# Electronic Supplementary Material (ESI) for Chemical Science # 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_LiCo(acac)3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H21 Co Li O6' _chemical_formula_sum 'C15 H21 Co Li O6' _chemical_formula_weight 363.19 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' Li Li -0.0003 0.0001 '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 Hexagonal _symmetry_space_group_name_H-M 'R -3 c ' _symmetry_space_group_name_Hall '-R 3 2"c ' _symmetry_int_tables_number 167 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 16.272(3) _cell_length_b 16.272(3) _cell_length_c 10.968(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2515.0(9) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2512 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.79 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1134 _exptl_absorpt_coefficient_mu 1.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS (Bruker-AXS, 2003) ; _exptl_absorpt_correction_T_min 0.7870 _exptl_absorpt_correction_T_max 0.9209 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area-detector' _diffrn_measurement_method '0.30\% \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3781 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 27.18 _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.908 _reflns_number_total 581 _reflns_number_gt 453 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART Ver. 5.622 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT Ver. 6.22 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT Ver. 6.22' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _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^)+(0.0102P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 581 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_diff_density_max 0.277 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.059 _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 1.0000 1.0000 0.2500 0.01304(18) Uani 1 6 d S . . Li1 Li 1.0000 1.0000 0.0000 0.0153(15) Uani 1 6 d S . . O1 O 0.95554(8) 0.88822(9) 0.13088(12) 0.0158(3) Uani 1 1 d . . . C1 C 0.96345(12) 0.81498(12) 0.14561(19) 0.0156(4) Uani 1 1 d . . . C2 C 1.0000 0.79439(15) 0.2500 0.0175(6) Uani 1 2 d S . . H2 H 1.0000 0.7360 0.2500 0.021 Uiso 1 2 calc SR . . C3 C 0.92800(13) 0.74487(13) 0.04133(18) 0.0212(5) Uani 1 1 d . . . H3A H 0.8588 0.7146 0.0360 0.032 Uiso 1 1 calc R . . H3B H 0.9458 0.6964 0.0554 0.032 Uiso 1 1 calc R . . H3C H 0.9564 0.7782 -0.0351 0.032 Uiso 1 1 calc 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 Co1 0.0148(2) 0.0148(2) 0.0095(3) 0.000 0.000 0.00741(11) Li1 0.019(2) 0.019(2) 0.008(4) 0.000 0.000 0.0095(11) O1 0.0205(7) 0.0161(6) 0.0112(8) -0.0009(5) -0.0011(5) 0.0094(6) C1 0.0115(9) 0.0158(9) 0.0164(11) -0.0005(8) 0.0033(8) 0.0045(8) C2 0.0199(13) 0.0152(9) 0.0188(17) -0.0003(6) -0.0006(12) 0.0100(7) C3 0.0237(11) 0.0196(10) 0.0205(13) -0.0051(8) -0.0038(9) 0.0111(9) _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 O1 2.0550(13) 5_675 yes Co1 O1 2.0550(13) 3_675 yes Co1 O1 2.0550(13) 6_765 yes Co1 O1 2.0550(13) 2_765 yes Co1 O1 2.0550(13) 4 yes Co1 O1 2.0550(13) . yes Co1 Li1 2.7421(6) 4 yes Co1 Li1 2.7421(6) . yes Li1 O1 2.1392(13) 20_565 ? Li1 O1 2.1392(13) 2_765 ? Li1 O1 2.1392(13) 21_655 ? Li1 O1 2.1392(13) 3_675 ? Li1 O1 2.1392(13) 19_775 ? Li1 O1 2.1393(13) . ? Li1 Co1 2.7421(6) 19_775 yes O1 C1 1.271(2) . ? C1 C2 1.406(2) . ? C1 C3 1.511(3) . ? C2 C1 1.406(2) 6_765 ? C2 H2 0.9500 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1 103.58(7) 5_675 3_675 yes O1 Co1 O1 83.89(5) 5_675 6_765 yes O1 Co1 O1 169.61(7) 3_675 6_765 yes O1 Co1 O1 89.68(7) 5_675 2_765 yes O1 Co1 O1 83.89(5) 3_675 2_765 yes O1 Co1 O1 103.58(7) 6_765 2_765 yes O1 Co1 O1 83.89(5) 5_675 4 yes O1 Co1 O1 89.68(7) 3_675 4 yes O1 Co1 O1 83.89(5) 6_765 4 yes O1 Co1 O1 169.61(6) 2_765 4 yes O1 Co1 O1 169.61(7) 5_675 . yes O1 Co1 O1 83.89(5) 3_675 . yes O1 Co1 O1 89.68(7) 6_765 . yes O1 Co1 O1 83.89(5) 2_765 . yes O1 Co1 O1 103.58(7) 4 . yes O1 Co1 Li1 50.52(4) 5_675 4 yes O1 Co1 Li1 129.48(4) 3_675 4 yes O1 Co1 Li1 50.52(4) 6_765 4 yes O1 Co1 Li1 129.48(4) 2_765 4 yes O1 Co1 Li1 50.52(4) 4 4 yes O1 Co1 Li1 129.48(4) . 4 yes O1 Co1 Li1 129.48(4) 5_675 . yes O1 Co1 Li1 50.52(4) 3_675 . yes O1 Co1 Li1 129.48(4) 6_765 . yes O1 Co1 Li1 50.52(4) 2_765 . yes O1 Co1 Li1 129.48(4) 4 . yes O1 Co1 Li1 50.52(4) . . yes Li1 Co1 Li1 180.0 4 . yes O1 Li1 O1 180.0 20_565 2_765 ? O1 Li1 O1 79.90(5) 20_565 21_655 ? O1 Li1 O1 100.10(5) 2_765 21_655 ? O1 Li1 O1 100.10(5) 20_565 3_675 ? O1 Li1 O1 79.90(5) 2_765 3_675 ? O1 Li1 O1 180.0 21_655 3_675 ? O1 Li1 O1 79.90(5) 20_565 19_775 ? O1 Li1 O1 100.10(5) 2_765 19_775 ? O1 Li1 O1 79.90(5) 21_655 19_775 ? O1 Li1 O1 100.10(5) 3_675 19_775 ? O1 Li1 O1 100.10(5) 20_565 . ? O1 Li1 O1 79.90(5) 2_765 . ? O1 Li1 O1 100.10(5) 21_655 . ? O1 Li1 O1 79.90(5) 3_675 . ? O1 Li1 O1 180.00(7) 19_775 . ? O1 Li1 Co1 47.85(3) 20_565 19_775 ? O1 Li1 Co1 132.15(3) 2_765 19_775 ? O1 Li1 Co1 47.85(3) 21_655 19_775 ? O1 Li1 Co1 132.15(3) 3_675 19_775 ? O1 Li1 Co1 47.85(3) 19_775 19_775 ? O1 Li1 Co1 132.15(3) . 19_775 ? O1 Li1 Co1 132.15(3) 20_565 . ? O1 Li1 Co1 47.85(3) 2_765 . ? O1 Li1 Co1 132.15(3) 21_655 . ? O1 Li1 Co1 47.85(3) 3_675 . ? O1 Li1 Co1 132.15(3) 19_775 . ? O1 Li1 Co1 47.85(3) . . ? Co1 Li1 Co1 180.0 19_775 . ? C1 O1 Co1 126.37(13) . . ? C1 O1 Li1 137.11(12) . . ? Co1 O1 Li1 81.63(5) . . ? O1 C1 C2 125.45(19) . . ? O1 C1 C3 115.59(18) . . ? C2 C1 C3 118.94(17) . . ? C1 C2 C1 126.5(2) . 6_765 ? C1 C2 H2 116.7 . . ? C1 C2 H2 116.7 6_765 . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? _database_code_depnum_ccdc_archive 'CCDC 954092' ####################################################################### # # 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_LiCo(tbaoac)3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H78 Co2 Li2 O18' _chemical_formula_sum 'C48 H78 Co2 Li2 O18' _chemical_formula_weight 1074.84 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' Li Li -0.0003 0.0001 '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 Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.333(2) _cell_length_b 12.275(2) _cell_length_c 12.460(2) _cell_angle_alpha 104.286(2) _cell_angle_beta 107.918(2) _cell_angle_gamma 110.038(2) _cell_volume 1424.