# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1702 data_suclf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H21 Co3 O19' _chemical_formula_weight 802.21 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Ticlinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 7.6191(15) _cell_length_b 12.213(2) _cell_length_c 18.533(4) _cell_angle_alpha 70.909(2) _cell_angle_beta 85.774(2) _cell_angle_gamma 83.702(2) _cell_volume 1618.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.600 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.809361 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6703 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0864 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 26.34 _reflns_number_total 6324 _reflns_number_gt 4559 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'TITAN and SHELXTL-PC' _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 w=1/[\s^2^(Fo^2^)+(0.1323P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_number_reflns 6324 _refine_ls_number_parameters 640 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.1896 _refine_ls_wR_factor_gt 0.1807 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.014 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O12 O 0.8627(13) 0.0024(7) 1.2007(5) 0.025(2) Uiso 1 d . . . C173 C 0.804(2) 0.2683(13) 1.3505(9) 0.043(4) Uani 1 d . . . H17A H 0.8223 0.3188 1.2977 0.064 Uiso 1 calc R . . H17B H 0.9191 0.2350 1.3723 0.064 Uiso 1 calc R . . H17C H 0.7418 0.3139 1.3808 0.064 Uiso 1 calc R . . O172 O 0.5503(17) 0.1678(9) 1.3747(6) 0.049(3) Uani 1 d . . . C172 C 0.700(2) 0.1749(11) 1.3514(7) 0.024(3) Uiso 1 d . . . O171 O 0.7890(16) 0.1046(8) 1.3191(5) 0.036(3) Uani 1 d . . . C171 C 0.699(2) 0.0048(12) 1.3139(7) 0.030(3) Uiso 1 d . . . H17D H 0.5790 0.0050 1.3385 0.036 Uiso 1 calc R . . H17E H 0.7668 -0.0696 1.3407 0.036 Uiso 1 calc R . . C17 C 0.6863(19) 0.0167(12) 1.2297(7) 0.025(3) Uani 1 d . . . H17 H 0.6285 0.0950 1.2010 0.030 Uiso 1 calc R . . C162 C 0.163(2) -0.1206(13) 1.3367(8) 0.037(4) Uani 1 d . . . H16A H 0.0892 -0.1250 1.2968 0.055 Uiso 1 calc R . . H16B H 0.1482 -0.0414 1.3397 0.055 Uiso 1 calc R . . H16C H 0.1267 -0.1754 1.3860 0.055 Uiso 1 calc R . . O162 O 0.4411(17) -0.2341(9) 1.3494(6) 0.051(3) Uani 1 d . . . C161 C 0.345(2) -0.1498(13) 1.3189(8) 0.032(4) Uiso 1 d . . . O161 O 0.4012(14) -0.0640(8) 1.2523(5) 0.030(2) Uani 1 d . . . C16 C 0.582(2) -0.0778(12) 1.2244(8) 0.028(3) Uiso 1 d . . . H16 H 0.6382 -0.1552 1.2551 0.034 Uiso 1 calc R . . C152 C 0.289(3) -0.2598(16) 1.0916(11) 0.059(5) Uani 1 d . . . H15A H 0.2202 -0.2947 