# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 816745' #TrackingRef '- n (1-4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C144 H136 Cl2 Mn7 N4 O44, 4(O0.50), 2(O0.50), 2(O0.50), 2(O0.50), 4(O)' _chemical_formula_sum 'C144 H136 Cl2 Mn7 N4 O54' _chemical_formula_weight 3242.06 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.6622(12) _cell_length_b 17.3679(14) _cell_length_c 20.5165(17) _cell_angle_alpha 66.9042(10) _cell_angle_beta 77.860(2) _cell_angle_gamma 68.1339(10) _cell_volume 4447.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1075 _cell_measurement_theta_min 2.277 _cell_measurement_theta_max 16.662 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1669.0 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8437 _exptl_absorpt_correction_T_max 0.8720 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24407 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.00 _reflns_number_total 17120 _reflns_number_gt 12492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+2.1162P] 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 17120 _refine_ls_number_parameters 1025 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.87154(19) 1.38781(17) -0.38004(14) 0.0393(6) Uani 1 1 d . . . C2 C 0.8778(2) 1.30299(18) -0.32067(17) 0.0532(8) Uani 1 1 d . . . C3 C 0.7934(2) 1.27948(18) -0.29102(14) 0.0437(7) Uani 1 1 d . . . H3 H 0.7322 1.3183 -0.3067 0.052 Uiso 1 1 calc R . . C4 C 0.8006(2) 1.19789(18) -0.23793(15) 0.0461(7) Uani 1 1 d . . . H4 H 0.7441 1.1822 -0.2181 0.055 Uiso 1 1 calc R . . C5 C 0.8921(2) 1.13980(17) -0.21448(14) 0.0444(7) Uani 1 1 d . . . C6 C 0.9765(2) 1.16331(17) -0.24412(15) 0.0431(7) Uani 1 1 d . . . H6 H 1.0377 1.1244 -0.2284 0.052 Uiso 1 1 calc R . . C7 C 0.96932(19) 1.24490(16) -0.29722(14) 0.0373(6) Uani 1 1 d . . . H7 H 1.0258 1.2606 -0.3170 0.045 Uiso 1 1 calc R . . C8 C 0.98005(19) 0.99708(15) -0.14493(14) 0.0362(6) Uani 1 1 d . . . H8A H 1.0082 1.0068 -0.1112 0.043 Uiso 1 1 calc R . . H8B H 1.0265 0.9961 -0.1862 0.043 Uiso 1 1 calc R . . C9 C 0.95691(19) 0.91247(16) -0.11187(13) 0.0341(5) Uani 1 1 d . . . C10 C 0.92766(17) 0.88020(15) -0.04020(13) 0.0286(5) Uani 1 1 d . . . C11 C 0.90575(17) 0.80320(16) -0.01282(13) 0.0307(5) Uani 1 1 d . . . C12 C 0.92233(17) 0.75228(17) -0.05603(13) 0.0314(5) Uani 1 1 d . . . C13 C 0.95140(17) 0.78618(16) -0.12714(13) 0.0305(5) Uani 1 1 d . . . C14 C 0.96737(18) 0.86747(17) -0.15617(13) 0.0332(5) Uani 1 1 d . . . C15 C 0.99385(19) 0.90501(17) -0.23671(13) 0.0369(6) Uani 1 1 d . . . H15B H 1.0640 0.8842 -0.2462 0.055 Uiso 1 1 calc R . . H15C H 0.9710 0.9684 -0.2525 0.055 Uiso 1 1 calc R . . H15A H 0.9630 0.8858 -0.2616 0.055 Uiso 1 1 calc R . . C16 C 0.9713(2) 0.73427(18) -0.17608(15) 0.0412(6) Uani 1 1 d . . . H16A H 1.0235 0.7465 -0.2123 0.049 Uiso 1 1 calc R . . H16B H 0.9908 0.6713 -0.1494 0.049 Uiso 1 1 calc R . . C17 C 0.9187(2) 0.92941(17) 0.00906(14) 0.0385(6) Uani 1 1 d . . . H17A H 0.8508 0.9622 0.0165 0.058 Uiso 1 1 calc R . . H17B H 0.9563 0.9694 -0.0120 0.058 Uiso 1 1 calc R . . H17C H 0.9435 0.8878 0.0538 0.058 Uiso 1 1 calc R . . C18 C 0.90526(18) 0.66604(16) -0.02259(13) 0.0325(5) Uani 1 1 d . . . H18A H 0.9046 0.6443 -0.0588 0.049 Uiso 1 1 calc R . . H18B H 0.8431 0.6730 0.0050 0.049 Uiso 1 1 calc R . . H18C H 0.9570 0.6248 0.0078 0.049 Uiso 1 1 calc R . . C19 C 0.8814(2) 0.72723(18) -0.25578(14) 0.0404(6) Uani 1 1 d . . . C20 C 0.79215(19) 0.75044(17) -0.28166(13) 0.0364(6) Uani 1 1 d . . . H20 H 0.7360 0.7874 -0.2651 0.044 Uiso 1 1 calc R . . C21 C 0.7859(2) 0.71909(17) -0.33190(13) 0.0364(6) Uani 1 1 d . . . H21 H 0.7256 0.7360 -0.3500 0.044 Uiso 1 1 calc R . . C22 C 0.86826(18) 0.66283(16) -0.35570(13) 0.0337(5) Uani 1 1 d . . . C23 C 0.9573(2) 0.64014(18) -0.33030(15) 0.0418(6) Uani 1 1 d . . . H23 H 1.0135 0.6035 -0.3472 0.050 Uiso 1 1 calc R . . C24 C 0.96428(19) 0.67142(17) -0.27984(14) 0.0405(6) Uani 1 1 d . . . H24 H 1.0247 0.6549 -0.2621 0.049 Uiso 1 1 calc R . . C25 C 0.86279(19) 0.62402(17) -0.40701(13) 0.0357(6) Uani 1 1 d . . . C26 C 0.85925(19) 0.77689(17) 0.06018(13) 0.0355(6) Uani 1 1 d . . . H26A H 0.8245 0.8292 0.0730 0.043 Uiso 1 1 calc R . . H26B H 0.8113 0.7499 0.0617 0.043 Uiso 1 1 calc R . . C27 C 0.89609(18) 0.69709(16) 0.17985(13) 0.0333(5) Uani 1 1 d . . . C28 C 0.8037(2) 0.74726(18) 0.20784(14) 0.0447(7) Uani 1 1 d . . . H28 H 0.7613 0.7971 0.1774 0.054 Uiso 1 1 calc R . . C29 C 0.7806(2) 0.72095(18) 0.27748(14) 0.0421(7) Uani 1 1 d . . . H29 H 0.7219 0.7544 0.2947 0.050 Uiso 1 1 calc R . . C30 C 0.83890(18) 0.64692(16) 0.32550(13) 0.0332(5) Uani 1 1 d . . . C31 C 0.92704(19) 0.60043(16) 0.29834(13) 0.0355(6) Uani 1 1 d . . . H31 H 0.9680 0.5504 0.3297 0.043 Uiso 1 1 calc R . . C32 C 0.9571(2) 0.62471(18) 0.22698(14) 0.0426(7) Uani 1 1 d . . . H32 H 1.0179 0.5925 0.2109 0.051 Uiso 1 1 calc R . . C33 C 0.80610(18) 0.62196(16) 0.40236(13) 0.0318(5) Uani 1 1 d . . . C34 C 0.7003(2) 0.87978(18) 0.40711(14) 0.0380(6) Uani 1 1 d . . . H34A H 0.7386 0.8208 0.4084 0.057 Uiso 1 1 calc R . . H34B H 0.7424 0.9158 0.3916 0.057 Uiso 1 1 calc R . . H34C H 0.6498 0.9042 0.3747 0.057 Uiso 1 1 calc R . . C35 C 0.6397(2) 0.95077(17) 0.49950(14) 0.0394(6) Uani 1 1 d . . . H35A H 0.6059 1.0050 0.4644 0.059 Uiso 1 1 calc R . . H35B H 0.7020 0.9528 0.5051 0.059 Uiso 1 1 calc R . . H35C H 0.6005 0.9433 0.5440 0.059 Uiso 1 1 calc R . . C36 C 0.61576(17) 0.81679(16) 0.51966(13) 0.0314(5) Uani 1 1 d . . . H36 H 0.6217 0.7709 0.5047 0.038 Uiso 1 1 calc R . . C37 C 0.61636(19) 0.60813(17) 0.73036(15) 0.0394(6) Uani 1 1 d . . . H37 H 0.6424 0.5887 0.6920 0.047 Uiso 1 1 calc R . . C38 C 0.62558(18) 0.60154(16) 0.84616(13) 0.0323(5) Uani 1 1 d . . . H38A H 0.5783 0.6595 0.8293 0.048 Uiso 1 1 calc R . . H38B H 0.6771 0.6043 0.8665 0.048 Uiso 1 1 calc R . . H38C H 0.5937 0.5621 0.8817 0.048 Uiso 1 1 calc R . . C39 C 0.7594(2) 0.50696(18) 0.78718(15) 0.0500(8) Uani 1 1 d . . . H39A H 0.7618 0.4748 0.7577 0.075 Uiso 1 1 calc R . . H39B H 0.7718 0.4668 0.8349 0.075 Uiso 1 1 calc R . . H39C H 0.8085 0.5359 0.7691 0.075 Uiso 1 1 calc R . . C40 C 0.30970(18) 0.88959(17) 0.69579(14) 0.0350(6) Uani 1 1 d . . . C41 C 0.31676(19) 0.92585(16) 0.74821(14) 0.0352(6) Uani 1 1 d . . . C42 C 0.23387(19) 0.98872(16) 0.76590(14) 0.0338(5) Uani 1 1 d . . . H42 H 0.1751 1.0059 0.7457 0.041 Uiso 1 1 calc R . . C43 C 0.23820(19) 1.02575(16) 0.81308(14) 0.0375(6) Uani 1 1 d . . . H43 H 0.1826 1.0679 0.8245 0.045 Uiso 1 1 calc R . . C44 C 0.32371(18) 1.00064(17) 0.84282(14) 0.0365(6) Uani 1 1 d . . . C45 C 0.40674(19) 0.93815(17) 0.82627(14) 0.0379(6) Uani 1 1 d . . . H45 H 0.4649 0.9208 0.8472 0.045 Uiso 1 1 calc R . . C46 C 0.4030(2) 0.90115(17) 0.77786(14) 0.0406(6) Uani 1 1 d . . . H46 H 0.4590 0.8598 0.7659 0.049 Uiso 1 1 calc R . . C47 C 0.41115(19) 1.01692(17) 0.92003(14) 0.0405(6) Uani 1 1 d . . . H47A H 0.4620 1.0297 0.8827 0.049 Uiso 1 1 calc R . . H47B H 0.4339 0.9547 0.9487 0.049 Uiso 1 1 calc R . . C48 C 0.38984(17) 1.07176(16) 0.96453(13) 0.0313(5) Uani 1 1 d . . . C49 C 0.4065(2) 1.15230(17) 0.93358(14) 0.0401(6) Uani 1 1 d . . . C50 C 0.39741(19) 1.19929(17) 0.97332(14) 0.0389(6) Uani 1 1 d . . . C51 C 0.36273(18) 1.17196(16) 1.04777(14) 0.0335(5) Uani 1 1 d . . . C52 C 0.33653(18) 1.09831(16) 1.07723(13) 0.0333(5) Uani 1 1 d . . . C53 C 0.35190(17) 1.04671(16) 1.03584(13) 0.0323(5) Uani 1 1 d . . . C54 C 0.32881(19) 0.96323(16) 1.07042(14) 0.0350(6) Uani 1 1 d . . . H54A H 0.3502 0.9351 1.1178 0.053 Uiso 1 1 calc R . . H54B H 0.3622 0.9247 1.0436 0.053 Uiso 1 1 calc R . . H54C H 0.2590 0.9755 1.0724 0.053 Uiso 1 1 calc R . . C55 C 0.4372(2) 1.17894(18) 0.85276(14) 0.0403(6) Uani 1 1 d . . . H55D H 0.4133 1.2421 0.8311 0.060 Uiso 1 1 calc R . . H55E H 0.4095 1.1529 0.8317 0.060 Uiso 1 1 calc R . . H55F H 0.5078 1.1583 0.8455 0.060 Uiso 1 1 calc R . . C56 C 0.35070(18) 1.22979(16) 1.08998(13) 0.0325(5) Uani 1 1 d . . . H56A H 0.2851 1.2712 1.0871 0.049 Uiso 1 1 calc R . . H56B H 0.3975 1.2613 1.0709 0.049 Uiso 1 1 calc R . . H56C H 0.3619 1.1936 1.1387 0.049 Uiso 1 1 calc R . . C57 C 0.41842(19) 1.28726(16) 0.93814(14) 0.0381(6) Uani 1 1 d . . . H57A H 0.4485 1.2981 0.9702 0.046 Uiso 1 1 calc R . . H57B H 0.4613 1.2886 0.8950 0.046 Uiso 1 1 calc R . . C58 C 0.3211(2) 1.42798(18) 0.87199(16) 0.0514(8) Uani 1 1 d . . . C59 C 0.3937(2) 1.45609(18) 0.83351(14) 0.0455(7) Uani 1 1 d . . . H59 H 0.4577 1.4176 0.8416 0.055 Uiso 1 1 calc R . . C60 C 0.3825(2) 1.53598(17) 0.78363(14) 0.0440(7) Uani 1 1 d . . . H60 H 0.4365 1.5540 0.7598 0.053 Uiso 1 1 calc R . . C61 C 0.2896(2) 1.58934(18) 0.76927(15) 0.0496(8) Uani 1 1 d . . . C62 C 0.2194(2) 1.56379(18) 0.81126(15) 0.0493(8) Uani 1 1 d . . . H62 H 0.1551 1.6019 0.8041 0.059 Uiso 1 1 calc R . . C63 C 0.2334(2) 1.48532(17) 0.86479(14) 0.0517(9) Uani 1 1 d . . . H63 H 0.1808 1.4725 0.8961 0.062 Uiso 1 1 calc R . . C64 C 0.27146(19) 1.67533(16) 0.71266(14) 0.0346(6) Uani 1 1 d . . . C65 C 0.29868(19) 1.07152(17) 1.15024(13) 0.0381(6) Uani 1 1 d . . . H65A H 0.2635 1.1230 1.1642 0.046 Uiso 1 1 calc R . . H65B H 0.2535 1.0396 1.1568 0.046 Uiso 1 1 calc R . . C66 C 0.36466(19) 0.98383(17) 1.26283(13) 0.0353(6) Uani 1 1 d . . . C67 C 0.27321(19) 1.00446(17) 1.29991(14) 0.0367(6) Uani 1 1 d . . . H67 H 0.2178 1.0435 1.2755 0.044 Uiso 1 1 calc R . . C68 C 0.2645(2) 0.96680(17) 1.37354(14) 0.0387(6) Uani 1 1 d . . . H68 H 0.2033 0.9806 1.3983 0.046 Uiso 1 1 calc R . . C69 C 0.34730(18) 0.90852(16) 1.41009(13) 0.0311(5) Uani 1 1 d . . . C70 C 0.43875(19) 0.88789(17) 1.37302(13) 0.0349(6) Uani 1 1 d . . . H70 H 0.4941 0.8489 1.3975 0.042 Uiso 1 1 calc R . . C71 C 0.44744(19) 0.92554(16) 1.29938(13) 0.0356(6) Uani 1 1 d . . . H71 H 0.5086 0.9117 1.2746 0.043 Uiso 1 1 calc R . . C72 C 0.33598(18) 0.86625(16) 1.48913(13) 0.0332(6) Uani 1 1 d . . . Cl1 Cl 0.55660(4) 0.61676(4) 0.58179(3) 0.03115(13) Uani 1 1 d . . . Mn1 Mn 1.0000 0.5000 0.5000 0.02507(11) Uani 1 2 d S . . Mn2 Mn 0.73292(3) 0.56698(2) 0.535937(19) 0.02999(9) Uani 1 1 d . . . Mn3 Mn 0.46270(3) 0.74545(2) 0.625976(19) 0.02989(9) Uani 1 1 d . . . Mn4 Mn 0.19310(3) 0.84558(3) 0.62123(2) 0.03618(10) Uani 1 1 d . . . N1 N 0.66761(16) 0.56919(14) 0.78706(12) 0.0417(5) Uani 1 1 d . . . N2 N 0.65554(15) 0.87765(13) 0.47703(11) 0.0330(5) Uani 1 1 d . . . O1 O 0.78591(12) 1.44161(11) -0.38753(9) 0.0360(4) Uani 1 1 d . . . O2 O 0.94531(13) 1.39842(11) -0.41675(9) 0.0397(4) Uani 1 1 d . . . O3 O 0.88951(13) 1.06368(12) -0.16475(10) 0.0464(5) Uani 1 1 d . . . O4 O 0.88216(13) 0.76223(12) -0.20721(10) 0.0409(4) Uani 1 1 d . . . O5 O 0.77701(13) 0.63741(12) -0.41945(10) 0.0395(4) Uani 1 1 d . . . O6 O 0.93878(12) 0.58436(11) -0.43332(9) 0.0334(4) Uani 1 1 d . . . O7 O 0.92863(12) 0.71713(11) 0.10997(9) 0.0353(4) Uani 1 1 d . . . O8 O 0.72308(12) 0.66369(10) 0.42225(8) 0.0307(4) Uani 1 1 d . . . O9 O 0.86155(12) 0.55334(11) 0.44552(9) 0.0334(4) Uani 1 1 d . . . O10 O 0.57201(12) 0.81624(11) 0.57692(9) 0.0322(4) Uani 1 1 d . . . O11 O 0.54106(13) 0.66494(11) 0.72475(9) 0.0359(4) Uani 1 1 d . . . O12 O 0.38691(12) 0.84254(11) 0.67600(8) 0.0317(4) Uani 1 1 d . . . O13 O 0.22717(12) 0.91087(11) 0.67529(9) 0.0347(4) Uani 1 1 d . . . O14 O 0.32101(13) 1.03804(12) 0.88974(10) 0.0398(4) Uani 1 1 d . . . O15 O 0.32378(13) 1.34934(12) 0.92322(10) 0.0511(6) Uani 1 1 d . . . O16 O 0.19106(12) 1.72965(11) 0.71292(9) 0.0332(4) Uani 1 1 d . . . O17 O 0.33310(12) 1.69578(11) 0.66791(8) 0.0318(4) Uani 1 1 d . . . O18 O 0.38032(12) 1.01597(11) 1.19231(9) 0.0351(4) Uani 1 1 d . . . O19 O 0.25451(13) 0.89085(11) 1.51827(9) 0.0377(4) Uani 1 1 d . . . O20 O 0.41067(12) 0.81471(11) 1.51858(9) 0.0325(4) Uani 1 1 d . . . O1W O 0.68269(13) 0.49324(11) 0.49410(9) 0.0341(4) Uani 1 1 d . . . O2W O 0.04136(14) 0.91632(14) 0.59356(11) 0.0492(5) Uani 1 1 d . . . O3W O 0.9809(4) 0.8192(4) 0.4546(3) 0.0291(12) Uani 0.30 1 d P . . O4W O 0.4075(3) 0.5920(3) 0.2909(2) 0.0333(9) Uani 0.40 1 d P . . O5W O 0.2951(4) 0.6532(4) 0.5033(3) 0.0372(14) Uani 0.30 1 d P . . O6W O 0.6881(2) 0.4546(2) 0.97888(17) 0.0342(8) Uani 0.50 1 d P . . O7W O 0.6102(3) 0.2993(2) 0.9529(2) 0.0466(10) Uani 0.50 1 d P . . O8W O 0.1733(5) 0.7862(4) 0.9818(3) 0.0441(15) Uani 0.30 1 d P . . O9W O 0.6571(3) 0.5140(3) 0.3568(2) 0.0431(11) Uani 0.40 1 d P . . O10W O 0.8228(4) 0.2199(4) 0.1080(3) 0.0318(12) Uani 0.30 1 d P . . O11W O 0.5929(3) 0.3547(2) 0.98316(19) 0.0395(9) Uani 0.50 1 d P . . O12W O 0.3857(3) 0.7471(2) 0.35585(18) 0.0332(8) Uani 0.50 1 d P . . O13W O 0.9479(3) 0.4721(2) 0.98286(18) 0.0338(8) Uani 0.50 1 d P . . O14W O 0.0641(3) 0.5948(3) 0.1215(2) 0.0492(10) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0337(14) 0.0351(14) 0.0310(13) -0.0001(11) 0.0043(11) -0.0069(11) C2 0.0363(15) 0.0355(15) 0.0538(18) 0.0066(13) 0.0111(13) -0.0062(12) C3 0.0327(14) 0.0400(15) 0.0352(14) 0.0124(12) -0.0070(11) -0.0113(11) C4 0.0371(15) 0.0389(15) 0.0406(16) 0.0125(12) -0.0084(12) -0.0137(12) C5 0.0391(15) 0.0336(14) 0.0353(14) 0.0121(12) 0.0017(12) -0.0125(11) C6 0.0380(14) 0.0316(13) 0.0412(15) 0.0089(12) 0.0018(12) -0.0166(11) C7 0.0346(14) 0.0340(13) 0.0340(14) 0.0020(11) -0.0011(11) -0.0165(11) C8 0.0361(14) 0.0286(12) 0.0320(13) 0.0027(11) -0.0121(11) -0.0063(10) C9 0.0374(14) 0.0265(12) 0.0305(13) -0.0065(10) -0.0029(11) -0.0053(10) C10 0.0286(12) 0.0322(12) 0.0282(12) -0.0068(10) -0.0088(10) -0.0135(10) C11 0.0255(12) 0.0330(13) 0.0315(13) -0.0112(11) 0.0016(10) -0.0092(10) C12 0.0277(12) 0.0401(13) 0.0372(14) -0.0160(11) -0.0037(10) -0.0192(10) C13 0.0233(11) 0.0346(13) 0.0352(13) -0.0128(11) -0.0044(10) -0.0091(10) C14 0.0319(13) 0.0403(14) 0.0278(13) -0.0094(11) -0.0055(10) -0.0128(11) C15 0.0338(14) 0.0395(14) 0.0312(13) -0.0111(11) 0.0053(11) -0.0104(11) C16 0.0398(15) 0.0399(14) 0.0389(15) -0.0155(12) -0.0150(12) 0.0008(12) C17 0.0419(15) 0.0385(14) 0.0353(14) -0.0127(12) -0.0100(12) -0.0094(12) C18 0.0339(13) 0.0359(13) 0.0322(13) -0.0157(11) -0.0019(10) -0.0123(11) C19 0.0372(14) 0.0388(14) 0.0369(14) -0.0157(12) -0.0111(12) 0.0039(11) C20 0.0326(13) 0.0409(14) 0.0282(13) -0.0147(11) -0.0033(10) -0.0004(11) C21 0.0375(14) 0.0391(14) 0.0288(13) -0.0129(11) -0.0004(11) -0.0081(11) C22 0.0323(13) 0.0330(13) 0.0329(13) -0.0129(11) -0.0044(11) -0.0048(10) C23 0.0398(15) 0.0412(15) 0.0397(15) -0.0174(13) -0.0150(12) 0.0020(12) C24 0.0330(14) 0.0385(14) 0.0375(14) -0.0148(12) -0.0162(11) 0.0109(11) C25 0.0383(14) 0.0389(14) 0.0306(13) -0.0168(11) -0.0090(11) -0.0046(11) C26 0.0369(14) 0.0391(14) 0.0235(12) -0.0005(11) -0.0076(10) -0.0129(11) C27 0.0349(13) 0.0324(13) 0.0261(12) -0.0023(10) -0.0055(10) -0.0103(10) C28 0.0406(15) 0.0382(15) 0.0262(13) 0.0020(11) -0.0085(11) 0.0081(12) C29 0.0337(14) 0.0408(15) 0.0313(14) -0.0044(12) -0.0060(11) 0.0034(11) C30 0.0341(13) 0.0310(12) 0.0241(12) -0.0044(10) -0.0064(10) -0.0025(10) C31 0.0370(14) 0.0284(12) 0.0273(12) -0.0047(10) -0.0081(11) 0.0023(10) C32 0.0471(16) 0.0385(14) 0.0289(13) -0.0136(12) -0.0074(12) 0.0052(12) C33 0.0317(13) 0.0317(12) 0.0268(12) -0.0050(10) -0.0024(10) -0.0101(10) C34 0.0367(14) 0.0397(14) 0.0360(14) -0.0174(12) 0.0125(11) -0.0141(11) C35 0.0372(14) 0.0369(14) 0.0401(15) -0.0178(12) 0.0203(12) -0.0155(11) C36 0.0313(13) 0.0340(13) 0.0323(13) -0.0114(11) -0.0019(10) -0.0144(10) C37 0.0339(14) 0.0384(14) 0.0375(14) 0.0012(12) -0.0177(11) -0.0096(11) C38 0.0309(13) 0.0360(13) 0.0398(14) -0.0127(11) -0.0145(11) -0.0156(10) C39 0.0393(15) 0.0381(15) 0.0356(15) 0.0065(12) -0.0147(12) 0.0134(12) C40 0.0309(13) 0.0351(13) 0.0364(14) -0.0143(11) 0.0064(11) -0.0105(10) C41 0.0359(14) 0.0336(13) 0.0353(14) -0.0142(11) 0.0068(11) -0.0131(11) C42 0.0352(13) 0.0326(13) 0.0361(14) -0.0154(11) 0.0029(11) -0.0130(11) C43 0.0380(14) 0.0314(13) 0.0328(13) -0.0125(11) -0.0169(11) 0.0091(11) C44 0.0305(13) 0.0361(13) 0.0363(14) -0.0129(12) -0.0027(11) -0.0029(10) C45 0.0323(13) 0.0346(13) 0.0336(14) -0.0104(11) -0.0069(11) 0.0044(11) C46 0.0389(15) 0.0367(14) 0.0334(14) -0.0126(12) -0.0001(11) 0.0008(11) C47 0.0357(14) 0.0338(13) 0.0365(14) -0.0131(12) -0.0177(11) 0.0147(11) C48 0.0219(11) 0.0326(13) 0.0285(12) -0.0080(11) -0.0021(10) 0.0005(10) C49 0.0395(15) 0.0312(13) 0.0328(14) -0.0021(11) -0.0032(11) -0.0024(11) C50 0.0339(14) 0.0355(14) 0.0369(14) -0.0044(12) -0.0055(11) -0.0071(11) C51 0.0291(13) 0.0334(13) 0.0366(14) -0.0130(11) -0.0063(11) -0.0053(10) C52 0.0307(13) 0.0331(13) 0.0295(13) -0.0088(11) -0.0057(10) -0.0034(10) C53 0.0269(12) 0.0300(12) 0.0301(13) -0.0057(10) -0.0056(10) -0.0016(10) C54 0.0354(14) 0.0361(13) 0.0373(14) -0.0146(11) 0.0020(11) -0.0160(11) C55 0.0365(14) 0.0371(14) 0.0325(14) 0.0016(11) 0.0011(11) -0.0123(11) C56 0.0350(13) 0.0392(14) 0.0333(13) -0.0107(11) -0.0122(11) -0.0197(11) C57 0.0355(14) 0.0349(13) 0.0326(14) 0.0037(11) -0.0183(11) -0.0070(11) C58 0.0353(15) 0.0335(14) 0.0426(16) 0.0122(12) 0.0120(12) 0.0003(11) C59 0.0367(15) 0.0401(15) 0.0349(15) 0.0067(12) 0.0083(12) -0.0122(12) C60 0.0386(15) 0.0368(14) 0.0349(15) 0.0041(12) 0.0071(12) -0.0115(12) C61 0.0413(16) 0.0358(15) 0.0393(16) 0.0062(12) 0.0123(13) -0.0062(12) C62 0.0347(15) 0.0405(15) 0.0389(15) 0.0145(13) -0.0036(12) -0.0053(12) C63 0.0347(14) 0.0347(14) 0.0317(14) 0.0120(12) 0.0141(12) 0.0135(11) C64 0.0316(14) 0.0316(13) 0.0367(14) -0.0078(11) -0.0039(11) -0.0099(11) C65 0.0352(14) 0.0316(13) 0.0309(13) -0.0073(11) -0.0028(11) 0.0035(11) C66 0.0342(13) 0.0368(14) 0.0262(12) -0.0055(11) -0.0002(10) -0.0091(11) C67 0.0304(13) 0.0394(14) 0.0313(13) -0.0114(11) -0.0032(11) -0.0019(11) C68 0.0354(14) 0.0355(14) 0.0323(14) -0.0087(11) 0.0043(11) -0.0044(11) C69 0.0354(13) 0.0330(13) 0.0254(12) -0.0100(10) 0.0007(10) -0.0131(10) C70 0.0348(14) 0.0385(14) 0.0258(12) -0.0034(11) 0.0002(10) -0.0152(11) C71 0.0329(13) 0.0324(13) 0.0250(12) -0.0016(10) -0.0008(10) -0.0022(10) C72 0.0307(13) 0.0308(13) 0.0303(13) -0.0074(11) 0.0046(11) -0.0086(10) Cl1 0.0355(3) 0.0324(3) 0.0222(3) -0.0095(2) -0.0032(2) -0.0067(2) Mn1 0.0306(3) 0.0200(2) 0.0184(2) -0.00472(19) -0.0010(2) -0.00381(19) Mn2 0.0350(2) 0.03138(19) 0.01990(17) -0.00846(15) -0.00345(15) -0.00639(15) Mn3 0.0351(2) 0.03131(19) 0.01996(17) -0.00865(15) -0.00313(15) -0.00676(15) Mn4 0.0356(2) 0.0358(2) 0.0337(2) -0.00487(17) 0.00144(17) -0.01753(17) N1 0.0382(12) 0.0336(11) 0.0392(13) -0.0043(10) -0.0182(10) 0.0032(9) N2 0.0354(11) 0.0337(11) 0.0307(11) -0.0110(9) -0.0016(9) -0.0127(9) O1 0.0306(9) 0.0373(9) 0.0340(9) -0.0077(8) -0.0047(7) -0.0081(7) O2 0.0341(10) 0.0366(10) 0.0353(10) 0.0047(8) -0.0017(8) -0.0161(8) O3 0.0314(9) 0.0348(10) 0.0389(10) 0.0115(8) 0.0076(8) -0.0050(8) O4 0.0372(10) 0.0379(10) 0.0388(10) -0.0139(8) -0.0161(8) 0.0053(8) O5 0.0397(10) 0.0388(10) 0.0395(10) -0.0149(8) -0.0069(8) -0.0085(8) O6 0.0367(9) 0.0352(9) 0.0320(9) -0.0172(8) -0.0040(7) -0.0089(7) O7 0.0304(9) 0.0351(9) 0.0300(9) -0.0089(8) -0.0064(7) 0.0003(7) O8 0.0366(9) 0.0309(9) 0.0219(8) -0.0093(7) -0.0032(7) -0.0070(7) O9 0.0301(9) 0.0356(9) 0.0266(9) -0.0053(7) -0.0016(7) -0.0081(7) O10 0.0345(9) 0.0384(9) 0.0321(9) -0.0180(8) -0.0003(7) -0.0158(8) O11 0.0378(10) 0.0367(9) 0.0327(9) -0.0106(8) -0.0182(8) -0.0045(8) O12 0.0364(9) 0.0329(9) 0.0225(8) -0.0101(7) -0.0032(7) -0.0065(7) O13 0.0362(9) 0.0324(9) 0.0321(9) -0.0032(8) 0.0015(7) -0.0180(8) O14 0.0343(10) 0.0405(10) 0.0354(10) -0.0135(8) -0.0082(8) 0.0013(8) O15 0.0343(10) 0.0364(10) 0.0371(10) 0.0127(8) 0.0161(8) 0.0008(8) O16 0.0342(10) 0.0363(9) 0.0255(9) -0.0039(7) 0.0002(7) -0.0158(8) O17 0.0357(9) 0.0330(9) 0.0212(8) -0.0084(7) -0.0038(7) -0.0053(7) O18 0.0359(9) 0.0331(9) 0.0270(9) -0.0034(7) -0.0051(7) -0.0070(7) O19 0.0346(10) 0.0346(9) 0.0360(10) -0.0112(8) 0.0171(8) -0.0142(8) O20 0.0344(9) 0.0375(9) 0.0251(8) -0.0091(7) -0.0034(7) -0.0122(8) O1W 0.0406(10) 0.0345(9) 0.0325(9) -0.0139(8) 0.0005(8) -0.0173(8) O2W 0.0339(10) 0.0654(13) 0.0421(11) -0.0196(10) -0.0112(9) -0.0037(9) O3W 0.033(3) 0.035(3) 0.032(3) -0.019(2) -0.003(2) -0.017(2) O4W 0.034(2) 0.036(2) 0.024(2) -0.0055(18) -0.0037(18) -0.0104(19) O5W 0.032(3) 0.031(3) 0.038(3) -0.006(3) 0.006(3) -0.010(2) O6W 0.0348(19) 0.0378(19) 0.0252(17) -0.0028(15) 0.0001(14) -0.0163(15) O7W 0.041(2) 0.0314(19) 0.038(2) 0.0001(17) 0.0133(17) -0.0024(16) O8W 0.040(3) 0.041(3) 0.045(4) -0.016(3) -0.007(3) -0.002(3) O9W 0.039(3) 0.042(3) 0.039(3) -0.012(2) -0.009(2) -0.002(2) O10W 0.039(3) 0.031(3) 0.024(3) -0.010(2) -0.005(2) -0.008(2) O11W 0.0347(19) 0.043(2) 0.036(2) -0.0055(17) -0.0205(16) -0.0071(16) O12W 0.040(2) 0.0337(18) 0.0318(18) -0.0121(15) -0.0027(15) -0.0171(15) O13W 0.042(2) 0.0334(18) 0.0319(18) -0.0122(15) -0.0034(15) -0.0176(16) O14W 0.033(2) 0.066(3) 0.044(2) -0.021(2) -0.0152(17) -0.0024(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.212(2) . ? C1 O1 1.252(3) . ? C1 C2 1.484(4) . ? C2 C3 1.390(4) . ? C2 C7 1.390(4) . ? C3 C4 1.390(3) . ? C3 H3 0.9300 . ? C4 C5 1.390(4) . ? C4 H4 0.9300 . ? C5 O3 1.324(2) . ? C5 C6 1.390(4) . ? C6 C7 1.390(3) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.407(2) . ? C8 C9 1.492(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.367(3) . ? C9 C10 1.388(3) . ? C10 C11 1.365(3) . ? C10 C17 1.519(3) . ? C11 C12 1.411(3) . ? C11 C26 1.477(3) . ? C12 C13 1.381(3) . ? C12 C18 1.476(3) . ? C13 C14 1.390(3) . ? C13 C16 1.516(3) . ? C14 C15 1.543(3) . