#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:18:11 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179684 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/06/7000662.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_7000662
loop_
_publ_author_name
'Sanina, Nataliya'
'Roudneva, Tatyana'
'Shilov, Gennady'
'Morgunov, Roman'
'Ovanesyan, Nikolay'
'Aldoshin, Sergey'
_publ_section_title
;
 Structure and properties of binuclear nitrosyl iron complex with
 benzimidazole-2-thiolyl
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              1703
_journal_page_last               1706
_journal_paper_doi               10.1039/b818443g
_journal_year                    2009
_chemical_formula_moiety         C14H10Fe2N8O4S2,2(C3H6O3)
_chemical_formula_sum            'C20 H22 Fe2 N8 O6 S2'
_chemical_formula_weight         646.28
_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                74.820(10)
_cell_angle_beta                 73.100(10)
_cell_angle_gamma                86.620(10)
_cell_formula_units_Z            1
_cell_length_a                   8.7370(10)
_cell_length_b                   9.0720(10)
_cell_length_c                   9.0830(10)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7
_cell_volume                     664.70(14)
_computing_cell_refinement       'XSCANS v2.2, 1995'
_computing_data_collection       'XSCANS v2.2, 1995'
_computing_data_reduction        'XSCANS v2.2, 1995'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  P4
_diffrn_measurement_method       theta/2theta
_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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2572
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.300
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0274
_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)+(0.0409P)²+0.3425P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                1884
_reflns_number_total             2080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b818443g.txt
_cod_data_source_block           nit200
_cod_original_cell_volume        664.70(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000662
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 0.12720(4) 0.15080(3) -0.20021(4) 0.02552(13) Uani 1 1 d . . .
S3 S 0.23995(7) 0.06132(6) 0.00553(7) 0.02831(17) Uani 1 1 d . . .
N3 N -0.0400(2) 0.0265(2) 0.2495(2) 0.0250(4) Uani 1 1 d . . .
C1 C 0.0965(3) 0.1043(2) 0.1654(3) 0.0242(5) Uani 1 1 d . . .
O3 O 0.3670(2) 0.42859(19) 0.1763(2) 0.0341(4) Uani 1 1 d . . .
N4 N 0.1140(2) 0.2230(2) 0.2240(2) 0.0269(4) Uani 1 1 d . . .
H1 H 0.1931 0.2873 0.1865 0.032 Uiso 1 1 calc R . .
C2 C -0.0156(3) 0.2240(3) 0.3533(3) 0.0259(5) Uani 1 1 d . . .
N2 N 0.2747(3) 0.2340(2) -0.3634(2) 0.0333(5) Uani 1 1 d . . .
O2 O 0.3559(3) 0.3269(2) -0.4678(2) 0.0570(6) Uani 1 1 d . . .
C7 C -0.0564(3) 0.3197(3) 0.4546(3) 0.0343(6) Uani 1 1 d . . .
H7 H 0.0091 0.4021 0.4414 0.041 Uiso 1 1 calc R . .
C3 C -0.1131(3) 0.0997(2) 0.3706(3) 0.0252(5) Uani 1 1 d . . .
O1 O -0.0649(3) 0.3921(2) -0.1114(3) 0.0602(6) Uani 1 1 d . . .
C4 C -0.2544(3) 0.0679(3) 0.4935(3) 0.0314(6) Uani 1 1 d . . .
H4 H -0.3202 -0.0145 0.5070 0.038 Uiso 1 1 calc R . .
N1 N -0.0042(3) 0.2808(2) -0.1390(2) 0.0318(5) Uani 1 1 d . . .
C8 C 0.5025(3) 0.3883(3) 0.1776(3) 0.0300(6) Uani 1 1 d . . .
C6 C -0.1977(3) 0.2883(3) 0.5758(3) 0.0369(6) Uani 1 1 d . . .
H6 H -0.2288 0.3511 0.6451 0.044 Uiso 1 1 calc R . .
