# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Zheming Wang' _publ_contact_author_email zmw@pku.edu.cn loop_ _publ_author_name 'Zheming Wang' 'Zhiming Duan' 'Song Gao' data_1-at-110K _database_code_depnum_ccdc_archive 'CCDC 784051' #TrackingRef '1-110K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H3 Co K O6' _chemical_formula_weight 233.08 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' K K 0.2009 0.2494 '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 'P 6(3)22' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' _cell_length_a 6.9978(2) _cell_length_b 6.9978(2) _cell_length_c 8.4687(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 359.15(2) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2186 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 30.034 _exptl_crystal_description 'hexagonal bipyramid' _exptl_crystal_colour pink _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 230 _exptl_absorpt_coefficient_mu 2.947 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.485 _exptl_absorpt_correction_T_max 0.559 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'NONIUS KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 7164 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 29.95 _reflns_number_total 355 _reflns_number_gt 295 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0363P)^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 SHELXL _refine_ls_extinction_coef 0.068(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 355 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0524 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.3333 0.6667 0.7500 0.01288(19) Uani 1 6 d S . . K1 K 1.0000 1.0000 0.7500 0.0183(2) Uani 1 6 d S . . O1 O 0.5958(2) 0.89895(18) 0.88981(13) 0.0189(3) Uani 1 1 d . . . C1 C 0.5650(4) 1.0000 1.0000 0.0234(6) Uani 1 2 d S . . H1 H 0.4293 1.0000 1.0000 0.028 Uiso 1 2 calc SR . . 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) 0.0091(3) 0.000 0.000 0.00739(11) K1 0.0175(3) 0.0175(3) 0.0199(4) 0.000 0.000 0.00875(14) O1 0.0197(6) 0.0204(6) 0.0153(5) -0.0041(6) -0.0006(5) 0.0091(5) C1 0.0197(9) 0.0264(15) 0.0262(13) -0.0114(10) -0.0057(5) 0.0132(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.1053(12) 11_556 ? Co1 O1 2.1053(12) 2_665 ? Co1 O1 2.1053(12) . ? Co1 O1 2.1053(12) 10_666 ? Co1 O1 2.1053(12) 12_566 ? Co1 O1 2.1053(12) 3_565 ? K1 O1 2.8110(12) 12_566 ? K1 O1 2.8110(12) 3_675 ? K1 O1 2.8110(12) 10_776 ? K1 O1 2.8110(12) 11_656 ? K1 O1 2.8110(12) 2_765 ? K1 O1 2.8110(12) . ? K1 K1 4.23435(18) 4_775 ? K1 K1 4.2343(2) 4_774 ? O1 C1 1.2528(16) . ? C1 O1 1.2528(16) 8_677 ? C1 H1 0.9500 . ? 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 81.85(6) 11_556 2_665 ? O1 Co1 O1 96.08(6) 11_556 . ? O1 Co1 O1 91.46(4) 2_665 . ? O1 Co1 O1 91.46(4) 11_556 10_666 ? O1 Co1 O1 96.08(6) 2_665 10_666 ? O1 Co1 O1 170.02(6) . 