# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 871835' #TrackingRef 'web_deposit_cif_file_0_ZongzeLi_1366566463.revised CCDC 871835.cif' _database_code_depnum_ccdc_archive 'CCDC 871835' #TrackingRef '- 871835.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H62 Co6 N8 O31' _chemical_formula_weight 1528.58 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 orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 15.0911(14) _cell_length_b 16.7006(16) _cell_length_c 24.236(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6108.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(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 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 1.686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7291 _exptl_absorpt_correction_T_max 0.7512 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42624 _diffrn_reflns_av_R_equivalents 0.0862 _diffrn_reflns_av_sigmaI/netI 0.1179 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.39 _reflns_number_total 14508 _reflns_number_gt 9474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material 'Diamond 3.1' _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^)+(0.0010P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(12) _refine_ls_number_reflns 14508 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.3642(3) 0.6317(3) -0.1179(2) 0.0346(13) Uani 1 1 d . . . H1A H 1.4172 0.6043 -0.1129 0.042 Uiso 1 1 calc R . . C2 C 1.3667(3) 0.7142(3) -0.1282(2) 0.0414(15) Uani 1 1 d . . . H2A H 1.4208 0.7404 -0.1318 0.050 Uiso 1 1 calc R . . C3 C 1.2886(3) 0.7561(3) -0.13275(19) 0.0284(12) Uani 1 1 d . . . C4 C 1.2098(4) 0.7138(3) -0.1276(2) 0.0450(15) Uani 1 1 d . . . H4A H 1.1558 0.7404 -0.1298 0.054 Uiso 1 1 calc R . . C5 C 1.2120(3) 0.6334(3) -0.1194(2) 0.0437(14) Uani 1 1 d . . . H5A H 1.1585 0.6061 -0.1166 0.052 Uiso 1 1 calc R . . C6 C 1.2929(3) 0.8445(3) -0.14445(18) 0.0281(11) Uani 1 1 d . . . C7 C 1.2108(4) 0.5069(3) 0.0019(2) 0.0454(14) Uani 1 1 d . . . H7A H 1.2600 0.5402 0.0045 0.055 Uiso 1 1 calc R . . C8 C 1.1521(3) 0.5061(3) 0.0454(2) 0.0481(15) Uani 1 1 d . . . H8A H 1.1611 0.5395 0.0756 0.058 Uiso 1 1 calc R . . C9 C 1.0811(3) 0.4563(3) 0.0439(2) 0.0306(12) Uani 1 1 d . . . C10 C 1.0703(3) 0.4099(3) -0.0018(2) 0.0386(14) Uani 1 1 d . . . H10A H 1.0231 0.3743 -0.0041 0.046 Uiso 1 1 calc R . . C11 C 1.1298(3) 0.4161(3) -0.0448(2) 0.0479(16) Uani 1 1 d . . . H11A H 1.1198 0.3861 -0.0765 0.057 Uiso 1 1 calc R . . C12 C 1.0157(3) 0.4511(3) 0.0908(2) 0.0309(12) Uani 1 1 d . . . C13 C 0.7966(4) 0.2173(3) 0.0726(2) 0.0401(14) Uani 1 1 d . . . H13 H 0.7821 0.1991 0.0374 0.048 Uiso 1 1 calc R . . C14 C 0.7100(4) 0.3150(3) 0.2112(2) 0.0385(14) Uani 1 1 d . . . H14 H 0.6763 0.2789 0.2316 0.046 Uiso 1 1 calc R . . C15 C 0.5498(4) 0.4454(4) 0.0918(2) 0.082(2) Uani 1 1 d . . . H15A H 0.5298 0.4169 0.1223 0.098 Uiso 1 1 calc R . . C16 C 0.4994(4) 0.4413(4) 0.0437(2) 0.080(2) Uani 1 1 d . . . H16A H 0.4467 0.4124 0.0435 0.096 Uiso 1 1 calc R . . C17 C 0.5259(4) 0.4780(5) -0.0016(2) 0.077(2) Uani 1 1 d . . . C18 C 0.6032(4) 0.5209(4) 0.0018(2) 0.070(2) Uani 1 1 d . . . H18A H 0.6250 0.5482 -0.0287 0.084 Uiso 1 1 calc R . . C19 C 0.6482(4) 0.5225(4) 0.0520(2) 0.069(2) Uani 1 1 d . . . H19A H 0.7007 0.5516 0.0538 0.082 Uiso 1 1 calc R . . C20 C 0.4759(3) 0.4762(3) -0.05550(19) 0.0294(12) Uani 1 1 d . . . C21 C 0.5336(3) 0.5935(3) 0.2026(2) 0.0530(17) Uani 1 1 d . . . H21A H 0.5554 0.6281 0.1758 0.064 Uiso 1 1 calc R . . C22 C 0.4514(3) 0.6103(3) 0.2256(2) 0.0524(17) Uani 1 1 d . . . H22A H 0.4171 0.6520 0.2118 0.063 Uiso 1 1 calc R . . C23 C 0.4215(3) 0.5652(3) 0.2686(2) 0.0289(12) Uani 1 1 d . . . C24 C 0.4738(3) 0.5034(3) 0.2862(2) 0.0448(15) Uani 1 1 d . . . H24A H 0.4566 0.4725 0.3163 0.054 Uiso 1 1 calc R . . C25 C 0.5538(3) 0.4867(3) 0.2585(2) 0.0403(14) Uani 1 1 d . . . H25A H 0.5873 0.4432 0.2703 0.048 Uiso 1 1 calc R . . C26 C 0.7918(3) 0.5162(3) 0.2869(2) 0.0477(16) Uani 1 1 d . . . H26 H 0.7359 0.5081 0.3020 0.057 Uiso 1 1 calc R . . C27 C 0.9836(3) 0.7194(3) 0.3534(2) 0.0360(13) Uani 1 1 d . . . H27 H 0.9500 0.7585 0.3709 0.043 Uiso 1 1 calc R . . C28 C 0.3335(3) 0.5799(3) 0.2965(2) 0.0278(11) Uani 1 1 d . . . C29 C 1.0462(3) 0.6332(3) 0.2099(2) 0.0349(13) Uani 1 1 d . . . H29 H 1.0342 0.6424 0.1728 0.042 Uiso 1 1 calc R . . C30 C 0.9737(3) 0.3839(3) 0.2550(2) 0.0397(14) Uani 1 1 d . . . H30 H 0.9782 0.3286 0.2589 0.048 Uiso 1 1 calc R . . Co1 Co 1.29349(4) 0.46289(4) -0.10929(2) 0.02254(14) Uani 1 1 d . . . Co2 Co 1.16536(4) 0.67268(3) 0.30570(3) 0.02272(15) Uani 1 1 d . . . Co3 Co 0.98946(4) 0.54278(4) 0.31912(3) 0.02656(15) Uani 1 1 d . . . Co4 Co 0.70021(4) 0.49673(4) 0.17073(2) 0.02396(15) Uani 1 1 d . . . Co5 Co 0.90663(4) 0.52073(3) 0.18193(3) 0.02322(15) Uani 1 1 d . . . Co6 Co 0.87505(4) 0.34796(4) 0.14522(3) 0.02477(16) Uani 1 1 d . . . N1 N 1.2880(3) 0.5908(2) -0.11506(16) 0.0316(10) Uani 1 1 d . . . N2 N 1.2017(3) 0.4638(2) -0.04274(15) 0.0293(9) Uani 1 1 d . . . N3 N 0.6215(2) 0.4854(2) 0.09704(16) 0.0305(10) Uani 1 1 d . . . N4 N 0.5836(2) 0.5295(2) 0.21678(15) 0.0302(10) Uani 1 1 d . . . O1 O 0.81459(16) 0.45749(16) 0.13435(11) 0.0230(7) Uani 1 1 d . . . H1B H 0.8173 0.4742 0.0956 0.028 Uiso 1 1 calc R . . O2 O 1.12537(17) 