#------------------------------------------------------------------------------
#$Date: 2020-05-02 05:01:40 +0300 (Sat, 02 May 2020) $
#$Revision: 251391 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/33/2243380.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_2243380
loop_
_publ_author_name
'Senchyk, Ganna A.'
'Lysenko, Andrey B.'
'Krautscheid, Harald'
'Domasevitch, Kostiantyn V.'
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of
 4,4'-(propane-1,3-diyl)bis(4H-1,2,4-triazol-1-ium)
 pentafluoridooxidovanadate(V)
;
_journal_coeditor_code           HB7908
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              780
_journal_page_last               784
_journal_paper_doi               10.1107/S205698902000585X
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '(C7 H12 N6) [V F5 O]'
_chemical_formula_moiety         'C7 H12 N6 2+, F5 O V 2-'
_chemical_formula_sum            'C7 H12 F5 N6 O V'
_chemical_formula_weight         342.17
_chemical_name_systematic
;
4,4'-(Propane-1,3-diyl)bis(4H-1,2,4-triazol-1-ium)
pentafluoridooxidovanadate(V)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 97.617(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5915(4)
_cell_length_b                   12.1969(10)
_cell_length_c                   15.5669(10)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.114
_cell_measurement_theta_min      3.221
_cell_volume                     1240.47(15)
_computing_cell_refinement
;
IPDS Software (Stoe & Cie, 2000)
;
_computing_data_collection
;
IPDS Software (Stoe & Cie, 2000)
;
_computing_data_reduction
;
IPDS Software (Stoe & Cie, 2000)
;
_computing_molecular_graphics
;
Diamond (Brandenburg, 1999)
;
_computing_publication_material
;
WinGX  (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2018/1 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Stoe Image plate diffraction system'
_diffrn_measurement_method       'φ oscillation scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10733
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.114
_diffrn_reflns_theta_min         3.221
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.3025
_exptl_absorpt_correction_T_min  0.2718
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0279
_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)+(0.0603P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                2513
_reflns_number_total             2965
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb7908sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243380
_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   0.812
_shelx_estimated_absorpt_t_max   0.845
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V V1 0.13004(4) 0.20736(2) 0.37557(2) 0.02234(9) Uani d 1 . .
O O1 -0.0838(2) 0.25118(10) 0.33158(9) 0.0429(3) Uani d 1 . .
F F1 0.41341(13) 0.14981(7) 0.43607(6) 0.0320(2) Uani d 1 . .
F F2 0.18077(15) 0.11480(7) 0.29038(6) 0.0361(2) Uani d 1 . .
F F3 0.28439(17) 0.31538(8) 0.33574(7) 0.0422(2) Uani d 1 . .
F F4 0.14112(15) 0.29233(6) 0.47771(6) 0.0310(2) Uani d 1 . .
F F5 0.03593(14) 0.09762(7) 0.43649(6) 0.0329(2) Uani d 1 . .
N N1 0.27600(18) -0.00076(9) 0.03807(8) 0.0250(2) Uani d 1 . .
H H1N 0.317783 -0.068386 0.043251 0.038 Uiso calc 1 . .
N N2 0.2150(2) 0.04943(10) -0.03920(8) 0.0290(3) Uani d 1 . .
N N3 0.19669(16) 0.16124(9) 0.07027(8) 0.0214(2) Uani d 1 . .
N N4 0.88170(17) 0.52627(10) 0.14823(8) 0.0260(3) Uani d 1 . .
H H2N 0.961582 0.566665 0.121121 0.039 Uiso calc 1 . .
N N5 0.8618(2) 0.53656(11) 0.23383(9) 0.0333(3) Uani d 1 . .
N N6 0.66746(17) 0.40329(9) 0.17358(8) 0.0237(2) Uani d 1 . .
C C1 0.2642(2) 0.06477(11) 0.10324(10) 0.0262(3) Uani d 1 . .
H H1 0.296938 0.047489 0.162296 0.031 Uiso calc 1 . .
C C2 0.1676(2) 0.14804(11) -0.01688(10) 0.0283(3) Uani d 1 . .
