Formation of a Dithiophosphinate Ligand Ph2PS2by Sulfur Insertion into the Metal−Phosphido Bond on Heterobimetallic Phosphido-Bridged Complex Cp(CO)2W(μ-PPh2)Mo(CO)5: A Rare Example of a Neutral Six-Electron Mixed-Metal Cluster with a Mo2WS4Core
Hossain, Md. Munkir; Lin, Hsiu-Mei; Shyu, Shin-Guang; Organometallics 26 (2007) 685–; doi:10.1021/om0608509

data_4072585
_publ_section_title
;
 Formation of a Dithiophosphinate Ligand Ph2PS2by Sulfur Insertion into
 the Metal&#x2212;Phosphido Bond on Heterobimetallic Phosphido-Bridged
 Complex Cp(CO)2W(\m-PPh2)Mo(CO)5:&#x00A0; A Rare Example of a Neutral
 Six-Electron Mixed-Metal Cluster with a Mo2WS4Core
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              685
_journal_paper_doi               10.1021/om0608509
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C41 H35 Mo2 P3 S10 W1'
_chemical_formula_sum            'C41 H35 Mo2 P3 S10 W'
_chemical_formula_weight         1316.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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             2006-10-30T18:32:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                81.8180(10)
_cell_angle_beta                 82.9540(10)
_cell_angle_gamma                75.1590(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4373(2)
_cell_length_b                   11.4761(2)
_cell_length_c                   20.4699(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     2560.26(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.067
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41385
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.01
_exptl_absorpt_coefficient_mu    3.253
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.846
_refine_diff_density_min         -2.414
_refine_diff_density_rms         0.494
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8948
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1507
_reflns_number_gt                6536
_reflns_number_total             8948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0608509si20061106_075045.cif
_cod_data_source_block           i6146
_cod_original_cell_volume        2560.27(8)
_cod_database_code               4072585