A three-dimensional lead iodide perovskite analog featuring hydrogen-bonded dual monovalent cations.
Wang, Wei; Liu, Cheng-Dong; Fan, Chang-Chun; Zhang, Wen; Chemical science 15 (2024) 18455–18462; doi:10.1039/d4sc05585c

data_1572858
_publ_section_title
;
 A three-dimensional lead iodide perovskite analog featuring
 hydrogen-bonded dual monovalent cations.
;
_journal_issue                   44
_journal_name_full               'Chemical science'
_journal_page_first              18455
_journal_page_last               18462
_journal_paper_doi               10.1039/d4sc05585c
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'I6 Pb2, C4 H10 N O, H4 N'
_chemical_formula_sum            'C4 H14 I6 N2 O Pb2'
_chemical_formula_weight         1281.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-09-28
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-28 deposited with the CCDC.	2024-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.579(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.3366(3)
_cell_length_b                   16.1613(7)
_cell_length_c                   10.1821(4)
_cell_measurement_reflns_used    5055
_cell_measurement_temperature    152.98(10)
_cell_measurement_theta_max      30.8560
_cell_measurement_theta_min      2.0120
_cell_volume                     1040.69(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      152.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.802
_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    -65.00 -15.00   0.50    1.20    --    4.75 -37.00 -30.00  100
  2  \w    -10.00  15.00   0.50    1.20    --   -5.92 -99.00 -30.00   50
  3  \w     -8.00  70.00   0.50    1.20    --    4.75  37.00 150.00  156
  4  \w    -28.00  14.00   0.50    1.20    --   -5.92  77.00  30.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0633113000
_diffrn_orient_matrix_UB_12      0.0026195000
_diffrn_orient_matrix_UB_13      0.0597764000
_diffrn_orient_matrix_UB_21      -0.0094135000
_diffrn_orient_matrix_UB_22      0.0437444000
_diffrn_orient_matrix_UB_23      -0.0013622000
_diffrn_orient_matrix_UB_31      -0.0921103000
_diffrn_orient_matrix_UB_32      -0.0026676000
_diffrn_orient_matrix_UB_33      0.0359468000
_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     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.802
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7163
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.802
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.928
_diffrn_reflns_theta_min         2.004
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    25.042
_exptl_absorpt_correction_T_max  0.255
_exptl_absorpt_correction_T_min  0.043
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.92a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.091
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.239
_refine_diff_density_min         -2.360
_refine_diff_density_rms         0.397
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         2731
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0660P)^2^+6.5136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2478
_reflns_number_total             2731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05585c2.cif
_cod_data_source_block           sc_11_153k_autoabs
_cod_depositor_comments          'Adding full bibliography for 1572858.cif.'
_cod_database_code               1572858
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C8  H16  I12  N2  O4  Pb4  '
_shelx_estimated_absorpt_t_max   0.315
_shelx_estimated_absorpt_t_min   0.037
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 N1-H1D = N1-H1C
 0.893 with sigma of 0.002
 H1E-N1
 0.893 with sigma of 0.002
 H1E-H1C \\sim H1E-H1C_$1 \\sim H1C-H1C_$1 \\sim H1D-H1C \\sim H1E-H1D \\sim
H1D-H1C_$1
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C1(H1A,H1B), C2(H2C,H2D)
;
_shelx_res_checksum              13952
_shelx_hkl_checksum              3354
_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 1.986
_oxdiff_exptl_absorpt_empirical_full_min 0.580