# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2023

####################################################################### 
# 
# 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_1Rac
_database_code_depnum_ccdc_archive 'CCDC 2265467'
loop_
_audit_author_name
_audit_author_address
'Cheng-Dong Liu'
;Southeast University
China
;
_audit_update_record             
;
2023-05-25 deposited with the CCDC.	2023-07-13 downloaded from the CCDC.
;
_audit_creation_date             2023-02-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 H12 N O2), I4 Pb'
_chemical_formula_sum            'C12 H24 I4 N2 O4 Pb'
_chemical_formula_weight         975.12
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c h o n i Pb'
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'
O O 0.0106 0.0060 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   13.0681(6)
_cell_length_b                   26.5774(15)
_cell_length_c                   6.5224(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2265.33(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6613
_cell_measurement_temperature    300.1(4)
_cell_measurement_theta_max      30.0470
_cell_measurement_theta_min      3.0450
_shelx_estimated_absorpt_T_max   0.182
_shelx_estimated_absorpt_T_min   0.182
_exptl_absorpt_coefficient_mu    12.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.859
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            27504
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.432
_diffrn_reflns_theta_min         3.066
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.1(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -2.00  80.00   0.50    0.50    --    9.28  77.00  90.00  164
  2  ω     -2.00  71.00   0.50    0.50    --    9.28  77.00 -30.00  146
  3  ω     -2.00  76.00   0.50    0.50    --    9.28  77.00-150.00  156
  4  ω    -22.00  21.00   0.50    0.50    --   -9.83  77.00 -90.00   86
  5  ω    -29.00  51.00   0.50    0.50    --   -9.83  77.00  30.00  160
  6  ω    -27.00  55.00   0.50    0.50    --   -9.83  77.00 150.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0048853000
_diffrn_orient_matrix_UB_12      0.0157138000
_diffrn_orient_matrix_UB_13      -0.0436955000
_diffrn_orient_matrix_UB_21      -0.0518640000
_diffrn_orient_matrix_UB_22      -0.0046900000
_diffrn_orient_matrix_UB_23      -0.0128248000
_diffrn_orient_matrix_UB_31      -0.0152376000
_diffrn_orient_matrix_UB_32      0.0210424000
_diffrn_orient_matrix_UB_33      0.0297358000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1969
_reflns_number_total             3154
_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       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.002
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         3154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0411
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0182P)²+5.5286P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0800
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C5(H5A,H5B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_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
N1 N 0.0967(5) 0.1354(3) 0.3594(11) 0.068(2) Uani 1 1 d . . . . .
H1A H 0.073160 0.155393 0.458242 0.082 Uiso 1 1 calc R U . . .
H1B H 0.043962 0.126185 0.281544 0.082 Uiso 1 1 calc R U . . .
C2 C 0.1878(6) 0.0557(4) 0.2828(14) 0.068(3) Uani 1 1 d . . . . .
H2 H 0.226755 0.028966 0.350896 0.082 Uiso 1 1 calc R U . . .
C5 C 0.1728(6) 0.1635(3) 0.2318(12) 0.060(2) Uani 1 1 d . . . . .
H5A H 0.140095 0.192744 0.171569 0.072 Uiso 1 1 calc R U . . .
H5B H 0.228284 0.175127 0.318378 0.072 Uiso 1 1 calc R U . . .
C6 C 0.1447(7) 0.0900(4) 0.4521(12) 0.070(3) Uani 1 1 d . . . . .
H6A H 0.094180 0.071756 0.531698 0.084 Uiso 1 1 calc R U . . .
H6B H 0.199450 0.100153 0.543619 0.084 Uiso 1 1 calc R U . . .
C3 C 0.2634(6) 0.0852(4) 0.1485(13) 0.065(2) Uani 1 1 d . . . . .
H3A H 0.323005 0.094327 0.228927 0.078 Uiso 1 1 calc R U . . .
H3B H 0.285843 0.064310 0.035299 0.078 Uiso 1 1 calc R U . . .
C4 C 0.2142(5) 0.1313(3) 0.0678(11) 0.0483(18) Uani 1 1 d . . . . .
H4A H 0.264009 0.150336 -0.010659 0.058 Uiso 1 1 calc R U . . .
H4B H 0.159155 0.121850 -0.024236 0.058 Uiso 1 1 calc R U . . .
O2 O 0.1228(5) 0.0168(3) -0.0212(13) 0.104(3) Uani 1 1 d . . . . .
Pb1 Pb -0.08096(3) 0.250000 0.80874(5) 0.03726(12) Uani 1 2 d S T P . .
I3 I -0.08148(5) 0.250000 0.31022(9) 0.04803(19) Uani 1 2 d S T P . .
I2 I -0.06724(4) 0.13059(2) 0.83955(9) 0.06185(18) Uani 1 1 d . . . . .
I1 I 0.17707(5) 0.250000 0.72161(10) 0.04836(19) Uani 1 2 d S T P . .
O1 O 0.0198(6) 0.0253(4) 0.2410(12) 0.116(3) Uani 1 1 d . . . . .
H1 H -0.020941 0.014331 0.156454 0.174 Uiso 1 1 calc R U . . .
C1 C 0.1054(7) 0.0306(3) 0.1588(16) 0.064(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C5 1.496(10) . ?
N1 C6 1.488(11) . ?
C2 H2 0.9800 . ?
C2 C6 1.539(12) . ?
C2 C3 1.536(11) . ?
C2 C1 1.502(13) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.473(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.480(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
O2 C1 1.251(11) . ?
Pb1 I3 3.2709(7) 1_556 ?
Pb1 I3 3.2515(7) . ?
Pb1 I2 3.1851(6) 8_565 ?
Pb1 I2 3.1851(6) . ?
Pb1 I1 3.4194(7) . ?
Pb1 I1 3.1684(7) 6_557 ?
O1 H1 0.8200 . ?
O1 C1 1.249(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
H1A N1 H1B 108.1 . . ?
C5 N1 H1A 109.6 . . ?
C5 N1 H1B 109.6 . . ?
C6 N1 H1A 109.6 . . ?
C6 N1 H1B 109.6 . . ?
C6 N1 C5 110.5(6) . . ?
C6 C2 H2 107.1 . . ?
C3 C2 H2 107.1 . . ?
C3 C2 C6 109.9(8) . . ?
C1 C2 H2 107.1 . . ?
C1 C2 C6 112.8(7) . . ?
C1 C2 C3 112.4(8) . . ?
N1 C5 H5A 109.4 . . ?
N1 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
C4 C5 N1 111.0(7) . . ?
C4 C5 H5A 109.4 . . ?
C4 C5 H5B 109.4 . . ?
N1 C6 C2 110.1(6) . . ?
N1 C6 H6A 109.6 . . ?
N1 C6 H6B 109.6 . . ?
C2 C6 H6A 109.6 . . ?
C2 C6 H6B 109.6 . . ?
