# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Balachandran Unni Nair' _publ_contact_author_email BCUNCHEM@REDIFFMAIL.COM _publ_section_title ; Biimidazole containing cobalt(III) mixed ligand complexes: Crystal structure and photonuclease activity ; loop_ _publ_author_name 'Balachandran Unni Nair' 'Ramasamy Indumathy' T.Weyhermuller # Attachment 'cobalt_bpy_complex.cif' data_5694 _database_code_depnum_ccdc_archive 'CCDC 630659' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C26 H22 Co N8]3+, 3 (Cl O4)-, 0.5 H2O, 0.5 MeCN' _chemical_formula_sum 'C27 H24.50 Cl3 Co N8.50 O12.50' _chemical_formula_weight 833.33 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 12.743(2) _cell_length_b 11.568(2) _cell_length_c 22.462(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.42(2) _cell_angle_gamma 90.00 _cell_volume 3275.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode, 50 kV, 80 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Kappa-CCD' _diffrn_measurement_method '935 images at 0.5 deg. stepwise rotation in omega and phi, 42 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18708 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4258 _reflns_number_gt 3042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS Collect Software' _computing_cell_refinement 'Bruker AXS Collect Software' _computing_data_reduction 'Bruker AXS Collect Software' _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^)+(0.1348P)^2^+24.9707P] 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 4258 _refine_ls_number_parameters 483 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1340 _refine_ls_R_factor_gt 0.1041 _refine_ls_wR_factor_ref 0.2979 _refine_ls_wR_factor_gt 0.2681 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.078 _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 0.78703(10) 0.26094(14) 0.06628(6) 0.0597(6) Uani 1 1 d . . . N1 N 0.8639(6) 0.3714(8) 0.1206(4) 0.061(2) Uani 1 1 d . . . C2 C 0.9668(8) 0.3960(11) 0.1264(5) 0.072(3) Uani 1 1 d . . . H2 H 1.0109 0.3494 0.1056 0.087 Uiso 1 1 calc R . . C3 C 1.0120(9) 0.4852(11) 0.1610(6) 0.075(3) Uani 1 1 d . . . H3 H 1.0858 0.5005 0.1640 0.090 Uiso 1 1 calc R . . C4 C 0.9498(9) 0.5508(11) 0.1907(6) 0.078(4) Uani 1 1 d . . . H4 H 0.9790 0.6151 0.2137 0.094 Uiso 1 1 calc R . . C5 C 0.8443(8) 0.5252(10) 0.1879(5) 0.065(3) Uani 1 1 d . . . H5 H 0.8005 0.5674 0.2110 0.078 Uiso 1 1 calc R . . C6 C 0.8033(8) 0.4358(10) 0.1505(5) 0.058(3) Uani 1 1 d . . . C7 C 0.6903(7) 0.4023(10) 0.1422(4) 0.057(3) Uani 1 1 d . . . C8 C 0.6140(8) 0.4480(10) 0.1714(5) 0.064(3) Uani 1 1 d . . . H8 H 0.6310 0.5071 0.2006 0.077 Uiso 1 1 calc R . . C9 C 0.5117(8) 0.4077(11) 0.1582(5) 0.073(3) Uani 1 1 d . . . H9 H 0.4578 0.4358 0.1795 0.088 Uiso 1 1 calc R . . C10 C 0.4892(8) 0.3275(13) 0.1144(5) 0.082(4) Uani 1 1 d . . . H10 H 0.4182 0.3016 0.1037 0.098 Uiso 1 1 calc R . . C11 C 0.5662(8) 0.2836(12) 0.0856(6) 0.078(4) Uani 1 1 d . . . H11 H 0.5487 0.2275 0.0549 0.093 Uiso 1 1 calc R . . N12 N 0.6669(6) 0.3183(9) 0.1000(4) 0.063(2) Uani 1 1 d . . . N21 N 0.9145(6) 0.2051(9) 0.0387(4) 0.063(2) Uani 1 1 d . . . C22 C 0.9593(9) 0.2454(11) -0.0060(6) 0.074(3) Uani 1 1 d . . . H22 H 0.9222 0.3030 -0.0309 0.088 Uiso 1 1 calc R . . C23 C 1.0553(9) 0.2106(12) -0.0191(6) 0.079(3) Uani 1 1 d . . . H23 H 1.0835 0.2409 -0.0528 0.094 Uiso 1 1 calc R . . C24 C 1.1091(8) 0.1308(13) 0.0177(7) 0.085(4) Uani 1 1 d . . . H24 H 1.1783 0.1079 0.0117 0.102 Uiso 1 1 calc R . . C25 C 1.0635(8) 0.0830(12) 0.0639(6) 0.081(4) Uani 1 1 d . . . H25 H 1.0999 0.0249 0.0888 0.097 Uiso 1 1 calc R . . C26 C 0.9641(7) 0.1203(11) 0.0737(5) 0.070(3) Uani 1 1 d . . . C27 C 0.9042(7) 0.0779(10) 0.1188(4) 0.060(3) Uani 1 1 d . . . C28 C 0.9300(9) -0.0163(12) 0.1543(6) 0.078(4) Uani 1 1 d . . . H28 H 0.9937 -0.0569 0.1510 0.094 Uiso 1 1 calc R . . C29 C 0.8678(10) -0.0536(11) 0.1939(5) 0.079(4) Uani 1 1 d . . . H29 H 0.8865 -0.1207 0.2175 0.095 Uiso 1 1 calc R . . C30 C 0.7738(9) 0.0088(11) 0.1998(5) 0.075(3) Uani 1 1 d . . . H30 H 0.7287 -0.0139 0.2279 0.090 Uiso 1 1 calc R . . C31 C 0.7512(8) 0.1015(11) 0.1640(5) 0.068(3) Uani 1 1 d . . . H31 H 0.6880 0.1434 0.1669 0.082 Uiso 1 1 calc R . . N32 N 0.8144(6) 0.1385(8) 0.1236(4) 0.060(2) Uani 1 1 d . . . N41 N 0.7579(7) 0.3727(10) 0.0036(4) 0.069(3) Uani 1 1 d . . . C42 C 0.7835(12) 0.4834(15) -0.0066(7) 0.100(5) Uani 1 1 d . . . H42 H 0.8254 0.5348 0.0200 0.120 Uiso 1 1 calc R . . C43 C 0.7321(18) 0.5062(19) -0.0679(8) 0.134(8) Uani 1 1 d . . . H43 H 0.7308 0.5779 -0.0886 0.161 Uiso 1 1 calc R . . N44 N 0.6879(16) 0.4087(17) -0.0892(6) 0.146(7) Uani 1 1 d . . . H44 H 0.6564 0.3987 -0.1264 0.175 Uiso 1 1 calc R . . C45 C 0.6971(12) 0.3285(16) -0.0474(5) 0.090(4) Uani 1 1 d . . . C46 C 0.6717(9) 0.2155(14) -0.0439(5) 0.076(4) Uani 1 1 d . . . N47 N 0.6133(8) 0.1389(15) -0.0808(5) 0.107(5) Uani 1 1 d . . . H47 H 0.5823 0.1533 -0.1177 0.128 Uiso 1 1 calc R . . C48 C 0.6105(8) 0.0360(18) -0.0514(7) 0.102(6) Uani 1 1 d . . . H48 H 0.5769 -0.0334 -0.0667 0.122 Uiso 1 1 calc R . . C49 C 0.6667(8) 0.0537(13) 0.0053(5) 0.078(4) Uani 1 1 d . . . H49 H 0.6778 -0.0019 0.0367 0.094 Uiso 1 1 calc R . . N50 N 0.7033(6) 0.1637(9) 0.0084(4) 0.066(3) Uani 1 1 d . . . Cl70 Cl 0.2452(2) 0.2683(3) -0.30795(13) 0.0682(9) Uani 1 1 d . . . O71 O 0.2804(7) 0.3305(10) -0.3546(4) 0.106(3) Uani 1 1 d . . . O72 O 0.3088(6) 0.2988(9) -0.2510(4) 0.103(3) Uani 1 1 d . . . O73 O 0.2600(6) 0.1473(9) -0.3161(4) 0.093(3) Uani 1 1 d . . . O74 O 0.1366(5) 0.2949(8) -0.3045(4) 0.083(2) Uani 1 1 d . . . Cl80 Cl 0.6522(2) 0.7412(3) 0.06752(13) 0.0665(8) Uani 1 1 d . . . O81 O 0.7469(6) 0.6799(9) 0.0851(5) 0.109(3) Uani 1 1 d . . . O82 O 0.6513(10) 0.8423(9) 0.1027(4) 0.114(3) Uani 1 1 d . . . O83 O 0.5668(7) 0.6706(9) 0.0770(5) 0.105(3) Uani 1 1 d . . . O84 O 0.6439(7) 0.7757(8) 0.0062(4) 0.094(3) Uani 1 1 d . . . Cl90 Cl 0.8302(8) 0.2081(10) -0.1902(5) 0.0590(13) Uani 0.50 1 d PD A 1 O91 O 0.9206(10) 0.1981(18) -0.2220(7) 0.072(4) Uani 0.50 1 d PD A 1 O92 O 0.7345(11) 0.1945(17) -0.2317(7) 0.087(4) Uani 0.50 1 d PD A 1 O93 O 0.8257(13) 0.3228(13) -0.1653(8) 0.086(4) Uani 0.50 1 d PD A 1 O94 O 0.8370(11) 0.1300(15) -0.1417(6) 0.081(4) Uani 0.50 1 d PD A 1 Cl95 Cl 0.8129(8) 0.2233(9) -0.1922(5) 0.0590(13) Uani 0.50 1 d PD B 2 O96 O 0.8791(12) 0.2286(17) -0.2392(7) 0.072(4) Uani 0.50 1 d PD B 2 O97 O 0.7519(12) 0.1188(14) -0.1982(8) 0.087(4) Uani 0.50 1 d PD B 2 O98 O 0.7359(12) 0.3159(13) -0.2003(7) 0.086(4) Uani 0.50 1 d PD B 2 O99 O 0.8733(11) 0.2350(17) -0.1347(6) 0.081(4) Uani 0.50 1 d PD B 2 N61 N 0.4734(11) 0.1370(13) -0.1850(6) 0.042(3) Uiso 0.50 1 d P C 1 C62 C 0.5107(13) 0.2064(15) -0.1978(7) 0.036(4) Uiso 0.50 1 d P C 1 C63 C 0.5743(13) 0.3408(14) -0.2078(8) 0.040(4) Uiso 0.50 1 d P C 1 H63A H 0.5515 0.3985 -0.1805 0.060 Uiso 0.50 1 calc PR C 1 H63B H 0.5549 0.3668 -0.2495 0.060 Uiso 