#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/71/2217130.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2217130
loop_
_publ_author_name
'Tingting Zhang'
'Mei Wang'
'Ping Li'
'Licheng Sun'
_publ_section_title
;Octacarbonyl(5-methoxy-2,3-dihydro-1H-benzimidazol-2-yl)di-μ₃-sulfido-diiron(I)iron(II)(2
 Fe---Fe)
;
_journal_coeditor_code           HY2102
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m217
_journal_page_last               m217
_journal_paper_doi               10.1107/S160053680706415X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Fe3 (C8 H8 N2 O) S2 (C O)8]'
_chemical_formula_moiety         'C16 H8 Fe3 N2 O9 S2'
_chemical_formula_sum            'C16 H8 Fe3 N2 O9 S2'
_chemical_formula_weight         603.91
_chemical_name_systematic
;
Octacarbonyl(5-methoxy-2,3-dihydro-1H-benzimidazol-2-yl)di-μ₃-
sulfido-diiron(I)iron(II)(2 Fe---Fe)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                112.332(3)
_cell_angle_beta                 108.728(3)
_cell_angle_gamma                96.229(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0068(4)
_cell_length_b                   11.4504(5)
_cell_length_c                   12.5976(6)
_cell_measurement_reflns_used    3399
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.34
_cell_measurement_theta_min      3.62
_cell_volume                     1098.03(10)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8226
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.56
_exptl_absorpt_coefficient_mu    2.196
_exptl_absorpt_correction_T_max  0.8103
_exptl_absorpt_correction_T_min  0.6098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0275
_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)+(0.0345P)²+0.1529P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                3584
_reflns_number_total             4253
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            hy2102.cif
_cod_data_source_block           I
_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 

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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1098.00(10)
_cod_database_code               2217130
_cod_database_fobs_code          2217130
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Fe Fe2 0.76196(4) 0.76148(3) 0.59336(3) 0.03973(10) Uani d . 1
Fe Fe1 0.94423(4) 1.00067(3) 0.75013(3) 0.03945(10) Uani d . 1
Fe Fe3 0.54802(4) 0.85600(3) 0.66569(3) 0.03970(10) Uani d . 1
S S2 0.70315(7) 0.94813(6) 0.59519(5) 0.03972(14) Uani d . 1
S S1 0.79595(7) 0.87177(6) 0.79494(5) 0.04141(14) Uani d . 1
N N1 0.9696(2) 1.2115(2) 0.98758(18) 0.0454(5) Uani d . 1
H H1A 1.0240 1.1784 1.0333 0.055 Uiso calc R 1
N N2 0.8456(2) 1.24400(19) 0.83051(17) 0.0439(5) Uani d . 1
H H2A 0.8050 1.2356 0.7554 0.053 Uiso calc R 1
