# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Jing-Ping Zhang' _publ_contact_author_address ; Faculty of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email zhangjingping66@yahoo.cn _publ_contact_author_fax +86-431-85098652 _publ_contact_author_phone +86-431-85099521 loop_ _publ_author_name 'Bo Li' 'Jingping Zhang' #============================================================================= data_CCDC-661243 _database_code_depnum_ccdc_archive 'CCDC 661243' #TrackingRef '- CCDC-661243.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H42 Co3 N16 O3' _chemical_formula_weight 1187.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9005(11) _cell_length_b 14.3387(12) _cell_length_c 16.4886(13) _cell_angle_alpha 71.040(1) _cell_angle_beta 81.626(1) _cell_angle_gamma 65.462(1) _cell_volume 2623.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1214 _exptl_absorpt_coefficient_mu 1.001 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6902 _exptl_absorpt_correction_T_max 0.8249 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13722 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.03 _reflns_number_total 9130 _reflns_number_gt 7104 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9130 _refine_ls_number_parameters 731 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.78611(4) 0.39075(3) 0.16921(3) 0.02686(13) Uani 1 1 d . . . Co2 Co 0.72976(3) 0.73858(3) 0.22547(2) 0.02291(12) Uani 1 1 d . . . Co3 Co 1.12698(4) 0.67443(3) 0.30333(3) 0.02488(13) Uani 1 1 d . . . C1 C 0.7774(3) 0.2723(3) 0.1468(2) 0.0312(8) Uani 1 1 d . . . C2 C 0.9388(3) 0.3098(2) 0.2021(2) 0.0296(7) Uani 1 1 d . . . C3 C 0.7430(3) 0.3428(3) 0.2839(2) 0.0372(8) Uani 1 1 d . . . C4 C 0.7876(3) 0.5131(3) 0.19027(19) 0.0262(7) Uani 1 1 d . . . C5 C 1.2769(3) 0.6578(3) 0.3230(2) 0.0330(8) Uani 1 1 d . . . C6 C 1.1898(3) 0.5295(3) 0.3067(2) 0.0337(8) Uani 1 1 d . . . C7 C 1.1491(3) 0.7161(3) 0.1845(2) 0.0321(8) Uani 1 1 d . . . C8 C 0.9815(3) 0.6856(2) 0.28128(18) 0.0247(7) Uani 1 1 d . . . C9 C 0.9246(3) 0.4198(3) 0.0075(2) 0.0313(8) Uani 1 1 d . . . H9 H 0.9891 0.3691 0.0387 0.038 Uiso 1 1 calc R . . C10 C 0.9374(3) 0.4676(3) -0.0792(2) 0.0371(8) Uani 1 1 d . . . H10 H 1.0092 0.4481 -0.1051 0.045 Uiso 1 1 calc R . . C11 C 0.8442(3) 0.5433(3) -0.1265(2) 0.0376(8) Uani 1 1 d . . . H11 H 0.8526 0.5769 -0.1842 0.045 Uiso 1 1 calc R . . C12 C 0.7349(3) 0.5703(3) -0.0870(2) 0.0319(8) Uani 1 1 d . . . C13 C 0.6302(3) 0.6467(3) -0.1293(2) 0.0385(9) Uani 1 1 d . . . H13 H 0.6319 0.6842 -0.1869 0.046 Uiso 1 1 calc R . . C14 C 0.5293(3) 0.6651(3) -0.0869(2) 0.0376(9) Uani 1 1 d . . . H14 H 0.4627 0.7142 -0.1161 0.045 Uiso 1 1 calc R . . C15 C 0.5227(3) 0.6103(2) 0.0025(2) 0.0305(8) Uani 1 1 d . . . C16 C 0.4207(3) 0.6240(3) 0.0513(2) 0.0369(9) Uani 1 1 d . . . H16 H 0.3508 0.6715 0.0260 0.044 Uiso 1 1 calc R . . C17 C 0.4260(3) 0.5665(3) 0.1360(2) 0.0380(9) Uani 1 1 d . . . H17 H 0.3593 0.5743 0.1685 0.046 Uiso 1 1 calc R . . C18 C 0.5304(3) 0.4965(3) 0.1738(2) 0.0350(8) Uani 1 1 d . . . H18 H 0.5322 0.4594 0.2318 0.042 Uiso 1 1 calc R . . C19 C 0.6242(3) 0.5364(2) 0.0453(2) 0.0276(7) Uani 1 1 d . . . C20 C 0.7303(3) 0.5164(2) 0.0005(2) 0.0265(7) Uani 1 1 d . . . C21 C 0.8723(3) 0.8138(3) 0.0642(2) 0.0341(8) Uani 1 1 d . . . H21 H 0.9288 0.7949 0.1026 0.041 Uiso 1 1 calc R . . C22 C 0.8967(3) 0.8450(3) -0.0240(2) 0.0411(9) Uani 1 1 d . . . H22 H 0.9676 0.8468 -0.0430 0.049 Uiso 1 1 calc R . . C23 C 0.8151(3) 0.8727(3) -0.0810(2) 0.0403(9) Uani 1 1 d . . . H23 H 0.8304 0.8920 -0.1396 0.048 Uiso 1 1 calc R . . C24 C 0.7075(3) 0.8722(2) -0.0512(2) 0.0331(8) Uani 1 1 d . . . C25 C 0.6156(4) 0.9036(3) -0.1061(2) 0.0441(10) Uani 1 1 d . . . H25 H 0.6266 0.9239 -0.1652 0.053 Uiso 1 1 calc R . . C26 C 0.5133(4) 0.9043(3) -0.0738(2) 0.0440(10) Uani 1 1 d . . . H26 H 0.4543 0.9274 -0.1113 0.053 Uiso 1 1 calc R . . C27 C 0.4928(3) 0.8703(3) 0.0168(2) 0.0358(8) Uani 1 1 d . . . C28 C 0.3892(3) 0.8672(3) 0.0540(3) 0.0434(10) Uani 1 1 d . . . H28 H 0.3272 0.8900 0.0196 0.052 Uiso 1 1 calc R . . C29 C 0.3794(3) 0.8307(3) 0.1407(2) 0.0407(9) Uani 1 1 d . . . H29 H 0.3111 0.8278 0.1659 0.049 Uiso 1 1 calc R . . C30 C 0.4737(3) 0.7976(3) 0.1917(2) 0.0349(8) Uani 1 1 d . . . H30 H 0.4662 0.7723 0.2509 0.042 Uiso 1 1 calc R . . C31 C 0.5833(3) 0.8366(2) 0.0729(2) 0.0272(7) Uani 1 1 d . . . C32 C 0.6908(3) 0.8394(2) 0.0382(2) 0.0280(7) Uani 1 1 d . . . C33 C 0.6454(3) 0.5903(3) 0.3814(2) 0.0318(8) Uani 1 1 d . . . H33 H 0.6565 0.5482 0.3457 0.038 Uiso 1 1 calc R . . C34 C 0.6124(3) 0.5546(3) 0.4664(2) 0.0360(8) Uani 1 1 d . . . H34 H 0.6016 0.4907 0.4862 0.043 Uiso 1 1 calc R . . C35 C 0.5962(3) 0.6149(3) 0.5202(2) 0.0384(9) Uani 1 1 d . . . H35 H 0.5745 0.5923 0.5771 0.046 Uiso 1 1 calc R . . C36 C 0.6127(3) 0.7117(3) 0.4883(2) 0.0338(8) Uani 1 1 d . . . C37 C 0.6002(3) 0.7794(3) 0.5397(2) 0.0467(10) Uani 1 1 d . . . H37 H 0.5800 0.7597 0.5973 0.056 Uiso 1 1 calc R . . C38 C 0.6173(3) 0.8710(3) 0.5062(2) 0.0457(10) Uani 1 1 d . . . H38 H 0.6097 0.9126 0.5415 0.055 Uiso 1 1 calc R . . C39 C 0.6467(3) 0.9059(3) 0.4181(2) 0.0356(8) Uani 1 1 d . . . C40 C 0.6639(3) 1.0012(3) 0.3793(3) 0.0449(10) Uani 1 1 d . . . H40 H 0.6554 1.0466 0.4114 0.054 Uiso 1 1 calc R . . C41 C 0.6932(3) 1.0272(3) 0.2944(3) 0.0441(9) Uani 1 1 d . . . H41 H 0.7041 1.0905 0.2682 0.053 Uiso 1 1 calc R . . C42 C 0.7065(3) 0.9575(2) 0.2471(2) 0.0332(8) Uani 1 1 d . . . H42 H 0.7290 0.9748 0.1899 0.040 Uiso 1 1 calc R . . C43 C 0.6593(3) 0.8414(2) 0.3654(2) 0.0275(7) Uani 1 1 d . . . C44 C 0.6437(3) 0.7421(2) 0.40162(19) 0.0269(7) Uani 1 1 d . . . C45 C 1.1085(3) 0.5504(3) 0.4871(2) 0.0304(7) Uani 1 1 d . . . H45 H 1.1444 0.4874 0.4714 0.037 Uiso 1 1 calc R . . C46 C 1.0743(3) 0.5435(3) 0.5720(2) 0.0361(8) Uani 1 1 d . . . H46 H 1.0878 0.4766 0.6118 0.043 Uiso 1 1 calc R . . C47 C 1.0212(3) 0.6338(3) 0.5974(2) 0.0396(9) Uani 1 1 d . . . H47 H 0.9993 0.6292 0.6544 0.048 Uiso 1 1 calc R . . C48 C 1.0001(3) 0.7348(3) 0.5358(2) 0.0349(8) Uani 1 1 d . . . C49 C 0.9420(3) 0.8359(3) 0.5534(2) 0.0471(10) Uani 1 1 d . . . H49 H 0.9150 0.8373 0.6086 0.057 Uiso 1 1 calc R . . C50 C 0.9257(3) 0.9294(3) 0.4909(2) 0.0458(10) Uani 1 1 d . . . H50 H 0.8884 0.9938 0.5041 0.055 Uiso 1 1 calc R . . C51 C 0.9647(3) 0.9308(3) 0.4053(2) 0.0348(8) Uani 1 1 d . . . C52 C 0.9524(3) 1.0242(3) 0.3378(2) 0.0426(9) Uani 1 1 d . . . H52 H 0.9173 1.0912 0.3471 0.051 Uiso 1 1 calc R . . C53 C 0.9928(3) 1.0156(3) 0.2576(2) 0.0403(9) Uani 1 1 d . . . H53 H 0.9857 1.0769 0.2125 0.048 Uiso 1 1 calc R . . C54 C 1.0443(3) 0.9153(3) 0.2438(2) 0.0351(8) Uani 1 1 d . . . H54 H 1.0693 0.9113 0.1887 0.042 Uiso 1 1 calc R . . C55 C 1.0199(3) 0.8333(2) 0.3862(2) 0.0274(7) Uani 1 1 d . . . C56 C 1.0378(3) 0.7345(2) 0.4520(2) 0.0275(7) Uani 1 1 d . . . C57 C 0.6826(6) 0.0619(5) 0.6439(3) 0.118(3) Uani 1 1 d . . . H57A H 0.6248 0.0448 0.6289 0.177 Uiso 1 1 calc R . . H57B H 0.6612 0.0812 0.6963 0.177 Uiso 1 1 calc R . . H57C H 0.7537 0.0006 0.6514 0.177 Uiso 1 1 calc R . . C58 C 0.6966(5) 0.1638(4) 0.5662(3) 0.0864(19) Uani 1 1 d . . . H58A H 0.6370 0.2311 0.5707 0.104 Uiso 1 1 calc R . . H58B H 0.7699 0.1661 0.5696 0.104 Uiso 1 1 calc R . . N1 N 0.7703(3) 0.2030(2) 0.13123(19) 0.0433(8) Uani 1 1 d . . . N2 N 1.0326(3) 0.2626(2) 0.22070(18) 0.0403(7) Uani 1 1 d . . . N3 N 0.7156(3) 0.3131(3) 0.3538(2) 0.0600(10) Uani 1 1 d . . . N4 N 0.7778(2) 0.5925(2) 0.19906(16) 0.0298(6) Uani 1 1 d . . . N5 N 1.3685(3) 0.6429(3) 0.3348(2) 0.0505(9) Uani 1 1 d . . . N6 N 1.2279(3) 0.4392(2) 0.31211(19) 0.0494(9) Uani 1 1 d . . . N7 N 1.1567(3) 0.7480(3) 0.11075(19) 0.0475(8) Uani 1 1 d . . . N8 N 0.8929(2) 0.6939(2) 0.26720(16) 0.0268(6) Uani 1 1 d . . . N9 N 0.8244(2) 0.44342(19) 0.04760(16) 0.0262(6) Uani 1 1 d . . . N10 N 0.6284(2) 0.48058(19) 0.12979(17) 0.0284(6) Uani 1 1 d . . . N11 N 0.7734(2) 0.8098(2) 0.09548(16) 0.0276(6) Uani 1 1 d . . . N12 N 0.5731(2) 0.80056(19) 0.15914(16) 0.0277(6) Uani 1 1 d . . . N13 N 0.6618(2) 0.68070(19) 0.34858(16) 0.0249(6) Uani 1 1 d . . . N14 N 0.6884(2) 0.86768(19) 0.28048(16) 0.0262(6) Uani 1 1 d . . . N15 N 1.0919(2) 0.64382(19) 0.42706(15) 0.0238(6) Uani 1 1 d . . . N16 N 1.0590(2) 0.8250(2) 0.30674(16) 0.0264(6) Uani 1 1 d . . . O1W O 0.8835(4) 0.0388(3) 0.0481(3) 0.0984(16) Uani 1 1 d . . . H1A H 0.855(6) 0.074(5) 0.083(4) 0.148 Uiso 1 1 d . . . H1B H 0.899(7) 0.066(6) 0.005(4) 0.148 Uiso 1 1 d . . . O3 O 0.6885(4) 0.1482(3) 0.4936(3) 0.1025(13) Uani 1 1 d D . . H3 H 0.698(6) 0.227(4) 0.446(4) 0.154 Uiso 1 1 d D . . O2W O 0.2548(6) 0.2171(5) 0.2951(4) 0.184(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0271(3) 0.0241(2) 0.0284(2) -0.00908(18) -0.00080(19) -0.0080(2) Co2 0.0202(2) 0.0230(2) 0.0237(2) -0.00406(17) -0.00366(17) -0.00781(18) Co3 0.0195(2) 0.0289(2) 0.0238(2) -0.00553(18) -0.00353(17) -0.00772(19) C1 0.0280(19) 0.0271(18) 0.0322(19) -0.0066(15) -0.0042(15) -0.0054(15) C2 0.034(2) 0.0249(17) 0.0285(18) -0.0095(14) -0.0025(15) -0.0082(16) C3 0.035(2) 0.0312(19) 0.042(2) -0.0121(16) -0.0016(17) -0.0079(17) C4 0.0241(18) 0.0291(18) 0.0224(16) -0.0061(14) -0.0013(13) -0.0083(14) C5 0.033(2) 0.037(2) 0.0252(18) -0.0012(15) -0.0055(15) -0.0144(17) C6 0.030(2) 0.039(2) 0.0260(18) -0.0102(15) -0.0076(15) -0.0061(17) C7 0.0169(17) 0.038(2) 0.035(2) -0.0090(16) 0.0001(15) -0.0060(15) C8 0.0261(19) 0.0211(16) 0.0212(16) -0.0043(13) -0.0011(13) -0.0051(14) C9 0.0298(19) 0.0309(18) 0.0340(19) -0.0139(15) -0.0004(15) -0.0094(15) C10 0.031(2) 0.049(2) 0.039(2) -0.0209(17) 0.0065(16) -0.0186(18) C11 0.046(2) 0.046(2) 0.0293(19) -0.0120(16) 0.0012(17) -0.0255(19) C12 0.036(2) 0.0297(18) 0.0348(19) -0.0113(15) -0.0041(16) -0.0153(16) C13 0.047(2) 0.032(2) 0.035(2) -0.0014(15) -0.0135(17) -0.0162(18) C14 0.037(2) 0.0286(19) 0.044(2) -0.0078(16) -0.0143(17) -0.0078(16) C15 0.0295(19) 0.0219(17) 0.044(2) -0.0142(15) -0.0055(16) -0.0085(15) C16 0.0279(19) 0.0290(19) 0.056(2) -0.0217(17) -0.0075(17) -0.0042(16) C17 0.0258(19) 0.037(2) 0.054(2) -0.0231(18) 0.0037(17) -0.0089(16) C18 0.033(2) 0.035(2) 0.038(2) -0.0166(16) 0.0052(16) -0.0114(16) C19 0.0287(18) 0.0218(17) 0.0366(19) -0.0140(14) -0.0032(15) -0.0089(14) C20 0.0285(18) 0.0228(16) 0.0325(18) -0.0125(14) -0.0036(14) -0.0099(14) C21 0.032(2) 0.0345(19) 0.0323(19) -0.0071(15) 0.0009(15) -0.0120(16) C22 0.039(2) 0.037(2) 0.041(2) -0.0084(16) 0.0092(17) -0.0145(18) C23 0.055(3) 0.033(2) 0.0262(18) -0.0082(15) 0.0056(17) -0.0122(18) C24 0.046(2) 0.0202(17) 0.0278(18) -0.0066(14) -0.0047(16) -0.0074(16) C25 0.064(3) 0.035(2) 0.0277(19) -0.0057(16) -0.0137(19) -0.012(2) C26 0.056(3) 0.033(2) 0.041(2) -0.0043(17) -0.027(2) -0.0119(19) C27 0.039(2) 0.0220(17) 0.046(2) -0.0094(15) -0.0172(17) -0.0068(16) C28 0.036(2) 0.0283(19) 0.065(3) -0.0078(18) -0.027(2) -0.0076(17) C29 0.027(2) 0.0295(19) 0.062(3) -0.0062(17) -0.0088(18) -0.0103(16) C30 0.029(2) 0.0287(19) 0.042(2) -0.0015(15) -0.0057(16) -0.0120(16) C31 0.0320(19) 0.0167(16) 0.0315(18) -0.0075(13) -0.0086(15) -0.0054(14) C32 0.0324(19) 0.0191(16) 0.0295(17) -0.0071(13) -0.0035(15) -0.0065(14) C33 0.0270(18) 0.0329(19) 0.0357(19) -0.0072(15) -0.0017(15) -0.0137(16) C34 0.030(2) 0.035(2) 0.037(2) 0.0020(16) -0.0044(16) -0.0148(16) C35 0.028(2) 0.046(2) 0.0278(18) 0.0014(16) -0.0008(15) -0.0104(17) C36 0.0265(19) 0.038(2) 0.0277(18) -0.0069(15) -0.0022(15) -0.0059(16) C37 0.046(2) 0.057(3) 0.0282(19) -0.0151(18) 0.0002(17) -0.010(2) C38 0.051(3) 0.047(2) 0.039(2) -0.0234(18) -0.0019(18) -0.011(2) C39 0.033(2) 0.034(2) 0.039(2) -0.0165(16) -0.0067(16) -0.0067(16) C40 0.043(2) 0.037(2) 0.063(3) -0.0255(19) -0.005(2) -0.0145(19) C41 0.043(2) 0.030(2) 0.061(3) -0.0089(18) -0.010(2) -0.0157(18) C42 0.0297(19) 0.0284(18) 0.038(2) -0.0021(15) -0.0084(15) -0.0115(15) C43 0.0191(17) 0.0286(17) 0.0303(18) -0.0084(14) -0.0038(14) -0.0040(14) C44 0.0181(16) 0.0295(17) 0.0284(17) -0.0069(14) -0.0034(13) -0.0052(14) C45 0.0242(18) 0.0277(18) 0.0342(19) -0.0032(14) -0.0081(15) -0.0073(15) C46 0.035(2) 0.036(2) 0.0286(19) 0.0048(15) -0.0080(15) -0.0143(17) C47 0.042(2) 0.053(2) 0.0232(18) -0.0061(16) -0.0012(16) -0.0214(19) C48 0.036(2) 0.041(2) 0.0283(18) -0.0082(15) -0.0033(15) -0.0161(17) C49 0.052(3) 0.056(3) 0.035(2) -0.0266(19) 0.0048(18) -0.015(2) C50 0.045(2) 0.043(2) 0.051(2) -0.0236(19) 0.0008(19) -0.0118(19) C51 0.034(2) 0.0316(19) 0.040(2) -0.0122(15) -0.0084(16) -0.0096(16) C52 0.041(2) 0.031(2) 0.055(2) -0.0112(17) -0.0075(19) -0.0116(17) C53 0.037(2) 0.0277(19) 0.048(2) 0.0026(16) -0.0103(18) -0.0119(17) C54 0.034(2) 0.035(2) 0.0317(19) 0.0001(15) -0.0059(15) -0.0150(17) C55 0.0241(17) 0.0278(17) 0.0303(18) -0.0059(14) -0.0070(14) -0.0101(14) C56 0.0224(17) 0.0328(18) 0.0287(17) -0.0076(14) -0.0058(14) -0.0114(15) C57 0.135(6) 0.088(4) 0.071(4) -0.022(3) 0.017(4) 0.006(4) C58 0.094(4) 0.067(3) 0.100(4) -0.052(3) -0.055(3) 0.005(3) N1 0.048(2) 0.0310(17) 0.053(2) -0.0123(15) -0.0102(16) -0.0140(15) N2 0.040(2) 0.0414(18) 0.0332(17) -0.0126(14) -0.0073(14) -0.0060(16) N3 0.070(3) 0.065(2) 0.0337(19) -0.0040(17) 0.0048(18) -0.025(2) N4 0.0303(16) 0.0298(16) 0.0292(15) -0.0109(12) -0.0008(12) -0.0099(13) N5 0.034(2) 0.063(2) 0.047(2) 0.0073(16) -0.0122(15) -0.0253(17) N6 0.056(2) 0.038(2) 0.0416(19) -0.0166(15) -0.0170(16) 0.0025(17) N7 0.0310(18) 0.065(2) 0.0317(18) -0.0091(16) -0.0005(14) -0.0079(16) N8 0.0231(15) 0.0268(15) 0.0280(15) -0.0036(11) -0.0055(12) -0.0091(12) N9 0.0261(15) 0.0222(14) 0.0301(15) -0.0104(11) -0.0024(12) -0.0066(12) N10 0.0261(15) 0.0226(14) 0.0355(16) -0.0115(12) 0.0000(12) -0.0064(12) N11 0.0254(15) 0.0259(14) 0.0269(14) -0.0048(11) -0.0034(12) -0.0069(12) N12 0.0249(15) 0.0218(14) 0.0331(15) -0.0041(11) -0.0064(12) -0.0072(12) N13 0.0215(14) 0.0233(14) 0.0272(14) -0.0045(11) -0.0031(11) -0.0074(11) N14 0.0223(14) 0.0245(14) 0.0288(15) -0.0044(11) -0.0045(12) -0.0075(12) N15 0.0180(14) 0.0252(14) 0.0253(14) -0.0045(11) -0.0046(11) -0.0066(11) N16 0.0210(14) 0.0281(15) 0.0263(14) -0.0025(11) -0.0040(11) -0.0090(12) O1W 0.104(3) 0.083(3) 0.101(3) -0.058(3) -0.019(3) -0.001(2) O3 