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_7707559
_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         '2(C5 H13 Cl N), 1(Cl4 O V)'
_chemical_formula_sum            'C10 H26 Cl6 N2 O V'
_chemical_formula_weight         453.97
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc26zv79
_audit_creation_date             2020-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-22 deposited with the CCDC.	2021-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8565(11)
_cell_length_b                   12.8565(11)
_cell_length_c                   12.8565(11)
_cell_measurement_reflns_used    71
_cell_measurement_temperature    363.00(10)
_cell_measurement_theta_max      34.1380
_cell_measurement_theta_min      5.9600
_cell_volume                     2125.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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      air
_diffrn_ambient_temperature      363.00(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 1.000
_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    -30.00  58.00   1.00    1.00    --  -31.88  77.00  60.00   88
  2  \w     60.00  92.00   1.00    3.47    --   95.69  77.00 -60.00   32
  3  \w    140.00 166.00   1.00    3.47    --   95.69  77.00 -60.00   26
  4  \w     55.00 146.00   1.00    3.47    --   95.69  77.00 120.00   91
;
_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      0.1032377000
_diffrn_orient_matrix_UB_12      -0.0263751000
_diffrn_orient_matrix_UB_13      0.0548109000
_diffrn_orient_matrix_UB_21      0.0445169000
_diffrn_orient_matrix_UB_22      -0.0409036000
_diffrn_orient_matrix_UB_23      -0.1034205000
_diffrn_orient_matrix_UB_31      0.0415915000
_diffrn_orient_matrix_UB_32      0.1095228000
_diffrn_orient_matrix_UB_33      -0.0253394000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            495
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        62.546
_diffrn_reflns_theta_max         62.546
_diffrn_reflns_theta_min         5.961
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (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    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.133
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         121
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      0.528
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0623
_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^)+(0.1920P)^2^+26.3574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.2389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                50
_reflns_number_total             121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01241j2.cif
_cod_data_source_block           exp_7385
_cod_depositor_comments
'Adding full bibliography for 7707559--7707561.cif.'
_cod_original_cell_volume        2125.0(5)
_cod_database_code               7707559
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.411
_shelx_estimated_absorpt_t_min   0.221
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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. Restrained distances
 C4-N1
 1.515 with sigma of 0.02
 C1-C2
 2.422 with sigma of 0.02
 C1-C4
 2.422 with sigma of 0.02
 C4-C2
 2.422 with sigma of 0.02
 C2-N1
 1.515 with sigma of 0.02
 C1-N1
 1.515 with sigma of 0.02
 N1-C4
 1.515 with sigma of 0.02
 V001-Cl1
 2.35 with sigma of 0.02
 V001-Cl4
 2.35 with sigma of 0.02
 Cl1-Cl4
 3.23 with sigma of 0.02
 C8-C4
 1.515 with sigma of 0.02
 N1-C8
 2.529 with sigma of 0.02
 V001-O1
 1.6 with sigma of 0.02
 Cl1-O1
 3.1 with sigma of 0.02
 Cl4-O1
 3.1 with sigma of 0.02
 Cl0A-C4
 2.671 with sigma of 0.02
 Cl0A-C8
 1.782 with sigma of 0.02
 C3-N1
 1.515 with sigma of 0.02
 C3-C4
 2.422 with sigma of 0.02
 C2-C3
 2.422 with sigma of 0.02
 C1-C3
 2.422 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim Cl1 \\sim V001 \\sim Cl4: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(V001)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(Cl0A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Fixed Sof: C1(0.04167) H1A(0.04167) H1B(0.04167) H1C(0.04167) Cl1(0.04167)
 Cl4(0.04167) O1(0.02083) C2(0.04167) H2A(0.04167) H2B(0.04167) H2C(0.04167)
 C3(0.04167) H3A(0.04167) H3B(0.04167) H3C(0.04167) C4(0.04167) H4A(0.04167)
 H4B(0.04167) C8(0.04167) H8A(0.04167) H8B(0.04167) V001(0.02083) N1(0.04167)
 Cl0A(0.04167)
5.a Riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B), C8(H8A,H8B)
;
_shelx_res_checksum              92052
_shelx_hkl_checksum              44945
_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 13.029
_oxdiff_exptl_absorpt_empirical_full_min 0.507