# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_sm_a
_database_code_depnum_ccdc_archive 'CCDC 1533306'
loop_
_audit_author_name
_audit_author_address
'Mi Hee Jung'
;Sejong University
South Korea
;
_audit_update_record             
;
2018-11-16 deposited with the CCDC.	2020-12-17 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            'C14 H20 I4 N2 Pb'
_chemical_formula_weight         931.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0024 0.0013 '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 0.0048 0.0026 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.6369 1.4867 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -1.8615 8.4434 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   9.126(2)
_cell_length_b                   8.627(2)
_cell_length_c                   28.397(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2235.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    55003
_cell_measurement_theta_min      0.36
_cell_measurement_theta_max      33.54

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.766
_exptl_crystal_F_000             1648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.032
_exptl_absorpt_coefficient_mu    9.453
_shelx_estimated_absorpt_T_min   0.322
_shelx_estimated_absorpt_T_max   0.752
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.630
_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            5565
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.271
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        22.210
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             3018
_reflns_number_gt                2752
_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 2014/5 (Sheldrick, 2014)'
_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)+(0.0428P)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     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.00317(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3018
_refine_ls_number_parameters     99
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0735
_refine_ls_wR_factor_gt          0.0626
_refine_ls_goodness_of_fit_ref   1.287
_refine_ls_restrained_S_all      1.287
_refine_ls_shift/su_max          0.002
_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
C1 C 0.5191(6) 0.5517(5) 0.60637(14) 0.0186(9) Uani 1 1 d . . . . .
H1 H 0.609825 0.554180 0.587277 0.022 Uiso 1 1 calc R U . . .
H00B H 0.472988 0.655421 0.604811 0.022 Uiso 1 1 calc R U . . .
Pb1 Pb 0.000000 0.500000 0.500000 0.00569(8) Uani 1 2 d S . P . .
I1 I 0.04318(3) 0.52163(3) 0.61134(2) 0.01139(9) Uani 1 1 d . . . . .
I2 I 0.20532(3) 0.20142(3) 0.49246(2) 0.00965(9) Uani 1 1 d . . . . .
C2 C 0.5564(5) 0.5138(5) 0.65661(15) 0.0124(8) Uani 1 1 d . . . . .
C3 C 0.6675(5) 0.4102(6) 0.66660(16) 0.0194(9) Uani 1 1 d . . . . .
H00C H 0.718823 0.361290 0.641557 0.023 Uiso 1 1 calc R U . . .
N3 N 0.4156(4) 0.4322(4) 0.58663(11) 0.0138(7) Uani 1 1 d . . . . .
H3A H 0.451102 0.335677 0.592670 0.021 Uiso 1 1 calc R U . . .
H3B H 0.407208 0.445738 0.554968 0.021 Uiso 1 1 calc R U . . .
H3C H 0.326089 0.443128 0.600335 0.021 Uiso 1 1 calc R U . . .
C4 C 0.7050(5) 0.3768(6) 0.71285(17) 0.0252(10) Uani 1 1 d . . . . .
H4 H 0.780962 0.304777 0.719468 0.030 Uiso 1 1 calc R U . . .
C6 C 0.5190(5) 0.5522(6) 0.74008(16) 0.0198(9) Uani 1 1 d . . . . .
H6 H 0.467872 0.600846 0.765202 0.024 Uiso 1 1 calc R U . . .
C5 C 0.6308(6) 0.4495(6) 0.74945(16) 0.0229(10) Uani 1 1 d . . . . .
H5 H 0.657324 0.428132 0.781143 0.028 Uiso 1 1 calc R U . . .
C7 C 0.4814(5) 0.5843(6) 0.69363(15) 0.0178(9) Uani 1 1 d . . . . .
H7 H 0.404005 0.654762 0.687086 0.021 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
C1 C2 1.503(6) . ?
C1 N3 1.506(6) . ?
C1 H1 0.9900 . ?
C1 H00B 0.9900 . ?
Pb1 I1 3.1917(3) 5_566 ?
Pb1 I1 3.1918(3) . ?
Pb1 I2 3.1924(6) 5_566 ?
Pb1 I2 3.1924(6) . ?
Pb1 I2 3.2090(6) 8_665 ?
Pb1 I2 3.2090(6) 4_456 ?
C2 C3 1.382(6) . ?
C2 C7 1.394(6) . ?
C3 C4 1.387(6) . ?
C3 H00C 0.9500 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
C4 C5 1.390(7) . ?
C4 H4 0.9500 . ?
C6 C5 1.377(7) . ?
C6 C7 1.391(6) . ?
C6 H6 0.9500 . ?
C5 H5 0.9500 . ?
C7 H7 0.9500 . ?

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
C2 C1 N3 110.3(4) . . ?
C2 C1 H1 109.6 . . ?
N3 C1 H1 109.6 . . ?
C2 C1 H00B 109.6 . . ?
N3 C1 H00B 109.6 . . ?
H1 C1 H00B 108.1 . . ?
I1 Pb1 I1 180.0 5_566 . ?
I1 Pb1 I2 92.361(7) 5_566 5_566 ?
I1 Pb1 I2 87.640(7) . 5_566 ?
I1 Pb1 I2 87.640(7) 5_566 . ?
I1 Pb1 I2 92.360(7) . . ?
I2 Pb1 I2 180.0 5_566 . ?
I1 Pb1 I2 93.956(7) 5_566 8_665 ?
I1 Pb1 I2 86.044(7) . 8_665 ?
I2 Pb1 I2 93.407(17) 5_566 8_665 ?
I2 Pb1 I2 86.593(17) . 8_665 ?
I1 Pb1 I2 86.044(8) 5_566 4_456 ?
I1 Pb1 I2 93.956(7) . 4_456 ?
I2 Pb1 I2 86.593(17) 5_566 4_456 ?
I2 Pb1 I2 93.408(17) . 4_456 ?
I2 Pb1 I2 180.0 8_665 4_456 ?
Pb1 I2 Pb1 157.564(9) . 4_556 ?
C3 C2 C7 119.2(4) . . ?
C3 C2 C1 120.1(4) . . ?
C7 C2 C1 120.7(4) . . ?
C2 C3 C4 120.6(4) . . ?
C2 C3 H00C 119.7 . . ?
C4 C3 H00C 119.7 . . ?
C1 N3 H3A 109.5 . . ?
C1 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C1 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C3 C4 C5 119.6(4) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C5 C6 C7 119.6(4) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C6 C5 C4 120.4(4) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C6 C7 C2 120.5(4) . . ?
C6 C7 H7 119.8 . . ?
C2 C7 H7 119.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3A I1 0.91 2.76 3.631(4) 160.2 8_655 yes
N3 H3B I2 0.91 3.31 3.847(3) 119.7 . yes
N3 H3B I2 0.91 3.01 3.710(3) 134.8 8_665 yes
N3 H3C I1 0.91 2.69 3.555(4) 159.8 . yes

