#------------------------------------------------------------------------------
#$Date: 2017-05-30 17:58:23 +0300 (Tue, 30 May 2017) $
#$Revision: 197043 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/26/2012640.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_2012640
loop_
_publ_author_name
'Pilia, Luca'
'Faulmann, Christophe'
'Malfant, Isabelle'
'Collière, Vincent'
'Mercuri, Maria Laura'
'Deplano, Paola'
'Cassoux, Patrick'
_publ_section_title
;
 (BETS)₂[Fe(tdas)₂]₂: a new metal in the molecular conductor
 family
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m240
_journal_page_last               m242
_journal_paper_doi               10.1107/S010827010200330X
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C10 H8 S4 Se4)2 [Fe2 (C2 N2 S3)4]'
_chemical_formula_moiety         '2C10 H8 S4 Se4 + , C8 Fe2 N8 S12 2-'
_chemical_formula_sum            'C28 H16 Fe2 N8 S20 Se8'
_chemical_formula_weight         1849.06
_chemical_name_common            (BETS)Fe(tdas)₂
_chemical_name_systematic
;
bis[4,5-ethylenedithio-2-(4,5-ethylenedithio-1,3-diselenacyclopent-4-en-2-
ylidene)-1,3-diselenacyclopent-4-enium]
bis(μ-1,2,5-thiadiazole-3,4-dithiolato-κ³S⁴,S⁵:S⁴)-
bis[(1,2,5-thiadiazole-3,4-dithiolato-κ²S⁴,S⁵)iron(III)]
;
_space_group_IT_number           2
_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
_cell_angle_alpha                109.293(14)
_cell_angle_beta                 99.966(16)
_cell_angle_gamma                95.140(10)
_cell_formula_units_Z            1
_cell_length_a                   8.5466(12)
_cell_length_b                   12.1018(16)
_cell_length_c                   12.9993(16)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2
_cell_volume                     1234.2(3)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        IPDS
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       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  0.061
_diffrn_reflns_av_sigmaI/netI    0.053
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13154
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         2.00
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    7.372
_exptl_absorpt_correction_T_max  0.478
_exptl_absorpt_correction_T_min  0.429
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(Parkin et al., 1995) Cubic fit to sinθ/λ with 24 parameters.
Correction applied to the full data set.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.488
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.89
_refine_diff_density_min         -0.82
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.049
_refine_ls_R_factor_gt           0.033
_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)+(0.0374P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.068
_refine_ls_wR_factor_ref         0.073
_reflns_number_gt                3449
_reflns_number_total             4503
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            jz1495.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

2017-05-15
Formula fixed to be consistent with Z value
The compound is indeed dinuclear                 miguel
;
_cod_original_formula_sum            'C14 H8 Fe N4 S10 Se4'
_cod_original_formula_iupac          '(C10 H8 S4 Se4) [Fe2 (C2 N2 S3)4]'
_cod_database_code               2012640
_cod_database_fobs_code          2012640
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Se1 0.10529(5) 0.38166(4) 0.21999(4) 0.01394(12) Uani d . 1 . . Se
