# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 915826' #TrackingRef 'cif of compounds 915826 and 915827.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H72 Co4 O22' _chemical_formula_weight 1212.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 Tetragonal _symmetry_space_group_name_H-M P4/ncc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 16.75200(10) _cell_length_b 16.75200(10) _cell_length_c 18.6693(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5239.16(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6421 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.60 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 1.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7595 _exptl_absorpt_correction_T_max 0.8574 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 18131 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_unetI/netI 0.0168 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2581 _reflns_number_gt 2087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The solvent methanol molecules is distorted, and which is refined by using restraints of DFIX and ISOR routines. In addition, ISOR routine was used to restrain the C11 from the coordinated methanol molecules. Besides, DFIX routine was also used restrain the distance between H11A ,H11B and H6A from coordinated and solvent methanol molecules,respectively. ; _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^)+(0.0714P)^2^+15.5302P] 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 2581 _refine_ls_number_parameters 173 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1488 _refine_ls_wR_factor_gt 0.1325 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.107 _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 1.16075(3) 0.78295(3) 0.05636(3) 0.0246(2) Uani 1 1 d . . . O1 O 1.14970(16) 0.79616(18) 0.16605(15) 0.0350(7) Uani 1 1 d . . . O2 O 1.05496(16) 0.72478(16) 0.05612(12) 0.0280(6) Uani 1 1 d . . . O3 O 0.92296(16) 0.64975(17) 0.02481(15) 0.0354(7) Uani 1 1 d . . . O4 O 1.22460(15) 0.67401(16) 0.05426(13) 0.0255(6) Uani 1 1 d . . . O5 O 1.11309(18) 0.90072(18) 0.04422(16) 0.0375(7) Uani 1 1 d . . . H5B H 1.1233(8) 0.9208(15) 0.011(2) 0.045 Uiso 1 1 d R . . C1 C 1.0913(2) 0.7773(3) 0.2030(2) 0.0350(9) Uani 1 1 d . . . H1A H 1.0939 0.7912 0.2512 0.042 Uiso 1 1 calc R . . C2 C 1.0201(2) 0.7367(3) 0.1807(2) 0.0328(9) Uani 1 1 d . . . C3 C 0.9626(3) 0.7209(3) 0.2345(2) 0.0416(11) Uani 1 1 d . . . H3A H 0.9721 0.7378 0.2812 0.050 Uiso 1 1 calc R . . C4 C 0.8940(3) 0.6816(3) 0.2194(2) 0.0423(10) Uani 1 1 d . . . H4A H 0.8567 0.6719 0.2553 0.051 Uiso 1 1 calc R . . C5 C 0.8795(2) 0.6555(2) 0.1490(2) 0.0366(9) Uani 1 1 d . . . H5A H 0.8327 0.6278 0.1388 0.044 Uiso 1 1 calc R . . C6 C 0.9332(2) 0.6703(2) 0.0953(2) 