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_7718024
_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, C7 H15 F N2'
_chemical_formula_sum            'C7 H15 Cl3 F K N2 O12'
_chemical_formula_weight         483.66
_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
_atom_sites_solution_primary     iterative
_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                 96.6675(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.05583(19)
_cell_length_b                   10.39932(12)
_cell_length_c                   10.67058(13)
_cell_measurement_reflns_used    6840
_cell_measurement_temperature    299(3)
_cell_measurement_theta_max      76.2010
_cell_measurement_theta_min      2.9450
_cell_volume                     1659.40(4)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299(3)
_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 0.963
_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  49.00   0.50    0.05    --   45.20 -65.00-178.00   50
  2  \w     40.00  73.00   0.50    0.05    --  108.36 -65.00-178.00   66
  3  \w     91.00 178.00   0.50    0.05    --  108.36  65.00 -43.00  174
  4  \w     90.00 167.00   0.50    0.05    --  108.36  30.00  90.00  154
  5  \w     47.00  91.00   0.50    0.05    --  108.36 -77.00 120.00   88
  6  \w     35.00  64.00   0.50    0.05    --  108.36 -61.00  90.00   58
  7  \w     48.00  73.00   0.50    0.05    --  108.36 -61.00  60.00   50
  8  \w     43.00  68.00   0.50    0.05    --  108.36 -61.00-120.00   50
  9  \w     44.00  73.00   0.50    0.05    --  108.36 -61.00-150.00   58
 10  \w     35.00  70.00   0.50    0.05    --  108.36 -94.00   0.00   70
 11  \w    -64.00 -37.00   0.50    0.05    --  -45.20  65.00 -43.00   54
 12  \w    -23.00  32.00   0.50    0.05    --  -45.20  19.00 -60.00  110
 13  \w    -17.00  21.00   0.50    0.05    --  -45.20  65.00 -43.00   76
 14  \w     36.00 103.00   0.50    0.05    --  108.36 -94.00 150.00  134
 15  \w    -24.00  30.00   0.50    0.05    --  -45.20  19.00 120.00  108
 16  \w    -59.00 -33.00   0.50    0.05    -- -102.00  61.00 150.00   52
 17  \w    -67.00 -41.00   0.50    0.05    -- -102.00  61.00  90.00   52
 18  \w    -72.00 -32.00   0.50    0.05    -- -102.00  65.00 -43.00   80
 19  \w   -161.00 -85.00   0.50    0.05    -- -102.00 -30.00-120.00  152
 20  \w   -175.00-119.00   0.50    0.05    -- -102.00 -61.00 -60.00  112
 21  \w   -170.00-144.00   0.50    0.05    -- -102.00 -65.00-178.00   52
 22  \w   -116.00 -24.00   0.50    0.05    --  -45.20 -65.00-178.00  184
;
_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      -0.0850688000
_diffrn_orient_matrix_UB_12      0.0398471000
_diffrn_orient_matrix_UB_13      0.0576045000
_diffrn_orient_matrix_UB_21      0.0536461000
_diffrn_orient_matrix_UB_22      0.1039031000
_diffrn_orient_matrix_UB_23      0.0791158000
_diffrn_orient_matrix_UB_31      -0.0223445000
_diffrn_orient_matrix_UB_32      0.0977778000
_diffrn_orient_matrix_UB_33      -0.1074874000
_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  0.0507
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10176
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.403
_diffrn_reflns_theta_min         2.955
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.015
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40216
_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    1.936
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0051(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0863P)^2^+0.6194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2976
_reflns_number_total             3348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03416c2.cif
_cod_data_source_block           lys-240318-2-300k_auto
_cod_depositor_comments
'Adding full bibliography for 7718017--7718027.cif.'
_cod_original_cell_volume        1659.40(3)
_cod_database_code               7718024
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N K Cl'
_shelx_estimated_absorpt_t_max   0.501
_shelx_estimated_absorpt_t_min   0.446
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C7(H7A,H7B), C2(H2A,H2B), C6(H6A,H6B), C1(H1A,H1B), C5(H5A,H5B),
 C3(H3A,H3B)
;
_shelx_res_checksum              18722
_shelx_hkl_checksum              61692
_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 1.985
_oxdiff_exptl_absorpt_empirical_full_min 0.529