N7 C55 -95.9(5) . . . . ? N5 Zr1 N7 C55 -57.7(3) . . . . ? N3 Zr1 N7 C55 -134.0(3) . . . . ? Zr2 Zr1 N7 C55 -95.6(3) . . . . ? N6 Zr1 N7 C56 -127.3(3) . . . . ? N4 Zr1 N7 C56 -22.3(3) . . . . ? O1 Zr1 N7 C56 87.2(5) . . . . ? N5 Zr1 N7 C56 125.4(3) . . . . ? N3 Zr1 N7 C56 49.2(3) . . . . ? Zr2 Zr1 N7 C56 87.5(3) . . . . ? N3 Zr2 N8 C58 128.0(3) . . . . ? N1 Zr2 N8 C58 -83.4(3) . . . . ? O2 Zr2 N8 C58 -159.7(3) . . . . ? O1 Zr2 N8 C58 -6.5(4) . . . . ? N5 Zr2 N8 C58 40.3(3) . . . . ? Zr3 Zr2 N8 C58 -119.4(3) . . . . ? Zr1 Zr2 N8 C58 57.4(3) . . . . ? N3 Zr2 N8 C57 -2.0(3) . . . . ? N1 Zr2 N8 C57 146.6(3) . . . . ? O2 Zr2 N8 C57 70.3(2) . . . . ? O1 Zr2 N8 C57 -136.4(2) . . . . ? N5 Zr2 N8 C57 -89.7(2) . . . . ? Zr3 Zr2 N8 C57 110.6(3) . . . . ? Zr1 Zr2 N8 C57 -72.6(3) . . . . ? N3 Zr2 N8 Zr3 -112.61(12) . . . . ? N1 Zr2 N8 Zr3 35.96(11) . . . . ? O2 Zr2 N8 Zr3 -40.35(9) . . . . ? O1 Zr2 N8 Zr3 112.92(18) . . . . ? N5 Zr2 N8 Zr3 159.64(11) . . . . ? Zr1 Zr2 N8 Zr3 176.76(2) . . . . ? N9 Zr3 N8 C58 -106.3(3) . . . . ? N10 Zr3 N8 C58 -6.0(3) . . . . ? N2 Zr3 N8 C58 103.0(3) . . . . ? O2 Zr3 N8 C58 167.1(3) . . . . ? N1 Zr3 N8 C58 97.4(3) . . . . ? Zr2 Zr3 N8 C58 127.0(3) . . . . ? N9 Zr3 N8 C57 9.3(2) . . . . ? N10 Zr3 N8 C57 109.6(2) . . . . ? N2 Zr3 N8 C57 -141.5(2) . . . . ? O2 Zr3 N8 C57 -77.4(2) . . . . ? N1 Zr3 N8 C57 -147.0(2) . . . . ? Zr2 Zr3 N8 C57 -117.4(2) . . . . ? N9 Zr3 N8 Zr2 126.72(12) . . . . ? N10 Zr3 N8 Zr2 -132.99(13) . . . . ? N2 Zr3 N8 Zr2 -24.0(2) . . . . ? O2 Zr3 N8 Zr2 40.08(9) . . . . ? N1 Zr3 N8 Zr2 -29.56(9) . . . . ? N10 Zr3 N9 C59 -157.5(3) . . . . ? N2 Zr3 N9 C59 109.4(3) . . . . ? O2 Zr3 N9 C59 13.3(3) . . . . ? N8 Zr3 N9 C59 -55.4(4) . . . . ? N1 Zr3 N9 C59 26.6(5) . . . . ? Zr2 Zr3 N9 C59 -14.6(4) . . . . ? N10 Zr3 N9 C60 21.3(3) . . . . ? N2 Zr3 N9 C60 -71.8(3) . . . . ? O2 Zr3 N9 C60 -167.9(3) . . . . ? N8 Zr3 N9 C60 123.4(3) . . . . ? N1 Zr3 N9 C60 -154.6(3) . . . . ? Zr2 Zr3 N9 C60 164.2(3) . . . . ? N9 Zr3 N10 C61 47.3(4) . . . . ? N2 Zr3 N10 C61 151.4(4) . . . . ? O2 Zr3 N10 C61 -87.9(6) . . . . ? N8 Zr3 N10 C61 -58.0(4) . . . . ? N1 Zr3 N10 C61 -134.4(3) . . . . ? Zr2 Zr3 N10 C61 -95.1(3) . . . . ? N9 Zr3 N10 C62 -130.1(3) . . . . ? N2 Zr3 N10 C62 -26.0(3) . . . . ? O2 Zr3 N10 C62 94.7(6) . . . . ? N8 Zr3 N10 C62 124.6(3) . . . . ? N1 Zr3 N10 C62 48.2(4) . . . . ? Zr2 Zr3 N10 C62 87.5(3) . . . . ? C6 C1 C2 O1 -170.0(3) . . . . ? C11 C1 C2 O1 5.6(5) . . . . ? C6 C1 C2 C3 9.8(5) . . . . ? C11 C1 C2 C3 -174.7(3) . . . . ? Zr2 O1 C2 C1 63.8(4) . . . . ? Zr1 O1 C2 C1 -140.5(3) . . . . ? Zr2 O1 C2 C3 -116.0(3) . . . . ? Zr1 O1 C2 C3 39.7(4) . . . . ? C1 C2 C3 C4 -7.5(5) . . . . ? O1 C2 C3 C4 172.3(3) . . . . ? C2 C3 C4 C5 -0.7(6) . . . . ? C3 C4 C5 C10 -171.5(4) . . . . ? C3 C4 C5 C6 6.0(6) . . . . ? C4 C5 C6 C7 -176.9(3) . . . . ? C10 C5 C6 C7 0.7(5) . . . . ? C4 C5 C6 C1 -3.5(5) . . . . ? C10 C5 C6 C1 174.1(3) . . . . ? C2 C1 C6 C7 168.8(4) . . . . ? C11 C1 C6 C7 -6.8(5) . . . . ? C2 C1 C6 C5 -4.3(5) . . . . ? C11 C1 C6 C5 -179.8(3) . . . . ? C5 C6 C7 C8 1.9(6) . . . . ? C1 C6 C7 C8 -171.3(4) . . . . ? C6 C7 C8 C9 -2.8(7) . . . . ? C7 C8 C9 C10 1.1(7) . . . . ? C8 C9 C10 C5 1.5(7) . . . . ? C4 C5 C10 C9 175.1(4) . . . . ? C6 C5 C10 C9 -2.4(6) . . . . ? C2 C1 C11 C12 -66.0(5) . . . . ? C6 C1 C11 C12 109.5(4) . . . . ? C2 C1 C11 C16 113.3(4) . . . . ? C6 C1 C11 C16 -71.2(4) . . . . ? C16 C11 C12 C13 1.9(5) . . . . ? C1 C11 C12 C13 -178.9(3) . . . . ? C16 C11 C12 N1 -176.4(3) . . . . ? C1 C11 C12 N1 2.9(5) . . . . ? C21 N1 C12 C11 -58.6(4) . . . . ? Zr2 N1 C12 C11 83.6(3) . . . . ? Zr3 N1 C12 C11 -177.0(2) . . . . ? C21 N1 C12 C13 123.1(3) . . . . ? Zr2 N1 C12 C13 -94.7(3) . . . . ? Zr3 N1 C12 C13 4.8(4) . . . . ? C11 C12 C13 C14 -2.3(6) . . . . ? N1 C12 C13 C14 176.1(3) . . . . ? C12 C13 C14 C15 1.8(6) . . . . ? C13 C14 C15 C20 178.0(4) . . . . ? C13 C14 C15 C16 -1.0(6) . . . . ? C14 C15 C16 C17 -179.3(3) . . . . ? C20 C15 C16 C17 1.7(5) . . . . ? C14 C15 C16 C11 0.6(5) . . . . ? C20 C15 C16 C11 -178.4(3) . . . . ? C12 C11 C16 C17 178.8(3) . . . . ? C1 C11 C16 C17 -0.5(5) . . . . ? C12 C11 C16 C15 -1.1(5) . . . . ? C1 C11 C16 C15 179.7(3) . . . . ? C15 C16 C17 C18 -1.0(5) . . . . ? C11 C16 C17 C18 179.1(3) . . . . ? C16 C17 C18 C19 -0.3(6) . . . . ? C17 C18 C19 C20 0.8(6) . . . . ? C18 C19 C20 C15 -0.1(6) . . . . ? C14 C15 C20 C19 179.8(4) . . . . ? C16 C15 C20 C19 -1.2(6) . . . . ? C12 N1 C21 C22 -90.0(3) . . . . ? Zr2 N1 C21 C22 134.5(2) . . . . ? Zr3 N1 C21 C22 42.8(3) . . . . ? C25 N2 C22 C23 1.3(4) . . . . ? Zr3 N2 C22 C23 -151.5(2) . . . . ? C25 N2 C22 C21 -176.5(3) . . . . ? Zr3 N2 C22 C21 30.6(4) . . . . ? N1 C21 C22 C23 127.8(4) . . . . ? N1 C21 C22 N2 -54.9(4) . . . . ? N2 C22 C23 C24 -1.2(4) . . . . ? C21 C22 C23 C24 176.2(3) . . . . ? C22 C23 C24 C25 0.6(4) . . . . ? C23 C24 C25 N2 0.2(4) . . . . ? C22 N2 C25 C24 -0.9(4) . . . . ? Zr3 N2 C25 C24 146.9(3) . . . . ? Zr2 O2 C27 C26 60.4(4) . . . . ? Zr3 O2 C27 C26 -141.8(3) . . . . ? Zr2 O2 C27 C28 -120.7(3) . . . . ? Zr3 O2 C27 C28 37.0(4) . . . . ? C31 C26 C27 O2 -174.3(3) . . . . ? C36 C26 C27 O2 6.5(5) . . . . ? C31 C26 C27 C28 6.9(5) . . . . ? C36 C26 C27 C28 -172.3(3) . . . . ? O2 C27 C28 C29 177.1(3) . . . . ? C26 C27 C28 C29 -4.0(5) . . . . ? C27 C28 C29 C30 -0.2(5) . . . . ? C28 C29 C30 C35 -177.8(4) . . . . ? C28 C29 C30 C31 1.3(5) . . . . ? C35 C30 C31 C32 1.6(5) . . . . ? C29 C30 C31 C32 -177.5(3) . . . . ? C35 C30 C31 C26 -179.2(3) . . . . ? C29 C30 C31 C26 1.7(5) . . . . ? C27 C26 C31 C32 173.4(3) . . . . ? C36 C26 C31 C32 -7.4(5) . . . . ? C27 C26 C31 C30 -5.8(5) . . . . ? C36 C26 C31 C30 173.5(3) . . . . ? C30 C31 C32 C33 -2.0(5) . . . . ? C26 C31 C32 C33 178.9(3) . . . . ? C31 C32 C33 C34 0.6(6) . . . . ? C32 C33 C34 C35 1.3(6) . . . . ? C33 C34 C35 C30 -1.6(6) . . . . ? C31 C30 C35 C34 0.2(6) . . . . ? C29 C30 C35 C34 179.2(4) . . . . ? C27 C26 C36 C37 -65.3(5) . . . . ? C31 C26 C36 C37 115.5(4) . . . . ? C27 C26 C36 C41 113.7(4) . . . . ? C31 C26 C36 C41 -65.6(4) . . . . ? C41 C36 C37 C38 1.2(5) . . . . ? C26 C36 C37 C38 -179.8(3) . . . . ? C41 C36 C37 N3 -175.8(3) . . . . ? C26 C36 C37 N3 3.2(5) . . . . ? C46 N3 C37 C36 -58.6(4) . . . . ? Zr2 N3 C37 C36 82.9(3) . . . . ? Zr1 N3 C37 C36 180.0(2) . . . . ? C46 N3 C37 C38 124.4(3) . . . . ? Zr2 N3 C37 C38 -94.2(3) . . . . ? Zr1 N3 C37 C38 2.9(4) . . . . ? C36 C37 C38 C39 -1.2(5) . . . . ? N3 C37 C38 C39 175.9(3) . . . . ? C37 C38 C39 C40 -0.5(5) . . . . ? C38 C39 C40 C45 -179.0(3) . . . . ? C38 C39 C40 C41 2.0(5) . . . . ? C39 C40 C41 C42 178.9(3) . . . . ? C45 C40 C41 C42 -0.1(5) . . . . ? C39 C40 C41 C36 -1.9(5) . . . . ? C45 C40 C41 C36 179.1(3) . . . . ? C37 C36 C41 C40 0.3(5) . . . . ? C26 C36 C41 C40 -178.7(3) . . . . ? C37 C36 C41 C42 179.4(3) . . . . ? C26 C36 C41 C42 0.4(5) . . . . ? C40 C41 C42 C43 -0.7(5) . . . . ? C36 C41 C42 C43 -179.8(3) . . . . ? C41 C42 C43 C44 0.6(5) . . . . ? C42 C43 C44 C45 0.3(5) . . . . ? C43 C44 C45 C40 -1.0(5) . . . . ? C39 C40 C45 C44 -178.1(3) . . . . ? C41 C40 C45 C44 0.9(5) . . . . ? C37 N3 C46 C47 -95.0(3) . . . . ? Zr2 N3 C46 C47 129.7(3) . . . . ? Zr1 N3 C46 C47 39.0(3) . . . . ? C50 N4 C47 C48 0.2(4) . . . . ? Zr1 N4 C47 C48 -163.8(2) . . . . ? C50 N4 C47 C46 -175.1(3) . . . . ? Zr1 N4 C47 C46 20.9(4) . . . . ? N3 C46 C47 C48 140.9(4) . . . . ? N3 C46 C47 N4 -45.1(4) . . . . ? N4 C47 C48 C49 -0.5(4) . . . . ? C46 C47 C48 C49 174.0(4) . . . . ? C47 C48 C49 C50 0.6(5) . . . . ? C48 C49 C50 N4 -0.5(5) . . . . ? C47 N4 C50 C49 0.2(4) . . . . ? Zr1 N4 C50 C49 162.6(3) . . . . ? C69 C64 C65 C66 0.0(6) . . . . ? C63 C64 C65 C66 -178.8(4) . . . . ? C64 C65 C66 C67 0.7(7) . . . . ? C65 C66 C67 C68 -1.3(7) . . . . ? C66 C67 C68 C69 1.2(7) . . . . ? C67 C68 C69 C64 -0.5(7) . . . . ? C65 C64 C69 C68 -0.1(6) . . . . ? C63 C64 C69 C68 178.7(4) . . . . ? C76 C71 C72 C73 -1.1(6) . . . . ? C70 C71 C72 C73 178.9(4) . . . . ? C71 C72 C73 C74 0.4(6) . . . . ? C72 C73 C74 C75 0.7(7) . . . . ? C73 C74 C75 C76 -0.9(7) . . . . ? C74 C75 C76 C71 0.1(7) . . . . ? C72 C71 C76 C75 0.9(7) . . . . ? C70 C71 C76 C75 -179.