#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/95/2019539.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_2019539
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 (C8 H8 N2) S2 (C O)8]'
_chemical_formula_moiety         'C16 H8 Fe3 N2 O8 S2'
_chemical_formula_sum            'C16 H8 Fe3 N2 O8 S2'
_chemical_formula_weight         587.93
_chemical_name_systematic
'Octacarbonyl(1-methylimidazo[1,5-a]pyridin-3-yl-κC³)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                108.477(5)
_cell_angle_beta                 107.608(2)
_cell_angle_gamma                96.455(8)
_cell_formula_units_Z            2
_cell_length_a                   8.9723(12)
_cell_length_b                   11.1249(11)
_cell_length_c                   12.0611(16)
_cell_measurement_reflns_used    4073
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      1.91
_cell_volume                     1059.1(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, 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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0417
_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       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9290
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    2.270
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008a)'
_exptl_crystal_colour            red-purple
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0284
_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)+(0.0392P)²+0.0391P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                4073
_reflns_number_total             4784
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wq3060sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 2019538--2019539.cif.'
_cod_database_code               2019539
_cod_database_fobs_code          2019539
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 0.3574(3) 0.6550(2) 0.6344(2) 0.0530(5) Uani d . 1 1
C C2 0.4721(3) 0.8911(2) 0.7945(2) 0.0529(5) Uani d . 1 1
C C3 0.9653(3) 0.7421(2) 0.6719(3) 0.0577(6) Uani d . 1 1
C C4 0.9925(3) 0.5436(2) 0.7588(2) 0.0501(5) Uani d . 1 1
C C5 1.1142(3) 0.7818(2) 0.9197(2) 0.0537(6) Uani d . 1 1
C C6 0.5227(3) 0.6540(2) 0.9021(2) 0.0558(6) Uani d . 1 1
C C7 0.8131(3) 0.7938(3) 1.0615(2) 0.0631(6) Uani d . 1 1
C C8 0.7822(3) 0.5441(2) 0.9280(2) 0.0562(6) Uani d . 1 1
C C9 0.5835(2) 0.80764(19) 0.5909(2) 0.0428(4) Uani d . 1 1
C C10 0.6107(4) 0.7103(3) 0.2754(3) 0.0819(9) Uani d . 1 1
H H10A 0.6841 0.6539 0.2783 0.123 Uiso calc R 1 1
H H10B 0.6404 0.7712 0.2401 0.123 Uiso calc R 1 1
H H10C 0.5036 0.6594 0.2245 0.123 Uiso calc R 1 1
C C11 0.6171(3) 0.7820(2) 0.4038(2) 0.0510(5) Uani d . 1 1
C C12 0.6796(3) 0.9107(2) 0.4800(2) 0.0471(5) Uani d . 1 1
C C13 0.7593(3) 1.0211(2) 0.4681(2) 0.0596(6) Uani d . 1 1