10_666 ? O1 Co1 O1 91.46(4) 11_556 12_566 ? O1 Co1 O1 170.02(6) 2_665 12_566 ? O1 Co1 O1 81.85(6) . 12_566 ? O1 Co1 O1 91.46(4) 10_666 12_566 ? O1 Co1 O1 170.02(6) 11_556 3_565 ? O1 Co1 O1 91.46(4) 2_665 3_565 ? O1 Co1 O1 91.46(4) . 3_565 ? O1 Co1 O1 81.85(6) 10_666 3_565 ? O1 Co1 O1 96.08(6) 12_566 3_565 ? O1 K1 O1 154.83(4) 12_566 3_675 ? O1 K1 O1 103.52(3) 12_566 10_776 ? O1 K1 O1 58.76(5) 3_675 10_776 ? O1 K1 O1 103.52(3) 12_566 11_656 ? O1 K1 O1 98.38(4) 3_675 11_656 ? O1 K1 O1 103.52(3) 10_776 11_656 ? O1 K1 O1 98.38(4) 12_566 2_765 ? O1 K1 O1 103.52(3) 3_675 2_765 ? O1 K1 O1 154.83(4) 10_776 2_765 ? O1 K1 O1 58.76(5) 11_656 2_765 ? O1 K1 O1 58.76(5) 12_566 . ? O1 K1 O1 103.52(3) 3_675 . ? O1 K1 O1 98.38(4) 10_776 . ? O1 K1 O1 154.83(4) 11_656 . ? O1 K1 O1 103.52(3) 2_765 . ? O1 K1 K1 114.91(2) 12_566 4_775 ? O1 K1 K1 65.09(2) 3_675 4_775 ? O1 K1 K1 114.91(2) 10_776 4_775 ? O1 K1 K1 114.91(2) 11_656 4_775 ? O1 K1 K1 65.09(2) 2_765 4_775 ? O1 K1 K1 65.09(2) . 4_775 ? O1 K1 K1 65.09(2) 12_566 4_774 ? O1 K1 K1 114.91(2) 3_675 4_774 ? O1 K1 K1 65.09(2) 10_776 4_774 ? O1 K1 K1 65.09(2) 11_656 4_774 ? O1 K1 K1 114.91(2) 2_765 4_774 ? O1 K1 K1 114.91(2) . 4_774 ? K1 K1 K1 180.0 4_775 4_774 ? C1 O1 Co1 121.66(12) . . ? C1 O1 K1 127.38(11) . . ? Co1 O1 K1 109.70(4) . . ? O1 C1 O1 126.0(2) 8_677 . ? O1 C1 H1 117.0 8_677 . ? O1 C1 H1 117.0 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.95 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.472 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.071 # Attachment '1-180K.cif' data_1-at-180K _database_code_depnum_ccdc_archive 'CCDC 784052' #TrackingRef '1-180K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H3 Co K O6' _chemical_formula_weight 233.08 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' K K 0.2009 0.2494 '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 'P 6(3)22' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' _cell_length_a 6.9930(13) _cell_length_b 6.9930(13) _cell_length_c 8.4439(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 357.60(11) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2886 _cell_measurement_theta_min 3.3617 _cell_measurement_theta_max 27.4835 _exptl_crystal_description 'hexagonal bipyramid' _exptl_crystal_colour pink _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 230 _exptl_absorpt_coefficient_mu 2.959 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8289 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_source_power '5.4 kW' _diffrn_source_voltage 50.0000 _diffrn_source_current 100.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_method CCD _diffrn_measurement_device_type 'Rigaku Mercury CCD (AFC7)' _diffrn_detector_area_resol_mean 15 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5906 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 27.43 _reflns_number_total 275 _reflns_number_gt 248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; data collect, cell refinement and data reduction: "CrystalClear" software, Rigaku Corp., Japan, 2000. absorption correction: Jacobson, R. (1998). Private Communication. Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0269P)^2^+0.0264P] 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 SHELXL _refine_ls_extinction_coef 0.027(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(4) _refine_ls_number_reflns 275 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.0189 _refine_ls_wR_factor_ref 0.0465 _refine_ls_wR_factor_gt 0.0454 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.178 _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 0.6667 0.3333 0.2500 0.0120(2) Uani 1 6 d S . . K1 K 0.0000 0.0000 0.2500 0.0202(3) Uani 1 6 d S . . O1 O 0.4045(2) 0.1009(2) 0.10966(14) 0.0195(3) Uani 1 1 d . . . C1 C 0.4346(4) 0.0000 0.0000 0.0256(7) Uani 1 2 d S . . H1 H 0.5704 0.0000 0.0000 0.031 Uiso 1 2 calc SR . . 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 0.0138(2) 0.0138(2) 0.0083(3) 0.000 0.000 0.00690(11) K1 0.0184(3) 0.0184(3) 0.0238(5) 0.000 0.000 0.00918(16) O1 0.0190(6) 0.0217(6) 0.0167(5) -0.0068(6) -0.0014(5) 0.0093(5) C1 0.0198(10) 0.0329(18) 0.0285(13) -0.0154(12) -0.0077(6) 0.0164(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 2.1040(13) 11_655 ? Co1 O1 2.1040(13) . ? Co1 O1 2.1040(13) 10_665 ? Co1 O1 2.1040(13) 2_655 ? Co1 O1 2.1040(13) 12 ? Co1 O1 2.1040(13) 3_665 ? K1 O1 2.8122(13) 12 ? K1 O1 2.8122(13) 3 ? K1 O1 2.8122(13) . ? K1 O1 2.8122(13) 2 ? K1 O1 2.8122(13) 10 ? K1 O1 2.8122(13) 11 ? K1 K1 4.2219(7) 4 ? K1 K1 4.2219(7) 4_554 ? O1 C1 1.2441(17) . ? C1 O1 1.2441(17) 8 ? C1 H1 0.9500 . ? 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 96.02(6) 11_655 . ? O1 Co1 O1 91.38(5) 11_655 10_665 ? O1 Co1 O1 170.19(6) . 10_665 ? O1 Co1 O1 82.03(6) 11_655 2_655 ? O1 Co1 O1 91.38(5) . 2_655 ? O1 Co1 O1 96.02(6) 10_665 2_655 ? O1 Co1 O1 91.38(5) 11_655 12 ? O1 Co1 O1 82.03(6) . 12 ? O1 Co1 O1 91.38(5) 10_665 12 ? O1 Co1 O1 170.19(6) 2_655 12 ? O1 Co1 O1 170.19(6) 11_655 3_665 ? O1 Co1 O1 91.38(5) . 3_665 ? O1 Co1 O1 82.03(6) 10_665 3_665 ? O1 Co1 O1 91.38(5) 2_655 3_665 ? O1 Co1 O1 96.02(6) 12 3_665 ? O1 K1 O1 154.90(5) 12 3 ? O1 K1 O1 58.81(5) 12 . ? O1 K1 O1 103.51(3) 3 . ? O1 K1 O1 98.34(5) 12 2 ? O1 K1 O1 103.51(3) 3 2 ? O1 K1 O1 103.51(3) . 2 ? O1 K1 O1 103.51(3) 12 10 ? O1 K1 O1 58.81(5) 3 10 ? O1 K1 O1 98.34(5) . 10 ? O1 K1 O1 154.90(5) 2 10 ? O1 K1 O1 103.51(3) 12 11 ? O1 K1 O1 98.34(5) 3 11 ? O1 K1 O1 154.90(5) . 11 ? O1 K1 O1 58.81(5) 2 11 ? O1 K1 O1 103.51(3) 10 11 ? O1 K1 K1 65.08(2) 12 4 ? O1 K1 K1 114.92(2) 3 4 ? O1 K1 K1 114.92(2) . 4 ? O1 K1 K1 114.92(2) 2 4 ? O1 K1 K1 65.08(2) 10 4 ? O1 K1 K1 65.08(2) 11 4 ? O1 K1 K1 114.92(2) 12 4_554 ? O1 K1 K1 65.08(2) 3 4_554 ? O1 K1 K1 65.08(2) . 