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C15 H15A 0.9600 . ? C16 O4 1.409(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O4 1.359(3) . ? C19 C20 1.375(4) . ? C19 C24 1.380(3) . ? C20 C21 1.373(4) . ? C20 H20 0.9300 . ? C21 C22 1.378(3) . ? C21 H21 0.9300 . ? C22 C23 1.369(4) . ? C22 C25 1.484(3) . ? C23 C24 1.380(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O6 1.214(3) . ? C25 O5 1.254(3) . ? C26 O7 1.405(2) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O7 1.360(2) . ? C27 C32 1.374(3) . ? C27 C28 1.453(4) . ? C28 C29 1.328(4) . ? C28 H28 0.9300 . ? C29 C30 1.377(3) . ? C29 H29 0.9300 . ? C30 C31 1.380(3) . ? C30 C33 1.485(3) . ? C31 C32 1.378(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O8 1.241(2) . ? C33 O9 1.272(2) . ? C34 N2 1.439(2) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 N2 1.440(2) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O10 1.213(2) . ? C36 N2 1.320(2) . ? C36 H36 0.9300 . ? C37 O11 1.166(3) . ? C37 N1 1.322(2) . ? C37 H37 0.9300 . ? C38 N1 1.459(2) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N1 1.376(2) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 O12 1.221(2) . ? C40 O13 1.240(3) . ? C40 C41 1.480(4) . ? C41 C46 1.366(4) . ? C41 C42 1.392(3) . ? C42 C43 1.378(3) . ? C42 H42 0.9300 . ? C43 C44 1.356(4) . ? C43 H43 0.9300 . ? C44 O14 1.344(3) . ? C44 C45 1.381(3) . ? C45 C46 1.397(4) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 O14 1.440(3) . ? C47 C48 1.476(3) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.383(4) . ? C48 C53 1.406(2) . ? C49 C50 1.320(4) . ? C49 C55 1.551(3) . ? C50 C51 1.450(3) . ? C50 C57 1.531(3) . ? C51 C52 1.346(4) . ? C51 C56 1.509(3) . ? C52 C53 1.393(3) . ? C52 C65 1.437(3) . ? C53 C54 1.476(3) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55D 0.9600 . ? C55 H55E 0.9600 . ? C55 H55F 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 O15 1.410(3) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C63 1.295(4) . ? C58 C59 1.314(4) . ? C58 O15 1.350(3) . ? C59 C60 1.336(4) . ? C59 H59 0.9300 . ? C60 C61 1.348(4) . ? C60 H60 0.9300 . ? C61 C62 1.290(4) . ? C61 C64 1.457(4) . ? C62 C63 1.348(3) . ? C62 H62 0.9300 . ? C63 H63 0.9300 . ? C64 O17 1.192(3) . ? C64 O16 1.205(3) . ? C65 O18 1.425(3) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 O18 1.334(3) . ? C66 C67 1.390(3) . ? C66 C71 1.390(3) . ? C67 C68 1.390(4) . ? C67 H67 0.9300 . ? C68 C69 1.390(4) . ? C68 H68 0.9300 . ? C69 C70 1.390(3) . ? C69 C72 1.496(3) . ? C70 C71 1.390(3) . ? C70 H70 0.9300 . ? C71 H71 0.9300 . ? C72 O19 1.219(3) . ? C72 O20 1.220(3) . ? Cl1 Mn2 2.5033(7) . ? Cl1 Mn3 2.5465(7) . ? Mn1 O2 2.1878(16) 1_546 ? Mn1 O2 2.1878(16) 2_775 ? Mn1 O6 2.2137(16) 2_765 ? Mn1 O6 2.2137(16) 1_556 ? Mn1 O9 2.2292(17) 2_766 ? Mn1 O9 2.2292(17) . ? Mn2 O1 2.0931(17) 1_546 ? Mn2 O5 2.1137(18) 1_556 ? Mn2 O1W 2.1796(17) . ? Mn2 O8 2.2737(16) . ? Mn2 O9 2.3654(17) . ? Mn3 O12 2.1481(16) . ? Mn3 O20 2.1972(17) 1_554 ? Mn3 O10 2.2164(17) . ? Mn3 O11 2.2230(16) . ? Mn3 O17 2.2464(18) 1_545 ? Mn4 O19 2.0773(17) 1_554 ? Mn4 O13 2.0994(18) . ? Mn4 O16 2.1548(16) 1_545 ? Mn4 O2W 2.1747(19) . ? O1 Mn2 2.0931(17) 1_564 ? O2 Mn1 2.1878(16) 1_564 ? O5 Mn2 2.1137(18) 1_554 ? O6 Mn1 2.2137(16) 1_554 ? O16 Mn4 2.1548(16) 1_565 ? O17 Mn3 2.2464(18) 1_565 ? O19 Mn4 2.0773(17) 1_556 ? O20 Mn3 2.1972(17) 1_556 ? O7W O11W 1.263(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 O2 C1 O1 126.5(2) . . ? O2 C1 C2 119.7(2) . . ? O1 C1 C2 113.7(2) . . ? C3 C2 C7 120.0(2) . . ? C3 C2 C1 120.3(3) . . ? C7 C2 C1 119.6(2) . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? O3 C5 C6 125.7(2) . . ? O3 C5 C4 114.3(2) . . ? C6 C5 C4 120.0(2) . . ? C5 C6 C7 120.0(3) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.0(2) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? O3 C8 C9 105.55(19) . . ? O3 C8 H8A 110.6 . . ? C9 C8 H8A 110.6 . . ? O3 C8 H8B 110.6 . . ? C9 C8 H8B 110.6 . . ? H8A C8 H8B 108.8 . . ? C14 C9 C10 121.5(2) . . ? C14 C9 C8 116.1(2) . . ? C10 C9 C8 122.4(2) . . ? C11 C10 C9 120.1(2) . . ? C11 C10 C17 118.7(2) . . ? C9 C10 C17 121.2(2) . . ? C10 C11 C12 119.6(2) . . ? C10 C11 C26 119.7(2) . . ? C12 C11 C26 120.7(2) . . ? C13 C12 C11 118.7(2) . . ? C13 C12 C18 123.6(2) . . ? C11 C12 C18 117.7(2) . . ? C12 C13 C14 121.6(2) . . ? C12 C13 C16 121.2(2) . . ? C14 C13 C16 117.2(2) . . ? C9 C14 C13 118.2(2) . . ? C9 C14 C15 122.2(2) . . ? C13 C14 C15 119.6(2) . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? O4 C16 C13 105.90(18) . . ? O4 C16 H16A 110.6 . . ? C13 C16 H16A 110.6 . . ? O4 C16 H16B 110.6 . . ? C13 C16 H16B 110.6 . . ? H16A C16 H16B 108.7 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C20 116.6(2) . . ? O4 C19 C24 123.7(2) . . ? C20 C19 C24 119.7(3) . . ? C21 C20 C19 120.0(2) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.5(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 119.5(2) . . ? C23 C22 C25 118.7(2) . . ? C21 C22 C25 121.7(2) . . ? C22 C23 C24 120.3(2) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 119.9(3) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? O6 C25 O5 126.3(2) . . ? O6 C25 C22 119.0(2) . . ? O5 C25 C22 114.6(2) . . ? O7 C26 C11 112.13(19) . . ? O7 C26 H26A 109.2 . . ? C11 C26 H26A 109.2 . . ? O7 C26 H26B 109.2 . . ? C11 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? O7 C27 C32 116.7(2) . . ? O7 C27 C28 125.0(2) . . ? C32 C27 C28 118.3(2) . . ? C29 C28 C27 119.1(2) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C30 123.6(3) . . ? C28 C29 H29 118.2 . . ? C30 C29 H29 118.2 . . ? C29 C30 C31 116.7(2) . . ? C29 C30 C33 119.7(2) . . ? C31 C30 C33 123.6(2) . . ? C32 C31 C30 123.1(2) . . ? C32 C31 H31 118.5 . . ? C30 C31 H31 118.5 . . ? C27 C32 C31 119.1(2) . . ? C27 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? O8 C33 O9 121.65(19) . . ? O8 C33 C30 119.8(2) . . ? O9 C33 C30 118.3(2) . . ? N2 C34 H34A 109.5 . . ? N2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C35 H35A 109.5 . . ? N2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O10 C36 N2 124.8(2) . . ? O10 C36 H36 117.6 . . ? N2 C36 H36 117.6 . . ? O11 C37 N1 125.0(3) . . ? O11 C37 H37 117.5 . . ? N1 C37 H37 117.5 . . ? N1 C38 H38A 109.5 . . ? N1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N1 C39 H39A 109.5 . . ? N1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O12 C40 O13 126.4(2) . . ? O12 C40 C41 116.2(2) . . ? O13 C40 C41 117.4(2) . . ? C46 C41 C42 119.5(2) . . ? C46 C41 C40 121.7(2) . . ? C42 C41 C40 118.8(2) . . ? C43 C42 C41 120.5(3) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C44 C43 C42 119.9(2) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? O14 C44 C43 116.2(2) . . ? O14 C44 C45 123.2(2) . . ? C43 C44 C45 120.6(3) . . ? C44 C45 C46 119.7(3) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C41 C46 C45 119.8(2) . . ? C41 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? O14 C47 C48 107.26(17) . . ? O14 C47 H47A 110.3 . . ? C48 C47 H47A 110.3 . . ? O14 C47 H47B 110.3 . . ? C48 C47 H47B 110.3 . . ? H47A C47 H47B 108.5 . . ? C49 C48 C53 119.0(2) . . ? C49 C48 C47 117.8(2) . . ? C53 C48 C47 123.2(2) . . ? C50 C49 C48 119.5(2) . . ? C50 C49 C55 125.2(2) . . ? C48 C49 C55 115.3(2) . . ? C49 C50 C51 121.6(2) . . ? C49 C50 C57 118.5(2) . . ? C51 C50 C57 119.78(19) . . ? C52 C51 C50 119.8(2) . . ? C52 C51 C56 120.9(2) . . ? C50 C51 C56 119.23(19) . . ? C51 C52 C53 117.9(2) . . ? C51 C52 C65 120.8(2) . . ? C53 C52 C65 121.2(2) . . ? C52 C53 C48 121.7(2) . . ? C52 C53 C54 117.2(2) . . ? C48 C53 C54 121.1(2) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C49 C55 H55D 109.5 . . ? C49 C55 H55E 109.5 . . ? H55D C55 H55E 109.5 . . ? C49 C55 H55F 109.5 . . ? H55D C55 H55F 109.5 . . ? H55E C55 H55F 109.5 . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O15 C57 C50 102.77(18) . . ? O15 C57 H57A 111.2 . . ? C50 C57 H57A 111.2 . . ? O15 C57 H57B 111.2 . . ? C50 C57 H57B 111.2 . . ? H57A C57 H57B 109.1 . . ? C63 C58 C59 116.6(3) . . ? C63 C58 O15 113.4(2) . . ? C59 C58 O15 129.8(3) . . ? C58 C59 C60 124.8(3) . . ? C58 C59 H59 117.6 . . ? C60 C59 H59 117.6 . . ? C59 C60 C61 117.2(3) . . ? C59 C60 H60 121.4 . . ? C61 C60 H60 121.4 . . ? C62 C61 C60 117.0(3) . . ? C62 C61 C64 122.4(3) . . ? C60 C61 C64 120.4(2) . . ? C61 C62 C63 124.1(3) . . ? C61 C62 H62 117.9 . . ? C63 C62 H62 117.9 . . ? C58 C63 C62 119.1(3) . . ? C58 C63 H63 120.4 . . ? C62 C63 H63 120.4 . . ? O17 C64 O16 118.4(2) . . ? O17 C64 C61 123.4(2) . . ? O16 C64 C61 118.1(2) . . ? O18 C65 C52 107.7(2) . . ? O18 C65 H65A 110.2 . . ? C52 C65 H65A 110.2 . . ? O18 C65 H65B 110.2 . . ? C52 C65 H65B 110.2 . . ? H65A C65 H65B 108.5 . . ? O18 C66 C67 124.4(2) . . ? O18 C66 C71 115.6(2) . . ? C67 C66 C71 120.0(2) . . ? C66 C67 C68 120.0(2) . . ? C66 C67 H67 120.0 . . ? C68 C67 H67 120.0 . . ? C69 C68 C67 120.0(2) . . ? C69 C68 H68 120.0 . . ? C67 C68 H68 120.0 . . ? C68 C69 C70 120.0(2) . . ? C68 C69 C72 119.2(2) . . ? C70 C69 C72 120.7(2) . . ? C71 C70 C69 120.0(2) . . ? C71 C70 H70 120.0 . . ? C69 C70 H70 120.0 . . ? C70 C71 C66 120.0(2) . . ? C70 C71 H71 120.0 . . ? C66 C71 H71 120.0 . . ? O19 C72 O20 126.2(2) . . ? O19 C72 C69 116.9(2) . . ? O20 C72 C69 116.7(2) . . ? Mn2 Cl1 Mn3 130.22(3) . . ? O2 Mn1 O2 180.00(8) 1_546 2_775 ? O2 Mn1 O6 91.25(7) 1_546 2_765 ? O2 Mn1 O6 88.75(7) 2_775 2_765 ? O2 Mn1 O6 88.75(7) 1_546 1_556 ? O2 Mn1 O6 91.25(7) 2_775 1_556 ? O6 Mn1 O6 180.00(6) 2_765 1_556 ? O2 Mn1 O9 89.94(6) 1_546 2_766 ? O2 Mn1 O9 90.06(6) 2_775 2_766 ? O6 Mn1 O9 93.32(6) 2_765 2_766 ? O6 Mn1 O9 86.68(6) 1_556 2_766 ? O2 Mn1 O9 90.06(6) 1_546 . ? O2 Mn1 O9 89.94(6) 2_775 . ? O6 Mn1 O9 86.68(6) 2_765 . ? O6 Mn1 O9 93.32(6) 1_556 . ? O9 Mn1 O9 180.000(1) 2_766 . ? O1 Mn2 O5 97.26(7) 1_546 1_556 ? O1 Mn2 O1W 81.73(7) 1_546 . ? O5 Mn2 O1W 177.40(7) 1_556 . ? O1 Mn2 O8 152.75(7) 1_546 . ? O5 Mn2 O8 98.33(7) 1_556 . ? O1W Mn2 O8 83.52(6) . . ? O1 Mn2 O9 98.96(6) 1_546 . ? O5 Mn2 O9 99.57(7) 1_556 . ? O1W Mn2 O9 82.97(6) . . ? O8 Mn2 O9 56.42(6) . . ? O1 Mn2 Cl1 101.43(5) 1_546 . ? O5 Mn2 Cl1 93.58(5) 1_556 . ? O1W Mn2 Cl1 84.29(5) . . ? O8 Mn2 Cl1 99.76(5) . . ? O9 Mn2 Cl1 154.08(5) . . ? O12 Mn3 O20 102.05(6) . 1_554 ? O12 Mn3 O10 87.98(6) . . ? O20 Mn3 O10 81.45(6) 1_554 . ? O12 Mn3 O11 86.43(6) . . ? O20 Mn3 O11 169.62(7) 1_554 . ? O10 Mn3 O11 92.98(7) . . ? O12 Mn3 O17 86.26(6) . 1_545 ? O20 Mn3 O17 92.28(6) 1_554 1_545 ? O10 Mn3 O17 170.43(6) . 1_545 ? O11 Mn3 O17 94.28(6) . 1_545 ? O12 Mn3 Cl1 173.05(5) . . ? O20 Mn3 Cl1 84.65(5) 1_554 . ? O10 Mn3 Cl1 94.92(5) . . ? O11 Mn3 Cl1 87.12(5) . . ? O17 Mn3 Cl1 91.65(5) 1_545 . ? O19 Mn4 O13 104.40(7) 1_554 . ? O19 Mn4 O16 144.62(7) 1_554 1_545 ? O13 Mn4 O16 95.68(7) . 1_545 ? O19 Mn4 O2W 94.95(8) 1_554 . ? O13 Mn4 O2W 107.27(7) . . ? O16 Mn4 O2W 106.64(7) 1_545 . ? C37 N1 C39 121.08(18) . . ? C37 N1 C38 116.34(16) . . ? C39 N1 C38 122.35(16) . . ? C36 N2 C34 123.16(15) . . ? C36 N2 C35 116.32(14) . . ? C34 N2 C35 119.93(14) . . ? C1 O1 Mn2 130.32(11) . 1_564 ? C1 O2 Mn1 141.84(12) . 1_564 ? C5 O3 C8 117.64(16) . . ? C19 O4 C16 117.58(15) . . ? C25 O5 Mn2 127.00(12) . 1_554 ? C25 O6 Mn1 143.73(12) . 1_554 ? C27 O7 C26 117.23(15) . . ? C33 O8 Mn2 93.43(11) . . ? C33 O9 Mn1 143.76(12) . . ? C33 O9 Mn2 88.41(11) . . ? Mn1 O9 Mn2 105.02(7) . . ? C36 O10 Mn3 121.88(11) . . ? C37 O11 Mn3 126.32(14) . . ? C40 O12 Mn3 149.55(12) . . ? C40 O13 Mn4 123.78(12) . . ? C44 O14 C47 118.23(15) . . ? C58 O15 C57 115.8(2) . . ? C64 O16 Mn4 106.90(16) . 1_565 ? C64 O17 Mn3 153.44(17) . 1_565 ? C66 O18 C65 119.4(2) . . ? C72 O19 Mn4 133.23(17) . 1_556 ? C72 O20 Mn3 139.67(16) . 1_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -161.9(3) . . . . ? O1 C1 C2 C3 16.3(4) . . . . ? O2 C1 C2 C7 14.7(5) . . . . ? O1 C1 C2 C7 -167.0(3) . . . . ? C7 C2 C3 C4 0.0(5) . . . . ? C1 C2 C3 C4 176.7(3) . . . . ? C2 C3 C4 C5 0.0(5) . . . . ? C3 C4 C5 O3 -178.8(3) . . . . ? C3 C4 C5 C6 0.0(5) . . . . ? O3 C5 C6 C7 178.7(3) . . . . ? C4 C5 C6 C7 0.0(5) . . . . ? C5 C6 C7 C2 0.0(5) . . . . ? C3 C2 C7 C6 0.0(5) . . . . ? C1 C2 C7 C6 -176.7(3) . . . . ? O3 C8 C9 C14 93.7(3) . . . . ? O3 C8 C9 C10 -87.2(3) . . . . ? C14 C9 C10 C11 -2.0(4) . . . . ? C8 C9 C10 C11 178.9(2) . . . . ? C14 C9 C10 C17 178.4(2) . . . . ? C8 C9 C10 C17 -0.7(4) . . . . ? C9 C10 C11 C12 6.3(4) . . . . ? C17 C10 C11 C12 -174.1(2) . . . . ? C9 C10 C11 C26 -170.0(2) . . . . ? C17 C10 C11 C26 9.7(3) . . . . ? C10 C11 C12 C13 -6.2(3) . . . . ? C26 C11 C12 C13 169.9(2) . . . . ? C10 C11 C12 C18 175.1(2) . . . . ? C26 C11 C12 C18 -8.7(3) . . . . ? C11 C12 C13 C14 2.0(4) . . . . ? C18 C12 C13 C14 -179.5(2) . . . . ? C11 C12 C13 C16 179.4(2) . . . . ? C18 C12 C13 C16 -2.0(4) . . . . ? C10 C9 C14 C13 -2.3(4) . . . . ? C8 C9 C14 C13 176.9(2) . . . . ? C10 C9 C14 C15 176.3(2) . . . . ? C8 C9 C14 C15 -4.5(4) . . . . ? C12 C13 C14 C9 2.2(4) . . . . ? C16 C13 C14 C9 -175.3(2) . . . . ? C12 C13 C14 C15 -176.4(2) . . . . ? C16 C13 C14 C15 6.0(3) . . . . ? C12 C13 C16 O4 93.3(3) . . . . ? C14 C13 C16 O4 -89.1(3) . . . . ? O4 C19 C20 C21 178.7(2) . . . . ? C24 C19 C20 C21 -0.9(4) . . . . ? C19 C20 C21 C22 1.4(4) . . . . ? C20 C21 C22 C23 -1.8(4) . . . . ? C20 C21 C22 C25 176.6(2) . . . . ? C21 C22 C23 C24 1.7(4) . . . . ? C25 C22 C23 C24 -176.7(3) . . . . ? C22 C23 C24 C19 -1.3(4) . . . . ? O4 C19 C24 C23 -178.8(2) . . . . ? C20 C19 C24 C23 0.8(4) . . . . ? C23 C22 C25 O6 -11.1(4) . . . . ? C21 C22 C25 O6 170.5(2) . . . . ? C23 C22 C25 O5 169.8(2) . . . . ? C21 C22 C25 O5 -8.6(4) . . . . ? C10 C11 C26 O7 -96.8(3) . . . . ? C12 C11 C26 O7 87.1(3) . . . . ? O7 C27 C28 C29 -179.6(3) . . . . ? C32 C27 C28 C29 -1.0(4) . . . . ? C27 C28 C29 C30 -1.3(5) . . . . ? C28 C29 C30 C31 2.0(5) . . . . ? C28 C29 C30 C33 -179.0(3) . . . . ? C29 C30 C31 C32 -0.5(4) . . . . ? C33 C30 C31 C32 -179.4(3) . . . . ? O7 C27 C32 C31 -178.8(2) . . . . ? C28 C27 C32 C31 2.5(4) . . . . ? C30 C31 C32 C27 -1.8(4) . . . . ? C29 C30 C33 O8 5.7(4) . . . . ? C31 C30 C33 O8 -175.4(2) . . . . ? C29 C30 C33 O9 -179.9(2) . . . . ? C31 C30 C33 O9 -1.0(4) . . . . ? O12 C40 C41 C46 -6.2(4) . . . . ? O13 C40 C41 C46 175.1(2) . . . . ? O12 C40 C41 C42 171.9(2) . . . . ? O13 C40 C41 C42 -6.8(3) . . . . ? C46 C41 C42 C43 -0.2(4) . . . . ? C40 C41 C42 C43 -178.3(2) . . . . ? C41 C42 C43 C44 -0.2(4) . . . . ? C42 C43 C44 O14 -178.2(2) . . . . ? C42 C43 C44 C45 0.0(4) . . . . ? O14 C44 C45 C46 178.8(2) . . . . ? C43 C44 C45 C46 0.7(4) . . . . ? C42 C41 C46 C45 0.9(4) . . . . ? C40 C41 C46 C45 178.9(2) . . . . ? C44 C45 C46 C41 -1.2(4) . . . . ? O14 C47 C48 C49 -92.8(3) . . . . ? O14 C47 C48 C53 85.9(2) . . . . ? C53 C48 C49 C50 7.7(4) . . . . ? C47 C48 C49 C50 -173.5(2) . . . . ? C53 C48 C49 C55 -173.46(16) . . . . ? C47 C48 C49 C55 5.3(3) . . . . ? C48 C49 C50 C51 -5.0(4) . . . . ? C55 C49 C50 C51 176.33(17) . . . . ? C48 C49 C50 C57 178.7(2) . . . . ? C55 C49 C50 C57 0.0(4) . . . . ? C49 C50 C51 C52 -1.8(3) . . . . ? C57 C50 C51 C52 174.5(2) . . . . ? C49 C50 C51 C56 -178.06(19) . . . . ? C57 C50 C51 C56 -1.8(3) . . . . ? C50 C51 C52 C53 5.4(3) . . . . ? C56 C51 C52 C53 -178.4(2) . . . . ? C50 C51 C52 C65 -177.8(2) . . . . ? C56 C51 C52 C65 -1.6(4) . . . . ? C51 C52 C53 C48 -2.5(3) . . . . ? C65 C52 C53 C48 -179.4(2) . . . . ? C51 C52 C53 C54 176.1(2) . . . . ? C65 C52 C53 C54 -0.7(3) . . . . ? C49 C48 C53 C52 -4.1(3) . . . . ? C47 C48 C53 C52 177.25(16) . . . . ? C49 C48 C53 C54 177.36(17) . . . . ? C47 C48 C53 C54 -1.3(3) . . . . ? C49 C50 C57 O15 95.8(2) . . . . ? C51 C50 C57 O15 -80.6(2) . . . . ? C63 C58 C59 C60 -6.4(6) . . . . ? O15 C58 C59 C60 179.8(3) . . . . ? C58 C59 C60 C61 -4.0(5) . . . . ? C59 C60 C61 C62 9.2(5) . . . . ? C59 C60 C61 C64 -176.3(3) . . . . ? C60 C61 C62 C63 -4.6(6) . . . . ? C64 C61 C62 C63 -179.0(3) . . . . ? C59 C58 C63 C62 11.1(6) . . . . ? O15 C58 C63 C62 -174.2(3) . . . . ? C61 C62 C63 C58 -6.0(6) . . . . ? C62 C61 C64 O17 -170.2(3) . . . . ? C60 C61 C64 O17 15.6(5) . . . . ? C62 C61 C64 O16 12.9(5) . . . . ? C60 C61 C64 O16 -161.3(3) . . . . ? C51 C52 C65 O18 -89.5(3) . . . . ? C53 C52 C65 O18 87.2(3) . . . . ? O18 C66 C67 C68 179.5(3) . . . . ? C71 C66 C67 C68 0.0(4) . . . . ? C66 C67 C68 C69 0.0(4) . . . . ? C67 C68 C69 C70 0.0(4) . . . . ? C67 C68 C69 C72 -177.9(2) . . . . ? C68 C69 C70 C71 0.0(4) . . . . ? C72 C69 C70 C71 177.9(2) . . . . ? C69 C70 C71 C66 0.0(4) . . . . ? O18 C66 C71 C70 -179.5(2) . . . . ? C67 C66 C71 C70 0.0(4) . . . . ? C68 C69 C72 O19 -5.5(4) . . . . ? C70 C69 C72 O19 176.5(2) . . . . ? C68 C69 C72 O20 179.1(2) . . . . ? C70 C69 C72 O20 1.1(4) . . . . ? Mn3 Cl1 Mn2 O1 116.36(6) . . . 1_546 ? Mn3 Cl1 Mn2 O5 18.21(6) . . . 1_556 ? Mn3 Cl1 Mn2 O1W -163.29(5) . . . . ? Mn3 Cl1 Mn2 O8 -80.88(5) . . . . ? Mn3 Cl1 Mn2 O9 -102.42(11) . . . . ? Mn2 Cl1 Mn3 O12 -97.0(4) . . . . ? Mn2 Cl1 Mn3 O20 98.39(5) . . . 