1.1387 0.089 Uiso 1 calc R . . H15B H 0.3915 -0.3140 1.0874 0.089 Uiso 1 calc R . . H15C H 0.2156 -0.2433 1.0476 0.089 Uiso 1 calc R . . O152 O 0.2912(18) -0.0531(10) 1.0612(7) 0.059(4) Uani 1 d . . . C151 C 0.353(2) -0.1487(14) 1.0935(9) 0.041(4) Uiso 1 d . . . O151 O 0.4942(15) -0.1701(7) 1.1364(5) 0.033(3) Uani 1 d . . . C15 C 0.581(2) -0.0718(12) 1.1399(8) 0.031(3) Uiso 1 d . . . H15 H 0.5155 0.0026 1.1094 0.037 Uiso 1 calc R . . C142 C 0.788(4) -0.1204(17) 0.9207(10) 0.080(8) Uani 1 d . . . H14A H 0.8983 -0.1480 0.8991 0.120 Uiso 1 calc R . . H14B H 0.7699 -0.0354 0.8996 0.120 Uiso 1 calc R . . H14C H 0.6889 -0.1545 0.9076 0.120 Uiso 1 calc R . . O142 O 0.840(2) -0.2532(10) 1.0479(7) 0.066(4) Uani 1 d . . . C141 C 0.797(3) -0.1557(15) 1.0049(9) 0.046(4) Uiso 1 d . . . O141 O 0.7663(16) -0.0628(8) 1.0290(5) 0.037(3) Uani 1 d . . . C14 C 0.765(2) -0.0795(12) 1.1091(7) 0.026(3) Uiso 1 d . . . H14 H 0.8228 -0.1588 1.1355 0.031 Uiso 1 calc R . . C13 C 0.872(2) 0.0096(11) 1.1205(7) 0.027(3) Uiso 1 d . . . H13 H 0.9978 -0.0049 1.1040 0.033 Uiso 1 calc R . . O11 O 0.8022(13) 0.1206(7) 1.0744(5) 0.026(2) Uiso 1 d . . . C12 C 0.928(2) 0.2087(12) 1.0602(8) 0.035(4) Uiso 1 d . . . H12A H 1.0461 0.1787 1.0455 0.042 Uiso 1 calc R . . H12B H 0.9372 0.2307 1.1065 0.042 Uiso 1 calc R . . C11 C 0.856(2) 0.3110(11) 0.9964(8) 0.032(4) Uani 1 d . . . Co11 Co 0.7930(3) 0.32273(14) 0.89815(10) 0.0277(5) Uani 1 d . . . C111 C 0.970(3) 0.2253(14) 0.8785(9) 0.042(4) Uiso 1 d . . . O111 O 1.080(2) 0.1592(12) 0.8702(8) 0.077(5) Uani 1 d . . . C112 C 0.633(2) 0.2207(13) 0.9129(8) 0.036(4) Uiso 1 d . . . O112 O 0.5338(18) 0.1514(10) 0.9241(6) 0.051(3) Uani 1 d . . . C113 C 0.731(2) 0.4265(13) 0.8045(9) 0.034(4) Uiso 1 d . . . O113 O 0.697(2) 0.4925(10) 0.7468(7) 0.069(4) Uani 1 d . . . Co12 Co 0.6557(3) 0.41758(15) 0.99060(11) 0.0321(5) Uani 1 d . . . C121 C 0.493(2) 0.3151(13) 1.0323(8) 0.035(4) Uiso 1 d . . . O121 O 0.3901(16) 0.2517(10) 1.0577(6) 0.045(3) Uani 1 d . . . C122 C 0.679(3) 0.4640(16) 1.0714(11) 0.054(5) Uiso 1 d . . . O122 O 0.706(3) 0.4886(16) 1.1230(9) 0.113(8) Uani 1 d . . . C123 C 0.522(3) 0.5443(17) 0.9300(11) 0.055(5) Uiso 1 d . . . O123 O 0.438(2) 0.6188(12) 0.8916(9) 0.091(6) Uani 1 d . . . Co13 Co 0.9603(3) 0.45138(15) 0.94052(11) 0.0306(5) Uani 1 d . . . C131 C 1.162(3) 0.4093(15) 0.8985(10) 0.047(4) Uiso 1 d . . . O131 O 1.2831(18) 0.3788(13) 0.8691(7) 0.065(4) Uani 1 d . . . C132 C 1.056(2) 0.4837(13) 1.0154(9) 0.038(4) Uiso 1 d . . . O132 O 1.121(2) 0.4993(11) 1.0644(7) 0.071(4) Uani 1 d . . . C133 C 0.901(2) 0.5949(14) 0.8702(9) 0.036(4) Uiso 