#------------------------------------------------------------------------------
#$Date: 2022-05-11 01:30:47 +0300 (Wed, 11 May 2022) $
#$Revision: 275307 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/49/7244908.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_7244908
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      orthorhombic
_space_group_IT_number           51
_space_group_name_Hall           '-P 2a 2a'
_space_group_name_H-M_alt        'P m m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-12-10
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5290(10)
_cell_length_b                   6.8257(5)
_cell_length_c                   3.9372(2)
_cell_measurement_reflns_used    1252
_cell_measurement_temperature    305.38(10)
_cell_measurement_theta_max      27.4410
_cell_measurement_theta_min      2.9940
_cell_volume                     363.58(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_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_environment      air
_diffrn_ambient_temperature      305.38(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      3.00  29.00   0.50    0.05    --    8.30  94.00  82.00   52
  2  ω    -32.00  56.00   0.50    0.05    --   -8.69  77.00 -15.00  176
  3  ω    -13.00  13.00   0.50    0.05    --    8.30 -99.00 -60.00   52
  4  ω     -8.00  42.00   0.50    0.05    --    8.30 -99.00-180.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0858646000
_diffrn_orient_matrix_UB_12      0.0313775000
_diffrn_orient_matrix_UB_13      0.0280810000
_diffrn_orient_matrix_UB_21      -0.0437668000
_diffrn_orient_matrix_UB_22      -0.1481862000
_diffrn_orient_matrix_UB_23      -0.0200339000
_diffrn_orient_matrix_UB_31      0.0388407000
_diffrn_orient_matrix_UB_32      -0.0975940000
_diffrn_orient_matrix_UB_33      0.0394732000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2316
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.323
_diffrn_reflns_theta_min         2.984
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.675
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    2.320
_exptl_crystal_description       irregular
_exptl_crystal_F_000             244
_refine_diff_density_max         1.769
_refine_diff_density_min         -1.250
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         562
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0484P)²+0.1846P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                506
_reflns_number_total             562
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00428c3.cif
_cod_data_source_block           x
_cod_database_code               7244908
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C N H O F Nb '
_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.
;
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_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 0.02
 N1-C1 \\sim N2-C2 \\sim N1-C3 \\sim N2-C3
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C3 \\sim C2 \\sim C1: within 3.8A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 3.8A
4. Others
 Fixed Sof: N1(0.25) H1(0.25) C3(0.25) H3(0.25) N2(0.25) H2(0.25) C2(0.25)
 H2a(0.25) C1(0.25) H1a(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), N2(H2), C2(H2a), C1(H1a)
;
_shelx_res_file
;
TITL fy210622_6_rt_a.res in Pmma
    x.res
    created by SHELXL-2018/1 at 15:35:56 on 20-Jul-2021
REM Old TITL fy210622_6_rt_a.res in Pmma
REM SHELXT solution in Pmma
REM R1 0.101, Rweak 0.009, Alpha 0.021, Orientation as input
REM Formula found by SHELXT: C6 O F4 Nb
REM eqiv $1 x, -y, z
rem sadi 0.02 C1 C2 N1 n1_$1
CELL 0.71073 13.529 6.8257 3.9372 90 90 90
ZERR 2 0.001 0.0005 0.0002 0 0 0
LATT 1
SYMM 0.5-X,-Y,+Z
SYMM -X,+Y,-Z
SYMM 0.5+X,-Y,-Z
SFAC C H N O F Nb
UNIT 6 10 4 2 8 2
EQIV $1 1.5-X,-Y,+Z
EQIV $2 -0.5+X,+Y,-Z
EQIV $3 1-X,1-Y,-Z
EQIV $4 1-X,-Y,-Z
EQIV $5 +X,-1+Y,-1+Z
SIMU 0.02 0.04 3.8 $n $c
DFIX 1.39 C1 C2
SADI 0.01 N1 C1 N2 C2 N1 C3 N2 C3

L.S. 74
PLAN  1
TEMP 27
CONF
HTAB N1 F1
HTAB N1 F1_$1
HTAB C3 F2
HTAB N2 F1_$2
HTAB N2 F2_$3
HTAB C2 F1_$4
HTAB C1 F2_$5
HTAB
BOND $H
list 4
fmap 2 53
acta
MORE -1
REM <olex2.extras>
REM <HklSrc "%.\\x.hkl">
REM </olex2.extras>

