#------------------------------------------------------------------------------
#$Date: 2016-01-14 04:27:54 +0100 (jue 14 de ene de 2016) $
#$Revision: 174447 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/14/2241462.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_2241462
loop_
_publ_author_name
'Britton, Doyle'
'Noland, Wayland E.'
'Tritch, Kenneth J.'
_publ_section_title
;
 Two new polytypes of 2,4,6-tribromobenzonitrile
;
_journal_coeditor_code           LH5796
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              178
_journal_page_last               183
_journal_paper_doi               10.1107/S2056989016000256
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C7 H2 Br3 N'
_chemical_formula_moiety         'C7 H2 Br3 N'
_chemical_formula_sum            'C7 H2 Br3 N'
_chemical_formula_weight         339.83
_chemical_name_systematic
;
 2,4,6-Tribromobenzonitrile - polytype I
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.8742(15)
_cell_length_b                   10.247(3)
_cell_length_c                   8.683(3)
_cell_measurement_reflns_used    2049
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.35
_cell_volume                     432.0(2)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), enCIFer (Allen et al.,
2004),
and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Bruker 1K area-detector diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1270
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4093
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        '< 1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.934
_exptl_absorpt_correction_T_max  0.248
_exptl_absorpt_correction_T_min  0.080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2002)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.356
_refine_diff_density_min         -1.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0462
_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)+(0.0690P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                856
_reflns_number_total             1024
_reflns_threshold_expression     '>2σ(I) '
_iucr_refine_instructions_details
;
TITL RCN-I in P2(1)/m
CELL 0.71073   4.8742  10.247   8.683  90.000  94.97  90.000
ZERR    2.00   0.0015   0.003   0.003   0.000   0.01   0.000
LATT  1
SYMM -X, 0.5+Y, -Z
SFAC C H N BR
UNIT 14 4 2 6
TEMP -100
L.S.10
BOND $h
FMAP 2
PLAN 5
acta
WGHT    0.069000
FVAR       0.43013
BR12   4    0.333556    0.473244    0.186758    11.00000    0.03343    0.01596 =
         0.03370   -0.00162   -0.00154   -0.00427
BR14   4    1.113227    0.750000    0.578201    10.50000    0.02285    0.02388 =
         0.02946    0.00000   -0.00178    0.00000
N17    3   -0.026313    0.750000   -0.014738    10.50000    0.04076    0.02098 =
         0.03072    0.00000   -0.00582    0.00000
C11    1    0.382769    0.750000    0.196030    10.50000    0.02250    0.02451 =
         0.01474    0.00000    0.00455    0.00000
C12    1    0.493243    0.632445    0.255884    11.00000    0.02338    0.01572 =
         0.02874    0.00146    0.00614   -0.00116
C13    1    0.710709    0.631326    0.368818    11.00000    0.02438    0.01705 =
         0.03276    0.00416    0.00732    0.00368
AFIX  43
H13    2    0.784217    0.551239    0.409105    11.00000   -1.20000
AFIX   0
C14    1    0.819959    0.750000    0.422392    10.50000    0.02362    0.02473 =
         0.01088    0.00000    0.00274    0.00000
C17    1    0.152257    0.750000    0.079888    10.50000    0.02952    0.01089 =
         0.03220    0.00000    0.00406    0.00000
HKLF 4
REM  new in P2(1)/m
REM R1 =  0.0462 for    856 Fo > 4sig(Fo)  and  0.0563 for all   1024 data
REM     58 parameters refined using      0 restraints
END
WGHT      0.0693      0.0000
REM Highest difference peak  1.356,  deepest hole -1.284,  1-sigma level  0.256
Q1    1   0.3194  0.5008  0.0803  11.00000  0.05    1.36
Q2    1   0.3055  0.4481  0.0816  11.00000  0.05    1.30
Q3    1   1.1380  0.7035  0.6615  11.00000  0.05    1.18
Q4    1   0.3424  0.5165  0.2638  11.00000  0.05    1.12
Q5    1   1.1261  0.7500  0.7037  10.50000  0.05    1.11
;
_cod_data_source_file            lh5796sup1.cif
_cod_data_source_block           RCN-I
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2241462
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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 Br12 0.33356(11) 0.47324(5) 0.18676(7) 0.0280(2) Uani d . 1 1
Br Br14 1.11323(14) 0.7500 0.57820(9) 0.0256(3) Uani d S 1 2
N N17 -0.0263(14) 0.7500 -0.0147(8) 0.0313(16) Uani d S 1 2
C C11 0.3828(14) 0.7500 0.1960(8) 0.0204(15) Uani d S 1 2
C C12 0.4932(10) 0.6324(5) 0.2559(6) 0.0224(11) Uani d . 1 1
C C13 0.7107(10) 0.6313(5) 0.3688(6) 0.0244(11) Uani d . 1 1
H H13 0.7842 0.5512 0.4091 0.029 Uiso calc R 1 1
C C14 0.8200(14) 0.7500 0.4224(8) 0.0197(15) Uani d S 1 2
C C17 0.1523(16) 0.7500 0.0799(9) 0.0241(16) Uani d S 1 2
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
Br12 0.0334(4) 0.0160(3) 0.0337(4) -0.0043(2) -0.0015(2) -0.0016(2)
Br14 0.0229(4) 0.0239(4) 0.0295(5) 0.000 -0.0018(3) 0.000
N17 0.041(4) 0.021(3) 0.031(4) 0.000 -0.006(3) 0.000
C11 0.022(3) 0.025(4) 0.015(4) 0.000 0.005(3) 0.000
C12 0.023(2) 0.016(2) 0.029(3) -0.0012(19) 0.006(2) 0.001(2)
C13 0.024(2) 0.017(3) 0.033(3) 0.004(2) 0.007(2) 0.004(2)
C14 0.024(3) 0.025(4) 0.011(3) 0.000 0.003(3) 0.000
C17 0.030(4) 0.011(3) 0.032(4) 0.000 0.004(3) 0.000
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'
N N 0.0061 0.0033 '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_3
_geom_angle
C12 C11 C12 4_575 118.6(6)
C12 C11 C17 . 120.7(3)
C13 C12 C11 . 121.2(5)
C13 C12 Br12 . 119.3(4)
C11 C12 Br12 . 119.4(4)
C12 C13 C14 . 118.6(5)
C12 C13 H13 . 120.7
C14 C13 H13 . 120.7
C13 C14 C13 4_575 121.9(6)
C13 C14 Br14 . 119.0(3)
N17 C17 C11 . 178.4(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Br12 C12 1.883(5)
Br14 C14 1.881(7)
C11 C12 1.401(6)
C11 C17 1.443(10)
C12 C13 1.380(8)
C13 C14 1.391(6)
C13 H13 0.9500
N17 C17 1.144(10)
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_1
_geom_torsion_site_symmetry_4
_geom_torsion
C12 C11 C12 C13 4_575 . -1.6(11)
C17 C11 C12 C13 . . -178.9(7)
C12 C11 C12 Br12 4_575 . 176.0(3)
C17 C11 C12 Br12 . . -1.3(9)
C11 C12 C13 C14 . . -0.2(10)
Br12 C12 C13 C14 . . -177.8(5)
C12 C13 C14 C13 . 4_575 2.0(12)
C12 C13 C14 Br14 . . 179.2(5)

_cod_database_fobs_code 2241462
