# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2135 data_wagchp _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69.57 H73.94 Cl8.69 Co7 N11.75 O18.69' _chemical_formula_weight 2094.30 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 14.407(4) _cell_length_b 14.512(4) _cell_length_c 23.321(6) _cell_angle_alpha 90.537(14) _cell_angle_beta 93.796(17) _cell_angle_gamma 113.40(2) _cell_volume 4462(2) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Rod _exptl_crystal_colour Purple _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.598 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.6994 _exptl_absorpt_correction_T_max 0.7994 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 'Omega-theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% ? _diffrn_reflns_number 10286 _diffrn_reflns_av_R_equivalents 0.3462 _diffrn_reflns_av_sigmaI/netI 0.1353 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 22.50 _reflns_number_total 9627 _reflns_number_gt 5168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _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^)+(0.0441P)^2^+39.9446P] 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 9627 _refine_ls_number_parameters 1022 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.1598 _refine_ls_R_factor_gt 0.0761 _refine_ls_wR_factor_ref 0.1943 _refine_ls_wR_factor_gt 0.1428 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.069 _refine_ls_shift/su_mean 0.003 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co4 Co 0.54995(15) 0.84913(14) 0.18665(8) 0.0469(6) Uani 1 1 d . . . Co5 Co 0.40704(16) 0.63059(15) 0.19377(9) 0.0570(6) Uani 1 1 d . . . Co6 Co 0.60788(14) 0.62635(14) 0.24313(8) 0.0451(5) Uani 1 1 d . . . Co7 Co 0.89716(14) 0.81493(14) 0.24930(8) 0.0450(5) Uani 1 1 d . . . Co3 Co 0.84320(14) 1.01160(14) 0.20702(8) 0.0477(6) Uani 1 1 d . . . Co2 Co 0.52451(14) 0.75581(13) 0.33664(8) 0.0433(5) Uani 1 1 d . . . Co1 Co 0.75829(13) 0.89463(13) 0.32067(8) 0.0389(5) Uani 1 1 d . . . O2 O 0.5694(6) 0.7169(6) 0.1872(4) 0.049(2) Uani 1 1 d . . . H2 H 0.5859 0.7037 0.1483 0.058 Uiso 1 1 calc R . . O1 O 0.7934(6) 0.8736(6) 0.2371(3) 0.038(2) Uani 1 1 d . . . H1 H 0.7327 0.8271 0.2136 0.046 Uiso 1 1 calc R . . O1B O 0.7415(7) 0.9219(6) 0.4035(4) 0.048(3) Uani 1 1 d . . . O2B O 0.5772(7) 0.8277(7) 0.4132(4) 0.050(3) Uani 1 1 d . . . C1B C 0.6660(13) 0.8904(11) 0.4319(6) 0.042(4) Uani 1 1 d . . . C2B C 0.6786(10) 0.9270(10) 0.4942(6) 0.062(5) Uani 1 1 d D A . C3B C 0.7806(16) 1.0095(18) 0.5113(13) 0.087(11) Uiso 0.53 1 d PD A 1 H3B1 H 0.7858 1.0704 0.4924 0.131 Uiso 0.53 1 d PR A 1 H3B2 H 0.8337 0.9897 0.4998 0.131 Uiso 0.53 1 d PR A 1 H3B3 H 0.7879 1.0216 0.5527 0.131 Uiso 0.53 1 d PR A 1 C4B C 0.669(3) 0.8363(18) 0.5290(14) 0.121(14) Uiso 0.53 1 d PD A 1 H4B1 H 0.5999 0.8027 0.5393 0.181 Uiso 0.53 1 d PR A 1 H4B2 H 0.7146 0.8574 0.5637 0.181 Uiso 0.53 1 d PR A 1 H4B3 H 0.6870 0.7904 0.5060 0.181 Uiso 0.53 1 d PR A 1 C5B C 0.5950(19) 0.959(2) 0.5088(16) 0.130(16) Uiso 0.53 1 d PD A 1 H5B1 H 0.5316 0.9005 0.5101 0.196 Uiso 0.53 1 d PR A 1 H5B2 H 0.5871 1.0032 0.4798 0.196 Uiso 0.53 1 d PR A 1 H5B3 H 0.6131 0.9942 0.5461 0.196 Uiso 0.53 1 d PR A 1 C3B' C 0.5829(17) 0.891(2) 0.5251(13) 0.075(11) Uiso 0.47 1 d PD A 2 H3B4 H 0.5312 0.9060 0.5034 0.112 Uiso 0.47 1 d PR A 2 H3B5 H 0.5973 0.9248 0.5627 0.112 Uiso 0.47 1 d PR A 2 H3B6 H 0.5589 0.8190 0.5295 0.112 Uiso 0.47 1 d PR A 2 C4B' C 0.720(2) 1.0403(14) 0.4918(15) 0.098(13) Uiso 0.47 1 d PD A 2 H4B4 H 0.7360 1.0696 0.5306 0.148 Uiso 0.47 1 d PR A 2 H4B5 H 0.6700 1.0602 0.4720 0.148 Uiso 0.47 1 d PR A 2 H4B6 H 0.7811 1.0636 0.4712 0.148 Uiso 0.47 1 d PR A 2 C5B' C 0.757(2) 0.897(3) 0.5245(14) 0.106(14) Uiso 0.47 1 d PD A 2 H5B4 H 0.8132 0.9562 0.5409 0.159 Uiso 0.47 1 d PR A 2 H5B5 H 0.7817 0.8624 0.4974 0.159 Uiso 0.47 1 d PR A 2 H5B6 H 0.7265 0.8523 0.5550 0.159 Uiso 0.47 1 d PR A 2 O2C O 0.3539(8) 0.6599(9) 0.1157(5) 0.074(3) Uani 1 1 d . . . O1C O 0.4687(9) 0.8199(8) 0.1100(4) 0.063(3) Uani 1 1 d . . . C1C C 0.3909(15) 0.7419(16) 0.0910(7) 0.065(5) Uani 1 1 d . . . C2C C 0.3383(13) 0.7531(13) 0.0347(7) 0.070(5) Uani 1 1 d . . . C3C C 0.2519(16) 0.7747(19) 0.0511(9) 0.140(9) Uani 1 1 d . . . H3C1 H 0.2363 0.8156 0.0225 0.210 Uiso 1 1 d R C . H3C2 H 0.2691 0.8105 0.0882 0.210 Uiso 1 1 d R . . H3C3 H 0.1933 0.7120 0.0536 0.210 Uiso 1 1 d R . . C4C C 0.307(2) 0.6600(19) -0.0018(9) 0.191(14) Uani 1 1 d . . . H4C1 H 0.3584 0.6329 0.0029 0.287 Uiso 1 1 d R C . H4C2 H 0.2991 0.6753 -0.0418 0.287 Uiso 1 1 d R . . H4C3 H 0.2429 0.6110 0.0096 0.287 Uiso 1 1 d R . . C5C C 0.4054(16) 0.8400(18) -0.0003(7) 0.137(9) Uani 1 1 d . . . H5C1 H 0.4374 0.9000 0.0245 0.205 Uiso 1 1 d R C . H5C2 H 0.3642 0.8523 -0.0314 0.205 Uiso 1 1 d R . . H5C3 H 0.4573 0.8226 -0.0160 0.205 Uiso 1 1 d R . . O1D O 0.3979(9) 0.4975(8) 0.1627(5) 0.075(3) Uani 1 1 d . . . O2D O 0.5497(9) 0.5001(7) 0.1920(5) 0.059(3) Uani 1 1 d . . . C1D C 0.4673(17) 0.4650(12) 0.1614(7) 0.066(5) Uani 1 1 d . . . C2D C 0.4456(9) 0.3768(10) 0.1178(6) 0.069(5) Uani 1 1 d D B . C3D C 0.523(2) 0.332(3) 0.1324(15) 0.076(14) Uiso 0.42 1 d PD B 1 H3D1 H 0.5914 0.3838 0.1308 0.114 Uiso 0.42 1 d PR B 1 H3D2 H 0.5133 0.2779 0.1050 0.114 Uiso 0.42 1 d PR B 1 H3D3 H 0.5151 0.3068 0.1708 0.114 Uiso 0.42 1 d PR B 1 C4D C 0.462(2) 0.423(2) 0.0595(9) 0.040(10) Uiso 0.42 1 d PD B 1 H4D1 H 0.5258 0.4819 0.0616 0.060 Uiso 0.42 1 d PR B 1 H4D2 H 0.4069 0.4436 0.0482 0.060 Uiso 0.42 1 d PR B 1 H4D3 H 0.4637 0.3747 0.0312 0.060 Uiso 0.42 1 d PR B 1 C5D C 0.3391(16) 0.297(3) 0.1193(18) 0.13(2) Uiso 0.42 1 d PD B 1 H5D1 H 0.3184 0.2598 0.0826 0.198 Uiso 0.42 1 d PR B 1 H5D2 H 0.2931 0.3290 0.1264 0.198 Uiso 0.42 1 d PR B 1 H5D3 H 0.3373 0.2512 0.1496 0.198 Uiso 0.42 1 d PR B 1 C3D' C 0.3325(13) 0.330(2) 0.1007(12) 0.087(11) Uiso 0.58 1 d PD B 2 H3D4 H 0.3125 0.3790 0.0816 0.131 Uiso 0.58 1 d PR B 2 H3D5 H 0.2955 0.3085 0.1348 0.131 Uiso 0.58 1 d PR B 2 H3D6 H 0.3172 0.2723 0.0747 0.131 Uiso 0.58 1 d PR B 2 C4D' C 0.481(2) 0.302(2) 0.1452(13) 0.096(12) Uiso 0.58 1 d PD B 2 H4D4 H 0.4545 0.2398 0.1218 0.144 Uiso 0.58 1 d PR B 2 H4D5 H 0.4575 0.2882 0.1834 0.144 Uiso 0.58 1 d PR B 2 H4D6 H 0.5549 0.3284 0.1479 0.144 Uiso 0.58 1 d PR B 2 C5D' C 0.504(2) 0.424(2) 0.0666(10) 0.092(13) Uiso 0.58 1 d PD B 2 H5D4 H 0.4772 0.4698 0.0492 0.138 Uiso 0.58 1 d PR B 2 H5D5 H 0.4976 0.3717 0.0386 0.138 Uiso 0.58 1 d PR B 2 H5D6 H 0.5749 0.4607 0.0794 0.138 Uiso 0.58 1 d PR B 2 O2A O 1.0304(7) 0.9296(8) 0.2440(4) 0.061(3) Uani 1 1 d . . . O1A O 0.9926(7) 1.0627(7) 0.2271(4) 0.061(3) Uani 1 1 d . . . C1A C 1.0538(13) 1.0208(12) 0.2395(6) 0.052(4) Uani 1 1 d . . . C2A C 1.1666(11) 1.0919(12) 0.2478(7) 0.061(4) Uani 1 1 d . . . C3A C 1.1843(12) 1.2030(11) 0.2429(7) 0.080(5) Uani 1 1 d . . . H3A1 H 1.2562 1.2430 0.2410 0.121 Uiso 1 1 d R C . H3A2 H 1.1606 1.2250 0.2762 0.121 Uiso 1 1 d R . . H3A3 H 1.1474 1.2112 0.2083 0.121 Uiso 1 1 d R . . C4A C 1.2186(11) 1.0600(12) 0.1992(7) 0.080(5) Uani 1 1 d . . . H4A1 H 1.2909 1.1008 0.2029 0.120 Uiso 1 1 d R C . H4A2 H 1.1901 1.0697 0.1620 0.120 Uiso 1 1 d R . . H4A3 H 1.2070 0.9898 0.2025 0.120 Uiso 1 1 d R . . C5A C 1.2128(13) 1.0750(13) 0.3057(8) 0.092(6) Uani 1 1 d . . . H5A1 H 1.1801 1.0923 0.3367 0.139 Uiso 1 1 d R C . H5A2 H 1.2848 1.1171 0.3094 0.139 Uiso 1 1 d R . . H5A3 H 1.2028 1.0050 0.3078 0.139 Uiso 1 1 d R . . N17 N 0.8984(10) 0.7217(10) 0.1824(5) 0.060(4) Uani 1 1 d . . . O27 O 0.7566(7) 0.6688(7) 0.2279(4) 0.059(3) Uani 1 1 d . . . C27 C 0.8067(13) 0.6428(13) 0.1903(7) 0.061(4) Uani 1 1 d . . . C37 C 0.7759(15) 0.5479(14) 0.1636(8) 0.098(7) Uani 1 1 d . . . H37 H 0.7123 0.4969 0.1692 0.117 Uiso 1 1 calc R . . C47 C 0.8402(18) 0.5314(17) 0.1293(10) 0.127(9) Uani 1 1 d . . . H47 H 0.8234 0.4672 0.1124 0.153 Uiso 1 1 calc R C . C57 C 0.932(2) 0.610(2) 0.1190(9) 0.137(10) Uani 1 1 d . . . H57 H 0.9766 0.6003 0.0944 0.165 Uiso 1 1 calc R . . C67 C 0.9560(12) 0.7013(16) 0.1452(8) 0.087(6) Uani 1 1 d . . . Cl7 Cl 1.0684(3) 0.8049(5) 0.1358(2) 0.113(2) Uani 1 1 d . . . N12 N 0.8299(10) 1.0043(9) 0.1171(5) 0.054(3) Uani 1 1 d . . . O22 O 0.6847(7) 0.9407(7) 0.1582(4) 0.055(3) Uani 1 1 d . . . C22 C 0.7265(13) 0.9590(10) 0.1094(7) 0.050(4) Uani 1 1 d . . . C32 C 0.6773(15) 0.9440(13) 0.0553(7) 0.083(6) Uani 1 1 d . . . H32 H 0.6061 0.9131 0.0503 0.100 Uiso 1 1 calc R . . C42 C 0.7349(19) 0.9756(17) 0.0085(8) 0.106(7) Uani 1 1 d . . . H42 H 0.7020 0.9675 -0.0285 0.127 Uiso 1 1 calc R C . C52 C 0.8387(19) 1.0185(15) 0.0149(8) 0.098(7) Uani 1 1 d . . . H52 H 0.8782 1.0392 -0.0168 0.118 Uiso 1 1 calc R . . C62 C 0.8813(12) 1.0294(12) 0.0696(9) 0.072(5) Uani 1 1 d . . . Cl2 Cl 1.0139(4) 1.0892(4) 0.0843(2) 0.117(2) Uani 1 1 d . . . N18 N 0.9299(8) 0.7531(9) 0.3242(5) 0.044(3) Uani 1 1 d . . . O28 O 0.9008(6) 0.8902(7) 0.3433(4) 0.048(3) Uani 1 1 d . . . C28 C 0.9297(10) 0.8248(12) 0.3629(7) 0.048(4) Uani 1 1 d . . . C38 C 0.9655(11) 0.8253(12) 0.4201(7) 0.059(4) Uani 1 1 d . . . H38 H 0.9712 0.8777 0.4459 0.071 Uiso 1 1 calc R . . C48 C 0.9919(12) 0.7499(14) 0.4383(7) 0.071(5) Uani 1 1 d . . . H48 H 1.0140 0.7489 0.4770 0.085 Uiso 1 1 calc R C . C58 C 0.9860(12) 0.6733(14) 0.3989(8) 0.071(5) Uani 1 1 d . . . H58 H 1.0036 0.6201 0.4105 0.085 Uiso 1 1 calc R . . C68 C 0.9541(11) 0.6793(11) 0.3438(7) 0.057(4) Uani 1 1 d . . . Cl8 Cl 0.9477(4) 0.5878(3) 0.2945(2) 0.0946(16) Uani 1 1 d . . . N14 N 0.3846(8) 0.7747(8) 0.3184(6) 0.046(3) Uani 1 1 d . . . O24 O 0.4196(7) 0.7647(7) 0.2274(4) 0.052(3) Uani 1 1 d . . . C24 C 0.3611(11) 0.7804(10) 0.2629(8) 0.049(4) Uani 1 1 d . . . C34 C 0.2759(11) 0.7990(12) 0.2424(8) 0.070(5) Uani 1 1 d . . . H34 H 0.2629 0.8055 0.2030 0.084 Uiso 1 1 calc R . . C44 C 0.2134(12) 0.8074(12) 0.2812(9) 0.078(5) Uani 1 1 d . . . H44 H 0.1546 0.8169 0.2685 0.093 Uiso 1 1 calc R C . C54 C 0.2356(13) 0.8019(12) 0.3397(8) 0.073(5) Uani 1 1 d . . . H54 H 0.1939 0.8091 0.3672 0.088 Uiso 1 1 calc R . . C64 C 0.3203(13) 0.7857(11) 0.3553(7) 0.068(5) Uani 1 1 d . . . Cl4 Cl 0.3461(3) 0.7718(4) 0.42786(19) 0.0863(15) Uani 1 1 d . . . N15 N 0.4516(8) 0.6042(8) 0.3692(5) 0.040(3) Uani 1 1 d . . . O25 O 0.4687(6) 0.6187(6) 0.2762(4) 0.045(2) Uani 1 1 d . . . C25 C 0.4286(11) 0.5533(13) 0.3179(8) 0.055(4) Uani 1 1 d . . . C35 C 0.3776(11) 0.4523(11) 0.3104(7) 0.060(4) Uani 1 1 d . . . H35 H 0.3621 0.4208 0.2736 0.072 Uiso 1 1 calc R . . C45 C 0.3497(14) 0.3984(13) 0.3584(8) 0.081(5) Uani 1 1 d . . . H45 H 0.3137 0.3284 0.3548 0.097 Uiso 1 1 calc R C . C55 C 0.3738(11) 0.4456(13) 0.4123(8) 0.065(5) Uani 1 1 d . . . H55 H 0.3564 0.4087 0.4457 0.078 Uiso 1 1 calc R . . C65 C 0.4243(11) 0.5484(12) 0.4155(6) 0.051(4) Uani 1 1 d . . . Cl5 Cl 0.4560(3) 0.6092(3) 0.48200(17) 0.0763(13) Uani 1 1 d . . . N11 N 0.8139(9) 1.1357(9) 0.2333(5) 0.053(3) Uani 1 1 d . . . O21 O 0.8351(7) 1.0461(7) 0.3053(4) 0.052(3) Uani 1 1 d . . . C21 C 0.8255(10) 1.1265(11) 0.2906(7) 0.049(4) Uani 1 1 d . . . C31 C 0.8277(12) 1.2033(13) 0.3299(8) 0.072(5) Uani 1 1 d . . . H31 H 0.8383 1.1995 0.3698 0.087 Uiso 1 1 calc R . . C41 C 0.8137(13) 1.2826(13) 0.3060(9) 0.071(5) Uani 1 1 d . . . H41 H 0.8148 1.3345 0.3308 0.085 Uiso 1 1 calc R C . C51 C 0.7987(14) 1.2911(13) 0.2505(10) 0.089(6) Uani 1 1 d . . . H51 H 0.7876 1.3467 0.2365 0.107 Uiso 1 1 calc R . . C61 C 0.7994(13) 1.2166(13) 0.2127(6) 0.067(5) Uani 1 1 d . . . Cl1 Cl 0.7808(6) 1.2166(4) 0.1400(2) 0.142(3) Uani 1 1 d . . . N13 N 0.5472(9) 0.9710(8) 0.2314(5) 0.048(3) Uani 1 1 d . . . O23 O 0.6103(6) 0.8856(6) 0.2898(4) 0.040(2) Uani 1 1 d . . . C23 C 0.5821(10) 0.9627(10) 0.2852(7) 0.038(4) Uani 1 1 d . . . C33 C 0.5826(12) 1.0261(11) 0.3299(7) 0.063(5) Uani 1 1 d . . . H33 H 0.6047 1.0181 0.3676 0.076 Uiso 1 1 calc R . . C43 C 0.5496(12) 1.1020(12) 0.3176(8) 0.070(5) Uani 1 1 d . . . H43 H 0.5510 1.1470 0.3473 0.084 Uiso 1 1 calc R C . C53 C 0.5156(12) 1.1123(12) 0.2638(8) 0.065(5) Uani 1 1 d . . . H53 H 0.4923 1.1629 0.2552 0.078 Uiso 1 1 calc R . . C63 C 0.5165(10) 1.0451(12) 0.2221(7) 0.053(4) Uani 1 1 d . . . Cl3 Cl 0.4734(4) 1.0525(4) 0.1519(2) 0.0976(17) Uani 1 1 d . . . N16 N 0.6473(7) 0.5761(8) 0.3223(4) 0.039(3) Uani 1 1 d D . . O26 O 0.6660(6) 0.7362(6) 0.3240(3) 0.039(2) Uani 1 1 d D . . C26 C 0.6775(10) 0.6642(11) 0.3513(6) 0.039(4) Uani 1 1 d D . . C36 C 0.7208(10) 0.6764(9) 0.4081(6) 0.045(4) Uani 1 1 d D . . H36 H 0.7414 0.7386 0.4283 0.054 Uiso 1 1 calc R . . C46 C 0.7326(11) 0.5969(12) 0.4337(6) 0.056(4) Uani 1 1 d D . . H46 H 0.7607 0.6030 0.4718 0.067 Uiso 1 1 calc R C . C56 C 0.7014(11) 0.5059(12) 0.4015(7) 0.058(4) Uani 1 1 d D . . H56 H 0.7108 0.4506 0.4173 0.069 Uiso 1 1 calc R . . C66 C 0.6584(10) 0.4985(10) 0.3480(6) 0.044(4) Uani 1 1 d D . . Cl6 Cl 0.6169(3) 0.3897(3) 0.30670(19) 0.0768(13) Uani 1 1 d D . . N19 N 0.1746(16) 0.4928(17) 0.1400(8) 0.150(11) Uiso 0.69 1 d PD C 1 H19 H 0.2223 0.5353 0.1210 0.180 Uiso 0.69 1 calc PR C 1 O29 O 0.2608(10) 0.5574(10) 0.2224(5) 0.100(4) Uiso 0.69 1 d PD C 1 C29 C 0.1785(18) 0.495(2) 0.1973(9) 0.140(13) Uiso 0.69 1 d PD C 1 C39 C 0.104(2) 0.428(2) 0.2300(10) 0.161(15) Uiso 0.69 1 d PD C 1 H39 H 0.1049 0.4387 0.2699 0.193 Uiso 0.69 1 calc PR C 1 C49 C 0.030(3) 0.347(2) 0.2015(12) 0.23(2) Uiso 0.69 1 d PD C 1 H49 H -0.0191 0.2967 0.2211 0.281 Uiso 0.69 1 calc PR C 1 C59 C 0.032(3) 0.341(2) 0.1414(12) 0.25(2) Uiso 0.69 1 d PD C 1 H59 H -0.0099 0.2813 0.1207 0.297 Uiso 0.69 1 calc PR C 1 C69 C 0.092(2) 0.420(2) 0.1137(9) 0.144(13) Uiso 0.69 1 d PD C 1 Cl69 Cl 0.0790(13) 0.4277(13) 0.0416(7) 0.290(8) Uiso 0.69 1 d PD C 1 N1S N 0.2608(10) 0.5574(10) 0.2224(5) 0.100(4) Uiso 0.31 1 d PD C 2 C2S C 0.195(3) 0.505(3) 0.252(2) 0.080(17) Uiso 0.31 1 d PD C 2 C3S C 0.108(3) 0.434(3) 0.281(2) 0.080(17) Uiso 0.31 1 d PD C 2 H3S1 H 0.0503 0.4517 0.2744 0.120 Uiso 0.31 1 d PR C 2 H3S2 H 0.1269 0.4364 0.3214 0.120 Uiso 0.31 1 d PR C 2 H3S3 H 0.0906 0.3663 0.2648 0.120 Uiso 0.31 1 d PR C 2 N1X N 0.138(3) 0.510(3) 0.4184(14) 0.144(14) Uiso 0.50 1 d PD D 1 C2X C 0.146(2) 0.542(2) 0.4669(14) 0.064(9) Uiso 0.50 1 d PD D 1 C3X C 0.145(4) 0.603(4) 0.5185(19) 0.15(2) Uiso 0.50 1 d PD D 1 H3X1 H 0.1860 0.5920 0.5504 0.227 Uiso 0.50 1 d PR D 1 H3X2 H 0.0757 0.5820 0.5288 0.227 Uiso 0.50 1 d PR D 1 H3X3 H 0.1720 0.6736 0.5101 0.227 Uiso 0.50 1 d PR D 1 N1X' N 0.113(5) 0.617(4) 0.541(2) 0.09(2) Uiso 0.25 1 d PD E 2 C2X' C 0.117(4) 0.563(4) 0.502(2) 0.030(13) Uiso 0.25 1 d PD E 2 C3X' C 0.085(5) 0.485(5) 0.454(3) 0.09(2) Uiso 0.25 1 d PD E 2 H3X4 H 0.1411 0.4931 0.4308 0.141 Uiso 0.25 1 d PR E 2 H3X5 H 0.0315 0.4939 0.4304 0.141 Uiso 0.25 1 d PR E 2 H3X6 H 0.0596 0.4187 0.4695 0.141 Uiso 0.25 1 d PR E 2 N1Y N 0.6645(14) 0.7027(14) 0.0845(7) 0.119(7) Uani 1 1 d D . . C2Y C 0.7417(13) 0.7308(14) 0.0615(8) 0.095(7) Uani 1 1 d D . . C3Y C 0.8355(14) 0.767(2) 0.0314(10) 0.168(12) Uani 1 1 d D . . H3Y1 H 0.8913 0.8117 0.0571 0.252 Uiso 1 1 d R . . H3Y2 H 0.8271 0.8033 -0.0020 0.252 Uiso 1 1 d R . . H3Y3 H 0.8500 0.7105 0.0191 0.252 Uiso 1 1 d R . . N1Z N 0.1283(16) 0.2867(13) 0.4241(11) 0.171(10) Uani 1 1 d D . . C2Z C 0.0749(14) 0.2008(13) 0.4152(8) 0.091(6) Uani 1 1 d D . . C3Z C 0.0066(13) 0.0941(12) 0.4061(8) 0.098(6) Uani 1 1 d D . . H3Z1 H 0.0449 0.0529 0.4132 0.147 Uiso 1 1 d R . . H3Z2 H -0.0233 0.0819 0.3669 0.147 Uiso 1 1 d R . . H3Z3 H -0.0466 0.0772 0.4325 0.147 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co4 0.0544(13) 0.0512(13) 0.0440(13) 0.0097(10) 0.0099(10) 0.0294(11) Co5 0.0593(14) 0.0582(14) 0.0543(14) 0.0054(11) -0.0027(11) 0.0252(12) Co6 0.0519(13) 0.0441(12) 0.0448(12) 0.0069(10) 0.0112(10) 0.0236(10) Co7 0.0473(13) 0.0504(13) 0.0472(13) 0.0107(10) 0.0140(10) 0.0281(11) Co3 0.0504(13) 0.0490(13) 0.0507(13) 0.0163(10) 0.0166(10) 0.0250(11) Co2 0.0433(12) 0.0452(12) 0.0469(12) 0.0074(10) 0.0112(10) 0.0222(10) Co1 0.0385(12) 0.0411(11) 0.0431(12) 0.0095(9) 0.0105(9) 0.0208(10) O2 0.058(6) 0.044(6) 0.049(6) 0.006(5) 0.018(5) 0.023(5) O1 0.038(5) 0.039(5) 0.040(5) 0.005(4) 0.007(4) 0.019(5) O1B 0.034(6) 0.058(6) 0.053(6) 0.003(5) 0.018(5) 0.017(5) O2B 0.046(7) 0.066(7) 0.038(6) -0.001(5) 0.009(5) 0.021(6) C1B 0.055(11) 0.042(9) 0.043(10) 0.006(8) 0.016(9) 0.033(9) C2B 0.065(11) 0.062(11) 0.059(11) -0.003(9) 0.033(9) 0.022(9) O2C 0.072(8) 0.068(8) 0.076(8) 0.008(7) -0.022(6) 0.024(7) O1C 0.076(8) 0.070(8) 0.052(7) 0.004(6) -0.003(6) 0.039(7) C1C 0.072(14) 0.087(15) 0.054(13) -0.023(11) -0.024(11) 0.057(13) C2C 0.066(12) 0.086(14) 0.066(13) -0.007(11) 0.000(11) 0.038(11) C3C 0.120(19) 0.23(3) 0.110(18) 0.046(18) 0.008(15) 0.12(2) C4C 0.38(4) 0.17(3) 0.065(16) -0.035(17) -0.04(2) 0.16(3) C5C 0.116(18) 0.22(3) 0.046(13) 0.047(15) -0.008(12) 0.040(18) O1D 0.097(10) 0.066(8) 0.065(8) -0.015(6) -0.010(7) 0.036(7) O2D 0.067(8) 0.041(7) 0.064(8) -0.011(6) 0.000(6) 0.018(6) C1D 0.094(17) 0.034(11) 0.048(12) 0.002(9) 0.018(12) 0.002(11) C2D 0.068(12) 0.061(11) 0.061(11) -0.008(9) 0.001(9) 0.009(9) O2A 0.046(7) 0.049(7) 0.089(8) 0.009(6) 0.027(6) 0.016(6) O1A 0.046(7) 0.059(7) 0.073(8) 0.004(6) 0.009(6) 0.014(6) C1A 0.064(12) 0.052(11) 0.046(10) 0.012(8) 0.029(9) 0.025(11) C2A 0.046(11) 0.073(12) 0.065(12) 0.016(9) 0.019(9) 0.023(10) C3A 0.078(13) 0.045(11) 0.102(14) -0.010(10) 0.019(11) 0.006(9) C4A 0.051(11) 0.075(12) 0.106(15) 0.012(11) 0.022(10) 0.015(10) C5A 0.076(13) 0.094(14) 0.110(16) 0.016(12) -0.006(12) 0.038(12) N17 0.054(9) 0.091(10) 0.047(8) 0.004(7) 0.016(7) 0.039(9) O27 0.052(7) 0.066(7) 0.076(7) 0.006(6) 0.023(6) 0.037(6) C27 0.064(12) 0.081(13) 0.058(11) -0.005(10) 0.012(10) 0.048(11) C37 0.102(16) 0.088(15) 0.120(17) -0.034(13) 0.020(13) 0.055(13) C47 0.101(18) 0.102(18) 0.18(2) -0.047(16) 0.048(18) 0.036(15) C57 0.13(2) 0.20(3) 0.101(18) -0.061(19) 0.031(16) 0.09(2) C67 0.058(12) 0.122(17) 0.080(14) -0.027(12) 0.023(11) 0.033(12) Cl7 0.062(3) 0.177(5) 0.084(4) -0.027(3) 0.029(3) 0.028(3) N12 0.060(9) 0.056(8) 0.053(9) 0.025(7) 0.031(8) 0.025(7) O22 0.062(7) 0.061(7) 0.050(7) 0.020(5) 0.018(6) 0.030(6) C22 0.068(13) 0.045(10) 0.045(12) 0.017(8) 0.023(10) 0.028(9) C32 0.104(15) 0.107(15) 0.042(12) 0.018(11) 0.016(12) 0.044(12) C42 0.12(2) 0.16(2) 0.066(15) 0.025(14) 0.029(15) 0.081(18) C52 0.13(2) 0.131(18) 0.043(14) 0.027(12) 0.046(14) 0.059(17) C62 0.063(12) 0.086(13) 0.076(14) 0.017(11) 0.047(12) 0.031(10) Cl2 0.089(4) 0.163(5) 0.092(4) 0.035(4) 0.051(3) 0.036(4) N18 0.040(7) 0.059(8) 0.046(8) 0.016(7) 0.000(6) 0.034(7) O28 0.043(6) 0.062(7) 0.047(6) 0.020(5) 0.003(5) 0.029(6) C28 0.033(9) 0.059(11) 0.052(12) 0.013(9) 0.017(8) 0.016(8) C38 0.058(11) 0.076(12) 0.055(12) 0.010(9) -0.003(9) 0.041(10) C48 0.074(13) 0.094(14) 0.051(12) 0.021(11) 0.013(10) 0.037(12) C58 0.068(12) 0.100(15) 0.066(13) 0.027(12) 0.009(10) 0.055(11) C68 0.046(10) 0.053(11) 0.069(13) 0.004(9) 0.007(9) 0.017(9) Cl8 0.136(5) 