1_554 ? Mn2 Cl1 Mn3 O10 17.48(6) . . . . ? Mn2 Cl1 Mn3 O11 -75.27(6) . . . . ? Mn2 Cl1 Mn3 O17 -169.48(5) . . . 1_545 ? O11 C37 N1 C39 -175.2(2) . . . . ? O11 C37 N1 C38 -0.6(3) . . . . ? O10 C36 N2 C34 -175.1(2) . . . . ? O10 C36 N2 C35 -3.9(3) . . . . ? O2 C1 O1 Mn2 1.3(4) . . . 1_564 ? C2 C1 O1 Mn2 -176.79(18) . . . 1_564 ? O1 C1 O2 Mn1 11.4(5) . . . 1_564 ? C2 C1 O2 Mn1 -170.57(17) . . . 1_564 ? C6 C5 O3 C8 -6.8(4) . . . . ? C4 C5 O3 C8 171.9(2) . . . . ? C9 C8 O3 C5 -158.7(2) . . . . ? C20 C19 O4 C16 175.4(2) . . . . ? C24 C19 O4 C16 -5.0(4) . . . . ? C13 C16 O4 C19 177.82(19) . . . . ? O6 C25 O5 Mn2 19.6(3) . . . 1_554 ? C22 C25 O5 Mn2 -161.37(14) . . . 1_554 ? O5 C25 O6 Mn1 -9.5(4) . . . 1_554 ? C22 C25 O6 Mn1 171.59(14) . . . 1_554 ? C32 C27 O7 C26 165.6(2) . . . . ? C28 C27 O7 C26 -15.8(3) . . . . ? C11 C26 O7 C27 171.80(19) . . . . ? O9 C33 O8 Mn2 -3.1(2) . . . . ? C30 C33 O8 Mn2 171.1(2) . . . . ? O1 Mn2 O8 C33 -26.57(19) 1_546 . . . ? O5 Mn2 O8 C33 97.71(12) 1_556 . . . ? O1W Mn2 O8 C33 -84.13(12) . . . . ? O9 Mn2 O8 C33 1.72(12) . . . . ? Cl1 Mn2 O8 C33 -167.17(12) . . . . ? O8 C33 O9 Mn1 -110.6(2) . . . . ? C30 C33 O9 Mn1 75.1(3) . . . . ? O8 C33 O9 Mn2 3.0(2) . . . . ? C30 C33 O9 Mn2 -171.3(2) . . . . ? O2 Mn1 O9 C33 156.93(19) 1_546 . . . ? O2 Mn1 O9 C33 -23.07(19) 2_775 . . . ? O6 Mn1 O9 C33 -111.82(19) 2_765 . . . ? O6 Mn1 O9 C33 68.18(19) 1_556 . . . ? O9 Mn1 O9 C33 0(100) 2_766 . . . ? O2 Mn1 O9 Mn2 48.42(7) 1_546 . . . ? O2 Mn1 O9 Mn2 -131.58(7) 2_775 . . . ? O6 Mn1 O9 Mn2 139.67(7) 2_765 . . . ? O6 Mn1 O9 Mn2 -40.33(7) 1_556 . . . ? O9 Mn1 O9 Mn2 0(100) 2_766 . . . ? O1 Mn2 O9 C33 165.64(11) 1_546 . . . ? O5 Mn2 O9 C33 -95.36(11) 1_556 . . . ? O1W Mn2 O9 C33 85.20(11) . . . . ? O8 Mn2 O9 C33 -1.67(11) . . . . ? Cl1 Mn2 O9 C33 24.07(17) . . . . ? O1 Mn2 O9 Mn1 -48.48(8) 1_546 . . . ? O5 Mn2 O9 Mn1 50.52(8) 1_556 . . . ? O1W Mn2 O9 Mn1 -128.91(8) . . . . ? O8 Mn2 O9 Mn1 144.22(10) . . . . ? Cl1 Mn2 O9 Mn1 169.96(6) . . . . ? N2 C36 O10 Mn3 156.74(14) . . . . ? O12 Mn3 O10 C36 -149.89(14) . . . . ? O20 Mn3 O10 C36 -47.39(14) 1_554 . . . ? O11 Mn3 O10 C36 123.79(14) . . . . ? O17 Mn3 O10 C36 -96.8(4) 1_545 . . . ? Cl1 Mn3 O10 C36 36.43(14) . . . . ? N1 C37 O11 Mn3 170.56(14) . . . . ? O12 Mn3 O11 C37 -158.50(16) . . . . ? O20 Mn3 O11 C37 -13.5(5) 1_554 . . . ? O10 Mn3 O11 C37 -70.71(16) . . . . ? O17 Mn3 O11 C37 115.52(16) 1_545 . . . ? Cl1 Mn3 O11 C37 24.08(16) . . . . ? O13 C40 O12 Mn3 -18.6(4) . . . . ? C41 C40 O12 Mn3 162.82(18) . . . . ? O20 Mn3 O12 C40 61.2(2) 1_554 . . . ? O10 Mn3 O12 C40 142.0(2) . . . . ? O11 Mn3 O12 C40 -124.8(2) . . . . ? O17 Mn3 O12 C40 -30.3(2) 1_545 . . . ? Cl1 Mn3 O12 C40 -103.0(4) . . . . ? O12 C40 O13 Mn4 16.5(3) . . . . ? C41 C40 O13 Mn4 -164.90(14) . . . . ? O19 Mn4 O13 C40 -76.76(14) 1_554 . . . ? O16 Mn4 O13 C40 73.87(14) 1_545 . . . ? O2W Mn4 O13 C40 -176.73(14) . . . . ? C43 C44 O14 C47 -176.9(2) . . . . ? C45 C44 O14 C47 4.9(3) . . . . ? C48 C47 O14 C44 175.36(19) . . . . ? C63 C58 O15 C57 -174.1(3) . . . . ? C59 C58 O15 C57 -0.1(5) . . . . ? C50 C57 O15 C58 -158.7(2) . . . . ? O17 C64 O16 Mn4 3.7(3) . . . 1_565 ? C61 C64 O16 Mn4 -179.3(2) . . . 1_565 ? O16 C64 O17 Mn3 94.8(4) . . . 1_565 ? C61 C64 O17 Mn3 -82.0(5) . . . 1_565 ? C67 C66 O18 C65 -3.7(4) . . . . ? C71 C66 O18 C65 175.8(2) . . . . ? C52 C65 O18 C66 178.4(2) . . . . ? O20 C72 O19 Mn4 -14.3(4) . . . 1_556 ? C69 C72 O19 Mn4 170.82(16) . . . 1_556 ? O19 C72 O20 Mn3 -7.9(4) . . . 1_556 ? C69 C72 O20 Mn3 167.05(17) . . . 1_556 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.681 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.047 data_2 _database_code_depnum_ccdc_archive 'CCDC 816746' #TrackingRef '- n (1-4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C144 H136 Cd7 Cl2 N4 O44, 2(O0.50), 2(O0.50), 2(O0.50), 2(O0.50), 2(O0.50), 2(O0.50), 4(O) ; _chemical_formula_sum 'C144 H164 Cd7 Cl2 N4 O54' _chemical_formula_weight 3644.35 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.8661(10) _cell_length_b 17.8974(12) _cell_length_c 20.5741(14) _cell_angle_alpha 67.2500(10) _cell_angle_beta 77.738(2) _cell_angle_gamma 67.8150(10) _cell_volume 4660.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3807 _cell_measurement_theta_min 2.207 _cell_measurement_theta_max 20.609 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1830.0 _exptl_absorpt_coefficient_mu 0.884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7836 _exptl_absorpt_correction_T_max 0.8361 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25607 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.02 _reflns_number_total 17983 _reflns_number_gt 15018 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+5.4451P] 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 17983 _refine_ls_number_parameters 1025 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8710(2) 1.3849(2) -0.37932(16) 0.0355(7) Uani 1 1 d . . . C2 C 0.8779(2) 1.3012(2) -0.31995(17) 0.0412(8) Uani 1 1 d . . . C3 C 0.7943(2) 1.2766(2) -0.29004(17) 0.0417(8) Uani 1 1 d . . . H3 H 0.7336 1.3145 -0.3051 0.050 Uiso 1 1 calc R . . C4 C 0.8010(2) 1.1974(2) -0.23868(17) 0.0417(8) Uani 1 1 d . . . H4 H 0.7452 1.1822 -0.2196 0.050 Uiso 1 1 calc R . . C5 C 0.8919(2) 1.1403(2) -0.21564(17) 0.0419(8) Uani 1 1 d . . . C6 C 0.9747(2) 1.1634(2) -0.24567(17) 0.0415(8) Uani 1 1 d . . . H6 H 1.0354 1.1250 -0.2310 0.050 Uiso 1 1 calc R . . C7 C 0.9685(2) 1.2433(2) -0.29752(17) 0.0387(7) Uani 1 1 d . . . H7 H 1.0247 1.2577 -0.3170 0.046 Uiso 1 1 calc R . . C8 C 0.9790(2) 0.99605(19) -0.14613(17) 0.0344(7) Uani 1 1 d . . . H8A H 1.0068 1.0049 -0.1122 0.041 Uiso 1 1 calc R . . H8B H 1.0252 0.9952 -0.1872 0.041 Uiso 1 1 calc R . . C9 C 0.9570(2) 0.91203(19) -0.11348(16) 0.0347(7) Uani 1 1 d . . . C10 C 0.9275(2) 0.88236(19) -0.04177(16) 0.0329(7) Uani 1 1 d . . . C11 C 0.9063(2) 0.80490(19) -0.01387(16) 0.0310(6) Uani 1 1 d . . . C12 C 0.9208(2) 0.75434(19) -0.05570(16) 0.0326(7) Uani 1 1 d . . . C13 C 0.9513(2) 0.78465(19) -0.12665(16) 0.0328(7) Uani 1 1 d . . . C14 C 0.9668(2) 0.8668(2) -0.15677(17) 0.0343(7) Uani 1 1 d . . . C15 C 0.9932(2) 0.9040(2) -0.23690(17) 0.0379(7) Uani 1 1 d . . . H15B H 1.0628 0.8857 -0.2461 0.057 Uiso 1 1 calc R . . H15C H 0.9680 0.9655 -0.2522 0.057 Uiso 1 1 calc R . . H15A H 0.9652 0.8839 -0.2622 0.057 Uiso 1 1 calc R . . C16 C 0.9703(2) 0.7319(2) -0.17454(17) 0.0374(7) Uani 1 1 d . . . H16A H 1.0229 0.7413 -0.2103 0.045 Uiso 1 1 calc R . . H16B H 0.9873 0.6713 -0.1472 0.045 Uiso 1 1 calc R . . C17 C 0.9183(2) 0.93090(19) 0.00773(16) 0.0308(6) Uani 1 1 d . . . H17A H 0.8507 0.9598 0.0178 0.046 Uiso 1 1 calc R . . H17B H 0.9517 0.9722 -0.0146 0.046 Uiso 1 1 calc R . . H17C H 0.9468 0.8911 0.0510 0.046 Uiso 1 1 calc R . . C18 C 0.9041(2) 0.66746(18) -0.02141(15) 0.0291(6) Uani 1 1 d . . . H18A H 0.9102 0.6435 -0.0572 0.044 Uiso 1 1 calc R . . H18B H 0.8400 0.6751 0.0024 0.044 Uiso 1 1 calc R . . H18C H 0.9517 0.6293 0.0121 0.044 Uiso 1 1 calc R . . C19 C 0.8799(2) 0.7252(2) -0.25302(17) 0.0350(7) Uani 1 1 d . . . C20 C 0.7907(2) 0.75124(19) -0.28023(15) 0.0291(6) Uani 1 1 d . . . H20 H 0.7358 0.7896 -0.2653 0.035 Uiso 1 1 calc R . . C21 C 0.7852(2) 0.71850(19) -0.33053(16) 0.0314(6) Uani 1 1 d . . . H21 H 0.7260 0.7350 -0.3490 0.038 Uiso 1 1 calc R . . C22 C 0.8674(2) 0.66150(19) -0.35322(16) 0.0311(6) Uani 1 1 d . . . C23 C 0.9567(2) 0.6377(2) -0.32664(16) 0.0326(7) Uani 1 1 d . . . H23 H 1.0124 0.6011 -0.3427 0.039 Uiso 1 1 calc R . . C24 C 0.9612(2) 0.6689(2) -0.27629(16) 0.0341(7) Uani 1 1 d . . . H24 H 1.0204 0.6518 -0.2575 0.041 Uiso 1 1 calc R . . C25 C 0.8599(2) 0.6240(2) -0.40455(17) 0.0355(7) Uani 1 1 d . . . C26 C 0.8577(2) 0.7790(2) 0.06050(16) 0.0348(7) Uani 1 1 d . . . H26A H 0.8238 0.8295 0.0742 0.042 Uiso 1 1 calc R . . H26B H 0.8102 0.7534 0.0615 0.042 Uiso 1 1 calc R . . C27 C 0.8963(2) 0.6986(2) 0.17963(17) 0.0375(7) Uani 1 1 d . . . C28 C 0.8052(2) 0.7482(2) 0.20535(17) 0.0406(8) Uani 1 1 d . . . H28 H 0.7644 0.7967 0.1745 0.049 Uiso 1 1 calc R . . C29 C 0.7797(2) 0.7220(2) 0.27725(17) 0.0385(7) Uani 1 1 d . . . H29 H 0.7215 0.7543 0.2948 0.046 Uiso 1 1 calc R . . C30 C 0.8386(2) 0.6486(2) 0.32392(16) 0.0358(7) Uani 1 1 d . . . C31 C 0.9283(2) 0.6008(2) 0.29849(17) 0.0392(7) Uani 1 1 d . . . H31 H 0.9684 0.5522 0.3298 0.047 Uiso 1 1 calc R . . C32 C 0.9579(2) 0.62630(19) 0.22552(16) 0.0340(7) Uani 1 1 d . . . H32 H 1.0175 0.5952 0.2085 0.041 Uiso 1 1 calc R . . C33 C 0.8054(2) 0.6225(2) 0.40126(17) 0.0354(7) Uani 1 1 d . . . C34 C 0.7007(2) 0.87918(19) 0.40664(16) 0.0325(7) Uani 1 1 d . . . H34A H 0.7373 0.8218 0.4074 0.049 Uiso 1 1 calc R . . H34B H 0.7436 0.9125 0.3924 0.049 Uiso 1 1 calc R . . H34C H 0.6514 0.9046 0.3738 0.049 Uiso 1 1 calc R . . C35 C 0.6398(2) 0.9520(2) 0.49792(17) 0.0373(7) Uani 1 1 d . . . H35A H 0.5920 1.0016 0.4703 0.056 Uiso 1 1 calc R . . H35B H 0.7000 0.9633 0.4908 0.056 Uiso 1 1 calc R . . H35C H 0.6171 0.9389 0.5470 0.056 Uiso 1 1 calc R . . C36 C 0.6162(2) 0.8173(2) 0.51860(16) 0.0322(6) Uani 1 1 d . . . H36 H 0.6216 0.7730 0.5034 0.039 Uiso 1 1 calc R . . C37 C 0.6156(2) 0.6077(2) 0.73138(17) 0.0366(7) Uani 1 1 d . . . H37 H 0.6404 0.5875 0.6937 0.044 Uiso 1 1 calc R . . C38 C 0.6284(2) 0.6013(2) 0.84317(17) 0.0368(7) Uani 1 1 d . . . H38A H 0.5800 0.6566 0.8264 0.055 Uiso 1 1 calc R . . H38B H 0.6793 0.6064 0.8615 0.055 Uiso 1 1 calc R . . H38C H 0.5990 0.5628 0.8799 0.055 Uiso 1 1 calc R . . C39 C 0.7581(3) 0.5071(2) 0.78540(19) 0.0533(10) Uani 1 1 d . . . H39A H 0.7598 0.4841 0.7499 0.080 Uiso 1 1 calc R . . H39B H 0.7682 0.4620 0.8304 0.080 Uiso 1 1 calc R . . H39C H 0.8086 0.5325 0.7734 0.080 Uiso 1 1 calc R . . C40 C 0.3100(2) 0.8908(2) 0.69602(17) 0.0349(7) Uani 1 1 d . . . C41 C 0.3123(2) 0.92836(19) 0.74918(16) 0.0319(7) Uani 1 1 d . . . C42 C 0.2341(2) 0.98872(19) 0.76628(16) 0.0327(7) Uani 1 1 d . . . H42 H 0.1756 1.0053 0.7468 0.039 Uiso 1 1 calc R . . C43 C 0.2386(2) 1.02590(19) 0.81121(17) 0.0346(7) Uani 1 1 d . . . H43 H 0.1849 1.0697 0.8202 0.042 Uiso 1 1 calc R . . C44 C 0.3250(2) 0.9979(2) 0.84407(16) 0.0351(7) Uani 1 1 d . . . C45 C 0.4091(2) 0.9359(2) 0.82700(16) 0.0374(7) Uani 1 1 d . . . H45 H 0.4671 0.9187 0.8473 0.045 Uiso 1 1 calc R . . C46 C 0.4031(2) 0.9025(2) 0.78068(17) 0.0371(7) Uani 1 1 d . . . H46 H 0.4579 0.8619 0.7683 0.045 Uiso 1 1 calc R . . C47 C 0.4111(2) 1.0156(2) 0.92114(17) 0.0361(7) Uani 1 1 d . . . H47A H 0.4622 1.0254 0.8841 0.043 Uiso 1 1 calc R . . H47B H 0.4319 0.9556 0.9507 0.043 Uiso 1 1 calc R . . C48 C 0.3912(2) 1.0710(2) 0.96387(17) 0.0352(7) Uani 1 1 d . . . C49 C 0.4083(2) 1.1505(2) 0.93180(16) 0.0368(7) Uani 1 1 d . . . C50 C 0.3979(2) 1.1983(2) 0.97324(17) 0.0360(7) Uani 1 1 d . . . C51 C 0.3634(2) 1.1724(2) 1.04550(17) 0.0345(7) Uani 1 1 d . . . C52 C 0.3385(2) 1.09839(19) 1.07591(17) 0.0356(7) Uani 1 1 d . . . C53 C 0.3527(2) 1.04697(19) 1.03586(17) 0.0351(7) Uani 1 1 d . . . C54 C 0.3292(2) 0.9633(2) 1.07094(17) 0.0350(7) Uani 1 1 d . . . H54A H 0.3454 0.9382 1.1192 0.053 Uiso 1 1 calc R . . H54B H 0.3665 0.9241 1.0461 0.053 Uiso 1 1 calc R . . H54C H 0.2610 0.9749 1.0695 0.053 Uiso 1 1 calc R . . C55 C 0.4378(2) 1.1786(2) 0.85248(17) 0.0412(8) Uani 1 1 d . . . H55D H 0.4166 1.2401 0.8331 0.062 Uiso 1 1 calc R . . H55E H 0.4081 1.1569 0.8298 0.062 Uiso 1 1 calc R . . H55F H 0.5074 1.1564 0.8448 0.062 Uiso 1 1 calc R . . C56 C 0.3519(2) 1.2296(2) 1.08867(16) 0.0341(7) Uani 1 1 d . . . H56A H 0.2881 1.2718 1.0845 0.051 Uiso 1 1 calc R . . H56B H 0.4002 1.2579 1.0709 0.051 Uiso 1 1 calc R . . H56C H 0.3605 1.1949 1.1374 0.051 Uiso 1 1 calc R . . C57 C 0.4204(2) 1.28653(19) 0.93565(18) 0.0388(7) Uani 1 1 d . . . H57A H 0.4498 1.2979 0.9670 0.047 Uiso 1 1 calc R . . H57B H 0.4628 1.2865 0.8928 0.047 Uiso 1 1 calc R . . C58 C 0.3225(2) 1.4284(2) 0.87070(18) 0.0466(9) Uani 1 1 d . . . C59 C 0.3946(2) 1.4536(2) 0.83310(17) 0.0396(8) Uani 1 1 d . . . H59 H 0.4579 1.4156 0.8398 0.048 Uiso 1 1 calc R . . C60 C 0.3806(2) 1.5344(2) 0.78384(18) 0.0412(8) Uani 1 1 d . . . H60 H 0.4340 1.5520 0.7613 0.049 Uiso 1 1 calc R . . C61 C 0.2912(2) 1.5875(2) 0.76820(18) 0.0430(8) Uani 1 1 d . . . C62 C 0.2207(2) 1.5622(2) 0.81151(17) 0.0443(9) Uani 1 1 d . . . H62 H 0.1573 1.5998 0.8052 0.053 Uiso 1 1 calc R . . C63 C 0.2338(3) 1.4863(2) 0.86402(19) 0.0586(12) Uani 1 1 d . . . H63 H 0.1816 1.4744 0.8951 0.070 Uiso 1 1 calc R . . C64 C 0.2706(2) 1.6752(2) 0.71476(16) 0.0342(7) Uani 1 1 d . . . C65 C 0.2989(2) 1.0738(2) 1.14939(17) 0.0352(7) Uani 1 1 d . . . H65A H 0.2663 1.1240 1.1635 0.042 Uiso 1 1 calc R . . H65B H 0.2523 1.0451 1.1555 0.042 Uiso 1 1 calc R . . C66 C 0.3639(2) 0.9857(2) 1.26292(16) 0.0345(7) Uani 1 1 d . . . C67 C 0.2745(2) 1.0066(2) 1.29701(16) 0.0335(7) Uani 1 1 d . . . H67 H 0.2199 1.0445 1.2725 0.040 Uiso 1 1 calc R . . C68 C 0.2674(2) 0.9679(2) 1.37230(17) 0.0367(7) Uani 1 1 d . . . H68 H 0.2069 0.9820 1.3971 0.044 Uiso 1 1 calc R . . C69 C 0.3477(2) 0.91014(19) 1.40968(16) 0.0308(6) Uani 1 1 d . . . C70 C 0.4357(2) 0.8919(2) 1.37165(16) 0.0346(7) Uani 1 1 d . . . H70 H 0.4904 0.8543 1.3960 0.041 Uiso 1 1 calc R . . C71 C 0.4476(3) 0.9268(2) 1.29783(18) 0.0457(9) Uani 1 1 d . . . H71 H 0.5080 0.9118 1.2731 0.055 Uiso 1 1 calc R . . C72 C 0.3357(2) 0.86822(19) 1.48763(16) 0.0328(7) Uani 1 1 d . . . Cd1 Cd 1.0000 0.5000 0.5000 0.03297(7) Uani 1 2 d S . . Cd2 Cd 0.732246(16) 0.567049(14) 0.536253(11) 0.02888(5) Uani 1 1 d . . . Cd3 Cd 0.463021(17) 0.745207(14) 0.626163(12) 0.03369(6) Uani 1 1 d . . . Cd4 Cd 0.196553(18) 0.842644(16) 0.621971(13) 0.03844(6) Uani 1 1 d . . . Cl1 Cl 0.55564(5) 0.61731(5) 0.58194(4) 0.03047(15) Uani 1 1 d . . . N1 N 0.6666(2) 0.57025(17) 0.78907(14) 0.0401(6) Uani 1 1 d . . . N2 N 0.6558(2) 0.87724(17) 0.47561(14) 0.0354(6) Uani 1 1 d . . . O1 O 0.78621(15) 1.44072(13) -0.38648(11) 0.0327(5) Uani 1 1 d . . . O2 O 0.94382(16) 1.39617(13) -0.41603(11) 0.0373(5) Uani 1 1 d . . . O3 O 0.88988(17) 1.06223(14) -0.16587(13) 0.0492(7) Uani 1 1 d . . . O4 O 0.88199(15) 0.76129(13) -0.20603(11) 0.0345(5) Uani 1 1 d . . . O5 O 0.77692(15) 0.63684(13) -0.41726(11) 0.0346(5) Uani 1 1 d . . . O6 O 0.93579(16) 0.58465(14) -0.43192(11) 0.0353(5) Uani 1 1 d . . . O7 O 0.92883(16) 0.71907(14) 0.10938(11) 0.0399(5) Uani 1 1 d . . . O8 O 0.72397(16) 0.66521(14) 0.42101(11) 0.0385(5) Uani 1 1 d . . . O9 O 0.85923(15) 0.55448(14) 0.44385(11) 0.0375(5) Uani 1 1 d . . . O10 O 0.57291(16) 0.81709(13) 0.57709(11) 0.0349(5) Uani 1 1 d . . . O11 O 0.54172(16) 0.66446(13) 0.72618(11) 0.0363(5) Uani 1 1 d . . . O12 O 0.38530(16) 0.84381(14) 0.67642(11) 0.0375(5) Uani 1 1 d . . . O13 O 0.22791(16) 0.91186(13) 0.67566(11) 0.0341(5) Uani 1 1 d . . . O14 O 0.32051(15) 1.03767(13) 0.89049(11) 0.0323(5) Uani 1 1 d . . . O15 O 0.32524(16) 1.34726(15) 0.92045(12) 0.0445(6) Uani 1 1 d . . . O16 O 0.33127(16) 1.69548(13) 0.66996(11) 0.0329(5) Uani 1 1 d . . . O17 O 0.19005(17) 1.72780(14) 0.71445(12) 0.0415(5) Uani 1 1 d . . . O18 O 0.38023(15) 1.01668(14) 1.19120(11) 0.0378(5) Uani 1 1 d . . . O19 O 0.25319(16) 0.89240(13) 1.51620(11) 0.0341(5) Uani 1 1 d . . . O20 O 0.40894(16) 0.81656(14) 1.51653(11) 0.0361(5) Uani 1 1 d . . . O1W O 0.67958(16) 0.48740(13) 0.49077(11) 0.0327(5) Uani 1 1 d . . . O2W O 0.04198(16) 0.91696(14) 0.59369(12) 0.0380(5) Uani 1 1 d . . . O3W O 0.7553(5) 0.2530(5) 0.9562(4) 0.0356(16) Uani 0.30 1 d P . . O4W O 0.2172(4) 0.6619(3) 0.5011(3) 0.0359(12) Uani 0.40 1 d P . . O5W O 0.4975(5) 0.3521(4) 0.6698(4) 0.0316(15) Uani 0.30 1 d P . . O6W O 0.6930(3) 0.2471(3) 0.8642(2) 0.0357(10) Uani 0.50 1 d P . . O7W O 0.8901(3) 0.7918(3) 0.4857(2) 0.0422(11) Uani 0.50 1 d P . . O8W O 0.7792(3) 0.2340(3) 0.1149(2) 0.0425(11) Uani 0.50 1 d P . . O9W O 0.4068(3) 0.7217(3) 0.4732(2) 0.0389(10) Uani 0.50 1 d P . . O10W O 0.8911(5) 0.5569(5) 0.8925(4) 0.0365(16) Uani 0.30 1 d P . . O11W O 0.2212(4) 0.5979(3) 0.9967(3) 0.0376(12) Uani 0.40 1 d P . . O12W O 0.9221(6) 0.1281(5) 0.5791(4) 0.0421(18) Uani 0.30 1 d P . . O13W O 0.4875(3) 0.6386(3) 0.9822(2) 0.0364(10) Uani 0.50 1 d P . . O14W O 0.7753(3) 0.4690(3) 0.2629(2) 0.0363(10) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0354(17) 0.0329(16) 0.0315(16) -0.0017(13) -0.0049(13) -0.0123(13) C2 0.0337(17) 0.0337(17) 0.0337(17) 0.0028(14) 0.0103(13) -0.0085(13) C3 0.0366(18) 0.0350(17) 0.0329(17) 0.0132(14) -0.0094(13) -0.0114(14) C4 0.0330(17) 0.0382(18) 0.0372(18) 0.0092(14) -0.0075(13) -0.0140(14) C5 0.0356(17) 0.0296(16) 0.0337(17) 0.0071(13) 0.0035(13) -0.0039(13) C6 0.0339(17) 0.0376(17) 0.0363(18) 0.0010(14) 0.0056(13) -0.0123(14) C7 0.0356(17) 0.0331(16) 0.0372(18) -0.0016(14) -0.0010(13) -0.0118(14) C8 0.0318(16) 0.0301(15) 0.0339(16) -0.0028(13) -0.0103(13) -0.0065(13) C9 0.0344(17) 0.0311(16) 0.0329(16) -0.0048(13) -0.0095(13) -0.0072(13) C10 0.0379(17) 0.0308(15) 0.0345(16) -0.0120(13) -0.0064(13) -0.0133(13) C11 0.0359(16) 0.0288(15) 0.0345(16) -0.0136(13) -0.0051(13) -0.0129(13) C12 0.0381(17) 0.0341(16) 0.0361(17) -0.0133(13) -0.0088(13) -0.0183(13) C13 0.0361(17) 0.0321(15) 0.0349(16) -0.0099(13) -0.0125(13) -0.0125(13) C14 0.0318(16) 0.0323(16) 0.0372(17) -0.0132(13) 0.0002(13) -0.0087(13) C15 0.0342(17) 0.0374(17) 0.0393(18) -0.0154(14) 0.0085(13) -0.0122(14) C16 0.0381(17) 0.0393(17) 0.0352(17) -0.0164(14) -0.0129(13) -0.0037(14) C17 0.0330(16) 0.0309(15) 0.0366(16) -0.0196(13) -0.0028(12) -0.0106(12) C18 0.0378(16) 0.0322(15) 0.0316(15) -0.0177(13) -0.0033(12) -0.0192(13) C19 0.0312(16) 0.0373(17) 0.0391(17) -0.0245(14) -0.0088(13) 0.0012(13) C20 0.0299(15) 0.0364(16) 0.0304(15) -0.0248(13) -0.0043(12) -0.0061(12) C21 0.0332(16) 0.0336(16) 0.0395(17) -0.0261(14) 0.0054(13) -0.0143(13) C22 0.0320(16) 0.0364(16) 0.0359(16) -0.0251(14) -0.0072(12) -0.0070(13) C23 0.0324(16) 0.0385(16) 0.0345(16) -0.0256(14) -0.0105(12) -0.0017(13) C24 0.0309(16) 0.0377(16) 0.0321(16) -0.0165(13) -0.0165(12) 0.0028(13) C25 0.0349(17) 0.0398(17) 0.0382(17) -0.0242(14) -0.0083(13) -0.0047(14) C26 0.0384(17) 0.0322(16) 0.0344(17) -0.0069(13) -0.0063(13) -0.0148(13) C27 0.0355(17) 0.0348(17) 0.0353(17) -0.0053(14) -0.0047(13) -0.0098(14) C28 0.0363(18) 0.0343(17) 0.0339(17) -0.0065(14) -0.0087(13) 0.0048(14) C29 0.0306(16) 0.0388(17) 0.0376(18) -0.0115(14) -0.0047(13) -0.0027(13) C30 0.0377(17) 0.0333(16) 0.0322(16) -0.0101(13) -0.0079(13) -0.0052(13) C31 0.0376(18) 0.0344(17) 0.0348(17) -0.0076(14) -0.0042(13) -0.0038(14) C32 0.0339(16) 0.0303(15) 0.0359(17) -0.0141(13) -0.0073(13) -0.0031(13) C33 0.0344(17) 0.0313(16) 0.0358(17) -0.0093(13) -0.0009(13) -0.0090(13) C34 0.0323(16) 0.0350(16) 0.0399(17) -0.0212(14) 0.0142(13) -0.0218(13) C35 0.0351(17) 0.0347(16) 0.0374(17) -0.0134(14) 0.0132(13) -0.0139(14) C36 0.0365(17) 0.0358(16) 0.0331(16) -0.0160(13) -0.0029(13) -0.0166(13) C37 0.0374(17) 0.0348(16) 0.0321(16) -0.0027(13) -0.0107(13) -0.0106(14) C38 0.0396(18) 0.0399(17) 0.0431(18) -0.0159(14) -0.0229(14) -0.0134(14) C39 