Synthesis and Reactivity of Hybrid Phosphido- and Hydrosulfido-Bridged Diruthenium Complexes: Transformations into Diruthenium and Tetraruthenium Complexes Bridged by Phosphido and Sulfido Ligands
Miyake, Yoshihiro; Moriyama, Taichi; Tanabe, Yoshiaki; Endo, Satoshi; Nishibayashi, Yoshiaki; Organometallics 31 (2012) 3292–; doi:10.1021/om3001247

data_4078108
_publ_section_title
;
 Synthesis and Reactivity of Hybrid Phosphido- and Hydrosulfido-Bridged
 Diruthenium Complexes: Transformations into Diruthenium and
 Tetraruthenium Complexes Bridged by Phosphido and Sulfido Ligands
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3292
_journal_paper_doi               10.1021/om3001247
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C52 H88 Cl2 O2 P2 Ru4 S2'
_chemical_formula_sum            'C52 H88 Cl2 O2 P2 Ru4 S2'
_chemical_formula_weight         1346.52
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 97.0320(16)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   13.9721(8)
_cell_length_b                   17.8282(13)
_cell_length_c                   22.6549(13)
_cell_measurement_reflns_used    21208
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.14
_cell_volume                     5600.8(6)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27110
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.3227
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2752.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.040
_refine_diff_density_min         -1.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6398
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[10.4000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1522
_reflns_number_gt                5097
_reflns_number_total             6398
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om3001247_si_001.cif
_cod_data_source_block           3_Cl_2C4H8O
_cod_database_code               4078108