# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Fei-Yan Yi' _publ_contact_author_email fyyi@ciac.jl.cn _publ_author_name 'Zhongming Sun' data_1 _database_code_depnum_ccdc_archive 'CCDC 865797' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H73 Cd3 N3 O24' _chemical_formula_weight 1605.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 11.287(5) _cell_length_b 15.825(6) _cell_length_c 23.361(9) _cell_angle_alpha 102.135(6) _cell_angle_beta 101.692(6) _cell_angle_gamma 90.413(7) _cell_volume 3989(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description brick _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 0.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6636 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21392 _diffrn_reflns_av_R_equivalents 0.0988 _diffrn_reflns_av_sigmaI/netI 0.2024 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.12 _reflns_number_total 15385 _reflns_number_gt 7766 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1646P)^2^+9.9716P] 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 15385 _refine_ls_number_parameters 853 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1968 _refine_ls_R_factor_gt 0.0973 _refine_ls_wR_factor_ref 0.3175 _refine_ls_wR_factor_gt 0.2550 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.0000 0.0379(3) Uani 1 2 d S . . Cd2 Cd -0.12373(6) -0.99455(6) 0.12564(3) 0.0429(3) Uani 1 1 d . . . Cd3 Cd -1.0068(15) -0.9958(15) -0.4940(7) 0.0366(16) Uani 0.50 1 d P . . Cd4 Cd -1.27505(7) -0.93699(8) -0.46385(5) 0.0780(4) Uani 1 1 d . . . N1 N -0.3740(9) -0.9981(9) 0.2370(5) 0.073(4) Uani 1 1 d . . . N2 N -0.037(2) 0.409(2) 0.0881(15) 0.178(11) Uani 1 1 d . . . N3 N 0.219(2) 0.755(2) 0.2427(9) 0.47(6) Uani 1 1 d D . . C1 C -0.7079(8) -0.3732(8) -0.2443(5) 0.040(3) Uani 1 1 d . . . C2 C -0.6976(8) -0.3941(8) -0.1838(5) 0.045(3) Uani 1 1 d . . . H2A H -0.6756 -0.3421 -0.1527 0.054 Uiso 1 1 calc R . . H2B H -0.7745 -0.4182 -0.1805 0.054 Uiso 1 1 calc R . . C3 C -0.7333(9) -0.4543(8) -0.2943(5) 0.051(3) Uani 1 1 d . . . H3A H -0.7427 -0.4395 -0.3331 0.062 Uiso 1 1 calc R . . H3B H -0.6678 -0.4934 -0.2899 0.062 Uiso 1 1 calc R . . C4 C -0.8040(8) -0.3097(8) -0.2534(5) 0.045(3) Uani 1 1 d . . . H4A H -0.8804 -0.3328 -0.2486 0.054 Uiso 1 1 calc R . . H4B H -0.7818 -0.2560 -0.2239 0.054 Uiso 1 1 calc R . . C5 C -0.5864(9) -0.3322(8) -0.2466(5) 0.047(3) Uani 1 1 d . . . H5A H -0.5225 -0.3715 -0.2388 0.056 Uiso 1 1 calc R . . H5B H -0.5893 -0.3209 -0.2861 0.056 Uiso 1 1 calc R . . C6 C -0.8984(9) -0.2380(9) -0.3288(5) 0.052(3) Uani 1 1 d . . . C7 C -0.9708(9) -0.1902(9) -0.2938(5) 0.055(3) Uani 1 1 d . . . H7A H -0.9677 -0.1970 -0.2550 0.066 Uiso 1 1 calc R . . C8 C -1.0468(10) -0.1330(10) -0.3169(6) 0.063(4) Uani 1 1 d . . . H8A H -1.0962 -0.1015 -0.2938 0.075 Uiso 1 1 calc R . . C9 C -1.0507(10) -0.1216(10) -0.3740(6) 0.059(4) Uani 1 1 d . . . C10 C -0.9806(13) -0.1683(11) -0.4078(6) 0.076(5) Uani 1 1 d . . . H10A H -0.9833 -0.1613 -0.4466 0.091 Uiso 1 1 calc R . . C11 C -0.9065(11) -0.2254(9) -0.3855(6) 0.061(4) Uani 1 1 d . . . H11A H -0.8592 -0.2574 -0.4096 0.073 Uiso 1 1 calc R . . C12 C -0.4540(8) -0.2105(9) -0.1929(5) 0.047(3) Uani 1 1 d . . . C13 C -0.4372(9) -0.1387(9) -0.1474(6) 0.053(3) Uani 1 1 d . . . H13A H -0.4995 -0.1218 -0.1275 0.063 Uiso 1 1 calc R . . C14 C -0.3258(8) -0.0903(8) -0.1305(5) 0.046(3) Uani 1 1 d . . . H14A H -0.3131 -0.0420 -0.0990 0.055 Uiso 1 1 calc R . . C15 C -0.2342(8) -0.1164(8) -0.1622(5) 0.040(3) Uani 1 1 d . . . C16 C -0.2562(8) -0.1864(9) -0.2076(5) 0.053(3) Uani 1 1 d . . . H16A H -0.1959 -0.2027 -0.2289 0.064 Uiso 1 1 calc R . . C17 C -0.3639(9) -0.2348(9) -0.2238(5) 0.054(3) Uani 1 1 d . . . H17A H -0.3756 -0.2831 -0.2552 0.064 Uiso 1 1 calc R . . C18 C -0.3067(8) -0.4109(8) -0.0510(5) 0.047(3) Uani 1 1 d . . . C19 C -0.2887(13) -0.3560(10) -0.0866(6) 0.071(4) Uani 1 1 d . . . H19A H -0.3155 -0.3720 -0.1280 0.086 Uiso 1 1 calc R . . C20 C -0.2298(10) -0.2763(9) -0.0603(5) 0.058(4) Uani 1 1 d . . . H20A H -0.2137 -0.2403 -0.0848 0.070 Uiso 1 1 calc R . . C21 C -0.1941(8) -0.2481(7) 0.0006(5) 0.041(3) Uani 1 1 d . . . C22 C -0.2143(9) -0.3063(8) 0.0338(5) 0.054(3) Uani 1 1 d . . . H22A H -0.1911 -0.2893 0.0753 0.065 Uiso 1 1 calc R . . C23 C -0.2660(9) -0.3870(8) 0.0104(5) 0.052(3) Uani 1 1 d . . . H23A H -0.2737 -0.4252 0.0349 0.063 Uiso 1 1 calc R . . C24 C -0.8849(9) -0.5702(9) -0.3214(7) 0.063(4) Uani 1 1 d . . . C25 C -0.9881(13) -0.6052(11) -0.3094(9) 0.111(8) Uani 1 1 d . . . H25A H -1.0225 -0.5747 -0.2788 0.134 Uiso 1 1 calc R . . C26 C -1.0401(12) -0.6836(10) -0.3416(7) 0.080(5) Uani 1 1 d . . . H26A H -1.1086 -0.7056 -0.3323 0.096 Uiso 1 1 calc R . . C27 C -0.9938(9) -0.7295(9) -0.3867(5) 0.052(3) Uani 1 1 d . . . C28 C -0.8882(9) -0.6976(9) -0.3977(6) 0.058(3) Uani 1 1 d . . . H28A H -0.8527 -0.7305 -0.4271 0.069 Uiso 1 1 calc R . . C29 C -0.8341(9) -0.6187(8) -0.3667(5) 0.052(3) Uani 1 1 d . . . H29A H -0.7644 -0.5978 -0.3758 0.062 Uiso 1 1 calc R . . C30 C -0.6146(9) -0.5101(8) -0.1381(5) 0.050(3) Uani 1 1 d . . . H30A H -0.6948 -0.5385 -0.1479 0.061 Uiso 1 1 calc R . . H30B H -0.6000 -0.4769 -0.0972 0.061 Uiso 1 1 calc R . . C31 C -0.5191(8) -0.5768(8) -0.1453(4) 0.041(3) Uani 1 1 d . . . C32 C -0.3943(9) -0.5322(8) -0.1320(5) 0.048(3) Uani 1 1 d . . . H32A H -0.3352 -0.5743 -0.1414 0.058 Uiso 1 1 calc R . . H32B H -0.3938 -0.4895 -0.1563 0.058 Uiso 1 1 calc R . . C33 C -0.5241(8) -0.6349(8) -0.1009(5) 0.043(3) Uani 1 1 d . . . H33A H -0.5062 -0.6013 -0.0601 0.052 Uiso 1 1 calc R . . H33B H -0.6037 -0.6638 -0.1087 0.052 Uiso 1 1 calc R . . C34 C -0.5351(8) -0.6303(8) -0.2088(5) 0.047(3) Uani 1 1 d . . . H34A H -0.5382 -0.5927 -0.2369 0.057 Uiso 1 1 calc R . . H34B H -0.4676 -0.6674 -0.2121 0.057 Uiso 1 1 calc R . . C35 C -0.6621(9) -0.7462(9) -0.2708(5) 0.051(3) Uani 1 1 d . . . C36 C -0.5924(9) -0.7579(9) -0.3125(6) 0.061(4) Uani 1 1 d . . . H36A H -0.5262 -0.7195 -0.3068 0.073 Uiso 1 1 calc R . . C37 C -0.6141(8) -0.8221(9) -0.3617(5) 0.051(3) Uani 1 1 d . . . H37A H -0.5665 -0.8256 -0.3902 0.061 Uiso 1 1 calc R . . C38 C -0.7086(8) -0.8838(8) -0.3697(5) 0.048(3) Uani 1 1 d . . . C39 C -0.7834(9) -0.8723(9) -0.3281(5) 0.055(3) Uani 1 1 d . . . H39A H -0.8495 -0.9108 -0.3340 0.066 Uiso 1 1 calc R . . C40 C -0.7614(9) -0.8061(9) -0.2793(5) 0.053(3) Uani 1 1 d . . . H40A H -0.8112 -0.8000 -0.2516 0.064 Uiso 1 1 calc R . . C41 C -1.0513(10) -0.8144(9) -0.4219(5) 0.053(3) Uani 1 1 d . . . C42 C -1.1369(14) -0.0564(12) -0.3956(6) 0.077(5) Uani 1 1 d . . . C43 C -0.7289(9) -0.9590(9) -0.4229(5) 0.050(3) Uani 1 1 d . . . C47 C -0.1167(7) -0.0661(8) -0.1438(4) 0.039(3) Uani 1 1 d . . . C48 C -0.2452(9) -0.9017(9) 0.0498(5) 0.053(3) Uani 1 1 d . . . C49 C -0.1371(9) -0.1637(8) 0.0248(5) 0.047(3) Uani 1 1 d . . . C50 C -0.3010(8) -0.8487(8) 0.0079(5) 0.045(3) Uani 1 1 d . . . C51 C -0.2572(10) -0.8472(9) -0.0431(6) 0.058(3) Uani 1 1 d . . . H51A H -0.1958 -0.8829 -0.0526 0.069 Uiso 1 1 calc R . . C52 C -0.3950(9) -0.7969(9) 0.0182(6) 0.054(3) Uani 1 1 d . . . H52A H -0.4276 -0.7975 0.0516 0.065 Uiso 1 1 calc R . . C53 C -0.3948(9) -0.7431(8) -0.0703(5) 0.046(3) Uani 1 1 d . . . C61 C -0.4417(9) -0.7442(9) -0.0198(6) 0.059(4) Uani 1 1 d . . . H61A H -0.5047 -0.7091 -0.0118 0.071 Uiso 1 1 calc R . . C62 C -0.3043(10) -0.7931(9) -0.0795(5) 0.055(3) Uani 1 1 d . . . H62A H -0.2708 -0.7913 -0.1125 0.066 Uiso 1 1 calc R . . C64 C -0.3183(10) -1.0348(10) 0.1945(6) 0.062(4) Uani 1 1 d . . . C81 C -0.3156(13) -0.9286(11) 0.2840(7) 0.084(5) Uani 1 1 d . . . H81A H -0.2367 -0.9153 0.2778 0.125 Uiso 1 1 calc R . . H81B H -0.3077 -0.9453 0.3218 0.125 Uiso 1 1 calc R . . H81C H -0.3631 -0.8785 0.2841 0.125 Uiso 1 1 calc R . . C82 C -0.4963(12) -1.0270(13) 0.2395(9) 0.110(7) Uani 1 1 d . . . H82A H -0.5264 -1.0737 0.2060 0.165 Uiso 1 1 calc R . . H82B H -0.5490 -0.9797 0.2383 0.165 Uiso 1 1 calc R . . H82C H -0.4936 -1.0463 0.2761 0.165 Uiso 1 1 calc R . . C83 C -0.3765(13) -1.1071(12) 0.1449(7) 0.096(6) Uani 1 1 d . . . H83A H -0.3224 -1.1239 0.1182 0.144 Uiso 1 1 calc R . . H83B H -0.4500 -1.0887 0.1235 0.144 Uiso 1 1 calc R . . H83C H -0.3948 -1.1555 0.1611 0.144 Uiso 1 1 calc R . . C85 C -0.005(2) 0.370(2) 0.1285(15) 0.131(10) Uani 1 1 d . . . C86 C 0.016(2) 0.5034(16) 0.1050(18) 0.203(17) Uani 1 1 d . . . H86A H 0.0485 0.5188 0.1473 0.305 Uiso 1 1 calc R . . H86B H -0.0474 0.5413 0.0947 0.305 Uiso 1 1 calc R . . H86C H 0.0785 0.5086 0.0836 0.305 Uiso 1 1 calc R . . C87 C -0.0443(17) 0.2733(14) 0.1183(9) 0.107(6) Uani 1 1 d . . . H87A H -0.0898 0.2537 0.0781 0.160 Uiso 1 1 calc R . . H87B H -0.0938 0.2663 0.1461 0.160 Uiso 1 1 calc R . . H87C H 0.0261 0.2400 0.1244 0.160 Uiso 1 1 calc R . . C88 C -0.099(2) 0.3767(19) 0.0265(11) 0.163(11) Uani 1 1 d . . . H88A H -0.1300 0.3184 0.0217 0.245 Uiso 1 1 calc R . . H88B H -0.0433 0.3776 0.0005 0.245 Uiso 1 1 calc R . . H88C H -0.1650 0.4125 0.0163 0.245 Uiso 1 1 calc R . . C89 C 0.131(3) 0.792(2) 0.2143(13) 0.149(11) Uani 1 1 d D . . C90 C 0.220(2) 0.6907(18) 0.2155(9) 0.132(9) Uani 1 1 d . . . H90A H 0.1441 0.6766 0.1878 0.198 Uiso 1 1 calc R . . H90B H 0.2335 0.6496 0.2408 0.198 Uiso 1 1 calc R . . H90C H 0.2843 0.6890 0.1939 0.198 Uiso 1 1 calc R . . C91 C 0.2869(16) 0.8296(19) 0.2861(10) 0.172(13) Uani 1 1 d D . . H91A H 0.2404 0.8801 0.2854 0.258 Uiso 1 1 calc R . . H91B H 0.3629 0.8395 0.2755 0.258 Uiso 1 1 calc R . . H91C H 0.3015 0.8178 0.3255 0.258 Uiso 1 1 calc R . . C92 C 0.044(3) 0.741(2) 0.1567(19) 0.31(3) Uani 1 1 d . . . H92A H 0.0698 0.6825 0.1470 0.458 Uiso 1 1 calc R . . H92B H 0.0465 0.7684 0.1240 0.458 Uiso 1 1 calc R . . H92C H -0.0367 0.7394 0.1634 0.458 Uiso 1 1 calc R . . O1 O -0.8439(7) -0.4930(7) -0.2879(5) 0.077(3) Uani 1 1 d . . . O2 O -0.8160(7) -0.2943(6) -0.3108(4) 0.058(2) Uani 1 1 d . . . O3 O -0.5622(6) -0.2546(6) -0.2034(4) 0.056(2) Uani 1 1 d . . . O4 O -0.6058(6) -0.4558(6) -0.1774(4) 0.058(2) Uani 1 1 d . . . O5 O -0.3643(7) -0.4911(6) -0.0699(3) 0.059(2) Uani 1 1 d . . . O6 O -0.4336(7) -0.6969(6) -0.1101(4) 0.056(2) Uani 1 1 d . . . O7 O -0.6455(6) -0.6813(6) -0.2216(4) 0.055(2) Uani 1 1 d . . . O8 O -0.0943(6) -0.0059(6) -0.0970(3) 0.049(2) Uani 1 1 d . . . O9 O -0.0388(5) -0.0870(6) -0.1744(3) 0.051(2) Uani 1 1 d . . . O10 O -0.1401(7) -0.1304(6) 0.0786(4) 0.063(2) Uani 1 1 d . . . O11 O -0.0866(7) -0.1258(6) -0.0064(4) 0.061(2) Uani 1 1 d . . . O13 O -0.6520(6) -0.9681(7) -0.4531(4) 0.072(3) Uani 1 1 d . . . O14 O -0.8240(6) -1.0058(6) -0.4338(3) 0.059(2) Uani 1 1 d . . . O15 O -0.9983(7) -0.8626(6) -0.4561(4) 0.055(2) Uani 1 1 d . . . O16 O -1.1297(7) -0.0351(6) -0.4436(4) 0.064(2) Uani 1 1 d . . . O17 O -1.2167(14) -0.0305(11) -0.3686(6) 0.145(7) Uani 1 1 d . . . O19 O -1.1567(8) -0.8294(8) -0.4140(6) 0.099(4) Uani 1 1 d . . . O20 O -0.2835(7) -0.9031(7) 0.0951(4) 0.077(3) Uani 1 1 d . . . O24 O -0.2120(6) -1.0063(6) 0.1989(4) 0.065(3) Uani 1 1 d . . . O28 O -0.1563(7) -0.9432(7) 0.0405(4) 0.067(3) Uani 1 1 d . . . O33 O 0.0620(16) 0.4065(14) 0.1830(10) 0.174(8) Uani 1 1 d . . . O35 O 0.082(3) 0.8837(19) 0.2241(18) 0.306(19) Uani 1 1 d . . . O1W O -1.4272(15) -0.8293(13) -0.5050(11) 0.260(15) Uani 1 1 d . . . H1WA H -1.4879 -0.8285 -0.4885 0.391 Uiso 1 1 d R . . H1WB H -1.3933 -0.7788 -0.4966 0.391 Uiso 1 1 d R . . H1WC H -1.4508 -0.8456 -0.5427 0.391 Uiso 1 1 d R . . O2W O -1.4101(8) -0.9612(9) -0.4129(5) 0.106(4) Uani 1 1 d . . . H2WA H -1.4689 -0.9287 -0.4192 0.159 Uiso 1 1 d R . . H2WB H -1.4360 -1.0139 -0.4241 0.159 Uiso 1 1 d R . . H2WC H -1.3780 -0.9504 -0.3758 0.159 Uiso 1 1 d 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 Cd1 0.0353(4) 0.0359(8) 0.0415(6) 0.0058(5) 0.0085(4) -0.0045(4) Cd2 0.0401(4) 0.0407(6) 0.0467(5) 0.0078(4) 0.0085(3) -0.0056(3) Cd3 0.030(3) 0.035(4) 0.037(5) -0.011(4) 0.007(2) 0.007(2) Cd4 0.0411(4) 0.0626(9) 0.1064(9) -0.0327(7) 0.0136(4) -0.0078(4) N1 0.070(6) 0.086(11) 0.076(8) 0.035(8) 0.025(6) -0.002(6) N2 0.128(17) 0.22(4) 0.18(3) 0.01(3) 0.047(17) 0.015(19) N3 0.27(4) 1.02(15) 0.043(13) -0.02(3) 0.027(17) -0.38(7) C1 0.036(4) 0.029(8) 0.053(6) 0.004(6) 0.010(4) 0.001(4) C2 0.036(4) 0.042(9) 0.055(7) 0.007(6) 0.009(4) 0.011(5) C3 0.045(5) 0.043(9) 0.061(7) 0.007(7) 0.005(5) -0.004(5) C4 0.037(4) 0.043(9) 0.056(6) 0.021(6) 0.001(4) 0.006(5) C5 0.047(5) 0.037(9) 0.049(6) -0.001(6) 0.009(4) -0.001(5) C6 0.046(5) 0.046(9) 0.063(7) 0.020(7) 0.003(5) 0.015(5) C7 0.059(6) 0.058(10) 0.052(7) 0.022(7) 0.013(5) 0.017(6) C8 0.054(6) 0.070(12) 0.067(8) 0.018(8) 0.013(5) 0.022(6) C9 0.061(6) 0.057(11) 0.060(8) 0.018(7) 0.008(6) 0.015(6) C10 0.104(10) 0.083(13) 0.049(8) 0.030(8) 0.020(7) 0.025(9) C11 0.078(7) 0.053(10) 0.062(8) 0.023(7) 0.027(6) 0.023(7) C12 0.038(4) 0.045(9) 0.055(7) 0.006(7) 0.006(4) -0.011(5) C13 0.044(5) 0.049(10) 0.068(8) 0.013(7) 0.018(5) -0.006(5) C14 0.050(5) 0.033(8) 0.058(7) 0.008(6) 0.018(5) -0.013(5) C15 0.038(4) 0.040(8) 0.045(6) 0.019(6) 0.005(4) 0.001(5) C16 0.042(5) 0.068(11) 0.048(7) 0.000(7) 0.020(4) -0.009(6) C17 0.050(5) 0.048(9) 0.052(7) -0.015(6) 0.016(5) -0.017(5) C18 0.043(5) 0.033(8) 0.060(7) 0.005(6) 0.006(4) -0.010(5) C19 0.102(9) 0.059(11) 0.046(7) 0.009(7) 0.001(6) -0.021(8) C20 0.074(7) 0.051(10) 0.046(7) 0.014(7) 0.002(5) -0.018(6) C21 0.048(5) 0.027(8) 0.052(6) 0.015(6) 0.016(4) 0.003(5) C22 0.053(5) 0.046(9) 0.057(7) 0.003(7) 0.006(5) -0.014(6) C23 0.052(5) 0.038(9) 0.063(7) 0.012(7) 0.003(5) -0.005(5) C24 0.048(5) 0.038(9) 0.094(10) -0.014(8) 0.023(6) -0.014(6) C25 0.087(9) 0.072(14) 0.158(17) -0.065(12) 0.085(11) -0.049(9) C26 0.068(7) 0.056(12) 0.104(12) -0.020(9) 0.032(8) -0.025(7) C27 0.049(5) 0.037(9) 0.054(7) -0.020(6) 0.005(5) -0.009(5) C28 0.052(6) 0.051(10) 0.062(8) -0.007(7) 0.013(5) 0.006(6) C29 0.048(5) 0.041(9) 0.064(7) -0.004(7) 0.024(5) -0.003(5) C30 0.056(5) 0.047(9) 0.050(6) 0.013(6) 0.009(5) 0.007(6) C31 0.054(5) 0.032(8) 0.039(6) 0.013(5) 0.009(4) 0.004(5) C32 0.058(5) 0.038(9) 0.043(6) 0.003(6) 0.003(4) -0.007(5) C33 0.046(5) 0.034(8) 0.042(6) -0.003(5) 0.001(4) 0.002(5) C34 0.042(5) 0.034(8) 0.057(7) -0.001(6) 0.001(4) -0.001(5) C35 0.051(5) 0.052(10) 0.044(7) 0.005(7) -0.003(4) -0.006(5) C36 0.043(5) 0.063(11) 0.068(8) -0.002(8) 0.008(5) -0.014(6) C37 0.042(5) 0.050(9) 0.049(7) -0.017(7) 0.009(4) -0.006(5) C38 0.040(5) 0.048(9) 0.051(6) 0.006(6) -0.001(4) -0.010(5) C39 0.045(5) 0.050(10) 0.063(8) 0.004(7) 0.006(5) -0.006(5) C40 0.046(5) 0.062(10) 0.047(7) 0.003(7) 0.010(4) -0.010(6) C41 0.056(6) 0.042(9) 0.046(7) -0.009(7) -0.005(5) -0.008(6) C42 0.098(10) 0.076(13) 