# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1948 data_cobs10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H47 Cl8 Co N6 O8 P' _chemical_formula_weight 981.23 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' 'P' 'P' 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M ? 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 15.3832(11) _cell_length_b 16.8991(12) _cell_length_c 17.8228(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.1540(10) _cell_angle_gamma 90.00 _cell_volume 4560.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 238(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2020 _exptl_absorpt_coefficient_mu 0.928 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7681 _exptl_absorpt_correction_T_max 0.9129 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 238(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31912 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10147 _reflns_number_gt 6201 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+1.5503P] 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 10147 _refine_ls_number_parameters 490 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1049 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.2086 _refine_ls_wR_factor_gt 0.1819 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.12016(3) 0.16088(3) 0.15856(3) 0.04290(17) Uani 1 1 d . . . N11 N 0.3878(2) 0.1811(2) 0.1806(2) 0.0599(9) Uani 1 1 d . . . N12 N 0.2447(2) 0.20362(19) 0.17058(16) 0.0478(7) Uani 1 1 d . . . N21 N 0.1979(2) 0.02183(19) -0.00577(15) 0.0475(7) Uani 1 1 d . . . N22 N 0.12734(19) 0.10369(17) 0.05948(15) 0.0417(7) Uani 1 1 d . . . N31 N 0.2374(2) -0.03284(19) 0.26982(17) 0.0495(8) Uani 1 1 d . . . N32 N 0.1486(2) 0.06651(17) 0.22838(15) 0.0425(7) Uani 1 1 d . . . C11 C 0.3060(3) 0.1483(2) 0.1654(2) 0.0494(9) Uani 1 1 d . . . C12 C 0.3765(3) 0.2597(3) 0.1947(3) 0.0669(12) Uani 1 1 d . . . H12A H 0.4219 0.2973 0.2066 0.080 Uiso 1 1 calc R . . C13 C 0.2886(3) 0.2741(2) 0.1888(2) 0.0552(10) Uani 1 1 d . . . C14 C 0.4730(3) 0.1387(4) 0.1804(4) 0.0916(17) Uani 1 1 d . . . H14A H 0.4538 0.0876 0.1558 0.110 Uiso 1 1 calc R . . C15 C 0.5146(6) 0.1158(7) 0.2548(5) 0.188(5) Uani 1 1 d . . . H15A H 0.4719 0.0897 0.2805 0.282 Uiso 1 1 calc R . . H15B H 0.5375 0.1623 0.2835 0.282 Uiso 1 1 calc R . . H15C H 0.5627 0.0797 0.2512 0.282 Uiso 1 1 calc R . . C16 C 0.5220(6) 0.1755(6) 0.1264(7) 0.181(5) Uani 1 1 d . . . H16A H 0.4893 0.1692 0.0750 0.272 Uiso 1 1 calc R . . H16B H 0.5793 0.1502 0.1303 0.272 Uiso 1 1 calc R . . H16C H 0.5301 0.2313 0.1380 0.272 Uiso 1 1 calc R . . C17 C 0.2409(3) 0.3500(3) 0.1969(3) 0.0665(12) Uani 1 1 d . . . H17A H 0.2040 0.3432 0.2366 0.080 Uiso 1 1 calc R . . C18 C 0.1812(4) 0.3724(3) 0.1220(4) 0.0917(17) Uani 1 1 d . . . H18A H 0.1366 0.3318 0.1084 0.138 Uiso 1 1 calc R . . H18B H 0.2164 0.3769 0.0821 0.138 Uiso 1 1 calc R . . H18C H 0.1528 0.4227 0.1280 0.138 Uiso 1 1 calc R . . C19 C 0.3074(4) 0.4176(3) 0.2212(4) 0.1001(19) Uani 1 1 d . . . H19A H 0.3450 0.4039 0.2690 0.150 Uiso 1 1 calc R . . H19B H 0.2756 0.4660 0.2277 0.150 Uiso 1 1 calc R . . H19C H 0.3434 0.4254 0.1823 0.150 Uiso 1 1 calc R . . C21 C 0.1984(2) 0.0562(2) 0.06216(18) 0.0445(8) Uani 1 1 d . . . C22 C 0.1228(3) 0.0482(2) -0.0544(2) 0.0537(10) Uani 1 1 d . . . H22A H 0.1050 0.0343 -0.1058 0.064 Uiso 1 1 calc R . . C23 C 0.0799(2) 0.0983(2) -0.01330(19) 0.0457(8) Uani 1 1 d . . . C24 C 0.2666(3) -0.0307(3) -0.0272(2) 0.0585(10) Uani 1 1 d . . . H24A H 0.2999 -0.0525 0.0210 0.070 Uiso 1 1 calc R . . C25 C 0.3315(5) 0.0162(4) -0.0627(5) 0.132(3) Uani 1 1 d . . . H25A H 0.3825 -0.0164 -0.0663 0.197 Uiso 1 1 calc R . . H25B H 0.3501 0.0623 -0.0315 0.197 Uiso 1 1 calc R . . H25C H 0.3038 0.0331 -0.1133 0.197 Uiso 1 1 calc R . . C26 