Supplememntary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Sumio Kaizaki' 'Akira Fuyuhiro' 'Md. Abdus Subhan' 'Takayoshi Suzuki' _publ_contact_author_name 'Prof Sumio Kaizaki' _publ_contact_author_address ; Department of Chemistry Osaka University, Graduate School of Science 1-1 Machikaneyama Toyonaka Osaka 560-0043 JAPAN ; _publ_contact_author_email KAIZAKI@CHEM.SCI.OSAKA-U.AC.JP _publ_section_title ; Synthesis, X-ray structures and NIR chiroptical properties of a series of dinuclear lanthanide(III) complexes [Ln2{m-(S-, or RS-pba)}4(HBpz3)2]; novel configurational chirality due to nonbonding Ln interaction ; data_Yb2RSpba _database_code_CSD 210009 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis(\m-2-phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) diytterbium(III) ; _chemical_name_common ; Tetrakis(mu-2- phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) diytterbium(iii) ; _chemical_melting_point ? _chemical_formula_moiety 'C58 H64 B2 N12 O8 Yb2' _chemical_formula_sum 'C58 H64 B2 N12 O8 Yb2' _chemical_formula_weight 1424.91 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.551(2) _cell_length_b 12.222(3) _cell_length_c 12.6247(17) _cell_angle_alpha 80.159(16) _cell_angle_beta 68.300(12) _cell_angle_gamma 66.306(16) _cell_volume 1515.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 710 _exptl_absorpt_coefficient_mu 3.128 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.486 _exptl_absorpt_correction_T_max 0.558 _exptl_absorpt_process_details Coppens_numerical _exptl_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.16 _diffrn_reflns_number 9189 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 30.02 _reflns_number_total 8807 _reflns_number_gt 6237 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS-86 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP _computing_publication_material 'SHELXL-97 and teXsan Ver. 1.11' _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^)+(0.0524P)^2^+1.3707P] 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 8807 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Yb Yb 0.116837(19) 0.49796(2) 0.089923(16) 0.05054(8) Uani 1 1 d . . . O1 O 0.1716(4) 0.5695(5) -0.0921(3) 0.0806(12) Uani 1 1 d . . . O2 O 0.0318(4) 0.5896(4) -0.1792(3) 0.0738(11) Uani 1 1 d . . . O3 O 0.2200(5) 0.3258(5) -0.0121(4) 0.0881(13) Uani 1 1 d . . . O4 O 0.0715(4) 0.3513(4) -0.0900(4) 0.0865(13) Uani 1 1 d . . . N11 N 0.3096(4) 0.3851(4) 0.2593(3) 0.0555(9) Uani 1 1 d . . . N12 N 0.2573(4) 0.3530(4) 0.1944(3) 0.0556(9) Uani 1 1 d . . . N21 N 0.3245(4) 0.5779(4) 0.1619(4) 0.0561(9) Uani 1 1 d . . . N22 N 0.2727(4) 0.5881(4) 0.0777(3) 0.0565(10) Uani 1 1 d . . . N31 N 0.1231(4) 0.5785(4) 0.3309(3) 0.0566(10) Uani 1 1 d . . . N32 N 0.0398(4) 0.5785(4) 0.2781(3) 0.0585(10) Uani 1 1 d . . . C1 C 0.1322(5) 0.5992(5) -0.1746(4) 0.0541(11) Uani 1 1 d . . . C2 C 0.2137(6) 0.6545(6) -0.2782(5) 0.0738(16) Uani 1 1 d . . . H2 H 0.2872 0.6543 -0.2569 0.088 Uiso 1 1 calc R . . C3 C 0.2783(7) 0.5803(6) -0.3765(6) 0.087(2) Uani 1 1 d . . . H3A H 0.3213 0.6231 -0.4405 0.103 Uiso 1 1 calc R . . H3B H 0.2097 0.5687 -0.3950 0.103 Uiso 1 1 calc R . . C4 C 0.3832(7) 0.4573(7) -0.3642(7) 0.094(2) Uani 1 1 d . . . H4A H 0.4632 0.4664 -0.3674 0.114 Uiso 1 1 calc R . . H4B H 0.4037 0.4078 -0.4250 0.114 Uiso 1 1 calc R . . H4C H 0.3483 0.4207 -0.2923 0.114 Uiso 1 1 calc R . . C5 C 0.1359(6) 0.7841(5) -0.2971(4) 0.0629(13) Uani 1 1 d . . . C6 C 0.1761(11) 0.8712(10) -0.2834(8) 0.127(4) Uani 1 1 d . . . H6 H 0.2490 0.8517 -0.2591 0.151 Uiso 1 1 calc R . . C7 C 0.1010(17) 0.9947(12) -0.3083(13) 0.177(7) Uani 1 1 d . . . H7 H 0.1259 1.0562 -0.3022 0.199 Uiso 1 1 calc R . . C8 C -0.0056(16) 1.0174(11) -0.3404(15) 0.183(8) Uani 1 1 d . . . H8 H -0.0562 1.0966 -0.3528 0.202 Uiso 1 1 calc R . . C9 C -0.0424(11) 0.9325(9) -0.3554(10) 0.140(4) Uani 1 1 d . . . H9 H -0.1144 0.9518 -0.3809 0.170 Uiso 1 1 calc R . . C10 C 0.0276(7) 0.8172(7) -0.3327(6) 0.0862(19) Uani 1 1 d . . . H10 H 0.0010 0.7580 -0.3418 0.105 Uiso 1 1 calc R . . C13 C 0.3017(6) 0.2336(5) 0.2014(5) 0.0663(13) Uani 1 1 d . . . H13 H 0.2803 0.1872 0.1659 0.080 Uiso 1 1 calc R . . C14 C 0.3826(6) 0.1882(6) 0.2673(5) 0.0753(16) Uani 1 1 d . . . H14 H 0.4259 0.1083 0.2843 0.090 Uiso 1 1 calc R . . C15 C 0.3856(5) 0.2869(5) 0.3028(5) 0.0669(14) Uani 1 1 d . . . H15 H 0.4326 0.2857 0.3492 0.079 Uiso 1 1 calc R . . C23 C 0.3358(6) 0.6471(6) -0.0086(5) 0.0711(15) Uani 1 1 d . . . H23 H 0.3199 0.6677 -0.0777 0.085 Uiso 1 1 calc R . . C24 C 0.4264(7) 0.6732(6) 0.0182(6) 0.0795(18) Uani 1 1 d . . . H24 H 0.4825 0.7126 -0.0276 0.095 Uiso 1 1 calc R . . C25 C 0.4165(6) 0.6289(6) 0.1267(5) 0.0706(15) Uani 1 1 d . . . H25 H 0.4653 0.6332 0.1691 0.085 Uiso 1 1 calc R . . C33 C -0.0848(5) 0.6344(5) 0.3476(5) 0.0676(14) Uani 1 1 d . . . H33 H -0.1628 0.6471 0.3335 0.082 Uiso 1 1 calc R . . C34 C -0.0802(7) 0.6708(6) 0.4442(5) 0.0813(18) Uani 1 1 d . . . H34 H -0.1525 0.7119 0.5054 0.096 Uiso 1 1 calc R . . C35 C 0.0521(7) 0.6336(6) 0.4301(4) 0.0715(15) Uani 1 1 d . . . H35 H 0.0873 0.6447 0.4811 0.088 Uiso 1 1 calc R . . C41 C 0.1768(5) 0.2899(5) -0.0685(4) 0.0618(12) Uani 1 1 d . . . C42 C 0.2527(8) 0.1639(6) -0.1130(10) 0.116(3) Uani 1 1 d . . . H42 H 0.1947 0.1646 -0.1536 0.137 Uiso 1 1 calc R . . C43 C 0.243(2) 0.0721(10) -0.0428(12) 0.262(12) Uani 1 1 d . . . H43A H 0.3006 0.0053 -0.0930 0.284 Uiso 1 1 calc R . . H43B H 0.2939 0.0709 0.0038 0.284 Uiso 1 1 calc R . . C44 C 0.160(2) 0.033(2) 0.0246(19) 0.39(2) Uani 1 1 d . . . H44A H 0.1577 0.0365 0.1008 0.361 Uiso 1 1 calc R . . H44B H 0.1836 -0.0481 0.0074 0.361 Uiso 1 1 calc R . . H44C H 0.0730 0.0807 0.0187 0.361 Uiso 1 1 calc R . . C45 C 0.3765(6) 0.1523(5) -0.2140(7) 0.0787(18) Uani 1 1 d . . . C46 C 0.4880(7) 0.1547(6) -0.2006(7) 0.089(2) Uani 1 1 d . . . H46 H 0.4844 0.1652 -0.1280 0.106 Uiso 1 1 calc R . . C47 C 0.6025(9) 0.1424(8) -0.2884(11) 0.125(3) Uani 1 1 d . . . H47 H 0.6756 0.1437 -0.2746 0.151 Uiso 1 1 calc R . . C48 C 0.6136(13) 0.1287(8) -0.3924(11) 0.131(4) Uani 1 1 d . . . H48 H 0.6939 0.1217 -0.4509 0.154 Uiso 1 1 calc R . . C49 C 0.5113(15) 0.1244(7) -0.4171(9) 0.131(4) Uani 1 1 d . . . H49 H 0.5203 0.1143 -0.4915 0.156 Uiso 1 1 calc R . . C50 C 0.3892(11) 0.1359(6) -0.3259(9) 0.115(3) Uani 1 1 d . . . H50 H 0.3175 0.1325 -0.3404 0.140 Uiso 1 1 calc R . . B1 B 0.2740(6) 0.5177(6) 0.2780(5) 0.0588(14) Uani 1 1 d . . . H1 H 0.3177 0.5235 0.3291 0.069 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 Yb 0.04467(10) 0.07264(15) 0.04003(10) 0.00898(8) -0.01586(7) -0.02990(9) O1 0.086(3) 0.127(4) 0.050(2) 0.023(2) -0.0287(19) -0.064(3) O2 0.071(2) 0.108(3) 0.062(2) 0.022(2) -0.0267(19) -0.058(2) O3 0.108(4) 0.103(3) 0.070(3) -0.012(2) -0.037(3) -0.045(3) O4 0.064(2) 0.107(3) 0.073(3) 0.022(2) -0.029(2) -0.021(2) N11 0.047(2) 0.067(3) 0.047(2) 0.0038(18) -0.0178(16) -0.0166(18) N12 0.056(2) 0.065(3) 0.050(2) 0.0028(18) -0.0203(18) -0.025(2) N21 0.053(2) 0.070(3) 0.054(2) 0.0046(19) -0.0215(18) -0.032(2) N22 0.057(2) 0.074(3) 0.048(2) 0.0092(19) -0.0189(17) -0.036(2) N31 0.058(2) 0.067(3) 0.045(2) 0.0010(18) -0.0214(17) -0.020(2) N32 0.046(2) 0.077(3) 0.047(2) -0.0012(19) -0.0126(16) -0.021(2) C1 0.050(2) 0.071(3) 0.039(2) 0.003(2) -0.0042(18) -0.030(2) C2 0.065(3) 0.095(4) 0.048(3) 0.018(3) -0.002(2) -0.040(3) C3 0.082(4) 0.086(4) 0.064(4) 0.008(3) 0.000(3) -0.029(4) C4 0.066(4) 0.094(5) 0.090(5) 0.012(4) -0.010(3) -0.017(4) C5 0.071(3) 0.071(3) 0.048(2) 0.003(2) -0.008(2) -0.039(3) C6 0.161(9) 0.149(9) 0.108(7) -0.015(6) -0.014(6) -0.117(8) C7 0.212(15) 0.124(10) 0.180(13) -0.043(9) 0.037(12) -0.125(11) C8 0.170(13) 0.079(7) 0.224(17) 0.008(8) 0.016(12) -0.050(8) C9 0.124(8) 0.095(7) 0.143(9) 0.024(6) -0.031(7) -0.006(6) C10 0.075(4) 0.085(4) 0.078(4) -0.002(3) -0.024(3) -0.011(3) C13 0.070(3) 0.061(3) 0.064(3) 0.004(2) -0.019(3) -0.025(3) C14 0.073(4) 0.065(4) 0.066(3) 0.011(3) -0.022(3) -0.009(3) C15 0.058(3) 0.074(4) 0.056(3) 0.010(3) -0.026(2) -0.010(3) C23 0.081(4) 0.091(4) 0.055(3) 0.014(3) -0.019(3) -0.055(3) C24 0.087(4) 0.099(5) 0.074(4) 0.007(3) -0.019(3) -0.066(4) C25 0.067(3) 0.084(4) 0.079(4) 0.002(3) -0.028(3) -0.045(3) C33 0.052(3) 0.072(4) 0.059(3) 0.004(3) -0.008(2) -0.016(3) C34 0.078(4) 0.083(4) 0.052(3) -0.005(3) -0.004(3) -0.014(3) C35 0.082(4) 0.078(4) 0.043(2) -0.005(2) -0.020(3) -0.018(3) C41 0.058(3) 0.068(3) 0.054(3) -0.001(2) -0.020(2) -0.017(2) C42 0.093(5) 0.063(4) 0.187(10) -0.023(5) -0.027(6) -0.033(4) C43 0.45(3) 0.091(7) 0.140(11) 0.022(7) 0.023(15) -0.120(13) C44 0.47(4) 0.61(5) 0.32(3) 0.30(3) -0.22(3) -0.46(4) C45 0.067(4) 0.048(3) 0.114(5) -0.022(3) -0.035(4) -0.002(3) C46 0.071(4) 0.080(4) 0.109(6) -0.031(4) -0.026(4) -0.012(3) C47 0.085(6) 0.106(7) 0.152(9) -0.046(7) -0.016(6) -0.006(5) C48 0.141(10) 0.079(6) 0.131(9) -0.016(6) -0.031(8) -0.008(6) C49 0.183(11) 0.063(5) 0.093(6) -0.013(4) -0.040(7) 0.008(6) C50 0.150(8) 0.055(4) 0.158(9) -0.018(5) -0.109(8) 0.002(4) B1 0.048(3) 0.081(4) 0.051(3) 0.003(3) -0.022(2) -0.025(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 Yb O4 2.214(4) 2_565 ? Yb O2 2.236(4) 2_565 ? Yb O1 2.265(4) . ? Yb O3 2.298(5) . ? Yb N22 2.411(4) . ? Yb N32 2.436(4) . ? Yb N12 2.446(4) . ? O1 C1 1.230(6) . ? O2 C1 1.234(6) . ? O2 Yb 2.236(4) 2_565 ? O3 C41 1.222(7) . ? O4 C41 1.248(6) . ? O4 Yb 2.214(4) 2_565 ? N11 C15 1.341(6) . ? N11 N12 1.363(6) . ? N11 B1 1.541(8) . ? N12 C13 1.338(7) . ? N21 C25 1.343(7) . ? N21 N22 1.366(6) . ? N21 B1 1.541(7) . ? N22 C23 1.343(6) . ? N31 C35 1.334(7) . ? N31 N32 1.359(6) . ? N31 B1 1.518(7) . ? N32 C33 1.337(6) . ? C1 C2 1.533(6) . ? C2 C3 1.440(9) . ? C2 C5 1.503(9) . ? C2 H2 0.9800 . ? C3 C4 1.532(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.370(9) . ? C5 C6 1.378(9) . ? C6 C7 1.455(18) . ? C6 H6 0.9300 . ? C7 C8 1.35(2) . ? C7 H7 0.9300 . ? C8 C9 1.332(18) . ? C8 H8 0.9300 . ? C9 C10 1.356(11) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C13 C14 1.369(8) . ? C13 H13 0.9300 . ? C14 C15 1.374(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C23 C24 1.371(8) . ? C23 H23 0.9300 . ? C24 C25 1.365(9) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C33 C34 1.393(9) . ? C33 H33 0.9300 . ? C34 C35 1.356(9) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C41 C42 1.517(9) . ? C42 C43 1.322(13) . ? C42 C45 1.497(11) . ? C42 H42 0.9800 . ? C43 C44 1.22(2) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.372(9) . ? C45 C50 1.406(11) . ? C46 C47 1.347(12) . ? C46 H46 0.9300 . ? C47 C48 1.304(14) . ? C47 H47 0.9300 . ? C48 C49 1.350(15) . ? C48 H48 0.9300 . ? C49 C50 1.425(15) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? B1 H1 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 O4 Yb O2 79.80(17) 2_565 2_565 ? O4 Yb O1 77.77(17) 2_565 . ? O2 Yb O1 128.88(14) 2_565 . ? O4 Yb O3 127.75(18) 2_565 . ? O2 Yb O3 80.60(18) 2_565 . ? O1 Yb O3 78.06(18) . . ? O4 Yb N22 105.67(17) 2_565 . ? O2 Yb N22 155.15(14) 2_565 . ? O1 Yb N22 75.70(14) . . ? O3 Yb N22 112.08(17) . . ? O4 Yb N32 78.58(16) 2_565 . ? O2 Yb N32 82.27(15) 2_565 . ? O1 Yb N32 135.62(17) . . ? O3 Yb N32 144.65(16) . . ? N22 Yb N32 75.33(14) . . ? O4 Yb N12 149.92(16) 2_565 . ? O2 Yb N12 86.03(14) 2_565 . ? O1 Yb N12 130.68(15) . . ? O3 Yb N12 74.89(16) . . ? N22 Yb N12 77.43(14) . . ? N32 Yb N12 73.28(14) . . ? O4 Yb C41 110.45(16) 2_565 . ? O2 Yb C41 72.36(16) 2_565 . ? O1 Yb C41 73.57(16) . . ? O3 Yb C41 17.48(15) . . ? N22 Yb C41 125.32(15) . . ? N32 Yb C41 150.53(15) . . ? N12 Yb C41 89.93(14) . . ? C1 O1 Yb 142.2(3) . . ? C1 O2 Yb 141.9(3) . 2_565 ? C41 O3 Yb 128.1(4) . . ? C41 O4 Yb 160.5(5) . 2_565 ? C15 N11 N12 109.6(5) . . ? C15 N11 B1 129.4(5) . . ? N12 N11 B1 121.0(4) . . ? C13 N12 N11 105.5(4) . . ? C13 N12 Yb 131.4(4) . . ? N11 N12 Yb 123.1(3) . . ? C25 N21 N22 109.8(4) . . ? C25 N21 B1 129.1(5) . . ? N22 N21 B1 121.0(4) . . ? C23 N22 N21 105.1(4) . . ? C23 N22 Yb 131.1(4) . . ? N21 N22 Yb 123.7(3) . . ? C35 N31 N32 110.2(4) . . ? C35 N31 B1 129.1(5) . . ? N32 N31 B1 120.7(4) . . ? C33 N32 N31 106.0(4) . . ? C33 N32 Yb 130.1(4) . . ? N31 N32 Yb 123.9(3) . . ? O1 C1 O2 125.1(4) . . ? O1 C1 C2 116.7(5) . . ? O2 C1 C2 118.2(5) . . ? C3 C2 C5 116.4(5) . . ? C3 C2 C1 112.3(5) . . ? C5 C2 C1 111.9(5) . . ? C3 C2 H2 105.0 . . ? C5 C2 H2 105.0 . . ? C1 C2 H2 105.0 . . ? C2 C3 C4 115.9(6) . . ? C2 C3 H3A 108.3 . . ? C4 C3 H3A 108.3 . . ? C2 C3 H3B 108.3 . . ? C4 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 118.9(8) . . ? C10 C5 C2 120.7(6) . . ? C6 C5 C2 120.3(7) . . ? C5 C6 C7 117.9(11) . . ? C5 C6 H6 121.0 . . ? C7 C6 H6 121.0 . . ? C8 C7 C6 118.1(11) . . ? C8 C7 H7 120.9 . . ? C6 C7 H7 120.9 . . ? C9 C8 C7 123.5(13) . . ? C9 C8 H8 118.2 . . ? C7 C8 H8 118.2 . . ? C8 C9 C10 118.4(13) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C9 C10 C5 123.0(9) . . ? C9 C10 H10 118.5 . . ? C5 C10 H10 118.5 . . ? N12 C13 C14 111.5(6) . . ? N12 C13 H13 124.2 . . ? C14 C13 H13 124.2 . . ? C13 C14 C15 104.7(5) . . ? C13 C14 H14 127.7 . . ? C15 C14 H14 127.7 . . ? N11 C15 C14 108.7(5) . . ? N11 C15 H15 125.7 . . ? C14 C15 H15 125.7 . . ? N22 C23 C24 111.4(5) . . ? N22 C23 H23 124.3 . . ? C24 C23 H23 124.3 . . ? C25 C24 C23 105.1(5) . . ? C25 C24 H24 127.5 . . ? C23 C24 H24 127.5 . . ? N21 C25 C24 108.6(5) . . ? N21 C25 H25 125.7 . . ? C24 C25 H25 125.7 . . ? N32 C33 C34 109.9(5) . . ? N32 C33 H33 125.1 . . ? C34 C33 H33 125.1 . . ? C35 C34 C33 105.4(5) . . ? C35 C34 H34 127.3 . . ? C33 C34 H34 127.3 . . ? N31 C35 C34 108.5(5) . . ? N31 C35 H35 125.7 . . ? C34 C35 H35 125.7 . . ? O3 C41 O4 123.1(6) . . ? O3 C41 C42 118.8(6) . . ? O4 C41 C42 118.1(6) . . ? O3 C41 Yb 34.4(3) . . ? O4 C41 Yb 89.0(4) . . ? C42 C41 Yb 152.3(5) . . ? C43 C42 C45 121.3(10) . . ? C43 C42 C41 119.6(10) . . ? C45 C42 C41 113.1(6) . . ? C43 C42 H42 98.1 . . ? C45 C42 H42 98.1 . . ? C41 C42 H42 98.1 . . ? C44 C43 C42 142(2) . . ? C44 C43 H43A 101.6 . . ? C42 C43 H43A 101.6 . . ? C44 C43 H43B 101.6 . . ? C42 C43 H43B 101.6 . . ? H43A C43 H43B 104.6 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 115.6(8) . . ? C46 C45 C42 120.3(8) . . ? C50 C45 C42 124.0(8) . . ? C47 C46 C45 122.5(9) . . ? C47 C46 H46 118.7 . . ? C45 C46 H46 118.7 . . ? C48 C47 C46 121.8(11) . . ? C48 C47 H47 119.1 . . ? C46 C47 H47 119.1 . . ? C47 C48 C49 121.6(12) . . ? C47 C48 H48 119.2 . . ? C49 C48 H48 119.2 . . ? C48 C49 C50 118.0(10) . . ? C48 C49 H49 121.0 . . ? C50 C49 H49 121.0 . . ? C45 C50 C49 120.4(9) . . ? C45 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? N31 B1 N21 110.1(4) . . ? N31 B1 N11 109.5(4) . . ? N21 B1 N11 108.7(4) . . ? N31 B1 H1 109.5 . . ? N21 B1 H1 109.5 . . ? N11 B1 H1 109.5 . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 #_geom_contact_publ_flag Yb Yb 4.1022(7) 2_565 ? Yb O2 3.748(5) . ? Yb O4 3.416(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 O4 Yb O1 C1 -49.6(7) 2_565 . . . ? O2 Yb O1 C1 16.4(8) 2_565 . . . ? O3 Yb O1 C1 83.7(7) . . . . ? N22 Yb O1 C1 -159.5(7) . . . . ? N32 Yb O1 C1 -108.9(7) . . . . ? N12 Yb O1 C1 141.5(7) . . . . ? C41 Yb O1 C1 66.3(7) . . . . ? O4 Yb O3 C41 -9.0(6) 2_565 . . . ? O2 Yb O3 C41 60.2(5) 2_565 . . . ? O1 Yb O3 C41 -73.1(5) . . . . ? N22 Yb O3 C41 -142.1(5) . . . . ? N32 Yb O3 C41 122.2(5) . . . . ? N12 Yb O3 C41 148.6(6) . . . . ? C15 N11 N12 C13 1.0(5) . . . . ? B1 N11 N12 C13 -176.5(4) . . . . ? C15 N11 N12 Yb -177.9(3) . . . . ? B1 N11 N12 Yb 4.6(6) . . . . ? O4 Yb N12 C13 116.5(5) 2_565 . . . ? O2 Yb N12 C13 54.8(5) 2_565 . . . ? O1 Yb N12 C13 -85.6(5) . . . . ? O3 Yb N12 C13 -26.6(5) . . . . ? N22 Yb N12 C13 -143.9(5) . . . . ? N32 Yb N12 C13 137.9(5) . . . . ? C41 Yb N12 C13 -17.6(5) . . . . ? O4 Yb N12 N11 -65.0(5) 2_565 . . . ? O2 Yb N12 N11 -126.7(4) 2_565 . . . ? O1 Yb N12 N11 93.0(4) . . . . ? O3 Yb N12 N11 152.0(4) . . . . ? N22 Yb N12 N11 34.7(3) . . . . ? N32 Yb N12 N11 -43.6(3) . . . . ? C41 Yb N12 N11 161.0(4) . . . . ? C25 N21 N22 C23 -0.3(6) . . . . ? B1 N21 N22 C23 178.3(5) . . . . ? C25 N21 N22 Yb 174.8(4) . . . . ? B1 N21 N22 Yb -6.6(6) . . . . ? O4 Yb N22 C23 -70.7(5) 2_565 . . . ? O2 Yb N22 C23 -170.4(5) 2_565 . . . ? O1 Yb N22 C23 1.9(5) . . . . ? O3 Yb N22 C23 72.4(6) . . . . ? N32 Yb N22 C23 -144.1(6) . . . . ? N12 Yb N22 C23 140.2(6) . . . . ? C41 Yb N22 C23 59.3(6) . . . . ? O4 Yb N22 N21 115.5(4) 2_565 . . . ? O2 Yb N22 N21 15.8(6) 2_565 . . . ? O1 Yb N22 N21 -171.8(4) . . . . ? O3 Yb N22 N21 -101.3(4) . . . . ? N32 Yb N22 N21 42.1(4) . . . . ? N12 Yb N22 N21 -33.6(4) . . . . ? C41 Yb N22 N21 -114.4(4) . . . . ? C35 N31 N32 C33 -0.4(6) . . . . ? B1 N31 N32 C33 177.7(5) . . . . ? C35 N31 N32 Yb 176.9(4) . . . . ? B1 N31 N32 Yb -4.9(6) . . . . ? O4 Yb N32 C33 30.2(5) 2_565 . . . ? O2 Yb N32 C33 -50.9(5) 2_565 . . . ? O1 Yb N32 C33 89.2(5) . . . . ? O3 Yb N32 C33 -112.4(5) . . . . ? N22 Yb N32 C33 140.0(5) . . . . ? N12 Yb N32 C33 -139.0(5) . . . . ? C41 Yb N32 C33 -81.3(6) . . . . ? O4 Yb N32 N31 -146.4(4) 2_565 . . . ? O2 Yb N32 N31 132.5(4) 2_565 . . . ? O1 Yb N32 N31 -87.4(4) . . . . ? O3 Yb N32 N31 70.9(5) . . . . ? N22 Yb N32 N31 -36.7(4) . . . . ? N12 Yb N32 N31 44.3(4) . . . . ? C41 Yb N32 N31 102.0(4) . . . . ? Yb O1 C1 O2 -4.2(11) . . . . ? Yb O1 C1 C2 174.6(5) . . . . ? Yb O2 C1 O1 -13.9(11) 2_565 . . . ? Yb O2 C1 C2 167.3(5) 2_565 . . . ? O1 C1 C2 C3 114.3(7) . . . . ? O2 C1 C2 C3 -66.8(8) . . . . ? O1 C1 C2 C5 -112.7(6) . . . . ? O2 C1 C2 C5 66.2(7) . . . . ? C5 C2 C3 C4 166.1(6) . . . . ? C1 C2 C3 C4 -63.1(8) . . . . ? C3 C2 C5 C10 61.9(8) . . . . ? C1 C2 C5 C10 -69.2(7) . . . . ? C3 C2 C5 C6 -115.3(8) . . . . ? C1 C2 C5 C6 113.7(7) . . . . ? C10 C5 C6 C7 -0.2(12) . . . . ? C2 C5 C6 C7 177.0(8) . . . . ? C5 C6 C7 C8 1.6(19) . . . . ? C6 C7 C8 C9 -3(2) . . . . ? C7 C8 C9 C10 3(2) . . . . ? C8 C9 C10 C5 -1.2(16) . . . . ? C6 C5 C10 C9 0.0(11) . . . . ? C2 C5 C10 C9 -177.2(7) . . . . ? N11 N12 C13 C14 -1.0(6) . . . . ? Yb N12 C13 C14 177.8(4) . . . . ? N12 C13 C14 C15 0.6(7) . . . . ? N12 N11 C15 C14 -0.7(6) . . . . ? B1 N11 C15 C14 176.5(5) . . . . ? C13 C14 C15 N11 0.1(7) . . . . ? N21 N22 C23 C24 0.6(7) . . . . ? Yb N22 C23 C24 -174.0(4) . . . . ? N22 C23 C24 C25 -0.7(8) . . . . ? N22 N21 C25 C24 -0.1(7) . . . . ? B1 N21 C25 C24 -178.5(6) . . . . ? C23 C24 C25 N21 0.5(8) . . . . ? N31 N32 C33 C34 0.5(6) . . . . ? Yb N32 C33 C34 -176.6(4) . . . . ? N32 C33 C34 C35 -0.5(7) . . . . ? N32 N31 C35 C34 0.1(7) . . . . ? B1 N31 C35 C34 -177.8(6) . . . . ? C33 C34 C35 N31 0.2(7) . . . . ? Yb O3 C41 O4 8.7(9) . . . . ? Yb O3 C41 C42 -170.1(5) . . . . ? Yb O4 C41 O3 -3.9(16) 2_565 . . . ? Yb O4 C41 C42 174.9(10) 2_565 . . . ? Yb O4 C41 Yb 1.0(12) 2_565 . . . ? O4 Yb C41 O3 172.4(5) 2_565 . . . ? O2 Yb C41 O3 -116.1(6) 2_565 . . . ? O1 Yb C41 O3 102.6(5) . . . . ? N22 Yb C41 O3 44.3(6) . . . . ? N32 Yb C41 O3 -84.3(6) . . . . ? N12 Yb C41 O3 -30.2(5) . . . . ? O4 Yb C41 O4 -0.4(4) 2_565 . . . ? O2 Yb C41 O4 71.2(3) 2_565 . . . ? O1 Yb C41 O4 -70.1(3) . . . . ? O3 Yb C41 O4 -172.8(7) . . . . ? N22 Yb C41 O4 -128.5(3) . . . . ? N32 Yb C41 O4 103.0(4) . . . . ? N12 Yb C41 O4 157.0(3) . . . . ? O4 Yb C41 C42 -168.7(10) 2_565 . . . ? O2 Yb C41 C42 -97.2(10) 2_565 . . . ? O1 Yb C41 C42 121.5(10) . . . . ? O3 Yb C41 C42 18.9(9) . . . . ? N22 Yb C41 C42 63.2(10) . . . . ? N32 Yb C41 C42 -65.3(11) . . . . ? N12 Yb C41 C42 -11.3(10) . . . . ? O3 C41 C42 C43 76.6(16) . . . . ? O4 C41 C42 C43 -102.2(16) . . . . ? Yb C41 C42 C43 64.6(18) . . . . ? O3 C41 C42 C45 -76.6(10) . . . . ? O4 C41 C42 C45 104.6(8) . . . . ? Yb C41 C42 C45 -88.7(13) . . . . ? C45 C42 C43 C44 -155(3) . . . . ? C41 C42 C43 C44 54(4) . . . . ? C43 C42 C45 C46 -79.2(15) . . . . ? C41 C42 C45 C46 73.5(10) . . . . ? C43 C42 C45 C50 99.2(16) . . . . ? C41 C42 C45 C50 -108.0(8) . . . . ? C50 C45 C46 C47 0.2(11) . . . . ? C42 C45 C46 C47 178.7(8) . . . . ? C45 C46 C47 C48 0.7(15) . . . . ? C46 C47 C48 C49 -1.0(17) . . . . ? C47 C48 C49 C50 0.3(15) . . . . ? C46 C45 C50 C49 -0.8(10) . . . . ? C42 C45 C50 C49 -179.3(7) . . . . ? C48 C49 C50 C45 0.6(12) . . . . ? C35 N31 B1 N21 -120.2(6) . . . . ? N32 N31 B1 N21 62.0(6) . . . . ? C35 N31 B1 N11 120.3(6) . . . . ? N32 N31 B1 N11 -57.4(6) . . . . ? C25 N21 B1 N31 122.6(6) . . . . ? N22 N21 B1 N31 -55.7(7) . . . . ? C25 N21 B1 N11 -117.4(6) . . . . ? N22 N21 B1 N11 64.3(6) . . . . ? C15 N11 B1 N31 -119.3(5) . . . . ? N12 N11 B1 N31 57.6(6) . . . . ? C15 N11 B1 N21 120.4(5) . . . . ? N12 N11 B1 N21 -62.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.196 _refine_diff_density_min -2.206 _refine_diff_density_rms 0.100 #==END data_Dy2Spba _database_code_CSD 210010 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis(\m-2-S-phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) didysprosium(III) ; _chemical_name_common ; Tetrakis(mu-2-S- phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) didysprosium(iii) ; _chemical_melting_point ? _chemical_formula_moiety 'C58 H64 B2 Dy2 N12 O8' _chemical_formula_sum 'C58 H64 B2 Dy2 N12 O8' _chemical_formula_weight 1403.83 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.0708(13) _cell_length_b 24.8098(18) _cell_length_c 19.2494(18) _cell_angle_alpha 90.00 _cell_angle_beta 103.903(4) _cell_angle_gamma 90.00 _cell_volume 6059.