0.054(8) 0.035(9) -0.015(7) -0.004(9) C43 0.044(5) 0.041(9) 0.052(7) -0.005(6) 0.000(5) -0.001(5) C47 0.035(4) 0.045(9) 0.039(6) 0.016(6) 0.007(4) -0.003(5) C48 0.044(5) 0.068(11) 0.051(6) 0.020(7) 0.015(4) -0.006(6) C49 0.054(5) 0.036(9) 0.046(7) -0.001(6) 0.010(5) 0.004(5) C50 0.041(5) 0.037(8) 0.060(7) 0.016(6) 0.012(4) 0.008(5) C51 0.059(6) 0.051(10) 0.074(8) 0.022(7) 0.026(6) 0.020(6) C52 0.057(6) 0.049(10) 0.067(8) 0.016(7) 0.031(5) 0.006(6) C53 0.051(5) 0.034(8) 0.049(6) 0.010(6) 0.004(4) 0.010(5) C61 0.047(5) 0.064(11) 0.072(8) 0.025(8) 0.016(5) 0.013(6) C62 0.070(7) 0.049(10) 0.054(7) 0.024(7) 0.023(5) 0.009(6) C64 0.057(6) 0.067(11) 0.064(8) 0.023(8) 0.012(5) -0.012(6) C81 0.081(9) 0.079(14) 0.087(11) 0.005(10) 0.023(8) -0.011(9) C82 0.062(8) 0.136(18) 0.159(17) 0.071(15) 0.045(9) -0.007(9) C83 0.083(9) 0.099(15) 0.084(11) -0.005(10) -0.007(7) -0.048(9) C85 0.095(14) 0.16(3) 0.13(2) 0.00(2) 0.041(15) 0.046(17) C86 0.127(17) 0.070(19) 0.42(5) 0.08(3) 0.04(2) -0.004(15) C87 0.117(13) 0.074(16) 0.121(16) -0.002(13) 0.029(11) -0.013(12) C88 0.16(2) 0.19(3) 0.113(19) 0.012(19) -0.004(16) -0.03(2) C89 0.15(2) 0.17(3) 0.14(2) 0.08(2) 0.015(16) -0.04(2) C90 0.17(2) 0.15(2) 0.058(13) -0.032(14) 0.028(13) -0.024(18) C91 0.077(11) 0.30(4) 0.102(16) 0.00(2) -0.003(10) -0.013(16) C92 0.22(3) 0.19(4) 0.38(6) 0.01(4) -0.16(4) -0.02(3) O1 0.060(4) 0.050(7) 0.105(8) -0.039(6) 0.037(5) -0.021(5) O2 0.062(4) 0.052(7) 0.064(5) 0.016(5) 0.018(4) 0.025(4) O3 0.045(3) 0.040(6) 0.074(6) -0.011(5) 0.016(3) -0.010(4) O4 0.058(4) 0.051(7) 0.081(6) 0.034(5) 0.030(4) 0.024(4) O5 0.082(5) 0.039(6) 0.045(4) 0.007(4) -0.008(4) -0.028(4) O6 0.065(4) 0.041(6) 0.065(5) 0.018(5) 0.016(4) 0.017(4) O7 0.046(3) 0.056(7) 0.054(5) -0.002(5) 0.010(3) -0.008(4) O8 0.051(4) 0.042(6) 0.046(5) 0.002(4) 0.001(3) -0.008(4) O9 0.042(3) 0.058(6) 0.049(4) 0.000(4) 0.011(3) -0.019(3) O10 0.074(5) 0.052(7) 0.063(6) 0.011(5) 0.015(4) -0.007(4) O11 0.070(4) 0.042(6) 0.070(5) 0.006(5) 0.021(4) -0.023(4) O13 0.046(4) 0.076(8) 0.073(6) -0.024(5) 0.010(4) -0.010(4) O14 0.052(4) 0.048(6) 0.058(5) 0.001(4) -0.021(3) -0.008(4) O15 0.072(5) 0.040(6) 0.044(5) -0.006(4) 0.007(4) 0.000(4) O16 0.063(4) 0.056(7) 0.064(5) 0.014(5) -0.007(4) -0.007(4) O17 0.177(13) 0.180(18) 0.092(9) 0.050(10) 0.034(9) 0.140(13) O19 0.074(6) 0.072(9) 0.133(10) -0.019(7) 0.027(6) -0.041(5) O20 0.071(5) 0.092(9) 0.093(7) 0.052(7) 0.042(5) 0.044(5) O24 0.054(4) 0.086(8) 0.056(5) 0.016(5) 0.015(3) -0.022(4) O28 0.064(5) 0.080(8) 0.073(6) 0.031(6) 0.036(4) 0.040(5) O33 0.139(13) 0.17(2) 0.178(18) -0.026(15) 0.027(13) 0.028(13) O35 0.26(3) 0.18(3) 0.49(5) 0.13(3) 0.03(3) 0.07(2) O1W 0.136(13) 0.17(2) 0.38(3) -0.17(2) 0.090(17) -0.052(13) O2W 0.071(5) 0.174(14) 0.085(7) 0.045(8) 0.023(5) 0.053(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O11 2.174(8) . ? Cd1 O11 2.174(8) 2 ? Cd1 O28 2.271(8) 1_565 ? Cd1 O28 2.271(8) 2_545 ? Cd1 O8 2.281(7) 2 ? Cd1 O8 2.281(7) . ? Cd2 O24 2.185(7) . ? Cd2 O10 2.187(10) 1_545 ? Cd2 O9 2.197(6) 2_545 ? Cd2 O28 2.266(8) . ? Cd2 O20 2.409(8) . ? Cd2 C48 2.705(11) . ? Cd3 Cd3 0.35(2) 2_334 ? Cd3 O15 2.10(2) . ? Cd3 O16 2.157(16) 1_545 ? Cd3 O14 2.277(19) . ? Cd3 O14 2.282(19) 2_334 ? Cd3 O15 2.31(2) 2_334 ? Cd3 O16 2.437(15) 2_344 ? Cd3 Cd4 3.340(13) . ? Cd4 O19 2.132(10) . ? Cd4 O13 2.193(9) 2_334 ? Cd4 O2W 2.193(10) . ? Cd4 O16 2.314(9) 1_545 ? Cd4 O1W 2.62(3) . ? N1 C64 1.316(17) . ? N1 C81 1.428(19) . ? N1 C82 1.468(14) . ? N2 C85 1.23(3) . ? N2 C88 1.45(3) . ? N2 C86 1.54(4) . ? N3 C90 1.08(4) . ? N3 C89 1.295(19) . ? N3 C91 1.476(18) . ? C1 C4 1.498(15) . ? C1 C2 1.498(14) . ? C1 C3 1.525(17) . ? C1 C5 1.529(12) . ? C2 O4 1.437(12) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O1 1.435(12) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O2 1.393(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O3 1.401(14) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O2 1.358(13) . ? C6 C11 1.366(15) . ? C6 C7 1.387(17) . ? C7 C8 1.371(16) . ? C7 H7A 0.9300 . ? C8 C9 1.375(16) . ? C8 H8A 0.9300 . ? C9 C10 1.346(18) . ? C9 C42 1.515(19) . ? C10 C11 1.349(18) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 O3 1.353(11) . ? C12 C13 1.366(17) . ? C12 C17 1.374(15) . ? C13 C14 1.408(13) . ? C13 H13A 0.9300 . ? C14 C15 1.407(15) . ? C14 H14A 0.9300 . ? C15 C16 1.344(16) . ? C15 C47 1.479(12) . ? C16 C17 1.372(14) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.363(16) . ? C18 O5 1.366(13) . ? C18 C23 1.384(16) . ? C19 C20 1.381(18) . ? C19 H19A 0.9300 . ? C20 C21 1.371(15) . ? C20 H20A 0.9300 . ? C21 C22 1.369(14) . ? C21 C49 1.429(16) . ? C22 C23 1.355(17) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 O1 1.328(15) . ? C24 C25 1.390(15) . ? C24 C29 1.396(17) . ? C25 C26 1.37(2) . ? C25 H25A 0.9300 . ? C26 C27 1.348(18) . ? C26 H26A 0.9300 . ? C27 C28 1.384(15) . ? C27 C41 1.486(17) . ? C28 C29 1.373(17) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 O4 1.397(12) . ? C30 C31 1.522(15) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.515(13) . ? C31 C34 1.520(16) . ? C31 C33 1.534(13) . ? C32 O5 1.430(13) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 O6 1.438(13) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O7 1.424(11) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 O7 1.350(15) . ? C35 C36 1.358(16) . ? C35 C40 1.418(15) . ? C36 C37 1.342(17) . ? C36 H36A 0.9300 . ? C37 C38 1.398(14) . ? C37 H37A 0.9300 . ? C38 C39 1.395(16) . ? C38 C43 1.508(17) . ? C39 C40 1.355(17) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C41 O15 1.233(14) . ? C41 O19 1.268(14) . ? C42 O17 1.225(19) . ? C42 O16 1.256(15) . ? C43 O13 1.217(13) . ? C43 O14 1.251(13) . ? C47 O9 1.247(12) . ? C47 O8 1.270(13) . ? C48 O20 1.225(13) . ? C48 O28 1.235(13) . ? C48 C50 1.470(15) . ? C49 O11 1.252(13) . ? C49 O10 1.263(14) . ? C50 C52 1.374(15) . ? C50 C51 1.384(15) . ? C51 C62 1.367(15) . ? C51 H51A 0.9300 . ? C52 C61 1.376(16) . ? C52 H52A 0.9300 . ? C53 O6 1.311(12) . ? C53 C62 1.321(16) . ? C53 C61 1.389(16) . ? C61 H61A 0.9300 . ? C62 H62A 0.9300 . ? C64 O24 1.256(12) . ? C64 C83 1.48(2) . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C85 O33 1.35(3) . ? C85 C87 1.55(4) . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C89 O35 1.55(4) . ? C89 C92 1.56(4) . ? C89 C90 1.90(4) . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? O9 Cd2 2.197(6) 2_545 ? O10 Cd2 2.187(10) 1_565 ? O13 Cd4 2.193(9) 2_334 ? O14 Cd3 2.28(2) 2_334 ? O15 Cd3 2.31(2) 2_334 ? O16 Cd3 2.157(16) 1_565 ? O16 Cd4 2.314(9) 1_565 ? O16 Cd3 2.437(15) 2_344 ? O28 Cd1 2.271(8) 1_545 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8501 . ? O1W H1WC 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O2W H2WC 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Cd1 O11 180.0(5) . 2 ? O11 Cd1 O28 86.1(3) . 1_565 ? O11 Cd1 O28 93.9(3) 2 1_565 ? O11 Cd1 O28 93.9(3) . 2_545 ? O11 Cd1 O28 86.1(3) 2 2_545 ? O28 Cd1 O28 180.0(4) 1_565 2_545 ? O11 Cd1 O8 91.4(3) . 2 ? O11 Cd1 O8 88.6(3) 2 2 ? O28 Cd1 O8 84.4(3) 1_565 2 ? O28 Cd1 O8 95.6(3) 2_545 2 ? O11 Cd1 O8 88.6(3) . . ? O11 Cd1 O8 91.4(3) 2 . ? O28 Cd1 O8 95.6(3) 1_565 . ? O28 Cd1 O8 84.4(3) 2_545 . ? O8 Cd1 O8 180.0(4) 2 . ? O24 Cd2 O10 98.9(3) . 1_545 ? O24 Cd2 O9 101.2(3) . 2_545 ? O10 Cd2 O9 129.7(3) 1_545 2_545 ? O24 Cd2 O28 140.6(3) . . ? O10 Cd2 O28 94.2(3) 1_545 . ? O9 Cd2 O28 98.4(3) 2_545 . ? O24 Cd2 O20 87.3(3) . . ? O10 Cd2 O20 117.6(4) 1_545 . ? O9 Cd2 O20 109.0(4) 2_545 . ? O28 Cd2 O20 53.9(3) . . ? O24 Cd2 C48 114.0(3) . . ? O10 Cd2 C48 107.8(4) 1_545 . ? O9 Cd2 C48 105.0(3) 2_545 . ? O28 Cd2 C48 27.0(3) . . ? O20 Cd2 C48 26.9(3) . . ? Cd3 Cd3 O15 122(8) 2_334 . ? Cd3 Cd3 O16 141(8) 2_334 1_545 ? O15 Cd3 O16 97.1(6) . 1_545 ? Cd3 Cd3 O14 86(6) 2_334 . ? O15 Cd3 O14 89.0(8) . . ? O16 Cd3 O14 101.5(7) 1_545 . ? Cd3 Cd3 O14 85(6) 2_334 2_334 ? O15 Cd3 O14 95.7(9) . 2_334 ? O16 Cd3 O14 85.4(6) 1_545 2_334 ? O14 Cd3 O14 171.2(5) . 2_334 ? Cd3 Cd3 O15 51(7) 2_334 2_334 ? O15 Cd3 O15 172.6(7) . 2_334 ? O16 Cd3 O15 90.2(9) 1_545 2_334 ? O14 Cd3 O15 90.4(8) . 2_334 ? O14 Cd3 O15 84.0(7) 2_334 2_334 ? Cd3 Cd3 O16 34(7) 2_334 2_344 ? O15 Cd3 O16 88.0(8) . 2_344 ? O16 Cd3 O16 174.8(11) 1_545 2_344 ? O14 Cd3 O16 79.3(5) . 2_344 ? O14 Cd3 O16 93.3(6) 2_334 2_344 ? O15 Cd3 O16 84.6(5) 2_334 2_344 ? Cd3 Cd3 Cd4 141(6) 2_334 . ? O15 Cd3 Cd4 70.1(4) . . ? O16 Cd3 Cd4 43.5(3) 1_545 . ? O14 Cd3 Cd4 132.2(5) . . ? O14 Cd3 Cd4 56.6(4) 2_334 . ? O15 Cd3 Cd4 115.3(7) 2_334 . ? O16 Cd3 Cd4 138.9(8) 2_344 . ? O19 Cd4 O13 151.6(4) . 2_334 ? O19 Cd4 O2W 109.7(5) . . ? O13 Cd4 O2W 98.1(4) 2_334 . ? O19 Cd4 O16 92.5(4) . 1_545 ? O13 Cd4 O16 86.4(3) 2_334 1_545 ? O2W Cd4 O16 103.4(4) . 1_545 ? O19 Cd4 O1W 89.1(5) . . ? O13 Cd4 O1W 87.3(5) 2_334 . ? O2W Cd4 O1W 85.5(5) . . ? O16 Cd4 O1W 169.8(5) 1_545 . ? O19 Cd4 Cd3 77.3(5) . . ? O13 Cd4 Cd3 84.0(4) 2_334 . ? O2W Cd4 Cd3 143.3(4) . . ? O16 Cd4 Cd3 39.9(4) 1_545 . ? O1W Cd4 Cd3 131.2(6) . . ? C64 N1 C81 120.8(11) . . ? C64 N1 C82 122.5(14) . . ? C81 N1 C82 116.7(13) . . ? C85 N2 C88 130(4) . . ? C85 N2 C86 112(3) . . ? C88 N2 C86 117(3) . . ? C90 N3 C89 106(3) . . ? C90 N3 C91 149(3) . . ? C89 N3 C91 102(3) . . ? C4 C1 C2 109.8(8) . . ? C4 C1 C3 111.0(8) . . ? C2 C1 C3 111.8(9) . . ? C4 C1 C5 108.9(9) . . ? C2 C1 C5 108.2(8) . . ? C3 C1 C5 107.0(8) . . ? O4 C2 C1 107.9(8) . . ? O4 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? O4 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? O1 C3 C1 104.8(9) . . ? O1 C3 H3A 110.8 . . ? C1 C3 H3A 110.8 . . ? O1 C3 H3B 110.8 . . ? C1 C3 H3B 110.8 . . ? H3A C3 H3B 108.9 . . ? O2 C4 C1 108.9(9) . . ? O2 C4 H4A 109.9 . . ? C1 C4 H4A 109.9 . . ? O2 C4 H4B 109.9 . . ? C1 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? O3 C5 C1 109.2(9) . . ? O3 C5 H5A 109.9 . . ? C1 C5 H5A 109.9 . . ? O3 C5 H5B 109.9 . . ? C1 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? O2 C6 C11 116.5(11) . . ? O2 C6 C7 125.7(10) . . ? C11 C6 C7 117.7(10) . . ? C8 C7 C6 119.6(11) . . ? C8 C7 H7A 120.2 . . ? C6 C7 H7A 120.2 . . ? C7 C8 C9 120.6(12) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? C10 C9 C8 119.5(11) . . ? C10 C9 C42 123.6(12) . . ? C8 C9 C42 116.9(12) . . ? C9 C10 C11 120.1(11) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C10 C11 C6 122.5(12) . . ? C10 C11 H11A 118.8 . . ? C6 C11 H11A 118.8 . . ? O3 C12 C13 115.2(10) . . ? O3 C12 C17 124.4(12) . . ? C13 C12 C17 120.4(9) . . ? C12 C13 C14 120.2(10) . . ? C12 C13 H13A 119.9 . . ? C14 C13 H13A 119.9 . . ? C15 C14 C13 118.6(11) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? C16 C15 C14 118.9(9) . . ? C16 C15 C47 122.7(9) . . ? C14 C15 C47 118.5(11) . . ? C15 C16 C17 122.9(10) . . ? C15 C16 H16A 118.5 . . ? C17 C16 H16A 118.5 . . ? C16 C17 C12 118.9(12) . . ? C16 C17 H17A 120.5 . . ? C12 C17 H17A 120.5 . . ? C19 C18 O5 126.0(11) . . ? C19 C18 C23 120.4(11) . . ? O5 C18 C23 113.6(10) . . ? C18 C19 C20 118.8(12) . . ? C18 C19 H19A 120.6 . . ? C20 C19 H19A 120.6 . . ? C21 C20 C19 122.8(11) . . ? C21 C20 H20A 118.6 . . ? C19 C20 H20A 118.6 . . ? C22 C21 C20 115.5(11) . . ? C22 C21 C49 124.7(10) . . ? C20 C21 C49 119.7(9) . . ? C23 C22 C21 124.3(12) . . ? C23 C22 H22A 117.8 . . ? C21 C22 H22A 117.8 . . ? C22 C23 C18 118.0(11) . . ? C22 C23 H23A 121.0 . . ? C18 C23 H23A 121.0 . . ? O1 C24 C25 115.9(12) . . ? O1 C24 C29 126.2(10) . . ? C25 C24 C29 117.8(12) . . ? C26 C25 C24 121.3(14) . . ? C26 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C27 C26 C25 121.3(12) . . ? C27 C26 H26A 119.4 . . ? C25 C26 H26A 119.4 . . ? C26 C27 C28 118.3(12) . . ? C26 C27 C41 121.0(11) . . ? C28 C27 C41 120.6(12) . . ? C29 C28 C27 122.0(12) . . ? C29 C28 H28A 119.0 . . ? C27 C28 H28A 119.0 . . ? C28 C29 C24 119.2(10) . . ? C28 C29 H29A 120.4 . . ? C24 C29 H29A 120.4 . . ? O4 C30 C31 107.0(8) . . ? O4 C30 H30A 110.3 . . ? C31 C30 H30A 110.3 . . ? O4 C30 H30B 110.3 . . ? C31 C30 H30B 110.3 . . ? H30A C30 H30B 108.6 . . ? C32 C31 C34 104.9(8) . . ? C32 C31 C30 110.3(10) . . ? C34 C31 C30 113.2(8) . . ? C32 C31 C33 109.7(8) . . ? C34 C31 C33 110.9(10) . . ? C30 C31 C33 107.8(8) . . ? O5 C32 C31 108.4(8) . . ? O5 C32 H32A 110.0 . . ? C31 C32 H32A 110.0 . . ? O5 C32 H32B 110.0 . . ? C31 C32 H32B 110.0 . . ? H32A C32 H32B 108.4 . . ? O6 C33 C31 105.3(8) . . ? O6 C33 H33A 110.7 . . ? C31 C33 H33A 110.7 . . ? O6 C33 H33B 110.7 . . ? C31 C33 H33B 110.7 . . ? H33A C33 H33B 108.8 . . ? O7 C34 C31 107.6(8) . . ? O7 C34 H34A 110.2 . . ? C31 C34 H34A 110.2 . . ? O7 C34 H34B 110.2 . . ? C31 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? O7 C35 C36 125.4(10) . . ? O7 C35 C40 116.8(10) . . ? C36 C35 C40 117.8(12) . . ? C37 C36 C35 123.4(11) . . ? C37 C36 H36A 118.3 . . ? C35 C36 H36A 118.3 . . ? C36 C37 C38 119.5(10) . . ? C36 C37 H37A 120.2 . . ? C38 C37 H37A 120.2 . . ? C39 C38 C37 118.2(11) . . ? C39 C38 C43 122.0(10) . . ? C37 C38 C43 119.8(10) . . ? C40 C39 C38 121.3(10) . . ? C40 C39 H39A 119.3 . . ? C38 C39 H39A 119.3 . . ? C39 C40 C35 119.6(10) . . ? C39 C40 H40A 120.2 . . ? C35 C40 H40A 120.2 . . ? O15 C41 O19 125.6(12) . . ? O15 C41 C27 120.6(11) . . ? O19 C41 C27 113.9(13) . . ? O17 C42 O16 121.4(15) . . ? O17 C42 C9 120.1(12) . . ? O16 C42 C9 118.3(16) . . ? O13 C43 O14 124.8(12) . . ? O13 C43 C38 116.9(9) . . ? O14 C43 C38 118.3(10) . . ? O9 C47 O8 121.2(8) . . ? O9 C47 C15 117.7(10) . . ? O8 C47 C15 121.1(9) . . ? O20 C48 O28 119.2(10) . . ? O20 C48 C50 120.8(11) . . ? O28 C48 C50 119.9(9) . . ? O20 C48 Cd2 63.0(6) . . ? O28 C48 Cd2 56.3(5) . . ? C50 C48 Cd2 175.0(7) . . ? O11 C49 O10 122.6(11) . . ? O11 C49 C21 120.5(11) . . ? O10 C49 C21 116.9(10) . . ? C52 C50 C51 117.3(10) . . ? C52 C50 C48 122.1(10) . . ? C51 C50 C48 120.6(10) . . ? C62 C51 C50 119.9(11) . . ? C62 C51 H51A 120.0 . . ? C50 C51 H51A 120.0 . . ? C50 C52 C61 121.3(10) . . ? C50 C52 H52A 119.3 . . ? C61 C52 H52A 119.3 . . ? O6 C53 C62 116.7(10) . . ? O6 C53 C61 125.4(11) . . ? C62 C53 C61 117.9(10) . . ? C52 C61 C53 120.1(11) . . ? C52 C61 H61A 120.0 . . ? C53 C61 H61A 120.0 . . ? C53 C62 C51 123.4(11) . . ? C53 C62 H62A 118.3 . . ? C51 C62 H62A 118.3 . . ? O24 C64 N1 116.1(13) . . ? O24 C64 C83 121.7(13) . . ? N1 C64 C83 122.1(11) . . ? N1 C81 H81A 109.5 . . ? N1 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N1 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N1 C82 H82A 109.5 . . ? N1 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? N1 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C64 C83 H83A 109.5 . . ? C64 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C64 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N2 C85 O33 124(4) . . ? N2 C85 C87 119(3) . . ? O33 C85 C87 116(3) . . ? N2 C86 H86A 109.5 . . ? N2 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? N2 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C85 C87 H87A 109.5 . . ? C85 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C85 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N2 C88 H88A 109.5 . . ? N2 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? N2 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? N3 C89 O35 135(3) . . ? N3 C89 C92 121(3) . . ? O35 C89 C92 104(3) . . ? N3 C89 C90 33.1(13) . . ? O35 C89 C90 168(3) . . ? C92 C89 C90 88(2) . . ? N3 C90 C89 41.0(19) . . ? N3 C90 H90A 109.5 . . ? C89 C90 H90A 70.3 . . ? N3 C90 H90B 109.5 . . ? C89 C90 H90B 135.3 . . ? H90A C90 H90B 109.5 . . ? N3 C90 H90C 109.5 . . ? C89 C90 H90C 112.3 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? N3 C91 H91A 109.5 . . ? N3 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? N3 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C89 C92 H92A 109.5 . . ? C89 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C89 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C24 O1 C3 119.9(9) . . ? C6 O2 C4 119.0(9) . . ? C12 O3 C5 120.1(9) . . ? C30 O4 C2 116.8(8) . . ? C18 O5 C32 121.2(8) . . ? C53 O6 C33 120.5(9) . . ? C35 O7 C34 115.7(8) . . ? C47 O8 Cd1 133.6(7) . . ? C47 O9 Cd2 104.9(7) . 