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.404 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.070 # Attachment 'H8-NOBIN.cif' data_H8NOBIN _database_code_depnum_ccdc_archive 'CCDC 687856' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H23 N O' _chemical_formula_sum 'C20 H23 N O' _chemical_formula_weight 293.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.2551(19) _cell_length_b 8.463(2) _cell_length_c 22.725(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1587.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 2627 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 22.26 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9852 _exptl_absorpt_correction_T_max 0.9881 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9169 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.43 _reflns_number_total 1895 _reflns_number_gt 1360 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.2380P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'None, Friedel Pairs merged' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1895 _refine_ls_number_parameters 218 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.1184(3) 0.3484(3) 0.89549(9) 0.0670(7) Uani 0.50 1 d P A 1 N1 N 0.0814(3) 0.7160(3) 0.84098(10) 0.0738(8) Uani 0.50 1 d P A 1 H1A H 0.0582 0.8051 0.8210 0.089 Uiso 0.75 1 d PR A 1 H1B H 0.0702 0.7134 0.8804 0.089 Uiso 0.75 1 d PR A 1 N1' N -0.1184(3) 0.3484(3) 0.89549(9) 0.0670(7) Uani 0.50 1 d P A 2 H1'A H -0.1067 0.3486 0.8559 0.080 Uiso 0.75 1 d PR A 2 H1'B H -0.2131 0.3148 0.9112 0.080 Uiso 0.75 1 d PR A 2 O1' O 0.0814(3) 0.7160(3) 0.84098(10) 0.0738(8) Uani 0.50 1 d P A 2 C1 C 0.0079(3) 0.3948(3) 0.93169(11) 0.0448(6) Uani 1 1 d . . . C2 C -0.0103(4) 0.3912(4) 0.99210(12) 0.0532(7) Uani 1 1 d . A . H2A H -0.1072 0.3572 1.0087 0.064 Uiso 1 1 calc R . . C3 C 0.1154(4) 0.4379(3) 1.02745(11) 0.0522(7) Uani 1 1 d . . . H3 H 0.1024 0.4331 1.0681 0.063 Uiso 1 1 calc R A . C4 C 0.2618(3) 0.4920(3) 1.00483(10) 0.0443(6) Uani 1 1 d . A . C5 C 0.3956(4) 0.5460(4) 1.04541(12) 0.0608(8) Uani 1 1 d D . . H5A H 0.3994 0.4758 1.0791 0.073 Uiso 1 1 calc R A 1 H5B H 0.3698 0.6510 1.0597 0.073 Uiso 1 1 calc R A 1 C6 C 0.5610(8) 0.5498(15) 1.0169(3) 0.064(2) Uani 0.615(16) 1 d PD A 1 H6A H 0.6010 0.4429 1.0117 0.077 Uiso 0.615(16) 1 calc PR A 1 H6B H 0.6364 0.6065 1.0419 0.077 Uiso 0.615(16) 1 calc PR A 1 C7 C 0.548(2) 0.6314(16) 0.9576(6) 0.075(3) Uani 0.615(16) 1 d PD A 1 H7A H 0.5091 0.7384 0.9635 0.090 Uiso 0.615(16) 1 calc PR A 1 H7B H 0.6550 0.6379 0.9401 0.090 Uiso 0.615(16) 1 calc PR A 1 C6' C 0.5247(17) 0.644(2) 1.0163(4) 0.069(4) Uani 0.385(16) 1 d PD A 2 H6'A H 0.6173 0.6531 1.0424 0.083 Uiso 0.385(16) 1 calc PR A 2 H6'B H 0.4835 0.7488 1.0085 0.083 Uiso 0.385(16) 1 calc PR A 2 C7' C 0.577(3) 0.566(3) 0.9589(9) 0.072(5) Uani 0.385(16) 1 d PD A 2 H7'A H 0.6612 0.6298 0.9408 0.086 Uiso 0.385(16) 1 calc PR A 2 H7'B H 0.6220 0.4629 0.9672 0.086 Uiso 0.385(16) 1 calc PR A 2 C8 C 0.4383(3) 0.5489(4) 0.91650(12) 0.0589(8) Uani 1 1 d . . . H8A H 0.4943 0.4577 0.9005 0.071 Uiso 1 1 calc R A 1 H8B H 0.4137 0.6191 0.8840 0.071 Uiso 1 1 calc R A 1 C9 C 0.2809(3) 0.4943(3) 0.94381(10) 0.0404(6) Uani 1 1 d . A . C10 C 0.1545(3) 0.4442(3) 0.90717(10) 0.0406(6) Uani 1 1 d . A . C11 C 0.1736(3) 0.4462(3) 0.84159(10) 0.0418(6) Uani 1 1 d . . . C12 C 0.2310(3) 0.3132(3) 0.81154(11) 0.0431(6) Uani 1 1 d . A . C13 C 0.2680(4) 0.1632(4) 0.84512(12) 0.0572(8) Uani 1 1 d . . . H13A H 0.3223 0.1910 0.8815 0.069 Uiso 1 1 calc R A . H13B H 0.1666 0.1121 0.8553 0.069 Uiso 1 1 calc R . . C14 C 0.3717(5) 0.0476(5) 0.81214(15) 0.0827(11) Uani 1 1 d . A . H14A H 0.4831 0.0840 0.8125 0.099 Uiso 1 1 calc R . . H14B H 0.3680 -0.0540 0.8318 0.099 Uiso 1 1 calc R . . C15 C 0.3171(5) 0.0281(5) 0.74998(16) 0.0856(12) Uani 1 1 d . . . H15A H 0.2071 -0.0121 0.7496 0.103 Uiso 1 1 calc R A . H15B H 0.3858 -0.0488 0.7305 0.103 Uiso 1 1 calc R . . C16 C 0.3234(5) 0.1810(5) 0.71692(13) 0.0747(10) Uani 1 1 d . A . H16A H 0.2649 0.1688 0.6802 0.090 Uiso 1 1 calc R . . H16B H 0.4354 0.2045 0.7074 0.090 Uiso 1 1 calc R . . C17 C 0.2523(3) 0.3195(4) 0.75043(11) 0.0516(7) Uani 1 1 d . . . C18 C 0.2095(4) 0.4568(4) 0.72156(11) 0.0590(9) Uani 1 1 d . A . H18 H 0.2203 0.4607 0.6809 0.071 Uiso 1 1 calc R . . C19 C 0.1517(4) 0.5878(4) 0.75026(13) 0.0599(8) Uani 1 1 d . . . H19 H 0.1242 0.6784 0.7293 0.072 Uiso 1 1 calc R A . C20 C 0.1349(3) 0.5832(3) 0.81101(11) 0.0494(7) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0469(12) 0.0951(19) 0.0591(14) -0.0031(13) -0.0021(11) -0.0152(13) N1 0.104(2) 0.0560(15) 0.0610(14) 0.0029(12) -0.0048(14) 0.0214(15) N1' 0.0469(12) 0.0951(19) 0.0591(14) -0.0031(13) -0.0021(11) -0.0152(13) O1' 0.104(2) 0.0560(15) 0.0610(14) 0.0029(12) -0.0048(14) 0.0214(15) C1 0.0425(14) 0.0479(16) 0.0439(14) 0.0007(12) 0.0031(12) 0.0004(13) C2 0.0495(16) 0.0614(18) 0.0487(16) 0.0044(14) 0.0152(14) 0.0014(15) C3 0.0643(18) 0.0579(17) 0.0346(13) 0.0014(13) 0.0105(14) 0.0077(15) C4 0.0520(16) 0.0461(15) 0.0346(12) -0.0027(11) 0.0012(11) 0.0059(13) C5 0.071(2) 0.067(2) 0.0441(15) -0.0068(15) -0.0068(15) 0.0027(18) C6 0.059(3) 0.072(6) 0.060(4) -0.011(4) -0.017(3) -0.007(3) C7 0.059(8) 0.090(8) 0.075(6) -0.019(5) 0.010(5) -0.027(6) C6' 0.081(8) 0.062(8) 0.065(7) -0.003(6) -0.016(5) -0.024(7) C7' 0.049(7) 0.105(15) 0.062(8) -0.026(9) -0.007(5) 0.003(10) C8 0.0508(17) 0.078(2) 0.0480(15) 0.0000(15) 0.0025(13) -0.0115(16) C9 0.0436(14) 0.0427(14) 0.0348(12) -0.0003(11) 0.0044(11) 0.0035(12) C10 0.0450(14) 0.0430(15) 0.0337(12) -0.0003(11) 0.0010(11) 0.0046(12) C11 0.0389(14) 0.0523(16) 0.0341(12) 0.0000(12) -0.0009(11) -0.0021(12) C12 0.0374(14) 0.0556(17) 0.0363(13) -0.0008(12) -0.0001(11) -0.0003(13) C13 0.0642(19) 0.0572(18) 0.0502(16) -0.0017(14) 0.0019(15) 0.0113(16) C14 0.092(3) 0.079(3) 0.077(2) -0.013(2) 0.007(2) 0.030(2) C15 0.094(3) 0.087(3) 0.076(2) -0.031(2) 0.006(2) 0.022(2) C16 0.077(2) 0.099(3) 0.0482(17) -0.0250(19) 0.0138(17) -0.007(2) C17 0.0484(16) 0.069(2) 0.0378(14) -0.0081(14) 0.0035(13) -0.0145(15) C18 0.0628(18) 0.085(2) 0.0294(12) 0.0048(15) -0.0028(13) -0.0217(18) C19 0.0653(19) 0.068(2) 0.0467(16) 0.0150(16) -0.0101(15) -0.0094(17) C20 0.0516(16) 0.0532(17) 0.0432(14) 0.0028(13) -0.0050(13) 0.0007(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.385(3) . ? O1 H1'A 0.9048 . ? O1 H1'B 0.9050 . ? N1 C20 1.386(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C1 C2 1.381(4) . ? C1 C10 1.397(4) . ? C2 C3 1.370(4) . ? C2 H2A 0.9300 . ? C3 C4 1.390(4) . ? C3 H3 0.9300 . ? C4 C9 1.396(3) . ? C4 C5 1.510(4) . ? C5 C6' 1.502(8) . ? C5 C6 1.511(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.519(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.478(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C6' C7' 1.522(9) . ? C6' H6'A 0.9700 . ? C6' H6'B 0.9700 . ? C7' C8 1.50(2) . ? C7' H7'A 0.9700 . ? C7' H7'B 0.9700 . ? C8 C9 1.512(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.400(3) . ? C10 C11 1.499(3) . ? C11 C20 1.389(4) . ? C11 C12 1.399(4) . ? C12 C17 1.401(3) . ? C12 C13 1.512(4) . ? C13 C14 1.501(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.492(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.497(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.516(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.381(4) . ? C18 C19 1.372(4) . ? C18 H18 0.9300 . ? C19 C20 1.388(4) . ? C19 H19 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 H1'A 120.7 . . ? C1 O1 H1'B 120.4 . . ? H1'A O1 H1'B 118.9 . . ? C20 N1 H1A 119.9 . . ? C20 N1 H1B 120.1 . . ? H1A N1 H1B 120.0 . . ? C2 C1 O1 120.2(3) . . ? C2 C1 C10 119.8(3) . . ? O1 C1 C10 120.0(2) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C4 122.4(2) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C3 C4 C9 118.0(2) . . ? C3 C4 C5 120.6(2) . . ? C9 C4 C5 121.3(3) . . ? C6' C5 C4 114.7(5) . . ? C6' C5 C6 32.7(5) . . ? C4 C5 C6 114.0(3) . . ? C6' C5 H5A 131.4 . . ? C4 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? C6' C5 H5B 78.4 . . ? C4 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C5 C6 C7 109.0(9) . . ? C5 C6 H6A 109.9 . . ? C7 C6 H6A 109.9 . . ? C5 C6 H6B 109.9 . . ? C7 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C8 C7 C6 112.9(9) . