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_7718025
_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, C7 H15 F N2'
_chemical_formula_sum            'C7 H15 Cl3 Cs F N2 O12'
_chemical_formula_weight         577.47
_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             2024-11-12
_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                 97.6196(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3570(2)
_cell_length_b                   10.64331(15)
_cell_length_c                   10.84725(18)
_cell_measurement_reflns_used    7526
_cell_measurement_temperature    300.00(10)
_cell_measurement_theta_max      72.2670
_cell_measurement_theta_min      5.0510
_cell_volume                     1757.32(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.128a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.128a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.128a (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      300.00(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 0.992
_diffrn_measured_fraction_theta_max 0.947
_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  48.00   0.50    0.05    --    8.00  67.00 149.92   54
  2  \w     94.00 119.00   0.50    0.05    --   70.62  43.00-164.92   50
  3  \w     97.00 122.00   0.50    0.05    --   77.76  34.00-120.32   50
  4  \w     86.00 114.00   0.50    0.05    --   70.62  58.00 -20.05   56
  5  \w     24.00  49.00   0.50    0.05    --   63.87 -94.00  60.00   50
  6  \w     25.00  52.00   0.50    0.05    --   63.87 -94.00 120.00   54
  7  \w     40.00  65.00   0.50    0.05    --   63.87 -94.00 150.00   50
  8  \w     45.00  83.00   0.50    0.05    --   77.37 -94.00 120.00   76
  9  \w     26.00  51.00   0.50    0.05    --   63.87 -94.00 -60.00   50
 10  \w     33.00  80.00   0.50    0.05    --   72.68 -94.00 -30.00   94
 11  \w     38.00  79.00   0.50    0.05    --   77.37 -94.00 -90.00   82
 12  \w     49.00  82.00   0.50    0.05    --   77.37 -94.00 -60.00   66
 13  \w     31.00  59.00   0.50    0.05    --   63.87 -94.00-120.00   56
 14  \w     50.00  75.00   0.50    0.05    --   77.37 -94.00-120.00   50
 15  \w     27.00  68.00   0.50    0.05    --   63.87 -94.00-150.00   82
 16  \w   -113.00 -74.00   0.50    0.05    --  -76.19 -11.00  93.60   78
 17  \w   -115.00 -90.00   0.50    0.05    --  -76.19 -68.00  27.31   50
 18  \w   -116.00 -86.00   0.50    0.05    --  -71.12 -59.00-110.97   60
 19  \w   -115.00 -88.00   0.50    0.05    --  -71.12 -42.00-154.65   54
 20  \w   -113.00 -87.00   0.50    0.05    --  -72.00 -55.00  -9.47   52
 21  \w   -118.00 -93.00   0.50    0.05    --  -76.19 -22.00 -39.59   50
 22  \w   -115.00 -89.00   0.50    0.05    --  -71.12 -25.00 -15.95   52
 23  \w   -114.00 -88.00   0.50    0.05    --  -71.12 -51.00  38.08   52
 24  \w    -70.00 -44.00   0.50    0.05    --  -28.00 -47.00  29.03   52
 25  \w   -116.00 -86.00   0.50    0.05    --  -71.12 -52.00 148.89   60
 26  \w    -45.00 -20.00   0.50    0.05    --  -64.37 125.00   0.00   50
 27  \w    -90.00 -58.00   0.50    0.05    --  -64.37 125.00   0.00   64
 28  \w    -86.00 -26.00   0.50    0.05    --  -70.60 125.00  30.00  120
 29  \w    -27.50 -20.00   0.50    0.05    --  -64.37 125.00  60.00   15
;
_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      -0.0736254000
_diffrn_orient_matrix_UB_12      -0.0076959000
_diffrn_orient_matrix_UB_13      -0.1109264000
_diffrn_orient_matrix_UB_21      -0.0644988000
_diffrn_orient_matrix_UB_22      -0.0463440000
_diffrn_orient_matrix_UB_23      0.0876040000
_diffrn_orient_matrix_UB_31      -0.0258595000
_diffrn_orient_matrix_UB_32      0.1368789000
_diffrn_orient_matrix_UB_33      0.0233396000
_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  0.0653
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12289
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.155
_diffrn_reflns_theta_min         2.903
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.362
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.128a (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    2.183
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.731
_refine_diff_density_min         -1.758
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3382
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0553
_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^)+(0.1190P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2848
_reflns_number_total             3382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03416c2.cif
_cod_data_source_block           lys-240413-1-r1-300k_auto
_cod_depositor_comments
'Adding full bibliography for 7718017--7718027.cif.'
_cod_database_code               7718025
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C Cl O Cs H F N'
_shelx_estimated_absorpt_t_max   0.224
_shelx_estimated_absorpt_t_min   0.060
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2. Restrained distances
 Cs2-O8 \\sim Cs2-O9
 with sigma of 0.02
 Cl2-O8 \\sim Cl2-O9
 with sigma of 0.02
 Cs2-O9 \\sim Cs2-O8
 with sigma of 0.02
3. Rigid bond restraints
 O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(O9)=1-FVAR(1)
 Sof(O8)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 N1(H1)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C6(H6A,H6B), C5(H5A,H5B), C4(H4A,H4B), C3(H3A,H3B),
 C7(H7A,H7B)
;
_shelx_res_checksum              79726
_shelx_hkl_checksum              22794
_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 8.581
_oxdiff_exptl_absorpt_empirical_full_min 0.298