Centimeter-Sized Single Crystals of 3D Perovskitiod (4-AP)Pb2X6 (X = Br, I) for Efficient and Stable X-ray Detection
Dai, Hongliang; Zhu, Zeng-Kui; You, Shihai; Luo, Junhua; Chemical Science  (2026) –; doi:10.1039/D6SC00616G

data_1577095
_publ_section_title
;
 Centimeter-Sized Single Crystals of 3D Perovskitiod (4-AP)Pb2X6 (X = Br,
 I) for Efficient and Stable X-ray Detection
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D6SC00616G
_journal_year                    2026
_chemical_formula_moiety         'Br6 Pb2, C6 H9 N3'
_chemical_formula_sum            'C6 H9 Br6 N3 Pb2'
_chemical_formula_weight         1008.068
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_Int_Tables_number      52
_atom_sites_solution_primary     direct
_audit_creation_date             2023-12-05
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-12-05 deposited with the CCDC.	2026-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.9011(15)
_cell_length_b                   15.7772(10)
_cell_length_c                   9.6867(5)
_cell_measurement_reflns_used    5812
_cell_measurement_temperature    295.00(10)
_cell_measurement_theta_max      28.5620
_cell_measurement_theta_min      3.6400
_cell_volume                     3652.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9961
_diffrn_measured_fraction_theta_max 0.8442
_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     -8.00  17.00   1.00   29.15    --   -7.31-113.00 163.00   25
  2  \w      3.00  48.00   1.00   29.15    --   -7.31  22.00 163.00   45
  3  \w     -9.00  72.00   1.00   29.15    --    6.30  38.00-120.00   81
  4  \w    -14.00  11.00   1.00   29.15    --   -7.31 -99.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0256988000
_diffrn_orient_matrix_UB_12      -0.0222016000
_diffrn_orient_matrix_UB_13      0.0052097000
_diffrn_orient_matrix_UB_21      -0.0136638000
_diffrn_orient_matrix_UB_22      0.0381251000
_diffrn_orient_matrix_UB_23      0.0191160000
_diffrn_orient_matrix_UB_31      -0.0055850000
_diffrn_orient_matrix_UB_32      0.0087219000
_diffrn_orient_matrix_UB_33      -0.0705084000
_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  0.0459
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.9961
_diffrn_reflns_Laue_measured_fraction_max 0.8442
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17692
_diffrn_reflns_point_group_measured_fraction_full 0.9961
_diffrn_reflns_point_group_measured_fraction_max 0.8442
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    31.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.666
_exptl_crystal_description       block
_exptl_crystal_F_000             3399.330
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.8409
_refine_diff_density_min         -2.3889
_refine_diff_density_rms         0.4988
_refine_ls_d_res_high            0.7368
_refine_ls_d_res_low             5.9753
_refine_ls_goodness_of_fit_ref   1.0612
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    16
_refine_ls_number_parameters     157
_refine_ls_number_reflns         4042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0612
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+3.3767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              31
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                2931
_reflns_number_total             4042
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d6sc00616g2.cif
_cod_data_source_block           3D_auto
_cod_database_code               1577095
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), N1(H1), C1(H1a), C4(H4)
2.b X=CH2 refined with riding coordinates:
 N3(H3a,H3b), N2(H2a,H2b)
;
_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 2.317
_oxdiff_exptl_absorpt_empirical_full_min 0.572