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

data_mo_20180623x44_1_0m
_database_code_depnum_ccdc_archive 'CCDC 1975873'
loop_
_audit_author_name
_audit_author_address
'Pengfei Hao'
;School of Chemical and Material Science, Shanxi Normal University
China
;
_audit_update_record             
;
2020-01-07 deposited with the CCDC.	2020-10-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H34 I12 N6 O3 Pb4'
_chemical_formula_sum            'C20 H34 I12 N6 O3 Pb4'
_chemical_formula_weight         2758.13

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '
_symmetry_space_group_name_Hall  '-P 1  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9265(6)
_cell_length_b                   11.5631(9)
_cell_length_c                   15.8748(12)
_cell_angle_alpha                81.696(2)
_cell_angle_beta                 83.649(2)
_cell_angle_gamma                77.133(2)
_cell_volume                     1398.95(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25617
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      28.390

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184
_exptl_absorpt_coefficient_mu    18.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.078
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25156
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         28.39
_reflns_number_total             7030
_reflns_number_gt                4697
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0533P)²+4.8861P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00051(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6972
_refine_ls_number_parameters     213
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1180
_refine_ls_wR_factor_gt          0.1050
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.026
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.07179(4) 0.75280(3) 0.26554(2) 0.04832(12) Uani 1 1 d . . .
Pb2 Pb 0.57384(4) 0.75345(3) 0.26569(2) 0.04988(12) Uani 1 1 d . . .
I1 I 0.27770(9) 0.96200(6) 0.18075(4) 0.05773(18) Uani 1 1 d . . .
I2 I 0.74367(9) 0.93085(6) 0.35159(4) 0.06114(19) Uani 1 1 d . . .
I3 I 0.39580(9) 0.57931(6) 0.18049(4) 0.06114(19) Uani 1 1 d . . .
I4 I -0.12138(9) 0.54065(6) 0.34006(5) 0.0646(2) Uani 1 1 d . . .
I5 I 0.29206(9) 0.72329(8) 0.42491(4) 0.0661(2) Uani 1 1 d . . .
I6 I 0.84599(9) 0.78379(8) 0.09995(4) 0.0695(2) Uani 1 1 d . . .
N1 N 0.2154(12) 0.2105(8) 0.3917(5) 0.066(2) Uani 1 1 d . . .
C1 C 0.2072(15) 0.2915(10) 0.4446(6) 0.064(3) Uani 1 1 d . . .
H1 H 0.1188 0.2996 0.4883 0.077 Uiso 1 1 calc R . .
C2 C 0.3220(15) 0.3612(10) 0.4364(7) 0.064(3) Uani 1 1 d . . .
H2 H 0.3115 0.4188 0.4730 0.077 Uiso 1 1 calc R . .
O1 O 0.7484(11) 0.2707(8) 0.2546(6) 0.087(2) Uani 1 1 d . . .
N3 N 0.6729(17) 0.2173(9) 0.0982(6) 0.088(3) Uani 1 1 d . . .
C3 C 0.4542(15) 0.3479(9) 0.3746(6) 0.059(3) Uani 1 1 d . . .
H3 H 0.5388 0.3932 0.3712 0.071 Uiso 1 1 calc R . .
N2 N 0.5549(14) 0.2293(8) 0.1740(5) 0.074(3) Uani 1 1 d . . .
H2A H 0.4508 0.2193 0.1733 0.089 Uiso 1 1 calc R . .
C4 C 0.4648(13) 0.2678(8) 0.3166(6) 0.054(2) Uani 1 1 d . . .
C5 C 0.3434(13) 0.1989(9) 0.3288(6) 0.060(3) Uani 1 1 d . . .
H5 H 0.3495 0.1418 0.2922 0.072 Uiso 1 1 calc R . .
C7 C 0.6063(13) 0.2564(9) 0.2464(7) 0.058(2) Uani 1 1 d . . .
C10 C 0.7137(19) 0.3350(12) 0.0648(8) 0.091(4) Uani 1 1 d U . .
H10A H 0.7971 0.3266 0.0162 0.137 Uiso 1 1 calc R . .
H10B H 0.7609 0.3648 0.1084 0.137 Uiso 1 1 calc R . .
H10C H 0.6096 0.3900 0.0481 0.137 Uiso 1 1 calc R . .
C6 C 0.0871(17) 0.1332(14) 0.4038(9) 0.101(5) Uani 1 1 d . . .
H6A H 0.0048 0.1546 0.4509 0.151 Uiso 1 1 calc R . .
H6B H 0.1457 0.0512 0.4153 0.151 Uiso 1 1 calc R . .
H6C H 0.0276 0.1437 0.3528 0.151 Uiso 1 1 calc R . .
C9 C 0.844(3) 0.1278(16) 0.1168(12) 0.138(6) Uani 1 1 d U . .
H9A H 0.8410 0.0522 0.0995 0.207 Uiso 1 1 calc R . .
H9B H 0.8584 0.1178 0.1769 0.207 Uiso 1 1 calc R . .
H9C H 0.9397 0.1577 0.0856 0.207 Uiso 1 1 calc R . .
C8 C 0.585(3) 0.1791(17) 0.0352(11) 0.136(6) Uani 1 1 d U . .
H8A H 0.5703 0.0987 0.0534 0.205 Uiso 1 1 calc R . .
H8B H 0.6523 0.1820 -0.0187 0.205 Uiso 1 1 calc R . .
H8C H 0.4727 0.2311 0.0294 0.205 Uiso 1 1 calc R . .
O2 O 0.199(3) 0.308(2) 0.1450(14) 0.119(7) Uani 0.50 1 d PU . .


