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_7718021
_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 K1 O12, 0.8(C7 H16 N2), 0.2(C7 N2)'
_chemical_formula_sum            'C7 H12.8 Cl3 K N2 O12'
_chemical_formula_weight         462.44
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-24
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-24 deposited with the CCDC.	2025-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            10
_cell_length_a                   10.2651(2)
_cell_length_b                   10.2651(2)
_cell_length_c                   45.4929(9)
_cell_measurement_reflns_used    7803
_cell_measurement_temperature    362.98(13)
_cell_measurement_theta_max      76.0900
_cell_measurement_theta_min      1.9130
_cell_volume                     4151.46(14)
_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      362.98(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_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    136.00 175.00   0.50    0.80    --  108.36 125.00  30.00   78
  2  \w     82.00 129.00   0.50    0.80    --  108.36 125.00  30.00   94
  3  \w     91.00 167.00   0.50    0.80    --  108.36  45.00 -30.00  152
  4  \w     85.00 178.00   0.50    0.80    --  108.36  16.00 102.00  186
  5  \w    -20.00  33.00   0.50    0.20    --  -45.45  16.00 102.00  106
  6  \w     -2.00  24.00   0.50    0.20    --  -45.45  20.00  14.00   52
  7  \w    -66.00 -29.00   0.50    0.80    -- -102.00  72.00 -35.00   74
  8  \w    -24.00  25.00   0.50    0.20    --  -45.45  19.00-120.00   98
  9  \w    -21.00  15.00   0.50    0.20    --  -45.45  19.00-180.00   72
 10  \w     48.00  73.00   0.50    0.80    --  108.36 -61.00   0.00   50
 11  \w     39.00  65.00   0.50    0.80    --  108.36 -61.00 150.00   52
 12  \w   -158.00 -81.00   0.50    0.80    -- -102.00 -20.00-152.00  154
;
_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      -0.0273709000
_diffrn_orient_matrix_UB_12      0.0344751000
_diffrn_orient_matrix_UB_13      0.0316142000
_diffrn_orient_matrix_UB_21      -0.1377523000
_diffrn_orient_matrix_UB_22      0.0090520000
_diffrn_orient_matrix_UB_23      -0.0106243000
_diffrn_orient_matrix_UB_31      -0.1016310000
_diffrn_orient_matrix_UB_32      -0.1696322000
_diffrn_orient_matrix_UB_33      0.0058409000
_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  0.0369
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            15468
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.371
_diffrn_reflns_theta_min         3.887
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.889
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14305
_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    1.850
_exptl_crystal_description       block
_exptl_crystal_F_000             2348
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.00036(6)
_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   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2894
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0783P)^2^+1.5146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2391
_reflns_number_total             2894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03416c2.cif
_cod_data_source_block           lys-240508-1-363k_auto
_cod_depositor_comments
'Adding full bibliography for 7718017--7718027.cif.'
_cod_original_cell_volume        4151.46(18)
_cod_original_formula_sum        'C7 H12.80 Cl3 K N2 O12'
_cod_database_code               7718021
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N K Cl O'
_shelx_estimated_absorpt_t_max   0.477
_shelx_estimated_absorpt_t_min   0.427
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C2 = C4-C2 = C2-C1 = N1-C2 = N2-N1 = N2-C1 = N2-C3 = C3-C2
 1.4 with sigma of 0.2
3. Rigid bond restraints
 N2, C4, C2, C1, N1, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
N2 \\sim C4 \\sim C2 \\sim C1 \\sim C3 \\sim N1: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
Uanis(N2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
5. Others
 Fixed Sof: H00C(0.333333) H00D(0.333333) H00E(0.333333) C4(0.25) C1(0.166667)
 H00N(0.333333) H00O(0.333333) H00P(0.333333) N2(0.166667) C2(0.5) C3(0.25)
 N1(0.166667)
6.a Ternary CH refined with riding coordinates:
 N00G(H00G), N00L(H00L)
6.b Secondary CH2 refined with riding coordinates:
 C00M(H00A,H00B), C00N(H00I,H00J), C00O(H00K,H00M), C00Q(H00F,H00H)
6.c Idealised Me refined as rotating group:
 C00P(H00C,H00D,H00E), C00T(H00N,H00O,H00P)
;
_shelx_res_checksum              21945
_shelx_hkl_checksum              60035
_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 5.280
_oxdiff_exptl_absorpt_empirical_full_min 0.604