# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# 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. 
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#######################################################################

data_2
_audit_block_doi                 10.5517/ccdc.csd.cc23xzdf
_database_code_depnum_ccdc_archive 'CCDC 1964265'
loop_
_audit_author_name
_audit_author_address
'Dongying Fu'
;Shangxi University
China
;
_audit_update_record             
;
2019-11-07 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;
_audit_creation_date             2019-11-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(I28 Pb8), C6 H18 N2, C H6 N'
_chemical_formula_sum            'C7 H24 I7 N3 Pb2'
_chemical_formula_weight         1452.97
_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'

_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      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, 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'
'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, y, z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   12.7220(5)
_cell_length_b                   12.5151(5)
_cell_length_c                   34.3778(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5473.5(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3553
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.37
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.179
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.1030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1367 before and 0.0738 after correction. The Ratio of minimum to maximum transmission is 0.3958. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.526
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4976
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            18778
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.375
_diffrn_reflns_theta_min         2.283
_diffrn_ambient_temperature      250.15
_diffrn_detector                 'Bruker APEX3 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX3 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1883
_reflns_number_total             2963
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.895
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.299
_refine_ls_extinction_coef       0.000061(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2963
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0537
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0734P)²+125.6864P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1663
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1_$1-N1_$1
 1.47 with sigma of 0.02
 C3-C2 = C3-C4
 1.5 with sigma of 0.02
 C3_$2-C4
 1.5 with sigma of 0.02
 C5-C3
 1.5 with sigma of 0.02
 H3b_$2-H3b
 2.1 with sigma of 0.02
 C5-C2
 2.3 with sigma of 0.04
 C3_$2-C3
 2.3 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N1 \\sim C1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N2 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
4. Others
 Fixed Sof: H3a(0.5) H4a(0.5) H4b(0.5) C5(0.5) H5a(0.5) H5b(0.5) H5c(0.5)
 C1(0.5) H1a(0.5) H1b(0.5) H1c(0.5) N1(0.5) H1d(0.5) H1e(0.5) H1f(0.5)
5.a Riding coordinates:
 C3(H3a,H3b)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C4(H4a,H4b)
5.c Idealised Me refined as rotating group:
