#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/95/2019538.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_2019538
loop_
_publ_author_name
'Yang, Wei'
'Fu, Qiang'
'Zhao, Jing'
'Cheng, Huan-Ren'
'Shi, Yao-Cheng'
_publ_section_title
;
 Two Fe₃(μ₃-S)₂(CO)₈ clusters with terminal N-heterocyclic
 carbenes
;
_journal_coeditor_code           WQ3060
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              528
_journal_page_last               532
_journal_paper_doi               10.1107/S2053229614009310
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Fe3 (C3 H6 N2) S2 (C O)8]'
_chemical_formula_moiety         'C11 H6 Fe3 N2 O8 S2'
_chemical_formula_sum            'C11 H6 Fe3 N2 O8 S2'
_chemical_formula_weight         525.87
_chemical_name_systematic
;
Octacarbonyl(imidazolidinyl-κC²)di-μ₃-sulfido-triiron(II)(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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                78.4565(14)
_cell_angle_beta                 72.7596(13)
_cell_angle_gamma                67.3315(14)
_cell_formula_units_Z            2
_cell_length_a                   8.7679(3)
_cell_length_b                   10.0811(3)
_cell_length_c                   11.8549(15)
_cell_measurement_reflns_used    4141
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      1.81
_cell_volume                     919.07(12)
_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, 2012)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008b)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7989
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    2.603
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008a)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.297
_refine_ls_extinction_coef       0.042(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008b)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4141
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0267
_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)+(0.0423P)²+0.1300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0800
_reflns_number_gt                3710
_reflns_number_total             4141
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wq3060sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 2019538--2019539.cif.'
_cod_database_code               2019538
_cod_database_fobs_code          2019538
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 0.6460(3) 0.6802(2) 0.7929(2) 0.0456(5) Uani d . 1 1
C C2 0.6362(3) 0.6785(2) 0.5752(2) 0.0431(5) Uani d . 1 1
C C3 0.3538(3) 0.2950(3) 0.8391(2) 0.0524(5) Uani d . 1 1
C C4 0.6398(3) 0.0960(3) 0.9071(2) 0.0505(5) Uani d . 1 1
C C5 0.6007(4) 0.0964(3) 0.6964(2) 0.0578(6) Uani d . 1 1
C C6 0.9491(3) 0.4399(2) 0.6604(2) 0.0457(5) Uani d . 1 1
C C7 0.9582(3) 0.2074(3) 0.5769(2) 0.0497(5) Uani d . 1 1
C C8 0.9745(3) 0.1859(3) 0.7959(2) 0.0501(5) Uani d . 1 1
C C9 0.3648(3) 0.6593(2) 0.75631(17) 0.0360(4) Uani d . 1 1
C C10 0.0884(3) 0.7427(3) 0.8751(2) 0.0628(7) Uani d . 1 1
H H10A 0.0333 0.8313 0.9138 0.075 Uiso calc R 1 1
H H10B 0.0363 0.6723 0.9185 0.075 Uiso calc R 1 1
C C11 0.0801(3) 0.7700(3) 0.7454(2) 0.0597(6) Uani d . 1 1
H H11A 0.0094 0.7241 0.7313 0.072 Uiso calc R 1 1
H H11B 0.0374 0.8726 0.7204 0.072 Uiso calc R 1 1
Fe Fe1 0.60847(3) 0.56686(3) 0.71292(2) 0.03342(10) Uani d . 1 1
Fe Fe2 0.58059(4) 0.23067(3) 0.78620(3) 0.03822(10) Uani d . 1 1
Fe Fe3 0.84395(3) 0.30967(3) 0.70201(2) 0.03373(10) Uani d . 1 1
H H1N 0.289(4) 0.694(3) 0.611(3) 0.059(8) Uiso d . 1 1
H H2N 0.316(4) 0.655(3) 0.922(3) 0.065(9) Uiso d . 1 1
N N1 0.2597(2) 0.7028(3) 0.68538(18) 0.0577(6) Uani d . 1 1
N N2 0.2706(3) 0.6871(3) 0.86465(17) 0.0559(5) Uani d . 1 1
O O1 0.6707(3) 0.7485(2) 0.8464(2) 0.0759(6) Uani d . 1 1
O O2 0.6545(3) 0.7497(2) 0.48830(17) 0.0669(5) Uani d . 1 1
O O3 0.2091(3) 0.3422(3) 0.8727(2) 0.0841(7) Uani d . 1 1
O O4 0.6810(3) 0.0131(2) 0.9822(2) 0.0787(6) Uani d . 1 1
O O5 0.6102(4) 0.0136(2) 0.6405(3) 0.0954(8) Uani d . 1 1
O O6 1.0352(2) 0.5076(2) 0.63203(19) 0.0673(5) Uani d . 1 1
O O7 1.0296(3) 0.1421(3) 0.4979(2) 0.0853(7) Uani d . 1 1
O O8 1.0564(3) 0.1054(2) 0.8551(2) 0.0825(6) Uani d . 1 1
S S1 0.63208(6) 0.39129(5) 0.86325(4) 0.03702(13) Uani d . 1 1
S S2 0.61240(6) 0.38781(5) 0.62498(4) 0.03564(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'
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
O1 C1 Fe1 177.8(2) ?
O2 C2 Fe1 179.4(2) ?
O3 C3 Fe2 176.9(2) ?
O4 C4 Fe2 177.9(2) ?
O5 C5 Fe2 178.8(3) ?
O6 C6 Fe3 171.1(2) y
O7 C7 Fe3 179.5(3) y
O8 C8 Fe3 178.7(2) ?
