#------------------------------------------------------------------------------
#$Date: 2019-11-17 15:38:40 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230932 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/01/7230195.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_7230195
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                 100.184(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.0233(2)
_cell_length_b                   10.7193(4)
_cell_length_c                   10.2355(5)
_cell_measurement_reflns_used    1637
_cell_measurement_temperature    303(2)
_cell_measurement_theta_max      28.1590
_cell_measurement_theta_min      4.0340
_cell_volume                     434.47(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      303(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  0.0217
_diffrn_reflns_av_unetI/netI     0.0180
_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            3078
_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         26.349
_diffrn_reflns_theta_min         2.775
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    18.446
_exptl_absorpt_correction_T_max  0.575
_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    3.010
_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         0.630
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.0163(12)
_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   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0228
_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)+(0.0284P)²+0.1507P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                745
_reflns_number_total             886
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cp08609a2.cif
_cod_data_source_block           TBB_303K
_cod_depositor_comments
'Adding full bibliography for 7230191--7230198.cif.'
_cod_database_code               7230195
_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   0.026
_shelx_estimated_absorpt_t_max   0.608
_shelx_res_file
;
TITL 303
    TBB_303K.res
    created by SHELXL-2017/1 at 11:33:44 on 10-Oct-2017
CELL  0.71073  4.02326 10.71927 10.23549 90.00000 100.18380 90.00000
ZERR 2  0.00024  0.00044  0.00045  0.00000  0.00500  0.00000
LATT 1
SYMM -X+ 0.50000, Y+ 0.50000, -Z+ 0.50000
SFAC BR C H
UNIT 8 12 4
TEMP 30
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    0.028400    0.150700
EXTI    0.016289
FVAR       1.23539
BR1   1    0.610129    0.792076    0.589739    11.00000    0.07461    0.03269 =
         0.04366   -0.00483    0.01112   -0.00546
BR2   1    0.368294    0.577932    0.795581    11.00000    0.06446    0.04444 =
         0.03386   -0.00240    0.01673    0.00426
C1    2    0.544933    0.623371    0.540192    11.00000    0.03705    0.02922 =
         0.03532   -0.00177    0.00316    0.00278
C2    2    0.446377    0.535501    0.624924    11.00000    0.03663    0.03759 =
         0.02744   -0.00205    0.00670    0.00150
C3    2    0.398983    0.412077    0.584601    11.00000    0.03770    0.03491 =
         0.03335    0.00198    0.00626   -0.00267
AFIX  43
H3    3    0.329846    0.353302    0.641045    11.00000   -1.20000
AFIX   0
HKLF 4




REM  303
REM R1 =  0.0228 for     745 Fo > 4sig(Fo)  and  0.0307 for all     886 data
REM     47 parameters refined using      0 restraints

END

WGHT      0.0284      0.1507

REM Highest difference peak  0.630,  deepest hole -0.284,  1-sigma level  0.091
Q1    1   0.5506  0.7849  0.6608  11.00000  0.05    0.63
Q2    1   0.4377  0.7639  0.5515  11.00000  0.05    0.39
Q3    1   0.7669  0.7621  0.5763  11.00000  0.05    0.36
Q4    1   0.5976  0.5711  0.8008  11.00000  0.05    0.36
Q5    1   0.0536  0.5715  0.7968  11.00000  0.05    0.33
Q6    1   0.3872  0.5611  0.7049  11.00000  0.05    0.31
Q7    1   0.3453  0.5630  0.8698  11.00000  0.05    0.26
Q8    1   0.9176  0.7996  0.5806  11.00000  0.05    0.25
Q9    1   0.3548  0.4843  0.5851  11.00000  0.05    0.25
Q10   1   0.4841  0.6353  0.7977  11.00000  0.05    0.25
Q11   1   0.4366  0.3948  0.5274  11.00000  0.05    0.25
Q12   1   1.1001  0.8714  0.5316  11.00000  0.05    0.24
Q13   1   0.2667  0.8068  0.5792  11.00000  0.05    0.24
Q14   1   0.5890  0.3058  0.7141  11.00000  0.05    0.23
Q15   1   0.5317  0.4615  0.6030  11.00000  0.05    0.22
Q16   1   0.4076  0.8804  0.6104  11.00000  0.05    0.22
Q17   1   0.1859  0.4933  0.8244  11.00000  0.05    0.22
Q18   1   0.2406  0.8381  0.4763  11.00000  0.05    0.22
Q19   1   0.6056  0.8479  0.5770  11.00000  0.05    0.21
Q20   1   0.1178  0.8236  0.6388  11.00000  0.05    0.21
;
_shelx_res_checksum              64574
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 0.61013(11) 0.79208(3) 0.58974(4) 0.05024(17) Uani 1 1 d . .
Br2 Br 0.36829(10) 0.57793(3) 0.79558(4) 0.04661(16) Uani 1 1 d . .
C1 C 0.5449(8) 0.6234(3) 0.5402(3) 0.0343(7) Uani 1 1 d . .
C2 C 0.4464(8) 0.5355(3) 0.6249(3) 0.0338(7) Uani 1 1 d . .
C3 C 0.3990(8) 0.4121(3) 0.5846(3) 0.0353(7) Uani 1 1 d . .
H3 H 0.329846 0.353302 0.641045 0.042 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 0.0746(3) 0.0327(2) 0.0437(2) -0.00483(15) 0.01112(19) -0.00546(17)
Br2 0.0645(3) 0.0444(2) 0.0339(2) -0.00240(14) 0.01673(17) 0.00426(17)
C1 0.0371(16) 0.0292(16) 0.0353(18) -0.0018(13) 0.0032(14) 0.0028(14)
C2 0.0366(17) 0.0376(18) 0.0274(16) -0.0021(13) 0.0067(13) 0.0015(14)
C3 0.0377(17) 0.0349(18) 0.0333(18) 0.0020(13) 0.0063(14) -0.0027(14)
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 120.1(3) . 3_666
C2 C1 Br1 121.7(3) . .
C3 C1 Br1 118.2(2) 3_666 .
C1 C2 C3 120.1(3) . .
C1 C2 Br2 122.0(2) . .
C3 C2 Br2 118.0(2) . .
C1 C3 C2 119.9(3) 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 1.884(3) .
Br2 C2 1.884(3) .
C1 C2 1.385(5) .
C1 C3 1.389(5) 3_666
C2 C3 1.389(4) .
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 -0.9(5) 3_666 .
Br1 C1 C2 C3 179.6(2) . .
C3 C1 C2 Br2 179.8(2) 3_666 .
Br1 C1 C2 Br2 0.3(4) . .
C1 C2 C3 C1 0.9(5) . 3_666
Br2 C2 C3 C1 -179.7(2) . 3_666
