# Electronic Supplementary Material (ESI) for Materials Chemistry Frontiers.
# This journal is © the Partner Organisations 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_4
_database_code_depnum_ccdc_archive 'CCDC 2107024'
loop_
_audit_author_name
_audit_author_address
'Mohamed Saber Lassoued'
;School of Chemistry Xian Key Laboratory of Sustainable Energy and Materials Chemistry
China
;
_audit_update_record             
;
2021-09-02 deposited with the CCDC.	2021-11-08 downloaded from the CCDC.
;
_audit_creation_date             2021-07-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C6 H18 N4 Pb, I6 Pb2'
_chemical_formula_sum            'C6 H18 I6 N4 Pb3'
_chemical_formula_weight         1529.21
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   8.8484(8)
_cell_length_b                   19.3860(18)
_cell_length_c                   15.5239(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.255(4)
_cell_angle_gamma                90.00
_cell_volume                     2408.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.55
_exptl_absorpt_coefficient_mu    28.607
_exptl_absorpt_correction_T_max  0.005
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    4.218
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.823
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.182
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21799
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.79
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                5307
_reflns_number_total             5536
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.628
_refine_diff_density_min         -2.529
_refine_diff_density_rms         0.480
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         5536
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0435
_refine_ls_restrained_S_all      1.185
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+274.3427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1225
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 C1-C3
 1.52 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 N3(H3), N2(H2)
4.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2A,H2B), C3(H3A,H3B), C4(H4C,H4D), C5(H5A,H5B),
 C6(H6A,H6B)
4.c X=CH2 refined with riding coordinates:
 N4(H4A,H4B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Pb1 Pb 0.08906(8) 0.40275(3) 0.51558(4) 0.01531(14) Uani 1 d . . . .
Pb2 Pb 0.50959(8) 0.55398(3) 0.86108(4) 0.01512(14) Uani 1 d . . . .
Pb3 Pb 1.01434(8) 0.53242(3) 0.85490(4) 0.01524(14) Uani 1 d . . . .
I3 I 0.79581(13) 0.43231(5) 0.91043(7) 0.0147(2) Uani 1 d . . . .
I1 I 1.30472(13) 0.42229(5) 0.89989(7) 0.0166(2) Uani 1 d . . . .
I5 I 0.24564(14) 0.66653(6) 0.85063(8) 0.0183(2) Uani 1 d . . . .
I4 I 0.34728(16) 0.53962(6) 0.64513(8) 0.0237(3) Uani 1 d . . . .
I6 I 0.75755(15) 0.65725(6) 0.83641(9) 0.0242(3) Uani 1 d . . . .
I2 I 0.84998(16) 0.47574(7) 0.64745(8) 0.0253(3) Uani 1 d . . . .
N1 N 0.247(2) 0.3441(8) 0.6673(11) 0.032(4) Uani 1 d . . . .
H1A H 0.2214 0.3632 0.7121 0.038 Uiso 1 calc . . R .
H1B H 0.2159 0.2995 0.6614 0.038 Uiso 1 calc . . R .
N3 N 0.072(2) 0.3059(8) 0.4027(11) 0.026(4) Uani 1 d . . . .
H3 H 0.0212 0.3247 0.3434 0.031 Uiso 1 calc . . R .
N4 N -0.132(3) 0.3103(10) 0.5101(13) 0.039(5) Uani 1 d . . . .
H4A H -0.0272 0.3137 0.5471 0.047 Uiso 1 calc . . R .
H4B H -0.2046 0.3279 0.5270 0.047 Uiso 1 calc . . R .
N2 N 0.378(2) 0.3697(8) 0.5299(15) 0.036(5) Uani 1 d . . . .
H2 H 0.4354 0.4098 0.5375 0.043 Uiso 1 calc . . R .
C1 C -0.040(2) 0.2476(9) 0.4027(13) 0.030(5) Uani 1 d . . D .
H1C H 0.0227 0.2152 0.4528 0.036 Uiso 1 calc . . R .
H1D H -0.0806 0.2234 0.3423 0.036 Uiso 1 calc . . R .
C2 C 0.469(3) 0.3285(11) 0.6170(17) 0.036(5) Uani 1 d . . . .
H2A H 0.5884 0.3348 0.6369 0.044 Uiso 1 calc . . R .
H2B H 0.4444 0.2801 0.6019 0.044 Uiso 1 calc . . R .