2_545 ? C49 O10 Cd2 130.0(8) . 1_565 ? C49 O11 Cd1 138.7(9) . . ? C43 O13 Cd4 107.9(7) . 2_334 ? C43 O14 Cd3 129.8(9) . . ? C43 O14 Cd3 127.1(9) . 2_334 ? Cd3 O14 Cd3 8.8(5) . 2_334 ? C41 O15 Cd3 135.9(9) . . ? C41 O15 Cd3 143.0(9) . 2_334 ? Cd3 O15 Cd3 7.4(7) . 2_334 ? C42 O16 Cd3 144.5(10) . 1_565 ? C42 O16 Cd4 109.3(10) . 1_565 ? Cd3 O16 Cd4 96.6(6) 1_565 1_565 ? C42 O16 Cd3 145.3(10) . 2_344 ? Cd3 O16 Cd3 5.2(11) 1_565 2_344 ? Cd4 O16 Cd3 99.2(6) 1_565 2_344 ? C41 O19 Cd4 124.7(10) . . ? C48 O20 Cd2 90.1(7) . . ? C64 O24 Cd2 127.1(8) . . ? C48 O28 Cd2 96.8(6) . . ? C48 O28 Cd1 162.8(7) . 1_545 ? Cd2 O28 Cd1 100.3(3) . 1_545 ? Cd4 O1W H1WA 108.4 . . ? Cd4 O1W H1WB 109.8 . . ? H1WA O1W H1WB 109.5 . . ? Cd4 O1W H1WC 110.2 . . ? H1WA O1W H1WC 109.5 . . ? H1WB O1W H1WC 109.5 . . ? Cd4 O2W H2WA 109.3 . . ? Cd4 O2W H2WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? Cd4 O2W H2WC 109.6 . . ? H2WA O2W H2WC 109.5 . . ? H2WB O2W H2WC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.817 _refine_diff_density_min -1.296 _refine_diff_density_rms 0.185 # Attachment '- 2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 865798' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H79 Co3 N8 O27' _chemical_formula_weight 1809.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.728(3) _cell_length_b 10.9381(13) _cell_length_c 34.326(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.917(2) _cell_angle_gamma 90.00 _cell_volume 9145.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description brick _exptl_crystal_colour purple _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3744 _exptl_absorpt_coefficient_mu 0.616 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6636 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24568 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 26.16 _reflns_number_total 9093 _reflns_number_gt 5858 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9093 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.2074 _refine_ls_wR_factor_gt 0.1790 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 Co1 Co 0.2500 0.2500 0.5000 0.0376(2) Uani 1 2 d S . . Co2 Co 0.18321(2) -0.04099(5) 0.502821(14) 0.04327(19) Uani 1 1 d . . . N1 N 0.09492(18) -0.3513(4) 0.52635(14) 0.0866(14) Uani 1 1 d . . . C31 C 0.1858(6) 0.0598(15) 0.7319(4) 0.207(5) Uiso 1 1 d . . . N3 N 0.0437(5) -0.8274(12) 0.5737(4) 0.231(5) Uiso 1 1 d . . . C43 C 0.079(2) 0.225(5) 0.8369(18) 0.60(3) Uiso 1 1 d . . . C1 C 0.42619(15) 0.0514(4) 0.78453(10) 0.0450(9) Uani 1 1 d . . . C2 C 0.46476(17) -0.0400(4) 0.76991(11) 0.0510(10) Uani 1 1 d . . . H2A H 0.4858 -0.0839 0.7920 0.061 Uiso 1 1 calc R . . H2B H 0.4441 -0.0986 0.7521 0.061 Uiso 1 1 calc R . . C3 C 0.39019(16) 0.1137(4) 0.74957(10) 0.0506(10) Uani 1 1 d . . . H3A H 0.3674 0.1758 0.7588 0.061 Uiso 1 1 calc R . . H3B H 0.4127 0.1522 0.7326 0.061 Uiso 1 1 calc R . . C4 C 0.39051(18) -0.0163(4) 0.81011(12) 0.0558(11) Uani 1 1 d . . . H4A H 0.3702 -0.0817 0.7951 0.067 Uiso 1 1 calc R . . H4B H 0.4132 -0.0510 0.8333 0.067 Uiso 1 1 calc R . . C5 C 0.45859(17) 0.1517(4) 0.80951(11) 0.0515(10) Uani 1 1 d . . . H5A H 0.4790 0.2006 0.7935 0.062 Uiso 1 1 calc R . . H5B H 0.4340 0.2049 0.8209 0.062 Uiso 1 1 calc R . . C6 C 0.33051(19) 0.0444(4) 0.69129(11) 0.0583(11) Uani 1 1 d . . . C7 C 0.32816(19) 0.1538(4) 0.67316(12) 0.0599(11) Uani 1 1 d . . . H7A H 0.3446 0.2217 0.6866 0.072 Uiso 1 1 calc R . . C8 C 0.30098(18) 0.1652(4) 0.63414(11) 0.0558(11) Uani 1 1 d . . . H8A H 0.3004 0.2406 0.6216 0.067 Uiso 1 1 calc R . . C9 C 0.27519(17) 0.0672(4) 0.61399(11) 0.0488(10) Uani 1 1 d . . . C10 C 0.2771(3) -0.0424(5) 0.63335(14) 0.092(2) Uani 1 1 d . . . H10A H 0.2598 -0.1102 0.6204 0.110 Uiso 1 1 calc R . . C11 C 0.3038(3) -0.0539(5) 0.67133(15) 0.108(3) Uani 1 1 d . . . H11A H 0.3040 -0.1291 0.6840 0.130 Uiso 1 1 calc R . . C12 C 0.24799(16) 0.0790(4) 0.57180(10) 0.0445(9) Uani 1 1 d . . . C13 C 0.33002(18) 0.0503(4) 0.85399(12) 0.0598(12) Uani 1 1 d . . . C14 C 0.3279(2) -0.0613(4) 0.87128(13) 0.0646(12) Uani 1 1 d . . . H14A H 0.3429 -0.1295 0.8610 0.078 Uiso 1 1 calc R . . C15 C 0.30304(18) -0.0722(4) 0.90436(12) 0.0577(11) Uani 1 1 d . . . H15A H 0.3020 -0.1479 0.9165 0.069 Uiso 1 1 calc R . . C16 C 0.27972(17) 0.0290(4) 0.91946(11) 0.0506(10) Uani 1 1 d . . . C17 C 0.28299(19) 0.1400(4) 0.90139(14) 0.0648(12) Uani 1 1 d . . . H17A H 0.2689 0.2091 0.9118 0.078 Uiso 1 1 calc R . . C18 C 0.3068(2) 0.1513(5) 0.86812(15) 0.0738(14) Uani 1 1 d . . . H18A H 0.3071 0.2263 0.8554 0.089 Uiso 1 1 calc R . . C19 C 0.25179(17) 0.0181(4) 0.95442(11) 0.0494(10) Uani 1 1 d . . . C20 C 0.52676(17) 0.1563(4) 0.86924(11) 0.0516(10) Uani 1 1 d . . . C21 C 0.5647(2) 0.0897(5) 0.89412(14) 0.0717(14) Uani 1 1 d . . . H21A H 0.5679 0.0061 0.8902 0.086 Uiso 1 1 calc R . . C22 C 0.59853(19) 0.1465(5) 0.92521(13) 0.0660(13) Uani 1 1 d . . . H22A H 0.6250 0.1010 0.9416 0.079 Uiso 1 1 calc R . . C23 C 0.59339(16) 0.2684(4) 0.93212(11) 0.0490(10) Uani 1 1 d . . . C24 C 0.55509(19) 0.3342(4) 0.90724(13) 0.0642(12) Uani 1 1 d . . . H24A H 0.5512 0.4173 0.9118 0.077 Uiso 1 1 calc R . . C25 C 0.5218(2) 0.2793(4) 0.87528(13) 0.0685(13) Uani 1 1 d . . . H25A H 0.4965 0.3255 0.8582 0.082 Uiso 1 1 calc R . . C26 C 0.63143(17) 0.3269(5) 0.96580(12) 0.0549(11) Uani 1 1 d . . . C27 C 0.12609(19) -0.2845(5) 0.50746(13) 0.0629(12) Uani 1 1 d . . . C28 C 0.1493(2) -0.3392(5) 0.47370(17) 0.0825(15) Uani 1 1 d . . . H28A H 0.1714 -0.2793 0.4633 0.124 Uiso 1 1 calc R . . H28B H 0.1198 -0.3645 0.4533 0.124 Uiso 1 1 calc R . . H28C H 0.1716 -0.4087 0.4830 0.124 Uiso 1 1 calc R . . C29 C 0.0817(3) -0.4795(6) 0.5155(2) 0.130(3) Uani 1 1 d . . . H29A H 0.1005 -0.5033 0.4944 0.195 Uiso 1 1 calc R . . H29B H 0.0428 -0.4877 0.5070 0.195 Uiso 1 1 calc R . . H29C H 0.0932 -0.5310 0.5381 0.195 Uiso 1 1 calc R . . C30 C 0.0710(3) -0.3004(7) 0.5576(2) 0.114(2) Uani 1 1 d . . . H30A H 0.0822 -0.2166 0.5615 0.171 Uiso 1 1 calc R . . H30B H 0.0830 -0.3458 0.5814 0.171 Uiso 1 1 calc R . . H30C H 0.0317 -0.3045 0.5508 0.171 Uiso 1 1 calc R . . N2 N 0.1744(13) -0.091(3) 0.7325(9) 0.504(16) Uiso 1 1 d . . . C32 C 0.2149(10) 0.171(3) 0.7502(7) 0.357(11) Uiso 1 1 d . . . C35 C 0.0877(8) -0.0492(17) 0.7942(6) 0.270(7) Uiso 1 1 d . . . C36 C 0.1300(9) -0.041(2) 0.6939(7) 0.327(10) Uiso 1 1 d . . . C37 C 0.1048(7) -0.9008(17) 0.5800(5) 0.278(8) Uiso 1 1 d . . . C38 C 0.0240(8) -0.868(2) 0.5317(7) 0.327(10) Uiso 1 1 d . . . C39 C 0.0332(18) -0.743(4) 0.6097(13) 0.50(2) Uiso 1 1 d . . . C40 C 0.0643(11) -0.803(2) 0.6327(8) 0.346(13) Uiso 1 1 d . . . C41 C 0.1503(8) -0.0007(18) 0.8518(6) 0.278(8) Uiso 1 1 d . . . O1 O 0.5000 0.0288(4) 0.7500 0.0633(11) Uani 1 2 d S . . O2 O 0.35687(14) 0.0200(3) 0.72863(8) 0.0740(10) Uani 1 1 d . . . O3 O 0.35405(14) 0.0718(3) 0.82132(9) 0.0754(10) Uani 1 1 d . . . O4 O 0.49545(13) 0.0892(3) 0.84026(9) 0.0692(9) Uani 1 1 d . . . O5 O 0.25248(12) 0.1784(3) 0.55529(7) 0.0554(7) Uani 1 1 d . . . O6 O 0.22212(13) -0.0141(3) 0.55613(8) 0.0586(8) Uani 1 1 d . . . O7 O 0.22474(13) 0.1095(3) 0.96315(9) 0.0653(8) Uani 1 1 d . . . O8 O 0.25448(13) -0.0765(3) 0.97406(8) 0.0628(8) Uani 1 1 d . . . O9 O 0.66505(12) 0.2594(3) 0.98750(9) 0.0632(8) Uani 1 1 d . . . O10 O 0.62672(13) 0.4403(3) 0.97055(9) 0.0653(8) Uani 1 1 d . . . O11 O 0.13540(13) -0.1743(3) 0.51755(9) 0.0651(8) Uani 1 1 d . . . O12 O 0.1434(8) 0.1647(19) 0.6972(6) 0.433(9) Uiso 1 1 d . . . O13 O -0.0100(9) -0.7316(17) 0.5683(6) 0.409(9) Uiso 1 1 d . . . C42 C 0.2237(10) -0.025(2) 0.7625(7) 0.335(10) Uiso 1 1 d . . . N5 N 0.1022(8) 0.0712(19) 0.8266(6) 0.311(7) Uiso 1 1 d . . . C44 C 0.0471(16) 0.106(5) 0.7974(12) 0.56(2) Uiso 1 1 d . . . O14 O 0.1092(17) 0.184(4) 0.8655(12) 0.64(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0479(4) 0.0389(4) 0.0250(3) -0.0023(3) 0.0031(3) -0.0040(3) Co2 0.0529(3) 0.0457(3) 0.0306(3) -0.0023(2) 0.0055(2) -0.0066(2) N1 0.077(3) 0.093(3) 0.089(3) 0.024(3) 0.011(2) -0.032(3) C1 0.049(2) 0.059(2) 0.0277(17) -0.0029(16) 0.0091(16) -0.0050(18) C2 0.060(2) 0.059(3) 0.037(2) -0.0004(18) 0.0153(18) -0.008(2) C3 0.057(2) 0.064(3) 0.0302(18) 0.0036(18) 0.0040(17) -0.013(2) C4 0.067(3) 0.065(3) 0.037(2) 0.0069(19) 0.0147(19) 0.002(2) C5 0.058(2) 0.061(3) 0.0340(19) -0.0020(18) 0.0012(17) 0.001(2) C6 0.073(3) 0.066(3) 0.0313(19) 0.0073(19) -0.0052(19) -0.022(2) C7 0.080(3) 0.054(3) 0.040(2) -0.0072(19) -0.005(2) -0.011(2) C8 0.077(3) 0.049(2) 0.036(2) 0.0040(18) -0.0031(19) -0.009(2) C9 0.060(3) 0.053(2) 0.0328(19) 0.0023(17) 0.0070(17) -0.0116(19) C10 0.140(5) 0.070(3) 0.048(3) 0.012(2) -0.029(3) -0.046(3) C11 0.170(6) 0.076(4) 0.058(3) 0.029(3) -0.038(4) -0.064(4) C12 0.050(2) 0.053(2) 0.0308(18) 0.0003(17) 0.0076(16) -0.0019(18) C13 0.065(3) 0.072(3) 0.048(2) 0.019(2) 0.026(2) 0.010(2) C14 0.089(3) 0.054(3) 0.060(3) 0.002(2) 0.036(3) 0.002(2) C15 0.080(3) 0.050(2) 0.048(2) 0.0056(19) 0.026(2) 0.001(2) C16 0.063(3) 0.051(2) 0.041(2) 0.0061(18) 0.0177(19) 0.0060(19) C17 0.079(3) 0.056(3) 0.068(3) 0.016(2) 0.038(2) 0.016(2) C18 0.092(4) 0.064(3) 0.075(3) 0.031(3) 0.042(3) 0.022(3) C19 0.058(2) 0.051(3) 0.041(2) 0.0035(19) 0.0138(19) -0.003(2) C20 0.058(2) 0.057(3) 0.036(2) -0.0044(18) -0.0006(18) 0.002(2) C21 0.078(3) 0.057(3) 0.071(3) -0.004(2) -0.013(3) 0.013(2) C22 0.067(3) 0.069(3) 0.053(3) 0.002(2) -0.017(2) 0.011(2) C23 0.048(2) 0.059(3) 0.038(2) 0.0000(18) 0.0013(17) -0.0018(19) C24 0.073(3) 0.053(3) 0.059(3) -0.006(2) -0.010(2) 0.006(2) C25 0.076(3) 0.063(3) 0.055(3) 0.001(2) -0.021(2) 0.007(2) C26 0.053(2) 0.072(3) 0.039(2) -0.005(2) 0.0065(19) -0.001(2) C27 0.062(3) 0.073(3) 0.052(3) 0.011(2) 0.004(2) -0.013(2) C28 0.089(4) 0.069(3) 0.091(4) -0.009(3) 0.020(3) -0.021(3) C29 0.143(6) 0.086(5) 0.159(7) 0.022(5) 0.021(5) -0.060(4) C30 0.099(5) 0.156(7) 0.096(5) 0.022(5) 0.042(4) -0.021(4) O1 0.075(3) 0.059(3) 0.066(3) 0.000 0.040(2) 0.000 O2 0.099(2) 0.078(2) 0.0356(15) 0.0167(15) -0.0152(15) -0.0345(19) O3 0.084(2) 0.089(2) 0.066(2) 0.0296(18) 0.0475(18) 0.0219(18) O4 0.084(2) 0.0610(19) 0.0517(17) -0.0101(15) -0.0196(16) 0.0006(16) O5 0.082(2) 0.0515(17) 0.0307(13) 0.0037(12) 0.0025(13) -0.0031(15) O6 0.080(2) 0.0580(18) 0.0347(14) -0.0002(13) 0.0014(13) -0.0182(15) O7 0.084(2) 0.061(2) 0.0590(18) 0.0069(15) 0.0350(16) 0.0169(17) O8 0.095(2) 0.0493(17) 0.0474(16) 0.0122(14) 0.0224(16) -0.0026(15) O9 0.0554(18) 0.080(2) 0.0482(16) 0.0032(15) -0.0077(14) 0.0013(16) O10 0.068(2) 0.064(2) 0.0579(18) -0.0102(15) -0.0063(15) 0.0024(16) O11 0.074(2) 0.063(2) 0.0620(18) -0.0026(16) 0.0217(15) -0.0205(16) _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 Co1 O5 2.044(3) . ? Co1 O5 2.044(3) 7_556 ? Co1 O9 2.073(3) 8_455 ? Co1 O9 2.073(3) 2_656 ? Co1 O8 2.108(3) 6 ? Co1 O8 2.108(3) 4_556 ? Co2 O6 1.938(3) . ? Co2 O10 1.964(3) 8_455 ? Co2 O7 1.988(3) 6 ? Co2 O11 1.996(3) . ? N1 C27 1.312(6) . ? N1 C30 1.423(8) . ? N1 C29 1.473(8) . ? C31 C32 1.50(3) . ? C31 C42 1.58(2) . ? C31 N2 1.67(3) . ? C31 O12 1.85(2) . ? N3 C38 1.51(2) . ? N3 C39 1.60(4) . ? N3 O13 1.68(2) . ? N3 C37 1.692(18) . ? C43 O14 1.21(7) . ? C43 N5 1.83(6) . ? C43 C44 1.95(6) . ? C1 C2 1.525(5) . ? C1 C3 1.526(5) . ? C1 C5 1.531(5) . ? C1 C4 1.537(5) . ? C2 O1 1.413(4) . ? C3 O2 1.429(5) . ? C4 O3 1.417(5) . ? C5 O4 1.443(5) . ? C6 C7 1.345(6) . ? C6 O2 1.361(5) . ? C6 C11 1.381(6) . ? C7 C8 1.397(5) . ? C8 C9 1.372(5) . ? C9 C10 1.368(6) . ? C9 C12 1.493(5) . ? C10 C11 1.362(7) . ? C12 O5 1.241(5) . ? C12 O6 1.271(5) . ? C13 C14 1.363(6) . ? C13 C18 1.372(6) . ? C13 O3 1.377(5) . ? C14 C15 1.386(6) . ? C15 C16 1.389(6) . ? C16 C17 1.372(6) . ? C16 C19 1.489(5) . ? C17 C18 1.377(6) . ? C19 O8 1.230(5) . ? C19 O7 1.267(5) . ? C20 O4 1.365(5) . ? C20 C21 1.366(6) . ? C20 C25 1.370(6) . ? C21 C22 1.384(6) . ? C22 C23 1.364(6) . ? C23 C24 1.366(6) . ? C23 C26 1.502(6) . ? C24 C25 1.389(6) . ? C26 O9 1.256(5) . ? C26 O10 1.259(5) . ? C27 O11 1.264(6) . ? C27 C28 1.503(7) . ? N2 C42 1.62(3) . ? N2 C36 1.66(3) . ? C35 N5 1.72(2) . ? C35 C44 1.98(5) . ? C39 C40 1.20(4) . ? C39 O13 1.63(4) . ? C41 N5 1.56(2) . ? O1 C2 1.413(4) 2_656 ? O7 Co2 1.988(3) 6_556 ? O8 Co1 2.108(3) 4_546 ? O9 Co1 2.073(3) 2_656 ? O10 Co2 1.964(3) 8_556 ? N5 C44 1.59(4) . ? N5 O14 1.81(4) . ? 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 O5 Co1 O5 180.000(1) . 7_556 ? O5 Co1 O9 92.32(12) . 8_455 ? O5 Co1 O9 87.68(12) 7_556 8_455 ? O5 Co1 O9 87.68(12) . 2_656 ? O5 Co1 O9 92.32(12) 7_556 2_656 ? O9 Co1 O9 180.00(4) 8_455 2_656 ? O5 Co1 O8 92.98(11) . 6 ? O5 Co1 O8 87.02(11) 7_556 6 ? O9 Co1 O8 89.60(12) 8_455 6 ? O9 Co1 O8 90.40(12) 2_656 6 ? O5 Co1 O8 87.02(11) . 4_556 ? O5 Co1 O8 92.98(11) 7_556 4_556 ? O9 Co1 O8 90.40(12) 8_455 4_556 ? O9 Co1 O8 89.60(12) 2_656 4_556 ? O8 Co1 O8 180.00(14) 6 4_556 ? O6 Co2 O10 129.55(14) . 8_455 ? O6 Co2 O7 118.23(14) . 