0.0300(8) Uani 1 1 d . . . C7 C 1.0067(2) 0.7117(2) 0.1088(2) 0.0271(8) Uani 1 1 d . . . C8 C 0.8476(3) 0.6153(3) 0.0055(3) 0.0471(11) Uani 1 1 d . . . H8A H 0.8042 0.6490 0.0219 0.057 Uiso 1 1 calc R . . H8B H 0.8418 0.5630 0.0273 0.057 Uiso 1 1 calc R . . C9 C 0.8458(4) 0.6082(4) -0.0747(3) 0.0685(17) Uani 1 1 d . . . H9A H 0.7971 0.5826 -0.0892 0.103 Uiso 1 1 calc R . . H9B H 0.8905 0.5770 -0.0905 0.103 Uiso 1 1 calc R . . H9C H 0.8485 0.6604 -0.0956 0.103 Uiso 1 1 calc R . . C10 C 1.2012(2) 0.6121(3) 0.1012(2) 0.0356(9) Uani 1 1 d . . . H10A H 1.2386 0.5688 0.0979 0.053 Uiso 1 1 calc R . . H10B H 1.1490 0.5934 0.0880 0.053 Uiso 1 1 calc R . . H10C H 1.2000 0.6319 0.1494 0.053 Uiso 1 1 calc R . . C11 C 1.0648(8) 0.9468(8) 0.0858(7) 0.171(5) Uani 1 1 d U . . H11A H 1.0931 0.9939 0.1003 0.256 Uiso 1 1 calc R . . H11B H 1.0489 0.9172 0.1275 0.256 Uiso 1 1 calc R . . H11C H 1.0183 0.9619 0.0590 0.256 Uiso 1 1 calc R . . C12 C 0.9752(11) 1.0248(11) 0.2500 0.306(13) Uani 1 2 d SDU . . H12A H 0.9206 1.0348 0.2606 0.459 Uiso 0.50 1 d PR . . H12B H 0.9791 1.0021 0.2018 0.459 Uiso 0.50 1 d PR . . H12C H 1.0056 1.0702 0.2526 0.459 Uiso 0.50 1 d PR . . O6 O 1.0104(9) 0.9700(10) 0.2967(8) 0.166(6) Uani 0.50 1 d PDU . . H6A H 0.9841 0.9287 0.2971 0.249 Uiso 0.50 1 calc PRD . . 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 0.0214(3) 0.0279(3) 0.0245(3) -0.00216(19) 0.00080(19) -0.00173(18) O1 0.0292(14) 0.0483(17) 0.0277(14) -0.0029(12) -0.0003(11) -0.0089(12) O2 0.0240(13) 0.0353(15) 0.0246(13) -0.0021(10) 0.0010(10) -0.0037(11) O3 0.0310(15) 0.0405(16) 0.0347(15) -0.0073(12) 0.0010(12) -0.0088(12) O4 0.0254(13) 0.0253(13) 0.0259(13) 0.0034(10) 0.0004(10) -0.0026(10) O5 0.0394(17) 0.0351(16) 0.0381(15) -0.0002(12) 0.0121(13) 0.0080(13) C1 0.033(2) 0.048(2) 0.0239(18) -0.0002(17) -0.0020(16) -0.0031(17) C2 0.028(2) 0.041(2) 0.0292(19) 0.0037(17) -0.0018(15) -0.0018(17) C3 0.037(2) 0.061(3) 0.027(2) 0.0025(19) 0.0004(17) -0.0051(19) C4 0.037(2) 0.058(3) 0.032(2) 0.008(2) 0.0062(18) -0.008(2) C5 0.029(2) 0.040(2) 0.040(2) 0.0055(18) 0.0015(17) -0.0084(17) C6 0.0281(19) 0.0299(19) 0.032(2) 0.0003(16) 0.0002(16) 0.0007(15) C7 0.0244(18) 0.0280(19) 0.0289(19) 0.0035(15) -0.0016(15) 0.0014(14) C8 0.038(2) 0.057(3) 0.046(3) -0.012(2) -0.001(2) -0.018(2) C9 0.064(4) 0.090(4) 0.051(3) -0.020(3) -0.005(3) -0.034(3) C10 0.034(2) 0.037(2) 0.036(2) 0.0092(18) -0.0025(17) -0.0063(17) C11 0.172(8) 0.159(8) 0.180(8) 0.026(7) 0.014(7) -0.017(7) C12 0.302(13) 0.302(13) 0.314(16) -0.003(7) -0.003(7) -0.014(10) O6 0.141(9) 0.174(10) 0.183(10) -0.036(8) 0.036(8) -0.053(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 Co1 O2 2.022(3) . ? Co1 O4 2.052(3) 2_765 ? Co1 O1 2.068(3) . ? Co1 O4 2.081(3) 11_675 ? Co1 O4 2.116(3) . ? Co1 O5 2.140(3) . ? O1 C1 