0.139(4) 0.079(3) 0.088(3) -0.027(2) 0.013(3) -0.043(3) O2W 0.174(6) 0.203(6) 0.177(5) -0.054(4) 0.000(4) -0.080(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 Co1 C2 1.878(4) . ? Co1 C3 1.878(4) . ? Co1 C1 1.900(3) . ? Co1 C4 1.903(3) . ? Co1 N9 1.968(3) . ? Co1 N10 1.971(3) . ? Co2 N8 2.080(3) . ? Co2 N4 2.097(3) . ? Co2 N13 2.138(3) . ? Co2 N12 2.142(3) . ? Co2 N11 2.158(3) . ? Co2 N14 2.159(3) . ? Co3 C7 1.870(3) . ? Co3 C6 1.876(4) . ? Co3 C8 1.894(3) . ? Co3 C5 1.910(4) . ? Co3 N15 1.968(2) . ? Co3 N16 1.981(3) . ? C1 N1 1.145(4) . ? C2 N2 1.144(4) . ? C3 N3 1.149(4) . ? C4 N4 1.147(4) . ? C5 N5 1.145(4) . ? C6 N6 1.155(4) . ? C7 N7 1.157(4) . ? C8 N8 1.150(4) . ? C9 N9 1.326(4) . ? C9 C10 1.389(4) . ? C10 C11 1.368(5) . ? C11 C12 1.416(5) . ? C12 C20 1.403(4) . ? C12 C13 1.434(5) . ? C13 C14 1.350(5) . ? C14 C15 1.436(5) . ? C15 C19 1.403(4) . ? C15 C16 1.413(5) . ? C16 C17 1.367(5) . ? C17 C18 1.388(5) . ? C18 N10 1.332(4) . ? C19 N10 1.358(4) . ? C19 C20 1.422(4) . ? C20 N9 1.365(4) . ? C21 N11 1.321(4) . ? C21 C22 1.405(5) . ? C22 C23 1.361(5) . ? C23 C24 1.406(5) . ? C24 C32 1.408(4) . ? C24 C25 1.425(5) . ? C25 C26 1.347(6) . ? C26 C27 1.436(5) . ? C27 C28 1.399(5) . ? C27 C31 1.417(4) . ? C28 C29 1.359(5) . ? C29 C30 1.403(5) . ? C30 N12 1.329(4) . ? C31 N12 1.353(4) . ? C31 C32 1.433(5) . ? C32 N11 1.365(4) . ? C33 N13 1.326(4) . ? C33 C34 1.396(5) . ? C34 C35 1.368(5) . ? C35 C36 1.409(5) . ? C36 C44 1.403(4) . ? C36 C37 1.431(5) . ? C37 C38 1.347(5) . ? C38 C39 1.424(5) . ? C39 C40 1.403(5) . ? C39 C43 1.412(4) . ? C40 C41 1.367(5) . ? C41 C42 1.399(5) . ? C42 N14 1.330(4) . ? C43 N14 1.366(4) . ? C43 C44 1.440(4) . ? C44 N13 1.365(4) . ? C45 N15 1.335(4) . ? C45 C46 1.390(4) . ? C46 C47 1.363(5) . ? C47 C48 1.415(5) . ? C48 C56 1.397(4) . ? C48 C49 1.432(5) . ? C49 C50 1.355(5) . ? C50 C51 1.424(5) . ? C51 C55 1.398(4) . ? C51 C52 1.401(5) . ? C52 C53 1.373(5) . ? C53 C54 1.391(5) . ? C54 N16 1.331(4) . ? C55 N16 1.358(4) . ? C55 C56 1.428(4) . ? C56 N15 1.362(4) . ? C57 C58 1.657(7) . ? C58 O3 1.313(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Co1 C3 88.39(14) . . ? C2 Co1 C1 90.99(14) . . ? C3 Co1 C1 90.15(14) . . ? C2 Co1 C4 91.68(13) . . ? C3 Co1 C4 89.85(14) . . ? C1 Co1 C4 177.32(14) . . ? C2 Co1 N9 94.01(12) . . ? C3 Co1 N9 177.56(13) . . ? C1 Co1 N9 89.36(12) . . ? C4 Co1 N9 90.53(11) . . ? C2 Co1 N10 177.10(13) . . ? C3 Co1 N10 94.21(13) . . ? C1 Co1 N10 90.29(12) . . ? C4 Co1 N10 87.04(12) . . ? N9 Co1 N10 83.40(11) . . ? N8 Co2 N4 91.28(10) . . ? N8 Co2 N13 96.22(10) . . ? N4 Co2 N13 92.11(10) . . ? N8 Co2 N12 168.75(10) . . ? N4 Co2 N12 90.04(10) . . ? N13 Co2 N12 94.89(10) . . ? N8 Co2 N11 91.62(10) . . ? N4 Co2 N11 89.98(10) . . ? N13 Co2 N11 171.83(10) . . ? N12 Co2 N11 77.21(10) . . ? N8 Co2 N14 83.30(10) . . ? N4 Co2 N14 167.79(10) . . ? N13 Co2 N14 77.68(9) . . ? N12 Co2 N14 97.41(9) . . ? N11 Co2 N14 101.07(9) . . ? C7 Co3 C6 91.01(14) . . ? C7 Co3 C8 87.21(13) . . ? C6 Co3 C8 90.16(13) . . ? C7 Co3 C5 91.54(14) . . ? C6 Co3 C5 87.39(15) . . ? C8 Co3 C5 177.24(14) . . ? C7 Co3 N15 174.62(12) . . ? C6 Co3 N15 93.81(12) . . ? C8 Co3 N15 90.39(11) . . ? C5 Co3 N15 91.06(12) . . ? C7 Co3 N16 92.20(13) . . ? C6 Co3 N16 176.79(12) . . ? C8 Co3 N16 89.84(11) . . ? C5 Co3 N16 92.67(13) . . ? N15 Co3 N16 82.98(10) . . ? N1 C1 Co1 178.0(3) . . ? N2 C2 Co1 178.2(3) . . ? N3 C3 Co1 179.0(4) . . ? N4 C4 Co1 173.0(3) . . ? N5 C5 Co3 176.9(3) . . ? N6 C6 Co3 177.5(3) . . ? N7 C7 Co3 175.6(3) . . ? N8 C8 Co3 179.0(3) . . ? N9 C9 C10 122.8(3) . . ? C11 C10 C9 119.9(3) . . ? C10 C11 C12 119.6(3) . . ? C20 C12 C11 116.3(3) . . ? C20 C12 C13 118.3(3) . . ? C11 C12 C13 125.4(3) . . ? C14 C13 C12 121.2(3) . . ? C13 C14 C15 121.4(3) . . ? C19 C15 C16 116.7(3) . . ? C19 C15 C14 118.3(3) . . ? C16 C15 C14 124.9(3) . . ? C17 C16 C15 119.2(3) . . ? C16 C17 C18 120.3(3) . . ? N10 C18 C17 122.3(3) . . ? N10 C19 C15 123.5(3) . . ? N10 C19 C20 116.3(3) . . ? C15 C19 C20 120.2(3) . . ? N9 C20 C12 123.5(3) . . ? N9 C20 C19 116.0(3) . . ? C12 C20 C19 120.5(3) . . ? N11 C21 C22 123.6(3) . . ? C23 C22 C21 118.9(4) . . ? C22 C23 C24 119.8(3) . . ? C23 C24 C32 117.2(3) . . ? C23 C24 C25 123.7(3) . . ? C32 C24 C25 119.0(3) . . ? C26 C25 C24 121.2(3) . . ? C25 C26 C27 121.8(3) . . ? C28 C27 C31 117.4(3) . . ? C28 C27 C26 124.4(3) . . ? C31 C27 C26 118.3(3) . . ? C29 C28 C27 119.9(3) . . ? C28 C29 C30 119.2(3) . . ? N12 C30 C29 122.9(3) . . ? N12 C31 C27 122.5(3) . . ? N12 C31 C32 117.8(3) . . ? C27 C31 C32 119.7(3) . . ? N11 C32 C24 122.9(3) . . ? N11 C32 C31 117.0(3) . . ? C24 C32 C31 120.1(3) . . ? N13 C33 C34 123.7(3) . . ? C35 C34 C33 119.1(3) . . ? C34 C35 C36 119.3(3) . . ? C44 C36 C35 117.6(3) . . ? C44 C36 C37 118.8(3) . . ? C35 C36 C37 123.6(3) . . ? C38 C37 C36 121.3(3) . . ? C37 C38 C39 121.7(3) . . ? C40 C39 C43 117.1(3) . . ? C40 C39 C38 124.3(3) . . ? C43 C39 C38 118.6(3) . . ? C41 C40 C39 120.0(3) . . ? C40 C41 C42 119.3(3) . . ? N14 C42 C41 122.9(3) . . ? N14 C43 C39 122.8(3) . . ? N14 C43 C44 117.5(3) . . ? C39 C43 C44 119.7(3) . . ? N13 C44 C36 122.9(3) . . ? N13 C44 C43 117.2(3) . . ? C36 C44 C43 119.8(3) . . ? N15 C45 C46 122.6(3) . . ? C47 C46 C45 120.5(3) . . ? C46 C47 C48 118.9(3) . . ? C56 C48 C47 116.9(3) . . ? C56 C48 C49 118.6(3) . . ? C47 C48 C49 124.6(3) . . ? C50 C49 C48 121.1(3) . . ? C49 C50 C51 121.3(3) . . ? C55 C51 C52 116.9(3) . . ? C55 C51 C50 118.7(3) . . ? C52 C51 C50 124.4(3) . . ? C53 C52 C51 119.1(3) . . ? C52 C53 C54 120.2(3) . . ? N16 C54 C53 122.2(3) . . ? N16 C55 C51 123.9(3) . . ? N16 C55 C56 115.9(3) . . ? C51 C55 C56 120.2(3) . . ? N15 C56 C48 124.0(3) . . ? N15 C56 C55 115.9(3) . . ? C48 C56 C55 120.1(3) . . ? O3 C58 C57 106.6(4) . . ? C4 N4 Co2 169.1(3) . . ? C8 N8 Co2 168.6(2) . . ? C9 N9 C20 117.9(3) . . ? C9 N9 Co1 130.0(2) . . ? C20 N9 Co1 112.1(2) . . ? C18 N10 C19 118.0(3) . . ? C18 N10 Co1 129.9(2) . . ? C19 N10 Co1 112.1(2) . . ? C21 N11 C32 117.4(3) . . ? C21 N11 Co2 128.8(2) . . ? C32 N11 Co2 113.0(2) . . ? C30 N12 C31 118.1(3) . . ? C30 N12 Co2 127.9(2) . . ? C31 N12 Co2 113.7(2) . . ? C33 N13 C44 117.3(3) . . ? C33 N13 Co2 128.7(2) . . ? C44 N13 Co2 113.7(2) . . ? C42 N14 C43 117.9(3) . . ? C42 N14 Co2 128.2(2) . . ? C43 N14 Co2 112.74(19) . . ? C45 N15 C56 117.2(3) . . ? C45 N15 Co3 130.1(2) . . ? C56 N15 Co3 112.7(2) . . ? C54 N16 C55 117.7(3) . . ? C54 N16 Co3 129.9(2) . . ? C55 N16 Co3 112.45(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Co1 C1 N1 -141(10) . . . . ? C3 Co1 C1 N1 131(10) . . . . ? C4 Co1 C1 N1 41(12) . . . . ? N9 Co1 C1 N1 -47(10) . . . . ? N10 Co1 C1 N1 37(10) . . . . ? C3 Co1 C2 N2 -142(10) . . . . ? C1 Co1 C2 N2 128(10) . . . . ? C4 Co1 C2 N2 -52(10) . . . . ? N9 Co1 C2 N2 38(10) . . . . ? N10 Co1 C2 N2 11(12) . . . . ? C2 Co1 C3 N3 -129(23) . . . . ? C1 Co1 C3 N3 -38(23) . . . . ? C4 Co1 C3 N3 139(23) . . . . ? N9 Co1 C3 N3 40(25) . . . . ? N10 Co1 C3 N3 52(23) . . . . ? C2 Co1 C4 N4 171(2) . . . . ? C3 Co1 C4 N4 -101(2) . . . . ? C1 