C C9 0.9253(3) 1.1612(2) 0.8629(2) 0.0406(5) Uani d . 1
O O8 0.2735(2) 0.7602(2) 0.4266(2) 0.0715(6) Uani d . 1
O O2 1.1025(3) 1.1243(2) 0.6350(2) 0.0833(7) Uani d . 1
C C15 0.8368(3) 1.3437(2) 0.9318(2) 0.0413(5) Uani d . 1
C C2 1.0438(3) 1.0765(3) 0.6799(2) 0.0530(6) Uani d . 1
O O1 1.2491(3) 0.9921(2) 0.9194(2) 0.0819(7) Uani d . 1
C C8 0.3784(3) 0.7992(2) 0.5209(3) 0.0475(6) Uani d . 1
C C1 1.1322(3) 0.9977(3) 0.8553(2) 0.0524(6) Uani d . 1
C C10 0.9171(3) 1.3231(2) 1.0340(2) 0.0443(5) Uani d . 1
O O5 0.5879(3) 0.6474(2) 0.3226(2) 0.0884(7) Uani d . 1
C C5 0.6572(3) 0.6905(3) 0.4274(3) 0.0555(6) Uani d . 1
C C4 0.7104(3) 0.6124(3) 0.6041(3) 0.0607(7) Uani d . 1
O O9 0.7147(3) 1.63452(19) 1.08295(19) 0.0690(5) Uani d . 1
C C14 0.7649(3) 1.4461(2) 0.9402(2) 0.0479(6) Uani d . 1
H H14A 0.7104 1.4583 0.8703 0.057 Uiso calc R 1
O O4 0.6759(3) 0.5192(2) 0.6127(3) 0.0997(9) Uani d . 1
C C13 0.7787(3) 1.5292(2) 1.0582(2) 0.0514(6) Uani d . 1
O O3 1.0797(3) 0.7445(3) 0.5882(3) 0.1048(9) Uani d . 1
C C3 0.9606(4) 0.7601(3) 0.5954(3) 0.0638(7) Uani d . 1
C C12 0.8608(4) 1.5093(3) 1.1619(3) 0.0606(7) Uani d . 1
H H12A 0.8691 1.5673 1.2402 0.073 Uiso calc R 1
O O7 0.3939(3) 0.6703(3) 0.7320(3) 0.1099(10) Uani d . 1
O O6 0.4779(4) 1.0948(3) 0.8090(3) 0.1222(11) Uani d . 1
C C16 0.6157(4) 1.6512(3) 0.9793(3) 0.0694(8) Uani d . 1
H H16A 0.5782 1.7280 1.0085 0.104 Uiso calc R 1
H H16B 0.5240 1.5760 0.9268 0.104 Uiso calc R 1
H H16C 0.6778 1.6608 0.9324 0.104 Uiso calc R 1
C C11 0.9296(4) 1.4067(3) 1.1513(2) 0.0596(7) Uani d . 1
H H11A 0.9830 1.3937 1.2208 0.072 Uiso calc R 1
C C6 0.5036(4) 1.0008(3) 0.7545(3) 0.0670(8) Uani d . 1
C C7 0.4532(3) 0.7432(3) 0.7076(3) 0.0630(8) Uani d . 1
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_publ_flag
C3 Fe2 C4 99.51(14) ?
C3 Fe2 C5 96.64(14) ?
C4 Fe2 C5 94.66(13) ?
C3 Fe2 S2 110.82(10) ?
C4 Fe2 S2 149.33(10) ?
C5 Fe2 S2 86.53(9) ?
C3 Fe2 S1 105.97(10) ?
C4 Fe2 S1 88.38(10) ?
C5 Fe2 S1 156.38(9) ?
S2 Fe2 S1 79.21(2) ?
C3 Fe2 Fe3 156.00(10) ?
C4 Fe2 Fe3 94.73(10) ?
C5 Fe2 Fe3 101.37(9) ?
S2 Fe2 Fe3 55.228(18) ?
S1 Fe2 Fe3 55.008(18) ?
C3 Fe2 Fe1 74.51(10) ?
C4 Fe2 Fe1 135.67(10) ?
C5 Fe2 Fe1 129.47(9) ?
S2 Fe2 Fe1 53.760(18) ?
S1 Fe2 Fe1 53.551(18) ?
Fe3 Fe2 Fe1 81.794(15) ?
C1 Fe1 C2 93.34(12) ?
C1 Fe1 C9 96.89(11) ?
C2 Fe1 C9 94.73(11) ?
C1 Fe1 S1 92.65(8) ?
C2 Fe1 S1 167.53(8) ?
C9 Fe1 S1 95.40(7) ?
C1 Fe1 S2 165.00(9) ?
C2 Fe1 S2 91.31(8) ?
C9 Fe1 S2 96.92(7) ?
S1 Fe1 S2 80.26(2) ?
C1 Fe1 Fe2 110.82(9) ?
C2 Fe1 Fe2 112.86(8) ?
C9 Fe1 Fe2 138.68(7) y
S1 Fe1 Fe2 54.701(19) ?
S2 Fe1 Fe2 54.352(18) ?
C8 Fe3 C6 99.45(14) ?
C8 Fe3 C7 91.77(12) ?
C6 Fe3 C7 99.30(15) ?
C8 Fe3 S1 156.98(9) ?
C6 Fe3 S1 102.43(11) ?
C7 Fe3 S1 91.72(9) ?
C8 Fe3 S2 90.45(8) ?
C6 Fe3 S2 97.38(10) ?
C7 Fe3 S2 162.57(10) ?
S1 Fe3 S2 79.75(2) ?
C8 Fe3 Fe2 101.57(9) ?