0.045(2) 0.0371(18) 0.0360(19) 0.0122(15) -0.0120(15) 0.0108(15) C40 0.0298(16) 0.0398(17) 0.0371(17) -0.0187(14) 0.0100(13) -0.0143(13) C41 0.0340(16) 0.0305(15) 0.0395(17) -0.0180(13) 0.0106(13) -0.0204(13) C42 0.0371(17) 0.0306(15) 0.0401(17) -0.0214(14) -0.0021(13) -0.0121(13) C43 0.0348(17) 0.0298(15) 0.0397(17) -0.0165(13) -0.0158(13) 0.0006(13) C44 0.0310(16) 0.0415(18) 0.0344(17) -0.0188(14) -0.0035(13) -0.0068(14) C45 0.0340(17) 0.0347(16) 0.0319(16) -0.0126(13) -0.0034(13) 0.0029(13) C46 0.0360(17) 0.0355(17) 0.0353(17) -0.0156(14) 0.0074(13) -0.0087(14) C47 0.0333(16) 0.0332(16) 0.0349(17) -0.0174(13) -0.0145(13) 0.0088(13) C48 0.0330(16) 0.0341(16) 0.0346(17) -0.0116(13) -0.0065(13) -0.0048(13) C49 0.0341(17) 0.0363(17) 0.0315(16) -0.0047(13) -0.0069(13) -0.0072(13) C50 0.0349(17) 0.0332(16) 0.0358(17) -0.0072(13) -0.0141(13) -0.0052(13) C51 0.0314(16) 0.0335(16) 0.0384(17) -0.0119(14) -0.0109(13) -0.0062(13) C52 0.0374(17) 0.0270(15) 0.0372(17) -0.0098(13) -0.0098(13) -0.0025(13) C53 0.0352(17) 0.0295(15) 0.0335(17) -0.0075(13) -0.0072(13) -0.0039(13) C54 0.0349(17) 0.0387(17) 0.0371(17) -0.0188(14) 0.0050(13) -0.0162(14) C55 0.0354(18) 0.0391(18) 0.0357(18) -0.0021(14) 0.0034(14) -0.0121(14) C56 0.0337(16) 0.0422(17) 0.0353(17) -0.0113(14) -0.0128(13) -0.0183(14) C57 0.0336(17) 0.0317(16) 0.0368(17) 0.0029(13) -0.0166(13) -0.0029(13) C58 0.0328(17) 0.0372(18) 0.0360(18) 0.0124(14) 0.0011(14) -0.0030(14) C59 0.0335(17) 0.0338(16) 0.0327(17) 0.0023(13) 0.0089(13) -0.0110(13) C60 0.0379(18) 0.0383(18) 0.0378(18) -0.0019(14) 0.0038(14) -0.0171(15) C61 0.0384(18) 0.0325(17) 0.0394(19) 0.0007(14) 0.0094(14) -0.0117(14) C62 0.0300(16) 0.0364(17) 0.0367(18) 0.0196(14) -0.0124(13) -0.0066(14) C63 0.0375(19) 0.0365(18) 0.040(2) 0.0149(15) 0.0213(15) 0.0115(15) C64 0.0398(18) 0.0330(16) 0.0271(16) -0.0094(13) 0.0057(13) -0.0143(14) C65 0.0309(16) 0.0321(16) 0.0389(17) -0.0142(14) -0.0073(13) -0.0018(13) C66 0.0294(16) 0.0407(17) 0.0318(16) -0.0138(14) -0.0033(12) -0.0077(13) C67 0.0364(17) 0.0329(16) 0.0338(16) -0.0175(13) 0.0013(13) -0.0099(13) C68 0.0343(17) 0.0337(16) 0.0362(17) -0.0120(14) 0.0071(13) -0.0099(13) C69 0.0340(16) 0.0327(15) 0.0325(16) -0.0132(13) 0.0002(12) -0.0173(13) C70 0.0349(17) 0.0367(16) 0.0298(16) -0.0070(13) -0.0025(13) -0.0136(14) C71 0.0403(19) 0.0358(17) 0.0349(18) -0.0025(14) -0.0020(14) 0.0050(15) C72 0.0357(17) 0.0278(15) 0.0344(17) -0.0150(13) 0.0036(13) -0.0088(13) Cd1 0.02954(16) 0.03183(16) 0.03323(17) -0.00868(13) -0.00244(12) -0.00788(13) Cd2 0.03048(11) 0.03090(11) 0.02779(11) -0.01098(9) -0.00444(8) -0.01053(9) Cd3 0.03745(13) 0.02963(11) 0.03548(12) -0.01437(9) -0.00035(9) -0.01046(9) Cd4 0.03855(13) 0.03994(13) 0.03262(12) -0.00565(10) -0.00354(9) -0.01480(10) Cl1 0.0310(4) 0.0334(4) 0.0322(4) -0.0174(3) 0.0000(3) -0.0110(3) N1 0.0383(15) 0.0386(15) 0.0349(15) -0.0054(12) -0.0147(12) -0.0047(12) N2 0.0389(15) 0.0341(14) 0.0354(14) -0.0108(11) 0.0000(11) -0.0167(12) O1 0.0327(11) 0.0333(11) 0.0321(11) -0.0088(9) -0.0055(9) -0.0117(9) O2 0.0391(12) 0.0297(11) 0.0356(12) 0.0016(9) -0.0003(9) -0.0178(10) O3 0.0369(13) 0.0330(12) 0.0430(14) 0.0151(10) 0.0061(10) -0.0081(10) O4 0.0332(11) 0.0362(11) 0.0359(12) -0.0183(10) -0.0168(9) 0.0006(9) O5 0.0340(12) 0.0306(11) 0.0396(12) -0.0112(9) -0.0044(9) -0.0110(9) O6 0.0356(12) 0.0396(12) 0.0315(11) -0.0168(10) -0.0005(9) -0.0095(10) O7 0.0320(12) 0.0400(12) 0.0343(12) -0.0074(10) -0.0055(9) -0.0013(10) O8 0.0396(13) 0.0324(11) 0.0336(12) -0.0107(9) 0.0019(9) -0.0044(10) O9 0.0290(11) 0.0372(12) 0.0380(12) -0.0056(10) -0.0012(9) -0.0102(9) O10 0.0349(12) 0.0359(11) 0.0340(12) -0.0156(9) 0.0060(9) -0.0125(9) O11 0.0401(12) 0.0319(11) 0.0362(12) -0.0101(9) -0.0108(9) -0.0084(9) O12 0.0377(12) 0.0364(12) 0.0384(12) -0.0203(10) 0.0140(9) -0.0135(10) O13 0.0364(12) 0.0313(11) 0.0334(11) -0.0053(9) -0.0024(9) -0.0160(9) O14 0.0308(11) 0.0350(11) 0.0306(11) -0.0188(9) -0.0095(8) 0.0015(9) O15 0.0349(12) 0.0387(12) 0.0325(12) 0.0020(10) 0.0018(9) 0.0003(10) O16 0.0388(12) 0.0320(11) 0.0305(11) -0.0139(9) 0.0013(9) -0.0134(9) O17 0.0378(13) 0.0380(12) 0.0392(13) -0.0057(10) -0.0024(10) -0.0103(10) O18 0.0300(11) 0.0405(12) 0.0345(12) -0.0072(10) -0.0046(9) -0.0072(9) O19 0.0357(12) 0.0318(11) 0.0338(11) -0.0054(9) -0.0034(9) -0.0156(9) O20 0.0390(12) 0.0397(12) 0.0325(11) -0.0051(10) -0.0107(9) -0.0191(10) O1W 0.0400(12) 0.0395(12) 0.0332(11) -0.0207(9) -0.0028(9) -0.0200(10) O2W 0.0377(12) 0.0411(12) 0.0396(12) -0.0193(10) -0.0133(10) -0.0063(10) O3W 0.037(4) 0.038(4) 0.034(4) -0.017(3) -0.015(3) -0.004(3) O4W 0.032(3) 0.036(3) 0.040(3) -0.018(2) -0.017(2) 0.000(2) O5W 0.036(4) 0.037(4) 0.045(4) -0.031(3) -0.006(3) -0.016(3) O6W 0.034(2) 0.045(3) 0.032(2) -0.021(2) 0.0032(18) -0.013(2) O7W 0.036(2) 0.038(2) 0.036(2) -0.003(2) -0.0070(19) -0.003(2) O8W 0.046(3) 0.035(2) 0.036(2) -0.013(2) 0.002(2) -0.003(2) O9W 0.031(2) 0.041(2) 0.040(3) -0.008(2) -0.0010(19) -0.0133(19) O10W 0.036(4) 0.041(4) 0.035(4) -0.017(3) 0.006(3) -0.016(3) O11W 0.044(3) 0.032(3) 0.038(3) -0.009(2) -0.015(2) -0.010(2) O12W 0.039(4) 0.037(4) 0.043(4) -0.005(3) -0.003(3) -0.013(3) O13W 0.037(2) 0.038(2) 0.035(2) -0.0180(19) -0.0192(19) 0.0014(19) O14W 0.038(2) 0.039(2) 0.033(2) -0.0042(19) -0.0111(18) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.217(3) . ? C1 O1 1.274(3) . ? C1 C2 1.507(4) . ? C2 C7 1.393(5) . ? C2 C3 1.412(5) . ? C3 C4 1.385(4) . ? C3 H3 0.9300 . ? C4 C5 1.397(4) . ? C4 H4 0.9300 . ? C5 O3 1.383(3) . ? C5 C6 1.390(5) . ? C6 C7 1.397(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.413(3) . ? C8 C9 1.522(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.372(4) . ? C9 C10 1.395(4) . ? C10 C11 1.410(4) . ? C10 C17 1.532(4) . ? C11 C12 1.408(4) . ? C11 C26 1.521(4) . ? C12 C13 1.387(4) . ? C12 C18 1.531(4) . ? C13 C14 1.446(4) . ? C13 C16 1.530(4) . ? C14 C15 1.546(4) . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C15 H15A 0.9600 . ? C16 O4 1.413(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O4 1.365(3) . ? C19 C24 1.383(4) . ? C19 C20 1.392(4) . ? C20 C21 1.401(4) . ? C20 H20 0.9300 . ? C21 C22 1.392(4) . ? C21 H21 0.9300 . ? C22 C23 1.393(4) . ? C22 C25 1.494(4) . ? C23 C24 1.378(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O5 1.232(3) . ? C25 O6 1.234(3) . ? C26 O7 1.428(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O7 1.373(3) . ? C27 C32 1.390(4) . ? C27 C28 1.433(4) . ? C28 C29 1.383(5) . ? C28 H28 0.9300 . ? C29 C30 1.388(4) . ? C29 H29 0.9300 . ? C30 C31 1.405(4) . ? C30 C33 1.503(4) . ? C31 C32 1.413(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O8 1.244(3) . ? C33 O9 1.275(3) . ? C33 Cd2 2.699(3) . ? C34 N2 1.427(3) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 N2 1.498(3) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O10 1.238(3) . ? C36 N2 1.342(3) . ? C36 H36 0.9300 . ? C37 O11 1.172(3) . ? C37 N1 1.348(3) . ? C37 H37 0.9300 . ? C38 N1 1.357(3) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N1 1.412(3) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 O12 1.218(3) . ? C40 O13 1.246(3) . ? C40 C41 1.501(4) . ? C41 C42 1.347(4) . ? C41 C46 1.456(5) . ? C42 C43 1.355(4) . ? C42 H42 0.9300 . ? C43 C44 1.406(4) . ? C43 H43 0.9300 . ? C44 O14 1.374(3) . ? C44 C45 1.410(4) . ? C45 C46 1.338(5) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 O14 1.461(3) . ? C47 C48 1.479(4) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.415(5) . ? C48 C53 1.428(3) . ? C49 C50 1.375(5) . ? C49 C55 1.528(3) . ? C50 C51 1.418(3) . ? C50 C57 1.596(3) . ? C51 C52 1.383(4) . ? C51 C56 1.541(4) . ? C52 C53 1.392(4) . ? C52 C65 1.459(5) . ? C53 C54 1.530(4) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55D 0.9600 . ? C55 H55E 0.9600 . ? C55 H55F 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 O15 1.429(4) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.301(5) . ? C58 C63 1.329(5) . ? C58 O15 1.408(4) . ? C59 C60 1.374(4) . ? C59 H59 0.9300 . ? C60 C61 1.329(5) . ? C60 H60 0.9300 . ? C61 C62 1.320(4) . ? C61 C64 1.488(4) . ? C62 C63 1.344(4) . ? C62 O14W 1.805(6) 2_676 ? C62 H62 0.9300 . ? C63 H63 0.9300 . ? C64 O16 1.196(4) . ? C64 O17 1.212(4) . ? C65 O18 1.441(4) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.354(4) . ? C66 O18 1.364(4) . ? C66 C71 1.407(4) . ? C67 C68 1.430(4) . ? C67 H67 0.9300 . ? C68 C69 1.388(4) . ? C68 H68 0.9300 . ? C69 C70 1.368(4) . ? C69 C72 1.488(4) . ? C70 C71 1.401(4) . ? C70 H70 0.9300 . ? C71 H71 0.9300 . ? C72 O20 1.218(4) . ? C72 O19 1.236(4) . ? Cd1 O6 2.269(2) 2_765 ? Cd1 O6 2.269(2) 1_556 ? Cd1 O2 2.283(2) 2_775 ? Cd1 O2 2.283(2) 1_546 ? Cd1 O9 2.298(2) . ? Cd1 O9 2.298(2) 2_766 ? Cd2 O1 2.162(2) 1_546 ? Cd2 O5 2.176(2) 1_556 ? Cd2 O8 2.337(2) . ? Cd2 O1W 2.3889(19) . ? Cd2 O9 2.390(2) . ? Cd2 Cl1 2.5313(8) . ? Cd3 O12 2.210(2) . ? Cd3 O20 2.265(2) 1_554 ? Cd3 O11 2.267(2) . ? Cd3 O10 2.286(2) . ? Cd3 O16 2.321(2) 1_545 ? Cd3 Cl1 2.5811(7) . ? Cd4 O19 2.128(2) 1_554 ? Cd4 O13 2.165(2) . ? Cd4 O17 2.214(2) 1_545 ? Cd4 O2W 2.247(2) . ? Cd4 O16 2.601(2) 1_545 ? O1 Cd2 2.162(2) 1_564 ? O2 Cd1 2.283(2) 1_564 ? O5 Cd2 2.176(2) 1_554 ? O6 Cd1 2.269(2) 1_554 ? O16 Cd3 2.321(2) 1_565 ? O16 Cd4 2.601(2) 1_565 ? O17 Cd4 2.214(2) 1_565 ? O19 Cd4 2.128(2) 1_556 ? O20 Cd3 2.265(2) 1_556 ? O14W C62 1.805(6) 2_676 ? 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 O2 C1 O1 124.4(2) . . ? O2 C1 C2 120.1(3) . . ? O1 C1 C2 115.5(3) . . ? C7 C2 C3 118.6(3) . . ? C7 C2 C1 120.2(3) . . ? C3 C2 C1 121.0(3) . . ? C4 C3 C2 121.3(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.7(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? O3 C5 C6 126.1(3) . . ? O3 C5 C4 114.5(3) . . ? C6 C5 C4 119.3(3) . . ? C5 C6 C7 121.3(3) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C2 C7 C6 119.8(3) . . ? C2 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? O3 C8 C9 107.0(2) . . ? O3 C8 H8A 110.3 . . ? C9 C8 H8A 110.3 . . ? O3 C8 H8B 110.3 . . ? C9 C8 H8B 110.3 . . ? H8A C8 H8B 108.6 . . ? C14 C9 C10 121.3(3) . . ? C14 C9 C8 117.9(3) . . ? C10 C9 C8 120.8(3) . . ? C9 C10 C11 119.0(3) . . ? C9 C10 C17 122.0(3) . . ? C11 C10 C17 119.0(3) . . ? C12 C11 C10 121.3(3) . . ? C12 C11 C26 118.5(3) . . ? C10 C11 C26 119.9(3) . . ? C13 C12 C11 118.5(3) . . ? C13 C12 C18 122.2(3) . . ? C11 C12 C18 119.2(3) . . ? C12 C13 C14 120.4(3) . . ? C12 C13 C16 121.0(3) . . ? C14 C13 C16 118.5(3) . . ? C9 C14 C13 119.3(3) . . ? C9 C14 C15 120.2(3) . . ? C13 C14 C15 120.6(3) . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? O4 C16 C13 105.2(2) . . ? O4 C16 H16A 110.7 . . ? C13 C16 H16A 110.7 . . ? O4 C16 H16B 110.7 . . ? C13 C16 H16B 110.7 . . ? H16A C16 H16B 108.8 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C24 123.5(3) . . ? O4 C19 C20 116.3(2) . . ? C24 C19 C20 120.1(3) . . ? C19 C20 C21 118.7(3) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? C22 C21 C20 120.7(3) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 119.9(3) . . ? C21 C22 C25 120.3(3) . . ? C23 C22 C25 119.9(3) . . ? C24 C23 C22 119.1(3) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C19 121.5(3) . . ? C23 C24 H24 119.3 . . ? C19 C24 H24 119.3 . . ? O5 C25 O6 125.1(2) . . ? O5 C25 C22 116.5(2) . . ? O6 C25 C22 118.5(3) . . ? O7 C26 C11 110.3(2) . . ? O7 C26 H26A 109.6 . . ? C11 C26 H26A 109.6 . . ? O7 C26 H26B 109.6 . . ? C11 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? O7 C27 C32 115.9(3) . . ? O7 C27 C28 123.0(3) . . ? C32 C27 C28 121.1(3) . . ? C29 C28 C27 118.2(3) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? C28 C29 C30 121.7(3) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C31 119.8(3) . . ? C29 C30 C33 119.1(3) . . ? C31 C30 C33 121.2(3) . . ? C30 C31 C32 120.2(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C27 C32 C31 118.9(3) . . ? C27 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? O8 C33 O9 122.1(3) . . ? O8 C33 C30 118.9(3) . . ? O9 C33 C30 118.9(3) . . ? O8 C33 Cd2 59.90(13) . . ? O9 C33 Cd2 62.35(13) . . ? C30 C33 Cd2 172.9(2) . . ? N2 C34 H34A 109.5 . . ? N2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C35 H35A 109.5 . . ? N2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O10 C36 N2 124.3(2) . . ? O10 C36 H36 117.8 . . ? N2 C36 H36 117.8 . . ? O11 C37 N1 123.5(3) . . ? O11 C37 H37 118.2 . . ? N1 C37 H37 118.2 . . ? N1 C38 H38A 109.5 . . ? N1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N1 C39 H39A 109.5 . . ? N1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O12 C40 O13 125.7(3) . . ? O12 C40 C41 119.4(3) . . ? O13 C40 C41 114.9(2) . . ? C42 C41 C46 118.6(3) . . ? C42 C41 C40 122.0(3) . . ? C46 C41 C40 119.4(3) . . ? C41 C42 C43 121.5(3) . . ? C41 C42 H42 119.2 . . ? C43 C42 H42 119.2 . . ? C42 C43 C44 119.7(3) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? O14 C44 C43 114.9(2) . . ? O14 C44 C45 124.3(3) . . ? C43 C44 C45 120.7(3) . . ? C46 C45 C44 117.9(3) . . ? C46 C45 H45 121.0 . . ? C44 C45 H45 121.0 . . ? C45 C46 C41 121.4(3) . . ? C45 C46 H46 119.3 . . ? C41 C46 H46 119.3 . . ? O14 C47 C48 107.0(2) . . ? O14 C47 H47A 110.3 . . ? C48 C47 H47A 110.3 . . ? O14 C47 H47B 110.3 . . ? C48 C47 H47B 110.3 . . ? H47A C47 H47B 108.6 . . ? C49 C48 C53 119.6(3) . . ? C49 C48 C47 118.9(3) . . ? C53 C48 C47 121.4(3) . . ? C50 C49 C48 118.7(3) . . ? C50 C49 C55 123.4(3) . . ? C48 C49 C55 117.9(3) . . ? C49 C50 C51 121.2(3) . . ? C49 C50 C57 117.3(3) . . ? C51 C50 C57 121.4(2) . . ? C52 C51 C50 120.5(3) . . ? C52 C51 C56 120.9(3) . . ? C50 C51 C56 118.5(2) . . ? C51 C52 C53 119.3(3) . . ? C51 C52 C65 120.5(3) . . ? C53 C52 C65 120.2(3) . . ? C52 C53 C48 120.4(3) . . ? C52 C53 C54 118.8(3) . . ? C48 C53 C54 120.8(2) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C49 C55 H55D 109.5 . . ? C49 C55 H55E 109.5 . . ? H55D C55 H55E 109.5 . . ? C49 C55 H55F 109.5 . . ? H55D C55 H55F 109.5 . . ? H55E C55 H55F 109.5 . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O15 C57 C50 102.0(2) . . ? O15 C57 H57A 111.4 . . ? C50 C57 H57A 111.4 . . ? O15 C57 H57B 111.4 . . ? C50 C57 H57B 111.4 . . ? H57A C57 H57B 109.2 . . ? C59 C58 C63 117.4(3) . . ? C59 C58 O15 128.7(3) . . ? C63 C58 O15 113.9(3) . . ? C58 C59 C60 122.3(3) . . ? C58 C59 H59 118.8 . . ? C60 C59 H59 118.8 . . ? C61 C60 C59 120.4(3) . . ? C61 C60 H60 119.8 . . ? C59 C60 H60 119.8 . . ? C62 C61 C60 114.6(3) . . ? C62 C61 C64 121.2(3) . . ? C60 C61 C64 123.3(3) . . ? C61 C62 C63 124.9(3) . . ? C61 C62 O14W 77.0(3) . 2_676 ? C63 C62 O14W 100.3(3) . 2_676 ? C61 C62 H62 117.5 . . ? C63 C62 H62 117.5 . . ? O14W C62 H62 92.9 2_676 . ? C58 C63 C62 118.9(3) . . ? C58 C63 H63 120.6 . . ? C62 C63 H63 120.6 . . ? O16 C64 O17 117.9(3) . . ? O16 C64 C61 121.8(3) . . ? O17 C64 C61 120.3(3) . . ? O18 C65 C52 106.6(3) . . ? O18 C65 H65A 110.4 . . ? C52 C65 H65A 110.4 . . ? O18 C65 H65B 110.4 . . ? C52 C65 H65B 110.4 . . ? H65A C65 H65B 108.6 . . ? C67 C66 O18 123.0(3) . . ? C67 C66 C71 123.1(3) . . ? O18 C66 C71 113.9(3) . . ? C66 C67 C68 117.1(3) . . ? C66 C67 H67 121.4 . . ? C68 C67 H67 121.4 . . ? C69 C68 C67 122.3(3) . . ? C69 C68 H68 118.8 . . ? C67 C68 H68 118.8 . . ? C70 C69 C68 117.3(3) . . ? C70 C69 C72 122.4(3) . . ? C68 C69 C72 120.3(3) . . ? C69 C70 C71 123.4(3) . . ? C69 C70 H70 118.3 . . ? C71 C70 H70 118.3 . . ? C70 C71 C66 116.8(3) . . ? C70 C71 H71 121.6 . . ? C66 C71 H71 121.6 . . ? O20 C72 O19 127.2(3) . . ? O20 C72 C69 116.5(3) . . ? O19 C72 C69 116.2(3) . . ? O6 Cd1 O6 180.000(2) 2_765 1_556 ? O6 Cd1 O2 89.99(8) 2_765 2_775 ? O6 Cd1 O2 90.01(8) 1_556 2_775 ? O6 Cd1 O2 90.01(8) 2_765 1_546 ? O6 Cd1 O2 89.99(8) 1_556 1_546 ? O2 Cd1 O2 180.00(9) 2_775 1_546 ? O6 Cd1 O9 87.48(8) 2_765 . ? O6 Cd1 O9 92.52(8) 1_556 . ? O2 Cd1 O9 90.21(8) 2_775 . ? O2 Cd1 O9 89.79(8) 1_546 . ? O6 Cd1 O9 92.52(8) 2_765 2_766 ? O6 Cd1 O9 87.48(8) 1_556 2_766 ? O2 Cd1 O9 89.79(8) 2_775 2_766 ? O2 Cd1 O9 90.21(8) 1_546 2_766 ? O9 Cd1 O9 180.00(10) . 2_766 ? O1 Cd2 O5 97.83(8) 1_546 1_556 ? O1 Cd2 O8 152.82(8) 1_546 . ? O5 Cd2 O8 97.09(8) 1_556 . ? O1 Cd2 O1W 80.39(8) 1_546 . ? O5 Cd2 O1W 177.19(8) 1_556 . ? O8 Cd2 O1W 85.40(8) . . ? O1 Cd2 O9 99.37(8) 1_546 . ? O5 Cd2 O9 99.94(8) 1_556 . ? O8 Cd2 O9 55.60(7) . . ? O1W Cd2 O9 82.53(8) . . ? O1 Cd2 Cl1 101.88(6) 1_546 . ? O5 Cd2 Cl1 93.62(6) 1_556 . ? O8 Cd2 Cl1 99.70(6) . . ? O1W Cd2 Cl1 84.66(5) . . ? O9 Cd2 Cl1 152.91(6) . . ? O1 Cd2 C33 126.63(7) 1_546 . ? O5 Cd2 C33 100.57(7) 1_556 . ? O8 Cd2 C33 27.43(7) . . ? O1W Cd2 C33 82.23(7) . . ? O9 Cd2 C33 28.20(7) . . ? Cl1 Cd2 C33 126.14(7) . . ? O12 Cd3 O20 100.29(8) . 1_554 ? O12 Cd3 O11 87.55(8) . . ? O20 Cd3 O11 170.20(8) 1_554 . ? O12 Cd3 O10 86.61(8) . . ? O20 Cd3 O10 81.42(8) 1_554 . ? O11 Cd3 O10 93.29(8) . . ? O12 Cd3 O16 86.48(7) . 1_545 ? O20 Cd3 O16 92.87(8) 1_554 1_545 ? O11 Cd3 O16 93.48(8) . 1_545 ? O10 Cd3 O16 170.11(7) . 1_545 ? O12 Cd3 Cl1 173.42(6) . . ? O20 Cd3 Cl1 85.84(6) 1_554 . ? O11 Cd3 Cl1 86.60(6) . . ? O10 Cd3 Cl1 96.72(5) . . ? O16 Cd3 Cl1 90.88(5) 1_545 . ? O19 Cd4 O13 103.02(8) 1_554 . ? O19 Cd4 O17 147.40(8) 1_554 1_545 ? O13 Cd4 O17 98.37(8) . 1_545 ? O19 Cd4 O2W 92.35(8) 1_554 . ? O13 Cd4 O2W 104.46(8) . . ? O17 Cd4 O2W 105.86(9) 1_545 . ? O19 Cd4 O16 102.14(7) 1_554 1_545 ? O13 Cd4 O16 98.68(7) . 1_545 ? O17 Cd4 O16 49.94(7) 1_545 1_545 ? O2W Cd4 O16 149.13(8) . 1_545 ? Cd2 Cl1 Cd3 129.53(3) . . ? C37 N1 C38 116.78(19) . . ? C37 N1 C39 117.0(2) . . ? C38 N1 C39 126.1(2) . . ? C36 N2 C34 123.59(19) . . ? C36 N2 C35 117.37(18) . . ? C34 N2 C35 118.52(17) . . ? C1 O1 Cd2 131.70(14) . 1_564 ? C1 O2 Cd1 142.23(15) . 1_564 ? C5 O3 C8 118.81(19) . . ? C19 O4 C16 117.19(18) . . ? C25 O5 Cd2 127.59(14) . 1_554 ? C25 O6 Cd1 145.05(15) . 1_554 ? C27 O7 C26 116.15(19) . . ? C33 O8 Cd2 92.67(14) . . ? C33 O9 Cd1 142.59(15) . . ? C33 O9 Cd2 89.45(14) . . ? Cd1 O9 Cd2 104.07(9) . . ? C36 O10 Cd3 120.37(14) . . ? C37 O11 Cd3 126.07(16) . . ? C40 O12 Cd3 150.76(16) . . ? C40 O13 Cd4 122.15(14) . . ? C44 O14 C47 116.49(17) . . ? C58 O15 C57 115.6(2) . . ? C64 O16 Cd3 153.9(2) . 1_565 ? C64 O16 Cd4 86.47(19) . 1_565 ? Cd3 O16 Cd4 96.65(7) 1_565 1_565 ? C64 O17 Cd4 105.6(2) . 1_565 ? C66 O18 C65 118.9(2) . . ? C72 O19 Cd4 130.0(2) . 1_556 ? C72 O20 Cd3 140.0(2) . 