#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:59:05 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180406 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/75/7207507.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_7207507
loop_
_publ_author_name
'Sørensen, Thomas Just'
'Hildebrandt, Christoffer B.'
'Elm, Jonas'
'Andreasen, Jens W.'
'Madsen, Anders Ø.'
'Westerlund, Fredrik'
'Laursen, Bo W.'
_publ_section_title
;
 Large area, soft crystalline thin films of
 N,N′,N′′-trialkyltriazatriangulenium salts with
 homeotropic alignment of the discotic cores in a lamellar lattice
;
_journal_issue                   11
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              4797
_journal_paper_doi               10.1039/c2jm15954f
_journal_volume                  22
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C37 H48 N3 +, B F4 -'
_chemical_formula_sum            'C37 H48 B F4 N3'
_chemical_formula_weight         621.23
_chemical_name_common
;N,N',N''-tris(3-methylpentyl)triazatriangulenium
tetrafluoroborate
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 and Encifer'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.570(1)
_cell_length_b                   12.570(1)
_cell_length_c                   35.496(2)
_cell_measurement_reflns_used    510
_cell_measurement_temperature    122.4(5)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.96
_cell_volume                     4857.1(6)
_computing_cell_refinement       'Nonius Collect postrefinement'
_computing_data_collection       'Nonius Collect suite'
_computing_data_reduction        'Nonius Collect suite'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Superflip
_diffrn_ambient_temperature      122.4(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            35280
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1991
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.563
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.563
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.1003
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3425
_refine_ls_wR_factor_ref         0.3734
_reflns_number_gt                1739
_reflns_number_total             2489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2jm15954f.txt
_cod_data_source_block           tata
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7207507
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
N N 0.34009(17) 0.44671(15) 0.11800(5) 0.0340(6) Uani 1 1 d . B .
C1 C 0.3333 0.6667 0.11808(9) 0.0237(8) Uani 1 3 d S . .
C2 C 0.22288(17) 0.55271(17) 0.11830(6) 0.0268(6) Uani 1 1 d . . .
C3 C 0.10773(18) 0.54990(19) 0.11887(6) 0.0315(6) Uani 1 1 d . . .
C4 C -0.0009(2) 0.4368(2) 0.12044(7) 0.0433(7) Uani 1 1 d . . .
H4 H -0.0768 0.4328 0.1209 0.052 Uiso 1 1 calc R . .
C5 C 0.0068(2) 0.3300(2) 0.12132(7) 0.0485(8) Uani 1 1 d . . .
H5 H -0.0660 0.2551 0.1229 0.058 Uiso 1 1 calc R . .
C6 C 0.1160(2) 0.3288(2) 0.12004(7) 0.0434(7) Uani 1 1 d . . .
H6 H 0.1161 0.2548 0.1200 0.052 Uiso 1 1 calc R . .
C7 C 0.22702(18) 0.44133(18) 0.11882(6) 0.0315(6) Uani 1 1 d . . .
C8 C 0.3424(3) 0.3299(2) 0.11603(8) 0.0548(8) Uani 1 1 d . . .
H8A H 0.2891 0.2739 0.1353 0.066 Uiso 1 1 calc R A 1
H8B H 0.4252 0.3459 0.1207 0.066 Uiso 1 1 calc R A 1
C9A C 0.2987(6) 0.2699(5) 0.07653(17) 0.0411(15) Uani 0.458(6) 1 d P B 1
H9A1 H 0.2617 0.1814 0.0786 0.049 Uiso 0.458(6) 1 calc PR B 1
H9A2 H 0.2373 0.2879 0.0668 0.049 Uiso 0.458(6) 1 calc PR B 1
C10A C 0.4071(7) 0.3197(5) 0.05000(18) 0.0465(16) Uani 0.458(6) 1 d P B 1
H10A H 0.4517 0.4095 0.0519 0.056 Uiso 0.458(6) 1 calc PR B 1
C11A C 0.4971(7) 0.2735(7) 0.0599(2) 0.067(2) Uani 0.458(6) 1 d P B 1
H11A H 0.5208 0.2909 0.0859 0.100 Uiso 0.458(6) 1 calc PR B 1
H11B H 0.5688 0.3145 0.0442 0.100 Uiso 0.458(6) 1 calc PR B 1
H11C H 0.4576 0.1865 0.0557 0.100 Uiso 0.458(6) 1 calc PR B 1
C9B C 0.3977(8) 0.3151(5) 0.0781(2) 0.074(2) Uani 0.542(6) 1 d P B 2
H9B1 H 0.4664 0.3937 0.0705 0.089 Uiso 0.542(6) 1 calc PR B 2
H9B2 H 0.4272 0.2577 0.0814 0.089 Uiso 0.542(6) 1 calc PR B 2
C10B C 0.2989(12) 0.2682(9) 0.0481(2) 0.100(3) Uani 0.542(6) 1 d P B 2
H10B H 0.2614 0.3203 0.0486 0.120 Uiso 0.542(6) 1 calc PR B 2
C11B C 0.1968(9) 0.1358(8) 0.0547(2) 0.104(3) Uani 0.542(6) 1 d P B 2
H11D H 0.2309 0.0825 0.0544 0.157 Uiso 0.542(6) 1 calc PR B 2
H11E H 0.1361 0.1119 0.0352 0.157 Uiso 0.542(6) 1 calc PR B 2
H11F H 0.1592 0.1300 0.0788 0.157 Uiso 0.542(6) 1 calc PR B 2
C12 C 0.3601(6) 0.2838(5) 0.00854(11) 0.1155(17) Uani 1 1 d . . .
