Synthesis, Structures, and Redox Properties of Octa(μ3-sulfido)hexarhenium(III) Complexes Having Terminal Pyridine Ligands
Takashi Yoshimura; Keisuke Umakoshi; Yoichi Sasaki; A. Geoffrey Sykes; Inorganic Chemistry 38 (1999) 5557–5564; doi:10.1021/ic9907922

data_4322439
_publ_contact_author_address
;
            Pr Yoichi Sasaki
    Division of Chemistry
    Graduate School of Science
    Hokkaido University
    Kita-ku, Sapporo 060-0810
    Japan
;
_publ_contact_author_email       ysasaki@science.hokudai.ac.jp
_publ_contact_author_fax         +81-11-706-3447
_publ_contact_author_name        ' Sasaki, Yoichi '
_publ_contact_author_phone       +81-11-706-3817
_publ_section_title
;
 Synthesis, Structures, and Redox Properties of
 Octa(\m3-sulfido)hexarhenium(III) Complexes Having Terminal Pyridine
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5557
_journal_page_last               5564
_journal_paper_doi               10.1021/ic9907922
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C46 H92 Cl4 N5 O2 Re6 S8'
_chemical_formula_weight         2262.80
_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'
_cell_angle_alpha                90
_cell_angle_beta                 115.76(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.693(8)
_cell_length_b                   19.464(4)
_cell_length_c                   18.592(4)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      12.7
_cell_volume                     8048(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_orient_matrix_UB_11      0.00460
_diffrn_orient_matrix_UB_12      -0.03712
_diffrn_orient_matrix_UB_13      0.03945
_diffrn_orient_matrix_UB_21      -0.04472
_diffrn_orient_matrix_UB_22      -0.00321
_diffrn_orient_matrix_UB_23      -0.02135
_diffrn_orient_matrix_UB_31      -0.00078
_diffrn_orient_matrix_UB_32      -0.03538
_diffrn_orient_matrix_UB_33      -0.03942
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_av_sigmaI/netI    0.061
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9705
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        -0.84
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.364
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.102
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             4260.00
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.22
_refine_diff_density_min         -1.70
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     220
_refine_ls_number_reflns         5271
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.1610
_refine_ls_shift/su_mean         0.0210
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00384|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                5271
_reflns_number_total             9488
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic9907922_1.cif
_cod_data_source_block           (Bu4N)2[trans-{Re6S8Cl4(py)2}]
_cod_original_cell_volume        8047(3)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C46 H92 Cl4 N5 O2 S8 Re6 '
_cod_database_code               4322439