_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 3.1667(7) . ?
Pb1 I3 3.1881(8) . ?
Pb1 I4 3.1931(7) . ?
Pb1 I2 3.2420(8) 1_455 ?
Pb1 I1 3.2648(7) . ?
Pb1 I6 3.2749(8) 1_455 ?
Pb2 I2 3.2129(8) . ?
Pb2 I5 3.2160(7) . ?
Pb2 I3 3.2172(8) . ?
Pb2 I1 3.2223(8) . ?
Pb2 I4 3.2294(8) 1_655 ?
Pb2 I6 3.2424(8) . ?
I2 Pb1 3.2420(8) 1_655 ?
I4 Pb2 3.2294(8) 1_455 ?
I6 Pb1 3.2749(8) 1_655 ?
N1 C1 1.332(13) . ?
N1 C5 1.342(12) . ?
N1 C6 1.477(14) . ?
C1 C2 1.328(15) . ?
C1 H1 0.9300 . ?
C2 C3 1.352(14) . ?
C2 H2 0.9300 . ?
O1 C7 1.198(11) . ?
N3 N2 1.443(12) . ?
N3 C8 1.45(2) . ?
N3 C10 1.479(15) . ?
N3 C9 1.54(2) . ?
C3 C4 1.381(12) . ?
C3 H3 0.9300 . ?
N2 C7 1.361(12) . ?
N2 H2A 0.8600 . ?
C4 C5 1.362(13) . ?
C4 C7 1.489(14) . ?
C5 H5 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 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
I5 Pb1 I3 86.77(2) . . ?
I5 Pb1 I4 94.74(2) . . ?
I3 Pb1 I4 93.53(2) . . ?
I5 Pb1 I2 93.17(2) . 1_455 ?
I3 Pb1 I2 179.58(2) . 1_455 ?
I4 Pb1 I2 86.88(2) . 1_455 ?
I5 Pb1 I1 86.77(2) . . ?
I3 Pb1 I1 83.918(19) . . ?
I4 Pb1 I1 176.97(2) . . ?
I2 Pb1 I1 95.67(2) 1_455 . ?
I5 Pb1 I6 179.65(2) . 1_455 ?
I3 Pb1 I6 93.02(2) . 1_455 ?
I4 Pb1 I6 85.55(2) . 1_455 ?
I2 Pb1 I6 87.04(2) 1_455 1_455 ?
I1 Pb1 I6 92.93(2) . 1_455 ?
I2 Pb2 I5 93.78(2) . . ?
I2 Pb2 I3 178.79(2) . . ?
I5 Pb2 I3 85.46(2) . . ?
I2 Pb2 I1 94.88(2) . . ?
I5 Pb2 I1 86.67(2) . . ?
I3 Pb2 I1 84.142(19) . . ?
I2 Pb2 I4 86.76(2) . 1_655 ?
I5 Pb2 I4 96.03(2) . 1_655 ?
I3 Pb2 I4 94.25(2) . 1_655 ?
I1 Pb2 I4 176.75(2) . 1_655 ?
I2 Pb2 I6 88.08(2) . . ?
I5 Pb2 I6 177.658(19) . . ?
I3 Pb2 I6 92.67(2) . . ?
I1 Pb2 I6 91.75(2) . . ?
I4 Pb2 I6 85.50(2) 1_655 . ?
Pb2 I1 Pb1 75.718(17) . . ?
Pb2 I2 Pb1 75.347(17) . 1_655 ?
Pb1 I3 Pb2 76.862(17) . . ?
Pb1 I4 Pb2 75.794(18) . 1_455 ?
Pb1 I5 Pb2 77.182(17) . . ?
Pb2 I6 Pb1 74.503(17) . 1_655 ?
C1 N1 C5 119.0(9) . . ?
C1 N1 C6 120.2(10) . . ?
C5 N1 C6 120.8(9) . . ?
C2 C1 N1 121.7(10) . . ?
C2 C1 H1 119.1 . . ?
N1 C1 H1 119.1 . . ?
C1 C2 C3 119.7(10) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
N2 N3 C8 107.4(12) . . ?
N2 N3 C10 109.2(9) . . ?
C8 N3 C10 109.0(12) . . ?
N2 N3 C9 111.8(10) . . ?
C8 N3 C9 111.0(13) . . ?
C10 N3 C9 108.4(12) . . ?
C2 C3 C4 120.5(10) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C7 N2 N3 120.8(10) . . ?
C7 N2 H2A 119.6 . . ?
N3 N2 H2A 119.6 . . ?
C5 C4 C3 116.7(10) . . ?
C5 C4 C7 122.6(9) . . ?
C3 C4 C7 120.7(9) . . ?
N1 C5 C4 122.2(9) . . ?
N1 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
O1 C7 N2 125.1(11) . . ?
O1 C7 C4 122.3(10) . . ?
N2 C7 C4 112.7(9) . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

