Synthesis of Bis{(2-dimethylphosphino)ethane-1-thiolato}bis(tert-butylthiolato)- molybdenum(IV) and Its Cluster-Forming Reactions with FeCl2 and CuBr
Yasuhiro Arikawa; Hiroyuki Kawaguchi; Kazuo Kashiwabara; Kazuyuki Tatsumi; Inorganic Chemistry 38 (1999) 4549–4553; doi:10.1021/ic990435r

data_4322287
_publ_contact_author_address
;
    Research Center for Materials Science, Nagoya University, Furo-cho, 
Chikusa-ku, Nagoya 464-8602, Japan
;
_publ_contact_author_name        ' Kazuyuki Tatsumi'
_publ_section_title
;
 Synthesis of
 Bis{(2-dimethylphosphino)ethane-1-thiolato}bis(tert-butylthiolato)-
 molybdenum(IV) and Its Cluster-Forming Reactions with FeCl2 and CuBr
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4549
_journal_page_last               4553
_journal_paper_doi               10.1021/ic990435r
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C31 H73 Br2 Cu4 Mo2 O P4 S8'
_chemical_formula_weight         1448.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Thu Apr  8 16:28:59 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 100.92(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            4
_cell_length_a                   16.156(8)
_cell_length_b                   13.482(3)
_cell_length_c                   26.102(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.7
_cell_measurement_theta_min      12.6
_cell_volume                     5582(4)
_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    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.02094
_diffrn_orient_matrix_UB_12      0.00431
_diffrn_orient_matrix_UB_13      0.06251
_diffrn_orient_matrix_UB_21      -0.03258
_diffrn_orient_matrix_UB_22      -0.01996
_diffrn_orient_matrix_UB_23      0.03900
_diffrn_orient_matrix_UB_31      0.00460
_diffrn_orient_matrix_UB_32      -0.05966
_diffrn_orient_matrix_UB_33      -0.00852
_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  0.034
_diffrn_reflns_av_sigmaI/netI    0.077
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            13845
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        -0.23
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.805
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2900.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7404
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.9300
_refine_ls_shift/su_mean         0.0020
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00152|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0586
_reflns_number_gt                7404
_reflns_number_total             13377
_reflns_threshold_expression     >3.0sigma(I)
_cod_data_source_file            ic990435r_3.cif
_cod_data_source_block           '[MoBr(dmsp)2(m3-S)Cu2]2(m-StBu)2'
_cod_original_cell_volume        5582(3)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C31 H73 Br2 Cu4 Mo2 O P4 S8 '
_cod_database_code               4322287