#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000107.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000107 _journal_name_full 'Chemistry of Materials' _journal_year 2001 _chemical_formula_sum 'C27 H21 Co3 K O23' _chemical_formula_weight 929.33 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 9.60960(10) _cell_length_b 12.56100(10) _cell_length_c 13.9736(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.2390(10) _cell_angle_gamma 90.00 _cell_volume 1592.50(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _exptl_crystal_description parallelepi _exptl_crystal_colour pink _exptl_crystal_size_max 0.00 _exptl_crystal_size_mid 0.00 _exptl_crystal_size_min 0.00 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 934 _exptl_absorpt_coefficient_mu 1.777 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_reflns_number 10777 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 29.53 _reflns_number_total 4094 _reflns_number_gt 3528 _reflns_threshold_expression >2sigma(I) _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^)+(0.0574P)^2^+0.1179P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0044(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4094 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.06016(3) 0.778027(19) 0.153419(17) 0.01533(9) Uani 1 1 d . . . Co2 Co 0.0000 1.0000 0.0000 0.01307(10) Uani 1 2 d S . . O1 O 0.05327(17) 0.62228(10) 0.18931(11) 0.0234(3) Uani 1 1 d . . . O2 O -0.00566(16) 0.72327(11) 0.00544(9) 0.0225(3) Uani 1 1 d . . . O3 O 0.0151(2) 1.12876(11) 0.08632(11) 0.0334(4) Uani 1 1 d . . . O4 O -0.3703(2) 1.27474(14) 0.1225(2) 0.0544(6) Uani 1 1 d . . . H4 H -0.3778 1.3385 0.1325 0.082 Uiso 1 1 calc R . . O5 O 0.4009(2) 1.27042(14) 0.12692(18) 0.0491(5) Uani 1 1 d . . . O6 O 0.16175(13) 0.91891(11) 0.12553(10) 0.0195(3) Uani 1 1 d . . . O7 O 0.29348(16) 0.77332(11) 0.15121(12) 0.0257(3) Uani 1 1 d . . . O8 O -0.13826(15) 0.81546(12) 0.17941(10) 0.0238(3) Uani 1 1 d . . . O9 O -0.14453(16) 0.93898(15) 0.06564(12) 0.0342(4) Uani 1 1 d . . . C1 C 0.0000 0.45712(19) 0.2500 0.0162(5) Uani 1 2 d S . . C2 C 0.0095(2) 0.40183(14) 0.16556(13) 0.0175(3) Uani 1 1 d . . . H2 H 0.0168 0.4389 0.1098 0.021 Uiso 1 1 calc R . . C3 C -0.0080(2) 0.70892(14) -0.16521(13) 0.0166(3) Uani 1 1 d . . . C4 C 0.0000 0.7632(2) -0.2500 0.0180(5) Uani 1 2 d S . . H4A H 0.0000 0.8373 -0.2500 0.022 Uiso 1 2 calc SR . . C5 C 0.0000 0.5765(2) 0.2500 0.0163(5) Uani 1 2 d S . . C6 C -0.0111(2) 0.77224(14) -0.07453(13) 0.0177(3) Uani 1 1 d . . . C7 C 0.5251(2) 1.10672(16) 0.12838(14) 0.0211(4) Uani 1 1 d . . . C8 C 0.40338(19) 1.04598(16) 0.12884(13) 0.0191(4) Uani 1 1 d . . . H8 H 0.3166 1.0794 0.1278 0.023 Uiso 1 1 calc R . . C9 C 0.41234(18) 0.93537(15) 0.13089(13) 0.0172(3) Uani 1 1 d . . . C10 C 0.54373(19) 0.88459(15) 0.13419(13) 0.0177(3) Uani 1 1 d . . . H10 H 0.5504 0.8107 0.1374 0.021 Uiso 1 1 calc R . . C11 C -0.33585(18) 0.94534(15) 0.13266(13) 0.0176(3) Uani 1 1 d . . . C12 C -0.3462(2) 1.05654(17) 0.12869(14) 0.0219(4) Uani 1 1 d . . . H12 H -0.2663 1.0970 0.1263 0.026 Uiso 1 1 calc R . . C13 C 0.5115(2) 1.22492(16) 0.12569(18) 0.0296(5) Uani 1 1 d . . . C14 C 0.28355(19) 0.87159(15) 0.13465(13) 0.0179(3) Uani 1 1 d . . . C15 C -0.19677(19) 0.89658(16) 0.12638(13) 0.0184(3) Uani 1 1 d . . . K1 K 0.3234(2) 0.5588(2) 0.1608(2) 0.0510(5) Uani 0.50 1 d P . 1 OW1 O 0.3778(7) 0.5681(6) 0.1573(7) 0.0626(19) Uani 0.50 1 d P A 2 OW2 O 0.2414(2) 0.42401(16) -0.00362(16) 0.0479(5) Uani 1 1 d . . . OW3 O 0.3817(3) 0.49040(17) 0.3638(2) 0.0619(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01967(14) 0.01299(13) 0.01701(13) -0.00008(8) 0.01102(10) -0.00163(9) Co2 0.01651(16) 0.01074(16) 0.01472(17) -0.00077(11) 0.00888(13) -0.00033(12) O1 0.0397(8) 0.0130(6) 0.0256(7) 0.0020(5) 0.0216(6) -0.0004(6) O2 0.0370(8) 0.0177(7) 0.0152(6) -0.0011(5) 0.0120(6) -0.0029(5) O3 0.0695(11) 0.0139(6) 0.0213(7) -0.0020(5) 0.0210(7) 0.0030(7) O4 0.0403(10) 0.0251(9) 0.1052(18) 0.0071(10) 0.0340(11) -0.0053(8) O5 0.0365(10) 0.0274(9) 0.0867(15) 0.0111(9) 0.0248(10) 0.0081(7) O6 0.0130(5) 0.0232(7) 0.0236(6) 0.0037(5) 0.0077(5) -0.0007(5) O7 0.0218(7) 0.0208(7) 0.0372(8) 0.0052(6) 0.0135(6) -0.0005(5) O8 0.0223(6) 0.0285(7) 0.0218(6) 0.0017(6) 0.0088(5) 0.0092(6) O9 0.0251(7) 0.0495(10) 0.0358(8) 0.0067(7) 0.0206(6) -0.0038(7) C1 0.0223(11) 0.0113(11) 0.0171(11) 0.000 0.0095(9) 0.000 C2 0.0264(9) 0.0132(8) 0.0149(7) 0.0014(6) 0.0094(7) -0.0001(7) C3 0.0241(8) 0.0132(8) 0.0143(7) -0.0018(6) 0.0088(6) 0.0006(7) C4 0.0254(12) 0.0119(11) 0.0184(11) 0.000 0.0097(10) 0.000 C5 0.0223(11) 0.0122(11) 0.0153(10) 0.000 0.0072(9) 0.000 C6 0.0250(9) 0.0149(8) 0.0155(8) -0.0031(6) 0.0098(7) -0.0011(7) C7 0.0198(8) 0.0206(9) 0.0226(8) 0.0047(7) 0.0067(7) -0.0004(7) C8 0.0145(8) 0.0234(9) 0.0194(8) 0.0032(7) 0.0053(6) 0.0019(7) C9 0.0141(7) 0.0225(9) 0.0157(7) 0.0025(7) 0.0059(6) -0.0012(7) C10 0.0169(8) 0.0196(9) 0.0173(8) 0.0035(7) 0.0064(6) 0.0010(7) C11 0.0140(7) 0.0231(9) 0.0167(8) 0.0045(7) 0.0062(6) 0.0017(7) C12 0.0173(8) 0.0253(10) 0.0237(9) 0.0050(8) 0.0077(7) -0.0034(7) C13 0.0258(10) 0.0226(10) 0.0388(11) 0.0070(9) 0.0085(9) 0.0000(8) C14 0.0163(8) 0.0231(9) 0.0150(8) 0.0022(7) 0.0061(6) -0.0015(7) C15 0.0135(7) 0.0251(9) 0.0169(8) -0.0023(7) 0.0054(6) -0.0019(7) K1 0.0517(11) 0.0381(7) 0.0740(10) -0.0065(7) 0.0355(10) 0.0028(9) OW1 0.050(4) 0.042(3) 0.092(4) -0.001(3) 0.018(4) 0.018(3) OW2 0.0396(9) 0.0352(9) 0.0650(12) 0.0060(9) 0.0118(9) -0.0031(8) OW3 0.0617(14) 0.0394(11) 0.0784(16) -0.0056(11) 0.0150(12) 0.0127(10)