#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:38:40 +0100 (dom 17 de nov de 2019) $
#$Revision: 230932 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/01/7230197.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_7230197
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                 100.671(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.0723(3)
_cell_length_b                   11.1474(6)
_cell_length_c                   9.8296(6)
_cell_measurement_reflns_used    1481
_cell_measurement_temperature    343(2)
_cell_measurement_theta_max      28.1570
_cell_measurement_theta_min      2.7870
_cell_volume                     438.50(5)
_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      343(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  0.0353
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_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            3134
_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         26.358
_diffrn_reflns_theta_min         2.790
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    18.276
_exptl_absorpt_correction_T_max  0.581
_exptl_absorpt_correction_T_min  0.048
_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    2.982
_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         0.579
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.034(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   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0372P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                666
_reflns_number_total             893
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cp08609a2.cif
_cod_data_source_block           TBB_343K
_cod_depositor_comments
'Adding full bibliography for 7230191--7230198.cif.'
_cod_database_code               7230197
_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   0.610
_shelx_res_file
;
TITL 343
    TBB_343K.res
    created by SHELXL-2017/1 at 11:35:18 on 10-Oct-2017
CELL 0.71073   4.072304  11.147446   9.829564  90.0000 100.6713  90.0000
ZERR    2.00   0.000301   0.000555   0.000585   0.0000   0.0065   0.0000
LATT 1
SYMM -X+ 0.50000, Y+ 0.50000, -Z+ 0.50000
SFAC BR C H
UNIT 8 12 4
TEMP 70
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    0.037200
EXTI    0.034107
FVAR       0.92873
BR1   1    0.535032    0.781270    0.594934    11.00000    0.09924    0.04780 =
         0.05951   -0.00559    0.02518   -0.00162
BR2   1    0.324857    0.566509    0.802428    11.00000    0.08493    0.06518 =
         0.04408   -0.00453    0.02630   -0.00019
C1    2    0.516342    0.618120    0.542026    11.00000    0.05158    0.04301 =
         0.04467   -0.00228    0.01017   -0.00037
C2    2    0.425441    0.529549    0.627710    11.00000    0.04471    0.05619 =
         0.03353   -0.00373    0.00954    0.00154
C3    2    0.409267    0.411373    0.584928    11.00000    0.05353    0.04871 =
         0.04187    0.00598    0.01093   -0.00429
AFIX  43
H3    3    0.348289    0.351830    0.641695    11.00000   -1.20000
AFIX   0
HKLF 4




REM  343
REM R1 =  0.0323 for     666 Fo > 4sig(Fo)  and  0.0526 for all     893 data
REM     47 parameters refined using      0 restraints

END

WGHT      0.0372      0.0000

REM Highest difference peak  0.579,  deepest hole -0.447,  1-sigma level  0.125
Q1    1   0.7438  0.7665  0.5842  11.00000  0.05    0.58
Q2    1   0.5575  0.5635  0.8286  11.00000  0.05    0.54
Q3    1   0.2831  0.7523  0.5712  11.00000  0.05    0.42
Q4    1   0.1902  0.8023  0.5816  11.00000  0.05    0.40
Q5    1   0.9247  0.7391  0.6523  11.00000  0.05    0.34
Q6    1   0.4038  0.6439  0.8214  11.00000  0.05    0.33
Q7    1  -0.0644  0.5776  0.7242  11.00000  0.05    0.32
Q8    1   0.5353  0.4155  0.8917  11.00000  0.05    0.31
Q9    1   0.1946  0.8427  0.4808  11.00000  0.05    0.30
Q10   1   0.4949  0.8549  0.5850  11.00000  0.05    0.30
Q11   1   0.3877  0.4853  0.8341  11.00000  0.05    0.30
Q12   1   0.6513  0.7057  0.6168  11.00000  0.05    0.29
Q13   1   0.8606  0.4346  0.5975  11.00000  0.05    0.29
Q14   1   0.7737  0.7812  0.5056  11.00000  0.05    0.29
Q15   1  -0.0208  0.2829  0.4671  11.00000  0.05    0.29
Q16   1   0.7875  0.5470  0.7903  11.00000  0.05    0.29
Q17   1   0.7636  0.3848  0.5929  11.00000  0.05    0.28
Q18   1   0.4867  0.6938  0.5667  11.00000  0.05    0.27
Q19   1   0.5635  0.7615  0.6745  11.00000  0.05    0.26
Q20   1   0.1446  0.7316  0.4683  11.00000  0.05    0.26
;
_shelx_res_checksum              29058
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 0.53503(15) 0.78127(5) 0.59493(6) 0.0675(3) Uani 1 1 d . .
Br2 Br 0.32486(14) 0.56651(5) 0.80243(6) 0.0629(3) Uani 1 1 d . .
C1 C 0.5163(11) 0.6181(4) 0.5420(5) 0.0463(11) Uani 1 1 d . .
C2 C 0.4254(11) 0.5295(4) 0.6277(5) 0.0445(11) Uani 1 1 d . .
C3 C 0.4093(11) 0.4114(4) 0.5849(5) 0.0478(12) Uani 1 1 d . .
H3 H 0.348289 0.351830 0.641695 0.057 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 0.0992(5) 0.0478(3) 0.0595(4) -0.0056(2) 0.0252(3) -0.0016(3)
Br2 0.0849(4) 0.0652(4) 0.0441(4) -0.0045(3) 0.0263(3) -0.0002(3)
C1 0.052(3) 0.043(2) 0.045(3) -0.002(2) 0.010(2) 0.000(2)
C2 0.045(2) 0.056(3) 0.034(3) -0.004(2) 0.010(2) 0.002(2)
C3 0.054(3) 0.049(3) 0.042(3) 0.006(2) 0.011(2) -0.004(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
C3 C1 C2 120.4(4) 3_666
C3 C1 Br1 118.3(4) 3_666
C2 C1 Br1 121.2(4) .
C3 C2 C1 119.7(5) .
C3 C2 Br2 118.7(4) .
C1 C2 Br2 121.6(4) .
C1 C3 C2 119.8(4) 3_666
C1 C3 H3 120.1 3_666
C2 C3 H3 120.1 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C1 1.889(4) .
Br2 C2 1.883(5) .
C1 C3 1.377(7) 3_666
C1 C2 1.392(7) .
C2 C3 1.381(6) .
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 -0.1(8) 3_666 .
Br1 C1 C2 C3 179.0(3) . .
C3 C1 C2 Br2 179.6(4) 3_666 .
Br1 C1 C2 Br2 -1.3(6) . .
C1 C2 C3 C1 0.1(8) . 3_666
Br2 C2 C3 C1 -179.6(4) . 3_666