Co1 C4 N4 -11(5) . . . . ? N9 Co1 C4 N4 77(2) . . . . ? N10 Co1 C4 N4 -7(2) . . . . ? C7 Co3 C5 N5 -90(6) . . . . ? C6 Co3 C5 N5 0(6) . . . . ? C8 Co3 C5 N5 -27(7) . . . . ? N15 Co3 C5 N5 94(6) . . . . ? N16 Co3 C5 N5 177(100) . . . . ? C7 Co3 C6 N6 178(100) . . . . ? C8 Co3 C6 N6 -95(7) . . . . ? C5 Co3 C6 N6 86(7) . . . . ? N15 Co3 C6 N6 -5(7) . . . . ? N16 Co3 C6 N6 -5(9) . . . . ? C6 Co3 C7 N7 150(4) . . . . ? C8 Co3 C7 N7 59(4) . . . . ? C5 Co3 C7 N7 -123(4) . . . . ? N15 Co3 C7 N7 -4(5) . . . . ? N16 Co3 C7 N7 -30(4) . . . . ? C7 Co3 C8 N8 -56(18) . . . . ? C6 Co3 C8 N8 -147(18) . . . . ? C5 Co3 C8 N8 -119(18) . . . . ? N15 Co3 C8 N8 120(18) . . . . ? N16 Co3 C8 N8 37(18) . . . . ? N9 C9 C10 C11 0.7(5) . . . . ? C9 C10 C11 C12 -1.7(5) . . . . ? C10 C11 C12 C20 0.6(5) . . . . ? C10 C11 C12 C13 -178.9(3) . . . . ? C20 C12 C13 C14 -1.4(5) . . . . ? C11 C12 C13 C14 178.1(3) . . . . ? C12 C13 C14 C15 1.0(5) . . . . ? C13 C14 C15 C19 0.0(5) . . . . ? C13 C14 C15 C16 -179.3(3) . . . . ? C19 C15 C16 C17 0.5(4) . . . . ? C14 C15 C16 C17 179.7(3) . . . . ? C15 C16 C17 C18 0.7(5) . . . . ? C16 C17 C18 N10 -1.4(5) . . . . ? C16 C15 C19 N10 -1.2(4) . . . . ? C14 C15 C19 N10 179.5(3) . . . . ? C16 C15 C19 C20 178.8(3) . . . . ? C14 C15 C19 C20 -0.5(4) . . . . ? C11 C12 C20 N9 1.5(4) . . . . ? C13 C12 C20 N9 -178.9(3) . . . . ? C11 C12 C20 C19 -178.7(3) . . . . ? C13 C12 C20 C19 0.8(4) . . . . ? N10 C19 C20 N9 -0.2(4) . . . . ? C15 C19 C20 N9 179.9(3) . . . . ? N10 C19 C20 C12 -179.9(3) . . . . ? C15 C19 C20 C12 0.1(4) . . . . ? N11 C21 C22 C23 -0.1(5) . . . . ? C21 C22 C23 C24 1.5(5) . . . . ? C22 C23 C24 C32 -1.7(5) . . . . ? C22 C23 C24 C25 177.7(3) . . . . ? C23 C24 C25 C26 -178.1(3) . . . . ? C32 C24 C25 C26 1.3(5) . . . . ? C24 C25 C26 C27 -2.1(5) . . . . ? C25 C26 C27 C28 -178.7(3) . . . . ? C25 C26 C27 C31 0.8(5) . . . . ? C31 C27 C28 C29 -1.3(5) . . . . ? C26 C27 C28 C29 178.1(3) . . . . ? C27 C28 C29 C30 0.6(5) . . . . ? C28 C29 C30 N12 0.4(5) . . . . ? C28 C27 C31 N12 1.3(5) . . . . ? C26 C27 C31 N12 -178.2(3) . . . . ? C28 C27 C31 C32 -179.2(3) . . . . ? C26 C27 C31 C32 1.3(4) . . . . ? C23 C24 C32 N11 0.6(4) . . . . ? C25 C24 C32 N11 -178.9(3) . . . . ? C23 C24 C32 C31 -179.8(3) . . . . ? C25 C24 C32 C31 0.8(4) . . . . ? N12 C31 C32 N11 -2.9(4) . . . . ? C27 C31 C32 N11 177.6(3) . . . . ? N12 C31 C32 C24 177.5(3) . . . . ? C27 C31 C32 C24 -2.0(4) . . . . ? N13 C33 C34 C35 -0.4(5) . . . . ? C33 C34 C35 C36 0.3(5) . . . . ? C34 C35 C36 C44 0.9(5) . . . . ? C34 C35 C36 C37 -178.6(3) . . . . ? C44 C36 C37 C38 0.3(5) . . . . ? C35 C36 C37 C38 179.8(4) . . . . ? C36 C37 C38 C39 1.0(6) . . . . ? C37 C38 C39 C40 179.1(4) . . . . ? C37 C38 C39 C43 -0.8(6) . . . . ? C43 C39 C40 C41 -0.9(5) . . . . ? C38 C39 C40 C41 179.3(4) . . . . ? C39 C40 C41 C42 -0.5(5) . . . . ? C40 C41 C42 N14 2.2(5) . . . . ? C40 C39 C43 N14 0.9(5) . . . . ? C38 C39 C43 N14 -179.3(3) . . . . ? C40 C39 C43 C44 179.4(3) . . . . ? C38 C39 C43 C44 -0.7(5) . . . . ? C35 C36 C44 N13 -2.1(5) . . . . ? C37 C36 C44 N13 177.4(3) . . . . ? C35 C36 C44 C43 178.7(3) . . . . ? C37 C36 C44 C43 -1.8(5) . . . . ? N14 C43 C44 N13 1.4(4) . . . . ? C39 C43 C44 N13 -177.2(3) . . . . ? N14 C43 C44 C36 -179.4(3) . . . . ? C39 C43 C44 C36 2.0(5) . . . . ? N15 C45 C46 C47 0.1(5) . . . . ? C45 C46 C47 C48 0.9(5) . . . . ? C46 C47 C48 C56 -1.2(5) . . . . ? C46 C47 C48 C49 177.9(3) . . . . ? C56 C48 C49 C50 -1.4(6) . . . . ? C47 C48 C49 C50 179.5(4) . . . . ? C48 C49 C50 C51 0.6(6) . . . . ? C49 C50 C51 C55 0.5(5) . . . . ? C49 C50 C51 C52 -179.0(4) . . . . ? C55 C51 C52 C53 1.0(5) . . . . ? C50 C51 C52 C53 -179.6(3) . . . . ? C51 C52 C53 C54 0.6(5) . . . . ? C52 C53 C54 N16 -1.7(5) . . . . ? C52 C51 C55 N16 -1.6(5) . . . . ? C50 C51 C55 N16 178.9(3) . . . . ? C52 C51 C55 C56 178.7(3) . . . . ? C50 C51 C55 C56 -0.8(5) . . . . ? C47 C48 C56 N15 0.6(5) . . . . ? C49 C48 C56 N15 -178.6(3) . . . . ? C47 C48 C56 C55 -179.8(3) . . . . ? C49 C48 C56 C55 1.0(5) . . . . ? N16 C55 C56 N15 0.0(4) . . . . ? C51 C55 C56 N15 179.7(3) . . . . ? N16 C55 C56 C48 -179.7(3) . . . . ? C51 C55 C56 C48 0.0(5) . . . . ? Co1 C4 N4 Co2 52(3) . . . . ? N8 Co2 N4 C4 138.4(13) . . . . ? N13 Co2 N4 C4 42.1(14) . . . . ? N12 Co2 N4 C4 -52.8(14) . . . . ? N11 Co2 N4 C4 -130.0(14) . . . . ? N14 Co2 N4 C4 75.0(15) . . . . ? Co3 C8 N8 Co2 5(19) . . . . ? N4 Co2 N8 C8 130.5(13) . . . . ? N13 Co2 N8 C8 -137.3(13) . . . . ? N12 Co2 N8 C8 33.8(16) . . . . ? N11 Co2 N8 C8 40.5(13) . . . . ? N14 Co2 N8 C8 -60.5(13) . . . . ? C10 C9 N9 C20 1.3(4) . . . . ? C10 C9 N9 Co1 -177.6(2) . . . . ? C12 C20 N9 C9 -2.5(4) . . . . ? C19 C20 N9 C9 177.8(3) . . . . ? C12 C20 N9 Co1 176.7(2) . . . . ? C19 C20 N9 Co1 -3.1(3) . . . . ? C2 Co1 N9 C9 4.1(3) . . . . ? C3 Co1 N9 C9 -165(3) . . . . ? C1 Co1 N9 C9 -86.8(3) . . . . ? C4 Co1 N9 C9 95.9(3) . . . . ? N10 Co1 N9 C9 -177.2(3) . . . . ? C2 Co1 N9 C20 -174.9(2) . . . . ? C3 Co1 N9 C20 16(3) . . . . ? C1 Co1 N9 C20 94.2(2) . . . . ? C4 Co1 N9 C20 -83.1(2) . . . . ? N10 Co1 N9 C20 3.83(19) . . . . ? C17 C18 N10 C19 0.8(5) . . . . ? C17 C18 N10 Co1 177.5(2) . . . . ? C15 C19 N10 C18 0.5(4) . . . . ? C20 C19 N10 C18 -179.4(3) . . . . ? C15 C19 N10 Co1 -176.7(2) . . . . ? C20 C19 N10 Co1 3.4(3) . . . . ? C2 Co1 N10 C18 -154(2) . . . . ? C3 Co1 N10 C18 -0.3(3) . . . . ? C1 Co1 N10 C18 89.9(3) . . . . ? C4 Co1 N10 C18 -89.9(3) . . . . ? N9 Co1 N10 C18 179.2(3) . . . . ? C2 Co1 N10 C19 23(2) . . . . ? C3 Co1 N10 C19 176.6(2) . . . . ? C1 Co1 N10 C19 -93.2(2) . . . . ? C4 Co1 N10 C19 86.9(2) . . . . ? N9 Co1 N10 C19 -3.9(2) . . . . ? C22 C21 N11 C32 -1.0(5) . . . . ? C22 C21 N11 Co2 168.1(2) . . . . ? C24 C32 N11 C21 0.7(4) . . . . ? C31 C32 N11 C21 -178.9(3) . . . . ? C24 C32 N11 Co2 -170.0(2) . . . . ? C31 C32 N11 Co2 10.3(3) . . . . ? N8 Co2 N11 C21 1.7(3) . . . . ? N4 Co2 N11 C21 -89.6(3) . . . . ? N13 Co2 N11 C21 165.5(6) . . . . ? N12 Co2 N11 C21 -179.6(3) . . . . ? N14 Co2 N11 C21 85.2(3) . . . . ? N8 Co2 N11 C32 171.2(2) . . . . ? N4 Co2 N11 C32 79.9(2) . . . . ? N13 Co2 N11 C32 -25.0(8) . . . . ? N12 Co2 N11 C32 -10.2(2) . . . . ? N14 Co2 N11 C32 -105.3(2) . . . . ? C29 C30 N12 C31 -0.5(5) . . . . ? C29 C30 N12 Co2 -173.1(2) . . . . ? C27 C31 N12 C30 -0.4(4) . . . . ? C32 C31 N12 C30 -179.8(3) . . . . ? C27 C31 N12 Co2 173.2(2) . . . . ? C32 C31 N12 Co2 -6.2(3) . . . . ? N8 Co2 N12 C30 -171.6(4) . . . . ? N4 Co2 N12 C30 91.6(3) . . . . ? N13 Co2 N12 C30 -0.5(3) . . . . ? N11 Co2 N12 C30 -178.4(3) . . . . ? N14 Co2 N12 C30 -78.7(3) . . . . ? N8 Co2 N12 C31 15.5(6) . . . . ? N4 Co2 N12 C31 -81.2(2) . . . . ? N13 Co2 N12 C31 -173.4(2) . . . . ? N11 Co2 N12 C31 8.73(19) . . . . ? N14 Co2 N12 C31 108.5(2) . . . . ? C34 C33 N13 C44 -0.8(5) . . . . ? C34 C33 N13 Co2 172.4(2) . . . . ? C36 C44 N13 C33 2.1(4) . . . . ? C43 C44 N13 C33 -178.7(3) . . . . ? C36 C44 N13 Co2 -172.1(2) . . . . ? C43 C44 N13 Co2 7.1(3) . . . . ? N8 Co2 N13 C33 -100.5(3) . . . . ? N4 Co2 N13 C33 -9.0(3) . . . . ? N12 Co2 N13 C33 81.2(3) . . . . ? N11 