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_7710076
_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         'Cd Cl4, 2(C9 H14 N)'
_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                 94.0760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   35.8807(16)
_cell_length_b                   5.4904(2)
_cell_length_c                   5.4314(2)
_cell_measurement_reflns_used    3203
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      24.73
_cell_measurement_theta_min      2.23
_cell_volume                     1067.28(7)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -45
_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            7237
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.588
_diffrn_reflns_theta_min         3.851
_exptl_absorpt_coefficient_mu    1.528
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction,2019)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 1045 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2353
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0138
_refine_ls_R_factor_gt           0.0137
_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^)+(0.0141P)^2^+0.1620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0338
_refine_ls_wR_factor_ref         0.0338
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.951
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                2348
_reflns_number_total             2353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00592a2.cif
_cod_data_source_block           1_ltp
_cod_database_code               7710076
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.657
_olex2_refinement_description
;
1. 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
2.a Ternary CH refined with riding coordinates:
 C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C6(H6), C9(H9), C5(H5)
2.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'