# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_H1_A_c
_database_code_depnum_ccdc_archive 'CCDC 1894433'
loop_
_audit_author_name
_audit_author_address
'MI-HEE JUNG'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2019-01-29 deposited with the CCDC.	2019-05-21 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            'C11.96 H31.91 I4 N2 Pb'
_chemical_formula_weight         918.57

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      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'

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

_cell_length_a                   32.798(5)
_cell_length_b                   8.9632(11)
_cell_length_c                   8.6995(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2557.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7939
_cell_measurement_theta_min      2.484
_cell_measurement_theta_max      24.146

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.386
_exptl_crystal_F_000             1647
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.760
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    10.874
_shelx_estimated_absorpt_T_min   0.044
_shelx_estimated_absorpt_T_max   0.355
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.4389
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.700
_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            7502
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.223
_diffrn_reflns_theta_max         27.820
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3010
_reflns_number_gt                1865
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_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)+(0.1013P)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       0.0016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3010
_refine_ls_number_parameters     105
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0595
_refine_ls_wR_factor_ref         0.1874
_refine_ls_wR_factor_gt          0.1472
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.875
_refine_ls_shift/su_mean         0.120

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 0.7499(2) 0.3546(11) 0.0513(4) Uani 1 2 d S T P . .
I1 I 0.500000 0.4477(3) 0.5507(3) 0.0746(17) Uani 1 2 d S T P A .
N1 N 0.5840(9) 0.815(3) 0.920(3) 0.112(9) Uani 1 1 d D . . . .
H1A H 0.594374 0.806473 1.014179 0.168 Uiso 1 1 calc R U . . .
H1B H 0.557027 0.803171 0.924324 0.168 Uiso 1 1 calc R U . . .
H1C H 0.589785 0.904407 0.882158 0.168 Uiso 1 1 calc R U . . .
C1 C 0.6016(18) 0.699(9) 0.820(15) 0.34(6) Uani 1 1 d D U . . .
H1D H 0.592310 0.704125 0.714669 0.406 Uiso 1 1 calc R U . . .
H1E H 0.598950 0.598810 0.860933 0.406 Uiso 1 1 calc R U . . .
I2 I 0.500000 0.9481(3) 0.6595(4) 0.0784(17) Uani 1 2 d S T P A .
C2 C 0.6423(15) 0.766(6) 0.845(10) 0.17(2) Uani 0.99(8) 1 d D U P . .
H2A H 0.640965 0.870839 0.817190 0.203 Uiso 0.99(8) 1 calc R U P . .
H2B H 0.648495 0.761501 0.954343 0.203 Uiso 0.99(8) 1 calc R U P . .
C3 C 0.676(2) 0.697(9) 0.760(15) 0.38(6) Uani 0.99(8) 1 d D U P . .
H3A H 0.677316 0.762319 0.671594 0.451 Uiso 0.99(8) 1 calc R U P . .
H3B H 0.662754 0.607813 0.722700 0.451 Uiso 0.99(8) 1 calc R U P . .
I3A I 0.5975(3) 0.7800(7) 0.3408(18) 0.072(3) Uani 0.5 1 d . . P A 1