H12A H 0.3092 0.1952 0.0069 0.139 Uiso 1 1 calc R B 1
H12B H 0.3094 0.3193 0.0022 0.139 Uiso 1 1 calc R B 1
C13 C 0.4594(9) 0.3251(9) -0.01852(19) 0.243(6) Uani 1 1 d . B .
H13A H 0.5317 0.3945 -0.0084 0.365 Uiso 1 1 calc R . .
H13B H 0.4362 0.3485 -0.0415 0.365 Uiso 1 1 calc R . .
H13C H 0.4761 0.2598 -0.0236 0.365 Uiso 1 1 calc R . .
B B 0.0000 0.0000 0.16334(17) 0.0462(13) Uani 1 3 d S . .
F1 F 0.12248(18) 0.06520(19) 0.16500(12) 0.0669(9) Uani 0.75 1 d P . .
F2 F 0.0756(8) 0.0438(6) 0.1318(3) 0.107(3) Uani 0.33 1 d P . .
F3 F 0.0780(10) 0.0348(7) 0.1954(3) 0.088(3) Uani 0.25 1 d P . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C7 N C3 121.87(15) . 2_665
C7 N C8 118.58(18) . .
C3 N C8 119.55(19) 2_665 .
C2 C1 C2 119.997(5) 3_565 2_665
C2 C1 C2 119.996(4) 3_565 .
C2 C1 C2 119.997(4) 2_665 .
C1 C2 C7 119.74(15) . .
C1 C2 C3 119.68(15) . .
C7 C2 C3 120.56(17) . .
N C3 C4 121.55(19) 3_565 .
N C3 C2 119.24(17) 3_565 .
C4 C3 C2 119.21(19) . .
C5 C4 C3 118.6(2) . .
C5 C4 H4 120.7 . .
C3 C4 H4 120.7 . .
C6 C5 C4 123.92(19) . .
C6 C5 H5 118.0 . .
C4 C5 H5 118.0 . .
C5 C6 C7 118.8(2) . .
C5 C6 H6 120.6 . .
C7 C6 H6 120.6 . .
N C7 C6 121.73(18) . .
N C7 C2 119.36(16) . .
C6 C7 C2 118.90(18) . .
N C8 C9A 110.2(3) . .
N C8 C9B 112.7(3) . .
C9A C8 C9B 40.5(3) . .
N C8 H8A 109.6 . .
C9A C8 H8A 109.6 . .
C9B C8 H8A 135.0 . .
N C8 H8B 109.6 . .
C9A C8 H8B 109.6 . .
C9B C8 H8B 71.2 . .
H8A C8 H8B 108.1 . .
C10A C9A C8 109.5(5) . .
C10A C9A H9A1 109.8 . .
C8 C9A H9A1 109.8 . .
C10A C9A H9A2 109.8 . .
C8 C9A H9A2 109.8 . .
H9A1 C9A H9A2 108.2 . .
C9A C10A C11A 112.4(5) . .
C9A C10A C12 109.5(6) . .
C11A C10A C12 110.2(5) . .
C9A C10A H10A 108.2 . .
C11A C10A H10A 108.2 . .
C12 C10A H10A 108.2 . .
C10B C9B C8 108.9(7) . .
C10B C9B H9B1 109.9 . .
C8 C9B H9B1 109.9 . .
C10B C9B H9B2 109.9 . .
C8 C9B H9B2 109.9 . .
H9B1 C9B H9B2 108.3 . .
C9B C10B C11B 113.3(6) . .
C9B C10B C12 109.0(9) . .
C11B C10B C12 111.5(6) . .
C9B C10B H10B 107.6 . .
C11B C10B H10B 107.6 . .
C12 C10B H10B 107.6 . .
C10B C11B H11D 109.5 . .
C10B C11B H11E 109.5 . .
