Structural chemistry of (PPh4)2M(WS4)2 materials
Crossland, Clare J.; Evans, Ivana Radosavljević; Evans, John S. O.; Dalton Transactions  (2008) 1597–1601; doi:10.1039/b716407f

data_7003476
_publ_section_title
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 Structural chemistry of (PPh4)2M(WS4)2 materials
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_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              1597
_journal_page_last               1601
_journal_paper_doi               10.1039/b716407f
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C192 H160 P8 S32 W8 Zn4'
_chemical_formula_sum            'C192 H160 P8 S32 W8 Zn4'
_chemical_formula_weight         5473.61
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             04-09-15
_audit_creation_method           CRYSTALS_ver_12.39
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   18.723(4)
_cell_length_b                   18.723(4)
_cell_length_c                   13.563(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4755(2)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type  Unknown
_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  0.048
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4564
_diffrn_reflns_theta_full        32.973
_diffrn_reflns_theta_max         34.708
_diffrn_reflns_theta_min         1.538
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.781
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       prism
_exptl_crystal_F_000             2656.000
_refine_diff_density_max         1.07
_refine_diff_density_min         -1.66
_refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.37(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2471
_refine_ls_number_restraints     333
_refine_ls_R_factor_all          0.1721
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.129484
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
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Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[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 (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.341 0.265 0.106
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1284
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0594
_reflns_limit_h_max              20
_reflns_limit_h_min              -19
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2471
_reflns_number_total             4564
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.03748(6)
_oxford_structure_analysis_title 'CIF000 I-4'
_cod_data_source_file            b716407f.txt
_cod_data_source_block           PPh4_2Zn_WS4_2
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 
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_cod_original_cell_volume        4754(2)
_cod_original_sg_symbol_H-M      'I -4 '
_cod_database_code               7003476