#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/24/2232405.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_2232405
loop_
_publ_author_name
'Shi, Yao-Cheng'
'Cheng, Huan-Ren'
'Yuan, Li-Min'
'Li, Qian-Kun'
_publ_section_title
;
 μ₄-Orthothiocarbonato-tetrakis[tricarbonyliron(I)](2
 Fe---Fe)
;
_journal_coeditor_code           NG5239
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1534
_journal_paper_doi               10.1107/S1600536811041936
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Fe4 (C S4) (C O)12]'
_chemical_formula_moiety         'C13 Fe4 O12 S4'
_chemical_formula_sum            'C13 Fe4 O12 S4'
_chemical_formula_weight         699.81
_chemical_name_systematic
;
μ₄-Orthothiocarbonato-tetrakis[tricarbonyliron(I)](2 Fe---Fe)
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.8859(12)
_cell_angle_beta                 92.4964(12)
_cell_angle_gamma                110.0857(12)
_cell_formula_units_Z            2
_cell_length_a                   9.0875(9)
_cell_length_b                   10.9002(11)
_cell_length_c                   12.6448(13)
_cell_measurement_reflns_used    4237
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.66
_cell_volume                     1142.2(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2003)'
_computing_molecular_graphics
'PLATON (Spek, 2009) and WinGX (Farrugia, 1999)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω and φ'
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10006
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    2.911
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5128
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0263
_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)+(0.0332P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                4237
_reflns_number_total             5128
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng5239.cif
_cod_data_source_block           I
_cod_database_code               2232405
_cod_database_fobs_code          2232405
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
_atom_site_symmetry_multiplicity
C C1 0.6561(3) 0.7935(2) 0.77984(18) 0.0440(5) Uani d U 1 1
C C2 0.8526(3) 0.8863(3) 0.6347(2) 0.0506(6) Uani d U 1 1
C C3 0.9578(3) 0.9654(3) 0.8400(2) 0.0495(6) Uani d U 1 1
C C4 1.1219(3) 0.7705(3) 0.5832(2) 0.0576(7) Uani d . 1 1
C C5 1.2260(3) 0.8567(3) 0.7869(2) 0.0499(6) Uani d . 1 1
C C6 1.1533(3) 0.5863(3) 0.6883(2) 0.0520(6) Uani d . 1 1
C C7 0.7715(3) 0.4656(3) 1.0044(2) 0.0518(6) Uani d . 1 1
C C8 0.6869(3) 0.2015(3) 0.9062(2) 0.0571(7) Uani d . 1 1
C C9 0.4644(3) 0.2955(2) 0.94124(17) 0.0461(6) Uani d . 1 1