0.50 1 calc PR C 1 H63C H 0.6514 0.3309 -0.1990 0.060 Uiso 0.50 1 calc PR C 1 O60 O 0.5095(12) -0.0657(13) -0.1978(7) 0.076(4) Uiso 0.50 1 d P D 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 0.0259(8) 0.0990(13) 0.0491(9) -0.0003(7) -0.0115(6) -0.0044(7) N1 0.022(4) 0.094(7) 0.063(5) -0.009(5) -0.014(4) -0.008(4) C2 0.039(6) 0.093(9) 0.079(8) 0.009(7) -0.011(5) -0.001(6) C3 0.037(6) 0.100(10) 0.083(8) 0.007(7) -0.012(6) -0.008(6) C4 0.041(6) 0.081(8) 0.105(10) 0.000(7) -0.015(6) -0.004(6) C5 0.041(6) 0.075(8) 0.074(7) -0.003(6) -0.003(5) -0.004(5) C6 0.042(6) 0.075(7) 0.052(6) 0.006(6) -0.012(5) 0.000(5) C7 0.035(5) 0.083(8) 0.048(6) 0.004(6) -0.010(5) 0.001(5) C8 0.038(6) 0.085(8) 0.066(7) -0.010(6) -0.007(5) -0.001(5) C9 0.040(6) 0.112(10) 0.063(7) -0.001(7) -0.008(5) -0.005(6) C10 0.034(6) 0.130(11) 0.077(8) -0.020(8) -0.006(6) -0.003(7) C11 0.036(6) 0.113(10) 0.078(8) -0.023(7) -0.013(6) -0.009(6) N12 0.024(4) 0.106(7) 0.054(5) -0.005(5) -0.011(4) -0.010(4) N21 0.028(4) 0.100(7) 0.055(5) -0.004(5) -0.006(4) -0.014(5) C22 0.049(7) 0.095(9) 0.075(8) -0.002(7) 0.002(6) -0.002(6) C23 0.048(7) 0.100(10) 0.088(9) -0.013(8) 0.011(6) -0.003(7) C24 0.024(6) 0.119(11) 0.112(11) -0.025(9) 0.006(7) -0.012(7) C25 0.027(6) 0.102(10) 0.105(10) -0.011(8) -0.018(6) -0.006(6) C26 0.026(5) 0.100(9) 0.077(8) -0.005(7) -0.017(5) -0.007(6) C27 0.022(5) 0.097(8) 0.051(6) 0.006(6) -0.024(4) -0.008(5) C28 0.049(7) 0.112(10) 0.068(8) 0.002(8) -0.008(6) -0.009(7) C29 0.069(8) 0.090(9) 0.065(8) 0.005(7) -0.033(6) -0.001(7) C30 0.058(7) 0.108(10) 0.050(6) 0.011(7) -0.016(5) -0.012(7) C31 0.039(6) 0.100(9) 0.062(7) -0.006(7) -0.003(5) -0.012(6) N32 0.028(4) 0.090(7) 0.055(5) -0.005(5) -0.015(4) -0.009(4) N41 0.042(5) 0.093(8) 0.071(6) -0.002(6) 0.007(4) 0.015(5) C42 0.087(10) 0.107(12) 0.113(12) 0.017(9) 0.035(9) 0.030(9) C43 0.20(2) 0.124(15) 0.089(13) 0.048(12) 0.050(13) 0.075(16) N44 0.225(19) 0.147(14) 0.060(8) 0.011(9) 0.000(9) 0.117(14) C45 0.100(11) 0.114(12) 0.050(8) -0.001(8) -0.007(7) 0.045(9) C46 0.040(6) 0.127(12) 0.053(7) -0.009(8) -0.017(5) 0.030(7) N47 0.052(7) 0.184(14) 0.072(8) -0.045(9) -0.032(6) 0.045(8) C48 0.019(5) 0.164(16) 0.112(12) -0.069(12) -0.026(6) 0.013(8) C49 0.025(5) 0.127(12) 0.078(8) -0.019(8) -0.008(5) 0.002(6) N50 0.031(4) 0.105(8) 0.058(6) -0.009(5) -0.012(4) -0.008(5) Cl70 0.0331(14) 0.102(2) 0.0648(18) -0.0033(16) -0.0087(12) -0.0001(13) O71 0.057(5) 0.159(9) 0.104(7) 0.058(7) 0.013(5) 0.017(5) O72 0.055(5) 0.161(9) 0.079(6) -0.030(6) -0.029(4) 0.005(5) O73 0.057(5) 0.117(8) 0.105(7) -0.016(6) 0.010(5) 0.003(5) O74 0.033(4) 0.121(7) 0.089(6) -0.003(5) -0.011(4) -0.001(4) Cl80 0.0399(15) 0.092(2) 0.0627(17) -0.0112(15) -0.0080(12) -0.0016(13) O81 0.035(4) 0.145(9) 0.138(8) -0.001(7) -0.012(5) 0.017(5) O82 0.158(10) 0.102(7) 0.077(6) -0.014(6) 0.001(6) 0.010(7) O83 0.062(5) 0.126(8) 0.128(8) 0.009(6) 0.015(5) -0.022(5) O84 0.084(6) 0.131(8) 0.061(5) -0.008(5) -0.013(4) -0.020(5) Cl90 0.036(3) 0.084(3) 0.0525(17) 0.0021(17) -0.0100(18) 0.003(2) O91 0.037(10) 0.106(11) 0.069(9) 0.004(7) -0.003(7) 0.000(8) O92 0.060(7) 0.129(14) 0.072(10) -0.015(7) 0.012(7) -0.032(8) O93 0.061(7) 0.095(9) 0.099(9) -0.031(8) 0.000(6) 0.005(7) O94 0.046(7) 0.134(12) 0.062(7) 0.009(9) 0.002(5) 0.016(7) Cl95 0.036(3) 0.084(3) 0.0525(17) 0.0021(17) -0.0100(18) 0.003(2) O96 0.037(10) 0.106(11) 0.069(9) 0.004(7) -0.003(7) 0.000(8) O97 0.060(7) 0.129(14) 0.072(10) -0.015(7) 0.012(7) -0.032(8) O98 0.061(7) 0.095(9) 0.099(9) -0.031(8) 0.000(6) 0.005(7) O99 0.046(7) 0.134(12) 0.062(7) 0.009(9) 0.002(5) 0.016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N41 1.907(11) . ? Co1 N32 1.912(9) . ? Co1 N50 1.921(9) . ? Co1 N12 1.923(9) . ? Co1 N21 1.932(9) . ? Co1 N1 1.932(8) . ? N1 C6 1.324(13) . ? N1 C2 1.329(13) . ? C2 C3 1.368(16) . ? C3 C4 1.342(17) . ? C4 C5 1.369(15) . ? C5 C6 1.385(15) . ? C6 C7 1.476(14) . ? C7 C8 1.358(14) . ? C7 N12 1.360(13) . ? C8 C9 1.375(14) . ? C9 C10 1.352(16) . ? C10 C11 1.351(16) . ? C11 N12 1.337(13) . ? N21 C22 1.312(14) . ? N21 C26 1.355(14) . ? C22 C23 1.361(16) . ? C23 C24 1.357(18) . ? C24 C25 1.376(18) . ? C25 C26 1.387(16) . ? C26 C27 1.440(16) . ? C27 N32 1.360(13) . ? C27 C28 1.361(16) . ? C28 C29 1.346(17) . ? C29 C30 1.422(17) . ? C30 C31 1.346(16) . ? C31 N32 1.365(14) . ? N41 C42 1.350(17) . ? N41 C45 1.385(16) . ? C42 C43 1.46(2) . ? C43 N44 1.32(2) . ? N44 C45 1.31(2) . ? C45 C46 1.35(2) . ? C46 N50 1.327(15) . ? C46 N47 1.360(17) . ? N47 C48 1.36(2) . ? C48 C49 1.382(17) . ? C49 N50 1.354(16) . ? Cl70 O71 1.397(9) . ? Cl70 O73 1.427(10) . ? Cl70 O74 1.432(8) . ? Cl70 O72 1.454(8) . ? Cl80 O83 1.402(9) . ? Cl80 O81 1.406(8) . ? Cl80 O82 1.412(10) . ? Cl80 O84 1.422(9) . ? Cl90 O94 1.409(13) . ? Cl90 O92 1.432(13) . ? Cl90 O93 1.445(14) . ? Cl90 O91 1.446(11) . ? Cl95 O99 1.409(13) . ? Cl95 O97 1.432(13) . ? Cl95 O98 1.446(14) . ? Cl95 O96 1.446(11) . ? N61 C62 0.997(18) . ? C62 C63 1.78(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N41 Co1 N32 174.9(4) . . ? N41 Co1 N50 82.5(4) . . ? N32 Co1 N50 92.9(4) . . ? N41 Co1 N12 88.6(4) . . ? N32 Co1 N12 93.9(4) . . ? N50 Co1 N12 94.2(4) . . ? N41 Co1 N21 94.1(4) . . ? N32 Co1 N21 83.6(4) . . ? N50 Co1 N21 89.9(4) . . ? N12 Co1 N21 175.4(3) . . ? N41 Co1 N1 92.5(4) . . ? N32 Co1 N1 92.2(4) . . ? N50 Co1 N1 174.4(4) . . ? N12 Co1 N1 83.2(4) . . ? N21 Co1 N1 93.0(4) . . ? C6 N1 C2 118.1(10) . . ? C6 N1 Co1 114.4(6) . . ? C2 N1 Co1 127.2(9) . . ? N1 C2 C3 122.9(12) . . ? C4 C3 C2 118.6(11) . . ? C3 C4 C5 120.1(12) . . ? C4 C5 C6 118.0(11) . . ? N1 C6 C5 122.1(9) . . ? N1 C6 C7 114.7(9) . . ? C5 C6 C7 123.2(10) . . ? C8 C7 N12 121.1(9) . . ? C8 C7 C6 126.2(10) . . ? N12 C7 C6 112.8(9) . . ? C7 C8 C9 119.1(11) . . ? C10 C9 C8 118.9(11) . . ? C11 C10 C9 120.9(11) . . ? N12 C11 C10 120.7(11) . . ? C11 N12 C7 119.1(10) . . ? C11 N12 Co1 126.4(8) . . ? C7 N12 Co1 114.5(6) . . ? C22 N21 C26 118.9(10) . . ? C22 N21 Co1 127.4(9) . . ? C26 N21 Co1 113.5(7) . . ? N21 C22 C23 124.5(13) . . ? C24 C23 C22 117.3(13) . . ? C23 C24 C25 120.2(11) . . ? C24 C25 C26 119.4(12) . . ? N21 C26 C25 119.5(12) . . ? N21 C26 C27 113.9(9) . . ? C25 C26 C27 126.6(12) . . ? N32 C27 C28 120.0(10) . . ? N32 C27 C26 114.8(10) . . ? C28 C27 C26 125.2(11) . . ? C29 C28 C27 121.9(12) . . ? C28 C29 C30 119.0(12) . . ? C31 C30 C29 117.2(12) . . ? C30 C31 N32 123.5(11) . . ? C27 N32 C31 118.4(10) . . ? C27 N32 Co1 113.6(7) . . ? C31 N32 Co1 127.8(8) . . ? C42 N41 C45 109.2(12) . . ? C42 N41 Co1 138.0(10) . . ? C45 N41 Co1 112.7(10) . . ? N41 C42 C43 104.3(16) . . ? N44 C43 C42 107.2(15) . . ? C45 N44 C43 110.9(15) . . ? N44 C45 C46 136.8(15) . . ? N44 C45 N41 108.2(16) . . ? C46 C45 N41 114.7(12) . . ? N50 C46 C45 116.5(11) . . ? N50 C46 N47 108.3(14) . . ? C45 C46 N47 135.1(13) . . ? C46 N47 C48 108.9(12) . . ? N47 C48 C49 105.7(14) . . ? N50 C49 C48 108.4(14) . . ? C46 