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C5 C6' C7' 110.0(16) . . ? C5 C6' H6'A 109.7 . . ? C7' C6' H6'A 109.7 . . ? C5 C6' H6'B 109.7 . . ? C7' C6' H6'B 109.7 . . ? H6'A C6' H6'B 108.2 . . ? C8 C7' C6' 112.1(14) . . ? C8 C7' H7'A 109.2 . . ? C6' C7' H7'A 109.2 . . ? C8 C7' H7'B 109.2 . . ? C6' C7' H7'B 109.2 . . ? H7'A C7' H7'B 107.9 . . ? C7 C8 C7' 23.2(8) . . ? C7 C8 C9 114.3(6) . . ? C7' C8 C9 114.9(10) . . ? C7 C8 H8A 108.7 . . ? C7' C8 H8A 87.4 . . ? C9 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? C7' C8 H8B 126.0 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C4 C9 C10 120.2(2) . . ? C4 C9 C8 120.6(2) . . ? C10 C9 C8 119.2(2) . . ? C1 C10 C9 119.9(2) . . ? C1 C10 C11 119.4(2) . . ? C9 C10 C11 120.6(2) . . ? C20 C11 C12 120.4(2) . . ? C20 C11 C10 118.8(2) . . ? C12 C11 C10 120.8(2) . . ? C11 C12 C17 119.7(3) . . ? C11 C12 C13 119.8(2) . . ? C17 C12 C13 120.5(3) . . ? C14 C13 C12 114.2(3) . . ? C14 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C13 111.9(3) . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C14 C15 C16 111.7(3) . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C17 113.8(2) . . ? C15 C16 H16A 108.8 . . ? C17 C16 H16A 108.8 . . ? C15 C16 H16B 108.8 . . ? C17 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C18 C17 C12 118.1(3) . . ? C18 C17 C16 120.7(2) . . ? C12 C17 C16 121.1(3) . . ? C19 C18 C17 122.9(2) . . ? C19 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? C18 C19 C20 119.0(3) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? N1 C20 C19 119.9(3) . . ? N1 C20 C11 120.3(2) . . ? C19 C20 C11 119.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -179.8(3) . . . . ? C10 C1 C2 C3 0.8(4) . . . . ? C1 C2 C3 C4 1.1(5) . . . . ? C2 C3 C4 C9 -1.7(4) . . . . ? C2 C3 C4 C5 178.5(3) . . . . ? C3 C4 C5 C6' -163.1(9) . . . . ? C9 C4 C5 C6' 17.1(9) . . . . ? C3 C4 C5 C6 160.9(5) . . . . ? C9 C4 C5 C6 -18.8(7) . . . . ? C6' C5 C6 C7 -51.7(12) . . . . ? C4 C5 C6 C7 47.1(12) . . . . ? C5 C6 C7 C8 -61.1(16) . . . . ? C4 C5 C6' C7' -46(2) . . . . ? C6 C5 C6' C7' 50.1(16) . . . . ? C5 C6' C7' C8 60(3) . . . . ? C6 C7 C8 C7' -53(3) . . . . ? C6 C7 C8 C9 44.1(14) . . . . ? C6' C7' C8 C7 52(2) . . . . ? C6' C7' C8 C9 -42(2) . . . . ? C3 C4 C9 C10 0.5(4) . . . . ? C5 C4 C9 C10 -179.7(3) . . . . ? C3 C4 C9 C8 -178.8(3) . . . . ? C5 C4 C9 C8 1.0(4) . . . . ? C7 C8 C9 C4 -13.6(6) . . . . ? C7' C8 C9 C4 12.0(9) . . . . ? C7 C8 C9 C10 167.1(6) . . . . ? C7' C8 C9 C10 -167.4(9) . . . . ? C2 C1 C10 C9 -1.9(4) . . . . ? O1 C1 C10 C9 178.7(3) . . . . ? C2 C1 C10 C11 179.4(3) . . . . ? O1 C1 C10 C11 -0.1(4) . . . . ? C4 C9 C10 C1 1.3(4) . . . . ? C8 C9 C10 C1 -179.4(3) . . . . ? C4 C9 C10 C11 180.0(2) . . . . ? C8 C9 C10 C11 -0.7(4) . . . . ? C1 C10 C11 C20 91.0(3) . . . . ? C9 C10 C11 C20 -87.7(3) . . . . ? C1 C10 C11 C12 -89.7(3) . . . . ? C9 C10 C11 C12 91.6(3) . . . . ? C20 C11 C12 C17 1.2(4) . . . . ? C10 C11 C12 C17 -178.1(2) . . . . ? C20 C11 C12 C13 -178.2(2) . . . . ? C10 C11 C12 C13 2.5(4) . . . . ? C11 C12 C13 C14 -163.2(3) . . . . ? C17 C12 C13 C14 17.4(4) . . . . ? C12 C13 C14 C15 -44.9(4) . . . . ? C13 C14 C15 C16 60.0(4) . . . . ? C14 C15 C16 C17 -45.8(4) . . . . ? C11 C12 C17 C18 -2.4(4) . . . . ? C13 C12 C17 C18 177.0(3) . . . . ? C11 C12 C17 C16 176.4(3) . . . . ? C13 C12 C17 C16 -4.2(4) . . . . ? C15 C16 C17 C18 -162.7(3) . . . . ? C15 C16 C17 C12 18.5(4) . . . . ? C12 C17 C18 C19 1.9(4) . . . . ? C16 C17 C18 C19 -176.9(3) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C18 C19 C20 N1 178.0(3) . . . . ? C18 C19 C20 C11 -1.2(4) . . . . ? C12 C11 C20 N1 -178.6(3) . . . . ? C10 C11 C20 N1 0.8(4) . . . . ? C12 C11 C20 C19 0.6(4) . . . . ? C10 C11 C20 C19 180.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.129 _refine_diff_density_min -0.151 _refine_diff_density_rms 0.032 # Attachment 'compound_17.cif' data_17 _database_code_depnum_ccdc_archive 'CCDC 691715' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C85 H89 N6 O3 Y' _chemical_formula_sum 'C85 H89 N6 O3 Y' _chemical_formula_weight 1331.53 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 14.0617(12) _cell_length_b 15.1344(13) _cell_length_c 36.245(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7713.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 13814 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.1 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9237 _exptl_absorpt_correction_T_max 0.9685 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 69212 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.1109 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.15 _reflns_number_total 17027 _reflns_number_gt 14607 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(4) _refine_ls_number_reflns 17027 _refine_ls_number_parameters 859 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1386 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.78162(2) 0.43181(2) 0.384389(8) 0.02842(9) Uani 1 1 d . . . N1 N 0.8187(2) 0.4791(2) 0.32064(7) 0.0318(6) Uani 1 1 d . . . N2 N 0.7411(2) 0.3186(2) 0.34092(7) 0.0349(7) Uani 1 1 d . . . N3 N 0.60353(19) 0.4438(2) 0.39076(8) 0.0340(6) Uani 1 1 d . . . N4 N 0.7393(2) 0.46005(19) 0.44691(7) 0.0309(6) Uani 1 1 d . . . N5 N 0.86398(19) 0.3126(2) 0.41619(7) 0.0313(6) Uani 1 1 d . . . N6 N 0.9412(2) 0.4759(2) 0.39753(8) 0.0332(6) Uani 1 1 d . . . O1 O 0.76764(16) 0.59597(15) 0.38660(6) 0.0336(5) Uani 1 1 d . . . O2 O 0.35786(19) 0.4782(2) 0.43654(8) 0.0517(8) Uani 1 1 d . . . O3 O 1.02587(17) 0.15826(17) 0.47128(6) 0.0356(6) Uani 1 1 d . . . C1 C 0.7364(2) 0.6512(2) 0.32621(10) 0.0340(8) Uani 1 1 d . . . C2 C 0.7052(3) 0.6384(2) 0.36188(10) 0.0382(8) Uani 1 1 d . . . C3 C 0.6145(3) 0.6633(3) 0.37346(12) 0.0473(10) Uani 1 1 d . . . H3 H 0.5957 0.6574 0.3985 0.057 Uiso 1 1 calc R . . C4 C 0.5528(3) 0.6967(3) 0.34728(14) 0.0597(13) Uani 1 1 d . . . H4 H 0.4915 0.7158 0.3549 0.072 Uiso 1 1 calc R . . C5 C 0.5774(3) 0.7033(3) 0.31020(13) 0.0562(12) Uani 1 1 d . . . C6 C 0.6703(3) 0.6792(3) 0.29933(11) 0.0450(10) Uani 1 1 d . . . C7 C 0.7006(3) 0.6817(3) 0.25923(11) 0.0506(11) Uani 1 1 d . . . H7A H 0.7358 0.6268 0.2534 0.061 Uiso 1 1 calc R . . H7B H 0.7446 0.7321 0.2555 0.061 Uiso 1 1 calc R . . C8 C 0.6175(4) 0.6908(5) 0.23281(14) 0.0797(19) Uani 1 1 d . . . H8A H 0.6417 0.7071 0.2081 0.096 Uiso 1 1 calc R . . H8B H 0.5848 0.6332 0.2306 0.096 Uiso 1 1 calc R . . C9 C 0.5473(4) 0.7595(5) 0.24542(17) 0.100(3) Uani 1 1 d . . . H9A H 0.4959 0.7653 0.2269 0.120 Uiso 1 1 calc R . . H9B H 0.5796 0.8174 0.2476 0.120 Uiso 1 1 calc R . . C10 C 0.5047(3) 0.7344(4) 0.28245(16) 0.0787(19) Uani 1 1 d . . . H10A H 0.4708 0.7862 0.2927 0.094 Uiso 1 1 calc R . . H10B H 0.4573 0.6868 0.2786 0.094 Uiso 1 1 calc R . . C11 C 0.8387(2) 0.6385(3) 0.31619(9) 0.0335(8) Uani 1 1 d . . . C12 C 0.8752(2) 0.5543(3) 0.31154(9) 0.0334(8) Uani 1 1 d . . . C13 C 0.9688(3) 0.5430(3) 0.30004(9) 0.0360(8) Uani 1 1 d . . . H13 H 0.9940 0.4853 0.2965 0.043 Uiso 1 1 calc R . . C14 C 1.0249(3) 0.6168(3) 0.29384(10) 0.0398(9) Uani 1 1 d . . . H14 H 1.0885 0.6088 0.2856 0.048 Uiso 1 1 calc R . . C15 C 0.9911(3) 0.7018(3) 0.29922(10) 0.0387(9) Uani 1 1 d . . . C16 C 0.8968(3) 0.7135(2) 0.31099(9) 0.0343(8) Uani 1 1 d . . . C17 C 0.8570(3) 0.8053(3) 0.31793(11) 0.0437(9) Uani 1 1 d . . . H17A H 0.8127 0.8204 0.2977 0.052 Uiso 1 1 calc R . . H17B H 0.8200 0.8043 0.3412 0.052 Uiso 1 1 calc R . . C18 C 0.9319(3) 0.8763(3) 0.32061(13) 0.0584(12) Uani 1 1 d . . . H18A H 0.9652 0.8716 0.3446 0.070 Uiso 1 1 calc R . . H18B H 0.9013 0.9352 0.3194 0.070 Uiso 1 1 calc R . . C19 C 1.0041(4) 0.8670(3) 0.28901(14) 0.0605(12) Uani 1 1 d . . . H19A H 0.9706 0.8710 0.2650 0.073 Uiso 1 1 calc R . . H19B H 1.0508 0.9158 0.2903 0.073 Uiso 1 1 calc R . . C20 C 1.0550(3) 0.7801(3) 0.29154(12) 0.0495(10) Uani 1 1 d . . . H20A H 1.1033 0.7840 0.3114 0.059 Uiso 1 1 calc R . . H20B H 1.0891 0.7696 0.2680 