# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wen-Zhen Wang' _publ_contact_author_email smpeng@ntu.edu.tw loop_ _publ_author_name 'Wen-Zhen Wang' 'Lin Hsieh' Rayyat.H.Ismayilov 'Chia-Hung Hsu' 'Po-Chun Liu' 'Yi-Hung Liu' 'Gene-Hsiang Lee' 'Shie-Ming Peng' data_ic13970 _database_code_depnum_ccdc_archive 'CCDC 875005' #TrackingRef '- ic13970 Cu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H88 Cl4 Cu2 N12 O22' _chemical_formula_weight 1982.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.8833(3) _cell_length_b 33.8521(9) _cell_length_c 19.1520(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.9954(12) _cell_angle_gamma 90.00 _cell_volume 8966.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16475 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4104 _exptl_absorpt_coefficient_mu 0.675 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42273 _diffrn_reflns_av_R_equivalents 0.1001 _diffrn_reflns_av_sigmaI/netI 0.1638 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15700 _reflns_number_gt 7157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1230P)^2^+10.9992P] 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 15700 _refine_ls_number_parameters 1197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1969 _refine_ls_R_factor_gt 0.0774 _refine_ls_wR_factor_ref 0.2667 _refine_ls_wR_factor_gt 0.2200 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.003 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 Cu1 Cu 0.26619(6) 0.32706(3) 0.75959(5) 0.0336(3) Uani 1 1 d . . . Cu2 Cu 0.26074(6) 0.41290(3) 0.76157(5) 0.0370(3) Uani 1 1 d . . . N1 N 0.2131(4) 0.32889(19) 0.6592(3) 0.0353(16) Uani 1 1 d . . . N2 N 0.2078(4) 0.39737(19) 0.6612(3) 0.0321(15) Uani 1 1 d . . . N3 N 0.2075(4) 0.46332(19) 0.6777(3) 0.0381(16) Uani 1 1 d . . . N4 N 0.3200(4) 0.32470(18) 0.8606(3) 0.0319(15) Uani 1 1 d . . . N5 N 0.3169(4) 0.3925(2) 0.8617(3) 0.0314(15) Uani 1 1 d . . . N6 N 0.3028(4) 0.4585(2) 0.8500(3) 0.0386(17) Uani 1 1 d . . . N7 N 0.3881(4) 0.2837(2) 0.7285(3) 0.0423(17) Uani 1 1 d . . . N8 N 0.3990(4) 0.3503(2) 0.7258(3) 0.0414(17) Uani 1 1 d . . . N9 N 0.3939(4) 0.4184(2) 0.7298(3) 0.0401(17) Uani 1 1 d . . . N10 N 0.1513(4) 0.27608(19) 0.7837(3) 0.0357(16) Uani 1 1 d . . . N11 N 0.1311(4) 0.34227(18) 0.7924(3) 0.0284(15) Uani 1 1 d . . . N12 N 0.1272(4) 0.41036(18) 0.7918(3) 0.0317(15) Uani 1 1 d . . . C1 C 0.1978(5) 0.2964(2) 0.6234(5) 0.040(2) Uani 1 1 d . . . H1 H 0.2108 0.2722 0.6475 0.049 Uiso 1 1 calc R . . C2 C 0.1631(5) 0.2940(2) 0.5512(4) 0.037(2) Uani 1 1 d . . . C3 C 0.1520(5) 0.2570(3) 0.5187(4) 0.043(2) Uani 1 1 d . . . H3 H 0.1657 0.2333 0.5443 0.052 Uiso 1 1 calc R . . C4 C 0.1208(6) 0.2560(3) 0.4487(5) 0.054(3) Uani 1 1 d . . . H4 H 0.1149 0.2313 0.4253 0.065 Uiso 1 1 calc R . . C5 C 0.0974(6) 0.2908(3) 0.4107(5) 0.049(2) Uani 1 1 d . . . H5 H 0.0745 0.2893 0.3626 0.059 Uiso 1 1 calc R . . C6 C 0.1073(5) 0.3265(3) 0.4425(4) 0.042(2) Uani 1 1 d . . . H6 H 0.0911 0.3500 0.4169 0.051 Uiso 1 1 calc R . . C7 C 0.1420(5) 0.3286(2) 0.5146(4) 0.036(2) Uani 1 1 d . . . C8 C 0.1552(5) 0.3658(2) 0.5517(4) 0.035(2) Uani 1 1 d . . . C9 C 0.1372(5) 0.4031(2) 0.5220(4) 0.0330(19) Uani 1 1 d . . . H9 H 0.1122 0.4051 0.4744 0.040 Uiso 1 1 calc R . . C10 C 0.1553(5) 0.4370(2) 0.5608(4) 0.035(2) Uani 1 1 d . . . C11 C 0.1381(5) 0.4775(2) 0.5344(5) 0.039(2) Uani 1 1 d . . . C12 C 0.1069(6) 0.4870(3) 0.4658(5) 0.046(2) Uani 1 1 d . . . H12 H 0.0967 0.4667 0.4318 0.056 Uiso 1 1 calc R . . C13 C 0.0905(5) 0.5259(3) 0.4464(5) 0.047(2) Uani 1 1 d . . . H13 H 0.0681 0.5320 0.3993 0.056 Uiso 1 1 calc R . . C14 C 0.1065(6) 0.5562(3) 0.4953(5) 0.050(2) Uani 1 1 d . . . H14 H 0.0959 0.5829 0.4814 0.061 Uiso 1 1 calc R . . C15 C 0.1373(6) 0.5476(3) 0.5630(5) 0.050(2) Uani 1 1 d . . . H15 H 0.1473 0.5683 0.5963 0.060 Uiso 1 1 calc R . . C16 C 0.1543(6) 0.5083(3) 0.5838(5) 0.044(2) Uani 1 1 d . . . C17 C 0.1887(6) 0.4991(3) 0.6545(5) 0.044(2) Uani 1 1 d . . . H17 H 0.1984 0.5204 0.6867 0.053 Uiso 1 1 calc R . . C18 C 0.1918(5) 0.3645(2) 0.6237(4) 0.0327(19) Uani 1 1 d . . . C19 C 0.1897(5) 0.4329(2) 0.6309(4) 0.0339(19) Uani 1 1 d . . . C20 C 0.3367(5) 0.2917(3) 0.8940(4) 0.040(2) Uani 1 1 d . . . H20 H 0.3223 0.2679 0.8690 0.047 Uiso 1 1 calc R . . C21 C 0.3750(5) 0.2883(2) 0.9654(4) 0.036(2) Uani 1 1 d . . . C22 C 0.3897(6) 0.2511(3) 0.9971(5) 0.046(2) Uani 1 1 d . . . H22 H 0.3735 0.2277 0.9713 0.055 Uiso 1 1 calc R . . C23 C 0.4276(6) 0.2489(3) 1.0650(5) 0.047(2) Uani 1 1 d . . . H23 H 0.4368 0.2238 1.0870 0.057 Uiso 1 1 calc R . . C24 C 0.4528(6) 0.2830(3) 1.1022(5) 0.048(2) Uani 1 1 d . . . H24 H 0.4808 0.2808 1.1491 0.058 Uiso 1 1 calc R . . C25 C 0.4385(6) 0.3196(3) 1.0736(4) 0.044(2) Uani 1 1 d . . . H25 H 0.4551 0.3426 1.1003 0.052 Uiso 1 1 calc R . . C26 C 0.3992(5) 0.3227(2) 1.0043(4) 0.037(2) Uani 1 1 d . . . C27 C 0.3769(5) 0.3598(2) 0.9678(4) 0.036(2) Uani 1 1 d . . . C28 C 0.3888(5) 0.3967(2) 1.0019(4) 0.038(2) Uani 1 1 d . . . H28 H 0.4132 0.3979 1.0497 0.046 Uiso 1 1 calc R . . C29 C 0.3648(5) 0.4313(2) 0.9653(4) 0.036(2) Uani 1 1 d . . . C30 C 0.3732(5) 0.4714(2) 0.9940(5) 0.037(2) Uani 1 1 d . . . C31 C 0.4073(5) 0.4803(3) 1.0620(5) 0.044(2) Uani 1 1 d . . . H31 H 0.4245 0.4597 1.0944 0.053 Uiso 1 1 calc R . . C32 C 0.4164(6) 0.5191(3) 1.0827(5) 0.053(2) Uani 1 1 d . . . H32 H 0.4409 0.5251 1.1294 0.063 Uiso 1 1 calc R . . C33 C 0.3908(6) 0.5496(3) 1.0372(6) 0.059(3) Uani 1 1 d . . . H33 H 0.3985 0.5761 1.0529 0.071 Uiso 1 1 calc R . . C34 C 0.3550(6) 0.5425(2) 0.9705(6) 0.052(2) Uani 1 1 d . . . H34 H 0.3356 0.5639 0.9403 0.062 Uiso 1 1 calc R . . C35 C 0.3465(6) 0.5028(2) 0.9457(5) 0.045(2) Uani 1 1 d . . . C36 C 0.3121(5) 0.4945(3) 0.8752(5) 0.043(2) Uani 1 1 d . . . H36 H 0.2951 0.5161 0.8448 0.052 Uiso 1 1 calc R . . C37 C 0.3389(5) 0.3598(2) 0.8972(4) 0.034(2) Uani 1 1 d . . . C38 C 0.3295(5) 0.4273(3) 0.8937(4) 0.034(2) Uani 1 1 d . . . C39 C 0.4256(6) 0.2496(3) 0.7231(4) 0.046(2) Uani 1 1 d . . . H39 H 0.3862 0.2273 0.7307 0.056 Uiso 1 1 calc R . . C40 C 0.5234(6) 0.2422(3) 0.7064(4) 0.046(2) Uani 1 1 d . . . C41 C 0.5593(7) 0.2044(3) 0.7048(5) 0.058(3) Uani 1 1 d . . . H41 H 0.5190 0.1828 0.7147 0.069 Uiso 1 1 calc R . . C42 C 0.6538(8) 0.1971(3) 0.6891(5) 0.064(3) Uani 1 1 d . . . H42 H 0.6784 0.1710 0.6873 0.077 Uiso 1 1 calc R . . C43 C 0.7107(7) 0.2297(3) 0.6761(5) 0.062(3) Uani 1 1 d . . . H43 H 0.7753 0.2252 0.6652 0.075 Uiso 1 1 calc R . . C44 C 0.6787(6) 0.2683(3) 0.6780(4) 0.054(2) Uani 1 1 d . . . H44 H 0.7201 0.2899 0.6697 0.065 Uiso 1 1 calc R . . C45 C 0.5813(6) 0.2746(3) 0.6930(4) 0.045(2) Uani 1 1 d . . . C46 C 0.5410(5) 0.3137(3) 0.6975(4) 0.040(2) Uani 1 1 d . . . C47 C 0.5867(6) 0.3498(3) 0.6862(4) 0.046(2) Uani 1 1 d . . . H47 H 0.6509 0.3497 0.6725 0.056 Uiso 1 1 calc R . . C48 C 0.5404(5) 0.3861(3) 0.6946(4) 0.041(2) Uani 1 1 d . . . C49 C 0.5845(6) 0.4239(3) 0.6877(4) 0.047(2) Uani 1 1 d . . . C50 C 0.6787(6) 0.4297(3) 0.6686(5) 0.061(3) Uani 1 1 d . . . H50 H 0.7172 0.4078 0.6575 0.073 Uiso 1 1 calc R . . C51 C 0.7146(7) 0.4672(3) 0.6662(5) 0.066(3) Uani 1 1 d . . . H51 H 0.7788 0.4704 0.6535 0.079 Uiso 1 1 calc R . . C52 C 0.6640(6) 0.5006(3) 0.6810(5) 0.060(3) Uani 1 1 d . . . H52 H 0.6921 0.5261 0.6785 0.072 Uiso 1 1 calc R . . C53 C 0.5696(6) 0.4958(3) 0.6997(5) 0.057(3) Uani 1 1 d . . . H53 H 0.5318 0.5182 0.7097 0.069 Uiso 1 1 calc R . . C54 C 0.5308(6) 0.4574(3) 0.7036(4) 0.044(2) Uani 1 1 d . . . C55 C 0.4356(5) 0.4524(3) 0.7239(4) 0.042(2) Uani 1 1 d . . . H55 H 0.4001 0.4754 0.7337 0.050 Uiso 1 1 calc R . . C56 C 0.4441(6) 0.3162(3) 0.7163(4) 0.044(2) Uani 1 1 d . . . C57 C 0.4444(6) 0.3853(3) 0.7160(4) 0.045(2) Uani 1 1 d . . . C58 C 0.1154(6) 0.2404(2) 0.7867(4) 0.040(2) Uani 1 1 d . . . H58 H 0.1563 0.2189 0.7771 0.048 Uiso 1 1 calc R . . C59 C 0.0190(5) 0.2311(2) 0.8034(4) 0.037(2) Uani 1 1 d . . . C60 C -0.0132(6) 0.1914(2) 0.8049(4) 0.044(2) Uani 1 1 d . . . H60 H 0.0296 0.1706 0.7952 0.053 Uiso 1 1 calc R . . C61 C -0.1034(6) 0.1829(3) 0.8198(5) 0.051(2) Uani 1 1 d . . . H61 H -0.1249 0.1563 0.8201 0.061 Uiso 1 1 calc R . . C62 C -0.1658(6) 0.2138(2) 0.8349(4) 0.048(2) Uani 1 1 d . . . H62 H -0.2297 0.2076 0.8453 0.058 Uiso 1 1 calc R . . C63 C -0.1384(6) 0.2522(2) 0.8353(4) 0.042(2) Uani 1 1 d . . . H63 H -0.1823 0.2723 0.8463 0.051 Uiso 1 1 calc R . . C64 C -0.0450(5) 0.2619(2) 0.8195(4) 0.0333(19) Uani 1 1 d . . . C65 C -0.0068(5) 0.3021(2) 0.8153(4) 0.0306(18) Uani 1 1 d . . . C66 C -0.0599(5) 0.3364(2) 0.8261(4) 0.0343(19) Uani 1 1 d . . . H66 H -0.1246 0.3346 0.8384 0.041 Uiso 1 1 calc R . . C67 C -0.0175(6) 0.3734(2) 0.8187(4) 0.035(2) Uani 1 1 d . . . C68 C -0.0698(5) 0.4102(2) 0.8250(4) 0.0338(19) Uani 1 1 d . . . C69 C -0.1655(6) 0.4125(2) 0.8371(4) 0.045(2) Uani 1 1 d . . . H69 H -0.2005 0.3889 0.8439 0.054 Uiso 1 1 calc R . . C70 C -0.2120(6) 0.4483(3) 0.8398(5) 0.052(2) Uani 1 1 d . . . H70 H -0.2783 0.4493 0.8484 0.062 Uiso 1 1 calc R . . C71 C -0.1602(7) 0.4839(3) 0.8294(4) 0.053(2) Uani 1 1 d . . . H71 H -0.1916 0.5087 0.8315 0.064 Uiso 1 1 calc R . . C72 C -0.0661(6) 0.4821(2) 0.8167(4) 0.044(2) Uani 1 1 d . . . H72 H -0.0313 0.5057 0.8096 0.053 Uiso 1 1 calc R . . C73 C -0.0196(5) 0.4455(2) 0.8139(4) 0.036(2) Uani 1 1 d . . . C74 C 0.0779(5) 0.4429(2) 0.7983(4) 0.037(2) Uani 1 1 d . . . H74 H 0.1107 0.4670 0.7919 0.044 Uiso 1 1 calc R . . C75 C 0.0892(5) 0.3070(2) 0.7990(4) 0.0327(19) Uani 1 1 d . . . C76 C 0.0792(5) 0.3752(2) 0.8017(4) 0.0281(18) Uani 1 1 d . . . Cl1 Cl 0.41845(14) 0.14272(6) 0.13686(11) 0.0408(5) Uani 1 1 d . . . O1 O 0.4921(4) 0.16918(15) 0.1620(3) 0.0429(14) Uani 1 1 d . . . O2 O 0.4488(5) 0.10337(16) 0.1524(3) 0.0610(17) Uani 1 1 d . . . O3 O 0.3990(4) 0.14728(17) 0.0633(3) 0.0587(17) Uani 1 1 d . . . O4 O 0.3339(4) 0.1506(2) 0.1716(3) 0.074(2) Uani 1 1 d . . . Cl2 Cl 0.11253(14) 0.15313(6) 0.37764(11) 0.0406(5) Uani 1 1 d . . . O5 O 0.1981(4) 0.16997(17) 0.3511(3) 0.0614(18) Uani 1 1 d . . . O6 O 0.0953(4) 0.11455(17) 0.3475(3) 0.0600(17) Uani 1 1 d . . . O7 O 0.0322(4) 0.17852(16) 0.3582(3) 0.0467(15) Uani 1 1 d . . . O8 O 0.1269(4) 0.14978(17) 0.4523(3) 0.0540(15) Uani 1 1 d . . . Cl3 Cl 0.6097(2) 0.08605(8) 0.79089(14) 0.0759(8) Uani 1 1 d . . . O9 O 0.6867(8) 0.0857(3) 0.8434(5) 0.167(5) Uani 1 1 d . . . O10 O 0.5574(8) 0.1192(3) 0.7939(6) 0.166(5) Uani 1 1 d . . . O11 O 0.5517(12) 0.0521(3) 0.8009(5) 0.218(7) Uani 1 1 d . . . O12 O 0.6416(7) 0.0806(3) 0.7242(4) 0.132(4) Uani 1 1 d . . . Cl4 Cl 0.09228(18) 0.08902(8) 0.73035(15) 0.0632(7) Uani 1 1 d . . . O13 O 0.0531(7) 0.0814(5) 0.6653(6) 0.229(8) Uani 1 1 d . . . O14 O 0.1468(9) 0.0583(3) 0.7508(5) 0.181(6) Uani 1 1 d . . . O15 O 0.1393(7) 0.1233(3) 0.7306(6) 0.159(5) Uani 1 1 d . . . O16 O 0.0166(6) 0.0945(2) 0.7739(4) 0.111(3) Uani 1 1 d . . . O17 O 0.8721(4) 0.3417(2) 0.0762(4) 0.076(2) Uani 1 1 d . . . C77 C 0.8710(9) 0.4060(4) 0.1295(8) 0.121(5) Uani 1 1 d . . . H77A H 0.9325 0.3987 0.1553 0.181 Uiso 1 1 calc R . . H77B H 0.8177 0.3999 0.1581 0.181 Uiso 1 1 calc R . . H77C H 0.8711 0.4344 0.1192 0.181 Uiso 1 1 calc R . . C78 C 0.8585(8) 0.3833(4) 0.0625(8) 0.104(4) Uani 1 1 d . . . H78A H 0.7929 0.3879 0.0394 0.124 Uiso 1 1 calc R . . H78B H 0.9061 0.3925 0.0305 0.124 Uiso 1 1 calc R . . C79 C 0.8626(8) 0.3177(4) 0.0133(6) 0.084(3) Uani 1 1 d . . . H79A H 0.9015 0.3291 -0.0226 0.101 Uiso 1 1 calc R . . H79B H 0.7941 0.3168 -0.0060 0.101 Uiso 1 1 calc R . . C80 C 0.8976(7) 0.2769(4) 0.0323(6) 0.085(3) Uani 1 1 d . . . H80A H 0.8635 0.2670 0.0714 0.127 Uiso 1 1 calc R . . H80B H 0.9672 0.2776 0.0460 0.127 Uiso 1 1 calc R . . H80C H 0.8849 0.2594 -0.0083 0.127 Uiso 1 1 calc R . . O18 O 0.1188(5) 0.4014(2) -0.0056(3) 0.074(2) Uani 1 1 d . . . C81 C 0.1062(8) 0.4709(4) -0.0155(6) 0.087(4) Uani 1 1 d . . . H81A H 0.0396 0.4690 -0.0368 0.131 Uiso 1 1 calc R . . H81B H 0.1510 0.4702 -0.0523 0.131 Uiso 1 1 calc R . . H81C H 0.1144 0.4958 0.0105 0.131 Uiso 1 1 calc R . . C82 C 0.1272(8) 0.4366(4) 0.0341(6) 0.080(3) Uani 1 1 d . . . H82A H 0.1933 0.4390 0.0576 0.096 Uiso 1 1 calc R . . H82B H 0.0806 0.4364 0.0704 0.096 Uiso 1 1 calc R . . C83 C 0.1348(8) 0.3686(3) 0.0387(6) 0.077(3) Uani 1 1 d . . . H83A H 0.0854 0.3676 0.0730 0.093 Uiso 1 1 calc R . . H83B H 0.1994 0.3704 0.0648 0.093 Uiso 1 1 calc R . . C84 C 0.1285(7) 0.3320(3) -0.0063(5) 0.072(3) Uani 1 1 d . . . H84A H 0.1707 0.3350 -0.0444 0.108 Uiso 1 1 calc R . . H84B H 0.0616 0.3282 -0.0260 0.108 Uiso 1 1 calc R . . H84C H 0.1492 0.3090 0.0223 0.108 Uiso 1 1 calc R . . O19 O 0.2299(5) 0.18706(19) 0.9104(3) 0.0710(19) Uani 1 1 d . . . C85 C 0.3459(8) 0.1608(3) 0.8340(5) 0.087(4) Uani 1 1 d . . . H85A H 0.4015 0.1757 0.8552 0.131 Uiso 1 1 calc R . . H85B H 0.3112 0.1768 0.7973 0.131 Uiso 1 1 calc R . . H85C H 0.3684 0.1363 0.8135 0.131 Uiso 1 1 calc R . . C86 C 0.2766(9) 0.1506(3) 0.8915(5) 0.085(3) Uani 1 1 d . . . H86A H 0.2275 0.1311 0.8732 0.102 Uiso 1 1 calc R . . H86B H 0.3137 0.1391 0.9331 0.102 Uiso 1 1 calc R . . C87 C 0.1688(8) 0.1799(3) 0.9664(5) 0.081(3) Uani 1 1 d . . . H87A H 0.2068 0.1683 1.0076 0.097 Uiso 1 1 calc R . . H87B H 0.1159 0.1614 0.9509 0.097 Uiso 1 1 calc R . . C88 C 0.1277(7) 0.2200(4) 0.9848(5) 0.084(3) Uani 1 1 d . . . H88A H 0.0928 0.2315 0.9430 0.127 Uiso 1 1 calc R . . H88B H 0.1808 0.2376 1.0017 0.127 Uiso 1 1 calc R . . H88C H 0.0834 0.2167 1.0215 0.127 Uiso 1 1 calc R . . O20 O 0.8955(5) 0.0882(3) 0.0244(4) 0.089(2) Uani 1 1 d . . . C89 C 0.9081(7) 0.1578(4) 0.0232(6) 0.088(4) Uani 1 1 d . . . H89A H 0.8591 0.1600 0.0569 0.133 Uiso 1 1 calc R . . H89B H 0.9047 0.1810 -0.0075 0.133 Uiso 1 1 calc R . . H89C H 0.9724 0.1563 0.0486 0.133 Uiso 1 1 calc R . . C90 C 0.8897(8) 0.1211(4) -0.0202(6) 0.093(4) Uani 1 1 d . . . H90A H 0.8248 0.1224 -0.0459 0.112 Uiso 1 1 calc R . . H90B H 0.9383 0.1188 -0.0548 0.112 Uiso 1 1 calc R . . C91 C 0.8819(9) 0.0526(4) -0.0150(6) 0.095(4) Uani 1 1 d . . . H91A H 0.9302 0.0508 -0.0500 0.114 Uiso 1 1 calc R . . H91B H 0.8165 0.0521 -0.0401 0.114 Uiso 1 1 calc R . . C92 C 0.8942(8) 0.0181(4) 0.0366(6) 0.102(4) Uani 1 1 d . . . H92A H 0.9616 0.0168 0.0564 0.153 Uiso 1 1 calc R . . H92B H 0.8768 -0.0066 0.0120 0.153 Uiso 1 1 calc R . . H92C H 0.8520 0.0221 0.0744 0.153 Uiso 1 1 calc R . . O21 O 0.7328(5) 0.30819(19) 0.1599(3) 0.076(2) Uani 1 1 d . . . H21A H 0.7890 0.3152 0.1415 0.114 Uiso 1 1 d R . . H21B H 0.7068 0.3326 0.1660 0.114 Uiso 1 1 d R . . O22 O 0.8282(5) 0.0996(3) 0.6716(4) 0.106(3) Uani 1 1 d . . . H22A H 0.8664 0.1009 0.7119 0.160 Uiso 1 1 d R . . H22B H 0.7740 0.0883 0.6865 0.160 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0277(5) 0.0379(6) 0.0357(6) 0.0000(5) 0.0058(4) 0.0013(4) Cu2 0.0283(5) 0.0471(6) 0.0362(6) -0.0007(5) 0.0059(4) -0.0003(5) N1 0.034(4) 0.031(4) 0.043(4) 0.002(4) 0.017(3) 0.002(3) N2 0.027(4) 0.038(4) 0.031(4) 0.006(4) 0.003(3) -0.001(3) N3 0.044(4) 0.026(4) 0.044(4) 0.006(4) 0.002(3) -0.005(3) N4 0.024(3) 0.024(4) 0.048(4) -0.001(4) 0.005(3) -0.003(3) N5 0.026(4) 0.036(4) 0.033(4) 0.002(4) 0.005(3) 0.005(3) N6 0.031(4) 0.043(5) 0.042(4) 0.009(4) 0.006(3) 0.003(3) N7 0.027(4) 0.063(5) 0.037(4) 0.007(4) 0.004(3) -0.001(4) N8 0.034(4) 0.061(5) 0.030(4) -0.001(4) 0.005(3) 0.004(4) N9 0.030(4) 0.056(5) 0.034(4) -0.002(4) 0.006(3) 0.001(4) N10 0.035(4) 0.036(4) 0.036(4) -0.001(3) 0.002(3) 0.000(3) N11 0.023(3) 0.034(4) 0.029(4) 0.004(3) 0.003(3) 0.001(3) N12 0.025(3) 0.029(4) 0.040(4) -0.001(3) 0.002(3) 0.000(3) C1 0.032(5) 0.038(5) 0.053(6) 0.003(5) 0.011(4) 0.012(4) C2 0.028(5) 0.045(6) 0.039(5) -0.010(5) 0.005(4) 0.006(4) C3 0.032(5) 0.055(6) 0.041(6) -0.001(5) 0.001(4) 0.006(4) C4 0.045(6) 0.056(7) 0.062(7) -0.023(6) 0.011(5) 0.005(5) C5 0.045(5) 0.057(7) 0.046(6) -0.012(5) 0.011(5) -0.002(5) C6 0.036(5) 0.051(6) 0.040(6) -0.001(5) 0.002(4) -0.001(4) C7 0.026(4) 0.044(5) 0.038(5) -0.001(5) 0.008(4) 0.002(4) C8 0.025(4) 0.047(6) 0.033(5) 0.005(4) 0.004(4) 0.004(4) C9 0.024(4) 0.048(6) 0.027(5) 0.001(4) 0.001(4) 0.004(4) C10 0.027(4) 0.041(5) 0.040(5) 0.005(5) 0.014(4) 0.003(4) C11 0.025(4) 0.046(6) 0.047(6) 0.006(5) 0.010(4) 0.002(4) C12 0.039(5) 0.054(6) 0.049(6) 0.007(5) 0.021(5) 0.004(4) C13 0.030(5) 0.058(6) 0.056(6) 0.021(5) 0.018(4) 0.006(4) C14 0.045(5) 0.038(6) 0.070(7) 0.005(6) 0.014(5) 0.003(4) C15 0.045(5) 0.043(6) 0.062(7) 0.017(5) 0.009(5) -0.005(4) C16 0.043(5) 0.046(6) 0.045(6) 0.010(5) 0.014(4) -0.010(4) C17 0.043(5) 0.040(6) 0.049(6) -0.008(5) 0.005(4) -0.014(4) C18 0.024(4) 0.037(5) 0.038(5) -0.001(4) 0.007(4) 0.001(4) C19 0.027(4) 0.039(5) 0.035(5) 0.004(5) 0.004(4) -0.006(4) C20 0.029(5) 0.041(6) 0.051(6) -0.014(5) 0.011(4) 0.003(4) C21 0.024(4) 0.037(5) 0.045(6) 0.007(5) 0.002(4) 0.003(4) C22 0.042(5) 0.043(6) 0.052(6) 0.002(5) 0.004(5) 0.001(4) C23 0.043(5) 0.046(6) 0.053(6) 0.017(5) 0.004(5) 0.005(4) C24 0.048(6) 0.059(7) 0.037(5) 0.002(5) 0.005(4) 0.008(5) C25 0.041(5) 0.054(6) 0.036(6) 0.006(5) 0.004(4) -0.002(4) C26 0.014(4) 0.049(6) 0.050(6) 0.003(5) 0.015(4) -0.003(4) C27 0.029(5) 0.039(5) 0.040(5) -0.001(4) 0.009(4) -0.001(4) C28 0.029(5) 0.049(6) 0.038(5) 0.002(5) 0.004(4) -0.008(4) C29 0.025(4) 0.041(5) 0.045(6) 0.003(5) 0.012(4) 0.001(4) C30 0.017(4) 0.043(5) 0.054(6) -0.010(5) 0.014(4) -0.002(4) C31 0.026(5) 0.055(6) 0.050(6) -0.013(5) 0.000(4) 0.001(4) C32 0.031(5) 0.060(7) 0.068(7) -0.022(6) 0.009(5) 0.000(5) C33 0.045(6) 0.047(6) 0.087(8) -0.027(6) 0.019(6) 0.001(5) C34 0.043(5) 0.031(5) 0.083(8) -0.003(5) 0.018(5) -0.001(4) C35 0.032(5) 0.040(6) 0.064(7) 0.002(5) 0.017(5) -0.002(4) C36 0.029(5) 0.044(6) 0.057(7) -0.007(5) 0.010(4) -0.005(4) C37 0.027(4) 0.045(6) 0.030(5) -0.005(4) 0.013(4) 0.000(4) C38 0.019(4) 0.047(6) 0.037(5) -0.001(5) 0.010(4) 0.000(4) C39 0.044(6) 0.055(6) 0.040(5) 0.006(5) 0.008(4) 0.000(5) C40 0.045(6) 0.066(7) 0.028(5) 0.003(5) 0.005(4) 0.004(5) C41 0.053(6) 0.067(7) 0.053(6) 0.004(5) 0.003(5) 0.007(5) C42 0.074(8) 0.073(7) 0.045(6) 0.005(5) 0.005(5) 0.014(6) C43 0.046(6) 0.087(8) 0.056(7) -0.009(6) 0.013(5) 0.019(6) C44 0.037(5) 0.087(8) 0.038(5) -0.002(5) 0.007(4) 0.010(5) C45 0.045(6) 0.060(6) 0.029(5) -0.003(4) 0.000(4) 0.013(5) C46 0.027(5) 0.069(7) 0.025(5) -0.001(4) 0.007(4) 0.003(4) C47 0.029(5) 0.082(7) 0.028(5) -0.011(5) 0.001(4) 0.011(5) C48 0.028(5) 0.064(6) 0.034(5) 0.001(4) 0.012(4) -0.003(4) C49 0.035(5) 0.071(7) 0.034(5) 0.006(5) -0.001(4) 0.004(5) C50 0.040(6) 0.074(7) 0.073(7) 0.008(6) 0.026(5) -0.012(5) C51 0.034(6) 0.105(9) 0.060(7) 0.002(6) 0.016(5) -0.006(6) C52 0.036(6) 0.081(8) 0.065(7) -0.001(6) 0.016(5) -0.015(5) C53 0.046(6) 0.067(7) 0.059(6) -0.001(5) 0.001(5) -0.004(5) C54 0.028(5) 0.063(6) 0.041(5) 0.008(5) 0.007(4) -0.008(4) C55 0.032(5) 0.048(6) 0.044(5) -0.001(4) -0.006(4) 0.001(4) C56 0.036(5) 0.064(7) 0.031(5) -0.001(4) -0.002(4) 0.010(5) C57 0.034(5) 0.068(7) 0.030(5) -0.004(5) -0.007(4) 0.009(5) C58 0.048(5) 0.041(6) 0.031(5) -0.006(4) -0.005(4) 0.010(4) C59 0.028(5) 0.045(5) 0.038(5) 0.001(4) 0.004(4) -0.001(4) C60 0.053(6) 0.038(5) 0.042(5) -0.002(4) 0.004(5) 0.005(4) C61 0.044(6) 0.044(6) 0.065(6) 0.006(5) 0.006(5) -0.015(4) C62 0.044(5) 0.042(6) 0.060(6) 0.002(5) 0.015(5) -0.004(4) C63 0.041(5) 0.038(5) 0.050(6) -0.001(4) 0.013(4) -0.003(4) C64 0.038(5) 0.035(5) 0.028(5) -0.001(4) 0.007(4) 0.002(4) C65 0.029(5) 0.041(5) 0.021(4) 0.005(4) -0.003(4) 0.000(4) C66 0.025(4) 0.050(6) 0.027(5) -0.002(4) 0.004(4) 0.001(4) C67 0.040(5) 0.036(5) 0.030(5) 0.004(4) 0.007(4) 0.001(4) C68 0.029(5) 0.041(5) 0.033(5) 0.000(4) 0.008(4) 0.000(4) C69 0.043(5) 0.035(5) 0.060(6) 0.004(4) 0.014(5) 0.002(4) C70 0.033(5) 0.054(6) 0.071(7) 0.002(5) 0.023(5) 0.009(4) C71 0.062(7) 0.037(5) 0.061(6) -0.007(5) 0.014(5) 0.005(5) C72 0.042(5) 0.041(5) 0.052(6) 0.001(4) 0.023(4) 0.002(4) C73 0.033(5) 0.035(5) 0.040(5) 0.004(4) 0.005(4) 0.006(4) C74 0.040(5) 0.032(5) 0.039(5) -0.001(4) 0.009(4) -0.012(4) C75 0.032(5) 0.045(5) 0.022(4) -0.001(4) 0.005(4) 0.004(4) C76 0.020(4) 0.036(5) 0.029(4) 0.001(4) 0.005(4) 0.003(4) Cl1 0.0393(12) 0.0402(13) 0.0427(14) -0.0017(10) 0.0024(10) -0.0012(10) O1 0.038(3) 0.051(4) 0.039(3) -0.001(3) 0.002(3) -0.009(3) O2 0.097(5) 0.040(4) 0.046(4) 0.001(3) 0.001(3) 0.006(3) O3 0.076(4) 0.051(4) 0.046(4) -0.006(3) -0.014(3) -0.002(3) O4 0.041(4) 0.088(5) 0.095(5) -0.009(4) 0.022(4) -0.005(3) Cl2 0.0357(12) 0.0441(13) 0.0423(14) 0.0003(11) 0.0059(10) -0.0001(10) O5 0.036(3) 0.058(4) 0.093(5) 0.014(3) 0.023(3) 0.001(3) O6 0.079(5) 0.047(4) 0.054(4) -0.009(3) 0.005(3) 0.001(3) O7 0.033(3) 0.058(4) 0.048(4) 0.002(3) -0.003(3) 0.011(3) O8 0.065(4) 0.055(4) 0.039(4) -0.002(3) -0.013(3) -0.001(3) Cl3 0.106(2) 0.0693(19) 0.0538(18) -0.0015(14) 0.0134(17) 0.0286(17) O9 0.174(10) 0.208(12) 0.103(7) -0.047(7) -0.074(7) 0.090(8) O10 0.162(9) 0.144(9) 0.185(11) -0.056(8) -0.017(8) 0.095(8) O11 0.43(2) 0.133(10) 0.094(8) -0.002(7) 0.056(10) -0.099(12) O12 0.148(8) 0.174(9) 0.081(6) -0.046(6) 0.044(6) -0.024(7) Cl4 0.0585(16) 0.0575(17) 0.0753(19) -0.0151(14) 0.0163(15) -0.0025(14) O13 0.075(6) 0.44(2) 0.170(11) -0.201(13) 0.000(7) 0.022(9) O14 0.252(13) 0.143(9) 0.159(10) 0.053(8) 0.084(9) 0.141(10) O15 0.133(8) 0.091(7) 0.272(14) -0.010(7) 0.124(9) -0.027(6) O16 0.147(7) 0.061(5) 0.137(7) 0.000(5) 0.080(6) 0.006(5) O17 0.059(4) 0.094(6) 0.075(5) 0.006(5) 0.008(4) 0.006(4) C77 0.085(9) 0.136(13) 0.144(13) -0.030(11) 0.030(9) -0.008(8) C78 0.069(8) 0.095(10) 0.147(14) 0.044(10) 0.013(8) 0.010(7) C79 0.061(7) 0.125(11) 0.065(8) 0.005(8) -0.005(6) 0.005(7) C80 0.060(7) 0.116(10) 0.077(8) -0.014(7) 0.000(6) 0.014(7) O18 0.075(5) 0.091(6) 0.059(5) -0.004(5) 0.014(4) -0.014(4) C81 0.068(7) 0.116(10) 0.079(8) -0.006(8) 0.015(6) -0.001(7) C82 0.080(8) 0.097(9) 0.068(8) -0.015(8) 0.028(6) 0.000(7) C83 0.067(7) 0.104(9) 0.062(7) 0.006(8) 0.015(6) -0.014(6) C84 0.049(6) 0.104(9) 0.064(7) -0.001(7) 0.013(5) -0.013(6) O19 0.063(4) 0.075(5) 0.074(5) 0.001(4) -0.002(4) 0.003(4) C85 0.078(8) 0.111(10) 0.073(8) -0.008(7) 0.015(7) 0.015(7) C86 0.124(10) 0.064(7) 0.065(7) -0.002(6) -0.011(7) 0.020(7) C87 0.066(7) 0.112(10) 0.067(8) 0.020(7) 0.017(6) 0.006(7) C88 0.075(8) 0.128(11) 0.050(7) -0.018(7) 0.005(6) 0.012(7) O20 0.080(5) 0.115(7) 0.072(5) 0.007(5) 0.011(4) -0.003(5) C89 0.067(7) 0.132(11) 0.066(8) -0.014(8) 0.000(6) -0.021(7) C90 0.065(8) 0.135(12) 0.080(9) 0.010(9) 0.019(7) -0.016(7) C91 0.093(9) 0.111(11) 0.082(9) -0.021(9) 0.006(7) 0.008(8) C92 0.079(9) 0.138(12) 0.086(9) 0.000(9) -0.005(7) 0.027(8) O21 0.089(5) 0.066(4) 0.076(5) 0.000(4) 0.025(4) 0.004(4) O22 0.088(6) 0.160(8) 0.073(5) 0.009(5) 0.020(5) 0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.000(6) . ? Cu1 N4 2.013(6) . ? Cu1 N11 2.094(5) . ? Cu1 N8 2.154(6) . ? Cu1 N7 2.355(7) . ? Cu1 N10 2.422(6) . ? Cu1 Cu2 2.9072(13) . ? Cu2 N12 1.992(6) . ? Cu2 N9 2.005(6) . ? Cu2 N2 2.066(6) . ? Cu2 N5 2.122(6) . ? Cu2 N6 2.328(7) . ? Cu2 N3 2.415(6) . ? N1 C1 1.305(9) . ? N1 C18 1.402(9) . ? N2 C18 1.333(9) . ? N2 C19 1.351(9) . ? N3 C17 1.309(10) . ? N3 C19 1.372(9) . ? N4 C20 1.298(9) . ? N4 C37 1.392(9) . ? N5 C37 1.323(9) . ? N5 C38 1.331(9) . ? N6 C36 1.315(10) . ? N6 C38 1.378(9) . ? N7 C39 1.275(10) . ? N7 C56 1.379(10) . ? N8 C56 1.333(10) . ? N8 C57 1.364(10) . ? N9 C55 1.296(9) . ? N9 C57 1.360(10) . ? N10 C58 1.311(9) . ? N10 C75 1.403(9) . ? N11 C75 1.339(9) . ? N11 C76 1.347(8) . ? N12 C74 1.307(9) . ? N12 C76 1.385(9) . ? C1 C2 1.427(11) . ? C2 C7 1.384(11) . ? C2 C3 1.401(11) . ? C3 C4 1.374(11) . ? C4 C5 1.407(12) . ? C5 C6 1.355(11) . ? C6 C7 1.423(11) . ? C7 C8 1.449(11) . ? C8 C9 1.398(10) . ? C8 C18 1.428(10) . ? C9 C10 1.378(10) . ? C10 C19 1.392(10) . ? C10 C11 1.474(11) . ? C11 C12 1.386(11) . ? C11 C16 1.413(11) . ? C12 C13 1.380(11) . ? C13 C14 1.395(11) . ? C14 C15 1.360(11) . ? C15 C16 1.403(11) . ? C16 C17 1.430(11) . ? C20 C21 1.427(11) . ? C21 C22 1.406(11) . ? C21 C26 1.407(11) . ? C22 C23 1.363(11) . ? C23 C24 1.385(11) . ? C24 C25 1.361(11) . ? C25 C26 1.394(11) . ? C26 C27 1.457(11) . ? C27 C37 1.407(11) . ? C27 C28 1.413(11) . ? C28 C29 1.389(11) . ? C29 C38 1.421(11) . ? C29 C30 1.467(11) . ? C30 C31 1.380(11) . ? C30 C35 1.435(11) . ? C31 C32 1.375(11) . ? C32 C33 1.378(12) . ? C33 C34 1.350(12) . ? C34 C35 1.429(12) . ? C35 C36 1.420(11) . ? C39 C40 1.443(11) . ? C40 C41 1.376(12) . ? C40 C45 1.395(11) . ? C41 C42 1.393(12) . ? C42 C43 1.392(13) . ? C43 C44 1.383(12) . ? C44 C45 1.422(11) . ? C45 C46 1.445(11) . ? C46 C47 1.403(11) . ? C46 C56 1.425(11) . ? C47 C48 1.401(11) . ? C48 C49 1.429(11) . ? C48 C57 1.430(11) . ? C49 C50 1.402(11) . ? C49 C54 1.406(11) . ? C50 C51 1.366(13) . ? C51 C52 1.374(13) . ? C52 C53 1.398(11) . ? C53 C54 1.412(11) . ? C54 C55 1.420(10) . ? C58 C59 1.437(10) . ? C59 C60 1.417(11) . ? C59 C64 1.422(10) . ? C60 C61 1.340(11) . ? C61 C62 1.405(11) . ? C62 C63 1.353(10) . ? C63 C64 1.397(10) . ? C64 C65 1.465(10) . ? C65 C66 1.401(10) . ? C65 C75 1.405(10) . ? C66 C67 1.394(10) . ? C67 C76 1.409(10) . ? C67 C68 1.454(10) . ? C68 C69 1.371(10) . ? C68 C73 1.410(10) . ? C69 C70 1.375(10) . ? C70 C71 1.427(11) . ? C71 C72 1.351(11) . ? C72 C73 1.398(10) . ? C73 C74 1.414(10) . ? Cl1 O1 1.413(5) . ? Cl1 O3 1.419(6) . ? Cl1 O2 1.421(6) . ? Cl1 O4 1.424(6) . ? Cl2 O8 1.430(6) . ? Cl2 O7 1.431(5) . ? Cl2 O6 1.440(6) . ? Cl2 O5 1.449(5) . ? Cl3 O10 1.342(8) . ? Cl3 O12 1.399(8) . ? Cl3 O9 1.401(9) . ? Cl3 O11 1.425(11) . ? Cl4 O14 1.325(8) . ? Cl4 O15 1.332(8) . ? Cl4 O13 1.340(10) . ? Cl4 O16 1.409(7) . ? O17 C78 1.442(13) . ? O17 C79 1.449(12) . ? C77 C78 1.494(16) . ? C79 C80 1.497(14) . ? O18 C83 1.404(11) . ? O18 C82 1.412(12) . ? C81 C82 1.512(14) . ? C83 C84 1.506(13) . ? O19 C87 1.445(11) . ? O19 C86 1.454(11) . ? C85 C86 1.564(13) . ? C87 C88 1.527(14) . ? O20 C90 1.402(13) . ? O20 C91 1.424(13) . ? C89 C90 1.505(14) . ? C91 C92 1.529(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N4 179.5(3) . . ? N1 Cu1 N11 91.0(2) . . ? N4 Cu1 N11 89.4(2) . . ? N1 Cu1 N8 87.3(2) . . ? N4 Cu1 N8 92.7(2) . . ? N11 Cu1 N8 144.4(3) . . ? N1 Cu1 N7 89.4(2) . . ? N4 Cu1 N7 90.2(2) . . ? N11 Cu1 N7 155.7(2) . . ? N8 Cu1 N7 60.0(2) . . ? N1 Cu1 N10 90.7(2) . . ? N4 Cu1 N10 89.1(2) . . ? N11 Cu1 N10 59.7(2) . . ? N8 Cu1 N10 155.8(2) . . ? N7 Cu1 N10 96.0(2) . . ? N1 Cu1 Cu2 88.50(19) . . ? N4 Cu1 Cu2 92.01(18) . . ? N11 Cu1 Cu2 74.05(16) . . ? N8 Cu1 Cu2 70.3(2) . . ? N7 Cu1 Cu2 130.26(17) . . ? N10 Cu1 Cu2 133.74(15) . . ? N12 Cu2 N9 177.0(3) . . ? N12 Cu2 N2 89.7(2) . . ? N9 Cu2 N2 90.2(2) . . ? N12 Cu2 N5 90.1(2) . . ? N9 Cu2 N5 91.6(2) . . ? N2 Cu2 N5 146.3(3) . . ? N12 Cu2 N6 89.9(2) . . ? N9 Cu2 N6 88.8(2) . . ? N2 Cu2 N6 153.2(2) . . ? N5 Cu2 N6 60.5(2) . . ? N12 Cu2 N3 89.2(2) . . ? N9 Cu2 N3 88.2(2) . . ? N2 Cu2 N3 59.8(2) . . ? N5 Cu2 N3 153.9(2) . . ? N6 Cu2 N3 93.3(2) . . ? N12 Cu2 Cu1 89.24(18) . . ? N9 Cu2 Cu1 93.7(2) . . ? N2 Cu2 Cu1 74.99(18) . . ? N5 Cu2 Cu1 71.29(18) . . ? N6 Cu2 Cu1 131.82(17) . . ? N3 Cu2 Cu1 134.80(16) . . ? C1 N1 C18 116.9(7) . . ? C1 N1 Cu1 120.6(6) . . ? C18 N1 Cu1 122.5(5) . . ? C18 N2 C19 119.8(7) . . ? C18 N2 Cu2 138.0(5) . . ? C19 N2 Cu2 102.1(5) . . ? C17 N3 C19 116.9(7) . . ? C17 N3 Cu2 157.0(6) . . ? C19 N3 Cu2 86.1(5) . . ? C20 N4 C37 117.8(7) . . ? C20 N4 Cu1 123.0(6) . . ? C37 N4 Cu1 119.2(5) . . ? C37 N5 C38 119.3(7) . . ? C37 N5 Cu2 141.9(6) . . ? C38 N5 Cu2 98.8(5) . . ? C36 N6 C38 118.4(7) . . ? C36 N6 Cu2 153.2(6) . . ? C38 N6 Cu2 88.4(5) . . ? C39 N7 C56 117.9(7) . . ? C39 N7 Cu1 153.2(6) . . ? C56 N7 Cu1 88.5(5) . . ? C56 N8 C57 120.3(7) . . ? C56 N8 Cu1 98.7(6) . . ? C57 N8 Cu1 140.9(6) . . ? C55 N9 C57 118.2(7) . . ? C55 N9 Cu2 122.7(6) . . ? C57 N9 Cu2 119.1(6) . . ? C58 N10 C75 115.8(6) . . ? C58 N10 Cu1 157.7(5) . . ? C75 N10 Cu1 86.3(4) . . ? C75 N11 C76 118.9(6) . . ? C75 N11 Cu1 102.5(4) . . ? C76 N11 Cu1 138.3(5) . . ? C74 N12 C76 116.6(6) . . ? C74 N12 Cu2 120.0(5) . . ? C76 N12 Cu2 123.2(5) . . ? N1 C1 C2 125.6(8) . . ? C7 C2 C3 121.5(8) . . ? C7 C2 C1 118.8(8) . . ? C3 C2 C1 119.7(8) . . ? C4 C3 C2 117.9(8) . . ? C3 C4 C5 121.5(8) . . ? C6 C5 C4 120.3(9) . . ? C5 C6 C7 119.6(8) . . ? C2 C7 C6 119.1(8) . . ? C2 C7 C8 118.3(7) . . ? C6 C7 C8 122.5(8) . . ? C9 C8 C18 117.2(7) . . ? C9 C8 C7 125.0(7) . . ? C18 C8 C7 117.8(7) . . ? C10 C9 C8 121.0(7) . . ? C9 C10 C19 118.0(7) . . ? C9 C10 C11 124.9(8) . . ? C19 C10 C11 117.0(8) . . ? C12 C11 C16 118.8(8) . . ? C12 C11 C10 124.8(8) . . ? C16 C11 C10 116.4(8) . . ? C13 C12 C11 120.6(9) . . ? C12 C13 C14 120.5(9) . . ? C15 C14 C13 119.9(8) . . ? C14 C15 C16 120.4(9) . . ? C15 C16 C11 119.8(8) . . ? C15 C16 C17 120.6(9) . . ? C11 C16 C17 119.6(8) . . ? N3 C17 C16 124.2(8) . . ? N2 C18 N1 116.0(7) . . ? N2 C18 C8 121.5(7) . . ? N1 C18 C8 122.5(7) . . ? N2 C19 N3 111.8(7) . . ? N2 C19 C10 122.5(7) . . ? N3 C19 C10 125.7(7) . . ? N4 C20 C21 125.3(7) . . ? C22 C21 C26 119.6(8) . . ? C22 C21 C20 120.9(8) . . ? C26 C21 C20 119.5(7) . . ? C23 C22 C21 119.4(8) . . ? C22 C23 C24 120.3(8) . . ? C25 C24 C23 122.0(9) . . ? C24 C25 C26 118.9(8) . . ? C25 C26 C21 119.8(8) . . ? C25 C26 C27 124.9(8) . . ? C21 C26 C27 115.3(8) . . ? C37 C27 C28 117.6(7) . . ? C37 C27 C26 120.4(7) . . ? C28 C27 C26 121.9(8) . . ? C29 C28 C27 119.9(8) . . ? C28 C29 C38 117.0(7) . . ? C28 C29 C30 125.7(8) . . ? C38 C29 C30 117.3(8) . . ? C31 C30 C35 119.7(8) . . ? C31 C30 C29 124.4(8) . . ? C35 C30 C29 115.9(8) . . ? C32 C31 C30 119.7(9) . . ? C31 C32 C33 121.4(9) . . ? C34 C33 C32 121.3(9) . . ? C33 C34 C35 119.7(9) . . ? C36 C35 C34 120.9(9) . . ? C36 C35 C30 120.9(8) . . ? C34 C35 C30 118.2(9) . . ? N6 C36 C35 123.1(8) . . ? N5 C37 N4 115.6(7) . . ? N5 C37 C27 122.9(7) . . ? N4 C37 C27 121.6(7) . . ? N5 C38 N6 112.3(7) . . ? N5 C38 C29 123.2(7) . . ? N6 C38 C29 124.4(8) . . ? N7 C39 C40 124.9(8) . . ? C41 C40 C45 120.7(8) . . ? C41 C40 C39 121.0(9) . . ? C45 C40 C39 118.3(8) . . ? C40 C41 C42 121.3(9) . . ? C43 C42 C41 117.3(9) . . ? C44 C43 C42 123.7(9) . . ? C43 C44 C45 117.3(9) . . ? C40 C45 C44 119.6(8) . . ? C40 C45 C46 118.5(8) . . ? C44 C45 C46 121.8(8) . . ? C47 C46 C56 116.0(8) . . ? C47 C46 C45 127.5(7) . . ? C56 C46 C45 116.6(8) . . ? C48 C47 C46 121.8(7) . . ? C47 C48 C49 124.7(7) . . ? C47 C48 C57 117.8(8) . . ? C49 C48 C57 117.4(8) . . ? C50 C49 C54 117.9(8) . . ? C50 C49 C48 124.5(8) . . ? C54 C49 C48 117.6(7) . . ? C51 C50 C49 119.5(9) . . ? C50 C51 C52 124.2(9) . . ? C51 C52 C53 117.7(9) . . ? C52 C53 C54 119.4(9) . . ? C49 C54 C53 121.3(7) . . ? C49 C54 C55 119.1(8) . . ? C53 C54 C55 119.5(8) . . ? N9 C55 C54 124.3(8) . . ? N8 C56 N7 112.8(7) . . ? N8 C56 C46 123.4(8) . . ? N7 C56 C46 123.7(8) . . ? N9 C57 N8 116.0(7) . . ? N9 C57 C48 123.3(8) . . ? N8 C57 C48 120.6(8) . . ? N10 C58 C59 125.2(7) . . ? C60 C59 C64 119.1(7) . . ? C60 C59 C58 120.9(7) . . ? C64 C59 C58 119.9(7) . . ? C61 C60 C59 120.7(8) . . ? C60 C61 C62 119.2(8) . . ? C63 C62 C61 122.6(8) . . ? C62 C63 C64 119.3(7) . . ? C63 C64 C59 119.0(7) . . ? C63 C64 C65 125.3(7) . . ? C59 C64 C65 115.7(6) . . ? C66 C65 C75 117.1(7) . . ? C66 C65 C64 124.4(7) . . ? C75 C65 C64 118.5(7) . . ? C67 C66 C65 119.7(7) . . ? C66 C67 C76 118.8(7) . . ? C66 C67 C68 122.8(7) . . ? C76 C67 C68 118.3(7) . . ? C69 C68 C73 118.5(7) . . ? C69 C68 C67 124.2(7) . . ? C73 C68 C67 117.3(6) . . ? C68 C69 C70 121.4(8) . . ? C69 C70 C71 119.7(7) . . ? C72 C71 C70 119.6(8) . . ? C71 C72 C73 120.2(8) . . ? C72 C73 C68 120.6(7) . . ? C72 C73 C74 121.2(7) . . ? C68 C73 C74 118.2(7) . . ? N12 C74 C73 126.4(7) . . ? N11 C75 N10 111.4(6) . . ? N11 C75 C65 123.7(7) . . ? N10 C75 C65 124.8(7) . . ? N11 C76 N12 115.1(6) . . ? N11 C76 C67 121.7(6) . . ? N12 C76 C67 123.2(6) . . ? O1 Cl1 O3 109.8(3) . . ? O1 Cl1 O2 109.3(4) . . ? O3 Cl1 O2 109.7(4) . . ? O1 Cl1 O4 108.9(3) . . ? O3 Cl1 O4 110.5(4) . . ? O2 Cl1 O4 108.7(4) . . ? O8 Cl2 O7 110.2(3) . . ? O8 Cl2 O6 109.4(4) . . ? O7 Cl2 O6 110.0(4) . . ? O8 Cl2 O5 109.5(4) . . ? O7 Cl2 O5 108.5(3) . . ? O6 Cl2 O5 109.2(4) . . ? O10 Cl3 O12 111.5(7) . . ? O10 Cl3 O9 111.0(6) . . ? O12 Cl3 O9 111.8(7) . . ? O10 Cl3 O11 110.7(9) . . ? O12 Cl3 O11 104.1(6) . . ? O9 Cl3 O11 107.5(8) . . ? O14 Cl4 O15 114.6(8) . . ? O14 Cl4 O13 107.4(8) . . ? O15 Cl4 O13 109.2(9) . . ? O14 Cl4 O16 111.3(6) . . ? O15 Cl4 O16 105.9(5) . . ? O13 Cl4 O16 108.2(6) . . ? C78 O17 C79 113.3(9) . . ? O17 C78 C77 110.1(11) . . ? O17 C79 C80 108.2(9) . . ? C83 O18 C82 110.0(8) . . ? O18 C82 C81 107.9(9) . . ? O18 C83 C84 107.9(9) . . ? C87 O19 C86 110.2(8) . . ? O19 C86 C85 107.6(8) . . ? O19 C87 C88 106.0(8) . . ? C90 O20 C91 110.6(9) . . ? O20 C90 C89 108.8(10) . . ? O20 C91 C92 107.6(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.708 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.131 data_ic14185 _database_code_depnum_ccdc_archive 'CCDC 875006' #TrackingRef '- ic14185-re-revised Ni.