WGHT    0.048400    0.184600
FVAR       0.99357
NB1   6    0.750000    0.500000    0.558890    10.25000    0.04272    0.04821 =
         0.02453    0.00000    0.00000    0.00000
F1    5    0.750000    0.224153    0.487612    10.50000    0.09569    0.04940 =
         0.09018    0.00176    0.00000    0.00000
F2    5    0.610943    0.500000    0.492126    10.50000    0.04327    0.10997 =
         0.11120    0.00000   -0.00073    0.00000
O1    4    0.750000    0.500000    0.000733    10.25000    0.11564    0.10528 =
         0.02987    0.00000    0.00000    0.00000
PART -1
N1    3    0.569851   -0.031362    0.142982    10.25000    0.05046    0.05738 =
         0.05575    0.00209   -0.00903    0.01844
AFIX  43
H1    2    0.623172   -0.056779    0.253432    10.25000   -1.20000
AFIX   0
C3    1    0.526081    0.142365    0.110811    10.25000    0.04650    0.05811 =
         0.05115    0.00321   -0.02028   -0.00212
AFIX  43
H3    2    0.550825    0.258390    0.200841    10.25000   -1.20000
AFIX   0
N2    3    0.442839    0.129419   -0.065507    10.25000    0.04352    0.05681 =
         0.06734    0.00656   -0.00837    0.01094
AFIX  43
H2    2    0.408761    0.221978   -0.156340    10.25000   -1.20000
AFIX   0
C2    1    0.425151   -0.061940   -0.067026    10.25000    0.05065    0.05285 =
         0.06868    0.01054   -0.00636   -0.00350
AFIX  43
H2A   2    0.363559   -0.121089   -0.089090    10.25000   -1.20000
AFIX   0
C1    1    0.514529   -0.157553   -0.029997    10.25000    0.05023    0.05488 =
         0.06970    0.00108   -0.00306    0.01061
AFIX  43
H1A   2    0.531927   -0.281447   -0.108013    10.25000   -1.20000
AFIX   0
HKLF 4




REM  fy210622_6_rt_a.res in Pmma
REM R1 =  0.0374 for     506 Fo > 4sig(Fo)  and  0.0429 for all     562 data
REM     66 parameters refined using     67 restraints

END

WGHT      0.0494      0.1930

REM Instructions for potential hydrogen bonds
HTAB N1 F1_$1
HTAB C3 F2
HTAB N2 F1_$2
HTAB N2 F2_$3
HTAB C2 F1_$4
HTAB C1 F2_$5

