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#$Date: 2021-07-28 08:23:42 +0300 (Wed, 28 Jul 2021) $
#$Revision: 267783 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/88/2108855.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2108855
loop_
_publ_author_name
'Bujak, Maciej'
'Podsiadło, Marcin'
'Katrusiak, Andrzej'
_publ_section_title
;
 Properties and interactions -- melting point of tribromobenzene isomers
;
_journal_coeditor_code           LO5092
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520621006399
_journal_volume                  77
_journal_year                    2021
_chemical_formula_moiety         'C6 H3 Br3'
_chemical_formula_sum            'C6 H3 Br3'
_chemical_formula_weight         314.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.00341(11)
_cell_length_b                   13.4119(3)
_cell_length_c                   14.0916(4)
_cell_measurement_reflns_used    3792
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      30.83
_cell_measurement_theta_min      4.18
_cell_volume                     756.62(3)
_computing_cell_refinement
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_collection
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_reduction
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10543
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.891
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    15.897
_exptl_absorpt_correction_T_max  0.274
_exptl_absorpt_correction_T_min  0.074
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(3)
_refine_ls_extinction_coef       0.00088(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0184
_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)+(0.0137P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0352
_refine_ls_wR_factor_ref         0.0357
_reflns_Friedel_coverage         0.631
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1395
_reflns_number_total             1476
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            lo5092sup1.cif
_cod_data_source_block           135TBB_100K
_cod_original_cell_volume        756.63(3)
_cod_database_code               2108855
_shelx_shelxl_version_number     2014/7
_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   0.072
_shelx_estimated_absorpt_t_max   0.299
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.2985(12) 0.2268(3) 0.3364(3) 0.0142(11) Uani 1 1 d . . . . .
Br11 Br 0.44078(12) 0.10520(3) 0.39217(4) 0.01827(14) Uani 1 1 d . . . . .
C12 C 0.1347(11) 0.2240(3) 0.2501(3) 0.0142(11) Uani 1 1 d . . . . .
H12 H 0.0941 0.1639 0.2192 0.017 Uiso 1 1 calc R U . . .
C13 C 0.0339(12) 0.3134(4) 0.2116(3) 0.0146(10) Uani 1 1 d . . . . .
Br13 Br -0.18586(12) 0.31174(4) 0.09210(4) 0.01805(13) Uani 1 1 d . . . . .
C14 C 0.0941(11) 0.4039(4) 0.2543(4) 0.0158(11) Uani 1 1 d . . . . .
H14 H 0.0253 0.4633 0.2266 0.019 Uiso 1 1 calc R U . . .
C15 C 0.2615(11) 0.4028(4) 0.3404(4) 0.0165(11) Uani 1 1 d . . . . .
Br15 Br 0.35576(11) 0.52517(3) 0.40228(4) 0.01976(14) Uani 1 1 d . . . . .
C16 C 0.3671(11) 0.3151(4) 0.3831(3) 0.0150(10) Uani 1 1 d . . . . .
H16 H 0.4796 0.3156 0.4408 0.018 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Br Br -0.2901 2.4595 '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
_geom_angle_publ_flag
C12 C11 C16 122.5(4) . . ?
C12 C11 Br11 118.9(4) . . ?
C16 C11 Br11 118.6(4) . . ?
C13 C12 C11 117.5(4) . . ?
C13 C12 H12 121.2 . . ?
C11 C12 H12 121.2 . . ?
C14 C13 C12 123.0(4) . . ?
C14 C13 Br13 118.7(4) . . ?
C12 C13 Br13 118.3(3) . . ?
C13 C14 C15 117.3(5) . . ?
C13 C14 H14 121.3 . . ?
C15 C14 H14 121.3 . . ?
C14 C15 C16 122.3(5) . . ?
C14 C15 Br15 119.3(4) . . ?
C16 C15 Br15 118.3(4) . . ?
C11 C16 C15 117.4(4) . . ?
C11 C16 H16 121.3 . . ?
C15 C16 H16 121.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 C12 1.382(7) . ?
C11 C16 1.383(6) . ?
C11 Br11 1.898(5) . ?
C12 C13 1.377(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.376(7) . ?
C13 Br13 1.900(4) . ?
C14 C15 1.386(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.387(7) . ?
C15 Br15 1.896(5) . ?
C16 H16 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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 C11 C12 C13 -1.1(7) . . . . ?
Br11 C11 C12 C13 179.8(3) . . . . ?
C11 C12 C13 C14 1.1(7) . . . . ?
C11 C12 C13 Br13 179.1(3) . . . . ?
C12 C13 C14 C15 -0.6(7) . . . . ?
Br13 C13 C14 C15 -178.6(3) . . . . ?
C13 C14 C15 C16 0.1(7) . . . . ?
C13 C14 C15 Br15 179.4(4) . . . . ?
C12 C11 C16 C15 0.6(7) . . . . ?
Br11 C11 C16 C15 179.7(3) . . . . ?
C14 C15 C16 C11 -0.1(7) . . . . ?
Br15 C15 C16 C11 -179.4(4) . . . . ?

_cod_database_fobs_code 2108855