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8828 _cell_measurement_theta_min 4.7 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 2.510 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.951 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_special_details ? _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 31781 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? #_diffrn_reflns_number 58820 _diffrn_reflns_av_R_equivalents 0.1282 _diffrn_reflns_av_sigmaI/netI 0.1583 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.65 _diffrn_reflns_theta_max 27.48 _reflns_number_total 25370 _reflns_number_gt 18715 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS-86 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP _computing_publication_material 'SHELXL-97 and teXsan Ver. 1.11' _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^)+(0.0353P)^2^+50.3082P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.008(16) _refine_ls_number_reflns 25370 _refine_ls_number_parameters 1447 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1299 _refine_ls_R_factor_gt 0.0925 _refine_ls_wR_factor_ref 0.1724 _refine_ls_wR_factor_gt 0.1566 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.32139(5) 0.47336(3) 1.07812(3) 0.02343(16) Uani 1 1 d . . . Dy2 Dy 0.09829(5) 0.49197(3) 0.90768(3) 0.02250(16) Uani 1 1 d . . . Dy11 Dy 0.58898(5) 0.23442(3) 0.42846(3) 0.02430(16) Uani 1 1 d . . . Dy12 Dy 0.85714(5) 0.24941(3) 0.57558(3) 0.02588(17) Uani 1 1 d . . . O1 O 0.1226(7) 0.4928(5) 1.0268(5) 0.029(2) Uani 1 1 d . . . O2 O 0.1927(8) 0.4972(5) 1.1415(5) 0.036(3) Uani 1 1 d . . . O3 O 0.3089(8) 0.4722(4) 0.9565(5) 0.031(2) Uani 1 1 d . . . O4 O 0.2308(8) 0.4834(5) 0.8433(5) 0.034(3) Uani 1 1 d . . . O5 O 0.2383(8) 0.3928(4) 1.0396(5) 0.030(2) Uani 1 1 d . . . O6 O 0.1300(8) 0.4004(4) 0.9308(5) 0.024(2) Uani 1 1 d . . . O7 O 0.3065(8) 0.5626(4) 1.0435(6) 0.032(3) Uani 1 1 d . . . O8 O 0.1895(8) 0.5691(4) 0.9373(6) 0.032(3) Uani 1 1 d . . . O11 O 0.7242(8) 0.3033(4) 0.5167(6) 0.040(3) Uani 1 1 d . . . O12 O 0.5994(9) 0.3294(5) 0.4290(6) 0.043(3) Uani 1 1 d . . . O13 O 0.7058(10) 0.1687(5) 0.4803(7) 0.050(3) Uani 1 1 d . . . O14 O 0.8594(9) 0.1577(5) 0.5560(8) 0.054(4) Uani 1 1 d . . . O15 O 0.7266(7) 0.2427(5) 0.3736(5) 0.038(3) Uani 1 1 d . . . O16 O 0.8725(7) 0.2482(5) 0.4610(5) 0.034(2) Uani 1 1 d . . . O17 O 0.5674(7) 0.2300(4) 0.5427(5) 0.028(2) Uani 1 1 d . . . O18 O 0.7184(7) 0.2255(5) 0.6229(5) 0.033(3) Uani 1 1 d . . . N11 N 0.5603(9) 0.4947(6) 1.1944(7) 0.040(3) Uani 1 1 d . . . N12 N 0.4829(9) 0.5182(5) 1.1467(8) 0.038(3) Uani 1 1 d . . . N16 N -0.1120(9) 0.4879(5) 0.7640(7) 0.034(3) Uani 1 1 d . . . N17 N -0.0074(9) 0.4783(5) 0.7846(6) 0.028(3) Uani 1 1 d . . . N21 N 0.4651(10) 0.4145(6) 1.2295(7) 0.037(3) Uani 1 1 d . . . N22 N 0.3669(9) 0.4284(5) 1.1952(6) 0.030(3) Uani 1 1 d . . . N26 N -0.1681(10) 0.4681(6) 0.8752(7) 0.035(3) Uani 1 1 d . . . N27 N -0.0733(10) 0.4536(5) 0.9179(6) 0.031(3) Uani 1 1 d . . . N31 N 0.5538(12) 0.4046(6) 1.1310(8) 0.046(4) Uani 1 1 d . . . N32 N 0.4703(10) 0.4108(5) 1.0753(7) 0.034(3) Uani 1 1 d . . . N36 N -0.1328(9) 0.5622(5) 0.8479(7) 0.030(3) Uani 1 1 d . . . N37 N -0.0317(9) 0.5675(6) 0.8857(7) 0.033(3) Uani 1 1 d . . . N111 N 0.3811(9) 0.1544(6) 0.3451(7) 0.031(3) Uani 1 1 d . . . N112 N 0.4775(10) 0.1539(6) 0.3932(7) 0.035(3) Uani 1 1 d . . . N116 N 1.1067(11) 0.2498(6) 0.6824(7) 0.042(3) Uani 1 1 d . . . N117 N 1.0336(9) 0.2184(5) 0.6388(6) 0.036(3) Uani 1 1 d . . . N121 N 0.3222(8) 0.2473(6) 0.3686(6) 0.031(3) Uani 1 1 d . . . N122 N 0.4050(9) 0.2661(5) 0.4199(7) 0.029(3) Uani 1 1 d . . . N126 N 1.0625(11) 0.3383(6) 0.6234(7) 0.039(4) Uani 1 1 d . . . N127 N 0.9746(11) 0.3275(6) 0.5692(6) 0.034(3) Uani 1 1 d . . . N131 N 0.4034(9) 0.2329(6) 0.2696(6) 0.033(3) Uani 1 1 d . . . N132 N 0.5091(8) 0.2446(5) 0.2968(6) 0.022(3) Uani 1 1 d . . . N136 N 0.9907(11) 0.3149(5) 0.7267(6) 0.031(3) Uani 1 1 d . . . N137 N 0.8920(10) 0.2962(5) 0.6938(6) 0.031(3) Uani 1 1 d . . . C1 C 0.1148(11) 0.5009(6) 1.0909(8) 0.026(3) Uani 1 1 d . . . C2 C 0.0058(12) 0.5172(7) 1.1018(9) 0.037(4) Uani 1 1 d . . . H2C H -0.0448 0.5168 1.0551 0.050 Uiso 1 1 calc R . . C3 C -0.0292(14) 0.4783(10) 1.1487(10) 0.068(7) Uani 1 1 d . . . H3A H 0.0187 0.4796 1.1957 0.082 Uiso 1 1 calc R . . H3B H -0.0259 0.4423 1.1296 0.082 Uiso 1 1 calc R . . C4 C -0.1429(16) 0.4891(14) 1.1562(13) 0.117(11) Uani 1 1 d . . . H4A H -0.1610 0.4632 1.1883 0.130 Uiso 1 1 calc R . . H4B H -0.1913 0.4861 1.1101 0.130 Uiso 1 1 calc R . . H4C H -0.1469 0.5248 1.1748 0.130 Uiso 1 1 calc R . . C5 C 0.0115(12) 0.5750(7) 1.1315(8) 0.031(4) Uani 1 1 d . . . C6 C -0.0488(15) 0.6155(9) 1.0892(10) 0.055(5) Uani 1 1 d . . . H6 H -0.0905 0.6070 1.0442 0.069 Uiso 1 1 calc R . . C7 C -0.046(2) 0.6677(10) 1.1144(16) 0.090(9) Uani 1 1 d . . . H7 H -0.0840 0.6946 1.0857 0.099 Uiso 1 1 calc R . . C8 C 0.0136(17) 0.6804(8) 1.1826(14) 0.067(6) Uani 1 1 d . . . H8 H 0.0164 0.7155 1.1999 0.082 Uiso 1 1 calc R . . C9 C 0.0674(17) 0.6402(9) 1.2229(12) 0.068(7) Uani 1 1 d . . . H9 H 0.1039 0.6479 1.2695 0.080 Uiso 1 1 calc R . . C10 C 0.0703(14) 0.5904(8) 1.1991(10) 0.054(6) Uani 1 1 d . . . H10 H 0.1126 0.5650 1.2280 0.066 Uiso 1 1 calc R . . C13 C 0.5071(14) 0.5710(8) 1.1512(8) 0.044(5) Uani 1 1 d . . . H13 H 0.4650 0.5985 1.1268 0.052 Uiso 1 1 calc R . . C14 C 0.6062(19) 0.5779(10) 1.1987(12) 0.078(7) Uani 1 1 d . . . H14 H 0.6438 0.6098 1.2098 0.093 Uiso 1 1 calc R . . C15 C 0.6349(16) 0.5289(8) 1.2243(10) 0.052(5) Uiso 1 1 d . . . H15 H 0.6970 0.5203 1.2577 0.083 Uiso 1 1 calc R . . C18 C 0.0262(12) 0.4635(7) 0.7288(8) 0.036(4) Uani 1 1 d . . . H18 H 0.0962 0.4574 0.7285 0.038 Uiso 1 1 calc R . . C19 C -0.0606(13) 0.4584(7) 0.6692(10) 0.042(4) Uiso 1 1 d . . . H19 H -0.0608 0.4460 0.6235 0.050 Uiso 1 1 calc R . . C20 C -0.1437(12) 0.4758(7) 0.6941(7) 0.035(4) Uani 1 1 d . . . H20 H -0.2125 0.4789 0.6667 0.042 Uiso 1 1 calc R . . C23 C 0.3049(16) 0.4060(7) 1.2324(9) 0.043(4) Uani 1 1 d . . . H23 H 0.2318 0.4077 1.2187 0.055 Uiso 1 1 calc R . . C24 C 0.3598(15) 0.3796(6) 1.2940(8) 0.036(4) Uani 1 1 d . . . H24 H 0.3340 0.3622 1.3291 0.043 Uiso 1 1 calc R . . C25 C 0.4606(16) 0.3859(7) 1.2892(8) 0.041(5) Uani 1 1 d . . . H25 H 0.5192 0.3725 1.3221 0.044 Uiso 1 1 calc R . . C28 C -0.0916(14) 0.4187(7) 0.9670(9) 0.040(4) Uani 1 1 d . . . H28 H -0.0405 0.4023 1.0028 0.051 Uiso 1 1 calc R . . C29 C -0.2034(17) 0.4112(9) 0.9547(11) 0.062(6) Uani 1 1 d . . . H29 H -0.2391 0.3900 0.9810 0.072 Uiso 1 1 calc R . . C30 C -0.2454(13) 0.4414(8) 0.8966(9) 0.045(4) Uani 1 1 d . . . H30 H -0.3168 0.4436 0.8746 0.054 Uiso 1 1 calc R . . C33 C 0.4861(14) 0.3793(6) 1.0242(9) 0.037(4) Uani 1 1 d . . . H33 H 0.4395 0.3766 0.9795 0.039 Uiso 1 1 calc R . . C34 C 0.5797(13) 0.3501(7) 1.0435(9) 0.043(4) Uani 1 1 d . . . H34 H 0.6070 0.3248 1.0173 0.051 Uiso 1 1 calc R . . C35 C 0.6210(12) 0.3688(7) 1.1117(9) 0.036(4) Uani 1 1 d . . . H35 H 0.6857 0.3585 1.1406 0.049 Uiso 1 1 calc R . . C38 C -0.0198(14) 0.6194(7) 0.9081(9) 0.038(4) Uani 1 1 d . . . H38 H 0.0424 0.6343 0.9352 0.046 Uiso 1 1 calc R . . C39 C -0.1130(15) 0.6468(8) 0.8851(11) 0.050(5) Uani 1 1 d . . . H39 H -0.1261 0.6830 0.8921 0.063 Uiso 1 1 calc R . . C40 C -0.1834(13) 0.6083(7) 0.8489(9) 0.037(4) Uani 1 1 d . . . H40 H -0.2546 0.6141 0.8286 0.047 Uiso 1 1 calc R . . C41 C 0.3142(11) 0.4776(6) 0.8916(7) 0.026(3) Uani 1 1 d . . . C42 C 0.4201(11) 0.4746(7) 0.8748(7) 0.031(3) Uani 1 1 d . . . H42 H 0.4628 0.4507 0.9109 0.039 Uiso 1 1 calc R . . C43 C 0.4160(14) 0.4481(8) 0.8012(9) 0.047(5) Uani 1 1 d . . . H43A H 0.3666 0.4679 0.7644 0.053 Uiso 1 1 calc R . . H43B H 0.4850 0.4511 0.7910 0.053 Uiso 1 1 calc R . . C44 C 0.3853(15) 0.3917(8) 0.7970(10) 0.049(5) Uani 1 1 d . . . H44A H 0.4348 0.3715 0.8324 0.057 Uiso 1 1 calc R . . H44B H 0.3847 0.3780 0.7503 0.057 Uiso 1 1 calc R . . H44C H 0.3162 0.3883 0.8056 0.057 Uiso 1 1 calc R . . C45 C 0.4718(14) 0.5289(6) 0.8868(9) 0.036(4) Uani 1 1 d . . . C46 C 0.5437(16) 0.5400(8) 0.9520(11) 0.053(5) Uani 1 1 d . . . H46 H 0.5571 0.5136 0.9874 0.069 Uiso 1 1 calc R . . C47 C 0.5968(16) 0.5905(11) 0.9659(15) 0.077(8) Uani 1 1 d . . . H47 H 0.6401 0.5984 1.0106 0.107 Uiso 1 1 calc R . . C48 C 0.581(2) 0.6286(10) 0.9082(16) 0.076(7) Uani 1 1 d . . . H48 H 0.6204 0.6603 0.9132 0.088 Uiso 1 1 calc R . . C49 C 0.507(2) 0.6179(8) 0.8451(15) 0.068(7) Uani 1 1 d . . . H49 H 0.4925 0.6438 0.8091 0.080 Uiso 1 1 calc R . . C50 C 0.4539(16) 0.5683(7) 0.8350(12) 0.053(5) Uani 1 1 d . . . H50 H 0.4050 0.5619 0.7920 0.066 Uiso 1 1 calc R . . C51 C 0.1764(11) 0.3730(6) 0.9847(7) 0.023(3) Uani 1 1 d . . . C52 C 0.1485(12) 0.3147(6) 0.9852(8) 0.032(4) Uani 1 1 d . . . H52 H 0.1042 0.3060 0.9378 0.038 Uiso 1 1 calc R . . C53 C 0.2464(15) 0.2782(6) 0.9973(9) 0.044(5) Uani 1 1 d . . . H53A H 0.2986 0.2907 1.0389 0.050 Uiso 1 1 calc R . . H53B H 0.2269 0.2416 1.0066 0.050 Uiso 1 1 calc R . . C54 C 0.2936(16) 0.2785(8) 0.9324(11) 0.059(5) Uani 1 1 d . . . H54A H 0.3110 0.3148 0.9223 0.075 Uiso 1 1 calc R . . H54B H 0.2433 0.2641 0.8918 0.075 Uiso 1 1 calc R . . H54C H 0.3562 0.2567 0.9421 0.075 Uiso 1 1 calc R . . C55 C 0.0827(12) 0.3056(6) 1.0383(8) 0.028(3) Uani 1 1 d . . . C56 C 0.1185(15) 0.3135(7) 1.1089(9) 0.044(5) Uani 1 1 d . . . H56 H 0.1863 0.3272 1.1247 0.051 Uiso 1 1 calc R . . C57 C 0.0643(17) 0.3033(9) 1.1589(10) 0.060(6) Uani 1 1 d . . . H57 H 0.0955 0.3085 1.2072 0.078 Uiso 1 1 calc R . . C58 C -0.0409(17) 0.2846(8) 1.1368(13) 0.063(6) Uani 1 1 d . . . H58 H -0.0809 0.2776 1.1697 0.073 Uiso 1 1 calc R . . C59 C -0.0822(18) 0.2771(9) 1.0634(11) 0.061(6) Uani 1 1 d . . . H59 H -0.1516 0.2660 1.0465 0.075 Uiso 1 1 calc R . . C60 C -0.0194(14) 0.2864(7) 1.0153(9) 0.042(4) Uani 1 1 d . . . H60 H -0.0466 0.2795 0.9669 0.051 Uiso 1 1 calc R . . C71 C 0.2669(11) 0.5866(6) 0.9833(8) 0.029(4) Uani 1 1 d . . . C72 C 0.3157(12) 0.6406(5) 0.9714(8) 0.027(3) Uani 1 1 d . . . H72 H 0.3873 0.6321 0.9675 0.033 Uiso 1 1 calc R . . C73 C 0.2616(13) 0.6650(6) 0.9004(9) 0.036(4) Uani 1 1 d . . . H73A H 0.1892 0.6731 0.9010 0.045 Uiso 1 1 calc R . . H73B H 0.2600 0.6384 0.8633 0.045 Uiso 1 1 calc R . . C74 C 0.3122(15) 0.7159(8) 0.8807(10) 0.056(5) Uani 1 1 d . . . H74A H 0.3139 0.7428 0.9168 0.065 Uiso 1 1 calc R . . H74B H 0.2720 0.7291 0.8354 0.065 Uiso 1 1 calc R . . H74C H 0.3828 0.7082 0.8774 0.065 Uiso 1 1 calc R . . C75 C 0.3294(11) 0.6783(5) 1.0334(9) 0.024(3) Uani 1 1 d . . . C76 C 0.4196(13) 0.7093(7) 1.0581(9) 0.043(4) Uani 1 1 d . . . H76 H 0.4762 0.7050 1.0372 0.055 Uiso 1 1 calc R . . C77 C 0.4274(17) 0.7456(9) 1.1117(10) 0.064(6) Uani 1 1 d . . . H77 H 0.4896 0.7650 1.1275 0.076 Uiso 1 1 calc R . . C78 C 0.3443(15) 0.7542(8) 1.1431(9) 0.050(5) Uani 1 1 d . . . H78 H 0.3514 0.7795 1.1797 0.059 Uiso 1 1 calc R . . C79 C 0.2505(14) 0.7261(7) 1.1212(9) 0.047(4) Uani 1 1 d . . . H79 H 0.1932 0.7331 1.1406 0.056 Uiso 1 1 calc R . . C80 C 0.2458(13) 0.6856(6) 1.0674(10) 0.043(5) Uani 1 1 d . . . H80 H 0.1865 0.6636 1.0547 0.049 Uiso 1 1 calc R . . C101 C 0.6729(10) 0.3404(6) 0.4816(7) 0.018(3) Uani 1 1 d . . . C102 C 0.6934(12) 0.3989(6) 0.5090(8) 0.033(4) Uani 1 1 d . . . H102 H 0.7602 0.3991 0.5455 0.039 Uiso 1 1 calc R . . C103 C 0.7043(13) 0.4378(6) 0.4514(9) 0.037(4) Uani 1 1 d . . . H103 H 0.6372 0.4414 0.4168 0.048 Uiso 1 1 calc R . . H203 H 0.7554 0.4241 0.4267 0.048 Uiso 1 1 calc R . . C104 C 0.7400(13) 0.4930(7) 0.4835(9) 0.048(4) Uani 1 1 d . . . H104 H 0.7465 0.5174 0.4460 0.060 Uiso 1 1 calc R . . H204 H 0.8070 0.4896 0.5172 0.060 Uiso 1 1 calc R . . H304 H 0.6890 0.5068 0.5074 0.060 Uiso 1 1 calc R . . C105 C 0.6079(13) 0.4121(7) 0.5456(10) 0.041(4) Uani 1 1 d . . . C106 C 0.6254(12) 0.4059(8) 0.6209(10) 0.041(4) Uani 1 1 d . . . H106 H 0.6916 0.3954 0.6474 0.046 Uiso 1 1 calc R . . C107 C 0.5473(19) 0.4148(8) 0.6551(11) 0.054(6) Uani 1 1 d . . . H107 H 0.5604 0.4086 0.7042 0.063 Uiso 1 1 calc R . . C108 C 0.4523(18) 0.4322(8) 0.6201(14) 0.065(6) Uani 1 1 d . . . H108 H 0.4013 0.4405 0.6448 0.079 Uiso 1 1 calc R . . C109 C 0.4308(17) 0.4377(9) 0.5471(12) 0.058(6) Uani 1 1 d . . . H109 H 0.3640 0.4487 0.5222 0.065 Uiso 1 1 calc R . . C110 C 0.5057(14) 0.4273(6) 0.5104(10) 0.040(4) Uani 1 1 d . . . H110 H 0.4883 0.4304 0.4608 0.048 Uiso 1 1 calc R . . C113 C 0.4931(12) 0.1026(7) 0.4116(9) 0.039(4) Uani 1 1 d . . . H113 H 0.5525 0.0897 0.4441 0.047 Uiso 1 1 calc R . . C114 C 0.4124(14) 0.0717(7) 0.3775(11) 0.053(6) Uani 1 1 d . . . H114 H 0.4067 0.0344 0.3808 0.061 Uiso 1 1 calc R . . C115 C 0.3416(14) 0.1052(7) 0.3375(9) 0.044(5) Uani 1 1 d . . . H115 H 0.2759 0.0955 0.3093 0.048 Uiso 1 1 calc R . . C118 C 1.0774(15) 0.1689(8) 0.6391(11) 0.062(6) Uani 1 1 d . . . H118 H 1.0442 0.1385 0.6157 0.079 Uiso 1 1 calc R . . C119 C 1.1816(18) 0.1711(9) 0.6807(14) 0.092(9) Uani 1 1 d . . . H119 H 1.2310 0.1434 0.6891 0.106 Uiso 1 1 calc R . . C120 C 1.1947(15) 0.2227(10) 0.7064(12) 0.085(8) Uani 1 1 d . . . H120 H 1.2560 0.2365 0.7361 0.091 Uiso 1 1 calc R . . C123 C 0.3687(12) 0.2983(7) 0.4637(9) 0.039(4) Uani 1 1 d . . . H123 H 0.4092 0.3153 0.5042 0.047 Uiso 1 1 calc R . . C124 C 0.2607(12) 0.3025(8) 0.4389(9) 0.043(5) Uani 1 1 d . . . H124 H 0.2155 0.3243 0.4571 0.051 Uiso 1 1 calc R . . C125 C 0.2345(11) 0.2686(7) 0.3833(8) 0.036(4) Uani 1 1 d . . . H125 H 0.1659 0.2609 0.3584 0.041 Uiso 1 1 calc R . . C128 C 0.9816(14) 0.3588(7) 0.5151(8) 0.042(4) Uani 1 1 d . . . H128 H 0.9336 0.3582 0.4708 0.045 Uiso 1 1 calc R . . C129 C 1.0677(15) 0.3924(7) 0.5316(9) 0.043(4) Uani 1 1 d . . . H129 H 1.0876 0.4187 0.5029 0.057 Uiso 1 1 calc R . . C130 C 1.1180(15) 0.3781(7) 0.6011(10) 0.049(5) Uani 1 1 d . . . H130 H 1.1800 0.3934 0.6280 0.060 Uiso 1 1 calc R . . C133 C 0.5439(11) 0.2677(6) 0.2448(7) 0.023(3) Uani 1 1 d . . . H133 H 0.6127 0.2797 0.2494 0.027 Uiso 1 1 calc R . . C134 C 0.4659(12) 0.2717(7) 0.1836(8) 0.037(4) Uani 1 1 d . . . H134 H 0.4706 0.2868 0.1402 0.047 Uiso 1 1 calc R . . C135 C 0.3787(12) 0.2486(7) 0.1998(7) 0.037(4) Uani 1 1 d . . . H135 H 0.3132 0.2444 0.1680 0.045 Uiso 1 1 calc R . . C138 C 0.8271(12) 0.3084(7) 0.7351(8) 0.033(4) Uani 1 1 d . . . H138 H 0.7563 0.2989 0.7257 0.042 Uiso 1 1 calc R . . C139 C 0.8804(16) 0.3369(8) 0.7934(9) 0.045(5) Uani 1 1 d . . . H139 H 0.8535 0.3515 0.8298 0.056 Uiso 1 1 calc R . . C140 C 0.9817(16) 0.3392(7) 0.7864(8) 0.044(5) Uani 1 1 d . . . H140 H 1.0370 0.3555 0.8191 0.056 Uiso 1 1 calc R . . C141 C 0.7830(13) 0.1403(7) 0.5103(9) 0.035(4) Uani 1 1 d . . . C142 C 0.7837(13) 0.0823(7) 0.4829(9) 0.043(5) Uani 1 1 d . . . H142 H 0.7122 0.0679 0.4763 0.051 Uiso 1 1 calc R . . C143 C 0.8099(17) 0.0830(7) 0.4087(10) 0.053(5) Uani 1 1 d . . . H143 H 0.7679 0.1107 0.3795 0.069 Uiso 1 1 calc R . . H243 H 0.8835 0.0926 0.4148 0.069 Uiso 1 1 calc R . . C144 C 0.790(2) 0.0316(9) 0.3712(16) 0.104(10) Uani 1 1 d . . . H144 H 0.8088 0.0344 0.3260 0.118 Uiso 1 1 calc R . . H244 H 0.7171 0.0225 0.3633 0.118 Uiso 1 1 calc R . . H344 H 0.8323 0.0040 0.3995 0.118 Uiso 1 1 calc R . . C145 C 0.8575(13) 0.0464(6) 0.5382(9) 0.036(4) Uani 1 1 d . . . C146 C 0.8125(14) 0.0184(7) 0.5847(10) 0.047(5) Uani 1 1 d . . . H146 H 0.7410 0.0223 0.5824 0.058 Uiso 1 1 calc R . . C147 C 0.875(3) -0.0163(11) 0.6360(12) 0.093(9) Uani 1 1 d . . . H147 H 0.8438 -0.0387 0.6636 0.112 Uiso 1 1 calc R . . C148 C 0.978(2) -0.0168(12) 0.6447(12) 0.088(8) Uani 1 1 d . . . H148 H 1.0209 -0.0352 0.6831 0.101 Uiso 1 1 calc R . . C149 C 1.0219(18) 0.0094(9) 0.5979(12) 0.075(7) Uani 1 1 d . . . H149 H 1.0940 0.0056 0.6021 0.084 Uiso 1 1 calc R . . C150 C 0.9634(16) 0.0423(8) 0.5424(9) 0.051(5) Uani 1 1 d . . . H150 H 0.9950 0.0603 0.5106 0.062 Uiso 1 1 calc R . . C151 C 0.8266(10) 0.2454(6) 0.3970(7) 0.023(3) Uani 1 1 d . . . C152 C 0.8899(12) 0.2411(7) 0.3403(8) 0.037(4) Uani 1 1 d . . . H152 H 0.8403 0.2354 0.2938 0.048 Uiso 1 1 calc R . . C153 C 0.9459(13) 0.2937(7) 0.3370(9) 0.041(4) Uani 1 1 d . . . H153 H 0.9907 0.2903 0.3036 0.051 Uiso 1 1 calc R . . H253 H 0.9906 0.3018 0.3838 0.051 Uiso 1 1 calc R . . C154 C 0.8662(16) 0.3412(9) 0.3127(12) 0.062(6) Uani 1 1 d . . . H154 H 0.9044 0.3740 0.3110 0.074 Uiso 1 1 calc R . . H254 H 0.8227 0.3451 0.3461 0.074 Uiso 1 1 calc R . . H354 H 0.8225 0.3336 0.2660 0.074 Uiso 1 1 calc R . . C155 C 0.9687(15) 0.1933(7) 0.3538(9) 0.041(4) Uani 1 1 d . . . C156 C 0.9666(17) 0.1566(7) 0.3027(10) 0.050(5) Uani 1 1 d . . . H156 H 0.9210 0.1606 0.2577 0.060 Uiso 1 1 calc R . . C157 C 1.0355(19) 0.1113(9) 0.3181(12) 0.063(6) Uani 1 1 d . . . H157 H 1.0327 0.0844 0.2840 0.073 Uiso 1 1 calc R . . C158 C 1.1037(18) 0.1078(10) 0.3812(14) 0.070(7) Uani 1 1 d . . . H158 H 1.1487 0.0782 0.3905 0.089 Uiso 1 1 calc R . . C159 C 1.1098(15) 0.1455(8) 0.4325(13) 0.055(5) Uani 1 1 d . . . H159 H 1.1596 0.1426 0.4758 0.069 Uiso 1 1 calc R . . C160 C 1.0406(12) 0.1888(8) 0.4195(9) 0.039(4) Uani 1 1 d . . . H160 H 1.0424 0.2148 0.4547 0.043 Uiso 1 1 calc R . . C171 C 0.6202(12) 0.2202(6) 0.6037(8) 0.030(4) Uani 1 1 d . . . C172 C 0.5689(14) 0.2002(6) 0.6604(8) 0.041(4) Uani 1 1 d . . . H172 H 0.6107 0.2125 0.7070 0.050 Uiso 1 1 calc R . . C173 C 0.4569(14) 0.2229(8) 0.6493(11) 0.057(5) Uani 1 1 d . . . H173 H 0.4186 0.2154 0.6005 0.072 Uiso 1 1 calc R . . H273 H 0.4215 0.2039 0.6808 0.072 Uiso 1 1 calc R . . C174 C 0.4512(19) 0.2810(9) 0.6624(11) 0.070(7) Uani 1 1 d . . . H174 H 0.4874 0.2889 0.7109 0.086 Uiso 1 1 calc R . . H274 H 0.3787 0.2917 0.6546 0.086 Uiso 1 1 calc R . . H374 H 0.4837 0.3004 0.6302 0.086 Uiso 1 1 calc R . . C175 C 0.5712(12) 0.1383(6) 0.6590(8) 0.031(4) Uani 1 1 d . . . C176 C 0.5146(14) 0.1104(8) 0.6002(10) 0.050(5) Uani 1 1 d . . . H176 H 0.4740 0.1291 0.5613 0.059 Uiso 1 1 calc R . . C177 C 0.5182(18) 0.0542(7) 0.5989(11) 0.058(6) Uani 1 1 d . . . H177 H 0.4811 0.0356 0.5588 0.075 Uiso 1 1 calc R . . C178 C 0.5767(15) 0.0262(8) 0.6568(13) 0.064(6) Uani 1 1 d . . . H178 H 0.5754 -0.0113 0.6571 0.082 Uiso 1 1 calc R . . C179 C 0.6377(17) 0.0543(8) 0.7151(11) 0.062(6) Uani 1 1 d . . . H179 H 0.6804 0.0359 0.7534 0.075 Uiso 1 1 calc R . . C180 C 0.6334(15) 0.1101(8) 0.7145(9) 0.048(5) Uani 1 1 d . . . H180 H 0.6740 0.1290 0.7532 0.060 Uiso 1 1 calc R . . B1 B 0.5595(19) 0.4329(9) 1.2031(13) 0.051(6) Uiso 1 1 d . . . H1B H 0.6241 0.4218 1.2376 0.073 Uiso 1 1 calc R . . B2 B -0.1744(14) 0.5070(7) 0.8161(10) 0.033(4) Uiso 1 1 d . . . H2B H -0.2484 0.5110 0.7904 0.044 Uiso 1 1 calc R . . B11 B 0.3310(14) 0.2079(7) 0.3110(9) 0.030(4) Uiso 1 1 d . . . H11B H 0.2615 0.2010 0.2792 0.048 Uiso 1 1 calc R . . B12 B 1.0852(15) 0.3090(8) 0.6953(10) 0.035(4) Uiso 1 1 d . . . H12B H 1.1472 0.3249 0.7277 0.039 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 Dy1 0.0252(3) 0.0231(4) 0.0189(3) -0.0002(3) -0.0007(3) 0.0004(3) Dy2 0.0222(3) 0.0235(4) 0.0193(3) 0.0012(3) 0.0000(3) -0.0004(3) Dy11 0.0201(3) 0.0266(4) 0.0241(3) 0.0025(3) 0.0012(3) 0.0018(3) Dy12 0.0244(3) 0.0266(4) 0.0221(3) -0.0013(3) -0.0034(3) 0.0006(3) O1 0.026(5) 0.038(6) 0.021(5) -0.007(5) 0.001(4) 0.001(5) O2 0.030(5) 0.059(8) 0.014(5) -0.010(5) -0.002(4) 0.009(6) O3 0.044(6) 0.029(6) 0.025(5) -0.005(5) 0.017(5) -0.009(5) O4 0.036(6) 0.048(8) 0.014(5) 0.000(5) -0.003(4) -0.001(5) O5 0.027(6) 0.032(6) 0.023(6) -0.001(5) -0.008(5) -0.009(5) O6 0.037(6) 0.011(5) 0.018(5) 0.001(4) -0.001(4) 0.003(4) O7 0.037(6) 0.012(5) 0.040(7) -0.001(5) -0.006(5) 0.000(4) O8 0.032(6) 0.017(5) 0.035(6) 0.010(5) -0.017(5) 0.000(4) O11 0.033(6) 0.039(7) 0.042(7) 0.004(5) 0.000(5) 0.012(5) O12 0.034(6) 0.061(9) 0.030(6) -0.006(6) -0.002(5) -0.006(6) O13 0.041(7) 0.042(8) 0.062(9) 0.024(7) 0.003(6) 0.014(6) O14 0.034(7) 0.035(7) 0.082(10) -0.017(7) -0.009(7) -0.003(5) O15 0.012(4) 0.066(8) 0.031(6) -0.009(6) -0.004(4) -0.004(5) O16 0.028(5) 0.054(7) 0.021(5) -0.009(5) 0.007(4) -0.006(5) O17 0.025(5) 0.041(6) 0.019(5) 0.009(5) 0.008(4) 0.008(5) O18 0.022(5) 0.043(7) 0.032(6) -0.003(5) 0.004(4) -0.003(5) N11 0.020(6) 0.033(7) 0.052(8) -0.022(7) -0.017(6) -0.002(6) N12 0.021(6) 0.026(7) 0.063(10) 0.009(7) -0.002(6) -0.003(5) N16 0.027(6) 0.025(7) 0.043(7) -0.002(7) -0.002(6) 0.001(6) N17 0.042(7) 0.018(7) 0.022(6) 0.009(5) 0.006(5) 0.005(6) N21 0.035(7) 0.036(8) 0.037(8) 0.013(6) 0.002(6) 0.021(6) N22 0.018(6) 0.041(8) 0.025(7) 0.004(6) -0.008(5) 0.012(5) N26 0.037(7) 0.033(8) 0.035(7) 0.006(6) 0.010(6) -0.005(6) N27 0.034(7) 0.027(7) 0.023(7) 0.012(5) -0.008(6) -0.008(5) N31 0.054(10) 0.027(8) 0.047(10) 0.006(7) -0.007(8) 0.007(7) N32 0.026(7) 0.025(7) 0.043(8) 0.002(6) -0.009(6) 0.010(5) N36 0.018(6) 0.034(8) 0.033(8) -0.001(6) -0.006(5) 0.015(5) N37 0.021(6) 0.036(8) 0.030(7) 0.003(6) -0.017(6) -0.002(6) N111 0.012(6) 0.040(9) 0.034(8) 0.012(6) -0.008(5) 0.001(5) N112 0.026(7) 0.035(8) 0.036(8) 0.001(6) -0.006(6) 0.015(6) N116 0.052(8) 0.037(8) 0.033(7) -0.008(7) -0.001(6) -0.008(7) N117 0.021(6) 0.048(9) 0.028(7) 0.007(6) -0.018(5) 0.012(6) N121 0.020(6) 0.034(8) 0.032(7) 0.002(6) -0.007(5) 0.004(6) N122 0.020(6) 0.040(8) 0.030(7) 0.003(6) 0.016(5) 0.000(5) N126 0.031(7) 0.059(10) 0.021(7) 0.002(7) -0.003(6) -0.012(7) N127 0.053(9) 0.039(8) 0.012(6) -0.004(6) 0.012(6) 0.001(7) N131 0.030(6) 0.047(9) 0.018(6) 0.004(6) 0.001(5) -0.009(6) N132 0.013(5) 0.028(7) 0.022(6) 0.003(5) 0.001(4) 0.003(5) N136 0.048(8) 0.036(8) 0.005(6) 0.005(5) -0.003(5) -0.012(6) N137 0.043(8) 0.028(8) 0.016(6) 0.000(5) -0.005(6) -0.001(6) C1 0.025(8) 0.019(8) 0.033(9) -0.007(7) 0.009(7) 0.002(6) C2 0.032(9) 0.047(10) 0.037(10) 0.008(8) 0.017(7) 0.018(8) C3 0.049(11) 0.10(2) 0.057(12) -0.010(13) 0.027(10) -0.009(13) C4 0.050(13) 0.21(3) 0.104(19) 0.01(2) 0.046(13) -0.063(18) C5 0.027(8) 0.045(10) 0.021(8) -0.009(7) 0.004(6) 0.010(7) C6 0.040(10) 0.080(16) 0.043(11) 0.000(11) 0.005(9) -0.004(10) C7 0.11(2) 0.047(15) 0.10(2) -0.005(14) 0.013(18) 0.028(14) C8 0.060(14) 0.043(12) 0.101(19) -0.024(13) 0.025(13) -0.004(10) C9 0.069(14) 0.057(14) 0.064(14) -0.020(11) -0.014(11) 0.021(11) C10 0.047(11) 0.065(14) 0.038(11) -0.030(10) -0.015(9) 0.020(10) C13 0.041(10) 0.061(13) 0.023(9) 0.013(8) -0.005(8) -0.001(9) C14 0.073(16) 0.068(16) 0.071(16) -0.001(13) -0.026(13) -0.016(12) C18 0.036(8) 0.042(10) 0.038(9) -0.020(8) 0.026(7) -0.015(7) C20 0.049(9) 0.033(9) 0.020(7) -0.010(7) -0.002(7) 0.000(8) C23 0.062(12) 0.041(11) 0.028(9) 0.004(8) 0.014(9) -0.011(9) C24 0.065(12) 0.025(9) 0.015(8) 0.007(6) 0.005(8) 0.011(8) C25 0.074(13) 0.023(9) 0.017(8) -0.007(7) -0.003(8) 0.008(8) C28 0.055(11) 0.039(10) 0.034(10) 0.012(8) 0.023(9) 0.007(8) C29 0.062(14) 0.075(15) 0.052(13) 0.016(11) 0.021(11) -0.020(12) C30 0.031(9) 0.058(12) 0.043(11) 0.003(9) 0.005(8) -0.008(8) C33 0.058(11) 0.023(9) 0.031(9) -0.007(7) 0.013(8) 0.013(8) C34 0.042(10) 0.042(11) 0.042(10) -0.001(8) 0.003(8) -0.002(8) C35 0.018(7) 0.045(11) 0.047(11) 0.022(8) 0.009(7) 