#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/25/2202544.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2202544 loop_ _publ_author_name ' Tetsuzo Ito ' _publ_section_title ; Tris(O-methyl dithiocarbonato)cobalt(III) ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m892 _journal_page_last m893 _journal_paper_doi 10.1107/S1600536803019937 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Co (C2 H3 O S2 )3 ] ' _chemical_formula_moiety 'C6 H9 Co O3 S6 ' _chemical_formula_sum 'C6 H9 Co O3 S6' _chemical_formula_weight 380.48 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90 _cell_angle_beta 106.235(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.5520(10) _cell_length_b 13.4610(10) _cell_length_c 11.3570(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296.1 _cell_measurement_theta_max 16.5 _cell_measurement_theta_min 16.2 _cell_volume 1402.0(2) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction ; CrystalStructure (Molecular Structure Corporation and Rigaku Corporation, 2002) ; _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996)' _computing_publication_material CrystalStructure _computing_structure_refinement CrystalStructure _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_measured_fraction_theta_full 0.9982 _diffrn_measured_fraction_theta_max 0.9982 _diffrn_measurement_device_type 'Rigaku AFC-5S' _diffrn_measurement_method \w-2\q _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 3550 _diffrn_reflns_theta_full 27.51 _diffrn_reflns_theta_max 27.51 _diffrn_standards_decay_% 0.55 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.104 _exptl_absorpt_correction_T_max 0.591 _exptl_absorpt_correction_T_min 0.379 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 768.00 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.41 _refine_diff_density_min -0.58 _refine_ls_extinction_coef 125.9(9) _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_goodness_of_fit_ref 1.660 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 146 _refine_ls_number_reflns 2629 _refine_ls_R_factor_gt 0.0290 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/\s^2^(Fo)' _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_ref 0.0360 _reflns_number_gt 2629 _reflns_number_total 3224 _reflns_threshold_expression I>3\s(I) _cod_data_source_file cm6056.cif _cod_data_source_block I _cod_original_cell_volume 1402.1(2) _cod_original_sg_symbol_H-M 'P 21/n' _cod_original_formula_sum 'C6 H9 Co O3 S6 ' _cod_database_code 2202544 _cod_database_fobs_code 2202544 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Co 0.67478(3) 0.49026(2) 0.26579(3) 0.03645(9) Uani d . 1.00 . . Co S1 0.89373(7) 0.56955(5) 0.31278(6) 0.0462(2) Uani d . 1.00 . . S S2 0.79324(7) 0.41501(5) 0.14264(6) 0.0487(2) Uani d . 1.00 . . S S3 0.74817(7) 0.38056(6) 0.42185(6) 0.0505(2) Uani d . 1.00 . . S S4 0.48902(7) 0.37859(6) 0.22818(7) 0.0506(2) Uani d . 1.00 . . S S5 0.57298(7) 0.59847(6) 0.37182(6) 0.0471(2) Uani d . 1.00 . . S S6 0.55566(7) 0.59945(5) 0.12015(6) 0.0451(2) Uani d . 1.00 . . S O1 1.0531(2) 0.48880(10) 0.1760(2) 0.0579(6) Uani d . 1.00 . . O O2 0.5380(2) 0.24410(10) 0.3997(2) 0.0597(6) Uani d . 1.00 . . O O3 0.4248(2) 0.73500(10) 0.2272(2) 0.0555(6) Uani d . 1.00 . . O C1 0.9309(3) 0.4929(2) 0.2085(2) 0.0442(7) Uani d . 1.00 . . C C2 0.5885(3) 0.3232(2) 0.3582(2) 0.0458(7) Uani d . 1.00 . . C C3 0.5076(3) 0.6557(2) 0.2354(2) 0.0423(7) Uani d . 1.00 . . C C4 1.1718(3) 0.5542(3) 0.2356(3) 0.0730(10) Uani d . 1.00 . . C C5 0.6331(4) 0.1964(3) 0.5081(3) 0.0760(10) Uani d . 1.00 . . C C6 0.3685(3) 0.7821(2) 0.1089(3) 0.0680(10) Uani d . 