C 0.2262(4) -0.0995(4) -0.0726(5) 0.121(3) Uani 1 1 d . . . H26A H 0.2724 -0.1348 -0.0830 0.181 Uiso 1 1 calc R . . H26B H 0.1921 -0.0809 -0.1203 0.181 Uiso 1 1 calc R . . H26C H 0.1877 -0.1277 -0.0441 0.181 Uiso 1 1 calc R . . C27 C -0.0018(3) 0.1472(2) -0.0395(2) 0.0526(10) Uani 1 1 d . . . H27A H -0.0367 0.1475 0.0022 0.063 Uiso 1 1 calc R . . C28 C -0.0593(3) 0.1117(3) -0.1097(3) 0.0762(14) Uani 1 1 d . . . H28A H -0.1124 0.1433 -0.1235 0.114 Uiso 1 1 calc R . . H28B H -0.0753 0.0580 -0.0988 0.114 Uiso 1 1 calc R . . H28C H -0.0268 0.1114 -0.1517 0.114 Uiso 1 1 calc R . . C29 C 0.0232(3) 0.2321(3) -0.0534(3) 0.0730(13) Uani 1 1 d . . . H29A H 0.0541 0.2549 -0.0062 0.110 Uiso 1 1 calc R . . H29B H -0.0299 0.2625 -0.0715 0.110 Uiso 1 1 calc R . . H29C H 0.0612 0.2332 -0.0914 0.110 Uiso 1 1 calc R . . C31 C 0.2188(2) 0.0243(2) 0.21686(18) 0.0426(8) Uani 1 1 d . . . C32 C 0.1760(3) -0.0271(2) 0.3169(2) 0.0538(10) Uani 1 1 d . . . H32A H 0.1728 -0.0596 0.3592 0.065 Uiso 1 1 calc R . . C33 C 0.1206(3) 0.0340(2) 0.29173(19) 0.0463(8) Uani 1 1 d . . . C34 C 0.3107(3) -0.0906(3) 0.2784(2) 0.0587(10) Uani 1 1 d . . . H34A H 0.3382 -0.0869 0.2323 0.070 Uiso 1 1 calc R . . C35 C 0.3802(4) -0.0693(4) 0.3459(4) 0.104(2) Uani 1 1 d . . . H35A H 0.3991 -0.0151 0.3408 0.155 Uiso 1 1 calc R . . H35B H 0.4304 -0.1045 0.3481 0.155 Uiso 1 1 calc R . . H35C H 0.3559 -0.0746 0.3923 0.155 Uiso 1 1 calc R . . C36 C 0.2763(4) -0.1731(3) 0.2820(4) 0.0938(18) Uani 1 1 d . . . H36A H 0.2278 -0.1816 0.2399 0.141 Uiso 1 1 calc R . . H36B H 0.2555 -0.1806 0.3299 0.141 Uiso 1 1 calc R . . H36C H 0.3231 -0.2107 0.2786 0.141 Uiso 1 1 calc R . . C37 C 0.0412(3) 0.0636(3) 0.3208(2) 0.0553(10) Uani 1 1 d . . . H37A H 0.0421 0.1222 0.3200 0.066 Uiso 1 1 calc R . . C38 C -0.0432(3) 0.0352(3) 0.2682(3) 0.0765(14) Uani 1 1 d . . . H38A H -0.0434 0.0542 0.2168 0.115 Uiso 1 1 calc R . . H38B H -0.0945 0.0556 0.2866 0.115 Uiso 1 1 calc R . . H38C H -0.0449 -0.0222 0.2681 0.115 Uiso 1 1 calc R . . C39 C 0.0416(4) 0.0365(3) 0.4029(3) 0.0826(15) Uani 1 1 d . . . H39A H 0.0932 0.0578 0.4359 0.124 Uiso 1 1 calc R . . H39B H 0.0433 -0.0208 0.4051 0.124 Uiso 1 1 calc R . . H39C H -0.0113 0.0553 0.4197 0.124 Uiso 1 1 calc R . . P P 0.28644(6) 0.04368(6) 0.14425(5) 0.0448(2) Uani 1 1 d . . . Cl1 Cl -0.01533(9) 0.25644(7) 0.19881(7) 0.0710(3) Uani 1 1 d . . . O11 O -0.0015(2) 0.2066(2) 0.13621(19) 0.0829(10) Uani 1 1 d . . . O12 O -0.0354(3) 0.3337(2) 0.1712(3) 0.1200(16) Uani 1 1 d . . . O13 O -0.0835(3) 0.2256(2) 0.2350(2) 0.0975(12) Uani 1 1 d . . . O14 O 0.0681(3) 0.2539(2) 0.2505(2) 0.0930(11) Uani 1 1 d . . . Cl2 Cl 0.44686(11) -0.15782(11) 0.11572(10) 0.0987(5) Uani 1 1 d . . . O21 O 0.4822(8) -0.2276(8) 0.1135(8) 0.346(8) Uani 1 1 d . . . O22 O 0.4666(5) -0.1032(7) 0.0672(6) 0.277(6) Uani 1 1 d . . . O23 O 0.4713(4) -0.1329(6) 0.1924(4) 0.206(4) Uani 1 1 d . . . O24 O 0.3530(3) -0.1627(3) 0.1048(3) 0.1168(15) Uani 1 1 d . . . C1 C -0.2722(5) 0.1609(4) 0.4326(3) 0.0953(18) Uani 1 1 d . . . H1A H -0.3173 0.2033 0.4260 0.114 Uiso 1 1 calc R . . Cl11 Cl -0.3226(2) 0.07141(16) 0.44759(14) 0.1733(11) Uani 1 1 d . . . Cl12 Cl -0.19039(17) 0.18397(14) 0.51065(11) 0.1377(8) Uani 1 1 d . . . Cl13 Cl -0.22644(15) 0.15441(12) 0.34983(10) 0.1244(7) Uani 1 1 d . . . C2 C 0.6457(4) -0.2025(3) 0.5593(3) 0.0814(15) Uani 1 1 d . . . H2A H 0.5996 -0.2347 0.5771 0.098 Uiso 1 1 calc R . . Cl21 Cl 0.59457(18) -0.13128(14) 0.49680(13) 0.1472(8) Uani 1 1 d . . . Cl22 Cl 0.70986(19) -0.15951(15) 0.63700(13) 0.1649(10) Uani 1 1 d . . . Cl23 Cl 0.70977(14) -0.26551(11) 0.51132(10) 0.1165(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0435(3) 0.0465(3) 0.0388(3) -0.0006(2) 0.0076(2) 0.0053(2) N11 0.043(2) 0.067(2) 0.069(2) -0.0059(18) 0.0077(16) -0.0039(16) N12 