H6A C6 H6B 108.2 . . ?
C2 C3 H3A 109.6 . . ?
C2 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 C2 110.3(6) . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
C5 C4 C3 112.4(7) . . ?
C5 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
I3 Pb1 I3 179.76(3) . 1_556 ?
I3 Pb1 I1 99.687(18) 1_556 . ?
I3 Pb1 I1 80.553(18) . . ?
I2 Pb1 I3 86.389(13) 8_565 1_556 ?
I2 Pb1 I3 86.389(13) . 1_556 ?
I2 Pb1 I3 93.625(13) 8_565 . ?
I2 Pb1 I3 93.624(13) . . ?
I2 Pb1 I2 170.30(2) 8_565 . ?
I2 Pb1 I1 87.420(12) 8_565 . ?
I2 Pb1 I1 87.420(12) . . ?
I1 Pb1 I3 86.298(18) 6_557 . ?
I1 Pb1 I3 93.462(19) 6_557 1_556 ?
I1 Pb1 I2 93.446(12) 6_557 . ?
I1 Pb1 I2 93.447(12) 6_557 8_565 ?
I1 Pb1 I1 166.852(12) 6_557 . ?
Pb1 I3 Pb1 179.76(3) . 1_554 ?
Pb1 I1 Pb1 174.01(2) 6_657 . ?
C1 O1 H1 109.5 . . ?
O2 C1 C2 120.3(8) . . ?
O1 C1 C2 117.4(9) . . ?
O1 C1 O2 122.2(10) . . ?

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
N1 C5 C4 C3 -57.9(9) . . . . ?
C2 C3 C4 C5 55.9(9) . . . . ?
C5 N1 C6 C2 -58.0(9) . . . . ?
C6 N1 C5 C4 58.6(9) . . . . ?
C6 C2 C3 C4 -54.4(9) . . . . ?
C6 C2 C1 O2 154.5(9) . . . . ?
C6 C2 C1 O1 -24.0(12) . . . . ?
C3 C2 C6 N1 56.1(9) . . . . ?
C3 C2 C1 O2 29.5(12) . . . . ?
C3 C2 C1 O1 -148.9(9) . . . . ?
C1 C2 C6 N1 -70.1(10) . . . . ?
C1 C2 C3 C4 72.0(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.028
_oxdiff_exptl_absorpt_empirical_full_min 0.473
####################################################################### 
# 
# 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_1R
_database_code_depnum_ccdc_archive 'CCDC 2265468'
loop_
_audit_author_name
_audit_author_address
'Cheng-Dong Liu'
;Southeast University
China
;
_audit_update_record             
;
2023-05-25 deposited with the CCDC.	2023-07-13 downloaded from the CCDC.
;
_audit_creation_date             2022-07-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '6(C6 H12 N O2), I12 Pb3'
_chemical_formula_sum            'C36 H72 I12 N6 O12 Pb3'
_chemical_formula_weight         2925.36
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c h o n i Pb'
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'
O O 0.0106 0.0060 '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      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   26.5063(9)
_cell_length_b                   6.7057(2)
_cell_length_c                   19.2086(7)
_cell_angle_alpha                90
_cell_angle_beta                 94.165(3)
_cell_angle_gamma                90
_cell_volume                     3405.2(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11433
_cell_measurement_temperature    300.18(10)
_cell_measurement_theta_max      30.2680
_cell_measurement_theta_min      1.9550
_shelx_estimated_absorpt_T_max   0.183
_shelx_estimated_absorpt_T_min   0.183
_exptl_absorpt_coefficient_mu    12.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.853
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20057
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.770
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.170
_diffrn_reflns_theta_min         2.126
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.18(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     30.00  67.00   0.50    0.80    --   10.60  77.00 -30.00   74
  2  ω    -10.00  77.00   0.50    0.80    --   10.60  77.00 -90.00  174
  3  ω     -5.00  84.00   0.50    0.80    --   10.60  77.00  30.00  178
  4  ω     -3.00  59.00   0.50    0.80    --   10.60  77.00 150.00  124
  5  ω     34.00  59.00   0.50    0.80    --  -11.22  77.00-150.00   50
  6  ω    -38.00   6.00   0.50    0.80    --  -11.22  77.00-150.00   88
  7  ω    -23.00  62.00   0.50    0.80    --  -11.22  77.00  90.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0052617000
_diffrn_orient_matrix_UB_12      -0.0991465000
_diffrn_orient_matrix_UB_13      -0.0111368000
_diffrn_orient_matrix_UB_21      0.0254399000
_diffrn_orient_matrix_UB_22      -0.0270953000
_diffrn_orient_matrix_UB_23      0.0095279000
_diffrn_orient_matrix_UB_31      -0.0067525000
_diffrn_orient_matrix_UB_32      -0.0249773000
_diffrn_orient_matrix_UB_33      0.0339780000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.649
_reflns_Friedel_fraction_full    0.908
_reflns_Friedel_fraction_max     0.658
_reflns_number_gt                6919
_reflns_number_total             7793
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.848
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details 
;
 Flack x determined using 2505 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         7793
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0268
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0194P)²+4.7266P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0521
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C8(H8), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B), C18(H18A,H18B), N1(H1A,H1B), N2(H2A,H2B), N3(H3C,H3D)
2.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O3(H3), O5(H5)
;
_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
C1 C -0.2125(3) -0.3121(14) -0.4340(5) 0.037(2) Uani 1 1 d . . . . .
C2 C -0.1814(3) -0.2188(12) -0.3729(4) 0.0290(18) Uani 1 1 d . . . . .
H2 H -0.183110 -0.304475 -0.331815 0.035 Uiso 1 1 calc R U . . .
C3 C -0.2012(3) -0.0162(16) -0.3566(5) 0.045(2) Uani 1 1 d . . . . .
H3A H -0.235540 -0.027141 -0.342804 0.055 Uiso 1 1 calc R U . . .
H3B H -0.201467 0.067823 -0.397691 0.055 Uiso 1 1 calc R U . . .
C4 C -0.1674(4) 0.0769(16) -0.2974(5) 0.055(3) Uani 1 1 d . . . . .
H4A H -0.180117 0.208728 -0.287419 0.066 Uiso 1 1 calc R U . . .
H4B H -0.169204 -0.003610 -0.255657 0.066 Uiso 1 1 calc R U . . .
C5 C -0.1133(4) 0.0935(15) -0.3144(5) 0.047(3) Uani 1 1 d . . . . .
H5A H -0.092794 0.144994 -0.274553 0.057 Uiso 1 1 calc R U . . .
H5B H -0.110460 0.183878 -0.353377 0.057 Uiso 1 1 calc R U . . .
C6 C -0.1268(3) -0.2052(15) -0.3915(5) 0.043(2) Uani 1 1 d . . . . .
H6A H -0.113955 -0.337673 -0.400265 0.051 Uiso 1 1 calc R U . . .
