# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3APPbI3_1_a
_database_code_depnum_ccdc_archive 'CCDC 2192958'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2022-07-27 deposited with the CCDC.	2023-10-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H20 I6 N4 Pb'
_chemical_formula_weight         1188.91

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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0064 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4611 1.7922 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.1439 9.9644 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6700(17)
_cell_length_b                   8.7800(18)
_cell_length_c                   10.557(2)
_cell_angle_alpha                91.10(3)
_cell_angle_beta                 108.87(3)
_cell_angle_gamma                112.65(3)
_cell_volume                     692.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15298
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       plate
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.852
_exptl_crystal_F_000             520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    12.164
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8340
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.036
_diffrn_reflns_theta_max         33.605
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.748
_diffrn_measured_fraction_theta_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.748
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.748
_diffrn_reflns_point_group_measured_fraction_full 0.931
_reflns_number_total             4275
_reflns_number_gt                4223
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0691P)²+0.6199P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0110(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4275
_refine_ls_number_parameters     107
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1289
_refine_ls_wR_factor_gt          0.1288
_refine_ls_goodness_of_fit_ref   1.418
_refine_ls_restrained_S_all      1.418
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 1.000000 0.500000 0.500000 0.03077(10) Uani 1 2 d S . P . .
N1 N 0.5135(9) 0.2640(8) 1.0044(5) 0.0494(14) Uani 1 1 d . . . . .
H1 H 0.467482 0.229729 1.064982 0.059 Uiso 1 1 calc R U . . .
C1 C 0.6592(9) 0.4047(9) 1.0389(6) 0.0480(14) Uani 1 1 d . . . . .
H1A H 0.708701 0.465968 1.125896 0.058 Uiso 1 1 calc R U . . .
I1 I 0.57241(4) 0.36265(5) 0.36817(4) 0.04105(12) Uani 1 1 d . . . . .
I3 I 1.01585(5) 0.74676(5) 0.73696(4) 0.04147(12) Uani 1 1 d . . . . .
C3 C 0.6577(8) 0.3680(8) 0.8134(6) 0.0432(12) Uani 1 1 d . . . . .
H3 H 0.706941 0.405316 0.747615 0.052 Uiso 1 1 calc R U . . .
I2 I 0.96402(5) 0.21082(4) 0.69033(4) 0.03891(12) Uani 1 1 d . . . . .
N2 N 0.2858(7) 0.1709(8) 0.5511(5) 0.0446(11) Uani 1 1 d . . . . .
H2A H 0.235645 0.107289 0.469769 0.067 Uiso 1 1 calc R U . . .
H2B H 0.201469 0.160982 0.585136 0.067 Uiso 1 1 calc R U . . .
H2C H 0.341060 0.277292 0.543384 0.067 Uiso 1 1 calc R U . . .
C2 C 0.7373(9) 0.4599(10) 0.9431(7) 0.0525(17) Uani 1 1 d . . . . .
H2 H 0.841705 0.557342 0.965647 0.063 Uiso 1 1 calc R U . . .
C5 C 0.4331(9) 0.1712(8) 0.8805(6) 0.0441(13) Uani 1 1 d . . . . .
H5 H 0.329132 0.073943 0.861206 0.053 Uiso 1 1 calc R U . . .
C4 C 0.5054(7) 0.2209(7) 0.7818(5) 0.0352(10) Uani 1 1 d . . . . .
C6 C 0.4193(9) 0.1156(8) 0.6443(6) 0.0419(12) Uani 1 1 d . . . . .
H6 H 0.359534 -0.000747 0.651830 0.050 Uiso 1 1 calc R U . . .
H00D H 0.510381 0.124942 0.606712 0.050 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 3.2077(13) . ?
Pb1 I1 3.2077(13) 2_766 ?
Pb1 I3 3.2109(11) . ?
Pb1 I3 3.2109(11) 2_766 ?
Pb1 I2 3.2516(10) 2_766 ?
Pb1 I2 3.2516(10) . ?
N1 C1 1.318(9) . ?
N1 C5 1.338(8) . ?
C1 C2 1.387(9) . ?
C3 C4 1.381(8) . ?
C3 C2 1.385(10) . ?
N2 C6 1.503(9) . ?
C5 C4 1.378(8) . ?
C4 C6 1.496(8) . ?

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 180.000(14) . 2_766 ?
I1 Pb1 I3 91.50(4) . . ?
I1 Pb1 I3 88.50(4) 2_766 . ?
I1 Pb1 I3 88.50(4) . 2_766 ?
I1 Pb1 I3 91.50(4) 2_766 2_766 ?
I3 Pb1 I3 180.0 . 2_766 ?
I1 Pb1 I2 89.45(3) . 2_766 ?
I1 Pb1 I2 90.55(3) 2_766 2_766 ?
I3 Pb1 I2 90.43(2) . 2_766 ?
I3 Pb1 I2 89.57(2) 2_766 2_766 ?
I1 Pb1 I2 90.55(3) . . ?
I1 Pb1 I2 89.45(3) 2_766 . ?
I3 Pb1 I2 89.57(2) . . ?
I3 Pb1 I2 90.43(2) 2_766 . ?
I2 Pb1 I2 180.0 2_766 . ?
C1 N1 C5 123.9(5) . . ?
N1 C1 C2 118.8(6) . . ?
C4 C3 C2 120.0(5) . . ?
C3 C2 C1 119.2(6) . . ?
N1 C5 C4 119.5(5) . . ?
C5 C4 C3 118.6(5) . . ?
C5 C4 C6 119.9(5) . . ?
C3 C4 C6 121.5(5) . . ?
C4 C6 N2 110.4(5) . . ?

