Oxidative Addition of Phosphine-Tethered Thiols to Iron Carbonyl: Binuclear Phosphinothiolate Complexes, (μ-SCH2CH2PPh2)2Fe2(CO)4, and Hydride Derivatives
Xuan Zhao; Yui-May Hsiao; Chia-Huei Lai; Joseph H. Reibenspies; Marcetta Y. Darensbourg; Inorganic Chemistry 41 (2002) 699–708; doi:10.1021/ic010741g

data_4317548
_publ_section_title
;
 Oxidative Addition of Phosphine-Tethered Thiols to Iron Carbonyl:
 Binuclear Phosphinothiolate Complexes, (\m-SCH2CH2PPh2)2Fe2(CO)4, and
 Hydride Derivatives
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              699
_journal_page_last               708
_journal_paper_doi               10.1021/ic010741g
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C32 H28 Fe2 O4 P2 S2'
_chemical_formula_weight         714.30
_chemical_name_systematic
;

   ?

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                103.83(3)
_cell_angle_beta                 104.83(2)
_cell_angle_gamma                94.23(2)
_cell_formula_units_Z            2
_cell_length_a                   11.242(3)
_cell_length_b                   12.021(2)
_cell_length_c                   12.030(3)
_cell_measurement_temperature    193(2)
_cell_volume                     1510.2(7)
_computing_cell_refinement       'XSCANS (SIEMENS, 1995)'
_computing_data_collection       'XSCANS (SIEMENS, 1995)'
_computing_molecular_graphics    'XP (SIEMENS, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_sigmaI/netI    0.1365
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5444
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+5.2465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1579
_reflns_number_gt                3012
_reflns_number_total             5152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010741g_3.cif
_cod_data_source_block           md242
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4317548