C C10 0.5449(3) 0.1072(3) 0.6532(2) 0.0533(6) Uani d . 1 1
C C11 0.3306(3) 0.2117(3) 0.69401(19) 0.0538(6) Uani d . 1 1
C C12 0.5320(3) 0.3000(2) 0.54991(19) 0.0461(5) Uani d . 1 1
C C13 0.7801(2) 0.5349(2) 0.75626(15) 0.0326(4) Uani d . 1 1
Fe Fe1 0.85275(4) 0.80727(3) 0.74597(2) 0.03532(9) Uani d U 1 1
Fe Fe2 1.06610(4) 0.71578(3) 0.70503(2) 0.03858(9) Uani d . 1 1
Fe Fe3 0.64765(4) 0.34558(3) 0.88425(2) 0.03604(9) Uani d . 1 1
Fe Fe4 0.54035(4) 0.27424(3) 0.68685(2) 0.03649(9) Uani d . 1 1
O O1 0.5347(2) 0.7883(2) 0.80095(16) 0.0652(5) Uani d . 1 1
O O2 0.8523(3) 0.9343(2) 0.56303(17) 0.0808(7) Uani d . 1 1
O O3 1.0252(3) 1.0659(2) 0.89976(17) 0.0801(6) Uani d . 1 1
O O4 1.1562(3) 0.8060(3) 0.50561(17) 0.0906(8) Uani d . 1 1
O O5 1.3234(2) 0.9495(2) 0.83931(18) 0.0764(6) Uani d . 1 1
O O6 1.2101(3) 0.5078(2) 0.67522(19) 0.0802(6) Uani d . 1 1
O O7 0.8437(3) 0.5364(2) 1.08183(16) 0.0849(7) Uani d . 1 1
O O8 0.7108(3) 0.1096(2) 0.9194(2) 0.0923(7) Uani d . 1 1
O O9 0.3472(2) 0.2622(2) 0.97500(15) 0.0716(6) Uani d . 1 1
O O10 0.5481(3) 0.0019(2) 0.63331(18) 0.0840(7) Uani d . 1 1
O O11 0.1982(3) 0.1726(3) 0.69931(18) 0.0901(7) Uani d . 1 1
O O12 0.5245(2) 0.3122(2) 0.46352(14) 0.0717(6) Uani d . 1 1
S S1 0.92568(6) 0.68363(5) 0.84778(4) 0.03454(12) Uani d . 1 1
S S2 0.80928(7) 0.60300(6) 0.63482(4) 0.03789(13) Uani d . 1 1
S S3 0.80213(6) 0.37272(5) 0.74843(4) 0.03674(12) Uani d . 1 1
S S4 0.57807(6) 0.47963(5) 0.79267(4) 0.03420(12) Uani d . 1 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'
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
O1 C1 Fe1 178.3(2) ?
O2 C2 Fe1 178.8(2) ?
O3 C3 Fe1 179.6(3) ?
O4 C4 Fe2 179.2(3) ?
O5 C5 Fe2 177.0(2) ?
O6 C6 Fe2 177.6(2) ?
O7 C7 Fe3 176.7(2) ?
O8 C8 Fe3 179.5(3) ?
O9 C9 Fe3 178.5(2) ?
O10 C10 Fe4 179.2(3) ?
O11 C11 Fe4 179.5(3) ?
O12 C12 Fe4 178.0(2) ?
S1 C13 S3 118.10(10) ?
S1 C13 S2 95.10(10) y
S3 C13 S2 117.13(11) ?
S1 C13 S4 116.95(11) ?
S3 C13 S4 94.73(9) y
S2 C13 S4 116.62(10) ?
C2 Fe1 C3 92.20(12) ?
C2 Fe1 C1 97.54(11) ?
C3 Fe1 C1 96.81(11) ?
C2 Fe1 S2 93.44(9) ?
C3 Fe1 S2 158.89(8) ?
C1 Fe1 S2 102.58(8) ?
C2 Fe1 S1 156.74(8) ?
C3 Fe1 S1 94.58(8) ?
C1 Fe1 S1 103.69(7) ?
S2 Fe1 S1 72.90(2) ?
C2 Fe1 Fe2 100.11(8) ?
C3 Fe1 Fe2 102.33(8) ?
C1 Fe1 Fe2 153.30(7) ?
S2 Fe1 Fe2 56.636(18) ?
S1 Fe1 Fe2 56.695(17) ?
C5 Fe2 C4 91.26(13) ?
C5 Fe2 C6 100.64(12) ?
C4 Fe2 C6 96.91(11) ?
C5 Fe2 S2 153.65(8) ?
C4 Fe2 S2 93.88(9) ?
C6 Fe2 S2 104.35(9) ?
C5 Fe2 S1 93.23(8) ?
C4 Fe2 S1 157.61(9) ?
C6 Fe2 S1 103.77(8) ?
S2 Fe2 S1 72.92(2) ?
C5 Fe2 Fe1 97.00(8) ?
C4 Fe2 Fe1 100.96(8) ?
C6 Fe2 Fe1 154.51(8) ?