4_554 ? O1 K1 K1 65.08(2) 2 4_554 ? O1 K1 K1 114.92(2) 10 4_554 ? O1 K1 K1 114.92(2) 11 4_554 ? K1 K1 K1 180.0 4 4_554 ? C1 O1 Co1 121.90(13) . . ? C1 O1 K1 127.25(12) . . ? Co1 O1 K1 109.58(5) . . ? O1 C1 O1 126.2(3) 8 . ? O1 C1 H1 116.9 8 . ? O1 C1 H1 116.9 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.173 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.053 # Attachment '1-293K.cif' data_1-at-293K _database_code_depnum_ccdc_archive 'CCDC 784053' #TrackingRef '1-293K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H3 Co K O6' _chemical_formula_weight 233.08 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' K K 0.2009 0.2494 '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 'P 6(3)22' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' _cell_length_a 7.0124(14) _cell_length_b 7.0124(14) _cell_length_c 8.4270(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 358.87(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2919 _cell_measurement_theta_min 3.3561 _cell_measurement_theta_max 27.4835 _exptl_crystal_description 'hexagonal bipyramid' _exptl_crystal_colour pink _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 230 _exptl_absorpt_coefficient_mu 2.949 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8759 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_source_power '5.4 kW' _diffrn_source_voltage 50.0000 _diffrn_source_current 100.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_method CCD _diffrn_measurement_device_type 'Rigaku Mercury CCD (AFC7)' _diffrn_detector_area_resol_mean 15 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 6113 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0102 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 27.43 _reflns_number_total 283 _reflns_number_gt 254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; data collect, cell refinement and data reduction: "CrystalClear" software, Rigaku Corp., Japan, 2000. absorption correction: Jacobson, R. (1998). Private Communication. Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0348P)^2^+0.0137P] 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 SHELXL _refine_ls_extinction_coef 0.077(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_number_reflns 283 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0532 _refine_ls_goodness_of_fit_ref 1.194 _refine_ls_restrained_S_all 1.194 _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 0.6667 0.3333 0.2500 0.0177(2) Uani 1 6 d S . . K1 K 0.0000 0.0000 0.2500 0.0319(3) Uani 1 6 d S . . O1 O 0.4051(2) 0.1010(2) 0.10933(15) 0.0292(3) Uani 1 1 d . . . C1 C 0.4334(4) 0.0000 0.0000 0.0365(8) Uani 1 2 d S . . H1 H 0.5660 0.0000 0.0000 0.044 Uiso 1 2 calc SR . . 