Construction of Halide-Bridged Tungsten-Copper-Sulfide Double Cubanelike Clusters from a New Precursor [(Tp*WS2)2(μ-S2)]
Li-Pei Wei; Zhi-Gang Ren; Lian-Wen Zhu; Wen-Yan Yan; Sha Sun; Hui-Fang Wang; Jian-Ping Lang; Zhen-Rong Sun; Inorganic Chemistry 50 (2011) 4493–4502; doi:10.1021/ic200147d

data_4325046
_publ_contact_author_address
;
 College of Chemistry, Chemical Engineering and Materials Science
 Soochow University
 Suzhou 215123, Jiangsu
 P.R.China
;
_publ_contact_author_email       jplang@suda.edu.cn
_publ_contact_author_fax         86-512-65880089
_publ_contact_author_name        'Jian-Ping Lang'
_publ_contact_author_phone       86-512-65882865
_publ_section_title
;
 Construction of Halide-Bridged Tungsten-Copper-Sulfide Double Cubanelike
 Clusters from a New Precursor [(Tp*WS2)2(\m-S2)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4493
_journal_page_last               4502
_journal_paper_doi               10.1021/ic200147d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
'(C30 H44 B2 Br5 Cu6 N12 S6 W2), (C6 H14 N), 1.5(C4 H10 O), 2(C H3)'
_chemical_formula_sum            'C44 H79 B2 Br5 Cu6 N13 O1.5 S6 W2'
_chemical_formula_weight         2176.67
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.702(4)
_cell_length_b                   24.328(5)
_cell_length_c                   15.580(3)
_cell_measurement_reflns_used    27113
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.4894
_cell_measurement_theta_min      3.1048
_cell_volume                     8226(3)
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku MercuryCCD area detector'
_diffrn_measurement_method       \w
_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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29006
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.922
_exptl_absorpt_correction_T_max  0.4233
_exptl_absorpt_correction_T_min  0.0854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       Chip
_exptl_crystal_F_000             4196
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.698
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7196
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+18.1372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                6308
_reflns_number_total             7196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200147d_si_002_1.cif
_cod_data_source_block           6
_cod_original_formula_sum        'C44 H79 B2 Br5 Cu6 N13 O1.50 S6 W2'
_cod_database_code               4325046