#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:38:40 +0100 (dom 17 de nov de 2019) $
#$Revision: 230932 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/01/7230198.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_7230198
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                 100.168(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.0108(2)
_cell_length_b                   10.6672(4)
_cell_length_c                   10.2811(4)
_cell_measurement_reflns_used    1749
_cell_measurement_temperature    283(2)
_cell_measurement_theta_max      28.2220
_cell_measurement_theta_min      4.0400
_cell_volume                     432.96(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      283(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  0.0297
_diffrn_reflns_av_unetI/netI     0.0226
_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            2945
_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         26.354
_diffrn_reflns_theta_min         2.774
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    18.510
_exptl_absorpt_correction_T_max  0.549
_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    3.020
_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         0.521
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.023(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   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0295
_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)+(0.0541P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                762
_reflns_number_total             877
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cp08609a2.cif
_cod_data_source_block           TBB_283K
_cod_depositor_comments
'Adding full bibliography for 7230191--7230198.cif.'
_cod_database_code               7230198
_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 283
    TBB_283K.res
    created by SHELXL-2017/1 at 11:30:40 on 10-Oct-2017
CELL  0.71073  4.01083 10.66722 10.28106 90.00000 100.16760 90.00000
ZERR 2  0.00020  0.00036  0.00038  0.00000  0.00400  0.00000
LATT 1
SYMM -X+ 0.50000, Y+ 0.50000, -Z+ 0.50000
SFAC BR C H
UNIT 8 12 4
TEMP 10
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    0.054100
EXTI    0.022656
FVAR       1.23457
BR1   1    0.618917    0.793434    0.588833    11.00000    0.06623    0.03123 =
         0.04234   -0.00438    0.00944   -0.00546
BR2   1    0.373689    0.579469    0.794909    11.00000    0.05776    0.04099 =
         0.03357   -0.00210    0.01488    0.00389
C1    2    0.549291    0.623430    0.539154    11.00000    0.03421    0.02821 =
         0.03497   -0.00232    0.00606   -0.00216
C2    2    0.448103    0.535410    0.624357    11.00000    0.02997    0.03288 =
         0.02928   -0.00259    0.00445    0.00448
C3    2    0.399256    0.412160    0.585375    11.00000    0.03331    0.03268 =
         0.03361    0.00265    0.00552   -0.00162
AFIX  43
H3    3    0.332200    0.353279    0.642298    11.00000   -1.20000
AFIX   0
HKLF 4




REM  283
REM R1 =  0.0295 for     762 Fo > 4sig(Fo)  and  0.0355 for all     877 data
REM     47 parameters refined using      0 restraints

END

WGHT      0.0541      0.0000

REM Highest difference peak  0.521,  deepest hole -0.542,  1-sigma level  0.142
Q1    1   0.8081  0.8004  0.6927  11.00000  0.05    0.52
Q2    1   0.4887  0.5248  0.8638  11.00000  0.05    0.52
Q3    1   0.7378  0.5969  0.9479  11.00000  0.05    0.52
Q4    1   0.3390  0.5176  0.8434  11.00000  0.05    0.51
Q5    1   0.3425  0.5244  0.7408  11.00000  0.05    0.49
Q6    1   0.5116  0.5804  0.9012  11.00000  0.05    0.45
Q7    1   0.2532  0.6147  0.7217  11.00000  0.05    0.44
Q8    1   0.7072  0.7418  0.6633  11.00000  0.05    0.44
Q9    1   0.5754  0.6606  0.9713  11.00000  0.05    0.42
Q10   1   0.5484  0.6206  0.8747  11.00000  0.05    0.41
Q11   1   0.6098  0.3770  0.7377  11.00000  0.05    0.41
Q12   1   0.2303  0.7952  0.4358  11.00000  0.05    0.39
Q13   1   0.4480  0.7992  0.4868  11.00000  0.05    0.39
Q14   1   0.3294  0.6405  0.7385  11.00000  0.05    0.38
Q15   1   0.2194  0.5806  0.7006  11.00000  0.05    0.38
Q16   1   0.4897  0.7588  0.5130  11.00000  0.05    0.38
Q17   1   0.8063  0.5659  0.8365  11.00000  0.05    0.37
Q18   1   0.9349  0.7942  0.6215  11.00000  0.05    0.37
Q19   1   0.7850  0.7524  0.5661  11.00000  0.05    0.35
Q20   1   0.2296  0.8020  0.6793  11.00000  0.05    0.35
;
_shelx_res_checksum              57871
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 0.61892(13) 0.79343(4) 0.58883(5) 0.0466(2) Uani 1 1 d . .
Br2 Br 0.37369(11) 0.57947(4) 0.79491(4) 0.0433(2) Uani 1 1 d . .
C1 C 0.5493(9) 0.6234(4) 0.5392(4) 0.0325(9) Uani 1 1 d . .
C2 C 0.4481(10) 0.5354(4) 0.6244(4) 0.0308(8) Uani 1 1 d . .
C3 C 0.3993(10) 0.4122(3) 0.5854(4) 0.0332(9) Uani 1 1 d . .
H3 H 0.332200 0.353279 0.642298 0.040 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 0.0662(4) 0.0312(3) 0.0423(3) -0.00438(17) 0.0094(2) -0.00546(19)
Br2 0.0578(4) 0.0410(3) 0.0336(3) -0.00210(17) 0.0149(2) 0.00389(19)
C1 0.0342(19) 0.0282(19) 0.035(2) -0.0023(16) 0.0061(17) -0.0022(16)
C2 0.0300(19) 0.033(2) 0.029(2) -0.0026(16) 0.0045(16) 0.0045(15)
C3 0.0333(19) 0.033(2) 0.034(2) 0.0026(17) 0.0055(16) -0.0016(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 120.3(4) 3_666 .
C3 C1 Br1 118.3(3) 3_666 .
C2 C1 Br1 121.5(3) . .
C3 C2 C1 120.2(4) . .
C3 C2 Br2 118.0(3) . .
C1 C2 Br2 121.8(3) . .
C2 C3 C1 119.6(4) . 3_666
C2 C3 H3 120.2 . .
C1 C3 H3 120.2 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 1.891(4) .
Br2 C2 1.889(4) .
C1 C3 1.385(6) 3_666
C1 C2 1.393(6) .
C2 C3 1.378(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 0.2(7) 3_666 .
Br1 C1 C2 C3 180.0(3) . .
C3 C1 C2 Br2 -179.8(3) 3_666 .
Br1 C1 C2 Br2 0.0(5) . .
C1 C2 C3 C1 -0.2(7) . 3_666
Br2 C2 C3 C1 179.8(3) . 3_666
