#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:38:40 +0100 (dom 17 de nov de 2019) $
#$Revision: 230932 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/01/7230193.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_7230193
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                 100.175(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.0172(2)
_cell_length_b                   10.6917(4)
_cell_length_c                   10.2615(4)
_cell_measurement_reflns_used    1634
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2360
_cell_measurement_theta_min      4.0290
_cell_volume                     433.81(3)
_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      293(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  0.0306
_diffrn_reflns_av_unetI/netI     0.0232
_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       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2971
_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         26.370
_diffrn_reflns_theta_min         2.774
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    18.474
_exptl_absorpt_correction_T_max  0.551
_exptl_absorpt_correction_T_min  0.049
_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    3.014
_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         0.496
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.020(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   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0296
_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)+(0.0518P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                757
_reflns_number_total             882
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cp08609a2.cif
_cod_data_source_block           TBB_293K
_cod_depositor_comments
'Adding full bibliography for 7230191--7230198.cif.'
_cod_database_code               7230193
_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   0.607
_shelx_res_file
;
TITL 293
    TBB_293K.res
    created by SHELXL-2017/1 at 11:33:23 on 10-Oct-2017
CELL  0.71073  4.01721 10.69170 10.26155 90.00000 100.17470 90.00000
ZERR 2  0.00022  0.00041  0.00042  0.00000  0.00450  0.00000
LATT 1
SYMM -X+ 0.50000, Y+ 0.50000, -Z+ 0.50000
SFAC BR C H
UNIT 8 12 4
TEMP 20
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    0.051800
EXTI    0.019718
FVAR       1.22471
BR1   1    0.615235    0.792836    0.589233    11.00000    0.06977    0.03258 =
         0.04422   -0.00464    0.01031   -0.00553
BR2   1    0.371527    0.578826    0.795192    11.00000    0.06036    0.04325 =
         0.03507   -0.00231    0.01592    0.00393
C1    2    0.546413    0.623770    0.539652    11.00000    0.03279    0.03222 =
         0.03518   -0.00097    0.00603   -0.00018
C2    2    0.446874    0.535297    0.624750    11.00000    0.03101    0.03635 =
         0.03061   -0.00470    0.00577    0.00372
C3    2    0.399311    0.412043    0.585237    11.00000    0.03576    0.03350 =
         0.03318    0.00378    0.00398   -0.00062
AFIX  43
H3    3    0.331245    0.353243    0.641950    11.00000   -1.20000
AFIX   0
HKLF 4




REM  293
REM R1 =  0.0296 for     757 Fo > 4sig(Fo)  and  0.0351 for all     882 data
REM     47 parameters refined using      0 restraints

END

WGHT      0.0518      0.0000

REM Highest difference peak  0.496,  deepest hole -0.563,  1-sigma level  0.133
Q1    1   0.3242  0.5349  0.7329  11.00000  0.05    0.50
Q2    1   0.4256  0.5195  0.8617  11.00000  0.05    0.46
Q3    1   0.4539  0.7757  0.5169  11.00000  0.05    0.46
Q4    1   0.5104  0.6180  0.8751  11.00000  0.05    0.45
Q5    1   0.7142  0.6024  0.9342  11.00000  0.05    0.45
Q6    1   0.5724  0.6604  0.9646  11.00000  0.05    0.44
Q7    1   0.5954  0.8517  0.5385  11.00000  0.05    0.42
Q8    1   0.5608  0.7387  0.5320  11.00000  0.05    0.40
Q9    1   0.7925  0.7889  0.6880  11.00000  0.05    0.40
Q10   1   0.5030  0.5407  0.8745  11.00000  0.05    0.39
Q11   1   0.5710  0.7436  0.6423  11.00000  0.05    0.38
Q12   1   0.0850  0.6156  0.4741  11.00000  0.05    0.37
Q13   1   0.8824  0.6189  0.6809  11.00000  0.05    0.37
Q14   1   0.2796  0.6238  0.7220  11.00000  0.05    0.35
Q15   1   0.7825  0.5449  0.7040  11.00000  0.05    0.33
Q16   1   0.0292  0.5403  0.8755  11.00000  0.05    0.32
Q17   1   0.7762  0.5918  0.8451  11.00000  0.05    0.32
Q18   1   0.7521  0.8505  0.6541  11.00000  0.05    0.32
Q19   1   0.3814  0.4554  0.8042  11.00000  0.05    0.31
Q20   1   1.0009  0.7844  0.5232  11.00000  0.05    0.31
;
_shelx_res_checksum              91219
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 0.61524(13) 0.79284(4) 0.58923(5) 0.0488(2) Uani 1 1 d . .
Br2 Br 0.37153(12) 0.57883(4) 0.79519(4) 0.0453(2) Uani 1 1 d . .
C1 C 0.5464(10) 0.6238(4) 0.5397(4) 0.0334(8) Uani 1 1 d . .
C2 C 0.4469(10) 0.5353(4) 0.6247(4) 0.0326(8) Uani 1 1 d . .
C3 C 0.3993(10) 0.4120(3) 0.5852(4) 0.0344(9) Uani 1 1 d . .
H3 H 0.331245 0.353243 0.641950 0.041 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 0.0698(4) 0.0326(3) 0.0442(3) -0.00464(18) 0.0103(2) -0.0055(2)
Br2 0.0604(4) 0.0432(3) 0.0351(3) -0.00231(17) 0.0159(2) 0.0039(2)
C1 0.0328(19) 0.032(2) 0.035(2) -0.0010(16) 0.0060(16) -0.0002(16)
C2 0.0310(19) 0.036(2) 0.031(2) -0.0047(17) 0.0058(16) 0.0037(16)
C3 0.036(2) 0.033(2) 0.033(2) 0.0038(16) 0.0040(16) -0.0006(17)
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
C3 C1 C2 120.0(4) 3_666 .
C3 C1 Br1 118.2(3) 3_666 .
C2 C1 Br1 121.8(3) . .
C3 C2 C1 120.2(4) . .
C3 C2 Br2 118.1(3) . .
C1 C2 Br2 121.7(3) . .
C2 C3 C1 119.8(4) . 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 1.885(4) .
Br2 C2 1.885(4) .
C1 C3 1.391(6) 3_666
C1 C2 1.393(6) .
C2 C3 1.382(5) .
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(7) 3_666 .
Br1 C1 C2 C3 -179.9(3) . .
C3 C1 C2 Br2 179.8(3) 3_666 .
Br1 C1 C2 Br2 0.4(5) . .
C1 C2 C3 C1 0.5(7) . 3_666
Br2 C2 C3 C1 -179.8(3) . 3_666
