# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Manfred Bochmann' 'Carlos Alonso-Moreno' 'Lewis Broomfield' 'Ruth H Howard' 'David L Hughes' 'Joseph Wright' _publ_contact_author_name 'Manfred Bochmann' _publ_contact_author_email M.BOCHMANN@UEA.AC.UK _publ_section_title ; Synthesis and Structures of Complexes with Axially Chiral Isoquinolinyl-Naphtholate Ligands ; # Attachment 'Chiral_ligands.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 728910' _chemical_formula_moiety 'C19 H25 Br O' _chemical_formula_structural 1-Br-2-OMe-3,6-Bu(t)-C10H4 _chemical_formula_sum 'C19 H25 Br O' _chemical_formula_weight 349.30 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.0253(5) _cell_length_b 19.8448(15) _cell_length_c 15.0745(7) _cell_angle_alpha 90.00 _cell_angle_beta 88.889(5) _cell_angle_gamma 90.00 _cell_volume 1802.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.85 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 2.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.276 _exptl_absorpt_correction_T_max 0.553 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 21770 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4110 _reflns_number_gt 2231 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0588P)^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_number_reflns 4110 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _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 Br1 Br 0.24040(6) 0.175444(15) 0.329497(17) 0.08456(16) Uani 1 1 d . . . C1 C 0.2896(4) 0.21060(11) 0.44498(13) 0.0474(5) Uani 1 1 d . . . C2 C 0.1959(3) 0.27092(11) 0.46824(14) 0.0437(5) Uani 1 1 d . . . O2 O 0.0582(3) 0.30404(8) 0.41099(11) 0.0570(4) Uani 1 1 d . . . C21 C -0.1583(4) 0.27465(16) 0.4006(2) 0.0801(9) Uani 1 1 d . . . H21A H -0.2415 0.3012 0.3596 0.120 Uiso 1 1 calc R . . H21B H -0.2349 0.2736 0.4570 0.120 Uiso 1 1 calc R . . H21C H -0.1427 0.2296 0.3782 0.120 Uiso 1 1 calc R . . C3 C 0.2517(3) 0.30272(11) 0.55047(14) 0.0423(5) Uani 1 1 d . . . C31 C 0.1701(4) 0.37382(11) 0.57482(16) 0.0520(6) Uani 1 1 d . . . C32 C 0.2571(5) 0.42432(13) 0.5052(2) 0.0781(8) Uani 1 1 d . . . H32A H 0.2058 0.4687 0.5202 0.117 Uiso 1 1 calc R . . H32B H 0.2034 0.4121 0.4478 0.117 Uiso 1 1 calc R . . H32C H 0.4164 0.4237 0.5039 0.117 Uiso 1 1 calc R . . C33 C -0.0868(4) 0.37625(15) 0.5804(2) 0.0764(8) Uani 1 1 d . . . H33A H -0.1341 0.4211 0.5953 0.115 Uiso 1 1 calc R . . H33B H -0.1393 0.3455 0.6252 0.115 Uiso 1 1 calc R . . H33C H -0.1462 0.3637 0.5241 0.115 Uiso 1 1 calc R . . C34 C 0.2545(4) 0.39598(14) 0.66491(18) 0.0722(8) Uani 1 1 d . . . H34A H 0.2012 0.4405 0.6780 0.108 Uiso 1 1 calc R . . H34B H 0.4139 0.3960 0.6636 0.108 Uiso 1 1 calc R . . H34C H 0.2017 0.3653 0.7098 0.108 Uiso 1 1 calc R . . C4 C 0.3888(3) 0.26749(10) 0.60506(14) 0.0450(5) Uani 1 1 d . . . H4 H 0.4240 0.2866 0.6594 0.054 Uiso 1 1 calc R . . C5 C 0.6254(3) 0.17049(10) 0.64250(14) 0.0458(5) Uani 1 1 d . . . H5 H 0.6560 0.1906 0.6966 0.055 Uiso 1 1 calc R . . C6 C 0.7217(3) 0.10997(10) 0.62225(14) 0.0451(5) Uani 1 1 d . . . C61 C 0.8742(4) 0.07305(11) 0.68665(15) 0.0518(6) Uani 1 1 d . . . C62 C 0.7290(5) 0.02672(14) 0.74440(19) 0.0788(8) Uani 1 1 d . . . H62A H 0.8202 0.0031 0.7856 0.118 Uiso 1 1 calc R . . H62B H 0.6548 -0.0052 0.7074 0.118 Uiso 1 1 calc R . . H62C H 0.6207 0.0532 0.7764 0.118 Uiso 1 1 calc R . . C63 C 0.9922(5) 0.12282(15) 0.7473(2) 0.0807(8) Uani 1 1 d . . . H63A H 1.0863 0.0985 0.7868 0.121 Uiso 1 1 calc R . . H63B H 0.8839 0.1479 0.7813 0.121 Uiso 1 1 calc R . . H63C H 1.0805 0.1533 0.7120 0.121 Uiso 1 1 calc R . . C64 C 1.0494(5) 0.03060(17) 0.6387(2) 0.0926(10) Uani 1 1 d . . . H64A H 1.1410 0.0088 0.6814 0.139 Uiso 1 1 calc R . . H64B H 1.1397 0.0591 0.6013 0.139 Uiso 1 1 calc R . . H64C H 0.9779 -0.0028 0.6031 0.139 Uiso 1 1 calc R . . C7 C 0.6699(4) 0.08070(12) 0.53973(16) 0.0570(6) Uani 1 1 d . . . H7 H 0.7328 0.0394 0.5246 0.068 Uiso 1 1 calc R . . C8 C 0.5310(4) 0.11091(11) 0.48148(16) 0.0583(6) Uani 1 1 d . . . H8 H 0.5005 0.0898 0.4280 0.070 Uiso 1 1 calc R . . C9 C 0.4324(4) 0.17398(10) 0.50130(14) 0.0445(5) Uani 1 1 d . . . C10 C 0.4797(3) 0.20386(10) 0.58361(13) 0.0410(5) Uani 1 1 d . . . 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 Br1 0.1317(3) 0.0779(2) 0.04527(18) -0.01568(13) -0.03316(16) 0.01907(17) C1 0.0636(14) 0.0465(13) 0.0324(11) -0.0025(9) -0.0083(10) -0.0051(11) C2 0.0461(12) 0.0452(13) 0.0400(12) 0.0080(9) -0.0043(9) -0.0037(10) O2 0.0581(10) 0.0615(10) 0.0521(10) 0.0119(8) -0.0157(7) 0.0005(8) C21 0.0616(17) 0.098(2) 0.082(2) -0.0018(16) -0.0270(14) -0.0060(16) C3 0.0405(12) 0.0438(12) 0.0427(12) -0.0003(9) 0.0005(9) -0.0030(9) C31 0.0518(14) 0.0435(13) 0.0608(15) -0.0026(11) -0.0035(11) 0.0080(11) C32 0.099(2) 0.0442(14) 0.091(2) 0.0086(14) 0.0023(16) 0.0017(14) C33 0.0587(17) 0.084(2) 0.087(2) -0.0168(16) -0.0040(14) 0.0189(14) C34 0.0785(18) 0.0582(16) 0.081(2) -0.0284(14) -0.0184(15) 0.0162(14) C4 0.0557(13) 0.0419(12) 0.0375(12) -0.0054(9) -0.0051(10) 0.0015(10) C5 0.0573(14) 0.0448(13) 0.0355(11) -0.0037(9) -0.0062(9) 0.0020(11) C6 0.0546(13) 0.0412(12) 0.0395(12) 0.0007(9) 0.0016(10) 0.0019(10) C61 0.0548(14) 0.0509(14) 0.0496(14) 0.0048(11) -0.0017(11) 0.0068(11) C62 0.0877(19) 0.073(2) 0.0755(19) 0.0287(16) -0.0079(15) -0.0010(15) C63 0.0870(19) 0.076(2) 0.080(2) 0.0046(15) -0.0363(16) 0.0050(16) C64 0.090(2) 0.114(3) 0.073(2) -0.0033(18) -0.0027(16) 0.0513(19) C7 0.0769(17) 0.0421(13) 0.0520(15) -0.0063(11) -0.0025(12) 0.0122(12) C8 0.0824(17) 0.0481(14) 0.0448(13) -0.0124(11) -0.0117(12) 0.0073(12) C9 0.0562(13) 0.0393(12) 0.0381(11) -0.0018(9) -0.0040(9) -0.0024(10) C10 0.0495(12) 0.0381(11) 0.0354(11) 0.0001(9) -0.0034(9) -0.0006(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 Br1 C1 1.904(2) . ? C1 C2 1.366(3) . ? C1 C9 1.421(3) . ? C2 O2 1.376(2) . ? C2 C3 1.437(3) . ? O2 C21 1.440(3) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C3 C4 1.369(3) . ? C3 C31 1.536(3) . ? C31 C34 1.524(3) . ? C31 C32 1.537(3) . ? C31 C33 1.549(3) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C4 C10 1.411(3) . ? C4 H4 0.9300 . ? C5 C6 1.366(3) . ? C5 C10 1.424(3) . ? C5 H5 0.9300 . ? C6 C7 1.413(3) . ? C6 C61 1.535(3) . ? C61 C64 1.522(3) . ? C61 C62 1.529(3) . ? C61 C63 1.531(4) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C7 C8 1.364(3) . ? C7 H7 0.9300 . ? C8 C9 1.415(3) . ? C8 H8 0.9300 . ? C9 C10 1.409(3) . ? 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 C1 C9 123.15(19) . . ? C2 C1 Br1 119.01(16) . . ? C9 C1 Br1 117.76(16) . . ? C1 C2 O2 120.58(19) . . ? C1 C2 C3 120.26(18) . . ? O2 C2 C3 119.03(19) . . ? C2 O2 C21 115.68(19) . . ? O2 C21 H21A 109.5 . . ? O2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C4 C3 C2 116.63(19) . . ? C4 C3 C31 121.29(19) . . ? C2 C3 C31 122.04(18) . . ? C34 C31 C3 111.53(19) . . ? C34 C31 C32 107.8(2) . . ? C3 C31 C32 109.41(19) . . ? C34 C31 C33 107.1(2) . . ? C3 C31 C33 110.88(19) . . ? C32 C31 C33 110.1(2) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C3 C4 C10 123.7(2) . . ? C3 C4 H4 118.1 . . ? C10 C4 H4 118.1 . . ? C6 C5 C10 122.28(19) . . ? C6 C5 H5 118.9 . . ? C10 C5 H5 118.9 . . ? C5 C6 C7 117.2(2) . . ? C5 C6 C61 122.36(19) . . ? C7 C6 C61 120.36(19) . . ? C64 C61 C62 108.8(2) . . ? C64 C61 C63 108.4(2) . . ? C62 C61 C63 108.4(2) . . ? C64 C61 C6 112.4(2) . . ? C62 C61 C6 107.70(19) . . ? C63 C61 C6 111.14(19) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C8 C7 C6 122.3(2) . . ? C8 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C7 C8 C9 120.9(2) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 117.85(19) . . ? C10 C9 C1 116.49(18) . . ? C8 C9 C1 125.65(19) . . ? C9 C10 C4 119.61(19) . . ? C9 C10 C5 119.40(19) . . ? C4 C10 C5 120.96(18) . . ? 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 C9 C1 C2 O2 -179.81(19) . . . . ? Br1 C1 C2 O2 3.5(3) . . . . ? C9 C1 C2 C3 4.3(3) . . . . ? Br1 C1 C2 C3 -172.36(15) . . . . ? C1 C2 O2 C21 72.5(3) . . . . ? C3 C2 O2 C21 -111.5(2) . . . . ? C1 C2 C3 C4 -4.2(3) . . . . ? O2 C2 C3 C4 179.83(19) . . . . ? C1 C2 C3 C31 173.39(19) . . . . ? O2 C2 C3 C31 -2.6(3) . . . . ? C4 C3 C31 C34 -1.9(3) . . . . ? C2 C3 C31 C34 -179.4(2) . . . . ? C4 C3 C31 C32 117.3(2) . . . . ? C2 C3 C31 C32 -60.2(3) . . . . ? C4 C3 C31 C33 -121.1(2) . . . . ? C2 C3 C31 C33 61.4(3) . . . . ? C2 C3 C4 C10 1.6(3) . . . . ? C31 C3 C4 C10 -175.97(19) . . . . ? C10 C5 C6 C7 -0.5(3) . . . . ? C10 C5 C6 C61 -178.4(2) . . . . ? C5 C6 C61 C64 -150.0(2) . . . . ? C7 C6 C61 C64 32.1(3) . . . . ? C5 C6 C61 C62 90.2(3) . . . . ? C7 C6 C61 C62 -87.7(3) . . . . ? C5 C6 C61 C63 -28.4(3) . . . . ? C7 C6 C61 C63 153.8(2) . . . . ? C5 C6 C7 C8 0.4(3) . . . . ? C61 C6 C7 C8 178.3(2) . . . . ? C6 C7 C8 C9 0.4(4) . . . . ? C7 C8 C9 C10 -1.1(3) . . . . ? C7 C8 C9 C1 178.6(2) . . . . ? C2 C1 C9 C10 -1.5(3) . . . . ? Br1 C1 C9 C10 175.14(15) . . . . ? C2 C1 C9 C8 178.8(2) . . . . ? Br1 C1 C9 C8 -4.5(3) . . . . ? C8 C9 C10 C4 178.55(19) . . . . ? C1 C9 C10 C4 -1.1(3) . . . . ? C8 C9 C10 C5 0.9(3) . . . . ? C1 C9 C10 C5 -178.73(19) . . . . ? C3 C4 C10 C9 1.0(3) . . . . ? C3 C4 C10 C5 178.6(2) . . . . ? C6 C5 C10 C9 -0.2(3) . . . . ? C6 C5 C10 C4 -177.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.386 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.048 #===END data_L(H)-H _database_code_depnum_ccdc_archive 'CCDC 728911' _chemical_formula_moiety 'C27 H29 N O' _chemical_formula_structural L(H)-H _chemical_formula_sum 'C27 H29 N O' _chemical_formula_weight 383.51 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.228(3) _cell_length_b 11.794(2) _cell_length_c 25.429(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.175(15) _cell_angle_gamma 90.00 _cell_volume 4697.1(14) _cell_formula_units_Z 8 _cell_measurement_temperature 295(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.85 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 29252 _diffrn_reflns_av_R_equivalents 0.1458 _diffrn_reflns_av_sigmaI/netI 0.1379 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 20.00 _reflns_number_total 4361 _reflns_number_gt 2295 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0197P)^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_number_reflns 4361 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1743 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0714 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 C1 C 0.4238(3) 0.3594(5) 0.2099(2) 0.0448(16) Uani 1 1 d . A . C2 C 0.4176(3) 0.2580(5) 0.1824(2) 0.0511(17) Uani 1 1 d . . . O2 O 0.3514(3) 0.1845(3) 0.18245(16) 0.0623(13) Uani 1 1 d . . . C3 C 0.4792(3) 0.2218(5) 0.1548(2) 0.0494(17) Uani 1 1 d . . . C31 C 0.4728(4) 0.1062(5) 0.1252(3) 0.0658(19) Uani 1 1 d . . . C32 C 0.3889(4) 0.0990(4) 0.0796(3) 0.097(2) Uani 1 1 d . . . H32A H 0.3413 0.1092 0.0950 0.146 Uiso 1 1 calc R . . H32B H 0.3849 0.0261 0.0623 0.146 Uiso 1 1 calc R . . H32C H 0.3882 0.1573 0.0531 0.146 Uiso 1 1 calc R . . C33 C 0.5474(3) 0.0882(4) 0.0994(3) 0.103(2) Uani 1 1 d . . . H33A H 0.6003 0.0905 0.1272 0.155 Uiso 1 1 calc R . . H33B H 0.5470 0.1469 0.0732 0.155 Uiso 1 1 calc R . . H33C H 0.5416 0.0157 0.0816 0.155 Uiso 1 1 calc R . . C34 C 0.4769(3) 0.0108(5) 0.1678(3) 0.097(2) Uani 1 1 d . . . H34A H 0.5299 0.0157 0.1954 0.145 Uiso 1 1 calc R . . H34B H 0.4729 -0.0617 0.1501 0.145 Uiso 1 1 calc R . . H34C H 0.4303 0.0194 0.1842 0.145 Uiso 1 1 calc R . . C4 C 0.5447(3) 0.2965(5) 0.1561(2) 0.0511(16) Uani 1 1 d . . . H4 H 0.5858 0.2761 0.1383 0.061 Uiso 1 1 calc R . . C5 C 0.6216(3) 0.4782(5) 0.1824(2) 0.0521(17) Uani 1 1 d . . . H5 H 0.6618 0.4556 0.1644 0.063 Uiso 1 1 calc R . . C6 C 0.6305(3) 0.5820(5) 0.2071(2) 0.0476(16) Uani 1 1 d . A . C61 C 0.7022(4) 0.6659(5) 0.2068(3) 0.070(2) Uani 1 1 d . . . C62 C 0.7676(6) 0.6190(7) 0.1804(5) 0.103(5) Uani 0.769(11) 1 d P A 1 H62A H 0.7399 0.5946 0.1440 0.154 Uiso 0.769(11) 1 calc PR A 1 H62B H 0.7960 0.5558 0.2012 0.154 Uiso 0.769(11) 1 calc PR A 1 H62C H 0.8087 0.6768 0.1790 0.154 Uiso 0.769(11) 1 calc PR A 1 C63 C 0.7432(8) 0.7097(14) 0.2624(5) 0.172(8) Uani 0.769(11) 1 d P A 1 H63A H 0.7002 0.7384 0.2785 0.258 Uiso 0.769(11) 1 calc PR A 1 H63B H 0.7822 0.7695 0.2600 0.258 Uiso 0.769(11) 1 calc PR A 1 H63C H 0.7738 0.6494 0.2845 0.258 Uiso 0.769(11) 1 calc PR A 1 C64 C 0.6598(6) 0.7664(9) 0.1678(7) 0.173(8) Uani 0.769(11) 1 d P A 1 H64A H 0.6160 0.8010 0.1814 0.260 Uiso 0.769(11) 1 calc PR A 1 H64B H 0.6352 0.7374 0.1318 0.260 Uiso 0.769(11) 1 calc PR A 1 H64C H 0.7025 0.8219 0.1664 0.260 Uiso 0.769(11) 1 calc PR A 1 C65 C 0.701(2) 0.775(3) 0.2342(18) 0.067(11) Uiso 0.231(11) 1 d P A 2 H65A H 0.7475 0.8208 0.2301 0.100 Uiso 0.231(11) 1 calc PR A 2 H65B H 0.7060 0.7619 0.2722 0.100 Uiso 0.231(11) 1 calc PR A 2 H65C H 0.6478 0.8128 0.2182 0.100 Uiso 0.231(11) 1 calc PR A 2 C66 C 0.710(2) 0.677(3) 0.1522(14) 0.102(14) Uiso 0.231(11) 1 d P A 2 H66A H 0.7013 0.6041 0.1345 0.153 Uiso 0.231(11) 1 calc PR A 2 H66B H 0.7667 0.7033 0.1531 0.153 Uiso 0.231(11) 1 calc PR A 2 H66C H 0.6688 0.7296 0.1324 0.153 Uiso 0.231(11) 1 calc PR A 2 C67 C 0.7936(14) 0.595(2) 0.2431(13) 0.069(11) Uiso 0.231(11) 1 d P A 2 H67A H 0.7954 0.5211 0.2277 0.104 Uiso 0.231(11) 1 calc PR A 2 H67B H 0.7924 0.5878 0.2805 0.104 Uiso 0.231(11) 1 calc PR A 2 H67C H 0.8432 0.6373 0.2411 0.104 Uiso 0.231(11) 1 calc PR A 2 C7 C 0.5679(3) 0.6122(4) 0.2339(2) 0.0545(17) Uani 1 1 d . . . H7 H 0.5720 0.6826 0.2509 0.065 Uiso 1 1 calc R A . C8 C 0.5018(3) 0.5432(5) 0.2361(2) 0.0510(16) Uani 1 1 d . A . H8 H 0.4628 0.5668 0.2549 0.061 Uiso 1 1 calc R . . C9 C 0.4915(3) 0.4352(5) 0.2100(2) 0.0421(15) Uani 1 1 d . . . C10 C 0.5535(3) 0.4036(4) 0.1832(2) 0.0418(15) Uani 1 1 d . A . C11 C 0.3654(3) 0.3884(5) 0.2448(3) 0.0435(16) Uani 1 1 d . . . N12 N 0.3043(3) 0.4631(4) 0.2257(2) 0.0519(13) Uani 1 1 d . A . C13 C 0.2552(3) 0.4987(4) 0.2589(3) 0.0595(19) Uani 1 1 d . . . H13 H 0.2127 0.5519 0.2454 0.071 Uiso 1 1 calc R A . C14 C 0.2654(4) 0.4605(5) 0.3103(3) 0.070(2) Uani 1 1 d . A . H14 H 0.2305 0.4875 0.3313 0.084 Uiso 1 1 calc R . . C15 C 0.3433(5) 0.3355(6) 0.3849(3) 0.097(2) Uani 1 1 d . A . H15 H 0.3102 0.3605 0.4075 0.116 Uiso 1 1 calc R . . C16 C 0.4041(6) 0.2573(7) 0.4035(4) 0.131(3) Uani 1 1 d . . . H16 H 0.4121 0.2281 0.4384 0.157 Uiso 1 1 calc R . . C17 C 0.4563(5) 0.2187(6) 0.3702(4) 0.116(3) Uani 1 1 d . A . H17 H 0.4990 0.1655 0.3836 0.139 Uiso 1 1 calc R . . C18 C 0.4439(4) 0.2598(5) 0.3185(3) 0.086(2) Uani 1 1 d . . . H18 H 0.4779 0.2340 0.2967 0.103 Uiso 1 1 calc R A . C19 C 0.3803(4) 0.3405(5) 0.2980(3) 0.0524(17) Uani 1 1 d . A . C20 C 0.3285(4) 0.3805(5) 0.3319(3) 0.0595(18) Uani 1 1 d . . . C1A C 0.6939(3) 0.1619(5) 0.5828(2) 0.0476(17) Uani 1 1 d . . . C2A C 0.7434(3) 0.0687(5) 0.5787(3) 0.0486(16) Uani 1 1 d . . . O2A O 0.7558(2) -0.0156(3) 0.6169(2) 0.0614(14) Uani 1 1 d . . . C3A C 0.7805(3) 0.0526(5) 0.5335(2) 0.0460(16) Uani 1 1 d . . . C31A C 0.8358(4) -0.0512(5) 0.5295(3) 0.0547(17) Uani 1 1 d . . . C32A C 0.9160(4) -0.0502(4) 0.5771(2) 0.084(2) Uani 1 1 d . . . H32D H 0.9507 -0.1148 0.5746 0.126 Uiso 1 1 calc R . . H32E H 0.8999 -0.0530 0.6108 0.126 Uiso 1 1 calc R . . H32F H 0.9478 0.0180 0.5758 0.126 Uiso 1 1 calc R . . C33A C 0.7866(3) -0.1622(4) 0.5302(2) 0.091(2) Uani 1 1 d . . . H33D H 0.8226 -0.2255 0.5276 0.137 Uiso 1 1 calc R . . H33E H 0.7368 -0.1633 0.4999 0.137 Uiso 1 1 calc R . . H33F H 0.7697 -0.1672 0.5636 0.137 Uiso 1 1 calc R . . C34A C 0.8652(3) -0.0498(4) 0.4766(2) 0.086(2) Uani 1 1 d . . . H34D H 0.8996 -0.1155 0.4754 0.129 Uiso 1 1 calc R . . H34E H 0.8981 0.0174 0.4756 0.129 Uiso 1 1 calc R . . H34F H 0.8161 -0.0504 0.4457 0.129 Uiso 1 1 calc R . . C4A C 0.7642(3) 0.1357(5) 0.4946(2) 0.0498(17) Uani 1 1 d . . . H4A H 0.7869 0.1273 0.4648 0.060 Uiso 1 1 calc R . . C5A C 0.7019(3) 0.3204(5) 0.4567(2) 0.0575(17) Uani 1 1 d . . . H5A H 0.7256 0.3109 0.4274 0.069 Uiso 1 1 calc R . . C6A C 0.6558(3) 0.4181(5) 0.4588(3) 0.0531(17) Uani 1 1 d . . . C61A C 0.6442(4) 0.5131(5) 0.4163(3) 0.070(2) Uani 1 1 d . . . C62A C 0.6755(4) 0.4784(5) 0.3670(3) 0.141(3) Uani 1 1 d . . . H62D H 0.6663 0.5396 0.3413 0.211 Uiso 1 1 calc R . . H62E H 0.6445 0.4128 0.3502 0.211 Uiso 1 1 calc R . . H62F H 0.7353 0.4609 0.3786 0.211 Uiso 1 1 calc R . . C63A C 0.6950(5) 0.6133(6) 0.4427(3) 0.207(5) Uani 1 1 d . . . H63D H 0.6879 0.6744 0.4169 0.310 Uiso 1 1 calc R . . H63E H 0.7543 0.5930 0.4546 0.310 Uiso 1 1 calc R . . H63F H 0.6754 0.6368 0.4735 0.310 Uiso 1 1 calc R . . C64A C 0.5508(4) 0.5441(5) 0.3954(3) 0.142(3) Uani 1 1 d . . . H64D H 0.5447 0.6038 0.3690 0.213 Uiso 1 1 calc R . . H64E H 0.5294 0.5692 0.4252 0.213 Uiso 1 1 calc R . . H64F H 0.5191 0.4789 0.3787 0.213 Uiso 1 1 calc R . . C7A C 0.6217(3) 0.4286(5) 0.5047(3) 0.0636(18) Uani 1 1 d . . . H7A H 0.5908 0.4934 0.5080 0.076 Uiso 1 1 calc R . . C8A C 0.6327(3) 0.3470(5) 0.5443(2) 0.0572(17) Uani 1 1 d . . . H8A H 0.6088 0.3575 0.5734 0.069 Uiso 1 1 calc R . . C9A C 0.6795(3) 0.2474(5) 0.5418(3) 0.0459(16) Uani 1 1 d . . . C10A C 0.7150(3) 0.2334(5) 0.4970(2) 0.0459(16) Uani 1 1 d . . . C11A C 0.6496(4) 0.1706(4) 0.6275(3) 0.0411(15) Uani 1 1 d . . . N12A N 0.6928(3) 0.2247(4) 0.6721(2) 0.0491(14) Uani 1 1 d . . . C13A C 0.6545(4) 0.2336(4) 0.7142(3) 0.0555(17) Uani 1 1 d . . . H13A H 0.6841 0.2710 0.7457 0.067 Uiso 1 1 calc R . . C14A C 0.5759(4) 0.1910(4) 0.7125(3) 0.0567(18) Uani 1 1 d . . . H14A H 0.5537 0.1968 0.7426 0.068 Uiso 1 1 calc R . . C15A C 0.4449(4) 0.0959(5) 0.6583(3) 0.070(2) Uani 1 1 d . . . H15A H 0.4200 0.0994 0.6873 0.083 Uiso 1 1 calc R . . C16A C 0.4014(4) 0.0507(5) 0.6104(4) 0.082(2) Uani 1 1 d . . . H16A H 0.3463 0.0239 0.6069 0.098 Uiso 1 1 calc R . . C17A C 0.4365(4) 0.0429(5) 0.5656(3) 0.078(2) Uani 1 1 d . . . H17A H 0.4049 0.0123 0.5328 0.093 Uiso 1 1 calc R . . C18A C 0.5180(4) 0.0810(5) 0.5709(3) 0.0635(18) Uani 1 1 d . . . H18A H 0.5422 0.0752 0.5416 0.076 Uiso 1 1 calc R . . C19A C 0.5653(4) 0.1289(4) 0.6202(3) 0.0476(16) Uani 1 1 d . . . C20A C 0.5290(4) 0.1383(4) 0.6646(3) 0.0484(16) Uani 1 1 d . . . H2A H 0.771(4) 0.001(4) 0.655(3) 0.10(3) Uiso 1 1 d . . . H2 H 0.296(4) 0.218(4) 0.179(2) 0.10(2) Uiso 1 1 d . . . 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 C1 0.035(4) 0.047(4) 0.056(5) 0.003(3) 0.018(4) 0.007(3) C2 0.033(4) 0.046(4) 0.079(5) 0.002(4) 0.024(4) -0.003(3) O2 0.042(3) 0.052(3) 0.095(4) -0.006(2) 0.022(3) -0.002(2) C3 0.039(4) 0.051(4) 0.063(5) -0.003(3) 0.022(4) 0.007(3) C31 0.060(5) 0.043(4) 0.094(6) -0.012(4) 0.018(5) 0.014(3) C32 0.070(5) 0.108(5) 0.102(6) -0.043(4) 0.004(5) -0.001(4) C33 0.079(5) 0.095(5) 0.147(7) -0.055(4) 0.051(5) 0.003(4) C34 0.085(5) 0.057(5) 0.145(8) -0.012(5) 0.025(5) 0.018(3) C4 0.045(4) 0.060(4) 0.053(5) -0.001(4) 0.022(4) 0.011(3) C5 0.047(4) 0.060(4) 0.055(5) -0.002(4) 0.025(4) -0.004(3) C6 0.045(4) 0.053(4) 0.046(5) 0.007(3) 0.015(4) 0.002(3) C61 0.066(6) 0.074(5) 0.084(7) -0.007(5) 0.045(5) -0.019(4) C62 0.065(8) 0.108(8) 0.155(13) -0.010(7) 0.062(9) -0.032(6) C63 0.148(15) 0.26(2) 0.116(14) -0.093(12) 0.049(11) -0.142(14) C64 0.134(11) 0.100(9) 0.31(2) 0.119(11) 0.108(13) 0.015(7) C7 0.053(5) 0.048(4) 0.067(5) -0.008(3) 0.023(4) -0.011(3) C8 0.052(5) 0.053(4) 0.055(5) -0.013(4) 0.028(4) 0.000(3) C9 0.028(4) 0.056(5) 0.042(4) 0.002(3) 0.008(3) 0.007(3) C10 0.037(4) 0.040(4) 0.045(4) 0.000(3) 0.005(3) 0.001(3) C11 0.033(4) 0.036(4) 0.064(6) 0.001(4) 0.019(4) 0.002(3) N12 0.041(3) 0.057(3) 0.059(4) -0.004(3) 0.016(3) 0.002(3) C13 0.053(5) 0.049(4) 0.086(7) -0.007(4) 0.035(5) 0.005(3) C14 0.073(6) 0.068(5) 0.084(7) -0.002(4) 0.047(5) -0.001(4) C15 0.132(8) 0.095(6) 0.084(8) 0.011(5) 0.063(6) 0.004(5) C16 0.176(10) 0.130(8) 0.105(8) 0.043(6) 0.070(8) 0.038(6) C17 0.139(8) 0.101(6) 0.117(9) 0.052(6) 0.051(7) 0.053(5) C18 0.107(6) 0.077(5) 0.080(7) 0.038(5) 0.034(5) 0.034(4) C19 0.055(5) 0.048(4) 0.060(6) 0.010(4) 0.026(4) -0.005(3) C20 0.070(5) 0.057(5) 0.059(6) 0.011(4) 0.030(5) -0.002(4) C1A 0.038(4) 0.052(5) 0.055(5) -0.001(4) 0.016(4) 0.012(3) C2A 0.048(4) 0.049(5) 0.051(5) 0.004(4) 0.017(4) -0.011(3) O2A 0.074(3) 0.056(3) 0.059(4) 0.003(3) 0.025(3) 0.005(2) C3A 0.038(4) 0.054(4) 0.042(5) -0.005(4) 0.001(4) 0.004(3) C31A 0.042(4) 0.059(5) 0.059(5) -0.017(4) 0.006(4) 0.013(3) C32A 0.067(5) 0.102(5) 0.078(6) -0.014(4) 0.009(5) 0.022(4) C33A 0.106(6) 0.048(4) 0.114(7) -0.019(4) 0.019(5) 0.001(4) C34A 0.093(5) 0.103(5) 0.067(6) -0.009(4) 0.032(5) 0.037(4) C4A 0.051(4) 0.059(4) 0.045(5) -0.009(4) 0.024(4) 0.011(3) C5A 0.066(5) 0.061(5) 0.055(5) 0.004(4) 0.033(4) -0.002(4) C6A 0.054(5) 0.055(5) 0.052(5) -0.007(4) 0.016(4) -0.007(3) C61A 0.088(6) 0.060(5) 0.063(6) 0.018(4) 0.021(5) 0.014(4) C62A 0.206(8) 0.145(7) 0.104(7) 0.066(5) 0.100(7) 0.077(6) C63A 0.365(13) 0.094(6) 0.117(8) 0.019(6) -0.016(8) -0.126(7) C64A 0.130(7) 0.172(7) 0.135(8) 0.086(6) 0.054(6) 0.079(6) C7A 0.067(5) 0.062(5) 0.068(5) 0.007(4) 0.027(4) 0.024(3) C8A 0.065(5) 0.052(4) 0.062(5) 0.006(4) 0.030(4) 0.010(3) C9A 0.039(4) 0.042(4) 0.054(5) -0.004(4) 0.007(4) 0.007(3) C10A 0.043(4) 0.060(5) 0.040(5) -0.007(4) 0.021(4) -0.003(3) C11A 0.041(5) 0.044(4) 0.037(5) -0.004(3) 0.009(4) 0.009(3) N12A 0.043(4) 0.059(3) 0.051(4) -0.003(3) 0.023(3) -0.002(2) C13A 0.053(5) 0.055(4) 0.058(5) -0.006(3) 0.012(4) 0.007(3) C14A 0.054(5) 0.059(4) 0.066(6) 0.002(4) 0.033(5) 0.006(3) C15A 0.055(6) 0.085(5) 0.077(6) -0.003(4) 0.033(5) -0.005(4) C16A 0.061(6) 0.092(5) 0.099(7) -0.007(5) 0.031(6) -0.018(4) C17A 0.050(5) 0.106(5) 0.071(6) -0.022(4) 0.006(5) -0.018(4) C18A 0.044(5) 0.086(5) 0.059(6) -0.009(4) 0.011(4) -0.011(4) C19A 0.032(5) 0.057(4) 0.055(5) -0.011(4) 0.015(5) 0.002(3) C20A 0.033(5) 0.053(4) 0.063(6) 0.000(4) 0.019(5) 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 C1 C2 1.376(6) . ? C1 C9 1.416(6) . ? C1 C11 1.498(6) . ? C2 O2 1.380(5) . ? C2 C3 1.429(6) . ? O2 H2 0.96(5) . ? C3 C4 1.376(6) . ? C3 C31 1.547(6) . ? C31 C33 1.536(6) . ? C31 C32 1.542(6) . ? C31 C34 1.552(7) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C4 C10 1.428(6) . ? C4 H4 0.9300 . ? C5 C6 1.366(6) . ? C5 C10 1.416(6) . ? C5 H5 0.9300 . ? C6 C7 1.409(6) . ? C6 C61 1.530(7) . ? C61 C66 1.43(3) . ? C61 C65 1.46(3) . ? C61 C63 1.488(11) . ? C61 C62 1.503(9) . ? C61 C64 1.583(11) . ? C61 C67 1.74(2) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C7 C8 1.359(5) . ? C7 H7 0.9300 . ? C8 C9 1.426(6) . ? C8 H8 0.9300 . ? C9 C10 1.404(6) . ? C11 N12 1.320(5) . ? C11 C19 1.426(7) . ? N12 C13 1.370(6) . ? C13 C14 1.351(7) . ? C13 H13 0.9300 . ? C14 C20 1.394(7) . ? C14 H14 0.9300 . ? C15 C16 1.344(8) . ? C15 C20 1.408(8) . ? C15 H15 0.9300 . ? C16 C17 1.420(9) . ? C16 H16 0.9300 . ? C17 C18 1.366(8) . ? C17 H17 0.9300 . ? C18 C19 1.401(7) . ? C18 H18 0.9300 . ? C19 C20 1.434(7) . ? C1A C2A 1.382(6) . ? C1A C9A 1.426(6) . ? C1A C11A 1.499(6) . ? C2A O2A 1.367(6) . ? C2A C3A 1.444(6) . ? O2A H2A 0.96(6) . ? C3A C4A 1.367(6) . ? C3A C31A 1.538(6) . ? C31A C32A 1.528(6) . ? C31A C33A 1.536(6) . ? C31A C34A 1.540(6) . ? C32A H32D 0.9600 . ? C32A H32E 0.9600 . ? C32A H32F 0.9600 . ? C33A H33D 0.9600 . ? C33A H33E 0.9600 . ? C33A H33F 0.9600 . ? C34A H34D 0.9600 . ? C34A H34E 0.9600 . ? C34A H34F 0.9600 . ? C4A C10A 1.413(6) . ? C4A H4A 0.9300 . ? C5A C6A 1.382(6) . ? C5A C10A 1.427(6) . ? C5A H5A 0.9300 . ? C6A C7A 1.422(6) . ? C6A C61A 1.534(7) . ? C61A C63A 1.496(7) . ? C61A C64A 1.515(7) . ? C61A C62A 1.525(7) . ? C62A H62D 0.9600 . ? C62A H62E 0.9600 . ? C62A H62F 0.9600 . ? C63A H63D 0.9600 . ? C63A H63E 0.9600 . ? C63A H63F 0.9600 . ? C64A H64D 0.9600 . ? C64A H64E 0.9600 . ? C64A H64F 0.9600 . ? C7A C8A 1.369(6) . ? C7A H7A 0.9300 . ? C8A C9A 1.409(6) . ? C8A H8A 0.9300 . ? C9A C10A 1.414(7) . ? C11A N12A 1.330(6) . ? C11A C19A 1.418(6) . ? N12A C13A 1.374(6) . ? C13A C14A 1.361(6) . ? C13A H13A 0.9300 . ? C14A C20A 1.401(6) . ? C14A H14A 0.9300 . ? C15A C16A 1.349(7) . ? C15A C20A 1.422(6) . ? C15A H15A 0.9300 . ? C16A C17A 1.405(7) . ? C16A H16A 0.9300 . ? C17A C18A 1.370(6) . ? C17A H17A 0.9300 . ? C18A C19A 1.405(6) . ? C18A H18A 0.9300 . ? C19A C20A 1.409(6) . ? 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 C1 C9 120.2(5) . . ? C2 C1 C11 121.7(5) . . ? C9 C1 C11 117.8(5) . . ? C1 C2 O2 119.9(5) . . ? C1 C2 C3 122.8(5) . . ? O2 C2 C3 117.2(6) . . ? C2 O2 H2 117(3) . . ? C4 C3 C2 115.6(5) . . ? C4 C3 C31 122.0(5) . . ? C2 C3 C31 122.4(5) . . ? C33 C31 C32 108.1(6) . . ? C33 C31 C3 111.7(5) . . ? C32 C31 C3 110.3(4) . . ? C33 C31 C34 107.7(5) . . ? C32 C31 C34 110.7(5) . . ? C3 C31 C34 108.3(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C3 C4 C10 123.9(5) . . ? C3 C4 H4 118.1 . . ? C10 C4 H4 118.1 . . ? C6 C5 C10 122.6(5) . . ? C6 C5 H5 118.7 . . ? C10 C5 H5 118.7 . . ? C5 C6 C7 116.5(5) . . ? C5 C6 C61 124.5(6) . . ? C7 C6 C61 119.0(6) . . ? C66 C61 C65 114(2) . . ? C66 C61 C63 139.2(15) . . ? C65 C61 C63 45.8(14) . . ? C66 C61 C62 49.0(15) . . ? C65 C61 C62 129.6(14) . . ? C63 C61 C62 111.1(9) . . ? C66 C61 C6 109.0(14) . . ? C65 C61 C6 117.2(14) . . ? C63 C61 C6 111.8(7) . . ? C62 C61 C6 113.1(6) . . ? C66 C61 C64 57.5(15) . . ? C65 C61 C64 65.4(13) . . ? C63 C61 C64 110.4(9) . . ? C62 C61 C64 103.7(7) . . ? C6 C61 C64 106.4(7) . . ? C66 C61 C67 105.9(19) . . ? C65 C61 C67 106.6(18) . . ? C63 C61 C67 63.6(11) . . ? C62 C61 C67 57.2(10) . . ? C6 C61 C67 103.3(9) . . ? C64 C61 C67 149.5(9) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C61 C65 H65A 109.5 . . ? C61 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C61 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C61 C66 H66A 109.5 . . ? C61 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C61 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C61 C67 H67A 109.5 . . ? C61 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C61 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C8 C7 C6 123.0(5) . . ? C8 C7 H7 118.5 . . ? C6 C7 H7 118.5 . . ? C7 C8 C9 120.8(5) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C1 119.1(5) . . ? C10 C9 C8 116.9(5) . . ? C1 C9 C8 124.1(5) . . ? C9 C10 C5 120.1(5) . . ? C9 C10 C4 118.4(5) . . ? C5 C10 C4 121.4(5) . . ? N12 C11 C19 122.5(5) . . ? N12 C11 C1 117.7(6) . . ? C19 C11 C1 119.7(5) . . ? C11 N12 C13 118.6(5) . . ? C14 C13 N12 123.4(6) . . ? C14 C13 H13 118.3 . . ? N12 C13 H13 118.3 . . ? C13 C14 C20 119.9(6) . . ? C13 C14 H14 120.1 . . ? C20 C14 H14 120.1 . . ? C16 C15 C20 121.3(7) . . ? C16 C15 H15 119.3 . . ? C20 C15 H15 119.3 . . ? C15 C16 C17 120.6(8) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C18 C17 C16 119.9(7) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.6(7) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C11 123.2(6) . . ? C18 C19 C20 119.4(6) . . ? C11 C19 C20 117.4(6) . . ? C14 C20 C15 123.7(7) . . ? C14 C20 C19 118.1(6) . . ? C15 C20 C19 118.2(6) . . ? C2A C1A C9A 119.6(6) . . ? C2A C1A C11A 121.0(6) . . ? C9A C1A C11A 119.2(5) . . ? O2A C2A C1A 120.3(6) . . ? O2A C2A C3A 117.1(6) . . ? C1A C2A C3A 122.5(6) . . ? C2A O2A H2A 122(3) . . ? C4A C3A C2A 116.1(5) . . ? C4A C3A C31A 121.9(6) . . ? C2A C3A C31A 122.0(6) . . ? C32A C31A C33A 109.6(5) . . ? C32A C31A C3A 109.4(5) . . ? C33A C31A C3A 111.3(5) . . ? C32A C31A C34A 107.4(5) . . ? C33A C31A C34A 107.5(5) . . ? C3A C31A C34A 111.6(5) . . ? C31A C32A H32D 109.5 . . ? C31A C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C31A C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C31A C33A H33D 109.5 . . ? C31A C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C31A C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? C31A C34A H34D 109.5 . . ? C31A C34A H34E 109.5 . . ? H34D C34A H34E 109.5 . . ? C31A C34A H34F 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? C3A C4A C10A 123.9(5) . . ? C3A C4A H4A 118.0 . . ? C10A C4A H4A 118.0 . . ? C6A C5A C10A 123.5(5) . . ? C6A C5A H5A 118.3 . . ? C10A C5A H5A 118.3 . . ? C5A C6A C7A 115.8(6) . . ? C5A C6A C61A 123.2(6) . . ? C7A C6A C61A 120.9(6) . . ? C63A C61A C64A 110.5(6) . . ? C63A C61A C62A 108.6(6) . . ? C64A C61A C62A 107.1(6) . . ? C63A C61A C6A 108.0(6) . . ? C64A C61A C6A 110.5(5) . . ? C62A C61A C6A 112.2(5) . . ? C61A C62A H62D 109.5 . . ? C61A C62A H62E 109.5 . . ? H62D C62A H62E 109.5 . . ? C61A C62A H62F 109.5 . . ? H62D C62A H62F 109.5 . . ? H62E C62A H62F 109.5 . . ? C61A C63A H63D 109.5 . . ? C61A C63A H63E 109.5 . . ? H63D C63A H63E 109.5 . . ? C61A C63A H63F 109.5 . . ? H63D C63A H63F 109.5 . . ? H63E C63A H63F 109.5 . . ? C61A C64A H64D 109.5 . . ? C61A C64A H64E 109.5 . . ? H64D C64A H64E 109.5 . . ? C61A C64A H64F 109.5 . . ? H64D C64A H64F 109.5 . . ? H64E C64A H64F 109.5 . . ? C8A C7A C6A 122.5(5) . . ? C8A C7A H7A 118.7 . . ? C6A C7A H7A 118.7 . . ? C7A C8A C9A 121.4(6) . . ? C7A C8A H8A 119.3 . . ? C9A C8A H8A 119.3 . . ? C8A C9A C10A 118.2(6) . . ? C8A C9A C1A 122.9(6) . . ? C10A C9A C1A 118.9(5) . . ? C4A C10A C9A 119.0(6) . . ? C4A C10A C5A 122.4(6) . . ? C9A C10A C5A 118.6(5) . . ? N12A C11A C19A 123.7(5) . . ? N12A C11A C1A 115.3(5) . . ? C19A C11A C1A 120.9(6) . . ? C11A N12A C13A 117.0(5) . . ? C14A C13A N12A 123.9(5) . . ? C14A C13A H13A 118.0 . . ? N12A C13A H13A 118.0 . . ? C13A C14A C20A 118.9(6) . . ? C13A C14A H14A 120.5 . . ? C20A C14A H14A 120.5 . . ? C16A C15A C20A 120.1(6) . . ? C16A C15A H15A 120.0 . . ? C20A C15A H15A 120.0 . . ? C15A C16A C17A 122.1(6) . . ? C15A C16A H16A 119.0 . . ? C17A C16A H16A 119.0 . . ? C18A C17A C16A 119.0(6) . . ? C18A C17A H17A 120.5 . . ? C16A C17A H17A 120.5 . . ? C17A C18A C19A 120.5(6) . . ? C17A C18A H18A 119.8 . . ? C19A C18A H18A 119.8 . . ? C18A C19A C20A 120.1(6) . . ? C18A C19A C11A 122.7(6) . . ? C20A C19A C11A 117.2(6) . . ? C14A C20A C19A 119.0(6) . . ? C14A C20A C15A 122.7(7) . . ? C19A C20A C15A 118.2(6) . . ? 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 C9 C1 C2 O2 -179.9(5) . . . . ? C11 C1 C2 O2 6.2(8) . . . . ? C9 C1 C2 C3 2.3(8) . . . . ? C11 C1 C2 C3 -171.5(5) . . . . ? C1 C2 C3 C4 -1.5(8) . . . . ? O2 C2 C3 C4 -179.3(5) . . . . ? C1 C2 C3 C31 178.5(5) . . . . ? O2 C2 C3 C31 0.7(8) . . . . ? C4 C3 C31 C33 0.5(8) . . . . ? C2 C3 C31 C33 -179.5(5) . . . . ? C4 C3 C31 C32 -119.8(6) . . . . ? C2 C3 C31 C32 60.2(7) . . . . ? C4 C3 C31 C34 119.0(6) . . . . ? C2 C3 C31 C34 -61.1(7) . . . . ? C2 C3 C4 C10 0.5(8) . . . . ? C31 C3 C4 C10 -179.6(5) . . . . ? C10 C5 C6 C7 0.0(8) . . . . ? C10 C5 C6 C61 -179.2(6) . . . . ? C5 C6 C61 C66 48(2) . . . . ? C7 C6 C61 C66 -132(2) . . . . ? C5 C6 C61 C65 178.5(19) . . . . ? C7 C6 C61 C65 -1(2) . . . . ? C5 C6 C61 C63 -131.3(10) . . . . ? C7 C6 C61 C63 49.6(11) . . . . ? C5 C6 C61 C62 -5.0(11) . . . . ? C7 C6 C61 C62 175.8(7) . . . . ? C5 C6 C61 C64 108.2(9) . . . . ? C7 C6 C61 C64 -71.0(10) . . . . ? C5 C6 C61 C67 -64.7(14) . . . . ? C7 C6 C61 C67 116.2(12) . . . . ? C5 C6 C7 C8 0.5(8) . . . . ? C61 C6 C7 C8 179.7(6) . . . . ? C6 C7 C8 C9 -1.1(8) . . . . ? C2 C1 C9 C10 -2.0(8) . . . . ? C11 C1 C9 C10 172.0(5) . . . . ? C2 C1 C9 C8 178.4(5) . . . . ? C11 C1 C9 C8 -7.6(8) . . . . ? C7 C8 C9 C10 1.2(7) . . . . ? C7 C8 C9 C1 -179.1(5) . . . . ? C1 C9 C10 C5 179.6(5) . . . . ? C8 C9 C10 C5 -0.8(7) . . . . ? C1 C9 C10 C4 1.0(7) . . . . ? C8 C9 C10 C4 -179.4(5) . . . . ? C6 C5 C10 C9 0.2(8) . . . . ? C6 C5 C10 C4 178.7(5) . . . . ? C3 C4 C10 C9 -0.3(8) . . . . ? C3 C4 C10 C5 -178.8(5) . . . . ? C2 C1 C11 N12 -105.5(6) . . . . ? C9 C1 C11 N12 80.5(6) . . . . ? C2 C1 C11 C19 78.1(7) . . . . ? C9 C1 C11 C19 -95.9(6) . . . . ? C19 C11 N12 C13 2.2(8) . . . . ? C1 C11 N12 C13 -174.1(4) . . . . ? C11 N12 C13 C14 -0.6(8) . . . . ? N12 C13 C14 C20 -0.2(9) . . . . ? C20 C15 C16 C17 0.9(13) . . . . ? C15 C16 C17 C18 -1.1(13) . . . . ? C16 C17 C18 C19 0.4(12) . . . . ? C17 C18 C19 C11 178.6(6) . . . . ? C17 C18 C19 C20 0.4(10) . . . . ? N12 C11 C19 C18 178.9(5) . . . . ? C1 C11 C19 C18 -4.9(8) . . . . ? N12 C11 C19 C20 -2.9(8) . . . . ? C1 C11 C19 C20 173.3(5) . . . . ? C13 C14 C20 C15 -179.6(6) . . . . ? C13 C14 C20 C19 -0.6(9) . . . . ? C16 C15 C20 C14 179.0(7) . . . . ? C16 C15 C20 C19 0.0(11) . . . . ? C18 C19 C20 C14 -179.7(6) . . . . ? C11 C19 C20 C14 2.0(8) . . . . ? C18 C19 C20 C15 -0.7(9) . . . . ? C11 C19 C20 C15 -178.9(6) . . . . ? C9A C1A C2A O2A -178.0(5) . . . . ? C11A C1A C2A O2A -2.7(8) . . . . ? C9A C1A C2A C3A -1.2(8) . . . . ? C11A C1A C2A C3A 174.1(5) . . . . ? O2A C2A C3A C4A 177.2(5) . . . . ? C1A C2A C3A C4A 0.3(8) . . . . ? O2A C2A C3A C31A -3.4(8) . . . . ? C1A C2A C3A C31A 179.7(5) . . . . ? C4A C3A C31A C32A 116.3(6) . . . . ? C2A C3A C31A C32A -63.0(6) . . . . ? C4A C3A C31A C33A -122.4(6) . . . . ? C2A C3A C31A C33A 58.2(7) . . . . ? C4A C3A C31A C34A -2.3(7) . . . . ? C2A C3A C31A C34A 178.3(5) . . . . ? C2A C3A C4A C10A 0.5(8) . . . . ? C31A C3A C4A C10A -178.9(5) . . . . ? C10A C5A C6A C7A 0.6(8) . . . . ? C10A C5A C6A C61A 178.0(5) . . . . ? C5A C6A C61A C63A -109.6(7) . . . . ? C7A C6A C61A C63A 67.7(8) . . . . ? C5A C6A C61A C64A 129.5(6) . . . . ? C7A C6A C61A C64A -53.2(8) . . . . ? C5A C6A C61A C62A 10.0(8) . . . . ? C7A C6A C61A C62A -172.7(6) . . . . ? C5A C6A C7A C8A -0.7(9) . . . . ? C61A C6A C7A C8A -178.2(5) . . . . ? C6A C7A C8A C9A 0.5(9) . . . . ? C7A C8A C9A C10A -0.2(8) . . . . ? C7A C8A C9A C1A 178.5(5) . . . . ? C2A C1A C9A C8A -177.3(5) . . . . ? C11A C1A C9A C8A 7.3(8) . . . . ? C2A C1A C9A C10A 1.3(8) . . . . ? C11A C1A C9A C10A -174.1(5) . . . . ? C3A C4A C10A C9A -0.4(8) . . . . ? C3A C4A C10A C5A 177.6(5) . . . . ? C8A C9A C10A C4A 178.2(5) . . . . ? C1A C9A C10A C4A -0.5(8) . . . . ? C8A C9A C10A C5A 0.1(7) . . . . ? C1A C9A C10A C5A -178.6(5) . . . . ? C6A C5A C10A C4A -178.3(5) . . . . ? C6A C5A C10A C9A -0.3(8) . . . . ? C2A C1A C11A N12A 92.8(6) . . . . ? C9A C1A C11A N12A -91.9(6) . . . . ? C2A C1A C11A C19A -90.7(7) . . . . ? C9A C1A C11A C19A 84.6(7) . . . . ? C19A C11A N12A C13A 4.1(8) . . . . ? C1A C11A N12A C13A -179.5(4) . . . . ? C11A N12A C13A C14A -0.2(8) . . . . ? N12A C13A C14A C20A -2.4(8) . . . . ? C20A C15A C16A C17A 0.5(10) . . . . ? C15A C16A C17A C18A 0.8(10) . . . . ? C16A C17A C18A C19A -1.0(9) . . . . ? C17A C18A C19A C20A -0.1(8) . . . . ? C17A C18A C19A C11A -179.4(5) . . . . ? N12A C11A C19A C18A 174.2(5) . . . . ? C1A C11A C19A C18A -2.0(8) . . . . ? N12A C11A C19A C20A -5.1(8) . . . . ? C1A C11A C19A C20A 178.7(5) . . . . ? C13A C14A C20A C19A 1.3(8) . . . . ? C13A C14A C20A C15A -177.1(5) . . . . ? C18A C19A C20A C14A -177.1(5) . . . . ? C11A C19A C20A C14A 2.2(7) . . . . ? C18A C19A C20A C15A 1.4(8) . . . . ? C11A C19A C20A C15A -179.3(5) . . . . ? C16A C15A C20A C14A 176.9(6) . . . . ? C16A C15A C20A C19A -1.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.168 _refine_diff_density_min -0.130 _refine_diff_density_rms 0.027 #===END data_L(Bu)-H _database_code_depnum_ccdc_archive 'CCDC 728912' _chemical_formula_structural L(Bu)-H _chemical_formula_moiety 'C31 H37 N O' _chemical_formula_sum 'C31 H37 N O' _chemical_formula_weight 439.62 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.055(4) _cell_length_b 12.368(2) _cell_length_c 17.991(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.732(13) _cell_angle_gamma 90.00 _cell_volume 5103.6(16) _cell_formula_units_Z 8 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 5836 _cell_measurement_theta_min 3.71 _cell_measurement_theta_max 27.50 _exptl_crystal_description rod _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.997 _exptl_absorpt_process_details '(ABSPACK; Oxford Diffraction, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32009 _diffrn_reflns_av_R_equivalents 0.1943 _diffrn_reflns_av_sigmaI/netI 0.2265 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5836 _reflns_number_gt 2253 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004) ; _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^ > 2\s(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^)+(0.0287P)^2^] 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_number_reflns 5836 _refine_ls_number_parameters 310 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2357 _refine_ls_R_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.000 _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 0.29495(9) 0.37599(17) 0.17113(14) 0.0290(6) Uani 1 1 d D . . N1 N 0.37501(10) 0.51089(18) 0.15975(14) 0.0189(6) Uani 1 1 d . . . C1 C 0.39496(13) 0.3801(2) 0.26451(17) 0.0184(7) Uani 1 1 d . . . C2 C 0.34115(13) 0.3301(2) 0.23343(18) 0.0217(8) Uani 1 1 d . . . C3 C 0.33016(13) 0.2294(2) 0.26297(18) 0.0212(8) Uani 1 1 d . . . C4 C 0.37827(13) 0.1761(2) 0.31562(18) 0.0233(8) Uani 1 1 d . . . H4 H 0.3727 0.1093 0.3376 0.028 Uiso 1 1 calc R . . C5 C 0.43627(13) 0.2148(2) 0.33951(18) 0.0224(8) Uani 1 1 d . . . C6 C 0.48486(13) 0.1487(2) 0.38192(18) 0.0258(8) Uani 1 1 d . . . H6 H 0.4784 0.0786 0.3981 0.031 Uiso 1 1 calc R . . C7 C 0.54114(13) 0.1813(2) 0.40082(18) 0.0228(8) Uani 1 1 d . . . C8 C 0.54855(13) 0.2872(2) 0.37909(17) 0.0215(8) Uani 1 1 d . . . H8 H 0.5870 0.3130 0.3923 0.026 Uiso 1 1 calc R . . C9 C 0.50288(13) 0.3548(2) 0.33973(17) 0.0210(7) Uani 1 1 d . . . H9 H 0.5103 0.4265 0.3275 0.025 Uiso 1 1 calc R . . C10 C 0.44484(13) 0.3201(2) 0.31680(17) 0.0198(7) Uani 1 1 d . . . C11 C 0.40023(12) 0.4928(2) 0.23897(18) 0.0194(7) Uani 1 1 d . . . C12 C 0.37821(12) 0.6115(2) 0.12919(19) 0.0203(7) Uani 1 1 d . . . C13 C 0.40614(12) 0.6938(2) 0.17952(18) 0.0228(8) Uani 1 1 d . . . H13 H 0.4095 0.7618 0.1572 0.027 Uiso 1 1 calc R . . C14 C 0.43019(12) 0.6802(2) 0.26429(18) 0.0219(8) Uani 1 1 d . . . C15 C 0.45448(13) 0.7673(3) 0.3181(2) 0.0293(8) Uani 1 1 d . . . H15 H 0.4578 0.8365 0.2974 0.035 Uiso 1 1 calc R . . C16 C 0.47304(13) 0.7525(3) 0.3993(2) 0.0323(9) Uani 1 1 d . . . H16 H 0.4896 0.8112 0.4354 0.039 Uiso 1 1 calc R . . C17 C 0.46798(13) 0.6512(3) 0.4303(2) 0.0319(9) Uani 1 1 d . . . H17 H 0.4804 0.6423 0.4873 0.038 Uiso 1 1 calc R . . C18 C 0.44562(12) 0.5652(3) 0.38030(19) 0.0270(8) Uani 1 1 d . . . H18 H 0.4429 0.4968 0.4025 0.032 Uiso 1 1 calc R . . C19 C 0.42642(12) 0.5775(2) 0.29554(19) 0.0190(7) Uani 1 1 d . . . C30 C 0.26858(13) 0.1834(3) 0.2359(2) 0.0308(9) Uani 1 1 d . . . C31 C 0.22746(13) 0.2663(3) 0.2485(2) 0.0462(10) Uani 1 1 d . . . H31A H 0.2436 0.2899 0.3053 0.069 Uiso 1 1 calc R . . H31B H 0.1892 0.2331 0.2350 0.069 Uiso 1 1 calc R . . H31C H 0.2234 0.3288 0.2131 0.069 Uiso 1 1 calc R . . C32 C 0.24551(14) 0.1506(3) 0.1464(2) 0.0464(11) Uani 1 1 d . . . H32A H 0.2481 0.2124 0.1139 0.070 Uiso 1 1 calc R . . H32B H 0.2048 0.1276 0.1280 0.070 Uiso 1 1 calc R . . H32C H 0.2690 0.0907 0.1400 0.070 Uiso 1 1 calc R . . C33 C 0.26750(14) 0.0827(3) 0.2846(2) 0.0544(12) Uani 1 1 d . . . H33A H 0.2906 0.0253 0.2743 0.082 Uiso 1 1 calc R . . H33B H 0.2272 0.0580 0.2681 0.082 Uiso 1 1 calc R . . H33C H 0.2840 0.1002 0.3427 0.082 Uiso 1 1 calc R . . C70 C 0.59310(14) 0.1052(3) 0.4377(2) 0.0298(9) Uani 1 1 d . . . C71 C 0.64889(17) 0.1644(3) 0.4848(3) 0.120(2) Uani 1 1 d . . . H71A H 0.6599 0.2075 0.4474 0.180 Uiso 1 1 calc R . . H71B H 0.6798 0.1122 0.5131 0.180 Uiso 1 1 calc R . . H71C H 0.6434 0.2123 0.5245 0.180 Uiso 1 1 calc R . . C72 C 0.58473(16) 0.0234(3) 0.4950(2) 0.0671(14) Uani 1 1 d . . . H72A H 0.6190 -0.0238 0.5170 0.101 Uiso 1 1 calc R . . H72B H 0.5500 -0.0203 0.4654 0.101 Uiso 1 1 calc R . . H72C H 0.5798 0.0614 0.5396 0.101 Uiso 1 1 calc R . . C73 C 0.59997(19) 0.0422(3) 0.3698(2) 0.0869(17) Uani 1 1 d . . . H73A H 0.6064 0.0926 0.3322 0.130 Uiso 1 1 calc R . . H73B H 0.5645 0.0001 0.3405 0.130 Uiso 1 1 calc R . . H73C H 0.6334 -0.0067 0.3927 0.130 Uiso 1 1 calc R . . C120 C 0.34748(13) 0.6204(2) 0.03745(18) 0.0233(8) Uani 1 1 d . . . C121 C 0.28269(12) 0.5958(3) 0.01213(19) 0.0373(9) Uani 1 1 d . . . H12A H 0.2780 0.5207 0.0257 0.056 Uiso 1 1 calc R . . H12B H 0.2619 0.6067 -0.0465 0.056 Uiso 1 1 calc R . . H12C H 0.2666 0.6444 0.0410 0.056 Uiso 1 1 calc R . . C122 C 0.37398(13) 0.5385(2) -0.00174(18) 0.0336(9) Uani 1 1 d . . . H12D H 0.3673 0.4651 0.0132 0.050 Uiso 1 1 calc R . . H12E H 0.4160 0.5515 0.0174 0.050 Uiso 1 1 calc R . . H12F H 0.3556 0.5464 -0.0609 0.050 Uiso 1 1 calc R . . C123 C 0.35419(13) 0.7331(2) 0.00803(19) 0.0348(9) Uani 1 1 d . . . H12G H 0.3341 0.7362 -0.0513 0.052 Uiso 1 1 calc R . . H12H H 0.3957 0.7491 0.0241 0.052 Uiso 1 1 calc R . . H12I H 0.3371 0.7866 0.0323 0.052 Uiso 1 1 calc R . . H1 H 0.3110(12) 0.424(2) 0.1545(18) 0.042 Uiso 1 1 d D . . 