Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name S.Brooker C.V.Depree J.D.Ewing _publ_contact_author_name 'Dr Sally Brooker' _publ_contact_author_address ; Chemistry University of Otago PO Box 56 Dunedin NEW ZEALAND ; _publ_contact_author_email SBROOKER@ALKALI.OTAGO.AC.NZ _publ_section_title ; First structurally characterised complexes of a triazolate-containing Schiff-base macrocycle: [CoII2L2(H2O)3(NCCH3)](ClO4)2 and [CoII2L2(NCO)2] ; data_cobt _database_code_CSD 186640 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H45 Cl2 Co2 N13 O12' _chemical_formula_weight 920.51 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.490(5) _cell_length_b 13.180(6) _cell_length_c 22.818(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.136(16) _cell_angle_gamma 90.00 _cell_volume 4041(3) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Orange _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 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type Semi-empirical(SADABS) _exptl_absorpt_correction_T_min 0.28 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 'Bruker SMART area detector' _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 17553 _diffrn_reflns_av_R_equivalents 0.2787 _diffrn_reflns_av_sigmaI/netI 0.6019 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.40 _reflns_number_total 7340 _reflns_number_gt 1799 _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^)+(0.0600P)^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 7340 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3020 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1844 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 0.698 _refine_ls_restrained_S_all 0.698 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.19121(10) 0.15688(11) 0.04531(6) 0.0271(4) Uani 1 1 d . . . Co2 Co 0.32944(11) -0.12700(10) 0.06729(7) 0.0271(5) Uani 1 1 d . . . N1 N 0.3369(6) 0.1071(6) 0.0431(4) 0.027(2) Uani 1 1 d . . . N2 N 0.3789(6) 0.0141(6) 0.0499(3) 0.026(2) Uani 1 1 d . . . C3 C 0.4757(8) 0.0334(8) 0.0687(5) 0.024(3) Uiso 1 1 d . . . N3 N 0.4979(6) 0.1356(6) 0.0708(4) 0.028(2) Uani 1 1 d . . . C5 C 0.4064(8) 0.1755(8) 0.0542(4) 0.025(3) Uiso 1 1 d . . . C6 C 0.3732(9) 0.2838(8) 0.0560(5) 0.032(3) Uani 1 1 d . . . C7 C 0.4487(7) 0.3680(7) 0.0636(5) 0.038(3) Uani 1 1 d . . . H7A H 0.4430 0.4115 0.0286 0.046 Uiso 1 1 calc R . . H7B H 0.5158 0.3390 0.0689 0.046 Uiso 1 1 calc R . . H7C H 0.4365 0.4085 0.0983 0.046 Uiso 1 1 calc R . . N4 N 0.2791(7) 0.2953(6) 0.0478(4) 0.028(2) Uani 1 1 d . . . C8 C 0.2357(9) 0.3977(8) 0.0474(5) 0.043(4) Uani 1 1 d . . . H8A H 0.2656 0.4400 0.0177 0.051 Uiso 1 1 calc R . . H8B H 0.2511 0.4297 0.0864 0.051 Uiso 1 1 calc R . . C9 C 0.1233(9) 0.3933(8) 0.0331(5) 0.042(3) Uani 1 1 d . . . H9A H 0.1084 0.3466 -0.0005 0.050 Uiso 1 1 calc R . . H9B H 0.0995 0.4616 0.0205 0.050 Uiso 1 1 calc R . . C10 C 0.0649(8) 0.3582(8) 0.0845(5) 0.044(3) Uani 1 1 d . . . H10A H 0.1136 0.3354 0.1169 0.053 Uiso 1 1 calc R . . H10B H 0.0300 0.4179 0.0991 0.053 Uiso 1 1 calc R . . C11 C -0.0092(8) 0.2764(8) 0.0727(5) 0.041(3) Uani 1 1 d . . . H11A H -0.0539 0.2945 0.0375 0.049 Uiso 1 1 calc R . . H11B H -0.0501 0.2711 0.1065 0.049 Uiso 1 1 calc R . . N5 N 0.0368(6) 0.1767(7) 0.0629(4) 0.027(2) Uani 1 1 d . . . C12 C -0.0091(8) 0.0938(9) 0.0764(4) 0.029(3) Uani 1 1 d . . . C13 C -0.1108(7) 0.0842(8) 0.0974(5) 0.034(3) Uani 1 1 d . . . H13A H -0.1164 0.1301 0.1307 0.040 Uiso 1 1 calc R . . H13B H -0.1213 0.0142 0.1098 0.040 Uiso 1 1 calc R . . H13C H -0.1610 0.1021 0.0654 0.040 Uiso 1 1 calc R . . N6 N 0.1388(6) 0.0124(6) 0.0520(3) 0.021(2) Uani 1 1 d . . . N7 N 0.1823(6) -0.0785(6) 0.0566(3) 0.022(2) Uani 1 1 d . . . C14 C 0.0485(8) 0.0014(9) 0.0699(5) 0.025(3) Uiso 1 1 d . . . N8 N 0.0287(6) -0.0961(6) 0.0872(4) 0.031(3) Uani 1 1 d . . . C15 C 0.1178(8) -0.1420(8) 0.0781(4) 0.026(3) Uiso 1 1 d . . . C16 C 0.1520(10) -0.2454(8) 0.0957(5) 0.034(3) Uani 1 1 d . . . C17 C 0.0804(7) -0.3230(8) 0.1138(5) 0.036(3) Uani 1 1 d . . . H17A H 0.0801 -0.3813 0.0871 0.043 Uiso 1 1 calc R . . H17B H 0.0136 -0.2935 0.1121 0.043 Uiso 1 1 calc R . . H17C H 0.1006 -0.3453 0.1540 0.043 Uiso 1 1 calc R . . N9 N 0.2475(7) -0.2577(6) 0.0941(4) 0.027(2) Uani 1 1 d . . . C18 C 0.2928(8) -0.3567(8) 0.1143(5) 0.042(3) Uani 1 1 d . . . H18A H 0.2881 -0.4060 0.0815 0.050 Uiso 1 1 calc R . . H18B H 0.2568 -0.3848 0.1466 0.050 Uiso 1 1 calc R . . C19 C 0.4039(8) -0.3378(8) 0.1362(4) 0.037(3) Uani 1 1 d . . . H19A H 0.4080 -0.2746 0.1598 0.044 Uiso 1 1 calc R . . H19B H 0.4267 -0.3941 0.1628 0.044 Uiso 1 1 calc R . . C20 C 0.4764(8) -0.3288(8) 0.0880(5) 0.034(3) Uani 1 1 d . . . H20A H 0.5173 -0.3911 0.0881 0.041 Uiso 1 1 calc R . . H20B H 0.4375 -0.3240 0.0492 0.041 Uiso 1 1 calc R . . C21 C 0.5450(8) -0.2374(8) 0.0959(5) 0.037(3) Uani 1 1 d . . . H21A H 0.5774 -0.2371 0.1366 0.044 Uiso 1 1 calc R . . H21B H 0.5979 -0.2435 0.0687 0.044 Uiso 1 1 calc R . . N10 N 0.4914(6) -0.1402(6) 0.0846(3) 0.027(2) Uani 1 1 d . . . C22 C 0.5398(8) -0.0566(8) 0.0823(5) 0.029(3) Uani 1 1 d . . . C23 C 0.6482(8) -0.0404(8) 0.1003(5) 0.037(3) Uani 1 1 d . . . H23A H 0.6602 -0.0457 0.1432 0.044 Uiso 1 1 calc R . . H23B H 0.6680 0.0271 0.0877 0.044 Uiso 1 1 calc R . . H23C H 0.6874 -0.0921 0.0818 0.044 Uiso 1 1 calc R . . O30 O 0.2200(5) 0.1585(5) 0.1401(3) 0.041(2) Uani 1 1 d . . . H30A H 0.2123 0.2114 0.1621 0.050 Uiso 1 1 d . . . H30B H 0.1997 0.1163 0.1658 0.050 Uiso 1 1 d . . . O31 O 0.1563(5) 0.1722(5) -0.0450(3) 0.038(2) Uani 1 1 d . . . H31A H 0.1811 0.2117 -0.0704 0.045 Uiso 1 1 d . . . H31B H 0.0923 0.1902 -0.0491 0.045 Uiso 1 1 d . . . O32 O 0.3294(5) -0.1874(5) -0.0175(3) 0.0275(19) Uani 1 1 d . . . H32A H 0.3090 -0.2477 -0.0142 0.033 Uiso 1 1 d . . . H32B H 0.3710 -0.1938 -0.0438 0.033 Uiso 1 1 d . . . N30 N 0.3375(7) -0.0812(7) 0.1607(4) 0.033(3) Uani 1 1 d . . . C30 C 0.3456(9) -0.0420(9) 0.2036(6) 0.035(3) Uani 1 1 d . . . C31 C 0.3537(9) 0.0095(9) 0.2617(5) 0.063(4) Uani 1 1 d . . . H31C H 0.3050 0.0648 0.2612 0.076 Uiso 1 1 calc R . . H31D H 0.4210 0.0373 0.2699 0.076 Uiso 1 1 calc R . . H31E H 0.3406 -0.0394 0.2924 0.076 Uiso 1 1 calc R . . O40 O 0.1991(6) 0.2993(5) -0.1316(3) 0.055(3) Uani 1 1 d . . . H40A H 0.2220 0.2681 -0.1617 0.066 Uiso 1 1 d . . . H40B H 0.2174 0.3579 -0.1196 0.066 Uiso 1 1 d . . . N40 N 0.1002(11) 0.0527(14) 0.2143(6) 0.119(6) Uani 1 1 d . . . C40 C 0.0508(14) -0.0108(18) 0.2330(7) 0.113(8) Uani 1 1 d . . . C41 C -0.0116(12) -0.0910(14) 0.2526(7) 0.143(9) Uani 1 1 d . . . H41A H -0.0448 -0.1259 0.2183 0.172 Uiso 1 1 calc R . . H41B H -0.0618 -0.0618 0.2762 0.172 Uiso 1 1 calc R . . H41C H 0.0295 -0.1395 0.2765 0.172 Uiso 1 1 calc R . . N50 N 0.1855(12) -0.2002(17) -0.2462(7) 0.178(10) Uani 1 1 d . . . C50 C 0.2672(16) -0.1928(13) -0.2303(7) 0.085(6) Uani 1 1 d . . . C51 C 0.3714(11) -0.1802(10) -0.2089(5) 0.074(5) Uani 1 1 d . . . H51A H 0.3902 -0.1087 -0.2120 0.089 Uiso 1 1 calc R . . H51B H 0.4128 -0.2217 -0.2327 0.089 Uiso 1 1 calc R . . H51C H 0.3813 -0.2017 -0.1677 0.089 Uiso 1 1 calc R . . Cl1 Cl 0.2524(2) 0.5729(2) -0.09119(15) 0.0409(9) Uani 1 1 d . . . O11 O 0.1606(6) 0.5248(7) -0.1129(4) 0.091(4) Uani 1 1 d . . . O12 O 0.3288(7) 0.4977(7) -0.0860(4) 0.081(3) Uani 1 1 d . . . O13 O 0.2380(6) 0.6173(5) -0.0342(3) 0.049(2) Uani 1 1 d . . . O14 O 0.2819(7) 0.6520(6) -0.1289(4) 0.085(3) Uani 1 1 d . . . Cl2 Cl 0.3476(3) 0.1492(3) -0.26679(15) 