A Thiophosphinidene Complex as a Vehicle in Phosphinidene Transmetalation: Easy Formation and Cleavage of a P-S Bond
Belén Alvarez; M. Angeles Alvarez; Inmaculada Amor; M. Esther García; Miguel A. Ruiz; Inorganic Chemistry 50 (2011) 10561–10563; doi:10.1021/ic202058h

data_4326801
_publ_section_title
;
 A Thiophosphinidene Complex as a Vehicle in Phosphinidene
 Transmetalation: Easy Formation and Cleavage of a P-S Bond
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10561
_journal_page_last               10563
_journal_paper_doi               10.1021/ic202058h
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C34 H39 Fe Mo2 O6 P S'
_chemical_formula_sum            'C34 H39 Fe Mo2 O6 P S'
_chemical_formula_weight         854.42
_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_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                77.456(2)
_cell_angle_beta                 83.659(2)
_cell_angle_gamma                89.924(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1160(4)
_cell_length_b                   10.9552(4)
_cell_length_c                   15.9379(5)
_cell_measurement_reflns_used    1916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      3.13
_cell_measurement_wavelength     0.71073
_cell_volume                     1713.11(11)
_computing_cell_refinement       'BRUKER APEX'
_computing_data_collection       'BRUKER APEX'
_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    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega/phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            39867
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.9
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0188
_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^)+(0.0181P)^2^+1.7190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.051
_reflns_number_gt                6534
_reflns_number_total             7054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202058h_si_002_3.cif
_cod_data_source_block           compound5
_cod_database_code               4326801