# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1386 data_zw _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H9 Co O4' _chemical_formula_weight 276.12 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 7.403(2) _cell_length_b 10.964(8) _cell_length_c 12.293(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.30(3) _cell_angle_gamma 90.00 _cell_volume 995.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 1.722 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 903 _diffrn_reflns_av_R_equivalents 0.1525 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 863 _reflns_number_gt 813 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+2.3318P] 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 0.0047(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 863 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2500 0.2500 0.0000 0.0194(3) Uani 1 2 d S . . C1 C 0.1767(2) 0.40294(16) 0.07854(11) 0.0254(6) Uani 1 1 d G . . C2 C 0.0313(2) 0.31820(16) 0.06855(12) 0.0306(6) Uani 1 1 d G . . H2 H -0.0261 0.2836 0.1258 0.037 Uiso 1 1 calc R . . C3 C -0.0109(2) 0.29554(16) -0.04422(14) 0.0339(7) Uani 1 1 d G . . H3 H -0.1009 0.2435 -0.0738 0.041 Uiso 1 1 calc R . . C4 C 0.1083(2) 0.36626(18) -0.10393(10) 0.0341(6) Uani 1 1 d G . . H4 H 0.1102 0.3687 -0.1795 0.041 Uiso 1 1 calc R . . C5 C 0.2243(2) 0.43264(15) -0.02805(14) 0.0271(6) Uani 1 1 d G . . H5 H 0.3154 0.4862 -0.0452 0.033 Uiso 1 1 calc R . . C6 C 0.2793(3) 0.4417(2) 0.1832(2) 0.0264(6) Uani 1 1 d . . . O1 O 0.3836(3) 0.53431(18) 0.17336(16) 0.0360(5) Uani 1 1 d . . . H1 H 0.5000 0.5818 0.2500 0.050 Uiso 1 2 d S . . O2 O 0.2597(3) 0.3841(2) 0.26695(15) 0.0429(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0154(4) 0.0214(4) 0.0217(4) -0.00045(14) 0.0038(2) 0.00484(14) C1 0.0214(12) 0.0253(13) 0.0299(13) -0.0040(10) 0.0053(9) 0.0092(9) C2 0.0185(12) 0.0336(14) 0.0409(14) -0.0061(11) 0.0099(10) 0.0067(10) C3 0.0178(13) 0.0353(17) 0.0477(16) -0.0090(13) -0.0044(11) 0.0090(11) C4 0.0370(15) 0.0346(15) 0.0292(13) 0.0019(11) -0.0072(11) 0.0139(12) C5 0.0289(13) 0.0199(13) 0.0324(12) 0.0035(11) 0.0014(10) 0.0066(10) C6 0.0247(12) 0.0271(13) 0.0283(12) -0.0045(10) 0.0071(10) 0.0067(10) O1 0.0370(11) 0.0322(11) 0.0375(11) 0.0018(8) -0.0062(8) -0.0029(8) O2 0.0455(12) 0.0574(13) 0.0269(10) -0.0011(9) 