_refine_diff_density_max         6.426
_refine_diff_density_min         -2.073
_refine_diff_density_rms         0.631

####################################################################### 
# 
# 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_GA2PbI4_a
_database_code_depnum_ccdc_archive 'CCDC 1879307'
loop_
_audit_author_name
_audit_author_address
'Mi Hee Jung'
;Sejong University
South Korea
;
_audit_update_record             
;
2018-11-16 deposited with the CCDC.	2020-12-17 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            'C2 H12 I4 N6 Pb'
_chemical_formula_weight         834.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4371 1.8409 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.4194 10.2008 '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/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.3165(11)
_cell_length_b                   27.144(3)
_cell_length_c                   12.8713(14)
_cell_angle_alpha                90
_cell_angle_beta                 90.699(5)
_cell_angle_gamma                90
_cell_volume                     3254.8(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    78464
_cell_measurement_theta_min      2.6535
_cell_measurement_theta_max      28.334

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.408
_exptl_crystal_F_000             2880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    17.766
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            75975
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.500
_diffrn_reflns_theta_max         28.381
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8125
_reflns_number_gt                6680
_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       'Bruker SMART APEXll'
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0733P)²+40.3576P] 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       0.00154(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8125
_refine_ls_number_parameters     237
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0473
_refine_ls_wR_factor_ref         0.1556
_refine_ls_wR_factor_gt          0.1443
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.109
_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 0.24294(4) 0.41096(2) 0.75469(3) 0.03576(13) Uani 1 1 d . . . . .
N1 N 0.5895(12) 0.4355(6) 1.0009(9) 0.078(4) Uani 1 1 d . . . . .
H1A H 0.542394 0.438024 0.943267 0.093 Uiso 1 1 calc R U . . .
H1B H 0.544363 0.433861 1.058669 0.093 Uiso 1 1 calc R U . . .
C1 C 0.2347(15) 0.5816(5) 0.4802(13) 0.058(3) Uani 1 1 d . . . . .
I1 I 0.50566(11) 0.34131(4) 0.21991(9) 0.0646(3) Uani 1 1 d . . . . .
Pb2 Pb 0.25022(4) 0.41496(2) 0.25644(3) 0.03530(13) Uani 1 1 d . . . . .
N2 N 0.7968(14) 0.4299(5) 1.0890(10) 0.074(4) Uani 1 1 d . . . . .
H2A H 0.750043 0.427972 1.146091 0.089 Uiso 1 1 calc R U . . .
H2B H 0.889085 0.429039 1.090218 0.089 Uiso 1 1 calc R U . . .
C2 C 0.7277(12) 0.4343(5) 1.0007(8) 0.042(3) Uani 1 1 d . . . . .
I2 I 0.02150(10) 0.33248(3) 0.25938(7) 0.0520(2) Uani 1 1 d . . . . .
I3 I -0.00030(8) 0.49863(3) 0.29137(6) 0.0457(2) Uani 1 1 d . . . . .
N3 N 0.7996(13) 0.4367(5) 0.9150(9) 0.066(3) Uani 1 1 d . . . . .
H3A H 0.754961 0.439201 0.856353 0.079 Uiso 1 1 calc R U . . .
H3B H 0.891895 0.435775 0.916876 0.079 Uiso 1 1 calc R U . . .
C3 C 0.1991(18) 0.2423(6) 0.9983(11) 0.062(3) Uani 1 1 d . . . . .
I4 I 0.30109(9) 0.39769(3) 0.50425(5) 0.0487(2) Uani 1 1 d . . . . .
N4 N 0.252(2) 0.2820(10) 1.0326(19) 0.151(9) Uani 1 1 d . U . . .
H4A H 0.314874 0.297551 0.997176 0.182 Uiso 1 1 calc R U . . .
H4B H 0.224146 0.293516 1.091287 0.182 Uiso 1 1 calc R U . . .
C4 C -0.228(2) 0.2682(6) 0.9867(14) 0.074(5) Uani 1 1 d . . . . .
I5 I 0.47567(10) 0.33297(3) 0.79779(8) 0.0540(2) Uani 1 1 d . . . . .
N5 N 0.238(3) 0.2261(10) 0.915(2) 0.180(12) Uani 1 1 d . . . . .
H5A H 0.207118 0.198018 0.893465 0.216 Uiso 1 1 calc R U . . .
H5B H 0.297145 0.242701 0.877899 0.216 Uiso 1 1 calc R U . . .
I6 I 0.19305(9) 0.42446(4) 1.00281(5) 0.0499(2) Uani 1 1 d . . . . .
N6 N 0.113(3) 0.2189(11) 1.054(2) 0.176(10) Uani 1 1 d . U . . .
H6A H 0.080624 0.190768 1.034424 0.212 Uiso 1 1 calc R U . . .
H6B H 0.086958 0.231042 1.112954 0.212 Uiso 1 1 calc R U . . .
I009 I 0.00234(10) 0.33074(3) 0.73765(8) 0.0552(2) Uani 1 1 d . . . . .
N9 N -0.1971(18) 0.2437(6) 0.9043(11) 0.092(5) Uani 1 1 d . . . . .
H9A H -0.146909 0.257115 0.856368 0.111 Uiso 1 1 calc R U . . .
H9B H -0.226677 0.213828 0.897209 0.111 Uiso 1 1 calc R U . . .
N8 N -0.185(2) 0.3118(6) 0.9975(13) 0.099(5) Uani 1 1 d . U . . .
H8A H -0.134835 0.325360 0.949701 0.119 Uiso 1 1 calc R U . . .
H8B H -0.205860 0.328064 1.052601 0.119 Uiso 1 1 calc R U . . .
I7 I 0.49870(8) 0.49604(3) 0.74660(6) 0.0448(2) Uani 1 1 d . . . . .
N7 N -0.293(3) 0.2446(11) 1.060(2) 0.169(10) Uani 1 1 d . U . . .
H7A H -0.308307 0.258696 1.118278 0.203 Uiso 1 1 calc R U . . .
H7B H -0.320874 0.214744 1.049472 0.203 Uiso 1 1 calc R U . . .
N11 N 0.304(2) 0.5491(7) 0.5216(14) 0.109(6) Uani 1 1 d . U . . .
H11A H 0.266068 0.531088 0.568778 0.131 Uiso 1 1 calc R U . . .
H11B H 0.391731 0.544104 0.503801 0.131 Uiso 1 1 calc R U . . .
N12 N 0.2937(15) 0.6031(6) 0.3953(13) 0.089(5) Uani 1 1 d . . . . .
H12A H 0.376103 0.593472 0.373739 0.106 Uiso 1 1 calc R U . . .
H12B H 0.248666 0.626312 0.363165 0.106 Uiso 1 1 calc R U . . .
N10 N 0.1044(14) 0.5921(6) 0.5008(10) 0.076(4) Uani 1 1 d . . . . .
H10A H 0.059531 0.575530 0.547239 0.091 Uiso 1 1 calc R U . . .
H10B H 0.061615 0.615664 0.468346 0.091 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 I5 3.0760(9) . ?
Pb1 I009 3.1309(10) . ?
Pb1 I6 3.2536(8) . ?
Pb1 I4 3.2950(8) . ?
Pb1 I7 3.3208(9) . ?
Pb1 I3 3.3840(9) 3_566 ?
N1 C2 1.288(15) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
C1 N11 1.22(2) . ?
C1 N10 1.277(18) . ?
C1 N12 1.36(2) . ?
I1 Pb2 3.1478(10) . ?
Pb2 I2 3.0912(9) . ?
Pb2 I4 3.2528(8) . ?
Pb2 I3 3.2913(9) . ?
Pb2 I6 3.3115(9) 1_554 ?
Pb2 I7 3.3634(9) 3_666 ?
N2 C2 1.305(15) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
C2 N3 1.299(15) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
C3 N5 1.22(2) . ?
C3 N6 1.26(3) . ?
C3 N4 1.26(3) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
C4 N8 1.26(2) . ?
C4 N9 1.29(2) . ?
C4 N7 1.29(3) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
N9 H9A 0.8600 . ?
N9 H9B 0.8600 . ?
N8 H8A 0.8600 . ?
N8 H8B 0.8600 . ?
N7 H7A 0.8600 . ?
N7 H7B 0.8600 . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?