S2 Fe2 Fe1 56.649(18) ?
S1 Fe2 Fe1 56.723(17) ?
C8 Fe3 C9 91.66(12) ?
C8 Fe3 C7 97.13(12) ?
C9 Fe3 C7 98.48(11) ?
C8 Fe3 S3 93.97(9) ?
C9 Fe3 S3 155.51(7) ?
C7 Fe3 S3 104.42(8) ?
C8 Fe3 S4 158.63(9) ?
C9 Fe3 S4 93.86(8) ?
C7 Fe3 S4 102.43(8) ?
S3 Fe3 S4 72.99(2) ?
C8 Fe3 Fe4 102.35(9) ?
C9 Fe3 Fe4 98.88(7) ?
C7 Fe3 Fe4 153.39(8) ?
S3 Fe3 Fe4 56.635(18) ?
S4 Fe3 Fe4 56.394(17) ?
C10 Fe4 C11 92.11(13) ?
C10 Fe4 C12 97.98(11) ?
C11 Fe4 C12 97.54(11) ?
C10 Fe4 S4 157.10(8) ?
C11 Fe4 S4 93.60(9) ?
C12 Fe4 S4 103.21(8) ?
C10 Fe4 S3 94.03(9) ?
C11 Fe4 S3 157.73(8) ?
C12 Fe4 S3 102.76(8) ?
S4 Fe4 S3 73.03(2) ?
C10 Fe4 Fe3 100.52(8) ?
C11 Fe4 Fe3 101.33(8) ?
C12 Fe4 Fe3 152.93(8) ?
S4 Fe4 Fe3 56.600(16) ?
S3 Fe4 Fe3 56.499(16) ?
C13 S1 Fe2 88.02(6) ?
C13 S1 Fe1 87.12(6) ?
Fe2 S1 Fe1 66.582(18) ?
C13 S2 Fe2 88.06(7) ?
C13 S2 Fe1 87.17(7) ?
Fe2 S2 Fe1 66.715(19) ?
C13 S3 Fe3 87.77(7) ?
C13 S3 Fe4 87.52(7) ?
Fe3 S3 Fe4 66.867(19) ?
C13 S4 Fe4 87.60(7) ?
C13 S4 Fe3 87.58(6) ?
Fe4 S4 Fe3 67.006(19) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 1.131(3) ?
C1 Fe1 1.819(3) ?
C2 O2 1.136(3) ?
C2 Fe1 1.795(2) ?
C3 O3 1.142(3) ?
C3 Fe1 1.796(3) ?
C4 O4 1.145(3) ?
C4 Fe2 1.795(3) ?
C5 O5 1.142(3) ?
C5 Fe2 1.795(3) ?
C6 O6 1.130(3) ?
C6 Fe2 1.824(3) ?
C7 O7 1.127(3) ?
C7 Fe3 1.818(3) ?
C8 O8 1.138(3) ?
C8 Fe3 1.796(3) ?
C9 O9 1.134(3) ?
C9 Fe3 1.798(3) ?
C10 O10 1.135(3) ?
C10 Fe4 1.798(3) ?
C11 O11 1.140(3) ?
C11 Fe4 1.804(3) ?
C12 O12 1.129(3) ?
C12 Fe4 1.813(2) ?
C13 S1 1.827(2) y
C13 S2 1.8300(19) y
C13 S3 1.830(2) y
C13 S4 1.837(2) y
Fe1 S1 2.2730(6) y
Fe1 S2 2.2688(7) y
Fe1 Fe2 2.4949(5) y
Fe2 S1 2.2723(6) y
Fe2 S2 2.2685(7) y
Fe3 S3 2.2676(6) y
Fe3 S4 2.2680(6) y
Fe3 Fe4 2.5007(5) y
Fe4 S3 2.2712(7) y
Fe4 S4 2.2626(6) y
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
S1 S2 2.6984(8)
S3 S4 2.6977(8)