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 0.0246(13) 0.0274(14) 0.0345(15) 0.0039(11) 0.0113(12) -0.0037(11) N1 0.0208(15) 0.0175(14) 0.0200(15) 0.0014(12) 0.0097(13) 0.0018(12) C1 0.0254(19) 0.0202(18) 0.0133(18) -0.0029(14) 0.0116(16) -0.0048(16) C2 0.0213(19) 0.0223(19) 0.0210(19) -0.0003(15) 0.0081(16) 0.0045(15) C3 0.0260(19) 0.0171(18) 0.0215(19) -0.0032(15) 0.0106(17) -0.0044(15) C4 0.033(2) 0.0184(18) 0.0225(19) 0.0008(15) 0.0154(17) -0.0096(16) C5 0.0234(19) 0.026(2) 0.0173(18) 0.0011(15) 0.0075(16) -0.0009(16) C6 0.036(2) 0.0175(18) 0.0225(19) 0.0037(15) 0.0109(17) -0.0027(16) C7 0.029(2) 0.0208(19) 0.0199(18) -0.0005(15) 0.0106(17) -0.0017(16) C8 0.0222(19) 0.026(2) 0.0182(18) -0.0043(15) 0.0099(16) -0.0047(16) C9 0.0268(19) 0.0200(18) 0.0186(18) -0.0011(15) 0.0118(16) -0.0047(16) C10 0.0262(19) 0.0222(19) 0.0130(17) -0.0022(14) 0.0099(16) -0.0034(15) C11 0.0149(17) 0.0247(19) 0.0206(19) -0.0008(15) 0.0094(15) 0.0019(15) C12 0.0161(17) 0.0249(19) 0.0215(19) -0.0018(15) 0.0091(16) 0.0005(15) C13 0.0216(19) 0.0212(19) 0.027(2) 0.0048(15) 0.0108(17) 0.0001(15) C14 0.0189(18) 0.0256(19) 0.025(2) -0.0032(16) 0.0126(16) -0.0017(15) C15 0.031(2) 0.026(2) 0.032(2) -0.0051(17) 0.0147(18) -0.0041(17) C16 0.037(2) 0.030(2) 0.030(2) -0.0135(16) 0.0138(19) -0.0022(17) C17 0.037(2) 0.038(2) 0.022(2) -0.0047(17) 0.0126(18) -0.0001(18) C18 0.030(2) 0.029(2) 0.027(2) -0.0001(16) 0.0162(18) -0.0014(16) C19 0.0189(18) 0.0222(19) 0.0186(18) -0.0025(14) 0.0103(15) -0.0016(14) C30 0.025(2) 0.027(2) 0.037(2) 0.0018(17) 0.0093(18) -0.0089(17) C31 0.034(2) 0.047(2) 0.065(3) -0.003(2) 0.028(2) -0.0070(19) C32 0.035(2) 0.042(2) 0.050(3) -0.0055(19) 0.006(2) -0.0073(18) C33 0.039(2) 0.049(3) 0.071(3) 0.012(2) 0.019(2) -0.0194(19) C70 0.029(2) 0.025(2) 0.032(2) 0.0052(16) 0.0093(18) 0.0011(16) C71 0.037(3) 0.047(3) 0.196(6) 0.015(3) -0.035(3) 0.006(2) C72 0.076(3) 0.070(3) 0.073(3) 0.041(2) 0.048(3) 0.040(2) C73 0.107(4) 0.114(4) 0.059(3) 0.024(3) 0.054(3) 0.074(3) C120 0.0239(19) 0.0271(19) 0.0186(19) 0.0014(15) 0.0080(16) -0.0016(16) C121 0.032(2) 0.049(2) 0.026(2) 0.0049(17) 0.0066(18) 0.0004(18) C122 0.038(2) 0.042(2) 0.022(2) 0.0001(17) 0.0126(18) 0.0038(17) C123 0.043(2) 0.035(2) 0.024(2) 0.0103(17) 0.0108(18) 0.0001(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.369(3) . ? O1 H1 0.839(17) . ? N1 C11 1.325(3) . ? N1 C12 1.376(3) . ? C1 C2 1.380(4) . ? C1 C10 1.432(4) . ? C1 C11 1.490(4) . ? C2 C3 1.424(4) . ? C3 C4 1.366(4) . ? C3 C30 1.529(4) . ? C4 C5 1.422(4) . ? C4 H4 0.9500 . ? C5 C10 1.407(4) . ? C5 C6 1.409(4) . ? C6 C7 1.371(4) . ? C6 H6 0.9500 . ? C7 C8 1.400(4) . ? C7 C70 1.525(4) . ? C8 C9 1.363(4) . ? C8 H8 0.9500 . ? C9 C10 1.409(4) . ? C9 H9 0.9500 . ? C11 C19 1.424(4) . ? C12 C13 1.355(4) . ? C12 C120 1.519(4) . ? C13 C14 1.406(4) . ? C13 H13 0.9500 . ? C14 C19 1.407(4) . ? C14 C15 1.412(4) . ? C15 C16 1.356(4) . ? C15 H15 0.9500 . ? C16 C17 1.397(4) . ? C16 H16 0.9500 . ? C17 C18 1.359(4) . ? C17 H17 0.9500 . ? C18 C19 1.410(4) . ? C18 H18 0.9500 . ? C30 C33 1.529(4) . ? C30 C32 1.531(4) . ? C30 C31 1.533(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C70 C71 1.502(5) . ? C70 C73 1.516(4) . ? C70 C72 1.518(4) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C120 C123 1.525(4) . ? C120 C121 1.529(4) . ? C120 C122 1.530(4) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C122 H12D 0.9800 . ? C122 H12E 0.9800 . ? C122 H12F 0.9800 . ? C123 H12G 0.9800 . ? C123 H12H 0.9800 . ? C123 H12I 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 H1 103(2) . . ? C11 N1 C12 120.2(3) . . ? C2 C1 C10 119.1(3) . . ? C2 C1 C11 119.2(3) . . ? C10 C1 C11 121.7(3) . . ? O1 C2 C1 120.8(3) . . ? O1 C2 C3 116.2(3) . . ? C1 C2 C3 123.0(3) . . ? C4 C3 C2 115.6(3) . . ? C4 C3 C30 122.5(3) . . ? C2 C3 C30 121.9(3) . . ? C3 C4 C5 123.8(3) . . ? C3 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C10 C5 C6 119.6(3) . . ? C10 C5 C4 118.7(3) . . ? C6 C5 C4 121.6(3) . . ? C7 C6 C5 122.8(3) . . ? C7 C6 H6 118.6 . . ? C5 C6 H6 118.6 . . ? C6 C7 C8 116.4(3) . . ? C6 C7 C70 122.6(3) . . ? C8 C7 C70 120.9(3) . . ? C9 C8 C7 122.7(3) . . ? C9 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? C8 C9 C10 121.1(3) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C5 C10 C9 117.2(3) . . ? C5 C10 C1 118.4(3) . . ? C9 C10 C1 124.0(3) . . ? N1 C11 C19 121.9(3) . . ? N1 C11 C1 115.2(3) . . ? C19 C11 C1 122.7(3) . . ? C13 C12 N1 120.7(3) . . ? C13 C12 C120 124.9(3) . . ? N1 C12 C120 114.4(3) . . ? C12 C13 C14 121.0(3) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C19 118.2(3) . . ? C13 C14 C15 122.0(3) . . ? C19 C14 C15 119.6(3) . . ? C16 C15 C14 120.1(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.3(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 121.1(3) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 120.1(3) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C14 C19 C18 118.7(3) . . ? C14 C19 C11 117.7(3) . . ? C18 C19 C11 123.5(3) . . ? C3 C30 C33 111.7(3) . . ? C3 C30 C32 109.8(3) . . ? C33 C30 C32 107.5(3) . . ? C3 C30 C31 110.9(3) . . ? C33 C30 C31 107.0(3) . . ? C32 C30 C31 109.9(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C71 C70 C73 108.8(4) . . ? C71 C70 C72 107.1(3) . . ? C73 C70 C72 107.3(3) . . ? C71 C70 C7 112.4(3) . . ? C73 C70 C7 108.7(3) . . ? C72 C70 C7 112.3(3) . . ? 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 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C12 C120 C123 111.4(3) . . ? C12 C120 C121 108.8(3) . . ? C123 C120 C121 109.3(3) . . ? C12 C120 C122 109.2(2) . . ? C123 C120 C122 108.5(3) . . ? C121 C120 C122 109.7(2) . . ? C120 C121 H12A 109.5 . . ? C120 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C120 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C120 C122 H12D 109.5 . . ? C120 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? C120 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? C120 C123 H12G 109.5 . . ? C120 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? C120 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 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 C10 C1 C2 O1 -166.7(3) . . . . ? C11 C1 C2 O1 9.8(4) . . . . ? C10 C1 C2 C3 13.0(4) . . . . ? C11 C1 C2 C3 -170.5(3) . . . . ? O1 C2 C3 C4 169.9(3) . . . . ? C1 C2 C3 C4 -9.9(4) . . . . ? O1 C2 C3 C30 -9.0(4) . . . . ? C1 C2 C3 C30 171.3(3) . . . . ? C2 C3 C4 C5 -1.3(4) . . . . ? C30 C3 C4 C5 177.5(3) . . . . ? C3 C4 C5 C10 8.8(4) . . . . ? C3 C4 C5 C6 -168.3(3) . . . . ? C10 C5 C6 C7 -1.7(5) . . . . ? C4 C5 C6 C7 175.4(3) . . . . ? C5 C6 C7 C8 3.0(5) . . . . ? C5 C6 C7 C70 -172.6(3) . . . . ? C6 C7 C8 C9 -1.4(5) . . . . ? C70 C7 C8 C9 174.3(3) . . . . ? C7 C8 C9 C10 -1.6(5) . . . . ? C6 C5 C10 C9 -1.3(4) . . . . ? C4 C5 C10 C9 -178.4(3) . . . . ? C6 C5 C10 C1 171.7(3) . . . . ? C4 C5 C10 C1 -5.5(4) . . . . ? C8 C9 C10 C5 2.8(4) . . . . ? C8 C9 C10 C1 -169.7(3) . . . . ? C2 C1 C10 C5 -4.8(4) . . . . ? C11 C1 C10 C5 178.8(3) . . . . ? C2 C1 C10 C9 167.6(3) . . . . ? C11 C1 C10 C9 -8.7(4) . . . . ? C12 N1 C11 C19 6.0(4) . . . . ? C12 N1 C11 C1 -178.6(2) . . . . ? C2 C1 C11 N1 -47.6(4) . . . . ? C10 C1 C11 N1 128.8(3) . . . . ? C2 C1 C11 C19 127.8(3) . . . . ? C10 C1 C11 C19 -55.9(4) . . . . ? C11 N1 C12 C13 -1.2(4) . . . . ? C11 N1 C12 C120 179.9(3) . . . . ? N1 C12 C13 C14 -3.0(4) . . . . ? C120 C12 C13 C14 175.8(3) . . . . ? C12 C13 C14 C19 2.3(4) . . . . ? C12 C13 C14 C15 -173.7(3) . . . . ? C13 C14 C15 C16 174.8(3) . . . . ? C19 C14 C15 C16 -1.2(5) . . . . ? C14 C15 C16 C17 -0.4(5) . . . . ? C15 C16 C17 C18 1.4(5) . . . . ? C16 C17 C18 C19 -0.7(5) . . . . ? C13 C14 C19 C18 -174.4(3) . . . . ? C15 C14 C19 C18 1.8(4) . . . . ? C13 C14 C19 C11 2.2(4) . . . . ? C15 C14 C19 C11 178.4(3) . . . . ? C17 C18 C19 C14 -0.9(4) . . . . ? C17 C18 C19 C11 -177.2(3) . . . . ? N1 C11 C19 C14 -6.5(4) . . . . ? C1 C11 C19 C14 178.5(3) . . . . ? N1 C11 C19 C18 169.9(3) . . . . ? C1 C11 C19 C18 -5.1(4) . . . . ? C4 C3 C30 C33 8.9(4) . . . . ? C2 C3 C30 C33 -172.3(3) . . . . ? C4 C3 C30 C32 -110.2(3) . . . . ? C2 C3 C30 C32 68.5(4) . . . . ? C4 C3 C30 C31 128.2(3) . . . . ? C2 C3 C30 C31 -53.1(4) . . . . ? C6 C7 C70 C71 -155.5(4) . . . . ? C8 C7 C70 C71 29.2(5) . . . . ? C6 C7 C70 C73 83.9(4) . . . . ? C8 C7 C70 C73 -91.4(4) . . . . ? C6 C7 C70 C72 -34.6(4) . . . . ? C8 C7 C70 C72 150.0(3) . . . . ? C13 C12 C120 C123 2.5(4) . . . . ? N1 C12 C120 C123 -178.6(2) . . . . ? C13 C12 C120 C121 -118.0(3) . . . . ? N1 C12 C120 C121 60.9(3) . . . . ? C13 C12 C120 C122 122.3(3) . . . . ? N1 C12 C120 C122 -58.8(3) . . . . ? 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 O1 H1 N1 0.839(17) 1.90(2) 2.679(3) 154(3) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.198 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.042 #===END data_[PdBr(PPh3)(mu-isoquinolinyl)]2 _database_code_depnum_ccdc_archive 'CCDC 728913' _chemical_formula_structural '[PdBr(PPh3)(mu-isoquinolinyl)]2.CH2Cl2.n(H2O)' _chemical_formula_moiety 'C54 H42 Br2 N2 P2 Pd2, C H2 Cl2, n(H2 O?)' _chemical_formula_sum 'C56 H47 Br2 Cl2 N2 O1.50 P2 Pd2' _chemical_formula_weight 1277.42 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3491(8) _cell_length_b 13.3734(10) _cell_length_c 18.5704(8) _cell_angle_alpha 109.028(6) _cell_angle_beta 99.561(5) _cell_angle_gamma 99.732(6) _cell_volume 2551.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1270 _exptl_absorpt_coefficient_mu 2.482 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_T_max 0.724 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 38734 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11670 _reflns_number_gt 8968 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28c4 beta ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0658P)^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_number_reflns 11670 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.007 _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 Pd1 Pd 0.74517(2) 0.629128(19) 0.233458(14) 0.01429(7) Uani 1 1 d . . . Pd2 Pd 0.71868(2) 0.40373(2) 0.258685(14) 0.01675(7) Uani 1 1 d . . . Br3 Br 0.78765(4) 0.42218(4) 0.39740(2) 0.03834(11) Uani 1 1 d . . . Br4 Br 0.54950(3) 0.68639(3) 0.21058(2) 0.02829(10) Uani 1 1 d . . . P1 P 0.52139(8) 0.32306(7) 0.24995(5) 0.01748(18) Uani 1 1 d . . . P2 P 0.83154(8) 0.78534(7) 0.33954(5) 0.01615(17) Uani 1 1 d . . . C11 C 0.4937(3) 0.1894(3) 0.2583(2) 0.0223(7) Uani 1 1 d . . . C12 C 0.3741(4) 0.1263(3) 0.2415(2) 0.0284(8) Uani 1 1 d . . . H12 H 0.3069 0.1507 0.2240 0.034 Uiso 1 1 calc R . . C13 C 0.3569(4) 0.0272(3) 0.2513(2) 0.0341(9) Uani 1 1 d . . . H13 H 0.2773 -0.0142 0.2411 0.041 Uiso 1 1 calc R . . C14 C 0.4539(4) -0.0113(3) 0.2754(2) 0.0341(10) Uani 1 1 d . . . H14 H 0.4405 -0.0787 0.2809 0.041 Uiso 1 1 calc R . . C15 C 0.5723(4) 0.0506(3) 0.2917(3) 0.0367(10) Uani 1 1 d . . . H15 H 0.6391 0.0250 0.3082 0.044 Uiso 1 1 calc R . . C16 C 0.5910(4) 0.1504(3) 0.2835(2) 0.0307(9) Uani 1 1 d . . . H16 H 0.6708 0.1922 0.2953 0.037 Uiso 1 1 calc R . . C21 C 0.4646(3) 0.4095(3) 0.3284(2) 0.0204(7) Uani 1 1 d . . . C22 C 0.3895(4) 0.3689(3) 0.3684(2) 0.0315(9) Uani 1 1 d . . . H22 H 0.3668 0.2941 0.3565 0.038 Uiso 1 1 calc R . . C23 C 0.3476(4) 0.4385(3) 0.4263(2) 0.0351(10) Uani 1 1 d . . . H23 H 0.2972 0.4106 0.4534 0.042 Uiso 1 1 calc R . . C24 C 0.3806(4) 0.5489(3) 0.4437(2) 0.0322(9) Uani 1 1 d . . . H24 H 0.3520 0.5957 0.4823 0.039 Uiso 1 1 calc R . . C25 C 0.4553(4) 0.5899(3) 0.4046(2) 0.0344(9) Uani 1 1 d . . . H25 H 0.4769 0.6647 0.4164 0.041 Uiso 1 1 calc R . . C26 C 0.4993(4) 0.5212(3) 0.3473(2) 0.0305(9) Uani 1 1 d . . . H26 H 0.5518 0.5499 0.3217 0.037 Uiso 1 1 calc R . . C31 C 0.4105(3) 0.3035(3) 0.1597(2) 0.0202(7) Uani 1 1 d . . . C32 C 0.3679(4) 0.2049(3) 0.0974(2) 0.0294(8) Uani 1 1 d . . . H32 H 0.3914 0.1434 0.1018 0.035 Uiso 1 1 calc R . . C33 C 0.2908(4) 0.1969(3) 0.0286(2) 0.0345(9) Uani 1 1 d . . . H33 H 0.2621 0.1299 -0.0125 0.041 Uiso 1 1 calc R . . C34 C 0.2563(4) 0.2863(4) 0.0205(2) 0.0354(10) Uani 1 1 d . . . H34 H 0.2046 0.2805 -0.0258 0.042 Uiso 1 1 calc R . . C35 C 0.2991(4) 0.3858(3) 0.0819(3) 0.0359(10) Uani 1 1 d . . . H35 H 0.2759 0.4470 0.0766 0.043 Uiso 1 1 calc R . . C36 C 0.3757(3) 0.3950(3) 0.1509(2) 0.0265(8) Uani 1 1 d . . . H36 H 0.4043 0.4624 0.1917 0.032 Uiso 1 1 calc R . . C41 C 0.9838(3) 0.7880(3) 0.3907(2) 0.0202(7) Uani 1 1 d . . . C42 C 1.0891(3) 0.8638(3) 0.3974(2) 0.0297(9) Uani 1 1 d . . . H42 H 1.0835 0.9197 0.3786 0.036 Uiso 1 1 calc R . . C43 C 1.2029(4) 0.8551(3) 0.4327(3) 0.0426(11) Uani 1 1 d . . . H43 H 1.2735 0.9062 0.4378 0.051 Uiso 1 1 calc R . . C44 C 1.2132(4) 0.7733(4) 0.4598(3) 0.0464(12) Uani 1 1 d . . . H44 H 1.2903 0.7687 0.4829 0.056 Uiso 1 1 calc R . . C45 C 1.1090(4) 0.6968(3) 0.4531(2) 0.0376(10) Uani 1 1 d . . . H45 H 1.1157 0.6413 0.4723 0.045 Uiso 1 1 calc R . . C46 C 0.9955(4) 0.7037(3) 0.4179(2) 0.0264(8) Uani 1 1 d . . . H46 H 0.9256 0.6514 0.4122 0.032 Uiso 1 1 calc R . . C51 C 0.8499(3) 0.9073(3) 0.3147(2) 0.0192(7) Uani 1 1 d . . . C52 C 0.8920(3) 1.0101(3) 0.3741(2) 0.0249(8) Uani 1 1 d . . . H52 H 0.9079 1.0165 0.4264 0.030 Uiso 1 1 calc R . . C53 C 0.9101(4) 1.1030(3) 0.3548(2) 0.0305(9) Uani 1 1 d . . . H53 H 0.9387 1.1715 0.3943 0.037 Uiso 1 1 calc R . . C54 C 0.8860(4) 1.0938(3) 0.2784(3) 0.0386(10) Uani 1 1 d . . . H54 H 0.8995 1.1561 0.2659 0.046 Uiso 1 1 calc R . . C55 C 0.8413(4) 0.9922(3) 0.2189(2) 0.0368(10) Uani 1 1 d . . . H55 H 0.8238 0.9864 0.1667 0.044 Uiso 1 1 calc R . . C56 C 0.8230(4) 0.9000(3) 0.2377(2) 0.0266(8) Uani 1 1 d . . . H56 H 0.7922 0.8319 0.1978 0.032 Uiso 1 1 calc R . . C61 C 0.7456(3) 0.8188(3) 0.41662(19) 0.0194(7) Uani 1 1 d . . . C62 C 0.6401(3) 0.8555(3) 0.4014(2) 0.0237(8) Uani 1 1 d . . . H62 H 0.6145 0.8623 0.3533 0.028 Uiso 1 1 calc R . . C63 C 0.5731(4) 0.8820(3) 0.4580(2) 0.0316(9) Uani 1 1 d . . . H63 H 0.5020 0.9058 0.4474 0.038 Uiso 1 1 calc R . . C64 C 0.6104(4) 0.8735(3) 0.5292(2) 0.0356(10) Uani 1 1 d . . . H64 H 0.5642 0.8902 0.5665 0.043 Uiso 1 1 calc R . . C65 C 0.7168(4) 0.8402(3) 0.5455(2) 0.0345(10) Uani 1 1 d . . . H65 H 0.7439 0.8366 0.5945 0.041 Uiso 1 1 calc R . . C66 C 0.7835(4) 0.8120(3) 0.4889(2) 0.0274(8) Uani 1 1 d . . . H66 H 0.8545 0.7883 0.4998 0.033 Uiso 1 1 calc R . . C71 C 0.9002(3) 0.5760(3) 0.24279(19) 0.0179(7) Uani 1 1 d . . . N72 N 0.8923(3) 0.4876(2) 0.26066(16) 0.0188(6) Uani 1 1 d . . . C73 C 0.9954(3) 0.4498(3) 0.2758(2) 0.0252(8) Uani 1 1 d . . . H73 H 0.9887 0.3896 0.2909 0.030 Uiso 1 1 calc R . . C74 C 1.1057(3) 0.4970(3) 0.2696(2) 0.0284(8) Uani 1 1 d . . . H74 H 1.1745 0.4715 0.2827 0.034 Uiso 1 1 calc R . . C75 C 1.2273(3) 0.6338(3) 0.2292(2) 0.0332(9) Uani 1 1 d . . . H75 H 1.2987 0.6112 0.2411 0.040 Uiso 1 1 calc R . . C76 C 1.2300(4) 0.7128(3) 0.1988(3) 0.0361(10) Uani 1 1 d . . . H76 H 1.3029 0.7427 0.1889 0.043 Uiso 1 1 calc R . . C77 C 1.1241(4) 0.7505(3) 0.1817(2) 0.0323(9) Uani 1 1 d . . . H77 H 1.1269 0.8039 0.1597 0.039 Uiso 1 1 calc R . . C78 C 1.0179(3) 0.7089(3) 0.1974(2) 0.0242(8) Uani 1 1 d . . . H78 H 0.9491 0.7360 0.1879 0.029 Uiso 1 1 calc R . . C79 C 1.0105(3) 0.6240(3) 0.2284(2) 0.0200(7) Uani 1 1 d . . . C80 C 1.1174(3) 0.5853(3) 0.2430(2) 0.0248(8) Uani 1 1 d . . . C91 C 0.6757(3) 0.3915(3) 0.14734(19) 0.0174(7) Uani 1 1 d . . . N92 N 0.6759(2) 0.4844(2) 0.13644(15) 0.0158(6) Uani 1 1 d . . . C93 C 0.6407(3) 0.4867(3) 0.0631(2) 0.0192(7) Uani 1 1 d . . . H93 H 0.6410 0.5535 0.0577 0.023 Uiso 1 1 calc R . . C94 C 0.6051(3) 0.3946(3) -0.0023(2) 0.0214(7) Uani 1 1 d . . . H94 H 0.5784 0.3980 -0.0514 0.026 Uiso 1 1 calc R . . C95 C 0.5785(4) 0.1938(3) -0.0601(2) 0.0300(9) Uani 1 1 d . . . H95 H 0.5509 0.1933 -0.1103 0.036 Uiso 1 1 calc R . . C96 C 0.5890(4) 0.1004(3) -0.0495(2) 0.0353(10) Uani 1 1 d . . . H96 H 0.5678 0.0356 -0.0927 0.042 Uiso 1 1 calc R . . C97 C 0.6314(4) 0.0992(3) 0.0256(2) 0.0334(9) Uani 1 1 d . . . H97 H 0.6416 0.0345 0.0315 0.040 Uiso 1 1 calc R . . C98 C 0.6574(4) 0.1921(3) 0.0896(2) 0.0255(8) Uani 1 1 d . . . H98 H 0.6818 0.1899 0.1393 0.031 Uiso 1 1 calc R . . C99 C 0.6477(3) 0.2919(3) 0.0815(2) 0.0199(7) Uani 1 1 d . . . C100 C 0.6096(3) 0.2931(3) 0.0056(2) 0.0217(7) Uani 1 1 d . . . Cl1 Cl 0.0716(8) 0.5290(8) 0.9876(5) 0.102(3) Uani 0.50 1 d P . . Cl2 Cl -0.0504(3) 0.3825(3) 1.0460(2) 0.0793(10) Uani 0.50 1 d P . . C1 C -0.0858(17) 0.4674(13) 1.0106(11) 0.022(3) Uiso 0.50 1 d P . . Cl3 Cl 0.0260(6) 0.1737(5) 0.1378(4) 0.1225(18) Uani 0.50 1 d P . . Cl4 Cl -0.0630(4) 0.1089(6) -0.0323(4) 0.136(2) Uani 0.50 1 d P . . C3 C -0.0304(17) 0.2254(16) 0.0634(11) 0.112(6) Uiso 0.50 1 d P . . C4 C 0.0874(17) 0.2150(15) 0.1839(11) 0.089(5) Uiso 0.50 1 d P . . C5 C -0.013(5) 0.076(4) 0.029(3) 0.154(17) Uiso 0.25 1 d P . . O6 O 0.0732(8) 0.0042(7) 0.1053(5) 0.071(2) Uiso 0.50 1 d P . . O7 O -0.0549(12) 0.1656(10) 0.1121(7) 0.099(4) Uiso 0.50 1 d P . . O8 O 0.0451(14) 0.3674(13) 0.4293(9) 0.156(5) Uiso 0.50 1 d P . . 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 Pd1 0.01351(13) 0.01279(12) 0.01566(13) 0.00432(10) 0.00219(9) 0.00374(9) Pd2 0.01802(14) 0.01641(13) 0.01745(13) 0.00768(10) 0.00400(10) 0.00549(10) Br3 0.0370(2) 0.0527(3) 0.0272(2) 0.0213(2) 0.00316(18) 0.0065(2) Br4 0.02401(19) 0.0280(2) 0.0302(2) 0.00750(16) 0.00235(15) 0.00946(15) P1 0.0206(4) 0.0143(4) 0.0194(4) 0.0075(3) 0.0060(3) 0.0050(3) P2 0.0171(4) 0.0140(4) 0.0162(4) 0.0048(3) 0.0019(3) 0.0041(3) C11 0.032(2) 0.0135(16) 0.0233(18) 0.0070(14) 0.0096(15) 0.0064(14) C12 0.035(2) 0.0219(19) 0.028(2) 0.0103(16) 0.0076(17) 0.0040(16) C13 0.046(3) 0.022(2) 0.030(2) 0.0091(17) 0.0098(19) -0.0030(18) C14 0.058(3) 0.0186(19) 0.029(2) 0.0129(16) 0.014(2) 0.0066(19) C15 0.049(3) 0.030(2) 0.043(2) 0.0218(19) 0.013(2) 0.021(2) C16 0.032(2) 0.024(2) 0.041(2) 0.0161(17) 0.0103(18) 0.0092(16) C21 0.0230(18) 0.0186(17) 0.0209(17) 0.0061(14) 0.0076(14) 0.0082(14) C22 0.040(2) 0.0230(19) 0.037(2) 0.0147(17) 0.0179(19) 0.0064(17) C23 0.049(3) 0.034(2) 0.034(2) 0.0170(18) 0.025(2) 0.016(2) C24 0.042(2) 0.033(2) 0.026(2) 0.0089(17) 0.0135(18) 0.0184(19) C25 0.045(2) 0.0178(19) 0.038(2) 0.0052(17) 0.015(2) 0.0053(17) C26 0.038(2) 0.0178(18) 0.035(2) 0.0065(16) 0.0154(18) 0.0034(16) C31 0.0191(17) 0.0211(17) 0.0237(18) 0.0109(14) 0.0072(14) 0.0056(14) C32 0.034(2) 0.026(2) 0.0263(19) 0.0064(16) 0.0050(17) 0.0101(17) C33 0.039(2) 0.031(2) 0.026(2) 0.0055(17) 0.0013(18) 0.0065(18) C34 0.027(2) 0.046(3) 0.030(2) 0.0163(19) -0.0029(17) 0.0059(19) C35 0.035(2) 0.030(2) 0.045(2) 0.0204(19) -0.0002(19) 0.0093(18) C36 0.0249(19) 0.0209(18) 0.032(2) 0.0103(16) 0.0011(16) 0.0059(15) C41 0.0196(17) 0.0195(17) 0.0180(16) 0.0034(14) 0.0005(14) 0.0062(14) C42 0.0230(19) 0.0224(19) 0.037(2) 0.0037(16) 0.0019(17) 0.0075(15) C43 0.022(2) 0.026(2) 0.059(3) -0.003(2) -0.004(2) 0.0029(17) C44 0.031(2) 0.038(3) 0.049(3) -0.004(2) -0.015(2) 0.017(2) C45 0.050(3) 0.032(2) 0.026(2) 0.0042(17) -0.0053(19) 0.023(2) C46 0.032(2) 0.0242(19) 0.0210(18) 0.0042(15) 0.0029(16) 0.0132(16) C51 0.0207(17) 0.0158(16) 0.0217(17) 0.0065(13) 0.0063(14) 0.0054(13) C52 0.0265(19) 0.0205(18) 0.0229(18) 0.0047(15) 0.0013(15) 0.0042(15) C53 0.034(2) 0.0167(18) 0.036(2) 0.0068(16) 0.0057(18) 0.0014(16) C54 0.050(3) 0.024(2) 0.047(3) 0.0216(19) 0.014(2) 0.0052(19) C55 0.058(3) 0.028(2) 0.028(2) 0.0147(17) 0.012(2) 0.011(2) C56 0.037(2) 0.0190(18) 0.0261(19) 0.0088(15) 0.0111(17) 0.0078(16) C61 0.0237(18) 0.0106(15) 0.0199(17) 0.0014(13) 0.0064(14) 0.0012(13) C62 0.0268(19) 0.0184(17) 0.0256(18) 0.0064(15) 0.0063(15) 0.0078(15) C63 0.031(2) 0.0187(19) 0.038(2) -0.0014(16) 0.0130(18) 0.0064(16) C64 0.043(3) 0.024(2) 0.032(2) -0.0017(17) 0.022(2) -0.0010(18) C65 0.050(3) 0.028(2) 0.0209(19) 0.0045(16) 0.0124(18) 0.0018(19) C66 0.031(2) 0.027(2) 0.0225(18) 0.0105(16) 0.0030(16) 0.0031(16) C71 0.0170(16) 0.0172(16) 0.0155(15) 0.0015(13) 0.0029(13) 0.0041(13) N72 0.0185(14) 0.0182(14) 0.0212(14) 0.0084(12) 0.0037(12) 0.0073(11) C73 0.0272(19) 0.0209(18) 0.0299(19) 0.0101(15) 0.0045(16) 0.0125(15) C74 0.0185(18) 0.030(2) 0.034(2) 0.0087(17) 0.0011(16) 0.0108(16) C75 0.0182(19) 0.033(2) 0.043(2) 0.0051(19) 0.0095(17) 0.0059(16) C76 0.025(2) 0.032(2) 0.046(3) 0.0071(19) 0.0171(19) 0.0006(17) C77 0.031(2) 0.025(2) 0.037(2) 0.0106(17) 0.0113(18) -0.0016(17) C78 0.0234(18) 0.0207(18) 0.0270(19) 0.0062(15) 0.0082(15) 0.0041(14) C79 0.0179(17) 0.0162(16) 0.0207(17) 0.0002(13) 0.0042(14) 0.0041(13) C80 0.0189(18) 0.0226(18) 0.0288(19) 0.0034(15) 0.0054(15) 0.0062(14) C91 0.0150(16) 0.0176(16) 0.0215(17) 0.0073(13) 0.0081(13) 0.0049(13) N92 0.0157(14) 0.0133(13) 0.0156(13) 0.0027(11) 0.0026(11) 0.0022(11) C93 0.0204(17) 0.0149(16) 0.0225(17) 0.0081(14) 0.0033(14) 0.0040(13) C94 0.0271(19) 0.0215(18) 0.0152(16) 0.0055(14) 0.0062(14) 0.0063(15) C95 0.044(2) 0.0198(19) 0.0200(18) 0.0011(15) 0.0097(17) 0.0030(17) C96 0.058(3) 0.0166(19) 0.026(2) -0.0003(15) 0.014(2) 0.0068(18) C97 0.052(3) 0.0164(18) 0.036(2) 0.0095(16) 0.019(2) 0.0105(18) C98 0.034(2) 0.0202(18) 0.0266(19) 0.0101(15) 0.0131(16) 0.0087(16) C99 0.0219(18) 0.0162(16) 0.0226(17) 0.0071(14) 0.0079(14) 0.0043(14) C100 0.0260(18) 0.0171(17) 0.0197(17) 0.0037(14) 0.0073(14) 0.0036(14) Cl1 0.097(5) 0.111(4) 0.070(3) 0.002(2) 0.003(3) 0.036(3) Cl2 0.0591(18) 0.103(3) 0.071(2) 0.0276(19) 0.0182(16) 0.0110(18) Cl3 0.110(4) 0.160(5) 0.116(4) 0.066(4) 0.054(4) 0.020(4) Cl4 0.068(2) 0.231(6) 0.165(5) 0.145(5) 0.023(3) 0.038(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 Pd1 C71 2.007(3) . ? Pd1 N92 2.086(3) . ? Pd1 P2 2.2779(9) . ? Pd1 Br4 2.4844(5) . ? Pd1 Pd2 3.1713(4) . ? Pd2 C91 1.989(3) . ? Pd2 N72 2.084(3) . ? Pd2 P1 2.2698(9) . ? Pd2 Br3 2.4819(5) . ? P1 C11 1.823(3) . ? P1 C21 1.828(3) . ? P1 C31 1.834(4) . ? P2 C41 1.817(3) . ? P2 C51 1.823(3) . ? P2 C61 1.842(3) . ? C11 C16 1.376(5) . ? C11 C12 1.397(5) . ? C12 C13 1.382(5) . ? C12 H12 0.9300 . ? C13 C14 1.362(6) . ? C13 H13 0.9300 . ? C14 C15 1.380(6) . ? C14 H14 0.9300 . ? C15 C16 1.377(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C22 1.375(5) . ? C21 C26 1.387(5) . ? C22 C23 1.384(5) . ? C22 H22 0.9300 . ? C23 C24 1.373(6) . ? C23 H23 0.9300 . ? C24 C25 1.362(6) . ? C24 H24 0.9300 . ? C25 C26 1.385(5) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C32 1.384(5) . ? C31 C36 1.398(5) . ? C32 C33 1.384(5) . ? C32 H32 0.9300 . ? C33 C34 1.364(6) . ? C33 H33 0.9300 . ? C34 C35 1.383(6) . ? C34 H34 0.9300 . ? C35 C36 1.379(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C42 1.389(5) . ? C41 C46 1.394(5) . ? C42 C43 1.390(6) . ? C42 H42 0.9300 . ? C43 C44 1.359(7) . ? C43 H43 0.9300 . ? C44 C45 1.385(7) . ? C44 H44 0.9300 . ? C45 C46 1.378(5) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C56 1.379(5) . ? C51 C52 1.396(5) . ? C52 C53 1.395(5) . ? C52 H52 0.9300 . ? C53 C54 1.360(6) . ? C53 H53 0.9300 . ? C54 C55 1.388(6) . ? C54 H54 0.9300 . ? C55 C56 1.380(5) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C61 C66 1.377(5) . ? C61 C62 1.390(5) . ? C62 C63 1.386(5) . ? C62 H62 0.9300 . ? C63 C64 1.368(6) . ? C63 H63 0.9300 . ? C64 C65 1.377(6) . ? C64 H64 0.9300 . ? C65 C66 1.386(5) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C71 N72 1.322(4) . ? C71 C79 1.416(5) . ? N72 C73 1.374(4) . ? C73 C74 1.344(5) . ? C73 H73 0.9300 . ? C74 C80 1.416(5) . ? C74 H74 0.9300 . ? C75 C76 1.348(6) . ? C75 C80 1.409(5) . ? C75 H75 0.9300 . ? C76 C77 1.408(6) . ? C76 H76 0.9300 . ? C77 C78 1.358(5) . ? C77 H77 0.9300 . ? C78 C79 1.426(5) . ? C78 H78 0.9300 . ? C79 C80 1.416(5) . ? C91 N92 1.323(4) . ? C91 C99 1.427(5) . ? N92 C93 1.366(4) . ? C93 C94 1.359(5) . ? C93 H93 0.9300 . ? C94 C100 1.420(5) . ? C94 H94 0.9300 . ? C95 C96 1.349(5) . ? C95 C100 1.420(5) . ? C95 H95 0.9300 . ? C96 C97 1.403(6) . ? C96 H96 0.9300 . ? C97 C98 1.356(5) . ? C97 H97 0.9300 . ? C98 C99 1.411(5) . ? C98 H98 0.9300 . ? C99 C100 1.411(5) . ? Cl1 Cl2 1.540(10) 2_567 ? Cl1 Cl1 1.874(18) 2_567 ? Cl1 C1 2.009(10) . ? Cl2 Cl1 1.540(10) 2_567 ? Cl2 C1 1.560(16) . ? C1 Cl1 0.15(3) 2_567 ? Cl3 O7 0.933(12) . ? Cl3 C4 0.941(16) . ? Cl3 C3 1.81(2) . ? Cl3 C5 1.93(5) . ? Cl4 C5 1.42(5) . ? Cl4 O6 1.641(10) 2 ? Cl4 C3 1.871(19) . ? C3 O7 1.42(2) . ? C3 C5 1.94(5) . ? C4 O7 1.78(2) . ? C5 O7 1.80(5) . ? O6 Cl4 1.641(10) 2 ? 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 C71 Pd1 N92 84.52(12) . . ? C71 Pd1 P2 92.34(9) . . ? N92 Pd1 P2 176.80(8) . . ? C71 Pd1 Br4 175.46(9) . . ? N92 Pd1 Br4 91.46(8) . . ? P2 Pd1 Br4 91.65(3) . . ? C71 Pd1 Pd2 64.87(10) . . ? N92 Pd1 Pd2 60.85(7) . . ? P2 Pd1 Pd2 118.30(2) . . ? Br4 Pd1 Pd2 114.885(14) . . ? C91 Pd2 N72 84.97(12) . . ? C91 Pd2 P1 90.82(10) . . ? N72 Pd2 P1 174.02(8) . . ? C91 Pd2 Br3 176.01(9) . . ? N72 Pd2 Br3 91.22(8) . . ? P1 Pd2 Br3 93.07(3) . . ? C91 Pd2 Pd1 65.08(9) . . ? N72 Pd2 Pd1 61.22(8) . . ? P1 Pd2 Pd1 113.11(2) . . ? Br3 Pd2 Pd1 113.993(16) . . ? C11 P1 C21 105.47(16) . . ? C11 P1 C31 103.99(16) . . ? C21 P1 C31 104.43(16) . . ? C11 P1 Pd2 117.06(13) . . ? C21 P1 Pd2 109.40(12) . . ? C31 P1 Pd2 115.34(11) . . ? C41 P2 C51 105.74(16) . . ? C41 P2 C61 104.68(16) . . ? C51 P2 C61 102.01(15) . . ? C41 P2 Pd1 113.23(11) . . ? C51 P2 Pd1 113.13(11) . . ? C61 P2 Pd1 116.81(11) . . ? C16 C11 C12 118.8(3) . . ? C16 C11 P1 120.1(3) . . ? C12 C11 P1 121.0(3) . . ? C13 C12 C11 119.2(4) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 121.5(4) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 119.5(4) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 119.7(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C11 C16 C15 121.2(4) . . ? C11 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C22 C21 C26 119.3(3) . . ? C22 C21 P1 123.2(3) . . ? C26 C21 P1 117.5(3) . . ? C21 C22 C23 120.4(4) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 119.9(4) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 120.1(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.6(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 119.6(4) . . ? C25 C26 H26 120.2 . . ? C21 C26 H26 120.2 . . ? C32 C31 C36 118.4(3) . . ? C32 C31 P1 123.3(3) . . ? C36 C31 P1 118.0(3) . . ? C31 C32 C33 120.7(4) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 120.7(4) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 119.4(4) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C36 C35 C34 120.6(4) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C31 120.2(4) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C42 C41 C46 119.0(3) . . ? C42 C41 P2 123.1(3) . . ? C46 C41 P2 117.6(3) . . ? C41 C42 C43 119.2(4) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C44 C43 C42 121.3(4) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 120.2(4) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C46 C45 C44 119.4(4) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C45 C46 C41 120.9(4) . . ? C45 C46 H46 119.5 . . ? C41 C46 H46 119.5 . . ? C56 C51 C52 119.0(3) . . ? C56 C51 P2 121.1(3) . . ? C52 C51 P2 119.9(3) . . ? C53 C52 C51 119.8(3) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C54 C53 C52 120.2(4) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C55 120.5(4) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C56 C55 C54 119.5(4) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? C51 C56 C55 120.9(4) . . ? C51 C56 H56 119.5 . . ? C55 C56 H56 119.5 . . ? C66 C61 C62 119.1(3) . . ? C66 C61 P2 122.8(3) . . ? C62 C61 P2 118.1(3) . . ? C63 C62 C61 119.9(4) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C64 C63 C62 120.6(4) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C63 C64 C65 119.7(4) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C64 C65 C66 120.0(4) . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C61 C66 C65 120.6(4) . . ? C61 C66 H66 119.7 . . ? C65 C66 H66 119.7 . . ? N72 C71 C79 120.3(3) . . ? N72 C71 Pd1 115.2(2) . . ? C79 C71 Pd1 124.4(2) . . ? C71 N72 C73 120.3(3) . . ? C71 N72 Pd2 118.0(2) . . ? C73 N72 Pd2 121.6(2) . . ? C74 C73 N72 122.1(3) . . ? C74 C73 H73 119.0 . . ? N72 C73 H73 119.0 . . ? C73 C74 C80 120.2(3) . . ? C73 C74 H74 119.9 . . ? C80 C74 H74 119.9 . . ? C76 C75 C80 120.7(4) . . ? C76 C75 H75 119.7 . . ? C80 C75 H75 119.7 . . ? C75 C76 C77 121.0(4) . . ? C75 C76 H76 119.5 . . ? C77 C76 H76 119.5 . . ? C78 C77 C76 119.9(4) . . ? C78 C77 H77 120.0 . . ? C76 C77 H77 120.0 . . ? C77 C78 C79 120.8(4) . . ? C77 C78 H78 119.6 . . ? C79 C78 H78 119.6 . . ? C71 C79 C80 119.5(3) . . ? C71 C79 C78 122.3(3) . . ? C80 C79 C78 118.2(3) . . ? C75 C80 C74 123.7(4) . . ? C75 C80 C79 119.3(4) . . ? C74 C80 C79 117.0(3) . . ? N92 C91 C99 120.1(3) . . ? N92 C91 Pd2 115.4(2) . . ? C99 C91 Pd2 124.6(2) . . ? C91 N92 C93 121.2(3) . . ? C91 N92 Pd1 118.1(2) . . ? C93 N92 Pd1 120.5(2) . . ? C94 C93 N92 122.2(3) . . ? C94 C93 H93 118.9 . . ? N92 C93 H93 118.9 . . ? C93 C94 C100 118.9(3) . . ? C93 C94 H94 120.6 . . ? C100 C94 H94 120.6 . . ? C96 C95 C100 119.8(4) . . ? C96 C95 H95 120.1 . . ? C100 C95 H95 120.1 . . ? C95 C96 C97 121.2(4) . . ? C95 C96 H96 119.4 . . ? C97 C96 H96 119.4 . . ? C98 C97 C96 120.2(4) . . ? C98 C97 H97 119.9 . . ? C96 C97 H97 119.9 . . ? C97 C98 C99 120.7(4) . . ? C97 C98 H98 119.7 . . ? C99 C98 H98 119.7 . . ? C98 C99 C100 118.7(3) . . ? C98 C99 C91 122.3(3) . . ? C100 C99 C91 118.9(3) . . ? C99 C100 C95 119.3(3) . . ? C99 C100 C94 118.4(3) . . ? C95 C100 C94 122.3(3) . . ? Cl2 Cl1 Cl1 110.4(8) 2_567 2_567 ? Cl2 Cl1 C1 108.6(4) 2_567 . ? Cl1 C1 Cl2 80(8) 2_567 . ? Cl2 C1 Cl1 103.1(8) . . ? O7 Cl3 C4 143.7(17) . . ? O7 Cl3 C3 50.9(10) . . ? C4 Cl3 C3 124.4(14) . . ? O7 Cl3 C5 67.9(17) . . ? C4 Cl3 C5 147.3(19) . . ? C3 Cl3 C5 62.3(16) . . ? C5 Cl4 O6 97(2) . 2 ? C5 Cl4 C3 71(2) . . ? O6 Cl4 C3 167.8(8) 2 . ? O7 C3 Cl4 98.9(12) . . ? Cl3 C3 Cl4 105.7(10) . . ? O7 C3 C5 62.7(17) . . ? Cl3 C3 C5 62.0(17) . . ? Cl4 C5 O7 102(3) . . ? Cl4 C5 Cl3 121(3) . . ? Cl4 C5 C3 66(2) . . ? Cl3 C5 C3 55.7(15) . . ? Cl3 O7 C3 98.4(14) . . ? C3 O7 C4 100.2(13) . . ? Cl3 O7 C5 83.5(19) . . ? C3 O7 C5 72.9(18) . . ? C4 O7 C5 101.4(18) . . ? 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 C71 Pd1 Pd2 C91 -94.32(14) . . . . ? N92 Pd1 Pd2 C91 3.77(13) . . . . ? P2 Pd1 Pd2 C91 -172.72(11) . . . . ? Br4 Pd1 Pd2 C91 80.67(10) . . . . ? C71 Pd1 Pd2 N72 4.00(13) . . . . ? N92 Pd1 Pd2 N72 102.09(12) . . . . ? P2 Pd1 Pd2 N72 -74.39(9) . . . . ? Br4 Pd1 Pd2 N72 179.00(9) . . . . ? C71 Pd1 Pd2 P1 -173.89(10) . . . . ? N92 Pd1 Pd2 P1 -75.80(9) . . . . ? P2 Pd1 Pd2 P1 107.72(4) . . . . ? Br4 Pd1 Pd2 P1 1.11(3) . . . . ? C71 Pd1 Pd2 Br3 81.41(10) . . . . ? N92 Pd1 Pd2 Br3 179.50(9) . . . . ? P2 Pd1 Pd2 Br3 3.02(3) . . . . ? Br4 Pd1 Pd2 Br3 -103.593(19) . . . . ? C91 Pd2 P1 C11 113.70(16) . . . . ? Br3 Pd2 P1 C11 -65.42(13) . . . . ? Pd1 Pd2 P1 C11 176.82(13) . . . . ? C91 Pd2 P1 C21 -126.48(15) . . . . ? Br3 Pd2 P1 C21 54.40(12) . . . . ? Pd1 Pd2 P1 C21 -63.35(12) . . . . ? C91 Pd2 P1 C31 -9.15(16) . . . . ? Br3 Pd2 P1 C31 171.73(13) . . . . ? Pd1 Pd2 P1 C31 53.98(13) . . . . ? C71 Pd1 P2 C41 -6.75(16) . . . . ? Br4 Pd1 P2 C41 175.40(13) . . . . ? Pd2 Pd1 P2 C41 55.82(13) . . . . ? C71 Pd1 P2 C51 113.54(16) . . . . ? Br4 Pd1 P2 C51 -64.31(12) . . . . ? Pd2 Pd1 P2 C51 176.11(12) . . . . ? C71 Pd1 P2 C61 -128.47(16) . . . . ? Br4 Pd1 P2 C61 53.68(13) . . . . ? Pd2 Pd1 P2 C61 -65.90(13) . . . . ? C21 P1 C11 C16 -109.9(3) . . . . ? C31 P1 C11 C16 140.5(3) . . . . ? Pd2 P1 C11 C16 12.0(4) . . . . ? C21 P1 C11 C12 68.2(3) . . . . ? C31 P1 C11 C12 -41.4(3) . . . . ? Pd2 P1 C11 C12 -169.9(3) . . . . ? C16 C11 C12 C13 0.4(5) . . . . ? P1 C11 C12 C13 -177.7(3) . . . . ? C11 C12 C13 C14 -1.2(6) . . . . ? C12 C13 C14 C15 1.0(6) . . . . ? C13 C14 C15 C16 0.1(6) . . . . ? C12 C11 C16 C15 0.6(6) . . . . ? P1 C11 C16 C15 178.7(3) . . . . ? C14 C15 C16 C11 -0.9(6) . . . . ? C11 P1 C21 C22 -14.9(4) . . . . ? C31 P1 C21 C22 94.4(3) . . . . ? Pd2 P1 C21 C22 -141.6(3) . . . . ? C11 P1 C21 C26 165.5(3) . . . . ? C31 P1 C21 C26 -85.2(3) . . . . ? Pd2 P1 C21 C26 38.8(3) . . . . ? C26 C21 C22 C23 0.8(6) . . . . ? P1 C21 C22 C23 -178.8(3) . . . . ? C21 C22 C23 C24 0.3(7) . . . . ? C22 C23 C24 C25 -0.5(7) . . . . ? C23 C24 C25 C26 -0.4(7) . . . . ? C24 C25 C26 C21 1.5(7) . . . . ? C22 C21 C26 C25 -1.7(6) . . . . ? P1 C21 C26 C25 177.9(3) . . . . ? C11 P1 C31 C32 -28.7(3) . . . . ? C21 P1 C31 C32 -139.0(3) . . . . ? Pd2 P1 C31 C32 100.9(3) . . . . ? C11 P1 C31 C36 157.0(3) . . . . ? C21 P1 C31 C36 46.6(3) . . . . ? Pd2 P1 C31 C36 -73.5(3) . . . . ? C36 C31 C32 C33 -1.2(6) . . . . ? P1 C31 C32 C33 -175.5(3) . . . . ? C31 C32 C33 C34 0.8(6) . . . . ? C32 C33 C34 C35 -0.1(7) . . . . ? C33 C34 C35 C36 -0.1(7) . . . . ? C34 C35 C36 C31 -0.4(6) . . . . ? C32 C31 C36 C35 1.0(6) . . . . ? P1 C31 C36 C35 175.6(3) . . . . ? C51 P2 C41 C42 -7.1(3) . . . . ? C61 P2 C41 C42 -114.4(3) . . . . ? Pd1 P2 C41 C42 117.3(3) . . . . ? C51 P2 C41 C46 178.8(3) . . . . ? C61 P2 C41 C46 71.5(3) . . . . ? Pd1 P2 C41 C46 -56.8(3) . . . . ? C46 C41 C42 C43 -1.4(6) . . . . ? P2 C41 C42 C43 -175.4(3) . . . . ? C41 C42 C43 C44 0.7(7) . . . . ? C42 C43 C44 C45 -0.4(7) . . . . ? C43 C44 C45 C46 0.8(7) . . . . ? C44 C45 C46 C41 -1.5(6) . . . . ? C42 C41 C46 C45 1.8(5) . . . . ? P2 C41 C46 C45 176.2(3) . . . . ? C41 P2 C51 C56 119.0(3) . . . . ? C61 P2 C51 C56 -131.8(3) . . . . ? Pd1 P2 C51 C56 -5.5(3) . . . . ? C41 P2 C51 C52 -60.9(3) . . . . ? C61 P2 C51 C52 48.3(3) . . . . ? Pd1 P2 C51 C52 174.7(3) . . . . ? C56 C51 C52 C53 -2.1(6) . . . . ? P2 C51 C52 C53 177.7(3) . . . . ? C51 C52 C53 C54 0.5(6) . . . . ? C52 C53 C54 C55 1.1(7) . . . . ? C53 C54 C55 C56 -1.0(7) . . . . ? C52 C51 C56 C55 2.2(6) . . . . ? P2 C51 C56 C55 -177.6(3) . . . . ? C54 C55 C56 C51 -0.7(7) . . . . ? C41 P2 C61 C66 -17.3(3) . . . . ? C51 P2 C61 C66 -127.4(3) . . . . ? Pd1 P2 C61 C66 108.8(3) . . . . ? C41 P2 C61 C62 160.7(3) . . . . ? C51 P2 C61 C62 50.7(3) . . . . ? Pd1 P2 C61 C62 -73.2(3) . . . . ? C66 C61 C62 C63 -1.6(5) . . . . ? P2 C61 C62 C63 -179.7(3) . . . . ? C61 C62 C63 C64 0.7(6) . . . . ? C62 C63 C64 C65 1.2(6) . . . . ? C63 C64 C65 C66 -2.1(6) . . . . ? C62 C61 C66 C65 0.7(5) . . . . ? P2 C61 C66 C65 178.7(3) . . . . ? C64 C65 C66 C61 1.2(6) . . . . ? N92 Pd1 C71 N72 -66.4(2) . . . . ? P2 Pd1 C71 N72 114.2(2) . . . . ? Pd2 Pd1 C71 N72 -6.1(2) . . . . ? N92 Pd1 C71 C79 110.8(3) . . . . ? P2 Pd1 C71 C79 -68.6(3) . . . . ? Pd2 Pd1 C71 C79 171.1(3) . . . . ? C79 C71 N72 C73 8.8(5) . . . . ? Pd1 C71 N72 C73 -173.9(2) . . . . ? C79 C71 N72 Pd2 -167.8(2) . . . . ? Pd1 C71 N72 Pd2 9.6(3) . . . . ? C91 Pd2 N72 C71 58.0(3) . . . . ? Br3 Pd2 N72 C71 -123.1(2) . . . . ? Pd1 Pd2 N72 C71 -6.2(2) . . . . ? C91 Pd2 N72 C73 -118.5(3) . . . . ? Br3 Pd2 N72 C73 60.4(3) . . . . ? Pd1 Pd2 N72 C73 177.3(3) . . . . ? C71 N72 C73 C74 -3.2(5) . . . . ? Pd2 N72 C73 C74 173.2(3) . . . . ? N72 C73 C74 C80 -3.1(6) . . . . ? C80 C75 C76 C77 1.4(6) . . . . ? C75 C76 C77 C78 1.4(6) . . . . ? C76 C77 C78 C79 -2.4(6) . . . . ? N72 C71 C79 C80 -8.1(5) . . . . ? Pd1 C71 C79 C80 174.8(3) . . . . ? N72 C71 C79 C78 170.2(3) . . . . ? Pd1 C71 C79 C78 -6.8(5) . . . . ? C77 C78 C79 C71 -177.7(3) . . . . ? C77 C78 C79 C80 0.7(5) . . . . ? C76 C75 C80 C74 175.4(4) . . . . ? C76 C75 C80 C79 -3.2(6) . . . . ? C73 C74 C80 C75 -175.0(4) . . . . ? C73 C74 C80 C79 3.6(5) . . . . ? C71 C79 C80 C75 -179.5(3) . . . . ? C78 C79 C80 C75 2.1(5) . . . . ? C71 C79 C80 C74 1.8(5) . . . . ? C78 C79 C80 C74 -176.6(3) . . . . ? N72 Pd2 C91 N92 -66.3(2) . . . . ? P1 Pd2 C91 N92 109.5(2) . . . . ? Pd1 Pd2 C91 N92 -5.7(2) . . . . ? N72 Pd2 C91 C99 112.7(3) . . . . ? P1 Pd2 C91 C99 -71.5(3) . . . . ? Pd1 Pd2 C91 C99 173.3(3) . . . . ? C99 C91 N92 C93 5.0(5) . . . . ? Pd2 C91 N92 C93 -175.9(2) . . . . ? C99 C91 N92 Pd1 -170.1(2) . . . . ? Pd2 C91 N92 Pd1 9.0(3) . . . . ? C71 Pd1 N92 C91 58.4(3) . . . . ? Br4 Pd1 N92 C91 -123.7(2) . . . . ? Pd2 Pd1 N92 C91 -5.8(2) . . . . ? C71 Pd1 N92 C93 -116.7(3) . . . . ? Br4 Pd1 N92 C93 61.2(2) . . . . ? Pd2 Pd1 N92 C93 179.1(3) . . . . ? C91 N92 C93 C94 -0.7(5) . . . . ? Pd1 N92 C93 C94 174.2(3) . . . . ? N92 C93 C94 C100 -2.7(5) . . . . ? C100 C95 C96 C97 -0.5(7) . . . . ? C95 C96 C97 C98 3.0(7) . . . . ? C96 C97 C98 C99 -2.9(6) . . . . ? C97 C98 C99 C100 0.5(6) . . . . ? C97 C98 C99 C91 -179.3(4) . . . . ? N92 C91 C99 C98 174.0(3) . . . . ? Pd2 C91 C99 C98 -5.0(5) . . . . ? N92 C91 C99 C100 -5.8(5) . . . . ? Pd2 C91 C99 C100 175.3(3) . . . . ? C98 C99 C100 C95 1.9(5) . . . . ? C91 C99 C100 C95 -178.3(3) . . . . ? C98 C99 C100 C94 -177.4(3) . . . . ? C91 C99 C100 C94 2.4(5) . . . . ? C96 C95 C100 C99 -1.9(6) . . . . ? C96 C95 C100 C94 177.4(4) . . . . ? C93 C94 C100 C99 1.7(5) . . . . ? C93 C94 C100 C95 -177.6(4) . . . . ? Cl1 Cl2 C1 Cl1 15(10) 2_567 . . . ? Cl2 Cl1 C1 Cl1 -145(21) 2_567 . . 