_refine_diff_density_max         5.408
_refine_diff_density_min         -1.639
_refine_diff_density_rms         0.322

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3appbsn_1_a_pl
_database_code_depnum_ccdc_archive 'CCDC 2192960'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2022-07-27 deposited with the CCDC.	2023-10-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H10 I4 N2 Pb0.50 Sn0.50'
_chemical_formula_weight         780.70

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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4611 1.7922 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0064 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.1439 9.9644 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6597 1.4093 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   9.4920(19)
_cell_length_b                   12.889(3)
_cell_length_c                   25.031(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                90
_cell_volume                     3062.4(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    63508
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       plate
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.387
_exptl_crystal_F_000             2704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    13.666
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36118
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.603
_diffrn_reflns_theta_max         33.525
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.835
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             10904
_reflns_number_gt                6420
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10904
_refine_ls_number_parameters     279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1403
_refine_ls_R_factor_gt           0.0980
_refine_ls_wR_factor_ref         0.3412
_refine_ls_wR_factor_gt          0.3041
_refine_ls_goodness_of_fit_ref   1.821
_refine_ls_restrained_S_all      1.821
_refine_ls_shift/su_max          3.952
_refine_ls_shift/su_mean         0.048

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
Pb2 Pb 0.27287(12) 0.250000 0.15825(5) 0.0449(3) Uani 1 2 d S T P . .
Pb4 Pb 0.81185(13) 0.750000 0.33845(5) 0.0492(3) Uani 1 2 d S T P . .
I005 I 0.68336(19) 0.750000 0.44768(7) 0.0404(4) Uani 1 2 d S T P . .
I006 I 1.18483(19) 0.750000 0.05239(7) 0.0414(4) Uani 1 2 d S T P . .
I007 I 0.42406(19) 0.250000 0.05144(7) 0.0425(4) Uani 1 2 d S T P . .
I008 I 0.92381(19) 0.250000 0.44804(7) 0.0432(4) Uani 1 2 d S T P . .
I009 I 0.9856(2) 0.750000 0.22020(8) 0.0483(5) Uani 1 2 d S T P . .
I00A I 0.4864(2) 0.750000 0.27992(8) 0.0501(5) Uani 1 2 d S T P . .
I00B I 1.09988(19) 0.750000 0.38544(8) 0.0493(5) Uani 1 2 d S T P . .
I00C I 1.59924(19) 0.750000 0.11462(9) 0.0512(5) Uani 1 2 d S T P . .
I00D I 0.80381(18) 0.50008(9) 0.33868(6) 0.0515(4) Uani 1 1 d . . . . .
I00E I 0.30319(18) 0.50002(9) 0.16123(6) 0.0518(4) Uani 1 1 d . . . . .
I00H I 0.00427(19) 0.250000 0.09307(9) 0.0525(5) Uani 1 2 d S T P . .
I00I I 0.50523(19) 0.250000 0.40708(9) 0.0528(5) Uani 1 2 d S T P . .
I00J I 0.5808(2) 0.250000 0.22628(9) 0.0537(5) Uani 1 2 d S T P . .
I0K I 1.0806(2) 0.250000 0.27328(9) 0.0525(5) Uani 1 2 d S T P . .
Sn1 Sn 0.77251(13) 0.250000 0.34163(5) 0.0141(2) Uani 1 2 d S T P . .
Sn3 Sn 1.31157(13) 0.750000 0.16143(5) 0.0171(3) Uani 1 2 d S T P . .
N1P N 0.877(3) 0.5782(16) 0.0350(9) 0.069(6) Uani 1 1 d . . . . .
