Effective enhancement of mechanical properties <i>via</i> H/F substitution in 3D cyanide hybrid perovskites.
Ji, Luan-Ying; Zhou, Jun-Si; Liu, Shu-Yi; Qin, Yan; Lv, Hui-Peng; Chen, Xiao-Gang; Chemical communications (Cambridge, England) 61 (2025) 13165–13168; doi:10.1039/d5cc03229f

data_7134869
_publ_section_title
;
 Effective enhancement of mechanical properties <i>via</i> H/F
 substitution in 3D cyanide hybrid perovskites.
;
_journal_issue                   70
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13165
_journal_page_last               13168
_journal_paper_doi               10.1039/d5cc03229f
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'C6 Fe K N6, 6(C0.25 H F0.17 N0.17), 6(C0.42 H1.33 F0.17 N0.17)  '
_chemical_formula_sum            'C10 H14 F2 Fe K N8'
_chemical_formula_weight         379.24
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-07-18 deposited with the CCDC.	2025-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.71500(10)
_cell_length_b                   11.71500(10)
_cell_length_c                   11.71500(10)
_cell_measurement_reflns_used    2762
_cell_measurement_temperature    272.99(10)
_cell_measurement_theta_max      75.1560
_cell_measurement_theta_min      5.3260
_cell_volume                     1607.78(2)
_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 1.3 (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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      272.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.961
_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     42.00  69.00   0.50    1.00    --  108.36 -61.00-180.00   54
  2  \w     35.00  63.00   0.50    1.00    --  108.36 -61.00-150.00   56
  3  \w     40.00  70.00   0.50    1.00    --  108.36 -61.00 -60.00   60
  4  \w     38.00  63.00   0.50    1.00    --  108.36 -61.00 -30.00   50
  5  \w     43.00  70.00   0.50    1.00    --  108.36 -61.00 150.00   54
  6  \w    -27.00  24.00   0.50    0.30    --   45.20 -13.00 101.00  102
  7  \w    -32.00  23.00   0.50    0.30    --   45.20 -19.00-120.00  110
  8  \w   -171.00-104.00   0.50    1.00    -- -102.00 -32.00  58.00  134
  9  \w   -152.00 -87.00   0.50    1.00    -- -102.00-115.00 -17.00  130
 10  \w    -68.00 -43.00   0.50    1.00    -- -102.00  61.00-180.00   50
 11  \w   -107.00 -44.00   0.50    1.00    -- -102.00 125.00-120.00  126
 12  \w    -31.00  30.00   0.50    0.30    --  -45.20  37.00  90.00  122
 13  \w     49.00  93.00   0.50    1.00    --  108.36-118.00  75.00   88
;
_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      -0.0340743000
_diffrn_orient_matrix_UB_12      -0.1170972000
_diffrn_orient_matrix_UB_13      -0.0492266000
_diffrn_orient_matrix_UB_21      -0.0631551000
_diffrn_orient_matrix_UB_22      0.0597851000
_diffrn_orient_matrix_UB_23      -0.0986211000
_diffrn_orient_matrix_UB_31      0.1102275000
_diffrn_orient_matrix_UB_32      -0.0019201000
_diffrn_orient_matrix_UB_33      -0.0716979000
_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  0.0248
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5742
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.316
_diffrn_reflns_theta_min         3.773
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59783
_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            'dark red'
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         583
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0941
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+18.1087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2180
_reflns_Friedel_coverage         0.000
_reflns_number_gt                579
_reflns_number_total             583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03229f2.cif
_cod_data_source_block           lmz_fyakfecn6_273k_cubic
_cod_depositor_comments
'Adding full bibliography for 7134868--7134871.cif.'
_cod_original_cell_volume        1607.78(4)
_cod_database_code               7134869
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N F K Fe  '
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.432(15)
 0.568(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
3. Restrained distances
 C3A-C2A = C3B-C2B = N2A-C2A = N2B-C2B
 1.45 with sigma of 0.02
 F1B-C3B = F1A-C3A
 1.3 with sigma of 0.02
 N2B-C3B
 2.4 with sigma of 0.02
 C3A-N2A
 2.4 with sigma of 0.02
 F1B-C2B
 2.3 with sigma of 0.02
 F1A-C2A
 2.3 with sigma of 0.02
 C3A-C2A = C3B-C2B
 1.53 with sigma of 0.01
 N2A-C2A = N2B-C2B
 1.48 with sigma of 0.01
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(N1B) = Uanis(C1B) = Uanis(C1A) = Uanis(N1A)
Uanis(F1A) = Uanis(F1B)
Uanis(N2A) = Uanis(N2B)
Uanis(C2A) = Uanis(C2B)
Uanis(C3A) = Uanis(C3B)
Uanis(F1B) = Uanis(F1A) = Uanis(C3A) = Uanis(C3B) = Uanis(C2A) = Uanis(C2B) =
Uanis(N2B) = Uanis(N2A)
6. Others
 Fixed Sof: N1B(0.5) C1B(0.5) C2A(0.08333) H2AA(0.08333) H2AB(0.08333)
 C3A(0.16667) H3AA(0.16667) H3AB(0.16667) N2A(0.16667) H2AC(0.16667)
 H2AD(0.16667) H2AE(0.16667) F1A(0.16667) F1B(0.16667) N2B(0.16667)
 H2BA(0.16667) H2BB(0.16667) H2BC(0.16667) C2B(0.25) H2BD(0.25) H2BE(0.25)
 C3B(0.16667) H3BA(0.16667) H3BB(0.16667) C1A(0.5) N1A(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C3A(H3AA,H3AB), C2B(H2BD,H2BE), C3B(H3BA,H3BB)
7.b Idealised Me refined as rotating group:
 N2A(H2AC,H2AD,H2AE), N2B(H2BA,H2BB,H2BC)
;
_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 1.372
_oxdiff_exptl_absorpt_empirical_full_min 0.783