#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/60/2006033.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_2006033 loop_ _publ_author_name 'Parvez, M.' 'Boorman, P. M.' 'Wang, M.' _publ_contact_author ; Masood Parvez Department of Chemistry University of Calgary 2500 University Drive N.W. Calgary, Alberta, Canada T2N 1N4 ; _publ_section_title ; Tetraphenylphosphonium (Hydrogensulfido-S)trisulfidotungstate(VI) ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 413 _journal_page_last 414 _journal_paper_doi 10.1107/S0108270196015405 _journal_volume 53 _journal_year 1997 _chemical_formula_analytical 'C24 H20 P. W S4 H ' _chemical_formula_iupac '[(C6 H5)4 P] [W (H S) S3]' _chemical_formula_moiety 'C24 H21 P S4 W ' _chemical_formula_structural 'C24 H20 P. W S4 H ' _chemical_formula_sum 'C24 H21 P S4 W' _chemical_formula_weight 652.49 _space_group_IT_number 82 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I -4' _symmetry_space_group_name_H-M 'I -4' _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_formula_units_Z 2 _cell_length_a 12.995(1) _cell_length_b 12.995 _cell_length_c 7.143(1) _cell_measurement_reflns_used 25 _cell_measurement_temperature 170 _cell_measurement_theta_max 15.0 _cell_measurement_theta_min 10.0 _cell_volume 1206.24(19) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1994)' _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _computing_structure_solution 'SAPI91 (Fan, 1991)' _diffrn_ambient_temperature 170 _diffrn_measurement_device ' Rigaku AFC-6S' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type ' Mo K\a ' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 639 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 2.0 _diffrn_standards_decay_% 1.3 _diffrn_standards_interval_count 200 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.3 _exptl_absorpt_correction_T_max 0.45 _exptl_absorpt_correction_T_min 0.41 _exptl_absorpt_correction_type 'empirical \y scans (North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details ' psi-scan (3 reflections ) ' _exptl_crystal_colour dark-orange _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_meas ? _exptl_crystal_description needle _exptl_crystal_F_000 636.00 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.40 _refine_diff_density_min -0.45 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.40 _refine_ls_matrix_type full _refine_ls_number_parameters 68 _refine_ls_number_reflns 575 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.024 _refine_ls_shift/esd_max 0.003 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.013(Fo^2^)]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.023 _reflns_number_observed 575 _reflns_number_total 587 _reflns_observed_criterion ' [I > 3.0\s(I)] ' _cod_data_source_file bk1296.cif _cod_data_source_block Sulfido_Tungstate _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) + 0.013(Fo^2^)]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo) + 0.013(Fo^2^)]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1206.3(2) _cod_original_formula_sum 'C24 H21 P S4 W ' _cod_database_code 2006033 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 W1 0.0226(2) 0.0000 0.0000 0.0226 0.0000 0.0366(4) S1 0.054(1) -0.012(1) 0.036(2) 0.039(1) -0.015(1) 0.083(2) P1 0.015(1) 0.000 0.000 0.015 0.000 0.021(2) C1 0.014(3) -0.002(3) 0.004(3) 0.018(3) -0.005(3) 0.022(4) C2 0.028(3) -0.005(3) -0.005(5) 0.022(3) 0.009(4) 0.028(8) C3 0.030(4) 0.000(4) -0.006(4) 0.043(5) 0.008(4) 0.029(5) C4 0.026(4) 0.000(4) -0.011(4) 0.040(5) -0.008(4) 0.033(5) C5 0.027(3) -0.002(3) 0.009(9) 0.022(3) -0.006(7) 0.050(7) C6 0.026(4) 0.003(3) -0.007(4) 0.014(3) -0.002(3) 0.030(5) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type W1 0.0000 0.0000 1.0000 0.02728(9) Uij S1 0.1323(2) -0.0422(2) 0.8310(4) 0.0587(8) Uij P1 0.5000 0.0000 0.7500 0.0168(5) Uij C1 0.3990(5) -0.0448(5) 0.600(1) 0.018(2) Uij C2 0.3570(5) 0.0241(5) 0.472(2) 0.026(2) Uij C3 0.2774(6) -0.0058(6) 0.356(1) 0.034(2) Uij C4 0.2424(6) -0.1073(6) 0.361(1) 0.033(2) Uij C5 0.2858(5) -0.1769(5) 0.486(3) 0.033(2) Uij C6 0.3643(5) -0.1466(5) 0.606(1) 0.023(2) Uij H1 0.3831 0.0922 0.4647 0.0309 Uij H2 0.2467 0.0424 0.2730 0.0409 Uij H3 0.1889 -0.1289 0.2797 0.0397 Uij H4 0.2616 -0.2459 0.4899 0.0395 Uij H5 0.3941 -0.1943 0.6907 0.0281 Uij H6 0.1953 -0.0513 0.8398 0.0505 Uij loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.003 0.002 'International Tables' H 0.000 0.000 'International Tables' P 0.102 0.094 'International Tables' S 0.125 0.123 'International Tables' W -0.849 6.872 'International Tables' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 W1 S1 . 2 112.4(2) yes S1 W1 S1 . 4_557 108.00(10) yes S1 W1 S1 3_557 . 108.00(10) no S1 W1 S1 3_557 2 108.00(10) no S1 W1 S1 4_557 2 108.00(10) no S1 W1 S1 3_557 4_557 112.4(2) no C1 P1 C1 7_556 . 111.1(2) yes C1 P1 C1 8_546 . 111.1(2) no C1 P1 C1 2_655 . 106.3(4) yes C1 P1 C1 8_546 7_556 106.3(4) no C1 P1 C1 8_546 2_655 111.1(2) no C1 P1 C1 7_556 2_655 111.1(2) no P1 C1 C2 . . 118.2(5) yes P1 C1 C6 . . 121.6(5) yes C2 C1 C6 . . 120.2(6) no C1 C2 C3 . . 120.5(6) no C2 C3 C4 . . 119.5(7) no C3 C4 C5 . . 120.0(8) no C4 C5 C6 . . 120.5(6) no C1 C6 C5 . . 119.1(7) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag W1 S1 . 2.171(2) yes W1 S1 3_557 2.171(2) no W1 S1 4_557 2.171(2) no W1 S1 2 2.171(2) no P1 C1 . 1.793(6) yes P1 C1 8_546 1.793(6) no P1 C1 7_556 1.793(6) no P1 C1 2_655 1.793(6) no C1 C2 . 1.39(1) no C1 C6 . 1.40(1) no C2 C3 . 1.38(1) no C3 C4 . 1.40(1) no C4 C5 . 1.39(2) no C5 C6 . 1.39(2) no