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6904 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 27.62 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 570 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS (Bruker-AXS, 2003) ; _exptl_absorpt_correction_T_min 0.8198 _exptl_absorpt_correction_T_max 0.9382 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area-detector' _diffrn_measurement_method '0.30\% \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15022 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.91 _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _reflns_number_total 6493 _reflns_number_gt 5646 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART Ver. 5.622 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT Ver. 6.22 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT Ver. 6.22' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _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^)+(0.0909P)^2^+0.8553P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6493 _refine_ls_number_parameters 328 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1486 _refine_ls_wR_factor_gt 0.1439 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.064 _refine_diff_density_max 1.506 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.079 _refine_ls_shift/su_max 0.001 _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 -0.09496(3) 0.85378(2) -0.02463(2) 0.02420(11) Uani 1 1 d . . . Li1 Li 0.1534(4) 0.9366(4) -0.0686(4) 0.0341(8) Uani 1 1 d . . . O1 O -0.1014(2) 0.64500(19) 0.19837(19) 0.0476(5) Uani 1 1 d . . . O2 O -0.12727(18) 0.76582(15) 0.09208(15) 0.0321(4) Uani 1 1 d . . . O3 O 0.07076(16) 0.81831(14) -0.00702(14) 0.0278(3) Uani 1 1 d . . . O4 O -0.01605(16) 0.95970(14) -0.12217(13) 0.0259(3) Uani 1 1 d . . . O5 O 0.1723(2) 0.89731(19) -0.21251(17) 0.0436(4) Uani 1 1 d . . . O6 O 0.1092(3) 0.8709(3) -0.4102(2) 0.0624(6) Uani 1 1 d . . . O7 O 0.25955(16) 1.10901(14) 0.04395(15) 0.0293(3) Uani 1 1 d . . . O8 O 0.22687(16) 1.31175(14) 0.17805(15) 0.0308(3) Uani 1 1 d . . . O9 O 0.43267(17) 1.47787(15) 0.31404(16) 0.0364(4) Uani 1 1 d . . . C1 C 0.1918(3) 0.6952(3) -0.0082(3) 0.0512(7) Uani 1 1 d . . . H1A H 0.1661 0.6738 -0.0960 0.077 Uiso 1 1 calc R . . H1B H 0.1920 0.6225 0.0109 0.077 Uiso 1 1 calc R . . H1C H 0.2849 0.7670 0.0393 0.077 Uiso 1 1 calc R . . C2 C 0.0878(3) 0.7297(2) 0.0243(2) 0.0334(5) Uani 1 1 d . . . C3 C 0.0232(3) 0.6708(3) 0.0844(3) 0.0412(6) Uani 1 1 d . . . H3 H 0.0439 0.6069 0.1025 0.049 Uiso 1 1 calc R . . C4 C -0.0732(3) 0.6989(2) 0.1216(2) 0.0371(5) Uani 1 1 d . . . C5 C -0.2087(3) 0.6519(3) 0.2394(3) 0.0482(7) Uani 1 1 d . . . C6 C -0.1780(4) 0.7862(3) 0.3066(3) 0.0610(9) Uani 1 1 d . . . H6A H -0.0799 0.8344 0.3660 0.091 Uiso 1 1 calc R . . H6B H -0.2371 0.7862 0.3499 0.091 Uiso 1 1 calc R . . H6C H -0.1972 0.8249 0.2476 0.091 Uiso 1 1 calc R . . C7 C -0.3452(4) 0.5802(3) 0.1305(3) 0.0547(8) Uani 1 1 d . . . H7A H -0.3472 0.6227 0.0734 0.082 Uiso 1 1 calc R . . H7B H -0.4195 0.5759 0.1564 0.082 Uiso 1 1 calc R . . H7C H -0.3591 0.4946 0.0897 0.082 Uiso 1 1 calc R . . C8 C -0.1967(4) 0.5852(3) 0.3283(3) 0.0604(8) Uani 1 1 d . . . H8A H -0.2071 0.5013 0.2864 0.091 Uiso 1 1 calc R . . H8B H -0.2699 0.5767 0.3565 0.091 Uiso 1 1 calc R . . H8C H -0.1053 0.6349 0.3990 0.091 Uiso 1 1 calc R . . C9 C -0.2134(3) 0.9511(3) -0.2746(2) 0.0382(5) Uani 1 1 d . . . H9A H -0.2782 0.8949 -0.2526 0.057 Uiso 1 1 calc R . . H9B H -0.2561 0.9288 -0.3633 0.057 Uiso 1 1 calc R . . H9C H -0.1917 1.0386 -0.2308 0.057 Uiso 1 1 calc R . . C10 C -0.0822(3) 0.9371(2) -0.2398(2) 0.0316(5) Uani 1 1 d . . . C11 C -0.0366(3) 0.9050(3) -0.3265(2) 0.0417(6) Uani 1 1 d . . . H11 H -0.0933 0.8898 -0.4080 0.050 Uiso 1 1 calc R . . C12 C 0.0891(3) 0.8916(3) -0.3067(3) 0.0448(6) Uani 1 1 d . . . C13 C 0.2345(5) 0.8581(4) -0.4074(4) 0.0705(10) Uani 1 1 d U . . C14 C 0.2188(8) 0.8417(8) -0.5353(6) 0.130(2) Uani 1 1 d U . . H14A H 0.2984 0.8333 -0.5446 0.195 Uiso 1 1 calc R . . H14B H 0.2151 0.9155 -0.5503 0.195 Uiso 1 1 calc R . . H14C H 0.1327 0.7657 -0.5945 0.195 Uiso 1 1 calc R . . C15 C 0.3659(6) 0.9823(6) -0.3293(7) 0.122(2) Uani 1 1 d U . . H15A H 0.3834 1.0049 -0.2429 0.182 Uiso 1 1 calc R . . H15B H 0.3541 1.0486 -0.3551 0.182 Uiso 1 1 calc R . . H15C H 0.4449 0.9735 -0.3396 0.182 Uiso 1 1 calc R . . C16 C 0.2309(8) 0.7471(6) -0.3832(6) 0.124(2) Uani 1 1 d U . . H16A H 0.2374 0.7597 -0.3003 0.185 Uiso 1 1 calc R . . H16B H 0.3094 0.7338 -0.3895 0.185 Uiso 1 1 calc R . . H16C H 0.1434 0.6730 -0.4433 0.185 Uiso 1 1 calc R . . C17 C 0.4871(3) 1.1441(3) 0.0760(4) 0.0729(12) Uani 1 1 d . . . H17A H 0.4800 1.0716 0.0981 0.109 Uiso 1 1 calc R . . H17B H 0.5826 1.2120 0.1230 0.109 Uiso 1 1 calc R . . H17C H 0.4627 1.1189 -0.0119 0.109 Uiso 1 1 calc R . . C18 C 0.3887(2) 1.1899(2) 0.1050(2) 0.0362(5) Uani 1 1 d . . . C19 C 0.4402(2) 1.3085(2) 0.1913(2) 0.0376(5) Uani 1 1 d . . . H19 H 0.5384 1.3585 0.2324 0.045 Uiso 1 1 calc R . . C20 C 0.3556(2) 1.3619(2) 0.2235(2) 0.0295(5) Uani 1 1 d . . . C21 C 0.3666(3) 1.5539(2) 0.3544(2) 0.0416(6) Uani 1 1 d . . . C22 C 0.2752(4) 1.4925(3) 0.4096(3) 0.0632(9) Uani 1 1 d . . . H22A H 0.1925 1.4167 0.3448 0.095 Uiso 1 1 calc R . . H22B H 0.2465 1.5518 0.4490 0.095 Uiso 1 1 calc R . . H22C H 0.3270 1.4689 0.4708 0.095 Uiso 1 1 calc R . . C23 C 0.2938(4) 1.5815(3) 0.2489(3) 0.0692(11) Uani 1 1 d . . . H23A H 0.3605 1.6228 0.2196 0.104 Uiso 1 1 calc R . . H23B H 0.2551 1.6372 0.2763 0.104 Uiso 1 1 calc R . . H23C H 0.2185 1.5023 0.1822 0.104 Uiso 1 1 calc R . . C24 C 0.4917(4) 1.6751(3) 0.4538(3) 0.0568(8) Uani 1 1 d . . . H24A H 0.5434 1.6557 0.5192 0.085 Uiso 1 1 calc R . . H24B H 0.4597 1.7341 0.4880 0.085 Uiso 1 1 calc R . . H24C H 0.5526 1.7134 0.4184 0.085 Uiso 1 1 calc 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 Co1 0.02507(17) 0.02061(16) 0.02644(17) 0.00813(12) 0.01238(12) 0.00951(12) Li1 0.0311(19) 0.0289(19) 0.049(2) 0.0170(17) 0.0219(18) 0.0154(16) O1 0.0559(12) 0.0504(11) 0.0578(12) 0.0346(10) 0.0349(10) 0.0284(10) O2 0.0409(9) 0.0305(8) 0.0361(8) 0.0171(7) 0.0236(7) 0.0189(7) O3 0.0278(7) 0.0243(7) 0.0322(8) 0.0105(6) 0.0137(6) 0.0125(6) O4 0.0294(8) 0.0229(7) 0.0235(7) 0.0075(6) 0.0128(6) 0.0095(6) O5 0.0516(11) 