1_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 12.9(5) . . . . ? O1 C1 C2 C7 -166.1(3) . . . . ? O2 C1 C2 C3 -161.8(3) . . . . ? O1 C1 C2 C3 19.2(5) . . . . ? C7 C2 C3 C4 1.0(6) . . . . ? C1 C2 C3 C4 175.7(3) . . . . ? C2 C3 C4 C5 0.1(6) . . . . ? C3 C4 C5 O3 -178.1(3) . . . . ? C3 C4 C5 C6 -1.2(6) . . . . ? O3 C5 C6 C7 177.7(3) . . . . ? C4 C5 C6 C7 1.2(6) . . . . ? C3 C2 C7 C6 -1.0(5) . . . . ? C1 C2 C7 C6 -175.8(3) . . . . ? C5 C6 C7 C2 -0.1(6) . . . . ? O3 C8 C9 C14 93.4(3) . . . . ? O3 C8 C9 C10 -86.5(3) . . . . ? C14 C9 C10 C11 -0.8(5) . . . . ? C8 C9 C10 C11 179.0(3) . . . . ? C14 C9 C10 C17 178.6(3) . . . . ? C8 C9 C10 C17 -1.6(5) . . . . ? C9 C10 C11 C12 4.4(5) . . . . ? C17 C10 C11 C12 -175.0(3) . . . . ? C9 C10 C11 C26 -169.5(3) . . . . ? C17 C10 C11 C26 11.1(4) . . . . ? C10 C11 C12 C13 -3.6(5) . . . . ? C26 C11 C12 C13 170.4(3) . . . . ? C10 C11 C12 C18 175.3(3) . . . . ? C26 C11 C12 C18 -10.7(4) . . . . ? C11 C12 C13 C14 -0.7(5) . . . . ? C18 C12 C13 C14 -179.6(3) . . . . ? C11 C12 C13 C16 178.8(3) . . . . ? C18 C12 C13 C16 -0.1(5) . . . . ? C10 C9 C14 C13 -3.4(5) . . . . ? C8 C9 C14 C13 176.8(3) . . . . ? C10 C9 C14 C15 176.1(3) . . . . ? C8 C9 C14 C15 -3.7(4) . . . . ? C12 C13 C14 C9 4.2(5) . . . . ? C16 C13 C14 C9 -175.3(3) . . . . ? C12 C13 C14 C15 -175.3(3) . . . . ? C16 C13 C14 C15 5.2(4) . . . . ? C12 C13 C16 O4 93.6(3) . . . . ? C14 C13 C16 O4 -86.9(3) . . . . ? O4 C19 C20 C21 177.8(3) . . . . ? C24 C19 C20 C21 0.8(5) . . . . ? C19 C20 C21 C22 -0.4(5) . . . . ? C20 C21 C22 C23 -1.1(5) . . . . ? C20 C21 C22 C25 177.3(3) . . . . ? C21 C22 C23 C24 2.2(5) . . . . ? C25 C22 C23 C24 -176.3(3) . . . . ? C22 C23 C24 C19 -1.8(5) . . . . ? O4 C19 C24 C23 -176.5(3) . . . . ? C20 C19 C24 C23 0.3(5) . . . . ? C21 C22 C25 O5 -9.7(5) . . . . ? C23 C22 C25 O5 168.8(3) . . . . ? C21 C22 C25 O6 168.9(3) . . . . ? C23 C22 C25 O6 -12.7(5) . . . . ? C12 C11 C26 O7 87.4(3) . . . . ? C10 C11 C26 O7 -98.5(3) . . . . ? O7 C27 C28 C29 -179.8(3) . . . . ? C32 C27 C28 C29 -0.3(5) . . . . ? C27 C28 C29 C30 -1.6(5) . . . . ? C28 C29 C30 C31 2.3(5) . . . . ? C28 C29 C30 C33 -178.6(3) . . . . ? C29 C30 C31 C32 -1.1(5) . . . . ? C33 C30 C31 C32 179.7(3) . . . . ? O7 C27 C32 C31 -179.1(3) . . . . ? C28 C27 C32 C31 1.5(5) . . . . ? C30 C31 C32 C27 -0.7(5) . . . . ? C29 C30 C33 O8 3.2(5) . . . . ? C31 C30 C33 O8 -177.7(3) . . . . ? C29 C30 C33 O9 179.2(3) . . . . ? C31 C30 C33 O9 -1.7(5) . . . . ? C29 C30 C33 Cd2 81.1(18) . . . . ? C31 C30 C33 Cd2 -99.8(18) . . . . ? O12 C40 C41 C42 171.7(3) . . . . ? O13 C40 C41 C42 -8.2(4) . . . . ? O12 C40 C41 C46 -5.0(4) . . . . ? O13 C40 C41 C46 175.1(3) . . . . ? C46 C41 C42 C43 0.6(5) . . . . ? C40 C41 C42 C43 -176.1(3) . . . . ? C41 C42 C43 C44 -3.6(5) . . . . ? C42 C43 C44 O14 -177.7(3) . . . . ? C42 C43 C44 C45 4.6(5) . . . . ? O14 C44 C45 C46 -179.8(3) . . . . ? C43 C44 C45 C46 -2.4(5) . . . . ? C44 C45 C46 C41 -0.6(5) . . . . ? C42 C41 C46 C45 1.6(5) . . . . ? C40 C41 C46 C45 178.4(3) . . . . ? O14 C47 C48 C49 -91.7(3) . . . . ? O14 C47 C48 C53 86.6(3) . . . . ? C53 C48 C49 C50 7.3(4) . . . . ? C47 C48 C49 C50 -174.4(3) . . . . ? C53 C48 C49 C55 -172.8(2) . . . . ? C47 C48 C49 C55 5.5(4) . . . . ? C48 C49 C50 C51 -4.8(4) . . . . ? C55 C49 C50 C51 175.3(2) . . . . ? C48 C49 C50 C57 178.5(2) . . . . ? C55 C49 C50 C57 -1.4(4) . . . . ? C49 C50 C51 C52 -0.6(3) . . . . ? C57 C50 C51 C52 175.9(2) . . . . ? C49 C50 C51 C56 -179.1(2) . . . . ? C57 C50 C51 C56 -2.7(3) . . . . ? C50 C51 C52 C53 3.4(4) . . . . ? C56 C51 C52 C53 -178.0(3) . . . . ? C50 C51 C52 C65 -177.2(2) . . . . ? C56 C51 C52 C65 1.3(5) . . . . ? C51 C52 C53 C48 -0.9(4) . . . . ? C65 C52 C53 C48 179.8(2) . . . . ? C51 C52 C53 C54 177.4(3) . . . . ? C65 C52 C53 C54 -2.0(4) . . . . ? C49 C48 C53 C52 -4.5(3) . . . . ? C47 C48 C53 C52 177.2(2) . . . . ? C49 C48 C53 C54 177.3(2) . . . . ? C47 C48 C53 C54 -1.0(3) . . . . ? C49 C50 C57 O15 96.2(3) . . . . ? C51 C50 C57 O15 -80.4(3) . . . . ? C63 C58 C59 C60 -5.3(6) . . . . ? O15 C58 C59 C60 176.9(4) . . . . ? C58 C59 C60 C61 -6.3(6) . . . . ? C59 C60 C61 C62 11.3(6) . . . . ? C59 C60 C61 C64 -179.1(3) . . . . ? C60 C61 C62 C63 -5.8(7) . . . . ? C64 C61 C62 C63 -175.6(4) . . . . ? C60 C61 C62 O14W -99.4(4) . . . 2_676 ? C64 C61 C62 O14W 90.8(4) . . . 2_676 ? C59 C58 C63 C62 10.8(7) . . . . ? O15 C58 C63 C62 -171.1(4) . . . . ? C61 C62 C63 C58 -5.4(7) . . . . ? O14W C62 C63 C58 75.8(5) 2_676 . . . ? C62 C61 C64 O16 -171.1(4) . . . . ? C60 C61 C64 O16 20.0(6) . . . . ? C62 C61 C64 O17 6.9(6) . . . . ? C60 C61 C64 O17 -162.0(4) . . . . ? C51 C52 C65 O18 -93.5(3) . . . . ? C53 C52 C65 O18 85.9(4) . . . . ? O18 C66 C67 C68 178.6(3) . . . . ? C71 C66 C67 C68 1.9(5) . . . . ? C66 C67 C68 C69 -1.1(5) . . . . ? C67 C68 C69 C70 0.9(5) . . . . ? C67 C68 C69 C72 -176.9(3) . . . . ? C68 C69 C70 C71 -1.5(5) . . . . ? C72 C69 C70 C71 176.2(3) . . . . ? C69 C70 C71 C66 2.2(5) . . . . ? C67 C66 C71 C70 -2.4(5) . . . . ? O18 C66 C71 C70 -179.4(3) . . . . ? C70 C69 C72 O20 0.4(4) . . . . ? C68 C69 C72 O20 178.1(3) . . . . ? C70 C69 C72 O19 177.5(3) . . . . ? C68 C69 C72 O19 -4.8(4) . . . . ? O8 C33 Cd2 O1 166.86(14) . . . 1_546 ? O9 C33 Cd2 O1 -16.80(18) . . . 1_546 ? C30 C33 Cd2 O1 85.0(18) . . . 1_546 ? O8 C33 Cd2 O5 -85.00(14) . . . 1_556 ? O9 C33 Cd2 O5 91.35(13) . . . 1_556 ? C30 C33 Cd2 O5 -166.8(18) . . . 1_556 ? O9 C33 Cd2 O8 176.3(3) . . . . ? C30 C33 Cd2 O8 -81.8(18) . . . . ? O8 C33 Cd2 O1W 95.00(14) . . . . ? O9 C33 Cd2 O1W -88.66(13) . . . . ? C30 C33 Cd2 O1W 13.2(18) . . . . ? O8 C33 Cd2 O9 -176.3(3) . . . . ? C30 C33 Cd2 O9 101.8(18) . . . . ? O8 C33 Cd2 Cl1 17.47(18) . . . . ? O9 C33 Cd2 Cl1 -166.19(12) . . . . ? C30 C33 Cd2 Cl1 -64.4(18) . . . . ? O1 Cd2 Cl1 Cd3 117.29(7) 1_546 . . . ? O5 Cd2 Cl1 Cd3 18.51(7) 1_556 . . . ? O8 Cd2 Cl1 Cd3 -79.32(7) . . . . ? O1W Cd2 Cl1 Cd3 -163.72(6) . . . . ? O9 Cd2 Cl1 Cd3 -101.73(13) . . . . ? C33 Cd2 Cl1 Cd3 -87.38(8) . . . . ? O12 Cd3 Cl1 Cd2 -102.6(5) . . . . ? O20 Cd3 Cl1 Cd2 98.37(6) 1_554 . . . ? O11 Cd3 Cl1 Cd2 -75.39(7) . . . . ? O10 Cd3 Cl1 Cd2 17.53(7) . . . . ? O16 Cd3 Cl1 Cd2 -168.82(6) 1_545 . . . ? O11 C37 N1 C38 0.0(4) . . . . ? O11 C37 N1 C39 -175.2(3) . . . . ? O10 C36 N2 C34 -176.3(2) . . . . ? O10 C36 N2 C35 -4.7(4) . . . . ? O2 C1 O1 Cd2 4.4(4) . . . 1_564 ? C2 C1 O1 Cd2 -176.60(18) . . . 1_564 ? O1 C1 O2 Cd1 10.0(5) . . . 1_564 ? C2 C1 O2 Cd1 -168.88(18) . . . 1_564 ? C6 C5 O3 C8 -5.0(5) . . . . ? C4 C5 O3 C8 171.7(3) . . . . ? C9 C8 O3 C5 -159.9(2) . . . . ? C24 C19 O4 C16 -6.8(4) . . . . ? C20 C19 O4 C16 176.3(3) . . . . ? C13 C16 O4 C19 178.7(2) . . . . ? O6 C25 O5 Cd2 19.9(4) . . . 1_554 ? C22 C25 O5 Cd2 -161.64(18) . . . 1_554 ? O5 C25 O6 Cd1 -10.4(5) . . . 1_554 ? C22 C25 O6 Cd1 171.16(19) . . . 1_554 ? C32 C27 O7 C26 165.0(3) . . . . ? C28 C27 O7 C26 -15.5(4) . . . . ? C11 C26 O7 C27 172.2(2) . . . . ? O9 C33 O8 Cd2 -3.8(3) . . . . ? C30 C33 O8 Cd2 172.0(3) . . . . ? O1 Cd2 O8 C33 -23.5(3) 1_546 . . . ? O5 Cd2 O8 C33 99.31(15) 1_556 . . . ? O1W Cd2 O8 C33 -81.99(15) . . . . ? O9 Cd2 O8 C33 2.09(15) . . . . ? Cl1 Cd2 O8 C33 -165.76(15) . . . . ? O8 C33 O9 Cd1 -109.1(3) . . . . ? C30 C33 O9 Cd1 75.1(4) . . . . ? Cd2 C33 O9 Cd1 -112.8(3) . . . . ? O8 C33 O9 Cd2 3.7(3) . . . . ? C30 C33 O9 Cd2 -172.1(3) . . . . ? O6 Cd1 O9 C33 -112.4(2) 2_765 . . . ? O6 Cd1 O9 C33 67.6(2) 1_556 . . . ? O2 Cd1 O9 C33 -22.5(2) 2_775 . . . ? O2 Cd1 O9 C33 157.5(2) 1_546 . . . ? O9 Cd1 O9 C33 119(100) 2_766 . . . ? O6 Cd1 O9 Cd2 139.40(9) 2_765 . . . ? O6 Cd1 O9 Cd2 -40.60(9) 1_556 . . . ? O2 Cd1 O9 Cd2 -130.61(9) 2_775 . . . ? O2 Cd1 O9 Cd2 49.39(9) 1_546 . . . ? O9 Cd1 O9 Cd2 11(100) 2_766 . . . ? O1 Cd2 O9 C33 166.41(15) 1_546 . . . ? O5 Cd2 O9 C33 -93.86(15) 1_556 . . . ? O8 Cd2 O9 C33 -2.04(15) . . . . ? O1W Cd2 O9 C33 87.49(15) . . . . ? Cl1 Cd2 O9 C33 25.1(2) . . . . ? O1 Cd2 O9 Cd1 -48.86(9) 1_546 . . . ? O5 Cd2 O9 Cd1 50.88(9) 1_556 . . . ? O8 Cd2 O9 Cd1 142.70(13) . . . . ? O1W Cd2 O9 Cd1 -127.77(9) . . . . ? Cl1 Cd2 O9 Cd1 169.79(6) . . . . ? C33 Cd2 O9 Cd1 144.74(17) . . . . ? N2 C36 O10 Cd3 157.24(18) . . . . ? O12 Cd3 O10 C36 -148.99(17) . . . . ? O20 Cd3 O10 C36 -48.04(17) 1_554 . . . ? O11 Cd3 O10 C36 123.66(17) . . . . ? O16 Cd3 O10 C36 -103.2(4) 1_545 . . . ? Cl1 Cd3 O10 C36 36.70(17) . . . . ? N1 C37 O11 Cd3 169.66(17) . . . . ? O12 Cd3 O11 C37 -159.5(2) . . . . ? O20 Cd3 O11 C37 -16.1(6) 1_554 . . . ? O10 Cd3 O11 C37 -73.1(2) . . . . ? O16 Cd3 O11 C37 114.1(2) 1_545 . . . ? Cl1 Cd3 O11 C37 23.5(2) . . . . ? O13 C40 O12 Cd3 -18.3(6) . . . . ? C41 C40 O12 Cd3 161.9(2) . . . . ? O20 Cd3 O12 C40 61.5(3) 1_554 . . . ? O11 Cd3 O12 C40 -124.4(3) . . . . ? O10 Cd3 O12 C40 142.1(3) . . . . ? O16 Cd3 O12 C40 -30.8(3) 1_545 . . . ? Cl1 Cd3 O12 C40 -97.2(6) . . . . ? O12 C40 O13 Cd4 16.6(4) . . . . ? C41 C40 O13 Cd4 -163.50(17) . . . . ? O19 Cd4 O13 C40 -80.51(17) 1_554 . . . ? O17 Cd4 O13 C40 74.73(17) 1_545 . . . ? O2W Cd4 O13 C40 -176.42(17) . . . . ? O16 Cd4 O13 C40 24.19(17) 1_545 . . . ? C43 C44 O14 C47 -175.0(3) . . . . ? C45 C44 O14 C47 2.6(4) . . . . ? C48 C47 O14 C44 175.2(2) . . . . ? C59 C58 O15 C57 5.4(6) . . . . ? C63 C58 O15 C57 -172.5(4) . . . . ? C50 C57 O15 C58 -163.8(3) . . . . ? O17 C64 O16 Cd3 96.8(5) . . . 1_565 ? C61 C64 O16 Cd3 -85.2(5) . . . 1_565 ? O17 C64 O16 Cd4 -1.2(3) . . . 1_565 ? C61 C64 O16 Cd4 176.8(3) . . . 1_565 ? O16 C64 O17 Cd4 1.4(4) . . . 1_565 ? C61 C64 O17 Cd4 -176.6(3) . . . 1_565 ? C67 C66 O18 C65 -0.5(5) . . . . ? C71 C66 O18 C65 176.5(3) . . . . ? C52 C65 O18 C66 178.0(3) . . . . ? O20 C72 O19 Cd4 -11.3(5) . . . 1_556 ? C69 C72 O19 Cd4 171.90(18) . . . 1_556 ? O19 C72 O20 Cd3 -11.0(6) . . . 1_556 ? C69 C72 O20 Cd3 165.8(2) . . . 1_556 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.959 _refine_diff_density_min -0.940 _refine_diff_density_rms 0.064 data_3 _database_code_depnum_ccdc_archive 'CCDC 816747' #TrackingRef '- n (1-4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C144 H138 Co7 N4 O46, 2(O0.50), 2(O0.50), 5.2(O0.50), 4.8(O)' _chemical_formula_sum 'C144 H168 Co7 N4 O57' _chemical_formula_weight 3249.10 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.2234(12) _cell_length_b 17.3461(12) _cell_length_c 20.4722(16) _cell_angle_alpha 67.0710(10) _cell_angle_beta 76.394(2) _cell_angle_gamma 64.9000(10) _cell_volume 4492.8(6) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1353 _cell_measurement_theta_min 2.184 _cell_measurement_theta_max 17.449 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1675.0 _exptl_absorpt_coefficient_mu 0.707 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8266 _exptl_absorpt_correction_T_max 0.8600 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24558 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.00 _reflns_number_total 17287 _reflns_number_gt 13562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+2.4302P] 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 17287 _refine_ls_number_parameters 1032 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.35722(19) 0.83995(18) 1.49052(13) 0.0427(6) Uani 1 1 d . . . C2 C 0.36222(18) 0.88595(16) 1.41285(13) 0.0388(6) Uani 1 1 d . . . C3 C 0.45134(17) 0.88040(16) 1.37236(12) 0.0348(5) Uani 1 1 d . . . H3 H 0.5105 0.8447 1.3946 0.042 Uiso 1 1 calc R . . C4 C 0.45351(18) 0.92591(16) 1.30126(13) 0.0374(5) Uani 1 1 d . . . H4 H 0.5138 0.9271 1.2753 0.045 Uiso 1 1 calc R . . C5 C 0.37005(17) 0.97029(16) 1.26611(12) 0.0349(5) Uani 1 1 d . . . C6 C 0.28241(18) 0.97448(16) 1.30328(13) 0.0384(6) Uani 1 1 d . . . H6 H 0.2249 1.0033 1.2790 0.046 Uiso 1 1 calc R . . C7 C 0.27739(18) 0.93642(16) 1.37696(13) 0.0388(6) Uani 1 1 d . . . H7 H 0.2156 0.9447 1.4033 0.047 Uiso 1 1 calc R . . C8 C 0.29652(18) 1.05207(17) 1.15723(13) 0.0413(6) Uani 1 1 d . . . H8A H 0.2519 1.1074 1.1684 0.050 Uiso 1 1 calc R . . H8B H 0.2614 1.0109 1.1692 0.050 Uiso 1 1 calc R . . C9 C 0.33622(17) 1.07503(16) 1.07787(12) 0.0344(5) Uani 1 1 d . . . C10 C 0.35215(17) 1.01866(16) 1.03858(12) 0.0360(5) Uani 1 1 d . . . C11 C 0.38563(17) 1.04600(16) 0.96494(12) 0.0345(5) Uani 1 1 d . . . C12 C 0.40177(17) 1.12488(16) 0.93419(13) 0.0364(5) Uani 1 1 d . . . C13 C 0.38795(18) 1.17734(16) 0.97473(13) 0.0373(6) Uani 1 1 d . . . C14 C 0.35709(18) 1.15139(16) 1.04635(13) 0.0386(6) Uani 1 1 d . . . C15 C 0.33257(17) 1.21370(16) 1.08985(13) 0.0364(5) Uani 1 1 d . . . H15B H 0.3615 1.1786 1.1355 0.055 Uiso 1 1 calc R . . H15C H 0.2618 1.2411 1.0984 0.055 Uiso 1 1 calc R . . H15A H 0.3588 1.2612 1.0634 0.055 Uiso 1 1 calc R . . C16 C 0.33358(18) 0.92858(16) 1.07091(13) 0.0383(6) Uani 1 1 d . . . H16B H 0.2837 0.9325 1.0457 0.058 Uiso 1 1 calc R . . H16C H 0.3113 0.9182 1.1215 0.058 Uiso 1 1 calc R . . H16A H 0.3941 0.8785 1.0658 0.058 Uiso 1 1 calc R . . C17 C 0.40540(17) 0.98778(16) 0.92024(13) 0.0358(5) Uani 1 1 d . . . H17A H 0.4603 0.9932 0.8839 0.043 Uiso 1 1 calc R . . H17B H 0.4224 0.9238 0.9505 0.043 Uiso 1 1 calc R . . C18 C 0.42629(17) 1.15805(16) 0.85431(12) 0.0351(5) Uani 1 1 d . . . H18A H 0.4023 1.2241 0.8369 0.053 Uiso 1 1 calc R . . H18B H 0.3954 1.1377 0.8307 0.053 Uiso 1 1 calc R . . H18C H 0.4970 1.1338 0.8437 0.053 Uiso 1 1 calc R . . C19 C 0.41964(18) 1.25693(17) 0.93924(13) 0.0403(6) Uani 1 1 d . . . H19A H 0.4415 1.2710 0.9736 0.048 Uiso 1 1 calc R . . H19B H 0.4713 1.2480 0.9001 0.048 Uiso 1 1 calc R . . C20 C 0.32772(17) 1.40372(15) 0.85943(12) 0.0315(5) Uani 1 1 d . . . C21 C 0.41076(18) 1.42487(16) 0.83794(12) 0.0359(5) Uani 1 1 d . . . H21 H 0.4691 1.3848 0.8604 0.043 Uiso 1 1 calc R . . C22 C 0.40843(18) 1.50469(16) 0.78362(13) 0.0366(5) Uani 1 1 d . . . H22 H 0.4652 1.5191 0.7689 0.044 Uiso 1 1 calc R . . C23 C 0.32307(19) 1.56336(18) 0.75079(13) 0.0435(6) Uani 1 1 d . . . C24 C 0.24003(19) 1.54221(16) 0.77228(14) 0.0424(6) Uani 1 1 d . . . H24 H 0.1817 1.5823 0.7498 0.051 Uiso 1 1 calc R . . C25 C 0.24236(19) 1.46239(18) 0.82660(14) 0.0463(7) Uani 1 1 d . . . H25 H 0.1856 1.4479 0.8413 0.056 Uiso 1 1 calc R . . C26 C 0.32549(18) 1.64639(16) 0.69158(12) 0.0356(5) Uani 1 1 d . . . C27 C 0.32177(17) 0.98423(16) 0.83690(13) 0.0339(5) Uani 1 1 d . . . C28 C 0.40399(19) 0.92028(17) 0.81550(13) 0.0419(6) Uani 1 1 d . . . H28 H 0.4642 0.9000 0.8345 0.050 Uiso 1 1 calc R . . C29 C 0.39818(18) 0.88600(17) 0.76624(13) 0.0396(6) Uani 1 1 d . . . H29 H 0.4544 0.8423 0.7516 0.048 Uiso 1 1 calc R . . C30 C 0.31014(17) 0.91569(16) 0.73838(13) 0.0352(5) Uani 1 1 d . . . C31 C 0.22791(17) 0.97965(16) 0.75978(13) 0.0351(5) Uani 1 1 d . . . H31 H 0.1677 0.9999 0.7407 0.042 Uiso 1 1 calc R . . C32 C 0.23373(17) 1.01392(16) 0.80904(12) 0.0335(5) Uani 1 1 d . . . H32 H 0.1775 1.0576 0.8237 0.040 Uiso 1 1 calc R . . C33 C 0.29980(18) 0.87928(16) 0.68686(13) 0.0370(5) Uani 1 1 d . . . C34 C 0.81562(17) 0.62614(15) 0.40510(11) 0.0304(5) Uani 1 1 d . . . C35 C 0.84648(17) 0.65196(15) 0.32774(11) 0.0317(5) Uani 1 1 d . . . C36 C 0.93176(17) 0.59627(16) 0.30101(12) 0.0355(5) Uani 1 1 d . . . H36 H 0.9727 0.5425 0.3326 0.043 Uiso 1 1 calc R . . C37 C 0.95711(17) 0.61920(15) 0.22809(12) 0.0315(5) Uani 1 1 d . . . H37 H 1.0154 0.5811 0.2098 0.038 Uiso 1 1 calc R . . C38 C 0.89717(18) 0.69784(16) 0.18190(12) 0.0356(5) Uani 1 1 d . . . C39 C 0.81189(18) 0.75354(17) 0.20864(13) 0.0409(6) Uani 1 1 d . . . H39 H 0.7709 0.8073 0.1771 0.049 Uiso 1 1 calc R . . C40 C 0.78654(18) 0.73060(16) 0.28156(12) 0.0359(5) Uani 1 1 d . . . H40 H 0.7283 0.7687 0.2998 0.043 Uiso 1 1 calc R . . C41 C 0.85976(18) 0.78347(17) 0.05969(12) 0.0382(6) Uani 1 1 d . . . H41A H 0.8257 0.8392 0.0725 0.046 Uiso 1 1 calc R . . H41B H 0.8108 0.7586 0.0622 0.046 Uiso 1 1 calc R . . C42 C 0.90652(17) 0.80518(15) -0.01346(12) 0.0308(5) Uani 1 1 d . . . C43 C 0.92349(17) 0.75503(16) -0.05662(12) 0.0322(5) Uani 1 1 d . . . C44 C 0.95506(17) 0.78591(16) -0.12765(12) 0.0327(5) Uani 1 1 d . . . C45 C 0.96699(18) 0.87002(16) -0.15720(13) 0.0370(5) Uani 1 1 d . . . C46 C 0.95458(17) 0.91534(15) -0.11221(12) 0.0318(5) Uani 1 1 d . . . C47 C 0.92716(16) 0.88390(15) -0.04047(12) 0.0292(5) Uani 1 1 d . . . C48 C 0.90972(18) 0.66565(15) -0.02597(12) 0.0338(5) Uani 1 1 d . . . H48A H 0.9626 0.6206 0.0040 0.051 Uiso 1 1 calc R . . H48B H 0.9105 0.6457 -0.0648 0.051 Uiso 1 1 calc R . . H48C H 0.8472 0.6729 0.0028 0.051 Uiso 1 1 calc R . . C49 C 0.97477(17) 0.73397(16) -0.17902(13) 0.0354(5) Uani 1 1 d . . . H49A H 1.0281 0.7437 -0.2156 0.042 Uiso 1 1 calc R . . H49B H 0.9937 0.6686 -0.1527 0.042 Uiso 1 1 calc R . . C50 C 0.98914(18) 0.91170(16) -0.23734(12) 0.0355(5) Uani 1 1 d . . . H50A H 0.9622 0.9776 -0.2506 0.053 Uiso 1 1 calc R . . H50B H 0.9596 0.8934 -0.2636 0.053 Uiso 1 1 calc R . . H50C H 1.0598 0.8907 -0.2490 0.053 Uiso 1 1 calc R . . C51 C 0.97578(17) 1.00168(15) -0.14323(13) 0.0362(5) Uani 1 1 d . . . H51A H 0.9976 1.0115 -0.1063 0.043 Uiso 1 1 calc R . . H51B H 1.0276 0.9978 -0.1828 0.043 Uiso 1 1 calc R . . C52 C 0.91258(17) 0.93423(16) 0.00943(13) 0.0353(5) Uani 1 1 d . . . H52A H 0.9588 0.9649 -0.0057 0.053 Uiso 1 1 calc R . . H52B H 0.9236 0.8916 0.0579 0.053 Uiso 1 1 calc R . . H52C H 0.8459 0.9789 0.0085 0.053 Uiso 1 1 calc R . . C53 C 0.89218(19) 1.15118(17) -0.21807(13) 0.0452(7) Uani 1 1 d . . . C54 C 0.97712(18) 1.16748(16) -0.24825(12) 0.0357(5) Uani 1 1 d . . . H54 H 1.0384 1.1225 -0.2334 0.043 Uiso 1 1 calc R . . C55 C 0.97240(19) 1.24955(16) -0.30020(12) 0.0392(6) Uani 1 1 d . . . H55 H 1.0305 1.2607 -0.3208 0.047 Uiso 1 1 calc R . . C56 C 0.88274(18) 1.31531(17) -0.32196(13) 0.0392(6) Uani 1 1 d . . . C57 C 0.79779(19) 1.29900(17) -0.29178(13) 0.0450(7) Uani 1 1 d . . . H57 H 0.7365 1.3439 -0.3067 0.054 Uiso 1 1 calc R . . C58 C 0.8025(2) 1.21694(17) -0.23984(13) 0.0489(7) Uani 1 1 d . . . H58 H 0.7445 1.2058 -0.2192 0.059 Uiso 1 1 calc R . . C59 C 0.87678(17) 1.40100(16) -0.38060(12) 0.0349(5) Uani 1 1 d . . . C60 C 0.88784(17) 0.73752(16) -0.26329(12) 0.0332(5) Uani 1 1 d . . . C61 C 0.97065(18) 0.67878(16) -0.28975(13) 0.0346(5) Uani 1 1 d . . . H61 H 1.0315 0.6577 -0.2713 0.042 Uiso 1 1 calc R . . C62 C 0.96443(17) 0.65086(16) -0.34329(12) 0.0327(5) Uani 1 1 d . . . H62 H 1.0225 0.6166 -0.3647 0.039 Uiso 1 1 calc R . . C63 C 0.87843(17) 0.67123(16) -0.36527(12) 0.0329(5) Uani 1 1 d . . . C64 C 0.79382(17) 0.72969(15) -0.33904(12) 0.0302(5) Uani 1 1 d . . . H64 H 0.7328 0.7477 -0.3561 0.036 Uiso 1 1 calc R . . C65 C 0.79972(18) 0.76048(16) -0.28898(13) 0.0362(5) Uani 1 1 d . . . H65 H 0.7417 0.7990 -0.2708 0.043 Uiso 1 1 calc R . . C66 C 0.87109(17) 0.63273(15) -0.41624(12) 0.0289(5) Uani 1 1 d . . . C67 C 0.62828(18) 0.61796(15) 0.72242(13) 0.0333(5) Uani 1 1 d . . . H67 H 0.6597 0.5932 0.6852 0.040 Uiso 1 1 calc R . . C68 C 0.7743(2) 0.52493(18) 0.78461(14) 0.0476(7) Uani 1 1 d . . . H68A H 0.7875 0.4873 0.7554 0.071 Uiso 1 1 calc R . . H68B H 0.7832 0.4868 0.8345 0.071 Uiso 1 1 calc R . . H68C H 0.8194 0.5569 0.7680 0.071 Uiso 1 1 calc R . . C69 C 0.63796(18) 0.62244(16) 0.83660(13) 0.0362(5) Uani 1 1 d . . . H69A H 0.6382 0.6833 0.8222 0.054 Uiso 1 1 calc R . . H69B H 0.6777 0.5828 0.8769 0.054 Uiso 1 1 calc R . . H69C H 0.5710 0.6246 0.8507 0.054 Uiso 1 1 calc R . . C70 C 0.60849(17) 0.82118(15) 0.52657(12) 0.0314(5) Uani 1 1 d . . . H70 H 0.6211 0.7790 0.5035 0.038 Uiso 1 1 calc R . . C71 C 0.70510(19) 0.88816(17) 0.42667(13) 0.0387(6) Uani 1 1 d . . . H71A H 0.7365 0.8272 0.4236 0.058 Uiso 1 1 calc R . . H71B H 0.7551 0.9111 0.4241 0.058 Uiso 1 1 calc R . . H71C H 0.6639 0.9279 0.3871 0.058 Uiso 1 1 calc R . . C72 C 0.62863(19) 0.95512(16) 0.52613(13) 0.0356(5) Uani 1 1 d . . . H72A H 0.5776 0.9539 0.5655 0.053 Uiso 1 1 calc R . . H72B H 0.6088 1.0147 0.4894 0.053 Uiso 1 1 calc R . . H72C H 0.6893 0.9429 0.5438 0.053 Uiso 1 1 calc R . . Co1 Co 1.0000 0.5000 0.5000 0.02843(10) Uani 1 2 d S . . Co2 Co 0.21643(3) 0.82821(2) 0.617563(18) 0.03806(8) Uani 