H H13 0.7797 1.0131 0.3952 0.072 Uiso calc R 1 1
C C14 0.8049(3) 1.1370(2) 0.5628(3) 0.0656(7) Uani d . 1 1
H H14 0.8564 1.2098 0.5553 0.079 Uiso calc R 1 1
C C15 0.7747(3) 1.1491(2) 0.6750(3) 0.0636(7) Uani d . 1 1
H H15 0.8046 1.2305 0.7390 0.076 Uiso calc R 1 1
C C16 0.7043(3) 1.0460(2) 0.6904(2) 0.0530(5) Uani d . 1 1
H H16 0.6881 1.0554 0.7651 0.064 Uiso calc R 1 1
Fe Fe1 0.55420(3) 0.75865(3) 0.72526(3) 0.04104(9) Uani d . 1 1
Fe Fe2 0.92683(3) 0.69495(3) 0.79106(3) 0.03959(9) Uani d . 1 1
Fe Fe3 0.72209(4) 0.68388(3) 0.90112(3) 0.04242(9) Uani d . 1 1
H H1N 0.512(3) 0.644(3) 0.443(2) 0.063(7) Uiso d . 1 1
N N1 0.5624(2) 0.72524(17) 0.47447(18) 0.0475(4) Uani d . 1 1
N N2 0.6555(2) 0.92438(16) 0.59346(16) 0.0435(4) Uani d . 1 1
O O1 0.2344(2) 0.5881(2) 0.5776(2) 0.0844(6) Uani d . 1 1
O O2 0.4161(3) 0.9707(2) 0.83834(19) 0.0780(6) Uani d . 1 1
O O3 0.9860(3) 0.7744(3) 0.5966(2) 0.0995(8) Uani d . 1 1
O O4 1.0315(2) 0.44821(17) 0.7375(2) 0.0792(6) Uani d . 1 1
O O5 1.2307(2) 0.8352(2) 1.0017(2) 0.0851(6) Uani d . 1 1
O O6 0.4007(2) 0.6263(2) 0.9108(2) 0.0825(6) Uani d . 1 1
O O7 0.8690(3) 0.8659(3) 1.16251(19) 0.0966(7) Uani d . 1 1
O O8 0.8154(3) 0.4526(2) 0.9421(2) 0.0831(6) Uani d . 1 1
S S1 0.66779(6) 0.58725(5) 0.69227(5) 0.04116(12) Uani d . 1 1
S S2 0.80693(6) 0.85570(5) 0.85743(5) 0.04302(13) 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'
Fe Fe 0.3463 0.8444 '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'
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 178.9(2) ?
O2 C2 Fe1 177.2(2) ?
O3 C3 Fe2 177.7(2) ?
O4 C4 Fe2 179.1(2) ?
O5 C5 Fe2 178.8(3) ?
O6 C6 Fe3 172.1(2) y
O7 C7 Fe3 178.3(3) y
O8 C8 Fe3 177.6(2) ?
N1 C9 N2 102.41(17) y
N1 C9 Fe1 126.24(14) y
N2 C9 Fe1 130.37(16) y
C11 C10 H10A 109.5 ?
C11 C10 H10B 109.5 ?
H10A C10 H10B 109.5 ?
C11 C10 H10C 109.5 ?
H10A C10 H10C 109.5 ?
H10B C10 H10C 109.5 ?
C12 C11 N1 105.01(19) ?
C12 C11 C10 130.7(2) ?
N1 C11 C10 124.2(2) ?
C11 C12 N2 106.24(17) ?
C11 C12 C13 134.6(2) ?
N2 C12 C13 119.2(2) ?
C14 C13 C12 119.4(2) ?
C14 C13 H13 120.3 ?
C12 C13 H13 120.3 ?
C13 C14 C15 120.3(2) ?
C13 C14 H14 119.9 ?
C15 C14 H14 119.9 ?
C16 C15 C14 121.6(2) ?
C16 C15 H15 119.2 ?
C14 C15 H15 119.2 ?
C15 C16 N2 119.3(2) ?
C15 C16 H16 120.3 ?
N2 C16 H16 120.3 ?
C1 Fe1 C2 91.72(11) ?
C1 Fe1 C9 95.87(10) ?
C2 Fe1 C9 99.14(10) ?
C1 Fe1 S2 167.63(8) ?
C2 Fe1 S2 94.02(8) ?
C9 Fe1 S2 94.02(7) ?
C1 Fe1 S1 91.33(8) ?
C2 Fe1 S1 163.43(8) ?
C9 Fe1 S1 96.75(6) ?
S2 Fe1 S1 80.14(2) ?
C1 Fe1 Fe3 113.41(8) ?
C2 Fe1 Fe3 109.23(8) ?
C9 Fe1 Fe3 137.75(6) ?
S2 Fe1 Fe3 54.301(16) ?
S1 Fe1 Fe3 54.850(17) ?
C3 Fe2 C5 99.42(12) ?
C3 Fe2 C4 98.80(11) ?
C5 Fe2 C4 92.05(10) ?
C3 Fe2 S2 96.58(8) ?
C5 Fe2 S2 91.21(7) ?
C4 Fe2 S2 163.53(7) ?
C3 Fe2 S1 101.03(9) ?
C5 Fe2 S1 158.50(8) ?