0.059 Uiso 1 1 calc R . . C21 C 0.7947(3) 0.6497(3) 0.41788(10) 0.0454(9) Uani 1 1 d . . . H21A H 0.8222 0.7054 0.4091 0.068 Uiso 1 1 calc R . . H21B H 0.8418 0.6179 0.4327 0.068 Uiso 1 1 calc R . . H21C H 0.7384 0.6621 0.4330 0.068 Uiso 1 1 calc R . . C22 C 0.8054(2) 0.4190(3) 0.29564(9) 0.0390(9) Uani 1 1 d . . . H22 H 0.8261 0.4298 0.2711 0.047 Uiso 1 1 calc R . . C23 C 0.7607(3) 0.3379(3) 0.30421(9) 0.0375(8) Uani 1 1 d . . . C24 C 0.7319(3) 0.2679(3) 0.28175(10) 0.0442(9) Uani 1 1 d . . . H24 H 0.7373 0.2647 0.2557 0.053 Uiso 1 1 calc R . . C25 C 0.6942(3) 0.2041(3) 0.30476(11) 0.0457(10) Uani 1 1 d . . . H25 H 0.6680 0.1488 0.2977 0.055 Uiso 1 1 calc R . . C26 C 0.7024(3) 0.2377(3) 0.34043(10) 0.0390(8) Uani 1 1 d . . . H26 H 0.6828 0.2068 0.3619 0.047 Uiso 1 1 calc R . . C27 C 0.4143(2) 0.3536(3) 0.40583(9) 0.0360(8) Uani 1 1 d . . . C28 C 0.3744(3) 0.3894(3) 0.43768(11) 0.0457(10) Uani 1 1 d . . . C29 C 0.3525(3) 0.3337(4) 0.46786(11) 0.0557(13) Uani 1 1 d . . . H29 H 0.3269 0.3579 0.4899 0.067 Uiso 1 1 calc R . . C30 C 0.3686(3) 0.2447(4) 0.46508(12) 0.0547(12) Uani 1 1 d . . . H30 H 0.3542 0.2080 0.4856 0.066 Uiso 1 1 calc R . . C31 C 0.4049(3) 0.2068(3) 0.43375(11) 0.0489(10) Uani 1 1 d . . . C32 C 0.4283(3) 0.2613(3) 0.40386(10) 0.0409(9) Uani 1 1 d . . . C33 C 0.4632(3) 0.2211(3) 0.36816(11) 0.0438(9) Uani 1 1 d . . . H33A H 0.5188 0.2551 0.3592 0.053 Uiso 1 1 calc R . . H33B H 0.4125 0.2259 0.3493 0.053 Uiso 1 1 calc R . . C34 C 0.4921(4) 0.1221(4) 0.37242(18) 0.0816(17) Uani 1 1 d . . . H34A H 0.4947 0.0951 0.3476 0.098 Uiso 1 1 calc R . . H34B H 0.5571 0.1195 0.3829 0.098 Uiso 1 1 calc R . . C35 C 0.4303(5) 0.0694(4) 0.39522(16) 0.0868(17) Uani 1 1 d . . . H35A H 0.4576 0.0094 0.3977 0.104 Uiso 1 1 calc R . . H35B H 0.3678 0.0636 0.3829 0.104 Uiso 1 1 calc R . . C36 C 0.4161(3) 0.1069(3) 0.43205(14) 0.0598(13) Uani 1 1 d . . . H36A H 0.4709 0.0900 0.4476 0.072 Uiso 1 1 calc R . . H36B H 0.3587 0.0796 0.4430 0.072 Uiso 1 1 calc R . . C37 C 0.4362(2) 0.4082(3) 0.37227(9) 0.0355(8) Uani 1 1 d . . . C38 C 0.5283(2) 0.4400(3) 0.36416(9) 0.0349(8) Uani 1 1 d . . . C39 C 0.5468(3) 0.4738(3) 0.32947(10) 0.0408(9) Uani 1 1 d . . . H39 H 0.6096 0.4918 0.3234 0.049 Uiso 1 1 calc R . . C40 C 0.4760(3) 0.4817(3) 0.30368(10) 0.0451(9) Uani 1 1 d . . . H40 H 0.4911 0.5030 0.2797 0.054 Uiso 1 1 calc R . . C41 C 0.3819(3) 0.4590(3) 0.31198(10) 0.0418(9) Uani 1 1 d . . . C42 C 0.3626(2) 0.4207(3) 0.34613(10) 0.0381(8) Uani 1 1 d . . . C43 C 0.2633(2) 0.3890(3) 0.35562(11) 0.0448(9) Uani 1 1 d . . . H43A H 0.2482 0.4071 0.3812 0.054 Uiso 1 1 calc R . . H43B H 0.2622 0.3236 0.3547 0.054 Uiso 1 1 calc R . . C44 C 0.1861(3) 0.4245(3) 0.32998(11) 0.0480(10) Uani 1 1 d . . . H44A H 0.1270 0.3899 0.3334 0.058 Uiso 1 1 calc R . . H44B H 0.1723 0.4868 0.3363 0.058 Uiso 1 1 calc R . . C45 C 0.2172(3) 0.4189(3) 0.29003(11) 0.0522(10) Uani 1 1 d . . . H45A H 0.1647 0.4387 0.2738 0.063 Uiso 1 1 calc R . . H45B H 0.2324 0.3568 0.2838 0.063 Uiso 1 1 calc R . . C46 C 0.3042(3) 0.4764(3) 0.28356(11) 0.0506(10) Uani 1 1 d . . . H46A H 0.2854 0.5394 0.2847 0.061 Uiso 1 1 calc R . . H46B H 0.3296 0.4648 0.2586 0.061 Uiso 1 1 calc R . . C47 C 0.3267(3) 0.5186(4) 0.46983(13) 0.0697(15) Uani 1 1 d . . . H47A H 0.2659 0.4927 0.4774 0.105 Uiso 1 1 calc R . . H47B H 0.3187 0.5822 0.4659 0.105 Uiso 1 1 calc R . . H47C H 0.3741 0.5087 0.4892 0.105 Uiso 1 1 calc R . . C48 C 0.5807(3) 0.4769(3) 0.42301(9) 0.0357(8) Uani 1 1 d . . . H48 H 0.5167 0.4945 0.4271 0.043 Uiso 1 1 calc R . . C49 C 0.6468(2) 0.4876(3) 0.45198(9) 0.0338(8) Uani 1 1 d . . . C50 C 0.6348(3) 0.5212(3) 0.48753(10) 0.0423(9) Uani 1 1 d . . . H50 H 0.5777 0.5438 0.4979 0.051 Uiso 1 1 calc R . . C51 C 0.7226(3) 0.5150(3) 0.50483(9) 0.0429(9) Uani 1 1 d . . . H51 H 0.7374 0.5329 0.5293 0.051 Uiso 1 1 calc R . . C52 C 0.7848(3) 0.4773(2) 0.47925(9) 0.0379(8) Uani 1 1 d . . . H52 H 0.8501 0.4654 0.4838 0.046 Uiso 1 1 calc R . . C53 C 0.9849(2) 0.1537(2) 0.40827(9) 0.0307(7) Uani 1 1 d . . . C54 C 1.0565(3) 0.1580(2) 0.43498(9) 0.0341(8) Uani 1 1 d . . . C55 C 1.1516(2) 0.1659(3) 0.42523(10) 0.0361(8) Uani 1 1 d . . . H55 H 1.1997 0.1700 0.4435 0.043 Uiso 1 1 calc R . . C56 C 1.1743(2) 0.1677(3) 0.38790(10) 0.0394(8) Uani 1 1 d . . . H56 H 1.2392 0.1727 0.3810 0.047 Uiso 1 1 calc R . . C57 C 1.1059(3) 0.1624(3) 0.36036(10) 0.0375(8) Uani 1 1 d . . . C58 C 1.0092(3) 0.1553(3) 0.37085(9) 0.0348(8) Uani 1 1 d . . . C59 C 0.9312(3) 0.1538(3) 0.34215(9) 0.0355(8) Uani 1 1 d . . . H59A H 0.8960 0.2104 0.3432 0.043 Uiso 1 1 calc R . . H59B H 0.8859 0.1059 0.3483 0.043 Uiso 1 1 calc R . . C60 C 0.9674(3) 0.1396(3) 0.30278(10) 0.0451(10) Uani 1 1 d . . . H60A H 0.9838 0.0766 0.2993 0.054 Uiso 1 1 calc R . . H60B H 0.9165 0.1549 0.2850 0.054 Uiso 1 1 calc R . . C61 C 1.0532(3) 0.1954(3) 0.29525(10) 0.0525(11) Uani 1 1 d . . . H61A H 1.0382 0.2583 0.2999 0.063 Uiso 1 1 calc R . . H61B H 1.0724 0.1891 0.2691 0.063 Uiso 1 1 calc R . . C62 C 1.1341(3) 0.1661(3) 0.32025(10) 0.0466(10) Uani 1 1 d . . . H62A H 1.1560 0.1069 0.3124 0.056 Uiso 1 1 calc R . . H62B H 1.1880 0.2076 0.3174 0.056 Uiso 1 1 calc R . . C63 C 0.8829(2) 0.1501(2) 0.42036(9) 0.0298(7) Uani 1 1 d . . . C64 C 0.8290(2) 0.2277(2) 0.42493(9) 0.0297(7) Uani 1 1 d . . . C65 C 0.7336(3) 0.2207(2) 0.43611(9) 0.0344(8) Uani 1 1 d . . . H65 H 0.6967 0.2727 0.4394 0.041 Uiso 1 1 calc R . . C66 C 0.6934(3) 0.1401(3) 0.44232(10) 0.0381(9) Uani 1 1 d . . . H66 H 0.6295 0.1371 0.4507 0.046 Uiso 1 1 calc R . . C67 C 0.7439(3) 0.0618(3) 0.43664(9) 0.0374(8) Uani 1 1 d . A . C68 C 0.8396(2) 0.0667(3) 0.42594(9) 0.0355(7) Uani 1 1 d . . . C69 C 0.8982(3) -0.0156(2) 0.42048(11) 0.0414(9) Uani 1 1 d . A . H69A H 0.9260 -0.0137 0.3954 0.050 Uiso 1 1 calc R . . H69B H 0.9516 -0.0142 0.4383 0.050 Uiso 1 1 calc R . . C70 C 0.8479(4) -0.1006(3) 0.42483(19) 0.0807(18) Uani 1 1 d D . . H70A H 0.8542 -0.1201 0.4499 0.097 Uiso 0.676(13) 1 d PR A 1 H70B H 0.8777 -0.1438 0.4093 0.097 Uiso 0.676(13) 1 d PR A 1 H70C H 0.8915 -0.1397 0.4370 0.097 Uiso 0.324(13) 1 d PR A 2 H70D H 0.8381 -0.1240 0.4005 0.097 Uiso 0.324(13) 1 d PR A 2 C71 C 0.7454(5) -0.0960(5) 0.4154(3) 0.067(3) Uani 0.676(13) 1 d PD A 1 H71A H 0.7158 -0.1548 0.4190 0.081 Uiso 0.676(13) 1 calc PR A 1 H71B H 0.7381 -0.0796 0.3891 0.081 Uiso 0.676(13) 1 calc PR A 1 C71' C 0.7537(7) -0.1096(7) 0.4454(4) 0.053(5) Uani 0.324(13) 1 d PD A 2 H71C H 0.7660 -0.1189 0.4720 0.063 Uiso 0.324(13) 1 calc PR A 2 H71D H 0.7185 -0.1615 0.4359 0.063 Uiso 0.324(13) 1 calc PR A 2 C72 C 0.6938(3) -0.0264(3) 0.44012(13) 0.0532(11) Uani 1 1 d D . . H72A H 0.6287 -0.0207 0.4324 0.064 Uiso 0.676(13) 1 d PR A 1 H72B H 0.6946 -0.0454 0.4654 0.064 Uiso 0.676(13) 1 d PR A 1 H72C H 0.6551 -0.0345 0.4185 0.064 Uiso 0.324(13) 1 d PR A 2 H72D H 0.6515 -0.0225 0.4608 0.064 Uiso 0.324(13) 1 d PR A 2 C73 C 1.0912(3) 0.1929(3) 0.49782(10) 0.0418(9) Uani 1 1 d . . . H73A H 1.1475 0.1548 0.4990 0.063 Uiso 1 1 calc R . . H73B H 1.0606 0.1948 0.5221 0.063 Uiso 1 1 calc R . . H73C H 1.1102 0.2527 0.4906 0.063 Uiso 1 1 calc R . . C74 C 0.9459(2) 0.3370(2) 0.43042(9) 0.0322(7) Uani 1 1 d . . . H74 H 0.9773 0.2990 0.4474 0.039 Uiso 1 1 calc R . . C75 C 0.9881(2) 0.4184(2) 0.42102(9) 0.0340(8) Uani 1 1 d . . . C76 C 1.0769(3) 0.4521(3) 0.43134(12) 0.0505(11) Uani 1 1 d . . . H76 H 1.1221 0.4253 0.4473 0.061 Uiso 1 1 calc R . . C77 C 1.0853(3) 0.5328(3) 0.41330(13) 0.0551(12) Uani 1 1 d . . . H77 H 1.1380 0.5719 0.4144 0.066 Uiso 1 1 calc R . . C78 C 1.0016(3) 0.5456(3) 0.39326(10) 0.0424(9) Uani 1 1 d . . . H78 H 0.9884 0.5963 0.3786 0.051 Uiso 1 1 calc R . . C79 C 0.2694(7) 0.6724(5) 0.3568(3) 0.168(4) Uani 1 1 d DU . . H79A H 0.3028 0.6746 0.3331 0.252 Uiso 1 1 calc R . . H79B H 0.2166 0.6303 0.3553 0.252 Uiso 1 1 calc R . . H79C H 0.3137 0.6535 0.3762 0.252 Uiso 1 1 calc R . . C80 C 0.2324(3) 0.7600(3) 0.36574(13) 0.0925(19) Uani 1 1 d GDU . . C81 C 0.2708(3) 0.8338(4) 0.34841(12) 0.117(2) Uani 1 1 d GDU . . H81 H 0.3189 0.8268 0.3302 0.141 Uiso 1 1 calc R . . C82 C 0.2387(4) 0.9178(3) 0.35765(16) 0.135(3) Uani 1 1 d