Formation of iminium ions during the processing of metal halide perovskites.
Möbs, Jakob; Tomori, Ajna; Heine, Johanna; Chemical communications (Cambridge, England) 60 (2024) 6488–6491; doi:10.1039/d4cc01735h

data_7133085
_publ_section_title
;
 Formation of iminium ions during the processing of metal halide
 perovskites.
;
_journal_issue                   51
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6488
_journal_page_last               6491
_journal_paper_doi               10.1039/d4cc01735h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'I3 Pb, C6 N'
_chemical_formula_sum            'C6 I3 N Pb'
_chemical_formula_weight         673.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_audit_creation_date             2023-11-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-06 deposited with the CCDC.	2024-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8521(4)
_cell_length_b                   11.3081(8)
_cell_length_c                   15.9901(9)
_cell_measurement_reflns_used    4452
_cell_measurement_temperature    230
_cell_measurement_theta_max      31.58
_cell_measurement_theta_min      2.55
_cell_volume                     1419.80(15)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
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X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
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_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      230
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
 550 frames, detector distance = 70 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  Stoe_Stadivari_Mo
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13193
_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_full        25.242
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_diffrn_source                   'GeniX Mo'
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_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.022
_exptl_crystal_size_rad          0.034
_refine_diff_density_max         1.423
_refine_diff_density_min         -2.326
_refine_diff_density_rms         0.311
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0676P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1242
_reflns_number_total             1887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01735h2.cif
_cod_data_source_block           jmx175_62_fcf
_cod_depositor_comments
'Adding full bibliography for 7133085--7133088.cif.'
_cod_database_code               7133085
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.688
_shelx_estimated_absorpt_t_min   0.289
_olex2_refinement_description
;
1. Others
 Fixed Sof: N1(0.5) C3(0.5)
;
_shelx_res_checksum              98873
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '70.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '8.4 cm'
_stoe_detector_size_y            '10.6 cm'
_stoe_evaluation_integration_a   6.0
_stoe_evaluation_integration_b   1.5
_stoe_evaluation_integration_ems 0.012
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 8
_stoe_evaluation_lana_bos_l_odd_max 5
_stoe_evaluation_lana_completeness 97.6
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 64.9
_stoe_evaluation_lana_max_2theta_desired 64.9
_stoe_evaluation_lana_mean_redundancy 3.5
_stoe_evaluation_lana_number_refls_after_or 21694
_stoe_evaluation_lana_number_refls_outliers 4739
_stoe_evaluation_lana_number_refls_total 26433
_stoe_evaluation_lana_number_refls_unique 6153
_stoe_evaluation_lana_number_refls_written 26475
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group mmm
_stoe_evaluation_lana_table
;
2Theta           7.8   14.6   21.4   28.2   35.0   41.8   48.6   55.4   62.2
<Resolution>    4.65   2.71   1.88   1.44   1.17   0.99   0.86   0.77   0.70
N(total)         192    691   1429   1691   3819   4800   5467   5964   2380
<Redundancy>     3.9    4.2    4.1    3.1    4.5    4.3    3.9    3.4    2.0
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0  100.0  100.0   89.9
<I/sigma>       49.2   53.3   25.2   22.1    9.0    6.3    3.1    1.7    0.8
R(int)         0.039  0.023  0.030  0.037  0.055  0.071  0.129  0.205  0.325
;
_stoe_measurement_identifier     jmx175
_stoe_measurement_max_exposure_per_frame '150.0 s'
_stoe_measurement_mean_exposure_per_frame '150.0 s'
_stoe_measurement_min_exposure_per_frame '150.0 s'
_stoe_measurement_total_exposure_time '22.9 h'
_stoe_measurement_total_frame_number 550
_stoe_measurement_total_run_number 8
_stoe_measurement_tube_power     '50.0 W'