N50 C49 108.7(10) . . ? C46 N50 Co1 113.6(9) . . ? C49 N50 Co1 137.7(8) . . ? O71 Cl70 O73 110.3(6) . . ? O71 Cl70 O74 110.4(5) . . ? O73 Cl70 O74 111.4(5) . . ? O71 Cl70 O72 109.6(6) . . ? O73 Cl70 O72 106.5(6) . . ? O74 Cl70 O72 108.6(5) . . ? O83 Cl80 O81 108.5(6) . . ? O83 Cl80 O82 109.1(7) . . ? O81 Cl80 O82 109.7(7) . . ? O83 Cl80 O84 111.2(6) . . ? O81 Cl80 O84 110.6(6) . . ? O82 Cl80 O84 107.7(6) . . ? O94 Cl90 O92 112.5(12) . . ? O94 Cl90 O93 106.9(10) . . ? O92 Cl90 O93 105.9(10) . . ? O94 Cl90 O91 111.6(10) . . ? O92 Cl90 O91 109.5(9) . . ? O93 Cl90 O91 110.2(10) . . ? O99 Cl95 O97 112.6(12) . . ? O99 Cl95 O98 108.3(10) . . ? O97 Cl95 O98 105.4(11) . . ? O99 Cl95 O96 111.5(10) . . ? O97 Cl95 O96 109.4(10) . . ? O98 Cl95 O96 109.5(10) . . ? N61 C62 C63 169.6(18) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.355 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.113 # Attachment 'cobalt_phen_complex.cif' data_6251 _database_code_depnum_ccdc_archive 'CCDC 692975' #TrackingRef 'cobalt_phen_complex.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C30 H22 Co N8)3+, 0.5 (O3 H7)+, 3.5 (Cl O4)-, (H2 O)' _chemical_formula_sum 'C30 H27.50 Cl3.50 Co N8 O16.50' _chemical_formula_weight 947.11 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7117(6) _cell_length_b 13.0089(6) _cell_length_c 14.0170(7) _cell_angle_alpha 85.538(2) _cell_angle_beta 68.407(2) _cell_angle_gamma 79.239(2) _cell_volume 1784.13(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent fragment' _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 0.834 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7762 _exptl_absorpt_correction_T_max 0.8922 _exptl_absorpt_process_details 'Bruker, SADABS 2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '1441 images at 1.0 deg.stepwise rotation in omega and phi, 40 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62891 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 30.00 _reflns_number_total 10370 _reflns_number_gt 9283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS Collect Software' _computing_cell_refinement 'Bruker AXS Collect Software' _computing_data_reduction 'Bruker AXS Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+5.0153P] 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 10370 _refine_ls_number_parameters 622 _refine_ls_number_restraints 211 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1699 _refine_ls_wR_factor_gt 0.1652 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.062 _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 0.23925(4) 0.24090(3) 1.25332(3) 0.02211(10) Uani 1 1 d . . . N1 N 0.3289(3) 0.19386(18) 1.35129(18) 0.0253(5) Uani 1 1 d . . . C2 C 0.3032(3) 0.1974(2) 1.4551(2) 0.0292(6) Uani 1 1 d . . . H2 H 0.2220 0.2313 1.5054 0.035 Uiso 1 1 calc R . . C3 C 0.4164(4) 0.1431(3) 1.4727(3) 0.0343(7) Uani 1 1 d . . . H3 H 0.4281 0.1334 1.5369 0.041 Uiso 1 1 calc R . . N4 N 0.5090(3) 0.1056(2) 1.3794(2) 0.0335(6) Uani 1 1 d . . . H4 H 0.5899 0.0674 1.3682 0.040 Uiso 1 1 calc R . . C5 C 0.4532(4) 0.1381(2) 1.3087(2) 0.0299(6) Uani 1 1 d . . . C6 C 0.4996(4) 0.1280(2) 1.1995(3) 0.0327(6) Uani 1 1 d . . . N7 N 0.6149(4) 0.0861(3) 1.1276(3) 0.0522(9) Uani 1 1 d . . . H7 H 0.6879 0.0513 1.1377 0.063 Uiso 1 1 calc R . . C8 C 0.5999(5) 0.1070(4) 1.0342(3) 0.0564(12) Uani 1 1 d . . . H8 H 0.6668 0.0871 0.9689 0.068 Uiso 1 1 calc R . . C9 C 0.4715(4) 0.1615(3) 1.0524(3) 0.0390(7) Uani 1 1 d . . . H9 H 0.4323 0.1861 1.0023 0.047 Uiso 1 1 calc R . . N10 N 0.4094(3) 0.17409(19) 1.15701(19) 0.0283(5) Uani 1 1 d . . . N21 N 0.1708(3) 0.28611(19) 1.14350(18) 0.0249(5) Uani 1 1 d . . . C22 C 0.1005(3) 0.2389(2) 1.1042(2) 0.0312(6) Uani 1 1 d . . . H22 H 0.0717 0.1754 1.1345 0.037 Uiso 1 1 calc R . . C23 C 0.0680(4) 0.2810(3) 1.0190(3) 0.0361(7) Uani 1 1 d . . . H23 H 0.0173 0.2461 0.9928 0.043 Uiso 1 1 calc R . . C24 C 0.1093(3) 0.3727(3) 0.9737(2) 0.0332(6) Uani 1 1 d . . . H24 H 0.0889 0.4007 0.9154 0.040 Uiso 1 1 calc R . . C25 C 0.1821(3) 0.4246(2) 1.0148(2) 0.0285(6) Uani 1 1 d . . . C26 C 0.2290(3) 0.5221(3) 0.9753(2) 0.0331(6) Uani 1 1 d . . . H26 H 0.2128 0.5538 0.9167 0.040 Uiso 1 1 calc R . . C27 C 0.2960(3) 0.5692(3) 1.0206(2) 0.0332(6) Uani 1 1 d . . . H27 H 0.3234 0.6343 0.9942 0.040 Uiso 1 1 calc R . . C28 C 0.3261(3) 0.5218(2) 1.1082(2) 0.0268(5) Uani 1 1 d . . . C29 C 0.3953(3) 0.5644(2) 1.1601(3) 0.0314(6) Uani 1 1 d . . . H29 H 0.4248 0.6297 1.1389 0.038 Uiso 1 1 calc R . . C30 C 0.4194(3) 0.5107(2) 1.2414(3) 0.0295(6) Uani 1 1 d . . . H30 H 0.4666 0.5386 1.2762 0.035 Uiso 1 1 calc R . . C31 C 0.3745(3) 0.4143(2) 1.2735(2) 0.0242(5) Uani 1 1 d . . . H31 H 0.3922 0.3780 1.3299 0.029 Uiso 1 1 calc R . . N32 N 0.3077(2) 0.37283(17) 1.22649(17) 0.0212(4) Uani 1 1 d . . . C33 C 0.2837(3) 0.4258(2) 1.1453(2) 0.0223(5) Uani 1 1 d . . . C34 C 0.2101(3) 0.3781(2) 1.0999(2) 0.0234(5) Uani 1 1 d . . . N41 N 0.1602(3) 0.11278(19) 1.2822(2) 0.0301(5) Uani 1 1 d . . . C42 C 0.2104(4) 0.0185(2) 1.2392(3) 0.0363(7) Uani 1 1 d . . . H42 H 0.2974 0.0073 1.1858 0.044 Uiso 1 1 calc R . . C43 C 0.1370(5) -0.0640(3) 1.2716(3) 0.0474(10) Uani 1 1 d . . . H43 H 0.1752 -0.1300 1.2394 0.057 Uiso 1 1 calc R . . C44 C 0.0116(5) -0.0523(3) 1.3483(3) 0.0487(10) Uani 1 1 d . . . H44 H -0.0372 -0.1090 1.3696 0.058 Uiso 1 1 calc R . . C45 C -0.0421(4) 0.0450(3) 1.3941(3) 0.0420(9) Uani 1 1 d . . . C46 C -0.1760(5) 0.0693(4) 1.4770(3) 0.0492(10) Uani 1 1 d . . . H46 H -0.2295 0.0159 1.5039 0.059 Uiso 1 1 calc R . . C47 C -0.2237(4) 0.1677(4) 1.5152(3) 0.0485(10) Uani 1 1 d . . . H47 H -0.3108 0.1822 1.5680 0.058 Uiso 1 1 calc R . . C48 C -0.1432(4) 0.2516(3) 1.4763(2) 0.0377(7) Uani 1 1 d . . . C49 C -0.1909(4) 0.3550(4) 1.5091(3) 0.0436(8) Uani 1 1 d . . . H49 H -0.2775 0.3739 1.5615 0.052 Uiso 1 1 calc R . . C50 C -0.1102(4) 0.4287(3) 1.4642(3) 0.0407(8) Uani 1 1 d . . . H50 H -0.1416 0.4998 1.4840 0.049 Uiso 1 1 calc R . . C51 C 0.0182(3) 0.3987(2) 1.3893(2) 0.0296(6) Uani 1 1 d . . . H51 H 0.0731 0.4508 1.3598 0.036 Uiso 1 1 calc R . . N52 N 0.0675(3) 0.30046(19) 1.35735(18) 0.0244(4) Uani 1 1 d . . . C53 C -0.0152(3) 0.2275(2) 1.4002(2) 0.0292(6) Uani 1 1 d . . . C54 C 0.0360(3) 0.1259(2) 1.3587(2) 0.0303(6) Uani 1 1 d . . . Cl7 Cl 0.27293(7) 0.70532(6) 0.72839(5) 0.02868(15) Uani 1 1 d D . . O71 O 0.3311(2) 0.6987(2) 0.80657(18) 0.0371(5) Uani 1 1 d D . . O72 O 0.1914(3) 0.80607(19) 0.7302(2) 0.0468(7) Uani 1 1 d D . . O73 O 0.3825(3) 0.6884(3) 0.62923(19) 0.0545(8) Uani 1 1 d D . . O74 O 0.1903(3) 0.62497(19) 0.74489(19) 0.0389(5) Uani 1 1 d D . . Cl6 Cl 1.46873(11) 0.18767(8) 0.76881(10) 0.0367(2) Uani 0.856(3) 1 d PD A 1 O61 O 1.5084(4) 0.1019(3) 0.6966(3) 0.0468(9) Uani 0.856(3) 1 d PD A 1 O62 O 1.3441(4) 0.1813(5) 0.8501(3) 0.0891(16) Uani 0.856(3) 1 d PD A 1 O63 O 1.4728(6) 0.2847(3) 0.7122(4) 0.0843(16) Uani 0.856(3) 1 d PD A 1 O64 O 1.5735(4) 0.1803(3) 0.8132(3) 0.0587(10) Uani 0.856(3) 1 d PD A 1 Cl8 Cl 1.0325(2) 0.31919(18) 0.72773(16) 0.0378(3) Uani 0.764(4) 1 d PD B 1 O81 O 1.0374(9) 0.4205(5) 0.7589(6) 0.0584(11) Uani 0.764(4) 1 d PD B 1 O82 O 1.1623(5) 0.2504(5) 0.7027(4) 0.0798(16) Uani 0.764(4) 1 d PD B 1 O83 O 0.9983(5) 0.3303(4) 0.6364(3) 0.0653(13) Uani 0.764(4) 1 d PD B 1 O84 O 0.9370(5) 0.2709(4) 0.8113(3) 0.0636(13) Uani 0.764(4) 1 d PD B 1 Cl9 Cl 0.0247(14) 0.9949(10) 1.0057(8) 0.0391(11) Uani 0.327(9) 1 d PD . 