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_7134442
_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            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-10-24
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.28699(15)
_cell_length_b                   6.38954(8)
_cell_length_c                   18.5355(3)
_cell_measurement_reflns_used    7186
_cell_measurement_temperature    325.00(11)
_cell_measurement_theta_max      29.9790
_cell_measurement_theta_min      1.9870
_cell_volume                     1455.19(3)
_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_environment      air
_diffrn_ambient_temperature      325.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.965
_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    -21.00  38.50   0.70   17.50    --   22.87  77.00   0.00   85
  2  \w    -67.00  38.00   0.70   17.50    --  -23.33  77.00 150.00  150
  3  \w    -65.00  68.00   0.70   17.50    --  -23.33  57.00 -90.00  190
  4  \w   -114.00  21.80   0.70   17.50    --  -23.33 -38.00 -30.00  194
  5  \w    -21.00  38.50   0.70   17.50    --   22.87  77.00 -60.00   85
  6  \w    -21.00  38.50   0.70   17.50    --   22.87  77.00 150.00   85
  7  \w      1.00  73.10   0.70   17.50    --   22.87 -99.00  30.00  103
  8  \w     61.00 123.30   0.70   17.50    --   22.87 178.00  90.00   89
  9  \w    -65.00  68.00   0.70   17.50    --  -23.33  57.00  90.00  190
 10  \w   -114.00  21.80   0.70   17.50    --  -23.33 -38.00 150.00  194
 11  \w    -21.00  38.50   0.70   17.50    --   22.87  77.00-180.00   85
 12  \w     61.00 123.30   0.70   17.50    --   22.87 178.00 -90.00   89
 13  \w    -21.00  36.40   0.70   17.50    --   22.87  77.00  60.00   82
 14  \w      1.00  73.10   0.70   17.50    --   22.87 -99.00   0.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0574763000
_diffrn_orient_matrix_UB_12      0.0060420000
_diffrn_orient_matrix_UB_13      0.0029879000
_diffrn_orient_matrix_UB_21      -0.0045399000
_diffrn_orient_matrix_UB_22      0.0011953000
_diffrn_orient_matrix_UB_23      0.0381372000
_diffrn_orient_matrix_UB_31      0.0030759000
_diffrn_orient_matrix_UB_32      -0.1108449000
_diffrn_orient_matrix_UB_33      0.0005700000
_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  0.0317
_diffrn_reflns_av_unetI/netI     0.0102
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18773
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.298
_diffrn_reflns_theta_min         1.989
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    22.505
_exptl_absorpt_correction_T_max  0.280
_exptl_absorpt_correction_T_min  0.033
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.144
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.842
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.00121(5)
_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   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         1195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0194
_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^)+(0.0203P)^2^+4.6163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1109
_reflns_number_total             1195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01232e2.cif
_cod_data_source_block           CsGPbI4_325K
_cod_depositor_comments
'Adding full bibliography for 7134427--7134444.cif.'
_cod_database_code               7134442
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: H5A(0.25) H5B(0.25) I2(0.25)
3.a X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N3(H3A,H3B)
;
_shelx_res_checksum              54242
_shelx_hkl_checksum              62851
_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 1.278
_oxdiff_exptl_absorpt_empirical_full_min 0.845