I3B I 0.5975(4) 0.7119(9) 0.3696(15) 0.086(3) Uani 0.5 1 d . . P A 2
C4 C 0.719(2) 0.645(10) 0.765(10) 0.26(4) Uani 0.99(8) 1 d D U P . .
H4A H 0.718243 0.566434 0.841711 0.317 Uiso 0.99(8) 1 calc R U P . .
H4B H 0.733205 0.726932 0.812287 0.317 Uiso 0.99(8) 1 calc R U P . .
C6 C 0.788(2) 0.625(7) 0.716(8) 0.22(3) Uani 1 1 d D U . . .
H6A H 0.802586 0.689357 0.646775 0.332 Uiso 1 1 calc R U . . .
H6B H 0.803342 0.535227 0.731903 0.332 Uiso 1 1 calc R U . . .
H6C H 0.784322 0.675235 0.812667 0.332 Uiso 1 1 calc R U . . .
C5 C 0.748(2) 0.588(12) 0.650(12) 0.33(5) Uani 1 1 d D U . . .
H5A H 0.745137 0.481421 0.636428 0.399 Uiso 1 1 calc R U . . .
H5B H 0.744216 0.637210 0.551732 0.399 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 3.182(10) 2_664 ?
Pb1 I2 3.192(10) . ?
Pb1 I2 3.195(7) 2_674 ?
Pb1 I1 3.201(7) . ?
Pb1 I3A 3.213(11) . ?
Pb1 I3A 3.213(11) 4_655 ?
Pb1 I3B 3.220(14) 4_655 ?
Pb1 I3B 3.220(14) . ?
N1 C1 1.469(14) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C1 C2 1.481(15) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C2 C3 1.471(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.474(14) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.473(14) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C5 1.470(14) . ?
C6 H6A 0.9772 . ?
C6 H6B 0.9781 . ?
C6 H6C 0.9763 . ?
C5 H5A 0.9700 . ?
C5 H5B 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
I1 Pb1 I2 180.0(3) 2_664 . ?
I1 Pb1 I2 91.7(3) 2_664 2_674 ?
I2 Pb1 I2 88.28(8) . 2_674 ?
I1 Pb1 I1 88.38(8) 2_664 . ?
I2 Pb1 I1 91.6(3) . . ?
I2 Pb1 I1 179.9(4) 2_674 . ?
I1 Pb1 I3A 90.89(17) 2_664 . ?
I2 Pb1 I3A 89.11(17) . . ?
I2 Pb1 I3A 84.78(14) 2_674 . ?
I1 Pb1 I3A 95.21(14) . . ?
I1 Pb1 I3A 90.89(17) 2_664 4_655 ?
I2 Pb1 I3A 89.11(17) . 4_655 ?
I2 Pb1 I3A 84.78(14) 2_674 4_655 ?
I1 Pb1 I3A 95.21(14) . 4_655 ?
I3A Pb1 I3A 169.5(3) . 4_655 ?
I1 Pb1 I3B 88.55(18) 2_664 4_655 ?
I2 Pb1 I3B 91.45(19) . 4_655 ?
I2 Pb1 I3B 96.38(16) 2_674 4_655 ?
I1 Pb1 I3B 83.62(16) . 4_655 ?
I3A Pb1 I3B 178.7(2) . 4_655 ?
I3A Pb1 I3B 11.77(10) 4_655 4_655 ?
I1 Pb1 I3B 88.55(18) 2_664 . ?
I2 Pb1 I3B 91.45(19) . . ?
I2 Pb1 I3B 96.38(16) 2_674 . ?
I1 Pb1 I3B 83.62(16) . . ?
I3B Pb1 I3B 167.0(3) 4_655 . ?
Pb1 I1 Pb1 156.0(3) 2_665 . ?
C1 N1 H1A 111.1 . . ?
C1 N1 H1B 109.3 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 107.9 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
N1 C1 C2 89(4) . . ?
N1 C1 H1D 115.6 . . ?
C2 C1 H1D 115.6 . . ?
N1 C1 H1E 112.2 . . ?
C2 C1 H1E 111.8 . . ?
H1D C1 H1E 111.1 . . ?
Pb1 I2 Pb1 155.9(3) . 2_675 ?
C3 C2 C1 116(6) . . ?
C3 C2 H2A 107.4 . . ?
C1 C2 H2A 106.4 . . ?
C3 C2 H2B 109.2 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 107.5 . . ?
C2 C3 C4 147(10) . . ?
C2 C3 H3A 100.7 . . ?
C4 C3 H3A 101.2 . . ?
C2 C3 H3B 99.2 . . ?
C4 C3 H3B 99.2 . . ?
H3A C3 H3B 104.1 . . ?
C3 C4 C5 135(8) . . ?
C3 C4 H4A 104.4 . . ?
C5 C4 H4A 104.3 . . ?
C3 C4 H4B 102.6 . . ?
C5 C4 H4B 102.2 . . ?
H4A C4 H4B 105.1 . . ?
C5 C6 H6A 110.6 . . ?
C5 C6 H6B 112.6 . . ?
H6A C6 H6B 107.5 . . ?
C5 C6 H6C 110.6 . . ?
H6A C6 H6C 107.6 . . ?
H6B C6 H6C 107.8 . . ?
C6 C5 C4 104(7) . . ?
C6 C5 H5A 109.7 . . ?
C4 C5 H5A 109.8 . . ?
C6 C5 H5B 112.1 . . ?
C4 C5 H5B 112.2 . . ?
H5A C5 H5B 109.0 . . ?

