#------------------------------------------------------------------------------
#$Date: 2016-03-22 14:10:13 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178986 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/09/4120995.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4120995
loop_
_publ_author_name
'Aleksandrs Prokofjevs'
'Jeff W. Kampf'
'Andrey Solovyev'
'Dennis P. Curran'
'Edwin Vedejs'
_publ_section_title
;
 Weakly Stabilized Primary Borenium Cations and Their Dicationic Dimers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15686
_journal_page_last               15689
_journal_paper_doi               10.1021/ja407458k
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C14 H28 B2 N4, 2(Al2 Br7)'
_chemical_formula_sum            'C14 H28 Al4 B2 Br14 N4'
_chemical_formula_weight         1500.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.386(7)
_cell_angle_beta                 92.646(7)
_cell_angle_gamma                93.785(7)
_cell_formula_units_Z            1
_cell_length_a                   9.4348(2)
_cell_length_b                   9.4885(2)
_cell_length_c                   11.5808(8)
_cell_measurement_reflns_used    17391
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.20
_cell_measurement_theta_min      3.90
_cell_volume                     1021.78(8)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85(2)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'micro-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26707
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         4.70
_exptl_absorpt_coefficient_mu    17.238
_exptl_absorpt_correction_T_max  0.2775
_exptl_absorpt_correction_T_min  0.1964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.439
_exptl_crystal_description       prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0371
_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)+(0.0404P)²+4.6037P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                3490
_reflns_number_total             3680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja407458k_si_002.cif
_cod_data_source_block           ap4145
_cod_database_code               4120995
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Br1 Br 0.06971(5) 0.60780(6) 0.21111(5) 0.02293(15) Uani 1 1 d .
Br2 Br 0.25264(6) 0.30618(6) 0.04934(5) 0.03025(17) Uani 1 1 d .
Br3 Br 0.33046(5) 0.40370(6) 0.37610(5) 0.02131(15) Uani 1 1 d .
Br4 Br 0.46478(5) 0.62739(5) 0.15348(4) 0.01665(14) Uani 1 1 d .
Br5 Br 0.47360(6) 1.02226(6) 0.18729(5) 0.02664(16) Uani 1 1 d .
Br6 Br 0.76101(5) 0.83782(6) 0.32804(5) 0.02324(16) Uani 1 1 d .
Br7 Br 0.38617(5) 0.82583(6) 0.44478(5) 0.02289(15) Uani 1 1 d .
Al1 Al 0.26560(14) 0.48160(15) 0.20708(12) 0.0144(3) Uani 1 1 d .
Al2 Al 0.52366(14) 0.84567(15) 0.29280(12) 0.0140(3) Uani 1 1 d .
N1 N 0.1533(4) -0.2114(5) -0.1629(4) 0.0224(10) Uani 1 1 d .
N2 N 0.0022(4) -0.1339(5) -0.2789(4) 0.0207(10) Uani 1 1 d .
C1 C 0.0523(5) -0.1161(6) -0.1681(5) 0.0258(13) Uani 1 1 d .
C2 C 0.1650(5) -0.2883(5) -0.2722(4) 0.0167(10) Uani 1 1 d .
C3 C 0.0690(5) -0.2386(6) -0.3448(4) 0.0173(11) Uani 1 1 d .
C4 C 0.2367(7) -0.2307(9) -0.0583(5) 0.0417(18) Uani 1 1 d .
H4A H 0.2689 -0.1371 -0.0141 0.063 Uiso 1 1 calc R
H4B H 0.3195 -0.2835 -0.0807 0.063 Uiso 1 1 calc R
H4C H 0.1780 -0.2845 -0.0096 0.063 Uiso 1 1 calc R
C6 C 0.0365(6) -0.2853(7) -0.4731(5) 0.0264(13) Uani 1 1 d .