2_567 ? Cl2 Cl1 C1 Cl2 -178.4(10) 2_567 . . . ? Cl1 Cl1 C1 Cl2 -34(20) 2_567 . . . ? C4 Cl3 C3 O7 -135(2) . . . . ? C5 Cl3 C3 O7 83(2) . . . . ? O7 Cl3 C3 Cl4 -80.9(14) . . . . ? C4 Cl3 C3 Cl4 144.5(16) . . . . ? C5 Cl3 C3 Cl4 2.1(17) . . . . ? O7 Cl3 C3 C5 -83(2) . . . . ? C4 Cl3 C3 C5 142(2) . . . . ? C5 Cl4 C3 O7 -33(2) . . . . ? O6 Cl4 C3 O7 -48(4) 2 . . . ? C5 Cl4 C3 Cl3 -3(2) . . . . ? O6 Cl4 C3 Cl3 -17(4) 2 . . . ? O6 Cl4 C3 C5 -14(4) 2 . . . ? C3 Cl3 C4 O7 69(2) . . . . ? C5 Cl3 C4 O7 160(5) . . . . ? O6 Cl4 C5 O7 -157.1(19) 2 . . . ? C3 Cl4 C5 O7 25.9(16) . . . . ? O6 Cl4 C5 Cl3 180(3) 2 . . . ? C3 Cl4 C5 Cl3 3(2) . . . . ? O6 Cl4 C5 C3 177.0(9) 2 . . . ? O7 Cl3 C5 Cl4 53(3) . . . . ? C4 Cl3 C5 Cl4 -114(4) . . . . ? C3 Cl3 C5 Cl4 -3(3) . . . . ? C4 Cl3 C5 O7 -168(3) . . . . ? C3 Cl3 C5 O7 -56.3(13) . . . . ? O7 Cl3 C5 C3 56.3(13) . . . . ? C4 Cl3 C5 C3 -111(3) . . . . ? O7 C3 C5 Cl4 142(2) . . . . ? Cl3 C3 C5 Cl4 177(2) . . . . ? Cl3 C3 C5 O7 34.7(8) . . . . ? Cl4 C3 C5 O7 -142(2) . . . . ? O7 C3 C5 Cl3 -34.7(8) . . . . ? Cl4 C3 C5 Cl3 -177(2) . . . . ? C4 Cl3 O7 C3 97(3) . . . . ? C5 Cl3 O7 C3 -71.6(19) . . . . ? C3 Cl3 O7 C4 -97(3) . . . . ? C5 Cl3 O7 C4 -169(3) . . . . ? C4 Cl3 O7 C5 169(3) . . . . ? C3 Cl3 O7 C5 71.6(19) . . . . ? Cl4 C3 O7 Cl3 105.7(12) . . . . ? C5 C3 O7 Cl3 80.5(19) . . . . ? Cl3 C3 O7 C4 18.4(9) . . . . ? Cl4 C3 O7 C4 124.1(10) . . . . ? C5 C3 O7 C4 98.8(19) . . . . ? Cl3 C3 O7 C5 -80.5(19) . . . . ? Cl4 C3 O7 C5 25.3(18) . . . . ? Cl3 C4 O7 C3 -86(3) . . . . ? Cl3 C4 O7 C5 -11(3) . . . . ? Cl4 C5 O7 Cl3 -136(3) . . . . ? C3 C5 O7 Cl3 -100.9(14) . . . . ? Cl4 C5 O7 C3 -35(2) . . . . ? Cl3 C5 O7 C3 100.9(14) . . . . ? Cl4 C5 O7 C4 -132(2) . . . . ? Cl3 C5 O7 C4 3.6(9) . . . . ? C3 C5 O7 C4 -97.3(14) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.962 _refine_diff_density_min -1.459 _refine_diff_density_rms 0.115 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 728914' _chemical_formula_structural '[Li2{L(H)}2(THF)2].THF' _chemical_formula_moiety 'C62 H72 Li2 N2 O4, C4 H8 O' _chemical_formula_sum 'C66 H80 Li2 N2 O5' _chemical_formula_weight 995.20 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.524(6) _cell_length_b 10.431(4) _cell_length_c 37.439(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.995(4) _cell_angle_gamma 90.00 _cell_volume 6429(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 897 _cell_measurement_theta_min 4.60 _cell_measurement_theta_max 29.26 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.518 _exptl_absorpt_correction_T_max 0.9962 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.7977 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 16.2smx' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD diffractometer' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31733 _diffrn_reflns_av_R_equivalents 0.0804 _diffrn_reflns_av_sigmaI/netI 0.1082 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 4.60 _diffrn_reflns_theta_max 28.38 _reflns_number_total 11065 _reflns_number_gt 5747 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004) ; _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^ > 2\s(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^)+(0.1277P)^2^] 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 0.0073(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11065 _refine_ls_number_parameters 706 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1354 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2263 _refine_ls_wR_factor_gt 0.1969 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _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 Li1 Li 0.5696(3) 0.3879(5) 0.18137(14) 0.0437(13) Uani 1 1 d . . . Li2 Li 0.4797(3) 0.1923(6) 0.17393(15) 0.0496(14) Uani 1 1 d . A . N1 N 0.53776(16) 0.5358(3) 0.14849(7) 0.0432(7) Uani 1 1 d . . . O1 O 0.56004(12) 0.2548(2) 0.14599(5) 0.0411(5) Uani 1 1 d . . . C1 C 0.60096(17) 0.4093(3) 0.10459(8) 0.0357(7) Uani 1 1 d . . . C2 C 0.60539(17) 0.2852(3) 0.11959(8) 0.0381(8) Uani 1 1 d . . . C3 C 0.66081(18) 0.1920(3) 0.10621(8) 0.0402(8) Uani 1 1 d . . . C4 C 0.71300(18) 0.2333(3) 0.08204(9) 0.0447(8) Uani 1 1 d . . . H4 H 0.7495 0.1727 0.0734 0.054 Uiso 1 1 calc R . . C5 C 0.71559(18) 0.3620(3) 0.06915(8) 0.0427(8) Uani 1 1 d . . . C6 C 0.77353(18) 0.4024(4) 0.04575(9) 0.0486(9) Uani 1 1 d . . . H6 H 0.8106 0.3411 0.0379 0.058 Uiso 1 1 calc R . . C7 C 0.77827(19) 0.5276(4) 0.03393(9) 0.0518(9) Uani 1 1 d . . . C8 C 0.7227(2) 0.6159(4) 0.04637(9) 0.0515(9) Uani 1 1 d . . . H8 H 0.7258 0.7031 0.0394 0.062 Uiso 1 1 calc R . . C9 C 0.66397(19) 0.5801(3) 0.06833(8) 0.0446(8) Uani 1 1 d . . . H9 H 0.6268 0.6425 0.0755 0.053 Uiso 1 1 calc R . . C10 C 0.65803(18) 0.4512(3) 0.08050(8) 0.0403(8) Uani 1 1 d . . . C11 C 0.53653(18) 0.5000(3) 0.11423(8) 0.0367(7) Uani 1 1 d . . . C12 C 0.4804(2) 0.6222(3) 0.15795(9) 0.0514(9) Uani 1 1 d . . . H12 H 0.4806 0.6450 0.1825 0.062 Uiso 1 1 calc R . . C13 C 0.4237(2) 0.6766(3) 0.13439(9) 0.0523(9) Uani 1 1 d . . . H13 H 0.3875 0.7394 0.1422 0.063 Uiso 1 1 calc R . . C14 C 0.4188(2) 0.6391(3) 0.09819(9) 0.0461(8) Uani 1 1 d . . . C15 C 0.3585(2) 0.6862(4) 0.07229(10) 0.0552(10) Uani 1 1 d . . . H15 H 0.3212 0.7493 0.0790 0.066 Uiso 1 1 calc R . . C16 C 0.3533(2) 0.6422(4) 0.03812(10) 0.0629(11) Uani 1 1 d . . . H16 H 0.3130 0.6756 0.0210 0.075 Uiso 1 1 calc R . . C17 C 0.4076(2) 0.5466(4) 0.02777(10) 0.0550(10) Uani 1 1 d . . . H17 H 0.4026 0.5144 0.0039 0.066 Uiso 1 1 calc R . . C18 C 0.46724(18) 0.5009(3) 0.05210(8) 0.0429(8) Uani 1 1 d . . . H18 H 0.5037 0.4374 0.0449 0.051 Uiso 1 1 calc R . . C19 C 0.47561(18) 0.5459(3) 0.08753(8) 0.0379(8) Uani 1 1 d . . . C30 C 0.66051(19) 0.0511(3) 0.11921(9) 0.0490(9) Uani 1 1 d . . . C31 C 0.5769(2) -0.0094(3) 0.10973(10) 0.0537(9) Uani 1 1 d . . . H31A H 0.5773 -0.0981 0.1183 0.080 Uiso 1 1 calc R . . H31B H 0.5645 -0.0083 0.0837 0.080 Uiso 1 1 calc R . . H31C H 0.5356 0.0396 0.1211 0.080 Uiso 1 1 calc R . . C32 C 0.6823(2) 0.0450(4) 0.16002(10) 0.0564(10) Uani 1 1 d . . . H32A H 0.6397 0.0874 0.1724 0.085 Uiso 1 1 calc R . . H32B H 0.7343 0.0885 0.1660 0.085 Uiso 1 1 calc R . . H32C H 0.6868 -0.0448 0.1676 0.085 Uiso 1 1 calc R . . C33 C 0.7234(2) -0.0311(4) 0.10152(12) 0.0684(11) Uani 1 1 d . . . H33A H 0.7219 -0.1192 0.1106 0.103 Uiso 1 1 calc R . . H33B H 0.7778 0.0048 0.1073 0.103 Uiso 1 1 calc R . . H33C H 0.7106 -0.0313 0.0755 0.103 Uiso 1 1 calc R . . C70 C 0.8416(2) 0.5735(4) 0.00894(11) 0.0677(12) Uani 1 1 d . . . C71 C 0.8005(2) 0.6484(5) -0.02217(12) 0.0833(14) Uani 1 1 d . . . H71A H 0.7621 0.5926 -0.0362 0.125 Uiso 1 1 calc R . . H71B H 0.8415 0.6797 -0.0374 0.125 Uiso 1 1 calc R . . H71C H 0.7712 0.7214 -0.0130 0.125 Uiso 1 1 calc R . . C72 C 0.9036(2) 0.6607(5) 0.03111(12) 0.0860(14) Uani 1 1 d . . . H72A H 0.9446 0.6912 0.0157 0.129 Uiso 1 1 calc R . . H72B H 0.9301 0.6116 0.0512 0.129 Uiso 1 1 calc R . . H72C H 0.8751 0.7342 0.0404 0.129 Uiso 1 1 calc R . . C73 C 0.8874(2) 0.4596(5) -0.00674(12) 0.0827(14) Uani 1 1 d . . . H73A H 0.8483 0.4033 -0.0203 0.124 Uiso 1 1 calc R . . H73B H 0.9162 0.4111 0.0129 0.124 Uiso 1 1 calc R . . H73C H 0.9265 0.4923 -0.0227 0.124 Uiso 1 1 calc R . . N11 N 0.65165(14) 0.3867(3) 0.22460(7) 0.0420(7) Uani 1 1 d . . . O11 O 0.48209(11) 0.3282(2) 0.20704(5) 0.0391(5) Uani 1 1 d . . . C101 C 0.53856(16) 0.4360(3) 0.25920(8) 0.0330(7) Uani 1 1 d . . . C102 C 0.47214(17) 0.4015(3) 0.23484(8) 0.0348(7) Uani 1 1 d . . . C103 C 0.39154(17) 0.4495(3) 0.24125(9) 0.0415(8) Uani 1 1 d . . . C104 C 0.38464(18) 0.5361(3) 0.26787(9) 0.0441(8) Uani 1 1 d . . . H104 H 0.3323 0.5692 0.2712 0.053 Uiso 1 1 calc R . . C105 C 0.45217(17) 0.5802(3) 0.29128(8) 0.0376(8) Uani 1 1 d . . . C106 C 0.44199(18) 0.6704(3) 0.31877(9) 0.0431(8) Uani 1 1 d . . . H106 H 0.3890 0.7026 0.3214 0.052 Uiso 1 1 calc R . . C107 C 0.50606(17) 0.7139(3) 0.34206(8) 0.0382(8) Uani 1 1 d . . . C108 C 0.58401(18) 0.6640(3) 0.33643(8) 0.0389(8) Uani 1 1 d . . . H108 H 0.6298 0.6930 0.3514 0.047 Uiso 1 1 calc R . . C109 C 0.59567(17) 0.5759(3) 0.31034(8) 0.0357(7) Uani 1 1 d . . . H109 H 0.6490 0.5453 0.3078 0.043 Uiso 1 1 calc R . . C110 C 0.52992(16) 0.5287(3) 0.28685(8) 0.0336(7) Uani 1 1 d . . . C111 C 0.61949(17) 0.3738(3) 0.25575(8) 0.0352(7) Uani 1 1 d . . . C112 C 0.72506(19) 0.3320(4) 0.22027(10) 0.0550(10) Uani 1 1 d . . . H112 H 0.7472 0.3424 0.1979 0.066 Uiso 1 1 calc R . . C113 C 0.7683(2) 0.2636(4) 0.24607(10) 0.0591(11) Uani 1 1 d . . . H113 H 0.8199 0.2295 0.2419 0.071 Uiso 1 1 calc R . . C114 C 0.73588(19) 0.2434(3) 0.27932(9) 0.0494(9) Uani 1 1 d . . . C115 C 0.7764(2) 0.1704(4) 0.30732(11) 0.0635(11) Uani 1 1 d . . . H115 H 0.8287 0.1361 0.3043 0.076 Uiso 1 1 calc R . . C116 C 0.7422(3) 0.1488(4) 0.33803(12) 0.0666(12) Uani 1 1 d . . . H116 H 0.7700 0.0981 0.3563 0.080 Uiso 1 1 calc R . . C117 C 0.6653(2) 0.2009(3) 0.34336(9) 0.0563(10) Uani 1 1 d . . . H117 H 0.6415 0.1847 0.3651 0.068 Uiso 1 1 calc R . . C118 C 0.6250(2) 0.2747(3) 0.31727(8) 0.0426(8) Uani 1 1 d . . . H118 H 0.5734 0.3098 0.3211 0.051 Uiso 1 1 calc R . . C119 C 0.65943(18) 0.2992(3) 0.28458(8) 0.0387(8) Uani 1 1 d . . . C130 C 0.31576(18) 0.3975(4) 0.21824(10) 0.0531(10) Uani 1 1 d . . . C131 C 0.3173(2) 0.4329(4) 0.17871(10) 0.0615(11) Uani 1 1 d . . . H13A H 0.2717 0.3914 0.1647 0.092 Uiso 1 1 calc R . . H13B H 0.3685 0.4040 0.1700 0.092 Uiso 1 1 calc R . . H13C H 0.3126 0.5261 0.1760 0.092 Uiso 1 1 calc R . . C132 C 0.3136(2) 0.2501(4) 0.22287(11) 0.0636(11) Uani 1 1 d . . . H13D H 0.2665 0.2151 0.2084 0.095 Uiso 1 1 calc R . . H13E H 0.3095 0.2292 0.2482 0.095 Uiso 1 1 calc R . . H13F H 0.3635 0.2127 0.2150 0.095 Uiso 1 1 calc R . . C133 C 0.2367(2) 0.4507(5) 0.23131(13) 0.0840(15) Uani 1 1 d . . . H13G H 0.2368 0.5445 0.2297 0.126 Uiso 1 1 calc R . . H13H H 0.2327 0.4249 0.2563 0.126 Uiso 1 1 calc R . . H13I H 0.1901 0.4167 0.2163 0.126 Uiso 1 1 calc R . . C170 C 0.49689(19) 0.8061(3) 0.37296(9) 0.0476(9) Uani 1 1 d . . . C171 C 0.4107(2) 0.8601(4) 0.37301(11) 0.0666(11) Uani 1 1 d . . . H17A H 0.3952 0.9016 0.3499 0.100 Uiso 1 1 calc R . . H17B H 0.4091 0.9231 0.3923 0.100 Uiso 1 1 calc R . . H17C H 0.3727 0.7903 0.3768 0.100 Uiso 1 1 calc R . . C172 C 0.5176(3) 0.7349(4) 0.40870(9) 0.0681(11) Uani 1 1 d . . . H17D H 0.4795 0.6637 0.4106 0.102 Uiso 1 1 calc R . . H17E H 0.5133 0.7943 0.4287 0.102 Uiso 1 1 calc R . . H17F H 0.5731 0.7013 0.4095 0.102 Uiso 1 1 calc R . . C173 C 0.5557(2) 0.9207(4) 0.37088(10) 0.0624(11) Uani 1 1 d . . . H17G H 0.6118 0.8895 0.3730 0.094 Uiso 1 1 calc R . . H17H H 0.5480 0.9807 0.3904 0.094 Uiso 1 1 calc R . . H17I H 0.5444 0.9645 0.3478 0.094 Uiso 1 1 calc R . . O211 O 0.38949(14) 0.1506(3) 0.13812(6) 0.0613(7) Uani 1 1 d . . . C201 C 0.3862(2) 0.2092(4) 0.10324(10) 0.0674(11) Uani 0.388(7) 1 d PD A 1 H20A H 0.4228 0.1657 0.0875 0.081 Uiso 0.388(7) 1 calc PR A 1 H20B H 0.4000 0.3015 0.1048 0.081 Uiso 0.388(7) 1 calc PR A 1 C202 C 0.3008(8) 0.1892(14) 0.0908(3) 0.080(2) Uani 0.388(7) 1 d PD A 1 H20C H 0.2899 0.2043 0.0647 0.096 Uiso 0.388(7) 1 calc PR A 1 H20D H 0.2638 0.2421 0.1041 0.096 Uiso 0.388(7) 1 calc PR A 1 C203 C 0.2968(13) 0.046(2) 0.1005(6) 0.120(4) Uani 0.388(7) 1 d PD A 1 H20E H 0.2409 0.0110 0.0971 0.144 Uiso 0.388(7) 1 calc PR A 1 H20F H 0.3338 -0.0074 0.0873 0.144 Uiso 0.388(7) 1 calc PR A 1 C204 C 0.3250(3) 0.0594(5) 0.13780(12) 0.0927(16) Uani 0.388(7) 1 d PD A 1 H20G H 0.2809 0.0912 0.1518 0.111 Uiso 0.388(7) 1 calc PR A 1 H20H H 0.3449 -0.0235 0.1480 0.111 Uiso 0.388(7) 1 calc PR A 1 C205 C 0.3862(2) 0.2092(4) 0.10324(10) 0.0674(11) Uani 0.612(7) 1 d PD A 2 H20I H 0.4417 0.2253 0.0963 0.081 Uiso 0.612(7) 1 calc PR A 2 H20J H 0.3568 0.2919 0.1033 0.081 Uiso 0.612(7) 1 calc PR A 2 C206 C 0.3414(5) 0.1154(9) 0.0772(2) 0.080(2) Uani 0.612(7) 1 d PD A 2 H20K H 0.3752 0.0404 0.0719 0.096 Uiso 0.612(7) 1 calc PR A 2 H20L H 0.3199 0.1570 0.0546 0.096 Uiso 0.612(7) 1 calc PR A 2 C207 C 0.2688(7) 0.0786(14) 0.1034(4) 0.120(4) Uani 0.612(7) 1 d PD A 2 H20M H 0.2298 0.1496 0.1055 0.144 Uiso 0.612(7) 1 calc PR A 2 H20N H 0.2394 -0.0008 0.0957 0.144 Uiso 0.612(7) 1 calc PR A 2 C208 C 0.3250(3) 0.0594(5) 0.13780(12) 0.0927(16) Uani 0.612(7) 1 d PD A 2 H20O H 0.2941 0.0719 0.1591 0.111 Uiso 0.612(7) 1 calc PR A 2 H20P H 0.3473 -0.0287 0.1386 0.111 Uiso 0.612(7) 1 calc PR A 2 O221 O 0.49211(18) 0.0454(2) 0.20804(6) 0.0715(8) Uani 1 1 d . . . C301 C 0.5289(3) 0.0642(4) 0.24393(10) 0.0843(14) Uani 0.657(8) 1 d PD A 1 H30A H 0.5051 0.1396 0.2552 0.101 Uiso 0.657(8) 1 calc PR A 1 H30B H 0.5882 0.0770 0.2439 0.101 Uiso 0.657(8) 1 calc PR A 1 C302 C 0.5105(5) -0.0568(7) 0.26333(17) 0.0536(16) Uani 0.657(8) 1 d PD A 1 H30C H 0.4630 -0.0447 0.2774 0.064 Uiso 0.657(8) 1 calc PR A 1 H30D H 0.5576 -0.0831 0.2798 0.064 Uiso 0.657(8) 1 calc PR A 1 C303 C 0.4924(7) -0.1566(7) 0.2341(2) 0.070(2) Uani 0.657(8) 1 d PD A 1 H30E H 0.5346 -0.2242 0.2358 0.084 Uiso 0.657(8) 1 calc PR A 1 H30F H 0.4389 -0.1970 0.2364 0.084 Uiso 0.657(8) 1 calc PR A 1 C304 C 0.4922(10) -0.0878(18) 0.1997(2) 0.094(4) Uani 0.657(8) 1 d PD A 1 H30G H 0.5410 -0.1103 0.1875 0.112 Uiso 0.657(8) 1 calc PR A 1 H30H H 0.4433 -0.1105 0.1838 0.112 Uiso 0.657(8) 1 calc PR A 1 C305 C 0.5289(3) 0.0642(4) 0.24393(10) 0.0843(14) Uani 0.343(8) 1 d PD A 2 H30I H 0.5759 0.1228 0.2433 0.101 Uiso 0.343(8) 1 calc PR A 2 H30J H 0.4890 0.1051 0.2586 0.101 Uiso 0.343(8) 1 calc PR A 2 C306 C 0.5542(10) -0.0481(15) 0.2594(4) 0.0536(16) Uani 0.343(8) 1 d PD A 2 H30K H 0.5221 -0.0704 0.2797 0.064 Uiso 0.343(8) 1 calc PR A 2 H30L H 0.6125 -0.0448 0.2680 0.064 Uiso 0.343(8) 1 calc PR A 2 C307 C 0.5388(12) -0.1424(16) 0.2286(5) 0.070(2) Uani 0.343(8) 1 d PD A 2 H30M H 0.5862 -0.1486 0.2142 0.084 Uiso 0.343(8) 1 calc PR A 2 H30N H 0.5254 -0.2288 0.2373 0.084 Uiso 0.343(8) 1 calc PR A 2 C308 C 0.473(2) -0.087(4) 0.2094(6) 0.094(4) Uani 0.343(8) 1 d PD A 2 H30O H 0.4229 -0.1005 0.2214 0.112 Uiso 0.343(8) 1 calc PR A 2 H30P H 0.4655 -0.1233 0.1849 0.112 Uiso 0.343(8) 1 calc PR A 2 O41 O 0.2133(3) 0.7878(4) 0.13329(14) 0.1325(16) Uani 1 1 d . . . C401 C 0.1474(6) 0.7390(10) 0.1127(2) 0.216(6) Uani 1 1 d . . . H40A H 0.1524 0.6450 0.1100 0.259 Uiso 1 1 calc R . . H40B H 0.1426 0.7787 0.0886 0.259 Uiso 1 1 calc R . . C402 C 0.0719(4) 0.7735(9) 0.13351(18) 0.169(4) Uani 1 1 d . . . H40C H 0.0546 0.8636 0.1295 0.203 Uiso 1 1 calc R . . H40D H 0.0254 0.7155 0.1271 0.203 Uiso 1 1 calc R . . C403 C 0.1072(3) 0.7523(5) 0.17014(15) 0.0978(16) Uani 1 1 d . . . H40E H 0.1080 0.6602 0.1765 0.117 Uiso 1 1 calc R . . H40F H 0.0780 0.8009 0.1877 0.117 Uiso 1 1 calc R . . C404 C 0.1930(3) 0.8046(6) 0.16749(15) 0.118(2) Uani 1 1 d . . . H40G H 0.1948 0.8969 0.1737 0.141 Uiso 1 1 calc R . . H40H H 0.2320 0.7586 0.1845 0.141 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 Li1 0.050(3) 0.040(3) 0.039(3) 0.001(3) -0.006(2) -0.006(2) Li2 0.052(3) 0.046(4) 0.051(3) -0.006(3) 0.000(3) -0.009(3) N1 0.0592(17) 0.0328(16) 0.0373(16) -0.0031(13) 0.0015(13) -0.0031(13) O1 0.0451(12) 0.0409(13) 0.0368(12) 0.0017(10) 0.0010(10) -0.0005(10) C1 0.0357(16) 0.0364(19) 0.0342(17) -0.0033(14) -0.0014(13) -0.0024(14) C2 0.0330(16) 0.042(2) 0.0385(18) -0.0025(15) -0.0034(14) -0.0044(14) C3 0.0381(17) 0.040(2) 0.0413(18) -0.0019(15) -0.0029(14) 0.0022(15) C4 0.0376(17) 0.047(2) 0.049(2) 0.0000(17) 0.0014(15) 0.0076(15) C5 0.0346(16) 0.051(2) 0.0410(19) 0.0033(17) -0.0027(14) 0.0021(16) C6 0.0351(17) 0.063(3) 0.048(2) 0.0033(19) 0.0039(15) 0.0028(16) C7 0.0359(18) 0.070(3) 0.049(2) 0.012(2) -0.0004(15) -0.0004(18) C8 0.050(2) 0.054(2) 0.049(2) 0.0107(18) -0.0011(17) -0.0096(18) C9 0.0459(18) 0.044(2) 0.0426(19) 0.0016(16) -0.0039(15) -0.0058(16) C10 0.0366(16) 0.045(2) 0.0383(18) -0.0008(16) -0.0044(14) -0.0050(15) C11 0.0432(17) 0.0321(18) 0.0344(17) 0.0014(14) 0.0019(14) -0.0083(14) C12 0.073(2) 0.040(2) 0.041(2) -0.0098(17) 0.0039(18) 0.0046(19) C13 0.073(2) 0.032(2) 0.052(2) -0.0068(17) 0.0047(19) 0.0083(18) C14 0.0500(19) 0.042(2) 0.047(2) 0.0013(17) 0.0069(16) 0.0008(16) C15 0.052(2) 0.059(3) 0.054(2) -0.0009(19) 0.0028(17) 0.0141(18) C16 0.053(2) 0.082(3) 0.051(2) 0.006(2) -0.0050(18) 0.013(2) C17 0.0427(19) 0.077(3) 0.045(2) -0.003(2) -0.0023(16) -0.0012(19) C18 0.0359(17) 0.053(2) 0.0391(19) -0.0066(16) 0.0019(14) -0.0001(15) C19 0.0406(17) 0.0337(19) 0.0398(18) 0.0023(15) 0.0059(14) -0.0042(14) C30 0.0475(19) 0.040(2) 0.058(2) 0.0040(17) 0.0009(16) 0.0057(16) C31 0.054(2) 0.040(2) 0.066(2) -0.0001(18) 0.0010(18) -0.0024(17) C32 0.048(2) 0.054(2) 0.064(2) 0.0131(19) -0.0120(17) 0.0068(17) C33 0.068(3) 0.050(3) 0.088(3) 0.007(2) 0.016(2) 0.017(2) C70 0.048(2) 0.085(3) 0.070(3) 0.027(2) 0.0058(19) -0.006(2) C71 0.064(3) 0.112(4) 0.076(3) 0.038(3) 0.020(2) 0.004(2) C72 0.062(3) 0.107(4) 0.090(3) 0.026(3) 0.012(2) -0.024(3) C73 0.054(2) 0.113(4) 0.086(3) 0.019(3) 0.029(2) 0.004(2) N11 0.0315(13) 0.0518(18) 0.0420(16) -0.0032(13) -0.0009(11) -0.0023(12) O11 0.0363(11) 0.0404(13) 0.0400(12) -0.0033(11) -0.0003(9) -0.0012(10) C101 0.0274(15) 0.0331(18) 0.0382(17) 0.0074(14) 0.0005(13) 0.0005(13) C102 0.0361(16) 0.0291(18) 0.0389(18) 0.0036(15) 0.0013(13) -0.0015(13) C103 0.0292(15) 0.042(2) 0.052(2) -0.0030(17) -0.0024(14) -0.0047(14) C104 0.0292(16) 0.045(2) 0.057(2) -0.0074(18) 0.0002(15) 0.0031(15) C105 0.0317(16) 0.0352(19) 0.0454(19) -0.0015(15) 0.0015(14) -0.0020(14) C106 0.0310(16) 0.040(2) 0.058(2) -0.0025(17) 0.0030(15) 0.0058(14) C107 0.0363(16) 0.0376(19) 0.0404(18) 0.0001(15) 0.0027(14) -0.0034(14) C108 0.0370(17) 0.0386(19) 0.0406(18) -0.0017(15) -0.0008(14) -0.0095(15) C109 0.0287(15) 0.0400(19) 0.0377(17) 0.0034(15) -0.0018(13) -0.0002(14) C110 0.0298(15) 0.0341(18) 0.0367(17) 0.0034(14) 0.0029(13) -0.0027(13) C111 0.0337(16) 0.0381(19) 0.0329(17) -0.0012(14) -0.0029(13) -0.0020(14) C112 0.0370(18) 0.080(3) 0.048(2) -0.016(2) 0.0035(16) 0.0014(18) C113 0.0392(18) 0.082(3) 0.055(2) -0.023(2) -0.0037(17) 0.0153(19) C114 0.0469(19) 0.046(2) 0.052(2) -0.0162(18) -0.0131(16) 0.0154(17) C115 0.071(2) 0.056(3) 0.058(3) -0.013(2) -0.022(2) 0.025(2) C116 0.087(3) 0.035(2) 0.069(3) 0.004(2) -0.038(2) 0.013(2) C117 0.078(3) 0.043(2) 0.044(2) 0.0049(17) -0.0160(18) -0.008(2) C118 0.0508(19) 0.0348(19) 0.0405(19) 0.0033(15) -0.0066(15) -0.0028(15) C119 0.0400(17) 0.0347(19) 0.0400(18) -0.0054(15) -0.0050(14) 0.0030(14) C130 0.0288(16) 0.064(3) 0.066(2) -0.017(2) -0.0043(15) -0.0062(16) C131 0.045(2) 0.064(3) 0.071(3) -0.007(2) -0.0230(18) 0.0012(18) C132 0.049(2) 0.065(3) 0.077(3) -0.013(2) 0.0053(19) -0.0203(19) C133 0.0311(19) 0.104(4) 0.114(4) -0.044(3) -0.008(2) -0.005(2) C170 0.0452(18) 0.049(2) 0.048(2) -0.0068(17) 0.0033(15) -0.0045(16) C171 0.055(2) 0.078(3) 0.067(3) -0.025(2) 0.0052(18) 0.010(2) C172 0.083(3) 0.076(3) 0.045(2) -0.004(2) 0.0056(19) 0.002(2) C173 0.070(2) 0.055(3) 0.063(2) -0.018(2) 0.0128(19) -0.014(2) O211 0.0619(15) 0.0647(18) 0.0558(16) -0.0016(14) -0.0037(12) -0.0231(13) C201 0.063(2) 0.074(3) 0.062(3) 0.010(2) -0.0146(19) 0.000(2) C202 0.084(5) 0.085(6) 0.067(5) -0.002(4) -0.018(4) -0.010(4) C203 0.071(9) 0.065(9) 0.208(8) 0.011(6) -0.068(7) 0.001(6) C204 0.109(4) 0.092(4) 0.074(3) -0.008(3) -0.006(3) -0.065(3) C205 0.063(2) 0.074(3) 0.062(3) 0.010(2) -0.0146(19) 0.000(2) C206 0.084(5) 0.085(6) 0.067(5) -0.002(4) -0.018(4) -0.010(4) C207 0.071(9) 0.065(9) 0.208(8) 0.011(6) -0.068(7) 0.001(6) C208 0.109(4) 0.092(4) 0.074(3) -0.008(3) -0.006(3) -0.065(3) O221 0.128(2) 0.0404(16) 0.0417(15) 0.0022(12) -0.0156(14) -0.0210(15) C301 0.140(4) 0.061(3) 0.047(2) 0.002(2) -0.022(2) -0.011(3) C302 0.069(5) 0.052(3) 0.040(3) 0.004(2) 0.010(4) -0.005(4) C303 0.124(8) 0.040(3) 0.048(4) 0.000(3) 0.009(5) -0.005(5) C304 0.217(10) 0.037(3) 0.024(6) 0.002(6) -0.011(6) -0.026(6) C305 0.140(4) 0.061(3) 0.047(2) 0.002(2) -0.022(2) -0.011(3) C306 0.069(5) 0.052(3) 0.040(3) 0.004(2) 0.010(4) -0.005(4) C307 0.124(8) 0.040(3) 0.048(4) 0.000(3) 0.009(5) -0.005(5) C308 0.217(10) 0.037(3) 0.024(6) 0.002(6) -0.011(6) -0.026(6) O41 0.137(4) 0.110(3) 0.164(4) -0.006(3) 0.087(3) -0.007(3) C401 0.231(9) 0.286(12) 0.149(7) -0.113(7) 0.117(7) -0.163(9) C402 0.137(6) 0.265(10) 0.111(5) -0.059(6) 0.044(4) -0.108(6) C403 0.111(4) 0.082(4) 0.108(4) -0.003(3) 0.051(3) -0.002(3) C404 0.100(4) 0.150(6) 0.112(4) 0.032(4) 0.060(3) 0.027(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Li1 O11 1.909(6) . ? Li1 O1 1.916(6) . ? Li1 N1 2.015(6) . ? Li1 N11 2.019(6) . ? Li1 Li2 2.525(8) . ? Li1 C2 2.662(6) . ? Li1 C102 2.680(6) . ? Li1 C11 2.783(6) . ? Li2 O1 1.877(6) . ? Li2 O11 1.882(6) . ? Li2 O211 1.965(6) . ? Li2 O221 1.993(7) . ? N1 C11 1.335(4) . ? N1 C12 1.376(4) . ? O1 C2 1.330(3) . ? C1 C2 1.411(4) . ? C1 C10 1.429(4) . ? C1 C11 1.491(4) . ? C2 C3 1.454(4) . ? C3 C4 1.372(4) . ? C3 C30 1.548(5) . ? C4 C5 1.429(5) . ? C4 H4 0.9500 . ? C5 C6 1.417(4) . ? C5 C10 1.421(4) . ? C6 C7 1.383(5) . ? C6 H6 0.9500 . ? C7 C8 1.408(5) . ? C7 C70 1.539(5) . ? C8 C9 1.376(4) . ? C8 H8 0.9500 . ? C9 C10 1.427(5) . ? C9 H9 0.9500 . ? C11 C19 1.438(4) . ? C12 C13 1.355(5) . ? C12 H12 0.9500 . ? C13 C14 1.406(4) . ? C13 H13 0.9500 . ? C14 C15 1.417(5) . ? C14 C19 1.431(4) . ? C15 C16 1.355(5) . ? C15 H15 0.9500 . ? C16 C17 1.417(5) . ? C16 H16 0.9500 . ? C17 C18 1.368(5) . ? C17 H17 0.9500 . ? C18 C19 1.403(4) . ? C18 H18 0.9500 . ? C30 C31 1.531(5) . ? C30 C32 1.540(5) . ? C30 C33 1.541(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C70 C71 1.514(5) . ? C70 C73 1.551(6) . ? C70 C72 1.555(6) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? N11 C111 1.330(4) . ? N11 C112 1.363(4) . ? O11 C102 1.313(3) . ? C101 C102 1.411(4) . ? C101 C110 1.433(4) . ? C101 C111 1.502(4) . ? C102 C103 1.462(4) . ? C103 C104 1.357(4) . ? C103 C130 1.554(4) . ? C104 C105 1.433(4) . ? C104 H104 0.9500 . ? C105 C106 1.415(4) . ? C105 C110 1.416(4) . ? C106 C107 1.388(4) . ? C106 H106 0.9500 . ? C107 C108 1.422(4) . ? C107 C170 1.522(4) . ? C108 C109 1.367(4) . ? C108 H108 0.9500 . ? C109 C110 1.424(4) . ? C109 H109 0.9500 . ? C111 C119 1.443(4) . ? C112 C113 1.353(5) . ? C112 H112 0.9500 . ? C113 C114 1.413(5) . ? C113 H113 0.9500 . ? C114 C115 1.416(5) . ? C114 C119 1.420(4) . ? C115 C116 1.344(5) . ? C115 H115 0.9500 . ? C116 C117 1.412(6) . ? C116 H116 0.9500 . ? C117 C118 1.370(4) . ? C117 H117 0.9500 . ? C118 C119 1.417(4) . ? C118 H118 0.9500 . ? C130 C131 1.528(5) . ? C130 C133 1.539(5) . ? C130 C132 1.548(5) . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C132 H13D 0.9800 . ? C132 H13E 0.9800 . ? C132 H13F 0.9800 . ? C133 H13G 0.9800 . ? C133 H13H 0.9800 . ? C133 H13I 0.9800 . ? C170 C171 1.532(5) . ? C170 C172 1.542(5) . ? C170 C173 1.546(5) . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C173 H17G 0.9800 . ? C173 H17H 0.9800 . ? C173 H17I 0.9800 . ? O211 C204 1.428(4) . ? O211 C201 1.439(4) . ? C201 C202 1.462(12) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 C203 1.54(3) . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.44(2) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C206 C207 1.661(19) . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? O221 C308 1.42(4) . ? O221 C304 1.424(19) . ? O221 C301 1.439(4) . ? C301 C302 1.501(8) . ? C301 H30A 0.9900 . ? C301 H30B 0.9900 . ? C302 C303 1.520(10) . ? C302 H30C 0.9900 . ? C302 H30D 0.9900 . ? C303 C304 1.474(12) . ? C303 H30E 0.9900 . ? C303 H30F 0.9900 . ? C304 H30G 0.9900 . ? C304 H30H 0.9900 . ? C306 C307 1.52(2) . ? C306 H30K 0.9900 . ? C306 H30L 0.9900 . ? C307 C308 1.38(2) . ? C307 H30M 0.9900 . ? C307 H30N 0.9900 . ? C308 H30O 0.9900 . ? C308 H30P 0.9900 . ? O41 C404 1.363(6) . ? O41 C401 1.375(8) . ? C401 C402 1.569(10) . ? C401 H40A 0.9900 . ? C401 H40B 0.9900 . ? C402 C403 1.460(8) . ? C402 H40C 0.9900 . ? C402 H40D 0.9900 . ? C403 C404 1.529(7) . ? C403 H40E 0.9900 . ? C403 H40F 0.9900 . ? C404 H40G 0.9900 . ? C404 H40H 0.9900 . ? 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 O11 Li1 O1 95.2(2) . . ? O11 Li1 N1 112.9(3) . . ? O1 Li1 N1 97.5(2) . . ? O11 Li1 N11 94.6(2) . . ? O1 Li1 N11 124.0(3) . . ? N1 Li1 N11 128.0(3) . . ? O11 Li1 Li2 47.78(19) . . ? O1 Li1 Li2 47.60(18) . . ? N1 Li1 Li2 115.6(3) . . ? N11 Li1 Li2 115.5(3) . . ? O11 Li1 C2 122.8(3) . . ? O1 Li1 C2 28.21(12) . . ? N1 Li1 C2 81.0(2) . . ? N11 Li1 C2 120.6(3) . . ? Li2 Li1 C2 75.6(2) . . ? O11 Li1 C102 27.17(12) . . ? O1 Li1 C102 122.4(3) . . ? N1 Li1 C102 105.9(2) . . ? N11 Li1 C102 78.86(19) . . ? Li2 Li1 C102 74.9(2) . . ? C2 Li1 C102 149.7(2) . . ? O11 Li1 C11 119.6(2) . . ? O1 Li1 C11 71.47(18) . . ? N1 Li1 C11 26.65(12) . . ? N11 Li1 C11 142.4(3) . . ? Li2 Li1 C11 99.9(2) . . ? C2 Li1 C11 54.92(14) . . ? C102 Li1 C11 124.7(2) . . ? O1 Li2 O11 97.5(3) . . ? O1 Li2 O211 103.2(3) . . ? O11 Li2 O211 126.0(3) . . ? O1 Li2 O221 125.9(3) . . ? O11 Li2 O221 99.3(3) . . ? O211 Li2 O221 107.3(3) . . ? O1 Li2 Li1 48.93(19) . . ? O11 Li2 Li1 48.69(19) . . ? O211 Li2 Li1 131.2(3) . . ? O221 Li2 Li1 121.6(3) . . ? C11 N1 C12 118.5(3) . . ? C11 N1 Li1 110.7(3) . . ? C12 N1 Li1 119.5(3) . . ? C2 O1 Li2 165.6(3) . . ? C2 O1 Li1 108.9(2) . . ? Li2 O1 Li1 83.5(2) . . ? C2 C1 C10 121.1(3) . . ? C2 C1 C11 119.9(3) . . ? C10 C1 C11 118.9(3) . . ? O1 C2 C1 120.1(3) . . ? O1 C2 C3 120.6(3) . . ? C1 C2 C3 119.3(3) . . ? C1 C2 Li1 88.2(2) . . ? C3 C2 Li1 139.7(2) . . ? C4 C3 C2 117.9(3) . . ? C4 C3 C30 121.6(3) . . ? C2 C3 C30 120.5(3) . . ? C3 C4 C5 123.8(3) . . ? C3 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C6 C5 C10 119.7(3) . . ? C6 C5 C4 122.0(3) . . ? C10 C5 C4 118.3(3) . . ? C7 C6 C5 122.6(3) . . ? C7 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? C6 C7 C8 117.0(3) . . ? C6 C7 C70 123.2(3) . . ? C8 C7 C70 119.7(4) . . ? C9 C8 C7 122.3(3) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? C8 C9 C10 121.2(3) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C5 C10 C9 117.1(3) . . ? C5 C10 C1 119.0(3) . . ? C9 C10 C1 123.9(3) . . ? N1 C11 C19 121.7(3) . . ? N1 C11 C1 117.3(3) . . ? C19 C11 C1 121.0(3) . . ? C19 C11 Li1 147.0(2) . . ? C1 C11 Li1 82.2(2) . . ? C13 C12 N1 124.0(3) . . ? C13 C12 H12 118.0 . . ? N1 C12 H12 118.0 . . ? C12 C13 C14 119.3(3) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 122.7(3) . . ? C13 C14 C19 118.3(3) . . ? C15 C14 C19 119.0(3) . . ? C16 C15 C14 120.7(3) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 120.5(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 121.2(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C14 118.6(3) . . ? C18 C19 C11 123.5(3) . . ? C14 C19 C11 118.0(3) . . ? C31 C30 C32 109.9(3) . . ? C31 C30 C33 107.4(3) . . ? C32 C30 C33 107.2(3) . . ? C31 C30 C3 110.2(3) . . ? C32 C30 C3 110.1(3) . . ? C33 C30 C3 111.9(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C71 C70 C7 110.2(3) . . ? C71 C70 C73 107.8(4) . . ? C7 C70 C73 111.8(3) . . ? C71 C70 C72 109.9(4) . . ? C7 C70 C72 108.0(3) . . ? C73 C70 C72 109.3(3) . . ? 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 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C111 N11 C112 119.3(3) . . ? C111 N11 Li1 114.3(2) . . ? C112 N11 Li1 116.7(3) . . ? C102 O11 Li2 164.6(3) . . ? C102 O11 Li1 111.2(2) . . ? Li2 O11 Li1 83.5(2) . . ? C102 C101 C110 121.2(3) . . ? C102 C101 C111 118.8(3) . . ? C110 C101 C111 119.9(2) . . ? O11 C102 C101 121.1(3) . . ? O11 C102 C103 120.5(3) . . ? C101 C102 C103 118.3(3) . . ? C101 C102 Li1 90.7(2) . . ? C103 C102 Li1 139.1(2) . . ? C104 C103 C102 119.0(3) . . ? C104 C103 C130 121.6(3) . . ? C102 C103 C130 119.4(3) . . ? C103 C104 C105 123.5(3) . . ? C103 C104 H104 118.3 . . ? C105 C104 H104 118.3 . . ? C106 C105 C110 120.3(3) . . ? C106 C105 C104 121.5(3) . . ? C110 C105 C104 118.2(3) . . ? C107 C106 C105 122.8(3) . . ? C107 C106 H106 118.6 . . ? C105 C106 H106 118.6 . . ? C106 C107 C108 116.0(3) . . ? C106 C107 C170 124.3(3) . . ? C108 C107 C170 119.7(3) . . ? C109 C108 C107 122.5(3) . . ? C109 C108 H108 118.7 . . ? C107 C108 H108 118.7 . . ? C108 C109 C110 121.7(3) . . ? C108 C109 H109 119.1 . . ? C110 C109 H109 119.1 . . ? C105 C110 C109 116.6(3) . . ? C105 C110 C101 119.3(3) . . ? C109 C110 C101 124.1(3) . . ? N11 C111 C119 121.2(3) . . ? N11 C111 C101 117.3(3) . . ? C119 C111 C101 121.4(3) . . ? C113 C112 N11 123.7(3) . . ? C113 C112 H112 118.1 . . ? N11 C112 H112 118.1 . . ? C112 C113 C114 119.4(3) . . ? C112 C113 H113 120.3 . . ? C114 C113 H113 120.3 . . ? C113 C114 C115 122.8(3) . . ? C113 C114 C119 118.1(3) . . ? C115 C114 C119 119.1(3) . . ? C116 C115 C114 121.1(4) . . ? C116 C115 H115 119.4 . . ? C114 C115 H115 119.4 . . ? C115 C116 C117 120.5(3) . . ? C115 C116 H116 119.8 . . ? C117 C116 H116 119.8 . . ? C118 C117 C116 120.2(4) . . ? C118 C117 H117 119.9 . . ? C116 C117 H117 119.9 . . ? C117 C118 C119 120.6(3) . . ? C117 C118 H118 119.7 . . ? C119 C118 H118 119.7 . . ? C118 C119 C114 118.3(3) . . ? C118 C119 C111 123.4(3) . . ? C114 C119 C111 118.2(3) . . ? C131 C130 C133 107.9(3) . . ? C131 C130 C132 110.6(3) . . ? C133 C130 C132 107.1(3) . . ? C131 C130 C103 111.9(3) . . ? C133 C130 C103 111.3(3) . . ? C132 C130 C103 108.0(3) . . ? C130 C131 H13A 109.5 . . ? C130 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C130 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C130 C132 H13D 109.5 . . ? C130 C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? C130 C132 H13F 109.5 . . ? H13D C132 H13F 109.5 . . ? H13E C132 H13F 109.5 . . ? C130 C133 H13G 109.5 . . ? C130 C133 H13H 109.5 . . ? H13G C133 H13H 109.5 . . ? C130 C133 H13I 109.5 . . ? H13G C133 H13I 109.5 . . ? H13H C133 H13I 109.5 . . ? C107 C170 C171 112.8(3) . . ? C107 C170 C172 109.0(3) . . ? C171 C170 C172 108.2(3) . . ? C107 C170 C173 110.2(3) . . ? C171 C170 C173 107.6(3) . . ? C172 C170 C173 108.9(3) . . ? C170 C171 H17A 109.5 . . ? C170 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C170 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C170 C172 H17D 109.5 . . ? C170 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C170 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C170 C173 H17G 109.5 . . ? C170 C173 H17H 109.5 . . ? H17G C173 H17H 109.5 . . ? C170 C173 H17I 109.5 . . ? H17G C173 H17I 109.5 . . ? H17H C173 H17I 109.5 . . ? C204 O211 C201 107.8(3) . . ? C204 O211 Li2 132.4(3) . . ? C201 O211 Li2 119.5(3) . . ? O211 C201 C202 100.9(6) . . ? O211 C201 H20A 111.6 . . ? C202 C201 H20A 111.6 . . ? O211 C201 H20B 111.6 . . ? C202 C201 H20B 111.6 . . ? H20A C201 H20B 109.4 . . ? C201 C202 C203 97.0(10) . . ? C201 C202 H20C 112.4 . . ? C203 C202 H20C 112.4 . . ? C201 C202 H20D 112.4 . . ? C203 C202 H20D 112.4 . . ? H20C C202 H20D 109.9 . . ? C204 C203 C202 96.7(14) . . ? C204 C203 H20E 112.4 . . ? C202 C203 H20E 112.4 . . ? C204 C203 H20F 112.4 . . ? C202 C203 H20F 112.4 . . ? H20E C203 H20F 110.0 . . ? O211 C204 C203 104.6(12) . . ? O211 C204 H20G 110.8 . . ? C203 C204 H20G 110.8 . . ? O211 C204 H20H 110.8 . . ? C203 C204 H20H 110.8 . . ? H20G C204 H20H 108.9 . . ? C207 C206 H20K 112.5 . . ? C207 C206 H20L 112.5 . . ? H20K C206 H20L 110.1 . . ? C206 C207 H20M 112.5 . . ? C206 C207 H20N 112.5 . . ? H20M C207 H20N 110.0 . . ? C308 O221 C301 100.2(9) . . ? C304 O221 C301 109.2(5) . . ? C308 O221 Li2 139.5(9) . . ? C304 O221 Li2 127.7(4) . . ? C301 O221 Li2 120.3(3) . . ? O221 C301 C302 104.5(4) . . ? O221 C301 H30A 110.9 . . ? C302 C301 H30A 110.9 . . ? O221 C301 H30B 110.9 . . ? C302 C301 H30B 110.9 . . ? H30A C301 H30B 108.9 . . ? C301 C302 C303 105.3(5) . . ? C301 C302 H30C 110.7 . . ? C303 C302 H30C 110.7 . . ? C301 C302 H30D 110.7 . . ? C303 C302 H30D 110.7 . . ? H30C C302 H30D 108.8 . . ? C304 C303 C302 106.3(8) . . ? C304 C303 H30E 110.5 . . ? C302 C303 H30E 110.5 . . ? C304 C303 H30F 110.5 . . ? C302 C303 H30F 110.5 . . ? H30E C303 H30F 108.7 . . ? O221 C304 C303 106.5(8) . . ? O221 C304 H30G 110.4 . . ? C303 C304 H30G 110.4 . . ? O221 C304 H30H 110.4 . . ? C303 C304 H30H 110.4 . . ? H30G C304 H30H 108.6 . . ? C307 C306 H30K 111.3 . . ? C307 C306 H30L 111.3 . . ? H30K C306 H30L 109.2 . . ? C308 C307 C306 101.3(15) . . ? C308 C307 H30M 111.5 . . ? C306 C307 H30M 111.5 . . ? C308 C307 H30N 111.5 . . ? C306 C307 H30N 111.5 . . ? H30M C307 H30N 109.3 . . ? C307 C308 O221 105(2) . . ? C307 C308 H30O 110.7 . . ? O221 C308 H30O 110.7 . . ? C307 C308 H30P 110.7 . . ? O221 C308 H30P 110.7 . . ? H30O C308 H30P 108.8 . . ? C404 O41 C401 109.1(5) . . ? O41 C401 C402 105.2(5) . . ? O41 C401 H40A 110.7 . . ? C402 C401 H40A 110.7 . . ? O41 C401 H40B 110.7 . . ? C402 C401 H40B 110.7 . . ? H40A C401 H40B 108.8 . . ? C403 C402 C401 99.3(7) . . ? C403 C402 H40C 111.9 . . ? C401 C402 H40C 111.9 . . ? C403 C402 H40D 111.9 . . ? C401 C402 H40D 111.9 . . ? H40C C402 H40D 109.6 . . ? C402 C403 C404 100.5(4) . . ? C402 C403 H40E 111.7 . . ? C404 C403 H40E 111.7 . . ? C402 C403 H40F 111.7 . . ? C404 C403 H40F 111.7 . . ? H40E C403 H40F 109.4 . . ? O41 C404 C403 108.7(5) . . ? O41 C404 H40G 110.0 . . ? C403 C404 H40G 110.0 . . ? O41 C404 H40H 110.0 . . ? C403 C404 H40H 110.0 . . ? H40G C404 H40H 108.3 . . ? 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 O11 Li1 Li2 O1 174.6(3) . . . . ? N1 Li1 Li2 O1 76.1(3) . . . . ? N11 Li1 Li2 O1 -113.7(3) . . . . ? C2 Li1 Li2 O1 3.68(14) . . . . ? C102 Li1 Li2 O1 176.8(3) . . . . ? C11 Li1 Li2 O1 53.4(2) . . . . ? O1 Li1 Li2 O11 -174.6(3) . . . . ? N1 Li1 Li2 O11 -98.5(3) . . . . ? N11 Li1 Li2 O11 71.7(3) . . . . ? C2 Li1 Li2 O11 -170.9(3) . . . . ? C102 Li1 Li2 O11 2.22(13) . . . . ? C11 Li1 Li2 O11 -121.2(3) . . . . ? O11 Li1 Li2 O211 105.7(4) . . . . ? O1 Li1 Li2 O211 -68.9(4) . . . . ? N1 Li1 Li2 O211 7.2(5) . . . . ? N11 Li1 Li2 O211 177.4(3) . . . . ? C2 Li1 Li2 O211 -65.2(4) . . . . ? C102 Li1 Li2 O211 107.9(4) . . . . ? C11 Li1 Li2 O211 -15.6(5) . . . . ? O11 Li1 Li2 O221 -73.3(3) . . . . ? O1 Li1 Li2 O221 112.1(4) . . . . ? N1 Li1 Li2 O221 -171.8(3) . . . . ? N11 Li1 Li2 O221 -1.6(5) . . . . ? C2 Li1 Li2 O221 115.8(3) . . . . ? C102 Li1 Li2 O221 -71.1(3) . . . . ? C11 Li1 Li2 O221 165.5(3) . . . . ? O11 Li1 N1 C11 -110.8(3) . . . . ? O1 Li1 N1 C11 -11.9(3) . . . . ? N11 Li1 N1 C11 133.1(3) . . . . ? Li2 Li1 N1 C11 -58.2(4) . . . . ? C2 Li1 N1 C11 11.1(2) . . . . ? C102 Li1 N1 C11 -138.7(2) . . . . ? O11 Li1 N1 C12 32.4(4) . . . . ? O1 Li1 N1 C12 131.4(3) . . . . ? N11 Li1 N1 C12 -83.6(4) . . . . ? Li2 Li1 N1 C12 85.1(4) . . . . ? C2 Li1 N1 C12 154.3(3) . . . . ? C102 Li1 N1 C12 4.5(4) . . . . ? C11 Li1 N1 C12 143.3(4) . . . . ? O11 Li2 O1 C2 -145.7(10) . . . . ? O211 Li2 O1 C2 -16.0(13) . . . . ? O221 Li2 O1 C2 107.0(11) . . . . ? Li1 Li2 O1 C2 -149.8(11) . . . . ? O11 Li2 O1 Li1 4.1(3) . . . . ? O211 Li2 O1 Li1 133.8(3) . . . . ? O221 Li2 O1 Li1 -103.1(4) . . . . ? O11 Li1 O1 C2 168.4(2) . . . . ? N1 Li1 O1 C2 54.5(3) . . . . ? N11 Li1 O1 C2 -92.5(4) . . . . ? Li2 Li1 O1 C2 172.4(3) . . . . ? C102 Li1 O1 C2 168.8(3) . . . . ? C11 Li1 O1 C2 48.9(2) . . . . ? O11 Li1 O1 Li2 -4.0(3) . . . . ? N1 Li1 O1 Li2 -118.0(3) . . . . ? N11 Li1 O1 Li2 95.1(4) . . . . ? C2 Li1 O1 Li2 -172.4(3) . . . . ? C102 Li1 O1 Li2 -3.7(3) . . . . ? C11 Li1 O1 Li2 -123.5(2) . . . . ? Li2 O1 C2 C1 100.8(11) . . . . ? Li1 O1 C2 C1 -47.4(3) . . . . ? Li2 O1 C2 C3 -80.1(12) . . . . ? Li1 O1 C2 C3 131.7(3) . . . . ? Li2 O1 C2 Li1 148.2(12) . . . . ? C10 C1 C2 O1 169.6(3) . . . . ? C11 C1 C2 O1 -9.5(4) . . . . ? C10 C1 C2 C3 -9.5(4) . . . . ? C11 C1 C2 C3 171.4(3) . . . . ? C10 C1 C2 Li1 139.5(3) . . . . ? C11 C1 C2 Li1 -39.6(3) . . . . ? O11 Li1 C2 O1 -13.8(3) . . . . ? N1 Li1 C2 O1 -125.2(3) . . . . ? N11 Li1 C2 O1 105.6(4) . . . . ? Li2 Li1 C2 O1 -5.8(2) . . . . ? C102 Li1 C2 O1 -19.0(4) . . . . ? C11 Li1 C2 O1 -119.2(3) . . . . ? O11 Li1 C2 C1 126.6(3) . . . . ? O1 Li1 C2 C1 140.4(3) . . . . ? N1 Li1 C2 C1 15.2(2) . . . . ? N11 Li1 C2 C1 -113.9(3) . . . . ? Li2 Li1 C2 C1 134.7(2) . . . . ? C102 Li1 C2 C1 121.4(5) . . . . ? C11 Li1 C2 C1 21.23(16) . . . . ? O11 Li1 C2 C3 -97.4(4) . . . . ? O1 Li1 C2 C3 -83.6(4) . . . . ? N1 Li1 C2 C3 151.2(4) . . . . ? N11 Li1 C2 C3 22.0(5) . . . . ? Li2 Li1 C2 C3 -89.4(4) . . . . ? C102 Li1 C2 C3 -102.6(5) . . . . ? C11 Li1 C2 C3 157.2(4) . . . . ? O1 C2 C3 C4 -172.3(3) . . . . ? C1 C2 C3 C4 6.8(4) . . . . ? Li1 C2 C3 C4 -120.4(4) . . . . ? O1 C2 C3 C30 7.4(4) . . . . ? C1 C2 C3 C30 -173.5(3) . . . . ? Li1 C2 C3 C30 59.3(5) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? C30 C3 C4 C5 179.9(3) . . . . ? C3 C4 C5 C6 176.4(3) . . . . ? C3 C4 C5 C10 -3.4(5) . . . . ? C10 C5 C6 C7 1.8(5) . . . . ? C4 C5 C6 C7 -178.0(3) . . . . ? C5 C6 C7 C8 0.4(5) . . . . ? C5 C6 C7 C70 179.1(3) . . . . ? C6 C7 C8 C9 -2.2(5) . . . . ? C70 C7 C8 C9 179.1(3) . . . . ? C7 C8 C9 C10 1.8(5) . . . . ? C6 C5 C10 C9 -2.2(4) . . . . ? C4 C5 C10 C9 177.6(3) . . . . ? C6 C5 C10 C1 -178.9(3) . . . . ? C4 C5 C10 C1 0.9(4) . . . . ? C8 C9 C10 C5 0.5(4) . . . . ? C8 C9 C10 C1 177.0(3) . . . . ? C2 C1 C10 C5 5.5(4) . . . . ? C11 C1 C10 C5 -175.3(3) . . . . ? C2 C1 C10 C9 -171.0(3) . . . . ? C11 C1 C10 C9 8.2(4) . . . . ? C12 N1 C11 C19 -2.0(4) . . . . ? Li1 N1 C11 C19 141.6(3) . . . . ? C12 N1 C11 C1 178.2(3) . . . . ? Li1 N1 C11 C1 -38.1(3) . . . . ? C12 N1 C11 Li1 -143.7(4) . . . . ? C2 C1 C11 N1 63.0(4) . . . . ? C10 C1 C11 N1 -116.2(3) . . . . ? C2 C1 C11 C19 -116.8(3) . . . . ? C10 C1 C11 C19 64.0(4) . . . . ? C2 C1 C11 Li1 38.0(3) . . . . ? C10 C1 C11 Li1 -141.2(3) . . . . ? O11 Li1 C11 N1 82.2(3) . . . . ? O1 Li1 C11 N1 167.6(3) . . . . ? N11 Li1 C11 N1 -70.4(5) . . . . ? Li2 Li1 C11 N1 128.9(3) . . . . ? C2 Li1 C11 N1 -166.6(3) . . . . ? C102 Li1 C11 N1 50.5(3) . . . . ? O11 Li1 C11 C19 6.5(6) . . . . ? O1 Li1 C11 C19 91.9(5) . . . . ? N1 Li1 C11 C19 -75.7(5) . . . . ? N11 Li1 C11 C19 -146.1(5) . . . . ? Li2 Li1 C11 C19 53.2(5) . . . . ? C2 Li1 C11 C19 117.7(4) . . . . ? C102 Li1 C11 C19 -25.2(6) . . . . ? O11 Li1 C11 C1 -131.4(3) . . . . ? O1 Li1 C11 C1 -46.0(2) . . . . ? N1 Li1 C11 C1 146.4(3) . . . . ? N11 Li1 C11 C1 76.0(5) . . . . ? Li2 Li1 C11 C1 -84.7(3) . . . . ? C2 Li1 C11 C1 -20.22(16) . . . . ? C102 Li1 C11 C1 -163.1(3) . . . . ? C11 N1 C12 C13 -2.0(5) . . . . ? Li1 N1 C12 C13 -142.5(4) . . . . ? N1 C12 C13 C14 3.6(6) . . . . ? C12 C13 C14 C15 176.5(4) . . . . ? C12 C13 C14 C19 -1.2(5) . . . . ? C13 C14 C15 C16 -176.3(3) . . . . ? C19 C14 C15 C16 1.3(5) . . . . ? C14 C15 C16 C17 0.9(6) . . . . ? C15 C16 C17 C18 -1.9(6) . . . . ? C16 C17 C18 C19 0.6(5) . . . . ? C17 C18 C19 C14 1.6(5) . . . . ? C17 C18 C19 C11 179.2(3) . . . . ? C13 C14 C19 C18 175.2(3) . . . . ? C15 C14 C19 C18 -2.5(5) . . . . ? C13 C14 C19 C11 -2.6(4) . . . . ? C15 C14 C19 C11 179.7(3) . . . . ? N1 C11 C19 C18 -173.4(3) . . . . ? C1 C11 C19 C18 6.4(5) . . . . ? Li1 C11 C19 C18 -122.9(4) . . . . ? N1 C11 C19 C14 4.3(4) . . . . ? C1 C11 C19 C14 -176.0(3) . . . . ? Li1 C11 C19 C14 54.8(6) . . . . ? C4 C3 C30 C31 -120.1(3) . . . . ? C2 C3 C30 C31 60.2(4) . . . . ? C4 C3 C30 C32 118.4(3) . . . . ? C2 C3 C30 C32 -61.3(4) . . . . ? C4 C3 C30 C33 -0.7(4) . . . . ? C2 C3 C30 C33 179.6(3) . . . . ? C6 C7 C70 C71 130.6(4) . . . . ? C8 C7 C70 C71 -50.8(5) . . . . ? C6 C7 C70 C73 10.8(5) . . . . ? C8 C7 C70 C73 -170.6(3) . . . . ? C6 C7 C70 C72 -109.5(4) . . . . ? C8 C7 C70 C72 69.2(4) . . . . ? O11 Li1 N11 C111 -13.0(4) . . . . ? O1 Li1 N11 C111 -112.4(4) . . . . ? N1 Li1 N11 C111 110.9(4) . . . . ? Li2 Li1 N11 C111 -57.8(4) . . . . ? C2 Li1 N11 C111 -145.7(3) . . . . ? C102 Li1 N11 C111 9.3(3) . . . . ? C11 Li1 N11 C111 143.3(4) . . . . ? O11 Li1 N11 C112 133.1(3) . . . . ? O1 Li1 N11 C112 33.7(5) . . . . ? N1 Li1 N11 C112 -103.0(4) . . . . ? Li2 Li1 N11 C112 88.3(4) . . . . ? C2 Li1 N11 C112 0.4(4) . . . . ? C102 Li1 N11 C112 155.4(3) . . . . ? C11 Li1 N11 C112 -70.6(5) . . . . ? O1 Li2 O11 C102 -167.4(8) . . . . ? O211 Li2 O11 C102 80.3(11) . . . . ? O221 Li2 O11 C102 -39.1(11) . . . . ? Li1 Li2 O11 C102 -163.3(10) . . . . ? O1 Li2 O11 Li1 -4.1(3) . . . . ? O211 Li2 O11 Li1 -116.4(4) . . . . ? O221 Li2 O11 Li1 124.2(3) . . . . ? O1 Li1 O11 C102 179.3(2) . . . . ? N1 Li1 O11 C102 -80.2(3) . . . . ? N11 Li1 O11 C102 54.6(3) . . . . ? Li2 Li1 O11 C102 175.3(3) . . . . ? C2 Li1 O11 C102 -174.2(3) . . . . ? C11 Li1 O11 C102 -109.0(3) . . . . ? O1 Li1 O11 Li2 4.0(3) . . . . ? N1 Li1 O11 Li2 104.5(3) . . . . ? N11 Li1 O11 Li2 -120.7(3) . . . . ? C2 Li1 O11 Li2 10.5(3) . . . . ? C102 Li1 O11 Li2 -175.3(3) . . . . ? C11 Li1 O11 Li2 75.6(3) . . . . ? Li2 O11 C102 C101 113.4(9) . . . . ? Li1 O11 C102 C101 -48.8(4) . . . . ? Li2 O11 C102 C103 -66.7(10) . . . . ? Li1 O11 C102 C103 131.1(3) . . . . ? Li2 O11 C102 Li1 162.2(10) . . . . ? C110 C101 C102 O11 171.9(3) . . . . ? C111 C101 C102 O11 -8.0(4) . . . . ? C110 C101 C102 C103 -8.0(4) . . . . ? C111 C101 C102 C103 172.1(3) . . . . ? C110 C101 C102 Li1 141.9(3) . . . . ? C111 C101 C102 Li1 -38.0(3) . . . . ? O1 Li1 C102 O11 -0.8(3) . . . . ? N1 Li1 C102 O11 109.2(3) . . . . ? N11 Li1 C102 O11 -124.1(3) . . . . ? Li2 Li1 C102 O11 -3.6(2) . . . . ? C2 Li1 C102 O11 9.7(4) . . . . ? C11 Li1 C102 O11 88.1(3) . . . . ? O11 Li1 C102 C101 139.9(3) . . . . ? O1 Li1 C102 C101 139.1(3) . . . . ? N1 Li1 C102 C101 -110.9(3) . . . . ? N11 Li1 C102 C101 15.8(2) . . . . ? Li2 Li1 C102 C101 136.3(2) . . . . ? C2 Li1 C102 C101 149.6(5) . . . . ? C11 Li1 C102 C101 -132.0(3) . . . . ? O11 Li1 C102 C103 -82.5(4) . . . . ? O1 Li1 C102 C103 -83.3(5) . . . . ? N1 Li1 C102 C103 26.8(5) . . . . ? N11 Li1 C102 C103 153.4(3) . . . . ? Li2 Li1 C102 C103 -86.1(4) . . . . ? C2 Li1 C102 C103 -72.8(6) . . . . ? C11 Li1 C102 C103 5.7(5) . . . . ? O11 C102 C103 C104 -172.8(3) . . . . ? C101 C102 C103 C104 7.1(4) . . . . ? Li1 C102 C103 C104 -123.0(4) . . . . ? O11 C102 C103 C130 8.9(4) . . . . ? C101 C102 C103 C130 -171.2(3) . . . . ? Li1 C102 C103 C130 58.8(5) . . . . ? C102 C103 C104 C105 -2.5(5) . . . . ? C130 C103 C104 C105 175.7(3) . . . . ? C103 C104 C105 C106 -179.8(3) . . . . ? C103 C104 C105 C110 -1.3(5) . . . . ? C110 C105 C106 C107 0.9(5) . . . . ? C104 C105 C106 C107 179.3(3) . . . . ? C105 C106 C107 C108 1.1(5) . . . . ? C105 C106 C107 C170 -177.1(3) . . . . ? C106 C107 C108 C109 -1.7(5) . . . . ? C170 C107 C108 C109 176.6(3) . . . . ? C107 C108 C109 C110 0.4(5) . . . . ? C106 C105 C110 C109 -2.2(4) . . . . ? C104 C105 C110 C109 179.3(3) . . . . ? C106 C105 C110 C101 179.0(3) . . . . ? C104 C105 C110 C101 0.6(4) . . . . ? C108 C109 C110 C105 1.6(4) . . . . ? C108 C109 C110 C101 -179.7(3) . . . . ? C102 C101 C110 C105 4.2(4) . . . . ? C111 C101 C110 C105 -175.8(3) . . . . ? C102 C101 C110 C109 -174.5(3) . . . . ? C111 C101 C110 C109 5.5(4) . . . . ? C112 N11 C111 C119 -2.3(5) . . . . ? Li1 N11 C111 C119 142.9(3) . . . . ? C112 N11 C111 C101 179.9(3) . . . . ? Li1 N11 C111 C101 -34.9(4) . . . . ? C102 C101 C111 N11 57.8(4) . . . . ? C110 C101 C111 N11 -122.1(3) . . . . ? C102 C101 C111 C119 -120.0(3) . . . . ? C110 C101 C111 C119 60.1(4) . . . . ? C111 N11 C112 C113 0.2(5) . . . . ? Li1 N11 C112 C113 -144.1(4) . . . . ? N11 C112 C113 C114 1.8(6) . . . . ? C112 C113 C114 C115 178.5(4) . . . . ? C112 C113 C114 C119 -1.6(5) . . . . ? C113 C114 C115 C116 -177.2(4) . . . . ? C119 C114 C115 C116 2.9(6) . . . . ? C114 C115 C116 C117 -1.3(6) . . . . ? C115 C116 C117 C118 -0.4(6) . . . . ? C116 C117 C118 C119 0.4(5) . . . . ? C117 C118 C119 C114 1.2(5) . . . . ? C117 C118 C119 C111 178.7(3) . . . . ? C113 C114 C119 C118 177.3(3) . . . . ? C115 C114 C119 C118 -2.8(5) . . . . ? C113 C114 C119 C111 -0.3(5) . . . . ? C115 C114 C119 C111 179.6(3) . . . . ? N11 C111 C119 C118 -175.2(3) . . . . ? C101 C111 C119 C118 2.5(5) . . . . ? N11 C111 C119 C114 2.3(4) . . . . ? C101 C111 C119 C114 -180.0(3) . . . . ? C104 C103 C130 C131 117.5(4) . . . . ? C102 C103 C130 C131 -64.3(4) . . . . ? C104 C103 C130 C133 -3.3(5) . . . . ? C102 C103 C130 C133 175.0(3) . . . . ? C104 C103 C130 C132 -120.6(3) . . . . ? C102 C103 C130 C132 57.6(4) . . . . ? C106 C107 C170 C171 -7.3(5) . . . . ? C108 C107 C170 C171 174.6(3) . . . . ? C106 C107 C170 C172 112.9(4) . . . . ? C108 C107 C170 C172 -65.2(4) . . . . ? C106 C107 C170 C173 -127.7(4) . . . . ? C108 C107 C170 C173 54.2(4) . . . . ? O1 Li2 O211 C204 152.4(4) . . . . ? O11 Li2 O211 C204 -98.1(5) . . . . ? O221 Li2 O211 C204 17.7(6) . . . . ? Li1 Li2 O211 C204 -161.4(4) . . . . ? O1 Li2 O211 C201 -20.7(4) . . . . ? O11 Li2 O211 C201 88.9(4) . . . . ? O221 Li2 O211 C201 -155.4(3) . . . . ? Li1 Li2 O211 C201 25.5(5) . . . . ? C204 O211 C201 C202 23.9(7) . . . . ? Li2 O211 C201 C202 -161.4(7) . . . . ? O211 C201 C202 C203 -48.1(13) . . . . ? C201 C202 C203 C204 55.4(15) . . . . ? C201 O211 C204 C203 12.7(10) . . . . ? Li2 O211 C204 C203 -161.0(10) . . . . ? C202 C203 C204 O211 -41.5(14) . . . . ? O1 Li2 O221 C308 -99(2) . . . . ? O11 Li2 O221 C308 155(2) . . . . ? O211 Li2 O221 C308 22(2) . . . . ? Li1 Li2 O221 C308 -158(2) . . . . ? O1 Li2 O221 C304 -76.0(9) . . . . ? O11 Li2 O221 C304 177.7(9) . . . . ? O211 Li2 O221 C304 45.3(9) . . . . ? Li1 Li2 O221 C304 -135.5(9) . . . . ? O1 Li2 O221 C301 83.1(5) . . . . ? O11 Li2 O221 C301 -23.3(4) . . . . ? O211 Li2 O221 C301 -155.6(3) . . . . ? Li1 Li2 O221 C301 23.6(5) . . . . ? C308 O221 C301 C302 -11.1(14) . . . . ? C304 O221 C301 C302 -29.8(9) . . . . ? Li2 O221 C301 C302 167.6(4) . . . . ? O221 C301 C302 C303 21.1(6) . . . . ? C301 C302 C303 C304 -5.9(10) . . . . ? C308 O221 C304 C303 -40(3) . . . . ? C301 O221 C304 C303 26.3(13) . . . . ? Li2 O221 C304 C303 -172.7(6) . . . . ? C302 C303 C304 O221 -11.7(13) . . . . ? C306 C307 C308 O221 44(2) . . . . ? C304 O221 C308 C307 78(5) . . . . ? C301 O221 C308 C307 -40(2) . . . . ? Li2 O221 C308 C307 141.7(11) . . . . ? C404 O41 C401 C402 20.8(9) . . . . ? O41 C401 C402 C403 -38.5(9) . . . . ? C401 C402 C403 C404 38.3(7) . . . . ? C401 O41 C404 C403 4.6(8) . . . . ? C402 C403 C404 O41 -29.