0.55606(15) 0.32251(12) 0.0227(7) Uani 1 1 d . . . H2B H 1.1495 0.5228 0.2928 0.027 Uiso 1 1 calc R . . O3 O 1.3678(2) 0.87332(18) -0.14912(14) 0.0338(9) Uani 1 1 d . . . O4 O 1.2197(2) 0.88141(17) -0.14939(13) 0.0311(8) Uani 1 1 d . . . O5 O 1.0060(2) 0.50988(18) 0.12103(13) 0.0355(8) Uani 1 1 d . . . O6 O 0.9752(2) 0.38441(19) 0.09366(13) 0.0369(9) Uani 1 1 d . . . O7 O 0.8196(2) 0.28986(18) 0.07693(13) 0.0420(10) Uani 1 1 d . . . O8 O 0.7914(2) 0.16727(16) 0.11154(12) 0.0288(7) Uani 1 1 d . . . O9 O 0.7859(2) 0.29263(17) 0.19896(12) 0.0269(8) Uani 1 1 d . . . O10 O 0.6733(2) 0.37946(19) 0.19963(15) 0.0440(10) Uani 1 1 d . . . O11 O 0.51878(19) 0.4940(2) -0.09803(12) 0.0394(9) Uani 1 1 d . . . O12 O 0.3948(2) 0.4578(2) -0.05223(12) 0.0349(8) Uani 1 1 d . . . O13 O 0.79503(19) 0.52065(19) 0.23572(12) 0.0324(8) Uani 1 1 d . . . O14 O 0.8523(2) 0.5212(2) 0.31925(13) 0.0499(10) Uani 1 1 d . . . O15 O 0.9496(2) 0.6536(2) 0.34908(14) 0.0422(10) Uani 1 1 d . . . O16 O 1.0597(2) 0.74033(17) 0.33679(13) 0.0303(8) Uani 1 1 d . . . O17 O 0.31672(19) 0.53905(18) 0.33762(12) 0.0324(8) Uani 1 1 d . . . O18 O 0.2854(2) 0.63357(18) 0.27427(13) 0.0338(8) Uani 1 1 d . . . O19 O 1.1085(2) 0.67141(18) 0.22945(13) 0.0323(8) Uani 1 1 d . . . O20 O 0.9954(2) 0.58180(18) 0.23417(12) 0.0286(8) Uani 1 1 d . . . O21 O 1.0037(3) 0.42418(19) 0.29357(14) 0.0509(11) Uani 1 1 d . . . O22 O 0.9384(2) 0.40806(18) 0.21183(13) 0.0360(9) 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 C1 0.029(3) 0.019(3) 0.055(4) 0.003(2) 0.008(3) 0.004(2) C2 0.024(3) 0.022(3) 0.078(5) 0.004(3) 0.007(3) -0.002(2) C3 0.030(3) 0.019(3) 0.036(3) -0.004(2) 0.007(2) 0.003(2) C4 0.033(3) 0.033(3) 0.068(4) -0.001(3) 0.003(3) -0.007(3) C5 0.028(3) 0.035(3) 0.068(4) 0.004(3) -0.007(3) -0.009(3) C6 0.024(3) 0.027(3) 0.033(3) 0.007(2) 0.001(2) 0.003(2) C7 0.051(4) 0.048(4) 0.037(3) -0.013(3) 0.010(3) -0.022(3) C8 0.044(3) 0.059(4) 0.041(3) -0.019(3) 0.013(3) -0.022(3) C9 0.024(3) 0.031(3) 0.037(3) 0.006(2) 0.008(2) 0.002(2) C10 0.027(3) 0.047(4) 0.042(3) -0.017(3) 0.007(3) -0.012(3) C11 0.051(4) 0.053(4) 0.040(4) -0.010(3) 0.012(3) -0.029(3) C12 0.033(3) 0.026(3) 0.034(3) 0.003(2) 0.003(2) 0.004(3) C13 0.063(4) 0.036(3) 0.021(3) 0.004(2) -0.011(3) 0.001(3) C14 0.040(3) 0.018(3) 0.057(4) -0.002(2) 0.026(3) 0.002(3) C15 0.091(5) 0.116(6) 0.038(4) 0.040(4) -0.022(4) -0.063(5) C16 0.051(4) 0.148(7) 0.041(4) 0.025(4) -0.021(3) -0.060(4) C17 0.045(4) 0.137(7) 0.047(4) 0.022(4) -0.022(3) -0.014(5) C18 0.057(4) 0.119(6) 0.034(3) 0.021(4) -0.017(3) -0.036(4) C19 0.055(4) 0.102(6) 0.048(4) 0.011(4) -0.011(3) -0.042(4) C20 0.030(3) 0.027(3) 0.031(3) 0.000(2) -0.004(2) 0.004(2) C21 0.042(4) 0.055(4) 0.063(4) 0.023(3) 0.024(3) 0.005(3) C22 0.036(3) 0.041(4) 0.080(5) 0.019(3) 0.025(3) 0.017(3) C23 0.018(3) 0.037(3) 0.032(3) -0.007(2) 0.002(2) 0.001(2) C24 0.040(3) 0.048(4) 0.046(4) 0.019(3) 0.018(3) 0.017(3) C25 0.029(3) 0.047(4) 0.045(3) 0.019(3) 0.013(2) 0.015(3) C26 0.026(3) 0.090(5) 0.027(3) -0.002(3) 0.008(3) -0.018(3) C27 0.036(3) 0.028(3) 0.045(3) -0.001(3) 0.008(3) 0.002(3) C28 0.023(3) 0.021(3) 0.040(3) -0.002(2) -0.001(2) 0.004(2) C29 0.035(3) 0.045(4) 0.025(3) 0.001(3) -0.007(2) -0.003(3) C30 0.057(4) 0.020(3) 0.042(4) 0.000(2) -0.017(3) 0.009(3) Co1 0.0210(3) 0.0227(3) 0.0239(3) 0.0001(3) 0.0015(3) -0.0003(3) Co2 0.0204(3) 0.0207(3) 0.0270(4) -0.0003(3) -0.0005(3) 0.0002(3) Co3 0.0228(3) 0.0297(4) 0.0272(4) -0.0009(3) -0.0026(3) -0.0043(3) Co4 0.0188(3) 0.0255(3) 0.0275(4) 0.0002(3) -0.0007(3) 0.0006(3) Co5 0.0211(3) 0.0221(3) 0.0265(4) 0.0002(3) 0.0001(3) -0.0010(3) Co6 0.0255(4) 0.0209(4) 0.0279(4) 0.0001(3) 0.0033(3) -0.0017(3) N1 0.022(2) 0.037(3) 0.035(3) 0.000(2) 0.006(2) -0.003(2) N2 0.029(2) 0.026(2) 0.033(2) -0.0013(19) 0.002(2) -0.007(2) N3 0.021(2) 0.036(3) 0.035(3) 0.002(2) -0.0063(19) -0.003(2) N4 0.021(2) 0.029(2) 0.040(3) 0.001(2) 0.0045(19) 0.004(2) O1 0.0181(17) 0.0240(17) 0.0268(17) -0.0002(14) -0.0028(13) -0.0010(14) O2 0.0216(16) 0.0200(16) 0.0266(18) 0.0021(14) -0.0072(14) 0.0001(14) O3 0.0231(19) 0.029(2) 0.050(2) 0.0103(17) 0.0010(17) 0.0008(16) O4 0.030(2) 0.0237(18) 0.040(2) 0.0053(16) 0.0036(16) 0.0045(16) O5 0.039(2) 0.031(2) 0.037(2) -0.0087(16) 0.0224(16) -0.0008(17) O6 0.042(2) 0.029(2) 0.040(2) -0.0035(16) 0.0130(17) -0.0075(18) O7 0.063(3) 0.023(2) 0.039(2) 0.0096(16) -0.0143(19) -0.0090(19) O8 0.035(2) 0.0170(17) 0.0341(19) 0.0007(15) -0.0053(17) 0.0004(16) O9 0.0222(18) 0.0282(18) 0.0303(19) 0.0019(15) 0.0059(15) 0.0001(15) O10 0.036(2) 0.027(2) 0.069(3) 0.0112(19) 0.0253(19) 0.0071(17) O11 0.0312(19) 0.068(3) 0.0193(18) 0.0005(17) -0.0003(15) -0.0057(19) O12 0.0213(18) 0.050(2) 0.034(2) 0.0002(18) -0.0046(15) -0.0042(17) O13 0.0229(17) 0.051(2) 0.0230(18) -0.0014(16) 0.0021(15) -0.0010(18) O14 0.032(2) 0.090(3) 0.028(2) 0.005(2) -0.0041(17) -0.017(2) O15 0.042(2) 0.033(2) 0.052(2) -0.0144(18) 0.0271(18) -0.0147(18) O16 0.0267(19) 0.0258(19) 0.038(2) -0.0015(16) 0.0072(16) -0.0023(15) O17 0.032(2) 0.0275(18) 0.037(2) 0.0125(16) 0.0109(15) 0.0039(16) O18 0.029(2) 0.029(2) 0.043(2) 0.0027(16) 0.0085(17) 0.0031(17) O19 0.036(2) 0.0267(19) 0.034(2) -0.0008(16) -0.0084(16) -0.0121(17) O20 0.0257(19) 0.033(2) 0.0267(19) -0.0002(15) -0.0026(16) -0.0063(16) O21 0.082(3) 0.027(2) 