0.082(3) 0.096(4) 0.011(3) 0.017(3) 0.073(3) N14 0.038(7) 0.052(8) 0.054(9) 0.008(6) 0.021(7) 0.023(6) O24 0.037(6) 0.058(7) 0.059(7) 0.007(5) 0.010(5) 0.014(5) C24 0.040(10) 0.039(9) 0.063(12) 0.011(8) 0.013(9) 0.008(8) C34 0.045(11) 0.091(13) 0.092(13) 0.011(10) 0.015(10) 0.045(10) C44 0.050(11) 0.095(14) 0.112(17) 0.025(12) 0.013(12) 0.052(11) C54 0.062(13) 0.095(14) 0.069(14) 0.000(11) 0.008(10) 0.039(11) C64 0.058(12) 0.061(11) 0.093(14) 0.020(10) 0.008(11) 0.030(10) Cl4 0.074(3) 0.124(4) 0.068(3) 0.013(3) 0.022(3) 0.046(3) N15 0.036(7) 0.048(7) 0.037(8) 0.008(7) 0.007(6) 0.018(6) O25 0.044(6) 0.043(6) 0.047(6) 0.007(5) 0.008(5) 0.016(5) C25 0.036(10) 0.072(13) 0.066(13) 0.009(11) -0.002(9) 0.030(10) C35 0.065(11) 0.037(10) 0.061(12) -0.006(9) -0.005(9) 0.006(9) C45 0.101(15) 0.062(12) 0.070(14) 0.016(12) 0.023(12) 0.019(11) C55 0.059(11) 0.064(13) 0.067(13) 0.029(10) 0.015(10) 0.015(10) C65 0.052(10) 0.065(12) 0.038(10) 0.000(9) -0.010(8) 0.026(9) Cl5 0.100(4) 0.078(3) 0.051(3) 0.016(2) 0.016(2) 0.034(3) N11 0.057(8) 0.064(9) 0.044(9) 0.008(7) 0.005(7) 0.029(7) O21 0.049(6) 0.044(6) 0.064(7) 0.015(5) 0.004(5) 0.021(5) C21 0.048(10) 0.034(10) 0.068(12) 0.011(9) 0.012(9) 0.018(8) C31 0.069(12) 0.070(12) 0.091(14) 0.003(12) 0.015(10) 0.040(11) C41 0.080(13) 0.067(13) 0.069(14) -0.008(11) 0.012(11) 0.032(11) C51 0.110(16) 0.063(13) 0.122(19) 0.007(13) 0.013(15) 0.063(12) C61 0.092(14) 0.076(13) 0.044(10) 0.017(10) -0.004(9) 0.046(11) Cl1 0.268(8) 0.121(5) 0.077(4) 0.012(3) -0.026(4) 0.127(5) N13 0.056(8) 0.037(8) 0.061(9) 0.012(6) 0.009(7) 0.027(7) O23 0.039(6) 0.039(6) 0.054(6) 0.006(5) 0.005(5) 0.028(5) C23 0.031(8) 0.032(9) 0.056(11) 0.005(8) 0.016(8) 0.015(7) C33 0.092(13) 0.063(11) 0.053(11) 0.014(9) 0.019(9) 0.049(11) C43 0.077(13) 0.057(12) 0.091(15) 0.006(10) 0.021(11) 0.039(10) C53 0.069(12) 0.055(11) 0.082(14) 0.006(11) -0.001(11) 0.036(10) C63 0.049(10) 0.057(10) 0.070(12) 0.021(9) 0.029(9) 0.033(9) Cl3 0.156(5) 0.099(4) 0.071(3) 0.020(3) -0.004(3) 0.088(4) N16 0.033(7) 0.040(8) 0.051(8) 0.002(7) 0.005(6) 0.021(6) O26 0.033(5) 0.045(6) 0.046(6) 0.012(5) 0.013(4) 0.021(5) C26 0.042(9) 0.043(10) 0.041(10) 0.021(8) 0.017(8) 0.026(8) C36 0.049(10) 0.027(9) 0.055(11) 0.013(8) 0.011(8) 0.011(7) C46 0.073(12) 0.071(12) 0.032(9) 0.011(9) 0.011(8) 0.036(10) C56 0.060(11) 0.063(12) 0.062(12) 0.022(10) 0.016(9) 0.036(9) C66 0.046(10) 0.042(10) 0.055(11) 0.014(8) -0.002(8) 0.029(8) Cl6 0.105(4) 0.050(3) 0.087(3) 0.003(2) 0.003(3) 0.044(3) N1Y 0.158(19) 0.133(16) 0.098(14) 0.019(12) 0.045(13) 0.085(15) C2Y 0.14(2) 0.104(17) 0.059(14) -0.003(12) 0.005(13) 0.070(17) C3Y 0.100(19) 0.24(3) 0.16(2) 0.08(2) 0.056(18) 0.06(2) N1Z 0.15(2) 0.128(19) 0.20(2) 0.013(18) 0.063(18) 0.011(16) C2Z 0.097(18) 0.114(18) 0.075(14) 0.013(15) 0.017(13) 0.054(15) C3Z 0.095(15) 0.082(14) 0.099(15) 0.012(12) -0.001(12) 0.017(12) _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 Co4 O1C 2.015(11) . ? Co4 O22 2.027(9) . ? Co4 O2 2.047(8) . ? Co4 N13 2.060(11) . ? Co4 O24 2.089(9) . ? Co5 O1D 2.008(11) . ? Co5 O24 2.028(9) . ? Co5 O2C 2.043(11) . ? Co5 O29 2.107(13) . ? Co5 O25 2.103(9) . ? Co5 O2 2.188(9) . ? Co6 O2D 2.022(10) . ? Co6 O27 2.038(9) . ? Co6 O2 2.061(9) . ? Co6 N16 2.117(10) . ? Co6 O25 2.158(8) . ? Co6 O26 2.339(8) . ? Co7 O2A 1.992(10) . ? Co7 O1 2.000(8) . ? Co7 N17 2.061(12) . ? Co7 N18 2.081(11) . ? Co7 O27 2.299(10) . ? Co3 O1A 1.998(10) . ? Co3 O1 1.992(8) . ? Co3 N12 2.091(11) . ? Co3 N11 2.101(12) . ? Co3 O22 2.310(10) . ? Co3 O21 2.362(9) . ? Co2 O2B 2.002(9) . ? Co2 O23 2.153(8) . ? Co2 N14 2.156(11) . ? Co2 N15 2.196(11) . ? Co2 O26 2.205(8) . ? Co2 O25 2.262(9) . ? Co1 O1B 2.018(9) . ? Co1 O21 2.078(9) . ? Co1 O1 2.096(8) . ? Co1 O28 2.112(9) . ? Co1 O23 2.157(8) . ? Co1 O26 2.156(8) . ? O1B C1B 1.240(15) . ? O2B C1B 1.284(16) . ? C1B C2B 1.517(19) . ? C2B C5B' 1.503(14) . ? C2B C3B' 1.503(14) . ? C2B C3B 1.506(14) . ? C2B C5B 1.508(14) . ? C2B C4B' 1.513(14) . ? C2B C4B 1.518(14) . ? O2C C1C 1.26(2) . ? O1C C1C 1.285(19) . ? C1C C2C 1.51(2) . ? C2C C3C 1.47(2) . ? C2C C4C 1.48(2) . ? C2C C5C 1.53(2) . ? O1D C1D 1.26(2) . ? O2D C1D 1.26(2) . ? C1D C2D 1.55(2) . ? C2D C4D' 1.509(13) . ? C2D C5D' 1.514(13) . ? C2D C5D 1.515(13) . ? C2D C4D 1.516(13) . ? C2D C3D' 1.519(13) . ? C2D C3D 1.523(13) . ? O2A C1A 1.237(16) . ? O1A C1A 1.275(16) . ? C1A C2A 1.54(2) . ? C2A C5A 1.53(2) . ? C2A C3A 1.537(19) . ? C2A C4A 1.562(19) . ? N17 C67 1.349(18) . ? N17 C27 1.388(18) . ? O27 C27 1.313(16) . ? C27 C37 1.39(2) . ? C37 C47 1.35(2) . ? C47 C57 1.40(3) . ? C57 C67 1.35(3) . ? C67 Cl7 1.745(18) . ? N12 C62 1.346(18) . ? N12 C22 1.367(17) . ? O22 C22 1.303(15) . ? C22 C32 1.38(2) . ? C32 C42 1.39(2) . ? C42 C52 1.37(2) . ? C52 C62 1.36(2) . ? C62 Cl2 1.764(17) . ? N18 C68 1.328(17) . ? N18 C28 1.373(17) . ? O28 C28 1.257(16) . ? C28 C38 1.397(19) . ? C38 C48 1.356(19) . ? C48 C58 1.41(2) . ? C58 C68 1.35(2) . ? C68 Cl8 1.719(16) . ? N14 C24 1.329(17) . ? N14 C64 1.358(18) . ? O24 C24 1.299(16) . ? C24 C34 1.412(19) . ? C34 C44 1.35(2) . ? C44 C54 1.39(2) . ? C54 C64 1.36(2) . ? C64 Cl4 1.740(17) . ? N15 C65 1.339(16) . ? N15 C25 1.350(17) . ? O25 C25 1.354(16) . ? C25 C35 1.357(19) . ? C35 C45 1.360(19) . ? C45 C55 1.38(2) . ? C55 C65 1.375(19) . ? C65 Cl5 1.719(14) . ? N11 C21 1.350(17) . ? N11 C61 1.358(18) . ? O21 C21 1.276(15) . ? C21 C31 1.43(2) . ? C31 C41 1.36(2) . ? C41 C51 1.31(2) . ? C51 C61 1.39(2) . ? C61 Cl1 1.697(15) . ? N13 C63 1.329(16) . ? N13 C23 1.345(16) . ? O23 C23 1.336(14) . ? C23 C33 1.383(18) . ? C33 C43 1.387(19) . ? C43 C53 1.35(2) . ? C53 C63 1.375(19) . ? C63 Cl3 1.733(16) . ? N16 C26 1.336(15) . ? N16 C66 1.338(14) . ? O26 C26 1.289(13) . ? C26 C36 1.404(17) . ? C36 C46 1.368(16) . ? C46 C56 1.407(18) . ? C56 C66 1.340(17) . ? C66 Cl6 1.710(14) . ? N19 C29 1.333(16) . ? N19 C69 1.348(16) . ? O29 C29 1.269(15) . ? C29 C39 1.407(18) . ? C39 C49 1.363(19) . ? C49 C59 1.40(2) . ? C59 C69 1.332(19) . ? C69 Cl69 1.690(16) . ? C2S C3S 1.481(10) . ? N1X C2X 1.200(10) . ? C2X C3X 1.489(10) . ? N1X' C2X' 1.212(10) . ? C2X' C3X' 1.489(10) . ? N1Y C2Y 1.188(9) . ? C2Y C3Y 1.472(9) . ? N1Z C2Z 1.184(9) . ? C2Z C3Z 1.472(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 O1C Co4 O22 97.2(4) . . ? O1C Co4 O2 95.3(4) . . ? O22 Co4 O2 99.5(3) . . ? O1C Co4 N13 113.3(5) . . ? O22 Co4 N13 88.6(4) . . ? O2 Co4 N13 149.1(4) . . ? O1C Co4 O24 90.4(4) . . ? O22 Co4 O24 171.8(4) . . ? O2 Co4 O24 82.7(3) . . ? N13 Co4 O24 85.6(4) . . ? O1D Co5 O24 178.0(4) . . ? O1D Co5 O2C 90.7(5) . . ? O24 Co5 O2C 91.2(4) . . ? O1D Co5 O29 88.9(5) . . ? O24 Co5 O29 91.6(4) . . ? O2C Co5 O29 93.5(5) . . ? O1D Co5 O25 95.6(4) . . ? O24 Co5 O25 82.5(3) . . ? O2C Co5 O25 173.3(4) . . ? O29 Co5 O25 89.0(4) . . ? O1D Co5 O2 98.4(4) . . ? O24 Co5 O2 80.7(3) . . ? O2C Co5 O2 99.0(4) . . ? O29 Co5 O2 165.4(4) . . ? O25 Co5 O2 77.7(3) . . ? O2D Co6 O27 98.2(4) . . ? O2D Co6 O2 96.6(4) . . ? O27 Co6 O2 99.8(4) . . ? O2D Co6 N16 103.5(4) . . ? O27 Co6 N16 85.6(4) . . ? O2 Co6 N16 158.3(4) . . ? O2D Co6 O25 98.4(4) . . ? O27 Co6 O25 163.4(4) . . ? O2 Co6 O25 79.3(3) . . ? N16 Co6 O25 89.5(4) . . ? O2D Co6 O26 162.5(4) . . ? O27 Co6 O26 86.5(3) . . ? O2 Co6 O26 99.3(3) . . ? N16 Co6 O26 59.8(4) . . ? O25 Co6 O26 77.4(3) . . ? O2A Co7 O1 105.3(4) . . ? O2A Co7 N17 101.0(5) . . ? O1 Co7 N17 114.1(4) . . ? O2A Co7 N18 99.4(4) . . ? O1 Co7 N18 126.8(4) . . ? N17 Co7 N18 106.1(5) . . ? O2A Co7 O27 161.7(4) . . ? O1 Co7 O27 81.2(3) . . ? N17 Co7 O27 61.0(4) . . ? N18 Co7 O27 89.6(4) . . ? O1A Co3 O1 102.3(4) . . ? O1A Co3 N12 103.9(5) . . ? O1 Co3 N12 110.1(4) . . ? O1A Co3 N11 100.8(4) . . ? O1 Co3 N11 129.3(4) . . ? N12 Co3 N11 107.1(5) . . ? O1A Co3 O22 163.0(4) . . ? O1 Co3 O22 79.6(3) . . ? N12 Co3 O22 60.1(4) . . ? N11 Co3 O22 90.5(4) . . ? O1A Co3 O21 84.4(4) . . ? O1 Co3 O21 79.1(3) . . ? N12 Co3 O21 165.4(4) . . ? N11 Co3 O21 59.1(4) . . ? O22 Co3 O21 112.5(3) . . ? O2B Co2 O23 93.1(4) . . ? O2B Co2 N14 103.3(4) . . ? O23 Co2 N14 93.0(4) . . ? O2B Co2 N15 96.8(4) . . ? O23 Co2 N15 165.6(4) . . ? N14 Co2 N15 94.8(4) . . ? O2B Co2 O26 93.3(3) . . ? O23 Co2 O26 76.7(3) . . ? N14 Co2 O26 161.0(4) . . ? N15 Co2 O26 92.4(3) . . ? O2B Co2 O25 153.6(4) . . ? O23 Co2 O25 108.7(3) . . ? N14 Co2 O25 90.6(4) . . ? N15 Co2 O25 59.2(4) . . ? O26 Co2 O25 78.1(3) . . ? O1B Co1 O21 93.3(4) . . ? O1B Co1 O1 173.5(4) . . ? O21 Co1 O1 83.8(3) . . ? O1B Co1 O28 91.2(3) . . ? O21 Co1 O28 87.7(4) . . ? O1 Co1 O28 83.0(3) . . ? O1B Co1 O23 94.5(3) . . ? O21 Co1 O23 95.8(3) . . ? O1 Co1 O23 91.6(3) . . ? O28 Co1 O23 173.2(3) . . ? O1B Co1 O26 93.1(3) . . ? O21 Co1 O26 171.2(3) . . ? O1 Co1 O26 90.5(3) . . ? O28 Co1 O26 98.2(3) . . ? O23 Co1 O26 77.6(3) . . ? Co4 O2 Co6 140.7(5) . . ? Co4 O2 Co5 91.4(3) . . ? Co6 O2 Co5 92.4(3) . . ? Co3 O1 Co7 115.8(4) . . ? Co3 O1 Co1 103.2(3) . . ? Co7 O1 Co1 103.5(4) . . ? C1B O1B Co1 131.0(9) . . ? C1B O2B Co2 131.4(8) . . ? O1B C1B O2B 125.4(13) . . ? O1B C1B C2B 118.0(14) . . ? O2B C1B C2B 116.5(12) . . ? C5B' C2B C3B' 110.9(12) . . ? C5B' C2B C3B 62.8(14) . . ? C3B' C2B C3B 130(2) . . ? C5B' C2B C5B 139(2) . . ? C3B' C2B C5B 39.3(13) . . ? C3B C2B C5B 110.2(12) . . ? C5B' C2B C4B' 109.3(12) . . ? C3B' C2B C4B' 109.1(11) . . ? C3B C2B C4B' 46.6(13) . . ? C5B C2B C4B' 72.8(14) . . ? C5B' C2B C4B 48.2(13) . . ? C3B' C2B C4B 69.4(13) . . ? C3B C2B C4B 107.7(12) . . ? C5B C2B C4B 108.0(12) . . ? C4B' C2B C4B 147(2) . . ? C5B' C2B C1B 107.3(17) . . ? C3B' C2B C1B 115.3(17) . . ? C3B C2B C1B 113.8(15) . . ? C5B C2B C1B 111.8(19) . . ? C4B' C2B C1B 104.6(17) . . ? C4B C2B C1B 105.0(17) . . ? C1C O2C Co5 125.0(11) . . ? C1C O1C Co4 130.5(11) . . ? O2C C1C O1C 126.0(16) . . ? O2C C1C C2C 118.3(17) . . ? O1C C1C C2C 115.7(18) . . ? C3C C2C C4C 112.9(19) . . ? C3C C2C C1C 105.1(14) . . ? C4C C2C C1C 109.9(16) . . ? C3C C2C C5C 108.5(17) . . ? C4C C2C C5C 107.2(17) . . ? C1C C2C C5C 113.4(16) . . ? C1D O1D Co5 128.6(11) . . ? C1D O2D Co6 128.9(11) . . ? O2D C1D O1D 124.7(16) . . ? O2D C1D C2D 120.1(18) . . ? O1D C1D C2D 115.2(18) . . ? C4D' C2D C5D' 112.3(11) . . ? C4D' C2D C5D 86.6(18) . . ? C5D' C2D C5D 129(2) . . ? C4D' C2D C4D 131(2) . . ? C5D' C2D C4D 23.3(15) . . ? C5D C2D C4D 111.1(12) . . ? C4D' C2D C3D' 111.4(11) . . ? C5D' C2D C3D' 110.4(11) . . ? C5D C2D C3D' 25.8(16) . . ? C4D C2D C3D' 88.7(16) . . ? C4D' C2D C3D 26.1(15) . . ? C5D' C2D C3D 88.4(16) . . ? C5D C2D C3D 110.4(12) . . ? C4D C2D C3D 110.0(12) . . ? C3D' C2D C3D 133(2) . . ? C4D' C2D C1D 108.9(17) . . ? C5D' C2D C1D 105.1(16) . . ? C5D C2D C1D 112(2) . . ? C4D C2D C1D 105.5(16) . . ? C3D' C2D C1D 108.4(17) . . ? C3D C2D C1D 107(2) . . ? C1A O2A Co7 132.0(10) . . ? C1A O1A Co3 134.2(10) . . ? O2A C1A O1A 125.9(15) . . ? O2A C1A C2A 118.4(15) . . ? O1A C1A C2A 115.7(14) . . ? C5A C2A C1A 110.2(13) . . ? C5A C2A C3A 110.5(14) . . ? C1A C2A C3A 112.8(13) . . ? C5A C2A C4A 108.0(13) . . ? C1A C2A C4A 105.3(13) . . ? C3A C2A C4A 109.8(12) . . ? C67 N17 C27 115.0(14) . . ? C67 N17 Co7 145.5(13) . . ? C27 N17 Co7 97.8(9) . . ? C27 O27 Co6 135.7(10) . . ? C27 O27 Co7 89.4(9) . . ? Co6 O27 Co7 132.2(4) . . ? O27 C27 N17 110.8(14) . . ? O27 C27 C37 125.5(17) . . ? N17 C27 C37 123.7(15) . . ? C47 C37 C27 117.9(19) . . ? C37 C47 C57 120(2) . . ? C67 C57 C47 118.9(19) . . ? C57 C67 N17 124.5(18) . . ? C57 C67 Cl7 123.0(17) . . ? N17 C67 Cl7 112.4(15) . . ? C62 N12 C22 117.2(14) . . ? C62 N12 Co3 144.7(13) . . ? C22 N12 Co3 98.0(9) . . ? C22 O22 Co4 137.3(10) . . ? C22 O22 Co3 89.9(9) . . ? Co4 O22 Co3 129.7(4) . . ? O22 C22 N12 112.0(14) . . ? O22 C22 C32 126.8(16) . . ? N12 C22 C32 121.1(14) . . ? C22 C32 C42 118.5(19) . . ? C52 C42 C32 122(2) . . ? C62 C52 C42 116.2(17) . . ? N12 C62 C52 125.3(17) . . ? N12 C62 Cl2 113.6(15) . . ? C52 C62 Cl2 120.9(15) . . ? C68 N18 C28 118.3(13) . . ? C68 N18 Co7 143.3(11) . . ? C28 N18 Co7 98.3(9) . . ? C28 O28 Co1 134.8(9) . . ? O28 C28 N18 116.4(14) . . ? O28 C28 C38 123.6(15) . . ? N18 C28 C38 119.9(15) . . ? C48 C38 C28 119.8(16) . . ? C38 C48 C58 119.8(16) . . ? C68 C58 C48 117.3(16) . . ? N18 C68 C58 124.5(15) . . ? N18 C68 Cl8 117.0(13) . . ? C58 C68 Cl8 118.5(14) . . ? C24 N14 C64 116.1(13) . . ? C24 N14 Co2 114.3(9) . . ? C64 N14 Co2 129.5(11) . . ? C24 O24 Co5 127.2(8) . . ? C24 O24 Co4 137.9(9) . . ? Co5 O24 Co4 94.9(4) . . ? O24 C24 N14 116.2(14) . . ? O24 C24 C34 120.9(15) . . ? N14 C24 C34 122.9(15) . . ? C44 C34 C24 118.3(16) . . ? C34 C44 C54 120.4(16) . . ? C64 C54 C44 117.1(16) . . ? N14 C64 C54 125.2(16) . . ? N14 C64 Cl4 116.7(13) . . ? C54 C64 Cl4 118.0(14) . . ? C65 N15 C25 116.0(13) . . ? C65 N15 Co2 146.6(11) . . ? C25 N15 Co2 97.3(9) . . ? C25 O25 Co5 130.5(9) . . ? C25 O25 Co6 118.6(8) . . ? Co5 O25 Co6 92.0(3) . . ? C25 O25 Co2 94.3(9) . . ? Co5 O25 Co2 117.7(4) . . ? Co6 O25 Co2 101.9(3) . . ? N15 C25 O25 109.0(14) . . ? N15 C25 C35 124.8(15) . . ? O25 C25 C35 126.2(16) . . ? C25 C35 C45 117.4(16) . . ? C35 C45 C55 120.7(16) . . ? C65 C55 C45 117.7(14) . . ? N15 C65 C55 123.4(14) . . ? N15 C65 Cl5 117.8(12) . . ? C55 C65 Cl5 118.8(13) . . ? C21 N11 C61 119.9(13) . . ? C21 N11 Co3 97.6(9) . . ? C61 N11 Co3 142.1(11) . . ? C21 O21 Co1 145.1(9) . . ? C21 O21 Co3 87.9(9) . . ? Co1 O21 Co3 92.1(4) . . ? O21 C21 N11 114.8(13) . . ? O21 C21 C31 124.5(16) . . ? N11 C21 C31 120.7(14) . . ? C41 C31 C21 115.9(16) . . ? C51 C41 C31 124.2(17) . . ? C41 C51 C61 119.1(17) . . ? N11 C61 C51 120.1(15) . . ? N11 C61 Cl1 115.2(13) . . ? C51 C61 Cl1 124.7(15) . . ? C63 N13 C23 117.5(13) . . ? C63 N13 Co4 138.3(11) . . ? C23 N13 Co4 104.0(9) . . ? C23 O23 Co2 120.7(7) . . ? C23 O23 Co1 126.1(8) . . ? Co2 O23 Co1 96.5(3) . . ? O23 C23 N13 112.8(12) . . ? O23 C23 C33 125.6(14) . . ? N13 C23 C33 121.6(13) . . ? C43 C33 C23 118.2(15) . . ? C53 C43 C33 121.0(16) . . ? C43 C53 C63 116.8(15) . . ? N13 C63 C53 124.8(15) . . ? N13 C63 Cl3 115.4(12) . . ? C53 C63 Cl3 119.8(13) . . ? C26 N16 C66 119.4(12) . . ? C26 N16 Co6 96.2(8) . . ? C66 N16 Co6 144.1(10) . . ? C26 O26 Co1 133.1(8) . . ? C26 O26 Co2 115.6(7) . . ? Co1 O26 Co2 95.0(3) . . ? C26 O26 Co6 87.5(8) . . ? Co1 O26 Co6 124.1(4) . . ? Co2 O26 Co6 98.1(3) . . ? O26 C26 N16 116.3(12) . . ? O26 C26 C36 122.8(13) . . ? N16 C26 C36 120.9(12) . . ? C46 C36 C26 119.3(13) . . ? C36 C46 C56 118.2(14) . . ? C66 C56 C46 119.5(14) . . ? C56 C66 N16 122.7(13) . . ? C56 C66 Cl6 122.1(11) . . ? N16 C66 Cl6 115.2(11) . . ? C29 N19 C69 115.1(15) . . ? C29 O29 Co5 131.7(14) . . ? O29 C29 N19 115.5(17) . . ? O29 C29 C39 119.5(18) . . ? N19 C29 C39 124.6(16) . . ? C49 C39 C29 117.2(17) . . ? C39 C49 C59 117.1(18) . . ? C69 C59 C49 120.2(19) . . ? C59 C69 N19 122.3(18) . . ? C59 C69 Cl69 122.6(16) . . ? N19 C69 Cl69 114.6(15) . . ? N1X C2X C3X 163(4) . . ? N1X' C2X' C3X' 162(4) . . ? N1Y C2Y C3Y 178(2) . . ? N1Z C2Z C3Z 178(2) . . ? _diffrn_measured_fraction_theta_max 0.824 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.824 _refine_diff_density_max 0.746 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.103 data_comecn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Co7(OH)2(chp)8(OBz)4(MeCN)].MeOH _chemical_formula_sum 'C71 H53 Cl8 Co7 N9 O19' _chemical_formula_weight 2032.33 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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 24.034(8) _cell_length_b 20.018(5) _cell_length_c 16.304(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7844(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 54 _cell_measurement_theta_min 10 _cell_measurement_theta_max 13.5 _exptl_crystal_description lath _exptl_crystal_colour pink _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4076 _exptl_absorpt_coefficient_mu 1.792 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.656 _exptl_absorpt_correction_T_max 0.793 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% ? _diffrn_reflns_number 3903 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.2127 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 20.00 _reflns_number_total 3788 _reflns_number_gt 1725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _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^)+(0.0817P)^2^+24.5522P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3788 _refine_ls_number_parameters 292 _refine_ls_number_restraints 143 _refine_ls_R_factor_all 0.2048 _refine_ls_R_factor_gt 0.0897 _refine_ls_wR_factor_ref 0.2317 _refine_ls_wR_factor_gt 0.1760 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.008 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.08712(16) 0.2500 -0.3347(2) 0.0298(11) Uani 1 2 d S . . Co2 Co 0.20452(16) 0.2500 -0.2347(2) 0.0348(12) Uani 1 2 d S . . Co3 Co 0.07238(11) 0.16517(14) -0.50012(16) 0.0312(8) Uani 1 1 d . . . Co4 Co 0.22490(11) 0.15369(16) -0.41123(17) 0.0418(9) Uani 1 1 d . . . Co5 Co 0.32222(17) 0.2500 -0.3733(3) 0.0515(15) Uani 1 2 d S . . O1 O 0.1073(7) 0.2500 -0.4591(10) 0.028(5) Uiso 1 2 d S . . H1 H 0.1485 0.2500 -0.4678 0.034 Uiso 1 2 calc SR . . O2 O 0.2471(7) 0.2500 -0.4466(11) 0.029(5) Uiso 1 2 d S . . H2 H 0.2573 0.2500 -0.5060 0.035 Uiso 1 2 calc SR . . N11 N 0.0509(6) 0.0856(6) -0.4273(8) 0.027(4) Uiso 1 1 d D . . C21 C 0.0230(7) 0.1166(8) -0.3673(11) 0.036(6) Uiso 1 1 d D . . C31 C -0.0100(7) 0.0819(8) -0.3113(10) 0.029(5) Uiso 1 1 d D . . H31 H -0.0321 0.1048 -0.2719 0.035 Uiso 1 1 calc R . . C41 C -0.0092(8) 0.0123(9) -0.3152(12) 0.047(6) Uiso 1 1 d D . . H41 H -0.0299 -0.0131 -0.2766 0.056 Uiso 1 1 calc R . . C51 C 0.0216(7) -0.0202(8) -0.3752(10) 0.029(5) Uiso 1 1 d D . . H51 H 0.0222 -0.0676 -0.3791 0.035 Uiso 1 1 calc R . . C61 C 0.0502(7) 0.0183(7) -0.4271(10) 0.031(5) Uiso 1 1 d D . . O21 O 0.0263(5) 0.1815(6) -0.3680(7) 0.031(4) Uiso 1 1 d D . . Cl1 Cl 0.0917(2) -0.0189(3) -0.5014(4) 0.0563(18) Uani 1 1 d D . . N12 N 0.1151(5) 0.1442(8) -0.6079(8) 0.034(5) Uiso 1 1 d D . . C22 C 0.1654(6) 0.1354(10) -0.5754(9) 0.036(6) Uiso 1 1 d D . . C32 C 0.2124(7) 0.1222(11) -0.6231(11) 0.060(7) Uiso 1 1 d D . . H32 H 0.2477 0.1132 -0.5994 0.073 Uiso 1 1 calc R . . C42 C 0.2041(8) 0.1229(12) -0.7086(11) 0.068(8) Uiso 1 1 d D . . H42 H 0.2351 0.1166 -0.7438 0.081 Uiso 1 1 calc R . . C52 C 0.1520(7) 0.1326(12) -0.7427(12) 0.072(8) Uiso 1 1 d D . . H52 H 0.1461 0.1314 -0.8003 0.087 Uiso 1 1 calc R . . C62 C 0.1104(6) 0.1436(10) -0.6898(9) 0.037(6) Uiso 1 1 d D . . O22 O 0.1660(5) 0.1355(6) -0.4957(7) 0.031(3) Uiso 1 1 d D . . Cl2 Cl 0.0441(2) 0.1579(3) -0.7282(3) 0.0457(15) Uani 1 1 d D . . N13 N 0.1889(6) 0.0814(7) -0.3360(9) 0.036(5) Uiso 1 1 d D . . C23 C 0.1544(7) 0.1199(8) -0.2922(10) 0.034(6) Uiso 1 1 d D . . C33 C 0.1211(7) 0.0940(8) -0.2309(11) 0.039(6) Uiso 1 1 d D . . H33 H 0.0974 0.1219 -0.1993 0.047 Uiso 1 1 calc R . . C43 C 0.1239(8) 