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.339 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.060 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 0.004 0.000 0.000 404.3 -9.5 2 0.962 0.500 0.500 404.3 -9.5 _platon_squeeze_details ; ; #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 728915' _chemical_formula_structural '[Pd(acac{L(H)}]' _chemical_formula_moiety 'C32 H35 N O3 Pd' _chemical_formula_sum 'C32 H35 N O3 Pd' _chemical_formula_weight 588.01 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2647(13) _cell_length_b 26.934(3) _cell_length_c 11.8122(14) _cell_angle_alpha 90.00 _cell_angle_beta 112.275(11) _cell_angle_gamma 90.00 _cell_volume 3316.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 4201 _cell_measurement_theta_min 3.5974 _cell_measurement_theta_max 27.4985 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.568 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details '(ABSPACK; Oxford Diffraction, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35477 _diffrn_reflns_av_R_equivalents 0.2114 _diffrn_reflns_av_sigmaI/netI 0.2998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 27.58 _reflns_number_total 7552 _reflns_number_gt 3004 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004) ; _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^)+(0.0674P)^2^] 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_number_reflns 7552 _refine_ls_number_parameters 355 _refine_ls_number_restraints 464 _refine_ls_R_factor_all 0.2249 _refine_ls_R_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1538 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.911 _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 Pd1 Pd 0.71484(6) 0.07914(3) 0.22357(6) 0.0281(2) Uani 1 1 d U . . N1 N 0.5833(5) 0.0770(3) 0.0527(5) 0.0272(15) Uani 1 1 d U . . O1 O 0.8386(5) 0.0496(2) 0.1604(5) 0.0275(13) Uani 1 1 d U . . O21 O 0.8541(5) 0.0756(3) 0.3896(4) 0.0383(15) Uani 1 1 d U . . O22 O 0.5875(5) 0.1085(2) 0.2841(5) 0.0341(15) Uani 1 1 d U . . C1 C 0.7522(8) 0.0955(3) -0.0237(7) 0.0193(16) Uani 1 1 d U . . C2 C 0.8558(7) 0.0772(3) 0.0735(6) 0.0229(16) Uani 1 1 d U . . C3 C 0.9844(7) 0.0873(3) 0.0817(6) 0.0188(16) Uani 1 1 d U . . C4 C 0.9996(8) 0.1182(3) -0.0020(7) 0.0287(19) Uani 1 1 d U . . H4 H 1.0838 0.1231 -0.0001 0.034 Uiso 1 1 calc R . . C5 C 0.8988(9) 0.1433(3) -0.0907(7) 0.0289(18) Uani 1 1 d U . . C6 C 0.9239(10) 0.1814(3) -0.1634(7) 0.040(2) Uani 1 1 d U A . H6 H 1.0095 0.1874 -0.1566 0.048 Uiso 1 1 calc R . . C7 C 0.8248(11) 0.2095(3) -0.2436(8) 0.045(2) Uani 1 1 d U . . C8 C 0.6977(10) 0.1982(3) -0.2540(7) 0.043(2) Uani 1 1 d U A . H8 H 0.6288 0.2169 -0.3096 0.052 Uiso 1 1 calc R . . C9 C 0.6706(9) 0.1620(3) -0.1883(7) 0.034(2) Uani 1 1 d U . . H9 H 0.5842 0.1561 -0.1975 0.041 Uiso 1 1 calc R A . C10 C 0.7702(8) 0.1329(3) -0.1062(7) 0.0274(18) Uani 1 1 d U A . C11 C 0.6211(7) 0.0780(3) -0.0448(6) 0.0245(17) Uani 1 1 d U . . C12 C 0.4589(7) 0.0631(3) 0.0341(8) 0.033(2) Uani 1 1 d U . . H12 H 0.4357 0.0620 0.1034 0.040 Uiso 1 1 calc R . . C13 C 0.3689(8) 0.0510(3) -0.0749(8) 0.040(2) Uani 1 1 d U . . H13 H 0.2833 0.0442 -0.0829 0.048 Uiso 1 1 calc R . . C14 C 0.4043(8) 0.0487(3) -0.1775(8) 0.0319(19) Uani 1 1 d U . . C15 C 0.3199(8) 0.0321(3) -0.2926(8) 0.035(2) Uani 1 1 d U . . H15 H 0.2341 0.0239 -0.3043 0.042 Uiso 1 1 calc R . . C16 C 0.3595(8) 0.0278(3) -0.3872(8) 0.037(2) Uani 1 1 d U . . H16 H 0.3007 0.0169 -0.4646 0.044 Uiso 1 1 calc R . . C17 C 0.4871(9) 0.0391(3) -0.3720(8) 0.037(2) Uani 1 1 d U . . H17 H 0.5130 0.0355 -0.4394 0.044 Uiso 1 1 calc R . . C18 C 0.5743(8) 0.0554(3) -0.2617(7) 0.0301(19) Uani 1 1 d U . . H18 H 0.6605 0.0621 -0.2517 0.036 Uiso 1 1 calc R . . C19 C 0.5336(8) 0.0621(3) -0.1626(7) 0.0282(19) Uani 1 1 d U . . C20 C 0.9614(8) 0.0871(4) 0.6011(7) 0.051(3) Uani 1 1 d U . . H20A H 0.9857 0.0522 0.6198 0.077 Uiso 1 1 calc R . . H20B H 0.9463 0.1022 0.6699 0.077 Uiso 1 1 calc R . . H20C H 1.0307 0.1048 0.5874 0.077 Uiso 1 1 calc R . . C21 C 0.8394(8) 0.0902(3) 0.4864(7) 0.037(2) Uani 1 1 d U . . C22 C 0.7283(8) 0.1096(3) 0.4942(7) 0.030(2) Uani 1 1 d U . . H22 H 0.7317 0.1181 0.5734 0.036 Uiso 1 1 calc R . . C23 C 0.6136(8) 0.1177(3) 0.3973(8) 0.033(2) Uani 1 1 d U . . C24 C 0.5021(8) 0.1414(4) 0.4211(8) 0.047(3) Uani 1 1 d U . . H24A H 0.4794 0.1731 0.3772 0.070 Uiso 1 1 calc R . . H24B H 0.5274 0.1473 0.5090 0.070 Uiso 1 1 calc R . . H24C H 0.4278 0.1191 0.3924 0.070 Uiso 1 1 calc R . . C30 C 1.1013(7) 0.0628(3) 0.1852(7) 0.031(2) Uani 1 1 d DU . . C31 C 1.0859(8) 0.0058(3) 0.1925(9) 0.048(3) Uani 1 1 d DU . . H31A H 1.0868 -0.0097 0.1178 0.072 Uiso 1 1 calc R . . H31B H 1.0044 -0.0015 0.2007 0.072 Uiso 1 1 calc R . . H31C H 1.1569 -0.0074 0.2635 0.072 Uiso 1 1 calc R . . C32 C 1.1146(8) 0.0866(4) 0.3073(7) 0.042(2) Uani 1 1 d DU . . H32A H 1.1906 0.0731 0.3728 0.063 Uiso 1 1 calc R . . H32B H 1.0381 0.0792 0.3247 0.063 Uiso 1 1 calc R . . H32C H 1.1237 0.1226 0.3024 0.063 Uiso 1 1 calc R . . C33 C 1.2279(7) 0.0715(4) 0.1661(8) 0.052(3) Uani 1 1 d DU . . H33A H 1.2976 0.0536 0.2291 0.078 Uiso 1 1 calc R . . H33B H 1.2475 0.1071 0.1721 0.078 Uiso 1 1 calc R . . H33C H 1.2189 0.0594 0.0851 0.078 Uiso 1 1 calc R . . C70 C 0.8540(11) 0.2528(4) -0.3156(9) 0.066(3) Uani 0.738(9) 1 d PDU A 1 C71 C 0.7848(15) 0.2416(5) -0.4531(10) 0.069(3) Uani 0.738(9) 1 d PDU A 1 H71A H 0.6921 0.2398 -0.4733 0.104 Uiso 0.738(9) 1 calc PR A 1 H71B H 0.8152 0.2098 -0.4722 0.104 Uiso 0.738(9) 1 calc PR A 1 H71C H 0.8031 0.2681 -0.5011 0.104 Uiso 0.738(9) 1 calc PR A 1 C72 C 0.8319(17) 0.3014(4) -0.2710(15) 0.074(4) Uani 0.738(9) 1 d PDU A 1 H72A H 0.7401 0.3057 -0.2896 0.111 Uiso 0.738(9) 1 calc PR A 1 H72B H 0.8617 0.3277 -0.3114 0.111 Uiso 0.738(9) 1 calc PR A 1 H72C H 0.8792 0.3034 -0.1824 0.111 Uiso 0.738(9) 1 calc PR A 1 C73 C 1.0015(13) 0.2514(6) -0.3047(15) 0.083(4) Uani 0.738(9) 1 d PDU A 1 H73A H 1.0164 0.2784 -0.3533 0.124 Uiso 0.738(9) 1 calc PR A 1 H73B H 1.0188 0.2195 -0.3353 0.124 Uiso 0.738(9) 1 calc PR A 1 H73C H 1.0588 0.2554 -0.2188 0.124 Uiso 0.738(9) 1 calc PR A 1 C170 C 0.8540(11) 0.2528(4) -0.3156(9) 0.066(3) Uani 0.262(9) 1 d PDU A 2 C171 C 0.716(2) 0.2745(14) -0.396(3) 0.069(3) Uani 0.262(9) 1 d PDU A 2 H17A H 0.6859 0.2957 -0.3453 0.104 Uiso 0.262(9) 1 calc PR A 2 H17B H 0.6557 0.2470 -0.4291 0.104 Uiso 0.262(9) 1 calc PR A 2 H17C H 0.7219 0.2940 -0.4639 0.104 Uiso 0.262(9) 1 calc PR A 2 C172 C 0.925(4) 0.2939(12) -0.231(3) 0.074(4) Uani 0.262(9) 1 d PDU A 2 H17D H 1.0160 0.2929 -0.2201 0.111 Uiso 0.262(9) 1 calc PR A 2 H17E H 0.9185 0.2894 -0.1510 0.111 Uiso 0.262(9) 1 calc PR A 2 H17F H 0.8884 0.3260 -0.2653 0.111 Uiso 0.262(9) 1 calc PR A 2 C173 C 0.912(4) 0.2356(15) -0.407(3) 0.083(4) Uani 0.262(9) 1 d PDU A 2 H17G H 0.9676 0.2618 -0.4174 0.124 Uiso 0.262(9) 1 calc PR A 2 H17H H 0.8436 0.2284 -0.4858 0.124 Uiso 0.262(9) 1 calc PR A 2 H17I H 0.9635 0.2055 -0.3757 0.124 Uiso 0.262(9) 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 Pd1 0.0229(3) 0.0421(4) 0.0240(3) 0.0060(4) 0.0141(2) 0.0045(4) N1 0.020(3) 0.035(4) 0.028(3) 0.013(4) 0.010(3) 0.019(4) O1 0.026(3) 0.029(4) 0.033(3) 0.013(3) 0.016(3) 0.013(3) O21 0.025(3) 0.072(5) 0.021(3) 0.012(3) 0.012(2) 0.009(3) O22 0.025(3) 0.054(4) 0.025(3) -0.003(3) 0.011(3) 0.005(3) C1 0.032(4) 0.008(4) 0.024(4) 0.000(3) 0.017(3) 0.009(3) C2 0.029(3) 0.017(4) 0.031(4) 0.010(4) 0.020(3) 0.007(4) C3 0.029(3) 0.005(4) 0.026(4) -0.005(3) 0.014(3) -0.004(3) C4 0.036(4) 0.028(5) 0.027(4) -0.003(3) 0.018(4) -0.008(4) C5 0.053(5) 0.019(5) 0.025(4) -0.002(3) 0.027(4) -0.009(4) C6 0.078(6) 0.025(6) 0.024(5) -0.003(3) 0.029(5) -0.015(4) C7 0.096(7) 0.016(5) 0.022(4) -0.009(3) 0.023(5) -0.025(4) C8 0.082(6) 0.029(6) 0.014(5) -0.002(4) 0.014(5) -0.004(5) C9 0.055(5) 0.022(5) 0.030(5) 0.001(4) 0.021(4) 0.009(4) C10 0.045(4) 0.017(5) 0.026(4) 0.000(3) 0.019(4) 0.004(4) C11 0.032(4) 0.023(5) 0.024(3) 0.018(4) 0.016(3) 0.015(4) C12 0.023(4) 0.050(7) 0.035(4) 0.004(4) 0.021(3) 0.008(4) C13 0.025(4) 0.054(6) 0.042(5) -0.004(5) 0.014(4) 0.007(4) C14 0.028(4) 0.033(5) 0.036(4) 0.009(4) 0.014(4) 0.018(4) C15 0.028(4) 0.031(6) 0.039(5) 0.005(4) 0.005(4) 0.010(4) C16 0.046(5) 0.026(5) 0.023(4) 0.002(4) -0.004(4) -0.002(4) C17 0.064(6) 0.023(5) 0.029(4) -0.003(4) 0.023(4) 0.001(5) C18 0.038(5) 0.027(5) 0.026(4) 0.005(4) 0.012(4) 0.005(4) C19 0.036(4) 0.024(5) 0.028(4) 0.001(3) 0.016(3) -0.002(4) C20 0.037(5) 0.089(9) 0.025(4) 0.012(5) 0.008(4) 0.018(6) C21 0.030(4) 0.054(7) 0.026(4) -0.001(4) 0.010(3) -0.009(4) C22 0.030(4) 0.043(6) 0.023(4) -0.004(4) 0.017(3) -0.013(4) C23 0.040(5) 0.035(6) 0.030(4) 0.001(4) 0.020(4) 0.001(4) C24 0.046(6) 0.058(7) 0.044(6) -0.015(5) 0.026(5) 0.003(5) C30 0.022(4) 0.037(5) 0.042(5) 0.005(4) 0.020(4) 0.008(4) C31 0.037(6) 0.035(5) 0.076(7) 0.017(5) 0.027(5) 0.019(4) C32 0.042(5) 0.051(7) 0.033(4) 0.006(4) 0.015(4) -0.006(5) C33 0.024(4) 0.083(9) 0.054(6) -0.003(6) 0.021(4) -0.008(5) C70 0.103(7) 0.040(6) 0.051(5) 0.018(4) 0.025(5) -0.024(5) C71 0.109(7) 0.059(7) 0.049(5) 0.028(4) 0.042(5) -0.015(6) C72 0.113(10) 0.025(6) 0.088(9) 0.020(6) 0.043(9) -0.020(7) C73 0.110(8) 0.072(11) 0.079(9) 0.023(7) 0.050(7) -0.018(8) C170 0.103(7) 0.040(6) 0.051(5) 0.018(4) 0.025(5) -0.024(5) C171 0.109(7) 0.059(7) 0.049(5) 0.028(4) 0.042(5) -0.015(6) C172 0.113(10) 0.025(6) 0.088(9) 0.020(6) 0.043(9) -0.020(7) C173 0.110(8) 0.072(11) 0.079(9) 0.023(7) 0.050(7) -0.018(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 Pd1 O1 1.981(5) . ? Pd1 O22 1.992(5) . ? Pd1 O21 1.996(5) . ? Pd1 N1 2.002(6) . ? N1 C11 1.371(8) . ? N1 C12 1.385(9) . ? O1 C2 1.339(8) . ? O21 C21 1.277(9) . ? O22 C23 1.280(9) . ? C1 C2 1.381(10) . ? C1 C10 1.467(10) . ? C1 C11 1.479(10) . ? C2 C3 1.440(9) . ? C3 C4 1.353(10) . ? C3 C30 1.563(10) . ? C4 C5 1.394(11) . ? C4 H4 0.9500 . ? C5 C10 1.418(11) . ? C5 C6 1.432(10) . ? C6 C7 1.384(13) . ? C6 H6 0.9500 . ? C7 C8 1.423(13) . ? C7 C70 1.551(12) . ? C8 C9 1.352(11) . ? C8 H8 0.9500 . ? C9 C10 1.411(11) . ? C9 H9 0.9500 . ? C11 C19 1.432(10) . ? C12 C13 1.343(11) . ? C12 H12 0.9500 . ? C13 C14 1.414(11) . ? C13 H13 0.9500 . ? C14 C15 1.404(11) . ? C14 C19 1.444(11) . ? C15 C16 1.356(11) . ? C15 H15 0.9500 . ? C16 C17 1.413(11) . ? C16 H16 0.9500 . ? C17 C18 1.373(11) . ? C17 H17 0.9500 . ? C18 C19 1.422(10) . ? C18 H18 0.9500 . ? C20 C21 1.523(10) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.393(11) . ? C22 C23 1.381(11) . ? C22 H22 0.9500 . ? C23 C24 1.527(11) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C30 C32 1.532(10) . ? C30 C33 1.543(9) . ? C30 C31 1.552(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C70 C72 1.467(13) . ? C70 C71 1.542(13) . ? C70 C73 1.618(13) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C173 H17G 0.9800 . ? C173 H17H 0.9800 . ? C173 H17I 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 O1 Pd1 O22 178.9(2) . . ? O1 Pd1 O21 87.0(2) . . ? O22 Pd1 O21 94.1(2) . . ? O1 Pd1 N1 88.1(2) . . ? O22 Pd1 N1 90.8(2) . . ? O21 Pd1 N1 174.4(3) . . ? C11 N1 C12 119.3(7) . . ? C11 N1 Pd1 120.0(5) . . ? C12 N1 Pd1 119.0(5) . . ? C2 O1 Pd1 113.1(5) . . ? C21 O21 Pd1 123.0(5) . . ? C23 O22 Pd1 122.8(5) . . ? C2 C1 C10 120.7(7) . . ? C2 C1 C11 120.1(7) . . ? C10 C1 C11 119.2(7) . . ? O1 C2 C1 120.9(6) . . ? O1 C2 C3 119.1(6) . . ? C1 C2 C3 120.0(7) . . ? C4 C3 C2 118.0(7) . . ? C4 C3 C30 121.9(7) . . ? C2 C3 C30 120.1(6) . . ? C3 C4 C5 123.8(8) . . ? C3 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C4 C5 C10 120.1(7) . . ? C4 C5 C6 120.6(8) . . ? C10 C5 C6 119.3(8) . . ? C7 C6 C5 120.7(9) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 117.8(8) . . ? C6 C7 C70 120.2(9) . . ? C8 C7 C70 121.9(10) . . ? C9 C8 C7 123.0(10) . . ? C9 C8 H8 118.5 . . ? C7 C8 H8 118.5 . . ? C8 C9 C10 120.1(9) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C5 119.1(8) . . ? C9 C10 C1 124.3(8) . . ? C5 C10 C1 116.3(7) . . ? N1 C11 C19 119.5(7) . . ? N1 C11 C1 118.2(7) . . ? C19 C11 C1 122.3(6) . . ? C13 C12 N1 124.7(7) . . ? C13 C12 H12 117.7 . . ? N1 C12 H12 117.7 . . ? C12 C13 C14 118.5(8) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 122.4(8) . . ? C15 C14 C19 118.6(7) . . ? C13 C14 C19 118.9(8) . . ? C16 C15 C14 120.8(8) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 120.9(8) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C18 C17 C16 121.1(8) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 118.9(8) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C18 C19 C11 121.3(7) . . ? C18 C19 C14 119.5(8) . . ? C11 C19 C14 119.0(7) . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O21 C21 C22 126.8(8) . . ? O21 C21 C20 113.6(7) . . ? C22 C21 C20 119.5(7) . . ? C23 C22 C21 126.0(7) . . ? C23 C22 H22 117.0 . . ? C21 C22 H22 117.0 . . ? O22 C23 C22 127.4(8) . . ? O22 C23 C24 113.3(7) . . ? C22 C23 C24 119.3(7) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C32 C30 C33 108.0(7) . . ? C32 C30 C31 109.5(7) . . ? C33 C30 C31 106.6(7) . . ? C32 C30 C3 108.3(6) . . ? C33 C30 C3 111.9(6) . . ? C31 C30 C3 112.4(7) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C72 C70 C71 117.8(11) . . ? C72 C70 C7 112.0(9) . . ? C71 C70 C7 107.6(8) . . ? C72 C70 C73 107.5(11) . . ? C71 C70 C73 100.0(9) . . ? C7 C70 C73 111.3(10) . . ? H17A C171 H17B 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? H17D C172 H17E 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? H17G C173 H17H 109.5 . . ? H17G C173 H17I 109.5 . . ? H17H C173 H17I 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 O1 Pd1 N1 C11 -25.8(7) . . . . ? O22 Pd1 N1 C11 154.5(7) . . . . ? O1 Pd1 N1 C12 139.2(6) . . . . ? O22 Pd1 N1 C12 -40.5(6) . . . . ? O21 Pd1 O1 C2 -123.8(5) . . . . ? N1 Pd1 O1 C2 58.8(5) . . . . ? O1 Pd1 O21 C21 -179.8(7) . . . . ? O22 Pd1 O21 C21 -0.2(7) . . . . ? O21 Pd1 O22 C23 -0.2(7) . . . . ? N1 Pd1 O22 C23 177.1(7) . . . . ? Pd1 O1 C2 C1 -48.3(9) . . . . ? Pd1 O1 C2 C3 132.3(6) . . . . ? C10 C1 C2 O1 168.8(7) . . . . ? C11 C1 C2 O1 -10.4(11) . . . . ? C10 C1 C2 C3 -11.9(11) . . . . ? C11 C1 C2 C3 169.0(7) . . . . ? O1 C2 C3 C4 -175.2(7) . . . . ? C1 C2 C3 C4 5.4(11) . . . . ? O1 C2 C3 C30 4.7(11) . . . . ? C1 C2 C3 C30 -174.7(7) . . . . ? C2 C3 C4 C5 4.2(12) . . . . ? C30 C3 C4 C5 -175.6(7) . . . . ? C3 C4 C5 C10 -7.3(12) . . . . ? C3 C4 C5 C6 170.0(7) . . . . ? C4 C5 C6 C7 -174.0(8) . . . . ? C10 C5 C6 C7 3.3(12) . . . . ? C5 C6 C7 C8 -2.0(12) . . . . ? C5 C6 C7 C70 176.0(8) . . . . ? C6 C7 C8 C9 0.9(13) . . . . ? C70 C7 C8 C9 -177.1(8) . . . . ? C7 C8 C9 C10 -1.0(13) . . . . ? C8 C9 C10 C5 2.2(12) . . . . ? C8 C9 C10 C1 174.9(7) . . . . ? C4 C5 C10 C9 174.0(7) . . . . ? C6 C5 C10 C9 -3.3(11) . . . . ? C4 C5 C10 C1 0.7(11) . . . . ? C6 C5 C10 C1 -176.6(7) . . . . ? C2 C1 C10 C9 -164.2(8) . . . . ? C11 C1 C10 C9 15.0(11) . . . . ? C2 C1 C10 C5 8.6(10) . . . . ? C11 C1 C10 C5 -172.2(7) . . . . ? C12 N1 C11 C19 -3.3(12) . . . . ? Pd1 N1 C11 C19 161.8(6) . . . . ? C12 N1 C11 C1 176.9(7) . . . . ? Pd1 N1 C11 C1 -18.1(10) . . . . ? C2 C1 C11 N1 48.2(11) . . . . ? C10 C1 C11 N1 -131.0(8) . . . . ? C2 C1 C11 C19 -131.7(8) . . . . ? C10 C1 C11 C19 49.1(11) . . . . ? C11 N1 C12 C13 -1.4(13) . . . . ? Pd1 N1 C12 C13 -166.6(7) . . . . ? N1 C12 C13 C14 4.8(14) . . . . ? C12 C13 C14 C15 174.2(8) . . . . ? C12 C13 C14 C19 -3.4(13) . . . . ? C13 C14 C15 C16 -176.2(8) . . . . ? C19 C14 C15 C16 1.4(12) . . . . ? C14 C15 C16 C17 0.8(13) . . . . ? C15 C16 C17 C18 -0.6(13) . . . . ? C16 C17 C18 C19 -1.7(12) . . . . ? C17 C18 C19 C11 178.7(8) . . . . ? C17 C18 C19 C14 3.9(12) . . . . ? N1 C11 C19 C18 -170.6(7) . . . . ? C1 C11 C19 C18 9.3(12) . . . . ? N1 C11 C19 C14 4.3(12) . . . . ? C1 C11 C19 C14 -175.8(7) . . . . ? C15 C14 C19 C18 -3.7(12) . . . . ? C13 C14 C19 C18 174.0(8) . . . . ? C15 C14 C19 C11 -178.7(8) . . . . ? C13 C14 C19 C11 -1.0(12) . . . . ? Pd1 O21 C21 C22 1.0(13) . . . . ? Pd1 O21 C21 C20 -176.1(6) . . . . ? O21 C21 C22 C23 -1.5(15) . . . . ? C20 C21 C22 C23 175.5(9) . . . . ? Pd1 O22 C23 C22 -0.1(12) . . . . ? Pd1 O22 C23 C24 178.4(5) . . . . ? C21 C22 C23 O22 1.0(15) . . . . ? C21 C22 C23 C24 -177.5(8) . . . . ? C4 C3 C30 C32 109.6(8) . . . . ? C2 C3 C30 C32 -70.2(9) . . . . ? C4 C3 C30 C33 -9.2(10) . . . . ? C2 C3 C30 C33 170.9(7) . . . . ? C4 C3 C30 C31 -129.2(8) . . . . ? C2 C3 C30 C31 50.9(9) . . . . ? C6 C7 C70 C72 -108.7(12) . . . . ? C8 C7 C70 C72 69.3(13) . . . . ? C6 C7 C70 C71 120.3(11) . . . . ? C8 C7 C70 C71 -61.7(13) . . . . ? C6 C7 C70 C73 11.8(13) . . . . ? C8 C7 C70 C73 -170.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.683 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.117 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 0.308 0.250 0.596 357.6 0.6 2 0.692 0.750 0.713 357.6 0.5 _platon_squeeze_details ; ; #===END data_11 _database_code_depnum_ccdc_archive 'CCDC 728916' _chemical_formula_structural '[PtCl2{L(H)-H}2].2PhMe' _chemical_formula_moiety 'C54 H58 Cl2 N2 O2 Pt, 2(C7 H8)' _chemical_formula_sum 'C68 H74 Cl2 N2 O2 Pt' _chemical_formula_weight 1217.28 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' Cl Cl 0.1484 0.1585 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3200(4) _cell_length_b 14.8220(6) _cell_length_c 19.2990(7) _cell_angle_alpha 84.676(2) _cell_angle_beta 77.397(2) _cell_angle_gamma 74.396(2) _cell_volume 3041.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10509 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 2.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5814 _exptl_absorpt_correction_T_max 0.8675 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42554 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.64 _reflns_number_total 13692 _reflns_number_gt 10404 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004) ; _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^ > 2\s(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^)+(0.0000P)^2^+36.2575P] 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_number_reflns 13692 _refine_ls_number_parameters 715 _refine_ls_number_restraints 163 _refine_ls_R_factor_all 0.1230 _refine_ls_R_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.1784 _refine_ls_wR_factor_gt 0.1583 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.126 _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 Pt1 Pt 0.82360(3) 0.00323(3) 0.258150(18) 0.03467(11) Uani 1 1 d . . . Cl1 Cl 0.6199(2) 0.08843(16) 0.26681(12) 0.0419(5) Uani 1 1 d . . . Cl2 Cl 1.0307(2) -0.07854(17) 0.25041(12) 0.0420(5) Uani 1 1 d D . . N1 N 0.8539(6) 0.0476(5) 0.1553(4) 0.0326(16) Uani 1 1 d . . . O1 O 1.1443(6) 0.0661(5) 0.1516(3) 0.0418(15) Uani 1 1 d D . . C1 C 0.9434(8) 0.1714(6) 0.1799(4) 0.0325(18) Uani 1 1 d . . . C2 C 1.0677(8) 0.1453(6) 0.1847(4) 0.0351(19) Uani 1 1 d . . . C3 C 1.1190(8) 0.1995(6) 0.2221(5) 0.037(2) Uani 1 1 d . . . C4 C 1.0381(8) 0.2766(7) 0.2543(5) 0.039(2) Uani 1 1 d . . . H4 H 1.0705 0.3136 0.2793 0.047 Uiso 1 1 calc R . . C5 C 0.9076(8) 0.3054(6) 0.2531(4) 0.0318(18) Uani 1 1 d . . . C6 C 0.8263(8) 0.3840(6) 0.2890(5) 0.038(2) Uani 1 1 d . . . H6 H 0.8590 0.4188 0.3156 0.045 Uiso 1 1 calc R . . C7 C 0.7012(8) 0.4118(6) 0.2871(4) 0.037(2) Uani 1 1 d . . . C8 C 0.6562(8) 0.3575(6) 0.2473(5) 0.0356(19) Uani 1 1 d . . . H8 H 0.5697 0.3751 0.2457 0.043 Uiso 1 1 calc R . . C9 C 0.7309(8) 0.2813(6) 0.2114(5) 0.037(2) Uani 1 1 d . . . H9 H 0.6968 0.2481 0.1844 0.044 Uiso 1 1 calc R . . C10 C 0.8599(8) 0.2513(6) 0.2142(4) 0.0323(18) Uani 1 1 d . . . C11 C 0.9013(7) 0.1198(6) 0.1300(4) 0.0330(19) Uani 1 1 d . . . C12 C 0.9136(8) 0.1484(6) 0.0581(4) 0.037(2) Uani 1 1 d . . . C13 C 0.9657(8) 0.2235(6) 0.0298(5) 0.038(2) Uani 1 1 d . . . H13 H 0.9945 0.2558 0.0604 0.045 Uiso 1 1 calc R . . C14 C 0.9759(10) 0.2512(8) -0.0398(5) 0.050(2) Uani 1 1 d . . . H14 H 1.0122 0.3017 -0.0577 0.060 Uiso 1 1 calc R . . C15 C 0.9312(10) 0.2034(7) -0.0862(5) 0.049(2) Uani 1 1 d . . . H15 H 0.9376 0.2225 -0.1349 0.058 Uiso 1 1 calc R . . C16 C 0.8802(9) 0.1316(7) -0.0609(5) 0.043(2) Uani 1 1 d . . . H16 H 0.8510 0.1007 -0.0921 0.052 Uiso 1 1 calc R . . C17 C 0.8695(8) 0.1016(6) 0.0111(4) 0.0351(19) Uani 1 1 d . . . C18 C 0.8188(8) 0.0256(6) 0.0414(5) 0.0347(19) Uani 1 1 d . . . H18 H 0.7887 -0.0080 0.0125 0.042 Uiso 1 1 calc R . . C19 C 0.8131(8) 0.0011(6) 0.1104(4) 0.0353(19) Uani 1 1 d . . . H19 H 0.7796 -0.0505 0.1291 0.042 Uiso 1 1 calc R . . C30 C 1.2575(9) 0.1726(7) 0.2243(5) 0.044(2) Uani 1 1 d . . . C31 C 1.2926(9) 0.2436(7) 0.2644(6) 0.053(3) Uani 1 1 d . . . H31A H 1.2674 0.3064 0.2427 0.079 Uiso 1 1 calc R . . H31B H 1.3833 0.2261 0.2617 0.079 Uiso 1 1 calc R . . H31C H 1.2494 0.2434 0.3142 0.079 Uiso 1 1 calc R . . C32 C 1.3384(9) 0.1670(9) 0.1490(6) 0.057(3) Uani 1 1 d . . . H32A H 1.3233 0.1183 0.1235 0.086 Uiso 1 1 calc R . . H32B H 1.4270 0.1515 0.1518 0.086 Uiso 1 1 calc R . . H32C H 1.3164 0.2276 0.1235 0.086 Uiso 1 1 calc R . . C33 C 1.2883(9) 0.0773(8) 0.2654(6) 0.056(3) Uani 1 1 d . . . H33A H 1.2358 0.0823 0.3132 0.085 Uiso 1 1 calc R . . H33B H 1.3768 0.0604 0.2689 0.085 Uiso 1 1 calc R . . H33C H 1.2720 0.0290 0.2402 0.085 Uiso 1 1 calc R . . C70 C 0.6116(9) 0.4983(7) 0.3255(5) 0.048(2) Uani 1 1 d . . . C71 C 0.6762(11) 0.5446(8) 0.3684(6) 0.063(3) Uani 1 1 d . . . H71A H 0.7122 0.4988 0.4031 0.095 Uiso 1 1 calc R . . H71B H 0.6150 0.5975 0.3933 0.095 Uiso 1 1 calc R . . H71C H 0.7430 0.5671 0.3363 0.095 Uiso 1 1 calc R . . C72 C 0.5586(10) 0.5690(7) 0.2700(6) 0.058(3) Uani 1 1 d . . . H72A H 0.6269 0.5898 0.2380 0.087 Uiso 1 1 calc R . . H72B H 0.4981 0.6231 0.2939 0.087 Uiso 1 1 calc R . . H72C H 0.5168 0.5394 0.2426 0.087 Uiso 1 1 calc R . . C73 C 0.5037(10) 0.4677(8) 0.3778(6) 0.060(3) Uani 1 1 d . . . H73A H 0.4625 0.4354 0.3520 0.089 Uiso 1 1 calc R . . H73B H 0.4428 0.5231 0.3997 0.089 Uiso 1 1 calc R . . H73C H 0.5376 0.4252 0.4149 0.089 Uiso 1 1 calc R . . N11 N 0.7767(7) -0.0448(6) 0.3595(3) 0.0376(17) Uani 1 1 d . . . O11 O 1.0003(8) -0.2680(6) 0.3665(4) 0.063(2) Uani 1 1 d D . . C101 C 0.8170(9) -0.2050(7) 0.3183(5) 0.045(2) Uani 1 1 d . . . C102 C 0.9309(9) -0.2676(7) 0.3182(4) 0.041(2) Uani 1 1 d . . . C103 C 0.9776(9) -0.3411(8) 0.2654(6) 0.050(3) Uani 1 1 d . . . C104 C 0.9072(10) -0.3384(7) 0.2168(5) 0.047(3) Uani 1 1 d . . . H104 H 0.9371 -0.3849 0.1820 0.057 Uiso 1 1 calc R . . C105 C 0.7921(9) -0.2718(6) 0.2135(5) 0.043(2) Uani 1 1 d . . . C106 C 0.7269(9) -0.2695(6) 0.1613(5) 0.042(2) Uani 1 1 d . . . H106 H 0.7629 -0.3125 0.1242 0.051 Uiso 1 1 calc R . . C107 C 0.6075(10) -0.2059(7) 0.1594(4) 0.044(2) Uani 1 1 d . . . C108 C 0.5633(11) -0.1436(8) 0.2160(5) 0.053(3) Uani 1 1 d . . . H108 H 0.4847 -0.0992 0.2175 0.063 Uiso 1 1 calc R . . C109 C 0.6257(9) -0.1433(7) 0.2678(4) 0.039(2) Uani 1 1 d . . . H109 H 0.5882 -0.1003 0.3047 0.047 Uiso 1 1 calc R . . C110 C 0.7441(10) -0.2043(7) 0.2695(5) 0.045(2) Uani 1 1 d . . . C111 C 0.7667(10) -0.1316(7) 0.3751(5) 0.048(3) Uani 1 1 d . . . C112 C 0.7394(9) 0.0198(7) 0.4122(5) 0.046(2) Uani 1 1 d . . . H112 H 0.7509 0.0810 0.4009 0.055 Uiso 1 1 calc R . . C113 C 0.6870(9) -0.0017(8) 0.4794(5) 0.050(3) Uani 1 1 d . . . H113 H 0.6643 0.0437 0.5149 0.060 Uiso 1 1 calc R . . C114 C 0.6659(9) -0.0912(8) 0.4970(5) 0.048(2) Uani 1 1 d . . . C115 C 0.6034(10) -0.1178(9) 0.5649(5) 0.059(3) Uani 1 1 d . . . H115 H 0.5736 -0.0737 0.6015 0.070 Uiso 1 1 calc R . . C116 C 0.5858(12) -0.2050(10) 0.5781(6) 0.073(4) Uani 1 1 d . . . H116 H 0.5374 -0.2198 0.6223 0.088 Uiso 1 1 calc R . . C117 C 0.6382(15) -0.2735(11) 0.5272(6) 0.089(5) Uani 1 1 d . . . H117 H 0.6298 -0.3356 0.5379 0.107 Uiso 1 1 calc R . . C118 C 0.7017(12) -0.2508(9) 0.4621(6) 0.069(3) Uani 1 1 d . . . H118 H 0.7384 -0.2978 0.4279 0.083 Uiso 1 1 calc R . . C119 C 0.7133(10) -0.1597(8) 0.4451(5) 0.052(3) Uani 1 1 d . . . C130 C 1.1007(11) -0.4118(8) 0.2653(6) 0.055(3) Uani 1 1 d . . . C131 C 1.2107(11) -0.3642(9) 0.2529(7) 0.069(3) Uani 1 1 d . . . H13A H 1.2030 -0.3176 0.2136 0.104 Uiso 1 1 calc R . . H13B H 1.2904 -0.4118 0.2412 0.104 Uiso 1 1 calc R . . H13C H 1.2081 -0.3333 0.2962 0.104 Uiso 1 1 calc R . . C132 C 1.1353(11) -0.4835(8) 0.2058(7) 0.067(3) Uani 1 1 d . . . H13D H 1.0689 -0.5161 0.2109 0.101 Uiso 1 1 calc R . . H13E H 1.2145 -0.5292 0.2095 0.101 Uiso 1 1 calc R . . H13F H 1.1443 -0.4505 0.1593 0.101 Uiso 1 1 calc R . . C133 C 1.1005(12) -0.4715(9) 0.3368(7) 0.071(3) Uani 1 1 d . . . H13G H 1.0928 -0.4309 0.3757 0.106 Uiso 1 1 calc R . . H13H H 1.1789 -0.5209 0.3329 0.106 Uiso 1 1 calc R . . H13I H 1.0296 -0.5001 0.3463 0.106 Uiso 1 1 calc R . . C170 C 0.5370(11) -0.2017(8) 0.1014(6) 0.056(3) Uani 1 1 d . . . C171 C 0.5146(15) -0.1025(9) 0.0664(8) 0.086(4) Uani 1 1 d . . . H17A H 0.4878 -0.0559 0.1033 0.129 Uiso 1 1 calc R . . H17B H 0.4494 -0.0934 0.0385 0.129 Uiso 1 1 calc R . . H17C H 0.5924 -0.0950 0.0351 0.129 Uiso 1 1 calc R . . C172 C 0.6051(12) -0.2720(9) 0.0442(6) 0.070(3) Uani 1 1 d . . . H17D H 0.6891 -0.2632 0.0251 0.105 Uiso 1 1 calc R . . H17E H 0.5582 -0.2623 0.0059 0.105 Uiso 1 1 calc R . . H17F H 0.6120 -0.3357 0.0647 0.105 Uiso 1 1 calc R . . C173 C 0.4099(11) -0.2218(10) 0.1359(7) 0.072(4) Uani 1 1 d . . . H17G H 0.4238 -0.2858 0.1564 0.108 Uiso 1 1 calc R . . H17H H 0.3589 -0.2150 0.0998 0.108 Uiso 1 1 calc R . . H17I H 0.3662 -0.1773 0.1734 0.108 Uiso 1 1 calc R . . C201 C 0.831(4) 0.4685(16) 0.0912(15) 0.110(10) Uani 0.50 1 d PDU A -1 H20A H 0.8441 0.4896 0.1350 0.164 Uiso 0.50 1 calc PR A -1 H20B H 0.8467 0.4001 0.0938 0.164 Uiso 0.50 1 calc PR A -1 H20C H 0.7453 0.4971 0.0854 0.164 Uiso 0.50 1 calc PR A -1 C202 C 0.901(2) 0.4906(11) 0.0428(11) 0.135(7) Uani 0.50 1 d PDU A -1 C203 C 1.005(3) 0.4467(16) 0.0719(14) 0.176(10) Uani 1 1 d DU . . H203 H 1.0066 0.4138 0.1165 0.211 Uiso 1 1 calc R B . C204 C 0.897(3) 0.5382(12) -0.0211(11) 0.138(8) Uani 1 1 d DU . . H204 H 0.8160 0.5639 -0.0315 0.166 Uiso 1 1 calc R B . C205 C 0.901(2) 0.4906(11) 0.0428(11) 0.135(7) Uani 0.50 1 d PDU B -1 H205 H 0.8223 0.4872 0.0711 0.162 Uiso 0.50 1 calc PR B -1 C301 C 0.3950(18) 0.6322(16) 0.9619(11) 0.128(6) Uani 0.50 1 d PDU C -1 H30A H 0.3087 0.6287 0.9653 0.191 Uiso 0.50 1 calc PR C -1 H30B H 0.4317 0.6453 0.9124 0.191 Uiso 0.50 1 calc PR C -1 H30C H 0.3953 0.6825 0.9915 0.191 Uiso 0.50 1 calc PR C -1 C302 C 0.499(2) 0.5727(18) 0.9193(17) 0.122(8) Uani 0.50 1 d PDU D -1 H302 H 0.5257 0.5918 0.8713 0.147 Uiso 0.50 1 calc PR D -1 C303 C 0.5646(15) 0.4865(16) 0.9451(8) 0.108(5) Uani 0.50 1 d PDU . . H303 H 0.6326 0.4500 0.9129 0.130 Uiso 0.50 1 calc PR D . C304 C 0.370(3) 0.589(3) 1.0305(16) 0.120(10) Uani 0.50 1 d PDU . . H304 H 0.2958 0.6199 1.0618 0.143 Uiso 0.50 1 calc PR D . C305 C 0.462(2) 0.551(2) 0.9846(14) 0.096(7) Uani 0.50 1 d PDU . . C306 C 0.3950(18) 0.6322(16) 0.9619(11) 0.128(6) Uani 0.50 1 d PDU D -1 H306 H 0.3491 0.6918 0.9471 0.153 Uiso 0.50 1 calc PR D -1 C307 C 0.5646(15) 0.4865(16) 0.9451(8) 0.108(5) Uani 0.50 1 d PDU . . H307 H 0.5870 0.5008 0.8958 0.130 Uiso 0.50 1 calc PR . . C401 C 0.004(2) 0.1526(15) 0.4384(12) 0.158(9) Uani 1 1 d . . . H40A H 0.0622 0.0944 0.4511 0.237 Uiso 1 1 calc R . . H40B H 0.0444 0.2044 0.4339 0.237 Uiso 1 1 calc R . . H40C H -0.0176 0.1458 0.3931 0.237 Uiso 1 1 calc R . . C402 C -0.1093(18) 0.1724(11) 0.4939(9) 0.095(5) Uani 1 1 d . . . C403 C -0.1148(19) 0.1264(10) 0.5589(9) 0.092(5) Uani 1 1 d . . . H403 H -0.0422 0.0821 0.5691 0.110 Uiso 1 1 calc R . . C404 C -0.227(2) 0.1434(14) 0.6112(10) 0.113(7) Uani 1 1 d . . . H404 H -0.2286 0.1127 0.6567 0.136 Uiso 1 1 calc R . . C405 C -0.329(2) 0.2032(13) 0.5952(10) 0.117(7) Uani 1 1 d . . . H405 H -0.4047 0.2147 0.6297 0.141 Uiso 1 1 calc R . . C406 C -0.3261(18) 0.2488(10) 0.5295(9) 0.102(5) Uani 1 1 d . . . H406 H -0.4000 0.2919 0.5197 0.123 Uiso 1 1 calc R . . C407 C -0.2193(15) 0.2334(10) 0.4782(9) 0.089(4) Uani 1 1 d . . . H407 H -0.2195 0.2635 0.4326 0.107 Uiso 1 1 calc R . . H1 H 1.122(13) 0.024(7) 0.137(4) 0.107 Uiso 1 1 d D . . H11 H 1.008(14) -0.212(4) 0.356(7) 0.107 Uiso 1 1 d D . . 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 Pt1 0.03561(18) 0.0424(2) 0.02706(16) -0.00775(12) -0.00115(12) -0.01371(14) Cl1 0.0336(11) 0.0446(13) 0.0446(12) -0.0076(10) 0.0017(9) -0.0106(10) Cl2 0.0370(11) 0.0547(15) 0.0364(11) 0.0034(10) -0.0087(9) -0.0160(11) N1 0.031(4) 0.037(4) 0.031(4) -0.005(3) -0.006(3) -0.009(3) O1 0.036(3) 0.045(4) 0.045(4) -0.012(3) -0.006(3) -0.008(3) C1 0.035(4) 0.030(5) 0.032(4) -0.005(3) -0.007(4) -0.006(4) C2 0.037(5) 0.035(5) 0.028(4) -0.004(3) 0.002(4) -0.007(4) C3 0.032(4) 0.042(5) 0.036(5) -0.002(4) -0.007(4) -0.010(4) C4 0.035(5) 0.051(6) 0.037(5) -0.003(4) -0.012(4) -0.017(4) C5 0.034(4) 0.030(4) 0.030(4) -0.001(3) -0.004(3) -0.008(4) C6 0.044(5) 0.037(5) 0.035(5) -0.005(4) -0.004(4) -0.017(4) C7 0.039(5) 0.038(5) 0.030(4) 0.006(4) 0.004(4) -0.014(4) C8 0.033(4) 0.036(5) 0.042(5) -0.002(4) -0.007(4) -0.015(4) C9 0.038(5) 0.035(5) 0.040(5) -0.003(4) -0.007(4) -0.014(4) C10 0.037(5) 0.037(5) 0.025(4) 0.006(3) -0.006(3) -0.016(4) C11 0.020(4) 0.039(5) 0.035(4) -0.007(4) -0.004(3) 0.000(4) C12 0.029(4) 0.046(5) 0.029(4) -0.004(4) 0.003(3) -0.004(4) C13 0.036(5) 0.042(5) 0.034(5) -0.003(4) -0.006(4) -0.010(4) C14 0.056(6) 0.056(6) 0.036(5) 0.002(4) 0.002(4) -0.021(5) C15 0.061(6) 0.051(6) 0.026(4) 0.005(4) -0.005(4) -0.006(5) C16 0.043(5) 0.051(6) 0.027(4) -0.005(4) -0.004(4) 0.001(5) C17 0.027(4) 0.042(5) 0.031(4) -0.010(4) -0.002(3) 0.001(4) C18 0.030(4) 0.039(5) 0.040(5) -0.013(4) -0.009(4) -0.012(4) C19 0.035(5) 0.043(5) 0.034(4) -0.005(4) -0.009(4) -0.017(4) C30 0.036(5) 0.048(6) 0.053(6) -0.004(4) -0.014(4) -0.013(4) C31 0.044(6) 0.050(6) 0.066(7) -0.008(5) -0.025(5) -0.001(5) C32 0.034(5) 0.081(8) 0.058(7) -0.007(6) -0.004(5) -0.020(5) C33 0.039(5) 0.069(8) 0.067(7) -0.013(6) -0.021(5) -0.012(5) C70 0.044(5) 0.042(6) 0.052(6) -0.013(4) 0.008(5) -0.012(5) C71 0.062(7) 0.055(7) 0.074(8) -0.034(6) 0.002(6) -0.020(6) C72 0.051(6) 0.043(6) 0.077(8) -0.003(5) -0.006(6) -0.011(5) C73 0.049(6) 0.058(7) 0.060(7) -0.007(5) 0.017(5) -0.015(5) N11 0.040(4) 0.052(5) 0.022(3) -0.007(3) -0.002(3) -0.016(4) O11 0.071(5) 0.069(5) 0.050(4) -0.005(4) -0.012(4) -0.018(5) C101 0.047(6) 0.056(6) 0.032(5) 0.011(4) 0.001(4) -0.022(5) C102 0.052(6) 0.053(6) 0.024(4) 0.001(4) -0.009(4) -0.021(5) C103 0.039(5) 0.057(7) 0.053(6) 0.011(5) -0.002(5) -0.019(5) C104 0.066(7) 0.063(7) 0.029(5) 0.008(4) -0.008(4) -0.050(6) C105 0.050(6) 0.031(5) 0.041(5) 0.000(4) 0.005(4) -0.011(4) C106 0.040(5) 0.039(5) 0.042(5) -0.007(4) 0.012(4) -0.015(4) C107 0.065(6) 0.047(6) 0.024(4) 0.003(4) -0.003(4) -0.029(5) C108 0.060(7) 0.056(7) 0.053(6) 0.005(5) -0.016(5) -0.029(5) C109 0.045(5) 0.050(6) 0.027(4) -0.002(4) -0.004(4) -0.020(5) C110 0.054(6) 0.048(6) 0.030(5) 0.009(4) 0.003(4) -0.019(5) C111 0.059(6) 0.058(7) 0.027(5) -0.009(4) 0.009(4) -0.027(5) C112 0.050(6) 0.052(6) 0.036(5) -0.015(4) -0.015(4) -0.002(5) C113 0.043(5) 0.075(8) 0.027(5) -0.018(5) -0.015(4) 0.007(5) C114 0.042(5) 0.068(7) 0.030(5) -0.010(5) -0.002(4) -0.008(5) C115 0.047(6) 0.090(9) 0.025(5) -0.010(5) -0.002(4) 0.003(6) C116 0.081(9) 0.100(11) 0.036(6) -0.002(6) 0.011(6) -0.038(8) C117 0.126(12) 0.105(11) 0.052(7) -0.007(7) 0.016(8) -0.081(10) C118 0.092(9) 0.078(9) 0.037(6) -0.002(5) 0.007(6) -0.036(7) C119 0.059(6) 0.065(7) 0.029(5) -0.008(4) 0.011(4) -0.023(6) C130 0.068(7) 0.050(6) 0.051(6) 0.005(5) -0.008(5) -0.028(6) C131 0.054(7) 0.068(8) 0.091(9) -0.011(7) -0.015(6) -0.022(6) C132 0.062(7) 0.061(8) 0.080(8) 0.005(6) -0.018(6) -0.017(6) C133 0.077(8) 0.063(8) 0.079(9) 0.011(6) -0.032(7) -0.021(7) C170 0.059(7) 0.065(7) 0.051(6) 0.007(5) -0.016(5) -0.025(6) C171 0.117(12) 0.064(9) 0.089(10) 0.024(7) -0.052(9) -0.028(8) C172 0.079(8) 0.077(9) 0.056(7) -0.014(6) -0.025(6) -0.012(7) C173 0.055(7) 0.096(10) 0.074(8) 0.000(7) -0.027(6) -0.024(7) C201 0.27(3) 0.030(12) 0.084(16) 0.024(12) -0.107(17) -0.080(18) C202 0.26(2) 0.065(10) 0.101(11) -0.033(8) -0.057(13) -0.051(11) C203 0.33(3) 0.094(14) 0.134(17) -0.028(13) -0.121(18) -0.040(17) C204 0.26(2) 0.066(10) 0.115(13) -0.034(9) -0.091(15) -0.024(13) C205 0.26(2) 0.065(10) 0.101(11) -0.033(8) -0.057(13) -0.051(11) C301 0.103(12) 0.170(16) 0.122(12) -0.021(11) -0.043(10) -0.034(9) C302 0.105(16) 0.20(2) 0.080(13) -0.020(13) -0.044(11) -0.038(13) C303 0.087(10) 0.175(15) 0.069(9) -0.035(9) -0.010(7) -0.039(9) C304 0.086(18) 0.15(2) 0.119(16) -0.031(16) -0.014(15) -0.021(18) C305 0.074(13) 0.166(18) 0.063(12) -0.037(12) -0.031(10) -0.031(11) C306 0.103(12) 0.170(16) 0.122(12) -0.021(11) -0.043(10) -0.034(9) C307 0.087(10) 0.175(15) 0.069(9) -0.035(9) -0.010(7) -0.039(9) C401 0.136(18) 0.131(18) 0.17(2) -0.013(15) 0.025(16) -0.013(15) C402 0.120(14) 0.086(11) 0.085(11) -0.006(9) -0.024(10) -0.036(10) C403 0.149(16) 0.069(9) 0.091(11) 0.030(8) -0.061(11) -0.065(10) C404 0.20(2) 0.100(14) 0.087(12) 0.035(10) -0.074(14) -0.087(15) C405 0.18(2) 0.085(13) 0.089(13) -0.015(10) -0.002(13) -0.051(14) C406 0.127(15) 0.055(9) 0.105(13) 0.005(8) -0.017(11) 0.002(9) C407 0.088(10) 0.068(9) 0.092(11) 0.003(8) -0.024(9) 0.014(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Pt1 N1 2.018(7) . ? Pt1 N11 2.027(7) . ? Pt1 Cl1 2.290(2) . ? Pt1 Cl2 2.310(2) . ? N1 C11 1.330(11) . ? N1 C19 1.378(10) . ? O1 C2 1.374(10) . ? O1 H1 0.83(2) . ? C1 C2 1.378(12) . ? C1 C10 1.416(11) . ? C1 C11 1.505(11) . ? C2 C3 1.430(12) . ? C3 C4 1.360(12) . ? C3 C30 1.519(12) . ? C4 C5 1.428(12) . ? C4 H4 0.9500 . ? C5 C6 1.407(12) . ? C5 C10 1.420(11) . ? C6 C7 1.372(12) . ? C6 H6 0.9500 . ? C7 C8 1.415(12) . ? C7 C70 1.540(12) . ? C8 C9 1.359(12) . ? C8 H8 0.9500 . ? C9 C10 1.419(12) . ? C9 H9 0.9500 . ? C11 C12 1.401(12) . ? C12 C13 1.410(12) . ? C12 C17 1.432(12) . ? C13 C14 1.358(12) . ? C13 H13 0.9500 . ? C14 C15 1.438(14) . ? C14 H14 0.9500 . ? C15 C16 1.347(14) . ? C15 H15 0.9500 . ? C16 C17 1.409(12) . ? C16 H16 0.9500 . ? C17 C18 1.420(12) . ? C18 C19 1.339(12) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C30 C32 1.536(14) . ? C30 C31 1.541(13) . ? C30 C33 1.547(15) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C70 C71 1.526(14) . ? C70 C72 1.528(15) . ? C70 C73 1.546(13) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? N11 C111 1.323(12) . ? N11 C112 1.380(11) . ? O11 C102 1.342(12) . ? O11 H11 0.86(2) . ? C101 C102 1.370(14) . ? C101 C110 1.378(14) . ? C101 C111 1.526(13) . ? C102 C103 1.472(14) . ? C103 C104 1.348(14) . ? C103 C130 1.501(15) . ? C104 C105 1.418(14) . ? C104 H104 0.9500 . ? C105 C106 1.365(14) . ? C105 C110 1.455(13) . ? C106 C107 1.431(14) . ? C106 H106 0.9500 . ? C107 C108 1.412(14) . ? C107 C170 1.499(14) . ? C108 C109 1.345(13) . ? C108 H108 0.9500 . ? C109 C110 1.406(13) . ? C109 H109 0.9500 . ? C111 C119 1.426(12) . ? C112 C113 1.351(13) . ? C112 H112 0.9500 . ? C113 C114 1.409(15) . ? C113 H113 0.9500 . ? C114 C119 1.409(13) . ? C114 C115 1.422(14) . ? C115 C116 1.354(17) . ? C115 H115 0.9500 . ? C116 C117 1.397(17) . ? C116 H116 0.9500 . ? C117 C118 1.366(15) . ? C117 H117 0.9500 . ? C118 C119 1.395(15) . ? C118 H118 0.9500 . ? C130 C132 1.552(16) . ? C130 C131 1.555(15) . ? C130 C133 1.568(15) . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C132 H13D 0.9800 . ? C132 H13E 0.9800 . ? C132 H13F 0.9800 . ? C133 H13G 0.9800 . ? C133 H13H 0.9800 . ? C133 H13I 0.9800 . ? C170 C172 1.519(15) . ? C170 C171 1.540(16) . ? C170 C173 1.542(15) . