#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:40:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179256 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/76/4317608.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_4317608
loop_
_publ_author_name
'Dmitry V. Fomitchev'
'Craig C. McLauchlan'
'R. H. Holm'
_publ_contact_author
;
        R.H. Holm
        Department of Chemistry and Chemical Biology
        Harvard University
        Cambridge, MA 02138
        USA
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_contact_author_fax         '+1 (617) 496-9289'
_publ_contact_author_phone       '+1 (617) 495-0853'
_publ_section_title
;
 Heterometal Cubane-Type MFe3S4 Clusters (M = Mo, V) Trigonally
 Symmetrized with Hydrotris(pyrazolyl)borate(1-) and
 Tris(pyrazolyl)methanesulfonate(1-) Capping Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              958
_journal_page_last               966
_journal_paper_doi               10.1021/ic011106d
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '(C31 H30 Fe3 N6 O6 S5 V) (C4 H12 N)2'
_chemical_formula_sum            'C39 H54 Fe3 N8 O6 S5 V'
_chemical_formula_weight         1109.69
_chemical_name_systematic
;

  ?

;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.396(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1546(11)
_cell_length_b                   15.6592(13)
_cell_length_c                   24.0043(19)
_cell_measurement_temperature    213(2)
_cell_volume                     4878.3(7)
_computing_cell_refinement       'SMART, Version 5.618 (Bruker AXS, 2000)'
_computing_data_collection       'SMART, Version 5.618 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+, Version 6.02 (Bruker AXS, 1999)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART CCD area detector system'
_diffrn_measurement_method       'ο, 0.3 deg/frame'
_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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16047
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    1.325
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed in SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          .245
_exptl_crystal_size_mid          .155
_exptl_crystal_size_min          .052
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8815
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0582
_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

  1/[σ²(Fo²)+(0.0635Fo²)²]

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1315
_reflns_number_gt                6367
_reflns_number_total             8815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011106d_9.cif
_cod_data_source_block           '[Me4N]2[11]'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4317608
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
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 -0.16188(6) 0.30099(6) 0.76871(4) 0.0304(2) Uani 1 1 d . . .
Fe2 Fe 0.05027(6) 0.30801(6) 0.78344(4) 0.0302(2) Uani 1 1 d . . .
Fe3 Fe -0.06148(7) 0.39593(6) 0.69786(4) 0.0288(2) Uani 1 1 d . . .
V1 V -0.05466(8) 0.21857(6) 0.69402(5) 0.0228(2) Uani 1 1 d . . .
S1 S -0.04849(13) 0.19201(11) 0.79041(7) 0.0305(4) Uani 1 1 d . . .
S2 S 0.08081(12) 0.31449(11) 0.69273(7) 0.0300(4) Uani 1 1 d . . .
S3 S -0.19933(12) 0.30780(11) 0.67285(7) 0.0291(4) Uani 1 1 d . . .
S4 S -0.06196(14) 0.41947(12) 0.79363(7) 0.0374(4) Uani 1 1 d . . .
S5 S -0.05008(16) -0.04929(12) 0.56381(8) 0.0440(5) Uani 1 1 d . . .
N1 N -0.1540(4) 0.1069(3) 0.6780(2) 0.0268(12) Uani 1 1 d . . .
N2 N 0.0542(4) 0.1140(4) 0.6935(2) 0.0309(13) Uani 1 1 d . . .
N3 N -0.0602(4) 0.2017(3) 0.6037(2) 0.0287(12) Uani 1 1 d . . .
N4 N -0.1412(4) 0.0442(3) 0.6398(2) 0.0305(12) Uani 1 1 d . . .
N5 N 0.0420(4) 0.0468(3) 0.6554(2) 0.0294(12) Uani 1 1 d . . .
N6 N -0.0524(4) 0.1243(3) 0.5780(2) 0.0293(12) Uani 1 1 d . . .
N7 N -0.0571(5) -0.2755(4) 0.7157(3) 0.0426(15) Uani 1 1 d . . .
N8 N 0.0960(7) 0.2869(5) 0.9839(3) 0.067(2) Uani 1 1 d . . .