1 O91 O 0.1346(19) 1.0532(16) 0.958(3) 0.075(4) Uani 0.327(9) 1 d PD . 1 O92 O 0.0767(15) 0.8940(9) 1.0369(14) 0.074(5) Uani 0.327(9) 1 d PD . 1 O93 O -0.041(4) 0.987(2) 0.9342(19) 0.072(5) Uani 0.327(9) 1 d PD . 1 O94 O -0.0689(13) 1.0539(10) 1.0948(9) 0.059(3) Uani 0.327(9) 1 d PD . 1 Cl6X Cl 1.5072(7) 0.1920(5) 0.7247(6) 0.0367(2) Uani 0.144(3) 1 d PD A 2 O61X O 1.556(2) 0.0870(10) 0.6837(19) 0.0468(9) Uani 0.144(3) 1 d PD A 2 O62X O 1.505(2) 0.193(2) 0.8272(9) 0.0891(16) Uani 0.144(3) 1 d PD A 2 O63X O 1.3683(13) 0.2215(15) 0.7274(19) 0.0843(16) Uani 0.144(3) 1 d PD A 2 O64X O 1.5974(17) 0.2581(13) 0.6582(13) 0.0587(10) Uani 0.144(3) 1 d PD A 2 Cl8X Cl 1.0124(8) 0.3354(7) 0.7176(6) 0.0378(3) Uani 0.236(4) 1 d PD B 2 O81X O 1.024(3) 0.4247(14) 0.7681(19) 0.0584(11) Uani 0.236(4) 1 d PD B 2 O82X O 1.1316(11) 0.3104(14) 0.6292(9) 0.0798(16) Uani 0.236(4) 1 d PD B 2 O83X O 0.8906(11) 0.3613(12) 0.6958(10) 0.0653(13) Uani 0.236(4) 1 d PD B 2 O84X O 1.0060(16) 0.2489(10) 0.7899(10) 0.0636(13) Uani 0.236(4) 1 d PD B 2 Cl9X Cl 0.009(3) 1.002(2) 1.0033(17) 0.0391(11) Uani 0.173(9) 1 d PD . 2 O91X O 0.138(3) 1.039(3) 0.969(5) 0.075(4) Uani 0.173(9) 1 d PD . 2 O92X O 0.013(3) 0.915(2) 1.071(3) 0.074(5) Uani 0.173(9) 1 d PD . 2 O93X O -0.016(8) 0.975(4) 0.915(3) 0.072(5) Uani 0.173(9) 1 d PD . 2 O94X O -0.094(3) 1.0878(17) 1.0578(19) 0.059(3) Uani 0.173(9) 1 d PD . 2 O100 O 0.7549(3) -0.0229(3) 1.2741(3) 0.0566(8) Uani 1 1 d D . . H101 H 0.827(4) -0.010(4) 1.235(4) 0.068 Uiso 1 1 d D . . H102 H 0.783(6) -0.070(4) 1.305(4) 0.068 Uiso 1 1 d D . . O200 O 1.3410(7) 0.4422(5) 0.6474(6) 0.0596(17) Uani 0.50 1 d P . . O210 O 1.3377(7) 0.4069(6) 0.5935(6) 0.0605(17) Uani 0.50 1 d P . . O300 O 1.4933(8) 0.4667(6) 0.4688(6) 0.0643(18) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0322(2) 0.01780(17) 0.02160(18) 0.00147(12) -0.01478(15) -0.00723(13) N1 0.0383(13) 0.0205(10) 0.0238(11) 0.0038(8) -0.0179(10) -0.0092(9) C2 0.0407(16) 0.0297(14) 0.0236(13) 0.0072(10) -0.0150(12) -0.0174(12) C3 0.0504(19) 0.0333(15) 0.0306(15) 0.0119(12) -0.0241(14) -0.0199(14) N4 0.0437(15) 0.0277(12) 0.0380(14) 0.0062(10) -0.0262(12) -0.0063(11) C5 0.0447(17) 0.0213(12) 0.0308(14) 0.0020(10) -0.0226(13) -0.0054(11) C6 0.0430(17) 0.0255(13) 0.0322(15) -0.0062(11) -0.0196(13) 0.0029(12) N7 0.0517(19) 0.057(2) 0.0436(18) -0.0223(15) -0.0243(16) 0.0243(16) C8 0.058(3) 0.068(3) 0.0358(19) -0.0250(19) -0.0166(18) 0.017(2) C9 0.050(2) 0.0405(17) 0.0257(14) -0.0105(13) -0.0159(14) 0.0039(15) N10 0.0409(14) 0.0231(11) 0.0245(11) -0.0027(9) -0.0170(10) -0.0021(10) N21 0.0326(12) 0.0233(11) 0.0234(11) -0.0001(8) -0.0148(9) -0.0056(9) C22 0.0432(17) 0.0297(14) 0.0298(14) -0.0005(11) -0.0218(13) -0.0100(12) C23 0.0459(18) 0.0401(17) 0.0315(15) -0.0033(13) -0.0245(14) -0.0064(14) C24 0.0385(16) 0.0401(16) 0.0239(13) -0.0003(12) -0.0174(12) -0.0014(13) C25 0.0308(14) 0.0316(14) 0.0217(12) 0.0019(10) -0.0109(11) 0.0003(11) C26 0.0331(15) 0.0363(16) 0.0258(14) 0.0092(12) -0.0098(12) -0.0020(12) C27 0.0344(15) 0.0299(14) 0.0309(15) 0.0104(12) -0.0084(12) -0.0064(12) C28 0.0257(13) 0.0232(12) 0.0292(13) 0.0048(10) -0.0074(11) -0.0057(10) C29 0.0308(14) 0.0246(13) 0.0381(16) 0.0045(11) -0.0100(12) -0.0100(11) C30 0.0275(13) 0.0269(13) 0.0373(15) -0.0012(11) -0.0133(12) -0.0086(11) C31 0.0246(12) 0.0241(12) 0.0265(12) -0.0006(10) -0.0117(10) -0.0053(10) N32 0.0248(10) 0.0181(9) 0.0224(10) 0.0008(8) -0.0103(8) -0.0042(8) C33 0.0234(12) 0.0215(11) 0.0216(11) 0.0019(9) -0.0082(9) -0.0034(9) C34 0.0259(12) 0.0241(12) 0.0201(11) 0.0005(9) -0.0088(10) -0.0032(10) N41 0.0486(15) 0.0215(11) 0.0329(13) 0.0043(9) -0.0271(12) -0.0125(10) C42 0.057(2) 0.0244(14) 0.0399(17) 0.0025(12) -0.0297(16) -0.0128(14) C43 0.076(3) 0.0286(16) 0.058(2) 0.0101(15) -0.045(2) -0.0206(17) C44 0.068(3) 0.0406(19) 0.059(2) 0.0198(17) -0.042(2) -0.0292(19) C45 0.059(2) 0.0377(17) 0.052(2) 0.0234(15) -0.0409(19) -0.0282(16) C46 0.056(2) 0.059(2) 0.046(2) 0.0230(18) -0.0298(19) -0.029(2) C47 0.046(2) 0.071(3) 0.0354(18) 0.0175(18) -0.0174(16) -0.0265(19) C48 0.0422(18) 0.053(2) 0.0252(14) 0.0074(13) -0.0185(13) -0.0151(15) C49 0.0391(18) 0.066(2) 0.0291(16) -0.0048(16) -0.0140(14) -0.0125(17) C50 0.0371(17) 0.054(2) 0.0342(16) -0.0115(15) -0.0161(14) -0.0054(15) C51 0.0309(14) 0.0329(14) 0.0307(14) -0.0048(11) -0.0164(12) -0.0063(11) N52 0.0288(11) 0.0273(11) 0.0228(10) 0.0032(9) -0.0133(9) -0.0118(9) C53 0.0362(15) 0.0349(15) 0.0263(13) 0.0096(11) -0.0196(12) -0.0167(12) C54 0.0413(16) 0.0302(14) 0.0320(14) 0.0123(11) -0.0246(13) -0.0181(12) Cl7 0.0312(3) 0.0325(3) 0.0278(3) 0.0091(3) -0.0141(3) -0.0153(3) O71 0.0373(12) 0.0471(14) 0.0351(12) 0.0066(10) -0.0216(10) -0.0120(10) O72 0.0627(18) 0.0322(12) 0.0577(17) 0.0110(11) -0.0383(15) -0.0080(12) O73 0.0416(15) 0.093(2) 0.0284(12) 0.0065(14) -0.0062(11) -0.0272(15) O74 0.0486(14) 0.0369(12) 0.0377(12) 0.0044(10) -0.0159(11) -0.0242(11) Cl6 0.0348(5) 0.0395(5) 0.0305(6) 0.0002(4) -0.0071(5) -0.0034(4) O61 0.060(2) 0.0473(17) 0.0386(17) -0.0015(13) -0.0127(19) -0.0316(17) O62 0.051(2) 0.137(5) 0.062(3) -0.015(3) 0.002(2) -0.015(3) O63 0.126(4) 0.044(2) 0.115(4) 0.022(2) -0.078(4) -0.031(2) O64 0.054(2) 0.061(2) 0.068(2) -0.0193(19) -0.0311(19) 0.0005(18) Cl8 0.0454(8) 0.0443(9) 0.0307(6) -0.0053(5) -0.0224(5) -0.0045(6) O81 0.102(3) 0.0415(16) 0.056(2) 0.0106(14) -0.052(2) -0.0255(18) O82 0.063(3) 0.108(4) 0.059(3) -0.025(3) -0.029(2) 0.032(3) O83 0.080(3) 0.078(3) 0.056(2) -0.021(2) -0.051(2) 0.008(2) O84 0.074(4) 0.052(2) 0.056(3) -0.0054(19) -0.007(2) -0.021(3) Cl9 0.033(3) 0.0445(18) 0.0420(12) -0.0085(10) -0.0122(15) -0.0104(18) O91 0.032(3) 0.031(6) 0.134(10) -0.012(5) -0.001(4) 0.004(3) O92 0.063(9) 0.071(7) 0.120(13) 0.042(8) -0.065(10) -0.038(7) O93 0.117(16) 0.041(7) 0.090(10) -0.018(5) -0.078(13) 0.001(6) O94 0.067(7) 0.055(7) 0.046(7) -0.014(5) -0.006(5) -0.016(6) Cl6X 0.0348(5) 0.0395(5) 0.0305(6) 0.0002(4) -0.0071(5) -0.0034(4) O61X 0.060(2) 0.0473(17) 0.0386(17) -0.0015(13) -0.0127(19) -0.0316(17) O62X 0.051(2) 0.137(5) 0.062(3) -0.015(3) 0.002(2) -0.015(3) O63X 0.126(4) 0.044(2) 0.115(4) 0.022(2) -0.078(4) -0.031(2) O64X 0.054(2) 0.061(2) 0.068(2) -0.0193(19) -0.0311(19) 0.0005(18) Cl8X 0.0454(8) 0.0443(9) 0.0307(6) -0.0053(5) -0.0224(5) -0.0045(6) O81X 0.102(3) 0.0415(16) 0.056(2) 0.0106(14) -0.052(2) -0.0255(18) O82X 0.063(3) 