0.0499(11) 0.0402(10) 0.0167(8) 0.0275(9) 0.0285(9) O6 0.0877(17) 0.0899(17) 0.0456(11) 0.0312(12) 0.0455(12) 0.0605(15) O7 0.0265(7) 0.0244(7) 0.0365(8) 0.0095(6) 0.0156(6) 0.0109(6) O8 0.0280(8) 0.0242(7) 0.0333(8) 0.0057(6) 0.0120(6) 0.0095(6) O9 0.0323(8) 0.0274(8) 0.0353(9) 0.0037(7) 0.0111(7) 0.0076(7) C1 0.0599(18) 0.0578(18) 0.075(2) 0.0414(16) 0.0447(17) 0.0435(16) C2 0.0371(12) 0.0324(11) 0.0369(12) 0.0155(10) 0.0172(10) 0.0200(10) C3 0.0532(15) 0.0418(14) 0.0539(15) 0.0308(12) 0.0311(13) 0.0333(13) C4 0.0479(14) 0.0366(12) 0.0392(12) 0.0216(10) 0.0250(11) 0.0220(11) C5 0.0507(16) 0.0488(16) 0.0477(15) 0.0239(13) 0.0269(13) 0.0170(13) C6 0.079(2) 0.063(2) 0.0534(18) 0.0244(16) 0.0413(17) 0.0327(18) C7 0.0627(19) 0.0606(19) 0.0540(17) 0.0332(15) 0.0340(15) 0.0268(16) C8 0.0592(19) 0.062(2) 0.0539(18) 0.0303(16) 0.0246(15) 0.0153(16) C9 0.0377(13) 0.0413(13) 0.0271(11) 0.0097(10) 0.0091(10) 0.0159(11) C10 0.0380(12) 0.0252(10) 0.0250(10) 0.0073(8) 0.0117(9) 0.0109(9) C11 0.0535(16) 0.0436(14) 0.0270(11) 0.0108(10) 0.0166(11) 0.0240(12) C12 0.0613(17) 0.0439(14) 0.0389(14) 0.0139(11) 0.0314(13) 0.0271(13) C13 0.098(3) 0.101(3) 0.063(2) 0.040(2) 0.058(2) 0.073(3) C14 0.185(6) 0.203(7) 0.112(4) 0.088(4) 0.111(4) 0.145(6) C15 0.111(4) 0.122(4) 0.177(6) 0.063(4) 0.096(4) 0.068(3) C16 0.175(6) 0.136(5) 0.108(4) 0.051(4) 0.081(5) 0.102(5) C17 0.0351(15) 0.0565(19) 0.104(3) -0.0043(19) 0.0341(17) 0.0172(14) C18 0.0271(11) 0.0335(12) 0.0474(14) 0.0120(10) 0.0203(10) 0.0121(10) C19 0.0254(11) 0.0330(12) 0.0449(13) 0.0080(10) 0.0161(10) 0.0072(9) C20 0.0310(11) 0.0232(10) 0.0288(10) 0.0090(8) 0.0127(9) 0.0073(9) C21 0.0437(14) 0.0289(12) 0.0424(13) 0.0053(10) 0.0141(11) 0.0160(11) C22 0.060(2) 0.0529(18) 0.068(2) 0.0077(16) 0.0366(17) 0.0200(16) C23 0.079(2) 0.0429(17) 0.062(2) 0.0086(15) 0.0054(18) 0.0331(17) C24 0.0576(18) 0.0387(15) 0.0516(17) 0.0022(13) 0.0159(14) 0.0156(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 O7 2.0269(16) 2_575 yes Co1 O3 2.0295(16) . yes Co1 O2 2.0607(16) . yes Co1 O8 2.0641(16) 2_575 yes Co1 O4 2.1492(15) . yes Co1 O4 2.1712(15) 2_575 yes Co1 Li1 2.919(4) . yes Co1 Li1 2.928(4) 2_575 yes Li1 O5 1.837(5) . yes Li1 O3 1.906(4) . yes Li1 O7 1.909(4) . yes Li1 O4 1.973(4) . yes Li1 C12 2.688(5) . yes Li1 Co1 2.928(4) 2_575 yes O1 C4 1.345(3) . ? O1 C5 1.475(4) . ? O2 C4 1.241(3) . ? O3 C2 1.295(3) . ? O4 C10 1.329(3) . ? O4 Co1 2.1711(15) 2_575 yes O5 C12 1.227(4) . ? O6 C12 1.356(3) . ? O6 C13 1.472(4) . ? O7 C18 1.286(3) . ? O7 Co1 2.0269(16) 2_575 yes O8 C20 1.238(3) . ? O8 Co1 2.0641(16) 2_575 yes O9 C20 1.346(3) . ? O9 C21 1.471(3) . ? C1 C2 1.512(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.366(4) . ? C3 C4 1.421(4) . ? C3 H3 0.9500 . ? C5 C7 1.482(4) . ? C5 C6 1.512(5) . ? C5 C8 1.532(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.497(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.366(4) . ? C11 C12 1.443(4) . ? C11 H11 0.9500 . ? C13 C16 1.457(7) . ? C13 C14 1.502(6) . ? C13 C15 1.519(8) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.505(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.369(3) . ? C19 C20 1.431(3) . ? C19 H19 0.9500 . ? C21 C23 1.505(4) . ? C21 C22 1.508(5) . ? C21 C24 1.524(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 O7 Co1 O3 178.99(6) 2_575 . yes O7 Co1 O2 92.93(7) 2_575 . yes O3 Co1 O2 88.07(7) . . yes O7 Co1 O8 88.04(6) 2_575 2_575 yes O3 Co1 O8 92.02(6) . 2_575 yes O2 Co1 O8 92.33(7) . 2_575 yes O7 Co1 O4 96.69(6) 2_575 . yes O3 Co1 O4 82.30(6) . . yes O2 Co1 O4 168.01(6) . . yes O8 Co1 O4 95.13(6) 2_575 . yes O7 Co1 O4 82.19(6) 2_575 2_575 yes O3 Co1 O4 97.66(6) . 2_575 yes O2 Co1 O4 92.70(6) . 2_575 yes O8 Co1 O4 169.22(6) 2_575 2_575 yes O4 Co1 O4 81.57(6) . 2_575 yes O7 Co1 Li1 138.48(9) 2_575 . yes O2 Co1 Li1 126.62(10) . . yes O8 Co1 Li1 100.89(10) 2_575 . yes O4 Co1 Li1 83.66(9) 2_575 . yes O7 Co1 Li1 40.40(9) 2_575 2_575 yes O3 Co1 Li1 139.30(9) . 2_575 yes O2 Co1 Li1 99.11(10) . 2_575 yes O8 Co1 Li1 127.26(10) 2_575 2_575 yes O4 Co1 Li1 83.80(9) . 2_575 yes Li1 Co1 Li1 111.97(9) . 2_575 yes O5 Li1 O3 125.7(2) . . yes O5 Li1 O7 116.4(2) . . yes O3 Li1 O7 116.5(2) . . yes O5 Li1 O4 100.5(2) . . yes O3 Li1 O4 90.32(17) . . yes O7 Li1 O4 90.67(18) . . yes O5 Li1 C12 22.93(11) . . yes O3 Li1 C12 125.5(2) . . yes O7 Li1 C12 116.6(2) . . yes O4 Li1 C12 77.52(16) . . yes O5 Li1 Co1 130.2(2) . . yes O3 Li1 Co1 43.78(9) . . yes O7 Li1 Co1 102.77(17) . . yes O4 Li1 Co1 47.42(9) . . yes C12 Li1 Co1 111.81(16) . . yes O5 Li1 Co1 123.0(2) . 2_575 yes O3 Li1 Co1 103.55(17) . 2_575 yes C12 Li1 Co1 105.99(15) . 2_575 yes Co1 Li1 Co1 68.03(9) . 2_575 yes C4 O1 C5 121.2(2) . . ? C4 O2 Co1 125.41(16) . . ? C2 O3 Li1 138.73(19) . . ? C2 O3 Co1 125.13(15) . . ? Li1 O3 Co1 95.69(14) . . ? C10 O4 Li1 118.91(19) . . ? C10 O4 Co1 125.97(14) . . ? Li1 O4 Co1 90.05(13) . . ? C10 O4 Co1 123.87(14) . 2_575 ? Li1 O4 Co1 89.79(13) . 2_575 ? Co1 O4 Co1 98.43(6) . 2_575 ? C12 O5 Li1 121.4(2) . . ? C12 O6 C13 119.0(3) . . ? C18 O7 Li1 137.30(19) . . ? C18 O7 Co1 126.12(15) . 2_575 ? Li1 O7 Co1 96.11(14) . 2_575 ? C20 O8 Co1 125.69(15) . 2_575 ? C20 O9 C21 120.88(19) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O3 C2 C3 125.5(2) . . ? O3 C2 C1 114.5(2) . . ? C3 C2 C1 120.0(2) . . ? C2 C3 C4 124.1(2) . . ? C2 C3 H3 117.9 . . ? C4 C3 H3 117.9 . . ? O2 C4 O1 120.9(2) . . ? O2 C4 C3 127.1(2) . . ? O1 C4 C3 112.0(2) . . ? O1 C5 C7 107.7(2) . . ? O1 C5 C6 112.5(2) . . ? C7 C5 C6 112.8(3) . . ? O1 C5 C8 101.8(3) . . ? C7 C5 C8 111.6(3) . . ? C6 C5 C8 109.9(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 C11 124.2(2) . . ? O4 C10 C9 115.9(2) . . ? C11 C10 C9 119.9(2) . . ? C10 C11 C12 126.5(2) . . ? C10 C11 H11 116.8 . . ? C12 C11 H11 116.8 . . ? O5 C12 O6 120.8(3) . . ? O5 C12 C11 128.3(2) . . ? O6 C12 C11 110.9(3) . . ? O6 C12 Li1 156.3(2) . . ? C16 C13 O6 109.6(4) . . ? C16 C13 C14 111.7(4) . . ? O6 C13 C14 101.7(3) . . ? C16 C13 C15 118.0(5) . . ? O6 C13 C15 111.8(3) . . ? C14 C13 C15 102.5(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O7 C18 C19 125.9(2) . . ? O7 C18 C17 114.3(2) . . ? C19 C18 C17 119.8(2) . . ? C18 C19 C20 124.1(2) . . ? C18 C19 H19 117.9 . . ? C20 C19 H19 117.9 . . ? O8 C20 O9 121.3(2) . . ? O8 C20 C19 126.7(2) . . ? O9 C20 C19 