6 ? O10 Co2 O7 103.07(14) 8_455 6 ? O6 Co2 O11 95.23(12) . . ? O10 Co2 O11 99.08(14) 8_455 . ? O7 Co2 O11 107.24(13) 6 . ? C27 N1 C30 120.7(5) . . ? C27 N1 C29 121.9(6) . . ? C30 N1 C29 117.4(5) . . ? C32 C31 C42 90.6(15) . . ? C32 C31 N2 150.2(19) . . ? C42 C31 N2 59.8(13) . . ? C32 C31 O12 86.7(13) . . ? C42 C31 O12 177.3(17) . . ? N2 C31 O12 122.8(16) . . ? C38 N3 C39 147(2) . . ? C38 N3 O13 87.7(13) . . ? C39 N3 O13 59.5(15) . . ? C38 N3 C37 96.7(13) . . ? C39 N3 C37 116(2) . . ? O13 N3 C37 169.6(14) . . ? O14 C43 N5 70(4) . . ? O14 C43 C44 116(5) . . ? N5 C43 C44 49.7(18) . . ? C2 C1 C3 110.3(3) . . ? C2 C1 C5 110.9(3) . . ? C3 C1 C5 107.4(3) . . ? C2 C1 C4 109.0(3) . . ? C3 C1 C4 110.5(3) . . ? C5 C1 C4 108.8(3) . . ? O1 C2 C1 106.5(3) . . ? O2 C3 C1 106.4(3) . . ? O3 C4 C1 106.4(3) . . ? O4 C5 C1 105.9(3) . . ? C7 C6 O2 125.8(4) . . ? C7 C6 C11 119.0(4) . . ? O2 C6 C11 115.2(4) . . ? C6 C7 C8 119.9(4) . . ? C9 C8 C7 121.3(4) . . ? C10 C9 C8 117.8(4) . . ? C10 C9 C12 121.2(4) . . ? C8 C9 C12 121.0(4) . . ? C11 C10 C9 121.1(4) . . ? C10 C11 C6 121.0(5) . . ? O5 C12 O6 125.9(3) . . ? O5 C12 C9 117.2(3) . . ? O6 C12 C9 116.8(4) . . ? C14 C13 C18 121.2(4) . . ? C14 C13 O3 124.2(4) . . ? C18 C13 O3 114.6(4) . . ? C13 C14 C15 119.3(4) . . ? C14 C15 C16 120.5(4) . . ? C17 C16 C15 118.4(4) . . ? C17 C16 C19 120.5(4) . . ? C15 C16 C19 121.1(4) . . ? C16 C17 C18 121.4(4) . . ? C13 C18 C17 119.1(4) . . ? O8 C19 O7 121.0(4) . . ? O8 C19 C16 121.3(4) . . ? O7 C19 C16 117.7(4) . . ? O4 C20 C21 114.3(4) . . ? O4 C20 C25 125.8(4) . . ? C21 C20 C25 119.9(4) . . ? C20 C21 C22 120.1(4) . . ? C23 C22 C21 120.7(4) . . ? C22 C23 C24 118.8(4) . . ? C22 C23 C26 119.1(4) . . ? C24 C23 C26 122.1(4) . . ? C23 C24 C25 121.2(4) . . ? C20 C25 C24 119.2(4) . . ? O9 C26 O10 124.7(4) . . ? O9 C26 C23 117.9(4) . . ? O10 C26 C23 117.4(4) . . ? O11 C27 N1 119.4(5) . . ? O11 C27 C28 121.0(4) . . ? N1 C27 C28 119.6(5) . . ? C42 N2 C36 133(3) . . ? C42 N2 C31 57.3(14) . . ? C36 N2 C31 75.9(18) . . ? N5 C35 C44 50.2(13) . . ? C40 C39 N3 91(3) . . ? C40 C39 O13 150(4) . . ? N3 C39 O13 62.6(19) . . ? C2 O1 C2 115.7(4) . 2_656 ? C6 O2 C3 118.3(3) . . ? C13 O3 C4 119.3(3) . . ? C20 O4 C5 119.1(3) . . ? C12 O5 Co1 140.3(3) . . ? C12 O6 Co2 130.8(3) . . ? C19 O7 Co2 102.7(3) . 6_556 ? C19 O8 Co1 170.7(3) . 4_546 ? C26 O9 Co1 134.1(3) . 2_656 ? C26 O10 Co2 123.6(3) . 8_556 ? C27 O11 Co2 135.6(3) . . ? C39 O13 N3 57.9(17) . . ? C31 C42 N2 62.8(15) . . ? C41 N5 C44 163(3) . . ? C41 N5 C35 91.5(15) . . ? C44 N5 C35 74(2) . . ? C41 N5 O14 88(2) . . ? C44 N5 O14 105(3) . . ? C35 N5 O14 169.8(19) . . ? C41 N5 C43 126(3) . . ? C44 N5 C43 69(2) . . ? C35 N5 C43 142(3) . . ? O14 N5 C43 39(2) . . ? N5 C44 C43 61(2) . . ? N5 C44 C35 56.2(17) . . ? C43 C44 C35 117(3) . . ? C43 O14 N5 72(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.16 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.686 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.168 # Attachment '- 3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 865799' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H59 Cd3 N7 O20' _chemical_formula_weight 1679.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.3592(14) _cell_length_b 15.488(2) _cell_length_c 16.108(3) _cell_angle_alpha 78.217(2) _cell_angle_beta 78.133(2) _cell_angle_gamma 84.160(2) _cell_volume 2232.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6157 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23177 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 26.09 _reflns_number_total 17255 _reflns_number_gt 15120 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0934P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(2) _refine_ls_number_reflns 17255 _refine_ls_number_parameters 887 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1524 _refine_ls_wR_factor_gt 0.1437 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.007 _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 Cd1 Cd 0.09064(4) 0.71769(3) -0.05520(3) 0.03467(12) Uani 1 1 d . . . Cd2 Cd 0.43905(4) 0.63169(3) -0.12321(3) 0.03599(12) Uani 1 1 d . . . Cd3 Cd -0.15358(5) 1.59800(3) -0.18747(3) 0.03794(14) Uani 1 1 d . . . N1 N -0.0510(7) 1.2317(4) 0.1641(5) 0.0518(15) Uani 1 1 d . . . N2 N -0.0153(8) 1.0779(4) 0.1914(5) 0.0543(17) Uani 1 1 d . . . N3 N -0.0300(8) 1.1554(4) 0.0511(4) 0.0566(17) Uani 1 1 d . . . N5 N -0.1068(7) 1.4708(4) -0.0893(4) 0.0457(14) Uani 1 1 d . . . N6 N -0.0476(12) 1.1530(11) 0.4798(7) 0.107(4) Uani 1 1 d . . . N4 N 0.0548(8) 0.8434(4) 0.0080(5) 0.0552(17) Uani 1 1 d . . . C1 C 0.4687(8) -0.0027(4) 0.2833(4) 0.0382(15) Uani 1 1 d . . . C2 C 0.3957(8) 0.0644(5) 0.2172(5) 0.0433(16) Uani 1 1 d . . . H2A H 0.3438 0.0341 0.1866 0.052 Uiso 1 1 calc R . . H2B H 0.3267 0.1049 0.2462 0.052 Uiso 1 1 calc R . . C3 C 0.5622(9) 0.0432(5) 0.3236(5) 0.0456(16) Uani 1 1 d . . . H3A H 0.5974 0.0021 0.3702 0.055 Uiso 1 1 calc R . . H3B H 0.6462 0.0649 0.2809 0.055 Uiso 1 1 calc R . . C4 C 0.3425(8) -0.0428(5) 0.3508(5) 0.0452(17) Uani 1 1 d . . . H4A H 0.2895 0.0018 0.3818 0.054 Uiso 1 1 calc R . . H4B H 0.2754 -0.0656 0.3232 0.054 Uiso 1 1 calc R . . C5 C 0.5602(8) -0.0716(5) 0.2393(4) 0.0413(15) Uani 1 1 d . . . H5A H 0.6442 -0.0455 0.1998 0.050 Uiso 1 1 calc R . . H5B H 0.5954 -0.1181 0.2819 0.050 Uiso 1 1 calc R . . C6 C 0.5628(9) 0.1742(5) 0.3777(5) 0.0450(17) Uani 1 1 d . . . H6A H 0.6165 0.2091 0.3258 0.054 Uiso 1 1 calc R . . H6B H 0.6322 0.1427 0.4121 0.054 Uiso 1 1 calc R . . C7 C 0.4555(8) 0.2335(4) 0.4290(4) 0.0358(14) Uani 1 1 d . . . C8 C 0.5458(9) 0.2873(5) 0.4655(5) 0.0422(17) Uani 1 1 d . . . H8A H 0.5995 0.2488 0.5055 0.051 Uiso 1 1 calc R . . H8B H 0.6153 0.3195 0.4193 0.051 Uiso 1 1 calc R . . C10 C 0.3570(9) 0.1758(5) 0.5016(5) 0.0473(18) Uani 1 1 d . . . H10A H 0.2919 0.2117 0.5380 0.057 Uiso 1 1 calc R . . H10B H 0.2986 0.1416 0.4785 0.057 Uiso 1 1 calc R . . C11 C 0.3563(8) 0.2911(4) 0.3750(4) 0.0385(14) Uani 1 1 d . . . H11A H 0.3062 0.2554 0.3484 0.046 Uiso 1 1 calc R . . H11B H 0.2837 0.3243 0.4104 0.046 Uiso 1 1 calc R . . C12 C 0.3835(8) 0.4105(5) 0.2534(4) 0.0453(16) Uani 1 1 d . . . C13 C 0.4774(9) 0.4695(6) 0.1940(6) 0.065(2) Uani 1 1 d . . . H13A H 0.5765 0.4656 0.1960 0.078 Uiso 1 1 calc R . . C14 C 0.3983(12) 0.4469(7) 0.6057(7) 0.078(3) Uani 1 1 d . . . H14A H 0.3003 0.4497 0.6014 0.094 Uiso 1 1 calc R . . C15 C 0.4030(10) 0.0463(6) 0.6068(6) 0.061(2) Uani 1 1 d . . . C16 C 0.2617(9) 0.0265(6) 0.6312(5) 0.058(2) Uani 1 1 d . . . H16A H 0.1906 0.0632 0.6064 0.070 Uiso 1 1 calc R . . C17 C 0.2209(9) -0.0475(5) 0.6926(5) 0.056(2) Uani 1 1 d . . . H17A H 0.1229 -0.0599 0.7104 0.067 Uiso 1 1 calc R . . C18 C 0.4720(9) 0.1905(5) 0.1108(5) 0.056(2) Uani 1 1 d . . . C19 C 0.3067(9) -0.1564(5) 0.4748(5) 0.0506(18) Uani 1 1 d . . . C20 C 0.1602(10) -0.1382(6) 0.4889(6) 0.071(3) Uani 1 1 d . . . H20A H 0.1178 -0.0946 0.4508 0.085 Uiso 1 1 calc R . . C21 C -0.0123(9) 1.0811(5) 0.1057(5) 0.0504(18) Uani 1 1 d . . . C22 C -0.0371(8) 1.1543(5) 0.2169(5) 0.0488(17) Uani 1 1 d . . . C23 C -0.0510(9) 1.2300(5) 0.0837(5) 0.0484(18) Uani 1 1 d . . . C24 C -0.0717(9) 1.3130(5) 0.0245(5) 0.0484(17) Uani 1 1 d . . . C25 C -0.0794(16) 1.3144(6) -0.0595(6) 0.085(4) Uani 1 1 d . . . H25A H -0.0695 1.2621 -0.0807 0.102 Uiso 1 1 calc R . . C26 C -0.0811(10) 1.3935(5) 0.0495(6) 0.058(2) Uani 1 1 d . . . H26A H -0.0764 1.3955 0.1062 0.069 Uiso 1 1 calc R . . C27 C -0.0402(9) 1.1547(6) 0.3099(6) 0.057(2) Uani 1 1 d . . . C28 C -0.0418(11) 1.2337(7) 0.3382(7) 0.071(3) Uani 1 1 d . . . H28A H -0.0415 1.2875 0.2998 0.085 Uiso 1 1 calc R . . C29 C -0.0458(13) 1.0775(7) 0.3713(7) 0.077(3) Uani 1 1 d . . . H29A H -0.0478 1.0229 0.3559 0.093 Uiso 1 1 calc R . . C30 C 0.0169(16) 0.9981(6) -0.0092(6) 0.089(4) Uani 1 1 d . . . H30A H 0.0025 1.0512 -0.0464 0.107 Uiso 1 1 calc R . . C31 C 0.0092(9) 0.9990(5) 0.0742(5) 0.0534(19) Uani 1 1 d . . . C32 C 0.0318(9) -0.3060(5) 0.6879(5) 0.0487(18) Uani 1 1 d . . . C33 C 0.1283(9) -0.2519(6) 0.6150(5) 0.0530(19) Uani 1 1 d . . . C34 C 0.7368(7) -0.3053(4) -0.0572(4) 0.0297(12) Uani 1 1 d . . . C35 C 0.6696(7) -0.2544(5) 0.0095(5) 0.0309(15) Uani 1 1 d . . . C36 C 0.2124(8) 0.6105(5) 0.0685(4) 0.0412(15) Uani 1 1 d . . . C37 C 0.2718(8) 0.5411(5) 0.1330(4) 0.0412(15) Uani 1 1 d . . . C38 C 0.2377(9) 0.4186(6) 0.2528(5) 0.058(2) Uani 1 1 d . . . H38A H 0.1755 0.3808 0.2933 0.070 Uiso 1 1 calc R . . C39 C 0.1807(9) 0.4823(6) 0.1924(5) 0.055(2) Uani 1 1 d . . . H39A H 0.0812 0.4859 0.1916 0.067 Uiso 1 1 calc R . . C40 C 0.3274(10) -0.1027(5) 0.7271(5) 0.0505(19) Uani 1 1 d . . . C41 C 0.5324(8) -0.2117(6) 0.0092(6) 0.054(2) Uani 1 1 d . . . H41A H 0.4814 -0.2159 -0.0336 0.065 Uiso 1 1 calc R . . C42 C 0.3764(9) 0.4381(5) -0.0416(5) 0.0527(19) Uani 1 1 d . . . C43 C 0.7374(8) -0.2504(5) 0.0766(5) 0.0447(16) Uani 1 1 d . . . H43A H 0.8258 -0.2825 0.0813 0.054 Uiso 1 1 calc R . . C44 C 0.4715(9) -0.1638(6) 0.0710(6) 0.059(2) Uani 1 1 d . . . H44A H 0.3793 -0.1352 0.0703 0.071 Uiso 1 1 calc R . . C45 C 0.2851(10) -0.1825(5) 0.7969(5) 0.0496(19) Uani 1 1 d . . . C46 C -0.0974(10) 1.4705(5) -0.0074(6) 0.058(2) Uani 1 1 d . . . H46A H -0.1020 1.5240 0.0110 0.070 Uiso 1 1 calc R . . C47 C 0.0335(10) 0.9165(5) 0.1240(6) 0.059(2) Uani 1 1 d . . . H47A H 0.0361 0.9119 0.1822 0.070 Uiso 1 1 calc R . . C48 C 0.0532(10) 0.8434(5) 0.0895(5) 0.056(2) Uani 1 1 d . . . H48A H 0.0665 0.7894 0.1256 0.067 Uiso 1 1 calc R . . C49 C 0.5451(9) -0.1577(6) 0.1332(6) 0.052(2) Uani 1 1 d . . . C50 C 0.6768(9) -0.2002(6) 0.1358(5) 0.054(2) Uani 1 1 d . . . H50A H 0.7268 -0.1952 0.1787 0.064 Uiso 1 1 calc R . . C51 C 0.4142(8) 0.3516(5) 0.0111(6) 0.056(2) Uani 1 1 d . . . C52 C 0.2761(11) -0.2701(8) 0.6006(7) 0.085(3) Uani 1 1 d . . . H52A H 0.3185 -0.3149 0.6375 0.102 Uiso 1 1 calc R . . C53 C 0.6334(14) 0.5414(6) 0.7238(5) 0.065(3) Uani 1 1 d . . . C55 C -0.0439(13) 1.2307(10) 0.4219(8) 0.087(3) Uani 1 1 d . . . H55A H -0.0428 1.2832 0.4413 0.104 Uiso 1 1 calc R . . C57 C 0.4718(11) -0.0868(7) 0.6979(6) 0.082(3) Uani 1 1 d . . . H57A H 0.5438 -0.1272 0.7175 0.098 Uiso 1 1 calc R . . C58 C 0.5104(12) -0.0108(8) 0.6396(8) 0.107(5) Uani 1 1 d . . . H58A H 0.6081 0.0022 0.6222 0.128 Uiso 1 1 calc R . . C59 C 0.5034(10) 0.3929(6) 0.5583(6) 0.059(2) Uani 1 1 d . . . C60 C 0.4432(12) 0.4944(6) 0.6573(7) 0.071(3) Uani 1 1 d . . . H60A H 0.3749 0.5309 0.6868 0.085 Uiso 1 1 calc R . . C61 C 0.5810(11) 0.4899(6) 0.6664(5) 0.054(2) Uani 1 1 d . . . C62 C 0.3622(12) -0.2203(8) 0.5295(7) 0.091(4) Uani 1 1 d . . . H62A H 0.4629 -0.2325 0.5201 0.110 Uiso 1 1 calc R . . C63 C 0.0749(11) -0.1850(7) 0.5604(6) 0.075(3) Uani 1 1 d . . . H63A H -0.0248 -0.1695 0.5716 0.090 Uiso 1 1 calc R . . C64 C -0.1023(16) 1.3950(6) -0.1128(6) 0.089(4) Uani 1 1 d . . . H64A H -0.1151 1.3948 -0.1685 0.107 Uiso 1 1 calc R . . C65 C -0.0481(16) 1.0833(9) 0.4507(8) 0.096(4) Uani 1 1 d . . . H65A H -0.0505 1.0304 0.4905 0.115 Uiso 1 1 calc R . . C66 C 0.0443(17) 0.9244(6) -0.0415(6) 0.098(4) Uani 1 1 d . . . H66A H 0.0569 0.9289 -0.1010 0.118 Uiso 1 1 calc R . . C67 C 0.3402(13) 0.2126(8) 0.0913(11) 0.139(7) Uani 1 1 d . . . H67A H 0.2679 0.1722 0.1084 0.167 Uiso 1 1 calc R . . C68 C 0.3121(14) 0.2940(9) 0.0463(12) 0.143(7) Uani 1 1 d . . . H68A H 0.2163 0.3108 0.0396 0.171 Uiso 1 1 calc R . . C69 C 0.5371(12) 0.3330(8) 0.0403(10) 0.110(5) Uani 1 1 d . . . H69A H 0.6033 0.3766 0.0297 0.132 Uiso 1 1 calc R . . C70 C 0.5707(12) 0.2510(8) 0.0859(10) 0.122(6) Uani 1 1 d . . . H70A H 0.6633 0.2377 0.0995 0.146 Uiso 1 1 calc R . . C71 C 0.6844(12) 0.4348(8) 0.6237(7) 0.078(3) Uani 1 1 d . . . H71A H 0.7812 0.4312 0.6306 0.094 Uiso 1 1 calc R . . C72 C 0.4236(9) 0.5327(6) 0.1333(5) 0.064(3) Uani 1 1 d . . . H72A H 0.4866 0.5699 0.0926 0.077 Uiso 1 1 calc R . . C73 C 0.6430(12) 0.3853(9) 0.5710(8) 0.087(4) Uani 1 1 d . . . H73A H 0.7113 0.3467 0.5443 0.105 Uiso 1 1 calc R . . O1 O 0.4793(6) 0.1140(4) 0.3558(4) 0.0556(14) Uani 1 1 d . . . O23 O 0.1998(5) 0.6057(3) -0.1326(3) 0.0400(11) Uani 1 1 d . . . O2 O 0.5110(6) 0.1115(4) 0.1583(4) 0.0691(18) Uani 1 1 d . . . O3 O 0.4010(6) -0.1116(4) 0.4082(4) 0.0612(15) Uani 1 1 d . . . O4 O 0.4488(5) 0.3502(3) 0.3097(3) 0.0495(12) Uani 1 1 d . . . O5 O 0.4479(7) 0.3469(4) 0.5086(4) 0.0636(16) Uani 1 1 d . . . O6 O 0.4543(7) 0.1187(5) 0.5497(4) 0.080(2) Uani 1 1 d . . . O7 O 0.4750(6) -0.1069(4) 0.1938(4) 0.0627(17) Uani 1 1 d . . . O8 O -0.0983(7) -0.2811(4) 0.7077(4) 0.0694(17) Uani 1 1 d . . . O9 O 0.0810(6) -0.3761(4) 0.7290(3) 0.0526(13) Uani 1 1 d . . . O10 O 0.1523(6) -0.1949(4) 0.8186(3) 0.0548(14) Uani 1 1 d . . . O11 O 0.0759(6) 0.6196(4) 0.0734(3) 0.0504(13) Uani 1 1 d . . . O12 O 0.2964(5) 0.6564(3) 0.0103(3) 0.0415(11) Uani 1 1 d . . . O14 O 0.6592(5) -0.3350(4) -0.0995(3) 0.0425(12) Uani 1 1 d . . . O17 O 0.4753(6) 0.4931(4) -0.0645(4) 0.0616(16) Uani 1 1 d . . . O18 O 0.2523(7) 0.4524(4) -0.0577(5) 0.086(2) Uani 1 1 d . . . O19 O 0.7571(10) 0.5197(5) 0.7396(4) 0.080(2) Uani 1 1 d . . . O20 O 0.8737(5) -0.3209(3) -0.0737(3) 0.0362(10) Uiso 1 1 d . . . O21 O 0.3873(7) -0.2272(4) 0.8272(4) 0.0625(16) Uani 1 1 d . . . O22 O 0.5438(10) 0.6025(4) 0.7488(4) 0.076(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0354(2) 0.0279(2) 0.0405(3) 0.00127(19) -0.0139(2) -0.00341(19) Cd2 0.0335(2) 0.0323(2) 0.0424(3) -0.0013(2) -0.0120(2) -0.00480(18) Cd3 0.0424(3) 0.0359(3) 0.0367(3) -0.0104(2) -0.0054(2) -0.0053(2) N1 0.054(4) 0.036(3) 0.068(4) -0.012(3) -0.017(3) -0.003(3) N2 0.057(4) 0.036(3) 0.067(4) -0.003(3) -0.013(3) 0.000(3) N3 0.070(5) 0.038(3) 0.059(4) -0.006(3) -0.012(3) 0.002(3) N5 0.057(4) 0.036(3) 0.044(3) -0.007(3) -0.010(3) -0.003(3) N6 0.083(7) 0.172(13) 0.066(6) -0.023(8) -0.022(5) 0.014(8) N4 0.064(4) 0.031(3) 0.071(4) -0.004(3) -0.021(3) 0.003(3) C1 0.044(4) 0.030(3) 0.040(4) -0.007(3) -0.005(3) -0.005(3) C2 0.039(4) 0.038(4) 0.047(4) 0.000(3) -0.003(3) -0.005(3) C3 0.055(4) 0.034(4) 0.052(4) -0.017(3) -0.014(3) 0.001(3) C4 0.051(4) 0.040(4) 0.040(4) -0.006(3) 0.003(3) -0.007(3) C5 0.050(4) 0.033(3) 0.041(4) -0.011(3) -0.003(3) -0.006(3) C6 0.059(5) 0.031(4) 0.052(4) -0.007(3) -0.028(4) -0.007(3) C7 0.052(4) 0.025(3) 0.031(3) -0.004(2) -0.012(3) -0.003(3) C8 0.057(4) 0.036(4) 0.040(4) -0.013(3) -0.019(3) -0.003(3) C10 0.065(5) 0.037(4) 0.037(4) 0.007(3) -0.015(3) -0.007(3) C11 0.053(4) 0.029(3) 0.035(3) 0.002(3) -0.016(3) -0.008(3) C12 0.051(4) 0.044(4) 0.037(3) 0.009(3) -0.013(3) -0.005(3) C13 0.039(4) 0.068(6) 0.076(6) 0.025(5) -0.020(4) -0.011(4) C14 0.064(6) 0.083(7) 0.106(8) -0.058(7) -0.035(6) 0.028(5) C15 0.065(5) 0.045(5) 0.061(5) 0.030(4) -0.018(4) -0.015(4) C16 0.056(5) 0.047(4) 0.062(5) 0.019(4) -0.021(4) 0.002(4) C17 0.055(5) 0.050(4) 0.052(4) 0.016(4) -0.009(4) -0.004(4) C18 0.043(4) 0.051(5) 0.061(5) 0.014(4) -0.003(4) -0.001(3) C19 