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#$Date: 2019-11-24 03:58:37 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236600 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/41/1554127.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_1554127
loop_
_publ_author_name
'Inokuchi, Daisuke'
'Hirao, Yasukazu'
'Takahashi, Kazuyuki'
'Matsumoto, Kouzou'
'Mori, Hatsumi'
'Kubo, Takashi'
_publ_section_title
;
 Dynamics of Water Molecules in a 3-Fold Interpenetrated Hydrogen-Bonded
 Organic Framework Based on Tetrakis(4-pyridyl)methane
;
_journal_issue                   11
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              6599
_journal_paper_doi               10.1021/acs.jpcc.8b12421
_journal_volume                  123
_journal_year                    2019
_chemical_formula_moiety         'C21 H18 N4 2+, (B1 F4 1-)2, C2H3N1'
_chemical_formula_sum            'C23 H21 B2 F8 N5'
_chemical_formula_weight         541.07
_chemical_name_systematic
'bis(4-Pyridyl)bis(pyridinium-4-yl)methane bis(tetrafluoroborate) acetonitrile solvate'
_space_group_crystal_system      hexagonal
_space_group_IT_number           178
_space_group_name_Hall           'P 61 2 (0 0 5)'
_space_group_name_H-M_alt        'P 61 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-12-20 deposited with the CCDC.
2018-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   10.6131(2)
_cell_length_b                   10.6131(2)
_cell_length_c                   37.846(3)
_cell_measurement_reflns_used    35110
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.24
_cell_measurement_theta_min      3.51
_cell_volume                     3691.8(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics
;
Yadokari-XG 2009 (K. Wakita, T. Nemoto, et al., 2009)
;
_computing_publication_material
;
Yadokari-XG 2009 (K. Wakita, T. Nemoto, et al., 2009)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    Sir2004
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Rigaku VariMax RAPID FR-E
;
_diffrn_measurement_method       ω
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            46220
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.239
_diffrn_reflns_theta_min         4.811
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical Absorption Correction   March 2001 T. Higashi
    Rigaku Corporation, Tokyo, Japan
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 783 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1108P)²+4.6658P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1944
_refine_ls_wR_factor_ref         0.1951
_reflns_Friedel_coverage         0.567
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2212
_reflns_number_total             2266
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jp8b12421_si_003.cif
_cod_data_source_block           1_AN-100K
_cod_original_sg_symbol_Hall     'P 61 2 (0 0 -1)'
_cod_database_code               1554127
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.600
_shelx_estimated_absorpt_t_max   0.804
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'x-y, x, z+1/6'
'y, -x+y, z+5/6'
'x-y, -y, -z'
'-x, -x+y, -z+2/3'
'y, x, -z+1/3'
'-y, -x, -z+5/6'
'x, x-y, -z+1/6'
'-x+y, y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
N1 N -0.0126(4) 0.2881(4) 0.11470(9) 0.0278(8) Uani 1 1 d . . .
H12 H -0.095463 0.266523 0.104476 0.033 Uiso 1 1 calc R U .
N2 N 0.7422(4) 0.5338(4) 0.09136(10) 0.0303(9) Uani 1 1 d . . .
N3 N 0.7641(13) 0.8821(6) 0.083333 0.153(9) Uani 1 2 d S T P
C1 C 0.3851(5) 0.3851(5) 0.166667 0.0194(11) Uani 1 2 d S T P
C2 C 0.2445(4) 0.3555(4) 0.14779(10) 0.0200(8) Uani 1 1 d . . .
C3 C 0.1927(5) 0.4525(4) 0.14757(10) 0.0224(9) Uani 1 1 d . . .
H1 H 0.245955 0.543782 0.159134 0.027 Uiso 1 1 calc R U .
C4 C 0.0645(5) 0.4165(5) 0.13062(11) 0.0249(9) Uani 1 1 d . . .
H2 H 0.030405 0.483981 0.130255 0.030 Uiso 1 1 calc R U .
C5 C 0.0332(5) 0.1908(5) 0.11389(12) 0.0322(10) Uani 1 1 d . . .
H3 H -0.023637 0.100070 0.102314 0.039 Uiso 1 1 calc R U .
