#------------------------------------------------------------------------------
#$Date: 2019-11-17 15:38:40 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230932 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/01/7230192.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_7230192
loop_
_publ_author_name
'Zakharov, Boris A.'
'Michalchuk, Adam A. L.'
'Morrison, Carole A.'
'Boldyreva, Elena V.'
_publ_section_title
;
 Anisotropic lattice softening near the structural phase transition in the
 thermosalient crystal 1,2,4,5-tetrabromobenzene.
;
_journal_issue                   13
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              8523
_journal_page_last               8532
_journal_paper_doi               10.1039/c7cp08609a
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C6 H2 Br4'
_chemical_formula_sum            'C6 H2 Br4'
_chemical_formula_weight         393.72
_chemical_name_common            1,2,4,5-tetrabromobenzene
_chemical_name_systematic        1,2,4,5-tetrabromobenzene
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-10-10 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.585(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.0549(3)
_cell_length_b                   11.0780(5)
_cell_length_c                   9.8719(5)
_cell_measurement_reflns_used    1482
_cell_measurement_temperature    313(2)
_cell_measurement_theta_max      28.1770
_cell_measurement_theta_min      4.2260
_cell_volume                     435.90(4)
_computing_cell_refinement
'CrysAlisPro 1.171.39.23a (Rigaku Oxford Diffraction, 2015)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2013)'
_computing_data_reduction
'CrysAlisPro 1.171.39.23a (Rigaku Oxford Diffraction, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      313(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3020
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.790
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    18.385
_exptl_absorpt_correction_T_max  0.561
_exptl_absorpt_correction_T_min  0.046
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.23a (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.000
_exptl_crystal_description       prism
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.720
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0523P)²+0.1883P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                725
_reflns_number_total             891
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cp08609a2.cif
_cod_data_source_block           TBB_313K
_cod_depositor_comments
'Adding full bibliography for 7230191--7230198.cif.'
_cod_database_code               7230192
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.027
_shelx_estimated_absorpt_t_max   0.609
_shelx_res_file
;
TITL 313
    TBB_313K.res
    created by SHELXL-2017/1 at 11:34:07 on 10-Oct-2017
CELL  0.71073  4.05490 11.07801  9.87189 90.00000 100.58460 90.00000
ZERR 2  0.00026  0.00048  0.00046  0.00000  0.00540  0.00000
LATT 1
SYMM -X+ 0.50000, Y+ 0.50000, -Z+ 0.50000
SFAC BR C H
UNIT 8 12 4
TEMP 40
SIZE 0.72 0.11 0.03
LIST 4
L.S. 50
FMAP 2
PLAN 20
SHEL 50 0.8
CONF
BOND
BOND $H
ACTA
WGHT    0.052300    0.188300
EXTI    0.014929
FVAR       1.20623
BR1   1    0.545629    0.783295    0.594741    11.00000    0.08243    0.04263 =
         0.05464   -0.00550    0.02059   -0.00227
BR2   1    0.328983    0.568312    0.802004    11.00000    0.06966    0.05699 =
         0.04151   -0.00397    0.02203    0.00063
C1    2    0.518389    0.619179    0.542817    11.00000    0.04101    0.03913 =
         0.03970   -0.00229    0.00731    0.00155
C2    2    0.426027    0.530137    0.627186    11.00000    0.03409    0.05099 =
         0.03344   -0.00236    0.00808    0.00040
C3    2    0.405937    0.411446    0.584988    11.00000    0.04671    0.04726 =
         0.03644    0.00310    0.00742   -0.00069
AFIX  43
H3    3    0.342170    0.351991    0.641500    11.00000   -1.20000
AFIX   0
HKLF 4




REM  313
REM R1 =  0.0333 for     725 Fo > 4sig(Fo)  and  0.0447 for all     891 data
REM     47 parameters refined using      0 restraints