0.0469(18) 0.0505(19) 0.0457(16) -0.0031(14) 0.0075(14) 0.0008(15) N21 0.0532(19) 0.0520(19) 0.0384(14) -0.0020(13) 0.0111(13) 0.0073(15) N22 0.0439(17) 0.0452(17) 0.0359(13) 0.0015(12) 0.0069(12) 0.0031(13) N31 0.0519(19) 0.0512(19) 0.0454(16) 0.0029(14) 0.0083(14) 0.0087(15) N32 0.0485(18) 0.0434(16) 0.0362(13) -0.0016(12) 0.0087(12) 0.0037(13) C11 0.047(2) 0.056(2) 0.0440(18) 0.0001(17) 0.0059(16) -0.0005(18) C12 0.055(3) 0.075(3) 0.069(3) -0.010(2) 0.006(2) -0.016(2) C13 0.063(3) 0.048(2) 0.053(2) -0.0060(18) 0.0068(19) -0.0053(19) C14 0.043(3) 0.103(4) 0.129(5) 0.002(4) 0.016(3) 0.003(3) C15 0.133(7) 0.273(13) 0.145(8) 0.023(8) -0.010(6) 0.122(8) C16 0.113(6) 0.181(9) 0.275(13) 0.044(9) 0.105(8) 0.058(6) C17 0.077(3) 0.055(3) 0.070(3) -0.009(2) 0.019(2) -0.008(2) C18 0.099(4) 0.065(3) 0.106(4) -0.009(3) 0.004(3) 0.009(3) C19 0.117(5) 0.068(4) 0.110(4) -0.023(3) 0.009(4) -0.012(3) C21 0.048(2) 0.048(2) 0.0366(16) 0.0002(15) 0.0067(15) -0.0011(17) C22 0.060(3) 0.061(2) 0.0372(17) -0.0035(17) 0.0018(17) 0.0037(19) C23 0.049(2) 0.050(2) 0.0371(17) 0.0046(15) 0.0048(15) 0.0005(17) C24 0.063(3) 0.066(3) 0.049(2) -0.0092(19) 0.0174(19) 0.010(2) C25 0.132(6) 0.100(5) 0.195(8) -0.002(5) 0.116(6) 0.008(4) C26 0.089(4) 0.094(4) 0.176(7) -0.075(5) 0.015(4) 0.011(3) C27 0.049(2) 0.062(3) 0.0441(19) 0.0059(17) 0.0033(16) 0.0078(18) C28 0.072(3) 0.076(3) 0.070(3) -0.003(2) -0.019(2) -0.001(3) C29 0.074(3) 0.060(3) 0.079(3) 0.007(2) -0.004(2) 0.009(2) C31 0.048(2) 0.044(2) 0.0344(16) 0.0013(14) 0.0048(15) 0.0038(16) C32 0.065(3) 0.058(2) 0.0402(18) 0.0044(17) 0.0137(18) 0.002(2) C33 0.054(2) 0.048(2) 0.0379(16) 0.0009(15) 0.0106(16) 0.0014(17) C34 0.062(3) 0.060(3) 0.054(2) 0.0087(19) 0.0104(19) 0.019(2) C35 0.070(4) 0.113(5) 0.113(5) -0.011(4) -0.023(3) 0.019(3) C36 0.086(4) 0.064(3) 0.132(5) 0.005(3) 0.020(4) 0.017(3) C37 0.067(3) 0.054(2) 0.049(2) 0.0012(18) 0.0209(19) 0.007(2) C38 0.065(3) 0.090(4) 0.079(3) -0.004(3) 0.026(3) 0.009(3) C39 0.102(4) 0.099(4) 0.054(2) 0.004(2) 0.034(3) 0.017(3) P 0.0433(5) 0.0520(6) 0.0388(4) -0.0011(4) 0.0065(4) 0.0076(4) Cl1 0.0738(8) 0.0670(7) 0.0741(7) 0.0032(6) 0.0185(6) 0.0183(6) O11 0.069(2) 0.107(3) 0.0707(19) 0.0016(19) 0.0086(16) 0.035(2) O12 0.144(4) 0.078(3) 0.149(4) 0.028(3) 0.054(3) 0.043(3) O13 0.082(2) 0.104(3) 0.119(3) 0.007(2) 0.051(2) 0.015(2) O14 0.085(3) 0.111(3) 0.081(2) -0.009(2) 0.008(2) 0.003(2) Cl2 0.0873(11) 0.1138(12) 0.0999(11) 0.0258(9) 0.0299(9) 0.0333(9) O21 0.320(13) 0.346(14) 0.393(15) -0.023(12) 0.124(12) 0.242(12) O22 0.142(6) 0.400(14) 0.294(11) 0.188(11) 0.048(6) -0.047(7) O23 0.120(5) 0.353(11) 0.135(5) -0.028(6) -0.009(4) 0.087(6) O24 0.104(4) 0.106(3) 0.138(4) 0.002(3) 0.015(3) 0.000(3) C1 0.115(5) 0.099(4) 0.080(3) 0.015(3) 0.040(3) 0.015(3) Cl11 0.251(3) 0.151(2) 0.1298(16) -0.0068(15) 0.0674(18) -0.083(2) Cl12 0.178(2) 0.1432(17) 0.0889(11) 0.0029(11) 0.0154(12) -0.0317(15) Cl13 0.1431(16) 0.1519(17) 0.0890(10) 0.0172(10) 0.0501(11) 0.0285(12) C2 0.094(4) 0.090(4) 0.061(3) -0.010(3) 0.016(3) -0.022(3) Cl21 0.173(2) 0.1368(17) 0.1272(15) 0.0192(13) 0.0138(14) 0.0383(15) Cl22 0.198(3) 0.175(2) 0.1050(13) -0.0631(14) -0.0206(14) -0.0191(17) Cl23 0.1424(16) 0.1107(13) 0.1012(11) -0.0171(10) 0.0346(11) 0.0124(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co O11 1.999(3) . ? Co N32 2.023(3) . ? Co N12 2.024(3) . ? Co N22 2.033(3) . ? Co O14 2.502(4) . ? N11 C11 1.358(5) . ? N11 C12 1.369(6) . ? N11 C14 1.493(6) . ? N12 C11 1.343(5) . ? N12 C13 1.379(5) . ? N21 C21 1.342(4) . ? N21 C22 1.389(5) . ? N21 C24 1.482(5) . ? N22 C21 1.350(5) . ? N22 C23 1.375(4) . ? N31 C31 1.345(4) . ? N31 C32 1.372(5) . ? N31 C34 1.480(5) . ? N32 C31 1.339(5) . ? N32 C33 1.391(4) . ? C11 P 1.821(4) . ? C12 C13 1.360(6) . ? C13 C17 1.499(6) . ? C14 