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_4319806
_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_formula_sum            'C28 H29 P S4 W'
_chemical_formula_weight         708.57
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.9410(10)
_cell_angle_beta                 84.8770(10)
_cell_angle_gamma                60.8260(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0377(6)
_cell_length_b                   11.1307(5)
_cell_length_c                   13.6286(7)
_cell_measurement_reflns_used    5881
_cell_measurement_temperature    193(2)
_cell_volume                     1450.05(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9588
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    4.342
_exptl_absorpt_correction_T_max  0.4904
_exptl_absorpt_correction_T_min  0.2644
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.141
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                4932
_reflns_number_total             5504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000970n_1.cif
_cod_data_source_block           (PPh4)WS3(SiBu)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319806