Structural Phase Transition and Switchable Dielectric Behaviour of a One-Dimensional Chains Niobium Oxyfluoride
Feng, Yan; Wang, Ze-Jie; Li, Long-He; Liao, Rong-Meng; Hu, Zhao-Bo; Li, Jian-Rong; Shi, Chao; Ye, Heng-Yun; CrystEngComm  (2022) –; doi:10.1039/D2CE00428C

data_7244908
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w      3.00  29.00   0.50    0.05    --    8.30  94.00  82.00   52
  2  \w    -32.00  56.00   0.50    0.05    --   -8.69  77.00 -15.00  176
  3  \w    -13.00  13.00   0.50    0.05    --    8.30 -99.00 -60.00   52
  4  \w     -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       '\w 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/[\s^2^(Fo^2^)+(0.0484P)^2^+0.1846P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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 '
_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_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