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C173 H17G 0.9800 . ? C173 H17H 0.9800 . ? C173 H17I 0.9800 . ? C201 C202 1.17(4) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C203 C204 1.368(16) 2_765 ? C203 H203 0.9500 . ? C204 C203 1.368(16) 2_765 ? C204 H204 0.9500 . ? C301 C305 1.34(3) . ? C301 H30A 0.9800 . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? C302 C303 1.40(2) . ? C302 H302 0.9500 . ? C303 C305 1.42(4) 2_667 ? C303 H303 0.9500 . ? C304 C303 1.28(4) 2_667 ? C304 H304 0.9500 . ? C305 C307 1.42(4) 2_667 ? C305 C303 1.42(4) 2_667 ? C305 C305 1.64(7) 2_667 ? C401 C402 1.46(2) . ? C401 H40A 0.9800 . ? C401 H40B 0.9800 . ? C401 H40C 0.9800 . ? C402 C403 1.37(2) . ? C402 C407 1.40(2) . ? C403 C404 1.41(3) . ? C403 H403 0.9500 . ? C404 C405 1.33(3) . ? C404 H404 0.9500 . ? C405 C406 1.38(2) . ? C405 H405 0.9500 . ? C406 C407 1.37(2) . ? C406 H406 0.9500 . ? C407 H407 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 N1 Pt1 N11 173.9(3) . . ? N1 Pt1 Cl1 87.5(2) . . ? N11 Pt1 Cl1 88.4(2) . . ? N1 Pt1 Cl2 92.5(2) . . ? N11 Pt1 Cl2 91.7(2) . . ? Cl1 Pt1 Cl2 178.16(9) . . ? C11 N1 C19 119.5(7) . . ? C11 N1 Pt1 125.4(6) . . ? C19 N1 Pt1 114.9(6) . . ? C2 O1 H1 127(10) . . ? C2 C1 C10 121.1(8) . . ? C2 C1 C11 118.2(7) . . ? C10 C1 C11 120.3(7) . . ? O1 C2 C1 118.8(8) . . ? O1 C2 C3 119.5(8) . . ? C1 C2 C3 121.6(8) . . ? C4 C3 C2 116.7(8) . . ? C4 C3 C30 122.1(8) . . ? C2 C3 C30 121.2(8) . . ? C3 C4 C5 124.2(8) . . ? C3 C4 H4 117.9 . . ? C5 C4 H4 117.9 . . ? C6 C5 C10 119.8(8) . . ? C6 C5 C4 122.4(8) . . ? C10 C5 C4 117.8(8) . . ? C7 C6 C5 122.2(8) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C6 C7 C8 117.0(8) . . ? C6 C7 C70 122.7(8) . . ? C8 C7 C70 120.3(8) . . ? C9 C8 C7 123.1(8) . . ? C9 C8 H8 118.5 . . ? C7 C8 H8 118.5 . . ? C8 C9 C10 120.1(8) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C1 C10 C9 123.6(8) . . ? C1 C10 C5 118.5(8) . . ? C9 C10 C5 117.8(8) . . ? N1 C11 C12 121.4(8) . . ? N1 C11 C1 119.1(7) . . ? C12 C11 C1 119.5(8) . . ? C11 C12 C13 122.4(8) . . ? C11 C12 C17 119.6(8) . . ? C13 C12 C17 118.0(8) . . ? C14 C13 C12 121.9(9) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 119.3(9) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.4(9) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 121.1(9) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C18 124.4(8) . . ? C16 C17 C12 119.3(9) . . ? C18 C17 C12 116.3(8) . . ? C19 C18 C17 120.6(8) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 N1 122.5(8) . . ? C18 C19 H19 118.7 . . ? N1 C19 H19 118.7 . . ? C3 C30 C32 111.1(8) . . ? C3 C30 C31 112.1(8) . . ? C32 C30 C31 107.6(8) . . ? C3 C30 C33 108.7(8) . . ? C32 C30 C33 110.7(9) . . ? C31 C30 C33 106.6(8) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C71 C70 C72 109.5(9) . . ? C71 C70 C7 112.4(8) . . ? C72 C70 C7 108.6(8) . . ? C71 C70 C73 107.6(9) . . ? C72 C70 C73 109.8(9) . . ? C7 C70 C73 109.0(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 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C111 N11 C112 119.8(8) . . ? C111 N11 Pt1 122.3(6) . . ? C112 N11 Pt1 117.3(7) . . ? C102 O11 H11 96(9) . . ? C102 C101 C110 123.6(9) . . ? C102 C101 C111 119.0(9) . . ? C110 C101 C111 117.4(9) . . ? O11 C102 C101 122.9(9) . . ? O11 C102 C103 117.7(9) . . ? C101 C102 C103 119.2(9) . . ? C104 C103 C102 116.6(10) . . ? C104 C103 C130 123.1(10) . . ? C102 C103 C130 120.2(9) . . ? C103 C104 C105 125.3(10) . . ? C103 C104 H104 117.3 . . ? C105 C104 H104 117.3 . . ? C106 C105 C104 123.0(9) . . ? C106 C105 C110 120.4(9) . . ? C104 C105 C110 116.6(9) . . ? C105 C106 C107 123.6(8) . . ? C105 C106 H106 118.2 . . ? C107 C106 H106 118.2 . . ? C108 C107 C106 113.9(9) . . ? C108 C107 C170 122.2(10) . . ? C106 C107 C170 123.8(9) . . ? C109 C108 C107 124.0(11) . . ? C109 C108 H108 118.0 . . ? C107 C108 H108 118.0 . . ? C108 C109 C110 122.7(9) . . ? C108 C109 H109 118.7 . . ? C110 C109 H109 118.7 . . ? C101 C110 C109 126.2(9) . . ? C101 C110 C105 118.4(9) . . ? C109 C110 C105 115.4(9) . . ? N11 C111 C119 121.5(8) . . ? N11 C111 C101 119.9(8) . . ? C119 C111 C101 118.5(9) . . ? C113 C112 N11 121.8(10) . . ? C113 C112 H112 119.1 . . ? N11 C112 H112 119.1 . . ? C112 C113 C114 120.1(9) . . ? C112 C113 H113 119.9 . . ? C114 C113 H113 119.9 . . ? C113 C114 C119 118.1(9) . . ? C113 C114 C115 124.0(9) . . ? C119 C114 C115 117.9(10) . . ? C116 C115 C114 120.8(10) . . ? C116 C115 H115 119.6 . . ? C114 C115 H115 119.6 . . ? C115 C116 C117 120.6(10) . . ? C115 C116 H116 119.7 . . ? C117 C116 H116 119.7 . . ? C118 C117 C116 119.8(13) . . ? C118 C117 H117 120.1 . . ? C116 C117 H117 120.1 . . ? C117 C118 C119 120.9(11) . . ? C117 C118 H118 119.6 . . ? C119 C118 H118 119.6 . . ? C118 C119 C114 119.7(9) . . ? C118 C119 C111 122.1(9) . . ? C114 C119 C111 118.1(10) . . ? C103 C130 C132 113.1(10) . . ? C103 C130 C131 111.7(9) . . ? C132 C130 C131 105.7(9) . . ? C103 C130 C133 111.8(9) . . ? C132 C130 C133 105.7(9) . . ? C131 C130 C133 108.4(10) . . ? C130 C131 H13A 109.5 . . ? C130 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C130 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C130 C132 H13D 109.5 . . ? C130 C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? C130 C132 H13F 109.5 . . ? H13D C132 H13F 109.5 . . ? H13E C132 H13F 109.5 . . ? C130 C133 H13G 109.5 . . ? C130 C133 H13H 109.5 . . ? H13G C133 H13H 109.5 . . ? C130 C133 H13I 109.5 . . ? H13G C133 H13I 109.5 . . ? H13H C133 H13I 109.5 . . ? C107 C170 C172 113.2(10) . . ? C107 C170 C171 109.1(9) . . ? C172 C170 C171 108.5(10) . . ? C107 C170 C173 107.5(9) . . ? C172 C170 C173 109.1(10) . . ? C171 C170 C173 109.4(11) . . ? C170 C171 H17A 109.5 . . ? C170 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C170 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C170 C172 H17D 109.5 . . ? C170 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C170 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C170 C173 H17G 109.5 . . ? C170 C173 H17H 109.5 . . ? H17G C173 H17H 109.5 . . ? C170 C173 H17I 109.5 . . ? H17G C173 H17I 109.5 . . ? H17H C173 H17I 109.5 . . ? C204 C203 H203 128.2 2_765 . ? C203 C204 H204 116.1 2_765 . ? C305 C301 H30A 109.5 . . ? C305 C301 H30B 109.5 . . ? C305 C301 H30C 109.5 . . ? C303 C302 H302 118.8 . . ? C302 C303 C305 125(2) . 2_667 ? C302 C303 H303 117.3 . . ? C305 C303 H303 117.3 2_667 . ? C303 C304 H304 116.2 2_667 . ? C301 C305 C307 123(2) . 2_667 ? C301 C305 C303 123(2) . 2_667 ? C301 C305 C305 177(3) . 2_667 ? C307 C305 C305 54.2(19) 2_667 2_667 ? C303 C305 C305 54.2(19) 2_667 2_667 ? C402 C401 H40A 109.5 . . ? C402 C401 H40B 109.5 . . ? H40A C401 H40B 109.5 . . ? C402 C401 H40C 109.5 . . ? H40A C401 H40C 109.5 . . ? H40B C401 H40C 109.5 . . ? C403 C402 C407 118.5(17) . . ? C403 C402 C401 121.8(19) . . ? C407 C402 C401 119.4(17) . . ? C402 C403 C404 121.4(17) . . ? C402 C403 H403 119.3 . . ? C404 C403 H403 119.3 . . ? C405 C404 C403 118.6(17) . . ? C405 C404 H404 120.7 . . ? C403 C404 H404 120.7 . . ? C404 C405 C406 121(2) . . ? C404 C405 H405 119.5 . . ? C406 C405 H405 119.5 . . ? C407 C406 C405 121.3(18) . . ? C407 C406 H406 119.3 . . ? C405 C406 H406 119.3 . . ? C406 C407 C402 119.1(16) . . ? C406 C407 H407 120.5 . . ? C402 C407 H407 120.5 . . ? 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 Cl1 Pt1 N1 C11 97.0(7) . . . . ? Cl2 Pt1 N1 C11 -81.2(7) . . . . ? Cl1 Pt1 N1 C19 -78.5(6) . . . . ? Cl2 Pt1 N1 C19 103.3(6) . . . . ? C10 C1 C2 O1 178.8(7) . . . . ? C11 C1 C2 O1 -8.5(12) . . . . ? C10 C1 C2 C3 -2.5(13) . . . . ? C11 C1 C2 C3 170.2(8) . . . . ? O1 C2 C3 C4 -179.4(8) . . . . ? C1 C2 C3 C4 1.9(13) . . . . ? O1 C2 C3 C30 1.5(13) . . . . ? C1 C2 C3 C30 -177.2(8) . . . . ? C2 C3 C4 C5 0.2(13) . . . . ? C30 C3 C4 C5 179.3(9) . . . . ? C3 C4 C5 C6 177.9(9) . . . . ? C3 C4 C5 C10 -1.6(13) . . . . ? C10 C5 C6 C7 -1.1(13) . . . . ? C4 C5 C6 C7 179.3(8) . . . . ? C5 C6 C7 C8 0.4(12) . . . . ? C5 C6 C7 C70 -179.3(8) . . . . ? C6 C7 C8 C9 -0.7(13) . . . . ? C70 C7 C8 C9 179.0(8) . . . . ? C7 C8 C9 C10 1.7(13) . . . . ? C2 C1 C10 C9 -179.6(8) . . . . ? C11 C1 C10 C9 7.8(12) . . . . ? C2 C1 C10 C5 1.0(12) . . . . ? C11 C1 C10 C5 -171.6(8) . . . . ? C8 C9 C10 C1 178.3(8) . . . . ? C8 C9 C10 C5 -2.3(12) . . . . ? C6 C5 C10 C1 -178.6(8) . . . . ? C4 C5 C10 C1 1.0(11) . . . . ? C6 C5 C10 C9 2.0(12) . . . . ? C4 C5 C10 C9 -178.4(8) . . . . ? C19 N1 C11 C12 -1.6(12) . . . . ? Pt1 N1 C11 C12 -176.9(6) . . . . ? C19 N1 C11 C1 178.8(7) . . . . ? Pt1 N1 C11 C1 3.5(10) . . . . ? C2 C1 C11 N1 94.5(10) . . . . ? C10 C1 C11 N1 -92.7(10) . . . . ? C2 C1 C11 C12 -85.1(10) . . . . ? C10 C1 C11 C12 87.7(10) . . . . ? N1 C11 C12 C13 -178.8(8) . . . . ? C1 C11 C12 C13 0.8(12) . . . . ? N1 C11 C12 C17 2.7(12) . . . . ? C1 C11 C12 C17 -177.7(7) . . . . ? C11 C12 C13 C14 -179.3(9) . . . . ? C17 C12 C13 C14 -0.7(13) . . . . ? C12 C13 C14 C15 0.7(15) . . . . ? C13 C14 C15 C16 -0.3(15) . . . . ? C14 C15 C16 C17 0.0(15) . . . . ? C15 C16 C17 C18 -178.9(9) . . . . ? C15 C16 C17 C12 0.0(13) . . . . ? C11 C12 C17 C16 179.0(8) . . . . ? C13 C12 C17 C16 0.4(12) . . . . ? C11 C12 C17 C18 -2.0(12) . . . . ? C13 C12 C17 C18 179.4(8) . . . . ? C16 C17 C18 C19 179.4(8) . . . . ? C12 C17 C18 C19 0.4(12) . . . . ? C17 C18 C19 N1 0.7(13) . . . . ? C11 N1 C19 C18 -0.1(13) . . . . ? Pt1 N1 C19 C18 175.7(7) . . . . ? C4 C3 C30 C32 -122.2(10) . . . . ? C2 C3 C30 C32 56.8(12) . . . . ? C4 C3 C30 C31 -1.8(13) . . . . ? C2 C3 C30 C31 177.2(8) . . . . ? C4 C3 C30 C33 115.7(10) . . . . ? C2 C3 C30 C33 -65.2(11) . . . . ? C6 C7 C70 C71 -3.2(13) . . . . ? C8 C7 C70 C71 177.1(9) . . . . ? C6 C7 C70 C72 118.0(10) . . . . ? C8 C7 C70 C72 -61.6(11) . . . . ? C6 C7 C70 C73 -122.4(10) . . . . ? C8 C7 C70 C73 58.0(12) . . . . ? Cl1 Pt1 N11 C111 106.8(8) . . . . ? Cl2 Pt1 N11 C111 -75.1(8) . . . . ? Cl1 Pt1 N11 C112 -65.1(6) . . . . ? Cl2 Pt1 N11 C112 113.1(6) . . . . ? C110 C101 C102 O11 -179.3(9) . . . . ? C111 C101 C102 O11 0.8(14) . . . . ? C110 C101 C102 C103 -2.7(14) . . . . ? C111 C101 C102 C103 177.4(8) . . . . ? O11 C102 C103 C104 -179.1(8) . . . . ? C101 C102 C103 C104 4.1(13) . . . . ? O11 C102 C103 C130 -1.8(13) . . . . ? C101 C102 C103 C130 -178.6(9) . . . . ? C102 C103 C104 C105 -1.1(14) . . . . ? C130 C103 C104 C105 -178.3(9) . . . . ? C103 C104 C105 C106 177.0(9) . . . . ? C103 C104 C105 C110 -3.3(13) . . . . ? C104 C105 C106 C107 176.5(8) . . . . ? C110 C105 C106 C107 -3.1(14) . . . . ? C105 C106 C107 C108 1.3(13) . . . . ? C105 C106 C107 C170 178.6(9) . . . . ? C106 C107 C108 C109 -0.5(14) . . . . ? C170 C107 C108 C109 -177.9(9) . . . . ? C107 C108 C109 C110 1.8(15) . . . . ? C102 C101 C110 C109 178.6(9) . . . . ? C111 C101 C110 C109 -1.5(14) . . . . ? C102 C101 C110 C105 -1.8(14) . . . . ? C111 C101 C110 C105 178.1(8) . . . . ? C108 C109 C110 C101 176.2(9) . . . . ? C108 C109 C110 C105 -3.4(13) . . . . ? C106 C105 C110 C101 -175.6(8) . . . . ? C104 C105 C110 C101 4.7(12) . . . . ? C106 C105 C110 C109 4.0(13) . . . . ? C104 C105 C110 C109 -175.7(8) . . . . ? C112 N11 C111 C119 2.5(15) . . . . ? Pt1 N11 C111 C119 -169.1(8) . . . . ? C112 N11 C111 C101 -175.3(9) . . . . ? Pt1 N11 C111 C101 13.0(13) . . . . ? C102 C101 C111 N11 100.4(12) . . . . ? C110 C101 C111 N11 -79.5(12) . . . . ? C102 C101 C111 C119 -77.5(12) . . . . ? C110 C101 C111 C119 102.6(11) . . . . ? C111 N11 C112 C113 -3.1(14) . . . . ? Pt1 N11 C112 C113 168.9(7) . . . . ? N11 C112 C113 C114 -1.7(14) . . . . ? C112 C113 C114 C119 6.9(15) . . . . ? C112 C113 C114 C115 -175.4(9) . . . . ? C113 C114 C115 C116 179.7(11) . . . . ? C119 C114 C115 C116 -2.5(16) . . . . ? C114 C115 C116 C117 6(2) . . . . ? C115 C116 C117 C118 -4(2) . . . . ? C116 C117 C118 C119 -1(2) . . . . ? C117 C118 C119 C114 4(2) . . . . ? C117 C118 C119 C111 -172.9(13) . . . . ? C113 C114 C119 C118 175.7(11) . . . . ? C115 C114 C119 C118 -2.2(16) . . . . ? C113 C114 C119 C111 -7.3(15) . . . . ? C115 C114 C119 C111 174.8(10) . . . . ? N11 C111 C119 C118 179.7(11) . . . . ? C101 C111 C119 C118 -2.4(17) . . . . ? N11 C111 C119 C114 2.7(16) . . . . ? C101 C111 C119 C114 -179.4(9) . . . . ? C104 C103 C130 C132 -2.5(14) . . . . ? C102 C103 C130 C132 -179.6(9) . . . . ? C104 C103 C130 C131 116.6(11) . . . . ? C102 C103 C130 C131 -60.5(12) . . . . ? C104 C103 C130 C133 -121.8(11) . . . . ? C102 C103 C130 C133 61.1(12) . . . . ? C108 C107 C170 C172 177.1(10) . . . . ? C106 C107 C170 C172 0.0(14) . . . . ? C108 C107 C170 C171 56.1(13) . . . . ? C106 C107 C170 C171 -121.0(11) . . . . ? C108 C107 C170 C173 -62.3(13) . . . . ? C106 C107 C170 C173 120.6(11) . . . . ? C407 C402 C403 C404 -4(2) . . . . ? C401 C402 C403 C404 -177.5(17) . . . . ? C402 C403 C404 C405 2(2) . . . . ? C403 C404 C405 C406 -1(3) . . . . ? C404 C405 C406 C407 1(3) . . . . ? C405 C406 C407 C402 -2(3) . . . . ? C403 C402 C407 C406 4(2) . . . . ? C401 C402 C407 C406 177.6(17) . . . . ? 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 O1 H1 Cl2 0.83(2) 2.72(8) 3.089(7) 109(6) . O11 H11 Cl2 0.86(2) 2.73(7) 3.470(8) 145(11) . _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.64 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.596 _refine_diff_density_min -0.914 _refine_diff_density_rms 0.175 #===END data_12 _database_code_depnum_ccdc_archive 'CCDC 728917' _chemical_formula_structural '[Ti{OPr(i)}2{L(H)}2]' _chemical_formula_moiety '2(C60 H70 N2 O4 Ti), 3(C4 H10 O)' _chemical_formula_sum 'C132 H170 N4 O11 Ti2' _chemical_formula_weight 2084.52 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7337(4) _cell_length_b 16.2802(5) _cell_length_c 42.8540(14) _cell_angle_alpha 96.2270(10) _cell_angle_beta 91.6590(10) _cell_angle_gamma 107.0150(10) _cell_volume 9089.6(5) _cell_formula_units_Z 3 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 36779 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description lath _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3366 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9345 _exptl_absorpt_correction_T_max 0.9962 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 146935 _diffrn_reflns_av_R_equivalents 0.1083 _diffrn_reflns_av_sigmaI/netI 0.1288 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 40617 _reflns_number_gt 23409 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004) ; _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^ > 2\s(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^)+(0.0529P)^2^+15.2065P] 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_number_reflns 40617 _refine_ls_number_parameters 2135 _refine_ls_number_restraints 285 _refine_ls_R_factor_all 0.1684 _refine_ls_R_factor_gt 0.0941 _refine_ls_wR_factor_ref 0.2021 _refine_ls_wR_factor_gt 0.1676 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.023 _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 Ti1 Ti 0.29912(4) 0.34617(4) 0.611695(13) 0.01853(14) Uani 1 1 d . . . N1 N 0.1415(2) 0.37335(18) 0.61205(6) 0.0204(6) Uani 1 1 d . . . O1 O 0.27531(16) 0.34745(14) 0.65654(5) 0.0190(5) Uani 1 1 d . . . C1 C 0.1789(2) 0.4463(2) 0.66551(7) 0.0181(7) Uani 1 1 d . . . C2 C 0.2588(2) 0.4144(2) 0.67424(7) 0.0189(7) Uani 1 1 d . . . C3 C 0.3218(2) 0.4510(2) 0.70311(7) 0.0187(7) Uani 1 1 d . . . C4 C 0.3041(2) 0.5213(2) 0.72010(7) 0.0191(7) Uani 1 1 d . . . H4 H 0.3419 0.5438 0.7397 0.023 Uiso 1 1 calc R . . C5 C 0.2319(2) 0.5621(2) 0.70990(7) 0.0186(7) Uani 1 1 d . . . C6 C 0.2251(3) 0.6405(2) 0.72657(8) 0.0232(7) Uani 1 1 d . . . H6 H 0.2654 0.6628 0.7457 0.028 Uiso 1 1 calc R . . C7 C 0.1623(3) 0.6852(2) 0.71604(8) 0.0243(8) Uani 1 1 d . . . C8 C 0.1029(3) 0.6495(2) 0.68714(8) 0.0243(8) Uani 1 1 d . . . H8 H 0.0603 0.6797 0.6789 0.029 Uiso 1 1 calc R . . C9 C 0.1057(3) 0.5727(2) 0.67095(8) 0.0222(7) Uani 1 1 d . . . H9 H 0.0638 0.5505 0.6521 0.027 Uiso 1 1 calc R . . C10 C 0.1700(2) 0.5253(2) 0.68177(8) 0.0197(7) Uani 1 1 d . . . C11 C 0.1044(2) 0.3976(2) 0.63907(7) 0.0186(7) Uani 1 1 d . . . C12 C 0.0735(3) 0.3320(2) 0.58678(8) 0.0255(8) Uani 1 1 d . . . H12 H 0.1001 0.3204 0.5671 0.031 Uiso 1 1 calc R . . C13 C -0.0297(3) 0.3072(2) 0.58867(8) 0.0279(9) Uani 1 1 d . . . H13 H -0.0732 0.2793 0.5706 0.033 Uiso 1 1 calc R . . C14 C -0.0716(3) 0.3229(2) 0.61750(8) 0.0253(8) Uani 1 1 d . . . C15 C -0.1780(3) 0.2896(2) 0.62180(10) 0.0323(9) Uani 1 1 d . . . H15 H -0.2229 0.2564 0.6047 0.039 Uiso 1 1 calc R . . C16 C -0.2160(3) 0.3048(2) 0.65012(10) 0.0326(9) Uani 1 1 d . . . H16 H -0.2870 0.2823 0.6527 0.039 Uiso 1 1 calc R . . C17 C -0.1496(3) 0.3541(2) 0.67564(9) 0.0286(8) Uani 1 1 d . . . H17 H -0.1766 0.3649 0.6953 0.034 Uiso 1 1 calc R . . C18 C -0.0465(3) 0.3866(2) 0.67253(8) 0.0242(8) Uani 1 1 d . . . H18 H -0.0033 0.4194 0.6900 0.029 Uiso 1 1 calc R . . C19 C -0.0040(2) 0.3717(2) 0.64328(8) 0.0202(7) Uani 1 1 d . . . C30 C 0.4071(2) 0.4132(2) 0.71363(8) 0.0210(7) Uani 1 1 d . . . C31 C 0.4904(3) 0.4279(3) 0.68976(8) 0.0286(8) Uani 1 1 d . . . H31A H 0.5180 0.4900 0.6883 0.043 Uiso 1 1 calc R . . H31B H 0.4610 0.3975 0.6691 0.043 Uiso 1 1 calc R . . H31C H 0.5454 0.4056 0.6967 0.043 Uiso 1 1 calc R . . C32 C 0.3632(3) 0.3161(2) 0.71646(8) 0.0283(8) Uani 1 1 d . . . H32A H 0.4178 0.2937 0.7236 0.042 Uiso 1 1 calc R . . H32B H 0.3334 0.2850 0.6959 0.042 Uiso 1 1 calc R . . H32C H 0.3102 0.3076 0.7317 0.042 Uiso 1 1 calc R . . C33 C 0.4579(3) 0.4572(3) 0.74598(8) 0.0298(9) Uani 1 1 d . . . H33A H 0.4061 0.4506 0.7615 0.045 Uiso 1 1 calc R . . H33B H 0.4907 0.5189 0.7448 0.045 Uiso 1 1 calc R . . H33C H 0.5094 0.4302 0.7522 0.045 Uiso 1 1 calc R . . C70 C 0.1570(3) 0.7723(2) 0.73295(9) 0.0317(9) Uani 1 1 d . . . C71 C 0.2212(4) 0.7978(3) 0.76392(11) 0.0577(15) Uani 1 1 d . . . H71A H 0.2918 0.7998 0.7601 0.087 Uiso 1 1 calc R . . H71B H 0.1939 0.7551 0.7783 0.087 Uiso 1 1 calc R . . H71C H 0.2193 0.8549 0.7733 0.087 Uiso 1 1 calc R . . C72 C 0.1976(5) 0.8412(3) 0.71133(13) 0.0728(17) Uani 1 1 d . . . H72A H 0.1930 0.8970 0.7212 0.109 Uiso 1 1 calc R . . H72B H 0.1569 0.8252 0.6912 0.109 Uiso 1 1 calc R . . H72C H 0.2689 0.8457 0.7076 0.109 Uiso 1 1 calc R . . C73 C 0.0461(4) 0.7669(3) 0.73970(12) 0.0609(15) Uani 1 1 d . . . H73A H 0.0209 0.7236 0.7541 0.091 Uiso 1 1 calc R . . H73B H 0.0035 0.7502 0.7200 0.091 Uiso 1 1 calc R . . H73C H 0.0432 0.8235 0.7494 0.091 Uiso 1 1 calc R . . N11 N 0.1799(2) 0.20884(18) 0.61000(6) 0.0198(6) Uani 1 1 d . . . O11 O 0.26975(17) 0.31909(14) 0.56610(5) 0.0212(5) Uani 1 1 d . . . C101 C 0.2263(2) 0.1666(2) 0.55768(7) 0.0186(7) Uani 1 1 d . . . C102 C 0.2773(2) 0.2470(2) 0.54907(7) 0.0194(7) Uani 1 1 d . . . C103 C 0.3363(2) 0.2536(2) 0.52138(7) 0.0214(7) Uani 1 1 d . . . C104 C 0.3487(3) 0.1776(2) 0.50685(8) 0.0238(8) Uani 1 1 d . . . H104 H 0.3865 0.1804 0.4886 0.029 Uiso 1 1 calc R . . C105 C 0.3087(2) 0.0960(2) 0.51755(7) 0.0215(7) Uani 1 1 d . . . C106 C 0.3281(3) 0.0196(2) 0.50266(8) 0.0241(8) Uani 1 1 d . . . H106 H 0.3696 0.0243 0.4852 0.029 Uiso 1 1 calc R . . C107 C 0.2888(3) -0.0600(2) 0.51272(8) 0.0235(8) Uani 1 1 d . . . C108 C 0.2300(3) -0.0647(2) 0.53931(8) 0.0245(8) Uani 1 1 d . . . H108 H 0.2046 -0.1187 0.5472 0.029 Uiso 1 1 calc R . . C109 C 0.2083(2) 0.0067(2) 0.55404(8) 0.0221(7) Uani 1 1 d . . . H109 H 0.1679 0.0008 0.5718 0.027 Uiso 1 1 calc R . . C110 C 0.2452(2) 0.0891(2) 0.54325(7) 0.0197(7) Uani 1 1 d . . . C111 C 0.1515(2) 0.1602(2) 0.58211(7) 0.0188(7) Uani 1 1 d . . . C112 C 0.0489(2) 0.1036(2) 0.57519(8) 0.0196(7) Uani 1 1 d . . . C113 C 0.0080(3) 0.0679(2) 0.54391(8) 0.0241(8) Uani 1 1 d . . . H113 H 0.0497 0.0804 0.5267 0.029 Uiso 1 1 calc R . . C114 C -0.0903(3) 0.0160(2) 0.53850(8) 0.0288(8) Uani 1 1 d . . . H114 H -0.1169 -0.0061 0.5176 0.035 Uiso 1 1 calc R . . C115 C -0.1525(3) -0.0048(3) 0.56373(9) 0.0328(9) Uani 1 1 d . . . H115 H -0.2198 -0.0432 0.5598 0.039 Uiso 1 1 calc R . . C116 C -0.1172(3) 0.0296(2) 0.59398(8) 0.0267(8) Uani 1 1 d . . . H116 H -0.1601 0.0153 0.6108 0.032 Uiso 1 1 calc R . . C117 C -0.0166(3) 0.0865(2) 0.60019(8) 0.0213(7) Uani 1 1 d . . . C118 C 0.0223(3) 0.1302(2) 0.63046(8) 0.0243(8) Uani 1 1 d . . . H118 H -0.0163 0.1168 0.6482 0.029 Uiso 1 1 calc R . . C119 C 0.1147(3) 0.1909(2) 0.63394(8) 0.0221(7) Uani 1 1 d . . . H119 H 0.1359 0.2232 0.6541 0.027 Uiso 1 1 calc R . . C130 C 0.3829(3) 0.3411(2) 0.50934(8) 0.0254(8) Uani 1 1 d . . . C131 C 0.3009(3) 0.3875(3) 0.50486(9) 0.0320(9) Uani 1 1 d . . . H13A H 0.2473 0.3518 0.4893 0.048 Uiso 1 1 calc R . . H13B H 0.3324 0.4436 0.4975 0.048 Uiso 1 1 calc R . . H13C H 0.2710 0.3965 0.5250 0.048 Uiso 1 1 calc R . . C132 C 0.4696(3) 0.3971(2) 0.53283(9) 0.0321(9) Uani 1 1 d . . . H13D H 0.4425 0.4056 0.5534 0.048 Uiso 1 1 calc R . . H13E H 0.4992 0.4533 0.5254 0.048 Uiso 1 1 calc R . . H13F H 0.5223 0.3680 0.5347 0.048 Uiso 1 1 calc R . . C133 C 0.4286(3) 0.3301(3) 0.47719(9) 0.0361(9) Uani 1 1 d . . . H13G H 0.4857 0.3062 0.4796 0.054 Uiso 1 1 calc R . . H13H H 0.4530 0.3866 0.4694 0.054 Uiso 1 1 calc R . . H13I H 0.3760 0.2907 0.4621 0.054 Uiso 1 1 calc R . . C170 C 0.3024(3) -0.1444(2) 0.49572(8) 0.0290(9) Uani 1 1 d . . . C171 C 0.3600(4) -0.1843(3) 0.51722(10) 0.0455(12) Uani 1 1 d . . . H17A H 0.3654 -0.2389 0.5064 0.068 Uiso 1 1 calc R . . H17B H 0.3235 -0.1954 0.5364 0.068 Uiso 1 1 calc R . . H17C H 0.4285 -0.1444 0.5228 0.068 Uiso 1 1 calc R . . C172 C 0.3594(5) -0.1281(3) 0.46581(12) 0.081(2) Uani 1 1 d . . . H17D H 0.4281 -0.0886 0.4713 0.121 Uiso 1 1 calc R . . H17E H 0.3224 -0.1022 0.4518 0.121 Uiso 1 1 calc R . . H17F H 0.3641 -0.1831 0.4552 0.121 Uiso 1 1 calc R . . C173 C 0.1963(4) -0.2084(3) 0.48674(13) 0.0627(16) Uani 1 1 d . . . H17G H 0.2031 -0.2606 0.4745 0.094 Uiso 1 1 calc R . . H17H H 0.1563 -0.1816 0.4741 0.094 Uiso 1 1 calc R . . H17I H 0.1615 -0.2238 0.5059 0.094 Uiso 1 1 calc R . . O21 O 0.40361(17) 0.30224(15) 0.61367(5) 0.0223(5) Uani 1 1 d . . . C211 C 0.4634(3) 0.2482(2) 0.62092(8) 0.0233(7) Uani 1 1 d . . . H211 H 0.5159 0.2803 0.6381 0.028 Uiso 1 1 calc R . . C212 C 0.3972(3) 0.1664(3) 0.63251(9) 0.0340(9) Uani 1 1 d . . . H21A H 0.3611 0.1821 0.6505 0.051 Uiso 1 1 calc R . . H21B H 0.4402 0.1319 0.6389 0.051 Uiso 1 1 calc R . . H21C H 0.3474 0.1326 0.6156 0.051 Uiso 1 1 calc R . . C213 C 0.5183(3) 0.2285(2) 0.59193(9) 0.0311(9) Uani 1 1 d . . . H21D H 0.4680 0.1947 0.5751 0.047 Uiso 1 1 calc R . . H21E H 0.5643 0.1953 0.5972 0.047 Uiso 1 1 calc R . . H21F H 0.5579 0.2829 0.5848 0.047 Uiso 1 1 calc R . . O31 O 0.35955(17) 0.46060(14) 0.61245(5) 0.0225(5) Uani 1 1 d . . . C311 C 0.3499(3) 0.5454(2) 0.61191(8) 0.0247(8) Uani 1 1 d . . . H311 H 0.2765 0.5424 0.6137 0.030 Uiso 1 1 calc R . . C312 C 0.3833(3) 0.5770(3) 0.58109(9) 0.0361(9) Uani 1 1 d . . . H31D H 0.4550 0.5798 0.5790 0.054 Uiso 1 1 calc R . . H31E H 0.3755 0.6347 0.5805 0.054 Uiso 1 1 calc R . . H31F H 0.3412 0.5370 0.5637 0.054 Uiso 1 1 calc R . . C313 C 0.4123(3) 0.6042(2) 0.64009(9) 0.0337(9) Uani 1 1 d . . . H31G H 0.3877 0.5810 0.6595 0.051 Uiso 1 1 calc R . . H31H H 0.4051 0.6624 0.6402 0.051 Uiso 1 1 calc R . . H31I H 0.4843 0.6071 0.6387 0.051 Uiso 1 1 calc R . . Ti2 Ti 0.30451(4) 0.67256(4) 0.940737(13) 0.01762(14) Uani 1 1 d . . . N41 N 0.1781(2) 0.53918(17) 0.93906(6) 0.0184(6) Uani 1 1 d . . . O41 O 0.26805(16) 0.64735(14) 0.89527(5) 0.0190(5) Uani 1 1 d . . . C401 C 0.2200(2) 0.4941(2) 0.88644(7) 0.0177(7) Uani 1 1 d . . . C402 C 0.2749(2) 0.5748(2) 0.87845(7) 0.0184(7) Uani 1 1 d . . . C403 C 0.3375(2) 0.5812(2) 0.85169(7) 0.0181(7) Uani 1 1 d . . . C404 C 0.3471(2) 0.5048(2) 0.83670(7) 0.0194(7) Uani 1 1 d . . . H404 H 0.3863 0.5076 0.8187 0.023 Uiso 1 1 calc R . . C405 C 0.3024(2) 0.4228(2) 0.84640(7) 0.0184(7) Uani 1 1 d . . . C406 C 0.3214(2) 0.3467(2) 0.83139(8) 0.0224(7) Uani 1 1 d . . . H406 H 0.3632 0.3517 0.8140 0.027 Uiso 1 1 calc R . . C407 C 0.2813(2) 0.2667(2) 0.84115(8) 0.0221(8) Uani 1 1 d . . . C408 C 0.2201(2) 0.2618(2) 0.86737(8) 0.0228(7) Uani 1 1 d . . . H408 H 0.1926 0.2075 0.8749 0.027 Uiso 1 1 calc R . . C409 C 0.1994(3) 0.3337(2) 0.88218(8) 0.0222(7) Uani 1 1 d . . . H409 H 0.1584 0.3276 0.8998 0.027 Uiso 1 1 calc R . . C410 C 0.2375(2) 0.4163(2) 0.87194(7) 0.0187(7) Uani 1 1 d . . . C411 C 0.1468(2) 0.4891(2) 0.91151(7) 0.0178(7) Uani 1 1 d . . . C412 C 0.1167(2) 0.5240(2) 0.96389(8) 0.0206(7) Uani 1 1 d . . . H412 H 0.1399 0.5584 0.9835 0.025 Uiso 1 1 calc R . . C413 C 0.0245(3) 0.4625(2) 0.96176(8) 0.0235(8) Uani 1 1 d . . . H413 H -0.0122 0.4511 0.9800 0.028 Uiso 1 1 calc R . . C414 C -0.0165(2) 0.4154(2) 0.93231(8) 0.0206(7) Uani 1 1 d . . . C415 C -0.1159(3) 0.3551(2) 0.92792(8) 0.0258(8) Uani 1 1 d . . . H415 H -0.1554 0.3419 0.9456 0.031 Uiso 1 1 calc R . . C416 C -0.1551(3) 0.3160(2) 0.89853(8) 0.0266(8) Uani 1 1 d . . . H416 H -0.2208 0.2747 0.8959 0.032 Uiso 1 1 calc R . . C417 C -0.0977(3) 0.3372(2) 0.87211(8) 0.0254(8) Uani 1 1 d . . . H417 H -0.1272 0.3130 0.8516 0.030 Uiso 1 1 calc R . . C418 C -0.0001(3) 0.3921(2) 0.87570(8) 0.0231(8) Uani 1 1 d . . . H418 H 0.0382 0.4041 0.8578 0.028 Uiso 1 1 calc R . . C419 C 0.0442(2) 0.4314(2) 0.90619(7) 0.0188(7) Uani 1 1 d . . . C430 C 0.3945(2) 0.6695(2) 0.84158(8) 0.0212(7) Uani 1 1 d . . . C431 C 0.4800(3) 0.7173(2) 0.86687(8) 0.0265(8) Uani 1 1 d . . . H43A H 0.4501 0.7262 0.8870 0.040 Uiso 1 1 calc R . . H43B H 0.5176 0.7734 0.8606 0.040 Uiso 1 1 calc R . . H43C H 0.5266 0.6825 0.8691 0.040 Uiso 1 1 calc R . . C432 C 0.3204(3) 0.7229(2) 0.83668(9) 0.0284(8) Uani 1 1 d . . . H43D H 0.2885 0.7322 0.8564 0.043 Uiso 1 1 calc R . . H43E H 0.2675 0.6915 0.8202 0.043 Uiso 1 1 calc R . . H43F H 0.3581 0.7789 0.8303 0.043 Uiso 1 1 calc R . . C433 C 0.4442(3) 0.6595(2) 0.81019(8) 0.0277(8) Uani 1 1 d . . . H43G H 0.4777 0.7168 0.8041 0.042 Uiso 1 1 calc R . . H43H H 0.3916 0.6266 0.7939 0.042 Uiso 1 1 calc R . . H43I H 0.4948 0.6286 0.8126 0.042 Uiso 1 1 calc R . . C470 C 0.2992(3) 0.1836(2) 0.82501(8) 0.0281(8) Uani 1 1 d . . . C471 C 0.3493(3) 0.1417(3) 0.84885(9) 0.0367(10) Uani 1 1 d . . . H47A H 0.3613 0.0893 0.8383 0.055 Uiso 1 1 calc R . . H47B H 0.3041 0.1263 0.8659 0.055 Uiso 1 1 calc R . . H47C H 0.4145 0.1826 0.8575 0.055 Uiso 1 1 calc R . . C472 C 0.3689(4) 0.2010(3) 0.79762(10) 0.0500(13) Uani 1 1 d . . . H47D H 0.4341 0.2435 0.8052 0.075 Uiso 1 1 calc R . . H47E H 0.3361 0.2236 0.7813 0.075 Uiso 1 1 calc R . . H47F H 0.3808 0.1469 0.7888 0.075 Uiso 1 1 calc R . . C473 C 0.1944(3) 0.1199(3) 0.81278(12) 0.0524(14) Uani 1 1 d . . . H47G H 0.1614 0.1464 0.7978 0.079 Uiso 1 1 calc R . . H47H H 0.1513 0.1065 0.8305 0.079 Uiso 1 1 calc R . . H47I H 0.2039 0.0666 0.8023 0.079 Uiso 1 1 calc R . . N51 N 0.1518(2) 0.70763(18) 0.94291(6) 0.0206(6) Uani 1 1 d . . . O51 O 0.28780(16) 0.67444(14) 0.98597(5) 0.0193(5) Uani 1 1 d . . . C501 C 0.1997(2) 0.7783(2) 0.99663(7) 0.0188(7) Uani 1 1 d . . . C502 C 0.2779(2) 0.7436(2) 1.00420(7) 0.0185(7) Uani 1 1 d . . . C503 C 0.3459(2) 0.7794(2) 1.03179(7) 0.0198(7) Uani 1 1 d . . . C504 C 0.3362(3) 0.8533(2) 1.04866(8) 0.0224(7) Uani 1 1 d . . . H504 H 0.3786 0.8765 1.0674 0.027 Uiso 1 1 calc R . . C505 C 0.2654(2) 0.8966(2) 1.03936(8) 0.0209(7) Uani 1 1 d . . . C506 C 0.2665(3) 0.9781(2) 1.05557(8) 0.0251(8) Uani 1 1 d . . . H506 H 0.3116 1.0013 1.0737 0.030 Uiso 1 1 calc R . . C507 C 0.2040(3) 1.0246(2) 1.04576(8) 0.0254(8) Uani 1 1 d . . . C508 C 0.1369(3) 0.9871(2) 1.01880(8) 0.0247(8) Uani 1 1 d . . . H508 H 0.0938 1.0179 1.0114 0.030 Uiso 1 1 calc R . . C509 C 0.1321(3) 0.9078(2) 1.00302(8) 0.0242(8) Uani 1 1 d . . . H509 H 0.0852 0.8846 0.9853 0.029 Uiso 1 1 calc R . . C510 C 0.1967(2) 0.8600(2) 1.01293(7) 0.0197(7) Uani 1 1 d . . . C511 C 0.1211(2) 0.7316(2) 0.97113(7) 0.0184(7) Uani 1 1 d . . . C512 C 0.0792(3) 0.6706(2) 0.91843(8) 0.0225(8) Uani 1 1 d . . . H512 H 0.1018 0.6607 0.8980 0.027 Uiso 1 1 calc R . . C513 C -0.0224(3) 0.6476(2) 0.92201(8) 0.0260(8) Uani 1 1 d . . . H513 H -0.0693 0.6234 0.9043 0.031 Uiso 1 1 calc R . . C514 C -0.0585(3) 0.6599(2) 0.95228(8) 0.0234(8) Uani 1 1 d . . . C515 C -0.1623(3) 0.6253(2) 0.95867(9) 0.0300(9) Uani 1 1 d . . . H515 H -0.2108 0.5942 0.9421 0.036 Uiso 1 1 calc R . . C516 C -0.1935(3) 0.6362(3) 0.98829(9) 0.0330(9) Uani 1 1 d . . . H516 H -0.2630 0.6118 0.9924 0.040 Uiso 1 1 calc R . . C517 C -0.1224(3) 0.6836(2) 1.01296(9) 0.0310(9) Uani 1 1 d . . . H517 H -0.1450 0.6920 1.0335 0.037 Uiso 1 1 calc R . . C518 C -0.0213(3) 0.7178(2) 1.00790(8) 0.0248(8) Uani 1 1 d . . . H518 H 0.0253 0.7493 1.0249 0.030 Uiso 1 1 calc R . . C519 C 0.0144(2) 0.7065(2) 0.97727(8) 0.0195(7) Uani 1 1 d . . . C530 C 0.4283(3) 0.7377(2) 1.04140(8) 0.0226(8) Uani 1 1 d . . . C531 C 0.3788(3) 0.6412(2) 1.04493(9) 0.0287(8) Uani 1 1 d . . . H53A H 0.3451 0.6104 1.0247 0.043 Uiso 1 1 calc R . . H53B H 0.3283 0.6360 1.0609 0.043 Uiso 1 1 calc R . . H53C H 0.4316 0.6158 1.0514 0.043 Uiso 1 1 calc R . . C532 C 0.5086(3) 0.7477(3) 1.01660(8) 0.0295(9) Uani 1 1 d . . . H53D H 0.5605 0.7209 1.0227 0.044 Uiso 1 1 calc R . . H53E H 0.5410 0.8093 1.0153 0.044 Uiso 1 1 calc R . . H53F H 0.4754 0.7192 0.9961 0.044 Uiso 1 1 calc R . . C533 C 0.4841(3) 0.7813(3) 1.07347(8) 0.0317(9) Uani 1 1 d . . . H53G H 0.5317 0.7504 1.0796 0.048 Uiso 1 1 calc R . . H53H H 0.4340 0.7795 1.0894 0.048 Uiso 1 1 calc R . . H53I H 0.5219 0.8416 1.0717 0.048 Uiso 1 1 calc R . . C570 C 0.2078(3) 1.1149(2) 1.06177(9) 0.0333(9) Uani 1 1 d . . . C571 C 0.2452(5) 1.1799(3) 1.03821(13) 0.0670(16) Uani 1 1 d . . . H57A H 0.2476 1.2379 1.0478 0.101 Uiso 1 1 calc R . . H57B H 0.1983 1.1636 1.0194 0.101 Uiso 1 1 calc R . . H57C H 0.3136 1.1797 1.0324 0.101 Uiso 1 1 calc R . . C572 C 0.2792(4) 1.1419(3) 1.09152(11) 0.0596(16) Uani 1 1 d . . . H57D H 0.3486 1.1436 1.0861 0.089 Uiso 1 1 calc R . . H57E H 0.2558 1.1001 1.1065 0.089 Uiso 1 1 calc R . . H57F H 0.2791 1.1995 1.1010 0.089 Uiso 1 1 calc R . . C573 C 0.1003(3) 1.1155(3) 1.07070(12) 0.0529(13) Uani 1 1 d . . . H57G H 0.0767 1.0752 1.0862 0.079 Uiso 1 1 calc R . . H57H H 0.0534 1.0977 1.0519 0.079 Uiso 1 1 calc R . . H57I H 0.1024 1.1740 1.0797 0.079 Uiso 1 1 calc R . . O22 O 0.37247(17) 0.78477(14) 0.94152(5) 0.0240(5) Uani 1 1 d . . . C221 C 0.3691(4) 0.8719(3) 0.94168(11) 0.0535(13) Uani 1 1 d . . . H221 H 0.2981 0.8709 0.9466 0.064 Uiso 1 1 calc R . . C222 C 0.3848(6) 0.9027(3) 0.91190(12) 0.092(2) Uani 1 1 d . . . H22A H 0.4536 0.9046 0.9059 0.138 Uiso 1 1 calc R . . H22B H 0.3771 0.9609 0.9132 0.138 Uiso 1 1 calc R . . H22C H 0.3344 0.8638 0.8961 0.138 Uiso 1 1 calc R . . C223 C 0.4384(4) 0.9293(3) 0.96857(11) 0.0534(13) Uani 1 1 d . . . H22D H 0.5086 0.9280 0.9659 0.080 Uiso 1 1 calc R . . H22E H 0.4160 0.9083 0.9885 0.080 Uiso 1 1 calc R . . H22F H 0.4356 0.9888 0.9687 0.080 Uiso 1 1 calc R . . O32 O 0.40214(17) 0.62001(15) 0.93970(5) 0.0224(5) Uani 1 1 d . . . C321 C 0.4446(2) 0.5497(2) 0.93639(9) 0.0255(8) Uani 1 1 d . . . H321 H 0.4292 0.5204 0.9143 0.031 Uiso 1 1 calc R . . C322 C 0.5599(3) 0.5864(2) 0.94255(9) 0.0316(9) Uani 1 1 d . . . H32D H 0.5873 0.6273 0.9275 0.047 Uiso 1 1 calc R . . H32E H 0.5908 0.5391 0.9401 0.047 Uiso 1 1 calc R . . H32F H 0.5758 0.6163 0.9640 0.047 Uiso 1 1 calc R . . C323 C 0.3970(3) 0.4851(3) 0.95856(13) 0.0535(13) Uani 1 1 d . . . H32G H 0.4135 0.5126 0.9803 0.080 Uiso 1 1 calc R . . H32H H 0.4240 0.4355 0.9554 0.080 Uiso 1 1 calc R . . H32I H 0.3228 0.4652 0.9543 0.080 Uiso 1 1 calc R . . Ti3 Ti 0.68892(4) 0.99514(4) 0.721639(14) 0.01889(14) Uani 1 1 d . . . N61 N 0.80809(19) 1.13172(17) 0.72536(6) 0.0163(6) Uani 1 1 d . . . O61 O 0.72700(17) 1.01347(14) 0.76663(5) 0.0203(5) Uani 1 1 d . . . C601 C 0.7662(2) 1.1651(2) 0.77901(7) 0.0185(7) Uani 1 1 d . . . C602 C 0.7152(2) 1.0813(2) 0.78532(8) 0.0195(7) Uani 1 1 d . . . C603 C 0.6508(2) 1.0670(2) 0.81139(8) 0.0207(7) Uani 1 1 d . . . C604 C 0.6352(2) 1.1392(2) 0.82784(8) 0.0218(7) Uani 1 1 d . . . H604 H 0.5939 1.1312 0.8453 0.026 Uiso 1 1 calc R . . C605 C 0.6769(2) 1.2245(2) 0.82031(8) 0.0196(7) Uani 1 1 d . . . C606 C 0.6512(2) 1.2952(2) 0.83692(8) 0.0207(7) Uani 1 1 d . . . H606 H 0.6066 1.2844 0.8535 0.025 Uiso 1 1 calc R . . C607 C 0.6888(2) 1.3786(2) 0.82977(7) 0.0201(7) Uani 1 1 d . . . C608 C 0.7551(2) 1.3920(2) 0.80482(8) 0.0216(7) Uani 1 1 d . . . H608 H 0.7821 1.4489 0.7993 0.026 Uiso 1 1 calc R . . C609 C 0.7815(2) 1.3251(2) 0.78827(8) 0.0208(7) Uani 1 1 d . . . H609 H 0.8254 1.3369 0.7715 0.025 Uiso 1 1 calc R . . C610 C 0.7445(2) 1.2389(2) 0.79575(7) 0.0185(7) Uani 1 1 d . . . C611 C 0.8386(2) 1.1767(2) 0.75387(7) 0.0184(7) Uani 1 1 d . . . C612 C 0.8695(2) 1.1527(2) 0.70069(7) 0.0206(7) Uani 1 1 d . . . H612 H 0.8470 1.1214 0.6805 0.025 Uiso 1 1 calc R . . C613 C 0.9605(3) 1.2159(2) 0.70395(8) 0.0218(7) Uani 1 1 d . . . H613 H 0.9970 1.2320 0.6860 0.026 Uiso 1 1 calc R . . C614 C 1.0005(2) 1.2576(2) 0.73427(8) 0.0207(7) Uani 1 1 d . . . C615 C 1.0993(3) 1.3200(2) 0.73959(8) 0.0263(8) Uani 1 1 d . . . H615 H 1.1379 1.3391 0.7223 0.032 Uiso 1 1 calc R . . C616 C 1.1381(3) 1.3520(2) 0.76991(9) 0.0310(9) Uani 1 1 d . . . H616 H 1.2038 1.3931 0.7735 0.037 Uiso 1 1 calc R . . C617 C 1.0808(3) 1.3243(2) 0.79579(8) 0.0271(8) Uani 1 1 d . . . H617 H 1.1100 1.3442 0.8166 0.032 Uiso 1 1 calc R . . C618 C 0.9841(2) 1.2691(2) 0.79104(8) 0.0218(7) Uani 1 1 d . . . H618 H 0.9456 1.2528 0.8086 0.026 Uiso 1 1 calc R . . C619 C 0.9401(2) 1.2357(2) 0.76005(7) 0.0178(7) Uani 1 1 d . . . C630 C 0.5983(3) 0.9751(2) 0.81927(8) 0.0260(8) Uani 1 1 d . . . C631 C 0.5142(3) 0.9285(3) 0.79342(9) 0.0365(9) Uani 1 1 d . . . H63A H 0.4798 0.8700 0.7983 0.055 Uiso 1 1 calc R . . H63B H 0.5448 0.9249 0.7731 0.055 Uiso 1 1 calc R . . H63C H 0.4646 0.9609 0.7923 0.055 Uiso 1 1 calc R . . C632 C 0.6759(3) 0.9238(3) 0.82196(9) 0.0346(9) Uani 1 1 d . . . H63D H 0.7310 0.9557 0.8377 0.052 Uiso 1 1 calc R . . H63E H 0.7044 0.9161 0.8015 0.052 Uiso 1 1 calc R . . H63F H 0.6416 0.8670 0.8284 0.052 Uiso 1 1 calc R . . C633 C 0.5479(3) 0.9768(3) 0.85065(9) 0.0346(9) Uani 1 1 d . . . H63G H 0.5996 1.0074 0.8675 0.052 Uiso 1 1 calc R . . H63H H 0.5160 0.9174 0.8551 0.052 Uiso 1 1 calc R . . H63I H 0.4957 1.0067 0.8494 0.052 Uiso 1 1 calc R . . C670 C 0.6621(3) 1.4556(2) 0.84772(8) 0.0234(8) Uani 1 1 d . . . C671 C 0.6216(3) 1.5045(2) 0.82408(9) 0.0317(9) Uani 1 1 d . . . H67A H 0.5593 1.4657 0.8127 0.048 Uiso 1 1 calc R . . H67B H 0.6733 1.5243 0.8091 0.048 Uiso 1 1 calc R . . H67C H 0.6065 1.5545 0.8354 0.048 Uiso 1 1 calc R . . C672 C 0.7599(3) 1.5171(2) 0.86543(9) 0.0340(9) Uani 1 1 d . . . H67D H 0.7440 1.5663 0.8771 0.051 Uiso 1 1 calc R . . H67E H 0.8108 1.5381 0.8503 0.051 Uiso 1 1 calc R . . H67F H 0.7870 1.4859 0.8802 0.051 Uiso 1 1 calc R . . C673 C 0.5811(3) 1.4272(3) 0.87121(8) 0.0325(9) Uani 1 1 d . . . H67G H 0.5629 1.4776 0.8808 0.049 Uiso 1 1 calc R . . H67H H 0.6081 1.4007 0.8876 0.049 Uiso 1 1 calc R . . H67I H 0.5203 1.3849 0.8603 0.049 Uiso 1 1 calc R . . N71 N 0.8455(2) 0.96732(18) 0.71798(6) 0.0212(6) Uani 1 1 d . . . O71 O 0.70572(17) 0.99759(14) 0.67618(5) 0.0209(5) Uani 1 1 d . . . C701 C 0.7868(2) 0.8881(2) 0.66622(7) 0.0190(7) Uani 1 1 d . . . C702 C 0.7110(2) 0.9253(2) 0.65859(7) 0.0187(7) Uani 1 1 d . . . C703 C 0.6388(2) 0.8875(2) 0.63195(7) 0.0197(7) Uani 1 1 d . . . C704 C 0.6426(3) 0.8095(2) 0.61675(8) 0.0232(8) Uani 1 1 d . . . H704 H 0.5974 0.7847 0.5987 0.028 Uiso 1 1 calc R . . C705 C 0.7098(2) 0.7641(2) 0.62639(7) 0.0198(7) Uani 1 1 d . . . C706 C 0.7029(3) 0.6790(2) 0.61241(8) 0.0220(7) Uani 1 1 d . . . H706 H 0.6553 0.6540 0.5950 0.026 Uiso 1 1 calc R . . C707 C 0.7620(3) 0.6315(2) 0.62304(8) 0.0228(7) Uani 1 1 d . . . C708 C 0.8325(3) 0.6706(2) 0.64909(8) 0.0240(8) Uani 1 1 d . . . H708 H 0.8730 0.6386 0.6573 0.029 Uiso 1 1 calc R . . C709 C 0.8438(3) 0.7536(2) 0.66281(8) 0.0236(8) Uani 1 1 d . . . H709 H 0.8929 0.7779 0.6799 0.028 Uiso 1 1 calc R . . C710 C 0.7835(2) 0.8038(2) 0.65186(7) 0.0187(7) Uani 1 1 d . . . C711 C 0.8705(2) 0.9371(2) 0.69004(8) 0.0196(7) Uani 1 1 d . . . C712 C 0.9224(3) 1.0085(2) 0.74072(8) 0.0262(8) Uani 1 1 d . . . H712 H 0.9041 1.0235 0.7613 0.031 Uiso 1 1 calc R . . C713 C 1.0231(3) 1.0286(2) 0.73515(9) 0.0290(9) Uani 1 1 d . . . H713 H 1.0732 1.0573 0.7516 0.035 Uiso 1 1 calc R . . C714 C 1.0536(3) 1.0070(2) 0.70489(8) 0.0261(8) Uani 1 1 d . . . C715 C 1.1562(3) 1.0333(2) 0.69652(10) 0.0320(9) Uani 1 1 d . . . H715 H 1.2080 1.0685 0.7115 0.038 Uiso 1 1 calc R . . C716 C 1.1814(3) 1.0088(3) 0.66721(10) 0.0347(9) Uani 1 1 d . . . H716 H 1.2507 1.0260 0.6621 0.042 Uiso 1 1 calc R . . C717 C 1.1052(3) 0.9579(3) 0.64444(9) 0.0332(9) Uani 1 1 d . . . H717 H 1.1236 0.9405 0.6241 0.040 Uiso 1 1 calc R . . C718 C 1.0047(3) 0.9334(2) 0.65142(8) 0.0255(8) Uani 1 1 d . . . H718 H 0.9540 0.9004 0.6357 0.031 Uiso 1 1 calc R . . C719 C 0.9756(3) 0.9568(2) 0.68193(8) 0.0223(7) Uani 1 1 d . . . C730 C 0.5586(3) 0.9313(2) 0.62219(8) 0.0237(8) Uani 1 1 d . . . C731 C 0.6118(3) 1.0265(2) 0.61692(9) 0.0302(9) Uani 1 1 d . . . H73D H 0.5606 1.0529 0.6100 0.045 Uiso 1 1 calc R . . H73E H 0.6613 1.0277 0.6008 0.045 Uiso 1 1 calc R . . H73F H 0.6473 1.0590 0.6367 0.045 Uiso 1 1 calc R . . C732 C 0.4816(3) 0.9276(3) 0.64767(9) 0.0304(9) Uani 1 1 d . . . H73G H 0.4306 0.9550 0.6413 0.046 Uiso 1 1 calc R . . H73H H 0.5174 0.9583 0.6676 0.046 Uiso 1 1 calc R . . H73I H 0.4476 0.8670 0.6503 0.046 Uiso 1 1 calc R . . C733 C 0.4997(3) 0.8858(3) 0.59095(9) 0.0351(10) Uani 1 1 d . . . H73J H 0.4633 0.8255 0.5933 0.053 Uiso 1 1 calc R . . H73K H 0.5477 0.8872 0.5744 0.053 Uiso 1 1 calc R . . H73L H 0.4505 0.9156 0.5852 0.053 Uiso 1 1 calc R . . C770 C 0.7486(3) 0.5371(2) 0.60903(8) 0.0256(8) Uani 1 1 d . . . C771 C 0.6727(3) 0.4770(3) 0.62799(12) 0.0530(13) Uani 1 1 d . . . H77A H 0.6070 0.4890 0.6266 0.079 Uiso 1 1 calc R . . H77B H 0.6987 0.4866 0.6500 0.079 Uiso 1 1 calc R . . H77C H 0.6637 0.4167 0.6195 0.079 Uiso 1 1 calc R . . C772 C 0.7086(4) 0.5214(3) 0.57456(10) 0.0557(14) Uani 1 1 d . . . H77D H 0.7045 0.4622 0.5658 0.084 Uiso 1 1 calc R . . H77E H 0.7550 0.5627 0.5627 0.084 Uiso 1 1 calc R . . H77F H 0.6406 0.5292 0.5731 0.084 Uiso 1 1 calc R . . C773 C 0.8503(3) 0.5161(2) 0.61049(10) 0.0369(10) Uani 1 1 d . . . H77G H 0.8732 0.5183 0.6325 0.055 Uiso 1 1 calc R . . H77H H 0.9014 0.5586 0.6003 0.055 Uiso 1 1 calc R . . H77I H 0.8411 0.4580 0.5996 0.055 Uiso 1 1 calc R . . O23 O 0.62310(17) 0.88258(15) 0.71877(6) 0.0254(5) Uani 1 1 d . . . C231 C 0.5949(3) 0.7909(2) 0.71203(10) 0.0388(10) Uani 1 1 d . . . H231 H 0.6063 0.7754 0.6895 0.047 Uiso 1 1 calc R . . C232 C 0.4832(4) 0.7539(3) 0.71722(11) 0.0572(14) Uani 1 1 d . . . H23A H 0.4721 0.7655 0.7395 0.086 Uiso 1 1 calc R . . H23B H 0.4618 0.6913 0.7108 0.086 Uiso 1 1 calc R . . H23C H 0.4432 0.7809 0.7046 0.086 Uiso 1 1 calc R . . C233 C 0.6637(4) 0.7576(3) 0.73295(15) 0.0723(17) Uani 1 1 d . . . H23D H 0.7347 0.7806 0.7277 0.108 Uiso 1 1 calc R . . H23E H 0.6430 0.6943 0.7295 0.108 Uiso 1 1 calc R . . H23F H 0.6573 0.7768 0.7551 0.108 Uiso 1 1 calc R . . O33 O 0.58921(17) 1.04601(15) 0.72419(5) 0.0239(5) Uani 1 1 d . . . C331 C 0.5438(3) 1.1139(2) 0.72908(9) 0.0299(9) Uani 1 1 d . . . H331 H 0.5578 1.1396 0.7516 0.036 Uiso 1 1 calc R . . C332 C 0.5909(3) 1.1839(3) 0.70855(12) 0.0499(12) Uani 1 1 d . . . H33D H 0.6643 1.2073 0.7141 0.075 Uiso 1 1 calc R . . H33E H 0.5590 1.2305 0.7120 0.075 Uiso 1 1 calc R . . H33F H 0.5796 1.1592 0.6864 0.075 Uiso 1 1 calc R . . C333 C 0.4293(3) 1.0767(3) 0.72241(10) 0.0363(10) Uani 1 1 d . . . H33G H 0.4146 1.0498 0.7005 0.055 Uiso 1 1 calc R . . H33H H 0.3975 1.1232 0.7259 0.055 Uiso 1 1 calc R . . H33I H 0.4020 1.0331 0.7365 0.055 Uiso 1 1 calc R . . C811 C 0.0991(4) 