0.0094(8) -0.0121(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 C2 2.0234(17) . ? Co1 C2 2.0234(17) 7 ? Co1 C3 2.0294(18) . ? Co1 C3 2.0294(17) 7 ? Co1 C1 2.0290(19) . ? Co1 C1 2.0290(19) 7 ? Co1 C4 2.0386(18) 7 ? Co1 C4 2.0386(18) . ? Co1 C5 2.038(2) 7 ? Co1 C5 2.038(2) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 C6 1.505(3) . ? C2 C3 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C6 O2 1.226(3) . ? C6 O1 1.287(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 C2 Co1 C2 180.00(18) . 7 ? C2 Co1 C3 41.0 . . ? C2 Co1 C3 138.98(14) 7 . ? C2 Co1 C3 138.98(14) . 7 ? C2 Co1 C3 41.0 7 7 ? C3 Co1 C3 180.00(17) . 7 ? C2 Co1 C1 41.0 . . ? C2 Co1 C1 138.98(14) 7 . ? C3 Co1 C1 69.0 . . ? C3 Co1 C1 111.04(15) 7 . ? C2 Co1 C1 139.0 . 7 ? C2 Co1 C1 41.02(14) 7 7 ? C3 Co1 C1 111.0 . 7 ? C3 Co1 C1 68.96(15) 7 7 ? C1 Co1 C1 180.00(7) . 7 ? C2 Co1 C4 111.11(15) . 7 ? C2 Co1 C4 68.9 7 7 ? C3 Co1 C4 139.14(15) . 7 ? C3 Co1 C4 40.9 7 7 ? C1 Co1 C4 111.22(15) . 7 ? C1 Co1 C4 68.78(15) 7 7 ? C2 Co1 C4 68.9 . . ? C2 Co1 C4 111.11(15) 7 . ? C3 Co1 C4 40.9 . . ? C3 Co1 C4 139.14(15) 7 . ? C1 Co1 C4 68.8 . . ? C1 Co1 C4 111.2 7 . ? C4 Co1 C4 180.0(2) 7 . ? C2 Co1 C5 111.10(15) . 7 ? C2 Co1 C5 68.9 7 7 ? C3 Co1 C5 111.22(16) . 7 ? C3 Co1 C5 68.8 7 7 ? C1 Co1 C5 139.13(15) . 7 ? C1 Co1 C5 40.87(15) 7 7 ? C4 Co1 C5 40.8 7 7 ? C4 Co1 C5 139.23(15) . 7 ? C2 Co1 C5 68.9 . . ? C2 Co1 C5 111.10(15) 7 . ? C3 Co1 C5 68.8 . . ? C3 Co1 C5 111.22(15) 7 . ? C1 Co1 C5 40.9 . . ? C1 Co1 C5 139.1 7 . ? C4 Co1 C5 139.23(15) 7 . ? C4 Co1 C5 40.8 . . ? C5 Co1 C5 180.0(2) 7 . ? C2 C1 C5 108.0 . . ? C2 C1 C6 126.10(15) . . ? C5 C1 C6 125.43(15) . . ? C2 C1 Co1 69.28(7) . . ? C5 C1 Co1 69.92(7) . . ? C6 C1 Co1 120.28(14) . . ? C3 C2 C1 108.0 . . ? C3 C2 Co1 69.72(7) . . ? C1 C2 Co1 69.70(7) . . ? C2 C3 C4 108.0 . . ? C2 C3 Co1 69.26(7) . . ? C4 C3 Co1 69.92(7) . . ? C5 C4 C3 108.0 . . ? C5 C4 Co1 69.61(8) . . ? C3 C4 Co1 69.22(7) . . ? C4 C5 C1 108.0 . . ? C4 C5 Co1 69.63(7) . . ? C1 C5 Co1 69.21(6) . . ? O2 C6 O1 126.5(2) . . ? O2 C6 C1 119.2(2) . . ? O1 C6 C1 114.2(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.567 _refine_diff_density_min -1.001 _refine_diff_density_rms 0.130 data_zwa _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H15 Co O7' _chemical_formula_weight 330.17 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.707(3) _cell_length_b 14.997(4) _cell_length_c 13.453(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.84(2) _cell_angle_gamma 90.00 _cell_volume 1333.