0.108(4) 0.059(3) -0.025(3) -0.029(2) 0.032(3) O83X 0.080(3) 0.078(3) 0.056(2) -0.021(2) -0.051(2) 0.008(2) O84X 0.074(4) 0.052(2) 0.056(3) -0.0054(19) -0.007(2) -0.021(3) Cl9X 0.033(3) 0.0445(18) 0.0420(12) -0.0085(10) -0.0122(15) -0.0104(18) O91X 0.032(3) 0.031(6) 0.134(10) -0.012(5) -0.001(4) 0.004(3) O92X 0.063(9) 0.071(7) 0.120(13) 0.042(8) -0.065(10) -0.038(7) O93X 0.117(16) 0.041(7) 0.090(10) -0.018(5) -0.078(13) 0.001(6) O94X 0.067(7) 0.055(7) 0.046(7) -0.014(5) -0.006(5) -0.016(6) O100 0.0338(14) 0.0543(18) 0.080(2) -0.0048(16) -0.0139(14) -0.0150(13) O200 0.052(4) 0.039(3) 0.087(5) -0.016(3) -0.022(4) -0.003(3) O210 0.059(4) 0.060(4) 0.072(5) 0.018(4) -0.032(4) -0.024(3) O300 0.075(5) 0.061(4) 0.064(4) -0.012(3) -0.037(4) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N10 1.919(3) . ? Co1 N52 1.944(3) . ? Co1 N21 1.945(2) . ? Co1 N32 1.947(2) . ? Co1 N1 1.950(2) . ? Co1 N41 1.957(2) . ? N1 C5 1.333(4) . ? N1 C2 1.380(4) . ? C2 C3 1.380(5) . ? C3 N4 1.378(5) . ? N4 C5 1.339(4) . ? C5 C6 1.434(4) . ? C6 N7 1.325(5) . ? C6 N10 1.341(4) . ? N7 C8 1.377(5) . ? C8 C9 1.367(6) . ? C9 N10 1.378(4) . ? N21 C22 1.333(4) . ? N21 C34 1.366(4) . ? C22 C23 1.407(4) . ? C23 C24 1.377(5) . ? C24 C25 1.409(4) . ? C25 C34 1.402(4) . ? C25 C26 1.446(4) . ? C26 C27 1.361(5) . ? C27 C28 1.447(4) . ? C28 C33 1.406(4) . ? C28 C29 1.413(4) . ? C29 C30 1.370(4) . ? C30 C31 1.408(4) . ? C31 N32 1.336(3) . ? N32 C33 1.364(3) . ? C33 C34 1.423(4) . ? N41 C42 1.337(4) . ? N41 C54 1.358(4) . ? C42 C43 1.397(5) . ? C43 C44 1.367(7) . ? C44 C45 1.388(6) . ? C45 C54 1.413(4) . ? C45 C46 1.472(6) . ? C46 C47 1.359(7) . ? C47 C48 1.466(5) . ? C48 C53 1.390(5) . ? C48 C49 1.396(6) . ? C49 C50 1.369(6) . ? C50 C51 1.396(5) . ? C51 N52 1.333(4) . ? N52 C53 1.371(4) . ? C53 C54 1.413(5) . ? Cl7 O72 1.429(3) . ? Cl7 O71 1.437(2) . ? Cl7 O74 1.445(2) . ? Cl7 O73 1.452(3) . ? Cl6 O62 1.412(4) . ? Cl6 O63 1.437(4) . ? Cl6 O64 1.456(3) . ? Cl6 O61 1.461(3) . ? Cl8 O84 1.434(4) . ? Cl8 O81 1.436(4) . ? Cl8 O82 1.443(4) . ? Cl8 O83 1.445(4) . ? Cl9 Cl9 0.60(3) 2_577 ? Cl9 O93 0.97(3) 2_577 ? Cl9 O92 1.428(7) . ? Cl9 O93 1.439(7) . ? Cl9 O91 1.442(6) . ? Cl9 O94 1.448(7) . ? Cl9 O94 1.466(19) 2_577 ? Cl9 O91 1.81(4) 2_577 ? Cl9 O92 1.84(2) 2_577 ? O91 O93 1.59(3) 2_577 ? O91 Cl9 1.81(4) 2_577 ? O92 O93 1.57(3) 2_577 ? O92 Cl9 1.84(2) 2_577 ? O93 Cl9 0.97(3) 2_577 ? O93 O94 1.13(3) 2_577 ? O93 O92 1.57(3) 2_577 ? O93 O91 1.59(3) 2_577 ? O94 O93 1.13(3) 2_577 ? O94 Cl9 1.466(19) 2_577 ? Cl6X O62X 1.430(8) . ? Cl6X O64X 1.436(8) . ? Cl6X O61X 1.451(7) . ? Cl6X O63X 1.453(7) . ? Cl8X O82X 1.420(7) . ? Cl8X O83X 1.422(7) . ? Cl8X O84X 1.448(7) . ? Cl8X O81X 1.455(7) . ? Cl9X Cl9X 0.26(8) 2_577 ? Cl9X O93X 1.23(5) 2_577 ? Cl9X O92X 1.427(8) . ? Cl9X O93X 1.440(8) . ? Cl9X O91X 1.446(7) . ? Cl9X O94X 1.447(8) . ? Cl9X O94X 1.46(4) 2_577 ? Cl9X O92X 1.49(5) 2_577 ? Cl9X O91X 1.66(8) 2_577 ? O91X Cl9X 1.66(8) 2_577 ? O91X O93X 1.69(5) 2_577 ? O92X O93X 1.48(6) 2_577 ? O92X Cl9X 1.49(5) 2_577 ? O92X O94X 1.69(4) 2_577 ? O93X Cl9X 1.23(5) 2_577 ? O93X O94X 1.46(5) 2_577 ? O93X O92X 1.48(6) 2_577 ? O93X O91X 1.69(5) 2_577 ? O94X Cl9X 1.46(4) 2_577 ? O94X O93X 1.46(5) 2_577 ? O94X O92X 1.69(4) 2_577 ? O200 O210 0.928(9) . ? O300 O300 1.339(13) 2_866 ? 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 N10 Co1 N52 176.03(10) . . ? N10 Co1 N21 91.18(10) . . ? N52 Co1 N21 91.90(10) . . ? N10 Co1 N32 89.28(10) . . ? N52 Co1 N32 93.50(10) . . ? N21 Co1 N32 84.55(10) . . ? N10 Co1 N1 82.63(11) . . ? N52 Co1 N1 94.39(10) . . ? N21 Co1 N1 173.38(11) . . ? N32 Co1 N1 93.01(10) . . ? N10 Co1 N41 93.54(12) . . ? N52 Co1 N41 83.76(11) . . ? N21 Co1 N41 93.90(10) . . ? N32 Co1 N41 176.81(11) . . ? N1 Co1 N41 88.83(10) . . ? C5 N1 C2 106.8(3) . . ? C5 N1 Co1 113.43(19) . . ? C2 N1 Co1 139.8(2) . . ? N1 C2 C3 107.9(3) . . ? N4 C3 C2 106.9(3) . . ? C5 N4 C3 107.3(3) . . ? N1 C5 N4 111.1(3) . . ? N1 C5 C6 114.9(3) . . ? N4 C5 C6 134.0(3) . . ? N7 C6 N10 110.3(3) . . ? N7 C6 C5 134.9(3) . . ? N10 C6 C5 114.7(3) . . ? C6 N7 C8 107.5(3) . . ? C9 C8 N7 107.7(3) . . ? C8 C9 N10 107.1(3) . . ? C6 N10 C9 107.4(3) . . ? C6 N10 Co1 114.3(2) . . ? C9 N10 Co1 138.2(2) . . ? C22 N21 C34 118.5(2) . . ? C22 N21 Co1 129.9(2) . . ? C34 N21 Co1 111.48(18) . . ? N21 C22 C23 121.5(3) . . ? C24 C23 C22 120.3(3) . . ? C23 C24 C25 119.1(3) . . ? C34 C25 C24 117.3(3) . . ? C34 C25 C26 118.3(3) . . ? C24 C25 C26 124.5(3) . . ? C27 C26 C25 121.3(3) . . ? C26 C27 C28 121.0(3) . . ? C33 C28 C29 116.9(3) . . ? C33 C28 C27 117.9(3) . . ? C29 C28 C27 125.2(3) . . ? C30 C29 C28 119.4(3) . . ? C29 C30 C31 120.3(3) . . ? N32 C31 C30 121.5(3) . . ? C31 N32 C33 118.5(2) . . ? C31 N32 Co1 129.58(19) . . ? C33 N32 Co1 111.86(18) . . ? N32 C33 C28 123.3(3) . . ? N32 C33 C34 115.6(2) . . ? C28 C33 C34 121.0(3) . . ? N21 C34 C25 123.3(3) . . ? N21 C34 C33 116.3(2) . . ? C25 C34 C33 120.4(3) . . ? C42 N41 C54 118.0(3) . . ? C42 N41 Co1 129.9(3) . . ? C54 N41 Co1 112.0(2) . . ? N41 C42 C43 121.0(4) . . ? C44 C43 C42 121.9(4) . . ? C43 C44 C45 118.0(3) . . ? C44 C45 C54 118.1(4) . . ? C44 C45 C46 124.1(3) . . ? C54 C45 C46 117.9(4) . . ? C47 C46 C45 120.5(4) . . ? C46 C47 C48 121.2(4) . . ? C53 C48 C49 118.6(3) . . ? C53 C48 C47 118.1(4) . . ? C49 C48 C47 123.2(4) . . ? C50 C49 C48 118.7(4) . . ? C49 C50 C51 119.7(4) . . ? N52 C51 C50 123.1(3) . . ? C51 N52 C53 117.0(3) . . ? C51 N52 Co1 130.6(2) . . ? C53 N52 Co1 112.3(2) . . ? N52 C53 C48 122.8(3) . . ? N52 C53 C54 115.5(3) . . ? C48 C53 C54 121.7(3) . . ? N41 C54 C53 116.3(3) . . ? N41 C54 C45 123.0(3) . . ? C53 C54 C45 120.7(3) . . ? O72 Cl7 O71 109.90(16) . . ? O72 Cl7 O74 109.75(17) . . ? O71 Cl7 O74 110.00(15) . . ? O72 Cl7 O73 109.97(19) . . ? O71 Cl7 O73 108.79(16) . . ? O74 Cl7 O73 108.39(17) . . ? O62 Cl6 O63 115.0(3) . . ? O62 Cl6 O64 107.6(3) . . ? O63 Cl6 O64 105.4(3) . . ? O62 Cl6 O61 112.0(3) . . ? O63 Cl6 O61 108.5(3) . . ? O64 Cl6 O61 107.9(2) . . ? O84 Cl8 O81 109.0(4) . . ? O84 Cl8 O82 106.7(4) . . ? O81 Cl8 O82 112.0(4) . . ? O84 Cl8 O83 112.7(3) . . ? O81 Cl8 O83 109.3(4) . . ? O82 Cl8 O83 107.1(3) . . ? Cl9 Cl9 O93 131(3) 2_577 2_577 ? Cl9 Cl9 O92 125(3) 2_577 . ? O93 Cl9 O92 79.2(15) 2_577 . ? Cl9 Cl9 O93 30.7(18) 2_577 . ? O93 Cl9 O93 161.8(15) 2_577 . ? O92 Cl9 O93 111.5(7) . . ? Cl9 Cl9 O91 119(3) 2_577 . ? O93 Cl9 O91 79(2) 2_577 . ? O92 Cl9 O91 109.7(7) . . ? O93 Cl9 O91 109.0(8) . . ? Cl9 Cl9 O94 79.8(19) 2_577 . ? O93 Cl9 O94 51.3(18) 2_577 . ? O92 Cl9 O94 109.8(8) . . ? O93 Cl9 O94 110.5(7) . . ? O91 Cl9 O94 106.3(7) . . ? Cl9 Cl9 O94 77(2) 2_577 2_577 ? O93 Cl9 O94 152(3) 2_577 2_577 ? O92 Cl9 O94 84.3(10) . 2_577 ? O93 Cl9 O94 45.9(14) . 2_577 ? O91 Cl9 O94 85.5(18) . 2_577 ? O94 Cl9 O94 156.4(12) . 2_577 ? Cl9 Cl9 O91 44(3) 2_577 2_577 ? O93 Cl9 O91 111(2) 2_577 2_577 ? O92 Cl9 O91 85.5(9) . 2_577 ? O93 Cl9 O91 57.1(9) . 