112.0(2) . . ? O9 C21 C23 108.7(2) . . ? O9 C21 C22 111.4(2) . . ? C23 C21 C22 114.6(3) . . ? O9 C21 C24 102.2(2) . . ? C23 C21 C24 109.7(3) . . ? C22 C21 C24 109.6(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _database_code_depnum_ccdc_archive 'CCDC 954093' ####################################################################### # # 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_LiCo(dhd)3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H78 Co2 Li2 O12' _chemical_formula_sum 'C48 H78 Co2 Li2 O12' _chemical_formula_weight 978.84 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn ' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.815(4) _cell_length_b 9.767(3) _cell_length_c 21.674(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.183(4) _cell_angle_gamma 90.00 _cell_volume 2713.0(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3505 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 24.52 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS (Bruker-AXS, 2003) ; _exptl_absorpt_correction_T_min 0.9245 _exptl_absorpt_correction_T_max 0.9426 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area-detector' _diffrn_measurement_method '0.30\% \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24211 _diffrn_reflns_av_R_equivalents 0.1264 _diffrn_reflns_av_sigmaI/netI 0.1120 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4768 _reflns_number_gt 2919 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART Ver. 5.622 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT Ver. 6.22 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT Ver. 6.22' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _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^)+(0.0594P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4768 _refine_ls_number_parameters 317 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1522 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _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 0.89319(4) -0.04582(6) 0.53342(3) 0.0277(2) Uani 1 1 d . . . Li1 Li 0.9035(5) 0.0690(8) 0.4106(4) 0.0343(19) Uani 1 1 d . . . O1 O 0.8132(2) 0.0336(3) 0.60389(13) 0.0340(8) Uani 1 1 d . . . O2 O 0.8114(2) 0.0821(3) 0.47826(13) 0.0298(8) Uani 1 1 d . . . O3 O 0.9742(2) -0.0820(3) 0.44923(13) 0.0275(7) Uani 1 1 d . . . O4 O 0.8720(2) -0.0069(3) 0.33659(14) 0.0392(8) Uani 1 1 d . B . O5 O 1.0260(2) 0.1781(3) 0.41445(13) 0.0279(7) Uani 1 1 d . . . O6 O 1.2101(2) 0.1953(3) 0.48276(15) 0.0362(8) Uani 1 1 d . . . C1 C 0.6538(3) 0.1439(6) 0.4330(2) 0.0447(14) Uani 1 1 d . . . H1A H 0.6819 0.2284 0.4152 0.067 Uiso 1 1 calc R . . H1B H 0.5804 0.1577 0.4440 0.067 Uiso 1 1 calc R . . H1C H 0.6590 0.0697 0.4027 0.067 Uiso 1 1 calc R . . C2 C 0.7147(3) 0.1069(4) 0.4894(2) 0.0291(11) Uani 1 1 d . . . C3 C 0.6698(3) 0.1058(5) 0.5458(2) 0.0328(12) Uani 1 1 d . . . H3 H 0.5974 0.1259 0.5479 0.039 Uiso 1 1 calc R . . C4 C 0.7214(3) 0.0773(4) 0.6013(2) 0.0310(11) Uani 1 1 d . A . C5 C 0.6687(4) 0.0998(5) 0.6625(2) 0.0408(13) Uani 1 1 d . . . C6 C 0.7024(10) -0.0052(13) 0.7064(6) 0.065(4) Uiso 0.50 1 d PD A 1 H6A H 0.7788 -0.0081 0.7078 0.097 Uiso 0.50 1 calc PR A 1 H6B H 0.6756 -0.0946 0.6933 0.097 Uiso 0.50 1 calc PR A 1 H6C H 0.6753 0.0167 0.7474 0.097 Uiso 0.50 1 calc PR A 1 C7 C 0.5516(8) 0.0977(13) 0.6596(6) 0.046(3) Uiso 0.50 1 d PD A 1 H7A H 0.5233 0.1019 0.7015 0.069 Uiso 0.50 1 calc PR A 1 H7B H 0.5283 0.0132 0.6395 0.069 Uiso 0.50 1 calc PR A 1 H7C H 0.5269 0.1768 0.6359 0.069 Uiso 0.50 1 calc PR A 1 C8 C 0.7111(10) 0.2422(13) 0.6860(6) 0.064(4) Uiso 0.50 1 d PD A 1 H8A H 0.6949 0.2528 0.7299 0.096 Uiso 0.50 1 calc PR A 1 H8B H 0.6778 0.3161 0.6625 0.096 Uiso 0.50 1 calc PR A 1 H8C H 0.7868 0.2461 0.6801 0.096 Uiso 0.50 1 calc PR A 1 C6X C 0.6685(11) -0.0462(12) 0.6946(6) 0.062(4) Uiso 0.50 1 d PD A 2 H6X1 H 0.7395 -0.0836 0.6948 0.094 Uiso 0.50 1 calc PR A 2 H6X2 H 0.6221 -0.1079 0.6718 0.094 Uiso 0.50 1 calc PR A 2 H6X3 H 0.6439 -0.0371 0.7372 0.094 Uiso 0.50 1 calc PR A 2 C7X C 0.5583(9) 0.1539(14) 0.6585(6) 0.055(4) Uiso 0.50 1 d PD A 2 H7X1 H 0.5310 0.1679 0.7002 0.082 Uiso 0.50 1 calc PR A 2 H7X2 H 0.5144 0.0876 0.6365 0.082 Uiso 0.50 1 calc PR A 2 H7X3 H 0.5581 0.2411 0.6361 0.082 Uiso 0.50 1 calc PR A 2 C8X C 0.7334(10) 0.1871(14) 0.7010(6) 0.067(4) Uiso 0.50 1 d PD A 2 H8X1 H 0.6930 0.2180 0.7367 0.100 Uiso 0.50 1 calc PR A 2 H8X2 H 0.7563 0.2668 0.6771 0.100 Uiso 0.50 1 calc PR A 2 H8X3 H 0.7946 0.1356 0.7152 0.100 Uiso 0.50 1 calc PR A 2 C9 C 1.0290(4) -0.3135(4) 0.4544(2) 0.0396(13) Uani 1 1 d . . . H9A H 1.0940 -0.2823 0.4738 0.059 Uiso 1 1 calc R . . H9B H 1.0442 -0.3887 0.4259 0.059 Uiso 1 1 calc R . . H9C H 0.9808 -0.3455 0.4863 0.059 Uiso 1 1 calc R . . C10 C 0.9806(3) -0.1984(5) 0.4200(2) 0.0310(11) Uani 1 1 d . . . C11 C 0.9474(3) -0.2187(5) 0.3617(2) 0.0363(12) Uani 1 1 d . B . H11 H 0.9589 -0.3076 0.3453 0.044 Uiso 1 1 calc R . . C12 C 0.8972(4) -0.1243(5) 0.3215(2) 0.0410(13) Uani 1 1 d . . . C13 C 0.8727(5) -0.1671(6) 0.2555(3) 0.0682(19) Uani 1 1 d D B 1 C14 C 0.7549(8) -0.181(2) 0.2534(10) 0.071(4) Uiso 0.40 1 d PD B 1 H14A H 0.7330 -0.2081 0.2118 0.107 Uiso 0.40 1 calc PR B 1 H14B H 0.7228 -0.0932 0.2641 0.107 Uiso 0.40 1 calc PR B 1 H14C H 0.7328 -0.2510 0.2831 0.107 Uiso 0.40 1 calc PR B 1 C15 C 0.9297(11) -0.2999(12) 0.2352(7) 0.045(3) Uiso 0.40 1 d PD B 1 H15A H 0.9110 -0.3214 0.1924 0.068 Uiso 0.40 1 calc PR B 1 H15B H 0.9088 -0.3758 0.2620 0.068 Uiso 0.40 1 calc PR B 1 H15C H 1.0053 -0.2864 0.2383 0.068 Uiso 0.40 1 calc PR B 1 C16 C 0.9096(17) -0.0489(17) 0.2147(9) 0.079(5) Uiso 0.40 1 d PD B 1 H16A H 0.8957 -0.0709 0.1713 0.119 Uiso 0.40 1 calc PR B 1 H16B H 0.9846 -0.0348 0.2207 0.119 Uiso 0.40 1 calc PR B 1 H16C H 0.8720 0.0349 0.2259 0.119 Uiso 0.40 1 calc PR B 1 C14X C 0.7697(13) -0.249(2) 0.2620(11) 0.071(4) Uiso 0.30 1 d PD B 2 H14D H 0.7468 -0.2806 0.2213 0.107 Uiso 0.30 1 calc PR B 2 H14E H 0.7159 -0.1897 0.2799 0.107 Uiso 0.30 1 calc PR B 2 H14F H 0.7812 -0.3279 0.2891 0.107 Uiso 0.30 1 calc PR B 2 C15X C 0.9596(11) -0.2498(18) 0.2249(8) 0.045(3) Uiso 0.30 1 d PD B 2 H15D H 0.9389 -0.2728 0.1825 0.068 Uiso 0.30 1 calc PR B 2 H15E H 0.9716 -0.3342 0.2483 0.068 Uiso 0.30 1 calc PR B 2 H15F H 1.0238 -0.1953 0.2241 0.068 Uiso 0.30 1 calc PR B 2 C16X C 0.837(2) -0.0511(18) 0.2157(10) 