1 d . . . O133 O 0.860(2) 0.6802(9) 0.8258(6) 0.058(4) Uani 1 d . . . O22 O 0.4388(13) -0.5444(7) 1.4092(5) 0.027(2) Uiso 1 d . . . C273 C 0.194(2) -0.7832(14) 1.2255(9) 0.042(4) Uani 1 d . . . H27A H 0.2495 -0.8233 1.1905 0.063 Uiso 1 calc R . . H27B H 0.0816 -0.7414 1.2055 0.063 Uiso 1 calc R . . H27C H 0.1727 -0.8403 1.2758 0.063 Uiso 1 calc R . . O272 O 0.4575(18) -0.6878(10) 1.2070(6) 0.052(3) Uani 1 d . . . C272 C 0.313(2) -0.6994(12) 1.2326(8) 0.028(3) Uiso 1 d . . . O271 O 0.2301(15) -0.6365(8) 1.2764(6) 0.035(3) Uani 1 d . . . C271 C 0.335(2) -0.5596(12) 1.2956(7) 0.028(3) Uiso 1 d . . . H27D H 0.3151 -0.4797 1.2594 0.033 Uiso 1 calc R . . H27E H 0.4623 -0.5860 1.2922 0.033 Uiso 1 calc R . . C27 C 0.284(2) -0.5602(12) 1.3757(8) 0.029(3) Uiso 1 d . . . H27 H 0.2418 -0.6376 1.4057 0.035 Uiso 1 calc R . . C262 C -0.254(2) -0.4091(12) 1.2651(8) 0.036(4) Uani 1 d . . . H26A H -0.3423 -0.4148 1.3071 0.054 Uiso 1 calc R . . H26B H -0.2397 -0.4823 1.2534 0.054 Uiso 1 calc R . . H26C H -0.2933 -0.3453 1.2198 0.054 Uiso 1 calc R . . O262 O -0.003(2) -0.3012(10) 1.2569(6) 0.063(4) Uani 1 d . . . C261 C -0.084(2) -0.3864(13) 1.2877(9) 0.036(4) Uiso 1 d . . . O261 O -0.0165(14) -0.4765(7) 1.3476(5) 0.033(3) Uani 1 d . . . C26 C 0.142(2) -0.4651(12) 1.3805(7) 0.026(3) Uiso 1 d . . . H26 H 0.1849 -0.3874 1.3524 0.032 Uiso 1 calc R . . C252 C -0.282(3) -0.2929(16) 1.5061(13) 0.067(6) Uani 1 d . . . H25A H -0.3602 -0.2720 1.4631 0.100 Uiso 1 calc R . . H25B H -0.2056 -0.2303 1.4991 0.100 Uiso 1 calc R . . H25C H -0.3530 -0.3042 1.5538 0.100 Uiso 1 calc R . . O252 O -0.2088(17) -0.4967(10) 1.5463(6) 0.054(3) Uani 1 d . . . C251 C -0.174(2) -0.3994(13) 1.5096(8) 0.035(4) Uiso 1 d . . . O251 O -0.0263(14) -0.3772(8) 1.4681(5) 0.033(2) Uani 1 d . . . C25 C 0.100(2) -0.4745(12) 1.4644(7) 0.025(3) Uiso 1 d . . . H25 H 0.0502 -0.5500 1.4925 0.030 Uiso 1 calc R . . C242 C 0.196(3) -0.4409(15) 1.6919(9) 0.059(6) Uani 1 d . . . H24A H 0.2000 -0.3759 1.7116 0.089 Uiso 1 calc R . . H24B H 0.2854 -0.5037 1.7166 0.089 Uiso 1 calc R . . H24C H 0.0788 -0.4696 1.7030 0.089 Uiso 1 calc R . . O242 O 0.261(2) -0.3024(9) 1.5706(6) 0.065(4) Uani 1 d . . . C241 C 0.234(2) -0.4004(14) 1.6070(9) 0.038(4) Uiso 1 d . . . O241 O 0.2321(15) -0.4884(7) 1.5796(5) 0.032(3) Uani 1 d . . . C24 C 0.2684(19) -0.4666(11) 1.4994(7) 0.024(3) Uiso 1 d . . . H24 H 0.3093 -0.3871 1.4756 0.028 Uiso 1 calc R . . C23 C 0.410(2) -0.5566(11) 1.4889(7) 0.026(3) Uiso 1 d . . . H23 H 0.5225 -0.5441 1.5086 0.031 Uiso 1 calc R . . C22 C 0.505(2) -0.7582(11) 1.5405(7) 0.026(3) Uiso 1 d . . . H22A H 0.6111 -0.7346 