C15 1.421(10) . ? C14 C16 1.463(11) . ? C17 C18 1.528(7) . ? C17 C19 1.543(7) . ? C21 P 1.822(4) . ? C22 C23 1.363(5) . ? C23 C27 1.508(5) . ? C24 C26 1.489(7) . ? C24 C25 1.500(8) . ? C27 C29 1.517(6) . ? C27 C28 1.523(6) . ? C31 P 1.828(4) . ? C32 C33 1.364(5) . ? C33 C37 1.494(5) . ? C34 C36 1.497(7) . ? C34 C35 1.506(7) . ? C37 C39 1.533(6) . ? C37 C38 1.538(7) . ? Cl1 O12 1.410(4) . ? Cl1 O13 1.424(4) . ? Cl1 O14 1.443(4) . ? Cl1 O11 1.443(4) . ? Cl2 O21 1.303(9) . ? Cl2 O22 1.335(7) . ? Cl2 O23 1.416(7) . ? Cl2 O24 1.425(5) . ? C1 Cl11 1.742(6) . ? C1 Cl13 1.746(6) . ? C1 Cl12 1.748(7) . ? C2 Cl22 1.714(5) . ? C2 Cl21 1.733(6) . ? C2 Cl23 1.770(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Co N32 121.41(14) . . ? O11 Co N12 135.97(16) . . ? N32 Co N12 96.77(12) . . ? O11 Co N22 101.71(13) . . ? N32 Co N22 96.92(11) . . ? N12 Co N22 93.79(12) . . ? O11 Co O14 59.42(14) . . ? N32 Co O14 98.76(12) . . ? N12 Co O14 96.47(13) . . ? N22 Co O14 160.08(12) . . ? C11 N11 C12 106.9(4) . . ? C11 N11 C14 125.9(4) . . ? C12 N11 C14 127.2(4) . . ? C11 N12 C13 107.3(3) . . ? C11 N12 Co 114.0(3) . . ? C13 N12 Co 138.4(3) . . ? C21 N21 C22 107.2(3) . . ? C21 N21 C24 126.9(3) . . ? C22 N21 C24 125.8(3) . . ? C21 N22 C23 106.6(3) . . ? C21 N22 Co 114.8(2) . . ? C23 N22 Co 138.6(3) . . ? C31 N31 C32 107.1(3) . . ? C31 N31 C34 127.6(3) . . ? C32 N31 C34 125.3(3) . . ? C31 N32 C33 106.7(3) . . ? C31 N32 Co 114.8(2) . . ? C33 N32 Co 138.2(2) . . ? N12 C11 N11 109.8(3) . . ? N12 C11 P 126.7(3) . . ? N11 C11 P 123.4(3) . . ? C13 C12 N11 108.4(4) . . ? C12 C13 N12 107.6(4) . . ? C12 C13 C17 130.0(4) . . ? N12 C13 C17 122.3(4) . . ? C15 C14 C16 122.0(7) . . ? C15 C14 N11 112.3(6) . . ? C16 C14 N11 110.7(6) . . ? C13 C17 C18 110.9(4) . . ? C13 C17 C19 110.5(4) . . ? C18 C17 C19 109.2(4) . . ? N21 C21 N22 110.4(3) . . ? N21 C21 P 124.0(3) . . ? N22 C21 P 125.5(3) . . ? C23 C22 N21 107.0(3) . . ? C22 C23 N22 108.7(3) . . ? C22 C23 C27 129.1(3) . . ? N22 C23 C27 122.0(3) . . ? N21 C24 C26 111.0(4) . . ? N21 C24 C25 110.5(4) . . ? C26 C24 C25 115.4(5) . . ? C23 C27 C29 110.4(3) . . ? C23 C27 C28 111.7(4) . . ? C29 C27 C28 111.4(4) . . ? N32 C31 N31 110.6(3) . . ? N32 C31 P 126.0(3) . . ? N31 C31 P 123.3(3) . . ? C33 C32 N31 108.0(3) . . ? C32 C33 N32 107.5(3) . . ? C32 C33 C37 129.9(3) . . ? N32 C33 C37 122.6(3) . . ? N31 C34 C36 110.5(4) . . ? N31 C34 C35 110.2(4) . . ? C36 C34 C35 113.3(5) . . ? C33 C37 C39 111.4(4) . . ? C33 C37 C38 109.7(3) . . ? C39 C37 C38 110.5(4) . . ? C11 P C21 97.21(17) . . ? C11 P C31 96.98(17) . . ? C21 P C31 98.87(16) . . ? O12 Cl1 O13 111.3(3) . . ? O12 Cl1 O14 111.4(3) . . ? O13 Cl1 O14 110.1(3) . . ? O12 Cl1 O11 108.9(3) . . ? O13 Cl1 O11 110.9(2) . . ? O14 Cl1 O11 103.9(2) . . ? Cl1 O11 Co 109.40(19) . . ? Cl1 O14 Co 87.24(17) . . ? O21 Cl2 O22 117.5(8) . . ? O21 Cl2 O23 104.9(7) . . ? O22 Cl2 O23 111.5(7) . . ? O21 Cl2 O24 111.2(7) . . ? O22 Cl2 O24 107.0(4) . . ? O23 Cl2 O24 103.8(4) . . ? Cl11 C1 Cl13 109.4(4) . . ? Cl11 C1 Cl12 110.4(3) . . ? Cl13 C1 Cl12 110.2(4) . . ? Cl22 C2 Cl21 110.9(3) . . ? Cl22 C2 Cl23 110.8(3) . . ? Cl21 C2 Cl23 109.6(3) . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 0.709 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.073 data_pims10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H55 Cl2 Co N6 O11 P' _chemical_formula_weight 824.59 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' 'P' 'P' 0.1023 0.0942 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6185(8) _cell_length_b 18.2452(11) _cell_length_c 17.6528(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.5370(10) _cell_angle_gamma 90.00 _cell_volume 4064.