GU . . H82 H 0.2650 0.9682 0.3458 0.162 Uiso 1 1 calc R . . C83 C 0.1683(4) 0.9281(2) 0.38423(17) 0.138(3) Uani 1 1 d GU . . H83 H 0.1465 0.9855 0.3905 0.166 Uiso 1 1 calc R . . C84 C 0.1300(3) 0.8543(3) 0.40156(13) 0.108(2) Uani 1 1 d GU . . H84 H 0.0818 0.8614 0.4197 0.130 Uiso 1 1 calc R . . C85 C 0.1620(3) 0.7703(3) 0.39232(13) 0.0915(19) Uani 1 1 d GDU . . H85 H 0.1357 0.7199 0.4042 0.110 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.02729(14) 0.03053(17) 0.02742(14) 0.00249(13) -0.00072(12) 0.00034(14) N1 0.0335(14) 0.0335(16) 0.0285(14) 0.0045(12) 0.0012(11) 0.0001(13) N2 0.0341(15) 0.0407(18) 0.0299(14) -0.0013(12) -0.0013(11) -0.0019(13) N3 0.0319(14) 0.0365(17) 0.0337(15) 0.0015(13) -0.0014(11) -0.0046(13) N4 0.0374(16) 0.0315(16) 0.0239(12) 0.0040(11) -0.0023(11) 0.0019(12) N5 0.0308(15) 0.0344(17) 0.0287(14) 0.0019(12) -0.0012(11) 0.0005(12) N6 0.0304(14) 0.0363(17) 0.0328(14) 0.0002(12) -0.0015(11) -0.0036(13) O1 0.0397(13) 0.0284(12) 0.0328(11) 0.0045(9) 0.0026(11) 0.0079(10) O2 0.0375(15) 0.066(2) 0.0513(17) -0.0161(15) 0.0108(12) -0.0066(15) O3 0.0378(13) 0.0433(15) 0.0255(11) 0.0016(10) -0.0027(10) 0.0051(12) C1 0.0326(18) 0.032(2) 0.0375(18) 0.0070(15) 0.0029(14) 0.0008(15) C2 0.0326(19) 0.035(2) 0.047(2) 0.0075(16) 0.0078(15) 0.0054(16) C3 0.042(2) 0.048(2) 0.052(2) 0.0212(18) 0.0196(17) 0.0130(19) C4 0.038(2) 0.064(3) 0.077(3) 0.031(3) 0.013(2) 0.019(2) C5 0.036(2) 0.066(3) 0.066(3) 0.034(2) 0.003(2) 0.006(2) C6 0.036(2) 0.047(3) 0.052(2) 0.0264(19) 0.0041(17) -0.0019(18) C7 0.034(2) 0.073(3) 0.045(2) 0.026(2) -0.0059(16) -0.006(2) C8 0.052(3) 0.132(5) 0.055(3) 0.042(3) -0.015(2) -0.014(3) C9 0.051(3) 0.153(7) 0.097(4) 0.079(5) -0.004(3) 0.016(4) C10 0.038(2) 0.098(4) 0.100(4) 0.058(4) -0.001(3) 0.013(3) C11 0.0301(17) 0.043(2) 0.0279(16) 0.0062(15) 0.0032(13) 0.0009(16) C12 0.0331(17) 0.039(2) 0.0276(15) 0.0038(15) 0.0000(13) -0.0006(15) C13 0.0362(18) 0.041(2) 0.0308(17) 0.0036(14) 0.0023(14) 0.0029(16) C14 0.0312(18) 0.056(3) 0.0318(17) 0.0023(17) 0.0024(14) 0.0007(18) C15 0.0380(19) 0.047(2) 0.0314(17) 0.0057(16) 0.0005(15) -0.0061(18) C16 0.0358(18) 0.034(2) 0.0330(17) 0.0078(15) 0.0009(14) 0.0001(16) C17 0.047(2) 0.037(2) 0.046(2) 0.0003(17) 0.0096(17) -0.0046(18) C18 0.062(3) 0.045(3) 0.068(3) -0.006(2) 0.023(2) -0.015(2) C19 0.067(3) 0.050(3) 0.065(3) 0.004(2) 0.021(2) -0.016(2) C20 0.043(2) 0.057(3) 0.047(2) 0.006(2) 0.0036(18) -0.014(2) C21 0.059(3) 0.036(2) 0.042(2) -0.0086(16) 0.0006(19) -0.005(2) C22 0.0358(18) 0.051(2) 0.0300(16) 0.0002(16) -0.0001(13) -0.0006(17) C23 0.0340(19) 0.045(2) 0.0339(17) -0.0032(16) -0.0021(14) -0.0036(16) C24 0.043(2) 0.052(3) 0.0379(18) -0.0135(17) -0.0009(16) -0.0068(19) C25 0.047(2) 0.049(3) 0.041(2) -0.0093(18) -0.0006(17) -0.0091(19) C26 0.038(2) 0.038(2) 0.0410(19) 0.0015(16) -0.0022(16) -0.0058(17) C27 0.0241(16) 0.057(3) 0.0272(16) -0.0033(15) -0.0014(13) -0.0089(16) C28 0.0306(18) 0.063(3) 0.044(2) -0.008(2) -0.0007(16) -0.0098(19) C29 0.037(2) 0.096(4) 0.035(2) -0.010(2) 0.0064(16) -0.027(2) C30 0.053(3) 0.071(3) 0.040(2) 0.012(2) -0.0087(19) -0.024(2) C31 0.035(2) 0.065(3) 0.047(2) 0.009(2) -0.0093(17) -0.017(2) C32 0.0324(18) 0.051(3) 0.0396(19) 0.0067(17) -0.0035(15) -0.0141(17) C33 0.036(2) 0.045(2) 0.051(2) -0.0026(18) -0.0043(17) -0.0031(18) C34 0.074(3) 0.067(4) 0.105(5) -0.011(3) 0.022(3) -0.011(3) C35 0.099(4) 0.075(4) 0.087(4) 0.021(3) -0.016(3) -0.008(4) C36 0.040(2) 0.058(3) 0.081(3) 0.022(2) -0.011(2) -0.016(2) C37 0.0318(17) 0.043(2) 0.0317(16) -0.0050(14) 0.0003(13) -0.0010(15) C38 0.0314(17) 0.042(2) 0.0308(16) -0.0009(16) 0.0002(13) -0.0007(17) C39 0.0338(18) 0.055(3) 0.0335(18) 0.0032(17) -0.0012(15) -0.0039(18) C40 0.043(2) 0.058(3) 0.0344(18) 0.0093(18) -0.0043(16) -0.008(2) C41 0.0371(19) 0.051(3) 0.0370(19) -0.0022(16) -0.0063(15) 0.0011(17) C42 0.0303(17) 0.042(2) 0.0422(19) -0.0065(17) -0.0003(14) 0.0004(16) C43 0.0313(19) 0.057(3) 0.046(2) -0.0005(18) -0.0046(16) -0.0007(18) C44 0.0299(17) 0.061(3) 0.053(2) -0.003(2) -0.0094(16) 0.0047(19) C45 0.0384(19) 0.067(3) 0.051(2) -0.007(2) -0.0162(18) 0.006(2) C46 0.045(2) 0.062(3) 0.045(2) 0.001(2) -0.0125(18) 0.008(2) C47 0.051(3) 0.100(4) 0.058(3) -0.034(3) 0.014(2) -0.011(3) C48 0.0348(18) 0.040(2) 0.0326(17) 0.0072(15) 0.0066(14) -0.0042(16) C49 0.0325(17) 0.040(2) 0.0286(16) -0.0001(15) 0.0022(13) -0.0038(16) C50 0.042(2) 0.052(2) 0.0334(18) -0.0103(17) 0.0068(15) -0.0073(19) C51 0.049(2) 0.050(2) 0.0297(16) -0.0015(15) -0.0021(16) -0.007(2) C52 0.0416(19) 0.040(2) 0.0324(16) 0.0040(15) -0.0068(16) -0.0033(18) C53 0.0344(17) 0.0289(19) 0.0286(15) -0.0032(13) -0.0013(13) 0.0010(14) C54 0.0375(18) 0.033(2) 0.0321(17) 0.0025(14) -0.0023(14) 0.0086(15) C55 0.0314(17) 0.041(2) 0.0359(18) 0.0025(16) -0.0055(14) 0.0029(16) C56 0.0326(17) 0.048(2) 0.0376(18) 0.0022(17) 0.0023(15) -0.0022(16) C57 0.0353(19) 0.042(2) 0.0347(18) 0.0008(16) 0.0017(15) -0.0032(17) C58 0.0369(18) 0.038(2) 0.0298(16) -0.0002(14) -0.0019(14) -0.0017(16) C59 0.0377(18) 0.038(2) 0.0309(17) -0.0040(15) -0.0050(14) -0.0010(16) C60 0.044(2) 0.060(3) 0.0305(18) -0.0020(17) -0.0005(16) -0.006(2) C61 0.054(2) 0.072(3) 0.0309(18) 0.0031(19) 0.0016(17) -0.016(2) C62 0.041(2) 0.060(3) 0.039(2) 0.0036(19) 0.0040(16) -0.0012(19) C63 0.0312(17) 0.034(2) 0.0241(15) -0.0007(13) -0.0012(13) 0.0035(14) C64 0.0316(17) 0.0305(19) 0.0271(16) -0.0012(14) -0.0007(13) 0.0025(14) C65 0.0359(19) 0.032(2) 0.0353(17) -0.0012(14) -0.0015(15) -0.0012(15) C66 0.0306(18) 0.049(2) 0.0347(18) -0.0015(16) -0.0037(14) -0.0055(16) C67 0.0442(19) 0.036(2) 0.0321(16) -0.0072(15) -0.0006(14) -0.0081(17) C68 0.0410(18) 0.037(2) 0.0283(15) -0.0074(16) -0.0013(13) -0.0023(18) C69 0.059(2) 0.028(2) 0.0373(19) -0.0044(16) 0.0004(17) 0.0001(18) C70 0.088(4) 0.042(3) 0.112(5) -0.012(3) 0.036(4) -0.002(3) C71 0.074(5) 0.034(4) 0.095(7) -0.018(4) -0.002(4) -0.008(3) C71' 0.064(9) 0.048(8) 0.046(9) -0.013(6) 0.023(6) -0.019(7) C72 0.054(3) 0.039(2) 0.066(3) -0.004(2) -0.002(2) -0.015(2) C73 0.042(2) 0.049(2) 0.0341(18) 0.0001(17) -0.0085(15) 0.0078(18) C74 0.0316(17) 0.033(2) 0.0325(17) 0.0009(14) -0.0051(14) 0.0081(15) C75 0.0286(16) 0.036(2) 0.0372(17) 0.0002(15) -0.0033(13) 0.0041(15) C76 0.0337(19) 0.059(3) 0.059(2) 0.014(2) -0.0117(18) -0.0086(19) C77 0.039(2) 0.053(3) 0.074(3) 0.009(2) -0.011(2) -0.019(2) C78 0.0382(19) 0.050(3) 0.0394(19) 0.0026(16) -0.0028(15) -0.0097(17) C79 0.167(7) 0.135(7) 0.203(8) -0.034(6) 0.012(7) -0.030(6) C80 0.086(4) 0.086(4) 0.106(4) -0.009(4) 0.004(4) 0.004(4) C81 0.073(4) 0.161(6) 0.117(5) 0.006(5) 0.001(4) -0.030(5) C82 0.134(6) 0.108(6) 0.164(7) 0.053(5) -0.050(5) -0.037(5) C83 0.128(6) 0.091(5) 0.196(7) 0.014(6) -0.071(6) -0.007(5) C84 0.104(5) 0.091(5) 0.130(5) -0.015(4) -0.028(4) 0.019(4) C85 0.102(4) 0.062(4) 0.111(5) 0.008(3) 0.022(4) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N4 2.382(3) . ? Y1 N6 2.389(3) . ? Y1 N2 2.396(3) . ? Y1 N5 2.434(3) . ? Y1 N1 2.475(3) . ? Y1 O1 2.493(2) . ? Y1 N3 2.522(3) . ? N1 C22 1.297(5) . ? N1 C12 1.426(5) . ? N2 C26 1.340(5) . ? N2 C23 1.390(4) . ? N3 C48 1.311(4) . ? N3 C38 1.433(4) . ? N4 C52 1.360(4) . ? N4 C49 1.379(4) . ? N5 C74 1.315(4) . ? N5 C64 1.412(5) . ? N6 C78 1.363(5) . ? N6 C75 1.384(4) . ? O1 C2 1.410(4) . ? O1 C21 1.446(4) . ? O2 C28 1.365(5) . ? O2 C47 1.421(5) . ? O3 C54 1.385(4) . ? O3 C73 1.429(4) . ? C1 C2 1.379(5) . ? C1 C6 1.411(5) . ? C1 C11 1.496(5) . ? C2 C3 1.395(5) . ? C3 C4 1.381(6) . ? C3 H3 0.9500 . ? C4 C5 1.391(6) . ? C4 H4 0.9500 . ? C5 C6 1.412(6) . ? C5 C10 1.510(6) . ? C6 C7 1.515(5) . ? C7 C8 1.518(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.505(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.518(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.384(5) . ? C11 C16 1.412(5) . ? C12 C13 1.392(5) . ? C13 C14 1.386(5) . ? C13 H13 0.9500 . ? C14 C15 1.386(6) . ? C14 H14 0.9500 . ? C15 C16 1.404(5) . ? C15 C20 1.513(6) . ? C16 C17 1.518(5) . ? C17 C18 1.509(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.537(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.500(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.414(5) . ? C22 