C6 Fe3 Fe2 145.32(10) y
C7 Fe3 Fe2 107.26(10) ?
S1 Fe3 Fe2 55.765(19) ?
S2 Fe3 Fe2 55.410(18) ?
Fe1 S2 Fe3 98.71(2) y
Fe1 S2 Fe2 71.89(2) y
Fe3 S2 Fe2 69.362(19) y
Fe1 S1 Fe3 98.96(2) y
Fe1 S1 Fe2 71.75(2) y
Fe3 S1 Fe2 69.23(2) y
C9 N1 C10 112.33(19) ?
C9 N1 H1A 123.8 ?
C10 N1 H1A 123.8 ?
C9 N2 C15 112.47(19) ?
C9 N2 H2A 123.8 ?
C15 N2 H2A 123.8 ?
N1 C9 N2 103.9(2) ?
N1 C9 Fe1 129.74(17) ?
N2 C9 Fe1 126.01(17) ?
C10 C15 N2 105.7(2) ?
C10 C15 C14 122.9(2) ?
N2 C15 C14 131.4(2) ?
O2 C2 Fe1 178.4(3) ?
O8 C8 Fe3 177.5(3) ?
O1 C1 Fe1 178.0(3) ?
C15 C10 C11 120.2(2) ?
C15 C10 N1 105.6(2) ?
C11 C10 N1 134.2(2) ?
O5 C5 Fe2 178.2(3) ?
O4 C4 Fe2 178.4(3) ?
C13 O9 C16 117.3(2) ?
C13 C14 C15 116.2(2) ?
C13 C14 H14A 121.9 ?
C15 C14 H14A 121.9 ?
O9 C13 C14 123.8(2) ?
O9 C13 C12 115.1(2) ?
C14 C13 C12 121.1(2) ?
O3 C3 Fe2 172.2(3) ?
C11 C12 C13 121.7(2) ?
C11 C12 H12A 119.1 ?
C13 C12 H12A 119.1 ?
O9 C16 H16A 109.5 ?
O9 C16 H16B 109.5 ?
H16A C16 H16B 109.5 ?
O9 C16 H16C 109.5 ?
H16A C16 H16C 109.5 ?
H16B C16 H16C 109.5 ?
C12 C11 C10 117.8(2) ?
C12 C11 H11A 121.1 ?
C10 C11 H11A 121.1 ?
O6 C6 Fe3 177.5(3) ?
O7 C7 Fe3 178.6(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Fe2 C3 1.783(3) ?
Fe2 C4 1.787(3) ?
Fe2 C5 1.788(3) ?
Fe2 S2 2.2505(7) y
Fe2 S1 2.2621(7) y
Fe2 Fe3 2.5582(5) y
Fe2 Fe1 2.6322(5) y
Fe1 C1 1.797(3) ?
Fe1 C2 1.807(3) ?
Fe1 C9 1.914(2) y
Fe1 S1 2.2294(6) y
Fe1 S2 2.2337(7) y
Fe3 C8 1.783(3) ?
Fe3 C6 1.784(3) ?
Fe3 C7 1.801(3) ?
Fe3 S1 2.2415(6) y
Fe3 S2 2.2455(6) y
N1 C9 1.348(3) ?
N1 C10 1.392(3) ?
N1 H1A 0.8600 ?
N2 C9 1.355(3) ?
N2 C15 1.384(3) ?
N2 H2A 0.8600 ?
O8 C8 1.135(3) ?
O2 C2 1.125(3) ?
C15 C10 1.380(3) ?
C15 C14 1.386(3) ?
O1 C1 1.128(3) ?
C10 C11 1.381(4) ?
O5 C5 1.134(3) ?
C4 O4 1.133(3) ?
O9 C13 1.366(3) ?
O9 C16 1.420(3) ?
C14 C13 1.383(4) ?
C14 H14A 0.9300 ?
C13 C12 1.395(4) ?
O3 C3 1.133(3) ?
C12 C11 1.369(4) ?
C12 H12A 0.9300 ?
O7 C7 1.132(3) ?
O6 C6 1.130(4) ?
C16 H16A 0.9600 ?
C16 H16B 0.9600 ?
C16 H16C 0.9600 ?
C11 H11A 0.9300 ?