1.5575 0.031 Uiso 1 calc R . . H22B H 0.5354 -0.7710 1.4908 0.031 Uiso 1 calc R . . O21 O 0.3616(13) -0.6680(7) 1.5322(5) 0.022(2) Uiso 1 d . . . C21 C 0.4507(19) -0.8666(11) 1.5976(7) 0.023(3) Uani 1 d . . . Co21 Co 0.3482(3) -0.89563(15) 1.69778(10) 0.0311(5) Uani 1 d . . . C211 C 0.481(3) -0.8003(15) 1.7243(9) 0.045(4) Uiso 1 d . . . O211 O 0.560(2) -0.7398(12) 1.7373(7) 0.072(4) Uani 1 d . . . C212 C 0.145(3) -0.7941(14) 1.6873(9) 0.039(4) Uiso 1 d . . . O212 O 0.0298(18) -0.7318(10) 1.6802(7) 0.058(4) Uani 1 d . . . C213 C 0.298(3) -1.0142(15) 1.7850(10) 0.046(4) Uiso 1 d . . . O213 O 0.264(3) -1.0887(11) 1.8383(7) 0.092(6) Uani 1 d . . . Co22 Co 0.5774(3) -1.01128(15) 1.64349(11) 0.0294(5) Uani 1 d . . . C221 C 0.719(2) -1.0173(12) 1.5636(8) 0.033(4) Uiso 1 d . . . O221 O 0.8046(17) -1.0106(8) 1.5099(6) 0.042(3) Uani 1 d . . . C222 C 0.737(2) -0.9877(13) 1.7026(9) 0.036(4) Uiso 1 d . . . O222 O 0.8347(17) -0.9682(11) 1.7372(7) 0.053(3) Uani 1 d . . . C223 C 0.542(2) -1.1623(14) 1.6927(9) 0.041(4) Uiso 1 d . . . O223 O 0.5166(19) -1.2595(9) 1.7221(7) 0.062(4) Uani 1 d . . . Co23 Co 0.2762(3) -0.96697(15) 1.59372(10) 0.0286(5) Uani 1 d . . . C231 C 0.344(2) -1.0190(13) 1.5151(9) 0.035(4) Uiso 1 d . . . O231 O 0.3793(17) -1.0560(10) 1.4666(6) 0.050(3) Uani 1 d . . . C232 C 0.104(3) -0.8545(15) 1.5489(10) 0.044(4) Uiso 1 d . . . O232 O -0.0029(18) -0.7855(9) 1.5198(7) 0.055(3) Uani 1 d . . . C233 C 0.156(3) -1.0879(14) 1.6543(10) 0.044(4) Uiso 1 d . . . O233 O 0.080(2) -1.1625(10) 1.6922(7) 0.066(4) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C173 0.046(13) 0.036(9) 0.044(10) -0.010(7) 0.000(8) -0.008(8) O172 0.060(10) 0.034(6) 0.053(7) -0.019(5) 0.008(6) 0.004(6) O171 0.048(8) 0.029(5) 0.029(5) -0.008(4) 0.008(5) -0.012(5) C17 0.017(9) 0.028(7) 0.027(7) -0.003(6) -0.006(6) -0.008(6) C162 0.037(12) 0.043(9) 0.029(8) -0.006(7) 0.012(7) -0.025(8) O162 0.055(9) 0.027(6) 0.057(7) -0.002(5) 0.015(6) 0.004(6) O161 0.033(7) 0.025(5) 0.024(5) 0.004(4) 0.006(4) -0.005(4) C152 0.063(16) 0.062(13) 0.054(11) -0.015(9) -0.011(10) -0.013(11) O152 0.057(10) 0.049(7) 0.063(8) -0.006(6) -0.012(7) -0.001(7) O151 0.044(8) 0.020(5) 0.032(5) -0.002(4) -0.012(5) -0.003(5) C142 0.14(3) 0.064(13) 0.048(11) -0.039(10) 0.002(14) -0.008(15) O142 0.105(13) 0.036(7) 0.062(8) -0.026(6) -0.011(8) 0.016(7) O141 0.057(9) 0.025(5) 0.023(5) -0.002(4) 0.002(5) 0.000(5) C11 0.051(12) 0.019(7) 0.026(7) -0.009(6) 0.002(7) -0.004(7) Co11 0.0381(15) 0.0230(10) 0.0204(9) -0.0047(8) 0.0005(9) -0.0046(9) O111 0.078(12) 0.073(9) 0.080(10) -0.036(8) 0.015(9) 0.021(8) O112 0.063(10) 