0.043(2) -0.0068(17) -0.031(2) 0.003(2) O22 0.061(2) 0.0221(19) 0.025(2) 0.0029(15) -0.0117(17) 0.0088(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.338(5) . ? C1 C2 1.401(6) . ? C1 H1A 0.9300 . ? C2 C3 1.375(6) . ? C2 H2A 0.9300 . ? C3 C4 1.389(6) . ? C3 C6 1.506(6) . ? C4 C5 1.358(6) . ? C4 H4A 0.9300 . ? C5 N1 1.353(6) . ? C5 H5A 0.9300 . ? C6 O3 1.233(5) . ? C6 O4 1.270(5) . ? C7 N2 1.307(5) . ? C7 C8 1.377(6) . ? C7 H7A 0.9300 . ? C8 C9 1.357(6) . ? C8 H8A 0.9300 . ? C9 C10 1.362(6) . ? C9 C12 1.507(6) . ? C10 C11 1.377(6) . ? C10 H10A 0.9300 . ? C11 N2 1.347(5) . ? C11 H11A 0.9300 . ? C12 O5 1.235(5) . ? C12 O6 1.272(5) . ? C13 O8 1.263(5) . ? C13 O7 1.265(5) . ? C13 H13 0.9300 . ? C14 O9 1.241(5) . ? C14 O10 1.244(5) . ? C14 H14 0.9300 . ? C15 N3 1.279(6) . ? C15 C16 1.394(7) . ? C15 H15A 0.9300 . ? C16 C17 1.318(7) . ? C16 H16A 0.9300 . ? C17 C18 1.371(7) . ? C17 C20 1.509(7) . ? C18 C19 1.395(7) . ? C18 H18A 0.9300 . ? C19 N3 1.318(6) . ? C19 H19A 0.9300 . ? C20 O11 1.253(5) . ? C20 O12 1.265(5) . ? C21 N4 1.353(6) . ? C21 C22 1.389(6) . ? C21 H21A 0.9300 . ? C22 C23 1.363(6) . ? C22 H22A 0.9300 . ? C23 C24 1.366(6) . ? C23 C28 1.510(6) . ? C24 C25 1.408(6) . ? C24 H24A 0.9300 . ? C25 N4 1.318(5) . ? C25 H25A 0.9300 . ? C26 O14 1.207(5) . ? C26 O13 1.242(5) . ? C26 H26 0.9300 . ? C27 O15 1.216(5) . ? C27 O16 1.267(5) . ? C27 H27 0.9300 . ? C28 O17 1.234(5) . ? C28 O18 1.273(5) . ? C29 O19 1.231(5) . ? C29 O20 1.293(5) . ? C29 H29 0.9300 . ? C30 O21 1.237(5) . ? C30 O22 1.243(5) . ? C30 H30 0.9300 . ? Co1 O12 2.063(3) 1_655 ? Co1 O2 2.081(3) 2_764 ? Co1 O17 2.103(3) 2_664 ? Co1 N2 2.126(4) . ? Co1 N1 2.143(4) . ? Co1 O8 2.175(3) 3 ? Co2 O19 2.038(3) . ? Co2 O18 2.071(3) 1_655 ? Co2 O2 2.079(3) . ? Co2 O16 2.094(3) . ? Co2 O8 2.111(3) 4_755 ? Co2 O9 2.137(3) 4_755 ? Co3 O2 2.065(3) . ? Co3 O15 2.078(3) . ? Co3 O21 2.086(3) . ? Co3 O14 2.102(3) . ? Co3 O11 2.104(3) 2_665 ? Co3 O20 2.161(3) . ? Co4 O1 2.046(3) . ? Co4 O10 2.119(3) . ? Co4 O4 2.120(3) 3_465 ? Co4 N3 2.153(4) . ? Co4 N4 2.155(4) . ? Co4 O13 2.165(3) . ? Co5 O3 2.026(3) 3_465 ? Co5 O22 2.072(3) . ? Co5 O1 2.092(3) . ? Co5 O20 2.107(3) . ? Co5 O5 2.112(3) . ? Co5 O13 2.130(3) . ? Co6 O6 2.053(3) . ? Co6 O1 2.061(3) . ? Co6 O9 2.088(3) . ? Co6 O7 2.093(3) . ? Co6 O16 2.095(3) 4_745 ? Co6 O22 2.128(3) . ? O1 H1B 0.9800 . ? O2 Co1 2.081(3) 2_765 ? O2 H2B 0.9800 . ? O3 Co5 2.026(3) 3_565 ? O4 Co4 2.120(3) 3_565 ? O8 Co2 2.111(3) 4_745 ? O8 Co1 2.175(3) 3_455 ? O9 Co2 2.137(3) 4_745 ? O11 Co3 2.104(3) 2_664 ? O12 Co1 2.063(3) 1_455 ? O16 Co6 2.095(3) 4_755 ? O17 Co1 2.103(3) 2_665 ? O18 Co2 2.071(3) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.3(5) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C3 C2 C1 119.4(5) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 117.9(4) . . ? C2 C3 C6 118.5(4) . . ? C4 C3 C6 123.6(5) . . ? C5 C4 C3 119.7(5) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? N1 C5 C4 123.4(5) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? O3 C6 O4 126.8(4) . . ? O3 C6 C3 116.1(4) . . ? O4 C6 C3 117.1(4) . . ? N2 C7 C8 124.1(5) . . ? N2 C7 H7A 117.9 . . ? C8 C7 H7A 117.9 . . ? C9 C8 C7 119.6(5) . . ? C9 C8 H8A 120.2 . . ? C7 C8 H8A 120.2 . . ? C8 C9 C10 117.7(4) . . ? C8 C9 C12 122.2(5) . . ? C10 C9 C12 120.2(5) . . ? C9 C10 C11 119.6(5) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? N2 C11 C10 122.8(5) . . ? N2 C11 H11A 118.6 . . ? C10 C11 H11A 118.6 . . ? O5 C12 O6 127.3(4) . . ? O5 C12 C9 118.6(4) . . ? O6 C12 C9 114.1(4) . . ? O8 C13 O7 126.0(5) . . ? O8 C13 H13 117.0 . . ? O7 C13 H13 117.0 . . ? O9 C14 O10 128.2(5) . . ? O9 C14 H14 115.9 . . ? O10 C14 H14 115.9 . . ? N3 C15 C16 124.8(5) . . ? N3 C15 H15A 117.6 . . ? C16 C15 H15A 117.6 . . ? C17 C16 C15 120.5(6) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C16 C17 C18 116.8(6) . . ? C16 C17 C20 124.0(6) . . ? C18 C17 C20 119.1(6) . . ? C17 C18 C19 118.5(6) . . ? C17 C18 H18A 120.8 . . ? C19 C18 H18A 120.8 . . ? N3 C19 C18 124.4(5) . . ? N3 C19 H19A 117.8 . . ? C18 C19 H19A 117.8 . . ? O11 C20 O12 127.5(4) . . ? O11 C20 C17 116.7(4) . . ? O12 C20 C17 115.7(4) . . ? N4 C21 C22 123.7(5) . . ? N4 C21 H21A 118.1 . . ? C22 C21 H21A 118.1 . . ? C23 C22 C21 119.4(5) . . ? C23 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? C22 C23 C24 117.7(5) . . ? C22 C23 C28 122.9(5) . . ? C24 C23 C28 119.4(5) . . ? C23 C24 C25 119.8(5) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? N4 C25 C24 123.4(5) . . ? N4 C25 H25A 118.3 . . ? C24 C25 H25A 118.3 . . ? O14 C26 O13 127.9(5) . . ? O14 C26 H26 116.0 . . ? O13 C26 H26 116.0 . . ? O15 C27 O16 127.2(5) . . ? O15 C27 H27 116.4 . . ? O16 C27 H27 116.4 . . ? O17 C28 O18 127.9(4) . . ? O17 C28 C23 116.8(4) . . ? O18 C28 C23 115.3(4) . . ? O19 C29 O20 128.4(5) . . ? O19 C29 H29 115.8 . . ? O20 C29 H29 115.8 . . ? O21 C30 O22 128.1(5) . . ? O21 C30 H30 116.0 . . ? O22 C30 H30 116.0 . . ? O12 Co1 O2 95.17(12) 1_655 2_764 ? O12 Co1 O17 174.54(13) 1_655 2_664 ? O2 Co1 O17 88.68(12) 2_764 2_664 ? O12 Co1 N2 88.55(13) 1_655 . ? O2 Co1 N2 170.72(13) 2_764 . ? O17 Co1 N2 87.07(13) 2_664 . ? O12 Co1 N1 96.50(15) 1_655 . ? O2 Co1 N1 97.03(13) 2_764 . ? O17 Co1 N1 86.85(14) 2_664 . ? N2 Co1 N1 90.98(15) . . ? O12 Co1 O8 89.23(13) 1_655 3 ? O2 Co1 O8 80.59(11) 2_764 3 ? O17 Co1 O8 87.58(12) 2_664 3 ? N2 Co1 O8 90.97(13) . 