0.051(4) 0.049(4) 0.042(4) 0.004(3) -0.001(3) 0.001(3) C20 0.062(5) 0.063(6) 0.068(6) 0.025(4) -0.003(4) -0.003(4) C21 0.059(5) 0.030(4) 0.060(5) -0.002(3) -0.014(4) 0.001(3) C22 0.043(4) 0.044(4) 0.059(4) -0.007(3) -0.009(3) -0.004(3) C23 0.057(5) 0.030(4) 0.060(5) -0.009(3) -0.015(4) -0.002(3) C24 0.051(4) 0.029(3) 0.065(5) -0.006(3) -0.014(4) -0.002(3) C25 0.167(12) 0.034(4) 0.060(5) -0.020(4) -0.032(6) 0.011(6) C26 0.082(6) 0.036(4) 0.060(5) -0.011(3) -0.027(4) 0.001(4) C27 0.044(4) 0.059(5) 0.065(5) -0.007(4) -0.008(4) -0.005(4) C28 0.068(6) 0.079(7) 0.071(6) -0.020(5) -0.009(5) -0.024(5) C29 0.093(8) 0.057(6) 0.073(7) -0.004(5) -0.007(6) 0.008(5) C30 0.166(12) 0.027(4) 0.066(6) 0.006(4) -0.027(7) 0.009(5) C31 0.065(5) 0.034(4) 0.060(5) -0.003(3) -0.018(4) 0.000(3) C32 0.059(5) 0.047(4) 0.039(4) 0.000(3) -0.010(3) -0.011(4) C33 0.058(5) 0.056(5) 0.042(4) 0.000(3) -0.006(3) -0.013(4) C34 0.034(3) 0.028(3) 0.032(3) -0.007(2) -0.012(3) -0.006(2) C35 0.021(3) 0.031(3) 0.041(4) -0.009(3) -0.003(3) -0.005(3) C36 0.048(4) 0.036(4) 0.038(3) -0.002(3) -0.011(3) 0.000(3) C37 0.043(4) 0.039(4) 0.039(3) 0.006(3) -0.014(3) -0.003(3) C38 0.061(5) 0.059(5) 0.045(4) 0.023(4) -0.013(4) -0.022(4) C39 0.050(4) 0.056(5) 0.056(5) 0.013(4) -0.021(4) -0.007(4) C40 0.072(5) 0.032(4) 0.043(4) 0.010(3) -0.016(4) -0.006(3) C41 0.036(4) 0.062(5) 0.081(6) -0.046(4) -0.022(4) 0.005(3) C42 0.047(4) 0.040(4) 0.064(5) 0.011(3) -0.014(4) -0.004(3) C43 0.037(4) 0.056(4) 0.044(4) -0.019(3) -0.009(3) 0.005(3) C44 0.037(4) 0.069(6) 0.081(6) -0.043(5) -0.012(4) 0.009(4) C45 0.078(6) 0.032(4) 0.040(4) 0.003(3) -0.020(4) -0.008(4) C46 0.083(6) 0.029(4) 0.066(5) -0.007(3) -0.025(4) -0.006(4) C47 0.077(6) 0.041(4) 0.059(5) -0.005(4) -0.022(4) 0.001(4) C48 0.085(6) 0.031(4) 0.054(5) 0.001(3) -0.030(4) 0.004(4) C49 0.041(4) 0.055(5) 0.066(5) -0.033(4) -0.003(4) -0.004(4) C50 0.053(5) 0.072(6) 0.045(4) -0.028(4) -0.016(4) 0.002(4) C51 0.039(4) 0.037(4) 0.080(6) 0.016(4) -0.010(4) -0.007(3) C52 0.060(6) 0.090(8) 0.082(7) 0.024(6) -0.004(5) -0.001(5) C53 0.103(8) 0.054(5) 0.039(4) -0.004(4) -0.011(5) -0.027(5) C55 0.077(7) 0.110(10) 0.081(8) -0.047(7) -0.006(6) -0.005(7) C57 0.065(6) 0.079(7) 0.081(6) 0.048(5) -0.022(5) -0.019(5) C58 0.061(6) 0.103(9) 0.132(10) 0.073(8) -0.044(6) -0.029(6) C59 0.072(6) 0.052(5) 0.066(5) -0.027(4) -0.027(4) -0.005(4) C60 0.075(6) 0.060(6) 0.094(7) -0.045(5) -0.028(6) 0.009(5) C61 0.078(6) 0.048(5) 0.044(4) -0.023(4) -0.012(4) -0.010(4) C62 0.068(6) 0.082(7) 0.088(7) 0.037(6) 0.014(5) -0.002(5) C63 0.054(5) 0.081(7) 0.067(6) 0.019(5) 0.008(4) -0.003(5) C64 0.179(13) 0.029(4) 0.057(5) -0.006(4) -0.021(6) 0.000(6) C65 0.135(12) 0.084(8) 0.066(7) -0.022(6) -0.021(7) 0.026(8) C66 0.194(14) 0.035(5) 0.056(5) 0.006(4) -0.029(7) 0.017(6) C67 0.067(7) 0.095(9) 0.220(16) 0.106(10) -0.059(9) -0.051(6) C68 0.072(7) 0.094(9) 0.227(18) 0.089(11) -0.060(10) -0.021(7) C69 0.058(6) 0.070(7) 0.176(13) 0.064(8) -0.035(7) -0.028(5) C70 0.055(6) 0.092(9) 0.182(14) 0.074(9) -0.032(7) -0.015(6) C71 0.069(6) 0.096(8) 0.088(7) -0.053(6) -0.019(5) -0.011(5) C72 0.046(4) 0.074(6) 0.060(5) 0.033(4) -0.018(4) -0.015(4) C73 0.070(7) 0.113(9) 0.104(8) -0.077(8) -0.019(6) -0.004(6) O1 0.050(3) 0.048(3) 0.079(4) -0.034(3) -0.016(3) 0.001(2) O23 0.034(2) 0.033(2) 0.055(3) -0.005(2) -0.017(2) -0.0011(19) O2 0.050(3) 0.049(3) 0.085(4) 0.032(3) -0.004(3) -0.001(3) O3 0.052(3) 0.060(4) 0.052(3) 0.015(3) 0.006(2) 0.006(3) O4 0.047(3) 0.045(3) 0.047(3) 0.020(2) -0.013(2) -0.007(2) O5 0.069(4) 0.061(4) 0.081(4) -0.046(3) -0.035(3) 0.011(3) O6 0.073(4) 0.075(4) 0.081(4) 0.048(3) -0.037(3) -0.027(3) O7 0.043(3) 0.076(4) 0.080(4) -0.055(3) 0.001(3) -0.004(3) O8 0.065(4) 0.068(4) 0.060(4) 0.009(3) 0.003(3) -0.008(3) O9 0.054(3) 0.056(3) 0.046(3) -0.004(2) -0.006(2) -0.015(3) O10 0.064(4) 0.046(3) 0.044(3) 0.015(2) -0.007(3) -0.012(3) O11 0.045(3) 0.053(3) 0.046(3) 0.009(2) -0.014(2) 0.005(2) O12 0.049(3) 0.033(2) 0.039(2) 0.008(2) -0.014(2) -0.007(2) O14 0.034(2) 0.051(3) 0.052(3) -0.024(2) -0.012(2) -0.006(2) O17 0.049(3) 0.040(3) 0.084(4) 0.013(3) -0.009(3) -0.003(2) O18 0.069(4) 0.044(3) 0.140(6) 0.032(4) -0.050(4) -0.013(3) O19 0.111(6) 0.078(5) 0.070(4) -0.029(4) -0.035(4) -0.027(4) O21 0.083(4) 0.036(3) 0.072(4) 0.017(3) -0.042(3) -0.016(3) O22 0.137(6) 0.052(4) 0.043(3) -0.022(3) -0.009(4) -0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O10 2.203(5) 1_564 ? Cd1 O20 2.266(5) 1_465 ? Cd1 O11 2.293(5) . ? Cd1 N4 2.340(7) . ? Cd1 O23 2.367(5) . ? Cd1 O12 2.403(5) . ? Cd1 C36 2.687(7) . ? Cd1 Cd2 3.4424(7) . ? Cd2 O17 2.184(5) . ? Cd2 O21 2.210(5) 1_564 ? Cd2 O22 2.208(6) 1_554 ? Cd2 O14 2.298(5) 1_565 ? Cd2 O23 2.355(5) . ? Cd2 O12 2.367(5) . ? Cd3 O19 2.178(6) 1_464 ? Cd3 O8 2.275(6) 1_574 ? Cd3 O14 2.316(5) 1_475 ? Cd3 N5 2.325(6) . ? Cd3 O9 2.353(5) 1_574 ? Cd3 O20 2.490(5) 1_475 ? Cd3 C32 2.669(7) 1_574 ? N1 C23 1.301(10) . ? N1 C22 1.332(10) . ? N2 C22 1.312(10) . ? N2 C21 1.367(11) . ? N3 C21 1.316(10) . ? N3 C23 1.344(10) . ? N5 C64 1.299(11) . ? N5 C46 1.339(10) . ? N6 C65 1.263(18) . ? N6 C55 1.362(18) . ? N4 C48 1.309(11) . ? N4 C66 1.349(11) . ? C1 C5 1.499(10) . ? C1 C3 1.498(10) . ? C1 C4 1.519(9) . ? C1 C2 1.543(10) . ? C2 O2 1.432(8) . ? C3 O1 1.402(9) . ? C4 O3 1.407(9) . ? C5 O7 1.402(9) . ? C6 O1 1.415(9) . ? C6 C7 1.522(10) . ? C7 C11 1.504(9) . ? C7 C8 1.518(10) . ? C7 C10 1.521(10) . ? C8 O5 1.414(9) . ? C10 O6 1.434(9) . ? C11 O4 1.445(8) . ? C12 O4 1.354(8) . ? C12 C38 1.360(11) . ? C12 C13 1.409(10) . ? C13 C72 1.371(11) . ? C14 C60 1.366(13) . ? C14 C59 1.425(12) . ? C15 C16 1.348(12) . ? C15 O6 1.357(9) . ? C15 C58 1.384(13) . ? C16 C17 1.382(10) . ? C17 C40 1.376(11) . ? C18 C67 1.329(14) . ? C18 C70 1.327(14) . ? C18 O2 1.364(9) . ? C19 C62 1.325(13) . ? C19 C20 1.353(12) . ? C19 O3 1.357(9) . ? C20 C63 1.374(11) . ? C21 C31 1.443(11) . ? C22 C27 1.494(12) . ? C23 C24 1.458(11) . ? C24 C25 1.366(12) . ? C24 C26 1.376(11) . ? C25 C64 1.387(13) . ? C26 C46 1.363(11) . ? C27 C29 1.385(14) . ? C27 C28 1.389(13) . ? C28 C55 1.335(15) . ? C29 C65 1.296(16) . ? C30 C66 1.328(14) . ? C30 C31 1.334(13) . ? C31 C47 1.388(11) . ? C32 O8 1.236(10) . ? C32 O9 1.248(9) . ? C32 C33 1.488(10) . ? C32 Cd3 2.669(7) 1_536 ? C33 C63 1.341(12) . ? C33 C52 1.365(13) . ? C34 O20 1.263(8) . ? C34 O14 1.266(8) . ? C34 C35 1.462(9) . ? C35 C43 1.376(10) . ? C35 C41 1.384(10) . ? C36 O12 1.241(8) . ? C36 O11 1.259(9) . ? C36 C37 1.485(9) . ? C37 C39 1.392(10) . ? C37 C72 1.415(10) . ? C38 C39 1.385(10) . ? C40 C57 1.367(13) . ? C40 C45 1.515(10) . ? C41 C44 1.360(11) . ? C42 O18 1.230(10) . ? C42 O17 1.269(9) . ? C42 C51 1.484(10) . ? C43 C50 1.350(10) . ? C44 C49 1.351(12) . ? C45 O21 1.245(10) . ? C45 O10 1.244(10) . ? C47 C48 1.341(12) . ? C49 C50 1.341(11) . ? C49 O7 1.395(9) . ? C51 C69 1.314(14) . ? C51 C68 1.332(14) . ? C52 C62 1.393(12) . ? C53 O19 1.235(13) . ? C53 O22 1.271(13) . ? C53 C61 1.517(12) . ? C57 C58 1.377(12) . ? C59 C73 1.353(14) . ? C59 O5 1.379(9) . ? C60 C61 1.321(14) . ? C61 C71 1.391(14) . ? C67 C68 1.350(15) . ? C69 C70 1.372(14) . ? C71 C73 1.387(13) . ? O8 Cd3 2.275(6) 1_536 ? O9 Cd3 2.353(5) 1_536 ? O10 Cd1 2.203(5) 1_546 ? O14 Cd2 2.298(5) 1_545 ? O14 Cd3 2.316(5) 1_635 ? O19 Cd3 2.178(6) 1_646 ? O20 Cd1 2.266(5) 1_645 ? O20 Cd3 2.490(5) 1_635 ? O21 Cd2 2.210(5) 1_546 ? O22 Cd2 2.208(6) 1_556 ? 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 O10 Cd1 O20 98.2(2) 1_564 1_465 ? O10 Cd1 O11 168.5(2) 1_564 . ? O20 Cd1 O11 91.36(18) 1_465 . ? O10 Cd1 N4 88.1(2) 1_564 . ? O20 Cd1 N4 110.0(2) 1_465 . ? O11 Cd1 N4 94.7(2) . . ? O10 Cd1 O23 83.24(19) 1_564 . ? O20 Cd1 O23 86.30(16) 1_465 . ? O11 Cd1 O23 91.03(19) . . ? N4 Cd1 O23 162.5(2) . . ? O10 Cd1 O12 113.42(19) 1_564 . ? O20 Cd1 O12 140.56(16) 1_465 . ? O11 Cd1 O12 55.30(17) . . ? N4 Cd1 O12 94.6(2) . . ? O23 Cd1 O12 75.17(17) . . ? O10 Cd1 C36 140.7(2) 1_564 . ? O20 Cd1 C36 116.2(2) 1_465 . ? O11 Cd1 C36 27.9(2) . . ? N4 Cd1 C36 96.9(2) . . ? O23 Cd1 C36 80.69(19) . . ? O12 Cd1 C36 27.51(18) . . ? O10 Cd1 Cd2 79.12(16) 1_564 . ? O20 Cd1 Cd2 129.36(12) 1_465 . ? O11 Cd1 Cd2 89.90(13) . . ? N4 Cd1 Cd2 120.32(18) . . ? O23 Cd1 Cd2 43.06(11) . . ? O12 Cd1 Cd2 43.40(12) . . ? C36 Cd1 Cd2 64.75(15) . . ? O17 Cd2 O21 175.1(3) . 1_564 ? O17 Cd2 O22 90.2(2) . 1_554 ? O21 Cd2 O22 94.4(3) 1_564 1_554 ? O17 Cd2 O14 91.4(2) . 1_565 ? O21 Cd2 O14 90.4(2) 1_564 1_565 ? O22 Cd2 O14 91.0(3) 1_554 1_565 ? O17 Cd2 O23 90.23(19) . . ? O21 Cd2 O23 87.47(19) 1_564 . ? O22 Cd2 O23 95.9(3) 1_554 . ? O14 Cd2 O23 172.83(18) 1_565 . ? O17 Cd2 O12 89.1(2) . . ? O21 Cd2 O12 86.1(2) 1_564 . ? O22 Cd2 O12 172.0(2) 1_554 . ? O14 Cd2 O12 96.97(17) 1_565 . ? O23 Cd2 O12 76.06(17) . . ? O17 Cd2 Cd1 113.12(15) . . ? O21 Cd2 Cd1 62.40(18) 1_564 . ? O22 Cd2 Cd1 129.5(2) 1_554 . ? O14 Cd2 Cd1 129.95(13) 1_565 . ? O23 Cd2 Cd1 43.33(12) . . ? O12 Cd2 Cd1 44.23(11) . . ? O19 Cd3 O8 99.4(3) 1_464 1_574 ? O19 Cd3 O14 110.3(3) 1_464 1_475 ? O8 Cd3 O14 97.5(2) 1_574 1_475 ? O19 Cd3 N5 90.2(3) 1_464 . ? O8 Cd3 N5 156.5(2) 1_574 . ? O14 Cd3 N5 99.1(2) 1_475 . ? O19 Cd3 O9 102.5(3) 1_464 1_574 ? O8 Cd3 O9 55.4(2) 1_574 1_574 ? O14 Cd3 O9 140.78(19) 1_475 1_574 ? N5 Cd3 O9 101.7(2) . 1_574 ? O19 Cd3 O20 162.1(2) 1_464 1_475 ? O8 Cd3 O20 91.2(2) 1_574 1_475 ? O14 Cd3 O20 53.61(14) 1_475 1_475 ? N5 Cd3 O20 85.48(19) . 1_475 ? O9 Cd3 O20 95.37(17) 1_574 1_475 ? O19 Cd3 C32 101.6(3) 1_464 1_574 ? O8 Cd3 C32 27.5(2) 1_574 1_574 ? O14 Cd3 C32 121.1(2) 1_475 1_574 ? N5 Cd3 C32 129.6(2) . 1_574 ? O9 Cd3 C32 27.9(2) 1_574 1_574 ? O20 Cd3 C32 94.5(2) 1_475 1_574 ? C23 N1 C22 117.2(7) . . ? C22 N2 C21 115.8(7) . . ? C21 N3 C23 116.6(7) . . ? C64 N5 C46 117.7(7) . . ? C64 N5 Cd3 118.2(6) . . ? C46 N5 Cd3 123.8(5) . . ? C65 N6 C55 116.9(11) . . ? C48 N4 C66 114.5(7) . . ? C48 N4 Cd1 125.2(5) . . ? C66 N4 Cd1 120.0(6) . . ? C5 C1 C3 109.8(6) . . ? C5 C1 C4 111.3(6) . . ? C3 C1 C4 110.5(6) . . ? C5 C1 C2 109.8(6) . . ? C3 C1 C2 110.4(6) . . ? C4 C1 C2 105.0(6) . . ? O2 C2 C1 106.6(6) . . ? O1 C3 C1 109.1(6) . . ? O3 C4 C1 108.0(6) . . ? O7 C5 C1 109.0(6) . . ? O1 C6 C7 106.8(6) . . ? C11 C7 C8 112.1(6) . . ? C11 C7 C10 106.4(6) . . ? C8 C7 C10 110.5(6) . . ? C11 C7 C6 112.2(6) . . ? C8 C7 C6 106.9(6) . . ? C10 C7 C6 108.8(6) . . ? O5 C8 C7 107.4(6) . . ? O6 C10 C7 105.3(6) . . ? O4 C11 C7 106.3(5) . . ? O4 C12 C38 124.9(6) . . ? O4 C12 C13 115.3(7) . . ? C38 C12 C13 119.7(6) . . ? C72 C13 C12 120.4(7) . . ? C60 C14 C59 119.3(9) . . ? C16 C15 O6 125.8(7) . . ? C16 C15 C58 119.9(7) . . ? O6 C15 C58 114.3(8) . . ? C15 C16 C17 120.9(7) . . ? C16 C17 C40 119.0(8) . . ? C67 C18 C70 117.9(9) . . ? C67 C18 O2 124.5(8) . . ? C70 C18 O2 117.5(8) . . ? C62 C19 C20 118.6(8) . . ? C62 C19 O3 117.8(8) . . ? C20 C19 O3 123.6(7) . . ? C19 C20 C63 118.9(8) . . ? N3 C21 N2 122.9(7) . . ? N3 C21 C31 118.8(7) . . ? N2 C21 C31 118.3(6) . . ? N2 C22 N1 123.9(8) . . ? N2 C22 C27 118.0(7) . . ? N1 C22 C27 118.0(7) . . ? N1 C23 N3 123.5(7) . . ? N1 C23 C24 119.0(7) . . ? N3 C23 C24 117.5(7) . . ? C25 C24 C26 116.7(7) . . ? C25 C24 C23 121.2(7) . . ? C26 C24 C23 122.1(8) . . ? C24 C25 C64 118.9(8) . . ? C46 C26 C24 121.1(8) . . ? C29 C27 C28 117.5(9) . . ? C29 C27 C22 121.9(9) . . ? C28 C27 C22 120.6(8) . . ? C55 C28 C27 118.4(11) . . ? C65 C29 C27 118.2(12) . . ? C66 C30 C31 122.9(8) . . ? C30 C31 C47 114.1(8) . . ? C30 C31 C21 121.1(7) . . ? C47 C31 C21 124.7(8) . . ? O8 C32 O9 120.0(7) . . ? O8 C32 C33 119.4(7) . . ? O9 C32 C33 120.6(8) . . ? O8 C32 Cd3 58.2(4) . 1_536 ? O9 C32 Cd3 61.8(4) . 1_536 ? C33 C32 Cd3 176.5(6) . 1_536 ? C63 C33 C52 117.4(8) . . ? C63 C33 C32 122.1(8) . . ? C52 C33 C32 120.4(8) . . ? O20 C34 O14 118.4(6) . . ? O20 C34 C35 120.7(6) . . ? O14 C34 C35 120.9(6) . . ? C43 C35 C41 117.7(7) . . ? C43 C35 C34 121.4(6) . . ? C41 C35 C34 120.9(7) . . ? O12 C36 O11 121.5(6) . . ? O12 C36 C37 120.3(6) . . ? O11 C36 C37 118.2(6) . . ? O12 C36 Cd1 63.4(4) . . ? O11 C36 Cd1 58.4(3) . . ? C37 C36 Cd1 172.0(5) . . ? C39 C37 C72 119.0(6) . . ? C39 C37 C36 121.0(6) . . ? C72 C37 C36 119.9(6) . . ? C12 C38 C39 120.8(7) . . ? C38 C39 C37 120.3(7) . . ? C57 C40 C17 120.4(7) . . ? C57 C40 C45 119.5(7) . . ? C17 C40 C45 120.0(8) . . ? C44 C41 C35 120.4(7) . . ? O18 C42 O17 124.9(7) . . ? O18 C42 C51 118.6(7) . . ? O17 C42 C51 116.5(7) . . ? C35 C43 C50 120.7(7) . . ? C49 C44 C41 119.9(7) . . ? O21 C45 O10 127.4(7) . . ? O21 C45 C40 116.2(8) . . ? O10 C45 C40 116.4(7) . . ? N5 C46 C26 121.5(7) . . ? C48 C47 C31 120.9(8) . . ? N4 C48 C47 124.1(7) . . ? C44 C49 C50 120.5(7) . . ? C44 C49 O7 116.2(7) . . ? C50 C49 O7 123.3(8) . . ? C49 C50 C43 120.6(7) . . ? C69 C51 C68 114.6(9) . . ? C69 C51 C42 123.7(8) . . ? C68 C51 C42 120.4(8) . . ? C33 C52 C62 118.7(9) . . ? O19 C53 O22 128.4(9) . . ? O19 C53 C61 116.5(9) . . ? O22 C53 C61 115.1(10) . . ? N6 C55 C28 122.0(12) . . ? C40 C57 C58 119.7(9) . . ? C15 C58 C57 119.7(9) . . ? C73 C59 O5 125.9(8) . . ? C73 C59 C14 118.6(8) . . ? O5 C59 C14 115.2(8) . . ? C61 C60 C14 121.7(9) . . ? C60 C61 C71 120.0(8) . . ? C60 C61 C53 122.8(9) . . ? C71 C61 C53 117.2(9) . . ? C19 C62 C52 122.8(10) . . ? C33 C63 C20 123.4(9) . . ? N5 C64 C25 123.8(9) . . ? N6 C65 C29 127.0(13) . . ? C30 C66 N4 123.1(9) . . ? C18 C67 C68 119.5(9) . . ? C51 C68 C67 123.5(11) . . ? C51 C69 C70 122.0(10) . . ? C18 C70 C69 120.5(10) . . ? C61 C71 C73 119.9(10) . . ? C13 C72 C37 119.6(7) . . ? C59 C73 C71 120.2(10) . . ? C3 O1 C6 114.3(6) . . ? Cd2 O23 Cd1 93.62(17) . . ? C18 O2 C2 116.9(6) . . ? C19 O3 C4 117.9(6) . . ? C12 O4 C11 117.5(5) . . ? C59 O5 C8 117.3(7) . . ? C15 O6 C10 119.5(7) . . ? C49 O7 C5 118.6(6) . . ? C32 O8 Cd3 94.3(5) . 1_536 ? C32 O9 Cd3 90.3(5) . 1_536 ? C45 O10 Cd1 114.4(5) . 1_546 ? C36 O11 Cd1 93.7(4) . . ? C36 O12 Cd2 133.3(5) . . ? C36 O12 Cd1 89.1(4) . . ? Cd2 O12 Cd1 92.37(16) . . ? C34 O14 Cd2 152.6(4) . 1_545 ? C34 O14 Cd3 98.0(4) . 1_635 ? Cd2 O14 Cd3 108.8(2) 1_545 1_635 ? C42 O17 Cd2 124.2(5) . . ? C53 O19 Cd3 118.4(7) . 1_646 ? C34 O20 Cd1 144.4(4) . 1_645 ? C34 O20 Cd3 89.9(4) . 1_635 ? Cd1 O20 Cd3 124.2(2) 1_645 1_635 ? C45 O21 Cd2 136.5(5) . 1_546 ? C53 O22 Cd2 133.8(6) . 1_556 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.361 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.179 # Attachment '- 4.CIF' data_4 _database_code_depnum_ccdc_archive 'CCDC 865800' #TrackingRef '- 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H60 Co3 N7 O21' _chemical_formula_weight 1536.