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
I5 Pb1 I009 92.08(3) . . ?
I5 Pb1 I6 90.53(3) . . ?
I009 Pb1 I6 92.08(3) . . ?
I5 Pb1 I4 88.70(3) . . ?
I009 Pb1 I4 88.94(3) . . ?
I6 Pb1 I4 178.74(2) . . ?
I5 Pb1 I7 88.85(3) . . ?
I009 Pb1 I7 174.19(3) . . ?
I6 Pb1 I7 93.65(2) . . ?
I4 Pb1 I7 85.34(2) . . ?
I5 Pb1 I3 177.00(3) . 3_566 ?
I009 Pb1 I3 90.92(3) . 3_566 ?
I6 Pb1 I3 89.26(2) . 3_566 ?
I4 Pb1 I3 91.45(2) . 3_566 ?
I7 Pb1 I3 88.18(2) . 3_566 ?
C2 N1 H1A 120.0 . . ?
C2 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
N11 C1 N10 125.0(18) . . ?
N11 C1 N12 116.4(16) . . ?
N10 C1 N12 117.8(14) . . ?
I2 Pb2 I1 93.69(3) . . ?
I2 Pb2 I4 88.62(3) . . ?
I1 Pb2 I4 87.34(3) . . ?
I2 Pb2 I3 90.46(3) . . ?
I1 Pb2 I3 175.79(3) . . ?
I4 Pb2 I3 93.47(2) . . ?
I2 Pb2 I6 88.04(3) . 1_554 ?
I1 Pb2 I6 90.86(3) . 1_554 ?
I4 Pb2 I6 176.10(3) . 1_554 ?
I3 Pb2 I6 88.57(2) . 1_554 ?
I2 Pb2 I7 179.51(3) . 3_666 ?
I1 Pb2 I7 85.83(3) . 3_666 ?
I4 Pb2 I7 91.26(2) . 3_666 ?
I3 Pb2 I7 90.02(2) . 3_666 ?
I6 Pb2 I7 92.07(2) 1_554 3_666 ?
C2 N2 H2A 120.0 . . ?
C2 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
N1 C2 N3 121.8(12) . . ?
N1 C2 N2 118.9(12) . . ?
N3 C2 N2 119.4(12) . . ?
Pb2 I3 Pb1 161.76(3) . 3_566 ?
C2 N3 H3A 120.0 . . ?
C2 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
N5 C3 N6 122(2) . . ?
N5 C3 N4 120(2) . . ?
N6 C3 N4 118(2) . . ?
Pb2 I4 Pb1 156.90(3) . . ?
C3 N4 H4A 120.0 . . ?
C3 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
N8 C4 N9 120.3(17) . . ?
N8 C4 N7 123(2) . . ?
N9 C4 N7 117(2) . . ?
C3 N5 H5A 120.0 . . ?
C3 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
Pb1 I6 Pb2 159.35(3) . 1_556 ?
C3 N6 H6A 120.0 . . ?
C3 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C4 N9 H9A 120.0 . . ?
C4 N9 H9B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
C4 N8 H8A 120.0 . . ?
C4 N8 H8B 120.0 . . ?
H8A N8 H8B 120.0 . . ?
Pb1 I7 Pb2 177.85(3) . 3_666 ?
C4 N7 H7A 120.0 . . ?
C4 N7 H7B 120.0 . . ?
H7A N7 H7B 120.0 . . ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12A 120.0 . . ?
C1 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
C1 N10 H10A 120.0 . . ?
C1 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?

