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_7718022
_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 K O12, 2(C4)'
_chemical_formula_sum            'C8 Cl3 K O12'
_chemical_formula_weight         433.53
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-11
_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            1
_cell_length_a                   7.5772(10)
_cell_length_b                   7.5772(10)
_cell_length_c                   7.5772(10)
_cell_measurement_reflns_used    228
_cell_measurement_temperature    422.9(2)
_cell_measurement_theta_max      72.6950
_cell_measurement_theta_min      5.8010
_cell_volume                     435.04(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      422.9(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.937
_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     72.00  98.00   0.50    0.09    --   45.20 146.00  -1.00   52
  2  \w     46.00 102.00   0.50    0.35    --  108.36 -94.00  30.00  112
  3  \w    -11.00  33.00   0.50    0.09    --  -45.20  19.00-150.00   88
  4  \w    -54.00 -28.00   0.50    0.35    -- -102.00  56.00-174.00   52
  5  \w    -56.00 -30.00   0.50    0.35    -- -102.00  66.00  74.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0927768000
_diffrn_orient_matrix_UB_12      -0.0083787000
_diffrn_orient_matrix_UB_13      0.1804538000
_diffrn_orient_matrix_UB_21      -0.1748137000
_diffrn_orient_matrix_UB_22      -0.0508359000
_diffrn_orient_matrix_UB_23      -0.0916870000
_diffrn_orient_matrix_UB_31      0.0478160000
_diffrn_orient_matrix_UB_32      -0.1966909000
_diffrn_orient_matrix_UB_33      0.0157763000
_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  0.0352
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            428
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.842
_diffrn_reflns_theta_min         5.839
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.468
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022)
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    1.655
_exptl_crystal_description       block
_exptl_crystal_F_000             214
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.1331
_refine_ls_R_factor_gt           0.1250
_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^)+(0.1000P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3060
_refine_ls_wR_factor_ref         0.3117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                85
_reflns_number_total             119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03416c2.cif
_cod_data_source_block           lys-240318-2-423k_autored
_cod_depositor_comments
'Adding full bibliography for 7718017--7718027.cif.'
_cod_original_cell_volume        435.04(17)
_cod_database_code               7718022
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N K Cl'
_shelx_estimated_absorpt_t_max   0.522
_shelx_estimated_absorpt_t_min   0.468
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2)
2. Others
 Fixed Sof: O1(0.25) C1(0.041667) C2(0.125)
;
_shelx_res_checksum              22374
_shelx_hkl_checksum              27916
_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 2.167
_oxdiff_exptl_absorpt_empirical_full_min 0.575