Se2 0.34615(5) 0.37223(3) 0.42946(4) 0.01019(11) Uani d . 1 . . Se
Se3 0.00052(5) 0.63386(4) 0.38264(4) 0.01563(12) Uani d . 1 . . Se
Se4 0.24385(5) 0.62543(3) 0.59168(4) 0.01130(11) Uani d . 1 . . Se
S1 0.16674(15) 0.14254(11) 0.06888(11) 0.0257(3) Uani d . 1 . . S
S2 0.43263(13) 0.13689(9) 0.30128(10) 0.0164(3) Uani d . 1 . . S
S4 0.16678(14) 0.85778(10) 0.74588(11) 0.0193(3) Uani d . 1 . . S
S3 -0.10301(14) 0.86119(9) 0.51426(11) 0.0204(3) Uani d . 1 . . S
C1 0.1935(5) 0.4515(3) 0.3735(4) 0.0102(9) Uani d . 1 . . C
C2 0.1507(5) 0.5537(3) 0.4395(4) 0.0115(9) Uani d . 1 . . C
C3 0.2142(5) 0.2510(3) 0.2024(4) 0.0126(10) Uani d . 1 . . C
C4 0.3173(5) 0.2458(3) 0.2917(4) 0.0109(9) Uani d . 1 . . C
C5 0.0238(5) 0.7563(3) 0.5211(4) 0.0137(10) Uani d . 1 . . C
C6 0.1257(5) 0.7522(3) 0.6105(4) 0.0122(10) Uani d . 1 . . C
C7 0.3525(6) 0.0824(4) 0.0700(4) 0.0207(11) Uani d . 1 . . C
H7A 0.3460 0.0204 -0.0035 0.025 Uiso calc R 1 . . H
H7B 0.4419 0.1461 0.0814 0.025 Uiso calc R 1 . . H
C8 0.3886(6) 0.0297(4) 0.1601(4) 0.0190(11) Uani d . 1 . . C
H8A 0.4818 -0.0125 0.1490 0.023 Uiso calc R 1 . . H
H8B 0.2951 -0.0296 0.1515 0.023 Uiso calc R 1 . . H
C9 -0.0451(6) 0.9745(4) 0.6518(5) 0.0251(12) Uani d . 1 . . C
H9A -0.0638 1.0517 0.6453 0.030 Uiso calc R 1 . . H
H9B -0.1158 0.9568 0.6990 0.030 Uiso calc R 1 . . H
C10 0.1282(6) 0.9863(4) 0.7102(5) 0.0236(12) Uani d . 1 . . C
H10A 0.1537 1.0575 0.7791 0.028 Uiso calc R 1 . . H
H10B 0.1997 0.9976 0.6609 0.028 Uiso calc R 1 . . H
Fe11 0.58858(7) 0.53843(5) 0.12290(5) 0.00994(15) Uani d . 1 . . Fe
S11 0.67885(14) 0.36917(9) 0.12074(10) 0.0163(3) Uani d . 1 . . S
S12 0.92605(14) 0.25783(10) -0.12913(11) 0.0213(3) Uani d . 1 . . S
S13 0.69297(12) 0.54212(9) -0.02362(10) 0.0112(2) Uani d . 1 . . S
S14 0.60282(14) 0.73501(9) 0.16334(10) 0.0155(3) Uani d . 1 . . S
S15 0.53959(13) 0.55249(9) 0.28927(10) 0.0139(2) Uani d . 1 . . S
S16 0.39416(16) 0.87059(10) 0.42992(11) 0.0227(3) Uani d . 1 . . S
N11 0.8512(4) 0.2466(3) -0.0236(3) 0.0185(9) Uani d . 1 . . N
N12 0.8626(4) 0.3795(3) -0.1349(4) 0.0192(9) Uani d . 1 . . N
N13 0.4192(4) 0.7342(3) 0.4201(3) 0.0170(9) Uani d . 1 . . N
N14 0.4709(5) 0.8780(3) 0.3240(3) 0.0197(9) Uani d . 1 . . N
C11 0.7752(5) 0.3375(4) 0.0097(4) 0.0156(10) Uani d . 1 . . C
C12 0.7827(5) 0.4137(4) -0.0544(4) 0.0128(10) Uani d . 1 . . C
C13 0.4846(5) 0.6922(3) 0.3339(4) 0.0113(9) Uani d . 1 . . C
C14 0.5145(5) 0.7748(4) 0.2784(4) 0.0123(9) Uani d . 1 . . C
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'
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'
Se Se -0.0929 2.2259 '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_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C3 Se1 C1 . 93.91(18) ?
C1 Se2 C4 . 93.82(18) ?
C2 Se3 C5 . 93.52(19) ?
C2 Se4 C6 . 93.60(18) ?
C3 S1 C7 . 99.4(2) ?
C4 S2 C8 . 103.8(2) ?
C6 S4 C10 . 98.5(2) ?
C5 S3 C9 . 103.8(2) ?
C2 C1 Se2 . 122.7(3) ?
C2 C1 Se1 . 122.5(3) ?
Se2 C1 Se1 . 114.8(2) ?
C1 C2 Se4 . 122.3(3) ?
C1 C2 Se3 . 122.5(3) ?
Se4 C2 Se3 . 115.2(2) ?
C4 C3 S1 . 125.5(3) ?
C4 C3 Se1 . 119.1(3) ?
S1 C3 Se1 . 115.4(2) ?
C3 C4 S2 . 129.5(3) ?
C3 C4 Se2 . 118.2(3) ?
S2 C4 Se2 . 112.3(2) ?
C6 C5 S3 . 128.6(4) ?
C6 C5 Se3 . 119.0(3) ?
S3 C5 Se3 . 112.4(3) ?
C5 C6 S4 . 126.2(3) ?
C5 C6 Se4 . 118.6(3) ?
S4 C6 Se4 . 115.1(2) ?
C8 C7 S1 . 112.5(4) ?
C8 C7 H7A . 109.1 ?
S1 C7 H7A . 109.1 ?
C8 C7 H7B . 109.1 ?
S1 C7 H7B . 109.1 ?
H7A C7 H7B . 107.8 ?
C7 C8 S2 . 114.5(3) ?
C7 C8 H8A . 108.6 ?
S2 C8 H8A . 108.6 ?