_refine_diff_density_max         3.383
_refine_diff_density_min         -1.640
_refine_diff_density_rms         0.550



####################################################################### 
# 
# 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_H2A_a
_database_code_depnum_ccdc_archive 'CCDC 1894434'
loop_
_audit_author_name
_audit_author_address
'MI-HEE JUNG'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2019-01-29 deposited with the CCDC.	2019-05-21 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            'C13 H0 I7 N3 Pb2'
_chemical_formula_weight         1500.84

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      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            cherry
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.809
_exptl_crystal_F_000             2536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    14.824
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.4670
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.700
_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         0.892
_diffrn_reflns_theta_max         27.839
_diffrn_reflns_theta_full        24.835
_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          
;
 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)+(0.1245P)²+35.2096P] 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       0.00074(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4395
_refine_ls_number_parameters     113
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_gt           0.0862
_refine_ls_wR_factor_ref         0.2598
_refine_ls_wR_factor_gt          0.2221
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.047
_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 0.42747(2) 0.25117(7) 0.69839(7) 0.0416(3) Uani 1 1 d . . . . .
C1 C 0.3596(7) 0.701(4) 0.671(5) 0.172(18) Uani 1 1 d D U . . .
N1 N 0.3759(5) 0.817(2) 0.599(3) 0.098(8) Uani 1 1 d D . . . .
I1 I 0.35830(4) 0.2110(2) 0.6656(2) 0.0771(6) Uani 1 1 d . . . . .
I2 I 0.43240(4) -0.04150(17) 0.90930(16) 0.0672(5) Uani 1 1 d . . . . .
N2 N 0.500000 -0.167(7) 0.750000 0.30(4) Uani 1 2 d DS TU P . .
C2 C 0.3277(6) 0.732(4) 0.662(6) 0.151(16) Uani 1 1 d D U . . .
I3 I 0.500000 0.2613(3) 0.750000 0.0677(7) Uani 1 2 d S T P . .
C3 C 0.3107(6) 0.620(4) 0.737(4) 0.156(16) Uani 1 1 d D . . . .
I4 I 0.42731(4) 0.54164(19) 0.48996(19) 0.0823(6) Uani 1 1 d . . . . .
C5 C 0.2598(7) 0.568(6) 0.802(5) 0.20(2) Uani 1 1 d D U . . .
C6 C 0.2286(7) 0.614(5) 0.759(5) 0.171(17) Uani 1 1 d D U . . .
C7 C 0.500000 -0.331(7) 0.750000 0.30(4) Uani 1 2 d DS TU P . .
C4 C 0.2786(6) 0.649(5) 0.707(4) 0.165(16) Uani 1 1 d D 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 3.1363(19) . ?
Pb1 I4 3.1710(14) 6_566 ?
Pb1 I4 3.1820(15) . ?
Pb1 I2 3.1991(14) 6 ?
Pb1 I2 3.2006(14) . ?
Pb1 I3 3.2644(8) . ?
C1 C2 1.470(10) . ?
C1 N1 1.473(10) . ?
N2 C7 1.467(10) . ?
C2 C3 1.472(10) . ?
C3 C4 1.468(10) . ?
C5 C4 1.468(10) . ?
C5 C6 1.474(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
I1 Pb1 I4 91.30(5) . 6_566 ?
I1 Pb1 I4 96.95(5) . . ?
I4 Pb1 I4 89.521(19) 6_566 . ?
I1 Pb1 I2 92.48(5) . 6 ?
I4 Pb1 I2 176.15(5) 6_566 6 ?
I4 Pb1 I2 90.71(4) . 6 ?
I1 Pb1 I2 86.89(5) . . ?
I4 Pb1 I2 90.83(4) 6_566 . ?
I4 Pb1 I2 176.14(5) . . ?
I2 Pb1 I2 88.684(19) 6 . ?
I1 Pb1 I3 174.36(5) . . ?
I4 Pb1 I3 89.45(5) 6_566 . ?
I4 Pb1 I3 88.65(5) . . ?
I2 Pb1 I3 86.71(4) 6 . ?
I2 Pb1 I3 87.51(5) . . ?
C2 C1 N1 113(2) . . ?
Pb1 I2 Pb1 159.35(6) 6_556 . ?
C1 C2 C3 115(2) . . ?
Pb1 I3 Pb1 176.82(8) 2_656 . ?
C4 C3 C2 112(2) . . ?
Pb1 I4 Pb1 161.03(7) 6_565 . ?
C4 C5 C6 110(2) . . ?
C3 C4 C5 117(2) . . ?

