Bis(tetra-<i>n</i>-butylammonium) tetrakis[chloro(μ~3~-sulfido)copper(I)]tungstate(VI): a second polymorph
Hossaini Sadr, Moayad; Seyed Ahmadian, Seyed Masoud; Brooks, Neil R.; Clegg, William; Acta Crystallographica Section E 60 (2004) m1952–m1954; doi:10.1107/S1600536804030582

data_2204752
_publ_section_title
;
 Bis(tetra-<i>n</i>-butylammonium)
 tetrakis[chloro(\m~3~-sulfido)copper(I)]tungstate(VI): a second
 polymorph
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1952
_journal_page_last               m1954
_journal_paper_doi               10.1107/S1600536804030582
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '(C16 H36 N)2 [W Cu4 Cl4 S4]'
_chemical_formula_moiety         '2C16 H36 N +, Cl4 Cu4 S4 W 2-'
_chemical_formula_sum            'C32 H72 Cl4 Cu4 N2 S4 W'
_chemical_formula_weight         1192.97
_chemical_name_systematic
;
Bis(tetra-n-butylammonium)
tetrakis[chloro(\m~3~-sulfido)copper(I)]tungstate(VI)
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3652(5)
_cell_length_b                   13.3652(5)
_cell_length_c                   13.668(2)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     2441.5(4)
_computing_cell_refinement       'EvalCCD (Duisenberg et al., 2003)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            42475
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         4.53
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.474
_exptl_absorpt_correction_T_max  0.637
_exptl_absorpt_correction_T_min  0.147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.591
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0216
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0199P)^2^+2.9221P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0558
_reflns_number_gt                2441
_reflns_number_total             2804
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6324.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               2204752
_cod_database_fobs_code          2204752