#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/82/2018247.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_2018247
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           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.486(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.3150(3)
_cell_length_b                   9.8178(4)
_cell_length_c                   9.8398(4)
_cell_measurement_reflns_used    7251
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7181
_cell_measurement_theta_min      2.9265
_cell_volume                     608.19(5)
_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      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Oxford Xcalibur Eos'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15682
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.79
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    19.762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.533
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0153
_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)+(0.0111P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0256
_refine_ls_wR_factor_ref         0.0260
_reflns_number_gt                1449
_reflns_number_total             1795
_reflns_threshold_expression     I>2σ(I)
_iucr_refine_instructions_details
;
TITL bromai in P2(1)/n
CELL 0.71073   6.3150     9.8178     9.8398    90.0000  94.486   90.0000
ZERR    2.00   0.0003     0.0004     0.0004     0.0000   0.004    0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H Br
UNIT 16 8 12
TEMP -173
SIZE 0.08 0.06 0.03
ACTA 60
CONF
FMAP   2
PLAN  5
L.S.   4
EQIV $1 -1+x,y,z
HTAB C3 Br3_$1
EQIV $2 1-x,-y,1-z
RTAB CONT Br1 Br1_$2
RTAB ANGL C4 Br1 Br1_$2
RTAB ANGL Br1 Br1_$2 C4_$2
EQIV $3 0.5-x,-0.5+y,0.5-z
RTAB CONT Br1 Br2_$3
RTAB ANGL C4 Br1 Br2_$3
RTAB ANGL Br1 Br2_$3 C4_$3
EQIV $4 0.5+x,0.5-y,0.5+z
RTAB CONT Br1 Br2_$4
RTAB ANGL C4 Br1 Br2_$4
RTAB ANGL Br1 Br2_$4 C4_$4
RTAB CONT Br1 Br3_$1
RTAB ANGL C4 Br1 Br3_$1
RTAB ANGL Br1 Br3_$1 C4_$1
EQIV $5 -0.5+x,0.5-y,0.5+z
RTAB CONT Br1 Br3_$5
RTAB ANGL C4 Br1 Br3_$5
RTAB ANGL Br1 Br3_$5 C4_$5
EQIV $6 1-x,1-y,-z
RTAB CONT Br2 Br2_$6
RTAB ANGL C4 Br2 Br2_$6
RTAB ANGL Br2 Br2_$6 C4_$6
RTAB CONT Br2 Br3_$1
RTAB ANGL C4 Br2 Br3_$1
RTAB ANGL Br2 Br3_$1 C4_$1
EQIV $7 1.5-x,0.5+y,0.5-z
RTAB CONT Br2 Br3_$7
RTAB ANGL C4 Br2 Br3_$7
RTAB ANGL Br2 Br3_$7 C4_$7
WGHT    0.011100
FVAR       2.19482
BR1   3    0.484972    0.146733    0.381850    11.00000    0.01701    0.01814 =
         0.00751   -0.00222    0.00278   -0.00361
BR2   3    0.453199    0.374588    0.153810    11.00000    0.02362    0.00858 =
         0.01762   -0.00269   -0.00595    0.00541
BR3   3    0.894486    0.247352    0.250342    11.00000    0.01056    0.01386 =
         0.01406   -0.00617    0.00036   -0.00266
C1    1    0.551617    0.097601    0.101375    11.00000    0.01001    0.00396 =
         0.00601    0.00059    0.00002    0.00077