H1P1 H 0.933214 0.619500 0.018556 0.04(6) Uiso 1 1 d R . . . .
N2P N 0.698(3) 0.526(2) 0.2037(11) 0.080(7) Uani 1 1 d . . . . .
H2P1 H 0.706483 0.516189 0.238806 0.16(18) Uiso 1 1 d R . . . .
H2P2 H 0.689685 0.593129 0.196826 0.08(9) Uiso 1 1 d R . . . .
H2P3 H 0.621915 0.492459 0.191966 0.5(6) Uiso 1 1 d R . . . .
C1P C 0.698(2) 0.441(2) 0.0862(12) 0.067(7) Uani 1 1 d . . . . .
H1P H 0.638891 0.397275 0.105074 0.04(6) Uiso 1 1 calc R . . . .
C2P C 0.687(3) 0.451(2) 0.0352(11) 0.061(7) Uani 1 1 d . . . . .
H2P H 0.622892 0.410562 0.016221 0.06(4) Uiso 1 1 calc R . . . .
C3P C 0.773(4) 0.526(3) 0.0082(13) 0.100(13) Uani 1 1 d . . . . .
H3P H 0.758747 0.538632 -0.027944 0.04(6) Uiso 1 1 calc R . . . .
C4P C 0.880(3) 0.5636(18) 0.0881(10) 0.055(5) Uani 1 1 d . . . . .
H4P H 0.941807 0.604350 0.107708 0.2(2) Uiso 1 1 calc R . . . .
C5P C 0.807(2) 0.5007(14) 0.1135(10) 0.046(5) Uani 1 1 d . . . . .
C6P C 0.830(4) 0.481(2) 0.1747(11) 0.076(8) Uani 1 1 d . . . . .
H6PA H 0.838629 0.407274 0.181718 0.5(6) Uiso 1 1 calc R . . . .
H6PB H 0.914411 0.515576 0.186872 2(4) Uiso 1 1 calc R . . . .
N3P N 0.190(3) 0.454(2) 0.4590(19) 0.117(13) Uani 1 1 d . . . . .
H3P1 H 0.123230 0.420622 0.474661 0.10(11) Uiso 1 1 d R . . . .
N4P N 0.200(2) 0.5315(19) 0.2982(9) 0.064(5) Uani 1 1 d . . . . .
H4P1 H 0.205916 0.522246 0.263033 0.2(2) Uiso 1 1 d R . . . .
H4P2 H 0.120276 0.504366 0.310276 2(4) Uiso 1 1 d R . . . .
H4P3 H 0.202426 0.599066 0.305536 0.15(16) Uiso 1 1 d R . . . .
C7P C 0.302(2) 0.4974(14) 0.3848(9) 0.042(4) Uani 1 1 d . . . . .
C8P C 0.207(3) 0.444(2) 0.4105(10) 0.058(6) Uani 1 1 d . . . . .
H8P H 0.151822 0.397045 0.391826 2(4) Uiso 1 1 calc R . . . .
C9P C 0.273(4) 0.521(3) 0.4927(14) 0.107(15) Uani 1 1 d . . . . .
H9P H 0.258894 0.525440 0.529399 0.13(14) Uiso 1 1 calc R . . . .
C10P C 0.378(3) 0.5793(17) 0.4653(9) 0.057(6) Uani 1 1 d . . . . .
H10P H 0.439131 0.623870 0.483188 2(4) Uiso 1 1 calc R . . . .
C11P C 0.384(2) 0.5663(15) 0.4138(10) 0.050(5) Uani 1 1 d . . . . .
H11P H 0.448419 0.606523 0.394923 0.02(4) Uiso 1 1 calc R . . . .
C12P C 0.323(3) 0.483(2) 0.3260(11) 0.070(8) Uani 1 1 d . . . . .
H12A H 0.409727 0.516368 0.314733 2(4) Uiso 1 1 calc R . . . .
H12B H 0.328433 0.410037 0.317326 0.04(5) Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Pb2 I00H 3.027(2) . ?
Pb2 I007 3.035(2) . ?
Pb2 I00E 3.2362(14) . ?
Pb2 I00E 3.2362(14) 4_565 ?
Pb2 I00J 3.383(2) . ?
Pb2 I0K 3.409(2) 1_455 ?
Pb4 I00B 2.976(2) . ?
Pb4 I005 2.994(2) . ?
Pb4 I00D 3.2221(13) 4_575 ?
Pb4 I00D 3.2222(13) . ?
Pb4 I009 3.388(2) . ?
Pb4 I00A 3.419(2) . ?
I006 Sn3 2.983(2) . ?
I008 Sn1 3.026(2) . ?
I00C Sn3 2.971(2) . ?
I00E Sn3 3.2230(13) 1_455 ?
I00I Sn1 3.020(2) . ?
N1P C4P 1.34(3) . ?
N1P C3P 1.37(4) . ?
N1P H1P1 0.8602 . ?
N2P C6P 1.56(4) . ?
N2P H2P1 0.8902 . ?
N2P H2P2 0.8900 . ?
N2P H2P3 0.8900 . ?
C1P C2P 1.29(4) . ?
C1P C5P 1.45(3) . ?
C1P H1P 0.9300 . ?
C2P C3P 1.43(5) . ?
C2P H2P 0.9300 . ?
C3P H3P 0.9300 . ?
C4P C5P 1.24(3) . ?
C4P H4P 0.9300 . ?
C5P C6P 1.57(4) . ?
C6P H6PA 0.9700 . ?
C6P H6PB 0.9700 . ?
N3P C8P 1.23(4) . ?
N3P C9P 1.44(5) . ?
N3P H3P1 0.8598 . ?
N4P C12P 1.49(4) . ?
N4P H4P1 0.8900 . ?
N4P H4P2 0.8900 . ?
N4P H4P3 0.8901 . ?
C7P C8P 1.30(3) . ?
C7P C11P 1.39(3) . ?
C7P C12P 1.50(3) . ?
C8P H8P 0.9300 . ?
C9P C10P 1.43(4) . ?
C9P H9P 0.9300 . ?
C10P C11P 1.30(3) . ?
C10P H10P 0.9300 . ?
C11P H11P 0.9300 . ?
C12P H12A 0.9700 . ?
C12P H12B 0.9700 . ?