H6B H -0.124837 -0.126638 -0.433630 0.051 Uiso 1 1 calc R U . . .
C7 C -0.2108(3) -1.1003(14) -0.0775(4) 0.036(2) Uani 1 1 d . . . . .
C8 C -0.1853(3) -0.9669(13) -0.0239(5) 0.039(2) Uani 1 1 d . . . . .
H8 H -0.211718 -0.895517 -0.000858 0.047 Uiso 1 1 calc R U . . .
C9 C -0.1513(4) -0.8099(14) -0.0557(4) 0.040(2) Uani 1 1 d . . . . .
H9A H -0.170355 -0.741033 -0.093442 0.048 Uiso 1 1 calc R U . . .
H9B H -0.140607 -0.712208 -0.020408 0.048 Uiso 1 1 calc R U . . .
C10 C -0.1053(3) -0.9080(14) -0.0831(5) 0.041(2) Uani 1 1 d . . . . .
H10A H -0.083074 -0.805893 -0.099331 0.049 Uiso 1 1 calc R U . . .
H10B H -0.115980 -0.991914 -0.122641 0.049 Uiso 1 1 calc R U . . .
C11 C -0.0766(3) -1.0332(15) -0.0279(5) 0.045(2) Uani 1 1 d . . . . .
H11A H -0.048611 -1.099729 -0.048057 0.054 Uiso 1 1 calc R U . . .
H11B H -0.062915 -0.947982 0.009637 0.054 Uiso 1 1 calc R U . . .
C12 C -0.1551(3) -1.0898(14) 0.0317(4) 0.041(2) Uani 1 1 d . . . . .
H12A H -0.143259 -1.004391 0.070233 0.049 Uiso 1 1 calc R U . . .
H12B H -0.176584 -1.192119 0.049612 0.049 Uiso 1 1 calc R U . . .
C13 C -0.2871(3) -1.4242(14) -0.2099(4) 0.0333(19) Uani 1 1 d . . . . .
C14 C -0.3281(3) -1.5428(13) -0.2497(4) 0.0300(17) Uani 1 1 d . . . . .
H14 H -0.352184 -1.589926 -0.217018 0.036 Uiso 1 1 calc R U . . .
C15 C -0.3052(4) -1.7234(13) -0.2848(5) 0.041(2) Uani 1 1 d . . . . .
H15A H -0.279646 -1.679388 -0.315026 0.049 Uiso 1 1 calc R U . . .
H15B H -0.289286 -1.811117 -0.249610 0.049 Uiso 1 1 calc R U . . .
C16 C -0.3470(4) -1.8355(13) -0.3276(5) 0.044(2) Uani 1 1 d . . . . .
H16A H -0.332411 -1.948287 -0.350579 0.053 Uiso 1 1 calc R U . . .
H16B H -0.371323 -1.886337 -0.296682 0.053 Uiso 1 1 calc R U . . .
C17 C -0.3738(4) -1.7009(14) -0.3821(5) 0.044(2) Uani 1 1 d . . . . .
H17A H -0.350171 -1.656537 -0.415079 0.053 Uiso 1 1 calc R U . . .
H17B H -0.400875 -1.773708 -0.407515 0.053 Uiso 1 1 calc R U . . .
C18 C -0.3559(3) -1.4086(14) -0.3041(4) 0.040(2) Uani 1 1 d . . . . .
H18A H -0.371711 -1.299045 -0.280844 0.048 Uiso 1 1 calc R U . . .
H18B H -0.331935 -1.352985 -0.334609 0.048 Uiso 1 1 calc R U . . .
I1 I 0.000000 -0.52250(13) 0.000000 0.03315(17) Uani 1 2 d S T P . .
I2 I 0.12333(2) -0.55695(9) -0.13757(3) 0.03714(14) Uani 1 1 d . . . . .
I3 I 0.02250(2) -0.06866(9) -0.18612(3) 0.04789(16) Uani 1 1 d . . . . .
I4 I -0.11403(2) -0.42598(9) -0.18861(3) 0.03870(15) Uani 1 1 d . . . . .
I5 I 0.00797(2) -0.57455(15) -0.33464(3) 0.05827(19) Uani 1 1 d . . . . .
I6 I -0.11951(2) -0.68631(9) -0.51077(3) 0.03699(14) Uani 1 1 d . . . . .
I7 I 0.000000 -1.10732(13) -0.500000 0.0595(3) Uani 1 2 d S T P . .
N1 N -0.0954(3) -0.1105(13) -0.3330(4) 0.047(2) Uani 1 1 d . . . . .
H1A H -0.063569 -0.101995 -0.344686 0.057 Uiso 1 1 calc R U . . .
H1B H -0.095591 -0.188537 -0.295501 0.057 Uiso 1 1 calc R U . . .
N2 N -0.1109(3) -1.1846(11) 0.0003(4) 0.0370(18) Uani 1 1 d . . . . .
H2A H -0.093650 -1.257351 0.032577 0.044 Uiso 1 1 calc R U . . .
H2B H -0.122180 -1.266046 -0.034028 0.044 Uiso 1 1 calc R U . . .
N3 N -0.3951(2) -1.5239(12) -0.3460(3) 0.0382(17) Uani 1 1 d . . . . .
H3C H -0.410397 -1.443939 -0.377900 0.046 Uiso 1 1 calc R U . . .
H3D H -0.418282 -1.566019 -0.318102 0.046 Uiso 1 1 calc R U . . .
O1 O -0.2334(3) -0.4826(10) -0.4167(3) 0.057(2) Uani 1 1 d . . . . .
H1 H -0.246640 -0.536053 -0.451862 0.085 Uiso 1 1 calc R U . . .
O2 O -0.2183(3) -0.2397(10) -0.4909(3) 0.0494(18) Uani 1 1 d . . . . .
O3 O -0.2296(3) -1.0102(11) -0.1343(4) 0.064(2) Uani 1 1 d . . . . .
H3 H -0.246046 -1.090138 -0.158942 0.096 Uiso 1 1 calc R U . . .
O4 O -0.2142(2) -1.2815(11) -0.0702(3) 0.0478(17) Uani 1 1 d . . . . .
O5 O -0.2695(2) -1.5166(10) -0.1540(3) 0.0529(17) Uani 1 1 d . . . . .
H5 H -0.255270 -1.436490 -0.126930 0.079 Uiso 1 1 calc R U . . .
O6 O -0.2718(2) -1.2643(10) -0.2287(3) 0.0452(17) Uani 1 1 d . . . . .
Pb1 Pb 0.00746(2) -0.51724(4) -0.16987(2) 0.03047(8) Uani 1 1 d . . . . .
Pb2 Pb 0.000000 -0.63286(7) -0.500000 0.03140(11) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.520(11) . ?
C1 O1 1.323(11) . ?
C1 O2 1.195(10) . ?
