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_4072584
_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_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C23 H21 Mo1 O5 P1 S6 W1'
_chemical_formula_sum            'C23 H21 Mo O5 P S6 W'
_chemical_formula_weight         880.52
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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             2006-10-23T21:21:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 120.183(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.204(6)
_cell_length_b                   6.7865(14)
_cell_length_c                   18.204(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                     3012.0(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      298(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 CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.034822
_diffrn_orient_matrix_UB_12      -0.002968
_diffrn_orient_matrix_UB_13      -0.056126
_diffrn_orient_matrix_UB_21      -0.021286
_diffrn_orient_matrix_UB_22      0.032134
_diffrn_orient_matrix_UB_23      0.028796
_diffrn_orient_matrix_UB_31      0.004042
_diffrn_orient_matrix_UB_32      0.143802
_diffrn_orient_matrix_UB_33      -0.007604
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1093
_diffrn_reflns_av_unetI/netI     0.1741
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3013
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.27
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.733
_exptl_absorpt_correction_T_max  0.382
_exptl_absorpt_correction_T_min  0.297
_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   5
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.066
_refine_diff_density_min         -2.166
_refine_diff_density_rms         0.249
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         2918
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.1696
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0882P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.132
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                1769
_reflns_number_total             2918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0608509si20061106_075023.cif
_cod_data_source_block           i5137
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4072584