0.0578(10) Uani 1 1 d . . . O21 O 0.2806(7) 0.1942(7) -0.2295(4) 0.084(3) Uani 1 1 d . . . O22 O 0.3785(6) 0.2280(8) -0.3077(4) 0.086(3) Uani 1 1 d . . . O23 O 0.4376(7) 0.1145(8) -0.2329(4) 0.094(4) Uani 1 1 d . . . O24 O 0.3085(11) 0.0705(9) -0.3023(6) 0.176(6) 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 0.0268(9) 0.0212(9) 0.0317(10) -0.0003(8) -0.0057(8) 0.0001(8) Co2 0.0288(10) 0.0205(9) 0.0304(10) -0.0020(8) -0.0063(8) 0.0013(8) N1 0.016(5) 0.024(6) 0.038(6) -0.003(5) -0.012(5) -0.008(4) N2 0.036(6) 0.019(6) 0.020(6) -0.001(4) -0.012(5) 0.010(5) N3 0.028(5) 0.023(6) 0.031(6) 0.003(5) -0.007(5) -0.007(5) C6 0.037(8) 0.019(7) 0.038(8) -0.005(6) 0.000(7) -0.009(6) C7 0.046(8) 0.018(7) 0.048(8) -0.002(6) -0.005(7) -0.014(6) N4 0.041(7) 0.013(6) 0.030(6) -0.005(5) -0.001(6) -0.004(5) C8 0.053(9) 0.026(8) 0.045(9) 0.004(6) -0.014(7) -0.007(6) C9 0.065(10) 0.014(7) 0.043(9) 0.008(6) -0.015(8) 0.001(6) C10 0.053(8) 0.010(7) 0.071(10) -0.001(7) 0.004(8) 0.014(6) C11 0.035(8) 0.021(8) 0.065(10) -0.001(7) -0.002(7) -0.009(6) N5 0.029(6) 0.017(6) 0.033(6) -0.007(5) 0.000(5) 0.003(5) C12 0.022(7) 0.054(9) 0.011(7) -0.014(6) 0.001(6) 0.008(6) C13 0.026(7) 0.035(8) 0.040(8) -0.011(6) 0.001(7) 0.004(6) N6 0.045(6) 0.003(5) 0.017(5) 0.004(4) 0.000(5) 0.004(4) N7 0.017(5) 0.032(6) 0.015(5) -0.011(5) -0.002(5) -0.012(5) N8 0.033(6) 0.035(6) 0.022(6) 0.001(5) -0.019(5) -0.002(5) C16 0.065(10) 0.006(7) 0.028(8) 0.003(5) -0.010(8) -0.011(7) C17 0.038(8) 0.036(8) 0.032(8) 0.009(6) -0.005(6) 0.006(6) N9 0.028(6) 0.016(6) 0.035(6) 0.003(5) -0.004(6) 0.008(5) C18 0.057(9) 0.015(7) 0.052(9) 0.014(6) -0.006(7) 0.001(6) C19 0.053(8) 0.033(8) 0.020(7) 0.003(6) -0.020(7) 0.012(6) C20 0.039(8) 0.024(8) 0.037(8) 0.007(6) -0.011(7) 0.008(6) C21 0.055(9) 0.029(8) 0.027(7) -0.010(6) 0.008(7) 0.025(7) N10 0.038(6) 0.015(6) 0.024(6) -0.008(5) -0.009(5) 0.005(5) C22 0.022(7) 0.028(8) 0.034(8) 0.004(6) -0.011(6) 0.006(6) C23 0.039(8) 0.037(8) 0.032(8) 0.003(6) -0.009(7) 0.008(6) O30 0.055(5) 0.033(5) 0.034(5) 0.000(4) -0.010(4) 0.002(4) O31 0.037(5) 0.037(5) 0.039(5) 0.008(4) 0.004(4) 0.001(4) O32 0.030(5) 0.020(4) 0.032(5) -0.008(4) 0.001(4) -0.001(3) N30 0.031(6) 0.018(6) 0.050(8) -0.009(6) 0.007(6) 0.009(5) C30 0.040(8) 0.032(9) 0.037(9) 0.004(7) 0.020(8) -0.001(6) C31 0.065(11) 0.082(11) 0.042(9) -0.016(8) -0.005(8) 0.021(8) O40 0.080(7) 0.036(6) 0.051(6) -0.004(4) 0.015(5) -0.006(5) N40 0.087(13) 0.193(19) 0.075(12) 0.012(11) -0.009(9) -0.067(11) C40 0.087(17) 0.20(3) 0.044(12) 0.023(14) -0.017(12) -0.042(14) C41 0.129(17) 0.21(2) 0.097(15) 0.070(14) 0.015(13) -0.093(15) N50 0.085(14) 0.35(3) 0.091(14) 0.064(15) -0.041(12) -0.020(16) C50 0.096(15) 0.117(15) 0.040(11) 0.029(10) -0.006(11) 0.002(14) C51 0.100(14) 0.075(12) 0.047(10) -0.005(8) 0.009(10) -0.021(10) Cl1 0.051(2) 0.029(2) 0.043(2) -0.0007(17) 0.006(2) 0.0008(17) O11 0.035(6) 0.098(8) 0.134(10) -0.054(7) -0.034(6) 0.000(6) O12 0.071(7) 0.071(7) 0.102(8) -0.017(6) 0.010(6) 0.042(6) O13 0.077(7) 0.024(5) 0.047(6) -0.005(4) 0.009(5) -0.003(4) O14 0.141(9) 0.055(7) 0.063(7) 0.025(6) 0.036(6) -0.029(6) Cl2 0.071(3) 0.064(3) 0.035(2) -0.004(2) -0.015(2) 0.019(2) O21 0.079(8) 0.133(10) 0.041(6) -0.022(6) 0.015(6) 0.037(7) O22 0.064(7) 0.117(9) 0.081(8) 0.043(7) 0.024(6) 0.016(6) O23 0.064(7) 0.155(10) 0.059(7) 0.028(7) -0.010(6) 0.063(7) O24 0.208(15) 0.123(12) 0.180(14) -0.066(10) -0.067(12) -0.027(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 N6 2.041(8) . y Co1 N1 2.077(8) . y Co1 O31 2.083(7) . y Co1 O30 2.162(7) . y Co1 N5 2.172(9) . y Co1 N4 2.174(8) . y Co2 N2 2.027(8) . y Co2 N7 2.078(8) . y Co2 O32 2.091(6) . y Co2 N9 2.164(9) . y Co2 N10 2.192(8) . y Co2 N30 2.209(10) . y N1 C5 1.309(11) . ? N1 N2 1.354(10) . ? N2 C3 1.361(12) . ? C3 N3 1.379(11) . ? C3 C22 1.484(13) . ? N3 C5 1.364(12) . ? C5 C6 1.498(13) . ? C6 N4 1.276(12) . ? C6 C7 1.506(13) . ? N4 C8 1.471(12) . ? C8 C9 1.523(13) . ? C9 C10 1.543(14) . ? C10 C11 1.477(13) . ? C11 N5 1.479(12) . ? N5 C12 1.306(12) . ? C12 C14 1.458(14) . ? C12 C13 1.498(13) . ? N6 C14 1.327(12) . ? N6 N7 1.335(10) . ? N7 C15 1.334(11) . ? C14 N8 1.378(12) . ? N8 C15 1.378(12) . ? C15 C16 1.482(13) . ? C16 N9 1.302(13) . ? C16 C17 1.491(13) . ? N9 C18 1.496(11) . ? C18 C19 1.557(13) . ? C19 C20 1.540(13) . ? C20 C21 1.519(13) . ? C21 N10 1.483(12) . ? N10 C22 1.284(12) . ? C22 C23 1.499(13) . ? N30 C30 1.104(12) . ? C30 C31 1.484(15) . ? N40 C40 1.174(19) . ? C40 C41 1.45(2) . ? N50 C50 1.134(19) . ? C50 C51 1.455(19) . ? Cl1 O12 1.427(8) . ? Cl1 O14 1.431(8) . ? Cl1 O11 1.440(8) . ? Cl1 O13 1.455(7) . ? Cl2 O24 1.390(11) . ? Cl2 O21 1.424(8) . ? Cl2 O23 1.454(8) . ? Cl2 O22 1.481(9) . ? 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 N6 Co1 N1 92.4(3) . . y N6 Co1 O31 96.6(3) . . y N1 Co1 O31 97.9(3) . . y N6 Co1 O30 88.1(3) . . y N1 Co1 O30 86.7(3) . . y O31 Co1 O30 173.3(3) . . y N6 Co1 N5 75.8(3) . . y N1 Co1 N5 165.4(3) . . y O31 Co1 N5 92.1(3) . . y O30 Co1 N5 84.4(3) . . y N6 Co1 N4 166.6(3) . . y N1 Co1 N4 75.6(3) . . y O31 Co1 N4 91.1(3) . . y O30 Co1 N4 85.2(3) . . y N5 Co1 N4 115.1(3) . . y N2 Co2 N7 91.3(3) . . y N2 Co2 O32 98.1(3) . . y N7 Co2 O32 95.0(3) . . y N2 Co2 N9 166.2(4) . . y N7 Co2 N9 76.8(3) . . y O32 Co2 N9 90.0(3) . . y N2 Co2 N10 76.6(3) . . y N7 Co2 N10 166.2(3) . . y O32 Co2 N10 93.1(3) . . y N9 Co2 N10 114.3(3) . . y N2 Co2 N30 87.1(3) . . y N7 Co2 N30 89.6(3) . . y O32 Co2 N30 172.9(3) . . y N9 Co2 N30 85.8(3) . . y N10 Co2 N30 83.5(3) . . y C5 N1 N2 108.4(9) . . ? C5 N1 Co1 116.1(7) . . ? N2 N1 Co1 132.1(7) . . y N1 N2 C3 104.3(8) . . ? N1 N2 Co2 135.4(7) . . y C3 N2 Co2 115.7(7) . . ? N2 C3 N3 113.1(9) . . ? N2 C3 C22 116.1(10) . . ? N3 C3 C22 130.7(10) . . ? C5 N3 C3 100.3(8) . . ? N1 C5 N3 113.7(10) . . ? N1 C5 C6 116.9(10) . . ? N3 C5 C6 128.7(10) . . ? N4 C6 C5 113.9(10) . . ? N4 C6 C7 125.7(10) . . ? C5 C6 C7 120.4(10) . . ? C6 N4 C8 120.0(9) . . ? C6 N4 Co1 115.9(7) . . ? C8 N4 Co1 123.7(7) . . ? N4 C8 C9 110.8(9) . . ? C8 C9 C10 114.5(9) . . ? C11 C10 C9 117.6(10) . . ? C10 C11 N5 113.0(10) . . ? C12 N5 C11 119.6(9) . . ? C12 N5 Co1 115.2(7) . . ? C11 N5 Co1 123.8(7) . . ? N5 C12 C14 114.0(10) . . ? N5 C12 C13 127.8(10) . . ? C14 C12 C13 118.2(11) . . ? C14 N6 N7 106.7(9) . . ? C14 N6 Co1 117.3(7) . . ? N7 N6 Co1 133.6(7) . . y C15 N7 N6 107.2(8) . . ? C15 N7 Co2 114.3(7) . . ? N6 N7 Co2 134.0(6) . . y N6 C14 N8 113.4(10) . . ? N6 C14 C12 116.8(10) . . ? N8 C14 C12 129.1(11) . . ? C15 N8 C14 100.0(9) . . ? N7 C15 N8 112.7(9) . . ? N7 C15 C16 118.6(10) . . ? N8 C15 C16 128.2(10) . . ? N9 C16 C15 113.1(10) . . ? N9 C16 C17 126.1(10) . . ? C15 C16 C17 120.8(11) . . ? C16 N9 C18 118.5(9) . . ? C16 N9 Co2 116.1(7) . . ? C18 N9 Co2 125.2(7) . . ? N9 C18 C19 108.3(8) . . ? C20 C19 C18 115.9(8) . . ? C21 C20 C19 113.3(9) . . ? N10 C21 C20 112.4(9) . . ? C22 N10 C21 120.5(9) . . ? C22 N10 Co2 115.3(7) . . ? C21 N10 Co2 124.2(7) . . ? N10 C22 C3 113.9(10) . . ? N10 C22 C23 126.7(10) . . ? C3 C22 C23 118.7(10) . . ? C30 N30 Co2 167.5(10) . . ? N30 C30 C31 178.3(14) . . ? N40 C40 C41 177(2) . . ? N50 C50 C51 178(2) . . ? O12 Cl1 O14 108.6(6) . . ? O12 Cl1 O11 108.4(6) . . ? O14 Cl1 O11 113.0(6) . . ? O12 Cl1 O13 110.9(5) . . ? O14 Cl1 O13 108.2(5) . . ? O11 Cl1 O13 107.8(5) . . ? O24 Cl2 O21 115.5(8) . . ? O24 Cl2 O23 109.3(8) . . ? O21 Cl2 O23 110.9(6) . . ? O24 Cl2 O22 105.6(8) . . ? O21 Cl2 O22 108.2(6) . . ? O23 Cl2 O22 