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_7246221
_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         '2(C8 F N), 4(Cd0.25 Cl)'
_chemical_formula_sum            'C16 Cd Cl4 F2 N2'
_chemical_formula_weight         512.39
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_audit_creation_date             2022-12-15
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.3186(4)
_cell_length_b                   5.3186(4)
_cell_length_c                   40.261(8)
_cell_measurement_reflns_used    1482
_cell_measurement_temperature    403.02(10)
_cell_measurement_theta_max      28.0470
_cell_measurement_theta_min      3.0110
_cell_volume                     1138.9(3)
_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      403.02(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.845
_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    -21.00   5.22   0.38    0.06    --   -5.54  84.00  -6.00   69
  2  \w      1.76  39.00   0.38    0.06    --    5.07 -99.00 150.00   98
  3  \w    -14.00  27.04   0.38    0.06    --    5.07 -99.00  30.00  108
  4  \w     -6.00  20.22   0.38    0.06    --   -5.54 -99.00-180.00   69
;
_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      -0.1029036000
_diffrn_orient_matrix_UB_12      -0.0498230000
_diffrn_orient_matrix_UB_13      -0.0090601000
_diffrn_orient_matrix_UB_21      -0.0721352000
_diffrn_orient_matrix_UB_22      0.1079986000
_diffrn_orient_matrix_UB_23      0.0039485000
_diffrn_orient_matrix_UB_31      0.0443223000
_diffrn_orient_matrix_UB_32      0.0602427000
_diffrn_orient_matrix_UB_33      -0.0145916000
_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  0.0444
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            2465
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.718
_diffrn_reflns_theta_min         2.023
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.866
_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    1.494
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         614
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.359
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0964P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1353
_reflns_Friedel_coverage         0.000
_reflns_number_gt                460
_reflns_number_total             614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01390h5.cif
_cod_data_source_block           2_403k
_cod_depositor_comments
'Adding full bibliography for 7246220--7246225.cif.'
_cod_database_code               7246221
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cd Cl C H N F'
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.869
_olex2_refinement_description
;
1. Restrained distances
 C6-C7 = C7-C8 = C8-N1
 1.48 with sigma of 0.001
 N1-C7 = C8-C6
 2.3 with sigma of 0.001
 C7-C1 = C7-C5
 2.3 with sigma of 0.02
 N1-C6
 3.8 with sigma of 0.02
 C2-F1
 1.3 with sigma of 0.02
2. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, F1
 with sigma of 0.1
3. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002 within 2A
C4: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
Uanis(C7) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C8(0.125) C7(0.125) C1(0.125) C2(0.125) C3(0.125) C4(0.125)
 C5(0.125) C6(0.125) F1(0.125)
6.a Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6)
;
_shelx_res_checksum              48822
_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 3.956
_oxdiff_exptl_absorpt_empirical_full_min 0.453