C5 C -0.2941(3) 0.1637(3) 0.5958(3) 0.0348(6) Uani 1 1 d . . .
H5 H -0.3877 0.1440 0.6797 0.042 Uiso 1 1 calc R . .
C9 C 0.6159(3) 0.4895(3) 0.2032(3) 0.0426(7) Uani 1 1 d . . .
H9A H 0.7150 0.4988 0.1202 0.064 Uiso 1 1 calc R . .
H9B H 0.6351 0.4460 0.3044 0.064 Uiso 1 1 calc R . .
H9C H 0.5703 0.5886 0.2014 0.064 Uiso 1 1 calc R . .
C10 C 0.5617(4) 0.2369(3) 0.1528(4) 0.0470(7) Uani 1 1 d . . .
H10A H 0.6108 0.1867 0.2341 0.070 Uiso 1 1 calc R . .
H10B H 0.6388 0.2509 0.0502 0.070 Uiso 1 1 calc R . .
H10C H 0.4736 0.1754 0.1581 0.070 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
N1 Fe1 N2 111.06(10) . . ?
N1 Fe1 N3 117.33(9) . 2 ?
N2 Fe1 N3 106.92(9) . 2 ?
N1 Fe1 S3 103.91(7) . . ?
N2 Fe1 S3 107.53(7) . . ?
N3 Fe1 S3 109.73(6) 2 . ?
C1 S3 Fe1 102.47(8) . . ?
C1 N3 C3 105.97(17) . . ?
C1 N3 Fe1 126.11(14) . 2 ?
C3 N3 Fe1 127.81(16) . 2 ?
N3 C1 N4 111.1(2) . . ?
N3 C1 S3 126.46(16) . . ?
N4 C1 S3 122.41(19) . . ?
C1 N4 C2 108.7(2) . . ?
C1 N4 H1 125.6 . . ?
C2 N4 H1 125.6 . . ?
N4 C2 C7 132.1(2) . . ?
N4 C2 C3 105.84(19) . . ?
C7 C2 C3 122.0(2) . . ?
O2 N2 Fe1 161.6(2) . . ?
C6 C7 C2 117.6(2) . . ?
C6 C7 H7 121.2 . . ?
C2 C7 H7 121.2 . . ?
C4 C3 C2 120.1(2) . . ?
C4 C3 N3 131.5(2) . . ?
C2 C3 N3 108.3(2) . . ?
C3 C4 C5 117.6(2) . . ?
C3 C4 H4 121.2 . . ?
C5 C4 H4 121.2 . . ?
O1 N1 Fe1 164.6(2) . . ?
O3 C8 C10 121.4(2) . . ?
O3 C8 C9 121.3(2) . . ?
C10 C8 C9 117.3(2) . . ?
C7 C6 C5 120.8(2) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C5 C4 121.8(2) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
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 N1 1.682(2) . ?
Fe1 N2 1.687(2) . ?
Fe1 N3 2.0214(18) 2 ?
Fe1 S3 2.3029(7) . ?
S3 C1 1.736(2) . ?
N3 C1 1.339(3) . ?
N3 C3 1.409(3) . ?
N3 Fe1 2.0215(18) 2 ?
C1 N4 1.354(3) . ?
O3 C8 1.221(3) . ?
N4 C2 1.376(3) . ?
N4 H1 0.8600 . ?
C2 C7 1.385(3) . ?
C2 C3 1.401(3) . ?
N2 O2 1.172(3) . ?
C7 C6 1.380(4) . ?
C7 H7 0.9300 . ?
C3 C4 1.387(4) . ?
O1 N1 1.164(3) . ?
C4 C5 1.393(3) . ?
C4 H4 0.9300 . ?
C8 C10 1.489(4) . ?
C8 C9 1.493(3) . ?
C6 C5 1.391(4) . ?
C6 H6 0.9300 . ?
C5 H5 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