106.6(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Co1 N1 C5 -162.7(8) . . . . ? O31 Co1 N1 C5 100.3(8) . . . . ? O30 Co1 N1 C5 -74.7(8) . . . . ? N5 Co1 N1 C5 -127.3(13) . . . . ? N4 Co1 N1 C5 11.2(7) . . . . ? N6 Co1 N1 N2 -6.0(9) . . . . ? O31 Co1 N1 N2 -103.0(9) . . . . ? O30 Co1 N1 N2 82.0(9) . . . . ? N5 Co1 N1 N2 29.4(18) . . . . ? N4 Co1 N1 N2 167.9(9) . . . . ? C5 N1 N2 C3 3.2(11) . . . . ? Co1 N1 N2 C3 -154.8(7) . . . . ? C5 N1 N2 Co2 156.6(8) . . . . ? Co1 N1 N2 Co2 -1.4(14) . . . . ? N7 Co2 N2 N1 9.1(9) . . . . ? O32 Co2 N2 N1 104.3(9) . . . . ? N9 Co2 N2 N1 -21(2) . . . . ? N10 Co2 N2 N1 -164.4(10) . . . . ? N30 Co2 N2 N1 -80.5(9) . . . . ? N7 Co2 N2 C3 160.3(8) . . . . ? O32 Co2 N2 C3 -104.4(8) . . . . ? N9 Co2 N2 C3 130.1(13) . . . . ? N10 Co2 N2 C3 -13.2(7) . . . . ? N30 Co2 N2 C3 70.8(8) . . . . ? N1 N2 C3 N3 -3.5(12) . . . . ? Co2 N2 C3 N3 -163.1(6) . . . . ? N1 N2 C3 C22 177.6(9) . . . . ? Co2 N2 C3 C22 18.0(12) . . . . ? N2 C3 N3 C5 2.3(12) . . . . ? C22 C3 N3 C5 -179.0(11) . . . . ? N2 N1 C5 N3 -1.9(13) . . . . ? Co1 N1 C5 N3 160.0(7) . . . . ? N2 N1 C5 C6 -173.0(9) . . . . ? Co1 N1 C5 C6 -11.1(13) . . . . ? C3 N3 C5 N1 -0.2(12) . . . . ? C3 N3 C5 C6 169.6(11) . . . . ? N1 C5 C6 N4 1.8(16) . . . . ? N3 C5 C6 N4 -167.8(10) . . . . ? N1 C5 C6 C7 -175.1(10) . . . . ? N3 C5 C6 C7 15.4(18) . . . . ? C5 C6 N4 C8 -179.0(9) . . . . ? C7 C6 N4 C8 -2.4(18) . . . . ? C5 C6 N4 Co1 7.9(13) . . . . ? C7 C6 N4 Co1 -175.4(8) . . . . ? N6 Co1 N4 C6 17(2) . . . . ? N1 Co1 N4 C6 -10.5(8) . . . . ? O31 Co1 N4 C6 -108.3(9) . . . . ? O30 Co1 N4 C6 77.4(9) . . . . ? N5 Co1 N4 C6 158.9(8) . . . . ? N6 Co1 N4 C8 -156.1(13) . . . . ? N1 Co1 N4 C8 176.8(9) . . . . ? O31 Co1 N4 C8 78.9(8) . . . . ? O30 Co1 N4 C8 -95.4(8) . . . . ? N5 Co1 N4 C8 -13.9(9) . . . . ? C6 N4 C8 C9 176.4(10) . . . . ? Co1 N4 C8 C9 -11.1(13) . . . . ? N4 C8 C9 C10 76.6(12) . . . . ? C8 C9 C10 C11 -130.0(10) . . . . ? C9 C10 C11 N5 70.0(13) . . . . ? C10 C11 N5 C12 151.3(10) . . . . ? C10 C11 N5 Co1 -14.8(14) . . . . ? N6 Co1 N5 C12 8.3(7) . . . . ? N1 Co1 N5 C12 -28.4(17) . . . . ? O31 Co1 N5 C12 104.6(8) . . . . ? O30 Co1 N5 C12 -81.2(8) . . . . ? N4 Co1 N5 C12 -163.2(7) . . . . ? N6 Co1 N5 C11 174.9(9) . . . . ? N1 Co1 N5 C11 138.2(12) . . . . ? O31 Co1 N5 C11 -88.8(8) . . . . ? O30 Co1 N5 C11 85.5(8) . . . . ? N4 Co1 N5 C11 3.4(9) . . . . ? C11 N5 C12 C14 -174.4(9) . . . . ? Co1 N5 C12 C14 -7.2(12) . . . . ? C11 N5 C12 C13 5.1(16) . . . . ? Co1 N5 C12 C13 172.3(8) . . . . ? N1 Co1 N6 C14 163.3(7) . . . . ? O31 Co1 N6 C14 -98.5(7) . . . . ? O30 Co1 N6 C14 76.7(7) . . . . ? N5 Co1 N6 C14 -8.1(7) . . . . ? N4 Co1 N6 C14 137.1(14) . . . . ? N1 Co1 N6 N7 3.4(9) . . . . ? O31 Co1 N6 N7 101.6(9) . . . . ? O30 Co1 N6 N7 -83.2(9) . . . . ? N5 Co1 N6 N7 -167.9(9) . . . . ? N4 Co1 N6 N7 -23(2) . . . . ? C14 N6 N7 C15 -1.0(11) . . . . ? Co1 N6 N7 C15 160.4(7) . . . . ? C14 N6 N7 Co2 -154.8(7) . . . . ? Co1 N6 N7 Co2 6.6(14) . . . . ? N2 Co2 N7 C15 -164.1(7) . . . . ? O32 Co2 N7 C15 97.6(7) . . . . ? N9 Co2 N7 C15 8.8(7) . . . . ? N10 Co2 N7 C15 -136.7(12) . . . . ? N30 Co2 N7 C15 -77.0(7) . . . . ? N2 Co2 N7 N6 -11.7(9) . . . . ? O32 Co2 N7 N6 -110.0(9) . . . . ? N9 Co2 N7 N6 161.2(9) . . . . ? N10 Co2 N7 N6 15.8(19) . . . . ? N30 Co2 N7 N6 75.4(9) . . . . ? N7 N6 C14 N8 0.3(12) . . . . ? Co1 N6 C14 N8 -164.6(6) . . . . ? N7 N6 C14 C12 172.0(8) . . . . ? Co1 N6 C14 C12 7.1(12) . . . . ? N5 C12 C14 N6 0.4(14) . . . . ? C13 C12 C14 N6 -179.1(9) . . . . ? N5 C12 C14 N8 170.6(10) . . . . ? C13 C12 C14 N8 -8.9(16) . . . . ? N6 C14 N8 C15 0.5(11) . . . . ? C12 C14 N8 C15 -170.0(11) . . . . ? N6 N7 C15 N8 1.4(11) . . . . ? Co2 N7 C15 N8 161.0(6) . . . . ? N6 N7 C15 C16 -171.5(9) . . . . ? Co2 N7 C15 C16 -11.9(12) . . . . ? C14 N8 C15 N7 -1.2(11) . . . . ? C14 N8 C15 C16 170.9(10) . . . . ? N7 C15 C16 N9 7.7(15) . . . . ? N8 C15 C16 N9 -163.9(10) . . . . ? N7 C15 C16 C17 -173.2(9) . . . . ? N8 C15 C16 C17 15.1(17) . . . . ? C15 C16 N9 C18 176.3(9) . . . . ? C17 C16 N9 C18 -2.7(17) . . . . ? C15 C16 N9 Co2 0.3(12) . . . . ? C17 C16 N9 Co2 -178.7(8) . . . . ? N2 Co2 N9 C16 26.3(19) . . . . ? N7 Co2 N9 C16 -4.8(8) . . . . ? O32 Co2 N9 C16 -99.9(8) . . . . ? N10 Co2 N9 C16 166.7(8) . . . . ? N30 Co2 N9 C16 85.8(8) . . . . ? N2 Co2 N9 C18 -149.4(12) . . . . ? N7 Co2 N9 C18 179.5(9) . . . . ? O32 Co2 N9 C18 84.4(8) . . . . ? N10 Co2 N9 C18 -9.0(9) . . . . ? N30 Co2 N9 C18 -89.9(9) . . . . ? C16 N9 C18 C19 -153.6(10) . . . . ? Co2 N9 C18 C19 22.0(12) . . . . ? N9 C18 C19 C20 -79.3(11) . . . . ? C18 C19 C20 C21 131.8(10) . . . . ? C19 C20 C21 N10 -70.0(12) . . . . ? C20 C21 N10 C22 -171.6(10) . . . . ? C20 C21 N10 Co2 6.0(12) . . . . ? N2 Co2 N10 C22 6.8(8) . . . . ? N7 Co2 N10 C22 -21.5(18) . . . . ? O32 Co2 N10 C22 104.4(8) . . . . ? N9 Co2 N10 C22 -164.2(8) . . . . ? N30 Co2 N10 C22 -81.8(8) . . . . ? N2 Co2 N10 C21 -170.8(8) . . . . ? N7 Co2 N10 C21 160.8(12) . . . . ? O32 Co2 N10 C21 -73.3(8) . . . . ? N9 Co2 N10 C21 18.2(8) . . . . ? N30 Co2 N10 C21 100.6(8) . . . . ? C21 N10 C22 C3 178.1(9) . . . . ? Co2 N10 C22 C3 0.4(12) . . . . ? C21 N10 C22 C23 -11.5(17) . . . . ? Co2 N10 C22 C23 170.8(9) . . . . ? N2 C3 C22 N10 -11.7(15) . . . . ? N3 C3 C22 N10 169.6(10) . . . . ? N2 C3 C22 C23 177.0(10) . . . . ? N3 C3 C22 C23 -1.7(18) . . . . ? N2 Co2 N30 C30 5(5) . . . . ? N7 Co2 N30 C30 -86(5) . . . . ? O32 Co2 N30 C30 143(4) . . . . ? N9 Co2 N30 C30 -163(5) . . . . ? N10 Co2 N30 C30 82(5) . . . . ? Co2 N30 C30 C31 130(47) . . . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 0.398 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.099 data_cobtyj _database_code_CSD 186641 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H28 Co2 N12 O2' _chemical_formula_weight 610.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.286(5) _cell_length_b 15.836(6) _cell_length_c 13.262(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.294(4) _cell_angle_gamma 90.00 _cell_volume 2543.1(15) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description trapezoid-block _exptl_crystal_colour magenta _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 1.351 _exptl_absorpt_correction_type Semi-empirical(SADABS) _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 'Bruker SMART area detector' _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 31449 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.41 _reflns_number_total 5131 _reflns_number_gt 3099 _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^)+(0.0308P)^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 5131 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0644 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.856 _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 0.11066(2) 0.056173(19) 0.34230(2) 0.02972(10) Uani 1 1 d . . . Co2 Co 0.38824(3) 0.045315(19) 0.66957(2) 0.03008(10) Uani 1 1 d . . . N1 N 0.27611(16) 0.08414(13) 0.40962(14) 0.0406(5) Uani 1 1 d . . . N2 N 0.36405(16) 0.07571(13) 0.51034(14) 0.0407(5) Uani 1 1 d . . . C3 C 0.44830(19) 0.11480(14) 0.49989(17) 0.0291(6) Uani 1 1 d . . . N3 N 0.42264(15) 0.14864(11) 0.39845(14) 0.0316(5) Uani 1 1 d . . . C5 C 0.3152(2) 0.12711(15) 0.34629(17) 0.0315(6) Uani 1 1 d . . . C6 C 0.2368(2) 0.14455(14) 0.23076(17) 0.0304(6) Uani 1 1 d . . . C7 C 0.2826(2) 0.18080(15) 0.15380(17) 0.0404(7) Uani 1 1 d . . . H7A H 0.3011 0.1348 0.1149 0.048 Uiso 1 1 calc R . . H7B H 