3 ? N1 Co1 O8 174.00(14) . 3 ? O19 Co2 O18 91.82(13) . 1_655 ? O19 Co2 O2 92.61(12) . . ? O18 Co2 O2 91.75(11) 1_655 . ? O19 Co2 O16 90.64(12) . . ? O18 Co2 O16 165.56(12) 1_655 . ? O2 Co2 O16 102.36(11) . . ? O19 Co2 O8 172.45(13) . 4_755 ? O18 Co2 O8 93.77(13) 1_655 4_755 ? O2 Co2 O8 82.15(11) . 4_755 ? O16 Co2 O8 85.20(12) . 4_755 ? O19 Co2 O9 96.14(12) . 4_755 ? O18 Co2 O9 88.58(12) 1_655 4_755 ? O2 Co2 O9 171.23(12) . 4_755 ? O16 Co2 O9 77.01(11) . 4_755 ? O8 Co2 O9 89.08(11) 4_755 4_755 ? O2 Co3 O15 100.26(12) . . ? O2 Co3 O21 90.64(13) . . ? O15 Co3 O21 168.40(14) . . ? O2 Co3 O14 175.60(13) . . ? O15 Co3 O14 82.37(14) . . ? O21 Co3 O14 86.52(15) . . ? O2 Co3 O11 92.99(11) . 2_665 ? O15 Co3 O11 84.83(13) . 2_665 ? O21 Co3 O11 90.68(13) . 2_665 ? O14 Co3 O11 83.69(12) . 2_665 ? O2 Co3 O20 87.95(12) . . ? O15 Co3 O20 94.37(12) . . ? O21 Co3 O20 89.96(12) . . ? O14 Co3 O20 95.40(12) . . ? O11 Co3 O20 178.86(12) 2_665 . ? O1 Co4 O10 90.48(11) . . ? O1 Co4 O4 94.88(11) . 3_465 ? O10 Co4 O4 173.83(13) . 3_465 ? O1 Co4 N3 94.57(12) . . ? O10 Co4 N3 94.99(15) . . ? O4 Co4 N3 87.64(14) 3_465 . ? O1 Co4 N4 173.54(14) . . ? O10 Co4 N4 84.65(14) . . ? O4 Co4 N4 89.78(14) 3_465 . ? N3 Co4 N4 90.09(14) . . ? O1 Co4 O13 79.34(11) . . ? O10 Co4 O13 93.26(13) . . ? O4 Co4 O13 84.75(12) 3_465 . ? N3 Co4 O13 169.79(14) . . ? N4 Co4 O13 96.67(13) . . ? O3 Co5 O22 175.41(13) 3_465 . ? O3 Co5 O1 91.87(12) 3_465 . ? O22 Co5 O1 83.55(12) . . ? O3 Co5 O20 89.83(12) 3_465 . ? O22 Co5 O20 94.73(12) . . ? O1 Co5 O20 176.52(12) . . ? O3 Co5 O5 90.34(13) 3_465 . ? O22 Co5 O5 90.14(13) . . ? O1 Co5 O5 92.46(11) . . ? O20 Co5 O5 90.57(12) . . ? O3 Co5 O13 90.70(12) 3_465 . ? O22 Co5 O13 88.17(12) . . ? O1 Co5 O13 79.16(11) . . ? O20 Co5 O13 97.78(12) . . ? O5 Co5 O13 171.59(12) . . ? O6 Co6 O1 89.13(12) . . ? O6 Co6 O9 170.07(12) . . ? O1 Co6 O9 100.79(11) . . ? O6 Co6 O7 87.16(13) . . ? O1 Co6 O7 97.66(12) . . ? O9 Co6 O7 91.75(12) . . ? O6 Co6 O16 92.03(12) . 4_745 ? O1 Co6 O16 174.86(12) . 4_745 ? O9 Co6 O16 78.06(11) . 4_745 ? O7 Co6 O16 87.40(12) . 4_745 ? O6 Co6 O22 89.51(13) . . ? O1 Co6 O22 82.94(11) . . ? O9 Co6 O22 91.42(12) . . ? O7 Co6 O22 176.60(14) . . ? O16 Co6 O22 92.06(12) 4_745 . ? C1 N1 C5 117.2(4) . . ? C1 N1 Co1 118.6(3) . . ? C5 N1 Co1 124.1(3) . . ? C7 N2 C11 116.1(4) . . ? C7 N2 Co1 124.3(3) . . ? C11 N2 Co1 119.5(3) . . ? C15 N3 C19 115.0(5) . . ? C15 N3 Co4 126.6(4) . . ? C19 N3 Co4 118.5(3) . . ? C25 N4 C21 115.7(4) . . ? C25 N4 Co4 122.6(3) . . ? C21 N4 Co4 121.6(3) . . ? Co4 O1 Co6 127.06(13) . . ? Co4 O1 Co5 99.26(11) . . ? Co6 O1 Co5 94.80(11) . . ? Co4 O1 H1B 110.9 . . ? Co6 O1 H1B 110.9 . . ? Co5 O1 H1B 110.9 . . ? Co3 O2 Co2 112.41(12) . . ? Co3 O2 Co1 126.85(14) . 2_765 ? Co2 O2 Co1 97.31(11) . 2_765 ? Co3 O2 H2B 106.2 . . ? Co2 O2 H2B 106.2 . . ? Co1 O2 H2B 106.2 2_765 . ? C6 O3 Co5 129.9(3) . 3_565 ? C6 O4 Co4 127.5(3) . 3_565 ? C12 O5 Co5 124.6(3) . . ? C12 O6 Co6 130.3(3) . . ? C13 O7 Co6 128.3(3) . . ? C13 O8 Co2 131.5(3) . 4_745 ? C13 O8 Co1 129.9(3) . 3_455 ? Co2 O8 Co1 93.56(11) 4_745 3_455 ? C14 O9 Co6 127.7(3) . . ? C14 O9 Co2 127.7(3) . 4_745 ? Co6 O9 Co2 99.21(13) . 4_745 ? C14 O10 Co4 142.1(3) . . ? C20 O11 Co3 133.2(3) . 2_664 ? C20 O12 Co1 131.7(3) . 1_455 ? C26 O13 Co5 129.9(3) . . ? C26 O13 Co4 133.5(3) . . ? Co5 O13 Co4 94.44(12) . . ? C26 O14 Co3 139.1(3) . . ? C27 O15 Co3 135.4(3) . . ? C27 O16 Co2 131.0(3) . . ? C27 O16 Co6 126.6(3) . 4_755 ? Co2 O16 Co6 100.39(13) . 4_755 ? C28 O17 Co1 131.7(3) . 2_665 ? C28 O18 Co2 124.4(3) . 1_455 ? C29 O19 Co2 132.6(3) . . ? C29 O20 Co5 115.1(3) . . ? C29 O20 Co3 131.2(3) . . ? Co5 O20 Co3 113.58(14) . . ? C30 O21 Co3 134.6(3) . . ? C30 O22 Co5 133.5(3) . . ? C30 O22 Co6 132.8(3) . . ? Co5 O22 Co6 93.40(12) . . ? 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 N1 C1 C2 C3 3.4(8) . . . . ? C1 C2 C3 C4 -0.8(8) . . . . ? C1 C2 C3 C6 -179.3(5) . . . . ? C2 C3 C4 C5 -1.2(8) . . . . ? C6 C3 C4 C5 177.2(5) . . . . ? C3 C4 C5 N1 0.9(9) . . . . ? C2 C3 C6 O3 0.0(7) . . . . ? C4 C3 C6 O3 -178.4(5) . . . . ? C2 C3 C6 O4 178.8(5) . . . . ? C4 C3 C6 O4 0.5(7) . . . . ? N2 C7 C8 C9 2.2(9) . . . . ? C7 C8 C9 C10 -1.2(8) . . . . ? C7 C8 C9 C12 178.4(5) . . . . ? C8 C9 C10 C11 -1.3(8) . . . . ? C12 C9 C10 C11 179.0(5) . . . . ? C9 C10 C11 N2 3.3(8) . . . . ? C8 C9 C12 O5 26.5(7) . . . . ? C10 C9 C12 O5 -153.9(5) . . . . ? C8 C9 C12 O6 -154.5(5) . . . . ? C10 C9 C12 O6 25.2(7) . . . . ? N3 C15 C16 C17 2.4(13) . . . . ? C15 C16 C17 C18 -1.3(12) . . . . ? C15 C16 C17 C20 179.5(6) . . . . ? C16 C17 C18 C19 0.3(11) . . . . ? C20 C17 C18 C19 179.6(6) . . . . ? C17 C18 C19 N3 -0.1(11) . . . . ? C16 C17 C20 O11 -161.0(7) . . . . ? C18 C17 C20 O11 19.8(9) . . . . ? C16 C17 C20 O12 20.1(10) . . . . ? C18 C17 C20 O12 -159.1(6) . . . . ? N4 C21 C22 C23 6.4(9) . . . . ? C21 C22 C23 C24 -1.7(8) . . . . ? C21 C22 C23 C28 179.4(5) . . . . ? C22 C23 C24 C25 -2.3(8) . . . . ? C28 C23 C24 C25 176.6(5) . . . . ? C23 C24 C25 N4 2.2(8) . . . . ? C22 C23 C28 O17 -174.6(5) . . . . ? C24 C23 C28 O17 6.5(7) . . . . ? C22 C23 C28 O18 5.3(7) . . . . ? C24 C23 C28 O18 -173.6(4) . . . . ? C2 C1 N1 C5 -3.7(7) . . . . ? C2 C1 N1 Co1 172.4(4) . . . . ? C4 