0.0248(9) -0.2173(12) 0.056(7) Uiso 1 1 d D . . H43 H 0.1000 0.0046 -0.1780 0.067 Uiso 1 1 calc R . . C53 C 0.1611(8) -0.0137(9) -0.2606(11) 0.053(7) Uiso 1 1 d D . . H53 H 0.1651 -0.0600 -0.2497 0.063 Uiso 1 1 calc R . . C63 C 0.1912(7) 0.0163(8) -0.3185(10) 0.033(6) Uiso 1 1 d D . . O23 O 0.1555(5) 0.1825(6) -0.3136(7) 0.031(3) Uiso 1 1 d D . . Cl3 Cl 0.2375(3) -0.0294(3) -0.3783(4) 0.065(2) Uani 1 1 d D . . N14 N 0.2519(6) 0.1678(8) -0.1778(8) 0.035(5) Uiso 1 1 d D . . C24 C 0.2822(7) 0.1492(9) -0.2425(9) 0.038(6) Uiso 1 1 d D . . C34 C 0.3192(8) 0.0963(9) -0.2401(11) 0.053(7) Uiso 1 1 d D . . H34 H 0.3418 0.0855 -0.2861 0.064 Uiso 1 1 calc R . . C44 C 0.3222(8) 0.0593(10) -0.1677(11) 0.055(7) Uiso 1 1 d D . . H44 H 0.3444 0.0200 -0.1653 0.066 Uiso 1 1 calc R . . C54 C 0.2930(8) 0.0799(9) -0.0998(11) 0.049(7) Uiso 1 1 d D . . H54 H 0.2953 0.0566 -0.0492 0.058 Uiso 1 1 calc R . . C64 C 0.2615(7) 0.1339(9) -0.1084(9) 0.046(6) Uiso 1 1 d D . . O24 O 0.2722(5) 0.1832(6) -0.3088(7) 0.044(4) Uiso 1 1 d D . . Cl4 Cl 0.2225(4) 0.1614(6) -0.0265(4) 0.172(6) Uani 1 1 d D . . O1A O -0.0008(5) 0.1950(7) -0.5466(8) 0.043(4) Uiso 1 1 d . . . C1A C -0.0214(10) 0.2500 -0.5568(18) 0.042(9) Uiso 1 2 d SD . . C2A C -0.0794(10) 0.2500 -0.5909(18) 0.040(8) Uiso 1 2 d SD . . C3A C -0.1085(9) 0.1914(11) -0.6010(16) 0.082(9) Uiso 1 1 d D . . H3A H -0.0915 0.1497 -0.5887 0.099 Uiso 1 1 calc R . . C4A C -0.1630(10) 0.1936(13) -0.6292(17) 0.097(10) Uiso 1 1 d D . . H4A H -0.1825 0.1526 -0.6343 0.116 Uiso 1 1 calc R . . C5A C -0.1899(15) 0.2500 -0.650(2) 0.085(13) Uiso 1 2 d SD . . H5A H -0.2250 0.2500 -0.6769 0.102 Uiso 1 2 calc SR . . O1B O 0.0646(7) 0.2500 -0.2173(10) 0.031(5) Uiso 1 2 d SD . . O2B O 0.1448(7) 0.2500 -0.1482(11) 0.044(6) Uiso 1 2 d SD . . C1B C 0.0944(10) 0.2500 -0.1525(13) 0.041(9) Uiso 1 2 d SD . . C2B C 0.0642(10) 0.2500 -0.0719(13) 0.043(9) Uiso 1 2 d SD . . C3B C 0.0939(10) 0.2500 0.0010(13) 0.031(8) Uiso 1 2 d SD . . H3B H 0.1334 0.2500 0.0003 0.037 Uiso 1 2 calc SR . . C4B C 0.0653(12) 0.2500 0.0749(16) 0.055(10) Uiso 1 2 d SD . . H4B H 0.0858 0.2500 0.1247 0.066 Uiso 1 2 calc SR . . C5B C 0.0093(13) 0.2500 0.078(2) 0.102(15) Uiso 1 2 d SD . . H5B H -0.0092 0.2500 0.1295 0.122 Uiso 1 2 calc SR . . C6B C -0.0221(16) 0.2500 0.004(3) 0.15(2) Uiso 1 2 d SD . . H6B H -0.0616 0.2500 0.0055 0.183 Uiso 1 2 calc SR . . C7B C 0.0071(12) 0.2500 -0.072(2) 0.107(16) Uiso 1 2 d SD . . H7B H -0.0127 0.2500 -0.1226 0.128 Uiso 1 2 calc SR . . O1C O 0.2915(6) 0.1079(7) -0.4655(9) 0.056(4) Uiso 1 1 d D . . O2C O 0.3625(6) 0.1737(8) -0.4287(9) 0.066(5) Uiso 1 1 d D . . C1C C 0.3428(9) 0.1213(11) -0.4511(15) 0.063(8) Uiso 1 1 d D . . C2C C 0.3796(9) 0.0602(11) -0.4524(16) 0.075(8) Uiso 1 1 d D . . C3C C 0.4317(10) 0.0663(14) -0.4143(19) 0.124(12) Uiso 1 1 d D . . H3C H 0.4437 0.1074 -0.3913 0.149 Uiso 1 1 calc R . . C4C C 0.4651(12) 0.0091(15) -0.412(2) 0.135(13) Uiso 1 1 d D . . H4C H 0.5021 0.0128 -0.3916 0.162 Uiso 1 1 calc R . . C5C C 0.4465(12) -0.0511(15) -0.4364(19) 0.114(12) Uiso 1 1 d D . . H5C H 0.4668 -0.0902 -0.4222 0.137 Uiso 1 1 calc R . . C6C C 0.3971(13) -0.0570(16) -0.483(2) 0.127(13) Uiso 1 1 d D . . H6C H 0.3876 -0.0970 -0.5114 0.153 Uiso 1 1 calc R . . C7C C 0.3624(11) 0.0012(13) -0.4857(17) 0.088(9) Uiso 1 1 d D . . H7C H 0.3268 -0.0013 -0.5109 0.105 Uiso 1 1 calc R . . N1S N 0.3809(11) 0.2500 -0.2721(19) 0.062(9) Uiso 1 2 d S . . C2S C 0.3932(14) 0.2500 -0.206(2) 0.051(10) Uiso 1 2 d S . . C3S C 0.4068(15) 0.2500 -0.120(2) 0.079(12) Uiso 1 2 d S . . H3S1 H 0.3792 0.2764 -0.0901 0.118 Uiso 0.50 1 d PR . . H3S2 H 0.4438 0.2695 -0.1125 0.118 Uiso 0.50 1 d PR . . H3S3 H 0.4067 0.2040 -0.0996 0.118 Uiso 0.50 1 d PR . . C1M C 0.3447(19) 0.234(3) 0.373(3) 0.11(2) Uiso 0.50 1 d PD A -1 H1M1 H 0.3069 0.2270 0.3517 0.166 Uiso 0.50 1 d PR A -1 H1M2 H 0.3586 0.2773 0.3550 0.166 Uiso 0.50 1 d PR A -1 H1M3 H 0.3442 0.2317 0.4328 0.166 Uiso 0.50 1 d PR A -1 O1M O 0.3811(18) 0.179(2) 0.344(3) 0.147(18) Uiso 0.50 1 d PD A -1 H1M H 0.3716 0.1418 0.3643 0.220 Uiso 0.50 1 d PR A -1 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 0.032(3) 0.041(3) 0.016(2) 0.000 0.001(2) 0.000 Co2 0.034(2) 0.048(3) 0.023(2) 0.000 -0.001(2) 0.000 Co3 0.0325(16) 0.0385(17) 0.0227(15) -0.0028(16) -0.0048(14) 0.0047(15) Co4 0.0366(18) 0.061(2) 0.0282(17) 0.0017(19) -0.0019(15) 0.0097(18) Co5 0.032(3) 0.095(4) 0.028(3) 0.000 0.002(2) 0.000 Cl1 0.050(4) 0.060(4) 0.059(4) -0.015(4) 0.003(4) 0.019(3) Cl2 0.064(4) 0.049(4) 0.024(3) 0.001(3) -0.013(3) 0.005(4) Cl3 0.073(4) 0.061(4) 0.061(4) -0.011(4) -0.006(4) 0.032(4) Cl4 0.216(10) 0.258(13) 0.042(5) 0.030(6) 0.032(5) 0.194(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1B 1.990(17) . ? Co1 O21 2.076(12) . ? Co1 O21 2.076(12) 8_565 ? Co1 O1 2.086(17) . ? Co1 O23 2.155(12) 8_565 ? Co1 O23 2.155(12) . ? Co2 O2B 2.012(18) . ? Co2 O23 2.207(12) . ? Co2 O23 2.207(12) 8_565 ? Co2 N14 2.207(14) 8_565 ? Co2 N14 2.207(14) . ? Co3 O1A 2.006(13) . ? Co3 O1 2.009(10) . ? Co3 N11 2.053(13) . ? Co3 N12 2.077(13) . ? Co3 O22 2.329(11) . ? Co4 O22 2.008(11) . ? Co4 O1C 2.046(14) . ? Co4 O2 2.082(7) . ? Co4 N13 2.086(14) . ? Co4 O24 2.104(13) . ? Co4 O23 2.377(12) . ? Co5 O2C 2.022(15) 8_565 ? Co5 O2C 2.022(15) . ? Co5 O24 2.084(13) 8_565 ? Co5 O24 2.084(13) . ? Co5 O2 2.165(17) . ? Co5 N1S 2.17(3) . ? O1 Co3 2.009(10) 8_565 ? O2 Co4 2.082(7) 8_565 ? N11 C21 1.340(15) . ? N11 C61 1.347(15) . ? C21 O21 1.301(14) . ? C21 C31 1.394(16) . ? C31 C41 1.396(17) . ? C41 C51 1.387(16) . ? C51 C61 1.336(16) . ? C61 Cl1 1.736(13) . ? N12 C22 1.331(15) . ? N12 C62 1.341(15) . ? C22 O22 1.300(14) . ? C22 C32 1.397(16) . ? C32 C42 1.408(17) . ? C42 C52 1.382(18) . ? C52 C62 1.339(17) . ? C62 Cl2 1.734(13) . ? N13 C63 1.334(15) . ? N13 C23 1.338(15) . ? C23 O23 1.301(14) . ? C23 C33 1.381(16) . ? C33 C43 1.405(17) . ? C43 C53 1.376(17) . ? C53 C63 1.332(16) . ? C63 Cl3 1.739(14) . ? N14 C24 1.335(15) . ? N14 C64 1.338(15) . ? C24 O24 1.299(14) . ? C24 C34 1.384(16) . ? C34 C44 1.396(17) . ? C44 C54 1.373(17) . ? C54 C64 1.328(16) . ? C64 Cl4 1.722(14) . ? O1A C1A 1.219(16) . ? C1A O1A 1.219(16) 8_565 ? C1A C2A 1.50(2) . ? C2A C3A 1.38(2) 8_565 ? C2A C3A 1.38(2) . ? C3A C4A 1.39(2) . ? C4A C5A 1.34(2) . ? C5A C4A 1.34(2) 8_565 ? O1B C1B 1.28(2) . ? O2B C1B 1.21(2) . ? C1B C2B 1.50(2) . ? C2B C7B 1.37(3) . ? C2B C3B 1.39(2) . ? C3B C4B 1.39(2) . ? C4B C5B 1.35(3) . ? C5B C6B 1.42(3) . ? C6B C7B 1.43(3) . ? O1C C1C 1.28(2) . ? O2C C1C 1.21(2) . ? C1C C2C 1.51(2) . ? C2C C7C 1.36(3) . ? C2C C3C 1.40(2) . ? C3C C4C 1.40(2) . ? C4C C5C 1.35(2) . ? C5C C6C 1.42(3) . ? C6C C7C 1.43(3) . ? N1S C2S 1.12(4) . ? C2S C3S 1.43(4) . ? C1M O1M 1.478(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 O1B Co1 O21 93.4(5) . . ? O1B Co1 O21 93.4(5) . 8_565 ? O21 Co1 O21 82.6(7) . 8_565 ? O1B Co1 O1 177.7(7) . . ? O21 Co1 O1 84.8(5) . . ? O21 Co1 O1 84.8(5) 8_565 . ? O1B Co1 O23 93.1(5) . 8_565 ? O21 Co1 O23 173.0(5) . 8_565 ? O21 Co1 O23 99.5(5) 8_565 8_565 ? O1 Co1 O23 88.7(5) . 8_565 ? O1B Co1 O23 93.1(5) . . ? O21 Co1 O23 99.5(5) . . ? O21 Co1 O23 173.0(5) 8_565 . ? O1 Co1 O23 88.7(5) . . ? O23 Co1 O23 77.7(6) 8_565 . ? O2B Co2 O23 91.6(5) . . ? O2B Co2 O23 91.6(5) . 8_565 ? O23 Co2 O23 75.6(6) . 8_565 ? O2B Co2 N14 94.2(5) . 8_565 ? O23 Co2 N14 167.9(5) . 8_565 ? O23 Co2 N14 93.7(5) 8_565 8_565 ? O2B Co2 N14 94.2(5) . . ? O23 Co2 N14 93.7(5) . . ? O23 Co2 N14 167.9(5) 8_565 . ? N14 Co2 N14 96.5(8) 8_565 . ? O1A Co3 O1 103.9(6) . . ? O1A Co3 N11 103.2(6) . . ? O1 Co3 N11 124.7(6) . . ? O1A Co3 N12 100.0(5) . . ? O1 Co3 N12 104.2(7) . . ? N11 Co3 N12 117.2(6) . . ? O1A Co3 O22 159.2(5) . . ? O1 Co3 O22 78.5(5) . . ? N11 Co3 O22 91.6(5) . . ? N12 Co3 O22 59.8(4) . . ? O22 Co4 O1C 100.0(5) . . ? O22 Co4 O2 99.1(6) . . ? O1C Co4 O2 95.4(6) . . ? O22 Co4 N13 89.2(5) . . ? O1C Co4 N13 105.6(6) . . ? O2 Co4 N13 155.8(6) . . ? O22 Co4 O24 167.3(5) . . ? O1C Co4 O24 92.7(5) . . ? O2 Co4 O24 79.7(6) . . ? N13 Co4 O24 87.3(5) . . ? O22 Co4 O23 90.5(4) . . ? O1C Co4 O23 161.4(5) . . ? O2 Co4 O23 98.1(5) . . ? N13 Co4 O23 58.9(4) . . ? O24 Co4 O23 77.3(5) . . ? O2C Co5 O2C 98.2(9) 8_565 . ? O2C Co5 O24 90.9(6) 8_565 8_565 ? O2C Co5 O24 170.7(6) . 8_565 ? O2C Co5 O24 170.7(6) 8_565 . ? O2C Co5 O24 90.9(6) . . ? O24 Co5 O24 79.9(7) 8_565 . ? O2C Co5 O2 98.8(5) 8_565 . ? O2C Co5 O2 98.8(5) . . ? O24 Co5 O2 78.3(5) 8_565 . ? O24 Co5 O2 78.3(5) . . ? O2C Co5 N1S 91.7(7) 8_565 . ? O2C Co5 N1S 91.7(7) . . ? O24 Co5 N1S 89.5(7) 8_565 . ? O24 Co5 N1S 89.5(7) . . ? O2 Co5 N1S 164.0(9) . . ? Co3 O1 Co3 115.4(8) 8_565 . ? Co3 O1 Co1 103.1(6) 8_565 . ? Co3 O1 Co1 103.1(6) . . ? Co4 O2 Co4 135.7(9) 8_565 . ? Co4 O2 Co5 93.5(5) 8_565 . ? Co4 O2 Co5 93.5(5) . . ? C21 N11 C61 117.1(13) . . ? C21 N11 Co3 100.8(10) . . ? C61 N11 Co3 141.3(11) . . ? O21 C21 N11 115.2(14) . . ? O21 C21 C31 122.6(14) . . ? N11 C21 C31 122.2(14) . . ? C21 C31 C41 117.3(15) . . ? C51 C41 C31 120.6(16) . . ? C61 C51 C41 116.8(15) . . ? C51 C61 N11 125.8(14) . . ? C51 C61 Cl1 119.4(12) . . ? N11 C61 Cl1 114.8(11) . . ? C21 O21 Co1 134.4(13) . . ? C22 N12 C62 118.1(13) . . ? C22 N12 Co3 98.0(9) . . ? C62 N12 Co3 143.4(11) . . ? O22 C22 N12 114.1(14) . . ? O22 C22 C32 123.2(14) . . ? N12 C22 C32 122.6(14) . . ? C22 C32 C42 115.7(16) . . ? C52 C42 C32 121.8(17) . . ? C62 C52 C42 116.2(16) . . ? C52 C62 N12 125.4(14) . . ? C52 C62 Cl2 118.8(12) . . ? N12 C62 Cl2 115.8(11) . . ? C22 O22 Co4 134.0(11) . . ? C22 O22 Co3 87.6(9) . . ? Co4 O22 Co3 131.0(6) . . ? C63 N13 C23 118.3(13) . . ? C63 N13 Co4 141.8(11) . . ? C23 N13 Co4 99.8(10) . . ? O23 C23 N13 113.6(14) . . ? O23 C23 C33 124.5(15) . . ? N13 C23 C33 121.9(14) . . ? C23 C33 C43 117.2(15) . . ? C53 C43 C33 120.1(16) . . ? C63 C53 C43 117.7(16) . . ? C53 C63 N13 124.6(14) . . ? C53 C63 Cl3 120.5(13) . . ? N13 C63 Cl3 114.8(12) . . ? C23 O23 Co1 129.2(12) . . ? C23 O23 Co2 116.4(12) . . ? Co1 O23 Co2 96.7(5) . . ? C23 O23 Co4 87.7(9) . . ? Co1 O23 Co4 125.5(5) . . ? Co2 O23 Co4 99.4(5) . . ? C24 N14 C64 115.7(13) . . ? C24 N14 Co2 99.0(10) . . ? C64 N14 Co2 145.3(11) . . ? O24 C24 N14 114.2(14) . . ? O24 C24 C34 123.0(15) . . ? N14 C24 C34 122.7(14) . . ? C24 C34 C44 117.7(16) . . ? C54 C44 C34 119.7(16) . . ? C64 C54 C44 116.8(16) . . ? C54 C64 N14 126.9(14) . . ? C54 C64 Cl4 119.3(13) . . ? N14 C64 Cl4 113.5(12) . . ? C24 O24 Co5 130.4(12) . . ? C24 O24 Co4 127.9(12) . . ? Co5 O24 Co4 95.3(5) . . ? C1A O1A Co3 132.5(15) . . ? O1A C1A O1A 129(2) 8_565 . ? O1A C1A C2A 115.3(12) 8_565 . ? O1A C1A C2A 115.3(12) . . ? C3A C2A C3A 117(3) 8_565 . ? C3A C2A C1A 121.1(13) 8_565 . ? C3A C2A C1A 121.1(13) . . ? C2A C3A C4A 119(2) . . ? C5A C4A C3A 124(3) . . ? C4A C5A C4A 114(3) 8_565 . ? C1B O1B Co1 130.1(15) . . ? C1B O2B Co2 132.2(16) . . ? O2B C1B O1B 127(2) . . ? O2B C1B C2B 116(2) . . ? O1B C1B C2B 117.0(19) . . ? C7B C2B C3B 121(2) . . ? C7B C2B C1B 119(2) . . ? C3B C2B C1B 120.1(19) . . ? C4B C3B C2B 119(2) . . ? C5B C4B C3B 122(3) . . ? C4B C5B C6B 120(3) . . ? C5B C6B C7B 119(3) . . ? C2B C7B C6B 119(3) . . ? C1C O1C Co4 125.4(14) . . ? C1C O2C Co5 127.2(15) . . ? O2C C1C O1C 128(2) . . ? O2C C1C C2C 118.6(18) . . ? O1C C1C C2C 113.1(18) . . ? C7C C2C C3C 121(2) . . ? C7C C2C C1C 122(2) . . ? C3C C2C C1C 116.6(19) . . ? C4C C3C C2C 117(2) . . ? C5C C4C C3C 122(3) . . ? C4C C5C C6C 121(3) . . ? C5C C6C C7C 116(3) . . ? C2C C7C C6C 121(2) . . ? C2S N1S Co5 155(3) . . ? N1S C2S C3S 178(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.748 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.139 data_ebduno _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '{[Co8Na2(OH)2(Hmhp)(mhp)9(PhCH2CO2)7].2.5MeCN}' _chemical_formula_sum 'C121 H119.50 Co8 N12.50 Na2 O26' _chemical_formula_weight 2682.21 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' 'Na' 'Na' 0.0362 0.0249 '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 14.325(5) _cell_length_b 17.769(5) _cell_length_c 25.176(10) _cell_angle_alpha 81.11(2) _cell_angle_beta 76.85(2) _cell_angle_gamma 82.24(3) _cell_volume 6132(4) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 52 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 16 _exptl_crystal_description 'plate developed in (010)' _exptl_crystal_colour Purple _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2758 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.479 _exptl_absorpt_correction_T_max 0.654 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 14819 _diffrn_reflns_av_R_equivalents 0.0929 _diffrn_reflns_av_sigmaI/netI 0.2265 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 20.04 _reflns_number_total 11476 _reflns_number_gt 5527 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _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^)+(0.0843P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0015(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11476 _refine_ls_number_parameters 769 _refine_ls_number_restraints 1461 _refine_ls_R_factor_all 0.2016 _refine_ls_R_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.2173 _refine_ls_wR_factor_gt 0.1731 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 0.956 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.21531(14) 0.13989(11) 0.23848(8) 0.0255(6) Uani 1 1 d . . . Co2 Co 0.13809(14) 0.01947(11) 0.17852(8) 0.0260(6) Uani 1 1 d . A . Co3 Co 0.22221(15) 0.10644(12) 0.36886(9) 0.0313(6) Uani 1 1 d . A . Co4 Co 0.11668(15) -0.05738(11) 0.31986(8) 0.0273(6) Uani 1 1 d . A . Co5 Co 0.19295(15) -0.17567(11) 0.23860(8) 0.0269(6) Uani 1 1 d . A . Co6 Co 0.35142(15) -0.06582(11) 0.20707(8) 0.0272(6) Uani 1 1 d . A . Co7 Co 0.42567(15) 0.10595(12) 0.26939(9) 0.0327(7) Uani 1 1 d . A . Co8 Co 0.15721(17) -0.46570(12) 0.21708(10) 0.0415(7) Uani 1 1 d . A . Na1 Na 0.2389(4) -0.3594(3) 0.2763(2) 0.0387(17) Uani 1 1 d . . . Na2 Na 0.2019(4) 0.3149(3) 0.2164(2) 0.0399(18) Uani 1 1 d . . . O1 O 0.2904(6) 0.0783(5) 0.2968(3) 0.023(3) Uiso 1 1 d . . . H1 H 0.2896 0.0227 0.2966 0.028 Uiso 1 1 calc R . . O2 O 0.2539(6) -0.1004(5) 0.2788(4) 0.026(3) Uiso 1 1 d . . . H2 H 0.2891 -0.1312 0.3057 0.032 Uiso 1 1 calc R A . O2A O 0.4253(7) 0.1907(6) 0.3130(4) 0.046(3) Uiso 1 1 d D . . O1A O 0.2929(7) 0.1901(6) 0.3793(4) 0.047(3) Uiso 1 1 d D . . C1A C 0.3691(9) 0.2178(7) 0.3520(6) 0.034(4) Uiso 1 1 d D . . C2A C 0.3883(9) 0.2899(8) 0.3712(7) 0.058(6) Uiso 1 1 d D . . H2A1 H 0.3674 0.3345 0.3469 0.069 Uiso 1 1 calc R . . H2A2 H 0.3494 0.2938 0.4083 0.069 Uiso 1 1 calc R . . C3A C 0.4916(9) 0.2924(9) 0.3720(6) 0.054(5) Uiso 1 1 d D . . C4A C 0.5195(14) 0.2891(14) 0.4212(7) 0.122(9) Uiso 1 1 d D . . H4A H 0.4737 0.2867 0.4546 0.147 Uiso 1 1 calc R . . C5A C 0.6175(16) 0.2894(16) 0.4207(9) 0.162(12) Uiso 1 1 d D . . H5A H 0.6382 0.2795 0.4541 0.194 Uiso 1 1 calc R . . C6A C 0.6823(14) 0.3034(13) 0.3740(9) 0.117(9) Uiso 1 1 d D . . H6A H 0.7460 0.3087 0.3755 0.141 Uiso 1 1 calc R . . C7A C 0.6582(12) 0.3102(12) 0.3249(8) 0.098(8) Uiso 1 1 d D . . H7A H 0.7039 0.3201 0.2920 0.117 Uiso 1 1 calc R . . C8A C 0.5628(10) 0.3021(9) 0.3243(6) 0.046(5) Uiso 1 1 d D . . H8A H 0.5459 0.3031 0.2902 0.056 Uiso 1 1 calc R . . O2B O 0.0899(7) 0.1249(5) 0.1449(4) 0.030(3) Uiso 1 1 d D . . O1B O 0.1443(7) 0.2112(5) 0.1836(4) 0.035(3) Uiso 1 1 d D . . C1B C 0.1009(10) 0.1914(7) 0.1501(5) 0.032(4) Uiso 1 1 d D . . C2B C 0.0640(8) 0.2558(7) 0.1109(5) 0.032(4) Uiso 1 1 d D . . H2B1 H 0.0994 0.3002 0.1085 0.038 Uiso 1 1 calc R . . H2B2 H 0.0771 0.2396 0.0742 0.038 Uiso 1 1 calc R . . C3B C -0.0418(8) 0.2796(7) 0.1280(6) 0.035(4) Uiso 1 1 d D . . C4B C -0.1078(10) 0.2336(8) 0.1586(6) 0.051(5) Uiso 1 1 d D . . H4B H -0.0866 0.1827 0.1705 0.061 Uiso 1 1 calc R . . C5B C -0.2059(11) 0.2585(9) 0.1732(7) 0.067(6) Uiso 1 1 d D . . H5B H -0.2490 0.2263 0.1969 0.081 Uiso 1 1 calc R . . C6B C -0.2379(12) 0.3303(9) 0.1525(7) 0.076(6) Uiso 1 1 d D . . H6B H -0.3040 0.3473 0.1608 0.091 Uiso 1 1 calc R . . C7B C -0.1760(11) 0.3768(10) 0.1205(8) 0.087(7) Uiso 1 1 d D . . H7B H -0.1994 0.4257 0.1058 0.105 Uiso 1 1 calc R . . C8B C -0.0772(10) 0.3542(8) 0.1085(6) 0.054(5) Uiso 1 1 d D . . H8B H -0.0344 0.3885 0.0875 0.064 Uiso 1 1 calc R . . O1C O 0.0868(7) -0.1608(5) 0.3687(4) 0.036(3) Uiso 1 1 d D . . O2C O 0.1497(7) -0.2474(5) 0.3111(4) 0.032(3) Uiso 1 1 d D A . C1C C 0.1005(10) -0.2273(7) 0.3558(5) 0.036(5) Uiso 1 1 d D A . C2C C 0.0563(8) -0.2899(7) 0.3987(6) 0.042(5) Uiso 1 1 d D . . H2C1 H 0.0725 -0.3390 0.3839 0.051 Uiso 1 1 calc R A . H2C2 H 0.0840 -0.2941 0.4313 0.051 Uiso 1 1 calc R . . C3C C -0.0509(8) -0.2743(8) 0.4150(5) 0.029(4) Uiso 1 1 d D A . C4C C -0.1109(10) -0.2803(9) 0.3808(6) 0.053(5) Uiso 1 1 d D . . H4C H -0.0848 -0.2958 0.3460 0.064 Uiso 1 1 calc R A . C5C C -0.2099(11) -0.2637(9) 0.3972(7) 0.066(6) Uiso 1 1 d D A . H5C H -0.2507 -0.2718 0.3746 0.080 Uiso 1 1 calc R . . C6C C -0.2474(11) -0.2363(10) 0.4452(7) 0.069(6) Uiso 1 1 d D . . H6C H -0.3142 -0.2227 0.4550 0.082 Uiso 1 1 calc R A . C7C C -0.1911(10) -0.2278(9) 0.4797(7) 0.063(6) Uiso 1 1 d D A . H7C H -0.2187 -0.2097 0.5136 0.076 Uiso 1 1 calc R . . C8C C -0.0919(9) -0.2462(8) 0.4648(5) 0.036(4) Uiso 1 1 d D . . H8C H -0.0523 -0.2396 0.4885 0.043 Uiso 1 1 calc R A . O2D O 0.4293(7) -0.1708(5) 0.2006(4) 0.035(3) Uiso 1 1 d D . . O1D O 0.3158(7) -0.2515(5) 0.2243(4) 0.035(3) Uiso 1 1 d D A . C1D C 0.4027(9) -0.2368(7) 0.2094(6) 0.036(5) Uiso 1 1 d D A . C2D C 0.4782(9) -0.3044(7) 0.1999(6) 0.051(5) Uiso 1 1 d D . . H2D1 H 0.4509 -0.3507 0.2203 0.061 Uiso 1 1 calc R A . H2D2 H 0.4922 -0.3103 0.1607 0.061 Uiso 1 1 calc R . . C3D C 0.5714(9) -0.2992(8) 0.2162(5) 0.038(5) Uiso 1 1 d D A . C4D C 0.6453(10) -0.2642(9) 0.1820(6) 0.059(6) Uiso 1 1 d D . . H4D H 0.6376 -0.2395 0.1472 0.071 Uiso 1 1 calc R A . C5D C 0.7325(11) -0.2645(10) 0.1979(7) 0.064(6) Uiso 1 1 d D A . H5D H 0.7835 -0.2407 0.1737 0.077 Uiso 1 1 calc R . . C6D C 0.7437(12) -0.2987(11) 0.2478(7) 0.087(7) Uiso 1 1 d D . . H6D H 0.8029 -0.2986 0.2581 0.104 Uiso 1 1 calc R A . C7D C 0.6722(11) -0.3331(10) 0.2836(7) 0.076(6) Uiso 1 1 d D A . H7D H 0.6812 -0.3569 0.3184 0.091 Uiso 1 1 calc R . . C8D C 0.5841(10) -0.3330(9) 0.2682(6) 0.049(5) Uiso 1 1 d D . . H8D H 0.5332 -0.3560 0.2931 0.059 Uiso 1 1 calc R A . O1E O 0.1168(7) -0.2233(5) 0.1939(4) 0.034(3) Uiso 1 1 d D . . O2E O 0.1493(7) -0.3483(5) 0.2087(4) 0.042(3) Uiso 1 1 d D A . C1E C 0.1009(10) -0.2891(7) 0.1900(5) 0.033(4) Uiso 1 1 d D A . C2E C 0.0220(9) -0.2958(8) 0.1610(5) 0.040(5) Uiso 1 1 d D . . H2E1 H 0.0093 -0.3496 0.1660 0.048 Uiso 1 1 calc R A . H2E2 H -0.0371 -0.2661 0.1779 0.048 Uiso 1 1 calc R . . C3E C 0.0470(10) -0.2680(7) 0.1010(5) 0.035(4) Uiso 1 1 d D A . C4E C 0.0979(12) -0.3141(8) 0.0640(6) 0.061(6) Uiso 1 1 d D . . H4E H 0.1133 -0.3662 0.0759 0.073 