0.3493 0.2135 0.1964 0.048 Uiso 1 1 calc R . . H7C H 0.2274 0.2177 0.0998 0.048 Uiso 1 1 calc R . . N4 N 0.13665(16) 0.12162(11) 0.20701(13) 0.0315(5) Uani 1 1 d . . . C8 C 0.05541(19) 0.12838(15) 0.09005(17) 0.0370(6) Uani 1 1 d . . . H8A H 0.0795 0.0923 0.0431 0.044 Uiso 1 1 calc R . . H8B H 0.0527 0.1875 0.0648 0.044 Uiso 1 1 calc R . . C9 C -0.05814(19) 0.10165(15) 0.07650(17) 0.0383(6) Uani 1 1 d . . . H9A H -0.0535 0.0445 0.1083 0.046 Uiso 1 1 calc R . . H9B H -0.1067 0.0982 -0.0034 0.046 Uiso 1 1 calc R . . C10 C -0.11092(19) 0.16166(15) 0.13195(18) 0.0379(6) Uani 1 1 d . . . H10A H -0.1782 0.1864 0.0738 0.045 Uiso 1 1 calc R . . H10B H -0.0587 0.2085 0.1667 0.045 Uiso 1 1 calc R . . C11 C -0.14263(19) 0.12137(16) 0.22030(17) 0.0374(6) Uani 1 1 d . . . H11A H -0.1951 0.1588 0.2344 0.045 Uiso 1 1 calc R . . H11B H -0.1801 0.0668 0.1924 0.045 Uiso 1 1 calc R . . N5 N -0.04431(15) 0.10705(11) 0.32540(14) 0.0298(5) Uani 1 1 d . . . C12 C -0.05096(19) 0.12414(13) 0.41810(17) 0.0281(6) Uani 1 1 d . . . C13 C -0.14759(19) 0.15947(14) 0.43454(18) 0.0343(6) Uani 1 1 d . . . H13A H -0.1636 0.2165 0.4033 0.041 Uiso 1 1 calc R . . H13B H -0.1303 0.1618 0.5138 0.041 Uiso 1 1 calc R . . H13C H -0.2122 0.1233 0.3973 0.041 Uiso 1 1 calc R . . C14 C 0.05116(19) 0.10655(14) 0.51847(17) 0.0275(6) Uani 1 1 d . . . N6 N 0.12781(16) 0.05730(12) 0.50721(14) 0.0332(5) Uani 1 1 d . . . N7 N 0.21500(15) 0.05752(12) 0.60866(14) 0.0336(5) Uani 1 1 d . . . C15 C 0.1840(2) 0.10728(14) 0.67271(17) 0.0300(6) Uani 1 1 d . . . N8 N 0.08036(15) 0.13940(12) 0.62046(14) 0.0321(5) Uani 1 1 d . . . C16 C 0.2657(2) 0.12591(14) 0.78583(17) 0.0318(6) Uani 1 1 d . . . C17 C 0.2234(2) 0.15995(16) 0.86633(17) 0.0441(7) Uani 1 1 d . . . H17A H 0.2168 0.1138 0.9125 0.053 Uiso 1 1 calc R . . H17B H 0.1508 0.1858 0.8258 0.053 Uiso 1 1 calc R . . H17C H 0.2749 0.2025 0.9134 0.053 Uiso 1 1 calc R . . N9 N 0.36684(16) 0.10907(11) 0.80415(14) 0.0318(5) Uani 1 1 d . . . C18 C 0.4541(2) 0.12304(16) 0.91685(17) 0.0412(7) Uani 1 1 d . . . H18A H 0.4608 0.0719 0.9622 0.049 Uiso 1 1 calc R . . H18B H 0.4322 0.1706 0.9520 0.049 Uiso 1 1 calc R . . C19 C 0.5657(2) 0.14254(16) 0.91533(19) 0.0473(7) Uani 1 1 d . . . H19A H 0.6145 0.1662 0.9883 0.057 Uiso 1 1 calc R . . H19B H 0.5550 0.1869 0.8593 0.057 Uiso 1 1 calc R . . C20 C 0.6250(2) 0.06805(16) 0.89049(18) 0.0437(7) Uani 1 1 d . . . H20A H 0.5777 0.0173 0.8760 0.052 Uiso 1 1 calc R . . H20B H 0.6942 0.0565 0.9563 0.052 Uiso 1 1 calc R . . C21 C 0.65266(19) 0.08406(16) 0.79105(17) 0.0386(6) Uani 1 1 d . . . H21A H 0.6939 0.1378 0.8016 0.046 Uiso 1 1 calc R . . H21B H 0.7001 0.0379 0.7849 0.046 Uiso 1 1 calc R . . N10 N 0.54976(15) 0.08845(12) 0.68820(14) 0.0318(5) Uani 1 1 d . . . C22 C 0.55473(19) 0.11600(13) 0.59841(18) 0.0293(6) Uani 1 1 d . . . C23 C 0.65486(19) 0.14671(15) 0.58485(18) 0.0383(6) Uani 1 1 d . . . H23A H 0.6853 0.1960 0.6325 0.046 Uiso 1 1 calc R . . H23B H 0.6345 0.1626 0.5075 0.046 Uiso 1 1 calc R . . H23C H 0.7104 0.1017 0.6057 0.046 Uiso 1 1 calc R . . N30 N 0.08464(16) -0.05379(13) 0.26843(16) 0.0409(5) Uani 1 1 d . . . C30 C 0.0712(2) -0.11804(17) 0.22196(19) 0.0350(6) Uani 1 1 d . . . O30 O 0.05776(16) -0.18486(11) 0.17291(14) 0.0590(6) Uani 1 1 d . . . N40 N 0.41355(16) -0.06980(13) 0.73030(15) 0.0407(5) Uani 1 1 d . . . C40 C 0.4271(2) -0.13627(17) 0.76899(19) 0.0373(6) Uani 1 1 d . . . O40 O 0.44194(16) -0.20630(12) 0.80961(16) 0.0682(6) 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 0.0274(2) 0.0350(2) 0.02409(18) -0.00140(14) 0.00791(15) -0.00103(16) Co2 0.0304(2) 0.0332(2) 0.02294(17) 0.00150(14) 0.00723(15) -0.00074(16) N1 0.0329(13) 0.0591(14) 0.0227(11) 0.0067(10) 0.0042(10) -0.0125(11) N2 0.0306(13) 0.0581(14) 0.0238(11) 0.0082(10) 0.0015(10) -0.0120(11) C3 0.0290(16) 0.0303(14) 0.0268(13) -0.0023(10) 0.0101(11) -0.0030(11) N3 0.0284(13) 0.0395(13) 0.0271(11) -0.0011(9) 0.0116(10) -0.0014(10) C5 0.0305(16) 0.0402(15) 0.0239(13) 0.0004(11) 0.0112(12) 0.0002(12) C6 0.0355(17) 0.0330(15) 0.0239(13) -0.0033(10) 0.0133(12) 0.0017(12) C7 0.0441(18) 0.0537(17) 0.0262(13) 0.0017(12) 0.0173(12) 0.0014(13) N4 0.0328(14) 0.0371(12) 0.0207(10) -0.0009(8) 0.0070(9) 0.0011(10) C8 0.0351(17) 0.0522(17) 0.0195(13) 0.0000(11) 0.0069(11) -0.0001(13) C9 0.0328(16) 0.0499(17) 0.0251(13) -0.0001(11) 0.0048(11) -0.0021(13) C10 0.0313(16) 0.0469(16) 0.0286(13) 0.0036(12) 0.0055(11) 0.0040(12) C11 0.0260(15) 0.0520(17) 0.0283(13) 0.0024(12) 0.0052(11) 0.0039(12) N5 0.0278(12) 0.0345(12) 0.0248(11) 0.0015(8) 0.0084(9) 0.0000(9) C12 0.0307(16) 0.0250(13) 0.0282(13) 0.0010(10) 0.0116(11) -0.0029(11) C13 0.0292(16) 0.0400(16) 0.0331(14) -0.0034(11) 0.0121(12) -0.0009(12) C14 0.0263(15) 0.0319(14) 0.0245(13) 0.0000(10) 0.0105(11) -0.0013(11) N6 0.0285(12) 0.0422(13) 0.0231(10) -0.0037(9) 0.0049(9) 0.0049(10) N7 0.0329(13) 0.0417(13) 0.0224(10) -0.0047(9) 0.0074(9) 0.0032(10) C15 0.0318(16) 0.0369(15) 0.0223(13) -0.0004(10) 0.0121(11) -0.0037(12) N8 0.0312(14) 0.0417(13) 0.0243(11) -0.0011(9) 0.0124(10) -0.0019(10) C16 0.0359(17) 0.0356(15) 0.0234(13) 0.0030(10) 0.0118(12) -0.0027(12) C17 0.0435(18) 0.0643(19) 0.0275(14) -0.0064(12) 0.0176(13) -0.0047(14) N9 0.0344(14) 0.0359(12) 0.0197(10) 0.0019(8) 0.0056(9) -0.0008(10) C18 0.0420(18) 0.0512(17) 0.0212(13) -0.0035(11) 0.0037(12) 0.0045(14) C19 0.0409(18) 0.0526(18) 0.0330(15) -0.0142(12) -0.0004(13) -0.0057(14) C20 0.0352(16) 0.0517(18) 0.0287(14) 0.0001(12) -0.0024(12) -0.0032(13) C21 0.0287(16) 0.0495(16) 0.0291(14) -0.0011(12) 0.0033(11) -0.0010(12) N10 0.0331(13) 0.0337(12) 0.0241(10) -0.0010(9) 0.0070(9) 0.0006(9) C22 0.0259(15) 0.0265(14) 0.0322(14) -0.0016(10) 0.0086(11) 0.0020(11) C23 0.0283(16) 0.0462(16) 0.0387(15) 0.0047(12) 0.0120(12) 0.0019(12) N30 0.0406(14) 0.0397(14) 0.0442(13) -0.0039(11) 0.0192(11) -0.0014(11) C30 0.0325(17) 0.0453(18) 0.0274(14) 0.0092(13) 0.0125(12) 0.0052(13) O30 0.0868(17) 0.0403(12) 0.0455(11) -0.0116(9) 0.0228(11) 0.0040(10) N40 0.0391(14) 0.0361(13) 0.0426(13) 0.0057(10) 0.0125(10) 0.0017(11) C40 0.0345(17) 0.0421(18) 0.0332(15) -0.0025(13) 0.0117(12) -0.0026(13) O40 0.0861(17) 0.0409(13) 0.0804(15) 0.0207(11) 0.0372(12) 0.0037(11) _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 N30 1.958(2) . y Co1 N1 2.052(2) . y Co1 N6 2.1036(18) . y Co1 N5 2.1351(19) . y Co1 N4 2.2186(18) . y Co2 N40 1.965(2) . y Co2 N2 2.0580(19) . y Co2 N7 2.111(2) . y Co2 N10 2.167(2) . y Co2 N9 2.1686(19) . y N1 C5 1.340(3) . ? N1 N2 1.372(2) . ? N2 C3 1.335(3) . ? C3 N3 1.355(3) . ? C3 C22 1.479(3) . ? N3 C5 1.349(3) . ? C5 C6 1.481(3) . ? C6 N4 1.288(3) . ? C6 C7 1.501(3) . ? N4 C8 1.485(3) . ? C8 C9 1.505(3) . ? C9 C10 1.536(3) . ? C10 C11 1.537(3) . ? C11 N5 1.484(3) . ? N5 C12 1.297(2) . ? C12 C14 1.485(3) . ? C12 C13 1.496(3) . ? C14 N6 1.339(3) . ? C14 N8 1.349(2) . ? N6 N7 1.367(2) . ? N7 C15 1.342(3) . ? C15 N8 1.360(3) . ? C15 C16 1.475(3) . ? C16 N9 1.291(3) . ? C16 C17 1.497(3) . ? N9 C18 1.484(3) . ? C18 C19 1.523(3) . ? C19 C20 1.528(3) . ? C20 C21 1.529(3) . ? C21 N10 1.483(3) . ? N10 C22 1.295(3) . ? C22 C23 1.495(3) . ? N30 C30 1.165(3) . y C30 O30 1.216(3) . y N40 C40 1.152(3) . y C40 O40 1.213(3) . y 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 N30 Co1 N1 110.29(8) . . y N30 Co1 N6 116.68(8) . . y N1 Co1 N6 84.69(7) . . y N30 Co1 N5 108.60(8) . . y N1 Co1 N5 141.11(8) . . y N6 Co1 N5 78.07(7) . . y N30 Co1 N4 93.73(7) . . y N1 Co1 N4 