C4 Fe2 S1 91.32(7) ?
S2 Fe2 S1 79.95(2) ?
C3 Fe2 Fe3 143.35(8) ?
C5 Fe2 Fe3 103.38(8) ?
C4 Fe2 Fe3 108.57(7) ?
S2 Fe2 Fe3 55.001(17) ?
S1 Fe2 Fe3 55.565(18) ?
C6 Fe3 C8 99.40(11) ?
C6 Fe3 C7 95.81(12) ?
C8 Fe3 C7 95.94(12) ?
C6 Fe3 S2 118.87(8) ?
C8 Fe3 S2 141.52(8) ?
C7 Fe3 S2 84.66(9) ?
C6 Fe3 S1 99.32(8) ?
C8 Fe3 S1 91.40(8) ?
C7 Fe3 S1 161.87(9) ?
S2 Fe3 S1 79.33(2) ?
C6 Fe3 Fe2 153.00(8) ?
C8 Fe3 Fe2 89.34(7) ?
C7 Fe3 Fe2 108.72(8) ?
S2 Fe3 Fe2 54.822(16) ?
S1 Fe3 Fe2 54.672(17) ?
C6 Fe3 Fe1 76.04(8) ?
C8 Fe3 Fe1 142.49(9) ?
C7 Fe3 Fe1 121.48(9) ?
S2 Fe3 Fe1 53.950(18) ?
S1 Fe3 Fe1 53.854(17) ?
Fe2 Fe3 Fe1 81.492(15) y
C9 N1 C11 114.84(18) ?
C9 N1 H1N 123.7(17) ?
C11 N1 H1N 121.3(17) ?
C9 N2 C16 128.35(19) ?
C9 N2 C12 111.49(17) ?
C16 N2 C12 120.16(18) ?
Fe1 S1 Fe2 98.60(2) y
Fe1 S1 Fe3 71.297(19) ?
Fe2 S1 Fe3 69.763(19) ?
Fe1 S2 Fe2 98.75(2) y
Fe1 S2 Fe3 71.75(2) ?
Fe2 S2 Fe3 70.177(19) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 1.129(3) ?
C1 Fe1 1.795(2) ?
C2 O2 1.132(3) ?
C2 Fe1 1.802(2) ?
C3 O3 1.133(3) ?
C3 Fe2 1.788(2) ?
C4 O4 1.132(3) ?
C4 Fe2 1.811(2) ?
C5 O5 1.134(3) ?
C5 Fe2 1.809(3) ?
C6 O6 1.149(3) ?
C6 Fe1 2.802(2) y
C6 Fe3 1.787(2) ?
C7 O7 1.140(3) ?
C7 Fe3 1.796(3) ?
C8 O8 1.141(3) ?
C8 Fe3 1.793(2) ?
C9 N1 1.354(3) y
C9 N2 1.371(2) y
C9 Fe1 1.944(2) y
C10 C11 1.480(3) ?
C10 H10A 0.9600 ?
C10 H10B 0.9600 ?
C10 H10C 0.9600 ?
C11 C12 1.372(3) ?
C11 N1 1.376(3) ?
C12 N2 1.414(3) ?
C12 C13 1.420(3) ?
C13 C14 1.342(4) ?
C13 H13 0.9300 ?
C14 C15 1.428(4) ?
C14 H14 0.9300 ?
C15 C16 1.339(3) ?
C15 H15 0.9300 ?
C16 N2 1.394(3) ?
C16 H16 0.9300 ?
Fe1 S2 2.2406(7) y
Fe1 S1 2.2437(6) y
Fe1 Fe2 3.4050(6) y
Fe1 Fe3 2.6319(5) y
Fe2 S2 2.2456(6) y
Fe2 S1 2.2473(7) y
Fe2 Fe3 2.5846(5) y
Fe3 S2 2.2505(6) y
Fe3 S1 2.2719(7) y
N1 H1N 0.86(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
N1 H1N S1 2_666 0.86(3) 2.59(3) 3.4404(19) 168(2) y
C16 H16 O5 2_777 0.93 2.51 3.359(3) 151.2 y
