#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/40/7204069.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_7204069
loop_
_publ_author_name
'Benoît Domercq'
'Thomas Devic'
'Marc Fourmigué'
'Pascale Auban-Senzier'
'Enric Canadell'
_publ_section_title
;
 HalHal interactions in a series of three isostructural salts of
 halogenated tetrathiafulvalenes. Contribution of the halogen atoms to
 the HOMO--HOMO overlap interactions
;
_journal_issue                   6
_journal_name_full               'J. Mater. Chem.'
_journal_page_first              1570
_journal_page_last               1575
_journal_paper_doi               10.1039/b100103p
_journal_volume                  11
_journal_year                    2001
_chemical_formula_moiety         '2(C8H4S6BR2), I3'
_chemical_formula_sum            'C8 H4 Br2 I1.5 S6'
_chemical_formula_weight         642.64
_chemical_name_common            '2(EDT-TTF-BR2), I3'
_chemical_name_systematic
; 
Bis(3,4-dibromo-3',4'-ethylenedithiotetrathiafulvalene)
triiodide
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.61(3)
_cell_angle_beta                 99.74(3)
_cell_angle_gamma                103.10(3)
_cell_formula_units_Z            2
_cell_length_a                   6.7796(14)
_cell_length_b                   7.5112(15)
_cell_length_c                   16.117(3)
_cell_measurement_reflns_used    6017
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.95
_cell_measurement_theta_min      2.6
_cell_volume                     779.9(3)
_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 0.934
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'rotation, phi incr. 1.4'
_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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7779
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    8.946
_exptl_absorpt_correction_T_max  0.5689
_exptl_absorpt_correction_T_min  0.2375
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             595
_exptl_crystal_size_max          0.3273
_exptl_crystal_size_mid          0.1155
_exptl_crystal_size_min          0.0674
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.845
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.845
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0256
_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)+(0.0190P)²+0.0000P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0527
_reflns_number_gt                2182
_reflns_number_total             2854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100103p.txt
_cod_data_source_block           tde89absm
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C8 H4 Br2 I1.50 S6'
_cod_database_code               7204069
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
I1 I 0.5000 0.5000 0.0000 0.03460(12) Uani 1 2 d S . .
I2 I 0.13110(6) 0.27030(5) 0.03999(2) 0.04567(11) Uani 1 1 d . . .
Br1 Br 0.50528(7) 1.50417(7) 0.26618(3) 0.03769(13) Uani 1 1 d . . .
Br2 Br 0.97927(7) 1.49884(6) 0.21009(3) 0.03363(13) Uani 1 1 d . . .
S1 S 0.76282(18) 1.67647(17) 0.44328(7) 0.0329(3) Uani 1 1 d . . .
S2 S 1.16328(18) 1.66956(17) 0.39717(7) 0.0324(3) Uani 1 1 d . . .
S3 S 0.99868(18) 1.14001(16) 0.36504(7) 0.0314(3) Uani 1 1 d . . .
S4 S 0.60247(18) 1.14852(16) 0.41306(7) 0.0326(3) Uani 1 1 d . . .
S5 S 0.81517(19) 0.96659(17) 0.18689(7) 0.0350(3) Uani 1 1 d . . .
S6 S 0.34544(19) 0.98203(18) 0.24708(8) 0.0392(3) Uani 1 1 d . . .
C1 C 0.7630(7) 1.5931(6) 0.3385(3) 0.0268(10) Uani 1 1 d . . .
C2 C 0.9428(7) 1.5904(6) 0.3172(3) 0.0283(10) Uani 1 1 d . . .
C3 C 1.0314(7) 1.7260(6) 0.4755(3) 0.0292(10) Uani 1 1 d . . .
C4 C 0.8688(7) 1.1958(6) 0.4438(3) 0.0277(10) Uani 1 1 d . . .
C5 C 0.7754(7) 1.0481(6) 0.2861(3) 0.0268(10) Uani 1 1 d . . .
C6 C 0.5935(7) 1.0536(5) 0.3086(3) 0.0267(10) Uani 1 1 d . . .
C7 C 0.5856(9) 1.0015(7) 0.1225(3) 0.0372(12) Uani 1 1 d . . .
H7A H 0.589(8) 1.118(7) 0.123(3) 0.035(14) Uiso 1 1 d . . .
H7B H 0.587(10) 0.950(8) 0.064(4) 0.07(2) Uiso 1 1 d . . .
C8 C 0.3875(9) 0.8980(7) 0.1444(3) 0.0370(12) Uani 1 1 d . . .
H8A H 0.256(9) 0.899(8) 0.107(4) 0.060(17) Uiso 1 1 d . . .
H8B H 0.396(10) 0.756(9) 0.146(4) 0.08(2) Uiso 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'
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'
I I -0.4742 1.8119 '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
I2 I1 I2 180.0 2_665 . ?
C1 S1 C3 94.5(2) . . ?
C3 S2 C2 95.1(2) . . ?
C4 S3 C5 95.5(2) . . ?
C4 S4 C6 95.5(2) . . ?
C5 S5 C7 98.3(2) . . ?
C6 S6 C8 103.4(2) . . ?
C2 C1 S1 118.2(3) . . ?
C2 C1 Br1 125.2(3) . . ?
S1 C1 Br1 116.6(3) . . ?
C1 C2 S2 117.2(3) . . ?
C1 C2 Br2 125.6(3) . . ?
S2 C2 Br2 117.2(3) . . ?
C4 C3 S2 122.2(4) 2_786 . ?
C4 C3 S1 122.7(4) 2_786 . ?
S2 C3 S1 115.1(2) . . ?
C3 C4 S4 122.0(4) 2_786 . ?
C3 C4 S3 122.6(4) 2_786 . ?
S4 C4 S3 115.5(2) . . ?
C6 C5 S5 127.5(3) . . ?
C6 C5 S3 116.4(3) . . ?
S5 C5 S3 116.0(3) . . ?
C5 C6 S6 128.9(3) . . ?
C5 C6 S4 117.2(3) . . ?
S6 C6 S4 113.9(3) . . ?
C8 C7 S5 113.7(4) . . ?
C7 C8 S6 114.2(3) . . ?
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
I1 I2 2.9075(10) 2_665 ?
I1 I2 2.9075(10) . ?
Br1 C1 1.867(4) . ?
Br2 C2 1.872(4) . ?
S1 C1 1.743(4) . ?
S1 C3 1.749(5) . ?
S2 C3 1.739(5) . ?
S2 C2 1.744(5) . ?
S3 C4 1.733(5) . ?
S3 C5 1.757(4) . ?
S4 C4 1.733(5) . ?
S4 C6 1.748(4) . ?
S5 C5 1.742(4) . ?
S5 C7 1.806(6) . ?
S6 C6 1.739(5) . ?
S6 C8 1.804(5) . ?
C1 C2 1.325(7) . ?
C3 C4 1.366(6) 2_786 ?
C4 C3 1.366(6) 2_786 ?
C5 C6 1.351(6) . ?
C7 C8 1.508(8) . ?