75.86(7) . . y N6 Co1 N4 148.26(7) . . y N5 Co1 N4 101.71(7) . . y N40 Co2 N2 124.44(8) . . y N40 Co2 N7 102.56(8) . . y N2 Co2 N7 84.29(7) . . y N40 Co2 N10 104.55(8) . . y N2 Co2 N10 76.85(7) . . y N7 Co2 N10 152.53(7) . . y N40 Co2 N9 98.79(8) . . y N2 Co2 N9 135.85(8) . . y N7 Co2 N9 77.34(7) . . y N10 Co2 N9 102.61(7) . . y C5 N1 N2 105.39(19) . . ? C5 N1 Co1 117.29(15) . . ? N2 N1 Co1 137.16(15) . . ? C3 N2 N1 105.56(18) . . ? C3 N2 Co2 115.55(15) . . ? N1 N2 Co2 137.10(16) . . ? N2 C3 N3 114.03(19) . . ? N2 C3 C22 116.9(2) . . ? N3 C3 C22 129.1(2) . . ? C5 N3 C3 100.95(18) . . ? N1 C5 N3 114.07(19) . . ? N1 C5 C6 117.0(2) . . ? N3 C5 C6 128.9(2) . . ? N4 C6 C5 114.6(2) . . ? N4 C6 C7 127.5(2) . . ? C5 C6 C7 117.8(2) . . ? C6 N4 C8 117.99(19) . . ? C6 N4 Co1 115.03(14) . . ? C8 N4 Co1 126.18(15) . . ? N4 C8 C9 111.51(18) . . ? C8 C9 C10 113.7(2) . . ? C9 C10 C11 115.5(2) . . ? N5 C11 C10 111.59(19) . . ? C12 N5 C11 118.79(19) . . ? C12 N5 Co1 114.71(15) . . ? C11 N5 Co1 126.47(14) . . ? N5 C12 C14 114.7(2) . . ? N5 C12 C13 127.8(2) . . ? C14 C12 C13 117.51(19) . . ? N6 C14 N8 114.73(19) . . ? N6 C14 C12 117.76(19) . . ? N8 C14 C12 127.3(2) . . ? C14 N6 N7 105.32(17) . . ? C14 N6 Co1 111.03(14) . . ? N7 N6 Co1 135.12(15) . . ? C15 N7 N6 105.54(19) . . ? C15 N7 Co2 112.45(15) . . ? N6 N7 Co2 136.48(14) . . ? N7 C15 N8 114.04(19) . . ? N7 C15 C16 118.2(2) . . ? N8 C15 C16 127.6(2) . . ? C14 N8 C15 100.36(18) . . ? N9 C16 C15 115.1(2) . . ? N9 C16 C17 127.4(2) . . ? C15 C16 C17 117.5(2) . . ? C16 N9 C18 118.69(19) . . ? C16 N9 Co2 114.83(14) . . ? C18 N9 Co2 125.87(16) . . ? N9 C18 C19 112.22(19) . . ? C18 C19 C20 116.0(2) . . ? C19 C20 C21 112.7(2) . . ? N10 C21 C20 110.1(2) . . ? C22 N10 C21 119.0(2) . . ? C22 N10 Co2 115.09(15) . . ? C21 N10 Co2 125.80(14) . . ? N10 C22 C3 114.6(2) . . ? N10 C22 C23 127.2(2) . . ? C3 C22 C23 118.2(2) . . ? C30 N30 Co1 177.3(2) . . y N30 C30 O30 179.4(3) . . y C40 N40 Co2 177.4(2) . . y N40 C40 O40 179.6(3) . . y 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 N30 Co1 N1 C5 90.91(19) . . . . ? N6 Co1 N1 C5 -152.57(19) . . . . ? N5 Co1 N1 C5 -89.1(2) . . . . ? N4 Co1 N1 C5 2.15(17) . . . . ? N30 Co1 N1 N2 -94.6(2) . . . . ? N6 Co1 N1 N2 22.0(2) . . . . ? N5 Co1 N1 N2 85.5(3) . . . . ? N4 Co1 N1 N2 176.7(3) . . . . ? C5 N1 N2 C3 0.6(3) . . . . ? Co1 N1 N2 C3 -174.40(19) . . . . ? C5 N1 N2 Co2 163.74(19) . . . . ? Co1 N1 N2 Co2 -11.2(4) . . . . ? N40 Co2 N2 C3 -107.14(18) . . . . ? N7 Co2 N2 C3 151.53(18) . . . . ? N10 Co2 N2 C3 -8.36(17) . . . . ? N9 Co2 N2 C3 86.3(2) . . . . ? N40 Co2 N2 N1 90.9(3) . . . . ? N7 Co2 N2 N1 -10.5(2) . . . . ? N10 Co2 N2 N1 -170.4(3) . . . . ? N9 Co2 N2 N1 -75.7(3) . . . . ? N1 N2 C3 N3 -0.3(3) . . . . ? Co2 N2 C3 N3 -167.64(15) . . . . ? N1 N2 C3 C22 179.36(19) . . . . ? Co2 N2 C3 C22 12.0(3) . . . . ? N2 C3 N3 C5 -0.2(3) . . . . ? C22 C3 N3 C5 -179.7(2) . . . . ? N2 N1 C5 N3 -0.7(3) . . . . ? Co1 N1 C5 N3 175.41(15) . . . . ? N2 N1 C5 C6 179.27(19) . . . . ? Co1 N1 C5 C6 -4.6(3) . . . . ? C3 N3 C5 N1 0.6(3) . . . . ? C3 N3 C5 C6 -179.4(2) . . . . ? N1 C5 C6 N4 5.2(3) . . . . ? N3 C5 C6 N4 -174.8(2) . . . . ? N1 C5 C6 C7 -171.0(2) . . . . ? N3 C5 C6 C7 9.0(4) . . . . ? C5 C6 N4 C8 -173.59(18) . . . . ? C7 C6 N4 C8 2.1(3) . . . . ? C5 C6 N4 Co1 -3.2(2) . . . . ? C7 C6 N4 Co1 172.49(18) . . . . ? N30 Co1 N4 C6 -109.22(17) . . . . ? N1 Co1 N4 C6 0.77(16) . . . . ? N6 Co1 N4 C6 54.7(2) . . . . ? N5 Co1 N4 C6 140.90(16) . . . . ? N30 Co1 N4 C8 60.24(18) . . . . ? N1 Co1 N4 C8 170.23(19) . . . . ? N6 Co1 N4 C8 -135.84(18) . . . . ? N5 Co1 N4 C8 -49.64(18) . . . . ? C6 N4 C8 C9 -178.4(2) . . . . ? Co1 N4 C8 C9 12.5(3) . . . . ? N4 C8 C9 C10 67.7(3) . . . . ? C8 C9 C10 C11 -121.2(2) . . . . ? C9 C10 C11 N5 76.1(2) . . . . ? C10 C11 N5 C12 138.0(2) . . . . ? C10 C11 N5 Co1 -44.1(3) . . . . ? N30 Co1 N5 C12 122.28(16) . . . . ? N1 Co1 N5 C12 -57.8(2) . . . . ? N6 Co1 N5 C12 7.87(15) . . . . ? N4 Co1 N5 C12 -139.68(15) . . . . ? N30 Co1 N5 C11 -55.68(19) . . . . ? N1 Co1 N5 C11 124.29(18) . . . . ? N6 Co1 N5 C11 -170.08(19) . . . . ? N4 Co1 N5 C11 42.36(18) . . . . ? C11 N5 C12 C14 179.18(18) . . . . ? Co1 N5 C12 C14 1.1(2) . . . . ? C11 N5 C12 C13 -1.4(3) . . . . ? Co1 N5 C12 C13 -179.50(18) . . . . ? N5 C12 C14 N6 -16.0(3) . . . . ? C13 C12 C14 N6 164.5(2) . . . . ? N5 C12 C14 N8 159.0(2) . . . . ? C13 C12 C14 N8 -20.5(3) . . . . ? N8 C14 N6 N7 -0.4(3) . . . . ? C12 C14 N6 N7 175.17(18) . . . . ? N8 C14 N6 Co1 -153.59(15) . . . . ? C12 C14 N6 Co1 22.0(2) . . . . ? N30 Co1 N6 C14 -120.79(16) . . . . ? N1 Co1 N6 C14 129.15(17) . . . . ? N5 Co1 N6 C14 -15.80(15) . . . . ? N4 Co1 N6 C14 77.2(2) . . . . ? N30 Co1 N6 N7 97.3(2) . . . . ? N1 Co1 N6 N7 -12.8(2) . . . . ? N5 Co1 N6 N7 -157.7(2) . . . . ? N4 Co1 N6 N7 -64.7(3) . . . . ? C14 N6 N7 C15 -0.3(2) . . . . ? Co1 N6 N7 C15 143.03(18) . . . . ? C14 N6 N7 Co2 -150.59(17) . . . . ? Co1 N6 N7 Co2 -7.2(3) . . . . ? N40 Co2 N7 C15 105.94(16) . . . . ? N2 Co2 N7 C15 -130.00(16) . . . . ? N10 Co2 N7 C15 -83.5(2) . . . . ? N9 Co2 N7 C15 9.60(15) . . . . ? N40 Co2 N7 N6 -105.2(2) . . . . ? N2 Co2 N7 N6 18.9(2) . . . . ? N10 Co2 N7 N6 65.4(3) . . . . ? N9 Co2 N7 N6 158.5(2) . . . . ? N6 N7 C15 N8 1.0(3) . . . . ? Co2 N7 C15 N8 159.28(15) . . . . ? N6 N7 C15 C16 -174.76(19) . . . . ? Co2 N7 C15 C16 -16.4(2) . . . . ? N6 C14 N8 C15 0.9(2) . . . . ? C12 C14 N8 C15 -174.2(2) . . . . ? N7 C15 N8 C14 -1.1(2) . . . . ? C16 C15 N8 C14 174.1(2) . . . . ? N7 C15 C16 N9 15.6(3) . . . . ? N8 C15 C16 N9 -159.4(2) . . . . ? N7 C15 C16 C17 -163.1(2) . . . . ? N8 C15 C16 C17 21.8(3) . . . . ? C15 C16 N9 C18 -177.88(19) . . . . ? C17 C16 N9 C18 0.7(4) . . . . ? C15 C16 N9 Co2 -6.3(3) . . . . ? C17 C16 N9 Co2 172.31(19) . . . . ? N40 Co2 N9 C16 -102.49(17) . . . . ? N2 Co2 N9 C16 66.3(2) . . . . ? N7 Co2 N9 C16 -1.49(16) . . . . ? N10 Co2 N9 C16 150.35(16) . . . . ? N40 Co2 N9 C18 68.37(18) . . . . ? N2 Co2 N9 C18 -122.82(18) . . . . ? N7 Co2 N9 C18 169.37(19) . . . . ? N10 Co2 N9 C18 -38.79(19) . . . . ? C16 N9 C18 C19 -152.1(2) . . . . ? Co2 N9 C18 C19 37.4(3) . . . . ? N9 C18 C19 C20 -73.3(3) . . . . ? C18 C19 C20 C21 123.4(2) . . . . ? C19 C20 C21 N10 -67.4(3) . . . . ? C20 C21 N10 C22 168.1(2) . . . . ? C20 C21 N10 Co2 -15.8(3) . . . . ? N40 Co2 N10 C22 126.21(16) . . . . ? N2 Co2 N10 C22 3.56(16) . . . . ? N7 Co2 N10 C22 -44.3(2) . . . . ? N9 Co2 N10 C22 -131.09(16) . . . . ? N40 Co2 N10 C21 -49.97(19) . . . . ? N2 Co2 N10 C21 -172.62(19) . . . . ? N7 Co2 N10 C21 139.49(18) . . . . ? N9 Co2 N10 C21 52.73(19) . . . . ? C21 N10 C22 C3 177.84(19) . . . . ? Co2 N10 C22 C3 1.4(2) . . . . ? C21 N10 C22 C23 -1.2(3) . . . . ? Co2 N10 C22 C23 -177.68(18) . . . . ? N2 C3 C22 N10 -8.8(3) . . . . ? N3 C3 C22 N10 170.8(2) . . . . ? N2 C3 C22 C23 170.4(2) . . . . ? N3 C3 C22 C23 -10.1(3) . . . . ? N1 Co1 N30 C30 -57(5) . . . . ? N6 Co1 N30 C30 -151(5) . . . . ? N5 Co1 N30 C30 123(5) . . . . ? N4 Co1 N30 C30 20(5) . . . . ? Co1 N30 C30 O30 5(39) . . . . ? N2 Co2 N40 C40 -159(5) . . . . ? N7 Co2 N40 C40 -67(5) . . . . ? N10 Co2 N40 C40 117(5) . . . . ? N9 Co2 N40 C40 12(5) . . . . ? Co2 N40 C40 O40 -140(48) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.243 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.073 data_cobclcc _database_code_CSD 197089 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H32.50 Cl2 Co2 N11.50' _chemical_formula_weight 658.86 