_refine_diff_density_max         2.910
_refine_diff_density_min         -1.745
_refine_diff_density_rms         0.340

####################################################################### 
# 
# 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_ImPbI3_1_a
_database_code_depnum_ccdc_archive 'CCDC 1879318'
loop_
_audit_author_name
_audit_author_address
'Mi Hee Jung'
;Sejong University
South Korea
;
_audit_update_record             
;
2018-11-16 deposited with the CCDC.	2020-12-17 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 H0 I7 N4 Pb2'
_chemical_formula_weight         1430.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4371 1.8409 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.4194 10.2008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   45.458(4)
_cell_length_b                   8.9432(8)
_cell_length_c                   8.8219(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.251(6)
_cell_angle_gamma                90
_cell_volume                     3549.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    15300
_cell_measurement_theta_min      2.7165
_cell_measurement_theta_max      21.261

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.678
_exptl_crystal_F_000             2396
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    15.415
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14499
_diffrn_reflns_av_unetI/netI     0.0978
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         0.905
_diffrn_reflns_theta_max         28.303
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4395
_reflns_number_gt                2431
_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       'Bruker SMART APEXll'
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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)+(0.1817P)²+46.7176P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.00081(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4395
_refine_ls_number_parameters     73
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1560
_refine_ls_R_factor_gt           0.0983
_refine_ls_wR_factor_ref         0.3364
_refine_ls_wR_factor_gt          0.2940
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          2.909
_refine_ls_shift/su_mean         0.190

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 0.42746(2) 0.25114(8) 0.69839(9) 0.0416(4) Uani 1 1 d . . . . .
N1 N 0.30098(2) 0.31904(8) 1.08128(9) 0.9(2) Uani 1 1 d R U . . .
C1 C 0.32903(2) 0.25018(8) 1.12611(9) 0.16(2) Uani 1 1 d R U . . .
N2 N 0.33683(2) 0.17177(8) 0.99769(9) 1.4(5) Uani 1 1 d R U . . .
C2 C 0.31360(2) 0.19217(8) 0.87349(9) 2.0(9) Uani 1 1 d R U . . .
C3 C 0.29145(2) 0.28319(8) 0.92515(9) 2.0(9) Uani 1 1 d R U . . .
I1 I 0.35835(5) 0.2113(3) 0.6660(3) 0.0775(7) Uani 1 1 d . . . . .
I2 I 0.42723(5) 0.5414(2) 0.4901(2) 0.0832(8) Uani 1 1 d . . . . .
I3 I 0.500000 0.2616(3) 0.750000 0.0679(8) Uani 1 2 d S T P . .
I4 I 0.43243(5) -0.0414(2) 0.9095(2) 0.0676(7) Uani 1 1 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 I1 3.134(2) . ?
Pb1 I2 3.1739(17) 6_566 ?
Pb1 I2 3.1795(18) . ?
Pb1 I4 3.1985(17) 6 ?
Pb1 I4 3.2005(17) . ?
Pb1 I3 3.2647(10) . ?
N1 C3 1.4200 . ?
N1 C1 1.4200 . ?
C1 N2 1.4200 . ?
N2 C2 1.4200 . ?
C2 C3 1.4200 . ?

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 I2 91.17(6) . 6_566 ?
I1 Pb1 I2 96.88(7) . . ?
I2 Pb1 I2 89.50(2) 6_566 . ?
I1 Pb1 I4 92.59(6) . 6 ?
I2 Pb1 I4 176.18(6) 6_566 6 ?
I2 Pb1 I4 90.74(5) . 6 ?
I1 Pb1 I4 86.92(6) . . ?
I2 Pb1 I4 90.82(5) 6_566 . ?
I2 Pb1 I4 176.18(6) . . ?
I4 Pb1 I4 88.69(2) 6 . ?
I1 Pb1 I3 174.41(6) . . ?
I2 Pb1 I3 89.49(6) 6_566 . ?
I2 Pb1 I3 88.67(6) . . ?
I4 Pb1 I3 86.71(5) 6 . ?
I4 Pb1 I3 87.52(6) . . ?
C3 N1 C1 108.0 . . ?
N2 C1 N1 108.0 . . ?
C1 N2 C2 108.0 . . ?
C3 C2 N2 108.0 . . ?
C2 C3 N1 108.0 . . ?
Pb1 I2 Pb1 161.04(9) 6_565 . ?
Pb1 I3 Pb1 176.71(10) . 2_656 ?
Pb1 I4 Pb1 159.37(8) 6_556 . ?

_refine_diff_density_max         5.336
_refine_diff_density_min         -2.677
_refine_diff_density_rms         1.025

####################################################################### 
# 
# 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_No2
_database_code_depnum_ccdc_archive 'CCDC 1879306'
loop_
_audit_author_name
_audit_author_address
'Mi Hee Jung'
;Sejong University
South Korea
;
_audit_update_record             
;
2018-11-16 deposited with the CCDC.	2020-12-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 I4 N2 Pb'
_chemical_formula_weight         934.97

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'
N N 0.0061 0.0033 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   32.5719(16)
_cell_length_b                   6.1388(3)
_cell_length_c                   6.1894(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.6350(19)
_cell_angle_gamma                90
_cell_volume                     1235.10(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    9151
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      28.35