1.238(5) . ? O2 C7 1.291(4) . ? O3 C6 1.371(5) . ? O3 C8 1.435(5) . ? O4 C10 1.413(5) . ? O4 Co1 2.052(3) 2_765 ? O4 Co1 2.081(3) 12_755 ? O5 C11 1.362(13) . ? O5 H5B 0.7269 . ? C1 C2 1.435(6) . ? C1 H1A 0.9300 . ? C2 C3 1.417(6) . ? C2 C7 1.425(5) . ? C3 C4 1.354(6) . ? C3 H3A 0.9300 . ? C4 C5 1.406(6) . ? C4 H4A 0.9300 . ? C5 C6 1.370(6) . ? C5 H5A 0.9300 . ? C6 C7 1.436(5) . ? C8 C9 1.502(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 O6 1.397(10) 8_775 ? C12 O6 1.397(10) . ? C12 H12A 0.9495 . ? C12 H12B 0.9790 . ? C12 H12C 0.9168 . ? O6 O6 1.80(3) 8_775 ? O6 H6A 0.8200 . ? 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 O2 Co1 O4 171.68(11) . 2_765 ? O2 Co1 O1 88.59(10) . . ? O4 Co1 O1 93.73(10) 2_765 . ? O2 Co1 O4 93.55(10) . 11_675 ? O4 Co1 O4 84.41(11) 2_765 11_675 ? O1 Co1 O4 177.17(11) . 11_675 ? O2 Co1 O4 91.57(10) . . ? O4 Co1 O4 80.19(11) 2_765 . ? O1 Co1 O4 98.97(11) . . ? O4 Co1 O4 82.83(11) 11_675 . ? O2 Co1 O5 96.72(12) . . ? O4 Co1 O5 91.33(11) 2_765 . ? O1 Co1 O5 88.44(12) . . ? O4 Co1 O5 89.47(11) 11_675 . ? O4 Co1 O5 169.03(11) . . ? C1 O1 Co1 126.5(3) . . ? C7 O2 Co1 128.9(2) . . ? C6 O3 C8 116.9(3) . . ? C10 O4 Co1 120.4(2) . 2_765 ? C10 O4 Co1 121.3(2) . 12_755 ? Co1 O4 Co1 96.51(10) 2_765 12_755 ? C10 O4 Co1 118.8(2) . . ? Co1 O4 Co1 99.77(11) 2_765 . ? Co1 O4 Co1 94.57(10) 12_755 . ? C11 O5 Co1 133.2(6) . . ? C11 O5 H5B 111.4 . . ? Co1 O5 H5B 115.4 . . ? O1 C1 C2 128.1(4) . . ? O1 C1 H1A 116.0 . . ? C2 C1 H1A 116.0 . . ? C3 C2 C7 120.4(4) . . ? C3 C2 C1 116.7(4) . . ? C7 C2 C1 122.9(4) . . ? C4 C3 C2 121.3(4) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C6 C5 C4 121.0(4) . . ? C6 C5 H5A 119.5 . . ? C4 C5 H5A 119.5 . . ? C5 C6 O3 125.1(4) . . ? C5 C6 C7 121.5(4) . . ? O3 C6 C7 113.4(3) . . ? O2 C7 C2 124.7(3) . . ? O2 C7 C6 119.1(3) . . ? C2 C7 C6 116.2(3) . . ? O3 C8 C9 107.5(4) . . ? O3 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? O3 C8 H8B 110.2 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 H10A 109.5 . . ? O4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 H11A 109.5 . . ? O5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O6 C12 O6 80.4(18) 8_775 . ? O6 C12 H12A 146.8 8_775 . ? O6 C12 H12A 113.1 . . ? O6 C12 H12B 38.5 8_775 . ? O6 C12 H12B 106.8 . . ? H12A C12 H12B 109.0 . . ? O6 C12 H12C 91.1 8_775 . ? O6 C12 H12C 106.1 . . ? H12A C12 H12C 112.2 . . ? H12B C12 H12C 109.6 . . ? C12 O6 O6 49.8(9) . 8_775 ? C12 O6 H6A 109.5 . . ? O6 O6 H6A 105.0 8_775 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.350 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.107 data_1 _database_code_depnum_ccdc_archive 'CCDC 915827' #TrackingRef 'cif of compounds 915826 and 915827.