#------------------------------------------------------------------------------
#$Date: 2017-11-27 11:41:41 +0200 (Mon, 27 Nov 2017) $
#$Revision: 203615 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/82/1548230.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_1548230
loop_
_publ_author_name
'Sachio Horiuchi'
'Kensuke Kobayashi'
'Reiji Kumai'
'Nao Minami'
'Fumitaka Kagawa'
'Yoshinori Tokura'
_publ_section_title
;
 Quantum ferroelectricity in charge-transfer complex crystals
;
_journal_name_full               'Nature Communications'
_journal_page_first              7469
_journal_paper_doi               10.1038/ncomms8469
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C12 H4 Br2 I2 O2 S4 '
_chemical_formula_sum            'C12 H4 Br2 I2 O2 S4'
_chemical_formula_weight         722.02
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                111.669(10)
_cell_angle_beta                 108.287(7)
_cell_angle_gamma                93.393(10)
_cell_formula_units_Z            1
_cell_length_a                   7.008(2)
_cell_length_b                   7.571(2)
_cell_length_c                   9.696(3)
_cell_measurement_reflns_used    8455
_cell_measurement_temperature    300(1)
_cell_measurement_theta_max      39.6
_cell_measurement_theta_min      2.4
_cell_volume                     444.9(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      300(1)
_diffrn_measured_fraction_theta_full 0.519
_diffrn_measured_fraction_theta_max 0.519
_diffrn_measurement_device_type  Rigaku_IPDSC
_diffrn_measurement_method       IP
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68888
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9351
_diffrn_reflns_theta_full        39.59
_diffrn_reflns_theta_max         39.59
_exptl_absorpt_coefficient_mu    7.723
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             332.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.63
_refine_diff_density_min         -2.58
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     108
_refine_ls_number_reflns         2109
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    6.1007    1.2524    5.0503
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0398
_reflns_number_gt                2098
_reflns_number_total             3059
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ncomms8469-s3.cif
_cod_data_source_block           '_TTF-25QBr2I2_300K'
_cod_original_cell_volume        445.0(2)
_cod_original_formula_sum        'C12 H4 Br2 I2 O2 S4 '
_cod_database_code               1548230
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -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
I(1) I 0.44631(8) -0.20667(9) 0.09866(5) 0.04505(5) Uani 0.92 1 d P . .
I(2) I 0.0612(6) -0.3196(9) 0.2457(5) 0.03942(3) Uani 0.08 1 d P . .
Br(1) Br 0.4677(16) -0.1812(18) 0.1167(14) 0.04432(5) Uani 0.08 1 d P . .
Br(2) Br 0.05393(8) -0.28398(15) 0.24085(7) 0.03905(3) Uani 0.92 1 d P . .
S(1) S 0.40961(11) 0.36000(15) 0.24106(7) 0.0356(2) Uani 1.00 1 d . . .
S(2) S 0.19888(10) 0.34413(15) 0.45783(8) 0.0345(2) Uani 1.00 1 d . . .
O(1) O 0.7942(3) 0.0913(5) 0.4036(3) 0.0480(7) Uani 1.00 1 d . . .
C(1) C 0.6620(3) 0.0463(5) 0.4475(3) 0.0320(7) Uani 1.00 1 d . . .
C(2) C 0.4655(3) -0.0917(5) 0.3322(2) 0.0296(7) Uani 1.00 1 d . . .
C(3) C 0.3130(3) -0.1266(5) 0.3807(3) 0.0285(7) Uani 1.00 1 d . . .
C(4) C 0.4183(3) 0.4380(5) 0.4368(2) 0.0288(7) Uani 1.00 1 d . . .
C(5) C 0.1615(5) 0.2239(6) 0.1566(3) 0.0390(8) Uani 1.00 1 d . . .
C(6) C 0.0656(4) 0.2185(6) 0.2542(3) 0.0384(9) Uani 1.00 1 d . . .
H(1) H 0.113(7) 0.169(7) 0.054(5) 0.045(12) Uiso 1.00 1 d . . .
