#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/82/2018248.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_2018248
loop_
_publ_author_name
'Jones, Peter G.'
'Hopf, Henning'
'Silaghi, Anamaria'
'Näther, Christian'
_publ_section_title
;
 Concomitant but disappearing: two polymorphs of
 1,4-bis(tribromomethyl)benzene
;
_journal_coeditor_code           FA3260
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o405
_journal_page_last               o408
_journal_paper_doi               10.1107/S0108270111037930
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C8 H4 Br6'
_chemical_formula_moiety         'C8 H4 Br6'
_chemical_formula_sum            'C8 H4 Br6'
_chemical_formula_weight         579.57
_chemical_name_systematic
;
1,4-bis(tribromomethyl)benzene
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.152(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1640(9)
_cell_length_b                   6.5048(7)
_cell_length_c                   19.3410(17)
_cell_measurement_reflns_used    5599
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      75.7158
_cell_measurement_theta_min      4.6729
_cell_volume                     1250.1(2)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'XP (Siemens, 1994)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Oxford Xcalibur Nova Atlas'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7801
_diffrn_reflns_theta_full        72.50
_diffrn_reflns_theta_max         75.90
_diffrn_reflns_theta_min         4.68
_exptl_absorpt_coefficient_mu    22.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis PRO (Oxford Diffraction, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.080
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.926
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0769P)²+1.4614P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                1163
_reflns_number_total             1271
_reflns_threshold_expression     I>2σ(I)
_iucr_refine_instructions_details
;
TITL bromorf in C2/c
CELL 1.54184  10.1640     6.5048    19.3410    90.0000 102.152   90.0000
ZERR    4.00   0.0009     0.0007     0.0017     0.0000   0.009    0.0000
LATT  7
SYMM -x, y,-z+1/2
SFAC C H Br
UNIT 32 16 24
TEMP -170
SIZE 0.04 0.04 0.015
FMAP   2
PLAN   10
L.S.   4
OMIT     0   8   1
OMIT     0   8   3
OMIT     0   8   2
OMIT    10   4   5
OMIT   -12   0  12
OMIT     0   2  23
OMIT   -10   2  17
OMIT    -8   6   9
OMIT     8   6   3
OMIT     7   5   9
OMIT    10   0  10
OMIT    -8   6   8
OMIT    11   1   7
OMIT    -8   6   6
OMIT     8   2  14
OMIT     9   5   4
OMIT     3   7   9
OMIT     8   4  11
OMIT    -6   6  14
OMIT    -9   1  20
OMIT     9   1  12
OMIT    10   4   4
OMIT     5   3  18
OMIT     9   5   3
OMIT    12   0   2
OMIT     6   2  17
OMIT    -8   6   7
OMIT     9   5   2
OMIT     8   2  13
OMIT    12   2   0
OMIT    -8   6   2
OMIT   -11   1  16
OMIT    11   1   6
OMIT     4   4  17
ACTA 145
CONF
EQIV $1 0.5-x,0.5+y,0.5-z
RTAB CONT BR1 BR2_$1
RTAB ANGL C4 BR1 BR2_$1
RTAB ANGL BR1 BR2_$1 C4_$1
EQIV $2 -0.5+x,-0.5+y,z
RTAB CONT BR1 BR3_$2
RTAB ANGL C4 BR1 BR3_$2
RTAB ANGL BR1 BR3_$2 C4_$2
EQIV $3 1-x,y,0.5-z
RTAB CONT BR2 BR2_$3
RTAB ANGL C4 BR2 BR2_$3
RTAB ANGL BR2 BR2_$3 C4_$3
EQIV $4 0.5-x,-0.5+y,0.5-z
RTAB CONT BR2 BR2_$4
RTAB ANGL C4 BR2 BR2_$4
RTAB ANGL BR2 BR2_$4 C4_$4
RTAB CONT BR2 BR2_$1
RTAB ANGL C4 BR2 BR2_$1
RTAB ANGL BR2 BR2_$1 C4_$1
RTAB CONT BR2 BR3_$2
RTAB ANGL C4 BR2 BR3_$2
RTAB ANGL BR2 BR3_$2 C4_$2
RTAB CONT BR2 BR3_$4
RTAB ANGL C4 BR2 BR3_$4
RTAB ANGL BR2 BR3_$4 C4_$4
RTAB CONT BR3 BR3_$3