0.079(5) Uiso 0.30 1 d PD B 2 H16D H 0.8228 -0.0849 0.1739 0.119 Uiso 0.30 1 calc PR B 2 H16E H 0.8913 0.0193 0.2141 0.119 Uiso 0.30 1 calc PR B 2 H16F H 0.7729 -0.0116 0.2329 0.119 Uiso 0.30 1 calc PR B 2 C14Y C 0.7664(14) -0.123(3) 0.2355(13) 0.092(9) Uiso 0.30 1 d PD B 3 H14G H 0.7543 -0.1516 0.1927 0.138 Uiso 0.30 1 calc PR B 3 H14H H 0.7613 -0.0228 0.2382 0.138 Uiso 0.30 1 calc PR B 3 H14I H 0.7139 -0.1645 0.2623 0.138 Uiso 0.30 1 calc PR B 3 C15Y C 0.8747(17) -0.3289(13) 0.2483(10) 0.064(6) Uiso 0.30 1 d PD B 3 H15G H 0.9440 -0.3635 0.2596 0.096 Uiso 0.30 1 calc PR B 3 H15H H 0.8592 -0.3535 0.2054 0.096 Uiso 0.30 1 calc PR B 3 H15I H 0.8223 -0.3697 0.2755 0.096 Uiso 0.30 1 calc PR B 3 C16Y C 0.944(2) -0.090(3) 0.2131(13) 0.116(13) Uiso 0.30 1 d PD B 3 H16G H 1.0169 -0.1124 0.2231 0.173 Uiso 0.30 1 calc PR B 3 H16H H 0.9331 0.0086 0.2183 0.173 Uiso 0.30 1 calc PR B 3 H16I H 0.9294 -0.1158 0.1703 0.173 Uiso 0.30 1 calc PR B 3 C17 C 0.9946(4) 0.3500(5) 0.3420(2) 0.0417(13) Uani 1 1 d . . . H17A H 0.9737 0.2811 0.3115 0.063 Uiso 1 1 calc R . . H17B H 1.0322 0.4242 0.3214 0.063 Uiso 1 1 calc R . . H17C H 0.9324 0.3870 0.3622 0.063 Uiso 1 1 calc R . . C18 C 1.0637(3) 0.2856(5) 0.3891(2) 0.0321(11) Uani 1 1 d . . . C19 C 1.1578(3) 0.3441(5) 0.4038(2) 0.0363(12) Uani 1 1 d . . . H19 H 1.1794 0.4209 0.3802 0.044 Uiso 1 1 calc R . . C20 C 1.2251(3) 0.2990(5) 0.4514(2) 0.0343(12) Uani 1 1 d . C . C21 C 1.3207(4) 0.3856(5) 0.4678(3) 0.0498(15) Uani 1 1 d . . . C22 C 1.3948(6) 0.3860(9) 0.4106(4) 0.063(2) Uani 0.656(5) 1 d PD C 1 H22A H 1.4547 0.4455 0.4188 0.094 Uiso 0.656(5) 1 calc PR C 1 H22B H 1.3567 0.4200 0.3744 0.094 Uiso 0.656(5) 1 calc PR C 1 H22C H 1.4192 0.2926 0.4026 0.094 Uiso 0.656(5) 1 calc PR C 1 C23 C 1.2958(6) 0.5173(8) 0.4891(5) 0.059(2) Uani 0.656(5) 1 d PD C 1 H23A H 1.2544 0.5101 0.5269 0.088 Uiso 0.656(5) 1 calc PR C 1 H23B H 1.2554 0.5659 0.4575 0.088 Uiso 0.656(5) 1 calc PR C 1 H23C H 1.3602 0.5680 0.4978 0.088 Uiso 0.656(5) 1 calc PR C 1 C24 C 1.3864(6) 0.3045(9) 0.5191(4) 0.054(2) Uani 0.656(5) 1 d PD C 1 H24A H 1.4024 0.2122 0.5041 0.081 Uiso 0.656(5) 1 calc PR C 1 H24B H 1.3455 0.2981 0.5571 0.081 Uiso 0.656(5) 1 calc PR C 1 H24C H 1.4517 0.3536 0.5275 0.081 Uiso 0.656(5) 1 calc PR C 1 C22X C 1.2853(12) 0.4536(19) 0.5302(9) 0.063(2) Uani 0.344(5) 1 d PD C 2 H22D H 1.2783 0.3828 0.5620 0.094 Uiso 0.344(5) 1 calc PR C 2 H22E H 1.2180 0.4993 0.5241 0.094 Uiso 0.344(5) 1 calc PR C 2 H22F H 1.3375 0.5209 0.5433 0.094 Uiso 0.344(5) 1 calc PR C 2 C23X C 1.4027(12) 0.3039(15) 0.4704(10) 0.059(2) Uani 0.344(5) 1 d PD C 2 H23D H 1.4644 0.3569 0.4825 0.088 Uiso 0.344(5) 1 calc PR C 2 H23E H 1.4143 0.2626 0.4298 0.088 Uiso 0.344(5) 1 calc PR C 2 H23F H 1.3902 0.2316 0.5008 0.088 Uiso 0.344(5) 1 calc PR C 2 C24X C 1.3308(11) 0.5156(15) 0.4221(8) 0.054(2) Uani 0.344(5) 1 d PD C 2 H24D H 1.3842 0.5784 0.4381 0.081 Uiso 0.344(5) 1 calc PR C 2 H24E H 1.2636 0.5632 0.4198 0.081 Uiso 0.344(5) 1 calc PR C 2 H24F H 1.3508 0.4841 0.3809 0.081 Uiso 0.344(5) 1 calc PR C 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 0.0223(3) 0.0297(4) 0.0311(4) -0.0002(3) -0.0091(2) 0.0005(3) Li1 0.027(4) 0.039(5) 0.037(5) 0.001(4) -0.008(3) 0.000(3) O1 0.0280(17) 0.0419(19) 0.032(2) 0.0023(16) -0.0073(14) 0.0025(15) O2 0.0218(16) 0.0343(19) 0.033(2) 0.0009(15) -0.0057(13) 0.0016(13) O3 0.0248(16) 0.0233(18) 0.0344(19) -0.0037(14) -0.0071(13) -0.0006(13) O4 0.0386(19) 0.044(2) 0.035(2) -0.0072(16) -0.0148(15) 0.0073(16) O5 0.0251(16) 0.0265(17) 0.0321(19) 0.0027(15) -0.0086(13) -0.0058(13) O6 0.0282(17) 0.034(2) 0.046(2) 0.0007(17) -0.0105(15) -0.0035(14) C1 0.031(3) 0.069(4) 0.034(3) 0.001(3) -0.013(2) 0.011(3) C2 0.026(3) 0.025(3) 0.036(3) -0.003(2) -0.012(2) -0.002(2) C3 0.025(2) 0.041(3) 0.032(3) -0.002(2) -0.007(2) 0.009(2) C4 0.027(3) 0.033(3) 0.033(3) 0.002(2) 0.000(2) 0.003(2) C5 0.032(3) 0.054(3) 0.036(3) -0.002(3) -0.004(2) 0.008(2) C9 0.043(3) 0.029(3) 0.047(3) -0.005(2) -0.014(2) 0.005(2) C10 0.024(2) 0.029(3) 0.040(3) -0.008(2) -0.004(2) -0.004(2) C11 0.036(3) 0.038(3) 0.035(3) -0.014(2) -0.013(2) 0.001(2) C12 0.033(3) 0.048(3) 0.042(3) -0.009(3) -0.014(2) 0.003(3) C13 0.078(4) 0.066(4) 0.060(4) -0.029(3) -0.036(3) 0.033(3) C17 0.044(3) 0.038(3) 0.043(3) 0.008(3) -0.007(2) 0.001(2) C18 0.033(3) 0.037(3) 0.027(3) -0.004(2) -0.001(2) 0.002(2) C19 0.032(3) 0.031(3) 0.046(3) 0.003(2) -0.001(2) -0.006(2) C20 0.022(2) 0.032(3) 0.049(3) -0.009(3) -0.001(2) -0.003(2) C21 0.036(3) 0.042(3) 0.072(4) 0.002(3) -0.015(3) -0.012(3) C22 0.035(4) 0.065(6) 0.089(7) 0.005(5) -0.009(4) -0.017(4) C23 0.041(5) 0.031(5) 0.104(8) -0.014(5) -0.025(5) -0.003(3) C24 0.040(4) 0.056(5) 0.067(6) -0.006(5) -0.028(4) -0.008(4) C22X 0.035(4) 0.065(6) 0.089(7) 0.005(5) -0.009(4) -0.017(4) C23X 0.041(5) 0.031(5) 0.104(8) -0.014(5) -0.025(5) -0.003(3) C24X 0.040(4) 0.056(5) 0.067(6) -0.006(5) -0.028(4) -0.008(4) _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 O1 1.999(3) . ? Co1 O6 2.001(3) 3_756 ? Co1 O5 2.002(3) 3_756 ? Co1 O2 2.020(3) . ? Co1 O3 2.132(3) . ? Co1 O3 2.141(3) 3_756 ? Co1 Li1 2.879(7) 3_756 ? Li1 O4 1.812(8) . ? Li1 O2 1.889(8) . ? Li1 O5 1.899(8) . ? Li1 O3 1.921(8) . ? Li1 Co1 2.879(7) 3_756 ? O1 C4 1.253(5) . ? O2 C2 1.287(5) . ? O3 C10 1.305(5) . ? O3 Co1 2.141(3) 3_756 ? O4 C12 1.236(5) . ? O5 C18 1.280(5) . ? O5 Co1 2.002(3) 3_756 ? O6 C20 1.235(5) . ? O6 Co1 2.001(3) 3_756 ? C1 C2 1.494(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.353(6) . ? C3 C4 1.398(6) . ? C3 H3 0.9500 . ? C4 C5 1.506(6) . ? C5 C8X 1.452(12) . ? C5 C6 1.463(13) . ? C5 C7 1.502(11) . ? C5 C7X 1.513(12) . ? C5 C8 1.577(13) . ? C5 C6X 1.587(13) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C6X H6X1 0.9800 . ? C6X H6X2 0.9800 . ? C6X H6X3 0.9800 . ? C7X H7X1 0.9800 . ? C7X H7X2 0.9800 . ? C7X H7X3 0.9800 . ? C8X H8X1 0.9800 . ? C8X H8X2 0.9800 . ? C8X H8X3 0.9800 . ? C9 C10 1.484(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.347(6) . ? C11 C12 1.420(6) . ? C11 H11 0.9500 . ? C12 C13 1.522(7) . ? C13 C14 1.516(10) . ? C13 C16 1.531(11) . ? C13 C15 1.554(9) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C14X H14D 0.9800 . ? C14X H14E 0.9800 . ? C14X H14F 0.9800 . ? C15X H15D 0.9800 . ? C15X H15E 0.9800 . ? C15X H15F 0.9800 . ? C16X H16D 0.9800 . ? C16X H16E 0.9800 . ? C16X H16F 0.9800 . ? C14Y H14G 0.9800 . ? C14Y H14H 0.9800 . ? C14Y H14I 0.9800 . ? C15Y H15G 0.9800 . ? C15Y H15H 0.9800 . ? C15Y H15I 0.9800 . ? C16Y H16G 0.9800 . ? C16Y H16H 0.9800 . ? C16Y H16I 0.9800 . ? C17 C18 1.489(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.370(6) . ? C19 C20 1.413(6) . ? C19 H19 0.9500 . ? C20 C21 1.530(6) . ? C21 C23X 1.320(15) . ? C21 C23 1.405(9) . ? C21 C22 1.564(10) . ? C21 C22X 1.575(17) . ? C21 C24 1.603(9) . ? C21 C24X 1.615(16) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C22X H22D 0.9800 . ? C22X H22E 0.9800 . ? C22X H22F 0.9800 . ? C23X H23D 0.9800 . ? C23X H23E 0.9800 . ? C23X H23F 0.9800 . ? C24X H24D 0.9800 . ? C24X H24E 0.9800 . ? C24X H24F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O6 94.38(12) . 