 N2(H2c,H2d,H2e), C5(H5a,H5b,H5c), C1(H1a,H1b,H1c), N1(H1d,H1e,H1f)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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
I1 I 0.500000 0.06483(3) 0.67599(2) 0.05756(19) Uani 1 2 d S T P . .
Pb1 Pb 0.500000 0.31459(2) 0.65615(2) 0.03709(8) Uani 1 2 d S T P . .
I2 I 0.500000 0.35409(8) 0.750000 0.0713(3) Uani 1 4 d S T P . .
Pb2 Pb 0.500000 0.81556(2) 0.65539(2) 0.03996(9) Uani 1 2 d S T P . .
I3 I 0.500000 0.25970(5) 0.56857(2) 0.0632(2) Uani 1 2 d S T P . .
I4 I 0.500000 0.56560(4) 0.64303(3) 0.0791(3) Uani 1 2 d S T P . .
I5 I 0.500000 0.86706(7) 0.56775(2) 0.0893(3) Uani 1 2 d S T P . .
I6 I 0.25029(3) 0.81641(4) 0.65677(2) 0.06369(16) Uani 1 1 d . . . . .
I7 I 0.500000 0.77818(8) 0.750000 0.0698(3) Uani 1 4 d S T P . .
C2 C 0.2251(10) 0.0091(7) 0.5582(3) 0.1685(11) Uani 1 1 d D U . . .
H2A H 0.257950 -0.059701 0.552133 0.202 Uiso 1 1 calc R . . . .
H2B H 0.151263 -0.003240 0.565014 0.202 Uiso 1 1 calc R . . . .
N2 N 0.2884(8) 0.0694(6) 0.5950(3) 0.140(2) Uani 1 1 d . U . . .
H2C H 0.355676 0.081088 0.588179 0.168 Uiso 1 1 calc GR . . . .
H2D H 0.286397 0.027196 0.616205 0.168 Uiso 1 1 calc GR . . . .
H2E H 0.256965 0.132089 0.600366 0.168 Uiso 1 1 calc GR . . . .
C3 C 0.2333(6) 0.0827(3) 0.52485(13) 0.1722(8) Uani 1 1 d D U . . .
H3A H 0.222778 0.159069 0.519901 0.207 Uiso 0.5 1 d R . . A -1
H3B H 0.304968 0.062519 0.517381 0.207 Uiso 1 1 d DR . . B .
C4 C 0.1775(8) 0.000000 0.500000 0.1728(12) Uani 1 2 d DS TU P B .
H4A H 0.131357 0.039916 0.482396 0.207 Uiso 0.5 1 calc R . . . .
H4B H 0.131357 -0.039916 0.517604 0.207 Uiso 0.5 1 calc R . . . .
C5 C 0.1719(11) 0.1776(7) 0.5366(6) 0.177(2) Uani 0.5 1 d D U . B -1
H5A H 0.097759 0.159496 0.537326 0.266 Uiso 0.5 1 calc GR . . B -1
H5B H 0.183264 0.234788 0.518078 0.266 Uiso 0.5 1 calc GR . . B -1
H5C H 0.194279 0.200721 0.562266 0.266 Uiso 0.5 1 calc GR . . B -1
C1 C 0.2703(12) -0.0234(7) 0.7460(12) 0.258(4) Uani 0.5 1 d D U . C -1
H1A H 0.209426 -0.069640 0.743592 0.388 Uiso 0.5 1 calc GR . . C -1
H1B H 0.301925 -0.033358 0.771464 0.388 Uiso 0.5 1 calc GR . . C -1
H1C H 0.321090 -0.041233 0.726027 0.388 Uiso 0.5 1 calc GR . . C -1
N1 N 0.2375(10) 0.0890(6) 0.7416(7) 0.251(4) Uani 0.5 1 d D U . C -1
H1D H 0.270746 0.129540 0.759342 0.301 Uiso 0.5 1 calc GR . . C -1
H1E H 0.167541 0.094124 0.745101 0.301 Uiso 0.5 1 calc GR . . C -1
H1F H 0.254066 0.111940 0.717526 0.301 Uiso 0.5 1 calc GR . . C -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0781(4) 0.02300(19) 0.0716(4) 0.0015(2) 0.000 0.000
Pb1 0.03082(15) 0.03027(12) 0.05017(18) 0.00005(12) 0.000 0.000
I2 0.0987(7) 0.0733(5) 0.0420(5) 0.000 0.000 0.000
Pb2 0.03260(16) 0.03318(13) 0.05409(19) -0.00016(12) 0.000 0.000
I3 0.0719(4) 0.0722(3) 0.0455(4) 0.0026(3) 0.000 0.000
I4 0.1106(6) 0.0239(2) 0.1027(5) -0.0006(3) 0.000 0.000
I5 0.1156(6) 0.0968(5) 0.0554(4) 0.0040(4) 0.000 0.000
I6 0.0249(2) 0.0756(3) 0.0906(4) 0.0000(2) -0.0022(2) -0.00280(18)
I7 0.0913(7) 0.0701(5) 0.0480(5) 0.000 0.000 0.000
C2 0.1683(19) 0.1624(18) 0.1749(19) 0.0096(19) -0.0033(18) -0.0118(18)
N2 0.141(4) 0.134(4) 0.144(4) 0.009(3) -0.013(4) -0.025(3)
C3 0.1727(14) 0.1653(14) 0.1787(14) 0.0097(14) -0.0018(14) -0.0057(14)
C4 0.174(2) 0.165(2) 0.179(2) 0.010(2) 0.000 0.000
C5 0.178(4) 0.169(4) 0.184(4) 0.007(4) -0.002(4) -0.005(4)
C1 0.203(7) 0.415(8) 0.157(8) 0.087(8) 0.119(8) 0.190(7)
N1 0.203(7) 0.399(8) 0.151(8) 0.095(8) 0.115(7) 0.204(6)