Co2 N13 C33 95.8(7) . . . . ? N14 Co2 N13 C33 177.8(3) . . . . ? N8 Co2 N13 C44 72.9(2) . . . . ? N4 Co2 N13 C44 164.4(2) . . . . ? N12 Co2 N13 C44 -105.4(2) . . . . ? N11 Co2 N13 C44 -90.8(7) . . . . ? N14 Co2 N13 C44 -8.8(2) . . . . ? C41 C42 N14 C43 -2.2(5) . . . . ? C41 C42 N14 Co2 -169.2(2) . . . . ? C39 C43 N14 C42 0.7(4) . . . . ? C44 C43 N14 C42 -177.9(3) . . . . ? C39 C43 N14 Co2 169.6(2) . . . . ? C44 C43 N14 Co2 -9.0(3) . . . . ? N8 Co2 N14 C42 79.1(3) . . . . ? N4 Co2 N14 C42 143.2(4) . . . . ? N13 Co2 N14 C42 177.0(3) . . . . ? N12 Co2 N14 C42 -89.6(3) . . . . ? N11 Co2 N14 C42 -11.3(3) . . . . ? N8 Co2 N14 C43 -88.4(2) . . . . ? N4 Co2 N14 C43 -24.3(6) . . . . ? N13 Co2 N14 C43 9.5(2) . . . . ? N12 Co2 N14 C43 102.9(2) . . . . ? N11 Co2 N14 C43 -178.7(2) . . . . ? C46 C45 N15 C56 -0.8(4) . . . . ? C46 C45 N15 Co3 -177.5(2) . . . . ? C48 C56 N15 C45 0.4(4) . . . . ? C55 C56 N15 C45 -179.2(3) . . . . ? C48 C56 N15 Co3 177.7(3) . . . . ? C55 C56 N15 Co3 -2.0(3) . . . . ? C7 Co3 N15 C45 152.9(13) . . . . ? C6 Co3 N15 C45 -0.8(3) . . . . ? C8 Co3 N15 C45 89.4(3) . . . . ? C5 Co3 N15 C45 -88.2(3) . . . . ? N16 Co3 N15 C45 179.2(3) . . . . ? C7 Co3 N15 C56 -23.9(14) . . . . ? C6 Co3 N15 C56 -177.6(2) . . . . ? C8 Co3 N15 C56 -87.4(2) . . . . ? C5 Co3 N15 C56 95.0(2) . . . . ? N16 Co3 N15 C56 2.4(2) . . . . ? C53 C54 N16 C55 1.1(5) . . . . ? C53 C54 N16 Co3 179.0(2) . . . . ? C51 C55 N16 C54 0.5(5) . . . . ? C56 C55 N16 C54 -179.7(3) . . . . ? C51 C55 N16 Co3 -177.7(3) . . . . ? C56 C55 N16 Co3 2.0(3) . . . . ? C7 Co3 N16 C54 -2.8(3) . . . . ? C6 Co3 N16 C54 180(100) . . . . ? C8 Co3 N16 C54 -90.0(3) . . . . ? C5 Co3 N16 C54 88.9(3) . . . . ? N15 Co3 N16 C54 179.6(3) . . . . ? C7 Co3 N16 C55 175.2(2) . . . . ? C6 Co3 N16 C55 -2(2) . . . . ? C8 Co3 N16 C55 88.0(2) . . . . ? C5 Co3 N16 C55 -93.1(2) . . . . ? N15 Co3 N16 C55 -2.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.134 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.076 #============================================================================= data_670637 _database_code_depnum_ccdc_archive 'CCDC 670637' #TrackingRef '- CCDC-670637.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H70 Co3 N20 O11' _chemical_formula_weight 1664.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1700(8) _cell_length_b 16.4977(11) _cell_length_c 20.0795(12) _cell_angle_alpha 94.498(1) _cell_angle_beta 93.493(1) _cell_angle_gamma 106.921(1) _cell_volume 3830.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'red orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1718 _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8698 _exptl_absorpt_correction_T_max 0.9317 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20094 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.1356 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13369 _reflns_number_gt 6791 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13369 _refine_ls_number_parameters 1030 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1304 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1588 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.61406(7) 0.82515(5) 0.83901(4) 0.0449(2) Uani 1 1 d . . . Co2 Co 0.76280(6) 0.38248(5) 0.56008(4) 0.0364(2) Uani 1 1 d . . . Co3 Co 0.87498(6) 1.02123(5) 0.30043(4) 0.0364(2) Uani 1 1 d . . . C1 C 0.7768(5) 0.3655(4) 0.6522(3) 0.0440(16) Uani 1 1 d . . . C2 C 0.6966(5) 0.2652(4) 0.5427(3) 0.0432(16) Uani 1 1 d . . . C3 C 0.9095(6) 0.3701(4) 0.5533(3) 0.0442(16) Uani 1 1 d . . . C4 C 0.7538(5) 0.3940(3) 0.4666(3) 0.0381(15) Uani 1 1 d . . . C5 C 0.8508(4) 1.1280(4) 0.2961(3) 0.0355(14) Uani 1 1 d . . . C6 C 1.0390(6) 1.0748(4) 0.3181(3) 0.0410(16) Uani 1 1 d . . . C7 C 0.8991(5) 1.0156(3) 0.2099(3) 0.0396(15) Uani 1 1 d . . . C8 C 0.7133(6) 0.9715(3) 0.2775(3) 0.0413(15) Uani 1 1 d . . . C9 C 0.7515(5) 0.8171(3) 0.9735(3) 0.0460(16) Uani 1 1 d . . . H9 H 0.8027 0.7988 0.9481 0.055 Uiso 1 1 calc R . . C10 C 0.7750(5) 0.8303(4) 1.0428(3) 0.0490(16) Uani 1 1 d . . . H10 H 0.8415 0.8220 1.0625 0.059 Uiso 1 1 calc R . . C11 C 0.7007(5) 0.8551(4) 1.0815(3) 0.0465(16) Uani 1 1 d . . . H11 H 0.7158 0.8638 1.1279 0.056 Uiso 1 1 calc R . . C12 C 0.6018(5) 0.8674(3) 1.0513(3) 0.0370(14) Uani 1 1 d . . . C13 C 0.5174(5) 0.8917(3) 1.0877(3) 0.0481(16) Uani 1 1 d . . . H13 H 0.5271 0.8997 1.1343 0.058 Uiso 1 1 calc R . . C14 C 0.4234(5) 0.9030(4) 1.0550(3) 0.0534(18) Uani 1 1 d . . . H14 H 0.3691 0.9179 1.0799 0.064 Uiso 1 1 calc R . . C15 C 0.4044(5) 0.8929(3) 0.9839(3) 0.0452(16) Uani 1 1 d . . . C16 C 0.3110(5) 0.9057(4) 0.9469(4) 0.0575(18) Uani 1 1 d . . . H16 H 0.2534 0.9203 0.9690 0.069 Uiso 1 1 calc R . . C17 C 0.3040(5) 0.8968(4) 0.8792(4) 0.0572(18) Uani 1 1 d . . . H17 H 0.2412 0.9049 0.8549 0.069 Uiso 1 1 calc R . . C18 C 0.3901(5) 0.8756(4) 0.8456(3) 0.0550(18) Uani 1 1 d . . . H18 H 0.3846 0.8712 0.7989 0.066 Uiso 1 1 calc R . . C19 C 0.4875(5) 0.8704(3) 0.9464(3) 0.0367(14) Uani 1 1 d . . . C20 C 0.5850(4) 0.8554(3) 0.9808(3) 0.0340(14) Uani 1 1 d . . . C21 C 0.7914(5) 1.0005(4) 0.8790(3) 0.0485(17) Uani 1 1 d . . . H21 H 0.8102 0.9785 0.9179 0.058 Uiso 1 1 calc R . . C22 C 0.8478(5) 1.0853(4) 0.8719(3) 0.0554(18) Uani 1 1 d . . . H22 H 0.9023 1.1188 0.9051 0.066 Uiso 1 1 calc R . . C23 C 0.8210(5) 1.1183(4) 0.8146(4) 0.0600(19) Uani 1 1 d . . . H23 H 0.8561 1.1752 0.8091 0.072 Uiso 1 1 calc R . . C24 C 0.7395(5) 1.0654(4) 0.7638(3) 0.0508(17) Uani 1 1 d . . . C25 C 0.7094(6) 1.0928(4) 0.7012(4) 0.0624(19) Uani 1 1 d . . . H25 H 0.7425 1.1489 0.6925 0.075 Uiso 1 1 calc R . . C26 C 0.6335(6) 1.0384(5) 0.6547(3) 0.0599(19) Uani 1 1 d . . . H26 H 0.6146 1.0572 0.6144 0.072 Uiso 1 1 calc R . . C27 C 0.5825(5) 0.9532(4) 0.6665(3) 0.0504(17) Uani 1 1 d . . . C28 C 0.5007(6) 0.8954(5) 0.6194(3) 0.0626(19) Uani 1 1 d . . . H28 H 0.4793 0.9122 0.5787 0.075 Uiso 1 1 calc R . . C29 C 0.4542(6) 0.8150(5) 0.6347(3) 0.067(2) Uani 1 1 d . . . H29 H 0.4010 0.7755 0.6041 0.081 Uiso 1 1 calc R . . C30 C 0.4861(6) 0.7910(4) 0.6971(3) 0.0597(19) Uani 1 1 d . . . H30 H 0.4518 0.7356 0.7069 0.072 Uiso 1 1 calc R . . C31 C 0.6086(5) 0.9243(4) 0.7267(3) 0.0440(16) Uani 1 1 d . . . C32 C 0.6899(5) 0.9817(4) 0.7760(3) 0.0431(16) Uani 1 1 d . . . C33 C 0.8520(7) 0.8114(4) 0.8143(3) 0.0610(19) Uani 1 1 d . . . H33 H 0.8783 0.8704 0.8225 0.073 Uiso 1 1 calc R . . C34 C 0.9336(7) 0.7667(5) 0.8017(4) 0.082(2) Uani 1 1 d . . . H34 H 1.0119 0.7954 0.8035 0.098 Uiso 1 1 calc R . . C35 C 0.8936(9) 0.6802(5) 0.7868(4) 0.086(3) Uani 1 1 d . . . H35 H 0.9453 0.6497 0.7779 0.104 Uiso 1 1 calc R . . C36 C 0.7768(9) 0.6375(5) 0.7850(3) 0.077(2) Uani 1 1 d . . . C37 C 0.7219(9) 0.5447(5) 0.7687(4) 0.085(3) Uani 1 1 d . . . H37 H 0.7679 0.5104 0.7575 0.102 Uiso 1 1 calc R . . C38 C 0.6117(10) 0.5098(6) 0.7694(4) 0.101(3) Uani 1 1 d . . . H38 H 0.5812 0.4516 0.7574 0.121 Uiso 1 1 calc R . . C39 C 0.5369(9) 0.5569(5) 0.7876(4) 0.083(3) Uani 1 1 d . . . C40 C 0.4192(10) 0.5226(6) 0.7928(5) 0.120(4) Uani 1 1 d . . . H40 