3_756 ? O1 Co1 O5 94.86(12) . 3_756 ? O6 Co1 O5 88.21(12) 3_756 3_756 ? O1 Co1 O2 86.90(12) . . ? O6 Co1 O2 90.33(12) 3_756 . ? O5 Co1 O2 177.79(12) 3_756 . ? O1 Co1 O3 166.10(11) . . ? O6 Co1 O3 93.03(12) 3_756 . ? O5 Co1 O3 97.10(11) 3_756 . ? O2 Co1 O3 81.32(11) . . ? O1 Co1 O3 92.76(12) . 3_756 ? O6 Co1 O3 168.69(11) 3_756 3_756 ? O5 Co1 O3 82.45(11) 3_756 3_756 ? O2 Co1 O3 98.81(11) . 3_756 ? O3 Co1 O3 81.86(12) . 3_756 ? O1 Co1 Li1 100.04(18) . 3_756 ? O6 Co1 Li1 127.87(18) 3_756 3_756 ? O5 Co1 Li1 41.08(17) 3_756 3_756 ? O2 Co1 Li1 139.90(17) . 3_756 ? O3 Co1 Li1 84.54(17) . 3_756 ? O3 Co1 Li1 41.86(17) 3_756 3_756 ? O4 Li1 O2 125.3(4) . . ? O4 Li1 O5 116.7(4) . . ? O2 Li1 O5 116.5(4) . . ? O4 Li1 O3 100.1(4) . . ? O2 Li1 O3 90.5(3) . . ? O5 Li1 O3 91.3(3) . . ? O4 Li1 Co1 122.6(3) . 3_756 ? O2 Li1 Co1 104.2(3) . 3_756 ? O5 Li1 Co1 43.85(17) . 3_756 ? O3 Li1 Co1 48.03(17) . 3_756 ? C4 O1 Co1 125.6(3) . . ? C2 O2 Li1 139.7(4) . . ? C2 O2 Co1 120.2(3) . . ? Li1 O2 Co1 95.4(3) . . ? C10 O3 Li1 119.2(4) . . ? C10 O3 Co1 126.3(3) . . ? Li1 O3 Co1 90.9(3) . . ? C10 O3 Co1 122.8(2) . 3_756 ? Li1 O3 Co1 90.1(2) . 3_756 ? Co1 O3 Co1 98.14(12) . 3_756 ? C12 O4 Li1 123.8(4) . . ? C18 O5 Li1 139.0(4) . . ? C18 O5 Co1 125.2(3) . 3_756 ? Li1 O5 Co1 95.1(3) . 3_756 ? C20 O6 Co1 127.3(3) . 3_756 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 C3 125.6(4) . . ? O2 C2 C1 113.1(4) . . ? C3 C2 C1 121.3(4) . . ? C2 C3 C4 125.2(4) . . ? C2 C3 H3 117.4 . . ? C4 C3 H3 117.4 . . ? O1 C4 C3 123.2(4) . . ? O1 C4 C5 115.7(4) . . ? C3 C4 C5 121.1(4) . . ? C6 C5 C7 108.1(8) . . ? C6 C5 C4 109.8(6) . . ? C7 C5 C4 114.3(6) . . ? C6 C5 C7X 123.8(8) . . ? C4 C5 C7X 115.0(6) . . ? C6 C5 C8 107.9(8) . . ? C7 C5 C8 111.6(7) . . ? C4 C5 C8 104.9(6) . . ? C4 C5 C6X 104.9(6) . . ? C7X C5 C6X 109.6(8) . . ? C8 C5 C6X 130.7(8) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? C5 C6X H6X1 109.5 . . ? C5 C6X H6X2 109.5 . . ? H6X1 C6X H6X2 109.5 . . ? C5 C6X H6X3 109.5 . . ? H6X1 C6X H6X3 109.5 . . ? H6X2 C6X H6X3 109.5 . . ? C5 C7X H7X1 109.5 . . ? C5 C7X H7X2 109.5 . . ? H7X1 C7X H7X2 109.5 . . ? C5 C7X H7X3 109.5 . . ? H7X1 C7X H7X3 109.5 . . ? H7X2 C7X H7X3 109.5 . . ? C5 C8X H8X1 109.5 . . ? C5 C8X H8X2 109.5 . . ? H8X1 C8X H8X2 109.5 . . ? C5 C8X H8X3 109.5 . . ? H8X1 C8X H8X3 109.5 . . ? H8X2 C8X H8X3 109.5 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O3 C10 C11 124.3(4) . . ? O3 C10 C9 116.3(4) . . ? C11 C10 C9 119.4(4) . . ? C10 C11 C12 128.4(5) . . ? C10 C11 H11 115.8 . . ? C12 C11 H11 115.8 . . ? O4 C12 C11 123.9(5) . . ? O4 C12 C13 116.7(4) . . ? C11 C12 C13 119.3(5) . . ? C14 C13 C12 104.8(9) . . ? C14 C13 C16 111.1(12) . . ? C12 C13 C16 105.9(9) . . ? C14 C13 C15 112.7(10) . . ? C12 C13 C15 113.6(7) . . ? C16 C13 C15 108.6(11) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? H14D C14X H14E 109.5 . . ? H14D C14X H14F 109.5 . . ? H14E C14X H14F 109.5 . . ? H15D C15X H15E 109.5 . . ? H15D C15X H15F 109.5 . . ? H15E C15X H15F 109.5 . . ? H16D C16X H16E 109.5 . . ? H16D C16X H16F 109.5 . . ? H16E C16X H16F 109.5 . . ? H14G C14Y H14H 109.5 . . ? H14G C14Y H14I 109.5 . . ? H14H C14Y H14I 109.5 . . ? H15G C15Y H15H 109.5 . . ? H15G C15Y H15I 109.5 . . ? H15H C15Y H15I 109.5 . . ? H16G C16Y H16H 109.5 . . ? H16G C16Y H16I 109.5 . . ? H16H C16Y H16I 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O5 C18 C19 125.1(4) . . ? O5 C18 C17 114.6(4) . . ? C19 C18 C17 120.3(4) . . ? C18 C19 C20 125.1(4) . . ? C18 C19 H19 117.5 . . ? C20 C19 H19 117.5 . . ? O6 C20 C19 124.1(4) . . ? O6 C20 C21 116.9(4) . . ? C19 C20 C21 118.9(4) . . ? C23X C21 C23 136.2(9) . . ? C23X C21 C20 108.2(8) . . ? C23 C21 C20 113.6(5) . . ? C23 C21 C22 113.5(7) . . ? C20 C21 C22 107.8(5) . . ? C23X C21 C22X 116.7(11) . . ? C20 C21 C22X 101.5(7) . . ? C22 C21 C22X 149.0(8) . . ? C23 C21 C24 110.1(6) . . ? C20 C21 C24 107.8(5) . . ? C22 C21 C24 103.5(5) . . ? C22X C21 C24 76.4(8) . . ? C23 C21 C24X 60.0(7) . . ? C20 C21 C24X 111.0(6) . . ? C22X C21 C24X 102.6(9) . . ? C24 C21 C24X 140.4(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? C21 C22X H22D 109.5 . . ? C21 C22X H22E 109.5 . . ? H22D C22X H22E 109.5 . . ? C21 C22X H22F 109.5 . . ? H22D C22X H22F 109.5 . . ? H22E C22X H22F 109.5 . . ? C21 C23X H23D 109.5 . . ? C21 C23X H23E 109.5 . . ? H23D C23X H23E 109.5 . . ? C21 C23X H23F 109.5 . . ? H23D C23X H23F 109.5 . . ? H23E C23X H23F 109.5 . . ? C21 C24X H24D 109.5 . . ? C21 C24X H24E 109.5 . . ? H24D C24X H24E 109.5 . . ? C21 C24X H24F 109.5 . . ? H24D C24X H24F 109.5 . . ? H24E C24X H24F 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.544 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.079 _database_code_depnum_ccdc_archive 'CCDC 954094' ####################################################################### # # 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_Co3(tbaoac)6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H78 Co3 O18' _chemical_formula_sum 'C48 H78 Co3 O18' _chemical_formula_weight 1119.89 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 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn ' _symmetry_int_tables_number 14 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 9.7761(11) _cell_length_b 16.9962(19) _cell_length_c 17.5593(19) _cell_angle_alpha 90.00 _cell_angle_beta 100.9190(10) _cell_angle_gamma 90.00 _cell_volume 2864.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9920 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.79 _exptl_crystal_description cube _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1182 _exptl_absorpt_coefficient_mu 0.