O1 O -0.0497(4) -0.1207(3) 0.6019(2) 0.0492(14) Uani 1 1 d . . .
O2 O 0.0441(5) -0.0390(4) 0.5416(2) 0.0576(15) Uani 1 1 d . . .
O3 O -0.1446(5) -0.0375(4) 0.5256(2) 0.0569(15) Uani 1 1 d . . .
O4 O -0.2841(4) 0.2715(4) 0.7960(2) 0.0502(14) Uani 1 1 d . . .
O5 O 0.1757(4) 0.2947(3) 0.8349(2) 0.0492(14) Uani 1 1 d . . .
O6 O -0.0640(4) 0.4993(3) 0.6543(2) 0.0427(12) Uani 1 1 d . . .
C1 C -0.2339(5) 0.0842(4) 0.7002(3) 0.0361(16) Uani 1 1 d . . .
H1A H -0.2593 0.1153 0.7284 0.043 Uiso 1 1 calc R . .
C2 C -0.2765(6) 0.0093(5) 0.6772(3) 0.048(2) Uani 1 1 d . . .
H2A H -0.3347 -0.0192 0.6860 0.057 Uiso 1 1 calc R . .
C3 C -0.2157(5) -0.0149(5) 0.6386(3) 0.0415(17) Uani 1 1 d . . .
H3A H -0.2245 -0.0637 0.6156 0.050 Uiso 1 1 calc R . .
C4 C 0.1377(5) 0.0938(5) 0.7287(3) 0.0402(17) Uani 1 1 d . . .
H4A H 0.1661 0.1283 0.7594 0.048 Uiso 1 1 calc R . .
C5 C 0.1796(6) 0.0167(5) 0.7160(4) 0.049(2) Uani 1 1 d . . .
H5A H 0.2388 -0.0102 0.7356 0.059 Uiso 1 1 calc R . .
C6 C 0.1165(5) -0.0119(5) 0.6690(3) 0.0390(17) Uani 1 1 d . . .
H6A H 0.1237 -0.0632 0.6497 0.047 Uiso 1 1 calc R . .
C7 C -0.0639(6) 0.2601(5) 0.5633(3) 0.0372(16) Uani 1 1 d . . .
H7A H -0.0706 0.3191 0.5687 0.045 Uiso 1 1 calc R . .
C8 C -0.0567(6) 0.2218(5) 0.5119(3) 0.0444(19) Uani 1 1 d . . .
H8A H -0.0569 0.2493 0.4771 0.053 Uiso 1 1 calc R . .
C9 C -0.0493(6) 0.1357(5) 0.5223(3) 0.0431(18) Uani 1 1 d . . .
H9A H -0.0433 0.0926 0.4958 0.052 Uiso 1 1 calc R . .
C10 C -0.0503(5) 0.0466(4) 0.6127(3) 0.0308(14) Uani 1 1 d . . .
C11 C -0.2845(5) 0.2599(6) 0.8525(3) 0.0432(18) Uani 1 1 d . . .
C12 C -0.2672(6) 0.3263(6) 0.8904(4) 0.052(2) Uani 1 1 d . . .
H12A H -0.2514 0.3808 0.8777 0.063 Uiso 1 1 calc R . .
C13 C -0.2726(7) 0.3143(6) 0.9467(4) 0.062(2) Uani 1 1 d . . .
H13A H -0.2645 0.3615 0.9712 0.075 Uiso 1 1 calc R . .
C14 C -0.2895(6) 0.2357(6) 0.9677(3) 0.052(2) Uani 1 1 d . . .
C15 C -0.3036(8) 0.1689(6) 0.9296(4) 0.067(3) Uani 1 1 d . . .
H15A H -0.3152 0.1138 0.9428 0.080 Uiso 1 1 calc R . .
C16 C -0.3013(8) 0.1802(6) 0.8740(4) 0.062(2) Uani 1 1 d . . .
H16A H -0.3112 0.1330 0.8495 0.075 Uiso 1 1 calc R . .
C17 C -0.2908(9) 0.2213(7) 1.0304(4) 0.079(3) Uani 1 1 d . . .
