#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/22/7012292.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_7012292
loop_
_publ_author_name
'Razavet, Mathieu'
'Davies, Sian C.'
'Hughes, David L.'
'Barclay, J. Elaine'
'Evans, David J.'
'Fairhurst, Shirley A.'
'Liu, Xiaoming'
'Pickett, Christopher J.'
_publ_section_title
;
 All-iron hydrogenase: synthesis, structure and properties of
 {2Fe3S}-assemblies related to the di-iron sub-site of the
 H-clusterElectronic supplementary information (ESI) available: crystal
 and structure refinement data for complexes 4a, 4b and 5a. See
 http://www.rsc.org/suppdata/dt/b2/b209690k/
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              586
_journal_paper_doi               10.1039/b209690k
_journal_year                    2003
_chemical_formula_moiety         'C17 H16 Fe2 O5 S3'
_chemical_formula_structural     '[Fe2(CO)5{PhCH2SCH2C(Me)(CH2S)2}]'
_chemical_formula_sum            'C17 H16 Fe2 O5 S3'
_chemical_formula_weight         508.18
_chemical_name_common            'Compound 4b'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                110.555(10)
_cell_angle_beta                 92.983(9)
_cell_angle_gamma                104.374(9)
_cell_formula_units_Z            2
_cell_length_a                   9.8755(11)
_cell_length_b                   11.3853(13)
_cell_length_c                   10.3912(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     1047.2(2)
_computing_cell_refinement       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_reduction        'CAD4 (Hursthouse, 1976)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'scintillation counter; ω/θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4297
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.708
_exptl_absorpt_correction_T_max  0.30
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated plates'
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0373
_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)+(0.0579P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.1047
_reflns_number_gt                2715
_reflns_number_total             3686
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b209690k.txt
_cod_data_source_block           math5
_cod_database_code               7012292
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 0.22416(5) 0.09208(5) 0.24546(5) 0.05051(17) Uani 1 1 d . . .
Fe2 Fe 0.48554(5) 0.19468(5) 0.29537(5) 0.04454(16) Uani 1 1 d . . .
S1 S 0.37303(10) 0.05117(8) 0.38571(9) 0.0482(2) Uani 1 1 d . . .
C1 C 0.3646(4) 0.1343(4) 0.5688(4) 0.0539(9) Uani 1 1 d . . .
H1A H 0.2664 0.1109 0.5819 0.065 Uiso 1 1 calc R . .
H1B H 0.4159 0.0995 0.6218 0.065 Uiso 1 1 calc R . .
S2 S 0.32786(11) 0.30558(9) 0.37748(9) 0.0519(2) Uani 1 1 d . . .
C2 C 0.3345(5) 0.3442(4) 0.5646(4) 0.0624(11) Uani 1 1 d . . .
H2A H 0.3715 0.4384 0.6116 0.075 Uiso 1 1 calc R . .
H2B H 0.2382 0.3199 0.5826 0.075 Uiso 1 1 calc R . .
S3 S 0.64995(10) 0.33229(8) 0.47697(9) 0.0480(2) Uani 1 1 d . . .
C3 C 0.5790(4) 0.3316(5) 0.6352(4) 0.0697(12) Uani 1 1 d . . .
H3A H 0.6238 0.2803 0.6712 0.084 Uiso 1 1 calc R . .
H3B H 0.6101 0.4208 0.7028 0.084 Uiso 1 1 calc R . .
C31 C 0.7950(4) 0.2647(4) 0.4911(4) 0.0612(10) Uani 1 1 d . . .
H31A H 0.7573 0.1772 0.4903 0.073 Uiso 1 1 calc R . .
H31B H 0.8424 0.2574 0.4104 0.073 Uiso 1 1 calc R . .
C311 C 0.9014(4) 0.3455(4) 0.6204(4) 0.0537(9) Uani 1 1 d . . .
C312 C 0.9597(5) 0.4791(4) 0.6583(5) 0.0740(12) Uani 1 1 d . . .
H312 H 0.9324 0.5210 0.6033 0.089 Uiso 1 1 calc R . .
C313 C 1.0581(5) 0.5506(5) 0.7774(5) 0.0860(15) Uani 1 1 d . . .
H313 H 1.0963 0.6403 0.8024 0.103 Uiso 1 1 calc R . .
C314 C 1.0994(5) 0.4899(6) 0.8582(5) 0.0812(14) Uani 1 1 d . . .