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS (Bruker-AXS, 2003) ; _exptl_absorpt_correction_T_min 0.8740 _exptl_absorpt_correction_T_max 0.8895 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area-detector' _diffrn_measurement_method '0.30\% \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 51810 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.92 _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 6666 _reflns_number_gt 5764 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART Ver. 5.622 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT Ver. 6.22 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT Ver. 6.22' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _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^)+(0.0494P)^2^+0.5227P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6666 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_diff_density_max 0.876 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.063 _refine_ls_shift/su_max 0.001 _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 0.0000 1.0000 0.0000 0.01580(8) Uani 1 2 d S . . Co2 Co 0.134439(19) 0.931154(11) 0.141420(11) 0.01786(7) Uani 1 1 d . . . O1 O 0.00326(10) 0.88507(6) 0.04417(6) 0.0193(2) Uani 1 1 d . . . O2 O 0.25239(11) 0.83122(6) 0.14434(6) 0.0264(2) Uani 1 1 d . . . O3 O 0.32693(13) 0.71668(7) 0.10305(7) 0.0333(3) Uani 1 1 d . . . O4 O 0.21016(10) 0.99116(6) 0.05538(6) 0.0190(2) Uani 1 1 d . . . O5 O 0.28990(11) 0.98079(7) 0.22239(6) 0.0237(2) Uani 1 1 d . . . O6 O 0.49616(11) 1.04009(7) 0.26522(6) 0.0289(3) Uani 1 1 d . . . O7 O -0.01237(10) 1.02094(6) 0.11647(6) 0.0184(2) Uani 1 1 d . . . O8 O 0.03725(11) 0.89718(6) 0.22867(6) 0.0237(2) Uani 1 1 d . . . O9 O -0.12402(11) 0.89402(7) 0.30429(6) 0.0282(3) Uani 1 1 d . . . C1 C -0.10214(17) 0.79738(10) -0.05531(9) 0.0280(3) Uani 1 1 d . . . H1A H -0.1905 0.7924 -0.0371 0.042 Uiso 1 1 calc R . . H1B H -0.0810 0.7477 -0.0789 0.042 Uiso 1 1 calc R . . H1C H -0.1097 0.8396 -0.0939 0.042 Uiso 1 1 calc R . . C2 C 0.01299(15) 0.81658(9) 0.01233(8) 0.0207(3) Uani 1 1 d . . . C3 C 0.11700(17) 0.76295(9) 0.03643(9) 0.0251(3) Uani 1 1 d . . . H3 H 0.1115 0.7139 0.0101 0.030 Uiso 1 1 calc R . . C4 C 0.23327(16) 0.77537(9) 0.09836(9) 0.0245(3) Uani 1 1 d . . . C5 C 0.45487(19) 0.71647(12) 0.16313(11) 0.0393(4) Uani 1 1 d . . . C6 C 0.5251(2) 0.64026(15) 0.14462(13) 0.0587(7) Uani 1 1 d . . . H6A H 0.4629 0.5957 0.1479 0.088 Uiso 1 1 calc R . . H6B H 0.6123 0.6330 0.1820 0.088 Uiso 1 1 calc R . . H6C H 0.5452 0.6433 0.0921 0.088 Uiso 1 1 calc R . . C7 C 0.4169(2) 0.71049(14) 0.24289(11) 0.0481(5) Uani 1 1 d . . . H7A H 0.3673 0.7582 0.2533 0.072 Uiso 1 1 calc R . . H7B H 0.5020 0.7048 0.2822 0.072 Uiso 1 1 calc R . . H7C H 0.3569 0.6646 0.2446 0.072 Uiso 1 1 calc R . . C8 C 0.5455(2) 0.78692(15) 0.15418(14) 0.0556(6) Uani 1 1 d . . . H8A H 0.5617 0.7892 0.1008 0.083 Uiso 1 1 calc R . . H8B H 0.6349 0.7820 0.1901 0.083 Uiso 1 1 calc R . . H8C H 0.4986 0.8352 0.1658 0.083 Uiso 1 1 calc R . . C9 C -0.21092(15) 1.10129(9) 0.11708(9) 0.0222(3) Uani 1 1 d . . . H9A H -0.1532 1.1486 0.1181 0.033 Uiso 1 1 calc R . . H9B H -0.2817 1.1099 0.1490 0.033 Uiso 1 1 calc R . . H9C H -0.2567 1.0901 0.0635 0.033 Uiso 1 1 calc R . . C10 C -0.12055(14) 1.03256(8) 0.14870(8) 0.0182(3) Uani 1 1 d . . . C11 C -0.15281(15) 0.98885(9) 0.20842(9) 0.0213(3) Uani 1 1 d . . . H11 H -0.2351 1.0021 0.2269 0.026 Uiso 1 1 calc R . . C12 C -0.07104(15) 0.92447(9) 0.24497(9) 0.0216(3) Uani 1 1 d . . . C13 C -0.04643(18) 0.83343(11) 0.35559(11) 0.0362(4) Uani 1 1 d . . . C14 C -0.0260(2) 0.75952(12) 0.31055(14) 0.0513(5) Uani 1 1 d . . . H14A H -0.1155 0.7433 0.2792 0.077 Uiso 1 1 calc R . . H14B H 0.0101 0.7173 0.3469 0.077 Uiso 1 1 calc R . . H14C H 0.0405 0.7702 0.2765 0.077 Uiso 1 1 calc R . . C15 C 0.0902(2) 0.86809(14) 0.39846(11) 0.0476(5) Uani 1 1 d . . . H15A H 0.1532 0.8764 0.3619 0.071 Uiso 1 1 calc R . . H15B H 0.1334 0.8317 0.4393 0.071 Uiso 1 1 calc R . . H15C H 0.0720 0.9185 0.4218 0.071 Uiso 1 1 calc R . . C16 C -0.1446(2) 0.81667(14) 0.41138(12) 0.0486(5) Uani 1 1 d . . . H16A H -0.1598 0.8651 0.4389 0.073 Uiso 1 1 calc R . . H16B H -0.1033 0.7766 0.4489 0.073 Uiso 1 1 calc R . . H16C H -0.2339 0.7976 0.3822 0.073 Uiso 1 1 calc R . . C17 C 0.35357(16) 1.07246(9) -0.00786(9) 0.0246(3) Uani 1 1 d . . . H17A H 0.3850 1.0319 -0.0403 0.037 Uiso 1 1 calc R . . H17B H 0.4272 1.1119 0.0064 0.037 Uiso 1 1 calc R . . H17C H 0.2696 1.0979 -0.0367 0.037 Uiso 1 1 calc R . . C18 C 0.32131(15) 1.03510(9) 0.06457(9) 0.0196(3) Uani 1 1 d . . . C19 C 0.40975(15) 1.04730(9) 0.13410(9) 0.0238(3) Uani 1 1 d . . . H19 H 0.4913 1.0773 0.1331 0.029 Uiso 1 1 calc R . . C20 C 0.39043(15) 1.01902(9) 0.20797(9) 0.0222(3) Uani 1 1 d . . . C21 C 0.49931(17) 1.01632(11) 0.34659(9) 0.0298(4) Uani 1 1 d . . . C22 C 0.3770(2) 1.05192(13) 0.37592(11) 0.0432(5) Uani 1 1 d . . . H22A H 0.3738 1.1087 0.3660 0.065 Uiso 1 1 calc R . . H22B H 0.3878 1.0425 0.4318 0.065 Uiso 1 1 calc R . . H22C H 0.2904 1.0276 0.3490 0.065 Uiso 1 1 calc R . . C23 C 0.5052(2) 0.92767(11) 0.35388(11) 0.0385(4) Uani 1 1 d . . . H23A H 0.4161 0.9052 0.3282 0.058 Uiso 1 1 calc R . . H23B H 0.5234 0.9130 0.4088 0.058 Uiso 1 1 calc R . . H23C H 0.5801 0.9074 0.3293 0.058 Uiso 1 1 calc R . . C24 C 0.6360(2) 1.05264(15) 0.38808(11) 0.0499(6) Uani 1 1 d . . . H24A H 0.7134 1.0309 0.3666 0.075 Uiso 1 1 calc R . . H24B H 0.6498 1.0406 0.4436 0.075 Uiso 1 1 calc R . . H24C H 0.6325 1.1098 0.3807 0.075 Uiso 1 1 calc 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 Co1 0.01436(14) 0.01729(14) 0.01572(14) 0.00142(10) 0.00275(10) 0.00021(9) Co2 0.01541(11) 0.02046(11) 0.01751(11) 0.00263(7) 0.00260(8) 0.00081(7) O1 0.0187(5) 0.0178(5) 0.0211(5) 0.0015(4) 0.0032(4) 0.0007(4) O2 0.0251(6) 0.0284(6) 0.0253(6) 0.0033(5) 0.0038(4) 0.0074(4) O3 0.0374(7) 0.0349(7) 0.0289(6) 0.0072(5) 0.0093(5) 0.0183(5) O4 0.0156(5) 0.0226(5) 0.0184(5) 0.0019(4) 0.0024(4) -0.0021(4) O5 0.0200(5) 0.0307(6) 0.0198(5) 0.0022(4) 0.0018(4) -0.0031(4) O6 0.0250(6) 0.0395(7) 0.0203(6) 0.0003(5) -0.0006(4) -0.0094(5) O7 0.0164(5) 0.0210(5) 0.0182(5) 0.0013(4) 0.0049(4) 0.0009(4) O8 0.0215(5) 0.0267(6) 0.0238(6) 