H6A H 0.0986 -0.3600 -0.5017 0.040 Uiso 1 1 calc R
H6B H 0.0527 -0.2035 -0.5149 0.040 Uiso 1 1 calc R
H6C H -0.0631 -0.3229 -0.4866 0.040 Uiso 1 1 calc R
C7 C -0.1095(6) -0.0534(6) -0.3295(6) 0.0292(13) Uani 1 1 d .
H7A H -0.1989 -0.0694 -0.2918 0.044 Uiso 1 1 calc R
H7B H -0.1237 -0.0867 -0.4137 0.044 Uiso 1 1 calc R
H7C H -0.0795 0.0487 -0.3163 0.044 Uiso 1 1 calc R
C11 C 0.2662(6) -0.3988(7) -0.2960(6) 0.0306(13) Uani 1 1 d .
H11A H 0.2553 -0.4408 -0.3787 0.046 Uiso 1 1 calc R
H11B H 0.2473 -0.4735 -0.2473 0.046 Uiso 1 1 calc R
H11C H 0.3635 -0.3559 -0.2779 0.046 Uiso 1 1 calc R
B1 B -0.0009(7) 0.0057(8) -0.0760(6) 0.0308(16) Uani 1 1 d .
H1A H -0.081(6) -0.052(6) -0.010(5) 0.026(16) Uiso 1 1 d .
H1B H -0.054(8) 0.107(8) -0.106(6) 0.04(2) Uiso 1 1 d .
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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Al1 Br4 Al2 113.27(5) . .
Br3 Al1 Br1 115.82(6) . .
Br3 Al1 Br2 113.04(7) . .
Br1 Al1 Br2 111.26(6) . .
Br3 Al1 Br4 107.72(6) . .
Br1 Al1 Br4 108.99(6) . .
Br2 Al1 Br4 98.44(5) . .
Br7 Al2 Br6 116.47(7) . .
Br7 Al2 Br5 115.56(6) . .
Br6 Al2 Br5 111.75(6) . .
Br7 Al2 Br4 105.52(5) . .
Br6 Al2 Br4 102.09(6) . .
Br5 Al2 Br4 103.30(6) . .
C1 N1 C2 109.8(4) . .
C1 N1 C4 125.6(5) . .
C2 N1 C4 124.6(5) . .
C1 N2 C3 110.6(5) . .
C1 N2 C7 126.8(5) . .
C3 N2 C7 122.6(5) . .
N2 C1 N1 106.1(4) . .
N2 C1 B1 120.3(6) . .
N1 C1 B1 133.4(5) . .
C3 C2 N1 106.2(4) . .
C3 C2 C11 130.7(5) . .
N1 C2 C11 123.1(5) . .
C2 C3 N2 107.3(4) . .
C2 C3 C6 128.7(5) . .
N2 C3 C6 124.0(5) . .
N1 C4 H4A 109.5 . .
N1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C3 C6 H6A 109.5 . .
C3 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C3 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N2 C7 H7A 109.5 . .
N2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C2 C11 H11A 109.5 . .
C2 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C2 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C1 B1 B1 122.3(8) . 2
C1 B1 H1A 108(3) . .
B1 B1 H1A 44(3) 2 .
C1 B1 H1B 121(3) . .
B1 B1 H1B 116(3) 2 .
H1A B1 H1B 110(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Al1 2.2662(16) .
Br2 Al1 2.2778(14) .
Br3 Al1 2.2635(16) .
Br4 Al1 2.4178(14) .
Br4 Al2 2.4479(14) .
Br5 Al2 2.2742(17) .
Br6 Al2 2.2656(14) .
Br7 Al2 2.2564(14) .
N1 C1 1.361(8) .
N1 C2 1.379(6) .
N1 C4 1.455(8) .
N2 C1 1.330(8) .
N2 C3 1.368(6) .
N2 C7 1.489(8) .
C1 B1 1.579(8) .
C2 C3 1.360(8) .
C2 C11 1.470(8) .
C3 C6 1.499(7) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
B1 B1 1.778(14) 2
B1 H1A 1.25(6) .
B1 H1B 1.20(7) .
