Tetraethylammonium [1-methylimidazole-2(3<i>H</i>)-thione]copper(I)-di-μ-sulfido-dioxotungstate(VI)
Beheshti, Azizolla; Brooks, Neil R.; Clegg, William; Khorrmdin, Rahman; Acta Crystallographica Section E 60 (2004) m1923–m1926; doi:10.1107/S1600536804030132

data_2204751
_publ_section_title
;Tetraethylammonium
 [1-methylimidazole-2(3<i>H</i>)-thione]copper(I)-di-\m-sulfido-dioxotungstate(VI)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1923
_journal_page_last               m1926
_journal_paper_doi               10.1107/S1600536804030132
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '(C8 H20 N) [W Cu O2 S2 (C4 H6 N2 S)]'
_chemical_formula_moiety         'C8 H20 N +, C4 H6 Cu N2 O2 S3 W -'
_chemical_formula_sum            'C12 H26 Cu N3 O2 S3 W'
_chemical_formula_weight         587.93
_chemical_name_systematic
;
[1-methylimidazole-2(3H)-thione-2\kS]dioxo-1\k^2^O-di-\m-sulfido-1:2\k^4^S:S-
copper(I)tungstate(VI)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   7.1985(5)
_cell_length_b                   16.3720(14)
_cell_length_c                   17.244(2)
_cell_measurement_reflns_used    17595
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.5
_cell_volume                     2032.3(3)
_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, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17533
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         4.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.018
_exptl_absorpt_correction_T_max  0.570
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.680
_refine_diff_density_min         -3.791
_refine_ls_abs_structure_details 'Flack (1983), 1483 Friedel pairs'
_refine_ls_abs_structure_Flack   0.35(5)
_refine_ls_extinction_coef       0.0029(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.237
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3557
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0924
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+149.3501P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2311
_refine_ls_wR_factor_ref         0.2329
_reflns_number_gt                3369
_reflns_number_total             3557
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6320.cif
_cod_data_source_block           I
_cod_database_code               2204751
_cod_database_fobs_code          2204751