Giant mechanical tunability by a coordination bond strategy in a 3D hybrid cyanide double perovskite ferroelastic with reconstructive phase transition
Lv, Hui-Peng; Hu, Sheng-Qian; Bai, Yong-Ju; Zhou, Jun-Si; Ji, Luan-Ying; Wang, Zhong-Xia; Ai, Yong; Qin, Yan; Chen, Xiao-Gang; Chemical Science 16 (2025) 9109–9116; doi:10.1039/D5SC00620A

data_1574470
_publ_section_title
;
 Giant mechanical tunability by a coordination bond strategy in a 3D
 hybrid cyanide double perovskite ferroelastic with reconstructive phase
 transition
;
_journal_issue                   21
_journal_name_full               'Chemical Science'
_journal_page_first              9109
_journal_page_last               9116
_journal_paper_doi               10.1039/D5SC00620A
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C12 Fe2 K2 N12, 4(C2 H8 N O)'
_chemical_formula_sum            'C20 H32.03 Fe2 K2 N16 O4'
_chemical_formula_weight         750.51
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-03-26 deposited with the CCDC.	2025-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9108(9)
_cell_length_b                   11.9108(9)
_cell_length_c                   11.9108(9)
_cell_measurement_reflns_used    421
_cell_measurement_temperature    388.01(10)
_cell_measurement_theta_max      24.6990
_cell_measurement_theta_min      2.9120
_cell_volume                     1689.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.129a 64-bit (release 29-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      388.01(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 0.991
_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     16.00  65.00   0.50   10.00    --    0.56  21.00 -97.00   98
  2  \w     22.00  57.00   0.50   10.00    --    0.56  19.00   0.00   70
;
_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      -0.0437528000
_diffrn_orient_matrix_UB_12      -0.0169837000
_diffrn_orient_matrix_UB_13      -0.0367527000
_diffrn_orient_matrix_UB_21      0.0295707000
_diffrn_orient_matrix_UB_22      -0.0502087000
_diffrn_orient_matrix_UB_23      -0.0121987000
_diffrn_orient_matrix_UB_31      -0.0275354000
_diffrn_orient_matrix_UB_32      -0.0273992000
_diffrn_orient_matrix_UB_33      0.0450806000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            1133
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.714
_diffrn_reflns_theta_min         2.962
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.129a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     19
_refine_ls_number_reflns         156
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0539
_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^)+(0.1132P)^2^+1.1588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                122
_reflns_number_total             156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00620a2.cif
_cod_data_source_block           eaoh_1_388k
_cod_depositor_comments
'Adding full bibliography for 1574470--1574474.cif.'
_cod_original_cell_volume        1689.8(4)
_cod_database_code               1574470
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N K Fe O'
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C2-C3
 1.53 with sigma of 0.01
 N2-C3
 2.41 with sigma of 0.01
 N2-O1
 2.8 with sigma of 0.01
 O1-C3
 1.43 with sigma of 0.01
 N2-C2
 1.47 with sigma of 0.01
 O1-C2
 2.46 with sigma of 0.01
 N2-C3
 2.49 with sigma of 0.04
 O1-C2 \\sim N2-C3
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O1 \\sim N2 \\sim C2 \\sim C3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(N2) = Uiso(C2) = Uiso(C3) = Uiso(O1)
Uanis(N1) = Uanis(C1) = Uanis(K1)
4. Rigid body (RIGU) restrains
 O1, N2, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N1(0.125) O1(0.04167) H1(0.04167) N2(0.04167) H2A(0.04167)
 H2B(0.04167) H2C(0.04167) C2(0.04167) H2D(0.04167) H2E(0.04167) C3(0.04167)
 H3A(0.04167) H3B(0.04167)
6.a Riding coordinates:
 O1(H1), N2(H2A,H2B,H2C)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2D,H2E), C3(H3A,H3B)
;
_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 6.098
_oxdiff_exptl_absorpt_empirical_full_min 0.635