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H56 Co4 O20' _chemical_formula_sum 'C40 H56 Co4 O20' _chemical_formula_weight 1092.57 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 Tetragonal _symmetry_space_group_name_H-M 'I4(1)/a ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 22.4649(17) _cell_length_b 22.4649(17) _cell_length_c 9.7584(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4924.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2171 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 22.31 _exptl_crystal_description strip _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 1.396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5420 _exptl_absorpt_correction_T_max 0.6121 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 13181 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_unetI/netI 0.0372 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2421 _reflns_number_gt 1678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+4.5125P] 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 2421 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.067029(19) 0.271838(18) 1.01442(4) 0.04577(17) Uani 1 1 d . . . O4 O 0.02095(9) 0.19311(9) 1.02332(19) 0.0443(5) Uani 1 1 d . . . O2 O 0.10195(10) 0.35499(10) 1.0070(2) 0.0534(6) Uani 1 1 d . . . C2 C 0.10968(16) 0.36718(16) 0.7625(3) 0.0609(9) Uani 1 1 d . . . O3 O 0.13019(11) 0.46479(10) 1.0527(3) 0.0689(7) Uani 1 1 d . . . C7 C 0.11294(13) 0.38735(14) 0.8995(3) 0.0495(8) Uani 1 1 d . . . C6 C 0.12928(14) 0.44794(15) 0.9185(4) 0.0568(9) Uani 1 1 d . . . C9 C 0.03814(16) 0.14446(15) 0.9377(4) 0.0620(9) Uani 1 1 d . . . H9A H 0.0123 0.1112 0.9542 0.093 Uiso 1 1 calc R . . H9B H 0.0784 0.1333 0.9579 0.093 Uiso 1 1 calc R . . H9C H 0.0352 0.1562 0.8433 0.093 Uiso 1 1 calc R . . C1 C 0.09155(19) 0.30843(18) 0.7266(4) 0.0762(12) Uani 1 1 d . . . H1A H 0.0913 0.3000 0.6333 0.091 Uiso 1 1 calc R . . C8 C 0.1540(2) 0.52181(18) 1.0852(6) 0.1150(18) Uani 1 1 d . . . H8A H 0.1520 0.5281 1.1824 0.172 Uiso 1 1 calc R . . H8B H 0.1314 0.5520 1.0392 0.172 Uiso 1 1 calc R . . H8C H 0.1947 0.5238 1.0558 0.172 Uiso 1 1 calc R . . C5 C 0.14168(18) 0.48438(17) 0.8078(5) 0.0793(12) Uani 1 1 d . . . H5A H 0.1519 0.5239 0.8231 0.095 Uiso 1 1 calc R . . C4 C 0.1391(2) 0.4632(2) 0.6750(5) 0.0966(15) Uani 1 1 d . . . H4A H 0.1484 0.4881 0.6018 0.116 Uiso 1 1 calc R . . C3 C 0.1232(2) 0.4066(2) 0.6523(4) 0.0900(14) Uani 1 1 d . . . H3A H 0.1210 0.3927 0.5627 0.108 Uiso 1 1 calc R . . C10 C 0.2050(2) 0.2320(3) 0.9791(6) 0.132(2) Uani 1 1 d . . . H10A H 0.2313 0.2012 1.0103 0.198 Uiso 1 1 calc R . . H10B H 0.2200 0.2700 1.0079 0.198 Uiso 1 1 calc R . . H10C H 0.2026 0.2310 0.8809 0.198 Uiso 1 1 calc R . . O1 O 0.07619(12) 0.26738(11) 0.8019(2) 0.0701(7) Uani 1 1 d . . . O5 O 0.14947(12) 0.22331(14) 1.0336(3) 0.0707(8) Uani 1 1 d . . . H5B H 0.1489(17) 