C3 C -0.187(2) 0.2745(10) 0.4182(16) 0.034(5) Uani 1 d . . D U
H3A H -0.2516 0.3060 0.3672 0.041 Uiso 1 calc . . R .
H3B H -0.2593 0.2363 0.4164 0.041 Uiso 1 calc . . R .
C4 C 0.228(3) 0.2823(10) 0.4107(18) 0.037(5) Uani 1 d . . . .
H4C H 0.2146 0.2638 0.3498 0.045 Uiso 1 calc . . R .
H4D H 0.2664 0.2452 0.4570 0.045 Uiso 1 calc . . R .
C5 C 0.428(4) 0.3473(12) 0.6992(18) 0.060(9) Uani 1 d . . . .
H5A H 0.4822 0.3155 0.7516 0.072 Uiso 1 calc . . R .
H5B H 0.4674 0.3935 0.7215 0.072 Uiso 1 calc . . R .
C6 C 0.361(3) 0.3407(11) 0.442(2) 0.046(7) Uani 1 d . . . .
H6A H 0.4672 0.3222 0.4487 0.056 Uiso 1 calc . . R .
H6B H 0.3269 0.3763 0.3931 0.056 Uiso 1 calc . . R .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N1 2.447(15) . ?
Pb1 N3 2.528(15) . ?
Pb1 N4 2.628(17) . ?
Pb1 N2 2.548(17) . ?
Pb2 I3 3.3028(12) . ?
Pb2 I1 3.3314(13) 1_455 ?
Pb2 I1 3.3879(12) 3_767 ?
Pb2 I5 3.1494(13) . ?
Pb2 I4 3.0447(13) . ?
Pb2 I6 3.1122(14) . ?
Pb3 I3 3.1099(12) . ?
Pb3 I3 3.3673(12) 3_767 ?
Pb3 I1 3.1806(13) . ?
Pb3 I5 3.3269(13) 1_655 ?
Pb3 I6 3.2474(13) . ?
Pb3 I2 3.1140(13) . ?
I3 Pb3 3.3673(12) 3_767 ?
I1 Pb2 3.3314(13) 1_655 ?
I1 Pb2 3.3879(12) 3_767 ?
I5 Pb3 3.3269(13) 1_455 ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 C5 1.46(4) . ?
N3 H3 0.9100 . ?
N3 C1 1.50(2) . ?
N3 C4 1.41(3) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N4 C3 1.47(3) . ?
N2 H2 0.9100 . ?
N2 C2 1.48(3) . ?
N2 C6 1.43(3) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C3 1.513(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C5 1.52(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C6 1.55(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 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
N1 Pb1 N3 99.4(5) . . ?
N1 Pb1 N4 80.0(6) . . ?
N1 Pb1 N2 70.0(7) . . ?
N3 Pb1 N4 69.4(6) . . ?
N3 Pb1 N2 68.6(6) . . ?
N2 Pb1 N4 122.4(6) . . ?
I3 Pb2 I1 82.95(3) . 3_767 ?
I3 Pb2 I1 80.41(3) . 1_455 ?
I1 Pb2 I1 87.31(3) 1_455 3_767 ?
I5 Pb2 I3 170.10(3) . . ?
I5 Pb2 I1 87.98(3) . 3_767 ?
I5 Pb2 I1 95.25(3) . 1_455 ?
I4 Pb2 I3 98.33(3) . . ?
I4 Pb2 I1 95.26(3) . 1_455 ?
I4 Pb2 I1 177.28(4) . 3_767 ?
I4 Pb2 I5 90.89(3) . . ?
I4 Pb2 I6 87.10(4) . . ?
I6 Pb2 I3 88.68(3) . . ?
I6 Pb2 I1 90.54(3) . 3_767 ?
I6 Pb2 I1 169.05(4) . 1_455 ?
I6 Pb2 I5 95.41(3) . . ?
I3 Pb3 I3 84.78(3) . 3_767 ?
I3 Pb3 I1 93.43(3) . . ?
I3 Pb3 I5 162.51(3) . 1_655 ?
I3 Pb3 I6 89.72(3) . . ?
I3 Pb3 I2 89.72(3) . . ?
I1 Pb3 I3 85.14(3) . 3_767 ?
I1 Pb3 I5 94.75(3) . 1_655 ?
I1 Pb3 I6 171.44(4) . . ?
I5 Pb3 I3 80.54(3) 1_655 3_767 ?
I6 Pb3 I3 87.22(3) . 3_767 ?