END

WGHT      0.0523      0.1883

REM Highest difference peak  0.669,  deepest hole -0.430,  1-sigma level  0.133
Q1    1   0.3879  0.7560  0.5268  11.00000  0.05    0.67
Q2    1   0.4581  0.5219  0.8656  11.00000  0.05    0.51
Q3    1   0.7083  0.7562  0.5815  11.00000  0.05    0.51
Q4    1   0.1185  0.5574  0.8434  11.00000  0.05    0.47
Q5    1   0.4904  0.6130  0.8895  11.00000  0.05    0.45
Q6    1   0.5984  0.5865  0.8809  11.00000  0.05    0.45
Q7    1   0.4995  0.5173  0.7644  11.00000  0.05    0.40
Q8    1   0.1279  0.7791  0.4296  11.00000  0.05    0.40
Q9    1   0.5703  0.5972  0.7527  11.00000  0.05    0.39
Q10   1   0.0051  0.5477  0.7482  11.00000  0.05    0.38
Q11   1   0.1660  0.6089  0.4822  11.00000  0.05    0.38
Q12   1   0.7201  0.7768  0.7148  11.00000  0.05    0.35
Q13   1   0.0829  0.5193  0.5461  11.00000  0.05    0.33
Q14   1   0.6391  0.6625  0.7468  11.00000  0.05    0.33
Q15   1   0.3918  0.6361  0.7665  11.00000  0.05    0.32
Q16   1   0.6954  0.5639  0.9596  11.00000  0.05    0.32
Q17   1   0.5475  0.3771  0.7375  11.00000  0.05    0.32
Q18   1   0.1958  0.5450  0.7255  11.00000  0.05    0.31
Q19   1   0.3744  0.6692  0.4552  11.00000  0.05    0.30
Q20   1   0.3020  0.7561  0.5980  11.00000  0.05    0.30
;
_shelx_res_checksum              68672
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Br1 Br 0.54563(16) 0.78330(5) 0.59474(6) 0.0589(3) Uani 1 1 d . .
Br2 Br 0.32898(14) 0.56831(5) 0.80200(6) 0.0546(3) Uani 1 1 d . .
C1 C 0.5184(12) 0.6192(4) 0.5428(5) 0.0400(10) Uani 1 1 d . .
C2 C 0.4260(11) 0.5301(5) 0.6272(5) 0.0393(10) Uani 1 1 d . .
C3 C 0.4059(12) 0.4114(5) 0.5850(5) 0.0435(11) Uani 1 1 d . .
H3 H 0.342170 0.351991 0.641500 0.052 Uiso 1 1 calc R U
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0824(5) 0.0426(3) 0.0546(4) -0.0055(2) 0.0206(3) -0.0023(3)
Br2 0.0697(4) 0.0570(4) 0.0415(4) -0.0040(2) 0.0220(3) 0.0006(3)
C1 0.041(2) 0.039(2) 0.040(3) -0.002(2) 0.007(2) 0.002(2)
C2 0.034(2) 0.051(3) 0.033(2) -0.002(2) 0.0081(19) 0.000(2)
C3 0.047(3) 0.047(3) 0.036(3) 0.003(2) 0.007(2) -0.001(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
C2 C1 C3 120.0(4) . 3_666
C2 C1 Br1 122.1(4) . .
C3 C1 Br1 118.0(4) 3_666 .
C3 C2 C1 120.3(5) . .
C3 C2 Br2 118.7(4) . .
C1 C2 Br2 121.0(4) . .
C2 C3 C1 119.7(5) . 3_666
C2 C3 H3 120.1 . .
C1 C3 H3 120.1 3_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C1 1.887(5) .
Br2 C2 1.887(5) .
C1 C2 1.386(7) .
C1 C3 1.394(7) 3_666
C2 C3 1.377(7) .
C3 H3 0.9300 .
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_4
C3 C1 C2 C3 -0.5(8) 3_666 .
Br1 C1 C2 C3 179.4(4) . .
C3 C1 C2 Br2 179.0(4) 3_666 .
Br1 C1 C2 Br2 -1.1(6) . .
C1 C2 C3 C1 0.5(8) . 3_666
Br2 C2 C3 C1 -179.0(4) . 3_666
