Synthesis and Characterization of Single Thiolato-Bridged Heterodinuclear Complexes: Irreversible Isomerization of Cp(CO)2W(μ-SPh)(μ-Cl)Ru(CO)(Cl)(PPh3) to Cp(CO)(Cl)W(μ-SPh)(μ-Cl)Ru(CO)2(PPh3) via Chloride and Carbonyl Ligand Migration
Hossain, Md. Munkir; Lin, Hsiu-Mei; Wang, Chih-Min; Shyu, Shin-Guang; Organometallics 28 (2009) 264–; doi:10.1021/om800789m

data_4068381
_publ_section_title
;
 Synthesis and Characterization of Single Thiolato-Bridged Heterodinuclear
 Complexes: Irreversible Isomerization of
 Cp(CO)2W(\m-SPh)(\m-Cl)Ru(CO)(Cl)(PPh3) to
 Cp(CO)(Cl)W(\m-SPh)(\m-Cl)Ru(CO)2(PPh3) via Chloride and Carbonyl Ligand
 Migration
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              264
_journal_paper_doi               10.1021/om800789m
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H25 Cl2 O3 P1 Ru1 S1 W1'
_chemical_formula_sum            'C32 H25 Cl2 O3 P Ru S W'
_chemical_formula_weight         876.37
_chemical_name_systematic
;
 ?
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2008-01-28T13:05:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 103.46(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6341(18)
_cell_length_b                   19.703(4)
_cell_length_c                   14.856(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     3027.2(11)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.0227
_diffrn_orient_matrix_UB_12      0.04288
_diffrn_orient_matrix_UB_13      -0.028542
_diffrn_orient_matrix_UB_21      0.032643
_diffrn_orient_matrix_UB_22      -0.027132
_diffrn_orient_matrix_UB_23      -0.04673
_diffrn_orient_matrix_UB_31      -0.088142
_diffrn_orient_matrix_UB_32      0.001006
_diffrn_orient_matrix_UB_33      -0.042336
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5618
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.75
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.627
_exptl_absorpt_correction_T_max  0.5644
_exptl_absorpt_correction_T_min  0.4426
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   2
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.326
_refine_diff_density_min         -1.631
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                3429
_reflns_number_total             5314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800789m_si_002.cif
_cod_data_source_block           i6006
_cod_original_cell_volume        3027.2(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4068381