_refine_diff_density_max         5.496
_refine_diff_density_min         -2.495
_refine_diff_density_rms         0.958



####################################################################### 
# 
# 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_H3_a
_database_code_depnum_ccdc_archive 'CCDC 1894435'
loop_
_audit_author_name
_audit_author_address
'MI-HEE JUNG'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2019-01-29 deposited with the CCDC.	2019-05-21 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 H44 I10 N4 Pb3'
_chemical_formula_weight         2159.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0192 0.0096 '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 0.0330 0.0189 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.2930 6.8966 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0816 8.6988 '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                   28.5014(11)
_cell_length_b                   8.8042(4)
_cell_length_c                   8.7102(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.206(4)
_cell_angle_gamma                90
_cell_volume                     2185.18(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    7500
_cell_measurement_theta_min      3.1460
_cell_measurement_theta_max      74.2820

_exptl_crystal_description       plate
_exptl_crystal_colour            'fluorescent light black'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.281
_exptl_crystal_F_000             1864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          120.000
_exptl_crystal_size_mid          50.000
_exptl_crystal_size_min          10.000
_exptl_absorpt_coefficient_mu    76.275
_shelx_estimated_absorpt_T_min   0.007
_shelx_estimated_absorpt_T_max   0.007
_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      93(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19200
_diffrn_reflns_av_unetI/netI     0.1048
_diffrn_reflns_av_R_equivalents  0.2910
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.102
_diffrn_reflns_theta_max         67.054
_diffrn_reflns_theta_full        67.054
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3919
_reflns_number_gt                3493
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.2000P)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         3919
_refine_ls_number_parameters     140
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.2970
_refine_ls_R_factor_gt           0.2953
_refine_ls_wR_factor_ref         0.6350
_refine_ls_wR_factor_gt          0.6309
_refine_ls_goodness_of_fit_ref   2.844
_refine_ls_restrained_S_all      2.820
_refine_ls_shift/su_max          0.093
_refine_ls_shift/su_mean         0.003

