Preparation of Mononuclear Tungsten Tris(sulfido) and Molybdenum Sulfido-Tetrasulfido Complexes with Hydridotris(pyrazolyl)borate Coligand and Conversion of the Former into Sulfido-Bridged Bimetallic Complex Having Pt(μ-S)2WS Core
Hidetake Seino; Yasushi Arai; Naohisa Iwata; Shoken Nagao; Yasushi Mizobe; Masanobu Hidai; Inorganic Chemistry 40 (2001) 1677–1682; doi:10.1021/ic0008823

data_4319444
_publ_contact_author_address
;
    Institute of Industrial Scienece, The University of Tokyo,
    Roppongi, Minato-ku, Tokyo 106-8558, Japan
;
_publ_contact_author_email       ymizobe@iis.u-tokyo.ac.jp
_publ_contact_author_fax         '(+81) 3 (3402) 6303'
_publ_contact_author_name        'Yasushi Mizobe'
_publ_section_title
;
 Preparation of Mononuclear Tungsten Tris(sulfido) and Molybdenum
 Sulfido-Tetrasulfido Complexes with Hydridotris(pyrazolyl)borate Coligand
 and Conversion of the Former into Sulfido-Bridged Bimetallic Complex
 Having Pt(\m-S)2WS Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1677
_journal_page_last               1682
_journal_paper_doi               10.1021/ic0008823
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C25 H45 B N8 S3 W'
_chemical_formula_weight         748.52
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_date             'Sat Nov 27 20:25:37 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.056(1)
_cell_length_b                   10.974(1)
_cell_length_c                   18.250(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      19.7
_cell_volume                     3215.6(5)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.06214
_diffrn_orient_matrix_UB_12      0.00364
_diffrn_orient_matrix_UB_13      -0.00295
_diffrn_orient_matrix_UB_21      -0.00387
_diffrn_orient_matrix_UB_22      0.07765
_diffrn_orient_matrix_UB_23      -0.02847
_diffrn_orient_matrix_UB_31      0.00156
_diffrn_orient_matrix_UB_32      0.04755
_diffrn_orient_matrix_UB_33      0.04672
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_sigmaI/netI    0.036
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            3884
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        -3.36
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.820
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            redbrown
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1512.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.60
_refine_ls_extinction_coef       0.0029(2)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.543
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3082
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.3060
_refine_ls_shift/su_mean         0.0230
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0250
_refine_ls_wR_factor_ref         0.0250
_reflns_number_gt                3082
_reflns_number_total             3883
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ic0008823_1.cif
_cod_data_source_block           '[NEt4][Tp*W(S)3]_(1a)'
_cod_original_cell_volume        3215.5(8)
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C25 H45 B N8 S3 W '
_cod_database_code               4319444