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 0.0207(3) 0.0207(3) 0.0118(3) 0.000 0.000 0.01035(13) K1 0.0291(4) 0.0291(4) 0.0377(6) 0.000 0.000 0.01453(19) O1 0.0286(7) 0.0322(7) 0.0240(6) -0.0106(7) -0.0025(5) 0.0131(6) C1 0.0293(11) 0.0451(19) 0.0402(16) -0.0241(14) -0.0121(7) 0.0226(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.1061(13) 11_655 ? Co1 O1 2.1061(13) 2_655 ? Co1 O1 2.1061(13) 10_665 ? Co1 O1 2.1061(13) . ? Co1 O1 2.1061(13) 12 ? Co1 O1 2.1061(13) 3_665 ? K1 O1 2.8220(13) 12 ? K1 O1 2.8220(13) 3 ? K1 O1 2.8220(13) . ? K1 O1 2.8220(13) 10 ? K1 O1 2.8220(13) 11 ? K1 O1 2.8220(13) 2 ? K1 K1 4.2135(9) 4 ? K1 K1 4.2135(9) 4_554 ? O1 C1 1.2372(18) . ? C1 O1 1.2372(18) 8 ? C1 H1 0.9300 . ? 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 82.07(7) 11_655 2_655 ? O1 Co1 O1 91.42(5) 11_655 10_665 ? O1 Co1 O1 95.89(7) 2_655 10_665 ? O1 Co1 O1 95.89(7) 11_655 . ? O1 Co1 O1 91.42(5) 2_655 . ? O1 Co1 O1 170.31(7) 10_665 . ? O1 Co1 O1 91.42(5) 11_655 12 ? O1 Co1 O1 170.31(7) 2_655 12 ? O1 Co1 O1 91.42(5) 10_665 12 ? O1 Co1 O1 82.07(7) . 12 ? O1 Co1 O1 170.31(7) 11_655 3_665 ? O1 Co1 O1 91.42(5) 2_655 3_665 ? O1 Co1 O1 82.07(7) 10_665 3_665 ? O1 Co1 O1 91.42(5) . 3_665 ? O1 Co1 O1 95.89(7) 12 3_665 ? O1 K1 O1 154.88(5) 12 3 ? O1 K1 O1 58.68(5) 12 . ? O1 K1 O1 103.61(3) 3 . ? O1 K1 O1 103.61(3) 12 10 ? O1 K1 O1 58.68(5) 3 10 ? O1 K1 O1 98.27(5) . 10 ? O1 K1 O1 103.61(3) 12 11 ? O1 K1 O1 98.27(5) 3 11 ? O1 K1 O1 154.88(5) . 11 ? O1 K1 O1 103.61(3) 10 11 ? O1 K1 O1 98.27(5) 12 2 ? O1 K1 O1 103.61(3) 3 2 ? O1 K1 O1 103.61(3) . 2 ? O1 K1 O1 154.88(5) 10 2 ? O1 K1 O1 58.68(5) 11 2 ? O1 K1 K1 65.16(3) 12 4 ? O1 K1 K1 114.84(3) 3 4 ? O1 K1 K1 114.84(3) . 4 ? O1 K1 K1 65.16(3) 10 4 ? O1 K1 K1 65.16(3) 11 4 ? O1 K1 K1 114.84(3) 2 4 ? O1 K1 K1 114.84(3) 12 4_554 ? O1 K1 K1 65.16(3) 3 4_554 ? O1 K1 K1 65.16(3) . 4_554 ? O1 K1 K1 114.84(3) 10 4_554 ? O1 K1 K1 114.84(3) 11 4_554 ? O1 K1 K1 65.16(3) 2 4_554 ? K1 K1 K1 180.0 4 4_554 ? C1 O1 Co1 122.35(14) . . ? C1 O1 K1 126.77(13) . . ? Co1 O1 K1 109.62(5) . . ? O1 C1 O1 126.9(3) 8 . ? O1 C1 H1 116.5 8 . ? O1 C1 H1 116.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.225 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.059 # Attachment '2-293K.cif' data_2-at-293K _database_code_depnum_ccdc_archive 'CCDC 784054' #TrackingRef '2-293K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H3 Co K O6' _chemical_formula_weight 233.08 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' K K 0.2009 0.2494 '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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.7489(6) _cell_length_b 8.9864(5) _cell_length_c 6.8879(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.466(3) _cell_angle_gamma 90.00 _cell_volume 662.30(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2714 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 3.