Uiso 1 1 calc R A . C5E C 0.1278(13) -0.2863(9) 0.0091(6) 0.072(6) Uiso 1 1 d D A . H5E H 0.1648 -0.3187 -0.0159 0.086 Uiso 1 1 calc R . . C6E C 0.1030(13) -0.2123(9) -0.0082(7) 0.077(7) Uiso 1 1 d D . . H6E H 0.1218 -0.1935 -0.0456 0.093 Uiso 1 1 calc R A . C7E C 0.0526(13) -0.1651(9) 0.0266(6) 0.065(6) Uiso 1 1 d D A . H7E H 0.0358 -0.1139 0.0133 0.078 Uiso 1 1 calc R . . C8E C 0.0242(11) -0.1902(7) 0.0823(6) 0.047(5) Uiso 1 1 d D . . H8E H -0.0094 -0.1561 0.1069 0.057 Uiso 1 1 calc R A . O2F O 0.2494(7) -0.5805(6) 0.2428(4) 0.050(3) Uiso 1 1 d D . . O1F O 0.3012(7) -0.4669(6) 0.2225(4) 0.045(3) Uiso 1 1 d D A . C1F C 0.3167(9) -0.5397(7) 0.2339(6) 0.045(5) Uiso 1 1 d D A . C2F C 0.4168(9) -0.5737(8) 0.2382(6) 0.056(5) Uiso 1 1 d D . . H2F1 H 0.4253 -0.5709 0.2753 0.067 Uiso 1 1 calc R A . H2F2 H 0.4232 -0.6280 0.2334 0.067 Uiso 1 1 calc R . . C3F C 0.4961(10) -0.5365(9) 0.1976(6) 0.050(5) Uiso 1 1 d D A . C4F C 0.5022(12) -0.5267(10) 0.1420(6) 0.068(6) Uiso 1 1 d D . . H4F H 0.4553 -0.5445 0.1277 0.081 Uiso 1 1 calc R A . C5F C 0.5776(12) -0.4906(10) 0.1062(7) 0.079(7) Uiso 1 1 d D A . H5F H 0.5831 -0.4855 0.0679 0.095 Uiso 1 1 calc R . . C6F C 0.6419(11) -0.4634(9) 0.1276(6) 0.059(6) Uiso 1 1 d D . . H6F H 0.6896 -0.4358 0.1037 0.070 Uiso 1 1 calc R A . C7F C 0.6413(12) -0.4736(10) 0.1812(7) 0.072(6) Uiso 1 1 d D A . H7F H 0.6913 -0.4582 0.1942 0.086 Uiso 1 1 calc R . . C8F C 0.5654(10) -0.5074(9) 0.2177(6) 0.055(5) Uiso 1 1 d D . . H8F H 0.5608 -0.5107 0.2559 0.066 Uiso 1 1 calc R A . O2G O 0.1850(8) -0.6049(6) 0.1392(4) 0.060(4) Uiso 1 1 d D . . O1G O 0.1765(8) -0.4798(5) 0.1388(4) 0.048(3) Uiso 1 1 d D . . C1G C 0.1958(11) -0.5396(7) 0.1140(5) 0.042(5) Uiso 1 1 d D A . C2G C 0.2388(12) -0.5284(8) 0.0536(5) 0.060(6) Uiso 1 1 d D . . H2G1 H 0.2168 -0.4765 0.0386 0.072 Uiso 1 1 calc R A . H2G2 H 0.3090 -0.5315 0.0488 0.072 Uiso 1 1 calc R . . C3G C 0.2159(11) -0.5835(8) 0.0210(6) 0.056(5) Uiso 1 1 d D A . C4G C 0.2673(11) -0.6527(8) 0.0127(6) 0.053(5) Uiso 1 1 d D . . H4G H 0.3204 -0.6681 0.0293 0.064 Uiso 1 1 calc R A . C5G C 0.2434(12) -0.7014(9) -0.0198(7) 0.069(6) Uiso 1 1 d D A . H5G H 0.2832 -0.7467 -0.0275 0.082 Uiso 1 1 calc R . . C6G C 0.1622(12) -0.6823(9) -0.0400(7) 0.069(6) Uiso 1 1 d D . . H6G H 0.1417 -0.7169 -0.0586 0.082 Uiso 1 1 calc R A . C7G C 0.1118(13) -0.6148(10) -0.0338(8) 0.092(7) Uiso 1 1 d D A . H7G H 0.0594 -0.6002 -0.0511 0.110 Uiso 1 1 calc R . . C8G C 0.1345(11) -0.5655(9) -0.0023(7) 0.064(6) Uiso 1 1 d D . . H8G H 0.0950 -0.5195 0.0035 0.076 Uiso 1 1 calc R A . N11 N 0.0900(8) 0.1692(6) 0.3785(4) 0.037(4) Uiso 1 1 d D . . C21 C 0.0916(9) 0.2276(7) 0.3372(5) 0.035(4) Uiso 1 1 d D . . C31 C 0.0224(10) 0.2904(7) 0.3423(6) 0.042(5) Uiso 1 1 d D . . H31 H 0.0244 0.3323 0.3144 0.050 Uiso 1 1 calc R . . C41 C -0.0490(11) 0.2900(8) 0.3890(6) 0.051(5) Uiso 1 1 d D . . H41 H -0.0956 0.3325 0.3932 0.061 Uiso 1 1 calc R . . C51 C -0.0538(10) 0.2284(7) 0.4299(6) 0.043(5) Uiso 1 1 d D . . H51 H -0.1043 0.2275 0.4612 0.052 Uiso 1 1 calc R . . C61 C 0.0172(10) 0.1686(7) 0.4235(5) 0.039(5) Uiso 1 1 d D . . O21 O 0.1596(7) 0.2212(5) 0.2932(4) 0.035(3) Uiso 1 1 d D . . C1M C 0.0190(11) 0.0983(7) 0.4654(6) 0.045(5) Uiso 1 1 d D . . H1M1 H 0.0747 0.0629 0.4530 0.068 Uiso 1 1 calc R . . H1M2 H -0.0393 0.0738 0.4699 0.068 Uiso 1 1 calc R . . H1M3 H 0.0229 0.1130 0.5004 0.068 Uiso 1 1 calc R . . N12 N 0.2637(8) 0.0154(6) 0.4256(4) 0.028(3) Uiso 1 1 d D . . C22 C 0.2160(10) -0.0378(7) 0.4130(5) 0.034(4) Uiso 1 1 d D A . C32 C 0.2252(10) -0.1129(7) 0.4366(6) 0.042(5) Uiso 1 1 d D . . H32 H 0.1933 -0.1502 0.4274 0.050 Uiso 1 1 calc R . . C42 C 0.2837(11) -0.1309(8) 0.4747(6) 0.062(6) Uiso 1 1 d D . . H42 H 0.2897 -0.1812 0.4927 0.074 Uiso 1 1 calc R . . C52 C 0.3334(11) -0.0766(7) 0.4866(6) 0.051(5) Uiso 1 1 d D . . H52 H 0.3736 -0.0901 0.5121 0.061 Uiso 1 1 calc R . . C62 C 0.3236(10) -0.0031(7) 0.4613(6) 0.040(5) Uiso 1 1 d D . . O22 O 0.1653(6) -0.0106(5) 0.3757(4) 0.029(3) Uiso 1 1 d D . . C2M C 0.3705(11) 0.0602(8) 0.4740(6) 0.052(5) Uiso 1 1 d D . . H2M1 H 0.3543 0.1074 0.4513 0.078 Uiso 1 1 calc R . . H2M2 H 0.4399 0.0476 0.4663 0.078 Uiso 1 1 calc R . . H2M3 H 0.3478 0.0668 0.5125 0.078 Uiso 1 1 calc R . . N13 N -0.0074(8) 0.0189(6) 0.3310(4) 0.033(3) Uiso 1 1 d D . . C23 C 0.0223(8) 0.0754(7) 0.2903(5) 0.029(4) Uiso 1 1 d D A . C33 C -0.0360(9) 0.1434(7) 0.2804(6) 0.036(4) Uiso 1 1 d D . . H33 H -0.0163 0.1809 0.2506 0.044 Uiso 1 1 calc R A . C43 C -0.1236(10) 0.1529(8) 0.3161(6) 0.043(5) Uiso 1 1 d D A . H43 H -0.1631 0.1995 0.3129 0.051 Uiso 1 1 calc R . . C53 C -0.1537(10) 0.0949(7) 0.3564(6) 0.043(5) Uiso 1 1 d D . . H53 H -0.2153 0.1009 0.3793 0.052 Uiso 1 1 calc R A . C63 C -0.0952(9) 0.0282(7) 0.3638(5) 0.031(4) Uiso 1 1 d D A . O23 O 0.1097(6) 0.0590(5) 0.2613(4) 0.030(3) Uiso 1 1 d D . . C3M C -0.1236(11) -0.0383(8) 0.4059(6) 0.051(5) Uiso 1 1 d D . . H3M1 H -0.0708 -0.0789 0.4036 0.076 Uiso 1 1 calc R A . H3M2 H -0.1799 -0.0568 0.3991 0.076 Uiso 1 1 calc R . . H3M3 H -0.1385 -0.0222 0.4423 0.076 Uiso 1 1 calc R . . N14 N 0.0043(7) -0.0316(6) 0.1894(4) 0.025(3) Uiso 1 1 d D . . C24 C -0.0009(8) -0.0811(7) 0.2354(5) 0.020(4) Uiso 1 1 d D A . C34 C -0.0844(9) -0.1148(8) 0.2609(6) 0.041(5) Uiso 1 1 d D . . H34 H -0.0891 -0.1458 0.2951 0.049 Uiso 1 1 calc R A . C44 C -0.1606(10) -0.1009(8) 0.2341(6) 0.046(5) Uiso 1 1 d D A . H44 H -0.2176 -0.1240 0.2496 0.055 Uiso 1 1 calc R . . C54 C -0.1533(10) -0.0539(8) 0.1851(6) 0.050(5) Uiso 1 1 d D . . H54 H -0.2042 -0.0462 0.1663 0.060 Uiso 1 1 calc R A . C64 C -0.0713(9) -0.0183(8) 0.1638(5) 0.042(5) Uiso 1 1 d D A . O24 O 0.0768(6) -0.0952(5) 0.2573(4) 0.034(3) Uiso 1 1 d D . . C4M C -0.0585(11) 0.0312(8) 0.1096(5) 0.055(5) Uiso 1 1 d D . . H4M1 H 0.0037 0.0510 0.1013 0.082 Uiso 1 1 calc R A . H4M2 H -0.1091 0.0735 0.1111 0.082 Uiso 1 1 calc R . . H4M3 H -0.0619 0.0012 0.0811 0.082 Uiso 1 1 calc R . . N15 N 0.2026(8) -0.0204(6) 0.0976(4) 0.026(3) Uiso 1 1 d D . . C25 C 0.2421(10) -0.0877(7) 0.1205(4) 0.025(4) Uiso 1 1 d D A . C35 C 0.2867(10) -0.1447(7) 0.0889(5) 0.038(5) Uiso 1 1 d D . . H35 H 0.3123 -0.1918 0.1052 0.046 Uiso 1 1 calc R A . C45 C 0.2927(11) -0.1310(7) 0.0327(5) 0.043(5) Uiso 1 1 d D A . H45 H 0.3234 -0.1686 0.0103 0.052 Uiso 1 1 calc R . . C55 C 0.2536(10) -0.0620(7) 0.0099(5) 0.038(5) Uiso 1 1 d D . . H55 H 0.2571 -0.0525 -0.0283 0.045 Uiso 1 1 calc R A . C65 C 0.2099(10) -0.0073(7) 0.0423(5) 0.028(4) Uiso 1 1 d D A . O25 O 0.2353(7) -0.0907(5) 0.1741(4) 0.029(3) Uiso 1 1 d D . . C5M C 0.1752(11) 0.0715(7) 0.0197(6) 0.048(5) Uiso 1 1 d D . . H5M1 H 0.1466 0.1011 0.0498 0.073 Uiso 1 1 calc R A . H5M2 H 0.1274 0.0686 -0.0015 0.073 Uiso 1 1 calc R . . H5M3 H 0.2291 0.0961 -0.0038 0.073 Uiso 1 1 calc R . . N16 N 0.4030(7) 0.0022(5) 0.1337(4) 0.020(3) Uiso 1 1 d D . . C26 C 0.3387(9) 0.0641(7) 0.1391(5) 0.026(4) Uiso 1 1 d D A . C36 C 0.3468(9) 0.1280(7) 0.0986(5) 0.032(4) Uiso 1 1 d D . . H36 H 0.3016 0.1715 0.1015 0.038 Uiso 1 1 calc R A . C46 C 0.4235(10) 0.1244(8) 0.0547(6) 0.045(5) Uiso 1 1 d D A . H46 H 0.4301 0.1664 0.0268 0.054 Uiso 1 1 calc R . . C56 C 0.4909(10) 0.0615(7) 0.0500(6) 0.041(5) Uiso 1 1 d D . . H56 H 0.5449 0.0613 0.0207 0.049 Uiso 1 1 calc R A . C66 C 0.4771(9) -0.0009(7) 0.0894(5) 0.040(5) Uiso 1 1 d D A . O26 O 0.2717(6) 0.0579(5) 0.1844(3) 0.024(3) Uiso 1 1 d D . . C6M C 0.5469(10) -0.0721(7) 0.0891(6) 0.051(5) Uiso 1 1 d D . . H6M1 H 0.5234 -0.1092 0.1202 0.076 Uiso 1 1 calc R A . H6M2 H 0.6093 -0.0594 0.0917 0.076 Uiso 1 1 calc R . . H6M3 H 0.5531 -0.0937 0.0552 0.076 Uiso 1 1 calc R . . N17 N 0.5113(8) 0.0168(6) 0.3017(4) 0.031(3) Uiso 1 1 d D . . C27 C 0.4939(9) -0.0414(7) 0.2777(5) 0.029(4) Uiso 1 1 d D A . C37 C 0.5294(11) -0.1164(8) 0.2916(6) 0.059(6) Uiso 1 1 d D . . H37 H 0.5141 -0.1566 0.2759 0.071 Uiso 1 1 calc R . . C47 C 0.5882(12) -0.1303(8) 0.3295(7) 0.066(6) Uiso 1 1 d D . . H47 H 0.6152 -0.1804 0.3391 0.079 Uiso 1 1 calc R . . C57 C 0.6073(11) -0.0703(8) 0.3533(6) 0.055(5) Uiso 1 1 d D . . H57 H 0.6460 -0.0801 0.3796 0.066 Uiso 1 1 calc R . . C67 C 0.5704(10) 0.0023(7) 0.3388(6) 0.043(5) Uiso 1 1 d D . . O27 O 0.4393(6) -0.0175(5) 0.2421(4) 0.027(3) Uiso 1 1 d D . . C7M C 0.5937(12) 0.0706(8) 0.3590(7) 0.061(6) Uiso 1 1 d D . . H7M1 H 0.5600 0.1165 0.3429 0.091 Uiso 1 1 calc R . . H7M2 H 0.6626 0.0740 0.3485 0.091 Uiso 1 1 calc R . . H7M3 H 0.5736 0.0658 0.3988 0.091 Uiso 1 1 calc R . . N18 N 0.4800(7) 0.1599(6) 0.1930(5) 0.037(4) Uiso 1 1 d D . . C28 C 0.4104(9) 0.2148(8) 0.1806(6) 0.045(5) Uiso 1 1 d D A . C38 C 0.4310(10) 0.2756(8) 0.1389(6) 0.047(5) Uiso 1 1 d D . . H38 H 0.3856 0.3181 0.1341 0.056 Uiso 1 1 calc R A . C48 C 0.5220(10) 0.2700(8) 0.1049(6) 0.047(5) Uiso 1 1 d D A . H48 H 0.5369 0.3068 0.0740 0.056 Uiso 1 1 calc R . . C58 C 0.5907(10) 0.2115(7) 0.1158(6) 0.044(5) Uiso 1 1 d D . . H58 H 0.6528 0.2096 0.0932 0.052 Uiso 1 1 calc R A . C68 C 0.5692(9) 0.1560(7) 0.1594(5) 0.033(4) Uiso 1 1 d D A . O28 O 0.3261(7) 0.2143(5) 0.2137(4) 0.036(3) Uiso 1 1 d D . . C8M C 0.6385(10) 0.0894(8) 0.1726(6) 0.054(5) Uiso 1 1 d D . . H8A H 0.6081 0.0570 0.2048 0.081 Uiso 1 1 calc R A . H8B H 0.6948 0.1074 0.1798 0.081 Uiso 1 1 calc R . . H8C H 0.6580 0.0601 0.1416 0.081 Uiso 1 1 calc R . . N19 N 0.0253(8) -0.4894(7) 0.2644(5) 0.051(4) Uiso 1 1 d D . . C29 C 0.0328(10) -0.4682(9) 0.3124(6) 0.051(5) Uiso 1 1 d D A . C39 C -0.0433(10) -0.4700(10) 0.3578(6) 0.065(6) Uiso 1 1 d D . . H39 H -0.0375 -0.4558 0.3913 0.078 Uiso 1 1 calc R A . C49 C -0.1283(11) -0.4938(11) 0.3518(7) 0.079(7) Uiso 1 1 d D A . H49 H -0.1805 -0.4979 0.3821 0.095 Uiso 1 1 calc R . . C59 C -0.1369(11) -0.5114(10) 0.3023(6) 0.072(6) Uiso 1 1 d D . . H59 H -0.1958 -0.5251 0.2982 0.087 Uiso 1 1 calc R A . C69 C -0.0603(10) -0.5092(10) 0.2589(6) 0.056(5) Uiso 1 1 d D A . O29 O 0.1185(7) -0.4502(6) 0.3131(4) 0.056(3) Uiso 1 1 d D A . C9M C -0.0596(14) -0.5308(12) 0.2036(6) 0.101(8) Uiso 1 1 d D . . H9M1 H 0.0033 -0.5252 0.1798 0.151 Uiso 1 1 calc R A . H9M2 H -0.1082 -0.4976 0.1875 0.151 Uiso 1 1 calc R . . H9M3 H -0.0734 -0.5836 0.2076 0.151 Uiso 1 1 calc R . . N110 N 0.2434(17) -0.5018(11) 0.3862(9) 0.055(8) Uiso 0.66(2) 1 d PD A 1 H110 H 0.2057 -0.4891 0.3628 0.066 Uiso 0.66(2) 1 calc PR A 1 C210 C 0.3245(18) -0.4677(14) 0.3764(10) 0.057(10) Uiso 0.66(2) 1 d PD A 1 C310 C 0.397(2) -0.4973(19) 0.4057(13) 0.138(18) Uiso 0.66(2) 1 d PD A 1 H310 H 0.4602 -0.4839 0.3947 0.166 Uiso 0.66(2) 1 calc PR A 1 C410 C 0.366(2) -0.5482(19) 0.4524(13) 0.127(17) Uiso 0.66(2) 1 d PD A 1 H410 H 0.4070 -0.5621 0.4776 0.152 Uiso 0.66(2) 1 calc PR A 1 C510 C 0.280(2) -0.5792(17) 0.4636(12) 0.108(15) Uiso 0.66(2) 1 d PD A 1 H510 H 0.2654 -0.6168 0.4940 0.130 Uiso 0.66(2) 1 calc PR A 1 C610 C 0.216(2) -0.5552(17) 0.4302(12) 0.091(14) Uiso 0.66(2) 1 d PD A 1 O210 O 0.3393(15) -0.4161(10) 0.3333(8) 0.064(7) Uiso 0.66(2) 1 d PD A 1 C10M C 0.136(2) -0.5996(18) 0.4267(14) 0.112(14) Uiso 0.66(2) 1 d PD A 1 H10M H 0.1066 -0.5753 0.3965 0.168 Uiso 0.66(2) 1 calc PR A 1 H11M H 0.0883 -0.6006 0.4609 0.168 Uiso 0.66(2) 1 calc PR A 1 H12M H 0.1623 -0.6515 0.4205 0.168 Uiso 0.66(2) 1 calc PR A 1 N11' N 0.202(3) -0.487(2) 0.4013(14) 0.040(14) Uiso 0.34(2) 1 d PD A 2 H11' H 0.1719 -0.4769 0.3742 0.048 Uiso 0.34(2) 1 calc PR A 2 C21' C 0.274(4) -0.445(3) 0.4013(19) 0.08(2) Uiso 0.34(2) 1 d PD A 2 C31' C 0.329(3) -0.465(3) 0.4413(18) 0.08(2) Uiso 0.34(2) 1 d PD A 2 H31' H 0.3864 -0.4422 0.4386 0.096 Uiso 0.34(2) 1 calc PR A 2 C41' C 0.296(4) -0.519(3) 0.4852(17) 0.09(2) Uiso 0.34(2) 1 d PD A 2 H41' H 0.3215 -0.5244 0.5172 0.103 Uiso 0.34(2) 1 calc PR A 2 C51' C 0.228(3) -0.564(2) 0.4824(17) 0.061(19) Uiso 0.34(2) 1 d PD A 2 H51' H 0.2169 -0.6082 0.5077 0.074 Uiso 0.34(2) 1 calc PR A 2 C61' C 0.175(3) -0.544(2) 0.4427(17) 0.07(2) Uiso 0.34(2) 1 d PD A 2 O21' O 0.296(3) -0.3925(19) 0.3590(15) 0.061(14) Uiso 0.34(2) 1 d PD A 2 C1M' C 0.073(3) -0.562(4) 0.451(2) 0.11(3) Uiso 0.34(2) 1 d PD A 2 H1M4 H 0.0483 -0.5431 0.4187 0.167 Uiso 0.34(2) 1 calc PR A 2 H1M5 H 0.0339 -0.5383 0.4824 0.167 Uiso 0.34(2) 1 calc PR A 2 H1M6 H 0.0714 -0.6173 0.4591 0.167 Uiso 0.34(2) 1 calc PR A 2 N1S N 0.4836(17) -0.2861(13) 0.0383(10) 0.151(9) Uiso 1 1 d D . . C2S C 0.4217(18) -0.3247(14) 0.0624(10) 0.105(8) Uiso 1 1 d D . . C3S C 0.3425(14) -0.3612(11) 0.0986(8) 0.083(7) Uiso 1 1 d D . . H3S1 H 0.2895 -0.3228 0.1095 0.124 Uiso 1 1 d R . . H3S2 H 0.3633 -0.3885 0.1311 0.124 Uiso 1 1 d R . . H3S3 H 0.3214 -0.3970 0.0795 0.124 Uiso 1 1 d R . . N1T N 0.527(2) 0.6642(17) 0.4319(12) 0.204(13) Uiso 1 1 d D . . C2T C 0.462(2) 0.702(2) 0.4126(14) 0.185(15) Uiso 1 1 d D . . C3T C 0.3890(19) 0.7344(15) 0.3797(11) 0.140(10) Uiso 1 1 d D . . H3T1 H 0.4169 0.7322 0.3410 0.210 Uiso 1 1 d R . . H3T2 H 0.3689 0.7873 0.3857 0.210 Uiso 1 1 d R . . H3T3 H 0.3336 0.7053 0.3907 0.210 Uiso 1 1 d R . . N1U N 0.237(4) 0.634(3) 0.503(2) 0.17(2) Uiso 0.50 1 d PD . . C2U C 0.292(5) 0.593(5) 0.527(3) 0.26(4) Uiso 0.50 1 d PD . . C3U C 0.368(4) 0.542(3) 0.549(2) 0.18(3) Uiso 0.50 1 d PD . . H3U1 H 0.3515 0.4895 0.5551 0.266 Uiso 0.50 1 d PR . . H3U2 H 0.3734 0.5563 0.5839 0.266 Uiso 0.50 1 d PR . . H3U3 H 0.4294 0.5451 0.5233 0.266 Uiso 0.50 1 d PR . . 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 0.0236(14) 0.0194(13) 0.0357(15) 0.0025(10) -0.0129(11) -0.0058(10) Co2 0.0211(13) 0.0258(13) 0.0340(15) 0.0014(11) -0.0136(11) -0.0056(10) Co3 0.0299(14) 0.0343(14) 0.0326(15) -0.0001(11) -0.0144(11) -0.0046(11) Co4 0.0273(14) 0.0215(13) 0.0349(15) 0.0024(11) -0.0116(11) -0.0066(11) Co5 0.0278(14) 0.0203(13) 0.0357(15) 0.0036(11) -0.0161(11) -0.0056(10) Co6 0.0253(14) 0.0260(14) 0.0348(15) 0.0013(11) -0.0167(11) -0.0069(11) Co7 0.0258(14) 0.0353(15) 0.0398(16) -0.0037(12) -0.0106(12) -0.0084(11) Co8 0.0485(17) 0.0282(14) 0.0536(18) -0.0023(12) -0.0214(13) -0.0090(12) Na1 0.049(4) 0.024(4) 0.051(4) 0.002(3) -0.025(3) -0.013(3) Na2 0.049(5) 0.028(4) 0.046(4) 0.002(3) -0.017(3) -0.012(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 O1B 2.074(10) . ? Co1 O1 2.101(9) . ? Co1 O26 2.102(9) . ? Co1 O21 2.103(9) . ? Co1 O28 2.126(9) . ? Co1 O23 2.149(9) . ? Co1 Na2 3.061(6) . ? Co2 O2B 2.032(9) . ? Co2 O26 2.160(9) . ? Co2 N14 2.173(10) . ? Co2 N15 2.218(10) . ? Co2 O23 2.234(9) . ? Co2 O25 2.246(9) . ? Co3 O1 1.959(9) . ? Co3 O1A 1.988(10) . ? Co3 N11 2.047(11) . ? Co3 N12 2.102(10) . ? Co3 O22 2.303(9) . ? Co4 O24 2.024(10) . ? Co4 O22 2.029(9) . ? Co4 N13 2.078(10) . ? Co4 O1C 2.086(9) . ? Co4 O2 2.105(9) . ? Co4 O23 2.352(9) . ? Co5 O24 2.060(9) . ? Co5 O1D 2.065(9) . ? Co5 O1E 2.067(10) . ? Co5 O2C 2.078(9) . ? Co5 O25 2.079(9) . ? Co5 O2 2.171(9) . ? Co5 Na1 3.278(6) . ? Co6 O27 2.031(9) . ? Co6 O2D 2.050(9) . ? Co6 O2 2.080(8) . ? Co6 N16 2.085(10) . ? Co6 O25 2.142(10) . ? Co6 O26 2.387(9) . ? Co7 O2A 1.995(10) . ? Co7 O1 2.004(9) . ? Co7 N18 2.044(11) . ? Co7 N17 2.051(11) . ? Co7 O27 2.370(9) . ? Co8 O1G 1.977(10) . ? Co8 N19 2.050(12) . ? Co8 O2E 2.055(10) . ? Co8 O1F 2.096(10) . ? Co8 O2F 2.362(10) . ? Co8 O29 2.404(11) . ? Co8 Na1 3.069(6) . ? Na1 O210 2.289(19) . ? Na1 O2E 2.326(12) . ? Na1 O21' 2.37(3) . ? Na1 O2C 2.389(11) . ? Na1 O1D 2.396(10) . ? Na1 O29 2.450(12) . ? Na1 O1F 2.462(11) . ? Na2 O2G 2.265(12) 1_565 ? Na2 O2F 2.298(12) 1_565 ? Na2 O28 2.343(11) . ? Na2 O21 2.371(10) . ? Na2 O1B 2.440(11) . ? O2A C1A 1.236(11) . ? O1A C1A 1.268(11) . ? C1A C2A 1.516(13) . ? C2A C3A 1.492(13) . ? C3A C4A 1.376(14) . ? C3A C8A 1.392(12) . ? C4A C5A 1.401(15) . ? C5A C6A 1.334(15) . ? C6A C7A 1.341(15) . ? C7A C8A 1.397(14) . ? O2B C1B 1.244(11) . ? O1B C1B 1.269(11) . ? C1B C2B 1.512(12) . ? C2B C3B 1.499(12) . ? C3B C4B 1.355(12) . ? C3B C8B 1.409(12) . ? C4B C5B 1.399(13) . ? C5B C6B 1.363(14) . ? C6B C7B 1.336(14) . ? C7B C8B 1.395(14) . ? O1C C1C 1.252(11) . ? O2C C1C 1.258(11) . ? C1C C2C 1.521(12) . ? C2C C3C 1.496(12) . ? C3C C4C 1.370(13) . ? C3C C8C 1.396(12) . ? C4C C5C 1.387(13) . ? C5C C6C 1.344(13) . ? C6C C7C 1.349(14) . ? C7C C8C 1.392(13) . ? O2D C1D 1.253(11) . ? O1D C1D 1.266(11) . ? C1D C2D 1.513(12) . ? C2D C3D 1.502(13) . ? C3D C4D 1.359(12) . ? C3D C8D 1.394(12) . ? C4D C5D 1.396(14) . ? C5D C6D 1.343(14) . ? C6D C7D 1.348(14) . ? C7D C8D 1.402(14) . ? O1E C1E 1.244(11) . ? O2E C1E 1.267(11) . ? C1E C2E 1.503(13) . ? C2E C3E 1.493(12) . ? C3E C4E 1.356(12) . ? C3E C8E 1.410(12) . ? C4E C5E 1.384(13) . ? C5E C6E 1.346(14) . ? C6E C7E 1.330(13) . ? C7E C8E 1.387(13) . ? O2F C1F 1.244(11) . ? O2F Na2 2.298(12) 1_545 ? O1F C1F 1.282(11) . ? C1F C2F 1.500(13) . ? C2F C3F 1.496(12) . ? C3F C4F 1.367(13) . ? C3F C8F 1.400(13) . ? C4F C5F 1.398(14) . ? C5F C6F 1.343(14) . ? C6F C7F 1.331(14) . ? C7F C8F 1.392(13) . ? O2G C1G 1.245(11) . ? O2G Na2 2.265(12) 1_545 ? O1G C1G 1.281(11) . ? C1G C2G 1.498(13) . ? C2G C3G 1.484(13) . ? C3G C4G 1.363(13) . ? C3G C8G 1.399(13) . ? C4G C5G 1.401(13) . ? C5G C6G 1.356(14) . ? C6G C7G 1.325(14) . ? C7G C8G 1.382(14) . ? N11 C21 1.349(11) . ? N11 C61 1.354(11) . ? C21 O21 1.306(10) . ? C21 C31 1.391(12) . ? C31 C41 1.370(12) . ? C41 C51 1.380(12) . ? C51 C61 1.370(12) . ? C61 C1M 1.507(12) . ? N12 C22 1.351(11) . ? N12 C62 1.356(11) . ? C22 O22 1.310(11) . ? C22 C32 1.376(12) . ? C32 C42 1.386(13) . ? C42 C52 1.379(12) . ? C52 C62 1.367(12) . ? C62 C2M 1.493(12) . ? N13 C63 1.343(11) . ? N13 C23 1.355(11) . ? C23 O23 1.318(10) . ? C23 C33 1.397(12) . ? C33 C43 1.374(12) . ? C43 C53 1.370(12) . ? C53 C63 1.370(12) . ? C63 C3M 1.494(12) . ? N14 C24 1.337(10) . ? N14 C64 1.359(11) . ? C24 O24 1.329(10) . ? C24 C34 1.389(11) . ? C34 C44 1.386(12) . ? C44 C54 1.369(12) . ? C54 C64 1.370(12) . ? C64 C4M 1.493(12) . ? N15 C25 1.355(11) . ? N15 C65 1.358(11) . ? C25 O25 1.324(10) . ? C25 C35 1.382(11) . ? C35 C45 1.382(12) . ? C45 C55 1.376(12) . ? C55 C65 1.361(11) . ? C65 C5M 1.491(12) . ? N16 C26 1.338(10) . ? N16 C66 1.356(11) . ? C26 O26 1.315(10) . ? C26 C36 1.402(11) . ? C36 C46 1.372(12) . ? C46 C56 1.376(12) . ? C56 C66 1.373(12) . ? C66 C6M 1.503(12) . ? N17 C27 1.353(11) . ? N17 C67 1.372(11) . ? C27 O27 1.308(11) . ? C27 C37 1.382(12) . ? C37 C47 1.386(13) . ? C47 C57 1.384(13) . ? C57 C67 1.355(12) . ? C67 C7M 1.490(12) . ? N18 C28 1.351(11) . ? N18 C68 1.362(11) . ? C28 O28 1.303(11) . ? C28 C38 1.397(12) . ? C38 C48 1.387(12) . ? C48 C58 1.372(12) . ? C58 C68 1.366(12) . ? C68 C8M 1.487(12) . ? N19 C29 1.351(11) . ? N19 C69 1.362(12) . ? C29 O29 1.314(11) . ? C29 C39 1.388(12) . ? C39 C49 1.389(13) . ? C49 C59 1.367(13) . ? C59 C69 1.362(12) . ? C69 C9M 1.498(13) . ? N110 C210 1.339(13) . ? N110 C610 1.364(13) . ? C210 O210 1.306(13) . ? C210 C310 1.405(14) . ? C310 C410 1.390(14) . ? C410 C510 1.374(14) . ? C510 C610 1.368(14) . ? C610 C10M 1.497(14) . ? N11' C21' 1.348(14) . ? N11' C61' 1.365(14) . ? C21' O21' 1.316(14) . ? C21' C31' 1.394(14) . ? C31' C41' 1.387(15) . ? C41' C51' 1.374(15) . ? C51' C61' 1.363(14) . ? C61' C1M' 1.492(15) . ? N1S C2S 1.19(2) . ? C2S C3S 1.44(2) . ? N1T C2T 1.22(3) . ? C2T C3T 1.48(3) . ? N1U C2U 1.21(3) . ? C2U C3U 1.48(3) . ? 