#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:39:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179255 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/75/4317546.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_4317546
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            'C31 H28 Fe O3 P2 S2'
_chemical_formula_weight         630.44
_chemical_name_systematic
;

   ?

;
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0409P)²+1.9188P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.08229(4) 0.222444(19) 0.149999(13) 0.02114(10) Uani 1 1 d . . .
Fe2 Fe 0.08615(4) 0.179259(19) 0.048705(12) 0.01954(10) Uani 1 1 d . . .
S1 S -0.10999(7) 0.14046(4) 0.10346(2) 0.02443(14) Uani 1 1 d . . .
S2 S 0.25362(7) 0.12707(3) 0.11834(2) 0.02156(13) Uani 1 1 d . . .
P1 P 0.05406(7) 0.14998(3) 0.22559(2) 0.02085(13) Uani 1 1 d . . .
P2 P 0.30875(7) 0.23581(4) 0.01936(2) 0.02191(14) Uani 1 1 d . . .
C1 C -0.0631(4) 0.30359(17) 0.14722(10) 0.0391(6) Uani 1 1 d . . .
O1 O -0.1561(3) 0.35711(15) 0.14527(9) 0.0726(8) Uani 1 1 d . . .
C2 C 0.2400(4) 0.28835(17) 0.17701(11) 0.0391(6) Uani 1 1 d . . .
O2 O 0.3408(3) 0.33210(16) 0.19675(11) 0.0746(8) Uani 1 1 d . . .
C3 C -0.0533(3) 0.25781(15) 0.02405(9) 0.0262(5) Uani 1 1 d . . .
O3 O -0.1483(2) 0.30776(12) 0.00968(7) 0.0380(4) Uani 1 1 d . . .
C4 C 0.0524(3) 0.10855(15) -0.00711(10) 0.0286(5) Uani 1 1 d . . .
O4 O 0.0229(3) 0.06508(12) -0.04406(8) 0.0474(5) Uani 1 1 d . . .
C5 C -0.0831(3) 0.04472(14) 0.14376(10) 0.0274(5) Uani 1 1 d . . .
H5A H 0.0234 0.0210 0.1401 0.080 Uiso 1 1 d R . .
H5B H -0.1672 0.0058 0.1309 0.080 Uiso 1 1 d R . .
C6 C -0.0954(3) 0.06767(15) 0.20414(10) 0.0271(5) Uani 1 1 d . . .
H6A H -0.2056 0.0866 0.2079 0.080 Uiso 1 1 d R . .
H6B H -0.0739 0.0206 0.2276 0.080 Uiso 1 1 d R . .
C7 C 0.2661(4) 0.01423(17) 0.25150(11) 0.0396(6) Uani 1 1 d . . .
H7A H 0.1766 -0.0197 0.2358 0.080 Uiso 1 1 d R . .
C8 C 0.4174(4) -0.0206(2) 0.27062(13) 0.0505(8) Uani 1 1 d . . .
H8A H 0.4315 -0.0789 0.2679 0.080 Uiso 1 1 d R . .
C9 C 0.5460(4) 0.0274(2) 0.29307(12) 0.0495(8) Uani 1 1 d . . .
H9A H 0.6504 0.0026 0.3059 0.080 Uiso 1 1 d R . .
C10 C 0.5248(3) 0.1116(2) 0.29704(13) 0.0485(7) Uani 1 1 d . . .
H10A H 0.6136 0.1455 0.3133 0.080 Uiso 1 1 d R . .
C11 C 0.3742(3) 0.14674(17) 0.27780(11) 0.0374(6) Uani 1 1 d . . .
H11A H 0.3593 0.2050 0.2803 0.080 Uiso 1 1 d R . .
C12 C 0.2434(3) 0.09862(15) 0.25467(9) 0.0255(5) Uani 1 1 d . . .
C13 C -0.0126(3) 0.14759(16) 0.33665(10) 0.0307(5) Uani 1 1 d . . .
H13A H 0.0429 0.0955 0.3386 0.080 Uiso 1 1 d R . .
C14 C -0.0807(3) 0.17810(17) 0.38256(10) 0.0358(6) Uani 1 1 d . . .
H14A H -0.0741 0.1468 0.4162 0.080 Uiso 1 1 d R . .
C15 C -0.1586(4) 0.25349(18) 0.37992(11) 0.0391(6) Uani 1 1 d . . .
H15A H -0.2081 0.2738 0.4114 0.080 Uiso 1 1 d R . .
C16 C -0.1670(4) 0.29881(19) 0.33209(12) 0.0510(8) Uani 1 1 d . . .
H16A H -0.2168 0.3523 0.3310 0.080 Uiso 1 1 d R . .
C17 C -0.0998(4) 0.26831(17) 0.28590(11) 0.0433(7) Uani 1 1 d . . .
H17A H -0.1077 0.2996 0.2522 0.080 Uiso 1 1 d R . .