C2 H2 0.9800 . ?
C2 C3 1.497(12) . ?
C2 C6 1.519(12) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.528(12) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.499(14) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 N1 1.499(13) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 N1 1.491(11) . ?
C7 C8 1.489(12) . ?
C7 O3 1.313(10) . ?
C7 O4 1.227(11) . ?
C8 H8 0.9800 . ?
C8 C9 1.540(13) . ?
C8 C12 1.528(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.513(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.514(12) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 N2 1.491(11) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 N2 1.498(11) . ?
C13 C14 1.509(11) . ?
C13 O5 1.298(10) . ?
C13 O6 1.211(11) . ?
C14 H14 0.9800 . ?
C14 C15 1.532(12) . ?
C14 C18 1.527(11) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.527(11) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.519(12) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 N3 1.505(11) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 N3 1.485(11) . ?
I1 Pb1 3.2834(3) . ?
I1 Pb1 3.2833(3) 2 ?
I2 Pb1 3.1004(6) . ?
I3 Pb1 3.0533(7) . ?
I4 Pb1 3.2718(6) . ?
I5 Pb1 3.1893(6) . ?
I5 Pb2 3.1921(6) . ?
I6 Pb2 3.1797(6) . ?
I7 Pb2 3.1815(10) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
O1 H1 0.8200 . ?
O3 H3 0.8200 . ?
O5 H5 0.8200 . ?

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
O1 C1 C2 112.1(8) . . ?
O2 C1 C2 124.4(9) . . ?
O2 C1 O1 123.5(9) . . ?
C1 C2 H2 109.0 . . ?
C3 C2 C1 110.9(7) . . ?
C3 C2 H2 109.0 . . ?
C3 C2 C6 110.4(7) . . ?
C6 C2 C1 108.4(7) . . ?
C6 C2 H2 109.0 . . ?
C2 C3 H3A 109.8 . . ?
C2 C3 H3B 109.8 . . ?
C2 C3 C4 109.4(7) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 C3 112.7(8) . . ?
C5 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
C4 C5 H5A 110.1 . . ?
C4 C5 H5B 110.1 . . ?
C4 C5 N1 108.0(7) . . ?
H5A C5 H5B 108.4 . . ?
N1 C5 H5A 110.1 . . ?
N1 C5 H5B 110.1 . . ?
C2 C6 H6A 109.7 . . ?
C2 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N1 C6 C2 109.7(7) . . ?
N1 C6 H6A 109.7 . . ?
N1 C6 H6B 109.7 . . ?
O3 C7 C8 115.1(8) . . ?
O4 C7 C8 123.3(8) . . ?
O4 C7 O3 121.6(8) . . ?
C7 C8 H8 107.6 . . ?
C7 C8 C9 112.7(7) . . ?
C7 C8 C12 110.3(7) . . ?
C9 C8 H8 107.6 . . ?
C12 C8 H8 107.6 . . ?
C12 C8 C9 110.8(7) . . ?
C8 C9 H9A 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
C10 C9 C8 110.5(7) . . ?
C10 C9 H9A 109.6 . . ?
C10 C9 H9B 109.6 . . ?
C9 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
C9 C10 C11 112.0(8) . . ?
H10A C10 H10B 107.9 . . ?
C11 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C10 C11 H11A 109.7 . . ?
C10 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
N2 C11 C10 110.0(7) . . ?
N2 C11 H11A 109.7 . . ?
N2 C11 H11B 109.7 . . ?
C8 C12 H12A 109.8 . . ?
C8 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?
N2 C12 C8 109.4(7) . . ?
N2 C12 H12A 109.8 . . ?
N2 C12 H12B 109.8 . . ?
O5 C13 C14 111.7(8) . . ?
O6 C13 C14 124.1(8) . . ?
O6 C13 O5 124.1(8) . . ?
C13 C14 H14 108.9 . . ?
C13 C14 C15 110.2(6) . . ?
C13 C14 C18 109.2(7) . . ?
C15 C14 H14 108.9 . . ?
C18 C14 H14 108.9 . . ?
C18 C14 C15 110.6(6) . . ?
C14 C15 H15A 109.8 . . ?
C14 C15 H15B 109.8 . . ?
H15A C15 H15B 108.3 . . ?
C16 C15 C14 109.4(7) . . ?
C16 C15 H15A 109.8 . . ?
C16 C15 H15B 109.8 . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 C15 111.3(8) . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C16 C17 H17A 109.9 . . ?
C16 C17 H17B 109.9 . . ?
H17A C17 H17B 108.3 . . ?
N3 C17 C16 108.9(7) . . ?
N3 C17 H17A 109.9 . . ?
N3 C17 H17B 109.9 . . ?
C14 C18 H18A 109.6 . . ?
C14 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
N3 C18 C14 110.3(7) . . ?
N3 C18 H18A 109.6 . . ?
N3 C18 H18B 109.6 . . ?
Pb1 I1 Pb1 178.77(3) 2 . ?
Pb1 I5 Pb2 175.97(2) . . ?
C5 N1 H1A 108.9 . . ?
C5 N1 H1B 108.9 . . ?
C6 N1 C5 113.5(8) . . ?
C6 N1 H1A 108.9 . . ?
C6 N1 H1B 108.9 . . ?
H1A N1 H1B 107.7 . . ?
C11 N2 C12 111.9(7) . . ?
C11 N2 H2A 109.2 . . ?
C11 N2 H2B 109.2 . . ?
C12 N2 H2A 109.2 . . ?
C12 N2 H2B 109.2 . . ?
H2A N2 H2B 107.9 . . ?
C17 N3 H3C 109.0 . . ?
C17 N3 H3D 109.0 . . ?
C18 N3 C17 112.9(7) . . ?
C18 N3 H3C 109.0 . . ?
C18 N3 H3D 109.0 . . ?
H3C N3 H3D 107.8 . . ?
C1 O1 H1 109.5 . . ?
C7 O3 H3 109.5 . . ?
C13 O5 H5 109.5 . . ?
I2 Pb1 I1 86.012(12) . . ?
I2 Pb1 I4 172.243(18) . . ?
I2 Pb1 I5 96.469(18) . . ?
I3 Pb1 I1 97.46(2) . . ?
I3 Pb1 I2 88.293(18) . . ?
I3 Pb1 I4 86.521(18) . . ?
I3 Pb1 I5 90.41(2) . . ?
I4 Pb1 I1 88.944(13) . . ?
I5 Pb1 I1 171.82(2) . . ?
I5 Pb1 I4 89.339(18) . . ?
I5 Pb2 I5 165.93(4) 2_554 . ?
I6 Pb2 I5 87.445(16) 2_554 . ?
I6 Pb2 I5 87.445(16) . 2_554 ?
I6 Pb2 I5 94.139(16) . . ?
I6 Pb2 I5 94.142(16) 2_554 2_554 ?
I6 Pb2 I6 167.06(3) 2_554 . ?