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 20.250(4) _cell_length_b 20.406(4) _cell_length_c 14.364(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.466(3) _cell_angle_gamma 90.00 _cell_volume 5662(2) _cell_formula_units_Z 8 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 1.397 _exptl_absorpt_correction_type Semi-empirical(SADABS) _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 'Bruker SMART area detector ' _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 36288 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 26.39 _reflns_number_total 9372 _reflns_number_gt 8967 _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^)+(0.0289P)^2^+2.6679P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.182(8) _refine_ls_number_reflns 9372 _refine_ls_number_parameters 734 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0536 _refine_ls_wR_factor_gt 0.0528 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.772690(16) 0.369950(14) 0.10355(2) 0.02045(7) Uani 1 1 d . . . Co2 Co 0.634436(16) 0.528925(14) 0.10309(2) 0.02149(7) Uani 1 1 d . . . Cl1 Cl 0.76795(3) 0.34720(3) -0.05810(4) 0.02851(13) Uani 1 1 d . . . Cl2 Cl 0.57790(3) 0.55882(3) -0.05376(4) 0.03023(13) Uani 1 1 d . . . N1 N 0.78025(10) 0.47090(8) 0.10911(15) 0.0215(4) Uani 1 1 d . . . N2 N 0.73702(11) 0.52041(9) 0.11360(15) 0.0214(4) Uani 1 1 d . . . C3 C 0.77796(13) 0.57204(10) 0.15026(17) 0.0212(5) Uani 1 1 d . . . N3 N 0.84550(10) 0.55959(9) 0.16939(15) 0.0242(4) Uani 1 1 d . . . C5 C 0.84396(12) 0.49558(11) 0.14326(16) 0.0208(5) Uani 1 1 d . . . C6 C 0.90147(12) 0.44837(11) 0.16358(16) 0.0217(5) Uani 1 1 d . . . C7 C 0.97400(13) 0.47450(12) 0.18887(19) 0.0297(5) Uani 1 1 d . . . H7A H 0.9988 0.4639 0.2570 0.036 Uiso 1 1 calc R . . H7B H 0.9726 0.5222 0.1802 0.036 Uiso 1 1 calc R . . H7C H 0.9980 0.4545 0.1460 0.036 Uiso 1 1 calc R . . N4 N 0.88342(10) 0.38769(9) 0.16158(14) 0.0231(4) Uani 1 1 d . . . C8 C 0.93842(13) 0.33772(12) 0.19600(19) 0.0308(5) Uani 1 1 d . . . H8A H 0.9762 0.3557 0.2510 0.037 Uiso 1 1 calc R . . H8B H 0.9580 0.3266 0.1426 0.037 Uiso 1 1 calc R . . C9 C 0.90916(14) 0.27603(13) 0.2291(2) 0.0329(6) Uani 1 1 d . . . H9A H 0.8807 0.2890 0.2714 0.039 Uiso 1 1 calc R . . H9B H 0.9481 0.2491 0.2689 0.039 Uiso 1 1 calc R . . C10 C 0.86437(15) 0.23359(12) 0.1444(2) 0.0349(6) Uani 1 1 d . . . H10A H 0.8569 0.2580 0.0825 0.042 Uiso 1 1 calc R . . H10B H 0.8902 0.1931 0.1400 0.042 Uiso 1 1 calc R . . C11 C 0.79526(14) 0.21489(11) 0.15465(19) 0.0315(6) Uani 1 1 d . . . H11A H 0.7736 0.1812 0.1054 0.038 Uiso 1 1 calc R . . H11B H 0.8017 0.1959 0.2202 0.038 Uiso 1 1 calc R . . N5 N 0.74898(11) 0.27292(9) 0.14124(14) 0.0232(4) Uani 1 1 d . . . C12 C 0.68814(13) 0.26497(11) 0.14744(16) 0.0231(5) Uani 1 1 d . . . C13 C 0.65785(15) 0.20165(12) 0.1706(2) 0.0339(6) Uani 1 1 d . . . H13A H 0.6482 0.1723 0.1141 0.041 Uiso 1 1 calc R . . H13B H 0.6148 0.2109 0.1860 0.041 Uiso 1 1 calc R . . H13C H 0.6909 0.1807 0.2269 0.041 Uiso 1 1 calc R . . N6 N 0.67024(11) 0.37738(9) 0.09720(16) 0.0228(4) Uani 1 1 d . . . N7 N 0.62839(11) 0.42780(9) 0.10365(16) 0.0239(4) Uani 1 1 d . . . C14 C 0.64532(12) 0.32493(11) 0.13192(16) 0.0221(5) Uani 1 1 d . . . N8 N 0.58871(11) 0.33740(9) 0.15924(15) 0.0252(4) Uani 1 1 d . . . C15 C 0.58143(12) 0.40243(11) 0.14162(17) 0.0226(5) Uani 1 1 d . . . C16 C 0.53583(12) 0.44872(12) 0.17078(17) 0.0245(5) Uani 1 1 d . . . C17 C 0.47532(13) 0.42175(13) 0.19770(19) 0.0316(5) Uani 1 1 d . . . H17A H 0.4885 0.4147 0.2684 0.038 Uiso 1 1 calc R . . H17B H 0.4611 0.3800 0.1639 0.038 Uiso 1 1 calc R . . H17C H 0.4368 0.4529 0.1785 0.038 Uiso 1 1 calc R . . N9 N 0.55482(11) 0.50921(10) 0.17322(14) 0.0256(4) Uani 1 1 d . . . C18 C 0.51595(14) 0.55772(12) 0.2144(2) 0.0333(6) Uani 1 1 d . . . H18A H 0.5042 0.5378 0.2702 0.040 Uiso 1 1 calc R . . H18B H 0.4721 0.5692 0.1641 0.040 Uiso 1 1 calc R . . C19 C 0.55803(15) 0.61942(12) 0.2481(2) 0.0337(6) Uani 1 1 d . . . H19A H 0.6049 0.6067 0.2891 0.040 Uiso 1 1 calc R . . H19B H 0.5362 0.6449 0.2896 0.040 Uiso 1 1 calc R . . C20 C 0.56518(14) 0.66391(12) 0.16513(19) 0.0333(6) Uani 1 1 d . . . H20A H 0.5448 0.6413 0.1021 0.040 Uiso 1 1 calc R . . H20B H 0.5383 0.7046 0.1644 0.040 Uiso 1 1 calc R . . C21 C 0.63851(14) 0.68185(12) 0.1742(2) 0.0321(6) Uani 1 1 d . . . H21A H 0.6391 0.7158 0.1252 0.039 Uiso 1 1 calc R . . H21B H 0.6608 0.7004 0.2398 0.039 Uiso 1 1 calc R . . N10 N 0.67815(11) 0.62408(9) 0.15911(15) 0.0238(4) Uani 1 1 d . . . C22 C 0.74282(13) 0.63159(11) 0.16945(16) 0.0218(5) Uani 1 1 d . . . C23 C 0.78367(14) 0.69376(12) 0.19902(19) 0.0307(6) Uani 1 1 d . . . H23A H 0.7592 0.7301 0.1585 0.037 Uiso 1 1 calc R . . H23B H 0.8295 0.6885 0.1901 0.037 Uiso 1 1 calc R . . H23C H 0.7889 0.7032 0.2678 0.037 Uiso 1 1 calc R . . Co3 Co 0.265739(16) 0.519677(14) -0.00664(2) 0.02185(7) Uani 1 1 d . . . Co4 Co 0.104474(16) 0.381442(14) -0.01704(2) 0.02010(7) Uani 1 1 d . . . Cl3 Cl 0.32346(3) 0.54576(3) 0.15235(4) 0.02990(13) Uani 1 1 d . . . Cl4 Cl 0.11158(3) 0.35388(3) 0.14361(4) 0.02961(13) Uani 1 1 d . . . N31 N 0.25503(10) 0.41957(9) -0.01720(15) 0.0232(4) Uani 1 1 d . . . N32 N 0.20608(11) 0.37545(9) -0.01520(16) 0.0234(4) Uani 1 1 d . . . C33 C 0.22358(12) 0.31965(11) -0.05041(17) 0.0230(5) Uani 1 1 d . . . N33 N 0.28241(11) 0.32393(9) -0.07511(15) 0.0263(4) Uani 1 1 d . . . C35 C 0.29929(12) 0.38730(11) -0.05397(17) 0.0222(5) Uani 1 1 d . . . C36 C 0.35601(12) 0.42652(12) -0.07013(17) 0.0251(5) Uani 1 1 d . . . C37 C 0.41233(14) 0.39189(13) -0.0978(2) 0.0330(6) Uani 1 1 d . . . H37A H 0.4091 0.4023 -0.1657 0.040 Uiso 1 1 calc R . . H37B H 0.4075 0.3445 -0.0911 0.040 Uiso 1 1 calc R . . H37C H 0.4574 0.4061 -0.0549 0.040 Uiso 1 1 calc R . . N34 N 0.35077(11) 0.48855(10) -0.05831(15) 0.0256(4) Uani 1 1 d . . . C38 C 0.40639(14) 0.53179(13) -0.0703(2) 0.0335(6) Uani 1 1 d . . . H38A H 0.4135 0.5233 -0.1344 0.040 Uiso 1 1 calc R . . H38B H 0.4502 0.5217 -0.0189 0.040 Uiso 1 1 calc R . . C39 C 0.38849(14) 0.60296(12) -0.06373(19) 0.0335(6) Uani 1 1 d . . . H39A H 0.4298 0.6299 -0.0603 0.040 Uiso 1 1 calc R . . H39B H 0.3764 0.6100 -0.0026 0.040 Uiso 1 1 calc R . . C40 C 0.32797(15) 0.62650(13) -0.1504(2) 0.0348(6) Uani 1 1 d . . . H40A H 0.3462 0.6565 -0.1908 0.042 Uiso 1 1 calc R . . H40B H 0.3077 0.5882 -0.1912 0.042 Uiso 1 1 calc R . . C41 C 0.27116(14) 0.66138(12) -0.12105(19) 0.0316(6) Uani 1 1 d . . . H41A H 0.2919 0.6953 -0.0717 0.038 Uiso 1 1 calc R . . H41B H 0.2396 0.6834 -0.1788 0.038 Uiso 1 1 calc R . . N35 N 0.23119(11) 0.61463(9) -0.08029(14) 0.0251(4) Uani 1 1 d . . . C42 C 0.17039(13) 0.63262(11) -0.08043(17) 0.0229(5) Uani 1 1 d . . . C43 C 0.13725(14) 0.69831(11) -0.11087(18) 0.0290(5) Uani 1 1 d . . . H43A H 0.1703 0.7331 -0.0816 0.035 Uiso 1 1 calc R . . H43B H 0.0961 0.7026 -0.0887 0.035 Uiso 1 1 calc R . . H43C H 0.1237 0.7020 -0.1821 0.035 Uiso 1 1 calc R . . N37 N 0.11307(10) 0.48270(9) -0.00940(15) 0.0210(4) Uani 1 1 d . . . C44 C 0.12950(12) 0.58079(10) -0.05223(16) 0.0205(5) Uani 1 1 d . . . N38 N 0.06026(10) 0.57743(9) -0.07068(14) 0.0227(4) Uani 1 1 d . . . C45 C 0.05347(12) 0.51482(11) -0.04460(16) 0.0207(5) Uani 1 1 d . . . C46 C -0.01031(13) 0.47595(11) -0.06204(16) 0.0221(5) Uani 1 1 d . . . C47 C -0.07817(13) 0.51091(13) -0.08489(19) 0.0303(5) Uani 1 1 d . . . H47A H -0.1109 0.4911 -0.1426 0.036 Uiso 1 1 calc R . . H47B H -0.0716 0.5572 -0.0978 0.036 Uiso 1 1 calc R . . H47C