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.061(8) _cell_length_b 28.353(16) _cell_length_c 17.069(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.653(9) _cell_angle_gamma 90.00 _cell_volume 7163(7) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description brick _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 0.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6491 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32577 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.1467 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 26.22 _reflns_number_total 21144 _reflns_number_gt 12535 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1968P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 21144 _refine_ls_number_parameters 913 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1554 _refine_ls_R_factor_gt 0.1035 _refine_ls_wR_factor_ref 0.3260 _refine_ls_wR_factor_gt 0.2847 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.049 _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 Co1 Co 0.47826(8) -0.02995(4) 1.13205(6) 0.0309(3) Uani 1 1 d . . . Co2 Co 0.48635(8) 0.06915(4) 1.24076(6) 0.0273(3) Uani 1 1 d . . . Co3 Co 0.48533(8) -0.03295(4) 1.34659(6) 0.0299(3) Uani 1 1 d . . . N1 N 0.5195(7) 0.3861(3) 1.2609(4) 0.053(2) Uani 1 1 d . . . N2 N 0.5122(7) 0.3142(3) 1.3264(5) 0.055(2) Uani 1 1 d . . . N3 N 0.5144(7) 0.3145(3) 1.1885(5) 0.058(3) Uani 1 1 d . . . N4 N 0.5309(6) 0.4339(3) 0.9793(4) 0.044(2) Uani 1 1 d . . . N5 N 0.5157(6) 0.4312(3) 1.5422(4) 0.041(2) Uani 1 1 d . . . N6 N 0.4911(6) 0.1442(3) 1.2464(4) 0.041(2) Uani 1 1 d . . . C1 C 0.0589(6) 0.1602(4) 0.7129(6) 0.042(2) Uani 1 1 d . . . H1A H 0.0507 0.1266 0.7192 0.051 Uiso 1 1 calc R . . H1B H 0.1167 0.1692 0.7446 0.051 Uiso 1 1 calc R . . C2 C -0.0790(7) 0.1570(4) 0.7647(6) 0.050(3) Uani 1 1 d . . . H2A H -0.0628 0.1240 0.7625 0.060 Uiso 1 1 calc R . . H2B H -0.1369 0.1617 0.7298 0.060 Uiso 1 1 calc R . . C3 C 0.0565(6) 0.1721(3) 0.6247(6) 0.039(2) Uani 1 1 d . . . C4 C -0.0864(6) 0.1700(3) 0.8490(5) 0.036(2) Uani 1 1 d . . . C5 C -0.0329(7) 0.1638(4) 0.5746(7) 0.052(3) Uani 1 1 d . . . H5A H -0.0759 0.1867 0.5871 0.063 Uiso 1 1 calc R . . H5B H -0.0290 0.1671 0.5188 0.063 Uiso 1 1 calc R . . C6 C 0.1274(7) 0.1385(4) 0.5983(6) 0.052(3) Uani 1 1 d . . . H6A H 0.1854 0.1421 0.6335 0.062 Uiso 1 1 calc R . . H6B H 0.1082 0.1060 0.6007 0.062 Uiso 1 1 calc R . . C7 C 0.0793(7) 0.2228(4) 0.6124(6) 0.046(2) Uani 1 1 d . . . H7A H 0.0742 0.2293 0.5559 0.055 Uiso 1 1 calc R . . H7B H 0.0378 0.2433 0.6333 0.055 Uiso 1 1 calc R . . C8 C -0.1133(7) 0.2197(4) 0.8551(6) 0.043(2) Uani 1 1 d . . . H8A H -0.1200 0.2269 0.9093 0.051 Uiso 1 1 calc R . . H8B H -0.0676 0.2405 0.8408 0.051 Uiso 1 1 calc R . . C9 C -0.1525(8) 0.1360(4) 0.8744(6) 0.055(3) Uani 1 1 d . . . H9A H -0.2100 0.1375 0.8379 0.066 Uiso 1 1 calc R . . H9B H -0.1296 0.1040 0.8745 0.066 Uiso 1 1 calc R . . C10 C 0.0026(7) 0.1638(4) 0.9020(6) 0.047(2) Uani 1 1 d . . . H10A H 0.0453 0.1865 0.8883 0.056 Uiso 1 1 calc R . . H10B H -0.0032 0.1691 0.9570 0.056 Uiso 1 1 calc R . . C11 C -0.1410(8) 0.1024(4) 0.5421(7) 0.055(3) Uani 1 1 d . . . C12 C -0.1714(9) 0.0596(4) 0.5614(8) 0.073(4) Uani 1 1 d . . . H12A H -0.1402 0.0428 0.6046 0.088 Uiso 1 1 calc R . . C13 C -0.2496(9) 0.0415(4) 0.5155(8) 0.073(4) Uani 1 1 d . . . H13A H -0.2692 0.0118 0.5281 0.088 Uiso 1 1 calc R . . C14 C -0.2992(7) 0.0653(4) 0.4525(6) 0.045(2) Uani 1 1 d . . . C15 C -0.2671(9) 0.1085(4) 0.4370(8) 0.080(4) Uani 1 1 d . . . H15A H -0.2991 0.1262 0.3953 0.096 Uiso 1 1 calc R . . C16 C -0.1880(9) 0.1273(5) 0.4815(8) 0.081(5) Uani 1 1 d . . . H16A H -0.1678 0.1569 0.4692 0.097 Uiso 1 1 calc R . . C17 C -0.3805(7) 0.0464(3) 0.4028(5) 0.035(2) Uani 1 1 d . . . C18 C 0.1915(9) 0.1238(5) 0.4846(8) 0.069(4) Uani 1 1 d . . . C19 C 0.2357(10) 0.0847(5) 0.5186(8) 0.080(4) Uani 1 1 d . . . H19A H 0.2306 0.0751 0.5696 0.097 Uiso 1 1 calc R . . C20 C 0.2888(8) 0.0597(4) 0.4736(6) 0.056(3) Uani 1 1 d . . . H20A H 0.3161 0.0318 0.4940 0.068 Uiso 1 1 calc R . . C21 C 0.3017(7) 0.0749(4) 0.4010(6) 0.046(2) Uani 1 1 d . . . C22 C 0.2583(8) 0.1148(5) 0.3716(7) 0.068(4) Uani 1 1 d . . . H22A H 0.2668 0.1258 0.3222 0.082 Uiso 1 1 calc R . . C23 C 0.2017(9) 0.1398(5) 0.4123(7) 0.075(4) Uani 1 1 d . . . H23A H 0.1717 0.1668 0.3903 0.090 Uiso 1 1 calc R . . C24 C 0.3624(7) 0.0503(3) 0.3562(5) 0.039(2) Uani 1 1 d . . . C25 C 0.2046(8) 0.2748(4) 0.6411(8) 0.062(3) Uani 1 1 d . . . C26 C 0.1597(9) 0.3095(5) 0.5979(10) 0.092(5) Uani 1 1 d . . . H26A H 0.1007 0.3049 0.5712 0.111 Uiso 1 1 calc R . . C27 C 0.2016(9) 0.3517(5) 0.5934(8) 0.075(4) Uani 1 1 d . . . H27A H 0.1695 0.3762 0.5648 0.089 Uiso 1 1 calc R . . C28 C 0.2888(8) 0.3593(4) 0.6292(7) 0.053(3) Uani 1 1 d . . . C29 C 0.3319(8) 0.3227(5) 0.6760(9) 0.073(4) Uani 1 1 d . . . H29A H 0.3904 0.3268 0.7041 0.087 Uiso 1 1 calc R . . C30 C 0.2897(9) 0.2825(5) 0.6802(10) 0.083(5) Uani 1 1 d . . . H30A H 0.3197 0.2585 0.7115 0.100 Uiso 1 1 calc R . . C31 C 0.3361(9) 0.4047(4) 0.6262(7) 0.055(3) Uani 1 1 d . . . C32 C -0.2372(8) 0.2700(4) 0.7970(7) 0.060(3) Uani 1 1 d . . . C33 C -0.234(2) 0.2999(9) 0.8615(11) 0.232(18) Uani 1 1 d . . . H33A H -0.1999 0.2919 0.9110 0.278 Uiso 1 1 calc R . . C34 C -0.2811(14) 0.3412(6) 0.8514(9) 0.125(8) Uani 1 1 d . . . H34A H -0.2797 0.3609 0.8952 0.150 Uiso 1 1 calc R . . C35 C -0.3289(7) 0.3545(4) 0.7818(6) 0.051(3) Uani 1 1 d . . . C36 C -0.3237(15) 0.3282(6) 0.7226(9) 0.142(9) Uani 1 1 d . . . H36A H -0.3438 0.3403 0.6717 0.170 Uiso 1 1 calc R . . C37 C -0.2885(15) 0.2807(8) 0.7295(10) 0.165(11) Uani 1 1 d . . . H37A H -0.3018 0.2591 0.6881 0.198 Uiso 1 1 calc R . . C38 C -0.3800(6) 0.4005(3) 0.7738(5) 0.034(2) Uani 1 1 d . . . C39 C -0.2189(8) 0.1224(5) 0.9888(7) 0.060(3) Uani 1 1 d . . . C40 C -0.2268(9) 0.1391(5) 1.0646(7) 0.078(4) Uani 1 1 d . . . H40A H -0.1921 0.1644 1.0875 0.094 Uiso 1 1 calc R . . C41 C -0.2863(9) 0.1174(5) 1.1041(7) 0.073(4) Uani 1 1 d . . . H41A H -0.2971 0.1303 1.1515 0.088 Uiso 1 1 calc R . . C42 C -0.3315(6) 0.0760(4) 1.0745(6) 0.046(3) Uani 1 1 d . . . C43 C -0.3216(9) 0.0608(4) 1.0011(7) 0.067(4) Uani 1 1 d . . . H43A H -0.3518 0.0336 0.9804 0.080 Uiso 1 1 calc R . . C44 C -0.2680(8) 0.0844(4) 0.9564(7) 0.060(3) Uani 1 1 d . . . H44A H -0.2654 0.0744 0.9049 0.072 Uiso 1 1 calc R . . C45 C -0.3959(7) 0.0533(3) 1.1199(6) 0.041(2) Uani 1 1 d . . . C46 C 0.1152(7) 0.1032(4) 0.9447(6) 0.048(3) Uani 1 1 d . . . C47 C 0.1364(9) 0.0588(5) 0.9357(9) 0.082(5) Uani 1 1 d . . . H47A H 0.0992 0.0395 0.8996 0.098 Uiso 1 1 calc R . . C48 C 0.2168(9) 0.0410(4) 0.9821(8) 0.079(5) Uani 1 1 d . . . H48A H 0.2341 0.0100 0.9758 0.095 Uiso 1 1 calc R . . C49 C 0.2686(6) 0.0695(4) 1.0360(5) 0.041(2) Uani 1 1 d . . . C50 C 0.2438(8) 0.1150(4) 1.0415(7) 0.057(3) Uani 1 1 d . . . H50A H 0.2803 0.1349 1.0771 0.068 Uiso 1 1 calc R . . C51 C 0.1668(8) 0.1324(4) 0.9965(8) 0.067(4) Uani 1 1 d . . . H51A H 0.1502 0.1637 1.0012 0.080 Uiso 1 1 calc R . . C52 C 0.3513(7) 0.0504(4) 1.0893(6) 0.039(2) Uani 1 1 d . . . C53 C 0.5182(9) 0.3614(3) 1.1934(5) 0.056(3) Uani 1 1 d . . . C54 C 0.5154(9) 0.3598(3) 1.3248(5) 0.051(3) Uani 1 1 d . . . C55 C 0.5092(8) 0.2932(4) 1.2558(5) 0.048(3) Uani 1 1 d . . . C56 C 0.5226(10) 0.3872(4) 1.1195(6) 0.063(3) Uani 1 1 d . . . C57 C 0.5229(10) 0.4356(4) 1.1154(6) 0.073(4) Uani 1 1 d . . . H57A H 0.5187 0.4533 1.1604 0.087 Uiso 1 1 calc R . . C58 C 0.5290(10) 0.4573(4) 1.0472(6) 0.067(4) Uani 1 1 d . . . H58A H 0.5322 0.4900 1.0467 0.081 Uiso 1 1 calc R . . C59 C 0.5301(11) 0.3882(4) 0.9820(7) 0.083(5) Uani 1 1 d . . . H59A H 0.5336 0.3712 0.9361 0.099 Uiso 1 1 calc R . . C60 C 0.5241(13) 0.3644(4) 1.0500(6) 0.092(5) Uani 1 1 d . . . H60A H 0.5211 0.3316 1.0487 0.111 Uiso 1 1 calc R . . C61 C 0.5154(8) 0.3851(3) 1.4000(5) 0.049(3) Uani 1 1 d . . . C62 C 0.5162(8) 0.4335(3) 1.4042(5) 0.050(3) Uani 1 1 d . . . H62A H 0.5166 0.4515 1.3587 0.061 Uiso 1 1 calc R . . C63 C 0.5164(8) 0.4548(3) 1.4762(5) 0.050(3) Uani 1 1 d . . . H63A H 0.5170 0.4876 1.4784 0.060 Uiso 1 1 calc R . . C64 C 0.5159(9) 0.3849(4) 1.5377(6) 0.053(3) Uani 1 1 d . . . H64A H 0.5159 0.3679 1.5843 0.064 Uiso 1 1 calc R . . C65 C 0.5162(8) 0.3597(3) 1.4678(5) 0.053(3) Uani 1 1 d . . . H65A H 0.5168 0.3269 1.4675 0.064 Uiso 1 1 calc R . . C66 C 0.5034(8) 0.2418(4) 1.2527(5) 0.047(3) Uani 1 1 d . . . C67 C 0.5021(10) 0.2178(3) 1.1825(6) 0.065(4) Uani 1 1 d . . . H67A H 0.5059 0.2343 1.1362 0.078 Uiso 1 1 calc R . . C68 C 0.4952(9) 0.1694(3) 1.1809(6) 0.058(3) Uani 1 1 d . . . H68A H 0.4934 0.1537 1.1328 0.070 Uiso 1 1 calc R . . C69 C 0.4916(9) 0.1678(3) 1.3137(6) 0.055(3) Uani 1 1 d . . . H69A H 0.4890 0.1508 1.3598 0.066 Uiso 1 1 calc R . . C70 C 0.4957(9) 0.2155(3) 1.3184(5) 0.055(3) Uani 1 1 d . . . H70A H 0.4933 0.2305 1.3665 0.066 Uiso 1 1 calc R . . O1 O -0.0120(5) 0.1855(3) 0.7381(4) 0.056(2) Uani 1 1 d . . . O1W O 0.5957(7) -0.0760(4) 1.1722(5) 0.098(4) Uani 1 1 d . . . O2 O -0.0622(5) 0.1170(3) 0.5896(5) 0.060(2) Uani 1 1 d . . . O3 O 0.1348(6) 0.1501(3) 0.5209(5) 0.074(3) Uani 1 1 d . . . O4 O 0.1690(5) 0.2312(3) 0.6525(5) 0.065(2) Uani 1 1 d . . . O5 O -0.1983(6) 0.2266(3) 0.8010(5) 0.075(3) Uani 1 1 d . . . O6 O -0.1634(6) 0.1488(3) 0.9511(5) 0.076(3) Uani 1 1 d . . . O7 O 0.0345(5) 0.1179(3) 0.8936(5) 0.065(2) Uani 1 1 d . . . O8 O -0.4262(5) 0.0735(2) 0.3535(4) 0.0461(17) Uani 1 1 d . . . O9 O -0.4015(4) 0.0040(2) 0.4111(4) 0.0380(15) Uani 1 1 d . . . O10 O 0.3951(5) 0.0118(2) 0.3820(4) 0.0436(17) Uani 1 1 d . . . O11 O 0.3764(4) 0.0691(3) 0.2944(4) 0.0472(16) Uani 1 1 d . . . O12 O 0.2955(6) 0.4332(3) 0.5685(5) 0.078(3) Uani 1 1 d . . . O13 O 0.4078(5) 0.4135(2) 0.6685(4) 0.0470(17) Uani 1 1 d . . . O14 O -0.3981(5) 0.4173(3) 0.7071(4) 0.053(2) Uani 1 1 d . . . O15 O -0.4004(6) 0.4167(3) 0.8353(4) 0.064(2) Uani 1 1 d . . . O16 O -0.4339(5) 0.0171(3) 1.0912(4) 0.0481(18) Uani 1 1 d . . . O17 O -0.4040(4) 0.0729(3) 1.1836(4) 0.0474(17) Uani 1 1 d . . . O18 O 0.4005(5) 0.0785(2) 1.1347(4) 0.0444(17) Uani 1 1 d . . . O19 O 0.3656(5) 0.0063(2) 1.0842(4) 0.0482(18) Uani 1 1 d . . . O20 O 0.5077(4) -0.0027(2) 1.2443(3) 0.0291(14) Uani 1 1 d . . . N7 N 0.570(3) 0.2068(18) 1.553(3) 0.37(2) Uiso 1 1 d . . . C71 C 0.529(3) 0.2485(15) 1.546(2) 0.251(18) Uiso 1 1 d . . . C72 C 0.366(8) 0.084(5) 1.611(7) 0.77(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0467(8) 0.0245(6) 0.0225(5) -0.0024(6) 0.0095(5) -0.0003(7) Co2 0.0404(7) 0.0198(6) 0.0232(6) -0.0005(6) 0.0096(5) 0.0012(6) Co3 0.0445(7) 0.0227(6) 0.0235(5) 0.0008(6) 0.0088(5) -0.0014(7) N1 0.111(8) 0.024(4) 0.028(4) 0.000(3) 0.025(4) -0.001(4) N2 0.118(8) 0.022(4) 0.028(4) 0.000(3) 0.021(5) -0.006(5) N3 0.116(8) 0.025(4) 0.037(5) 0.006(3) 0.025(5) 0.000(5) N4 0.087(7) 0.020(4) 0.029(4) 0.003(3) 0.017(4) 0.002(4) N5 0.063(6) 0.032(4) 0.028(4) 0.003(3) 0.010(4) 0.004(4) N6 0.080(6) 0.019(4) 0.027(4) 0.000(3) 0.017(4) -0.004(4) C1 0.033(5) 0.050(6) 0.049(6) -0.009(5) 0.022(4) -0.009(5) C2 0.056(7) 0.041(6) 0.058(6) 0.008(5) 0.025(5) 0.005(5) C3 0.030(5) 0.042(5) 0.048(5) -0.013(4) 0.018(4) -0.008(4) C4 0.033(5) 0.045(6) 0.035(5) 0.004(4) 0.018(4) 0.004(4) C5 0.057(7) 0.039(6) 0.064(7) -0.003(5) 0.021(6) -0.010(5) C6 0.046(6) 0.055(7) 0.062(7) -0.009(5) 0.029(5) 0.005(5) C7 0.036(6) 0.043(6) 0.061(6) -0.006(5) 0.014(5) -0.011(5) C8 0.043(6) 0.044(6) 0.045(5) 0.004(4) 0.020(5) 0.011(5) C9 0.061(7) 0.063(7) 0.048(6) -0.009(5) 0.031(5) -0.024(6) C10 0.042(6) 0.040(6) 0.057(6) 0.009(5) 0.004(5) 0.012(5) C11 0.055(7) 0.039(6) 0.062(7) -0.006(5) -0.009(5) -0.022(5) C12 0.088(10) 0.052(8) 0.067(8) 0.012(6) -0.021(7) -0.025(7) C13 0.083(9) 0.052(7) 0.071(8) 0.026(6) -0.024(7) -0.031(7) C14 0.055(6) 0.035(5) 0.040(5) 0.002(4) -0.003(4) 0.004(5) C15 0.092(10) 0.042(7) 0.086(9) 0.017(7) -0.036(8) -0.009(7) C16 0.087(10) 0.051(8) 0.086(9) 0.031(7) -0.034(8) -0.029(7) C17 0.052(6) 0.020(4) 0.032(5) 0.000(3) 0.009(4) -0.002(4) C18 0.093(10) 0.058(8) 0.068(8) -0.001(6) 0.046(7) 0.026(7) C19 0.113(11) 0.083(10) 0.063(8) 0.012(7) 0.060(8) 0.026(9) C20 0.069(7) 0.058(7) 0.047(6) 0.008(5) 0.023(5) 0.022(6) C21 0.059(6) 0.040(6) 0.050(6) 0.006(5) 0.035(5) 0.007(5) C22 0.085(9) 0.086(10) 0.046(6) 0.011(6) 0.044(6) 0.019(8) C23 0.097(10) 0.088(10) 0.047(7) 0.015(6) 0.034(7) 0.035(8) C24 0.057(7) 0.034(5) 0.030(5) 0.004(4) 0.019(4) 0.002(5) C25 0.054(8) 0.047(7) 0.079(8) 0.012(6) 0.000(6) -0.012(6) C26 0.057(8) 0.075(10) 0.128(13) 0.041(9) -0.025(8) -0.039(8) C27 0.074(9) 0.053(8) 0.087(9) 0.012(7) -0.010(7) -0.020(7) C28 0.054(7) 0.045(6) 0.057(7) 0.000(5) 0.001(5) -0.012(5) C29 0.054(8) 0.057(8) 0.099(10) 0.017(7) -0.006(7) -0.029(6) C30 0.052(8) 0.059(8) 0.126(13) 0.038(8) -0.013(8) -0.011(7) C31 0.071(9) 0.047(7) 0.050(6) -0.003(5) 0.016(6) -0.009(6) C32 0.063(8) 0.049(7) 0.063(7) -0.003(5) -0.003(6) 0.038(6) C33 0.43(4) 0.19(2) 0.061(11) 0.028(13) 0.014(18) 0.24(3) C34 0.20(2) 0.103(13) 0.060(9) -0.016(8) 0.000(11) 0.096(14) C35 0.060(7) 0.057(7) 0.035(5) 0.001(5) 0.006(5) 0.026(6) C36 0.24(2) 0.105(13) 0.067(10) -0.017(9) -0.021(12) 0.126(15) C37 0.23(2) 0.166(19) 0.064(10) -0.042(11) -0.052(13) 0.132(19) C38 0.042(6) 0.033(5) 0.030(5) 0.002(4) 0.009(4) 0.010(4) C39 0.065(8) 0.073(8) 0.051(6) 0.001(6) 0.031(6) -0.018(7) C40 0.097(10) 0.088(10) 0.061(7) -0.021(7) 0.043(7) -0.054(8) C41 0.102(10) 0.077(9) 0.051(7) -0.028(6) 0.041(7) -0.044(8) C42 0.046(6) 0.058(7) 0.041(5) -0.003(5) 0.023(4) -0.017(5) C43 0.095(9) 0.061(8) 0.058(7) -0.026(6) 0.050(7) -0.042(7) C44 0.074(8) 0.067(8) 0.049(6) -0.011(5) 0.037(6) -0.024(6) C45 0.055(7) 0.035(5) 0.036(5) -0.001(4) 0.018(5) -0.009(5) C46 0.033(6) 0.055(7) 0.054(6) 0.007(5) -0.002(5) 0.016(5) C47 0.068(9) 0.053(8) 0.104(11) -0.024(7) -0.038(7) 0.019(7) C48 0.082(10) 0.043(7) 0.091(10) -0.017(6) -0.041(8) 0.026(7) C49 0.039(5) 0.039(5) 0.042(5) -0.001(5) -0.002(4) 0.014(5) C50 0.048(7) 0.045(7) 0.072(8) -0.009(6) -0.003(6) 0.006(5) C51 0.065(8) 0.040(7) 0.083(9) -0.009(6) -0.021(7) 0.023(6) C52 0.037(6) 0.042(6) 0.037(5) 0.007(4) 0.003(4) 0.008(5) C53 0.121(10) 0.025(5) 0.025(5) 0.000(4) 0.019(5) 0.000(6) C54 0.109(9) 0.023(5) 0.022(4) -0.002(4) 0.012(5) 0.002(5) C55 0.098(9) 0.021(5) 0.026(5) 0.001(3) 0.015(5) -0.003(5) C56 0.132(11) 0.027(5) 0.033(5) 0.002(4) 0.019(6) -0.004(6) C57 0.172(14) 0.029(6) 0.019(5) -0.003(4) 0.023(6) 0.006(7) C58 0.146(12) 0.024(6) 0.040(6) 0.007(4) 0.038(7) 0.010(6) C59 0.189(16) 0.031(6) 0.037(6) 0.004(5) 0.047(8) 0.007(8) C60 0.213(17) 0.035(6) 0.033(6) 0.000(5) 0.036(8) 0.001(9) C61 0.102(9) 0.030(5) 0.017(4) 0.004(4) 0.017(5) 0.005(5) C62 0.100(9) 0.029(5) 