Two W/Cu/S clusters: tetraethylammonium bromidodi-μ~2~-sulfido-sulfido[tris(3,5-dimethylpyrazol-1-yl)borato]copper(I)tungsten(VI) and tetraethylammonium dibromido-μ~3~-sulfido-di-μ~2~-sulfido-[tris(3,5-dimethylpyrazol-1-yl)borato]dicopper(I)tungsten(VI)
Wei, Zhenhong; You, Xiuli; Acta Crystallographica Section C 67 (2011) m307–m310; doi:10.1107/S0108270111032586

data_2018214
_publ_section_title
;
 Two W/Cu/S clusters: tetraethylammonium
 bromidodi-\m~2~-sulfido-sulfido[tris(3,5-dimethylpyrazol-1-yl)borato]copper(I)tungsten(VI)
 and tetraethylammonium
 dibromido-\m~3~-sulfido-di-\m~2~-sulfido-[tris(3,5-dimethylpyrazol-1-yl)borato]dicopper(I)tungsten(VI)
;
_journal_coeditor_code           BI3020
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m307
_journal_page_last               m310
_journal_paper_doi               10.1107/S0108270111032586
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C8 H20 N) [Cu2 W Br2 (C15 H22 B N6) S3]'
_chemical_formula_moiety         'C8 H20 N +, C15 H22 B Br2 Cu2 N6 S3 W -'
_chemical_formula_sum            'C23 H42 B Br2 Cu2 N7 S3 W'
_chemical_formula_weight         994.40
_chemical_name_systematic
;
tetraethylammonium
dibromido-\m~3~-sulfido-di-\m~2~-sulfido-[tris(3,5-
dimethylpyrazol-1-yl)borato]dicopper(I)tungsten(VI)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   12.808(3)
_cell_length_b                   11.768(2)
_cell_length_c                   22.569(5)
_cell_measurement_reflns_used    12018
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3491
_cell_measurement_theta_min      3.1387
_cell_volume                     3401.7(12)
_computing_cell_refinement       'CrystalClear (Rigaku, 2001)'
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_data_reduction        'CrystalStructure (Rigaku, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32255
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.14
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.172
_exptl_absorpt_correction_T_max  0.295
_exptl_absorpt_correction_T_min  0.087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.478
_refine_diff_density_min         -1.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.069P)^2^+4.773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1196
_reflns_number_gt                2999
_reflns_number_total             3282
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi3020.cif
_cod_data_source_block           II
_cod_database_code               2018214
_cod_database_fobs_code          2018214