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9377 _exptl_absorpt_correction_T_max 0.9377 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(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 28024 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9302 _reflns_number_gt 7543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+2.6687P] 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 SHELXL _refine_ls_extinction_coef 0.0003(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9302 _refine_ls_number_parameters 522 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1294 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 4.172 _refine_ls_shift/su_mean 0.172 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 Co Co 0.05853(2) 0.138059(16) 0.207900(16) 0.02968(10) Uani 1 1 d . . . O1 O 0.0522(2) 0.24658(11) 0.17159(12) 0.0457(4) Uani 1 1 d . . . H1A H 0.005(3) 0.264(2) 0.158(2) 0.071(13) Uiso 1 1 d . . . H1B H 0.099(3) 0.263(2) 0.141(2) 0.082(13) Uiso 1 1 d . . . O2 O 0.17729(14) 0.16466(11) 0.28693(11) 0.0461(4) Uani 1 1 d . . . H2 H 0.174(3) 0.142(2) 0.333(2) 0.083(12) Uiso 1 1 d . . . C2 C 0.2646(3) 0.2126(3) 0.2930(3) 0.1017(15) Uani 1 1 d . . . H2A H 0.3270 0.1891 0.2724 0.152 Uiso 1 1 calc R . . H2B H 0.2771 0.2246 0.3458 0.152 Uiso 1 1 calc R . . H2C H 0.2496 0.2571 0.2647 0.152 Uiso 1 1 calc R . . N11 N -0.22474(15) 0.06420(11) 0.10897(11) 0.0355(4) Uani 1 1 d . . . N12 N -0.06032(15) 0.10158(10) 0.12987(10) 0.0328(4) Uani 1 1 d . . . N21 N 0.00036(16) -0.07731(11) 0.28784(11) 0.0373(4) Uani 1 1 d . . . N22 N 0.06871(15) 0.02621(10) 0.24356(10) 0.0315(4) Uani 1 1 d . . . N31 N -0.19554(17) 0.13425(11) 0.36559(12) 0.0389(5) Uani 1 1 d . . . N32 N -0.05823(15) 0.16048(11) 0.29313(10) 0.0325(4) Uani 1 1 d . . . C11 C -0.14387(17) 0.06751(12) 0.15956(12) 0.0308(4) Uani 1 1 d . . . C12 C -0.1904(2) 0.09746(15) 0.04404(14) 0.0428(6) Uani 1 1 d . . . H12A H -0.2300 0.1038 -0.0009 0.051 Uiso 1 1 calc R . . C13 C -0.0889(2) 0.11967(13) 0.05629(13) 0.0371(5) Uani 1 1 d . . . C14 C -0.3339(2) 0.03925(17) 0.12427(17) 0.0501(7) Uani 1 1 d . . . H14A H -0.3300 -0.0009 0.1619 0.060 Uiso 1 1 calc R . . C15 C -0.3855(3) 0.0095(3) 0.0536(2) 0.0885(14) Uani 1 1 d . . . H15A H -0.3945 0.0487 0.0171 0.133 Uiso 1 1 calc R . . H15B H -0.4541 -0.0110 0.0660 0.133 Uiso 1 1 calc R . . H15C H -0.3410 -0.0285 0.0323 0.133 Uiso 1 1 calc R . . C16 C -0.3961(3) 0.1015(3) 0.1587(4) 0.122(2) Uani 1 1 d . . . H16A H -0.3620 0.1169 0.2055 0.182 Uiso 1 1 calc R . . H16B H -0.4676 0.0851 0.1692 0.182 Uiso 1 1 calc R . . H16C H -0.3986 0.1423 0.1235 0.182 Uiso 1 1 calc R . . C17 C -0.0145(2) 0.15164(16) -0.00090(14) 0.0471(6) Uani 1 1 d . . . H17A H 0.0340 0.1859 0.0256 0.056 Uiso 1 1 calc R . . C18 C 0.0517(3) 0.0913(2) -0.0369(2) 0.0736(10) Uani 1 1 d . . . H18A H 0.0872 0.0632 0.0025 0.110 Uiso 1 1 calc R . . H18B H 0.1041 0.1131 -0.0698 0.110 Uiso 1 1 calc R . . H18C H 0.0059 0.0592 -0.0663 0.110 Uiso 1 1 calc R . . C19 C -0.0761(3) 0.1945(2) -0.06140(18) 0.0679(9) Uani 1 1 d . . . H19A H -0.1167 0.1607 -0.0926 0.102 Uiso 1 1 calc R . . H19B H -0.0268 0.2213 -0.0929 0.102 Uiso 1 1 calc R . . H19C H -0.1238 0.2287 -0.0371 0.102 Uiso 1 1 calc R . . C21 C -0.02069(18) -0.00872(12) 0.26188(12) 0.0310(4) Uani 1 1 d . . . C22 C 0.1085(2) -0.08596(15) 0.28508(15) 0.0446(6) Uani 1 1 d . . . H22A H 0.1466 -0.1280 0.2995 0.054 Uiso 1 1 calc R . . C23 C 0.15047(19) -0.02252(14) 0.25767(13) 0.0372(5) Uani 1 1 d . . . C24 C -0.0782(2) -0.13231(14) 0.31347(16) 0.0455(6) Uani 1 1 d . . . H24A H -0.1410 -0.1056 0.3322 0.055 Uiso 1 1 calc R . . C25 C -0.0333(3) -0.1774(2) 0.3787(2) 0.0752(10) Uani 1 1 d . . . H25A H 0.0227 -0.2089 0.3603 0.113 Uiso 1 1 calc R . . H25B H -0.0891 -0.2072 0.4002 0.113 Uiso 1 1 calc R . . H25C H -0.0050 -0.1448 0.4173 0.113 Uiso 1 1 calc R . . C26 C -0.1132(4) -0.1796(2) 0.2484(2) 0.0871(13) Uani 1 1 