0.7394(3) 0.60627(12) 0.0541(12) Uani 1 1 d DU . . H81A H 0.0714 0.6758 0.6014 0.065 Uiso 1 1 calc R . . H81B H 0.0680 0.7578 0.6253 0.065 Uiso 1 1 calc R . . C812 C 0.2132(4) 0.7649(4) 0.61209(13) 0.0621(14) Uani 1 1 d DU . . H81C H 0.2435 0.7459 0.5932 0.093 Uiso 1 1 calc R . . H81D H 0.2303 0.7374 0.6298 0.093 Uiso 1 1 calc R . . H81E H 0.2401 0.8279 0.6170 0.093 Uiso 1 1 calc R . . C813 C -0.0317(3) 0.7584(3) 0.57317(12) 0.0553(13) Uani 1 1 d DU . . H81F H -0.0658 0.7754 0.5918 0.066 Uiso 1 1 calc R . . H81G H -0.0604 0.6951 0.5674 0.066 Uiso 1 1 calc R . . C814 C -0.0507(4) 0.8042(4) 0.54657(16) 0.0816(19) Uani 1 1 d DU . . H81H H -0.0193 0.8667 0.5520 0.122 Uiso 1 1 calc R . . H81I H -0.1243 0.7921 0.5423 0.122 Uiso 1 1 calc R . . H81J H -0.0209 0.7842 0.5278 0.122 Uiso 1 1 calc R . . O81 O 0.0752(2) 0.7799(2) 0.58061(8) 0.0473(8) Uani 1 1 d DU . . C821 C 1.0169(4) 0.5468(3) 0.78932(14) 0.0612(14) Uani 1 1 d U . . H82A H 1.0763 0.5745 0.7776 0.073 Uiso 1 1 calc R . . H82B H 1.0070 0.4836 0.7868 0.073 Uiso 1 1 calc R . . C822 C 1.0361(4) 0.5820(4) 0.82350(14) 0.0763(17) Uani 1 1 d U . . H82C H 1.0443 0.6442 0.8259 0.114 Uiso 1 1 calc R . . H82D H 1.0984 0.5721 0.8318 0.114 Uiso 1 1 calc R . . H82E H 0.9782 0.5526 0.8351 0.114 Uiso 1 1 calc R . . C823 C 0.9014(5) 0.5328(3) 0.74504(12) 0.0696(15) Uani 1 1 d U . . H82F H 0.8881 0.4693 0.7419 0.084 Uiso 1 1 calc R . . H82G H 0.9587 0.5593 0.7323 0.084 Uiso 1 1 calc R . . C824 C 0.8078(5) 0.5553(5) 0.73478(14) 0.098(2) Uani 1 1 d U . . H82H H 0.7508 0.5275 0.7470 0.147 Uiso 1 1 calc R . . H82I H 0.7904 0.5348 0.7124 0.147 Uiso 1 1 calc R . . H82J H 0.8211 0.6182 0.7382 0.147 Uiso 1 1 calc R . . O82 O 0.9269(2) 0.5641(2) 0.77702(7) 0.0475(8) Uani 1 1 d U . . C831 C 0.1162(5) 0.1081(4) 0.93318(13) 0.0763(17) Uani 1 1 d U . . H83A H 0.0677 0.0900 0.9495 0.092 Uiso 1 1 calc R . . H83B H 0.1512 0.1708 0.9382 0.092 Uiso 1 1 calc R . . C832 C 0.1925(5) 0.0597(5) 0.93309(14) 0.0869(19) Uani 1 1 d U . . H83C H 0.1576 -0.0024 0.9283 0.130 Uiso 1 1 calc R . . H83D H 0.2292 0.0712 0.9538 0.130 Uiso 1 1 calc R . . H83E H 0.2410 0.0783 0.9171 0.130 Uiso 1 1 calc R . . C833 C -0.0179(4) 0.1303(4) 0.90232(17) 0.0817(18) Uani 1 1 d U . . H83F H 0.0099 0.1939 0.9075 0.098 Uiso 1 1 calc R . . H83G H -0.0677 0.1080 0.9179 0.098 Uiso 1 1 calc R . . C834 C -0.0687(5) 0.1087(4) 0.8702(2) 0.101(2) Uani 1 1 d U . . H83H H -0.0197 0.1334 0.8550 0.151 Uiso 1 1 calc R . . H83I H -0.1263 0.1326 0.8694 0.151 Uiso 1 1 calc R . . H83J H -0.0936 0.0456 0.8649 0.151 Uiso 1 1 calc R . . O83 O 0.0622(3) 0.0917(2) 0.90320(9) 0.0626(9) Uani 1 1 d U . . C841 C 0.1134(5) 0.1859(4) 0.17759(19) 0.089(2) Uani 1 1 d U . . H84A H 0.1388 0.1424 0.1652 0.107 Uiso 1 1 calc R . . H84B H 0.1000 0.1675 0.1987 0.107 Uiso 1 1 calc R . . C842 C 0.1918(5) 0.2705(4) 0.18064(18) 0.091(2) Uani 1 1 d U . . H84C H 0.2061 0.2883 0.1597 0.137 Uiso 1 1 calc R . . H84D H 0.2543 0.2663 0.1910 0.137 Uiso 1 1 calc R . . H84E H 0.1672 0.3135 0.1932 0.137 Uiso 1 1 calc R . . C843 C -0.0548(5) 0.1117(4) 0.15784(18) 0.090(2) Uani 1 1 d U . . H84F H -0.0695 0.0884 0.1782 0.108 Uiso 1 1 calc R . . H84G H -0.0316 0.0695 0.1439 0.108 Uiso 1 1 calc R . . C844 C -0.1475(5) 0.1208(5) 0.14377(19) 0.112(3) Uani 1 1 d U . . H84H H -0.1703 0.1630 0.1574 0.168 Uiso 1 1 calc R . . H84I H -0.2005 0.0647 0.1413 0.168 Uiso 1 1 calc R . . H84J H -0.1344 0.1408 0.1231 0.168 Uiso 1 1 calc R . . O84 O 0.0228(3) 0.1892(2) 0.16293(10) 0.0737(11) Uani 1 1 d U . . C851 C -0.016(3) 0.526(3) 0.4710(6) 0.121(10) Uani 0.222(13) 1 d PDU A 1 H85A H 0.0482 0.5364 0.4599 0.145 Uiso 0.222(13) 1 calc PR A 1 H85B H -0.0331 0.5809 0.4742 0.145 Uiso 0.222(13) 1 calc PR A 1 C852 C -0.100(8) 0.459(6) 0.4510(16) 0.11(2) Uani 0.222(13) 1 d PDU A 1 H85C H -0.0976 0.4009 0.4544 0.169 Uiso 0.222(13) 1 calc PR A 1 H85D H -0.0914 0.4665 0.4288 0.169 Uiso 0.222(13) 1 calc PR A 1 H85E H -0.1661 0.4654 0.4568 0.169 Uiso 0.222(13) 1 calc PR A 1 C853 C 0.086(3) 0.558(2) 0.5182(8) 0.109(10) Uani 0.222(13) 1 d PDU A 1 H85F H 0.0720 0.6142 0.5243 0.130 Uiso 0.222(13) 1 calc PR A 1 H85G H 0.1464 0.5694 0.5056 0.130 Uiso 0.222(13) 1 calc PR A 1 C854 C 0.105(7) 0.520(5) 0.5469(14) 0.105(18) Uani 0.222(13) 1 d PDU A 1 H85H H 0.0416 0.4993 0.5572 0.157 Uiso 0.222(13) 1 calc PR A 1 H85I H 0.1550 0.5645 0.5614 0.157 Uiso 0.222(13) 1 calc PR A 1 H85J H 0.1328 0.4719 0.5410 0.157 Uiso 0.222(13) 1 calc PR A 1 O85 O 0.0000 0.5000 0.5000 0.084(6) Uani 0.44(3) 2 d SPDU A 1 C861 C -0.084(2) 0.507(3) 0.4833(7) 0.109(8) Uani 0.278(13) 1 d PDU A 2 H86A H -0.0796 0.5685 0.4833 0.131 Uiso 0.278(13) 1 calc PR A 2 H86B H -0.1468 0.4789 0.4938 0.131 Uiso 0.278(13) 1 calc PR A 2 C862 C -0.093(5) 0.464(4) 0.4498(8) 0.095(14) Uani 0.278(13) 1 d PDU A 2 H86C H -0.1472 0.4784 0.4379 0.142 Uiso 0.278(13) 1 calc PR A 2 H86D H -0.1106 0.4015 0.4496 0.142 Uiso 0.278(13) 1 calc PR A 2 H86E H -0.0283 0.4858 0.4402 0.142 Uiso 0.278(13) 1 calc PR A 2 C863 C 0.036(2) 0.557(2) 0.5279(6) 0.110(8) Uani 0.278(13) 1 d PDU A 2 H86F H 0.0027 0.5306 0.5461 0.132 Uiso 0.278(13) 1 calc PR A 2 H86G H 0.0184 0.6117 0.5265 0.132 Uiso 0.278(13) 1 calc PR A 2 C864 C 0.148(2) 0.575(3) 0.5320(10) 0.161(15) Uani 0.278(13) 1 d PDU A 2 H86H H 0.1638 0.5343 0.5450 0.241 Uiso 0.278(13) 1 calc PR A 2 H86I H 0.1786 0.6346 0.5424 0.241 Uiso 0.278(13) 1 calc PR A 2 H86J H 0.1761 0.5695 0.5114 0.241 Uiso 0.278(13) 1 calc PR A 2 O86 O 0.0000 0.5000 0.5000 0.104(6) Uani 0.56(3) 2 d SPDU 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 Ti1 0.0191(3) 0.0177(3) 0.0175(3) -0.0008(2) -0.0005(2) 0.0047(2) N1 0.0243(15) 0.0210(15) 0.0160(13) -0.0017(12) -0.0041(11) 0.0089(12) O1 0.0208(12) 0.0179(12) 0.0182(11) 0.0008(9) -0.0004(9) 0.0063(10) C1 0.0187(17) 0.0176(16) 0.0163(15) 0.0011(13) -0.0002(13) 0.0034(14) C2 0.0216(17) 0.0181(17) 0.0150(15) 0.0015(13) 0.0019(13) 0.0029(14) C3 0.0183(17) 0.0188(17) 0.0191(16) 0.0038(13) -0.0017(13) 0.0054(14) C4 0.0199(17) 0.0203(17) 0.0152(15) -0.0005(13) -0.0018(13) 0.0041(14) C5 0.0216(17) 0.0192(17) 0.0137(15) 0.0018(13) -0.0009(13) 0.0042(14) C6 0.0266(19) 0.0198(17) 0.0208(17) -0.0002(14) -0.0015(14) 0.0047(15) C7 0.0293(19) 0.0173(17) 0.0242(18) -0.0004(14) -0.0042(15) 0.0054(15) C8 0.0270(19) 0.0254(19) 0.0229(17) 0.0008(15) -0.0049(14) 0.0127(16) C9 0.0218(18) 0.0203(17) 0.0231(17) -0.0003(14) -0.0032(14) 0.0057(14) C10 0.0156(16) 0.0183(17) 0.0232(17) 0.0018(14) -0.0014(13) 0.0024(13) C11 0.0229(17) 0.0154(16) 0.0178(16) 0.0011(13) -0.0016(13) 0.0070(14) C12 0.029(2) 0.031(2) 0.0170(16) -0.0036(15) -0.0059(14) 0.0121(16) C13 0.028(2) 0.028(2) 0.0268(19) -0.0082(16) -0.0125(15) 0.0122(16) C14 0.0264(19) 0.0181(18) 0.0306(19) -0.0005(15) -0.0068(15) 0.0073(15) C15 0.0205(19) 0.028(2) 0.044(2) -0.0021(18) -0.0097(17) 0.0041(16) C16 0.0197(19) 0.027(2) 0.049(2) 0.0087(18) -0.0027(17) 0.0041(16) C17 0.0257(19) 0.030(2) 0.033(2) 0.0062(16) 0.0060(16) 0.0119(16) C18 0.0210(18) 0.0245(19) 0.0270(18) 0.0019(15) -0.0008(14) 0.0072(15) C19 0.0198(17) 0.0158(16) 0.0245(17) 0.0017(14) -0.0025(14) 0.0050(14) C30 0.0192(17) 0.0243(18) 0.0196(16) 0.0008(14) -0.0021(13) 0.0076(14) C31 0.0227(19) 0.039(2) 0.0245(18) -0.0022(16) -0.0049(15) 0.0129(17) C32 0.032(2) 0.030(2) 0.0270(19) 0.0042(16) -0.0036(16) 0.0155(17) C33 0.032(2) 0.040(2) 0.0225(18) -0.0003(16) -0.0047(15) 0.0195(18) C70 0.046(2) 0.0232(19) 0.029(2) -0.0016(16) -0.0100(17) 0.0173(18) C71 0.084(4) 0.041(3) 0.050(3) -0.024(2) -0.029(3) 0.036(3) C72 0.125(5) 0.026(3) 0.068(4) 0.004(2) 0.010(3) 0.023(3) C73 0.061(3) 0.055(3) 0.069(3) -0.029(3) -0.015(3) 0.035(3) N11 0.0188(14) 0.0200(15) 0.0199(14) -0.0004(12) 0.0016(11) 0.0057(12) O11 0.0265(13) 0.0190(12) 0.0168(11) -0.0011(10) 0.0006(9) 0.0061(10) C101 0.0178(16) 0.0201(17) 0.0163(16) 0.0002(13) 0.0016(13) 0.0038(14) C102 0.0191(17) 0.0235(18) 0.0149(15) -0.0003(14) -0.0024(13) 0.0067(14) C103 0.0206(17) 0.0248(18) 0.0172(16) 0.0021(14) 0.0007(13) 0.0046(15) C104 0.0235(18) 0.0276(19) 0.0201(17) 0.0000(15) 0.0021(14) 0.0082(16) C105 0.0198(17) 0.0278(19) 0.0155(16) -0.0029(14) -0.0016(13) 0.0070(15) C106 0.0265(19) 0.029(2) 0.0183(17) -0.0027(15) 0.0030(14) 0.0117(16) C107 0.0261(19) 0.028(2) 0.0171(16) -0.0036(15) -0.0037(14) 0.0128(16) C108 0.0259(19) 0.0223(18) 0.0242(18) 0.0003(15) -0.0026(14) 0.0067(15) C109 0.0196(17) 0.0232(18) 0.0208(17) -0.0021(14) 0.0027(13) 0.0035(14) C110 0.0155(16) 0.0229(18) 0.0178(16) -0.0032(14) -0.0019(13) 0.0034(14) C111 0.0216(17) 0.0192(17) 0.0179(16) 0.0025(13) 0.0020(13) 0.0095(14) C112 0.0202(17) 0.0194(17) 0.0202(16) 0.0018(14) 0.0012(13) 0.0078(14) C113 0.0220(18) 0.0273(19) 0.0234(17) -0.0011(15) 0.0020(14) 0.0094(15) C114 0.0240(19) 0.035(2) 0.0241(18) -0.0041(16) -0.0034(15) 0.0070(17) C115 0.0198(19) 0.035(2) 0.037(2) -0.0075(18) -0.0043(16) 0.0035(17) C116 0.0200(18) 0.031(2) 0.0273(19) -0.0010(16) 0.0032(15) 0.0071(16) C117 0.0223(18) 0.0199(17) 0.0226(17) 0.0004(14) 0.0014(14) 0.0084(15) C118 0.0271(19) 0.0248(19) 0.0216(17) 0.0014(15) 0.0042(14) 0.0089(16) C119 0.0252(18) 0.0216(18) 0.0194(17) -0.0010(14) 0.0028(14) 0.0079(15) C130 0.029(2) 0.027(2) 0.0204(17) 0.0075(15) 0.0043(15) 0.0057(16) C131 0.040(2) 0.031(2) 0.0266(19) 0.0071(16) 0.0011(17) 0.0114(18) C132 0.030(2) 0.026(2) 0.034(2) 0.0065(17) 0.0000(16) -0.0024(17) C133 0.049(3) 0.036(2) 0.024(2) 0.0071(17) 0.0096(18) 0.012(2) C170 0.039(2) 0.025(2) 0.0242(18) -0.0040(16) -0.0016(16) 0.0154(17) C171 0.059(3) 0.048(3) 0.037(2) -0.007(2) -0.011(2) 0.032(2) C172 0.163(6) 0.053(3) 0.049(3) 0.006(3) 0.048(4) 0.061(4) C173 0.063(3) 0.046(3) 0.076(4) -0.034(3) -0.033(3) 0.029(3) O21 0.0234(12) 0.0203(12) 0.0236(12) 0.0028(10) 0.0018(10) 0.0072(10) C211 0.0218(18) 0.0254(19) 0.0230(17) 0.0005(15) -0.0013(14) 0.0085(15) C212 0.038(2) 0.035(2) 0.035(2) 0.0113(18) 0.0068(18) 0.0172(19) C213 0.030(2) 0.031(2) 0.036(2) 0.0047(17) 0.0080(17) 0.0136(17) O31 0.0261(13) 0.0165(12) 0.0240(12) 0.0023(10) 0.0017(10) 0.0047(10) C311 0.0275(19) 0.0208(18) 0.0258(18) 0.0024(15) 0.0019(15) 0.0072(15) C312 0.050(3) 0.031(2) 0.028(2) 0.0084(17) 0.0051(18) 0.0122(19) C313 0.044(2) 0.023(2) 0.029(2) -0.0026(16) 0.0015(17) 0.0037(18) Ti2 0.0177(3) 0.0163(3) 0.0175(3) -0.0007(2) -0.0018(2) 0.0042(2) N41 0.0210(14) 0.0197(15) 0.0149(13) 0.0013(11) 0.0004(11) 0.0070(12) O41 0.0222(12) 0.0176(12) 0.0170(11) 0.0002(9) 0.0001(9) 0.0062(10) C401 0.0147(16) 0.0199(17) 0.0154(15) -0.0014(13) -0.0027(12) 0.0021(13) C402 0.0161(16) 0.0190(17) 0.0202(16) -0.0045(13) -0.0049(13) 0.0083(14) C403 0.0164(16) 0.0176(17) 0.0174(16) -0.0012(13) -0.0017(13) 0.0019(13) C404 0.0156(16) 0.0236(18) 0.0174(16) -0.0002(14) 0.0013(13) 0.0045(14) C405 0.0137(16) 0.0201(17) 0.0185(16) -0.0019(13) -0.0012(12) 0.0026(13) C406 0.0204(17) 0.0236(19) 0.0220(17) -0.0020(14) 0.0005(14) 0.0067(15) C407 0.0190(17) 0.0205(18) 0.0245(17) -0.0064(14) -0.0089(14) 0.0066(14) C408 0.0216(18) 0.0181(17) 0.0258(18) 0.0003(14) -0.0010(14) 0.0025(14) C409 0.0204(17) 0.0209(18) 0.0250(18) 0.0017(14) -0.0006(14) 0.0063(14) C410 0.0168(16) 0.0186(17) 0.0195(16) -0.0014(13) -0.0041(13) 0.0049(14) C411 0.0211(17) 0.0139(16) 0.0192(16) 0.0020(13) 0.0002(13) 0.0066(14) C412 0.0250(18) 0.0175(17) 0.0175(16) 0.0001(13) 0.0019(14) 0.0042(14) C413 0.0274(19) 0.0204(18) 0.0214(17) -0.0001(14) 0.0063(14) 0.0058(15) C414 0.0200(17) 0.0188(17) 0.0220(17) 0.0031(14) 0.0034(13) 0.0035(14) C415 0.0223(18) 0.027(2) 0.0262(18) 0.0020(15) 0.0027(15) 0.0050(16) C416 0.0157(17) 0.029(2) 0.0299(19) 0.0020(16) 0.0022(14) 0.0001(15) C417 0.0188(18) 0.030(2) 0.0250(18) -0.0045(15) -0.0045(14) 0.0062(15) C418 0.0247(18) 0.0272(19) 0.0183(17) -0.0007(14) 0.0012(14) 0.0104(15) C419 0.0169(16) 0.0187(17) 0.0204(16) 0.0014(14) 0.0005(13) 0.0050(14) C430 0.0215(17) 0.0218(18) 0.0198(17) 0.0021(14) 0.0023(13) 0.0057(14) C431 0.0257(19) 0.0233(19) 0.0266(19) 0.0047(15) 0.0036(15) 0.0008(15) C432 0.029(2) 0.026(2) 0.031(2) 0.0067(16) 0.0000(16) 0.0083(16) C433 0.032(2) 0.0242(19) 0.0270(19) 0.0073(15) 0.0083(16) 0.0062(16) C470 0.037(2) 0.0218(19) 0.0274(19) -0.0052(15) -0.0047(16) 0.0144(17) C471 0.045(2) 0.032(2) 0.038(2) 0.0039(18) -0.0006(19) 0.020(2) C472 0.087(4) 0.042(3) 0.033(2) -0.003(2) 0.017(2) 0.038(3) C473 0.052(3) 0.036(2) 0.065(3) -0.026(2) -0.025(2) 0.020(2) N51 0.0206(15) 0.0187(15) 0.0213(14) -0.0015(12) -0.0024(11) 0.0056(12) O51 0.0223(12) 0.0166(12) 0.0181(11) 0.0001(9) -0.0025(9) 0.0053(10) C501 0.0186(17) 0.0180(17) 0.0180(16) 0.0000(13) -0.0017(13) 0.0035(14) C502 0.0215(17) 0.0154(16) 0.0178(16) 0.0003(13) 0.0006(13) 0.0050(14) C503 0.0189(17) 0.0222(18) 0.0179(16) 0.0021(14) -0.0023(13) 0.0061(14) C504 0.0242(18) 0.0209(18) 0.0204(17) -0.0020(14) -0.0060(14) 0.0065(15) C505 0.0212(17) 0.0189(17) 0.0211(17) -0.0006(14) -0.0023(13) 0.0052(14) C506 0.0285(19) 0.0215(18) 0.0221(17) -0.0057(15) -0.0097(15) 0.0066(15) C507 0.030(2) 0.0180(17) 0.0277(19) 0.0009(15) -0.0014(15) 0.0067(15) C508 0.0297(19) 0.0208(18) 0.0255(18) 0.0007(15) -0.0050(15) 0.0118(16) C509 0.0226(18) 0.0213(18) 0.0259(18) -0.0009(15) -0.0069(14) 0.0046(15) C510 0.0212(17) 0.0201(17) 0.0176(16) 0.0011(14) -0.0016(13) 0.0063(14) C511 0.0186(16) 0.0174(16) 0.0197(16) -0.0001(13) -0.0034(13) 0.0076(14) C512 0.0255(18) 0.0234(18) 0.0188(17) -0.0019(14) -0.0046(14) 0.0098(15) C513 0.0255(19) 0.0265(19) 0.0242(18) -0.0056(15) -0.0097(15) 0.0091(16) C514 0.0207(18) 0.0209(18) 0.0297(19) -0.0021(15) -0.0059(14) 0.0104(15) C515 0.0221(19) 0.031(2) 0.034(2) 0.0022(17) -0.0069(16) 0.0050(16) C516 0.0192(19) 0.042(2) 0.038(2) 0.0114(19) 0.0009(16) 0.0064(17) C517 0.0218(19) 0.037(2) 0.034(2) 0.0036(17) -0.0004(16) 0.0090(17) C518 0.0262(19) 0.0261(19) 0.0225(18) 0.0012(15) -0.0034(14) 0.0096(16) C519 0.0211(17) 0.0155(16) 0.0218(17) 0.0012(13) -0.0047(13) 0.0065(14) C530 0.0225(18) 0.0273(19) 0.0193(17) -0.0011(14) -0.0055(14) 0.0113(15) C531 0.033(2) 0.029(2) 0.0289(19) 0.0049(16) -0.0030(16) 0.0163(17) C532 0.0225(19) 0.040(2) 0.0270(19) -0.0004(17) -0.0029(15) 0.0125(17) C533 0.032(2) 0.038(2) 0.0276(19) -0.0028(17) -0.0129(16) 0.0170(18) C570 0.043(2) 0.0220(19) 0.036(2) -0.0057(17) -0.0096(18) 0.0153(18) C571 0.103(4) 0.022(2) 0.071(4) 0.002(2) 0.007(3) 0.012(3) C572 0.074(3) 0.042(3) 0.062(3) -0.033(2) -0.036(3) 0.034(3) C573 0.053(3) 0.043(3) 0.063(3) -0.022(2) -0.008(2) 0.026(2) O22 0.0257(13) 0.0163(12) 0.0258(13) -0.0005(10) -0.0032(10) 0.0014(10) C221 0.088(4) 0.019(2) 0.042(3) 0.0080(19) -0.009(2) -0.003(2) C222 0.185(7) 0.035(3) 0.048(3) 0.001(3) -0.029(4) 0.027(4) C223 0.081(4) 0.024(2) 0.043(3) 0.0009(19) -0.018(2) -0.001(2) O32 0.0211(12) 0.0236(13) 0.0226(12) 0.0007(10) -0.0004(10) 0.0077(10) C321 0.0184(17) 0.0258(19) 0.034(2) -0.0026(16) -0.0018(15) 0.0123(15) C322 0.0235(19) 0.032(2) 0.040(2) 0.0000(18) -0.0008(16) 0.0115(17) C323 0.037(2) 0.041(3) 0.096(4) 0.037(3) 0.017(2) 0.021(2) Ti3 0.0184(3) 0.0160(3) 0.0205(3) -0.0008(2) -0.0016(2) 0.0037(2) N61 0.0188(14) 0.0146(13) 0.0157(13) 0.0015(11) -0.0008(11) 0.0055(11) O61 0.0241(12) 0.0175(12) 0.0180(11) -0.0003(9) -0.0002(9) 0.0051(10) C601 0.0152(16) 0.0189(17) 0.0201(16) -0.0014(14) -0.0019(13) 0.0048(13) C602 0.0189(17) 0.0175(17) 0.0208(16) -0.0009(14) -0.0043(13) 0.0050(14) C603 0.0186(17) 0.0221(18) 0.0201(17) 0.0019(14) -0.0020(13) 0.0046(14) C604 0.0201(17) 0.0255(19) 0.0182(16) 0.0040(14) 0.0021(13) 0.0039(15) C605 0.0151(16) 0.0202(17) 0.0206(17) -0.0003(14) -0.0030(13) 0.0020(14) C606 0.0176(17) 0.0255(18) 0.0195(16) 0.0007(14) 0.0009(13) 0.0076(14) C607 0.0168(16) 0.0252(18) 0.0170(16) -0.0006(14) -0.0005(13) 0.0057(14) C608 0.0200(17) 0.0192(17) 0.0248(18) 0.0017(14) -0.0012(14) 0.0052(14) C609 0.0203(17) 0.0240(18) 0.0184(16) 0.0049(14) 0.0035(13) 0.0062(14) C610 0.0171(16) 0.0188(17) 0.0185(16) -0.0003(13) -0.0028(13) 0.0049(14) C611 0.0216(17) 0.0164(16) 0.0178(16) 0.0016(13) -0.0002(13) 0.0072(14) C612 0.0252(18) 0.0207(17) 0.0164(16) -0.0009(14) 0.0003(13) 0.0089(15) C613 0.0221(18) 0.0211(18) 0.0209(17) 0.0003(14) 0.0041(14) 0.0050(14) C614 0.0195(17) 0.0190(17) 0.0234(17) -0.0003(14) 0.0001(14) 0.0064(14) C615 0.0241(19) 0.028(2) 0.0251(18) 0.0020(15) 0.0045(15) 0.0048(16) C616 0.0194(18) 0.032(2) 0.035(2) -0.0063(17) -0.0035(15) 0.0014(16) C617 0.0200(18) 0.034(2) 0.0233(18) -0.0058(16) -0.0035(14) 0.0060(16) C618 0.0192(17) 0.0242(18) 0.0211(17) -0.0010(14) -0.0002(14) 0.0067(15) C619 0.0185(16) 0.0146(16) 0.0205(16) 0.0014(13) 0.0014(13) 0.0054(13) C630 0.029(2) 0.0233(19) 0.0246(18) 0.0058(15) 0.0059(15) 0.0049(16) C631 0.035(2) 0.028(2) 0.039(2) 0.0056(18) 0.0040(18) -0.0039(17) C632 0.043(2) 0.030(2) 0.034(2) 0.0137(17) 0.0088(18) 0.0125(19) C633 0.039(2) 0.027(2) 0.036(2) 0.0082(17) 0.0097(18) 0.0044(18) C670 0.0229(18) 0.0241(18) 0.0232(17) -0.0039(15) -0.0045(14) 0.0098(15) C671 0.034(2) 0.033(2) 0.031(2) -0.0014(17) -0.0018(16) 0.0173(18) C672 0.034(2) 0.029(2) 0.036(2) -0.0084(17) -0.0079(17) 0.0110(18) C673 0.038(2) 0.037(2) 0.0261(19) -0.0037(17) 0.0039(16) 0.0188(19) N71 0.0236(15) 0.0178(14) 0.0212(14) -0.0008(12) -0.0044(12) 0.0062(12) O71 0.0228(12) 0.0169(12) 0.0222(12) -0.0016(10) -0.0023(10) 0.0065(10) C701 0.0157(16) 0.0188(17) 0.0205(16) 0.0016(14) -0.0025(13) 0.0026(13) C702 0.0217(17) 0.0157(16) 0.0170(16) 0.0012(13) -0.0003(13) 0.0035(14) C703 0.0187(17) 0.0204(17) 0.0200(16) 0.0044(14) -0.0020(13) 0.0052(14) C704 0.0247(18) 0.0243(18) 0.0184(16) -0.0040(14) -0.0068(14) 0.0071(15) C705 0.0202(17) 0.0186(17) 0.0200(16) 0.0015(14) -0.0023(13) 0.0055(14) C706 0.0240(18) 0.0210(18) 0.0191(16) -0.0016(14) -0.0014(14) 0.0054(15) C707 0.0235(18) 0.0211(18) 0.0224(17) 0.0003(14) -0.0017(14) 0.0057(15) C708 0.0224(18) 0.0216(18) 0.0285(18) 0.0017(15) -0.0032(14) 0.0085(15) C709 0.0228(18) 0.0259(19) 0.0219(17) -0.0027(15) -0.0066(14) 0.0097(15) C710 0.0179(16) 0.0173(16) 0.0190(16) -0.0009(13) 0.0003(13) 0.0033(13) C711 0.0193(17) 0.0155(16) 0.0231(17) 0.0022(14) -0.0046(13) 0.0047(14) C712 0.030(2) 0.0230(19) 0.0249(18) -0.0052(15) -0.0116(15) 0.0114(16) C713 0.029(2) 0.026(2) 0.031(2) -0.0038(16) -0.0146(16) 0.0101(16) C714 0.0226(18) 0.0237(19) 0.032(2) 0.0005(16) -0.0068(15) 0.0084(15) C715 0.0220(19) 0.026(2) 0.045(2) 0.0042(17) -0.0088(17) 0.0023(16) C716 0.0220(19) 0.037(2) 0.047(2) 0.0167(19) 0.0040(17) 0.0070(17) C717 0.031(2) 0.038(2) 0.037(2) 0.0102(18) 0.0064(17) 0.0159(18) C718 0.0248(19) 0.0249(19) 0.0284(19) 0.0048(15) -0.0029(15) 0.0096(16) C719 0.0215(18) 0.0199(17) 0.0264(18) 0.0028(14) -0.0028(14) 0.0080(14) C730 0.0215(18) 0.0275(19) 0.0221(17) -0.0018(15) -0.0062(14) 0.0100(15) C731 0.037(2) 0.031(2) 0.0292(19) 0.0086(16) -0.0009(16) 0.0189(18) C732 0.0216(19) 0.035(2) 0.034(2) -0.0029(17) -0.0057(16) 0.0116(17) C733 0.042(2) 0.040(2) 0.028(2) -0.0067(18) -0.0140(17) 0.025(2) C770 0.0291(19) 0.0183(18) 0.0293(19) -0.0029(15) -0.0042(15) 0.0094(15) C771 0.051(3) 0.022(2) 0.084(4) 0.002(2) 0.026(3) 0.005(2) C772 0.089(4) 0.036(3) 0.046(3) -0.019(2) -0.028(3) 0.036(3) C773 0.030(2) 0.023(2) 0.056(3) -0.0008(19) 0.0032(19) 0.0083(17) O23 0.0254(13) 0.0175(12) 0.0288(13) -0.0016(10) -0.0021(10) 0.0011(10) C231 0.050(3) 0.0177(19) 0.043(2) 0.0006(17) 0.015(2) 0.0011(18) C232 0.058(3) 0.043(3) 0.044(3) -0.008(2) 0.007(2) -0.020(2) C233 0.079(4) 0.050(3) 0.105(5) 0.041(3) 0.024(3) 0.033(3) O33 0.0212(12) 0.0223(13) 0.0272(13) -0.0009(10) -0.0006(10) 0.0065(10) C331 0.0224(19) 0.032(2) 0.036(2) -0.0031(17) -0.0019(16) 0.0123(17) C332 0.030(2) 0.041(3) 0.086(4) 0.027(3) 0.001(2) 0.016(2) C333 0.023(2) 0.042(2) 0.043(2) -0.0075(19) -0.0036(17) 0.0129(18) C811 0.051(3) 0.050(3) 0.057(3) 0.012(2) 0.011(2) 0.005(2) C812 0.051(3) 0.065(4) 0.072(4) 0.021(3) 0.007(3) 0.015(3) C813 0.037(2) 0.046(3) 0.075(3) 0.000(2) 0.005(2) 0.002(2) C814 0.041(3) 0.068(4) 0.138(6) 0.040(4) -0.008(3) 0.011(3) O81 0.0321(16) 0.0443(18) 0.063(2) 0.0137(16) 0.0083(14) 0.0041(14) C821 0.042(3) 0.049(3) 0.098(4) 0.028(3) 0.030(3) 0.013(2) C822 0.044(3) 0.100(5) 0.085(4) 0.030(4) -0.009(3) 0.017(3) C823 0.103(4) 0.044(3) 0.044(3) 0.002(2) 0.022(3) -0.007(3) C824 0.105(5) 0.118(6) 0.046(3) 0.021(4) -0.015(3) -0.009(4) O82 0.0490(18) 0.0440(18) 0.0474(18) 0.0048(15) 0.0082(14) 0.0103(15) C831 0.091(4) 0.063(4) 0.060(3) -0.009(3) 0.030(3) 0.003(3) C832 0.088(5) 0.111(6) 0.062(4) 0.018(4) 0.019(3) 0.025(4) C833 0.059(3) 0.042(3) 0.142(6) 0.009(3) 0.046(3) 0.009(3) C834 0.060(4) 0.055(4) 0.186(7) 0.001(5) -0.006(4) 0.020(3) O83 0.059(2) 0.044(2) 0.084(3) 0.0076(19) 0.0307(19) 0.0125(17) C841 0.067(4) 0.062(4) 0.139(6) 0.011(4) -0.003(4) 0.022(3) C842 0.078(4) 0.065(4) 0.123(6) 0.008(4) -0.012(4) 0.015(3) C843 0.068(4) 0.055(4) 0.142(6) -0.009(4) 0.010(4) 0.019(3) C844 0.091(5) 0.085(5) 0.152(7) -0.036(5) -0.039(5) 0.037(4) O84 0.068(2) 0.050(2) 0.105(3) -0.003(2) -0.009(2) 0.0248(19) C851 0.122(19) 0.114(18) 0.124(16) 0.031(14) -0.026(15) 0.028(17) C852 0.12(4) 0.12(4) 0.10(2) -0.02(3) -0.01(2) 0.05(3) C853 0.103(18) 0.098(17) 0.132(18) 0.006(15) -0.025(14) 0.046(16) C854 0.09(3) 0.12(4) 0.13(3) 0.00(2) -0.02(2) 0.06(3) O85 0.087(11) 0.081(11) 0.106(11) 0.001(10) -0.007(10) 0.064(9) C861 0.105(15) 0.120(17) 0.113(15) 0.000(14) 0.002(11) 0.056(15) C862 0.10(3) 0.06(2) 0.124(17) -0.017(19) -0.021(18) 0.03(2) C863 0.133(16) 0.097(15) 0.113(16) -0.020(12) -0.006(13) 0.068(15) C864 0.135(18) 0.14(3) 0.19(4) 0.00(3) -0.07(2) 0.03(2) O86 0.100(11) 0.101(12) 0.108(11) -0.006(10) -0.011(10) 0.034(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O21 1.785(2) . ? Ti1 O31 1.800(2) . ? Ti1 O1 1.958(2) . ? Ti1 O11 1.959(2) . ? Ti1 N1 2.332(3) . ? Ti1 N11 2.345(3) . ? N1 C11 1.345(4) . ? N1 C12 1.383(4) . ? O1 C2 1.338(4) . ? C1 C2 1.402(4) . ? C1 C10 1.435(4) . ? C1 C11 1.490(4) . ? C2 C3 1.453(4) . ? C3 C4 1.375(4) . ? C3 C30 1.550(4) . ? C4 C5 1.429(4) . ? C4 H4 0.9500 . ? C5 C10 1.422(4) . ? C5 C6 1.423(4) . ? C6 C7 1.375(5) . ? C6 H6 0.9500 . ? C7 C8 1.430(4) . ? C7 C70 1.544(4) . ? C8 C9 1.375(4) . ? C8 H8 0.9500 . ? C9 C10 1.428(4) . ? C9 H9 0.9500 . ? C11 C19 1.446(5) . ? C12 C13 1.363(5) . ? C12 H12 0.9500 . ? C13 C14 1.408(5) . ? C13 H13 0.9500 . ? C14 C19 1.426(4) . ? C14 C15 1.427(5) . ? C15 C16 1.361(5) . ? C15 H15 0.9500 . ? C16 C17 1.413(5) . ? C16 H16 0.9500 . ? C17 C18 1.374(5) . ? C17 H17 0.9500 . ? C18 C19 1.425(5) . ? C18 H18 0.9500 . ? C30 C33 1.536(4) . ? C30 C32 1.539(5) . ? C30 C31 1.541(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C70 C71 1.520(5) . ? C70 C72 1.522(7) . ? C70 C73 1.537(6) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? N11 C111 1.340(4) . ? N11 C119 1.380(4) . ? O11 C102 1.345(4) . ? C101 C102 1.387(5) . ? C101 C110 1.441(4) . ? C101 C111 1.478(4) . ? C102 C103 1.452(5) . ? C103 C104 1.382(4) . ? C103 C130 1.533(5) . ? C104 C105 1.412(5) . ? C104 H104 0.9500 . ? C105 C110 1.418(5) . ? C105 C106 1.435(4) . ? C106 C107 1.371(5) . ? C106 H106 0.9500 . ? C107 C108 1.411(5) . ? C107 C170 1.547(4) . ? C108 C109 1.376(4) . ? C108 H108 0.9500 . ? C109 C110 1.421(5) . ? C109 H109 0.9500 . ? C111 C112 1.442(5) . ? C112 C117 1.417(5) . ? C112 C113 1.431(4) . ? C113 C114 1.364(5) . ? C113 H113 0.9500 . ? C114 C115 1.407(5) . ? C114 H114 0.9500 . ? C115 C116 1.370(5) . ? C115 H115 0.9500 . ? C116 C117 1.420(5) . ? C116 H116 0.9500 . ? C117 C118 1.418(4) . ? C118 C119 1.354(5) . ? C118 H118 0.9500 . ? C119 H119 0.9500 . ? C130 C132 1.536(5) . ? C130 C133 1.545(5) . ? C130 C131 1.547(5) . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C132 H13D 0.9800 . ? C132 H13E 0.9800 . ? C132 H13F 0.9800 . ? C133 H13G 0.9800 . ? C133 H13H 0.9800 . ? C133 H13I 0.9800 . ? C170 C171 1.512(5) . ? C170 C172 1.528(6) . ? C170 C173 1.533(6) . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C173 H17G 0.9800 . ? C173 H17H 0.9800 . ? C173 H17I 0.9800 . ? O21 C211 1.419(4) . ? C211 C212 1.519(5) . ? C211 C213 1.524(5) . ? C211 H211 1.0000 . ? C212 H21A 0.9800 . ? C212 H21B 0.9800 . ? C212 H21C 0.9800 . ? C213 H21D 0.9800 . ? C213 H21E 0.9800 . ? C213 H21F 0.9800 . ? O31 C311 1.427(4) . ? C311 C312 1.505(5) . ? C311 C313 1.523(5) . ? C311 H311 1.0000 . ? C312 H31D 0.9800 . ? C312 H31E 0.9800 . ? C312 H31F 0.9800 . ? C313 H31G 0.9800 . ? C313 H31H 0.9800 . ? C313 H31I 0.9800 . ? Ti2 O22 1.788(2) . ? Ti2 O32 1.788(2) . ? Ti2 O51 1.957(2) . ? Ti2 O41 1.966(2) . ? Ti2 N51 2.331(3) . ? Ti2 N41 2.342(3) . ? N41 C411 1.342(4) . ? N41 C412 1.376(4) . ? O41 C402 1.345(3) . ? C401 C402 1.394(5) . ? C401 C410 1.436(4) . ? C401 C411 1.485(4) . ? C402 C403 1.448(4) . ? C403 C404 1.379(4) . ? C403 C430 1.538(5) . ? C404 C405 1.410(5) . ? C404 H404 0.9500 . ? C405 C410 1.425(4) . ? C405 C406 1.429(4) . ? C406 C407 1.374(5) . ? C406 H406 0.9500 . ? C407 C408 1.418(5) . ? C407 C470 1.540(4) . ? C408 C409 1.377(4) . ? C408 H408 0.9500 . ? C409 C410 1.417(5) . ? C409 H409 0.9500 . ? C411 C419 1.443(5) . ? C412 C413 1.359(5) . ? C412 H412 0.9500 . ? C413 C414 1.412(4) . ? C413 H413 0.9500 . ? C414 C419 1.416(5) . ? C414 C415 1.422(5) . ? C415 C416 1.366(5) . ? C415 H415 0.9500 . ? C416 C417 1.414(5) . ? C416 H416 0.9500 . ? C417 C418 1.370(5) . ? C417 H417 0.9500 . ? C418 C419 1.425(4) . ? C418 H418 0.9500 . ? C430 C431 1.538(5) . ? C430 C433 1.541(5) . ? C430 C432 1.542(5) . ? C431 H43A 0.9800 . ? C431 H43B 0.9800 . ? C431 H43C 0.9800 . ? C432 H43D 0.9800 . ? C432 H43E 0.9800 . ? C432 H43F 0.9800 . ? C433 H43G 0.9800 . ? C433 H43H 0.9800 . ? C433 H43I 0.9800 . ? C470 C472 1.533(6) . ? C470 C471 1.540(5) . ? C470 C473 1.545(5) . ? C471 H47A 0.9800 . ? C471 H47B 0.9800 . ? C471 H47C 0.9800 . ? C472 H47D 0.9800 . ? C472 H47E 0.9800 . ? C472 H47F 0.9800 . ? C473 H47G 0.9800 . ? C473 H47H 0.9800 . ? C473 H47I 0.9800 . ? N51 C511 1.347(4) . ? N51 C512 1.382(4) . ? O51 C502 1.342(3) . ? C501 C502 1.397(4) . ? C501 C510 1.446(4) . ? C501 C511 1.487(4) . ? C502 C503 1.442(4) . ? C503 C504 1.377(4) . ? C503 C530 1.548(4) . ? C504 C505 1.429(4) . ? C504 H504 0.9500 . ? C505 C510 1.411(4) . ? C505 C506 1.426(4) . ? C506 C507 1.383(5) . ? C506 H506 0.9500 . ? C507 C508 1.419(5) . ? C507 C570 1.539(5) . ? C508 C509 1.373(4) . ? C508 H508 0.9500 . ? C509 C510 1.424(4) . ? C509 H509 0.9500 . ? C511 C519 1.442(5) . ? C512 C513 1.352(5) . ? C512 H512 0.9500 . ? C513 C514 1.416(5) . ? C513 H513 0.9500 . ? C514 C515 1.419(5) . ? C514 C519 1.429(4) . ? C515 C516 1.361(5) . ? C515 H515 0.9500 . ? C516 C517 1.410(5) . ? C516 H516 0.9500 . ? C517 C518 1.369(5) . ? C517 H517 0.9500 . ? C518 C519 1.427(5) . ? C518 H518 0.9500 . ? C530 C532 1.540(5) . ? C530 C531 1.545(5) . ? C530 C533 1.546(4) . ? C531 H53A 0.9800 . ? C531 H53B 0.9800 . ? C531 H53C 0.9800 . ? C532 H53D 0.9800 . ? C532 H53E 0.9800 . ? C532 H53F 0.9800 . ? C533 H53G 0.9800 . ? C533 H53H 0.9800 . ? C533 H53I 0.9800 . ? C570 C572 1.528(5) . ? C570 C571 1.532(7) . ? C570 C573 1.538(6) . ? C571 H57A 0.9800 . ? C571 H57B 0.9800 . ? C571 H57C 0.9800 . ? C572 H57D 0.9800 . ? C572 H57E 0.9800 . ? C572 H57F 0.9800 . ? C573 H57G 0.9800 . ? C573 H57H 0.9800 . ? C573 H57I 0.9800 . ? O22 C221 1.431(5) . ? C221 C222 1.421(7) . ? C221 C223 1.513(6) . ? C221 H221 1.0000 . ? C222 H22A 0.9800 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C223 H22D 0.9800 . ? C223 H22E 0.9800 . ? C223 H22F 0.9800 . ? O32 C321 1.424(4) . ? C321 C323 1.512(6) . ? C321 C322 1.524(5) . ? C321 H321 1.0000 . ? C322 H32D 0.9800 . ? C322 H32E 0.9800 . ? C322 H32F 0.9800 . ? C323 H32G 0.9800 . ? C323 H32H 0.9800 . ? C323 H32I 0.9800 . ? Ti3 O23 1.779(2) . ? Ti3 O33 1.796(2) . ? Ti3 O61 1.951(2) . ? Ti3 O71 1.972(2) . ? Ti3 N61 2.329(3) . ? Ti3 N71 2.329(3) . ? N61 C611 1.342(4) . ? N61 C612 1.381(4) . ? O61 C602 1.345(4) . ? C601 C602 1.398(5) . ? C601 C610 1.443(4) . ? C601 C611 1.477(5) . ? C602 C603 1.442(5) . ? C603 C604 1.379(4) . ? C603 C630 1.538(5) . ? C604 C605 1.415(5) . ? C604 H604 0.9500 . ? C605 C610 1.417(5) . ? C605 C606 1.425(4) . ? C606 C607 1.375(5) . ? C606 H606 0.9500 . ? C607 C608 1.417(5) . ? C607 C670 1.541(4) . ? C608 C609 1.378(4) . ? C608 H608 0.9500 . ? C609 C610 1.422(5) . ? C609 H609 0.9500 . ? C611 C619 1.442(5) . ? C612 C613 1.359(5) . ? C612 H612 0.9500 . ? C613 C614 1.414(4) . ? C613 H613 0.9500 . ? C614 C619 1.414(5) . ? C614 C615 1.432(5) . ? C615 C616 1.376(5) . ? C615 H615 0.9500 . ? C616 C617 1.415(5) . ? C616 H616 0.9500 . ? C617 C618 1.363(5) . ? C617 H617 0.9500 . ? C618 C619 1.424(4) . ? C618 H618 0.9500 . ? C630 C633 1.532(5) . ? C630 C631 1.539(5) . ? C630 C632 1.543(5) . ? C631 H63A 0.9800 . ? C631 H63B 0.9800 . ? C631 H63C 0.9800 . ? C632 H63D 0.9800 . ? C632 H63E 0.9800 . ? C632 H63F 0.9800 . ? C633 H63G 0.9800 . ? C633 H63H 0.9800 . ? C633 H63I 0.9800 . ? C670 C673 1.526(5) . ? C670 C671 1.539(5) . ? C670 C672 1.540(5) . ? C671 H67A 0.9800 . ? C671 H67B 0.9800 . ? C671 H67C 0.9800 . ? C672 H67D 0.9800 . ? C672 H67E 0.9800 . ? C672 H67F 0.9800 . ? C673 H67G 0.9800 . ? C673 H67H 0.9800 . ? C673 H67I 0.9800 . ? N71 C711 1.338(4) . ? N71 C712 1.378(4) . ? O71 C702 1.349(4) . ? C701 C702 1.395(4) . ? C701 C710 1.430(4) . ? C701 C711 1.490(4) . ? C702 C703 1.446(4) . ? C703 C704 1.377(4) . ? C703 C730 1.549(4) . ? C704 C705 1.418(4) . ? C704 H704 0.9500 . ? C705 C706 1.424(4) . ? C705 C710 1.426(4) . ? C706 C707 1.373(5) . ? C706 H706 0.9500 . ? C707 C708 1.418(5) . ? C707 C770 1.544(4) . ? C708 C709 1.376(4) . ? C708 H708 0.9500 . ? C709 C710 1.425(4) . ? C709 H709 0.9500 . ? C711 C719 1.445(5) . ? C712 C713 1.360(5) . ? C712 H712 0.9500 . ? C713 C714 1.414(5) . ? C713 H713 0.9500 . ? C714 C715 1.417(5) . ? C714 C719 1.427(5) . ? C715 C716 1.362(5) . ? C715 H715 0.9500 . ? C716 C717 1.412(5) . ? C716 H716 0.9500 . ? C717 C718 1.371(5) . ? C717 H717 0.9500 . ? C718 C719 1.424(5) . ? C718 H718 0.9500 . ? C730 C732 1.535(5) . ? C730 C733 1.539(4) . ? C730 C731 1.551(5) . ? C731 H73D 0.9800 . ? C731 H73E 0.9800 . ? C731 H73F 0.9800 . ? C732 H73G 0.9800 . ? C732 H73H 0.9800 . ? C732 H73I 0.9800 . ? C733 H73J 0.9800 . ? C733 H73K 0.9800 . ? C733 H73L 0.9800 . ? C770 C771 1.526(6) . ? C770 C772 1.529(5) . ? C770 C773 1.533(5) . ? C771 H77A 0.9800 . ? C771 H77B 0.9800 . ? C771 H77C 0.9800 . ? C772 H77D 0.9800 . ? C772 H77E 0.9800 . ? C772 H77F 0.9800 . ? C773 H77G 0.9800 . ? C773 H77H 0.9800 . ? C773 H77I 0.9800 . ? O23 C231 1.422(4) . ? C231 C232 1.508(6) . ? C231 C233 1.531(7) . ? C231 H231 1.0000 . ? C232 H23A 0.9800 . ? C232 H23B 0.9800 . ? C232 H23C 0.9800 . ? C233 H23D 0.9800 . ? C233 H23E 0.9800 . ? C233 H23F 0.9800 . ? O33 C331 1.419(4) . ? C331 C333 1.517(5) . ? C331 C332 1.521(6) . ? C331 H331 1.0000 . ? C332 H33D 0.9800 . ? C332 H33E 0.9800 . ? C332 H33F 0.9800 . ? C333 H33G 0.9800 . ? C333 H33H 0.9800 . ? C333 H33I 0.9800 . ? C811 O81 1.419(6) . ? C811 C812 1.505(6) . ? C811 H81A 0.9900 . ? C811 H81B 0.9900 . ? C812 H81C 0.9800 . ? C812 H81D 0.9800 . ? C812 H81E 0.9800 . ? C813 O81 1.424(5) . ? C813 C814 1.485(7) . ? C813 H81F 0.9900 . ? C813 H81G 0.9900 . ? C814 H81H 0.9800 . ? C814 H81I 0.9800 . ? C814 H81J 0.9800 . ? C821 O82 1.443(5) . ? C821 C822 1.500(7) . ? C821 H82A 0.9900 . ? C821 H82B 0.9900 . ? C822 H82C 0.9800 . ? C822 H82D 0.9800 . ? C822 H82E 0.9800 . ? C823 O82 1.406(5) . ? C823 C824 1.502(8) . ? C823 H82F 0.9900 . ? C823 H82G 0.9900 . ? C824 H82H 0.9800 . ? C824 H82I 0.9800 . ? C824 H82J 0.9800 . ? C831 O83 1.424(7) . ? C831 C832 1.483(8) . ? C831 H83A 0.9900 . ? C831 H83B 0.9900 . ? C832 H83C 0.9800 . ? C832 H83D 0.9800 . ? C832 H83E 0.9800 . ? C833 O83 1.419(6) . ? C833 C834 1.485(9) . ? C833 H83F 0.9900 . ? C833 H83G 0.9900 . ? C834 H83H 0.9800 . ? C834 H83I 0.9800 . ? C834 H83J 0.9800 . ? C841 O84 1.396(6) . ? C841 C842 1.470(8) . ? C841 H84A 0.9900 . ? C841 H84B 0.9900 . ? C842 H84C 0.9800 . ? C842 H84D 0.9800 . ? C842 H84E 0.9800 . ? C843 O84 1.383(7) . ? C843 C844 1.446(8) . ? C843 H84F 0.9900 . ? C843 H84G 0.9900 . ? C844 H84H 0.9800 . ? C844 H84I 0.9800 . ? C844 H84J 0.9800 . ? C851 O85 1.385(17) . ? C851 C852 1.51(2) . ? C851 H85A 0.9900 . ? C851 H85B 0.9900 . ? C852 H85C 0.9800 . ? C852 H85D 0.9800 . ? C852 H85E 0.9800 . ? C853 O85 1.424(17) . ? C853 C854 1.49(2) . ? C853 H85F 0.9900 . ? C853 H85G 0.9900 . ? C854 H85H 0.9800 . ? C854 H85I 0.9800 . ? C854 H85J 0.9800 . ? C861 O86 1.383(16) . ? C861 C862 1.51(2) . ? C861 H86A 0.9900 . ? C861 H86B 0.9900 . ? C862 H86C 0.9800 . ? C862 H86D 0.9800 . ? C862 H86E 0.9800 . ? C863 O86 1.412(15) . ? C863 C864 1.49(2) . ? C863 H86F 0.9900 . ? C863 H86G 0.9900 . ? C864 H86H 0.9800 . ? C864 H86I 0.9800 . ? C864 H86J 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 O21 Ti1 O31 103.77(11) . . ? O21 Ti1 O1 95.40(10) . . ? O31 Ti1 O1 97.03(10) . . ? O21 Ti1 O11 96.47(10) . . ? O31 Ti1 O11 97.31(10) . . ? O1 Ti1 O11 158.64(10) . . ? O21 Ti1 N1 167.12(11) . . ? O31 Ti1 N1 88.67(10) . . ? O1 Ti1 N1 79.52(9) . . ? O11 Ti1 N1 85.07(9) . . ? O21 Ti1 N11 91.88(10) . . ? O31 Ti1 N11 164.34(10) . . ? O1 Ti1 N11 81.20(9) . . ? O11 Ti1 N11 80.71(10) . . ? N1 Ti1 N11 75.70(10) . . ? C11 N1 C12 118.6(3) . . ? C11 N1 Ti1 121.3(2) . . ? C12 N1 Ti1 115.5(2) . . ? C2 O1 Ti1 123.6(2) . . ? C2 C1 C10 120.0(3) . . ? C2 C1 C11 119.2(3) . . ? C10 C1 C11 120.7(3) . . ? O1 C2 C1 120.0(3) . . ? O1 C2 C3 119.2(3) . . ? C1 C2 C3 120.7(3) . . ? C4 C3 C2 117.2(3) . . ? C4 C3 C30 121.9(3) . . ? C2 C3 C30 120.9(3) . . ? C3 C4 C5 123.4(3) . . ? C3 C4 H4 118.3 . . ? C5 C4 H4 118.3 . . ? C10 C5 C6 120.2(3) . . ? C10 C5 C4 118.8(3) . . ? C6 C5 C4 121.0(3) . . ? C7 C6 C5 122.5(3) . . ? C7 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C6 C7 C8 117.1(3) . . ? C6 C7 C70 123.5(3) . . ? C8 C7 C70 119.4(3) . . ? C9 C8 C7 121.8(3) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C10 121.6(3) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C5 C10 C9 116.7(3) . . ? C5 C10 C1 118.7(3) . . ? C9 C10 C1 124.5(3) . . ? N1 C11 C19 121.2(3) . . ? N1 C11 C1 117.9(3) . . ? C19 C11 C1 120.7(3) . . ? C13 C12 N1 123.3(3) . . ? C13 C12 H12 118.4 . . ? N1 C12 H12 118.4 . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C19 118.1(3) . . ? C13 C14 C15 122.2(3) . . ? C19 C14 C15 119.7(3) . . ? C16 C15 C14 120.8(3) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 119.8(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 121.2(3) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 120.6(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C14 C19 C18 118.0(3) . . ? C14 C19 C11 118.4(3) . . ? C18 C19 C11 123.5(3) . . ? C33 C30 C32 106.9(3) . . ? C33 C30 C31 107.7(3) . . ? C32 C30 C31 110.3(3) . . ? C33 C30 C3 111.8(3) . . ? C32 C30 C3 110.7(3) . . ? C31 C30 C3 109.5(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C71 C70 C72 108.8(4) . . ? C71 C70 C73 108.4(4) . . ? C72 C70 C73 109.8(4) . . ? C71 C70 C7 111.9(3) . . ? C72 C70 C7 107.6(3) . . ? C73 C70 C7 110.3(3) . . ? 