C5 N1 C1 1.6(8) . . . . ? C4 C5 N1 Co1 -174.3(4) . . . . ? O12 Co1 N1 C1 43.3(4) 1_655 . . . ? O2 Co1 N1 C1 -52.8(4) 2_764 . . . ? O17 Co1 N1 C1 -141.0(4) 2_664 . . . ? N2 Co1 N1 C1 131.9(4) . . . . ? O8 Co1 N1 C1 -119.1(12) 3 . . . ? O12 Co1 N1 C5 -140.9(4) 1_655 . . . ? O2 Co1 N1 C5 123.1(4) 2_764 . . . ? O17 Co1 N1 C5 34.8(4) 2_664 . . . ? N2 Co1 N1 C5 -52.2(4) . . . . ? O8 Co1 N1 C5 56.7(14) 3 . . . ? C8 C7 N2 C11 -0.3(8) . . . . ? C8 C7 N2 Co1 -178.6(4) . . . . ? C10 C11 N2 C7 -2.4(8) . . . . ? C10 C11 N2 Co1 176.0(4) . . . . ? O12 Co1 N2 C7 43.8(4) 1_655 . . . ? O2 Co1 N2 C7 157.6(7) 2_764 . . . ? O17 Co1 N2 C7 -139.5(4) 2_664 . . . ? N1 Co1 N2 C7 -52.7(4) . . . . ? O8 Co1 N2 C7 133.0(4) 3 . . . ? O12 Co1 N2 C11 -134.5(4) 1_655 . . . ? O2 Co1 N2 C11 -20.6(11) 2_764 . . . ? O17 Co1 N2 C11 42.3(4) 2_664 . . . ? N1 Co1 N2 C11 129.0(4) . . . . ? O8 Co1 N2 C11 -45.3(4) 3 . . . ? C16 C15 N3 C19 -2.1(10) . . . . ? C16 C15 N3 Co4 178.2(5) . . . . ? C18 C19 N3 C15 1.0(9) . . . . ? C18 C19 N3 Co4 -179.2(5) . . . . ? O1 Co4 N3 C15 124.7(5) . . . . ? O10 Co4 N3 C15 33.9(5) . . . . ? O4 Co4 N3 C15 -140.5(5) 3_465 . . . ? N4 Co4 N3 C15 -50.8(5) . . . . ? O13 Co4 N3 C15 177.7(7) . . . . ? O1 Co4 N3 C19 -55.0(4) . . . . ? O10 Co4 N3 C19 -145.9(4) . . . . ? O4 Co4 N3 C19 39.7(4) 3_465 . . . ? N4 Co4 N3 C19 129.5(4) . . . . ? O13 Co4 N3 C19 -2.1(10) . . . . ? C24 C25 N4 C21 2.0(8) . . . . ? C24 C25 N4 Co4 -174.6(4) . . . . ? C22 C21 N4 C25 -6.4(8) . . . . ? C22 C21 N4 Co4 170.3(4) . . . . ? O1 Co4 N4 C25 -17.8(14) . . . . ? O10 Co4 N4 C25 23.3(4) . . . . ? O4 Co4 N4 C25 -154.0(4) 3_465 . . . ? N3 Co4 N4 C25 118.3(4) . . . . ? O13 Co4 N4 C25 -69.3(4) . . . . ? O1 Co4 N4 C21 165.8(10) . . . . ? O10 Co4 N4 C21 -153.1(4) . . . . ? O4 Co4 N4 C21 29.6(4) 3_465 . . . ? N3 Co4 N4 C21 -58.0(4) . . . . ? O13 Co4 N4 C21 114.3(4) . . . . ? O10 Co4 O1 Co6 -11.32(18) . . . . ? O4 Co4 O1 Co6 165.63(17) 3_465 . . . ? N3 Co4 O1 Co6 -106.36(19) . . . . ? N4 Co4 O1 Co6 29.6(12) . . . . ? O13 Co4 O1 Co6 81.91(17) . . . . ? O10 Co4 O1 Co5 -114.58(13) . . . . ? O4 Co4 O1 Co5 62.36(13) 3_465 . . . ? N3 Co4 O1 Co5 150.37(14) . . . . ? N4 Co4 O1 Co5 -73.6(12) . . . . ? O13 Co4 O1 Co5 -21.35(11) . . . . ? O6 Co6 O1 Co4 -177.79(17) . . . . ? O9 Co6 O1 Co4 1.93(18) . . . . ? O7 Co6 O1 Co4 95.19(18) . . . . ? O16 Co6 O1 Co4 -74.7(13) 4_745 . . . ? O22 Co6 O1 Co4 -88.18(18) . . . . ? O6 Co6 O1 Co5 -72.38(12) . . . . ? O9 Co6 O1 Co5 107.34(11) . . . . ? O7 Co6 O1 Co5 -159.39(12) . . . . ? O16 Co6 O1 Co5 30.7(13) 4_745 . . . ? O22 Co6 O1 Co5 17.24(12) . . . . ? O3 Co5 O1 Co4 -68.61(13) 3_465 . . . ? O22 Co5 O1 Co4 111.10(13) . . . . ? O20 Co5 O1 Co4 50.5(19) . . . . ? O5 Co5 O1 Co4 -159.04(12) . . . . ? O13 Co5 O1 Co4 21.74(12) . . . . ? O3 Co5 O1 Co6 162.60(12) 3_465 . . . ? O22 Co5 O1 Co6 -17.69(12) . . . . ? O20 Co5 O1 Co6 -78.3(18) . . . . ? O5 Co5 O1 Co6 72.18(12) . . . . ? O13 Co5 O1 Co6 -107.05(12) . . . . ? O15 Co3 O2 Co2 -34.47(17) . . . . ? O21 Co3 O2 Co2 149.54(15) . . . . ? O14 Co3 O2 Co2 -160.8(17) . . . . ? O11 Co3 O2 Co2 -119.75(15) 2_665 . . . ? O20 Co3 O2 Co2 59.60(15) . . . . ? O15 Co3 O2 Co1 84.28(18) . . . 2_765 ? O21 Co3 O2 Co1 -91.71(17) . . . 2_765 ? O14 Co3 O2 Co1 -42.0(18) . . . 2_765 ? O11 Co3 O2 Co1 -1.00(18) 2_665 . . 2_765 ? O20 Co3 O2 Co1 178.36(17) . . . 2_765 ? O19 Co2 O2 Co3 -59.18(15) . . . . ? O18 Co2 O2 Co3 -151.08(15) 1_655 . . . ? O16 Co2 O2 Co3 32.05(17) . . . . ? O8 Co2 O2 Co3 115.36(15) 4_755 . . . ? O9 Co2 O2 Co3 116.9(7) 4_755 . . . ? O19 Co2 O2 Co1 165.84(12) . . . 2_765 ? O18 Co2 O2 Co1 73.93(13) 1_655 . . 2_765 ? O16 Co2 O2 Co1 -102.93(12) . . . 2_765 ? O8 Co2 O2 Co1 -19.63(12) 4_755 . . 2_765 ? O9 Co2 O2 Co1 -18.1(8) 4_755 . . 2_765 ? O4 C6 O3 Co5 -15.1(7) . . . 3_565 ? C3 C6 O3 Co5 163.6(3) . . . 3_565 ? O3 C6 O4 Co4 2.9(7) . . . 3_565 ? C3 C6 O4 Co4 -175.8(3) . . . 3_565 ? O6 C12 O5 Co5 -7.4(7) . . . . ? C9 C12 O5 Co5 171.5(3) . . . . ? O3 Co5 O5 C12 -126.7(4) 3_465 . . . ? O22 Co5 O5 C12 48.7(4) . . . . ? O1 Co5 O5 C12 -34.9(4) . . . . ? O20 Co5 O5 C12 143.4(4) . . . . ? O13 Co5 O5 C12 -29.7(11) . . . . ? O5 C12 O6 Co6 3.4(8) . . . . ? C9 C12 O6 Co6 -175.5(3) . . . . ? O1 Co6 O6 C12 42.6(4) . . . . ? O9 Co6 O6 C12 -135.8(7) . . . . ? O7 Co6 O6 C12 140.3(4) . . . . ? O16 Co6 O6 C12 -132.4(4) 4_745 . . . ? O22 Co6 O6 C12 -40.3(4) . . . . ? O8 C13 O7 Co6 10.3(9) . . . . ? O6 Co6 O7 C13 126.5(5) . . . . ? O1 Co6 O7 C13 -144.8(5) . . . . ? O9 Co6 O7 C13 -43.6(5) . . . . ? O16 Co6 O7 C13 34.3(5) 4_745 . . . ? O22 Co6 O7 C13 115(2) . . . . ? O7 C13 O8 Co2 -10.7(9) . . . 4_745 ? O7 C13 O8 Co1 -158.8(4) . . . 3_455 ? O10 C14 O9 Co6 -9.1(8) . . . . ? O10 C14 O9 Co2 -157.7(4) . . . 4_745 ? O6 Co6 O9 C14 -169.2(7) . . . . ? O1 Co6 O9 C14 12.4(4) . . . . ? O7 Co6 O9 C14 -85.7(4) . . . . ? O16 Co6 O9 C14 -172.7(4) 4_745 . . . ? O22 Co6 O9 C14 95.5(4) . . . . ? O6 Co6 O9 Co2 -13.9(8) . . . 4_745 ? O1 Co6 O9 Co2 167.76(11) . . . 4_745 ? O7 Co6 O9 Co2 69.62(13) . . . 4_745 ? O16 Co6 O9 Co2 -17.35(12) 4_745 . . 4_745 ? O22 Co6 O9 Co2 -109.16(13) . . . 4_745 ? O9 C14 O10 Co4 -14.9(9) . . . . ? O1 Co4 O10 C14 23.5(6) . . . . ? O4 Co4 O10 C14 -126.8(11) 3_465 . . . ? N3 Co4 O10 C14 118.1(6) . . . . ? N4 Co4 O10 C14 -152.3(6) . . . . ? O13 Co4 O10 C14 -55.9(6) . . . . ? O12 C20 O11 Co3 -32.8(8) . . . 