#------------------------------------------------------------------------------
#$Date: 2022-05-11 00:30:47 +0200 (Wed 11 de May de 2022) $
#$Revision: 275307 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/49/7244907.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_7244907
loop_
_publ_author_name
'Feng, Yan'
'Wang, Ze-Jie'
'Li, Long-He'
'Liao, Rong-Meng'
'Hu, Zhao-Bo'
'Li, Jian-Rong'
'Shi, Chao'
'Ye, Heng-Yun'
_publ_section_title
;
 Structural Phase Transition and Switchable Dielectric Behaviour of a
 One-Dimensional Chains Niobium Oxyfluoride
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00428C
_journal_year                    2022
_chemical_formula_moiety         'F4 Nb O, C3 H5 N2'
_chemical_formula_sum            'C3 H5 F4 N2 Nb O'
_chemical_formula_weight         254.00
_chemical_name_systematic        '[HImidazole][(NbOF4]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-10-20
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2021-12-21 deposited with the CCDC.	2022-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.765(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.7682(7)
_cell_length_b                   3.9248(4)
_cell_length_c                   13.5199(15)
_cell_measurement_reflns_used    2058
_cell_measurement_temperature    270(2)
_cell_measurement_theta_max      29.8200
_cell_measurement_theta_min      3.0010
_cell_volume                     358.72(7)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution
'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      270(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  HyPix
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            639
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.021
_diffrn_reflns_theta_max         25.021
_diffrn_reflns_theta_min         3.013
_exptl_absorpt_coefficient_mu    1.698
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62688
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.352
_exptl_crystal_description       irregular
_exptl_crystal_F_000             693
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.966
_refine_diff_density_min         -3.727
_refine_diff_density_rms         0.342
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         639
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0895
_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)+(0.0554P)²+8.8685P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2225
_refine_ls_wR_factor_ref         0.2241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                617
_reflns_number_total             639
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00428c3.cif
_cod_data_source_block           x_tw
_cod_database_code               7244907
_shelx_shelxl_version_number     2018/1
_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_max   0.750
_shelx_estimated_absorpt_t_min   0.728
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C1-C2
 1.39 with sigma of 0.01
 N1-C1 = N2-C2 = N1-C3 = N2-C3
 1.4 with sigma of 0.02
 N1-C2 \\sim N2-C1 \\sim C1-C3 \\sim C2-C3
 with sigma of 0.02
3. Restrained planarity
 N1, N2, C1, C2, C3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3: within 3.8A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 3.8A
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O1(0.5) N1(0.5) H1(0.5) N2(0.5) H2(0.5) C1(0.5) H1a(0.5) C2(0.5)
 H2a(0.5) C3(0.5) H3(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C1(H1a), C2(H2a), C3(H3)
;
_shelx_res_file
;
TITL 1_a.res in C2/c New:P2/c
    x_tw.res
    created by SHELXL-2018/1 at 20:03:57 on 04-Oct-2021
rem isor 0.01 O1
REM Instructions for potential hydrogen bonds
CELL 0.71073 6.7682 3.9248 13.5199 90 92.765 90
ZERR 2 0.0007 0.0004 0.0015 0 0.01 0
LATT 1
SYMM -X,+Y,0.5-Z
SFAC C H F N Nb O
UNIT 6 10 8 4 2 2
EQIV $1 +X,1+Y,+Z
EQIV $2 1-X,+Y,0.5-Z
EQIV $3 1+X,1+Y,+Z
EQIV $4 1-X,-Y,-Z
EQIV $5 2-X,1-Y,-Z
EQIV $6 1+X,-Y,-0.5+Z
FLAT N1 N2 C1 C2 C3
DFIX 1.39 0.01 C1 C2
DFIX 1.4 N1 C1 N2 C2 N1 C3 N2 C3
SADI N1 C2 N2 C1 C1 C3 C2 C3
SIMU 0.02 0.04 3.8 $n $c
ISOR 0.01 0.02 O1

L.S. 5
PLAN  1
SIZE 0.18 0.2 0.19
CONF
HTAB N1 F1_$3
HTAB N2 F1_$4
HTAB N2 F2_$4
HTAB C1 F2_$3
HTAB C1 F2_$5
HTAB C2 F1_$6
HTAB C3 F2_$1
HTAB C3 O1_$2
FREE O1 O1_$2
BOND $h
htab
MORE -1
fmap 2
acta
SHEL 999 0.84
REM <olex2.extras>
REM <HklSrc "%.\\x_tw.hkl">
REM </olex2.extras>

