#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:38:40 +0100 (dom 17 de nov de 2019) $
#$Revision: 230932 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/01/7230196.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_7230196
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                 100.618(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.0618(3)
_cell_length_b                   11.1039(5)
_cell_length_c                   9.8533(5)
_cell_measurement_reflns_used    1477
_cell_measurement_temperature    323(2)
_cell_measurement_theta_max      28.1790
_cell_measurement_theta_min      2.8230
_cell_volume                     436.79(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      323(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  0.0258
_diffrn_reflns_av_unetI/netI     0.0203
_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            3093
_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         26.352
_diffrn_reflns_theta_min         2.791
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    18.347
_exptl_absorpt_correction_T_max  0.579
_exptl_absorpt_correction_T_min  0.045
_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    2.994
_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         0.557
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.0228(16)
_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   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0277
_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)+(0.0349P)²+0.1960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                721
_reflns_number_total             892
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cp08609a2.cif
_cod_data_source_block           TBB_323K
_cod_depositor_comments
'Adding full bibliography for 7230191--7230198.cif.'
_cod_database_code               7230196
_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   0.609
_shelx_res_file
;
TITL 323
    TBB_323K.res
    created by SHELXL-2017/1 at 11:34:34 on 10-Oct-2017
CELL  0.71073  4.06179 11.10392  9.85331 90.00000 100.61810 90.00000
ZERR 2  0.00027  0.00048  0.00046  0.00000  0.00540  0.00000
LATT 1
SYMM -X+ 0.50000, Y+ 0.50000, -Z+ 0.50000
SFAC BR C H
UNIT 8 12 4
TEMP 50
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    0.034900    0.196000
EXTI    0.022804
FVAR       1.19612
BR1   1    0.541288    0.782517    0.594894    11.00000    0.08922    0.04304 =
         0.05345   -0.00535    0.02219   -0.00222
BR2   1    0.327158    0.567583    0.802275    11.00000    0.07590    0.05877 =
         0.03934   -0.00408    0.02316    0.00069
C1    2    0.519189    0.618882    0.542643    11.00000    0.04387    0.03801 =
         0.03985   -0.00262    0.00965    0.00134
C2    2    0.426981    0.530127    0.628002    11.00000    0.03677    0.05336 =
         0.03177   -0.00380    0.00835   -0.00291
C3    2    0.407704    0.411306    0.585339    11.00000    0.04795    0.04525 =
         0.03796    0.00566    0.00949   -0.00300
AFIX  43
H3    3    0.345977    0.351784    0.642161    11.00000   -1.20000
AFIX   0
HKLF 4




REM  323
REM R1 =  0.0277 for     721 Fo > 4sig(Fo)  and  0.0391 for all     892 data
REM     47 parameters refined using      0 restraints

END

WGHT      0.0349      0.1960

REM Highest difference peak  0.557,  deepest hole -0.441,  1-sigma level  0.116
Q1    1   0.5552  0.5609  0.8202  11.00000  0.05    0.56
Q2    1   0.3809  0.7576  0.5319  11.00000  0.05    0.45
Q3    1   0.7551  0.7592  0.5985  11.00000  0.05    0.44
Q4    1  -0.0082  0.5484  0.7580  11.00000  0.05    0.35
Q5    1   0.3554  0.6409  0.7860  11.00000  0.05    0.33
Q6    1   0.4774  0.7596  0.6610  11.00000  0.05    0.33
Q7    1   0.8015  0.4470  0.6376  11.00000  0.05    0.30
Q8    1   0.7917  0.5928  0.7574  11.00000  0.05    0.30
Q9    1   0.1601  0.5278  0.8442  11.00000  0.05    0.29
Q10   1   0.9892  0.8333  0.5781  11.00000  0.05    0.27
Q11   1   0.9404  0.7173  0.6184  11.00000  0.05    0.27
Q12   1   0.3513  0.8038  0.6649  11.00000  0.05    0.27
Q13   1   0.6674  0.8528  0.5590  11.00000  0.05    0.25
Q14   1   0.1416  0.5714  0.8597  11.00000  0.05    0.25
Q15   1   0.1222  0.5328  0.4365  11.00000  0.05    0.24
Q16   1   0.7701  0.4854  0.7436  11.00000  0.05    0.24
Q17   1   0.4739  0.3584  0.6552  11.00000  0.05    0.24
Q18   1   0.9162  0.6432  0.5407  11.00000  0.05    0.24
Q19   1   0.1323  0.7082  0.4853  11.00000  0.05    0.24
Q20   1   0.8567  0.7505  0.5045  11.00000  0.05    0.24
;
_shelx_res_checksum              84782
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 0.54129(13) 0.78252(4) 0.59489(5) 0.0608(2) Uani 1 1 d . .
Br2 Br 0.32716(13) 0.56758(4) 0.80227(5) 0.0564(2) Uani 1 1 d . .
C1 C 0.5192(10) 0.6189(4) 0.5426(4) 0.0403(9) Uani 1 1 d . .
C2 C 0.4270(10) 0.5301(4) 0.6280(4) 0.0404(9) Uani 1 1 d . .
C3 C 0.4077(10) 0.4113(4) 0.5853(4) 0.0435(9) Uani 1 1 d . .
H3 H 0.345977 0.351784 0.642161 0.052 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 0.0892(4) 0.0430(3) 0.0534(3) -0.0054(2) 0.0222(3) -0.0022(2)
Br2 0.0759(4) 0.0588(3) 0.0393(3) -0.0041(2) 0.0232(2) 0.0007(2)
C1 0.044(2) 0.038(2) 0.040(2) -0.0026(17) 0.0097(18) 0.0013(17)
C2 0.0368(19) 0.053(2) 0.032(2) -0.0038(17) 0.0084(17) -0.0029(18)
C3 0.048(2) 0.045(2) 0.038(2) 0.0057(18) 0.0095(18) -0.003(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
_geom_angle_site_symmetry_3
C3 C1 C2 120.3(4) 3_666 .
C3 C1 Br1 118.2(3) 3_666 .
C2 C1 Br1 121.5(3) . .
C3 C2 C1 119.9(4) . .
C3 C2 Br2 118.6(3) . .
C1 C2 Br2 121.5(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 1.886(4) .
Br2 C2 1.882(4) .
C1 C3 1.389(6) 3_666
C1 C2 1.391(6) .
C2 C3 1.383(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 0.0(7) 3_666 .
Br1 C1 C2 C3 178.9(3) . .
C3 C1 C2 Br2 179.8(3) 3_666 .
Br1 C1 C2 Br2 -1.2(5) . .
C1 C2 C3 C1 0.0(7) . 3_666
Br2 C2 C3 C1 -179.8(3) . 3_666