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.783 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'NONIUS KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5596 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 27.45 _reflns_number_total 757 _reflns_number_gt 655 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0354P)^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 SHELXL _refine_ls_extinction_coef 0.0073(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 757 _refine_ls_number_parameters 54 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2500 0.2500 0.5000 0.01791(18) Uani 1 2 d S . . K1 K 0.5000 0.39660(7) 0.2500 0.0279(2) Uani 1 2 d S . . O1 O 0.25438(15) 0.45203(16) 0.3459(2) 0.0286(4) Uani 1 1 d . . . O2 O 0.16783(15) 0.66688(16) 0.2419(2) 0.0286(4) Uani 1 1 d . . . O3 O 0.43046(15) 0.68982(18) 0.1215(2) 0.0273(4) Uani 1 1 d . . . C1 C 0.1840(2) 0.5599(2) 0.3570(3) 0.0266(5) Uani 1 1 d . . . H1 H 0.1374 0.5614 0.4640 0.032 Uiso 1 1 calc R . . C2 C 0.5000 0.7519(3) 0.2500 0.0282(7) Uani 1 2 d S . . H2 H 0.5000 0.8554 0.2500 0.034 Uiso 1 2 calc SR . . 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 0.0165(3) 0.0175(2) 0.0193(2) 0.00135(14) -0.00023(15) -0.00048(15) K1 0.0286(4) 0.0228(3) 0.0338(4) 0.000 0.0109(3) 0.000 O1 0.0293(9) 0.0237(8) 0.0337(8) 0.0073(6) 0.0076(6) 0.0060(7) O2 0.0324(9) 0.0250(8) 0.0295(8) 0.0089(6) 0.0091(6) 0.0089(7) O3 0.0210(8) 0.0334(8) 0.0261(8) -0.0040(6) -0.0054(6) 0.0029(7) C1 0.0313(13) 0.0253(11) 0.0240(10) 0.0028(9) 0.0071(9) 0.0048(10) C2 0.0264(17) 0.0236(16) 0.0336(17) 0.000 -0.0030(14) 0.000 _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 2.0965(14) 4_545 ? Co1 O2 2.0965(14) 6_566 ? Co1 O1 2.1060(14) . ? Co1 O1 2.1060(14) 7_556 ? Co1 O3 2.1085(15) 4_545 ? Co1 O3 2.1086(15) 6_566 ? Co1 K1 3.5782(3) 7_556 ? Co1 K1 3.5782(3) . ? K1 O2 2.7456(15) 4_545 ? K1 O2 2.7456(15) 3_545 ? K1 O1 2.8260(16) . ? K1 O1 2.8260(16) 2_655 ? K1 O3 2.8412(15) 5_665 ? K1 O3 2.8412(15) 6_566 ? K1 O3 2.8565(17) 2_655 ? K1 O3 2.8565(17) . ? K1 C2 3.193(3) . ? K1 Co1 3.5782(3) 2_655 ? K1 K1 3.9134(7) 5_666 ? O1 C1 1.237(3) . ? O2 C1 1.247(2) . ? O2 Co1 2.0965(14) 4 ? O2 K1 2.7456(15) 3_455 ? O3 C2 1.236(2) . ? O3 Co1 2.1085(15) 4 ? O3 K1 2.8412(15) 5_665 ? C1 H1 0.9300 . ? C2 O3 1.236(2) 2_655 ? C2 H2 0.9300 . ? 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 O2 180.0 4_545 6_566 ? O2 Co1 O1 82.82(6) 4_545 . ? O2 Co1 O1 97.18(6) 6_566 . ? O2 Co1 O1 97.18(6) 4_545 7_556 ? O2 Co1 O1 82.82(6) 6_566 7_556 ? O1 Co1 O1 180.0 . 7_556 ? O2 Co1 O3 91.98(6) 4_545 4_545 ? O2 Co1 O3 88.02(6) 6_566 4_545 ? O1 Co1 O3 94.88(6) . 4_545 ? O1 Co1 O3 85.12(6) 7_556 4_545 ? O2 Co1 O3 88.02(6) 4_545 6_566 ? O2 Co1 O3 91.98(6) 6_566 6_566 ? O1 Co1 O3 85.12(6) . 6_566 ? O1 Co1 O3 94.88(6) 7_556 6_566 ? O3 Co1 O3 180.00(8) 4_545 6_566 ? O2 Co1 K1 130.08(4) 4_545 7_556 ? O2 Co1 K1 49.92(4) 6_566 7_556 ? O1 Co1 K1 127.87(4) . 