I6 Pb3 I5 80.16(3) . 1_655 ?
I2 Pb3 I3 171.04(4) . 3_767 ?
I2 Pb3 I1 88.13(3) . . ?
I2 Pb3 I5 105.96(3) . 1_655 ?
I2 Pb3 I6 99.85(4) . . ?
Pb2 I3 Pb3 94.89(3) . 3_767 ?
Pb3 I3 Pb2 89.77(3) . . ?
Pb3 I3 Pb3 95.22(3) . 3_767 ?
Pb2 I1 Pb2 92.69(3) 1_655 3_767 ?
Pb3 I1 Pb2 84.08(3) . 1_655 ?
Pb3 I1 Pb2 96.79(3) . 3_767 ?
Pb2 I5 Pb3 84.64(3) . 1_455 ?
Pb2 I6 Pb3 90.75(3) . . ?
Pb1 N1 H1A 108.8 . . ?
Pb1 N1 H1B 108.8 . . ?
H1A N1 H1B 107.7 . . ?
C5 N1 Pb1 113.7(15) . . ?
C5 N1 H1A 108.8 . . ?
C5 N1 H1B 108.8 . . ?
Pb1 N3 H3 105.1 . . ?
C1 N3 Pb1 113.7(11) . . ?
C1 N3 H3 105.1 . . ?
C4 N3 Pb1 114.4(13) . . ?
C4 N3 H3 105.1 . . ?
C4 N3 C1 112.1(15) . . ?
Pb1 N4 H4A 49.5 . . ?
Pb1 N4 H4B 111.2 . . ?
H4A N4 H4B 120.0 . . ?
C3 N4 Pb1 106.7(11) . . ?
C3 N4 H4A 120.0 . . ?
C3 N4 H4B 120.0 . . ?
Pb1 N2 H2 106.4 . . ?
C2 N2 Pb1 110.8(14) . . ?
C2 N2 H2 106.4 . . ?
C6 N2 Pb1 108.9(14) . . ?
C6 N2 H2 106.4 . . ?
C6 N2 C2 117.2(17) . . ?
N3 C1 H1C 109.5 . . ?
N3 C1 H1D 109.5 . . ?
N3 C1 C3 110.7(15) . . ?
H1C C1 H1D 108.1 . . ?
C3 C1 H1C 109.5 . . ?
C3 C1 H1D 109.5 . . ?
N2 C2 H2A 108.8 . . ?
N2 C2 H2B 108.8 . . ?
N2 C2 C5 113.8(18) . . ?
H2A C2 H2B 107.7 . . ?
C5 C2 H2A 108.8 . . ?
C5 C2 H2B 108.8 . . ?
N4 C3 C1 111.4(17) . . ?
N4 C3 H3A 109.3 . . ?
N4 C3 H3B 109.3 . . ?
C1 C3 H3A 109.3 . . ?
C1 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
N3 C4 H4C 109.2 . . ?
N3 C4 H4D 109.2 . . ?
N3 C4 C6 112.0(16) . . ?
H4C C4 H4D 107.9 . . ?
C6 C4 H4C 109.2 . . ?
C6 C4 H4D 109.2 . . ?
N1 C5 C2 109.1(17) . . ?
N1 C5 H5A 109.9 . . ?
N1 C5 H5B 109.9 . . ?
C2 C5 H5A 109.9 . . ?
C2 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N2 C6 C4 109.8(19) . . ?
N2 C6 H6A 109.7 . . ?
N2 C6 H6B 109.7 . . ?
C4 C6 H6A 109.7 . . ?
C4 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2107027'
loop_
_audit_author_name
_audit_author_address
'Mohamed Saber Lassoued'
;School of Chemistry Xian Key Laboratory of Sustainable Energy and Materials Chemistry
China
;
_audit_update_record             
;
2021-09-02 deposited with the CCDC.	2021-11-08 downloaded from the CCDC.