2_577 ? O91 Cl9 O91 163.3(7) . 2_577 ? O94 Cl9 O91 73.6(9) . 2_577 ? O94 Cl9 O91 89(2) 2_577 2_577 ? Cl9 Cl9 O92 39(2) 2_577 2_577 ? O93 Cl9 O92 111.0(16) 2_577 2_577 ? O92 Cl9 O92 164.6(13) . 2_577 ? O93 Cl9 O92 55.7(9) . 2_577 ? O91 Cl9 O92 84.0(12) . 2_577 ? O94 Cl9 O92 71.3(7) . 2_577 ? O94 Cl9 O92 90.1(10) 2_577 2_577 ? O91 Cl9 O92 80.1(12) 2_577 2_577 ? Cl9 O91 O93 37.2(13) . 2_577 ? Cl9 O91 Cl9 16.7(7) . 2_577 ? O93 O91 Cl9 49.6(12) 2_577 2_577 ? Cl9 O92 O93 37.5(10) . 2_577 ? Cl9 O92 Cl9 15.4(13) . 2_577 ? O93 O92 Cl9 49.2(6) 2_577 2_577 ? Cl9 O93 O94 86(3) 2_577 2_577 ? Cl9 O93 Cl9 18.2(15) 2_577 . ? O94 O93 Cl9 68.3(15) 2_577 . ? Cl9 O93 O92 63.2(15) 2_577 2_577 ? O94 O93 O92 120(3) 2_577 2_577 ? Cl9 O93 O92 75.1(10) . 2_577 ? Cl9 O93 O91 63.4(15) 2_577 2_577 ? O94 O93 O91 115.5(18) 2_577 2_577 ? Cl9 O93 O91 73.2(15) . 2_577 ? O92 O93 O91 96.0(12) 2_577 2_577 ? O93 O94 Cl9 42.2(13) 2_577 . ? O93 O94 Cl9 65.8(9) 2_577 2_577 ? Cl9 O94 Cl9 23.6(12) . 2_577 ? O62X Cl6X O64X 110.9(10) . . ? O62X Cl6X O61X 110.5(10) . . ? O64X Cl6X O61X 107.3(9) . . ? O62X Cl6X O63X 108.5(10) . . ? O64X Cl6X O63X 112.9(9) . . ? O61X Cl6X O63X 106.6(9) . . ? O82X Cl8X O83X 113.6(8) . . ? O82X Cl8X O84X 108.5(8) . . ? O83X Cl8X O84X 111.5(9) . . ? O82X Cl8X O81X 109.2(10) . . ? O83X Cl8X O81X 107.8(10) . . ? O84X Cl8X O81X 106.0(9) . . ? Cl9X Cl9X O93X 138(10) 2_577 2_577 ? Cl9X Cl9X O92X 98(10) 2_577 . ? O93X Cl9X O92X 67(3) 2_577 . ? Cl9X Cl9X O93X 35(10) 2_577 . ? O93X Cl9X O93X 173(3) 2_577 . ? O92X Cl9X O93X 111.1(10) . . ? Cl9X Cl9X O91X 142(10) 2_577 . ? O93X Cl9X O91X 78(4) 2_577 . ? O92X Cl9X O91X 109.3(10) . . ? O93X Cl9X O91X 108.9(10) . . ? Cl9X Cl9X O94X 87(9) 2_577 . ? O93X Cl9X O94X 65(2) 2_577 . ? O92X Cl9X O94X 110.1(10) . . ? O93X Cl9X O94X 110.3(10) . . ? O91X Cl9X O94X 107.0(10) . . ? Cl9X Cl9X O94X 83(9) 2_577 2_577 ? O93X Cl9X O94X 123(4) 2_577 2_577 ? O92X Cl9X O94X 71.5(18) . 2_577 ? O93X Cl9X O94X 60(2) . 2_577 ? O91X Cl9X O94X 81(3) . 2_577 ? O94X Cl9X O94X 170(3) . 2_577 ? Cl9X Cl9X O92X 72(10) 2_577 2_577 ? O93X Cl9X O92X 120(4) 2_577 2_577 ? O92X Cl9X O92X 170(3) . 2_577 ? O93X Cl9X O92X 61(3) . 2_577 ? O91X Cl9X O92X 80(3) . 2_577 ? O94X Cl9X O92X 70.1(16) . 2_577 ? O94X Cl9X O92X 106(2) 2_577 2_577 ? Cl9X Cl9X O91X 32(10) 2_577 2_577 ? O93X Cl9X O91X 107(4) 2_577 2_577 ? O92X Cl9X O91X 74.5(17) . 2_577 ? O93X Cl9X O91X 65.7(17) . 2_577 ? O91X Cl9X O91X 174.5(16) . 2_577 ? O94X Cl9X O91X 74.7(16) . 2_577 ? O94X Cl9X O91X 96(4) 2_577 2_577 ? O92X Cl9X O91X 96(4) 2_577 2_577 ? Cl9X O91X Cl9X 5.5(16) . 2_577 ? Cl9X O91X O93X 45(3) . 2_577 ? Cl9X O91X O93X 51(2) 2_577 2_577 ? Cl9X O92X O93X 50.2(18) . 2_577 ? Cl9X O92X Cl9X 10(3) . 2_577 ? O93X O92X Cl9X 58(2) 2_577 2_577 ? Cl9X O92X O94X 55.0(16) . 2_577 ? O93X O92X O94X 97(3) 2_577 2_577 ? Cl9X O92X O94X 53.9(14) 2_577 2_577 ? Cl9X O93X Cl9X 7(3) 2_577 . ? Cl9X O93X O94X 64(3) 2_577 2_577 ? Cl9X O93X O94X 60.3(18) . 2_577 ? Cl9X O93X O92X 63(3) 2_577 2_577 ? Cl9X O93X O92X 61(2) . 2_577 ? O94X O93X O92X 107(5) 2_577 2_577 ? Cl9X O93X O91X 56.6(19) 2_577 2_577 ? Cl9X O93X O91X 63(3) . 2_577 ? O94X O93X O91X 95(2) 2_577 2_577 ? O92X O93X O91X 95(2) 2_577 2_577 ? Cl9X O94X Cl9X 10(3) . 2_577 ? Cl9X O94X O93X 50.3(19) . 2_577 ? Cl9X O94X O93X 59.2(18) 2_577 2_577 ? Cl9X O94X O92X 56.0(15) . 2_577 ? Cl9X O94X O92X 53.4(13) 2_577 2_577 ? O93X O94X O92X 97(3) 2_577 2_577 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.431 _refine_diff_density_min -1.366 _refine_diff_density_rms 0.100 # Attachment '6763.cif' data_test _database_code_depnum_ccdc_archive 'CCDC 755466' #TrackingRef '6763.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 Co N8, 3(Cl O4), 3(H2 O)' _chemical_formula_sum 'C26 H28 Cl3 Co N8 O15' _chemical_formula_weight 857.84 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 22.144(2) _cell_length_b 12.6464(8) _cell_length_c 23.798(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6664.4(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.937 _exptl_absorpt_process_details 'SADABS 2006/1, Bruker AXS (2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Kappa-CCD' _diffrn_measurement_method '692 images at 1.0 deg. stepwise rotation in omega and phi, 80 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 111311 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9684 _reflns_number_gt 6834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _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^)+(0.0718P)^2^+15.5873P] 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 9684 _refine_ls_number_parameters 545 _refine_ls_number_restraints 98 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1764 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.003 _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 0.437755(19) 0.76199(3) 0.126763(16) 0.02751(11) Uani 1 1 d . . . N1 N 0.40847(12) 0.9013(2) 0.14668(11) 0.0309(6) Uani 1 1 d . . . C2 C 0.43032(16) 0.9940(3) 0.12802(14) 0.0356(7) Uani 1 1 d . . . H2 H 0.4593 0.9941 0.0986 0.043 Uiso 1 1 calc R . . C3 C 0.41157(19) 1.0895(3) 0.15063(17) 0.0463(9) Uani 1 1 d . . . H3 H 0.4270 1.1542 0.1364 0.056 Uiso 1 1 calc R . . C4 C 0.3703(2) 1.0896(3) 0.19398(19) 0.0526(10) Uani 1 1 d . . . H4 H 0.3571 1.1544 0.2100 0.063 Uiso 1 1 calc R . . C5 C 0.34841(18) 0.9952(3) 0.21363(16) 0.0462(9) Uani 1 1 d . . . H5 H 0.3204 0.9940 0.2438 0.055 Uiso 1 1 calc R . . C6 C 0.36758(15) 0.9010(3) 0.18911(13) 0.0344(7) Uani 1 1 d . . . C7 C 0.34764(14) 0.7961(3) 0.20579(13) 0.0345(7) Uani 1 1 d . . . C8 C 0.30289(16) 0.7763(4) 0.24527(15) 0.0442(9) Uani 1 1 d . . . H8 H 0.2844 0.8332 0.2649 0.053 Uiso 1 1 calc R . . C9 C 0.28554(17) 0.6734(4) 0.25580(17) 0.0505(10) Uani 1 1 d . . . H9 H 0.2551 0.6585 0.2828 0.061 Uiso 1 1 calc R . . C10 C 0.31298(16) 0.5923(4) 0.22650(17) 0.0470(9) Uani 1 1 d . . . H10 H 0.3011 0.5211 0.2326 0.056 Uiso 1 1 calc R . . C11 C 0.35815(15) 0.6160(3) 0.18795(15) 0.0389(8) Uani 1 1 d . . . H11 H 0.3771 0.5601 0.1680 0.047 Uiso 1 1 calc R . . N12 N 0.37554(11) 0.7154(2) 0.17836(11) 0.0316(6) Uani 1 1 d . . . N21 N 0.38624(13) 0.7410(2) 0.06263(11) 0.0326(6) Uani 1 1 d . . . C22 C 0.34936(16) 0.8134(3) 0.03972(14) 0.0376(7) Uani 1 1 d . . . H22 H 0.3440 0.8792 0.0583 0.045 Uiso 1 1 calc R . . C23 C 0.31908(19) 0.7950(3) -0.00983(16) 0.0470(9) Uani 1 1 d . . . H23 H 0.2938 0.8478 -0.0257 0.056 Uiso 1 1 calc R . . C24 C 0.3262(2) 0.6981(4) -0.03618(17) 0.0507(10) Uani 1 1 d . . . H24 H 0.3057 0.6838 -0.0704 0.061 Uiso 1 1 calc R . . C25 C 0.36311(18) 0.6224(3) -0.01245(16) 0.0448(8) Uani 1 1 d . . . H25 H 0.3679 0.5553 -0.0299 0.054 Uiso 1 1 calc R . . C26 C 0.39310(15) 0.6456(3) 0.03721(14) 0.0330(7) Uani 1 1 d . . . C27 C 0.43550(14) 0.5751(3) 0.06549(14) 0.0325(6) Uani 1 1 d . . . C28 C 0.44685(17) 0.4705(3) 0.05003(15) 0.0388(8) Uani 1 1 d . . . H28 H 0.4264 0.4392 