Unusual symmetry breaking in high-temperature enantiomeric ferroelectrics with large spontaneous polarization
Li, Yu-Kong; Ying, Ting-Ting; Zhang, Hao; Tan, Yu-Hui; Tang, Yun-Zhi; Wang, Fang-Xin; Wan, Ming-Yang; Dalton Transactions  (2022) –; doi:10.1039/D2DT00592A

data_7710077
_publ_section_title
;
 Unusual symmetry breaking in high-temperature enantiomeric ferroelectrics
 with large spontaneous polarization
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00592A
_journal_year                    2022
_chemical_absolute_configuration ad.
_chemical_formula_moiety         '2(C9 H14 N), Cd Cl4'
_chemical_formula_sum            'C18 H28 Cd Cl4 N2'
_chemical_formula_weight         526.62
_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
_audit_creation_date             2022-03-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-19 deposited with the CCDC.	2022-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.000(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   35.9424(11)
_cell_length_b                   5.5098(2)
_cell_length_c                   5.4475(2)
_cell_measurement_reflns_used    7921
_cell_measurement_temperature    298.98(12)
_cell_measurement_theta_max      30.5130
_cell_measurement_theta_min      2.2600
_cell_volume                     1076.17(6)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.98(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_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    -82.00 -12.00   0.50    0.05    --   -8.69 -48.00-107.00  140
  2  \w    -15.00  61.00   0.50    0.05    --   -8.69  48.00  40.00  152
  3  \w    -18.00  25.00   0.50    0.05    --    8.30 -99.00-120.00   86
  4  \w    -56.00 -13.00   0.50    0.05    --    8.30 -37.00 150.00   86
  5  \w    -64.00  31.00   0.50    0.05    --    8.30 -77.00 -30.00  190
  6  \w     -8.00  40.00   0.50    0.05    --    8.30 -99.00-180.00   96
  7  \w    -83.00  -6.00   0.50    0.05    --   -8.69 -37.00 150.00  154
;
_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      0.0752844000
_diffrn_orient_matrix_UB_12      0.0636653000
_diffrn_orient_matrix_UB_13      -0.0120290000
_diffrn_orient_matrix_UB_21      0.1065689000
_diffrn_orient_matrix_UB_22      -0.0422321000
_diffrn_orient_matrix_UB_23      0.0105101000
_diffrn_orient_matrix_UB_31      0.0028198000
_diffrn_orient_matrix_UB_32      -0.1036172000
_diffrn_orient_matrix_UB_33      -0.0116746000
_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  0.0257
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8132
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.967
_diffrn_reflns_theta_min         2.272
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86695
_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 whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2580
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0224
_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^)+(0.0327P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0540
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                2566
_reflns_number_total             2580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00592a2.cif
_cod_data_source_block           2_LTP
_cod_database_code               7710077
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.805
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.98(3)
 0.02(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C00B(H00G)
3.b Secondary CH2 refined with riding coordinates:
 C00J(H00J,H00K)
3.c Aromatic/amide H refined with riding coordinates:
 C00D(H00H), C00E(H00I), C00K(H00L), C00N(H00N), C00P(H00P)
3.d Idealised Me refined as rotating group:
 N006(H00A,H00B,H00C), C009(H00D,H00E,H00F)
;
_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 1.253
_oxdiff_exptl_absorpt_empirical_full_min 0.860