_exptl_crystal_description       Plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.514
_exptl_crystal_F_000             808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    11.828
_shelx_estimated_absorpt_T_min   0.164
_shelx_estimated_absorpt_T_max   0.331
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.073
_exptl_absorpt_correction_T_max  0.242
_exptl_absorpt_process_details   '(SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24619
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.506
_diffrn_reflns_theta_max         28.351
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1688
_reflns_number_gt                1678
_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       'D8 Venture'
_computing_cell_refinement       'D8 Venture'
_computing_data_reduction        'D8 Venture'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0498P)²+7.2789P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1688
_refine_ls_number_parameters     85
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.0804
_refine_ls_wR_factor_gt          0.0802
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.102
_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 0.0000 1.0000 1.0000 0.02261(11) Uani 1 4 d S T P . .
I1 I 0.09858(2) 1.0000 1.04631(9) 0.04288(15) Uani 1 2 d S T P . .
I2 I -0.00090(3) 0.5000 0.87790(14) 0.03215(19) Uani 0.5 2 d S T P . .
I3 I 0.0000 1.11905(15) 0.5000 0.03148(19) Uani 0.5 2 d S T P . .
C1 C 0.1705(2) 0.4346(11) 0.4930(9) 0.038(2) Uani 0.5 1 d DG . P . .
C2 C 0.1839(3) 0.2334(11) 0.5726(13) 0.062(4) Uani 0.5 1 d DG . P . .
C3 C 0.2087(3) 0.1032(13) 0.451(2) 0.086(6) Uani 0.5 1 d G . P . .
C4 C 0.2201(3) 0.174(2) 0.2506(19) 0.090(5) Uani 0.5 1 d G U P . .
C5 C 0.2067(3) 0.376(2) 0.1709(12) 0.096(8) Uani 0.5 1 d G . P . .
C6 C 0.1819(2) 0.5011(15) 0.2921(10) 0.057(2) Uani 1 2 d G T P . .
C7 C 0.1428(3) 0.5727(15) 0.6157(15) 0.061(4) Uani 0.5 1 d D . P . .
C8 C 0.0982(3) 0.604(5) 0.565(3) 0.066(9) Uiso 0.25 1 d D . P . .
C8* C 0.0994(4) 0.472(5) 0.597(2) 0.039(5) Uiso 0.25 1 d D . P . .
N1 N 0.0810(4) 0.5000 0.3632(19) 0.119(5) Uani 1 2 d DS T P . .


_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 I2 3.1608(3) . ?
Pb1 I2 3.1608(3) 5_577 ?
Pb1 I2 3.1608(3) 5_567 ?
Pb1 I2 3.1608(3) 1_565 ?
Pb1 I3 3.1798(3) . ?
Pb1 I3 3.1798(3) 5_576 ?
Pb1 I3 3.1798(3) 1_556 ?
Pb1 I3 3.1798(3) 5_577 ?
Pb1 I1 3.2055(5) . ?
Pb1 I1 3.2055(5) 5_577 ?
I2 I2 1.5089(18) 5_567 ?
I2 Pb1 3.1608(3) 1_545 ?
I3 I3 1.4617(18) 5_576 ?
I3 Pb1 3.1798(3) 1_554 ?
C1 C1 0.803(14) 6_565 ?
C1 C7 1.217(6) 6_565 ?
C1 C2 1.3900 . ?
C1 C6 1.3814 . ?
C1 C7 1.482(2) . ?
C2 C3 1.3900 . ?
C2 C7 1.824(15) 6_565 ?
C3 C3 1.267(16) 6 ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3739 . ?
C5 C5 1.53(3) 6_565 ?
C6 C5 1.367(15) 6_565 ?
C6 C1 1.378(5) 6_565 ?
C7 C7 0.892(19) 6_565 ?
C7 C1 1.216(6) 6_565 ?
C7 C8* 1.439(18) 6_565 ?
C7 C8 1.481(2) . ?
C7 C8* 1.540(2) . ?
C7 C8 1.826(16) 6_565 ?
C7 C2 1.824(15) 6_565 ?
C8 C8* 0.51(4) 6_565 ?
C8 C8* 0.83(5) . ?
C8 C8 1.28(6) 6_565 ?
C8 N1 1.479(2) . ?
C8 C7 1.826(16) 6_565 ?
C8* C8* 0.34(6) 6_565 ?
C8* C8 0.51(4) 6_565 ?
C8* C7 1.439(18) 6_565 ?
C8* N1 1.539(2) . ?
N1 C8 1.479(2) 6_565 ?
N1 C8* 1.539(2) 6_565 ?

