#------------------------------------------------------------------------------
#$Date: 2016-02-20 17:35:30 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/57/2215788.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_2215788
loop_
_publ_author_name
'Fuks, Gad'
'Saffon, Nathalie'
'Bourissou, Didier'
'Bertrand, Guy'
_publ_section_title
;
 2,2,4,4-Tetrabromo-1,1,3,3-tetramethylcyclodiborazane
;
_journal_coeditor_code           BR2057
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4476
_journal_page_last               o4476
_journal_paper_doi               10.1107/S1600536807052385
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C4 H12 B2 Br4 N2'
_chemical_formula_moiety         'C4 H12 B2 Br4 N2'
_chemical_formula_sum            'C4 H12 B2 Br4 N2'
_chemical_formula_weight         429.42
_chemical_melting_point          340
_chemical_name_common
;
Bis(μ-dimethylamine-N:N)bis(dibromoboron)
;
_chemical_name_systematic
;
2,2,4,4-Tetrabromo-1,1,3,3-tetramethylcyclodiborazane
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 120.074(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1089(13)
_cell_length_b                   8.7842(10)
_cell_length_c                   6.9077(8)
_cell_measurement_reflns_used    1609
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      3.14
_cell_volume                     583.33(12)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'SMART (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2006)'
_computing_publication_material  'SHELXTL (Bruker, 2006)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2689
_diffrn_reflns_theta_full        28.18
_diffrn_reflns_theta_max         28.18
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    13.751
_exptl_absorpt_correction_T_max  0.662
_exptl_absorpt_correction_T_min  0.210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.744
_refine_diff_density_min         -1.423
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0389P)²+1.911P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                683
_reflns_number_total             769
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            br2057.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2215788
_cod_database_fobs_code          2215788
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Br Br1 1.17185(5) 0.0000 0.31107(9) 0.03261(19) Uani d S 1
Br Br2 1.28193(6) 0.0000 0.83699(9) 0.0429(2) Uani d S 1
N N1 1.0000 0.1319(4) 0.5000 0.0230(8) Uani d S 1
B B1 1.1096(5) 0.0000 0.5364(8) 0.0205(9) Uani d S 1
C C1 1.0398(4) 0.2347(5) 0.6963(9) 0.0449(10) Uani d . 1
H H1A 1.1199 0.2969 0.7227 0.067 Uiso calc R 1
H H1C 1.0644 0.1731 0.8293 0.067 Uiso calc R 1
H H1B 0.9613 0.3012 0.6651 0.067 Uiso calc R 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 0.0359(3) 0.0390(3) 0.0348(3) 0.000 0.0266(2) 0.000
Br2 0.0411(3) 0.0391(4) 0.0231(3) 0.000 -0.0028(2) 0.000
N1 0.0233(18) 0.0197(18) 0.0300(19) 0.000 0.0164(16) 0.000
B1 0.018(2) 0.023(2) 0.022(2) 0.000 0.0107(18) 0.000
C1 0.042(2) 0.037(2) 0.069(3) -0.0175(17) 0.037(2) -0.032(2)
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'
B B 0.0013 0.0007 '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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 N1 C1 . 2_756 106.0(5) yes
C1 N1 B1 . 5_756 115.7(2) yes
C1 N1 B1 2_756 5_756 115.8(3) ?
C1 N1 B1 . . 115.8(3) ?
C1 N1 B1 2_756 . 115.7(2) ?
B1 N1 B1 5_756 . 87.7(3) yes
N1 B1 N1 5_756 . 92.3(3) ?
N1 B1 Br1 5_756 . 114.2(2) yes
N1 B1 Br1 . . 114.2(2) ?
N1 B1 Br2 5_756 . 114.8(2) ?
N1 B1 Br2 . . 114.8(2) ?
Br1 B1 Br2 . . 106.5(2) ?
N1 C1 H1A . . 109.5 ?
N1 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
N1 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
H1C C1 H1B . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 B1 . 1.995(5) yes
Br2 B1 . 1.998(5) yes
N1 C1 . 1.499(4) yes
N1 C1 2_756 1.499(4) ?
N1 B1 5_756 1.606(4) ?
N1 B1 . 1.606(4) yes
B1 N1 5_756 1.606(4) ?
C1 H1A . 0.9800 ?
C1 H1C . 0.9800 ?
C1 H1B . 0.9800 ?
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
C1 H1A Br1 7_756 0.98 3.02 3.982(4) 166.8