H H2 0.119140 0.203342 -0.056412 0.034 Uiso calc 1 . .
C C3 0.7655(2) 0.44809(10) 0.11223(9) 0.0238(3) Uani d 1 . .
H H3 0.752834 0.426919 0.053704 0.029 Uiso calc 1 . .
C C4 0.7297(2) 0.46124(12) 0.24712(10) 0.0312(3) Uani d 1 . .
H H4 0.682993 0.448455 0.300737 0.037 Uiso calc 1 . .
C C5 0.1521(2) 0.26078(11) 0.11809(10) 0.0261(3) Uani d 1 . .
H H5A 0.139985 0.240949 0.178200 0.031 Uiso calc 1 . .
H H5B 0.020264 0.290896 0.092153 0.031 Uiso calc 1 . .
C C6 0.3158(2) 0.34849(11) 0.11766(10) 0.0270(3) Uani d 1 . .
H H6A 0.330379 0.367237 0.057561 0.032 Uiso calc 1 . .
H H6B 0.272302 0.414699 0.145844 0.032 Uiso calc 1 . .
C C7 0.5216(2) 0.31175(11) 0.16388(10) 0.0274(3) Uani d 1 . .
H H7A 0.504179 0.282923 0.221218 0.033 Uiso calc 1 . .
H H7B 0.575771 0.252713 0.130794 0.033 Uiso calc 1 . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
V V 0.3005 0.5294 '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
O1 V1 F5 . . 97.49(6) y
O1 V1 F2 . . 97.75(6) y
F5 V1 F2 . . 91.86(5) y
O1 V1 F3 . . 96.57(6) y
F5 V1 F3 . . 164.75(5) y
F2 V1 F3 . . 92.06(5) y
O1 V1 F4 . . 96.44(6) y
F5 V1 F4 . . 86.68(4) y
F2 V1 F4 . . 165.81(4) y
F3 V1 F4 . . 85.92(4) y
O1 V1 F1 . . 179.08(6) y
F5 V1 F1 . . 82.13(4) ?
F2 V1 F1 . . 83.11(4) ?
F3 V1 F1 . . 83.73(5) ?
F4 V1 F1 . . 82.71(4) ?
C1 N1 N2 . . 111.79(11) y
C1 N1 H1N . . 124.1 ?
N2 N1 H1N . . 124.1 ?
C2 N2 N1 . . 103.46(12) y
C1 N3 C2 . . 106.01(12) ?
C1 N3 C5 . . 127.58(13) ?
C2 N3 C5 . . 126.34(12) ?
C3 N4 N5 . . 111.17(12) y
C3 N4 H2N . . 124.4 ?
N5 N4 H2N . . 124.4 ?
C4 N5 N4 . . 104.11(12) y
C3 N6 C4 . . 105.54(12) ?
C3 N6 C7 . . 127.50(12) ?
C4 N6 C7 . . 126.96(13) ?
N1 C1 N3 . . 107.01(12) ?
N1 C1 H1 . . 126.5 ?
N3 C1 H1 . . 126.5 ?
N2 C2 N3 . . 111.73(13) ?
N2 C2 H2 . . 124.1 ?
N3 C2 H2 . . 124.1 ?
N4 C3 N6 . . 107.69(13) ?
N4 C3 H3 . . 126.2 ?
N6 C3 H3 . . 126.2 ?
N5 C4 N6 . . 111.47(14) ?
N5 C4 H4 . . 124.3 ?
N6 C4 H4 . . 124.3 ?
N3 C5 C6 . . 112.85(12) ?
N3 C5 H5A . . 109.0 ?
C6 C5 H5A . . 109.0 ?
N3 C5 H5B . . 109.0 ?
C6 C5 H5B . . 109.0 ?
H5A C5 H5B . . 107.8 ?
C7 C6 C5 . . 112.37(11) ?
C7 C6 H6A . . 109.1 ?
C5 C6 H6A . . 109.1 ?
C7 C6 H6B . . 109.1 ?
C5 C6 H6B . . 109.1 ?