H17A H -0.2797 0.2752 1.0503 0.118 Uiso 1 1 calc R . .
H17B H -0.2366 0.1816 1.0453 0.118 Uiso 1 1 calc R . .
H17C H -0.3570 0.1980 1.0354 0.118 Uiso 1 1 calc R . .
C18 C 0.2582(5) 0.3431(5) 0.8440(3) 0.0328(15) Uani 1 1 d . . .
C19 C 0.2575(6) 0.4289(6) 0.8309(4) 0.058(2) Uani 1 1 d . . .
H19A H 0.1958 0.4546 0.8135 0.070 Uiso 1 1 calc R . .
C20 C 0.3476(7) 0.4790(6) 0.8431(4) 0.062(3) Uani 1 1 d . . .
H20A H 0.3441 0.5380 0.8355 0.074 Uiso 1 1 calc R . .
C21 C 0.4395(6) 0.4435(6) 0.8655(3) 0.050(2) Uani 1 1 d . . .
C22 C 0.4398(5) 0.3573(5) 0.8782(3) 0.0404(17) Uani 1 1 d . . .
H22A H 0.5019 0.3314 0.8948 0.048 Uiso 1 1 calc R . .
C23 C 0.3529(5) 0.3087(5) 0.8672(3) 0.0376(16) Uani 1 1 d . . .
H23A H 0.3572 0.2500 0.8757 0.045 Uiso 1 1 calc R . .
C24 C 0.5372(7) 0.4974(7) 0.8795(4) 0.076(3) Uani 1 1 d . . .
H24A H 0.5222 0.5558 0.8674 0.113 Uiso 1 1 calc R . .
H24B H 0.5901 0.4744 0.8600 0.113 Uiso 1 1 calc R . .
H24C H 0.5612 0.4962 0.9199 0.113 Uiso 1 1 calc R . .
C25 C -0.0824(5) 0.4890(4) 0.5977(3) 0.0402(18) Uani 1 1 d . . .
C26 C -0.1816(6) 0.4904(5) 0.5682(3) 0.047(2) Uani 1 1 d . . .
H26A H -0.2367 0.5010 0.5877 0.057 Uiso 1 1 calc R . .
C27 C -0.2018(8) 0.4764(6) 0.5105(4) 0.064(2) Uani 1 1 d . . .
H27A H -0.2704 0.4765 0.4918 0.076 Uiso 1 1 calc R . .
C28 C -0.1225(9) 0.4622(5) 0.4797(4) 0.059(2) Uani 1 1 d . . .
C29 C -0.0225(8) 0.4638(5) 0.5092(4) 0.058(2) Uani 1 1 d . . .
H29A H 0.0329 0.4551 0.4896 0.070 Uiso 1 1 calc R . .
C30 C -0.0025(6) 0.4781(5) 0.5672(4) 0.053(2) Uani 1 1 d . . .
H30A H 0.0661 0.4803 0.5860 0.063 Uiso 1 1 calc R . .
C31 C -0.1417(10) 0.4437(7) 0.4160(4) 0.087(4) Uani 1 1 d . . .
H31A H -0.0763 0.4361 0.4030 0.131 Uiso 1 1 calc R . .
H31B H -0.1785 0.4912 0.3961 0.131 Uiso 1 1 calc R . .
H31C H -0.1825 0.3921 0.4087 0.131 Uiso 1 1 calc R . .
C32 C -0.0469(9) -0.1851(6) 0.7364(4) 0.073(3) Uani 1 1 d . . .
H32A H -0.1033 -0.1717 0.7564 0.110 Uiso 1 1 calc R . .
H32B H -0.0489 -0.1467 0.7045 0.110 Uiso 1 1 calc R . .
H32C H 0.0181 -0.1782 0.7617 0.110 Uiso 1 1 calc R . .
C33 C -0.0563(11) -0.3353(6) 0.7639(4) 0.094(4) Uani 1 1 d . . .
H33A H -0.1146 -0.3232 0.7827 0.141 Uiso 1 1 calc R . .
H33B H 0.0072 -0.3282 0.7903 0.141 Uiso 1 1 calc R . .