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82.27 H63.10 Cl4 N14.42 Ni2 O20.50' _chemical_formula_weight 1840.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.4297(2) _cell_length_b 35.6133(5) _cell_length_c 19.3597(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.9636(7) _cell_angle_gamma 90.00 _cell_volume 9119.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37821 _cell_measurement_theta_min 1.21 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3783 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.749 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37821 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15949 _reflns_number_gt 9153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The distance restrains are applied for 2 dmf molecules. One perchlorate (CL4, O13, O14, O15 and O16) is restrained using SADI in the refinement. There are 3 short distances contacts [ O23 (dmf molecule)-O24 (water) = 1.496\A, O25-O26 = 2.175\A, O27-O28 = 2.504\A]. The disorder treatments are applied for those 3 short contacts' molecules and the occupancy factors are alos refined. When the crystal is leaved from the solution, it is easy to decompose so the Uiso values are larger. The water molecule O29 is moved away from inversion center and treated with 50% disorder. The Uiso value is reduced from 0.39(4) to 0.23(2). ; _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^)+(0.1019P)^2^+35.5343P] 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 15949 _refine_ls_number_parameters 1047 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.1688 _refine_ls_R_factor_gt 0.1084 _refine_ls_wR_factor_ref 0.3155 _refine_ls_wR_factor_gt 0.2906 _refine_ls_goodness_of_fit_ref 1.248 _refine_ls_restrained_S_all 1.272 _refine_ls_shift/su_max 0.014 _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 Ni1 Ni 0.19945(8) 0.33199(3) 0.25247(5) 0.0412(3) Uani 1 1 d . . . Ni2 Ni 0.21833(8) 0.42570(3) 0.24397(5) 0.0419(3) Uani 1 1 d . . . N1 N 0.1436(5) 0.33295(18) 0.1454(3) 0.0436(16) Uani 1 1 d . . . N2 N 0.1596(5) 0.3974(2) 0.1440(3) 0.0448(16) Uani 1 1 d . . . N3 N 0.1823(5) 0.45933(19) 0.1550(4) 0.0473(17) Uani 1 1 d . . . N4 N 0.2568(5) 0.33636(18) 0.3585(3) 0.0424(16) Uani 1 1 d . . . N5 N 0.2659(5) 0.40063(18) 0.3480(3) 0.0410(16) Uani 1 1 d . . . N6 N 0.2713(5) 0.46184(19) 0.3249(4) 0.0492(17) Uani 1 1 d . . . N7 N 0.3088(5) 0.29266(18) 0.2359(3) 0.0420(16) Uani 1 1 d . . . N8 N 0.3423(5) 0.35410(18) 0.2257(3) 0.0409(16) Uani 1 1 d . . . N9 N 0.3628(5) 0.41774(18) 0.2215(3) 0.0446(16) Uani 1 1 d . . . N10 N 0.0738(5) 0.3024(2) 0.2727(3) 0.0485(17) Uani 1 1 d . . . N11 N 0.0658(5) 0.3645(2) 0.2712(3) 0.0452(16) Uani 1 1 d . . . N12 N 0.0727(5) 0.4295(2) 0.2660(3) 0.0496(18) Uani 1 1 d . . . C1 C 0.1176(6) 0.3013(3) 0.1116(4) 0.050(2) Uani 1 1 d . . . H1 H 0.1232 0.2788 0.1381 0.060 Uiso 1 1 calc R . . C2 C 0.0815(7) 0.2987(3) 0.0378(5) 0.054(2) Uani 1 1 d . . . C3 C 0.0582(7) 0.2634(3) 0.0068(5) 0.063(3) Uani 1 1 d . . . H3 H 0.0665 0.2412 0.0344 0.075 Uiso 1 1 calc R . . C4 C 0.0235(9) 0.2615(4) -0.0642(6) 0.084(4) Uani 1 1 d . . . H4 H 0.0083 0.2377 -0.0858 0.101 Uiso 1 1 calc R . . C5 C 0.0103(9) 0.2937(4) -0.1045(6) 0.082(3) Uani 1 1 d . . . H5 H -0.0152 0.2919 -0.1534 0.098 Uiso 1 1 calc R . . C6 C 0.0334(8) 0.3284(3) -0.0751(5) 0.075(3) Uani 1 1 d . . . H6 H 0.0245 0.3502 -0.1036 0.090 Uiso 1 1 calc R . . C7 C 0.0706(7) 0.3316(3) -0.0023(4) 0.053(2) Uani 1 1 d . . . C8 C 0.0983(6) 0.3671(3) 0.0330(4) 0.051(2) Uani 1 1 d . . . C9 C 0.0934(7) 0.4017(3) -0.0002(5) 0.054(2) Uani 1 1 d . . . H9 H 0.0696 0.4030 -0.0493 0.065 Uiso 1 1 calc R . . C10 C 0.1222(6) 0.4341(3) 0.0366(4) 0.050(2) Uani 1 1 d . . . C11 C 0.1219(6) 0.4718(3) 0.0084(5) 0.055(2) Uani 1 1 d . . . C12 C 0.0944(7) 0.4810(3) -0.0638(5) 0.066(3) Uani 1 1 d . . . H12 H 0.0753 0.4618 -0.0975 0.079 Uiso 1 1 calc R . . C13 C 0.0957(7) 0.5173(4) -0.0841(6) 0.072(3) Uani 1 1 d . . . H13 H 0.0777 0.5230 -0.1326 0.087 Uiso 1 1 calc R . . C14 C 0.1223(7) 0.5466(3) -0.0372(6) 0.074(3) Uani 1 1 d . . . H14 H 0.1207 0.5718 -0.0536 0.089 Uiso 1 1 calc R . . C15 C 0.1512(7) 0.5391(3) 0.0338(6) 0.063(3) Uani 1 1 d . . . H15 H 0.1699 0.5589 0.0663 0.075 Uiso 1 1 calc R . . C16 C 0.1522(6) 0.5018(3) 0.0564(5) 0.055(2) Uani 1 1 d . . . C17 C 0.1809(6) 0.4936(3) 0.1298(5) 0.055(2) Uani 1 1 d . . . H17 H 0.1997 0.5138 0.1615 0.066 Uiso 1 1 calc R . . C18 C 0.1336(6) 0.3657(2) 0.1071(4) 0.045(2) Uani 1 1 d . . . C19 C 0.1534(6) 0.4299(2) 0.1093(4) 0.044(2) Uani 1 1 d . . . C20 C 0.2685(6) 0.3063(2) 0.3985(4) 0.047(2) Uani 1 1 d . . . H20 H 0.2518 0.2826 0.3767 0.056 Uiso 1 1 calc R . . C21 C 0.3046(6) 0.3067(2) 0.4729(4) 0.048(2) Uani 1 1 d . . . C22 C 0.3141(8) 0.2730(3) 0.5117(5) 0.065(3) Uani 1 1 d . . . H22 H 0.2983 0.2497 0.4887 0.078 Uiso 1 1 calc R . . C23 C 0.3463(8) 0.2742(3) 0.5827(6) 0.075(3) Uani 1 1 d . . . H23 H 0.3512 0.2515 0.6089 0.090 Uiso 1 1 calc R . . C24 C 0.3721(9) 0.3080(3) 0.6172(6) 0.077(3) Uani 1 1 d . . . H24 H 0.3952 0.3085 0.6664 0.092 Uiso 1 1 calc R . . C25 C 0.3634(8) 0.3408(3) 0.5787(5) 0.069(3) Uani 1 1 d . . . H25 H 0.3813 0.3638 0.6022 0.083 Uiso 1 1 calc R . . C26 C 0.3292(7) 0.3412(3) 0.5068(5) 0.053(2) Uani 1 1 d . . . C27 C 0.3183(6) 0.3743(2) 0.4640(4) 0.046(2) Uani 1 1 d . . . C28 C 0.3418(7) 0.4106(3) 0.4902(5) 0.056(2) Uani 1 1 d . . . H28 H 0.3677 0.4138 0.5387 0.067 Uiso 1 1 calc R . . C29 C 0.3281(7) 0.4419(2) 0.4470(4) 0.052(2) Uani 1 1 d . . . C30 C 0.3484(8) 0.4806(3) 0.4674(5) 0.061(2) Uani 1 1 d . . . C31 C 0.3882(9) 0.4922(3) 0.5346(5) 0.080(3) Uani 1 1 d . . . H31 H 0.4012 0.4743 0.5715 0.095 Uiso 1 1 calc R . . C32 C 0.4093(10) 0.5299(3) 0.5486(6) 0.085(4) Uani 1 1 d . . . H32 H 0.4369 0.5374 0.5950 0.102 Uiso 1 1 calc R . . C33 C 0.3909(11) 0.5565(3) 0.4964(6) 0.095(4) Uani 1 1 d . . . H33 H 0.4070 0.5821 0.5067 0.114 Uiso 1 1 calc R . . C34 C 0.3490(10) 0.5459(3) 0.4290(6) 0.084(3) Uani 1 1 d . . . H34 H 0.3331 0.5643 0.3932 0.100 Uiso 1 1 calc R . . C35 C 0.3299(8) 0.5074(3) 0.4138(5) 0.064(3) Uani 1 1 d . . . C36 C 0.2897(8) 0.4968(3) 0.3434(5) 0.062(3) Uani 1 1 d . . . H36 H 0.2759 0.5158 0.3087 0.074 Uiso 1 1 calc R . . C37 C 0.2800(6) 0.3707(2) 0.3905(4) 0.0417(19) Uani 1 1 d . . . C38 C 0.2894(6) 0.4343(2) 0.3763(4) 0.047(2) Uani 1 1 d . . . C39 C 0.3326(7) 0.2575(2) 0.2329(4) 0.046(2) Uani 1 1 d . . . H39 H 0.2873 0.2394 0.2459 0.055 Uiso 1 1 calc R . . C40 C 0.4225(6) 0.2443(2) 0.2111(4) 0.046(2) Uani 1 1 d . . . C41 C 0.4402(8) 0.2057(3) 0.2060(5) 0.058(2) Uani 1 1 d . . . H41 H 0.3923 0.1882 0.2177 0.070 Uiso 1 1 calc R . . C42 C 0.5239(8) 0.1932(3) 0.1847(5) 0.069(3) Uani 1 1 d . . . H42 H 0.5359 0.1670 0.1818 0.082 Uiso 1 1 calc R . . C43 C 0.5931(8) 0.2189(3) 0.1670(6) 0.073(3) Uani 1 1 d . . . H43 H 0.6526 0.2099 0.1521 0.088 Uiso 1 1 calc R . . C44 C 0.5779(7) 0.2569(3) 0.1704(5) 0.061(2) Uani 1 1 d . . . H44 H 0.6259 0.2739 0.1576 0.073 Uiso 1 1 calc R . . C45 C 0.4911(6) 0.2703(2) 0.1929(4) 0.048(2) Uani 1 1 d . . . C46 C 0.4682(6) 0.3098(2) 0.1975(4) 0.0427(19) Uani 1 1 d . . . C47 C 0.5271(7) 0.3400(2) 0.1857(5) 0.052(2) Uani 1 1 d . . . H47 H 0.5907 0.3357 0.1720 0.062 Uiso 1 1 calc R . . C48 C 0.4953(6) 0.3767(2) 0.1934(5) 0.050(2) Uani 1 1 d . . . C49 C 0.5546(7) 0.4094(3) 0.1801(6) 0.065(3) Uani 1 1 d . . . C50 C 0.6479(8) 0.4073(3) 0.1595(8) 0.097(4) Uani 1 1 d . . . H50 H 0.6770 0.3834 0.1539 0.117 Uiso 1 1 calc R . . C51 C 0.6990(11) 0.4393(4) 0.1470(10) 0.133(6) Uani 1 1 d . . . H51 H 0.7644 0.4375 0.1349 0.159 Uiso 1 1 calc R . . C52 C 0.6539(11) 0.4752(4) 0.1521(10) 0.138(7) Uani 1 1 d . . . H52 H 0.6863 0.4972 0.1393 0.166 Uiso 1 1 calc R . . C53 C 0.5637(9) 0.4778(3) 0.1755(8) 0.103(5) Uani 1 1 d . . . H53 H 0.5358 0.5017 0.1828 0.124 Uiso 1 1 calc R . . C54 C 0.5125(7) 0.4448(3) 0.1886(6) 0.067(3) Uani 1 1 d . . . C55 C 0.4175(7) 0.4466(2) 0.2106(5) 0.054(2) Uani 1 1 d . . . H55 H 0.3915 0.4708 0.2179 0.064 Uiso 1 1 calc R . . C56 C 0.3754(6) 0.3191(2) 0.2182(4) 0.044(2) Uani 1 1 d . . . C57 C 0.4007(6) 0.3828(2) 0.2134(4) 0.0396(18) Uani 1 1 d . . . C58 C 0.0371(7) 0.2691(3) 0.2787(4) 0.056(2) Uani 1 1 d . . . H58 H 0.0770 0.2478 0.2718 0.067 Uiso 1 1 calc R . . C59 C -0.0628(7) 0.2632(3) 0.2955(5) 0.060(3) Uani 1 1 d . . . C60 C -0.0981(8) 0.2264(3) 0.3025(5) 0.072(3) Uani 1 1 d . . . H60 H -0.0569 0.2053 0.2963 0.086 Uiso 1 1 calc R . . C61 C -0.1948(10) 0.2213(4) 0.3186(6) 0.094(4) Uani 1 1 d . . . H61 H -0.2199 0.1968 0.3246 0.113 Uiso 1 1 calc R . . C62 C -0.2540(10) 0.2530(5) 0.3259(6) 0.096(4) Uani 1 1 d . . . H62 H -0.3204 0.2492 0.3354 0.115 Uiso 1 1 calc R . . C63 C -0.2210(8) 0.2890(4) 0.3199(5) 0.079(3) Uani 1 1 d . . . H63 H -0.2629 0.3097 0.3263 0.094 Uiso 1 1 calc R . . C64 C -0.1224(7) 0.2948(3) 0.3038(5) 0.061(3) Uani 1 1 d . . . C65 C -0.0811(7) 0.3316(3) 0.2970(5) 0.058(2) Uani 1 1 d . . . C66 C -0.1284(7) 0.3657(3) 0.3046(5) 0.063(3) Uani 1 1 d . . . H66 H -0.1944 0.3660 0.3159 0.076 Uiso 1 1 calc R . . C67 C -0.0791(7) 0.3999(3) 0.2958(5) 0.063(3) Uani 1 1 d . . . C68 C -0.1221(8) 0.4364(3) 0.3022(6) 0.072(3) Uani 1 1 d . . . C69 C -0.2186(10) 0.4421(4) 0.3208(8) 0.114(5) Uani 1 1 d . . . H69 H -0.2565 0.4212 0.3322 0.137 Uiso 1 1 calc R . . C70 C -0.2572(13) 0.4772(5) 0.3225(10) 0.145(7) Uani 1 1 d . . . H70 H -0.3226 0.4807 0.3338 0.174 Uiso 1 1 calc R . . C71 C -0.2001(14) 0.5083(5) 0.3075(10) 0.150(7) Uani 1 1 d . . . H71 H -0.2285 0.5327 0.3084 0.179 Uiso 1 1 calc R . . C72 C -0.1038(10) 0.5047(4) 0.2915(7) 0.105(5) Uani 1 1 d . . . H72 H -0.0649 0.5260 0.2831 0.126 Uiso 1 1 calc R . . C73 C -0.0662(8) 0.4679(3) 0.2881(6) 0.074(3) Uani 1 1 d . . . C74 C 0.0318(7) 0.4624(3) 0.2711(5) 0.058(2) Uani 1 1 d . . . H74 H 0.0697 0.4840 0.2630 0.069 Uiso 1 1 calc R . . C75 C 0.0171(6) 0.3332(3) 0.2805(4) 0.046(2) Uani 1 1 d . . . C76 C 0.0199(6) 0.3975(3) 0.2772(4) 0.051(2) Uani 1 1 d . . . Cl1 Cl 0.56845(17) 0.35572(7) 0.39057(13) 0.0594(6) Uani 1 1 d . . . O1 O 0.5083(6) 0.3878(2) 0.3672(4) 0.091(2) Uani 1 1 d . . . O2 O 0.5337(9) 0.3241(2) 0.3524(4) 0.126(4) Uani 1 1 d . . . O3 O 0.5688(7) 0.3492(2) 0.4623(4) 0.103(3) Uani 1 1 d . . . O4 O 0.6670(7) 0.3637(3) 0.3830(7) 0.147(4) Uani 1 1 d . . . Cl2 Cl 0.4138(3) 0.08653(8) 0.26677(17) 0.0847(9) Uani 1 1 d . . . O5 O 0.3675(19) 0.1164(5) 0.2485(15) 0.353(15) Uani 1 1 d . . . O6 O 0.3901(13) 0.0525(3) 0.2472(9) 0.224(8) Uani 1 1 d . . . O7 O 0.4629(16) 0.0854(5) 0.3309(7) 0.271(10) Uani 1 1 d . . . O8 O 0.480(2) 0.0927(9) 0.2265(15) 0.348(13) Uiso 1 1 d . . . Cl3 Cl 0.3376(2) 0.16325(8) 0.60208(15) 0.0730(7) Uani 1 1 d . . . O9 O 0.3354(8) 0.1684(4) 0.5309(5) 0.154(5) Uani 1 1 d . . . O10 O 0.2496(6) 0.1746(2) 0.6244(5) 0.104(3) Uani 1 1 d . . . O11 O 0.4167(6) 0.1885(2) 0.6366(4) 0.097(3) Uani 1 1 d . . . O12 O 0.3698(7) 0.1274(2) 0.6288(5) 0.105(3) Uani 1 1 d . . . Cl4 Cl 0.5017(5) 0.5631(2) 0.2750(3) 0.197(3) Uani 1 1 d D . . O13 O 0.5496(10) 0.5663(4) 0.2155(6) 0.188(5) Uiso 1 1 d D . . O14 O 0.5553(10) 0.5788(4) 0.3340(7) 0.200 Uiso 1 1 d D . . O15 O 0.5077(11) 0.5203(3) 0.2948(7) 0.200 Uiso 1 1 d D . . O16 O 0.3970(9) 0.5664(4) 0.2553(7) 0.200 Uiso 1 1 d D . . N13 N 0.1338(9) 0.2103(3) 0.1644(6) 0.109(4) Uani 1 1 d . . . C77 C 0.1486(12) 0.1808(4) 0.1505(7) 0.111(5) Uani 1 1 d . . . C78 C 0.1594(16) 0.1439(6) 0.1285(11) 0.183(8) Uiso 1 1 d . . . H78A H 0.2214 0.1418 0.1085 0.275 Uiso 1 1 calc R . . H78B H 0.1011 0.1372 0.0929 0.275 Uiso 1 1 calc R . . H78C H 0.1633 0.1269 0.1687 0.275 Uiso 1 1 calc R . . O22 O 0.2203(7) 0.2174(3) 0.3522(5) 0.116(3) Uiso 1 1 d D . . N14 N 0.1640(13) 0.1643(5) 0.3854(9) 0.167(6) Uiso 1 1 d D . . C79 C 0.2326(16) 0.1830(5) 0.3564(11) 0.173(5) Uiso 1 1 d D . . H79 H 0.2870 0.1707 0.3401 0.208 Uiso 1 1 calc R . . C80 C 0.1140(15) 0.1886(5) 0.4346(10) 0.173(5) Uiso 1 1 d D . . H80A H 0.0576 0.2025 0.4074 0.260 Uiso 1 1 calc R . . H80B H 0.1637 0.2064 0.4592 0.260 Uiso 1 1 calc R . . H80C H 0.0888 0.1726 0.4689 0.260 Uiso 1 1 calc R . . C81 C 0.174(3) 0.1226(7) 0.3928(18) 0.321(18) Uiso 1 1 d D . . H81A H 0.2144 0.1130 0.3591 0.481 Uiso 1 1 calc R . . H81B H 0.1067 0.1111 0.3837 0.481 Uiso 1 1 calc R . . H81C H 0.2074 0.1164 0.4405 0.481 Uiso 1 1 calc R . . O23 O 0.277(4) 0.4020(14) -0.105(3) 0.251(19) Uiso 0.423(14) 1 d PD A 1 N15 N 0.344(3) 0.3625(12) -0.015(3) 0.191(17) Uiso 0.423(14) 1 d PD A 1 C82 C 0.299(5) 0.3677(16) -0.083(3) 0.251(19) Uiso 0.423(14) 1 d PD A 1 H82 H 0.2851 0.3469 -0.1142 0.301 Uiso 0.423(14) 1 calc PR A 1 C83 C 0.349(5) 0.3962(17) 0.034(3) 0.274(15) Uiso 0.423(14) 1 d PD A 1 H83A H 0.3470 0.4194 0.0064 0.411 Uiso 0.423(14) 1 calc PR A 1 H83B H 0.4115 0.3953 0.0683 0.411 Uiso 0.423(14) 1 calc PR A 1 H83C H 0.2908 0.3957 0.0586 0.411 Uiso 0.423(14) 1 calc PR A 1 C84 C 0.351(4) 0.3240(13) 0.022(3) 0.18(2) Uiso 0.423(14) 1 d PD A 1 H84A H 0.3445 0.3042 -0.0140 0.275 Uiso 0.423(14) 1 calc PR A 1 H84B H 0.2959 0.3216 0.0488 0.275 Uiso 0.423(14) 1 calc PR A 1 H84C H 0.4159 0.3218 0.0529 0.275 Uiso 0.423(14) 1 calc PR A 1 O24 O 0.236(3) 0.3942(11) -0.180(2) 0.274(15) Uiso 0.577(14) 1 d P A 2 O25 O 0.085(2) 0.4475(7) 0.4364(13) 0.181(7) Uiso 0.547(14) 1 d P B 3 O26 O -0.001(2) 0.4388(9) 0.5206(16) 0.181(7) Uiso 0.453(14) 1 d P B 4 O27 O 0.522(4) 0.1918(15) -0.031(3) 0.294(14) Uiso 0.43(2) 1 d P C 5 O28 O 0.375(3) 0.2241(11) 0.005(2) 0.294(14) Uiso 0.57(2) 1 d P C 6 O29 O 0.464(4) 0.5136(14) 0.018(3) 0.33(2) Uiso 0.50 1 d P . 7 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 Ni1 0.0422(6) 0.0411(6) 0.0416(6) -0.0002(5) 0.0104(5) -0.0015(5) Ni2 0.0438(6) 0.0412(6) 0.0414(6) 0.0007(5) 0.0096(5) 0.0039(5) N1 0.044(4) 0.044(4) 0.046(4) -0.003(3) 0.014(3) 0.000(3) N2 0.040(4) 0.053(4) 0.041(4) 0.003(4) 0.008(3) 0.007(3) N3 0.050(4) 0.049(4) 0.045(4) 0.003(3) 0.015(3) 0.009(3) N4 0.044(4) 0.041(4) 0.045(4) 0.002(3) 0.014(3) 0.001(3) N5 0.045(4) 0.038(4) 0.039(4) 0.002(3) 0.006(3) 0.001(3) N6 0.060(5) 0.041(4) 0.046(4) -0.001(3) 0.010(3) 0.002(3) N7 0.043(4) 0.041(4) 0.044(4) 0.001(3) 0.011(3) -0.005(3) N8 0.040(4) 0.045(4) 0.036(4) -0.001(3) 0.002(3) 0.003(3) N9 0.045(4) 0.040(4) 0.050(4) 0.006(3) 0.011(3) -0.003(3) N10 0.046(4) 0.058(5) 0.041(4) 0.002(3) 0.006(3) -0.009(4) N11 0.040(4) 0.054(4) 0.042(4) 0.000(3) 0.009(3) 0.001(4) N12 0.053(4) 0.055(5) 0.042(4) 0.002(3) 0.014(3) 0.004(4) C1 0.044(5) 0.060(6) 0.047(5) -0.003(4) 0.009(4) -0.001(4) C2 0.048(5) 0.072(6) 0.043(5) -0.015(5) 0.010(4) -0.007(5) C3 0.061(6) 0.071(6) 0.058(6) -0.016(5) 0.014(5) -0.011(5) C4 0.081(8) 0.105(10) 0.069(8) -0.037(7) 0.021(6) -0.030(7) C5 0.086(8) 0.110(10) 0.048(6) -0.022(7) 0.005(6) -0.022(7) C6 0.069(7) 0.096(9) 0.054(6) 0.001(6) -0.003(5) -0.002(6) C7 0.049(5) 0.067(6) 0.043(5) -0.009(5) 0.009(4) -0.003(5) C8 0.041(5) 0.071(6) 0.040(5) -0.002(4) 0.005(4) 0.003(4) C9 0.052(5) 0.073(7) 0.039(5) 0.006(5) 0.008(4) 0.006(5) C10 0.040(5) 0.063(6) 0.049(5) 0.011(5) 0.013(4) 0.013(4) C11 0.038(5) 0.070(6) 0.057(6) 0.013(5) 0.011(4) 0.007(4) C12 0.050(6) 0.095(8) 0.053(6) 0.026(6) 0.006(5) -0.001(5) C13 0.054(6) 0.097(9) 0.064(7) 0.035(7) 0.008(5) 0.001(6) C14 0.050(6) 0.081(8) 0.096(9) 0.043(7) 0.027(6) 0.012(6) C15 0.048(5) 0.061(6) 0.082(7) 0.024(5) 0.022(5) 0.008(5) C16 0.042(5) 0.067(6) 0.058(6) 0.022(5) 0.016(4) 0.011(4) C17 0.050(5) 0.047(5) 0.071(6) 0.007(5) 0.021(5) 0.012(4) C18 0.038(4) 0.056(5) 0.043(5) -0.002(4) 0.012(4) 0.001(4) C19 0.036(4) 0.056(5) 0.040(5) 0.004(4) 0.008(4) 0.008(4) C20 0.049(5) 0.047(5) 0.046(5) 0.003(4) 0.014(4) -0.001(4) C21 0.046(5) 0.053(5) 0.046(5) 0.013(4) 0.009(4) 0.000(4) C22 0.074(7) 0.053(6) 0.070(7) 0.011(5) 0.021(6) 0.003(5) C23 0.084(8) 0.082(8) 0.058(7) 0.030(6) 0.012(6) 0.008(6) C24 0.091(8) 0.082(8) 0.057(7) 0.010(6) 0.011(6) -0.004(6) C25 0.080(7) 0.078(7) 0.046(6) 0.012(5) 0.002(5) -0.008(6) C26 0.053(5) 0.058(6) 0.050(6) 0.006(4) 0.009(4) -0.009(4) C27 0.046(5) 0.049(5) 0.043(5) 0.004(4) 0.009(4) 0.000(4) C28 0.060(6) 0.069(6) 0.037(5) -0.004(5) 0.004(4) -0.013(5) C29 0.059(6) 0.051(5) 0.045(5) -0.001(4) 0.007(4) -0.010(4) C30 0.079(7) 0.057(6) 0.047(6) -0.009(5) 0.013(5) -0.013(5) C31 0.108(9) 0.077(7) 0.057(7) -0.016(6) 0.023(6) -0.034(7) C32 0.124(10) 0.075(8) 0.060(7) -0.025(6) 0.026(7) -0.038(7) C33 0.144(12) 0.064(7) 0.079(8) -0.024(7) 0.028(8) -0.031(7) C34 0.133(11) 0.052(6) 0.068(7) -0.007(5) 0.024(7) -0.012(6) C35 0.092(8) 0.046(6) 0.056(6) -0.013(5) 0.014(5) -0.010(5) C36 0.080(7) 0.048(6) 0.061(6) 0.003(5) 0.017(5) 0.001(5) C37 0.040(4) 0.043(5) 0.043(5) 0.001(4) 0.011(4) -0.001(4) C38 0.051(5) 0.042(5) 0.049(5) 0.002(4) 0.014(4) 0.001(4) C39 0.057(5) 0.036(5) 0.046(5) -0.001(4) 0.010(4) -0.004(4) C40 0.055(5) 0.045(5) 0.035(5) 0.000(4) 0.003(4) 0.003(4) C41 0.074(7) 0.045(5) 0.055(6) -0.001(4) 0.008(5) 0.007(5) C42 0.076(7) 0.050(6) 0.078(7) -0.006(5) 0.010(6) 0.017(6) C43 0.062(6) 0.068(7) 0.088(8) -0.018(6) 0.011(6) 0.025(6) C44 0.048(5) 0.064(6) 0.070(6) -0.003(5) 0.009(5) 0.013(5) C45 0.050(5) 0.050(5) 0.042(5) -0.005(4) 0.004(4) 0.013(4) C46 0.041(5) 0.050(5) 0.038(5) 0.001(4) 0.009(4) 0.005(4) C47 0.043(5) 0.056(6) 0.059(6) 0.007(4) 0.017(4) 0.008(4) C48 0.044(5) 0.051(5) 0.056(5) 0.005(4) 0.012(4) -0.001(4) C49 0.049(6) 0.052(6) 0.096(8) 0.005(5) 0.023(5) -0.005(5) C50 0.061(7) 0.065(7) 0.181(13) 0.015(8) 0.063(8) -0.003(6) C51 0.090(10) 0.085(10) 0.24(2) 0.024(11) 0.089(12) 0.007(8) C52 0.095(10) 0.074(9) 0.26(2) 0.037(11) 0.088(12) -0.006(8) C53 0.070(8) 0.053(7) 0.195(15) 0.016(8) 0.046(9) -0.005(6) C54 0.049(6) 0.046(6) 0.109(9) 0.011(5) 0.024(6) -0.002(5) C55 0.051(5) 0.042(5) 0.067(6) 0.003(4) 0.011(5) 0.005(4) C56 0.041(5) 0.052(5) 0.037(5) -0.002(4) 0.004(4) 0.003(4) C57 0.038(4) 0.038(5) 0.043(5) 0.002(4) 0.009(4) 0.000(4) C58 0.062(6) 0.064(6) 0.042(5) -0.001(4) 0.009(4) -0.010(5) C59 0.058(6) 0.079(7) 0.041(5) 0.002(5) 0.004(4) -0.028(5) C60 0.079(7) 0.083(8) 0.050(6) -0.003(5) 0.005(5) -0.030(6) C61 0.096(10) 0.119(11) 0.067(8) 0.001(7) 0.011(7) -0.063(9) C62 0.081(9) 0.128(12) 0.082(9) -0.003(8) 0.022(7) -0.051(9) C63 0.054(6) 0.112(9) 0.071(7) -0.004(6) 0.015(5) -0.027(6) C64 0.053(6) 0.083(7) 0.046(5) -0.007(5) 0.005(4) -0.017(5) C65 0.045(5) 0.084(7) 0.044(5) 0.006(5) 0.007(4) -0.017(5) C66 0.049(5) 0.081(7) 0.062(6) 0.005(5) 0.020(5) 0.007(5) C67 0.048(5) 0.082(7) 0.061(6) 0.009(5) 0.015(5) 0.007(5) C68 0.059(6) 0.080(7) 0.085(8) 0.014(6) 0.035(6) 0.027(6) C69 0.098(10) 0.113(11) 0.149(13) 0.030(9) 0.074(10) 0.034(9) C70 0.126(13) 0.115(12) 0.22(2) 0.055(13) 0.112(14) 0.064(11) C71 0.150(15) 0.110(12) 0.22(2) 0.030(12) 0.111(14) 0.072(11) C72 0.109(10) 0.078(8) 0.143(12) 0.004(8) 0.065(9) 0.038(8) C73 0.066(7) 0.083(8) 0.079(7) 0.011(6) 0.030(6) 0.033(6) C74 0.064(6) 0.056(6) 0.056(6) 0.003(5) 0.019(5) 0.018(5) C75 0.044(5) 0.055(5) 0.041(5) 0.002(4) 0.008(4) 0.001(4) C76 0.045(5) 0.072(6) 0.038(5) 0.002(4) 0.014(4) 0.004(5) Cl1 0.0518(13) 0.0673(15) 0.0588(15) -0.0084(12) 0.0087(11) -0.0082(12) O1 0.088(5) 0.092(6) 0.084(5) 0.000(4) -0.004(4) 0.027(4) O2 0.207(11) 0.077(6) 0.073(5) -0.008(4) -0.033(6) -0.038(6) O3 0.140(8) 0.107(6) 0.060(5) 0.005(4) 0.010(5) 0.001(6) O4 0.093(7) 0.131(8) 0.238(13) 0.039(8) 0.091(8) 0.011(6) Cl2 0.104(2) 0.0620(18) 0.086(2) 0.0013(15) 0.0115(18) 0.0025(16) O5 0.31(3) 0.155(14) 0.55(4) 0.16(2) -0.05(3) 0.046(16) O6 0.286(18) 0.109(9) 0.318(19) -0.084(11) 0.167(16) -0.103(11) O7 0.35(2) 0.29(2) 0.111(10) 0.011(11) -0.126(13) -0.007(17) Cl3 0.0616(16) 0.087(2) 0.0737(18) 0.0027(15) 0.0200(13) 0.0017(14) O9 0.117(8) 0.273(15) 0.071(6) 0.008(8) 0.010(6) 0.007(8) O10 0.074(5) 0.088(6) 0.161(9) 0.008(5) 0.055(6) 0.009(4) O11 0.078(5) 0.103(6) 0.106(6) 0.008(5) 0.002(5) -0.025(5) O12 0.105(6) 0.074(6) 0.143(8) -0.015(5) 0.041(6) 0.005(5) Cl4 0.187(5) 0.293(8) 0.112(4) -0.024(4) 0.029(4) 0.113(5) N13 0.118(9) 0.076(7) 0.124(10) -0.026(7) -0.007(7) -0.014(7) C77 0.152(13) 0.058(8) 0.101(10) -0.014(7) -0.038(9) -0.002(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N4 2.069(7) . ? Ni1 N1 2.079(7) . ? Ni1 N10 2.082(7) . ? Ni1 N7 2.094(7) . ? Ni1 N8 2.217(7) . ? Ni1 N11 2.219(7) . ? Ni2 N6 2.057(7) . ? Ni2 N12 2.078(7) . ? Ni2 N9 2.080(7) . ? Ni2 N3 2.086(7) . ? Ni2 N5 2.195(6) . ? Ni2 N2 2.205(7) . ? N1 C1 1.318(10) . ? N1 C18 1.377(10) . ? N2 C19 1.335(10) . ? N2 C18 1.347(10) . ? N3 C17 1.313(10) . ? N3 C19 1.383(10) . ? N4 C20 1.316(10) . ? N4 C37 1.382(10) . ? N5 C38 1.335(10) . ? N5 C37 1.339(10) . ? N6 C36 1.306(11) . ? N6 C38 1.387(10) . ? N7 C39 1.298(10) . ? N7 C56 1.382(10) . ? N8 C57 1.335(10) . ? N8 C56 1.338(10) . ? N9 C55 1.302(10) . ? N9 C57 1.362(10) . ? N10 C58 1.298(11) . ? N10 C75 1.358(11) . ? N11 C75 1.321(10) . ? N11 C76 1.342(11) . ? N12 C74 1.303(11) . ? N12 C76 1.378(11) . ? C1 C2 1.431(12) . ? C2 C7 1.398(13) . ? C2 C3 1.405(12) . ? C3 C4 1.374(14) . ? C4 C5 1.384(16) . ? C5 C6 1.371(15) . ? C6 C7 1.416(13) . ? C7 C8 1.455(12) . ? C8 C9 1.385(12) . ? C8 C18 1.432(11) . ? C9 C10 1.377(12) . ? C10 C19 1.404(11) . ? C10 C11 1.447(12) . ? C11 C12 1.422(12) . ? C11 C16 1.429(13) . ? C12 C13 1.352(14) . ? C13 C14 1.390(15) . ? C14 C15 1.387(14) . ? C15 C16 1.398(12) . ? C16 C17 1.437(12) . ? C20 C21 1.438(11) . ? C21 C26 1.406(12) . ? C21 C22 1.409(12) . ? C22 C23 1.368(14) . ? C23 C24 1.391(15) . ? C24 C25 1.379(14) . ? C25 C26 1.389(12) . ? C26 C27 1.433(12) . ? C27 C28 1.406(12) . ? C27 C37 1.433(11) . ? C28 C29 1.387(12) . ? C29 C38 1.404(12) . ? C29 C30 1.447(12) . ? C30 C31 1.383(13) . ? C30 C35 1.400(13) . ? C31 C32 1.387(14) . ? C32 C33 1.375(16) . ? C33 C34 1.380(15) . ? C34 C35 1.416(13) . ? C35 C36 1.426(13) . ? C39 C40 1.425(12) . ? C40 C45 1.394(12) . ? C40 C41 1.401(12) . ? C41 C42 1.339(13) . ? C42 C43 1.388(14) . ? C43 C44 1.372(13) . ? C44 C45 1.396(12) . ? C45 C46 1.449(11) . ? C46 C47 1.377(12) . ? C46 C56 1.413(11) . ? C47 C48 1.391(12) . ? C48 C57 1.409(11) . ? C48 C49 1.459(12) . ? C49 C50 1.381(13) . ? C49 C54 1.403(13) . ? C50 C51 1.372(16) . ? C51 C52 1.427(18) . ? C52 C53 1.368(17) . ? C53 C54 1.404(13) . ? C54 C55 1.415(12) . ? C58 C59 1.450(13) . ? C59 C64 1.405(14) . ? C59 C60 1.409(13) . ? C60 C61 1.399(16) . ? C61 C62 1.401(18) . ? C62 C63 1.369(16) . ? C63 C64 1.426(13) . ? C64 C65 1.440(13) . ? C65 C66 1.389(13) . ? C65 C75 1.411(12) . ? C66 C67 1.410(14) . ? C67 C68 1.436(14) . ? C67 C76 1.439(12) . ? C68 C73 1.403(15) . ? C68 C69 1.419(15) . ? C69 C70 1.354(18) . ? C70 C71 1.41(2) . ? C71 C72 1.388(18) . ? C72 C73 1.409(15) . ? C73 C74 1.424(13) . ? Cl1 O2 1.382(8) . ? Cl1 O4 1.386(9) . ? Cl1 O3 1.407(8) . ? Cl1 O1 1.428(8) . ? Cl2 O5 1.253(16) . ? Cl2 O6 1.294(11) . ? Cl2 O8 1.30(3) . ? Cl2 O7 1.302(12) . ? Cl3 O9 1.385(10) . ? Cl3 O10 1.387(8) . ? Cl3 O12 1.415(9) . ? Cl3 O11 1.462(8) . ? Cl4 O14 1.358(11) . ? Cl4 O16 1.396(11) . ? Cl4 O13 1.418(11) . ? Cl4 O15 1.571(11) . ? N13 C77 1.110(14) . ? C77 C78 1.40(2) . ? O22 C79 1.240(15) . ? N14 C79 1.336(15) . ? N14 C81 1.496(18) . ? N14 C80 1.527(15) . ? O23 C82 1.31(2) . ? N15 C82 1.37(2) . ? N15 C83 1.52(2) . ? N15 C84 1.53(2) . ? O29 O29 1.59(9) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ni1 N1 174.7(3) . . ? N4 Ni1 N10 91.5(3) . . ? N1 Ni1 N10 91.8(3) . . ? N4 Ni1 N7 92.9(2) . . ? N1 Ni1 N7 90.0(2) . . ? N10 Ni1 N7 107.6(3) . . ? N4 Ni1 N8 91.0(2) . . ? N1 Ni1 N8 86.5(2) . . ? N10 Ni1 N8 170.3(3) . . ? N7 Ni1 N8 62.8(2) . . ? N4 Ni1 N11 88.4(2) . . ? N1 Ni1 N11 89.5(2) . . ? N10 Ni1 N11 61.9(3) . . ? N7 Ni1 N11 169.5(3) . . ? N8 Ni1 N11 127.6(3) . . ? N6 Ni2 N12 90.9(3) . . ? N6 Ni2 N9 91.9(3) . . ? N12 Ni2 N9 175.9(3) . . ? N6 Ni2 N3 105.7(3) . . ? N12 Ni2 N3 92.3(3) . . ? N9 Ni2 N3 89.8(3) . . ? N6 Ni2 N5 63.2(3) . . ? N12 Ni2 N5 88.4(3) . . ? N9 Ni2 N5 90.2(2) . . ? N3 Ni2 N5 168.8(3) . . ? N6 Ni2 N2 168.3(3) . . ? N12 Ni2 N2 90.2(3) . . ? N9 Ni2 N2 87.6(3) . . ? N3 Ni2 N2 62.7(3) . . ? N5 Ni2 N2 128.5(2) . . ? C1 N1 C18 117.7(7) . . ? C1 N1 Ni1 119.9(6) . . ? C18 N1 Ni1 122.4(5) . . ? C19 N2 C18 118.1(7) . . ? C19 N2 Ni2 91.5(5) . . ? C18 N2 Ni2 150.3(6) . . ? C17 N3 C19 118.9(8) . . ? C17 N3 Ni2 145.7(7) . . ? C19 N3 Ni2 95.3(5) . . ? C20 N4 C37 117.5(7) . . ? C20 N4 Ni1 120.6(6) . . ? C37 N4 Ni1 121.9(5) . . ? C38 N5 C37 117.8(7) . . ? C38 N5 Ni2 91.2(5) . . ? C37 N5 Ni2 151.1(6) . . ? C36 N6 C38 118.3(8) . . ? C36 N6 Ni2 146.0(6) . . ? C38 N6 Ni2 95.7(5) . . ? C39 N7 C56 118.2(7) . . ? C39 N7 Ni1 146.9(6) . . ? C56 N7 Ni1 94.7(5) . . ? C57 N8 C56 118.6(7) . . ? C57 N8 Ni1 150.7(5) . . ? C56 N8 Ni1 90.6(5) . . ? C55 N9 C57 118.0(7) . . ? C55 N9 Ni2 120.0(6) . . ? C57 N9 Ni2 121.9(5) . . ? C58 N10 C75 119.9(8) . . ? C58 N10 Ni1 144.3(7) . . ? C75 N10 Ni1 95.8(5) . . ? C75 N11 C76 118.9(7) . . ? C75 N11 Ni1 90.8(5) . . ? C76 N11 Ni1 150.3(6) . . ? C74 N12 C76 119.7(8) . . ? C74 N12 Ni2 119.9(6) . . ? C76 N12 Ni2 120.4(6) . . ? N1 C1 C2 124.5(8) . . ? C7 C2 C3 121.2(8) . . ? C7 C2 C1 119.0(8) . . ? C3 C2 C1 119.8(9) . . ? C4 C3 C2 118.9(10) . . ? C3 C4 C5 120.7(11) . . ? C6 C5 C4 121.0(10) . . ? C5 C6 C7 120.1(11) . . ? C2 C7 C6 118.1(9) . . ? C2 C7 C8 118.2(8) . . ? C6 C7 C8 123.7(9) . . ? C9 C8 C18 118.4(8) . . ? C9 C8 C7 124.6(8) . . ? C18 C8 C7 117.1(8) . . ? C10 C9 C8 121.3(8) . . ? C9 C10 C19 115.9(8) . . ? C9 C10 C11 126.9(8) . . ? C19 C10 C11 117.2(8) . . ? C12 C11 C16 117.6(9) . . ? C12 C11 C10 124.6(9) . . ? C16 C11 C10 117.8(8) . . ? C13 C12 C11 119.5(11) . . ? C12 C13 C14 122.8(10) . . ? C15 C14 C13 120.0(10) . . ? C14 C15 C16 118.6(10) . . ? C15 C16 C11 121.4(9) . . ? C15 C16 C17 119.3(10) . . ? C11 C16 C17 119.2(8) . . ? N3 C17 C16 122.6(9) . . ? N2 C18 N1 115.5(7) . . ? N2 C18 C8 120.9(8) . . ? N1 C18 C8 123.5(8) . . ? N2 C19 N3 110.5(7) . . ? N2 C19 C10 125.4(8) . . ? N3 C19 C10 124.2(8) . . ? N4 C20 C21 124.5(8) . . ? C26 C21 C22 120.2(8) . . ? C26 C21 C20 119.2(8) . . ? C22 C21 C20 120.6(8) . . ? C23 C22 C21 119.6(10) . . ? C22 C23 C24 121.1(10) . . ? C25 C24 C23 118.9(10) . . ? C24 C25 C26 122.2(10) . . ? C25 C26 C21 118.0(8) . . ? C25 C26 C27 124.8(9) . . ? C21 C26 C27 117.2(8) . . ? C28 C27 C26 123.7(8) . . ? C28 C27 C37 117.4(7) . . ? C26 C27 C37 118.9(8) . . ? C29 C28 C27 121.6(8) . . ? C28 C29 C38 115.0(8) . . ? C28 C29 C30 127.0(8) . . ? C38 C29 C30 118.0(8) . . ? C31 C30 C35 119.0(9) . . ? C31 C30 C29 124.4(9) . . ? C35 C30 C29 116.5(8) . . ? C30 C31 C32 120.3(11) . . ? C33 C32 C31 121.2(11) . . ? C32 C33 C34 119.9(10) . . ? C33 C34 C35 119.4(11) . . ? C30 C35 C34 120.2(9) . . ? C30 C35 C36 121.0(8) . . ? C34 C35 C36 118.8(9) . . ? N6 C36 C35 122.6(9) . . ? N5 C37 N4 115.6(7) . . ? N5 C37 C27 121.9(7) . . ? N4 C37 C27 122.6(7) . . ? N5 C38 N6 110.0(7) . . ? N5 C38 C29 126.4(8) . . ? N6 C38 C29 123.6(8) . . ? N7 C39 C40 124.0(8) . . ? C45 C40 C41 120.3(8) . . ? C45 C40 C39 119.2(7) . . ? C41 C40 C39 120.4(8) . . ? C42 C41 C40 120.6(9) . . ? C41 C42 C43 119.4(9) . . ? C44 C43 C42 121.7(9) . . ? C43 C44 C45 119.4(10) . . ? C40 C45 C44 118.5(8) . . ? C40 C45 C46 118.2(7) . . ? C44 C45 C46 123.3(8) . . ? C47 C46 C56 115.2(7) . . ? C47 C46 C45 127.9(8) . . ? C56 C46 C45 116.9(7) . . ? C46 C47 C48 121.3(8) . . ? C47 C48 C57 119.0(8) . . ? C47 C48 C49 123.0(8) . . ? C57 C48 C49 118.0(8) . . ? C50 C49 C54 119.1(9) . . ? C50 C49 C48 123.9(9) . . ? C54 C49 C48 117.0(8) . . ? C51 C50 C49 120.8(11) . . ? C50 C51 C52 120.1(12) . . ? C53 C52 C51 119.5(11) . . ? C52 C53 C54 119.5(11) . . ? C49 C54 C53 120.7(9) . . ? C49 C54 C55 118.5(8) . . ? C53 C54 C55 120.8(9) . . ? N9 C55 C54 125.3(8) . . ? N8 C56 N7 111.5(7) . . ? N8 C56 C46 125.0(8) . . ? N7 C56 C46 123.4(7) . . ? N8 C57 N9 115.9(7) . . ? N8 C57 C48 121.0(7) . . ? N9 C57 C48 123.1(7) . . ? N10 C58 C59 122.2(9) . . ? C64 C59 C60 121.8(9) . . ? C64 C59 C58 118.5(9) . . ? C60 C59 C58 119.7(10) . . ? C61 C60 C59 118.8(12) . . ? C60 C61 C62 118.9(12) . . ? C63 C62 C61 123.2(12) . . ? C62 C63 C64 118.8(12) . . ? C59 C64 C63 118.5(10) . . ? C59 C64 C65 118.9(9) . . ? C63 C64 C65 122.6(10) . . ? C66 C65 C75 116.9(9) . . ? C66 C65 C64 126.6(9) . . ? C75 C65 C64 116.5(9) . . ? C65 C66 C67 120.6(9) . . ? C66 C67 C68 124.6(9) . . ? C66 C67 C76 116.9(9) . . ? C68 C67 C76 118.5(9) . . ? C73 C68 C69 118.5(10) . . ? C73 C68 C67 118.1(9) . . ? C69 C68 C67 123.4(11) . . ? C70 C69 C68 120.6(14) . . ? C69 C70 C71 119.9(13) . . ? C72 C71 C70 122.3(13) . . ? C71 C72 C73 116.9(13) . . ? C68 C73 C72 121.8(10) . . ? C68 C73 C74 118.8(9) . . ? C72 C73 C74 119.4(11) . . ? N12 C74 C73 124.0(10) . . ? N11 C75 N10 111.5(7) . . ? N11 C75 C65 124.6(8) . . ? N10 C75 C65 123.9(8) . . ? N11 C76 N12 117.0(7) . . ? N11 C76 C67 122.1(9) . . ? N12 C76 C67 120.9(9) . . ? O2 Cl1 O4 110.6(7) . . ? O2 Cl1 O3 109.7(5) . . ? O4 Cl1 O3 107.3(7) . . ? O2 Cl1 O1 111.3(6) . . ? O4 Cl1 O1 107.4(6) . . ? O3 Cl1 O1 110.4(5) . . ? O5 Cl2 O6 129.0(15) . . ? O5 Cl2 O8 92.5(16) . . ? O6 Cl2 O8 98.1(14) . . ? O5 Cl2 O7 116.2(16) . . ? O6 Cl2 O7 107.9(12) . . ? O8 Cl2 O7 106.9(17) . . ? O9 Cl3 O10 113.5(6) . . ? O9 Cl3 O12 115.8(7) . . ? O10 Cl3 O12 111.8(5) . . ? O9 Cl3 O11 105.2(6) . . ? O10 Cl3 O11 105.7(5) . . ? O12 Cl3 O11 103.6(5) . . ? O14 Cl4 O16 123.9(8) . . ? O14 Cl4 O13 113.6(8) . . ? O16 Cl4 O13 110.3(8) . . ? O14 Cl4 O15 101.3(7) . . ? O16 Cl4 O15 98.9(8) . . ? O13 Cl4 O15 105.3(7) . . ? N13 C77 C78 174.9(17) . . ? C79 N14 C81 119(2) . . ? C79 N14 C80 112.9(18) . . ? C81 N14 C80 123(2) . . ? O22 C79 N14 115(2) . . ? C82 N15 C83 117(5) . . ? C82 N15 C84 123(5) . . ? C83 N15 C84 116(5) . . ? O23 C82 N15 118(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.748 _refine_diff_density_min -1.144 _refine_diff_density_rms 0.194 # Attachment '- ic14328-re-revised-Co.cif' data_ic14328 _database_code_depnum_ccdc_archive 'CCDC 875007' #TrackingRef '- ic14328-re-revised-Co.