2_664 ? C17 C20 O11 Co3 148.4(4) . . . 2_664 ? O11 C20 O12 Co1 -9.5(8) . . . 1_455 ? C17 C20 O12 Co1 169.4(4) . . . 1_455 ? O14 C26 O13 Co5 10.5(9) . . . . ? O14 C26 O13 Co4 169.5(4) . . . . ? O3 Co5 O13 C26 -123.6(5) 3_465 . . . ? O22 Co5 O13 C26 60.8(5) . . . . ? O1 Co5 O13 C26 144.6(5) . . . . ? O20 Co5 O13 C26 -33.7(5) . . . . ? O5 Co5 O13 C26 139.4(8) . . . . ? O3 Co5 O13 Co4 71.50(13) 3_465 . . . ? O22 Co5 O13 Co4 -104.06(13) . . . . ? O1 Co5 O13 Co4 -20.27(11) . . . . ? O20 Co5 O13 Co4 161.42(12) . . . . ? O5 Co5 O13 Co4 -25.6(9) . . . . ? O1 Co4 O13 C26 -143.3(5) . . . . ? O10 Co4 O13 C26 -53.4(5) . . . . ? O4 Co4 O13 C26 120.7(5) 3_465 . . . ? N3 Co4 O13 C26 162.7(7) . . . . ? N4 Co4 O13 C26 31.6(5) . . . . ? O1 Co4 O13 Co5 20.73(11) . . . . ? O10 Co4 O13 Co5 110.60(12) . . . . ? O4 Co4 O13 Co5 -75.25(12) 3_465 . . . ? N3 Co4 O13 Co5 -33.3(8) . . . . ? N4 Co4 O13 Co5 -164.41(14) . . . . ? O13 C26 O14 Co3 3.1(11) . . . . ? O2 Co3 O14 C26 -128.0(16) . . . . ? O15 Co3 O14 C26 105.2(6) . . . . ? O21 Co3 O14 C26 -78.2(6) . . . . ? O11 Co3 O14 C26 -169.2(6) 2_665 . . . ? O20 Co3 O14 C26 11.5(6) . . . . ? O16 C27 O15 Co3 3.6(9) . . . . ? O2 Co3 O15 C27 20.6(5) . . . . ? O14 Co3 O15 C27 -163.0(5) . . . . ? O11 Co3 O15 C27 112.7(5) 2_665 . . . ? O20 Co3 O15 C27 -68.1(5) . . . . ? O15 C27 O16 Co2 -9.5(8) . . . . ? O15 C27 O16 Co6 -170.1(4) . . . 4_755 ? O19 Co2 O16 C27 82.1(4) . . . . ? O18 Co2 O16 C27 -178.1(5) 1_655 . . . ? O2 Co2 O16 C27 -10.7(4) . . . . ? O8 Co2 O16 C27 -91.6(4) 4_755 . . . ? O9 Co2 O16 C27 178.3(4) 4_755 . . . ? O19 Co2 O16 Co6 -113.59(13) . . . 4_755 ? O18 Co2 O16 Co6 -13.8(6) 1_655 . . 4_755 ? O2 Co2 O16 Co6 153.60(12) . . . 4_755 ? O8 Co2 O16 Co6 72.73(13) 4_755 . . 4_755 ? O9 Co2 O16 Co6 -17.44(12) 4_755 . . 4_755 ? O18 C28 O17 Co1 -0.7(7) . . . 2_665 ? C23 C28 O17 Co1 179.2(3) . . . 2_665 ? O17 C28 O18 Co2 4.2(7) . . . 1_455 ? C23 C28 O18 Co2 -175.7(3) . . . 1_455 ? O20 C29 O19 Co2 2.2(8) . . . . ? O18 Co2 O19 C29 117.5(4) 1_655 . . . ? O2 Co2 O19 C29 25.7(4) . . . . ? O16 Co2 O19 C29 -76.7(4) . . . . ? O8 Co2 O19 C29 -20.2(12) 4_755 . . . ? O9 Co2 O19 C29 -153.7(4) 4_755 . . . ? O19 C29 O20 Co5 -173.1(4) . . . . ? O19 C29 O20 Co3 3.4(7) . . . . ? O3 Co5 O20 C29 -49.7(3) 3_465 . . . ? O22 Co5 O20 C29 130.8(3) . . . . ? O1 Co5 O20 C29 -168.8(17) . . . . ? O5 Co5 O20 C29 40.6(3) . . . . ? O13 Co5 O20 C29 -140.4(3) . . . . ? O3 Co5 O20 Co3 133.10(15) 3_465 . . . ? O22 Co5 O20 Co3 -46.37(16) . . . . ? O1 Co5 O20 Co3 14.0(19) . . . . ? O5 Co5 O20 Co3 -136.56(15) . . . . ? O13 Co5 O20 Co3 42.43(15) . . . . ? O2 Co3 O20 C29 -34.6(4) . . . . ? O15 Co3 O20 C29 65.6(4) . . . . ? O21 Co3 O20 C29 -125.2(4) . . . . ? O14 Co3 O20 C29 148.3(4) . . . . ? O11 Co3 O20 C29 111(7) 2_665 . . . ? O2 Co3 O20 Co5 142.03(15) . . . . ? O15 Co3 O20 Co5 -117.84(15) . . . . ? O21 Co3 O20 Co5 51.39(16) . . . . ? O14 Co3 O20 Co5 -35.11(17) . . . . ? O11 Co3 O20 Co5 -72(7) 2_665 . . . ? O22 C30 O21 Co3 16.8(10) . . . . ? O2 Co3 O21 C30 -128.6(5) . . . . ? O15 Co3 O21 C30 71.4(9) . . . . ? O14 Co3 O21 C30 54.7(5) . . . . ? O11 Co3 O21 C30 138.4(5) 2_665 . . . ? O20 Co3 O21 C30 -40.7(5) . . . . ? O21 C30 O22 Co5 -2.5(9) . . . . ? O21 C30 O22 Co6 -174.4(4) . . . . ? O3 Co5 O22 C30 -153.5(15) 3_465 . . . ? O1 Co5 O22 C30 -157.0(5) . . . . ? O20 Co5 O22 C30 19.9(5) . . . . ? O5 Co5 O22 C30 110.5(5) . . . . ? O13 Co5 O22 C30 -77.7(5) . . . . ? O3 Co5 O22 Co6 20.6(17) 3_465 . . . ? O1 Co5 O22 Co6 17.08(11) . . . . ? O20 Co5 O22 Co6 -165.96(12) . . . . ? O5 Co5 O22 Co6 -75.37(13) . . . . ? O13 Co5 O22 Co6 96.38(13) . . . . ? O6 Co6 O22 C30 -114.0(5) . . . . ? O1 Co6 O22 C30 156.8(5) . . . . ? O9 Co6 O22 C30 56.1(5) . . . . ? O7 Co6 O22 C30 -103(2) . . . . ? O16 Co6 O22 C30 -22.0(5) 4_745 . . . ? O6 Co6 O22 Co5 71.82(14) . . . . ? O1 Co6 O22 Co5 -17.37(12) . . . . ? O9 Co6 O22 Co5 -118.07(13) . . . . ? O7 Co6 O22 Co5 83(2) . . . . ? O16 Co6 O22 Co5 163.83(13) 4_745 . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.970 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.076 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.073 0.043 0.643 2888 841 ' ' _platon_squeeze_details ; The asymmetric unit contains 4 DMF and 5 water molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; data_2 _database_code_depnum_ccdc_archive 'CCDC 921457' #TrackingRef 'web_deposit_cif_file_1_ZongzeLi_1366566463.revised CCDC 921457.cif' _database_code_depnum_ccdc_archive 'CCDC 921457' #TrackingRef '- 921457.