#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:39:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179255 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/75/4317548.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4317548
loop_
_publ_author_name
'Xuan Zhao'
'Yui-May Hsiao'
'Chia-Huei Lai'
'Joseph H. Reibenspies'
'Marcetta Y. Darensbourg'
_publ_section_title
;
 Oxidative Addition of Phosphine-Tethered Thiols to Iron Carbonyl:
 Binuclear Phosphinothiolate Complexes, (μ-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            '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       ω
_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/[σ²(Fo²)+(0.0366P)²+5.2465P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.69337(10) 0.72419(9) 0.90489(9) 0.0196(3) Uani 1 1 d . . .
Fe2 Fe 0.48421(10) 0.64616(9) 0.73874(9) 0.0201(3) Uani 1 1 d . . .
S1 S 0.62136(18) 0.53591(16) 0.81486(18) 0.0230(5) Uani 1 1 d . . .
S2 S 0.50300(18) 0.70378(16) 0.93713(17) 0.0218(5) Uani 1 1 d . . .
P1 P 0.83947(19) 0.70265(17) 0.81166(18) 0.0215(5) Uani 1 1 d . . .
P2 P 0.37377(19) 0.78865(17) 0.72125(17) 0.0208(5) Uani 1 1 d . . .
O1 O 0.8268(6) 0.7245(6) 1.1481(5) 0.0495(18) Uani 1 1 d . . .
O2 O 0.7390(6) 0.9728(5) 0.9368(5) 0.0355(15) Uani 1 1 d . . .
O3 O 0.2761(6) 0.4559(5) 0.6469(6) 0.0504(18) Uani 1 1 d . . .
O4 O 0.5264(5) 0.6451(5) 0.5082(5) 0.0356(15) Uani 1 1 d . . .
C1 C 0.7778(8) 0.7237(7) 1.0517(7) 0.0274(19) Uani 1 1 d . . .
C2 C 0.7162(7) 0.8741(7) 0.9236(6) 0.0227(18) Uani 1 1 d . . .
C3 C 0.3541(8) 0.5338(7) 0.6836(7) 0.029(2) Uani 1 1 d . . .
C4 C 0.5147(7) 0.6435(6) 0.6024(7) 0.0229(18) Uani 1 1 d . . .
C5 C 0.7230(8) 0.4790(6) 0.7259(7) 0.0274(19) Uani 1 1 d . . .
H5A H 0.7865 0.4428 0.7733 0.033 Uiso 1 1 calc R . .
H5B H 0.6734 0.4179 0.6545 0.033 Uiso 1 1 calc R . .
C6 C 0.7876(7) 0.5707(7) 0.6862(7) 0.0249(18) Uani 1 1 d . . .
H6A H 0.7298 0.5879 0.6172 0.030 Uiso 1 1 calc R . .
H6B H 0.8600 0.5429 0.6615 0.030 Uiso 1 1 calc R . .
C7 C 0.9899(7) 0.6804(7) 0.9015(7) 0.0241(18) Uani 1 1 d . . .
C8 C 1.0520(8) 0.5893(7) 0.8667(8) 0.030(2) Uani 1 1 d . . .
H8 H 1.0147 0.5320 0.7936 0.036 Uiso 1 1 calc R . .
C9 C 1.1673(8) 0.5801(8) 0.9362(9) 0.041(2) Uani 1 1 d . . .
H9 H 1.2073 0.5155 0.9115 0.049 Uiso 1 1 calc R . .
C10 C 1.2254(8) 0.6637(8) 1.0416(8) 0.040(2) Uani 1 1 d . . .
H10 H 1.3067 0.6595 1.0872 0.047 Uiso 1 1 calc R . .
C11 C 1.1624(8) 0.7537(9) 1.0792(8) 0.039(2) Uani 1 1 d . . .
H11 H 1.1998 0.8108 1.1524 0.046 Uiso 1 1 calc R . .
C12 C 1.0451(7) 0.7608(7) 1.0103(7) 0.031(2) Uani 1 1 d . . .
H12 H 1.0018 0.8217 1.0381 0.037 Uiso 1 1 calc R . .
C13 C 0.8875(7) 0.8139(6) 0.7438(7) 0.0225(18) Uani 1 1 d . . .
C14 C 0.9873(8) 0.9002(7) 0.8050(8) 0.033(2) Uani 1 1 d . . .
H14 H 1.0330 0.9016 0.8836 0.040 Uiso 1 1 calc R . .
C15 C 1.0216(9) 0.9842(7) 0.7541(9) 0.042(2) Uani 1 1 d . . .
H15 H 1.0907 1.0421 0.7981 0.050 Uiso 1 1 calc R . .
C16 C 0.9584(10) 0.9854(8) 0.6425(9) 0.045(3) Uani 1 1 d . . .
H16 H 0.9833 1.0429 0.6076 0.054 Uiso 1 1 calc R . .
C17 C 0.8575(9) 0.9018(9) 0.5803(9) 0.043(2) Uani 1 1 d . . .
