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#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/11/7051187.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_7051187
loop_
_publ_author_name
'Thomas Devic'
'Josep N. Bertran'
'Benoît Domercq'
'Enric Canadell'
'Narcis Avarvari'
'Pascale Auban-Senzier'
'Marc Fourmigué'
_publ_section_title
;
 Cation radical salts of cyano(ethylenedithio)tetrathiafulvalene with
 halogenated anions: annihilation of the CN···Hal
 interaction and stabilisation of conducting, antiferromagnetic square
 or chain-type salts
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              1418
_journal_page_last               1424
_journal_paper_doi               10.1039/b104640n
_journal_volume                  25
_journal_year                    2001
_chemical_formula_moiety         'C9H5NS6, FeBr4'
_chemical_formula_sum            'C9 H5 Br4 Fe N S6'
_chemical_formula_weight         694.99
_chemical_name_common            'EDT-TTF-CN, FeBr4'
_chemical_name_systematic
; 
3-cyano -3',4'-ethylenedithiotetrathiafulvalene, tetrabromoferrate (III)  
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 106.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.2930(13)
_cell_length_b                   28.506(6)
_cell_length_c                   11.126(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.89
_cell_measurement_theta_min      9.31
_cell_volume                     1913.5(7)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 EXPRESS'
_computing_data_reduction        'XCAD4 [Harms, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       w--2q
_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  0.1134
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3859
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.785
_exptl_absorpt_correction_T_max  0.12123
_exptl_absorpt_correction_T_min  0.03499
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SHELXTL
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.931
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.637
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.637
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_gt           0.0486
_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)+(0.0260P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                2124
_reflns_number_total             3757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104640n.txt
_cod_data_source_block           tde41cm
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7051187
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.11211(17) 0.38033(4) 0.16910(10) 0.0443(3) Uani 1 1 d . . .
Br2 Br 0.04323(14) 0.30027(3) 0.18986(8) 0.0582(3) Uani 1 1 d . . .
Br3 Br 0.07612(13) 0.42107(3) 0.34469(8) 0.0564(2) Uani 1 1 d . . .
Br4 Br 0.47607(14) 0.38333(3) 0.16052(10) 0.0726(3) Uani 1 1 d . . .
Br5 Br -0.11124(15) 0.41420(4) -0.01258(9) 0.0713(3) Uani 1 1 d . . .
S1 S -0.2633(3) 0.28517(7) 0.3983(2) 0.0507(5) Uani 1 1 d . . .
S2 S -0.5836(3) 0.23781(7) 0.5021(2) 0.0526(5) Uani 1 1 d . . .
C1 C -0.2917(12) 0.2250(2) 0.3783(7) 0.0417(18) Uani 1 1 d . . .
C2 C -0.4408(12) 0.2038(3) 0.4231(7) 0.0472(19) Uani 1 1 d . . .
H2 H -0.4673 0.1718 0.4123 0.057 Uiso 1 1 calc R . .
C3 C -0.4555(11) 0.2893(2) 0.4807(7) 0.0422(18) Uani 1 1 d . . .
C9 C -0.1501(12) 0.2007(3) 0.3181(7) 0.0470(19) Uani 1 1 d . . .
N1 N -0.0350(12) 0.1833(2) 0.2693(7) 0.065(2) Uani 1 1 d . . .
S3 S -0.3492(3) 0.38129(7) 0.52785(19) 0.0465(5) Uani 1 1 d . . .
S4 S -0.6955(3) 0.33599(7) 0.61070(19) 0.0463(5) Uani 1 1 d . . .
S5 S -0.3583(4) 0.46978(7) 0.6584(2) 0.0579(6) Uani 1 1 d . . .
S6 S -0.7776(4) 0.41513(7) 0.7596(2) 0.0612(6) Uani 1 1 d . . .
C4 C -0.4973(10) 0.3307(2) 0.5303(6) 0.0351(17) Uani 1 1 d . . .
C5 C -0.4601(11) 0.4136(2) 0.6287(7) 0.0421(18) Uani 1 1 d . . .
C6 C -0.6247(11) 0.3920(2) 0.6645(7) 0.0410(18) Uani 1 1 d . . .
C7 C -0.6003(14) 0.4966(3) 0.6868(9) 0.067(3) Uani 1 1 d . . .
H7A H -0.5693 0.5295 0.7070 0.081 Uiso 1 1 calc R . .
H7B H -0.7224 0.4950 0.6106 0.081 Uiso 1 1 calc R . .
C8 C -0.6685(15) 0.4738(3) 0.7906(9) 0.069(3) Uani 1 1 d . . .
H8A H -0.7801 0.4933 0.8107 0.082 Uiso 1 1 calc R . .
H8B H -0.5411 0.4728 0.8642 0.082 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
Br5 Fe1 Br4 108.02(6) . . ?
Br5 Fe1 Br3 110.05(6) . . ?
Br4 Fe1 Br3 110.32(6) . . ?
Br5 Fe1 Br2 114.05(6) . . ?
Br4 Fe1 Br2 104.59(5) . . ?
Br3 Fe1 Br2 109.65(5) . . ?
Fe1 Br2 N1 171.48(13) . . ?
C3 S1 C1 94.3(4) . . ?
C2 S2 C3 94.4(4) . . ?
C2 C1 C9 123.7(7) . . ?
C2 C1 S1 117.4(6) . . ?
C9 C1 S1 118.9(6) . . ?
C1 C2 S2 117.6(6) . . ?
C4 C3 S1 121.6(5) . . ?
C4 C3 S2 122.0(5) . . ?
S1 C3 S2 116.3(4) . . ?
N1 C9 C1 177.0(9) . . ?
C9 N1 Br2 82.0(5) . . ?
C4 S3 C5 96.6(3) . . ?
C6 S4 C4 96.2(3) . . ?
C5 S5 C7 98.1(4) . . ?
C6 S6 C8 102.7(4) . . ?
C3 C4 S3 123.5(5) . . ?
C3 C4 S4 122.4(5) . . ?
S3 C4 S4 114.0(4) . . ?
C6 C5 S5 129.6(6) . . ?
C6 C5 S3 115.4(6) . . ?
S5 C5 S3 114.8(4) . . ?
C5 C6 S4 117.5(6) . . ?
C5 C6 S6 127.2(6) . . ?
S4 C6 S6 115.3(4) . . ?
C8 C7 S5 113.1(6) . . ?
C7 C8 S6 115.7(6) . . ?
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 Br5 2.3190(15) . ?
Fe1 Br4 2.3209(14) . ?
Fe1 Br3 2.3383(14) . ?
Fe1 Br2 2.3467(14) . ?
Br2 N1 3.518(7) . ?
S1 C3 1.717(7) . ?
S1 C1 1.732(7) . ?
S2 C2 1.722(7) . ?
S2 C3 1.724(7) . ?
C1 C2 1.327(9) . ?
C1 C9 1.436(10) . ?
C3 C4 1.358(9) . ?
C9 N1 1.136(9) . ?
S3 C4 1.722(7) . ?
S3 C5 1.743(8) . ?
S4 C6 1.720(7) . ?
S4 C4 1.736(7) . ?
S5 C5 1.722(7) . ?
S5 C7 1.810(8) . ?
S6 C6 1.748(7) . ?
S6 C8 1.802(8) . ?
C5 C6 1.358(10) . ?
C7 C8 1.492(11) . ?
