Tetraphenylphosphonium (Hydrogensulfido-<i>S</i>)trisulfidotungstate(VI)
Parvez, M.; Boorman, P. M.; Wang, M.; Acta Crystallographica Section C 53 (1997) 413–414; doi:10.1107/S0108270196015405

data_2006033
_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-<i>S</i>)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