#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:38:40 +0100 (dom 17 de nov de 2019) $
#$Revision: 230932 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/01/7230191.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_7230191
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                 100.172(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.0055(2)
_cell_length_b                   10.6493(4)
_cell_length_c                   10.2948(4)
_cell_measurement_reflns_used    1774
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.2060
_cell_measurement_theta_min      4.3530
_cell_volume                     432.23(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      273(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  0.0348
_diffrn_reflns_av_unetI/netI     0.0263
_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            2898
_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         26.367
_diffrn_reflns_theta_min         2.775
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    18.541
_exptl_absorpt_correction_T_max  0.574
_exptl_absorpt_correction_T_min  0.108
_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    3.025
_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         0.604
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.024(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   1.034
_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      1.034
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0278
_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)+(0.0473P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                763
_reflns_number_total             877
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cp08609a2.cif
_cod_data_source_block           TBB_273K
_cod_depositor_comments
'Adding full bibliography for 7230191--7230198.cif.'
_cod_original_cell_volume        432.24(3)
_cod_database_code               7230191
_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   0.606
_shelx_res_file
;

TITL 273
    TBB_273K.res
    created by SHELXL-2017/1 at 11:30:58 on 10-Oct-2017
CELL  0.71073  4.00554 10.64933 10.29482 90.00000 100.17150 90.00000
ZERR 2  0.00020  0.00037  0.00040  0.00000  0.00420  0.00000
LATT 1
SYMM -X+ 0.50000, Y+ 0.50000, -Z+ 0.50000
SFAC BR C H
UNIT 8 12 4
TEMP 0
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    0.047300
EXTI    0.023830
FVAR       1.12595
BR1   1    0.622305    0.793847    0.588657    11.00000    0.06571    0.02802 =
         0.03889   -0.00410    0.00653   -0.00527
BR2   1    0.375834    0.580035    0.794711    11.00000    0.05748    0.03748 =
         0.03073   -0.00187    0.01215    0.00373
C1    2    0.548936    0.624866    0.538966    11.00000    0.03379    0.02533 =
         0.03249   -0.00204    0.00293   -0.00005
C2    2    0.448480    0.536230    0.624175    11.00000    0.03140    0.02978 =
         0.02510   -0.00146    0.00370    0.00569
C3    2    0.399645    0.412088    0.585655    11.00000    0.03661    0.02802 =
         0.02948    0.00074    0.00394   -0.00037
AFIX  43
H3    3    0.332617    0.353503    0.642930    11.00000   -1.20000
AFIX   0
HKLF 4




REM  273
REM R1 =  0.0278 for     763 Fo > 4sig(Fo)  and  0.0335 for all     877 data
REM     47 parameters refined using      0 restraints

END

WGHT      0.0473      0.0000

REM Highest difference peak  0.604,  deepest hole -0.560,  1-sigma level  0.141
Q1    1   0.6484  0.5660  0.8374  11.00000  0.05    0.60
Q2    1   0.4016  0.7785  0.5477  11.00000  0.05    0.50
Q3    1   0.9456  0.7995  0.6332  11.00000  0.05    0.49
Q4    1   0.2460  0.5815  0.9438  11.00000  0.05    0.44
Q5    1   0.3639  0.5191  0.7396  11.00000  0.05    0.43
Q6    1   0.8209  0.7411  0.5614  11.00000  0.05    0.43
Q7    1   0.6119  0.6236  0.9569  11.00000  0.05    0.42
Q8    1   0.0576  0.5795  0.7525  11.00000  0.05    0.40
Q9    1   0.4880  0.4664  0.6641  11.00000  0.05    0.38
Q10   1   0.6343  0.4954  0.7419  11.00000  0.05    0.37
Q11   1   1.1047  0.7647  0.6143  11.00000  0.05    0.36
Q12   1   0.2063  0.5156  0.8415  11.00000  0.05    0.34
Q13   1   0.0280  0.6596  0.7269  11.00000  0.05    0.34
Q14   1   0.5515  0.6153  0.7803  11.00000  0.05    0.33
Q15   1   0.1324  0.7397  0.4898  11.00000  0.05    0.33
Q16   1   0.6537  0.7004  0.9183  11.00000  0.05    0.32
Q17   1   0.6053  0.3947  0.5771  11.00000  0.05    0.32
Q18   1   0.6996  0.7831  0.4636  11.00000  0.05    0.32
Q19   1   0.1064  0.7079  0.7010  11.00000  0.05    0.30
Q20   1   0.4792  0.3842  0.5434  11.00000  0.05    0.30
;
_shelx_res_checksum              11709
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 0.62231(12) 0.79385(4) 0.58866(5) 0.0445(2) Uani 1 1 d . .
Br2 Br 0.37583(11) 0.58004(4) 0.79471(4) 0.0414(2) Uani 1 1 d . .
C1 C 0.5489(9) 0.6249(4) 0.5390(4) 0.0309(8) Uani 1 1 d . .
C2 C 0.4485(9) 0.5362(3) 0.6242(4) 0.0289(8) Uani 1 1 d . .
C3 C 0.3996(10) 0.4121(3) 0.5857(4) 0.0316(8) Uani 1 1 d . .
H3 H 0.332617 0.353503 0.642930 0.038 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 0.0657(4) 0.0280(3) 0.0389(3) -0.00410(17) 0.0065(2) -0.00527(18)
Br2 0.0575(3) 0.0375(3) 0.0307(3) -0.00187(16) 0.0121(2) 0.00373(18)
C1 0.0338(18) 0.0253(19) 0.032(2) -0.0020(15) 0.0029(16) -0.0001(16)
C2 0.0314(17) 0.0298(18) 0.0251(19) -0.0015(15) 0.0037(15) 0.0057(15)
C3 0.0366(19) 0.0280(18) 0.029(2) 0.0007(15) 0.0039(16) -0.0004(16)
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 119.6(3) 3_666 .
C3 C1 Br1 118.7(3) 3_666 .
C2 C1 Br1 121.7(3) . .
C3 C2 C1 120.5(4) . .
C3 C2 Br2 117.7(3) . .
C1 C2 Br2 121.8(3) . .
C2 C3 C1 119.9(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 1.880(4) .
Br2 C2 1.888(4) .
C1 C3 1.392(6) 3_666
C1 C2 1.395(5) .
C2 C3 1.384(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 0.0(6) 3_666 .
Br1 C1 C2 C3 -179.3(3) . .
C3 C1 C2 Br2 179.8(3) 3_666 .
Br1 C1 C2 Br2 0.5(5) . .
C1 C2 C3 C1 0.0(6) . 3_666
Br2 C2 C3 C1 -179.8(3) . 3_666