0.040(7) 0.049(7) -0.007(5) -0.006(6) -0.021(6) O113 0.117(14) 0.037(7) 0.045(7) 0.002(6) -0.026(8) -0.003(8) Co12 0.0347(15) 0.0242(11) 0.0355(11) -0.0087(8) 0.0087(10) -0.0049(9) O121 0.039(8) 0.060(7) 0.040(6) -0.016(5) 0.007(5) -0.028(6) O122 0.154(18) 0.156(15) 0.083(11) -0.095(11) 0.074(11) -0.116(14) O123 0.058(11) 0.053(8) 0.110(12) 0.030(8) 0.012(9) 0.026(8) Co13 0.0323(14) 0.0240(10) 0.0323(11) -0.0029(8) -0.0010(9) -0.0075(9) O131 0.035(9) 0.105(11) 0.049(8) -0.025(7) 0.001(6) 0.008(8) O132 0.091(13) 0.060(8) 0.063(8) -0.010(7) -0.035(8) -0.022(8) O133 0.092(11) 0.029(6) 0.043(7) 0.005(5) -0.008(7) -0.009(7) C273 0.044(13) 0.056(10) 0.037(9) -0.030(8) 0.020(8) -0.015(9) O272 0.057(10) 0.059(8) 0.042(7) -0.017(6) 0.007(6) -0.019(7) O271 0.034(7) 0.035(6) 0.041(6) -0.017(5) -0.004(5) -0.002(5) C262 0.043(12) 0.020(8) 0.037(9) 0.000(6) 0.001(8) -0.003(7) O262 0.083(11) 0.038(7) 0.048(7) 0.022(5) -0.024(7) -0.021(7) O261 0.034(7) 0.018(5) 0.035(5) 0.006(4) -0.008(5) 0.001(4) C252 0.052(16) 0.060(13) 0.096(16) -0.039(12) -0.003(12) 0.004(11) O252 0.044(9) 0.042(7) 0.056(7) 0.007(6) 0.012(6) -0.004(6) O251 0.031(7) 0.022(5) 0.042(6) -0.007(4) 0.002(5) -0.004(4) C242 0.11(2) 0.042(10) 0.022(8) -0.012(7) 0.014(10) -0.017(11) O242 0.131(14) 0.020(6) 0.044(7) -0.012(5) 0.025(7) -0.020(7) O241 0.044(8) 0.020(5) 0.029(5) -0.004(4) 0.003(5) -0.005(5) C21 0.013(9) 0.028(7) 0.029(7) -0.012(6) 0.008(6) -0.004(6) Co21 0.0421(16) 0.0251(10) 0.0214(10) -0.0035(8) 0.0044(9) 0.0003(9) O211 0.097(13) 0.066(9) 0.069(9) -0.040(8) -0.009(8) -0.017(8) O212 0.047(10) 0.046(7) 0.065(8) -0.004(6) 0.004(7) 0.016(7) O213 0.158(18) 0.049(8) 0.041(7) 0.012(6) 0.039(9) -0.004(9) Co22 0.0318(14) 0.0212(10) 0.0322(11) -0.0055(8) -0.0015(9) 0.0013(9) O221 0.058(9) 0.029(6) 0.034(6) -0.005(4) 0.000(6) 0.001(5) O222 0.042(9) 0.069(8) 0.065(8) -0.043(7) -0.007(6) -0.006(6) O223 0.080(11) 0.024(6) 0.067(8) 0.006(5) -0.010(7) -0.006(6) Co23 0.0318(15) 0.0224(10) 0.0301(11) -0.0059(8) 0.0002(9) -0.0048(9) O231 0.072(10) 0.046(7) 0.036(6) -0.017(5) 0.011(6) -0.016(6) O232 0.048(9) 0.035(7) 0.075(8) -0.004(6) -0.022(7) -0.001(6) O233 0.086(12) 0.040(7) 0.061(8) -0.005(6) 0.038(8) -0.017(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O12 C17 1.425(17) . y O12 C13 1.456(15) . y C173 C172 1.46(2) . ? O172 C172 1.189(18) . ? C172 O171 1.306(16) . ? O171 C171 1.496(17) . y C171 C17 1.528(18) . y C17 C16 1.505(19) . y C162 C161 1.43(2) . ? O162 C161 1.198(18) . ? C161 O161 1.408(16) . ? O161 C16 1.444(18) . y C16 C15 1.545(19) . y C152 C151 1.50(2) . ? O152 C151 1.185(19) . ? C151 O151 