WGHT    0.055400    8.868501
FVAR      13.77026
NB1   5    0.500000    0.068226    0.250000    10.50000    0.03438    0.02476 =
         0.03221    0.00000   -0.00181    0.00000
F1    3    0.222775   -0.001713    0.245867    11.00000    0.03036    0.09213 =
         0.08711   -0.00066    0.00248   -0.00291
F2    3    0.490054    0.006958    0.110938    11.00000    0.08749    0.10057 =
         0.02575    0.00267    0.00160   -0.00098
O1    6    0.467062    0.508921    0.264926    10.50000    0.04970    0.02214 =
         0.04903    0.00557    0.01176   -0.00404
PART -1
N1    4    1.048378    0.634809    0.075937    10.50000    0.04234    0.06235 =
         0.03602   -0.00930    0.00750   -0.01344
AFIX  43
H1    2    1.085595    0.727500    0.131388    10.50000   -1.20000
AFIX   0
N2    4    0.864662    0.385076   -0.042443    10.50000    0.04287    0.06414 =
         0.03809   -0.01875    0.00504   -0.01062
AFIX  43
H2    2    0.765595    0.292709   -0.074389    10.50000   -1.20000
AFIX   0
C1    1    1.167914    0.573855   -0.002268    10.50000    0.04105    0.06752 =
         0.03307   -0.01610    0.00685   -0.01385
AFIX  43
H1A   2    1.301422    0.627623   -0.004656    10.50000   -1.20000
AFIX   0
C2    1    1.052133    0.418080   -0.076300    10.50000    0.03894    0.06079 =
         0.03383   -0.01519    0.00481   -0.01334
AFIX  43
H2A   2    1.093478    0.348426   -0.137715    10.50000   -1.20000
AFIX   0
C3    1    0.861610    0.523687    0.050662    10.50000    0.03973    0.06061 =
         0.03768   -0.01809    0.00580   -0.01480
AFIX  43
H3    2    0.752197    0.539104    0.089474    10.50000   -1.20000
AFIX   0
HKLF 5




REM  1_a.res in C2/c New:P2/c
REM R1 =  0.0895 for     617 Fo > 4sig(Fo)  and  0.0920 for all     639 data
REM     78 parameters refined using     79 restraints

END

WGHT      0.0554      8.8686

REM Instructions for potential hydrogen bonds
HTAB N1 F1_$3
HTAB N2 F1_$4
HTAB N2 F2_$4
HTAB C1 F2_$3
HTAB C1 F2_$5
HTAB C2 F1_$6
HTAB C3 F2_$1
HTAB C3 O1_$2