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H64.50 Cl4 Co2 N15.50 O17.50' _chemical_formula_weight 1866.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.6511(2) _cell_length_b 70.3157(11) _cell_length_c 18.9770(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.703(2) _cell_angle_gamma 90.00 _cell_volume 17955.2(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12668 _cell_measurement_theta_min 3.1398 _cell_measurement_theta_max 75.9578 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7656 _exptl_absorpt_coefficient_mu 4.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74887 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55043 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.1154 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -68 _diffrn_reflns_limit_k_max 84 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 68.00 _reflns_number_total 32434 _reflns_number_gt 17397 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. During the structure refinement, the atoms of the (MeCN & Ether & water) solvent molecule were observed but could not be modelled satisfactorily. The atoms of solvent were refined isotropically with restrained geometry, some of MeCN used anisotropic restraints. 2175 parameters refined using 195 restraints. H atoms were placed in calculated positions and treated as riding atoms using SHELXL default parameters. ; _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^)+(0.1200P)^2^+24.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 32434 _refine_ls_number_parameters 2175 _refine_ls_number_restraints 189 _refine_ls_R_factor_all 0.2003 _refine_ls_R_factor_gt 0.1398 _refine_ls_wR_factor_ref 0.3707 _refine_ls_wR_factor_gt 0.3507 _refine_ls_goodness_of_fit_ref 1.502 _refine_ls_restrained_S_all 1.504 _refine_ls_shift/su_max 0.098 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.21319(11) 0.03670(2) 0.73917(7) 0.0291(4) Uani 1 1 d . . . Co2 Co 0.18584(11) 0.08382(2) 0.74296(7) 0.0290(4) Uani 1 1 d . . . Co3 Co 0.64765(12) 0.16616(2) 0.24357(8) 0.0328(4) Uani 1 1 d . . . Co4 Co 0.62546(12) 0.21358(2) 0.22926(8) 0.0320(4) Uani 1 1 d . . . N1 N 0.0681(6) 0.03407(11) 0.7662(4) 0.0349(19) Uani 1 1 d . . . N2 N 0.0540(6) 0.06655(11) 0.7663(4) 0.0317(18) Uani 1 1 d . . . N3 N 0.0572(6) 0.09839(12) 0.7632(4) 0.0345(19) Uani 1 1 d . . . N4 N 0.3567(6) 0.04167(11) 0.7140(4) 0.0319(18) Uani 1 1 d . . . N5 N 0.3303(6) 0.07377(11) 0.7149(4) 0.0321(18) Uani 1 1 d . . . N6 N 0.2903(6) 0.10471(11) 0.7205(4) 0.0320(18) Uani 1 1 d . . . N7 N 0.2716(6) 0.01858(11) 0.8234(4) 0.0337(19) Uani 1 1 d . . . N8 N 0.2633(5) 0.04958(11) 0.8450(4) 0.0283(17) Uani 1 1 d . . . N9 N 0.2482(6) 0.08205(12) 0.8547(4) 0.0342(19) Uani 1 1 d . . . N10 N 0.1773(6) 0.01807(11) 0.6496(4) 0.0297(18) Uani 1 1 d . . . N11 N 0.1496(5) 0.04947(10) 0.6341(4) 0.0267(17) Uani 1 1 d . . . N12 N 0.1260(6) 0.08170(11) 0.6305(4) 0.0307(18) Uani 1 1 d . . . N13 N 0.7055(6) 0.17025(11) 0.3533(4) 0.0334(19) Uani 1 1 d . . . N14 N 0.6866(6) 0.20264(10) 0.3375(4) 0.0331(19) Uani 1 1 d . . . N15 N 0.6636(7) 0.23351(11) 0.3114(4) 0.039(2) Uani 1 1 d . . . N16 N 0.5867(6) 0.16531(11) 0.1320(4) 0.039(2) Uani 1 1 d . . . N17 N 0.5774(6) 0.19828(11) 0.1274(4) 0.0335(19) Uani 1 1 d . . . N18 N 0.5756(6) 0.22992(11) 0.1347(4) 0.036(2) Uani 1 1 d . . . N19 N 0.5384(6) 0.14688(12) 0.2678(4) 0.0358(19) Uani 1 1 d . . . N20 N 0.5020(6) 0.17822(11) 0.2631(4) 0.0314(18) Uani 1 1 d . . . N21 N 0.4790(6) 0.21056(12) 0.2526(4) 0.037(2) Uani 1 1 d . . . N22 N 0.7714(6) 0.14963(12) 0.2251(4) 0.039(2) Uani 1 1 d . . . N23 N 0.7792(6) 0.18160(12) 0.2134(4) 0.038(2) Uani 1 1 d . . . N24 N 0.7724(6) 0.21435(12) 0.2043(4) 0.041(2) Uani 1 1 d . . . C1 C 0.0332(8) 0.01768(16) 0.7764(5) 0.040(2) Uani 1 1 d . . . H1A H 0.0738 0.0070 0.7711 0.048 Uiso 1 1 calc R . . C2 C -0.0630(8) 0.01409(15) 0.7954(5) 0.041(3) Uani 1 1 d . . . C3 C -0.0976(9) -0.00502(17) 0.8027(6) 0.055(3) Uani 1 1 d . . . H3A H -0.0564 -0.0156 0.7970 0.067 Uiso 1 1 calc R . . C4 C -0.1892(10) -0.0076(2) 0.8178(7) 0.066(4) Uani 1 1 d . . . H4A H -0.2130 -0.0201 0.8222 0.079 Uiso 1 1 calc R . . C5 C -0.2513(10) 0.00800(19) 0.8273(7) 0.065(4) Uani 1 1 d . . . H5A H -0.3157 0.0056 0.8381 0.078 Uiso 1 1 calc R . . C6 C -0.2202(8) 0.02690(16) 0.8214(6) 0.047(3) Uani 1 1 d . . . H6A H -0.2626 0.0372 0.8278 0.056 Uiso 1 1 calc R . . C7 C -0.1231(8) 0.03012(16) 0.8053(5) 0.043(3) Uani 1 1 d . . . C8 C -0.0848(7) 0.04834(14) 0.7954(5) 0.032(2) Uani 1 1 d . . . C9 C 0.0127(7) 0.04979(14) 0.7765(5) 0.032(2) Uani 1 1 d . . . C10 C -0.1340(7) 0.06524(15) 0.8020(5) 0.039(3) Uani 1 1 d . . . H10A H -0.1988 0.0648 0.8140 0.047 Uiso 1 1 calc R . . C11 C -0.0928(7) 0.08301(15) 0.7919(5) 0.036(2) Uani 1 1 d . . . C12 C 0.0031(7) 0.08233(14) 0.7748(5) 0.033(2) Uani 1 1 d . . . C13 C -0.1374(8) 0.10124(15) 0.7975(5) 0.038(2) Uani 1 1 d . . . C14 C -0.2327(8) 0.10398(17) 0.8134(5) 0.047(3) Uani 1 1 d . . . H14A H -0.2722 0.0933 0.8211 0.056 Uiso 1 1 calc R . . C15 C -0.2696(9) 0.12207(18) 0.8179(6) 0.055(3) Uani 1 1 d . . . H15A H -0.3348 0.1237 0.8281 0.066 Uiso 1 1 calc R . . C16 C -0.2128(9) 0.13793(17) 0.8077(6) 0.053(3) Uani 1 1 d . . . H16A H -0.2385 0.1503 0.8127 0.064 Uiso 1 1 calc R . . C17 C -0.1202(8) 0.13579(16) 0.7905(5) 0.046(3) Uani 1 1 d . . . H17A H -0.0825 0.1466 0.7814 0.055 Uiso 1 1 calc R . . C18 C -0.0821(8) 0.11765(14) 0.7867(5) 0.039(3) Uani 1 1 d . . . C19 C 0.0166(8) 0.11487(15) 0.7676(5) 0.040(3) Uani 1 1 d . . . H19A H 0.0528 0.1258 0.7578 0.048 Uiso 1 1 calc R . . C20 C 0.4134(7) 0.02713(14) 0.7042(5) 0.032(2) Uani 1 1 d . . . H20A H 0.3884 0.0147 0.7100 0.039 Uiso 1 1 calc R . . C21 C 0.5114(7) 0.02876(14) 0.6853(5) 0.035(2) Uani 1 1 d . . . C22 C 0.5638(8) 0.01267(15) 0.6744(6) 0.044(3) Uani 1 1 d . . . H22A H 0.5368 0.0005 0.6806 0.053 Uiso 1 1 calc R . . C23 C 0.6556(9) 0.01433(17) 0.6543(6) 0.057(3) Uani 1 1 d . . . H23A H 0.6922 0.0033 0.6462 0.069 Uiso 1 1 calc R . . C24 C 0.6955(9) 0.03279(17) 0.6458(7) 0.058(3) Uani 1 1 d . . . H24A H 0.7599 0.0340 0.6335 0.070 Uiso 1 1 calc R . . C25 C 0.6423(8) 0.04851(16) 0.6550(6) 0.051(3) Uani 1 1 d . . . H25A H 0.6691 0.0607 0.6482 0.061 Uiso 1 1 calc R . . C26 C 0.5469(7) 0.04700(14) 0.6747(5) 0.034(2) Uani 1 1 d . . . C27 C 0.4855(7) 0.06323(13) 0.6836(4) 0.030(2) Uani 1 1 d . . . C28 C 0.3900(7) 0.05971(13) 0.7026(4) 0.027(2) Uani 1 1 d . . . C29 C 0.5125(7) 0.08195(14) 0.6739(5) 0.032(2) Uani 1 1 d . . . H29A H 0.5737 0.0846 0.6584 0.039 Uiso 1 1 calc R . . C30 C 0.4511(7) 0.09693(14) 0.6868(5) 0.033(2) Uani 1 1 d . . . C31 C 0.3615(7) 0.09181(14) 0.7063(4) 0.029(2) Uani 1 1 d . . . C32 C 0.4715(7) 0.11699(13) 0.6789(5) 0.033(2) Uani 1 1 d . . . C33 C 0.5597(8) 0.12459(15) 0.6624(5) 0.039(2) Uani 1 1 d . . . H33A H 0.6129 0.1164 0.6559 0.047 Uiso 1 1 calc R . . C34 C 0.5684(9) 0.14381(17) 0.6557(6) 0.054(3) Uani 1 1 d . . . H34A H 0.6275 0.1487 0.6420 0.065 Uiso 1 1 calc R . . C35 C 0.4959(8) 0.15671(16) 0.6678(6) 0.048(3) Uani 1 1 d . . . H35A H 0.5055 0.1700 0.6630 0.058 Uiso 1 1 calc R . . C36 C 0.4081(8) 0.14958(15) 0.6873(5) 0.043(3) Uani 1 1 d . . . H36A H 0.3579 0.1581 0.6971 0.052 Uiso 1 1 calc R . . C37 C 0.3950(7) 0.13003(14) 0.6923(5) 0.033(2) Uani 1 1 d . . . C38 C 0.3080(7) 0.12270(14) 0.7136(5) 0.032(2) Uani 1 1 d . . . H38A H 0.2593 0.1315 0.7236 0.039 Uiso 1 1 calc R . . C39 C 0.2946(9) 0.00109(16) 0.8433(6) 0.050(3) Uani 1 1 d . . . H39A H 0.2824 -0.0086 0.8082 0.060 Uiso 1 1 calc R . . C40 C 0.3370(8) -0.00430(15) 0.9148(5) 0.042(3) Uani 1 1 d . . . C41 C 0.3604(10) -0.02317(16) 0.9310(7) 0.058(3) Uani 1 1 d . . . H41A H 0.3486 -0.0326 0.8946 0.070 Uiso 1 1 calc R . . C42 C 0.4003(9) -0.02812(19) 0.9991(7) 0.060(3) Uani 1 1 d . . . H42A H 0.4158 -0.0410 1.0105 0.072 Uiso 1 1 calc R . . C43 C 0.4187(10) -0.01403(17) 1.0530(7) 0.060(3) Uani 1 1 d . . . H43A H 0.4489 -0.0175 1.1001 0.071 Uiso 1 1 calc R . . C44 C 0.3933(9) 0.00444(17) 1.0376(6) 0.052(3) Uani 1 1 d . . . H44A H 0.4039 0.0137 1.0744 0.062 Uiso 1 1 calc R . . C45 C 0.3525(8) 0.00976(15) 0.9690(5) 0.041(3) Uani 1 1 d . . . C46 C 0.3280(7) 0.02942(15) 0.9468(5) 0.038(2) Uani 1 1 d . . . C47 C 0.2882(7) 0.03254(14) 0.8741(5) 0.034(2) Uani 1 1 d . . . C48 C 0.3407(8) 0.04552(15) 0.9908(5) 0.040(3) Uani 1 1 d . . . H48A H 0.3664 0.0441 1.0402 0.048 Uiso 1 1 calc R . . C49 C 0.3163(7) 0.06342(15) 0.9632(5) 0.033(2) Uani 1 1 d . . . C50 C 0.2753(7) 0.06471(14) 0.8872(5) 0.031(2) Uani 1 1 d . . . C51 C 0.3246(7) 0.08065(16) 1.0033(5) 0.041(3) Uani 1 1 d . . . C52 C 0.3569(9) 0.08101(18) 1.0779(6) 0.057(3) Uani 1 1 d . . . H52A H 0.3748 0.0696 1.1033 0.069 Uiso 1 1 calc R . . C53 C 0.3622(9) 0.09801(18) 1.1132(6) 0.056(3) Uani 1 1 d . . . H53A H 0.3857 0.0982 1.1633 0.067 Uiso 1 1 calc R . . C54 C 0.3342(9) 0.11496(18) 1.0781(6) 0.058(3) Uani 1 1 d . . . H54A H 0.3382 0.1266 1.1041 0.069 Uiso 1 1 calc R . . C55 C 0.3015(8) 0.11488(16) 1.0072(6) 0.048(3) Uani 1 1 d . . . H55A H 0.2831 0.1265 0.9829 0.057 Uiso 1 1 calc R . . C56 C 0.2944(7) 0.09771(15) 0.9690(5) 0.037(2) Uani 1 1 d . . . C57 C 0.2561(7) 0.09747(15) 0.8917(5) 0.038(2) Uani 1 1 d . . . H57A H 0.2364 0.1091 0.8683 0.046 Uiso 1 1 calc R . . C58 C 0.1777(7) 0.00044(14) 0.6267(5) 0.035(2) Uani 1 1 d . . . H58A H 0.1982 -0.0095 0.6600 0.042 Uiso 1 1 calc R . . C59 C 0.1476(7) -0.00424(14) 0.5516(5) 0.036(2) Uani 1 1 d . . . C60 C 0.1462(8) -0.02363(15) 0.5317(6) 0.045(3) Uani 1 1 d . . . H60A H 0.1650 -0.0332 0.5666 0.054 Uiso 1 1 calc R . . C61 C 0.1169(8) -0.02847(16) 0.4604(6) 0.045(3) Uani 1 1 d . . . H61A H 0.1137 -0.0414 0.4461 0.055 Uiso 1 1 calc R . . C62 C 0.0918(8) -0.01373(17) 0.4090(6) 0.049(3) Uani 1 1 d . . . H62A H 0.0741 -0.0170 0.3599 0.059 Uiso 1 1 calc R . . C63 C 0.0925(7) 0.00507(16) 0.4286(5) 0.041(3) Uani 1 1 d . . . H63A H 0.0747 0.0146 0.3935 0.050 Uiso 1 1 calc R . . C64 C 0.1198(7) 0.01014(15) 0.5014(6) 0.038(2) Uani 1 1 d . . . C65 C 0.1189(7) 0.02958(14) 0.5274(5) 0.033(2) Uani 1 1 d . . . C66 C 0.1489(6) 0.03233(13) 0.6014(5) 0.029(2) Uani 1 1 d . . . C67 C 0.0882(7) 0.04560(14) 0.4882(5) 0.033(2) Uani 1 1 d . . . H67A H 0.0677 0.0444 0.4380 0.040 Uiso 1 1 calc R . . C68 C 0.0862(7) 0.06339(14) 0.5193(5) 0.030(2) Uani 1 1 d . . . C69 C 0.1218(6) 0.06468(13) 0.5953(5) 0.028(2) Uani 1 1 d . . . C70 C 0.0529(7) 0.08057(14) 0.4821(5) 0.033(2) Uani 1 1 d . . . C71 C 0.0123(8) 0.08100(16) 0.4086(5) 0.042(3) Uani 1 1 d . . . H71A H 0.0059 0.0697 0.3806 0.051 Uiso 1 1 calc R . . C72 C -0.0179(8) 0.09851(17) 0.3785(5) 0.051(3) Uani 1 1 d . . . H72A H -0.0418 0.0990 0.3285 0.061 Uiso 1 1 calc R . . C73 C -0.0154(8) 0.11520(18) 0.4170(6) 0.051(3) Uani 1 1 d . . . H73A H -0.0410 0.1267 0.3947 0.061 Uiso 1 1 calc R . . C74 C 0.0251(7) 0.11486(15) 0.4884(6) 0.041(3) Uani 1 1 d . . . H74A H 0.0316 0.1263 0.5153 0.050 Uiso 1 1 calc R . . C75 C 0.0564(7) 0.09773(15) 0.5213(5) 0.033(2) Uani 1 1 d . . . C76 C 0.0957(6) 0.09731(14) 0.5948(5) 0.030(2) Uani 1 1 d . . . H76A H 0.1007 0.1090 0.6203 0.036 Uiso 1 1 calc R . . C77 C 0.7321(7) 0.15548(14) 0.3950(5) 0.034(2) Uani 1 1 d . . . H77A H 0.7252 0.1432 0.3739 0.040 Uiso 1 1 calc R . . C78 C 0.7704(7) 0.15659(14) 0.4697(5) 0.035(2) Uani 1 1 d . . . C79 C 0.7957(7) 0.13995(15) 0.5095(6) 0.040(3) Uani 1 1 d . . . H79A H 0.7908 0.1278 0.4871 0.049 Uiso 1 1 calc R . . C80 C 0.8277(9) 0.14169(16) 0.5814(6) 0.056(3) Uani 1 1 d . . . H80A H 0.8443 0.1305 0.6091 0.067 Uiso 1 1 calc R . . C81 C 0.8368(8) 0.15932(15) 0.6156(5) 0.048(3) Uani 1 1 d . . . H81A H 0.8609 0.1599 0.6655 0.057 Uiso 1 1 calc R . . C82 C 0.8114(8) 0.17601(16) 0.5779(6) 0.048(3) Uani 1 1 d . . . H82A H 0.8164 0.1880 0.6015 0.058 Uiso 1 1 calc R . . C83 C 0.7777(7) 0.17466(14) 0.5030(5) 0.035(2) Uani 1 1 d . . . C84 C 0.7503(7) 0.19111(14) 0.4578(5) 0.036(2) Uani 1 1 d . . . C85 C 0.7144(7) 0.18821(13) 0.3844(5) 0.030(2) Uani 1 1 d . . . C86 C 0.7582(8) 0.20980(14) 0.4834(5) 0.038(2) Uani 1 1 d . . . H86A H 0.7841 0.2123 0.5322 0.045 Uiso 1 1 calc R . . C87 C 0.7276(8) 0.22477(15) 0.4365(6) 0.042(3) Uani 1 1 d . . . C88 C 0.6954(7) 0.22010(13) 0.3652(5) 0.032(2) Uani 1 1 d . . . C89 C 0.7373(8) 0.24506(14) 0.4562(6) 0.040(2) Uani 1 1 d . . . C90 C 0.7758(8) 0.25195(15) 0.5243(5) 0.042(3) Uani 1 1 d . . . H90A H 0.7957 0.2433 0.5626 0.051 Uiso 1 1 calc R . . C91 C 0.7847(8) 0.27116(16) 0.5356(6) 0.049(3) Uani 1 1 d . . . H91A H 0.8120 0.2758 0.5818 0.059 Uiso 1 1 calc R . . C92 C 0.7544(9) 0.28398(16) 0.4806(7) 0.057(3) Uani 1 1 d . . . H92A H 0.7606 0.2972 0.4897 0.069 Uiso 1 1 calc R . . C93 C 0.7155(8) 0.27765(15) 0.4127(6) 0.048(3) Uani 1 1 d . . . H93A H 0.6947 0.2864 0.3751 0.057 Uiso 1 1 calc R . . C94 C 0.7074(8) 0.25811(15) 0.4005(6) 0.044(3) Uani 1 1 d . . . C95 C 0.6721(8) 0.25118(15) 0.3282(6) 0.044(3) Uani 1 1 d . . . H95A H 0.6543 0.2603 0.2914 0.053 Uiso 1 1 calc R . . C96 C 0.5741(8) 0.14928(15) 0.1001(5) 0.040(3) Uani 1 1 d . . . H96A H 0.5883 0.1382 0.1286 0.048 Uiso 1 1 calc R . . C97 C 0.5406(7) 0.14657(15) 0.0254(5) 0.038(2) Uani 1 1 d . . . C98 C 0.5324(8) 0.12842(16) -0.0035(6) 0.047(3) Uani 1 1 d . . . H98A H 0.5480 0.1177 0.0269 0.056 Uiso 1 1 calc R . . C99 C 0.5017(9) 0.12570(17) -0.0759(6) 0.050(3) Uani 1 1 d . . . H99A H 0.4962 0.1133 -0.0963 0.060 Uiso 1 1 calc R . . C100 C 0.4794(9) 0.1417(2) -0.1173(6) 0.062(4) Uani 1 1 d . . . H10B H 0.4602 0.1401 -0.1674 0.075 Uiso 1 1 calc R . . C101 C 0.4834(8) 0.15988(16) -0.0905(5) 0.046(3) Uani 1 1 d . . . H10C H 0.4644 0.1704 -0.1211 0.055 Uiso 1 1 calc R . . C102 C 0.5156(7) 0.16250(15) -0.0184(5) 0.039(2) Uani 1 1 d . . . C103 C 0.5278(7) 0.18121(14) 0.0174(5) 0.035(2) Uani 1 1 d . . . C104 C 0.5632(7) 0.18163(14) 0.0918(5) 0.033(2) Uani 1 1 d . . . C105 C 0.5082(7) 0.19802(14) -0.0187(5) 0.036(2) Uani 1 1 d . . . H10D H 0.4848 0.1979 -0.0688 0.043 Uiso 1 1 calc R . . C106 C 0.5220(7) 0.21505(14) 0.0171(5) 0.035(2) Uani 1 1 d . . . C107 C 0.5578(7) 0.21423(14) 0.0905(5) 0.033(2) Uani 1 1 d . . . C108 C 0.5039(7) 0.23431(14) -0.0150(5) 0.037(2) Uani 1 1 d . . . C109 C 0.4680(8) 0.23719(16) -0.0879(5) 0.043(3) Uani 1 1 d . . . H10E H 0.4548 0.2268 -0.1203 0.052 Uiso 1 1 calc R . . C110 C 0.4525(9) 0.25600(17) -0.1105(7) 0.055(3) Uani 1 1 d . . . H11A H 0.4258 0.2581 -0.1594 0.067 Uiso 1 1 calc R . . C111 C 0.4729(10) 0.27158(18) -0.0675(6) 0.061(4) Uani 1 1 d . . . H11B H 0.4612 0.2841 -0.0863 0.074 Uiso 1 1 calc R . . C112 C 0.5111(9) 0.26873(16) 0.0046(7) 0.057(3) Uani 1 1 d . . . H11C H 0.5280 0.2792 0.0357 0.068 Uiso 1 1 calc R . . C113 C 0.5244(7) 0.24963(14) 0.0309(5) 0.039(2) Uani 1 1 d . . . C114 C 0.5603(8) 0.24670(15) 0.1059(6) 0.041(3) Uani 1 1 d . . . H11D H 0.5733 0.2575 0.1359 0.049 Uiso 1 1 calc R . . C115 C 0.5155(8) 0.12936(15) 0.2774(5) 0.042(3) Uani 1 1 d . . . H11E H 0.5628 0.1198 0.2717 0.050 Uiso 1 1 calc R . . C116 C 0.4201(9) 0.12338(16) 0.2966(5) 0.044(3) Uani 1 1 d . . . C117 C 0.4037(10) 0.10398(16) 0.3080(5) 0.053(3) Uani 1 1 d . . . H11F H 0.4527 0.0948 0.3026 0.064 Uiso 1 1 calc RD . . C118 C 0.3149(10) 0.09872(19) 0.3271(6) 0.060(4) Uani 1 1 d . . . H11G H 0.3031 0.0858 0.3371 0.072 Uiso 1 1 calc RD . . C119 C 0.2425(10) 0.1122(2) 0.3320(6) 0.065(4) Uani 1 1 d . . . H11H H 0.1801 0.1082 0.3426 0.078 Uiso 1 1 calc R . . C120 C 0.2581(9) 0.13075(18) 0.3221(6) 0.052(3) Uani 1 1 d . . . H12A H 0.2080 0.1398 0.3274 0.062 Uiso 1 1 calc R . . C121 C 0.3499(8) 0.13696(16) 0.3035(5) 0.043(3) Uani 1 1 d . . . C122 C 0.3745(8) 0.15674(15) 0.2941(5) 0.039(3) Uani 1 1 d . . . C123 C 0.4692(7) 0.16096(15) 0.2757(5) 0.034(2) Uani 1 1 d . . . C124 C 0.3141(8) 0.17232(17) 0.2980(5) 0.045(3) Uani 1 1 d . . . H12B H 0.2504 0.1704 0.3106 0.054 Uiso 1 1 calc R . . C125 C 0.3430(7) 0.19081(16) 0.2842(5) 0.039(2) Uani 1 1 d . . . C126 C 0.4436(7) 0.19299(14) 0.2674(5) 0.032(2) Uani 1 1 d . . . C127 C 0.2846(9) 0.20770(19) 0.2847(7) 0.062(4) Uani 1 1 d . . . C128 C 0.1890(10) 0.2074(2) 0.3034(10) 0.096(6) Uani 1 1 d . . . H12C H 0.1611 0.1958 0.3158 0.115 Uiso 1 1 calc R . . C129 C 0.1377(13) 0.2236(2) 0.3038(12) 0.118(4) Uani 1 1 d U . . H12D H 0.0720 0.2234 0.3142 0.142 Uiso 1 1 calc R . . C130 C 0.1823(13) 0.2414(2) 0.2884(12) 0.122(4) Uani 1 1 d U . . H13A H 0.1475 0.2529 0.2915 0.147 Uiso 1 1 calc R . . C131 C 0.2727(12) 0.2417(2) 0.2696(11) 0.114(4) Uani 1 1 d U . . H13B H 0.2992 0.2532 0.2550 0.137 Uiso 1 1 calc R . . C132 C 0.3264(11) 0.2253(2) 0.2715(11) 0.101(4) Uani 1 1 d U . . C133 C 0.4236(9) 0.22516(16) 0.2543(6) 0.049(3) Uani 1 1 d . . . H13C H 0.4501 0.2371 0.2430 0.059 Uiso 1 1 calc R . . C134 C 0.8073(8) 0.13275(14) 0.2202(5) 0.037(2) Uani 1 1 d . . . H13D H 0.7689 0.1223 0.2316 0.044 Uiso 1 1 calc R . . C135 C 0.9008(8) 0.12880(15) 0.1988(5) 0.042(3) Uani 1 1 d . . . C136 C 0.9322(9) 0.10999(16) 0.1926(5) 0.050(3) Uani 1 1 d . . . H13E H 0.8904 0.0997 0.2002 0.060 Uiso 1 1 calc R . . C137 C 1.0264(10) 0.10676(17) 0.1750(6) 0.056(3) Uani 1 1 d . . . H13F H 1.0509 0.0942 0.1726 0.067 Uiso 1 1 calc R . . C138 C 1.0833(10) 0.1222(2) 0.1610(6) 0.066(4) Uani 1 1 d . . . H13G H 1.1465 0.1196 0.1484 0.079 Uiso 1 1 calc R . . C139 C 1.0556(9) 0.14076(18) 0.1640(6) 0.057(3) Uani 1 1 d . . . H13H H 1.0976 0.1509 0.1545 0.069 Uiso 1 1 calc R . . C140 C 0.9610(9) 0.14402(16) 0.1819(6) 0.048(3) Uani 1 1 d . . . C141 C 0.9195(8) 0.16357(17) 0.1872(6) 0.047(3) Uani 1 1 d . . . C142 C 0.8278(8) 0.16498(14) 0.2079(5) 0.037(2) Uani 1 1 d . . . C143 C 0.9647(9) 0.18014(17) 0.1711(7) 0.058(3) Uani 1 1 d . . . H14B H 1.0291 0.1798 0.1585 0.070 Uiso 1 1 calc R . . C144 C 0.9161(9) 0.19734(17) 0.1734(7) 0.057(3) Uani 1 1 d . . . C145 C 0.8249(8) 0.19778(15) 0.1981(5) 0.041(3) Uani 1 1 d . . . C146 C 0.9578(13) 0.2155(2) 0.1546(12) 0.119(4) Uani 1 1 d U . . C147 C 1.0399(13) 0.2171(2) 0.1253(12) 0.127(4) Uani 1 1 d U . . H14C H 1.0737 0.2063 0.1120 0.152 Uiso 1 1 calc R . . C148 C 1.0744(14) 0.2357(2) 0.1151(12) 0.130(4) Uani 1 1 d U . . H14D H 1.1391 0.2371 0.1036 0.156 Uiso 1 1 calc R . . C149 C 1.0215(13) 0.2517(2) 0.1205(11) 0.128(4) Uani 1 1 d U . . H14E H 1.0422 0.2636 0.1041 0.153 Uiso 1 1 calc RD . . C150 C 0.9365(13) 0.2503(2) 0.1506(11) 0.120(4) Uani 1 1 d U . . H15B H 0.9025 0.2614 0.1615 0.144 Uiso 1 1 calc R . . C151 C 0.9005(13) 0.2320(2) 0.1652(12) 0.116(3) Uani 1 1 d U . . C152 C 0.8106(11) 0.23042(19) 0.1901(10) 0.103(4) Uani 1 1 d U . . H15C H 0.7755 0.2417 0.1969 0.124 Uiso 1 1 calc R . . Cl1 Cl 0.55762(19) 0.07017(3) 0.88136(13) 0.0393(6) Uani 1 1 d . . . O1 O 0.4953(6) 0.05407(11) 0.8599(4) 0.058(2) Uani 1 1 d . . . O2 O 0.5531(7) 0.07497(12) 0.9538(4) 0.065(2) Uani 1 1 d . . . O3 O 0.5265(8) 0.08594(12) 0.8354(4) 0.087(3) Uani 1 1 d . . . O4 O 0.6585(6) 0.06534(14) 0.8773(6) 0.093(3) Uani 1 1 d . . . Cl2 Cl 0.1806(2) -0.08540(5) 0.40552(18) 0.0649(9) Uani 1 1 d . . . O5 O 0.2608(6) -0.09179(11) 0.3742(5) 0.062(2) Uani 1 1 d . . . O6 O 0.1424(9) -0.06832(14) 0.3784(5) 0.095(3) Uani 1 1 d . . . O7 O 0.0982(7) -0.09883(15) 0.3703(5) 0.087(3) Uani 1 1 d . . . O8 O 0.1854(9) -0.0905(2) 0.4757(5) 0.122(4) Uani 1 1 d . . . Cl3 Cl 0.2724(2) 0.17211(4) 0.09337(14) 0.0502(7) Uani 1 1 d . . . O9 O 0.2741(8) 0.16672(14) 0.0209(5) 0.090(3) Uani 1 1 d . . . O10 O 0.2883(11) 0.15590(15) 0.1376(5) 0.132(5) Uani 1 1 d . . . O11 O 0.3396(8) 0.18750(15) 0.1149(5) 0.090(3) Uani 1 1 d . . . O12 O 0.1759(8) 0.17856(17) 0.0994(8) 0.127(5) Uani 1 1 d . . . Cl4 Cl 0.5209(3) 0.32718(5) -0.1112(2) 0.0723(10) Uani 1 1 d . . . O13 O 0.5813(8) 0.33686(16) -0.1528(6) 0.104(4) Uani 1 1 d . . . O14 O 0.4544(9) 0.31412(18) -0.1515(7) 0.131(5) Uani 1 1 d . . . O15 O 0.5964(10) 0.31340(18) -0.0664(7) 0.136(5) Uani 1 1 d . . . O16 O 0.4959(10) 0.3375(2) -0.0534(7) 0.143(5) Uani 1 1 d . . . Cl5 Cl 0.3526(3) 0.20371(5) 0.74191(18) 0.0718(10) Uani 1 1 d . . . O17 O 0.3114(9) 0.22184(14) 0.7501(6) 0.104(4) Uani 1 1 d . . . O18 O 0.3735(14) 0.20086(19) 0.6766(6) 0.172(8) Uani 1 1 d . . . O19 O 0.4294(12) 0.2000(2) 0.7956(6) 0.155(6) Uani 1 1 d . . . O20 O 0.2820(13) 0.1891(2) 0.7529(15) 0.253(12) Uani 1 1 d . . . Cl6 Cl -0.0497(3) 0.21354(5) 0.7243(2) 0.0727(10) Uani 1 1 d . . . O21 O -0.0717(9) 0.19450(13) 0.7334(6) 0.098(4) Uani 1 1 d . . . O22 O 0.0578(9) 0.21493(17) 0.7189(8) 0.131(5) Uani 1 1 d . . . O23 O -0.0605(12) 0.22415(19) 0.7853(7) 0.150(6) Uani 1 1 d . . . O24 O -0.1099(10) 0.22047(16) 0.6665(6) 0.124(5) Uani 1 1 d . . . Cl7 Cl 0.8915(3) 0.04338(6) 0.25038(18) 0.0852(13) Uani 1 1 d . . . O25 O 0.8864(11) 0.03281(17) 0.1911(6) 0.126(5) Uani 1 1 d . . . O26 O 0.7800(10) 0.0373(2) 0.2646(9) 0.156(6) Uani 1 1 d . . . O27 O 0.8845(10) 0.06224(15) 0.2470(6) 0.118(4) Uani 1 1 d . . . O28 O 0.9464(8) 0.03696(15) 0.3140(5) 0.093(3) Uani 1 1 d . . . Cl8 Cl 0.4717(6) 0.03870(8) 0.2344(3) 0.139(3) Uani 1 1 d . . . O29 O 0.495(2) 0.0572(3) 0.2423(16) 0.38(2) Uani 1 1 d . . . O30 O 0.421(2) 0.0358(3) 0.2923(8) 0.242(12) Uani 1 1 d . . . O31 O 0.5384(16) 0.0238(3) 0.2371(11) 0.225(11) Uani 1 1 d . . . O32 O 0.4028(12) 0.0373(2) 0.1747(6) 0.145(6) Uani 1 1 d . . . N25 N 0.7200(9) 0.10685(17) 0.3510(6) 0.074(3) Uani 1 1 d . . . C153 C 0.7172(9) 0.0914(2) 0.3595(6) 0.052(3) Uani 1 1 d . . . C154 C 0.7169(12) 0.07086(18) 0.3716(8) 0.083(5) Uani 1 1 d . . . H15D H 0.7825 0.0656 0.3684 0.124 Uiso 1 1 calc R . . H15E H 0.6667 0.0649 0.3354 0.124 Uiso 1 1 calc R . . H15F H 0.7012 0.0683 0.4193 0.124 Uiso 1 1 calc R . . N26 N 0.1023(8) 0.14552(16) 0.6508(7) 0.073(3) Uani 1 1 d . . . C155 C 0.1000(9) 0.1605(2) 0.6342(6) 0.060(3) Uani 1 1 d . . . C156 C 0.0989(14) 0.18104(18) 0.6073(9) 0.097(6) Uani 1 1 d . . . H15G H 0.1671 0.1859 0.6133 0.146 Uiso 1 1 calc R . . H15H H 0.0597 0.1889 0.6348 0.146 Uiso 1 1 calc R . . H15I H 0.0690 0.1814 0.5566 0.146 Uiso 1 1 calc R . . N27 N 0.3689(11) 0.0097(2) 0.5376(9) 0.115(5) Uani 1 1 d DU . . C157 C 0.3939(12) -0.0067(3) 0.5391(10) 0.096(5) Uani 1 1 d DU . . C158 C 0.4236(13) -0.0269(3) 0.5442(10) 0.112(5) Uani 1 1 d DU . . H15J H 0.4898 -0.0283 0.5314 0.169 Uiso 1 1 calc R . . H15K H 0.3756 -0.0345 0.5115 0.169 Uiso 1 1 calc R . . H15L H 0.4250 -0.0314 0.5933 0.169 Uiso 1 1 calc R . . N28 N 0.2034(10) 0.14180(19) 0.8424(7) 0.084(4) Uiso 1 1 d . . . C159 C 0.1754(13) 0.1557(3) 0.8475(9) 0.091(5) Uiso 1 1 d . . . C160 C 0.141(2) 0.1756(4) 0.8535(15) 0.205(12) Uiso 1 1 d . . . H16B H 0.1960 0.1834 0.8776 0.308 Uiso 1 1 calc R . . H16C H 0.0864 0.1758 0.8812 0.308 Uiso 1 1 calc R . . H16D H 0.1174 0.1808 0.8056 0.308 Uiso 1 1 calc R . . N29 N 0.3006(10) 0.1097(2) 0.5311(7) 0.099(4) Uiso 1 1 d . . . C161 C 0.2853(11) 0.1254(2) 0.5180(8) 0.077(4) Uiso 1 1 d . . . C162 C 0.2651(13) 0.1444(2) 0.5016(9) 0.103(6) Uiso 1 1 d . . . H16E H 0.2004 0.1455 0.4704 0.155 Uiso 1 1 calc R . . H16F H 0.3168 0.1496 0.4770 0.155 Uiso 1 1 calc R . . H16G H 0.2639 0.1516 0.5457 0.155 Uiso 1 1 calc R . . N30 N 0.6244(9) 0.10458(18) 0.1637(7) 0.081(4) Uiso 1 1 d . . . C163 C 0.6376(12) 0.0899(2) 0.1483(8) 0.081(4) Uiso 1 1 d . . . C164 C 0.6489(15) 0.0691(3) 0.1271(11) 0.135(7) Uiso 1 1 d . . . H16H H 0.5912 0.0618 0.1364 0.203 Uiso 1 1 calc R . . H16I H 0.7095 0.0638 0.1553 0.203 Uiso 1 1 calc R . . H16J H 0.6531 0.0683 0.0761 0.203 Uiso 1 1 calc R . . N31 N 0.075(3) 0.0440(6) 0.941(2) 0.184(17) Uiso 0.50 1 d P . . C165 C 0.098(2) 0.0155(5) 0.9517(17) 0.087(9) Uiso 0.50 1 d P . . C166 C 0.106(3) -0.0010(5) 0.9644(19) 0.102(11) Uiso 0.50 1 d P . . H16K H 0.1674 -0.0033 0.9985 0.153 Uiso 0.50 1 calc PR . . H16L H 0.1091 -0.0080 0.9201 0.153 Uiso 0.50 1 calc PR . . H16M H 0.0490 -0.0053 0.9849 0.153 Uiso 0.50 1 calc PR . . N32 N -0.246(3) 0.2159(5) 1.0141(18) 0.126(11) Uiso 0.50 1 d PD . . C167 C -0.251(5) 0.2327(6) 1.001(3) 0.23(3) Uiso 0.50 1 d PD . . C168 C -0.247(4) 0.2534(6) 1.021(3) 0.168(19) Uiso 0.50 1 d PD . . H16N H -0.2296 0.2546 1.0734 0.253 Uiso 0.50 1 calc PR . . H16O H -0.3121 0.2592 1.0050 0.253 Uiso 0.50 1 calc PR . . H16P H -0.1967 0.2598 0.9986 0.253 Uiso 0.50 1 calc PR . . O33 O -0.1451(18) 0.1522(4) 0.9851(14) 0.280 Uiso 1 1 d D . . C169 C -0.066(2) 0.1809(3) 0.9510(19) 0.263 Uiso 1 1 d D . . H16Q H -0.0093 0.1731 0.9712 0.394 Uiso 1 1 calc R . . H16R H -0.0573 0.1939 0.9701 0.394 Uiso 1 1 calc RD . . H16S H -0.0721 0.1813 0.8988 0.394 Uiso 1 1 calc R . . C170 C -0.167(2) 0.1719(4) 0.9719(17) 0.226 Uiso 1 1 d D . . H171 H -0.1831 0.1781 1.0152 0.271 Uiso 1 1 calc R . . H172 H -0.2232 0.1735 0.9323 0.271 Uiso 1 1 calc R . . C171 C -0.207(3) 0.1366(4) 1.008(2) 0.295 Uiso 1 1 d D . . H173 H -0.2735 0.1388 0.9795 0.354 Uiso 1 1 calc R . . H174 H -0.2127 0.1400 1.0576 0.354 Uiso 1 1 calc R . . C172 C -0.197(2) 0.1144(4) 1.0104(17) 0.229 Uiso 1 1 d D . . H175 H -0.1764 0.1099 0.9664 0.343 Uiso 1 1 calc R . . H176 H -0.2617 0.1088 1.0146 0.343 Uiso 1 1 calc R . . H177 H -0.1478 0.1107 1.0516 0.343 Uiso 1 1 calc R . . O34 O 0.655(3) -0.0588(5) 0.5264(17) 0.216 Uiso 0.50 1 d PD . . C173 C 0.568(2) -0.0899(5) 0.5358(10) 0.220 Uiso 0.50 1 d PD . . H17B H 0.6323 -0.0947 0.5270 0.330 Uiso 0.50 1 calc PR . . H17C H 0.5144 -0.0963 0.5034 0.330 Uiso 0.50 1 calc PR . . H17D H 0.5610 -0.0926 0.5854 0.330 Uiso 0.50 1 calc PR . . C174 C 0.561(2) -0.0680(5) 0.522(2) 0.133 Uiso 0.50 1 d PD . . H17E H 0.5220 -0.0657 0.4742 0.160 Uiso 0.50 1 calc PR . . H17F H 0.5252 -0.0621 0.5577 0.160 Uiso 0.50 1 calc PR . . C175 C 0.709(3) -0.0500(6) 0.591(2) 0.156 Uiso 0.50 1 d PD . . H17G H 0.6506 -0.0455 0.6107 0.187 Uiso 0.50 1 calc PR . . H17H H 0.7314 -0.0386 0.5679 0.187 Uiso 0.50 1 calc PR . . C176 C 0.785(3) -0.0491(4) 0.661(2) 0.163 Uiso 0.50 1 d PD . . H17I H 0.7709 -0.0591 0.6933 0.244 Uiso 0.50 1 calc PR . . H17J H 0.7805 -0.0366 0.6834 0.244 Uiso 0.50 1 calc PR . . H17K H 0.8523 -0.0508 0.6500 0.244 Uiso 0.50 1 calc PR . . O35 O 0.4850(19) 0.2277(4) 0.4288(13) 0.126 Uiso 0.50 1 d PD . . C177 C 0.421(4) 0.2633(4) 0.444(3) 0.185 Uiso 0.50 1 d PD . . H17L H 0.3835 0.2648 0.3956 0.277 Uiso 0.50 1 calc PR . . H17M H 0.4555 0.2751 0.4596 0.277 Uiso 0.50 1 calc PR . . H17N H 0.3744 0.2601 0.4768 0.277 Uiso 0.50 1 calc PR . . C178 C 0.498(3) 0.2468(5) 0.4449(16) 0.200 Uiso 0.50 1 d PD . . H17O H 0.5436 0.2514 0.4133 0.240 Uiso 0.50 1 calc PR . . H17P H 0.5365 0.2471 0.4939 0.240 Uiso 0.50 1 calc PR . . C179 C 0.451(4) 0.2098(6) 0.451(3) 0.204 Uiso 0.50 1 d PD . . H17Q H 0.5098 0.2023 0.4443 0.245 Uiso 0.50 1 calc PR . . H17R H 0.4025 0.2072 0.4070 0.245 Uiso 0.50 1 calc PR . . C180 C 0.409(5) 0.1958(8) 0.500(3) 0.258 Uiso 0.50 1 d PD . . H18A H 0.4330 0.1993 0.5501 0.388 Uiso 0.50 1 calc PR . . H18B H 0.4308 0.1829 0.4912 0.388 Uiso 0.50 1 calc PR . . H18C H 0.3362 0.1964 0.4906 0.388 Uiso 0.50 1 calc PR . . O36 O 0.5222(12) 0.1400(2) 0.4619(9) 0.061(4) Uiso 0.50 1 d P . . O37 O 0.4470(16) -0.1118(3) 0.5128(12) 0.096(7) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0338(9) 0.0334(9) 0.0209(7) -0.0008(6) 0.0068(6) -0.0021(7) Co2 0.0310(9) 0.0347(9) 0.0222(8) -0.0008(7) 0.0066(6) -0.0015(7) Co3 0.0385(9) 0.0344(9) 0.0260(8) 0.0006(7) 0.0064(7) -0.0028(7) Co4 0.0367(9) 0.0330(9) 0.0272(8) 0.0001(7) 0.0081(7) -0.0024(7) N1 0.046(5) 0.036(5) 0.024(4) 0.003(3) 0.012(4) -0.006(4) N2 0.038(5) 0.042(5) 0.017(4) -0.001(3) 0.010(3) -0.003(4) N3 0.046(5) 0.040(5) 0.019(4) 0.001(3) 0.010(4) -0.005(4) N4 0.039(5) 0.035(5) 0.022(4) -0.003(3) 0.006(3) -0.005(4) N5 0.036(5) 0.037(5) 0.022(4) 0.007(3) 0.002(3) 0.003(4) N6 0.036(5) 0.042(5) 0.020(4) -0.002(3) 0.008(3) 0.003(4) N7 0.033(5) 0.039(5) 0.029(4) 0.002(4) 0.004(4) -0.003(4) N8 0.025(4) 0.034(5) 0.028(4) 0.001(3) 0.011(3) 0.000(3) N9 0.033(5) 0.044(5) 0.029(4) 0.004(4) 0.015(4) -0.004(4) N10 0.033(5) 0.032(4) 0.025(4) -0.003(3) 0.010(3) -0.003(4) N11 0.029(4) 0.031(4) 0.021(4) -0.001(3) 0.005(3) -0.001(3) N12 0.029(4) 0.036(5) 0.029(4) -0.001(4) 0.008(3) -0.002(4) N13 0.036(5) 0.036(5) 0.030(4) -0.003(4) 0.010(4) -0.003(4) N14 0.044(5) 0.023(4) 0.034(5) -0.001(3) 0.012(4) -0.002(4) N15 0.053(6) 0.033(5) 0.033(5) -0.001(4) 0.012(4) -0.008(4) N16 0.045(5) 0.031(5) 0.045(5) -0.003(4) 0.018(4) -0.004(4) N17 0.034(5) 0.039(5) 0.031(4) 0.002(4) 0.017(4) -0.002(4) N18 0.032(5) 0.039(5) 0.040(5) -0.003(4) 0.016(4) 0.001(4) N19 0.040(5) 0.041(5) 0.025(4) 0.003(4) 0.005(4) -0.005(4) N20 0.027(4) 0.041(5) 0.024(4) 0.003(3) -0.002(3) -0.004(4) N21 0.044(5) 0.039(5) 0.028(4) -0.001(4) 0.006(4) 0.003(4) N22 0.047(5) 0.039(5) 0.029(4) 0.009(4) 0.004(4) -0.007(4) N23 0.039(5) 0.044(5) 0.029(4) 0.000(4) 0.005(4) -0.002(4) N24 0.050(6) 0.040(5) 0.034(5) -0.001(4) 0.012(4) 0.000(4) C1 0.037(6) 0.052(7) 0.032(5) -0.002(5) 0.012(5) -0.004(5) C2 0.039(6) 0.048(7) 0.040(6) 0.002(5) 0.012(5) -0.015(5) C3 0.066(9) 0.052(7) 0.052(7) 0.000(6) 0.019(6) -0.008(6) C4 0.064(9) 0.071(9) 0.072(9) -0.003(7) 0.039(8) -0.023(7) C5 0.069(9) 0.072(9) 0.062(8) 0.000(7) 0.033(7) -0.023(7) C6 0.045(7) 0.058(7) 0.044(6) 0.002(5) 0.023(5) -0.012(6) C7 0.048(7) 0.054(7) 0.032(6) -0.002(5) 0.019(5) -0.008(5) C8 0.041(6) 0.034(6) 0.022(5) -0.003(4) 0.005(4) -0.003(5) C9 0.039(6) 0.037(6) 0.019(5) -0.005(4) 0.005(4) -0.008(5) C10 0.030(6) 0.063(7) 0.027(5) -0.002(5) 0.012(4) -0.011(5) C11 0.036(6) 0.049(6) 0.024(5) 0.002(4) 0.005(4) 0.005(5) C12 0.034(6) 0.043(6) 0.020(5) 0.006(4) 0.005(4) -0.001(5) C13 0.038(6) 0.060(7) 0.018(5) 0.004(4) 0.007(4) 0.005(5) C14 0.054(7) 0.057(7) 0.031(6) 0.007(5) 0.014(5) 0.015(6) C15 0.048(7) 0.078(9) 0.040(7) 0.011(6) 0.014(6) 0.022(7) C16 0.070(9) 0.056(8) 0.035(6) 0.006(5) 0.014(6) 0.026(7) C17 0.054(7) 0.056(7) 0.029(6) 0.007(5) 0.011(5) 0.008(6) C18 0.049(7) 0.040(6) 0.031(5) 0.002(4) 0.010(5) 0.012(5) C19 0.041(6) 0.047(7) 0.029(5) 0.005(5) -0.002(5) -0.002(5) C20 0.035(6) 0.033(6) 0.027(5) -0.003(4) 0.003(4) -0.003(4) C21 0.036(6) 0.042(6) 0.027(5) 0.003(4) 0.005(4) 0.009(5) C22 0.048(7) 0.037(6) 0.050(7) -0.005(5) 0.013(5) 0.005(5) C23 0.060(8) 0.056(8) 0.058(8) -0.001(6) 0.017(6) 0.014(6) C24 0.052(8) 0.051(8) 0.080(9) -0.003(6) 0.034(7) 0.004(6) C25 0.050(7) 0.045(7) 0.062(8) -0.004(6) 0.025(6) -0.002(6) C26 0.032(6) 0.041(6) 0.030(5) 0.000(4) 0.007(4) 0.005(5) C27 0.036(6) 0.038(6) 0.017(4) -0.004(4) 0.005(4) -0.002(4) C28 0.034(5) 0.030(5) 0.019(4) -0.005(4) 0.009(4) -0.002(4) C29 0.031(5) 0.048(6) 0.020(5) -0.004(4) 0.009(4) -0.005(5) C30 0.037(6) 0.039(6) 0.023(5) -0.003(4) 0.006(4) -0.005(5) C31 0.028(5) 0.041(6) 0.017(4) -0.002(4) 0.000(4) -0.005(4) C32 0.034(6) 0.036(6) 0.025(5) 0.002(4) -0.003(4) 0.001(4) C33 0.038(6) 0.049(7) 0.035(6) 0.001(5) 0.016(5) -0.010(5) C34 0.049(7) 0.054(8) 0.063(8) -0.002(6) 0.019(6) -0.017(6) C35 0.049(7) 0.046(7) 0.050(7) -0.003(5) 0.008(6) -0.009(6) C36 0.058(7) 0.041(6) 0.029(5) 0.004(5) -0.001(5) -0.001(5) C37 0.040(6) 0.037(6) 0.022(5) 0.001(4) 0.001(4) -0.004(5) C38 0.035(6) 0.033(6) 0.027(5) -0.009(4) 0.000(4) -0.001(4) C39 0.076(9) 0.043(7) 0.037(6) 0.001(5) 0.024(6) -0.007(6) C40 0.054(7) 0.045(6) 0.029(6) 0.009(5) 0.007(5) 0.004(5) C41 0.085(10) 0.040(7) 0.051(7) 0.005(6) 0.015(7) 0.008(6) C42 