I6 Pb2 I7 83.528(13) . . ?
I6 Pb2 I7 83.528(13) 2_554 . ?
I7 Pb2 I5 97.04(2) . . ?
I7 Pb2 I5 97.04(2) . 2_554 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2 I4 0.98 3.29 4.090(7) 139.6 . yes
C5 H5B I6 0.97 3.14 4.042(10) 155.7 1_565 yes
C6 H6A I6 0.97 3.15 3.970(9) 142.7 . yes
C6 H6B I6 0.97 3.31 4.178(11) 149.8 1_565 yes
C8 H8 O4 0.98 2.59 3.551(11) 167.8 4_455 yes
C10 H10A I4 0.97 3.15 3.813(9) 127.3 . yes
C10 H10B I4 0.97 3.18 4.019(9) 146.2 1_545 yes
C11 H11A I1 0.97 3.22 3.875(10) 126.3 1_545 yes
C11 H11B I1 0.97 3.32 3.998(10) 128.9 . yes
C12 H12A I2 0.97 3.29 4.167(9) 150.6 2 yes
C12 H12B I2 0.97 3.24 3.796(9) 118.3 2_545 yes
C16 H16A I6 0.97 3.28 3.945(9) 127.2 4_434 yes
C16 H16B I2 0.97 3.28 4.070(10) 140.3 3_435 yes
C17 H17B I6 0.97 3.25 3.848(9) 122.0 4_434 yes
C17 H17B I7 0.97 3.26 3.951(9) 129.8 3_445 yes
C18 H18A I2 0.97 3.21 4.043(9) 145.5 3_445 yes
N1 H1B I4 0.89 2.67 3.551(8) 169.8 . yes
N2 H2A I1 0.89 3.15 3.713(7) 122.9 1_545 yes
N2 H2A I2 0.89 2.99 3.664(7) 133.7 2_545 yes
N2 H2B I4 0.89 3.18 3.968(7) 148.9 1_545 yes
N2 H2B O4 0.89 2.49 3.034(9) 120.0 . yes
N3 H3C I6 0.89 2.90 3.606(8) 136.9 4_444 yes
N3 H3D I3 0.89 3.08 3.907(7) 156.0 3_435 yes
O1 H1 O2 0.82 1.95 2.727(8) 158.4 4_444 yes
O3 H3 O6 0.82 1.87 2.674(9) 167.0 . yes
O5 H5 O4 0.82 1.81 2.623(9) 170.4 . yes

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
C1 C2 C3 C4 -177.2(8) . . . . ?
C1 C2 C6 N1 178.9(8) . . . . ?
C2 C3 C4 C5 58.0(11) . . . . ?
C2 C6 N1 C5 -57.9(10) . . . . ?
C3 C2 C6 N1 57.2(10) . . . . ?
C3 C4 C5 N1 -56.0(11) . . . . ?
C4 C5 N1 C6 56.6(10) . . . . ?
C6 C2 C3 C4 -57.0(10) . . . . ?
C7 C8 C9 C10 -69.6(9) . . . . ?
C7 C8 C12 N2 68.7(9) . . . . ?
C8 C9 C10 C11 -54.2(10) . . . . ?
C8 C12 N2 C11 59.6(9) . . . . ?
C9 C8 C12 N2 -56.7(9) . . . . ?
C9 C10 C11 N2 56.0(10) . . . . ?
C10 C11 N2 C12 -59.0(10) . . . . ?
C12 C8 C9 C10 54.5(9) . . . . ?
C13 C14 C15 C16 -177.3(7) . . . . ?
C13 C14 C18 N3 177.6(7) . . . . ?
C14 C15 C16 C17 57.9(10) . . . . ?
C14 C18 N3 C17 -57.5(9) . . . . ?
C15 C14 C18 N3 56.1(9) . . . . ?
C15 C16 C17 N3 -57.6(11) . . . . ?
C16 C17 N3 C18 57.8(10) . . . . ?
C18 C14 C15 C16 -56.4(10) . . . . ?
O1 C1 C2 C3 -120.4(8) . . . . ?
O1 C1 C2 C6 118.1(9) . . . . ?
O2 C1 C2 C3 58.6(12) . . . . ?
O2 C1 C2 C6 -62.8(11) . . . . ?
O3 C7 C8 C9 -43.2(10) . . . . ?
O3 C7 C8 C12 -167.6(8) . . . . ?
O4 C7 C8 C9 136.7(9) . . . . ?
O4 C7 C8 C12 12.4(12) . . . . ?
O5 C13 C14 C15 -71.9(9) . . . . ?
O5 C13 C14 C18 166.4(7) . . . . ?
O6 C13 C14 C15 106.7(10) . . . . ?
O6 C13 C14 C18 -15.0(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.699
_oxdiff_exptl_absorpt_empirical_full_min 0.706
####################################################################### 
# 
# 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_1S
_database_code_depnum_ccdc_archive 'CCDC 2265469'
loop_
_audit_author_name
_audit_author_address
'Cheng-Dong Liu'
;Southeast University
China
;
_audit_update_record             
;
2023-05-25 deposited with the CCDC.	2023-07-13 downloaded from the CCDC.
;
_audit_creation_date             2022-07-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '6(C6 H12 N O2), I12 Pb3'
_chemical_formula_sum            'C36 H72 I12 N6 O12 Pb3'
_chemical_formula_weight         2925.36
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c h n o i Pb'
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'
O O 0.0106 0.0060 '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      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   26.4701(9)
_cell_length_b                   6.7028(2)
_cell_length_c                   19.2218(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.167(3)
_cell_angle_gamma                90
_cell_volume                     3401.39(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8151
_cell_measurement_temperature    300.00(10)
_cell_measurement_theta_max      30.7590
_cell_measurement_theta_min      2.5190
_shelx_estimated_absorpt_T_max   0.182
_shelx_estimated_absorpt_T_min   0.182
_exptl_absorpt_coefficient_mu    12.902
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.856
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2616
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.801
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12748
_diffrn_reflns_point_group_measured_fraction_full 0.885
_diffrn_reflns_point_group_measured_fraction_max 0.645
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.829
_diffrn_reflns_theta_min         2.125
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.801
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     38.00  66.00   0.50    0.80    --   -5.57  57.00  60.00   56
  2  ω     -6.00  37.00   0.50    0.80    --    4.87 -99.00-180.00   86
  3  ω    -72.00   8.00   0.50    0.80    --   -5.57 -57.00 -90.00  160
  4  ω    -75.00 -41.00   0.50    0.80    --   -5.57 -38.00   0.00   68
  5  ω    -18.00   7.00   0.50    0.80    --   -5.57 -38.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0031112000
_diffrn_orient_matrix_UB_12      -0.1049306000
_diffrn_orient_matrix_UB_13      -0.0019034000
_diffrn_orient_matrix_UB_21      0.0182896000
_diffrn_orient_matrix_UB_22      0.0130148000
_diffrn_orient_matrix_UB_23      -0.0248137000
_diffrn_orient_matrix_UB_31      0.0194335000
_diffrn_orient_matrix_UB_32      0.0044935000
_diffrn_orient_matrix_UB_33      0.0273705000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.494
_reflns_Friedel_fraction_full    0.747
_reflns_Friedel_fraction_max     0.462
_reflns_number_gt                5867
_reflns_number_total             6906
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.775
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.259
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.014(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6906
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0317
_refine_ls_restrained_S_all      0.960
_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)+(0.0248P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0658
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C8(H8), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B), C18(H18A,H18B), N1(H1A,H1B), N2(H2A,H2B), N3(H3C,H3D)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3), O5(H5)
;
_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
C1 C 0.7128(4) 0.3536(18) 0.9335(5) 0.033(2) Uani 1 1 d . . . . .