REM Highest difference peak  2.966,  deepest hole -3.727,  1-sigma level  0.342
Q1    1   0.4165 -0.1963  0.2492  11.00000  0.05    2.97
;
_shelx_res_checksum              67493
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.500000 0.0682(5) 0.250000 0.0306(7) Uani 1 2 d S T P . .
F1 F 0.2228(15) -0.002(3) 0.2459(10) 0.070(3) Uani 1 1 d . . . . .
F2 F 0.4901(19) 0.007(3) 0.1109(7) 0.071(4) Uani 1 1 d . . . . .
O1 O 0.467(4) 0.509(5) 0.265(2) 0.040(7) Uani 0.5 1 d . U P . .
N1 N 1.048(7) 0.635(7) 0.0759(18) 0.047(6) Uani 0.5 1 d D U P A -1
H1 H 1.085595 0.727500 0.131388 0.056 Uiso 0.5 1 calc R U P A -1
N2 N 0.865(5) 0.385(8) -0.042(3) 0.048(6) Uani 0.5 1 d D U P A -1
H2 H 0.765595 0.292709 -0.074389 0.058 Uiso 0.5 1 calc R U P A -1
C1 C 1.168(3) 0.574(10) -0.002(4) 0.047(6) Uani 0.5 1 d D U P A -1
H1A H 1.301422 0.627623 -0.004656 0.056 Uiso 0.5 1 calc R U P A -1
C2 C 1.052(8) 0.418(9) -0.0763(17) 0.044(6) Uani 0.5 1 d D U P A -1
H2A H 1.093478 0.348426 -0.137715 0.053 Uiso 0.5 1 calc R U P A -1
C3 C 0.862(5) 0.524(9) 0.051(3) 0.046(6) Uani 0.5 1 d D U P A -1
H3 H 0.752197 0.539104 0.089474 0.055 Uiso 0.5 1 calc R U P A -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nb1 0.0344(11) 0.0248(11) 0.0322(11) 0.000 -0.0018(8) 0.000
F1 0.030(5) 0.092(9) 0.087(8) -0.001(8) 0.002(5) -0.003(6)
F2 0.087(8) 0.101(10) 0.026(5) 0.003(5) 0.002(5) -0.001(8)
O1 0.050(11) 0.022(8) 0.049(11) 0.006(7) 0.012(8) -0.004(7)
N1 0.042(14) 0.062(12) 0.036(11) -0.009(10) 0.008(11) -0.013(12)
N2 0.043(13) 0.064(12) 0.038(13) -0.019(11) 0.005(10) -0.011(12)
C1 0.041(12) 0.068(13) 0.033(13) -0.016(12) 0.007(11) -0.014(12)
C2 0.039(14) 0.061(13) 0.034(11) -0.015(10) 0.005(11) -0.013(13)
C3 0.040(13) 0.061(13) 0.038(13) -0.018(11) 0.006(11) -0.015(12)
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'
F F 0.0171 0.0103 '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'
Nb Nb -2.0727 0.6215 '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'
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
_geom_angle_publ_flag
F1 Nb1 F1 163.3(8) . 2_655 ?
F1 Nb1 O1 87.6(8) . 2_645 ?
F1 Nb1 O1 75.8(8) 2_655 2_645 ?
F1 Nb1 O1 75.8(8) . 1_545 ?
F1 Nb1 O1 87.6(8) 2_655 1_545 ?
F2 Nb1 F1 89.9(6) . 2_655 ?
F2 Nb1 F1 88.0(6) . . ?
F2 Nb1 F1 89.9(6) 2_655 . ?
F2 Nb1 F1 88.0(6) 2_655 2_655 ?
F2 Nb1 F2 165.4(8) . 2_655 ?
F2 Nb1 O1 88.0(8) 2_655 2_645 ?
F2 Nb1 O1 77.5(8) 2_655 1_545 ?
F2 Nb1 O1 77.5(8) . 2_645 ?
F2 Nb1 O1 88.0(8) . 1_545 ?
O1 Nb1 F1 105.7(10) . 2_655 ?
O1 Nb1 F1 90.9(10) . . ?
O1 Nb1 F1 105.7(10) 2_655 . ?
O1 Nb1 F1 90.9(10) 2_655 2_655 ?
O1 Nb1 F2 90.6(10) 2_655 . ?
O1 Nb1 F2 103.9(10) . . ?
O1 Nb1 F2 90.6(10) . 2_655 ?
O1 Nb1 F2 103.9(10) 2_655 2_655 ?
O1 Nb1 O1 20.2(13) 2_655 . ?
O1 Nb1 O1 161.9(12) 2_655 2_645 ?
O1 Nb1 O1 161.9(12) . 1_545 ?
O1 Nb1 O1 177.9(2) 2_655 1_545 ?
O1 Nb1 O1 16.0(10) 2_645 1_545 ?
O1 Nb1 O1 177.9(2) . 2_645 ?
Nb1 O1 Nb1 161.9(12) . 1_565 ?
C1 N1 H1 125.6 . . ?
C3 N1 H1 125.6 . . ?
C3 N1 C1 108.8(11) . . ?
C2 N2 H2 125.6 . . ?
C3 N2 H2 125.6 . . ?
C3 N2 C2 108.8(11) . . ?
N1 C1 H1A 126.3 . . ?
N1 C1 C2 107.3(10) . . ?
C2 C1 H1A 126.3 . . ?
N2 C2 C1 107.5(10) . . ?
N2 C2 H2A 126.3 . . ?
C1 C2 H2A 126.3 . . ?
N1 C3 N2 107.6(10) . . ?
N1 C3 H3 126.2 . . ?
N2 C3 H3 126.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 F1 1.894(10) 2_655 ?
Nb1 F1 1.894(10) . ?
Nb1 F2 1.893(10) . ?
Nb1 F2 1.893(10) 2_655 ?
Nb1 O1 2.217(18) 1_545 ?
Nb1 O1 1.757(19) 2_655 ?
Nb1 O1 2.217(18) 2_645 ?
Nb1 O1 1.757(19) . ?
N1 H1 0.8600 . ?
N1 C1 1.383(18) . ?
N1 C3 1.365(19) . ?
N2 H2 0.8600 . ?
N2 C2 1.376(18) . ?
N2 C3 1.372(18) . ?
C1 H1A 0.9300 . ?
C1 C2 1.383(10) . ?
C2 H2A 0.9300 . ?
C3 H3 0.9300 . ?
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
_geom_hbond_publ_flag
N1 H1 F1 0.86 2.06 2.91(2) 167.2 1_665 yes
N2 H2 F1 0.86 2.59 3.17(4) 125.4 3_655 yes
N2 H2 F2 0.86 2.13 2.96(2) 162.6 3_655 yes
C1 H1A F2 0.93 2.51 3.25(3) 136.3 3_765 yes
C1 H1A F2 0.93 2.47 3.11(4) 126.0 1_665 yes
C2 H2A F1 0.93 2.29 3.17(2) 158.6 4_655 yes
C3 H3 F2 0.93 2.58 3.28(3) 132.9 1_565 yes
C3 H3 O1 0.93 2.52 3.42(3) 162.0 2_655 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F1 Nb1 O1 Nb1 -138(6) . . . 1_565 ?
F1 Nb1 O1 Nb1 44(6) 2_655 . . 1_565 ?
F2 Nb1 O1 Nb1 -50(6) . . . 1_565 ?
F2 Nb1 O1 Nb1 132(6) 2_655 . . 1_565 ?
O1 Nb1 O1 Nb1 0.000(17) 2_655 . . 1_565 ?
O1 Nb1 O1 Nb1 180.001(17) 1_545 . . 1_565 ?
N1 C1 C2 N2 0(2) . . . . ?
C1 N1 C3 N2 1(2) . . . . ?
C2 N2 C3 N1 -2(3) . . . . ?
C3 N1 C1 C2 -1(2) . . . . ?
C3 N2 C2 C1 1(3) . . . . ?