0.060(8) 0.062(8) 0.058(8) 0.025(7) 0.008(6) 0.013(7) C43 0.080(9) 0.059(8) 0.045(7) 0.017(6) 0.025(7) 0.022(7) C44 0.061(8) 0.066(8) 0.030(6) 0.013(5) 0.013(5) 0.019(6) C45 0.050(7) 0.048(6) 0.029(5) 0.007(5) 0.022(5) 0.003(5) C46 0.037(6) 0.049(6) 0.026(5) 0.006(5) 0.000(4) 0.007(5) C47 0.036(6) 0.049(6) 0.019(5) -0.002(4) 0.011(4) -0.009(5) C48 0.043(6) 0.058(7) 0.019(5) -0.008(5) 0.003(4) 0.003(5) C49 0.022(5) 0.052(6) 0.026(5) 0.001(4) 0.011(4) 0.007(4) C50 0.025(5) 0.049(6) 0.021(5) -0.005(4) 0.006(4) -0.002(4) C51 0.034(6) 0.058(7) 0.030(5) -0.009(5) 0.004(4) -0.007(5) C52 0.071(9) 0.066(8) 0.037(6) -0.012(6) 0.014(6) 0.003(7) C53 0.065(8) 0.070(9) 0.028(6) -0.019(6) -0.006(5) 0.007(7) C54 0.076(9) 0.059(8) 0.039(7) -0.027(6) 0.011(6) -0.006(7) C55 0.054(7) 0.043(7) 0.046(7) -0.013(5) 0.009(6) 0.001(5) C56 0.029(5) 0.054(7) 0.028(5) -0.011(5) 0.002(4) -0.005(5) C57 0.041(6) 0.048(6) 0.024(5) -0.010(5) 0.002(4) -0.008(5) C58 0.035(6) 0.037(6) 0.035(5) -0.002(4) 0.009(4) -0.007(5) C59 0.027(5) 0.040(6) 0.044(6) -0.015(5) 0.014(5) -0.004(4) C60 0.042(6) 0.044(7) 0.055(7) -0.014(5) 0.021(5) -0.002(5) C61 0.039(6) 0.048(7) 0.055(7) -0.020(6) 0.022(5) -0.004(5) C62 0.029(6) 0.068(8) 0.050(7) -0.028(6) 0.007(5) 0.001(5) C63 0.035(6) 0.061(7) 0.031(5) -0.013(5) 0.014(5) 0.005(5) C64 0.026(5) 0.045(6) 0.045(6) -0.012(5) 0.016(5) -0.007(5) C65 0.027(5) 0.040(6) 0.032(5) -0.014(4) 0.010(4) 0.000(4) C66 0.020(5) 0.042(6) 0.025(5) -0.001(4) 0.007(4) -0.005(4) C67 0.028(5) 0.054(7) 0.017(5) -0.003(4) 0.002(4) -0.006(5) C68 0.025(5) 0.047(6) 0.019(4) 0.000(4) 0.005(4) -0.002(4) C69 0.021(5) 0.039(6) 0.026(5) -0.001(4) 0.007(4) -0.008(4) C70 0.030(5) 0.044(6) 0.025(5) 0.000(4) 0.006(4) -0.001(4) C71 0.042(6) 0.061(7) 0.022(5) 0.003(5) 0.002(4) -0.004(5) C72 0.056(7) 0.071(8) 0.020(5) 0.012(5) -0.010(5) -0.006(6) C73 0.040(7) 0.062(8) 0.047(7) 0.022(6) -0.001(5) -0.005(6) C74 0.037(6) 0.041(6) 0.047(6) 0.006(5) 0.009(5) -0.004(5) C75 0.019(5) 0.053(6) 0.028(5) 0.008(5) 0.007(4) -0.006(4) C76 0.024(5) 0.039(6) 0.030(5) -0.007(4) 0.010(4) -0.002(4) C77 0.030(5) 0.030(5) 0.042(6) 0.001(4) 0.011(5) -0.004(4) C78 0.033(6) 0.043(6) 0.029(5) 0.004(4) 0.007(4) -0.005(5) C79 0.032(6) 0.038(6) 0.051(7) 0.011(5) 0.007(5) -0.006(5) C80 0.072(9) 0.038(7) 0.055(7) 0.017(6) 0.005(6) 0.010(6) C81 0.061(8) 0.049(7) 0.026(5) 0.008(5) -0.014(5) -0.011(6) C82 0.058(8) 0.040(6) 0.048(7) 0.001(5) 0.010(6) -0.002(5) C83 0.037(6) 0.039(6) 0.025(5) 0.011(4) -0.007(4) -0.003(4) C84 0.039(6) 0.035(6) 0.035(6) 0.004(4) 0.008(5) 0.003(5) C85 0.032(5) 0.038(6) 0.021(5) 0.006(4) 0.005(4) -0.004(4) C86 0.044(6) 0.040(6) 0.027(5) 0.003(4) 0.000(5) -0.004(5) C87 0.047(7) 0.039(6) 0.040(6) -0.001(5) 0.010(5) -0.005(5) C88 0.032(6) 0.033(6) 0.032(5) 0.002(4) 0.003(4) -0.005(4) C89 0.042(6) 0.033(6) 0.043(6) -0.005(5) 0.005(5) 0.002(5) C90 0.053(7) 0.039(6) 0.034(6) -0.005(5) 0.005(5) -0.001(5) C91 0.050(7) 0.052(7) 0.048(7) -0.007(6) 0.018(6) -0.001(6) C92 0.065(8) 0.032(6) 0.074(9) -0.016(6) 0.011(7) -0.005(6) C93 0.056(7) 0.037(6) 0.048(7) -0.002(5) 0.003(6) 0.003(5) C94 0.054(7) 0.034(6) 0.045(6) -0.006(5) 0.008(5) 0.000(5) C95 0.054(7) 0.033(6) 0.049(7) 0.007(5) 0.016(6) 0.000(5) C96 0.049(7) 0.040(6) 0.032(5) 0.004(5) 0.009(5) 0.003(5) C97 0.031(6) 0.047(6) 0.037(6) -0.005(5) 0.006(5) -0.002(5) C98 0.051(7) 0.046(7) 0.041(6) -0.003(5) 0.001(5) -0.005(5) C99 0.059(8) 0.046(7) 0.043(7) -0.016(5) 0.006(6) -0.003(6) C100 0.060(8) 0.088(10) 0.034(6) -0.017(7) -0.007(6) 0.003(7) C101 0.052(7) 0.047(7) 0.033(6) -0.002(5) -0.009(5) 0.003(5) C102 0.037(6) 0.047(6) 0.035(6) -0.006(5) 0.008(5) 0.001(5) C103 0.030(6) 0.043(6) 0.033(5) -0.004(5) 0.013(4) -0.001(5) C104 0.028(5) 0.041(6) 0.030(5) -0.008(4) 0.005(4) 0.000(4) C105 0.035(6) 0.044(6) 0.030(5) 0.000(5) 0.011(4) 0.000(5) C106 0.031(6) 0.044(6) 0.029(5) 0.011(4) 0.002(4) -0.005(5) C107 0.035(6) 0.040(6) 0.026(5) 0.004(4) 0.009(4) -0.002(5) C108 0.036(6) 0.041(6) 0.033(5) 0.004(5) 0.004(5) -0.001(5) C109 0.052(7) 0.049(7) 0.027(5) 0.011(5) -0.001(5) -0.005(5) C110 0.050(7) 0.061(8) 0.052(7) 0.019(6) -0.002(6) -0.009(6) C111 0.082(10) 0.051(8) 0.046(7) 0.018(6) -0.006(7) -0.015(7) C112 0.064(8) 0.042(7) 0.059(8) 0.013(6) -0.003(6) -0.005(6) C113 0.036(6) 0.040(6) 0.037(6) 0.010(5) -0.003(5) -0.007(5) C114 0.043(6) 0.038(6) 0.042(6) 0.005(5) 0.010(5) -0.002(5) C115 0.044(7) 0.041(6) 0.039(6) -0.001(5) 0.005(5) -0.006(5) C116 0.055(7) 0.045(7) 0.031(6) 0.007(5) 0.006(5) -0.013(6) C117 0.074(9) 0.049(7) 0.034(6) 0.001(5) 0.001(6) -0.025(6) C118 0.075(9) 0.066(9) 0.035(6) 0.013(6) 0.001(6) -0.029(8) C119 0.057(9) 0.086(10) 0.049(8) 0.023(7) 0.002(6) -0.024(8) C120 0.050(7) 0.064(8) 0.038(6) 0.007(6) -0.003(5) -0.022(6) C121 0.049(7) 0.061(7) 0.018(5) -0.002(5) 0.002(5) -0.018(6) C122 0.039(6) 0.051(7) 0.028(5) 0.003(5) 0.009(5) -0.016(5) C123 0.034(6) 0.048(6) 0.017(4) 0.000(4) -0.008(4) -0.007(5) C124 0.028(6) 0.082(9) 0.028(5) 0.004(5) 0.012(4) -0.005(6) C125 0.029(6) 0.054(7) 0.036(6) -0.001(5) 0.009(5) -0.006(5) C126 0.030(5) 0.046(6) 0.020(5) -0.002(4) 0.005(4) 0.005(5) C127 0.046(8) 0.073(9) 0.078(9) -0.007(7) 0.039(7) 0.009(6) C128 0.057(9) 0.056(9) 0.192(19) 0.004(10) 0.073(11) 0.004(7) C129 0.084(7) 0.068(6) 0.222(11) 0.002(7) 0.086(8) 0.001(6) C130 0.088(7) 0.072(7) 0.225(11) -0.001(7) 0.079(8) 0.007(6) C131 0.082(7) 0.066(6) 0.215(11) 0.000(7) 0.085(8) 0.002(6) C132 0.071(7) 0.054(6) 0.202(11) -0.003(7) 0.090(7) 0.003(5) C133 0.064(8) 0.043(7) 0.042(6) -0.012(5) 0.017(6) -0.006(6) C134 0.043(6) 0.037(6) 0.029(5) -0.005(4) 0.004(5) -0.001(5) C135 0.058(7) 0.045(6) 0.023(5) 0.004(4) 0.004(5) 0.014(5) C136 0.073(9) 0.051(7) 0.024(5) 0.002(5) -0.001(5) 0.014(6) C137 0.081(10) 0.047(7) 0.046(7) 0.006(6) 0.025(7) 0.022(7) C138 0.060(9) 0.090(11) 0.047(7) 0.003(7) 0.010(6) 0.029(8) C139 0.046(7) 0.068(9) 0.061(8) 0.006(6) 0.019(6) 0.019(6) C140 0.055(7) 0.052(7) 0.039(6) 0.002(5) 0.015(5) 0.003(6) C141 0.043(7) 0.061(8) 0.037(6) 0.013(5) 0.008(5) 0.014(6) C142 0.040(6) 0.041(6) 0.029(5) 0.002(4) 0.008(4) 0.004(5) C143 0.044(7) 0.050(7) 0.083(9) 0.012(7) 0.022(7) -0.002(6) C144 0.042(7) 0.057(8) 0.081(9) -0.002(7) 0.038(7) 0.000(6) C145 0.040(6) 0.047(7) 0.035(6) 0.005(5) 0.005(5) -0.001(5) C146 0.104(6) 0.059(5) 0.225(9) 0.022(6) 0.119(7) 0.000(5) C147 0.108(7) 0.066(5) 0.238(10) 0.021(6) 0.123(7) 0.003(5) C148 0.111(7) 0.070(5) 0.240(9) 0.023(6) 0.118(7) -0.001(5) C149 0.110(7) 0.066(5) 0.237(9) 0.023(6) 0.120(7) -0.001(5) C150 0.106(6) 0.060(5) 0.226(9) 0.025(6) 0.118(7) -0.002(5) C151 0.102(6) 0.055(5) 0.223(9) 0.022(6) 0.118(7) 0.000(5) C152 0.096(7) 0.045(5) 0.201(10) 0.017(6) 0.116(7) -0.001(5) Cl1 0.0468(15) 0.0387(14) 0.0330(13) 0.0038(10) 0.0081(11) 0.0064(11) O1 0.063(6) 0.054(5) 0.056(5) -0.001(4) 0.002(4) -0.012(4) O2 0.097(7) 0.071(6) 0.027(4) -0.001(4) 0.004(4) -0.010(5) O3 0.157(10) 0.047(5) 0.047(5) 0.008(4) -0.011(6) 0.025(6) O4 0.045(6) 0.086(7) 0.159(10) -0.012(7) 0.054(6) -0.005(5) Cl2 0.060(2) 0.075(2) 0.070(2) 0.0274(17) 0.0379(17) 0.0178(17) O5 0.054(5) 0.059(5) 0.079(6) -0.007(5) 0.028(5) 0.004(4) O6 0.143(10) 0.070(6) 0.069(7) -0.006(5) 0.008(6) 0.044(7) O7 0.068(7) 0.105(8) 0.082(7) 0.000(6) -0.003(5) -0.026(6) O8 0.103(9) 0.206(14) 0.052(6) -0.001(8) 0.003(6) 0.023(9) Cl3 0.0609(18) 0.0523(17) 0.0396(14) 0.0116(12) 0.0151(13) 0.0176(14) O9 0.130(9) 0.090(7) 0.051(6) -0.012(5) 0.021(6) -0.017(6) O10 0.257(16) 0.078(7) 0.050(6) 0.025(5) -0.005(8) 0.059(9) O11 0.092(8) 0.119(9) 0.054(6) 0.000(6) -0.003(5) -0.042(7) O12 0.071(7) 0.115(9) 0.217(14) -0.003(9) 0.084(9) 0.007(7) Cl4 0.069(2) 0.061(2) 0.097(3) -0.0005(19) 0.041(2) -0.0005(17) O13 0.095(8) 0.120(9) 0.112(9) 0.001(7) 0.056(7) -0.021(7) O14 0.117(10) 0.127(10) 0.121(10) 0.069(8) -0.064(8) -0.057(8) O15 0.141(12) 0.123(10) 0.125(11) 0.006(8) -0.035(9) 0.059(9) O16 0.127(11) 0.216(15) 0.103(10) 0.005(10) 0.070(9) 0.000(10) Cl5 0.091(3) 0.065(2) 0.057(2) -0.0096(16) 0.0043(18) 0.0111(19) O17 0.135(10) 0.064(7) 0.120(9) 0.007(6) 0.042(8) 0.019(7) O18 0.33(2) 0.132(11) 0.065(8) 0.008(7) 0.065(11) 0.125(13) O19 0.201(15) 0.167(13) 0.066(8) -0.028(8) -0.069(9) 0.068(11) O20 0.141(15) 0.135(14) 0.50(4) 0.019(18) 0.09(2) -0.052(12) Cl6 0.086(3) 0.060(2) 0.069(2) -0.0144(17) 0.0034(19) -0.0055(18) O21 0.131(10) 0.061(6) 0.088(8) 0.003(5) -0.025(7) -0.026(6) O22 0.079(8) 0.103(9) 0.214(15) -0.054(9) 0.033(9) -0.014(7) O23 0.218(16) 0.116(10) 0.101(10) -0.053(8) -0.015(10) 0.044(10) O24 0.151(11) 0.096(8) 0.094(8) 0.015(7) -0.069(8) -0.021(8) Cl7 0.114(3) 0.077(3) 0.052(2) -0.0220(18) -0.021(2) 0.042(2) O25 0.176(13) 0.110(9) 0.082(8) -0.040(7) -0.011(8) -0.007(9) O26 0.084(9) 0.146(12) 0.239(18) -0.028(12) 0.028(10) -0.022(9) O27 0.179(13) 0.072(8) 0.097(9) 0.014(6) 0.002(8) -0.035(8) O28 0.099(8) 0.107(8) 0.061(6) 0.025(6) -0.020(5) -0.035(6) Cl8 0.244(8) 0.097(4) 0.062(3) 0.014(3) -0.016(4) -0.060(4) O29 0.41(4) 0.129(15) 0.48(4) 0.13(2) -0.28(3) -0.14(2) O30 0.45(3) 0.196(18) 0.087(11) 0.027(12) 0.053(16) 0.14(2) O31 0.24(2) 0.24(2) 0.23(2) 0.144(18) 0.158(18) 0.075(18) O32 0.197(15) 0.153(12) 0.068(8) -0.016(8) -0.028(9) -0.036(11) N25 0.079(9) 0.065(8) 0.072(8) 0.029(6) -0.007(6) 0.000(7) C153 0.054(8) 0.065(9) 0.037(6) 0.005(6) 0.004(5) -0.002(7) C154 0.105(12) 0.049(8) 0.087(11) -0.009(8) -0.006(9) -0.008(8) N26 0.062(8) 0.053(7) 0.095(9) 0.015(7) -0.013(6) -0.001(6) C155 0.057(8) 0.080(10) 0.039(7) -0.005(7) -0.006(6) 0.007(7) C156 0.155(17) 0.043(8) 0.096(12) -0.012(8) 0.028(11) -0.007(9) N27 0.071(9) 0.135(12) 0.126(10) -0.001(11) -0.016(8) -0.003(9) C157 0.055(9) 0.129(13) 0.103(10) 0.004(12) 0.008(8) -0.009(10) C158 0.079(10) 0.130(12) 0.121(11) 0.011(11) -0.004(9) 0.005(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N7 2.094(8) . ? Co1 N4 2.122(8) . ? Co1 N10 2.137(7) . ? Co1 N1 2.135(8) . ? Co1 N8 2.204(8) . ? Co1 N11 2.226(7) . ? Co2 N3 2.124(8) . ? Co2 N6 2.139(8) . ? Co2 N9 2.152(8) . ? Co2 N12 2.158(8) . ? Co2 N5 2.242(8) . ? Co2 N2 2.276(8) . ? Co3 N13 2.118(8) . ? Co3 N19 2.123(8) . ? Co3 N22 2.128(9) . ? Co3 N16 2.142(9) . ? Co3 N20 2.249(8) . ? Co3 N23 2.254(8) . ? Co4 N15 2.096(8) . ? Co4 N21 2.130(8) . ? Co4 N24 2.138(9) . ? Co4 N18 2.143(8) . ? Co4 N17 2.213(8) . ? Co4 N14 2.220(8) . ? N1 C1 1.274(12) . ? N1 C9 1.373(12) . ? N2 C12 1.333(12) . ? N2 C9 1.334(11) . ? N3 C19 1.293(12) . ? N3 C12 1.387(12) . ? N4 C20 1.314(12) . ? N4 C28 1.377(11) . ? N5 C28 1.327(11) . ? N5 C31 1.357(11) . ? N6 C38 1.298(11) . ? N6 C31 1.388(12) . ? N7 C39 1.309(13) . ? N7 C47 1.367(11) . ? N8 C50 1.325(11) . ? N8 C47 1.339(12) . ? N9 C57 1.286(12) . ? N9 C50 1.388(12) . ? N10 C58 1.314(12) . ? N10 C66 1.368(11) . ? N11 C69 1.317(11) . ? N11 C66 1.355(11) . ? N12 C76 1.319(11) . ? N12 C69 1.367(11) . ? N13 C77 1.320(11) . ? N13 C85 1.391(12) . ? N14 C88 1.333(11) . ? N14 C85 1.361(11) . ? N15 C95 1.283(12) . ? N15 C88 1.403(12) . ? N16 C96 1.277(12) . ? N16 C104 1.386(12) . ? N17 C107 1.325(12) . ? N17 C104 1.349(12) . ? N18 C114 1.302(12) . ? N18 C107 1.382(12) . ? N19 C115 1.291(12) . ? N19 C123 1.394(12) . ? N20 C126 1.320(12) . ? N20 C123 1.329(12) . ? N21 C133 1.278(13) . ? N21 C126 1.373(12) . ? N22 C134 1.293(12) . ? N22 C142 1.395(12) . ? N23 C145 1.352(13) . ? N23 C142 1.357(12) . ? N24 C152 1.291(14) . ? N24 C145 1.384(13) . ? C1 C2 1.442(13) . ? C2 C7 1.424(15) . ? C2 C3 1.439(15) . ? C3 C4 1.341(16) . ? C4 C5 1.415(17) . ? C5 C6 1.405(15) . ? C6 C7 1.427(14) . ? C7 C8 1.408(14) . ? C8 C10 1.381(14) . ? C8 C9 1.439(13) . ? C10 C11 1.398(14) . ? C11 C12 1.402(13) . ? C11 C13 1.430(14) . ? C13 C14 1.397(14) . ? C13 C18 1.412(14) . ? C14 C15 1.377(15) . ? C15 C16 1.390(16) . ? C16 C17 1.365(15) . ? C17 C18 1.384(14) . ? C18 C19 1.466(14) . ? C20 C21 1.448(13) . ? C21 C22 1.372(13) . ? C21 C26 1.398(13) . ? C22 C23 1.375(15) . ? C23 C24 1.428(16) . ? C24 C25 1.350(15) . ? C25 C26 1.419(14) . ? C26 C27 1.443(13) . ? C27 C29 1.387(13) . ? C27 C28 1.431(13) . ? C29 C30 1.393(13) . ? C30 C31 1.385(13) . ? C30 C32 1.450(13) . ? C32 C33 1.400(13) . ? C32 C37 1.444(13) . ? C33 C34 1.365(14) . ? C34 C35 1.390(15) . ? C35 C36 1.406(15) . ? C36 C37 1.392(13) . ? C37 C38 1.416(13) . ? C39 C40 1.433(14) . ? C40 C41 1.387(14) . ? C40 C45 1.416(14) . ? C41 C42 1.361(16) . ? C42 C43 1.416(17) . ? C43 C44 1.363(15) . ? C44 C45 1.378(14) . ? C45 C46 1.468(14) . ? C46 C48 1.400(13) . ? C46 C47 1.411(12) . ? C48 C49 1.382(13) . ? C49 C51 1.425(14) . ? C49 C50 1.459(12) . ? C51 C56 1.393(14) . ? C51 C52 1.410(14) . ? C52 C53 1.367(15) . ? C53 C54 1.387(16) . ? C54 C55 1.345(15) . ? C55 C56 1.403(13) . ? C56 C57 1.471(13) . ? C58 C59 1.452(13) . ? C59 C64 1.398(14) . ? C59 C60 1.414(13) . ? C60 C61 1.386(14) . ? C61 C62 1.426(15) . ? C62 C63 1.373(14) . ? C63 C64 1.414(13) . ? C64 C65 1.454(13) . ? C65 C67 1.376(13) . ? C65 C66 1.408(12) . ? C67 C68 1.386(13) . ? C68 C70 1.434(13) . ? C68 C69 1.444(12) . ? C70 C75 1.414(13) . ? C70 C71 1.413(12) . ? C71 C72 1.390(15) . ? C72 C73 1.380(16) . ? C73 C74 1.374(14) . ? C74 C75 1.390(13) . ? C75 C76 1.408(12) . ? C77 C78 1.427(13) . ? C78 C79 1.404(13) . ? C78 C83 1.415(13) . ? C79 C80 1.367(15) . ? C80 C81 1.394(15) . ? C81 C82 1.387(14) . ? C82 C83 1.421(14) . ? C83 C84 1.452(13) . ? C84 C86 1.399(13) . ? C84 C85 1.411(13) . ? C86 C87 1.397(13) . ? C87 C88 1.390(13) . ? C87 C89 1.475(14) . ? C89 C90 1.398(14) . ? C89 C94 1.407(14) . ? C90 C91 1.370(14) . ? C91 C92 1.388(16) . ? C92 C93 1.382(15) . ? C93 C94 1.395(14) . ? C94 C95 1.458(14) . ? C96 C97 1.428(13) . ? C97 C98 1.385(14) . ? C97 C102 1.402(14) . ? C98 C99 1.381(14) . ? C99 C100 1.378(16) . ? C100 C101 1.372(15) . ? C101 C102 1.378(13) . ? C102 C103 1.477(13) . ? C103 C105 1.370(13) . ? C103 C104 1.412(13) . ? C105 C106 1.374(13) . ? C106 C107 1.398(13) . ? C106 C108 1.489(13) . ? C108 C113 1.383(14) . ? C108 C109 1.401(13) . ? C109 C110 1.395(15) . ? C110 C111 1.366(16) . ? C111 C112 1.394(15) . ? C112 C113 1.433(14) . ? C113 C114 1.441(14) . ? C115 C116 1.472(14) . ? C116 C121 1.374(15) . ? C116 C117 1.405(14) . ? C117 C118 1.373(16) . ? C118 C119 1.385(18) . ? C119 C120 1.339(16) . ? C120 C121 1.426(15) . ? C121 C122 1.449(14) . ? C122 C124 1.381(15) . ? C122 C123 1.426(13) . ? C124 C125 1.397(15) . ? C125 C127 1.431(15) . ? C125 C126 1.469(13) . ? C127 C132 1.402(17) . ? C127 C128 1.409(16) . ? C128 C129 1.339(19) . ? C129 C130 1.44(2) . ? C130 C131 1.341(19) . ? C131 C132 1.361(19) . ? C132 C133 1.420(16) . ? C134 C135 1.431(14) . ? C135 C136 1.401(14) . ? C135 C140 1.419(15) . ? C136 C137 1.402(16) . ? C137 C138 1.386(17) . ? C138 C139 1.363(17) . ? C139 C140 1.409(15) . ? C140 C141 1.496(15) . ? C141 C142 1.378(14) . ? C141 C143 1.376(15) . ? C143 C144 1.383(16) . ? C144 C145 1.402(14) . ? C144 C146 1.465(17) . ? C146 C147 1.337(18) . ? C146 C151 1.434(19) . ? C147 C148 1.42(2) . ? C148 C149 1.35(2) . ? C149 C150 1.381(19) . ? C150 C151 1.421(18) . ? C151 C152 1.392(17) . ? Cl1 O2 1.427(7) . ? Cl1 O3 1.431(8) . ? Cl1 O4 1.434(8) . ? Cl1 O1 1.433(8) . ? Cl2 O8 1.369(11) . ? Cl2 O6 1.374(9) . ? Cl2 O5 1.404(8) . ? Cl2 O7 1.534(9) . ? Cl3 O10 1.410(9) . ? Cl3 O12 1.416(10) . ? Cl3 O9 1.431(9) . ? Cl3 O11 1.433(9) . ? Cl4 O16 1.404(13) . ? Cl4 O13 1.409(10) . ? Cl4 O14 1.421(11) . ? Cl4 O15 1.558(11) . ? Cl5 O18 1.332(11) . ? Cl5 O19 1.357(11) . ? Cl5 O17 1.413(10) . ? Cl5 O20 1.445(15) . ? Cl6 O24 1.345(10) . ? Cl6 O21 1.389(9) . ? Cl6 O23 1.405(11) . ? Cl6 O22 1.492(12) . ? Cl7 O27 1.330(11) . ? Cl7 O25 1.340(11) . ? Cl7 O28 1.385(9) . ? Cl7 O26 1.646(13) . ? Cl8 O29 1.343(17) . ? Cl8 O32 1.349(12) . ? Cl8 O31 1.383(18) . ? Cl8 O30 1.41(2) . ? N25 C153 1.099(14) . ? C153 C154 1.464(18) . ? N26 C155 1.102(15) . ? C155 C156 1.528(19) . ? N27 C157 1.20(2) . ? C157 C158 1.48(2) . ? N28 C159 1.060(18) . ? C159 C160 1.49(3) . ? N29 C161 1.147(17) . ? C161 C162 1.39(2) . ? N30 C163 1.097(16) . ? C163 C164 1.53(2) . ? C165 C166 1.19(4) . ? N32 C167 1.21(3) . ? C167 C168 1.50(3) . ? O33 C170 1.43(2) . ? O33 C171 1.49(2) . ? C169 C170 1.62(2) . ? C171 C172 1.56(2) . ? O34 C174 1.420(16) . ? O34 C175 1.456(17) . ? C173 C174 1.565(17) . ? C175 C176 1.542(17) . ? O35 C178 1.38(2) . ? O35 C179 1.43(2) . ? C177 C178 1.56(2) . ? C179 C180 1.53(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Co1 N4 91.4(3) . . ? N7 Co1 N10 104.0(3) . . ? N4 Co1 N10 91.0(3) . . ? N7 Co1 N1 90.8(3) . . ? N4 Co1 N1 175.4(3) . . ? N10 Co1 N1 92.3(3) . . ? N7 Co1 N8 62.3(3) . . ? N4 Co1 N8 88.9(3) . . ? N10 Co1 N8 166.2(3) . . ? N1 Co1 N8 88.6(3) . . ? N7 Co1 N11 166.0(3) . . ? N4 Co1 N11 88.1(3) . . ? N10 Co1 N11 62.1(3) . . ? N1 Co1 N11 90.7(3) . . ? N8 Co1 N11 131.7(3) . . ? N3 Co2 N6 107.7(3) . . ? N3 Co2 N9 92.9(3) . . ? N6 Co2 N9 94.0(3) . . ? N3 Co2 N12 91.5(3) . . ? N6 Co2 N12 90.2(3) . . ? N9 Co2 N12 172.6(3) . . ? N3 Co2 N5 169.3(3) . . ? N6 Co2 N5 61.7(3) . . ? N9 Co2 N5 89.9(3) . . ? N12 Co2 N5 86.8(3) . . ? N3 Co2 N2 61.1(3) . . ? N6 Co2 N2 168.7(3) . . ? N9 Co2 N2 88.4(3) . . ? N12 Co2 N2 88.6(3) . . ? N5 Co2 N2 129.4(3) . . ? N13 Co3 N19 91.9(3) . . ? N13 Co3 N22 93.5(3) . . ? N19 Co3 N22 107.1(3) . . ? N13 Co3 N16 173.8(3) . . ? N19 Co3 N16 91.5(3) . . ? N22 Co3 N16 90.5(3) . . ? N13 Co3 N20 88.9(3) . . ? N19 Co3 N20 62.1(3) . . ? N22 Co3 N20 169.0(3) . . ? N16 Co3 N20 88.1(3) . . ? N13 Co3 N23 90.2(3) . . ? N19 Co3 N23 169.1(3) . . ? N22 Co3 N23 62.1(3) . . ? N16 Co3 N23 87.4(3) . . ? N20 Co3 N23 128.7(3) . . ? N15 Co4 N21 92.1(3) . . ? N15 Co4 N24 91.3(3) . . ? N21 Co4 N24 175.7(3) . . ? N15 Co4 N18 105.6(3) . . ? N21 Co4 N18 92.9(3) . . ? N24 Co4 N18 88.7(3) . . ? N15 Co4 N17 167.1(3) . . ? N21 Co4 N17 89.0(3) . . ? N24 Co4 N17 88.3(3) . . ? N18 Co4 N17 61.5(3) . . ? N15 Co4 N14 62.4(3) . . ? N21 Co4 N14 89.6(3) . . ? N24 Co4 N14 89.6(3) . . ? N18 Co4 N14 167.8(3) . . ? N17 Co4 N14 130.5(3) . . ? C1 N1 C9 118.5(9) . . ? C1 N1 Co1 120.1(7) . . ? C9 N1 Co1 121.4(6) . . ? C12 N2 C9 118.4(8) . . ? C12 N2 Co2 91.4(6) . . ? C9 N2 Co2 150.1(7) . . ? C19 N3 C12 118.3(9) . . ? C19 N3 Co2 145.2(7) . . ? C12 N3 Co2 96.6(6) . . ? C20 N4 C28 118.4(8) . . ? C20 N4 Co1 119.4(6) . . ? C28 N4 Co1 122.0(6) . . ? C28 N5 C31 117.4(8) . . ? C28 N5 Co2 150.2(7) . . ? C31 N5 Co2 92.3(6) . . ? C38 N6 C31 118.0(8) . . ? C38 N6 Co2 146.1(7) . . ? C31 N6 Co2 95.9(6) . . ? C39 N7 C47 117.9(9) . . ? C39 N7 Co1 146.5(7) . . ? C47 N7 Co1 95.6(6) . . ? C50 N8 C47 118.2(8) . . ? C50 N8 Co1 150.3(7) . . ? C47 N8 Co1 91.5(6) . . ? C57 N9 C50 120.4(9) . . ? C57 N9 Co2 118.2(7) . . ? C50 N9 Co2 121.3(6) . . ? C58 N10 C66 119.2(8) . . ? C58 N10 Co1 145.9(7) . . ? C66 N10 Co1 94.8(5) . . ? C69 N11 C66 119.2(8) . . ? C69 N11 Co1 149.4(6) . . ? C66 N11 Co1 91.3(5) . . ? C76 N12 C69 119.6(8) . . ? C76 N12 Co2 118.9(6) . . ? C69 N12 Co2 121.5(6) . . ? C77 N13 C85 117.6(8) . . ? C77 N13 Co3 120.2(6) . . ? C85 N13 Co3 122.2(6) . . ? C88 N14 C85 115.6(8) . . ? C88 N14 Co4 92.3(6) . . ? C85 N14 Co4 152.1(6) . . ? C95 N15 C88 117.8(9) . . ? C95 N15 Co4 146.4(8) . . ? C88 N15 Co4 95.7(6) . . ? C96 N16 C104 118.1(9) . . ? C96 N16 Co3 119.5(7) . . ? C104 N16 Co3 122.4(6) . . ? C107 N17 C104 118.1(9) . . ? C107 N17 Co4 93.1(6) . . ? C104 N17 Co4 148.8(7) . . ? C114 N18 C107 118.0(9) . . ? C114 N18 Co4 147.4(7) . . ? C107 N18 Co4 94.5(6) . . ? C115 N19 C123 118.6(9) . . ? C115 N19 Co3 146.6(8) . . ? C123 N19 Co3 94.8(6) . . ? C126 N20 C123 118.8(9) . . ? C126 N20 Co3 150.1(7) . . ? C123 N20 Co3 91.1(6) . . ? C133 N21 C126 119.2(9) . . ? C133 N21 Co4 120.3(8) . . ? C126 N21 Co4 120.5(6) . . ? C134 N22 C142 117.6(9) . . ? C134 N22 Co3 146.5(7) . . ? C142 N22 Co3 95.8(6) . . ? C145 N23 C142 117.3(9) . . ? C145 N23 Co3 151.2(7) . . ? C142 N23 Co3 91.4(6) . . ? C152 N24 C145 119.1(10) . . ? C152 N24 Co4 119.7(8) . . ? C145 N24 Co4 121.1(7) . . ? N1 C1 C2 125.2(10) . . ? C7 C2 C3 121.4(10) . . ? C7 C2 C1 117.6(9) . . ? C3 C2 C1 121.0(10) . . ? C4 C3 C2 118.6(12) . . ? C3 C4 C5 121.5(12) . . ? C6 C5 C4 121.8(12) . . ? C5 C6 C7 118.1(11) . . ? C8 C7 C6 123.5(10) . . ? C8 C7 C2 117.9(9) . . ? C6 C7 C2 118.6(10) . . ? C10 C8 C7 125.0(10) . . ? C10 C8 C9 116.5(9) . . ? C7 C8 C9 118.5(9) . . ? N2 C9 N1 115.7(9) . . ? N2 C9 C8 122.0(9) . . ? N1 C9 C8 122.3(9) . . ? C8 C10 C11 122.9(9) . . ? C10 C11 C12 114.5(9) . . ? C10 C11 C13 127.2(9) . . ? C12 C11 C13 118.3(9) . . ? N2 C12 N3 110.9(8) . . ? N2 C12 C11 125.6(9) . . ? N3 C12 C11 123.5(9) . . ? C14 C13 C18 117.3(10) . . ? C14 C13 C11 124.2(10) . . ? C18 C13 C11 118.5(9) . . ? C15 C14 C13 120.3(11) . . ? C14 C15 C16 120.9(11) . . ? C17 C16 C15 120.3(11) . . ? C16 C17 C18 119.0(11) . . ? C17 C18 C13 122.1(10) . . ? C17 C18 C19 120.3(10) . . ? C13 C18 C19 117.5(9) . . ? N3 C19 C18 123.9(10) . . ? N4 C20 C21 124.4(9) . . ? C22 C21 C26 122.2(10) . . ? C22 C21 C20 120.0(10) . . ? C26 C21 C20 117.7(9) . . ? C21 C22 C23 119.6(11) . . ? C22 C23 C24 119.5(11) . . ? C25 C24 C23 120.4(11) . . ? C24 C25 C26 120.7(11) . . ? C21 C26 C25 117.5(9) . . ? C21 C26 C27 119.1(9) . . ? C25 C26 C27 123.3(9) . . ? C29 C27 C28 118.1(8) . . ? C29 C27 C26 124.2(9) . . ? C28 C27 C26 117.7(9) . . ? N5 C28 N4 115.4(8) . . ? N5 C28 C27 121.9(8) . . ? N4 C28 C27 122.6(8) . . ? C27 C29 C30 120.9(9) . . ? C31 C30 C29 115.8(9) . . ? C31 C30 C32 118.2(9) . . ? C29 C30 C32 125.9(9) . . ? N5 C31 C30 125.8(9) . . ? N5 C31 N6 110.1(8) . . ? C30 C31 N6 124.2(9) . . ? C33 C32 C37 118.1(9) . . ? C33 C32 C30 125.5(9) . . ? C37 C32 C30 116.3(9) . . ? C34 C33 C32 119.4(10) . . ? C33 C34 C35 123.7(10) . . ? C34 C35 C36 118.3(10) . . ? C37 C36 C35 119.7(10) . . ? C36 C37 C38 120.2(9) . . ? C36 C37 C32 120.7(9) . . ? C38 C37 C32 119.0(9) . . ? N6 C38 C37 124.2(9) . . ? N7 C39 C40 124.1(10) . . ? C41 C40 C45 120.4(10) . . ? C41 C40 C39 120.2(11) . . ? C45 C40 C39 119.3(10) . . ? C42 C41 C40 119.7(12) . . ? C41 C42 C43 120.1(12) . . ? C44 C43 C42 120.3(11) . . ? C43 C44 C45 120.6(12) . . ? C44 C45 C40 118.9(10) . . ? C44 C45 C46 124.3(10) . . ? C40 C45 C46 116.7(9) . . ? C48 C46 C47 116.5(9) . . ? C48 C46 C45 126.2(9) . . ? C47 C46 C45 117.3(9) . . ? N8 C47 N7 110.6(8) . . ? N8 C47 C46 124.9(9) . . ? N7 C47 C46 124.5(9) . . ? C49 C48 C46 120.9(9) . . ? C48 C49 C51 125.5(9) . . ? C48 C49 C50 117.3(9) . . ? C51 C49 C50 117.2(9) . . ? N8 C50 N9 116.1(8) . . ? N8 C50 C49 122.3(9) . . ? N9 C50 C49 121.5(9) . . ? C56 C51 C52 118.1(10) . . ? C56 C51 C49 119.5(9) . . ? C52 C51 C49 122.3(11) . . ? C53 C52 C51 119.3(12) . . ? C52 C53 C54 121.9(11) . . ? C55 C54 C53 119.7(11) . . ? C54 C55 C56 120.2(11) . . ? C51 C56 C55 120.7(10) . . ? C51 C56 C57 118.9(9) . . ? C55 C56 C57 120.4(10) . . ? N9 C57 C56 122.5(10) . . ? N10 C58 C59 121.4(9) . . ? C64 C59 C60 121.7(10) . . ? C64 C59 C58 120.3(9) . . ? C60 C59 C58 118.0(10) . . ? C61 C60 C59 119.1(11) . . ? C60 C61 C62 119.1(10) . . ? C63 C62 C61 121.6(10) . . ? C62 C63 C64 119.8(11) . . ? C59 C64 C63 118.7(9) . . ? C59 C64 C65 117.8(9) . . ? C63 C64 C65 123.5(10) . . ? C67 C65 C66 115.9(9) . . ? C67 C65 C64 127.3(9) . . ? C66 C65 C64 116.7(9) . . ? N11 C66 N10 111.6(8) . . ? N11 C66 C65 123.8(9) . . ? N10 C66 C65 124.6(9) . . ? C65 C67 C68 122.4(9) . . ? C67 C68 C70 125.3(8) . . ? C67 C68 C69 117.0(9) . . ? C70 C68 C69 117.6(9) . . ? N11 C69 N12 116.9(8) . . ? N11 C69 C68 121.6(8) . . ? N12 C69 C68 121.5(9) . . ? C75 C70 C71 118.3(9) . . ? C75 C70 C68 118.7(8) . . ? C71 C70 C68 122.9(9) . . ? C72 C71 C70 117.7(10) . . ? C73 C72 C71 123.8(10) . . ? C74 C73 C72 118.5(11) . . ? C73 C74 C75 120.0(11) . . ? C74 C75 C76 120.0(10) . . ? C74 C75 C70 121.6(9) . . ? C76 C75 C70 118.4(9) . . ? N12 C76 C75 124.1(9) . . ? N13 C77 C78 124.8(9) . . ? C79 C78 C83 121.0(9) . . ? C79 C78 C77 120.3(9) . . ? C83 C78 C77 118.6(9) . . ? C80 C79 C78 118.1(10) . . ? C79 C80 C81 122.1(10) . . ? C82 C81 C80 121.2(10) . . ? C81 C82 C83 118.0(10) . . ? C78 C83 C82 119.6(9) . . ? C78 C83 C84 117.4(9) . . ? C82 C83 C84 123.0(9) . . ? C86 C84 C85 118.2(9) . . ? C86 C84 C83 123.1(9) . . ? C85 C84 C83 118.7(9) . . ? N14 C85 N13 113.8(8) . . ? N14 C85 C84 123.4(9) . . ? N13 C85 C84 122.8(8) . . ? C84 C86 C87 119.3(9) . . ? C88 C87 C86 117.0(9) . . ? C88 C87 C89 118.4(9) . . ? C86 C87 C89 124.3(10) . . ? N14 C88 C87 126.5(9) . . ? N14 C88 N15 109.6(8) . . ? C87 C88 N15 123.9(9) . . ? C90 C89 C94 119.0(9) . . ? C90 C89 C87 125.0(10) . . ? C94 C89 C87 116.0(9) . . ? C91 C90 C89 119.8(10) . . ? C90 C91 C92 121.0(11) . . ? C93 C92 C91 120.7(10) . . ? C92 C93 C94 118.7(11) . . ? C93 C94 C89 120.8(10) . . ? C93 C94 C95 119.4(10) . . ? C89 C94 C95 119.7(9) . . ? N15 C95 C94 124.0(10) . . ? N16 C96 C97 125.7(10) . . ? C98 C97 C102 120.4(10) . . ? C98 C97 C96 120.4(10) . . ? C102 C97 C96 119.1(9) . . ? C99 C98 C97 120.8(11) . . ? C100 C99 C98 117.0(11) . . ? C101 C100 C99 124.0(11) . . ? C100 C101 C102 118.6(11) . . ? C101 C102 C97 119.1(10) . . ? C101 C102 C103 124.7(10) . . ? C97 C102 C103 116.2(9) . . ? C105 C103 C104 119.2(9) . . ? C105 C103 C102 122.7(9) . . ? C104 C103 C102 118.1(9) . . ? N17 C104 N16 116.3(8) . . ? N17 C104 C103 120.9(9) . . ? N16 C104 C103 122.8(9) . . ? C103 C105 C106 120.3(9) . . ? C105 C106 C107 116.9(9) . . ? C105 C106 C108 126.2(9) . . ? C107 C106 C108 116.8(9) . . ? N17 C107 N18 110.8(8) . . ? N17 C107 C106 124.6(9) . . ? N18 C107 C106 124.6(9) . . ? C113 C108 C109 120.6(10) . . ? C113 C108 C106 116.7(9) . . ? C109 C108 C106 122.8(9) . . ? C108 C109 C110 116.7(11) . . ? C111 C110 C109 124.9(11) . . ? C110 C111 C112 118.4(11) . . ? C111 C112 C113 118.7(11) . . ? C108 C113 C112 120.7(10) . . ? C108 C113 C114 120.7(9) . . ? C112 C113 C114 118.7(10) . . ? N18 C114 C113 123.2(10) . . ? N19 C115 C116 123.5(10) . . ? C121 C116 C117 121.9(11) . . ? C121 C116 C115 119.1(10) . . ? C117 C116 C115 119.1(11) . . ? C118 C117 C116 118.2(12) . . ? C117 C118 C119 120.3(12) . . ? C120 C119 C118 121.7(12) . . ? C119 C120 C121 120.0(13) . . ? C116 C121 C120 117.8(11) . . ? C116 C121 C122 118.4(10) . . ? C120 C121 C122 123.8(11) . . ? C124 C122 C123 115.0(9) . . ? C124 C122 C121 127.0(10) . . ? C123 C122 C121 118.0(10) . . ? N20 C123 N19 112.0(8) . . ? N20 C123 C122 125.5(10) . . ? N19 C123 C122 122.5(9) . . ? C122 C124 C125 122.5(9) . . ? C124 C125 C127 126.6(10) . . ? C124 C125 C126 116.2(9) . . ? C127 C125 C126 117.2(10) . . ? N20 C126 N21 117.3(9) . . ? N20 C126 C125 121.9(9) . . ? N21 C126 C125 120.8(9) . . ? C132 C127 C128 118.6(12) . . ? C132 C127 C125 119.2(11) . . ? C128 C127 C125 122.1(12) . . ? C129 C128 C127 119.9(14) . . ? C128 C129 C130 119.8(15) . . ? C131 C130 C129 120.5(16) . . ? C130 C131 C132 119.7(15) . . ? C131 C132 C127 121.2(13) . . ? C131 C132 C133 121.3(13) . . ? C127 C132 C133 117.3(12) . . ? N21 C133 C132 126.2(11) . . ? N22 C134 C135 124.4(10) . . ? C136 C135 C140 119.7(11) . . ? C136 C135 C134 120.5(11) . . ? C140 C135 C134 119.8(10) . . ? C135 C136 C137 118.6(12) . . ? C138 C137 C136 119.0(11) . . ? C139 C138 C137 125.0(12) . . ? C138 C139 C140 116.0(12) . . ? C139 C140 C135 121.4(11) . . ? C139 C140 C141 122.6(11) . . ? C135 C140 C141 115.9(10) . . ? C142 C141 C143 117.7(11) . . ? C142 C141 C140 117.2(10) . . ? C143 C141 C140 125.0(10) . . ? N23 C142 C141 124.3(10) . . ? N23 C142 N22 110.6(9) . . ? C141 C142 N22 125.1(10) . . ? C141 C143 C144 119.9(11) . . ? C143 C144 C145 119.2(11) . . ? C143 C144 C146 123.0(11) . . ? C145 C144 C146 117.7(11) . . ? N23 C145 N24 115.2(9) . . ? N23 C145 C144 121.4(10) . . ? N24 C145 C144 123.3(10) . . ? C147 C146 C151 120.2(13) . . ? C147 C146 C144 124.4(14) . . ? C151 C146 C144 115.3(12) . . ? C146 C147 C148 117.3(15) . . ? C149 C148 C147 124.4(15) . . ? C148 C149 C150 118.0(15) . . ? C149 C150 C151 119.2(15) . . ? C152 C151 C150 119.5(13) . . ? C152 C151 C146 121.0(13) . . ? C150 C151 C146 119.4(13) . . ? N24 C152 C151 123.4(13) . . ? O2 Cl1 O3 110.3(5) . . ? O2 Cl1 O4 107.8(6) . . ? O3 Cl1 O4 109.9(7) . . ? O2 Cl1 O1 109.9(5) . . ? O3 Cl1 O1 109.8(6) . . ? O4 Cl1 O1 109.1(5) . . ? O8 Cl2 O6 123.1(7) . . ? O8 Cl2 O5 114.5(7) . . ? O6 Cl2 O5 113.3(6) . . ? O8 Cl2 O7 100.0(7) . . ? O6 Cl2 O7 99.8(7) . . ? O5 Cl2 O7 100.7(6) . . ? O10 Cl3 O12 105.2(8) . . ? O10 Cl3 O9 109.4(6) . . ? O12 Cl3 O9 109.2(8) . . ? O10 Cl3 O11 114.4(7) . . ? O12 Cl3 O11 107.2(7) . . ? O9 Cl3 O11 111.1(6) . . ? O16 Cl4 O13 115.4(8) . . ? O16 Cl4 O14 122.5(9) . . ? O13 Cl4 O14 113.1(8) . . ? O16 Cl4 O15 97.0(8) . . ? O13 Cl4 O15 102.1(8) . . ? O14 Cl4 O15 101.3(7) . . ? O18 Cl5 O19 114.2(10) . . ? O18 Cl5 O17 112.9(7) . . ? O19 Cl5 O17 111.2(8) . . ? O18 Cl5 O20 106.2(14) . . ? O19 Cl5 O20 101.9(13) . . ? O17 Cl5 O20 109.6(10) . . ? O24 Cl6 O21 109.7(7) . . ? O24 Cl6 O23 110.1(9) . . ? O21 Cl6 O23 110.7(8) . . ? O24 Cl6 O22 113.1(9) . . ? O21 Cl6 O22 107.9(7) . . ? O23 Cl6 O22 105.2(9) . . ? O27 Cl7 O25 121.3(8) . . ? O27 Cl7 O28 113.0(7) . . ? O25 Cl7 O28 119.6(8) . . ? O27 Cl7 O26 102.0(8) . . ? O25 Cl7 O26 94.3(9) . . ? O28 Cl7 O26 98.7(8) . . ? O29 Cl8 O32 106.3(12) . . ? O29 Cl8 O31 126.3(18) . . ? O32 Cl8 O31 109.7(13) . . ? O29 Cl8 O30 101.0(19) . . ? O32 Cl8 O30 106.2(13) . . ? O31 Cl8 O30 105.5(10) . . ? N25 C153 C154 178.2(15) . . ? N26 C155 C156 176.8(15) . . ? N27 C157 C158 177(2) . . ? N28 C159 C160 177(2) . . ? N29 C161 C162 179.0(19) . . ? N30 C163 C164 176.2(18) . . ? N32 C167 C168 154(6) . . ? C170 O33 C171 131(2) . . ? O33 C170 C169 105.4(19) . . ? O33 C171 C172 134(3) . . ? C174 O34 C175 124(3) . . ? O34 C174 C173 114(2) . . ? O34 C175 C176 156(4) . . ? C178 O35 C179 146(3) . . ? O35 C178 C177 131(3) . . ? O35 C179 C180 157(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 68.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.929 _refine_diff_density_min -0.940 _refine_diff_density_rms 0.161 # Attachment '- ic14331-re-revised Zn.cif' data_ic14331 _database_code_depnum_ccdc_archive 'CCDC 875008' #TrackingRef '- ic14331-re-revised Zn.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C177 H133.50 Cl8 N32.50 O34 Zn4' _chemical_formula_weight 3804.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.6133(3) _cell_length_b 69.9138(14) _cell_length_c 19.1264(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.834(2) _cell_angle_gamma 90.00 _cell_volume 17936.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14867 _cell_measurement_theta_min 3.1579 _cell_measurement_theta_max 75.9996 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7804 _exptl_absorpt_coefficient_mu 2.387 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88823 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56887 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 84 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 68.00 _reflns_number_total 32452 _reflns_number_gt 22120 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. During the structure refinement, the atoms of the (MeCN & Ether) solvent molecule were observed but could not be modelled satisfactorily. The atoms of solvent were refined isotropically with restrained geometry. 2242 parameters refined using 180 restraints H atoms were placed in calculated positions and treated as riding atoms using SHELXL default parameters. ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 32452 _refine_ls_number_parameters 2242 _refine_ls_number_restraints 198 _refine_ls_R_factor_all 0.1583 _refine_ls_R_factor_gt 0.1237 _refine_ls_wR_factor_ref 0.3157 _refine_ls_wR_factor_gt 0.3040 _refine_ls_goodness_of_fit_ref 1.831 _refine_ls_restrained_S_all 1.832 _refine_ls_shift/su_max 0.080 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.71040(7) 0.037091(13) 0.23901(5) 0.0382(2) Uani 1 1 d . . . Zn2 Zn 0.68339(7) 0.084560(14) 0.24244(5) 0.0400(2) Uani 1 1 d . . . Zn3 Zn 0.15164(8) 0.165855(14) 0.74387(5) 0.0418(2) Uani 1 1 d . . . Zn4 Zn 0.12597(8) 0.213662(14) 0.72763(5) 0.0434(3) Uani 1 1 d . . . N1 N 0.8549(4) 0.04187(8) 0.2132(3) 0.0360(12) Uani 1 1 d . . . N2 N 0.8285(4) 0.07428(8) 0.2147(3) 0.0343(12) Uani 1 1 d . . . N3 N 0.7898(5) 0.10558(8) 0.2215(3) 0.0393(13) Uani 1 1 d . . . N4 N 0.5643(5) 0.03458(9) 0.2660(3) 0.0401(13) Uani 1 1 d . . . N5 N 0.5494(4) 0.06728(9) 0.2659(3) 0.0397(13) Uani 1 1 d . . . N6 N 0.5548(5) 0.09925(9) 0.2638(3) 0.0444(14) Uani 1 1 d . . . N7 N 0.7702(5) 0.01820(9) 0.3238(3) 0.0420(14) Uani 1 1 d . . . N8 N 0.7609(4) 0.04968(9) 0.3454(3) 0.0379(13) Uani 1 1 d . . . N9 N 0.7454(4) 0.08251(9) 0.3537(3) 0.0403(13) Uani 1 1 d . . . N10 N 0.6750(5) 0.01761(8) 0.1484(3) 0.0384(13) Uani 1 1 d . . . N11 N 0.6487(4) 0.04913(8) 0.1336(3) 0.0359(12) Uani 1 1 d . . . N12 N 0.6235(4) 0.08173(8) 0.1312(3) 0.0355(12) Uani 1 1 d . . . N13 N 0.2070(5) 0.17061(8) 0.8523(3) 0.0405(13) Uani 1 1 d . . . N14 N 0.1881(5) 0.20331(8) 0.8378(3) 0.0400(13) Uani 1 1 d . . . N15 N 0.1639(5) 0.23444(9) 0.8102(3) 0.0447(14) Uani 1 1 d . . . N16 N 0.0915(4) 0.16534(8) 0.6327(3) 0.0386(13) Uani 1 1 d . . . N17 N 0.0794(5) 0.19833(8) 0.6264(3) 0.0425(14) Uani 1 1 d . . . N18 N 0.0756(5) 0.23049(8) 0.6322(3) 0.0439(14) Uani 1 1 d . . . N19 N 0.2794(5) 0.14967(9) 0.7252(3) 0.0466(15) Uani 1 1 d . . . N20 N 0.2838(5) 0.18172(9) 0.7125(3) 0.0441(14) Uani 1 1 d . . . N21 N 0.2745(5) 0.21439(9) 0.7025(3) 0.0473(15) Uani 1 1 d . . . N22 N 0.0389(5) 0.14621(9) 0.7674(3) 0.0443(14) Uani 1 1 d . B . N23 N 0.0027(5) 0.17793(9) 0.7632(3) 0.0422(14) Uani 1 1 d . B . N24 N -0.0199(5) 0.21026(9) 0.7526(3) 0.0440(14) Uani 1 1 d . B . C1 C 0.9116(5) 0.02751(10) 0.2049(4) 0.0395(15) Uani 1 1 d . . . H1A H 0.8868 0.0151 0.2126 0.047 Uiso 1 1 calc R . . C2 C 1.0085(6) 0.02850(11) 0.1852(4) 0.0441(17) Uani 1 1 d . . . C3 C 1.0635(7) 0.01241(11) 0.1755(5) 0.053(2) Uani 1 1 d . . . H3A H 1.0376 0.0001 0.1827 0.063 Uiso 1 1 calc R . . C4 C 1.1541(8) 0.01410(14) 0.1560(6) 0.067(3) Uani 1 1 d . . . H4A H 1.1906 0.0030 0.1478 0.081 Uiso 1 1 calc R . . C5 C 1.1945(8) 0.03241(14) 0.1476(6) 0.076(3) Uani 1 1 d . . . H5A H 1.2591 0.0335 0.1357 0.092 Uiso 1 1 calc R . . C6 C 1.1413(7) 0.04866(12) 0.1566(5) 0.058(2) Uani 1 1 d . . . H6A H 1.1693 0.0609 0.1506 0.069 Uiso 1 1 calc R . . C7 C 1.0468(6) 0.04737(11) 0.1744(4) 0.0445(17) Uani 1 1 d . . . C8 C 0.9848(5) 0.06360(10) 0.1840(3) 0.0353(14) Uani 1 1 d . . . C9 C 1.0133(5) 0.08236(11) 0.1752(4) 0.0389(15) Uani 1 1 d . . . H9A H 1.0760 0.0850 0.1618 0.047 Uiso 1 1 calc R . . C10 C 0.9501(5) 0.09743(10) 0.1860(3) 0.0364(15) Uani 1 1 d . . . C11 C 0.9728(5) 0.11771(10) 0.1801(4) 0.0395(15) Uani 1 1 d . . . C12 C 1.0588(6) 0.12507(11) 0.1607(4) 0.0459(17) Uani 1 1 d . . . H12A H 1.1099 0.1167 0.1511 0.055 Uiso 1 1 calc R . . C13 C 1.0699(8) 0.14462(13) 0.1555(5) 0.066(2) Uani 1 1 d . . . H13A H 1.1288 0.1494 0.1413 0.079 Uiso 1 1 calc R . . C14 C 0.9996(7) 0.15736(12) 0.1698(5) 0.059(2) Uani 1 1 d . . . H14A H 1.0103 0.1707 0.1664 0.071 Uiso 1 1 calc R . . C15 C 0.9119(7) 0.15046(11) 0.1895(4) 0.0502(19) Uani 1 1 d . . . H15A H 0.8623 0.1592 0.1993 0.060 Uiso 1 1 calc R . . C16 C 0.8970(6) 0.13067(11) 0.1949(4) 0.0428(16) Uani 1 1 d . . . C17 C 0.8087(6) 0.12366(10) 0.2149(4) 0.0408(16) Uani 1 1 d . . . H17A H 0.7602 0.1327 0.2240 0.049 Uiso 1 1 calc R . . C18 C 0.8594(5) 0.09251(10) 0.2065(3) 0.0344(14) Uani 1 1 d . . . C19 C 0.8907(5) 0.06000(10) 0.2041(3) 0.0352(14) Uani 1 1 d . . . C20 C 0.5282(6) 0.01748(13) 0.2753(4) 0.0508(19) Uani 1 1 d . . . H20A H 0.5674 0.0066 0.2686 0.061 Uiso 1 1 calc R . . C21 C 0.4341(6) 0.01454(13) 0.2947(4) 0.0508(19) Uani 1 1 d . . . C22 C 0.3990(8) -0.00459(15) 0.3030(5) 0.069(3) Uani 1 1 d . . . H22A H 0.4410 -0.0152 0.2984 0.083 Uiso 1 1 calc R . . C23 C 0.3071(10) -0.00747(16) 0.3172(6) 0.083(3) Uani 1 1 d . . . H23A H 0.2838 -0.0201 0.3218 0.100 Uiso 1 1 calc R . . C24 C 0.2448(10) 0.00813(19) 0.3254(7) 0.095(4) Uani 1 1 d . . . H24A H 0.1796 0.0057 0.3347 0.114 Uiso 1 1 calc R . . C25 C 0.2762(8) 0.02698(16) 0.3203(5) 0.070(3) Uani 1 1 d . . . H25A H 0.2344 0.0374 0.3273 0.084 Uiso 1 1 calc R . . C26 C 0.3724(7) 0.02989(13) 0.3043(4) 0.055(2) Uani 1 1 d . . . C27 C 0.4097(6) 0.04927(12) 0.2940(4) 0.0467(18) Uani 1 1 d . . . C28 C 0.3617(6) 0.06586(13) 0.3012(4) 0.053(2) Uani 1 1 d . . . H28A H 0.2970 0.0654 0.3136 0.064 Uiso 1 1 calc R . . C29 C 0.4033(6) 0.08354(13) 0.2913(4) 0.0462(18) Uani 1 1 d . . . C30 C 0.3576(7) 0.10204(13) 0.2965(4) 0.053(2) Uani 1 1 d . . . C31 C 0.2631(7) 0.10479(16) 0.3123(5) 0.065(2) Uani 1 1 d . . . H31A H 0.2233 0.0941 0.3197 0.078 Uiso 1 1 calc R . . C32 C 0.2261(8) 0.12308(17) 0.3173(5) 0.074(3) Uani 1 1 d . . . H32A H 0.1613 0.1248 0.3285 0.089 Uiso 1 1 calc R . . C33 C 0.2815(8) 0.13873(16) 0.3066(5) 0.071(3) Uani 1 1 d . . . H33A H 0.2538 0.1511 0.3095 0.085 Uiso 1 1 calc R . . C34 C 0.3765(7) 0.13704(14) 0.2915(4) 0.060(2) Uani 1 1 d . . . H34A H 0.4147 0.1481 0.2851 0.072 Uiso 1 1 calc R . . C35 C 0.4159(7) 0.11841(13) 0.2858(4) 0.054(2) Uani 1 1 d . . . C36 C 0.5143(6) 0.11608(12) 0.2683(4) 0.0487(18) Uani 1 1 d . . . H36A H 0.5508 0.1272 0.2597 0.058 Uiso 1 1 calc R . . C37 C 0.5007(6) 0.08307(11) 0.2744(3) 0.0401(16) Uani 1 1 d . . . C38 C 0.5072(6) 0.05032(11) 0.2753(4) 0.0436(17) Uani 1 1 d . . . C39 C 0.7927(7) 0.00076(12) 0.3431(4) 0.052(2) Uani 1 1 d . . . H39A H 0.7809 -0.0092 0.3089 0.063 Uiso 1 1 calc R . . C40 C 0.8349(7) -0.00386(13) 0.4148(5) 0.058(2) Uani 1 1 d . . . C41 C 0.8606(9) -0.02372(14) 0.4313(5) 0.071(3) Uani 1 1 d . . . H41A H 0.8486 -0.0333 0.3956 0.085 Uiso 1 1 calc R . . C42 C 0.9024(9) -0.02829(16) 0.4991(6) 0.080(3) Uani 1 1 d . . . H42A H 0.9212 -0.0411 0.5108 0.096 Uiso 1 1 calc R . . C43 C 0.9179(9) -0.01413(15) 0.5519(5) 0.074(3) Uani 1 1 d . . . H43A H 0.9464 -0.0177 0.5989 0.089 Uiso 1 1 calc R . . C44 C 0.8931(8) 0.00503(15) 0.5377(5) 0.065(2) Uani 1 1 d . . . H44A H 0.9038 0.0144 0.5742 0.078 Uiso 1 1 calc R . . C45 C 0.8514(7) 0.00998(13) 0.4671(4) 0.054(2) Uani 1 1 d . . . C46 C 0.8272(6) 0.02952(12) 0.4454(4) 0.0505(19) Uani 1 1 d . . . C47 C 0.8387(6) 0.04583(13) 0.4884(4) 0.0509(19) Uani 1 1 d . . . H47A H 0.8644 0.0446 0.5376 0.061 Uiso 1 1 calc R . . C48 C 0.8130(6) 0.06386(12) 0.4602(4) 0.0476(18) Uani 1 1 d . . . C49 C 0.8241(6) 0.08104(13) 0.5019(4) 0.054(2) Uani 1 1 d . . . C50 C 0.8608(8) 0.08175(16) 0.5745(5) 0.070(3) Uani 1 1 d . . . H50A H 0.8827 0.0704 0.5997 0.084 Uiso 1 1 calc R . . C51 C 0.8651(9) 0.09920(18) 0.6095(5) 0.080(3) Uani 1 1 d . . . H51A H 0.8901 0.0995 0.6590 0.095 Uiso 1 1 calc R . . C52 C 0.8341(8) 0.11623(16) 0.5749(5) 0.071(3) Uani 1 1 d . . . H52A H 0.8375 0.1279 0.6004 0.085 Uiso 1 1 calc R . . C53 C 0.7985(7) 0.11581(14) 0.5033(5) 0.062(2) Uani 1 1 d . . . H53A H 0.7781 0.1274 0.4789 0.074 Uiso 1 1 calc R . . C54 C 0.7919(6) 0.09847(13) 0.4660(4) 0.0507(19) Uani 1 1 d . . . C55 C 0.7530(6) 0.09773(12) 0.3915(4) 0.0481(18) Uani 1 1 d . . . H55A H 0.7312 0.1094 0.3685 0.058 Uiso 1 1 calc R . . C56 C 0.7737(5) 0.06521(11) 0.3878(4) 0.0407(16) Uani 1 1 d . . . C57 C 0.7866(5) 0.03273(11) 0.3736(4) 0.0408(16) Uani 1 1 d . . . C58 C 0.6760(6) -0.00002(11) 0.1244(4) 0.0442(17) Uani 1 1 d . . . H58A H 0.6969 -0.0100 0.1571 0.053 Uiso 1 1 calc R . . C59 C 0.6474(5) -0.00466(11) 0.0518(4) 0.0411(16) Uani 1 1 d . . . C60 C 0.6468(6) -0.02397(11) 0.0302(5) 0.052(2) Uani 1 1 d . . . H60A H 0.6658 -0.0338 0.0642 0.063 Uiso 1 1 calc R . . C61 C 0.6187(6) -0.02847(12) -0.0401(5) 0.053(2) Uani 1 1 d . . . H61A H 0.6169 -0.0415 -0.0546 0.063 Uiso 1 1 calc R . . C62 C 0.5932(6) -0.01437(14) -0.0898(5) 0.057(2) Uani 1 1 d . . . H62A H 0.5758 -0.0178 -0.1384 0.069 Uiso 1 1 calc R . . C63 C 0.5921(6) 0.00501(12) -0.0707(4) 0.0476(18) Uani 1 1 d . . . H63A H 0.5725 0.0146 -0.1056 0.057 Uiso 1 1 calc R . . C64 C 0.6205(5) 0.00998(11) 0.0014(4) 0.0433(17) Uani 1 1 d . . . C65 C 0.6183(5) 0.02933(11) 0.0275(4) 0.0382(15) Uani 1 1 d . . . C66 C 0.5889(5) 0.04539(11) -0.0115(4) 0.0408(16) Uani 1 1 d . . . H66A H 0.5692 0.0443 -0.0614 0.049 Uiso 1 1 calc R . . C67 C 0.5871(5) 0.06343(10) 0.0208(3) 0.0362(15) Uani 1 1 d . . . C68 C 0.5526(6) 0.08089(11) -0.0180(4) 0.0421(16) Uani 1 1 d . . . C69 C 0.5145(6) 0.08113(12) -0.0910(4) 0.0503(19) Uani 1 1 d . . . H69A H 0.5114 0.0697 -0.1182 0.060 Uiso 1 1 calc R . . C70 C 0.4813(8) 0.09847(14) -0.1230(5) 0.064(2) Uani 1 1 d . . . H70A H 0.4535 0.0989 -0.1720 0.077 Uiso 1 1 calc R . . C71 C 0.4891(7) 0.11517(13) -0.0826(5) 0.058(2) Uani 1 1 d . . . H71A H 0.4694 0.1270 -0.1049 0.069 Uiso 1 1 calc R . . C72 C 0.5234(6) 0.11472(12) -0.0136(4) 0.0488(18) Uani 1 1 d . . . H72A H 0.5252 0.1262 0.0130 0.059 Uiso 1 1 calc R . . C73 C 0.5575(5) 0.09759(11) 0.0213(4) 0.0404(16) Uani 1 1 d . . . C74 C 0.5942(5) 0.09714(10) 0.0952(4) 0.0397(16) Uani 1 1 d . . . H74A H 0.5977 0.1089 0.1203 0.048 Uiso 1 1 calc R . . C75 C 0.6203(5) 0.06460(10) 0.0944(3) 0.0336(14) Uani 1 1 d . . . C76 C 0.6480(5) 0.03202(10) 0.1020(4) 0.0350(14) Uani 1 1 d . . . C77 C 0.2341(6) 0.15603(10) 0.8944(4) 0.0430(17) Uani 1 1 d . . . H77A H 0.2305 0.1436 0.8736 0.052 Uiso 1 1 calc R . . C78 C 0.2681(6) 0.15735(10) 0.9683(4) 0.0438(17) Uani 1 1 d . . . C79 C 0.2952(6) 0.14063(11) 1.0097(5) 0.0509(19) Uani 1 1 d . . . H79A H 0.2917 0.1285 0.9874 0.061 Uiso 1 1 calc R . . C80 C 0.3263(7) 0.14204(12) 1.0814(5) 0.058(2) Uani 1 1 d . . . H80A H 0.3424 0.1309 1.1092 0.069 Uiso 1 1 calc R . . C81 C 0.3340(8) 0.15998(13) 1.1130(5) 0.066(3) Uani 1 1 d . . . H81A H 0.3573 0.1609 1.1626 0.079 Uiso 1 1 calc R . . C82 C 0.3090(7) 0.17658(12) 1.0748(4) 0.055(2) Uani 1 1 d . . . H82A H 0.3140 0.1886 1.0982 0.066 Uiso 1 1 calc R . . C83 C 0.2763(6) 0.17557(11) 1.0011(4) 0.0446(17) Uani 1 1 d . . . C84 C 0.2500(6) 0.19165(10) 0.9570(4) 0.0426(16) Uani 1 1 d . . . C85 C 0.2573(6) 0.21069(11) 0.9811(4) 0.0486(19) Uani 1 1 d . . . H85A H 0.2818 0.2133 1.0297 0.058 Uiso 1 1 calc R . . C86 C 0.2284(6) 0.22582(10) 0.9337(4) 0.0456(17) Uani 1 1 d . . . C87 C 0.2371(7) 0.24598(12) 0.9527(5) 0.055(2) Uani 1 1 d . . . C88 C 0.2749(7) 0.25282(12) 1.0210(5) 0.057(2) Uani 1 1 d . . . H88A H 0.2962 0.2442 1.0590 0.068 Uiso 1 1 calc R . . C89 C 0.2803(8) 0.27260(13) 1.0317(6) 0.067(3) Uani 1 1 d . . . H89A H 0.3032 0.2773 1.0782 0.080 Uiso 1 1 calc R . . C90 C 0.2538(8) 0.28543(13) 0.9776(5) 0.065(2) Uani 1 1 d . . . H90A H 0.2615 0.2988 0.9862 0.078 Uiso 1 1 calc R . . C91 C 0.2159(8) 0.27876(12) 0.9102(5) 0.065(3) Uani 1 1 d . . . H91A H 0.1968 0.2876 0.8727 0.078 Uiso 1 1 calc R . . C92 C 0.2055(7) 0.25925(12) 0.8969(5) 0.057(2) Uani 1 1 d . . . C93 C 0.1708(6) 0.25235(11) 0.8273(5) 0.052(2) Uani 1 1 d . . . H93A H 0.1513 0.2615 0.7908 0.063 Uiso 1 1 calc R . . C94 C 0.1954(6) 0.22109(10) 0.8631(4) 0.0438(17) Uani 1 1 d . . . C95 C 0.2150(5) 0.18867(10) 0.8826(4) 0.0371(15) Uani 1 1 d . . . C96 C 0.0810(6) 0.14885(11) 0.6011(4) 0.0468(18) Uani 1 1 d . . . H96A H 0.0988 0.1378 0.6294 0.056 Uiso 1 1 calc R . . C97 C 0.0449(6) 0.14600(11) 0.5271(4) 0.0431(16) Uani 1 1 d . . . C98 C 0.0396(7) 0.12732(11) 0.4977(4) 0.0505(19) Uani 1 1 d . . . H98A H 0.0591 0.1166 0.5273 0.061 Uiso 1 1 calc R . . C99 C 0.0072(7) 0.12484(12) 0.4280(5) 0.056(2) Uani 1 1 d . . . H99A H 0.0060 0.1124 0.4080 0.067 Uiso 1 1 calc R . . C100 C -0.0250(8) 0.14053(13) 0.3849(5) 0.066(3) Uani 1 1 d . . . H10A H -0.0510 0.1385 0.3361 0.079 Uiso 1 1 calc R . . C101 C -0.0198(8) 0.15902(13) 0.4113(5) 0.063(2) Uani 1 1 d . . . H10B H -0.0407 0.1696 0.3811 0.076 Uiso 1 1 calc R . . C102 C 0.0174(6) 0.16180(11) 0.4844(4) 0.0465(18) Uani 1 1 d . . . C103 C 0.0277(6) 0.18049(11) 0.5178(4) 0.0423(16) Uani 1 1 d . . . C104 C 0.0075(6) 0.19772(11) 0.4813(4) 0.0455(17) Uani 1 1 d . . . H10C H -0.0160 0.1975 0.4316 0.055 Uiso 1 1 calc R . . C105 C 0.0208(6) 0.21498(12) 0.5157(4) 0.0491(18) Uani 1 1 d . . . C106 C 0.0046(6) 0.23395(11) 0.4833(5) 0.0509(19) Uani 1 1 d . . . C107 C -0.0306(7) 0.23662(13) 0.4108(5) 0.058(2) Uani 1 1 d . . . H10D H -0.0438 0.2260 0.3798 0.070 Uiso 1 1 calc R . . C108 C -0.0457(8) 0.25525(13) 0.3851(6) 0.066(2) Uani 1 1 d . . . H10E H -0.0695 0.2572 0.3360 0.079 Uiso 1 1 calc R . . C109 C -0.0270(8) 0.27081(14) 0.4288(6) 0.068(3) Uani 1 1 d . . . H10F H -0.0382 0.2833 0.4098 0.082 Uiso 1 1 calc R . . C110 C 0.0074(8) 0.26844(12) 0.4989(5) 0.063(2) Uani 1 1 d . . . H11A H 0.0203 0.2793 0.5287 0.076 Uiso 1 1 calc R . . C111 C 0.0245(6) 0.24982(11) 0.5285(5) 0.0484(18) Uani 1 1 d . . . C112 C 0.0592(7) 0.24726(11) 0.6012(5) 0.053(2) Uani 1 1 d . . . H11B H 0.0718 0.2584 0.6299 0.064 Uiso 1 1 calc R . . C113 C 0.0568(5) 0.21452(10) 0.5889(4) 0.0413(16) Uani 1 1 d . . . C114 C 0.0657(5) 0.18141(10) 0.5909(4) 0.0419(16) Uani 1 1 d . . . C115 C 0.3165(6) 0.13254(10) 0.7207(4) 0.0410(16) Uani 1 1 d . . . H11C H 0.2791 0.1219 0.7326 0.049 Uiso 1 1 calc R . . C116 C 0.4113(7) 0.12886(11) 0.6988(4) 0.054(2) Uani 1 1 d . . . C117 C 0.4448(7) 0.11015(13) 0.6929(4) 0.055(2) Uani 1 1 d . . . H11D H 0.4044 0.0996 0.7017 0.066 Uiso 1 1 calc R . . C118 C 0.5360(8) 0.10703(14) 0.6743(5) 0.065(3) Uani 1 1 d . . . H11E H 0.5604 0.0943 0.6724 0.078 Uiso 1 1 calc R . . C119 C 0.5929(8) 0.12233(16) 0.6583(6) 0.072(3) Uani 1 1 d . . . H11F H 0.6551 0.1200 0.6437 0.087 Uiso 1 1 calc R . . C120 C 0.5610(7) 0.14108(14) 0.6632(5) 0.063(2) Uani 1 1 d . . . H12B H 0.6017 0.1514 0.6527 0.076 Uiso 1 1 calc R . . C121 C 0.4695(7) 0.14484(13) 0.6835(5) 0.056(2) Uani 1 1 d . . . C122 C 0.4274(6) 0.16370(13) 0.6865(5) 0.054(2) Uani 1 1 d . . . C123 C 0.4681(7) 0.18062(15) 0.6688(6) 0.073(3) Uani 1 1 d . A . H12C H 0.5309 0.1804 0.6535 0.088 Uiso 1 1 calc R . . C124 C 0.4216(8) 0.19752(13) 0.6724(6) 0.071(3) Uani 1 1 d . . . C125 C 0.4756(17) 0.2172(4) 0.6698(13) 0.056(6) Uani 0.50 1 d P A 1 C126 C 0.5674(19) 0.2190(4) 0.6544(15) 0.080(8) Uani 0.50 1 d P A 1 H12D H 0.6112 0.2084 0.6549 0.095 Uiso 0.50 1 calc PR A 1 C127 C 0.595(2) 0.2378(3) 0.6372(17) 0.089(9) Uani 0.50 1 d P A 1 H12E H 0.6542 0.2394 0.6178 0.107 Uiso 0.50 1 calc PR A 1 C128 C 0.537(2) 0.2543(3) 0.6477(18) 0.093(10) Uani 0.50 1 d P A 1 H12F H 0.5636 0.2667 0.6421 0.112 Uiso 0.50 1 calc PR A 1 C129 C 0.447(2) 0.2525(4) 0.6653(14) 0.069(8) Uani 0.50 1 d P A 1 H12G H 0.4109 0.2633 0.6764 0.082 Uiso 0.50 1 calc PR A 1 C25' C 0.4430(18) 0.2155(4) 0.6391(18) 0.073(9) Uani 0.50 1 d P A 2 C26' C 0.525(2) 0.2172(3) 0.602(2) 0.109(13) Uani 0.50 1 d P A 2 H26A H 0.5634 0.2062 0.5947 0.131 Uiso 0.50 1 calc PR A 2 C27' C 0.551(2) 0.2357(5) 0.575(3) 0.137(17) Uani 0.50 1 d P A 2 H27A H 0.6043 0.2369 0.5484 0.165 Uiso 0.50 1 calc PR A 2 C28' C 0.498(3) 0.2508(4) 0.588(3) 0.132(16) Uani 0.50 1 d P A 2 H28B H 0.5122 0.2631 0.5705 0.159 Uiso 0.50 1 calc PR A 2 C29' C 0.422(2) 0.2489(4) 0.627(2) 0.100(12) Uani 0.50 1 d P A 2 H29A H 0.3772 0.2593 0.6259 0.120 Uiso 0.50 1 calc PR A 2 C130 C 0.4048(8) 0.23283(14) 0.6671(7) 0.074(3) Uani 1 1 d . . . C131 C 0.3124(7) 0.23071(13) 0.6883(5) 0.059(2) Uani 1 1 d . A . H13B H 0.2747 0.2419 0.6927 0.071 Uiso 1 1 calc R . . C132 C 0.3269(6) 0.19785(12) 0.6958(4) 0.0486(18) Uani 1 1 d . A . C133 C 0.3320(6) 0.16500(11) 0.7077(4) 0.0437(17) Uani 1 1 d . . . C134 C 0.0163(7) 0.12854(12) 0.7770(4) 0.0485(19) Uani 1 1 d . . . H13C H 0.0639 0.1190 0.7713 0.058 Uiso 1 1 calc R . . C135 C -0.0755(7) 0.12270(12) 0.7953(4) 0.054(2) Uani 1 1 d . . . C136 C -0.0953(8) 0.10299(13) 0.8053(4) 0.062(2) Uani 1 1 d . . . H13D H -0.0470 0.0936 0.7990 0.075 Uiso 1 1 calc R . . C137 C -0.1834(9) 0.09747(16) 0.8240(5) 0.073(3) Uani 1 1 d . . . H13E H -0.1958 0.0843 0.8314 0.088 Uiso 1 1 calc R . . C138 C -0.2544(9) 0.11096(17) 0.8319(6) 0.077(3) Uani 1 1 d . . . H13F H -0.3154 0.1068 0.8447 0.093 Uiso 1 1 calc R . . C139 C -0.2404(7) 0.13032(15) 0.8221(5) 0.063(2) Uani 1 1 d . . . H13G H -0.2912 0.1393 0.8272 0.076 Uiso 1 1 calc R . . C140 C -0.1488(7) 0.13650(13) 0.8042(4) 0.054(2) Uani 1 1 d . . . C141 C -0.1230(6) 0.15616(12) 0.7945(4) 0.0472(18) Uani 1 1 d . B . C142 C -0.1847(6) 0.17195(13) 0.7986(4) 0.055(2) Uani 1 1 d . . . H14B H -0.2485 0.1701 0.8113 0.066 Uiso 1 1 calc R . . C143 C -0.1550(6) 0.19026(12) 0.7846(4) 0.0508(19) Uani 1 1 d . B . C144 C -0.2148(8) 0.20696(15) 0.7850(6) 0.072(3) Uani 1 1 d . . . C149 C -0.1732(8) 0.22492(15) 0.7714(7) 0.078(3) Uani 1 1 d U B . C145 C -0.317(2) 0.2075(4) 0.7851(13) 0.056(6) Uani 0.50 1 d P B 1 H14C H -0.3499 0.1957 0.7905 0.067 Uiso 0.50 1 calc PR B 1 C146 C -0.375(2) 0.2242(5) 0.7776(18) 0.084(9) Uani 0.50 1 d P B 1 H14D H -0.4401 0.2236 0.7896 0.101 Uiso 0.50 1 calc PR B 1 C147 C -0.343(2) 0.2421(5) 0.753(2) 0.110(12) Uani 0.50 1 d P B 1 H14E H -0.3860 0.2526 0.7387 0.132 Uiso 0.50 1 calc PR B 1 C148 C -0.2422(19) 0.2419(4) 0.7540(16) 0.083(5) Uani 0.50 1 d PU B 1 H14F H -0.2128 0.2536 0.7424 0.100 Uiso 0.50 1 calc PR B 1 C45' C -0.304(2) 0.2059(5) 0.8191(15) 0.072(9) Uani 0.50 1 d P B 2 H45A H -0.3254 0.1943 0.8377 0.087 Uiso 0.50 1 calc PR B 2 C46' C -0.355(3) 0.2230(5) 0.822(2) 0.103(12) Uani 0.50 1 d P B 2 H46A H -0.4209 0.2230 0.8320 0.123 Uiso 0.50 1 calc PR B 2 C47' C -0.3078(18) 0.2401(4) 0.810(2) 0.103(11) Uani 0.50 1 d P B 2 H47B H -0.3436 0.2516 0.8149 0.124 Uiso 0.50 1 calc PR B 2 C48' C -0.211(2) 0.2421(4) 0.7920(16) 0.084(5) Uani 0.50 1 d PU B 2 H48A H -0.1763 0.2539 0.7938 0.101 Uiso 0.50 1 calc PR B 2 C150 C -0.0767(6) 0.22531(13) 0.7534(5) 0.054(2) Uani 1 1 d . . . H15B H -0.0515 0.2373 0.7409 0.065 Uiso 1 1 calc R B . C151 C -0.0563(6) 0.19280(11) 0.7670(4) 0.0427(16) Uani 1 1 d . . . C152 C -0.0295(5) 0.15998(11) 0.7754(3) 0.0392(16) Uani 1 1 d . . . Cl1 Cl 0.4444(4) 0.21422(4) 0.2186(2) 0.1103(13) Uani 1 1 d . . . O1 O 0.5522(10) 0.21538(17) 0.2076(9) 0.170(6) Uani 1 1 d . . . O2 O 0.4274(9) 0.19515(12) 0.2304(5) 0.116(3) Uani 1 1 d . . . O3 O 0.4512(10) 0.22548(15) 0.2764(8) 0.166(6) Uani 1 1 d . . . O4 O 0.3898(12) 0.22053(15) 0.1615(8) 0.192(8) Uani 1 1 d . . . Cl2 Cl -0.22425(16) 0.17245(3) 0.59451(11) 0.0533(5) Uani 1 1 d . . . O5 O -0.3199(6) 0.17979(13) 0.5957(6) 0.109(3) Uani 1 1 d . . . O6 O -0.2167(6) 0.16654(10) 0.5251(4) 0.081(2) Uani 1 1 d . . . O7 O -0.1551(6) 0.18758(12) 0.6149(4) 0.089(2) Uani 1 1 d . . . O8 O -0.2080(8) 0.15678(11) 0.6417(4) 0.105(3) Uani 1 1 d . . . Cl3 Cl 1.05483(14) 0.06986(3) 0.37999(9) 0.0445(4) Uani 1 1 d . . . O9 O 1.1568(6) 0.06567(13) 0.3775(6) 0.106(3) Uani 1 1 d . . . O10 O 1.0222(8) 0.08563(10) 0.3361(4) 0.102(3) Uani 1 1 d . . . O11 O 1.0500(6) 0.07463(9) 0.4517(3) 0.0729(19) Uani 1 1 d . . . O12 O 0.9951(5) 0.05331(9) 0.3583(3) 0.0639(16) Uani 1 1 d . . . Cl4 Cl 0.68205(18) -0.08522(3) -0.09396(13) 0.0656(6) Uani 1 1 d . . . O13 O 0.6811(8) -0.0888(2) -0.0253(5) 0.137(4) Uani 1 1 d . . . O14 O 0.6021(6) -0.09949(12) -0.1268(5) 0.094(2) Uani 1 1 d . . . O15 O 0.6416(7) -0.06872(11) -0.1261(4) 0.093(3) Uani 1 1 d . . . O16 O 0.7637(5) -0.09174(9) -0.1220(4) 0.0740(19) Uani 1 1 d . . . Cl5 Cl 0.5205(2) 0.17294(4) 0.88738(19) 0.0837(8) Uani 1 1 d . . . O17 O 0.5979(11) 0.18564(19) 0.9318(8) 0.182(6) Uani 1 1 d . . . O18 O 0.4925(10) 0.1637(2) 0.9452(7) 0.174(6) Uani 1 1 d . . . O19 O 0.4596(8) 0.18634(14) 0.8471(6) 0.129(4) Uani 1 1 d . . . O20 O 0.5823(9) 0.16288(14) 0.8496(7) 0.136(4) Uani 1 1 d . . . Cl6 Cl 0.8455(3) 0.20282(4) 0.24625(17) 0.0888(9) Uani 1 1 d . . . O21 O 0.7725(13) 0.18896(18) 0.2644(9) 0.195(7) Uani 1 1 d . . . O22 O 0.9301(11) 0.19886(16) 0.2976(6) 0.152(5) Uani 1 1 d . . . O23 O 0.8589(10) 0.19972(13) 0.1766(5) 0.124(4) Uani 1 1 d . . . O24 O 0.8114(9) 0.22180(13) 0.2520(5) 0.119(3) Uani 1 1 d . . . Cl7 Cl -0.0250(5) 0.03919(6) 0.73170(19) 0.1371(19) Uani 1 1 d . . . O25 O -0.077(2) 0.0363(3) 0.7882(7) 0.290(14) Uani 1 1 d . . . O26 O 0.011(2) 0.0563(3) 0.7266(17) 0.39(2) Uani 1 1 d . . . O27 O 0.0432(15) 0.0242(3) 0.7363(11) 0.242(10) Uani 1 1 d . . . O28 O -0.0951(12) 0.0375(2) 0.6725(6) 0.171(6) Uani 1 1 d . . . Cl8 Cl 0.3950(3) 0.04329(4) 0.75075(14) 0.0921(10) Uani 1 1 d . . . O29 O 0.3888(9) 0.03197(16) 0.6949(6) 0.135(4) Uani 1 1 d . . . O30 O 0.2848(9) 0.03782(16) 0.7648(8) 0.152(5) Uani 1 1 d . . . O31 O 0.3859(9) 0.06259(13) 0.7444(6) 0.127(4) Uani 1 1 d . . . O32 O 0.4512(8) 0.03686(14) 0.8128(5) 0.115(3) Uani 1 1 d . . . N25 N 0.0239(13) 0.1461(3) 0.9578(9) 0.158(5) Uiso 1 1 d U . . C153 C 0.0336(17) 0.1294(4) 0.9693(12) 0.152(6) Uiso 1 1 d U . . C154 C 0.0559(16) 0.1090(3) 0.9856(11) 0.151(5) Uiso 1 1 d U . . H15C H 0.0854 0.1032 0.9473 0.226 Uiso 1 1 calc R . . H15D H -0.0060 0.1022 0.9899 0.226 Uiso 1 1 calc R . . H15E H 0.1028 0.1080 1.0304 0.226 Uiso 1 1 calc R . . N26 N 0.1330(9) 0.10366(16) 0.6657(6) 0.099(3) Uiso 1 1 d DU . . C155 C 0.1431(11) 0.08926(18) 0.6459(8) 0.097(3) Uiso 1 1 d DU . . C156 C 0.1667(14) 0.0699(2) 0.6229(10) 0.138(5) Uiso 1 1 d DU . . H15F H 0.2036 0.0709 0.5832 0.207 Uiso 1 1 calc R . . H15G H 0.1047 0.0628 0.6076 0.207 Uiso 1 1 calc R . . H15H H 0.2076 0.0632 0.6625 0.207 Uiso 1 1 calc R . . N27 N 0.2213(7) 0.10758(12) 0.8508(5) 0.073(2) Uiso 1 1 d DU . . C157 C 0.2180(8) 0.09167(13) 0.8577(5) 0.064(2) Uiso 1 1 d DU . . C158 C 0.2166(10) 0.07122(15) 0.8690(7) 0.085(3) Uiso 1 1 d DU . . H15I H 0.2835 0.0660 0.8693 0.127 Uiso 1 1 calc R . . H15J H 0.1696 0.0652 0.8307 0.127 Uiso 1 1 calc R . . H15K H 0.1959 0.0686 0.9146 0.127 Uiso 1 1 calc R . . N28 N 0.129(2) -0.0089(4) 0.9676(15) 0.254(9) Uiso 1 1 d DU . . C159 C 0.110(3) 0.0070(4) 0.9658(18) 0.239(9) Uiso 1 1 d DU . . C160 C 0.076(2) 0.0271(4) 0.9596(17) 0.249(9) Uiso 1 1 d DU . . H16A H 0.0808 0.0319 0.9123 0.373 Uiso 1 1 calc R . . H16B H 0.1174 0.0348 0.9957 0.373 Uiso 1 1 calc R . . H16C H 0.0061 0.0277 0.9666 0.373 Uiso 1 1 calc R . . N29 N 0.6008(8) 0.14551(14) 0.1481(5) 0.087(3) Uiso 1 1 d DU . . C161 C 0.6011(8) 0.16090(14) 0.1316(6) 0.074(3) Uiso 1 1 d DU . . C162 C 0.6038(10) 0.18082(16) 0.1085(7) 0.095(3) Uiso 1 1 d DU . . H16D H 0.6646 0.1830 0.0887 0.143 Uiso 1 1 calc R . . H16E H 0.6032 0.1893 0.1492 0.143 Uiso 1 1 calc R . . H16F H 0.5454 0.1835 0.0722 0.143 Uiso 1 1 calc R . . N30 N -0.1971(12) 0.1095(2) 1.0303(8) 0.139(4) Uiso 1 1 d DU . . C163 C -0.2117(13) 0.1251(2) 1.0191(9) 0.120(4) Uiso 1 1 d DU . . C164 C -0.2309(15) 0.1450(2) 1.0008(10) 0.140(5) Uiso 1 1 d DU . . H16G H -0.1910 0.1489 0.9651 0.210 Uiso 1 1 calc R . . H16H H -0.2129 0.1529 1.0433 0.210 Uiso 1 1 calc R . . H16I H -0.3018 0.1467 0.9816 0.210 Uiso 1 1 calc R . . N31 N 0.5924(19) 0.0170(3) 0.4498(13) 0.110(6) Uiso 0.50 1 d PDU . . C165 C 0.610(2) 0.0016(3) 0.4634(16) 0.104(6) Uiso 0.50 1 d PDU . . C166 C 0.615(2) -0.0190(3) 0.4785(16) 0.108(6) Uiso 0.50 1 d PDU . . H16J H 0.5565 -0.0228 0.4991 0.162 Uiso 0.50 1 calc PR . . H16K H 0.6757 -0.0219 0.5121 0.162 Uiso 0.50 1 calc PR . . H16L H 0.6151 -0.0261 0.4344 0.162 Uiso 0.50 1 calc PR . . N32 N 0.7021(14) 0.1445(3) 0.3377(10) 0.161(5) Uiso 1 1 d DU . . C167 C 0.6580(17) 0.1556(3) 0.3588(13) 0.167(6) Uiso 1 1 d DU . . C168 C 0.6077(19) 0.1742(3) 0.3631(13) 0.192(7) Uiso 1 1 d DU . . H16M H 0.6572 0.1845 0.3676 0.289 Uiso 1 1 calc R . . H16N H 0.5742 0.1742 0.4045 0.289 Uiso 1 1 calc R . . H16O H 0.5584 0.1761 0.3199 0.289 Uiso 1 1 calc R . . N33 N -0.043(5) 0.2130(9) 0.954(3) 0.285(18) Uiso 0.50 1 d PDU . . C181 C -0.118(5) 0.2180(12) 0.965(4) 0.282(19) Uiso 0.50 1 d PDU . . C182 C -0.208(5) 0.2222(11) 0.996(4) 0.283(19) Uiso 0.50 1 d PDU . . H18A H -0.2018 0.2162 1.0430 0.425 Uiso 0.50 1 calc PR . . H18B H -0.2671 0.2170 0.9651 0.425 Uiso 0.50 1 calc PR . . H18C H -0.2156 0.2360 1.0006 0.425 Uiso 0.50 1 calc PR . . N34 N 0.260(3) 0.2246(7) 0.518(2) 0.209(12) Uiso 0.50 1 d PDU . . C183 C 0.317(4) 0.2261(9) 0.482(3) 0.215(13) Uiso 0.50 1 d PDU . . C184 C 0.411(4) 0.2302(8) 0.455(3) 0.208(13) Uiso 0.50 1 d PDU . . H18D H 0.4153 0.2440 0.4458 0.312 Uiso 0.50 1 calc PR . . H18E H 0.4125 0.2231 0.4113 0.312 Uiso 0.50 1 calc PR . . H18F H 0.4682 0.2264 0.4910 0.312 Uiso 0.50 1 calc PR . . O33 O -0.2515(16) 0.0543(3) 0.8686(11) 0.232(6) Uiso 1 1 d DU . . C169 C -0.149(2) 0.0592(4) 0.9928(14) 0.235(8) Uiso 1 1 d DU . . H16P H -0.0811 0.0630 0.9884 0.353 Uiso 1 1 calc R . . H16Q H -0.1482 0.0528 1.0386 0.353 Uiso 1 1 calc R . . H16R H -0.1917 0.0705 0.9899 0.353 Uiso 1 1 calc R . . C170 C -0.193(2) 0.0442(4) 0.9276(15) 0.238(9) Uiso 1 1 d DU . . H17B H -0.1369 0.0376 0.9112 0.286 Uiso 1 1 calc R . . H17C H -0.2353 0.0344 0.9454 0.286 Uiso 1 1 calc R . . C171 C -0.296(2) 0.0454(3) 0.8127(13) 0.187(7) Uiso 1 1 d DU . . H17D H -0.3509 0.0377 0.8256 0.224 Uiso 1 1 calc R . . H17E H -0.2478 0.0366 0.7963 0.224 Uiso 1 1 calc R . . C172 C -0.339(2) 0.0591(4) 0.7501(13) 0.212(7) Uiso 1 1 d DU . . H17F H -0.4070 0.0629 0.7547 0.318 Uiso 1 1 calc R . . H17G H -0.3402 0.0525 0.7048 0.318 Uiso 1 1 calc R . . H17H H -0.2970 0.0705 0.7517 0.318 Uiso 1 1 calc R . . O34 O 0.278(2) 0.1841(4) 0.3951(13) 0.150(7) Uiso 0.50 1 d PDU . . C173 C 0.374(3) 0.1595(5) 0.482(2) 0.166(9) Uiso 0.50 1 d PDU . . H17S H 0.3959 0.1557 0.4373 0.249 Uiso 0.50 1 calc PR . . H17T H 0.3484 0.1483 0.5033 0.249 Uiso 0.50 1 calc PR . . H17U H 0.4303 0.1649 0.5142 0.249 Uiso 0.50 1 calc PR . . C174 C 0.286(3) 0.1755(6) 0.4644(18) 0.160(9) Uiso 0.50 1 d PDU . . H17V H 0.2217 0.1694 0.4684 0.192 Uiso 0.50 1 calc PR . . H17W H 0.2985 0.1856 0.5008 0.192 Uiso 0.50 1 calc PR . . C175 C 0.192(3) 0.1921(6) 0.3671(18) 0.157(9) Uiso 0.50 1 d PDU . . H17X H 0.1793 0.2029 0.3974 0.189 Uiso 0.50 1 calc PR . . H17Y H 0.1384 0.1826 0.3674 0.189 Uiso 0.50 1 calc PR . . C176 C 0.188(3) 0.1995(6) 0.2899(17) 0.153(8) Uiso 0.50 1 d PDU . . H17I H 0.2360 0.2099 0.2897 0.230 Uiso 0.50 1 calc PR . . H17J H 0.1206 0.2041 0.2716 0.230 Uiso 0.50 1 calc PR . . H17K H 0.2045 0.1890 0.2599 0.230 Uiso 0.50 1 calc PR . . O35 O 0.4286(19) 0.0935(3) 0.4947(14) 0.152(7) Uiso 0.50 1 d PDU . . C177 C 0.558(3) 0.0665(5) 0.488(2) 0.168(9) Uiso 0.50 1 d PDU . . H17L H 0.5270 0.0607 0.5256 0.252 Uiso 0.50 1 calc PR . . H17M H 0.6308 0.0654 0.5008 0.252 Uiso 0.50 1 calc PR . . H17N H 0.5353 0.0599 0.4432 0.252 Uiso 0.50 1 calc PR . . C178 C 0.527(3) 0.0889(5) 0.480(3) 0.183(10) Uiso 0.50 1 d PDU . . H17O H 0.5771 0.0964 0.5127 0.220 Uiso 0.50 1 calc PR . . H17P H 0.5312 0.0930 0.4312 0.220 Uiso 0.50 1 calc PR . . C179 C 0.417(3) 0.1126(4) 0.492(2) 0.161(9) Uiso 0.50 1 d PDU . . H17Q H 0.4220 0.1172 0.4437 0.193 Uiso 0.50 1 calc PR . . H17R H 0.4715 0.1187 0.5258 0.193 Uiso 0.50 1 calc PR . . C180 C 0.313(3) 0.1185(5) 0.511(2) 0.162(9) Uiso 0.50 1 d PDU . . H18G H 0.2602 0.1113 0.4815 0.243 Uiso 0.50 1 calc PR . . H18H H 0.3022 0.1322 0.5023 0.243 Uiso 0.50 1 calc PR . . H18I H 0.3126 0.1158 0.5612 0.243 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0407(5) 0.0437(5) 0.0300(5) -0.0004(4) 0.0054(4) -0.0013(4) Zn2 0.0380(5) 0.0448(5) 0.0372(5) -0.0042(4) 0.0068(4) -0.0004(4) Zn3 0.0435(6) 0.0420(5) 0.0407(5) 0.0024(4) 0.0093(4) -0.0032(4) Zn4 0.0451(6) 0.0429(5) 0.0432(6) 0.0026(4) 0.0106(4) -0.0004(4) N1 0.041(3) 0.039(3) 0.025(3) -0.002(2) -0.004(2) -0.002(2) N2 0.036(3) 0.038(3) 0.028(3) -0.004(2) 0.001(2) 0.000(2) N3 0.044(4) 0.042(3) 0.031(3) -0.007(2) 0.003(2) 0.000(3) N4 0.044(3) 0.048(3) 0.029(3) 0.000(2) 0.010(2) -0.004(3) N5 0.035(3) 0.055(4) 0.028(3) -0.003(2) 0.003(2) -0.003(3) N6 0.041(4) 0.060(4) 0.032(3) -0.003(3) 0.002(2) 0.006(3) N7 0.041(3) 0.048(4) 0.037(3) 0.007(3) 0.005(3) -0.003(3) N8 0.035(3) 0.049(3) 0.031(3) -0.005(2) 0.007(2) -0.003(3) N9 0.031(3) 0.054(4) 0.036(3) -0.006(3) 0.006(2) 0.001(3) N10 0.042(3) 0.038(3) 0.035(3) -0.002(2) 0.008(3) -0.001(3) N11 0.031(3) 0.048(3) 0.029(3) 0.000(2) 0.006(2) -0.002(2) N12 0.029(3) 0.041(3) 0.037(3) 0.002(2) 0.006(2) -0.002(2) N13 0.043(3) 0.036(3) 0.043(3) 0.003(2) 0.009(3) -0.007(3) N14 0.040(3) 0.035(3) 0.043(3) -0.001(2) 0.003(3) -0.004(3) N15 0.051(4) 0.039(3) 0.045(4) 0.001(3) 0.010(3) -0.006(3) N16 0.040(3) 0.035(3) 0.041(3) 0.001(2) 0.010(3) -0.003(2) N17 0.050(4) 0.038(3) 0.042(3) 0.001(3) 0.014(3) 0.002(3) N18 0.045(4) 0.037(3) 0.053(4) 0.006(3) 0.015(3) 0.008(3) N19 0.057(4) 0.041(3) 0.044(4) 0.006(3) 0.013(3) 0.002(3) N20 0.035(3) 0.048(4) 0.049(4) 0.008(3) 0.007(3) 0.002(3) N21 0.050(4) 0.047(4) 0.045(4) 0.005(3) 0.008(3) -0.004(3) N22 0.050(4) 0.048(4) 0.034(3) 0.001(3) 0.004(3) -0.010(3) N23 0.039(3) 0.055(4) 0.033(3) -0.002(3) 0.008(2) -0.003(3) N24 0.049(4) 0.046(4) 0.037(3) -0.004(3) 0.007(3) 0.001(3) C1 0.041(4) 0.037(4) 0.037(4) -0.002(3) -0.001(3) -0.004(3) C2 0.045(4) 0.044(4) 0.044(4) 0.000(3) 0.009(3) 0.004(3) C3 0.053(5) 0.038(4) 0.068(6) 0.002(4) 0.012(4) 0.008(3) C4 0.064(6) 0.056(5) 0.085(7) 0.000(5) 0.024(5) 0.019(5) C5 0.062(6) 0.064(6) 0.115(9) 0.009(6) 0.049(6) 0.011(5) C6 0.062(6) 0.043(4) 0.075(6) 0.004(4) 0.029(5) -0.002(4) C7 0.046(4) 0.048(4) 0.042(4) 0.002(3) 0.014(3) 0.000(3) C8 0.037(4) 0.042(4) 0.026(3) 0.000(3) 0.003(3) 0.005(3) C9 0.030(4) 0.054(4) 0.032(3) -0.003(3) 0.004(3) 0.001(3) C10 0.034(4) 0.047(4) 0.025(3) -0.006(3) -0.001(3) -0.001(3) C11 0.037(4) 0.042(4) 0.036(4) 0.000(3) -0.005(3) 0.000(3) C12 0.040(4) 0.047(4) 0.050(4) 0.003(3) 0.006(3) 0.002(3) C13 0.066(6) 0.054(5) 0.079(7) -0.001(4) 0.017(5) -0.019(4) C14 0.067(6) 0.037(4) 0.068(6) 0.002(4) 0.000(4) -0.007(4) C15 0.060(5) 0.037(4) 0.051(5) 0.003(3) 0.001(4) 0.000(4) C16 0.043(4) 0.045(4) 0.037(4) -0.008(3) -0.004(3) -0.001(3) C17 0.043(4) 0.044(4) 0.033(4) -0.008(3) 0.000(3) 0.006(3) C18 0.035(4) 0.041(4) 0.024(3) -0.003(3) -0.002(3) 0.000(3) C19 0.038(4) 0.042(4) 0.025(3) -0.004(3) 0.003(3) 0.002(3) C20 0.049(5) 0.064(5) 0.040(4) -0.001(4) 0.011(3) -0.011(4) C21 0.051(5) 0.065(5) 0.036(4) -0.005(3) 0.007(3) -0.013(4) C22 0.073(7) 0.069(6) 0.071(6) 0.001(5) 0.027(5) -0.015(5) C23 0.099(9) 0.068(7) 0.095(8) -0.002(6) 0.052(7) -0.019(6) C24 0.100(9) 0.108(9) 0.091(9) -0.009(7) 0.054(7) -0.050(8) C25 0.059(6) 0.085(7) 0.073(6) -0.008(5) 0.034(5) -0.013(5) C26 0.057(5) 0.066(5) 0.045(4) -0.003(4) 0.015(4) -0.016(4) C27 0.040(4) 0.067(5) 0.034(4) -0.001(3) 0.008(3) 0.001(4) C28 0.041(4) 0.083(6) 0.037(4) 0.000(4) 0.012(3) -0.004(4) C29 0.036(4) 0.075(5) 0.026(3) -0.002(3) 0.002(3) 0.003(4) C30 0.054(5) 0.076(6) 0.029(4) 0.002(3) 0.002(3) 0.009(4) C31 0.056(6) 0.088(7) 0.055(5) 0.007(5) 0.019(4) 0.020(5) C32 0.060(6) 0.107(8) 0.059(6) 0.021(5) 0.019(5) 0.038(6) C33 0.077(7) 0.085(7) 0.055(5) 0.013(5) 0.019(5) 0.041(6) C34 0.061(6) 0.075(6) 0.043(5) 0.011(4) 0.010(4) 0.022(5) C35 0.051(5) 0.076(6) 0.034(4) 0.003(4) 0.005(3) 0.028(4) C36 0.052(5) 0.059(5) 0.033(4) 0.004(3) 0.002(3) 0.008(4) C37 0.043(4) 0.053(4) 0.022(3) -0.001(3) -0.001(3) 