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
I00H Pb2 I007 85.61(6) . . ?
I00H Pb2 I00E 95.01(4) . . ?
I007 Pb2 I00E 88.75(3) . . ?
I00H Pb2 I00E 95.01(4) . 4_565 ?
I007 Pb2 I00E 88.75(3) . 4_565 ?
I00E Pb2 I00E 169.46(7) . 4_565 ?
I00H Pb2 I00J 177.60(7) . . ?
I007 Pb2 I00J 91.99(6) . . ?
I00E Pb2 I00J 84.93(4) . . ?
I00E Pb2 I00J 84.93(4) 4_565 . ?
I00H Pb2 I0K 90.25(6) . 1_455 ?
I007 Pb2 I0K 175.86(6) . 1_455 ?
I00E Pb2 I0K 91.61(3) . 1_455 ?
I00E Pb2 I0K 91.62(3) 4_565 1_455 ?
I00J Pb2 I0K 92.15(7) . 1_455 ?
I00B Pb4 I005 90.76(7) . . ?
I00B Pb4 I00D 91.21(4) . 4_575 ?
I005 Pb4 I00D 89.35(3) . 4_575 ?
I00B Pb4 I00D 91.21(4) . . ?
I005 Pb4 I00D 89.35(3) . . ?
I00D Pb4 I00D 177.28(7) 4_575 . ?
I00B Pb4 I009 84.15(6) . . ?
I005 Pb4 I009 174.91(6) . . ?
I00D Pb4 I009 90.75(4) 4_575 . ?
I00D Pb4 I009 90.75(4) . . ?
I00B Pb4 I00A 177.91(7) . . ?
I005 Pb4 I00A 91.33(6) . . ?
I00D Pb4 I00A 88.82(4) 4_575 . ?
I00D Pb4 I00A 88.82(4) . . ?
I009 Pb4 I00A 93.76(6) . . ?
Sn3 I00E Pb2 176.11(7) 1_455 . ?
I00I Sn1 I008 85.48(7) . . ?
I00C Sn3 I006 90.56(7) . . ?
I00C Sn3 I00E 91.26(4) . 1_655 ?
I006 Sn3 I00E 89.35(4) . 1_655 ?
I00C Sn3 I00E 91.26(4) . 4_675 ?
I006 Sn3 I00E 89.35(4) . 4_675 ?
I00E Sn3 I00E 177.17(8) 1_655 4_675 ?
C4P N1P C3P 115(3) . . ?
C4P N1P H1P1 123.2 . . ?
C3P N1P H1P1 121.3 . . ?
C6P N2P H2P1 109.8 . . ?
C6P N2P H2P2 110.0 . . ?
H2P1 N2P H2P2 109.5 . . ?
C6P N2P H2P3 108.6 . . ?
H2P1 N2P H2P3 109.5 . . ?
H2P2 N2P H2P3 109.5 . . ?
C2P C1P C5P 118(3) . . ?
C2P C1P H1P 120.8 . . ?
C5P C1P H1P 120.8 . . ?
C1P C2P C3P 119(3) . . ?
C1P C2P H2P 120.5 . . ?
C3P C2P H2P 120.6 . . ?
N1P C3P C2P 121(3) . . ?
N1P C3P H3P 119.6 . . ?
C2P C3P H3P 119.6 . . ?
C5P C4P N1P 126(3) . . ?
C5P C4P H4P 117.1 . . ?
N1P C4P H4P 117.0 . . ?
C4P C5P C1P 120(3) . . ?
C4P C5P C6P 122(2) . . ?
C1P C5P C6P 118(2) . . ?
N2P C6P C5P 107(2) . . ?
N2P C6P H6PA 110.4 . . ?
C5P C6P H6PA 110.4 . . ?
N2P C6P H6PB 110.4 . . ?
C5P C6P H6PB 110.4 . . ?
H6PA C6P H6PB 108.6 . . ?
C8P N3P C9P 124(3) . . ?
C8P N3P H3P1 119.6 . . ?
C9P N3P H3P1 115.9 . . ?
C12P N4P H4P1 111.1 . . ?
C12P N4P H4P2 110.1 . . ?
H4P1 N4P H4P2 109.5 . . ?
C12P N4P H4P3 107.2 . . ?
H4P1 N4P H4P3 109.5 . . ?
H4P2 N4P H4P3 109.5 . . ?
C8P C7P C11P 118(2) . . ?
C8P C7P C12P 121(2) . . ?
C11P C7P C12P 121(2) . . ?
N3P C8P C7P 122(3) . . ?
N3P C8P H8P 119.2 . . ?
C7P C8P H8P 119.2 . . ?
N3P C9P C10P 115(3) . . ?
N3P C9P H9P 122.6 . . ?
C10P C9P H9P 122.7 . . ?
C11P C10P C9P 116(3) . . ?
C11P C10P H10P 122.0 . . ?
C9P C10P H10P 122.0 . . ?
C10P C11P C7P 125(2) . . ?
C10P C11P H11P 117.4 . . ?
C7P C11P H11P 117.4 . . ?
N4P C12P C7P 108(2) . . ?
N4P C12P H12A 110.2 . . ?
C7P C12P H12A 110.2 . . ?
N4P C12P H12B 110.1 . . ?
C7P C12P H12B 110.1 . . ?
H12A C12P H12B 108.5 . . ?