H22 0.9500 . ? C23 C24 1.396(5) . ? C24 C25 1.381(6) . ? C24 H24 0.9500 . ? C25 C26 1.394(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.394(5) . ? C27 C32 1.412(6) . ? C27 C37 1.503(5) . ? C28 C29 1.415(6) . ? C29 C30 1.369(7) . ? C29 H29 0.9500 . ? C30 C31 1.371(6) . ? C30 H30 0.9500 . ? C31 C32 1.401(5) . ? C31 C36 1.521(7) . ? C32 C33 1.512(5) . ? C33 C34 1.561(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.441(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.464(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.412(5) . ? C37 C42 1.416(5) . ? C38 C39 1.382(5) . ? C39 C40 1.370(5) . ? C39 H39 0.9500 . ? C40 C41 1.400(5) . ? C40 H40 0.9500 . ? C41 C42 1.393(5) . ? C41 C46 1.524(5) . ? C42 C43 1.516(5) . ? C43 C44 1.526(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.515(6) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.520(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.411(5) . ? C48 H48 0.9500 . ? C49 C50 1.396(5) . ? C50 C51 1.388(5) . ? C50 H50 0.9500 . ? C51 C52 1.397(5) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.399(5) . ? C53 C58 1.399(5) . ? C53 C63 1.500(5) . ? C54 C55 1.387(5) . ? C55 C56 1.391(5) . ? C55 H55 0.9500 . ? C56 C57 1.388(5) . ? C56 H56 0.9500 . ? C57 C58 1.416(5) . ? C57 C62 1.508(5) . ? C58 C59 1.512(5) . ? C59 C60 1.530(5) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.497(6) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.520(6) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.408(5) . ? C63 C68 1.416(5) . ? C64 C65 1.405(5) . ? C65 C66 1.363(5) . ? C65 H65 0.9500 . ? C66 C67 1.397(5) . ? C66 H66 0.9500 . ? C67 C68 1.403(5) . ? C67 C72 1.514(6) . ? C68 C69 1.506(5) . ? C69 C70 1.478(6) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.483(7) . ? C70 C71' 1.525(8) . ? C70 H70A 0.9601 . ? C70 H70B 0.9599 . ? C70 H70C 0.9599 . ? C70 H70D 0.9597 . ? C71 C72 1.562(7) . ? C71 H70D 1.4734 . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C71 H72C 1.5783 . ? C71' C72 1.527(9) . ? C71' H70A 1.4322 . ? C71' H71C 0.9900 . ? C71' H71D 0.9900 . ? C71' H72B 1.4701 . ? C72 H72A 0.9600 . ? C72 H72B 0.9601 . ? C72 H72C 0.9600 . ? C72 H72D 0.9601 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C75 1.409(5) . ? C74 H74 0.9500 . ? C75 C76 1.400(5) . ? C76 C77 1.391(6) . ? C76 H76 0.9500 . ? C77 C78 1.397(6) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C80 1.461(7) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C81 1.3900 . ? C80 C85 1.3900 . ? C81 C82 1.3900 . ? C81 H81 0.9500 . ? C82 C83 1.3900 . ? C82 H82 0.9500 . ? C83 C84 1.3900 . ? C83 H83 0.9500 . ? C84 C85 1.3900 . ? C84 H84 0.9500 . ? C85 H85 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Y1 N6 89.70(10) . . ? N4 Y1 N2 134.00(10) . . ? N6 Y1 N2 123.62(10) . . ? N4 Y1 N5 78.53(9) . . ? N6 Y1 N5 70.46(10) . . ? N2 Y1 N5 83.95(10) . . ? N4 Y1 N1 152.78(10) . . ? N6 Y1 N1 84.69(9) . . ? N2 Y1 N1 69.08(10) . . ? N5 Y1 N1 123.80(9) . . ? N4 Y1 O1 76.76(8) . . ? N6 Y1 O1 77.85(9) . . ? N2 Y1 O1 135.63(9) . . ? N5 Y1 O1 139.53(9) . . ? N1 Y1 O1 76.02(9) . . ? N4 Y1 N3 69.63(9) . . ? N6 Y1 N3 153.45(10) . . ? N2 Y1 N3 82.87(10) . . ? N5 Y1 N3 118.86(9) . . ? N1 Y1 N3 105.90(9) . . ? O1 Y1 N3 81.19(9) . . ? C22 N1 C12 118.6(3) . . ? C22 N1 Y1 114.8(2) . . ? C12 N1 Y1 124.3(2) . . ? C26 N2 C23 105.1(3) . . ? C26 N2 Y1 139.3(2) . . ? C23 N2 Y1 115.6(2) . . ? C48 N3 C38 115.8(3) . . ? C48 N3 Y1 110.6(2) . . ? C38 N3 Y1 132.0(2) . . ? C52 N4 C49 105.7(3) . . ? C52 N4 Y1 137.5(2) . . ? C49 N4 Y1 114.6(2) . . ? C74 N5 C64 118.2(3) . . ? C74 N5 Y1 113.2(2) . . ? C64 N5 Y1 128.0(2) . . ? C78 N6 C75 105.1(3) . . ? C78 N6 Y1 141.1(2) . . ? C75 N6 Y1 113.2(2) . . ? C2 O1 C21 114.0(3) . . ? C2 O1 Y1 118.9(2) . . ? C21 O1 Y1 124.4(2) . . ? C28 O2 C47 116.7(4) . . ? C54 O3 C73 116.1(3) . . ? C2 C1 C6 118.7(3) . . ? C2 C1 C11 121.0(3) . . ? C6 C1 C11 120.3(3) . . ? C1 C2 C3 122.4(3) . . ? C1 C2 O1 117.5(3) . . ? C3 C2 O1 120.1(3) . . ? C4 C3 C2 117.8(4) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C3 C4 C5 122.2(4) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C4 C5 C6 118.8(4) . . ? C4 C5 C10 119.8(4) . . ? C6 C5 C10 121.4(4) . . ? C1 C6 C5 119.6(4) . . ? C1 C6 C7 118.9(3) . . ? C5 C6 C7 121.5(4) . . ? C6 C7 C8 113.0(4) . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C7 112.1(5) . . ? C9 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? C9 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C10 110.7(5) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C5 C10 C9 113.6(4) . . ? C5 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? C5 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C16 120.7(3) . . ? C12 C11 C1 120.3(3) . . ? C16 C11 C1 119.0(3) . . ? C11 C12 C13 120.0(3) . . ? C11 C12 N1 120.0(3) . . ? C13 C12 N1 119.9(3) . . ? C14 C13 C12 119.2(4) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 122.1(3) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C14 C15 C16 118.9(4) . . ? C14 C15 C20 119.9(4) . . ? C16 C15 C20 121.2(4) . . ? C15 C16 C11 119.1(3) . . ? C15 C16 C17 120.9(3) . . ? C11 C16 C17 120.0(3) . . ? C18 C17 C16 113.9(3) . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? C16 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C17 C18 C19 110.3(4) . . ? C17 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? C17 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? C20 C19 C18 110.5(4) . . ? C20 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C19 C20 C15 114.4(4) . . ? C19 C20 H20A 108.7 . . ? C15 C20 H20A 108.7 . . ? C19 C20 H20B 108.7 . . ? C15 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C23 121.3(3) . . ? N1 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? N2 C23 C24 110.0(3) . . ? N2 C23 C22 118.8(3) . . ? C24 C23 C22 131.3(3) . . ? C25 C24 C23 106.8(3) . . ? C25 C24 H24 126.6 . . ? C23 C24 H24 126.6 . . ? C24 C25 C26 105.9(4) . . ? C24 C25 H25 127.1 . . ? C26 C25 H25 127.1 . . ? N2 C26 C25 112.3(3) . . ? N2 C26 H26 123.9 . . ? C25 C26 H26 123.9 . . ? C28 C27 C32 118.8(4) . . ? C28 C27 C37 122.6(4) . . ? C32 C27 C37 118.3(3) . . ? O2 C28 C27 115.2(4) . . ? O2 C28 C29 125.0(4) . . ? C27 C28 C29 119.8(4) . . ? C30 C29 C28 119.6(4) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 122.3(4) . . ? C29 C30 H30 118.8 . . ? C31 C30 H30 118.8 . . ? C30 C31 C32 118.7(4) . . ? C30 C31 C36 119.3(4) . . ? C32 C31 C36 122.0(4) . . ? C31 C32 C27 120.7(4) . . ? C31 C32 C33 120.0(4) . . ? C27 C32 C33 119.1(3) . . ? C32 C33 C34 112.7(4) . . ? C32 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? C32 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C35 C34 C33 115.6(5) . . ? C35 C34 H34A 108.4 . . ? C33 C34 H34A 108.4 . . ? C35 C34 H34B 108.4 . . ? C33 C34 H34B 108.4 . . ? H34A C34 H34B 107.5 . . ? C34 C35 C36 113.0(5) . . ? C34 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? C34 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C35 C36 C31 115.9(4) . . ? C35 C36 H36A 108.3 . . ? C31 C36 H36A 108.3 . . ? C35 C36 H36B 108.3 . . ? C31 C36 H36B 108.3 . . ? H36A C36 H36B 107.4 . . ? C38 C37 C42 119.1(3) . . ? C38 C37 C27 122.9(3) . . ? C42 C37 C27 117.7(3) . . ? C39 C38 C37 119.2(3) . . ? C39 C38 N3 117.3(3) . . ? C37 C38 N3 123.4(3) . . ? C40 C39 C38 121.1(3) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C39 C40 C41 121.2(4) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C42 C41 C40 118.5(3) . . ? C42 C41 C46 122.2(3) . . ? C40 C41 C46 119.3(3) . . ? C41 C42 C37 120.5(3) . . ? C41 C42 C43 120.8(3) . . ? C37 C42 C43 118.6(3) . . ? C42 C43 C44 113.9(3) . . ? C42 C43 H43A 108.8 . . ? C44 C43 H43A 108.8 . . ? C42 C43 H43B 108.8 . . ? C44 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? C45 C44 C43 110.9(3) . . ? C45 C44 H44A 109.5 . . ? C43 C44 H44A 109.5 . . ? C45 C44 H44B 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 108.0 . . ? C44 C45 C46 110.3(3) . . ? C44 C45 H45A 109.6 . . ? C46 C45 H45A 109.6 . . ? C44 C45 H45B 109.6 . . ? C46 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? C45 C46 