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_4317546
_publ_section_title
;
 Oxidative Addition of Phosphine-Tethered Thiols to Iron Carbonyl:
 Binuclear Phosphinothiolate Complexes, (\m-SCH2CH2PPh2)2Fe2(CO)4, and
 Hydride Derivatives
;
_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            'C31 H28 Fe O3 P2 S2'
_chemical_formula_weight         630.44
_chemical_name_systematic
;

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;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.15(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.123(2)
_cell_length_b                   16.296(4)
_cell_length_c                   24.286(6)
_cell_measurement_temperature    193(2)
_cell_volume                     3196.3(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5769
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.7585
_exptl_absorpt_correction_T_min  0.7112
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+1.9188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                4981
_reflns_number_total             5629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010741g_1.cif
_cod_data_source_block           md47
_cod_database_code               4317546