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
I2 Pb1 I2 180.0 . 5_577 ?
I2 Pb1 I2 27.62(3) . 5_567 ?
I2 Pb1 I2 152.38(3) 5_577 5_567 ?
I2 Pb1 I2 152.38(3) . 1_565 ?
I2 Pb1 I2 27.62(3) 5_577 1_565 ?
I2 Pb1 I2 180.0 5_567 1_565 ?
I2 Pb1 I3 89.49(2) . . ?
I2 Pb1 I3 90.51(2) 5_577 . ?
I2 Pb1 I3 117.09(2) 5_567 . ?
I2 Pb1 I3 62.91(2) 1_565 . ?
I2 Pb1 I3 62.91(2) . 5_576 ?
I2 Pb1 I3 117.09(2) 5_577 5_576 ?
I2 Pb1 I3 90.51(2) 5_567 5_576 ?
I2 Pb1 I3 89.49(2) 1_565 5_576 ?
I3 Pb1 I3 26.58(3) . 5_576 ?
I2 Pb1 I3 117.09(2) . 1_556 ?
I2 Pb1 I3 62.91(2) 5_577 1_556 ?
I2 Pb1 I3 89.49(2) 5_567 1_556 ?
I2 Pb1 I3 90.51(2) 1_565 1_556 ?
I3 Pb1 I3 153.42(3) . 1_556 ?
I3 Pb1 I3 180.0 5_576 1_556 ?
I2 Pb1 I3 90.51(2) . 5_577 ?
I2 Pb1 I3 89.49(2) 5_577 5_577 ?
I2 Pb1 I3 62.91(2) 5_567 5_577 ?
I2 Pb1 I3 117.09(2) 1_565 5_577 ?
I3 Pb1 I3 180.00(3) . 5_577 ?
I3 Pb1 I3 153.42(3) 5_576 5_577 ?
I3 Pb1 I3 26.58(3) 1_556 5_577 ?
I2 Pb1 I1 90.882(17) . . ?
I2 Pb1 I1 89.116(17) 5_577 . ?
I2 Pb1 I1 89.116(17) 5_567 . ?
I2 Pb1 I1 90.884(17) 1_565 . ?
I3 Pb1 I1 91.446(10) . . ?
I3 Pb1 I1 91.446(9) 5_576 . ?
I3 Pb1 I1 88.554(9) 1_556 . ?
I3 Pb1 I1 88.554(9) 5_577 . ?
I2 Pb1 I1 89.117(17) . 5_577 ?
I2 Pb1 I1 90.885(17) 5_577 5_577 ?
I2 Pb1 I1 90.884(17) 5_567 5_577 ?
I2 Pb1 I1 89.116(17) 1_565 5_577 ?
I3 Pb1 I1 88.554(9) . 5_577 ?
I3 Pb1 I1 88.554(9) 5_576 5_577 ?
I3 Pb1 I1 91.446(9) 1_556 5_577 ?
I3 Pb1 I1 91.446(9) 5_577 5_577 ?
I1 Pb1 I1 180.0 . 5_577 ?
I2 I2 Pb1 76.191(16) 5_567 . ?
I2 I2 Pb1 76.191(15) 5_567 1_545 ?
Pb1 I2 Pb1 152.38(3) . 1_545 ?
I3 I3 Pb1 76.712(16) 5_576 1_554 ?
I3 I3 Pb1 76.712(16) 5_576 . ?
Pb1 I3 Pb1 153.42(3) 1_554 . ?
C1 C1 C7 92.1(7) 6_565 6_565 ?
C1 C1 C2 152.7(3) 6_565 . ?
C7 C1 C2 88.5(8) 6_565 . ?
C1 C1 C6 72.8(3) 6_565 . ?
C7 C1 C6 145.6(7) 6_565 . ?
C2 C1 C6 119.0 . . ?
C1 C1 C7 55.1(4) 6_565 . ?
C7 C1 C7 37.0(9) 6_565 . ?
C2 C1 C7 120.9(2) . . ?
C6 C1 C7 120.0(2) . . ?
C3 C2 C1 120.0 . . ?
C3 C2 C7 155.8(4) . 6_565 ?
C1 C2 C7 41.8(3) . 6_565 ?
C3 C3 C2 125.1 6 . ?
C3 C3 C4 108.3 6 . ?
C2 C3 C4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C6 C5 C4 119.2 . . ?
C6 C5 C5 55.9 . 6_565 ?
C4 C5 C5 152.7 . 6_565 ?
C5 C6 C1 122.6(10) 6_565 6_565 ?
C5 C6 C5 67.8(9) 6_565 . ?
C1 C6 C5 148.8(3) 6_565 . ?
C5 C6 C1 149.3(4) 6_565 . ?
C1 C6 C1 33.8(5) 6_565 . ?
C5 C6 C1 121.8 . . ?
C7 C7 C1 87.9(7) 6_565 6_565 ?
C7 C7 C8* 78.9(12) 6_565 6_565 ?
C1 C7 C8* 134.9(10) 6_565 6_565 ?
C7 C7 C8 97.5(13) 6_565 . ?
C1 C7 C8 128.9(12) 6_565 . ?
C8* C7 C8 20.1(16) 6_565 . ?
C7 C7 C1 55.1(4) 6_565 . ?
C1 C7 C1 32.8(6) 6_565 . ?
C8* C7 C1 118.4(12) 6_565 . ?
C8 C7 C1 125.9(9) . . ?
C7 C7 C8* 66.4(11) 6_565 . ?
C1 C7 C8* 130.7(10) 6_565 . ?
C8* C7 C8* 12(2) 6_565 . ?
C8 C7 C8* 32(2) . . ?
C1 C7 C8* 108.6(11) . . ?
C7 C7 C8 53.5(9) 6_565 6_565 ?
C1 C7 C8 118.9(11) 6_565 6_565 ?
C8* C7 C8 26.3(16) 6_565 6_565 ?
C8 C7 C8 44(2) . 6_565 ?
C1 C7 C8 94.3(11) . 6_565 ?
C8* C7 C8 14.5(14) . 6_565 ?
C7 C7 C2 130.8(5) 6_565 6_565 ?
C1 C7 C2 49.6(5) 6_565 6_565 ?
C8* C7 C2 147.2(13) 6_565 6_565 ?
C8 C7 C2 127.1(16) . 6_565 ?
C1 C7 C2 79.7(7) . 6_565 ?
C8* C7 C2 158.3(12) . 6_565 ?
C8 C7 C2 161.2(7) 6_565 6_565 ?
C8* C8 C8* 9.2(15) 6_565 . ?
C8* C8 C8 23.1(10) 6_565 6_565 ?
C8* C8 C8 13.9(10) . 6_565 ?
C8* C8 N1 86.9(14) 6_565 . ?
C8* C8 N1 78.0(12) . . ?
C8 C8 N1 64.4(14) 6_565 . ?
C8* C8 C7 75.3(18) 6_565 . ?
C8* C8 C7 77.9(12) . . ?
C8 C8 C7 82.5(13) 6_565 . ?
N1 C8 C7 115.9(10) . . ?
C8* C8 C7 49.1(16) 6_565 6_565 ?
C8* C8 C7 49.9(10) . 6_565 ?
C8 C8 C7 53.5(9) 6_565 6_565 ?
N1 C8 C7 98.2(12) . 6_565 ?
C7 C8 C7 29.0(7) . 6_565 ?
C8* C8* C8 156.9(10) 6_565 6_565 ?
C8* C8* C8 13.9(9) 6_565 . ?
C8 C8* C8 143.0(12) 6_565 . ?
C8* C8* C7 101.1(12) 6_565 6_565 ?
C8 C8* C7 85(3) 6_565 6_565 ?
C8 C8* C7 103.7(11) . 6_565 ?
C8* C8* N1 83.7(11) 6_565 . ?
C8 C8* N1 73.7(4) 6_565 . ?
C8 C8* N1 70.1(7) . . ?
C7 C8* N1 114.8(11) 6_565 . ?
C8* C8* C7 66.5(12) 6_565 . ?
C8 C8* C7 116(3) 6_565 . ?
C8 C8* C7 70.1(8) . . ?
C7 C8* C7 34.6(7) 6_565 . ?
N1 C8* C7 109.1(9) . . ?
C8 N1 C8 51(3) . 6_565 ?
C8 N1 C8* 19.4(15) . 6_565 ?
C8 N1 C8* 32(2) 6_565 6_565 ?
C8 N1 C8* 32(2) . . ?
C8 N1 C8* 19.4(15) 6_565 . ?
C8* N1 C8* 13(2) 6_565 . ?