0.025(5) 0.004(4) 0.018(5) -0.006(5) C63 0.103(9) 0.019(5) 0.032(5) 0.000(4) 0.020(5) -0.002(5) C64 0.105(9) 0.031(6) 0.024(5) 0.001(4) 0.016(5) 0.004(6) C65 0.112(9) 0.022(5) 0.031(5) 0.001(4) 0.027(5) 0.001(5) C66 0.099(9) 0.021(5) 0.024(5) -0.003(3) 0.017(5) -0.004(5) C67 0.153(12) 0.023(5) 0.023(5) -0.002(4) 0.028(6) -0.004(6) C68 0.126(10) 0.023(5) 0.025(5) -0.005(4) 0.014(6) -0.009(6) C69 0.128(10) 0.013(4) 0.030(5) -0.001(4) 0.031(6) -0.005(5) C70 0.124(10) 0.026(5) 0.019(4) 0.001(4) 0.022(5) 0.000(6) O1 0.067(5) 0.042(4) 0.075(5) -0.001(4) 0.053(4) -0.006(4) O1W 0.118(8) 0.124(9) 0.051(5) 0.003(5) 0.015(5) 0.075(7) O2 0.050(5) 0.051(5) 0.070(5) 0.006(4) -0.012(4) -0.017(4) O3 0.099(6) 0.080(6) 0.057(5) 0.011(4) 0.056(5) 0.039(5) O4 0.041(5) 0.054(5) 0.098(6) 0.017(5) 0.003(4) -0.018(4) O5 0.082(6) 0.050(5) 0.083(6) -0.012(4) -0.013(5) 0.039(5) O6 0.091(6) 0.092(7) 0.060(5) -0.013(5) 0.050(5) -0.050(5) O7 0.053(5) 0.040(4) 0.090(6) -0.011(4) -0.017(4) 0.018(4) O8 0.066(5) 0.032(4) 0.033(3) -0.003(3) -0.010(3) 0.004(3) O9 0.042(4) 0.027(3) 0.040(4) -0.001(3) -0.008(3) -0.005(3) O10 0.055(4) 0.042(4) 0.041(4) 0.009(3) 0.026(3) 0.011(3) O11 0.061(4) 0.044(4) 0.043(4) 0.009(3) 0.026(3) 0.007(4) O12 0.088(6) 0.053(5) 0.079(6) 0.017(4) -0.023(5) -0.020(5) O13 0.054(5) 0.040(4) 0.044(4) -0.001(3) 0.001(3) -0.021(4) O14 0.079(5) 0.050(4) 0.035(4) 0.014(3) 0.024(4) 0.029(4) O15 0.113(7) 0.035(4) 0.047(4) 0.003(3) 0.021(4) 0.039(4) O16 0.067(5) 0.046(4) 0.037(4) -0.007(3) 0.027(3) -0.020(4) O17 0.054(4) 0.047(4) 0.049(4) -0.013(3) 0.029(3) -0.019(4) O18 0.059(4) 0.037(4) 0.032(3) -0.002(3) -0.006(3) 0.004(3) O19 0.052(5) 0.033(4) 0.051(4) -0.002(3) -0.013(3) 0.009(3) O20 0.045(4) 0.023(3) 0.020(3) 0.002(2) 0.006(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O19 2.023(7) . ? Co1 O20 2.037(5) . ? Co1 O15 2.053(7) 2_547 ? Co1 O16 2.088(7) 1_655 ? Co1 N4 2.141(7) 2_647 ? Co1 O1W 2.204(9) . ? Co2 O11 2.034(6) 1_556 ? Co2 O18 2.038(6) . ? Co2 O20 2.062(6) . ? Co2 O17 2.070(6) 1_655 ? Co2 O8 2.125(6) 1_656 ? Co2 N6 2.131(8) . ? Co3 O20 2.028(5) . ? Co3 O14 2.028(7) 2_547 ? Co3 O10 2.031(6) 1_556 ? Co3 O9 2.126(6) 1_656 ? Co3 N5 2.156(8) 2_648 ? Co3 O13 2.260(7) 2_647 ? N1 C54 1.334(11) . ? N1 C53 1.347(12) . ? N2 C54 1.293(12) . ? N2 C55 1.339(11) . ? N3 C55 1.314(11) . ? N3 C53 1.333(13) . ? N4 C59 1.295(13) . ? N4 C58 1.340(12) . ? N4 Co1 2.141(7) 2_657 ? N5 C63 1.313(11) . ? N5 C64 1.315(12) . ? N5 Co3 2.156(8) 2_658 ? N6 C69 1.328(11) . ? N6 C68 1.338(12) . ? C1 O1 1.419(11) . ? C1 C3 1.536(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O1 1.431(12) . ? C2 C4 1.510(13) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C5 1.475(14) . ? C3 C7 1.501(14) . ? C3 C6 1.559(13) . ? C4 C8 1.475(13) . ? C4 C10 1.483(13) . ? C4 C9 1.507(13) . ? C5 O2 1.436(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O3 1.385(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O4 1.417(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O5 1.446(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O6 1.398(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O7 1.404(12) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.340(16) . ? C11 C12 1.358(16) . ? C11 O2 1.372(12) . ? C12 C13 1.388(16) . ? C12 H12A 0.9300 . ? C13 C14 1.368(14) . ? C13 H13A 0.9300 . ? C14 C15 1.361(16) . ? C14 C17 1.457(14) . ? C15 C16 1.395(17) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 O8 1.248(11) . ? C17 O9 1.259(10) . ? C18 C23 1.351(16) . ? C18 C19 1.365(18) . ? C18 O3 1.366(12) . ? C19 C20 1.400(15) . ? C19 H19A 0.9300 . ? C20 C21 1.359(13) . ? C20 H20A 0.9300 . ? C21 C22 1.355(15) . ? C21 C24 1.471(12) . ? C22 C23 1.390(15) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 O11 1.235(10) . ? C24 O10 1.245(11) . ? C25 C26 1.337(17) . ? C25 C30 1.349(17) . ? C25 O4 1.374(13) . ? C26 C27 1.362(17) . ? C26 H26A 0.9300 . ? C27 C28 1.359(16) . ? C27 H27A 0.9300 . ? C28 C29 1.394(16) . ? C28 C31 1.477(15) . ? C29 C30 1.313(16) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 O13 1.210(13) . ? C31 O12 1.331(14) . ? C32 C37 1.299(18) . ? C32 O5 1.360(12) . ? C32 C33 1.38(2) . ? C33 C34 1.37(2) . ? C33 H33A 0.9300 . ? C34 C35 1.324(18) . ? C34 H34A 0.9300 . ? C35 C36 1.270(17) . ? C35 C38 1.507(13) . ? C36 C37 1.44(2) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C38 O14 1.217(10) . ? C38 O15 1.237(11) . ? C39 C44 1.366(16) . ? C39 O6 1.367(12) . ? C39 C40 1.404(16) . ? C40 C41 1.362(15) . ? C40 H40A 0.9300 . ? C41 C42 1.404(15) . ? C41 H41A 0.9300 . ? C42 C43 1.359(13) . ? C42 C45 1.494(12) . ? C43 C44 1.382(14) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C45 O16 1.230(11) . ? C45 O17 1.248(11) . ? C46 C47 1.315(16) . ? C46 C51 1.347(16) . ? C46 O7 1.421(12) . ? C47 C48 1.411(16) . ? C47 H47A 0.9300 . ? C48 C49 1.358(15) . ? C48 H48A 0.9300 . ? C49 C50 1.350(15) . ? C49 C52 1.503(13) . ? C50 C51 1.360(15) . ? C50 H50A 0.9300 . ? C51 H51A 0.9300 . ? C52 O18 1.254(12) . ? C52 O19 1.272(11) . ? C53 C56 1.471(13) . ? C54 C61 1.469(12) . ? C55 C66 1.459(14) . ? C56 C60 1.355(14) . ? C56 C57 1.374(14) . ? C57 C58 1.335(13) . ? C57 H57A 0.9300 . ? C58 H58A 0.9300 . ? C59 C60 1.359(15) . ? C59 H59A 0.9300 . ? C60 H60A 0.9300 . ? C61 C65 1.362(12) . ? C61 C62 1.375(13) . ? C62 C63 1.369(12) . ? C62 H62A 0.9300 . ? C63 H63A 0.9300 . ? C64 C65 1.390(13) . ? C64 H64A 0.9300 . ? C65 H65A 0.9300 . ? C66 C70 1.369(12) . ? C66 C67 1.374(12) . ? C67 C68 1.377(14) . ? C67 H67A 0.9300 . ? C68 H68A 0.9300 . ? C69 C70 1.356(13) . ? C69 H69A 0.9300 . ? C70 H70A 0.9300 . ? O8 Co2 2.125(6) 1_454 ? O9 Co3 2.126(6) 1_454 ? O10 Co3 2.031(6) 1_554 ? O11 Co2 2.034(6) 1_554 ? O13 Co3 2.260(7) 2_657 ? O14 Co3 2.028(7) 2_557 ? O15 Co1 2.053(7) 2_557 ? O16 Co1 2.088(6) 1_455 ? O17 Co2 2.070(6) 1_455 ? N7 C71 1.33(5) . ? 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 O19 Co1 O20 102.0(3) . . ? O19 Co1 O15 90.3(3) . 2_547 ? O20 Co1 O15 93.4(3) . 2_547 ? O19 Co1 O16 94.3(3) . 1_655 ? O20 Co1 O16 91.8(2) . 1_655 ? O15 Co1 O16 172.2(3) 2_547 1_655 ? O19 Co1 N4 88.5(3) . 2_647 ? O20 Co1 N4 169.5(3) . 2_647 ? O15 Co1 N4 86.6(3) 2_547 2_647 ? O16 Co1 N4 87.2(3) 1_655 2_647 ? O19 Co1 O1W 172.8(3) . . ? O20 Co1 O1W 84.8(3) . . ? O15 Co1 O1W 86.8(4) 2_547 . ? O16 Co1 O1W 87.8(4) 1_655 . ? N4 Co1 O1W 84.7(3) 2_647 . ? O11 Co2 O18 88.0(3) 1_556 . ? O11 Co2 O20 97.0(3) 1_556 . ? O18 Co2 O20 103.0(2) . . ? O11 Co2 O17 176.8(3) 1_556 1_655 ? O18 Co2 O17 90.3(3) . 1_655 ? O20 Co2 O17 86.1(3) . 1_655 ? O11 Co2 O8 90.7(3) 1_556 1_656 ? O18 Co2 O8 169.1(3) . 1_656 ? O20 Co2 O8 87.9(2) . 1_656 ? O17 Co2 O8 90.5(3) 1_655 1_656 ? O11 Co2 N6 90.2(3) 1_556 . ? O18 Co2 N6 85.5(3) . . ? O20 Co2 N6 169.1(3) . . ? O17 Co2 N6 87.0(3) 1_655 . ? O8 Co2 N6 83.7(3) 1_656 . ? O20 Co3 O14 95.8(3) . 2_547 ? O20 Co3 O10 102.6(3) . 1_556 ? O14 Co3 O10 99.0(3) 2_547 1_556 ? O20 Co3 O9 89.6(2) . 1_656 ? O14 Co3 O9 165.3(3) 2_547 1_656 ? O10 Co3 O9 93.1(3) 1_556 1_656 ? O20 Co3 N5 170.6(3) . 2_648 ? O14 Co3 N5 87.7(3) 2_547 2_648 ? O10 Co3 N5 85.3(3) 1_556 2_648 ? O9 Co3 N5 85.0(3) 1_656 2_648 ? O20 Co3 O13 87.2(2) . 2_647 ? O14 Co3 O13 84.1(3) 2_547 2_647 ? O10 Co3 O13 169.3(3) 1_556 2_647 ? O9 Co3 O13 82.6(3) 1_656 2_647 ? N5 Co3 O13 84.6(3) 2_648 2_647 ? C54 N1 C53 114.3(8) . . ? C54 N2 C55 114.9(8) . . ? C55 N3 C53 114.4(8) . . ? C59 N4 C58 117.5(8) . . ? C59 N4 Co1 120.8(7) . 2_657 ? C58 N4 Co1 121.5(6) . 2_657 ? C63 N5 C64 117.3(8) . . ? C63 N5 Co3 121.2(6) . 2_658 ? C64 N5 Co3 121.5(6) . 2_658 ? C69 N6 C68 117.4(8) . . ? C69 N6 Co2 122.5(6) . . ? C68 N6 Co2 120.1(6) . . ? O1 C1 C3 107.6(8) . . ? O1 C1 H1A 110.2 . . ? C3 C1 H1A 110.2 . . ? O1 C1 H1B 110.2 . . ? C3 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? O1 C2 C4 110.1(9) . . ? O1 C2 H2A 109.6 . . ? C4 C2 H2A 109.6 . . ? O1 C2 H2B 109.6 . . ? C4 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C5 C3 C7 106.3(9) . . ? C5 C3 C1 112.7(8) . . ? C7 C3 C1 112.6(8) . . ? C5 C3 C6 109.5(8) . . ? C7 C3 C6 111.0(8) . . ? C1 C3 C6 104.8(8) . . ? C8 C4 C10 107.5(8) . . ? C8 C4 C9 112.7(8) . . ? C10 C4 C9 108.6(9) . . ? C8 C4 C2 111.7(8) . . ? C10 C4 C2 109.6(8) . . ? C9 C4 C2 106.7(8) . . ? O2 C5 C3 108.9(9) . . ? O2 C5 H5A 109.9 . . ? C3 C5 H5A 109.9 . . ? O2 C5 H5B 109.9 . . ? C3 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? O3 C6 C3 108.1(9) . . ? O3 C6 H6A 110.1 . . ? C3 C6 H6A 110.1 . . ? O3 C6 H6B 110.1 . . ? C3 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? O4 C7 C3 108.4(9) . . ? O4 C7 H7A 110.0 . . ? C3 C7 H7A 110.0 . . ? O4 C7 H7B 110.0 . . ? C3 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? O5 C8 C4 107.8(8) . . ? O5 C8 H8A 110.1 . . ? C4 C8 H8A 110.1 . . ? O5 C8 H8B 110.1 . . ? C4 C8 H8B 110.1 . . ? H8A C8 H8B 108.5 . . ? O6 C9 C4 107.5(8) . . ? O6 C9 H9A 110.2 . . ? C4 C9 H9A 110.2 . . ? O6 C9 H9B 110.2 . . ? C4 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? O7 C10 C4 109.7(9) . . ? O7 C10 H10A 109.7 . . ? C4 C10 H10A 109.7 . . ? O7 C10 H10B 109.7 . . ? C4 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C16 C11 C12 120.3(11) . . ? C16 C11 O2 125.0(10) . . ? C12 C11 O2 114.7(11) . . ? C11 C12 C13 118.8(11) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? C14 C13 C12 123.0(11) . . ? C14 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? C15 C14 C13 115.8(10) . . ? C15 C14 C17 120.5(9) . . ? C13 C14 C17 123.7(10) . . ? C14 C15 C16 122.4(11) . . ? C14 C15 H15A 118.8 . . ? C16 C15 H15A 118.8 . . ? C11 C16 C15 119.7(11) . . ? C11 C16 H16A 120.2 . . ? C15 C16 H16A 120.2 . . ? O8 C17 O9 123.1(9) . . ? O8 C17 C14 117.8(8) . . ? O9 C17 C14 119.1(9) . . ? C23 C18 C19 122.2(11) . . ? C23 C18 O3 114.6(11) . . ? C19 C18 O3 123.2(11) . . ? C18 C19 C20 117.5(11) . . ? C18 C19 H19A 121.3 . . ? C20 C19 H19A 121.3 . . ? C21 C20 C19 122.2(11) . . ? C21 C20 H20A 118.9 . . ? C19 C20 H20A 118.9 . . ? C22 C21 C20 117.5(9) . . ? C22 C21 C24 120.4(9) . . ? C20 C21 C24 122.1(9) . . ? C21 C22 C23 122.7(10) . . ? C21 C22 H22A 118.7 . . ? C23 C22 H22A 118.7 . . ? C18 C23 C22 117.9(12) . . ? C18 C23 H23A 121.0 . . ? C22 C23 H23A 121.0 . . ? O11 C24 O10 124.2(9) . . ? O11 C24 C21 117.4(9) . . ? O10 C24 C21 118.4(8) . . ? C26 C25 C30 119.4(11) . . ? C26 C25 O4 124.7(11) . . ? C30 C25 O4 115.9(11) . . ? C25 C26 C27 119.1(12) . . ? C25 C26 H26A 120.5 . . ? C27 C26 H26A 120.5 . . ? C28 C27 C26 122.3(13) . . ? C28 C27 H27A 118.9 . . ? C26 C27 H27A 118.9 . . ? C27 C28 C29 116.6(11) . . ? C27 C28 C31 123.7(11) . . ? C29 C28 C31 119.5(10) . . ? C30 C29 C28 119.9(12) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C25 122.6(12) . . ? C29 C30 H30A 118.7 . . ? C25 C30 H30A 118.7 . . ? O13 C31 O12 123.6(10) . . ? O13 C31 C28 122.8(11) . . ? O12 C31 C28 113.4(10) . . ? C37 C32 O5 115.9(12) . . ? C37 C32 C33 119.4(13) . . ? O5 C32 C33 124.2(11) . . ? C34 C33 C32 118.9(15) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? C35 C34 C33 122.8(15) . . ? C35 C34 H34A 118.6 . . ? C33 C34 H34A 118.6 . . ? C36 C35 C34 116.4(12) . . ? C36 C35 C38 122.7(10) . . ? C34 C35 C38 120.7(10) . . ? C35 C36 C37 123.9(14) . . ? C35 C36 H36A 118.1 . . ? C37 C36 H36A 118.1 . . ? C32 C37 C36 116.2(15) . . ? C32 C37 H37A 121.9 . . ? C36 C37 H37A 121.9 . . ? O14 C38 O15 126.9(9) . . ? O14 C38 C35 116.5(8) . . ? O15 C38 C35 116.6(8) . . ? C44 C39 O6 125.1(10) . . ? C44 C39 C40 120.5(10) . . ? O6 C39 C40 114.4(11) . . ? C41 C40 C39 118.7(11) . . ? C41 C40 H40A 120.6 . . ? C39 C40 H40A 120.6 . . ? C40 C41 C42 121.2(10) . . ? C40 C41 H41A 119.4 . . ? C42 C41 H41A 119.4 . . ? C43 C42 C41 117.9(9) . . ? C43 C42 C45 122.3(9) . . ? C41 C42 C45 119.5(9) . . ? C42 C43 C44 122.1(10) . . ? C42 C43 H43A 118.9 . . ? C44 C43 H43A 118.9 . . ? C39 C44 C43 119.1(10) . . ? C39 C44 H44A 120.5 . . ? C43 C44 H44A 120.5 . . ? O16 C45 O17 127.2(9) . . ? O16 C45 C42 116.9(8) . . ? O17 C45 C42 115.9(9) . . ? C47 C46 C51 122.7(10) . . ? C47 C46 O7 114.0(10) . . ? C51 C46 O7 123.2(10) . . ? C46 C47 C48 118.6(11) . . ? C46 C47 H47A 120.7 . . ? C48 C47 H47A 120.7 . . ? C49 C48 C47 119.5(11) . . ? C49 C48 H48A 120.2 . . ? C47 C48 H48A 120.2 . . ? C50 C49 C48 119.0(9) . . ? C50 C49 C52 120.7(9) . . ? C48 C49 C52 120.2(9) . . ? C49 C50 C51 121.5(11) . . ? C49 C50 H50A 119.2 . . ? C51 C50 H50A 119.2 . . ? C46 C51 C50 118.5(11) . . ? C46 C51 H51A 120.7 . . ? C50 C51 H51A 120.7 . . ? O18 C52 O19 125.3(9) . . ? O18 C52 C49 118.2(9) . . ? O19 C52 C49 116.4(9) . . ? N3 C53 N1 124.6(8) . . ? N3 C53 C56 116.8(8) . . ? N1 C53 C56 118.6(9) . . ? N2 C54 N1 125.8(8) . . ? N2 C54 C61 117.6(8) . . ? N1 C54 C61 116.6(8) . . ? N3 C55 N2 125.8(9) . . ? N3 C55 C66 116.1(8) . . ? N2 C55 C66 118.0(8) . . ? C60 C56 C57 115.6(10) . . ? C60 C56 C53 121.6(9) . . ? C57 C56 C53 122.8(9) . . ? C58 C57 C56 120.3(9) . . ? C58 C57 H57A 119.8 . . ? C56 C57 H57A 119.8 . . ? C57 C58 N4 122.9(9) . . ? C57 C58 H58A 118.6 . . ? N4 C58 H58A 118.6 . . ? N4 C59 C60 122.0(10) . . ? N4 C59 H59A 119.0 . . ? C60 C59 H59A 119.0 . . ? C56 C60 C59 121.6(11) . . ? C56 C60 H60A 119.2 . . ? C59 C60 H60A 119.2 . . ? C65 C61 C62 118.9(8) . . ? C65 C61 C54 118.9(8) . . ? C62 C61 C54 122.1(8) . . ? C63 C62 C61 119.2(8) . . ? C63 C62 H62A 120.4 . . ? C61 C62 H62A 120.4 . . ? N5 C63 C62 123.0(9) . . ? N5 C63 H63A 118.5 . . ? C62 C63 H63A 118.5 . . ? N5 C64 C65 124.3(9) . . ? N5 C64 H64A 117.8 . . ? C65 C64 H64A 117.9 . . ? C61 C65 C64 117.2(9) . . ? C61 C65 H65A 121.4 . . ? C64 C65 H65A 121.4 . . ? C70 C66 C67 117.1(9) . . ? C70 C66 C55 121.8(8) . . ? C67 C66 C55 121.1(8) . . ? C66 C67 C68 119.9(9) . . ? C66 C67 H67A 120.0 . . ? C68 C67 H67A 120.0 . . ? N6 C68 C67 122.1(8) . . ? N6 C68 H68A 119.0 . . ? C67 C68 H68A 119.0 . . ? N6 C69 C70 123.1(8) . . ? N6 C69 H69A 118.4 . . ? C70 C69 H69A 118.4 . . ? C69 C70 C66 120.3(8) . . ? C69 C70 H70A 119.9 . . ? C66 C70 H70A 119.9 . . ? C1 O1 C2 115.1(8) . . ? C11 O2 C5 115.7(9) . . ? C18 O3 C6 118.0(9) . . ? C25 O4 C7 116.4(9) . . ? C32 O5 C8 118.4(9) . . ? C39 O6 C9 119.1(9) . . ? C10 O7 C46 118.6(8) . . ? C17 O8 Co2 138.3(6) . 1_454 ? C17 O9 Co3 127.3(6) . 1_454 ? C24 O10 Co3 133.3(6) . 1_554 ? C24 O11 Co2 131.8(7) . 1_554 ? C31 O13 Co3 130.3(7) . 2_657 ? C38 O14 Co3 135.2(6) . 2_557 ? C38 O15 Co1 138.5(6) . 2_557 ? C45 O16 Co1 132.6(6) . 1_455 ? C45 O17 Co2 127.1(6) . 1_455 ? C52 O18 Co2 132.2(6) . . ? C52 O19 Co1 127.7(7) . . ? Co3 O20 Co1 127.4(3) . . ? Co3 O20 Co2 113.1(3) . . ? Co1 O20 Co2 110.0(3) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.22 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.016 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.220 # Attachment '- 5.CIF' data_5 _database_code_depnum_ccdc_archive 'CCDC 865801' #TrackingRef '- 5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H52 Co3 N8 O24' _chemical_formula_weight 1638.