C41 111.9(3) . . ? C45 C46 H46A 109.2 . . ? C41 C46 H46A 109.2 . . ? C45 C46 H46B 109.2 . . ? C41 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? O2 C47 H47A 109.5 . . ? O2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N3 C48 C49 123.1(3) . . ? N3 C48 H48 118.5 . . ? C49 C48 H48 118.5 . . ? N4 C49 C50 110.3(3) . . ? N4 C49 C48 119.2(3) . . ? C50 C49 C48 130.5(3) . . ? C51 C50 C49 106.5(3) . . ? C51 C50 H50 126.7 . . ? C49 C50 H50 126.7 . . ? C50 C51 C52 106.5(3) . . ? C50 C51 H51 126.7 . . ? C52 C51 H51 126.7 . . ? N4 C52 C51 110.9(3) . . ? N4 C52 H52 124.6 . . ? C51 C52 H52 124.6 . . ? C54 C53 C58 119.6(3) . . ? C54 C53 C63 119.2(3) . . ? C58 C53 C63 121.2(3) . . ? O3 C54 C55 122.8(3) . . ? O3 C54 C53 115.7(3) . . ? C55 C54 C53 121.4(3) . . ? C54 C55 C56 118.1(3) . . ? C54 C55 H55 120.9 . . ? C56 C55 H55 120.9 . . ? C57 C56 C55 122.6(3) . . ? C57 C56 H56 118.7 . . ? C55 C56 H56 118.7 . . ? C56 C57 C58 118.5(3) . . ? C56 C57 C62 120.6(3) . . ? C58 C57 C62 120.9(3) . . ? C53 C58 C57 119.8(3) . . ? C53 C58 C59 119.3(3) . . ? C57 C58 C59 120.9(3) . . ? C58 C59 C60 113.7(3) . . ? C58 C59 H59A 108.8 . . ? C60 C59 H59A 108.8 . . ? C58 C59 H59B 108.8 . . ? C60 C59 H59B 108.8 . . ? H59A C59 H59B 107.7 . . ? C61 C60 C59 111.1(3) . . ? C61 C60 H60A 109.4 . . ? C59 C60 H60A 109.4 . . ? C61 C60 H60B 109.4 . . ? C59 C60 H60B 109.4 . . ? H60A C60 H60B 108.0 . . ? C60 C61 C62 109.2(4) . . ? C60 C61 H61A 109.8 . . ? C62 C61 H61A 109.8 . . ? C60 C61 H61B 109.8 . . ? C62 C61 H61B 109.8 . . ? H61A C61 H61B 108.3 . . ? C57 C62 C61 112.9(3) . . ? C57 C62 H62A 109.0 . . ? C61 C62 H62A 109.0 . . ? C57 C62 H62B 109.0 . . ? C61 C62 H62B 109.0 . . ? H62A C62 H62B 107.8 . . ? C64 C63 C68 119.7(3) . . ? C64 C63 C53 121.2(3) . . ? C68 C63 C53 119.0(3) . . ? C65 C64 C63 118.9(3) . . ? C65 C64 N5 117.8(3) . . ? C63 C64 N5 123.1(3) . . ? C66 C65 C64 120.8(4) . . ? C66 C65 H65 119.6 . . ? C64 C65 H65 119.6 . . ? C65 C66 C67 121.6(3) . . ? C65 C66 H66 119.2 . . ? C67 C66 H66 119.2 . . ? C66 C67 C68 118.9(4) . . ? C66 C67 C72 119.9(3) . . ? C68 C67 C72 121.1(4) . . ? C67 C68 C63 119.9(4) . . ? C67 C68 C69 121.2(4) . . ? C63 C68 C69 118.9(3) . . ? C70 C69 C68 116.3(4) . . ? C70 C69 H69A 108.2 . . ? C68 C69 H69A 108.2 . . ? C70 C69 H69B 108.2 . . ? C68 C69 H69B 108.2 . . ? H69A C69 H69B 107.4 . . ? C69 C70 C71 113.6(5) . . ? C69 C70 C71' 123.1(6) . . ? C71 C70 C71' 43.4(6) . . ? C69 C70 H70A 108.9 . . ? C71 C70 H70A 108.9 . . ? C71' C70 H70A 65.9 . . ? C69 C70 H70B 108.7 . . ? C71 C70 H70B 108.7 . . ? C71' C70 H70B 127.3 . . ? H70A C70 H70B 107.8 . . ? C69 C70 H70C 106.3 . . ? C71 C70 H70C 139.1 . . ? C71' C70 H70C 106.0 . . ? H70A C70 H70C 46.8 . . ? H70B C70 H70C 64.6 . . ? C69 C70 H70D 106.9 . . ? C71 C70 H70D 70.5 . . ? C71' C70 H70D 107.0 . . ? H70A C70 H70D 140.4 . . ? H70B C70 H70D 43.3 . . ? H70C C70 H70D 106.7 . . ? C70 C71 C72 110.5(5) . . ? C70 C71 H70D 37.9 . . ? C72 C71 H70D 144.6 . . ? C70 C71 H71A 109.5 . . ? C72 C71 H71A 109.5 . . ? H70D C71 H71A 99.3 . . ? C70 C71 H71B 109.5 . . ? C72 C71 H71B 109.5 . . ? H70D C71 H71B 79.1 . . ? H71A C71 H71B 108.1 . . ? C70 C71 H72C 142.4 . . ? C72 C71 H72C 35.6 . . ? H70D C71 H72C 155.2 . . ? H71A C71 H72C 100.5 . . ? H71B C71 H72C 80.7 . . ? C70 C71' C72 110.2(7) . . ? C70 C71' H70A 37.7 . . ? C72 C71' H70A 130.6 . . ? C70 C71' H71C 109.6 . . ? C72 C71' H71C 109.6 . . ? H70A C71' H71C 72.5 . . ? C70 C71' H71D 109.6 . . ? C72 C71' H71D 109.6 . . ? H70A C71' H71D 116.4 . . ? H71C C71' H71D 108.1 . . ? C70 C71' H72B 132.3 . . ? C72 C71' H72B 37.3 . . ? H70A C71' H72B 125.1 . . ? H71C C71' H72B 73.3 . . ? H71D C71' H72B 114.4 . . ? C67 C72 C71' 118.7(5) . . ? C67 C72 C71 109.3(4) . . ? C71' C72 C71 42.2(5) . . ? C67 C72 H72A 109.9 . . ? C71' C72 H72A 129.5 . . ? C71 C72 H72A 109.7 . . ? C67 C72 H72B 109.7 . . ? C71' C72 H72B 68.1 . . ? C71 C72 H72B 109.9 . . ? H72A C72 H72B 108.4 . . ? C67 C72 H72C 108.0 . . ? C71' C72 H72C 108.0 . . ? C71 C72 H72C 73.1 . . ? H72A C72 H72C 40.2 . . ? H72B C72 H72C 138.2 . . ? C67 C72 H72D 107.4 . . ? C71' C72 H72D 107.2 . . ? C71 C72 H72D 141.1 . . ? H72A C72 H72D 68.4 . . ? H72B C72 H72D 43.9 . . ? H72C C72 H72D 107.1 . . ? O3 C73 H73A 109.5 . . ? O3 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? O3 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N5 C74 C75 121.3(3) . . ? N5 C74 H74 119.4 . . ? C75 C74 H74 119.4 . . ? N6 C75 C76 111.1(3) . . ? N6 C75 C74 119.9(3) . . ? C76 C75 C74 128.9(3) . . ? C77 C76 C75 105.6(4) . . ? C77 C76 H76 127.2 . . ? C75 C76 H76 127.2 . . ? C76 C77 C78 107.2(4) . . ? C76 C77 H77 126.4 . . ? C78 C77 H77 126.4 . . ? N6 C78 C77 110.9(4) . . ? N6 C78 H78 124.5 . . ? C77 C78 H78 124.5 . . ? C80 C79 H79A 109.5 . . ? C80 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C80 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C81 C80 C85 120.0 . . ? C81 C80 C79 119.4(3) . . ? C85 C80 C79 120.6(3) . . ? C82 C81 C80 120.0 . . ? C82 C81 H81 120.0 . . ? C80 C81 H81 120.0 . . ? C81 C82 C83 120.0 . . ? C81 C82 H82 120.0 . . ? C83 C82 H82 120.0 . . ? C84 C83 C82 120.0 . . ? C84 C83 H83 120.0 . . ? C82 C83 H83 120.0 . . ? C83 C84 C85 120.0 . . ? C83 C84 H84 120.0 . . ? C85 C84 H84 120.0 . . ? C84 C85 C80 120.0 . . ? C84 C85 H85 120.0 . . ? C80 C85 H85 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Y1 N1 C22 -156.8(2) . . . . ? N6 Y1 N1 C22 124.3(3) . . . . ? N2 Y1 N1 C22 -4.8(2) . . . . ? N5 Y1 N1 C22 62.1(3) . . . . ? O1 Y1 N1 C22 -156.9(3) . . . . ? N3 Y1 N1 C22 -80.5(3) . . . . ? N4 Y1 N1 C12 40.8(4) . . . . ? N6 Y1 N1 C12 -38.1(3) . . . . ? N2 Y1 N1 C12 -167.2(3) . . . . ? N5 Y1 N1 C12 -100.3(3) . . . . ? O1 Y1 N1 C12 40.7(2) . . . . ? N3 Y1 N1 C12 117.1(3) . . . . ? N4 Y1 N2 C26 -15.4(4) . . . . ? N6 Y1 N2 C26 113.9(4) . . . . ? N5 Y1 N2 C26 52.2(4) . . . . ? N1 Y1 N2 C26 -178.0(4) . . . . ? O1 Y1 N2 C26 -137.6(3) . . . . ? N3 Y1 N2 C26 -68.0(4) . . . . ? N4 Y1 N2 C23 163.6(2) . . . . ? N6 Y1 N2 C23 -67.1(3) . . . . ? N5 Y1 N2 C23 -128.7(3) . . . . ? N1 Y1 N2 C23 1.0(2) . . . . ? O1 Y1 N2 C23 41.5(3) . . . . ? N3 Y1 N2 C23 111.1(3) . . . . ? N4 Y1 N3 C48 12.9(2) . . . . ? N6 Y1 N3 C48 -28.0(4) . . . . ? N2 Y1 N3 C48 155.4(3) . . . . ? N5 Y1 N3 C48 76.4(3) . . . . ? N1 Y1 N3 C48 -138.8(2) . . . . ? O1 Y1 N3 C48 -66.1(2) . . . . ? N4 Y1 N3 C38 177.4(3) . . . . ? N6 Y1 N3 C38 136.4(3) . . . . ? N2 Y1 N3 C38 -40.1(3) . . . . ? N5 Y1 N3 C38 -119.2(3) . . . . ? N1 Y1 N3 C38 25.7(3) . . . . ? O1 Y1 N3 C38 98.3(3) . . . . ? N6 Y1 N4 C52 -11.3(3) . . . . ? N2 Y1 N4 C52 128.6(3) . . . . ? N5 Y1 N4 C52 58.9(3) . . . . ? N1 Y1 N4 C52 -89.0(4) . . . . ? O1 Y1 N4 C52 -88.8(3) . . . . ? N3 Y1 N4 C52 -174.2(4) . . . . ? N6 Y1 N4 C49 148.8(3) . . . . ? N2 Y1 N4 C49 -71.3(3) . . . . ? N5 Y1 N4 C49 -141.1(3) . . . . ? N1 Y1 N4 C49 71.1(3) . . . . ? O1 Y1 N4 C49 71.2(2) . . . . ? N3 Y1 N4 C49 -14.1(2) . . . . ? N4 Y1 N5 C74 -81.9(2) . . . . ? N6 Y1 N5 C74 11.9(2) . . . . ? N2 Y1 N5 C74 140.8(2) . . . . ? N1 Y1 N5 C74 81.0(2) . . . . ? O1 Y1 N5 C74 -28.7(3) . . . . ? N3 Y1 N5 C74 -140.8(2) . . . . ? N4 Y1 N5 C64 88.9(3) . . . . ? N6 Y1 N5 C64 -177.3(3) . . . . ? N2 Y1 N5 C64 -48.3(3) . . . . ? N1 Y1 N5 C64 -108.1(3) . . . . ? O1 Y1 N5 C64 142.2(2) . . . . ? N3 Y1 N5 C64 30.1(3) . . . . ? N4 Y1 N6 C78 -101.8(4) . . . . ? N2 Y1 N6 C78 112.0(4) . . . . ? N5 Y1 N6 C78 -179.7(4) . . . . ? N1 Y1 N6 C78 51.5(4) . . . . ? O1 Y1 N6 C78 -25.3(4) . . . . ? N3 Y1 N6 C78 -63.9(4) . . . . ? N4 Y1 N6 C75 67.5(2) . . . . ? N2 Y1 N6 C75 -78.7(2) . . . . ? N5 Y1 N6 C75 -10.4(2) . . . . ? N1 Y1 N6 C75 -139.2(2) . . . . ? O1 Y1 N6 C75 144.0(2) . . . . ? N3 Y1 N6 C75 105.4(3) . . . . ? N4 Y1 O1 C2 -124.1(2) . . . . ? N6 Y1 O1 C2 143.3(2) . . . . ? N2 Y1 O1 C2 17.1(3) . . . . ? N5 Y1 O1 C2 -177.9(2) . . . . ? N1 Y1 O1 C2 55.8(2) . . . . ? N3 Y1 O1 C2 -53.1(2) . . . . ? N4 Y1 O1 C21 35.7(3) . . . . ? N6 Y1 O1 C21 -56.8(3) . . . . ? N2 Y1 O1 C21 177.0(3) . . . . ? N5 Y1 O1 C21 -18.1(3) . . . . ? N1 Y1 O1 C21 -144.3(3) . . . . ? N3 Y1 O1 C21 106.8(3) . . . . ? C6 C1 C2 C3 -8.8(6) . . . . ? C11 C1 C2 C3 169.4(4) . . . . ? C6 C1 C2 O1 