C18 C -0.0241(3) 0.19219(14) 0.28756(9) 0.0252(5) Uani 1 1 d . . .
C19 C 0.4646(3) 0.16561(16) 0.11578(10) 0.0304(5) Uani 1 1 d . . .
H19A H 0.5308 0.1226 0.1026 0.080 Uiso 1 1 d R . .
H19B H 0.5112 0.1797 0.1526 0.080 Uiso 1 1 d R . .
C20 C 0.4719(3) 0.23974(15) 0.07811(10) 0.0292(5) Uani 1 1 d . . .
H20A H 0.4588 0.2887 0.0992 0.080 Uiso 1 1 d R . .
H20B H 0.5782 0.2421 0.0643 0.080 Uiso 1 1 d R . .
C21 C 0.3771(4) 0.36735(16) -0.05177(11) 0.0380(6) Uani 1 1 d . . .
H21A H 0.4351 0.3282 -0.0721 0.080 Uiso 1 1 d R . .
C22 C 0.3689(4) 0.44925(18) -0.06824(12) 0.0489(8) Uani 1 1 d . . .
H22A H 0.4190 0.4665 -0.1004 0.080 Uiso 1 1 d R . .
C23 C 0.2901(4) 0.50580(17) -0.03824(13) 0.0479(7) Uani 1 1 d . . .
H23A H 0.2827 0.5620 -0.0501 0.080 Uiso 1 1 d R . .
C24 C 0.2198(4) 0.48205(17) 0.00794(14) 0.0488(8) Uani 1 1 d . . .
H24A H 0.1662 0.5220 0.0290 0.080 Uiso 1 1 d R . .
C25 C 0.2250(3) 0.40003(16) 0.02429(12) 0.0384(6) Uani 1 1 d . . .
H25A H 0.1764 0.3834 0.0569 0.080 Uiso 1 1 d R . .
C26 C 0.3040(3) 0.34180(14) -0.00572(10) 0.0268(5) Uani 1 1 d . . .
C27 C 0.3139(3) 0.17829(15) -0.08890(10) 0.0320(6) Uani 1 1 d . . .
H27A H 0.2192 0.2131 -0.0973 0.080 Uiso 1 1 d R . .
C28 C 0.3699(4) 0.12967(16) -0.13003(11) 0.0389(6) Uani 1 1 d . . .
H28A H 0.3162 0.1325 -0.1672 0.080 Uiso 1 1 d R . .
C29 C 0.5032(4) 0.07750(16) -0.11776(13) 0.0420(7) Uani 1 1 d . . .
H29A H 0.5399 0.0429 -0.1460 0.080 Uiso 1 1 d R . .
C30 C 0.5829(3) 0.07512(17) -0.06470(13) 0.0421(7) Uani 1 1 d . . .
H30A H 0.6753 0.0389 -0.0561 0.080 Uiso 1 1 d R . .
C31 C 0.5309(3) 0.12526(16) -0.02335(11) 0.0344(6) Uani 1 1 d . . .
H31A H 0.5877 0.1238 0.0134 0.080 Uiso 1 1 d R . .
C32 C 0.3947(3) 0.17695(14) -0.03495(10) 0.0264(5) Uani 1 1 d . . .
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'
P P 0.1023 0.0942 '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'
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 90.84(14) . . ?
C2 Fe1 P1 98.83(9) . . ?
C1 Fe1 P1 107.58(9) . . ?
C2 Fe1 S1 172.10(9) . . ?
C1 Fe1 S1 90.00(10) . . ?
P1 Fe1 S1 88.40(3) . . ?
C2 Fe1 S2 95.54(10) . . ?
C1 Fe1 S2 158.11(8) . . ?
P1 Fe1 S2 92.14(3) . . ?
S1 Fe1 S2 80.93(3) . . ?
C2 Fe1 Fe2 116.49(9) . . ?
C1 Fe1 Fe2 104.21(8) . . ?
P1 Fe1 Fe2 131.47(3) . . ?
S1 Fe1 Fe2 55.75(2) . . ?
S2 Fe1 Fe2 54.33(2) . . ?
C3 Fe2 C4 99.78(11) . . ?
C3 Fe2 P2 96.04(8) . . ?
C4 Fe2 P2 95.10(8) . . ?
C3 Fe2 S2 148.34(8) . . ?
C4 Fe2 S2 111.34(8) . . ?
P2 Fe2 S2 87.12(3) . . ?
C3 Fe2 S1 86.31(7) . . ?
C4 Fe2 S1 101.86(8) . . ?
P2 Fe2 S1 162.25(3) . . ?
S2 Fe2 S1 81.87(3) . . ?
C3 Fe2 Fe1 93.03(7) . . ?
C4 Fe2 Fe1 153.30(8) . . ?
P2 Fe2 Fe1 106.80(3) . . ?
S2 Fe2 Fe1 56.22(2) . . ?
S1 Fe2 Fe1 55.45(2) . . ?
C5 S1 Fe1 101.44(8) . . ?