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 O1B Co1 O1 173.9(4) . . ? O1B Co1 O26 94.5(4) . . ? O1 Co1 O26 90.4(4) . . ? O1B Co1 O21 86.1(4) . . ? O1 Co1 O21 89.0(4) . . ? O26 Co1 O21 179.4(4) . . ? O1B Co1 O28 86.7(4) . . ? O1 Co1 O28 88.9(4) . . ? O26 Co1 O28 99.1(3) . . ? O21 Co1 O28 80.9(4) . . ? O1B Co1 O23 94.8(4) . . ? O1 Co1 O23 89.8(4) . . ? O26 Co1 O23 77.5(3) . . ? O21 Co1 O23 102.4(3) . . ? O28 Co1 O23 176.4(3) . . ? O1B Co1 Na2 52.6(3) . . ? O1 Co1 Na2 121.3(3) . . ? O26 Co1 Na2 129.8(3) . . ? O21 Co1 Na2 50.6(3) . . ? O28 Co1 Na2 49.8(3) . . ? O23 Co1 Na2 133.5(3) . . ? O2B Co2 O26 92.4(4) . . ? O2B Co2 N14 96.3(4) . . ? O26 Co2 N14 168.2(4) . . ? O2B Co2 N15 93.8(4) . . ? O26 Co2 N15 92.4(4) . . ? N14 Co2 N15 94.9(4) . . ? O2B Co2 O23 90.9(3) . . ? O26 Co2 O23 74.5(3) . . ? N14 Co2 O23 97.3(4) . . ? N15 Co2 O23 166.4(4) . . ? O2B Co2 O25 151.9(3) . . ? O26 Co2 O25 79.6(3) . . ? N14 Co2 O25 96.1(4) . . ? N15 Co2 O25 60.1(3) . . ? O23 Co2 O25 112.3(3) . . ? O1 Co3 O1A 103.4(4) . . ? O1 Co3 N11 121.0(4) . . ? O1A Co3 N11 95.3(4) . . ? O1 Co3 N12 104.6(4) . . ? O1A Co3 N12 102.5(4) . . ? N11 Co3 N12 125.1(4) . . ? O1 Co3 O22 81.7(3) . . ? O1A Co3 O22 162.8(4) . . ? N11 Co3 O22 96.0(4) . . ? N12 Co3 O22 60.4(3) . . ? O24 Co4 O22 173.3(4) . . ? O24 Co4 N13 90.5(4) . . ? O22 Co4 N13 89.8(4) . . ? O24 Co4 O1C 89.5(4) . . ? O22 Co4 O1C 96.8(4) . . ? N13 Co4 O1C 108.4(4) . . ? O24 Co4 O2 81.6(4) . . ? O22 Co4 O2 95.4(4) . . ? N13 Co4 O2 155.6(4) . . ? O1C Co4 O2 94.6(4) . . ? O24 Co4 O23 81.3(3) . . ? O22 Co4 O23 93.0(3) . . ? N13 Co4 O23 60.2(3) . . ? O1C Co4 O23 165.1(4) . . ? O2 Co4 O23 95.6(3) . . ? O24 Co5 O1D 174.5(4) . . ? O24 Co5 O1E 89.3(4) . . ? O1D Co5 O1E 96.1(4) . . ? O24 Co5 O2C 92.8(4) . . ? O1D Co5 O2C 86.6(4) . . ? O1E Co5 O2C 94.7(4) . . ? O24 Co5 O25 82.0(3) . . ? O1D Co5 O25 97.8(4) . . ? O1E Co5 O25 92.8(4) . . ? O2C Co5 O25 170.9(4) . . ? O24 Co5 O2 79.2(4) . . ? O1D Co5 O2 95.4(4) . . ? O1E Co5 O2 166.3(4) . . ? O2C Co5 O2 93.3(4) . . ? O25 Co5 O2 78.3(3) . . ? O24 Co5 Na1 135.0(3) . . ? O1D Co5 Na1 46.8(3) . . ? O1E Co5 Na1 77.9(3) . . ? O2C Co5 Na1 46.6(3) . . ? O25 Co5 Na1 140.7(3) . . ? O2 Co5 Na1 115.6(3) . . ? O27 Co6 O2D 98.6(4) . . ? O27 Co6 O2 97.7(4) . . ? O2D Co6 O2 95.9(4) . . ? O27 Co6 N16 87.7(4) . . ? O2D Co6 N16 105.3(4) . . ? O2 Co6 N16 157.0(4) . . ? O27 Co6 O25 165.5(4) . . ? O2D Co6 O25 95.8(4) . . ? O2 Co6 O25 78.9(4) . . ? N16 Co6 O25 90.2(4) . . ? O27 Co6 O26 89.8(3) . . ? O2D Co6 O26 162.3(4) . . ? O2 Co6 O26 98.4(3) . . ? N16 Co6 O26 59.2(3) . . ? O25 Co6 O26 76.8(3) . . ? O2A Co7 O1 101.2(4) . . ? O2A Co7 N18 98.5(4) . . ? O1 Co7 N18 125.7(4) . . ? O2A Co7 N17 104.5(4) . . ? O1 Co7 N17 105.6(4) . . ? N18 Co7 N17 117.5(4) . . ? O2A Co7 O27 162.3(4) . . ? O1 Co7 O27 78.6(3) . . ? N18 Co7 O27 95.8(4) . . ? N17 Co7 O27 59.2(3) . . ? O1G Co8 N19 115.0(5) . . ? O1G Co8 O2E 99.1(4) . . ? N19 Co8 O2E 103.5(5) . . ? O1G Co8 O1F 99.5(4) . . ? N19 Co8 O1F 141.3(5) . . ? O2E Co8 O1F 87.1(4) . . ? O1G Co8 O2F 95.9(4) . . ? N19 Co8 O2F 99.0(4) . . ? O2E Co8 O2F 144.4(4) . . ? O1F Co8 O2F 58.5(3) . . ? O1G Co8 O29 174.7(4) . . ? N19 Co8 O29 59.8(4) . . ? O2E Co8 O29 81.9(4) . . ? O1F Co8 O29 85.7(4) . . ? O2F Co8 O29 86.1(4) . . ? O1G Co8 Na1 132.8(3) . . ? N19 Co8 Na1 107.1(4) . . ? O2E Co8 Na1 49.3(3) . . ? O1F Co8 Na1 53.0(3) . . ? O2F Co8 Na1 97.8(3) . . ? O29 Co8 Na1 51.4(3) . . ? O210 Na1 O2E 158.2(6) . . ? O210 Na1 O21' 22.2(9) . . ? O2E Na1 O21' 163.9(8) . . ? O210 Na1 O2C 109.8(7) . . ? O2E Na1 O2C 90.9(4) . . ? O21' Na1 O2C 89.5(11) . . ? O210 Na1 O1D 105.2(5) . . ? O2E Na1 O1D 86.9(4) . . ? O21' Na1 O1D 108.6(7) . . ? O2C Na1 O1D 72.9(3) . . ? O210 Na1 O29 93.8(5) . . ? O2E Na1 O29 75.7(4) . . ? O21' Na1 O29 88.3(7) . . ? O2C Na1 O29 99.1(4) . . ? O1D Na1 O29 160.9(4) . . ? O210 Na1 O1F 85.8(7) . . ? O2E Na1 O1F 73.3(4) . . ? O21' Na1 O1F 105.6(11) . . ? O2C Na1 O1F 164.3(5) . . ? O1D Na1 O1F 105.5(4) . . ? O29 Na1 O1F 77.3(4) . . ? O210 Na1 Co8 116.9(5) . . ? O2E Na1 Co8 42.0(3) . . ? O21' Na1 Co8 126.9(8) . . ? O2C Na1 Co8 123.7(3) . . ? O1D Na1 Co8 119.5(3) . . ? O29 Na1 Co8 50.1(3) . . ? O1F Na1 Co8 42.8(3) . . ? O210 Na1 Co5 127.1(5) . . ? O2E Na1 Co5 73.4(3) . . ? O21' Na1 Co5 115.8(9) . . ? O2C Na1 Co5 39.2(2) . . ? O1D Na1 Co5 38.9(2) . . ? O29 Na1 Co5 125.7(3) . . ? O1F Na1 Co5 131.7(3) . . ? Co8 Na1 Co5 115.5(2) . . ? O2G Na2 O2F 84.4(4) 1_565 1_565 ? O2G Na2 O28 120.6(4) 1_565 . ? O2F Na2 O28 109.7(4) 1_565 . ? O2G Na2 O21 157.3(5) 1_565 . ? O2F Na2 O21 110.8(4) 1_565 . ? O28 Na2 O21 71.2(3) . . ? O2G Na2 O1B 91.4(4) 1_565 . ? O2F Na2 O1B 175.3(5) 1_565 . ? O28 Na2 O1B 74.1(4) . . ? O21 Na2 O1B 72.7(4) . . ? O2G Na2 Co1 130.2(4) 1_565 . ? O2F Na2 Co1 142.2(4) 1_565 . ? O28 Na2 Co1 43.9(2) . . ? O21 Na2 Co1 43.3(2) . . ? O1B Na2 Co1 42.5(2) . . ? Co3 O1 Co7 117.2(5) . . ? Co3 O1 Co1 107.0(4) . . ? Co7 O1 Co1 104.1(4) . . ? Co6 O2 Co4 135.8(5) . . ? Co6 O2 Co5 92.9(4) . . ? Co4 O2 Co5 92.2(4) . . ? C1A O2A Co7 135.3(9) . . ? C1A O1A Co3 132.8(9) . . ? O2A C1A O1A 125.4(12) . . ? O2A C1A C2A 120.6(11) . . ? O1A C1A C2A 114.0(11) . . ? C3A C2A C1A 113.5(11) . . ? C4A C3A C8A 117.0(13) . . ? C4A C3A C2A 120.2(13) . . ? C8A C3A C2A 122.8(13) . . ? C3A C4A C5A 118.7(15) . . ? C6A C5A C4A 122.0(17) . . ? C5A C6A C7A 121.2(17) . . ? C6A C7A C8A 117.7(15) . . ? C3A C8A C7A 122.8(13) . . ? C1B O2B Co2 134.0(9) . . ? C1B O1B Co1 127.2(8) . . ? C1B O1B Na2 147.6(8) . . ? Co1 O1B Na2 85.0(4) . . ? O2B C1B O1B 126.7(11) . . ? O2B C1B C2B 117.6(11) . . ? O1B C1B C2B 115.6(11) . . ? C3B C2B C1B 113.3(10) . . ? C4B C3B C8B 116.8(11) . . ? C4B C3B C2B 125.1(11) . . ? C8B C3B C2B 118.0(10) . . ? C3B C4B C5B 122.9(13) . . ? C6B C5B C4B 118.6(14) . . ? C7B C6B C5B 120.5(14) . . ? C6B C7B C8B 121.2(15) . . ? C7B C8B C3B 119.8(12) . . ? C1C O1C Co4 129.5(8) . . ? C1C O2C Co5 126.5(8) . . ? C1C O2C Na1 139.0(8) . . ? Co5 O2C Na1 94.1(4) . . ? O1C C1C O2C 125.9(11) . . ? O1C C1C C2C 117.0(11) . . ? O2C C1C C2C 117.1(11) . . ? C3C C2C C1C 112.1(11) . . ? C4C C3C C8C 117.9(11) . . ? C4C C3C C2C 122.6(11) . . ? C8C C3C C2C 119.3(11) . . ? C3C C4C C5C 120.7(13) . . ? C6C C5C C4C 120.1(14) . . ? C5C C6C C7C 121.3(14) . . ? C6C C7C C8C 119.5(14) . . ? C7C C8C C3C 120.4(12) . . ? C1D O2D Co6 130.9(8) . . ? C1D O1D Co5 128.3(8) . . ? C1D O1D Na1 133.7(9) . . ? Co5 O1D Na1 94.3(4) . . ? O2D C1D O1D 124.7(11) . . ? O2D C1D C2D 118.7(11) . . ? O1D C1D C2D 116.6(11) . . ? C3D C2D C1D 115.6(11) . . ? C4D C3D C8D 118.1(12) . . ? C4D C3D C2D 122.8(12) . . ? C8D C3D C2D 119.0(12) . . ? C3D C4D C5D 120.7(13) . . ? C6D C5D C4D 120.1(14) . . ? C5D C6D C7D 121.5(15) . . ? C6D C7D C8D 119.0(14) . . ? C3D C8D C7D 120.5(12) . . ? C1E O1E Co5 135.9(9) . . ? C1E O2E Co8 140.8(9) . . ? C1E O2E Na1 128.1(9) . . ? Co8 O2E Na1 88.7(4) . . ? O1E C1E O2E 122.1(12) . . ? O1E C1E C2E 117.0(11) . . ? O2E C1E C2E 120.9(11) . . ? C3E C2E C1E 112.5(11) . . ? C4E C3E C8E 118.4(11) . . ? C4E C3E C2E 121.8(12) . . ? C8E C3E C2E 119.6(11) . . ? C3E C4E C5E 121.5(13) . . ? C6E C5E C4E 119.1(14) . . ? C7E C6E C5E 121.4(15) . . ? C6E C7E C8E 121.2(14) . . ? C7E C8E C3E 118.3(12) . . ? C1F O2F Na2 143.0(10) . 1_545 ? C1F O2F Co8 84.7(8) . . ? Na2 O2F Co8 112.1(5) 1_545 . ? C1F O1F Co8 95.9(8) . . ? C1F O1F Na1 135.3(10) . . ? Co8 O1F Na1 84.3(4) . . ? O2F C1F O1F 120.4(12) . . ? O2F C1F C2F 121.2(12) . . ? O1F C1F C2F 118.4(11) . . ? C3F C2F C1F 115.2(11) . . ? C4F C3F C8F 118.3(12) . . ? C4F C3F C2F 123.4(13) . . ? C8F C3F C2F 118.2(12) . . ? C3F C4F C5F 120.7(14) . . ? C6F C5F C4F 118.5(14) . . ? C7F C6F C5F 123.1(14) . . ? C6F C7F C8F 119.1(14) . . ? C7F C8F C3F 119.9(13) . . ? C1G O2G Na2 145.3(11) . 1_545 ? C1G O1G Co8 132.4(9) . . ? O2G C1G O1G 121.9(12) . . ? O2G C1G C2G 120.9(12) . . ? O1G C1G C2G 117.1(11) . . ? C3G C2G C1G 115.7(12) . . ? C4G C3G C8G 116.3(12) . . ? C4G C3G C2G 124.9(13) . . ? C8G C3G C2G 118.8(13) . . ? C3G C4G C5G 122.1(13) . . ? C6G C5G C4G 119.0(14) . . ? C7G C6G C5G 120.1(15) . . ? C6G C7G C8G 121.5(15) . . ? C7G C8G C3G 120.5(13) . . ? C21 N11 C61 120.4(10) . . ? C21 N11 Co3 109.2(8) . . ? C61 N11 Co3 128.7(9) . . ? O21 C21 N11 116.9(10) . . ? O21 C21 C31 123.0(11) . . ? N11 C21 C31 120.2(10) . . ? C41 C31 C21 118.6(11) . . ? C31 C41 C51 121.3(12) . . ? C61 C51 C41 117.9(12) . . ? N11 C61 C51 121.5(11) . . ? N11 C61 C1M 116.0(10) . . ? C51 C61 C1M 122.5(11) . . ? C21 O21 Co1 137.6(9) . . ? C21 O21 Na2 128.3(8) . . ? Co1 O21 Na2 86.1(3) . . ? C22 N12 C62 121.4(10) . . ? C22 N12 Co3 97.1(7) . . ? C62 N12 Co3 141.0(8) . . ? O22 C22 N12 113.1(10) . . ? O22 C22 C32 125.5(11) . . ? N12 C22 C32 121.3(11) . . ? C22 C32 C42 117.0(12) . . ? C52 C42 C32 121.3(13) . . ? C62 C52 C42 119.6(12) . . ? N12 C62 C52 119.2(11) . . ? N12 C62 C2M 117.5(11) . . ? C52 C62 C2M 123.2(12) . . ? C22 O22 Co4 134.3(8) . . ? C22 O22 Co3 89.3(7) . . ? Co4 O22 Co3 130.0(4) . . ? C63 N13 C23 119.7(10) . . ? C63 N13 Co4 141.6(8) . . ? C23 N13 Co4 98.6(7) . . ? O23 C23 N13 113.6(10) . . ? O23 C23 C33 124.2(10) . . ? N13 C23 C33 122.2(10) . . ? C43 C33 C23 116.8(11) . . ? C53 C43 C33 120.3(12) . . ? C43 C53 C63 120.8(12) . . ? N13 C63 C53 120.0(10) . . ? N13 C63 C3M 116.0(10) . . ? C53 C63 C3M 124.0(11) . . ? C23 O23 Co1 122.6(8) . . ? C23 O23 Co2 123.2(9) . . ? Co1 O23 Co2 95.2(3) . . ? C23 O23 Co4 87.5(6) . . ? Co1 O23 Co4 127.3(4) . . ? Co2 O23 Co4 102.2(3) . . ? C24 N14 C64 119.4(10) . . ? C24 N14 Co2 105.6(7) . . ? C64 N14 Co2 134.6(8) . . ? O24 C24 N14 117.2(10) . . ? O24 C24 C34 120.6(10) . . ? N14 C24 C34 122.1(10) . . ? C44 C34 C24 117.3(11) . . ? C54 C44 C34 120.5(12) . . ? C44 C54 C64 119.4(12) . . ? N14 C64 C54 120.9(11) . . ? N14 C64 C4M 117.5(11) . . ? C54 C64 C4M 121.4(12) . . ? C24 O24 Co4 134.4(9) . . ? C24 O24 Co5 127.4(9) . . ? Co4 O24 Co5 97.9(4) . . ? C25 N15 C65 119.7(9) . . ? C25 N15 Co2 93.1(7) . . ? C65 N15 Co2 146.9(8) . . ? O25 C25 N15 113.2(10) . . ? O25 C25 C35 125.6(11) . . ? N15 C25 C35 121.2(10) . . ? C45 C35 C25 118.6(11) . . ? C55 C45 C35 119.6(12) . . ? C65 C55 C45 120.2(12) . . ? N15 C65 C55 120.6(10) . . ? N15 C65 C5M 116.2(10) . . ? C55 C65 C5M 123.0(11) . . ? C25 O25 Co5 130.9(8) . . ? C25 O25 Co6 121.8(8) . . ? Co5 O25 Co6 93.7(4) . . ? C25 O25 Co2 92.7(7) . . ? Co5 O25 Co2 113.6(4) . . ? Co6 O25 Co2 101.6(4) . . ? C26 N16 C66 121.6(9) . . ? C26 N16 Co6 99.9(7) . . ? C66 N16 Co6 138.5(8) . . ? O26 C26 N16 113.9(9) . . ? O26 C26 C36 125.8(10) . . ? N16 C26 C36 120.3(10) . . ? C46 C36 C26 117.3(11) . . ? C36 C46 C56 122.3(12) . . ? C66 C56 C46 118.1(11) . . ? N16 C66 C56 120.3(10) . . ? N16 C66 C6M 116.7(10) . . ? C56 C66 C6M 122.7(11) . . ? C26 O26 Co1 128.5(8) . . ? C26 O26 Co2 116.7(9) . . ? Co1 O26 Co2 98.8(3) . . ? C26 O26 Co6 87.0(6) . . ? Co1 O26 Co6 126.3(4) . . ? Co2 O26 Co6 96.7(3) . . ? C27 N17 C67 119.4(10) . . ? C27 N17 Co7 101.0(7) . . ? C67 N17 Co7 139.5(8) . . ? O27 C27 N17 111.7(10) . . ? O27 C27 C37 126.1(11) . . ? N17 C27 C37 122.1(11) . . ? C27 C37 C47 117.7(12) . . ? C57 C47 C37 120.0(13) . . ? C67 C57 C47 120.4(13) . . ? C57 C67 N17 120.3(11) . . ? C57 C67 C7M 123.7(12) . . ? N17 C67 C7M 116.0(11) . . ? C27 O27 Co6 135.8(8) . . ? C27 O27 Co7 87.8(7) . . ? Co6 O27 Co7 130.7(4) . . ? C28 N18 C68 120.1(10) . . ? C28 N18 Co7 106.4(8) . . ? C68 N18 Co7 133.0(8) . . ? O28 C28 N18 117.0(11) . . ? O28 C28 C38 120.8(11) . . ? N18 C28 C38 121.6(11) . . ? C48 C38 C28 116.5(11) . . ? C58 C48 C38 121.0(12) . . ? C68 C58 C48 120.2(12) . . ? N18 C68 C58 119.8(10) . . ? N18 C68 C8M 116.9(10) . . ? C58 C68 C8M 123.3(11) . . ? C28 O28 Co1 136.9(9) . . ? C28 O28 Na2 125.6(8) . . ? Co1 O28 Na2 86.3(4) . . ? C29 N19 C69 119.8(11) . . ? C29 N19 Co8 99.9(8) . . ? C69 N19 Co8 139.7(9) . . ? O29 C29 N19 114.6(12) . . ? O29 C29 C39 123.6(12) . . ? N19 C29 C39 121.7(12) . . ? C29 C39 C49 117.2(13) . . ? C59 C49 C39 120.7(14) . . ? C69 C59 C49 120.1(14) . . ? C59 C69 N19 120.4(12) . . ? C59 C69 C9M 124.9(13) . . ? N19 C69 C9M 114.7(12) . . ? C29 O29 Co8 85.3(8) . . ? C29 O29 Na1 145.9(10) . . ? Co8 O29 Na1 78.4(3) . . ? C210 N110 C610 124.3(15) . . ? O210 C210 N110 117.0(16) . . ? O210 C210 C310 122.2(17) . . ? N110 C210 C310 119.7(15) . . ? C410 C310 C210 114.2(16) . . ? C510 C410 C310 123.5(18) . . ? C610 C510 C410 119.7(17) . . ? N110 C610 C510 116.8(16) . . ? N110 C610 C10M 115.7(17) . . ? C510 C610 C10M 124.2(18) . . ? C210 O210 Na1 130.5(13) . . ? C21' N11' C61' 121.8(17) . . ? O21' C21' N11' 117.1(19) . . ? O21' C21' C31' 122(2) . . ? N11' C21' C31' 120.3(17) . . ? C41' C31' C21' 116.8(18) . . ? C51' C41' C31' 120.5(19) . . ? C61' C51' C41' 119.7(19) . . ? C51' C61' N11' 118.7(17) . . ? C51' C61' C1M' 122(2) . . ? N11' C61' C1M' 116(2) . . ? C21' O21' Na1 131.9(19) . . ? N1S C2S C3S 169(3) . . ? N1T C2T C3T 167(4) . . ? N1U C2U C3U 172(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 20.04 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.565 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.112 data_phtaco _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C119 H76 Cl26 Co13 N20 O30' _chemical_formula_weight 3953.79 _chemical_melting_point ? _chemical_compound_source ? 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 17.165(5) _cell_length_b 18.243(7) _cell_length_c 26.613(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.63(4) _cell_angle_gamma 90.00 _cell_volume 8277.9(47) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description lath _exptl_crystal_colour Purple _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method ? _exptl_crystal_F_000 3926 _exptl_absorpt_coefficient_mu 1.753 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.453 _exptl_absorpt_correction_T_max 0.742 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method 'omega with learnt profile' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11996 _diffrn_reflns_av_R_equivalents 0.2207 _diffrn_reflns_av_sigmaI/netI 0.1626 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 22.59 _reflns_number_total 10866 _reflns_number_observed 5657 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 119 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+132.5922P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10747 _refine_ls_number_parameters 961 _refine_ls_number_restraints 1672 _refine_ls_R_factor_all 0.1881 _refine_ls_R_factor_obs 0.0926 _refine_ls_wR_factor_all 0.2744 _refine_ls_wR_factor_obs 0.2013 _refine_ls_goodness_of_fit_all 1.021 _refine_ls_goodness_of_fit_obs 1.120 _refine_ls_restrained_S_all 1.007 _refine_ls_restrained_S_obs 0.992 _refine_ls_shift/esd_max 0.018 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.5000 0.5000 0.0000 0.0228(7) Uani 1 d SU . Co2 Co 0.48915(11) 0.69975(11) 0.08733(8) 0.0260(5) Uani 1 d U . Co3 Co 0.38580(11) 0.71383(11) -0.03405(8) 0.0266(5) Uani 1 d U . Co4 Co 0.35465(11) 0.58474(11) 0.04424(7) 0.0225(5) Uani 1 d U . Co5 Co 0.28721(11) 0.71361(11) 0.14330(8) 0.0271(5) Uani 1 d U . Co6 Co 0.18788(11) 0.72425(11) 0.02953(8) 0.0275(5) Uani 1 d U . Co7 Co 0.14124(12) 0.85086(13) 0.12393(8) 0.0353(6) Uani 1 d U . O1 O 0.3883(5) 0.6971(5) 0.0398(3) 0.023(2) Uani 1 d U . H1 H 0.3482(5) 0.7289(5) 0.0535(3) 0.028 Uiso 1 calc R . N11 N 0.5268(6) 0.6150(4) 0.1370(3) 0.026(2) Uani 1 d DU . C21 C 0.5572(8) 0.6101(4) 0.1859(3) 0.031(3) Uani 1 d DU . C31 C 0.5696(8) 0.5456(4) 0.2119(3) 0.031(3) Uani 1 d DU . H31 H 0.5945(8) 0.5445(4) 0.2457(3) 0.037 Uiso 1 calc R . C41 C 0.5440(8) 0.4822(5) 0.1865(4) 0.036(3) Uani 1 d DU . H41 H 0.5477(8) 0.4367(5) 0.2040(4) 0.044 Uiso 1 calc R . C51 C 0.5133(8) 0.4841(4) 0.1368(4) 0.034(3) Uani 1 d DU . H51 H 0.4983(8) 0.4401(4) 0.1192(4) 0.040 Uiso 1 calc R . C61 C 0.5045(8) 0.5525(5) 0.1121(3) 0.028(3) Uani 1 d DU . O61 O 0.4764(5) 0.5613(4) 0.0649(2) 0.025(2) Uani 1 d DU . Cl1 Cl 0.5855(3) 0.6924(2) 0.2157(2) 0.0476(12) Uani 1 d DU . N12 N 0.2726(6) 0.6188(4) 0.1860(3) 0.032(2) Uani 1 d DU . C22 C 0.2338(8) 0.5893(5) 0.2222(4) 0.037(3) Uani 1 d DU . C32 C 0.2225(9) 0.5160(5) 0.2285(5) 0.047(4) Uani 1 d DU . H32 H 0.1919(9) 0.4978(5) 0.2533(5) 0.057 Uiso 1 calc R . C42 C 0.2577(9) 0.4694(5) 0.1967(5) 0.042(4) Uani 1 d DU . H42 H 0.2550(9) 0.4178(5) 0.2015(5) 0.050 Uiso 1 calc R . C52 C 0.2964(8) 0.4965(4) 0.1586(4) 0.036(3) Uani 1 d DU . H52 H 0.3201(8) 0.4644(4) 0.1368(4) 0.044 Uiso 1 calc R . C62 C 0.3004(7) 0.5730(5) 0.1522(4) 0.028(3) Uani 1 d DU . O62 O 0.3305(5) 0.6062(4) 0.1159(3) 0.031(2) Uani 1 d DU . Cl2 Cl 0.1947(3) 0.6520(3) 0.2618(2) 0.0546(13) Uani 1 d DU . N13 N 0.1159(4) 0.6378(4) -0.0052(5) 0.035(3) Uani 1 d DU . C23 C 0.0452(5) 0.6136(6) -0.0252(7) 0.050(4) Uani 1 d DU . C33 C 0.0309(5) 0.5456(6) -0.0458(7) 0.058(5) Uani 1 d DU . H33 H -0.0200(5) 0.5313(6) -0.0603(7) 0.069 Uiso 1 calc R . C43 C 0.0945(6) 0.4985(6) -0.0444(7) 0.058(5) Uani 1 d DU . H43 H 0.0875(6) 0.4509(6) -0.0588(7) 0.069 Uiso 1 calc R . C53 C 0.1674(5) 0.5194(5) -0.0227(5) 0.037(3) Uani 1 d DU . H53 H 0.2103(5) 0.4862(5) -0.0208(5) 0.045 Uiso 1 calc R . C63 C 0.1774(5) 0.5909(5) -0.0031(6) 0.036(3) Uani 1 d DU . O63 O 0.2435(4) 0.6188(5) 0.0168(4) 0.030(2) Uani 1 d DU . Cl3 Cl -0.0324(2) 0.6742(3) -0.0212(3) 0.080(2) Uani 1 d DU . N14 N 0.3386(6) 0.6391(4) -0.0875(3) 0.035(3) Uani 1 d DU . C24 C 0.2933(10) 0.6435(5) -0.1320(5) 0.058(5) Uani 1 d DU . C34 C 0.2593(11) 0.5847(5) -0.1580(5) 0.064(5) Uani 1 d DU . H34 H 0.2272(11) 0.5904(5) -0.1893(5) 0.077 Uiso 1 calc R . C44 C 0.2743(9) 0.5163(5) -0.1362(5) 0.049(4) Uani 1 d DU . H44 H 0.2498(9) 0.4742(5) -0.1520(5) 0.059 Uiso 1 calc R . C54 C 0.3237(7) 0.5084(4) -0.0924(4) 0.031(3) Uani 1 d DU . H54 H 0.3355(7) 0.4611(4) -0.0786(4) 0.038 Uiso 1 calc R . C64 C 0.3566(7) 0.5717(4) -0.0682(3) 0.026(3) Uani 1 d DU . O64 O 0.4018(5) 0.5716(4) -0.0255(3) 0.023(2) Uani 1 d DU . Cl4 Cl 0.2781(5) 0.7314(3) -0.1573(2) 0.100(2) Uani 1 d DU . N15 N 0.4958(5) 0.8008(4) 0.1237(3) 0.027(2) Uani 1 d DU . C25 C 0.5369(7) 0.8635(5) 0.1229(5) 0.036(3) Uani 1 d DU . C35 C 0.5263(8) 0.9234(6) 0.1521(5) 0.047(4) Uani 1 d DU . H35 H 0.5571(8) 0.9664(6) 0.1504(5) 0.057 Uiso 1 calc R . C45 C 0.4683(8) 0.9188(6) 0.1841(5) 0.046(4) Uani 1 d DU . H45 H 0.4580(8) 0.9599(6) 0.2043(5) 0.056 Uiso 1 calc R . C55 C 0.4257(8) 0.8558(6) 0.1872(5) 0.042(4) Uani 1 d DU . H55 H 0.3868(8) 0.8525(6) 0.2097(5) 0.050 Uiso 1 calc R . C65 C 0.4406(6) 0.7963(5) 0.1562(4) 0.029(3) Uani 1 d DU . O65 O 0.4035(5) 0.7339(4) 0.1544(4) 0.033(2) Uani 1 d DU . Cl5 Cl 0.6068(3) 0.8660(2) 