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
C5P C1P C2P C3P -5(3) . . . . ?
C4P N1P C3P C2P -7(4) . . . . ?
C1P C2P C3P N1P 7(4) . . . . ?
C3P N1P C4P C5P 7(4) . . . . ?
N1P C4P C5P C1P -6(4) . . . . ?
N1P C4P C5P C6P 173(2) . . . . ?
C2P C1P C5P C4P 4(3) . . . . ?
C2P C1P C5P C6P -175(2) . . . . ?
C4P C5P C6P N2P 111(3) . . . . ?
C1P C5P C6P N2P -70(3) . . . . ?
C9P N3P C8P C7P -3(5) . . . . ?
C11P C7P C8P N3P 1(4) . . . . ?
C12P C7P C8P N3P 179(3) . . . . ?
C8P N3P C9P C10P 2(5) . . . . ?
N3P C9P C10P C11P 1(4) . . . . ?
C9P C10P C11P C7P -4(3) . . . . ?
C8P C7P C11P C10P 3(3) . . . . ?
C12P C7P C11P C10P -176(2) . . . . ?
C8P C7P C12P N4P 73(3) . . . . ?
C11P C7P C12P N4P -108(2) . . . . ?

_refine_diff_density_max         15.272
_refine_diff_density_min         -9.613
_refine_diff_density_rms         0.704

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3apsni3_1_b_pl
_database_code_depnum_ccdc_archive 'CCDC 2192959'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2022-07-27 deposited with the CCDC.	2023-10-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H10 I4 N2 Sn'
_chemical_formula_weight         736.45

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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4611 1.7922 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0064 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6597 1.4093 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   9.4960(19)
_cell_length_b                   12.830(3)
_cell_length_c                   24.979(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3043.3(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    59275
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       plate
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.215
_exptl_crystal_F_000             2576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    9.250
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34636
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.606
_diffrn_reflns_theta_max         33.580
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             5553
_reflns_number_gt                4559
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0769P)²+2.1118P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5553
_refine_ls_number_parameters     130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1324
_refine_ls_wR_factor_gt          0.1285
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
I1I I 0.92356(6) 0.750000 0.27307(2) 0.05346(14) Uani 1 2 d S T P . .
I2I I 0.99490(5) 0.750000 0.09292(2) 0.05145(13) Uani 1 2 d S T P . .
I3I I 0.57878(5) 0.750000 0.05249(2) 0.04191(11) Uani 1 2 d S T P . .
I4I I 0.70005(5) 0.50005(2) 0.16041(2) 0.05081(12) Uani 1 1 d . . . . .
I5I I 1.01618(5) 0.250000 0.22064(2) 0.04899(13) Uani 1 2 d S T P . .
I6I I 0.81697(5) 0.250000 0.05273(2) 0.04102(11) Uani 1 2 d S T P . .
I7I I 0.40614(5) 0.250000 0.11371(2) 0.05018(13) Uani 1 2 d S T P . .
Sn3I Sn 0.72895(4) 0.750000 0.15754(2) 0.02881(9) Uani 1 2 d S T P . .
C3I C 0.3104(8) -0.0461(7) 0.0348(3) 0.077(2) Uani 1 1 d . . . . .
H3I H 0.376503 -0.085694 0.016264 0.092 Uiso 1 1 calc R U . . .
Sn4I Sn 0.69051(4) 0.250000 0.16072(2) 0.02924(10) Uani 1 2 d S T P . .
C4I C 0.2256(9) 0.0240(8) 0.0074(3) 0.089(3) Uani 1 1 d . . . . .
H4I H 0.235771 0.032560 -0.029355 0.107 Uiso 1 1 calc R U . . .
N1I N 0.3022(7) 0.0288(5) 0.2029(2) 0.0694(14) Uani 1 1 d . . . . .
H1I1 H 0.292396 0.019881 0.238029 0.104 Uiso 1 1 calc R U . . .
H1I2 H 0.381103 -0.002076 0.191976 0.104 Uiso 1 1 calc R U . . .
H1I3 H 0.306426 0.096560 0.195535 0.104 Uiso 1 1 calc R U . . .
C1I C 0.1992(6) -0.0020(3) 0.1152(3) 0.0477(12) Uani 1 1 d . . . . .
C2I C 0.2976(7) -0.0563(5) 0.0857(3) 0.0653(17) Uani 1 1 d . . . . .
H2I H 0.357257 -0.102254 0.103477 0.078 Uiso 1 1 calc R U . . .
N5I N 0.1275(7) 0.0800(4) 0.0347(2) 0.0714(17) Uani 1 1 d . . . . .
H7I H 0.074138 0.123469 0.018100 0.086 Uiso 1 1 calc R U . . .
C6I C 0.1830(8) -0.0169(5) 0.1755(3) 0.0593(14) Uani 1 1 d . . . . .
H6IA H 0.096691 0.015955 0.187535 0.071 Uiso 1 1 calc R U . . .
H6IB H 0.177437 -0.090697 0.183686 0.071 Uiso 1 1 calc R U . . .
C5I C 0.1149(6) 0.0666(4) 0.0882(2) 0.0535(12) Uani 1 1 d . . . . .
H5I H 0.047670 0.104634 0.106991 0.064 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
I2I Sn3I 2.9973(7) . ?
I3I Sn3I 2.9865(7) . ?
I4I Sn4I 3.2094(8) . ?
I4I Sn3I 3.2194(8) . ?
I6I Sn4I 2.9528(7) . ?
I7I Sn4I 2.9447(8) . ?
C3I C2I 1.285(11) . ?
C3I C4I 1.387(14) . ?
C3I H3I 0.9300 . ?
C4I N5I 1.359(11) . ?
C4I H4I 0.9300 . ?
N1I C6I 1.447(10) . ?
N1I H1I1 0.8900 . ?
N1I H1I2 0.8900 . ?
N1I H1I3 0.8900 . ?
C1I C5I 1.367(7) . ?
C1I C2I 1.379(8) . ?
C1I C6I 1.525(9) . ?
C2I H2I 0.9300 . ?
N5I C5I 1.354(8) . ?
N5I H7I 0.8600 . ?
C6I H6IA 0.9700 . ?
C6I H6IB 0.9700 . ?
C5I H5I 0.9300 . ?

