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_1574473
_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         'C6 Fe K N6, 2(C2 H8 N O)'
_chemical_formula_sum            'C10 H16 Fe K N8 O2'
_chemical_formula_weight         375.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                 92.024(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7784(5)
_cell_length_b                   11.6709(4)
_cell_length_c                   11.9663(5)
_cell_measurement_reflns_used    10085
_cell_measurement_temperature    300.00(10)
_cell_measurement_theta_max      49.7720
_cell_measurement_theta_min      2.3620
_cell_volume                     1643.92(11)
_computing_cell_refinement       'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.129a (Rigaku OD, 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      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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     19.00  44.00   0.50    2.17    --    0.76  46.00 -48.32   50
  2  \w     17.00  42.00   0.50    2.17    --    0.76  43.00  -7.85   50
  3  \w     19.00  44.00   0.50    2.17    --    0.76  48.00 -65.19   50
  4  \w     24.00  53.00   0.50    2.17    --   17.18  19.00-180.00   58
  5  \w     25.00  53.00   0.50    2.17    --   17.18  19.00-150.00   56
  6  \w    -23.00   2.00   0.50    2.17    --   20.00 -49.00 -37.90   50
  7  \w    -47.00 -22.00   0.50    2.17    --    0.76 -31.00-118.28   50
  8  \w    -12.00  17.00   0.50    2.17    --   32.00 -34.00-139.87   58
  9  \w    -16.00   9.00   0.50    2.17    --   28.00 -48.00 -23.00   50
 10  \w    -46.00 -16.00   0.50    2.17    --  -15.66 -19.00-150.00   60
 11  \w    -59.00 -16.00   0.50    2.17    --  -15.66 -19.00-180.00   86
;
_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      0.0110256000
_diffrn_orient_matrix_UB_12      0.0033512000
_diffrn_orient_matrix_UB_13      0.0585340000
_diffrn_orient_matrix_UB_21      -0.0278790000
_diffrn_orient_matrix_UB_22      -0.0532493000
_diffrn_orient_matrix_UB_23      0.0070605000
_diffrn_orient_matrix_UB_31      0.0522854000
_diffrn_orient_matrix_UB_32      -0.0291212000
_diffrn_orient_matrix_UB_33      -0.0062383000
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13784
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.385
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79315
_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_colour_primary    red
_exptl_crystal_density_diffrn    1.516
_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          0.1
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2885
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0434P)^2^+3.1310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2286
_reflns_number_total             2885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00620a2.cif
_cod_data_source_block           eaoh__1_300k_cool_auto
_cod_depositor_comments
'Adding full bibliography for 1574470--1574474.cif.'
_cod_original_cell_volume        1643.93(12)
_cod_database_code               1574473
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Fe K '
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.833
_reflns_odcompleteness_completeness 99.92
_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 C(H,H,H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C8-C7 = C9-C10
 1.53 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(N3) = Uanis(C3)
4. Others
 Fixed Sof: O1(0.7) H1(0.7) O3(0.3) H3(0.3) H7AA(0.75) H7AB(0.75) H7BC(0.25)
 H7BD(0.25)
5.a Riding coordinates:
 O1(H1), O3(H3), N7(H7A,H7B,H7C), N8(H8C,H8D,H8E)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7AA,H7AB), C7(H7BC,H7BD), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
5.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_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 1.412
_oxdiff_exptl_absorpt_empirical_full_min 0.783