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 1.316 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2230 _diffrn_reflns_av_R_equivalents 0.06 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 25.0 _reflns_number_total 2230 _reflns_number_gt 1488 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1361P)^2^+11.2787P] 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 2230 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1260 _refine_ls_R_factor_gt 0.0851 _refine_ls_wR_factor_ref 0.2467 _refine_ls_wR_factor_gt 0.2220 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1A Co 0.12393(17) 0.21236(8) 0.95806(9) 0.0247(4) Uani 0.96 1 d P . 1 Co1B Co 0.616(4) 0.2123(19) 0.956(2) 0.029(6) Uiso 0.04 1 d P . 2 C1 C 0.4024(9) 0.1748(4) 1.0283(4) 0.0266(18) Uani 1 1 d G . . C2 C 0.3967(10) 0.2678(4) 1.0086(4) 0.037(2) Uani 1 1 d G . . H2 H 0.4236 0.3128 1.0567 0.044 Uiso 1 1 calc R A 1 C3 C 0.3428(11) 0.2802(4) 0.9028(5) 0.045(2) Uani 1 1 d G . . H3 H 0.3281 0.3347 0.8693 0.054 Uiso 1 1 calc R B 1 C4 C 0.3151(11) 0.1948(5) 0.8570(3) 0.046(3) Uani 1 1 d G . . H4 H 0.2792 0.1835 0.7883 0.055 Uiso 1 1 calc R C 1 C5 C 0.3520(9) 0.1296(3) 0.9346(5) 0.035(2) Uani 1 1 d G . . H5 H 0.3444 0.0681 0.9256 0.042 Uiso 1 1 calc R D 1 C6 C 0.4522(12) 0.1353(6) 1.1310(7) 0.033(2) Uani 1 1 d . . . O1 O 0.4010(11) 0.0514(4) 1.1326(5) 0.0438(17) Uani 1 1 d . . . O2 O 0.5330(11) 0.1771(5) 1.2017(5) 0.0481(18) Uani 1 1 d . . . C7 C -0.0821(8) 0.1801(4) 1.0448(3) 0.0244(17) Uani 1 1 d G . . C8 C -0.0813(10) 0.2737(3) 1.0293(4) 0.035(2) Uani 1 1 d G . . H8 H -0.0533 0.3169 1.0794 0.042 Uiso 1 1 calc R E 1 C9 C -0.1309(10) 0.2899(3) 0.9240(5) 0.042(2) Uani 1 1 d G . . H9 H -0.1410 0.3455 0.8930 0.051 Uiso 1 1 calc R F 1 C10 C -0.1623(10) 0.2062(4) 0.8744(3) 0.039(2) Uani 1 1 d G . . H10 H -0.1966 0.1974 0.8051 0.046 Uiso 1 1 calc R G 1 C11 C -0.1321(8) 0.1384(3) 0.9491(4) 0.030(2) Uani 1 1 d G . . H11 H -0.1432 0.0773 0.9373 0.036 Uiso 1 1 calc R H 1 C12 C -0.0308(12) 0.1378(6) 1.1453(7) 0.031(2) Uani 1 1 d . . . O3 O -0.0842(10) 0.0521(4) 1.1430(5) 0.0414(16) Uani 1 1 d . . . O4 O 0.0490(10) 0.1759(5) 1.2186(5) 0.0402(16) Uani 1 1 d . . . O5 O 