0.001(7) C38 0.045(10) 0.029(10) 0.043(10) 0.005(8) 0.014(8) 0.020(8) C39 0.049(12) 0.045(12) 0.057(13) -0.008(10) 0.016(10) 0.004(9) C40 0.036(9) 0.042(10) 0.036(10) 0.016(8) 0.013(8) 0.011(8) C41 0.037(8) 0.027(9) 0.019(7) -0.005(7) 0.015(6) 0.004(7) C42 0.031(8) 0.043(9) 0.023(7) 0.006(7) 0.014(6) 0.002(7) C43 0.040(10) 0.065(13) 0.039(10) 0.012(9) 0.016(8) 0.009(9) C44 0.045(11) 0.058(13) 0.047(12) -0.018(10) 0.017(9) -0.004(9) C45 0.046(10) 0.025(9) 0.034(9) 0.004(7) 0.005(8) 0.021(7) C46 0.060(13) 0.048(12) 0.060(13) 0.002(10) 0.029(11) 0.001(10) C47 0.039(12) 0.088(19) 0.11(2) -0.052(17) 0.025(13) 0.001(12) C48 0.068(16) 0.068(17) 0.10(2) -0.012(16) 0.044(16) -0.019(13) C49 0.086(17) 0.031(11) 0.10(2) 0.017(12) 0.057(16) 0.003(11) C50 0.051(12) 0.036(11) 0.070(14) -0.006(10) 0.011(10) 0.001(9) C51 0.020(7) 0.030(9) 0.014(7) -0.001(6) -0.004(6) 0.002(6) C52 0.034(8) 0.038(10) 0.021(8) 0.009(7) -0.002(7) 0.006(7) C53 0.077(13) 0.015(8) 0.040(10) -0.005(7) 0.013(9) 0.004(8) C54 0.062(13) 0.054(12) 0.068(14) -0.017(10) 0.028(11) 0.006(10) C55 0.038(9) 0.015(8) 0.033(9) 0.011(6) 0.012(7) -0.002(6) C56 0.057(12) 0.049(12) 0.028(10) 0.009(8) 0.017(9) -0.008(9) C57 0.069(14) 0.079(16) 0.034(11) -0.007(10) 0.015(10) -0.020(12) C58 0.071(15) 0.046(13) 0.081(16) -0.013(11) 0.039(13) -0.025(11) C59 0.075(14) 0.069(15) 0.047(12) -0.005(11) 0.028(11) -0.037(12) C60 0.053(11) 0.035(10) 0.030(9) -0.007(8) -0.006(8) -0.008(8) C71 0.023(8) 0.033(9) 0.026(8) 0.003(7) -0.003(6) 0.019(7) C72 0.032(8) 0.008(7) 0.041(9) 0.007(7) 0.009(7) 0.004(6) C73 0.040(9) 0.023(9) 0.039(10) 0.006(7) -0.005(8) 0.005(7) C74 0.050(11) 0.052(13) 0.059(12) 0.020(10) 0.000(9) -0.011(9) C75 0.020(7) 0.006(7) 0.048(10) 0.009(6) 0.012(7) -0.001(5) C76 0.037(9) 0.047(10) 0.044(10) -0.016(8) 0.010(8) -0.023(8) C77 0.074(13) 0.061(14) 0.045(11) -0.011(11) -0.008(10) -0.020(12) C78 0.064(12) 0.056(12) 0.035(9) -0.014(9) 0.019(9) -0.027(10) C79 0.051(10) 0.048(11) 0.043(10) -0.009(9) 0.014(8) 0.009(9) C80 0.040(9) 0.009(7) 0.064(12) -0.002(7) -0.016(8) 0.007(6) C101 0.016(6) 0.015(7) 0.020(7) 0.010(6) -0.002(6) 0.001(5) C102 0.024(8) 0.032(9) 0.040(10) -0.012(7) 0.003(7) -0.006(6) C103 0.038(9) 0.032(9) 0.046(11) 0.012(8) 0.020(8) 0.003(7) C104 0.040(9) 0.051(11) 0.052(11) 0.021(10) 0.008(8) -0.013(9) C105 0.038(9) 0.034(10) 0.050(11) 0.000(8) 0.005(8) 0.013(7) C106 0.021(8) 0.059(12) 0.043(11) 0.016(9) 0.006(7) 0.011(8) C107 0.099(17) 0.039(11) 0.039(11) 0.015(9) 0.044(12) 0.005(11) C108 0.065(14) 0.034(12) 0.089(18) -0.018(11) 0.007(13) 0.014(10) C109 0.048(12) 0.065(15) 0.056(14) -0.008(11) 0.004(10) 0.008(10) C110 0.057(11) 0.024(9) 0.043(10) 0.011(8) 0.018(9) 0.011(8) C113 0.028(8) 0.036(10) 0.044(10) 0.012(8) -0.010(7) 0.010(7) C114 0.039(10) 0.022(9) 0.088(15) 0.018(9) -0.006(10) -0.017(8) C115 0.047(11) 0.040(11) 0.040(11) -0.007(8) 0.000(8) -0.019(9) C118 0.042(11) 0.049(12) 0.075(15) -0.006(10) -0.024(10) 0.032(10) C119 0.058(14) 0.049(14) 0.13(2) -0.011(14) -0.044(14) 0.024(11) C120 0.037(11) 0.093(19) 0.099(17) -0.008(14) -0.032(11) 0.043(12) C123 0.021(8) 0.051(11) 0.046(11) 0.007(9) 0.009(7) -0.001(7) C124 0.017(7) 0.075(14) 0.045(11) 0.010(10) 0.023(7) 0.019(8) C125 0.018(7) 0.056(11) 0.035(9) -0.012(8) 0.010(7) -0.003(7) C128 0.065(12) 0.044(11) 0.009(7) 0.004(7) -0.008(7) -0.015(9) C129 0.069(13) 0.032(10) 0.035(10) 0.005(8) 0.026(9) -0.006(9) C130 0.054(12) 0.038(11) 0.055(12) 0.002(9) 0.013(10) -0.018(9) C133 0.025(7) 0.030(8) 0.017(7) -0.001(6) 0.007(6) -0.001(6) C134 0.036(9) 0.050(11) 0.026(9) 0.002(8) 0.009(7) 0.012(8) C135 0.040(8) 0.041(10) 0.020(7) -0.005(7) -0.013(6) -0.005(8) C138 0.032(8) 0.040(10) 0.032(9) 0.011(7) 0.014(7) 0.018(7) C139 0.073(14) 0.041(11) 0.020(9) -0.005(8) 0.007(9) -0.001(10) C140 0.076(14) 0.023(9) 0.021(9) 0.000(7) -0.013(8) -0.024(9) C141 0.038(9) 0.024(9) 0.033(10) 0.003(7) -0.014(8) 0.011(7) C142 0.035(9) 0.051(12) 0.031(9) -0.004(8) -0.020(7) 0.015(8) C143 0.073(14) 0.025(10) 0.066(14) 0.002(9) 0.025(11) 0.010(9) C144 0.13(3) 0.048(16) 0.12(2) -0.023(15) 0.006(19) 0.009(15) C145 0.042(10) 0.020(9) 0.044(10) -0.005(7) 0.009(8) 0.008(7) C146 0.040(10) 0.039(10) 0.066(13) -0.019(10) 0.021(9) -0.006(8) C147 0.15(3) 0.08(2) 0.049(13) 0.042(14) 0.021(16) 0.005(19) C148 0.11(2) 0.10(2) 0.041(13) 0.026(14) 0.000(14) 0.029(19) C149 0.075(15) 0.066(15) 0.067(15) -0.019(12) -0.016(12) 0.052(12) C150 0.070(13) 0.054(12) 0.028(9) -0.002(9) 0.012(9) 0.023(10) C151 0.031(7) 0.019(8) 0.022(7) -0.002(6) 0.014(6) 0.014(6) C152 0.041(8) 0.048(11) 0.022(7) 0.007(8) 0.010(7) -0.019(8) C153 0.032(9) 0.058(12) 0.038(10) 0.026(9) 0.019(8) 0.015(8) C154 0.062(13) 0.067(15) 0.061(14) 0.016(11) 0.022(11) 0.001(11) C155 0.062(12) 0.028(9) 0.041(11) -0.015(8) 0.025(9) -0.009(8) C156 0.083(15) 0.037(11) 0.046(11) -0.006(9) 0.045(11) 0.000(10) C157 0.085(17) 0.057(14) 0.069(15) -0.022(12) 0.060(14) 0.006(12) C158 0.067(15) 0.063(15) 0.087(18) 0.018(14) 0.032(14) 0.041(12) C159 0.038(11) 0.036(11) 0.089(16) 0.004(11) 0.007(10) 0.003(8) C160 0.022(8) 0.062(12) 0.031(9) -0.009(8) 0.002(7) -0.015(8) C171 0.037(9) 0.017(9) 0.032(9) 0.007(6) 0.003(7) 0.009(6) C172 0.052(11) 0.039(10) 0.024(9) -0.006(7) -0.010(8) 0.003(8) C173 0.034(9) 0.067(15) 0.071(14) 0.001(11) 0.016(9) -0.013(9) C174 0.090(17) 0.080(16) 0.060(14) 0.001(12) 0.058(13) 0.028(13) C175 0.039(9) 0.033(9) 0.015(7) 0.008(7) -0.003(7) -0.003(7) C176 0.041(10) 0.050(12) 0.053(12) 0.009(10) 0.000(9) -0.003(9) C177 0.087(16) 0.031(11) 0.048(12) -0.020(9) 0.000(11) -0.018(10) C178 0.049(12) 0.032(11) 0.113(19) 0.001(11) 0.022(12) 0.003(9) C179 0.075(14) 0.043(12) 0.051(12) 0.001(9) -0.020(11) -0.025(10) C180 0.063(12) 0.057(13) 0.020(9) 0.000(8) 0.001(8) -0.016(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 Dy1 O3 2.308(9) . ? Dy1 O5 2.311(10) . ? Dy1 O7 2.306(10) . ? Dy1 O2 2.378(10) . ? Dy1 N22 2.456(12) . ? Dy1 N12 2.469(13) . ? Dy1 N32 2.500(12) . ? Dy1 O1 2.593(9) . ? Dy2 O1 2.237(9) . ? Dy2 O8 2.255(10) . ? Dy2 O6 2.333(9) . ? Dy2 O4 2.368(10) . ? Dy2 N17 2.462(11) . ? Dy2 N27 2.488(12) . ? Dy2 N37 2.496(13) . ? Dy2 O3 2.731(10) . ? Dy11 O17 2.287(9) . ? Dy11 O13 2.291(11) . ? Dy11 O15 2.304(9) . ? Dy11 O12 2.361(14) . ? Dy11 N112 2.470(14) . ? Dy11 N122 2.497(12) . ? Dy11 N132 2.511(10) . ? Dy11 O11 2.736(11) . ? Dy12 O16 2.262(9) . ? Dy12 O11 2.268(10) . ? Dy12 O18 2.294(10) . ? Dy12 O14 2.308(12) . ? Dy12 N117 2.459(11) . ? Dy12 N137 2.498(12) . ? Dy12 N127 2.493(14) . ? O1 C1 1.278(16) . ? O2 C1 1.232(16) . ? O3 C41 1.276(15) . ? O4 C41 1.259(16) . ? O5 C51 1.265(16) . ? O6 C51 1.266(16) . ? O7 C71 1.296(17) . ? O8 C71 1.251(17) . ? O11 C101 1.239(16) . ? O12 C101 1.248(16) . ? O13 C141 1.253(18) . ? O14 C141 1.240(18) . ? O15 C151 1.279(15) . ? O16 C151 1.236(15) . ? O17 C171 1.234(16) . ? O18 C171 1.255(17) . ? N11 C15 1.32(2) . ? N11 N12 1.328(17) . ? N11 B1 1.54(3) . ? N12 C13 1.34(2) . ? N16 C20 1.345(17) . ? N16 N17 1.349(16) . ? N16 B2 1.51(2) . ? N17 C18 1.307(17) . ? N21 N22 1.339(16) . ? N21 C25 1.36(2) . ? N21 B1 1.51(3) . ? N22 C23 1.33(2) . ? N26 C30 1.35(2) . ? N26 N27 1.361(16) . ? N26 B2 1.48(2) . ? N27 C28 1.344(19) . ? N31 N32 1.343(18) . ? N31 C35 1.36(2) . ? N31 B1 1.54(3) . ? N32 C33 1.312(19) . ? N36 C40 1.32(2) . ? N36 N37 1.353(15) . ? N36 B2 1.55(2) . ? N37 C38 1.36(2) . ? N111 C115 1.32(2) . ? N111 N112 1.373(16) . ? N111 B11 1.55(2) . ? N112 C113 1.32(2) . ? N116 C120 1.32(2) . ? N116 N117 1.357(17) . ? N116 B12 1.53(2) . ? N117 C118 1.35(2) . ? N121 N122 1.360(16) . ? N121 C125 1.353(18) . ? N121 B11 1.50(2) . ? N122 C123 1.33(2) . ? N126 C130 1.36(2) . ? N126 N127 1.380(17) . ? N126 B12 1.53(2) . ? N127 C128 1.321(19) . ? N131 C135 1.363(18) . ? N131 N132 1.385(14) . ? N131 B11 1.51(2) . ? N132 C133 1.327(17) . ? N136 C140 1.33(2) . ? N136 N137 1.374(17) . ? N136 B12 1.51(2) . ? N137 C138 1.327(19) . ? C1 C2 1.543(19) . ? C2 C3 1.47(2) . ? C2 C5 1.54(2) . ? C2 H2C 0.9800 . ? C3 C4 1.55(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.40(2) . ? C5 C6 1.41(2) . ? C6 C7 1.38(3) . ? C6 H6 0.9300 . ? C7 C8 1.39(3) . ? C7 H7 0.9300 . ? C8 C9 1.35(3) . ? C8 H8 0.9300 . ? C9 C10 1.32(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C13 C14 1.41(3) . ? C13 H13 0.9300 . ? C14 C15 1.33(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C18 C19 1.41(2) . ? C18 H18 0.9300 . ? C19 C20 1.36(2) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C23 C24 1.39(2) . ? C23 H23 0.9300 . ? C24 C25 1.35(2) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C28 C29 1.44(3) . ? C28 H28 0.9300 . ? C29 C30 1.35(3) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C33 C34 1.39(2) . ? C33 H33 0.9300 . ? C34 C35 1.37(2) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C38 C39 1.37(2) . ? C38 H38 0.9300 . ? C39 C40 1.39(3) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.496(19) . ? C42 C45 1.50(2) . ? C42 C43 1.55(2) . ? C42 H42 0.9800 . ? C43 C44 1.45(3) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C50 1.38(2) . ? C45 C46 1.40(3) . ? C46 C47 1.43(3) . ? C46 H46 0.9300 . ? C47 C48 1.44(3) . ? C47 H47 0.9300 . ? C48 C49 1.39(3) . ? C48 H48 0.9300 . ? C49 C50 1.40(3) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C52 1.49(2) . ? C52 C55 1.50(2) . ? C52 C53 1.54(2) . ? C52 H52 0.9800 . ? C53 C54 1.52(2) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.34(2) . ? C55 C60 1.39(2) . ? C56 C57 1.35(2) . ? C56 H56 0.9300 . ? C57 C58 1.42(3) . ? C57 H57 0.9300 . ? C58 C59 1.40(3) . ? C58 H58 0.9300 . ? C59 C60 1.39(2) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C71 C72 1.53(2) . ? C72 C75 1.49(2) . ? C72 C73 1.51(2) . ? C72 H72 0.9800 . ? C73 C74 1.52(2) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 C76 1.39(2) . ? C75 C80 1.41(2) . ? C76 C77 1.35(2) . ? C76 H76 0.9300 . ? C77 C78 1.38(3) . ? C77 H77 0.9300 . ? C78 C79 1.39(2) . ? C78 H78 0.9300 . ? C79 C80 1.43(2) . ? C79 H79 0.9300 . ? C80 H80 0.9300 . ? C101 C102 1.55(2) . ? C102 C105 1.49(2) . ? C102 C103 1.50(2) . ? C102 H102 0.9800 . ? C103 C104 1.53(2) . ? C103 H103 0.9700 . ? C103 H203 0.9700 . ? C104 H104 0.9600 . ? C104 H204 0.9600 . ? C104 H304 0.9600 . ? C105 C110 1.40(2) . ? C105 C106 1.42(2) . ? C106 C107 1.36(2) . ? C106 H106 0.9300 . ? C107 C108 1.34(3) . ? C107 H107 0.9300 . ? C108 C109 1.37(3) . ? C108 H108 0.9300 . ? C109 C110 1.36(3) . ? C109 H109 0.9300 . ? C110 H110 0.9300 . ? C113 C114 1.34(2) . ? C113 H113 0.9300 . ? C114 C115 1.34(2) . ? C114 H114 0.9300 . ? C115 H115 0.9300 . ? C118 C119 1.41(3) . ? C118 H118 0.9300 . ? C119 C120 1.37(3) . ? C119 H119 0.9300 . ? C120 H120 0.9300 . ? C123 C124 1.38(2) . ? C123 H123 0.9300 . ? C124 C125 1.34(2) . ? C124 H124 0.9300 . ? C125 H125 0.9300 . ? C128 C129 1.38(2) . ? C128 H128 0.9300 . ? C129 C130 1.39(2) . ? C129 H129 0.9300 . ? C130 H130 0.9300 . ? C133 C134 1.363(19) . ? C133 H133 0.9300 . ? C134 C135 1.38(2) . ? C134 H134 0.9300 . ? C135 H135 0.9300 . ? C138 C139 1.37(2) . ? C138 H138 0.9300 . ? C139 C140 1.36(3) . ? C139 H139 0.9300 . ? C140 H140 0.9300 . ? C141 C142 1.53(2) . ? C142 C145 1.54(2) . ? C142 C143 1.55(2) . ? C142 H142 0.9800 . ? C143 C144 1.46(3) . ? C143 H143 0.9700 . ? C143 H243 0.9700 . ? C144 H144 0.9600 . ? C144 H244 0.9600 . ? C144 H344 0.9600 . ? C145 C150 1.37(2) . ? C145 C146 1.37(2) . ? C146 C147 1.41(3) . ? C146 H146 0.9300 . ? C147 C148 1.32(3) . ? C147 H147 0.9300 . ? C148 C149 1.34(3) . ? C148 H148 0.9300 . ? C149 C150 1.41(3) . ? C149 H149 0.9300 . ? C150 H150 0.9300 . ? C151 C152 1.524(18) . ? C152 C153 1.50(2) . ? C152 C155 1.55(2) . ? C152 H152 0.9800 . ? C153 C154 1.57(2) . ? C153 H153 0.9700 . ? C153 H253 0.9700 . ? C154 H154 0.9600 . ? C154 H254 0.9600 . ? C154 H354 0.9600 . ? C155 C156 1.34(2) . ? C155 C160 1.39(2) . ? C156 C157 1.43(3) . ? C156 H156 0.9300 . ? C157 C158 1.33(3) . ? C157 H157 0.9300 . ? C158 C159 1.35(3) . ? C158 H158 0.9300 . ? C159 C160 1.39(2) . ? C159 H159 0.9300 . ? C160 H160 0.9300 . ? C171 C172 1.50(2) . ? C172 C173 1.53(2) . ? C172 C175 1.54(2) . ? C172 H172 0.9800 . ? C173 C174 1.47(3) . ? C173 H173 0.9700 . ? C173 H273 0.9700 . ? C174 H174 0.9600 . ? C174 H274 0.9600 . ? C174 H374 0.9600 . ? C175 C180 1.37(2) . ? C175 C176 1.38(2) . ? C176 C177 1.40(2) . ? C176 H176 0.9300 . ? C177 C178 1.38(3) . ? C177 H177 0.9300 . ? C178 C179 1.40(3) . ? C178 H178 0.9300 . ? C179 C180 1.39(3) . ? C179 H179 0.9300 . ? C180 H180 0.9300 . ? B1 H1B 0.9800 . ? B2 H2B 0.9800 . ? B11 H11B 0.9800 . ? B12 H12B 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 O3 Dy1 O5 75.5(4) . . ? O3 Dy1 O7 74.9(4) . . ? O5 Dy1 O7 137.5(4) . . ? O3 Dy1 O2 129.6(3) . . ? O5 Dy1 O2 92.5(4) . . ? O7 Dy1 O2 83.6(4) . . ? O3 Dy1 N22 150.2(4) . . ? O5 Dy1 N22 83.9(4) . . ? O7 Dy1 N22 133.3(4) . . ? O2 Dy1 N22 71.8(4) . . ? O3 Dy1 N12 113.0(4) . . ? O5 Dy1 N12 146.8(4) . . ? O7 Dy1 N12 73.9(4) . . ? O2 Dy1 N12 103.5(4) . . ? N22 Dy1 N12 74.2(4) . . ? O3 Dy1 N32 80.6(4) . . ? O5 Dy1 N32 76.4(4) . . ? O7 Dy1 N32 127.0(4) . . ? O2 Dy1 N32 144.6(4) . . ? N22 Dy1 N32 73.7(4) . . ? N12 Dy1 N32 73.8(4) . . ? O3 Dy1 O1 78.2(3) . . ? O5 Dy1 O1 71.8(4) . . ? O7 Dy1 O1 72.8(4) . . ? O2 Dy1 O1 51.8(3) . . ? N22 Dy1 O1 115.7(4) . . ? N12 Dy1 O1 140.3(4) . . ? N32 Dy1 O1 145.2(4) . . ? O1 Dy2 O8 78.3(4) . . ? O1 Dy2 O6 80.7(4) . . ? O8 Dy2 O6 136.0(4) . . ? O1 Dy2 O4 126.5(3) . . ? O8 Dy2 O4 78.4(4) . . ? O6 Dy2 O4 83.9(4) . . ? O1 Dy2 N17 153.6(4) . . ? O8 Dy2 N17 120.0(4) . . ? O6 Dy2 N17 94.7(4) . . ? O4 Dy2 N17 78.3(3) . . ? O1 Dy2 N27 80.3(4) . . ? O8 Dy2 N27 137.5(4) . . ? O6 Dy2 N27 74.6(4) . . ? O4 Dy2 N27 142.5(4) . . ? N17 Dy2 N27 73.5(4) . . ? O1 Dy2 N37 95.2(4) . . ? O8 Dy2 N37 72.7(4) . . ? O6 Dy2 N37 147.8(4) . . ? O4 Dy2 N37 122.1(4) . . ? N17 Dy2 N37 74.9(4) . . ? N27 Dy2 N37 73.2(4) . . ? O1 Dy2 O3 76.4(3) . . ? O8 Dy2 O3 68.8(3) . . ? O6 Dy2 O3 69.0(3) . . ? O4 Dy2 O3 50.3(3) . . ? N17 Dy2 O3 126.3(3) . . ? N27 Dy2 O3 139.2(3) . . ? N37 Dy2 O3 141.5(4) . . ? O17 Dy11 O13 76.7(4) . . ? O17 Dy11 O15 137.4(3) . . ? O13 Dy11 O15 75.6(4) . . ? O17 Dy11 O12 93.7(4) . . ? O13 Dy11 O12 132.6(4) . . ? O15 Dy11 O12 82.1(4) . . ? O17 Dy11 N112 91.4(4) . . ? O13 Dy11 N112 80.3(4) . . ? O15 Dy11 N112 114.8(4) . . ? O12 Dy11 N112 147.0(4) . . ? O17 Dy11 N122 74.9(4) . . ? O13 Dy11 N122 141.5(4) . . ? O15 Dy11 N122 141.9(4) . . ? O12 Dy11 N122 74.9(4) . . ? N112 Dy11 N122 75.0(4) . . ? O17 Dy11 N132 149.1(3) . . ? O13 Dy11 N132 125.6(4) . . ? O15 Dy11 N132 73.1(3) . . ? O12 Dy11 N132 85.1(4) . . ? N112 Dy11 N132 74.3(4) . . ? N122 Dy11 N132 75.0(4) . . ? O17 Dy11 O11 69.1(4) . . ? O13 Dy11 O11 84.9(4) . . ? O15 Dy11 O11 76.7(4) . . ? O12 Dy11 O11 49.2(3) . . ? N112 Dy11 O11 157.8(4) . . ? N122 Dy11 O11 108.2(4) . . ? N132 Dy11 O11 127.9(4) . . ? O16 Dy12 O11 76.0(4) . . ? O16 Dy12 O18 130.4(3) . . ? O11 Dy12 O18 76.5(4) . . ? O16 Dy12 O14 79.7(5) . . ? O11 Dy12 O14 122.5(4) . . ? O18 Dy12 O14 81.5(4) . . ? O16 Dy12 N117 100.7(4) . . ? O11 Dy12 N117 161.2(4) . . ? O18 Dy12 N117 117.4(4) . . ? O14 Dy12 N117 74.0(4) . . ? O16 Dy12 N137 148.8(4) . . ? O11 Dy12 N137 97.5(4) . . ? O18 Dy12 N137 75.3(4) . . ? O14 Dy12 N137 126.9(5) . . ? N117 Dy12 N137 75.6(4) . . ? O16 Dy12 N127 76.2(4) . . ? O11 Dy12 N127 85.7(4) . . ? O18 Dy12 N127 140.8(4) . . ? O14 Dy12 N127 136.5(5) . . ? N117 Dy12 N127 75.6(5) . . ? N137 Dy12 N127 72.8(4) . . ? C1 O1 Dy2 164.9(9) . . ? C1 O1 Dy1 88.1(8) . . ? Dy2 O1 Dy1 105.8(4) . . ? C1 O2 Dy1 99.5(8) . . ? C41 O3 Dy1 170.2(10) . . ? C41 O3 Dy2 86.1(8) . . ? Dy1 O3 Dy2 99.6(3) . . ? C41 O4 Dy2 103.7(8) . . ? C51 O5 Dy1 139.5(10) . . ? C51 O6 Dy2 134.9(9) . . ? C71 O7 Dy1 133.4(10) . . ? C71 O8 Dy2 139.6(10) . . ? C101 O11 Dy12 163.6(10) . . ? C101 O11 Dy11 86.7(8) . . ? Dy12 O11 Dy11 104.2(4) . . ? C101 O12 Dy11 104.7(10) . . ? C141 O13 Dy11 168.5(12) . . ? C141 O14 Dy12 114.8(11) . . ? C151 O15 Dy11 133.4(9) . . ? C151 O16 Dy12 146.8(9) . . ? C171 O17 Dy11 138.9(9) . . ? C171 O18 Dy12 139.5(10) . . ? C15 N11 N12 112.3(15) . . ? C15 N11 B1 128.1(16) . . ? N12 N11 B1 119.3(14) . . ? N11 N12 C13 104.8(13) . . ? N11 N12 Dy1 125.6(9) . . ? C13 N12 Dy1 129.1(10) . . ? C20 N16 N17 107.6(12) . . ? C20 N16 B2 130.4(13) . . ? N17 N16 B2 122.0(12) . . ? C18 N17 N16 109.0(12) . . ? C18 N17 Dy2 127.4(10) . . ? N16 N17 Dy2 123.6(9) . . ? N22 N21 C25 108.7(14) . . ? N22 N21 B1 121.2(14) . . ? C25 N21 B1 130.0(15) . . ? C23 N22 N21 105.2(13) . . ? C23 N22 Dy1 129.9(11) . . ? N21 N22 Dy1 124.2(10) . . ? C30 N26 N27 109.0(13) . . ? C30 N26 B2 130.2(14) . . ? N27 N26 B2 120.8(13) . . ? C28 N27 N26 107.8(13) . . ? C28 N27 Dy2 128.2(11) . . ? N26 N27 Dy2 124.0(9) . . ? N32 N31 C35 108.1(14) . . ? N32 N31 B1 121.4(15) . . ? C35 N31 B1 130.4(16) . . ? C33 N32 N31 106.6(13) . . ? C33 N32 Dy1 130.6(11) . . ? N31 N32 Dy1 122.8(10) . . ? C40 N36 N37 109.6(14) . . ? C40 N36 B2 129.9(14) . . ? N37 N36 B2 120.3(12) . . ? N36 N37 C38 106.6(13) . . ? N36 N37 Dy2 123.8(10) . . ? C38 N37 Dy2 129.6(10) . . ? C115 N111 N112 109.8(14) . . ? C115 N111 B11 129.0(14) . . ? N112 N111 B11 121.2(13) . . ? C113 N112 N111 104.3(13) . . ? C113 N112 Dy11 131.4(10) . . ? N111 N112 Dy11 124.3(10) . . ? C120 N116 N117 110.4(16) . . ? C120 N116 B12 127.8(16) . . ? N117 N116 B12 121.6(13) . . ? C118 N117 N116 106.6(13) . . ? C118 N117 Dy12 129.2(11) . . ? N116 N117 Dy12 124.3(10) . . ? N122 N121 C125 106.3(12) . . ? N122 N121 B11 124.7(12) . . ? C125 N121 B11 128.9(13) . . ? C123 N122 N121 108.9(12) . . ? C123 N122 Dy11 129.2(10) . . ? N121 N122 Dy11 121.7(9) . . ? C130 N126 N127 108.2(14) . . ? C130 N126 B12 129.2(15) . . ? N127 N126 B12 122.5(14) . . ? C128 N127 N126 106.2(13) . . ? C128 N127 Dy12 131.0(11) . . ? N126 N127 Dy12 121.6(10) . . ? C135 N131 N132 106.9(11) . . ? C135 N131 B11 127.4(13) . . ? N132 N131 B11 125.6(11) . . ? C133 N132 N131 107.3(10) . . ? C133 N132 Dy11 132.1(9) . . ? N131 N132 Dy11 119.7(8) . . ? C140 N136 N137 106.4(14) . . ? C140 N136 B12 130.1(15) . . ? N137 N136 B12 123.5(13) . . ? C138 N137 N136 108.2(12) . . ? C138 N137 Dy12 130.4(11) . . ? N136 N137 Dy12 121.5(9) . . ? O2 C1 O1 120.6(12) . . ? O2 C1 C2 121.7(13) . . ? O1 C1 C2 117.6(13) . . ? C3 C2 C5 112.3(15) . . ? C3 C2 C1 110.2(14) . . ? C5 C2 C1 109.4(13) . . ? C3 C2 H2C 108.3 . . ? C5 C2 H2C 108.3 . . ? C1 C2 H2C 108.3 . . ? C2 C3 C4 113.0(19) . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 116.7(16) . . ? C10 C5 C2 124.6(15) . . ? C6 C5 C2 118.7(14) . . ? C7 C6 C5 120.1(19) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120(2) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 118(2) . . ? C9 C8 H8 121.0 . . ? C7 C8 H8 121.0 . . ? C10 C9 C8 123(2) . . ? C10 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? C9 C10 C5 121.6(18) . . ? C9 C10 H10 119.2 . . ? C5 C10 H10 119.2 . . ? N12 C13 C14 109.0(17) . . ? N12 C13 H13 125.5 . . ? C14 C13 H13 125.5 . . ? C15 C14 C13 105.3(19) . . ? C15 C14 H14 127.3 . . ? C13 C14 H14 127.3 . . ? N11 C15 C14 108.2(18) . . ? N11 C15 H15 125.9 . . ? C14 C15 H15 125.9 . . ? N17 C18 C19 109.3(14) . . ? N17 C18 H18 125.3 . . ? C19 C18 H18 125.3 . . ? C20 C19 C18 103.8(14) . . ? C20 C19 H19 128.1 . . ? C18 C19 H19 128.1 . . ? N16 C20 C19 110.1(14) . . ? N16 C20 H20 124.9 . . ? C19 C20 H20 124.9 . . ? N22 C23 C24 113.6(17) . . ? N22 C23 H23 123.2 . . ? C24 C23 H23 123.2 . . ? C25 C24 C23 101.4(15) . . ? C25 C24 H24 129.3 . . ? C23 C24 H24 129.3 . . ? C24 C25 N21 111.0(15) . . ? C24 C25 H25 124.5 . . ? N21 C25 H25 124.5 . . ? N27 C28 C29 108.3(16) . . ? N27 C28 H28 125.9 . . ? C29 C28 H28 125.9 . . ? C30 C29 C28 105.0(16) . . ? C30 C29 H29 127.5 . . ? C28 C29 H29 127.5 . . ? N26 C30 C29 109.9(16) . . ? N26 C30 H30 125.1 . . ? C29 C30 H30 125.1 . . ? N32 C33 C34 113.4(16) . . ? N32 C33 H33 123.3 . . ? C34 C33 H33 123.3 . . ? C35 C34 C33 101.4(15) . . ? C35 C34 H34 129.3 . . ? C33 C34 H34 129.3 . . ? N31 C35 C34 110.5(15) . . ? N31 C35 H35 124.8 . . ? C34 C35 H35 124.8 . . ? N37 C38 C39 110.0(17) . . ? N37 C38 H38 125.0 . . ? C39 C38 H38 125.0 . . ? C38 C39 C40 104.6(17) . . ? C38 C39 H39 127.7 . . ? C40 C39 H39 127.7 . . ? N36 C40 C39 109.1(15) . . ? N36 C40 H40 125.5 . . ? C39 C40 H40 125.5 . . ? O4 C41 O3 119.5(13) . . ? O4 C41 C42 122.0(12) . . ? O3 C41 C42 118.5(13) . . ? C41 C42 C45 109.1(13) . . ? C41 C42 C43 112.8(13) . . ? C45 C42 C43 115.9(13) . . ? C41 C42 H42 106.1 . . ? C45 C42 H42 106.1 . . ? C43 C42 H42 106.1 . . ? C44 C43 C42 114.1(14) . . ? C44 C43 H43A 108.7 . . ? C42 C43 H43A 108.7 . . ? C44 C43 H43B 108.7 . . ? C42 C43 H43B 108.7 . . ? H43A C43 H43B 107.6 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 118.0(17) . . ? C50 C45 C42 122.3(16) . . ? C46 C45 C42 119.6(15) . . ? C45 C46 C47 122(2) . . ? C45 C46 H46 119.0 . . ? C47 C46 H46 119.0 . . ? C46 C47 C48 118(2) . . ? C46 C47 H47 121.2 . . ? C48 C47 H47 121.2 . . ? C49 C48 C47 119(2) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C48 C49 C50 120(2) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C45 C50 C49 122(2) . . ? C45 C50 H50 119.0 . . ? C49 C50 H50 119.0 . . ? O5 C51 O6 124.1(14) . . ? O5 C51 C52 118.6(13) . . ? O6 C51 C52 117.1(12) . . ? C51 C52 C55 109.3(13) . . ? C51 C52 C53 112.0(13) . . ? C55 C52 C53 113.6(12) . . ? C51 C52 H52 107.2 . . ? C55 C52 H52 107.2 . . ? C53 C52 H52 107.2 . . ? C54 C53 C52 111.1(14) . . ? C54 C53 H53A 109.4 . . ? C52 C53 H53A 109.4 . . ? C54 C53 H53B 109.4 . . ? C52 C53 H53B 109.4 . . ? H53A C53 H53B 108.0 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 C60 116.6(15) . . ? C56 C55 C52 123.4(15) . . ? C60 C55 C52 119.9(15) . . ? C55 C56 C57 125.5(18) . . ? C55 C56 H56 117.2 . . ? C57 C56 H56 117.2 . . ? C56 C57 C58 119.0(19) . . ? C56 C57 H57 120.5 . . ? C58 C57 H57 120.5 . . ? C59 C58 C57 117.3(19) . . ? C59 C58 H58 121.4 . . ? C57 C58 H58 121.4 . . ? C58 C59 C60 120.2(19) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C55 C60 C59 121.3(16) . . ? C55 C60 H60 119.3 . . ? C59 C60 H60 119.3 . . ? O8 C71 O7 123.8(15) . . ? O8 C71 C72 119.6(13) . . ? O7 C71 C72 116.5(13) . . ? C75 C72 C73 