C2 C 0.6813(4) 0.2610(17) 0.8740(5) 0.032(2) Uani 1 1 d . . . . .
H2 H 0.682869 0.346654 0.832891 0.038 Uiso 1 1 calc R U . . .
C3 C 0.7007(4) 0.056(2) 0.8566(6) 0.046(3) Uani 1 1 d . . . . .
H3A H 0.735346 0.067010 0.843523 0.055 Uiso 1 1 calc R U . . .
H3B H 0.700755 -0.028523 0.897525 0.055 Uiso 1 1 calc R U . . .
C4 C 0.6683(5) -0.037(2) 0.7976(6) 0.055(4) Uani 1 1 d . . . . .
H4A H 0.670607 0.041084 0.755561 0.066 Uiso 1 1 calc R U . . .
H4B H 0.680719 -0.170558 0.788707 0.066 Uiso 1 1 calc R U . . .
C5 C 0.6144(5) -0.049(2) 0.8149(6) 0.051(3) Uani 1 1 d . . . . .
H5A H 0.611635 -0.139038 0.853991 0.061 Uiso 1 1 calc R U . . .
H5B H 0.593934 -0.102306 0.775313 0.061 Uiso 1 1 calc R U . . .
C6 C 0.6267(4) 0.246(2) 0.8920(6) 0.039(3) Uani 1 1 d . . . . .
H6A H 0.624742 0.167384 0.933959 0.047 Uiso 1 1 calc R U . . .
H6B H 0.613844 0.378775 0.900944 0.047 Uiso 1 1 calc R U . . .
C7 C 0.7111(4) 0.1436(18) 0.5777(5) 0.036(3) Uani 1 1 d . . . . .
C8 C 0.6849(4) 0.0071(17) 0.5246(5) 0.035(3) Uani 1 1 d . . . . .
H8 H 0.711389 -0.064704 0.501647 0.042 Uiso 1 1 calc R U . . .
C9 C 0.6515(5) -0.1488(17) 0.5558(5) 0.038(3) Uani 1 1 d . . . . .
H9A H 0.640804 -0.246560 0.520486 0.046 Uiso 1 1 calc R U . . .
H9B H 0.670492 -0.217584 0.593576 0.046 Uiso 1 1 calc R U . . .
C10 C 0.6053(4) -0.0496(18) 0.5830(5) 0.039(3) Uani 1 1 d . . . . .
H10A H 0.583234 -0.151710 0.599719 0.047 Uiso 1 1 calc R U . . .
H10B H 0.616151 0.034820 0.622298 0.047 Uiso 1 1 calc R U . . .
C11 C 0.5756(4) 0.076(2) 0.5284(6) 0.042(3) Uani 1 1 d . . . . .
H11A H 0.561620 -0.009259 0.490949 0.050 Uiso 1 1 calc R U . . .
H11B H 0.547886 0.142258 0.549126 0.050 Uiso 1 1 calc R U . . .
C12 C 0.6551(5) 0.1323(19) 0.4679(5) 0.046(3) Uani 1 1 d . . . . .
H12A H 0.676816 0.234543 0.450436 0.055 Uiso 1 1 calc R U . . .
H12B H 0.643237 0.047504 0.429222 0.055 Uiso 1 1 calc R U . . .
C13 C 0.7876(4) 0.4672(16) 0.7101(5) 0.030(2) Uani 1 1 d . . . . .
C14 C 0.8275(4) 0.5828(19) 0.7495(5) 0.034(2) Uani 1 1 d . . . . .
H14 H 0.851608 0.630166 0.716805 0.040 Uiso 1 1 calc R U . . .
C15 C 0.8051(4) 0.7647(18) 0.7850(6) 0.039(3) Uani 1 1 d . . . . .
H15A H 0.789147 0.852547 0.749761 0.047 Uiso 1 1 calc R U . . .
H15B H 0.779309 0.720798 0.814950 0.047 Uiso 1 1 calc R U . . .
C16 C 0.8459(5) 0.8776(19) 0.8278(6) 0.046(3) Uani 1 1 d . . . . .
H16A H 0.830638 0.988119 0.851279 0.055 Uiso 1 1 calc R U . . .
H16B H 0.869872 0.932236 0.797084 0.055 Uiso 1 1 calc R U . . .
C17 C 0.8739(5) 0.7444(19) 0.8818(6) 0.043(3) Uani 1 1 d . . . . .
H17A H 0.901267 0.818411 0.906134 0.051 Uiso 1 1 calc R U . . .
H17B H 0.850873 0.700947 0.915865 0.051 Uiso 1 1 calc R U . . .
C18 C 0.8560(4) 0.4474(19) 0.8040(6) 0.038(3) Uani 1 1 d . . . . .
H18A H 0.832159 0.389707 0.834396 0.046 Uiso 1 1 calc R U . . .
H18B H 0.872316 0.339361 0.780685 0.046 Uiso 1 1 calc R U . . .
I1 I 0.500000 0.56418(17) 0.500000 0.0327(2) Uani 1 2 d S T P . .
I2 I 0.37662(3) 0.59852(12) 0.63753(3) 0.03642(17) Uani 1 1 d . . . . .
I3 I 0.47745(3) 0.11017(12) 0.68600(4) 0.0471(2) Uani 1 1 d . . . . .
I4 I 0.61405(3) 0.46750(12) 0.68856(4) 0.03780(18) Uani 1 1 d . . . . .
I5 I 0.49206(3) 0.6165(2) 0.83469(4) 0.0578(3) Uani 1 1 d . . . . .
I6 I 0.61953(3) 0.72804(12) 1.01075(4) 0.03669(18) Uani 1 1 d . . . . .
I7 I 0.500000 1.14915(19) 1.000000 0.0591(4) Uani 1 2 d S T P . .
N1 N 0.5949(3) 0.1519(17) 0.8331(5) 0.045(3) Uani 1 1 d . . . . .
H1A H 0.563187 0.140035 0.845170 0.054 Uiso 1 1 calc R U . . .
