μ~3~-Bromido-oxidotri-μ~3~-sulfido-tris(triphenylphosphane-κ<i>P</i>)tricopper(I)tungsten(VI)
Huang, Wenjiang; Zhang, Jinfang; Zhang, Chi; Acta Crystallographica Section E 68 (2012) m281–; doi:10.1107/S1600536812004631

data_2233959
_publ_section_title
;
 \m~3~-Bromido-oxidotri-\m~3~-sulfido-tris(triphenylphosphane-\k<i>P</i>)tricopper(I)tungsten(VI)
;
_journal_coeditor_code           PV2509
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m281
_journal_paper_doi               10.1107/S1600536812004631
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu3 W Br O S3 (C18 H15 P)3]'
_chemical_formula_moiety         'C54 H45 Br Cu3 O P3 S3 W'
_chemical_formula_sum            'C54 H45 Br Cu3 O P3 S3 W'
_chemical_formula_weight         1353.41
_chemical_name_systematic
;
\m~3~-bromo-tri-\m~3~-sulfido-oxo-tris
(triphenylphosphane-<i>\kp</i>)-tricopper(I)-tungsten(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           'SHELXTL (Sheldrick, 2008)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8600(13)
_cell_length_b                   17.6436(17)
_cell_length_c                   22.732(2)
_cell_measurement_reflns_used    20240
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3491
_cell_measurement_theta_min      3.1195
_cell_volume                     5157.8(9)
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49122
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.471
_exptl_absorpt_correction_T_max  0.5536
_exptl_absorpt_correction_T_min  0.3037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.971
_refine_ls_abs_structure_details 'Flack (1983), 4199 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.014(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         9409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                8353
_reflns_number_total             9409
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pv2509.cif
_cod_data_source_block           I
_cod_database_code               2233959
_cod_database_fobs_code          2233959