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_7133087
_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         '3(I Pb0.333), C5 H12 N'
_chemical_formula_sum            'C5 H12 I3 N Pb'
_chemical_formula_weight         674.05
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-11
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_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                120
_cell_formula_units_Z            6
_cell_length_a                   16.745(4)
_cell_length_b                   16.745(4)
_cell_length_c                   8.387(3)
_cell_measurement_reflns_used    1977
_cell_measurement_temperature    273.00
_cell_measurement_theta_max      23.01
_cell_measurement_theta_min      2.43
_cell_volume                     2036.6(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.00
_diffrn_detector                 'PHOTON III C14'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Quest D8'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1402
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21901
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.433
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.202
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1075 before and 0.0811 after correction.
The Ratio of minimum to maximum transmission is 0.7866.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.298
_exptl_crystal_description       needle
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.666
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1438
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0071P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                845
_reflns_number_total             1438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01735h2.cif
_cod_data_source_block           jmx116a_176
_cod_depositor_comments
'Adding full bibliography for 7133085--7133088.cif.'
_cod_original_cell_volume        2036.5(12)
_cod_database_code               7133087
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.3 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1_1-C1_1 \\sim N1_1-C2_1
 N1_2-C1_2 \\sim N1_2-C2_2
 with sigma of 0.02
 C3_1-C4_1 \\sim C4_1-C5_1
 C3_2-C4_2 \\sim C4_2-C5_2
 with sigma of 0.02
 N1_1-C3_1 \\sim N1_1-C5_1
 N1_2-C3_2 \\sim N1_2-C5_2
 with sigma of 0.04
 C1_1-C4_1 \\sim C2_1-C4_1
 C1_2-C4_2 \\sim C2_2-C4_2
 with sigma of 0.04
3. Restrained planarity
 C1_1, C2_1, C3_1, C4_1, C5_1, N1_1
 C1_2, C2_2, C3_2, C4_2, C5_2, N1_2
 with sigma of 0.05
4. Uiso/Uaniso restraints and constraints
C1_1 \\sim C2_1 \\sim C3_1 \\sim C4_1 \\sim C5_1 \\sim N1_1 \\sim C1_2 \\sim
C2_2 \\sim C3_2 \\sim C4_2 \\sim C5_2 \\sim N1_2: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
5. Others
 Fixed Sof: C1(0.25) H1A(0.25) H1B(0.25) H1C(0.25) C2(0.25) H2A(0.25)
 H2B(0.25) H2C(0.25) C3(0.25) H3A(0.25) H3B(0.25) H3C(0.25) C4(0.25) C5(0.25)
 H5A(0.25) H5B(0.25) H5C(0.25) N1(0.25) C1(0.25) H1A(0.25) H1B(0.25) H1C(0.25)
 C2(0.25) H2A(0.25) H2B(0.25) H2C(0.25) C3(0.25) H3A(0.25) H3B(0.25) H3C(0.25)
 C4(0.25) C5(0.25) H5A(0.25) H5B(0.25) H5C(0.25) N1(0.25)
6.a Free rotating group:
 C1(C2,C3,C4,C5,N1)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C1(H1A,
 H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              59604
_olex2_submission_special_instructions 'No special instructions were received'