H314 H 1.1679 0.5376 0.9364 0.097 Uiso 1 1 calc R . .
C315 C 1.0409(5) 0.3608(6) 0.8246(5) 0.0837(14) Uani 1 1 d . . .
H315 H 1.0663 0.3202 0.8818 0.100 Uiso 1 1 calc R . .
C316 C 0.9425(4) 0.2881(5) 0.7046(5) 0.0683(11) Uani 1 1 d . . .
H316 H 0.9041 0.1987 0.6814 0.082 Uiso 1 1 calc R . .
C4 C 0.4207(4) 0.2814(4) 0.6316(3) 0.0517(9) Uani 1 1 d . . .
C41 C 0.3999(5) 0.3225(5) 0.7870(4) 0.0739(13) Uani 1 1 d . . .
H41A H 0.4293 0.4163 0.8309 0.111 Uiso 1 1 calc R . .
H41B H 0.4555 0.2867 0.8333 0.111 Uiso 1 1 calc R . .
H41C H 0.3018 0.2901 0.7927 0.111 Uiso 1 1 calc R . .
C13 C 0.0604(5) 0.0553(4) 0.3073(5) 0.0707(12) Uani 1 1 d . . .
O13 O -0.0452(4) 0.0306(4) 0.3465(5) 0.1119(13) Uani 1 1 d . . .
C14 C 0.1721(5) 0.1447(5) 0.1128(5) 0.0766(13) Uani 1 1 d . . .
O14 O 0.1400(5) 0.1770(4) 0.0275(4) 0.1212(15) Uani 1 1 d . . .
C15 C 0.2186(4) -0.0629(4) 0.1179(4) 0.0645(11) Uani 1 1 d . . .
O15 O 0.2186(4) -0.1609(3) 0.0380(4) 0.1012(12) Uani 1 1 d . . .
C24 C 0.5185(4) 0.2744(4) 0.1774(4) 0.0622(10) Uani 1 1 d . . .
O24 O 0.5368(4) 0.3234(3) 0.0979(3) 0.0931(11) Uani 1 1 d . . .
C25 C 0.5690(4) 0.0777(4) 0.2013(4) 0.0586(10) Uani 1 1 d . . .
O25 O 0.6193(4) -0.0011(4) 0.1396(3) 0.0918(10) 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'
Fe Fe 0.3463 0.8444 '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'
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
C13 Fe1 C15 101.7(2) . . ?
C13 Fe1 C14 100.1(2) . . ?
C15 Fe1 C14 90.6(2) . . ?
C13 Fe1 S1 102.77(15) . . ?
C15 Fe1 S1 86.59(15) . . ?
C14 Fe1 S1 157.09(17) . . ?
C13 Fe1 S2 104.02(15) . . ?
C15 Fe1 S2 154.12(14) . . ?
C14 Fe1 S2 87.23(15) . . ?
S1 Fe1 S2 85.49(4) . . ?
C13 Fe1 Fe2 149.39(15) . . ?
C15 Fe1 Fe2 99.04(13) . . ?
C14 Fe1 Fe2 101.94(16) . . ?
S1 Fe1 Fe2 56.27(3) . . ?
S2 Fe1 Fe2 56.43(3) . . ?
C24 Fe2 C25 90.24(19) . . ?
C24 Fe2 S3 100.39(13) . . ?
C25 Fe2 S3 103.99(13) . . ?
C24 Fe2 S1 158.84(13) . . ?
C25 Fe2 S1 88.69(13) . . ?
S3 Fe2 S1 100.37(4) . . ?
C24 Fe2 S2 90.00(15) . . ?
C25 Fe2 S2 164.93(13) . . ?
S3 Fe2 S2 90.78(4) . . ?
S1 Fe2 S2 85.68(4) . . ?
C24 Fe2 Fe1 104.23(14) . . ?
C25 Fe2 Fe1 108.93(13) . . ?
S3 Fe2 Fe1 138.34(3) . . ?
S1 Fe2 Fe1 56.49(3) . . ?
S2 Fe2 Fe1 56.52(3) . . ?
C1 S1 Fe2 110.74(12) . . ?
C1 S1 Fe1 112.04(13) . . ?
Fe2 S1 Fe1 67.25(3) . . ?
C4 C1 S1 118.3(3) . . ?
C4 C1 H1A 107.7 . . ?