0.0804(2) 0.0565(13) Uani 1 d DU . N16 N 0.1662(6) 0.8892(6) 0.2019(3) 0.043(3) Uani 1 d DU . C26 C 0.1531(8) 0.9371(7) 0.2384(4) 0.049(4) Uani 1 d DU . C36 C 0.1899(9) 0.9358(8) 0.2867(4) 0.061(5) Uani 1 d DU . H36 H 0.1785(9) 0.9709(8) 0.3112(4) 0.073 Uiso 1 calc R . C46 C 0.2444(9) 0.8806(8) 0.2983(4) 0.054(5) Uani 1 d DU . H46 H 0.2704(9) 0.8769(8) 0.3317(4) 0.065 Uiso 1 calc R . C56 C 0.2614(8) 0.8314(7) 0.2625(3) 0.048(4) Uani 1 d DU . H56 H 0.2988(8) 0.7936(7) 0.2707(3) 0.058 Uiso 1 calc R . C66 C 0.2224(8) 0.8377(7) 0.2131(3) 0.039(4) Uani 1 d DU . O66 O 0.2348(5) 0.7958(5) 0.1753(3) 0.034(2) Uani 1 d DU . Cl6 Cl 0.0828(3) 1.0041(3) 0.2211(2) 0.086(2) Uani 1 d DU . N17 N 0.2429(5) 0.8997(4) 0.0955(4) 0.028(2) Uani 1 d DU . C27 C 0.2571(6) 0.9725(4) 0.0971(6) 0.037(4) Uani 1 d DU . C37 C 0.3190(7) 1.0056(5) 0.0781(6) 0.044(4) Uani 1 d DU . H37 H 0.3248(7) 1.0574(5) 0.0782(6) 0.053 Uiso 1 calc R . C47 C 0.3728(7) 0.9600(5) 0.0588(7) 0.048(4) Uani 1 d DU . H47 H 0.4182(7) 0.9805(5) 0.0471(7) 0.058 Uiso 1 calc R . C57 C 0.3615(6) 0.8861(5) 0.0565(5) 0.032(3) Uani 1 d DU . H57 H 0.3975(6) 0.8554(5) 0.0420(5) 0.039 Uiso 1 calc R . C67 C 0.2954(6) 0.8559(4) 0.0760(5) 0.028(3) Uani 1 d DU . O67 O 0.2814(5) 0.7857(3) 0.0764(3) 0.024(2) Uani 1 d DU . Cl7 Cl 0.1884(3) 1.0270(2) 0.1230(2) 0.0516(12) Uani 1 d DU . N18 N 0.3432(4) 0.8183(4) -0.0529(4) 0.027(3) Uani 1 d DU . C28 C 0.3707(5) 0.8823(5) -0.0688(6) 0.036(4) Uani 1 d DU . C38 C 0.3266(5) 0.9439(5) -0.0791(6) 0.045(4) Uani 1 d DU . H38 H 0.3483(5) 0.9874(5) -0.0913(6) 0.054 Uiso 1 calc R . C48 C 0.2484(6) 0.9399(6) -0.0708(7) 0.049(4) Uani 1 d DU . H48 H 0.2157(6) 0.9817(6) -0.0769(7) 0.059 Uiso 1 calc R . C58 C 0.2176(5) 0.8765(5) -0.0541(6) 0.038(4) Uani 1 d DU . H58 H 0.1639(5) 0.8739(5) -0.0488(6) 0.045 Uiso 1 calc R . C68 C 0.2669(5) 0.8151(5) -0.0447(5) 0.030(3) Uani 1 d DU . O68 O 0.2441(5) 0.7510(4) -0.0307(4) 0.033(2) Uani 1 d DU . Cl8 Cl 0.4700(2) 0.8836(2) -0.0770(2) 0.0610(15) Uani 1 d DU . N19 N 0.0811(5) 0.7483(4) 0.1378(4) 0.042(3) Uani 1 d DU . C29 C 0.0162(7) 0.7448(5) 0.1618(6) 0.051(4) Uani 1 d DU . C39 C -0.0210(7) 0.6814(5) 0.1723(7) 0.067(5) Uani 1 d DU . H39 H -0.0671(7) 0.6818(5) 0.1889(7) 0.080 Uiso 1 calc R . C49 C 0.0115(8) 0.6166(5) 0.1576(7) 0.063(5) Uani 1 d DU . H49 H -0.0123(8) 0.5713(5) 0.1645(7) 0.076 Uiso 1 calc R . C59 C 0.0773(7) 0.6168(5) 0.1333(6) 0.050(4) Uani 1 d DU . H59 H 0.0990(7) 0.5721(5) 0.1230(6) 0.060 Uiso 1 calc R . C69 C 0.1125(6) 0.6846(5) 0.1237(5) 0.034(3) Uani 1 d DU . O69 O 0.1780(4) 0.6900(4) 0.1035(3) 0.029(2) Uani 1 d DU . Cl9 Cl -0.0217(3) 0.8283(3) 0.1795(2) 0.071(2) Uani 1 d DU . N110 N 0.0440(5) 0.8959(6) 0.0710(3) 0.040(3) Uani 1 d DU . C210 C -0.0203(7) 0.9383(7) 0.0623(4) 0.044(4) Uani 1 d DU . C310 C -0.0688(7) 0.9404(8) 0.0178(4) 0.047(4) Uani 1 d DU . H310 H -0.1133(7) 0.9716(8) 0.0135(4) 0.057 Uiso 1 calc R . C410 C -0.0499(7) 0.8946(8) -0.0206(4) 0.052(4) Uani 1 d DU . H410 H -0.0834(7) 0.8923(8) -0.0515(4) 0.062 Uiso 1 calc R . C510 C 0.0165(6) 0.8526(7) -0.0143(3) 0.040(4) Uani 1 d DU . H510 H 0.0318(6) 0.8246(7) -0.0416(3) 0.048 Uiso 1 calc R . C610 C 0.0620(6) 0.8516(7) 0.0333(3) 0.036(3) Uani 1 d DU . O610 O 0.1242(4) 0.8115(5) 0.0445(3) 0.030(2) Uani 1 d DU . Cl10 Cl -0.0390(3) 0.9950(3) 0.1122(2) 0.0634(14) Uani 1 d DU . O1P O 0.4251(5) 0.4215(5) 0.0182(4) 0.029(2) Uani 1 d U . O2P O 0.3214(6) 0.4785(5) 0.0459(4) 0.030(2) Uani 1 d U . C1P C 0.3594(8) 0.4206(8) 0.0350(5) 0.024(3) Uani 1 d U . C2P C 0.3233(8) 0.3498(8) 0.0444(6) 0.028(3) Uani 1 d U . C3P C 0.2543(8) 0.3437(8) 0.0642(5) 0.026(3) Uani 1 d U . H3P H 0.2275(8) 0.3870(8) 0.0719(5) 0.031 Uiso 1 calc R . C4P C 0.2208(9) 0.2743(8) 0.0737(6) 0.038(4) Uani 1 d U . H4P H 0.1730(9) 0.2709(8) 0.0883(6) 0.046 Uiso 1 calc R . C5P C 0.2607(9) 0.2115(9) 0.0607(7) 0.047(4) Uani 1 d U . H5P H 0.2395(9) 0.1646(9) 0.0667(7) 0.056 Uiso 1 calc R . C6P C 0.3282(9) 0.2159(9) 0.0400(6) 0.042(4) Uani 1 d U . H6P H 0.3528(9) 0.1722(9) 0.0306(6) 0.050 Uiso 1 calc R . C7P C 0.3633(8) 0.2839(8) 0.0318(5) 0.028(3) Uani 1 d U . C8P C 0.4385(9) 0.2882(9) 0.0079(6) 0.036(3) Uani 1 d U . O3P O 0.5001(6) 0.2810(5) 0.0404(4) 0.033(2) Uani 1 d U . O4P O 0.4337(5) 0.2900(5) -0.0383(4) 0.032(2) Uani 1 d U . C1S C 0.7580(14) 0.2594(9) 0.5977(13) 0.144(13) Uani 1 d DU . H1S1 H 0.7037(14) 0.2567(9) 0.5805(13) 0.173 Uiso 1 calc R . H1S2 H 0.7561(14) 0.2526(9) 0.6344(13) 0.173 Uiso 1 calc R . Cl1S Cl 0.8165(5) 0.1889(4) 0.5741(3) 0.118(3) Uani 1 d DU . Cl2S Cl 0.7983(5) 0.3440(5) 0.5866(4) 0.142(3) Uani 1 d DU . C1T C 0.5338(15) 0.2396(12) 0.3269(16) 0.083(11) Uani 0.50 d PDU . H1T1 H 0.4843(15) 0.2378(12) 0.3038(16) 0.100 Uiso 0.30 calc PR 1 H1T2 H 0.5209(15) 0.2440(12) 0.3620(16) 0.100 Uiso 0.30 calc PR 1 H1TA H 0.5471(15) 0.2247(12) 0.3626(16) 0.100 Uiso 0.20 calc PR 2 H1TB H 0.5409(15) 0.1971(12) 0.3047(16) 0.100 Uiso 0.20 calc PR 2 Cl1T Cl 0.5910(7) 0.3144(6) 0.3117(5) 0.087(4) Uani 0.50 d PDU . Cl2T Cl 0.5900(14) 0.1590(9) 0.3201(9) 0.099(7) Uani 0.30 d PDU 1 Cl3T Cl 0.4357(14) 0.2747(18) 0.3159(16) 0.116(12) Uani 0.20 d PDU 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 0.0225(15) 0.021(2) 0.026(2) 0.0004(13) 0.0071(12) -0.0026(12) Co2 0.0217(11) 0.0276(12) 0.0284(12) -0.0007(9) 0.0021(9) -0.0010(9) Co3 0.0263(11) 0.0273(12) 0.0267(11) 0.0024(10) 0.0048(9) 0.0028(9) Co4 0.0200(10) 0.0226(11) 0.0252(11) 0.0022(9) 0.0038(8) 0.0004(8) Co5 0.0242(11) 0.0292(12) 0.0285(12) 0.0027(10) 0.0052(9) 0.0045(9) Co6 0.0225(11) 0.0306(12) 0.0295(12) 0.0060(10) 0.0037(9) 0.0025(9) Co7 0.0309(12) 0.0436(14) 0.0327(12) 0.0062(11) 0.0093(10) 0.0125(10) O1 0.016(4) 0.028(4) 0.026(4) -0.003(4) 0.006(3) -0.009(4) N11 0.026(6) 0.033(5) 0.021(5) -0.001(4) 0.010(5) 0.002(5) C21 0.025(8) 0.041(6) 0.026(6) -0.006(5) -0.001(6) 0.014(7) C31 0.025(8) 0.051(6) 0.015(7) 0.004(5) 0.003(6) 0.007(7) C41 0.045(10) 0.043(7) 0.025(7) 0.013(6) 0.015(7) -0.001(7) C51 0.027(8) 0.035(7) 0.038(7) 0.004(6) 0.000(7) -0.001(7) C61 0.026(7) 0.036(6) 0.022(5) 0.002(5) -0.002(5) -0.005(6) O61 0.025(4) 0.030(5) 0.020(4) -0.006(4) 0.002(4) 0.008(4) Cl1 0.048(3) 0.050(3) 0.040(3) -0.014(2) -0.014(2) 0.003(2) N12 0.037(7) 0.032(5) 0.026(6) 0.004(4) 0.000(5) 0.000(5) C22 0.037(9) 0.046(7) 0.028(8) 0.005(6) 0.001(6) 0.007(7) C32 0.044(10) 0.053(7) 0.046(10) 0.016(7) 0.013(8) -0.005(8) C42 0.048(10) 0.027(7) 0.049(10) 0.011(6) -0.002(7) -0.009(7) C52 0.045(9) 0.034(6) 0.030(8) 0.000(6) 0.000(6) 0.003(7) C62 0.018(7) 0.036(6) 0.029(7) 0.002(6) -0.001(6) -0.004(6) O62 0.029(5) 0.029(4) 0.037(5) 0.004(4) 0.015(4) 0.002(4) Cl2 0.057(3) 0.072(3) 0.039(3) 0.003(2) 0.025(2) 0.010(3) N13 0.020(4) 0.036(6) 0.049(7) 0.008(5) 0.004(5) -0.007(4) C23 0.023(6) 0.047(8) 0.077(13) 0.010(8) -0.011(8) 0.003(5) C33 0.026(7) 0.062(10) 0.082(14) -0.009(10) -0.010(9) -0.009(6) C43 0.040(8) 0.046(9) 0.083(14) -0.005(10) -0.010(9) -0.004(6) C53 0.032(7) 0.032(7) 0.046(10) 0.015(7) -0.002(7) -0.002(6) C63 0.019(5) 0.045(7) 0.042(9) 0.000(7) 0.001(6) 0.000(5) O63 0.016(4) 0.030(4) 0.045(6) 0.002(4) 0.007(4) -0.001(3) Cl3 0.025(2) 0.056(3) 0.154(6) 0.009(4) -0.010(3) 0.005(2) N14 0.041(8) 0.034(5) 0.029(6) -0.009(4) -0.002(5) 0.015(6) C24 0.074(13) 0.042(7) 0.052(10) -0.007(7) -0.023(8) 0.021(9) C34 0.086(14) 0.060(7) 0.038(10) -0.017(7) -0.030(9) 0.016(10) C44 0.053(11) 0.044(7) 0.047(10) -0.025(7) -0.012(7) 0.007(8) C54 0.025(8) 0.037(7) 0.032(8) -0.012(6) 0.005(6) 0.002(6) C64 0.023(7) 0.035(6) 0.020(6) -0.004(5) 0.010(5) 0.008(6) O64 0.021(5) 0.027(5) 0.023(4) -0.002(4) 0.004(3) -0.005(4) Cl4 0.178(7) 0.052(3) 0.057(4) 0.000(3) -0.042(4) 0.027(4) N15 0.043(7) 0.023(5) 0.014(6) -0.003(4) 0.005(5) 0.003(5) C25 0.049(10) 0.024(7) 0.034(9) -0.003(6) 0.004(6) -0.001(6) C35 0.051(10) 0.039(8) 0.054(11) -0.025(8) 0.008(7) -0.022(8) C45 0.056(11) 0.035(8) 0.050(11) -0.007(8) 0.012(8) 0.000(7) C55 0.043(10) 0.043(8) 0.042(10) -0.011(7) 0.016(7) -0.003(7) C65 0.022(7) 0.044(7) 0.020(7) -0.005(6) -0.004(5) 0.007(5) O65 0.025(4) 0.040(6) 0.034(6) -0.004(5) 0.008(4) 0.004(4) Cl5 0.073(3) 0.041(3) 0.062(3) -0.013(2) 0.031(3) -0.023(2) N16 0.046(8) 0.054(8) 0.033(5) 0.006(5) 0.018(5) 0.025(5) C26 0.038(10) 0.061(11) 0.050(8) -0.008(7) 0.011(7) 0.021(7) C36 0.072(12) 0.076(13) 0.037(7) 0.007(8) 0.022(7) 0.025(9) C46 0.051(11) 0.073(13) 0.036(8) -0.006(8) -0.001(8) 0.014(8) C56 0.053(10) 0.071(11) 0.023(6) 0.008(7) 0.015(6) 0.015(8) C66 0.039(9) 0.046(9) 0.033(6) -0.003(6) 0.009(6) 0.011(7) O66 0.032(5) 0.039(5) 0.030(4) 0.002(4) 0.007(4) 0.014(4) Cl6 0.091(4) 0.097(5) 0.074(4) 0.001(3) 0.025(3) 0.067(4) N17 0.028(5) 0.024(5) 0.031(7) 0.002(5) 0.001(5) 0.009(4) C27 0.036(8) 0.026(6) 0.050(10) -0.003(7) 0.006(7) 0.018(5) C37 0.046(9) 0.027(7) 0.060(11) 0.006(8) 0.011(8) 0.007(6) C47 0.042(9) 0.037(7) 0.070(12) 0.009(9) 0.026(8) 0.002(7) C57 0.029(8) 0.031(6) 0.038(9) 0.013(7) 0.012(7) 0.012(6) C67 0.026(7) 0.024(5) 0.035(8) -0.001(5) 0.006(6) 0.003(5) O67 0.019(4) 0.027(4) 0.028(4) 0.003(3) 0.007(4) 0.001(3) Cl7 0.059(3) 0.037(3) 0.062(3) 0.001(2) 0.019(2) 0.025(2) N18 0.028(5) 0.027(5) 0.029(7) 0.003(5) 0.011(5) -0.001(4) C28 0.033(7) 0.031(7) 0.044(10) 0.010(7) 0.005(8) 0.001(5) C38 0.050(7) 0.025(7) 0.064(12) 0.007(8) 0.020(9) 0.004(6) C48 0.051(8) 0.029(8) 0.070(12) 0.018(9) 0.016(9) 0.019(7) C58 0.028(7) 0.041(8) 0.044(10) 0.015(8) 0.005(8) 0.002(5) C68 0.031(6) 0.025(6) 0.033(8) -0.001(6) 0.004(6) 0.000(5) O68 0.036(6) 0.030(5) 0.034(5) 0.003(4) 0.016(4) -0.004(4) Cl8 0.036(2) 0.044(3) 0.106(4) 0.021(3) 0.022(3) -0.002(2) N19 0.028(6) 0.066(6) 0.033(7) 0.016(5) 0.007(5) 0.005(4) C29 0.025(8) 0.088(8) 0.040(10) 0.022(9) 0.010(7) 0.010(7) C39 0.030(9) 0.106(8) 0.067(13) 0.046(11) 0.020(8) 0.013(8) C49 0.041(10) 0.089(9) 0.061(12) 0.041(11) 0.015(8) -0.006(9) C59 0.031(9) 0.065(8) 0.056(11) 0.018(9) 0.011(7) -0.017(7) C69 0.025(6) 0.050(6) 0.026(8) 0.007(7) -0.003(5) -0.009(6) O69 0.023(4) 0.034(6) 0.031(4) 0.012(4) 0.002(3) -0.008(4) Cl9 0.050(3) 0.112(4) 0.057(3) 0.022(3) 0.029(3) 0.034(3) N110 0.023(5) 0.052(8) 0.046(6) 0.011(5) 0.013(5) 0.016(5) C210 0.035(8) 0.053(10) 0.045(8) 0.027(7) 0.011(6) 0.021(7) C310 0.037(9) 0.054(11) 0.050(8) 0.025(7) 0.003(6) 0.020(8) C410 0.036(9) 0.049(11) 0.068(10) 0.011(8) -0.003(8) 0.014(7) C510 0.025(8) 0.050(10) 0.043(7) 0.017(7) -0.002(6) 0.008(7) C610 0.032(8) 0.050(9) 0.030(6) 0.017(7) 0.015(5) 0.014(6) O610 0.025(5) 0.031(5) 0.032(4) 0.013(4) 0.002(4) 0.009(4) Cl10 0.056(3) 0.072(4) 0.066(3) 0.011(3) 0.022(3) 0.036(3) O1P 0.019(5) 0.021(5) 0.048(7) -0.003(4) 0.004(4) -0.004(4) O2P 0.035(5) 0.022(4) 0.033(6) 0.000(4) 0.009(5) -0.001(4) C1P 0.018(6) 0.023(5) 0.029(8) 0.005(6) -0.002(6) 0.006(5) C2P 0.021(7) 0.027(5) 0.037(9) 0.003(7) 0.008(6) 0.000(5) C3P 0.024(7) 0.023(6) 0.032(8) 0.004(7) 0.008(6) 0.009(5) C4P 0.024(8) 0.031(7) 0.061(11) 0.011(8) 0.010(7) 0.001(6) C5P 0.037(9) 0.024(7) 0.083(13) 0.022(9) 0.019(8) 0.009(7) C6P 0.040(8) 0.026(6) 0.061(11) 0.014(8) 0.014(8) 0.007(6) C7P 0.028(6) 0.030(6) 0.027(8) 0.006(7) 0.007(6) 0.006(5) C8P 0.034(7) 0.039(9) 0.037(7) 0.003(8) 0.013(5) 0.002(7) O3P 0.031(5) 0.028(6) 0.042(6) 0.005(5) 0.012(4) 0.000(5) O4P 0.028(6) 0.036(6) 0.033(5) -0.009(5) 0.011(4) -0.003(5) C1S 0.074(19) 0.113(13) 0.252(40) 0.049(22) 0.049(22) 0.043(13) Cl1S 0.115(6) 0.124(6) 0.110(6) -0.014(5) -0.007(5) 0.051(5) Cl2S 0.127(7) 0.116(6) 0.174(9) 0.017(6) -0.026(6) 0.003(5) C1T 0.125(26) 0.074(19) 0.057(27) 0.011(25) 0.036(26) 0.005(14) Cl1T 0.099(9) 0.061(7) 0.097(9) 0.002(7) -0.004(7) -0.001(7) Cl2T 0.109(17) 0.068(9) 0.120(19) 0.018(13) 0.014(15) 0.009(12) Cl3T 0.115(15) 0.068(22) 0.169(37) -0.025(23) 0.025(26) -0.016(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1P 2.020(9) . ? Co1 O1P 2.020(9) 3_665 ? Co1 O61 2.136(7) 3_665 ? Co1 O61 2.136(7) . ? Co1 O64 2.178(7) . ? Co1 O64 2.178(7) 3_665 ? Co2 O4P 1.972(9) 3_665 ? Co2 O1 2.023(9) . ? Co2 N15 2.078(7) . ? Co2 N11 2.088(8) . ? Co3 O1 1.986(9) . ? Co3 O3P 1.987(10) 3_665 ? Co3 N14 2.067(8) . ? Co3 N18 2.082(7) . ? Co4 O2P 2.023(10) . ? Co4 O62 2.035(7) . ? Co4 O63 2.058(7) . ? Co4 O64 2.122(8) . ? Co4 O1 2.136(9) . ? Co4 O61 2.142(8) . ? Co5 O66 1.991(7) . ? Co5 O65 2.018(8) . ? Co5 O69 2.088(9) . ? Co5 N12 2.101(8) . ? Co5 O67 2.205(8) . ? Co5 O62 2.247(8) . ? Co6 O610 1.996(7) . ? Co6 O68 2.024(8) . ? Co6 O69 2.091(9) . ? Co6 N13 2.145(8) . ? Co6 O63 2.191(8) . ? Co6 O67 2.220(8) . ? Co7 N17 2.172(8) . ? Co7 N16 2.184(8) . ? Co7 N19 2.188(8) . ? Co7 N110 2.214(8) . ? Co7 O610 2.221(9) . ? Co7 O66 2.225(8) . ? N11 C21 1.347(8) . ? N11 C61 1.352(8) . ? C21 C31 1.368(9) . ? C21 Cl1 1.741(7) . ? C31 C41 1.386(9) . ? C41 C51 1.368(9) . ? C51 C61 1.410(8) . ? C61 O61 1.303(7) . ? N12 C22 1.344(8) . ? N12 C62 1.354(8) . ? C22 C32 1.365(9) . ? C22 Cl2 1.741(7) . ? C32 C42 1.386(9) . ? C42 C52 1.368(9) . ? C52 C62 1.408(8) . ? C62 O62 1.298(7) . ? N13 C23 1.343(8) . ? N13 C63 1.354(8) . ? C23 C33 1.367(9) . ? C23 Cl3 1.745(7) . ? C33 C43 1.388(9) . ? C43 C53 1.370(9) . ? C53 C63 1.409(8) . ? C63 O63 1.300(7) . ? N14 C24 1.344(8) . ? N14 C64 1.354(8) . ? C24 C34 1.368(9) . ? C24 Cl4 1.747(7) . ? C34 C44 1.388(9) . ? C44 C54 1.366(9) . ? C54 C64 1.410(8) . ? C64 O64 1.299(7) . ? N15 C25 1.345(8) . ? N15 C65 1.357(8) . ? C25 C35 1.365(9) . ? C25 Cl5 1.742(7) . ? C35 C45 1.385(9) . ? C45 C55 1.370(9) . ? C55 C65 1.405(8) . ? C65 O65 1.302(7) . ? N16 C26 1.346(8) . ? N16 C66 1.355(8) . ? C26 C36 1.367(9) . ? C26 Cl6 1.741(7) . ? C36 C46 1.384(9) . ? C46 C56 1.367(9) . ? C56 C66 1.409(8) . ? C66 O66 1.299(7) . ? N17 C27 1.350(8) . ? N17 C67 1.353(8) . ? C27 C37 1.368(9) . ? C27 Cl7 1.744(7) . ? C37 C47 1.385(9) . ? C47 C57 1.362(9) . ? C57 C67 1.413(8) . ? C67 O67 1.303(7) . ? N18 C28 1.346(8) . ? N18 C68 1.353(8) . ? C28 C38 1.365(9) . ? C28 Cl8 1.744(7) . ? C38 C48 1.387(9) . ? C48 C58 1.367(9) . ? C58 C68 1.408(8) . ? C68 O68 1.302(7) . ? N19 C29 1.349(8) . ? N19 C69 1.352(8) . ? C29 C39 1.366(9) . ? C29 Cl9 1.743(7) . ? C39 C49 1.382(9) . ? C49 C59 1.365(9) . ? C59 C69 1.412(8) . ? C69 O69 1.305(7) . ? N110 C210 1.345(8) . ? N110 C610 1.350(8) . ? C210 C310 1.366(9) . ? C210 Cl10 1.743(7) . ? C310 C410 1.388(9) . ? C410 C510 1.367(9) . ? C510 C610 1.410(8) . ? C610 O610 1.300(7) . ? O1P C1P 1.26(2) . ? O2P C1P 1.29(2) . ? C1P C2P 1.47(2) . ? C2P C3P 1.35(2) . ? C2P C7P 1.44(2) . ? C3P C4P 1.42(2) . ? C4P C5P 1.40(2) . ? C5P C6P 1.34(2) . ? C6P C7P 1.41(2) . ? C7P C8P 1.51(2) . ? C8P O4P 1.22(2) . ? C8P O3P 1.29(2) . ? O3P Co3 1.987(10) 3_665 ? O4P Co2 1.972(9) 3_665 ? C1S Cl2S 1.73(2) . ? C1S Cl1S 1.79(2) . ? C1T Cl1T 1.75(2) . ? C1T Cl2T 1.78(2) . ? C1T Cl3T 1.79(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 O1P Co1 O1P 180.000(1) . 3_665 ? O1P Co1 O61 90.4(4) . 3_665 ? O1P Co1 O61 89.6(4) 3_665 3_665 ? O1P Co1 O61 89.6(4) . . ? O1P Co1 O61 90.4(4) 3_665 . ? O61 Co1 O61 180.000(1) 3_665 . ? O1P Co1 O64 90.5(3) . . ? O1P Co1 O64 89.5(3) 3_665 . ? O61 Co1 O64 105.9(3) 3_665 . ? O61 Co1 O64 74.1(3) . . ? O1P Co1 O64 89.5(3) . 3_665 ? O1P Co1 O64 90.5(3) 3_665 3_665 ? O61 Co1 O64 74.1(3) 3_665 3_665 ? O61 Co1 O64 105.9(3) . 3_665 ? O64 Co1 O64 180.0 . 3_665 ? O4P Co2 O1 100.4(4) 3_665 . ? O4P Co2 N15 102.6(3) 3_665 . ? O1 Co2 N15 108.0(4) . . ? O4P Co2 N11 107.9(4) 3_665 . ? O1 Co2 N11 123.9(4) . . ? N15 Co2 N11 111.4(3) . . ? O1 Co3 O3P 100.5(4) . 3_665 ? O1 Co3 N14 122.8(4) . . ? O3P Co3 N14 106.5(5) 3_665 . ? O1 Co3 N18 110.2(4) . . ? O3P Co3 N18 105.0(3) 3_665 . ? N14 Co3 N18 109.8(4) . . ? O2P Co4 O62 94.3(4) . . ? O2P Co4 O63 92.6(4) . . ? O62 Co4 O63 89.6(4) . . ? O2P Co4 O64 92.7(4) . . ? O62 Co4 O64 168.6(3) . . ? O63 Co4 O64 98.9(3) . . ? O2P Co4 O1 178.0(4) . . ? O62 Co4 O1 87.3(3) . . ? O63 Co4 O1 86.3(3) . . ? O64 Co4 O1 85.9(3) . . ? O2P Co4 O61 94.2(4) . . ? O62 Co4 O61 95.5(3) . . ? O63 Co4 O61 171.2(4) . . ? O64 Co4 O61 75.1(3) . . ? O1 Co4 O61 86.8(3) . . ? O66 Co5 O65 106.7(4) . . ? O66 Co5 O69 87.1(3) . . ? O65 Co5 O69 157.9(3) . . ? O66 Co5 N12 107.5(3) . . ? O65 Co5 N12 104.5(4) . . ? O69 Co5 N12 87.0(4) . . ? O66 Co5 O67 85.2(3) . . ? O65 Co5 O67 87.8(3) . . ? O69 Co5 O67 76.1(3) . . ? N12 Co5 O67 158.5(4) . . ? O66 Co5 O62 168.2(3) . . ? O65 Co5 O62 81.3(3) . . ? O69 Co5 O62 88.1(3) . . ? N12 Co5 O62 61.5(2) . . ? O67 Co5 O62 104.1(3) . . ? O610 Co6 O68 106.7(4) . . ? O610 Co6 O69 86.9(3) . . ? O68 Co6 O69 156.3(3) . . ? O610 Co6 N13 111.8(3) . . ? O68 Co6 N13 98.0(4) . . ? O69 Co6 N13 94.6(4) . . ? O610 Co6 O63 171.5(4) . . ? O68 Co6 O63 80.4(3) . . ? O69 Co6 O63 88.1(3) . . ? N13 Co6 O63 61.8(2) . . ? O610 Co6 O67 82.1(3) . . ? O68 Co6 O67 86.8(3) . . ? O69 Co6 O67 75.7(3) . . ? N13 Co6 O67 163.0(3) . . ? O63 Co6 O67 103.3(3) . . ? N17 Co7 N16 97.0(5) . . ? N17 Co7 N19 145.4(3) . . ? N16 Co7 N19 99.1(5) . . ? N17 Co7 N110 101.7(4) . . ? N16 Co7 N110 122.5(3) . . ? N19 Co7 N110 95.1(5) . . ? N17 Co7 O610 79.8(4) . . ? N16 Co7 O610 176.2(4) . . ? N19 Co7 O610 82.6(4) . . ? N110 Co7 O610 60.5(2) . . ? N17 Co7 O66 81.3(4) . . ? N16 Co7 O66 60.8(2) . . ? N19 Co7 O66 80.3(4) . . ? N110 Co7 O66 174.9(4) . . ? O610 Co7 O66 116.5(3) . . ? Co3 O1 Co2 122.3(4) . . ? Co3 O1 Co4 103.1(4) . . ? Co2 O1 Co4 101.9(4) . . ? C21 N11 C61 118.2(6) . . ? C21 N11 Co2 135.9(5) . . ? C61 N11 Co2 105.3(5) . . ? N11 C21 C31 124.5(6) . . ? N11 C21 Cl1 116.0(6) . . ? C31 C21 Cl1 119.4(6) . . ? C21 C31 C41 116.6(6) . . ? C51 C41 C31 121.1(7) . . ? C41 C51 C61 118.8(7) . . ? O61 C61 N11 114.9(6) . . ? O61 C61 C51 124.5(7) . . ? N11 C61 C51 120.6(6) . . ? C61 O61 Co1 129.2(7) . . ? C61 O61 Co4 120.9(8) . . ? Co1 O61 Co4 99.6(3) . . ? C22 N12 C62 118.1(6) . . ? C22 N12 Co5 144.8(6) . . ? C62 N12 Co5 94.3(5) . . ? N12 C22 C32 124.7(6) . . ? N12 C22 Cl2 115.3(6) . . ? C32 C22 Cl2 120.0(6) . . ? C22 C32 C42 116.6(7) . . ? C52 C42 C32 120.9(7) . . ? C42 C52 C62 118.9(7) . . ? O62 C62 N12 114.1(6) . . ? O62 C62 C52 125.5(7) . . ? N12 C62 C52 120.4(6) . . ? C62 O62 Co4 138.6(7) . . ? C62 O62 Co5 89.4(5) . . ? Co4 O62 Co5 125.6(4) . . ? C23 N13 C63 118.2(6) . . ? C23 N13 Co6 149.5(5) . . ? C63 N13 Co6 92.3(4) . . ? N13 C23 C33 124.8(6) . . ? N13 C23 Cl3 115.4(6) . . ? C33 C23 Cl3 119.8(6) . . ? C23 C33 C43 116.5(7) . . ? C53 C43 C33 121.1(7) . . ? C43 C53 C63 118.7(7) . . ? O63 C63 N13 114.1(6) . . ? O63 C63 C53 125.2(7) . . ? N13 C63 C53 120.6(6) . . ? C63 O63 Co4 139.2(6) . . ? C63 O63 Co6 91.8(5) . . ? Co4 O63 Co6 127.8(4) . . ? C24 N14 C64 118.2(6) . . ? C24 N14 Co3 135.2(5) . . ? C64 N14 Co3 106.5(5) . . ? N14 C24 C34 124.6(6) . . ? N14 C24 Cl4 116.1(6) . . ? C34 C24 Cl4 119.3(6) . . ? C24 C34 C44 116.5(7) . . ? C54 C44 C34 121.2(7) . . ? C44 C54 C64 118.7(7) . . ? O64 C64 N14 114.9(6) . . ? O64 C64 C54 124.5(7) . . ? N14 C64 C54 120.5(6) . . ? C64 O64 Co4 121.0(8) . . ? C64 O64 