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H15 Co N3 O5' _chemical_formula_weight 376.23 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 Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 6.3070(10) _cell_length_b 12.611(2) _cell_length_c 10.4919(17) _cell_angle_alpha 90.00 _cell_angle_beta 91.227(2) _cell_angle_gamma 90.00 _cell_volume 834.3(2) _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 purple _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 1.058 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7490 _exptl_absorpt_correction_T_max 0.7779 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4658 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.24 _reflns_number_total 2244 _reflns_number_gt 1917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material 'Diamond 3.1' _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^)+(0.0992P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(4) _refine_ls_number_reflns 2244 _refine_ls_number_parameters 218 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1419 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.023 _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 C5 C 0.7927(9) 0.3961(5) 1.1378(6) 0.0385(15) Uani 1 1 d . . . N1 N 0.9823(8) 0.3562(4) 1.1190(5) 0.0349(12) Uani 1 1 d . . . C12 C 1.0233(9) 1.0880(5) 0.3653(6) 0.0341(14) Uani 1 1 d . . . Co1 Co 0.6280(2) 0.75374(5) 0.74005(18) 0.0305(3) Uani 1 1 d . . . O1 O 0.5592(7) 0.6432(4) 0.9013(5) 0.0438(12) Uani 1 1 d . . . O2 O 0.8658(7) 0.6524(3) 0.8048(5) 0.0450(12) Uani 1 1 d . . . O3 O 1.2114(7) 1.1153(4) 0.3767(5) 0.0446(12) Uani 1 1 d . . . O4 O 0.8998(7) 1.1345(3) 0.2845(5) 0.0438(11) Uani 1 1 d . . . O5 O 0.2145(19) 0.2873(10) 0.7626(13) 0.154(5) Uani 1 1 d . . . N2 N 0.7708(8) 0.8437(4) 0.6024(5) 0.0357(12) Uani 1 1 d . . . N3 N 0.5363(18) 0.2634(7) 0.6728(13) 0.096(2) Uani 1 1 d U . . C1 C 1.1011(11) 0.3979(6) 1.0265(8) 0.0467(18) Uani 1 1 d . . . H1A H 1.2355 0.3702 1.0132 0.056 Uiso 1 1 calc R . . C2 C 1.0289(11) 0.4814(6) 0.9501(7) 0.0500(19) Uani 1 1 d . . . H2A H 1.1134 0.5087 0.8864 0.060 Uiso 1 1 calc R . . C3 C 0.8276(10) 0.5233(5) 0.9708(7) 0.0380(15) Uani 1 1 d . . . C4 C 0.7089(10) 0.4807(5) 1.0664(7) 0.0404(16) Uani 1 1 d . . . H4A H 0.5752 0.5076 1.0834 0.048 Uiso 1 1 calc R . . H5A H 0.7089 0.3665 1.1998 0.048 Uiso 1 1 d R . . C6 C 0.7424(11) 0.6148(5) 0.8905(7) 0.0385(16) Uani 1 1 d . . . C7 C 0.9693(10) 0.8791(5) 0.6158(7) 0.0405(15) Uani 1 1 d . . . H7A H 1.0532 0.8494 0.6805 0.049 Uiso 1 1 calc R . . C8 C 1.0587(10) 0.9552(5) 0.5426(7) 0.0406(15) Uani 1 1 d . . . H8A H 1.1966 0.9782 0.5591 0.049 Uiso 1 1 calc R . . C9 C 0.9363(10) 0.9984(5) 0.4408(7) 0.0365(14) Uani 1 1 d . . . C10 C 0.7330(10) 0.9599(5) 0.4238(7) 0.0456(17) Uani 1 1 d . . . H10A H 0.6467 0.9867 0.3584 0.055 Uiso 1 1 calc R . . C11 C 0.6575(10) 0.8831(5) 0.5015(7) 0.0411(16) Uani 1 1 d . . . H11A H 0.5222 0.8564 0.4849 0.049 Uiso 1 1 calc R . . C13 C 0.321(2) 0.2485(8) 0.6791(17) 0.098(3) Uani 1 1 d U . . H13A H 0.2541 0.2070 0.6170 0.117 Uiso 1 1 calc R . . C14 C 0.630(2) 0.3259(11) 0.7717(15) 0.123(3) Uani 1 1 d U . . H14A H 0.7801 0.3310 0.7593 0.185 Uiso 1 1 calc R . . H14B H 0.6045 0.2933 0.8526 0.185 Uiso 1 1 calc R . . H14C H 0.5689 0.3956 0.7700 0.185 Uiso 1 1 calc R . . C15 C 0.650(2) 0.2189(11) 0.5740(16) 0.112(3) Uani 1 1 d U . . H15A H 0.5559 0.1784 0.5199 0.168 Uiso 1 1 calc R . . H15B H 0.7587 0.1734 0.6088 0.168 Uiso 1 1 calc R . . H15C H 0.7139 0.2743 0.5252 0.168 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C5 0.043(3) 0.036(3) 0.037(4) 0.006(3) 0.015(3) -0.003(3) N1 0.038(3) 0.036(3) 0.032(3) 0.004(3) 0.006(2) -0.001(2) C12 0.045(3) 0.030(3) 0.027(3) 0.004(3) -0.002(3) -0.001(3) Co1 0.0449(4) 0.0204(3) 0.0263(4) 0.0005(4) 0.0005(3) 0.0013(3) O1 0.049(3) 0.042(3) 0.040(3) 0.009(2) 0.006(2) 0.019(2) O2 0.056(3) 0.034(2) 0.045(3) 0.013(2) 0.005(2) 0.006(2) O3 0.041(3) 0.052(3) 0.041(3) 0.017(2) -0.003(2) -0.011(2) O4 0.051(2) 0.037(2) 0.043(3) 0.017(2) -0.008(2) -0.0050(19) O5 0.195(13) 0.172(9) 0.097(8) -0.007(9) 0.052(9) 0.047(9) N2 0.042(3) 0.032(3) 0.034(3) 0.012(2) -0.002(2) 0.000(2) N3 0.102(3) 0.091(4) 0.095(4) -0.013(3) 0.001(3) -0.001(3) C1 0.045(4) 0.037(4) 0.058(5) -0.001(4) 0.010(4) 0.007(3) C2 0.052(4) 0.046(4) 0.052(5) 0.019(4) 0.022(4) 0.011(3) C3 0.045(3) 0.033(4) 0.036(4) 0.007(3) 0.003(3) 0.001(3) C4 0.041(3) 0.041(4) 0.040(4) 0.011(3) 0.008(3) 0.010(3) C6 0.048(4) 0.037(4) 0.031(4) 0.005(3) 0.006(3) 0.006(3) C7 0.048(3) 0.029(3) 0.044(4) 0.013(3) -0.013(3) -0.001(3) C8 0.040(3) 0.040(4) 0.042(4) 0.011(3) -0.007(3) -0.002(3) C9 0.043(3) 0.030(3) 0.037(4) 0.006(3) -0.002(3) -0.005(2) C10 0.049(4) 0.050(4) 0.038(4) 0.014(3) -0.011(3) -0.006(3) C11 0.049(4) 0.031(3) 0.042(4) 0.009(3) -0.015(3) -0.007(3) C13 0.102(3) 0.095(4) 0.095(4) -0.003(3) 0.004(3) 0.001(3) C14 0.127(5) 0.124(5) 0.118(5) -0.023(4) -0.012(4) -0.005(4) C15 0.113(5) 0.117(5) 0.107(5) -0.010(4) 0.011(4) 0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C5 N1 1.316(8) . ? C5 C4 1.400(9) . ? C5 H5A 0.9259 . ? N1 C1 1.345(9) . ? N1 Co1 2.081(5) 2_565 ? C12 O3 1.239(7) . ? C12 O4 1.282(7) . ? C12 C9 1.491(9) . ? C12 Co1 2.487(6) 2_574 ? Co1 N2 2.059(5) . ? Co1 O2 2.073(4) . ? Co1 O4 2.075(4) 2_475 ? Co1 N1 2.081(5) 2_464 ? Co1 O1 2.242(5) . ? Co1 O3 2.242(5) 2_475 ? Co1 C6 2.456(7) . ? Co1 C12 2.487(6) 2_475 ? O1 C6 1.218(8) . ? O2 C6 1.292(9) . ? O3 Co1 2.242(5) 2_574 ? O4 Co1 2.075(4) 2_574 ? O5 C13 1.219(19) . ? N2 C7 1.333(8) . ? N2 C11 1.359(8) . ? N3 C13 1.372(18) . ? N3 C15 1.391(18) . ? N3 C14 1.422(17) . ? C1 C2 1.394(10) . ? C1 H1A 0.9300 . ? C2 C3 1.396(9) . ? C2 H2A 0.9300 . ? C3 C4 1.374(9) . ? C3 C6 1.520(9) . ? C4 H4A 0.9300 . ? C7 C8 1.359(9) . ? C7 H7A 0.9300 . ? C8 C9 1.414(9) . ? C8 H8A 0.9300 . ? C9 C10 1.379(9) . ? C10 C11 1.359(9) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 H13A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C5 C4 123.0(6) . . ? N1 C5 H5A 119.0 . . ? C4 C5 H5A 118.0 . . ? C5 N1 C1 118.7(6) . . ? C5 N1 Co1 123.7(5) . 