Two-dimensional organic–inorganic hybrid perovskite ferroelastics: (PEA)2[CdCl4], (3-FPEA)2[CdCl4], and (4-FPEA)2[CdCl4]
Yue, Zhi-Yuan; Luo, Wang; Wang, Na; Li, Hua-Kai; Xu, Ze-Jiang; Feng, Yan; Shi, Chao; Ye, Heng-Yun; Miao, Le-Ping; CrystEngComm 25 (2023) 1270–1275; doi:10.1039/D2CE01390H

data_7246223
_publ_section_title
;
 Two-dimensional organic--inorganic hybrid perovskite ferroelastics:
 (PEA)2[CdCl4], (3-FPEA)2[CdCl4], and (4-FPEA)2[CdCl4]
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1270
_journal_page_last               1275
_journal_paper_doi               10.1039/D2CE01390H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'Cd Cl4, 2(C8 H11 F N)'
_chemical_formula_sum            'C16 H22 Cd Cl4 F2 N2'
_chemical_formula_weight         534.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-09-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-12-15 deposited with the CCDC.	2023-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.274(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.0721(17)
_cell_length_b                   7.3523(6)
_cell_length_c                   7.4427(5)
_cell_measurement_reflns_used    6091
_cell_measurement_temperature    293.00(10)
_cell_measurement_theta_max      31.0210
_cell_measurement_theta_min      2.9690
_cell_volume                     1095.31(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.807
_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    -24.00  10.00   0.50    0.06    --    5.00  91.00 122.00   68
  2  \w     -9.00  36.00   0.50    0.06    --    5.00 -99.00 150.00   90
  3  \w    -33.00  -7.00   0.50    0.06    --    5.00 -91.00   8.00   52
  4  \w      1.00  28.00   0.50    0.06    --    5.00 -91.00   8.00   54
  5  \w    -17.00  33.00   0.50    0.06    --    5.00 -99.00-120.00  100
  6  \w    -17.00  28.00   0.50    0.06    --   -5.46 -99.00 -30.00   90
  7  \w    -78.00   1.00   0.50    0.06    --   -5.46 -37.00 120.00  158
;
_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      -0.0215743000
_diffrn_orient_matrix_UB_12      0.0358629000
_diffrn_orient_matrix_UB_13      -0.0711423000
_diffrn_orient_matrix_UB_21      0.0193226000
_diffrn_orient_matrix_UB_22      0.0807388000
_diffrn_orient_matrix_UB_23      0.0007889000
_diffrn_orient_matrix_UB_31      0.0203323000
_diffrn_orient_matrix_UB_32      -0.0387295000
_diffrn_orient_matrix_UB_33      -0.0640108000
_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  0.0711
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10742
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.034
_diffrn_reflns_theta_min         2.035
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.928
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         3498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0706P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2324
_reflns_number_total             3498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01390h5.cif
_cod_data_source_block           3_293k
_cod_depositor_comments
'Adding full bibliography for 7246220--7246225.cif.'
_cod_database_code               7246223
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'F Cd Cl C H N'
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.864
_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
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 N12(H12A,H12B,H12C)
;
_shelx_res_checksum              56004
_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 5.557
_oxdiff_exptl_absorpt_empirical_full_min 0.168