H -0.0965 0.5073 -0.0292 0.036 Uiso 1 1 calc R . . N39 N -0.00114(10) 0.41319(9) -0.05752(14) 0.0214(4) Uani 1 1 d . . . C48 C -0.06219(13) 0.37083(11) -0.07217(19) 0.0277(5) Uani 1 1 d . . . H48A H -0.0944 0.3781 -0.1384 0.033 Uiso 1 1 calc R . . H48B H -0.0867 0.3826 -0.0243 0.033 Uiso 1 1 calc R . . C49 C -0.04147(13) 0.29858(11) -0.06002(18) 0.0294(5) Uani 1 1 d . . . H49A H -0.0821 0.2724 -0.0575 0.035 Uiso 1 1 calc R . . H49B H -0.0050 0.2929 0.0031 0.035 Uiso 1 1 calc R . . C50 C -0.01465(14) 0.27160(13) -0.1423(2) 0.0308(6) Uani 1 1 d . . . H50A H -0.0496 0.2412 -0.1829 0.037 Uiso 1 1 calc R . . H50B H -0.0096 0.3085 -0.1844 0.037 Uiso 1 1 calc R . . C51 C 0.05410(13) 0.23592(11) -0.10626(19) 0.0306(5) Uani 1 1 d . . . H51A H 0.0535 0.2062 -0.0520 0.037 Uiso 1 1 calc R . . H51B H 0.0614 0.2091 -0.1597 0.037 Uiso 1 1 calc R . . N40 N 0.11123(10) 0.28361(9) -0.07228(14) 0.0233(4) Uani 1 1 d . . . C52 C 0.17185(13) 0.26626(11) -0.07240(17) 0.0239(5) Uani 1 1 d . . . C53 C 0.19429(15) 0.19975(11) -0.0958(2) 0.0328(6) Uani 1 1 d . . . H53A H 0.1852 0.1673 -0.0509 0.039 Uiso 1 1 calc R . . H53B H 0.2439 0.2005 -0.0889 0.039 Uiso 1 1 calc R . . H53C H 0.1684 0.1880 -0.1631 0.039 Uiso 1 1 calc R . . N36 N 0.16243(11) 0.52557(9) -0.01462(15) 0.0214(4) Uani 1 1 d . . . N100 N 0.78194(14) 0.39588(12) 0.2867(2) 0.0460(6) Uani 1 1 d D . . C100 C 0.75761(14) 0.43465(13) 0.32340(19) 0.0321(6) Uani 1 1 d D . . C101 C 0.7248(2) 0.48550(18) 0.3652(3) 0.0570(10) Uani 1 1 d D . . H10C H 0.7541 0.5247 0.3780 0.068 Uiso 1 1 calc R . . H10D H 0.7187 0.4697 0.4265 0.068 Uiso 1 1 calc R . . H10E H 0.6796 0.4963 0.3193 0.068 Uiso 1 1 calc R . . N110 N 0.09470(13) 0.41111(12) -0.1974(2) 0.0425(6) Uani 1 1 d . . . C110 C 0.12794(15) 0.44287(13) -0.2305(2) 0.0328(6) Uani 1 1 d . . . C111 C 0.17401(18) 0.48384(15) -0.2673(2) 0.0448(7) Uani 1 1 d . . . H11C H 0.2090 0.5040 -0.2123 0.054 Uiso 1 1 calc R . . H11D H 0.1469 0.5182 -0.3096 0.054 Uiso 1 1 calc R . . H11E H 0.1969 0.4567 -0.3048 0.054 Uiso 1 1 calc R . . N120 N 0.4999(4) 0.2405(4) -0.0260(7) 0.122(3) Uani 0.58 1 d PD A 1 C120 C 0.4631(5) 0.2157(4) 0.0098(7) 0.085(3) Uani 0.58 1 d PD A 1 C121 C 0.4042(6) 0.1806(5) 0.0228(8) 0.106(3) Uani 0.58 1 d PD A 1 H12A H 0.3819 0.1552 -0.0361 0.127 Uiso 0.58 1 calc PR A 1 H12B H 0.3710 0.2120 0.0346 0.127 Uiso 0.58 1 calc PR A 1 H12C H 0.4200 0.1510 0.0788 0.127 Uiso 0.58 1 calc PR A 1 N130 N 0.4088(6) 0.2737(5) 0.1114(8) 0.124(5) Uani 0.42 1 d PD B 2 C130 C 0.4253(7) 0.2272(6) 0.0754(8) 0.080(3) Uani 0.42 1 d PD B 2 C131 C 0.4638(9) 0.1670(6) 0.0773(13) 0.118(6) Uani 0.42 1 d PD B 2 H13D H 0.4729 0.1462 0.1414 0.142 Uiso 0.42 1 calc PR B 2 H13E H 0.5078 0.1770 0.0652 0.142 Uiso 0.42 1 calc PR B 2 H13F H 0.4367 0.1372 0.0267 0.142 Uiso 0.42 1 calc PR B 2 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 0.02009(16) 0.01801(14) 0.02481(16) -0.00027(12) 0.00912(12) 0.00094(12) Co2 0.01910(16) 0.02010(14) 0.02637(17) 0.00074(12) 0.00849(13) 0.00261(12) Cl1 0.0305(3) 0.0315(3) 0.0262(3) -0.0051(2) 0.0125(2) -0.0030(2) Cl2 0.0250(3) 0.0355(3) 0.0284(3) 0.0051(2) 0.0052(2) 0.0005(2) N1 0.0188(11) 0.0199(9) 0.0266(11) -0.0025(8) 0.0080(8) 0.0023(7) N2 0.0192(10) 0.0187(9) 0.0269(11) -0.0020(7) 0.0079(8) 0.0010(7) C3 0.0237(12) 0.0197(10) 0.0214(11) -0.0010(8) 0.0083(9) -0.0009(9) N3 0.0223(10) 0.0235(10) 0.0278(10) -0.0033(8) 0.0090(8) -0.0021(8) C5 0.0201(12) 0.0227(11) 0.0202(11) -0.0029(8) 0.0071(9) -0.0021(9) C6 0.0184(12) 0.0277(12) 0.0203(11) -0.0032(9) 0.0078(9) 0.0006(9) C7 0.0198(12) 0.0369(13) 0.0317(13) -0.0032(10) 0.0067(10) -0.0026(10) N4 0.0199(10) 0.0272(10) 0.0228(9) -0.0011(8) 0.0075(8) 0.0057(8) C8 0.0220(13) 0.0309(12) 0.0376(14) -0.0001(10) 0.0063(10) 0.0096(10) C9 0.0287(14) 0.0337(13) 0.0350(15) 0.0054(11) 0.0074(11) 0.0104(11) C10 0.0384(16) 0.0272(12) 0.0418(14) -0.0022(10) 0.0162(12) 0.0097(11) C11 0.0370(15) 0.0177(11) 0.0404(14) 0.0014(10) 0.0128(12) 0.0072(10) N5 0.0283(11) 0.0187(9) 0.0225(10) -0.0008(7) 0.0078(8) 0.0040(8) C12 0.0316(13) 0.0192(10) 0.0196(11) -0.0029(8) 0.0094(10) -0.0038(9) C13 0.0419(16) 0.0221(12) 0.0413(15) 0.0011(10) 0.0178(12) -0.0043(11) N6 0.0221(11) 0.0189(9) 0.0296(11) 0.0002(8) 0.0110(9) 0.0003(7) N7 0.0205(10) 0.0219(9) 0.0328(11) 0.0019(8) 0.0135(9) 0.0036(8) C14 0.0235(13) 0.0201(11) 0.0246(12) -0.0011(8) 0.0099(10) -0.0041(9) N8 0.0226(11) 0.0255(10) 0.0298(11) -0.0006(8) 0.0112(8) -0.0033(8) C15 0.0185(12) 0.0257(11) 0.0233(11) -0.0011(9) 0.0061(9) -0.0018(9) C16 0.0196(12) 0.0323(13) 0.0213(11) 0.0030(9) 0.0056(9) 0.0027(10) C17 0.0229(13) 0.0403(14) 0.0352(14) 0.0013(11) 0.0142(11) 0.0028(11) N9 0.0262(11) 0.0274(10) 0.0259(10) 0.0019(8) 0.0116(8) 0.0054(8) C18 0.0327(14) 0.0336(13) 0.0420(15) 0.0023(11) 0.0242(12) 0.0086(11) C19 0.0379(16) 0.0328(13) 0.0359(15) -0.0049(11) 0.0192(12) 0.0082(11) C20 0.0339(15) 0.0284(13) 0.0389(14) -0.0014(10) 0.0130(12) 0.0110(11) C21 0.0350(15) 0.0222(12) 0.0404(14) -0.0033(10) 0.0130(11) 0.0085(10) N10 0.0271(12) 0.0197(9) 0.0246(10) -0.0021(7) 0.0080(9) 0.0047(8) C22 0.0284(13) 0.0203(10) 0.0175(10) 0.0006(8) 0.0083(9) -0.0003(9) C23 0.0350(15) 0.0234(12) 0.0359(13) -0.0051(10) 0.0138(11) -0.0053(10) Co3 0.01904(16) 0.02162(15) 0.02569(17) -0.00085(12) 0.00791(13) -0.00293(12) Co4 0.01805(15) 0.01838(14) 0.02533(16) 0.00012(11) 0.00871(12) -0.00034(11) Cl3 0.0270(3) 0.0320(3) 0.0280(3) -0.0045(2) 0.0041(2) 0.0008(2) Cl4 0.0369(3) 0.0271(3) 0.0273(3) 0.0050(2) 0.0135(3) 0.0023(2) N31 0.0179(10) 0.0237(9) 0.0292(11) -0.0031(8) 0.0088(8) -0.0009(8) N32 0.0219(11) 0.0202(9) 0.0309(12) -0.0007(8) 0.0123(9) -0.0016(8) C33 0.0226(12) 0.0221(11) 0.0260(12) 0.0021(9) 0.0099(9) 0.0019(9) N33 0.0253(11) 0.0252(10) 0.0305(11) 0.0008(8) 0.0119(9) 0.0037(8) C35 0.0189(12) 0.0253(11) 0.0240(12) 0.0018(9) 0.0089(9) 0.0025(9) C36 0.0170(12) 0.0338(13) 0.0242(12) 0.0005(9) 0.0055(9) 0.0013(9) C37 0.0253(14) 0.0401(14) 0.0382(14) 0.0035(11) 0.0167(11) 0.0036(11) N34 0.0181(10) 0.0326(11) 0.0276(10) 0.0009(8) 0.0092(8) -0.0043(8) C38 0.0231(14) 0.0387(14) 0.0428(15) 0.0033(11) 0.0159(11) -0.0071(11) C39 0.0278(14) 0.0341(13) 0.0401(14) -0.0003(11) 0.0125(11) -0.0112(11) C40 0.0342(15) 0.0382(14) 0.0356(15) 0.0060(11) 0.0157(12) -0.0106(12) C41 0.0308(14) 0.0289(12) 0.0366(13) 0.0065(10) 0.0121(11) -0.0090(11) N35 0.0252(11) 0.0257(10) 0.0241(10) 0.0026(8) 0.0068(8) -0.0058(8) C42 0.0286(13) 0.0199(11) 0.0193(11) 0.0002(8) 0.0058(10) -0.0042(9) C43 0.0360(14) 0.0218(11) 0.0292(12) 0.0019(9) 0.0098(11) -0.0011(10) N37 0.0185(10) 0.0207(9) 0.0242(10) 0.0025(8) 0.0069(8) -0.0013(7) C44 0.0218(12) 0.0190(10) 0.0197(11) -0.0008(8) 0.0048(9) -0.0010(9) N38 0.0231(11) 0.0215(9) 0.0232(10) 0.0010(7) 0.0064(8) 0.0015(8) C45 0.0196(12) 0.0243(11) 0.0198(11) 0.0002(8) 0.0082(9) 0.0003(9) C46 0.0200(12) 0.0283(12) 0.0198(11) 0.0038(9) 0.0087(9) 0.0024(9) C47 0.0221(13) 0.0352(13) 0.0346(13) 0.0029(10) 0.0097(10) 0.0048(10) N39 0.0175(10) 0.0265(10) 0.0218(9) 0.0018(8) 0.0081(7) -0.0030(8) C48 0.0192(12) 0.0301(12) 0.0349(13) 0.0011(10) 0.0097(10) -0.0045(10) C49 0.0245(13) 0.0298(12) 0.0365(13) 0.0007(10) 0.0132(11) -0.0063(10) C50 0.0257(13) 0.0328(13) 0.0336(14) -0.0046(10) 0.0084(11) -0.0101(10) C51 0.0313(14) 0.0240(11) 0.0391(14) -0.0045(10) 0.0145(11) -0.0075(10) N40 0.0256(11) 0.0220(9) 0.0246(10) -0.0011(7) 0.0110(8) -0.0030(8) C52 0.0295(13) 0.0195(10) 0.0246(12) 0.0002(9) 0.0111(10) -0.0012(9) C53 