0.000(3) C38 0.047(4) 0.058(5) 0.023(3) -0.003(3) -0.001(3) -0.011(4) C39 0.061(5) 0.052(5) 0.045(4) 0.006(4) 0.012(4) -0.004(4) C40 0.072(6) 0.059(5) 0.043(5) 0.014(4) 0.008(4) 0.002(4) C41 0.092(8) 0.056(5) 0.060(6) 0.012(4) 0.002(5) 0.003(5) C42 0.109(9) 0.070(6) 0.062(6) 0.028(5) 0.015(6) 0.030(6) C43 0.093(8) 0.083(7) 0.048(5) 0.027(5) 0.020(5) 0.036(6) C44 0.076(7) 0.083(7) 0.035(4) 0.004(4) 0.007(4) 0.009(5) C45 0.058(5) 0.069(5) 0.037(4) 0.015(4) 0.013(4) 0.012(4) C46 0.052(5) 0.060(5) 0.038(4) 0.003(3) 0.004(3) 0.006(4) C47 0.047(5) 0.076(6) 0.027(4) -0.004(3) 0.002(3) 0.008(4) C48 0.035(4) 0.071(5) 0.038(4) -0.007(4) 0.009(3) 0.001(4) C49 0.043(4) 0.076(6) 0.043(4) -0.019(4) 0.008(3) 0.004(4) C50 0.070(7) 0.089(7) 0.047(5) -0.014(5) 0.000(4) 0.006(5) C51 0.082(8) 0.109(9) 0.042(5) -0.032(5) -0.005(5) 0.006(6) C52 0.069(6) 0.087(7) 0.058(6) -0.033(5) 0.014(5) -0.003(5) C53 0.054(5) 0.072(6) 0.061(6) -0.027(4) 0.014(4) 0.002(4) C54 0.039(4) 0.068(5) 0.045(4) -0.020(4) 0.006(3) 0.004(4) C55 0.039(4) 0.057(5) 0.049(5) -0.011(4) 0.008(3) -0.002(3) C56 0.033(4) 0.058(5) 0.032(3) -0.005(3) 0.007(3) -0.003(3) C57 0.035(4) 0.052(4) 0.036(4) 0.002(3) 0.009(3) -0.001(3) C58 0.042(4) 0.040(4) 0.051(4) -0.003(3) 0.010(3) -0.004(3) C59 0.034(4) 0.049(4) 0.041(4) -0.007(3) 0.008(3) -0.001(3) C60 0.053(5) 0.042(4) 0.065(5) -0.013(4) 0.021(4) -0.003(4) C61 0.047(5) 0.052(5) 0.062(5) -0.019(4) 0.015(4) 0.000(4) C62 0.041(4) 0.078(6) 0.052(5) -0.031(4) 0.007(4) 0.003(4) C63 0.039(4) 0.058(5) 0.048(4) -0.013(3) 0.014(3) 0.004(3) C64 0.033(4) 0.048(4) 0.050(4) -0.012(3) 0.010(3) -0.004(3) C65 0.028(3) 0.051(4) 0.037(4) -0.004(3) 0.010(3) -0.004(3) C66 0.041(4) 0.053(4) 0.028(3) -0.003(3) 0.005(3) 0.003(3) C67 0.032(4) 0.049(4) 0.029(3) -0.001(3) 0.007(3) -0.001(3) C68 0.039(4) 0.053(4) 0.036(4) 0.007(3) 0.010(3) 0.002(3) C69 0.051(5) 0.053(5) 0.045(4) 0.011(3) 0.004(3) -0.004(4) C70 0.075(7) 0.069(6) 0.047(5) 0.011(4) 0.007(4) 0.002(5) C71 0.052(5) 0.054(5) 0.064(6) 0.016(4) -0.001(4) -0.002(4) C72 0.046(5) 0.046(4) 0.054(5) 0.009(3) 0.007(4) -0.005(3) C73 0.027(4) 0.049(4) 0.045(4) 0.001(3) 0.008(3) -0.003(3) C74 0.032(4) 0.039(4) 0.050(4) 0.001(3) 0.015(3) 0.004(3) C75 0.029(3) 0.040(4) 0.032(3) 0.003(3) 0.005(3) -0.002(3) C76 0.028(3) 0.039(4) 0.039(4) -0.004(3) 0.009(3) -0.009(3) C77 0.040(4) 0.035(4) 0.053(4) 0.007(3) 0.003(3) -0.005(3) C78 0.048(4) 0.039(4) 0.044(4) 0.004(3) 0.006(3) -0.004(3) C79 0.053(5) 0.036(4) 0.062(5) 0.005(3) 0.006(4) -0.011(3) C80 0.072(6) 0.046(5) 0.052(5) 0.010(4) -0.001(4) 0.000(4) C81 0.087(7) 0.060(5) 0.046(5) 0.014(4) -0.005(4) -0.013(5) C82 0.071(6) 0.044(4) 0.046(5) 0.002(3) 0.001(4) -0.014(4) C83 0.046(4) 0.041(4) 0.048(4) 0.002(3) 0.010(3) -0.008(3) C84 0.046(4) 0.038(4) 0.044(4) 0.003(3) 0.006(3) -0.005(3) C85 0.057(5) 0.049(4) 0.037(4) 0.000(3) 0.003(3) -0.012(4) C86 0.041(4) 0.036(4) 0.059(5) 0.002(3) 0.009(3) -0.008(3) C87 0.062(5) 0.043(4) 0.061(5) -0.007(4) 0.017(4) -0.008(4) C88 0.072(6) 0.045(5) 0.054(5) -0.004(4) 0.015(4) -0.014(4) C89 0.088(7) 0.048(5) 0.067(6) -0.014(4) 0.024(5) -0.007(5) C90 0.088(7) 0.040(5) 0.065(6) -0.006(4) 0.008(5) -0.003(4) C91 0.093(8) 0.036(4) 0.070(6) 0.002(4) 0.021(5) 0.001(4) C92 0.067(6) 0.041(4) 0.064(6) -0.003(4) 0.015(4) 0.000(4) C93 0.056(5) 0.037(4) 0.066(5) 0.008(4) 0.019(4) 0.005(4) C94 0.043(4) 0.039(4) 0.052(4) 0.005(3) 0.015(3) -0.004(3) C95 0.038(4) 0.039(4) 0.032(3) 0.000(3) 0.002(3) -0.006(3) C96 0.049(5) 0.043(4) 0.050(4) 0.009(3) 0.014(4) 0.002(3) C97 0.046(4) 0.043(4) 0.039(4) -0.002(3) 0.005(3) -0.005(3) C98 0.056(5) 0.046(4) 0.049(5) 0.001(3) 0.007(4) 0.003(4) C99 0.064(6) 0.046(5) 0.059(5) -0.013(4) 0.010(4) 0.000(4) C100 0.091(7) 0.062(6) 0.039(5) -0.008(4) -0.004(4) -0.004(5) C101 0.087(7) 0.055(5) 0.045(5) 0.002(4) 0.002(4) 0.004(5) C102 0.052(5) 0.045(4) 0.043(4) -0.002(3) 0.011(3) -0.001(3) C103 0.042(4) 0.047(4) 0.039(4) -0.003(3) 0.007(3) 0.002(3) C104 0.047(5) 0.047(4) 0.040(4) 0.000(3) 0.002(3) -0.002(3) C105 0.049(5) 0.049(5) 0.049(4) 0.008(3) 0.009(4) 0.008(4) C106 0.052(5) 0.045(4) 0.058(5) 0.013(4) 0.015(4) 0.009(4) C107 0.067(6) 0.050(5) 0.056(5) 0.011(4) 0.006(4) 0.006(4) C108 0.072(6) 0.056(5) 0.065(6) 0.020(4) -0.004(5) 0.004(5) C109 0.067(6) 0.056(6) 0.076(7) 0.024(5) 0.001(5) 0.003(5) C110 0.077(7) 0.042(5) 0.069(6) 0.012(4) 0.007(5) 0.007(4) C111 0.045(5) 0.039(4) 0.060(5) 0.013(3) 0.009(4) 0.000(3) C112 0.059(5) 0.035(4) 0.069(6) 0.003(4) 0.016(4) 0.000(4) C113 0.036(4) 0.038(4) 0.049(4) 0.004(3) 0.007(3) 0.001(3) C114 0.036(4) 0.042(4) 0.049(4) 0.001(3) 0.010(3) -0.001(3) C115 0.042(4) 0.042(4) 0.038(4) 0.003(3) 0.002(3) -0.001(3) C116 0.078(6) 0.043(4) 0.041(4) 0.007(3) 0.012(4) 0.010(4) C117 0.076(6) 0.057(5) 0.032(4) 0.006(3) 0.006(4) 0.008(4) C118 0.089(7) 0.055(5) 0.054(5) -0.001(4) 0.017(5) 0.023(5) C119 0.063(6) 0.084(7) 0.074(7) 0.007(5) 0.021(5) 0.024(5) C120 0.051(5) 0.067(6) 0.076(6) 0.018(5) 0.021(5) 0.019(4) C121 0.056(5) 0.068(6) 0.049(5) 0.005(4) 0.021(4) 0.011(4) C122 0.044(5) 0.060(5) 0.060(5) 0.016(4) 0.012(4) 0.006(4) C123 0.051(6) 0.073(6) 0.103(8) 0.026(6) 0.031(5) 0.008(5) C124 0.059(6) 0.051(5) 0.111(8) 0.013(5) 0.043(6) 0.007(4) C125 0.036(14) 0.071(13) 0.064(14) -0.009(11) 0.019(10) -0.024(11) C126 0.054(14) 0.091(18) 0.092(18) -0.031(15) 0.009(12) 0.004(12) C127 0.081(18) 0.064(13) 0.14(2) 0.025(15) 0.073(18) -0.012(12) C128 0.12(2) 0.051(13) 0.14(2) 0.008(14) 0.09(2) -0.021(13) C129 0.10(2) 0.037(12) 0.080(16) -0.002(10) 0.040(14) -0.024(11) C25' 0.027(12) 0.059(14) 0.13(3) 0.026(16) 0.003(13) -0.021(10) C26' 0.068(16) 0.057(13) 0.23(4) 0.055(19) 0.10(2) 0.022(12) C27' 0.07(2) 0.12(3) 0.23(5) 0.10(3) 0.07(2) 0.016(18) C28' 0.16(4) 0.048(15) 0.22(4) 0.03(2) 0.12(4) 0.007(17) C29' 0.052(15) 0.054(15) 0.20(4) -0.01(2) 0.04(2) -0.003(11) C130 0.053(6) 0.059(6) 0.119(9) 0.025(6) 0.039(6) 0.006(5) C131 0.060(6) 0.053(5) 0.067(6) 0.014(4) 0.020(4) 0.000(4) C132 0.043(4) 0.055(5) 0.048(4) 0.012(4) 0.009(3) -0.001(4) C133 0.043(4) 0.046(4) 0.042(4) 0.008(3) 0.009(3) 0.003(3) C134 0.060(5) 0.050(4) 0.032(4) 0.002(3) -0.003(3) -0.013(4) C135 0.069(6) 0.059(5) 0.030(4) 0.006(3) 0.001(4) -0.024(4) C136 0.084(7) 0.061(5) 0.038(4) 0.008(4) 0.000(4) -0.023(5) C137 0.084(8) 0.072(7) 0.063(6) 0.013(5) 0.011(5) -0.031(6) C138 0.070(7) 0.093(8) 0.069(6) 0.014(5) 0.014(5) -0.042(6) C139 0.056(6) 0.079(6) 0.054(5) -0.002(4) 0.005(4) -0.018(5) C140 0.056(5) 0.074(6) 0.031(4) 0.000(4) 0.004(3) -0.024(4) C141 0.044(4) 0.063(5) 0.035(4) -0.006(3) 0.006(3) -0.010(4) C142 0.045(5) 0.077(6) 0.046(5) -0.006(4) 0.017(4) -0.010(4) C143 0.041(4) 0.062(5) 0.052(5) -0.014(4) 0.015(4) -0.006(4) C144 0.053(6) 0.069(6) 0.104(8) -0.015(5) 0.039(6) -0.003(5) C149 0.055(6) 0.061(5) 0.128(9) -0.025(6) 0.042(6) 0.001(4) C145 0.049(12) 0.066(13) 0.063(15) 0.011(13) 0.037(13) -0.003(9) C146 0.040(12) 0.093(19) 0.13(3) 0.01(2) 0.036(16) -0.001(12) C147 0.053(16) 0.11(2) 0.16(3) -0.05(2) 0.014(18) 0.010(15) C148 0.063(9) 0.064(7) 0.130(12) -0.018(9) 0.039(8) 0.004(7) C45' 0.059(16) 0.091(17) 0.084(19) 0.019(17) 0.060(18) 0.010(12) C46' 0.10(3) 0.074(18) 0.15(3) 0.00(2) 0.06(3) 0.024(16) C47' 0.042(14) 0.065(14) 0.22(4) -0.02(2) 0.062(18) 0.013(11) C48' 0.063(9) 0.067(7) 0.131(12) -0.025(9) 0.038(8) 0.000(7) C150 0.047(5) 0.059(5) 0.059(5) -0.012(4) 0.014(4) -0.006(4) C151 0.044(4) 0.051(4) 0.033(4) -0.004(3) 0.004(3) -0.001(3) C152 0.040(4) 0.052(4) 0.024(3) -0.002(3) 0.000(3) -0.010(3) Cl1 0.157(4) 0.0626(17) 0.123(3) -0.0287(18) 0.057(3) -0.030(2) O1 0.119(10) 0.119(9) 0.288(18) -0.032(10) 0.081(11) -0.002(7) O2 0.167(10) 0.081(6) 0.099(7) -0.019(5) 0.017(6) -0.050(6) O3 0.159(11) 0.097(7) 0.211(13) -0.081(8) -0.055(9) 0.046(7) O4 0.245(16) 0.077(6) 0.195(13) 0.020(7) -0.126(12) -0.057(8) Cl2 0.0556(12) 0.0580(11) 0.0470(10) 0.0125(8) 0.0106(9) 0.0085(9) O5 0.076(6) 0.091(6) 0.170(9) 0.001(6) 0.053(6) 0.002(5) O6 0.117(6) 0.075(5) 0.053(4) 0.011(3) 0.019(4) 0.002(4) O7 0.085(5) 0.114(6) 0.060(4) 0.015(4) -0.011(4) -0.030(5) O8 0.179(10) 0.074(5) 0.055(4) 0.021(4) 0.005(5) 0.030(5) Cl3 0.0495(10) 0.0444(9) 0.0396(9) 0.0046(7) 0.0075(7) 0.0062(8) O9 0.052(4) 0.103(6) 0.172(9) -0.023(6) 0.047(5) -0.004(4) O10 0.185(10) 0.057(4) 0.048(4) -0.002(3) -0.024(5) 0.027(5) O11 0.107(6) 0.068(4) 0.043(3) 0.004(3) 0.009(3) -0.005(4) O12 0.074(4) 0.059(4) 0.054(4) 0.002(3) -0.002(3) -0.009(3) Cl4 0.0636(14) 0.0657(13) 0.0750(15) 0.0199(11) 0.0329(11) 0.0126(11) O13 0.113(8) 0.232(13) 0.063(6) 0.006(7) 0.008(5) 0.021(8) O14 0.081(6) 0.085(5) 0.113(7) -0.009(4) 0.010(5) -0.025(4) O15 0.115(7) 0.072(5) 0.081(5) -0.025(4) -0.014(4) 0.035(4) O16 0.065(4) 0.059(4) 0.105(6) 0.008(3) 0.035(4) 0.008(3) Cl5 0.0721(17) 0.0579(14) 0.132(3) -0.0097(14) 0.0478(17) -0.0053(12) O17 0.161(12) 0.148(11) 0.209(15) 0.047(10) -0.048(10) -0.076(9) O18 0.145(11) 0.247(15) 0.156(11) -0.049(10) 0.097(9) -0.057(10) O19 0.118(8) 0.114(7) 0.132(8) -0.064(6) -0.046(6) 0.061(6) O20 0.138(9) 0.104(7) 0.189(11) 0.028(7) 0.090(8) 0.039(7) Cl6 0.116(3) 0.0690(16) 0.0805(19) -0.0192(13) 0.0157(17) 0.0126(16) O21 0.234(17) 0.114(9) 0.260(18) 0.021(10) 0.107(14) -0.059(10) O22 0.205(13) 0.129(9) 0.098(8) -0.019(6) -0.040(8) 0.056(9) O23 0.212(12) 0.087(6) 0.078(6) -0.006(4) 0.035(7) 0.047(7) O24 0.170(10) 0.076(5) 0.116(8) 0.009(5) 0.044(7) 0.034(6) Cl7 0.241(6) 0.095(2) 0.0640(19) 0.0063(17) -0.007(3) -0.057(3) O25 0.58(4) 0.232(17) 0.077(9) 0.035(10) 0.093(15) 0.16(2) O26 0.36(3) 0.136(13) 0.56(5) 0.12(2) -0.23(3) -0.117(18) O27 0.26(2) 0.220(17) 0.29(2) 0.147(16) 0.183(18) 0.070(15) O28 0.226(16) 0.185(12) 0.093(8) -0.044(8) 0.000(9) -0.051(11) Cl8 0.128(3) 0.0824(18) 0.0566(15) -0.0108(12) -0.0095(15) 0.0425(18) O29 0.162(11) 0.132(8) 0.094(7) -0.039(6) -0.031(7) 0.011(7) O30 0.119(9) 0.113(8) 0.232(15) -0.010(8) 0.054(9) -0.005(7) O31 0.173(11) 0.073(6) 0.122(8) 0.018(5) -0.009(7) -0.026(6) O32 0.130(8) 0.126(7) 0.080(6) 0.026(5) -0.012(5) -0.036(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.135(6) . ? Zn1 N7 2.141(6) . ? Zn1 N4 2.145(6) . ? Zn1 N10 2.193(6) . ? Zn1 N11 2.214(6) . ? Zn1 N8 2.215(6) . ? Zn2 N6 2.129(6) . ? Zn2 N3 2.149(6) . ? Zn2 N12 2.153(6) . ? Zn2 N9 2.156(6) . ? Zn2 N2 2.249(6) . ? Zn2 N5 2.295(6) . ? Zn3 N13 2.109(6) . ? Zn3 N16 2.145(6) . ? Zn3 N19 2.155(7) . ? Zn3 N22 2.164(6) . ? Zn3 N20 2.279(6) . ? Zn3 N23 2.284(6) . ? Zn4 N24 2.134(7) . ? Zn4 N15 2.143(6) . ? Zn4 N21 2.157(7) . ? Zn4 N18 2.182(6) . ? Zn4 N17 2.209(6) . ? Zn4 N14 2.252(6) . ? N1 C1 1.292(9) . ? N1 C19 1.380(9) . ? N2 C19 1.347(9) . ? N2 C18 1.359(9) . ? N3 C17 1.300(9) . ? N3 C18 1.382(9) . ? N4 C20 1.317(10) . ? N4 C38 1.377(10) . ? N5 C37 1.313(9) . ? N5 C38 1.343(10) . ? N6 C36 1.309(10) . ? N6 C37 1.384(10) . ? N7 C39 1.295(10) . ? N7 C57 1.385(10) . ? N8 C57 1.324(9) . ? N8 C56 1.349(9) . ? N9 C55 1.280(10) . ? N9 C56 1.397(10) . ? N10 C58 1.316(9) . ? N10 C76 1.351(9) . ? N11 C75 1.334(9) . ? N11 C76 1.339(9) . ? N12 C74 1.304(9) . ? N12 C75 1.387(9) . ? N13 C77 1.312(9) . ? N13 C95 1.386(9) . ? N14 C94 1.332(9) . ? N14 C95 1.345(9) . ? N15 C93 1.293(10) . ? N15 C94 1.390(10) . ? N16 C96 1.298(10) . ? N16 C114 1.389(9) . ? N17 C113 1.347(9) . ? N17 C114 1.361(9) . ? N18 C112 1.316(10) . ? N18 C113 1.387(10) . ? N19 C115 1.308(9) . ? N19 C133 1.362(10) . ? N20 C132 1.335(10) . ? N20 C133 1.351(10) . ? N21 C131 1.300(10) . ? N21 C132 1.376(10) . ? N22 C134 1.294(10) . ? N22 C152 1.365(10) . ? N23 C151 1.323(10) . ? N23 C152 1.363(9) . ? N24 C150 1.307(10) . ? N24 C151 1.363(10) . ? C1 C2 1.434(11) . ? C2 C3 1.381(10) . ? C2 C7 1.446(11) . ? C3 C4 1.354(13) . ? C4 C5 1.412(14) . ? C5 C6 1.374(12) . ? C6 C7 1.389(11) . ? C7 C8 1.445(10) . ? C8 C9 1.387(10) . ? C8 C19 1.420(10) . ? C9 C10 1.398(10) . ? C10 C18 1.400(10) . ? C10 C11 1.460(10) . ? C11 C12 1.386(10) . ? C11 C16 1.438(10) . ? C12 C13 1.381(12) . ? C13 C14 1.369(13) . ? C14 C15 1.399(12) . ? C15 C16 1.404(11) . ? C16 C17 1.410(11) . ? C20 C21 1.407(11) . ? C21 C26 1.395(13) . ? C21 C22 1.438(12) . ? C22 C23 1.341(14) . ? C23 C24 1.405(17) . ? C24 C25 1.394(15) . ? C25 C26 1.410(12) . ? C26 C27 1.471(12) . ? C27 C28 1.350(12) . ? C27 C38 1.435(11) . ? C28 C29 1.386(12) . ? C29 C37 1.417(10) . ? C29 C30 1.446(12) . ? C30 C31 1.385(12) . ? C30 C35 1.427(13) . ? C31 C32 1.384(14) . ? C32 C33 1.364(16) . ? C33 C34 1.377(13) . ? C34 C35 1.420(12) . ? C35 C36 1.444(11) . ? C39 C40 1.431(11) . ? C40 C45 1.382(13) . ? C40 C41 1.453(13) . ? C41 C42 1.363(13) . ? C42 C43 1.403(16) . ? C43 C44 1.397(13) . ? C44 C45 1.416(11) . ? C45 C46 1.449(12) . ? C46 C47 1.399(12) . ? C46 C57 1.408(10) . ? C47 C48 1.392(12) . ? C48 C56 1.399(10) . ? C48 C49 1.437(11) . ? C49 C50 1.393(12) . ? C49 C54 1.430(13) . ? C50 C51 1.389(14) . ? C51 C52 1.392(16) . ? C52 C53 1.373(13) . ? C53 C54 1.403(11) . ? C54 C55 1.433(11) . ? C58 C59 1.414(10) . ? C59 C64 1.411(11) . ? C59 C60 1.411(10) . ? C60 C61 1.370(12) . ? C61 C62 1.372(13) . ? C62 C63 1.404(12) . ? C63 C64 1.410(11) . ? C64 C65 1.444(10) . ? C65 C66 1.369(10) . ? C65 C76 1.426(9) . ? C66 C67 1.406(10) . ? C67 C75 1.405(9) . ? C67 C68 1.464(10) . ? C68 C73 1.384(11) . ? C68 C69 1.404(10) . ? C69 C70 1.398(12) . ? C70 C71 1.394(13) . ? C71 C72 1.322(12) . ? C72 C73 1.411(11) . ? C73 C74 1.417(10) . ? C77 C78 1.414(11) . ? C78 C83 1.416(10) . ? C78 C79 1.425(11) . ? C79 C80 1.368(12) . ? C80 C81 1.389(13) . ? C81 C82 1.382(12) . ? C82 C83 1.404(11) . ? C83 C84 1.415(10) . ? C84 C85 1.407(11) . ? C84 C95 1.437(10) . ? C85 C86 1.404(11) . ? C86 C94 1.388(11) . ? C86 C87 1.456(11) . ? C87 C88 1.403(12) . ? C87 C92 1.425(13) . ? C88 C89 1.398(12) . ? C89 C90 1.372(14) . ? C90 C91 1.384(13) . ? C91 C92 1.390(12) . ? C92 C93 1.418(12) . ? C96 C97 1.432(11) . ? C97 C102 1.386(11) . ? C97 C98 1.419(11) . ? C98 C99 1.341(12) . ? C99 C100 1.397(13) . ? C100 C101 1.385(12) . ? C101 C102 1.417(11) . ? C102 C103 1.451(10) . ? C103 C104 1.396(11) . ? C103 C114 1.407(10) . ? C104 C105 1.371(11) . ? C105 C113 1.403(11) . ? C105 C106 1.465(11) . ? C106 C107 1.399(12) . ? C106 C111 1.405(12) . ? C107 C108 1.395(12) . ? C108 C109 1.369(14) . ? C109 C110 1.354(13) . ? C110 C111 1.423(11) . ? C111 C112 1.400(12) . ? C115 C116 1.446(12) . ? C116 C117 1.397(11) . ? C116 C121 1.429(12) . ? C117 C118 1.365(13) . ? C118 C119 1.386(15) . ? C119 C120 1.390(13) . ? C120 C121 1.390(12) . ? C121 C122 1.443(12) . ? C122 C123 1.373(13) . ? C122 C133 1.428(11) . ? C123 C124 1.348(13) . ? C124 C132 1.436(12) . ? C124 C25' 1.46(3) . ? C124 C125 1.57(3) . ? C125 C126 1.34(4) . ? C125 C130 1.45(3) . ? C126 C127 1.42(4) . ? C127 C128 1.43(4) . ? C128 C129 1.33(4) . ? C129 C130 1.49(2) . ? C25' C26' 1.43(4) . ? C25' C130 1.46(3) . ? C26' C27' 1.46(3) . ? C27' C28' 1.33(4) . ? C28' C29' 1.38(4) . ? C29' C130 1.40(4) . ? C130 C131 1.394(12) . ? C134 C135 1.415(12) . ? C135 C140 1.419(13) . ? C135 C136 1.424(12) . ? C136 C137 1.363(14) . ? C137 C138 1.377(16) . ? C138 C139 1.384(14) . ? C139 C140 1.417(12) . ? C140 C141 1.438(12) . ? C141 C142 1.397(12) . ? C141 C152 1.409(10) . ? C142 C143 1.382(12) . ? C143 C144 1.424(13) . ? C143 C151 1.451(11) . ? C144 C145 1.39(3) . ? C144 C149 1.420(14) . ? C144 C45' 1.48(3) . ? C149 C48' 1.39(3) . ? C149 C150 1.414(12) . ? C149 C148 1.52(3) . ? C145 C146 1.41(4) . ? C146 C147 1.43(5) . ? C147 C148 1.37(4) . ? C45' C46' 1.39(5) . ? C46' C47' 1.39(4) . ? C47' C48' 1.42(3) . ? Cl1 O4 1.289(11) . ? Cl1 O3 1.347(11) . ? Cl1 O2 1.378(9) . ? Cl1 O1 1.520(12) . ? Cl2 O5 1.404(8) . ? Cl2 O6 1.410(7) . ? Cl2 O8 1.412(7) . ? Cl2 O7 1.425(8) . ? Cl3 O10 1.411(7) . ? Cl3 O11 1.424(6) . ? Cl3 O9 1.428(7) . ? Cl3 O12 1.434(6) . ? Cl4 O13 1.340(10) . ? Cl4 O15 1.377(8) . ? Cl4 O16 1.391(7) . ? Cl4 O14 1.530(8) . ? Cl5 O18 1.388(13) . ? Cl5 O20 1.391(10) . ? Cl5 O19 1.393(9) . ? Cl5 O17 1.521(12) . ? Cl6 O23 1.392(9) . ? Cl6 O22 1.408(11) . ? Cl6 O24 1.416(9) . ? Cl6 O21 1.470(12) . ? Cl7 O26 1.306(16) . ? Cl7 O28 1.356(13) . ? Cl7 O27 1.392(17) . ? Cl7 O25 1.41(2) . ? Cl8 O29 1.321(10) . ? Cl8 O31 1.359(9) . ? Cl8 O32 1.372(9) . ? Cl8 O30 1.614(12) . ? N25 C153 1.19(2) . ? C153 C154 1.48(3) . ? N26 C155 1.092(11) . ? C155 C156 1.476(14) . ? N27 C157 1.122(10) . ? C157 C158 1.447(11) . ? N28 C159 1.143(15) . ? C159 C160 1.475(16) . ? N29 C161 1.121(10) . ? C161 C162 1.464(12) . ? N30 C163 1.121(12) . ? C163 C164 1.448(14) . ? N31 C165 1.129(14) . ? C165 C166 1.470(15) . ? N32 C167 1.098(14) . ? C167 C168 1.476(15) . ? N33 C181 1.130(17) . ? C181 C182 1.479(17) . ? N34 C183 1.132(16) . ? C183 C184 1.481(17) . ? O33 C171 1.29(2) . ? O33 C170 1.45(2) . ? C169 C170 1.66(3) . ? C171 C172 1.57(2) . ? O34 C175 1.32(2) . ? O34 C174 1.44(3) . ? C173 C174 1.63(3) . ? C175 C176 1.55(3) . ? O35 C179 1.35(2) . ? O35 C178 1.46(3) . ? C177 C178 1.62(3) . ? C179 C180 1.58(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N7 91.5(2) . . ? N1 Zn1 N4 175.7(2) . . ? N7 Zn1 N4 90.9(2) . . ? N1 Zn1 N10 90.1(2) . . ? N7 Zn1 N10 102.7(2) . . ? N4 Zn1 N10 93.0(2) . . ? N1 Zn1 N11 87.2(2) . . ? N7 Zn1 N11 163.8(2) . . ? N4 Zn1 N11 91.6(2) . . ? N10 Zn1 N11 61.2(2) . . ? N1 Zn1 N8 89.8(2) . . ? N7 Zn1 N8 62.1(2) . . ? N4 Zn1 N8 88.1(2) . . ? N10 Zn1 N8 164.7(2) . . ? N11 Zn1 N8 134.1(2) . . ? N6 Zn2 N3 108.0(2) . . ? N6 Zn2 N12 92.8(2) . . ? N3 Zn2 N12 91.8(2) . . ? N6 Zn2 N9 92.2(2) . . ? N3 Zn2 N9 93.8(2) . . ? N12 Zn2 N9 170.9(2) . . ? N6 Zn2 N2 169.6(2) . . ? N3 Zn2 N2 61.8(2) . . ? N12 Zn2 N2 86.4(2) . . ? N9 Zn2 N2 90.0(2) . . ? N6 Zn2 N5 60.6(2) . . ? N3 Zn2 N5 168.6(2) . . ? N12 Zn2 N5 88.0(2) . . ? N9 Zn2 N5 87.8(2) . . ? N2 Zn2 N5 129.6(2) . . ? N13 Zn3 N16 171.8(2) . . ? N13 Zn3 N19 94.8(2) . . ? N16 Zn3 N19 90.5(2) . . ? N13 Zn3 N22 92.4(2) . . ? N16 Zn3 N22 91.8(2) . . ? N19 Zn3 N22 108.8(2) . . ? N13 Zn3 N20 91.0(2) . . ? N16 Zn3 N20 86.1(2) . . ? N19 Zn3 N20 61.1(2) . . ? N22 Zn3 N20 169.6(2) . . ? N13 Zn3 N23 87.7(2) . . ? N16 Zn3 N23 88.1(2) . . ? N19 Zn3 N23 170.0(2) . . ? N22 Zn3 N23 61.3(2) . . ? N20 Zn3 N23 128.7(2) . . ? N24 Zn4 N15 91.5(2) . . ? N24 Zn4 N21 174.9(2) . . ? N15 Zn4 N21 91.8(3) . . ? N24 Zn4 N18 94.4(2) . . ? N15 Zn4 N18 104.7(2) . . ? N21 Zn4 N18 88.5(2) . . ? N24 Zn4 N17 90.2(2) . . ? N15 Zn4 N17 166.4(2) . . ? N21 Zn4 N17 87.4(2) . . ? N18 Zn4 N17 61.7(2) . . ? N24 Zn4 N14 88.3(2) . . ? N15 Zn4 N14 61.5(2) . . ? N21 Zn4 N14 90.0(2) . . ? N18 Zn4 N14 166.1(2) . . ? N17 Zn4 N14 132.1(2) . . ? C1 N1 C19 117.8(6) . . ? C1 N1 Zn1 120.0(5) . . ? C19 N1 Zn1 122.2(5) . . ? C19 N2 C18 117.6(6) . . ? C19 N2 Zn2 150.7(5) . . ? C18 N2 Zn2 91.7(4) . . ? C17 N3 C18 118.0(6) . . ? C17 N3 Zn2 146.5(5) . . ? C18 N3 Zn2 95.4(4) . . ? C20 N4 C38 118.4(7) . . ? C20 N4 Zn1 119.4(6) . . ? C38 N4 Zn1 122.2(5) . . ? C37 N5 C38 119.3(7) . . ? C37 N5 Zn2 91.0(5) . . ? C38 N5 Zn2 149.7(5) . . ? C36 N6 C37 119.0(7) . . ? C36 N6 Zn2 144.7(6) . . ? C37 N6 Zn2 96.3(5) . . ? C39 N7 C57 119.5(7) . . ? C39 N7 Zn1 146.9(6) . . ? C57 N7 Zn1 93.7(4) . . ? C57 N8 C56 118.5(6) . . ? C57 N8 Zn1 92.2(4) . . ? C56 N8 Zn1 149.3(5) . . ? C55 N9 C56 117.8(7) . . ? C55 N9 Zn2 118.9(6) . . ? C56 N9 Zn2 123.3(5) . . ? C58 N10 C76 119.2(6) . . ? C58 N10 Zn1 147.5(5) . . ? C76 N10 Zn1 93.1(4) . . ? C75 N11 C76 119.5(6) . . ? C75 N11 Zn1 147.9(5) . . ? C76 N11 Zn1 92.5(4) . . ? C74 N12 C75 117.7(6) . . ? C74 N12 Zn2 118.5(5) . . ? C75 N12 Zn2 123.7(4) . . ? C77 N13 C95 117.3(7) . . ? C77 N13 Zn3 119.7(5) . . ? C95 N13 Zn3 123.0(5) . . ? C94 N14 C95 118.9(6) . . ? C94 N14 Zn4 91.9(5) . . ? C95 N14 Zn4 149.2(5) . . ? C93 N15 C94 117.8(7) . . ? C93 N15 Zn4 147.2(6) . . ? C94 N15 Zn4 95.0(5) . . ? C96 N16 C114 117.0(7) . . ? C96 N16 Zn3 118.0(5) . . ? C114 N16 Zn3 125.0(5) . . ? C113 N17 C114 117.7(7) . . ? C113 N17 Zn4 93.7(5) . . ? C114 N17 Zn4 148.6(5) . . ? C112 N18 C113 116.7(7) . . ? C112 N18 Zn4 149.6(6) . . ? C113 N18 Zn4 93.7(4) . . ? C115 N19 C133 118.6(7) . . ? C115 N19 Zn3 145.4(6) . . ? C133 N19 Zn3 95.8(5) . . ? C132 N20 C133 118.4(7) . . ? C132 N20 Zn3 150.8(6) . . ? C133 N20 Zn3 90.6(4) . . ? C131 N21 C132 119.2(8) . . ? C131 N21 Zn4 119.2(6) . . ? C132 N21 Zn4 121.4(5) . . ? C134 N22 C152 118.3(7) . . ? C134 N22 Zn3 146.1(6) . . ? C152 N22 Zn3 95.6(4) . . ? C151 N23 C152 119.9(7) . . ? C151 N23 Zn3 149.7(5) . . ? C152 N23 Zn3 90.4(5) . . ? C150 N24 C151 118.8(7) . . ? C150 N24 Zn4 119.2(6) . . ? C151 N24 Zn4 122.0(5) . . ? N1 C1 C2 126.2(7) . . ? C3 C2 C1 122.7(7) . . ? C3 C2 C7 120.5(7) . . ? C1 C2 C7 116.8(7) . . ? C4 C3 C2 120.4(8) . . ? C3 C4 C5 120.0(8) . . ? C6 C5 C4 120.8(9) . . ? C5 C6 C7 120.4(8) . . ? C6 C7 C8 124.5(7) . . ? C6 C7 C2 117.8(7) . . ? C8 C7 C2 117.8(7) . . ? C9 C8 C19 119.0(6) . . ? C9 C8 C7 123.0(7) . . ? C19 C8 C7 117.9(6) . . ? C8 C9 C10 120.1(7) . . ? C9 C10 C18 116.8(7) . . ? C9 C10 C11 125.2(7) . . ? C18 C10 C11 118.0(6) . . ? C12 C11 C16 119.1(7) . . ? C12 C11 C10 125.6(7) . . ? C16 C11 C10 115.4(6) . . ? C13 C12 C11 119.7(8) . . ? C14 C13 C12 122.7(9) . . ? C13 C14 C15 119.2(8) . . ? C14 C15 C16 120.0(8) . . ? C15 C16 C17 120.2(7) . . ? C15 C16 C11 119.3(7) . . ? C17 C16 C11 120.5(7) . . ? N3 C17 C16 123.8(7) . . ? N2 C18 N3 111.1(6) . . ? N2 C18 C10 124.6(6) . . ? N3 C18 C10 124.4(6) . . ? N2 C19 N1 114.7(6) . . ? N2 C19 C8 121.9(6) . . ? N1 C19 C8 123.5(6) . . ? N4 C20 C21 123.1(8) . . ? C26 C21 C20 121.2(8) . . ? C26 C21 C22 118.8(8) . . ? C20 C21 C22 120.0(9) . . ? C23 C22 C21 120.1(10) . . ? C22 C23 C24 120.5(10) . . ? C25 C24 C23 121.9(10) . . ? C24 C25 C26 117.3(10) . . ? C21 C26 C25 121.4(8) . . ? C21 C26 C27 117.5(8) . . ? C25 C26 C27 121.1(9) . . ? C28 C27 C38 117.7(8) . . ? C28 C27 C26 126.4(8) . . ? C38 C27 C26 115.8(8) . . ? C27 C28 C29 122.4(8) . . ? C28 C29 C37 115.5(8) . . ? C28 C29 C30 126.7(8) . . ? C37 C29 C30 117.8(8) . . ? C31 C30 C35 118.7(9) . . ? C31 C30 C29 124.5(9) . . ? C35 C30 C29 116.8(8) . . ? C32 C31 C30 120.4(11) . . ? C33 C32 C31 120.9(10) . . ? C32 C33 C34 121.7(10) . . ? C33 C34 C35 118.4(10) . . ? C34 C35 C30 119.9(8) . . ? C34 C35 C36 119.9(9) . . ? C30 C35 C36 120.2(8) . . ? N6 C36 C35 122.3(8) . . ? N5 C37 N6 112.1(7) . . ? N5 C37 C29 124.1(7) . . ? N6 C37 C29 123.8(7) . . ? N5 C38 N4 115.1(7) . . ? N5 C38 C27 121.0(8) . . ? N4 C38 C27 123.9(7) . . ? N7 C39 C40 121.5(8) . . ? C45 C40 C39 121.6(8) . . ? C45 C40 C41 120.6(8) . . ? C39 C40 C41 117.7(8) . . ? C42 C41 C40 118.4(10) . . ? C41 C42 C43 120.4(9) . . ? C44 C43 C42 122.4(9) . . ? C43 C44 C45 117.6(9) . . ? C40 C45 C44 120.5(8) . . ? C40 C45 C46 116.9(7) . . ? C44 C45 C46 122.6(8) . . ? C47 C46 C57 115.4(7) . . ? C47 C46 C45 127.1(8) . . ? C57 C46 C45 117.5(7) . . ? C48 C47 C46 121.0(7) . . ? C47 C48 C56 118.2(7) . . ? C47 C48 C49 123.1(8) . . ? C56 C48 C49 118.7(8) . . ? C50 C49 C54 118.5(8) . . ? C50 C49 C48 124.7(9) . . ? C54 C49 C48 116.8(7) . . ? C51 C50 C49 119.4(10) . . ? C50 C51 C52 122.5(9) . . ? C53 C52 C51 118.8(9) . . ? C52 C53 C54 120.5(10) . . ? C53 C54 C49 120.2(8) . . ? C53 C54 C55 121.2(9) . . ? C49 C54 C55 118.6(7) . . ? N9 C55 C54 124.9(8) . . ? N8 C56 N9 114.8(6) . . ? N8 C56 C48 121.9(7) . . ? N9 C56 C48 123.3(7) . . ? N8 C57 N7 112.1(6) . . ? N8 C57 C46 124.9(7) . . ? N7 C57 C46 123.0(7) . . ? N10 C58 C59 122.6(7) . . ? C64 C59 C60 120.4(7) . . ? C64 C59 C58 120.0(7) . . ? C60 C59 C58 119.5(7) . . ? C61 C60 C59 119.5(8) . . ? C60 C61 C62 120.7(8) . . ? C61 C62 C63 121.7(8) . . ? C62 C63 C64 118.6(8) . . ? C59 C64 C63 119.0(7) . . ? C59 C64 C65 117.5(7) . . ? C63 C64 C65 123.4(7) . . ? C66 C65 C76 116.3(6) . . ? C66 C65 C64 127.0(7) . . ? C76 C65 C64 116.7(7) . . ? C65 C66 C67 121.5(7) . . ? C75 C67 C66 117.7(6) . . ? C75 C67 C68 118.7(6) . . ? C66 C67 C68 123.6(6) . . ? C73 C68 C69 120.4(7) . . ? C73 C68 C67 116.5(7) . . ? C69 C68 C67 123.1(7) . . ? C70 C69 C68 118.8(8) . . ? C71 C70 C69 119.7(9) . . ? C72 C71 C70 120.9(8) . . ? C71 C72 C73 121.6(8) . . ? C68 C73 C72 118.6(7) . . ? C68 C73 C74 119.9(7) . . ? C72 C73 C74 121.5(7) . . ? N12 C74 C73 124.7(7) . . ? N11 C75 N12 115.7(6) . . ? N11 C75 C67 121.9(6) . . ? N12 C75 C67 122.4(6) . . ? N11 C76 N10 113.0(6) . . ? N11 C76 C65 123.1(6) . . ? N10 C76 C65 123.8(6) . . ? N13 C77 C78 124.9(7) . . ? C77 C78 C83 119.4(7) . . ? C77 C78 C79 120.8(7) . . ? C83 C78 C79 119.9(7) . . ? C80 C79 C78 120.3(8) . . ? C79 C80 C81 119.3(8) . . ? C82 C81 C80 122.3(9) . . ? C81 C82 C83 119.7(8) . . ? C82 C83 C84 124.3(7) . . ? C82 C83 C78 118.5(7) . . ? C84 C83 C78 117.2(7) . . ? C85 C84 C83 124.1(7) . . ? C85 C84 C95 117.0(7) . . ? C83 C84 C95 118.9(7) . . ? C86 C85 C84 120.3(7) . . ? C94 C86 C85 117.2(7) . . ? C94 C86 C87 118.2(7) . . ? C85 C86 C87 124.5(8) . . ? C88 C87 C92 119.5(8) . . ? C88 C87 C86 124.3(8) . . ? C92 C87 C86 116.2(8) . . ? C89 C88 C87 118.4(9) . . ? C90 C89 C88 122.4(9) . . ? C89 C90 C91 119.4(8) . . ? C90 C91 C92 120.7(9) . . ? C91 C92 C93 120.9(8) . . ? C91 C92 C87 119.5(9) . . ? C93 C92 C87 119.4(7) . . ? N15 C93 C92 124.4(8) . . ? N14 C94 N15 111.6(7) . . ? N14 C94 C86 124.6(7) . . ? N15 C94 C86 123.8(7) . . ? N14 C95 N13 115.7(6) . . ? N14 C95 C84 122.0(6) . . ? N13 C95 C84 122.3(6) . . ? N16 C96 C97 125.1(7) . . ? C102 C97 C98 120.7(7) . . ? C102 C97 C96 119.0(7) . . ? C98 C97 C96 120.4(7) . . ? C99 C98 C97 119.9(8) . . ? C98 C99 C100 120.1(8) . . ? C101 C100 C99 121.8(8) . . ? C100 C101 C102 118.4(8) . . ? C97 C102 C101 119.1(7) . . ? C97 C102 C103 117.6(7) . . ? C101 C102 C103 123.3(7) . . ? C104 C103 C114 117.7(7) . . ? C104 C103 C102 124.2(7) . . ? C114 C103 C102 118.0(7) . . ? C105 C104 C103 121.4(7) . . ? C104 C105 C113 117.0(7) . . ? C104 C105 C106 126.6(8) . . ? C113 C105 C106 116.4(7) . . ? C107 C106 C111 120.1(7) . . ? C107 C106 C105 122.7(8) . . ? C111 C106 C105 117.1(8) . . ? C108 C107 C106 118.6(9) . . ? C109 C108 C107 121.7(9) . . ? C110 C109 C108 120.3(9) . . ? C109 C110 C111 120.8(9) . . ? C112 C111 C106 120.4(7) . . ? C112 C111 C110 121.1(8) . . ? C106 C111 C110 118.4(8) . . ? N18 C112 C111 124.3(8) . . ? N17 C113 N18 110.9(7) . . ? N17 C113 C105 124.0(7) . . ? N18 C113 C105 125.1(7) . . ? N17 C114 N16 114.6(7) . . ? N17 C114 C103 122.1(7) . . ? N16 C114 C103 123.3(7) . . ? N19 C115 C116 123.8(7) . . ? C117 C116 C121 121.0(9) . . ? C117 C116 C115 120.7(8) . . ? C121 C116 C115 118.3(7) . . ? C118 C117 C116 119.7(9) . . ? C117 C118 C119 120.1(9) . . ? C118 C119 C120 121.3(9) . . ? C121 C120 C119 120.2(10) . . ? C120 C121 C116 117.6(8) . . ? C120 C121 C122 124.4(9) . . ? C116 C121 C122 117.9(8) . . ? C123 C122 C133 116.1(8) . . ? C123 C122 C121 126.7(8) . . ? C133 C122 C121 117.2(8) . . ? C124 C123 C122 122.0(9) . . ? C123 C124 C132 119.0(9) . . ? C123 C124 C25' 127.0(15) . . ? C132 C124 C25' 112.3(14) . . ? C123 C124 C125 122.9(13) . . ? C132 C124 C125 116.6(12) . . ? C25' C124 C125 25.8(12) . . ? C126 C125 C130 124(2) . . ? C126 C125 C124 123(2) . . ? C130 C125 C124 110.5(15) . . ? C125 C126 C127 115(3) . . ? C126 C127 C128 123(2) . . ? C129 C128 C127 120(2) . . ? C128 C129 C130 118(2) . . ? C26' C25' C130 118(2) . . ? C26' C25' C124 121(2) . . ? C130 C25' C124 116(2) . . ? C25' C26' C27' 121(2) . . ? C28' C27' C26' 118(3) . . ? C27' C28' C29' 120(3) . . ? C28' C29' C130 126(3) . . ? C131 C130 C29' 119.3(14) . . ? C131 C130 C125 122.4(12) . . ? C29' C130 C125 116.6(17) . . ? C131 C130 C25' 114.5(13) . . ? C29' C130 C25' 111.0(19) . . ? C125 C130 C25' 27.2(11) . . ? C131 C130 C129 118.4(14) . . ? C29' C130 C129 32.0(16) . . ? C125 C130 C129 115.9(17) . . ? C25' C130 C129 126.5(16) . . ? N21 C131 C130 124.3(9) . . ? N20 C132 N21 115.6(7) . . ? N20 C132 C124 121.1(8) . . ? N21 C132 C124 123.4(7) . . ? N20 C133 N19 112.5(7) . . ? N20 C133 C122 123.4(7) . . ? N19 C133 C122 124.1(7) . . ? N22 C134 C135 123.5(9) . . ? C134 C135 C140 120.2(8) . . ? C134 C135 C136 120.6(9) . . ? C140 C135 C136 119.2(8) . . ? C137 C136 C135 120.3(11) . . ? C136 C137 C138 120.0(10) . . ? C137 C138 C139 122.6(9) . . ? C138 C139 C140 118.6(10) . . ? C139 C140 C135 119.2(8) . . ? C139 C140 C141 124.5(9) . . ? C135 C140 C141 116.2(7) . . ? C142 C141 C152 116.3(7) . . ? C142 C141 C140 125.9(8) . . ? C152 C141 C140 117.8(8) . . ? C143 C142 C141 121.5(8) . . ? C142 C143 C144 124.9(8) . . ? C142 C143 C151 118.1(8) . . ? C144 C143 C151 117.0(8) . . ? C145 C144 C149 114.1(14) . . ? C145 C144 C143 126.3(15) . . ? C149 C144 C143 118.5(8) . . ? C145 C144 C45' 26.1(14) . . ? C149 C144 C45' 120.7(16) . . ? C143 C144 C45' 118.4(15) . . ? C48' C149 C150 117.3(14) . . ? C48' C149 C144 122.1(14) . . ? C150 C149 C144 118.5(9) . . ? C48' C149 C148 30.6(14) . . ? C150 C149 C148 119.9(14) . . ? C144 C149 C148 118.8(13) . . ? C144 C145 C146 124(2) . . ? C145 C146 C147 124(2) . . ? C146 C147 C148 110(3) . . ? C149 C148 C147 126(3) . . ? C46' C45' C144 115(3) . . ? C45' C46' C47' 119(3) . . ? C48' C47' C46' 126(2) . . ? C149 C48' C47' 113(2) . . ? N24 C150 C149 124.3(9) . . ? N23 C151 N24 116.6(7) . . ? N23 C151 C143 120.8(7) . . ? N24 C151 C143 122.7(7) . . ? N23 C152 N22 112.6(6) . . ? N23 C152 C141 123.4(7) . . ? N22 C152 C141 124.0(7) . . ? O4 Cl1 O3 116.4(9) . . ? O4 Cl1 O2 112.4(7) . . ? O3 Cl1 O2 114.8(8) . . ? O4 Cl1 O1 107.1(12) . . ? O3 Cl1 O1 98.7(9) . . ? O2 Cl1 O1 105.5(8) . . ? O5 Cl2 O6 109.8(6) . . ? O5 Cl2 O8 108.5(6) . . ? O6 Cl2 O8 110.2(5) . . ? O5 Cl2 O7 107.2(6) . . ? O6 Cl2 O7 108.9(5) . . ? O8 Cl2 O7 112.2(5) . . ? O10 Cl3 O11 109.2(4) . . ? O10 Cl3 O9 110.5(6) . . ? O11 Cl3 O9 106.6(6) . . ? O10 Cl3 O12 110.7(5) . . ? O11 Cl3 O12 110.5(4) . . ? O9 Cl3 O12 109.3(5) . . ? O13 Cl4 O15 121.7(7) . . ? O13 Cl4 O16 117.3(6) . . ? O15 Cl4 O16 112.7(5) . . ? O13 Cl4 O14 98.8(7) . . ? O15 Cl4 O14 99.3(5) . . ? O16 Cl4 O14 100.8(5) . . ? O18 Cl5 O20 116.8(8) . . ? O18 Cl5 O19 122.4(9) . . ? O20 Cl5 O19 114.1(7) . . ? O18 Cl5 O17 94.9(9) . . ? O20 Cl5 O17 99.3(9) . . ? O19 Cl5 O17 101.9(7) . . ? O23 Cl6 O22 114.2(8) . . ? O23 Cl6 O24 108.5(6) . . ? O22 Cl6 O24 111.7(7) . . ? O23 Cl6 O21 109.1(9) . . ? O22 Cl6 O21 102.2(10) . . ? O24 Cl6 O21 110.9(8) . . ? O26 Cl7 O28 103.9(12) . . ? O26 Cl7 O27 116.0(17) . . ? O28 Cl7 O27 110.7(13) . . ? O26 Cl7 O25 116(2) . . ? O28 Cl7 O25 104.6(14) . . ? O27 Cl7 O25 105.3(9) . . ? O29 Cl8 O31 122.0(7) . . ? O29 Cl8 O32 116.9(7) . . ? O31 Cl8 O32 115.6(6) . . ? O29 Cl8 O30 93.5(8) . . ? O31 Cl8 O30 100.2(7) . . ? O32 Cl8 O30 100.1(7) . . ? N25 C153 C154 175(2) . . ? N26 C155 C156 174.5(18) . . ? N27 C157 C158 177.9(12) . . ? N28 C159 C160 175(4) . . ? N29 C161 C162 178.1(13) . . ? N30 C163 C164 177(2) . . ? N31 C165 C166 170(3) . . ? N32 C167 C168 158(3) . . ? N33 C181 C182 166(9) . . ? N34 C183 C184 162(6) . . ? C171 O33 C170 122(2) . . ? O33 C170 C169 111(2) . . ? O33 C171 C172 113(2) . . ? C175 O34 C174 119(2) . . ? O34 C174 C173 114(3) . . ? O34 C175 C176 115(3) . . ? C179 O35 C178 108(2) . . ? O35 C178 C177 115(3) . . ? O35 C179 C180 111(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 68.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.798 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.136 # Attachment '- ic14419-re-revised Fe.cif' data_ic14419 _database_code_depnum_ccdc_archive 'CCDC 875009' #TrackingRef '- ic14419-re-revised Fe.