#------------------------------------------------------------------------------
#$Date: 2024-07-05 16:12:34 +0300 (Fri, 05 Jul 2024) $
#$Revision: 292766 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/30/7133085.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7133085
loop_
_publ_author_name
'Möbs, Jakob'
'Tomori, Ajna'
'Heine, Johanna'
_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)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_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, ω 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
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.474
_diffrn_reflns_theta_min         2.548
_diffrn_source                   'GeniX Mo'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.363
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_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(μ₂-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/[σ²(Fo²)+(0.0676P)²] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_file
;
TITL jmx175_62_a.res in Pnma
    jmx175_62_fcf.res
    created by SHELXL-2018/3 at 16:03:17 on 02-Nov-2023
REM Old TITL jmx175_62 in Pnma
REM SHELXT solution in Pnma: R1 0.119, Rweak 0.002, Alpha 0.012
REM <I/s> 0.351 for 136 systematic absences, Orientation as input
REM Formula found by SHELXT: N3 I3 Pb
CELL 0.71073 7.8521 11.3081 15.9901 90 90 90
ZERR 4 0.0004 0.0008 0.0009 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C I N Pb
UNIT 24 12 4 4
EQIV $1 +X,1.5-Y,+Z

L.S. 10
PLAN  12
SIZE 0.022 0.035 0.09
TEMP -43.15
CONF
FREE N1 N1_$1
FREE C3 N1
FREE C3 C3_$1
list 4
MORE -1
fmap 2 53
acta
OMIT 0 57
REM <olex2.extras>
REM <HklSrc "%.\\jmx175_merged.fcf.hkl">
REM </olex2.extras>

WGHT    0.067600
FVAR       0.50970
PB1   4    0.573077    0.250000    0.250666    10.50000    0.02092    0.03586 =
         0.03473    0.00000    0.00026    0.00000
I1    2    0.320708    0.445502    0.167998    11.00000    0.03340    0.03387 =
         0.04320    0.00652   -0.00095    0.00004
I2    2    0.327569    0.250000    0.408636    10.50000    0.03439    0.04137 =
         0.02921    0.00000    0.00107    0.00000
C1    1    0.538404    0.750000    0.274151    10.50000    0.03234    0.07054 =
         0.04535    0.00000    0.00242    0.00000
C5    1    0.094780    0.750000    0.455506    10.50000    0.03437    0.05333 =
         0.05636    0.00000   -0.00611    0.00000
C2    1    0.547020    0.750000    0.369136    10.50000    0.03706    0.06145 =
         0.04485    0.00000   -0.00050    0.00000
C4    1    0.312973    0.580383    0.412616    11.00000    0.08824    0.04502 =
         0.05180   -0.01607    0.00536   -0.00207
PART 1
N1    3    0.258571    0.705666    0.423126    10.50000    0.02975
C3    1    0.371434    0.716950    0.405226    10.50000    0.04013
HKLF 4




REM  jmx175_62_a.res in Pnma
REM wR2 = 0.1181, GooF = S = 1.003, Restrained GooF = 1.003 for all data
REM R1 = 0.0421 for 1242 Fo > 4sig(Fo) and 0.0740 for all 1887 data
REM 57 parameters refined using 0 restraints