0.0365(15) 0.0221(11) 0.0438(15) -0.0034(10) 0.0183(12) 0.0029(10) N36 0.0203(11) 0.0184(9) 0.0256(11) 0.0008(7) 0.0072(8) -0.0028(7) N100 0.0433(16) 0.0318(12) 0.0714(19) -0.0038(12) 0.0299(14) -0.0065(11) C100 0.0297(14) 0.0396(14) 0.0285(14) 0.0024(11) 0.0110(11) -0.0119(12) C101 0.057(2) 0.068(2) 0.058(2) -0.0292(18) 0.0356(18) -0.0236(18) N110 0.0381(14) 0.0355(13) 0.0598(16) 0.0049(11) 0.0234(13) 0.0064(11) C110 0.0356(15) 0.0323(13) 0.0284(14) -0.0007(11) 0.0066(11) 0.0105(12) C111 0.056(2) 0.0458(16) 0.0376(17) 0.0120(13) 0.0222(15) 0.0065(14) N120 0.086(6) 0.139(8) 0.124(7) -0.025(6) 0.007(5) 0.043(6) C120 0.097(7) 0.087(6) 0.089(6) -0.014(5) 0.055(5) 0.004(5) C121 0.144(11) 0.090(7) 0.096(7) -0.002(6) 0.057(7) 0.023(7) N130 0.118(10) 0.125(9) 0.097(8) 0.014(7) -0.014(7) -0.051(8) C130 0.090(9) 0.081(8) 0.066(7) -0.003(6) 0.019(6) -0.012(7) C131 0.139(16) 0.110(11) 0.142(15) 0.013(9) 0.096(13) -0.016(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N6 2.055(2) . y Co1 N1 2.0654(18) . y Co1 N5 2.1448(19) . y Co1 N4 2.175(2) . y Co1 Cl1 2.3415(8) . y Co2 N2 2.044(2) . y Co2 N7 2.0674(19) . y Co2 N9 2.180(2) . y Co2 N10 2.185(2) . y Co2 Cl2 2.2827(8) . y N1 C5 1.334(3) . ? N1 N2 1.351(3) . ? N2 C3 1.346(3) . ? C3 N3 1.336(3) . ? C3 C22 1.475(3) . ? N3 C5 1.357(3) . ? C5 C6 1.472(3) . ? C6 N4 1.289(3) . ? C6 C7 1.501(3) . ? N4 C8 1.481(3) . ? C8 C9 1.527(4) . ? C9 C10 1.546(4) . ? C10 C11 1.500(4) . ? C11 N5 1.486(3) . ? N5 C12 1.272(3) . ? C12 C14 1.477(3) . ? C12 C13 1.510(3) . ? N6 C14 1.342(3) . ? N6 N7 1.354(3) . ? N7 C15 1.335(3) . ? C14 N8 1.343(3) . ? N8 C15 1.351(3) . ? C15 C16 1.467(3) . ? C16 N9 1.290(3) . ? C16 C17 1.496(3) . ? N9 C18 1.493(3) . ? C18 C19 1.516(4) . ? C19 C20 1.539(4) . ? C20 C21 1.497(4) . ? C21 N10 1.478(3) . ? N10 C22 1.282(3) . ? C22 C23 1.504(3) . ? Co3 N31 2.0550(19) . y Co3 N36 2.064(2) . y Co3 N34 2.165(2) . y Co3 N35 2.218(2) . y Co3 Cl3 2.2941(8) . y Co4 N32 2.053(2) . y Co4 N37 2.0738(18) . y Co4 N39 2.141(2) . y Co4 N40 2.1678(19) . y Co4 Cl4 2.3373(8) . y N31 C35 1.342(3) . ? N31 N32 1.346(3) . ? N32 C33 1.336(3) . ? C33 N33 1.344(3) . ? C33 C52 1.478(3) . ? N33 C35 1.349(3) . ? C35 C36 1.474(3) . ? C36 N34 1.286(3) . ? C36 C37 1.494(3) . ? N34 C38 1.481(3) . ? C38 C39 1.507(4) . ? C39 C40 1.538(4) . ? C40 C41 1.516(4) . ? C41 N35 1.481(3) . ? N35 C42 1.284(3) . ? C42 C44 1.473(3) . ? C42 C43 1.504(3) . ? N37 C45 1.333(3) . ? N37 N36 1.347(3) . ? C44 N36 1.338(3) . ? C44 N38 1.348(3) . ? N38 C45 1.350(3) . ? C45 C46 1.472(3) . ? C46 N39 1.293(3) . ? C46 C47 1.495(3) . ? N39 C48 1.471(3) . ? C48 C49 1.528(3) . ? C49 C50 1.543(4) . ? C50 C51 1.518(4) . ? C51 N40 1.478(3) . ? N40 C52 1.278(3) . ? C52 C53 1.501(3) . ? N100 C100 1.141(4) . ? C100 C101 1.455(4) . ? N110 C110 1.137(4) . ? C110 C111 1.465(4) . ? N120 C120 1.141(9) . ? C120 C121 1.451(9) . ? N130 C130 1.176(10) . ? C130 C131 1.450(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 N6 Co1 N1 89.44(8) . . y N6 Co1 N5 77.27(8) . . y N1 Co1 N5 158.52(8) . . y N6 Co1 N4 156.30(8) . . y N1 Co1 N4 76.31(7) . . y N5 Co1 N4 109.88(7) . . y N6 Co1 Cl1 103.31(6) . . y N1 Co1 Cl1 102.51(6) . . y N5 Co1 Cl1 96.99(5) . . y N4 Co1 Cl1 98.27(6) . . y N2 Co2 N7 88.57(8) . . y N2 Co2 N9 145.72(8) . . y N7 Co2 N9 76.18(8) . . y N2 Co2 N10 75.99(8) . . y N7 Co2 N10 154.63(8) . . y N9 Co2 N10 105.54(8) . . y N2 Co2 Cl2 107.04(6) . . y N7 Co2 Cl2 104.94(6) . . y N9 Co2 Cl2 106.50(6) . . y N10 Co2 Cl2 98.84(6) . . y C5 N1 N2 105.62(18) . . ? C5 N1 Co1 116.30(15) . . ? N2 N1 Co1 134.92(16) . . y C3 N2 N1 105.79(19) . . ? C3 N2 Co2 117.08(15) . . ? N1 N2 Co2 135.94(15) . . y N3 C3 N2 113.82(19) . . ? N3 C3 C22 129.8(2) . . ? N2 C3 C22 116.3(2) . . ? C3 N3 C5 100.90(18) . . ? N1 C5 N3 113.9(2) . . ? N1 C5 C6 116.5(2) . . ? N3 C5 C6 128.6(2) . . ? N4 C6 C5 115.0(2) . . ? N4 C6 C7 126.7(2) . . ? C5 C6 C7 118.3(2) . . ? C6 N4 C8 118.3(2) . . ? C6 N4 Co1 114.91(15) . . ? C8 N4 Co1 126.78(15) . . ? N4 C8 C9 110.4(2) . . ? C8 C9 C10 114.0(2) . . ? C11 C10 C9 114.1(2) . . ? N5 C11 C10 110.8(2) . . ? C12 N5 C11 118.4(2) . . ? C12 N5 Co1 115.50(15) . . ? C11 N5 Co1 126.01(16) . . ? N5 C12 C14 114.9(2) . . ? N5 C12 C13 126.2(2) . . ? C14 C12 C13 118.9(2) . . ? C14 N6 N7 105.5(2) . . ? C14 N6 Co1 114.33(16) . . ? N7 N6 Co1 134.23(15) . . ? C15 N7 N6 105.70(18) . . ? C15 N7 Co2 116.05(16) . . ? N6 N7 Co2 136.00(16) . . ? N6 C14 N8 114.0(2) . . ? N6 C14 C12 116.6(2) . . ? N8 C14 C12 128.8(2) . . ? C14 N8 C15 100.73(19) . . ? N7 C15 N8 114.0(2) . . ? N7 C15 C16 117.0(2) . . ? N8 C15 C16 128.4(2) . . ? N9 C16 C15 114.6(2) . . ? N9 C16 C17 127.3(2) . . ? C15 C16 C17 118.1(2) . . ? C16 N9 C18 117.2(2) . . ? C16 N9 Co2 114.82(16) . . ? C18 N9 Co2 127.72(16) . . ? N9 C18 C19 111.4(2) . . ? C18 C19 C20 114.6(2) . . ? C21 C20 C19 113.5(2) . . ? N10 C21 C20 111.1(2) . . ? C22 N10 C21 117.9(2) . . ? C22 N10 Co2 115.83(15) . . ? C21 N10 Co2 125.80(17) . . ? N10 C22 C3 114.4(2) . . ? N10 C22 C23 126.1(2) . . ? C3 C22 C23 119.5(2) . . ? N31 Co3 N36 88.34(7) . . y N31 Co3 N34 76.13(8) . . y N36 Co3 N34 153.54(8) . . y N31 Co3 N35 145.29(8) . . y N36 Co3 N35 75.72(7) . . y N34 Co3 N35 105.20(8) . . y N31 Co3 Cl3 108.36(6) . . y N36 Co3 Cl3 104.29(6) . . y N34 Co3 Cl3 100.91(6) . . y N35 Co3 Cl3 105.41(5) . . y N32 Co4 N37 89.47(7) . . y N32 Co4 N39 159.52(8) . . y N37 Co4 N39 76.94(7) . . y N32 Co4 N40 77.10(7) . . y N37 Co4 N40 157.44(8) . . y N39 Co4 N40 110.30(7) . . y N32 Co4 Cl4 102.03(6) . . y N37 Co4 Cl4 102.02(6) . . y N39 Co4 Cl4 95.82(5) . . y N40 Co4 Cl4 98.50(6) . . y C35 N31 N32 105.27(18) . . ? C35 N31 Co3 116.67(16) . . ? N32 N31 Co3 136.51(15) . . y C33 N32 N31 106.3(2) . . ? C33 N32 Co4 115.12(16) . . ? N31 N32 Co4 134.55(15) . . y N32 C33 N33 113.7(2) . . ? N32 C33 C52 117.2(2) . . ? N33 C33 C52 128.2(2) . . ? C33 N33 C35 100.82(19) . . ? N31 C35 N33 113.9(2) . . ? N31 C35 C36 116.1(2) . . ? N33 C35 C36 129.9(2) . . ? N34 C36 C35 114.5(2) . . ? N34 C36 C37 126.9(2) . . ? C35 C36 C37 118.6(2) . . ? C36 N34 C38 118.4(2) . . ? C36 N34 Co3 116.09(16) . . ? C38 N34 Co3 125.16(16) . . ? N34 C38 C39 111.2(2) . . ? C38 C39 C40 113.5(2) . . ? C41 C40 C39 114.1(2) . . ? N35 C41 C40 111.0(2) . . ? C42 N35 C41 116.9(2) . . ? C42 N35 Co3 114.55(15) . . ? C41 N35 Co3 128.31(17) . . ? N35 C42 C44 114.3(2) . . ? N35 C42 C43 126.8(2) . . ? C44 C42 C43 118.8(2) . . ? C45 N37 N36 105.20(18) . . ? C45 N37 Co4 114.70(15) . . ? N36 N37 Co4 134.10(16) . . ? N36 C44 N38 113.5(2) . . ? N36 C44 C42 117.6(2) . . ? N38 C44 C42 128.3(2) . . ? C44 N38 C45 100.38(18) . . ? N37 C45 N38 114.5(2) . . ? N37 C45 C46 116.6(2) . . ? N38 C45 C46 128.3(2) . . ? N39 C46 C45 114.8(2) . . ? N39 C46 C47 126.3(2) . . ? C45 C46 C47 118.8(2) . . ? C46 N39 C48 118.2(2) . . ? C46 N39 Co4 115.46(16) . . ? C48 N39 Co4 126.10(15) . . ? N39 C48 C49 111.1(2) . . ? C48 C49 C50 113.9(2) . . ? C51 C50 C49 114.1(2) . . ? N40 C51 C50 110.11(19) . . ? C52 N40 C51 118.3(2) . . ? C52 N40 Co4 114.95(15) . . ? C51 N40 Co4 126.73(16) . . ? N40 C52 C33 114.5(2) . . ? N40 C52 C53 127.3(2) . . ? C33 C52 C53 118.1(2) . . ? C44 N36 N37 106.3(2) . . ? C44 N36 Co3 116.45(16) . . ? N37 N36 Co3 135.70(15) . . ? N100 C100 C101 177.0(3) . . ? N110 C110 C111 176.5(3) . . ? N120 C120 C121 161.7(12) . . ? N130 C130 C131 153.7(14) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.362 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.043