114.4(12) . . ? C75 C72 C71 113.9(12) . . ? C73 C72 C71 111.6(13) . . ? C75 C72 H72 105.3 . . ? C73 C72 H72 105.3 . . ? C71 C72 H72 105.3 . . ? C72 C73 C74 115.1(13) . . ? C72 C73 H73A 108.5 . . ? C74 C73 H73A 108.5 . . ? C72 C73 H73B 108.5 . . ? C74 C73 H73B 108.5 . . ? H73A C73 H73B 107.5 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 C80 117.1(15) . . ? C76 C75 C72 123.3(14) . . ? C80 C75 C72 119.5(13) . . ? C77 C76 C75 122.0(17) . . ? C77 C76 H76 119.0 . . ? C75 C76 H76 119.0 . . ? C76 C77 C78 120.9(18) . . ? C76 C77 H77 119.6 . . ? C78 C77 H77 119.6 . . ? C77 C78 C79 121.3(17) . . ? C77 C78 H78 119.3 . . ? C79 C78 H78 119.3 . . ? C78 C79 C80 117.1(17) . . ? C78 C79 H79 121.5 . . ? C80 C79 H79 121.5 . . ? C75 C80 C79 121.3(15) . . ? C75 C80 H80 119.3 . . ? C79 C80 H80 119.3 . . ? O11 C101 O12 119.4(14) . . ? O11 C101 C102 119.0(13) . . ? O12 C101 C102 121.2(13) . . ? C105 C102 C103 114.9(14) . . ? C105 C102 C101 106.2(12) . . ? C103 C102 C101 113.0(13) . . ? C105 C102 H102 107.5 . . ? C103 C102 H102 107.5 . . ? C101 C102 H102 107.5 . . ? C102 C103 C104 110.6(13) . . ? C102 C103 H103 109.5 . . ? C104 C103 H103 109.5 . . ? C102 C103 H203 109.5 . . ? C104 C103 H203 109.5 . . ? H103 C103 H203 108.1 . . ? C103 C104 H104 109.5 . . ? C103 C104 H204 109.5 . . ? H104 C104 H204 109.5 . . ? C103 C104 H304 109.5 . . ? H104 C104 H304 109.5 . . ? H204 C104 H304 109.5 . . ? C110 C105 C106 115.2(16) . . ? C110 C105 C102 124.6(16) . . ? C106 C105 C102 120.1(14) . . ? C107 C106 C105 121.4(16) . . ? C107 C106 H106 119.3 . . ? C105 C106 H106 119.3 . . ? C108 C107 C106 121.6(19) . . ? C108 C107 H107 119.2 . . ? C106 C107 H107 119.2 . . ? C107 C108 C109 119(2) . . ? C107 C108 H108 120.4 . . ? C109 C108 H108 120.4 . . ? C110 C109 C108 121(2) . . ? C110 C109 H109 119.4 . . ? C108 C109 H109 119.4 . . ? C109 C110 C105 121.5(18) . . ? C109 C110 H110 119.3 . . ? C105 C110 H110 119.3 . . ? N112 C113 C114 111.5(14) . . ? N112 C113 H113 124.2 . . ? C114 C113 H113 124.2 . . ? C115 C114 C113 106.1(15) . . ? C115 C114 H114 126.9 . . ? C113 C114 H114 126.9 . . ? N111 C115 C114 108.2(15) . . ? N111 C115 H115 125.9 . . ? C114 C115 H115 125.9 . . ? N117 C118 C119 108.5(18) . . ? N117 C118 H118 125.7 . . ? C119 C118 H118 125.7 . . ? C120 C119 C118 105.3(18) . . ? C120 C119 H119 127.4 . . ? C118 C119 H119 127.4 . . ? N116 C120 C119 109.1(18) . . ? N116 C120 H120 125.4 . . ? C119 C120 H120 125.4 . . ? N122 C123 C124 108.4(16) . . ? N122 C123 H123 125.8 . . ? C124 C123 H123 125.8 . . ? C125 C124 C123 105.9(15) . . ? C125 C124 H124 127.0 . . ? C123 C124 H124 127.0 . . ? C124 C125 N121 110.2(13) . . ? C124 C125 H125 124.9 . . ? N121 C125 H125 124.9 . . ? N127 C128 C129 112.5(14) . . ? N127 C128 H128 123.8 . . ? C129 C128 H128 123.8 . . ? C128 C129 C130 103.9(14) . . ? C128 C129 H129 128.1 . . ? C130 C129 H129 128.1 . . ? N126 C130 C129 109.1(16) . . ? N126 C130 H130 125.5 . . ? C129 C130 H130 125.5 . . ? N132 C133 C134 111.3(13) . . ? N132 C133 H133 124.4 . . ? C134 C133 H133 124.4 . . ? C133 C134 C135 105.2(14) . . ? C133 C134 H134 127.4 . . ? C135 C134 H134 127.4 . . ? N131 C135 C134 109.2(13) . . ? N131 C135 H135 125.4 . . ? C134 C135 H135 125.4 . . ? N137 C138 C139 109.7(16) . . ? N137 C138 H138 125.2 . . ? C139 C138 H138 125.2 . . ? C138 C139 C140 104.8(15) . . ? C138 C139 H139 127.6 . . ? C140 C139 H139 127.6 . . ? N136 C140 C139 110.9(15) . . ? N136 C140 H140 124.5 . . ? C139 C140 H140 124.5 . . ? O14 C141 O13 123.6(16) . . ? O14 C141 C142 120.0(14) . . ? O13 C141 C142 116.2(14) . . ? C141 C142 C145 111.1(12) . . ? C141 C142 C143 109.1(15) . . ? C145 C142 C143 113.9(14) . . ? C141 C142 H142 107.5 . . ? C145 C142 H142 107.5 . . ? C143 C142 H142 107.5 . . ? C144 C143 C142 113.2(19) . . ? C144 C143 H143 108.9 . . ? C142 C143 H143 108.9 . . ? C144 C143 H243 108.9 . . ? C142 C143 H243 108.9 . . ? H143 C143 H243 107.7 . . ? C143 C144 H144 109.5 . . ? C143 C144 H244 109.5 . . ? H144 C144 H244 109.5 . . ? C143 C144 H344 109.5 . . ? H144 C144 H344 109.5 . . ? H244 C144 H344 109.5 . . ? C150 C145 C146 120.7(17) . . ? C150 C145 C142 122.7(17) . . ? C146 C145 C142 116.6(16) . . ? C145 C146 C147 119.7(19) . . ? C145 C146 H146 120.1 . . ? C147 C146 H146 120.1 . . ? C148 C147 C146 120(2) . . ? C148 C147 H147 120.1 . . ? C146 C147 H147 120.1 . . ? C147 C148 C149 120(2) . . ? C147 C148 H148 120.2 . . ? C149 C148 H148 120.2 . . ? C148 C149 C150 123(2) . . ? C148 C149 H149 118.4 . . ? C150 C149 H149 118.4 . . ? C145 C150 C149 116(2) . . ? C145 C150 H150 121.9 . . ? C149 C150 H150 121.9 . . ? O16 C151 O15 124.4(12) . . ? O16 C151 C152 120.1(12) . . ? O15 C151 C152 115.4(12) . . ? C153 C152 C151 108.9(14) . . ? C153 C152 C155 111.1(12) . . ? C151 C152 C155 112.7(12) . . ? C153 C152 H152 108.0 . . ? C151 C152 H152 108.0 . . ? C155 C152 H152 108.0 . . ? C152 C153 C154 111.6(14) . . ? C152 C153 H153 109.3 . . ? C154 C153 H153 109.3 . . ? C152 C153 H253 109.3 . . ? C154 C153 H253 109.3 . . ? H153 C153 H253 108.0 . . ? C153 C154 H154 109.5 . . ? C153 C154 H254 109.5 . . ? H154 C154 H254 109.5 . . ? C153 C154 H354 109.5 . . ? H154 C154 H354 109.5 . . ? H254 C154 H354 109.5 . . ? C156 C155 C160 120.5(19) . . ? C156 C155 C152 120.2(17) . . ? C160 C155 C152 119.4(15) . . ? C155 C156 C157 119(2) . . ? C155 C156 H156 120.5 . . ? C157 C156 H156 120.5 . . ? C158 C157 C156 119.6(19) . . ? C158 C157 H157 120.2 . . ? C156 C157 H157 120.2 . . ? C157 C158 C159 122(2) . . ? C157 C158 H158 118.9 . . ? C159 C158 H158 118.9 . . ? C158 C159 C160 119(2) . . ? C158 C159 H159 120.5 . . ? C160 C159 H159 120.5 . . ? C159 C160 C155 119.7(18) . . ? C159 C160 H160 120.2 . . ? C155 C160 H160 120.2 . . ? O17 C171 O18 124.0(15) . . ? O17 C171 C172 120.8(14) . . ? O18 C171 C172 115.2(13) . . ? C171 C172 C173 110.9(14) . . ? C171 C172 C175 107.7(13) . . ? C173 C172 C175 112.6(15) . . ? C171 C172 H172 108.5 . . ? C173 C172 H172 108.5 . . ? C175 C172 H172 108.5 . . ? C174 C173 C172 114.9(17) . . ? C174 C173 H173 108.5 . . ? C172 C173 H173 108.5 . . ? C174 C173 H273 108.5 . . ? C172 C173 H273 108.5 . . ? H173 C173 H273 107.5 . . ? C173 C174 H174 109.5 . . ? C173 C174 H274 109.5 . . ? H174 C174 H274 109.5 . . ? C173 C174 H374 109.5 . . ? H174 C174 H374 109.5 . . ? H274 C174 H374 109.5 . . ? C180 C175 C176 118.9(16) . . ? C180 C175 C172 120.5(14) . . ? C176 C175 C172 120.5(14) . . ? C175 C176 C177 120.2(17) . . ? C175 C176 H176 119.9 . . ? C177 C176 H176 119.9 . . ? C178 C177 C176 120.2(18) . . ? C178 C177 H177 119.9 . . ? C176 C177 H177 119.9 . . ? C177 C178 C179 119.8(18) . . ? C177 C178 H178 120.1 . . ? C179 C178 H178 120.1 . . ? C180 C179 C178 118.6(18) . . ? C180 C179 H179 120.7 . . ? C178 C179 H179 120.7 . . ? C175 C180 C179 122.1(16) . . ? C175 C180 H180 118.9 . . ? C179 C180 H180 118.9 . . ? N21 B1 N11 111.3(16) . . ? N21 B1 N31 107.4(16) . . ? N11 B1 N31 110.8(16) . . ? N21 B1 H1B 109.1 . . ? N11 B1 H1B 109.1 . . ? N31 B1 H1B 109.1 . . ? N26 B2 N16 111.5(14) . . ? N26 B2 N36 109.0(13) . . ? N16 B2 N36 110.2(13) . . ? N26 B2 H2B 108.7 . . ? N16 B2 H2B 108.7 . . ? N36 B2 H2B 108.7 . . ? N121 B11 N131 106.9(13) . . ? N121 B11 N111 110.0(13) . . ? N131 B11 N111 108.6(13) . . ? N121 B11 H11B 110.4 . . ? N131 B11 H11B 110.4 . . ? N111 B11 H11B 110.4 . . ? N136 B12 N126 108.5(14) . . ? N136 B12 N116 111.1(14) . . ? N126 B12 N116 108.3(14) . . ? N136 B12 H12B 109.6 . . ? N126 B12 H12B 109.6 . . ? N116 B12 H12B 109.6 . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 #_geom_contact_publ_flag Dy1 Dy2 3.8578(9) . ? Dy11 Dy12 3.9590(9) . ? Dy12 O13 3.09(1) . ? 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 O8 Dy2 O1 C1 85(4) . . . . ? O6 Dy2 O1 C1 -134(4) . . . . ? O4 Dy2 O1 C1 151(4) . . . . ? N17 Dy2 O1 C1 -52(4) . . . . ? N27 Dy2 O1 C1 -58(4) . . . . ? N37 Dy2 O1 C1 14(4) . . . . ? O3 Dy2 O1 C1 156(4) . . . . ? O8 Dy2 O1 Dy1 -71.2(4) . . . . ? O6 Dy2 O1 Dy1 70.0(4) . . . . ? O4 Dy2 O1 Dy1 -5.3(6) . . . . ? N17 Dy2 O1 Dy1 151.7(7) . . . . ? N27 Dy2 O1 Dy1 145.8(5) . . . . ? N37 Dy2 O1 Dy1 -142.3(4) . . . . ? O3 Dy2 O1 Dy1 -0.5(4) . . . . ? O3 Dy1 O1 C1 -173.4(9) . . . . ? O5 Dy1 O1 C1 108.1(9) . . . . ? O7 Dy1 O1 C1 -95.8(9) . . . . ? O2 Dy1 O1 C1 -0.3(8) . . . . ? N22 Dy1 O1 C1 34.6(9) . . . . ? N12 Dy1 O1 C1 -61.5(11) . . . . ? N32 Dy1 O1 C1 133.0(9) . . . . ? O3 Dy1 O1 Dy2 0.6(4) . . . . ? O5 Dy1 O1 Dy2 -77.9(4) . . . . ? O7 Dy1 O1 Dy2 78.2(5) . . . . ? O2 Dy1 O1 Dy2 173.6(7) . . . . ? N22 Dy1 O1 Dy2 -151.4(4) . . . . ? N12 Dy1 O1 Dy2 112.5(6) . . . . ? N32 Dy1 O1 Dy2 -53.0(8) . . . . ? O3 Dy1 O2 C1 9.2(12) . . . . ? O5 Dy1 O2 C1 -64.0(10) . . . . ? O7 Dy1 O2 C1 73.5(10) . . . . ? N22 Dy1 O2 C1 -146.7(11) . . . . ? N12 Dy1 O2 C1 145.2(10) . . . . ? N32 Dy1 O2 C1 -133.8(10) . . . . ? O1 Dy1 O2 C1 0.4(9) . . . . ? O5 Dy1 O3 C41 -162(6) . . . . ? O7 Dy1 O3 C41 49(6) . . . . ? O2 Dy1 O3 C41 117(6) . . . . ? N22 Dy1 O3 C41 -114(6) . . . . ? N12 Dy1 O3 C41 -16(6) . . . . ? N32 Dy1 O3 C41 -83(6) . . . . ? O1 Dy1 O3 C41 124(6) . . . . ? O5 Dy1 O3 Dy2 73.6(4) . . . . ? O7 Dy1 O3 Dy2 -75.6(4) . . . . ? O2 Dy1 O3 Dy2 -7.5(6) . . . . ? N22 Dy1 O3 Dy2 121.3(7) . . . . ? N12 Dy1 O3 Dy2 -140.4(4) . . . . ? N32 Dy1 O3 Dy2 151.8(4) . . . . ? O1 Dy1 O3 Dy2 -0.5(4) . . . . ? O1 Dy2 O3 C41 -171.4(9) . . . . ? O8 Dy2 O3 C41 -88.9(9) . . . . ? O6 Dy2 O3 C41 103.5(9) . . . . ? O4 Dy2 O3 C41 3.6(8) . . . . ? N17 Dy2 O3 C41 23.5(10) . . . . ? N27 Dy2 O3 C41 131.6(9) . . . . ? N37 Dy2 O3 C41 -90.3(10) . . . . ? O1 Dy2 O3 Dy1 0.5(4) . . . . ? O8 Dy2 O3 Dy1 83.0(4) . . . . ? O6 Dy2 O3 Dy1 -84.6(4) . . . . ? O4 Dy2 O3 Dy1 175.5(6) . . . . ? N17 Dy2 O3 Dy1 -164.6(4) . . . . ? N27 Dy2 O3 Dy1 -56.4(7) . . . . ? N37 Dy2 O3 Dy1 81.7(7) . . . . ? O1 Dy2 O4 C41 2.3(11) . . . . ? O8 Dy2 O4 C41 68.2(10) . . . . ? O6 Dy2 O4 C41 -71.4(10) . . . . ? N17 Dy2 O4 C41 -167.5(10) . . . . ? N27 Dy2 O4 C41 -126.0(10) . . . . ? N37 Dy2 O4 C41 129.0(10) . . . . ? O3 Dy2 O4 C41 -3.7(9) . . . . ? O3 Dy1 O5 C51 -31.3(14) . . . . ? O7 Dy1 O5 C51 15.8(17) . . . . ? O2 Dy1 O5 C51 99.1(15) . . . . ? N22 Dy1 O5 C51 170.5(15) . . . . ? N12 Dy1 O5 C51 -141.4(14) . . . . ? N32 Dy1 O5 C51 -114.9(15) . . . . ? O1 Dy1 O5 C51 50.8(14) . . . . ? O1 Dy2 O6 C51 -23.0(13) . . . . ? O8 Dy2 O6 C51 39.3(15) . . . . ? O4 Dy2 O6 C51 105.6(13) . . . . ? N17 Dy2 O6 C51 -176.7(13) . . . . ? N27 Dy2 O6 C51 -105.3(13) . . . . ? N37 Dy2 O6 C51 -107.9(14) . . . . ? O3 Dy2 O6 C51 56.0(13) . . . . ? O3 Dy1 O7 C71 24.4(13) . . . . ? O5 Dy1 O7 C71 -22.8(16) . . . . ? O2 Dy1 O7 C71 -109.6(13) . . . . ? N22 Dy1 O7 C71 -167.0(12) . . . . ? N12 Dy1 O7 C71 144.4(14) . . . . ? N32 Dy1 O7 C71 89.8(14) . . . . ? O1 Dy1 O7 C71 -57.6(13) . . . . ? O1 Dy2 O8 C71 42.8(16) . . . . ? O6 Dy2 O8 C71 -20.3(19) . . . . ? O4 Dy2 O8 C71 -88.7(16) . . . . ? N17 Dy2 O8 C71 -157.7(15) . . . . ? N27 Dy2 O8 C71 104.1(16) . . . . ? N37 Dy2 O8 C71 142.1(17) . . . . ? O3 Dy2 O8 C71 -37.0(15) . . . . ? O16 Dy12 O11 C101 -63(4) . . . . ? O18 Dy12 O11 C101 159(4) . . . . ? O14 Dy12 O11 C101 -130(4) . . . . ? N117 Dy12 O11 C101 19(4) . . . . ? N137 Dy12 O11 C101 86(4) . . . . ? N127 Dy12 O11 C101 14(4) . . . . ? O16 Dy12 O11 Dy11 67.6(4) . . . . ? O18 Dy12 O11 Dy11 -70.7(4) . . . . ? O14 Dy12 O11 Dy11 -0.2(7) . . . . ? N117 Dy12 O11 Dy11 149.5(11) . . . . ? N137 Dy12 O11 Dy11 -143.6(4) . . . . ? N127 Dy12 O11 Dy11 144.5(4) . . . . ? O17 Dy11 O11 C101 -113.0(9) . . . . ? O13 Dy11 O11 C101 169.3(9) . . . . ? O15 Dy11 O11 C101 92.9(9) . . . . ? O12 Dy11 O11 C101 1.9(8) . . . . ? N112 Dy11 O11 C101 -142.7(10) . . . . ? N122 Dy11 O11 C101 -47.8(9) . . . . ? N132 Dy11 O11 C101 37.1(10) . . . . ? O17 Dy11 O11 Dy12 79.5(4) . . . . ? O13 Dy11 O11 Dy12 1.8(5) . . . . ? O15 Dy11 O11 Dy12 -74.6(5) . . . . ? O12 Dy11 O11 Dy12 -165.5(7) . . . . ? N112 Dy11 O11 Dy12 49.8(11) . . . . ? N122 Dy11 O11 Dy12 144.7(4) . . . . ? N132 Dy11 O11 Dy12 -130.4(4) . . . . ? O17 Dy11 O12 C101 56.1(9) . . . . ? O13 Dy11 O12 C101 -19.2(12) . . . . ? O15 Dy11 O12 C101 -81.3(9) . . . . ? N112 Dy11 O12 C101 154.4(9) . . . . ? N122 Dy11 O12 C101 129.4(10) . . . . ? N132 Dy11 O12 C101 -154.9(10) . . . . ? O11 Dy11 O12 C101 -2.0(8) . . . . ? O17 Dy11 O13 C141 -98(6) . . . . ? O15 Dy11 O13 C141 50(6) . . . . ? O12 Dy11 O13 C141 -15(7) . . . . ? N112 Dy11 O13 C141 169(6) . . . . ? N122 Dy11 O13 C141 -141(6) . . . . ? N132 Dy11 O13 C141 106(6) . . . . ? O11 Dy11 O13 C141 -28(6) . . . . ? O16 Dy12 O14 C141 -65.1(14) . . . . ? O11 Dy12 O14 C141 0.8(16) . . . . ? O18 Dy12 O14 C141 68.8(14) . . . . ? N117 Dy12 O14 C141 -169.5(15) . . . . ? N137 Dy12 O14 C141 133.1(13) . . . . ? N127 Dy12 O14 C141 -122.1(13) . . . . ? O17 Dy11 O15 C151 2.2(18) . . . . ? O13 Dy11 O15 C151 -48.7(15) . . . . ? O12 Dy11 O15 C151 89.1(15) . . . . ? N112 Dy11 O15 C151 -120.6(14) . . . . ? N122 Dy11 O15 C151 142.0(13) . . . . ? N132 Dy11 O15 C151 176.3(16) . . . . ? O11 Dy11 O15 C151 39.3(14) . . . . ? O11 Dy12 O16 C151 -42.5(19) . . . . ? O18 Dy12 O16 C151 16(2) . . . . ? O14 Dy12 O16 C151 85(2) . . . . ? N117 Dy12 O16 C151 156.4(19) . . . . ? N137 Dy12 O16 C151 -123.8(19) . . . . ? N127 Dy12 O16 C151 -131(2) . . . . ? O13 Dy11 O17 C171 32.0(16) . . . . ? O15 Dy11 O17 C171 -18.6(18) . . . . ? O12 Dy11 O17 C171 -101.0(16) . . . . ? N112 Dy11 O17 C171 111.7(16) . . . . ? N122 Dy11 O17 C171 -174.3(17) . . . . ? N132 Dy11 O17 C171 172.5(14) . . . . ? O11 Dy11 O17 C171 -57.5(15) . . . . ? O16 Dy12 O18 C171 -22.7(17) . . . . ? O11 Dy12 O18 C171 35.3(15) . . . . ? O14 Dy12 O18 C171 -91.3(16) . . . . ? N117 Dy12 O18 C171 -158.3(15) . . . . ? N137 Dy12 O18 C171 136.9(16) . . . . ? N127 Dy12 O18 C171 100.6(16) . . . . ? C15 N11 N12 C13 -4.7(19) . . . . ? B1 N11 N12 C13 -179.0(16) . . . . ? C15 N11 N12 Dy1 -177.9(12) . . . . ? B1 N11 N12 Dy1 8(2) . . . . ? O3 Dy1 N12 N11 -115.7(12) . . . . ? O5 Dy1 N12 N11 -16.9(18) . . . . ? O7 Dy1 N12 N11 179.0(14) . . . . ? O2 Dy1 N12 N11 99.8(13) . . . . ? N22 Dy1 N12 N11 33.5(12) . . . . ? N32 Dy1 N12 N11 -43.7(13) . . . . ? O1 Dy1 N12 N11 144.9(11) . . . . ? C1 Dy1 N12 N11 116.7(12) . . . . ? O3 Dy1 N12 C13 72.8(15) . . . . ? O5 Dy1 N12 C13 171.6(12) . . . . ? O7 Dy1 N12 C13 7.5(14) . . . . ? O2 Dy1 N12 C13 -71.7(15) . . . . ? N22 Dy1 N12 C13 -138.0(15) . . . . ? N32 Dy1 N12 C13 144.8(16) . . . . ? O1 Dy1 N12 C13 -26.6(18) . . . . ? C20 N16 N17 C18 3.3(17) . . . . ? B2 N16 N17 C18 -178.6(14) . . . . ? C20 N16 N17 Dy2 -179.6(10) . . . . ? B2 N16 N17 Dy2 -1.5(19) . . . . ? O1 Dy2 N17 C18 -150.5(12) . . . . ? O8 Dy2 N17 C18 79.9(13) . . . . ? O6 Dy2 N17 C18 -72.0(13) . . . . ? O4 Dy2 N17 C18 10.8(12) . . . . ? N27 Dy2 N17 C18 -144.4(13) . . . . ? N37 Dy2 N17 C18 139.0(13) . . . . ? O3 Dy2 N17 C18 -4.7(14) . . . . ? O1 Dy2 N17 N16 32.9(16) . . . . ? O8 Dy2 N17 N16 -96.7(11) . . . . ? O6 Dy2 N17 N16 111.5(11) . . . . ? O4 Dy2 N17 N16 -165.8(12) . . . . ? N27 Dy2 N17 N16 39.1(11) . . . . ? N37 Dy2 N17 N16 -37.5(11) . . . . ? O3 Dy2 N17 N16 178.7(10) . . . . ? C25 N21 N22 C23 -2.8(18) . . . . ? B1 N21 N22 C23 -179.7(16) . . . . ? C25 N21 N22 Dy1 -174.2(10) . . . . ? B1 N21 N22 Dy1 9(2) . . . . ? O3 Dy1 N22 C23 -102.6(15) . . . . ? O5 Dy1 N22 C23 -56.5(14) . . . . ? O7 Dy1 N22 C23 100.1(15) . . . . ? O2 Dy1 N22 C23 38.2(14) . . . . ? N12 Dy1 N22 C23 148.6(15) . . . . ? N32 Dy1 N22 C23 -134.0(15) . . . . ? O1 Dy1 N22 C23 9.9(15) . . . . ? O3 Dy1 N22 N21 66.6(15) . . . . ? O5 Dy1 N22 N21 112.7(12) . . . . ? O7 Dy1 N22 N21 -90.7(13) . . . . ? O2 Dy1 N22 N21 -152.6(13) . . . . ? N12 Dy1 N22 N21 -42.2(12) . . . . ? N32 Dy1 N22 N21 35.2(12) . . . . ? O1 Dy1 N22 N21 179.1(11) . . . . ? C30 N26 N27 C28 -1.3(19) . . . . ? B2 N26 N27 C28 179.2(14) . . . . ? C30 N26 N27 Dy2 -177.6(11) . . . . ? B2 N26 N27 Dy2 3(2) . . . . ? O1 Dy2 N27 C28 -38.7(14) . . . . ? O8 Dy2 N27 C28 -99.3(14) . . . . ? O6 Dy2 N27 C28 44.2(13) . . . . ? O4 Dy2 N27 C28 101.5(14) . . . . ? N17 Dy2 N27 C28 144.0(14) . . . . ? N37 Dy2 N27 C28 -137.2(14) . . . . ? O3 Dy2 N27 C28 17.0(16) . . . . ? O1 Dy2 N27 N26 136.8(12) . . . . ? O8 Dy2 N27 N26 76.2(13) . . . . ? O6 Dy2 N27 N26 -140.2(12) . . . . ? O4 Dy2 N27 N26 -83.0(13) . . . . ? N17 Dy2 N27 N26 -40.4(11) . . . . ? N37 Dy2 N27 N26 38.3(12) . . . . ? O3 Dy2 N27 N26 -167.5(10) . . . . ? C35 N31 N32 C33 0.6(19) . . . . ? B1 N31 N32 C33 -176.1(16) . . . . ? C35 N31 N32 Dy1 -178.7(10) . . . . ? B1 N31 N32 Dy1 5(2) . . . . ? O3 Dy1 N32 C33 -25.5(15) . . . . ? O5 Dy1 N32 C33 51.8(15) . . . . ? O7 Dy1 N32 C33 -88.3(16) . . . . ? O2 Dy1 N32 C33 126.5(14) . . . . ? N22 Dy1 N32 C33 139.3(16) . . . . ? N12 Dy1 N32 C33 -142.9(16) . . . . ? O1 Dy1 N32 C33 27.5(19) . . . . ? O3 Dy1 N32 N31 153.7(13) . . . . ? O5 Dy1 N32 N31 -129.0(13) . . . . ? O7 Dy1 N32 N31 90.9(13) . . . . ? O2 Dy1 N32 N31 -54.4(15) . . . . ? N22 Dy1 N32 N31 -41.5(12) . . . . ? N12 Dy1 N32 N31 36.2(12) . . . . ? O1 Dy1 N32 N31 -153.3(10) . . . . ? C40 N36 N37 C38 -2.3(18) . . . . ? B2 N36 N37 C38 -178.2(14) . . . . ? C40 N36 N37 Dy2 176.6(10) . . . . ? B2 N36 N37 Dy2 0.7(19) . . . . ? O1 Dy2 N37 N36 -117.5(12) . . . . ? O8 Dy2 N37 N36 166.5(13) . . . . ? O6 Dy2 N37 N36 -36.7(16) . . . . ? O4 Dy2 N37 N36 102.9(12) . . . . ? N17 Dy2 N37 N36 37.6(11) . . . . ? N27 Dy2 N37 N36 -39.3(11) . . . . ? O3 Dy2 N37 N36 167.8(9) . . . . ? O1 Dy2 N37 C38 61.2(14) . . . . ? O8 Dy2 N37 C38 -14.8(13) . . . . ? O6 Dy2 N37 C38 142.0(12) . . . . ? O4 Dy2 N37 C38 -78.5(14) . . . . ? N17 Dy2 N37 C38 -143.7(14) . . . . ? N27 Dy2 N37 C38 139.4(14) . . . . ? O3 Dy2 N37 C38 -13.5(17) . . . . ? C115 N111 N112 C113 1.4(18) . . . . ? B11 N111 N112 C113 178.6(14) . . . . ? C115 N111 N112 Dy11 179.8(11) . . . . ? B11 N111 N112 Dy11 -3.0(19) . . . . ? O17 Dy11 N112 C113 -68.6(15) . . . . ? O13 Dy11 N112 C113 7.7(15) . . . . ? O15 Dy11 N112 C113 76.8(15) . . . . ? O12 Dy11 N112 C113 -167.5(13) . . . . ? N122 Dy11 N112 C113 -142.5(16) . . . . ? N132 Dy11 N112 C113 139.2(16) . . . . ? O11 Dy11 N112 C113 -41(2) . . . . ? O17 Dy11 N112 N111 113.5(12) . . . . ? O13 Dy11 N112 N111 -170.2(12) . . . . ? O15 Dy11 N112 N111 -101.2(12) . . . . ? O12 Dy11 N112 N111 14.5(16) . . . . ? N122 Dy11 N112 N111 39.5(11) . . . . ? N132 Dy11 N112 N111 -38.8(11) . . . . ? O11 Dy11 N112 N111 141.1(10) . . . . ? C120 N116 N117 C118 3(2) . . . . ? B12 N116 N117 C118 179.9(17) . . . . ? C120 N116 N117 Dy12 -177.7(14) . . . . ? B12 N116 N117 Dy12 -1(2) . . . . ? O16 Dy12 N117 C118 -70.0(17) . . . . ? O11 Dy12 N117 C118 -147.8(17) . . . . ? O18 Dy12 N117 C118 77.1(17) . . . . ? O14 Dy12 N117 C118 5.9(17) . . . . ? N137 Dy12 N117 C118 141.8(17) . . . . ? N127 Dy12 N117 C118 -142.6(17) . . . . ? O16 Dy12 N117 N116 111.1(12) . . . . ? O11 Dy12 N117 N116 33(2) . . . . ? O18 Dy12 N117 N116 -101.8(12) . . . . ? O14 Dy12 N117 N116 -173.0(13) . . . . ? N137 Dy12 N117 N116 -37.1(11) . . . . ? N127 Dy12 N117 N116 38.4(11) . . . . ? C125 N121 N122 C123 -0.7(17) . . . . ? B11 N121 N122 C123 -177.5(14) . . . . ? C125 N121 N122 Dy11 174.5(10) . . . . ? B11 N121 N122 Dy11 -2.2(19) . . . . ? O17 Dy11 N122 C123 41.4(13) . . . . ? O13 Dy11 N122 C123 85.2(15) . . . . ? O15 Dy11 N122 C123 -111.7(13) . . . . ? O12 Dy11 N122 C123 -56.8(13) . . . . ? N112 Dy11 N122 C123 137.0(14) . . . . ? N132 Dy11 N122 C123 -145.6(14) . . . . ? O11 Dy11 N122 C123 -20.1(14) . . . . ? O17 Dy11 N122 N121 -132.8(11) . . . . ? O13 Dy11 N122 N121 -89.0(12) . . . . ? O15 Dy11 N122 N121 74.2(13) . . . . ? O12 Dy11 N122 N121 129.1(11) . . . . ? N112 Dy11 N122 N121 -37.1(11) . . . . ? N132 Dy11 N122 N121 40.2(10) . . . . ? O11 Dy11 N122 N121 165.8(10) . . . . ? C130 N126 N127 C128 2.8(19) . . . . ? B12 N126 N127 C128 -178.5(16) . . . . ? C130 N126 N127 Dy12 171.9(11) . . . . ? B12 N126 N127 Dy12 -9(2) . . . . ? O16 Dy12 N127 C128 28.4(15) . . . . ? O11 Dy12 N127 C128 -48.2(16) . . . . ? O18 Dy12 N127 C128 -110.6(15) . . . . ? O14 Dy12 N127 C128 86.6(17) . . . . ? N117 Dy12 N127 C128 133.5(16) . . . . ? N137 Dy12 N127 C128 -147.5(16) . . . . ? O16 Dy12 N127 N126 -137.6(12) . . . . ? O11 Dy12 N127 N126 145.8(12) . . . . ? O18 Dy12 N127 N126 83.3(13) . . . . ? O14 Dy12 N127 N126 -79.4(13) . . . . ? N117 Dy12 N127 N126 -32.6(11) . . . . ? N137 Dy12 N127 N126 46.5(11) . . . . ? C135 N131 N132 C133 1.6(17) . . . . ? B11 N131 N132 C133 -177.9(15) . . . . ? C135 N131 N132 Dy11 172.1(10) . . . . ? B11 N131 N132 Dy11 -7(2) . . . . ? O17 Dy11 N132 C133 146.1(11) . . . . ? O13 Dy11 N132 C133 -83.6(14) . . . . ? O15 Dy11 N132 C133 -26.1(12) . . . . ? O12 Dy11 N132 C133 57.1(13) . . . . ? N112 Dy11 N132 C133 -148.9(13) . . . . ? N122 Dy11 N132 C133 132.8(13) . . . . ? O11 Dy11 N132 C133 31.2(14) . . . . ? O17 Dy11 N132 N131 -21.7(15) . . . . ? O13 Dy11 N132 N131 108.7(11) . . . . ? O15 Dy11 N132 N131 166.2(12) . . . . ? O12 Dy11 N132 N131 -110.6(11) . . . . ? N112 Dy11 N132 N131 43.4(11) . . . . ? N122 Dy11 N132 N131 -34.9(11) . . . . ? O11 Dy11 N132 N131 -136.6(10) . . . . ? C140 N136 N137 C138 -1.5(16) . . . . ? B12 N136 N137 C138 -179.4(14) . . . . ? C140 N136 N137 Dy12 177.7(10) . . . . ? B12 N136 N137 Dy12 -0.2(18) . . . . ? O16 Dy12 N137 C138 129.4(12) . . . . ? O11 Dy12 N137 C138 54.1(13) . . . . ? O18 Dy12 N137 C138 -19.8(13) . . . . ? O14 Dy12 N137 C138 -87.0(14) . . . . ? N117 Dy12 N137 C138 -143.7(14) . . . . ? N127 Dy12 N137 C138 137.2(14) . . . . ? O16 Dy12 N137 N136 -49.6(14) . . . . ? O11 Dy12 N137 N136 -124.9(10) . . . . ? O18 Dy12 N137 N136 161.2(11) . . . . ? O14 Dy12 N137 N136 94.0(11) . . . . ? N117 Dy12 N137 N136 37.3(10) . . . . ? N127 Dy12 N137 N136 -41.9(10) . . . . ? Dy1 O2 C1 O1 -0.7(16) . . . . ? Dy1 O2 C1 C2 -178.6(12) . . . . ? Dy2 O1 C1 O2 -157(3) . . . . ? Dy1 O1 C1 O2 0.6(15) . . . . ? Dy2 O1 C1 C2 22(5) . . . . ? Dy1 O1 C1 C2 178.7(12) . . . . ? Dy2 O1 C1 Dy1 -157(4) . . . . ? O2 C1 C2 C3 -60(2) . . . . ? O1 C1 C2 C3 121.8(17) . . . . ? O2 C1 C2 C5 63.7(19) . . . . ? O1 C1 C2 C5 -114.3(15) . . . . ? C5 C2 C3 C4 63(2) . . . . ? C1 C2 C3 C4 -174.5(17) . . . . ? C3 C2 C5 C10 56(2) . . . . ? C1 C2 C5 C10 -67(2) . . . . ? C3 C2 C5 C6 -121.9(17) . . . . ? C1 C2 C5 C6 115.4(16) . . . . ? C10 C5 C6 C7 1(3) . . . . ? C2 