1.34(2) . ? O151 C15 1.453(17) . y C15 C14 1.48(2) . y C142 C141 1.48(2) . ? O142 C141 1.223(19) . ? C141 O141 1.342(19) . ? O141 C14 1.430(15) . y C14 C13 1.504(19) . y C13 O11 1.415(16) . y O11 C12 1.463(18) . y C12 C11 1.49(2) . y C11 Co11 1.874(14) . y C11 Co12 1.880(16) . y C11 Co13 1.912(14) . y Co11 C111 1.796(18) . ? Co11 C112 1.782(17) . ? Co11 C113 1.841(16) . ? Co11 Co12 2.478(2) . y Co11 Co13 2.471(3) . y C111 O111 1.14(2) . ? C112 O112 1.154(18) . ? C113 O113 1.138(17) . ? Co12 C122 1.791(19) . ? Co12 C121 1.810(17) . ? Co12 C123 1.84(2) . ? Co12 Co13 2.461(3) . y C121 O121 1.127(18) . ? C122 O122 1.13(2) . ? C123 O123 1.12(2) . ? Co13 C131 1.77(2) . ? Co13 C132 1.783(17) . ? Co13 C133 1.841(16) . ? C131 O131 1.13(2) . ? C132 O132 1.145(19) . ? C133 O133 1.127(17) . ? O22 C27 1.433(18) . y O22 C23 1.438(15) . y C273 C272 1.48(2) . ? O272 C272 1.171(19) . ? C272 O271 1.369(16) . ? O271 C271 1.441(17) . y C271 C27 1.505(18) . y C27 C26 1.519(19) . y C262 C261 1.47(2) . ? O262 C261 1.222(19) . ? C261 O261 1.368(18) . ? O261 C26 1.431(18) . y C26 C25 1.533(18) . y C252 C251 1.45(2) . ? O252 C251 1.207(18) . ? C251 O251 1.316(18) . ? O251 C25 1.461(16) . y C25 C24 1.51(2) . y C242 C241 1.50(2) . ? O242 C241 1.199(18) . ? C241 O241 1.332(17) . ? O241 C24 1.433(15) . y C24 C23 1.503(19) . y C23 O21 1.408(15) . y C22 O21 1.444(16) . y C22 C21 1.478(18) . y C21 Co21 1.897(13) . y C21 Co22 1.882(14) . y C21 Co23 1.924(14) . y Co21 C211 1.83(2) . ? Co21 C213 1.831(18) . ? Co21 C212 1.853(19) . ? Co21 Co22 2.487(3) . y Co21 Co23 2.478(3) . y C211 O211 1.09(2) . ? C212 O212 1.083(19) . ? C213 O213 1.138(19) . ? Co22 C221 1.785(15) . ? Co22 C222 1.798(17) . ? Co22 C223 1.811(17) . ? Co22 Co23 2.475(3) . y C221 O221 1.132(17) . ? C222 O222 1.112(19) . ? C223 O223 1.164(18) . ? Co23 C231 1.793(15) . ? Co23 C232 1.822(19) . ? Co23 C233 1.825(18) . ? C231 O231 1.135(16) . ? C232 O232 1.13(2) . ? C233 O233 1.139(19) . ? 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 C17 O12 C13 113.0(10) . . y O172 C172 O171 124.9(13) . . ? O172 C172 C173 124.3(14) . . ? O171 C172 C173 110.7(14) . . ? C172 O171 C171 117.5(12) . . ? O171 C171 C17 108.9(10) . . y O12 C17 C16 110.3(11) . . y O12 C17 C171 106.6(11) . . y C16 C17 C171 108.7(11) . . y O162 C161 O161 120.7(15) . . ? O162 C161 C162 129.8(15) . . ? O161 C161 C162 109.4(13) . . ? C161 O161 C16 118.0(11) . . ? O161 C16 C17 111.3(11) . . y O161 C16 C15 108.8(12) . . y C17 C16 C15 108.8(11) . . y O152 C151 O151 122.6(16) . . ? O152 C151 C152 126.5(18) . . ? O151 C151 C152 110.9(15) . . ? C151 O151 C15 