169.1(3) . . . . ? C11 C1 C2 O1 -12.7(5) . . . . ? C21 O1 C2 C1 118.4(4) . . . . ? Y1 O1 C2 C1 -79.7(4) . . . . ? C21 O1 C2 C3 -63.7(5) . . . . ? Y1 O1 C2 C3 98.2(4) . . . . ? C1 C2 C3 C4 4.1(7) . . . . ? O1 C2 C3 C4 -173.7(4) . . . . ? C2 C3 C4 C5 2.1(8) . . . . ? C3 C4 C5 C6 -3.3(8) . . . . ? C3 C4 C5 C10 175.7(5) . . . . ? C2 C1 C6 C5 7.4(6) . . . . ? C11 C1 C6 C5 -170.8(4) . . . . ? C2 C1 C6 C7 -172.0(4) . . . . ? C11 C1 C6 C7 9.8(6) . . . . ? C4 C5 C6 C1 -1.5(7) . . . . ? C10 C5 C6 C1 179.5(5) . . . . ? C4 C5 C6 C7 177.8(5) . . . . ? C10 C5 C6 C7 -1.2(8) . . . . ? C1 C6 C7 C8 165.8(5) . . . . ? C5 C6 C7 C8 -13.5(7) . . . . ? C6 C7 C8 C9 44.7(6) . . . . ? C7 C8 C9 C10 -61.8(7) . . . . ? C4 C5 C10 C9 165.9(6) . . . . ? C6 C5 C10 C9 -15.1(9) . . . . ? C8 C9 C10 C5 45.7(8) . . . . ? C2 C1 C11 C12 77.7(5) . . . . ? C6 C1 C11 C12 -104.1(4) . . . . ? C2 C1 C11 C16 -103.3(4) . . . . ? C6 C1 C11 C16 74.9(5) . . . . ? C16 C11 C12 C13 -2.9(5) . . . . ? C1 C11 C12 C13 176.1(3) . . . . ? C16 C11 C12 N1 173.4(3) . . . . ? C1 C11 C12 N1 -7.6(5) . . . . ? C22 N1 C12 C11 125.1(4) . . . . ? Y1 N1 C12 C11 -73.1(4) . . . . ? C22 N1 C12 C13 -58.6(4) . . . . ? Y1 N1 C12 C13 103.1(3) . . . . ? C11 C12 C13 C14 0.9(5) . . . . ? N1 C12 C13 C14 -175.4(3) . . . . ? C12 C13 C14 C15 0.9(5) . . . . ? C13 C14 C15 C16 -0.6(5) . . . . ? C13 C14 C15 C20 -179.2(3) . . . . ? C14 C15 C16 C11 -1.4(5) . . . . ? C20 C15 C16 C11 177.1(3) . . . . ? C14 C15 C16 C17 178.9(3) . . . . ? C20 C15 C16 C17 -2.5(5) . . . . ? C12 C11 C16 C15 3.2(5) . . . . ? C1 C11 C16 C15 -175.8(3) . . . . ? C12 C11 C16 C17 -177.2(3) . . . . ? C1 C11 C16 C17 3.9(5) . . . . ? C15 C16 C17 C18 -14.8(5) . . . . ? C11 C16 C17 C18 165.5(4) . . . . ? C16 C17 C18 C19 46.3(5) . . . . ? C17 C18 C19 C20 -62.2(5) . . . . ? C18 C19 C20 C15 45.1(5) . . . . ? C14 C15 C20 C19 165.1(4) . . . . ? C16 C15 C20 C19 -13.4(5) . . . . ? C12 N1 C22 C23 171.8(3) . . . . ? Y1 N1 C22 C23 8.4(4) . . . . ? C26 N2 C23 C24 0.7(4) . . . . ? Y1 N2 C23 C24 -178.6(2) . . . . ? C26 N2 C23 C22 -178.0(3) . . . . ? Y1 N2 C23 C22 2.6(4) . . . . ? N1 C22 C23 N2 -7.7(5) . . . . ? N1 C22 C23 C24 173.9(4) . . . . ? N2 C23 C24 C25 -0.1(4) . . . . ? C22 C23 C24 C25 178.5(4) . . . . ? C23 C24 C25 C26 -0.6(5) . . . . ? C23 N2 C26 C25 -1.1(4) . . . . ? Y1 N2 C26 C25 178.0(3) . . . . ? C24 C25 C26 N2 1.1(5) . . . . ? C47 O2 C28 C27 -173.5(3) . . . . ? C47 O2 C28 C29 7.7(6) . . . . ? C32 C27 C28 O2 -176.1(3) . . . . ? C37 C27 C28 O2 -1.1(5) . . . . ? C32 C27 C28 C29 2.7(5) . . . . ? C37 C27 C28 C29 177.8(3) . . . . ? O2 C28 C29 C30 177.1(4) . . . . ? C27 C28 C29 C30 -1.7(6) . . . . ? C28 C29 C30 C31 -0.5(6) . . . . ? C29 C30 C31 C32 1.5(6) . . . . ? C29 C30 C31 C36 -176.9(4) . . . . ? C30 C31 C32 C27 -0.4(6) . . . . ? C36 C31 C32 C27 178.0(4) . . . . ? C30 C31 C32 C33 -176.6(4) . . . . ? C36 C31 C32 C33 1.8(6) . . . . ? C28 C27 C32 C31 -1.8(5) . . . . ? C37 C27 C32 C31 -177.0(3) . . . . ? C28 C27 C32 C33 174.5(3) . . . . ? C37 C27 C32 C33 -0.8(5) . . . . ? C31 C32 C33 C34 -13.9(5) . . . . ? C27 C32 C33 C34 169.8(4) . . . . ? C32 C33 C34 C35 40.7(7) . . . . ? C33 C34 C35 C36 -54.2(7) . . . . ? C34 C35 C36 C31 40.0(7) . . . . ? C30 C31 C36 C35 164.1(4) . . . . ? C32 C31 C36 C35 -14.2(6) . . . . ? C28 C27 C37 C38 99.5(4) . . . . ? C32 C27 C37 C38 -85.4(4) . . . . ? C28 C27 C37 C42 -86.7(4) . . . . ? C32 C27 C37 C42 88.4(4) . . . . ? C42 C37 C38 C39 -6.9(6) . . . . ? C27 C37 C38 C39 166.8(4) . . . . ? C42 C37 C38 N3 169.5(3) . . . . ? C27 C37 C38 N3 -16.7(6) . . . . ? C48 N3 C38 C39 130.2(4) . . . . ? Y1 N3 C38 C39 -33.6(5) . . . . ? C48 N3 C38 C37 -46.3(5) . . . . ? Y1 N3 C38 C37 149.9(3) . . . . ? C37 C38 C39 C40 3.9(6) . . . . ? N3 C38 C39 C40 -172.7(4) . . . . ? C38 C39 C40 C41 2.4(7) . . . . ? C39 C40 C41 C42 -5.5(7) . . . . ? C39 C40 C41 C46 174.7(4) . . . . ? C40 C41 C42 C37 2.3(6) . . . . ? C46 C41 C42 C37 -177.9(4) . . . . ? C40 C41 C42 C43 -175.8(4) . . . . ? C46 C41 C42 C43 4.0(6) . . . . ? C38 C37 C42 C41 3.8(6) . . . . ? C27 C37 C42 C41 -170.2(4) . . . . ? C38 C37 C42 C43 -178.0(4) . . . . ? C27 C37 C42 C43 7.9(5) . . . . ? C41 C42 C43 C44 -15.5(6) . . . . ? C37 C42 C43 C44 166.4(4) . . . . ? C42 C43 C44 C45 44.4(5) . . . . ? C43 C44 C45 C46 -62.8(5) . . . . ? C44 C45 C46 C41 50.0(5) . . . . ? C42 C41 C46 C45 -21.4(6) . . . . ? C40 C41 C46 C45 158.4(4) . . . . ? C38 N3 C48 C49 -178.3(3) . . . . ? Y1 N3 C48 C49 -11.1(4) . . . . ? C52 N4 C49 C50 -0.5(4) . . . . ? Y1 N4 C49 C50 -166.7(3) . . . . ? C52 N4 C49 C48 -179.0(3) . . . . ? Y1 N4 C49 C48 14.8(4) . . . . ? N3 C48 C49 N4 -1.9(6) . . . . ? N3 C48 C49 C50 -180.0(4) . . . . ? N4 C49 C50 C51 0.6(5) . . . . ? C48 C49 C50 C51 178.8(4) . . . . ? C49 C50 C51 C52 -0.4(5) . . . . ? C49 N4 C52 C51 0.3(4) . . . . ? Y1 N4 C52 C51 161.5(3) . . . . ? C50 C51 C52 N4 0.1(5) . . . . ? C73 O3 C54 C55 18.0(5) . . . . ? C73 O3 C54 C53 -158.9(3) . . . . ? C58 C53 C54 O3 178.4(3) . . . . ? C63 C53 C54 O3 0.2(5) . . . . ? C58 C53 C54 C55 1.5(6) . . . . ? C63 C53 C54 C55 -176.7(3) . . . . ? O3 C54 C55 C56 -178.0(3) . . . . ? C53 C54 C55 C56 -1.3(6) . . . . ? C54 C55 C56 C57 0.4(6) . . . . ? C55 C56 C57 C58 0.3(6) . . . . ? C55 C56 C57 C62 179.0(4) . . . . ? C54 C53 C58 C57 -0.8(6) . . . . ? C63 C53 C58 C57 177.4(3) . . . . ? C54 C53 C58 C59 -177.9(3) . . . . ? C63 C53 C58 C59 0.2(5) . . . . ? C56 C57 C58 C53 -0.1(6) . . . . ? C62 C57 C58 C53 -178.8(4) . . . . ? C56 C57 C58 C59 177.0(3) . . . . ? C62 C57 C58 C59 -1.7(6) . . . . ? C53 C58 C59 C60 -169.9(4) . . . . ? C57 C58 C59 C60 12.9(5) . . . . ? C58 C59 C60 C61 -44.2(5) . . . . ? C59 C60 C61 C62 64.1(5) . . . . ? C56 C57 C62 C61 -157.4(4) . . . . ? C58 C57 C62 C61 21.3(6) . . . . ? C60 C61 C62 C57 -51.9(5) . . . . ? C54 C53 C63 C64 91.1(4) . . . . ? C58 C53 C63 C64 -87.1(4) . . . . ? C54 C53 C63 C68 -91.2(4) . . . . ? C58 C53 C63 C68 90.6(4) . . . . ? C68 C63 C64 C65 1.9(5) . . . . ? C53 C63 C64 C65 179.6(3) . . . . ? C68 C63 C64 N5 -173.2(3) . . . . ? C53 C63 C64 N5 4.5(5) . . . . ? C74 N5 C64 C65 132.3(3) . . . . ? Y1 N5 C64 C65 -38.2(4) . . . . ? C74 N5 C64 C63 -52.6(4) . . . . ? Y1 N5 C64 C63 137.0(3) . . . . ? C63 C64 C65 C66 -0.2(5) . . . . ? N5 C64 C65 C66 175.1(3) . . . . ? C64 C65 C66 C67 -2.3(5) . . . . ? C65 C66 C67 C68 3.0(5) . . . . ? C65 C66 C67 C72 -173.8(4) . . . . ? C66 C67 C68 C63 -1.3(5) . . . . ? C72 C67 C68 C63 175.5(3) . . . . ? C66 C67 C68 C69 178.2(3) . . . . ? C72 C67 C68 C69 -5.0(5) . . . . ? C64 C63 C68 C67 -1.2(5) . . . . ? C53 C63 C68 C67 -178.9(3) . . . . ? C64 C63 C68 C69 179.3(3) . . . . ? C53 C63 C68 C69 1.6(4) . . . . ? C67 C68 C69 C70 3.5(6) . . . . ? C63 C68 C69 C70 -177.0(4) . . . . ? C68 C69 C70 C71 29.0(7) . . . . ? C68 C69 C70 C71' -19.5(10) . . . . ? C69 C70 C71 C72 -58.8(8) . . . . ? C71' C70 C71 C72 55.0(7) . . . . ? C69 C70 C71' C72 33.6(13) . . . . ? C71 C70 C71' C72 -56.8(7) . . . . ? C66 C67 C72 C71' -161.8(7) . . . . ? C68 C67 C72 C71' 21.4(8) . . . . ? C66 C67 C72 C71 152.9(5) . . . . ? C68 C67 C72 C71 -23.9(6) . . . . ? C70 C71' C72 C67 -33.2(12) . . . . ? C70 C71' C72 C71 54.3(7) . . . . ? C70 C71 C72 C67 55.0(8) . . . . ? C70 C71 C72 C71' -56.9(7) . . . . ? C64 N5 C74 C75 175.8(3) . . . . ? Y1 N5 C74 C75 -12.3(4) . . . . ? C78 N6 C75 C76 0.0(4) . . . . ? Y1 N6 C75 C76 -173.0(3) . . . . ? C78 N6 C75 C74 -178.1(3) . . . . ? Y1 N6 C75 C74 8.9(4) . . . . ? N5 C74 C75 N6 2.6(5) . . . . ? N5 C74 C75 C76 -175.1(4) . . . . ? N6 C75 C76 C77 -0.5(5) . . . . ? C74 C75 C76 C77 177.4(4) . . . . ? C75 C76 C77 C78 0.7(5) . . . . ? C75 N6 C78 C77 0.5(4) . . . . ? Y1 N6 C78 C77 170.3(3) . . . . ? C76 C77 C78 N6 -0.8(5) . . . . ? C85 C80 C81 C82 0.0 . . . . ? C79 C80 C81 C82 -177.5(7) . . . . ? C80 C81 C82 C83 0.0 . . . . ? C81 C82 C83 C84 0.0 . . . . ? C82 C83 C84 C85 0.0 . . . . ? C83 C84 C85 C80 0.0 . . . . ? C81 C80 C85 C84 0.0 . . . . ? C79 C80 C85 C84 177.5(7) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.139 0.250 0.000 603.2 62.9 2 0.128 0.750 0.500 603.1 63.2 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.585 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.064