1 1 d . . . Co3 Co 0.47597(2) 0.73515(2) 0.621247(17) 0.03045(7) Uani 1 1 d . . . Co4 Co 0.75155(2) 0.57851(2) 0.531951(15) 0.02949(7) Uani 1 1 d . . . N1 N 0.67704(15) 0.58855(13) 0.77868(11) 0.0381(5) Uani 1 1 d . . . N2 N 0.64404(15) 0.88567(13) 0.49549(10) 0.0347(4) Uani 1 1 d . . . O1 O 0.26948(12) 0.85769(11) 1.52054(9) 0.0392(4) Uani 1 1 d . . . O2 O 0.43009(12) 0.79203(10) 1.52158(8) 0.0317(3) Uani 1 1 d . . . O3 O 0.38282(12) 1.00866(11) 1.19545(8) 0.0387(4) Uani 1 1 d . . . O4 O 0.32425(11) 1.32703(10) 0.91216(8) 0.0302(3) Uani 1 1 d . . . O5 O 0.40441(11) 1.65103(10) 0.66340(8) 0.0316(3) Uani 1 1 d . . . O6 O 0.24317(13) 1.70551(11) 0.67871(9) 0.0426(4) Uani 1 1 d . . . O7 O 0.31745(11) 1.01929(10) 0.88647(8) 0.0347(4) Uani 1 1 d . . . O8 O 0.21753(13) 0.90033(11) 0.66920(9) 0.0395(4) Uani 1 1 d . . . O9 O 0.37284(12) 0.82442(11) 0.66347(9) 0.0339(4) Uani 1 1 d . . . O10 O 0.54691(12) 0.67389(11) 0.71516(8) 0.0344(4) Uani 1 1 d . . . O11 O 0.55931(12) 0.81355(10) 0.58464(8) 0.0326(4) Uani 1 1 d . . . O12 O 0.07957(12) 0.85348(11) 0.60361(9) 0.0364(4) Uani 1 1 d . . . H12A H 0.0438 0.8582 0.6410 0.055 Uiso 1 1 calc R . . O13 O 0.73232(11) 0.67589(10) 0.42651(7) 0.0281(3) Uani 1 1 d . . . O14 O 0.86577(11) 0.55733(10) 0.44887(8) 0.0297(3) Uani 1 1 d . . . O15 O 0.93195(12) 0.71800(11) 0.11006(8) 0.0374(4) Uani 1 1 d . . . O16 O 0.88706(12) 1.07405(11) -0.16856(9) 0.0435(4) Uani 1 1 d . . . O17 O 0.79473(11) 1.46536(10) -0.38708(8) 0.0299(3) Uani 1 1 d . . . O18 O 0.95462(12) 1.40429(11) -0.42034(8) 0.0383(4) Uani 1 1 d . . . O19 O 0.88628(12) 0.76788(11) -0.21173(8) 0.0336(4) Uani 1 1 d . . . O20 O 0.94815(11) 0.58444(11) -0.43974(8) 0.0332(4) Uani 1 1 d . . . O21 O 0.78609(11) 0.65198(10) -0.43094(8) 0.0303(3) Uani 1 1 d . . . O1W O 0.59698(11) 0.62994(10) 0.57789(8) 0.0305(3) Uani 1 1 d . . . O2W O 0.70177(12) 0.51095(10) 0.49812(8) 0.0322(3) Uani 1 1 d . . . O3W O 0.5229(2) 0.5099(2) 0.61349(18) 0.0447(9) Uani 0.50 1 d P . . O4W O 0.8311(3) 0.3690(2) 0.47979(19) 0.0424(8) Uani 0.50 1 d P . . O5W O 0.2838(4) 0.6907(4) 0.9534(3) 0.0423(14) Uani 0.30 1 d P . . O6W O 0.6891(3) 0.3156(3) 0.5088(2) 0.0331(9) Uani 0.40 1 d P . . O7W O 0.3725(5) 0.5871(4) 0.1582(3) 0.0565(18) Uani 0.30 1 d P . . O8W O 0.9824(2) 0.87892(18) 0.43455(14) 0.0339(6) Uani 0.60 1 d P . . O9W O 0.2597(3) 0.6696(3) 0.8577(2) 0.0364(9) Uani 0.40 1 d P . . O10W O 0.4481(2) 0.3911(2) 0.64808(15) 0.0418(7) Uani 0.60 1 d P . . O11W O 0.5570(4) 0.3074(4) 0.7405(3) 0.0444(15) Uani 0.30 1 d P . . O12W O 0.5000 0.5000 0.0000 0.0406(7) Uani 0.80 2 d SP . . O13W O 0.8230(4) 0.3152(4) 0.9085(3) 0.0429(14) Uani 0.30 1 d P . . O14W O 0.1718(3) 0.4870(3) 0.0330(2) 0.0412(10) Uani 0.40 1 d P . . O15W O 0.7238(2) 0.2440(2) 0.96433(17) 0.0378(8) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0338(14) 0.0510(15) 0.0330(13) -0.0045(11) -0.0040(10) -0.0142(12) C2 0.0321(13) 0.0330(12) 0.0386(13) 0.0063(10) -0.0057(10) -0.0153(10) C3 0.0305(12) 0.0404(13) 0.0344(12) -0.0066(10) -0.0061(10) -0.0174(11) C4 0.0317(13) 0.0412(13) 0.0359(13) -0.0035(10) -0.0028(10) -0.0188(11) C5 0.0305(12) 0.0412(13) 0.0287(12) -0.0062(10) 0.0021(9) -0.0166(11) C6 0.0286(12) 0.0391(13) 0.0345(13) 0.0045(10) -0.0031(10) -0.0155(11) C7 0.0270(12) 0.0388(13) 0.0335(13) 0.0029(10) 0.0013(10) -0.0120(10) C8 0.0305(13) 0.0356(13) 0.0337(13) -0.0011(10) -0.0003(10) -0.0010(10) C9 0.0264(12) 0.0363(13) 0.0313(12) -0.0023(10) -0.0046(9) -0.0100(10) C10 0.0303(12) 0.0384(13) 0.0306(12) -0.0011(10) -0.0100(10) -0.0102(10) C11 0.0266(12) 0.0380(13) 0.0323(12) -0.0067(10) -0.0044(9) -0.0094(10) C12 0.0298(12) 0.0316(12) 0.0324(12) 0.0020(10) -0.0126(10) -0.0036(10) C13 0.0348(13) 0.0348(13) 0.0318(12) 0.0029(10) -0.0090(10) -0.0127(11) C14 0.0340(13) 0.0316(12) 0.0360(13) -0.0039(10) -0.0019(10) -0.0064(10) C15 0.0287(12) 0.0395(13) 0.0390(13) -0.0069(10) -0.0200(10) -0.0073(10) C16 0.0318(13) 0.0393(13) 0.0367(13) -0.0029(11) -0.0077(10) -0.0128(11) C17 0.0280(12) 0.0353(12) 0.0345(13) -0.0084(10) -0.0125(10) -0.0008(10) C18 0.0282(12) 0.0351(12) 0.0374(13) -0.0050(10) 0.0023(10) -0.0165(10) C19 0.0357(14) 0.0423(14) 0.0373(13) 0.0025(11) -0.0118(11) -0.0189(11) C20 0.0332(12) 0.0323(12) 0.0354(12) -0.0085(10) -0.0134(10) -0.0149(10) C21 0.0334(13) 0.0335(12) 0.0360(13) 0.0022(10) -0.0133(10) -0.0149(10) C22 0.0321(13) 0.0358(13) 0.0384(13) -0.0013(10) -0.0091(10) -0.0161(11) C23 0.0387(14) 0.0470(15) 0.0343(13) 0.0115(11) -0.0168(11) -0.0215(12) C24 0.0325(13) 0.0336(13) 0.0473(15) 0.0074(11) -0.0123(11) -0.0138(11) C25 0.0328(14) 0.0430(14) 0.0481(15) 0.0098(12) -0.0130(11) -0.0179(12) C26 0.0400(14) 0.0340(12) 0.0269(12) -0.0078(10) 0.0060(10) -0.0148(11) C27 0.0244(11) 0.0337(12) 0.0370(13) -0.0155(10) -0.0024(10) -0.0015(10) C28 0.0333(13) 0.0407(14) 0.0343(13) -0.0162(11) 0.0040(10) 0.0019(11) C29 0.0281(12) 0.0418(14) 0.0405(14) -0.0192(11) 0.0105(10) -0.0071(11) C30 0.0294(12) 0.0381(13) 0.0358(13) -0.0167(10) 0.0170(10) -0.0167(10) C31 0.0294(12) 0.0402(13) 0.0363(13) -0.0173(11) 0.0041(10) -0.0126(10) C32 0.0303(12) 0.0333(12) 0.0347(12) -0.0143(10) -0.0045(10) -0.0061(10) C33 0.0360(13) 0.0377(13) 0.0376(13) -0.0134(11) 0.0114(10) -0.0205(11) C34 0.0338(12) 0.0326(12) 0.0230(11) -0.0015(9) -0.0052(9) -0.0162(10) C35 0.0320(12) 0.0348(12) 0.0242(11) -0.0026(9) -0.0037(9) -0.0144(10) C36 0.0312(12) 0.0397(13) 0.0277(12) -0.0042(10) -0.0065(10) -0.0101(10) C37 0.0270(12) 0.0337(12) 0.0292(11) -0.0108(9) -0.0090(9) -0.0033(10) C38 0.0336(13) 0.0336(12) 0.0280(12) -0.0018(10) -0.0040(10) -0.0086(10) C39 0.0310(13) 0.0354(13) 0.0305(12) 0.0030(10) -0.0038(10) -0.0006(10) C40 0.0367(13) 0.0351(12) 0.0271(12) -0.0040(10) -0.0043(10) -0.0099(11) C41 0.0329(13) 0.0376(13) 0.0293(12) 0.0054(10) -0.0051(10) -0.0132(11) C42 0.0305(12) 0.0314(12) 0.0290(11) -0.0075(9) -0.0004(9) -0.0134(10) C43 0.0327(12) 0.0378(12) 0.0349(12) -0.0075(10) -0.0132(10) -0.0196(10) C44 0.0288(12) 0.0408(13) 0.0329(12) -0.0129(10) -0.0041(9) -0.0153(10) C45 0.0368(13) 0.0370(13) 0.0334(13) -0.0110(10) -0.0018(10) -0.0115(11) C46 0.0329(12) 0.0340(12) 0.0283(11) -0.0046(9) -0.0031(9) -0.0171(10) C47 0.0275(11) 0.0328(12) 0.0281(11) -0.0062(9) -0.0050(9) -0.0141(10) C48 0.0385(13) 0.0335(12) 0.0339(12) -0.0090(10) -0.0107(10) -0.0155(11) C49 0.0298(12) 0.0386(13) 0.0402(13) -0.0162(11) -0.0066(10) -0.0102(10) C50 0.0318(13) 0.0400(13) 0.0337(13) -0.0135(10) 0.0036(10) -0.0145(11) C51 0.0317(12) 0.0334(12) 0.0357(13) 0.0048(10) -0.0084(10) -0.0168(10) C52 0.0302(12) 0.0385(13) 0.0406(13) -0.0173(11) -0.0003(10) -0.0134(11) C53 0.0354(14) 0.0403(14) 0.0328(13) 0.0122(11) 0.0009(10) -0.0133(11) C54 0.0372(13) 0.0320(12) 0.0292(12) 0.0017(10) -0.0031(10) -0.0154(11) C55 0.0362(13) 0.0365(13) 0.0283(12) 0.0064(10) -0.0043(10) -0.0129(11) C56 0.0311(13) 0.0381(13) 0.0333(13) 0.0077(10) -0.0048(10) -0.0154(11) C57 0.0330(13) 0.0397(14) 0.0357(13) 0.0143(11) 0.0037(10) -0.0170(11) C58 0.0386(14) 0.0387(14) 0.0354(14) 0.0172(11) 0.0015(11) -0.0123(12) C59 0.0301(12) 0.0382(13) 0.0246(11) 0.0087(10) -0.0062(9) -0.0170(11) C60 0.0340(13) 0.0370(13) 0.0332(12) -0.0180(10) -0.0028(10) -0.0117(10) C61 0.0354(13) 0.0341(12) 0.0395(13) -0.0199(10) -0.0042(10) -0.0098(10) C62 0.0331(13) 0.0384(13) 0.0294(12) -0.0166(10) -0.0011(10) -0.0118(10) C63 0.0358(13) 0.0360(12) 0.0327(12) -0.0153(10) -0.0028(10) -0.0151(11) C64 0.0314(12) 0.0312(12) 0.0340(12) -0.0133(10) -0.0064(9) -0.0128(10) C65 0.0356(13) 0.0369(13) 0.0376(13) -0.0189(11) -0.0079(10) -0.0063(11) C66 0.0305(12) 0.0298(11) 0.0324(12) -0.0142(9) -0.0011(9) -0.0138(10) C67 0.0347(13) 0.0314(12) 0.0333(12) -0.0019(10) -0.0093(10) -0.0164(11) C68 0.0431(15) 0.0396(14) 0.0377(14) -0.0107(11) -0.0140(12) 0.0087(12) C69 0.0362(13) 0.0354(13) 0.0429(14) -0.0168(11) -0.0134(11) -0.0100(11) C70 0.0351(13) 0.0299(12) 0.0343(13) -0.0112(10) -0.0051(10) -0.0150(10) C71 0.0374(14) 0.0357(13) 0.0410(14) -0.0130(11) 0.0076(11) -0.0170(11) C72 0.0421(14) 0.0331(12) 0.0401(13) -0.0142(10) -0.0098(11) -0.0164(11) Co1 0.0308(2) 0.0313(2) 0.0222(2) -0.00604(17) -0.00008(17) -0.01419(19) Co2 0.03635(19) 0.03729(18) 0.03572(18) -0.00401(14) -0.00530(14) -0.01534(15) Co3 0.03120(17) 0.03180(16) 0.03250(16) -0.00745(13) -0.00903(13) -0.01503(13) Co4 0.03143(17) 0.03259(16) 0.02241(15) -0.00425(12) -0.00038(12) -0.01534(13) N1 0.0372(12) 0.0325(10) 0.0446(12) -0.0146(9) -0.0147(9) -0.0054(9) N2 0.0375(11) 0.0324(10) 0.0366(11) -0.0133(9) 0.0000(9) -0.0152(9) O1 0.0357(9) 0.0377(9) 0.0371(9) -0.0035(7) -0.0044(7) -0.0145(8) O2 0.0357(9) 0.0354(8) 0.0330(8) -0.0100(7) -0.0086(7) -0.0196(7) O3 0.0378(10) 0.0341(9) 0.0297(8) 0.0024(7) -0.0027(7) -0.0121(8) O4 0.0353(9) 0.0305(8) 0.0335(8) -0.0135(7) -0.0080(7) -0.0148(7) O5 0.0329(9) 0.0312(8) 0.0352(9) -0.0064(7) -0.0090(7) -0.0170(7) O6 0.0432(10) 0.0381(9) 0.0369(9) -0.0047(8) -0.0055(8) -0.0122(8) O7 0.0281(8) 0.0328(8) 0.0330(9) -0.0127(7) -0.0076(7) 0.0022(7) O8 0.0384(10) 0.0377(9) 0.0368(9) -0.0045(7) -0.0040(7) -0.0157(8) O9 0.0328(9) 0.0346(9) 0.0400(9) -0.0135(7) -0.0045(7) -0.0159(7) O10 0.0309(9) 0.0391(9) 0.0361(9) -0.0114(7) -0.0083(7) -0.0136(8) O11 0.0334(9) 0.0360(9) 0.0339(9) -0.0139(7) -0.0018(7) -0.0162(7) O12 0.0396(10) 0.0355(9) 0.0382(9) -0.0142(8) -0.0088(7) -0.0127(8) O13 0.0337(8) 0.0313(8) 0.0235(7) -0.0060(6) -0.0069(6) -0.0163(7) O14 0.0341(9) 0.0305(8) 0.0230(7) -0.0045(6) -0.0023(6) -0.0145(7) O15 0.0296(9) 0.0367(9) 0.0327(9) 0.0008(7) -0.0019(7) -0.0115(7) O16 0.0278(9) 0.0373(9) 0.0413(10) 0.0122(8) -0.0008(7) -0.0139(7) O17 0.0321(9) 0.0322(8) 0.0230(8) -0.0038(6) 0.0000(6) -0.0158(7) O18 0.0341(9) 0.0338(9) 0.0315(9) 0.0025(7) -0.0008(7) -0.0114(7) O19 0.0335(9) 0.0356(9) 0.0350(9) -0.0177(7) -0.0026(7) -0.0106(7) O20 0.0307(9) 0.0346(9) 0.0339(9) -0.0148(7) 0.0021(7) -0.0113(7) O21 0.0291(8) 0.0352(8) 0.0259(8) -0.0062(6) -0.0006(6) -0.0157(7) O1W 0.0300(8) 0.0328(8) 0.0322(8) -0.0086(7) -0.0065(7) -0.0148(7) O2W 0.0347(9) 0.0350(8) 0.0257(8) -0.0057(7) 0.0003(7) -0.0174(7) O3W 0.0336(19) 0.0353(18) 0.042(2) 0.0125(15) -0.0067(15) -0.0122(15) O4W 0.0360(19) 0.0396(19) 0.045(2) -0.0154(16) 0.0105(16) -0.0137(16) O5W 0.034(3) 0.033(3) 0.038(3) -0.004(2) 0.009(2) -0.006(2) O6W 0.035(2) 0.034(2) 0.038(2) -0.0219(18) -0.0106(18) -0.0077(18) O7W 0.047(4) 0.046(4) 0.045(4) 0.018(3) 0.003(3) -0.022(3) O8W 0.0357(15) 0.0368(15) 0.0424(15) -0.0177(12) -0.0110(12) -0.0172(12) O9W 0.027(2) 0.045(2) 0.035(2) -0.0115(19) -0.0107(17) -0.0096(18) O10W 0.0395(16) 0.0441(16) 0.0353(15) -0.0126(13) 0.0066(12) -0.0149(14) O11W 0.034(3) 0.034(3) 0.038(3) 0.019(2) -0.008(2) -0.013(3) O12W 0.0399(17) 0.0349(16) 0.0374(16) 0.0020(13) -0.0065(13) -0.0160(14) O13W 0.042(3) 0.039(3) 0.046(3) -0.017(3) 0.017(3) -0.021(3) O14W 0.042(3) 0.041(2) 0.042(2) -0.0078(19) -0.016(2) -0.016(2) O15W 0.0361(19) 0.0439(19) 0.0368(18) -0.0174(15) -0.0204(15) -0.0051(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.210(3) . ? C1 O1 1.292(3) . ? C1 C2 1.475(3) . ? C2 C3 1.400(3) . ? C2 C7 1.400(3) . ? C3 C4 1.359(3) . ? C3 H3 0.9500 . ? C4 C5 1.376(3) . ? C4 H4 0.9500 . ? C5 O3 1.342(2) . ? C5 C6 1.359(3) . ? C6 C7 1.389(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O3 1.446(2) . ? C8 C9 1.550(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.366(3) . ? C9 C10 1.408(4) . ? C10 C11 1.430(3) . ? C10 C16 1.562(3) . ? C11 C12 1.368(3) . ? C11 C17 1.510(3) . ? C12 C13 1.380(4) . ? C12 C18 1.519(3) . ? C13 C14 1.384(3) . ? C13 C19 1.512(3) . ? C14 C15 1.533(4) . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C15 H15A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C16 H16A 0.9800 . ? C17 O7 1.446(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O4 1.500(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O4 1.361(2) . ? C20 C21 1.390(3) . ? C20 C25 1.390(3) . ? C21 C22 1.390(3) . ? C21 H21 0.9500 . ? C22 C23 1.390(3) . ? C22 H22 0.9500 . ? C23 C24 1.390(3) . ? C23 C26 1.486(3) . ? C24 C25 1.390(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 O5 1.226(2) . ? C26 O6 1.243(2) . ? C27 O7 1.349(2) . ? C27 C28 1.390(3) . ? C27 C32 1.390(3) . ? C28 C29 1.390(4) . ? C28 H28 0.9500 . ? C29 C30 1.390(4) . ? C29 H29 0.9500 . ? C30 C31 1.390(3) . ? C30 C33 1.489(4) . ? C31 C32 1.390(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 O8 1.247(3) . ? C33 O9 1.256(2) . ? C34 O14 1.235(2) . ? C34 O13 1.284(2) . ? C34 C35 1.485(3) . ? C34 Co4 2.490(2) . ? C35 C36 1.390(3) . ? C35 C40 1.390(3) . ? C36 C37 1.390(3) . ? C36 H36 0.9500 . ? C37 C38 1.390(3) . ? C37 H37 0.9500 . ? C38 C39 1.390(3) . ? C38 O15 1.399(2) . ? C39 C40 1.390(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 O15 1.457(2) . ? C41 C42 1.476(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.380(3) . ? C42 C47 1.401(3) . ? C43 C44 1.384(3) . ? C43 C48 1.516(3) . ? C44 C45 1.419(3) . ? C44 C49 1.539(3) . ? C45 C46 1.363(3) . ? C45 C50 1.533(3) . ? C46 C47 1.382(3) . ? C46 C51 1.524(2) . ? C47 C52 1.510(2) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 O19 1.433(2) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 O16 1.433(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 O16 1.348(3) . ? C53 C54 1.390(3) . ? C53 C58 1.390(4) . ? C54 C55 1.390(3) . ? C54 H54 0.9500 . ? C55 C56 1.390(3) . ? C55 H55 0.9500 . ? C56 C57 1.390(3) . ? C56 C59 1.485(3) . ? C57 C58 1.390(3) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 O17 1.266(3) . ? C59 O18 1.279(3) . ? C60 O19 1.343(3) . ? C60 C61 1.393(3) . ? C60 C65 1.396(3) . ? C61 C62 1.395(3) . ? C61 H61 0.9500 . ? C62 C63 1.343(3) . ? C62 H62 0.9500 . ? C63 C64 1.402(3) . ? C63 C66 1.486(3) . ? C64 C65 1.362(3) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C66 O20 1.234(3) . ? C66 O21 1.271(3) . ? C67 O10 1.205(3) . ? C67 N1 1.327(3) . ? C67 H67 0.9500 . ? C68 N1 1.421(3) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 N1 1.421(3) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 O11 1.239(3) . ? C70 N2 1.321(3) . ? C70 H70 0.9500 . ? C71 N2 1.490(3) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 N2 1.476(3) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? Co1 O18 2.0559(15) 2_775 ? Co1 O18 2.0559(15) 1_546 ? Co1 O20 2.0639(15) 2_765 ? Co1 O20 2.0639(15) 1_556 ? Co1 O14 2.1752(15) . ? Co1 O14 2.1752(15) 2_766 ? Co2 O1 1.9139(17) 1_554 ? Co2 O6 1.9213(17) 1_545 ? Co2 O8 1.9335(18) . ? Co2 O12 2.0056(17) . ? Co3 O9 1.9878(16) . ? Co3 O5 1.9964(15) 1_545 ? Co3 O2 2.0352(15) 1_554 ? Co3 O11 2.0599(16) . ? Co3 O10 2.0984(16) . ? Co3 O1W 2.2699(16) . ? Co4 O17 1.9787(15) 1_546 ? Co4 O21 1.9973(16) 1_556 ? Co4 O2W 2.0150(16) . ? Co4 O14 2.1459(15) . ? Co4 O13 2.1529(14) . ? Co4 O1W 2.2470(16) . ? O1 Co2 1.9139(17) 1_556 ? O2 Co3 2.0352(15) 1_556 ? O5 Co3 1.9964(15) 1_565 ? O6 Co2 1.9213(17) 1_565 ? O12 H12A 0.8400 . ? O17 Co4 1.9787(15) 1_564 ? O18 Co1 2.0559(15) 1_564 ? O20 Co1 2.0639(15) 1_554 ? O21 Co4 1.9972(16) 1_554 ? 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 O2 C1 O1 124.9(2) . . ? O2 C1 C2 121.5(2) . . ? O1 C1 C2 113.6(2) . . ? C3 C2 C7 117.6(2) . . ? C3 C2 C1 121.5(2) . . ? C7 C2 C1 120.8(2) . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 121.2(2) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? O3 C5 C6 124.7(2) . . ? O3 C5 C4 115.34(19) . . ? C6 C5 C4 120.0(2) . . ? C5 C6 C7 119.6(2) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C2 120.8(2) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? O3 C8 C9 103.97(17) . . ? O3 C8 H8A 111.0 . . ? C9 C8 H8A 111.0 . . ? O3 C8 H8B 111.0 . . ? C9 C8 H8B 111.0 . . ? H8A C8 H8B 109.0 . . ? C14 C9 C10 120.0(2) . . ? C14 C9 C8 118.5(2) . . ? C10 C9 C8 121.5(2) . . ? C9 C10 C11 118.3(2) . . ? C9 C10 C16 123.4(2) . . ? C11 C10 C16 118.3(2) . . ? C12 C11 C10 120.3(2) . . ? C12 C11 C17 119.0(2) . . ? C10 C11 C17 120.7(2) . . ? C11 C12 C13 119.9(2) . . ? C11 C12 C18 119.5(2) . . ? C13 C12 C18 120.4(2) . . ? C12 C13 C14 120.7(2) . . ? C12 C13 C19 116.6(2) . . ? C14 C13 C19 122.3(2) . . ? C9 C14 C13 120.7(2) . . ? C9 C14 C15 118.1(2) . . ? C13 C14 C15 120.7(2) . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? C10 C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C10 C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? O7 C17 C11 106.98(17) . . ? O7 C17 H17A 110.3 . . ? C11 C17 H17A 110.3 . . ? O7 C17 H17B 110.3 . . ? C11 C17 H17B 110.3 . . ? H17A C17 H17B 108.6 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C13 98.17(17) . . ? O4 C19 H19A 112.1 . . ? C13 C19 H19A 112.1 . . ? O4 C19 H19B 112.1 . . ? C13 C19 H19B 112.1 . . ? H19A C19 H19B 109.8 . . ? O4 C20 C21 123.45(19) . . ? O4 C20 C25 116.55(19) . . ? C21 C20 C25 120.0(2) . . ? C20 C21 C22 120.0(2) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0(2) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.0(2) . . ? C24 C23 C26 122.2(2) . . ? C22 C23 C26 117.7(2) . . ? C25 C24 C23 120.0(2) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C20 120.0(2) . . ? C24 C25 H25 120.0 . . ? C20 C25 H25 120.0 . . ? O5 C26 O6 127.80(19) . . ? O5 C26 C23 119.1(2) . . ? O6 C26 C23 113.1(2) . . ? O7 C27 C28 125.3(2) . . ? O7 C27 C32 114.59(18) . . ? C28 C27 C32 120.0(2) . . ? C27 C28 C29 120.0(2) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C30 120.0(2) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.0(2) . . ? C31 C30 C33 118.1(2) . . ? C29 C30 C33 121.9(2) . . ? C32 C31 C30 120.0(2) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C27 120.0(2) . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? O8 C33 O9 119.7(2) . . ? O8 C33 C30 119.8(2) . . ? O9 C33 C30 120.4(2) . . ? O14 C34 O13 119.24(17) . . ? O14 C34 C35 122.3(2) . . ? O13 C34 C35 118.41(18) . . ? O14 C34 Co4 59.53(9) . . ? O13 C34 Co4 59.85(8) . . ? C35 C34 Co4 174.13(17) . . ? C36 C35 C40 120.0(2) . . ? C36 C35 C34 120.7(2) . . ? C40 C35 C34 119.2(2) . . ? C37 C36 C35 120.0(2) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 120.0(2) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.0(2) . . ? C37 C38 O15 115.7(2) . . ? C39 C38 O15 124.17(19) . . ? C38 C39 C40 120.0(2) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C35 120.0(2) . . ? C39 C40 H40 120.0 . . ? C35 C40 H40 120.0 . . ? O15 C41 C42 110.63(18) . . ? O15 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? O15 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C43 C42 C47 120.0(2) . . ? C43 C42 C41 122.6(2) . . ? C47 C42 C41 117.3(2) . . ? C42 C43 C44 119.6(2) . . ? C42 C43 C48 120.1(2) . . ? C44 C43 C48 120.2(2) . . ? C43 C44 C45 120.8(2) . . ? C43 C44 C49 122.5(2) . . ? C45 C44 C49 116.7(2) . . ? C46 C45 C44 117.8(2) . . ? C46 C45 C50 120.1(2) . . ? C44 C45 C50 122.0(2) . . ? C45 C46 C47 122.3(2) . . ? C45 C46 C51 117.52(18) . . ? C47 C46 C51 120.17(19) . . ? C46 C47 C42 119.1(2) . . ? C46 C47 C52 122.45(18) . . ? C42 C47 C52 118.38(18) . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O19 C49 C44 106.87(17) . . ? O19 C49 H49A 110.3 . . ? C44 C49 H49A 110.3 . . ? O19 C49 H49B 110.3 . . ? C44 C49 H49B 110.3 . . ? H49A C49 H49B 108.6 . . ? C45 C50 H50A 109.5 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O16 C51 C46 106.94(16) . . ? O16 C51 H51A 110.3 . . ? C46 C51 H51A 110.3 . . ? O16 C51 H51B 110.3 . . ? C46 C51 H51B 110.3 . . ? H51A C51 H51B 108.6 . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O16 C53 C54 125.8(2) . . ? O16 C53 C58 114.2(2) . . ? C54 C53 C58 120.0(2) . . ? C53 C54 C55 120.0(2) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C56 C55 C54 120.0(2) . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C57 120.0(2) . . ? C55 C56 C59 120.7(2) . . ? C57 C56 C59 119.2(2) . . ? C58 C57 C56 120.0(2) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C53 120.0(2) . . ? C57 C58 H58 120.0 . . ? C53 C58 H58 120.0 . . ? O17 C59 O18 125.1(2) . . ? O17 C59 C56 117.1(2) . . ? O18 C59 C56 117.7(2) . . ? O19 C60 C61 124.5(2) . . ? O19 C60 C65 118.4(2) . . ? C61 C60 C65 116.9(2) . . ? C60 C61 C62 120.1(2) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C63 C62 C61 121.6(2) . . ? C63 C62 H62 119.2 . . ? C61 C62 H62 119.2 . . ? C62 C63 C64 119.0(2) . . ? C62 C63 C66 121.4(2) . . ? C64 C63 C66 119.5(2) . . ? C65 C64 C63 119.5(2) . . ? C65 C64 H64 120.2 . . ? C63 C64 H64 120.2 . . ? C64 C65 C60 122.5(2) . . ? C64 C65 H65 118.8 . . ? C60 C65 H65 118.8 . . ? O20 C66 O21 126.3(2) . . ? O20 C66 C63 116.8(2) . . ? O21 C66 C63 116.9(2) . . ? O10 C67 N1 124.6(2) . . ? O10 C67 H67 117.7 . . ? N1 C67 H67 117.7 . . ? N1 C68 H68A 109.5 . . ? N1 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? N1 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N1 C69 H69A 109.5 . . ? N1 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N1 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? O11 C70 N2 122.6(2) . . ? O11 C70 H70 118.7 . . ? N2 C70 H70 118.7 . . ? N2 C71 H71A 109.5 . . ? N2 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? N2 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N2 C72 H72A 109.5 . . ? N2 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N2 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O18 Co1 O18 180.00(8) 2_775 1_546 ? O18 Co1 O20 91.60(7) 2_775 2_765 ? O18 Co1 O20 88.40(7) 1_546 2_765 ? O18 Co1 O20 88.40(7) 2_775 1_556 ? O18 Co1 O20 91.60(7) 1_546 1_556 ? O20 Co1 O20 180.000(1) 2_765 1_556 ? O18 Co1 O14 88.67(6) 2_775 . ? O18 Co1 O14 91.33(6) 1_546 . ? O20 Co1 O14 85.63(6) 2_765 . ? O20 Co1 O14 94.37(6) 1_556 . ? O18 Co1 O14 91.33(6) 2_775 2_766 ? O18 Co1 O14 88.67(6) 1_546 2_766 ? O20 Co1 O14 94.37(6) 2_765 2_766 ? O20 Co1 O14 85.63(6) 1_556 2_766 ? O14 Co1 O14 180.00(7) . 2_766 ? O1 Co2 O6 121.89(8) 1_554 1_545 ? O1 Co2 O8 115.25(7) 1_554 . ? O6 Co2 O8 110.35(7) 1_545 . ? O1 Co2 O12 100.05(7) 1_554 . ? O6 Co2 O12 95.54(7) 1_545 . ? O8 Co2 O12 110.67(7) . . ? O9 Co3 O5 90.84(7) . 1_545 ? O9 Co3 O2 97.70(7) . 1_554 ? O5 Co3 O2 98.36(6) 1_545 1_554 ? O9 Co3 O11 90.92(6) . . ? O5 Co3 O11 174.60(6) 1_545 . ? O2 Co3 O11 86.47(6) 1_554 . ? O9 Co3 O10 89.32(7) . . ? O5 Co3 O10 88.19(6) 1_545 . ? O2 Co3 O10 170.28(7) 1_554 . ? O11 Co3 O10 86.71(6) . . ? O9 Co3 O1W 177.34(6) . . ? O5 Co3 O1W 88.92(6) 1_545 . ? O2 Co3 O1W 84.95(6) 1_554 . ? O11 Co3 O1W 89.09(6) . . ? O10 Co3 O1W 88.02(6) . . ? O17 Co4 O21 96.01(6) 1_546 1_556 ? O17 Co4 O2W 85.28(6) 1_546 . ? O21 Co4 O2W 173.85(7) 1_556 . ? O17 Co4 O14 104.00(6) 1_546 . ? O21 Co4 O14 101.31(6) 1_556 . ? O2W Co4 O14 84.16(6) . . ? O17 Co4 O13 163.18(6) 1_546 . ? O21 Co4 O13 94.18(6) 1_556 . ? O2W Co4 O13 86.01(6) . . ? O14 Co4 O13 60.75(6) . . ? O17 Co4 O1W 95.76(6) 1_546 . ? O21 Co4 O1W 90.41(6) 1_556 . ? O2W Co4 O1W 83.47(6) . . ? O14 Co4 O1W 155.68(6) . . ? O13 Co4 O1W 97.51(6) . . ? O17 Co4 C34 133.15(5) 1_546 . ? O21 Co4 C34 100.28(5) 1_556 . ? O2W Co4 C34 83.05(5) . . ? O14 Co4 C34 29.74(5) . . ? O13 Co4 C34 31.06(5) . . ? O1W Co4 C34 127.46(5) . . ? C67 N1 C69 122.5(2) . . ? C67 N1 C68 123.4(2) . . ? C69 N1 C68 114.1(2) . . ? C70 N2 C72 123.5(2) . . ? C70 N2 C71 119.0(2) . . ? C72 N2 C71 117.47(19) . . ? C1 O1 Co2 133.48(11) . 1_556 ? C1 O2 Co3 141.00(12) . 1_556 ? C5 O3 C8 116.07(14) . . ? C20 O4 C19 116.49(13) . . ? C26 O5 Co3 143.15(11) . 1_565 ? C26 O6 Co2 125.58(12) . 1_565 ? C27 O7 C17 117.43(14) . . ? C33 O8 Co2 113.13(11) . . ? C33 O9 Co3 172.43(12) . . ? C67 O10 Co3 125.31(16) . . ? C70 O11 Co3 122.44(14) . . ? Co2 O12 H12A 109.5 . . ? C34 O13 Co4 89.10(9) . . ? C34 O14 Co4 90.73(11) . . ? C34 O14 Co1 141.86(10) . . ? Co4 O14 Co1 104.98(6) . . ? C38 O15 C41 115.73(14) . . ? C53 O16 C51 118.48(18) . . ? C59 O17 Co4 128.68(14) . 1_564 ? C59 O18 Co1 137.59(15) . 1_564 ? C60 O19 C49 117.82(15) . . ? C66 O20 Co1 141.14(15) . 1_554 ? C66 O21 Co4 124.22(14) . 1_554 ? Co4 O1W Co3 148.68(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -3.8(4) . . . . ? O1 C1 C2 C3 174.8(2) . . . . ? O2 C1 C2 C7 175.8(2) . . . . ? O1 C1 C2 C7 -5.6(4) . . . . ? C7 C2 C3 C4 2.6(4) . . . . ? C1 C2 C3 C4 -177.8(2) . . . . ? C2 C3 C4 C5 -7.0(4) . . . . ? C3 C4 C5 O3 -176.7(2) . . . . ? C3 C4 C5 C6 4.6(4) . . . . ? O3 C5 C6 C7 -176.4(2) . . . . ? C4 C5 C6 C7 2.2(4) . . . . ? C5 C6 C7 C2 -6.5(4) . . . . ? C3 C2 C7 C6 4.1(4) . . . . ? C1 C2 C7 C6 -175.5(3) . . . . ? O3 C8 C9 C14 -82.1(2) . . . . ? O3 C8 C9 C10 97.0(2) . . . . ? C14 C9 C10 C11 -3.1(3) . . . . ? C8 C9 C10 C11 177.8(2) . . . . ? C14 C9 C10 C16 178.0(2) . . . . ? C8 C9 C10 C16 -1.2(3) . . . . ? C9 C10 C11 C12 0.2(3) . . . . ? C16 C10 C11 C12 179.2(2) . . . . ? C9 C10 C11 C17 179.1(2) . . . . ? C16 C10 C11 C17 -1.8(3) . . . . ? C10 C11 C12 C13 1.6(3) . . . . ? C17 C11 C12 C13 -177.4(2) . . . . ? C10 C11 C12 C18 -173.2(2) . . . . ? C17 C11 C12 C18 7.9(3) . . . . ? C11 C12 C13 C14 -0.5(4) . . . . ? C18 C12 C13 C14 174.2(2) . . . . ? C11 C12 C13 C19 172.4(2) . . . . ? C18 C12 C13 C19 -13.0(3) . . . . ? C10 C9 C14 C13 4.2(4) . . . . ? C8 C9 C14 C13 -176.7(2) . . . . ? C10 C9 C14 C15 176.2(2) . . . . ? C8 C9 C14 C15 -4.6(3) . . . . ? C12 C13 C14 C9 -2.4(4) . . . . ? C19 C13 C14 C9 -174.8(2) . . . . ? C12 C13 C14 C15 -174.3(2) . . . . ? C19 C13 C14 C15 13.3(4) . . . . ? C12 C11 C17 O7 -87.6(2) . . . . ? C10 C11 C17 O7 93.5(2) . . . . ? C12 C13 C19 O4 92.9(2) . . . . ? C14 C13 C19 O4 -94.4(2) . . . . ? O4 C20 C21 C22 -179.9(2) . . . . ? C25 C20 C21 C22 0.0(4) . . . . ? C20 C21 C22 C23 0.0(4) . . . . ? C21 C22 C23 C24 0.0(4) . . . . ? C21 C22 C23 C26 -178.2(2) . . . . ? C22 C23 C24 C25 0.0(5) . . . . ? C26 C23 C24 C25 178.1(3) . . . . ? C23 C24 C25 C20 0.0(5) . . . . ? O4 C20 C25 C24 179.9(2) . . . . ? C21 C20 C25 C24 0.0(4) . . . . ? C24 C23 C26 O5 -162.1(3) . . . . ? C22 C23 C26 O5 16.1(4) . . . . ? C24 C23 C26 O6 20.5(4) . . . . ? C22 C23 C26 O6 -161.4(2) . . . . ? O7 C27 C28 C29 176.9(2) . . . . ? C32 C27 C28 C29 0.0(4) . . . . ? C27 C28 C29 C30 0.0(4) . . . . ? C28 C29 C30 C31 0.0(4) . . . . ? C28 C29 C30 C33 -178.5(2) . . . . ? C29 C30 C31 C32 0.0(4) . . . . ? C33 C30 C31 C32 178.5(2) . . . . ? C30 C31 C32 C27 0.0(4) . . . . ? O7 C27 C32 C31 -177.2(2) . . . . ? C28 C27 C32 C31 0.0(4) . . . . ? C31 C30 C33 O8 -6.3(3) . . . . ? C29 C30 C33 O8 172.1(2) . . . . ? C31 C30 C33 O9 176.8(2) . . . . ? C29 C30 C33 O9 -4.7(3) . . . . ? O14 C34 C35 C36 3.5(3) . . . . ? O13 C34 C35 C36 -174.2(2) . . . . ? Co4 C34 C35 C36 -103.0(17) . . . . ? O14 C34 C35 C40 -179.7(2) . . . . ? O13 C34 C35 C40 2.6(3) . . . . ? Co4 C34 C35 C40 73.8(18) . . . . ? C40 C35 C36 C37 0.0(4) . . . . ? C34 C35 C36 C37 176.8(2) . . . . ? C35 C36 C37 C38 0.0(4) . . . . ? C36 C37 C38 C39 0.0(4) . . . . ? C36 C37 C38 O15 176.1(2) . . . . ? C37 C38 C39 C40 0.0(4) . . . . ? O15 C38 C39 C40 -175.7(2) . . . . ? C38 C39 C40 C35 0.0(4) . . . . ? C36 C35 C40 C39 0.0(4) . . . . ? C34 C35 C40 C39 -176.8(2) . . . . ? O15 C41 C42 C43 86.8(3) . . . . ? O15 C41 C42 C47 -97.9(2) . . . . ? C47 C42 C43 C44 -4.1(3) . . . . ? C41 C42 C43 C44 171.1(2) . . . . ? C47 C42 C43 C48 174.6(2) . . . . ? C41 C42 C43 C48 -10.3(3) . . . . ? C42 C43 C44 C45 -2.2(3) . . . . ? C48 C43 C44 C45 179.2(2) . . . . ? C42 C43 C44 C49 -179.6(2) . . . . ? C48 C43 C44 C49 1.8(3) . . . . ? C43 C44 C45 C46 5.6(4) . . . . ? C49 C44 C45 C46 -176.9(2) . . . . ? C43 C44 C45 C50 -172.0(2) . . . . ? C49 C44 C45 C50 5.5(3) . . . . ? C44 C45 C46 C47 -2.8(4) . . . . ? C50 C45 C46 C47 174.9(2) . . . . ? C44 C45 C46 C51 175.00(18) . . . . ? C50 C45 C46 C51 -7.3(3) . . . . ? C45 C46 C47 C42 -3.3(4) . . . . ? C51 C46 C47 C42 178.96(18) . . . . ? C45 C46 C47 C52 -179.5(2) . . . . ? C51 C46 C47 C52 2.8(3) . . . . ? C43 C42 C47 C46 6.8(3) . . . . ? C41 C42 C47 C46 -168.6(2) . . . . ? C43 C42 C47 C52 -176.84(18) . . . . ? C41 C42 C47 C52 7.8(3) . . . . ? C43 C44 C49 O19 92.1(2) . . . . ? C45 C44 C49 O19 -85.4(2) . . . . ? C45 C46 C51 O16 89.0(2) . . . . ? C47 C46 C51 O16 -93.13(19) . . . . ? O16 C53 C54 C55 178.5(3) . . . . ? C58 C53 C54 C55 0.0(4) . . . . ? C53 C54 C55 C56 0.0(4) . . . . ? C54 C55 C56 C57 0.0(4) . . . . ? C54 C55 C56 C59 -176.1(2) . . . . ? C55 C56 C57 C58 0.0(5) . . . . ? C59 C56 C57 C58 176.1(3) . . . . ? C56 C57 C58 C53 0.0(5) . . . . ? O16 C53 C58 C57 -178.7(3) . . . . ? C54 C53 C58 C57 0.0(5) . . . . ? C55 C56 C59 O17 -164.4(2) . . . . ? C57 C56 C59 O17 19.5(4) . . . . ? C55 C56 C59 O18 15.3(4) . . . . ? C57 C56 C59 O18 -160.8(3) . . . . ? O19 C60 C61 C62 179.7(2) . . . . ? C65 C60 C61 C62 4.6(4) . . . . ? C60 C61 C62 C63 -7.3(4) . . . . ? C61 C62 C63 C64 6.7(4) . . . . ? C61 C62 C63 C66 -172.9(2) . . . . ? C62 C63 C64 C65 -3.7(3) . . . . ? C66 C63 C64 C65 175.9(2) . . . . ? C63 C64 C65 C60 1.3(4) . . . . ? O19 C60 C65 C64 -177.2(2) . . . . ? C61 C60 C65 C64 -1.8(4) . . . . ? C62 C63 C66 O20 -3.1(3) . . . . ? C64 C63 C66 O20 177.3(2) . . . . ? C62 C63 C66 O21 176.3(2) . . . . ? C64 C63 C66 O21 -3.3(3) . . . . ? O14 C34 Co4 O17 -13.57(14) . . . 1_546 ? O13 C34 Co4 O17 170.65(10) . . . 1_546 ? C35 C34 Co4 O17 96.4(17) . . . 1_546 ? O14 C34 Co4 O21 94.85(9) . . . 1_556 ? O13 C34 Co4 O21 -80.94(9) . . . 1_556 ? C35 C34 Co4 O21 -155.2(17) . . . 1_556 ? O14 C34 Co4 O2W -90.39(9) . . . . ? O13 C34 Co4 O2W 93.82(9) . . . . ? C35 C34 Co4 O2W 19.5(17) . . . . ? O13 C34 Co4 O14 -175.79(18) . . . . ? C35 C34 Co4 O14 109.9(17) . . . . ? O14 C34 Co4 O13 175.79(18) . . . . ? C35 C34 Co4 O13 -74.3(17) . . . . ? O14 C34 Co4 O1W -166.64(10) . . . . ? O13 C34 Co4 O1W 17.57(12) . . . . ? C35 C34 Co4 O1W -56.7(17) . . . . ? O10 C67 N1 C69 -1.5(4) . . . . ? O10 C67 N1 C68 -177.6(2) . . . . ? O11 C70 N2 C72 -0.4(4) . . . . ? O11 C70 N2 C71 178.1(2) . . . . ? O2 C1 O1 Co2 4.7(4) . . . 1_556 ? C2 C1 O1 Co2 -173.91(13) . . . 1_556 ? O1 C1 O2 Co3 -16.2(4) . . . 1_556 ? C2 C1 O2 Co3 162.23(14) . . . 1_556 ? C6 C5 O3 C8 -4.1(3) . . . . ? C4 C5 O3 C8 177.3(2) . . . . ? C9 C8 O3 C5 -170.93(18) . . . . ? C21 C20 O4 C19 -9.8(3) . . . . ? C25 C20 O4 C19 170.2(2) . . . . ? C13 C19 O4 C20 -161.71(16) . . . . ? O6 C26 O5 Co3 34.7(4) . . . 1_565 ? C23 C26 O5 Co3 -142.31(17) . . . 1_565 ? O5 C26 O6 Co2 -7.9(3) . . . 1_565 ? C23 C26 O6 Co2 169.26(14) . . . 1_565 ? C28 C27 O7 C17 -0.1(3) . . . . ? C32 C27 O7 C17 176.95(19) . . . . ? C11 C17 O7 C27 172.12(17) . . . . ? O9 C33 O8 Co2 8.5(2) . . . . ? C30 C33 O8 Co2 -168.38(16) . . . . ? O1 Co2 O8 C33 -75.68(12) 1_554 . . . ? O6 Co2 O8 C33 67.25(13) 1_545 . . . ? O12 Co2 O8 C33 171.73(12) . . . . ? O8 C33 O9 Co3 -7.7(10) . . . . ? C30 C33 O9 Co3 169.2(9) . . . . ? O5 Co3 O9 C33 -48.2(9) 1_545 . . . ? O2 Co3 O9 C33 50.3(9) 1_554 . . . ? O11 Co3 O9 C33 136.9(9) . . . . ? O10 Co3 O9 C33 -136.4(9) . . . . ? O1W Co3 O9 C33 -132.9(11) . . . . ? N1 C67 O10 Co3 170.59(17) . . . . ? O9 Co3 O10 C67 -168.43(18) . . . . ? O5 Co3 O10 C67 100.71(19) 1_545 . . . ? O2 Co3 O10 C67 -31.9(5) 1_554 . . . ? O11 Co3 O10 C67 -77.47(18) . . . . ? O1W Co3 O10 C67 11.73(18) . . . . ? N2 C70 O11 Co3 164.33(17) . . . . ? O9 Co3 O11 C70 -142.79(18) . . . . ? O5 Co3 O11 C70 108.3(7) 1_545 . . . ? O2 Co3 O11 C70 -45.13(18) 1_554 . . . ? O10 Co3 O11 C70 127.94(18) . . . . ? O1W Co3 O11 C70 39.87(18) . . . . ? O14 C34 O13 Co4 -4.16(17) . . . . ? C35 C34 O13 Co4 173.57(19) . . . . ? O17 Co4 O13 C34 -24.2(2) 1_546 . . . ? O21 Co4 O13 C34 103.02(10) 1_556 . . . ? O2W Co4 O13 C34 -83.14(10) . . . . ? O14 Co4 O13 C34 2.39(10) . . . . ? O1W Co4 O13 C34 -166.01(10) . . . . ? O13 C34 O14 Co4 4.18(17) . . . . ? C35 C34 O14 Co4 -173.5(2) . . . . ? O13 C34 O14 Co1 -111.58(17) . . . . ? C35 C34 O14 Co1 70.8(3) . . . . ? Co4 C34 O14 Co1 -115.76(18) . . . . ? O17 Co4 O14 C34 169.84(10) 1_546 . . . ? O21 Co4 O14 C34 -90.95(10) 1_556 . . . ? O2W Co4 O14 C34 86.20(10) . . . . ? O13 Co4 O14 C34 -2.49(10) . . . . ? O1W Co4 O14 C34 26.44(18) . . . . ? O17 Co4 O14 Co1 -45.31(8) 1_546 . . . ? O21 Co4 O14 Co1 53.89(7) 1_556 . . . ? O2W Co4 O14 Co1 -128.96(7) . . . . ? O13 Co4 O14 Co1 142.36(8) . . . . ? O1W Co4 O14 Co1 171.29(11) . . . . ? C34 Co4 O14 Co1 144.85(12) . . . . ? O18 Co1 O14 C34 -18.08(18) 2_775 . . . ? O18 Co1 O14 C34 161.92(18) 1_546 . . . ? O20 Co1 O14 C34 -109.79(18) 2_765 . . . ? O20 Co1 O14 C34 70.21(18) 1_556 . . . ? O14 Co1 O14 C34 146(100) 2_766 . . . ? O18 Co1 O14 Co4 -129.30(7) 2_775 . . . ? O18 Co1 O14 Co4 50.70(7) 1_546 . . . ? O20 Co1 O14 Co4 138.99(7) 2_765 . . . ? O20 Co1 O14 Co4 -41.00(7) 1_556 . . . ? O14 Co1 O14 Co4 34(100) 2_766 . . . ? C37 C38 O15 C41 162.7(2) . . . . ? C39 C38 O15 C41 -21.4(3) . . . . ? C42 C41 O15 C38 174.91(18) . . . . ? C54 C53 O16 C51 0.8(4) . . . . ? C58 C53 O16 C51 179.3(2) . . . . ? C46 C51 O16 C53 -158.6(2) . . . . ? O18 C59 O17 Co4 14.1(4) . . . 1_564 ? C56 C59 O17 Co4 -166.19(17) . . . 1_564 ? O17 C59 O18 Co1 7.7(4) . . . 1_564 ? C56 C59 O18 Co1 -171.98(18) . . . 1_564 ? C61 C60 O19 C49 -3.4(3) . . . . ? C65 C60 O19 C49 171.60(18) . . . . ? C44 C49 O19 C60 174.83(15) . . . . ? O21 C66 O20 Co1 -7.3(4) . . . 1_554 ? C63 C66 O20 Co1 172.04(16) . . . 1_554 ? O20 C66 O21 Co4 21.8(3) . . . 1_554 ? C63 C66 O21 Co4 -157.47(15) . . . 1_554 ? O17 Co4 O1W Co3 114.82(14) 1_546 . . . ? O21 Co4 O1W Co3 18.74(14) 1_556 . . . ? O2W Co4 O1W Co3 -160.62(15) . . . . ? O14 Co4 O1W Co3 -100.73(18) . . . . ? O13 Co4 O1W Co3 -75.53(14) . . . . ? C34 Co4 O1W Co3 -84.57(14) . . . . ? O9 Co3 O1W Co4 -78.9(13) . . . . ? O5 Co3 O1W Co4 -163.59(14) 1_545 . . . ? O2 Co3 O1W Co4 97.93(14) 1_554 . . . ? O11 Co3 O1W Co4 11.39(14) . . . . ? O10 Co3 O1W Co4 -75.35(14) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.674 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.047 data_4 _database_code_depnum_ccdc_archive 'CCDC 816748' #TrackingRef '- n (1-4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H34 Cl Co2 N O12), 4(C3 H7 N O), 3(O)' _chemical_formula_sum 'C84 H106 Cl2 Co4 N6 O29' _chemical_formula_weight 1992.29 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.6360(6) _cell_length_b 35.5231(14) _cell_length_c 17.7388(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.067(3) _cell_angle_gamma 90.00 _cell_volume 5438.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 5271 _cell_measurement_theta_min 2.260 _cell_measurement_theta_max 21.728 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064.0 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8245 _exptl_absorpt_correction_T_max 0.8699 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29707 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10610 _reflns_number_gt 8001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+1.6548P] 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 10610 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2785(3) 0.75162(7) 0.46773(16) 0.0349(6) Uani 1 1 d . . . C2 C 0.2766(3) 0.79375(7) 0.47690(16) 0.0349(6) Uani 1 1 d . . . C3 C 0.1495(3) 0.80991(7) 0.51077(16) 0.0356(6) Uani 1 1 d . . . H3 H 0.0671 0.7950 0.5252 0.043 Uiso 1 1 calc R . . C4 C 0.1475(3) 0.84857(7) 0.52278(16) 0.0364(6) Uani 1 1 d . . . H4 H 0.0632 0.8598 0.5450 0.044 Uiso 1 1 calc R . . C5 C 0.2710(3) 0.87025(7) 0.50154(16) 0.0348(6) Uani 1 1 d . . . C6 C 0.3969(3) 0.85417(7) 0.46686(15) 0.0331(6) Uani 1 1 d . . . H6 H 0.4785 0.8690 0.4513 0.040 Uiso 1 1 calc R . . C7 C 0.3984(3) 0.81608(7) 0.45607(17) 0.0363(6) Uani 1 1 d . . . H7 H 0.4833 0.8050 0.4342 0.044 Uiso 1 1 calc R . . C8 C 0.3808(3) 0.93289(7) 0.49994(15) 0.0294(5) Uani 1 1 d . . . H8A H 0.4057 0.9307 0.4472 0.035 Uiso 1 1 calc R . . H8B H 0.4728 0.9272 0.5308 0.035 Uiso 1 1 calc R . . C9 C 0.3236(3) 0.97174(7) 0.51657(14) 0.0290(5) Uani 1 1 d . . . C10 C 0.3559(3) 0.98858(7) 0.58614(14) 0.0300(5) Uani 1 1 d . . . C11 C 0.2980(3) 1.02479(7) 0.60149(15) 0.0317(6) Uani 1 1 d . . . C12 C 0.2158(3) 1.04518(6) 0.54335(14) 0.0255(5) Uani 1 1 d . . . C13 C 0.1758(3) 1.02717(7) 0.47530(14) 0.0287(5) Uani 1 1 d . . . C14 C 0.2311(3) 0.99030(7) 0.46127(14) 0.0270(5) Uani 1 1 d . . . C15 C 0.1881(3) 0.97110(7) 0.38785(14) 0.0294(5) Uani 1 1 d . . . H15A H 0.1302 0.9487 0.3976 0.044 Uiso 1 1 calc R . . H15B H 0.2806 0.9646 0.3624 0.044 Uiso 1 1 calc R . . H15C H 0.1261 0.9878 0.3567 0.044 Uiso 1 1 calc R . . C16 C 0.4494(3) 0.96820(8) 0.64701(15) 0.0361(6) Uani 1 1 d . . . H16B H 0.4521 0.9418 0.6355 0.054 Uiso 1 1 calc R . . H16C H 0.4024 0.9719 0.6947 0.054 Uiso 1 1 calc R . . H16A H 0.5531 0.9780 0.6495 0.054 Uiso 1 1 calc R . . C17 C 0.1745(3) 1.08622(6) 0.55396(15) 0.0276(5) Uani 1 1 d . . . H17A H 0.2161 1.1009 0.5139 0.041 Uiso 1 1 calc R . . H17B H 0.2173 1.0949 0.6015 0.041 Uiso 1 1 calc R . . H17C H 0.0638 1.0889 0.5531 0.041 Uiso 1 1 calc R . . C18 C 0.0667(3) 1.04601(7) 0.42039(15) 0.0322(6) Uani 1 1 d . . . H18A H -0.0075 1.0279 0.3997 0.039 Uiso 1 1 calc R . . H18B H 0.0105 1.0658 0.4452 0.039 Uiso 1 1 calc R . . C19 C 0.0732(3) 1.08091(7) 0.30658(14) 0.0299(6) Uani 1 1 d . . . C20 C 0.1573(3) 1.09406(7) 0.24659(16) 0.0345(6) Uani 1 1 d . . . H20 H 0.2621 1.0883 0.2447 0.041 Uiso 1 1 calc R . . C21 C 0.0885(3) 1.11550(7) 0.18981(15) 0.0319(6) Uani 1 1 d . . . H21 H 0.1468 1.1243 0.1504 0.038 Uiso 1 1 calc R . . C22 C -0.0684(3) 1.12390(7) 0.19181(14) 0.0297(6) Uani 1 1 d . . . C23 C -0.1525(3) 1.11011(7) 0.25076(14) 0.0318(6) Uani 1 1 d . . . H23 H -0.2582 1.1150 0.2518 0.038 Uiso 1 1 calc R . . C24 C -0.0831(3) 1.08942(7) 0.30743(16) 0.0335(6) Uani 1 1 d . . . H24 H -0.1415 1.0810 0.3471 0.040 Uiso 1 1 calc R . . C25 C -0.1418(3) 1.14791(7) 0.13049(14) 0.0313(6) Uani 1 1 d . . . C26 C 0.3189(3) 1.04151(7) 0.67797(14) 0.0291(5) Uani 1 1 d . . . H26A H 0.2283 1.0562 0.6897 0.035 Uiso 1 1 calc R . . H26B H 0.3310 1.0217 0.7153 0.035 Uiso 1 1 calc R . . C27 C 0.4856(3) 1.08499(8) 0.74504(16) 0.0355(6) Uani 1 1 d . . . C28 C 0.6179(3) 1.10797(7) 0.74642(15) 0.0320(6) Uani 1 1 d . . . H28 H 0.6827 1.1084 0.7057 0.038 Uiso 1 1 calc R . . C29 C 0.6499(3) 1.12986(7) 0.80913(15) 0.0332(6) Uani 1 1 d . . . H29 H 0.7361 1.1456 0.8098 0.040 Uiso 1 1 calc R . . C30 C 0.5572(3) 1.12907(7) 0.87130(16) 0.0373(6) Uani 1 1 d . . . C31 C 0.4266(3) 1.10607(8) 0.86996(15) 0.0363(6) Uani 1 1 d . . . H31 H 0.3634 1.1053 0.9113 0.044 Uiso 1 1 calc R . . C32 C 0.3911(3) 1.08438(7) 0.80716(15) 0.0362(6) Uani 1 1 d . . . H32 H 0.3033 1.0692 0.8062 0.043 Uiso 1 1 calc