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
Sn4I I4I Sn3I 176.537(18) . . ?
I3I Sn3I I2I 85.94(2) . . ?
I3I Sn3I I4I 88.789(9) . 8_575 ?
I2I Sn3I I4I 94.807(10) . 8_575 ?
I3I Sn3I I4I 88.788(9) . . ?
I2I Sn3I I4I 94.807(10) . . ?
I4I Sn3I I4I 169.89(2) 8_575 . ?
C2I C3I C4I 119.9(7) . . ?
C2I C3I H3I 120.0 . . ?
C4I C3I H3I 120.0 . . ?
I7I Sn4I I6I 90.49(2) . . ?
I7I Sn4I I4I 91.429(10) . . ?
I6I Sn4I I4I 89.214(9) . . ?
I7I Sn4I I4I 91.429(10) . 8_565 ?
I6I Sn4I I4I 89.214(9) . 8_565 ?
I4I Sn4I I4I 176.75(2) . 8_565 ?
N5I C4I C3I 119.6(7) . . ?
N5I C4I H4I 120.2 . . ?
C3I C4I H4I 120.2 . . ?
C6I N1I H1I1 109.5 . . ?
C6I N1I H1I2 109.5 . . ?
H1I1 N1I H1I2 109.5 . . ?
C6I N1I H1I3 109.5 . . ?
H1I1 N1I H1I3 109.5 . . ?
H1I2 N1I H1I3 109.5 . . ?
C5I C1I C2I 117.3(6) . . ?
C5I C1I C6I 120.6(5) . . ?
C2I C1I C6I 122.1(6) . . ?
C3I C2I C1I 122.8(7) . . ?
C3I C2I H2I 118.6 . . ?
C1I C2I H2I 118.6 . . ?
C5I N5I C4I 119.2(6) . . ?
C5I N5I H7I 120.4 . . ?
C4I N5I H7I 120.4 . . ?
N1I C6I C1I 109.7(6) . . ?
N1I C6I H6IA 109.7 . . ?
C1I C6I H6IA 109.7 . . ?
N1I C6I H6IB 109.7 . . ?
C1I C6I H6IB 109.7 . . ?
H6IA C6I H6IB 108.2 . . ?
N5I C5I C1I 121.1(6) . . ?
N5I C5I H5I 119.4 . . ?
C1I C5I H5I 119.4 . . ?

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
C2I C3I C4I N5I -1.2(11) . . . . ?
C4I C3I C2I C1I 1.8(11) . . . . ?
C5I C1I C2I C3I -1.3(9) . . . . ?
C6I C1I C2I C3I 178.5(6) . . . . ?
C3I C4I N5I C5I 0.3(10) . . . . ?
C5I C1I C6I N1I -108.6(6) . . . . ?
C2I C1I C6I N1I 71.5(7) . . . . ?
C4I N5I C5I C1I 0.2(9) . . . . ?
C2I C1I C5I N5I 0.3(8) . . . . ?
C6I C1I C5I N5I -179.5(6) . . . . ?