_refine_diff_density_max         2.366
_refine_diff_density_min         -1.581
_refine_diff_density_rms         0.165

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_butylaminepbi2_a
_database_code_depnum_ccdc_archive 'CCDC 1879292'
loop_
_audit_author_name
_audit_author_address
'Mi Hee Jung'
;Sejong University
South Korea
;
_audit_update_record             
;
2018-11-16 deposited with the CCDC.	2020-12-17 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            'C8 H24 I4 N2 Pb'
_chemical_formula_weight         863.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4371 1.8409 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.4194 10.2008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   8.8570(18)
_cell_length_b                   8.6750(17)
_cell_length_c                   27.435(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2108.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    13783
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.720
_exptl_crystal_F_000             1520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.075
_exptl_absorpt_coefficient_mu    13.715
_shelx_estimated_absorpt_T_min   0.290
_shelx_estimated_absorpt_T_max   0.426
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(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            12647
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.462
_diffrn_reflns_theta_max         33.217
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             3565
_reflns_number_gt                2447
_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 2014/5 (Sheldrick, 2014)'
_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)+(0.1084P)²+0.5256P] 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(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3565
_refine_ls_number_parameters     72
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0626
_refine_ls_wR_factor_ref         0.1770
_refine_ls_wR_factor_gt          0.1602
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.000
_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 0.500000 0.500000 0.500000 0.05162(18) Uani 1 2 d S . P . .
I1 I 0.53272(12) 0.48620(7) 0.38460(3) 0.0812(2) Uani 1 1 d . . . . .
C1 C 0.0283(19) 0.4741(16) 0.3805(5) 0.131(6) Uani 1 1 d D U . . .
H1A H 0.005302 0.367960 0.388809 0.157 Uiso 1 1 calc R U . . .
H1AB H 0.131000 0.495536 0.390789 0.157 Uiso 1 1 calc R U . . .
N1 N -0.0746(8) 0.5759(10) 0.4057(3) 0.093(2) Uani 1 1 d D . . . .
H1B H -0.065810 0.561889 0.437755 0.139 Uiso 1 1 calc R U . . .
H1C H -0.052565 0.673282 0.398418 0.139 Uiso 1 1 calc R U . . .
H1D H -0.168870 0.555240 0.396585 0.139 Uiso 1 1 calc R U . . .
I2 I 0.19669(6) 0.69493(6) 0.49583(2) 0.0749(2) Uani 1 1 d . . . . .
C2 C 0.015(2) 0.4955(14) 0.3277(6) 0.169(12) Uani 1 1 d D U . . .
H2A H -0.079111 0.451558 0.316555 0.202 Uiso 1 1 calc R U . . .
H2B H 0.014059 0.604858 0.320400 0.202 Uiso 1 1 calc R U . . .
C3 C 0.140(2) 0.423(4) 0.3016(8) 0.324(16) Uani 1 1 d D U . . .
H3A H 0.207105 0.503939 0.290324 0.389 Uiso 1 1 calc R U . . .
H3B H 0.196057 0.360418 0.324555 0.389 Uiso 1 1 calc R U . . .
C4 C 0.101(3) 0.329(3) 0.2610(8) 0.306(15) Uani 1 1 d D U . . .
H4A H 0.026391 0.255221 0.270613 0.459 Uiso 1 1 calc R U . . .
H4AB H 0.189484 0.276616 0.249469 0.459 Uiso 1 1 calc R U . . .
H4AC H 0.061255 0.392918 0.235361 0.459 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 I2 3.1705(6) 8_655 ?
Pb1 I2 3.1705(6) 4_566 ?
Pb1 I2 3.1764(7) 5_666 ?
Pb1 I2 3.1764(6) . ?
Pb1 I1 3.1813(11) 5_666 ?
Pb1 I1 3.1814(11) . ?
C1 N1 1.446(9) . ?
C1 C2 1.465(10) . ?
C1 H1A 0.9700 . ?
C1 H1AB 0.9700 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
C2 C3 1.456(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.423(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4AB 0.9600 . ?
C4 H4AC 0.9600 . ?

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
I2 Pb1 I2 180.00(2) 8_655 4_566 ?
I2 Pb1 I2 91.239(15) 8_655 5_666 ?
I2 Pb1 I2 88.761(15) 4_566 5_666 ?
I2 Pb1 I2 88.761(16) 8_655 . ?
I2 Pb1 I2 91.239(16) 4_566 . ?
I2 Pb1 I2 180.0 5_666 . ?
I2 Pb1 I1 90.987(15) 8_655 5_666 ?
I2 Pb1 I1 89.013(15) 4_566 5_666 ?
I2 Pb1 I1 93.514(19) 5_666 5_666 ?
I2 Pb1 I1 86.487(19) . 5_666 ?
I2 Pb1 I1 89.014(15) 8_655 . ?
I2 Pb1 I1 90.986(15) 4_566 . ?
I2 Pb1 I1 86.487(19) 5_666 . ?
I2 Pb1 I1 93.513(19) . . ?
I1 Pb1 I1 180.0 5_666 . ?
N1 C1 C2 110.3(11) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1AB 109.6 . . ?
C2 C1 H1AB 109.6 . . ?
H1A C1 H1AB 108.1 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
H1B N1 H1D 109.5 . . ?
H1C N1 H1D 109.5 . . ?
Pb1 I2 Pb1 155.21(2) 4_466 . ?
C3 C2 C1 111.9(13) . . ?
C3 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 C2 116.7(11) . . ?
C4 C3 H3A 108.1 . . ?
C2 C3 H3A 108.1 . . ?
C4 C3 H3B 108.1 . . ?
C2 C3 H3B 108.1 . . ?
H3A C3 H3B 107.3 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4AB 109.5 . . ?
H4A C4 H4AB 109.5 . . ?
C3 C4 H4AC 109.5 . . ?
H4A C4 H4AC 109.5 . . ?
H4AB C4 H4AC 109.5 . . ?