H1B H 0.594531 0.230570 0.795800 0.054 Uiso 1 1 calc R U . . .
N2 N 0.6106(4) 0.2275(15) 0.5001(4) 0.038(2) Uani 1 1 d . . . . .
H2A H 0.622029 0.308180 0.534507 0.045 Uiso 1 1 calc R U . . .
H2B H 0.593317 0.301209 0.468061 0.045 Uiso 1 1 calc R U . . .
N3 N 0.8948(3) 0.5661(17) 0.8463(4) 0.041(2) Uani 1 1 d . . . . .
H3C H 0.918170 0.607435 0.818509 0.049 Uiso 1 1 calc R U . . .
H3D H 0.910063 0.487006 0.878513 0.049 Uiso 1 1 calc R U . . .
O1 O 0.7333(4) 0.5256(14) 0.9164(4) 0.053(3) Uani 1 1 d . . . . .
H1 H 0.747275 0.577278 0.951347 0.080 Uiso 1 1 calc R U . . .
O2 O 0.7185(3) 0.2800(14) 0.9907(4) 0.050(2) Uani 1 1 d . . . . .
O3 O 0.7298(4) 0.0528(16) 0.6344(5) 0.068(3) Uani 1 1 d . . . . .
H3 H 0.736995 0.135691 0.664927 0.102 Uiso 1 1 calc R U . . .
O4 O 0.7147(3) 0.3219(13) 0.5695(4) 0.043(2) Uani 1 1 d . . . . .
O5 O 0.7698(3) 0.5570(14) 0.6531(4) 0.051(2) Uani 1 1 d . . . . .
H5 H 0.745762 0.493457 0.635293 0.076 Uiso 1 1 calc R U . . .
O6 O 0.7716(3) 0.3035(13) 0.7292(4) 0.043(2) Uani 1 1 d . . . . .
Pb1 Pb 0.49252(2) 0.55886(6) 0.66984(2) 0.02971(10) Uani 1 1 d . . . . .
Pb2 Pb 0.500000 0.67441(9) 1.000000 0.03110(14) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.500(14) . ?
C1 O1 1.325(14) . ?
C1 O2 1.204(12) . ?
C2 H2 0.9800 . ?
C2 C3 1.512(17) . ?
C2 C6 1.513(15) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.509(15) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.491(18) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 N1 1.493(17) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 N1 1.501(13) . ?
C7 C8 1.502(15) . ?
C7 O3 1.314(13) . ?
C7 O4 1.210(14) . ?
C8 H8 0.9800 . ?
C8 C9 1.521(15) . ?
C8 C12 1.545(15) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.517(16) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.517(15) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 N2 1.504(14) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 N2 1.511(15) . ?
C13 C14 1.473(15) . ?
C13 O5 1.308(12) . ?
C13 O6 1.241(14) . ?
C14 H14 0.9800 . ?
C14 C15 1.538(16) . ?
C14 C18 1.542(15) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.513(16) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.520(16) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 N3 1.502(15) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 N3 1.493(14) . ?
I1 Pb1 3.2853(4) 2_656 ?
I1 Pb1 3.2852(4) . ?
I2 Pb1 3.0971(8) . ?
I3 Pb1 3.0526(9) . ?
I4 Pb1 3.2687(9) . ?
I5 Pb1 3.1929(8) . ?
I5 Pb2 3.1930(7) . ?
I6 Pb2 3.1761(8) . ?
I7 Pb2 3.1821(14) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
O1 H1 0.8200 . ?
O3 H3 0.8200 . ?
O5 H5 0.8200 . ?

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
O1 C1 C2 112.7(9) . . ?
O2 C1 C2 123.6(11) . . ?
O2 C1 O1 123.8(10) . . ?
C1 C2 H2 108.6 . . ?
C1 C2 C3 111.4(9) . . ?
C1 C2 C6 109.8(9) . . ?
C3 C2 H2 108.6 . . ?
C3 C2 C6 109.8(10) . . ?
C6 C2 H2 108.6 . . ?
C2 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 C2 111.1(10) . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C5 C4 C3 110.8(10) . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C4 C5 H5A 109.4 . . ?
C4 C5 H5B 109.4 . . ?
C4 C5 N1 111.0(11) . . ?
H5A C5 H5B 108.0 . . ?
N1 C5 H5A 109.4 . . ?
N1 C5 H5B 109.4 . . ?
C2 C6 H6A 109.6 . . ?
C2 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
N1 C6 C2 110.4(9) . . ?
N1 C6 H6A 109.6 . . ?
N1 C6 H6B 109.6 . . ?
O3 C7 C8 114.1(11) . . ?
O4 C7 C8 123.3(10) . . ?
O4 C7 O3 122.5(11) . . ?
C7 C8 H8 107.2 . . ?
C7 C8 C9 113.8(9) . . ?
C7 C8 C12 109.6(10) . . ?
C9 C8 H8 107.2 . . ?
C9 C8 C12 111.6(10) . . ?
C12 C8 H8 107.2 . . ?
C8 C9 H9A 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
C10 C9 C8 110.0(9) . . ?
C10 C9 H9A 109.7 . . ?
C10 C9 H9B 109.7 . . ?
C9 C10 H10A 109.0 . . ?
C9 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C11 C10 C9 113.1(9) . . ?
C11 C10 H10A 109.0 . . ?
C11 C10 H10B 109.0 . . ?
C10 C11 H11A 109.9 . . ?
C10 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N2 C11 C10 108.9(9) . . ?
N2 C11 H11A 109.9 . . ?
N2 C11 H11B 109.9 . . ?
C8 C12 H12A 110.0 . . ?
C8 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
N2 C12 C8 108.3(8) . . ?
N2 C12 H12A 110.0 . . ?
N2 C12 H12B 110.0 . . ?
O5 C13 C14 112.9(10) . . ?
O6 C13 C14 124.2(9) . . ?
O6 C13 O5 122.9(10) . . ?
C13 C14 H14 108.5 . . ?
C13 C14 C15 111.1(9) . . ?
C13 C14 C18 109.6(10) . . ?
C15 C14 H14 108.5 . . ?
C15 C14 C18 110.5(8) . . ?
C18 C14 H14 108.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
C16 C15 C14 110.8(9) . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C15 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
C15 C16 C17 111.8(11) . . ?
H16A C16 H16B 107.9 . . ?
C17 C16 H16A 109.3 . . ?
C17 C16 H16B 109.3 . . ?
C16 C17 H17A 109.8 . . ?
C16 C17 H17B 109.8 . . ?
H17A C17 H17B 108.2 . . ?
N3 C17 C16 109.5(9) . . ?
N3 C17 H17A 109.8 . . ?
N3 C17 H17B 109.8 . . ?
C14 C18 H18A 109.7 . . ?
C14 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
N3 C18 C14 109.8(10) . . ?
N3 C18 H18A 109.7 . . ?