_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
I1 Pb1 3.1993(5) . ?
I1 Pb2 3.1991(5) 1_545 ?
Pb1 I2 3.2640(4) . ?
Pb1 I3 3.0881(7) . ?
Pb1 I4 3.1736(6) . ?
Pb1 I6 3.1843(4) 5_545 ?
Pb1 I6 3.1843(4) 15_545 ?
Pb2 I4 3.1570(6) . ?
Pb2 I5 3.0810(9) . ?
Pb2 I6 3.1772(4) . ?
Pb2 I6 3.1772(4) 11_655 ?
Pb2 I7 3.2860(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 N2 1.678(14) . ?
C2 C3 1.475(9) . ?
N2 H2C 0.9000 . ?
N2 H2D 0.9000 . ?
N2 H2E 0.9000 . ?
C3 H3A 0.9801 . ?
C3 H3B 0.9798 . ?
C3 C4 1.519(7) . ?
C3 C5 1.479(11) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 H3A 0.8969 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C1 N1 1.476(12) . ?
N1 H1D 0.9000 . ?
N1 H1E 0.9000 . ?
N1 H1F 0.9000 . ?

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
Pb2 I1 Pb1 154.90(3) 1_545 . ?
I1 Pb1 I2 86.40(2) . . ?
I3 Pb1 I1 89.457(18) . . ?
I3 Pb1 I2 175.86(2) . . ?
I3 Pb1 I4 94.68(2) . . ?
I3 Pb1 I6 90.467(11) . 15_545 ?
I3 Pb1 I6 90.467(11) . 5_545 ?
I4 Pb1 I1 175.86(2) . . ?
I4 Pb1 I2 89.46(2) . . ?
I4 Pb1 I6 89.651(9) . 15_545 ?
I4 Pb1 I6 89.651(9) . 5_545 ?
I6 Pb1 I1 90.317(9) 15_545 . ?
I6 Pb1 I1 90.317(9) 5_545 . ?
I6 Pb1 I2 89.557(11) 5_545 . ?
I6 Pb1 I2 89.557(11) 15_545 . ?
I6 Pb1 I6 178.88(2) 15_545 5_545 ?
Pb1 I2 Pb1 162.58(4) 10_557 . ?
I1 Pb2 I7 85.39(2) 1_565 . ?
I4 Pb2 I1 174.94(2) . 1_565 ?
I4 Pb2 I6 90.304(9) . 11_655 ?
I4 Pb2 I6 90.305(9) . . ?
I4 Pb2 I7 89.55(2) . . ?
I5 Pb2 I1 90.71(2) . 1_565 ?
I5 Pb2 I4 94.34(2) . . ?
I5 Pb2 I6 90.800(11) . 11_655 ?
I5 Pb2 I6 90.800(11) . . ?
I5 Pb2 I7 176.11(2) . . ?
I6 Pb2 I1 89.625(9) 11_655 1_565 ?
I6 Pb2 I1 89.624(9) . 1_565 ?
I6 Pb2 I6 178.24(2) 11_655 . ?
I6 Pb2 I7 89.177(11) 11_655 . ?
I6 Pb2 I7 89.177(11) . . ?
Pb2 I4 Pb1 164.10(3) . . ?
Pb2 I6 Pb1 178.62(2) . 5_455 ?
Pb2 I7 Pb2 163.63(3) . 10_557 ?
H2A C2 H2B 108.7 . . ?
N2 C2 H2A 110.6 . . ?
N2 C2 H2B 110.6 . . ?
C3 C2 H2A 110.6 . . ?
C3 C2 H2B 110.6 . . ?
C3 C2 N2 105.8(7) . . ?
C2 N2 H2C 109.5 . . ?
C2 N2 H2D 109.5 . . ?
C2 N2 H2E 109.5 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
C2 C3 H3A 137.2 . . ?
C2 C3 H3B 96.3 . . ?
C2 C3 C4 88.8(5) . . ?
C2 C3 C5 104.5(8) . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3A 120.2 . . ?
C4 C3 H3B 96.4 . . ?
C5 C3 H3A 36.1 . . ?
C5 C3 H3B 140.4 . . ?
C5 C3 C4 117.0(8) . . ?
C3 C4 C3 124.2(9) . 3_556 ?
C3 C4 H4A 106.3 . . ?
C3 C4 H4A 106.3 3_556 . ?
C3 C4 H4B 106.3 3_556 . ?
C3 C4 H4B 106.3 . . ?
H4A C4 H4B 106.4 . . ?
C3 C5 H3A 40.1 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H3A C5 H5A 131.1 . . ?
H3A C5 H5B 70.2 . . ?
H3A C5 H5C 116.6 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
C1 N1 H1F 109.5 . . ?
H1D N1 H1E 109.5 . . ?
H1D N1 H1F 109.5 . . ?
H1E N1 H1F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C3 C4 C3 -94.0(5) . . . 3_556 ?
N2 C2 C3 C4 176.6(8) . . . . ?
N2 C2 C3 C5 -65.8(10) . . . . ?
C5 C3 C4 C3 160.3(8) . . . 3_556 ?

_olex2_submission_special_instructions 'No special instructions were received'