;
_audit_creation_date             2021-07-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'I8 Pb3, C6 H18 N4 Pb'
_chemical_formula_sum            'C6 H18 I8 N4 Pb4'
_chemical_formula_weight         1990.19
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   24.937(4)
_cell_length_b                   9.1908(14)
_cell_length_c                   26.522(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.213(2)
_cell_angle_gamma                90
_cell_volume                     6062.2(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6849
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      27.671
_cell_measurement_theta_min      2.2
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    30.299
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    4.361
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             6672
_exptl_crystal_size_max          0.632
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.086
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   0.23
_exptl_transmission_factor_min   0.02
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            13192
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.671
_diffrn_reflns_theta_min         1.638
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5385
_reflns_number_total             6849
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         10.676
_refine_diff_density_min         -3.436
_refine_diff_density_rms         0.739
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         6849
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0670
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1086P)²+497.4207P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.1922
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 C5-C4
 1.52 with sigma of 0.01
 C4-N3
 1.46 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 N2(H2), N1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C5(H5A,H5B), N3(H3A,H3B), C3(H3C,H3D), N4(H4A,H4B),
 C4(H4C,H4D), C6(H6A,H6B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.25106(2) 0.88710(7) 0.24867(3) 0.01427(18) Uani 1 1 d . . . . .
Pb2 Pb 0.16326(3) 0.64151(7) 0.11126(3) 0.01685(18) Uani 1 1 d . . . . .
Pb3 Pb 0.15550(3) 1.13359(7) 0.11949(3) 0.01790(19) Uani 1 1 d . . . . .
Pb4 Pb 0.92819(2) 0.65238(7) 0.04482(3) 0.01911(19) Uani 1 1 d . . . . .
I1 I 0.28657(4) 1.14519(12) 0.17546(5) 0.0154(3) Uani 1 1 d . . . . .
I2 I 0.28534(4) 0.62891(12) 0.17526(5) 0.0166(3) Uani 1 1 d . . . . .
I3 I 0.20382(4) 0.37872(11) 0.04923(5) 0.0161(3) Uani 1 1 d . . . . .
I4 I 0.12692(4) 0.87977(12) 0.19907(5) 0.0177(3) Uani 1 1 d . . . . .
I5 I 0.20974(4) 0.89084(12) 0.05038(5) 0.0199(3) Uani 1 1 d . . . . .
I6 I 0.06474(4) 0.66073(15) 0.03603(6) 0.0281(3) Uani 1 1 d . . . . .
I7 I 0.12863(4) 1.38782(12) 0.19977(5) 0.0188(3) Uani 1 1 d . . . . .
I8 I 0.04256(5) 1.14097(15) 0.07129(6) 0.0322(4) Uani 1 1 d . . . . .
C2 C 0.9127(8) 0.949(3) 0.1234(9) 0.038(6) Uani 1 1 d . . . . .
H2A H 0.9315 1.0365 0.1354 0.045 Uiso 1 1 calc R . . . .
H2B H 0.8868 0.9243 0.1476 0.045 Uiso 1 1 calc R . . . .
C1 C 0.9633(8) 0.749(3) 0.1685(8) 0.034(5) Uani 1 1 d . . . . .
H1A H 0.9296 0.7238 0.1824 0.040 Uiso 1 1 calc R . . . .
H1B H 0.9834 0.8119 0.1925 0.040 Uiso 1 1 calc R . . . .
N2 N 0.9689(6) 0.5120(19) 0.1231(6) 0.027(4) Uani 1 1 d . . . . .
H2 H 0.9967 0.4474 0.1115 0.032 Uiso 1 1 calc R . . . .
C5 C 0.9284(8) 0.418(3) 0.1467(9) 0.041(6) Uani 1 1 d D . . . .
H5A H 0.9084 0.4750 0.1697 0.049 Uiso 1 1 calc R . . . .
H5B H 0.9464 0.3394 0.1656 0.049 Uiso 1 1 calc R . . . .
N3 N 0.8623(6) 0.4709(18) 0.0742(8) 0.037(5) Uani 1 1 d D . . . .
H3A H 0.8390 0.5155 0.0928 0.044 Uiso 1 1 calc R . . . .
H3B H 0.8441 0.4310 0.0476 0.044 Uiso 1 1 calc R . . . .
C3 C 0.8836(9) 0.978(2) 0.0721(11) 0.043(6) Uani 1 1 d . . . . .
H3C H 0.8580 1.0566 0.0749 0.051 Uiso 1 1 calc R . . . .
H3D H 0.9093 1.0079 0.0484 0.051 Uiso 1 1 calc R . . . .
N4 N 0.8556(7) 0.8470(19) 0.0536(8) 0.038(5) Uani 1 1 d . . . . .
H4A H 0.8379 0.8639 0.0239 0.045 Uiso 1 1 calc R . . . .
H4B H 0.8323 0.8180 0.0754 0.045 Uiso 1 1 calc R . . . .
