Syntheses, Structures, and Stabilities of [PPh4][WS3(SR)] (R = iBu, iPr, tBu, Benzyl, Allyl) and [PPh4][MoS3(StBu)]
Naomi L. Kruhlak; Meiping Wang; P. Michael Boorman; Masood Parvez; Robert McDonald; Inorganic Chemistry 40 (2001) 3141–3148; doi:10.1021/ic000970n

data_4319808
_publ_section_title
;
 Syntheses, Structures, and Stabilities of [PPh4][WS3(SR)] (R = iBu, iPr,
 tBu, Benzyl, Allyl) and [PPh4][MoS3(StBu)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3141
_journal_page_last               3148
_journal_paper_doi               10.1021/ic000970n
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'synthesized by authors'
_chemical_formula_analytical     'C28 H29 P S4 W '
_chemical_formula_sum            'C28 H29 P S4 W'
_chemical_formula_weight         708.57
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2000-04-26
_audit_creation_method           'by teXsan v1.7'
_cell_angle_alpha                90
_cell_angle_beta                 101.67(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.667(2)
_cell_length_b                   17.578(2)
_cell_length_c                   16.117(3)
_cell_measurement_reflns_used    17
_cell_measurement_temperature    296
_cell_measurement_theta_max      21.1
_cell_measurement_theta_min      19.6
_cell_volume                     2959.5(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution    'DIRDIF92 PATTY (Beurskens, 1992)'
_diffrn_ambient_temperature      296
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.094
_diffrn_reflns_av_sigmaI/netI    0.100
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5747
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.33
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.67
_refine_diff_density_min         -1.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.72
_refine_ls_goodness_of_fit_obs   1.72
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     307
_refine_ls_number_reflns         2438
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_obs          0.044
_refine_ls_shift/esd_max         0.04
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00008|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.042
_refine_ls_wR_factor_obs         0.042
_reflns_number_observed          2438
_reflns_number_total             5443
_reflns_observed_criterion       'I > 3.00\s(I)'
_cod_data_source_file            ic000970n_3.cif
_cod_data_source_block           (PPh4)WS3(StBu)
_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) +
0.00008|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) + 0.00008|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2959.4(7)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C28 H29 P S4 W '
_cod_database_code               4319808