0.4649(14) -0.0296(5) 1.3195(6) 0.058(2) Uani 1 1 d . . . O6 O -0.0237(16) -0.0409(5) 1.3243(6) 0.069(3) Uani 1 1 d . . . O7 O 0.244(2) -0.0023(7) 1.5065(8) 0.116(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1A 0.0230(6) 0.0261(6) 0.0255(6) -0.0019(5) 0.0050(4) 0.0000(5) C1 0.017(4) 0.037(4) 0.027(4) -0.004(4) 0.005(3) -0.006(3) C2 0.028(4) 0.035(5) 0.051(6) -0.004(4) 0.013(4) -0.002(4) C3 0.031(5) 0.063(7) 0.046(6) 0.007(5) 0.018(4) 0.001(5) C4 0.042(5) 0.060(7) 0.036(5) -0.003(5) 0.010(4) 0.008(5) C5 0.023(4) 0.047(6) 0.036(5) -0.013(4) 0.007(4) 0.004(4) C6 0.024(4) 0.037(5) 0.038(5) -0.003(4) 0.004(4) -0.002(4) O1 0.049(4) 0.032(4) 0.047(4) -0.005(3) -0.001(3) -0.003(3) O2 0.047(4) 0.053(4) 0.037(4) -0.009(3) -0.012(3) -0.001(4) C7 0.014(4) 0.027(4) 0.034(4) -0.004(4) 0.009(3) 0.001(3) C8 0.029(4) 0.026(5) 0.052(6) -0.012(4) 0.011(4) 0.003(4) C9 0.035(5) 0.030(5) 0.061(6) 0.006(5) 0.006(4) 0.011(4) C10 0.028(4) 0.058(6) 0.028(4) 0.012(5) -0.001(4) 0.009(5) C11 0.011(3) 0.037(5) 0.042(5) -0.005(4) 0.007(3) 0.002(3) C12 0.020(4) 0.040(5) 0.039(5) -0.010(4) 0.016(4) -0.001(4) O3 0.049(4) 0.036(4) 0.038(4) -0.005(3) 0.004(3) -0.011(3) O4 0.040(3) 0.050(4) 0.030(3) -0.016(3) 0.006(3) -0.007(3) O5 0.086(6) 0.035(4) 0.053(5) 0.026(3) 0.010(4) 0.018(4) O6 0.125(8) 0.041(4) 0.035(4) 0.023(3) -0.002(5) -0.020(5) O7 0.182(14) 0.076(7) 0.077(8) 0.011(6) -0.015(8) -0.037(8) _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 Co1A C7 2.014(5) . ? Co1A C1 2.024(6) . ? Co1A C2 2.019(6) . ? Co1A C5 2.036(6) . ? Co1A C3 2.028(7) . ? Co1A C8 2.028(6) . ? Co1A C4 2.039(6) . ? Co1A C11 2.031(5) . ? Co1A C9 2.053(6) . ? Co1A C10 2.055(6) . ? Co1B C2 1.93(3) . ? Co1B C1 1.95(3) . ? Co1B C10 2.00(3) 1_655 ? Co1B C11 2.04(3) 1_655 ? Co1B C3 2.11(3) . ? Co1B C5 2.14(3) . ? Co1B C9 2.16(3) 1_655 ? Co1B C4 2.24(3) . ? Co1B C7 2.22(3) 1_655 ? Co1B C8 2.29(3) 1_655 ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 C6 1.488(10) . ? C2 C3 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C6 O2 1.191(11) . ? C6 O1 1.305(11) . ? C7 C8 1.4200 . ? C7 C11 1.4200 . ? C7 C12 1.479(10) . ? C7 Co1B 2.22(3) 1_455 ? C8 C9 1.4200 . ? C8 Co1B 2.29(3) 1_455 ? C9 C10 1.4200 . ? C9 Co1B 2.16(3) 1_455 ? C10 C11 1.4200 . ? C10 Co1B 2.00(3) 1_455 ? C11 Co1B 2.04(3) 1_455 ? C12 O4 1.186(10) . ? C12 O3 1.333(11) . ? 