C4 C 0.8907(10) 0.357(2) 0.1043(9) 0.062(9) Uani 1 1 d D . . . .
H4C H 0.9113 0.2982 0.0823 0.074 Uiso 1 1 calc R . . . .
H4D H 0.8646 0.2945 0.1187 0.074 Uiso 1 1 calc R . . . .
C6 C 0.9955(8) 0.612(3) 0.1601(9) 0.036(5) Uani 1 1 d . . . . .
H6A H 1.0301 0.6393 0.1488 0.044 Uiso 1 1 calc R . . . .
H6B H 1.0018 0.5615 0.1921 0.044 Uiso 1 1 calc R . . . .
N1 N 0.9524(6) 0.827(2) 0.1201(8) 0.031(4) Uani 1 1 d . . . . .
H1 H 0.9864 0.8726 0.1129 0.038 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.2300(13) . ?
Pb1 I1 3.1859(13) 4_545 ?
Pb1 I2 3.2243(13) . ?
Pb1 I2 3.1785(13) 4 ?
Pb1 I4 3.2743(14) . ?
Pb1 I7 3.2045(13) 4_545 ?
Pb2 I2 3.3768(14) . ?
Pb2 I3 3.1318(13) . ?
Pb2 I4 3.3690(14) . ?
Pb2 I5 3.0784(14) . ?
Pb2 I6 3.0543(14) . ?
Pb3 I3 3.2140(13) 1_565 ?
Pb3 I4 3.2598(14) . ?
Pb3 I5 3.2451(14) . ?
Pb3 I7 3.2637(14) . ?
Pb3 I8 3.0070(14) . ?
Pb4 N2 2.588(15) . ?
Pb4 N3 2.505(15) . ?
Pb4 N4 2.567(17) . ?
Pb4 N1 2.596(19) . ?
I1 Pb1 3.1859(13) 4 ?
I2 Pb1 3.1785(13) 4_545 ?
I3 Pb3 3.2141(13) 1_545 ?
I7 Pb1 3.2044(13) 4 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.52(3) . ?
C2 N1 1.51(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C6 1.52(3) . ?
C1 N1 1.48(3) . ?
N2 H2 0.9800 . ?
N2 C5 1.50(3) . ?
N2 C6 1.47(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.517(10) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C4 1.466(10) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C3 N4 1.46(3) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N1 H1 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
I1 Pb1 I1 176.98(3) 4_545 . ?
I1 Pb1 I2 88.35(4) 4_545 . ?
I1 Pb1 I4 85.74(3) 4_545 . ?
I1 Pb1 I4 93.81(3) . . ?
I1 Pb1 I7 92.40(3) 4_545 4_545 ?
I2 Pb1 I1 88.62(4) 4 4_545 ?
I2 Pb1 I1 94.65(4) . . ?
I2 Pb1 I1 88.38(4) 4 . ?
I2 Pb1 I2 176.96(3) 4 . ?
I2 Pb1 I4 91.55(3) . . ?
I2 Pb1 I4 87.92(3) 4 . ?
I2 Pb1 I7 91.70(3) 4 4_545 ?
I7 Pb1 I1 88.03(3) 4_545 . ?
I7 Pb1 I2 88.73(3) 4_545 . ?
I7 Pb1 I4 178.11(4) 4_545 . ?
I3 Pb2 I2 85.62(3) . . ?
I3 Pb2 I4 167.99(4) . . ?
I4 Pb2 I2 87.32(3) . . ?
I5 Pb2 I2 85.92(3) . . ?
I5 Pb2 I3 98.62(4) . . ?
I5 Pb2 I4 90.55(4) . . ?
I6 Pb2 I2 169.29(4) . . ?
I6 Pb2 I3 88.67(4) . . ?
I6 Pb2 I4 99.77(4) . . ?
I6 Pb2 I5 85.99(4) . . ?
I3 Pb3 I4 170.46(4) 1_565 . ?
I3 Pb3 I5 87.99(4) 1_565 . ?
I3 Pb3 I7 88.86(3) 1_565 . ?
I4 Pb3 I7 91.42(4) . . ?
I5 Pb3 I4 89.64(3) . . ?
I5 Pb3 I7 167.10(4) . . ?
I8 Pb3 I3 96.72(4) . 1_565 ?
I8 Pb3 I4 92.80(4) . . ?
I8 Pb3 I5 101.05(4) . . ?
I8 Pb3 I7 91.74(4) . . ?