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H62.50 Cl4 Fe2 N16.50 O16.50' _chemical_formula_weight 1856.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.6597(4) _cell_length_b 70.1804(14) _cell_length_c 19.0319(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.028(3) _cell_angle_gamma 90.00 _cell_volume 17966.1(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9466 _cell_measurement_theta_min 3.1459 _cell_measurement_theta_max 77.8386 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7616 _exptl_absorpt_coefficient_mu 4.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82132 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67258 _diffrn_reflns_av_R_equivalents 0.0897 _diffrn_reflns_av_sigmaI/netI 0.1711 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -84 _diffrn_reflns_limit_k_max 76 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 67.99 _reflns_number_total 32643 _reflns_number_gt 15173 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. During the structure refinement, the atoms of the (MeCN & Ether) solvent molecule were observed but could not be modelled satisfactorily. The geometrical and anisotropic restraints are applied, Some of MeCN were refined isotropically with restrained geometry. 2323 parameters refined using 377 restraints. H atoms were placed in calculated positions and treated as riding atoms using SHELXL default parameters ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 32643 _refine_ls_number_parameters 2323 _refine_ls_number_restraints 377 _refine_ls_R_factor_all 0.1870 _refine_ls_R_factor_gt 0.1002 _refine_ls_wR_factor_ref 0.2711 _refine_ls_wR_factor_gt 0.2382 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.28681(9) 0.037812(16) 0.25990(6) 0.0255(3) Uani 1 1 d . . . Fe2 Fe 0.31247(9) 0.083716(16) 0.25444(6) 0.0256(3) Uani 1 1 d . . . N1 N 0.1397(5) 0.04220(9) 0.2867(3) 0.0259(14) Uani 1 1 d . . . N2 N 0.1665(5) 0.07425(9) 0.2846(3) 0.0240(13) Uani 1 1 d . . . N3 N 0.2057(5) 0.10531(9) 0.2782(3) 0.0270(14) Uani 1 1 d . . . N4 N 0.4332(5) 0.03413(9) 0.2311(3) 0.0250(13) Uani 1 1 d . . . N5 N 0.4470(5) 0.06666(9) 0.2308(3) 0.0275(14) Uani 1 1 d . . . N6 N 0.4460(5) 0.09874(9) 0.2339(4) 0.0301(14) Uani 1 1 d . . . N7 N 0.2254(5) 0.01791(9) 0.1763(4) 0.0288(14) Uani 1 1 d . . . N8 N 0.2353(5) 0.04902(9) 0.1516(3) 0.0242(13) Uani 1 1 d . . . N9 N 0.2505(5) 0.08131(9) 0.1417(3) 0.0260(13) Uani 1 1 d . . . N10 N 0.3215(5) 0.01769(9) 0.3510(4) 0.0280(14) Uani 1 1 d . . . N11 N 0.3493(5) 0.04917(9) 0.3664(3) 0.0249(13) Uani 1 1 d . . . N12 N 0.3729(5) 0.08154(9) 0.3680(3) 0.0243(13) Uani 1 1 d . . . C1 C 0.0834(6) 0.02759(11) 0.2954(4) 0.0317(18) Uani 1 1 d . . . H1A H 0.1080 0.0152 0.2885 0.038 Uiso 1 1 calc R . . C2 C -0.0133(6) 0.02916(12) 0.3148(5) 0.0339(18) Uani 1 1 d . . . C3 C -0.0683(7) 0.01295(12) 0.3255(5) 0.041(2) Uani 1 1 d . . . H3A H -0.0425 0.0007 0.3186 0.049 Uiso 1 1 calc R . . C4 C -0.1576(7) 0.01470(14) 0.3455(6) 0.047(2) Uani 1 1 d . . . H4A H -0.1938 0.0037 0.3544 0.057 Uiso 1 1 calc R . . C5 C -0.1974(8) 0.03298(14) 0.3533(6) 0.053(3) Uani 1 1 d . . . H5A H -0.2620 0.0343 0.3647 0.064 Uiso 1 1 calc R . . C6 C -0.1427(8) 0.04876(14) 0.3443(6) 0.048(2) Uani 1 1 d . . . H6A H -0.1695 0.0610 0.3510 0.058 Uiso 1 1 calc R . . C7 C -0.0506(7) 0.04749(12) 0.3261(5) 0.0336(18) Uani 1 1 d . . . C8 C 0.0113(6) 0.06363(11) 0.3164(4) 0.0269(16) Uani 1 1 d . . . C9 C -0.0156(6) 0.08233(11) 0.3251(4) 0.0289(16) Uani 1 1 d . . . H9A H -0.0775 0.0850 0.3391 0.035 Uiso 1 1 calc R . . C10 C 0.0470(6) 0.09735(11) 0.3136(4) 0.0289(17) Uani 1 1 d . . . C11 C 0.0263(6) 0.11752(12) 0.3197(4) 0.0294(17) Uani 1 1 d . . . C12 C -0.0622(7) 0.12503(12) 0.3392(5) 0.0354(19) Uani 1 1 d . . . H12A H -0.1131 0.1167 0.3486 0.042 Uiso 1 1 calc R . . C13 C -0.0738(7) 0.14445(13) 0.3444(5) 0.044(2) Uani 1 1 d . . . H13A H -0.1330 0.1494 0.3572 0.053 Uiso 1 1 calc R . . C14 C 0.0014(7) 0.15710(12) 0.3309(5) 0.042(2) Uani 1 1 d . . . H14A H -0.0075 0.1705 0.3350 0.050 Uiso 1 1 calc R . . C15 C 0.0870(7) 0.15016(12) 0.3117(4) 0.0355(19) Uani 1 1 d . . . H15A H 0.1368 0.1588 0.3023 0.043 Uiso 1 1 calc R . . C16 C 0.1016(6) 0.13032(11) 0.3061(4) 0.0289(17) Uani 1 1 d . . . C17 C 0.1890(6) 0.12307(12) 0.2853(4) 0.0323(18) Uani 1 1 d . . . H17A H 0.2380 0.1319 0.2762 0.039 Uiso 1 1 calc R . . C18 C 0.1373(6) 0.09207(10) 0.2926(4) 0.0259(16) Uani 1 1 d . . . C19 C 0.1046(6) 0.06014(11) 0.2958(4) 0.0253(16) Uani 1 1 d . . . C20 C 0.4701(6) 0.01754(11) 0.2220(4) 0.0323(18) Uani 1 1 d . . . H20A H 0.4307 0.0068 0.2286 0.039 Uiso 1 1 calc R . . C21 C 0.5638(7) 0.01405(12) 0.2031(5) 0.0358(19) Uani 1 1 d . . . C22 C 0.5975(8) -0.00484(13) 0.1952(6) 0.047(2) Uani 1 1 d . . . H22A H 0.5558 -0.0154 0.2009 0.057 Uiso 1 1 calc R . . C23 C 0.6886(9) -0.00778(14) 0.1796(6) 0.056(3) Uani 1 1 d . . . H23A H 0.7105 -0.0204 0.1736 0.068 Uiso 1 1 calc R . . C24 C 0.7540(9) 0.00809(15) 0.1720(6) 0.057(3) Uani 1 1 d . . . H24A H 0.8192 0.0058 0.1630 0.068 Uiso 1 1 calc R . . C25 C 0.7210(8) 0.02676(14) 0.1778(5) 0.044(2) Uani 1 1 d . . . H25A H 0.7622 0.0373 0.1711 0.053 Uiso 1 1 calc R . . C26 C 0.6262(7) 0.02965(12) 0.1936(5) 0.0361(19) Uani 1 1 d . . . C27 C 0.5863(7) 0.04853(12) 0.2036(4) 0.0318(18) Uani 1 1 d . . . C28 C 0.6375(6) 0.06513(12) 0.1969(4) 0.0323(18) Uani 1 1 d . . . H28A H 0.7026 0.0646 0.1858 0.039 Uiso 1 1 calc R . . C29 C 0.5941(6) 0.08297(12) 0.2062(4) 0.0300(17) Uani 1 1 d . . . C30 C 0.6411(6) 0.10136(12) 0.2007(4) 0.0313(17) Uani 1 1 d . . . C31 C 0.7354(7) 0.10406(13) 0.1862(5) 0.039(2) Uani 1 1 d . . . H31A H 0.7752 0.0934 0.1793 0.047 Uiso 1 1 calc R . . C32 C 0.7723(8) 0.12218(14) 0.1818(5) 0.047(2) Uani 1 1 d . . . H32A H 0.8377 0.1239 0.1720 0.056 Uiso 1 1 calc R . . C33 C 0.7147(8) 0.13814(13) 0.1915(5) 0.047(2) Uani 1 1 d . . . H33A H 0.7411 0.1506 0.1882 0.056 Uiso 1 1 calc R . . C34 C 0.6226(7) 0.13603(13) 0.2054(5) 0.040(2) Uani 1 1 d . . . H34A H 0.5840 0.1470 0.2111 0.048 Uiso 1 1 calc R . . C35 C 0.5823(7) 0.11781(12) 0.2116(4) 0.0331(18) Uani 1 1 d . . . C36 C 0.4861(7) 0.11522(12) 0.2284(4) 0.0348(19) Uani 1 1 d . . . H36A H 0.4489 0.1262 0.2361 0.042 Uiso 1 1 calc R . . C37 C 0.4982(6) 0.08256(11) 0.2229(4) 0.0270(16) Uani 1 1 d . . . C38 C 0.4915(6) 0.04985(11) 0.2220(4) 0.0290(17) Uani 1 1 d . . . C39 C 0.2030(7) 0.00040(11) 0.1580(5) 0.0352(19) Uani 1 1 d . . . H39A H 0.2146 -0.0092 0.1937 0.042 Uiso 1 1 calc R . . C40 C 0.1613(7) -0.00512(13) 0.0859(5) 0.041(2) Uani 1 1 d . . . C41 C 0.1369(8) -0.02420(13) 0.0704(6) 0.052(3) Uani 1 1 d . . . H41A H 0.1477 -0.0336 0.1071 0.062 Uiso 1 1 calc R . . C42 C 0.0971(9) -0.02923(14) 0.0020(6) 0.052(3) Uani 1 1 d . . . H42A H 0.0795 -0.0421 -0.0086 0.063 Uiso 1 1 calc R . . C43 C 0.0819(8) -0.01579(14) -0.0523(5) 0.047(2) Uani 1 1 d . . . H43A H 0.0550 -0.0196 -0.0996 0.056 Uiso 1 1 calc R . . C44 C 0.1055(7) 0.00268(14) -0.0380(5) 0.044(2) Uani 1 1 d . . . H44A H 0.0948 0.0118 -0.0755 0.052 Uiso 1 1 calc R . . C45 C 0.1451(6) 0.00861(12) 0.0308(4) 0.0327(18) Uani 1 1 d . . . C46 C 0.1699(6) 0.02872(12) 0.0521(4) 0.0324(18) Uani 1 1 d . . . C47 C 0.1589(6) 0.04450(12) 0.0080(4) 0.0329(18) Uani 1 1 d . . . H47A H 0.1336 0.0430 -0.0414 0.039 Uiso 1 1 calc R . . C48 C 0.1844(6) 0.06235(11) 0.0352(4) 0.0300(17) Uani 1 1 d . . . C49 C 0.1742(6) 0.07938(12) -0.0090(5) 0.0345(19) Uani 1 1 d . . . C50 C 0.1387(8) 0.07954(15) -0.0815(5) 0.049(2) Uani 1 1 d . . . H50A H 0.1189 0.0680 -0.1059 0.059 Uiso 1 1 calc R . . C51 C 0.1321(8) 0.09669(15) -0.1187(5) 0.054(3) Uani 1 1 d . . . H51A H 0.1073 0.0968 -0.1685 0.065 Uiso 1 1 calc R . . C52 C 0.1618(8) 0.11375(14) -0.0833(5) 0.049(2) Uani 1 1 d . . . H52A H 0.1572 0.1254 -0.1094 0.059 Uiso 1 1 calc R . . C53 C 0.1970(7) 0.11393(13) -0.0124(5) 0.044(2) Uani 1 1 d . . . H53A H 0.2175 0.1256 0.0111 0.053 Uiso 1 1 calc R . . C54 C 0.2033(6) 0.09678(12) 0.0263(5) 0.0341(18) Uani 1 1 d . . . C55 C 0.2400(6) 0.09647(11) 0.1018(4) 0.0314(17) Uani 1 1 d . . . H55A H 0.2581 0.1083 0.1244 0.038 Uiso 1 1 calc R . . C56 C 0.2235(5) 0.06400(11) 0.1086(4) 0.0266(16) Uani 1 1 d . . . C57 C 0.2092(6) 0.03185(11) 0.1243(4) 0.0288(17) Uani 1 1 d . . . C58 C 0.3233(6) -0.00012(11) 0.3753(5) 0.0312(18) Uani 1 1 d . . . H58A H 0.3040 -0.0102 0.3424 0.037 Uiso 1 1 calc R . . C59 C 0.3533(6) -0.00459(11) 0.4488(5) 0.0315(18) Uani 1 1 d . . . C60 C 0.3553(6) -0.02400(12) 0.4694(5) 0.0353(19) Uani 1 1 d . . . H60A H 0.3371 -0.0337 0.4349 0.042 Uiso 1 1 calc R . . C61 C 0.3838(6) -0.02842(12) 0.5398(5) 0.038(2) Uani 1 1 d . . . H61A H 0.3856 -0.0414 0.5544 0.046 Uiso 1 1 calc R . . C62 C 0.4104(6) -0.01414(13) 0.5907(5) 0.040(2) Uani 1 1 d . . . H62A H 0.4298 -0.0176 0.6394 0.048 Uiso 1 1 calc R . . C63 C 0.4091(6) 0.00500(12) 0.5719(4) 0.0319(18) Uani 1 1 d . . . H63A H 0.4267 0.0146 0.6069 0.038 Uiso 1 1 calc R . . C64 C 0.3809(6) 0.00972(12) 0.4991(5) 0.0303(17) Uani 1 1 d . . . C65 C 0.3806(6) 0.02934(11) 0.4729(4) 0.0282(17) Uani 1 1 d . . . C66 C 0.4126(6) 0.04568(11) 0.5124(4) 0.0295(17) Uani 1 1 d . . . H66A H 0.4346 0.0447 0.5624 0.035 Uiso 1 1 calc R . . C67 C 0.4128(5) 0.06330(11) 0.4800(4) 0.0249(16) Uani 1 1 d . . . C68 C 0.4477(6) 0.08034(12) 0.5184(4) 0.0318(18) Uani 1 1 d . . . C69 C 0.4886(7) 0.08096(13) 0.5912(5) 0.039(2) Uani 1 1 d . . . H69A H 0.4936 0.0697 0.6193 0.046 Uiso 1 1 calc R . . C70 C 0.5221(8) 0.09845(14) 0.6221(5) 0.047(2) Uani 1 1 d . . . H70A H 0.5504 0.0989 0.6713 0.057 Uiso 1 1 calc R . . C71 C 0.5148(7) 0.11511(13) 0.5823(5) 0.044(2) Uani 1 1 d . . . H71A H 0.5364 0.1268 0.6049 0.053 Uiso 1 1 calc R . . C72 C 0.4773(7) 0.11493(12) 0.5118(5) 0.0366(19) Uani 1 1 d . . . H72A H 0.4749 0.1264 0.4849 0.044 Uiso 1 1 calc R . . C73 C 0.4415(6) 0.09762(11) 0.4778(4) 0.0274(16) Uani 1 1 d . . . C74 C 0.4035(6) 0.09711(10) 0.4036(4) 0.0267(16) Uani 1 1 d . . . H74A H 0.3999 0.1088 0.3779 0.032 Uiso 1 1 calc R . . C75 C 0.3787(5) 0.06442(10) 0.4055(4) 0.0235(15) Uani 1 1 d . . . C76 C 0.3519(5) 0.03200(10) 0.3993(4) 0.0249(16) Uani 1 1 d . . . Fe3 Fe 0.85080(10) 0.166698(18) 0.75353(7) 0.0300(3) Uani 1 1 d . . . Fe4 Fe 0.87343(10) 0.213162(18) 0.76771(7) 0.0301(3) Uani 1 1 d . . . N13 N 0.7926(5) 0.17054(9) 0.6426(4) 0.0297(14) Uani 1 1 d . . . N14 N 0.8100(5) 0.20304(9) 0.6560(4) 0.0293(14) Uani 1 1 d . . . N15 N 0.8334(5) 0.23426(9) 0.6837(4) 0.0329(15) Uani 1 1 d . . . N16 N 0.9124(5) 0.16595(9) 0.8668(4) 0.0290(14) Uani 1 1 d . . . N17 N 0.9221(5) 0.19873(10) 0.8722(3) 0.0304(15) Uani 1 1 d . . . N18 N 0.9234(5) 0.23059(9) 0.8644(4) 0.0303(15) Uani 1 1 d . . . N19 N 0.9654(6) 0.14702(9) 0.7285(4) 0.0343(16) Uani 1 1 d . . . N20 N 0.9998(5) 0.17860(10) 0.7331(4) 0.0304(15) Uani 1 1 d . . . N21 N 1.0234(5) 0.21095(10) 0.7460(4) 0.0342(16) Uani 1 1 d . . . N22 N 0.7229(6) 0.14968(10) 0.7725(4) 0.0346(16) Uani 1 1 d . . . N23 N 0.7173(5) 0.18143(10) 0.7858(4) 0.0329(15) Uani 1 1 d . . . N24 N 0.7242(5) 0.21408(9) 0.7938(4) 0.0313(15) Uani 1 1 d . . . C77 C 0.7656(6) 0.15605(11) 0.6009(4) 0.0317(18) Uani 1 1 d . . . H77A H 0.7703 0.1438 0.6222 0.038 Uiso 1 1 calc R . . C78 C 0.7295(6) 0.15708(11) 0.5256(4) 0.0299(17) Uani 1 1 d . . . C79 C 0.7031(7) 0.14070(12) 0.4850(5) 0.038(2) Uani 1 1 d . . . H79A H 0.7083 0.1286 0.5076 0.046 Uiso 1 1 calc R . . C80 C 0.6697(7) 0.14196(13) 0.4129(5) 0.043(2) Uani 1 1 d . . . H80A H 0.6540 0.1308 0.3852 0.052 Uiso 1 1 calc R . . C81 C 0.6593(7) 0.15959(13) 0.3811(5) 0.044(2) Uani 1 1 d . . . H81A H 0.6337 0.1604 0.3315 0.053 Uiso 1 1 calc R . . C82 C 0.6841(8) 0.17593(13) 0.4179(5) 0.044(2) Uani 1 1 d . . . H82A H 0.6775 0.1879 0.3942 0.053 Uiso 1 1 calc R . . C83 C 0.7201(6) 0.17485(11) 0.4926(4) 0.0317(17) Uani 1 1 d . . . C84 C 0.7476(6) 0.19155(11) 0.5376(4) 0.0294(17) Uani 1 1 d . . . C85 C 0.7394(6) 0.21040(12) 0.5126(4) 0.0336(18) Uani 1 1 d . . . H85A H 0.7146 0.2129 0.4637 0.040 Uiso 1 1 calc R . . C86 C 0.7675(6) 0.22515(11) 0.5592(4) 0.0315(18) Uani 1 1 d . . . C87 C 0.7582(7) 0.24560(12) 0.5399(5) 0.0360(19) Uani 1 1 d . . . C88 C 0.7182(7) 0.25251(12) 0.4726(5) 0.0374(19) Uani 1 1 d . . . H88A H 0.6969 0.2438 0.4348 0.045 Uiso 1 1 calc R . . C89 C 0.7089(7) 0.27181(12) 0.4601(5) 0.040(2) Uani 1 1 d . . . H89A H 0.6816 0.2764 0.4138 0.048 Uiso 1 1 calc R . . C90 C 0.7393(8) 0.28445(12) 0.5148(6) 0.047(2) Uani 1 1 d . . . H90A H 0.7331 0.2978 0.5060 0.057 Uiso 1 1 calc R . . C91 C 0.7785(8) 0.27806(12) 0.5817(5) 0.045(2) Uani 1 1 d . . . H91A H 0.7995 0.2869 0.6191 0.054 Uiso 1 1 calc R . . C92 C 0.7874(7) 0.25877(12) 0.5948(5) 0.041(2) Uani 1 1 d . . . C93 C 0.8254(7) 0.25213(12) 0.6654(5) 0.040(2) Uani 1 1 d . . . H93A H 0.8460 0.2614 0.7013 0.049 Uiso 1 1 calc R . . C94 C 0.8021(6) 0.22070(11) 0.6296(5) 0.0312(18) Uani 1 1 d . . . C95 C 0.7826(6) 0.18865(11) 0.6118(4) 0.0288(17) Uani 1 1 d . . . C96 C 0.9255(7) 0.14939(12) 0.8984(5) 0.037(2) Uani 1 1 d . . . H96A H 0.9105 0.1383 0.8699 0.045 Uiso 1 1 calc R . . C97 C 0.9612(7) 0.14677(12) 0.9737(5) 0.0358(19) Uani 1 1 d . . . C98 C 0.9687(7) 0.12835(12) 1.0029(5) 0.041(2) Uani 1 1 d . . . H98A H 0.9533 0.1176 0.9728 0.049 Uiso 1 1 calc R . . C99 C 0.9977(7) 0.12600(13) 1.0732(5) 0.044(2) Uani 1 1 d . . . H99A H 1.0014 0.1136 1.0932 0.053 Uiso 1 1 calc R . . C100 C 1.0227(8) 0.14189(14) 1.1177(5) 0.054(3) Uani 1 1 d . . . H10A H 1.0440 0.1401 1.1675 0.064 Uiso 1 1 calc R . . C101 C 1.0167(8) 0.16022(13) 1.0896(5) 0.044(2) Uani 1 1 d . . . H10B H 1.0342 0.1709 1.1200 0.052 Uiso 1 1 calc R . . C102 C 0.9848(6) 0.16297(12) 1.0167(4) 0.0312(17) Uani 1 1 d . . . C103 C 0.9714(6) 0.18141(11) 0.9819(4) 0.0299(17) Uani 1 1 d . . . C104 C 0.9921(6) 0.19868(12) 1.0185(4) 0.0348(19) Uani 1 1 d . . . H10C H 1.0169 0.1986 1.0683 0.042 Uiso 1 1 calc R . . C105 C 0.9767(6) 0.21573(12) 0.9827(5) 0.0331(18) Uani 1 1 d . . . C106 C 0.9931(6) 0.23451(12) 1.0146(5) 0.0344(19) Uani 1 1 d . . . C107 C 1.0299(7) 0.23736(13) 1.0861(5) 0.0372(19) Uani 1 1 d . . . H10D H 1.0439 0.2268 1.1177 0.045 Uiso 1 1 calc R . . C108 C 1.0463(8) 0.25605(15) 1.1114(6) 0.051(3) Uani 1 1 d . . . H10E H 1.0748 0.2581 1.1600 0.061 Uiso 1 1 calc R . . C109 C 1.0216(9) 0.27186(14) 1.0667(6) 0.055(3) Uani 1 1 d . . . H10F H 1.0296 0.2844 1.0856 0.066 Uiso 1 1 calc R . . C110 C 0.9863(8) 0.26913(13) 0.9962(6) 0.052(3) Uani 1 1 d . . . H11A H 0.9719 0.2797 0.9651 0.063 Uiso 1 1 calc R . . C111 C 0.9712(7) 0.25040(12) 0.9698(5) 0.039(2) Uani 1 1 d . . . C112 C 0.9381(7) 0.24736(12) 0.8942(5) 0.037(2) Uani 1 1 d . . . H11B H 0.9262 0.2583 0.8643 0.045 Uiso 1 1 calc R . . C113 C 0.9436(6) 0.21502(11) 0.9097(4) 0.0293(17) Uani 1 1 d . . . C114 C 0.9353(6) 0.18208(11) 0.9073(4) 0.0298(17) Uani 1 1 d . . . C115 C 0.9875(7) 0.12963(13) 0.7194(4) 0.038(2) Uani 1 1 d . . . H11C H 0.9404 0.1201 0.7255 0.045 Uiso 1 1 calc R . . C116 C 1.0809(7) 0.12370(13) 0.7001(4) 0.040(2) Uani 1 1 d . . . C117 C 1.1002(8) 0.10417(14) 0.6892(5) 0.048(3) Uani 1 1 d . . . H11D H 1.0514 0.0949 0.6945 0.058 Uiso 1 1 calc R . . C118 C 1.1865(9) 0.09870(15) 0.6714(5) 0.055(3) Uani 1 1 d . . . H11E H 1.1989 0.0856 0.6636 0.066 Uiso 1 1 calc R . . C119 C 1.2589(9) 0.11252(17) 0.6644(6) 0.063(3) Uani 1 1 d . . . H11F H 1.3196 0.1086 0.6510 0.076 Uiso 1 1 calc R . . C120 C 1.2437(8) 0.13151(15) 0.6765(5) 0.049(2) Uani 1 1 d . . . H12B H 1.2945 0.1406 0.6732 0.058 Uiso 1 1 calc R . . C121 C 1.1537(7) 0.13736(14) 0.6937(5) 0.041(2) Uani 1 1 d . . . C122 C 1.1281(7) 0.15697(13) 0.7043(4) 0.037(2) Uani 1 1 d . . . C123 C 1.1901(7) 0.17284(14) 0.7013(5) 0.044(2) Uani 1 1 d . . . H12C H 1.2541 0.1711 0.6891 0.053 Uiso 1 1 calc R . . C124 C 1.1586(6) 0.19128(13) 0.7160(5) 0.0363(19) Uani 1 1 d . . . C125 C 1.2205(9) 0.20794(15) 0.7173(6) 0.055(3) Uani 1 1 d . . . C126 C 1.3170(9) 0.20771(18) 0.7034(9) 0.077(4) Uani 1 1 d . . . H12D H 1.3454 0.1961 0.6906 0.092 Uiso 1 1 calc R . . C127 C 1.3710(12) 0.2241(2) 0.7081(12) 0.125(5) Uani 1 1 d U . . H12E H 1.4375 0.2237 0.6997 0.150 Uiso 1 1 calc R . . C128 C 1.3310(12) 0.2416(2) 0.7251(12) 0.127(5) Uani 1 1 d U . . H12F H 1.3698 0.2529 0.7290 0.152 Uiso 1 1 calc R . . C129 C 1.2345(11) 0.24191(18) 0.7357(11) 0.119(5) Uani 1 1 d U . . H12G H 1.2057 0.2538 0.7449 0.143 Uiso 1 1 calc R . . C130 C 1.1776(8) 0.22559(15) 0.7335(7) 0.057(3) Uani 1 1 d . . . C131 C 1.0797(7) 0.22557(13) 0.7481(5) 0.043(2) Uani 1 1 d . . . H13B H 1.0535 0.2374 0.7605 0.052 Uiso 1 1 calc R . . C132 C 1.0607(7) 0.19354(12) 0.7316(4) 0.0346(19) Uani 1 1 d . . . C133 C 1.0325(6) 0.16086(11) 0.7220(4) 0.0307(18) Uani 1 1 d . . . C134 C 0.6865(7) 0.13265(12) 0.7783(4) 0.0342(18) Uani 1 1 d . . . H13C H 0.7242 0.1220 0.7671 0.041 Uiso 1 1 calc R . . C135 C 0.5928(7) 0.12897(12) 0.8004(4) 0.0360(19) Uani 1 1 d . . . C136 C 0.5607(8) 0.11035(13) 0.8061(4) 0.043(2) Uani 1 1 d . . . H13D H 0.6013 0.1001 0.7959 0.052 Uiso 1 1 calc R . . C137 C 0.4710(9) 0.10666(13) 0.8263(5) 0.051(3) Uani 1 1 d . . . H13E H 0.4492 0.0939 0.8303 0.061 Uiso 1 1 calc R . . C138 C 0.4117(9) 0.12209(15) 0.8410(6) 0.055(3) Uani 1 1 d . . . H13F H 0.3485 0.1197 0.8537 0.066 Uiso 1 1 calc R . . C139 C 0.4448(8) 0.14065(14) 0.8370(6) 0.051(3) Uani 1 1 d . . . H13G H 0.4051 0.1510 0.8482 0.061 Uiso 1 1 calc R . . C140 C 0.5341(7) 0.14414(13) 0.8171(5) 0.039(2) Uani 1 1 d . . . C141 C 0.5767(7) 0.16291(13) 0.8146(5) 0.041(2) Uani 1 1 d . . . C142 C 0.5347(8) 0.17996(14) 0.8335(6) 0.051(3) Uani 1 1 d . . . H14B H 0.4728 0.1797 0.8497 0.061 Uiso 1 1 calc R . . C143 C 0.5827(7) 0.19747(13) 0.8288(6) 0.046(2) Uani 1 1 d . . . C144 C 0.5437(11) 0.21574(16) 0.8498(10) 0.095(3) Uani 1 1 d U . . C145 C 0.4703(11) 0.21729(18) 0.8867(10) 0.105(3) Uani 1 1 d U . . H14C H 0.4367 0.2060 0.8969 0.126 Uiso 1 1 calc R . . C146 C 0.4398(12) 0.23496(18) 0.9115(11) 0.109(3) Uani 1 1 d U . . H14D H 0.3886 0.2356 0.9393 0.130 Uiso 1 1 calc R . . C147 C 0.4900(11) 0.25218(18) 0.8927(11) 0.107(3) Uani 1 1 d U . . H14E H 0.4687 0.2644 0.9049 0.129 Uiso 1 1 calc R . . C148 C 0.5679(11) 0.25030(16) 0.8573(10) 0.099(3) Uani 1 1 d U . . H14F H 0.6026 0.2613 0.8456 0.119 Uiso 1 1 calc R . . C149 C 0.5964(10) 0.23225(15) 0.8382(10) 0.092(3) Uani 1 1 d U . . C150 C 0.6863(7) 0.23049(12) 0.8085(5) 0.0364(19) Uani 1 1 d . . . H15B H 0.7198 0.2418 0.7991 0.044 Uiso 1 1 calc R . . C151 C 0.6741(7) 0.19766(12) 0.8021(5) 0.0350(19) Uani 1 1 d . . . C152 C 0.6699(6) 0.16503(12) 0.7907(4) 0.0317(18) Uani 1 1 d . . . Cl1 Cl -0.05881(15) 0.07089(3) 0.11685(11) 0.0334(4) Uani 1 1 d . . . O1 O 0.0051(5) 0.05500(9) 0.1406(4) 0.0505(17) Uani 1 1 d . . . O2 O -0.0358(6) 0.08670(9) 0.1647(4) 0.0563(19) Uani 1 1 d . . . O3 O -0.0476(6) 0.07612(10) 0.0453(4) 0.0563(19) Uani 1 1 d . . . O4 O -0.1582(6) 0.06531(11) 0.1168(5) 0.070(2) Uani 1 1 d . . . Cl2 Cl 0.5441(2) 0.21346(4) 0.27186(16) 0.0598(7) Uani 1 1 d . . . O5 O 0.4398(8) 0.21492(14) 0.2789(7) 0.101(4) Uani 1 1 d . . . O6 O 0.5672(8) 0.19387(12) 0.2623(5) 0.089(3) Uani 1 1 d . . . O7 O 0.6022(9) 0.22074(14) 0.3325(6) 0.113(4) Uani 1 1 d . . . O8 O 0.5575(9) 0.22466(14) 0.2116(6) 0.110(4) Uani 1 1 d . . . Cl3 Cl 0.22718(18) 0.17107(3) 0.90653(12) 0.0414(5) Uani 1 1 d . . . O9 O 0.1538(6) 0.18559(13) 0.8845(4) 0.070(2) Uani 1 1 d . . . O10 O 0.2209(8) 0.16540(12) 0.9774(4) 0.080(3) Uani 1 1 d . . . O11 O 0.2125(8) 0.15533(11) 0.8594(4) 0.081(3) Uani 1 1 d . . . O12 O 0.3215(7) 0.17853(12) 0.9064(6) 0.093(4) Uani 1 1 d . . . Cl4 Cl 0.4794(2) 0.17278(4) 0.61137(18) 0.0620(7) Uani 1 1 d . . . O13 O 0.5420(8) 0.18588(15) 0.6508(7) 0.125(5) Uani 1 1 d . . . O14 O 0.4244(10) 0.16253(17) 0.6518(7) 0.127(5) Uani 1 1 d . . . O15 O 0.5115(11) 0.1626(2) 0.5568(8) 0.151(6) Uani 1 1 d . . . O16 O 0.3990(11) 0.1850(2) 0.5667(8) 0.165(7) Uani 1 1 d . . . Cl5 Cl 0.6082(3) 0.04345(4) 0.74876(15) 0.0775(11) Uani 1 1 d . . . O17 O 0.6154(8) 0.06262(12) 0.7534(5) 0.093(3) Uani 1 1 d . . . O18 O 0.5523(7) 0.03703(13) 0.6862(5) 0.082(3) Uani 1 1 d . . . O19 O 0.6078(9) 0.03307(16) 0.8085(6) 0.111(4) Uani 1 1 d . . . O20 O 0.7156(9) 0.03791(15) 0.7351(8) 0.127(5) Uani 1 1 d . . . Cl6 Cl 0.1435(2) 0.20372(4) 0.25595(15) 0.0609(7) Uani 1 1 d . . . O21 O 0.1845(8) 0.22207(12) 0.2500(6) 0.086(3) Uani 1 1 d . . . O22 O 0.0596(12) 0.20063(18) 0.2064(7) 0.162(7) Uani 1 1 d . . . O23 O 0.1273(11) 0.20078(14) 0.3247(5) 0.116(5) Uani 1 1 d . . . O24 O 0.2132(12) 0.18951(18) 0.2430(12) 0.203(10) Uani 1 1 d . . . Cl7 Cl 0.6804(2) 0.08534(4) 0.40578(16) 0.0597(7) Uani 1 1 d . . . O25 O 0.7603(5) 0.09205(10) 0.3762(5) 0.0579(19) Uani 1 1 d . . . O26 O 0.6392(8) 0.06873(12) 0.3768(5) 0.088(3) Uani 1 1 d . . . O27 O 0.5971(7) 0.09896(13) 0.3714(6) 0.085(3) Uani 1 1 d . . . O28 O 0.6822(9) 0.0897(2) 0.4756(5) 0.126(5) Uani 1 1 d . . . Cl8 Cl 0.0201(5) 0.03797(6) 0.7657(2) 0.1162(19) Uani 1 1 d . . . O29 O 0.0909(10) 0.03633(16) 0.8248(6) 0.121(4) Uani 1 1 d . . . O30 O -0.0488(14) 0.0239(3) 0.7541(10) 0.208(10) Uani 1 1 d . . . O31 O 0.049(2) 0.0391(3) 0.7044(7) 0.279(14) Uani 1 1 d . . . O32 O -0.0142(18) 0.0555(2) 0.7758(14) 0.349(19) Uani 1 1 d . . . N25 N 0.2950(10) 0.14130(13) 0.1537(6) 0.092(4) Uani 1 1 d DU . . C153 C 0.3261(12) 0.15573(15) 0.1468(7) 0.091(4) Uani 1 1 d DU . . C154 C 0.3705(14) 0.17506(18) 0.1372(10) 0.138(6) Uani 1 1 d DU . . H15C H 0.4021 0.1800 0.1838 0.207 Uiso 1 1 calc R . . H15D H 0.3179 0.1838 0.1155 0.207 Uiso 1 1 calc R . . H15E H 0.4203 0.1739 0.1061 0.207 Uiso 1 1 calc RD . . N26 N 0.8717(9) 0.10458(14) 0.8341(6) 0.081(3) Uani 1 1 d U . . C155 C 0.8542(13) 0.09053(17) 0.8512(8) 0.091(4) Uani 1 1 d U . . C156 C 0.8383(14) 0.0714(2) 0.8749(9) 0.131(6) Uani 1 1 d U . . H15F H 0.8865 0.0686 0.9181 0.196 Uiso 1 1 calc R . . H15G H 0.8467 0.0623 0.8373 0.196 Uiso 1 1 calc R . . H15H H 0.7707 0.0704 0.8853 0.196 Uiso 1 1 calc R . . N27 N 0.7824(8) 0.10755(13) 0.6468(6) 0.063(2) Uani 1 1 d U . . C157 C 0.7840(8) 0.09188(15) 0.6405(6) 0.050(2) Uani 1 1 d U . . C158 C 0.7852(10) 0.07110(15) 0.6304(7) 0.071(3) Uani 1 1 d U . . H15I H 0.7175 0.0666 0.6126 0.107 Uiso 1 1 calc R . . H15J H 0.8108 0.0649 0.6760 0.107 Uiso 1 1 calc R . . H15K H 0.8280 0.0679 0.5957 0.107 Uiso 1 1 calc R . . N28 N 0.9846(12) 0.1465(3) 0.5397(9) 0.120(6) Uani 1 1 d U . . C159 C 0.9669(12) 0.1316(4) 0.5305(10) 0.107(7) Uani 1 1 d U . . C160 C 0.9490(12) 0.1101(3) 0.5133(9) 0.122(6) Uani 1 1 d U . . H16A H 0.9943 0.1058 0.4818 0.183 Uiso 1 1 calc R . . H16B H 0.8801 0.1082 0.4896 0.183 Uiso 1 1 calc R . . H16C H 0.9614 0.1027 0.5578 0.183 Uiso 1 1 calc R . . N29 N 0.1989(9) 0.10939(19) 0.4650(6) 0.084(3) Uani 1 1 d U . . C161 C 0.2153(10) 0.1252(2) 0.4785(7) 0.075(4) Uani 1 1 d U . . C162 C 0.2374(11) 0.1450(2) 0.4951(8) 0.091(4) Uani 1 1 d U . . H16D H 0.2835 0.1459 0.5406 0.136 Uiso 1 1 calc R . . H16E H 0.1758 0.1518 0.4988 0.136 Uiso 1 1 calc R . . H16F H 0.2680 0.1507 0.4572 0.136 Uiso 1 1 calc R . . N30 N 0.3964(8) 0.14561(12) 0.3478(6) 0.063(2) Uani 1 1 d U . . C163 C 0.3964(9) 0.16068(16) 0.3649(6) 0.056(3) Uani 1 1 d U . . C164 C 0.3933(11) 0.18115(15) 0.3897(7) 0.077(4) Uani 1 1 d U . . H16G H 0.3241 0.1855 0.3830 0.116 Uiso 1 1 calc R . . H16H H 0.4309 0.1892 0.3619 0.116 Uiso 1 1 calc R . . H16I H 0.4228 0.1820 0.4404 0.116 Uiso 1 1 calc R . . N31 N 0.1292(10) 0.0092(2) 0.4621(8) 0.099(4) Uani 1 1 d U . . C165 C 0.1073(11) -0.0075(3) 0.4610(8) 0.085(4) Uani 1 1 d U . . C166 C 0.0762(12) -0.0273(2) 0.4600(9) 0.099(4) Uani 1 1 d U . . H16J H 0.0132 -0.0283 0.4776 0.148 Uiso 1 1 calc R . . H16K H 0.1271 -0.0349 0.4906 0.148 Uiso 1 1 calc R . . H16L H 0.0675 -0.0322 0.4110 0.148 Uiso 1 1 calc R . . N32 N 0.408(2) 0.0172(3) 0.0481(17) 0.119(9) Uiso 0.50 1 d PDU . . C167 C 0.396(2) 0.0000(3) 0.0366(15) 0.077(7) Uiso 0.50 1 d PDU . . C168 C 0.386(2) -0.0222(3) 0.0207(18) 0.099(9) Uiso 0.50 1 d PDU . . H16M H 0.4283 -0.0257 -0.0143 0.149 Uiso 0.50 1 calc PR . . H16N H 0.3171 -0.0254 0.0016 0.149 Uiso 0.50 1 calc PR . . H16O H 0.4083 -0.0294 0.0650 0.149 Uiso 0.50 1 calc PR . . N33 N 1.0129(16) 0.2221(4) 0.5749(10) 0.087(7) Uani 0.50 1 d PDU . . C169 C 1.043(2) 0.2093(4) 0.5423(12) 0.091(7) Uani 0.50 1 d PDU . . C170 C 1.093(2) 0.1951(4) 0.4944(15) 0.112(8) Uani 0.50 1 d PDU . . H17B H 1.0584 0.1961 0.4448 0.168 Uiso 0.50 1 calc PR . . H17C H 1.0871 0.1821 0.5115 0.168 Uiso 0.50 1 calc PR . . H17D H 1.1628 0.1984 0.4973 0.168 Uiso 0.50 1 calc PR . . N34 N -0.146(2) 0.2072(4) 0.3527(12) 0.103(8) Uiso 0.50 1 d PDU . . C171 C -0.167(2) 0.2039(4) 0.2943(12) 0.082(7) Uiso 0.50 1 d PDU . . C172 C -0.190(2) 0.1985(4) 0.2162(12) 0.086(7) Uiso 0.50 1 d PDU . . H17E H -0.1650 0.2084 0.1877 0.129 Uiso 0.50 1 calc PR . . H17F H -0.2625 0.1974 0.2014 0.129 Uiso 0.50 1 calc PR . . H17G H -0.1587 0.1863 0.2091 0.129 Uiso 0.50 1 calc PR . . N35 N 0.459(3) 0.1098(5) 0.029(3) 0.189(14) Uiso 0.50 1 d PDU . . C173 C 0.474(4) 0.0930(6) 0.024(3) 0.173(16) Uiso 0.50 1 d PDU . . C174 C 0.461(4) 0.0709(6) 0.015(3) 0.193(16) Uiso 0.50 1 d PDU . . H17H H 0.3946 0.0673 0.0238 0.289 Uiso 0.50 1 calc PR . . H17I H 0.5116 0.0644 0.0493 0.289 Uiso 0.50 1 calc PR . . H17J H 0.4673 0.0672 -0.0336 0.289 Uiso 0.50 1 calc PR . . O33 O 0.2545(10) 0.05587(16) 0.6320(8) 0.046(3) Uani 0.50 1 d PU . . C175 C 0.3424(17) 0.0579(3) 0.7452(13) 0.058(5) Uani 0.50 1 d PU . . H17K H 0.4145 0.0575 0.7469 0.088 Uiso 0.50 1 calc PR . . H17L H 0.3263 0.0523 0.7889 0.088 Uiso 0.50 1 calc PR . . H17M H 0.3195 0.0712 0.7412 0.088 Uiso 0.50 1 calc PR . . C176 C 0.2939(14) 0.0473(2) 0.6844(11) 0.042(3) Uani 0.50 1 d PU . . H17N H 0.3438 0.0386 0.6697 0.051 Uiso 0.50 1 calc PR . . H17O H 0.2425 0.0392 0.7004 0.051 Uiso 0.50 1 calc PR . . C177 C 0.1882(15) 0.0462(3) 0.5762(11) 0.048(3) Uani 0.50 1 d PU . . H17P H 0.1308 0.0413 0.5958 0.057 Uiso 0.50 1 calc PR . . H17Q H 0.2233 0.0353 0.5594 0.057 Uiso 0.50 1 calc PR . . C178 C 0.1500(13) 0.0592(2) 0.5126(10) 0.042(4) Uani 0.50 1 d PU . . H17R H 0.0891 0.0656 0.5204 0.064 Uiso 0.50 1 calc PR . . H17S H 0.1358 0.0516 0.4689 0.064 Uiso 0.50 1 calc PR . . H17T H 0.2007 0.0688 0.5076 0.064 Uiso 0.50 1 calc PR . . O34 O -0.370(3) 0.1543(6) 0.0146(15) 0.171(11) Uani 0.50 1 d PU . . C179 C -0.312(4) 0.1196(7) -0.009(2) 0.167(12) Uani 0.50 1 d PU . . H17U H -0.3524 0.1168 0.0272 0.250 Uiso 0.50 1 calc PR . . H17V H -0.2498 0.1122 0.0009 0.250 Uiso 0.50 1 calc PR . . H17W H -0.3483 0.1160 -0.0563 0.250 Uiso 0.50 1 calc PR . . C180 C -0.289(4) 0.1389(8) -0.008(2) 0.171(11) Uani 0.50 1 d PU . . H18A H -0.2779 0.1424 -0.0567 0.205 Uiso 0.50 1 calc PR . . H18B H -0.2254 0.1408 0.0246 0.205 Uiso 0.50 1 calc PR . . C181 C -0.319(4) 0.1706(7) 0.031(2) 0.173(11) Uani 0.50 1 d PU . . H18C H -0.3039 0.1776 -0.0109 0.207 Uiso 0.50 1 calc PR . . H18D H -0.2603 0.1693 0.0688 0.207 Uiso 0.50 1 calc PR . . C182 C -0.420(2) 0.1777(7) 0.058(2) 0.188(13) Uani 0.50 1 d PU . . H18E H -0.4737 0.1794 0.0174 0.283 Uiso 0.50 1 calc PR . . H18F H -0.4072 0.1898 0.0840 0.283 Uiso 0.50 1 calc PR . . H18G H -0.4403 0.1681 0.0906 0.283 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0262(6) 0.0261(6) 0.0245(6) 0.0005(5) 0.0052(5) 0.0020(5) Fe2 0.0239(6) 0.0259(6) 0.0282(6) 0.0018(5) 0.0082(5) 0.0025(5) N1 0.027(3) 0.027(3) 0.026(3) 0.006(3) 0.008(3) 0.008(3) N2 0.025(3) 0.028(3) 0.020(3) 0.001(2) 0.006(3) 0.000(3) N3 0.030(4) 0.023(3) 0.027(3) 0.001(2) 0.001(3) 0.004(3) N4 0.024(3) 0.028(3) 0.026(3) -0.001(3) 0.010(3) 0.005(3) N5 0.026(4) 0.032(3) 0.026(3) -0.002(3) 0.010(3) 0.005(3) N6 0.031(4) 0.029(3) 0.031(3) 0.002(3) 0.008(3) 0.002(3) N7 0.030(4) 0.026(3) 0.032(3) -0.001(3) 0.008(3) 0.000(3) N8 0.020(3) 0.027(3) 0.027(3) 0.004(3) 0.008(3) 0.005(2) N9 0.020(3) 0.026(3) 0.034(3) -0.003(3) 0.010(3) -0.001(2) N10 0.030(4) 0.020(3) 0.035(3) 0.007(3) 0.006(3) 0.004(3) N11 0.019(3) 0.028(3) 0.028(3) 0.008(3) 0.007(3) 0.002(2) N12 0.018(3) 0.028(3) 0.028(3) 0.000(3) 0.007(2) 0.003(2) C1 0.035(5) 0.025(4) 0.034(4) 0.003(3) 0.003(4) 0.000(3) C2 0.028(4) 0.035(4) 0.038(5) 0.006(4) 0.007(4) -0.005(3) C3 0.040(5) 0.032(4) 0.048(5) 0.004(4) 0.003(4) -0.005(4) C4 0.038(5) 0.048(5) 0.061(6) 0.002(5) 0.024(5) -0.020(4) C5 0.041(6) 0.046(5) 0.082(8) -0.001(5) 0.036(6) -0.004(4) C6 0.047(6) 0.042(5) 0.061(6) 0.002(4) 0.028(5) 0.001(4) C7 0.033(5) 0.036(4) 0.035(4) -0.002(3) 0.013(4) -0.003(4) C8 0.026(4) 0.034(4) 0.021(3) 0.002(3) 0.005(3) -0.003(3) C9 0.023(4) 0.036(4) 0.029(4) 0.000(3) 0.009(3) 0.001(3) C10 0.032(4) 0.031(4) 0.023(4) 0.001(3) 0.002(3) 0.002(3) C11 0.024(4) 0.039(4) 0.025(4) 0.001(3) 0.004(3) 0.006(3) C12 0.031(5) 0.037(5) 0.041(5) -0.005(4) 0.017(4) 0.002(4) C13 0.034(5) 0.048(5) 0.054(6) 0.000(4) 0.015(4) 0.017(4) C14 0.048(6) 0.030(4) 0.047(5) -0.002(4) 0.005(4) 0.010(4) C15 0.041(5) 0.031(4) 0.034(4) 0.001(3) 0.003(4) -0.003(4) C16 0.033(4) 0.028(4) 0.026(4) 0.000(3) 0.005(3) 0.005(3) C17 0.033(5) 0.039(5) 0.025(4) 0.005(3) 0.006(3) -0.004(4) C18 0.027(4) 0.027(4) 0.020(3) -0.001(3) -0.005(3) 0.002(3) C19 0.027(4) 0.027(4) 0.021(3) 0.003(3) 0.002(3) 0.003(3) C20 0.036(5) 0.028(4) 0.034(4) 0.003(3) 0.010(4) 0.001(3) C21 0.033(5) 0.037(5) 0.038(5) 0.000(4) 0.009(4) 0.013(4) C22 0.053(6) 0.032(5) 0.059(6) 0.003(4) 0.017(5) 0.006(4) C23 0.064(7) 0.044(6) 0.070(7) 0.004(5) 0.035(6) 0.020(5) C24 0.052(7) 0.057(6) 0.067(7) 0.007(5) 0.028(6) 0.030(5) C25 0.047(6) 0.045(5) 0.046(5) 0.002(4) 0.023(5) 0.007(4) C26 0.041(5) 0.035(4) 0.034(4) 0.003(4) 0.011(4) 0.012(4) C27 0.035(5) 0.035(4) 0.026(4) 0.006(3) 0.007(3) 0.006(3) C28 0.026(4) 0.043(5) 0.031(4) -0.001(3) 0.013(3) 0.000(4) C29 0.028(4) 0.039(4) 0.025(4) 0.001(3) 0.010(3) 0.001(3) C30 0.033(5) 0.039(4) 0.023(4) 0.001(3) 0.008(3) -0.002(4) C31 0.037(5) 0.047(5) 0.037(5) -0.005(4) 0.016(4) -0.011(4) C32 0.043(6) 0.060(6) 0.039(5) -0.006(4) 0.015(4) -0.023(5) C33 0.064(7) 0.044(5) 0.037(5) -0.006(4) 0.020(5) -0.025(5) C34 0.040(5) 0.041(5) 0.040(5) -0.006(4) 0.007(4) -0.004(4) C35 0.033(5) 0.038(4) 0.029(4) -0.002(3) 0.006(3) -0.005(4) C36 0.039(5) 0.031(4) 0.034(4) -0.005(3) 0.004(4) 0.002(4) C37 0.031(4) 0.035(4) 0.016(3) 0.000(3) 0.005(3) -0.002(3) C38 0.032(5) 0.029(4) 0.025(4) -0.001(3) 0.003(3) 0.006(3) C39 0.039(5) 0.032(4) 0.036(4) 0.001(3) 0.010(4) -0.001(4) C40 0.045(6) 0.033(4) 0.045(5) -0.004(4) 0.011(4) -0.002(4) C41 0.071(8) 0.031(5) 0.053(6) -0.010(4) 0.010(5) -0.011(5) C42 0.067(7) 0.039(5) 0.051(6) -0.014(4) 0.008(5) -0.011(5) C43 0.058(6) 0.048(5) 0.039(5) -0.017(4) 0.020(5) -0.018(5) C44 0.049(6) 0.050(5) 0.033(5) -0.004(4) 0.012(4) -0.011(4) C45 0.033(5) 0.036(4) 0.030(4) -0.005(3) 0.008(4) -0.008(3) C46 0.028(4) 0.036(4) 0.034(4) -0.002(3) 0.007(3) -0.004(3) C47 0.030(4) 0.046(5) 0.023(4) 0.001(3) 0.005(3) -0.001(4) C48 0.024(4) 0.034(4) 0.035(4) 0.003(3) 0.012(3) 0.000(3) C49 0.025(4) 0.046(5) 0.034(4) 0.008(4) 0.008(3) 0.003(4) C50 0.053(6) 0.055(6) 0.038(5) 0.016(4) 0.005(4) -0.005(5) C51 0.063(7) 0.060(6) 0.038(5) 0.020(5) 0.001(5) 0.004(5) C52 0.052(6) 0.049(6) 0.049(6) 0.026(5) 0.013(5) 0.009(5) C53 0.047(6) 0.032(4) 0.053(6) 0.012(4) 0.007(5) 0.005(4) C54 0.024(4) 0.041(5) 0.038(5) 0.010(4) 0.008(3) 0.002(3) C55 0.031(4) 0.027(4) 0.037(4) 0.003(3) 0.009(4) 0.002(3) C56 0.014(4) 0.033(4) 0.035(4) 0.003(3) 0.013(3) 0.001(3) C57 