Disorder in Bis(tetraethylammonium) Bis(μ-sulfido)bis[(1,2,3,4-tetrathiabutane-1,4-diyl-<i>S</i>,<i>S</i>)thiotungstate(V)]
Mukherjee, A. K.; Das, P. K.; Mukherjee, M.; Chakraborty, P. K.; Bhattacharya, R.; Acta Crystallographica Section C 53 (1997) 209–212; doi:10.1107/S0108270196011699

data_2005913
_publ_section_title
;Disorder in Bis(tetraethylammonium)
 Bis(\m-sulfido)bis[(1,2,3,4-tetrathiabutane-1,4-diyl-<i>S</i>,<i>S</i>)thiotungstate(V)]
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              209
_journal_page_last               212
_journal_paper_doi               10.1107/S0108270196011699
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[(C2 H5)4 N]2 [W2 S12]'
_chemical_formula_moiety         'C16 H40 N2 S12 W2'
_chemical_formula_sum            'C16 H40 N2 S12 W2'
_chemical_formula_weight         1012.92
_chemical_name_systematic
;
Bis(tetraethylammonium)
bis(\m-sulfido)-bis[(1,2,3,4-tetrathiabutan-1,4-diyl-S,S)thiotungstate(V)]
;
_space_group_IT_number           120
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 -2c'
_symmetry_space_group_name_H-M   'I -4 c 2'
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_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
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_cell_length_b                   21.174(4)
_cell_length_c                   15.119(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      7.5
_cell_volume                     6778(2)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CAD-4 Software'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
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_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        3
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_exptl_absorpt_coefficient_mu    7.534
_exptl_absorpt_correction_T_max  0.471
_exptl_absorpt_correction_T_min  0.151
_exptl_absorpt_correction_type   '\y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            maroon
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_meas      1.97
_exptl_crystal_density_method
'flotation in ethyl iodide/1,3-dibromopropane'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.80
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_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.47(4)
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_refine_ls_goodness_of_fit_obs   1.090
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_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_obs          0.0484
_refine_ls_shift/esd_max         0.610
_refine_ls_shift/esd_mean        0.060
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.07P)^2^+74.7P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1244
_refine_ls_wR_factor_obs         0.1139
_reflns_number_observed          2190
_reflns_number_total             2828
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1055.cif
_cod_data_source_block           tungstate
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'NO' changed to 'no' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.07P)^2^+74.7P] where P=(Fo^2^+2Fc^2^)/3' 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^2^)+(0.07P)^2^+74.7P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2005913