d . . . H26A H -0.1396 -0.1488 0.2075 0.131 Uiso 1 1 calc R . . H26B H -0.1691 -0.2123 0.2649 0.131 Uiso 1 1 calc R . . H26C H -0.0537 -0.2082 0.2306 0.131 Uiso 1 1 calc R . . C27 C 0.2641(2) -0.00567(16) 0.24012(15) 0.0442(6) Uani 1 1 d . . . H27A H 0.2725 0.0483 0.2392 0.053 Uiso 1 1 calc R . . C28 C 0.3393(3) -0.0363(3) 0.3007(2) 0.0878(13) Uani 1 1 d . . . H28A H 0.3252 -0.0128 0.3488 0.132 Uiso 1 1 calc R . . H28B H 0.4120 -0.0267 0.2862 0.132 Uiso 1 1 calc R . . H28C H 0.3285 -0.0887 0.3054 0.132 Uiso 1 1 calc R . . C29 C 0.2913(3) -0.0349(2) 0.16182(19) 0.0622(8) Uani 1 1 d . . . H29A H 0.2921 -0.0881 0.1630 0.093 Uiso 1 1 calc R . . H29B H 0.3605 -0.0170 0.1472 0.093 Uiso 1 1 calc R . . H29C H 0.2385 -0.0183 0.1254 0.093 Uiso 1 1 calc R . . C31 C -0.13511(18) 0.11166(12) 0.30738(12) 0.0311(4) Uani 1 1 d . . . C32 C -0.1558(2) 0.20015(14) 0.38918(16) 0.0477(6) Uani 1 1 d . . . H32A H -0.1822 0.2290 0.4289 0.057 Uiso 1 1 calc R . . C33 C -0.0713(2) 0.21647(13) 0.34498(14) 0.0393(5) Uani 1 1 d . . . C34 C -0.2889(2) 0.09691(16) 0.39833(16) 0.0478(6) Uani 1 1 d . . . H34A H -0.2983 0.0490 0.3729 0.057 Uiso 1 1 calc R . . C35 C -0.3876(3) 0.1427(3) 0.3852(3) 0.1016(17) Uani 1 1 d . . . H35A H -0.3793 0.1897 0.4102 0.152 Uiso 1 1 calc R . . H35B H -0.4485 0.1173 0.4057 0.152 Uiso 1 1 calc R . . H35C H -0.3980 0.1503 0.3313 0.152 Uiso 1 1 calc R . . C36 C -0.2722(3) 0.0841(2) 0.4818(2) 0.0796(11) Uani 1 1 d . . . H36A H -0.2043 0.0602 0.4901 0.119 Uiso 1 1 calc R . . H36B H -0.3284 0.0530 0.5008 0.119 Uiso 1 1 calc R . . H36C H -0.2730 0.1306 0.5083 0.119 Uiso 1 1 calc R . . C37 C -0.0044(2) 0.28462(14) 0.34759(15) 0.0458(6) Uani 1 1 d . . . H37A H 0.0537 0.2789 0.3108 0.055 Uiso 1 1 calc R . . C38 C -0.0708(3) 0.35086(17) 0.3240(2) 0.0676(9) Uani 1 1 d . . . H38A H -0.1009 0.3425 0.2740 0.101 Uiso 1 1 calc R . . H38B H -0.0262 0.3942 0.3230 0.101 Uiso 1 1 calc R . . H38C H -0.1274 0.3580 0.3601 0.101 Uiso 1 1 calc R . . C39 C 0.0446(3) 0.2957(2) 0.42567(18) 0.0706(10) Uani 1 1 d . . . H39A H -0.0111 0.3010 0.4627 0.106 Uiso 1 1 calc R . . H39B H 0.0881 0.3395 0.4255 0.106 Uiso 1 1 calc R . . H39C H 0.0882 0.2536 0.4386 0.106 Uiso 1 1 calc R . . C3 C 0.0795(4) 0.0614(3) 0.4430(2) 0.0831(11) Uani 1 1 d . . . H3A H 0.0870 0.0514 0.4968 0.125 Uiso 1 1 calc R . . H3B H 0.0722 0.0155 0.4157 0.125 Uiso 1 1 calc R . . H3C H 0.0171 0.0913 0.4343 0.125 Uiso 1 1 calc R . . O3 O 0.1671(3) 0.0978(3) 0.41813(18) 0.1252(17) Uani 1 1 d . . . H3 H 0.203(5) 0.109(3) 0.450(3) 0.12(2) Uiso 1 1 d . . . P P -0.15464(4) 0.02781(3) 0.25397(3) 0.02926(13) Uani 1 1 d . . . Cl1 Cl 0.27291(6) 0.17543(5) 0.09140(6) 0.0697(3) Uani 1 1 d . . . O11 O 0.18939(16) 0.12927(11) 0.12138(11) 0.0504(5) Uani 1 1 d . . . O12 O 0.2786(4) 0.1610(3) 0.0106(2) 0.1504(17) Uani 1 1 d . . . O13 O 0.2465(2) 0.25043(15) 0.0999(2) 0.1004(11) Uani 1 1 d . . . O14 O 0.3670(2) 0.1581(2) 0.1239(3) 0.161(2) Uani 1 1 d . . . Cl2 Cl -0.1418(8) 0.3603(5) 0.0833(6) 0.0762(12) Uani 0.424(4) 1 d PD A 1 O21 O -0.1487(7) 0.3003(6) 0.1301(6) 0.083(3) Uani 0.424(4) 1 d PD A 1 O22 O -0.2037(14) 0.3543(9) 0.0210(8) 0.292(12) Uani 0.424(4) 1 d PD A 1 O23 O -0.0366(6) 0.3676(6) 0.0628(5) 0.109(4) Uani 0.424(4) 1 d PD A 1 O24 O -0.1658(11) 0.4203(4) 0.1290(7) 0.138(5) Uani 0.424(4) 1 d PD A 1 Cl2A Cl -0.1286(6) 0.3793(4) 0.0794(5) 0.0762(12) Uani 0.58 1 d PD A 2 O21A O -0.1439(9) 0.3094(5) 0.1061(6) 0.148(5) Uani 0.576(4) 1 d PD A 2 O22A O -0.0729(15) 0.4230(8) 0.1211(11) 0.396(18) Uani 0.576(4) 1 d PD A 2 O23A O -0.2279(6) 0.4065(5) 0.0707(7) 0.141(4) Uani 0.576(4) 1 d PD A 2 O24A O -0.0899(16) 0.3727(7) 0.0097(8) 0.345(14) Uani 0.576(4) 1 d PD A 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 Co 0.02693(16) 0.02994(17) 0.03215(16) 0.00080(11) 