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_7133088
_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
_audit_creation_date             2022-03-29
_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                   16.4064(4)
_cell_length_b                   16.4064(4)
_cell_length_c                   8.3883(3)
_cell_measurement_reflns_used    19527
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.05
_cell_measurement_theta_min      2.48
_cell_volume                     1955.38(10)
_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)
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_computing_data_reduction
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X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
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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 1.88, Darmstadt 2019
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
 816 frames, detector distance = 50 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
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_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
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_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            38204
_diffrn_reflns_point_group_measured_fraction_full 0.999
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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    3.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.057
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_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.843
_refine_diff_density_min         -1.749
_refine_diff_density_rms         0.365
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+0.8555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1825
_reflns_number_total             2586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01735h2.cif
_cod_data_source_block           jmx112
_cod_depositor_comments
'Adding full bibliography for 7133085--7133088.cif.'
_cod_original_cell_volume        1955.38(12)
_cod_database_code               7133088
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.604
_shelx_estimated_absorpt_t_min   0.395
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6111(11)
 0.3889(11)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{N1, C1}
{C2, N2}
4. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C1)
Uanis(C2) = Uanis(N2)
5. Others
 Sof(C1)=Sof(N2)=0.5*(1-FVAR(2))
 Sof(N1)=Sof(C2)=0.5*FVAR(2)
6.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              32281
_olex2_submission_special_instructions 'No special instructions were received'