#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:07:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179094 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/56/4305673.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_4305673
loop_
_publ_author_name
'Christine M. Thomas'
'Tianbiao Liu'
'Michael B. Hall'
'Marcetta Y. Darensbourg'
_publ_contact_author_address
;Department of Chemistry
Texas A&M University
College Station, TX, 77843
;
_publ_contact_author_email       marcetta@mail.chem.tamu.edu
_publ_contact_author_name        'Marcetta Darensbourg'
_publ_section_title
;
Series of Mixed Valent Fe(II)Fe(I) Complexes That Model the Hox State of
[FeFe]Hydrogenase: Redox Properties, Density-Functional Theory
Investigation, and Reactivities with Extrinsic CO
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7009
_journal_page_last               7024
_journal_paper_doi               10.1021/ic800654a
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C21 H22 Fe2 N2 O5 S2'
_chemical_formula_weight         558.23
_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                103.22(3)
_cell_angle_beta                 91.81(3)
_cell_angle_gamma                100.43(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2476(16)
_cell_length_b                   8.4092(17)
_cell_length_c                   17.620(4)
_cell_measurement_temperature    273(2)
_cell_volume                     1166.6(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9488
_diffrn_reflns_theta_full        25.43
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    1.457
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             572
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0526
_reflns_number_gt                3204
_reflns_number_total             4226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800654a-file003_2.cif
_cod_data_source_block           ct05
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1166.6(4)
_cod_database_code               4305673
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 0.32093(5) 0.38464(5) 0.13976(2) 0.02010(11) Uani 1 1 d . . .
Fe2 Fe 0.11874(5) 0.23034(5) 0.21530(2) 0.01854(11) Uani 1 1 d . . .
N1 N -0.0756(3) -0.1163(3) 0.20842(12) 0.0225(6) Uani 1 1 d . . .
N2 N 0.0494(3) -0.0083(3) 0.32124(12) 0.0235(6) Uani 1 1 d . . .
O1 O 0.5803(3) 0.3635(3) 0.02989(12) 0.0457(6) Uani 1 1 d . . .
O2 O 0.4870(2) 0.6983(3) 0.24438(11) 0.0374(6) Uani 1 1 d . . .
O3 O -0.1871(2) 0.3357(3) 0.17931(12) 0.0420(6) Uani 1 1 d . . .
O4 O 0.1689(2) 0.5026(2) 0.35538(11) 0.0340(5) Uani 1 1 d . . .
O5 O 0.0863(3) 0.5569(3) 0.07782(12) 0.0410(6) Uani 1 1 d . . .
S1 S 0.14381(9) 0.14362(9) 0.08475(4) 0.02186(18) Uani 1 1 d . . .
S2 S 0.39772(8) 0.24585(9) 0.22669(4) 0.01965(17) Uani 1 1 d . . .
C1 C 0.4782(4) 0.3721(4) 0.07246(17) 0.0281(7) Uani 1 1 d . . .
C2 C 0.4199(3) 0.5752(4) 0.20445(16) 0.0244(7) Uani 1 1 d . . .
C3 C -0.0688(4) 0.2885(3) 0.19329(16) 0.0257(7) Uani 1 1 d . . .
C4 C 0.1470(3) 0.3883(4) 0.30328(16) 0.0245(7) Uani 1 1 d . . .
C5 C 0.1794(4) 0.4890(4) 0.10005(16) 0.0280(7) Uani 1 1 d . . .
C6 C 0.2549(3) -0.0286(3) 0.05800(15) 0.0258(7) Uani 1 1 d . . .
H6A H 0.1777 -0.1256 0.0282 0.031 Uiso 1 1 calc R . .
H6B H 0.3393 0.0010 0.0238 0.031 Uiso 1 1 calc R . .
C7 C 0.3365(3) -0.0765(3) 0.12531(15) 0.0240(7) Uani 1 1 d . . .
H7A H 0.3845 -0.1734 0.1049 0.029 Uiso 1 1 calc R . .
H7B H 0.2529 -0.1073 0.1596 0.029 Uiso 1 1 calc R . .
C8 C 0.4709(3) 0.0626(3) 0.17260(15) 0.0240(7) Uani 1 1 d . . .
H8A H 0.5503 0.0974 0.1373 0.029 Uiso 1 1 calc R . .