0.024(4) 0.032(4) 0.032(4) -0.002(3) 0.011(3) 0.000(3) C58 0.021(4) 0.027(4) 0.048(5) -0.003(3) 0.013(4) 0.001(3) C59 0.019(4) 0.029(4) 0.048(5) 0.012(4) 0.013(4) 0.000(3) C60 0.026(4) 0.030(4) 0.053(5) 0.007(4) 0.018(4) 0.004(3) C61 0.029(5) 0.034(4) 0.059(6) 0.019(4) 0.025(4) 0.008(3) C62 0.027(4) 0.049(5) 0.045(5) 0.027(4) 0.009(4) 0.002(4) C63 0.018(4) 0.043(5) 0.036(4) 0.010(4) 0.007(3) -0.001(3) C64 0.014(4) 0.038(4) 0.043(5) 0.006(4) 0.015(3) 0.000(3) C65 0.017(4) 0.035(4) 0.035(4) 0.007(3) 0.008(3) 0.005(3) C66 0.023(4) 0.034(4) 0.031(4) 0.002(3) 0.005(3) 0.004(3) C67 0.011(3) 0.035(4) 0.031(4) -0.003(3) 0.009(3) -0.002(3) C68 0.031(5) 0.033(4) 0.032(4) -0.003(3) 0.010(3) 0.001(3) C69 0.041(5) 0.044(5) 0.033(4) -0.008(4) 0.010(4) -0.002(4) C70 0.058(6) 0.049(5) 0.030(4) -0.012(4) -0.007(4) 0.006(5) C71 0.039(5) 0.042(5) 0.049(5) -0.015(4) 0.001(4) -0.005(4) C72 0.037(5) 0.031(4) 0.043(5) -0.005(4) 0.008(4) -0.001(4) C73 0.021(4) 0.031(4) 0.032(4) -0.002(3) 0.010(3) 0.007(3) C74 0.021(4) 0.027(4) 0.036(4) 0.005(3) 0.013(3) 0.001(3) C75 0.017(4) 0.026(4) 0.029(4) 0.006(3) 0.007(3) 0.004(3) C76 0.013(3) 0.027(4) 0.037(4) 0.000(3) 0.010(3) 0.007(3) Fe3 0.0321(7) 0.0295(6) 0.0292(6) 0.0002(5) 0.0073(5) 0.0046(5) Fe4 0.0301(7) 0.0308(6) 0.0302(6) 0.0011(5) 0.0077(5) 0.0030(5) N13 0.031(4) 0.025(3) 0.033(3) -0.001(3) 0.006(3) 0.001(3) N14 0.029(4) 0.026(3) 0.034(4) -0.001(3) 0.009(3) 0.003(3) N15 0.039(4) 0.028(3) 0.031(4) 0.004(3) 0.002(3) 0.001(3) N16 0.032(4) 0.025(3) 0.033(3) 0.001(3) 0.012(3) 0.001(3) N17 0.031(4) 0.034(4) 0.029(3) 0.002(3) 0.011(3) 0.008(3) N18 0.033(4) 0.029(3) 0.031(3) 0.000(3) 0.011(3) -0.005(3) N19 0.041(4) 0.032(4) 0.031(4) 0.001(3) 0.007(3) 0.010(3) N20 0.021(3) 0.039(4) 0.032(3) 0.003(3) 0.007(3) 0.001(3) N21 0.026(4) 0.042(4) 0.035(4) 0.006(3) 0.008(3) 0.003(3) N22 0.043(4) 0.031(4) 0.031(4) -0.003(3) 0.010(3) -0.001(3) N23 0.034(4) 0.035(4) 0.030(3) -0.002(3) 0.006(3) 0.009(3) N24 0.029(4) 0.031(4) 0.036(4) 0.000(3) 0.012(3) 0.003(3) C77 0.029(4) 0.028(4) 0.039(5) 0.007(3) 0.007(4) 0.007(3) C78 0.025(4) 0.033(4) 0.032(4) 0.001(3) 0.006(3) 0.003(3) C79 0.035(5) 0.031(4) 0.049(5) -0.007(4) 0.010(4) 0.004(4) C80 0.045(6) 0.036(5) 0.047(5) -0.011(4) 0.001(4) -0.001(4) C81 0.050(6) 0.043(5) 0.035(5) -0.011(4) -0.004(4) 0.005(4) C82 0.054(6) 0.036(5) 0.039(5) 0.002(4) 0.002(4) 0.003(4) C83 0.027(4) 0.033(4) 0.035(4) -0.004(3) 0.005(3) 0.004(3) C84 0.029(4) 0.029(4) 0.029(4) -0.002(3) 0.005(3) 0.002(3) C85 0.031(5) 0.036(4) 0.032(4) 0.004(3) 0.001(3) 0.008(3) C86 0.033(5) 0.028(4) 0.034(4) 0.008(3) 0.006(4) 0.003(3) C87 0.033(5) 0.035(4) 0.043(5) 0.009(4) 0.011(4) 0.001(4) C88 0.038(5) 0.034(4) 0.041(5) 0.003(4) 0.008(4) 0.001(4) C89 0.042(5) 0.035(5) 0.043(5) 0.011(4) 0.003(4) 0.002(4) C90 0.050(6) 0.025(4) 0.066(6) 0.014(4) 0.010(5) 0.001(4) C91 0.054(6) 0.025(4) 0.054(6) -0.001(4) 0.007(5) 0.000(4) C92 0.040(5) 0.032(4) 0.052(5) 0.001(4) 0.007(4) 0.000(4) C93 0.044(5) 0.028(4) 0.047(5) -0.003(4) 0.001(4) -0.001(4) C94 0.026(4) 0.024(4) 0.043(5) 0.002(3) 0.004(4) 0.005(3) C95 0.029(4) 0.022(4) 0.035(4) 0.000(3) 0.005(3) 0.003(3) C96 0.043(5) 0.034(5) 0.034(4) -0.001(4) 0.006(4) 0.004(4) C97 0.036(5) 0.038(5) 0.034(4) 0.005(4) 0.009(4) 0.000(4) C98 0.045(6) 0.031(4) 0.046(5) 0.004(4) 0.004(4) 0.002(4) C99 0.045(6) 0.037(5) 0.050(6) 0.012(4) 0.010(4) 0.006(4) C100 0.067(7) 0.053(6) 0.036(5) 0.007(4) -0.007(5) 0.004(5) C101 0.055(6) 0.038(5) 0.032(5) 0.000(4) -0.005(4) -0.002(4) C102 0.026(4) 0.038(4) 0.029(4) 0.007(3) 0.004(3) 0.001(3) C103 0.027(4) 0.031(4) 0.033(4) 0.002(3) 0.007(3) -0.005(3) C104 0.034(5) 0.043(5) 0.026(4) 0.000(3) 0.000(3) 0.002(4) C105 0.027(4) 0.033(4) 0.039(5) -0.009(4) 0.008(4) -0.002(3) C106 0.031(5) 0.031(4) 0.042(5) -0.005(4) 0.008(4) -0.002(3) C107 0.034(5) 0.041(5) 0.037(5) -0.010(4) 0.006(4) 0.001(4) C108 0.048(6) 0.057(6) 0.046(5) -0.020(5) 0.002(5) 0.004(5) C109 0.073(8) 0.034(5) 0.055(6) -0.020(4) 0.002(5) 0.004(5) C110 0.064(7) 0.032(5) 0.060(6) -0.008(4) 0.006(5) 0.003(4) C111 0.036(5) 0.035(5) 0.045(5) -0.011(4) 0.007(4) 0.008(4) C112 0.040(5) 0.028(4) 0.046(5) 0.001(4) 0.015(4) -0.003(4) C113 0.023(4) 0.026(4) 0.039(4) -0.005(3) 0.005(3) 0.000(3) C114 0.022(4) 0.032(4) 0.036(4) -0.004(3) 0.006(3) 0.000(3) C115 0.041(5) 0.044(5) 0.028(4) -0.003(4) 0.004(4) 0.007(4) C116 0.051(6) 0.044(5) 0.022(4) -0.003(4) 0.001(4) 0.013(4) C117 0.064(7) 0.045(5) 0.033(5) -0.001(4) 0.003(5) 0.020(5) C118 0.067(7) 0.052(6) 0.043(5) -0.017(5) 0.001(5) 0.030(5) C119 0.060(8) 0.072(8) 0.058(7) -0.012(6) 0.009(6) 0.030(6) C120 0.040(5) 0.066(7) 0.040(5) 0.002(5) 0.009(4) 0.022(5) C121 0.047(6) 0.048(5) 0.027(4) -0.001(4) 0.003(4) 0.011(4) C122 0.039(5) 0.047(5) 0.024(4) 0.003(4) 0.006(4) 0.010(4) C123 0.030(5) 0.060(6) 0.046(5) -0.006(4) 0.017(4) 0.011(4) C124 0.028(5) 0.049(5) 0.034(4) 0.002(4) 0.010(4) 0.006(4) C125 0.047(6) 0.055(6) 0.071(7) 0.007(5) 0.028(6) 0.006(5) C126 0.050(7) 0.061(7) 0.129(13) 0.000(8) 0.044(8) -0.002(6) C127 0.076(7) 0.063(6) 0.263(15) -0.002(8) 0.107(9) -0.010(6) C128 0.083(8) 0.057(6) 0.266(15) 0.001(8) 0.104(9) -0.013(6) C129 0.079(7) 0.046(6) 0.259(15) -0.001(7) 0.104(9) -0.012(5) C130 0.046(6) 0.051(6) 0.082(8) 0.012(6) 0.031(6) 0.001(5) C131 0.041(5) 0.040(5) 0.050(6) 0.012(4) 0.015(4) 0.005(4) C132 0.041(5) 0.038(5) 0.025(4) 0.003(3) 0.006(4) 0.003(4) C133 0.036(5) 0.036(4) 0.020(4) 0.006(3) 0.004(3) 0.009(4) C134 0.038(5) 0.032(4) 0.031(4) -0.005(3) 0.001(4) 0.004(4) C135 0.047(5) 0.033(4) 0.028(4) -0.004(3) 0.006(4) -0.007(4) C136 0.059(6) 0.046(5) 0.022(4) 0.001(4) 0.002(4) -0.002(5) C137 0.075(8) 0.035(5) 0.041(5) 0.001(4) 0.007(5) -0.013(5) C138 0.057(7) 0.057(6) 0.053(6) -0.015(5) 0.017(5) -0.025(5) C139 0.056(7) 0.044(5) 0.054(6) -0.010(5) 0.016(5) -0.012(5) C140 0.039(5) 0.040(5) 0.038(5) -0.003(4) 0.011(4) -0.007(4) C141 0.039(5) 0.040(5) 0.042(5) -0.006(4) 0.003(4) 0.001(4) C142 0.034(5) 0.052(6) 0.072(7) -0.010(5) 0.022(5) 0.000(4) C143 0.040(5) 0.034(5) 0.067(7) -0.004(4) 0.019(5) 0.000(4) C144 0.079(5) 0.036(4) 0.196(8) -0.032(5) 0.095(6) -0.001(4) C145 0.087(5) 0.046(4) 0.206(8) -0.027(5) 0.095(6) -0.008(4) C146 0.091(5) 0.052(4) 0.209(8) -0.031(5) 0.097(6) -0.008(4) C147 0.087(6) 0.050(4) 0.209(9) -0.025(5) 0.098(6) -0.011(4) C148 0.082(5) 0.042(4) 0.200(8) -0.027(5) 0.097(6) -0.009(4) C149 0.074(5) 0.036(4) 0.193(8) -0.029(5) 0.095(6) -0.008(4) C150 0.032(5) 0.031(4) 0.046(5) -0.002(4) 0.006(4) 0.002(3) C151 0.035(5) 0.032(4) 0.039(5) -0.008(4) 0.010(4) 0.005(4) C152 0.034(5) 0.035(4) 0.029(4) 0.002(3) 0.011(3) 0.005(4) Cl1 0.0345(11) 0.0322(9) 0.0339(10) -0.0046(8) 0.0071(8) -0.0045(8) O1 0.051(4) 0.048(4) 0.047(4) -0.005(3) -0.004(3) 0.006(3) O2 0.086(6) 0.039(4) 0.038(4) -0.007(3) -0.004(4) -0.004(4) O3 0.085(6) 0.048(4) 0.037(4) 0.002(3) 0.013(4) 0.008(4) O4 0.039(4) 0.067(5) 0.113(7) -0.014(5) 0.037(5) -0.011(4) Cl2 0.0670(18) 0.0438(13) 0.0652(16) 0.0108(12) 0.0018(13) 0.0057(12) O5 0.068(7) 0.087(7) 0.148(11) 0.033(7) 0.019(7) 0.007(5) O6 0.109(8) 0.064(5) 0.079(6) -0.006(5) -0.022(6) 0.026(5) O7 0.135(11) 0.076(6) 0.106(9) -0.024(6) -0.045(7) 0.015(6) O8 0.143(11) 0.077(7) 0.102(8) 0.043(6) -0.005(7) -0.019(7) Cl3 0.0466(13) 0.0399(11) 0.0389(11) -0.0096(9) 0.0107(9) -0.0106(9) O9 0.051(5) 0.105(7) 0.050(4) -0.012(4) 0.000(4) 0.018(4) O10 0.132(9) 0.064(5) 0.047(4) 0.005(4) 0.021(5) 0.010(5) O11 0.132(9) 0.049(4) 0.058(5) -0.013(4) 0.005(5) -0.028(5) O12 0.058(6) 0.067(5) 0.166(11) -0.026(6) 0.056(7) -0.012(4) Cl4 0.0623(17) 0.0417(12) 0.092(2) -0.0025(13) 0.0424(16) -0.0008(12) O13 0.105(9) 0.103(8) 0.139(10) 0.070(7) -0.056(7) -0.055(7) O14 0.146(12) 0.123(9) 0.128(10) -0.043(8) 0.074(9) -0.078(9) O15 0.140(12) 0.167(13) 0.182(14) -0.012(11) 0.123(12) 0.019(10) O16 0.137(13) 0.178(14) 0.148(13) -0.052(11) -0.065(10) 0.064(10) Cl5 0.111(3) 0.0614(17) 0.0478(15) 0.0146(13) -0.0211(16) -0.0416(17) O17 0.129(10) 0.057(5) 0.087(7) -0.016(5) -0.002(6) 0.026(5) O18 0.080(7) 0.083(6) 0.070(6) -0.021(5) -0.025(5) 0.013(5) O19 0.139(11) 0.102(8) 0.084(7) 0.037(6) -0.010(7) -0.013(7) O20 0.073(7) 0.085(7) 0.225(16) 0.006(9) 0.030(9) 0.016(6) Cl6 0.076(2) 0.0486(14) 0.0563(15) 0.0064(11) 0.0062(14) -0.0091(13) O21 0.094(8) 0.056(5) 0.112(8) -0.008(5) 0.030(6) -0.020(5) O22 0.224(17) 0.120(10) 0.104(9) 0.039(8) -0.075(10) -0.085(11) O23 0.213(14) 0.078(7) 0.064(6) -0.006(5) 0.047(8) -0.056(8) O24 0.136(14) 0.083(9) 0.41(3) -0.005(13) 0.090(17) 0.029(9) Cl7 0.0507(15) 0.0620(15) 0.0769(18) -0.0292(13) 0.0405(14) -0.0188(12) O25 0.044(4) 0.049(4) 0.085(6) -0.003(4) 0.024(4) 0.000(3) O26 0.121(9) 0.054(5) 0.087(7) 0.014(5) 0.014(6) -0.039(5) O27 0.056(6) 0.080(6) 0.120(9) 0.006(6) 0.020(6) 0.011(5) O28 0.091(8) 0.234(15) 0.051(6) -0.006(8) 0.011(5) -0.044(9) Cl8 0.198(6) 0.075(2) 0.060(2) -0.0138(18) -0.023(3) 0.041(3) O29 0.167(13) 0.100(8) 0.083(8) 0.013(7) -0.010(8) 0.010(8) O30 0.206(19) 0.206(17) 0.25(2) -0.135(16) 0.145(17) -0.051(15) O31 0.50(4) 0.28(2) 0.057(9) -0.011(12) 0.047(15) -0.20(3) O32 0.36(3) 0.165(16) 0.41(3) -0.166(19) -0.25(3) 0.175(18) N25 0.137(10) 0.045(5) 0.081(7) 0.000(5) -0.022(7) 0.002(6) C153 0.144(11) 0.036(6) 0.072(7) 0.000(5) -0.040(8) -0.001(7) C154 0.199(14) 0.056(7) 0.133(11) 0.024(8) -0.040(11) -0.015(9) N26 0.107(9) 0.050(5) 0.075(7) 0.010(5) -0.013(6) 0.004(5) C155 0.130(11) 0.045(6) 0.075(8) 0.014(6) -0.043(7) -0.017(7) C156 0.177(13) 0.069(8) 0.120(11) 0.035(8) -0.050(10) -0.046(9) N27 0.063(6) 0.051(5) 0.074(6) -0.008(5) 0.011(5) 0.001(4) C157 0.047(6) 0.056(6) 0.047(5) 0.003(5) 0.009(4) 0.002(5) C158 0.088(8) 0.048(6) 0.074(7) 0.009(5) 0.003(6) -0.001(6) N28 0.062(8) 0.217(18) 0.079(8) 0.015(12) 0.005(7) -0.022(10) C159 0.041(7) 0.21(2) 0.063(8) 0.023(13) 0.003(6) -0.022(11) C160 0.074(9) 0.215(18) 0.074(9) 0.025(11) 0.002(7) -0.047(11) N29 0.066(7) 0.115(9) 0.064(6) -0.004(7) -0.011(5) 0.000(7) C161 0.050(7) 0.125(10) 0.047(6) 0.002(7) 0.002(5) -0.013(7) C162 0.069(8) 0.131(11) 0.071(8) 0.005(8) 0.009(7) -0.012(8) N30 0.065(6) 0.044(5) 0.077(6) -0.012(4) 0.000(5) -0.001(4) C163 0.064(7) 0.055(6) 0.047(5) 0.002(5) 0.002(5) -0.012(5) C164 0.100(9) 0.044(6) 0.080(8) -0.001(6) -0.002(7) -0.007(6) N31 0.072(8) 0.117(9) 0.106(9) -0.001(8) 0.008(7) 0.012(7) C165 0.067(8) 0.112(10) 0.077(8) -0.008(8) 0.012(7) 0.003(8) C166 0.079(9) 0.110(10) 0.106(10) -0.010(9) 0.013(8) -0.014(8) N33 0.053(11) 0.18(2) 0.029(9) 0.011(11) 0.014(8) 0.010(12) C169 0.073(14) 0.16(2) 0.040(11) 0.048(12) 0.010(10) 0.017(13) C170 0.097(15) 0.17(2) 0.067(13) 0.027(14) 0.012(12) 0.026(15) O33 0.046(6) 0.030(5) 0.062(6) -0.011(5) 0.014(5) -0.002(4) C175 0.061(11) 0.031(8) 0.080(11) 0.007(8) 0.002(9) 0.003(8) C176 0.037(7) 0.026(6) 0.063(7) -0.009(6) 0.005(6) 0.008(5) C177 0.044(7) 0.036(6) 0.064(7) -0.011(6) 0.014(6) -0.002(6) C178 0.030(8) 0.037(8) 0.054(9) -0.008(7) -0.010(7) 0.009(7) O34 0.18(3) 0.24(3) 0.080(12) 0.032(18) -0.002(13) 0.02(2) C179 0.18(3) 0.24(3) 0.063(14) 0.02(2) -0.024(16) 0.02(3) C180 0.18(3) 0.24(3) 0.079(13) 0.035(18) 0.001(14) 0.02(2) C181 0.18(3) 0.24(3) 0.086(13) 0.038(18) 0.004(14) 0.02(2) C182 0.19(3) 0.25(3) 0.114(18) 0.04(2) -0.004(18) 0.01(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 Fe1 N7 2.173(7) . ? Fe1 N4 2.179(6) . ? Fe1 N1 2.179(6) . ? Fe1 N8 2.203(6) . ? Fe1 N11 2.206(7) . ? Fe1 N10 2.223(6) . ? Fe2 N9 2.171(7) . ? Fe2 N12 2.179(6) . ? Fe2 N6 2.200(7) . ? Fe2 N3 2.203(6) . ? Fe2 N2 2.268(6) . ? Fe2 N5 2.303(6) . ? N1 C1 1.310(10) . ? N1 C19 1.369(10) . ? N2 C18 1.329(10) . ? N2 C19 1.344(10) . ? N3 C17 1.279(10) . ? N3 C18 1.379(10) . ? N4 C20 1.292(10) . ? N4 C38 1.389(10) . ? N5 C37 1.339(10) . ? N5 C38 1.350(10) . ? N6 C36 1.292(11) . ? N6 C37 1.376(10) . ? N7 C39 1.299(10) . ? N7 C57 1.382(10) . ? N8 C56 1.326(10) . ? N8 C57 1.336(10) . ? N9 C55 1.301(10) . ? N9 C56 1.388(10) . ? N10 C58 1.331(10) . ? N10 C76 1.376(10) . ? N11 C75 1.326(10) . ? N11 C76 1.356(10) . ? N12 C74 1.316(10) . ? N12 C75 1.393(9) . ? C1 C2 1.436(12) . ? C2 C3 1.398(11) . ? C2 C7 1.413(12) . ? C3 C4 1.346(13) . ? C4 C5 1.411(14) . ? C5 C6 1.362(13) . ? C6 C7 1.366(13) . ? C7 C8 1.444(11) . ? C8 C9 1.381(11) . ? C8 C19 1.418(11) . ? C9 C10 1.398(11) . ? C10 C18 1.412(11) . ? C10 C11 1.452(11) . ? C11 C16 1.423(12) . ? C11 C12 1.427(11) . ? C12 C13 1.377(12) . ? C13 C14 1.414(13) . ? C14 C15 1.374(13) . ? C15 C16 1.413(11) . ? C16 C17 1.416(12) . ? C20 C21 1.409(12) . ? C21 C26 1.419(13) . ? C21 C22 1.420(12) . ? C22 C23 1.345(14) . ? C23 C24 1.451(15) . ? C24 C25 1.397(13) . ? C25 C26 1.394(13) . ? C26 C27 1.458(11) . ? C27 C28 1.376(12) . ? C27 C38 1.403(12) . ? C28 C29 1.410(11) . ? C29 C37 1.401(11) . ? C29 C30 1.453(11) . ? C30 C31 1.377(12) . ? C30 C35 1.442(12) . ? C31 C32 1.376(12) . ? C32 C33 1.400(14) . ? C33 C34 1.337(13) . ? C34 C35 1.406(12) . ? C35 C36 1.417(12) . ? C39 C40 1.444(12) . ? C40 C41 1.399(12) . ? C40 C45 1.413(12) . ? C41 C42 1.368(14) . ? C42 C43 1.387(14) . ? C43 C44 1.352(13) . ? C44 C45 1.390(12) . ? C45 C46 1.491(11) . ? C46 C47 1.382(12) . ? C46 C57 1.401(11) . ? C47 C48 1.377(11) . ? C48 C56 1.411(11) . ? C48 C49 1.455(11) . ? C49 C50 1.380(13) . ? C49 C54 1.417(12) . ? C50 C51 1.391(13) . ? C51 C52 1.399(15) . ? C52 C53 1.350(14) . ? C53 C54 1.406(12) . ? C54 C55 1.437(12) . ? C58 C59 1.422(12) . ? C59 C64 1.394(12) . ? C59 C60 1.417(11) . ? C60 C61 1.365(13) . ? C61 C62 1.396(14) . ? C62 C63 1.389(12) . ? C63 C64 1.411(12) . ? C64 C65 1.464(11) . ? C65 C66 1.399(11) . ? C65 C76 1.400(11) . ? C66 C67 1.382(11) . ? C67 C75 1.415(11) . ? C67 C68 1.439(11) . ? C68 C69 1.401(12) . ? C68 C73 1.433(11) . ? C69 C70 1.403(12) . ? C70 C71 1.387(13) . ? C71 C72 1.350(13) . ? C72 C73 1.422(11) . ? C73 C74 1.418(11) . ? Fe3 N13 2.140(7) . ? Fe3 N16 2.174(7) . ? Fe3 N22 2.197(7) . ? Fe3 N19 2.201(7) . ? Fe3 N23 2.273(7) . ? Fe3 N20 2.295(7) . ? Fe4 N21 2.165(7) . ? Fe4 N15 2.178(7) . ? Fe4 N24 2.181(7) . ? Fe4 N18 2.216(7) . ? Fe4 N17 2.228(7) . ? Fe4 N14 2.265(7) . ? N13 C77 1.303(10) . ? N13 C95 1.396(10) . ? N14 C95 1.326(10) . ? N14 C94 1.335(10) . ? N15 C93 1.301(11) . ? N15 C94 1.412(11) . ? N16 C96 1.307(10) . ? N16 C114 1.375(10) . ? N17 C114 1.342(10) . ? N17 C113 1.353(10) . ? N18 C112 1.306(11) . ? N18 C113 1.389(10) . ? N19 C115 1.277(11) . ? N19 C133 1.356(11) . ? N20 C132 1.342(11) . ? N20 C133 1.352(10) . ? N21 C131 1.279(12) . ? N21 C132 1.369(11) . ? N22 C134 1.307(11) . ? N22 C152 1.375(10) . ? N23 C152 1.332(11) . ? N23 C151 1.343(10) . ? N24 C150 1.313(10) . ? N24 C151 1.364(11) . ? C77 C78 1.434(11) . ? C78 C83 1.393(11) . ? C78 C79 1.396(12) . ? C79 C80 1.372(13) . ? C80 C81 1.374(13) . ? C81 C82 1.355(12) . ? C82 C83 1.423(12) . ? C83 C84 1.461(11) . ? C84 C85 1.404(11) . ? C84 C95 1.425(11) . ? C85 C86 1.374(12) . ? C86 C94 1.377(12) . ? C86 C87 1.482(11) . ? C87 C88 1.388(12) . ? C87 C92 1.400(13) . ? C88 C89 1.377(12) . ? C89 C90 1.376(14) . ? C90 C91 1.368(14) . ? C91 C92 1.379(12) . ? C92 C93 1.431(13) . ? C96 C97 1.442(12) . ? C97 C98 1.405(12) . ? C97 C102 1.405(12) . ? C98 C99 1.338(13) . ? C99 C100 1.406(14) . ? C100 C101 1.390(13) . ? C101 C102 1.392(12) . ? C102 C103 1.451(11) . ? C103 C104 1.402(11) . ? C103 C114 1.421(11) . ? C104 C105 1.375(12) . ? C105 C113 1.385(12) . ? C105 C106 1.452(11) . ? C106 C107 1.382(12) . ? C106 C111 1.404(13) . ? C107 C108 1.402(13) . ? C108 C109 1.403(15) . ? C109 C110 1.357(15) . ? C110 C111 1.410(12) . ? C111 C112 1.446(13) . ? C115 C116 1.447(13) . ? C116 C121 1.402(14) . ? C116 C117 1.418(12) . ? C117 C118 1.338(15) . ? C118 C119 1.407(17) . ? C119 C120 1.374(15) . ? C120 C121 1.390(13) . ? C121 C122 1.442(12) . ? C122 C123 1.406(13) . ? C122 C133 1.430(12) . ? C123 C124 1.408(13) . ? C124 C132 1.429(12) . ? C124 C125 1.440(14) . ? C125 C126 1.390(15) . ? C125 C130 1.427(14) . ? C126 C127 1.362(17) . ? C127 C128 1.404(19) . ? C128 C129 1.367(18) . ? C129 C130 1.381(15) . ? C130 C131 1.412(14) . ? C134 C135 1.439(13) . ? C135 C136 1.389(12) . ? C135 C140 1.402(13) . ? C136 C137 1.371(15) . ? C137 C138 1.410(15) . ? C138 C139 1.385(13) . ? C139 C140 1.361(13) . ? C140 C141 1.444(12) . ? C141 C142 1.400(13) . ? C141 C152 1.432(12) . ? C142 C143 1.403(13) . ? C143 C151 1.427(13) . ? C143 C144 1.471(13) . ? C144 C145 1.324(16) . ? C144 C149 1.402(15) . ? C145 C146 1.415(16) . ? C146 C147 1.464(17) . ? C147 C148 1.360(16) . ? C148 C149 1.392(14) . ? C149 C150 1.443(13) . ? Cl1 O4 1.414(7) . ? Cl1 O2 1.435(7) . ? Cl1 O1 1.439(7) . ? Cl1 O3 1.445(7) . ? Cl2 O7 1.380(10) . ? Cl2 O8 1.428(10) . ? Cl2 O6 1.429(9) . ? Cl2 O5 1.457(10) . ? Cl3 O12 1.391(9) . ? Cl3 O11 1.415(8) . ? Cl3 O10 1.423(8) . ? Cl3 O9 1.439(8) . ? Cl4 O14 1.369(10) . ? Cl4 O13 1.384(11) . ? Cl4 O15 1.395(12) . ? Cl4 O16 1.528(13) . ? Cl5 O19 1.351(10) . ? Cl5 O17 1.351(9) . ? Cl5 O18 1.373(8) . ? Cl5 O20 1.582(11) . ? Cl6 O22 1.370(12) . ? Cl6 O23 1.380(10) . ? Cl6 O21 1.417(8) . ? Cl6 O24 1.429(13) . ? Cl7 O28 1.359(10) . ? Cl7 O26 1.368(9) . ? Cl7 O25 1.394(7) . ? Cl7 O27 1.541(9) . ? Cl8 O31 1.298(16) . ? Cl8 O32 1.343(14) . ? Cl8 O29 1.354(12) . ? Cl8 O30 1.358(17) . ? N25 C153 1.115(12) . ? C153 C154 1.510(13) . ? N26 C155 1.078(16) . ? C155 C156 1.442(16) . ? N27 C157 1.107(13) . ? C157 C158 1.472(14) . ? N28 C159 1.08(3) . ? C159 C160 1.56(3) . ? N29 C161 1.154(18) . ? C161 C162 1.444(19) . ? N30 C163 1.106(14) . ? C163 C164 1.516(14) . ? N31 C165 1.210(19) . ? C165 C166 1.45(2) . ? N32 C167 1.230(13) . ? C167 C168 1.591(13) . ? N33 C169 1.206(13) . ? C169 C170 1.576(13) . ? N34 C171 1.121(13) . ? C171 C172 1.513(13) . ? N35 C173 1.204(17) . ? C173 C174 1.566(17) . ? O33 C176 1.21(2) . ? O33 C177 1.44(2) . ? C175 C176 1.44(3) . ? C177 C178 1.53(3) . ? O34 C181 1.34(5) . ? O34 C180 1.65(6) . ? C179 C180 1.39(6) . ? C181 C182 1.64(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Fe1 N4 89.7(2) . . ? N7 Fe1 N1 90.5(2) . . ? N4 Fe1 N1 178.4(2) . . ? N7 Fe1 N8 61.6(2) . . ? N4 Fe1 N8 88.0(2) . . ? N1 Fe1 N8 90.7(2) . . ? N7 Fe1 N11 160.6(2) . . ? N4 Fe1 N11 92.8(2) . . ? N1 Fe1 N11 87.6(2) . . ? N8 Fe1 N11 137.7(2) . . ? N7 Fe1 N10 99.6(2) . . ? N4 Fe1 N10 92.3(2) . . ? N1 Fe1 N10 89.3(2) . . ? N8 Fe1 N10 161.2(2) . . ? N11 Fe1 N10 61.1(2) . . ? N9 Fe2 N12 171.5(2) . . ? N9 Fe2 N6 93.1(2) . . ? N12 Fe2 N6 91.6(2) . . ? N9 Fe2 N3 95.6(2) . . ? N12 Fe2 N3 89.7(2) . . ? N6 Fe2 N3 107.8(2) . . ? N9 Fe2 N2 91.1(2) . . ? N12 Fe2 N2 85.8(2) . . ? N6 Fe2 N2 167.9(2) . . ? N3 Fe2 N2 60.5(2) . . ? N9 Fe2 N5 87.4(2) . . ? N12 Fe2 N5 88.8(2) . . ? N6 Fe2 N5 60.0(2) . . ? N3 Fe2 N5 167.6(2) . . ? N2 Fe2 N5 131.6(2) . . ? C1 N1 C19 118.5(7) . . ? C1 N1 Fe1 120.3(5) . . ? C19 N1 Fe1 121.2(5) . . ? C18 N2 C19 117.7(7) . . ? C18 N2 Fe2 92.7(5) . . ? C19 N2 Fe2 149.5(5) . . ? C17 N3 C18 119.8(7) . . ? C17 N3 Fe2 146.0(6) . . ? C18 N3 Fe2 94.2(5) . . ? C20 N4 C38 117.0(7) . . ? C20 N4 Fe1 122.5(6) . . ? C38 N4 Fe1 120.5(5) . . ? C37 N5 C38 117.3(7) . . ? C37 N5 Fe2 92.2(5) . . ? C38 N5 Fe2 150.4(6) . . ? C36 N6 C37 119.2(7) . . ? C36 N6 Fe2 145.0(6) . . ? C37 N6 Fe2 95.7(5) . . ? C39 N7 C57 118.5(7) . . ? C39 N7 Fe1 147.9(6) . . ? C57 N7 Fe1 93.6(5) . . ? C56 N8 C57 118.6(7) . . ? C56 N8 Fe1 147.7(6) . . ? C57 N8 Fe1 93.6(5) . . ? C55 N9 C56 117.2(7) . . ? C55 N9 Fe2 119.9(5) . . ? C56 N9 Fe2 122.9(5) . . ? C58 N10 C76 118.0(7) . . ? C58 N10 Fe1 148.8(6) . . ? C76 N10 Fe1 93.2(4) . . ? C75 N11 C76 118.4(7) . . ? C75 N11 Fe1 147.0(5) . . ? C76 N11 Fe1 94.5(5) . . ? C74 N12 C75 117.8(7) . . ? C74 N12 Fe2 119.0(5) . . ? C75 N12 Fe2 123.2(5) . . ? N1 C1 C2 124.0(7) . . ? C3 C2 C7 120.1(8) . . ? C3 C2 C1 121.1(8) . . ? C7 C2 C1 118.8(7) . . ? C4 C3 C2 120.3(9) . . ? C3 C4 C5 119.8(8) . . ? C6 C5 C4 119.8(9) . . ? C5 C6 C7 121.9(9) . . ? C6 C7 C2 118.0(8) . . ? C6 C7 C8 124.5(8) . . ? C2 C7 C8 117.4(8) . . ? C9 C8 C19 117.9(7) . . ? C9 C8 C7 123.8(8) . . ? C19 C8 C7 118.3(7) . . ? C8 C9 C10 121.0(7) . . ? C9 C10 C18 115.8(7) . . ? C9 C10 C11 126.2(8) . . ? C18 C10 C11 118.1(7) . . ? C16 C11 C12 119.1(8) . . ? C16 C11 C10 116.4(7) . . ? C12 C11 C10 124.5(8) . . ? C13 C12 C11 119.8(8) . . ? C12 C13 C14 120.8(8) . . ? C15 C14 C13 120.2(8) . . ? C14 C15 C16 120.5(8) . . ? C15 C16 C17 120.8(8) . . ? C15 C16 C11 119.5(8) . . ? C17 C16 C11 119.7(7) . . ? N3 C17 C16 123.7(8) . . ? N2 C18 N3 112.6(7) . . ? N2 C18 C10 125.0(7) . . ? N3 C18 C10 122.4(7) . . ? N2 C19 N1 114.4(7) . . ? N2 C19 C8 122.5(7) . . ? N1 C19 C8 123.1(7) . . ? N4 C20 C21 125.7(8) . . ? C20 C21 C26 119.4(8) . . ? C20 C21 C22 121.0(9) . . ? C26 C21 C22 119.6(8) . . ? C23 C22 C21 119.8(9) . . ? C22 C23 C24 120.9(9) . . ? C25 C24 C23 120.0(9) . . ? C26 C25 C24 118.6(9) . . ? C25 C26 C21 121.1(8) . . ? C25 C26 C27 122.9(8) . . ? C21 C26 C27 116.0(8) . . ? C28 C27 C38 118.3(8) . . ? C28 C27 C26 123.4(8) . . ? C38 C27 C26 118.4(8) . . ? C27 C28 C29 120.6(8) . . ? C37 C29 C28 116.1(8) . . ? C37 C29 C30 118.5(7) . . ? C28 C29 C30 125.5(7) . . ? C31 C30 C35 118.9(8) . . ? C31 C30 C29 125.2(8) . . ? C35 C30 C29 115.9(8) . . ? C32 C31 C30 120.4(9) . . ? C31 C32 C33 120.7(9) . . ? C34 C33 C32 120.5(9) . . ? C33 C34 C35 120.9(9) . . ? C34 C35 C36 121.9(8) . . ? C34 C35 C30 118.7(8) . . ? C36 C35 C30 119.4(8) . . ? N6 C36 C35 123.8(8) . . ? N5 C37 N6 112.1(7) . . ? N5 C37 C29 124.7(8) . . ? N6 C37 C29 123.2(7) . . ? N5 C38 N4 113.5(7) . . ? N5 C38 C27 122.9(8) . . ? N4 C38 C27 123.6(7) . . ? N7 C39 C40 122.9(8) . . ? C41 C40 C45 119.8(9) . . ? C41 C40 C39 119.8(9) . . ? C45 C40 C39 120.5(8) . . ? C42 C41 C40 119.2(10) . . ? C41 C42 C43 121.1(9) . . ? C44 C43 C42 120.2(9) . . ? C43 C44 C45 121.1(9) . . ? C44 C45 C40 118.7(8) . . ? C44 C45 C46 124.9(8) . . ? C40 C45 C46 116.4(8) . . ? C47 C46 C57 116.9(8) . . ? C47 C46 C45 126.7(8) . . ? C57 C46 C45 116.5(7) . . ? C48 C47 C46 120.5(8) . . ? C47 C48 C56 118.3(7) . . ? C47 C48 C49 122.5(8) . . ? C56 C48 C49 119.1(8) . . ? C50 C49 C54 119.1(8) . . ? C50 C49 C48 124.5(9) . . ? C54 C49 C48 116.3(8) . . ? C49 C50 C51 119.8(10) . . ? C50 C51 C52 120.5(10) . . ? C53 C52 C51 120.8(9) . . ? C52 C53 C54 119.6(9) . . ? C53 C54 C49 120.2(8) . . ? C53 C54 C55 121.1(8) . . ? C49 C54 C55 118.8(7) . . ? N9 C55 C54 125.5(8) . . ? N8 C56 N9 114.8(7) . . ? N8 C56 C48 122.0(7) . . ? N9 C56 C48 123.1(7) . . ? N8 C57 N7 111.1(7) . . ? N8 C57 C46 123.7(7) . . ? N7 C57 C46 125.2(7) . . ? N10 C58 C59 122.2(8) . . ? C64 C59 C60 120.9(8) . . ? C64 C59 C58 120.9(7) . . ? C60 C59 C58 118.2(8) . . ? C61 C60 C59 118.6(9) . . ? C60 C61 C62 120.9(8) . . ? C63 C62 C61 121.7(8) . . ? C62 C63 C64 118.0(8) . . ? C59 C64 C63 120.0(8) . . ? C59 C64 C65 117.4(8) . . ? C63 C64 C65 122.6(8) . . ? C66 C65 C76 115.8(7) . . ? C66 C65 C64 127.4(8) . . ? C76 C65 C64 116.7(7) . . ? C67 C66 C65 121.3(8) . . ? C66 C67 C75 118.1(7) . . ? C66 C67 C68 122.9(7) . . ? C75 C67 C68 119.0(7) . . ? C69 C68 C73 118.9(8) . . ? C69 C68 C67 124.6(8) . . ? C73 C68 C67 116.5(7) . . ? C68 C69 C70 119.0(9) . . ? C71 C70 C69 121.5(9) . . ? C72 C71 C70 120.9(8) . . ? C71 C72 C73 120.1(8) . . ? C74 C73 C72 120.8(7) . . ? C74 C73 C68 119.5(7) . . ? C72 C73 C68 119.6(8) . . ? N12 C74 C73 124.3(7) . . ? N11 C75 N12 115.0(7) . . ? N11 C75 C67 122.2(7) . . ? N12 C75 C67 122.8(7) . . ? N11 C76 N10 111.0(7) . . ? N11 C76 C65 124.2(7) . . ? N10 C76 C65 124.8(7) . . ? N13 Fe3 N16 174.1(2) . . ? N13 Fe3 N22 93.5(3) . . ? N16 Fe3 N22 90.3(3) . . ? N13 Fe3 N19 91.2(3) . . ? N16 Fe3 N19 91.9(3) . . ? N22 Fe3 N19 108.1(3) . . ? N13 Fe3 N23 91.8(3) . . ? N16 Fe3 N23 86.2(2) . . ? N22 Fe3 N23 60.3(3) . . ? N19 Fe3 N23 168.1(3) . . ? N13 Fe3 N20 88.6(3) . . ? N16 Fe3 N20 88.6(2) . . ? N22 Fe3 N20 168.4(3) . . ? N19 Fe3 N20 60.4(3) . . ? N23 Fe3 N20 131.1(3) . . ? N21 Fe4 N15 91.9(3) . . ? N21 Fe4 N24 176.8(3) . . ? N15 Fe4 N24 91.3(3) . . ? N21 Fe4 N18 91.9(3) . . ? N15 Fe4 N18 103.7(3) . . ? N24 Fe4 N18 87.7(3) . . ? N21 Fe4 N17 89.6(3) . . ? N15 Fe4 N17 164.2(3) . . ? N24 Fe4 N17 87.5(3) . . ? N18 Fe4 N17 60.6(3) . . ? N21 Fe4 N14 91.0(3) . . ? N15 Fe4 N14 61.2(2) . . ? N24 Fe4 N14 90.2(3) . . ? N18 Fe4 N14 164.7(2) . . ? N17 Fe4 N14 134.5(2) . . ? C77 N13 C95 117.3(7) . . ? C77 N13 Fe3 121.3(5) . . ? C95 N13 Fe3 121.4(5) . . ? C95 N14 C94 118.2(7) . . ? C95 N14 Fe4 148.6(6) . . ? C94 N14 Fe4 93.2(5) . . ? C93 N15 C94 117.0(7) . . ? C93 N15 Fe4 148.3(6) . . ? C94 N15 Fe4 94.7(5) . . ? C96 N16 C114 118.3(7) . . ? C96 N16 Fe3 118.5(6) . . ? C114 N16 Fe3 123.2(5) . . ? C114 N17 C113 118.4(7) . . ? C114 N17 Fe4 146.4(6) . . ? C113 N17 Fe4 95.2(5) . . ? C112 N18 C113 116.1(7) . . ? C112 N18 Fe4 149.2(6) . . ? C113 N18 Fe4 94.6(5) . . ? C115 N19 C133 119.5(8) . . ? C115 N19 Fe3 145.5(7) . . ? C133 N19 Fe3 95.1(5) . . ? C132 N20 C133 119.6(7) . . ? C132 N20 Fe3 149.2(6) . . ? C133 N20 Fe3 91.1(5) . . ? C131 N21 C132 118.6(8) . . ? C131 N21 Fe4 121.4(6) . . ? C132 N21 Fe4 119.9(6) . . ? C134 N22 C152 118.1(8) . . ? C134 N22 Fe3 146.7(6) . . ? C152 N22 Fe3 94.8(5) . . ? C152 N23 C151 118.6(8) . . ? C152 N23 Fe3 92.7(5) . . ? C151 N23 Fe3 148.6(6) . . ? C150 N24 C151 119.4(7) . . ? C150 N24 Fe4 119.6(6) . . ? C151 N24 Fe4 120.7(5) . . ? N13 C77 C78 125.6(7) . . ? C83 C78 C79 119.6(8) . . ? C83 C78 C77 118.9(7) . . ? C79 C78 C77 121.5(8) . . ? C80 C79 C78 120.6(8) . . ? C79 C80 C81 119.3(8) . . ? C82 C81 C80 122.5(9) . . ? C81 C82 C83 118.8(9) . . ? C78 C83 C82 119.1(8) . . ? C78 C83 C84 117.4(8) . . ? C82 C83 C84 123.5(8) . . ? C85 C84 C95 117.6(7) . . ? C85 C84 C83 124.1(8) . . ? C95 C84 C83 118.3(7) . . ? C86 C85 C84 119.7(8) . . ? C85 C86 C94 117.8(7) . . ? C85 C86 C87 124.6(8) . . ? C94 C86 C87 117.4(8) . . ? C88 C87 C92 118.2(8) . . ? C88 C87 C86 124.7(8) . . ? C92 C87 C86 117.0(8) . . ? C89 C88 C87 120.9(9) . . ? C90 C89 C88 119.7(9) . . ? C91 C90 C89 120.7(8) . . ? C90 C91 C92 119.8(9) . . ? C91 C92 C87 120.6(9) . . ? C91 C92 C93 119.7(9) . . ? C87 C92 C93 119.7(8) . . ? N15 C93 C92 124.4(8) . . ? N14 C94 C86 124.7(8) . . ? N14 C94 N15 110.9(7) . . ? C86 C94 N15 124.4(7) . . ? N14 C95 N13 115.5(7) . . ? N14 C95 C84 122.0(7) . . ? N13 C95 C84 122.5(7) . . ? N16 C96 C97 124.5(8) . . ? C98 C97 C102 121.3(8) . . ? C98 C97 C96 120.0(8) . . ? C102 C97 C96 118.7(8) . . ? C99 C98 C97 119.9(9) . . ? C98 C99 C100 120.2(9) . . ? C101 C100 C99 120.6(9) . . ? C100 C101 C102 120.0(9) . . ? C101 C102 C97 117.9(8) . . ? C101 C102 C103 124.8(8) . . ? C97 C102 C103 117.2(7) . . ? C104 C103 C114 118.2(7) . . ? C104 C103 C102 123.1(8) . . ? C114 C103 C102 118.7(7) . . ? C105 C104 C103 120.4(8) . . ? C104 C105 C113 117.4(8) . . ? C104 C105 C106 125.8(8) . . ? C113 C105 C106 116.8(8) . . ? C107 C106 C111 119.1(8) . . ? C107 C106 C105 123.1(8) . . ? C111 C106 C105 117.8(8) . . ? C106 C107 C108 118.9(9) . . ? C107 C108 C109 121.6(9) . . ? C110 C109 C108 119.7(9) . . ? C109 C110 C111 119.3(10) . . ? C106 C111 C110 121.4(9) . . ? C106 C111 C112 118.9(8) . . ? C110 C111 C112 119.6(9) . . ? N18 C112 C111 124.2(8) . . ? N17 C113 C105 124.2(8) . . ? N17 C113 N18 109.6(7) . . ? C105 C113 N18 126.1(7) . . ? N17 C114 N16 116.1(7) . . ? N17 C114 C103 121.3(7) . . ? N16 C114 C103 122.6(7) . . ? N19 C115 C116 123.3(9) . . ? C121 C116 C117 119.7(10) . . ? C121 C116 C115 119.6(8) . . ? C117 C116 C115 120.7(10) . . ? C118 C117 C116 120.6(11) . . ? C117 C118 C119 119.4(10) . . ? C120 C119 C118 121.6(11) . . ? C119 C120 C121 119.5(11) . . ? C120 C121 C116 119.3(9) . . ? C120 C121 C122 124.1(10) . . ? C116 C121 C122 116.6(9) . . ? C123 C122 C133 116.1(8) . . ? C123 C122 C121 126.0(9) . . ? C133 C122 C121 117.9(9) . . ? C122 C123 C124 120.8(8) . . ? C123 C124 C132 118.3(8) . . ? C123 C124 C125 123.4(9) . . ? C132 C124 C125 118.3(8) . . ? C126 C125 C130 119.3(11) . . ? C126 C125 C124 124.2(10) . . ? C130 C125 C124 116.5(10) . . ? C127 C126 C125 119.9(12) . . ? C126 C127 C128 121.8(13) . . ? C129 C128 C127 118.1(13) . . ? C128 C129 C130 122.4(13) . . ? C129 C130 C131 122.9(11) . . ? C129 C130 C125 118.4(11) . . ? C131 C130 C125 118.7(10) . . ? N21 C131 C130 125.4(9) . . ? N20 C132 N21 116.1(8) . . ? N20 C132 C124 121.6(8) . . ? N21 C132 C124 122.3(8) . . ? N20 C133 N19 113.5(7) . . ? N20 C133 C122 123.6(8) . . ? N19 C133 C122 123.0(8) . . ? N22 C134 C135 124.0(8) . . ? C136 C135 C140 119.8(9) . . ? C136 C135 C134 120.0(9) . . ? C140 C135 C134 120.2(8) . . ? C137 C136 C135 120.6(9) . . ? C136 C137 C138 118.9(9) . . ? C139 C138 C137 120.4(10) . . ? C140 C139 C138 120.1(10) . . ? C139 C140 C135 120.1(9) . . ? C139 C140 C141 124.0(9) . . ? C135 C140 C141 115.8(8) . . ? C142 C141 C152 114.8(9) . . ? C142 C141 C140 125.8(9) . . ? C152 C141 C140 119.4(8) . . ? C141 C142 C143 121.0(9) . . ? C142 C143 C151 118.6(9) . . ? C142 C143 C144 123.5(10) . . ? C151 C143 C144 118.0(9) . . ? C145 C144 C149 118.2(11) . . ? C145 C144 C143 124.0(11) . . ? C149 C144 C143 117.2(10) . . ? C144 C145 C146 122.8(12) . . ? C145 C146 C147 117.7(13) . . ? C148 C147 C146 118.7(12) . . ? C147 C148 C149 119.7(12) . . ? C148 C149 C144 122.4(11) . . ? C148 C149 C150 118.5(10) . . ? C144 C149 C150 119.1(9) . . ? N24 C150 C149 123.6(8) . . ? N23 C151 N24 116.1(8) . . ? N23 C151 C143 121.3(8) . . ? N24 C151 C143 122.5(8) . . ? N23 C152 N22 112.1(7) . . ? N23 C152 C141 125.5(8) . . ? N22 C152 C141 122.3(8) . . ? O4 Cl1 O2 108.6(5) . . ? O4 Cl1 O1 108.4(5) . . ? O2 Cl1 O1 110.2(4) . . ? O4 Cl1 O3 109.2(5) . . ? O2 Cl1 O3 110.8(4) . . ? O1 Cl1 O3 109.6(4) . . ? O7 Cl2 O8 109.4(7) . . ? O7 Cl2 O6 110.8(6) . . ? O8 Cl2 O6 111.5(7) . . ? O7 Cl2 O5 109.1(8) . . ? O8 Cl2 O5 107.4(7) . . ? O6 Cl2 O5 108.7(6) . . ? O12 Cl3 O11 108.7(6) . . ? O12 Cl3 O10 108.4(7) . . ? O11 Cl3 O10 110.9(5) . . ? O12 Cl3 O9 109.4(6) . . ? O11 Cl3 O9 110.7(6) . . ? O10 Cl3 O9 108.7(5) . . ? O14 Cl4 O13 113.1(8) . . ? O14 Cl4 O15 115.0(8) . . ? O13 Cl4 O15 120.1(9) . . ? O14 Cl4 O16 101.2(9) . . ? O13 Cl4 O16 104.3(7) . . ? O15 Cl4 O16 99.3(9) . . ? O19 Cl5 O17 119.5(7) . . ? O19 Cl5 O18 118.0(7) . . ? O17 Cl5 O18 114.0(6) . . ? O19 Cl5 O20 98.4(8) . . ? O17 Cl5 O20 101.4(7) . . ? O18 Cl5 O20 99.7(7) . . ? O22 Cl6 O23 112.1(9) . . ? O22 Cl6 O21 112.6(7) . . ? O23 Cl6 O21 110.1(6) . . ? O22 Cl6 O24 105.9(11) . . ? O23 Cl6 O24 106.3(10) . . ? O21 Cl6 O24 109.7(8) . . ? O28 Cl7 O26 121.4(7) . . ? O28 Cl7 O25 115.9(6) . . ? O26 Cl7 O25 115.0(6) . . ? O28 Cl7 O27 99.3(7) . . ? O26 Cl7 O27 97.8(6) . . ? O25 Cl7 O27 101.0(5) . . ? O31 Cl8 O32 103.9(17) . . ? O31 Cl8 O29 117.8(15) . . ? O32 Cl8 O29 100.1(10) . . ? O31 Cl8 O30 102.1(11) . . ? O32 Cl8 O30 116.3(15) . . ? O29 Cl8 O30 116.6(12) . . ? N25 C153 C154 179(2) . . ? N26 C155 C156 176(2) . . ? N27 C157 C158 178.7(13) . . ? N28 C159 C160 175(2) . . ? N29 C161 C162 179.0(17) . . ? N30 C163 C164 177.9(14) . . ? N31 C165 C166 177.3(17) . . ? N32 C167 C168 177(3) . . ? N33 C169 C170 171(3) . . ? N34 C171 C172 176(4) . . ? N35 C173 C174 164(6) . . ? C176 O33 C177 120.5(15) . . ? O33 C176 C175 118.9(16) . . ? O33 C177 C178 112.8(15) . . ? C181 O34 C180 106(4) . . ? C179 C180 O34 119(5) . . ? O34 C181 C182 85(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 67.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.606 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.130