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_4317547
_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            'C33 H29 F3 Fe2 O7 P2 S3'
_chemical_formula_weight         864.38
_chemical_name_systematic
;

   ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.973(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.322(3)
_cell_length_b                   12.859(4)
_cell_length_c                   18.621(4)
_cell_measurement_temperature    110(2)
_cell_volume                     3613.4(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_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  0.0786
_diffrn_reflns_av_sigmaI/netI    0.1167
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24480
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    1.126
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.871
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.692
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         9342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.692
_refine_ls_R_factor_all          0.1321
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          2.081
_refine_ls_shift/su_mean         0.410
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1909P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.2168
_reflns_number_gt                4809
_reflns_number_total             9342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010741g_2.cif
_cod_data_source_block           mdx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        3613.2(14)
_cod_database_code               4317547