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_7133086
_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         'I, C5 H12 N'
_chemical_formula_sum            'C5 H12 I N'
_chemical_formula_weight         213.06
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-04
_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                90
_cell_formula_units_Z            2
_cell_length_a                   7.38460(10)
_cell_length_b                   7.38460(10)
_cell_length_c                   7.2299(2)
_cell_measurement_reflns_used    27457
_cell_measurement_temperature    100
_cell_measurement_theta_max      39.03
_cell_measurement_theta_min      3.90
_cell_volume                     394.263(13)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_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 1.88, Darmstadt 2019
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 2934 frames, detector distance = 40 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  0.0172
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         42.627
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_diffrn_source                   'GeniX Mo'
_diffrn_source_current           1.000
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_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.964
_exptl_absorpt_correction_T_max  0.8036
_exptl_absorpt_correction_T_min  0.2828
_exptl_absorpt_correction_type   multi-scan
_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    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             204
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.798
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         755
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0172
_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^)+(0.0213P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_ref         0.0375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                719
_reflns_number_total             755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01735h2.cif
_cod_data_source_block           jmx114
_cod_depositor_comments
'Adding full bibliography for 7133085--7133088.cif.'
_cod_original_cell_volume        394.263(15)
_cod_database_code               7133086
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.592
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1_1-C1_1 \\sim N1_1-C2_1
 with sigma of 0.02
 C3_1-C4_1 \\sim C4_1-C5_1
 with sigma of 0.02
3. Restrained planarity
 C1_1, C2_1, C3_1, C4_1, C5_1, N1_1
 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: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 C1_1, C2_1, C3_1, C4_1, C5_1, N1_1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: C1(0.125) H1A(0.125) H1B(0.125) H1C(0.125) C2(0.125) H2A(0.125)
 H2B(0.125) H2C(0.125) C3(0.125) H3A(0.125) H3B(0.125) H3C(0.125) C4(0.125)
 C5(0.125) H5A(0.125) H5B(0.125) H5C(0.125) N1(0.125)
7.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              41336
_olex2_submission_special_instructions 'No special instructions were received'