REM Highest difference peak  1.769,  deepest hole -1.250,  1-sigma level  0.117
Q1    1   0.7500  0.5000  0.3971  10.25000  0.05    1.77
;
_shelx_res_checksum              41856
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.142
_oxdiff_exptl_absorpt_empirical_full_min 0.872
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z'
'-x-1/2, y, z'
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 0.750000 0.500000 0.55889(14) 0.0385(3) Uani 1 4 d S T P . .
F1 F 0.750000 0.2242(7) 0.4876(12) 0.0784(12) Uani 1 2 d S T P . .
F2 F 0.6109(4) 0.500000 0.4921(13) 0.0881(14) Uani 1 2 d S T P . .
O1 O 0.750000 0.500000 0.0007(17) 0.084(3) Uani 1 4 d S T P . .
N1 N 0.570(2) -0.031(4) 0.143(7) 0.055(5) Uani 0.25 1 d D U P A -1
H1 H 0.623172 -0.056779 0.253432 0.065 Uiso 0.25 1 calc R U P A -1
C3 C 0.526(2) 0.142(4) 0.111(9) 0.052(5) Uani 0.25 1 d D U P A -1
H3 H 0.550825 0.258390 0.200841 0.062 Uiso 0.25 1 calc R U P A -1
N2 N 0.4428(16) 0.129(4) -0.066(10) 0.056(5) Uani 0.25 1 d D U P A -1
H2 H 0.408761 0.221978 -0.156340 0.067 Uiso 0.25 1 calc R U P A -1
C2 C 0.425(3) -0.062(4) -0.067(11) 0.057(6) Uani 0.25 1 d D U P A -1
H2A H 0.363559 -0.121089 -0.089090 0.069 Uiso 0.25 1 calc R U P A -1
C1 C 0.515(2) -0.158(3) -0.030(10) 0.058(6) Uani 0.25 1 d D U P A -1
H1A H 0.531927 -0.281447 -0.108013 0.070 Uiso 0.25 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 0.0427(4) 0.0482(4) 0.0245(4) 0.000 0.000 0.000
F1 0.096(4) 0.049(2) 0.090(3) 0.002(2) 0.000 0.000
F2 0.043(2) 0.110(4) 0.111(3) 0.000 -0.001(2) 0.000
O1 0.116(7) 0.105(7) 0.030(3) 0.000 0.000 0.000
N1 0.050(7) 0.057(12) 0.056(10) 0.002(9) -0.009(7) 0.018(11)
C3 0.047(12) 0.058(9) 0.051(10) 0.003(8) -0.020(10) -0.002(11)
N2 0.044(10) 0.057(10) 0.067(10) 0.007(9) -0.008(10) 0.011(10)
C2 0.051(9) 0.053(11) 0.069(12) 0.011(9) -0.006(9) -0.003(10)
C1 0.050(12) 0.055(7) 0.070(13) 0.001(9) -0.003(11) 0.011(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'
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'
Nb Nb -2.0727 0.6215 '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 163.0(3) . 2_665 ?
F1 Nb1 O1 81.52(14) . . ?
F1 Nb1 O1 81.52(14) 2_665 . ?
F2 Nb1 F1 88.83(3) 2_665 2_665 ?
F2 Nb1 F1 88.83(3) . . ?
F2 Nb1 F1 88.83(3) 2_665 . ?
F2 Nb1 F1 88.83(3) . 2_665 ?
F2 Nb1 F2 164.1(3) 2_665 . ?
F2 Nb1 O1 82.05(15) 2_665 . ?
F2 Nb1 O1 82.05(15) . . ?
O1 Nb1 F1 98.48(14) 1_556 . ?
O1 Nb1 F1 98.48(14) 1_556 2_665 ?
O1 Nb1 F2 97.95(15) 1_556 . ?
O1 Nb1 F2 97.95(15) 1_556 2_665 ?
O1 Nb1 O1 180.0 1_556 . ?
Nb1 O1 Nb1 180.0 1_554 . ?
C3 N1 H1 126.9 . . ?
C1 N1 H1 126.9 . . ?
C1 N1 C3 106(2) . . ?
N1 C3 H3 124.2 . . ?
N2 C3 N1 112(3) . . ?
N2 C3 H3 124.2 . . ?
C3 N2 H2 128.6 . . ?
C3 N2 C2 103(4) . . ?
C2 N2 H2 128.6 . . ?
N2 C2 H2A 126.1 . . ?
N2 C2 C1 108(3) . . ?
C1 C2 H2A 126.1 . . ?
N1 C1 C2 103.9(19) . . ?
N1 C1 H1A 128.0 . . ?
C2 C1 H1A 128.0 . . ?
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 1.904(5) 2_665 ?
Nb1 F1 1.904(5) . ?
Nb1 F2 1.900(5) . ?
Nb1 F2 1.900(5) 2_665 ?
Nb1 O1 2.198(7) . ?
Nb1 O1 1.740(7) 1_556 ?
N1 H1 0.8600 . ?
N1 C3 1.331(13) . ?
N1 C1 1.329(13) . ?
C3 H3 0.9300 . ?
C3 N2 1.326(13) . ?
N2 H2 0.8600 . ?
N2 C2 1.328(13) . ?
C2 H2A 0.9300 . ?
C2 C1 1.38(2) . ?
C1 H1A 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 2.73 3.29(3) 123.8 . yes
N1 H1 F1 0.86 2.26 3.08(2) 161.0 2_655 yes
C3 H3 F2 0.93 2.17 3.09(3) 170.0 . yes
N2 H2 F1 0.86 2.51 3.16(3) 132.7 6 yes
N2 H2 F2 0.86 2.33 3.12(3) 153.7 5_665 yes
C2 H2A F1 0.93 2.31 3.10(4) 142.5 5_655 yes
C1 H1A F2 0.93 2.42 3.27(2) 152.6 1_544 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
N1 C3 N2 C2 15(4) . . . . ?
C3 N1 C1 C2 -18(5) . . . . ?
C3 N2 C2 C1 -26(4) . . . . ?
N2 C2 C1 N1 28(5) . . . . ?
C1 N1 C3 N2 2(4) . . . . ?
