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_4319448
_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            'C23 H42 B Cl2 N7 Pt S3 W'
_chemical_formula_weight         973.47
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_date             'Wed May 24 12:50:04 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.271(4)
_cell_length_b                   18.961(2)
_cell_length_c                   20.337(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      19.8
_cell_measurement_theta_min      16.6
_cell_volume                     6660(2)
_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      0.00491
_diffrn_orient_matrix_UB_12      0.00554
_diffrn_orient_matrix_UB_13      -0.04872
_diffrn_orient_matrix_UB_21      -0.01341
_diffrn_orient_matrix_UB_22      0.05112
_diffrn_orient_matrix_UB_23      0.00408
_diffrn_orient_matrix_UB_31      0.05611
_diffrn_orient_matrix_UB_32      0.01173
_diffrn_orient_matrix_UB_33      0.00524
_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_R_equivalents  0.191
_diffrn_reflns_av_sigmaI/netI    0.115
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7648
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        -1.07
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.010
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3744.00
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.91
_refine_diff_density_min         -1.35
_refine_ls_extinction_coef       0.00029(3)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.451
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4292
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.0040
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0425
_reflns_number_gt                4292
_reflns_number_total             7647
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ic0008823_5.cif
_cod_data_source_block           '[NEt4][Tp*WS(mu-S)2PtCl2]_(10)'
_cod_original_cell_volume        6659(1)
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C23 H42 B Cl2 N7 Pt S3 W '
_cod_database_code               4319448