H17 H 0.8116 0.9026 0.5023 0.052 Uiso 1 1 calc R . .
C18 C 0.8219(8) 0.8162(8) 0.6303(7) 0.035(2) Uani 1 1 d . . .
H18 H 0.7521 0.7590 0.5862 0.042 Uiso 1 1 calc R . .
C19 C 0.4370(7) 0.8386(7) 0.9625(7) 0.0257(18) Uani 1 1 d . . .
H19A H 0.4124 0.8520 1.0374 0.031 Uiso 1 1 calc R . .
H19B H 0.4997 0.9044 0.9701 0.031 Uiso 1 1 calc R . .
C20 C 0.3240(7) 0.8303(7) 0.8579(6) 0.0252(19) Uani 1 1 d . . .
H20A H 0.2928 0.9058 0.8648 0.030 Uiso 1 1 calc R . .
H20B H 0.2567 0.7715 0.8562 0.030 Uiso 1 1 calc R . .
C21 C 0.2302(7) 0.7505(6) 0.5970(7) 0.0193(17) Uani 1 1 d . . .
C22 C 0.1269(7) 0.6865(7) 0.6038(7) 0.0283(19) Uani 1 1 d . . .
H22 H 0.1279 0.6651 0.6751 0.034 Uiso 1 1 calc R . .
C23 C 0.0211(8) 0.6531(7) 0.5068(7) 0.035(2) Uani 1 1 d . . .
H23 H -0.0504 0.6101 0.5125 0.042 Uiso 1 1 calc R . .
C24 C 0.0196(8) 0.6822(7) 0.4029(7) 0.031(2) Uani 1 1 d . . .
H24 H -0.0530 0.6592 0.3369 0.037 Uiso 1 1 calc R . .
C25 C 0.1228(8) 0.7446(7) 0.3941(7) 0.033(2) Uani 1 1 d . . .
H25 H 0.1215 0.7638 0.3217 0.039 Uiso 1 1 calc R . .
C26 C 0.2290(8) 0.7796(7) 0.4907(7) 0.0271(19) Uani 1 1 d . . .
H26 H 0.3002 0.8229 0.4847 0.033 Uiso 1 1 calc R . .
C27 C 0.4379(7) 0.9281(6) 0.7071(6) 0.0232(18) Uani 1 1 d . . .
C28 C 0.5476(8) 0.9412(7) 0.6783(7) 0.032(2) Uani 1 1 d . . .
H28 H 0.5942 0.8786 0.6689 0.038 Uiso 1 1 calc R . .
C29 C 0.5903(9) 1.0458(7) 0.6628(8) 0.037(2) Uani 1 1 d . . .
H29 H 0.6658 1.0533 0.6419 0.045 Uiso 1 1 calc R . .
C30 C 0.5273(9) 1.1382(8) 0.6767(8) 0.040(2) Uani 1 1 d . . .
H30 H 0.5581 1.2093 0.6656 0.049 Uiso 1 1 calc R . .
C31 C 0.4179(10) 1.1262(8) 0.7070(8) 0.046(3) Uani 1 1 d . . .
H31 H 0.3735 1.1901 0.7195 0.056 Uiso 1 1 calc R . .
C32 C 0.3732(8) 1.0214(7) 0.7192(8) 0.035(2) Uani 1 1 d . . .
H32 H 0.2956 1.0130 0.7363 0.042 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Fe1 C1 97.9(3) . . ?
C2 Fe1 P1 90.5(3) . . ?
C1 Fe1 P1 101.2(3) . . ?
C2 Fe1 S1 158.7(2) . . ?
C1 Fe1 S1 103.4(3) . . ?
P1 Fe1 S1 86.78(9) . . ?
C2 Fe1 S2 99.7(3) . . ?
C1 Fe1 S2 95.0(3) . . ?
P1 Fe1 S2 159.54(9) . . ?
S1 Fe1 S2 77.26(8) . . ?
C2 Fe1 Fe2 105.7(2) . . ?
C1 Fe1 Fe2 144.0(3) . . ?
P1 Fe1 Fe2 105.30(7) . . ?
S1 Fe1 Fe2 55.07(7) . . ?
S2 Fe1 Fe2 54.93(6) . . ?
C4 Fe2 C3 97.9(4) . . ?
C4 Fe2 P2 90.2(3) . . ?
C3 Fe2 P2 95.6(3) . . ?
C4 Fe2 S1 102.2(3) . . ?
C3 Fe2 S1 95.3(3) . . ?
P2 Fe2 S1 162.21(9) . . ?
C4 Fe2 S2 158.9(2) . . ?
C3 Fe2 S2 103.2(3) . . ?
P2 Fe2 S2 86.72(8) . . ?
S1 Fe2 S2 77.10(8) . . ?
C4 Fe2 Fe1 106.9(2) . . ?
C3 Fe2 Fe1 143.9(3) . . ?
P2 Fe2 Fe1 109.88(7) . . ?
S1 Fe2 Fe1 54.51(6) . . ?
S2 Fe2 Fe1 55.20(6) . . ?