H11D C11B H11E 109.5 . .
C10B C11B H11F 109.5 . .
H11D C11B H11F 109.5 . .
H11E C11B H11F 109.5 . .
C13 C12 C10A 112.7(6) . .
C13 C12 C10B 157.0(7) . .
C10A C12 C10B 44.3(4) . .
C13 C12 H12A 109.0 . .
C10A C12 H12A 109.0 . .
C10B C12 H12A 84.9 . .
C13 C12 H12B 109.0 . .
C10A C12 H12B 109.0 . .
C10B C12 H12B 82.6 . .
H12A C12 H12B 107.8 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
F1 B F1 119.80(5) 3 2
F1 B F1 119.80(5) 3 .
F1 B F1 119.81(5) 2 .
F1 B F2 107.7(4) 3 2
F1 B F2 56.2(5) 2 2
F1 B F2 111.1(4) . 2
F1 B F2 56.2(5) 3 3
F1 B F2 111.1(4) 2 3
F1 B F2 107.7(4) . 3
F2 B F2 61.9(8) 2 3
F1 B F2 111.1(4) 3 .
F1 B F2 107.7(4) 2 .
F1 B F2 56.2(5) . .
F2 B F2 61.9(8) 2 .
F2 B F2 61.9(8) 3 .
F1 B F3 102.1(5) 3 .
F1 B F3 108.3(5) 2 .
F1 B F3 50.9(5) . .
F2 B F3 150.2(5) 2 .
F2 B F3 140.6(5) 3 .
F2 B F3 107.1(7) . .
F1 B F3 50.9(5) 3 3
F1 B F3 102.1(5) 2 3
F1 B F3 108.3(5) . 3
F2 B F3 140.6(5) 2 3
F2 B F3 107.1(7) 3 3
F2 B F3 150.2(5) . 3
F3 B F3 62.5(9) . 3
F1 B F3 108.3(5) 3 2
F1 B F3 50.9(5) 2 2
F1 B F3 102.1(5) . 2
F2 B F3 107.1(7) 2 2
F2 B F3 150.2(5) 3 2
F2 B F3 140.6(5) . 2
F3 B F3 62.5(9) . 2
F3 B F3 62.5(9) 3 2
F3 F1 F2 132.3(5) . .
F3 F1 B 68.3(5) . .
F2 F1 B 64.1(4) . .
F1 F2 B 59.7(4) . .
F1 F2 F2 111.6(3) . 2
B F2 F2 59.1(4) . 2
F1 F2 F2 108.2(4) . 3
B F2 F2 59.1(4) . 3
F2 F2 F2 60.001(1) 2 3
F1 F3 B 60.9(5) . .
F1 F3 F3 113.9(4) . 3
B F3 F3 58.8(5) . 3
F1 F3 F3 107.0(5) . 2
B F3 F3 58.8(5) . 2
F3 F3 F3 59.999(1) 3 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N C7 1.389(3) .
N C3 1.390(3) 2_665
N C8 1.485(3) .
C1 C2 1.4109(19) 3_565
C1 C2 1.4109(19) 2_665
C1 C2 1.4109(19) .
C2 C7 1.427(3) .
C2 C3 1.430(3) .
C3 N 1.390(2) 3_565
C3 C4 1.395(3) .
C4 C5 1.393(4) .
C4 H4 0.9300 .
C5 C6 1.382(4) .
C5 H5 0.9300 .
C6 C7 1.406(3) .
C6 H6 0.9300 .
C8 C9A 1.557(7) .
C8 C9B 1.568(7) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9A C10A 1.511(10) .
C9A H9A1 0.9700 .
C9A H9A2 0.9700 .
C10A C11A 1.549(9) .
C10A C12 1.566(8) .
C10A H10A 0.9800 .
C11A H11A 0.9600 .
C11A H11B 0.9600 .
C11A H11C 0.9600 .
C9B C10B 1.514(14) .
C9B H9B1 0.9700 .
C9B H9B2 0.9700 .
C10B C11B 1.528(14) .
C10B C12 1.566(10) .
C10B H10B 0.9800 .
C11B H11D 0.9600 .
C11B H11E 0.9600 .
C11B H11F 0.9600 .
C12 C13 1.450(10) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
B F1 1.336(2) 3
B F1 1.336(2) 2
B F1 1.336(2) .
B F2 1.392(8) 2
B F2 1.392(8) 3
B F2 1.392(8) .
B F3 1.420(9) .
B F3 1.420(9) 3
B F3 1.420(9) 2
F1 F3 1.186(12) .
F1 F2 1.286(10) .
F2 F2 1.431(16) 2
F2 F2 1.431(16) 3
F3 F3 1.473(18) 3
F3 F3 1.473(18) 2