H33C H -0.0610 -0.3936 0.7500 0.141 Uiso 1 1 calc R . .
C34 C -0.1532(7) -0.2881(7) 0.6754(5) 0.081(3) Uani 1 1 d . . .
H34A H -0.2119 -0.2777 0.6942 0.122 Uiso 1 1 calc R . .
H34B H -0.1559 -0.3463 0.6613 0.122 Uiso 1 1 calc R . .
H34C H -0.1551 -0.2487 0.6441 0.122 Uiso 1 1 calc R . .
C35 C 0.0302(7) -0.2943(7) 0.6858(5) 0.071(3) Uani 1 1 d . . .
H35A H 0.0247 -0.3526 0.6719 0.106 Uiso 1 1 calc R . .
H35B H 0.0945 -0.2873 0.7116 0.106 Uiso 1 1 calc R . .
H35C H 0.0285 -0.2553 0.6542 0.106 Uiso 1 1 calc R . .
C36 C 0.1132(18) 0.2815(10) 1.0449(6) 0.179(9) Uani 1 1 d . . .
H36A H 0.0801 0.3295 1.0602 0.268 Uiso 1 1 calc R . .
H36B H 0.1866 0.2829 1.0589 0.268 Uiso 1 1 calc R . .
H36C H 0.0844 0.2286 1.0564 0.268 Uiso 1 1 calc R . .
C37 C 0.1451(11) 0.2110(7) 0.9616(6) 0.106(4) Uani 1 1 d . . .
H37A H 0.1276 0.2097 0.9207 0.158 Uiso 1 1 calc R . .
H37B H 0.1204 0.1593 0.9771 0.158 Uiso 1 1 calc R . .
H37C H 0.2194 0.2146 0.9723 0.158 Uiso 1 1 calc R . .
C38 C 0.1493(11) 0.3645(8) 0.9662(6) 0.117(5) Uani 1 1 d . . .
H38A H 0.1181 0.4153 0.9792 0.176 Uiso 1 1 calc R . .
H38B H 0.1426 0.3658 0.9254 0.176 Uiso 1 1 calc R . .
H38C H 0.2217 0.3626 0.9826 0.176 Uiso 1 1 calc R . .
C39 C -0.0083(11) 0.2961(13) 0.9624(9) 0.187(10) Uani 1 1 d . . .
H39A H -0.0349 0.3462 0.9790 0.281 Uiso 1 1 calc R . .
H39B H -0.0454 0.2459 0.9716 0.281 Uiso 1 1 calc R . .
H39C H -0.0171 0.3028 0.9217 0.281 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'
V V 0.3005 0.5294 '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
O4 Fe1 S1 107.53(19) . . ?
O4 Fe1 S3 107.84(17) . . ?
S1 Fe1 S3 107.03(7) . . ?
O4 Fe1 S4 126.16(19) . . ?
S1 Fe1 S4 102.76(7) . . ?
S3 Fe1 S4 104.23(7) . . ?
O4 Fe1 Fe3 150.13(18) . . ?
S1 Fe1 Fe3 100.61(6) . . ?
S3 Fe1 Fe3 52.89(5) . . ?
S4 Fe1 Fe3 54.02(5) . . ?
O4 Fe1 Fe2 149.96(17) . . ?
S1 Fe1 Fe2 52.21(5) . . ?
S3 Fe1 Fe2 100.10(6) . . ?
S4 Fe1 Fe2 53.84(5) . . ?
Fe3 Fe1 Fe2 58.68(3) . . ?
O4 Fe1 V1 131.44(19) . . ?
S1 Fe1 V1 54.14(5) . . ?
S3 Fe1 V1 54.36(5) . . ?
S4 Fe1 V1 102.38(6) . . ?
Fe3 Fe1 V1 60.41(3) . . ?
Fe2 Fe1 V1 59.38(3) . . ?
O5 Fe2 S1 108.22(16) . . ?
O5 Fe2 S2 110.78(19) . . ?
S1 Fe2 S2 107.46(7) . . ?
O5 Fe2 S4 120.80(19) . . ?
S1 Fe2 S4 102.33(8) . . ?