Co1 129.5(7) . . ? Co4 O64 Co1 98.9(3) . . ? C25 N15 C65 117.8(6) . . ? C25 N15 Co2 138.4(5) . . ? C65 N15 Co2 103.8(4) . . ? N15 C25 C35 124.6(6) . . ? N15 C25 Cl5 115.7(6) . . ? C35 C25 Cl5 119.7(6) . . ? C25 C35 C45 117.0(7) . . ? C55 C45 C35 120.9(7) . . ? C45 C55 C65 118.6(7) . . ? O65 C65 N15 113.9(6) . . ? O65 C65 C55 125.1(7) . . ? N15 C65 C55 121.0(6) . . ? C65 O65 Co5 129.6(8) . . ? C26 N16 C66 117.8(6) . . ? C26 N16 Co7 149.6(5) . . ? C66 N16 Co7 92.5(4) . . ? N16 C26 C36 124.8(6) . . ? N16 C26 Cl6 115.7(6) . . ? C36 C26 Cl6 119.5(6) . . ? C26 C36 C46 116.7(7) . . ? C56 C46 C36 121.0(7) . . ? C46 C56 C66 118.8(7) . . ? O66 C66 N16 114.4(6) . . ? O66 C66 C56 124.9(7) . . ? N16 C66 C56 120.8(6) . . ? C66 O66 Co5 153.7(6) . . ? C66 O66 Co7 92.3(5) . . ? Co5 O66 Co7 114.0(4) . . ? C27 N17 C67 117.9(6) . . ? C27 N17 Co7 122.8(5) . . ? C67 N17 Co7 119.3(5) . . ? N17 C27 C37 124.6(6) . . ? N17 C27 Cl7 116.5(6) . . ? C37 C27 Cl7 118.9(6) . . ? C27 C37 C47 116.8(7) . . ? C57 C47 C37 120.9(7) . . ? C47 C57 C67 119.1(7) . . ? O67 C67 N17 116.4(6) . . ? O67 C67 C57 123.0(6) . . ? N17 C67 C57 120.6(6) . . ? C67 O67 Co5 127.0(9) . . ? C67 O67 Co6 127.8(9) . . ? Co5 O67 Co6 96.6(3) . . ? C28 N18 C68 117.9(6) . . ? C28 N18 Co3 138.1(5) . . ? C68 N18 Co3 104.0(4) . . ? N18 C28 C38 124.8(6) . . ? N18 C28 Cl8 115.7(6) . . ? C38 C28 Cl8 119.5(6) . . ? C28 C38 C48 116.6(7) . . ? C58 C48 C38 121.0(7) . . ? C48 C58 C68 118.9(7) . . ? O68 C68 N18 114.4(6) . . ? O68 C68 C58 124.8(7) . . ? N18 C68 C58 120.7(6) . . ? C68 O68 Co6 129.0(8) . . ? C29 N19 C69 117.8(6) . . ? C29 N19 Co7 123.5(5) . . ? C69 N19 Co7 118.5(5) . . ? N19 C29 C39 124.7(7) . . ? N19 C29 Cl9 116.1(6) . . ? C39 C29 Cl9 119.1(6) . . ? C29 C39 C49 116.9(7) . . ? C59 C49 C39 121.0(7) . . ? C49 C59 C69 118.9(7) . . ? O69 C69 N19 116.0(6) . . ? O69 C69 C59 123.3(7) . . ? N19 C69 C59 120.7(6) . . ? C69 O69 Co6 125.3(9) . . ? C69 O69 Co5 124.9(9) . . ? Co6 O69 Co5 104.5(3) . . ? C210 N110 C610 118.0(6) . . ? C210 N110 Co7 149.9(5) . . ? C610 N110 Co7 91.7(4) . . ? N110 C210 C310 124.8(6) . . ? N110 C210 Cl10 115.5(6) . . ? C310 C210 Cl10 119.7(6) . . ? C210 C310 C410 116.7(7) . . ? C510 C410 C310 120.7(7) . . ? C410 C510 C610 119.0(7) . . ? O610 C610 N110 114.8(6) . . ? O610 C610 C510 124.5(7) . . ? N110 C610 C510 120.6(6) . . ? C610 O610 Co6 149.0(7) . . ? C610 O610 Co7 92.8(5) . . ? Co6 O610 Co7 115.6(3) . . ? C1P O1P Co1 135.5(9) . . ? C1P O2P Co4 128.9(9) . . ? O1P C1P O2P 124.4(13) . . ? O1P C1P C2P 118.9(12) . . ? O2P C1P C2P 116.6(12) . . ? C3P C2P C7P 118.8(13) . . ? C3P C2P C1P 123.0(13) . . ? C7P C2P C1P 118.2(12) . . ? C2P C3P C4P 122.2(14) . . ? C5P C4P C3P 117.6(14) . . ? C6P C5P C4P 121.5(15) . . ? C5P C6P C7P 121.5(15) . . ? C6P C7P C2P 118.4(13) . . ? C6P C7P C8P 121.0(14) . . ? C2P C7P C8P 120.6(13) . . ? O4P C8P O3P 129.1(14) . . ? O4P C8P C7P 117.7(14) . . ? O3P C8P C7P 112.7(13) . . ? C8P O3P Co3 132.5(10) . 3_665 ? C8P O4P Co2 134.0(10) . 3_665 ? Cl2S C1S Cl1S 109.3(13) . . ? Cl1T C1T Cl2T 107.2(14) . . ? Cl1T C1T Cl3T 103.0(14) . . ? _refine_diff_density_max 1.315 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.154 data_coas12 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C65.75 H70.25 Cl8.75 Co7 N9.75 O20' _chemical_formula_weight 2039.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' -2.3653 3.6143 '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 13.976(7) _cell_length_b 15.049(8) _cell_length_c 22.158(12) _cell_angle_alpha 86.48(4) _cell_angle_beta 89.39(3) _cell_angle_gamma 66.66(4) _cell_volume 4270(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 70 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Purple _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2062 _exptl_absorpt_coefficient_mu 13.494 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.105 _exptl_absorpt_correction_T_max 0.562 _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'Omega-theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3 _diffrn_reflns_number 15140 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1816 _diffrn_reflns_limit_h_min -16 _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 27 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 70.24 _reflns_number_total 15140 _reflns_number_gt 7428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution sir92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL' _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_details 'calc w=1/[\s^2^(Fo^2^)+(0.1468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00027(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 15140 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.2016 _refine_ls_R_factor_gt 0.0994 _refine_ls_wR_factor_ref 0.2826 _refine_ls_wR_factor_gt 0.2227 _refine_ls_goodness_of_fit_all 0.986 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 1.089 _refine_ls_shift/su_mean 0.007 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co5 Co -0.14060(15) 0.40599(13) 0.31547(9) 0.0277(5) Uani 1 d . . . Co3 Co 0.34430(14) 0.22547(13) 0.23606(8) 0.0218(4) Uani 1 d . . . Co4 Co 0.06227(14) 0.40781(12) 0.26557(8) 0.0226(4) Uani 1 d . . . Co6 Co -0.00732(14) 0.18847(12) 0.31102(8) 0.0203(4) Uani 1 d . . . Co7 Co 0.29856(15) 0.02630(12) 0.28537(8) 0.0222(4) Uani 1 d . . . Co2 Co -0.06549(14) 0.28638(12) 0.16788(8) 0.0213(4) Uani 1 d . . . Co1 Co 0.18120(14) 0.16364(12) 0.16981(7) 0.0175(4) Uani 1 d . . . O1H O 0.3854(7) 0.3312(6) 0.1955(4) 0.037(2) Uani 1 d . . . H1H1 H 0.3486 0.3850 0.2089 0.055 Uiso 1 calc R . . O2 O 0.0228(6) 0.3109(5) 0.3214(3) 0.0243(18) Uani 1 d . . . H2H H 0.0495 0.3088 0.3634 0.029 Uiso 1 calc R . . O1 O 0.2415(5) 0.1641(5) 0.2542(3) 0.0193(17) Uani 1 d . . . H1H H 0.1854 0.2048 0.2811 0.023 Uiso 1 calc R . . O2A O 0.4461(6) -0.0135(6) 0.2676(4) 0.036(2) Uani 1 d . . . O1A O 0.4725(6) 0.1087(6) 0.2187(4) 0.035(2) Uani 1 d . . . C1A C 0.4974(9) 0.0203(9) 0.2322(6) 0.030(3) Uani 1 d . . . C2A C 0.5899(11) -0.0546(10) 0.2037(6) 0.049(4) Uani 1 d D . . C3A C 0.6438(17) -0.0103(15) 0.1581(9) 0.069(7) Uiso 0.80 d PD A 1 H3A1 H 0.5983 0.0177 0.1226 0.104 Uiso 0.80 calc PR A 1 H3A2 H 0.7094 -0.0608 0.1459 0.104 Uiso 0.80 calc PR A 1 H3A3 H 0.6582 0.0406 0.1768 0.104 Uiso 0.80 calc PR A 1 C4A C 0.5544(17) -0.1200(15) 0.1664(9) 0.074(7) Uiso 0.80 d PD A 1 H4A1 H 0.5296 -0.1597 0.1938 0.111 Uiso 0.80 calc PR A 1 H4A2 H 0.6132 -0.1622 0.1432 0.111 Uiso 0.80 calc PR A 1 H4A3 H 0.4978 -0.0793 0.1386 0.111 Uiso 0.80 calc PR A 1 C5A C 0.6681(17) -0.1168(16) 0.2513(9) 0.078(7) Uiso 0.80 d PD A 1 H5A1 H 0.6892 -0.0755 0.2758 0.117 Uiso 0.80 calc PR A 1 H5A2 H 0.7293 -0.1628 0.2317 0.117 Uiso 0.80 calc PR A 1 H5A3 H 0.6365 -0.1526 0.2772 0.117 Uiso 0.80 calc PR A 1 C3A' C 0.610(5) -0.161(2) 0.218(3) 0.039(16) Uiso 0.20 d PD A 2 H3A4 H 0.5488 -0.1725 0.2060 0.058 Uiso 0.20 calc PR A 2 H3A5 H 0.6237 -0.1769 0.2613 0.058 Uiso 0.20 calc PR A 2 H3A6 H 0.6707 -0.2017 0.1953 0.058 Uiso 0.20 calc PR A 2 C4A' C 0.666(6) -0.034(6) 0.244(3) 0.10(4) Uiso 0.20 d PD A 2 H4A4 H 0.7380 -0.0724 0.2322 0.144 Uiso 0.20 calc PR A 2 H4A5 H 0.6570 -0.0517 0.2864 0.144 Uiso 0.20 calc PR A 2 H4A6 H 0.6530 0.0351 0.2396 0.144 Uiso 0.20 calc PR A 2 C5A' C 0.619(7) -0.041(5) 0.1384(15) 0.078(7) Uiso 0.20 d PD A 2 H5A4 H 0.6175 0.0243 0.1309 0.117 Uiso 0.20 calc PR A 2 H5A5 H 0.5692 -0.0500 0.1111 0.117 Uiso 0.20 calc PR A 2 H5A6 H 0.6893 -0.0891 0.1311 0.117 Uiso 0.20 calc PR A 2 O2C O -0.1263(7) 0.5130(6) 0.3617(4) 0.041(2) Uani 1 d . . . O1C O 0.0224(7) 0.5140(6) 0.3254(4) 0.034(2) Uani 1 d . . . C1C C -0.0597(11) 0.5494(8) 0.3540(5) 0.033(3) Uani 1 d . . . C2C C -0.0838(10) 0.6445(9) 0.3843(6) 0.040(3) Uani 1 d D . . C3C C -0.0440(15) 0.6201(14) 0.4489(7) 0.069(6) Uiso 0.90 d PD B 1 H3C1 H 0.0317 0.5833 0.4492 0.104 Uiso 0.90 calc PR B 1 H3C2 H -0.0775 0.5811 0.4699 0.104 Uiso 0.90 calc PR B 1 H3C3 H -0.0603 0.6801 0.4694 0.104 Uiso 0.90 calc PR B 1 C4C C -0.2011(12) 0.7023(13) 0.3858(8) 0.063(5) Uiso 0.90 d PD B 1 H4C1 H -0.2155 0.7695 0.3944 0.095 Uiso 0.90 calc PR B 1 H4C2 H -0.2312 0.6733 0.4175 0.095 Uiso 0.90 calc PR B 1 H4C3 H -0.2322 0.7012 0.3466 0.095 Uiso 0.90 calc PR B 1 C5C C -0.0341(16) 0.7047(15) 0.3506(9) 0.086(7) Uiso 0.90 d PD B 1 H5C1 H -0.0555 0.7676 0.3684 0.129 Uiso 0.90 calc PR B 1 H5C2 H -0.0562 0.7147 0.3080 0.129 Uiso 0.90 calc PR B 1 H5C3 H 0.0420 0.6709 0.3535 0.129 Uiso 0.90 calc PR B 1 C3C' C -0.171(5) 0.726(5) 0.350(4) 0.03(3) Uiso 0.10 d PD B 2 H3C4 H -0.2349 0.7151 0.3525 0.043 Uiso 0.10 calc PR B 2 H3C5 H -0.1514 0.7290 0.3071 0.043 Uiso 0.10 calc PR B 2 H3C6 H -0.1814 0.7880 0.3669 0.043 Uiso 0.10 calc PR B 2 C4C' C 0.011(4) 0.671(7) 0.384(4) 0.02(2) Uiso 0.10 d PD B 2 H4C4 H -0.0114 0.7396 0.3909 0.034 Uiso 0.10 calc PR B 2 H4C5 H 0.0445 0.6580 0.3444 0.034 Uiso 0.10 calc PR B 2 H4C6 H 0.0601 0.6315 0.4156 0.034 Uiso 0.10 calc PR B 2 C5C' C -0.117(8) 0.638(10) 0.4492(18) 0.086(7) Uiso 0.10 d PD B 2 H5C4 H -0.0648 0.6440 0.4764 0.129 Uiso 0.10 calc PR B 2 H5C5 H -0.1220 0.5758 0.4581 0.129 Uiso 0.10 calc PR B 2 H5C6 H -0.1846 0.6910 0.4551 0.129 Uiso 0.10 calc PR B 2 O2B O -0.0332(6) 0.2440(6) 0.0831(3) 0.0287(19) Uani 1 d . . . O1B O 0.1364(6) 0.1522(6) 0.0859(3) 0.0269(19) Uani 1 d . . . C1B C 0.0489(10) 0.1889(7) 0.0602(5) 0.023(3) Uani 1 d . . . C2B C 0.0473(10) 0.1647(9) -0.0063(5) 0.031(3) Uani 1 d . . . C3B C 0.1116(13) 0.0564(10) -0.0119(7) 0.057(5) Uani 1 d . . . H3B1 H 0.1837 0.0405 0.0010 0.086 Uiso 1 calc R . . H3B2 H 0.1104 0.0406 -0.0541 0.086 Uiso 1 calc R . . H3B3 H 0.0818 0.0188 0.0138 0.086 Uiso 1 calc R . . C4B C 0.0970(11) 0.2246(11) -0.0442(6) 0.046(4) Uani 1 d . . . H4B1 H 0.0556 0.2939 -0.0405 0.070 Uiso 1 calc R . . H4B2 H 0.0988 0.2096 -0.0868 0.070 Uiso 1 calc R . . H4B3 H 0.1682 0.2082 -0.0294 0.070 Uiso 1 calc R . . C5B C -0.0644(11) 0.1914(9) -0.0277(5) 0.041(4) Uani 1 d . . . H5B1 H -0.0934 0.1495 -0.0056 0.062 Uiso 1 calc R . . H5B2 H -0.0652 0.1825 -0.0711 0.062 Uiso 1 calc R . . H5B3 H -0.1064 0.2592 -0.0202 0.062 Uiso 1 calc R . . O1D O -0.1928(7) 0.3550(6) 0.3909(4) 0.036(2) Uani 1 d . . . O2D O -0.0832(7) 0.1999(6) 0.3904(3) 0.035(2) Uani 1 d . . . C1D C -0.1557(11) 0.2670(9) 0.4133(5) 0.034(3) Uani 1 d . . . C2D C -0.2042(9) 0.2434(8) 0.4725(5) 0.039(3) Uani 1 d D . . C3D C -0.1225(16) 0.1585(13) 0.5082(10) 0.061(7) Uiso 0.70 d PD C 1 H3D1 H -0.0600 0.1718 0.5137 0.091 Uiso 0.70 calc PR C 1 H3D2 H -0.1044 0.0996 0.4861 0.091 Uiso 0.70 calc PR C 1 H3D3 H -0.1502 0.1492 0.5478 0.091 Uiso 0.70 calc PR C 1 C4D C -0.2919(15) 0.2177(15) 0.4508(10) 0.055(6) Uiso 0.70 d PD C 1 H4D1 H -0.3268 0.2015 0.4858 0.083 Uiso 0.70 calc PR C 1 H4D2 H -0.2635 0.1619 0.4258 0.083 Uiso 0.70 calc PR C 1 H4D3 H -0.3422 0.2732 0.4269 0.083 Uiso 0.70 calc PR C 1 C5D C -0.2469(19) 0.3306(14) 0.5095(11) 0.066(8) Uiso 0.70 d PD C 1 H5D1 H -0.2915 0.3870 0.4839 0.099 Uiso 0.70 calc PR C 1 H5D2 H -0.1892 0.3433 0.5262 0.099 Uiso 0.70 calc PR C 1 H5D3 H -0.2879 0.3184 0.5427 0.099 Uiso 0.70 calc PR C 1 C3D' C -0.3162(18) 0.265(3) 0.4548(19) 0.039(12) Uiso 0.30 d PD C 2 H3D4 H -0.3174 0.2330 0.4177 0.058 Uiso 0.30 calc PR C 2 H3D5 H -0.3546 0.3351 0.4478 0.058 Uiso 0.30 calc PR C 2 H3D6 H -0.3490 0.2406 0.4874 0.058 Uiso 0.30 calc PR C 2 C4D' C -0.204(3) 0.3111(18) 0.5204(12) 0.012(7) Uiso 0.30 d PD C 2 H4D4 H -0.2273 0.3774 0.5022 0.018 Uiso 0.30 calc PR C 2 H4D5 H -0.1340 0.2906 0.5374 0.018 Uiso 0.30 calc PR C 2 H4D6 H -0.2524 0.3092 0.5526 0.018 Uiso 0.30 calc PR C 2 C5D' C -0.148(3) 0.1390(14) 0.4952(15) 0.018(8) Uiso 0.30 d PD C 2 H5D4 H -0.1554 0.0966 0.4655 0.027 Uiso 0.30 calc PR C 2 H5D5 H -0.1781 0.1277 0.5336 0.027 Uiso 0.30 calc PR C 2 H5D6 H -0.0739 0.1249 0.5015 0.027 Uiso 0.30 calc PR C 2 O22 O 0.2164(6) 0.3482(5) 0.2846(3) 0.0253(18) Uani 1 d . . . N12 N 0.3660(8) 0.2459(7) 0.3277(4) 0.030(2) Uani 1 d . . . C22 C 0.2663(10) 0.3157(9) 0.3354(5) 0.031(3) Uani 1 d . . . C32 C 0.2317(13) 0.3409(12) 0.3925(7) 0.057(4) Uani 1 d . . . H32 H 0.1627 0.3863 0.3986 0.068 Uiso 1 calc R . . C42 C 0.2991(15) 0.2990(15) 0.4410(7) 0.079(6) Uani 1 d . . . H42 H 0.2770 0.3196 0.4804 0.095 Uiso 1 calc R . . C52 C 0.3975(13) 0.2282(12) 0.4341(6) 0.059(5) Uani 1 d . . . H52 H 0.4423 0.1963 0.4676 0.070 Uiso 1 calc R . . C62 C 0.4261(10) 0.2069(9) 0.3759(6) 0.036(3) Uani 1 d . . . Cl62 Cl 0.5503(3) 0.1244(3) 0.36182(18) 0.0548(10) Uani 1 d . . . O21 O 0.2964(6) 0.2118(6) 0.1445(3) 0.0259(18) Uani 1 d . . . N11 N 0.3955(8) 0.2690(8) 0.0862(4) 0.034(3) Uani 1 d . . . H11 H 0.3896 0.3132 0.1119 0.040 Uiso 1 calc R . . C21 C 0.3491(9) 0.2052(9) 0.0964(5) 0.027(3) Uani 1 d . . . C31 C 0.3617(10) 0.1359(11) 0.0540(6) 0.043(4) Uani 1 d . . . H31 H 0.3297 0.0909 0.0604 0.051 Uiso 1 calc R . . C41 C 0.4197(13) 0.1328(12) 0.0033(6) 0.059(5) Uani 1 d . . . H41 H 0.4280 0.0858 -0.0252 0.070 Uiso 1 calc R . . C51 C 0.4668(13) 0.1987(14) -0.0063(7) 0.062(5) Uani 1 d . . . H51 H 0.5079 0.1983 -0.0408 0.074 Uiso 1 calc R . . C61 C 0.4501(11) 0.2618(12) 0.0359(7) 0.050(4) Uani 1 d . . . Cl61 Cl 0.5024(3) 0.3519(4) 0.02725(19) 0.0720(14) Uani 1 d . . . O27 O 0.1367(6) 0.0936(5) 0.3381(3) 0.0249(18) Uani 1 d . . . N17 N 0.2941(7) 0.0211(6) 0.3791(4) 0.025(2) Uani 1 d . . . C27 C 0.1903(11) 0.0730(8) 0.3873(5) 0.029(3) Uani 1 d . . . C37 C 0.1524(11) 0.0960(9) 0.4449(5) 0.034(3) Uani 1 d . . . H37 H 0.0799 0.1314 0.4505 0.041 Uiso 1 calc R . . C47 C 0.2181(13) 0.0681(11) 0.4928(6) 0.048(4) Uani 1 d . . . H47 H 0.1920 0.0852 0.5321 0.058 Uiso 1 calc R . . C57 C 0.3268(14) 0.0130(10) 0.4850(6) 0.052(4) Uani 1 d . . . H57 H 0.3748 -0.0080 0.5181 0.062 Uiso 1 calc R . . C67 C 0.3571(10) -0.0075(8) 0.4272(6) 0.029(3) Uani 1 d . . . Cl67 Cl 0.4865(3) -0.0755(3) 0.41363(18) 0.0624(12) Uani 1 d . . . O28 O 0.2857(6) 0.0199(5) 0.1709(4) 0.030(2) Uani 1 d . . . N18 N 0.2606(8) -0.0752(7) 0.2458(4) 0.027(2) Uani 1 d . . . C28 C 0.2759(9) -0.0615(8) 0.1842(5) 0.023(3) Uani 1 d . . . C38 C 0.2774(11) -0.1257(9) 0.1438(6) 0.042(4) Uani 1 d . . . H38 H 0.2882 -0.1140 0.1022 0.050 Uiso 1 calc R . . C48 C 0.2633(13) -0.2080(10) 0.1632(7) 0.057(5) Uani 1 d . . . H48 H 0.2673 -0.2554 0.1357 0.069 Uiso 1 calc R . . C58 C 0.2431(13) -0.2206(10) 0.2241(7) 0.058(5) Uani 1 d . . . H58 H 0.2286 -0.2748 0.2383 0.069 Uiso 1 calc R . . C68 C 0.2442(11) -0.1552(9) 0.2626(6) 0.039(3) Uani 1 d . . . Cl68 Cl 0.2189(4) -0.1667(3) 0.33869(18) 0.0647(12) Uani 1 d . . . O26 O 0.0428(6) 0.1544(5) 0.2113(3) 0.0194(17) Uani 1 d . . . N16 N -0.0301(7) 0.0748(6) 0.2712(4) 0.021(2) Uani 1 d . . . C26 C 0.0145(9) 0.0784(8) 0.2163(5) 0.019(2) Uani 1 d . . . C36 C 0.0204(10) 0.0170(9) 0.1729(5) 0.032(3) Uani 1 d . . . H36 H 0.0464 0.0250 0.1340 0.039 Uiso 1 calc R . . C46 C -0.0119(12) -0.0572(10) 0.1863(6) 0.045(4) Uani 1 d . . . H46 H -0.0053 -0.1034 0.1575 0.054 Uiso 1 calc R . . C56 C -0.0542(13) -0.0634(10) 0.2422(6) 0.048(4) Uani 1 d . . . H56 H -0.0768 -0.1141 0.2526 0.058 Uiso 1 calc R . . C66 C -0.0628(11) 0.0031(9) 0.2814(6) 0.037(3) Uani 1 d . . . Cl66 Cl -0.1157(4) -0.0007(3) 0.35273(18) 0.0766(16) Uani 1 d . . . O24 O -0.0899(6) 0.4566(5) 0.2382(3) 0.0267(19) Uani 1 d . . . N14 N -0.1592(8) 0.4398(7) 0.1490(4) 0.028(2) Uani 1 d . . . C24 C -0.1401(10) 0.4966(8) 0.1885(5) 0.027(3) Uani 1 d . . . C34 C -0.1770(10) 0.5982(9) 0.1758(6) 0.036(3) Uani 1 d . . . H34 H -0.1638 0.6381 0.2034 0.044 Uiso 1 calc R . . C44 C -0.2317(12) 0.6378(10) 0.1236(6) 0.052(4) Uani 1 d . . . H44 H -0.2529 0.7052 0.1133 0.063 Uiso 1 calc R . . C54 C -0.2569(11) 0.5795(10) 0.0848(6) 0.042(4) Uani 1 d . . . H54 H -0.2995 0.6068 0.0498 0.051 Uiso 1 calc R . . C64 C -0.2180(9) 0.4830(9) 0.0995(6) 0.033(3) Uani 1 d . . . Cl64 Cl -0.2482(3) 0.4085(3) 0.05379(16) 0.0523(10) Uani 1 d . . . O23 O 0.0762(6) 0.3128(5) 0.1771(3) 0.0222(18) Uani 1 d . . . N13 N 0.0938(7) 0.4533(7) 0.1785(4) 0.023(2) Uani 1 d . . . C23 C 0.0908(9) 0.3869(7) 0.1457(6) 0.024(3) Uani 1 d . . . C33 C 0.1043(10) 0.3872(9) 0.0834(5) 0.031(3) Uani 1 d . . . H33 H 0.1028 0.3367 0.0602 0.037 Uiso 1 calc R . . C43 C 0.1199(12) 0.4669(10) 0.0578(6) 0.044(4) Uani 1 d . . . H43 H 0.1281 0.4720 0.0153 0.053 Uiso 1 calc R . . C53 C 0.1238(11) 0.5378(9) 0.0917(6) 0.043(4) Uani 1 d . . . H53 H 0.1374 0.5906 0.0740 0.051 Uiso 1 calc R . . C63 C 0.1073(10) 0.5297(8) 0.1533(6) 0.031(3) Uani 1 d . . . Cl63 Cl 0.0991(3) 0.6214(3) 0.19801(18) 0.0576(11) Uani 1 d . . . O25 O -0.1338(6) 0.2954(5) 0.2609(3) 0.0221(17) Uani 1 d . . . N15 N -0.1978(7) 0.2461(7) 0.1847(4) 0.026(2) Uani 1 d . . . C25 C -0.2128(9) 0.2763(7) 0.2406(5) 0.023(3) Uani 1 d . . . C35 C -0.3019(10) 0.2860(9) 0.2742(6) 0.033(3) Uani 1 d . . . H35 H -0.3117 0.3084 0.3139 0.040 Uiso 1 calc R . . C45 C -0.3758(12) 0.2604(10) 0.2454(7) 0.047(4) Uiso 1 d . . . H45 H -0.4379 0.2659 0.2658 0.056 Uiso 1 calc R . . C55 C -0.3596(9) 0.2281(10) 0.1890(6) 0.036(3) Uani 1 d . . . H55 H -0.4105 0.2120 0.1699 0.043 Uiso 1 calc R . . C65 C -0.2678(10) 0.2185(10) 0.1588(6) 0.040(3) Uani 1 d . . . Cl65 Cl -0.2421(3) 0.1742(3) 0.08953(16) 0.0497(9) Uani 1 d . . . O29 O -0.2943(8) 0.4970(8) 0.2873(5) 0.061(3) Uani 0.75 d P D 1 N19 N -0.3655(12) 0.5440(10) 0.3743(7) 0.037(4) Uani 0.75 d P D 1 H19 H -0.3219 0.4879 0.3906 0.045 Uiso 0.75 calc PR D 1 C29 C -0.3595(16) 0.5615(12) 0.3147(11) 0.047(5) Uani 0.75 d P D 1 C39 C -0.4331(17) 0.6517(14) 0.2887(11) 0.061(7) Uani 0.75 d P D 1 H39 H -0.4377 0.6650 0.2461 0.073 Uiso 0.75 calc PR D 1 C49 C -0.4936(17) 0.7153(15) 0.3242(14) 0.080(9) Uani 0.75 d P D 1 H49 H -0.5357 0.7781 0.3071 0.096 Uiso 0.75 calc PR D 1 C59 C -0.5002(18) 0.6962(18) 0.3869(13) 0.070(7) Uani 0.75 d P D 1 H59 H -0.5481 0.7424 0.4117 0.084 Uiso 0.75 calc PR D 1 C69 C -0.4316(18) 0.6047(14) 0.4102(10) 0.055(6) Uani 0.75 d P D 1 Cl69 Cl -0.4311(5) 0.5770(5) 0.4851(3) 0.0813(19) Uani 0.75 d P D 1 O29' O -0.2943(8) 0.4970(8) 0.2873(5) 0.061(3) Uani 0.25 d P D 2 C11S C 0.396(3) 0.480(2) 0.3505(15) 0.051(8) Uiso 0.50 d P . . C12S C 0.448(2) 0.5220(18) 0.1798(11) 0.031(6) Uiso 0.50 d P . . C21S C 0.289(2) 0.5389(17) 0.3399(13) 0.048(8) Uani 0.50 d P . . H21A H 0.2676 0.5263 0.3005 0.072 Uiso 0.50 calc PR . . H21B H 0.2778 0.6075 0.3403 0.072 Uiso 0.50 calc PR . . H21C H 0.2477 0.5235 0.3717 0.072 Uiso 0.50 calc PR . . C22S C 0.5492(19) 0.5094(19) 0.1538(12) 0.040(7) Uani 0.50 d P . . H22A H 0.5429 0.5690 0.1305 0.061 Uiso 0.50 calc PR . . H22B H 0.5714 0.4554 0.1271 0.061 Uiso 0.50 calc PR . . H22C H 0.6009 0.4953 0.1864 0.061 Uiso 0.50 calc PR . . N2S N 0.376(2) 0.5289(17) 0.1974(14) 0.067(9) Uani 0.50 d P . . N1S N 0.472(3) 0.435(2) 0.3651(12) 0.075(10) Uani 0.50 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 Co5 0.0236(12) 0.0240(10) 0.0347(11) 0.0052(8) 0.0090(9) -0.0097(9) Co3 0.0168(11) 