END

WGHT      0.0676      0.0000

REM Highest difference peak  1.423,  deepest hole -2.326,  1-sigma level  0.311
Q1    1   0.6357  0.3033  0.2453  11.00000  0.05    1.42
Q2    1   0.5885  0.3140  0.2104  11.00000  0.05    1.28
Q3    1   0.5029  0.3035  0.2513  11.00000  0.05    1.26
Q4    1   0.1849  0.7500  0.5751  10.50000  0.05    1.20
Q5    1   0.3261  0.3777  0.2096  11.00000  0.05    1.19
Q6    1   0.3273  0.7500  0.4807  10.50000  0.05    1.16
Q7    1   0.1827  0.2500  0.5172  10.50000  0.05    1.15
Q8    1   0.3269  0.5187  0.1363  11.00000  0.05    1.14
Q9    1   0.5625  0.1779  0.2910  11.00000  0.05    1.12
Q10   1  -0.0484  0.7500  0.3982  10.50000  0.05    1.05
Q11   1   0.3714  0.3825  0.1403  11.00000  0.05    1.04
Q12   1   0.3991  0.1839  0.3978  11.00000  0.05    0.96
;
_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'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.57308(6) 0.250000 0.25067(4) 0.03050(17) Uani 1 2 d S T P . .
I1 I 0.32071(8) 0.44550(6) 0.16800(4) 0.0368(2) Uani 1 1 d . . . . .
I2 I 0.32757(13) 0.250000 0.40864(6) 0.0350(2) Uani 1 2 d S T P . .
C1 C 0.538(2) 0.750000 0.2742(11) 0.049(4) Uani 1 2 d S T P . .
C5 C 0.095(2) 0.750000 0.4555(12) 0.048(4) Uani 1 2 d S T P . .
C2 C 0.547(2) 0.750000 0.3691(11) 0.048(4) Uani 1 2 d S T P . .
C4 C 0.313(2) 0.5804(12) 0.4126(8) 0.062(4) Uani 1 1 d . . . . .
N1 N 0.259(2) 0.7057(14) 0.4231(10) 0.030(4) Uiso 0.5 1 d . . P A 1
C3 C 0.371(3) 0.7170(18) 0.4052(13) 0.040(5) Uiso 0.5 1 d . . P A 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0209(2) 0.0359(3) 0.0347(3) 0.000 0.0003(2) 0.000
I1 0.0334(4) 0.0339(4) 0.0432(4) 0.0065(3) -0.0010(3) 0.0000(3)
I2 0.0344(5) 0.0414(5) 0.0292(4) 0.000 0.0011(4) 0.000
C1 0.032(8) 0.071(13) 0.045(9) 0.000 0.002(8) 0.000
C5 0.034(9) 0.053(11) 0.056(11) 0.000 -0.006(8) 0.000
C2 0.037(9) 0.061(12) 0.045(10) 0.000 0.000(8) 0.000
C4 0.088(11) 0.045(7) 0.052(8) -0.016(6) 0.005(8) -0.002(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 86.76(3) 6_656 4 ?
I1 Pb1 I1 93.75(2) 6_656 . ?
I1 Pb1 I1 179.48(2) 4 . ?
I1 Pb1 I1 93.75(2) 4 7_565 ?
I1 Pb1 I1 179.48(2) 6_656 7_565 ?
I1 Pb1 I1 85.73(3) . 7_565 ?
I1 Pb1 I2 86.85(2) 6_656 6_656 ?
I1 Pb1 I2 86.85(2) 4 6_656 ?
I2 Pb1 I1 92.60(2) . 4 ?
I2 Pb1 I1 87.33(2) . 7_565 ?
I2 Pb1 I1 93.23(2) 6_656 . ?
I2 Pb1 I1 87.33(2) . . ?
I2 Pb1 I1 92.60(2) . 6_656 ?
I2 Pb1 I1 93.23(2) 6_656 7_565 ?
I2 Pb1 I2 179.24(4) . 6_656 ?
Pb1 I1 Pb1 74.738(15) 6_556 . ?
Pb1 I2 Pb1 75.46(2) . 6_556 ?
N1 C5 N1 39.8(13) 7_575 . ?
C1 C2 C3 109.5(15) . . ?
C1 C2 C3 109.5(15) . 7_575 ?
C3 C2 C3 28.1(16) . 7_575 ?
N1 C4 C3 34.9(9) . . ?
C5 N1 C4 127.8(14) . . ?
C3 N1 C5 116.8(14) 7_575 . ?
C3 N1 C4 115.3(16) 7_575 . ?
C2 C3 C4 120.9(15) . . ?
N1 C3 C2 122.6(16) 7_575 . ?
N1 C3 C4 116.2(17) 7_575 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.2187(8) 6_656 ?
Pb1 I1 3.2187(8) 4 ?
Pb1 I1 3.2499(8) . ?
Pb1 I1 3.2499(8) 7_565 ?
Pb1 I2 3.1775(11) . ?
Pb1 I2 3.2375(12) 6_656 ?
C1 C2 1.52(2) . ?
C5 N1 1.47(2) 7_575 ?
C5 N1 1.47(2) . ?
C2 C3 1.54(3) . ?
C2 C3 1.54(3) 7_575 ?
C4 N1 1.49(2) . ?
C4 C3 1.62(2) . ?
N1 C3 1.28(2) 7_575 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 82.1(16) . . . . ?
C1 C2 C3 N1 -91(2) . . . 7_575 ?
N1 C5 N1 C4 179.8(13) 7_575 . . . ?
N1 C5 N1 C3 3.3(19) 7_575 . . 7_575 ?
N1 C4 C3 C2 -174(3) . . . . ?
N1 C4 C3 N1 -1.0(6) . . . 7_575 ?
C3 C2 C3 C4 177.2(13) 7_575 . . . ?
C3 C2 C3 N1 4(2) 7_575 . . 7_575 ?
C3 C4 N1 C5 -176(3) . . . . ?
C3 C4 N1 C3 0.7(5) . . . 7_575 ?
