#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:21:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179106 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/68/4306879.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_4306879
loop_
_publ_author_name
'Weiming Gao'
'Jesper Ekström'
'Jianhui Liu'
'Changneng Chen'
'Lars Eriksson'
'Linhong Weng'
'Björn Åkermark'
'Licheng Sun'
_publ_section_title
;
Binuclear Iron-Sulfur Complexes with Bidentate Phosphine Ligands as
Active Site Models of Fe-Hydrogenase and Their Catalytic Proton Reduction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1981
_journal_page_last               1991
_journal_paper_doi               10.1021/ic0610278
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C46 H46 Fe4 N2 O10 P2 S4'
_chemical_formula_weight         1200.43
_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                104.3780(10)
_cell_angle_beta                 93.1110(10)
_cell_angle_gamma                118.5390(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9583(2)
_cell_length_b                   11.2692(2)
_cell_length_c                   12.8333(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1320.50(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6825
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.350
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             614
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0754P)²+3.0214P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                4261
_reflns_number_total             4572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0610278si20060609_025154.cif
_cod_data_source_block           m
_cod_original_cell_volume        1320.49(5)
_cod_database_code               4306879
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 0.64482(6) 0.29256(6) 0.35034(5) 0.03174(18) Uani 1 1 d . . .
Fe2 Fe 0.52345(6) 0.28576(7) 0.17554(5) 0.0387(2) Uani 1 1 d . . .
S1 S 0.58228(12) 0.12189(12) 0.18764(9) 0.0428(3) Uani 1 1 d . . .
S2 S 0.75498(12) 0.44421(12) 0.25456(9) 0.0405(3) Uani 1 1 d . . .
P1 P 0.81259(10) 0.27856(10) 0.44419(8) 0.0285(2) Uani 1 1 d . . .
O1 O 0.4605(5) 0.5107(5) 0.2661(5) 0.0864(14) Uani 1 1 d . . .
O2 O 0.2294(5) 0.0711(5) 0.1624(5) 0.0952(17) Uani 1 1 d . . .
O3 O 0.5092(7) 0.2827(8) -0.0535(4) 0.122(2) Uani 1 1 d . . .
O4 O 0.3990(5) 0.0948(5) 0.4195(4) 0.0908(16) Uani 1 1 d . . .
O5 O 0.6604(4) 0.5389(4) 0.5083(3) 0.0651(10) Uani 1 1 d . . .
N1 N 0.8675(4) 0.2740(5) 0.1812(3) 0.0494(10) Uani 1 1 d . . .
C1 C 0.4862(5) 0.4241(6) 0.2298(5) 0.0520(12) Uani 1 1 d . . .
C2 C 0.3449(6) 0.1553(6) 0.1670(5) 0.0563(13) Uani 1 1 d . . .
C3 C 0.5176(6) 0.2837(7) 0.0347(5) 0.0649(15) Uani 1 1 d . . .
C4 C 0.4960(5) 0.1707(5) 0.3931(4) 0.0494(12) Uani 1 1 d . . .
C5 C 0.6538(5) 0.4408(5) 0.4483(4) 0.0416(10) Uani 1 1 d . . .
C6 C 0.7349(5) 0.1443(6) 0.1248(4) 0.0524(12) Uani 1 1 d . . .
H6A H 0.7472 0.0639 0.1219 0.063 Uiso 1 1 calc R . .
H6B H 0.7140 0.1424 0.0498 0.063 Uiso 1 1 calc R . .
C7 C 0.8676(5) 0.3992(6) 0.1734(4) 0.0508(12) Uani 1 1 d . . .
H7A H 0.8362 0.3853 0.0969 0.061 Uiso 1 1 calc R . .
H7B H 0.9641 0.4790 0.1972 0.061 Uiso 1 1 calc R . .
C8 C 0.9948(6) 0.2707(7) 0.1491(4) 0.0616(14) Uani 1 1 d . . .
H8A H 0.9892 0.1845 0.1561 0.074 Uiso 1 1 calc R . .
H8B H 1.0783 0.3505 0.2011 0.074 Uiso 1 1 calc R . .
C9 C 1.0157(7) 0.2761(9) 0.0344(5) 0.079(2) Uani 1 1 d . . .
H9A H 0.9338 0.1955 -0.0186 0.095 Uiso 1 1 calc R . .
H9B H 1.0218 0.3620 0.0264 0.095 Uiso 1 1 calc R . .
C10 C 1.1492(9) 0.2737(14) 0.0089(7) 0.132(4) Uani 1 1 d . . .
H10A H 1.1560 0.2741 -0.0653 0.198 Uiso 1 1 calc R . .
H10B H 1.1443 0.1894 0.0175 0.198 Uiso 1 1 calc R . .
H10C H 1.2312 0.3561 0.0585 0.198 Uiso 1 1 calc R . .
C11 C 0.8309(5) 0.1231(4) 0.3869(3) 0.0345(9) Uani 1 1 d . . .