2_565 ? C1 N1 Co1 117.1(5) . 2_565 ? O3 C12 O4 120.2(5) . . ? O3 C12 C9 121.5(5) . . ? O4 C12 C9 118.2(5) . . ? O3 C12 Co1 64.1(3) . 2_574 ? O4 C12 Co1 56.4(3) . 2_574 ? C9 C12 Co1 173.6(4) . 2_574 ? N2 Co1 O2 104.2(2) . . ? N2 Co1 O4 95.7(2) . 2_475 ? O2 Co1 O4 147.7(2) . 2_475 ? N2 Co1 N1 97.6(2) . 2_464 ? O2 Co1 N1 95.53(19) . 2_464 ? O4 Co1 N1 106.9(2) 2_475 2_464 ? N2 Co1 O1 165.15(18) . . ? O2 Co1 O1 61.32(18) . . ? O4 Co1 O1 96.1(2) 2_475 . ? N1 Co1 O1 87.5(2) 2_464 . ? N2 Co1 O3 86.7(2) . 2_475 ? O2 Co1 O3 94.96(19) . 2_475 ? O4 Co1 O3 60.68(17) 2_475 2_475 ? N1 Co1 O3 167.30(18) 2_464 2_475 ? O1 Co1 O3 91.3(2) . 2_475 ? N2 Co1 C6 135.8(2) . . ? O2 Co1 C6 31.7(2) . . ? O4 Co1 C6 122.4(2) 2_475 . ? N1 Co1 C6 92.1(2) 2_464 . ? O1 Co1 C6 29.6(2) . . ? O3 Co1 C6 93.0(3) 2_475 . ? N2 Co1 C12 93.1(2) . 2_475 ? O2 Co1 C12 121.3(2) . 2_475 ? O4 Co1 C12 30.98(18) 2_475 2_475 ? N1 Co1 C12 137.6(2) 2_464 2_475 ? O1 Co1 C12 92.4(2) . 2_475 ? O3 Co1 C12 29.80(18) 2_475 2_475 ? C6 Co1 C12 108.1(2) . 2_475 ? C6 O1 Co1 85.0(4) . . ? C6 O2 Co1 90.7(4) . . ? C12 O3 Co1 86.1(4) . 2_574 ? C12 O4 Co1 92.6(4) . 2_574 ? C7 N2 C11 115.9(6) . . ? C7 N2 Co1 122.3(4) . . ? C11 N2 Co1 121.1(4) . . ? C13 N3 C15 120.4(13) . . ? C13 N3 C14 115.9(13) . . ? C15 N3 C14 123.7(13) . . ? N1 C1 C2 122.0(7) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C1 C2 C3 118.9(7) . . ? C1 C2 H2A 120.5 . . ? C3 C2 H2A 120.5 . . ? C4 C3 C2 118.5(6) . . ? C4 C3 C6 120.6(6) . . ? C2 C3 C6 120.9(6) . . ? C3 C4 C5 118.9(5) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? O1 C6 O2 123.0(7) . . ? O1 C6 C3 119.8(7) . . ? O2 C6 C3 117.0(6) . . ? O1 C6 Co1 65.4(4) . . ? O2 C6 Co1 57.6(3) . . ? C3 C6 Co1 173.3(5) . . ? N2 C7 C8 125.2(6) . . ? N2 C7 H7A 117.4 . . ? C8 C7 H7A 117.4 . . ? C7 C8 C9 118.2(6) . . ? C7 C8 H8A 120.9 . . ? C9 C8 H8A 120.9 . . ? C10 C9 C8 116.9(6) . . ? C10 C9 C12 123.4(6) . . ? C8 C9 C12 119.5(5) . . ? C11 C10 C9 120.7(6) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 N2 122.9(6) . . ? C10 C11 H11A 118.6 . . ? N2 C11 H11A 118.6 . . ? O5 C13 N3 122.7(16) . . ? O5 C13 H13A 118.6 . . ? N3 C13 H13A 118.6 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 C4 C5 N1 C1 -0.3(10) . . . . ? C4 C5 N1 Co1 170.6(5) . . . 2_565 ? N2 Co1 O1 C6 -12.1(11) . . . . ? O2 Co1 O1 C6 1.0(4) . . . . ? O4 Co1 O1 C6 -154.6(4) 2_475 . . . ? N1 Co1 O1 C6 98.7(4) 2_464 . . . ? O3 Co1 O1 C6 -93.9(4) 2_475 . . . ? C12 Co1 O1 C6 -123.7(4) 2_475 . . . ? N2 Co1 O2 C6 175.6(4) . . . . ? O4 Co1 O2 C6 49.3(6) 2_475 . . . ? N1 Co1 O2 C6 -85.1(4) 2_464 . . . ? O1 Co1 O2 C6 -1.0(4) . . . . ? O3 Co1 O2 C6 87.8(4) 2_475 . . . ? C12 Co1 O2 C6 73.0(4) 2_475 . . . ? O4 C12 O3 Co1 5.9(6) . . . 2_574 ? C9 C12 O3 Co1 -176.4(6) . . . 2_574 ? O3 C12 O4 Co1 -6.4(7) . . . 2_574 ? C9 C12 O4 Co1 175.8(5) . . . 2_574 ? O2 Co1 N2 C7 -39.8(5) . . . . ? O4 Co1 N2 C7 114.6(5) 2_475 . . . ? N1 Co1 N2 C7 -137.5(5) 2_464 . . . ? O1 Co1 N2 C7 -27.9(12) . . . . ? O3 Co1 N2 C7 54.5(5) 2_475 . . . ? C6 Co1 N2 C7 -36.5(7) . . . . ? C12 Co1 N2 C7 83.6(5) 2_475 . . . ? O2 Co1 N2 C11 150.0(5) . . . . ? O4 Co1 N2 C11 -55.7(5) 2_475 . . . ? N1 Co1 N2 C11 52.3(5) 2_464 . . . ? O1 Co1 N2 C11 161.8(7) . . . . ? O3 Co1 N2 C11 -115.7(5) 2_475 . . . ? C6 Co1 N2 C11 153.3(5) . . . . ? C12 Co1 N2 C11 -86.6(5) 2_475 . . . ? C5 N1 C1 C2 -0.4(11) . . . . ? Co1 N1 C1 C2 -172.0(6) 2_565 . . . ? N1 C1 C2 C3 0.4(11) . . . . ? C1 C2 C3 C4 0.3(11) . . . . ? C1 C2 C3 C6 179.6(7) . . . . ? C2 C3 C4 C5 -1.0(10) . . . . ? C6 C3 C4 C5 179.7(6) . . . . ? N1 C5 C4 C3 1.0(11) . . . . ? Co1 O1 C6 O2 -1.7(7) . . . . ? Co1 O1 C6 C3 -175.2(6) . . . . ? Co1 O2 C6 O1 1.8(8) . . . . ? Co1 O2 C6 C3 175.5(5) . . . . ? C4 C3 C6 O1 -8.0(11) . . . . ? C2 C3 C6 O1 172.7(7) . . . . ? C4 C3 C6 O2 178.1(6) . . . . ? C2 C3 C6 O2 -1.2(10) . . . . ? C4 C3 C6 Co1 -147(4) . . . . ? C2 C3 C6 Co1 33(4) . . . . ? N2 Co1 C6 O1 175.6(4) . . . . ? O2 Co1 C6 O1 -178.3(7) . . . . ? O4 Co1 C6 O1 30.4(5) 2_475 . . . ? N1 Co1 C6 O1 -81.2(4) 2_464 . . . ? O3 Co1 C6 O1 87.2(4) 2_475 . . . ? C12 Co1 C6 O1 61.0(4) 2_475 . . . ? N2 Co1 C6 O2 -6.1(6) . . . . ? O4 Co1 C6 O2 -151.3(4) 2_475 . . . ? N1 Co1 C6 O2 97.1(4) 2_464 . . . ? O1 Co1 C6 O2 178.3(7) . . . . ? O3 Co1 C6 O2 -94.5(4) 2_475 . . . ? C12 Co1 C6 O2 -120.7(4) 2_475 . . . ? N2 Co1 C6 C3 -43(4) . . . . ? O2 Co1 C6 C3 -37(4) . . . . ? O4 Co1 C6 C3 172(4) 2_475 . . . ? N1 Co1 C6 C3 60(4) 2_464 . . . ? O1 Co1 C6 C3 142(4) . . . . ? O3 Co1 C6 C3 -131(4) 2_475 . . . ? C12 Co1 C6 C3 -157(4) 2_475 . . . ? C11 N2 C7 C8 4.6(10) . . . . ? Co1 N2 C7 C8 -166.1(6) . . . . ? N2 C7 C8 C9 -2.4(11) . . . . ? C7 C8 C9 C10 0.2(10) . . . . ? C7 C8 C9 C12 175.1(6) . . . . ? O3 C12 C9 C10 -174.6(7) . . . . ? O4 C12 C9 C10 3.2(10) . . . . ? Co1 C12 C9 C10 36(5) 2_574 . . . ? O3 C12 C9 C8 11.0(10) . . . . ? O4 C12 C9 C8 -171.3(6) . . . . ? Co1 C12 C9 C8 -138(4) 2_574 . . . ? C8 C9 C10 C11 -0.6(10) . . . . ? C12 C9 C10 C11 -175.3(7) . . . . ? C9 C10 C11 N2 3.1(11) . . . . ? C7 N2 C11 C10 -4.9(10) . . . . ? Co1 N2 C11 C10 165.9(5) . . . . ? C15 N3 C13 O5 -178.8(14) . . . . ? C14 N3 C13 O5 1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.282 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.089