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_7707560
_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           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-20
_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                 95.9650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.75140(10)
_cell_length_b                   9.04080(10)
_cell_length_c                   12.5409(2)
_cell_measurement_reflns_used    8654
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      75.4700
_cell_measurement_theta_min      3.5450
_cell_volume                     986.86(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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    -55.00 -11.00   1.00    1.00    --  -41.00 -57.00-120.00   44
  2  \w    -83.00 -13.00   1.00    1.00    --  -41.00 125.00  90.00   70
  3  \w    -38.00  -7.00   1.00    1.00    --  -41.00 -77.00 -60.00   31
  4  \w    -43.00  -7.00   1.00    1.00    --  -41.00 -77.00-180.00   36
  5  \w   -119.00 -23.00   1.00    1.00    --  -41.00 -77.00 150.00   96
  6  \w    -69.00  25.00   1.00    1.00    --  -41.00  57.00 -90.00   94
  7  \w   -118.00 -65.00   1.00    1.00    --  -41.00 -77.00   0.00   53
  8  \w    -47.00 -19.00   1.00    1.00    --  -41.00 -77.00   0.00   28
  9  \w   -115.00 -89.00   1.00    1.00    --  -41.00 -57.00-120.00   26
 10  \w   -117.00 -74.00   1.00    1.00    --  -41.00 -77.00 -60.00   43
 11  \w   -119.00  -8.00   1.00    1.00    --  -41.00 -77.00  60.00  111
 12  \w     15.00  42.00   1.00    1.00    --   41.00  57.00 -60.00   27
 13  \w     53.00  83.00   1.00    1.00    --   41.00 -99.00 -90.00   30
 14  \w    -29.00  67.00   1.00    1.00    --   41.00 -57.00   0.00   96
 15  \w     57.00  82.00   1.00    1.00    --   41.00  57.00 -60.00   25
 16  \w     81.00 108.00   1.00    3.00    --  111.51  61.00 120.00   27
 17  \w     81.00 140.00   1.00    3.00    --  111.51  61.00-150.00   59
 18  \w     81.00 120.00   1.00    3.00    --  111.51  61.00 -60.00   39
 19  \w     81.00 117.00   1.00    3.00    --  111.51  61.00  30.00   36
 20  \w     81.00 106.00   1.00    3.00    --  111.51  61.00 -90.00   25
 21  \w     38.00 116.00   1.00    3.00    --  111.51-125.00  30.00   78
 22  \w    139.00 177.00   1.00    3.00    --  111.51  61.00-107.31   38
 23  \w     78.00 165.00   1.00    3.00    --  111.51  77.00 150.00   87
 24  \w     82.00 178.00   1.00    3.00    --  111.51  61.00   0.00   96
 25  \w    148.00 174.00   1.00    3.00    --  111.51  61.00 -90.00   26
 26  \w     78.00 133.00   1.00    3.00    --  111.51  77.00  30.00   55
 27  \w     79.00 105.00   1.00    3.00    --  111.51  77.00-180.00   26
 28  \w     81.00 108.00   1.00    3.00    --  111.51  61.00 -30.00   27
 29  \w     27.00  92.00   1.00    3.00    --  111.51 -94.00 -90.00   65
 30  \w     78.00 111.00   1.00    3.00    --  111.51  77.00 -90.00   33
 31  \w     78.00 103.00   1.00    3.00    --  111.51  77.00  60.00   25
 32  \w     78.00 170.00   1.00    3.00    --  111.51  77.00-150.00   92
 33  \w     87.00 113.00   1.00    3.00    --  111.51  45.00   0.00   26
 34  \w     81.00 107.00   1.00    3.00    --  111.51  61.00 150.00   26
 35  \w     33.00 139.00   1.00    3.00    --  111.51 -77.00  30.00  106
 36  \w     79.00 104.00   1.00    3.00    --  111.51  77.00   0.00   25
 37  \w     78.00 175.00   1.00    3.00    --  111.51  77.00 -60.00   97
 38  \w     81.00 127.00   1.00    3.00    --  111.51  61.00  90.00   46
 39  \w    115.00 177.00   1.00    3.00    --  111.51  77.00  90.00   62
 40  \w     81.00 176.00   1.00    3.00    --  111.51  61.00  60.00   95
 41  \w     82.00 108.00   1.00    3.00    --  111.51  61.00-180.00   26
 42  \w     81.00 176.00   1.00    3.00    --  111.51  61.00-120.00   95
 43  \w     78.00 103.00   1.00    3.00    --  111.51  77.00  90.00   25
 44  \w     37.00 118.00   1.00    3.00    --  111.51-125.00-120.00   81
 45  \w     81.00 106.00   1.00    3.00    --  111.51  61.00-107.31   25
 46  \w     84.00 144.00   1.00    3.00    --  111.51  47.00 150.29   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1448732000
_diffrn_orient_matrix_UB_12      -0.0297987000
_diffrn_orient_matrix_UB_13      -0.0777847000
_diffrn_orient_matrix_UB_21      -0.0440882000
_diffrn_orient_matrix_UB_22      -0.1278636000
_diffrn_orient_matrix_UB_23      0.0720529000
_diffrn_orient_matrix_UB_31      -0.0917074000
_diffrn_orient_matrix_UB_32      0.1085760000
_diffrn_orient_matrix_UB_33      0.0633488000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_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            13844
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.615
_diffrn_reflns_theta_min         3.544
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.654
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.271(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         4026
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0691P)^2^+0.6454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3863
_reflns_number_total             4026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01241j2.cif
_cod_data_source_block           exp_11054
_cod_depositor_comments
'Adding full bibliography for 7707559--7707561.cif.'
_cod_database_code               7707560
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C10 N2 Cl6 V O'
_shelx_estimated_absorpt_t_max   0.204
_shelx_estimated_absorpt_t_min   0.128
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.729(13)
 0.271(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C6(H6a,H6b), C9(H9a,H9b), C00K(H00a,H00b)
3.b Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C7(H7a,
 H7b,H7c), C8(H8a,H8b,H8c)
;
_shelx_res_checksum              27349
_shelx_hkl_checksum              55578
_olex2_date_sample_data_collection 2020-06-07
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.448
_oxdiff_exptl_absorpt_empirical_full_min 0.733