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 C7 Co1A C1 109.4(2) . . ? C7 Co1A C2 125.1(2) . . ? C1 Co1A C2 41.13(11) . . ? C7 Co1A C5 123.5(2) . . ? C1 Co1A C5 40.95(10) . . ? C2 Co1A C5 69.03(13) . . ? C7 Co1A C3 160.7(3) . . ? C1 Co1A C3 69.08(14) . . ? C2 Co1A C3 41.07(12) . . ? C5 Co1A C3 68.85(15) . . ? C7 Co1A C8 41.13(11) . . ? C1 Co1A C8 123.6(2) . . ? C2 Co1A C8 107.6(2) . . ? C5 Co1A C8 159.8(3) . . ? C3 Co1A C8 122.5(2) . . ? C7 Co1A C4 158.0(3) . . ? C1 Co1A C4 68.88(14) . . ? C2 Co1A C4 68.97(15) . . ? C5 Co1A C4 40.79(11) . . ? C3 Co1A C4 40.87(12) . . ? C8 Co1A C4 158.3(3) . . ? C7 Co1A C11 41.10(10) . . ? C1 Co1A C11 125.4(2) . . ? C2 Co1A C11 162.5(3) . . ? C5 Co1A C11 107.9(2) . . ? C3 Co1A C11 155.5(3) . . ? C8 Co1A C11 68.95(13) . . ? C4 Co1A C11 120.7(2) . . ? C7 Co1A C9 68.78(14) . . ? C1 Co1A C9 158.2(3) . . ? C2 Co1A C9 120.9(2) . . ? C5 Co1A C9 158.3(3) . . ? C3 Co1A C9 105.1(2) . . ? C8 Co1A C9 40.71(11) . . ? C4 Co1A C9 121.3(2) . . ? C11 Co1A C9 68.47(14) . . ? C7 Co1A C10 68.75(13) . . ? C1 Co1A C10 160.8(3) . . ? C2 Co1A C10 155.6(3) . . ? C5 Co1A C10 123.0(2) . . ? C3 Co1A C10 119.2(2) . . ? C8 Co1A C10 68.49(15) . . ? C4 Co1A C10 105.3(2) . . ? C11 Co1A C10 40.67(10) . . ? C9 Co1A C10 40.44(11) . . ? C2 Co1B C1 43.0(6) . . ? C2 Co1B C10 155.4(18) . 1_655 ? C1 Co1B C10 160.4(18) . 1_655 ? C2 Co1B C11 160.7(19) . 1_655 ? C1 Co1B C11 123.5(17) . 1_655 ? C10 Co1B C11 41.2(6) 1_655 1_655 ? C2 Co1B C3 40.9(6) . . ? C1 Co1B C3 68.9(9) . . ? C10 Co1B C3 121.3(16) 1_655 . ? C11 Co1B C3 157.7(18) 1_655 . ? C2 Co1B C5 68.6(9) . . ? C1 Co1B C5 40.3(6) . . ? C10 Co1B C5 125.1(16) 1_655 . ? C11 Co1B C5 110.6(15) 1_655 . ? C3 Co1B C5 65.4(8) . . ? C2 Co1B C9 121.0(16) . 1_655 ? C1 Co1B C9 157.8(18) . 1_655 ? C10 Co1B C9 39.7(6) 1_655 1_655 ? C11 Co1B C9 66.3(9) 1_655 1_655 ? C3 Co1B C9 109.8(15) . 1_655 ? C5 Co1B C9 160.8(17) . 1_655 ? C2 Co1B C4 66.6(9) . . ? C1 Co1B C4 66.3(9) . . ? C10 Co1B C4 110.3(15) 1_655 . ? C11 Co1B C4 125.4(16) 1_655 . ? C3 Co1B C4 38.0(5) . . ? C5 Co1B C4 37.8(5) . . ? C9 Co1B C4 127.2(16) 1_655 . ? C2 Co1B C7 125.4(15) . 1_655 ? C1 Co1B C7 110.5(13) . 1_655 ? C10 Co1B C7 65.7(11) 1_655 1_655 ? C11 Co1B C7 38.6(9) 1_655 1_655 ? C3 Co1B C7 161.1(15) . 1_655 ? C5 Co1B C7 127.1(14) . 1_655 ? C9 Co1B C7 63.2(10) 1_655 1_655 ? C4 Co1B C7 160.4(15) . 