0.0191 0.047 Uiso 1 1 calc R . . C29 C 0.48894(17) 0.4132(3) 0.08104(17) 0.0432(9) Uani 1 1 d . . . H29 H 0.4976 0.3420 0.0713 0.052 Uiso 1 1 calc R . . C30 C 0.51791(16) 0.4596(3) 0.12570(16) 0.0422(8) Uani 1 1 d . . . H30 H 0.5470 0.4212 0.1467 0.051 Uiso 1 1 calc R . . C31 C 0.50403(15) 0.5631(3) 0.13963(16) 0.0374(7) Uani 1 1 d . . . H31 H 0.5238 0.5950 0.1708 0.045 Uiso 1 1 calc R . . N32 N 0.46360(12) 0.6195(2) 0.11050(11) 0.0314(6) Uani 1 1 d . . . N41 N 0.49740(12) 0.7845(2) 0.18449(11) 0.0318(6) Uani 1 1 d . . . C42 C 0.50088(16) 0.7811(3) 0.24218(14) 0.0379(7) Uani 1 1 d . . . H42 H 0.4704 0.7565 0.2670 0.045 Uiso 1 1 calc R . . C43 C 0.55677(17) 0.8200(3) 0.25735(16) 0.0433(8) Uani 1 1 d . . . H43 H 0.5719 0.8272 0.2945 0.052 Uiso 1 1 calc R . . N44 N 0.58638(13) 0.8465(2) 0.20845(13) 0.0386(6) Uani 1 1 d . . . H44 H 0.6231 0.8727 0.2059 0.046 Uiso 1 1 calc R . . C45 C 0.54963(14) 0.8253(3) 0.16590(14) 0.0325(7) Uani 1 1 d . . . C46 C 0.55272(15) 0.8391(3) 0.10614(14) 0.0333(7) Uani 1 1 d . . . N47 N 0.59431(14) 0.8722(3) 0.06936(14) 0.0441(7) Uani 1 1 d . . . H47 H 0.6313 0.8928 0.0774 0.053 Uiso 1 1 calc R . . C48 C 0.56908(19) 0.8681(3) 0.01696(17) 0.0511(10) Uani 1 1 d . . . H48 H 0.5883 0.8870 -0.0173 0.061 Uiso 1 1 calc R . . C49 C 0.51138(18) 0.8323(3) 0.02270(14) 0.0412(8) Uani 1 1 d . . . H49 H 0.4831 0.8217 -0.0067 0.049 Uiso 1 1 calc R . . N50 N 0.50166(12) 0.8142(2) 0.07931(11) 0.0312(6) Uani 1 1 d . . . Cl70 Cl 0.58658(4) 0.13798(7) 0.13876(3) 0.03567(18) Uani 1 1 d . A 1 O71 O 0.59417(14) 0.2466(2) 0.15389(13) 0.0514(7) Uani 1 1 d . A 1 O72 O 0.54871(16) 0.1280(3) 0.09140(13) 0.0742(11) Uani 1 1 d . A 1 O73 O 0.64559(15) 0.0944(3) 0.12828(13) 0.0626(9) Uani 1 1 d . A 1 O74 O 0.56034(15) 0.0815(2) 0.18599(12) 0.0543(7) Uani 1 1 d . A 1 Cl60 Cl 0.6664(2) 0.6193(5) 0.1191(2) 0.0329(5) Uani 0.712(10) 1 d PD B 1 O61 O 0.6937(4) 0.5181(5) 0.1206(3) 0.084(2) Uani 0.712(10) 1 d PDU B 1 O62 O 0.7110(5) 0.7012(6) 0.1072(4) 0.0659(18) Uani 0.712(10) 1 d PDU B 1 O63 O 0.6413(2) 0.6439(5) 0.17266(17) 0.0431(11) Uani 0.712(10) 1 d PDU B 1 O64 O 0.6204(5) 0.6212(12) 0.0765(4) 0.0410(10) Uani 0.712(10) 1 d PDU B 1 Cl65 Cl 0.6739(6) 0.6152(12) 0.1152(5) 0.0329(5) Uani 0.288(10) 1 d PD B 2 O66 O 0.7131(9) 0.5330(16) 0.0997(8) 0.084(2) Uani 0.288(10) 1 d PDU B 2 O67 O 0.7051(14) 0.7164(16) 0.1174(12) 0.0659(18) Uani 0.288(10) 1 d PDU B 2 O68 O 0.6491(5) 0.5968(12) 0.1696(5) 0.0431(11) Uani 0.288(10) 1 d PDU B 2 O69 O 0.6262(12) 0.623(3) 0.0741(9) 0.0410(10) Uani 0.288(10) 1 d PDU B 2 Cl80 Cl 0.18681(18) 0.8469(4) 0.12495(17) 0.0422(6) Uani 0.490(3) 1 d PD C 1 O81 O 0.2392(4) 0.7824(12) 0.1137(6) 0.068(2) Uani 0.490(3) 1 d PD C 1 O82 O 0.1341(3) 0.7943(5) 0.1056(3) 0.0588(15) Uani 0.490(3) 1 d PD C 1 O83 O 0.1829(3) 0.8626(5) 0.1849(3) 0.0544(16) Uani 0.490(3) 1 d PD C 1 O84 O 0.1917(6) 0.9487(6) 0.0971(4) 0.062(2) Uani 0.490(3) 1 d PD C 1 Cl85 Cl 0.1901(3) 0.8390(6) 0.1076(3) 0.0422(6) Uani 0.334(4) 1 d PD D 2 O86 O 0.2477(6) 0.7908(18) 0.1189(9) 0.068(2) Uani 0.334(4) 1 d PD D 2 O87 O 0.1558(4) 0.7720(7) 0.0717(4) 0.0588(15) Uani 0.334(4) 1 d PD D 2 O88 O 0.1575(5) 0.8550(8) 0.1592(4) 0.0544(16) Uani 0.334(4) 1 d PD D 2 O89 O 0.1980(9) 0.9392(9) 0.0785(6) 0.062(2) Uani 0.334(4) 1 d PD D 2 Cl90 Cl 0.2027(4) 0.8451(8) 0.1091(4) 0.0422(6) Uani 0.176(4) 1 d PD E 3 O91 O 0.2288(9) 0.7433(12) 0.1198(11) 0.068(2) Uani 0.176(4) 1 d PD E 3 O94 O 0.2443(7) 0.9227(12) 0.1295(6) 0.062(2) Uani 0.176(4) 1 d PD E 3 O92 O 0.1924(7) 0.8675(13) 0.0507(5) 0.0588(15) Uani 0.176(4) 1 d PD E 3 O93 O 0.1459(6) 0.8539(16) 0.1401(7) 0.0544(16) Uani 0.176(4) 1 d PD E 3 O100 O 0.70103(15) 0.9005(3) 0.17439(14) 0.0598(8) Uani 1 1 d D . . H101 H 0.707(3) 0.873(4) 0.1431(14) 0.090 Uiso 1 1 d D . . H102 H 0.696(3) 0.9665(16) 0.169(2) 0.090 Uiso 1 1 d D . . O200 O 0.20526(19) 0.5656(3) 0.05964(19) 0.0794(11) Uani 1 1 d D . . H201 H 0.208(3) 0.567(5) 0.0236(8) 0.119 Uiso 1 1 d D . . H202 H 0.222(3) 0.622(4) 0.072(2) 0.119 Uiso 1 1 d D . . O300 O 0.7065(2) 0.9411(4) 0.0509(2) 0.0945(14) Uani 1 1 d D . . H301 H 0.710(3) 0.873(2) 0.062(3) 0.142 Uiso 1 1 d D . . H302 H 0.739(2) 0.972(5) 0.063(3) 0.142 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0261(2) 0.0339(2) 0.02258(19) 0.00226(16) 0.00048(15) 0.00613(16) N1 0.0308(13) 0.0377(14) 0.0242(12) -0.0041(10) -0.0024(10) 0.0046(11) C2 0.0372(17) 0.0373(17) 0.0323(16) -0.0048(13) 0.0008(13) 0.0035(14) C3 0.049(2) 0.0401(19) 0.050(2) -0.0127(17) 0.0021(17) -0.0003(16) C4 0.056(2) 0.046(2) 0.056(2) -0.0208(19) 0.0067(19) 0.0037(19) C5 0.0408(19) 0.055(2) 0.043(2) -0.0166(17) 0.0060(16) 0.0053(17) C6 0.0279(15) 0.0474(19) 0.0279(15) -0.0059(13) -0.0013(12) 0.0060(14) C7 0.0252(14) 0.052(2) 0.0264(15) -0.0016(13) -0.0013(11) 0.0058(14) C8 0.0295(16) 0.067(2) 0.0361(18) -0.0031(17) 0.0030(14) 0.0054(17) C9 0.0301(18) 0.081(3) 0.041(2) 0.013(2) 0.0084(15) 0.0016(19) C10 0.0291(17) 0.063(2) 0.049(2) 0.0185(19) 0.0032(15) -0.0019(16) C11 0.0277(16) 0.049(2) 0.0406(18) 0.0115(15) 0.0023(13) 0.0027(14) N12 0.0230(12) 0.0442(15) 0.0276(12) 0.0046(11) -0.0009(10) 0.0053(11) N21 0.0334(14) 0.0343(14) 0.0300(13) -0.0024(11) -0.0021(11) 0.0075(11) C22 0.0399(18) 0.0388(18) 0.0340(17) -0.0032(14) -0.0089(14) 0.0113(15) C23 0.050(2) 0.051(2) 0.0402(19) -0.0036(16) -0.0139(17) 0.0107(18) C24 0.056(2) 0.055(2) 0.041(2) -0.0054(17) -0.0149(18) 0.0056(19) C25 0.051(2) 0.0424(19) 0.0410(19) -0.0091(16) -0.0054(16) 0.0040(17) C26 0.0345(16) 0.0335(16) 0.0309(15) -0.0029(12) 0.0014(12) 0.0045(13) C27 0.0290(15) 0.0352(16) 0.0332(16) 0.0022(12) 0.0085(12) 0.0028(13) C28 0.0418(18) 0.0331(16) 0.0416(18) 0.0022(14) 0.0151(14) 0.0037(14) C29 0.0412(19) 0.0327(17) 0.056(2) 0.0089(16) 0.0209(17) 0.0078(14) C30 0.0301(16) 0.0423(19) 0.054(2) 0.0169(17) 0.0121(15) 0.0101(14) C31 0.0299(16) 0.0384(18) 0.0440(18) 0.0123(14) 0.0029(13) 0.0065(13) N32 0.0284(13) 0.0339(14) 0.0319(13) 0.0075(11) 0.0033(10) 0.0055(11) N41 0.0271(12) 0.0446(15) 0.0237(12) 0.0043(11) 0.0011(10) 0.0046(11) C42 0.0337(16) 0.052(2) 0.0276(15) 0.0068(14) 0.0003(12) 0.0077(15) C43 0.0408(19) 0.053(2) 0.0360(18) 0.0034(16) -0.0083(15) 0.0061(17) N44 0.0311(14) 0.0433(16) 0.0414(16) 0.0019(13) -0.0028(12) 0.0024(12) C45 0.0277(14) 0.0365(16) 0.0334(16) 0.0050(13) 0.0013(12) 0.0038(12) C46 0.0314(16) 0.0339(16) 0.0348(16) 0.0069(13) 0.0070(12) 0.0048(13) N47 0.0380(16) 0.0473(17) 0.0470(18) 0.0134(14) 0.0164(13) 0.0041(13) C48 0.055(2) 0.056(2) 0.043(2) 0.0189(18) 0.0213(18) 0.0162(19) C49 0.057(2) 0.0422(18) 0.0243(15) 0.0058(13) 0.0071(14) 0.0183(16) N50 0.0355(14) 0.0322(13) 0.0258(12) 0.0038(10) 0.0069(10) 0.0073(11) Cl70 0.0343(4) 0.0371(4) 0.0356(4) -0.0048(3) -0.0008(3) 0.0044(3) O71 0.069(2) 0.0290(12) 0.0564(17) 0.0000(11) 0.0113(15) 0.0078(12) O72 0.069(2) 0.106(3) 0.0474(18) 0.0211(18) -0.0238(16) -0.029(2) O73 0.0598(19) 0.074(2) 