H8B H 0.5284 0.0183 0.2095 0.029 Uiso 1 1 calc R . .
C9 C -0.1057(4) -0.2351(4) 0.25143(17) 0.0310(8) Uani 1 1 d . . .
H9 H -0.1681 -0.3422 0.2343 0.037 Uiso 1 1 calc R . .
C10 C -0.0285(4) -0.1677(4) 0.32210(17) 0.0338(8) Uani 1 1 d . . .
H10 H -0.0273 -0.2181 0.3639 0.041 Uiso 1 1 calc R . .
C11 C 0.0238(3) 0.0289(3) 0.25018(15) 0.0202(7) Uani 1 1 d . . .
C12 C -0.1508(3) -0.1461(4) 0.12810(15) 0.0280(7) Uani 1 1 d . . .
H12A H -0.1644 -0.0421 0.1175 0.042 Uiso 1 1 calc R . .
H12B H -0.2567 -0.2189 0.1229 0.042 Uiso 1 1 calc R . .
H12C H -0.0802 -0.1968 0.0916 0.042 Uiso 1 1 calc R . .
C13 C 0.1304(3) 0.1087(4) 0.39187(15) 0.0230(7) Uani 1 1 d . . .
C14 C 0.0375(3) 0.2088(4) 0.43836(15) 0.0244(7) Uani 1 1 d . . .
C15 C 0.1162(4) 0.3192(4) 0.50569(15) 0.0272(7) Uani 1 1 d . . .
H15 H 0.0571 0.3905 0.5365 0.033 Uiso 1 1 calc R . .
C16 C 0.2806(4) 0.3268(4) 0.52866(16) 0.0318(8) Uani 1 1 d . . .
C17 C 0.3666(4) 0.2196(4) 0.48211(16) 0.0316(8) Uani 1 1 d . . .
H17 H 0.4765 0.2229 0.4971 0.038 Uiso 1 1 calc R . .
C18 C 0.2937(4) 0.1069(4) 0.41360(16) 0.0286(7) Uani 1 1 d . . .
C19 C 0.3867(4) -0.0143(4) 0.36599(17) 0.0442(9) Uani 1 1 d . . .
H19A H 0.5028 0.0328 0.3725 0.066 Uiso 1 1 calc R . .
H19B H 0.3487 -0.0372 0.3118 0.066 Uiso 1 1 calc R . .
H19C H 0.3679 -0.1159 0.3833 0.066 Uiso 1 1 calc R . .
C20 C -0.1432(3) 0.1976(4) 0.41718(17) 0.0388(9) Uani 1 1 d . . .
H20A H -0.1556 0.2318 0.3693 0.058 Uiso 1 1 calc R . .
H20B H -0.1885 0.2689 0.4582 0.058 Uiso 1 1 calc R . .
H20C H -0.2007 0.0847 0.4105 0.058 Uiso 1 1 calc R . .
C21 C 0.3658(4) 0.4492(4) 0.60208(16) 0.0446(9) Uani 1 1 d . . .
H21A H 0.4406 0.3981 0.6268 0.067 Uiso 1 1 calc R . .
H21B H 0.2844 0.4807 0.6373 0.067 Uiso 1 1 calc R . .
H21C H 0.4262 0.5463 0.5886 0.067 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'
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 96.80(13) . . ?
C2 Fe1 C5 90.86(12) . . ?
C1 Fe1 C5 104.43(13) . . ?
C2 Fe1 S1 163.50(10) . . ?
C1 Fe1 S1 99.57(10) . . ?
C5 Fe1 S1 87.02(9) . . ?
C2 Fe1 S2 89.12(9) . . ?
C1 Fe1 S2 102.92(9) . . ?
C5 Fe1 S2 152.45(10) . . ?
S1 Fe1 S2 85.29(4) . . ?
C2 Fe1 Fe2 107.77(10) . . ?
C1 Fe1 Fe2 146.65(10) . . ?
C5 Fe1 Fe2 97.54(10) . . ?
S1 Fe1 Fe2 56.44(3) . . ?
S2 Fe1 Fe2 56.52(3) . . ?
C3 Fe2 C4 88.84(12) . . ?
C3 Fe2 C11 97.60(12) . . ?
C4 Fe2 C11 102.77(12) . . ?