C5 S1 Fe1 108.1(3) . . ?
C5 S1 Fe2 116.6(3) . . ?
Fe1 S1 Fe2 70.43(7) . . ?
C19 S2 Fe2 106.4(3) . . ?
C19 S2 Fe1 113.5(3) . . ?
Fe2 S2 Fe1 69.87(7) . . ?
C7 P1 C13 101.6(4) . . ?
C7 P1 C6 105.1(4) . . ?
C13 P1 C6 104.0(4) . . ?
C7 P1 Fe1 115.2(3) . . ?
C13 P1 Fe1 121.2(2) . . ?
C6 P1 Fe1 108.2(3) . . ?
C27 P2 C21 101.4(3) . . ?
C27 P2 C20 103.1(4) . . ?
C21 P2 C20 105.8(3) . . ?
C27 P2 Fe2 123.1(3) . . ?
C21 P2 Fe2 115.1(2) . . ?
C20 P2 Fe2 106.7(3) . . ?
O1 C1 Fe1 176.5(8) . . ?
O2 C2 Fe1 175.7(7) . . ?
O3 C3 Fe2 175.2(8) . . ?
O4 C4 Fe2 174.7(7) . . ?
C6 C5 S1 112.9(5) . . ?
C5 C6 P1 108.7(5) . . ?
C8 C7 C12 118.1(7) . . ?
C8 C7 P1 123.9(6) . . ?
C12 C7 P1 118.0(6) . . ?
C7 C8 C9 121.1(8) . . ?
C10 C9 C8 120.8(9) . . ?
C9 C10 C11 118.6(8) . . ?
C10 C11 C12 120.2(9) . . ?
C7 C12 C11 121.1(8) . . ?
C14 C13 C18 117.5(7) . . ?
C14 C13 P1 121.7(6) . . ?
C18 C13 P1 120.7(6) . . ?
C15 C14 C13 121.4(8) . . ?
C16 C15 C14 121.0(9) . . ?
C15 C16 C17 118.9(8) . . ?
C16 C17 C18 120.7(9) . . ?
C13 C18 C17 120.4(8) . . ?
C20 C19 S2 108.9(5) . . ?
C19 C20 P2 107.1(5) . . ?
C22 C21 C26 119.6(7) . . ?
C22 C21 P2 120.9(6) . . ?
C26 C21 P2 119.4(6) . . ?
C21 C22 C23 120.3(8) . . ?
C24 C23 C22 120.2(8) . . ?
C23 C24 C25 120.2(8) . . ?
C24 C25 C26 120.3(7) . . ?
C25 C26 C21 119.4(8) . . ?
C28 C27 C32 117.9(8) . . ?
C28 C27 P2 121.4(6) . . ?
C32 C27 P2 120.6(7) . . ?
C27 C28 C29 119.9(9) . . ?
C30 C29 C28 122.0(9) . . ?
C29 C30 C31 118.4(8) . . ?
C30 C31 C32 119.8(9) . . ?
C31 C32 C27 121.9(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C2 1.753(8) . ?
Fe1 C1 1.780(8) . ?
Fe1 P1 2.211(2) . ?
Fe1 S1 2.250(2) . ?
Fe1 S2 2.277(2) . ?
Fe1 Fe2 2.6032(18) . ?
Fe2 C4 1.753(8) . ?
Fe2 C3 1.785(9) . ?
Fe2 P2 2.207(2) . ?
Fe2 S1 2.265(2) . ?
Fe2 S2 2.269(2) . ?
S1 C5 1.820(8) . ?
S2 C19 1.824(8) . ?
P1 C7 1.836(8) . ?
P1 C13 1.841(8) . ?
P1 C6 1.844(8) . ?
P2 C27 1.838(8) . ?
P2 C21 1.838(8) . ?
P2 C20 1.839(8) . ?
O1 C1 1.147(9) . ?
O2 C2 1.159(9) . ?
O3 C3 1.150(9) . ?
O4 C4 1.179(9) . ?
C5 C6 1.511(11) . ?
C7 C8 1.381(11) . ?
C7 C12 1.386(11) . ?
C8 C9 1.379(11) . ?
C9 C10 1.383(13) . ?
C10 C11 1.385(13) . ?
C11 C12 1.388(11) . ?
C13 C14 1.385(11) . ?
C13 C18 1.384(11) . ?
C14 C15 1.379(11) . ?
C15 C16 1.353(13) . ?
C16 C17 1.376(13) . ?
C17 C18 1.393(11) . ?
C19 C20 1.520(10) . ?
C21 C22 1.376(10) . ?
C21 C26 1.401(10) . ?
C22 C23 1.390(11) . ?
C23 C24 1.372(11) . ?
C24 C25 1.376(12) . ?
C25 C26 1.391(11) . ?
C27 C28 1.373(11) . ?
C27 C32 1.380(11) . ?
C28 C29 1.383(11) . ?
C29 C30 1.360(12) . ?
C30 C31 1.377(13) . ?
C31 C32 1.376(12) . ?