H 0.3831 0.4650 0.7803 0.144 Uiso 1 1 calc R . . C41 C 0.3567(8) 0.5743(6) 0.8166(6) 0.129(4) Uani 1 1 d . . . H41 H 0.2792 0.5507 0.8228 0.154 Uiso 1 1 calc R . . C42 C 0.4072(7) 0.6601(5) 0.8311(4) 0.095(3) Uani 1 1 d . . . H42 H 0.3622 0.6939 0.8453 0.114 Uiso 1 1 calc R . . C43 C 0.5838(8) 0.6459(5) 0.8046(3) 0.067(2) Uani 1 1 d . . . C44 C 0.7020(7) 0.6866(4) 0.8012(3) 0.058(2) Uani 1 1 d . . . C45 C 0.5078(5) 0.3506(4) 0.5616(3) 0.0456(16) Uani 1 1 d . . . H45 H 0.4988 0.2930 0.5509 0.055 Uiso 1 1 calc R . . C46 C 0.4099(5) 0.3767(4) 0.5696(3) 0.0563(18) Uani 1 1 d . . . H46 H 0.3369 0.3374 0.5639 0.068 Uiso 1 1 calc R . . C47 C 0.4231(5) 0.4611(4) 0.5859(3) 0.0518(18) Uani 1 1 d . . . H47 H 0.3585 0.4792 0.5918 0.062 Uiso 1 1 calc R . . C48 C 0.5317(5) 0.5200(4) 0.5937(3) 0.0418(15) Uani 1 1 d . . . C49 C 0.5546(6) 0.6090(4) 0.6109(3) 0.0500(17) Uani 1 1 d . . . H49 H 0.4932 0.6309 0.6165 0.060 Uiso 1 1 calc R . . C50 C 0.6624(6) 0.6621(4) 0.6193(3) 0.0492(17) Uani 1 1 d . . . H50 H 0.6745 0.7197 0.6318 0.059 Uiso 1 1 calc R . . C51 C 0.7597(5) 0.6308(3) 0.6093(3) 0.0375(14) Uani 1 1 d . . . C52 C 0.8737(6) 0.6816(4) 0.6188(3) 0.0499(17) Uani 1 1 d . . . H52 H 0.8916 0.7395 0.6321 0.060 Uiso 1 1 calc R . . C53 C 0.9589(6) 0.6449(4) 0.6083(3) 0.0540(18) Uani 1 1 d . . . H53 H 1.0358 0.6779 0.6135 0.065 Uiso 1 1 calc R . . C54 C 0.9301(5) 0.5574(4) 0.5897(3) 0.0432(15) Uani 1 1 d . . . H54 H 0.9892 0.5334 0.5825 0.052 Uiso 1 1 calc R . . C55 C 0.7374(5) 0.5438(3) 0.5920(3) 0.0335(14) Uani 1 1 d . . . C56 C 0.6234(5) 0.4879(3) 0.5841(3) 0.0353(14) Uani 1 1 d . . . C57 C 0.9237(5) 0.8566(4) 0.2657(3) 0.0605(19) Uani 1 1 d . . . H57 H 0.9268 0.8692 0.2214 0.073 Uiso 1 1 calc R . . C58 C 0.9450(6) 0.7826(4) 0.2820(3) 0.075(2) Uani 1 1 d . . . H58 H 0.9639 0.7470 0.2493 0.090 Uiso 1 1 calc R . . C59 C 0.9381(7) 0.7619(4) 0.3466(3) 0.081(3) Uani 1 1 d . . . H59 H 0.9535 0.7125 0.3580 0.098 Uiso 1 1 calc R . . C60 C 0.9079(5) 0.8150(4) 0.3957(3) 0.0497(17) Uani 1 1 d . . . C61 C 0.8937(5) 0.7990(4) 0.4641(3) 0.0550(18) Uani 1 1 d . . . H61 H 0.9047 0.7495 0.4785 0.066 Uiso 1 1 calc R . . C62 C 0.8652(5) 0.8531(3) 0.5079(3) 0.0474(16) Uani 1 1 d . . . H62 H 0.8550 0.8403 0.5519 0.057 Uiso 1 1 calc R . . C63 C 0.8502(4) 0.9305(3) 0.4876(3) 0.0374(14) Uani 1 1 d . . . C64 C 0.8233(5) 0.9920(4) 0.5306(3) 0.0475(16) Uani 1 1 d . . . H64 H 0.8133 0.9837 0.5754 0.057 Uiso 1 1 calc R . . C65 C 0.8121(5) 1.0636(4) 0.5058(3) 0.0514(17) Uani 1 1 d . . . H65 H 0.7958 1.1051 0.5342 0.062 Uiso 1 1 calc R . . C66 C 0.8245(5) 1.0763(4) 0.4386(3) 0.0456(16) Uani 1 1 d . . . H66 H 0.8136 1.1251 0.4227 0.055 Uiso 1 1 calc R . . C67 C 0.8640(4) 0.9481(3) 0.4213(3) 0.0339(14) Uani 1 1 d . . . C68 C 0.8910(5) 0.8889(3) 0.3751(3) 0.0366(14) Uani 1 1 d . . . C69 C 0.7455(7) 0.5925(4) 0.0231(5) 0.085(3) Uani 1 1 d . . . H69 H 0.8162 0.5819 0.0210 0.102 Uiso 1 1 calc R . . C70 C 0.6709(9) 0.5743(4) -0.0343(4) 0.086(3) Uani 1 1 d . . . H70 H 0.6906 0.5505 -0.0737 0.103 Uiso 1 1 calc R . . C71 C 0.5679(8) 0.5915(5) -0.0327(4) 0.082(2) Uani 1 1 d . . . H71 H 0.5189 0.5812 -0.0719 0.099 Uiso 1 1 calc R . . C72 C 0.5338(9) 0.6248(4) 0.0271(5) 0.079(2) Uani 1 1 d . . . C73 C 0.4286(8) 0.6425(5) 0.0319(6) 0.103(3) Uani 1 1 d . . . H73 H 0.3766 0.6332 -0.0058 0.124 Uiso 1 1 calc R . . C74 C 0.4033(9) 0.6725(5) 0.0900(7) 0.113(4) Uani 1 1 d . . . H74 H 0.3320 0.6822 0.0922 0.136 Uiso 1 1 calc R . . C75 C 0.4788(12) 0.6904(5) 0.1488(6) 0.110(4) Uani 1 1 d . . . C76 C 0.4495(12) 0.7217(6) 0.2089(7) 0.131(5) Uani 1 1 d . . . H76 H 0.3791 0.7327 0.2114 0.157 Uiso 1 1 calc R . . C77 C 0.5235(15) 0.7357(7) 0.2628(8) 0.171(9) Uani 1 1 d . . . H77 H 0.5043 0.7547 0.3041 0.205 Uiso 1 1 calc R . . C78 C 0.6282(12) 0.7221(6) 0.2570(6) 0.137(5) Uani 1 1 d . . . H78 H 0.6805 0.7355 0.2949 0.164 Uiso 1 1 calc R . . C79 C 0.5843(10) 0.6743(5) 0.1460(5) 0.085(3) Uani 1 1 d . . . C80 C 0.6150(9) 0.6414(4) 0.0840(5) 0.082(3) Uani 1 1 d . . . N1 N 0.7890(5) 0.3547(3) 0.7079(3) 0.0656(16) Uani 1 1 d . . . N2 N 0.6492(5) 0.1925(3) 0.5333(3) 0.0571(15) Uani 1 1 d . . . N3 N 1.0019(5) 0.3689(3) 0.5503(3) 0.0593(16) Uani 1 1 d . . . N4 N 0.7497(4) 0.3999(3) 0.4096(3) 0.0456(13) Uani 1 1 d . . . N5 N 0.8330(4) 1.1921(3) 0.2928(2) 0.0479(14) Uani 1 1 d . . . N6 N 1.1360(4) 1.1067(3) 0.3273(2) 0.0480(14) Uani 1 1 d . . . N7 N 0.9164(4) 1.0124(3) 0.1544(3) 0.0510(14) Uani 1 1 d . . . N8 N 0.6156(5) 0.9431(3) 0.2637(3) 0.0641(17) Uani 1 1 d . . . N9 N 0.6591(4) 0.8295(3) 0.9415(2) 0.0377(12) Uani 1 1 d . . . N10 N 0.4797(4) 0.8613(3) 0.8782(2) 0.0408(12) Uani 1 1 d . . . N11 N 0.7130(4) 0.9492(3) 0.8342(2) 0.0439(13) Uani 1 1 d . . . N12 N 0.5632(4) 0.8441(3) 0.7427(2) 0.0460(13) Uani 1 1 d . . . N13 N 0.7417(5) 0.7733(3) 0.8150(2) 0.0489(14) Uani 1 1 d . . . N14 N 0.5199(6) 0.6970(3) 0.8254(3) 0.0654(17) Uani 1 1 d . . . N15 N 0.6131(4) 0.4047(3) 0.5685(2) 0.0358(12) Uani 1 1 d . . . N16 N 0.8229(4) 0.5073(3) 0.5819(2) 0.0359(11) Uani 1 1 d . . . N17 N 0.8990(4) 0.9104(3) 0.3107(2) 0.0387(12) Uani 1 1 d . . . N18 N 0.8516(4) 1.0199(3) 0.3964(2) 0.0355(11) Uani 1 1 d . . . N19 N 0.7215(6) 0.6248(4) 0.0819(3) 0.085(2) Uani 1 1 d . . . N20 N 0.6603(7) 0.6907(4) 0.2008(4) 0.109(3) Uani 1 1 d . . . O1W O 0.9533(4) 0.0623(4) 0.0255(2) 0.0687(14) Uani 1 1 d D . . O2W O 0.8046(5) 0.3490(3) 0.2732(3) 0.118(2) Uani 1 1 d . . . O3W O 0.9516(5) 0.7220(4) 0.1174(3) 0.129(2) Uani 1 1 d . . . O4W O 0.9186(5) 0.3740(4) 0.8295(3) 0.123(2) Uani 1 1 d . . . O5W O 0.4163(5) 0.1267(4) 0.5912(3) 0.145(2) Uani 1 1 d . . . O6W O 0.0043(4) 0.7621(3) 0.9848(3) 0.0957(17) Uani 1 1 d . . . O7W O 0.8859(6) 0.4563(6) 0.9484(4) 0.208(4) Uani 1 1 d . . . O8W O 0.1690(8) 0.4567(7) 0.6614(5) 0.301(6) Uani 1 1 d . . . O9W O 0.1289(7) 0.4112(5) 0.7913(5) 0.214(4) Uani 1 1 d . . . O10W O 0.0823(7) 0.5648(5) 0.8205(4) 0.186(3) Uani 1 1 d . . . O11W O 0.0728(10) 0.6269(8) 0.9407(6) 0.312(6) Uiso 1 1 d . . . H1B H 0.945(4) 0.045(3) 0.064(2) 0.040(18) Uiso 1 1 d D . . H1A H 0.980(14) 0.125(3) 0.024(9) 0.45(12) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0588(6) 0.0426(5) 0.0360(5) -0.0039(4) -0.0013(4) 0.0226(4) Co2 0.0449(5) 0.0378(5) 0.0333(5) 0.0016(4) 0.0039(4) 0.0231(4) Co3 0.0462(5) 0.0408(5) 0.0278(5) 0.0006(3) 0.0036(4) 0.0225(4) C1 0.051(4) 0.044(4) 0.042(4) 0.006(3) 0.004(3) 0.021(3) C2 0.056(4) 0.052(4) 0.035(4) 0.010(3) 0.010(3) 0.035(4) C3 0.064(4) 0.046(4) 0.036(4) 0.011(3) 0.007(3) 0.035(4) C4 0.042(4) 0.029(3) 0.049(4) 0.001(3) 0.000(3) 0.021(3) C5 0.041(4) 0.050(4) 0.021(3) 0.001(3) 0.003(3) 0.020(3) C6 0.069(5) 0.045(4) 0.017(3) -0.001(3) 0.000(3) 0.031(4) C7 0.047(4) 0.038(4) 0.039(4) 0.008(3) -0.001(3) 0.021(3) C8 0.059(4) 0.036(4) 0.031(4) 0.002(3) 0.005(3) 0.018(3) C9 0.047(4) 0.048(4) 0.055(5) 0.014(3) 0.010(3) 0.028(3) C10 0.049(4) 0.059(4) 0.041(4) 0.014(3) -0.007(3) 0.020(3) C11 0.051(4) 0.053(4) 0.032(4) 0.002(3) -0.001(3) 0.013(3) C12 0.046(4) 0.034(3) 0.029(3) 0.001(3) 0.003(3) 0.009(3) C13 0.067(5) 0.046(4) 