N3 C18 H18B 109.7 . . ?
Pb1 I1 Pb1 178.76(4) . 2_656 ?
Pb1 I5 Pb2 176.02(3) . . ?
C5 N1 C6 111.9(10) . . ?
C5 N1 H1A 109.2 . . ?
C5 N1 H1B 109.2 . . ?
C6 N1 H1A 109.2 . . ?
C6 N1 H1B 109.2 . . ?
H1A N1 H1B 107.9 . . ?
C11 N2 C12 112.4(10) . . ?
C11 N2 H2A 109.1 . . ?
C11 N2 H2B 109.1 . . ?
C12 N2 H2A 109.1 . . ?
C12 N2 H2B 109.1 . . ?
H2A N2 H2B 107.9 . . ?
C17 N3 H3C 108.7 . . ?
C17 N3 H3D 108.7 . . ?
C18 N3 C17 114.2(9) . . ?
C18 N3 H3C 108.7 . . ?
C18 N3 H3D 108.7 . . ?
H3C N3 H3D 107.6 . . ?
C1 O1 H1 109.5 . . ?
C7 O3 H3 109.5 . . ?
C13 O5 H5 109.5 . . ?
I2 Pb1 I1 85.991(15) . . ?
I2 Pb1 I4 172.21(2) . . ?
I2 Pb1 I5 96.52(2) . . ?
I3 Pb1 I1 97.44(3) . . ?
I3 Pb1 I2 88.29(2) . . ?
I3 Pb1 I4 86.51(2) . . ?
I3 Pb1 I5 90.47(3) . . ?
I4 Pb1 I1 88.942(16) . . ?
I5 Pb1 I1 171.78(3) . . ?
I5 Pb1 I4 89.32(2) . . ?
I5 Pb2 I5 166.03(5) . 2_657 ?
I6 Pb2 I5 94.11(2) 2_657 2_657 ?
I6 Pb2 I5 94.11(2) . . ?
I6 Pb2 I5 87.47(2) . 2_657 ?
I6 Pb2 I5 87.47(2) 2_657 . ?
I6 Pb2 I6 167.00(4) 2_657 . ?
I6 Pb2 I7 83.501(18) . . ?
I6 Pb2 I7 83.501(18) 2_657 . ?
I7 Pb2 I5 96.99(3) . 2_657 ?
I7 Pb2 I5 96.99(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2 I4 0.98 3.31 4.107(10) 140.1 . yes
C5 H5A I6 0.97 3.13 4.043(13) 156.5 1_545 yes
C6 H6A I6 0.97 3.30 4.170(13) 150.0 1_545 yes
C6 H6B I6 0.97 3.15 3.966(12) 143.0 . yes
C8 H8 O4 0.98 2.58 3.544(14) 167.5 4_646 yes
C10 H10A I4 0.97 3.15 3.818(12) 127.8 1_545 yes
C10 H10B I4 0.97 3.17 4.014(12) 146.5 . yes
C11 H11A I1 0.97 3.30 3.987(13) 129.2 1_545 yes
C11 H11B I1 0.97 3.21 3.857(13) 125.4 . yes
C12 H12A I2 0.97 3.23 3.786(12) 117.8 2_656 yes
C12 H12B I2 0.97 3.30 4.167(12) 150.0 2_646 yes
C16 H16A I6 0.97 3.29 3.946(12) 126.2 4_657 yes
C16 H16B I2 0.97 3.28 4.083(12) 141.3 3 yes
C17 H17A I6 0.97 3.24 3.841(12) 121.5 4_657 yes
C17 H17A I7 0.97 3.27 3.951(12) 128.9 3_545 yes
C18 H18B I2 0.97 3.20 4.033(11) 145.0 3_545 yes
N1 H1B I4 0.89 2.68 3.558(10) 168.3 . yes
N2 H2A I4 0.89 3.17 3.958(9) 148.9 . yes
N2 H2A O4 0.89 2.50 3.039(12) 119.8 . yes
N2 H2B I1 0.89 3.13 3.696(10) 123.4 . yes
N2 H2B I2 0.89 2.99 3.665(9) 133.7 2_656 yes
N3 H3C I3 0.89 3.09 3.917(9) 156.0 3 yes
N3 H3D I6 0.89 2.90 3.603(10) 137.3 4_647 yes
O1 H1 O2 0.82 1.94 2.719(11) 158.6 4_657 yes
O3 H3 O6 0.82 1.86 2.660(13) 164.0 . yes
O5 H5 O4 0.82 1.86 2.618(11) 153.9 . yes

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
C1 C2 C3 C4 179.0(11) . . . . ?
C1 C2 C6 N1 -179.4(10) . . . . ?
C2 C3 C4 C5 -56.9(16) . . . . ?
C2 C6 N1 C5 56.7(13) . . . . ?
C3 C2 C6 N1 -56.5(13) . . . . ?
C3 C4 C5 N1 55.8(16) . . . . ?
C4 C5 N1 C6 -56.3(13) . . . . ?
C6 C2 C3 C4 57.1(13) . . . . ?
C7 C8 C9 C10 69.8(12) . . . . ?
C7 C8 C12 N2 -70.0(11) . . . . ?
C8 C9 C10 C11 54.7(13) . . . . ?
C8 C12 N2 C11 -59.5(11) . . . . ?
C9 C8 C12 N2 57.0(12) . . . . ?
C9 C10 C11 N2 -56.0(13) . . . . ?
C10 C11 N2 C12 58.8(12) . . . . ?
C12 C8 C9 C10 -54.8(12) . . . . ?
C13 C14 C15 C16 177.5(9) . . . . ?
C13 C14 C18 N3 -177.4(8) . . . . ?
C14 C15 C16 C17 -56.5(13) . . . . ?
C14 C18 N3 C17 56.3(12) . . . . ?
C15 C14 C18 N3 -54.6(12) . . . . ?
C15 C16 C17 N3 55.4(14) . . . . ?
C16 C17 N3 C18 -56.3(13) . . . . ?
C18 C14 C15 C16 55.6(12) . . . . ?
O1 C1 C2 C3 121.0(11) . . . . ?
O1 C1 C2 C6 -117.2(11) . . . . ?
O2 C1 C2 C3 -59.4(15) . . . . ?
O2 C1 C2 C6 62.4(15) . . . . ?
O3 C7 C8 C9 42.4(14) . . . . ?
O3 C7 C8 C12 168.2(10) . . . . ?
O4 C7 C8 C9 -137.3(11) . . . . ?
O4 C7 C8 C12 -11.6(15) . . . . ?
O5 C13 C14 C15 72.4(12) . . . . ?
O5 C13 C14 C18 -165.2(9) . . . . ?
O6 C13 C14 C15 -106.3(13) . . . . ?
O6 C13 C14 C18 16.1(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.499
_oxdiff_exptl_absorpt_empirical_full_min 0.766