H(2) H -0.058(9) 0.164(8) 0.235(6) 0.069(16) Uiso 1.00 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 0.0019 0.0015
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.010 0.0057
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Br Br -0.185 2.346
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.488 1.723
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1051 0.1168
;
International Tables for Crystallography
(1992, 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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
Br(1) I(1) C(2) 56(4) yes . . .
Br(2) I(2) C(3) 73.8(7) yes . . .
I(1) Br(1) C(2) 118(4) yes . . .
I(2) Br(2) C(3) 97.6(7) yes . . .
C(4) S(1) C(5) 94.75(15) yes . . .
C(4) S(2) C(6) 94.59(15) yes . . .
O(1) C(1) C(2) 121.7(2) yes . . .
O(1) C(1) C(3) 121.6(2) yes . . 2_656
C(2) C(1) C(3) 116.7(2) yes . . 2_656
I(1) C(2) Br(1) 5.2(3) yes . . .
I(1) C(2) C(1) 114.7(2) yes . . .
I(1) C(2) C(3) 124.25(16) yes . . .
Br(1) C(2) C(1) 109.7(3) yes . . .
Br(1) C(2) C(3) 129.1(3) yes . . .
C(1) C(2) C(3) 121.0(2) yes . . .
I(2) C(3) Br(2) 8.6(2) yes . . .
I(2) C(3) C(1) 112.5(2) yes . . 2_656
I(2) C(3) C(2) 124.5(2) yes . . .
Br(2) C(3) C(1) 114.4(2) yes . . 2_656
Br(2) C(3) C(2) 123.52(19) yes . . .
C(1) C(3) C(2) 122.1(2) yes 2_656 . .
S(1) C(4) S(2) 114.98(12) yes . . .
S(1) C(4) C(4) 122.6(2) yes . . 2_666
S(2) C(4) C(4) 122.4(2) yes . . 2_666
S(1) C(5) C(6) 117.8(2) yes . . .
S(2) C(6) C(5) 117.7(2) yes . . .
S(1) C(5) H(1) 115(3) no . . .
C(6) C(5) H(1) 127(3) no . . .
S(2) C(6) H(2) 111(4) no . . .
C(5) C(6) H(2) 131(4) no . . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
I(1) Br(1) 0.213(10) yes . .
I(1) C(2) 2.060(2) yes . .
I(2) Br(2) 0.295(7) yes . .
I(2) C(3) 1.948(4) yes . .
Br(1) C(2) 1.950(14) yes . .
Br(2) C(3) 1.887(2) yes . .
S(1) C(4) 1.747(2) yes . .
S(1) C(5) 1.740(3) yes . .
S(2) C(4) 1.756(3) yes . .
S(2) C(6) 1.739(2) yes . .
O(1) C(1) 1.214(4) yes . .
C(1) C(2) 1.496(3) yes . .
C(1) C(3) 1.494(3) yes . 2_656
C(2) C(3) 1.344(4) yes . .
C(4) C(4) 1.356(2) yes . 2_666
C(5) C(6) 1.332(5) yes . .
C(5) H(1) 0.87(4) no . .
C(6) H(2) 0.87(6) no . .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
I(1) S(1) 3.5524(9) . 2_655
I(2) S(1) 3.541(6) . 1_545
I(2) C(5) 3.414(8) . 1_545
I(2) C(6) 3.531(8) . 1_545
S(1) I(1) 3.5524(9) . 2_655
S(1) I(2) 3.541(6) . 1_565
S(2) O(1) 3.108(3) . 1_455
S(2) C(1) 3.509(4) . 2_656
S(2) C(3) 3.556(4) . .
O(1) S(2) 3.108(3) . 1_655
O(1) O(1) 3.567(4) . 2_756
O(1) C(6) 3.031(5) . 1_655
C(1) S(2) 3.509(4) . 2_656
C(1) C(4) 3.527(5) . .
C(3) S(2) 3.556(4) . .
C(3) C(6) 3.593(6) . .
C(4) C(1) 3.527(5) . .