R . . C33 C 0.5881(3) 1.15250(7) 0.93951(16) 0.0338(6) Uani 1 1 d . . . C34 C 0.6490(3) 0.77149(8) 0.57512(15) 0.0346(6) Uani 1 1 d . . . H34 H 0.5930 0.7493 0.5683 0.042 Uiso 1 1 calc R . . C35 C 0.4532(3) 0.79373(8) 0.66256(16) 0.0374(6) Uani 1 1 d . . . H35A H 0.4785 0.7814 0.7096 0.056 Uiso 1 1 calc R . . H35B H 0.3841 0.7781 0.6327 0.056 Uiso 1 1 calc R . . H35C H 0.4040 0.8174 0.6721 0.056 Uiso 1 1 calc R . . C36 C 0.6677(3) 0.83733(7) 0.63497(16) 0.0384(7) Uani 1 1 d . . . H36A H 0.7582 0.8344 0.6675 0.058 Uiso 1 1 calc R . . H36B H 0.5963 0.8541 0.6580 0.058 Uiso 1 1 calc R . . H36C H 0.6972 0.8476 0.5875 0.058 Uiso 1 1 calc R . . C37 C 0.0557(3) 0.73566(7) 0.66131(15) 0.0311(6) Uani 1 1 d . . . H37 H -0.0040 0.7495 0.6265 0.037 Uiso 1 1 calc R . . C38 C 0.2065(3) 0.73311(8) 0.78739(16) 0.0387(7) Uani 1 1 d . . . H38A H 0.2409 0.7100 0.7654 0.058 Uiso 1 1 calc R . . H38B H 0.1623 0.7279 0.8352 0.058 Uiso 1 1 calc R . . H38C H 0.2930 0.7499 0.7946 0.058 Uiso 1 1 calc R . . C39 C 0.0187(3) 0.78690(8) 0.75950(16) 0.0380(7) Uani 1 1 d . . . H39A H -0.0110 0.8013 0.7155 0.057 Uiso 1 1 calc R . . H39B H 0.0931 0.8009 0.7897 0.057 Uiso 1 1 calc R . . H39C H -0.0710 0.7820 0.7883 0.057 Uiso 1 1 calc R . . C40 C 0.8872(3) 0.65459(7) 0.73854(17) 0.0368(6) Uani 1 1 d . . . H40 H 0.8696 0.6548 0.6865 0.044 Uiso 1 1 calc R . . C41 C 0.6873(3) 0.70576(8) 0.74917(17) 0.0400(7) Uani 1 1 d . . . H41A H 0.6896 0.7034 0.6953 0.060 Uiso 1 1 calc R . . H41B H 0.7083 0.7314 0.7633 0.060 Uiso 1 1 calc R . . H41C H 0.5868 0.6987 0.7658 0.060 Uiso 1 1 calc R . . C42 C 0.8341(3) 0.68130(8) 0.86815(15) 0.0380(6) Uani 1 1 d . . . H42A H 0.8277 0.6561 0.8876 0.057 Uiso 1 1 calc R . . H42B H 0.7567 0.6967 0.8904 0.057 Uiso 1 1 calc R . . H42C H 0.9350 0.6914 0.8802 0.057 Uiso 1 1 calc R . . Cl1 Cl 0.64337(7) 0.690523(18) 0.34582(4) 0.03559(15) Uani 1 1 d . . . Co1 Co 0.43147(4) 0.685036(10) 0.42420(2) 0.03309(10) Uani 1 1 d . . . Co2 Co 0.07381(4) 0.686225(10) 0.52101(2) 0.03441(10) Uani 1 1 d . . . N1 N 0.5927(2) 0.80011(6) 0.62245(12) 0.0318(5) Uani 1 1 d . . . N2 N 0.0881(3) 0.75089(6) 0.73639(13) 0.0357(5) Uani 1 1 d . . . N3 N 0.8075(3) 0.68062(6) 0.78519(13) 0.0371(5) Uani 1 1 d . . . O1 O 0.4003(2) 0.73889(5) 0.44111(10) 0.0343(4) Uani 1 1 d . . . O2 O 0.1685(2) 0.73269(5) 0.48291(10) 0.0341(4) Uani 1 1 d . . . O3 O 0.25720(19) 0.90792(5) 0.51737(10) 0.0295(4) Uani 1 1 d . . . O4 O 0.15555(19) 1.06142(5) 0.36178(9) 0.0277(4) Uani 1 1 d . . . O5 O -0.0616(2) 1.15836(5) 0.07929(10) 0.0320(4) Uani 1 1 d . . . O6 O -0.2827(2) 1.15641(5) 0.13851(10) 0.0311(4) Uani 1 1 d . . . O7 O 0.45583(19) 1.06556(5) 0.68044(9) 0.0285(4) Uani 1 1 d . . . O8 O 0.7141(2) 1.16747(5) 0.94660(10) 0.0349(4) Uani 1 1 d . . . O9 O 0.5006(2) 1.15980(5) 0.98879(11) 0.0415(5) Uani 1 1 d . . . O10 O 0.7688(2) 0.77572(5) 0.54376(10) 0.0402(5) Uani 1 1 d . . . O11 O 0.1076(2) 0.70410(5) 0.64316(10) 0.0353(4) Uani 1 1 d . . . O12 O 0.9800(2) 0.63169(5) 0.76805(11) 0.0374(4) Uani 1 1 d . . . O1W O 0.0292(2) 0.62850(5) 0.57233(10) 0.0327(4) Uani 1 1 d . . . O2W O -0.1382(2) 0.70578(5) 0.49588(11) 0.0391(5) Uani 1 1 d . . . O3W O 0.9998(7) 0.49453(16) 0.3130(3) 0.0363(14) Uani 0.30 1 d P . . O4W O 0.4219(7) 0.51688(19) 0.3653(4) 0.0388(15) Uani 0.30 1 d P . . O5W O 0.5006(7) 0.57733(16) 0.4489(3) 0.0330(14) Uani 0.30 1 d P . . O6W O 0.8413(7) 0.43676(16) 0.4348(3) 0.0362(14) Uani 0.30 1 d P . . O7W O 0.2290(7) 0.04381(17) 0.0292(4) 0.0397(15) Uani 0.30 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0386(16) 0.0269(13) 0.0381(16) -0.0002(11) -0.0165(12) 0.0080(12) C2 0.0296(14) 0.0256(13) 0.0485(17) 0.0017(12) -0.0133(12) -0.0018(10) C3 0.0336(14) 0.0248(13) 0.0472(17) -0.0045(12) -0.0155(12) 0.0036(11) C4 0.0332(14) 0.0307(14) 0.0455(17) 0.0051(12) 0.0060(12) 0.0037(11) C5 0.0346(14) 0.0288(14) 0.0409(16) 0.0021(11) -0.0020(12) 0.0014(11) C6 0.0311(14) 0.0308(13) 0.0376(15) -0.0024(11) 0.0054(11) -0.0019(11) C7 0.0331(14) 0.0275(13) 0.0476(17) 0.0060(12) -0.0108(12) -0.0011(11) C8 0.0268(12) 0.0271(13) 0.0345(14) -0.0015(11) 0.0012(10) -0.0020(10) C9 0.0334(13) 0.0329(13) 0.0208(12) 0.0054(10) 0.0011(10) -0.0006(11) C10 0.0246(12) 0.0360(14) 0.0290(14) -0.0016(11) -0.0061(10) 0.0035(10) C11 0.0352(14) 0.0316(14) 0.0283(14) 0.0062(11) 0.0011(11) 0.0009(11) C12 0.0292(13) 0.0229(12) 0.0247(13) 0.0008(9) 0.0050(10) 0.0001(9) C13 0.0262(12) 0.0327(13) 0.0274(13) -0.0045(10) 0.0020(10) 0.0005(10) C14 0.0225(12) 0.0251(12) 0.0328(14) -0.0047(10) -0.0086(10) -0.0016(9) C15 0.0313(13) 0.0287(13) 0.0278(13) -0.0015(10) -0.0050(10) 0.0029(10) C16 0.0254(13) 0.0421(15) 0.0390(16) -0.0064(12) -0.0236(11) 0.0066(11) C17 0.0307(13) 0.0177(11) 0.0350(14) 0.0018(10) 0.0091(11) 0.0003(9) C18 0.0319(14) 0.0278(13) 0.0368(15) -0.0029(11) -0.0006(11) 0.0010(10) C19 0.0291(13) 0.0311(13) 0.0293(14) -0.0127(11) -0.0020(10) -0.0056(10) C20 0.0322(14) 0.0307(14) 0.0411(16) -0.0087(12) 0.0066(12) -0.0088(11) C21 0.0315(14) 0.0351(14) 0.0294(14) -0.0085(11) 0.0047(11) -0.0086(11) C22 0.0312(13) 0.0322(13) 0.0255(13) -0.0102(10) -0.0004(10) -0.0117(11) C23 0.0293(13) 0.0354(14) 0.0302(14) -0.0055(11) -0.0047(10) -0.0158(11) C24 0.0324(14) 0.0318(14) 0.0367(15) -0.0006(11) 0.0058(11) 0.0013(11) C25 0.0343(14) 0.0332(14) 0.0262(14) -0.0063(11) -0.0005(11) -0.0099(11) C26 0.0299(13) 0.0252(13) 0.0322(14) 0.0000(10) 0.0019(10) 0.0029(10) C27 0.0344(14) 0.0383(15) 0.0329(15) 0.0038(12) -0.0115(11) 0.0003(11) C28 0.0282(13) 0.0295(13) 0.0372(15) 0.0159(11) -0.0140(11) 0.0059(10) C29 0.0384(14) 0.0284(13) 0.0318(15) 0.0149(11) -0.0149(11) 0.0044(11) C30 0.0423(16) 0.0319(14) 0.0362(16) 0.0033(11) -0.0193(12) -0.0041(12) C31 0.0393(15) 0.0392(15) 0.0289(14) 0.0082(12) -0.0174(11) -0.0103(12) C32 0.0424(16) 0.0322(14) 0.0334(15) -0.0044(11) -0.0067(12) -0.0008(12) C33 0.0420(16) 0.0194(12) 0.0399(16) 0.0047(11) -0.0007(13) 0.0081(11) C34 0.0282(13) 0.0386(15) 0.0365(15) -0.0161(12) -0.0063(11) 0.0015(11) C35 0.0368(15) 0.0406(15) 0.0349(15) -0.0032(12) 0.0036(12) 0.0139(12) C36 0.0406(15) 0.0332(14) 0.0395(16) -0.0110(12) -0.0242(12) -0.0033(12) C37 0.0359(14) 0.0214(12) 0.0360(15) 0.0098(10) 0.0007(11) -0.0146(11) C38 0.0439(16) 0.0319(14) 0.0387(16) -0.0179(12) -0.0200(13) 0.0168(12) C39 0.0340(14) 0.0405(15) 0.0403(16) 0.0127(13) 0.0134(12) 0.0133(12) C40 0.0385(15) 0.0295(14) 0.0420(16) -0.0029(12) -0.0029(12) -0.0094(12) C41 0.0381(15) 0.0422(16) 0.0385(16) 0.0055(13) -0.0138(12) 0.0003(12) C42 0.0363(15) 0.0414(16) 0.0361(15) 0.0134(12) -0.0033(12) 0.0091(12) Cl1 0.0358(3) 0.0325(3) 0.0391(4) 0.0068(3) 0.0092(3) 0.0112(3) Co1 0.03281(19) 0.03055(19) 0.0362(2) 0.00096(15) 0.00556(15) 0.00101(15) Co2 0.0395(2) 0.03168(19) 0.0330(2) 0.00048(16) 0.01479(16) 0.00752(16) N1 0.0271(11) 0.0368(12) 0.0305(12) -0.0061(9) -0.0139(9) 0.0046(9) N2 0.0323(12) 0.0398(13) 0.0355(13) 0.0104(10) 0.0058(10) 0.0135(10) N3 0.0404(13) 0.0304(12) 0.0400(13) 0.0051(10) -0.0037(10) -0.0054(10) O1 0.0373(10) 0.0320(10) 0.0327(10) -0.0001(8) -0.0118(8) -0.0018(8) O2 0.0351(10) 0.0291(9) 0.0365(10) 0.0021(8) -0.0195(8) 0.0023(8) O3 0.0260(9) 0.0315(9) 0.0319(10) -0.0013(7) 0.0120(7) -0.0002(7) O4 0.0284(9) 0.0279(9) 0.0270(9) -0.0174(7) 0.0017(7) -0.0043(7) O5 0.0337(10) 0.0306(9) 0.0320(10) 0.0034(8) 0.0049(8) -0.0030(7) O6 0.0316(10) 0.0302(9) 0.0320(10) -0.0070(7) 0.0079(8) -0.0083(7) O7 0.0297(9) 0.0253(9) 0.0304(10) 0.0062(7) -0.0003(7) 0.0059(7) O8 0.0338(10) 0.0364(10) 0.0330(10) -0.0067(8) -0.0188(8) 0.0099(8) O9 0.0492(12) 0.0387(11) 0.0367(11) -0.0098(9) 0.0015(9) 0.0011(9) O10 0.0457(12) 0.0432(11) 0.0320(10) -0.0233(9) 0.0032(9) -0.0195(9) O11 0.0316(10) 0.0367(11) 0.0364(11) 0.0004(8) -0.0148(8) 0.0083(8) O12 0.0355(10) 0.0329(10) 0.0429(11) 0.0043(8) -0.0099(8) -0.0178(8) O1W 0.0325(9) 0.0310(10) 0.0356(10) 0.0043(8) 0.0128(8) 0.0116(7) O2W 0.0365(10) 0.0329(10) 0.0465(12) 0.0056(9) -0.0172(9) -0.0070(8) O3W 0.048(4) 0.030(3) 0.031(3) -0.009(3) 0.000(3) -0.012(3) O4W 0.028(3) 0.055(4) 0.033(3) 0.005(3) -0.007(3) 0.011(3) O5W 0.039(3) 0.027(3) 0.034(3) 0.013(3) 0.010(3) 0.009(3) O6W 0.045(4) 0.028(3) 0.035(3) 0.000(3) -0.008(3) -0.010(3) O7W 0.038(4) 0.037(3) 0.043(4) -0.012(3) -0.010(3) 0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.202(3) . ? C1 O1 1.253(3) . ? C1 C2 1.505(4) . ? C2 C7 1.378(4) . ? C2 C3 1.394(4) . ? C3 C4 1.390(4) . ? C3 H3 0.9300 . ? C4 C5 1.379(4) . ? C4 H4 0.9300 . ? C5 O3 1.373(3) . ? C5 C6 1.391(4) . ? C6 C7 1.367(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.430(3) . ? C8 C9 1.499(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.391(4) . ? C9 C14 1.406(3) . ? C10 C11 1.410(4) . ? C10 C16 1.509(3) . ? C11 C12 1.428(4) . ? C11 C26 1.486(4) . ? C12 C13 1.398(3) . ? C12 C17 1.514(3) . ? C13 C14 1.419(3) . ? C13 C18 1.489(4) . ? C14 C15 1.505(3) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C16 H16A 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 O4 1.424(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O4 1.376(3) . ? C19 C24 1.384(4) . ? C19 C20 1.391(4) . ? C20 C21 1.380(4) . ? C20 H20 0.9300 . ? C21 C22 1.389(4) . ? C21 H21 0.9300 . ? C22 C23 1.384(4) . ? C22 C25 1.504(4) . ? C23 C24 1.366(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O5 1.220(3) . ? C25 O6 1.267(3) . ? C26 O7 1.458(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O7 1.354(3) . ? C27 C32 1.395(4) . ? C27 C28 1.403(4) . ? C28 C29 1.377(4) . ? C28 H28 0.9300 . ? C29 C30 1.386(4) . ? C29 H29 0.9300 . ? C30 C31 1.392(4) . ? C30 C33 1.485(4) . ? C31 C32 1.380(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O9 1.204(3) . ? C33 O8 1.214(3) . ? C34 O10 1.202(3) . ? C34 N1 1.416(3) . ? C34 H34 0.9300 . ? C35 N1 1.439(3) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 N1 1.486(3) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 O11 1.254(3) . ? C37 N2 1.455(4) . ? C37 H37 0.9300 . ? C38 N2 1.482(3) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N2 1.477(3) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 O12 1.244(3) . ? C40 N3 1.434(4) . ? C40 H40 0.9300 . ? C41 N3 1.495(3) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 N3 1.481(4) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? Cl1 Co1 2.3461(7) . ? Co1 O9 1.861(2) 2_646 ? Co1 O6 1.9543(19) 2_545 ? Co1 O1 1.9566(18) . ? Co2 O2 1.9722(19) . ? Co2 O2W 1.9938(19) . ? Co2 O8 2.0128(18) 2_646 ? Co2 O5 2.0353(18) 2_545 ? Co2 O11 2.2667(19) . ? Co2 O1W 2.2819(17) . ? O5 Co2 2.0353(18) 2 ? O6 Co1 1.9543(19) 2 ? O8 Co2 2.0128(18) 2_656 ? O9 Co1 1.861(2) 2_656 ? 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 O2 C1 O1 124.3(2) . . ? O2 C1 C2 121.3(2) . . ? O1 C1 C2 114.3(2) . . ? C7 C2 C3 119.9(2) . . ? C7 C2 C1 122.1(3) . . ? C3 C2 C1 117.9(2) . . ? C4 C3 C2 119.2(3) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 119.7(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? O3 C5 C4 114.5(2) . . ? O3 C5 C6 124.4(2) . . ? C4 C5 C6 121.1(2) . . ? C7 C6 C5 118.7(2) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C6 C7 C2 121.4(3) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? O3 C8 C9 105.94(19) . . ? O3 C8 H8A 110.5 . . ? C9 C8 H8A 110.5 . . ? O3 C8 H8B 110.5 . . ? C9 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? C10 C9 C14 120.6(2) . . ? C10 C9 C8 120.9(2) . . ? C14 C9 C8 118.5(2) . . ? C9 C10 C11 120.1(2) . . ? C9 C10 C16 120.9(2) . . ? C11 C10 C16 118.9(2) . . ? C10 C11 C12 119.6(2) . . ? C10 C11 C26 120.6(2) . . ? C12 C11 C26 119.8(2) . . ? C13 C12 C11 119.5(2) . . ? C13 C12 C17 119.7(2) . . ? C11 C12 C17 120.8(2) . . ? C12 C13 C14 120.0(2) . . ? C12 C13 C18 119.3(2) . . ? C14 C13 C18 120.6(2) . . ? C9 C14 C13 119.8(2) . . ? C9 C14 C15 120.5(2) . . ? C13 C14 C15 119.7(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C10 C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 C13 107.8(2) . . ? O4 C18 H18A 110.1 . . ? C13 C18 H18A 110.1 . . ? O4 C18 H18B 110.1 . . ? C13 C18 H18B 110.1 . . ? H18A C18 H18B 108.5 . . ? O4 C19 C24 125.6(2) . . ? O4 C19 C20 116.3(2) . . ? C24 C19 C20 118.1(3) . . ? C21 C20 C19 121.4(3) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 119.7(2) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 118.8(3) . . ? C23 C22 C25 121.9(2) . . ? C21 C22 C25 119.3(2) . . ? C24 C23 C22 121.2(3) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C19 120.8(2) . . ? C23 C24 H24 119.6 . . ? C19 C24 H24 119.6 . . ? O5 C25 O6 125.8(3) . . ? O5 C25 C22 118.4(2) . . ? O6 C25 C22 115.8(2) . . ? O7 C26 C11 109.5(2) . . ? O7 C26 H26A 109.8 . . ? C11 C26 H26A 109.8 . . ? O7 C26 H26B 109.8 . . ? C11 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? O7 C27 C32 124.2(2) . . ? O7 C27 C28 116.2(2) . . ? C32 C27 C28 119.6(3) . . ? C29 C28 C27 118.9(3) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C28 C29 C30 121.7(3) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C31 119.3(3) . . ? C29 C30 C33 123.0(3) . . ? C31 C30 C33 117.7(3) . . ? C32 C31 C30 119.8(3) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C27 120.7(3) . . ? C31 C32 H32 119.7 . . ? C27 C32 H32 119.7 . . ? O9 C33 O8 114.5(3) . . ? O9 C33 C30 127.8(3) . . ? O8 C33 C30 117.6(3) . . ? O10 C34 N1 120.3(2) . . ? O10 C34 H34 119.8 . . ? N1 C34 H34 119.8 . . ? N1 C35 H35A 109.5 . . ? N1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N1 C36 H36A 109.5 . . ? N1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O11 C37 N2 120.6(2) . . ? O11 C37 H37 119.7 . . ? N2 C37 H37 119.7 . . ? N2 C38 H38A 109.5 . . ? N2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N2 C39 H39A 109.5 . . ? N2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O12 C40 N3 119.6(3) . . ? O12 C40 H40 120.2 . . ? N3 C40 H40 120.2 . . ? N3 C41 H41A 109.5 . . ? N3 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N3 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 H42A 109.5 . . ? N3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O9 Co1 O6 113.74(8) 2_646 2_545 ? O9 Co1 O1 112.63(8) 2_646 . ? O6 Co1 O1 120.33(7) 2_545 . ? O9 Co1 Cl1 107.58(7) 2_646 . ? O6 Co1 Cl1 102.51(5) 2_545 . ? O1 Co1 Cl1 97.13(6) . . ? O2 Co2 O2W 91.17(7) . . ? O2 Co2 O8 89.47(7) . 2_646 ? O2W Co2 O8 176.27(8) . 2_646 ? O2 Co2 O5 96.69(7) . 2_545 ? O2W Co2 O5 87.46(8) . 2_545 ? O8 Co2 O5 96.12(7) 2_646 2_545 ? O2 Co2 O11 93.00(7) . . ? O2W Co2 O11 101.64(7) . . ? O8 Co2 O11 74.65(7) 2_646 . ? O5 Co2 O11 166.58(7) 2_545 . ? O2 Co2 O1W 165.19(7) . . ? O2W Co2 O1W 103.63(7) . . ? O8 Co2 O1W 75.73(7) 2_646 . ? O5 Co2 O1W 84.70(7) 2_545 . ? O11 Co2 O1W 83.58(7) . . ? C34 N1 C35 119.5(2) . . ? C34 N1 C36 124.8(2) . . ? C35 N1 C36 115.8(2) . . ? C37 N2 C39 120.7(2) . . ? C37 N2 C38 120.4(2) . . ? C39 N2 C38 118.5(2) . . ? C40 N3 C42 121.6(2) . . ? C40 N3 C41 118.6(2) . . ? C42 N3 C41 119.7(2) . . ? C1 O1 Co1 122.17(17) . . ? C1 O2 Co2 152.30(17) . . ? C5 O3 C8 119.28(19) . . ? C19 O4 C18 115.79(19) . . ? C25 O5 Co2 141.80(18) . 2 ? C25 O6 Co1 132.41(17) . 2 ? C27 O7 C26 116.94(19) . . ? C33 O8 Co2 167.89(19) . 2_656 ? C33 O9 Co1 121.2(2) . 2_656 ? C37 O11 Co2 117.45(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 -176.5(3) . . . . ? O1 C1 C2 C7 1.2(4) . . . . ? O2 C1 C2 C3 6.4(4) . . . . ? O1 C1 C2 C3 -175.9(2) . . . . ? C7 C2 C3 C4 0.3(4) . . . . ? C1 C2 C3 C4 177.4(2) . . . . ? C2 C3 C4 C5 -0.4(4) . . . . ? C3 C4 C5 O3 -178.9(2) . . . . ? C3 C4 C5 C6 1.2(4) . . . . ? O3 C5 C6 C7 178.3(3) . . . . ? C4 C5 C6 C7 -1.9(4) . . . . ? C5 C6 C7 C2 1.8(4) . . . . ? C3 C2 C7 C6 -1.0(4) . . . . ? C1 C2 C7 C6 -178.0(3) . . . . ? O3 C8 C9 C10 94.3(3) . . . . ? O3 C8 C9 C14 -83.3(3) . . . . ? C14 C9 C10 C11 -0.9(4) . . . . ? C8 C9 C10 C11 -178.4(2) . . . . ? C14 C9 C10 C16 177.4(2) . . . . ? C8 C9 C10 C16 -0.1(4) . . . . ? C9 C10 C11 C12 -4.7(4) . . . . ? C16 C10 C11 C12 177.0(2) . . . . ? C9 C10 C11 C26 174.1(2) . . . . ? C16 C10 C11 C26 -4.3(4) . . . . ? C10 C11 C12 C13 8.5(4) . . . . ? C26 C11 C12 C13 -170.2(2) . . . . ? C10 C11 C12 C17 -170.2(2) . . . . ? C26 C11 C12 C17 11.0(4) . . . . ? C11 C12 C13 C14 -6.8(4) . . . . ? C17 C12 C13 C14 172.0(2) . . . . ? C11 C12 C13 C18 169.2(2) . . . . ? C17 C12 C13 C18 -12.0(3) . . . . ? C10 C9 C14 C13 2.7(4) . . . . ? C8 C9 C14 C13 -179.7(2) . . . . ? C10 C9 C14 C15 -176.3(2) . . . . ? C8 C9 C14 C15 1.3(4) . . . . ? C12 C13 C14 C9 1.2(4) . . . . ? C18 C13 C14 C9 -174.7(2) . . . . ? C12 C13 C14 C15 -179.8(2) . . . . ? C18 C13 C14 C15 4.3(4) . . . . ? C12 C13 C18 O4 102.6(2) . . . . ? C14 C13 C18 O4 -81.4(3) . . . . ? O4 C19 C20 C21 -176.8(2) . . . . ? C24 C19 C20 C21 1.0(4) . . . . ? C19 C20 C21 C22 -0.7(4) . . . . ? C20 C21 C22 C23 -0.6(4) . . . . ? C20 C21 C22 C25 178.8(2) . . . . ? C21 C22 C23 C24 1.8(4) . . . . ? C25 C22 C23 C24 -177.7(2) . . . . ? C22 C23 C24 C19 -1.5(4) . . . . ? O4 C19 C24 C23 177.7(2) . . . . ? C20 C19 C24 C23 0.1(4) . . . . ? C23 C22 C25 O5 -178.3(2) . . . . ? C21 C22 C25 O5 2.3(3) . . . . ? C23 C22 C25 O6 3.8(3) . . . . ? C21 C22 C25 O6 -175.7(2) . . . . ? C10 C11 C26 O7 95.5(3) . . . . ? C12 C11 C26 O7 -85.8(3) . . . . ? O7 C27 C28 C29 176.8(2) . . . . ? C32 C27 C28 C29 -0.9(4) . . . . ? C27 C28 C29 C30 1.5(4) . . . . ? C28 C29 C30 C31 -1.2(4) . . . . ? C28 C29 C30 C33 -179.6(2) . . . . ? C29 C30 C31 C32 0.1(4) . . . . ? C33 C30 C31 C32 178.6(2) . . . . ? C30 C31 C32 C27 0.5(4) . . . . ? O7 C27 C32 C31 -177.6(2) . . . . ? C28 C27 C32 C31 -0.2(4) . . . . ? C29 C30 C33 O9 163.3(3) . . . . ? C31 C30 C33 O9 -15.1(4) . . . . ? C29 C30 C33 O8 -14.0(4) . . . . ? C31 C30 C33 O8 167.6(2) . . . . ? O10 C34 N1 C35 -176.8(3) . . . . ? O10 C34 N1 C36 3.0(4) . . . . ? O11 C37 N2 C39 -176.0(2) . . . . ? O11 C37 N2 C38 11.8(4) . . . . ? O12 C40 N3 C42 0.7(4) . . . . ? O12 C40 N3 C41 -175.2(2) . . . . ? O2 C1 O1 Co1 -2.6(4) . . . . ? C2 C1 O1 Co1 179.74(17) . . . . ? O9 Co1 O1 C1 -82.7(2) 2_646 . . . ? O6 Co1 O1 C1 55.8(2) 2_545 . . . ? Cl1 Co1 O1 C1 164.86(19) . . . . ? O1 C1 O2 Co2 36.7(6) . . . . ? C2 C1 O2 Co2 -145.8(3) . . . . ? O2W Co2 O2 C1 -176.3(4) . . . . ? O8 Co2 O2 C1 7.4(4) 2_646 . . . ? O5 Co2 O2 C1 -88.7(4) 2_545 . . . ? O11 Co2 O2 C1 82.0(4) . . . . ? O1W Co2 O2 C1 5.9(6) . . . . ? C4 C5 O3 C8 178.1(2) . . . . ? C6 C5 O3 C8 -2.1(4) . . . . ? C9 C8 O3 C5 174.5(2) . . . . ? C24 C19 O4 C18 6.3(3) . . . . ? C20 C19 O4 C18 -176.1(2) . . . . ? C13 C18 O4 C19 -178.36(19) . . . . ? O6 C25 O5 Co2 -7.8(5) . . . 2 ? C22 C25 O5 Co2 174.53(18) . . . 2 ? O5 C25 O6 Co1 4.2(4) . . . 2 ? C22 C25 O6 Co1 -178.10(15) . . . 2 ? C32 C27 O7 C26 -2.5(4) . . . . ? C28 C27 O7 C26 180.0(2) . . . . ? C11 C26 O7 C27 175.8(2) . . . . ? O9 C33 O8 Co2 60.1(9) . . . 2_656 ? C30 C33 O8 Co2 -122.3(8) . . . 2_656 ? O8 C33 O9 Co1 -10.1(3) . . . 2_656 ? C30 C33 O9 Co1 172.5(2) . . . 2_656 ? N2 C37 O11 Co2 -173.05(16) . . . . ? O2 Co2 O11 C37 53.43(18) . . . . ? O2W Co2 O11 C37 -38.39(18) . . . . ? O8 Co2 O11 C37 142.06(19) 2_646 . . . ? O5 Co2 O11 C37 -170.3(3) 2_545 . . . ? O1W Co2 O11 C37 -141.03(18) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.322 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.050