C5 C6 C7 179.7(19) . . . . ? C5 C6 C7 C8 -2(4) . . . . ? C6 C7 C8 C9 0(4) . . . . ? C7 C8 C9 C10 4(4) . . . . ? C8 C9 C10 C5 -5(4) . . . . ? C6 C5 C10 C9 2(3) . . . . ? C2 C5 C10 C9 -176.3(19) . . . . ? N11 N12 C13 C14 5(2) . . . . ? Dy1 N12 C13 C14 177.9(14) . . . . ? N12 C13 C14 C15 -4(3) . . . . ? N12 N11 C15 C14 2(2) . . . . ? B1 N11 C15 C14 176(2) . . . . ? C13 C14 C15 N11 1(3) . . . . ? N16 N17 C18 C19 -5.3(18) . . . . ? Dy2 N17 C18 C19 177.8(10) . . . . ? N17 C18 C19 C20 5.1(19) . . . . ? N17 N16 C20 C19 0.0(19) . . . . ? B2 N16 C20 C19 -177.9(16) . . . . ? C18 C19 C20 N16 -3.0(19) . . . . ? N21 N22 C23 C24 3.4(19) . . . . ? Dy1 N22 C23 C24 174.1(11) . . . . ? N22 C23 C24 C25 -3(2) . . . . ? C23 C24 C25 N21 0.7(18) . . . . ? N22 N21 C25 C24 1.3(19) . . . . ? B1 N21 C25 C24 177.9(17) . . . . ? N26 N27 C28 C29 -0.3(19) . . . . ? Dy2 N27 C28 C29 175.8(12) . . . . ? N27 C28 C29 C30 2(2) . . . . ? N27 N26 C30 C29 2(2) . . . . ? B2 N26 C30 C29 -178.0(18) . . . . ? C28 C29 C30 N26 -3(2) . . . . ? N31 N32 C33 C34 1(2) . . . . ? Dy1 N32 C33 C34 -179.9(11) . . . . ? N32 C33 C34 C35 -2(2) . . . . ? N32 N31 C35 C34 -1.8(19) . . . . ? B1 N31 C35 C34 174.4(18) . . . . ? C33 C34 C35 N31 2.2(19) . . . . ? N36 N37 C38 C39 0.4(19) . . . . ? Dy2 N37 C38 C39 -178.5(12) . . . . ? N37 C38 C39 C40 2(2) . . . . ? N37 N36 C40 C39 3.4(19) . . . . ? B2 N36 C40 C39 178.7(16) . . . . ? C38 C39 C40 N36 -3(2) . . . . ? Dy2 O4 C41 O3 7.1(16) . . . . ? Dy2 O4 C41 C42 -175.6(13) . . . . ? Dy1 O3 C41 O4 -132(5) . . . . ? Dy2 O3 C41 O4 -6.0(14) . . . . ? Dy1 O3 C41 C42 51(7) . . . . ? Dy2 O3 C41 C42 176.6(13) . . . . ? O4 C41 C42 C45 98.3(17) . . . . ? O3 C41 C42 C45 -84.3(17) . . . . ? O4 C41 C42 C43 -32(2) . . . . ? O3 C41 C42 C43 145.4(14) . . . . ? C41 C42 C43 C44 -65.0(19) . . . . ? C45 C42 C43 C44 168.1(15) . . . . ? C41 C42 C45 C50 -85.7(19) . . . . ? C43 C42 C45 C50 43(2) . . . . ? C41 C42 C45 C46 96.4(17) . . . . ? C43 C42 C45 C46 -135.0(16) . . . . ? C50 C45 C46 C47 1(3) . . . . ? C42 C45 C46 C47 178.7(16) . . . . ? C45 C46 C47 C48 -5(3) . . . . ? C46 C47 C48 C49 7(3) . . . . ? C47 C48 C49 C50 -5(3) . . . . ? C46 C45 C50 C49 2(3) . . . . ? C42 C45 C50 C49 -176.3(16) . . . . ? C48 C49 C50 C45 1(3) . . . . ? Dy1 O5 C51 O6 -9(2) . . . . ? Dy1 O5 C51 C52 176.8(10) . . . . ? Dy2 O6 C51 O5 -15(2) . . . . ? Dy2 O6 C51 C52 159.7(10) . . . . ? O5 C51 C52 C55 67.8(17) . . . . ? O6 C51 C52 C55 -107.2(15) . . . . ? O5 C51 C52 C53 -59.0(18) . . . . ? O6 C51 C52 C53 126.0(14) . . . . ? C51 C52 C53 C54 -70.2(17) . . . . ? C55 C52 C53 C54 165.4(14) . . . . ? C51 C52 C55 C56 -64.2(19) . . . . ? C53 C52 C55 C56 62(2) . . . . ? C51 C52 C55 C60 118.1(16) . . . . ? C53 C52 C55 C60 -116.0(17) . . . . ? C60 C55 C56 C57 1(3) . . . . ? C52 C55 C56 C57 -176.4(18) . . . . ? C55 C56 C57 C58 -3(3) . . . . ? C56 C57 C58 C59 1(3) . . . . ? C57 C58 C59 C60 2(3) . . . . ? C56 C55 C60 C59 2(3) . . . . ? C52 C55 C60 C59 179.4(16) . . . . ? C58 C59 C60 C55 -3(3) . . . . ? Dy2 O8 C71 O7 -18(3) . . . . ? Dy2 O8 C71 C72 166.0(11) . . . . ? Dy1 O7 C71 O8 32(2) . . . . ? Dy1 O7 C71 C72 -151.4(10) . . . . ? O8 C71 C72 C75 129.3(15) . . . . ? O7 C71 C72 C75 -47.4(17) . . . . ? O8 C71 C72 C73 -2(2) . . . . ? O7 C71 C72 C73 -178.8(13) . . . . ? C75 C72 C73 C74 55(2) . . . . ? C71 C72 C73 C74 -173.9(15) . . . . ? C73 C72 C75 C76 -92.6(18) . . . . ? C71 C72 C75 C76 137.4(15) . . . . ? C73 C72 C75 C80 84.1(17) . . . . ? C71 C72 C75 C80 -45.9(18) . . . . ? C80 C75 C76 C77 -1(3) . . . . ? C72 C75 C76 C77 175.9(17) . . . . ? C75 C76 C77 C78 -2(3) . . . . ? C76 C77 C78 C79 0(3) . . . . ? C77 C78 C79 C80 3(3) . . . . ? C76 C75 C80 C79 5(2) . . . . ? C72 C75 C80 C79 -172.2(14) . . . . ? C78 C79 C80 C75 -6(2) . . . . ? Dy12 O11 C101 O12 129(3) . . . . ? Dy11 O11 C101 O12 -3.2(13) . . . . ? Dy12 O11 C101 C102 -58(4) . . . . ? Dy11 O11 C101 C102 170.0(12) . . . . ? Dy12 O11 C101 Dy11 132(4) . . . . ? Dy11 O12 C101 O11 3.8(16) . . . . ? Dy11 O12 C101 C102 -169.3(11) . . . . ? O11 C101 C102 C105 -99.5(16) . . . . ? O12 C101 C102 C105 73.6(18) . . . . ? O11 C101 C102 C103 133.7(14) . . . . ? O12 C101 C102 C103 -53.2(19) . . . . ? C105 C102 C103 C104 66.0(18) . . . . ? C101 C102 C103 C104 -171.8(12) . . . . ? C103 C102 C105 C110 46(2) . . . . ? C101 C102 C105 C110 -80(2) . . . . ? C103 C102 C105 C106 -138.9(17) . . . . ? C101 C102 C105 C106 95.3(18) . . . . ? C110 C105 C106 C107 -1(3) . . . . ? C102 C105 C106 C107 -176.4(17) . . . . ? C105 C106 C107 C108 -3(3) . . . . ? C106 C107 C108 C109 4(3) . . . . ? C107 C108 C109 C110 -2(3) . . . . ? C108 C109 C110 C105 -2(3) . . . . ? C106 C105 C110 C109 3(3) . . . . ? C102 C105 C110 C109 178.6(17) . . . . ? N111 N112 C113 C114 0(2) . . . . ? Dy11 N112 C113 C114 -177.9(13) . . . . ? N112 C113 C114 C115 -2(2) . . . . ? N112 N111 C115 C114 -3(2) . . . . ? B11 N111 C115 C114 -179.6(16) . . . . ? C113 C114 C115 N111 3(2) . . . . ? N116 N117 C118 C119 -3(2) . . . . ? Dy12 N117 C118 C119 177.6(16) . . . . ? N117 C118 C119 C120 2(3) . . . . ? N117 N116 C120 C119 -2(3) . . . . ? B12 N116 C120 C119 -178(2) . . . . ? C118 C119 C120 N116 0(3) . . . . ? N121 N122 C123 C124 -2.5(19) . . . . ? Dy11 N122 C123 C124 -177.3(11) . . . . ? N122 C123 C124 C125 5(2) . . . . ? C123 C124 C125 N121 -5(2) . . . . ? N122 N121 C125 C124 3.8(19) . . . . ? B11 N121 C125 C124 -179.6(16) . . . . ? N126 N127 C128 C129 -3(2) . . . . ? Dy12 N127 C128 C129 -170.9(12) . . . . ? N127 C128 C129 C130 2(2) . . . . ? N127 N126 C130 C129 -1(2) . . . . ? B12 N126 C130 C129 -180.0(17) . . . . ? C128 C129 C130 N126 0(2) . . . . ? N131 N132 C133 C134 -0.4(17) . . . . ? Dy11 N132 C133 C134 -169.3(10) . . . . ? N132 C133 C134 C135 -0.9(18) . . . . ? N132 N131 C135 C134 -2.2(19) . . . . ? B11 N131 C135 C134 177.3(16) . . . . ? C133 C134 C135 N131 1.9(19) . . . . ? N136 N137 C138 C139 2.5(18) . . . . ? Dy12 N137 C138 C139 -176.6(11) . . . . ? N137 C138 C139 C140 -2.5(19) . . . . ? N137 N136 C140 C139 -0.1(18) . . . . ? B12 N136 C140 C139 177.6(16) . . . . ? C138 C139 C140 N136 2(2) . . . . ? Dy12 O14 C141 O13 -5(2) . . . . ? Dy12 O14 C141 C142 169.5(13) . . . . ? Dy11 O13 C141 O14 31(8) . . . . ? Dy11 O13 C141 C142 -144(6) . . . . ? O14 C141 C142 C145 25(2) . . . . ? O13 C141 C142 C145 -160.4(16) . . . . ? O14 C141 C142 C143 -101.8(19) . . . . ? O13 C141 C142 C143 73(2) . . . . ? C141 C142 C143 C144 -167.5(18) . . . . ? C145 C142 C143 C144 68(2) . . . . ? C141 C142 C145 C150 -86(2) . . . . ? C143 C142 C145 C150 38(2) . . . . ? C141 C142 C145 C146 93.4(19) . . . . ? C143 C142 C145 C146 -142.9(16) . . . . ? C150 C145 C146 C147 -2(3) . . . . ? C142 C145 C146 C147 178.7(18) . . . . ? C145 C146 C147 C148 8(4) . . . . ? C146 C147 C148 C149 -10(4) . . . . ? C147 C148 C149 C150 6(4) . . . . ? C146 C145 C150 C149 -2(3) . . . . ? C142 C145 C150 C149 177.6(15) . . . . ? C148 C149 C150 C145 0(3) . . . . ? Dy12 O16 C151 O15 2(3) . . . . ? Dy12 O16 C151 C152 -173.6(14) . . . . ? Dy11 O15 C151 O16 -6(3) . . . . ? Dy11 O15 C151 C152 169.9(11) . . . . ? O16 C151 C152 C153 -68.9(18) . . . . ? O15 C151 C152 C153 114.8(15) . . . . ? O16 C151 C152 C155 54.8(19) . . . . ? O15 C151 C152 C155 -121.5(15) . . . . ? C151 C152 C153 C154 -63.4(17) . . . . ? C155 C152 C153 C154 171.9(14) . . . . ? C153 C152 C155 C156 -112.0(19) . . . . ? C151 C152 C155 C156 125.5(17) . . . . ? C153 C152 C155 C160 68.4(19) . . . . ? C151 C152 C155 C160 -54(2) . . . . ? C160 C155 C156 C157 3(3) . . . . ? C152 C155 C156 C157 -176.1(16) . . . . ? C155 C156 C157 C158 -3(3) . . . . ? C156 C157 C158 C159 1(3) . . . . ? C157 C158 C159 C160 2(3) . . . . ? C158 C159 C160 C155 -2(3) . . . . ? C156 C155 C160 C159 -1(3) . . . . ? C152 C155 C160 C159 178.6(15) . . . . ? Dy11 O17 C171 O18 24(3) . . . . ? Dy11 O17 C171 C172 -155.2(11) . . . . ? Dy12 O18 C171 O17 -2(3) . . . . ? Dy12 O18 C171 C172 177.5(10) . . . . ? O17 C171 C172 C173 -31(2) . . . . ? O18 C171 C172 C173 149.2(14) . . . . ? O17 C171 C172 C175 92.2(17) . . . . ? O18 C171 C172 C175 -87.2(16) . . . . ? C171 C172 C173 C174 -69(2) . . . . ? C175 C172 C173 C174 169.9(16) . . . . ? C171 C172 C175 C180 111.3(18) . . . . ? C173 C172 C175 C180 -126.0(18) . . . . ? C171 C172 C175 C176 -65(2) . . . . ? C173 C172 C175 C176 57(2) . . . . ? C180 C175 C176 C177 2(3) . . . . ? C172 C175 C176 C177 179.1(18) . . . . ? C175 C176 C177 C178 1(3) . . . . ? C176 C177 C178 C179 -4(3) . . . . ? C177 C178 C179 C180 3(3) . . . . ? C176 C175 C180 C179 -3(3) . . . . ? C172 C175 C180 C179 -179.8(18) . . . . ? C178 C179 C180 C175 0(3) . . . . ? N22 N21 B1 N11 54(2) . . . . ? C25 N21 B1 N11 -122.1(19) . . . . ? N22 N21 B1 N31 -67(2) . . . . ? C25 N21 B1 N31 116.5(19) . . . . ? C15 N11 B1 N21 123(2) . . . . ? N12 N11 B1 N21 -64(2) . . . . ? C15 N11 B1 N31 -117(2) . . . . ? N12 N11 B1 N31 56(2) . . . . ? N32 N31 B1 N21 59(2) . . . . ? C35 N31 B1 N21 -117(2) . . . . ? N32 N31 B1 N11 -63(2) . . . . ? C35 N31 B1 N11 121(2) . . . . ? C30 N26 B2 N16 -121.8(19) . . . . ? N27 N26 B2 N16 57.7(19) . . . . ? C30 N26 B2 N36 116.4(19) . . . . ? N27 N26 B2 N36 -64.1(18) . . . . ? C20 N16 B2 N26 118.2(18) . . . . ? N17 N16 B2 N26 -59.5(19) . . . . ? C20 N16 B2 N36 -120.7(18) . . . . ? N17 N16 B2 N36 61.6(19) . . . . ? C40 N36 B2 N26 -112.7(18) . . . . ? N37 N36 B2 N26 62.2(18) . . . . ? C40 N36 B2 N16 124.7(17) . . . . ? N37 N36 B2 N16 -60.4(18) . . . . ? N122 N121 B11 N131 -58.1(18) . . . . ? C125 N121 B11 N131 125.9(17) . . . . ? N122 N121 B11 N111 59.7(19) . . . . ? C125 N121 B11 N111 -116.2(17) . . . . ? C135 N131 B11 N121 -115.2(18) . . . . ? N132 N131 B11 N121 64.2(19) . . . . ? C135 N131 B11 N111 126.1(17) . . . . ? N132 N131 B11 N111 -54(2) . . . . ? C115 N111 B11 N121 120.5(18) . . . . ? N112 N111 B11 N121 -56.1(18) . . . . ? C115 N111 B11 N131 -122.8(17) . . . . ? N112 N111 B11 N131 60.6(18) . . . . ? C140 N136 B12 N126 -116.7(18) . . . . ? N137 N136 B12 N126 60.7(19) . . . . ? C140 N136 B12 N116 124.3(17) . . . . ? N137 N136 B12 N116 -58.3(19) . . . . ? C130 N126 B12 N136 123.7(19) . . . . ? N127 N126 B12 N136 -55(2) . . . . ? C130 N126 B12 N116 -116(2) . . . . ? N127 N126 B12 N116 66.0(19) . . . . ? C120 N116 B12 N136 -125(2) . . . . ? N117 N116 B12 N136 59(2) . . . . ? C120 N116 B12 N126 116(2) . . . . ? N117 N116 B12 N126 -59.9(19) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.085 _refine_diff_density_min -2.057 _refine_diff_density_rms 0.187 #==END #==END data_Gd2RSpba _database_code_CSD 210011 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis(\m-2-phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) digadolinium(III) ; _chemical_name_common ; Tetrakis(mu-2- phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) digadolinium(iii) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H66 B2 Gd2 N12 O8' _chemical_formula_weight 1395.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Gd Gd -0.1653 3.9035 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.610(3) _cell_length_b 12.185(3) _cell_length_c 12.622(3) _cell_angle_alpha 80.72(2) _cell_angle_beta 68.804(17) _cell_angle_gamma 65.780(19) _cell_volume 1518.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 2.228 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.485 _exptl_absorpt_correction_T_max 0.666 _exptl_absorpt_process_details Coppens_numerical _exptl_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.83 _diffrn_reflns_number 9095 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8692 _reflns_number_gt 7521 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS-86 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP _computing_publication_material 'SHELXL-97 and teXsan Ver. 1.11' _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^)+(0.0745P)^2^+2.2276P] 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 except for those bound to the disordered C atoms which were not included ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8692 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1322 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd Gd 0.122286(18) 0.490352(18) 0.083834(16) 0.04183(8) Uani 1 1 d . . . O1 O 0.1766(4) 0.5713(4) -0.0991(3) 0.0634(9) Uani 1 1 d . . . O2 O 0.0251(4) 0.6046(4) -0.1809(3) 0.0597(8) Uani 1 1 d . . . O3 O 0.2507(4) 0.3067(4) -0.0172(4) 0.0687(10) Uani 1 1 d . . . O4 O 0.0816(4) 0.3672(4) -0.0786(3) 0.0648(9) Uani 1 1 d . . . N11 N 0.3130(4) 0.3873(4) 0.2621(3) 0.0513(8) Uani 1 1 d . . . N12 N 0.2660(4) 0.3496(4) 0.1973(4) 0.0526(9) Uani 1 1 d . . . N21 N 0.3227(4) 0.5822(4) 0.1652(4) 0.0530(9) Uani 1 1 d . . . N22 N 0.2745(4) 0.5907(4) 0.0788(4) 0.0534(9) Uani 1 1 d . . . N31 N 0.1210(4) 0.5812(4) 0.3303(3) 0.0507(8) Uani 1 1 d . . . N32 N 0.0393(4) 0.5790(4) 0.2763(3) 0.0528(9) Uani 1 1 d . . . C1 C 0.1313(5) 0.6063(5) -0.1789(4) 0.0510(10) Uani 1 1 d . . . C2A C 0.2202(12) 0.6619(13) -0.2718(9) 0.041(2) Uani 0.50 1 d P . . C2B C 0.1976(17) 0.6511(16) -0.3002(11) 0.065(4) Uani 0.50 1 d P . . C3A C 0.2754(9) 0.5826(8) -0.3807(7) 0.0430(17) Uani 0.50 1 d P . . C3B C 0.339(2) 0.5862(18) -0.3386(16) 0.117(7) Uani 0.50 1 d P . . C4 C 0.3833(7) 0.4556(6) -0.3655(7) 0.084(2) Uani 1 1 d . . . C5 C 0.1400(6) 0.7899(5) -0.2994(4) 0.0562(11) Uani 1 1 d . . . C6A C 0.1634(19) 0.891(2) -0.2874(16) 0.072(5) Uani 0.50 1 d P . . C6B C 0.035(5) 0.849(3) -0.337(4) 0.092(11) Uani 0.50 1 d P . . C7 C 0.073(2) 1.0228(13) -0.3132(15) 0.150(8) Uani 1 1 d . . . C8 C -0.0115(14) 1.0144(17) -0.3481(12) 0.143(5) Uani 1 1 d . . . C9A C -0.0448(14) 0.9379(11) -0.3581(12) 0.075(4) Uani 0.50 1 d P . . C9B C 0.149(5) 0.972(2) -0.281(2) 0.167(19) Uani 0.50 1 d P . . C10A C 0.029(3) 0.817(2) -0.341(3) 0.062(6) Uani 0.50 1 d P . . C10B C 0.205(3) 0.8493(19) -0.2672(17) 0.083(6) Uani 0.50 1 d P . . C13 C 0.3136(6) 0.2295(5) 0.2055(5) 0.0631(13) Uani 1 1 d . . . H13 H 0.2953 0.1801 0.1703 0.076 Uiso 1 1 calc R . . C14 C 0.3941(7) 0.1886(5) 0.2736(5) 0.0744(17) Uani 1 1 d . . . H14 H 0.4400 0.1092 0.2918 0.088 Uiso 1 1 calc R . . C15 C 0.3909(6) 0.2910(5) 0.3083(5) 0.0657(14) Uani 1 1 d . . . H15 H 0.4350 0.2937 0.3557 0.080 Uiso 1 1 calc R . . C23 C 0.3373(6) 0.6477(6) -0.0060(5) 0.0684(15) Uani 1 1 d . . . H23 H 0.3247 0.6646 -0.0765 0.082 Uiso 1 1 calc R . . C24 C 0.4233(7) 0.6785(7) 0.0236(6) 0.0786(18) Uani 1 1 d . . . H24 H 0.4774 0.7192 -0.0205 0.092 Uiso 1 1 calc R . . C25 C 0.4110(6) 0.6355(6) 0.1330(6) 0.0692(15) Uani 1 1 d . . . H25 H 0.4565 0.6423 0.1775 0.082 Uiso 1 1 calc R . . C33 C -0.0865(5) 0.6316(5) 0.3468(4) 0.0605(12) Uani 1 1 d . . . H33 H -0.1631 0.6411 0.3322 0.072 Uiso 1 1 calc R . . C34 C -0.0856(7) 0.6694(6) 0.4436(5) 0.0746(17) Uani 1 1 d . . . H34 H -0.1593 0.7100 0.5043 0.089 Uiso 1 1 calc R . . C35 C 0.0466(7) 0.6344(5) 0.4314(5) 0.0667(14) Uani 1 1 d . . . H35 H 0.0794 0.6457 0.4842 0.080 Uiso 1 1 calc R . . C41 C 0.1905(5) 0.2882(4) -0.0721(4) 0.0508(10) Uani 1 1 d . . . C42 C 0.2505(6) 0.1707(5) -0.1355(5) 0.0635(13) Uani 1 1 d . . . H42 H 0.1873 0.1733 -0.1713 0.077 Uiso 1 1 calc R . . C43 C 0.2638(10) 0.0649(7) -0.0523(7) 0.102(3) Uani 1 1 d . . . H43A H 0.3078 -0.0090 -0.0949 0.126 Uiso 1 1 calc R . . H43B H 0.3207 0.0643 -0.0116 0.126 Uiso 1 1 calc R . . C44 C 0.1341(15) 0.0667(12) 0.0318(11) 0.181(7) Uani 1 1 d . . . H44A H 0.1479 -0.0093 0.0716 0.203 Uiso 1 1 calc R . . H44B H 0.0718 0.0806 -0.0071 0.203 Uiso 1 1 calc R . . H44C H 0.0989 0.1298 0.0851 0.203 Uiso 1 1 calc R . . C45 C 0.3817(5) 0.1528(4) -0.2284(5) 0.0567(11) Uani 1 1 d . . . C46 C 0.4913(6) 0.1493(6) -0.2069(6) 0.0723(16) Uani 1 1 d . . . H46 H 0.4853 0.1571 -0.1328 0.087 Uiso 1 1 calc R . . C47 C 0.6101(7) 0.1342(8) -0.2943(8) 0.103(3) Uani 1 1 d . . . H47 H 0.6824 0.1335 -0.2782 0.120 Uiso 1 1 calc R . . C48 C 0.6232(8) 0.1202(8) -0.4038(8) 0.098(3) Uani 1 1 d . . . H48 H 0.7041 0.1091 -0.4615 0.116 Uiso 1 1 calc R . . C49 C 0.5177(9) 0.1225(6) -0.4275(6) 0.086(2) Uani 1 1 d . . . H49 H 0.5258 0.1132 -0.5018 0.102 Uiso 1 1 calc R . . C50 C 0.3958(7) 0.1390(5) -0.3398(5) 0.0700(15) Uani 1 1 d . . . H50 H 0.3235 0.1406 -0.3568 0.084 Uiso 1 1 calc R . . B1 B 0.2731(5) 0.5212(5) 0.2794(5) 0.0510(11) Uani 1 1 d . . . H1 H 0.3138 0.5295 0.3319 0.061 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 Gd 0.03485(11) 0.05372(13) 0.03599(11) -0.00246(8) -0.00699(7) -0.01940(8) O1 0.062(2) 0.092(3) 0.0439(17) 0.0077(17) -0.0119(15) -0.044(2) O2 0.064(2) 0.077(2) 0.0471(17) 0.0074(16) -0.0123(15) -0.0428(19) O3 0.069(2) 0.074(2) 0.059(2) -0.0222(18) -0.0199(19) -0.0170(19) O4 0.0418(17) 0.069(2) 0.061(2) 0.0054(17) -0.0085(15) -0.0085(15) N11 0.0449(19) 0.058(2) 0.0444(19) 0.0006(16) -0.0154(15) -0.0136(16) N12 0.050(2) 0.056(2) 0.050(2) 0.0011(16) -0.0176(17) -0.0174(17) N21 0.051(2) 0.063(2) 0.053(2) -0.0006(17) -0.0170(17) -0.0291(18) N22 0.055(2) 0.069(2) 0.047(2) 0.0046(17) -0.0162(17) -0.036(2) N31 0.054(2) 0.056(2) 0.0406(18) -0.0070(15) -0.0169(16) -0.0160(17) N32 0.0411(18) 0.066(2) 0.0453(19) -0.0094(17) -0.0093(15) -0.0157(17) C1 0.049(2) 0.061(3) 0.039(2) 0.0011(18) 0.0003(17) -0.031(2) C2A 0.041(4) 0.066(6) 0.026(5) 0.010(4) -0.012(3) -0.033(4) C2B 0.062(9) 0.083(9) 0.033(6) 0.008(6) 0.003(5) -0.031(7) C3A 0.037(4) 0.053(4) 0.028(3) 0.001(3) -0.003(3) -0.014(3) C3B 0.108(14) 0.111(13) 0.089(12) 0.015(10) 0.027(10) -0.057(11) C4 0.058(3) 0.074(4) 0.086(5) 0.008(3) -0.004(3) -0.012(3) C5 0.064(3) 0.069(3) 0.037(2) 0.0062(19) -0.0081(19) -0.036(2) C6A 0.073(9) 0.091(14) 0.056(8) 0.012(7) -0.014(6) -0.046(9) C6B 0.082(13) 0.11(3) 0.071(12) -0.032(17) -0.020(9) -0.022(19) C7 0.178(17) 0.095(8) 0.126(12) 0.023(7) 0.006(10) -0.058(10) C8 0.101(9) 0.170(14) 0.116(9) 0.019(9) -0.008(7) -0.041(9) C9A 0.066(7) 0.048(5) 0.073(8) 0.009(5) -0.011(6) 0.000(5) C9B 0.32(5) 0.091(15) 0.091(15) -0.017(12) 0.02(2) -0.14(3) C10A 0.059(10) 0.048(7) 0.051(9) -0.004(7) -0.012(7) 0.003(7) C10B 0.134(19) 0.080(12) 0.063(9) 0.009(8) -0.041(10) -0.065(12) C13 0.070(3) 0.052(3) 0.056(3) 0.001(2) -0.012(2) -0.020(2) C14 0.072(4) 0.056(3) 0.064(3) 0.008(2) -0.019(3) -0.001(3) C15 0.051(3) 0.073(3) 0.059(3) 0.008(2) -0.023(2) -0.009(2) C23 0.075(4) 0.090(4) 0.057(3) 0.009(3) -0.017(3) -0.055(3) C24 0.080(4) 0.095(4) 0.079(4) 0.006(3) -0.014(3) -0.063(4) C25 0.067(3) 0.083(4) 0.077(4) -0.003(3) -0.026(3) -0.046(3) C33 0.048(2) 0.065(3) 0.048(2) -0.003(2) -0.003(2) -0.013(2) C34 0.069(4) 0.068(3) 0.049(3) -0.011(2) -0.002(2) -0.002(3) C35 0.080(4) 0.067(3) 0.044(2) -0.009(2) -0.020(2) -0.016(3) C41 0.043(2) 0.054(2) 0.040(2) -0.0079(17) -0.0062(17) -0.0084(18) C42 0.056(3) 0.060(3) 0.068(3) -0.021(2) -0.006(2) -0.021(2) C43 0.128(7) 0.070(4) 0.075(5) -0.001(3) 0.001(4) -0.036(4) C44 0.212(15) 0.169(12) 0.124(9) -0.026(8) 0.057(10) -0.126(12) C45 0.052(2) 0.043(2) 0.063(3) -0.0168(19) -0.009(2) -0.0077(18) C46 0.054(3) 0.078(4) 0.074(4) -0.030(3) -0.012(3) -0.013(3) C47 0.055(4) 0.116(6) 0.117(7) -0.054(5) -0.001(4) -0.019(4) C48 0.073(5) 0.089(5) 0.091(5) -0.019(4) 0.007(4) -0.015(4) C49 0.096(5) 0.065(3) 0.057(3) -0.008(3) -0.009(3) -0.004(3) C50 0.073(4) 0.051(3) 0.071(4) -0.011(2) -0.026(3) -0.004(2) B1 0.044(2) 0.066(3) 0.048(2) -0.002(2) -0.018(2) -0.022(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd O4 2.307(4) 2_565 ? Gd O2 2.328(3) 2_565 ? Gd O1 2.329(4) . ? Gd O3 2.380(4) . ? Gd N22 2.508(4) . ? Gd N32 2.510(4) . ? Gd N12 2.522(4) . ? O1 C1 1.239(6) . ? O2 C1 1.250(6) . ? O2 Gd 2.328(3) 2_565 ? O3 C41 1.245(6) . ? O4 C41 1.258(6) . ? O4 Gd 2.307(4) 2_565 ? N11 C15 1.351(6) . ? N11 N12 1.352(6) . ? N11 B1 1.532(7) . ? N12 C13 1.337(7) . ? N21 C25 1.342(7) . ? N21 N22 1.367(6) . ? N21 B1 1.538(7) . ? N22 C23 1.331(7) . ? N31 C35 1.343(6) . ? N31 N32 1.364(6) . ? N31 B1 1.529(7) . ? N32 C33 1.346(6) . ? C1 C2A 1.530(12) . ? C1 C2B 1.568(14) . ? C2A C5 1.514(15) . ? C2A C3A 1.587(15) . ? C2B C3B 1.43(3) . ? C2B C5 1.543(19) . ? C3A C4 1.577(11) . ? C3B C4 1.51(2) . ? C5 C6B 1.35(4) . ? C5 C6A 1.41(2) . ? C5 C10B 1.42(2) . ? C5 C10A 1.46(3) . ? C6A C7 1.57(2) . ? C6B C8 1.86(4) . ? C7 C9B 1.04(5) . ? C7 C8 1.25(2) . ? C8 C9A 1.18(2) . ? C9A C10A 1.40(2) . ? C9B C10B 1.38(3) . ? C13 C14 1.385(9) . ? C13 H13 0.9300 . ? C14 C15 1.370(10) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C23 C24 1.378(8) . ? C23 H23 0.9300 . ? C24 C25 1.374(10) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C33 C34 1.378(9) . ? C33 H33 0.9300 . ? C34 C35 1.369(10) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C41 C42 1.524(7) . ? C42 C45 1.503(7) . ? C42 C43 1.518(10) . ? C42 H42 0.9800 . ? C43 C44 1.491(13) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.376(8) . ? C45 C50 1.386(8) . ? C46 C47 1.382(10) . ? C46 H46 0.9300 . ? C47 C48 1.366(13) . ? C47 H47 0.9300 . ? C48 C49 1.351(12) . ? C48 H48 0.9300 . ? C49 C50 1.405(10) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? B1 H1 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 O4 Gd O2 76.93(15) 2_565 2_565 ? O4 Gd O1 77.46(14) 2_565 . ? O2 Gd O1 133.15(13) 2_565 . ? O4 Gd O3 127.87(15) 2_565 . ? O2 Gd O3 83.94(15) 2_565 . ? O1 Gd O3 81.76(16) . . ? O4 Gd N22 110.26(15) 2_565 . ? O2 Gd N22 151.67(14) 2_565 . ? O1 Gd N22 74.66(13) . . ? O3 Gd N22 109.31(15) . . ? O4 Gd N32 81.34(14) 2_565 . ? O2 Gd N32 81.11(14) 2_565 . ? O1 Gd N32 132.08(15) . . ? O3 Gd N32 142.71(15) . . ? N22 Gd N32 73.30(14) . . ? O4 Gd N12 149.47(14) 2_565 . ? O2 Gd N12 84.71(14) 2_565 . ? O1 Gd N12 131.77(14) . . ? O3 Gd N12 72.98(14) . . ? N22 Gd N12 75.99(14) . . ? N32 Gd N12 71.77(14) . . ? C1 O1 Gd 139.7(3) . . ? C1 O2 Gd 138.3(3) . 2_565 ? C41 O3 Gd 111.7(3) . . ? C41 O4 Gd 177.8(4) . 