0.1992(16) 1.082(4) 0.060(13) Uiso 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 0.0544(3) 0.0448(3) 0.0381(2) -0.00082(18) 0.00711(18) -0.0035(2) O4 0.0539(13) 0.0414(12) 0.0377(11) -0.0025(9) 0.0041(9) 0.0008(9) O2 0.0638(15) 0.0501(13) 0.0462(13) 0.0008(10) 0.0040(10) -0.0093(11) C2 0.073(2) 0.061(2) 0.048(2) 0.0072(17) 0.0099(17) -0.0087(18) O3 0.0725(17) 0.0487(15) 0.0854(18) -0.0098(13) -0.0045(14) -0.0045(12) C7 0.0390(18) 0.049(2) 0.060(2) 0.0046(16) 0.0045(15) -0.0031(14) C6 0.047(2) 0.051(2) 0.072(2) 0.0021(18) -0.0012(17) 0.0008(16) C9 0.078(3) 0.049(2) 0.058(2) -0.0104(16) 0.0136(18) 0.0026(18) C1 0.115(4) 0.074(3) 0.039(2) -0.0004(18) 0.016(2) -0.018(2) C8 0.150(5) 0.052(3) 0.142(5) -0.021(3) -0.023(4) -0.002(3) C5 0.077(3) 0.055(2) 0.106(4) 0.022(2) 0.001(2) -0.011(2) C4 0.131(4) 0.084(3) 0.075(3) 0.029(3) 0.013(3) -0.024(3) C3 0.123(4) 0.084(3) 0.063(3) 0.016(2) 0.016(2) -0.022(3) C10 0.080(4) 0.143(5) 0.174(6) 0.057(4) 0.049(4) 0.007(3) O1 0.108(2) 0.0596(16) 0.0432(13) -0.0047(12) 0.0142(13) -0.0207(14) O5 0.0618(18) 0.0717(19) 0.0787(19) 0.0196(16) 0.0227(14) 0.0065(14) _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 O2 2.027(2) . ? Co1 O4 2.051(2) . ? Co1 O4 2.0839(19) 12_668 ? Co1 O1 2.087(2) . ? Co1 O4 2.129(2) 6_454 ? Co1 O5 2.157(3) . ? O4 C9 1.429(3) . ? O4 Co1 2.0839(19) 15_557 ? O4 Co1 2.129(2) 6_454 ? O2 C7 1.300(3) . ? C2 C7 1.413(4) . ? C2 C1 1.425(5) . ? C2 C3 1.426(5) . ? O3 C6 1.364(4) . ? O3 C8 1.424(5) . ? C7 C6 1.422(4) . ? C6 C5 1.384(5) . ? C1 O1 1.228(4) . ? C5 C4 1.382(6) . ? C4 C3 1.339(6) . ? C10 O5 1.370(5) . ? 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 O2 Co1 O4 172.44(8) . . ? O2 Co1 O4 94.98(8) . 12_668 ? O4 Co1 O4 83.94(8) . 12_668 ? O2 Co1 O1 88.30(9) . . ? O4 Co1 O1 92.90(8) . . ? O4 Co1 O1 176.65(9) 12_668 . ? O2 Co1 O4 91.14(8) . 6_454 ? O4 Co1 O4 81.30(8) . 6_454 ? O4 Co1 O4 82.04(8) 12_668 6_454 ? O1 Co1 O4 98.62(9) . 6_454 ? O2 Co1 O5 97.85(10) . . ? O4 Co1 O5 89.65(10) . . ? O4 Co1 O5 90.17(10) 12_668 . ? O1 Co1 O5 88.69(11) . . ? O4 Co1 O5 168.60(9) 6_454 . ? C9 O4 Co1 119.89(19) . . ? C9 O4 Co1 119.69(19) . 15_557 ? Co1 O4 Co1 97.56(8) . 15_557 ? C9 O4 Co1 120.64(19) . 6_454 ? Co1 O4 Co1 98.50(8) . 6_454 ? Co1 O4 Co1 95.15(8) 15_557 6_454 ? C7 O2 Co1 128.1(2) . . ? C7 C2 C1 123.0(3) . . ? C7 C2 C3 120.2(4) . . ? C1 C2 C3 116.8(3) . . ? C6 O3 C8 118.0(3) . . ? O2 C7 C2 125.0(3) . . ? O2 C7 C6 118.6(3) . . ? C2 C7 C6 116.3(3) . . ? O3 C6 C5 125.6(3) . . ? O3 C6 C7 113.3(3) . . ? C5 C6 C7 121.1(4) . . ? O1 C1 C2 128.9(3) . . ? C4 C5 C6 121.3(4) . . ? C3 C4 C5 119.6(4) . . ? C4 C3 C2 121.4(4) . . ? C1 O1 Co1 125.9(2) . . ? C10 O5 Co1 132.5(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.259 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.051