#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/4/4060179.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_4060179 _journal_name_full 'Organometallics' _journal_year 2005 _chemical_formula_sum 'C38 H32 Co4 Fe O14 S2' _chemical_formula_weight 1068.33 _symmetry_cell_setting monoclinic _space_group_IT_number 13 _symmetry_space_group_name_Hall '-P 2yc' _symmetry_space_group_name_H-M 'P 1 2/c 1' _[local]_cod_cif_authors_sg_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 14.4980(5) _cell_length_b 10.8391(3) _cell_length_c 14.0975(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.5140(10) _cell_angle_gamma 90.00 _cell_volume 2100.70(11) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 2.048 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5343 _exptl_absorpt_correction_T_max 0.7912 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12057 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4785 _reflns_number_gt 4147 _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^)+(0.0520P)^2^+3.5275P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4785 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 -0.29661(3) -0.10495(4) -0.45006(3) 0.03087(13) Uani 1 1 d . . . Co2 Co -0.36877(3) -0.26839(4) -0.37374(3) 0.02699(12) Uani 1 1 d . . . Fe1 Fe 0.0000 -0.26772(5) -0.2500 0.02334(14) Uani 1 2 d S . . S1 S -0.06750(8) -0.66613(11) -0.36663(9) 0.0610(3) Uani 1 1 d . . . C8 C -0.0990(2) -0.1639(3) -0.2057(2) 0.0312(6) Uani 1 1 d . . . H8A H -0.1097 -0.0776 -0.2143 0.037 Uiso 1 1 calc R . . C7 C -0.0316(2) -0.2222(3) -0.1222(2) 0.0360(7) Uani 1 1 d . . . H7A H 0.0105 -0.1814 -0.0652 0.043 Uiso 1 1 calc R . . C6 C -0.0376(2) -0.3520(3) -0.1379(2) 0.0328(7) Uani 1 1 d . . . H6A H -0.0005 -0.4127 -0.0934 0.039 Uiso 1 1 calc R . . C5 C -0.1093(2) -0.3746(3) -0.2326(2) 0.0275(6) Uani 1 1 d . . . H5A H -0.1282 -0.4531 -0.2625 0.033 Uiso 1 1 calc R . . C4 C -0.14785(19) -0.2574(3) -0.2745(2) 0.0243(5) Uani 1 1 d . . . C3 C -0.2295(2) -0.2413(3) -0.3646(2) 0.0244(5) Uani 1 1 d . . . C2 C -0.2811(2) -0.2844(3) -0.4549(2) 0.0258(6) Uani 1 1 d . . . C1 C -0.2755(2) -0.3802(3) -0.5300(2) 0.0305(6) Uani 1 1 d . . . C13 C -0.2087(3) -0.3359(4) -0.5884(3) 0.0424(8) Uani 1 1 d . . . H13C H -0.1439 -0.3183 -0.5416 0.064 Uiso 1 1 calc R . . H13B H -0.2358 -0.2608 -0.6256 0.064 Uiso 1 1 calc R . . H13A H -0.2038 -0.4003 -0.6353 0.064 Uiso 1 1 calc R . . C12 C -0.3777(3) -0.4101(4) -0.6012(3) 0.0462(9) Uani 1 1 d . . . H12C H -0.4172 -0.4452 -0.5629 0.069 Uiso 1 1 calc R . . H12B H -0.3726 -0.4698 -0.6515 0.069 Uiso 1 1 calc R . . H12A H -0.4084 -0.3343 -0.6346 0.069 Uiso 1 1 calc R . . C11 C -0.2265(3) -0.5966(4) -0.5185(3) 0.0507(9) Uani 1 1 d . . . H11B H -0.1814 -0.5860 -0.5579 0.061 Uiso 1 1 calc R . . H11A H -0.2913 -0.6191 -0.5650 0.061 Uiso 1 1 calc R . . C10 C -0.1907(3) -0.6951(4) -0.4438(4) 0.0578(11) Uani 1 1 d . . . H10B H -0.1938 -0.7752 -0.4784 0.069 Uiso 1 1 calc R . . H10A H -0.2331 -0.7005 -0.4010 0.069 Uiso 1 1 calc R . . C9 C -0.0491(4) -0.8031(4) -0.2859(5) 0.0821(18) Uani 1 1 d . . . H9A H -0.0974 -0.8034 -0.2495 0.099 Uiso 1 1 calc R . . H9B H -0.0590 -0.8786 -0.3275 0.099 Uiso 1 1 calc R . . O201 O -0.57102(18) -0.2409(3) -0.5065(2) 0.0587(8) Uani 1 1 d . . . C201 C -0.4937(2) -0.2526(3) -0.4553(3) 0.0385(7) Uani 1 1 d . . . O202 O -0.3677(2) -0.5334(3) -0.3340(2) 0.0546(7) Uani 1 1 d . . . C202 C -0.3682(2) -0.4308(3) -0.3479(2) 0.0345(7) Uani 1 1 d . . . O203 O -0.3527(3) -0.1601(3) -0.1774(2) 0.0665(9) Uani 1 1 d . . . C203 C -0.3624(2) -0.2001(3) -0.2537(3) 0.0381(7) Uani 1 1 d . . . O103 O -0.4676(2) -0.0556(3) -0.6265(2) 0.0715(10) Uani 1 1 d . . . C103 C -0.4022(3) -0.0722(4) -0.5585(3) 0.0452(8) Uani 1 1 d . . . O102 O -0.1434(2) -0.0145(3) -0.5259(3) 0.0643(8) Uani 1 1 d . . . C102 C -0.2023(3) -0.0486(3) -0.4959(3) 0.0428(8) Uani 1 1 d . . . O101 O -0.2955(2) 0.0830(3) -0.2985(2) 0.0615(8) Uani 1 1 d . . . C101 C -0.2968(3) 0.0134(3) -0.3584(3) 0.0424(8) Uani 1 1 d . . . O1 O -0.23314(17) -0.4844(2) -0.46837(16) 0.0347(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0249(2) 0.0289(2) 0.0353(2) 0.00506(17) 0.00458(17) 0.00162(15) Co2 0.0184(2) 0.0337(2) 0.0284(2) -0.00090(16) 0.00671(15) 0.00045(14) Fe1 0.0166(3) 0.0299(3) 0.0226(3) 0.000 0.0049(2) 0.000 S1 0.0531(6) 0.0511(6) 0.0675(7) 0.0016(5) 0.0031(5) -0.0014(5) C8 0.0240(14) 0.0345(16) 0.0336(15) -0.0087(13) 0.0071(12) 0.0017(12) C7 0.0237(14) 0.058(2) 0.0250(14) -0.0079(14) 0.0062(12) 0.0006(13) C6 0.0256(14) 0.0494(19) 0.0245(14) 0.0107(13) 0.0094(11) 0.0055(13) C5 0.0211(13) 0.0329(15) 0.0302(14) 0.0028(12) 0.0107(11) 0.0001(11) C4 0.0177(12) 0.0310(14) 0.0236(13) -0.0010(11) 0.0057(11) 0.0014(10) C3 0.0186(12) 0.0259(13) 0.0293(14) 0.0010(11) 0.0083(11) 0.0004(10) C2 0.0180(12) 0.0307(14) 0.0294(14) 0.0026(11) 0.0085(11) -0.0005(10) C1 0.0266(14) 0.0384(16) 0.0255(14) -0.0053(12) 0.0070(11) -0.0022(12) C13 0.047(2) 0.051(2) 0.0357(17) -0.0020(16) 0.0225(15) -0.0052(16) C12 0.0344(18) 0.063(2) 0.0354(17) -0.0154(17) 0.0029(14) -0.0060(16) C11 0.053(2) 0.044(2) 0.053(2) -0.0180(17) 0.0129(18) 0.0046(17) C10 0.051(2) 0.036(2) 0.077(3) -0.012(2) 0.007(2) 0.0019(17) C9 0.080(4) 0.042(2) 0.096(4) 0.004(3) -0.014(3) -0.003(2) O201 0.0224(12) 0.081(2) 0.0616(18) 0.0067(15) -0.0026(12) 0.0033(12) C201 0.0279(16) 0.0447(19) 0.0433(19) 0.0004(15) 0.0118(14) -0.0007(13) O202 0.0722(19) 0.0416(16) 0.0566(16) 0.0060(13) 0.0296(15) -0.0048(13) C202 0.0301(15) 0.0413(19) 0.0337(16) -0.0005(14) 0.0123(13) -0.0034(13) O203 0.091(2) 0.068(2) 0.0467(16) -0.0126(15) 0.0314(16) 0.0071(18) C203 0.0348(17) 0.0437(18) 0.0394(18) -0.0010(15) 0.0169(14) 0.0048(14) O103 0.0446(16) 0.085(2) 0.0653(19) 0.0310(18) -0.0100(14) -0.0012(16) C103 0.0377(18) 0.0434(19) 0.050(2) 0.0134(17) 0.0077(16) 0.0008(15) O102 0.0551(18) 0.0551(17) 0.091(2) 0.0257(17) 0.0351(17) -0.0045(14) C102 0.0390(18) 0.0343(17) 0.051(2) 0.0123(16) 0.0083(16) 0.0008(14) O101 0.0621(19) 0.0471(16) 0.070(2) -0.0163(15) 0.0140(16) 0.0023(14) C101 0.0345(17) 0.0347(17) 0.052(2) 0.0020(16) 0.0048(15) 0.0039(14) O1 0.0424(13) 0.0310(11) 0.0321(11) -0.0058(9) 0.0137(10) 0.0005(9) _cod_database_code 4060179