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 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C111 N11 C119 117.6(3) . . ? C111 N11 Ti1 118.7(2) . . ? C119 N11 Ti1 119.8(2) . . ? C102 O11 Ti1 124.4(2) . . ? C102 C101 C110 121.0(3) . . ? C102 C101 C111 119.6(3) . . ? C110 C101 C111 119.4(3) . . ? O11 C102 C101 119.6(3) . . ? O11 C102 C103 120.0(3) . . ? C101 C102 C103 120.4(3) . . ? C104 C103 C102 116.7(3) . . ? C104 C103 C130 122.2(3) . . ? C102 C103 C130 121.1(3) . . ? C103 C104 C105 123.9(3) . . ? C103 C104 H104 118.0 . . ? C105 C104 H104 118.0 . . ? C104 C105 C110 119.0(3) . . ? C104 C105 C106 121.9(3) . . ? C110 C105 C106 119.0(3) . . ? C107 C106 C105 122.3(3) . . ? C107 C106 H106 118.8 . . ? C105 C106 H106 118.8 . . ? C106 C107 C108 117.7(3) . . ? C106 C107 C170 123.4(3) . . ? C108 C107 C170 118.9(3) . . ? C109 C108 C107 121.8(4) . . ? C109 C108 H108 119.1 . . ? C107 C108 H108 119.1 . . ? C108 C109 C110 121.2(3) . . ? C108 C109 H109 119.4 . . ? C110 C109 H109 119.4 . . ? C105 C110 C109 117.7(3) . . ? C105 C110 C101 118.0(3) . . ? C109 C110 C101 124.2(3) . . ? N11 C111 C112 121.4(3) . . ? N11 C111 C101 119.2(3) . . ? C112 C111 C101 119.4(3) . . ? C117 C112 C113 118.1(3) . . ? C117 C112 C111 118.8(3) . . ? C113 C112 C111 123.0(3) . . ? C114 C113 C112 120.8(3) . . ? C114 C113 H113 119.6 . . ? C112 C113 H113 119.6 . . ? C113 C114 C115 120.4(3) . . ? C113 C114 H114 119.8 . . ? C115 C114 H114 119.8 . . ? C116 C115 C114 120.7(3) . . ? C116 C115 H115 119.6 . . ? C114 C115 H115 119.6 . . ? C115 C116 C117 120.1(3) . . ? C115 C116 H116 120.0 . . ? C117 C116 H116 120.0 . . ? C118 C117 C112 117.1(3) . . ? C118 C117 C116 123.2(3) . . ? C112 C117 C116 119.7(3) . . ? C119 C118 C117 119.9(3) . . ? C119 C118 H118 120.1 . . ? C117 C118 H118 120.1 . . ? C118 C119 N11 123.9(3) . . ? C118 C119 H119 118.0 . . ? N11 C119 H119 118.0 . . ? C103 C130 C132 109.1(3) . . ? C103 C130 C133 111.5(3) . . ? C132 C130 C133 107.7(3) . . ? C103 C130 C131 110.8(3) . . ? C132 C130 C131 110.5(3) . . ? C133 C130 C131 107.2(3) . . ? C130 C131 H13A 109.5 . . ? C130 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C130 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C130 C132 H13D 109.5 . . ? C130 C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? C130 C132 H13F 109.5 . . ? H13D C132 H13F 109.5 . . ? H13E C132 H13F 109.5 . . ? C130 C133 H13G 109.5 . . ? C130 C133 H13H 109.5 . . ? H13G C133 H13H 109.5 . . ? C130 C133 H13I 109.5 . . ? H13G C133 H13I 109.5 . . ? H13H C133 H13I 109.5 . . ? C171 C170 C172 109.0(4) . . ? C171 C170 C173 108.7(4) . . ? C172 C170 C173 108.7(4) . . ? C171 C170 C107 110.6(3) . . ? C172 C170 C107 111.6(3) . . ? C173 C170 C107 108.2(3) . . ? C170 C171 H17A 109.5 . . ? C170 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C170 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C170 C172 H17D 109.5 . . ? C170 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C170 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C170 C173 H17G 109.5 . . ? C170 C173 H17H 109.5 . . ? H17G C173 H17H 109.5 . . ? C170 C173 H17I 109.5 . . ? H17G C173 H17I 109.5 . . ? H17H C173 H17I 109.5 . . ? C211 O21 Ti1 160.9(2) . . ? O21 C211 C212 110.4(3) . . ? O21 C211 C213 108.9(3) . . ? C212 C211 C213 112.2(3) . . ? O21 C211 H211 108.4 . . ? C212 C211 H211 108.4 . . ? C213 C211 H211 108.4 . . ? C211 C212 H21A 109.5 . . ? C211 C212 H21B 109.5 . . ? H21A C212 H21B 109.5 . . ? C211 C212 H21C 109.5 . . ? H21A C212 H21C 109.5 . . ? H21B C212 H21C 109.5 . . ? C211 C213 H21D 109.5 . . ? C211 C213 H21E 109.5 . . ? H21D C213 H21E 109.5 . . ? C211 C213 H21F 109.5 . . ? H21D C213 H21F 109.5 . . ? H21E C213 H21F 109.5 . . ? C311 O31 Ti1 148.8(2) . . ? O31 C311 C312 109.3(3) . . ? O31 C311 C313 108.7(3) . . ? C312 C311 C313 112.6(3) . . ? O31 C311 H311 108.7 . . ? C312 C311 H311 108.7 . . ? C313 C311 H311 108.7 . . ? C311 C312 H31D 109.5 . . ? C311 C312 H31E 109.5 . . ? H31D C312 H31E 109.5 . . ? C311 C312 H31F 109.5 . . ? H31D C312 H31F 109.5 . . ? H31E C312 H31F 109.5 . . ? C311 C313 H31G 109.5 . . ? C311 C313 H31H 109.5 . . ? H31G C313 H31H 109.5 . . ? C311 C313 H31I 109.5 . . ? H31G C313 H31I 109.5 . . ? H31H C313 H31I 109.5 . . ? O22 Ti2 O32 104.19(11) . . ? O22 Ti2 O51 96.82(10) . . ? O32 Ti2 O51 96.32(10) . . ? O22 Ti2 O41 97.56(10) . . ? O32 Ti2 O41 94.98(9) . . ? O51 Ti2 O41 158.94(10) . . ? O22 Ti2 N51 89.55(10) . . ? O32 Ti2 N51 166.21(11) . . ? O51 Ti2 N51 80.74(9) . . ? O41 Ti2 N51 84.06(9) . . ? O22 Ti2 N41 164.88(10) . . ? O32 Ti2 N41 90.89(10) . . ? O51 Ti2 N41 82.27(9) . . ? O41 Ti2 N41 79.84(10) . . ? N51 Ti2 N41 75.39(10) . . ? C411 N41 C412 118.4(3) . . ? C411 N41 Ti2 120.0(2) . . ? C412 N41 Ti2 119.0(2) . . ? C402 O41 Ti2 121.8(2) . . ? C402 C401 C410 120.8(3) . . ? C402 C401 C411 119.5(3) . . ? C410 C401 C411 119.7(3) . . ? O41 C402 C401 119.9(3) . . ? O41 C402 C403 119.6(3) . . ? C401 C402 C403 120.5(3) . . ? C404 C403 C402 116.9(3) . . ? C404 C403 C430 121.9(3) . . ? C402 C403 C430 121.2(3) . . ? C403 C404 C405 124.1(3) . . ? C403 C404 H404 118.0 . . ? C405 C404 H404 118.0 . . ? C404 C405 C410 118.9(3) . . ? C404 C405 C406 121.5(3) . . ? C410 C405 C406 119.6(3) . . ? C407 C406 C405 122.4(3) . . ? C407 C406 H406 118.8 . . ? C405 C406 H406 118.8 . . ? C406 C407 C408 117.3(3) . . ? C406 C407 C470 123.4(3) . . ? C408 C407 C470 119.3(3) . . ? C409 C408 C407 121.7(3) . . ? C409 C408 H408 119.1 . . ? C407 C408 H408 119.1 . . ? C408 C409 C410 121.9(3) . . ? C408 C409 H409 119.1 . . ? C410 C409 H409 119.1 . . ? C409 C410 C405 116.9(3) . . ? C409 C410 C401 124.9(3) . . ? C405 C410 C401 118.1(3) . . ? N41 C411 C419 121.0(3) . . ? N41 C411 C401 118.7(3) . . ? C419 C411 C401 120.4(3) . . ? C413 C412 N41 123.4(3) . . ? C413 C412 H412 118.3 . . ? N41 C412 H412 118.3 . . ? C412 C413 C414 119.9(3) . . ? C412 C413 H413 120.1 . . ? C414 C413 H413 120.1 . . ? C413 C414 C419 117.6(3) . . ? C413 C414 C415 122.8(3) . . ? C419 C414 C415 119.5(3) . . ? C416 C415 C414 120.5(3) . . ? C416 C415 H415 119.7 . . ? C414 C415 H415 119.7 . . ? C415 C416 C417 119.9(3) . . ? C415 C416 H416 120.0 . . ? C417 C416 H416 120.0 . . ? C418 C417 C416 120.9(3) . . ? C418 C417 H417 119.6 . . ? C416 C417 H417 119.6 . . ? C417 C418 C419 120.4(3) . . ? C417 C418 H418 119.8 . . ? C419 C418 H418 119.8 . . ? C414 C419 C418 118.5(3) . . ? C414 C419 C411 118.5(3) . . ? C418 C419 C411 123.0(3) . . ? C403 C430 C431 108.5(3) . . ? C403 C430 C433 111.6(3) . . ? C431 C430 C433 107.8(3) . . ? C403 C430 C432 110.7(3) . . ? C431 C430 C432 111.2(3) . . ? C433 C430 C432 106.9(3) . . ? C430 C431 H43A 109.5 . . ? C430 C431 H43B 109.5 . . ? H43A C431 H43B 109.5 . . ? C430 C431 H43C 109.5 . . ? H43A C431 H43C 109.5 . . ? H43B C431 H43C 109.5 . . ? C430 C432 H43D 109.5 . . ? C430 C432 H43E 109.5 . . ? H43D C432 H43E 109.5 . . ? C430 C432 H43F 109.5 . . ? H43D C432 H43F 109.5 . . ? H43E C432 H43F 109.5 . . ? C430 C433 H43G 109.5 . . ? C430 C433 H43H 109.5 . . ? H43G C433 H43H 109.5 . . ? C430 C433 H43I 109.5 . . ? H43G C433 H43I 109.5 . . ? H43H C433 H43I 109.5 . . ? C472 C470 C407 112.4(3) . . ? C472 C470 C471 107.8(3) . . ? C407 C470 C471 110.1(3) . . ? C472 C470 C473 109.6(3) . . ? C407 C470 C473 108.0(3) . . ? C471 C470 C473 108.8(3) . . ? C470 C471 H47A 109.5 . . ? C470 C471 H47B 109.5 . . ? H47A C471 H47B 109.5 . . ? C470 C471 H47C 109.5 . . ? H47A C471 H47C 109.5 . . ? H47B C471 H47C 109.5 . . ? C470 C472 H47D 109.5 . . ? C470 C472 H47E 109.5 . . ? H47D C472 H47E 109.5 . . ? C470 C472 H47F 109.5 . . ? H47D C472 H47F 109.5 . . ? H47E C472 H47F 109.5 . . ? C470 C473 H47G 109.5 . . ? C470 C473 H47H 109.5 . . ? H47G C473 H47H 109.5 . . ? C470 C473 H47I 109.5 . . ? H47G C473 H47I 109.5 . . ? H47H C473 H47I 109.5 . . ? C511 N51 C512 118.9(3) . . ? C511 N51 Ti2 119.0(2) . . ? C512 N51 Ti2 116.87(19) . . ? C502 O51 Ti2 123.0(2) . . ? C502 C501 C510 120.3(3) . . ? C502 C501 C511 119.4(3) . . ? C510 C501 C511 120.3(3) . . ? O51 C502 C501 119.4(3) . . ? O51 C502 C503 119.7(3) . . ? C501 C502 C503 120.9(3) . . ? C504 C503 C502 117.3(3) . . ? C504 C503 C530 121.6(3) . . ? C502 C503 C530 121.0(3) . . ? C503 C504 C505 123.1(3) . . ? C503 C504 H504 118.5 . . ? C505 C504 H504 118.5 . . ? C510 C505 C506 119.6(3) . . ? C510 C505 C504 119.5(3) . . ? C506 C505 C504 120.8(3) . . ? C507 C506 C505 122.2(3) . . ? C507 C506 H506 118.9 . . ? C505 C506 H506 118.9 . . ? C506 C507 C508 117.0(3) . . ? C506 C507 C570 123.2(3) . . ? C508 C507 C570 119.8(3) . . ? C509 C508 C507 122.5(3) . . ? C509 C508 H508 118.8 . . ? C507 C508 H508 118.8 . . ? C508 C509 C510 120.7(3) . . ? C508 C509 H509 119.6 . . ? C510 C509 H509 119.6 . . ? C505 C510 C509 118.0(3) . . ? C505 C510 C501 118.0(3) . . ? C509 C510 C501 124.0(3) . . ? N51 C511 C519 120.7(3) . . ? N51 C511 C501 118.8(3) . . ? C519 C511 C501 120.4(3) . . ? C513 C512 N51 123.4(3) . . ? C513 C512 H512 118.3 . . ? N51 C512 H512 118.3 . . ? C512 C513 C514 119.6(3) . . ? C512 C513 H513 120.2 . . ? C514 C513 H513 120.2 . . ? C513 C514 C515 122.6(3) . . ? C513 C514 C519 117.8(3) . . ? C515 C514 C519 119.6(3) . . ? C516 C515 C514 120.8(3) . . ? C516 C515 H515 119.6 . . ? C514 C515 H515 119.6 . . ? C515 C516 C517 119.9(4) . . ? C515 C516 H516 120.0 . . ? C517 C516 H516 120.0 . . ? C518 C517 C516 121.2(4) . . ? C518 C517 H517 119.4 . . ? C516 C517 H517 119.4 . . ? C517 C518 C519 120.4(3) . . ? C517 C518 H518 119.8 . . ? C519 C518 H518 119.8 . . ? C518 C519 C514 118.0(3) . . ? C518 C519 C511 123.1(3) . . ? C514 C519 C511 118.6(3) . . ? C532 C530 C531 110.6(3) . . ? C532 C530 C533 107.8(3) . . ? C531 C530 C533 106.8(3) . . ? C532 C530 C503 109.6(3) . . ? C531 C530 C503 110.3(3) . . ? C533 C530 C503 111.6(3) . . ? C530 C531 H53A 109.5 . . ? C530 C531 H53B 109.5 . . ? H53A C531 H53B 109.5 . . ? C530 C531 H53C 109.5 . . ? H53A C531 H53C 109.5 . . ? H53B C531 H53C 109.5 . . ? C530 C532 H53D 109.5 . . ? C530 C532 H53E 109.5 . . ? H53D C532 H53E 109.5 . . ? C530 C532 H53F 109.5 . . ? H53D C532 H53F 109.5 . . ? H53E C532 H53F 109.5 . . ? C530 C533 H53G 109.5 . . ? C530 C533 H53H 109.5 . . ? H53G C533 H53H 109.5 . . ? C530 C533 H53I 109.5 . . ? H53G C533 H53I 109.5 . . ? H53H C533 H53I 109.5 . . ? C572 C570 C571 109.4(4) . . ? C572 C570 C507 112.1(3) . . ? C571 C570 C507 107.9(3) . . ? C572 C570 C573 108.5(4) . . ? C571 C570 C573 109.1(4) . . ? C507 C570 C573 109.8(3) . . ? C570 C571 H57A 109.5 . . ? C570 C571 H57B 109.5 . . ? H57A C571 H57B 109.5 . . ? C570 C571 H57C 109.5 . . ? H57A C571 H57C 109.5 . . ? H57B C571 H57C 109.5 . . ? C570 C572 H57D 109.5 . . ? C570 C572 H57E 109.5 . . ? H57D C572 H57E 109.5 . . ? C570 C572 H57F 109.5 . . ? H57D C572 H57F 109.5 . . ? H57E C572 H57F 109.5 . . ? C570 C573 H57G 109.5 . . ? C570 C573 H57H 109.5 . . ? H57G C573 H57H 109.5 . . ? C570 C573 H57I 109.5 . . ? H57G C573 H57I 109.5 . . ? H57H C573 H57I 109.5 . . ? C221 O22 Ti2 148.3(3) . . ? C222 C221 O22 113.3(4) . . ? C222 C221 C223 114.7(5) . . ? O22 C221 C223 109.7(4) . . ? C222 C221 H221 106.1 . . ? O22 C221 H221 106.1 . . ? C223 C221 H221 106.1 . . ? C221 C222 H22A 109.5 . . ? C221 C222 H22B 109.5 . . ? H22A C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C223 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? H22D C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22D C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C321 O32 Ti2 157.2(2) . . ? O32 C321 C323 109.9(3) . . ? O32 C321 C322 108.1(3) . . ? C323 C321 C322 112.4(3) . . ? O32 C321 H321 108.8 . . ? C323 C321 H321 108.8 . . ? C322 C321 H321 108.8 . . ? C321 C322 H32D 109.5 . . ? C321 C322 H32E 109.5 . . ? H32D C322 H32E 109.5 . . ? C321 C322 H32F 109.5 . . ? H32D C322 H32F 109.5 . . ? H32E C322 H32F 109.5 . . ? C321 C323 H32G 109.5 . . ? C321 C323 H32H 109.5 . . ? H32G C323 H32H 109.5 . . ? C321 C323 H32I 109.5 . . ? H32G C323 H32I 109.5 . . ? H32H C323 H32I 109.5 . . ? O23 Ti3 O33 104.08(11) . . ? O23 Ti3 O61 97.58(11) . . ? O33 Ti3 O61 96.01(10) . . ? O23 Ti3 O71 95.63(10) . . ? O33 Ti3 O71 97.13(10) . . ? O61 Ti3 O71 158.49(10) . . ? O23 Ti3 N61 166.89(10) . . ? O33 Ti3 N61 89.01(10) . . ? O61 Ti3 N61 80.12(10) . . ? O71 Ti3 N61 83.17(9) . . ? O23 Ti3 N71 91.31(10) . . ? O33 Ti3 N71 164.55(11) . . ? O61 Ti3 N71 83.04(9) . . ? O71 Ti3 N71 79.76(9) . . ? N61 Ti3 N71 75.62(9) . . ? C611 N61 C612 118.7(3) . . ? C611 N61 Ti3 119.0(2) . . ? C612 N61 Ti3 118.87(19) . . ? C602 O61 Ti3 121.6(2) . . ? C602 C601 C610 120.4(3) . . ? C602 C601 C611 119.1(3) . . ? C610 C601 C611 120.4(3) . . ? O61 C602 C601 119.0(3) . . ? O61 C602 C603 119.9(3) . . ? C601 C602 C603 121.1(3) . . ? C604 C603 C602 116.7(3) . . ? C604 C603 C630 122.0(3) . . ? C602 C603 C630 121.2(3) . . ? C603 C604 C605 124.1(3) . . ? C603 C604 H604 118.0 . . ? C605 C604 H604 118.0 . . ? C604 C605 C610 119.0(3) . . ? C604 C605 C606 120.9(3) . . ? C610 C605 C606 120.1(3) . . ? C607 C606 C605 122.4(3) . . ? C607 C606 H606 118.8 . . ? C605 C606 H606 118.8 . . ? C606 C607 C608 117.1(3) . . ? C606 C607 C670 122.8(3) . . ? C608 C607 C670 120.2(3) . . ? C609 C608 C607 122.2(3) . . ? C609 C608 H608 118.9 . . ? C607 C608 H608 118.9 . . ? C608 C609 C610 121.3(3) . . ? C608 C609 H609 119.3 . . ? C610 C609 H609 119.3 . . ? C605 C610 C609 117.0(3) . . ? C605 C610 C601 118.2(3) . . ? C609 C610 C601 124.7(3) . . ? N61 C611 C619 120.9(3) . . ? N61 C611 C601 119.0(3) . . ? C619 C611 C601 120.1(3) . . ? C613 C612 N61 123.2(3) . . ? C613 C612 H612 118.4 . . ? N61 C612 H612 118.4 . . ? C612 C613 C614 119.6(3) . . ? C612 C613 H613 120.2 . . ? C614 C613 H613 120.2 . . ? C619 C614 C613 118.1(3) . . ? C619 C614 C615 119.5(3) . . ? C613 C614 C615 122.4(3) . . ? C616 C615 C614 119.6(3) . . ? C616 C615 H615 120.2 . . ? C614 C615 H615 120.2 . . ? C615 C616 C617 120.6(3) . . ? C615 C616 H616 119.7 . . ? C617 C616 H616 119.7 . . ? C618 C617 C616 120.4(3) . . ? C618 C617 H617 119.8 . . ? C616 C617 H617 119.8 . . ? C617 C618 C619 120.8(3) . . ? C617 C618 H618 119.6 . . ? C619 C618 H618 119.6 . . ? C614 C619 C618 118.7(3) . . ? C614 C619 C611 118.4(3) . . ? C618 C619 C611 122.8(3) . . ? C633 C630 C603 111.6(3) . . ? C633 C630 C631 107.7(3) . . ? C603 C630 C631 108.8(3) . . ? C633 C630 C632 107.3(3) . . ? C603 C630 C632 111.1(3) . . ? C631 C630 C632 110.3(3) . . ? C630 C631 H63A 109.5 . . ? C630 C631 H63B 109.5 . . ? H63A C631 H63B 109.5 . . ? C630 C631 H63C 109.5 . . ? H63A C631 H63C 109.5 . . ? H63B C631 H63C 109.5 . . ? C630 C632 H63D 109.5 . . ? C630 C632 H63E 109.5 . . ? H63D C632 H63E 109.5 . . ? C630 C632 H63F 109.5 . . ? H63D C632 H63F 109.5 . . ? H63E C632 H63F 109.5 . . ? C630 C633 H63G 109.5 . . ? C630 C633 H63H 109.5 . . ? H63G C633 H63H 109.5 . . ? C630 C633 H63I 109.5 . . ? H63G C633 H63I 109.5 . . ? H63H C633 H63I 109.5 . . ? C673 C670 C671 108.4(3) . . ? C673 C670 C672 109.2(3) . . ? C671 C670 C672 109.1(3) . . ? C673 C670 C607 112.4(3) . . ? C671 C670 C607 109.3(3) . . ? C672 C670 C607 108.5(3) . . ? C670 C671 H67A 109.5 . . ? C670 C671 H67B 109.5 . . ? H67A C671 H67B 109.5 . . ? C670 C671 H67C 109.5 . . ? H67A C671 H67C 109.5 . . ? H67B C671 H67C 109.5 . . ? C670 C672 H67D 109.5 . . ? C670 C672 H67E 109.5 . . ? H67D C672 H67E 109.5 . . ? C670 C672 H67F 109.5 . . ? H67D C672 H67F 109.5 . . ? H67E C672 H67F 109.5 . . ? C670 C673 H67G 109.5 . . ? C670 C673 H67H 109.5 . . ? H67G C673 H67H 109.5 . . ? C670 C673 H67I 109.5 . . ? H67G C673 H67I 109.5 . . ? H67H C673 H67I 109.5 . . ? C711 N71 C712 118.6(3) . . ? C711 N71 Ti3 119.1(2) . . ? C712 N71 Ti3 118.6(2) . . ? C702 O71 Ti3 118.8(2) . . ? C702 C701 C710 120.8(3) . . ? C702 C701 C711 119.0(3) . . ? C710 C701 C711 120.3(3) . . ? O71 C702 C701 119.5(3) . . ? O71 C702 C703 119.8(3) . . ? C701 C702 C703 120.7(3) . . ? C704 C703 C702 116.8(3) . . ? C704 C703 C730 122.2(3) . . ? C702 C703 C730 120.9(3) . . ? C703 C704 C705 123.9(3) . . ? C703 C704 H704 118.0 . . ? C705 C704 H704 118.0 . . ? C704 C705 C706 122.1(3) . . ? C704 C705 C710 118.7(3) . . ? C706 C705 C710 119.1(3) . . ? C707 C706 C705 122.9(3) . . ? C707 C706 H706 118.5 . . ? C705 C706 H706 118.5 . . ? C706 C707 C708 117.3(3) . . ? C706 C707 C770 122.2(3) . . ? C708 C707 C770 120.3(3) . . ? C709 C708 C707 121.8(3) . . ? C709 C708 H708 119.1 . . ? C707 C708 H708 119.1 . . ? C708 C709 C710 121.4(3) . . ? C708 C709 H709 119.3 . . ? C710 C709 H709 119.3 . . ? C709 C710 C705 117.3(3) . . ? C709 C710 C701 124.3(3) . . ? C705 C710 C701 118.2(3) . . ? N71 C711 C719 121.4(3) . . ? N71 C711 C701 118.3(3) . . ? C719 C711 C701 120.1(3) . . ? C713 C712 N71 123.2(3) . . ? C713 C712 H712 118.4 . . ? N71 C712 H712 118.4 . . ? C712 C713 C714 120.2(3) . . ? C712 C713 H713 119.9 . . ? C714 C713 H713 119.9 . . ? C713 C714 C715 123.3(3) . . ? C713 C714 C719 117.2(3) . . ? C715 C714 C719 119.4(3) . . ? C716 C715 C714 120.7(3) . . ? C716 C715 H715 119.6 . . ? C714 C715 H715 119.6 . . ? C715 C716 C717 120.4(4) . . ? C715 C716 H716 119.8 . . ? C717 C716 H716 119.8 . . ? C718 C717 C716 120.5(4) . . ? C718 C717 H717 119.8 . . ? C716 C717 H717 119.8 . . ? C717 C718 C719 120.8(3) . . ? C717 C718 H718 119.6 . . ? C719 C718 H718 119.6 . . ? C718 C719 C714 118.2(3) . . ? C718 C719 C711 123.1(3) . . ? C714 C719 C711 118.6(3) . . ? C732 C730 C733 108.3(3) . . ? C732 C730 C703 109.7(3) . . ? C733 C730 C703 111.4(3) . . ? C732 C730 C731 110.6(3) . . ? C733 C730 C731 106.6(3) . . ? C703 C730 C731 110.2(3) . . ? C730 C731 H73D 109.5 . . ? C730 C731 H73E 109.5 . . ? H73D C731 H73E 109.5 . . ? C730 C731 H73F 109.5 . . ? H73D C731 H73F 109.5 . . ? H73E C731 H73F 109.5 . . ? C730 C732 H73G 109.5 . . ? C730 C732 H73H 109.5 . . ? H73G C732 H73H 109.5 . . ? C730 C732 H73I 109.5 . . ? H73G C732 H73I 109.5 . . ? H73H C732 H73I 109.5 . . ? C730 C733 H73J 109.5 . . ? C730 C733 H73K 109.5 . . ? H73J C733 H73K 109.5 . . ? C730 C733 H73L 109.5 . . ? H73J C733 H73L 109.5 . . ? H73K C733 H73L 109.5 . . ? C771 C770 C772 109.5(4) . . ? C771 C770 C773 109.1(3) . . ? C772 C770 C773 107.8(3) . . ? C771 C770 C707 108.5(3) . . ? C772 C770 C707 110.8(3) . . ? C773 C770 C707 111.2(3) . . ? C770 C771 H77A 109.5 . . ? C770 C771 H77B 109.5 . . ? H77A C771 H77B 109.5 . . ? C770 C771 H77C 109.5 . . ? H77A C771 H77C 109.5 . . ? H77B C771 H77C 109.5 . . ? C770 C772 H77D 109.5 . . ? C770 C772 H77E 109.5 . . ? H77D C772 H77E 109.5 . . ? C770 C772 H77F 109.5 . . ? H77D C772 H77F 109.5 . . ? H77E C772 H77F 109.5 . . ? C770 C773 H77G 109.5 . . ? C770 C773 H77H 109.5 . . ? H77G C773 H77H 109.5 . . ? C770 C773 H77I 109.5 . . ? H77G C773 H77I 109.5 . . ? H77H C773 H77I 109.5 . . ? C231 O23 Ti3 164.0(2) . . ? O23 C231 C232 109.0(3) . . ? O23 C231 C233 108.2(4) . . ? C232 C231 C233 112.8(4) . . ? O23 C231 H231 108.9 . . ? C232 C231 H231 108.9 . . ? C233 C231 H231 108.9 . . ? C231 C232 H23A 109.5 . . ? C231 C232 H23B 109.5 . . ? H23A C232 H23B 109.5 . . ? C231 C232 H23C 109.5 . . ? H23A C232 H23C 109.5 . . ? H23B C232 H23C 109.5 . . ? C231 C233 H23D 109.5 . . ? C231 C233 H23E 109.5 . . ? H23D C233 H23E 109.5 . . ? C231 C233 H23F 109.5 . . ? H23D C233 H23F 109.5 . . ? H23E C233 H23F 109.5 . . ? C331 O33 Ti3 158.0(2) . . ? O33 C331 C333 109.1(3) . . ? O33 C331 C332 109.8(3) . . ? C333 C331 C332 112.2(3) . . ? O33 C331 H331 108.6 . . ? C333 C331 H331 108.6 . . ? C332 C331 H331 108.6 . . ? C331 C332 H33D 109.5 . . ? C331 C332 H33E 109.5 . . ? H33D C332 H33E 109.5 . . ? C331 C332 H33F 109.5 . . ? H33D C332 H33F 109.5 . . ? H33E C332 H33F 109.5 . . ? C331 C333 H33G 109.5 . . ? C331 C333 H33H 109.5 . . ? H33G C333 H33H 109.5 . . ? C331 C333 H33I 109.5 . . ? H33G C333 H33I 109.5 . . ? H33H C333 H33I 109.5 . . ? O81 C811 C812 109.0(4) . . ? O81 C811 H81A 109.9 . . ? C812 C811 H81A 109.9 . . ? O81 C811 H81B 109.9 . . ? C812 C811 H81B 109.9 . . ? H81A C811 H81B 108.3 . . ? C811 C812 H81C 109.5 . . ? C811 C812 H81D 109.5 . . ? H81C C812 H81D 109.5 . . ? C811 C812 H81E 109.5 . . ? H81C C812 H81E 109.5 . . ? H81D C812 H81E 109.5 . . ? O81 C813 C814 109.7(4) . . ? O81 C813 H81F 109.7 . . ? C814 C813 H81F 109.7 . . ? O81 C813 H81G 109.7 . . ? C814 C813 H81G 109.7 . . ? H81F C813 H81G 108.2 . . ? C813 C814 H81H 109.5 . . ? C813 C814 H81I 109.5 . . ? H81H C814 H81I 109.5 . . ? C813 C814 H81J 109.5 . . ? H81H C814 H81J 109.5 . . ? H81I C814 H81J 109.5 . . ? C811 O81 C813 112.8(4) . . ? O82 C821 C822 109.1(4) . . ? O82 C821 H82A 109.9 . . ? C822 C821 H82A 109.9 . . ? O82 C821 H82B 109.9 . . ? C822 C821 H82B 109.9 . . ? H82A C821 H82B 108.3 . . ? C821 C822 H82C 109.5 . . ? C821 C822 H82D 109.5 . . ? H82C C822 H82D 109.5 . . ? C821 C822 H82E 109.5 . . ? H82C C822 H82E 109.5 . . ? H82D C822 H82E 109.5 . . ? O82 C823 C824 109.0(4) . . ? O82 C823 H82F 109.9 . . ? C824 C823 H82F 109.9 . . ? O82 C823 H82G 109.9 . . ? C824 C823 H82G 109.9 . . ? H82F C823 H82G 108.3 . . ? C823 C824 H82H 109.5 . . ? C823 C824 H82I 109.5 . . ? H82H C824 H82I 109.5 . . ? C823 C824 H82J 109.5 . . ? H82H C824 H82J 109.5 . . ? H82I C824 H82J 109.5 . . ? C823 O82 C821 113.7(4) . . ? O83 C831 C832 110.0(4) . . ? O83 C831 H83A 109.7 . . ? C832 C831 H83A 109.7 . . ? O83 C831 H83B 109.7 . . ? C832 C831 H83B 109.7 . . ? H83A C831 H83B 108.2 . . ? C831 C832 H83C 109.5 . . ? C831 C832 H83D 109.5 . . ? H83C C832 H83D 109.5 . . ? C831 C832 H83E 109.5 . . ? H83C C832 H83E 109.5 . . ? H83D C832 H83E 109.5 . . ? O83 C833 C834 108.3(5) . . ? O83 C833 H83F 110.0 . . ? C834 C833 H83F 110.0 . . ? O83 C833 H83G 110.0 . . ? C834 C833 H83G 110.0 . . ? H83F C833 H83G 108.4 . . ? C833 C834 H83H 109.5 . . ? C833 C834 H83I 109.5 . . ? H83H C834 H83I 109.5 . . ? C833 C834 H83J 109.5 . . ? H83H C834 H83J 109.5 . . ? H83I C834 H83J 109.5 . . ? C833 O83 C831 113.1(4) . . ? O84 C841 C842 111.3(5) . . ? O84 C841 H84A 109.4 . . ? C842 C841 H84A 109.4 . . ? O84 C841 H84B 109.4 . . ? C842 C841 H84B 109.4 . . ? H84A C841 H84B 108.0 . . ? C841 C842 H84C 109.5 . . ? C841 C842 H84D 109.5 . . ? H84C C842 H84D 109.5 . . ? C841 C842 H84E 109.5 . . ? H84C C842 H84E 109.5 . . ? H84D C842 H84E 109.5 . . ? O84 C843 C844 112.7(6) . . ? O84 C843 H84F 109.1 . . ? C844 C843 H84F 109.1 . . ? O84 C843 H84G 109.1 . . ? C844 C843 H84G 109.1 . . ? H84F C843 H84G 107.8 . . ? C843 C844 H84H 109.5 . . ? C843 C844 H84I 109.5 . . ? H84H C844 H84I 109.5 . . ? C843 C844 H84J 109.5 . . ? H84H C844 H84J 109.5 . . ? H84I C844 H84J 109.5 . . ? C843 O84 C841 115.8(5) . . ? O85 C851 C852 112(2) . . ? O85 C851 H85A 109.3 . . ? C852 C851 H85A 109.3 . . ? O85 C851 H85B 109.3 . . ? C852 C851 H85B 109.3 . . ? H85A C851 H85B 107.9 . . ? O85 C853 C854 109(3) . . ? O85 C853 H85F 109.8 . . ? C854 C853 H85F 109.8 . . ? O85 C853 H85G 109.8 . . ? C854 C853 H85G 109.8 . . ? H85F C853 H85G 108.2 . . ? C851 O85 C853 113(2) . . ? O86 C861 C862 112(2) . . ? O86 C861 H86A 109.2 . . ? C862 C861 H86A 109.2 . . ? O86 C861 H86B 109.2 . . ? C862 C861 H86B 109.2 . . ? H86A C861 H86B 107.9 . . ? C861 C862 H86C 109.5 . . ? C861 C862 H86D 109.5 . . ? H86C C862 H86D 109.5 . . ? C861 C862 H86E 109.5 . . ? H86C C862 H86E 109.5 . . ? H86D C862 H86E 109.5 . . ? O86 C863 C864 109(2) . . ? O86 C863 H86F 110.0 . . ? C864 C863 H86F 110.0 . . ? O86 C863 H86G 110.0 . . ? C864 C863 H86G 110.0 . . ? H86F C863 H86G 108.4 . . ? C863 C864 H86H 109.5 . . ? C863 C864 H86I 109.5 . . ? H86H C864 H86I 109.5 . . ? C863 C864 H86J 109.5 . . ? H86H C864 H86J 109.5 . . ? H86I C864 H86J 109.5 . . ? C861 O86 C863 117.9(15) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.818 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.074 #===END data_13 _database_code_depnum_ccdc_archive 'CCDC 728918' _chemical_formula_structural '[Zn{L(H)}2].2(CH2Cl2)' _chemical_formula_moiety 'C54 H56 N2 O2 Zn, 2(C H2 Cl2)' _chemical_formula_sum 'C56 H60 Cl4 N2 O2 Zn' _chemical_formula_weight 1000.23 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3702(7) _cell_length_b 22.8448(8) _cell_length_c 19.5818(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.385(5) _cell_angle_gamma 90.00 _cell_volume 4986.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.751 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_T_max 0.893 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 60843 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11364 _reflns_number_gt 7776 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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_number_reflns 11364 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Zn Zn 0.61836(2) 0.770232(11) 0.372243(11) 0.01485(8) Uani 1 1 d . . . C1 C 0.56694(18) 0.81494(9) 0.50790(10) 0.0139(4) Uani 1 1 d . . . C2 C 0.50411(18) 0.76502(9) 0.47873(10) 0.0127(4) Uani 1 1 d . . . O2 O 0.54996(12) 0.72742(6) 0.43914(7) 0.0147(3) Uani 1 1 d . . . C3 C 0.38541(18) 0.75320(9) 0.49236(10) 0.0139(4) Uani 1 1 d . . . C4 C 0.32900(19) 0.79743(10) 0.51998(10) 0.0173(4) Uani 1 1 d . . . H4 H 0.2516 0.7909 0.5271 0.021 Uiso 1 1 calc R . . C5 C 0.3159(2) 0.89886(10) 0.56030(10) 0.0181(4) Uani 1 1 d . . . H5 H 0.2352 0.8925 0.5606 0.022 Uiso 1 1 calc R . . C6 C 0.3646(2) 0.95277(10) 0.58123(11) 0.0191(5) Uani 1 1 d . . . C7 C 0.4873(2) 0.95976(10) 0.57944(11) 0.0219(5) Uani 1 1 d . . . H7 H 0.5239 0.9954 0.5933 0.026 Uiso 1 1 calc R . . C8 C 0.5547(2) 0.91628(10) 0.55812(11) 0.0201(5) Uani 1 1 d . . . H8 H 0.6354 0.9231 0.5582 0.024 Uiso 1 1 calc R . . C9 C 0.50397(19) 0.86102(9) 0.53582(10) 0.0150(4) Uani 1 1 d . . . C10 C 0.38234(19) 0.85285(9) 0.53841(10) 0.0160(4) Uani 1 1 d . . . C11 C 0.69718(18) 0.81958(9) 0.50790(10) 0.0144(4) Uani 1 1 d . . . N12 N 0.73265(15) 0.81384(8) 0.44723(9) 0.0147(4) Uani 1 1 d . . . C13 C 0.85118(19) 0.81846(9) 0.44384(11) 0.0173(4) Uani 1 1 d . . . H13 H 0.8727 0.8157 0.4005 0.021 Uiso 1 1 calc R . . C14 C 0.93871(19) 0.82697(10) 0.50095(12) 0.0204(5) Uani 1 1 d . . . H14 H 1.0182 0.8313 0.4965 0.024 Uiso 1 1 calc R . . C15 C 0.9957(2) 0.83171(10) 0.62972(12) 0.0238(5) Uani 1 1 d . . . H15 H 1.0765 0.8340 0.6275 0.029 Uiso 1 1 calc R . . C16 C 0.9629(2) 0.83086(11) 0.69269(12) 0.0266(5) Uani 1 1 d . . . H16 H 1.0214 0.8323 0.7332 0.032 Uiso 1 1 calc R . . C17 C 0.8410(2) 0.82788(10) 0.69706(12) 0.0255(5) Uani 1 1 d . . . H17 H 0.8194 0.8274 0.7405 0.031 Uiso 1 1 calc R . . C18 C 0.7537(2) 0.82571(10) 0.63781(11) 0.0203(5) Uani 1 1 d . . . H18 H 0.6734 0.8240 0.6414 0.024 Uiso 1 1 calc R . . C19 C 0.78471(19) 0.82608(9) 0.57142(11) 0.0163(4) Uani 1 1 d . . . C20 C 0.90762(19) 0.82920(9) 0.56699(11) 0.0176(4) Uani 1 1 d . . . C301 C 0.32729(19) 0.69309(9) 0.47525(11) 0.0164(4) Uani 1 1 d . . . C302 C 0.2137(2) 0.68689(11) 0.50559(12) 0.0246(5) Uani 1 1 d . . . H30A H 0.1791 0.6489 0.4943 0.037 Uiso 1 1 calc R . . H30B H 0.1570 0.7165 0.4862 0.037 Uiso 1 1 calc R . . H30C H 0.2338 0.6913 0.5553 0.037 Uiso 1 1 calc R . . C303 C 0.4136(2) 0.64478(10) 0.50848(13) 0.0241(5) Uani 1 1 d . . . H30D H 0.3764 0.6073 0.4978 0.036 Uiso 1 1 calc R . . H30E H 0.4323 0.6501 0.5581 0.036 Uiso 1 1 calc R . . H30F H 0.4860 0.6467 0.4903 0.036 Uiso 1 1 calc R . . C304 C 0.2943(2) 0.68357(11) 0.39624(11) 0.0250(5) Uani 1 1 d . . . H30G H 0.2578 0.6458 0.3867 0.038 Uiso 1 1 calc R . . H30H H 0.3656 0.6856 0.3769 0.038 Uiso 1 1 calc R . . H30I H 0.2390 0.7134 0.3756 0.038 Uiso 1 1 calc R . . C601 C 0.2872(2) 1.00104(10) 0.60403(11) 0.0222(5) Uani 1 1 d . . . C602 C 0.1869(2) 1.01846(11) 0.54285(13) 0.0295(6) Uani 1 1 d . . . H60A H 0.1400 0.9846 0.5262 0.044 Uiso 1 1 calc R . . H60B H 0.2216 1.0343 0.5060 0.044 Uiso 1 1 calc R . . H60C H 0.1365 1.0474 0.5581 0.044 Uiso 1 1 calc R . . C603 C 0.2287(3) 0.97921(11) 0.66362(13) 0.0313(6) Uani 1 1 d . . . H60D H 0.1823 0.9447 0.6489 0.047 Uiso 1 1 calc R . . H60E H 0.1773 1.0092 0.6758 0.047 Uiso 1 1 calc R . . H60F H 0.2900 0.9701 0.7034 0.047 Uiso 1 1 calc R . . C604 C 0.3609(2) 1.05578(10) 0.62950(12) 0.0268(5) Uani 1 1 d . . . H60G H 0.3095 1.0849 0.6435 0.040 Uiso 1 1 calc R . . H60H H 0.3962 1.0710 0.5925 0.040 Uiso 1 1 calc R . . H60I H 0.4231 1.0457 0.6684 0.040 Uiso 1 1 calc R . . C31 C 0.66423(18) 0.82124(9) 0.23749(10) 0.0141(4) Uani 1 1 d . . . C32 C 0.73390(17) 0.77283(9) 0.26572(9) 0.0128(4) Uani 1 1 d . . . O32 O 0.69229(13) 0.73278(6) 0.30424(7) 0.0155(3) Uani 1 1 d . . . C33 C 0.85331(18) 0.76597(9) 0.25164(10) 0.0145(4) Uani 1 1 d . . . C34 C 0.90202(19) 0.81175(10) 0.22245(10) 0.0180(4) Uani 1 1 d . . . H34 H 0.9798 0.8078 0.2147 0.022 Uiso 1 1 calc R . . C35 C 0.8978(2) 0.91307(10) 0.17743(11) 0.0191(5) Uani 1 1 d . . . H35 H 0.9785 0.9096 0.1753 0.023 Uiso 1 1 calc R . . C36 C 0.8395(2) 0.96425(10) 0.15552(10) 0.0192(5) Uani 1 1 d . . . C37 C 0.7172(2) 0.96775(10) 0.16075(11) 0.0211(5) Uani 1 1 d . . . H37 H 0.6746 1.0018 0.1462 0.025 Uiso 1 1 calc R . . C38 C 0.6598(2) 0.92284(10) 0.18641(11) 0.0192(5) Uani 1 1 d . . . H38 H 0.5799 0.9275 0.1898 0.023 Uiso 1 1 calc R . . C39 C 0.71837(19) 0.86943(9) 0.20797(10) 0.0154(4) Uani 1 1 d . . . C40 C 0.84046(19) 0.86536(10) 0.20303(10) 0.0164(4) Uani 1 1 d . . . C41 C 0.53457(18) 0.82259(9) 0.23885(10) 0.0142(4) Uani 1 1 d . . . N42 N 0.50055(15) 0.81518(8) 0.29971(9) 0.0160(4) Uani 1 1 d . . . C43 C 0.3823(2) 0.81916(10) 0.30375(12) 0.0210(5) Uani 1 1 d . . . H43 H 0.3611 0.8149 0.3470 0.025 Uiso 1 1 calc R . . C44 C 0.2939(2) 0.82915(10) 0.24680(12) 0.0231(5) Uani 1 1 d . . . H44 H 0.2147 0.8338 0.2518 0.028 Uiso 1 1 calc R . . C45 C 0.2353(2) 0.83631(11) 0.11818(12) 0.0263(5) Uani 1 1 d . . . H45 H 0.1547 0.8395 0.1207 0.032 Uiso 1 1 calc R . . C46 C 0.2676(2) 0.83536(10) 0.05500(12) 0.0270(5) Uani 1 1 d . . . H46 H 0.2089 0.8375 0.0146 0.032 Uiso 1 1 calc R . . C47 C 0.3885(2) 0.83113(10) 0.05005(12) 0.0245(5) Uani 1 1 d . . . H47 H 0.4093 0.8304 0.0065 0.029 Uiso 1 1 calc R . . C48 C 0.4765(2) 0.82805(10) 0.10894(11) 0.0202(5) Uani 1 1 d . . . H48 H 0.5565 0.8256 0.1050 0.024 Uiso 1 1 calc R . . C49 C 0.44626(19) 0.82861(9) 0.17566(11) 0.0157(4) Uani 1 1 d . . . C50 C 0.32369(19) 0.83240(10) 0.18058(12) 0.0204(5) Uani 1 1 d . . . C331 C 0.92100(19) 0.70806(10) 0.26981(11) 0.0176(4) Uani 1 1 d . . . C332 C 0.8439(2) 0.65689(10) 0.23602(13) 0.0261(5) Uani 1 1 d . . . H33A H 0.8867 0.6209 0.2475 0.039 Uiso 1 1 calc R . . H33B H 0.8265 0.6619 0.1864 0.039 Uiso 1 1 calc R . . H33C H 0.7703 0.6558 0.2530 0.039 Uiso 1 1 calc R . . C333 C 0.9533(2) 0.69898(11) 0.34897(11) 0.0247(5) Uani 1 1 d . . . H33D H 0.9958 0.6627 0.3590 0.037 Uiso 1 1 calc R . . H33E H 0.8812 0.6979 0.3675 0.037 Uiso 1 1 calc R . . H33F H 1.0030 0.7307 0.3699 0.037 Uiso 1 1 calc R . . C334 C 1.0371(2) 0.70665(11) 0.24134(13) 0.0272(5) Uani 1 1 d . . . H33G H 1.0777 0.6702 0.2536 0.041 Uiso 1 1 calc R . . H33H H 1.0881 0.7384 0.2610 0.041 Uiso 1 1 calc R . . H33I H 1.0184 0.7105 0.1916 0.041 Uiso 1 1 calc R . . C361 C 0.8991(2) 1.01636(10) 0.12651(12) 0.0241(5) Uani 1 1 d . . . C362 C 0.8331(3) 1.02875(11) 0.05155(13) 0.0330(6) Uani 1 1 d . . . H36A H 0.8701 1.0614 0.0332 0.049 Uiso 1 1 calc R . . H36B H 0.7506 1.0377 0.0515 0.049 Uiso 1 1 calc R . . H36C H 0.8375 0.9949 0.0232 0.049 Uiso 1 1 calc R . . C363 C 0.8928(3) 1.07065(12) 0.17134(15) 0.0448(8) Uani 1 1 d . . . H36D H 0.9299 1.1031 0.1527 0.067 Uiso 1 1 calc R . . H36E H 0.9341 1.0631 0.2182 0.067 Uiso 1 1 calc R . . H36F H 0.8104 1.0798 0.1713 0.067 Uiso 1 1 calc R . . C364 C 1.0306(2) 1.00444(12) 0.12452(15) 0.0365(6) Uani 1 1 d . . . H36G H 1.0643 1.0380 0.1059 0.055 Uiso 1 1 calc R . . H36H H 1.0360 0.9711 0.0955 0.055 Uiso 1 1 calc R . . H36I H 1.0742 0.9968 0.1709 0.055 Uiso 1 1 calc R . . C51 C 0.2143(3) 0.94330(15) 0.37346(18) 0.0598(9) Uani 1 1 d . . . H51A H 0.2569 0.9474 0.4213 0.072 Uiso 1 1 calc R . . H51B H 0.2727 0.9335 0.3453 0.072 Uiso 1 1 calc R . . Cl52 Cl 0.11059(9) 0.88474(5) 0.36906(5) 0.0682(3) Uani 1 1 d . . . Cl53 Cl 0.14977(11) 1.00928(5) 0.34565(5) 0.0807(3) Uani 1 1 d . . . C61 C 0.1469(3) 0.49125(17) 0.37649(18) 0.0648(10) Uani 1 1 d . . . H61A H 0.1194 0.4513 0.3798 0.078 Uiso 1 1 calc R . . H61B H 0.2324 0.4923 0.3955 0.078 Uiso 1 1 calc R . . Cl62 Cl 0.12091(11) 0.51251(7) 0.28903(6) 0.1053(5) Uani 1 1 d . . . Cl63 Cl 0.07347(9) 0.53670(5) 0.42488(6) 0.0815(3) Uani 1 1 d . . . 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 Zn 0.01319(12) 0.02021(14) 0.01148(12) 0.00022(10) 0.00322(8) 0.00011(11) C1 0.0124(10) 0.0185(11) 0.0108(9) 0.0016(8) 0.0022(8) -0.0015(8) C2 0.0138(10) 0.0155(11) 0.0089(9) 0.0017(8) 0.0021(7) 0.0020(8) O2 0.0147(7) 0.0162(8) 0.0146(7) -0.0009(6) 0.0059(5) 0.0000(6) C3 0.0137(10) 0.0166(11) 0.0108(9) 0.0027(7) 0.0008(8) -0.0001(8) C4 0.0121(10) 0.0241(12) 0.0165(10) 0.0001(9) 0.0050(8) -0.0009(9) C5 0.0167(11) 0.0210(12) 0.0177(10) 0.0016(8) 0.0063(8) 0.0016(9) C6 0.0238(12) 0.0189(12) 0.0154(10) 0.0010(8) 0.0055(9) 0.0052(9) C7 0.0266(12) 0.0188(12) 0.0209(11) -0.0022(9) 0.0062(9) -0.0033(10) C8 0.0184(11) 0.0212(12) 0.0220(11) -0.0019(9) 0.0067(9) -0.0034(9) C9 0.0156(10) 0.0177(11) 0.0120(9) 0.0013(8) 0.0036(8) 0.0000(8) C10 0.0181(11) 0.0171(11) 0.0129(10) 0.0009(8) 0.0033(8) 0.0012(9) C11 0.0145(10) 0.0123(11) 0.0161(10) -0.0002(8) 0.0025(8) -0.0011(8) N12 0.0132(9) 0.0166(9) 0.0147(8) -0.0003(7) 0.0040(7) -0.0009(7) C13 0.0154(10) 0.0191(11) 0.0196(11) -0.0007(8) 0.0086(8) -0.0006(9) C14 0.0110(10) 0.0222(12) 0.0290(12) -0.0024(9) 0.0063(9) -0.0011(9) C15 0.0172(11) 0.0237(13) 0.0276(12) -0.0033(9) -0.0029(9) -0.0017(9) C16 0.0287(13) 0.0225(13) 0.0233(12) -0.0011(9) -0.0081(10) -0.0020(10) C17 0.0332(14) 0.0270(14) 0.0152(11) -0.0002(9) 0.0022(10) -0.0027(11) C18 0.0215(12) 0.0229(12) 0.0168(11) -0.0004(9) 0.0045(9) -0.0025(9) C19 0.0167(11) 0.0134(11) 0.0177(10) -0.0012(8) 0.0010(8) -0.0015(8) C20 0.0171(11) 0.0132(11) 0.0213(11) -0.0012(8) 0.0009(9) -0.0011(9) C301 0.0144(10) 0.0172(11) 0.0177(10) -0.0015(8) 0.0030(8) -0.0035(8) C302 0.0190(12) 0.0255(13) 0.0310(13) -0.0038(10) 0.0094(10) -0.0083(10) C303 0.0229(12) 0.0184(12) 0.0322(13) 0.0045(9) 0.0083(10) -0.0019(9) C304 0.0210(12) 0.0327(14) 0.0207(11) -0.0050(9) 0.0022(9) -0.0074(10) C601 0.0292(13) 0.0179(12) 0.0210(11) -0.0006(9) 0.0092(10) 0.0047(10) C602 0.0306(14) 0.0263(14) 0.0308(13) 0.0014(10) 0.0045(11) 0.0088(11) C603 0.0455(16) 0.0217(13) 0.0321(13) 0.0006(10) 0.0209(12) 0.0090(11) C604 0.0364(15) 0.0183(12) 0.0263(12) -0.0009(10) 0.0077(11) 0.0041(10) C31 0.0125(10) 0.0192(11) 0.0111(9) -0.0012(8) 0.0031(8) 0.0002(8) C32 0.0139(10) 0.0161(11) 0.0081(9) -0.0028(8) 0.0012(7) -0.0021(8) O32 0.0161(7) 0.0166(8) 0.0149(7) 0.0017(6) 0.0055(6) -0.0007(6) C33 0.0128(10) 0.0194(11) 0.0108(9) -0.0024(8) 0.0010(7) -0.0002(8) C34 0.0121(10) 0.0256(12) 0.0165(10) -0.0006(9) 0.0036(8) 0.0004(9) C35 0.0161(11) 0.0244(13) 0.0175(10) -0.0007(9) 0.0052(8) -0.0032(9) C36 0.0231(12) 0.0220(12) 0.0131(10) -0.0036(8) 0.0051(9) -0.0037(9) C37 0.0245(12) 0.0188(12) 0.0192(11) 0.0023(9) 0.0027(9) 0.0023(9) C38 0.0161(11) 0.0212(12) 0.0206(11) 0.0011(9) 0.0044(9) 0.0024(9) C39 0.0158(10) 0.0192(11) 0.0108(9) 0.0002(8) 0.0018(8) -0.0001(8) C40 0.0159(10) 0.0210(12) 0.0123(10) -0.0013(8) 0.0030(8) -0.0024(9) C41 0.0142(10) 0.0115(11) 0.0169(10) 0.0004(8) 0.0030(8) 0.0001(8) N42 0.0137(9) 0.0170(10) 0.0181(9) 0.0001(7) 0.0051(7) 0.0013(7) C43 0.0164(11) 0.0248(13) 0.0238(11) 0.0046(9) 0.0092(9) 0.0037(9) C44 0.0106(10) 0.0275(13) 0.0319(13) 0.0054(10) 0.0061(9) 0.0028(9) C45 0.0145(11) 0.0271(14) 0.0334(13) 0.0046(10) -0.0047(10) 0.0009(10) C46 0.0254(13) 0.0233(13) 0.0250(12) 0.0023(9) -0.0130(10) 0.0009(10) C47 0.0290(13) 0.0254(13) 0.0169(11) 0.0001(9) -0.0007(10) 0.0019(10) C48 0.0191(11) 0.0203(12) 0.0202(11) 0.0003(9) 0.0017(9) 0.0018(9) C49 0.0149(10) 0.0131(11) 0.0180(10) 0.0006(8) 0.0007(8) 0.0006(8) C50 0.0142(11) 0.0184(12) 0.0264(12) 0.0028(9) -0.0015(9) 0.0012(9) C331 0.0135(10) 0.0216(12) 0.0184(10) -0.0009(8) 0.0048(8) 0.0027(9) C332 0.0258(13) 0.0217(13) 0.0320(13) -0.0074(10) 0.0087(10) 0.0016(10) C333 0.0227(12) 0.0290(14) 0.0211(11) 0.0044(9) 0.0010(9) 0.0107(10) C334 0.0196(12) 0.0287(14) 0.0360(14) 0.0036(10) 0.0122(10) 0.0078(10) C361 0.0301(14) 0.0187(12) 0.0248(12) 0.0003(9) 0.0085(10) -0.0049(10) C362 0.0456(16) 0.0243(14) 0.0304(13) 0.0089(10) 0.0110(12) -0.0004(12) C363 0.069(2) 0.0285(16) 0.0435(17) -0.0104(12) 0.0270(16) -0.0195(14) C364 0.0305(14) 0.0367(16) 0.0456(16) 0.0102(12) 0.0155(12) -0.0080(12) C51 0.058(2) 0.067(2) 0.056(2) -0.0220(18) 0.0156(17) -0.0114(19) Cl52 0.0676(6) 0.0799(7) 0.0664(6) -0.0109(5) 0.0359(5) -0.0257(5) Cl53 0.1047(9) 0.0730(7) 0.0525(5) 0.0097(5) -0.0135(5) -0.0078(6) C61 0.046(2) 0.066(2) 0.071(3) -0.0046(19) -0.0162(18) 0.0033(18) Cl62 0.0789(8) 0.1420(12) 0.0837(8) 0.0254(7) -0.0116(6) -0.0415(8) Cl63 0.0523(6) 0.0606(6) 0.1203(9) -0.0146(6) -0.0102(6) 0.0021(5) _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 Zn O32 1.9114(14) . ? Zn O2 1.9182(14) . ? Zn N12 2.0209(17) . ? Zn N42 2.0286(18) . ? C1 C2 1.406(3) . ? C1 C9 1.440(3) . ? C1 C11 1.485(3) . ? C2 O2 1.331(2) . ? C2 C3 1.452(3) . ? C3 C4 1.365(3) . ? C3 C301 1.532(3) . ? C4 C10 1.419(3) . ? C4 H4 0.9300 . ? C5 C6 1.379(3) . ? C5 C10 1.410(3) . ? C5 H5 0.9300 . ? C6 C7 1.412(3) . ? C6 C601 1.531(3) . ? C7 C8 1.369(3) . ? C7 H7 0.9300 . ? C8 C9 1.420(3) . ? C8 H8 0.9300 . ? C9 C10 1.406(3) . ? C11 N12 1.334(3) . ? C11 C19 1.439(3) . ? N12 C13 1.366(3) . ? C13 C14 1.356(3) . ? C13 H13 0.9300 . ? C14 C20 1.407(3) . ? C14 H14 0.9300 . ? C15 C16 1.357(3) . ? C15 C20 1.425(3) . ? C15 H15 0.9300 . ? C16 C17 1.408(4) . ? C16 H16 0.9300 . ? C17 C18 1.370(3) . ? C17 H17 0.9300 . ? C18 C19 1.413(3) . ? C18 H18 0.9300 . ? C19 C20 1.419(3) . ? C301 C302 1.531(3) . ? C301 C303 1.534(3) . ? C301 C304 1.534(3) . ? C302 H30A 0.9600 . ? C302 H30B 0.9600 . ? C302 H30C 0.9600 . ? C303 H30D 0.9600 . ? C303 H30E 0.9600 . ? C303 H30F 0.9600 . ? C304 H30G 0.9600 . ? C304 H30H 0.9600 . ? C304 H30I 0.9600 . ? C601 C604 1.533(3) . ? C601 C602 1.534(3) . ? C601 C603 1.536(3) . ? C602 H60A 0.9600 . ? C602 H60B 0.9600 . ? C602 H60C 0.9600 . ? C603 H60D 0.9600 . ? C603 H60E 0.9600 . ? C603 H60F 0.9600 . ? C604 H60G 0.9600 . ? C604 H60H 0.9600 . ? C604 H60I 0.9600 . ? C31 C32 1.408(3) . ? C31 C39 1.437(3) . ? C31 C41 1.480(3) . ? C32 O32 1.331(2) . ? C32 C33 1.446(3) . ? C33 C34 1.361(3) . ? C33 C331 1.537(3) . ? C34 C40 1.425(3) . ? C34 H34 0.9300 . ? C35 C36 1.371(3) . ? C35 C40 1.412(3) . ? C35 H35 0.9300 . ? C36 C37 1.416(3) . ? C36 C361 1.534(3) . ? C37 C38 1.364(3) . ? C37 H37 0.9300 . ? C38 C39 1.414(3) . ? C38 H38 0.9300 . ? C39 C40 1.414(3) . ? C41 N42 1.334(3) . ? C41 C49 1.438(3) . ? N42 C43 1.366(3) . ? C43 C44 1.365(3) . ? C43 H43 0.9300 . ? C44 C50 1.405(3) . ? C44 H44 0.9300 . ? C45 C46 1.359(3) . ? C45 C50 1.424(3) . ? C45 H45 0.9300 . ? C46 C47 1.401(3) . ? C46 H46 0.9300 . ? C47 C48 1.371(3) . ? C47 H47 0.9300 . ? C48 C49 1.415(3) . ? C48 H48 0.9300 . ? C49 C50 1.418(3) . ? C331 C332 1.531(3) . ? C331 C334 1.531(3) . ? C331 C333 1.535(3) . ? C332 H33A 0.9600 . ? C332 H33B 0.9600 . ? C332 H33C 0.9600 . ? C333 H33D 0.9600 . ? C333 H33E 0.9600 . ? C333 H33F 0.9600 . ? C334 H33G 0.9600 . ? C334 H33H 0.9600 . ? C334 H33I 0.9600 . ? C361 C364 1.528(3) . ? C361 C363 1.529(3) . ? C361 C362 1.537(3) . ? C362 H36A 0.9600 . ? C362 H36B 0.9600 . ? C362 H36C 0.9600 . ? C363 H36D 0.9600 . ? C363 H36E 0.9600 . ? C363 H36F 0.9600 . ? C364 H36G 0.9600 . ? C364 H36H 0.9600 . ? C364 H36I 0.9600 . ? C51 Cl53 1.717(4) . ? C51 Cl52 1.774(4) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C61 Cl63 1.728(4) . ? C61 Cl62 1.748(4) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? 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 O32 Zn O2 122.74(6) . . ? O32 Zn N12 114.75(7) . . ? O2 Zn N12 92.54(6) . . ? O32 Zn N42 93.40(6) . . ? O2 Zn N42 115.82(7) . . ? N12 Zn N42 120.02(7) . . ? C2 C1 C9 119.75(18) . . ? C2 C1 C11 119.01(18) . . ? C9 C1 C11 121.22(18) . . ? O2 C2 C1 122.30(18) . . ? O2 C2 C3 118.18(18) . . ? C1 C2 C3 119.52(18) . . ? C2 O2 Zn 109.09(12) . . ? C4 C3 C2 117.50(19) . . ? C4 C3 C301 122.28(19) . . ? C2 C3 C301 120.21(18) . . ? C3 C4 C10 123.4(2) . . ? C3 C4 H4 118.3 . . ? C10 C4 H4 118.3 . . ? C6 C5 C10 123.2(2) . . ? C6 C5 H5 118.4 . . ? C10 C5 H5 118.4 . . ? C5 C6 C7 115.8(2) . . ? C5 C6 C601 120.6(2) . . ? C7 C6 C601 123.6(2) . . ? C8 C7 C6 122.7(2) . . ? C8 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? C7 C8 C9 121.4(2) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C10 C9 C8 116.69(19) . . ? C10 C9 C1 118.87(19) . . ? C8 C9 C1 124.35(19) . . ? C9 C10 C5 120.1(2) . . ? C9 C10 C4 118.88(19) . . ? C5 C10 C4 121.0(2) . . ? N12 C11 C19 120.05(19) . . ? N12 C11 C1 118.02(17) . . ? C19 C11 C1 121.80(18) . . ? C11 N12 C13 120.67(18) . . ? C11 N12 Zn 115.56(14) . . ? C13 N12 Zn 120.11(14) . . ? C14 C13 N12 122.77(19) . . ? C14 C13 H13 118.6 . . ? N12 C13 H13 118.6 . . ? C13 C14 C20 119.1(2) . . ? C13 C14 H14 120.4 . . ? C20 C14 H14 120.4 . . ? C16 C15 C20 120.7(2) . . ? C16 C15 H15 119.7 . . ? C20 C15 H15 119.7 . . ? C15 C16 C17 120.4(2) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 120.5(2) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 120.6(2) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C20 118.96(19) . . ? C18 C19 C11 122.6(2) . . ? C20 C19 C11 118.28(19) . . ? C14 C20 C19 118.91(19) . . ? C14 C20 C15 122.2(2) . . ? C19 C20 C15 118.9(2) . . ? C302 C301 C3 111.02(18) . . ? C302 C301 C303 106.66(18) . . ? C3 C301 C303 109.88(17) . . ? C302 C301 C304 108.76(18) . . ? C3 C301 C304 110.89(17) . . ? C303 C301 C304 109.53(19) . . ? C301 C302 H30A 109.5 . . ? C301 C302 H30B 109.5 . . ? H30A C302 H30B 109.5 . . ? C301 C302 H30C 109.5 . . ? H30A C302 H30C 109.5 . . ? H30B C302 H30C 109.5 . . ? C301 C303 H30D 109.5 . . ? C301 C303 H30E 109.5 . . ? H30D C303 H30E 109.5 . . ? C301 C303 H30F 109.5 . . ? H30D C303 H30F 109.5 . . ? H30E C303 H30F 109.5 . . ? C301 C304 H30G 109.5 . . ? C301 C304 H30H 109.5 . . ? H30G C304 H30H 109.5 . . ? C301 C304 H30I 109.5 . . ? H30G C304 H30I 109.5 . . ? H30H C304 H30I 109.5 . . ? C6 C601 C604 111.9(2) . . ? C6 C601 C602 109.89(18) . . ? C604 C601 C602 108.47(19) . . ? C6 C601 C603 110.35(18) . . ? C604 C601 C603 107.97(19) . . ? C602 C601 C603 108.1(2) . . ? C601 C602 H60A 109.5 . . ? C601 C602 H60B 109.5 . . ? H60A C602 H60B 109.5 . . ? C601 C602 H60C 109.5 . . ? H60A C602 H60C 109.5 . . ? H60B C602 H60C 109.5 . . ? C601 C603 H60D 109.5 . . ? C601 C603 H60E 109.5 . . ? H60D C603 H60E 109.5 . . ? C601 C603 H60F 109.5 . . ? H60D C603 H60F 109.5 . . ? H60E C603 H60F 109.5 . . ? C601 C604 H60G 109.5 . . ? C601 C604 H60H 109.5 . . ? H60G C604 H60H 109.5 . . ? C601 C604 H60I 109.5 . . ? H60G C604 H60I 109.5 . . ? H60H C604 H60I 109.5 . . ? C32 C31 C39 120.46(18) . . ? C32 C31 C41 119.63(18) . . ? C39 C31 C41 119.91(18) . . ? O32 C32 C31 121.81(18) . . ? O32 C32 C33 119.05(18) . . ? C31 C32 C33 119.13(18) . . ? C32 O32 Zn 109.98(12) . . ? C34 C33 C32 118.16(19) . . ? C34 C33 C331 122.14(19) . . ? C32 C33 C331 119.70(18) . . ? C33 C34 C40 123.6(2) . . ? C33 C34 H34 118.2 . . ? C40 C34 H34 118.2 . . ? C36 C35 C40 122.7(2) . . ? C36 C35 H35 118.6 . . ? C40 C35 H35 118.6 . . ? C35 C36 C37 116.5(2) . . ? C35 C36 C361 123.8(2) . . ? C37 C36 C361 119.7(2) . . ? C38 C37 C36 122.1(2) . . ? C38 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? C37 C38 C39 121.8(2) . . ? C37 C38 H38 119.1 . . ? C39 C38 H38 119.1 . . ? C40 C39 C38 116.57(19) . . ? C40 C39 C31 118.79(19) . . ? C38 C39 C31 124.55(19) . . ? C35 C40 C39 120.1(2) . . ? C35 C40 C34 121.4(2) . . ? C39 C40 C34 118.40(19) . . ? N42 C41 C49 120.29(19) . . ? N42 C41 C31 118.60(17) . . ? C49 C41 C31 121.02(18) . . ? C41 N42 C43 120.38(18) . . ? C41 N42 Zn 114.94(14) . . ? C43 N42 Zn 120.98(14) . . ? C44 C43 N42 122.6(2) . . ? C44 C43 H43 118.7 . . ? N42 C43 H43 118.7 . . ? C43 C44 C50 119.3(2) . . ? C43 C44 H44 120.3 . . ? C50 C44 H44 120.3 . . ? C46 C45 C50 120.6(2) . . ? C46 C45 H45 119.7 . . ? C50 C45 H45 119.7 . . ? C45 C46 C47 120.7(2) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C48 C47 C46 120.6(2) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C49 120.4(2) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C48 C49 C50 118.96(19) . . ? C48 C49 C41 122.5(2) . . ? C50 C49 C41 118.42(19) . . ? C44 C50 C49 118.61(19) . . ? C44 C50 C45 122.5(2) . . ? C49 C50 C45 118.8(2) . . ? C332 C331 C334 106.71(18) . . ? C332 C331 C333 109.61(19) . . ? C334 C331 C333 108.26(19) . . ? C332 C331 C33 109.86(18) . . ? C334 C331 C33 111.24(18) . . ? C333 C331 C33 111.05(17) . . ? C331 C332 H33A 109.5 . . ? C331 C332 H33B 109.5 . . ? H33A C332 H33B 109.5 . . ? C331 C332 H33C 109.5 . . ? H33A C332 H33C 109.5 . . ? H33B C332 H33C 109.5 . . ? C331 C333 H33D 109.5 . . ? C331 C333 H33E 109.5 . . ? H33D C333 H33E 109.5 . . ? C331 C333 H33F 109.5 . . ? H33D C333 H33F 109.5 . . ? H33E C333 H33F 109.5 . . ? C331 C334 H33G 109.5 . . ? C331 C334 H33H 109.5 . . ? H33G C334 H33H 109.5 . . ? C331 C334 H33I 109.5 . . ? H33G C334 H33I 109.5 . . ? H33H C334 H33I 109.5 . . ? C364 C361 C363 108.4(2) . . ? C364 C361 C36 112.2(2) . . ? C363 C361 C36 110.05(19) . . ? C364 C361 C362 107.7(2) . . ? C363 C361 C362 109.2(2) . . ? C36 C361 C362 109.19(19) . . ? C361 C362 H36A 109.5 . . ? C361 C362 H36B 109.5 . . ? H36A C362 H36B 109.5 . . ? C361 C362 H36C 109.5 . . ? H36A C362 H36C 109.5 . . ? H36B C362 H36C 109.5 . . ? C361 C363 H36D 109.5 . . ? C361 C363 H36E 109.5 . . ? H36D C363 H36E 109.5 . . ? C361 C363 H36F 109.5 . . ? H36D C363 H36F 109.5 . . ? H36E C363 H36F 109.5 . . ? C361 C364 H36G 109.5 . . ? C361 C364 H36H 109.5 . . ? H36G C364 H36H 109.5 . . ? C361 C364 H36I 109.5 . . ? H36G C364 H36I 109.5 . . ? H36H C364 H36I 109.5 . . ? Cl53 C51 Cl52 114.1(2) . . ? Cl53 C51 H51A 108.7 . . ? Cl52 C51 H51A 108.7 . . ? Cl53 C51 H51B 108.7 . . ? Cl52 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? Cl63 C61 Cl62 111.3(2) . . ? Cl63 C61 H61A 109.4 . . ? Cl62 C61 H61A 109.4 . . ? Cl63 C61 H61B 109.4 . . ? Cl62 C61 H61B 109.4 . . ? H61A C61 H61B 108.0 . . ? 