C3 Fe2 S1 88.92(10) . . ?
C4 Fe2 S1 151.28(10) . . ?
C11 Fe2 S1 105.90(8) . . ?
C3 Fe2 S2 157.50(10) . . ?
C4 Fe2 S2 86.60(9) . . ?
C11 Fe2 S2 104.89(8) . . ?
S1 Fe2 S2 84.63(4) . . ?
C3 Fe2 Fe1 102.89(10) . . ?
C4 Fe2 Fe1 96.84(10) . . ?
C11 Fe2 Fe1 151.80(8) . . ?
S1 Fe2 Fe1 55.93(3) . . ?
S2 Fe2 Fe1 55.96(3) . . ?
C11 N1 C9 112.3(2) . . ?
C11 N1 C12 126.0(2) . . ?
C9 N1 C12 121.6(2) . . ?
C11 N2 C10 112.5(2) . . ?
C11 N2 C13 125.6(2) . . ?
C10 N2 C13 121.5(2) . . ?
C6 S1 Fe1 110.83(9) . . ?
C6 S1 Fe2 114.58(9) . . ?
Fe1 S1 Fe2 67.63(4) . . ?
C8 S2 Fe1 108.28(9) . . ?
C8 S2 Fe2 115.37(9) . . ?
Fe1 S2 Fe2 67.52(3) . . ?
O1 C1 Fe1 179.2(3) . . ?
O2 C2 Fe1 177.9(3) . . ?
O3 C3 Fe2 176.2(3) . . ?
O4 C4 Fe2 172.7(3) . . ?
O5 C5 Fe1 177.0(3) . . ?
C7 C6 S1 115.89(18) . . ?
C6 C7 C8 113.0(2) . . ?
C7 C8 S2 115.08(18) . . ?
C10 C9 N1 107.1(3) . . ?
C9 C10 N2 106.6(3) . . ?
N1 C11 N2 101.5(2) . . ?
N1 C11 Fe2 129.29(19) . . ?
N2 C11 Fe2 129.1(2) . . ?
C14 C13 C18 122.4(3) . . ?
C14 C13 N2 118.4(2) . . ?
C18 C13 N2 119.0(3) . . ?
C15 C14 C13 117.7(3) . . ?
C15 C14 C20 120.8(3) . . ?
C13 C14 C20 121.4(3) . . ?
C14 C15 C16 122.1(3) . . ?
C17 C16 C15 118.1(3) . . ?
C17 C16 C21 120.3(3) . . ?
C15 C16 C21 121.6(3) . . ?
C16 C17 C18 122.2(3) . . ?
C13 C18 C17 117.3(3) . . ?
C13 C18 C19 121.4(3) . . ?
C17 C18 C19 121.3(3) . . ?
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 1.779(3) . ?
Fe1 C1 1.786(3) . ?
Fe1 C5 1.795(3) . ?
Fe1 S1 2.2631(12) . ?
Fe1 S2 2.2656(10) . ?
Fe1 Fe2 2.5265(10) . ?
Fe2 C3 1.762(3) . ?
Fe2 C4 1.774(3) . ?
Fe2 C11 1.971(3) . ?
Fe2 S1 2.2767(10) . ?
Fe2 S2 2.2807(9) . ?
N1 C11 1.376(3) . ?
N1 C9 1.380(3) . ?
N1 C12 1.475(3) . ?
N2 C11 1.377(3) . ?
N2 C10 1.381(3) . ?
N2 C13 1.454(3) . ?
O1 C1 1.146(3) . ?
O2 C2 1.143(3) . ?
O3 C3 1.157(3) . ?
O4 C4 1.150(3) . ?
O5 C5 1.145(3) . ?
S1 C6 1.831(3) . ?
S2 C8 1.830(3) . ?
C6 C7 1.513(3) . ?
C7 C8 1.522(4) . ?
C9 C10 1.332(4) . ?
C13 C14 1.388(4) . ?
C13 C18 1.392(4) . ?
C14 C15 1.386(4) . ?
C14 C20 1.505(3) . ?
C15 C16 1.388(4) . ?
C16 C17 1.385(4) . ?
C16 C21 1.516(4) . ?
C17 C18 1.393(4) . ?
C18 C19 1.504(4) . ?