0.033(4) -0.003(3) 0.014(3) 0.019(3) C14 0.062(5) 0.059(4) 0.050(5) 0.001(3) 0.022(4) 0.032(4) C15 0.042(4) 0.045(4) 0.053(4) 0.002(3) 0.008(3) 0.019(3) C16 0.053(4) 0.064(5) 0.066(5) 0.005(4) 0.011(4) 0.032(4) C17 0.047(4) 0.070(5) 0.061(5) 0.007(4) -0.005(4) 0.029(4) C18 0.053(4) 0.065(4) 0.050(4) -0.003(3) -0.008(4) 0.027(4) C19 0.039(4) 0.035(3) 0.035(4) 0.000(3) -0.004(3) 0.012(3) C20 0.034(3) 0.029(3) 0.040(4) 0.002(3) 0.004(3) 0.010(3) C21 0.057(4) 0.053(4) 0.044(4) -0.004(3) 0.007(3) 0.032(4) C22 0.058(4) 0.060(5) 0.049(5) -0.009(4) 0.005(4) 0.023(4) C23 0.066(5) 0.049(4) 0.069(5) -0.005(4) 0.015(4) 0.025(4) C24 0.056(4) 0.056(4) 0.047(4) -0.002(4) 0.012(4) 0.027(4) C25 0.068(5) 0.060(5) 0.067(6) 0.015(4) 0.017(4) 0.028(4) C26 0.063(5) 0.081(6) 0.047(5) 0.010(4) 0.010(4) 0.037(4) C27 0.053(4) 0.062(5) 0.043(4) -0.003(4) 0.005(4) 0.030(4) C28 0.077(5) 0.080(5) 0.041(4) 0.009(4) 0.011(4) 0.038(5) C29 0.085(6) 0.078(6) 0.043(5) -0.017(4) -0.006(4) 0.038(5) C30 0.078(5) 0.061(5) 0.049(5) -0.012(4) 0.001(4) 0.041(4) C31 0.054(4) 0.053(4) 0.034(4) -0.005(3) 0.004(3) 0.032(4) C32 0.054(4) 0.043(4) 0.043(4) 0.003(3) 0.015(3) 0.029(3) C33 0.095(6) 0.060(5) 0.046(4) 0.007(3) 0.034(4) 0.045(5) C34 0.106(6) 0.099(6) 0.068(6) 0.024(5) 0.053(5) 0.062(6) C35 0.153(9) 0.079(6) 0.065(6) 0.018(4) 0.059(6) 0.080(7) C36 0.145(8) 0.080(6) 0.027(4) 0.011(4) 0.021(5) 0.061(6) C37 0.182(10) 0.055(6) 0.041(5) 0.003(4) 0.018(6) 0.068(6) C38 0.175(10) 0.062(6) 0.061(6) -0.009(5) -0.020(7) 0.036(8) C39 0.134(8) 0.046(5) 0.058(5) -0.003(4) -0.043(6) 0.020(6) C40 0.137(10) 0.057(6) 0.133(9) 0.006(6) -0.085(8) 0.000(7) C41 0.091(7) 0.072(7) 0.198(12) 0.047(7) -0.065(8) -0.008(6) C42 0.058(6) 0.069(6) 0.141(9) 0.029(5) -0.037(6) -0.004(5) C43 0.097(6) 0.056(5) 0.040(4) 0.002(4) -0.025(4) 0.019(5) C44 0.112(6) 0.053(5) 0.021(4) -0.003(3) 0.004(4) 0.045(5) C45 0.048(4) 0.041(4) 0.052(4) 0.001(3) 0.005(3) 0.019(3) C46 0.044(4) 0.061(5) 0.066(5) 0.003(4) 0.003(3) 0.019(4) C47 0.052(4) 0.068(5) 0.050(4) 0.001(3) 0.011(3) 0.042(4) C48 0.046(4) 0.050(4) 0.039(4) 0.004(3) 0.004(3) 0.029(3) C49 0.069(5) 0.047(4) 0.048(4) 0.000(3) 0.004(4) 0.042(4) C50 0.078(5) 0.039(4) 0.038(4) -0.006(3) 0.001(4) 0.033(4) C51 0.054(4) 0.034(3) 0.027(3) 0.003(3) 0.000(3) 0.017(3) C52 0.076(5) 0.036(4) 0.038(4) -0.002(3) -0.007(4) 0.020(4) C53 0.060(4) 0.044(4) 0.047(4) -0.001(3) -0.006(4) 0.002(4) C54 0.044(4) 0.047(4) 0.039(4) 0.001(3) 0.002(3) 0.016(3) C55 0.048(4) 0.038(3) 0.022(3) 0.004(3) 0.000(3) 0.026(3) C56 0.043(4) 0.041(4) 0.029(3) 0.003(3) 0.003(3) 0.023(3) C57 0.098(5) 0.068(5) 0.034(4) -0.002(3) 0.007(4) 0.056(4) C58 0.143(7) 0.071(5) 0.038(4) -0.010(4) 0.000(5) 0.079(5) C59 0.161(8) 0.060(5) 0.049(5) -0.002(4) -0.008(5) 0.078(5) C60 0.079(5) 0.041(4) 0.037(4) -0.004(3) -0.009(4) 0.033(4) C61 0.088(5) 0.042(4) 0.043(4) 0.005(3) -0.005(4) 0.033(4) C62 0.069(4) 0.046(4) 0.031(4) 0.003(3) 0.002(3) 0.024(3) C63 0.041(4) 0.042(4) 0.031(4) -0.001(3) 0.003(3) 0.018(3) C64 0.064(4) 0.062(4) 0.027(4) 0.005(3) 0.012(3) 0.034(4) C65 0.074(5) 0.063(4) 0.032(4) -0.001(3) 0.012(3) 0.042(4) C66 0.061(4) 0.048(4) 0.039(4) 0.002(3) 0.006(3) 0.035(3) C67 0.037(3) 0.038(3) 0.029(3) -0.007(3) -0.002(3) 0.017(3) C68 0.047(4) 0.039(3) 0.026(3) 0.002(3) -0.001(3) 0.018(3) C69 0.110(7) 0.051(5) 0.091(7) -0.008(5) 0.020(6) 0.020(5) C70 0.124(8) 0.054(5) 0.067(6) 0.003(4) 0.024(6) 0.005(5) C71 0.095(7) 0.061(5) 0.083(7) 0.025(5) 0.006(6) 0.006(5) C72 0.114(8) 0.042(5) 0.071(6) 0.008(4) 0.026(6) 0.006(5) C73 0.096(8) 0.067(6) 0.145(11) 0.020(6) 0.029(7) 0.015(5) C74 0.134(10) 0.054(6) 0.153(11) 0.011(6) 0.070(9) 0.018(6) C75 0.158(12) 0.049(6) 0.106(10) 0.010(6) 0.059(9) -0.006(7) C76 0.201(14) 0.060(7) 0.129(11) 0.007(7) 0.088(11) 0.019(7) C77 0.26(2) 0.064(7) 0.143(13) -0.008(8) 0.143(15) -0.035(10) C78 0.189(13) 0.083(8) 0.078(8) -0.006(6) 0.045(8) -0.057(8) C79 0.118(8) 0.048(5) 0.068(7) 0.001(4) 0.030(7) -0.011(5) C80 0.121(8) 0.032(4) 0.078(7) 0.005(4) 0.027(7) -0.004(5) N1 0.078(4) 0.079(4) 0.044(4) 0.006(3) 0.008(3) 0.030(3) N2 0.078(4) 0.046(3) 0.057(4) 0.005(3) 0.003(3) 0.035(3) N3 0.067(4) 0.075(4) 0.058(4) 0.024(3) 0.011(3) 0.050(3) N4 0.056(3) 0.053(3) 0.036(3) 0.004(3) 0.003(3) 0.029(3) N5 0.059(3) 0.050(3) 0.045(3) 0.006(3) 0.002(3) 0.033(3) N6 0.045(3) 0.059(4) 0.043(3) 0.002(3) 0.002(3) 0.021(3) N7 0.066(4) 0.064(4) 0.030(3) 0.004(3) 0.007(3) 0.030(3) N8 0.052(4) 0.071(4) 0.064(4) -0.004(3) 0.001(3) 0.013(3) N9 0.043(3) 0.040(3) 0.037(3) 0.004(2) 0.006(2) 0.022(2) N10 0.040(3) 0.046(3) 0.038(3) -0.001(2) -0.003(2) 0.019(2) N11 0.053(3) 0.046(3) 0.037(3) -0.014(3) -0.001(3) 0.028(3) N12 0.058(3) 0.045(3) 0.036(3) -0.012(3) -0.005(3) 0.022(3) N13 0.071(4) 0.047(3) 0.032(3) 0.002(2) 0.014(3) 0.022(3) N14 0.083(5) 0.052(4) 0.060(4) 0.010(3) -0.014(4) 0.022(4) N15 0.038(3) 0.039(3) 0.034(3) 0.001(2) 0.004(2) 0.019(3) N16 0.043(3) 0.041(3) 0.027(3) 0.002(2) -0.001(2) 0.019(3) N17 0.053(3) 0.042(3) 0.028(3) -0.002(2) 0.005(2) 0.027(2) N18 0.045(3) 0.036(3) 0.031(3) 0.002(2) 0.002(2) 0.021(2) N19 0.111(6) 0.052(4) 0.079(5) -0.002(3) 0.011(5) 0.008(4) N20 0.158(8) 0.062(5) 0.075(6) -0.005(4) 0.033(6) -0.022(5) O1W 0.086(4) 0.101(4) 0.037(3) 0.018(3) 0.017(3) 0.050(3) O2W 0.172(6) 0.100(4) 0.094(5) 0.020(3) -0.030(4) 0.066(4) O3W 0.163(6) 0.116(5) 0.109(5) -0.022(4) -0.035(4) 0.062(4) O4W 0.131(5) 0.188(6) 0.075(4) 0.016(4) -0.013(4) 0.089(5) O5W 0.124(5) 0.165(6) 0.148(7) 0.027(5) 0.012(5) 0.044(5) O6W 0.090(4) 0.086(4) 0.113(5) -0.004(3) 0.005(3) 0.034(3) O7W 0.167(7) 0.275(10) 0.194(9) -0.062(7) 0.025(6) 0.102(7) O8W 0.211(10) 0.342(14) 0.260(13) 0.142(10) -0.054(8) -0.070(9) O9W 0.200(8) 0.181(8) 0.239(11) -0.026(7) -0.008(7) 0.039(6) O10W 0.237(8) 0.182(7) 0.184(8) 0.037(6) 0.084(7) 0.116(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N13 2.044(5) . ? Co1 N11 2.063(5) . ? Co1 N12 2.070(5) . ? Co1 N10 2.074(4) . ? Co1 N14 2.078(6) . ? Co1 N9 2.088(4) . ? Co2 C2 1.862(6) . ? Co2 C3 1.867(6) . ? Co2 C1 1.896(7) . ? Co2 C4 1.902(6) . ? Co2 N15 1.974(4) . ? Co2 N16 1.977(4) . ? Co3 C7 1.859(6) . ? Co3 C5 1.877(6) . ? Co3 C8 1.910(7) . ? Co3 C6 1.931(7) . ? Co3 N17 1.958(4) . ? Co3 N18 1.966(4) . ? C1 N1 1.155(7) . ? C2 N2 1.164(6) . ? C3 N3 1.136(6) . ? C4 N4 1.154(6) . ? C5 N5 1.145(6) . ? C6 N6 1.141(6) . ? C7 N7 1.145(7) . ? C8 N8 1.151(6) . ? C9 N9 1.336(6) . ? C9 C10 1.390(7) . ? C10 C11 1.357(7) . ? C11 C12 1.390(7) . ? C12 C20 1.407(7) . ? C12 C13 1.426(7) . ? C13 C14 1.352(7) . ? C14 C15 1.419(8) . ? C15 C16 1.396(7) . ? C15 C19 1.414(7) . ? C16 C17 1.351(8) . ? C17 C18 1.393(8) . ? C18 N10 1.328(6) . ? C19 N10 1.359(6) . ? C19 C20 1.429(7) . ? C20 N9 1.370(6) . ? C21 N11 1.320(7) . ? C21 C22 1.390(8) . ? C22 C23 1.372(8) . ? C23 C24 1.422(8) . ? C24 C32 1.384(8) . ? C24 C25 1.431(8) . ? C25 C26 1.346(8) . ? C26 C27 1.406(8) . ? C27 C31 1.387(8) . ? C27 C28 1.409(8) . ? C28 C29 1.349(8) . ? C29 C30 1.408(8) . ? C30 N12 1.333(7) . ? C31 N12 1.350(7) . ? C31 C32 1.429(8) . ? C32 N11 1.371(7) . ? C33 N13 