0.00020(11) -0.00228(11) O1 0.0490(12) 0.0379(10) 0.0503(11) 0.0068(8) 0.0031(9) 0.0007(9) O2 0.0387(10) 0.0531(11) 0.0463(10) -0.0012(9) -0.0080(8) -0.0093(8) C2 0.075(3) 0.123(4) 0.106(3) -0.008(3) -0.015(2) -0.050(3) N11 0.0326(10) 0.0365(10) 0.0373(10) 0.0037(8) -0.0067(8) -0.0040(8) N12 0.0335(10) 0.0326(10) 0.0322(9) 0.0029(7) -0.0022(7) -0.0035(8) N21 0.0404(11) 0.0309(10) 0.0407(10) 0.0060(8) 0.0055(8) 0.0052(8) N22 0.0291(9) 0.0323(9) 0.0332(9) 0.0013(7) -0.0010(7) 0.0024(7) N31 0.0393(11) 0.0348(10) 0.0428(11) -0.0039(8) 0.0139(9) -0.0006(8) N32 0.0322(10) 0.0304(9) 0.0350(9) -0.0028(7) 0.0025(8) -0.0018(8) C11 0.0313(11) 0.0283(10) 0.0327(10) 0.0006(8) -0.0024(9) -0.0002(9) C12 0.0460(14) 0.0464(14) 0.0358(12) 0.0068(10) -0.0116(10) -0.0057(11) C13 0.0443(13) 0.0365(12) 0.0305(11) 0.0035(9) -0.0043(10) -0.0036(10) C14 0.0337(13) 0.0593(17) 0.0571(16) 0.0115(13) -0.0112(12) -0.0115(12) C15 0.078(2) 0.119(3) 0.068(2) 0.031(2) -0.0364(19) -0.060(2) C16 0.046(2) 0.121(4) 0.198(6) -0.024(4) 0.020(3) 0.014(2) C17 0.0556(16) 0.0513(15) 0.0342(12) 0.0084(11) -0.0021(11) -0.0135(13) C18 0.087(3) 0.071(2) 0.063(2) 0.0034(17) 0.0309(19) -0.0038(19) C19 0.078(2) 0.077(2) 0.0487(16) 0.0276(16) -0.0110(15) -0.0222(18) C21 0.0327(11) 0.0281(10) 0.0322(10) 0.0006(8) -0.0001(9) 0.0030(9) C22 0.0422(14) 0.0409(13) 0.0508(14) 0.0079(11) 0.0031(11) 0.0147(11) C23 0.0325(12) 0.0413(13) 0.0378(12) 0.0001(10) -0.0001(9) 0.0087(10) C24 0.0535(16) 0.0333(13) 0.0498(14) 0.0093(11) 0.0136(12) 0.0011(11) C25 0.095(3) 0.061(2) 0.070(2) 0.0319(17) 0.0072(19) 0.0017(19) C26 0.106(3) 0.085(3) 0.070(2) 0.000(2) 0.006(2) -0.051(2) C27 0.0331(13) 0.0525(15) 0.0470(14) 0.0013(12) 0.0013(10) 0.0079(11) C28 0.0434(18) 0.143(4) 0.077(2) 0.028(2) -0.0090(17) 0.016(2) C29 0.0500(17) 0.072(2) 0.0645(19) -0.0097(16) 0.0179(14) 0.0068(15) C31 0.0310(11) 0.0295(10) 0.0329(10) 0.0006(8) 0.0030(8) 0.0022(9) C32 0.0539(16) 0.0388(13) 0.0508(14) -0.0116(11) 0.0179(12) -0.0033(12) C33 0.0438(13) 0.0322(12) 0.0422(12) -0.0073(10) 0.0075(10) -0.0020(10) C34 0.0469(15) 0.0443(15) 0.0527(15) 0.0005(12) 0.0210(12) -0.0046(12) C35 0.048(2) 0.125(4) 0.132(4) 0.053(3) 0.031(2) 0.017(2) C36 0.097(3) 0.082(3) 0.060(2) 0.0121(18) 0.0204(19) -0.019(2) C37 0.0506(15) 0.0379(13) 0.0491(14) -0.0119(11) 0.0132(12) -0.0089(11) C38 0.073(2) 0.0375(15) 0.093(2) -0.0029(15) 0.0153(19) -0.0050(14) C39 0.080(2) 0.075(2) 0.0570(18) -0.0159(16) 0.0045(16) -0.0327(19) C3 0.092(3) 0.097(3) 0.060(2) 0.007(2) -0.013(2) -0.003(2) O3 0.119(3) 0.189(4) 0.0672(18) 0.047(2) -0.0427(19) -0.063(3) P 0.0277(3) 0.0274(3) 0.0327(3) 0.0020(2) 0.0005(2) -0.0011(2) Cl1 0.0436(4) 0.0712(5) 0.0948(6) 0.0274(5) 0.0251(4) 0.0020(4) O11 0.0479(11) 0.0515(11) 0.0520(11) 0.0102(9) 0.0154(9) 0.0014(9) O12 0.180(4) 0.180(4) 0.093(2) 0.008(2) 0.079(3) -0.053(3) O13 0.0674(16) 0.0599(15) 0.175(3) 0.0376(18) 0.0387(18) -0.0013(13) O14 0.0454(16) 0.127(3) 0.308(6) 0.080(4) -0.028(2) -0.0105(18) Cl2 0.0633(15) 0.070(3) 0.0950(13) 0.0184(18) 0.0094(10) 0.0216(18) O21 0.059(4) 0.093(6) 0.096(5) 0.040(4) -0.011(3) 0.036(4) O22 0.289(19) 0.42(3) 0.168(12) -0.042(15) -0.179(13) 0.23(2) O23 0.068(4) 0.172(10) 0.087(6) 0.029(6) 0.042(4) 0.041(5) O24 0.202(12) 0.060(5) 0.155(9) 0.019(5) 0.111(9) 0.075(7) Cl2A 0.0633(15) 0.070(3) 0.0950(13) 0.0184(18) 0.0094(10) 0.0216(18) O21A 0.154(8) 0.089(7) 0.202(12) -0.051(7) 0.048(7) -0.057(6) O22A 0.43(3) 0.27(2) 0.49(3) 0.176(19) -0.38(2) -0.23(2) O23A 0.091(5) 0.144(7) 0.187(9) 0.075(7) 0.030(6) 0.046(5) O24A 0.54(3) 0.180(11) 0.322(18) -0.032(12) 0.37(2) -0.044(15) _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 Co O1 2.083(2) . ? Co O2 2.0948(18) . ? Co N12 2.1332(18) . ? Co N22 2.1392(19) . ? Co N32 2.1549(18) . ? Co O11 2.2655(19) . ? O2 C2 1.410(4) . ? N11 