C7 C8 H8B . 108.6 ?
S2 C8 H8B . 108.6 ?
H8A C8 H8B . 107.6 ?
C10 C9 S3 . 114.8(3) ?
C10 C9 H9A . 108.6 ?
S3 C9 H9A . 108.6 ?
C10 C9 H9B . 108.6 ?
S3 C9 H9B . 108.6 ?
H9A C9 H9B . 107.6 ?
C9 C10 S4 . 112.0(3) ?
C9 C10 H10A . 109.2 ?
S4 C10 H10A . 109.2 ?
C9 C10 H10B . 109.2 ?
S4 C10 H10B . 109.2 ?
H10A C10 H10B . 107.9 ?
S15 Fe11 S11 . 85.95(5) ?
S15 Fe11 S14 . 91.82(5) ?
S11 Fe11 S14 . 156.47(5) ?
S15 Fe11 S13 . 167.46(5) ?
S11 Fe11 S13 . 92.48(5) ?
S14 Fe11 S13 . 84.66(5) ?
S15 Fe11 S13 2_665 93.89(5) ?
S11 Fe11 S13 2_665 99.56(4) ?
S14 Fe11 S13 2_665 103.96(5) ?
S13 Fe11 S13 2_665 98.64(4) ?
C11 S11 Fe11 . 102.66(16) yes
N12 S12 N11 . 99.2(2) ?
C12 S13 Fe11 . 102.29(17) yes
C12 S13 Fe11 2_665 101.60(13) ?
Fe11 S13 Fe11 2_665 81.36(4) ?
C14 S14 Fe11 . 101.42(14) yes
C13 S15 Fe11 . 101.75(17) yes
N14 S16 N13 . 98.9(2) ?
C11 N11 S12 . 107.1(3) ?
C12 N12 S12 . 106.2(3) ?
C13 N13 S16 . 106.5(3) ?
C14 N14 S16 . 106.8(3) ?
N11 C11 C12 . 112.8(4) ?
N11 C11 S11 . 125.6(4) ?
C12 C11 S11 . 121.6(3) ?
N12 C12 C11 . 114.8(4) ?
N12 C12 S13 . 124.2(4) ?
C11 C12 S13 . 121.0(4) ?
N13 C13 C14 . 114.2(4) ?
N13 C13 S15 . 124.9(4) ?
C14 C13 S15 . 120.8(4) ?
N14 C14 C13 . 113.6(4) ?
N14 C14 S14 . 125.8(4) ?
C13 C14 S14 . 120.6(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Se1 C3 . 1.875(4) ?
Se1 C1 . 1.875(4) ?
Se2 C1 . 1.873(4) ?
Se2 C4 . 1.892(4) ?
Se3 C2 . 1.872(4) ?
Se3 C5 . 1.880(5) ?
Se4 C2 . 1.870(5) ?
Se4 C6 . 1.883(4) ?
S1 C3 . 1.748(4) ?
S1 C7 . 1.804(5) ?
S2 C4 . 1.739(4) ?
S2 C8 . 1.815(5) ?
S4 C6 . 1.753(4) ?
S4 C10 . 1.806(5) ?
S3 C5 . 1.755(4) ?
S3 C9 . 1.810(5) ?
C1 C2 . 1.374(6) ?
C3 C4 . 1.353(6) ?
C5 C6 . 1.345(7) ?
C7 C8 . 1.509(7) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 C10 . 1.513(7) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
Fe11 S15 . 2.2282(15) yes
Fe11 S11 . 2.2460(12) yes
Fe11 S14 . 2.2473(12) yes
Fe11 S13 . 2.2500(14) yes
Fe11 S13 2_665 2.4656(12) ?
S11 C11 . 1.735(5) yes
S12 N12 . 1.634(4) ?
S12 N11 . 1.650(5) ?
S13 C12 . 1.753(4) yes
S13 Fe11 2_665 2.4656(12) ?
S14 C14 . 1.737(5) yes
S15 C13 . 1.734(4) yes
S16 N14 . 1.648(5) ?
S16 N13 . 1.650(4) ?
N11 C11 . 1.316(5) ?
N12 C12 . 1.321(6) ?
N13 C13 . 1.311(6) ?
N14 C14 . 1.311(6) ?
C11 C12 . 1.437(7) ?
C13 C14 . 1.442(6) ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Se1 S11 3.6220(10) 1_455 yes
Se3 S15 3.8500(10) 1_455 yes
Se2 S15 3.3990(10) 2_666 yes
Se4 S11 3.660(2) 2_666 yes
Se4 S15 3.5190(10) 2_666 yes
S2 S16 3.585(2) 2_666 yes
Se1 S13 3.624(2) 2_665 yes