0.0065(4) 0.0066(4) 0.0019(4) O9 0.0242(6) 0.0349(6) 0.0272(6) 0.0125(5) 0.0097(5) 0.0031(5) C1 0.0292(8) 0.0253(8) 0.0292(8) -0.0061(7) 0.0044(7) -0.0032(6) C2 0.0229(7) 0.0210(7) 0.0202(7) 0.0015(6) 0.0089(6) -0.0029(6) C3 0.0319(8) 0.0193(7) 0.0258(8) 0.0012(6) 0.0104(7) 0.0030(6) C4 0.0276(8) 0.0238(8) 0.0247(8) 0.0089(6) 0.0117(6) 0.0084(6) C5 0.0348(10) 0.0518(12) 0.0318(9) 0.0150(8) 0.0076(8) 0.0217(8) C6 0.0599(14) 0.0693(15) 0.0482(13) 0.0155(11) 0.0135(11) 0.0426(12) C7 0.0485(12) 0.0633(14) 0.0328(10) 0.0161(9) 0.0088(9) 0.0251(10) C8 0.0281(10) 0.0778(16) 0.0597(14) 0.0220(12) 0.0052(9) 0.0108(10) C9 0.0203(7) 0.0217(7) 0.0250(8) 0.0001(6) 0.0054(6) 0.0022(6) C10 0.0169(7) 0.0196(7) 0.0179(7) -0.0029(6) 0.0027(5) -0.0020(5) C11 0.0178(7) 0.0257(8) 0.0215(7) 0.0002(6) 0.0067(6) -0.0006(6) C12 0.0200(7) 0.0264(8) 0.0187(7) 0.0016(6) 0.0042(6) -0.0053(6) C13 0.0316(9) 0.0427(10) 0.0360(10) 0.0217(8) 0.0107(7) 0.0068(7) C14 0.0582(13) 0.0365(11) 0.0645(14) 0.0213(10) 0.0249(11) 0.0075(9) C15 0.0359(10) 0.0710(15) 0.0349(10) 0.0230(10) 0.0041(8) 0.0043(10) C16 0.0412(11) 0.0626(14) 0.0459(12) 0.0318(10) 0.0182(9) 0.0083(10) C17 0.0216(8) 0.0303(8) 0.0223(8) 0.0025(6) 0.0051(6) -0.0044(6) C18 0.0172(7) 0.0203(7) 0.0222(7) 0.0001(6) 0.0056(6) 0.0018(5) C19 0.0189(7) 0.0278(8) 0.0245(8) 0.0013(6) 0.0038(6) -0.0048(6) C20 0.0183(7) 0.0252(8) 0.0225(8) -0.0026(6) 0.0024(6) 0.0010(6) C21 0.0276(8) 0.0413(10) 0.0193(8) -0.0008(7) 0.0010(6) -0.0071(7) C22 0.0482(12) 0.0524(12) 0.0287(9) -0.0074(9) 0.0066(8) 0.0034(9) C23 0.0360(10) 0.0446(11) 0.0312(10) 0.0066(8) -0.0032(8) 0.0035(8) C24 0.0442(12) 0.0758(15) 0.0253(9) 0.0002(10) -0.0047(8) -0.0242(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.0997(10) . yes Co1 O1 2.0997(10) 3_575 yes Co1 O7 2.1018(10) . yes Co1 O7 2.1018(10) 3_575 yes Co1 O4 2.1053(10) . yes Co1 O4 2.1053(10) 3_575 yes Co1 Co2 2.8331(3) 3_575 yes Co1 Co2 2.8331(3) . yes Co2 O8 2.0334(10) . yes Co2 O2 2.0481(11) . yes Co2 O5 2.0553(11) . yes Co2 O4 2.0723(10) . yes Co2 O7 2.0838(10) . yes Co2 O1 2.0843(10) . yes O1 C2 1.3027(18) . ? O2 C4 1.237(2) . ? O3 C4 1.3460(18) . ? O3 C5 1.476(2) . ? O4 C18 1.3031(17) . ? O5 C20 1.2435(19) . ? O6 C20 1.3467(18) . ? O6 C21 1.4796(19) . ? O7 C10 1.3055(17) . ? O8 C12 1.2380(18) . ? O9 C12 1.3511(18) . ? O9 C13 1.4794(19) . ? C1 C2 1.509(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.371(2) . ? C3 C4 1.432(2) . ? C3 H3 0.9500 . ? C5 C8 1.515(3) . ? C5 C7 1.519(3) . ? C5 C6 1.530(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.506(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.370(2) . ? C11 C12 1.433(2) . ? C11 H11 0.9500 . ? C13 C14 1.518(3) . ? C13 C15 1.522(3) . ? C13 C16 1.522(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.507(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.372(2) . ? C19 C20 1.429(2) . ? C19 H19 0.9500 . ? C21 C23 1.512(3) . ? C21 C22 1.514(3) . ? C21 C24 1.526(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1 180.0 . 3_575 yes O1 Co1 O7 78.33(4) . . yes O1 Co1 O7 101.67(4) 3_575 . yes O1 Co1 O7 101.67(4) . 3_575 yes O1 Co1 O7 78.33(4) 3_575 3_575 yes O7 Co1 O7 180.0 . 3_575 yes O1 Co1 O4 79.50(4) . . yes O1 Co1 O4 100.50(4) 3_575 . yes O7 Co1 O4 78.09(4) . . yes O7 Co1 O4 101.91(4) 3_575 . yes O1 Co1 O4 100.50(4) . 3_575 yes O1 Co1 O4 79.50(4) 3_575 3_575 yes O7 Co1 O4 101.91(4) . 3_575 yes O7 Co1 O4 78.09(4) 3_575 3_575 yes O4 Co1 O4 180.0 . 3_575 yes O1 Co1 Co2 132.85(3) . 3_575 yes O1 Co1 Co2 47.15(3) 3_575 3_575 yes O7 Co1 Co2 132.87(3) . 3_575 yes O7 Co1 Co2 47.14(3) 3_575 3_575 yes O4 Co1 Co2 133.19(3) . 3_575 yes O4 Co1 Co2 46.81(3) 3_575 3_575 yes O1 Co1 Co2 47.15(3) . . yes O1 Co1 Co2 132.85(3) 3_575 . yes O7 Co1 Co2 47.13(3) . . yes O7 Co1 Co2 132.86(3) 3_575 . yes O4 Co1 Co2 46.81(3) . . yes O4 Co1 Co2 133.19(3) 3_575 . yes Co2 Co1 Co2 180.0 3_575 . yes O8 Co2 O2 94.99(4) . . yes O8 Co2 O5 89.15(4) . . yes O2 Co2 O5 89.09(4) . . yes O8 Co2 O4 166.28(4) . . yes O2 Co2 O4 98.58(4) . . yes O5 Co2 O4 89.02(4) . . yes O8 Co2 O7 87.98(4) . . yes O2 Co2 O7 167.07(4) . . yes O5 Co2 O7 103.56(4) . . yes O4 Co2 O7 79.24(4) . . yes O8 Co2 O1 101.99(4) . . yes O2 Co2 O1 87.99(4) . . yes O5 Co2 O1 168.68(4) . . yes O4 Co2 O1 80.62(4) . . yes O7 Co2 O1 79.08(4) . . yes O8 Co2 Co1 124.91(3) . . yes O2 Co2 Co1 122.00(3) . . yes O5 Co2 Co1 126.60(3) . . yes O4 Co2 Co1 47.79(3) . . yes O7 Co2 Co1 47.67(3) . . yes O1 Co2 Co1 47.61(3) . . yes C2 O1 Co2 127.14(9) . . ? C2 O1 Co1 132.07(9) . . ? Co2 O1 Co1 85.24(4) . . ? C4 O2 Co2 127.24(10) . . ? C4 O3 C5 121.34(14) . . ? C18 O4 Co2 126.61(9) . . ? C18 O4 Co1 137.24(9) . . ? Co2 O4 Co1 85.40(4) . . ? C20 O5 Co2 125.66(10) . . ? C20 O6 C21 121.39(12) . . ? C10 O7 Co2 127.01(9) . . ? C10 O7 Co1 130.39(9) . . ? Co2 O7 Co1 85.20(4) . . ? C12 O8 Co2 127.59(10) . . ? C12 O9 C13 120.58(12) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.86(14) . . ? O1 C2 C1 115.26(13) . . ? C3 C2 C1 119.87(14) . . ? C2 C3 C4 124.88(14) . . ? C2 C3 H3 117.6 . . ? C4 C3 H3 117.6 . . ? O2 C4 O3 120.78(15) . . ? O2 C4 C3 127.49(14) . . ? O3 C4 C3 111.72(14) . . ? O3 C5 C8 110.93(14) . . ? O3 C5 C7 109.72(15) . . ? C8 C5 C7 113.47(19) . . ? O3 C5 C6 101.78(17) . . ? C8 C5 C6 110.61(18) . . ? C7 C5 C6 109.71(16) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O7 C10 C11 124.93(13) . . ? O7 C10 C9 115.11(12) . . ? C11 C10 C9 119.93(13) . . ? C10 C11 C12 124.55(14) . . ? C10 C11 H11 117.7 . . ? C12 C11 H11 117.7 . . ? O8 C12 O9 120.29(14) . . ? O8 C12 C11 127.68(14) . . ? O9 C12 C11 112.02(13) . . ? O9 C13 C14 111.21(15) . . ? O9 C13 C15 109.41(15) . . ? C14 C13 C15 112.86(17) . . ? O9 C13 C16 102.06(13) . . ? C14 C13 C16 109.97(17) . . ? C15 C13 C16 110.81(17) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 C19 124.55(14) . . ? O4 C18 C17 116.09(13) . . ? C19 C18 C17 119.34(13) . . ? C18 C19 C20 125.99(14) . . ? C18 C19 H19 117.0 . . ? C20 C19 H19 117.0 . . ? O5 C20 O6 120.76(14) . . ? O5 C20 C19 127.31(14) . . ? O6 C20 C19 111.92(13) . . ? O6 C21 C23 110.32(14) . . ? O6 C21 C22 110.24(14) . . ? C23 C21 C22 112.92(16) . . ? O6 C21 C24 101.93(13) . . ? C23 C21 C24 110.28(17) . . ? C22 C21 C24 110.62(16) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? #---END _database_code_depnum_ccdc_archive 'CCDC 954095'