H6A C6 H6B . . 107.9 ?
N6 C7 C6 . . 110.88(11) ?
N6 C7 H7A . . 109.5 ?
C6 C7 H7A . . 109.5 ?
N6 C7 H7B . . 109.5 ?
C6 C7 H7B . . 109.5 ?
H7A C7 H7B . . 108.1 ?
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
V1 O1 . 1.5767(12) y
V1 F5 . 1.7977(9) y
V1 F2 . 1.8062(9) y
V1 F3 . 1.8228(10) y
V1 F4 . 1.8913(9) y
V1 F1 . 2.0981(9) y
N1 C1 . 1.3019(19) ?
N1 N2 . 1.3621(18) ?
N1 H1N . 0.8700 ?
N2 C2 . 1.3014(19) ?
N3 C1 . 1.3361(16) ?
N3 C2 . 1.354(2) ?
N3 C5 . 1.4740(17) ?
N4 C3 . 1.3022(17) ?
N4 N5 . 1.362(2) ?
N4 H2N . 0.8700 ?
N5 C4 . 1.301(2) ?
N6 C3 . 1.3387(19) ?
N6 C4 . 1.3615(19) ?
N6 C7 . 1.4683(17) ?
C1 H1 . 0.9400 ?
C2 H2 . 0.9400 ?
C3 H3 . 0.9400 ?
C4 H4 . 0.9400 ?
C5 C6 . 1.5201(19) ?
C5 H5A . 0.9800 ?
C5 H5B . 0.9800 ?
C6 C7 . 1.5160(19) ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C7 H7A . 0.9800 ?
C7 H7B . 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
_geom_hbond_publ_flag
N1 H1N F4 2_545 0.87 1.76 2.6007(14) 163 yes
N4 H2N F1 2_655 0.87 1.64 2.5072(15) 173 yes
C1 H1 F2 . 0.94 2.37 3.0962(18) 133 yes
C1 H1 N5 2_645 0.94 2.59 3.3122(19) 134 yes
C2 H2 F1 4_565 0.94 2.24 3.0163(16) 139 yes
C3 H3 F1 4_665 0.94 2.42 3.2565(18) 148 yes
C3 H3 F5 4_665 0.94 2.18 2.9980(17) 144 yes
C4 H4 N2 4_666 0.94 2.47 3.343(2) 154 yes
C5 H5A F2 . 0.98 2.32 3.2039(18) 150 yes
C5 H5B F1 4_565 0.98 2.54 3.2422(18) 128 yes
C6 H6A F5 4_665 0.98 2.50 3.4021(19) 153 yes
C7 H7A F3 . 0.98 2.47 3.2728(19) 139 yes
C7 H7B F4 4_665 0.98 2.54 3.3522(19) 141 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 N1 N2 C2 . . . . 0.38(16) ?
C3 N4 N5 C4 . . . . 0.12(16) ?
N2 N1 C1 N3 . . . . -0.72(16) ?
C2 N3 C1 N1 . . . . 0.74(15) ?
C5 N3 C1 N1 . . . . 177.92(12) ?
N1 N2 C2 N3 . . . . 0.11(16) ?
C1 N3 C2 N2 . . . . -0.54(17) ?
C5 N3 C2 N2 . . . . -177.76(13) ?
N5 N4 C3 N6 . . . . -0.88(15) ?
C4 N6 C3 N4 . . . . 1.23(14) ?
C7 N6 C3 N4 . . . . -179.39(12) ?
N4 N5 C4 N6 . . . . 0.68(17) ?
C3 N6 C4 N5 . . . . -1.21(16) ?
C7 N6 C4 N5 . . . . 179.41(12) ?
C1 N3 C5 C6 . . . . 104.60(16) ?
C2 N3 C5 C6 . . . . -78.76(17) ?
N3 C5 C6 C7 . . . . -63.73(17) y
C3 N6 C7 C6 . . . . -75.14(17) ?
C4 N6 C7 C6 . . . . 104.11(16) ?
C5 C6 C7 N6 . . . . -171.58(12) y

_cod_database_fobs_code 2243380