C6 C 0.1620(5) 0.2226(5) 0.12977(11) 0.0250(9) Uani 1 1 d . . .
H4 H 0.195594 0.154882 0.128621 0.030 Uiso 1 1 calc R U .
C7 C 0.5090(5) 0.4327(4) 0.13924(11) 0.0225(9) Uani 1 1 d . . .
C8 C 0.6529(5) 0.4983(5) 0.15067(12) 0.0287(9) Uani 1 1 d . . .
H5 H 0.674276 0.510432 0.175223 0.034 Uiso 1 1 calc R U .
C9 C 0.7646(5) 0.5458(5) 0.12632(12) 0.0297(10) Uani 1 1 d . . .
H6 H 0.861691 0.588949 0.134776 0.036 Uiso 1 1 calc R U .
C10 C 0.6046(5) 0.4700(5) 0.08009(12) 0.0304(10) Uani 1 1 d . . .
H7 H 0.586686 0.459829 0.055373 0.036 Uiso 1 1 calc R U .
C11 C 0.4860(5) 0.4178(5) 0.10299(11) 0.0256(9) Uani 1 1 d . . .
H8 H 0.389771 0.372128 0.093824 0.031 Uiso 1 1 calc R U .
C12 C 0.4740(10) 0.7370(5) 0.083333 0.055(2) Uani 1 2 d S T P
H9 H 0.438419 0.666800 0.063840 0.082 Uiso 0.5 1 calc R U P
H10 H 0.438419 0.805616 0.080352 0.082 Uiso 0.5 1 calc R U P
H11 H 0.438419 0.685213 0.105808 0.082 Uiso 0.5 1 calc R U P
C13 C 0.630(3) 0.8148(15) 0.083333 0.134(8) Uani 1 2 d S T P
F1 F 0.2268(5) 0.2818(4) 0.03412(8) 0.0557(10) Uani 1 1 d . . .
F2 F 0.1827(5) 0.4499(4) 0.05843(9) 0.0640(12) Uani 1 1 d . . .
F3 F 0.1373(8) 0.3975(7) 0.00166(11) 0.107(2) Uani 1 1 d . . .
F4 F 0.3608(7) 0.5123(5) 0.01847(16) 0.117(2) Uani 1 1 d . . .
B1 B 0.2214(8) 0.4057(7) 0.02827(14) 0.0400(14) Uani 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'
N N 0.0311 0.0180 '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'
F F 0.0727 0.0534 '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
C4 N1 C5 121.6(4) . .
C4 N1 H12 119.2 . .
C5 N1 H12 119.2 . .
C10 N2 C9 117.4(4) . .
C2 C1 C2 108.1(4) 9 .
C2 C1 C7 110.9(2) 9 .
C2 C1 C7 109.5(2) . .
C2 C1 C7 109.5(2) 9 9
C2 C1 C7 110.9(2) . 9
C7 C1 C7 108.0(4) . 9
C3 C2 C6 117.4(4) . .
C3 C2 C1 123.7(3) . .
C6 C2 C1 118.9(3) . .
C4 C3 C2 120.1(4) . .
C4 C3 H1 120.0 . .
C2 C3 H1 120.0 . .
N1 C4 C3 120.7(4) . .
N1 C4 H2 119.6 . .
C3 C4 H2 119.6 . .
N1 C5 C6 120.0(4) . .
N1 C5 H3 120.0 . .
C6 C5 H3 120.0 . .
C5 C6 C2 120.1(4) . .
C5 C6 H4 119.9 . .
C2 C6 H4 119.9 . .
C11 C7 C8 116.8(4) . .
C11 C7 C1 123.5(4) . .
C8 C7 C1 119.7(3) . .
C9 C8 C7 120.1(4) . .
C9 C8 H5 120.0 . .
C7 C8 H5 120.0 . .
N2 C9 C8 123.0(4) . .
N2 C9 H6 118.5 . .
C8 C9 H6 118.5 . .
N2 C10 C11 123.0(4) . .
N2 C10 H7 118.5 . .
C11 C10 H7 118.5 . .
C7 C11 C10 119.7(4) . .
C7 C11 H8 120.1 . .