1.00 . . C H1 1.2002 0.5407 0.3211 0.090 Uiso c . 1.00 . . H H2 1.2525 0.5440 0.2036 0.090 Uiso c . 1.00 . . H H3 1.1400 0.6212 0.2222 0.090 Uiso c . 1.00 . . H H4 0.5866 0.1397 0.5300 0.098 Uiso c . 1.00 . . H H5 0.7210 0.1767 0.4912 0.098 Uiso c . 1.00 . . H H6 0.6547 0.2426 0.5740 0.098 Uiso c . 1.00 . . H H7 0.3106 0.8380 0.1159 0.077 Uiso c . 1.00 . . H H8 0.4479 0.8031 0.0799 0.077 Uiso c . 1.00 . . H H9 0.3107 0.7358 0.0529 0.077 Uiso c . 1.00 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co 0.0272(2) 0.0454(2) 0.0364(2) -0.00270(10) 0.00830(10) -0.00440(10) S1 0.0338(3) 0.0553(4) 0.0508(4) -0.0086(3) 0.0139(3) -0.0163(3) S2 0.0373(3) 0.0557(4) 0.0534(4) -0.0049(3) 0.0132(3) -0.0197(3) S3 0.0382(3) 0.0637(5) 0.0463(4) 0.0018(3) 0.0063(3) 0.0058(3) S4 0.0336(3) 0.0578(4) 0.0557(4) -0.0088(3) 0.0047(3) 0.0004(3) S5 0.0403(3) 0.0631(4) 0.0390(3) 0.0037(3) 0.0131(3) -0.0069(3) S6 0.0434(3) 0.0545(4) 0.0382(3) 0.0020(3) 0.0127(3) -0.0008(3) O1 0.0362(9) 0.0710(10) 0.0730(10) -0.0049(9) 0.0259(9) -0.0200(10) O2 0.0660(10) 0.0550(10) 0.0670(10) -0.0070(10) 0.0320(10) 0.0070(10) O3 0.0470(10) 0.0560(10) 0.0600(10) 0.0110(10) 0.0080(10) -0.0080(10) C1 0.0320(10) 0.0510(10) 0.0500(10) -0.0010(10) 0.0120(10) -0.0060(10) C2 0.0410(10) 0.049(2) 0.051(2) 0.0000(10) 0.0200(10) -0.0010(10) C3 0.0310(10) 0.0480(10) 0.0470(10) -0.0030(10) 0.0090(10) -0.0080(10) C4 0.0340(10) 0.086(2) 0.104(3) -0.011(2) 0.028(2) -0.017(2) C5 0.114(3) 0.065(2) 0.065(2) 0.012(2) 0.051(2) 0.016(2) C6 0.065(2) 0.057(2) 0.070(2) 0.008(2) -0.002(2) -0.001(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; C C 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag S1 Co S2 76.69(3) yes S1 Co S3 93.40(3) yes S1 Co S4 166.57(3) yes S1 Co S5 94.38(3) yes S1 Co S6 96.20(3) yes S2 Co S3 95.33(3) yes S2 Co S4 94.97(3) yes S2 Co S5 166.68(3) yes S2 Co S6 94.29(3) yes S3 Co S4 76.71(3) yes S3 Co S5 95.05(3) yes S3 Co S6 167.74(3) yes S4 Co S5 95.52(3) yes S4 Co S6 94.90(3) yes S5 Co S6 76.66(3) yes Co S1 C1 84.70(10) no Co S2 C1 84.90(10) no Co S3 C2 85.30(10) no Co S4 C2 84.80(10) no Co S5 C3 84.80(10) no Co S6 C3 85.10(10) no C1 O1 C4 118.8(2) no C2 O2 C5 117.2(2) no C3 O3 C6 118.8(2) no S1 C1 S2 113.7(2) no S1 C1 O1 126.9(2) no S2 C1 O1 119.4(2) no S3 C2 S4 113.2(2) no S3 C2 O2 126.8(2) no S4 C2 O2 120.0(2) no S5 C3 S6 113.4(2) no S5 C3 O3 119.7(2) no S6 C3 O3 126.8(2) no O1 C4 H1 108.9 no O1 C4 H2 110.2 no H1 C4 H2 109.5 no O1 C4 H3 109.3 no H1 C4 H3 109.5 no H2 C4 H3 109.5 no O2 C5 H4 110.3 no O2 C5 H5 109.2 no H4 C5 H5 109.5 no O2 C5 H6 108.8 no H4 C5 H6 109.5 no H5 C5 H6 109.5 no O3 C6 H7 110.1 no O3 C6 H8 109.1 no H7 C6 H8 109.5 no O3 C6 H9 109.2 no H7 C6 H9 109.5 no H8 C6 H9 109.5 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co S1 . . 2.2746(7) yes Co S2 . . 2.2688(7) yes Co S3 . . 2.2623(8) yes Co S4 . . 2.2731(7) yes Co S5 . . 2.2742(7) yes Co S6 . . 2.2668(7) yes S1 C1 . . 1.682(3) yes S2 C1 . . 1.684(3) yes S3 C2 . . 1.682(3) yes S4 C2 . . 1.690(3) yes S5 C3 . . 1.686(3) yes S6 C3 . . 1.683(3) yes O1 C1 . . 1.321(3) yes O1 C4 . . 1.446(3) yes O2 C2 . . 1.310(3) yes O2 C5 . . 1.459(4) yes O3 C3 . . 1.317(3) yes O3 C6 . . 1.446(3) yes C4 H1 . . 0.950 no C4 H2 . . 0.950 no C4 H3 . . 0.950 no C5 H4 . . 0.950 no C5 H5 . . 0.950 no C5 H6 . . 0.950 no C6 H7 . . 0.950 no C6 H8 . . 0.950 no C6 H9 . . 0.950 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag S1 O2 3.557(2) 3_655 no O1 O2 3.591(3) 3_655 no O1 O3 3.577(3) 3_645 no O1 C5 3.353(4) 4_554 no O2 C4 3.345(4) 3_645 no O3 C4 3.449(4) 1_455 no O3 C5 3.335(4) 2_666 no C3 C4 3.487(4) 1_455 no