S1 C1 H1A 107.7 . . ?
C4 C1 H1B 107.7 . . ?
S1 C1 H1B 107.7 . . ?
H1A C1 H1B 107.1 . . ?
C2 S2 Fe2 110.12(13) . . ?
C2 S2 Fe1 113.84(14) . . ?
Fe2 S2 Fe1 67.05(3) . . ?
C4 C2 S2 118.0(2) . . ?
C4 C2 H2A 107.8 . . ?
S2 C2 H2A 107.8 . . ?
C4 C2 H2B 107.8 . . ?
S2 C2 H2B 107.8 . . ?
H2A C2 H2B 107.1 . . ?
C31 S3 C3 99.8(2) . . ?
C31 S3 Fe2 110.66(13) . . ?
C3 S3 Fe2 108.02(13) . . ?
C4 C3 S3 120.3(3) . . ?
C4 C3 H3A 107.2 . . ?
S3 C3 H3A 107.2 . . ?
C4 C3 H3B 107.2 . . ?
S3 C3 H3B 107.2 . . ?
H3A C3 H3B 106.9 . . ?
C311 C31 S3 113.3(3) . . ?
C311 C31 H31A 108.9 . . ?
S3 C31 H31A 108.9 . . ?
C311 C31 H31B 108.9 . . ?
S3 C31 H31B 108.9 . . ?
H31A C31 H31B 107.7 . . ?
C316 C311 C312 118.1(4) . . ?
C316 C311 C31 120.2(4) . . ?
C312 C311 C31 121.7(4) . . ?
C313 C312 C311 120.4(4) . . ?
C313 C312 H312 119.8 . . ?
C311 C312 H312 119.8 . . ?
C314 C313 C312 120.2(5) . . ?
C314 C313 H313 119.9 . . ?
C312 C313 H313 119.9 . . ?
C315 C314 C313 120.0(4) . . ?
C315 C314 H314 120.0 . . ?
C313 C314 H314 120.0 . . ?
C314 C315 C316 120.1(5) . . ?
C314 C315 H315 119.9 . . ?
C316 C315 H315 119.9 . . ?
C311 C316 C315 121.2(5) . . ?
C311 C316 H316 119.4 . . ?
C315 C316 H316 119.4 . . ?
C1 C4 C3 113.5(3) . . ?
C1 C4 C2 111.0(3) . . ?
C3 C4 C2 113.4(3) . . ?
C1 C4 C41 106.1(3) . . ?
C3 C4 C41 104.9(3) . . ?
C2 C4 C41 107.3(3) . . ?
C4 C41 H41A 109.5 . . ?
C4 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C4 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O13 C13 Fe1 179.4(5) . . ?
O14 C14 Fe1 179.1(5) . . ?
O15 C15 Fe1 178.2(4) . . ?
O24 C24 Fe2 178.0(4) . . ?
O25 C25 Fe2 177.9(4) . . ?
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 C13 1.779(5) . ?
Fe1 C15 1.782(4) . ?
Fe1 C14 1.784(5) . ?
Fe1 S1 2.2574(11) . ?
Fe1 S2 2.2617(11) . ?
Fe1 Fe2 2.4969(8) . ?
Fe2 C24 1.764(4) . ?
Fe2 C25 1.767(4) . ?
Fe2 S3 2.2347(10) . ?
Fe2 S1 2.2516(10) . ?
Fe2 S2 2.2594(11) . ?
S1 C1 1.820(4) . ?
C1 C4 1.507(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
S2 C2 1.830(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
S3 C31 1.808(4) . ?
S3 C3 1.822(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C31 C311 1.504(5) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C311 C316 1.360(6) . ?
C311 C312 1.387(6) . ?
C312 C313 1.383(6) . ?
C312 H312 0.9300 . ?
C313 C314 1.364(7) . ?
C313 H313 0.9300 . ?
C314 C315 1.346(7) . ?
C314 H314 0.9300 . ?
C315 C316 1.391(6) . ?
C315 H315 0.9300 . ?
C316 H316 0.9300 . ?
C4 C3 1.519(6) . ?
C4 C2 1.521(5) . ?
C4 C41 1.556(5) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C13 O13 1.145(5) . ?
C14 O14 1.131(5) . ?
C15 O15 1.133(5) . ?
C24 O24 1.147(5) . ?
C25 O25 1.146(5) . ?