2_565 ? C15 N11 N12 109.5(5) . . ? C15 N11 B1 128.7(5) . . ? N12 N11 B1 121.8(4) . . ? C13 N12 N11 106.4(4) . . ? C13 N12 Gd 130.1(4) . . ? N11 N12 Gd 123.5(3) . . ? C25 N21 N22 109.5(4) . . ? C25 N21 B1 129.3(5) . . ? N22 N21 B1 121.2(4) . . ? C23 N22 N21 105.7(4) . . ? C23 N22 Gd 130.2(4) . . ? N21 N22 Gd 123.6(3) . . ? C35 N31 N32 109.5(4) . . ? C35 N31 B1 129.1(5) . . ? N32 N31 B1 121.3(4) . . ? C33 N32 N31 106.1(4) . . ? C33 N32 Gd 130.0(4) . . ? N31 N32 Gd 123.8(3) . . ? O1 C1 O2 125.9(4) . . ? O1 C1 C2A 109.0(5) . . ? O2 C1 C2A 124.9(5) . . ? O1 C1 C2B 128.3(8) . . ? O2 C1 C2B 105.6(7) . . ? C2A C1 C2B 21.2(6) . . ? C5 C2A C1 111.2(9) . . ? C5 C2A C3A 108.3(7) . . ? C1 C2A C3A 105.2(8) . . ? C3B C2B C5 119.8(14) . . ? C3B C2B C1 111.0(13) . . ? C5 C2B C1 107.6(9) . . ? C4 C3A C2A 110.2(8) . . ? C2B C3B C4 114.8(17) . . ? C3B C4 C3A 40.5(10) . . ? C6B C5 C6A 97.5(16) . . ? C6B C5 C10B 123.3(17) . . ? C6A C5 C10B 25.9(9) . . ? C6B C5 C10A 17(2) . . ? C6A C5 C10A 114.8(13) . . ? C10B C5 C10A 140.6(14) . . ? C6B C5 C2A 138.0(15) . . ? C6A C5 C2A 124.4(9) . . ? C10B C5 C2A 98.6(10) . . ? C10A C5 C2A 120.8(11) . . ? C6B C5 C2B 117.4(15) . . ? C6A C5 C2B 144.3(11) . . ? C10B C5 C2B 119.1(12) . . ? C10A C5 C2B 100.3(12) . . ? C2A C5 C2B 21.5(6) . . ? C5 C6A C7 122.0(16) . . ? C5 C6B C8 113(2) . . ? C9B C7 C8 142(2) . . ? C9B C7 C6A 35.3(15) . . ? C8 C7 C6A 107.2(16) . . ? C9A C8 C7 137.5(18) . . ? C9A C8 C6B 37.6(17) . . ? C7 C8 C6B 100.1(18) . . ? C8 C9A C10A 121(2) . . ? C7 C9B C10B 129(3) . . ? C9A C10A C5 117(2) . . ? C9B C10B C5 112(2) . . ? N12 C13 C14 110.8(6) . . ? N12 C13 H13 124.6 . . ? C14 C13 H13 124.6 . . ? C15 C14 C13 104.6(5) . . ? C15 C14 H14 127.7 . . ? C13 C14 H14 127.7 . . ? N11 C15 C14 108.7(5) . . ? N11 C15 H15 125.7 . . ? C14 C15 H15 125.7 . . ? N22 C23 C24 111.5(6) . . ? N22 C23 H23 124.2 . . ? C24 C23 H23 124.2 . . ? C25 C24 C23 104.4(5) . . ? C25 C24 H24 127.8 . . ? C23 C24 H24 127.8 . . ? N21 C25 C24 108.8(5) . . ? N21 C25 H25 125.6 . . ? C24 C25 H25 125.6 . . ? N32 C33 C34 110.3(5) . . ? N32 C33 H33 124.8 . . ? C34 C33 H33 124.8 . . ? C35 C34 C33 105.4(5) . . ? C35 C34 H34 127.3 . . ? C33 C34 H34 127.3 . . ? N31 C35 C34 108.7(5) . . ? N31 C35 H35 125.7 . . ? C34 C35 H35 125.7 . . ? O3 C41 O4 120.6(5) . . ? O3 C41 C42 120.1(5) . . ? O4 C41 C42 119.3(5) . . ? C45 C42 C43 110.9(6) . . ? C45 C42 C41 113.6(4) . . ? C43 C42 C41 110.2(5) . . ? C45 C42 H42 107.3 . . ? C43 C42 H42 107.3 . . ? C41 C42 H42 107.3 . . ? C44 C43 C42 114.1(9) . . ? C44 C43 H43A 108.7 . . ? C42 C43 H43A 108.7 . . ? C44 C43 H43B 108.7 . . ? C42 C43 H43B 108.7 . . ? H43A C43 H43B 107.6 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 117.7(6) . . ? C46 C45 C42 122.0(5) . . ? C50 C45 C42 120.3(5) . . ? C45 C46 C47 120.7(7) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C48 C47 C46 121.2(8) . . ? C48 C47 H47 119.4 . . ? C46 C47 H47 119.4 . . ? C49 C48 C47 119.5(7) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C48 C49 C50 120.0(7) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C45 C50 C49 120.9(7) . . ? C45 C50 H50 119.6 . . ? C49 C50 H50 119.6 . . ? N31 B1 N11 109.4(4) . . ? N31 B1 N21 110.0(4) . . ? N11 B1 N21 110.1(4) . . ? N31 B1 H1 109.1 . . ? N11 B1 H1 109.1 . . ? N21 B1 H1 109.1 . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 #_geom_contact_publ_flag Gd Gd 4.0290(9) 2_565 ? Gd O2 3.783(4) . ? Gd O4 2.992(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 O4 Gd O1 C1 -40.1(6) 2_565 . . . ? O2 Gd O1 C1 18.1(7) 2_565 . . . ? O3 Gd O1 C1 91.7(6) . . . . ? N22 Gd O1 C1 -155.5(6) . . . . ? N32 Gd O1 C1 -106.0(6) . . . . ? N12 Gd O1 C1 150.0(5) . . . . ? O4 Gd O3 C41 -4.6(5) 2_565 . . . ? O2 Gd O3 C41 63.7(4) 2_565 . . . ? O1 Gd O3 C41 -71.6(4) . . . . ? N22 Gd O3 C41 -142.1(4) . . . . ? N32 Gd O3 C41 130.3(4) . . . . ? N12 Gd O3 C41 150.0(4) . . . . ? C15 N11 N12 C13 1.0(6) . . . . ? B1 N11 N12 C13 -176.5(4) . . . . ? C15 N11 N12 Gd -177.5(3) . . . . ? B1 N11 N12 Gd 4.9(6) . . . . ? O4 Gd N12 C13 108.8(5) 2_565 . . . ? O2 Gd N12 C13 56.0(5) 2_565 . . . ? O1 Gd N12 C13 -91.0(5) . . . . ? O3 Gd N12 C13 -29.3(5) . . . . ? N22 Gd N12 C13 -144.9(5) . . . . ? N32 Gd N12 C13 138.3(5) . . . . ? O4 Gd N12 N11 -73.0(5) 2_565 . . . ? O2 Gd N12 N11 -125.9(4) 2_565 . . . ? O1 Gd N12 N11 87.2(4) . . . . ? O3 Gd N12 N11 148.9(4) . . . . ? N22 Gd N12 N11 33.2(3) . . . . ? N32 Gd N12 N11 -43.5(3) . . . . ? C25 N21 N22 C23 1.2(6) . . . . ? B1 N21 N22 C23 179.9(5) . . . . ? C25 N21 N22 Gd 174.1(4) . . . . ? B1 N21 N22 Gd -7.2(6) . . . . ? O4 Gd N22 C23 -72.1(6) 2_565 . . . ? O2 Gd N22 C23 -172.3(5) 2_565 . . . ? O1 Gd N22 C23 -2.1(5) . . . . ? O3 Gd N22 C23 73.2(6) . . . . ? N32 Gd N22 C23 -146.0(6) . . . . ? N12 Gd N22 C23 139.2(6) . . . . ? O4 Gd N22 N21 116.8(4) 2_565 . . . ? O2 Gd N22 N21 16.6(6) 2_565 . . . ? O1 Gd N22 N21 -173.1(4) . . . . ? O3 Gd N22 N21 -97.8(4) . . . . ? N32 Gd N22 N21 43.0(4) . . . . ? N12 Gd N22 N21 -31.9(4) . . . . ? C35 N31 N32 C33 -0.3(6) . . . . ? B1 N31 N32 C33 175.8(5) . . . . ? C35 N31 N32 Gd -180.0(4) . . . . ? B1 N31 N32 Gd -3.9(6) . . . . ? O4 Gd N32 C33 28.6(5) 2_565 . . . ? O2 Gd N32 C33 -49.4(5) 2_565 . . . ? O1 Gd N32 C33 93.0(5) . . . . ? O3 Gd N32 C33 -116.9(5) . . . . ? N22 Gd N32 C33 142.9(5) . . . . ? N12 Gd N32 C33 -136.7(5) . . . . ? O4 Gd N32 N31 -151.7(4) 2_565 . . . ? O2 Gd N32 N31 130.3(4) 2_565 . . . ? O1 Gd N32 N31 -87.4(4) . . . . ? O3 Gd N32 N31 62.7(5) . . . . ? N22 Gd N32 N31 -37.4(4) . . . . ? N12 Gd N32 N31 43.0(4) . . . . ? Gd O1 C1 O2 -1.2(9) . . . . ? Gd O1 C1 C2A 174.2(7) . . . . ? Gd O1 C1 C2B -175.6(9) . . . . ? Gd O2 C1 O1 -18.1(9) 2_565 . . . ? Gd O2 C1 C2A 167.2(7) 2_565 . . . ? Gd O2 C1 C2B 157.4(8) 2_565 . . . ? O1 C1 C2A C5 -123.6(6) . . . . ? O2 C1 C2A C5 51.9(10) . . . . ? C2B C1 C2A C5 79(3) . . . . ? O1 C1 C2A C3A 119.4(7) . . . . ? O2 C1 C2A C3A -65.1(11) . . . . ? C2B C1 C2A C3A -38(3) . . . . ? O1 C1 C2B C3B 35.3(19) . . . . ? O2 C1 C2B C3B -140.0(14) . . . . ? C2A C1 C2B C3B 63(3) . . . . ? O1 C1 C2B C5 -97.6(11) . . . . ? O2 C1 C2B C5 87.1(10) . . . . ? C2A C1 C2B C5 -70(3) . . . . ? C5 C2A C3A C4 168.4(7) . . . . ? C1 C2A C3A C4 -72.7(9) . . . . ? C5 C2B C3B C4 -164.3(11) . . . . ? C1 C2B C3B C4 69(2) . . . . ? C2B C3B C4 C3A 40.4(14) . . . . ? C2A C3A C4 C3B -38.0(10) . . . . ? C1 C2A C5 C6B -59(3) . . . . ? C3A C2A C5 C6B 56(3) . . . . ? C1 C2A C5 C6A 119.7(11) . . . . ? C3A C2A C5 C6A -125.2(11) . . . . ? C1 C2A C5 C10B 117.6(11) . . . . ? C3A C2A C5 C10B -127.3(11) . . . . ? C1 C2A C5 C10A -59.8(17) . . . . ? C3A C2A C5 C10A 55.3(18) . . . . ? C1 C2A C5 C2B -79(2) . . . . ? C3A C2A C5 C2B 36(2) . . . . ? C3B C2B C5 C6B 137(3) . . . . ? C1 C2B C5 C6B -95(2) . . . . ? C3B C2B C5 C6A -31(2) . . . . ? C1 C2B C5 C6A 97.4(17) . . . . ? C3B C2B C5 C10B -39(2) . . . . ? C1 C2B C5 C10B 89.2(14) . . . . ? C3B C2B C5 C10A 139(2) . . . . ? C1 C2B C5 C10A -93.1(16) . . . . ? C3B C2B C5 C2A -58(3) . . . . ? C1 C2B C5 C2A 70(2) . . . . ? C6B C5 C6A C7 2(3) . . . . ? C10B C5 C6A C7 -173(5) . . . . ? C10A C5 C6A C7 2(2) . . . . ? C2A C5 C6A C7 -177.7(12) . . . . ? C2B C5 C6A C7 170.5(12) . . . . ? C6A C5 C6B C8 0(3) . . . . ? C10B C5 C6B C8 2(4) . . . . ? C10A C5 C6B C8 -180(13) . . . . ? C2A C5 C6B C8 178.8(9) . . . . ? C2B C5 C6B C8 -173.1(15) . . . . ? C5 C6A C7 C9B 172(3) . . . . ? C5 C6A C7 C8 -3(2) . . . . ? C9B C7 C8 C9A 2(6) . . . . ? C6A C7 C8 C9A 7(3) . . . . ? C9B C7 C8 C6B -3(5) . . . . ? C6A C7 C8 C6B 2(2) . . . . ? C5 C6B C8 C9A -176(5) . . . . ? C5 C6B C8 C7 -1(3) . . . . ? C7 C8 C9A C10A -9(3) . . . . ? C6B C8 C9A C10A -1(4) . . . . ? C8 C7 C9B C10B 6(7) . . . . ? C6A C7 C9B C10B -2(2) . . . . ? C8 C9A C10A C5 6(3) . . . . ? C6B C5 C10A C9A -2(8) . . . . ? C6A C5 C10A C9A -3(3) . . . . ? C10B C5 C10A C9A 0(4) . . . . ? C2A C5 C10A C9A 176.4(17) . . . . ? C2B C5 C10A C9A -176(2) . . . . ? C7 C9B C10B C5 -3(4) . . . . ? C6B C5 C10B C9B -1(3) . . . . ? C6A C5 C10B C9B 5(2) . . . . ? C10A C5 C10B C9B -2(3) . . . . ? C2A C5 C10B C9B -178.4(18) . . . . ? C2B C5 C10B C9B 174.5(16) . . . . ? N11 N12 C13 C14 -1.3(6) . . . . ? Gd N12 C13 C14 177.1(4) . . . . ? N12 C13 C14 C15 1.0(7) . . . . ? N12 N11 C15 C14 -0.4(6) . . . . ? B1 N11 C15 C14 177.0(5) . . . . ? C13 C14 C15 N11 -0.4(7) . . . . ? N21 N22 C23 C24 -1.1(8) . . . . ? Gd N22 C23 C24 -173.4(4) . . . . ? N22 C23 C24 C25 0.6(8) . . . . ? N22 N21 C25 C24 -0.8(7) . . . . ? B1 N21 C25 C24 -179.4(6) . . . . ? C23 C24 C25 N21 0.2(8) . . . . ? N31 N32 C33 C34 1.3(6) . . . . ? Gd N32 C33 C34 -179.0(4) . . . . ? N32 C33 C34 C35 -1.8(7) . . . . ? N32 N31 C35 C34 -0.9(7) . . . . ? B1 N31 C35 C34 -176.5(5) . . . . ? C33 C34 C35 N31 1.6(7) . . . . ? Gd O3 C41 O4 6.7(6) . . . . ? Gd O3 C41 C42 -175.3(4) . . . . ? Gd O4 C41 O3 -82(11) 2_565 . . . ? Gd O4 C41 C42 100(11) 2_565 . . . ? O3 C41 C42 C45 -62.9(7) . . . . ? O4 C41 C42 C45 115.2(6) . . . . ? O3 C41 C42 C43 62.2(8) . . . . ? O4 C41 C42 C43 -119.7(7) . . . . ? C45 C42 C43 C44 -171.0(8) . . . . ? C41 C42 C43 C44 62.3(10) . . . . ? C43 C42 C45 C46 -65.3(8) . . . . ? C41 C42 C45 C46 59.4(8) . . . . ? C43 C42 C45 C50 114.5(7) . . . . ? C41 C42 C45 C50 -120.7(6) . . . . ? C50 C45 C46 C47 1.0(10) . . . . ? C42 C45 C46 C47 -179.2(7) . . . . ? C45 C46 C47 C48 -1.2(13) . . . . ? C46 C47 C48 C49 0.8(14) . . . . ? C47 C48 C49 C50 -0.1(12) . . . . ? C46 C45 C50 C49 -0.3(8) . . . . ? C42 C45 C50 C49 179.8(5) . . . . ? C48 C49 C50 C45 -0.1(10) . . . . ? C35 N31 B1 N11 116.9(6) . . . . ? N32 N31 B1 N11 -58.4(6) . . . . ? C35 N31 B1 N21 -122.1(6) . . . . ? N32 N31 B1 N21 62.7(6) . . . . ? C15 N11 B1 N31 -119.3(5) . . . . ? N12 N11 B1 N31 57.8(6) . . . . ? C15 N11 B1 N21 119.7(5) . . . . ? N12 N11 B1 N21 -63.2(6) . . . . ? C25 N21 B1 N31 122.4(6) . . . . ? N22 N21 B1 N31 -56.1(6) . . . . ? C25 N21 B1 N11 -117.0(6) . . . . ? N22 N21 B1 N11 64.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 3.932 _refine_diff_density_min -2.068 _refine_diff_density_rms 0.126 #==RND data_Ho2RSpba _database_code_CSD 210012 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis(\m-2-phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) diholmium(III) ; _chemical_name_common ;Tetrakis(mu-2- phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) diholmium(iii) ; _chemical_melting_point ? _chemical_formula_moiety 'C58 H64 B2 Ho2 N12 O8' _chemical_formula_sum 'C58 H64 B2 Ho2 N12 O8' _chemical_formula_weight 1408.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ho Ho -0.2175 4.6783 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.587(3) _cell_length_b 12.207(4) _cell_length_c 12.622(3) _cell_angle_alpha 80.31(3) _cell_angle_beta 68.43(2) _cell_angle_gamma 66.11(2) _cell_volume 1517.7(7) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 2.650 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.332 _exptl_absorpt_correction_T_max 0.517 _exptl_absorpt_process_details Coppens_numerical _exptl_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.52 _diffrn_reflns_number 9186 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8782 _reflns_number_gt 5763 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS-86 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP _computing_publication_material 'SHELXL-97 and teXsan Ver. 1.11' _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^)+(0.0840P)^2^+1.5700P] 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 8782 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1523 _refine_ls_wR_factor_gt 0.1322 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho Ho 0.11877(3) 0.49569(3) 0.08773(2) 0.04828(10) Uani 1 1 d . . . O1 O 0.1727(6) 0.5721(6) -0.0948(4) 0.0763(15) Uani 1 1 d . . . O2 O 0.0288(5) 0.5960(5) -0.1791(4) 0.0673(12) Uani 1 1 d . . . O3 O 0.2314(7) 0.3195(6) -0.0142(5) 0.0841(16) Uani 1 1 d . . . O4 O 0.0757(5) 0.3567(6) -0.0864(5) 0.0902(19) Uani 1 1 d . . . N11 N 0.3112(5) 0.3858(5) 0.2608(4) 0.0535(11) Uani 1 1 d . . . N12 N 0.2613(5) 0.3509(5) 0.1957(4) 0.0532(11) Uani 1 1 d . . . N21 N 0.3239(5) 0.5800(5) 0.1634(4) 0.0541(12) Uani 1 1 d . . . N22 N 0.2744(5) 0.5884(5) 0.0786(4) 0.0567(12) Uani 1 1 d . . . N31 N 0.1237(5) 0.5795(5) 0.3308(4) 0.0546(12) Uani 1 1 d . . . N32 N 0.0401(5) 0.5794(5) 0.2787(4) 0.0572(12) Uani 1 1 d . . . C1 C 0.1314(6) 0.6027(6) -0.1758(5) 0.0531(13) Uani 1 1 d . . . C2 C 0.2130(8) 0.6556(8) -0.2807(6) 0.078(2) Uani 1 1 d . . . H2 H 0.2848 0.6559 -0.2575 0.095 Uiso 1 1 calc R . . C3 C 0.2811(13) 0.5832(9) -0.3749(9) 0.118(4) Uani 1 1 d . . . H3A H 0.3278 0.6257 -0.4359 0.125 Uiso 1 1 calc R . . H3B H 0.2151 0.5742 -0.3991 0.125 Uiso 1 1 calc R . . C4 C 0.3818(9) 0.4588(8) -0.3635(8) 0.090(3) Uani 1 1 d . . . H4A H 0.3392 0.4159 -0.3012 0.107 Uiso 1 1 calc R . . H4B H 0.4547 0.4654 -0.3494 0.107 Uiso 1 1 calc R . . H4C H 0.4152 0.4165 -0.4327 0.107 Uiso 1 1 calc R . . C5 C 0.1365(7) 0.7869(6) -0.2986(5) 0.0612(16) Uani 1 1 d . . . C6 C 0.1738(14) 0.8746(12) -0.2815(10) 0.125(5) Uani 1 1 d . . . H6 H 0.2450 0.8548 -0.2549 0.148 Uiso 1 1 calc R . . C7 C 0.098(2) 1.0005(15) -0.3060(16) 0.180(10) Uani 1 1 d . . . H7 H 0.1201 1.0631 -0.2972 0.211 Uiso 1 1 calc R . . C8 C -0.003(2) 1.0186(14) -0.3419(18) 0.173(9) Uani 1 1 d . . . H8 H -0.0527 1.0974 -0.3576 0.205 Uiso 1 1 calc R . . C9 C -0.0399(16) 0.9366(13) -0.3569(13) 0.147(6) Uani 1 1 d . . . H9 H -0.1123 0.9570 -0.3819 0.183 Uiso 1 1 calc R . . C10 C 0.0295(10) 0.8214(9) -0.3356(8) 0.092(3) Uani 1 1 d . . . H10 H 0.0034 0.7626 -0.3465 0.114 Uiso 1 1 calc R . . C13 C 0.3061(7) 0.2320(6) 0.2028(6) 0.0645(16) Uani 1 1 d . . . H13 H 0.2859 0.1849 0.1669 0.078 Uiso 1 1 calc R . . C14 C 0.3856(8) 0.1880(7) 0.2697(7) 0.073(2) Uani 1 1 d . . . H14 H 0.4286 0.1082 0.2879 0.087 Uiso 1 1 calc R . . C15 C 0.3878(7) 0.2876(7) 0.3040(6) 0.0675(18) Uani 1 1 d . . . H15 H 0.4349 0.2872 0.3500 0.080 Uiso 1 1 calc R . . C23 C 0.3368(8) 0.6482(7) -0.0074(7) 0.0702(19) Uani 1 1 d . . . H23 H 0.3220 0.6682 -0.0770 0.084 Uiso 1 1 calc R . . C24 C 0.4258(8) 0.6759(8) 0.0214(7) 0.080(2) Uani 1 1 d . . . H24 H 0.4803 0.7169 -0.0230 0.094 Uiso 1 1 calc R . . C25 C 0.4165(8) 0.6302(7) 0.1283(7) 0.0714(19) Uani 1 1 d . . . H25 H 0.4660 0.6331 0.1707 0.087 Uiso 1 1 calc R . . C33 C -0.0850(7) 0.6333(7) 0.3486(6) 0.0669(18) Uani 1 1 d . . . H33 H -0.1622 0.6445 0.3342 0.080 Uiso 1 1 calc R . . C34 C -0.0824(9) 0.6697(8) 0.4442(7) 0.081(2) Uani 1 1 d . . . H34 H -0.1554 0.7104 0.5052 0.098 Uiso 1 1 calc R . . C35 C 0.0499(8) 0.6337(7) 0.4314(6) 0.0700(19) Uani 1 1 d . . . H35 H 0.0834 0.6449 0.4836 0.084 Uiso 1 1 calc R . . C41 C 0.1820(7) 0.2892(6) -0.0701(5) 0.0566(14) Uani 1 1 d . . . C42 C 0.2525(10) 0.1670(8) -0.1250(10) 0.095(3) Uani 1 1 d . . . H42 H 0.1925 0.1666 -0.1629 0.113 Uiso 1 1 calc R . . C43 C 0.258(2) 0.0686(12) -0.0492(12) 0.171(8) Uani 1 1 d . . . H43A H 0.3032 -0.0022 -0.0955 0.203 Uiso 1 1 calc R . . H43B H 0.3166 0.0652 -0.0092 0.203 Uiso 1 1 calc R . . C44 C 0.146(2) 0.055(2) 0.033(2) 0.278(17) Uani 1 1 d . . . H44A H 0.1728 -0.0164 0.0780 0.309 Uiso 1 1 calc R . . H44B H 0.0890 0.0486 -0.0033 0.309 Uiso 1 1 calc R . . H44C H 0.0975 0.1231 0.0814 0.309 Uiso 1 1 calc R . . C45 C 0.3792(7) 0.1531(6) -0.2204(8) 0.0699(19) Uani 1 1 d . . . C46 C 0.4897(9) 0.1530(8) -0.2044(9) 0.084(2) Uani 1 1 d . . . H46 H 0.4854 0.1620 -0.1312 0.101 Uiso 1 1 calc R . . C47 C 0.6059(10) 0.1401(11) -0.2922(12) 0.121(4) Uani 1 1 d . . . H47 H 0.6784 0.1415 -0.2777 0.146 Uiso 1 1 calc R . . C48 C 0.6175(13) 0.1258(10) -0.3959(12) 0.114(4) Uani 1 1 d . . . H48 H 0.6987 0.1166 -0.4535 0.134 Uiso 1 1 calc R . . C49 C 0.5169(14) 0.1239(8) -0.4230(9) 0.106(4) Uani 1 1 d . . . H49 H 0.5273 0.1143 -0.4980 0.127 Uiso 1 1 calc R . . C50 C 0.3920(12) 0.1370(7) -0.3324(10) 0.101(3) Uani 1 1 d . . . H50 H 0.3206 0.1348 -0.3480 0.122 Uiso 1 1 calc R . . B1 B 0.2731(7) 0.5184(7) 0.2791(6) 0.0560(16) Uani 1 1 d . . . H1 H 0.3156 0.5250 0.3308 0.066 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 Ho 0.04004(13) 0.06825(19) 0.04146(13) 0.00524(10) -0.01277(9) -0.02825(12) O1 0.079(3) 0.118(4) 0.050(2) 0.019(3) -0.025(2) -0.060(3) O2 0.065(3) 0.093(3) 0.059(3) 0.013(2) -0.018(2) -0.052(3) O3 0.101(4) 0.096(4) 0.068(3) -0.013(3) -0.033(3) -0.041(3) O4 0.052(3) 0.111(5) 0.077(4) 0.021(3) -0.017(3) -0.014(3) N11 0.048(3) 0.063(3) 0.048(2) 0.004(2) -0.020(2) -0.017(2) N12 0.052(3) 0.061(3) 0.049(2) 0.002(2) -0.019(2) -0.024(2) N21 0.053(3) 0.072(3) 0.051(3) 0.007(2) -0.022(2) -0.037(3) N22 0.056(3) 0.078(3) 0.045(2) 0.003(2) -0.013(2) -0.039(3) N31 0.053(3) 0.064(3) 0.047(2) -0.001(2) -0.018(2) -0.022(2) N32 0.040(2) 0.075(3) 0.049(3) -0.010(2) -0.007(2) -0.017(2) C1 0.048(3) 0.071(4) 0.040(3) 0.002(2) -0.004(2) -0.033(3) C2 0.061(4) 0.095(5) 0.056(4) 0.021(4) 0.005(3) -0.037(4) C3 0.126(9) 0.082(6) 0.085(6) 0.012(5) 0.016(6) -0.029(6) C4 0.062(5) 0.093(6) 0.080(5) 0.002(5) -0.002(4) -0.018(4) C5 0.069(4) 0.069(4) 0.047(3) 0.003(3) -0.009(3) -0.038(3) C6 0.146(11) 0.153(11) 0.107(8) -0.024(7) 0.002(7) -0.116(10) C7 0.24(2) 0.129(12) 0.168(15) -0.046(10) 0.041(15) -0.144(15) C8 0.20(2) 0.088(9) 0.202(19) 0.010(10) -0.012(15) -0.083(12) C9 0.122(11) 0.109(10) 0.130(11) 0.018(8) -0.012(9) -0.001(8) C10 0.081(6) 0.093(6) 0.078(5) -0.010(5) -0.023(5) -0.009(5) C13 0.067(4) 0.060(4) 0.061(4) 0.004(3) -0.012(3) -0.029(3) C14 0.071(5) 0.062(4) 0.065(4) 0.010(3) -0.018(4) -0.012(4) C15 0.054(4) 0.081(5) 0.058(4) 0.011(3) -0.023(3) -0.017(3) C23 0.076(5) 0.084(5) 0.062(4) 0.013(3) -0.018(3) -0.051(4) C24 0.078(5) 0.106(6) 0.076(5) 0.009(4) -0.015(4) -0.066(5) C25 0.066(4) 0.085(5) 0.082(5) -0.002(4) -0.025(4) -0.046(4) C33 0.048(3) 0.076(4) 0.058(4) 0.006(3) -0.006(3) -0.017(3) C34 0.074(5) 0.076(5) 0.057(4) -0.009(3) 0.002(3) -0.010(4) C35 0.077(5) 0.071(4) 0.049(3) -0.010(3) -0.020(3) -0.012(4) C41 0.053(3) 0.059(4) 0.049(3) -0.004(3) -0.014(3) -0.014(3) C42 0.084(6) 0.069(5) 0.124(8) -0.030(5) -0.004(5) -0.037(5) C43 0.222(19) 0.101(9) 0.113(10) 0.002(7) 0.027(11) -0.061(11) C44 0.29(3) 0.29(3) 0.22(2) -0.08(2) 0.11(2) -0.21(3) C45 0.055(4) 0.048(3) 0.097(5) -0.025(3) -0.022(4) -0.002(3) C46 0.067(5) 0.080(5) 0.100(6) -0.030(5) -0.024(5) -0.014(4) C47 0.064(6) 0.118(9) 0.140(11) -0.056(8) 0.002(6) -0.007(6) C48 0.098(8) 0.080(7) 0.109(9) -0.020(6) -0.003(7) -0.002(6) C49 0.123(9) 0.062(5) 0.081(6) -0.010(4) -0.020(6) 0.006(6) C50 0.121(9) 0.053(4) 0.132(9) -0.014(5) -0.073(8) -0.004(5) B1 0.042(3) 0.076(5) 0.047(3) -0.004(3) -0.009(3) -0.023(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 Ho O4 2.248(5) 2_565 ? Ho O2 2.275(4) 2_565 ? Ho O1 2.293(5) . ? Ho O3 2.326(6) . ? Ho N22 2.450(5) . ? Ho N32 2.478(5) . ? Ho N12 2.488(5) . ? O1 C1 1.225(8) . ? O2 C1 1.240(7) . ? O2 Ho 2.275(4) 2_565 ? O3 C41 1.232(8) . ? O4 C41 1.243(8) . ? O4 Ho 2.248(5) 2_565 ? N11 C15 1.340(8) . ? N11 N12 1.362(7) . ? N11 B1 1.531(10) . ? N12 C13 1.328(9) . ? N21 C25 1.348(8) . ? N21 N22 1.361(7) . ? N21 B1 1.549(9) . ? N22 C23 1.348(8) . ? N31 C35 1.345(8) . ? N31 N32 1.356(7) . ? N31 B1 1.506(9) . ? N32 C33 1.340(8) . ? C1 C2 1.533(8) . ? C2 C3 1.384(13) . ? C2 C5 1.510(11) . ? C2 H2 0.9800 . ? C3 C4 1.517(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.367(12) . ? C5 C6 1.380(12) . ? C6 C7 1.47(2) . ? C6 H6 0.9300 . ? C7 C8 1.34(3) . ? C7 H7 0.9300 . ? C8 C9 1.30(2) . ? C8 H8 0.9300 . ? C9 C10 1.347(15) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C13 C14 1.368(11) . ? C13 H13 0.9300 . ? C14 C15 1.370(12) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C23 C24 1.382(11) . ? C23 H23 0.9300 . ? C24 C25 1.353(12) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C33 C34 1.368(12) . ? C33 H33 0.9300 . ? C34 C35 1.365(12) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C41 C42 1.522(10) . ? C42 C43 1.400(16) . ? C42 C45 1.484(12) . ? C42 H42 0.9800 . ? C43 C44 1.39(2) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.367(11) . ? C45 C50 1.405(13) . ? C46 C47 1.362(14) . ? C46 H46 0.9300 . ? C47 C48 1.300(18) . ? C47 H47 0.9300 . ? C48 C49 1.339(17) . ? C48 H48 0.9300 . ? C49 C50 1.444(17) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? B1 H1 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 O4 Ho O2 78.7(2) 2_565 2_565 ? O4 Ho O1 77.4(2) 2_565 . ? O2 Ho O1 130.26(18) 2_565 . ? O4 Ho O3 127.8(2) 2_565 . ? O2 Ho O3 81.5(2) 2_565 . ? O1 Ho O3 79.7(2) . . ? O4 Ho N22 107.9(2) 2_565 . ? O2 Ho N22 153.97(18) 2_565 . ? O1 Ho N22 75.50(18) . . ? O3 Ho N22 110.7(2) . . ? O4 Ho N32 79.7(2) 2_565 . ? O2 Ho N32 82.43(19) 2_565 . ? O1 Ho N32 134.0(2) . . ? O3 Ho N32 144.0(2) . . ? N22 Ho N32 74.35(18) . . ? O4 Ho N12 149.8(2) 2_565 . ? O2 Ho N12 85.51(18) 2_565 . ? O1 Ho N12 131.30(19) . . ? O3 Ho N12 74.02(19) . . ? N22 Ho N12 76.58(18) . . ? N32 Ho N12 72.71(18) . . ? C1 O1 Ho 141.0(4) . . ? C1 O2 Ho 140.8(4) . 2_565 ? C41 O3 Ho 122.2(5) . . ? C41 O4 Ho 167.3(6) . 2_565 ? C15 N11 N12 108.6(6) . . ? C15 N11 B1 130.0(6) . . ? N12 N11 B1 121.3(5) . . ? C13 N12 N11 106.5(5) . . ? C13 N12 Ho 130.7(5) . . ? N11 N12 Ho 122.8(4) . . ? C25 N21 N22 109.8(5) . . ? C25 N21 B1 129.7(6) . . ? N22 N21 B1 120.5(5) . . ? C23 N22 N21 105.1(5) . . ? C23 N22 Ho 130.6(5) . . ? N21 N22 Ho 124.2(4) . . ? C35 N31 N32 108.8(6) . . ? C35 N31 B1 129.9(6) . . ? N32 N31 B1 121.2(5) . . ? C33 N32 N31 106.9(6) . . ? C33 N32 Ho 129.6(5) . . ? N31 N32 Ho 123.5(4) . . ? O1 C1 O2 125.5(6) . . ? O1 C1 C2 116.7(6) . . ? O2 C1 C2 117.8(6) . . ? C3 C2 C5 118.0(7) . . ? C3 C2 C1 114.7(8) . . ? C5 C2 C1 111.5(6) . . ? C3 C2 H2 103.4 . . ? C5 C2 H2 103.4 . . ? C1 C2 H2 103.4 . . ? C2 C3 C4 118.5(10) . . ? C2 C3 H3A 107.7 . . ? C4 C3 H3A 107.7 . . ? C2 C3 H3B 107.7 . . ? C4 C3 H3B 107.7 . . ? H3A C3 H3B 107.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 118.2(10) . . ? C10 C5 C2 120.1(8) . . ? C6 C5 C2 121.6(10) . . ? C5 C6 C7 118.6(14) . . ? C5 C6 H6 120.7 . . ? C7 C6 H6 120.7 . . ? C8 C7 C6 115.5(12) . . ? C8 C7 H7 122.3 . . ? C6 C7 H7 122.3 . . ? C9 C8 C7 126.2(18) . . ? C9 C8 H8 116.9 . . ? C7 C8 H8 116.9 . . ? C8 C9 C10 118.5(18) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C9 C10 C5 123.0(13) . . ? C9 C10 H10 118.5 . . ? C5 C10 H10 118.5 . . ? N12 C13 C14 111.2(7) . . ? N12 C13 H13 124.4 . . ? C14 C13 H13 124.4 . . ? C13 C14 C15 104.6(6) . . ? C13 C14 H14 127.7 . . ? C15 C14 H14 127.7 . . ? N11 C15 C14 109.2(7) . . ? N11 C15 H15 125.4 . . ? C14 C15 H15 125.4 . . ? N22 C23 C24 111.0(7) . . ? N22 C23 H23 124.5 . . ? C24 C23 H23 124.5 . . ? C25 C24 C23 105.0(6) . . ? C25 C24 H24 127.5 . . ? C23 C24 H24 127.5 . . ? N21 C25 C24 109.0(6) . . ? N21 C25 H25 125.5 . . ? C24 C25 H25 125.5 . . ? N32 C33 C34 110.0(7) . . ? N32 C33 H33 125.0 . . ? C34 C33 H33 125.0 . . ? C35 C34 C33 105.6(7) . . ? C35 C34 H34 127.2 . . ? C33 C34 H34 127.2 . . ? N31 C35 C34 108.7(7) . . ? N31 C35 H35 125.6 . . ? C34 C35 H35 125.6 . . ? O3 C41 O4 122.2(7) . . ? O3 C41 C42 120.4(7) . . ? O4 C41 C42 117.3(8) . . ? C43 C42 C45 114.8(10) . . ? C43 C42 C41 115.5(10) . . ? C45 C42 C41 114.3(7) . . ? C43 C42 H42 103.3 . . ? C45 C42 H42 103.3 . . ? C41 C42 H42 103.3 . . ? C44 C43 C42 123.5(19) . . ? C44 C43 H43A 106.5 . . ? C42 C43 H43A 106.5 . . ? C44 C43 H43B 106.5 . . ? C42 C43 H43B 106.5 . . ? H43A C43 H43B 106.