#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:29:39 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180184 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/80/7108032.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_7108032
loop_
_publ_author_name
'Alessandro Del Grosso'
'Ewan Clark'
'Nicholas Montoute'
'Michael Ingleson'
_publ_section_title
;
 Tricationic analogues of boroxines and polyborate anions
;
_journal_name_full               Chem.Commun.
_journal_page_first              7589
_journal_paper_doi               10.1039/c2cc32605a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C5 H5 B Cl2 N, Al Cl4'
_chemical_formula_sum            'C5 H5 Al B Cl6 N'
_chemical_formula_weight         329.59
_chemical_name_systematic
;
?
;
_space_group_IT_number           158
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2"c'
_symmetry_space_group_name_H-M   'P 3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                120.000(5)
_cell_formula_units_Z            6
_cell_length_a                   12.708(5)
_cell_length_b                   12.708(5)
_cell_length_c                   13.720(5)
_cell_measurement_reflns_used    4894
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3961
_cell_measurement_theta_min      2.9644
_cell_volume                     1918.8(13)
_computing_cell_refinement       'SHELXS-97 (Sheldrick, 1990)'
_computing_data_collection       'SHELXS-97 (Sheldrick, 1990)'
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_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  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12034
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    1.371
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2621
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0327
_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)+(0.0398P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                2187
_reflns_number_total             2621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32605a.txt
_cod_data_source_block           omji118_attempt1
_cod_database_code               7108032
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, z+1/2'
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
Cl7 Cl 0.0000 0.0000 0.24414(11) 0.0247(3) Uani 1 3 d S
Cl3 Cl 0.30312(8) 0.49441(7) 0.00423(7) 0.0283(2) Uani 1 1 d .
Cl8 Cl 0.16005(7) 0.00404(10) 0.45259(8) 0.02908(19) Uani 1 1 d .
Cl6 Cl 0.68711(8) 0.50129(7) 0.40263(7) 0.0299(2) Uani 1 1 d .
Cl2 Cl 0.35845(8) 0.42761(8) 0.33808(7) 0.0347(2) Uani 1 1 d .
Al3 Al 0.0000 0.0000 0.40007(13) 0.0188(4) Uani 1 3 d S
Cl4 Cl 0.3333 0.6667 0.20856(12) 0.0338(4) Uani 1 3 d S
Cl5 Cl 0.6667 0.3333 0.19656(11) 0.0310(4) Uani 1 3 d S
Cl1 Cl 0.35680(9) 0.29749(8) 0.15711(8) 0.0387(3) Uani 1 1 d .
Al2 Al 0.6667 0.3333 0.35214(13) 0.0189(4) Uani 1 3 d S
Al1 Al 0.3333 0.6667 0.05179(15) 0.0189(4) Uani 1 3 d S
N1 N 0.5325(2) 0.5380(2) 0.19230(19) 0.0199(6) Uani 1 1 d .
C1 C 0.5830(3) 0.5392(3) 0.1045(2) 0.0230(8) Uani 1 1 d .
H1 H 0.5478 0.4696 0.0661 0.028 Uiso 1 1 calc R
C3 C 0.7370(3) 0.7452(3) 0.1283(2) 0.0244(8) Uani 1 1 d .
H3 H 0.8052 0.8152 0.1062 0.029 Uiso 1 1 calc R
B1 B 0.4221(4) 0.4267(3) 0.2268(3) 0.0230(9) Uani 1 1 d .
C4 C 0.6857(3) 0.7426(3) 0.2183(3) 0.0257(8) Uani 1 1 d .
H4 H 0.7206 0.8113 0.2578 0.031 Uiso 1 1 calc R
C5 C 0.5850(3) 0.6404(3) 0.2486(3) 0.0233(8) Uani 1 1 d .
H5 H 0.5510 0.6399 0.3088 0.028 Uiso 1 1 calc R
C2 C 0.6833(3) 0.6399(3) 0.0721(2) 0.0267(8) Uani 1 1 d .
H2 H 0.7165 0.6388 0.0120 0.032 Uiso 1 1 calc R
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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
B B 0.0013 0.0007 '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
Cl8 Al3 Cl8 109.20(5) 3 .
Cl8 Al3 Cl8 109.20(5) 3 2
Cl8 Al3 Cl8 109.20(5) . 2
Cl8 Al3 Cl7 109.74(5) 3 .
Cl8 Al3 Cl7 109.74(5) . .
Cl8 Al3 Cl7 109.74(5) 2 .
Cl6 Al2 Cl6 109.98(5) 3_665 2_655
Cl6 Al2 Cl6 109.98(5) 3_665 .
Cl6 Al2 Cl6 109.98(5) 2_655 .
Cl6 Al2 Cl5 108.95(6) 3_665 .
Cl6 Al2 Cl5 108.95(6) 2_655 .
Cl6 Al2 Cl5 108.95(6) . .
Cl3 Al1 Cl3 111.03(6) 3_565 2_665
Cl3 Al1 Cl3 111.03(6) 3_565 .
Cl3 Al1 Cl3 111.03(6) 2_665 .
Cl3 Al1 Cl4 107.87(6) 3_565 .
Cl3 Al1 Cl4 107.87(6) 2_665 .
Cl3 Al1 Cl4 107.87(6) . .
C1 N1 C5 119.1(3) . .
C1 N1 B1 120.6(3) . .
C5 N1 B1 120.3(3) . .
C2 C1 N1 121.2(3) . .
C2 C1 H1 119.4 . .
N1 C1 H1 119.4 . .
C4 C3 C2 118.1(3) . .
C4 C3 H3 120.9 . .
C2 C3 H3 120.9 . .
N1 B1 Cl1 120.5(3) . .
N1 B1 Cl2 119.8(3) . .
Cl1 B1 Cl2 119.7(2) . .
C5 C4 C3 120.2(3) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C4 C5 N1 121.1(3) . .
C4 C5 H5 119.5 . .
N1 C5 H5 119.5 . .
C1 C2 C3 120.3(3) . .
C1 C2 H2 119.8 . .
C3 C2 H2 119.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl7 Al3 2.139(2) .
Cl3 Al1 2.1272(13) .
Cl8 Al3 2.1341(12) .
Cl6 Al2 2.1327(13) .
Cl2 B1 1.730(4) .
Al3 Cl8 2.1341(12) 3
Al3 Cl8 2.1341(12) 2
Cl4 Al1 2.151(3) .
Cl5 Al2 2.135(3) .
Cl1 B1 1.714(4) .
Al2 Cl6 2.1327(13) 3_665
Al2 Cl6 2.1327(13) 2_655
Al1 Cl3 2.1272(13) 3_565
Al1 Cl3 2.1272(13) 2_665
N1 C1 1.361(4) .
N1 C5 1.367(4) .
N1 B1 1.487(5) .
C1 C2 1.352(5) .
C1 H1 0.9300 .
C3 C4 1.389(5) .
C3 C2 1.392(5) .
C3 H3 0.9300 .
C4 C5 1.356(5) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C2 H2 0.9300 .