C12 C 0.7095(5) -0.0105(5) 0.3586(5) 0.0512(12) Uani 1 1 d . . .
H12A H 0.6218 -0.0182 0.3636 0.061 Uiso 1 1 calc R . .
C13 C 0.7178(6) -0.1316(6) 0.3234(6) 0.0671(16) Uani 1 1 d . . .
H13A H 0.6359 -0.2203 0.3062 0.081 Uiso 1 1 calc R . .
C14 C 0.8457(7) -0.1230(6) 0.3133(5) 0.0653(15) Uani 1 1 d . . .
H14A H 0.8503 -0.2055 0.2890 0.078 Uiso 1 1 calc R . .
C15 C 0.9678(6) 0.0091(6) 0.3394(5) 0.0643(15) Uani 1 1 d . . .
H15A H 1.0547 0.0157 0.3323 0.077 Uiso 1 1 calc R . .
C16 C 0.9602(5) 0.1314(5) 0.3760(4) 0.0499(12) Uani 1 1 d . . .
H16A H 1.0423 0.2200 0.3935 0.060 Uiso 1 1 calc R . .
C17 C 0.7958(4) 0.2698(4) 0.5845(3) 0.0334(9) Uani 1 1 d . . .
C18 C 0.8755(5) 0.2290(5) 0.6390(4) 0.0421(10) Uani 1 1 d . . .
H18A H 0.9377 0.2070 0.6042 0.050 Uiso 1 1 calc R . .
C19 C 0.8634(5) 0.2210(6) 0.7435(4) 0.0491(11) Uani 1 1 d . . .
H19A H 0.9181 0.1942 0.7787 0.059 Uiso 1 1 calc R . .
C20 C 0.7713(6) 0.2520(6) 0.7968(4) 0.0523(12) Uani 1 1 d . . .
H20A H 0.7620 0.2442 0.8667 0.063 Uiso 1 1 calc R . .
C21 C 0.6933(6) 0.2948(7) 0.7450(4) 0.0582(14) Uani 1 1 d . . .
H21A H 0.6320 0.3175 0.7806 0.070 Uiso 1 1 calc R . .
C22 C 0.7058(5) 0.3042(6) 0.6396(4) 0.0460(11) Uani 1 1 d . . .
H22A H 0.6531 0.3339 0.6056 0.055 Uiso 1 1 calc R . .
C23 C 0.9946(4) 0.4291(4) 0.4695(3) 0.0296(8) Uani 1 1 d . . .
H23A H 1.0584 0.4143 0.5129 0.035 Uiso 1 1 calc R . .
H23B H 1.0240 0.4334 0.4000 0.035 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'
N N 0.0061 0.0033 '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
C5 Fe1 C4 91.6(2) . . ?
C5 Fe1 P1 98.85(15) . . ?
C4 Fe1 P1 97.97(17) . . ?
C5 Fe1 S2 85.93(15) . . ?
C4 Fe1 S2 155.25(17) . . ?
P1 Fe1 S2 106.75(4) . . ?
C5 Fe1 S1 158.37(15) . . ?
C4 Fe1 S1 89.27(17) . . ?
P1 Fe1 S1 102.43(4) . . ?
S2 Fe1 S1 84.27(5) . . ?
C5 Fe1 Fe2 102.35(15) . . ?
C4 Fe1 Fe2 100.35(16) . . ?
P1 Fe1 Fe2 151.42(4) . . ?
S2 Fe1 Fe2 56.47(3) . . ?
S1 Fe1 Fe2 56.31(4) . . ?
C2 Fe2 C3 100.1(3) . . ?
C2 Fe2 C1 90.6(3) . . ?
C3 Fe2 C1 100.0(3) . . ?
C2 Fe2 S1 87.30(18) . . ?
C3 Fe2 S1 105.6(2) . . ?
C1 Fe2 S1 154.29(18) . . ?
C2 Fe2 S2 157.08(19) . . ?
C3 Fe2 S2 102.6(2) . . ?
C1 Fe2 S2 88.05(17) . . ?
S1 Fe2 S2 84.15(5) . . ?
C2 Fe2 Fe1 101.52(18) . . ?
C3 Fe2 Fe1 150.72(19) . . ?
C1 Fe2 Fe1 99.25(17) . . ?
S1 Fe2 Fe1 56.31(3) . . ?
S2 Fe2 Fe1 56.26(3) . . ?
C6 S1 Fe2 111.51(19) . . ?
C6 S1 Fe1 112.35(17) . . ?
Fe2 S1 Fe1 67.38(4) . . ?
C7 S2 Fe1 113.15(18) . . ?
C7 S2 Fe2 109.67(18) . . ?
Fe1 S2 Fe2 67.27(4) . . ?
C11 P1 C23 103.32(18) . . ?
C11 P1 C17 100.14(19) . . ?
C23 P1 C17 101.03(18) . . ?
C11 P1 Fe1 117.14(14) . . ?
C23 P1 Fe1 115.90(13) . . ?
C17 P1 Fe1 116.74(14) . . ?
