Redox-Active Dithiafulvenyldiphenylphosphine as a Mono- or Bidentate Ligand: Intramolecular Coupling Reaction in the Coordination Sphere of a Metal Carbonyl Fragment
Michel Guerro; Thierry Roisnel; Pascal Pellon; Dominique Lorcy; Inorganic Chemistry 44 (2005) 3347–3355; doi:10.1021/ic0501465

data_4308855
_publ_section_title
;
Redox-Active Dithiafulvenyldiphenylphosphine as a Mono- or Bidentate
Ligand: Intramolecular Coupling Reaction in the Coordination Sphere of a
Metal Carbonyl Fragment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3347
_journal_page_last               3355
_journal_paper_doi               10.1021/ic0501465
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C40 H32 Mo1 O4 P2 S4, C0.5 O0.5 H2'
_chemical_formula_sum            'C40.5 H34 Mo O4.5 P2 S4'
_chemical_formula_weight         878.8
_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      2.2
_audit_creation_date             2004-12-21T17:39:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                108.153(5)
_cell_angle_beta                 97.856(5)
_cell_angle_gamma                100.075(5)
_cell_formula_units_Z            4
_cell_length_a                   12.361(5)
_cell_length_b                   17.884(5)
_cell_length_c                   19.837(5)
_cell_measurement_reflns_used    42095
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     4016(2)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_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    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.80743E-1
_diffrn_orient_matrix_UB_12      -0.10853E-2
_diffrn_orient_matrix_UB_13      0.1614E-2
_diffrn_orient_matrix_UB_21      -0.108587E-1
_diffrn_orient_matrix_UB_22      0.106826E-1
_diffrn_orient_matrix_UB_23      -0.467359E-1
_diffrn_orient_matrix_UB_31      -0.201732E-1
_diffrn_orient_matrix_UB_32      -0.595053E-1
_diffrn_orient_matrix_UB_33      -0.273384E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59157
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.03
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     939
_refine_ls_number_reflns         16996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+7.2812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.1182
_reflns_number_gt                9722
_reflns_number_total             16996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0501465si20050128_123303.cif
_cod_data_source_block           mg52
_cod_original_formula_sum        'C40.50 H34 Mo O4.50 P2 S4'
_cod_database_code               4308855