Effect of pressure and temperature on the structure and optical properties of two-dimensional lead iodide perovskites
Drushliak, Viktoriia; Szafrański, Marek; Chemical Communications 61 (2025) 8019–8022; doi:10.1039/D5CC01232E

data_7134428
_publ_section_title
;
 Effect of pressure and temperature on the structure and optical
 properties of two-dimensional lead iodide perovskites
;
_journal_issue                   44
_journal_name_full               'Chemical Communications'
_journal_page_first              8019
_journal_page_last               8022
_journal_paper_doi               10.1039/D5CC01232E
_journal_volume                  61
_journal_year                    2025
_chemical_formula_sum            'C2 H12 I4 N6 Pb'
_chemical_formula_weight         834.97
_chemical_name_systematic        'Guanidinium lead(II) tetraiodide'
_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   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2024-10-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 88.992(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.742(6)
_cell_length_b                   26.9140(17)
_cell_length_c                   9.2472(4)
_cell_measurement_pressure       150000(30000)
_cell_measurement_reflns_used    2037
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.3780
_cell_measurement_theta_min      2.6540
_cell_volume                     3170.7(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.301
_diffrn_measured_fraction_theta_max 0.235
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -35.00  19.75   0.75   60.00   0.00 -30.00   0.00    --    73
  2  \f    140.00 200.00   0.75   60.00   0.00 -30.00   0.00    --    80
  3  \f    160.00 217.00   0.75   60.00   0.00  30.00   0.00    --    76
  4  \f    -20.00  34.75   0.75   60.00   0.00  30.00   0.00    --    73
  5  \w    -24.00  24.00   0.75   60.00    --   30.00  39.46 -12.90   64
  6  \w    -24.00  24.00   0.75   60.00    --   30.00  39.46 167.10   64
  7  \w    -50.00  10.00   0.75   60.00    --  -30.00  39.46 167.10   80
  8  \w    -50.00  10.00   0.75   60.00    --  -30.00  39.46 -12.90   80
  9  \w    -64.00  -8.50   0.75   60.00    --  -30.00  81.40 -28.90   74
 10  \w    -64.00  -8.50   0.75   60.00    --  -30.00  81.40 151.10   74
 11  \w    -19.00   8.00   0.75   60.00    --   30.00  81.40 151.10   36
 12  \w    -19.00   8.00   0.75   60.00    --   30.00  81.40 -28.90   36
 13  \w    -43.00 -21.25   0.75   60.00    --   30.00 134.60 -56.90   29
 14  \w    -43.00 -21.25   0.75   60.00    --   30.00 134.60 123.10   29
 15  \w    -90.00 -36.00   0.75   60.00    --  -30.00 134.60 123.10   72
 16  \w    -90.00 -36.00   0.75   60.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0019354000
_diffrn_orient_matrix_UB_12      -0.0071520000
_diffrn_orient_matrix_UB_13      -0.0534815000
_diffrn_orient_matrix_UB_21      0.0334159000
_diffrn_orient_matrix_UB_22      -0.0227661000
_diffrn_orient_matrix_UB_23      0.0146055000
_diffrn_orient_matrix_UB_31      -0.0690819000
_diffrn_orient_matrix_UB_32      -0.0112041000
_diffrn_orient_matrix_UB_33      0.0044831000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.301
_diffrn_reflns_Laue_measured_fraction_max 0.235
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14294
_diffrn_reflns_point_group_measured_fraction_full 0.301
_diffrn_reflns_point_group_measured_fraction_max 0.235
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.357
_diffrn_reflns_theta_min         1.513
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    18.410
_exptl_absorpt_correction_T_max  0.23279
_exptl_absorpt_correction_T_min  0.21238
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.498
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.032
_exptl_crystal_size_rad          0.04
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       0.000097(13)
_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   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1864
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0228P)^2^+130.6049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1094
_reflns_number_total             1864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01232e2.cif
_cod_data_source_block           G2PbI4_0_15
_cod_depositor_comments
'Adding full bibliography for 7134427--7134444.cif.'
_cod_original_cell_volume        3170.9(14)
_cod_database_code               7134428
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
; 
Data were collected at room temperature and pressure of 0.15(3) GPa
(150000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Restrained distances
 C3-N58
 1.3 with sigma of 0.02
 C17-N11
 1.3 with sigma of 0.02
3. Others
 Uiso(N4)=Uiso(N5)=Uiso(N11)=Uiso(N19)=Uiso(N25)=Uiso(N26)=Uiso(N28)=Uiso(N30)=
 Uiso(N33)=Uiso(N48)=Uiso(N54)=Uiso(N58)=FVAR(1)
 Uiso(C3)=Uiso(C17)=Uiso(C38)=Uiso(C47)=FVAR(2)
4.a X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N5(H5A,H5B), N11(H11A,H11B), N19(H19A,H19B), N25(H25A,H25B),
 N26(H26A,H26B), N28(H28A,H28B), N30(H30A,H30B), N33(H33A,H33B), N48(H48A,H48B),
  N54(H54A,H54B), N58(H58A,H58B)
;
_shelx_res_checksum              38575
_shelx_hkl_checksum              94270
_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 1.685
_oxdiff_exptl_absorpt_empirical_full_min 0.755