C11 1.351(3) . ? N11 C12 1.371(3) . ? N11 C14 1.478(3) . ? N12 C11 1.335(3) . ? N12 C13 1.385(3) . ? N21 C21 1.358(3) . ? N21 C22 1.375(3) . ? N21 C24 1.484(3) . ? N22 C21 1.338(3) . ? N22 C23 1.383(3) . ? N31 C31 1.350(3) . ? N31 C32 1.366(3) . ? N31 C34 1.482(3) . ? N32 C31 1.343(3) . ? N32 C33 1.382(3) . ? C11 P 1.823(2) . ? C12 C13 1.360(4) . ? C13 C17 1.503(4) . ? C14 C15 1.502(4) . ? C14 C16 1.511(6) . ? C17 C18 1.525(5) . ? C17 C19 1.530(4) . ? C21 P 1.821(2) . ? C22 C23 1.364(4) . ? C23 C27 1.502(3) . ? C24 C26 1.500(5) . ? C24 C25 1.520(4) . ? C27 C29 1.524(4) . ? C27 C28 1.528(4) . ? C31 P 1.813(2) . ? C32 C33 1.361(4) . ? C33 C37 1.503(3) . ? C34 C36 1.504(4) . ? C34 C35 1.515(5) . ? C37 C39 1.519(4) . ? C37 C38 1.526(4) . ? C3 O3 1.366(5) . ? Cl1 O14 1.351(3) . ? Cl1 O13 1.417(3) . ? Cl1 O11 1.453(2) . ? Cl1 O12 1.453(4) . ? Cl2 O24 1.395(10) . ? Cl2 O23 1.385(10) . ? Cl2 O22 1.347(11) . ? Cl2 O21 1.374(9) . ? Cl2A O22A 1.289(10) . ? Cl2A O21A 1.373(9) . ? Cl2A O23A 1.356(9) . ? Cl2A O24A 1.333(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co O2 90.57(8) . . ? O1 Co N12 94.19(8) . . ? O2 Co N12 175.20(8) . . ? O1 Co N22 178.53(8) . . ? O2 Co N22 89.11(7) . . ? N12 Co N22 86.12(7) . . ? O1 Co N32 90.56(8) . . ? O2 Co N32 88.89(7) . . ? N12 Co N32 91.66(7) . . ? N22 Co N32 90.87(7) . . ? O1 Co O11 83.45(8) . . ? O2 Co O11 86.79(8) . . ? N12 Co O11 93.16(8) . . ? N22 Co O11 95.09(7) . . ? N32 Co O11 172.57(7) . . ? C2 O2 Co 138.4(2) . . ? C11 N11 C12 106.89(19) . . ? C11 N11 C14 126.3(2) . . ? C12 N11 C14 126.2(2) . . ? C11 N12 C13 106.24(19) . . ? C11 N12 Co 116.40(14) . . ? C13 N12 Co 134.95(16) . . ? C21 N21 C22 106.5(2) . . ? C21 N21 C24 126.7(2) . . ? C22 N21 C24 126.8(2) . . ? C21 N22 C23 106.23(19) . . ? C21 N22 Co 118.50(14) . . ? C23 N22 Co 135.16(16) . . ? C31 N31 C32 107.0(2) . . ? C31 N31 C34 127.8(2) . . ? C32 N31 C34 125.2(2) . . ? C31 N32 C33 106.00(19) . . ? C31 N32 Co 120.32(15) . . ? C33 N32 Co 133.54(16) . . ? N12 C11 N11 110.83(19) . . ? N12 C11 P 127.56(16) . . ? N11 C11 P 121.60(17) . . ? C13 C12 N11 107.7(2) . . ? C12 C13 N12 108.4(2) . . ? C12 C13 C17 127.1(2) . . ? N12 C13 C17 124.3(2) . . ? N11 C14 C15 110.9(3) . . ? N11 C14 C16 109.3(3) . . ? C15 C14 C16 112.5(3) . . ? C13 C17 C18 110.4(2) . . ? C13 C17 C19 110.6(2) . . ? C18 C17 C19 110.8(3) . . ? N22 C21 N21 110.97(19) . . ? N22 C21 P 126.24(16) . . ? N21 C21 P 122.79(17) . . ? C23 C22 N21 107.7(2) . . ? C22 C23 N22 108.5(2) . . ? C22 C23 C27 128.5(2) . . ? N22 C23 C27 122.9(2) . . ? N21 C24 C26 110.4(2) . . ? N21 C24 C25 110.6(3) . . ? C26 C24 C25 112.0(3) . . ? C23 C27 C29 109.8(2) . . ? C23 C27 C28 111.6(2) . . ? C29 C27 C28 111.3(3) . . ? N32 C31 N31 110.8(2) . . ? N32 C31 P 123.88(16) . . ? N31 C31 P 125.36(17) . . ? C33 C32 N31 107.8(2) . . ? C32 C33 N32 108.5(2) . . ? C32 C33 C37 127.3(2) . . ? N32 C33 C37 124.2(2) . . ? N31 C34 C36 110.4(3) . . ? N31 C34 C35 110.0(3) . . ? C36 C34 C35 110.1(3) . . ? C33 C37 C39 111.2(2) . . ? C33 C37 C38 109.9(2) . . ? C39 C37 C38 111.1(3) . . ? C31 P C21 98.48(10) . . ? C31 P C11 97.43(10) . . ? C21 P C11 97.95(10) . . ? O14 Cl1 O13 112.8(3) . . ? O14 Cl1 O11 110.34(19) . . ? O13 Cl1 O11 110.41(14) . . ? O14 Cl1 O12 108.8(3) . . ? O13 Cl1 O12 107.0(3) . . ? O11 Cl1 O12 107.19(19) . . ? Cl1 O11 Co 137.77(13) . . ? O24 Cl2 O23 106.8(8) . . ? O24 Cl2 O22 114.1(9) . . ? O23 Cl2 O22 110.2(12) . . ? O24 Cl2 O21 105.1(9) . . ? O23 Cl2 O21 107.4(8) . . ? O22 Cl2 O21 112.7(10) . . ? O22A Cl2A O21A 117.1(9) . . ? O22A Cl2A O23A 109.7(9) . . ? O21A Cl2A O23A 104.2(7) . . ? O22A Cl2A O24A 112.4(9) . . ? O21A Cl2A O24A 106.7(8) . . ? O23A Cl2A O24A 106.0(9) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.815 _refine_diff_density_min -0.830 _refine_diff_density_rms 0.057