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
N2 H2A O2 0.86 2.10 2.83(2) 143.3 .

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.39
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.903
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.199
_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2016978'
loop_
_audit_author_name
_audit_author_address
'Jun-ju Shen'
;shanxi normal university
China
;
_audit_update_record             
;
2020-07-17 deposited with the CCDC.	2020-10-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H17 N3 O, I3 Pb, O'
_chemical_formula_sum            'C10 H17 I3 N3 O2 Pb'
_chemical_formula_weight         799.16

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 0.0061 0.0033 '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'
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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '
_symmetry_space_group_name_Hall  '-p 2ybc  '

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

_cell_length_a                   14.2985(9)
_cell_length_b                   7.9199(5)
_cell_length_c                   17.4889(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.076(2)
_cell_angle_gamma                90.00
_cell_volume                     1975.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    9869
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      28.34

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.018
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_absorpt_coefficient_mu    13.230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26964
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.33
_diffrn_reflns_theta_max         28.37
_reflns_number_total             4928
_reflns_number_gt                3985
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0475P)²+1.1812P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4928
_refine_ls_number_parameters     176
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0960
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_restrained_S_all      1.305
_refine_ls_shift/su_max          0.004
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.000829(15) 0.08246(3) 0.249737(12) 0.03743(9) Uani 1 1 d . . .
I1 I 1.11516(3) -0.16828(5) 0.14481(2) 0.04176(11) Uani 1 1 d . . .
I2 I 0.92409(3) 0.34225(5) 0.11310(2) 0.04728(12) Uani 1 1 d . . .
I3 I 0.82240(3) -0.16821(5) 0.22951(3) 0.04826(13) Uani 1 1 d . . .
C1 C 0.1079(5) 0.1689(9) -0.0167(4) 0.0569(19) Uani 1 1 d . . .
H1A H 0.1185 0.0594 -0.0380 0.085 Uiso 1 1 calc R . .
H1B H 0.0863 0.2448 -0.0570 0.085 Uiso 1 1 calc R . .
H1C H 0.0613 0.1604 0.0200 0.085 Uiso 1 1 calc R . .
C2 C 0.2004(4) 0.3915(9) 0.0486(4) 0.0451(14) Uani 1 1 d . . .
H2 H 0.1469 0.4586 0.0443 0.054 Uiso 1 1 calc R . .
C3 C 0.2826(4) 0.4556(8) 0.0826(4) 0.0467(15) Uani 1 1 d . . .
H3 H 0.2849 0.5660 0.1008 0.056 Uiso 1 1 calc R . .
C4 C 0.3611(4) 0.3558(7) 0.0895(4) 0.0423(14) Uani 1 1 d . . .
C5 C 0.3522(5) 0.1895(8) 0.0591(4) 0.0548(18) Uani 1 1 d . . .
H5 H 0.4045 0.1195 0.0608 0.066 Uiso 1 1 calc RD . .
C6 C 0.2724(5) 0.1336(9) 0.0290(4) 0.0542(17) Uani 1 1 d . . .
H6 H 0.2677 0.0222 0.0122 0.065 Uiso 1 1 calc R . .
C7 C 0.4512(4) 0.4306(8) 0.1266(4) 0.0457(15) Uani 1 1 d . . .
C8 C 0.5936(6) 0.4493(11) 0.2567(4) 0.069(2) Uani 1 1 d . . .
H8A H 0.5580 0.5518 0.2506 0.103 Uiso 1 1 calc R . .