0.0541(18) -0.0052(15) 0.0005(14) 0.0351(17) O74 0.077(2) 0.0447(15) 0.0410(15) 0.0104(12) -0.0016(14) -0.0061(14) Cl60 0.0257(14) 0.0392(6) 0.0340(8) -0.0074(5) 0.0035(7) 0.0039(8) O61 0.087(5) 0.064(3) 0.101(5) -0.040(3) -0.044(3) 0.044(3) O62 0.065(3) 0.078(3) 0.055(4) -0.011(3) 0.008(2) -0.034(3) O63 0.0425(18) 0.057(3) 0.0302(14) -0.006(2) 0.0045(13) 0.012(2) O64 0.045(2) 0.0443(14) 0.0337(14) -0.0026(12) -0.0066(15) 0.0001(19) Cl65 0.0257(14) 0.0392(6) 0.0340(8) -0.0074(5) 0.0035(7) 0.0039(8) O66 0.087(5) 0.064(3) 0.101(5) -0.040(3) -0.044(3) 0.044(3) O67 0.065(3) 0.078(3) 0.055(4) -0.011(3) 0.008(2) -0.034(3) O68 0.0425(18) 0.057(3) 0.0302(14) -0.006(2) 0.0045(13) 0.012(2) O69 0.045(2) 0.0443(14) 0.0337(14) -0.0026(12) -0.0066(15) 0.0001(19) Cl80 0.0299(10) 0.0416(8) 0.055(2) 0.0006(14) 0.0151(13) 0.0017(8) O81 0.033(3) 0.106(5) 0.066(3) -0.003(3) -0.002(3) 0.018(4) O82 0.050(3) 0.057(3) 0.069(4) 0.016(3) -0.020(3) -0.012(3) O83 0.050(4) 0.052(2) 0.060(4) 0.000(3) 0.016(3) 0.000(3) O84 0.055(4) 0.060(3) 0.070(6) 0.018(3) 0.014(4) -0.016(2) Cl85 0.0299(10) 0.0416(8) 0.055(2) 0.0006(14) 0.0151(13) 0.0017(8) O86 0.033(3) 0.106(5) 0.066(3) -0.003(3) -0.002(3) 0.018(4) O87 0.050(3) 0.057(3) 0.069(4) 0.016(3) -0.020(3) -0.012(3) O88 0.050(4) 0.052(2) 0.060(4) 0.000(3) 0.016(3) 0.000(3) O89 0.055(4) 0.060(3) 0.070(6) 0.018(3) 0.014(4) -0.016(2) Cl90 0.0299(10) 0.0416(8) 0.055(2) 0.0006(14) 0.0151(13) 0.0017(8) O91 0.033(3) 0.106(5) 0.066(3) -0.003(3) -0.002(3) 0.018(4) O94 0.055(4) 0.060(3) 0.070(6) 0.018(3) 0.014(4) -0.016(2) O92 0.050(3) 0.057(3) 0.069(4) 0.016(3) -0.020(3) -0.012(3) O93 0.050(4) 0.052(2) 0.060(4) 0.000(3) 0.016(3) 0.000(3) O100 0.0440(16) 0.073(2) 0.0625(19) 0.0172(16) -0.0052(15) -0.0110(16) O200 0.063(2) 0.069(2) 0.106(3) -0.001(2) -0.003(2) 0.0098(19) O300 0.079(3) 0.093(3) 0.112(4) 0.015(3) -0.007(2) -0.027(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N21 1.924(3) . ? Co1 N41 1.927(3) . ? Co1 N50 1.927(3) . ? Co1 N32 1.929(3) . ? Co1 N1 1.936(3) . ? Co1 N12 1.937(3) . ? N1 C2 1.344(5) . ? N1 C6 1.356(4) . ? C2 C3 1.386(5) . ? C3 C4 1.379(6) . ? C4 C5 1.371(6) . ? C5 C6 1.392(5) . ? C6 C7 1.453(5) . ? C7 N12 1.360(4) . ? C7 C8 1.388(5) . ? C8 C9 1.381(6) . ? C9 C10 1.380(6) . ? C10 C11 1.390(5) . ? C11 N12 1.334(5) . ? N21 C22 1.342(4) . ? N21 C26 1.359(4) . ? C22 C23 1.376(5) . ? C23 C24 1.386(6) . ? C24 C25 1.381(6) . ? C25 C26 1.387(5) . ? C26 C27 1.459(5) . ? C27 N32 1.360(4) . ? C27 C28 1.396(5) . ? C28 C29 1.392(5) . ? C29 C30 1.373(6) . ? C30 C31 1.385(5) . ? C31 N32 1.339(4) . ? N41 C45 1.341(4) . ? N41 C42 1.376(4) . ? C42 C43 1.380(5) . ? C43 N44 1.377(5) . ? N44 C45 1.326(4) . ? C45 C46 1.434(5) . ? C46 N50 1.336(4) . ? C46 N47 1.338(4) . ? N47 C48 1.367(5) . ? C48 C49 1.363(6) . ? C49 N50 1.383(4) . ? Cl70 O72 1.410(3) . ? Cl70 O71 1.430(3) . ? Cl70 O73 1.440(3) . ? Cl70 O74 1.453(3) . ? Cl60 O61 1.415(5) . ? Cl60 O63 1.425(4) . ? Cl60 O64 1.436(4) . ? Cl60 O62 1.458(5) . ? Cl65 O66 1.404(8) . ? Cl65 O68 1.425(8) . ? Cl65 O69 1.441(7) . ? Cl65 O67 1.456(8) . ? Cl80 O82 1.420(6) . ? Cl80 O83 1.442(7) . ? Cl80 O81 1.443(6) . ? Cl80 O84 1.452(6) . ? Cl85 O87 1.423(8) . ? Cl85 O86 1.438(8) . ? Cl85 O88 1.441(8) . ? Cl85 O89 1.455(7) . ? Cl90 O94 1.430(9) . ? Cl90 O91 1.434(9) . ? Cl90 O92 1.436(10) . ? Cl90 O93 1.462(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 N21 Co1 N41 172.94(11) . . ? N21 Co1 N50 91.01(12) . . ? N41 Co1 N50 82.17(12) . . ? N21 Co1 N32 83.57(12) . . ? N41 Co1 N32 94.47(12) . . ? N50 Co1 N32 89.10(11) . . ? N21 Co1 N1 96.95(11) . . ? N41 Co1 N1 85.43(11) . . ? N50 Co1 N1 94.46(12) . . ? N32 Co1 N1 176.38(11) . . ? N21 Co1 N12 92.25(12) . . ? N41 Co1 N12 94.63(11) . . ? N50 Co1 N12 176.25(12) . . ? N32 Co1 N12 93.10(12) . . ? N1 Co1 N12 83.31(12) . . ? C2 N1 C6 119.2(3) . . ? C2 N1 Co1 126.3(2) . . ? C6 N1 Co1 113.8(2) . . ? N1 C2 C3 121.6(3) . . ? C4 C3 C2 119.4(4) . . ? C5 C4 C3 119.2(4) . . ? C4 C5 C6 119.6(3) . . ? N1 C6 C5 120.9(3) . . ? N1 C6 C7 114.1(3) . . ? C5 C6 C7 125.0(3) . . ? N12 C7 C8 120.9(4) . . ? N12 C7 C6 114.6(3) . . ? C8 C7 C6 124.5(3) . . ? C9 C8 C7 119.4(4) . . ? C10 C9 C8 119.1(3) . . ? C9 C10 C11 119.4(4) . . ? N12 C11 C10 121.5(4) . . ? C11 N12 C7 119.6(3) . . ? C11 N12 Co1 126.9(2) . . ? C7 N12 Co1 113.5(2) . . ? C22 N21 C26 119.5(3) . . ? C22 N21 Co1 126.1(2) . . ? C26 N21 Co1 114.2(2) . . ? N21 C22 C23 122.0(3) . . ? C22 C23 C24 118.8(4) . . ? C25 C24 C23 119.7(4) . . ? C24 C25 C26 119.0(3) . . ? N21 C26 C25 120.9(3) . . ? N21 C26 C27 114.2(3) . . ? C25 C26 C27 124.9(3) . . ? N32 C27 C28 121.1(3) . . ? N32 C27 C26 113.9(3) . . ? C28 C27 C26 125.0(3) . . ? C29 C28 C27 118.3(4) . . ? C30 C29 C28 120.1(3) . . ? C29 C30 C31 119.0(3) . . ? N32 C31 C30 121.9(4) . . ? C31 N32 C27 119.6(3) . . ? C31 N32 Co1 126.3(3) . . ? C27 N32 Co1 114.1(2) . . ? C45 N41 C42 107.0(3) . . ? C45 N41 Co1 114.4(2) . . ? C42 N41 Co1 138.2(2) . . ? N41 C42 C43 107.5(3) . . ? N44 C43 C42 107.0(3) . . ? C45 N44 C43 107.7(3) . . ? N44 C45 N41 110.8(3) . . ? N44 C45 C46 134.7(3) . . ? N41 C45 C46 114.5(3) . . ? N50 C46 N47 110.1(3) . . ? N50 C46 C45 113.9(3) . . ? N47 C46 C45 136.0(3) . . ? C46 N47 C48 107.7(3) . . ? C49 C48 N47 107.7(3) . . ? C48 C49 N50 107.4(3) . . ? C46 N50 C49 107.1(3) . . ? C46 N50 Co1 115.0(2) . . ? C49 N50 Co1 137.9(3) . . ? O72 Cl70 O71 110.9(2) . . ? O72 Cl70 O73 111.5(2) . . ? O71 Cl70 O73 107.7(2) . . ? O72 Cl70 O74 109.65(19) . . ? O71 Cl70 O74 108.92(18) . . ? O73 Cl70 O74 108.0(2) . . ? O61 Cl60 O63 109.9(4) . . ? O61 Cl60 O64 109.6(5) . . ? O63 Cl60 O64 110.6(4) . . ? O61 Cl60 O62 111.0(5) . . ? O63 Cl60 O62 106.4(4) . . ? O64 Cl60 O62 109.3(4) . . ? O66 Cl65 O68 110.8(10) . . ? O66 Cl65 O69 109.0(10) . . ? O68 Cl65 O69 110.2(11) . . ? O66 Cl65 O67 111.5(11) . . ? O68 Cl65 O67 107.1(10) . . ? O69 Cl65 O67 108.2(10) . . ? O82 Cl80 O83 109.6(5) . . ? O82 Cl80 O81 109.6(6) . . ? O83 Cl80 O81 108.1(6) . . ? O82 Cl80 O84 109.1(6) . . ? O83 Cl80 O84 109.5(5) . . ? O81 Cl80 O84 110.9(6) . . ? O87 Cl85 O86 109.5(9) . . ? O87 Cl85 O88 109.2(7) . . ? O86 Cl85 O88 110.2(9) . . ? O87 Cl85 O89 107.3(8) . . ? O86 Cl85 O89 110.6(9) . . ? O88 Cl85 O89 110.1(7) . . ? O94 Cl90 O91 107.2(11) . . ? O94 Cl90 O92 107.2(9) . . ? O91 Cl90 O92 114.4(12) . . ? O94 Cl90 O93 109.3(10) . . ? O91 Cl90 O93 109.0(10) . . ? O92 Cl90 O93 109.6(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N44 H44 O100 0.88 1.91 2.751(4) 158.3 . N47 H47 O300 0.88 1.88 2.669(5) 147.7 . O100 H101 O300 0.836(19) 2.36(4) 2.987(6) 132(4) . O100 H101 O62 0.836(19) 2.33(4) 2.993(9) 136(5) . O100 H102 O73 0.850(19) 2.20(4) 2.954(5) 148(5) 1_565 O200 H201 O300 0.86(2) 1.78(2) 2.631(7) 174(7) 4_465 O300 H302 O61 0.87(2) 2.11(4) 2.932(9) 158(7) 8_765 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.364 _refine_diff_density_min -0.974 _refine_diff_density_rms 0.094