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 0.0617(11) Uani 1 2 d S . P . .
I1 I 0.50000(12) 0.6906(4) 0.1896(4) 0.0697(12) Uani 1 1 d . . . . .
C1 C 0.8316(14) 0.554(6) 1.035(9) 0.10(2) Uani 1 1 d D U . . .
H1A H 0.813240 0.569307 1.129328 0.123 Uiso 1 1 calc R U . . .
H1AB H 0.832666 0.652790 0.980826 0.123 Uiso 1 1 calc R U . . .
N1 N 0.8067(11) 0.444(5) 0.936(5) 0.063(10) Uani 1 1 d D U . . .
H1B H 0.775505 0.465484 0.934300 0.095 Uiso 1 1 calc R U . . .
H1C H 0.811366 0.348617 0.974043 0.095 Uiso 1 1 calc R U . . .
H1D H 0.817968 0.449578 0.839493 0.095 Uiso 1 1 calc R U . . .
Pb2 Pb 0.72676(7) 0.5001(2) 0.5032(3) 0.0606(10) Uani 1 1 d . . . . .
I2 I 0.61118(12) 0.4934(4) 0.4965(5) 0.0661(13) Uani 1 1 d . . . . .
C2 C 0.8797(14) 0.511(5) 1.081(9) 0.086(18) Uani 1 1 d D U . . .
H2A H 0.897089 0.483483 0.987712 0.103 Uiso 1 1 calc R U . . .
H2B H 0.878471 0.419933 1.147139 0.103 Uiso 1 1 calc R U . . .
N2 N 0.5950(18) 0.092(7) 0.595(7) 0.085(11) Uani 1 1 d D U . . .
H2C H 0.615627 0.169814 0.610877 0.127 Uiso 1 1 calc R U . . .
H2D H 0.587589 0.049787 0.686237 0.127 Uiso 1 1 calc R U . . .
H2E H 0.568552 0.128344 0.547364 0.127 Uiso 1 1 calc R U . . .
C3 C 0.9059(13) 0.631(5) 1.164(7) 0.080(15) Uani 1 1 d D U . . .
H3A H 0.908927 0.719794 1.094806 0.096 Uiso 1 1 calc R U . . .
H3B H 0.887501 0.663403 1.252938 0.096 Uiso 1 1 calc R U . . .
I3 I 0.71944(12) 0.1989(4) 0.6996(4) 0.0655(12) Uani 1 1 d . . . . .
C4 C 0.9531(12) 0.586(5) 1.218(7) 0.078(14) Uani 1 1 d D U . . .
H4A H 0.950444 0.491571 1.279293 0.093 Uiso 1 1 calc R U . . .
H4B H 0.972503 0.562954 1.128373 0.093 Uiso 1 1 calc R U . . .
I4 I 0.72427(13) 0.7053(4) 0.7967(5) 0.0707(12) Uani 1 1 d . . . . .
C5 C 0.9774(10) 0.701(4) 1.313(5) 0.051(9) Uani 1 1 d D U . . .
H5A H 0.974164 0.800845 1.260944 0.062 Uiso 1 1 calc R U . . .
H5B H 0.961496 0.708732 1.412495 0.062 Uiso 1 1 calc R U . . .
I5 I 0.83530(13) 0.4609(5) 0.5278(5) 0.0698(12) Uani 1 1 d . . . . .
C6 C 1.0275(11) 0.672(7) 1.343(8) 0.083(16) Uani 1 1 d D U . . .
H6A H 1.037476 0.722409 1.437981 0.124 Uiso 1 1 calc R U . . .
H6AB H 1.045748 0.711010 1.257190 0.124 Uiso 1 1 calc R U . . .
H6AC H 1.032647 0.562087 1.352522 0.124 Uiso 1 1 calc R U . . .
C7 C 0.617(2) -0.023(8) 0.497(8) 0.085(11) Uani 1 1 d D U . . .
H7A H 0.640851 -0.078006 0.556094 0.127 Uiso 1 1 calc R U . . .
H7AB H 0.630895 0.026243 0.408465 0.127 Uiso 1 1 calc R U . . .
H7AC H 0.592552 -0.095011 0.460601 0.127 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 3.170(4) 3_666 ?
Pb1 I2 3.170(4) . ?
Pb1 I1 3.182(4) 3_666 ?
Pb1 I1 3.182(4) . ?
Pb1 I1 3.186(4) 2_645 ?
Pb1 I1 3.186(4) 4_576 ?
C1 N1 1.470(10) . ?
C1 C2 1.470(10) . ?
C1 H1A 0.9900 . ?
C1 H1AB 0.9900 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 H1D 0.9100 . ?
Pb2 I5 3.116(4) . ?
Pb2 I4 3.132(4) . ?
Pb2 I4 3.157(4) 4_575 ?
Pb2 I3 3.165(4) . ?
Pb2 I3 3.175(4) 4_565 ?
Pb2 I2 3.294(4) . ?
C2 C3 1.472(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N2 C7 1.470(10) . ?
N2 H2C 0.9100 . ?
N2 H2D 0.9100 . ?
N2 H2E 0.9100 . ?
C3 C4 1.471(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.470(10) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.469(10) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9802 . ?
C6 H6AB 0.9802 . ?
C6 H6AC 0.9802 . ?
C7 H7A 0.9800 . ?
C7 H7AB 0.9800 . ?
C7 H7AC 0.9800 . ?