7_556 ? O1 Co1 K1 52.13(4) 7_556 7_556 ? O3 Co1 K1 52.54(4) 4_545 7_556 ? O3 Co1 K1 127.46(4) 6_566 7_556 ? O2 Co1 K1 49.92(4) 4_545 . ? O2 Co1 K1 130.08(4) 6_566 . ? O1 Co1 K1 52.13(4) . . ? O1 Co1 K1 127.87(4) 7_556 . ? O3 Co1 K1 127.46(4) 4_545 . ? O3 Co1 K1 52.54(4) 6_566 . ? K1 Co1 K1 180.0 7_556 . ? O2 K1 O2 82.49(7) 4_545 3_545 ? O2 K1 O1 59.84(4) 4_545 . ? O2 K1 O1 140.13(5) 3_545 . ? O2 K1 O1 140.13(5) 4_545 2_655 ? O2 K1 O1 59.84(4) 3_545 2_655 ? O1 K1 O1 159.70(7) . 2_655 ? O2 K1 O3 92.43(5) 4_545 5_665 ? O2 K1 O3 63.03(4) 3_545 5_665 ? O1 K1 O3 126.18(4) . 5_665 ? O1 K1 O3 60.40(4) 2_655 5_665 ? O2 K1 O3 63.03(4) 4_545 6_566 ? O2 K1 O3 92.43(5) 3_545 6_566 ? O1 K1 O3 60.40(4) . 6_566 ? O1 K1 O3 126.18(4) 2_655 6_566 ? O3 K1 O3 148.28(7) 5_665 6_566 ? O2 K1 O3 147.18(4) 4_545 2_655 ? O2 K1 O3 123.15(5) 3_545 2_655 ? O1 K1 O3 89.29(5) . 2_655 ? O1 K1 O3 71.77(5) 2_655 2_655 ? O3 K1 O3 116.60(5) 5_665 2_655 ? O3 K1 O3 93.24(4) 6_566 2_655 ? O2 K1 O3 123.15(5) 4_545 . ? O2 K1 O3 147.18(4) 3_545 . ? O1 K1 O3 71.77(5) . . ? O1 K1 O3 89.29(5) 2_655 . ? O3 K1 O3 93.24(4) 5_665 . ? O3 K1 O3 116.60(5) 6_566 . ? O3 K1 O3 45.43(6) 2_655 . ? O2 K1 C2 138.75(3) 4_545 . ? O2 K1 C2 138.75(3) 3_545 . ? O1 K1 C2 79.85(3) . . ? O1 K1 C2 79.85(3) 2_655 . ? O3 K1 C2 105.86(3) 5_665 . ? O3 K1 C2 105.86(3) 6_566 . ? O3 K1 C2 22.71(3) 2_655 . ? O3 K1 C2 22.71(3) . . ? O2 K1 Co1 104.95(4) 4_545 2_655 ? O2 K1 Co1 35.75(3) 3_545 2_655 ? O1 K1 Co1 159.80(3) . 2_655 ? O1 K1 Co1 36.03(3) 2_655 2_655 ? O3 K1 Co1 36.09(3) 5_665 2_655 ? O3 K1 Co1 127.36(4) 6_566 2_655 ? O3 K1 Co1 107.60(3) 2_655 2_655 ? O3 K1 Co1 112.13(3) . 2_655 ? C2 K1 Co1 111.603(10) . 2_655 ? O2 K1 Co1 35.75(3) 4_545 . ? O2 K1 Co1 104.95(4) 3_545 . ? O1 K1 Co1 36.03(3) . . ? O1 K1 Co1 159.80(3) 2_655 . ? O3 K1 Co1 127.36(4) 5_665 . ? O3 K1 Co1 36.09(3) 6_566 . ? O3 K1 Co1 112.13(3) 2_655 . ? O3 K1 Co1 107.60(3) . . ? C2 K1 Co1 111.603(10) . . ? Co1 K1 Co1 136.79(2) 2_655 . ? O2 K1 K1 106.51(3) 4_545 5_666 ? O2 K1 K1 115.46(3) 3_545 5_666 ? O1 K1 K1 68.43(3) . 5_666 ? O1 K1 K1 101.55(3) 2_655 5_666 ? O3 K1 K1 160.80(4) 5_665 5_666 ? O3 K1 K1 46.78(3) 6_566 5_666 ? O3 K1 K1 46.46(3) 2_655 5_666 ? O3 K1 K1 79.21(4) . 5_666 ? C2 K1 K1 61.648(17) . 5_666 ? Co1 K1 K1 131.400(3) 2_655 5_666 ? Co1 K1 K1 71.843(5) . 5_666 ? C1 O1 Co1 126.97(13) . . ? C1 O1 K1 138.03(14) . . ? Co1 O1 K1 91.84(5) . . ? C1 O2 Co1 137.38(14) . 4 ? C1 O2 K1 128.21(13) . 3_455 ? Co1 O2 K1 94.33(5) 4 3_455 ? C2 O3 Co1 129.72(14) . 4 ? C2 O3 K1 125.13(10) . 5_665 ? Co1 O3 K1 91.36(5) 4 5_665 ? C2 O3 K1 94.13(14) . . ? Co1 O3 K1 124.28(7) 4 . ? K1 O3 K1 86.76(4) 5_665 . ? O1 C1 O2 127.86(19) . . ? O1 C1 H1 116.1 . . ? O2 C1 H1 116.1 . . ? O3 C2 O3 126.3(3) . 2_655 ? O3 C2 K1 63.16(14) . . ? O3 C2 K1 63.16(14) 2_655 . ? O3 C2 H2 116.8 . . ? O3 C2 H2 116.8 2_655 . ? K1 C2 H2 180.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.581 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.158