_refine_diff_density_max         1.366
_refine_diff_density_min         -2.733
_refine_diff_density_rms         0.405

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_43apfapbsn_1_a_pl
_database_code_depnum_ccdc_archive 'CCDC 2192961'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2022-07-27 deposited with the CCDC.	2023-10-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H10 I7 N4 Pb Sn'
_chemical_formula_weight         1364.37

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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4611 1.7922 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0064 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.1439 9.9644 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6597 1.4093 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.215(3)
_cell_length_b                   18.204(4)
_cell_length_c                   8.7630(18)
_cell_angle_alpha                90
_cell_angle_beta                 97.13(3)
_cell_angle_gamma                90
_cell_volume                     2566.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    47372
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       plate
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.531
_exptl_crystal_F_000             2332
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    15.155
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25596
_diffrn_reflns_av_unetI/netI     0.1623
_diffrn_reflns_av_R_equivalents  0.1648
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.246
_diffrn_reflns_theta_max         32.933
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.778
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.778
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.778
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             7841
_reflns_number_gt                3018
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7841
_refine_ls_number_parameters     181
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.2407
_refine_ls_R_factor_gt           0.1271
_refine_ls_wR_factor_ref         0.3969
_refine_ls_wR_factor_gt          0.3559
_refine_ls_goodness_of_fit_ref   1.652
_refine_ls_restrained_S_all      1.653
_refine_ls_shift/su_max          0.414
_refine_ls_shift/su_mean         0.027

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 0.19051(10) 0.62639(7) 0.78705(15) 0.0632(5) Uani 1 1 d . . . . .
I0I I -0.00694(13) 0.61403(16) 0.7428(3) 0.0780(9) Uani 1 1 d . . . . .
I005 I -0.39775(13) 0.62763(11) 0.6717(3) 0.0565(6) Uani 1 1 d . . . . .
I007 I 0.21126(15) 0.50448(12) 1.0469(2) 0.0616(7) Uani 1 1 d . . . . .
I009 I 0.38127(13) 0.65982(12) 0.8546(3) 0.0617(7) Uani 1 1 d . . . . .
I00B I -0.21006(17) 0.75011(13) 0.9545(3) 0.0723(8) Uani 1 1 d . . . . .
I00C I 0.17264(18) 0.75510(13) 1.0234(3) 0.0710(8) Uani 1 1 d . . . . .
I00D I 0.21935(17) 0.50659(13) 0.5400(3) 0.0738(8) Uani 1 1 d . . . . .
Sn3 Sn -0.21014(9) 0.62276(8) 0.69988(16) 0.0201(3) Uani 1 1 d . . . . .
N3 N 0.4104(18) 0.1748(19) 0.320(3) 0.077(10) Uani 1 1 d . . . . .
H3A H 0.388116 0.215122 0.346157 0.092 Uiso 1 1 calc R U . . .
N5R N 0.669(2) 0.161(3) 0.241(5) 0.17(2) Uani 1 1 d D . . . .
H5R1 H 0.708981 0.151808 0.181851 0.251 Uiso 1 1 calc R U . . .
H5R2 H 0.659747 0.208845 0.243318 0.251 Uiso 1 1 calc R U . . .
H5R3 H 0.685475 0.144689 0.335907 0.251 Uiso 1 1 calc R U . . .
C2 C 0.515(2) 0.113(2) 0.207(5) 0.074(11) Uani 1 1 d . . . . .
C3 C 0.473(3) 0.0503(17) 0.288(4) 0.087(14) Uani 1 1 d . . . . .
H3 H 0.498040 0.004363 0.286051 0.105 Uiso 1 1 calc R U . . .
C4 C 0.411(2) 0.054(2) 0.356(3) 0.062(10) Uani 1 1 d . . . . .
H4 H 0.389194 0.013318 0.403613 0.074 Uiso 1 1 calc R U . . .
C5 C 0.379(2) 0.1174(15) 0.355(3) 0.047(8) Uani 1 1 d . . . . .
H5 H 0.325571 0.120669 0.382659 0.056 Uiso 1 1 calc R U . . .
C6 C 0.470(2) 0.1790(17) 0.253(4) 0.076(12) Uani 1 1 d . . . . .
H6 H 0.489716 0.225135 0.229759 0.091 Uiso 1 1 calc R U . . .
C7 C 0.594(3) 0.123(3) 0.179(10) 0.24(4) Uani 1 1 d D U . . .
H7A H 0.585641 0.140593 0.073407 0.291 Uiso 1 1 calc R U . . .
H7AB H 0.612836 0.072781 0.171274 0.291 Uiso 1 1 calc R U . . .
N1 N -0.016(4) 0.075(3) 0.355(7) 0.48(10) Uani 1 1 d D . . . .
N2 N -0.028(4) 0.177(4) 0.166(9) 0.43(8) Uani 1 1 d D . . . .
C1 C 0.024(4) 0.122(3) 0.251(5) 0.11(2) Uani 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 I009 3.136(3) . ?
Pb1 I00C 3.148(2) 4_575 ?
Pb1 I00D 3.149(2) . ?
Pb1 I00C 3.164(2) . ?
Pb1 I007 3.168(2) . ?
Pb1 I0I 3.185(3) . ?
I005 Sn3 3.023(3) . ?
I007 Sn3 3.209(2) 3_567 ?
I00B Sn3 3.159(2) 4_576 ?
I00B Sn3 3.217(2) . ?
I00D Sn3 3.147(2) 3_566 ?
N3 C6 1.20(4) . ?
N3 C5 1.22(4) . ?
N3 H3A 0.8600 . ?
N5R C7 1.454(10) . ?
N5R H5R1 0.8900 . ?
N5R H5R2 0.8900 . ?
N5R H5R3 0.8900 . ?
C2 C7 1.35(6) . ?
C2 C6 1.48(5) . ?
C2 C3 1.54(6) . ?
C3 C4 1.24(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.27(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7AB 0.9700 . ?
N1 C1 1.450(10) . ?
N2 C1 1.452(10) . ?

