#------------------------------------------------------------------------------
#$Date: 2019-11-17 15:38:40 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230932 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/01/7230194.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_7230194
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                 100.640(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.0686(3)
_cell_length_b                   11.1298(5)
_cell_length_c                   9.8431(5)
_cell_measurement_reflns_used    1547
_cell_measurement_temperature    333(2)
_cell_measurement_theta_max      28.1900
_cell_measurement_theta_min      2.8230
_cell_volume                     438.06(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      333(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  0.0382
_diffrn_reflns_av_unetI/netI     0.0281
_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            3048
_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         26.362
_diffrn_reflns_theta_min         2.790
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    18.295
_exptl_absorpt_correction_T_max  0.563
_exptl_absorpt_correction_T_min  0.050
_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    2.985
_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         0.775
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.022(3)
_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   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0385
_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)+(0.0613P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                696
_reflns_number_total             895
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cp08609a2.cif
_cod_data_source_block           TBB_333K
_cod_depositor_comments
'Adding full bibliography for 7230191--7230198.cif.'
_cod_database_code               7230194
_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 333
    TBB_333K.res
    created by SHELXL-2017/1 at 11:34:55 on 10-Oct-2017
CELL 0.71073   4.068577  11.129841   9.843072  90.0000 100.6404  90.0000
ZERR    2.00   0.000269   0.000487   0.000485   0.0000   0.0057   0.0000
LATT 1
SYMM -X+ 0.50000, Y+ 0.50000, -Z+ 0.50000
SFAC BR C H
UNIT 8 12 4
TEMP 60
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    0.061300
EXTI    0.022264
FVAR       1.12733
BR1   1    0.537729    0.781887    0.594995    11.00000    0.09364    0.04737 =
         0.06028   -0.00573    0.02444   -0.00131
BR2   1    0.325675    0.567040    0.802345    11.00000    0.08015    0.06429 =
         0.04492   -0.00418    0.02540    0.00030
C1    2    0.516867    0.619384    0.542143    11.00000    0.04661    0.04369 =
         0.04600   -0.00351    0.01139    0.00092
C2    2    0.423735    0.530173    0.627021    11.00000    0.03992    0.05684 =
         0.03355   -0.00235    0.00556   -0.00029
C3    2    0.407702    0.411001    0.584767    11.00000    0.05311    0.04742 =
         0.04181   -0.00002    0.01090    0.00154
AFIX  43
H3    3    0.346294    0.351676    0.641764    11.00000   -1.20000
AFIX   0
HKLF 4




REM  333
REM R1 =  0.0385 for     696 Fo > 4sig(Fo)  and  0.0533 for all     895 data
REM     47 parameters refined using      0 restraints

END

WGHT      0.0613      0.0000

REM Highest difference peak  0.775,  deepest hole -0.592,  1-sigma level  0.163
Q1    1   0.7478  0.7590  0.5790  11.00000  0.05    0.78
Q2    1   0.3387  0.7536  0.5250  11.00000  0.05    0.67
Q3    1   0.8282  0.6569  0.6438  11.00000  0.05    0.48
Q4    1   0.5339  0.5463  0.8363  11.00000  0.05    0.45
Q5    1   0.9612  0.7872  0.5272  11.00000  0.05    0.44
Q6    1   0.0822  0.5631  0.8316  11.00000  0.05    0.41
Q7    1   0.8539  0.7061  0.7400  11.00000  0.05    0.41
Q8    1   0.5318  0.8357  0.5876  11.00000  0.05    0.40
Q9    1   0.7973  0.4389  0.6397  11.00000  0.05    0.40
Q10   1   0.6028  0.6694  0.9587  11.00000  0.05    0.39
Q11   1   0.5115  0.6245  0.8842  11.00000  0.05    0.38
Q12   1  -0.0863  0.5577  0.7866  11.00000  0.05    0.37
Q13   1   0.7253  0.5661  0.7074  11.00000  0.05    0.36
Q14   1   0.7072  0.8447  0.5262  11.00000  0.05    0.35
Q15   1  -0.0481  0.3840  0.5318  11.00000  0.05    0.32
Q16   1   0.6137  0.4478  0.8384  11.00000  0.05    0.32
Q17   1   0.7379  0.6208  0.9301  11.00000  0.05    0.31
Q18   1   0.4118  0.6313  0.7884  11.00000  0.05    0.31
Q19   1   0.4982  0.4595  0.6281  11.00000  0.05    0.31
Q20   1   0.9342  0.6749  0.5592  11.00000  0.05    0.30
;
_shelx_res_checksum              25242
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 0.53773(17) 0.78189(5) 0.59499(7) 0.0658(3) Uani 1 1 d . .
Br2 Br 0.32568(16) 0.56704(5) 0.80234(6) 0.0614(3) Uani 1 1 d . .
C1 C 0.5169(13) 0.6194(5) 0.5421(6) 0.0451(12) Uani 1 1 d . .
C2 C 0.4237(12) 0.5302(5) 0.6270(5) 0.0436(11) Uani 1 1 d . .
C3 C 0.4077(13) 0.4110(4) 0.5848(6) 0.0472(12) Uani 1 1 d . .
H3 H 0.346294 0.351676 0.641764 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 0.0936(6) 0.0474(4) 0.0603(5) -0.0057(3) 0.0244(4) -0.0013(3)
Br2 0.0801(5) 0.0643(5) 0.0449(4) -0.0042(3) 0.0254(3) 0.0003(3)
C1 0.047(3) 0.044(3) 0.046(3) -0.004(2) 0.011(2) 0.001(2)
C2 0.040(2) 0.057(3) 0.034(3) -0.002(2) 0.006(2) 0.000(2)
C3 0.053(3) 0.047(3) 0.042(3) 0.000(2) 0.011(2) 0.002(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 119.8(5) 3_666
C3 C1 Br1 118.6(4) 3_666
C2 C1 Br1 121.5(4) .
C3 C2 C1 120.3(5) .
C3 C2 Br2 118.4(4) .
C1 C2 Br2 121.3(4) .
C1 C3 C2 119.9(5) 3_666
C1 C3 H3 120.0 3_666
C2 C3 H3 120.0 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C1 1.880(5) .
Br2 C2 1.887(5) .
C1 C3 1.382(7) 3_666
C1 C2 1.394(8) .
C2 C3 1.388(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 0.2(9) 3_666 .
Br1 C1 C2 C3 179.4(4) . .
C3 C1 C2 Br2 178.9(4) 3_666 .
Br1 C1 C2 Br2 -1.9(6) . .
C1 C2 C3 C1 -0.2(9) . 3_666
Br2 C2 C3 C1 -179.0(4) . 3_666