N2 C9 N1 107.11(19) y
N2 C9 Fe1 125.81(16) y
N1 C9 Fe1 127.06(15) y
N2 C10 C11 101.87(19) ?
N2 C10 H10A 111.4 ?
C11 C10 H10A 111.4 ?
N2 C10 H10B 111.4 ?
C11 C10 H10B 111.4 ?
H10A C10 H10B 109.3 ?
N1 C11 C10 101.51(19) ?
N1 C11 H11A 111.5 ?
C10 C11 H11A 111.5 ?
N1 C11 H11B 111.5 ?
C10 C11 H11B 111.5 ?
H11A C11 H11B 109.3 ?
C1 Fe1 C2 93.25(11) ?
C1 Fe1 C9 93.83(9) ?
C2 Fe1 C9 94.43(9) ?
C1 Fe1 S1 91.35(8) ?
C2 Fe1 S1 166.56(7) ?
C9 Fe1 S1 97.85(6) ?
C1 Fe1 S2 167.25(8) ?
C2 Fe1 S2 93.01(7) ?
C9 Fe1 S2 96.75(6) ?
S1 Fe1 S2 80.19(2) ?
C1 Fe1 Fe3 112.25(7) ?
C2 Fe1 Fe3 111.75(7) ?
C9 Fe1 Fe3 140.93(6) ?
S1 Fe1 Fe3 54.894(15) ?
S2 Fe1 Fe3 55.044(15) ?
C3 Fe2 C5 98.20(12) ?
C3 Fe2 C4 100.26(11) ?
C5 Fe2 C4 92.60(12) ?
C3 Fe2 S2 100.61(8) ?
C5 Fe2 S2 91.48(9) ?
C4 Fe2 S2 157.92(8) ?
C3 Fe2 S1 97.66(8) ?
C5 Fe2 S1 163.11(9) ?
C4 Fe2 S1 90.25(8) ?
S2 Fe2 S1 79.92(2) ?
C3 Fe2 Fe3 144.06(8) ?
C5 Fe2 Fe3 107.88(9) ?
C4 Fe2 Fe3 102.73(7) ?
S2 Fe2 Fe3 55.470(15) ?
S1 Fe2 Fe3 55.298(15) ?
C7 Fe3 C8 93.34(11) ?
C7 Fe3 C6 97.10(11) ?
C8 Fe3 C6 97.96(11) ?
C7 Fe3 S1 157.49(8) ?
C8 Fe3 S1 90.38(8) ?
C6 Fe3 S1 104.36(7) ?
C7 Fe3 S2 87.25(8) ?
C8 Fe3 S2 151.60(8) ?
C6 Fe3 S2 110.16(8) ?
S1 Fe3 S2 79.13(2) ?
C7 Fe3 Fe2 102.74(8) ?
C8 Fe3 Fe2 97.80(8) ?
C6 Fe3 Fe2 153.80(7) ?
S1 Fe3 Fe2 54.748(16) ?
S2 Fe3 Fe2 54.655(16) ?
C7 Fe3 Fe1 129.23(8) ?
C8 Fe3 Fe1 136.70(8) ?
C6 Fe3 Fe1 72.29(7) ?
S1 Fe3 Fe1 54.085(15) ?
S2 Fe3 Fe1 54.060(15) ?
Fe2 Fe3 Fe1 81.885(12) y
C9 N1 C11 114.0(2) ?
C9 N1 H1N 125(2) ?
C11 N1 H1N 120.6(19) ?
C9 N2 C10 114.58(19) ?
C9 N2 H2N 119(2) ?
C10 N2 H2N 125(2) ?
Fe1 S1 Fe2 98.84(2) y
Fe1 S1 Fe3 71.021(18) ?
Fe2 S1 Fe3 69.954(17) ?
Fe1 S2 Fe2 98.85(2) y
Fe1 S2 Fe3 70.896(17) ?
Fe2 S2 Fe3 69.875(18) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 1.137(3) ?
C1 Fe1 1.795(2) ?
C2 O2 1.138(3) ?
C2 Fe1 1.798(2) ?
C3 O3 1.143(3) ?
C3 Fe2 1.788(2) ?
C4 O4 1.133(3) ?
C4 Fe2 1.812(2) ?
C5 O5 1.131(3) ?
C5 Fe2 1.811(3) ?
C6 O6 1.142(3) ?
C6 Fe1 2.686(3) y
C6 Fe3 1.795(2) ?
C7 O7 1.133(3) ?
C7 Fe3 1.789(2) ?
C8 O8 1.135(3) ?
C8 Fe3 1.790(2) ?
C9 N2 1.322(3) y
C9 N1 1.323(3) y
C9 Fe1 1.925(2) y
C10 N2 1.450(3) ?
C10 C11 1.525(4) ?
C10 H10A 0.9700 ?
C10 H10B 0.9700 ?
C11 N1 1.467(3) ?
C11 H11A 0.9700 ?
C11 H11B 0.9700 ?
Fe1 S1 2.2418(6) y
Fe1 S2 2.2428(5) y
Fe1 Fe2 3.4111(6) y
Fe1 Fe3 2.6176(4) y
Fe2 S2 2.2479(6) y
Fe2 S1 2.2494(6) y
Fe2 Fe3 2.5876(4) y
Fe3 S1 2.2645(5) y
Fe3 S2 2.2704(6) y
N1 H1N 0.85(3) ?
N2 H2N 0.84(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C11 H11A O6 1_455 0.97 2.59 3.391(3) 140.5 y
N1 H1N S2 2_666 0.85(3) 2.87(3) 3.707(2) 170(2) y
N2 H2N S1 2_667 0.84(3) 2.64(3) 3.442(2) 162(3) y