118.3(11) . . ? O151 C15 C14 109.2(11) . . y O151 C15 C16 108.3(11) . . y C14 C15 C16 109.5(12) . . y O142 C141 O141 122.5(15) . . ? O142 C141 C142 126.5(16) . . ? O141 C141 C142 110.7(15) . . ? C141 O141 C14 119.1(11) . . ? O141 C14 C15 110.1(12) . . y O141 C14 C13 108.1(11) . . y C15 C14 C13 112.7(12) . . y O11 C13 O12 110.7(10) . . y O11 C13 C14 107.8(12) . . y O12 C13 C14 110.2(10) . . y C13 O11 C12 112.4(11) . . y O11 C12 C11 106.1(13) . . y C12 C11 Co11 130.9(10) . . y C12 C11 Co12 132.2(11) . . y Co11 C11 Co12 82.6(6) . . y C12 C11 Co13 129.8(12) . . y Co11 C11 Co13 81.5(5) . . y Co12 C11 Co13 80.9(5) . . y C112 Co11 C111 93.3(8) . . ? C112 Co11 C113 100.8(7) . . ? C111 Co11 C113 105.7(7) . . ? C112 Co11 C11 105.0(7) . . ? C111 Co11 C11 97.7(7) . . ? C113 Co11 C11 143.8(6) . . ? C112 Co11 Co13 152.5(5) . . ? C111 Co11 Co13 100.6(6) . . ? C113 Co11 Co13 98.0(5) . . ? C11 Co11 Co13 49.9(4) . . ? C112 Co11 Co12 96.3(5) . . ? C111 Co11 Co12 146.5(5) . . ? C113 Co11 Co12 103.8(5) . . ? C11 Co11 Co12 48.8(5) . . ? Co13 Co11 Co12 59.66(8) . . y O111 C111 Co11 176.0(15) . . ? O112 C112 Co11 177.4(15) . . ? O113 C113 Co11 178.0(15) . . ? C122 Co12 C121 98.3(8) . . ? C122 Co12 C123 100.4(8) . . ? C121 Co12 C123 102.3(8) . . ? C122 Co12 C11 101.7(8) . . ? C121 Co12 C11 98.7(7) . . ? C123 Co12 C11 146.7(7) . . ? C122 Co12 Co13 94.2(7) . . ? C121 Co12 Co13 148.3(5) . . ? C123 Co12 Co13 103.9(6) . . ? C11 Co12 Co13 50.1(4) . . ? C122 Co12 Co11 148.5(7) . . ? C121 Co12 Co11 96.8(5) . . ? C123 Co12 Co11 103.1(6) . . ? C11 Co12 Co11 48.6(4) . . ? Co13 Co12 Co11 60.03(8) . . y O121 C121 Co12 179.4(15) . . ? O122 C122 Co12 175(2) . . ? O123 C123 Co12 177.3(18) . . ? C131 Co13 C132 96.5(8) . . ? C131 Co13 C133 100.7(8) . . ? C132 Co13 C133 104.3(7) . . ? C131 Co13 C11 106.5(7) . . ? C132 Co13 C11 101.1(7) . . ? C133 Co13 C11 140.1(8) . . ? C131 Co13 Co12 151.3(6) . . ? C132 Co13 Co12 102.5(5) . . ? C133 Co13 Co12 95.3(6) . . ? C11 Co13 Co12 49.0(5) . . ? C131 Co13 Co11 92.9(6) . . ? C132 Co13 Co11 149.7(5) . . ? C133 Co13 Co11 102.1(5) . . ? C11 Co13 Co11 48.6(4) . . ? Co12 Co13 Co11 60.31(8) . . y O131 C131 Co13 174.7(17) . . ? O132 C132 Co13 176.7(15) . . ? O133 C133 Co13 176.7(15) . . ? C27 O22 C23 112.5(11) . . y O272 C272 O271 123.3(14) . . ? O272 C272 C273 127.0(14) . . ? O271 C272 C273 109.6(13) . . ? C272 O271 C271 116.4(12) . . ? O271 C271 C27 108.7(12) . . y O22 C27 C271 107.5(12) . . y O22 C27 C26 107.9(11) . . y C271 C27 C26 114.4(12) . . y O262 C261 O261 121.0(16) . . ? O262 C261 C262 126.7(15) . . ? O261 C261 C262 112.2(13) . . ? C261 O261 C26 119.5(11) . . ? O261 