C7 N1 C6 112.6(4) . . ?
C7 N1 C8 111.9(4) . . ?
C6 N1 C8 113.5(4) . . ?
O1 C1 Fe2 178.3(5) . . ?
O2 C2 Fe2 179.4(5) . . ?
O3 C3 Fe2 177.3(6) . . ?
O4 C4 Fe1 177.9(5) . . ?
O5 C5 Fe1 177.3(4) . . ?
N1 C6 S1 114.9(3) . . ?
N1 C6 H6A 108.5 . . ?
S1 C6 H6A 108.5 . . ?
N1 C6 H6B 108.5 . . ?
S1 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
N1 C7 S2 114.3(3) . . ?
N1 C7 H7A 108.7 . . ?
S2 C7 H7A 108.7 . . ?
N1 C7 H7B 108.7 . . ?
S2 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
N1 C8 C9 116.2(5) . . ?
N1 C8 H8A 108.2 . . ?
C9 C8 H8A 108.2 . . ?
N1 C8 H8B 108.2 . . ?
C9 C8 H8B 108.2 . . ?
H8A C8 H8B 107.4 . . ?
C10 C9 C8 112.6(6) . . ?
C10 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 118.4(4) . . ?
C12 C11 P1 117.8(3) . . ?
C16 C11 P1 123.6(3) . . ?
C13 C12 C11 120.7(5) . . ?
C13 C12 H12A 119.7 . . ?
C11 C12 H12A 119.7 . . ?
C12 C13 C14 120.7(5) . . ?
C12 C13 H13A 119.6 . . ?
C14 C13 H13A 119.6 . . ?
C15 C14 C13 119.6(5) . . ?
C15 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
C14 C15 C16 119.9(5) . . ?
C14 C15 H15A 120.1 . . ?
C16 C15 H15A 120.1 . . ?
C11 C16 C15 120.7(5) . . ?
C11 C16 H16A 119.7 . . ?
C15 C16 H16A 119.7 . . ?
C18 C17 C22 118.0(4) . . ?
C18 C17 P1 120.1(3) . . ?
C22 C17 P1 121.9(3) . . ?
C19 C18 C17 120.9(4) . . ?
C19 C18 H18A 119.6 . . ?
C17 C18 H18A 119.6 . . ?
C18 C19 C20 120.9(4) . . ?
C18 C19 H19A 119.5 . . ?
C20 C19 H19A 119.5 . . ?
C21 C20 C19 119.1(4) . . ?
C21 C20 H20A 120.5 . . ?
C19 C20 H20A 120.5 . . ?
C20 C21 C22 120.4(4) . . ?
C20 C21 H21A 119.8 . . ?
C22 C21 H21A 119.8 . . ?
C21 C22 C17 120.8(4) . . ?
C21 C22 H22A 119.6 . . ?
C17 C22 H22A 119.6 . . ?
C23 C23 P1 111.5(3) 2_766 . ?
C23 C23 H23A 109.3 2_766 . ?
P1 C23 H23A 109.3 . . ?
C23 C23 H23B 109.3 2_766 . ?
P1 C23 H23B 109.3 . . ?
H23A C23 H23B 108.0 . . ?
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 C5 1.780(5) . ?
Fe1 C4 1.783(5) . ?
Fe1 P1 2.2330(11) . ?
Fe1 S2 2.2632(12) . ?
Fe1 S1 2.2626(13) . ?
Fe1 Fe2 2.5101(8) . ?
Fe2 C2 1.774(6) . ?
Fe2 C3 1.799(6) . ?
Fe2 C1 1.784(5) . ?
Fe2 S1 2.2625(13) . ?
Fe2 S2 2.2686(13) . ?
S1 C6 1.832(5) . ?
S2 C7 1.828(5) . ?
P1 C11 1.833(4) . ?
P1 C23 1.840(4) . ?
P1 C17 1.842(4) . ?
O1 C1 1.139(6) . ?
O2 C2 1.150(7) . ?
O3 C3 1.129(7) . ?
O4 C4 1.136(6) . ?
O5 C5 1.147(6) . ?
N1 C7 1.439(7) . ?
N1 C6 1.450(7) . ?
N1 C8 1.491(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.514(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.527(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.390(6) . ?
C11 C16 1.392(6) . ?
C12 C13 1.375(7) . ?
C12 H12A 0.9300 . ?
C13 C14 1.374(8) . ?
C13 H13A 0.9300 . ?
C14 C15 1.386(8) . ?
C14 H14A 0.9300 . ?
C15 C16 1.386(7) . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
C17 C18 1.392(6) . ?
C17 C22 1.388(6) . ?
C18 C19 1.376(7) . ?
C18 H18A 0.9300 . ?
C19 C20 1.379(7) . ?
C19 H19A 0.9300 . ?
C20 C21 1.377(7) . ?
C20 H20A 0.9300 . ?
C21 C22 1.392(7) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9300 . ?
C23 C23 1.539(7) 2_766 ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