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 16.965(7) _cell_length_b 28.706(11) _cell_length_c 14.825(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.490(5) _cell_angle_gamma 90.00 _cell_volume 7049(6) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description brick _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1674 _exptl_absorpt_coefficient_mu 0.394 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6182 _exptl_absorpt_correction_T_max 0.7448 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19428 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.1077 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10917 _reflns_number_gt 7099 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1332P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0130(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 10917 _refine_ls_number_parameters 467 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2351 _refine_ls_wR_factor_gt 0.2062 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.056 _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 Co1 Co 0.5000 0.30203(4) 0.0000 0.0414(3) Uani 1 2 d S . . Co2 Co 0.39408(4) 0.40497(3) -0.00939(6) 0.0402(3) Uani 1 1 d . . . O1 O 0.6531(4) 0.7555(2) 0.5269(4) 0.093(2) Uani 1 1 d . . . O2 O 0.5000 0.6886(3) 0.5000 0.090(3) Uani 1 2 d S . . O3 O 0.5403(4) 0.6435(2) 0.3038(4) 0.0874(18) Uani 1 1 d . . . O4 O 0.6923(5) 0.7186(2) 0.3185(6) 0.112(3) Uani 1 1 d . . . O5 O 0.8909(3) 0.79612(19) 0.9068(4) 0.0760(16) Uani 1 1 d . . . O6 O 0.8334(3) 0.86527(17) 0.8795(4) 0.0601(14) Uani 1 1 d . . . O7 O 0.8539(3) 0.86043(18) 0.0841(4) 0.0609(13) Uani 1 1 d . . . O8 O 0.9397(3) 0.8009(2) 0.1069(4) 0.0775(16) Uani 1 1 d . . . O11 O 0.5000 0.3722(2) 0.0000 0.059(2) Uani 1 2 d S . . O9 O 0.4466(3) 0.4534(2) 0.0958(4) 0.0725(16) Uani 1 1 d . . . O10 O 0.5779(3) 0.4537(2) 0.1028(4) 0.0724(17) Uani 1 1 d . . . N3 N 0.5000 0.2280(3) 0.0000 0.062(2) Uani 1 2 d S . . N1 N 0.4309(3) 0.0585(2) 0.0033(6) 0.073(2) Uani 1 1 d . . . N2 N 0.5000 -0.0127(3) 0.0000 0.071(3) Uani 1 2 d S . . N4 N 0.2173(3) -0.05930(18) 0.0151(4) 0.0505(15) Uani 1 1 d . . . C1 C 0.5995(4) 0.7020(2) 0.4098(5) 0.0530(17) Uani 1 1 d . . . C3 C 0.6168(5) 0.7332(3) 0.3338(6) 0.069(2) Uani 1 1 d . . . H3A H 0.5751 0.7297 0.2780 0.083 Uiso 1 1 calc R . . H3B H 0.6190 0.7655 0.3529 0.083 Uiso 1 1 calc R . . C2 C 0.6597(6) 0.7091(3) 0.4980(6) 0.075(2) Uani 1 1 d . . . H2A H 0.6492 0.6877 0.5447 0.090 Uiso 1 1 calc R . . H2B H 0.7138 0.7034 0.4889 0.090 Uiso 1 1 calc R . . C5 C 0.5164(5) 0.7144(3) 0.4254(5) 0.062(2) Uani 1 1 d . . . H5A H 0.5142 0.7474 0.4384 0.075 Uiso 1 1 calc R . . H5B H 0.4759 0.7077 0.3700 0.075 Uiso 1 1 calc R . . C4 C 0.6037(5) 0.6513(3) 0.3843(5) 0.063(2) Uani 1 1 d . . . H4A H 0.6559 0.6443 0.3708 0.075 Uiso 1 1 calc R . . H4B H 0.5960 0.6316 0.4348 0.075 Uiso 1 1 calc R . . C6 C 0.7000(6) 0.7693(3) 0.6115(6) 0.081(3) Uani 1 1 d . . . C11 C 0.7597(7) 0.7433(3) 0.6626(7) 0.108(4) Uani 1 1 d . . . H11A H 0.7718 0.7141 0.6419 0.129 Uiso 1 1 calc R . . C20 C 0.5383(5) 0.5993(3) 0.2638(6) 0.073(2) Uani 1 1 d . . . C21 C 0.6010(7) 0.5740(5) 0.2624(14) 0.184(9) Uani 1 1 d . . . H21A H 0.6513 0.5830 0.2965 0.221 Uiso 1 1 calc R . . C25 C 0.4669(6) 0.5822(4) 0.2250(10) 0.126(5) Uani 1 1 d . . . H25A H 0.4209 0.5993 0.2277 0.151 Uiso 1 1 calc R . . C13 C 0.7325(6) 0.7465(3) 0.2683(7) 0.086(3) Uani 1 1 d . . . C14 C 0.7058(5) 0.7877(3) 0.2250(7) 0.081(3) Uani 1 1 d . . . H14A H 0.6549 0.7989 0.2275 0.097 Uiso 1 1 calc R . . C15 C 0.7522(5) 0.8119(3) 0.1794(6) 0.070(2) Uani 1 1 d . . . H15A H 0.7348 0.8408 0.1543 0.084 Uiso 1 1 calc R . . C16 C 0.8251(4) 0.7946(3) 0.1691(5) 0.0598(19) Uani 1 1 d . . . C17 C 0.8507(6) 0.7539(3) 0.2081(8) 0.096(3) Uani 1 1 d . . . H17A H 0.8995 0.7419 0.1997 0.115 Uiso 1 1 calc R . . C18 C 0.8074(8) 0.7290(4) 0.2603(10) 0.136(6) Uani 1 1 d . . . H18A H 0.8274 0.7013 0.2893 0.164 Uiso 1 1 calc R . . C27 C 0.4314(4) 0.2031(2) 0.0011(7) 0.075(3) Uani 1 1 d . . . H27A H 0.3838 0.2192 0.0014 0.090 Uiso 1 1 calc R . . C28 C 0.4307(4) 0.1559(2) 0.0018(7) 0.080(3) Uani 1 1 d . . . H28A H 0.3831 0.1402 0.0037 0.096 Uiso 1 1 d R . . C29 C 0.5000 0.1309(3) 0.0000 0.063(3) Uani 1 2 d S . . C30 C 0.5000 0.0803(4) 0.0000 0.068(3) Uani 1 2 d S . . C31 C 0.4341(4) 0.0118(2) 0.0037(6) 0.066(2) Uani 1 1 d . . . C12 C 0.8431(4) 0.8237(3) 0.8608(6) 0.0573(19) Uani 1 1 d . . . C9 C 0.7911(4) 0.8042(3) 0.7737(5) 0.0613(18) Uani 1 1 d . . . C8 C 0.7311(6) 0.8301(3) 0.7187(6) 0.092(3) Uani 1 1 d . . . H8A H 0.7211 0.8601 0.7373 0.111 Uiso 1 1 calc R . . C7 C 0.6863(6) 0.8134(3) 0.6381(7) 0.096(3) Uani 1 1 d . . . H7A H 0.6468 0.8318 0.6016 0.115 Uiso 1 1 calc R . . C10 C 0.8025(7) 0.7604(3) 0.7455(7) 0.095(3) Uani 1 1 d . . . H10A H 0.8403 0.7414 0.7831 0.114 Uiso 1 1 calc R . . C34 C 0.2196(4) -0.0123(3) 0.0117(7) 0.074(3) Uani 1 1 d . . . H34A H 0.1726 0.0044 0.0113 0.089 Uiso 1 1 calc R . . C33 C 0.2897(4) 0.0115(3) 0.0089(7) 0.073(2) Uani 1 1 d . . . H33A H 0.2898 0.0439 0.0077 0.088 Uiso 1 1 calc R . . C32 C 0.3594(4) -0.0127(2) 0.0078(6) 0.066(2) Uani 1 1 d . . . C36 C 0.3571(4) -0.0609(2) 0.0127(7) 0.071(2) Uani 1 1 d . . . H36A H 0.4034 -0.0784 0.0137 0.085 Uiso 1 1 calc R . . C35 C 0.2867(4) -0.0821(2) 0.0163(6) 0.062(2) Uani 1 1 d . . . H35A H 0.2863 -0.1145 0.0197 0.075 Uiso 1 1 calc R . . C26 C 0.5154(4) 0.4700(3) 0.1192(5) 0.0541(18) Uani 1 1 d . . . C19 C 0.8770(4) 0.8206(2) 0.1163(6) 0.0556(18) Uani 1 1 d . . . C23 C 0.5223(4) 0.5155(3) 0.1707(5) 0.0561(18) Uani 1 1 d . . . C24 C 0.4588(6) 0.5407(4) 0.1816(10) 0.122(5) Uani 1 1 d . . . H24A H 0.4072 0.5292 0.1584 0.147 Uiso 1 1 calc R . . C22 C 0.5934(6) 0.5325(5) 0.2091(12) 0.162(7) Uani 1 1 d . . . H22A H 0.6397 0.5170 0.2013 0.195 Uiso 1 1 calc R . . O2W O 0.657(3) 0.7476(18) 0.895(3) 0.51(2) Uiso 1 1 d . . . C38 C 0.652(3) 0.6468(18) 1.042(3) 0.39(2) Uiso 1 1 d . . . N5 N 0.702(3) 0.699(2) 0.961(3) 0.46(3) Uiso 1 1 d . . . C37 C 0.700(4) 0.631(3) 0.928(4) 0.48(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0269(6) 0.0248(6) 0.0750(9) 0.000 0.0164(5) 0.000 Co2 0.0256(3) 0.0267(4) 0.0699(6) -0.0019(4) 0.0137(3) 0.0012(3) O1 0.124(6) 0.052(3) 0.088(4) -0.025(3) -0.011(4) 0.002(4) O2 0.143(8) 0.055(5) 0.104(6) 0.000 0.097(6) 0.000 O3 0.096(4) 0.064(4) 0.100(4) -0.045(3) 0.017(3) -0.006(3) O4 0.119(6) 0.080(5) 0.174(7) 0.035(5) 0.110(5) 0.010(4) O5 0.061(3) 0.041(3) 0.110(4) -0.013(3) -0.016(3) -0.001(3) O6 0.049(3) 0.044(3) 0.080(4) -0.020(2) -0.003(2) 0.007(2) O7 0.048(3) 0.054(3) 0.089(4) 0.011(3) 0.036(3) 0.006(2) O8 0.072(3) 0.055(3) 0.121(5) 0.026(3) 0.056(3) 0.020(3) O11 0.029(3) 0.022(3) 0.133(7) 0.000 0.029(4) 0.000 O9 0.042(3) 0.064(4) 0.117(4) -0.039(3) 0.029(3) -0.010(3) O10 0.038(3) 0.062(3) 0.116(4) -0.042(3) 0.014(3) 0.001(2) N3 0.031(4) 0.029(4) 0.131(8) 0.000 0.031(4) 0.000 N1 0.030(3) 0.030(3) 0.168(7) -0.002(4) 0.040(3) -0.006(2) N2 0.029(4) 0.030(4) 0.159(9) 0.000 0.034(5) 0.000 N4 0.029(3) 0.025(3) 0.101(5) 0.005(3) 0.020(3) -0.002(2) C1 0.068(4) 0.045(4) 0.055(4) -0.014(3) 0.031(3) -0.019(3) C3 0.083(5) 0.060(5) 0.079(5) -0.003(4) 0.051(4) -0.010(4) C2 0.093(6) 0.053(5) 0.075(6) -0.016(4) 0.012(4) -0.008(4) C5 0.085(5) 0.055(4) 0.058(5) -0.003(4) 0.040(4) -0.013(4) C4 0.081(5) 0.054(4) 0.060(5) -0.021(4) 0.030(4) -0.020(4) C6 0.096(6) 0.046(5) 0.086(6) -0.027(4) -0.016(5) -0.004(5) C11 0.129(9) 0.058(6) 0.113(8) -0.045(6) -0.026(7) 0.020(6) C20 0.071(5) 0.066(5) 0.085(6) -0.041(5) 0.022(4) -0.009(4) C21 0.065(6) 0.131(12) 0.34(2) -0.159(15) 0.007(10) -0.003(7) C25 0.065(6) 0.090(8) 0.212(13) -0.091(9) 0.006(7) 0.009(6) C13 0.093(7) 0.065(6) 0.122(8) 0.019(5) 0.071(6) -0.005(5) C14 0.065(5) 0.075(6) 0.116(7) 0.023(5) 0.052(5) 0.006(4) C15 0.074(5) 0.061(5) 0.088(6) 0.018(4) 0.046(4) 0.006(4) C16 0.057(4) 0.057(5) 0.075(5) 0.014(4) 0.034(4) 0.004(4) C17 0.082(6) 0.072(6) 0.157(9) 0.042(6) 0.081(6) 0.017(5) C18 0.144(10) 0.111(9) 0.200(13) 0.080(9) 0.137(10) 0.053(8) C27 0.042(4) 0.023(4) 0.168(8) -0.001(4) 0.037(4) 0.000(3) C28 0.029(3) 0.032(4) 0.184(9) 0.000(5) 0.035(4) -0.003(3) C29 0.021(4) 0.033(5) 0.140(10) 0.000 0.028(5) 0.000 C30 0.033(4) 0.032(5) 0.141(10) 0.000 0.021(5) 0.000 C31 0.035(3) 0.024(3) 0.143(7) 0.005(4) 0.029(4) 0.003(3) C12 0.041(3) 0.042(4) 0.083(5) -0.005(4) 0.002(3) 0.002(3) C9 0.058(4) 0.047(4) 0.074(5) -0.014(4) 0.004(4) -0.007(4) C8 0.094(7) 0.063(6) 0.097(7) -0.044(5) -0.029(5) 0.024(5) C7 0.094(7) 0.070(6) 0.099(7) -0.026(5) -0.031(5) 0.025(5) C10 0.101(7) 0.055(6) 0.114(8) -0.007(5) -0.011(6) 0.008(5) C34 0.027(3) 0.037(4) 0.161(8) -0.002(4) 0.027(4) -0.001(3) C33 0.038(3) 0.026(3) 0.160(8) -0.001(4) 0.031(4) -0.004(3) C32 0.032(3) 0.031(4) 0.138(7) 0.000(4) 0.025(4) 0.004(3) C36 0.032(4) 0.036(4) 0.149(8) 0.004(4) 0.029(4) 0.001(3) C35 0.035(3) 0.034(4) 0.123(6) 0.003(4) 0.029(4) -0.004(3) C26 0.039(4) 0.050(4) 0.075(5) -0.014(4) 0.015(3) -0.007(3) C19 0.049(4) 0.040(4) 0.087(5) 0.007(4) 0.034(4) -0.001(3) C23 0.053(4) 0.048(4) 0.067(5) -0.021(3) 0.013(3) -0.003(3) C24 0.058(5) 0.108(9) 0.198(12) -0.096(9) 0.023(6) -0.008(6) C22 0.060(6) 0.151(12) 0.270(17) -0.158(13) 0.025(8) -0.023(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O11 2.013(6) . ? Co1 O5 2.064(5) 4_646 ? Co1 O5 2.064(5) 3_444 ? Co1 O8 2.065(5) 3_445 ? Co1 O8 2.065(5) 4_645 ? Co1 N3 2.125(8) . ? Co2 O11 2.007(3) . ? Co2 O6 2.083(5) 3_444 ? Co2 O10 2.094(5) 2_655 ? Co2 O7 2.104(5) 3_445 ? Co2 N4 2.136(5) 4 ? Co2 O9 2.136(5) . ? O1 C6 1.389(10) . ? O1 C2 1.411(10) . ? O2 C5 1.408(9) 2_656 ? O2 C5 1.408(9) . ? O3 C20 1.399(9) . ? O3 C4 1.441(10) . ? O4 C13 1.372(10) . ? O4 C3 1.411(10) . ? O5 C12 1.229(8) . ? O5 Co1 2.064(5) 3_556 ? O6 C12 1.243(8) . ? O6 Co2 2.083(5) 3_556 ? O7 C19 1.268(8) . ? O7 Co2 2.104(5) 3 ? O8 C19 1.238(8) . ? O8 Co1 2.065(5) 3 ? O11 Co2 2.007(3) 2_655 ? O9 C26 1.237(8) . ? O10 C26 1.231(8) . ? O10 Co2 2.094(5) 2_655 ? N3 C27 1.367(8) 2_655 ? N3 C27 1.367(8) . ? N1 C30 1.338(7) . ? N1 C31 1.343(9) . ? N2 C31 1.332(8) 2_655 ? N2 C31 1.332(8) . ? N4 C35 1.344(8) . ? N4 C34 1.350(9) . ? N4 Co2 2.136(5) 4_545 ? C1 C2 1.489(11) . ? C1 C4 1.508(10) . ? C1 C3 1.515(10) . ? C1 C5 1.520(10) . ? C6 C11 1.351(13) . ? C6 C7 1.362(12) . ? C11 C10 1.376(13) . ? C20 C21 1.291(14) . ? C20 C25 1.317(13) . ? C21 C22 1.420(14) . ? C25 C24 1.345(13) . ? C13 C14 1.375(12) . ? C13 C18 1.396(14) . ? C14 C15 1.338(11) . ? C15 C16 1.373(10) . ? C16 C17 1.335(11) . ? C16 C19 1.497(9) . ? C17 C18 1.377(12) . ? C27 C28 1.357(10) . ? C28 C29 1.383(8) . ? C29 C28 1.383(8) 2_655 ? C29 C30 1.453(14) . ? C30 N1 1.338(7) 2_655 ? C31 C32 1.461(9) . ? C12 C9 1.507(10) . ? C9 C10 1.351(12) . ? C9 C8 1.376(11) . ? C8 C7 1.357(11) . ? C34 C33 1.382(9) . ? C33 C32 1.375(9) . ? C32 C36 1.386(10) . ? C36 C35 1.353(9) . ? C26 C23 1.506(10) . ? C23 C22 1.311(12) . ? C23 C24 1.336(12) . ? O2W N5 1.78(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Co1 O5 94.71(15) . 4_646 ? O11 Co1 O5 94.71(15) . 3_444 ? O5 Co1 O5 170.6(3) 4_646 3_444 ? O11 Co1 O8 90.88(17) . 3_445 ? O5 Co1 O8 90.4(3) 4_646 3_445 ? O5 Co1 O8 89.5(3) 3_444 3_445 ? O11 Co1 O8 90.88(17) . 4_645 ? O5 Co1 O8 89.5(3) 4_646 4_645 ? O5 Co1 O8 90.4(3) 3_444 4_645 ? O8 Co1 O8 178.2(3) 3_445 4_645 ? O11 Co1 N3 180.0 . . ? O5 Co1 N3 85.29(15) 4_646 . ? O5 Co1 N3 85.29(15) 3_444 . ? O8 Co1 N3 89.12(17) 3_445 . ? O8 Co1 N3 89.12(17) 4_645 . ? O11 Co2 O6 94.60(17) . 3_444 ? O11 Co2 O10 91.80(18) . 2_655 ? O6 Co2 O10 89.2(2) 3_444 2_655 ? O11 Co2 O7 94.70(18) . 3_445 ? O6 Co2 O7 90.8(2) 3_444 3_445 ? O10 Co2 O7 173.5(2) 2_655 3_445 ? O11 Co2 N4 178.20(19) . 4 ? O6 Co2 N4 87.1(2) 3_444 4 ? O10 Co2 N4 88.8(2) 2_655 4 ? O7 Co2 N4 84.7(2) 3_445 4 ? O11 Co2 O9 91.65(18) . . ? O6 Co2 O9 172.2(2) 3_444 . ? O10 Co2 O9 86.0(3) 2_655 . ? O7 Co2 O9 93.3(2) 3_445 . ? N4 Co2 O9 86.7(2) 4 . ? C6 O1 C2 118.3(7) . . ? C5 O2 C5 116.6(9) 2_656 . ? C20 O3 C4 116.0(7) . . ? C13 O4 C3 119.3(7) . . ? C12 O5 Co1 135.0(5) . 3_556 ? C12 O6 Co2 129.4(5) . 3_556 ? C19 O7 Co2 132.7(4) . 3 ? C19 O8 Co1 131.2(5) . 3 ? Co2 O11 Co2 124.0(3) 2_655 . ? Co2 O11 Co1 117.99(15) 2_655 . ? Co2 O11 Co1 117.99(15) . . ? C26 O9 Co2 132.4(5) . . ? C26 O10 Co2 135.5(5) . 2_655 ? C27 N3 C27 117.1(8) 2_655 . ? C27 N3 Co1 121.4(4) 2_655 . ? C27 N3 Co1 121.4(4) . . ? C30 N1 C31 115.5(6) . . ? C31 N2 C31 116.3(8) 2_655 . ? C35 N4 C34 117.1(5) . . ? C35 N4 Co2 122.1(4) . 4_545 ? C34 N4 Co2 120.6(4) . 4_545 ? C2 C1 C4 107.0(7) . . ? C2 C1 C3 111.5(7) . . ? C4 C1 C3 110.8(6) . . ? C2 C1 C5 108.4(6) . . ? C4 C1 C5 111.0(6) . . ? C3 C1 C5 108.1(7) . . ? O4 C3 C1 105.8(7) . . ? O1 C2 C1 108.2(7) . . ? O2 C5 C1 110.1(6) . . ? O3 C4 C1 106.9(7) . . ? C11 C6 C7 120.4(8) . . ? C11 C6 O1 124.3(8) . . ? C7 C6 O1 115.2(8) . . ? C6 C11 C10 119.4(8) . . ? C21 C20 C25 117.8(9) . . ? C21 C20 O3 124.9(9) . . ? C25 C20 O3 117.3(8) . . ? C20 C21 C22 120.3(10) . . ? C20 C25 C24 121.8(9) . . ? O4 C13 C14 127.1(8) . . ? O4 C13 C18 113.8(9) . . ? C14 C13 C18 119.0(8) . . ? C15 C14 C13 120.9(8) . . ? C14 C15 C16 120.7(8) . . ? C17 C16 C15 119.0(7) . . ? C17 C16 C19 119.4(7) . . ? C15 C16 C19 121.6(7) . . ? C16 C17 C18 122.4(9) . . ? C17 C18 C13 117.8(10) . . ? C28 C27 N3 122.1(7) . . ? C27 C28 C29 120.6(7) . . ? C28 C29 C28 117.5(9) 2_655 . ? C28 C29 C30 121.3(4) 2_655 . ? C28 C29 C30 121.3(4) . . ? N1 C30 N1 124.4(9) 2_655 . ? N1 C30 C29 117.8(5) 2_655 . ? N1 C30 C29 117.8(5) . . ? N2 C31 N1 124.1(6) . . ? N2 C31 C32 119.4(6) . . ? N1 C31 C32 116.5(6) . . ? O5 C12 O6 126.8(7) . . ? O5 C12 C9 115.4(7) . . ? O6 C12 C9 117.8(7) . . ? C10 C9 C8 117.2(7) . . ? C10 C9 C12 121.0(8) . . ? C8 C9 C12 121.8(7) . . ? C7 C8 C9 122.1(8) . . ? C8 C7 C6 119.1(8) . . ? C9 C10 C11 121.7(9) . . ? N4 C34 C33 121.8(6) . . ? C32 C33 C34 119.9(7) . . ? C33 C32 C36 118.0(6) . . ? C33 C32 C31 120.9(6) . . ? C36 C32 C31 121.1(6) . . ? C35 C36 C32 119.2(6) . . ? N4 C35 C36 123.9(6) . . ? O10 C26 O9 126.8(7) . . ? O10 C26 C23 117.0(6) . . ? O9 C26 C23 116.2(6) . . ? O8 C19 O7 124.9(6) . . ? O8 C19 C16 116.6(6) . . ? O7 C19 C16 118.5(6) . . ? C22 C23 C24 115.9(8) . . ? C22 C23 C26 120.4(8) . . ? C24 C23 C26 123.7(7) . . ? C23 C24 C25 122.3(9) . . ? C23 C22 C21 121.1(10) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.651 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.167