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 C9 C1 C2 O2 165.12(18) . . . . ? C11 C1 C2 O2 -13.6(3) . . . . ? C9 C1 C2 C3 -15.5(3) . . . . ? C11 C1 C2 C3 165.80(18) . . . . ? C1 C2 O2 Zn -46.2(2) . . . . ? C3 C2 O2 Zn 134.41(15) . . . . ? O32 Zn O2 C2 -179.22(11) . . . . ? N12 Zn O2 C2 58.99(13) . . . . ? N42 Zn O2 C2 -66.31(13) . . . . ? O2 C2 C3 C4 -166.38(18) . . . . ? C1 C2 C3 C4 14.2(3) . . . . ? O2 C2 C3 C301 13.1(3) . . . . ? C1 C2 C3 C301 -166.34(18) . . . . ? C2 C3 C4 C10 -2.7(3) . . . . ? C301 C3 C4 C10 177.87(18) . . . . ? C10 C5 C6 C7 0.1(3) . . . . ? C10 C5 C6 C601 179.64(19) . . . . ? C5 C6 C7 C8 0.3(3) . . . . ? C601 C6 C7 C8 -179.2(2) . . . . ? C6 C7 C8 C9 0.4(3) . . . . ? C7 C8 C9 C10 -1.5(3) . . . . ? C7 C8 C9 C1 175.2(2) . . . . ? C2 C1 C9 C10 5.2(3) . . . . ? C11 C1 C9 C10 -176.16(18) . . . . ? C2 C1 C9 C8 -171.47(19) . . . . ? C11 C1 C9 C8 7.2(3) . . . . ? C8 C9 C10 C5 1.9(3) . . . . ? C1 C9 C10 C5 -174.99(19) . . . . ? C8 C9 C10 C4 -176.91(19) . . . . ? C1 C9 C10 C4 6.2(3) . . . . ? C6 C5 C10 C9 -1.3(3) . . . . ? C6 C5 C10 C4 177.51(19) . . . . ? C3 C4 C10 C9 -7.5(3) . . . . ? C3 C4 C10 C5 173.7(2) . . . . ? C2 C1 C11 N12 54.3(3) . . . . ? C9 C1 C11 N12 -124.4(2) . . . . ? C2 C1 C11 C19 -121.5(2) . . . . ? C9 C1 C11 C19 59.8(3) . . . . ? C19 C11 N12 C13 -5.0(3) . . . . ? C1 C11 N12 C13 179.13(19) . . . . ? C19 C11 N12 Zn 153.47(16) . . . . ? C1 C11 N12 Zn -22.4(2) . . . . ? O32 Zn N12 C11 -153.85(14) . . . . ? O2 Zn N12 C11 -25.79(15) . . . . ? N42 Zn N12 C11 96.16(15) . . . . ? O32 Zn N12 C13 4.72(18) . . . . ? O2 Zn N12 C13 132.79(16) . . . . ? N42 Zn N12 C13 -105.26(16) . . . . ? C11 N12 C13 C14 2.3(3) . . . . ? Zn N12 C13 C14 -155.18(18) . . . . ? N12 C13 C14 C20 2.2(3) . . . . ? C20 C15 C16 C17 -0.4(4) . . . . ? C15 C16 C17 C18 0.1(4) . . . . ? C16 C17 C18 C19 0.4(4) . . . . ? C17 C18 C19 C20 -0.5(3) . . . . ? C17 C18 C19 C11 175.4(2) . . . . ? N12 C11 C19 C18 -172.7(2) . . . . ? C1 C11 C19 C18 3.1(3) . . . . ? N12 C11 C19 C20 3.2(3) . . . . ? C1 C11 C19 C20 178.92(19) . . . . ? C13 C14 C20 C19 -3.8(3) . . . . ? C13 C14 C20 C15 173.1(2) . . . . ? C18 C19 C20 C14 177.2(2) . . . . ? C11 C19 C20 C14 1.2(3) . . . . ? C18 C19 C20 C15 0.1(3) . . . . ? C11 C19 C20 C15 -175.9(2) . . . . ? C16 C15 C20 C14 -176.7(2) . . . . ? C16 C15 C20 C19 0.3(3) . . . . ? C4 C3 C301 C302 -10.7(3) . . . . ? C2 C3 C301 C302 169.85(18) . . . . ? C4 C3 C301 C303 -128.5(2) . . . . ? C2 C3 C301 C303 52.1(2) . . . . ? C4 C3 C301 C304 110.3(2) . . . . ? C2 C3 C301 C304 -69.1(2) . . . . ? C5 C6 C601 C604 176.36(19) . . . . ? C7 C6 C601 C604 -4.2(3) . . . . ? C5 C6 C601 C602 -63.0(3) . . . . ? C7 C6 C601 C602 116.4(2) . . . . ? C5 C6 C601 C603 56.1(3) . . . . ? C7 C6 C601 C603 -124.4(2) . . . . ? C39 C31 C32 O32 167.76(18) . . . . ? C41 C31 C32 O32 -11.7(3) . . . . ? C39 C31 C32 C33 -13.1(3) . . . . ? C41 C31 C32 C33 167.36(18) . . . . ? C31 C32 O32 Zn -46.6(2) . . . . ? C33 C32 O32 Zn 134.31(15) . . . . ? O2 Zn O32 C32 -178.78(11) . . . . ? N12 Zn O32 C32 -68.01(14) . . . . ? N42 Zn O32 C32 57.38(13) . . . . ? O32 C32 C33 C34 -169.16(18) . . . . ? C31 C32 C33 C34 11.7(3) . . . . ? O32 C32 C33 C331 10.8(3) . . . . ? C31 C32 C33 C331 -168.32(18) . . . . ? C32 C33 C34 C40 -2.0(3) . . . . ? C331 C33 C34 C40 178.04(18) . . . . ? C40 C35 C36 C37 1.0(3) . . . . ? C40 C35 C36 C361 -179.1(2) . . . . ? C35 C36 C37 C38 0.2(3) . . . . ? C361 C36 C37 C38 -179.7(2) . . . . ? C36 C37 C38 C39 -1.4(3) . . . . ? C37 C38 C39 C40 1.3(3) . . . . ? C37 C38 C39 C31 177.9(2) . . . . ? C32 C31 C39 C40 4.7(3) . . . . ? C41 C31 C39 C40 -175.78(18) . . . . ? C32 C31 C39 C38 -171.75(19) . . . . ? C41 C31 C39 C38 7.7(3) . . . . ? C36 C35 C40 C39 -1.0(3) . . . . ? C36 C35 C40 C34 177.10(19) . . . . ? C38 C39 C40 C35 -0.2(3) . . . . ? C31 C39 C40 C35 -176.91(19) . . . . ? C38 C39 C40 C34 -178.34(18) . . . . ? C31 C39 C40 C34 4.9(3) . . . . ? C33 C34 C40 C35 175.5(2) . . . . ? C33 C34 C40 C39 -6.4(3) . . . . ? C32 C31 C41 N42 54.2(3) . . . . ? C39 C31 C41 N42 -125.3(2) . . . . ? C32 C31 C41 C49 -122.6(2) . . . . ? C39 C31 C41 C49 57.9(3) . . . . ? C49 C41 N42 C43 -6.6(3) . . . . ? C31 C41 N42 C43 176.59(19) . . . . ? C49 C41 N42 Zn 151.90(16) . . . . ? C31 C41 N42 Zn -24.9(2) . . . . ? O32 Zn N42 C41 -22.64(15) . . . . ? O2 Zn N42 C41 -151.74(14) . . . . ? N12 Zn N42 C41 98.60(15) . . . . ? O32 Zn N42 C43 135.76(17) . . . . ? O2 Zn N42 C43 6.67(19) . . . . ? N12 Zn N42 C43 -103.00(17) . . . . ? C41 N42 C43 C44 1.7(3) . . . . ? Zn N42 C43 C44 -155.50(18) . . . . ? N42 C43 C44 C50 3.6(4) . . . . ? C50 C45 C46 C47 -0.7(4) . . . . ? C45 C46 C47 C48 -0.2(4) . . . . ? C46 C47 C48 C49 0.5(4) . . . . ? C47 C48 C49 C50 0.0(3) . . . . ? C47 C48 C49 C41 176.9(2) . . . . ? N42 C41 C49 C48 -170.6(2) . . . . ? C31 C41 C49 C48 6.1(3) . . . . ? N42 C41 C49 C50 6.2(3) . . . . ? C31 C41 C49 C50 -177.07(19) . . . . ? C43 C44 C50 C49 -3.7(3) . . . . ? C43 C44 C50 C45 173.0(2) . . . . ? C48 C49 C50 C44 176.0(2) . . . . ? C41 C49 C50 C44 -1.0(3) . . . . ? C48 C49 C50 C45 -0.8(3) . . . . ? C41 C49 C50 C45 -177.8(2) . . . . ? C46 C45 C50 C44 -175.5(2) . . . . ? C46 C45 C50 C49 1.2(3) . . . . ? C34 C33 C331 C332 -126.2(2) . . . . ? C32 C33 C331 C332 53.9(2) . . . . ? C34 C33 C331 C334 -8.3(3) . . . . ? C32 C33 C331 C334 171.79(18) . . . . ? C34 C33 C331 C333 112.4(2) . . . . ? C32 C33 C331 C333 -67.6(2) . . . . ? C35 C36 C361 C364 0.3(3) . . . . ? C37 C36 C361 C364 -179.7(2) . . . . ? C35 C36 C361 C363 -120.5(3) . . . . ? C37 C36 C361 C363 59.5(3) . . . . ? C35 C36 C361 C362 119.6(2) . . . . ? C37 C36 C361 C362 -60.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.063 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.066 #===END data_14 _database_code_depnum_ccdc_archive 'CCDC 728919' _chemical_formula_structural '[{Mg{L(H)}2}2].C6H14' _chemical_formula_moiety 'C108 H112 Mg2 N4 O4, 2(C6 H14)' _chemical_formula_sum 'C120 H140 Mg2 N4 O4' _chemical_formula_weight 1750.98 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' Mg Mg 0.0486 0.0363 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.690(2) _cell_length_b 17.4249(15) _cell_length_c 22.9030(18) _cell_angle_alpha 90.00 _cell_angle_beta 109.804(7) _cell_angle_gamma 90.00 _cell_volume 11148.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 11123 _cell_measurement_theta_min 3.5343 _cell_measurement_theta_max 27.4999 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.043 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3776 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details '(ABSPACK; Oxford Diffraction, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64046 _diffrn_reflns_av_R_equivalents 0.0909 _diffrn_reflns_av_sigmaI/netI 0.1383 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.71 _reflns_number_total 12817 _reflns_number_gt 5533 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ; SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004) ; _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^ > 2\s(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^)+(0.0848P)^2^] 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_number_reflns 12817 _refine_ls_number_parameters 600 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1505 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1605 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 0.835 _refine_ls_restrained_S_all 0.843 _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 Mg1 Mg 0.44417(3) 0.18526(4) 0.23744(3) 0.0267(2) Uani 1 1 d . . . N1 N 0.43663(7) 0.07548(11) 0.19149(8) 0.0280(5) Uani 1 1 d . . . O1 O 0.49326(5) 0.20366(9) 0.19231(7) 0.0263(4) Uani 1 1 d . . . C1 C 0.44769(8) 0.13611(13) 0.10263(10) 0.0250(5) Uani 1 1 d . . . C2 C 0.47262(8) 0.20201(14) 0.13036(10) 0.0260(5) Uani 1 1 d . . . C3 C 0.47579(8) 0.26633(14) 0.09297(11) 0.0282(6) Uani 1 1 d . . . C4 C 0.45346(8) 0.25967(14) 0.03027(11) 0.0298(6) Uani 1 1 d . . . H4 H 0.4573 0.3003 0.0047 0.036 Uiso 1 1 calc R . . C5 C 0.42514(8) 0.19647(14) 0.00112(10) 0.0277(5) Uani 1 1 d . . . C6 C 0.39950(8) 0.19613(14) -0.06403(10) 0.0291(6) Uani 1 1 d . . . H6 H 0.4023 0.2391 -0.0881 0.035 Uiso 1 1 calc R . . C7 C 0.37116(8) 0.13649(14) -0.09292(11) 0.0314(6) Uani 1 1 d . . . C8 C 0.36652(9) 0.07537(14) -0.05564(11) 0.0333(6) Uani 1 1 d . . . H8 H 0.3461 0.0337 -0.0744 0.040 Uiso 1 1 calc R . . C9 C 0.39035(8) 0.07374(14) 0.00684(11) 0.0308(6) Uani 1 1 d . . . H9 H 0.3861 0.0311 0.0303 0.037 Uiso 1 1 calc R . . C10 C 0.42133(8) 0.13412(13) 0.03754(10) 0.0250(5) Uani 1 1 d . . . C11 C 0.44837(8) 0.06671(14) 0.14066(10) 0.0264(5) Uani 1 1 d . . . C12 C 0.43229(9) 0.01139(15) 0.22346(11) 0.0337(6) Uani 1 1 d . . . H12 H 0.4225 0.0180 0.2585 0.040 Uiso 1 1 calc R . . C13 C 0.44092(9) -0.06012(15) 0.20873(11) 0.0369(6) Uani 1 1 d . . . H13 H 0.4353 -0.1028 0.2312 0.044 Uiso 1 1 calc R . . C14 C 0.45845(9) -0.07099(14) 0.15952(11) 0.0332(6) Uani 1 1 d . . . C15 C 0.47358(10) -0.14362(15) 0.14548(12) 0.0420(7) Uani 1 1 d . . . H15 H 0.4693 -0.1878 0.1673 0.050 Uiso 1 1 calc R . . C16 C 0.49406(10) -0.15075(16) 0.10149(12) 0.0424(7) Uani 1 1 d . . . H16 H 0.5043 -0.1997 0.0927 0.051 Uiso 1 1 calc R . . C17 C 0.50022(9) -0.08600(15) 0.06877(11) 0.0361(6) Uani 1 1 d . . . H17 H 0.5159 -0.0911 0.0390 0.043 Uiso 1 1 calc R . . C18 C 0.48417(8) -0.01630(15) 0.07896(10) 0.0303(6) Uani 1 1 d . . . H18 H 0.4872 0.0264 0.0547 0.036 Uiso 1 1 calc R . . C19 C 0.46298(8) -0.00607(14) 0.12520(10) 0.0278(5) Uani 1 1 d . . . C30 C 0.50123(9) 0.34151(14) 0.12082(11) 0.0330(6) Uani 1 1 d . . . C31 C 0.55460(9) 0.32865(16) 0.15717(14) 0.0498(8) Uani 1 1 d . . . H31A H 0.5696 0.3028 0.1305 0.075 Uiso 1 1 calc R . . H31B H 0.5580 0.2967 0.1936 0.075 Uiso 1 1 calc R . . H31C H 0.5702 0.3783 0.1706 0.075 Uiso 1 1 calc R . . C32 C 0.47675(11) 0.37708(17) 0.16354(15) 0.0573(9) Uani 1 1 d . . . H32A H 0.4940 0.4235 0.1829 0.086 Uiso 1 1 calc R . . H32B H 0.4769 0.3401 0.1958 0.086 Uiso 1 1 calc R . . H32C H 0.4436 0.3904 0.1392 0.086 Uiso 1 1 calc R . . C33 C 0.49869(12) 0.40054(16) 0.07113(13) 0.0577(9) Uani 1 1 d . . . H33A H 0.4651 0.4121 0.0477 0.087 Uiso 1 1 calc R . . H33B H 0.5142 0.3801 0.0429 0.087 Uiso 1 1 calc R . . H33C H 0.5151 0.4475 0.0907 0.087 Uiso 1 1 calc R . . C70 C 0.34606(9) 0.13210(15) -0.16385(11) 0.0371(6) Uani 1 1 d . . . C71 C 0.29195(9) 0.11841(18) -0.18024(12) 0.0494(8) Uani 1 1 d . . . H71A H 0.2775 0.1624 -0.1665 0.074 Uiso 1 1 calc R . . H71B H 0.2867 0.0718 -0.1594 0.074 Uiso 1 1 calc R . . H71C H 0.2771 0.1123 -0.2252 0.074 Uiso 1 1 calc R . . C72 C 0.35310(12) 0.20516(18) -0.19614(12) 0.0589(9) Uani 1 1 d . . . H72A H 0.3873 0.2125 -0.1890 0.088 Uiso 1 1 calc R . . H72B H 0.3408 0.2491 -0.1794 0.088 Uiso 1 1 calc R . . H72C H 0.3357 0.2009 -0.2408 0.088 Uiso 1 1 calc R . . C73 C 0.36803(10) 0.06489(17) -0.18717(12) 0.0462(7) Uani 1 1 d . . . H73A H 0.3536 0.0613 -0.2324 0.069 Uiso 1 1 calc R . . H73B H 0.3620 0.0172 -0.1683 0.069 Uiso 1 1 calc R . . H73C H 0.4026 0.0728 -0.1758 0.069 Uiso 1 1 calc R . . N11 N 0.40546(7) 0.14545(11) 0.30023(9) 0.0294(5) Uani 1 1 d . . . O11 O 0.38999(5) 0.25148(9) 0.19808(7) 0.0306(4) Uani 1 1 d . . . C101 C 0.33009(8) 0.18726(14) 0.22547(11) 0.0295(6) Uani 1 1 d . . . C102 C 0.34473(8) 0.23268(14) 0.18565(11) 0.0290(6) Uani 1 1 d . . . C103 C 0.30779(8) 0.26315(14) 0.13061(11) 0.0289(6) Uani 1 1 d . . . C104 C 0.26314(8) 0.23116(14) 0.11387(11) 0.0323(6) Uani 1 1 d . . . H104 H 0.2394 0.2496 0.0773 0.039 Uiso 1 1 calc R . . C105 C 0.25025(8) 0.17256(14) 0.14756(11) 0.0321(6) Uani 1 1 d . . . C106 C 0.20537(9) 0.13503(15) 0.12539(12) 0.0393(7) Uani 1 1 d . . . H106 H 0.1832 0.1498 0.0862 0.047 Uiso 1 1 calc R . . C107 C 0.19257(9) 0.07855(15) 0.15784(13) 0.0413(7) Uani 1 1 d . . . C108 C 0.22619(9) 0.05988(16) 0.21657(13) 0.0435(7) Uani 1 1 d . . . H108 H 0.2182 0.0213 0.2408 0.052 Uiso 1 1 calc R . . C109 C 0.26978(9) 0.09539(15) 0.23976(12) 0.0408(7) Uani 1 1 d . . . H109 H 0.2911 0.0812 0.2796 0.049 Uiso 1 1 calc R . . C110 C 0.28367(9) 0.15253(15) 0.20580(11) 0.0339(6) Uani 1 1 d . . . C111 C 0.36179(8) 0.17457(14) 0.28978(11) 0.0296(6) Uani 1 1 d . . . C112 C 0.43165(9) 0.12491(15) 0.35931(11) 0.0366(6) Uani 1 1 d . . . H112 H 0.4618 0.1014 0.3660 0.044 Uiso 1 1 calc R . . C113 C 0.41797(10) 0.13548(17) 0.40890(12) 0.0462(7) Uani 1 1 d . . . H113 H 0.4366 0.1157 0.4484 0.055 Uiso 1 1 calc R . . C114 C 0.37522(10) 0.17671(18) 0.40123(12) 0.0470(7) Uani 1 1 d . . . C115 C 0.36171(13) 0.2005(2) 0.45195(15) 0.0701(10) Uani 1 1 d . . . H115 H 0.3804 0.1861 0.4930 0.084 Uiso 1 1 calc R . . C116 C 0.32152(15) 0.2442(2) 0.44154(18) 0.0801(11) Uani 1 1 d . . . H116 H 0.3128 0.2613 0.4756 0.096 Uiso 1 1 calc R . . C117 C 0.29335(13) 0.2636(2) 0.38134(17) 0.0686(10) Uani 1 1 d . . . H117 H 0.2654 0.2938 0.3749 0.082 Uiso 1 1 calc R . . C118 C 0.30477(10) 0.24068(17) 0.33185(14) 0.0497(8) Uani 1 1 d . . . H118 H 0.2848 0.2543 0.2911 0.060 Uiso 1 1 calc R . . C119 C 0.34648(9) 0.19622(16) 0.34047(12) 0.0383(6) Uani 1 1 d . . . C130 C 0.31894(9) 0.32930(14) 0.09479(11) 0.0338(6) Uani 1 1 d . . . C131 C 0.34126(10) 0.39508(16) 0.13943(13) 0.0460(7) Uani 1 1 d . . . H13A H 0.3191 0.4113 0.1605 0.069 Uiso 1 1 calc R . . H13B H 0.3477 0.4384 0.1161 0.069 Uiso 1 1 calc R . . H13C H 0.3713 0.3777 0.1703 0.069 Uiso 1 1 calc R . . C132 C 0.35316(9) 0.30193(17) 0.06209(12) 0.0428(7) Uani 1 1 d . . . H13D H 0.3821 0.2807 0.0928 0.064 Uiso 1 1 calc R . . H13E H 0.3619 0.3453 0.0408 0.064 Uiso 1 1 calc R . . H13F H 0.3375 0.2622 0.0317 0.064 Uiso 1 1 calc R . . C133 C 0.27387(9) 0.36123(16) 0.04552(12) 0.0420(7) Uani 1 1 d . . . H13G H 0.2586 0.3207 0.0158 0.063 Uiso 1 1 calc R . . H13H H 0.2827 0.4039 0.0237 0.063 Uiso 1 1 calc R . . H13I H 0.2515 0.3795 0.0656 0.063 Uiso 1 1 calc R . . C170 C 0.14519(10) 0.03499(17) 0.13427(14) 0.0504(8) Uani 1 1 d . . . C171 C 0.15601(12) -0.05078(18) 0.13185(17) 0.0684(10) Uani 1 1 d . . . H17A H 0.1259 -0.0792 0.1146 0.103 Uiso 1 1 calc R . . H17B H 0.1734 -0.0694 0.1739 0.103 Uiso 1 1 calc R . . H17C H 0.1757 -0.0586 0.1055 0.103 Uiso 1 1 calc R . . C172 C 0.11810(12) 0.0473(2) 0.17990(18) 0.0762(11) Uani 1 1 d . . . H17D H 0.1123 0.1022 0.1831 0.114 Uiso 1 1 calc R . . H17E H 0.1373 0.0273 0.2208 0.114 Uiso 1 1 calc R . . H17F H 0.0874 0.0201 0.1649 0.114 Uiso 1 1 calc R . . C173 C 0.11407(12) 0.0609(2) 0.07106(17) 0.0842(13) Uani 1 1 d . . . H17G H 0.1071 0.1158 0.0723 0.126 Uiso 1 1 calc R . . H17H H 0.0840 0.0319 0.0583 0.126 Uiso 1 1 calc R . . H17I H 0.1307 0.0521 0.0413 0.126 Uiso 1 1 calc R . . C201 C 0.2437(2) 0.0794(3) 0.3917(3) 0.148(2) Uani 1 1 d U . . H20A H 0.2724 0.1048 0.3889 0.222 Uiso 1 1 calc R . . H20B H 0.2151 0.1025 0.3617 0.222 Uiso 1 1 calc R . . H20C H 0.2449 0.0246 0.3825 0.222 Uiso 1 1 calc R . . C202 C 0.2421(2) 0.0886(3) 0.4541(3) 0.1350(19) Uani 1 1 d U . . H20D H 0.2117 0.0660 0.4548 0.162 Uiso 1 1 calc R . . H20E H 0.2409 0.1442 0.4623 0.162 Uiso 1 1 calc R . . C203 C 0.28138(17) 0.0549(3) 0.5058(2) 0.1066(15) Uani 1 1 d U . . H20F H 0.2841 0.0004 0.4953 0.128 Uiso 1 1 calc R . . H20G H 0.3113 0.0805 0.5065 0.128 Uiso 1 1 calc R . . C204 C 0.2803(3) 0.0568(5) 0.5686(3) 0.187(3) Uani 1 1 d U . . H204 H 0.2471 0.0578 0.5705 0.224 Uiso 1 1 calc R . . C205 C 0.3146(5) 0.1267(7) 0.6082(5) 0.349(7) Uani 1 1 d U . . H20H H 0.3137 0.1275 0.6505 0.524 Uiso 1 1 calc R . . H20I H 0.3030 0.1759 0.5879 0.524 Uiso 1 1 calc R . . H20J H 0.3476 0.1183 0.6096 0.524 Uiso 1 1 calc R . . C206 C 0.31223(19) -0.0013(4) 0.6114(3) 0.158(2) Uani 1 1 d U . . H20K H 0.3046 -0.0526 0.5931 0.237 Uiso 1 1 calc R . . H20L H 0.3072 -0.0001 0.6515 0.237 Uiso 1 1 calc R . . H20M H 0.3457 0.0108 0.6174 0.237 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 Mg1 0.0226(4) 0.0360(5) 0.0203(4) 0.0013(4) 0.0056(3) 0.0000(4) N1 0.0263(11) 0.0377(12) 0.0205(11) 0.0005(9) 0.0088(9) -0.0038(9) O1 0.0230(8) 0.0353(9) 0.0190(9) 0.0014(7) 0.0049(7) -0.0021(7) C1 0.0232(12) 0.0331(14) 0.0196(12) 0.0020(10) 0.0083(10) 0.0008(10) C2 0.0211(12) 0.0370(14) 0.0203(13) 0.0006(11) 0.0075(10) -0.0005(10) C3 0.0222(12) 0.0352(14) 0.0270(14) 0.0043(11) 0.0081(11) -0.0004(11) C4 0.0308(13) 0.0336(14) 0.0275(14) 0.0054(11) 0.0131(11) 0.0001(11) C5 0.0266(13) 0.0358(15) 0.0222(13) 0.0009(11) 0.0103(10) 0.0050(11) C6 0.0333(14) 0.0346(14) 0.0213(13) 0.0048(11) 0.0116(11) 0.0056(11) C7 0.0299(14) 0.0418(16) 0.0223(13) -0.0040(12) 0.0085(11) 0.0071(12) C8 0.0331(14) 0.0391(15) 0.0266(14) -0.0030(12) 0.0087(12) -0.0024(12) C9 0.0298(14) 0.0369(15) 0.0246(14) 0.0009(11) 0.0078(11) -0.0023(11) C10 0.0206(12) 0.0354(14) 0.0194(12) -0.0001(10) 0.0072(10) 0.0045(10) C11 0.0217(12) 0.0366(15) 0.0176(12) -0.0025(10) 0.0024(10) -0.0047(10) C12 0.0354(15) 0.0422(17) 0.0268(14) 0.0017(12) 0.0148(12) -0.0048(12) C13 0.0468(16) 0.0351(16) 0.0315(15) 0.0050(12) 0.0168(13) -0.0050(13) C14 0.0335(14) 0.0364(15) 0.0278(14) -0.0007(11) 0.0081(12) -0.0059(12) C15 0.0546(18) 0.0339(16) 0.0410(16) 0.0024(13) 0.0209(14) -0.0014(13) C16 0.0482(17) 0.0394(16) 0.0413(17) -0.0045(13) 0.0173(14) 0.0071(13) C17 0.0357(15) 0.0462(17) 0.0256(14) -0.0018(12) 0.0092(12) 0.0004(12) C18 0.0299(14) 0.0387(15) 0.0216(13) 0.0018(11) 0.0076(11) -0.0011(11) C19 0.0262(13) 0.0351(14) 0.0207(13) 0.0005(11) 0.0060(10) -0.0004(11) C30 0.0309(14) 0.0344(15) 0.0295(14) 0.0035(11) 0.0047(11) -0.0069(11) C31 0.0367(16) 0.0469(18) 0.0567(19) 0.0036(14) 0.0040(14) -0.0140(13) C32 0.060(2) 0.0457(19) 0.070(2) -0.0162(16) 0.0268(18) -0.0183(15) C33 0.070(2) 0.0428(18) 0.0451(19) 0.0111(14) -0.0005(16) -0.0209(16) C70 0.0395(15) 0.0484(17) 0.0207(13) -0.0028(12) 0.0066(12) 0.0053(13) C71 0.0395(17) 0.073(2) 0.0287(15) -0.0076(14) 0.0021(13) 0.0119(15) C72 0.085(2) 0.065(2) 0.0193(15) 0.0026(14) 0.0079(15) -0.0015(18) C73 0.0413(17) 0.067(2) 0.0289(15) -0.0116(14) 0.0098(13) 0.0046(14) N11 0.0240(11) 0.0390(12) 0.0239(11) 0.0039(9) 0.0062(9) -0.0001(9) O11 0.0204(9) 0.0389(10) 0.0306(9) 0.0022(8) 0.0061(7) -0.0002(7) C101 0.0226(12) 0.0346(14) 0.0289(14) 0.0043(11) 0.0058(11) 0.0023(11) C102 0.0238(13) 0.0354(14) 0.0261(13) -0.0016(11) 0.0063(11) 0.0025(11) C103 0.0261(13) 0.0327(14) 0.0273(13) 0.0011(11) 0.0084(11) 0.0027(11) C104 0.0276(13) 0.0366(15) 0.0273(14) 0.0041(11) 0.0024(11) 0.0049(11) C105 0.0239(13) 0.0356(15) 0.0334(14) 0.0037(11) 0.0053(11) 0.0011(11) C106 0.0310(15) 0.0417(16) 0.0375(16) 0.0045(13) 0.0013(12) 0.0016(12) C107 0.0317(15) 0.0408(16) 0.0486(18) 0.0050(13) 0.0098(13) -0.0030(12) C108 0.0317(15) 0.0483(18) 0.0462(17) 0.0159(14) 0.0077(13) -0.0013(13) C109 0.0293(15) 0.0486(17) 0.0394(16) 0.0150(13) 0.0053(12) 0.0019(13) C110 0.0280(14) 0.0424(16) 0.0307(14) 0.0068(12) 0.0095(12) 0.0035(12) C111 0.0255(13) 0.0364(14) 0.0275(13) 0.0018(11) 0.0098(11) -0.0034(11) C112 0.0248(13) 0.0528(18) 0.0297(15) 0.0111(12) 0.0059(11) 0.0003(12) C113 0.0361(16) 0.074(2) 0.0253(15) 0.0112(14) 0.0058(12) -0.0037(15) C114 0.0411(17) 0.070(2) 0.0326(16) -0.0016(14) 0.0165(13) -0.0045(15) C115 0.073(2) 0.108(3) 0.0366(18) -0.0111(18) 0.0279(18) -0.012(2) C116 0.088(3) 0.109(3) 0.062(3) -0.020(2) 0.050(2) 0.000(2) C117 0.067(2) 0.080(3) 0.073(3) -0.007(2) 0.043(2) 0.0101(19) C118 0.0439(17) 0.061(2) 0.0509(18) -0.0048(15) 0.0245(15) 0.0046(15) C119 0.0325(15) 0.0509(17) 0.0338(15) -0.0005(13) 0.0144(12) -0.0024(13) C130 0.0279(13) 0.0382(15) 0.0347(15) 0.0080(12) 0.0096(12) 0.0023(11) C131 0.0410(16) 0.0409(16) 0.0535(18) 0.0058(14) 0.0125(14) -0.0005(13) C132 0.0341(15) 0.0575(19) 0.0372(16) 0.0133(13) 0.0126(13) 0.0047(13) C133 0.0382(15) 0.0450(17) 0.0436(16) 0.0159(13) 0.0149(13) 0.0062(13) C170 0.0444(18) 0.0444(18) 0.058(2) 0.0073(15) 0.0116(16) -0.0063(14) C171 0.055(2) 0.059(2) 0.089(3) -0.0004(19) 0.021(2) -0.0116(17) C172 0.0419(19) 0.079(3) 0.110(3) -0.012(2) 0.028(2) -0.0180(18) C173 0.051(2) 0.076(3) 0.095(3) 0.029(2) -0.015(2) -0.0276(19) C201 0.202(6) 0.140(5) 0.110(4) -0.012(4) 0.063(4) -0.037(4) C202 0.132(5) 0.135(5) 0.142(4) 0.016(4) 0.051(4) 0.013(4) C203 0.095(3) 0.096(3) 0.116(3) 0.011(3) 0.021(3) -0.020(3) C204 0.261(9) 0.213(7) 0.113(4) -0.018(4) 0.097(5) 0.049(6) C205 0.382(15) 0.275(8) 0.315(12) -0.125(9) 0.018(11) 0.109(9) C206 0.098(4) 0.240(6) 0.125(5) 0.067(5) 0.023(3) -0.023(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Mg1 O11 1.9362(17) . ? Mg1 O1 2.0291(16) 2_655 ? Mg1 O1 2.0776(17) . ? Mg1 N1 2.158(2) . ? Mg1 N11 2.234(2) . ? Mg1 C2 2.867(2) . ? Mg1 Mg1 3.1668(15) 2_655 ? N1 C11 1.332(3) . ? N1 C12 1.365(3) . ? O1 C2 1.342(3) . ? O1 Mg1 2.0290(16) 2_655 ? C1 C2 1.397(3) . ? C1 C10 1.430(3) . ? C1 C11 1.487(3) . ? C2 C3 1.433(3) . ? C3 C4 1.368(3) . ? C3 C30 1.539(3) . ? C4 C5 1.409(3) . ? C4 H4 0.9500 . ? C5 C10 1.397(3) . ? C5 C6 1.427(3) . ? C6 C7 1.360(3) . ? C6 H6 0.9500 . ? C7 C8 1.401(3) . ? C7 C70 1.543(3) . ? C8 C9 1.365(3) . ? C8 H8 0.9500 . ? C9 C10 1.417(3) . ? C9 H9 0.9500 . ? C11 C19 1.423(3) . ? C12 C13 1.338(3) . ? C12 H12 0.9500 . ? C13 C14 1.405(3) . ? C13 H13 0.9500 . ? C14 C19 1.410(3) . ? C14 C15 1.416(4) . ? C15 C16 1.347(4) . ? C15 H15 0.9500 . ? C16 C17 1.400(4) . ? C16 H16 0.9500 . ? C17 C18 1.353(3) . ? C17 H17 0.9500 . ? C18 C19 1.415(3) . ? C18 H18 0.9500 . ? C30 C33 1.517(4) . ? C30 C32 1.533(4) . ? C30 C31 1.536(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C70 C72 1.522(4) . ? C70 C73 1.523(4) . ? C70 C71 1.540(4) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? N11 C111 1.336(3) . ? N11 C112 1.360(3) . ? O11 C102 1.317(3) . ? C101 C102 1.384(3) . ? C101 C110 1.431(3) . ? C101 C111 1.471(3) . ? C102 C103 1.462(3) . ? C103 C104 1.368(3) . ? C103 C130 1.515(3) . ? C104 C105 1.409(3) . ? C104 H104 0.9500 . ? C105 C110 1.410(3) . ? C105 C106 1.415(3) . ? C106 C107 1.363(4) . ? C106 H106 0.9500 . ? C107 C108 1.415(4) . ? C107 C170 1.527(4) . ? C108 C109 1.369(3) . ? C108 H108 0.9500 . ? C109 C110 1.409(3) . ? C109 H109 0.9500 . ? C111 C119 1.433(3) . ? C112 C113 1.342(4) . ? C112 H112 0.9500 . ? C113 C114 1.416(4) . ? C113 H113 0.9500 . ? C114 C119 1.406(4) . ? C114 C115 1.413(4) . ? C115 C116 1.366(5) . ? C115 H115 0.9500 . ? C116 C117 1.391(5) . ? C116 H116 0.9500 . ? C117 C118 1.349(4) . ? C117 H117 0.9500 . ? C118 C119 1.417(4) . ? C118 H118 0.9500 . ? C130 C132 1.529(3) . ? C130 C131 1.529(4) . ? C130 C133 1.533(3) . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C132 H13D 0.9800 . ? C132 H13E 0.9800 . ? C132 H13F 0.9800 . ? C133 H13G 0.9800 . ? C133 H13H 0.9800 . ? C133 H13I 0.9800 . ? C170 C173 1.499(4) . ? C170 C171 1.533(4) . ? C170 C172 1.534(4) . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C173 H17G 0.9800 . ? C173 H17H 0.9800 . ? C173 H17I 0.9800 . ? C201 C202 1.455(6) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C202 C203 1.474(6) . ? C202 H20D 0.9900 . ? C202 H20E 0.9900 . ? C203 C204 1.450(7) . ? C203 H20F 0.9900 . ? C203 H20G 0.9900 . ? C204 C206 1.501(8) . ? C204 C205 1.649(12) . ? C204 H204 1.0000 . ? C205 H20H 0.9800 . ? C205 H20I 0.9800 . ? C205 H20J 0.9800 . ? C206 H20K 0.9800 . ? C206 H20L 0.9800 . ? C206 H20M 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 O11 Mg1 O1 131.91(7) . 2_655 ? O11 Mg1 O1 106.78(7) . . ? O1 Mg1 O1 76.23(7) 2_655 . ? O11 Mg1 N1 111.63(8) . . ? O1 Mg1 N1 116.27(7) 2_655 . ? O1 Mg1 N1 82.45(7) . . ? O11 Mg1 N11 87.55(7) . . ? O1 Mg1 N11 94.07(7) 2_655 . ? O1 Mg1 N11 165.67(7) . . ? N1 Mg1 N11 92.73(8) . . ? O11 Mg1 C2 88.86(7) . . ? O1 Mg1 C2 101.91(7) 2_655 . ? O1 Mg1 C2 25.70(6) . . ? N1 Mg1 C2 71.64(7) . . ? N11 Mg1 C2 161.34(7) . . ? O11 Mg1 Mg1 137.56(6) . 2_655 ? O1 Mg1 Mg1 40.11(5) 2_655 2_655 ? O1 Mg1 Mg1 38.99(4) . 2_655 ? N1 Mg1 Mg1 91.02(6) . 2_655 ? N11 Mg1 Mg1 128.19(6) . 2_655 ? C2 Mg1 Mg1 64.00(5) . 2_655 ? C11 N1 C12 118.4(2) . . ? C11 N1 Mg1 120.87(16) . . ? C12 N1 Mg1 118.47(15) . . ? C2 O1 Mg1 143.38(14) . 2_655 ? C2 O1 Mg1 112.13(13) . . ? Mg1 O1 Mg1 100.91(7) 2_655 . ? C2 C1 C10 120.8(2) . . ? C2 C1 C11 120.2(2) . . ? C10 C1 C11 119.0(2) . . ? O1 C2 C1 118.7(2) . . ? O1 C2 C3 121.1(2) . . ? C1 C2 C3 120.2(2) . . ? C1 C2 Mg1 92.34(14) . . ? C3 C2 Mg1 133.54(16) . . ? C4 C3 C2 117.0(2) . . ? C4 C3 C30 120.2(2) . . ? C2 C3 C30 122.7(2) . . ? C3 C4 C5 124.3(2) . . ? C3 C4 H4 117.9 . . ? C5 C4 H4 117.9 . . ? C10 C5 C4 118.7(2) . . ? C10 C5 C6 119.9(2) . . ? C4 C5 C6 121.3(2) . . ? C7 C6 C5 122.3(2) . . ? C7 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C6 C7 C8 117.2(2) . . ? C6 C7 C70 123.3(2) . . ? C8 C7 C70 119.5(2) . . ? C9 C8 C7 122.1(2) . . ? C9 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C8 C9 C10 121.6(2) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C5 C10 C9 116.8(2) . . ? C5 C10 C1 118.5(2) . . ? C9 C10 C1 124.7(2) . . ? N1 C11 C19 120.8(2) . . ? N1 C11 C1 117.6(2) . . ? C19 C11 C1 121.6(2) . . ? C13 C12 N1 124.5(2) . . ? C13 C12 H12 117.8 . . ? N1 C12 H12 117.8 . . ? C12 C13 C14 118.8(2) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C13 C14 C19 118.0(2) . . ? C13 C14 C15 122.3(2) . . ? C19 C14 C15 119.5(2) . . ? C16 C15 C14 120.7(3) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 120.0(3) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.9(2) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.9(2) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C14 C19 C18 117.8(2) . . ? C14 C19 C11 118.8(2) . . ? C18 C19 C11 123.3(2) . . ? C33 C30 C32 106.9(2) . . ? C33 C30 C31 106.6(2) . . ? C32 C30 C31 109.7(2) . . ? C33 C30 C3 111.9(2) . . ? C32 C30 C3 109.7(2) . . ? C31 C30 C3 111.8(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C72 C70 C73 109.1(2) . . ? C72 C70 C71 108.4(2) . . ? C73 C70 C71 109.3(2) . . ? C72 C70 C7 111.9(2) . . ? C73 C70 C7 107.2(2) . . ? C71 C70 C7 110.9(2) . . ? 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 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C111 N11 C112 118.1(2) . . ? C111 N11 Mg1 116.51(15) . . ? C112 N11 Mg1 118.46(15) . . ? C102 O11 Mg1 125.32(15) . . ? C102 C101 C110 121.2(2) . . ? C102 C101 C111 120.5(2) . . ? C110 C101 C111 118.2(2) . . ? O11 C102 C101 121.7(2) . . ? O11 C102 C103 120.6(2) . . ? C101 C102 C103 117.7(2) . . ? C104 C103 C102 117.8(2) . . ? C104 C103 C130 121.8(2) . . ? C102 C103 C130 120.4(2) . . ? C103 C104 C105 124.0(2) . . ? C103 C104 H104 118.0 . . ? C105 C104 H104 118.0 . . ? C104 C105 C110 117.6(2) . . ? C104 C105 C106 122.4(2) . . ? C110 C105 C106 120.0(2) . . ? C107 C106 C105 122.7(2) . . ? C107 C106 H106 118.6 . . ? C105 C106 H106 118.6 . . ? C106 C107 C108 116.6(2) . . ? C106 C107 C170 124.1(2) . . ? C108 C107 C170 119.4(2) . . ? C109 C108 C107 122.3(3) . . ? C109 C108 H108 118.8 . . ? C107 C108 H108 118.8 . . ? C108 C109 C110 121.4(2) . . ? C108 C109 H109 119.3 . . ? C110 C109 H109 119.3 . . ? C109 C110 C105 116.9(2) . . ? C109 C110 C101 123.8(2) . . ? C105 C110 C101 119.2(2) . . ? N11 C111 C119 120.6(2) . . ? N11 C111 C101 119.3(2) . . ? C119 C111 C101 120.0(2) . . ? C113 C112 N11 124.8(2) . . ? C113 C112 H112 117.6 . . ? N11 C112 H112 117.6 . . ? C112 C113 C114 118.7(2) . . ? C112 C113 H113 120.7 . . ? C114 C113 H113 120.7 . . ? C119 C114 C115 119.8(3) . . ? C119 C114 C113 117.6(2) . . ? C115 C114 C113 122.6(3) . . ? C116 C115 C114 119.6(3) . . ? C116 C115 H115 120.2 . . ? C114 C115 H115 120.2 . . ? C115 C116 C117 120.4(3) . . ? C115 C116 H116 119.8 . . ? C117 C116 H116 119.8 . . ? C118 C117 C116 121.5(3) . . ? C118 C117 H117 119.3 . . ? C116 C117 H117 119.3 . . ? C117 C118 C119 120.1(3) . . ? C117 C118 H118 119.9 . . ? C119 C118 H118 119.9 . . ? C114 C119 C118 118.6(3) . . ? C114 C119 C111 119.0(2) . . ? C118 C119 C111 122.2(2) . . ? C103 C130 C132 109.3(2) . . ? C103 C130 C131 109.4(2) . . ? C132 C130 C131 110.6(2) . . ? C103 C130 C133 112.2(2) . . ? C132 C130 C133 108.2(2) . . ? C131 C130 C133 107.0(2) . . ? C130 C131 H13A 109.5 . . ? C130 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C130 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C130 C132 H13D 109.5 . . ? C130 C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? C130 C132 H13F 109.5 . . ? H13D C132 H13F 109.5 . . ? H13E C132 H13F 109.5 . . ? C130 C133 H13G 109.5 . . ? C130 C133 H13H 109.5 . . ? H13G C133 H13H 109.5 . . ? C130 C133 H13I 109.5 . . ? H13G C133 H13I 109.5 . . ? H13H C133 H13I 109.5 . . ? C173 C170 C107 112.6(2) . . ? C173 C170 C171 109.1(3) . . ? C107 C170 C171 108.5(2) . . ? C173 C170 C172 108.8(3) . . ? C107 C170 C172 108.8(2) . . ? C171 C170 C172 109.0(3) . . ? C170 C171 H17A 109.5 . . ? C170 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C170 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C170 C172 H17D 109.5 . . ? C170 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C170 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C170 C173 H17G 109.5 . . ? C170 C173 H17H 109.5 . . ? H17G C173 H17H 109.5 . . ? C170 C173 H17I 109.5 . . ? H17G C173 H17I 109.5 . . ? H17H C173 H17I 109.5 . . ? C202 C201 H20A 109.5 . . ? C202 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C202 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C201 C202 C203 117.7(5) . . ? C201 C202 H20D 107.9 . . ? C203 C202 H20D 107.9 . . ? C201 C202 H20E 107.9 . . ? C203 C202 H20E 107.9 . . ? H20D C202 H20E 107.2 . . ? C204 C203 C202 120.7(6) . . ? C204 C203 H20F 107.2 . . ? C202 C203 H20F 107.2 . . ? C204 C203 H20G 107.2 . . ? C202 C203 H20G 107.2 . . ? H20F C203 H20G 106.8 . . ? C203 C204 C206 114.2(6) . . ? C203 C204 C205 110.1(8) . . ? C206 C204 C205 90.2(7) . . ? C203 C204 H204 113.4 . . ? C206 C204 H204 113.4 . . ? C205 C204 H204 113.4 . . ? C204 C205 H20H 109.5 . . ? C204 C205 H20I 109.5 . . ? H20H C205 H20I 109.5 . . ? C204 C205 H20J 109.5 . . ? H20H C205 H20J 109.5 . . ? H20I C205 H20J 109.5 . . ? C204 C206 H20K 109.5 . . ? C204 C206 H20L 109.5 . . ? H20K C206 H20L 109.5 . . ? C204 C206 H20M 109.5 . . ? H20K C206 H20M 109.5 . . ? H20L C206 H20M 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 O11 Mg1 N1 C11 82.40(18) . . . . ? O1 Mg1 N1 C11 -93.25(18) 2_655 . . . ? O1 Mg1 N1 C11 -22.71(17) . . . . ? N11 Mg1 N1 C11 170.85(17) . . . . ? C2 Mg1 N1 C11 1.27(16) . . . . ? Mg1 Mg1 N1 C11 -60.84(17) 2_655 . . . ? O11 Mg1 N1 C12 -115.13(17) . . . . ? O1 Mg1 N1 C12 69.22(18) 2_655 . . . ? O1 Mg1 N1 C12 139.76(17) . . . . ? N11 Mg1 N1 C12 -26.68(17) . . . . ? C2 Mg1 N1 C12 163.74(18) . . . . ? Mg1 Mg1 N1 C12 101.63(17) 2_655 . . . ? O11 Mg1 O1 C2 -47.60(16) . . . . ? O1 Mg1 O1 C2 -177.73(12) 2_655 . . . ? N1 Mg1 O1 C2 62.79(15) . . . . ? N11 Mg1 O1 C2 133.9(3) . . . . ? Mg1 Mg1 O1 C2 163.89(18) 2_655 . . . ? O11 Mg1 O1 Mg1 148.51(7) . . . 2_655 ? O1 Mg1 O1 Mg1 18.39(9) 2_655 . . 2_655 ? N1 Mg1 O1 Mg1 -101.10(8) . . . 2_655 ? N11 Mg1 O1 Mg1 -30.0(3) . . . 2_655 ? C2 Mg1 O1 Mg1 -163.89(18) . . . 2_655 ? Mg1 O1 C2 C1 95.1(3) 2_655 . . . ? Mg1 O1 C2 C1 -57.7(2) . . . . ? Mg1 O1 C2 C3 -85.0(3) 2_655 . . . ? Mg1 O1 C2 C3 122.19(19) . . . . ? Mg1 O1 C2 Mg1 152.8(3) 2_655 . . . ? C10 C1 C2 O1 174.1(2) . . . . ? C11 C1 C2 O1 -6.1(3) . . . . ? C10 C1 C2 C3 -5.8(3) . . . . ? C11 C1 C2 C3 174.1(2) . . . . ? C10 C1 C2 Mg1 139.51(19) . . . . ? C11 C1 C2 Mg1 -40.7(2) . . . . ? O11 Mg1 C2 O1 134.99(15) . . . . ? O1 Mg1 C2 O1 2.26(12) 2_655 . . . ? N1 Mg1 C2 O1 -111.74(15) . . . . ? N11 Mg1 C2 O1 -146.1(2) . . . . ? Mg1 Mg1 C2 O1 -11.20(12) 2_655 . . . ? O11 Mg1 C2 C1 -92.89(14) . . . . ? O1 Mg1 C2 C1 134.38(14) 2_655 . . . ? O1 Mg1 C2 C1 132.1(2) . . . . ? N1 Mg1 C2 C1 20.38(14) . . . . ? N11 Mg1 C2 C1 -14.0(3) . . . . ? Mg1 Mg1 C2 C1 120.92(14) 2_655 . . . ? O11 Mg1 C2 C3 44.3(2) . . . . ? O1 Mg1 C2 C3 -88.4(2) 2_655 . . . ? O1 Mg1 C2 C3 -90.7(2) . . . . ? N1 Mg1 C2 C3 157.6(2) . . . . ? N11 Mg1 C2 C3 123.2(3) . . . . ? Mg1 Mg1 C2 C3 -101.9(2) 2_655 . . . ? O1 C2 C3 C4 -179.7(2) . . . . ? C1 C2 C3 C4 0.2(3) . . . . ? Mg1 C2 C3 C4 -128.1(2) . . . . ? O1 C2 C3 C30 -2.0(3) . . . . ? C1 C2 C3 C30 177.9(2) . . . . ? Mg1 C2 C3 C30 49.6(3) . . . . ? C2 C3 C4 C5 4.6(4) . . . . ? C30 C3 C4 C5 -173.1(2) . . . . ? C3 C4 C5 C10 -3.7(4) . . . . ? C3 C4 C5 C6 174.5(2) . . . . ? C10 C5 C6 C7 -0.4(4) . . . . ? C4 C5 C6 C7 -178.6(2) . . . . ? C5 C6 C7 C8 2.2(4) . . . . ? C5 C6 C7 C70 -175.3(2) . . . . ? C6 C7 C8 C9 -2.0(4) . . . . ? C70 C7 C8 C9 175.7(2) . . . . ? C7 C8 C9 C10 -0.1(4) . . . . ? C4 C5 C10 C9 176.5(2) . . . . ? C6 C5 C10 C9 -1.7(3) . . . . ? C4 C5 C10 C1 -2.1(3) . . . . ? C6 C5 C10 C1 179.7(2) . . . . ? C8 C9 C10 C5 1.9(3) . . . . ? C8 C9 C10 C1 -179.5(2) . . . . ? C2 C1 C10 C5 6.7(3) . . . . ? C11 C1 C10 C5 -173.1(2) . . . . ? C2 C1 C10 C9 -171.8(2) . . . . ? C11 C1 C10 C9 8.4(3) . . . . ? C12 N1 C11 C19 -9.2(3) . . . . ? Mg1 N1 C11 C19 153.26(17) . . . . ? C12 N1 C11 C1 173.4(2) . . . . ? Mg1 N1 C11 C1 -24.1(3) . . . . ? C2 C1 C11 N1 52.3(3) . . . . ? C10 C1 C11 N1 -127.9(2) . . . . ? C2 C1 C11 C19 -125.1(2) . . . . ? C10 C1 C11 C19 54.7(3) . . . . ? C11 N1 C12 C13 2.8(4) . . . . ? Mg1 N1 C12 C13 -160.1(2) . . . . ? N1 C12 C13 C14 4.1(4) . . . . ? C12 C13 C14 C19 -4.3(4) . . . . ? C12 C13 C14 C15 172.7(2) . . . . ? C13 C14 C15 C16 -174.2(3) . . . . ? C19 C14 C15 C16 2.8(4) . . . . ? C14 C15 C16 C17 -0.5(4) . . . . ? C15 C16 C17 C18 -2.6(4) . . . . ? C16 C17 C18 C19 3.3(4) . . . . ? C13 C14 C19 C18 175.1(2) . . . . ? C15 C14 C19 C18 -2.0(3) . . . . ? C13 C14 C19 C11 -1.8(3) . . . . ? C15 C14 C19 C11 -178.9(2) . . . . ? C17 C18 C19 C14 -1.0(3) . . . . ? C17 C18 C19 C11 175.7(2) . . . . ? N1 C11 C19 C14 8.8(3) . . . . ? C1 C11 C19 C14 -173.9(2) . . . . ? N1 C11 C19 C18 -167.9(2) . . . . ? C1 C11 C19 C18 9.4(3) . . . . ? C4 C3 C30 C33 -1.5(3) . . . . ? C2 C3 C30 C33 -179.1(2) . . . . ? C4 C3 C30 C32 117.0(3) . . . . ? C2 C3 C30 C32 -60.6(3) . . . . ? C4 C3 C30 C31 -121.0(3) . . . . ? C2 C3 C30 C31 61.3(3) . . . . ? C6 C7 C70 C72 -5.4(3) . . . . ? C8 C7 C70 C72 177.1(2) . . . . ? C6 C7 C70 C73 114.3(3) . . . . ? C8 C7 C70 C73 -63.2(3) . . . . ? C6 C7 C70 C71 -126.5(3) . . . . ? C8 C7 C70 C71 56.0(3) . . . . ? O11 Mg1 N11 C111 2.36(17) . . . . ? O1 Mg1 N11 C111 134.21(17) 2_655 . . . ? O1 Mg1 N11 C111 -179.0(3) . . . . ? N1 Mg1 N11 C111 -109.20(17) . . . . ? C2 Mg1 N11 C111 -76.8(3) . . . . ? Mg1 Mg1 N11 C111 157.34(14) 2_655 . . . ? O11 Mg1 N11 C112 -148.02(18) . . . . ? O1 Mg1 N11 C112 -16.16(19) 2_655 . . . ? O1 Mg1 N11 C112 30.6(4) . . . . ? N1 Mg1 N11 C112 100.43(18) . . . . ? C2 Mg1 N11 C112 132.9(2) . . . . ? Mg1 Mg1 N11 C112 7.0(2) 2_655 . . . ? O1 Mg1 O11 C102 -133.41(17) 2_655 . . . ? O1 Mg1 O11 C102 140.22(17) . . . . ? N1 Mg1 O11 C102 51.83(19) . . . . ? N11 Mg1 O11 C102 -40.14(18) . . . . ? C2 Mg1 O11 C102 121.54(18) . . . . ? Mg1 Mg1 O11 C102 169.37(15) 2_655 . . . ? Mg1 O11 C102 C101 37.0(3) . . . . ? Mg1 O11 C102 C103 -146.55(18) . . . . ? C110 C101 C102 O11 -165.4(2) . . . . ? C111 C101 C102 O11 15.7(4) . . . . ? C110 C101 C102 C103 18.1(3) . . . . ? C111 C101 C102 C103 -160.8(2) . . . . ? O11 C102 C103 C104 168.3(2) . . . . ? C101 C102 C103 C104 -15.2(3) . . . . ? O11 C102 C103 C130 -13.2(3) . . . . ? C101 C102 C103 C130 163.3(2) . . . . ? C102 C103 C104 C105 2.2(4) . . . . ? C130 C103 C104 C105 -176.3(2) . . . . ? C103 C104 C105 C110 8.0(4) . . . . ? C103 C104 C105 C106 -172.9(2) . . . . ? C104 C105 C106 C107 -179.7(3) . . . . ? C110 C105 C106 C107 -0.7(4) . . . . ? C105 C106 C107 C108 1.6(4) . . . . ? C105 C106 C107 C170 -177.8(3) . . . . ? C106 C107 C108 C109 -1.0(4) . . . . ? C170 C107 C108 C109 178.4(3) . . . . ? C107 C108 C109 C110 -0.5(4) . . . . ? C108 C109 C110 C105 1.4(4) . . . . ? C108 C109 C110 C101 -174.9(3) . . . . ? C104 C105 C110 C109 178.2(2) . . . . ? C106 C105 C110 C109 -0.8(4) . . . . ? C104 C105 C110 C101 -5.3(4) . . . . ? C106 C105 C110 C101 175.6(2) . . . . ? C102 C101 C110 C109 168.3(3) . . . . ? C111 C101 C110 C109 -12.8(4) . . . . ? C102 C101 C110 C105 -7.9(4) . . . . ? C111 C101 C110 C105 171.1(2) . . . . ? C112 N11 C111 C119 10.9(3) . . . . ? Mg1 N11 C111 C119 -139.5(2) . . . . ? C112 N11 C111 C101 -171.6(2) . . . . ? Mg1 N11 C111 C101 38.0(3) . . . . ? C102 C101 C111 N11 -56.4(3) . . . . ? C110 C101 C111 N11 124.7(2) . . . . ? C102 C101 C111 C119 121.1(3) . . . . ? C110 C101 C111 C119 -57.8(3) . . . . ? C111 N11 C112 C113 -3.8(4) . . . . ? Mg1 N11 C112 C113 146.1(2) . . . . ? N11 C112 C113 C114 -5.7(4) . . . . ? C112 C113 C114 C119 7.6(4) . . . . ? C112 C113 C114 C115 -170.4(3) . . . . ? C119 C114 C115 C116 -1.9(5) . . . . ? C113 C114 C115 C116 176.0(3) . . . . ? C114 C115 C116 C117 1.6(6) . . . . ? C115 C116 C117 C118 -0.4(6) . . . . ? C116 C117 C118 C119 -0.5(5) . . . . ? C115 C114 C119 C118 1.0(4) . . . . ? C113 C114 C119 C118 -177.0(3) . . . . ? C115 C114 C119 C111 177.3(3) . . . . ? C113 C114 C119 C111 -0.7(4) . . . . ? C117 C118 C119 C114 0.2(4) . . . . ? C117 C118 C119 C111 -175.9(3) . . . . ? N11 C111 C119 C114 -8.8(4) . . . . ? C101 C111 C119 C114 173.7(2) . . . . ? N11 C111 C119 C118 167.3(2) . . . . ? C101 C111 C119 C118 -10.1(4) . . . . ? C104 C103 C130 C132 -112.2(3) . . . . ? C102 C103 C130 C132 69.3(3) . . . . ? C104 C103 C130 C131 126.5(2) . . . . ? C102 C103 C130 C131 -52.0(3) . . . . ? C104 C103 C130 C133 7.8(3) . . . . ? C102 C103 C130 C133 -170.6(2) . . . . ? C106 C107 C170 C173 0.2(4) . . . . ? C108 C107 C170 C173 -179.1(3) . . . . ? C106 C107 C170 C171 121.1(3) . . . . ? C108 C107 C170 C171 -58.3(4) . . . . ? C106 C107 C170 C172 -120.5(3) . . . . ? C108 C107 C170 C172 60.2(4) . . . . ? C201 C202 C203 C204 -175.4(6) . . . . ? C202 C203 C204 C206 159.9(6) . . . . ? C202 C203 C204 C205 -100.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.71 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.344 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.053 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 0.000 0.133 0.250 442.3 -4.5 2 0.000 -0.133 0.750 442.2 -4.3 3 0.500 0.367 0.750 442.2 -4.3 4 0.500 0.633 0.250 442.3 -4.5 _platon_squeeze_details ; The strucuture contains a disorered molecule of isohexane, which may be also be only partial occupancy. This could not be modelled in a physically-reasonable manner, and was handled using SQUEEZE. ; #===END