RTAB ANGL C4 BR3 BR3_$3
RTAB ANGL BR3 BR3_$3 C4_$3
WGHT    0.076900    1.461400
FVAR       1.60521
BR1   3    0.230640    0.886931    0.393913    11.00000    0.01199    0.02709 =
         0.02901    0.00151    0.00582    0.00241
BR2   3    0.333137    0.578251    0.289806    11.00000    0.02231    0.02960 =
         0.02017   -0.00249    0.00242   -0.00253
BR3   3    0.512520    0.951641    0.353316    11.00000    0.01427    0.03090 =
         0.02590    0.00412    0.00464   -0.00473
C1    1    0.450742    0.615011    0.438337    11.00000    0.00883    0.02424 =
         0.02365   -0.00233    0.00504    0.00000
C2    1    0.548975    0.695903    0.492905    11.00000    0.01335    0.02339 =
         0.02513    0.00009    0.00391   -0.00560
AFIX  43
H2    2    0.582385    0.830698    0.488677    11.00000   -1.20000
AFIX   0
C3    1    0.401233    0.419394    0.446238    11.00000    0.01494    0.02630 =
         0.02462   -0.00328    0.00272   -0.00145
AFIX  43
H3    2    0.332893    0.363421    0.409945    11.00000   -1.20000
AFIX   0
C4    1    0.389484    0.743340    0.374600    11.00000    0.01040    0.02052 =
         0.02174   -0.00070    0.00410    0.00016
HKLF 4
;
_cod_data_source_file            fa3260.cif
_cod_data_source_block           Ib
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2018248
_cod_database_fobs_code          2018248
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Br Br1 0.23064(4) 0.88693(8) 0.39391(2) 0.0225(2) Uani d . 1 1
Br Br2 0.33314(5) 0.57825(9) 0.28981(2) 0.0243(2) Uani d . 1 1
Br Br3 0.51252(4) 0.95164(9) 0.35332(2) 0.0236(2) Uani d . 1 1
C C1 0.4507(4) 0.6150(8) 0.4383(2) 0.0187(9) Uani d . 1 1
C C2 0.5490(4) 0.6959(8) 0.4929(2) 0.0206(9) Uani d . 1 1
H H2 0.5824 0.8307 0.4887 0.025 Uiso calc R 1 1
C C3 0.4012(5) 0.4194(8) 0.4462(3) 0.0222(10) Uani d . 1 1
H H3 0.3329 0.3634 0.4099 0.027 Uiso calc R 1 1
C C4 0.3895(4) 0.7433(7) 0.3746(2) 0.0174(8) Uani d . 1 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br1 0.0120(3) 0.0271(3) 0.0290(3) 0.00241(17) 0.0058(2) 0.00151(19)
Br2 0.0223(3) 0.0296(3) 0.0202(3) -0.00253(19) 0.0024(2) -0.00249(18)
Br3 0.0143(3) 0.0309(4) 0.0259(3) -0.00473(18) 0.0046(2) 0.00412(19)
C1 0.0088(18) 0.024(3) 0.024(2) 0.0000(17) 0.0050(16) -0.0023(18)
C2 0.0134(19) 0.023(3) 0.025(2) -0.0056(17) 0.0039(15) 0.0001(18)
C3 0.015(2) 0.026(3) 0.025(2) -0.0015(18) 0.0027(16) -0.0033(19)
C4 0.0104(18) 0.021(2) 0.0217(19) 0.0002(15) 0.0041(14) -0.0007(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.6763 1.2805 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C3 C1 C2 . . 118.7(5)
C3 C1 C4 . . 120.0(4)
C2 C1 C4 . . 121.0(4)
C1 C2 C3 . 5_666 120.6(5)
C1 C3 C2 . 5_666 120.6(5)
C1 C4 Br2 . . 112.4(3)
C1 C4 Br3 . . 112.6(3)
Br2 C4 Br3 . . 107.14(18)
C1 C4 Br1 . . 108.7(3)
Br2 C4 Br1 . . 108.3(2)
Br3 C4 Br1 . . 107.4(2)
C1 C2 H2 . . 119.7
C3 C2 H2 5_666 . 119.7
C1 C3 H3 . . 119.7
C2 C3 H3 5_666 . 119.7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Br1 C4 . 1.968(4)
Br2 C4 . 1.943(4)
Br3 C4 . 1.946(4)
C1 C3 . 1.389(7)
C1 C2 . 1.394(6)
C1 C4 . 1.510(6)
C3 C2 5_666 1.398(7)
C2 C3 5_666 1.398(7)
C2 H2 . 0.9500
C3 H3 . 0.9500
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_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C3 C1 C2 C3 5_666 1.4(7) ?
C4 C1 C2 C3 5_666 175.8(4) ?
C2 C1 C3 C2 5_666 -1.4(8) ?
C4 C1 C3 C2 5_666 -175.9(4) ?
C3 C1 C4 Br2 . -35.3(5) y
C2 C1 C4 Br2 . 150.3(4) y
C3 C1 C4 Br3 . -156.5(4) y
C2 C1 C4 Br3 . 29.1(5) y
C3 C1 C4 Br1 . 84.6(5) y
C2 C1 C4 Br1 . -89.8(4) y
