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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/7/05/11/7051186.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_7051186
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, InBr4'
_chemical_formula_sum            'C9 H5 Br4 In N S6'
_chemical_formula_weight         753.96
_chemical_name_common            '(EDT-TTF-CN), InBr4'
_chemical_name_systematic
; 
3-cyano -3',4'-ethylenedithiotetrathiafulvalene, tetrabromoindate (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                 106.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.3990(13)
_cell_length_b                   28.687(6)
_cell_length_c                   11.222(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.05
_cell_volume                     1978.9(7)
_computing_cell_refinement       'CELL, Stoe-IPDS'
_computing_data_collection       'EXPOSE, Stoe-IPDS'
_computing_data_reduction        'INTEGRATE, Stoe-IPDS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  ?area_detector
_diffrn_measurement_method       'rotation, phi incr. 0.8'
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0606
_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            15693
_diffrn_reflns_theta_full        25.90
_diffrn_reflns_theta_max         25.90
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    9.894
_exptl_absorpt_correction_T_max  0.4950
_exptl_absorpt_correction_T_min  0.2170
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.3157
_exptl_crystal_size_mid          0.1156
_exptl_crystal_size_min          0.0770
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.771
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.771
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0276
_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          0.0577
_refine_ls_wR_factor_ref         0.0611
_reflns_number_gt                2399
_reflns_number_total             3702
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104640n.txt
_cod_data_source_block           tde120absm
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7051186
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
In1 In 0.11188(6) 0.382465(12) 0.16858(3) 0.03926(10) Uani 1 1 d . . .
Br2 Br 0.04789(10) 0.297203(19) 0.19284(5) 0.05321(16) Uani 1 1 d . . .
Br3 Br 0.07599(9) 0.42515(2) 0.35581(5) 0.05227(16) Uani 1 1 d . . .
Br4 Br 0.49635(10) 0.38553(2) 0.16063(7) 0.0722(2) Uani 1 1 d . . .
Br5 Br -0.11543(11) 0.41825(3) -0.02487(5) 0.0688(2) Uani 1 1 d . . .
S1 S -0.2643(2) 0.28373(5) 0.39880(12) 0.0463(3) Uani 1 1 d . . .
S2 S -0.5766(2) 0.23531(5) 0.50231(13) 0.0501(4) Uani 1 1 d . . .
S3 S 0.6464(2) 0.37880(5) 0.52622(12) 0.0447(3) Uani 1 1 d . . .
S4 S 0.3080(2) 0.33353(4) 0.61063(12) 0.0421(3) Uani 1 1 d . . .
S5 S 0.6327(2) 0.46739(5) 0.65331(13) 0.0524(4) Uani 1 1 d . . .
S6 S 0.2222(3) 0.41246(5) 0.75600(13) 0.0560(4) Uani 1 1 d . . .
C1 C -0.2893(8) 0.22332(17) 0.3799(4) 0.0393(12) Uani 1 1 d . . .
C2 C -0.4327(9) 0.20221(18) 0.4257(4) 0.0465(13) Uani 1 1 d . . .
H2 H -0.4551 0.1702 0.4168 0.056 Uiso 1 1 calc R . .
C3 C -0.4528(8) 0.28709(16) 0.4822(4) 0.0365(11) Uani 1 1 d . . .
C4 C 0.5010(8) 0.32902(16) 0.5316(4) 0.0378(12) Uani 1 1 d . . .
C5 C 0.5349(8) 0.41066(16) 0.6239(4) 0.0374(12) Uani 1 1 d . . .
C6 C 0.3752(8) 0.39006(16) 0.6636(4) 0.0379(12) Uani 1 1 d . . .
C7 C 0.3951(11) 0.4930(2) 0.6824(6) 0.0651(17) Uani 1 1 d . . .
H7A H 0.4220 0.5259 0.6998 0.078 Uiso 1 1 calc R . .
H7B H 0.2745 0.4904 0.6079 0.078 Uiso 1 1 calc R . .
C8 C 0.3318(10) 0.4713(2) 0.7869(5) 0.0628(17) Uani 1 1 d . . .
H8A H 0.2237 0.4909 0.8080 0.075 Uiso 1 1 calc R . .
H8B H 0.4584 0.4703 0.8585 0.075 Uiso 1 1 calc R . .
C9 C -0.1509(10) 0.20041(17) 0.3184(5) 0.0473(14) Uani 1 1 d . . .
N1 N -0.0366(9) 0.18364(17) 0.2680(5) 0.0670(14) Uani 1 1 d . . .
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'
In In -0.7276 1.3100 '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 In1 Br4 107.45(4) . . ?
Br5 In1 Br3 111.44(3) . . ?
Br4 In1 Br3 109.62(3) . . ?
Br5 In1 Br2 115.21(3) . . ?
Br4 In1 Br2 103.37(3) . . ?
Br3 In1 Br2 109.34(3) . . ?
C3 S1 C1 93.8(2) . . ?
C2 S2 C3 94.7(3) . . ?
C4 S3 C5 95.4(2) . . ?
C4 S4 C6 95.8(2) . . ?
C5 S5 C7 98.0(3) . . ?
C6 S6 C8 101.8(3) . . ?
C2 C1 C9 124.8(5) . . ?
C2 C1 S1 117.3(4) . . ?
C9 C1 S1 117.9(4) . . ?
C1 C2 S2 118.1(4) . . ?
C4 C3 S1 121.6(4) 1_455 . ?
C4 C3 S2 122.4(4) 1_455 . ?
S1 C3 S2 116.0(3) . . ?
C3 C4 S4 122.4(4) 1_655 . ?
C3 C4 S3 121.9(4) 1_655 . ?
S4 C4 S3 115.6(3) . . ?
C6 C5 S3 117.3(4) . . ?
C6 C5 S5 127.4(4) . . ?
S3 C5 S5 115.1(3) . . ?
C5 C6 S6 129.5(4) . . ?
C5 C6 S4 115.5(4) . . ?
S6 C6 S4 115.0(3) . . ?
C8 C7 S5 113.7(4) . . ?
C7 C8 S6 114.5(4) . . ?
N1 C9 C1 177.3(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
In1 Br5 2.4755(10) . ?
In1 Br4 2.4880(9) . ?
In1 Br3 2.4969(7) . ?
In1 Br2 2.5072(8) . ?
S1 C3 1.723(5) . ?
S1 C1 1.748(5) . ?
S2 C2 1.711(5) . ?
S2 C3 1.728(5) . ?
S3 C4 1.715(5) . ?
S3 C5 1.726(5) . ?
S4 C4 1.713(5) . ?
S4 C6 1.739(5) . ?
S5 C5 1.742(5) . ?
S5 C7 1.799(7) . ?
S6 C6 1.735(5) . ?
S6 C8 1.824(6) . ?
C1 C2 1.317(7) . ?
C1 C9 1.426(8) . ?
C3 C4 1.390(6) 1_455 ?
C4 C3 1.390(6) 1_655 ?
C5 C6 1.358(7) . ?
C7 C8 1.481(8) . ?
C9 N1 1.147(7) . ?
