Bis(tetraphenylphosphonium) tetrasulfidotungstate(VI)
Leyva Bailen, Patricia; Powell, Anthony V.; Vaqueiro, Paz; Acta Crystallographica Section E 64 (2008) m574–; doi:10.1107/S1600536808007472

data_2217893
_publ_section_title
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 Bis(tetraphenylphosphonium) tetrasulfidotungstate(VI)
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_journal_coeditor_code           CS2070
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m574
_journal_paper_doi               10.1107/S1600536808007472
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '(C24 H20 P)2 [W S4]'
_chemical_formula_moiety         '2(C24 H20 P +), S4 W 2-'
_chemical_formula_sum            'C48 H40 P2 S4 W'
_chemical_formula_weight         990.86
_chemical_name_systematic
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Bis(tetraphenylphosphonium) tetrasulfidotungstate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 91.242(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1069(4)
_cell_length_b                   19.4557(6)
_cell_length_c                   20.2373(6)
_cell_measurement_reflns_used    6646
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.5077
_cell_measurement_theta_min      2.0131
_cell_volume                     4372.1(2)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'ATOMS (Dowty, 2000)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Bruker--Nonius APEXII CCD area-detector diffractometer
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26702
_diffrn_reflns_theta_full        30.508
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.013
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.939
_exptl_absorpt_correction_T_max  0.4141
_exptl_absorpt_correction_T_min  0.3514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.47
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4008
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.002621
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial,
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 2.09 -0.539 1.80
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0377
_refine_ls_wR_factor_gt          0.0312
_refine_ls_wR_factor_ref         0.0312
_reflns_number_gt                4008
_reflns_number_total             6646
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            cs2070.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2217893
_cod_database_fobs_code          2217893