0.0236(9) 0.0280(10) 0.0050(7) 0.0009(8) -0.0120(8) Co4 0.0196(11) 0.0201(9) 0.0274(10) 0.0079(7) 0.0036(8) -0.0086(8) Co6 0.0209(11) 0.0184(9) 0.0228(10) 0.0073(7) 0.0041(8) -0.0103(8) Co7 0.0213(11) 0.0199(9) 0.0241(10) 0.0090(7) -0.0037(8) -0.0082(8) Co2 0.0160(11) 0.0195(9) 0.0275(10) 0.0103(7) -0.0016(8) -0.0078(8) Co1 0.0145(10) 0.0186(8) 0.0183(9) 0.0084(7) -0.0017(7) -0.0066(7) O1H 0.033(6) 0.032(5) 0.051(6) 0.009(4) 0.006(4) -0.021(4) O2 0.023(5) 0.029(4) 0.022(4) 0.006(3) 0.006(3) -0.013(4) O1 0.004(4) 0.028(4) 0.028(4) 0.007(3) 0.000(3) -0.011(3) O2A 0.023(5) 0.040(5) 0.043(5) 0.019(4) -0.008(4) -0.013(4) O1A 0.024(5) 0.025(4) 0.051(6) 0.003(4) 0.005(4) -0.004(4) C1A 0.006(6) 0.031(7) 0.043(8) -0.007(6) 0.000(5) 0.004(5) C2A 0.033(9) 0.040(8) 0.067(11) 0.006(7) 0.008(8) -0.007(7) O2C 0.045(6) 0.038(5) 0.045(6) -0.015(4) 0.024(5) -0.021(5) O1C 0.038(6) 0.025(4) 0.039(5) -0.004(4) 0.010(4) -0.012(4) C1C 0.044(9) 0.023(6) 0.027(7) -0.004(5) 0.005(6) -0.008(6) C2C 0.044(9) 0.026(7) 0.048(9) 0.005(6) -0.003(7) -0.012(6) O2B 0.019(5) 0.040(5) 0.028(5) 0.006(4) -0.004(4) -0.013(4) O1B 0.024(5) 0.032(4) 0.022(4) 0.009(3) 0.000(4) -0.011(4) C1B 0.032(8) 0.016(5) 0.017(6) 0.000(4) 0.003(5) -0.006(5) C2B 0.031(8) 0.038(7) 0.019(6) 0.006(5) -0.010(5) -0.011(6) C3B 0.065(12) 0.041(9) 0.057(10) -0.002(7) -0.020(9) -0.011(8) C4B 0.040(9) 0.075(11) 0.026(7) 0.008(7) 0.000(6) -0.026(8) C5B 0.054(10) 0.039(7) 0.023(7) 0.002(5) -0.005(6) -0.011(7) O1D 0.027(5) 0.034(5) 0.041(5) 0.000(4) 0.024(4) -0.006(4) O2D 0.041(6) 0.041(5) 0.022(4) 0.010(4) 0.019(4) -0.017(5) C1D 0.046(9) 0.036(7) 0.024(7) -0.002(5) 0.018(6) -0.021(7) C2D 0.045(9) 0.040(8) 0.032(7) -0.001(6) 0.014(6) -0.018(7) O22 0.025(5) 0.029(4) 0.025(4) 0.004(3) -0.009(4) -0.016(4) N12 0.033(7) 0.031(5) 0.029(6) 0.013(4) -0.007(5) -0.017(5) C22 0.034(8) 0.039(7) 0.028(7) -0.001(5) -0.006(6) -0.023(6) C32 0.039(10) 0.075(12) 0.048(10) 0.005(8) 0.001(8) -0.016(9) C42 0.069(14) 0.129(18) 0.019(8) -0.007(9) 0.008(8) -0.018(13) C52 0.066(12) 0.065(11) 0.030(8) 0.013(7) -0.016(8) -0.012(9) C62 0.031(8) 0.043(8) 0.040(8) 0.009(6) -0.012(6) -0.024(7) Cl62 0.038(2) 0.053(2) 0.065(3) 0.0179(18) -0.0276(19) -0.0129(18) O21 0.019(5) 0.041(5) 0.019(4) 0.007(3) 0.001(3) -0.014(4) N11 0.027(6) 0.050(7) 0.026(6) 0.010(5) -0.004(5) -0.019(5) C21 0.021(7) 0.033(7) 0.022(6) 0.016(5) -0.005(5) -0.008(6) C31 0.023(8) 0.060(9) 0.036(8) -0.010(7) 0.008(6) -0.007(7) C41 0.055(11) 0.071(12) 0.033(8) -0.011(8) 0.028(8) -0.007(9) C51 0.057(12) 0.105(15) 0.022(8) 0.004(8) 0.012(7) -0.031(11) C61 0.033(9) 0.066(10) 0.039(9) 0.029(8) -0.002(7) -0.012(8) Cl61 0.060(3) 0.103(3) 0.069(3) 0.039(2) 0.000(2) -0.055(3) O27 0.026(5) 0.029(4) 0.019(4) 0.006(3) 0.000(3) -0.011(4) N17 0.018(6) 0.021(5) 0.037(6) 0.013(4) -0.004(4) -0.010(4) C27 0.053(9) 0.033(6) 0.011(6) 0.009(5) 0.004(6) -0.031(6) C37 0.046(9) 0.047(8) 0.016(6) 0.001(5) 0.009(6) -0.026(7) C47 0.061(11) 0.057(9) 0.024(7) -0.005(6) 0.012(7) -0.019(8) C57 0.095(14) 0.047(9) 0.020(7) 0.006(6) -0.009(8) -0.034(9) C67 0.029(8) 0.023(6) 0.036(7) 0.011(5) -0.012(6) -0.011(5) Cl67 0.043(2) 0.077(3) 0.057(2) 0.029(2) -0.0281(19) -0.017(2) O28 0.026(5) 0.023(4) 0.033(5) 0.010(3) 0.002(4) -0.003(4) N18 0.033(6) 0.024(5) 0.026(5) 0.006(4) 0.004(5) -0.015(5) C28 0.025(7) 0.020(5) 0.023(6) -0.002(4) -0.003(5) -0.006(5) C38 0.047(9) 0.029(7) 0.033(7) -0.007(5) -0.014(6) 0.003(6) C48 0.087(14) 0.032(8) 0.051(10) -0.012(7) -0.016(9) -0.021(8) C58 0.081(13) 0.036(8) 0.068(11) 0.003(7) -0.011(9) -0.036(9) C68 0.048(10) 0.029(7) 0.044(8) 0.009(6) -0.017(7) -0.019(7) Cl68 0.091(3) 0.064(3) 0.050(2) 0.0237(19) 0.003(2) -0.046(2) O26 0.018(4) 0.026(4) 0.017(4) 0.011(3) -0.001(3) -0.014(3) N16 0.020(6) 0.024(5) 0.023(5) 0.010(4) 0.000(4) -0.015(4) C26 0.020(7) 0.022(5) 0.018(6) 0.008(4) 0.001(5) -0.011(5) C36 0.035(8) 0.033(7) 0.027(7) -0.001(5) 0.006(6) -0.012(6) C46 0.071(11) 0.038(8) 0.042(8) -0.004(6) 0.009(7) -0.039(8) C56 0.084(13) 0.044(8) 0.041(8) -0.006(6) 0.013(8) -0.049(9) C66 0.050(10) 0.031(7) 0.038(8) 0.007(6) 0.009(7) -0.025(7) Cl66 0.140(5) 0.067(3) 0.055(2) -0.012(2) 0.056(3) -0.075(3) O24 0.021(5) 0.030(4) 0.025(4) 0.014(3) 0.004(4) -0.009(4) N14 0.020(6) 0.026(5) 0.037(6) 0.020(4) -0.008(5) -0.010(4) C24 0.030(8) 0.024(6) 0.035(7) 0.010(5) 0.006(6) -0.021(6) C34 0.040(9) 0.024(6) 0.041(8) 0.013(6) 0.005(6) -0.011(6) C44 0.056(11) 0.034(8) 0.045(9) 0.015(7) 0.003(8) 0.003(7) C54 0.037(9) 0.041(8) 0.029(7) 0.009(6) -0.003(6) 0.004(7) C64 0.015(7) 0.031(7) 0.047(8) 0.011(6) -0.006(6) -0.003(6) Cl64 0.047(2) 0.055(2) 0.048(2) 0.0107(17) -0.0212(18) -0.0142(18) O23 0.023(5) 0.014(4) 0.026(4) 0.011(3) 0.001(3) -0.005(3) N13 0.015(5) 0.032(5) 0.030(6) 0.010(4) -0.002(4) -0.018(4) C23 0.017(7) 0.012(5) 0.043(7) 0.010(5) 0.000(5) -0.008(5) C33 0.043(9) 0.033(7) 0.028(7) 0.001(5) 0.008(6) -0.027(6) C43 0.068(11) 0.042(8) 0.035(8) 0.005(6) 0.011(7) -0.035(8) C53 0.060(10) 0.022(6) 0.049(9) 0.023(6) -0.006(7) -0.023(7) C63 0.038(8) 0.016(5) 0.043(8) 0.000(5) 0.006(6) -0.015(5) Cl63 0.084(3) 0.0417(19) 0.065(3) -0.0057(17) 0.007(2) -0.045(2) O25 0.022(5) 0.019(4) 0.031(4) 0.004(3) 0.005(3) -0.014(3) N15 0.009(5) 0.025(5) 0.040(6) 0.004(4) 0.002(4) -0.004(4) C25 0.023(7) 0.017(5) 0.030(6) 0.005(4) 0.001(5) -0.010(5) C35 0.029(8) 0.053(8) 0.026(7) 0.000(6) 0.009(6) -0.026(7) C55 0.007(7) 0.051(8) 0.050(9) 0.003(6) -0.003(6) -0.013(6) C65 0.021(8) 0.050(8) 0.055(9) 0.015(7) -0.006(6) -0.022(7) Cl65 0.043(2) 0.068(2) 0.047(2) -0.0082(17) -0.0021(17) -0.0315(19) O29 0.034(7) 0.055(7) 0.091(9) 0.019(6) -0.006(6) -0.018(6) N19 0.036(10) 0.026(7) 0.047(10) 0.006(7) 0.003(7) -0.010(7) C29 0.039(13) 0.019(8) 0.088(17) -0.003(9) 0.007(11) -0.018(9) C39 0.051(15) 0.035(11) 0.078(17) 0.025(11) -0.004(12) -0.001(11) C49 0.035(14) 0.029(11) 0.15(3) 0.021(14) -0.009(16) 0.014(10) C59 0.043(15) 0.064(16) 0.10(2) -0.013(14) 0.029(14) -0.015(13) C69 0.065(16) 0.040(11) 0.056(14) -0.015(10) 0.027(11) -0.014(11) Cl69 0.084(5) 0.087(5) 0.066(4) -0.015(3) 0.029(3) -0.026(4) O29' 0.034(7) 0.055(7) 0.091(9) 0.019(6) -0.006(6) -0.018(6) C21S 0.07(2) 0.018(12) 0.06(2) 0.009(12) -0.005(16) -0.020(14) C22S 0.020(15) 0.041(16) 0.053(18) -0.003(13) 0.016(13) -0.005(12) N2S 0.049(18) 0.034(13) 0.13(3) -0.023(15) 0.050(17) -0.034(13) N1S 0.09(2) 0.11(3) 0.049(18) 0.027(17) -0.009(17) -0.07(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 Co5 O2C 2.037(9) . ? Co5 O1D 2.044(8) . ? Co5 O24 2.063(7) . ? Co5 O25 2.088(8) . ? Co5 O29 2.114(10) . ? Co5 O2 2.162(8) . ? Co3 O1A 2.006(8) . ? Co3 O1 2.018(7) . ? Co3 O1H 2.052(8) . ? Co3 N12 2.115(10) . ? Co3 O21 2.191(8) . ? Co3 O22 2.313(8) . ? Co4 O22 2.016(8) . ? Co4 O1C 2.039(8) . ? Co4 O24 2.040(8) . ? Co4 O2 2.089(7) . ? Co4 N13 2.108(9) . ? Co6 O27 2.023(8) . ? Co6 O2D 2.024(8) . ? Co6 O2 2.072(8) . ? Co6 N16 2.104(9) . ? Co6 O25 2.125(8) . ? Co6 O26 2.336(7) . ? Co7 O2A 1.948(9) . ? Co7 O1 1.986(7) . ? Co7 N18 2.050(10) . ? Co7 N17 2.075(10) . ? Co7 O27 2.404(8) . ? Co2 O2B 2.010(8) . ? Co2 O26 2.140(7) . ? Co2 N14 2.172(9) . ? Co2 O23 2.182(8) . ? Co2 N15 2.184(10) . ? Co2 O25 2.251(8) . ? Co1 O1B 2.007(8) . ? Co1 O1 2.060(7) . ? Co1 O21 2.071(8) . ? Co1 O28 2.075(8) . ? Co1 O23 2.156(7) . ? Co1 O26 2.183(7) . ? O2A C1A 1.272(15) . ? O1A C1A 1.251(14) . ? C1A C2A 1.502(17) . ? C2A C5A 1.508(15) . ? C2A C5A' 1.523(19) . ? C2A C3A' 1.523(19) . ? C2A C3A 1.526(16) . ? C2A C4A' 1.536(19) . ? C2A C4A 1.546(16) . ? O2C C1C 1.258(15) . ? O1C C1C 1.242(15) . ? C1C C2C 1.531(16) . ? C2C C5C 1.504(15) . ? C2C C3C 1.512(15) . ? C2C C5C' 1.514(19) . ? C2C C3C' 1.516(19) . ? C2C C4C' 1.521(19) . ? C2C C4C 1.523(15) . ? O2B C1B 1.243(13) . ? O1B C1B 1.251(13) . ? C1B C2B 1.543(15) . ? C2B C5B 1.522(17) . ? C2B C3B 1.529(17) . ? C2B C4B 1.546(17) . ? O1D C1D 1.285(14) . ? O2D C1D 1.244(14) . ? C1D C2D 1.555(16) . ? C2D C5D 1.502(15) . ? C2D C5D' 1.507(16) . ? C2D C4D 1.514(14) . ? C2D C4D' 1.516(15) . ? C2D C3D 1.517(14) . ? C2D C3D' 1.519(16) . ? O22 C22 1.293(13) . ? N12 C62 1.320(14) . ? N12 C22 1.389(16) . ? C22 C32 1.370(18) . ? C32 C42 1.38(2) . ? C42 C52 1.38(2) . ? C52 C62 1.365(19) . ? C62 Cl62 1.726(14) . ? O21 C21 1.273(13) . ? N11 C61 1.329(17) . ? N11 C21 1.365(15) . ? C21 C31 1.406(18) . ? C31 C41 1.370(18) . ? C41 C51 1.40(2) . ? C51 C61 1.33(2) . ? C61 Cl61 1.777(17) . ? O27 C27 1.280(13) . ? N17 C67 1.326(14) . ? N17 C27 1.365(15) . ? C27 C37 1.387(15) . ? C37 C47 1.346(18) . ? C47 C57 1.43(2) . ? C57 C67 1.360(17) . ? C67 Cl67 1.722(13) . ? O28 C28 1.301(13) . ? N18 C68 1.343(14) . ? N18 C28 1.395(13) . ? C28 C38 1.349(15) . ? C38 C48 1.373(19) . ? C48 C58 1.39(2) . ? C58 C68 1.347(18) . ? C68 Cl68 1.731(14) . ? O26 C26 1.348(12) . ? N16 C66 1.335(14) . ? N16 C26 1.369(13) . ? C26 C36 1.353(15) . ? C36 C46 1.377(16) . ? C46 C56 1.381(18) . ? C56 C66 1.335(18) . ? C66 Cl66 1.745(13) . ? O24 C24 1.292(13) . ? N14 C64 1.347(14) . ? N14 C24 1.357(15) . ? C24 C34 1.418(14) . ? C34 C44 1.361(18) . ? C44 C54 1.41(2) . ? C54 C64 1.354(16) . ? C64 Cl64 1.727(14) . ? O23 C23 1.361(11) . ? N13 C23 1.285(14) . ? N13 C63 1.326(13) . ? C23 C33 1.391(15) . ? C33 C43 1.390(15) . ? C43 C53 1.361(18) . ? C53 C63 1.388(17) . ? C63 Cl63 1.714(12) . ? O25 C25 1.335(13) . ? N15 C25 1.333(14) . ? N15 C65 1.349(15) . ? C25 C35 1.406(16) . ? C35 C45 1.407(18) . ? C45 C55 1.353(18) . ? C55 C65 1.401(17) . ? C65 Cl65 1.689(15) . ? O29 C29 1.22(2) . ? N19 C69 1.31(2) . ? N19 C29 1.34(2) . ? C29 C39 1.43(2) . ? C39 C49 1.30(3) . ? C49 C59 1.41(3) . ? C59 C69 1.40(3) . ? C69 Cl69 1.69(2) . ? C11S N1S 1.06(4) . ? C11S C21S 1.41(4) . ? C12S N2S 1.04(3) . ? C12S C22S 1.47(4) . ? 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 O2C Co5 O1D 91.1(4) . . ? O2C Co5 O24 89.9(3) . . ? O1D Co5 O24 178.8(4) . . ? O2C Co5 O25 170.8(3) . . ? O1D Co5 O25 96.3(3) . . ? O24 Co5 O25 82.8(3) . . ? O2C Co5 O29 91.7(4) . . ? O1D Co5 O29 91.8(4) . . ? O24 Co5 O29 87.6(4) . . ? O25 Co5 O29 93.5(4) . . ? O2C Co5 O2 95.5(3) . . ? O1D Co5 O2 99.7(3) . . ? O24 Co5 O2 80.9(3) . . ? O25 Co5 O2 77.9(3) . . ? O29 Co5 O2 166.3(4) . . ? O1A Co3 O1 101.0(3) . . ? O1A Co3 O1H 99.1(4) . . ? O1 Co3 O1H 152.3(3) . . ? O1A Co3 N12 103.1(4) . . ? O1 Co3 N12 94.4(3) . . ? O1H Co3 N12 99.4(4) . . ? O1A Co3 O21 84.1(3) . . ? O1 Co3 O21 79.1(3) . . ? O1H Co3 O21 84.2(3) . . ? N12 Co3 O21 171.2(4) . . ? O1A Co3 O22 163.1(3) . . ? O1 Co3 O22 79.4(3) . . ? O1H Co3 O22 86.8(3) . . ? N12 Co3 O22 60.2(3) . . ? O21 Co3 O22 112.3(3) . . ? O22 Co4 O1C 97.2(3) . . ? O22 Co4 O24 173.1(3) . . ? O1C Co4 O24 89.7(3) . . ? O22 Co4 O2 96.6(3) . . ? O1C Co4 O2 95.7(3) . . ? O24 Co4 O2 83.2(3) . . ? O22 Co4 N13 89.6(3) . . ? O1C Co4 N13 113.3(4) . . ? O24 Co4 N13 87.2(3) . . ? O2 Co4 N13 149.4(3) . . ? O27 Co6 O2D 99.9(3) . . ? O27 Co6 O2 94.9(3) . . ? O2D Co6 O2 93.6(3) . . ? O27 Co6 N16 88.9(3) . . ? O2D Co6 N16 103.6(4) . . ? O2 Co6 N16 161.5(3) . . ? O27 Co6 O25 163.2(3) . . ? O2D Co6 O25 96.1(3) . . ? O2 Co6 O25 79.1(3) . . ? N16 Co6 O25 92.1(3) . . ? O27 Co6 O26 88.2(3) . . ? O2D Co6 O26 161.8(3) . . ? O2 Co6 O26 101.9(3) . . ? N16 Co6 O26 60.0(3) . . ? O25 Co6 O26 77.8(3) . . ? O2A Co7 O1 101.5(3) . . ? O2A Co7 N18 103.0(4) . . ? O1 Co7 N18 121.5(3) . . ? O2A Co7 N17 104.0(4) . . ? O1 Co7 N17 108.7(3) . . ? N18 Co7 N17 115.3(4) . . ? O2A Co7 O27 159.9(3) . . ? O1 Co7 O27 77.5(3) . . ? N18 Co7 O27 94.3(3) . . ? N17 Co7 O27 58.5(3) . . ? O2B Co2 O26 95.7(3) . . ? O2B Co2 N14 100.1(4) . . ? O26 Co2 N14 160.8(3) . . ? O2B Co2 O23 93.5(3) . . ? O26 Co2 O23 76.3(3) . . ? N14 Co2 O23 91.8(3) . . ? O2B Co2 N15 99.1(4) . . ? O26 Co2 N15 92.9(3) . . ? N14 Co2 N15 95.3(4) . . ? O23 Co2 N15 164.3(3) . . ? O2B Co2 O25 157.9(3) . . ? O26 Co2 O25 79.5(3) . . ? N14 Co2 O25 89.7(3) . . ? O23 Co2 O25 106.1(3) . . ? N15 Co2 O25 60.0(3) . . ? O1B Co1 O1 174.2(3) . . ? O1B Co1 O21 96.7(3) . . ? O1 Co1 O21 81.0(3) . . ? O1B Co1 O28 89.1(3) . . ? O1 Co1 O28 85.7(3) . . ? O21 Co1 O28 91.7(3) . . ? O1B Co1 O23 96.0(3) . . ? O1 Co1 O23 89.3(3) . . ? O21 Co1 O23 88.4(3) . . ? O28 Co1 O23 174.9(3) . . ? O1B Co1 O26 93.6(3) . . ? O1 Co1 O26 90.1(3) . . ? O21 Co1 O26 162.1(3) . . ? O28 Co1 O26 103.1(3) . . ? O23 Co1 O26 75.9(3) . . ? Co6 O2 Co4 136.8(4) . . ? Co6 O2 Co5 92.8(3) . . ? Co4 O2 Co5 91.4(3) . . ? Co7 O1 Co3 117.3(3) . . ? Co7 O1 Co1 104.8(3) . . ? Co3 O1 Co1 102.7(3) . . ? C1A O2A Co7 134.1(7) . . ? C1A O1A Co3 131.5(8) . . ? O2A C1A O1A 124.3(11) . . ? O1A C1A C2A 120.6(12) . . ? O2A C1A C2A 115.0(11) . . ? C1A C2A C5A 110.8(14) . . ? C1A C2A C5A' 122(3) . . ? C5A C2A C5A' 123(4) . . ? C1A C2A C3A' 118(3) . . ? C5A C2A C3A' 58(2) . . ? C5A' C2A C3A' 109(2) . . ? C1A C2A C3A 112.8(13) . . ? C5A C2A C3A 109.2(13) . . ? C5A' C2A C3A 31(3) . . ? C3A' C2A C3A 129(3) . . ? C1A C2A C4A' 92(4) . . ? C5A C2A C4A' 48(3) . . ? C5A' C2A C4A' 107(2) . . ? C3A' C2A C4A' 106(2) . . ? C3A C2A C4A' 78(3) . . ? C1A C2A C4A 110.0(13) . . ? C5A C2A C4A 109.2(13) . . ? C5A' C2A C4A 73(3) . . ? C3A' C2A C4A 52(2) . . ? C3A C2A C4A 104.6(13) . . ? C4A' C2A C4A 154(3) . . ? C1C O2C Co5 127.4(8) . . ? C1C O1C Co4 128.4(8) . . ? O2C C1C O1C 125.8(11) . . ? O1C C1C C2C 118.9(12) . . ? O2C C1C C2C 115.3(11) . . ? C5C C2C C3C 111.0(12) . . ? C5C C2C C5C' 134(5) . . ? C3C C2C C5C' 36(4) . . ? C5C C2C C3C' 73(3) . . ? C3C C2C C3C' 137(4) . . ? C5C' C2C C3C' 109(2) . . ? C5C C2C C4C' 37(3) . . ? C3C C2C C4C' 77(4) . . ? C5C' C2C C4C' 108(2) . . ? C3C' C2C C4C' 107(2) . . ? C5C C2C C4C 109.2(12) . . ? C3C C2C C4C 107.7(12) . . ? C5C' C2C C4C 73(4) . . ? C3C' C2C C4C 39(4) . . ? C4C' C2C C4C 135(4) . . ? C5C C2C C1C 110.7(13) . . ? C3C C2C C1C 108.1(11) . . ? C5C' C2C C1C 112(5) . . ? C3C' C2C C1C 110(4) . . ? C4C' C2C C1C 111(4) . . ? C4C C2C C1C 110.1(12) . . ? C1B O2B Co2 131.4(7) . . ? C1B O1B Co1 130.9(8) . . ? O1B C1B O2B 125.7(10) . . ? O2B C1B C2B 119.2(10) . . ? O1B C1B C2B 115.1(10) . . ? C5B C2B C3B 110.2(11) . . ? C5B C2B C1B 110.1(10) . . ? C3B C2B C1B 109.2(9) . . ? C5B C2B C4B 110.0(10) . . ? C3B C2B C4B 109.8(12) . . ? C1B C2B C4B 107.4(10) . . ? C1D O1D Co5 125.9(8) . . ? C1D O2D Co6 133.7(8) . . ? O2D C1D O1D 123.6(11) . . ? O2D C1D C2D 118.4(10) . . ? O1D C1D C2D 118.0(10) . . ? C5D C2D C5D' 127.3(18) . . ? C5D C2D C4D 110.1(13) . . ? C5D' C2D C4D 88.3(15) . . ? C5D C2D C4D' 22.7(14) . . ? C5D' C2D C4D' 110.8(15) . . ? C4D C2D C4D' 129.5(18) . . ? C5D C2D C3D 110.8(13) . . ? C5D' C2D C3D 23.8(14) . . ? C4D C2D C3D 111.4(13) . . ? C4D' C2D C3D 90.6(15) . . ? C5D C2D C3D' 87.0(17) . . ? C5D' C2D C3D' 111.2(17) . . ? C4D C2D C3D' 25.4(15) . . ? C4D' C2D C3D' 108.6(16) . . ? C3D C2D C3D' 132(2) . . ? C5D C2D C1D 110.6(14) . . ? C5D' C2D C1D 111.8(17) . . ? C4D C2D C1D 104.3(12) . . ? C4D' C2D C1D 110.1(16) . . ? C3D C2D C1D 109.6(13) . . ? C3D' C2D C1D 104.2(19) . . ? C22 O22 Co4 130.9(8) . . ? C22 O22 Co3 90.0(7) . . ? Co4 O22 Co3 127.4(3) . . ? C62 N12 C22 118.8(11) . . ? C62 N12 Co3 143.4(10) . . ? C22 N12 Co3 96.1(7) . . ? O22 C22 C32 128.0(13) . . ? O22 C22 N12 112.3(11) . . ? C32 C22 N12 119.7(12) . . ? C22 C32 C42 118.8(15) . . ? C52 C42 C32 122.0(15) . . ? C62 C52 C42 115.6(13) . . ? N12 C62 C52 125.0(14) . . ? N12 C62 Cl62 115.6(11) . . ? C52 C62 Cl62 119.4(11) . . ? C21 O21 Co1 132.7(8) . . ? C21 O21 Co3 126.8(8) . . ? Co1 O21 Co3 96.6(3) . . ? C61 N11 C21 117.3(13) . . ? O21 C21 N11 117.7(11) . . ? O21 C21 C31 123.6(12) . . ? N11 C21 C31 118.8(12) . . ? C41 C31 C21 120.3(15) . . ? C31 C41 C51 120.1(15) . . ? C61 C51 C41 115.5(14) . . ? C51 C61 N11 128.0(16) . . ? C51 C61 Cl61 119.6(13) . . ? N11 C61 Cl61 112.4(13) . . ? C27 O27 Co6 135.7(8) . . ? C27 O27 Co7 87.6(7) . . ? Co6 O27 Co7 132.2(3) . . ? C67 N17 C27 118.7(11) . . ? C67 N17 Co7 140.9(9) . . ? C27 N17 Co7 100.1(7) . . ? O27 C27 N17 113.2(10) . . ? O27 C27 C37 126.6(13) . . ? N17 C27 C37 120.2(11) . . ? C47 C37 C27 120.1(14) . . ? C37 C47 C57 120.4(13) . . ? C67 C57 C47 115.7(13) . . ? N17 C67 C57 124.9(13) . . ? N17 C67 Cl67 116.1(10) . . ? C57 C67 Cl67 119.0(11) . . ? C28 O28 Co1 132.7(8) . . ? C68 N18 C28 115.9(10) . . ? C68 N18 Co7 138.3(8) . . ? C28 N18 Co7 104.6(7) . . ? O28 C28 C38 125.2(12) . . ? O28 C28 N18 112.3(9) . . ? C38 C28 N18 122.6(12) . . ? C28 C38 C48 119.7(13) . . ? C38 C48 C58 118.5(13) . . ? C68 C58 C48 119.3(14) . . ? N18 C68 C58 123.9(13) . . ? N18 C68 Cl68 114.6(9) . . ? C58 C68 Cl68 121.4(12) . . ? C26 O26 Co2 117.3(6) . . ? C26 O26 Co1 129.0(7) . . ? Co2 O26 Co1 95.6(3) . . ? C26 O26 Co6 89.9(6) . . ? Co2 O26 Co6 98.0(3) . . ? Co1 O26 Co6 124.9(3) . . ? C66 N16 C26 116.2(10) . . ? C66 N16 Co6 144.0(8) . . ? C26 N16 Co6 99.5(7) . . ? O26 C26 C36 126.7(10) . . ? O26 C26 N16 110.3(9) . . ? C36 C26 N16 122.8(11) . . ? C26 C36 C46 118.6(12) . . ? C36 C46 C56 119.1(12) . . ? C66 C56 C46 118.7(12) . . ? C56 C66 N16 124.4(12) . . ? C56 C66 Cl66 121.0(10) . . ? N16 C66 Cl66 114.6(10) . . ? C24 O24 Co4 134.5(7) . . ? C24 O24 Co5 129.5(7) . . ? Co4 O24 Co5 95.7(3) . . ? C64 N14 C24 118.4(10) . . ? C64 N14 Co2 127.8(9) . . ? C24 N14 Co2 112.9(7) . . ? O24 C24 N14 118.9(10) . . ? O24 C24 C34 120.8(11) . . ? N14 C24 C34 120.3(11) . . ? C44 C34 C24 119.0(13) . . ? C34 C44 C54 120.3(13) . . ? C64 C54 C44 117.3(12) . . ? N14 C64 C54 124.5(13) . . ? N14 C64 Cl64 116.5(9) . . ? C54 C64 Cl64 119.0(10) . . ? C23 O23 Co1 121.9(7) . . ? C23 O23 Co2 122.5(7) . . ? Co1 O23 Co2 95.1(3) . . ? C23 N13 C63 120.4(10) . . ? C23 N13 Co4 102.8(7) . . ? C63 N13 Co4 136.6(9) . . ? N13 C23 O23 114.5(11) . . ? N13 C23 C33 124.1(10) . . ? O23 C23 C33 121.4(10) . . ? C43 C33 C23 114.9(11) . . ? C53 C43 C33 122.0(13) . . ? C43 C53 C63 117.3(11) . . ? N13 C63 C53 121.2(11) . . ? N13 C63 Cl63 118.6(10) . . ? C53 C63 Cl63 120.1(9) . . ? C25 O25 Co5 128.0(7) . . ? C25 O25 Co6 121.5(6) . . ? Co5 O25 Co6 93.4(3) . . ? C25 O25 Co2 91.5(6) . . ? Co5 O25 Co2 120.5(3) . . ? Co6 O25 Co2 101.1(3) . . ? C25 N15 C65 119.9(11) . . ? C25 N15 Co2 94.5(7) . . ? C65 N15 Co2 144.7(9) . . ? N15 C25 O25 112.5(10) . . ? N15 C25 C35 123.2(11) . . ? O25 C25 C35 124.3(11) . . ? C25 C35 C45 115.9(12) . . ? C55 C45 C35 120.8(14) . . ? C45 C55 C65 120.2(13) . . ? N15 C65 C55 119.9(13) . . ? N15 C65 Cl65 118.4(10) . . ? C55 C65 Cl65 121.7(11) . . ? C29 O29 Co5 128.0(13) . . ? C69 N19 C29 124.7(17) . . ? O29 C29 N19 116.8(17) . . ? O29 C29 C39 126(2) . . ? N19 C29 C39 116.8(19) . . ? C49 C39 C29 119(2) . . ? C39 C49 C59 124(2) . . ? C69 C59 C49 116(2) . . ? N19 C69 C59 120(2) . . ? N19 C69 Cl69 121.2(17) . . ? C59 C69 Cl69 118.9(17) . . ? N1S C11S C21S 171(4) . . ? N2S C12S C22S 178(3) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 70.24 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 1.470 _refine_diff_density_min -1.260 _refine_diff_density_rms 0.159