Ferroelectric properties, narrow band gap and ultra-large reversible entropy change in a novel nonlinear ionic chromium(VI) compound.
Han, Ding-Chong; Gong, Zhi-Xiang; Song, Ning; Tan, Yu-Hui; Li, Yu-Kong; Tang, Yun-Zhi; Du, Peng-Kang; Zhang, Hao; Chemical communications (Cambridge, England) 57 (2021) 11225–11228; doi:10.1039/d1cc04751e

data_7129053
_publ_section_title
;
 Ferroelectric properties, narrow band gap and ultra-large reversible
 entropy change in a novel nonlinear ionic chromium(VI) compound.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11225
_journal_page_last               11228
_journal_paper_doi               10.1039/d1cc04751e
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'Cl Cr O3, 2(C3.5 H8.5 Cl0.5 N0.5)'
_chemical_formula_sum            'C7 H17 Cl2 Cr N O3'
_chemical_formula_weight         286.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-20 deposited with the CCDC.	2021-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.414(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8344(6)
_cell_length_b                   7.8851(3)
_cell_length_c                   14.4218(12)
_cell_measurement_reflns_used    5371
_cell_measurement_temperature    297.98(10)
_cell_measurement_theta_max      30.3970
_cell_measurement_theta_min      3.0680
_cell_volume                     1234.96(14)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.98(10)
_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 0.999
_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     -5.00  81.00   0.50    0.21    --    7.32  37.00  90.00  172
  2  \w    -21.00  41.00   0.50    0.21    --    7.32 -99.00   0.00  124
  3  \w    -21.00  26.00   0.50    0.21    --   -7.71 -99.00  90.00   94
  4  \w    -81.00   5.00   0.50    0.21    --   -7.71 -37.00-180.00  172
  5  \w    -66.00  20.00   0.50    0.21    --    7.32 -37.00 -90.00  172
;
_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      -0.0022160000
_diffrn_orient_matrix_UB_12      0.0898044000
_diffrn_orient_matrix_UB_13      -0.0032113000
_diffrn_orient_matrix_UB_21      -0.0522962000
_diffrn_orient_matrix_UB_22      -0.0051569000
_diffrn_orient_matrix_UB_23      -0.0473177000
_diffrn_orient_matrix_UB_31      -0.0401852000
_diffrn_orient_matrix_UB_32      0.0017697000
_diffrn_orient_matrix_UB_33      0.0249414000
_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  0.0161
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7197
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.495
_diffrn_reflns_theta_min         3.078
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90878
_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            'metallic orangish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2527
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.1816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                2346
_reflns_number_total             2527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04751e2.cif
_cod_data_source_block           1_c_89a_298k
_cod_depositor_comments          'Adding full bibliography for 7129053.cif.'
_cod_database_code               7129053
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.775
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(4)
 0.46(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 1*[Sof(Cl3)+Sof(C1)+Sof(H1a)+Sof(H1b)+Sof(H1c)+Sof(H3bc)+Sof(H3bd)+Sof(H4aa)+
 Sof(H4ab)]+1*[Sof(Cl3A)+Sof(C1A)+Sof(H1Aa)+Sof(H1Ab)+Sof(H1Ac)+Sof(H3aa)+
 Sof(H3ab)+Sof(H4bc)+Sof(H4bd)]=0.5 with esd of 0.0001
 1*[Sof(Cl2)+Sof(C2)+Sof(H2a)+Sof(H2b)+Sof(H2c)+Sof(H5aa)+Sof(H5ab)+Sof(H6aa)+
 Sof(H6ab)]+1*[Sof(Cl2A)+Sof(C2A)+Sof(H2Aa)+Sof(H2Ab)+Sof(H2Ac)+Sof(H5bc)+
 Sof(H5bd)+Sof(H6bc)+Sof(H6bd)]=0.5 with esd of 0.0001
 Sof(C1)=Sof(H1a)=Sof(H1b)=Sof(H1c)=Sof(H4aa)=Sof(H4ab)=1-FVAR(1)
 Sof(Cl3)=Sof(H3bc)=Sof(H3bd)=FVAR(1)
 Sof(C1A)=Sof(H1Aa)=Sof(H1Ab)=Sof(H1Ac)=Sof(H3aa)=Sof(H3ab)=1-FVAR(2)
 Sof(Cl3A)=Sof(H4bc)=Sof(H4bd)=FVAR(2)
 Sof(C2)=Sof(H2a)=Sof(H2b)=Sof(H2c)=Sof(H6aa)=Sof(H6ab)=1-FVAR(3)
 Sof(Cl2)=Sof(H5aa)=Sof(H5ab)=FVAR(3)
 Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=Sof(H2Ac)=Sof(H5bc)=Sof(H5bd)=1-FVAR(4)
 Sof(Cl2A)=Sof(H6bc)=Sof(H6bd)=FVAR(4)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5aa,H5ab), C5(H5bc,H5bd), C6(H6bc,H6bd), C6(H6aa,H6ab), C3(H3bc,H3bd),
 C3(H3aa,H3ab), C4(H4bc,H4bd), C4(H4aa,H4ab)
4.b Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C2A(H2Aa,H2Ab,H2Ac), C1(H1a,H1b,H1c), C1A(H1Aa,H1Ab,H1Ac)
;
_shelx_res_checksum              6653
_shelx_hkl_checksum              75603
_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 1.284
_oxdiff_exptl_absorpt_empirical_full_min 0.822