Three-dimensional perchlorate-based alkali metal hybrid perovskite molecular ferroelastic crystals.
Liu, Yu-Si; Xu, Zhe-Kun; Zhang, Jia-Mei; Chen, Xiao-Gang; Qin, Yan; Wang, Zhong-Xia; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4706–4714; doi:10.1039/d4dt03416c

data_7718020
_publ_section_title
;
 Three-dimensional perchlorate-based alkali metal hybrid perovskite
 molecular ferroelastic crystals.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4706
_journal_page_last               4714
_journal_paper_doi               10.1039/d4dt03416c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'Cl3 Cs O12, C8'
_chemical_formula_sum            'C8 Cl3 Cs O12'
_chemical_formula_weight         527.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-11-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-12 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            4
_cell_length_a                   10.5830(3)
_cell_length_b                   10.9576(3)
_cell_length_c                   15.4652(3)
_cell_measurement_reflns_used    3866
_cell_measurement_temperature    363.00(10)
_cell_measurement_theta_max      70.8750
_cell_measurement_theta_min      5.6910
_cell_volume                     1793.41(8)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      363.00(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 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     70.00 124.00   0.50    0.14    --   75.12  23.00 -73.00  108
  2  \w     77.00 121.00   0.50    0.14    --   75.18  30.00   0.00   88
  3  \w     80.00 120.00   0.50    0.14    --   75.18  30.00  60.00   80
  4  \w     81.00 121.00   0.50    0.14    --   75.18  30.00  90.00   80
  5  \w     11.00  36.00   0.50    0.14    --   60.54 -30.00   0.00   50
  6  \w     23.00  89.00   0.50    0.14    --   60.54-125.00  90.00  132
  7  \w     62.00 106.00   0.50    0.14    --   75.18-127.00  65.00   88
  8  \w     34.00  67.00   0.50    0.14    --   75.18-101.00 -39.00   66
  9  \w     11.00  36.00   0.50    0.14    --   60.54 -30.00 -60.00   50
 10  \w     24.00  49.00   0.50    0.14    --   60.54-101.00 -39.00   50
 11  \w     11.00  38.00   0.50    0.14    --   60.54 -30.00-150.00   54
 12  \w     40.00  68.00   0.50    0.14    --   60.54 -94.00-180.00   56
 13  \w     60.00  88.00   0.50    0.14    --   60.54-125.00-180.00   56
 14  \w     25.00  51.00   0.50    0.14    --   60.54-125.00-180.00   52
 15  \w     43.00  84.00   0.50    0.14    --   75.18 -94.00  60.00   82
 16  \w     55.00  85.00   0.50    0.14    --   75.18 -94.00 120.00   60
 17  \w    -96.00 -56.00   0.50    0.14    --  -60.72 -23.00 121.00   80
 18  \w   -103.00 -77.00   0.50    0.14    --  -75.50 125.00  60.00   52
 19  \w   -121.00 -77.00   0.50    0.14    --  -74.13 -30.00 -30.00   88
 20  \w   -102.00 -69.00   0.50    0.14    --  -60.72 -30.00 -90.00   66
 21  \w   -119.00 -77.00   0.50    0.14    --  -74.13 -30.00-180.00   84
 22  \w   -112.00 -86.00   0.50    0.14    --  -74.13-143.00-103.00   52
 23  \w   -116.00 -80.00   0.50    0.14    --  -74.13-125.00 -30.00   72
;
_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      0.1358184000
_diffrn_orient_matrix_UB_12      0.0321622000
_diffrn_orient_matrix_UB_13      -0.0277796000
_diffrn_orient_matrix_UB_21      0.0293097000
_diffrn_orient_matrix_UB_22      -0.1365801000
_diffrn_orient_matrix_UB_23      -0.0124740000
_diffrn_orient_matrix_UB_31      -0.0436010000
_diffrn_orient_matrix_UB_32      0.0083703000
_diffrn_orient_matrix_UB_33      -0.0948270000
_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  0.1085
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5686
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.565
_diffrn_reflns_theta_max         66.565
_diffrn_reflns_theta_min         5.722
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27352
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.804
_refine_diff_density_min         -1.992
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         867
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.1101
_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^)+(0.1000P)^2^+180.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2725
_refine_ls_wR_factor_ref         0.2745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                784
_reflns_number_total             867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03416c2.cif
_cod_data_source_block           lys-240413-1-re-363k_r
_cod_depositor_comments
'Adding full bibliography for 7718017--7718027.cif.'
_cod_database_code               7718020
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N F Cl O Cs'
_shelx_estimated_absorpt_t_max   0.231
_shelx_estimated_absorpt_t_min   0.190
_olex2_refinement_description
;
1. Restrained distances
 O5-O4
 2.1 with sigma of 0.02
2. Rigid bond restraints
 C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O3, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C3, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Cl2, Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O2(0.5) C3(0.25) C6(0.5) C5(0.25) C2(0.5) O1(0.5) C4(0.5)
;
_shelx_res_checksum              97491
_shelx_hkl_checksum              37247
_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 2.242
_oxdiff_exptl_absorpt_empirical_full_min 0.244