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 3_666 . ?
I2 Pb1 I1 89.07(9) 3_666 3_666 ?
I2 Pb1 I1 90.93(9) . 3_666 ?
I2 Pb1 I1 90.93(9) 3_666 . ?
I2 Pb1 I1 89.07(9) . . ?
I1 Pb1 I1 180.0 3_666 . ?
I2 Pb1 I1 91.81(9) 3_666 2_645 ?
I2 Pb1 I1 88.19(9) . 2_645 ?
I1 Pb1 I1 89.40(3) 3_666 2_645 ?
I1 Pb1 I1 90.60(3) . 2_645 ?
I2 Pb1 I1 88.19(9) 3_666 4_576 ?
I2 Pb1 I1 91.81(9) . 4_576 ?
I1 Pb1 I1 90.60(3) 3_666 4_576 ?
I1 Pb1 I1 89.40(3) . 4_576 ?
I1 Pb1 I1 180.00(12) 2_645 4_576 ?
Pb1 I1 Pb1 153.06(14) . 2_655 ?
N1 C1 C2 115.1(16) . . ?
N1 C1 H1A 108.5 . . ?
C2 C1 H1A 108.5 . . ?
N1 C1 H1AB 108.5 . . ?
C2 C1 H1AB 108.5 . . ?
H1A C1 H1AB 107.5 . . ?
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 . . ?
I5 Pb2 I4 92.72(11) . . ?
I5 Pb2 I4 98.08(11) . 4_575 ?
I4 Pb2 I4 89.45(6) . 4_575 ?
I5 Pb2 I3 86.95(11) . . ?
I4 Pb2 I3 92.26(12) . . ?
I4 Pb2 I3 174.61(11) 4_575 . ?
I5 Pb2 I3 92.52(11) . 4_565 ?
I4 Pb2 I3 174.66(11) . 4_565 ?
I4 Pb2 I3 88.76(11) 4_575 4_565 ?
I3 Pb2 I3 89.08(6) . 4_565 ?
I5 Pb2 I2 172.06(13) . . ?
I4 Pb2 I2 89.13(10) . . ?
I4 Pb2 I2 89.66(11) 4_575 . ?
I3 Pb2 I2 85.26(10) . . ?
I3 Pb2 I2 85.83(10) 4_565 . ?
Pb1 I2 Pb2 177.41(14) . . ?
C1 C2 C3 114.1(15) . . ?
C1 C2 H2A 108.7 . . ?
C3 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
C3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C7 N2 H2C 109.5 . . ?
C7 N2 H2D 109.4 . . ?
H2C N2 H2D 109.5 . . ?
C7 N2 H2E 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
C4 C3 C2 114.6(15) . . ?
C4 C3 H3A 108.6 . . ?
C2 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
C2 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
Pb2 I3 Pb2 155.29(14) . 4_566 ?
C5 C4 C3 114.3(15) . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
C3 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
Pb2 I4 Pb2 159.80(16) . 4_576 ?
C6 C5 C4 114.9(16) . . ?
C6 C5 H5A 108.5 . . ?
C4 C5 H5A 108.5 . . ?
C6 C5 H5B 108.6 . . ?
C4 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6AB 109.5 . . ?
H6A C6 H6AB 109.5 . . ?
C5 C6 H6AC 109.5 . . ?
H6A C6 H6AC 109.5 . . ?
H6AB C6 H6AC 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7AB 109.5 . . ?
H7A C7 H7AB 109.5 . . ?
N2 C7 H7AC 109.5 . . ?
H7A C7 H7AC 109.5 . . ?
H7AB C7 H7AC 109.5 . . ?

_refine_diff_density_max         18.795
_refine_diff_density_min         -4.891
_refine_diff_density_rms         1.740



