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_4322285
_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            'C16 H38 Mo P2 S4'
_chemical_formula_weight         516.60
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             'Thu Apr  8 15:24:55 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 93.63(5)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   64.12(3)
_cell_length_b                   9.195(4)
_cell_length_c                   17.28(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      6.0
_cell_measurement_theta_min      2.2
_cell_volume                     10168(13)
_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      -0.00344
_diffrn_orient_matrix_UB_12      0.09766
_diffrn_orient_matrix_UB_13      0.02129
_diffrn_orient_matrix_UB_21      -0.01520
_diffrn_orient_matrix_UB_22      -0.02523
_diffrn_orient_matrix_UB_23      -0.00434
_diffrn_orient_matrix_UB_31      0.00120
_diffrn_orient_matrix_UB_32      -0.04065
_diffrn_orient_matrix_UB_33      0.05375
_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  0.264
_diffrn_reflns_av_sigmaI/netI    0.156
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2436
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         19.95
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        -12.80
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4320.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.58
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.383
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     255
_refine_ls_number_reflns         1508
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00073|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                1508
_reflns_number_total             2354
_reflns_threshold_expression     >1.0sigma(I)
_cod_data_source_file            ic990435r_1.cif
_cod_data_source_block           Mo(dmsp)2(StBu)2
_cod_original_cell_volume        10169(11)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C16 H38 Mo P2 S4 '
_cod_database_code               4322285