High phase transition temperature and photoluminescence properties in low-dimensional molecular perovskite ferroelastic crystals
Zhang, Jia-Mei; Xu, Zhe-Kun; Qin, Yan; Li, Peng-Fei; Wang, Zhong-Xia; CrystEngComm 27 (2025) 1534–1540; doi:10.1039/D5CE00012B

data_7249939
_publ_section_title
;
 High phase transition temperature and photoluminescence properties in
 low-dimensional molecular perovskite ferroelastic crystals
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              1534
_journal_page_last               1540
_journal_paper_doi               10.1039/D5CE00012B
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'Cd4 Cl12, 4(C5 H10 N)'
_chemical_formula_sum            'C20 H40 Cd4 Cl12 N4'
_chemical_formula_weight         1211.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-01-31 deposited with the CCDC.	2025-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.6713(11)
_cell_length_b                   6.7314(3)
_cell_length_c                   18.1716(10)
_cell_measurement_reflns_used    3358
_cell_measurement_temperature    403.02(10)
_cell_measurement_theta_max      69.2190
_cell_measurement_theta_min      4.8480
_cell_volume                     2161.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.129a 64-bit (release 29-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (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-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_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    -93.00 -34.00   0.50    0.06    --  -75.50 125.00  60.00  118
  2  \w   -103.00 -74.00   0.50    0.06    --  -60.72 -30.00   0.00   58
  3  \w   -115.00 -88.00   0.50    0.06    --  -74.13-125.00 120.00   54
  4  \w   -113.00 -80.00   0.50    0.06    --  -75.50-125.00  90.00   66
  5  \w   -118.00 -76.00   0.50    0.06    --  -74.13-125.00-120.00   84
  6  \w   -117.00 -75.00   0.50    0.06    --  -74.13 -30.00-180.00   84
  7  \w   -122.00 -84.00   0.50    0.06    --  -74.13 -30.00 -30.00   76
  8  \w    -98.00 -72.00   0.50    0.06    --  -60.72 -30.00 -60.00   52
  9  \w     11.00  36.00   0.50    0.06    --   60.54 -30.00-150.00   50
 10  \w     11.00  36.00   0.50    0.06    --   60.54 -30.00 -90.00   50
 11  \w     78.00 122.00   0.50    0.06    --   75.18  30.00 -60.00   88
 12  \w     80.00 116.00   0.50    0.06    --   75.18  30.00 -30.00   72
 13  \w     63.00 110.00   0.50    0.06    --   60.54  30.00  30.00   94
 14  \w     75.00 104.00   0.50    0.06    --   60.54  15.00 150.00   58
 15  \w     30.00  60.00   0.50    0.06    --   60.54  15.00 150.00   60
 16  \w     11.00  37.00   0.50    0.06    --   60.54 -30.00 150.00   52
 17  \w     69.00  95.00   0.50    0.06    --   60.54   0.00 -30.00   52
 18  \w     21.00  47.00   0.50    0.06    --   60.54   0.00 -30.00   52
 19  \w     44.00  83.00   0.50    0.06    --   75.18 -94.00  30.00   78
 20  \w     38.00  85.00   0.50    0.06    --   75.18 -94.00 -30.00   94
 21  \w     21.00  63.00   0.50    0.06    --   60.54 -94.00  30.00   84
 22  \w     38.00  80.00   0.50    0.06    --   75.18 -94.00  60.00   84
 23  \w     32.00  61.00   0.50    0.06    --   60.54 -94.00  90.00   58
 24  \w     37.00  75.00   0.50    0.06    --   75.12 -94.00 150.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1116849000
_diffrn_orient_matrix_UB_12      -0.0398486000
_diffrn_orient_matrix_UB_13      0.0642075000
_diffrn_orient_matrix_UB_21      -0.1958046000
_diffrn_orient_matrix_UB_22      -0.0075618000
_diffrn_orient_matrix_UB_23      0.0443264000
_diffrn_orient_matrix_UB_31      -0.0389257000
_diffrn_orient_matrix_UB_32      -0.0744546000
_diffrn_orient_matrix_UB_33      -0.0389714000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1187
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14430
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.491
_diffrn_reflns_theta_min         3.489
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.129a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pinkish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.976
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         2292
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0836
_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^)+(0.1515P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2809
_refine_ls_wR_factor_ref         0.3203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1163
_reflns_number_total             2292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00012b2.cif
_cod_data_source_block           gjq-231024-1-403k_r
_cod_depositor_comments
'Adding full bibliography for 7249938--7249941.cif.'
_cod_database_code               7249939
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N Cd Cl'
_shelx_estimated_absorpt_t_max   0.212
_shelx_estimated_absorpt_t_min   0.212
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C1 = N1-C2 = N1-C3
 1.43 with sigma of 0.02
 C5-C4
 1.43 with sigma of 0.02
 C1-C2 = C2-C3 = C1-C3
 2.3 with sigma of 0.02
 C4-C3
 1.53 with sigma of 0.02
 C5-C3
 2.5 with sigma of 0.02
 C8-C10
 2.4 with sigma of 0.02
 N2-C8 = N2-C7 = N2-C6
 1.43 with sigma of 0.02
 C9-C8
 1.53 with sigma of 0.02
 C6-C7 = C6-C8 = C7-C8
 2.3 with sigma of 0.02
 C4-C5
 1.2 with sigma of 0.03
 N1-Cl3
 3.35 with sigma of 0.02
 C9-C10 = C4-C5
 1 with sigma of 0.02
 C9-C10
 1.1 with sigma of 0.02
 C10-C8
 2.63 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1 \\sim C3 \\sim C4 \\sim C2 \\sim C1 \\sim C5: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
N2 \\sim C8 \\sim C6 \\sim C7 \\sim C9 \\sim C10: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
Uanis(N2) = Uanis(C8) = Uanis(C6) = Uanis(C7) = Uanis(C9) = Uanis(C10) =
Uanis(N1) = Uanis(C3) = Uanis(C4) = Uanis(C2) = Uanis(C1) = Uanis(C5)
4. Others
 Fixed Sof: N2(0.5) H2(0.5) C8(0.5) H8A(0.5) H8B(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) N1(0.5) H1(0.5) C5(0.5) H5(0.5) C9(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 H2C(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C4(0.5) C10(0.5) H10(0.5) C6(0.5)
 H6A(0.5) H6B(0.5) H6C(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
5.a Riding coordinates:
 C1(H1A,H1B,H1C)
5.b Ternary CH refined with riding coordinates:
 N2(H2), N1(H1)
5.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C3(H3A,H3B)
5.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
5.e :
 C5(H5), C10(H10)
;
_shelx_res_checksum              6910
_shelx_hkl_checksum              75712
_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 9.958
_oxdiff_exptl_absorpt_empirical_full_min 0.309