C26 C27 110.3(11) . . y O261 C26 C25 108.6(12) . . y C27 C26 C25 109.7(11) . . y O252 C251 O251 123.1(15) . . ? O252 C251 C252 126.0(17) . . ? O251 C251 C252 110.9(15) . . ? C251 O251 C25 118.8(11) . . ? O251 C25 C24 108.7(10) . . y O251 C25 C26 109.2(11) . . y C24 C25 C26 108.3(12) . . y O242 C241 O241 126.2(14) . . ? O242 C241 C242 123.7(14) . . ? O241 C241 C242 110.1(13) . . ? C241 O241 C24 118.1(11) . . ? O241 C24 C23 108.7(10) . . y O241 C24 C25 107.8(11) . . y C23 C24 C25 110.8(11) . . y O21 C23 O22 111.9(10) . . y O21 C23 C24 109.0(11) . . y O22 C23 C24 110.3(11) . . y O21 C22 C21 108.9(12) . . y C23 O21 C22 113.2(10) . . y C22 C21 Co22 131.6(11) . . y C22 C21 Co21 131.1(9) . . y Co22 C21 Co21 82.3(5) . . y C22 C21 Co23 130.7(11) . . y Co21 C21 Co23 80.8(5) . . y Co22 C21 Co23 81.1(5) . . y C211 Co21 C213 107.3(8) . . ? C211 Co21 C212 93.9(8) . . ? C213 Co21 C212 102.9(8) . . ? C211 Co21 C21 95.4(7) . . ? C213 Co21 C21 142.0(7) . . ? C212 Co21 C21 105.5(6) . . ? C211 Co21 Co23 145.4(5) . . ? C213 Co21 Co23 103.8(5) . . ? C212 Co21 Co23 93.5(5) . . ? C21 Co21 Co23 50.1(4) . . ? C211 Co21 Co22 101.7(6) . . ? C213 Co21 Co22 96.3(5) . . ? C212 Co21 Co22 150.4(5) . . ? C21 Co21 Co22 48.6(4) . . ? Co23 Co21 Co22 59.79(8) . . y O211 C211 Co21 177.0(16) . . ? O212 C212 Co21 177.6(16) . . ? O213 C213 Co21 178.2(18) . . ? C221 Co22 C222 99.3(7) . . ? C221 Co22 C223 103.4(7) . . ? C222 Co22 C223 101.1(7) . . ? C221 Co22 C21 98.5(6) . . ? C222 Co22 C21 107.0(6) . . ? C223 Co22 C21 140.8(7) . . ? C221 Co22 Co23 104.9(5) . . ? C222 Co22 Co23 148.6(5) . . ? C223 Co22 Co23 92.4(6) . . ? C21 Co22 Co23 50.2(4) . . ? C221 Co22 Co21 147.4(5) . . ? C222 Co22 Co21 89.0(5) . . ? C223 Co22 Co21 105.8(5) . . ? C21 Co22 Co21 49.1(4) . . ? Co23 Co22 Co21 59.91(8) . . y O221 C221 Co22 173.7(13) . . ? O222 C222 Co22 176.9(14) . . ? O223 C223 Co22 177.6(15) . . ? C231 Co23 C232 99.6(7) . . ? C231 Co23 C233 100.1(7) . . ? C232 Co23 C233 104.5(8) . . ? C231 Co23 C21 106.2(7) . . ? C232 Co23 C21 98.0(7) . . ? C233 Co23 C21 141.8(7) . . ? C231 Co23 Co22 92.0(6) . . ? C232 Co23 Co22 146.7(6) . . ? C233 Co23 Co22 104.0(6) . . ? C21 Co23 Co22 48.7(4) . . ? C231 Co23 Co21 150.6(6) . . ? C232 Co23 Co21 99.7(5) . . ? C233 Co23 Co21 96.3(5) . . ? C21 Co23 Co21 49.1(4) . . ? Co22 Co23 Co21 60.30(8) . . y O231 C231 Co23 176.1(15) . . ? O232 C232 Co23 178.6(15) . . ? O233 C233 Co23 179.3(16) . . ? _diffrn_measured_fraction_theta_max 0.808 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.808 _refine_diff_density_max 2.624 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.161