C2    1    0.705964    0.047544    0.023161    11.00000    0.00733    0.01092 =
         0.01027   -0.00013    0.00029   -0.00183
AFIX  43
H2    2    0.847771    0.079693    0.038053    11.00000   -1.20000
AFIX   0
C3    1    0.343697    0.049565    0.077367    11.00000    0.01265    0.00966 =
         0.00878   -0.00086    0.00348    0.00225
AFIX  43
H3    2    0.235441    0.083459    0.130072    11.00000   -1.20000
AFIX   0
C4    1    0.595852    0.204343    0.210513    11.00000    0.00871    0.00883 =
         0.01000    0.00021    0.00038   -0.00014
HKLF 4
;
_cod_data_source_file            fa3260.cif
_cod_data_source_block           Ia
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2018247
_cod_database_fobs_code          2018247
loop_
_symmetry_equiv_pos_as_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_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 0.48497(3) 0.14673(2) 0.38185(2) 0.01413(5) Uani d . 1 1
Br Br2 0.45320(3) 0.37459(2) 0.15381(2) 0.01700(6) Uani d . 1 1
Br Br3 0.89449(3) 0.24735(2) 0.25034(2) 0.01286(5) Uani d . 1 1
C C1 0.5516(3) 0.09760(18) 0.10138(19) 0.0067(4) Uani d . 1 1
C C2 0.7060(3) 0.04754(19) 0.0232(2) 0.0095(4) Uani d . 1 1
H H2 0.8478 0.0797 0.0381 0.011 Uiso calc R 1 1
C C3 0.3437(3) 0.04956(19) 0.0774(2) 0.0102(4) Uani d . 1 1
H H3 0.2354 0.0835 0.1301 0.012 Uiso calc R 1 1
C C4 0.5959(3) 0.20434(19) 0.2105(2) 0.0092(4) 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 0.01701(11) 0.01814(12) 0.00751(10) -0.00361(9) 0.00278(8) -0.00222(8)
Br2 0.02362(12) 0.00858(10) 0.01762(11) 0.00541(9) -0.00595(9) -0.00269(8)
Br3 0.01056(10) 0.01386(11) 0.01406(11) -0.00266(8) 0.00036(8) -0.00617(8)
C1 0.0100(10) 0.0040(9) 0.0060(10) 0.0008(7) 0.0000(8) 0.0006(7)
C2 0.0073(9) 0.0109(10) 0.0103(10) -0.0018(8) 0.0003(8) -0.0001(8)
C3 0.0127(10) 0.0097(10) 0.0088(10) 0.0022(8) 0.0035(8) -0.0009(8)
C4 0.0087(10) 0.0088(10) 0.0100(10) -0.0001(8) 0.0004(8) 0.0002(8)
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C2 C1 C3 . . 118.76(17)
C2 C1 C4 . . 122.99(17)
C3 C1 C4 . . 118.24(17)
C1 C2 C3 . 3_655 120.73(17)
C2 C3 C1 3_655 . 120.51(18)
C1 C4 Br3 . . 114.63(13)
C1 C4 Br1 . . 110.66(12)
Br3 C4 Br1 . . 107.21(9)
C1 C4 Br2 . . 109.51(13)
Br3 C4 Br2 . . 106.83(9)
Br1 C4 Br2 . . 107.70(9)
C1 C2 H2 . . 119.6
C3 C2 H2 3_655 . 119.6
C2 C3 H3 3_655 . 119.7
C1 C3 H3 . . 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 . 1.959(2)
Br2 C4 . 1.9590(19)
Br3 C4 . 1.9424(19)
C1 C2 . 1.379(3)
C1 C3 . 1.398(3)
C1 C4 . 1.511(3)
C2 C3 3_655 1.392(3)
C3 C2 3_655 1.392(3)
C2 H2 . 0.9500
C3 H3 . 0.9500
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C3 H3 Br3 1_455 0.95 3.00 3.933(2) 166.2
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 3_655 -0.4(3) ?
C4 C1 C2 C3 3_655 -179.16(18) ?
C2 C1 C3 C2 3_655 0.4(3) ?
C4 C1 C3 C2 3_655 179.22(17) ?
C2 C1 C4 Br3 . -8.3(2) y
C3 C1 C4 Br3 . 172.88(14) y
C2 C1 C4 Br1 . -129.69(17) y
C3 C1 C4 Br1 . 51.5(2) y
C2 C1 C4 Br2 . 111.73(18) y
C3 C1 C4 Br2 . -67.09(19) y