C(5) I(2) 3.414(8) . 1_565
C(6) I(2) 3.531(8) . 1_565
C(6) O(1) 3.031(5) . 1_455
C(6) C(3) 3.593(6) . .
I(2) H(1) 3.41(6) . 2_555
Br(2) H(1) 3.18(6) . 2_555
Br(2) H(2) 3.55(7) . .
O(1) H(2) 2.39(8) . 1_655
C(1) H(2) 3.55(7) . 1_655
C(5) H(1) 3.01(4) . 2_555
C(6) H(1) 3.13(4) . 2_555
H(1) I(2) 3.41(6) . 2_555
H(1) Br(2) 3.18(6) . 2_555
H(1) C(5) 3.01(4) . 2_555
H(1) C(6) 3.13(4) . 2_555
H(1) H(1) 2.57(7) . 2_555
H(1) H(2) 2.88(7) . 2_555
H(2) Br(2) 3.55(7) . .
H(2) O(1) 2.39(8) . 1_455
H(2) C(1) 3.55(7) . 1_455
H(2) H(1) 2.88(7) . 2_555
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Br(1) I(1) C(2) C(1) -18(4) . . . .
Br(1) I(1) C(2) C(3) 159(4) . . . .
Br(2) I(2) C(3) C(2) -86.4(10) . . . .
Br(2) I(2) C(3) C(1) 104.5(10) . . . 2_656
I(1) Br(1) C(2) C(1) 163(3) . . . .
I(1) Br(1) C(2) C(3) -23(4) . . . .
I(2) Br(2) C(3) C(2) 99.4(10) . . . .
I(2) Br(2) C(3) C(1) -79.2(10) . . . 2_656
C(4) S(1) C(5) C(6) -0.8(4) . . . .
C(5) S(1) C(4) S(2) 2.5(2) . . . .
C(5) S(1) C(4) C(4) -177.3(3) . . . 2_666
C(4) S(2) C(6) C(5) 2.6(4) . . . .
C(6) S(2) C(4) S(1) -3.0(2) . . . .
C(6) S(2) C(4) C(4) 176.8(3) . . . 2_666
O(1) C(1) C(2) I(1) 2.9(5) . . . .
O(1) C(1) C(2) Br(1) 1.2(6) . . . .
O(1) C(1) C(2) C(3) -173.9(4) . . . .
O(1) C(1) C(3) I(2) 4.4(5) . . 2_656 2_656
O(1) C(1) C(3) Br(2) -4.8(5) . . 2_656 2_656
O(1) C(1) C(3) C(2) 173.8(4) . . 2_656 2_656
C(2) C(1) C(3) I(2) -175.4(3) . . 2_656 2_656
C(2) C(1) C(3) Br(2) 175.5(2) . . 2_656 2_656
C(2) C(1) C(3) C(2) -5.9(6) . . 2_656 2_656
C(3) C(1) C(2) I(1) -177.3(2) 2_656 . . .
C(3) C(1) C(2) Br(1) -179.1(5) 2_656 . . .
C(3) C(1) C(2) C(3) 5.8(5) 2_656 . . .
I(1) C(2) C(3) I(2) 9.2(6) . . . .
I(1) C(2) C(3) Br(2) -1.2(5) . . . .
I(1) C(2) C(3) C(1) 177.3(3) . . . 2_656
Br(1) C(2) C(3) I(2) 11.6(8) . . . .
Br(1) C(2) C(3) Br(2) 1.3(8) . . . .
Br(1) C(2) C(3) C(1) 179.8(3) . . . 2_656
C(1) C(2) C(3) I(2) -174.3(3) . . . .
C(1) C(2) C(3) Br(2) 175.3(3) . . . .
C(1) C(2) C(3) C(1) -6.2(6) . . . 2_656
S(1) C(4) C(4) S(2) -0.2(3) . . 2_666 2_666
S(2) C(4) C(4) S(1) 0.2(3) . . 2_666 2_666
S(1) C(5) C(6) S(2) -1.3(5) . . . .
