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_7718017
_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(C7.25 N2)'
_chemical_formula_sum            'C7.05 H12.8 Cl3 K N2 O12'
_chemical_formula_weight         463.04
_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_block_doi                 10.5517/ccdc.csd.cc2lml83
_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                   10.20150(10)
_cell_length_b                   10.20150(10)
_cell_length_c                   45.3252(6)
_cell_measurement_reflns_used    8638
_cell_measurement_temperature    299.99(10)
_cell_measurement_theta_max      75.9840
_cell_measurement_theta_min      1.9480
_cell_volume                     4085.06(8)
_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      299.99(10)
_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 0.985
_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     56.00  99.00   0.50    0.30    --  108.36-132.00  34.00   86
  2  \w    -24.00   8.00   0.50    0.10    --  -45.45  19.00  60.00   64
  3  \w   -115.00 -36.00   0.50    0.30    -- -102.00 132.00 104.00  158
  4  \w   -165.00 -82.00   0.50    0.30    -- -102.00 -15.00-120.00  166
  5  \w   -110.00 -67.00   0.50    0.10    --  -45.45-137.00-142.00   86
  6  \w    -27.00  59.00   0.50    0.10    --   45.45 -69.00-163.00  172
  7  \w     38.00  81.00   0.50    0.30    --  108.36 -69.00-163.00   86
  8  \w     35.00  60.00   0.50    0.30    --  108.36 -61.00 -90.00   50
  9  \w     44.00  69.00   0.50    0.30    --  108.36 -61.00  90.00   50
 10  \w     42.00  67.00   0.50    0.30    --  108.36 -61.00 150.00   50
 11  \w     92.00 175.00   0.50    0.30    --  108.36  45.00 120.00  166
;
_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      -0.0206820000
_diffrn_orient_matrix_UB_12      -0.0703750000
_diffrn_orient_matrix_UB_13      -0.0309280000
_diffrn_orient_matrix_UB_21      -0.1358099000
_diffrn_orient_matrix_UB_22      -0.1480972000
_diffrn_orient_matrix_UB_23      0.0113383000
_diffrn_orient_matrix_UB_31      -0.1073901000
_diffrn_orient_matrix_UB_32      0.0593035000
_diffrn_orient_matrix_UB_33      -0.0083835000
_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  0.0472
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            15002
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.352
_diffrn_reflns_theta_min         3.901
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48952
_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    1.882
_exptl_crystal_description       block
_exptl_crystal_F_000             2351
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.00060(7)
_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   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2863
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0696P)^2^+2.2676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2428
_reflns_number_total             2863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03416c2.cif
_cod_data_source_block           lys-240508-1-300k_autored
_cod_depositor_comments
'Adding full bibliography for 7718017--7718027.cif.'
_cod_original_cell_volume        4085.06(10)
_cod_original_formula_sum        'C7.05 H12.80 Cl3 K N2 O12'
_cod_database_code               7718017
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N K Cl O'
_shelx_estimated_absorpt_t_max   0.501
_shelx_estimated_absorpt_t_min   0.446
_reflns_odcompleteness_completeness 99.84
_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
 C9-C10 = C8-C10
 1.54 with sigma of 0.01
 N6-C9 = N6-C8
 1.47 with sigma of 0.01
 N6-C7
 1.47 with sigma of 0.01
 N5-N6
 1.45 with sigma of 0.01
 C7-C8
 2.21 with sigma of 0.02
 N5-C9
 2.21 with sigma of 0.02
 C10-N6
 2.21 with sigma of 0.02
 N6-C9 \\sim N6-C8
 with sigma of 0.02
 C9-C10 \\sim C8-C10
 with sigma of 0.02
3. Rigid bond restraints
 C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
N6 \\sim N5 \\sim C7 \\sim C9 \\sim C8 \\sim C10: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N5) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N6, N5, C7, C9, C8, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Fixed Sof: H1C(0.333333) H1A(0.333333) H1B(0.333333) N5(0.166667) C9(0.125)
 H6A(0.333333) H6B(0.333333) H6C(0.333333) N6(0.166667) C10(0.333333) C7(0.25)
 C8(0.5)
7.a Ternary CH refined with riding coordinates:
 N2(H2), N3(H3)
7.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B), C4(H4A,H4B), C3(H3B,H3A)
7.c Idealised Me refined as rotating group:
 C1(H1C,H1A,H1B), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              46644
_shelx_hkl_checksum              79682
_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 1.715
_oxdiff_exptl_absorpt_empirical_full_min 0.509