H8B H 0.6543 0.4738 0.2811 0.103 Uiso 1 1 calc R . .
H8C H 0.5614 0.3714 0.2877 0.103 Uiso 1 1 calc R . .
C9 C 0.6626(5) 0.2157(10) 0.1914(6) 0.072(2) Uani 1 1 d . . .
H9A H 0.6287 0.1344 0.2193 0.109 Uiso 1 1 calc R . .
H9B H 0.7204 0.2430 0.2199 0.109 Uiso 1 1 calc R . .
H9C H 0.6757 0.1693 0.1426 0.109 Uiso 1 1 calc R . .
C10 C 0.6523(6) 0.4903(11) 0.1275(5) 0.075(2) Uani 1 1 d . . .
H10A H 0.6536 0.4405 0.0776 0.113 Uiso 1 1 calc R . .
H10B H 0.7153 0.5110 0.1481 0.113 Uiso 1 1 calc R . .
H10C H 0.6185 0.5950 0.1236 0.113 Uiso 1 1 calc R . .
N1 N 0.1969(3) 0.2340(7) 0.0217(3) 0.0416(11) Uani 1 1 d . . .
N2 N 0.5178(4) 0.3151(7) 0.1448(4) 0.0541(15) Uani 1 1 d . . .
H2A H 0.5080 0.2096 0.1357 0.065 Uiso 1 1 calc RD . .
N3 N 0.6047(4) 0.3723(8) 0.1794(4) 0.0523(14) Uani 1 1 d . . .
O1 O 0.4561(4) 0.5826(6) 0.1410(3) 0.0658(15) Uani 1 1 d D . .
O2 O 0.4130(6) 0.8234(7) 0.0155(5) 0.103(2) Uani 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I2 3.1875(5) 2_745 ?
Pb1 I3 3.2077(5) 2_755 ?
Pb1 I1 3.2265(5) . ?
Pb1 I3 3.2322(5) . ?
Pb1 I1 3.2379(5) 2_755 ?
Pb1 I2 3.2825(5) . ?
I1 Pb1 3.2379(5) 2_745 ?
I2 Pb1 3.1875(5) 2_755 ?
I3 Pb1 3.2077(5) 2_745 ?
C1 N1 1.488(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.333(9) . ?
C2 C3 1.376(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.422(8) . ?
C4 C7 1.520(8) . ?
C5 C6 1.301(9) . ?
C5 H5 0.9300 . ?
C6 N1 1.340(9) . ?
C6 H6 0.9300 . ?
C7 O1 1.231(8) . ?
C7 N2 1.343(8) . ?
C8 N3 1.502(9) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N3 1.498(9) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 N3 1.499(10) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
N2 N3 1.417(7) . ?
N2 H2A 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
I2 Pb1 I3 93.539(13) 2_745 2_755 ?
I2 Pb1 I1 84.462(12) 2_745 . ?
I3 Pb1 I1 90.929(13) 2_755 . ?
I2 Pb1 I3 86.375(13) 2_745 . ?
I3 Pb1 I3 179.756(9) 2_755 . ?
I1 Pb1 I3 89.290(12) . . ?
I2 Pb1 I1 95.393(13) 2_745 2_755 ?
I3 Pb1 I1 89.521(12) 2_755 2_755 ?
I1 Pb1 I1 179.535(12) . 2_755 ?
I3 Pb1 I1 90.260(12) . 2_755 ?
I2 Pb1 I2 177.782(13) 2_745 . ?
I3 Pb1 I2 85.207(12) 2_755 . ?
I1 Pb1 I2 97.378(13) . . ?
I3 Pb1 I2 94.871(13) . . ?
I1 Pb1 I2 82.776(12) 2_755 . ?
Pb1 I1 Pb1 75.554(10) . 2_745 ?
Pb1 I2 Pb1 75.462(10) 2_755 . ?
Pb1 I3 Pb1 75.891(11) 2_745 . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 120.5(6) . . ?
N1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C3 C2 119.6(6) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 116.8(6) . . ?
C3 C4 C7 118.4(6) . . ?
C5 C4 C7 124.8(5) . . ?
C6 C5 C4 121.3(6) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 N1 121.0(7) . . ?
C5 C6 H6 119.5 . . ?
N1 C6 H6 119.5 . . ?
O1 C7 N2 126.1(6) . . ?
O1 C7 C4 120.2(6) . . ?
N2 C7 C4 113.6(5) . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C2 N1 C6 120.8(6) . . ?
C2 N1 C1 119.6(5) . . ?
C6 N1 C1 119.7(6) . . ?
C7 N2 N3 118.0(5) . . ?
C7 N2 H2A 121.0 . . ?
N3 N2 H2A 121.0 . . ?
N2 N3 C9 104.7(5) . . ?
N2 N3 C10 111.3(6) . . ?
C9 N3 C10 109.3(7) . . ?
N2 N3 C8 111.6(6) . . ?
C9 N3 C8 107.6(6) . . ?
C10 N3 C8 111.9(6) . . ?

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
N2 H2A O2 0.86 2.96 3.229(10) 100.6 3_665

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.37
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.525
_refine_diff_density_min         -2.021
_refine_diff_density_rms         0.686