S2 Fe2 S4 106.32(7) . . ?
O5 Fe2 Fe3 148.83(16) . . ?
S1 Fe2 Fe3 102.62(6) . . ?
S2 Fe2 Fe3 53.82(5) . . ?
S4 Fe2 Fe3 54.61(5) . . ?
O5 Fe2 V1 136.43(18) . . ?
S1 Fe2 V1 54.81(5) . . ?
S2 Fe2 V1 54.50(5) . . ?
S4 Fe2 V1 102.64(6) . . ?
Fe3 Fe2 V1 61.48(3) . . ?
O5 Fe2 Fe1 146.17(18) . . ?
S1 Fe2 Fe1 52.71(5) . . ?
S2 Fe2 Fe1 102.22(5) . . ?
S4 Fe2 Fe1 52.88(5) . . ?
Fe3 Fe2 Fe1 60.58(3) . . ?
V1 Fe2 Fe1 60.61(3) . . ?
O6 Fe3 S3 115.05(16) . . ?
O6 Fe3 S2 112.41(17) . . ?
S3 Fe3 S2 105.74(7) . . ?
O6 Fe3 S4 113.66(16) . . ?
S3 Fe3 S4 103.03(7) . . ?
S2 Fe3 S4 106.01(7) . . ?
O6 Fe3 Fe2 143.26(16) . . ?
S3 Fe3 Fe2 101.68(6) . . ?
S2 Fe3 Fe2 53.66(5) . . ?
S4 Fe3 Fe2 54.46(5) . . ?
O6 Fe3 Fe1 145.36(17) . . ?
S3 Fe3 Fe1 52.75(5) . . ?
S2 Fe3 Fe1 102.22(6) . . ?
S4 Fe3 Fe1 52.91(5) . . ?
Fe2 Fe3 Fe1 60.74(3) . . ?
O6 Fe3 V1 145.03(16) . . ?
S3 Fe3 V1 54.22(5) . . ?
S2 Fe3 V1 53.81(5) . . ?
S4 Fe3 V1 101.31(6) . . ?
Fe2 Fe3 V1 59.96(4) . . ?
Fe1 Fe3 V1 60.16(4) . . ?
N3 V1 N2 79.5(2) . . ?
N3 V1 N1 78.7(2) . . ?
N2 V1 N1 76.75(19) . . ?
N3 V1 S2 88.05(15) . . ?
N2 V1 S2 88.85(16) . . ?
N1 V1 S2 161.94(15) . . ?
N3 V1 S1 162.78(15) . . ?
N2 V1 S1 87.45(16) . . ?
N1 V1 S1 87.43(15) . . ?
S2 V1 S1 102.96(7) . . ?
N3 V1 S3 87.85(15) . . ?
N2 V1 S3 163.08(16) . . ?
N1 V1 S3 89.89(15) . . ?
S2 V1 S3 101.99(7) . . ?
S1 V1 S3 102.47(7) . . ?
N3 V1 Fe2 140.72(15) . . ?
N2 V1 Fe2 98.15(15) . . ?
N1 V1 Fe2 139.42(15) . . ?
S2 V1 Fe2 52.67(5) . . ?
S1 V1 Fe2 52.00(5) . . ?
S3 V1 Fe2 98.76(6) . . ?
N3 V1 Fe1 139.77(15) . . ?
N2 V1 Fe1 139.31(16) . . ?
N1 V1 Fe1 97.72(15) . . ?
S2 V1 Fe1 100.32(6) . . ?
S1 V1 Fe1 51.88(5) . . ?
S3 V1 Fe1 51.94(5) . . ?
Fe2 V1 Fe1 60.01(3) . . ?
N3 V1 Fe3 99.11(14) . . ?
N2 V1 Fe3 140.95(16) . . ?
N1 V1 Fe3 141.79(15) . . ?
S2 V1 Fe3 52.18(5) . . ?
S1 V1 Fe3 98.10(6) . . ?
S3 V1 Fe3 51.95(5) . . ?
Fe2 V1 Fe3 58.56(4) . . ?
Fe1 V1 Fe3 59.43(4) . . ?
