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_2018213
_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) [Cu W Br (C15 H22 B N6) S3]'
_chemical_formula_moiety         'C8 H20 N +, C15 H22 B Br Cu N6 S3 W -'
_chemical_formula_sum            'C23 H42 B Br Cu N7 S3 W'
_chemical_formula_weight         850.95
_chemical_name_systematic
;
tetraethylammonium
bromidodi-\m~2~-sulfido-sulfido[tris(3,5-
dimethylpyrazol-1-yl)borato]copper(I)tungsten(VI)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 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                   19.058(4)
_cell_length_b                   10.276(2)
_cell_length_c                   16.323(3)
_cell_measurement_reflns_used    12205
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3491
_cell_measurement_theta_min      3.1730
_cell_volume                     3196.7(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29584
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.17
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.732
_exptl_absorpt_correction_T_max  0.239
_exptl_absorpt_correction_T_min  0.147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.594
_refine_ls_abs_structure_details 'Flack (1983), 2678 Friedel pairs'
_refine_ls_abs_structure_Flack   0.004(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5710
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+1.3297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                5342
_reflns_number_total             5857
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi3020.cif
_cod_data_source_block           I
_cod_original_cell_volume        3196.6(11)
_cod_database_code               2018213
_cod_database_fobs_code          2018213