_refine_diff_density_max         3.217
_refine_diff_density_min         -2.910
_refine_diff_density_rms         0.529

####################################################################### 
# 
# 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_EAPbI3_1_a
_database_code_depnum_ccdc_archive 'CCDC 1879309'
loop_
_audit_author_name
_audit_author_address
'Mi Hee Jung'
;Sejong University
South Korea
;
_audit_update_record             
;
2018-11-16 deposited with the CCDC.	2020-12-17 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            'C2 H8 I3 N Pb'
_chemical_formula_weight         633.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4371 1.8409 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.4194 10.2008 '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, 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'

_cell_length_a                   8.1520(16)
_cell_length_b                   8.7470(18)
_cell_length_c                   15.148(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1080.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15449
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.899
_exptl_crystal_F_000             1072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    23.904
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.788
_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     0.71073
_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            10824
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_av_R_equivalents  0.1475
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.838
_diffrn_reflns_theta_max         34.099
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             2070
_reflns_number_gt                1872
_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 2014/5 (Sheldrick, 2014)'
_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)+(0.1184P)²+1.6134P] 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       0.026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2070
_refine_ls_number_parameters     43
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0617
_refine_ls_wR_factor_ref         0.2039
_refine_ls_wR_factor_gt          0.2007
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.252
_refine_ls_shift/su_mean         0.022

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
Pb01 Pb 0.51162(5) 0.250000 0.75280(2) 0.0507(2) Uani 1 2 d S T P . .
C1 C 0.382(4) -0.250000 0.630(2) 0.183(16) Uani 1 2 d DS T P . .
H1A H 0.313746 -0.200562 0.672943 0.275 Uiso 0.5 1 calc R U P . .
H1AB H 0.483793 -0.195996 0.624686 0.275 Uiso 0.5 1 calc R U P . .
H1AC H 0.402522 -0.353442 0.647749 0.275 Uiso 0.5 1 calc R U P . .
I002 I 0.74231(8) 0.50272(6) 0.67183(6) 0.0726(3) Uani 1 1 d . . . . .
C2 C 0.298(3) -0.250000 0.545(2) 0.26(3) Uani 1 2 d DS T P . .
H2A H 0.325881 -0.340361 0.510643 0.310 Uiso 0.5 1 calc R U P . .
H2AB H 0.325881 -0.159639 0.510643 0.310 Uiso 0.5 1 calc R U P . .
I003 I 0.28997(15) 0.250000 0.58396(5) 0.0838(4) Uani 1 2 d S T P . .
N3 N 0.124(2) -0.250000 0.5700(19) 0.180(14) Uani 1 2 d DS T P . .
H3A H 0.112162 -0.297275 0.621612 0.270 Uiso 0.5 1 calc R U P . .
H3B H 0.065742 -0.298652 0.528980 0.270 Uiso 0.5 1 calc R U P . .
H3C H 0.088619 -0.154073 0.574631 0.270 Uiso 0.5 1 calc R U P . .


_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
Pb01 I003 3.1315(10) . ?
Pb01 I002 3.1508(8) . ?
Pb01 I002 3.1508(7) 7_565 ?
Pb01 I002 3.3181(8) 4_456 ?
Pb01 I002 3.3181(8) 6_557 ?
Pb01 I003 3.3562(11) 6_657 ?
C1 C2 1.457(10) . ?
C1 H1A 1.0449 . ?
C1 H1AB 1.0448 . ?
C1 H1AC 1.0418 . ?
C2 N3 1.472(10) . ?
C2 H2A 0.9700 . ?
C2 H2AB 0.9700 . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
N3 H3A 0.9(2) 7 ?
N3 H3B 0.9(2) 7 ?
N3 H3C 0.890(5) 7 ?

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
I003 Pb01 I002 91.52(3) . . ?
I003 Pb01 I002 91.52(2) . 7_565 ?
I002 Pb01 I002 89.11(3) . 7_565 ?
I003 Pb01 I002 84.22(2) . 4_456 ?
I002 Pb01 I002 175.04(2) . 4_456 ?
I002 Pb01 I002 93.52(3) 7_565 4_456 ?
I003 Pb01 I002 84.22(2) . 6_557 ?
I002 Pb01 I002 93.52(3) . 6_557 ?
I002 Pb01 I002 175.04(2) 7_565 6_557 ?
I002 Pb01 I002 83.55(3) 4_456 6_557 ?
I003 Pb01 I003 172.70(4) . 6_657 ?
I002 Pb01 I003 83.30(2) . 6_657 ?
I002 Pb01 I003 83.30(2) 7_565 6_657 ?
I002 Pb01 I003 101.17(2) 4_456 6_657 ?
I002 Pb01 I003 101.17(2) 6_557 6_657 ?
C2 C1 H1A 118.3 . . ?
C2 C1 H1AB 118.4 . . ?
H1A C1 H1AB 99.4 . . ?
C2 C1 H1AC 117.9 . . ?
H1A C1 H1AC 99.5 . . ?
H1AB C1 H1AC 99.7 . . ?
Pb01 I002 Pb01 78.086(19) . 6_657 ?
C1 C2 N3 103(2) . . ?
C1 C2 H2A 111.1 . . ?
N3 C2 H2A 111.3 . . ?
C1 C2 H2AB 111.1 . . ?
N3 C2 H2AB 111.3 . . ?
H2A C2 H2AB 109.2 . . ?
Pb01 I003 Pb01 77.78(2) . 6_557 ?
C2 N3 H3A 109.5 . . ?
C2 N3 H3B 109.4 . . ?
H3A N3 H3B 109.5 . . ?
C2 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C2 N3 H3A 110(6) . 7 ?
H3A N3 H3A 55.4 . 7 ?
H3B N3 H3A 141.0 . 7 ?
H3C N3 H3A 57.1 . 7 ?
C2 N3 H3B 109(6) . 7 ?
H3A N3 H3B 141.0 . 7 ?
H3B N3 H3B 57.1 . 7 ?
H3C N3 H3B 55.4 . 7 ?
H3A N3 H3B 109.5 7 7 ?
C2 N3 H3C 109.47(12) . 7 ?
H3A N3 H3C 57.1 . 7 ?
H3B N3 H3C 55.4 . 7 ?
H3C N3 H3C 141.0 . 7 ?
H3A N3 H3C 109.5 7 7 ?
H3B N3 H3C 109.5 7 7 ?

_refine_diff_density_max         2.685
_refine_diff_density_min         -2.605
_refine_diff_density_rms         0.377