Fe2 S1 Fe1 75.07(6) . . ?
Fe2 S1 V1 73.19(6) . . ?
Fe1 S1 V1 73.98(6) . . ?
Fe2 S2 Fe3 72.52(6) . . ?
Fe2 S2 V1 72.83(6) . . ?
Fe3 S2 V1 74.01(6) . . ?
Fe1 S3 Fe3 74.37(6) . . ?
Fe1 S3 V1 73.70(6) . . ?
Fe3 S3 V1 73.83(6) . . ?
Fe1 S4 Fe2 73.27(6) . . ?
Fe1 S4 Fe3 73.06(6) . . ?
Fe2 S4 Fe3 70.93(6) . . ?
O3 S5 O2 117.4(4) . . ?
O3 S5 O1 114.7(4) . . ?
O2 S5 O1 114.1(4) . . ?
O3 S5 C10 101.8(3) . . ?
O2 S5 C10 103.2(3) . . ?
O1 S5 C10 102.7(3) . . ?
C1 N1 N4 105.8(5) . . ?
C1 N1 V1 130.3(5) . . ?
N4 N1 V1 123.9(4) . . ?
C4 N2 N5 103.7(6) . . ?
C4 N2 V1 131.3(5) . . ?
N5 N2 V1 124.8(4) . . ?
C7 N3 N6 106.0(5) . . ?
C7 N3 V1 129.5(5) . . ?
N6 N3 V1 124.3(4) . . ?
C3 N4 N1 109.8(6) . . ?
C3 N4 C10 131.2(6) . . ?
N1 N4 C10 118.7(5) . . ?
C6 N5 N2 111.0(5) . . ?
C6 N5 C10 131.3(6) . . ?
N2 N5 C10 117.4(5) . . ?
C9 N6 N3 110.1(5) . . ?
C9 N6 C10 131.8(6) . . ?
N3 N6 C10 118.1(5) . . ?
C34 N7 C35 107.8(8) . . ?
C34 N7 C33 108.8(8) . . ?
C35 N7 C33 110.2(8) . . ?
C34 N7 C32 111.4(7) . . ?
C35 N7 C32 108.3(7) . . ?
C33 N7 C32 110.4(7) . . ?
C39 N8 C36 111.2(15) . . ?
C39 N8 C37 114.1(11) . . ?
C36 N8 C37 108.2(11) . . ?
C39 N8 C38 106.8(12) . . ?
C36 N8 C38 109.3(10) . . ?
C37 N8 C38 107.1(9) . . ?
C11 O4 Fe1 121.2(4) . . ?
C18 O5 Fe2 130.5(4) . . ?
C25 O6 Fe3 115.6(4) . . ?
N1 C1 C2 111.8(6) . . ?
C3 C2 C1 105.2(6) . . ?
N4 C3 C2 107.4(7) . . ?
N2 C4 C5 113.0(7) . . ?
C6 C5 C4 105.0(6) . . ?
N5 C6 C5 107.3(6) . . ?
N3 C7 C8 110.7(6) . . ?
C9 C8 C7 105.9(6) . . ?
N6 C9 C8 107.3(6) . . ?
N4 C10 N5 109.7(5) . . ?
N4 C10 N6 109.6(5) . . ?
N5 C10 N6 109.4(5) . . ?
N4 C10 S5 109.9(4) . . ?
N5 C10 S5 110.5(4) . . ?
N6 C10 S5 107.7(4) . . ?
O4 C11 C12 121.8(8) . . ?
O4 C11 C16 121.2(8) . . ?
C12 C11 C16 117.0(8) . . ?
C11 C12 C13 121.0(8) . . ?
C14 C13 C12 121.6(8) . . ?
C13 C14 C15 117.0(8) . . ?
C13 C14 C17 121.8(9) . . ?
C15 C14 C17 121.2(9) . . ?
C16 C15 C14 122.1(9) . . ?
C15 C16 C11 121.2(9) . . ?
O5 C18 C19 123.4(6) . . ?
O5 C18 C23 120.4(7) . . ?
C19 C18 C23 116.3(7) . . ?