C5 S1 Fe2 119.73(8) . . ?
Fe1 S1 Fe2 68.80(2) . . ?
C19 S2 Fe2 109.96(8) . . ?
C19 S2 Fe1 112.68(9) . . ?
Fe2 S2 Fe1 69.45(2) . . ?
C12 P1 C18 101.91(10) . . ?
C12 P1 C6 106.11(11) . . ?
C18 P1 C6 103.27(11) . . ?
C12 P1 Fe1 114.03(8) . . ?
C18 P1 Fe1 123.87(8) . . ?
C6 P1 Fe1 106.07(8) . . ?
C32 P2 C26 104.53(11) . . ?
C32 P2 C20 106.15(11) . . ?
C26 P2 C20 102.29(11) . . ?
C32 P2 Fe2 113.70(8) . . ?
C26 P2 Fe2 120.72(8) . . ?
C20 P2 Fe2 108.06(8) . . ?
O1 C1 Fe1 179.1(3) . . ?
O2 C2 Fe1 177.2(3) . . ?
O3 C3 Fe2 177.1(2) . . ?
O4 C4 Fe2 176.3(2) . . ?
C6 C5 S1 106.65(16) . . ?
C5 C6 P1 109.88(15) . . ?
C8 C7 C12 120.3(3) . . ?
C9 C8 C7 120.6(3) . . ?
C8 C9 C10 119.8(3) . . ?
C11 C10 C9 119.8(3) . . ?
C10 C11 C12 120.8(3) . . ?
C7 C12 C11 118.7(2) . . ?
C7 C12 P1 122.9(2) . . ?
C11 C12 P1 118.26(19) . . ?
C14 C13 C18 120.4(2) . . ?
C15 C14 C13 120.1(2) . . ?
C16 C15 C14 120.0(2) . . ?
C15 C16 C17 120.2(3) . . ?
C18 C17 C16 120.6(2) . . ?
C17 C18 C13 118.8(2) . . ?
C17 C18 P1 120.37(18) . . ?
C13 C18 P1 120.77(18) . . ?
C20 C19 S2 112.93(16) . . ?
C19 C20 P2 111.55(16) . . ?
C26 C21 C22 120.6(3) . . ?
C23 C22 C21 120.1(3) . . ?
C24 C23 C22 120.3(3) . . ?
C23 C24 C25 120.2(3) . . ?
C24 C25 C26 120.4(3) . . ?
C21 C26 C25 118.6(2) . . ?
C21 C26 P2 123.82(19) . . ?
C25 C26 P2 117.57(19) . . ?
C28 C27 C32 120.5(2) . . ?
C29 C28 C27 120.3(3) . . ?
C30 C29 C28 119.8(2) . . ?
C29 C30 C31 120.5(3) . . ?
C30 C31 C32 120.2(3) . . ?
C31 C32 C27 118.7(2) . . ?
C31 C32 P2 121.79(19) . . ?
C27 C32 P2 119.28(18) . . ?
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 1.745(3) . ?
Fe1 C1 1.770(3) . ?
Fe1 P1 2.2153(8) . ?
Fe1 S1 2.2635(8) . ?
Fe1 S2 2.2745(7) . ?
Fe1 Fe2 2.5621(7) . ?
Fe2 C3 1.771(2) . ?
Fe2 C4 1.778(2) . ?
Fe2 P2 2.2142(8) . ?
Fe2 S2 2.2229(8) . ?
Fe2 S1 2.2716(8) . ?
S1 C5 1.842(2) . ?
S2 C19 1.833(2) . ?
P1 C12 1.826(2) . ?
P1 C18 1.829(2) . ?
P1 C6 1.846(2) . ?
P2 C32 1.829(2) . ?
P2 C26 1.831(2) . ?
P2 C20 1.842(2) . ?
C1 O1 1.151(3) . ?
C2 O2 1.151(3) . ?
C3 O3 1.149(3) . ?
C4 O4 1.148(3) . ?
C5 C6 1.527(3) . ?
C7 C8 1.388(4) . ?
C7 C12 1.391(4) . ?
C8 C9 1.371(5) . ?
C9 C10 1.388(5) . ?
C10 C11 1.386(4) . ?
C11 C12 1.389(4) . ?
C13 C14 1.389(3) . ?
C13 C18 1.391(3) . ?
C14 C15 1.380(4) . ?
C15 C16 1.372(4) . ?
C16 C17 1.391(4) . ?
C17 C18 1.383(4) . ?
C19 C20 1.520(3) . ?
C21 C26 1.385(4) . ?
C21 C22 1.393(4) . ?
C22 C23 1.375(4) . ?
C23 C24 1.368(4) . ?
C24 C25 1.394(4) . ?
C25 C26 1.394(4) . ?
C27 C28 1.389(4) . ?
C27 C32 1.401(3) . ?
C28 C29 1.384(4) . ?
C29 C30 1.379(4) . ?
C30 C31 1.395(4) . ?
C31 C32 1.395(3) . ?
