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_7003475
_publ_section_title
;
 Structural chemistry of (PPh4)2M(WS4)2 materials
;
_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 unk
_chemical_formula_moiety         'C48 H40 P2 S8 W2 Zn1'
_chemical_formula_sum            'C48 H40 P2 S8 W2 Zn'
_chemical_formula_weight         1368.40
_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             04-08-13
_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                   13.2295(3)
_cell_length_b                   13.2295(3)
_cell_length_c                   6.7770(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1186.11(5)
_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    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.954
_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  0.034
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20241
_diffrn_reflns_theta_full        32.582
_diffrn_reflns_theta_max         34.661
_diffrn_reflns_theta_min         2.177
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.793
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_description       needle
_exptl_crystal_F_000             664
_refine_diff_density_max         1.42
_refine_diff_density_min         -0.42
_refine_ls_extinction_coef       3.4(14)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   0.7270
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0177
_refine_ls_shift/su_max          0.000297
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
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:
2.98 3.67 1.18
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0402
_refine_ls_wR_factor_gt          0.0396
_refine_ls_wR_factor_ref         0.0396
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_gt                1175
_reflns_number_total             1292
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.14793(6)
_oxford_structure_analysis_title '019subsad in I-4'
_cod_data_source_file            b716407f.txt
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
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 
;
_cod_original_sg_symbol_H-M      'I -4 '
_cod_original_formula_sum        'C48 H40 P2 S8 W2 Zn1'
_cod_database_code               7003475