C10 C11 H8 120.1 . .
C13 C12 H9 109.5 . .
C13 C12 H10 109.5 . .
H9 C12 H10 109.5 . .
C13 C12 H11 109.5 . .
H9 C12 H11 109.5 . .
H10 C12 H11 109.5 . .
C13 C12 H9 109(3) . 11_565
H9 C12 H9 141.1 . 11_565
H10 C12 H9 56.3 . 11_565
H11 C12 H9 56.2 . 11_565
C13 C12 H10 109.5(7) . 11_565
H9 C12 H10 56.3 . 11_565
H10 C12 H10 141.1 . 11_565
H11 C12 H10 56.3 . 11_565
H9 C12 H10 109.5 11_565 11_565
C13 C12 H11 109(2) . 11_565
H9 C12 H11 56.3 . 11_565
H10 C12 H11 56.3 . 11_565
H11 C12 H11 141.1 . 11_565
H9 C12 H11 109.5 11_565 11_565
H10 C12 H11 109.5 11_565 11_565
N3 C13 C12 180.0 . .
F3 B1 F1 114.5(6) . .
F3 B1 F2 110.5(5) . .
F1 B1 F2 111.0(4) . .
F3 B1 F4 105.0(6) . .
F1 B1 F4 106.7(5) . .
F2 B1 F4 108.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C4 1.332(6) .
N1 C5 1.343(6) .
N1 H12 0.8800 .
N2 C10 1.336(6) .
N2 C9 1.339(6) .
N3 C13 1.24(3) .
C1 C2 1.539(5) 9
C1 C2 1.539(5) .
C1 C7 1.548(5) .
C1 C7 1.549(5) 9
C2 C3 1.388(6) .
C2 C6 1.409(6) .
C3 C4 1.375(6) .
C3 H1 0.9500 .
C4 H2 0.9500 .
C5 C6 1.372(6) .
C5 H3 0.9500 .
C6 H4 0.9500 .
C7 C11 1.389(6) .
C7 C8 1.393(6) .
C8 C9 1.382(6) .
C8 H5 0.9500 .
C9 H6 0.9500 .
C10 C11 1.395(6) .
C10 H7 0.9500 .
C11 H8 0.9500 .
C12 C13 1.43(3) .
C12 H9 0.9800 .
C12 H10 0.9800 .
C12 H11 0.9800 .
C12 H9 0.98(13) 11_565
C12 H10 0.98(4) 11_565
C12 H11 0.98(10) 11_565
F1 B1 1.363(6) .
F2 B1 1.373(6) .
F3 B1 1.319(8) .
F4 B1 1.391(8) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H12 N2 0.88 1.87 2.741(5) 168.7 11_455
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
_geom_torsion_site_symmetry_1
C2 C1 C2 C3 137.7(4) 9
C7 C1 C2 C3 -101.4(4) .
C7 C1 C2 C3 17.7(5) 9
C2 C1 C2 C6 -41.9(3) 9
C7 C1 C2 C6 79.0(5) .
C7 C1 C2 C6 -161.9(4) 9
C6 C2 C3 C4 0.9(6) .
C1 C2 C3 C4 -178.7(3) .
C5 N1 C4 C3 -1.5(6) .
C2 C3 C4 N1 1.0(6) .
C4 N1 C5 C6 0.2(7) .
N1 C5 C6 C2 1.7(7) .
C3 C2 C6 C5 -2.2(6) .
C1 C2 C6 C5 177.4(4) .
C2 C1 C7 C11 105.8(4) 9
C2 C1 C7 C11 -13.4(5) .
C7 C1 C7 C11 -134.2(4) 9
C2 C1 C7 C8 -76.1(5) 9
C2 C1 C7 C8 164.7(4) .
C7 C1 C7 C8 43.8(3) 9
C11 C7 C8 C9 0.4(6) .
C1 C7 C8 C9 -177.8(4) .
C10 N2 C9 C8 -1.3(7) .
C7 C8 C9 N2 0.9(7) .
C9 N2 C10 C11 0.5(6) .
C8 C7 C11 C10 -1.2(6) .
C1 C7 C11 C10 176.9(4) .
N2 C10 C11 C7 0.7(7) .
