A polar oxyhalogen-vanadate compound (C<sub>5</sub>NH<sub>13</sub>Cl)<sub>2</sub>VOCl<sub>4</sub> with optical and two-staged dielectric switch behavior.
Kong, Qing-Rong; Wang, Bin; Liu, Xiao-Lin; Zhao, Hai-Xia; Long, La-Sheng; Zheng, Lan-Sun; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9293–9297; doi:10.1039/d1dt01241j

data_7707561
_publ_section_title
;
 A polar oxyhalogen-vanadate compound
 (C<sub>5</sub>NH<sub>13</sub>Cl)<sub>2</sub>VOCl<sub>4</sub> with optical
 and two-staged dielectric switch behavior.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9293
_journal_page_last               9297
_journal_paper_doi               10.1039/d1dt01241j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'Cl4 O V, 2(C5 H13 Cl N)'
_chemical_formula_sum            'C10 H26 Cl6 N2 O V'
_chemical_formula_weight         453.97
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-12 deposited with the CCDC.	2021-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.135(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7533(4)
_cell_length_b                   9.0953(4)
_cell_length_c                   12.7626(6)
_cell_measurement_reflns_used    4871
_cell_measurement_temperature    300.00(11)
_cell_measurement_theta_max      73.7250
_cell_measurement_theta_min      4.8390
_cell_volume                     1012.00(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_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     25.00  72.00   0.50    0.31    --   43.22-105.00 -78.00   94
  2  \w     36.00  62.00   0.50    0.31    --   43.22 -99.00   0.00   52
  3  \w     65.00 110.00   0.50    1.24    --  107.45-105.00 -78.00   90
  4  \w     55.00  81.00   0.50    1.24    --  107.45 -94.00  30.00   52
  5  \w     33.00  62.00   0.50    1.24    --  107.45-105.00 -78.00   58
  6  \w     33.00 100.00   0.50    1.24    --  107.45 -94.00 120.00  134
  7  \w     91.00 116.00   0.50    1.24    --  107.45-125.00 120.00   50
  8  \w     33.00  85.00   0.50    1.24    --  107.45-125.00 120.00  104
  9  \w     89.00 123.00   0.50    1.24    --  107.45  77.00  90.00   68
 10  \w    138.00 178.00   0.50    1.24    --  107.45  77.00  90.00   80
 11  \w    149.00 178.00   0.50    1.24    --  107.45 125.00 120.00   58
 12  \w    106.00 132.00   0.50    1.24    --  107.45 105.00  22.00   52
 13  \w     93.00 174.00   0.50    1.24    --  107.45 125.00 -30.00  162
 14  \w    107.00 133.00   0.50    1.24    --  107.45 125.00 120.00   52
 15  \w    -63.00 -31.00   0.50    1.24    --  -90.25 105.00  22.00   64
 16  \w    -85.00 -22.00   0.50    0.31    --  -43.22 105.00  22.00  126
 17  \w   -108.00 -74.00   0.50    0.31    --  -43.22-125.00 -60.00   68
 18  \w   -116.00 -73.00   0.50    0.31    --  -43.22-125.00-120.00   86
 19  \w   -122.00 -81.00   0.50    1.24    --  -90.25-105.00 -78.00   82
 20  \w   -115.00 -70.00   0.50    0.31    --  -43.22-125.00   0.00   90
 21  \w   -113.00 -74.00   0.50    0.31    --  -43.22-125.00  60.00   78
 22  \w   -115.00 -74.00   0.50    0.31    --  -43.22-125.00  90.00   82
 23  \w   -134.00 -94.00   0.50    1.24    --  -90.25 -94.00  30.00   80
 24  \w   -159.00 -72.00   0.50    1.24    --  -90.25 -45.00 120.00  174
 25  \w    -18.00   8.00   0.50    0.30    --  -43.22 103.00  25.00   52
 26  \w   -118.00 -67.00   0.50    0.30    --  -43.22 -57.00-180.00  102
 27  \w    -62.00 -20.00   0.50    0.30    --  -43.22 -57.00-180.00   84
 28  \w     38.00  84.00   0.50    0.30    --   43.22-125.00-120.00   92
 29  \w      4.00  31.00   0.50    0.30    --   43.22 -99.00 -90.00   54
 30  \w    -87.00 -52.00   0.50    0.20    --  -90.25 125.00  30.00   70
 31  \w    -43.00 -17.00   0.50    0.20    --  -90.25 125.00  90.00   52
 32  \w    -46.00 -16.00   0.50    0.20    --  -90.25 125.00  30.00   60
 33  \w   -113.00 -23.00   0.50    0.20    --  -90.25  45.00  60.00  180
 34  \w     35.00  79.00   0.50    0.20    --  107.45-125.00 -90.00   88
 35  \w    146.00 176.00   0.50    0.20    --  107.45  45.00 150.00   60
 36  \w     94.00 136.00   0.50    0.20    --  107.45 -77.00 150.00   84
 37  \w    103.00 128.00   0.50    0.20    --  107.45  45.00 150.00   50
 38  \w    131.00 178.00   0.50    0.20    --  107.45  61.00  60.00   94
 39  \w     83.00 112.00   0.50    0.20    --  107.45-125.00 -90.00   58
 40  \w     92.00 117.00   0.50    0.20    --  107.45-125.00  60.00   50
 41  \w     35.00  61.00   0.50    0.20    --  107.45-125.00  60.00   52
 42  \w     36.00  90.00   0.50    0.20    --  107.45-125.00-180.00  108
 43  \w     54.00  79.00   0.50    0.20    --  107.45 -94.00 -60.00   50
 44  \w     93.00 119.00   0.50    0.20    --  107.45  61.00  60.00   52
 45  \w     38.00  65.00   0.50    0.20    --  107.45 -77.00 150.00   54
 46  \w    116.00 141.00   0.50    0.20    --  107.45 103.00  25.00   50
 47  \w    -62.00 -37.00   0.50    0.30    --  -43.22 103.00  25.00   50
 48  \w     46.00  71.00   0.50    0.20    --  107.45-103.00 -77.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0396035000
_diffrn_orient_matrix_UB_12      0.1461190000
_diffrn_orient_matrix_UB_13      0.0573178000
_diffrn_orient_matrix_UB_21      -0.0345788000
_diffrn_orient_matrix_UB_22      -0.0705459000
_diffrn_orient_matrix_UB_23      0.1050683000
_diffrn_orient_matrix_UB_31      0.1685923000
_diffrn_orient_matrix_UB_32      -0.0486255000
_diffrn_orient_matrix_UB_33      0.0195583000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10601
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.061
_diffrn_reflns_theta_min         5.892
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.365
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0758
_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/[\s^2^(Fo^2^)+(0.1063P)^2^+1.3623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1635
_reflns_number_total             2013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01241j2.cif
_cod_data_source_block           exp_8741
_cod_depositor_comments
'Adding full bibliography for 7707559--7707561.cif.'
_cod_database_code               7707561
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.342
_shelx_estimated_absorpt_t_min   0.210
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Cl4)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=1-FVAR(1)
 Sof(Cl3)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=FVAR(1)
 Fixed Sof: O1(0.5) V1(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              15328
_shelx_hkl_checksum              59189
_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 3.337
_oxdiff_exptl_absorpt_empirical_full_min 0.628