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
I009 Pb1 I00C 90.25(7) . 4_575 ?
I009 Pb1 I00D 92.13(8) . . ?
I00C Pb1 I00D 88.74(8) 4_575 . ?
I009 Pb1 I00C 84.32(7) . . ?
I00C Pb1 I00C 88.01(4) 4_575 . ?
I00D Pb1 I00C 175.17(8) . . ?
I009 Pb1 I007 89.19(7) . . ?
I00C Pb1 I007 178.47(8) 4_575 . ?
I00D Pb1 I007 89.86(7) . . ?
I00C Pb1 I007 93.35(7) . . ?
I009 Pb1 I0I 171.80(8) . . ?
I00C Pb1 I0I 87.68(8) 4_575 . ?
I00D Pb1 I0I 95.75(8) . . ?
I00C Pb1 I0I 87.69(8) . . ?
I007 Pb1 I0I 93.07(8) . . ?
Pb1 I007 Sn3 173.47(9) . 3_567 ?
Sn3 I00B Sn3 179.01(10) 4_576 . ?
Pb1 I00C Pb1 168.60(10) 4_576 . ?
Sn3 I00D Pb1 168.12(11) 3_566 . ?
I005 Sn3 I00D 90.21(8) . 3_566 ?
I005 Sn3 I00B 90.48(8) . 4_575 ?
I00D Sn3 I00B 95.59(8) 3_566 4_575 ?
I005 Sn3 I007 89.18(7) . 3_567 ?
I00D Sn3 I007 85.29(7) 3_566 3_567 ?
I00B Sn3 I007 179.06(8) 4_575 3_567 ?
I005 Sn3 I00B 87.09(8) . . ?
I00D Sn3 I00B 176.41(9) 3_566 . ?
I00B Sn3 I00B 86.80(4) 4_575 . ?
I007 Sn3 I00B 92.31(7) 3_567 . ?
C6 N3 C5 124(3) . . ?
C6 N3 H3A 117.8 . . ?
C5 N3 H3A 117.8 . . ?
C7 N5R H5R1 110.1 . . ?
C7 N5R H5R2 109.5 . . ?
H5R1 N5R H5R2 109.5 . . ?
C7 N5R H5R3 108.8 . . ?
H5R1 N5R H5R3 109.5 . . ?
H5R2 N5R H5R3 109.5 . . ?
C7 C2 C6 116(4) . . ?
C7 C2 C3 132(4) . . ?
C6 C2 C3 103(3) . . ?
C4 C3 C2 128(4) . . ?
C4 C3 H3 115.9 . . ?
C2 C3 H3 116.0 . . ?
C3 C4 C5 113(4) . . ?
C3 C4 H4 123.4 . . ?
C5 C4 H4 123.5 . . ?
N3 C5 C4 127(4) . . ?
N3 C5 H5 116.3 . . ?
C4 C5 H5 116.3 . . ?
N3 C6 C2 122(3) . . ?
N3 C6 H6 118.9 . . ?
C2 C6 H6 119.0 . . ?
C2 C7 N5R 141(7) . . ?
C2 C7 H7A 101.8 . . ?
N5R C7 H7A 101.5 . . ?
C2 C7 H7AB 102.1 . . ?
N5R C7 H7AB 102.1 . . ?
H7A C7 H7AB 104.8 . . ?
N2 C1 N1 117(5) . . ?

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
C7 C2 C3 C4 153(6) . . . . ?
C6 C2 C3 C4 9(5) . . . . ?
C2 C3 C4 C5 1(6) . . . . ?
C6 N3 C5 C4 16(6) . . . . ?
C3 C4 C5 N3 -14(6) . . . . ?
C5 N3 C6 C2 -1(6) . . . . ?
C7 C2 C6 N3 -159(5) . . . . ?
C3 C2 C6 N3 -9(5) . . . . ?
C6 C2 C7 N5R 43(11) . . . . ?
C3 C2 C7 N5R -97(9) . . . . ?

_refine_diff_density_max         10.628
_refine_diff_density_min         -6.904
_refine_diff_density_rms         1.061