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 116.5(9) . . ? C46 C45 C42 122.3(9) . . ? C50 C45 C42 121.1(9) . . ? C47 C46 C45 122.2(10) . . ? C47 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? C48 C47 C46 121.3(13) . . ? C48 C47 H47 119.4 . . ? C46 C47 H47 119.4 . . ? C47 C48 C49 122.5(12) . . ? C47 C48 H48 118.7 . . ? C49 C48 H48 118.7 . . ? C48 C49 C50 118.0(11) . . ? C48 C49 H49 121.0 . . ? C50 C49 H49 121.0 . . ? C45 C50 C49 119.5(10) . . ? C45 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? N31 B1 N11 110.5(5) . . ? N31 B1 N21 109.8(6) . . ? N11 B1 N21 109.4(5) . . ? N31 B1 H1 109.0 . . ? N11 B1 H1 109.0 . . ? N21 B1 H1 109.0 . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 #_geom_contact_publ_flag Ho Ho 4.0817(11) 2_565 ? Ho O2 3.753(6) . ? Ho O4 3.272(7) . ? 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 O4 Ho O1 C1 -47.1(9) 2_565 . . . ? O2 Ho O1 C1 16.1(10) 2_565 . . . ? O3 Ho O1 C1 85.7(9) . . . . ? N22 Ho O1 C1 -159.6(9) . . . . ? N32 Ho O1 C1 -109.1(8) . . . . ? N12 Ho O1 C1 143.5(8) . . . . ? O4 Ho O3 C41 -7.6(7) 2_565 . . . ? O2 Ho O3 C41 61.0(6) 2_565 . . . ? O1 Ho O3 C41 -72.8(6) . . . . ? N22 Ho O3 C41 -142.8(6) . . . . ? N32 Ho O3 C41 125.5(6) . . . . ? N12 Ho O3 C41 148.7(6) . . . . ? C15 N11 N12 C13 1.5(7) . . . . ? B1 N11 N12 C13 -176.1(6) . . . . ? C15 N11 N12 Ho -177.6(4) . . . . ? B1 N11 N12 Ho 4.9(7) . . . . ? O4 Ho N12 C13 113.0(7) 2_565 . . . ? O2 Ho N12 C13 54.6(6) 2_565 . . . ? O1 Ho N12 C13 -88.0(6) . . . . ? O3 Ho N12 C13 -27.9(6) . . . . ? N22 Ho N12 C13 -144.4(6) . . . . ? N32 Ho N12 C13 138.0(6) . . . . ? O4 Ho N12 N11 -68.2(6) 2_565 . . . ? O2 Ho N12 N11 -126.6(5) 2_565 . . . ? O1 Ho N12 N11 90.8(5) . . . . ? O3 Ho N12 N11 150.9(5) . . . . ? N22 Ho N12 N11 34.4(4) . . . . ? N32 Ho N12 N11 -43.1(4) . . . . ? C25 N21 N22 C23 -1.7(8) . . . . ? B1 N21 N22 C23 178.7(6) . . . . ? C25 N21 N22 Ho 174.0(5) . . . . ? B1 N21 N22 Ho -5.6(8) . . . . ? O4 Ho N22 C23 -70.4(7) 2_565 . . . ? O2 Ho N22 C23 -171.5(6) 2_565 . . . ? O1 Ho N22 C23 1.0(7) . . . . ? O3 Ho N22 C23 73.8(7) . . . . ? N32 Ho N22 C23 -143.8(7) . . . . ? N12 Ho N22 C23 140.7(7) . . . . ? O4 Ho N22 N21 115.1(5) 2_565 . . . ? O2 Ho N22 N21 13.9(8) 2_565 . . . ? O1 Ho N22 N21 -173.6(6) . . . . ? O3 Ho N22 N21 -100.7(5) . . . . ? N32 Ho N22 N21 41.6(5) . . . . ? N12 Ho N22 N21 -33.9(5) . . . . ? C35 N31 N32 C33 -0.3(8) . . . . ? B1 N31 N32 C33 176.0(6) . . . . ? C35 N31 N32 Ho 178.5(5) . . . . ? B1 N31 N32 Ho -5.3(8) . . . . ? O4 Ho N32 C33 29.8(6) 2_565 . . . ? O2 Ho N32 C33 -50.0(6) 2_565 . . . ? O1 Ho N32 C33 91.0(6) . . . . ? O3 Ho N32 C33 -114.2(6) . . . . ? N22 Ho N32 C33 141.9(6) . . . . ? N12 Ho N32 C33 -137.6(6) . . . . ? O4 Ho N32 N31 -148.6(5) 2_565 . . . ? O2 Ho N32 N31 131.6(5) 2_565 . . . ? O1 Ho N32 N31 -87.4(5) . . . . ? O3 Ho N32 N31 67.3(6) . . . . ? N22 Ho N32 N31 -36.6(5) . . . . ? N12 Ho N32 N31 43.9(5) . . . . ? Ho O1 C1 O2 -1.6(14) . . . . ? Ho O1 C1 C2 177.3(6) . . . . ? Ho O2 C1 O1 -17.1(13) 2_565 . . . ? Ho O2 C1 C2 164.1(6) 2_565 . . . ? O1 C1 C2 C3 110.0(10) . . . . ? O2 C1 C2 C3 -71.1(11) . . . . ? O1 C1 C2 C5 -112.4(8) . . . . ? O2 C1 C2 C5 66.5(10) . . . . ? C5 C2 C3 C4 166.9(9) . . . . ? C1 C2 C3 C4 -58.4(14) . . . . ? C3 C2 C5 C10 64.6(12) . . . . ? C1 C2 C5 C10 -71.5(10) . . . . ? C3 C2 C5 C6 -113.7(12) . . . . ? C1 C2 C5 C6 110.2(9) . . . . ? C10 C5 C6 C7 -1.3(15) . . . . ? C2 C5 C6 C7 177.1(10) . . . . ? C5 C6 C7 C8 1(2) . . . . ? C6 C7 C8 C9 0(3) . . . . ? C7 C8 C9 C10 0(3) . . . . ? C8 C9 C10 C5 0(2) . . . . ? C6 C5 C10 C9 0.7(15) . . . . ? C2 C5 C10 C9 -177.7(10) . . . . ? N11 N12 C13 C14 -0.9(8) . . . . ? Ho N12 C13 C14 178.1(5) . . . . ? N12 C13 C14 C15 -0.1(9) . . . . ? N12 N11 C15 C14 -1.5(8) . . . . ? B1 N11 C15 C14 175.7(6) . . . . ? C13 C14 C15 N11 1.0(8) . . . . ? N21 N22 C23 C24 0.9(9) . . . . ? Ho N22 C23 C24 -174.5(6) . . . . ? N22 C23 C24 C25 0.3(11) . . . . ? N22 N21 C25 C24 2.0(9) . . . . ? B1 N21 C25 C24 -178.5(7) . . . . ? C23 C24 C25 N21 -1.4(10) . . . . ? N31 N32 C33 C34 0.9(8) . . . . ? Ho N32 C33 C34 -177.7(5) . . . . ? N32 C33 C34 C35 -1.1(10) . . . . ? N32 N31 C35 C34 -0.4(9) . . . . ? B1 N31 C35 C34 -176.3(7) . . . . ? C33 C34 C35 N31 0.9(10) . . . . ? Ho O3 C41 O4 8.4(10) . . . . ? Ho O3 C41 C42 -173.4(6) . . . . ? Ho O4 C41 O3 -9(3) 2_565 . . . ? Ho O4 C41 C42 173(2) 2_565 . . . ? O3 C41 C42 C43 67.8(15) . . . . ? O4 C41 C42 C43 -113.9(14) . . . . ? O3 C41 C42 C45 -68.6(12) . . . . ? O4 C41 C42 C45 109.7(9) . . . . ? C45 C42 C43 C44 -168.3(18) . . . . ? C41 C42 C43 C44 55(3) . . . . ? C43 C42 C45 C46 -70.3(14) . . . . ? C41 C42 C45 C46 66.5(12) . . . . ? C43 C42 C45 C50 108.5(14) . . . . ? C41 C42 C45 C50 -114.8(9) . . . . ? C50 C45 C46 C47 1.1(14) . . . . ? C42 C45 C46 C47 179.9(10) . . . . ? C45 C46 C47 C48 -0.8(18) . . . . ? C46 C47 C48 C49 1(2) . . . . ? C47 C48 C49 C50 -0.6(18) . . . . ? C46 C45 C50 C49 -1.2(12) . . . . ? C42 C45 C50 C49 180.0(8) . . . . ? C48 C49 C50 C45 1.0(14) . . . . ? C35 N31 B1 N11 118.0(8) . . . . ? N32 N31 B1 N11 -57.4(8) . . . . ? C35 N31 B1 N21 -121.2(7) . . . . ? N32 N31 B1 N21 63.4(8) . . . . ? C15 N11 B1 N31 -119.4(7) . . . . ? N12 N11 B1 N31 57.6(7) . . . . ? C15 N11 B1 N21 119.6(7) . . . . ? N12 N11 B1 N21 -63.4(7) . . . . ? C25 N21 B1 N31 123.3(8) . . . . ? N22 N21 B1 N31 -57.3(8) . . . . ? C25 N21 B1 N11 -115.3(8) . . . . ? N22 N21 B1 N11 64.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.499 _refine_diff_density_min -1.672 _refine_diff_density_rms 0.134 #==END data_Nd2RSpba _database_code_CSD 210013 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis(\m-2-phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) dineodymium(III) ; _chemical_name_common ; Tetrakis(mu-2- phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) dineodymium(iii) ; _chemical_melting_point ? _chemical_formula_moiety 'C58 H64 B N12 Nd2 O8' _chemical_formula_sum 'C58 H64 B N12 Nd2 O8' _chemical_formula_weight 1356.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.661(2) _cell_length_b 12.258(2) _cell_length_c 12.637(2) _cell_angle_alpha 80.239(14) _cell_angle_beta 68.926(13) _cell_angle_gamma 65.244(13) _cell_volume 1530.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 685 _exptl_absorpt_coefficient_mu 1.739 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 0.713 _exptl_absorpt_process_details Coppens_numerical _exptl_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.72 _diffrn_reflns_number 9295 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8911 _reflns_number_gt 5095 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS-86 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP _computing_publication_material 'SHELXL-97 and teXsan Ver. 1.11' _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^)+(0.0955P)^2^+0.5264P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ; geom constr except for those bound to the disordered C atoms which were not included ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8911 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1283 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1674 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.005 _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 Nd Nd 0.12374(3) 0.49205(3) 0.08160(2) 0.04790(11) Uani 1 1 d . . . O1 O 0.1794(5) 0.5779(5) -0.1033(4) 0.0735(13) Uani 1 1 d . . . O2 O 0.0254(5) 0.6063(5) -0.1816(4) 0.0759(14) Uani 1 1 d . . . O3 O 0.2568(5) 0.3032(5) -0.0161(4) 0.0800(15) Uani 1 1 d . . . O4 O 0.0877(5) 0.3672(5) -0.0762(4) 0.0775(14) Uani 1 1 d . . . N11 N 0.3169(5) 0.3901(5) 0.2647(4) 0.0556(12) Uani 1 1 d . . . N12 N 0.2698(5) 0.3516(4) 0.2007(4) 0.0579(12) Uani 1 1 d . . . N21 N 0.3217(5) 0.5854(5) 0.1676(5) 0.0587(12) Uani 1 1 d . . . N22 N 0.2776(5) 0.5928(5) 0.0805(4) 0.0590(12) Uani 1 1 d . . . N31 N 0.1210(5) 0.5823(4) 0.3322(4) 0.0535(11) Uani 1 1 d . . . N32 N 0.0401(5) 0.5817(5) 0.2779(4) 0.0543(11) Uani 1 1 d . . . C1 C 0.1321(6) 0.6074(6) -0.1804(5) 0.0571(14) Uani 1 1 d . . . C2 C 0.2057(9) 0.6590(8) -0.2912(7) 0.108(4) Uani 1 1 d . . . C3A C 0.2785(14) 0.5842(12) -0.3816(10) 0.059(3) Uani 0.50 1 d P . . C3B C 0.3412(16) 0.5851(16) -0.3429(14) 0.081(5) Uani 0.50 1 d P . . C4 C 0.3802(8) 0.4553(8) -0.3651(8) 0.094(3) Uani 1 1 d . . . C5 C 0.1399(7) 0.7916(7) -0.3015(5) 0.0665(17) Uani 1 1 d . . . C6 C 0.1859(15) 0.8649(13) -0.2753(10) 0.142(5) Uani 1 1 d . . . H6 H 0.2588 0.8312 -0.2491 0.170 Uiso 1 1 calc R . . C7 C 0.125(3) 0.994(3) -0.287(2) 0.26(2) Uani 1 1 d . . . H7 H 0.1506 1.0482 -0.2680 0.333 Uiso 1 1 calc R . . C8 C 0.018(4) 1.0262(18) -0.333(2) 0.25(2) Uani 1 1 d . . . H8 H -0.0264 1.1080 -0.3447 0.286 Uiso 1 1 calc R . . C9 C -0.023(2) 0.9604(19) -0.3578(13) 0.213(13) Uani 1 1 d . . . H9 H -0.0931 0.9929 -0.3877 0.245 Uiso 1 1 calc R . . C10 C 0.0347(10) 0.8383(11) -0.3418(8) 0.118(4) Uani 1 1 d . . . H10 H 0.0023 0.7879 -0.3583 0.144 Uiso 1 1 calc R . . C13 C 0.3202(8) 0.2316(6) 0.2093(6) 0.0703(18) Uani 1 1 d . . . H13 H 0.3041 0.1815 0.1737 0.086 Uiso 1 1 calc R . . C14 C 0.3996(8) 0.1922(7) 0.2785(7) 0.082(2) Uani 1 1 d . . . H14 H 0.4460 0.1134 0.2981 0.097 Uiso 1 1 calc R . . C15 C 0.3943(7) 0.2941(7) 0.3111(6) 0.0722(19) Uani 1 1 d . . . H15 H 0.4379 0.2972 0.3586 0.088 Uiso 1 1 calc R . . C23 C 0.3407(8) 0.6500(7) -0.0021(6) 0.0735(19) Uani 1 1 d . . . H23 H 0.3293 0.6676 -0.0731 0.088 Uiso 1 1 calc R . . C24 C 0.4246(9) 0.6802(8) 0.0289(8) 0.087(2) Uani 1 1 d . . . H24 H 0.4792 0.7200 -0.0148 0.102 Uiso 1 1 calc R . . C25 C 0.4104(8) 0.6395(8) 0.1367(8) 0.081(2) Uani 1 1 d . . . H25 H 0.4538 0.6470 0.1825 0.097 Uiso 1 1 calc R . . C33 C -0.0848(6) 0.6317(6) 0.3484(5) 0.0642(16) Uani 1 1 d . . . H33 H -0.1606 0.6399 0.3335 0.077 Uiso 1 1 calc R . . C34 C -0.0867(8) 0.6695(7) 0.4463(6) 0.073(2) Uani 1 1 d . . . H34 H -0.1605 0.7091 0.5069 0.088 Uiso 1 1 calc R . . C35 C 0.0451(8) 0.6351(7) 0.4329(6) 0.0708(18) Uani 1 1 d . . . H35 H 0.0777 0.6465 0.4856 0.084 Uiso 1 1 calc R . . C41 C 0.1969(6) 0.2853(6) -0.0701(5) 0.0575(14) Uani 1 1 d . . . C42 C 0.2551(8) 0.1677(7) -0.1323(7) 0.077(2) Uani 1 1 d . . . H42 H 0.1906 0.1731 -0.1676 0.094 Uiso 1 1 calc R . . C43 C 0.2647(13) 0.0647(9) -0.0520(9) 0.121(4) Uani 1 1 d . . . H43A H 0.3049 -0.0079 -0.0951 0.144 Uiso 1 1 calc R . . H43B H 0.3248 0.0595 -0.0128 0.144 Uiso 1 1 calc R . . C44 C 0.1400(16) 0.0673(14) 0.0325(12) 0.190(9) Uani 1 1 d . . . H44A H 0.1183 0.1157 0.0947 0.215 Uiso 1 1 calc R . . H44B H 0.1493 -0.0130 0.0597 0.215 Uiso 1 1 calc R . . H44C H 0.0701 0.1010 -0.0010 0.215 Uiso 1 1 calc R . . C45 C 0.3835(7) 0.1501(5) -0.2266(6) 0.0629(16) Uani 1 1 d . . . C46 C 0.4950(8) 0.1445(8) -0.2071(7) 0.083(2) Uani 1 1 d . . . H46 H 0.4912 0.1522 -0.1338 0.098 Uiso 1 1 calc R . . C47 C 0.6113(9) 0.1278(11) -0.2951(10) 0.115(4) Uani 1 1 d . . . H47 H 0.6855 0.1225 -0.2793 0.136 Uiso 1 1 calc R . . C48 C 0.6228(12) 0.1186(10) -0.4032(10) 0.111(3) Uani 1 1 d . . . H48 H 0.7023 0.1102 -0.4612 0.131 Uiso 1 1 calc R . . C49 C 0.5173(11) 0.1219(8) -0.4259(7) 0.096(3) Uani 1 1 d . . . H49 H 0.5248 0.1130 -0.5000 0.112 Uiso 1 1 calc R . . C50 C 0.3945(9) 0.1387(6) -0.3379(7) 0.081(2) Uani 1 1 d . . . H50 H 0.3216 0.1420 -0.3545 0.098 Uiso 1 1 calc R . . B1 B 0.2746(7) 0.5230(7) 0.2808(6) 0.0564(16) Uani 1 1 d . . . H1 H 0.3147 0.5319 0.3333 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd 0.03988(15) 0.0616(2) 0.04227(15) -0.00777(11) -0.00774(10) -0.02191(12) O1 0.084(3) 0.093(4) 0.052(2) 0.007(2) -0.022(2) -0.047(3) O2 0.085(3) 0.092(4) 0.066(3) -0.003(3) -0.013(2) -0.057(3) O3 0.079(3) 0.088(4) 0.071(3) -0.031(3) -0.018(3) -0.024(3) O4 0.051(2) 0.086(3) 0.067(3) 0.000(2) -0.008(2) -0.010(2) N11 0.051(3) 0.057(3) 0.048(2) 0.000(2) -0.016(2) -0.011(2) N12 0.060(3) 0.049(3) 0.058(3) -0.004(2) -0.015(2) -0.017(2) N21 0.057(3) 0.072(3) 0.059(3) 0.000(2) -0.022(2) -0.034(3) N22 0.066(3) 0.069(3) 0.052(3) 0.003(2) -0.017(2) -0.039(3) N31 0.060(3) 0.053(3) 0.047(2) -0.007(2) -0.017(2) -0.019(2) N32 0.049(3) 0.064(3) 0.043(2) -0.007(2) -0.0104(19) -0.018(2) C1 0.055(3) 0.065(4) 0.048(3) -0.006(3) 0.003(2) -0.034(3) C2 0.088(6) 0.088(6) 0.075(5) 0.025(4) 0.026(4) -0.018(5) C3A 0.057(7) 0.066(8) 0.038(5) 0.008(5) -0.006(5) -0.021(6) C3B 0.058(8) 0.096(12) 0.067(9) 0.013(8) 0.013(7) -0.040(8) C4 0.064(5) 0.085(6) 0.088(6) 0.000(4) 0.006(4) -0.013(4) C5 0.072(4) 0.077(4) 0.042(3) 0.010(3) -0.010(3) -0.032(4) C6 0.185(13) 0.166(12) 0.107(8) -0.026(8) 0.013(8) -0.140(11) C7 0.42(5) 0.27(3) 0.150(19) -0.076(19) 0.07(2) -0.29(4) C8 0.40(5) 0.086(10) 0.15(2) 0.001(11) 0.06(2) -0.093(19) C9 0.165(16) 0.183(17) 0.093(9) 0.015(12) 0.007(10) 0.068(14) C10 0.081(6) 0.141(9) 0.072(5) -0.018(6) -0.017(4) 0.012(6) C13 0.083(5) 0.051(4) 0.062(4) -0.001(3) -0.010(3) -0.023(3) C14 0.073(5) 0.058(4) 0.081(5) 0.009(4) -0.016(4) -0.005(4) C15 0.060(4) 0.073(5) 0.064(4) 0.008(3) -0.024(3) -0.008(3) C23 0.088(5) 0.089(5) 0.056(4) 0.006(3) -0.012(3) -0.058(4) C24 0.089(6) 0.097(6) 0.091(6) 0.011(5) -0.017(4) -0.068(5) C25 0.081(5) 0.100(6) 0.092(5) -0.006(4) -0.029(4) -0.060(5) C33 0.049(3) 0.068(4) 0.058(3) -0.008(3) -0.006(3) -0.013(3) C34 0.074(4) 0.068(4) 0.047(3) -0.011(3) -0.002(3) -0.010(3) C35 0.087(5) 0.070(4) 0.051(3) -0.012(3) -0.025(3) -0.020(4) C41 0.048(3) 0.056(3) 0.048(3) -0.008(2) -0.005(2) -0.008(3) C42 0.073(5) 0.066(4) 0.089(5) -0.022(4) -0.013(4) -0.028(4) C43 0.153(10) 0.086(6) 0.083(6) 0.001(5) 0.004(6) -0.045(7) C44 0.232(19) 0.151(13) 0.126(11) -0.022(9) 0.054(12) -0.105(13) C45 0.056(3) 0.042(3) 0.072(4) -0.018(3) -0.011(3) -0.004(3) C46 0.070(4) 0.092(5) 0.079(5) -0.037(4) -0.015(4) -0.019(4) C47 0.060(5) 0.129(9) 0.135(9) -0.054(7) -0.005(5) -0.020(5) C48 0.108(8) 0.100(7) 0.092(7) -0.021(6) 0.009(6) -0.038(6) C49 0.116(8) 0.068(5) 0.058(4) -0.011(3) -0.010(5) -0.005(5) C50 0.093(6) 0.053(4) 0.086(5) -0.016(3) -0.044(4) 0.002(4) B1 0.050(3) 0.068(4) 0.059(4) -0.008(3) -0.018(3) -0.027(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 Nd O4 2.362(5) 2_565 ? Nd O1 2.374(5) . ? Nd O2 2.395(5) 2_565 ? Nd O3 2.423(5) . ? Nd N22 2.565(5) . ? Nd N32 2.568(5) . ? Nd N12 2.577(5) . ? O1 C1 1.219(8) . ? O2 C1 1.255(8) . ? O2 Nd 2.395(5) 2_565 ? O3 C41 1.235(8) . ? O4 C41 1.268(8) . ? O4 Nd 2.362(5) 2_565 ? N11 C15 1.341(8) . ? N11 N12 1.358(7) . ? N11 B1 1.519(9) . ? N12 C13 1.338(8) . ? N21 N22 1.348(7) . ? N21 C25 1.364(8) . ? N21 B1 1.533(9) . ? N22 C23 1.324(8) . ? N31 C35 1.346(8) . ? N31 N32 1.355(7) . ? N31 B1 1.547(8) . ? N32 C33 1.341(7) . ? C1 C2 1.545(9) . ? C2 C3A 1.368(16) . ? C2 C3B 1.416(17) . ? C2 C5 1.484(11) . ? C3A C4 1.563(16) . ? C3B C4 1.51(2) . ? C5 C6 1.357(13) . ? C5 C10 1.361(12) . ? C6 C7 1.44(3) . ? C6 H6 0.9300 . ? C7 C8 1.44(5) . ? C7 H7 0.9300 . ? C8 C9 1.22(4) . ? C8 H8 0.9300 . ? C9 C10 1.37(2) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C13 C14 1.386(11) . ? C13 H13 0.9300 . ? C14 C15 1.351(12) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C23 C24 1.370(11) . ? C23 H23 0.9300 . ? C24 C25 1.345(12) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C33 C34 1.382(10) . ? C33 H33 0.9300 . ? C34 C35 1.365(11) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C41 C42 1.529(9) . ? C42 C43 1.471(13) . ? C42 C45 1.498(10) . ? C42 H42 0.9800 . ? C43 C44 1.453(15) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.381(11) . ? C45 C50 1.391(10) . ? C46 C47 1.370(12) . ? C46 H46 0.9300 . ? C47 C48 1.343(15) . ? C47 H47 0.9300 . ? C48 C49 1.344(15) . ? C48 H48 0.9300 . ? C49 C50 1.419(13) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? B1 H1 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 O4 Nd O1 78.51(18) 2_565 . ? O4 Nd O2 75.52(19) 2_565 2_565 ? O1 Nd O2 134.51(18) . 2_565 ? O4 Nd O3 127.73(19) 2_565 . ? O1 Nd O3 83.86(19) . . ? O2 Nd O3 83.38(19) 2_565 . ? O4 Nd N22 112.5(2) 2_565 . ? O1 Nd N22 74.58(17) . . ? O2 Nd N22 150.41(17) 2_565 . ? O3 Nd N22 109.29(18) . . ? O4 Nd N32 82.13(17) 2_565 . ? O1 Nd N32 130.98(18) . . ? O2 Nd N32 81.27(17) 2_565 . ? O3 Nd N32 141.12(18) . . ? N22 Nd N32 72.18(17) . . ? O4 Nd N12 148.34(17) 2_565 . ? O1 Nd N12 131.70(18) . . ? O2 Nd N12 84.74(18) 2_565 . ? O3 Nd N12 72.74(17) . . ? N22 Nd N12 74.38(17) . . ? N32 Nd N12 70.44(16) . . ? O4 Nd C41 105.68(19) 2_565 . ? O1 Nd C41 77.75(18) . . ? O2 Nd C41 74.26(17) 2_565 . ? O3 Nd C41 22.06(17) . . ? N22 Nd C41 126.28(17) . . ? N32 Nd C41 151.21(17) . . ? N12 Nd C41 92.11(16) . . ? C1 O1 Nd 135.8(4) . . ? C1 O2 Nd 138.3(5) . 2_565 ? C41 O3 Nd 110.4(4) . . ? C41 O4 Nd 175.3(5) . 2_565 ? C15 N11 N12 108.7(6) . . ? C15 N11 B1 129.7(6) . . ? N12 N11 B1 121.4(5) . . ? C13 N12 N11 106.2(6) . . ? C13 N12 Nd 129.7(5) . . ? N11 N12 Nd 124.0(4) . . ? N22 N21 C25 109.5(6) . . ? N22 N21 B1 122.2(5) . . ? C25 N21 B1 128.3(6) . . ? C23 N22 N21 105.2(6) . . ? C23 N22 Nd 130.6(5) . . ? N21 N22 Nd 123.9(4) . . ? C35 N31 N32 108.8(5) . . ? C35 N31 B1 129.7(6) . . ? N32 N31 B1 121.5(5) . . ? C33 N32 N31 106.1(5) . . ? C33 N32 Nd 129.7(4) . . ? N31 N32 Nd 124.2(3) . . ? O1 C1 O2 128.4(6) . . ? O1 C1 C2 118.2(7) . . ? O2 C1 C2 113.3(7) . . ? C3A C2 C3B 42.9(9) . . ? C3A C2 C5 124.2(8) . . ? C3B C2 C5 127.8(9) . . ? C3A C2 C1 116.9(9) . . ? C3B C2 C1 115.4(9) . . ? C5 C2 C1 112.5(6) . . ? C2 C3A C4 119.4(10) . . ? C2 C3B C4 120.1(13) . . ? C3B C4 C3A 38.8(8) . . ? C6 C5 C10 120.4(11) . . ? C6 C5 C2 121.0(11) . . ? C10 C5 C2 118.5(10) . . ? C5 C6 C7 121.7(18) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C8 C7 C6 109.8(17) . . ? C8 C7 H7 125.1 . . ? C6 C7 H7 125.1 . . ? C9 C8 C7 129(3) . . ? C9 C8 H8 115.7 . . ? C7 C8 H8 115.7 . . ? C8 C9 C10 120(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C5 C10 C9 119.5(17) . . ? C5 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? N12 C13 C14 110.6(7) . . ? N12 C13 H13 124.7 . . ? C14 C13 H13 124.7 . . ? C15 C14 C13 104.4(6) . . ? C15 C14 H14 127.8 . . ? C13 C14 H14 127.8 . . ? N11 C15 C14 110.0(7) . . ? N11 C15 H15 125.0 . . ? C14 C15 H15 125.0 . . ? N22 C23 C24 112.3(7) . . ? N22 C23 H23 123.8 . . ? C24 C23 H23 123.8 . . ? C25 C24 C23 104.6(6) . . ? C25 C24 H24 127.7 . . ? C23 C24 H24 127.7 . . ? C24 C25 N21 108.4(6) . . ? C24 C25 H25 125.8 . . ? N21 C25 H25 125.8 . . ? N32 C33 C34 111.4(6) . . ? N32 C33 H33 124.3 . . ? C34 C33 H33 124.3 . . ? C35 C34 C33 103.7(6) . . ? C35 C34 H34 128.2 . . ? C33 C34 H34 128.2 . . ? N31 C35 C34 110.0(6) . . ? N31 C35 H35 125.0 . . ? C34 C35 H35 125.0 . . ? O3 C41 O4 119.2(6) . . ? O3 C41 C42 120.7(6) . . ? O4 C41 C42 120.0(7) . . ? C43 C42 C45 112.8(8) . . ? C43 C42 C41 111.1(7) . . ? C45 C42 C41 113.3(6) . . ? C43 C42 H42 106.4 . . ? C45 C42 H42 106.4 . . ? C41 C42 H42 106.4 . . ? C44 C43 C42 116.1(11) . . ? C44 C43 H43A 108.3 . . ? C42 C43 H43A 108.3 . . ? C44 C43 H43B 108.3 . . ? C42 C43 H43B 108.3 . . ? H43A C43 H43B 107.4 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 117.5(7) . . ? C46 C45 C42 121.7(7) . . ? C50 C45 C42 120.8(7) . . ? C47 C46 C45 120.3(8) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C48 C47 C46 122.8(10) . . ? C48 C47 H47 118.6 . . ? C46 C47 H47 118.6 . . ? C47 C48 C49 118.8(10) . . ? C47 C48 H48 120.6 . . ? C49 C48 H48 120.6 . . ? C48 C49 C50 120.7(9) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C45 C50 C49 119.8(9) . . ? C45 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? N11 B1 N21 110.8(5) . . ? N11 B1 N31 109.5(5) . . ? N21 B1 N31 109.9(5) . . ? N11 B1 H1 108.9 . . ? N21 B1 H1 108.9 . . ? N31 B1 H1 108.9 . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 #_geom_contact_publ_flag Nd Nd 4.0363(9) 2_565 ? Nd O2 3.763(6) . ? Nd O4 2.945(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 O4 Nd O1 C1 -42.2(7) 2_565 . . . ? O2 Nd O1 C1 13.9(8) 2_565 . . . ? O3 Nd O1 C1 88.3(7) . . . . ? N22 Nd O1 C1 -159.7(7) . . . . ? N32 Nd O1 C1 -111.0(7) . . . . ? N12 Nd O1 C1 148.6(6) . . . . ? O4 Nd O3 C41 -2.1(6) 2_565 . . . ? O1 Nd O3 C41 -72.4(5) . . . . ? O2 Nd O3 C41 63.8(5) 2_565 . . . ? N22 Nd O3 C41 -143.7(5) . . . . ? N32 Nd O3 C41 131.1(5) . . . . ? N12 Nd O3 C41 150.4(5) . . . . ? C15 N11 N12 C13 -0.1(7) . . . . ? B1 N11 N12 C13 -176.7(6) . . . . ? C15 N11 N12 Nd -177.0(4) . . . . ? B1 N11 N12 Nd 6.4(7) . . . . ? O4 Nd N12 C13 108.1(6) 2_565 . . . ? O1 Nd N12 C13 -92.5(6) . . . . ? O2 Nd N12 C13 56.9(6) 2_565 . . . ? O3 Nd N12 C13 -27.7(6) . . . . ? N22 Nd N12 C13 -144.2(6) . . . . ? N32 Nd N12 C13 139.5(6) . . . . ? O4 Nd N12 N11 -75.7(6) 2_565 . . . ? O1 Nd N12 N11 83.7(5) . . . . ? O2 Nd N12 N11 -126.8(4) 2_565 . . . ? O3 Nd N12 N11 148.5(5) . . . . ? N22 Nd N12 N11 32.0(4) . . . . ? N32 Nd N12 N11 -44.3(4) . . . . ? C25 N21 N22 C23 0.6(8) . . . . ? B1 N21 N22 C23 -179.0(6) . . . . ? C25 N21 N22 Nd 174.7(5) . . . . ? B1 N21 N22 Nd -4.9(8) . . . . ? O4 Nd N22 C23 -72.8(7) 2_565 . . . ? O1 Nd N22 C23 -2.6(6) . . . . ? O2 Nd N22 C23 -173.3(6) 2_565 . . . ? O3 Nd N22 C23 75.0(7) . . . . ? N32 Nd N22 C23 -146.0(7) . . . . ? N12 Nd N22 C23 139.9(7) . . . . ? O4 Nd N22 N21 114.7(5) 2_565 . . . ? O1 Nd N22 N21 -175.1(5) . . . . ? O2 Nd N22 N21 14.2(7) 2_565 . . . ? O3 Nd N22 N21 -97.5(5) . . . . ? N32 Nd N22 N21 41.5(5) . . . . ? N12 Nd N22 N21 -32.6(5) . . . . ? C35 N31 N32 C33 -1.7(7) . . . . ? B1 N31 N32 C33 175.5(6) . . . . ? C35 N31 N32 Nd -179.6(4) . . . . ? B1 N31 N32 Nd -2.5(8) . . . . ? O4 Nd N32 C33 28.3(6) 2_565 . . . ? O1 Nd N32 C33 95.5(6) . . . . ? O2 Nd N32 C33 -48.2(6) 2_565 . . . ? O3 Nd N32 C33 -116.1(6) . . . . ? N22 Nd N32 C33 145.1(6) . . . . ? N12 Nd N32 C33 -135.7(6) . . . . ? O4 Nd N32 N31 -154.3(5) 2_565 . . . ? O1 Nd N32 N31 -87.0(5) . . . . ? O2 Nd N32 N31 129.3(5) 2_565 . . . ? O3 Nd N32 N31 61.4(6) . . . . ? N22 Nd N32 N31 -37.5(4) . . . . ? N12 Nd N32 N31 41.8(4) . . . . ? Nd O1 C1 O2 4.6(12) . . . . ? Nd O1 C1 C2 -178.6(5) . . . . ? Nd O2 C1 O1 -21.9(12) 2_565 . . . ? Nd O2 C1 C2 161.1(6) 2_565 . . . ? O1 C1 C2 C3A 103.5(12) . . . . ? O2 C1 C2 C3A -79.2(12) . . . . ? O1 C1 C2 C3B 55.4(15) . . . . ? O2 C1 C2 C3B -127.3(13) . . . . ? O1 C1 C2 C5 -103.2(9) . . . . ? O2 C1 C2 C5 74.1(11) . . . . ? C5 C2 C3A C4 160.0(11) . . . . ? C1 C2 C3A C4 -50.2(17) . . . . ? C5 C2 C3B C4 -154.1(12) . . . . ? C1 C2 C3B C4 51(2) . . . . ? C3A C2 C5 C6 -109.6(14) . . . . ? C3B C2 C5 C6 -56.0(18) . . . . ? C1 C2 C5 C6 99.4(10) . . . . ? C3A C2 C5 C10 68.1(15) . . . . ? C3B C2 C5 C10 121.7(16) . . . . ? C1 C2 C5 C10 -82.9(11) . . . . ? C10 C5 C6 C7 1.0(17) . . . . ? C2 C5 C6 C7 178.7(13) . . . . ? C5 C6 C7 C8 -2(3) . . . . ? C6 C7 C8 C9 1(4) . . . . ? C7 C8 C9 C10 1(4) . . . . ? C6 C5 C10 C9 1.2(14) . . . . ? C2 C5 C10 C9 -176.5(10) . . . . ? C8 C9 C10 C5 -2(3) . . . . ? N11 N12 C13 C14 0.0(8) . . . . ? Nd N12 C13 C14 176.7(5) . . . . ? N12 C13 C14 C15 0.1(9) . . . . ? N12 N11 C15 C14 0.1(8) . . . . ? B1 N11 C15 C14 176.3(6) . . . . ? C13 C14 C15 N11 -0.1(9) . . . . ? N21 N22 C23 C24 -0.1(9) . . . . ? Nd N22 C23 C24 -173.7(6) . . . . ? N22 C23 C24 C25 -0.4(11) . . . . ? C23 C24 C25 N21 0.8(10) . . . . ? N22 N21 C25 C24 -0.9(9) . . . . ? B1 N21 C25 C24 178.7(7) . . . . ? N31 N32 C33 C34 2.5(8) . . . . ? Nd N32 C33 C34 -179.7(5) . . . . ? N32 C33 C34 C35 -2.3(9) . . . . ? N32 N31 C35 C34 0.2(8) . . . . ? B1 N31 C35 C34 -176.6(6) . . . . ? C33 C34 C35 N31 1.2(9) . . . . ? Nd O3 C41 O4 6.5(8) . . . . ? Nd O3 C41 C42 -175.5(5) . . . . ? Nd O4 C41 O3 -124(6) 2_565 . . . ? Nd O4 C41 C42 58(6) 2_565 . . . ? O3 C41 C42 C43 63.8(11) . . . . ? O4 C41 C42 C43 -118.2(9) . . . . ? O3 C41 C42 C45 -64.3(10) . . . . ? O4 C41 C42 C45 113.7(8) . . . . ? C45 C42 C43 C44 -171.5(11) . . . . ? C41 C42 C43 C44 60.0(15) . . . . ? C43 C42 C45 C46 -66.9(11) . . . . ? C41 C42 C45 C46 60.4(10) . . . . ? C43 C42 C45 C50 113.1(10) . . . . ? C41 C42 C45 C50 -119.6(8) . . . . ? C50 C45 C46 C47 -0.3(13) . . . . ? C42 C45 C46 C47 179.7(8) . . . . ? C45 C46 C47 C48 1.5(17) . . . . ? C46 C47 C48 C49 -2.4(18) . . . . ? C47 C48 C49 C50 2.1(16) . . . . ? C46 C45 C50 C49 0.1(11) . . . . ? C42 C45 C50 C49 -179.9(7) . . . . ? C48 C49 C50 C45 -1.0(13) . . . . ? C15 N11 B1 N21 120.3(7) . . . . ? N12 N11 B1 N21 -63.9(7) . . . . ? C15 N11 B1 N31 -118.4(7) . . . . ? N12 N11 B1 N31 57.4(7) . . . . ? N22 N21 B1 N11 63.5(8) . . . . ? C25 N21 B1 N11 -115.9(8) . . . . ? N22 N21 B1 N31 -57.6(8) . . . . ? C25 N21 B1 N31 122.9(7) . . . . ? C35 N31 B1 N11 116.4(7) . . . . ? N32 N31 B1 N11 -60.1(7) . . . . ? C35 N31 B1 N21 -121.7(7) . . . . ? N32 N31 B1 N21 61.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.610 _refine_diff_density_min -1.300 _refine_diff_density_rms 0.121 #==END data_Dy2RSpba _database_code_CSD 210014 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis(\m-2-phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) didysprosium(III) ; _chemical_name_common ; Tetrakis(mu-2- phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) didysprosium(iii) ; _chemical_melting_point ? _chemical_formula_moiety 'C58 H64 B2 Dy2 N12 O8' _chemical_formula_sum 'C58 H64 B2 Dy2 N12 O8' _chemical_formula_weight 1403.83 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.589(5) _cell_length_b 12.174(5) _cell_length_c 12.633(4) _cell_angle_alpha 80.52(3) _cell_angle_beta 68.49(3) _cell_angle_gamma 66.12(3) _cell_volume 1515.9(10) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 702 _exptl_absorpt_coefficient_mu 2.508 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min Coppens_numerical _exptl_absorpt_correction_T_max 0.374 _exptl_absorpt_process_details 0.627 _exptl_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.02 _diffrn_reflns_number 9214 _diffrn_reflns_av_R_equivalents 0.0128 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 30.01 _reflns_number_total 8830 _reflns_number_gt 6811 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS-86 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP _computing_publication_material 'SHELXL-97 and teXsan Ver. 1.11' _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^)+(0.1091P)^2^+2.2171P] 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 8830 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1712 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.015 _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 Dy Dy 0.11968(3) 0.49388(3) 0.08666(2) 0.04544(11) Uani 1 1 d . . . O1 O 0.1749(6) 0.5710(6) -0.0961(5) 0.0690(14) Uani 1 1 d . . . O2 O 0.0283(6) 0.5987(6) -0.1801(5) 0.0665(14) Uani 1 1 d . . . O3 O 0.2379(8) 0.3153(7) -0.0156(6) 0.0816(18) Uani 1 1 d . . . O4 O 0.0775(6) 0.3607(6) -0.0838(6) 0.0797(18) Uani 1 1 d . . . N11 N 0.3122(6) 0.3853(5) 0.2616(5) 0.0528(12) Uani 1 1 d . . . N12 N 0.2615(6) 0.3508(5) 0.1963(5) 0.0515(12) Uani 1 1 d . . . N21 N 0.3236(6) 0.5801(6) 0.1647(5) 0.0531(12) Uani 1 1 d . . . N22 N 0.2744(6) 0.5893(6) 0.0785(5) 0.0539(13) Uani 1 1 d . . . N31 N 0.1229(6) 0.5800(5) 0.3303(5) 0.0515(12) Uani 1 1 d . . . N32 N 0.0398(5) 0.5796(6) 0.2781(5) 0.0538(13) Uani 1 1 d . . . C1 C 0.1315(6) 0.6045(7) -0.1762(5) 0.0504(14) Uani 1 1 d . . . C2 C 0.2137(9) 0.6576(9) -0.2802(7) 0.079(3) Uani 1 1 d . . . H2 H 0.2861 0.6574 -0.2575 0.096 Uiso 1 1 calc R . . C3 C 0.2805(14) 0.5842(10) -0.3763(9) 0.106(4) Uani 1 1 d . . . H3A H 0.3267 0.6263 -0.4380 0.117 Uiso 1 1 calc R . . H3B H 0.2135 0.5750 -0.3990 0.117 Uiso 1 1 calc R . . C4 C 0.3825(10) 0.4580(10) -0.3637(10) 0.091(3) Uani 1 1 d . . . H4A H 0.3411 0.4174 -0.2984 0.109 Uiso 1 1 calc R . . H4B H 0.4577 0.4649 -0.3543 0.109 Uiso 1 1 calc R . . H4C H 0.4122 0.4129 -0.4307 0.109 Uiso 1 1 calc R . . C5 C 0.1371(8) 0.7888(7) -0.2983(6) 0.0606(17) Uani 1 1 d . . . C6 C 0.1763(17) 0.8754(14) -0.2807(12) 0.119(5) Uani 1 1 d . . . H6 H 0.2483 0.8541 -0.2550 0.138 Uiso 1 1 calc R . . C7 C 0.103(3) 1.000(2) -0.303(2) 0.192(14) Uani 1 1 d . . . H7 H 0.1234 1.0627 -0.2914 0.228 Uiso 1 1 calc R . . C8 C 0.000(3) 1.0202(16) -0.3437(19) 0.176(11) Uani 1 1 d . . . H8 H -0.0454 1.0989 -0.3630 0.197 Uiso 1 1 calc R . . C9 C -0.0375(17) 0.9387(15) -0.3569(14) 0.141(7) Uani 1 1 d . . . H9 H -0.1108 0.9602 -0.3809 0.167 Uiso 1 1 calc R . . C10 C 0.0298(10) 0.8222(10) -0.3359(9) 0.085(3) Uani 1 1 d . . . H10 H 0.0033 0.7636 -0.3470 0.106 Uiso 1 1 calc R . . C13 C 0.3078(8) 0.2304(7) 0.2035(7) 0.0610(17) Uani 1 1 d . . . H13 H 0.2890 0.1820 0.1676 0.074 Uiso 1 1 calc R . . C14 C 0.3871(9) 0.1884(7) 0.2716(7) 0.069(2) Uani 1 1 d . . . H14 H 0.4311 0.1088 0.2900 0.082 Uiso 1 1 calc R . . C15 C 0.3871(7) 0.2891(8) 0.3062(7) 0.0628(18) Uani 1 1 d . . . H15 H 0.4323 0.2900 0.3534 0.076 Uiso 1 1 calc R . . C23 C 0.3369(9) 0.6478(8) -0.0063(7) 0.068(2) Uani 1 1 d . . . H23 H 0.3227 0.6672 -0.0761 0.082 Uiso 1 1 calc R . . C24 C 0.4260(10) 0.6757(9) 0.0231(8) 0.076(2) Uani 1 1 d . . . H24 H 0.4819 0.7153 -0.0214 0.091 Uiso 1 1 calc R . . C25 C 0.4136(9) 0.6325(8) 0.1308(8) 0.070(2) Uani 1 1 d . . . H25 H 0.4601 0.6383 0.1746 0.086 Uiso 1 1 calc R . . C33 C -0.0861(8) 0.6331(7) 0.3480(7) 0.0656(19) Uani 1 1 d . . . H33 H -0.1632 0.6439 0.3336 0.078 Uiso 1 1 calc R . . C34 C -0.0828(10) 0.6695(8) 0.4450(7) 0.078(3) Uani 1 1 d . . . H34 H -0.1554 0.7100 0.5065 0.095 Uiso 1 1 calc R . . C35 C 0.0491(10) 0.6335(8) 0.4307(7) 0.068(2) Uani 1 1 d . . . H35 H 0.0830 0.6443 0.4828 0.082 Uiso 1 1 calc R . . C41 C 0.1848(7) 0.2895(6) -0.0716(6) 0.0532(14) Uani 1 1 d . . . C42 C 0.2511(10) 0.1679(9) -0.1298(10) 0.082(3) Uani 1 1 d . . . H42 H 0.1899 0.1668 -0.1660 0.100 Uiso 1 1 calc R . . C43 C 0.263(2) 0.0660(12) -0.0493(12) 0.137(7) Uani 1 1 d . . . H43A H 0.3096 -0.0074 -0.0925 0.173 Uiso 1 1 calc R . . H43B H 0.3194 0.0669 -0.0085 0.173 Uiso 1 1 calc R . . C44 C 0.140(2) 0.0609(19) 0.0333(19) 0.220(15) Uani 1 1 d . . . H44A H 0.0682 0.1028 0.0035 0.245 Uiso 1 1 calc R . . H44B H 0.1217 0.0981 0.1021 0.245 Uiso 1 1 calc R . . H44C H 0.1490 -0.0214 0.0492 0.245 Uiso 1 1 calc R . . C45 C 0.3802(8) 0.1526(6) -0.2237(8) 0.0634(19) Uani 1 1 d . . . C46 C 0.4898(9) 0.1537(8) -0.2058(9) 0.076(2) Uani 1 1 d . . . H46 H 0.4840 0.1649 -0.1327 0.091 Uiso 1 1 calc R . . C47 C 0.6075(12) 0.1384(12) -0.2938(13) 0.109(4) Uani 1 1 d . . . H47 H 0.6806 0.1373 -0.2786 0.133 Uiso 1 1 calc R . . C48 C 0.6196(14) 0.1252(11) -0.3999(12) 0.103(4) Uani 1 1 d . . . H48 H 0.7003 0.1168 -0.4578 0.122 Uiso 1 1 calc R . . C49 C 0.5173(14) 0.1236(9) -0.4253(9) 0.100(4) Uani 1 1 d . . . H49 H 0.5271 0.1137 -0.4999 0.119 Uiso 1 1 calc R . . C50 C 0.3941(12) 0.1374(8) -0.3364(11) 0.090(3) Uani 1 1 d . . . H50 H 0.3226 0.1363 -0.3527 0.108 Uiso 1 1 calc R . . B1 B 0.2736(7) 0.5198(7) 0.2785(7) 0.0515(16) Uani 1 1 d . . . H1 H 0.3153 0.5276 0.3303 0.061 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 Dy 0.03850(15) 0.05915(19) 0.04016(15) 0.00759(11) -0.01137(10) -0.02451(12) O1 0.069(3) 0.098(4) 0.050(3) 0.014(3) -0.018(2) -0.049(3) O2 0.070(3) 0.088(4) 0.057(3) 0.020(3) -0.023(3) -0.053(3) O3 0.103(5) 0.088(4) 0.065(4) -0.013(3) -0.030(3) -0.041(4) O4 0.049(3) 0.089(4) 0.074(4) 0.024(3) -0.016(3) -0.013(3) N11 0.047(3) 0.058(3) 0.044(3) 0.007(2) -0.014(2) -0.015(2) N12 0.049(3) 0.052(3) 0.050(3) 0.004(2) -0.017(2) -0.018(2) N21 0.050(3) 0.064(3) 0.056(3) 0.002(3) -0.019(2) -0.031(3) N22 0.054(3) 0.069(3) 0.049(3) 0.009(2) -0.019(2) -0.036(3) N31 0.053(3) 0.053(3) 0.045(3) -0.001(2) -0.016(2) -0.016(2) N32 0.039(2) 0.066(3) 0.046(3) -0.006(2) -0.007(2) -0.015(2) C1 0.045(3) 0.066(4) 0.035(3) 0.004(2) -0.001(2) -0.029(3) C2 0.058(4) 0.094(6) 0.058(4) 0.026(4) 0.005(3) -0.034(4) C3 0.111(9) 0.075(6) 0.071(6) 0.014(5) 0.016(6) -0.023(6) C4 0.059(5) 0.082(6) 0.085(6) 0.010(5) 0.002(4) -0.011(4) C5 0.068(4) 0.068(4) 0.046(3) 0.005(3) -0.008(3) -0.038(4) C6 0.145(12) 0.131(11) 0.105(9) -0.011(8) -0.005(8) -0.106(10) C7 0.27(3) 0.159(18) 0.152(17) -0.052(14) 0.048(18) -0.18(2) C8 0.23(3) 0.080(9) 0.147(17) 0.016(10) 0.018(16) -0.071(14) C9 0.109(11) 0.111(11) 0.117(11) 0.036(9) -0.013(9) 0.008(9) C10 0.069(5) 0.085(6) 0.074(6) 0.000(5) -0.019(5) -0.007(5) C13 0.064(4) 0.048(3) 0.058(4) 0.003(3) -0.012(3) -0.018(3) C14 0.067(5) 0.055(4) 0.060(4) 0.011(3) -0.018(4) -0.006(3) C15 0.050(4) 0.072(5) 0.054(4) 0.013(3) -0.021(3) -0.013(3) C23 0.076(5) 0.085(5) 0.057(4) 0.016(4) -0.017(4) -0.055(5) C24 0.079(6) 0.094(6) 0.071(5) 0.010(4) -0.013(4) -0.062(5) C25 0.073(5) 0.081(5) 0.082(6) 0.002(4) -0.033(4) -0.050(5) C33 0.044(3) 0.064(4) 0.061(4) 0.005(3) -0.003(3) -0.009(3) C34 0.074(5) 0.068(5) 0.052(4) -0.007(4) 0.000(4) -0.005(4) C35 0.080(5) 0.070(5) 0.044(3) -0.003(3) -0.023(4) -0.015(4) C41 0.048(3) 0.049(3) 0.047(3) -0.006(3) -0.010(3) -0.006(3) C42 0.070(5) 0.067(5) 0.104(7) -0.021(5) -0.011(5) -0.028(4) C43 0.182(16) 0.081(7) 0.093(8) -0.001(6) 0.019(9) -0.054(9) C44 0.23(3) 0.18(2) 0.174(19) -0.059(16) 0.105(18) -0.13(2) C45 0.057(4) 0.041(3) 0.081(5) -0.018(3) -0.019(4) -0.005(3) C46 0.063(5) 0.069(5) 0.088(6) -0.025(5) -0.022(4) -0.013(4) C47 0.070(6) 0.092(8) 0.126(11) -0.037(7) 0.000(6) -0.008(6) C48 0.085(8) 0.081(7) 0.103(9) -0.015(6) 0.001(7) -0.017(6) C49 0.114(9) 0.064(5) 0.065(5) -0.010(4) -0.010(6) 0.007(6) C50 0.101(8) 0.053(4) 0.112(8) -0.012(5) -0.058(7) -0.003(5) B1 0.038(3) 0.060(4) 0.050(4) -0.008(3) -0.008(3) -0.015(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 Dy O4 2.263(6) 2_565 ? Dy O2 2.290(5) 2_565 ? Dy O1 2.304(5) . ? Dy O3 2.342(7) . ? Dy N22 2.468(6) . ? Dy N32 2.490(6) . ? Dy N12 2.492(6) . ? O1 C1 1.230(9) . ? O2 C1 1.247(8) . ? O2 Dy 2.290(5) 2_565 ? O3 C41 1.237(9) . ? O4 C41 1.243(9) . ? O4 Dy 2.263(6) 2_565 ? N11 C15 1.327(9) . ? N11 N12 1.367(8) . ? N11 B1 1.543(10) . ? N12 C13 1.342(9) . ? N21 C25 1.342(9) . ? N21 N22 1.372(8) . ? N21 B1 1.525(10) . ? N22 C23 1.333(9) . ? N31 C35 1.338(9) . ? N31 N32 1.354(8) . ? N31 B1 1.517(9) . ? N32 C33 1.344(9) . ? C1 C2 1.533(9) . ? C2 C3 1.407(15) . ? C2 C5 1.507(13) . ? C2 H2 0.9800 . ? C3 C4 1.540(15) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.378(13) . ? C5 C6 1.380(13) . ? C6 C7 1.45(3) . ? C6 H6 0.9300 . ? C7 C8 1.38(4) . ? C7 H7 0.9300 . ? C8 C9 1.29(3) . ? C8 H8 0.9300 . ? C9 C10 1.350(17) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C13 C14 1.378(12) . ? C13 H13 0.9300 . ? C14 C15 1.368(13) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C23 C24 1.389(12) . ? C23 H23 0.9300 . ? C24 C25 1.353(13) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C33 C34 1.388(13) . ? C33 H33 0.9300 . ? C34 C35 1.357(14) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C41 C42 1.531(11) . ? C42 C43 1.464(18) . ? C42 C45 1.492(13) . ? C42 H42 0.9800 . ? C43 C44 1.44(2) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.374(12) . ? C45 C50 1.407(14) . ? C46 C47 1.372(16) . ? C46 H46 0.9300 . ? C47 C48 1.33(2) . ? C47 H47 0.9300 . ? C48 C49 1.344(19) . ? C48 H48 0.9300 . ? C49 C50 1.422(18) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? B1 H1 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 O4 Dy O2 78.0(2) 2_565 2_565 ? O4 Dy O1 77.6(2) 2_565 . ? O2 Dy O1 131.3(2) 2_565 . ? O4 Dy O3 127.7(3) 2_565 . ? O2 Dy O3 82.7(3) 2_565 . ? O1 Dy O3 80.0(2) . . ? O4 Dy N22 108.8(2) 2_565 . ? O2 Dy N22 153.2(2) 2_565 . ? O1 Dy N22 75.2(2) . . ? O3 Dy N22 110.0(2) . . ? O4 Dy N32 80.5(2) 2_565 . ? O2 Dy N32 82.0(2) 2_565 . ? O1 Dy N32 133.5(2) . . ? O3 Dy N32 143.7(2) . . ? N22 Dy N32 74.0(2) . . ? O4 Dy N12 149.7(2) 2_565 . ? O2 Dy N12 85.1(2) 2_565 . ? O1 Dy N12 131.4(2) . . ? O3 Dy N12 73.8(2) . . ? N22 Dy N12 76.5(2) . . ? N32 Dy N12 72.3(2) . . ? C1 O1 Dy 140.6(5) . . ? C1 O2 Dy 139.7(5) . 2_565 ? C41 O3 Dy 118.4(6) . . ? C41 O4 Dy 171.8(7) . 2_565 ? C15 N11 N12 109.9(6) . . ? C15 N11 B1 129.8(7) . . ? N12 N11 B1 120.2(5) . . ? C13 N12 N11 105.6(6) . . ? C13 N12 Dy 130.5(5) . . ? N11 N12 Dy 123.8(4) . . ? C25 N21 N22 109.2(6) . . ? C25 N21 B1 129.5(7) . . ? N22 N21 B1 121.2(5) . . ? C23 N22 N21 105.6(6) . . ? C23 N22 Dy 130.6(5) . . ? N21 N22 Dy 123.5(4) . . ? C35 N31 N32 108.7(6) . . ? C35 N31 B1 129.6(7) . . ? N32 N31 B1 121.6(5) . . ? C33 N32 N31 107.2(6) . . ? C33 N32 Dy 129.4(6) . . ? N31 N32 Dy 123.4(4) . . ? O1 C1 O2 126.0(6) . . ? O1 C1 C2 116.2(7) . . ? O2 C1 C2 117.8(7) . . ? C3 C2 C5 117.3(8) . . ? C3 C2 C1 114.1(9) . . ? C5 C2 C1 111.5(6) . . ? C3 C2 H2 104.1 . . ? C5 C2 H2 104.1 . . ? C1 C2 H2 104.1 . . ? C2 C3 C4 117.2(11) . . ? C2 C3 H3A 108.0 . . ? C4 C3 H3A 108.0 . . ? C2 C3 H3B 108.0 . . ? C4 C3 H3B 108.0 . . ? H3A C3 H3B 107.3 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 119.8(11) . . ? C10 C5 C2 119.7(9) . . ? C6 C5 C2 120.4(11) . . ? C5 C6 C7 118.6(17) . . ? C5 C6 H6 120.7 . . ? C7 C6 H6 120.7 . . ? C8 C7 C6 115.2(14) . . ? C8 C7 H7 122.4 . . ? C6 C7 H7 122.4 . . ? C9 C8 C7 125(2) . . ? C9 C8 H8 117.3 . . ? C7 C8 H8 117.3 . . ? C8 C9 C10 120(2) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C5 120.9(15) . . ? C9 C10 H10 119.5 . . ? C5 C10 H10 119.5 . . ? N12 C13 C14 110.6(7) . . ? N12 C13 H13 124.7 . . ? C14 C13 H13 124.7 . . ? C15 C14 C13 105.0(7) . . ? C15 C14 H14 127.5 . . ? C13 C14 H14 127.5 . . ? N11 C15 C14 109.0(7) . . ? N11 C15 H15 125.5 . . ? C14 C15 H15 125.5 . . ? N22 C23 C24 111.0(8) . . ? N22 C23 H23 124.5 . . ? C24 C23 H23 124.5 . . ? C25 C24 C23 104.8(7) . . ? C25 C24 H24 127.6 . . ? C23 C24 H24 127.6 . . ? N21 C25 C24 109.4(7) . . ? N21 C25 H25 125.3 . . ? C24 C25 H25 125.3 . . ? N32 C33 C34 109.3(8) . . ? N32 C33 H33 125.4 . . ? C34 C33 H33 125.4 . . ? C35 C34 C33 105.1(7) . . ? C35 C34 H34 127.4 . . ? C33 C34 H34 127.4 . . ? N31 C35 C34 109.7(8) . . ? N31 C35 H35 125.2 . . ? C34 C35 H35 125.2 . . ? O3 C41 O4 121.7(7) . . ? O3 C41 C42 120.5(8) . . ? O4 C41 C42 117.8(8) . . ? C43 C42 C45 112.0(10) . . ? C43 C42 C41 113.1(10) . . ? C45 C42 C41 113.7(7) . . ? C43 C42 H42 105.8 . . ? C45 C42 H42 105.8 . . ? C41 C42 H42 105.8 . . ? C44 C43 C42 116.6(18) . . ? C44 C43 H43A 108.1 . . ? C42 C43 H43A 108.1 . . ? C44 C43 H43B 108.1 . . ? C42 C43 H43B 108.1 . . ? H43A C43 H43B 107.3 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 116.9(9) . . ? C46 C45 C42 122.6(9) . . ? C50 C45 C42 120.6(9) . . ? C47 C46 C45 121.2(11) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C48 C47 C46 121.7(14) . . ? C48 C47 H47 119.2 . . ? C46 C47 H47 119.2 . . ? C47 C48 C49 121.1(13) . . ? C47 C48 H48 119.4 . . ? C49 C48 H48 119.4 . . ? C48 C49 C50 119.1(11) . . ? C48 C49 H49 120.5 . . ? C50 C49 H49 120.5 . . ? C45 C50 C49 120.1(11) . . ? C45 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? N31 B1 N21 110.1(6) . . ? N31 B1 N11 109.7(6) . . ? N21 B1 N11 110.0(5) . . ? N31 B1 H1 109.0 . . ? N21 B1 H1 109.0 . . ? N11 B1 H1 109.0 . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 #_geom_contact_publ_flag Dy Dy 4.0651(15) 2_565 ? Dy O2 3.771(7) . ? Dy O4 3.173(9) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Dy O1 C1 -42.9(9) 2_565 . . . ? O2 Dy O1 C1 18.6(10) 2_565 . . . ? O3 Dy O1 C1 89.5(9) . . . . ? N22 Dy O1 C1 -156.5(9) . . . . ? N32 Dy O1 C1 -106.7(9) . . . . ? N12 Dy O1 C1 147.2(8) . . . . ? O4 Dy O3 C41 -6.5(8) 2_565 . . . ? O2 Dy O3 C41 62.2(6) 2_565 . . . ? O1 Dy O3 C41 -72.1(6) . . . . ? N22 Dy O3 C41 -142.1(6) . . . . ? N32 Dy O3 C41 127.8(6) . . . . ? N12 Dy O3 C41 149.3(7) . . . . ? C15 N11 N12 C13 0.3(8) . . . . ? B1 N11 N12 C13 -176.8(6) . . . . ? C15 N11 N12 Dy -177.9(5) . . . . ? B1 N11 N12 Dy 4.9(8) . . . . ? O4 Dy N12 C13 111.6(7) 2_565 . . . ? O2 Dy N12 C13 55.5(6) 2_565 . . . ? O1 Dy N12 C13 -88.4(7) . . . . ? O3 Dy N12 C13 -28.3(6) . . . . ? N22 Dy N12 C13 -144.2(7) . . . . ? N32 Dy N12 C13 138.6(7) . . . . ? O4 Dy N12 N11 -70.6(7) 2_565 . . . ? O2 Dy N12 N11 -126.7(5) 2_565 . . . ? O1 Dy N12 N11 89.4(5) . . . . ? O3 Dy N12 N11 149.5(5) . . . . ? N22 Dy N12 N11 33.6(5) . . . . ? N32 Dy N12 N11 -43.6(5) . . . . ? C25 N21 N22 C23 0.1(9) . . . . ? B1 N21 N22 C23 178.9(7) . . . . ? C25 N21 N22 Dy 174.6(6) . . . . ? B1 N21 N22 Dy -6.5(9) . . . . ? O4 Dy N22 C23 -70.9(8) 2_565 . . . ? O2 Dy N22 C23 -171.7(7) 2_565 . . . ? O1 Dy N22 C23 0.1(8) . . . . ? O3 Dy N22 C23 73.4(8) . . . . ? N32 Dy N22 C23 -144.6(8) . . . . ? N12 Dy N22 C23 140.2(8) . . . . ? O4 Dy N22 N21 116.0(6) 2_565 . . . ? O2 Dy N22 N21 15.2(9) 2_565 . . . ? O1 Dy N22 N21 -172.9(6) . . . . ? O3 Dy N22 N21 -99.7(6) . . . . ? N32 Dy N22 N21 42.3(5) . . . . ? N12 Dy N22 N21 -32.9(5) . . . . ? C35 N31 N32 C33 -0.3(9) . . . . ? B1 N31 N32 C33 176.3(7) . . . . ? C35 N31 N32 Dy 179.2(5) . . . . ? B1 N31 N32 Dy -4.2(9) . . . . ? O4 Dy N32 C33 29.4(7) 2_565 . . . ? O2 Dy N32 C33 -49.7(7) 2_565 . . . ? O1 Dy N32 C33 92.1(7) . . . . ? O3 Dy N32 C33 -115.5(7) . . . . ? N22 Dy N32 C33 142.3(7) . . . . ? N12 Dy N32 C33 -137.1(7) . . . . ? O4 Dy N32 N31 -150.0(6) 2_565 . . . ? O2 Dy N32 N31 130.9(6) 2_565 . . . ? O1 Dy N32 N31 -87.3(6) . . . . ? O3 Dy N32 N31 65.1(7) . . . . ? N22 Dy N32 N31 -37.1(5) . . . . ? N12 Dy N32 N31 43.5(5) . . . . ? Dy O1 C1 O2 -4.2(14) . . . . ? Dy O1 C1 C2 176.1(7) . . . . ? Dy O2 C1 O1 -15.0(14) 2_565 . . . ? Dy O2 C1 C2 164.7(7) 2_565 . . . ? O1 C1 C2 C3 109.6(11) . . . . ? O2 C1 C2 C3 -70.1(12) . . . . ? O1 C1 C2 C5 -114.7(9) . . . . ? O2 C1 C2 C5 65.6(11) . . . . ? C5 C2 C3 C4 167.1(9) . . . . ? C1 C2 C3 C4 -59.9(15) . . . . ? C3 C2 C5 C10 63.1(13) . . . . ? C1 C2 C5 C10 -71.0(11) . . . . ? C3 C2 C5 C6 -114.8(13) . . . . ? C1 C2 C5 C6 111.0(10) . . . . ? C10 C5 C6 C7 -0.3(17) . . . . ? C2 C5 C6 C7 177.7(12) . . . . ? C5 C6 C7 C8 -2(3) . . . . ? C6 C7 C8 C9 4(3) . . . . ? C7 C8 C9 C10 -3(3) . . . . ? C8 C9 C10 C5 1(2) . . . . ? C6 C5 C10 C9 0.5(16) . . . . ? C2 C5 C10 C9 -177.5(10) . . . . ? N11 N12 C13 C14 -0.3(8) . . . . ? Dy N12 C13 C14 177.8(5) . . . . ? N12 C13 C14 C15 0.2(9) . . . . ? N12 N11 C15 C14 -0.3(9) . . . . ? B1 N11 C15 C14 176.6(7) . . . . ? C13 C14 C15 N11 0.1(9) . . . . ? N21 N22 C23 C24 0.4(10) . . . . ? Dy N22 C23 C24 -173.6(6) . . . . ? N22 C23 C24 C25 -0.7(12) . . . . ? N22 N21 C25 C24 -0.5(10) . . . . ? B1 N21 C25 C24 -179.2(8) . . . . ? C23 C24 C25 N21 0.7(12) . . . . ? N31 N32 C33 C34 0.9(9) . . . . ? Dy N32 C33 C34 -178.5(6) . . . . ? N32 C33 C34 C35 -1.2(10) . . . . ? N32 N31 C35 C34 -0.5(10) . . . . ? B1 N31 C35 C34 -176.8(8) . . . . ? C33 C34 C35 N31 1.0(11) . . . . ? Dy O3 C41 O4 7.1(10) . . . . ? Dy O3 C41 C42 -173.6(6) . . . . ? Dy O4 C41 O3 -10(5) 2_565 . . . ? Dy O4 C41 C42 171(4) 2_565 . . . ? O3 C41 C42 C43 62.7(14) . . . . ? O4 C41 C42 C43 -118.0(13) . . . . ? O3 C41 C42 C45 -66.5(12) . . . . ? O4 C41 C42 C45 112.8(10) . . . . ? C45 C42 C43 C44 -169.4(15) . . . . ? C41 C42 C43 C44 61(2) . . . . ? C43 C42 C45 C46 -67.4(13) . . . . ? C41 C42 C45 C46 62.3(13) . . . . ? C43 C42 C45 C50 113.2(12) . . . . ? C41 C42 C45 C50 -117.1(9) . . . . ? C50 C45 C46 C47 -1.1(14) . . . . ? C42 C45 C46 C47 179.5(10) . . . . ? C45 C46 C47 C48 1.8(19) . . . . ? C46 C47 C48 C49 -1(2) . . . . ? C47 C48 C49 C50 0.5(19) . . . . ? C46 C45 C50 C49 0.2(13) . . . . ? C42 C45 C50 C49 179.6(9) . . . . ? C48 C49 C50 C45 0.2(16) . . . . ? C35 N31 B1 N21 -121.6(8) . . . . ? N32 N31 B1 N21 62.5(8) . . . . ? C35 N31 B1 N11 117.1(8) . . . . ? N32 N31 B1 N11 -58.7(9) . . . . ? C25 N21 B1 N31 122.4(9) . . . . ? N22 N21 B1 N31 -56.2(9) . . . . ? C25 N21 B1 N11 -116.6(9) . . . . ? N22 N21 B1 N11 64.8(8) . . . . ? C15 N11 B1 N31 -118.6(8) . . . . ? N12 N11 B1 N31 58.0(8) . . . . ? C15 N11 B1 N21 120.1(8) . . . . ? N12 N11 B1 N21 -63.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.506 _refine_diff_density_min -3.395 _refine_diff_density_rms 0.191