C18 C19 C20 121.3(7) . . ?
C21 C20 C19 121.1(8) . . ?
C20 C21 C22 117.2(7) . . ?
C20 C21 C24 121.5(8) . . ?
C22 C21 C24 121.2(7) . . ?
C23 C22 C21 122.0(7) . . ?
C22 C23 C18 122.0(7) . . ?
O6 C25 C26 120.9(7) . . ?
O6 C25 C30 121.3(7) . . ?
C26 C25 C30 117.8(8) . . ?
C25 C26 C27 121.5(8) . . ?
C26 C27 C28 121.2(9) . . ?
C29 C28 C27 117.1(8) . . ?
C29 C28 C31 120.0(10) . . ?
C27 C28 C31 122.9(10) . . ?
C28 C29 C30 121.5(8) . . ?
C25 C30 C29 120.8(8) . . ?
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 O4 1.890(5) . ?
Fe1 S1 2.270(2) . ?
Fe1 S3 2.2756(19) . ?
Fe1 S4 2.296(2) . ?
Fe1 Fe3 2.7533(13) . ?
Fe1 Fe2 2.7574(12) . ?
Fe1 V1 2.7739(14) . ?
Fe2 O5 1.904(5) . ?
Fe2 S1 2.255(2) . ?
Fe2 S2 2.2801(19) . ?
Fe2 S4 2.325(2) . ?
Fe2 Fe3 2.7001(13) . ?
Fe2 V1 2.7397(14) . ?
Fe3 O6 1.924(5) . ?
Fe3 S3 2.2799(18) . ?
Fe3 S2 2.2849(19) . ?
Fe3 S4 2.3291(19) . ?
Fe3 V1 2.7808(13) . ?
V1 N3 2.174(6) . ?
V1 N2 2.177(6) . ?
V1 N1 2.179(5) . ?
V1 S2 2.3347(19) . ?
V1 S1 2.3390(19) . ?
V1 S3 2.3487(19) . ?
S5 O3 1.431(6) . ?
S5 O2 1.436(6) . ?
S5 O1 1.444(5) . ?
S5 C10 1.906(7) . ?
N1 C1 1.303(8) . ?
N1 N4 1.371(7) . ?
N2 C4 1.311(9) . ?
N2 N5 1.385(7) . ?
N3 C7 1.328(9) . ?
N3 N6 1.372(7) . ?
N4 C3 1.345(8) . ?
N4 C10 1.453(8) . ?
N5 C6 1.345(8) . ?
N5 C10 1.456(8) . ?
N6 C9 1.355(8) . ?
N6 C10 1.472(8) . ?
N7 C34 1.474(11) . ?
N7 C35 1.480(11) . ?
N7 C33 1.487(11) . ?
N7 C32 1.500(10) . ?
N8 C39 1.392(15) . ?
N8 C36 1.447(15) . ?
N8 C37 1.493(13) . ?
N8 C38 1.499(13) . ?
O4 C11 1.368(9) . ?
O5 C18 1.312(8) . ?
O6 C25 1.348(9) . ?
C1 C2 1.376(10) . ?
C2 C3 1.371(11) . ?
C4 C5 1.382(10) . ?
C5 C6 1.364(10) . ?
C7 C8 1.389(10) . ?
C8 C9 1.372(10) . ?
C11 C12 1.377(11) . ?
C11 C16 1.382(12) . ?
C12 C13 1.378(12) . ?
C13 C14 1.363(13) . ?
C14 C15 1.381(13) . ?
C14 C17 1.525(12) . ?
C15 C16 1.352(12) . ?
C18 C19 1.379(11) . ?
C18 C23 1.389(9) . ?
C19 C20 1.412(12) . ?
C20 C21 1.359(11) . ?
C21 C22 1.384(11) . ?
C21 C24 1.528(11) . ?
C22 C23 1.363(10) . ?
C25 C26 1.380(9) . ?
C25 C30 1.386(11) . ?
C26 C27 1.386(12) . ?
C27 C28 1.392(14) . ?
C28 C29 1.388(13) . ?
C28 C31 1.536(12) . ?
C29 C30 1.393(12) . ?