1.308(7) . ? C33 C34 1.422(8) . ? C34 C35 1.369(10) . ? C35 C36 1.388(10) . ? C36 C44 1.420(9) . ? C36 C37 1.481(10) . ? C37 C38 1.297(11) . ? C38 C39 1.404(11) . ? C39 C40 1.392(12) . ? C39 C43 1.417(9) . ? C40 C41 1.376(13) . ? C41 C42 1.369(10) . ? C42 N14 1.346(8) . ? C43 N14 1.362(8) . ? C43 C44 1.408(9) . ? C44 N13 1.369(7) . ? C45 N15 1.323(6) . ? C45 C46 1.394(7) . ? C46 C47 1.364(7) . ? C47 C48 1.385(8) . ? C48 C56 1.386(7) . ? C48 C49 1.421(7) . ? C49 C50 1.341(8) . ? C50 C51 1.441(7) . ? C51 C52 1.389(7) . ? C51 C55 1.393(7) . ? C52 C53 1.364(8) . ? C53 C54 1.396(7) . ? C54 N16 1.317(6) . ? C55 N16 1.363(6) . ? C55 C56 1.417(7) . ? C56 N15 1.351(6) . ? C57 N17 1.326(6) . ? C57 C58 1.378(7) . ? C58 C59 1.369(8) . ? C59 C60 1.402(8) . ? C60 C68 1.384(7) . ? C60 C61 1.431(8) . ? C61 C62 1.337(7) . ? C62 C63 1.428(7) . ? C63 C67 1.395(7) . ? C63 C64 1.403(7) . ? C64 C65 1.358(7) . ? C65 C66 1.392(7) . ? C66 N18 1.335(6) . ? C67 N18 1.364(6) . ? C67 C68 1.416(7) . ? C68 N17 1.369(6) . ? C69 N19 1.340(9) . ? C69 C70 1.380(10) . ? C70 C71 1.366(10) . ? C71 C72 1.415(10) . ? C72 C73 1.401(11) . ? C72 C80 1.419(10) . ? C73 C74 1.321(12) . ? C74 C75 1.407(13) . ? C75 C76 1.383(13) . ? C75 C79 1.387(12) . ? C76 C77 1.325(17) . ? C77 C78 1.367(17) . ? C78 N20 1.333(12) . ? C79 N20 1.350(10) . ? C79 C80 1.433(11) . ? C80 N19 1.402(10) . ? 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 N13 Co1 N11 94.7(2) . . ? N13 Co1 N12 97.39(18) . . ? N11 Co1 N12 79.3(2) . . ? N13 Co1 N10 168.5(2) . . ? N11 Co1 N10 93.32(17) . . ? N12 Co1 N10 92.14(18) . . ? N13 Co1 N14 80.2(2) . . ? N11 Co1 N14 169.5(2) . . ? N12 Co1 N14 92.1(2) . . ? N10 Co1 N14 93.2(2) . . ? N13 Co1 N9 91.85(18) . . ? N11 Co1 N9 92.93(18) . . ? N12 Co1 N9 168.37(17) . . ? N10 Co1 N9 79.54(18) . . ? N14 Co1 N9 96.41(19) . . ? C2 Co2 C3 90.5(2) . . ? C2 Co2 C1 87.5(2) . . ? C3 Co2 C1 88.5(2) . . ? C2 Co2 C4 90.2(2) . . ? C3 Co2 C4 88.6(2) . . ? C1 Co2 C4 176.3(2) . . ? C2 Co2 N15 93.7(2) . . ? C3 Co2 N15 175.8(2) . . ? C1 Co2 N15 91.7(2) . . ? C4 Co2 N15 91.4(2) . . ? C2 Co2 N16 175.8(2) . . ? C3 Co2 N16 93.3(2) . . ? C1 Co2 N16 91.0(2) . . ? C4 Co2 N16 91.5(2) . . ? N15 Co2 N16 82.49(18) . . ? C7 Co3 C5 90.5(2) . . ? C7 Co3 C8 89.6(2) . . ? C5 Co3 C8 87.5(2) . . ? C7 Co3 C6 87.1(2) . . ? C5 Co3 C6 90.6(2) . . ? C8 Co3 C6 176.2(3) . . ? C7 Co3 N17 92.9(2) . . ? C5 Co3 N17 176.6(2) . . ? C8 Co3 N17 92.6(2) . . ? C6 Co3 N17 89.5(2) . . ? C7 Co3 N18 176.2(2) . . ? C5 Co3 N18 93.3(2) . . ? C8 Co3 N18 90.7(2) . . ? C6 Co3 N18 92.7(2) . . ? N17 Co3 N18 83.26(18) . . ? N1 C1 Co2 177.6(6) . . ? N2 C2 Co2 175.9(5) . . ? N3 C3 Co2 174.9(6) . . ? N4 C4 Co2 178.6(5) . . ? N5 C5 Co3 178.2(5) . . ? N6 C6 Co3 178.8(6) . . ? N7 C7 Co3 178.6(5) . . ? N8 C8 Co3 178.7(5) . . ? N9 C9 C10 123.3(6) . . ? C11 C10 C9 119.9(6) . . ? C10 C11 C12 119.5(6) . . ? C11 C12 C20 117.7(5) . . ? C11 C12 C13 123.6(5) . . ? C20 C12 C13 118.7(5) . . ? C14 C13 C12 120.4(6) . . ? C13 C14 C15 122.5(6) . . ? C16 C15 C19 116.1(6) . . ? C16 C15 C14 125.5(6) . . ? C19 C15 C14 118.4(5) . . ? C17 C16 C15 120.2(6) . . ? C16 C17 C18 120.5(6) . . ? N10 C18 C17 121.8(6) . . ? N10 C19 C15 123.4(5) . . ? N10 C19 C20 117.4(5) . . ? C15 C19 C20 119.3(5) . . ? N9 C20 C12 123.1(5) . . ? N9 C20 C19 116.3(5) . . ? C12 C20 C19 120.6(5) . . ? N11 C21 C22 124.3(6) . . ? C23 C22 C21 118.3(6) . . ? C22 C23 C24 119.9(7) . . ? C32 C24 C23 116.7(6) . . ? C32 C24 C25 119.1(6) . . ? C23 C24 C25 124.1(7) . . ? C26 C25 C24 120.7(7) . . ? C25 C26 C27 120.7(7) . . ? C31 C27 C26 120.4(6) . . ? C31 C27 C28 117.6(7) . . ? C26 C27 C28 122.0(7) . . ? C29 C28 C27 118.6(7) . . ? C28 C29 C30 120.0(6) . . ? N12 C30 C29 123.0(7) . . ? N12 C31 C27 124.5(6) . . ? N12 C31 C32 116.4(6) . . ? C27 C31 C32 119.1(6) . . ? N11 C32 C24 123.7(6) . . ? N11 C32 C31 116.4(6) . . ? C24 C32 C31 119.9(6) . . ? N13 C33 C34 123.0(7) . . ? C35 C34 C33 118.2(8) . . ? C34 C35 C36 120.7(7) . . ? C35 C36 C44 117.4(8) . . ? C35 C36 C37 126.3(8) . . ? C44 C36 C37 116.3(8) . . ? C38 C37 C36 122.2(9) . . ? C37 C38 C39 122.4(10) . . ? C40 C39 C38 125.1(9) . . ? C40 C39 C43 116.4(9) . . ? C38 C39 C43 118.5(10) . . ? C41 C40 C39 119.7(9) . . ? C42 C41 C40 120.8(10) . . ? N14 C42 C41 122.0(9) . . ? N14 C43 C44 115.9(6) . . ? N14 C43 C39 123.4(8) . . ? C44 C43 C39 120.7(8) . . ? N13 C44 C43 118.3(6) . . ? N13 C44 C36 121.9(8) . . ? C43 C44 C36 119.8(7) . . ? N15 C45 C46 122.4(5) . . ? C47 C46 C45 118.8(6) . . ? C46 C47 C48 120.7(5) . . ? C47 C48 C56 116.0(5) . . ? C47 C48 C49 125.1(5) . . ? C56 C48 C49 118.8(6) . . ? C50 C49 C48 121.9(5) . . ? C49 C50 C51 120.7(5) . . ? C52 C51 C55 118.4(5) . . ? C52 C51 C50 123.9(5) . . ? C55 C51 C50 117.6(5) . . ? C53 C52 C51 118.8(6) . . ? C52 C53 C54 119.6(6) . . ? N16 C54 C53 123.0(6) . . ? N16 C55 C51 122.5(5) . . ? N16 C55 C56 116.1(5) . . ? C51 C55 C56 121.4(5) . . ? N15 C56 C48 124.5(5) . . ? N15 C56 C55 115.9(5) . . ? C48 C56 C55 119.6(5) . . ? N17 C57 C58 122.6(6) . . ? C59 C58 C57 119.5(6) . . ? C58 C59 C60 120.2(6) . . ? C68 C60 C59 116.2(6) . . ? C68 C60 C61 118.1(5) . . ? C59 C60 C61 125.6(6) . . ? C62 C61 C60 122.0(6) . . ? C61 C62 C63 120.3(6) . . ? C67 C63 C64 116.7(5) . . ? C67 C63 C62 119.1(5) . . ? C64 C63 C62 124.1(6) . . ? C65 C64 C63 119.0(6) . . ? C64 C65 C66 121.3(5) . . ? N18 C66 C65 121.5(5) . . ? N18 C67 C63 124.2(5) . . ? N18 C67 C68 116.1(5) . . ? C63 C67 C68 119.8(5) . . ? N17 C68 C60 123.8(5) . . ? N17 C68 C67 115.6(5) . . ? C60 C68 C67 120.7(5) . . ? N19 C69 C70 123.5(8) . . ? C71 C70 C69 119.2(8) . . ? C70 C71 C72 121.6(9) . . ? C73 C72 C71 124.1(10) . . ? C73 C72 C80 120.2(9) . . ? C71 C72 C80 115.7(9) . . ? C74 C73 C72 120.0(11) . . ? C73 C74 C75 123.2(11) . . ? C76 C75 C79 119.7(13) . . ? C76 C75 C74 121.7(14) . . ? C79 C75 C74 118.6(11) . . ? C77 C76 C75 118.9(16) . . ? C76 C77 C78 119.3(15) . . ? N20 C78 C77 124.4(13) . . ? N20 C79 C75 121.0(10) . . ? N20 C79 C80 118.9(11) . . ? C75 C79 C80 120.0(10) . . ? N19 C80 C72 122.5(8) . . ? N19 C80 C79 119.6(10) . . ? C72 C80 C79 117.9(10) . . ? C9 N9 C20 116.5(5) . . ? C9 N9 Co1 130.1(4) . . ? C20 N9 Co1 113.2(3) . . ? C18 N10 C19 118.0(5) . . ? C18 N10 Co1 128.5(4) . . ? C19 N10 Co1 113.5(4) . . ? C21 N11 C32 117.0(6) . . ? C21 N11 Co1 129.5(5) . . ? C32 N11 Co1 113.5(4) . . ? C30 N12 C31 116.3(5) . . ? C30 N12 Co1 129.4(5) . . ? C31 N12 Co1 114.1(4) . . ? C33 N13 C44 118.8(6) . . ? C33 N13 Co1 128.6(4) . . ? C44 N13 Co1 112.5(5) . . ? C42 N14 C43 117.7(7) . . ? C42 N14 Co1 129.3(5) . . ? C43 N14 Co1 112.9(5) . . ? C45 N15 C56 117.4(5) . . ? C45 N15 Co2 129.5(4) . . ? C56 N15 Co2 113.1(4) . . ? C54 N16 C55 117.6(5) . . ? C54 N16 Co2 129.9(4) . . ? C55 N16 Co2 112.4(4) . . ? C57 N17 C68 117.6(5) . . ? C57 N17 Co3 129.7(4) . . ? C68 N17 Co3 112.7(3) . . ? C66 N18 C67 117.4(5) . . ? C66 N18 Co3 130.2(4) . . ? C67 N18 Co3 112.4(3) . . ? C69 N19 C80 117.4(7) . . ? C78 N20 C79 116.6(10) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.955 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.079