1_655 ? C2 Co1B C8 110.1(15) . 1_655 ? C1 Co1B C8 125.1(16) . 1_655 ? C10 Co1B C8 64.3(8) 1_655 1_655 ? C11 Co1B C8 63.8(8) 1_655 1_655 ? C3 Co1B C8 127.3(15) . 1_655 ? C5 Co1B C8 160.4(17) . 1_655 ? C9 Co1B C8 37.0(5) 1_655 1_655 ? C4 Co1B C8 161.1(16) . 1_655 ? C7 Co1B C8 36.6(8) 1_655 1_655 ? C2 C1 C5 108.0 . . ? C2 C1 C6 124.0(5) . . ? C5 C1 C6 128.0(5) . . ? C2 C1 Co1B 67.7(9) . . ? C5 C1 Co1B 77.2(9) . . ? C6 C1 Co1B 120.7(10) . . ? C2 C1 Co1A 69.3(2) . . ? C5 C1 Co1A 70.0(2) . . ? C6 C1 Co1A 126.0(5) . . ? Co1B C1 Co1A 112.7(9) . . ? C1 C2 C3 108.0 . . ? C1 C2 Co1B 69.2(9) . . ? C3 C2 Co1B 76.6(9) . . ? C1 C2 Co1A 69.6(2) . . ? C3 C2 Co1A 69.8(2) . . ? Co1B C2 Co1A 113.7(9) . . ? C4 C3 C2 108.0 . . ? C4 C3 Co1A 70.0(2) . . ? C2 C3 Co1A 69.1(2) . . ? C4 C3 Co1B 75.7(8) . . ? C2 C3 Co1B 62.5(8) . . ? Co1A C3 Co1B 105.9(8) . . ? C5 C4 C3 108.0 . . ? C5 C4 Co1A 69.5(2) . . ? C3 C4 Co1A 69.2(2) . . ? C5 C4 Co1B 67.5(8) . . ? C3 C4 Co1B 66.3(8) . . ? Co1A C4 Co1B 101.2(8) . . ? C4 C5 C1 108.0 . . ? C4 C5 Co1A 69.7(2) . . ? C1 C5 Co1A 69.1(2) . . ? C4 C5 Co1B 74.7(8) . . ? C1 C5 Co1B 62.4(8) . . ? Co1A C5 Co1B 104.6(8) . . ? O2 C6 O1 125.4(9) . . ? O2 C6 C1 122.1(8) . . ? O1 C6 C1 112.5(7) . . ? C8 C7 C11 108.0 . . ? C8 C7 C12 123.5(5) . . ? C11 C7 C12 128.4(5) . . ? C8 C7 Co1A 70.0(2) . . ? C11 C7 Co1A 70.1(2) . . ? C12 C7 Co1A 123.9(4) . . ? C8 C7 Co1B 74.4(8) . 1_455 ? C11 C7 Co1B 63.6(8) . 1_455 ? C12 C7 Co1B 129.2(9) . 1_455 ? Co1A C7 Co1B 106.8(8) . 1_455 ? C9 C8 C7 108.0 . . ? C9 C8 Co1A 70.6(2) . . ? C7 C8 Co1A 68.9(2) . . ? C9 C8 Co1B 66.5(8) . 1_455 ? C7 C8 Co1B 68.9(8) . 1_455 ? Co1A C8 Co1B 103.7(8) . 1_455 ? C8 C9 C10 108.0 . . ? C8 C9 Co1A 68.7(2) . . ? C10 C9 Co1A 69.8(2) . . ? C8 C9 Co1B 76.5(8) . 1_455 ? C10 C9 Co1B 63.9(8) . 1_455 ? Co1A C9 Co1B 107.6(8) . 1_455 ? C11 C10 C9 108.0 . . ? C11 C10 Co1B 70.9(9) . 1_455 ? C9 C10 Co1B 76.4(9) . 1_455 ? C11 C10 Co1A 68.8(2) . . ? C9 C10 Co1A 69.7(2) . . ? Co1B C10 Co1A 114.2(9) 1_455 . ? C10 C11 C7 108.0 . . ? C10 C11 Co1A 70.6(2) . . ? C7 C11 Co1A 68.8(2) . . ? C10 C11 Co1B 67.9(9) . 1_455 ? C7 C11 Co1B 77.7(8) . 1_455 ? Co1A C11 Co1B 113.5(8) . 1_455 ? O4 C12 O3 124.4(9) . . ? O4 C12 C7 123.7(8) . . ? O3 C12 C7 111.9(7) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.637 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.064