N2 Pb4 N1 68.6(6) . . ?
N3 Pb4 N2 69.3(5) . . ?
N3 Pb4 N4 87.3(6) . . ?
N3 Pb4 N1 107.0(6) . . ?
N4 Pb4 N2 120.8(6) . . ?
N4 Pb4 N1 68.0(5) . . ?
Pb1 I1 Pb1 91.51(3) 4 . ?
Pb1 I2 Pb1 91.75(3) 4_545 . ?
Pb1 I2 Pb2 90.52(3) . . ?
Pb1 I2 Pb2 93.10(3) 4_545 . ?
Pb2 I3 Pb3 94.97(4) . 1_545 ?
Pb1 I4 Pb2 89.81(3) . . ?
Pb3 I4 Pb1 90.01(3) . . ?
Pb3 I4 Pb2 86.26(4) . . ?
Pb2 I5 Pb3 91.54(4) . . ?
Pb1 I7 Pb3 92.65(3) 4 . ?
H2A C2 H2B 108.1 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 C3 110.5(19) . . ?
H1A C1 H1B 108.2 . . ?
C6 C1 H1A 109.7 . . ?
C6 C1 H1B 109.7 . . ?
N1 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
N1 C1 C6 109.8(18) . . ?
Pb4 N2 H2 107.2 . . ?
C5 N2 Pb4 112.6(12) . . ?
C5 N2 H2 107.2 . . ?
C6 N2 Pb4 110.9(13) . . ?
C6 N2 H2 107.2 . . ?
C6 N2 C5 111.5(17) . . ?
N2 C5 H5A 110.2 . . ?
N2 C5 H5B 110.2 . . ?
N2 C5 C4 107.7(19) . . ?
H5A C5 H5B 108.5 . . ?
C4 C5 H5A 110.2 . . ?
C4 C5 H5B 110.2 . . ?
Pb4 N3 H3A 109.7 . . ?
Pb4 N3 H3B 109.7 . . ?
H3A N3 H3B 108.2 . . ?
C4 N3 Pb4 110.0(12) . . ?
C4 N3 H3A 109.7 . . ?
C4 N3 H3B 109.7 . . ?
C2 C3 H3C 109.7 . . ?
C2 C3 H3D 109.7 . . ?
H3C C3 H3D 108.2 . . ?
N4 C3 C2 110(2) . . ?
N4 C3 H3C 109.7 . . ?
N4 C3 H3D 109.7 . . ?
Pb4 N4 H4A 110.4 . . ?
Pb4 N4 H4B 110.4 . . ?
C3 N4 Pb4 106.5(12) . . ?
C3 N4 H4A 110.4 . . ?
C3 N4 H4B 110.4 . . ?
H4A N4 H4B 108.6 . . ?
C5 C4 H4C 109.0 . . ?
C5 C4 H4D 109.0 . . ?
N3 C4 C5 112.9(19) . . ?
N3 C4 H4C 109.0 . . ?
N3 C4 H4D 109.0 . . ?
H4C C4 H4D 107.8 . . ?
C1 C6 H6A 108.8 . . ?
C1 C6 H6B 108.8 . . ?
N2 C6 C1 113.6(16) . . ?
N2 C6 H6A 108.8 . . ?
N2 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
Pb4 N1 H1 105.7 . . ?
C2 N1 Pb4 113.0(12) . . ?
C2 N1 H1 105.7 . . ?
C1 N1 Pb4 112.9(13) . . ?
C1 N1 C2 112.9(17) . . ?
C1 N1 H1 105.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb4 N2 C5 C4 36(2) . . . . ?
Pb4 N2 C6 C1 44(2) . . . . ?
Pb4 N3 C4 C5 52(2) . . . . ?
C2 C3 N4 Pb4 -61(2) . . . . ?
N2 C5 C4 N3 -60(3) . . . . ?
C5 N2 C6 C1 -83(2) . . . . ?
C3 C2 N1 Pb4 -24(2) . . . . ?
C3 C2 N1 C1 -153.8(19) . . . . ?
C6 C1 N1 Pb4 40.3(19) . . . . ?
C6 C1 N1 C2 170.0(18) . . . . ?
C6 N2 C5 C4 161.3(18) . . . . ?
N1 C2 C3 N4 59(3) . . . . ?
N1 C1 C6 N2 -58(2) . . . . ?
_olex2_submission_special_instructions 'No special instructions were received'
