# Electronic Supplementary Material (ESI) for Materials Horizons.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_je296m
_audit_block_doi                 10.5517/ccdc.csd.cc1ztf29
_database_code_depnum_ccdc_archive 'CCDC 1841681'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1021/acs.chemmater.8b04064 2019
loop_
_audit_author_name
_audit_author_address
'Rakesh Ganguly'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2018-05-07 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H45 I8 N4 Pb2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1915.30
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   12.3353(2)
_cell_length_b                   12.2206(3)
_cell_length_c                   32.2371(8)
_cell_angle_alpha                90
_cell_angle_beta                 94.2960(10)
_cell_angle_gamma                90
_cell_volume                     4845.92(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9852
_cell_measurement_theta_min      2.4654
_cell_measurement_theta_max      29.6115
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    2.625
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3412

_exptl_absorpt_coefficient_mu    12.061
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.12
_exptl_absorpt_correction_T_max  0.79

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Multilayer Mirror'

_diffrn_measurement_device_type  'Photon II CPADs detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 7.4074

_diffrn_reflns_number            30212
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         29.64
_diffrn_reflns_theta_full        29.64
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       44

_refine_special_details          
;

Refined as a 2-component inversion twin.
;

_reflns_number_total             12542
_reflns_number_gt                12154
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1045
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.125
_refine_ls_number_reflns         12542
_refine_ls_number_parameters     420
_refine_ls_number_restraints     2
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0710P)²+6.9304P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.839
_refine_diff_density_min         -3.544
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.564(9)

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'

_computing_data_collection       'APEX3 (Bruker AXS Inc., 2017)'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'XS, VERSION 2013/1'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2017)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.2872(9) 0.0875(9) 0.6720(3) 0.035(2) Uani d . . . 1 . .
C C2 0.3193(10) -0.0114(9) 0.6863(4) 0.046(3) Uani d . . . 1 . .
H H2 0.387875 -0.040029 0.680044 0.056 Uiso calc U . R 1 . .
C C3 0.2482(12) -0.0749(9) 0.7115(4) 0.051(3) Uani d . . . 1 . .
H H3 0.27191 -0.143357 0.722751 0.062 Uiso calc U . R 1 . .
C C4 0.1508(12) -0.0371(10) 0.7187(4) 0.054(3) Uani d . . . 1 . .
H H4 0.105664 -0.080002 0.734889 0.065 Uiso calc U . R 1 . .
C C5 0.1111(7) 0.0654(9) 0.7029(3) 0.0371(19) Uani d . . . 1 . .
H H5 0.040886 0.091664 0.708074 0.045 Uiso calc U . R 1 . .
C C6 0.1849(15) 0.1280(9) 0.6784(5) 0.044(3) Uani d . . . 1 . .
H H6 0.162557 0.196585 0.666871 0.053 Uiso calc U . R 1 . .
C C7 0.3560(10) 0.1527(9) 0.6450(4) 0.042(2) Uani d . . . 1 . .
H H7 0.421697 0.186881 0.655374 0.05 Uiso calc U . R 1 . .
C C8 0.3140(10) 0.1602(8) 0.6002(4) 0.040(2) Uani d . . . 1 . .
H H8A 0.365438 0.202361 0.584308 0.048 Uiso calc U . R 1 . .
H H8B 0.242903 0.198176 0.597909 0.048 Uiso calc U . R 1 . .
C C9 0.7851(9) 0.0923(9) 0.6725(3) 0.036(2) Uani d . . . 1 . .
C C10 0.8254(8) -0.0123(8) 0.6811(3) 0.0346(18) Uani d . . . 1 . .
H H10 0.890095 -0.036943 0.669836 0.041 Uiso calc U . R 1 . .
C C11 0.7681(12) -0.0801(9) 0.7067(4) 0.050(3) Uani d . . . 1 . .
H H11 0.79934 -0.148316 0.715176 0.06 Uiso calc U . R 1 . .
C C12 0.6725(11) -0.0533(12) 0.7195(4) 0.058(3) Uani d . . . 1 . .
H H12 0.636156 -0.103213 0.736309 0.069 Uiso calc U . R 1 . .
C C13 0.6223(10) 0.0497(13) 0.7086(4) 0.055(3) Uani d . . . 1 . .
H H13 0.551394 0.068725 0.715737 0.066 Uiso calc U . R 1 . .
C C14 0.6836(18) 0.1163(14) 0.6875(7) 0.073(7) Uani d . . . 1 . .
H H14 0.65575 0.187776 0.68204 0.087 Uiso calc U . R 1 . .
C C15 0.8402(10) 0.1689(8) 0.6444(4) 0.043(2) Uani d . . . 1 . .
H H15 0.877133 0.232527 0.654812 0.052 Uiso calc U . R 1 . .
C C16 0.8345(12) 0.1414(15) 0.6012(6) 0.068(5) Uani d . . . 1 . .
H H16 0.897414 0.134641 0.586109 0.082 Uiso calc U . R 1 . .
C C17 0.2919(8) 0.6606(8) 0.3281(3) 0.0326(19) Uani d . . . 1 . .
C C18 0.3928(12) 0.6332(8) 0.3153(4) 0.032(3) Uani d . . . 1 . .
H H18 0.42844 0.566596 0.32318 0.039 Uiso calc U . R 1 . .
C C19 0.4388(10) 0.7111(12) 0.2898(4) 0.051(3) Uani d . . . 1 . .
H H19 0.505825 0.691773 0.279011 0.061 Uiso calc U . R 1 . .
C C20 0.3989(12) 0.8084(12) 0.2791(3) 0.057(3) Uani d . . . 1 . .
H H20 0.438248 0.859558 0.263819 0.069 Uiso calc U . R 1 . .
C C21 0.2921(10) 0.8320(10) 0.2920(4) 0.045(3) Uani d . . . 1 . .
H H21 0.2569 0.899147 0.284673 0.054 Uiso calc U . R 1 . .
C C22 0.2447(8) 0.7591(8) 0.3140(3) 0.036(2) Uani d . . . 1 . .
H H22 0.172712 0.773975 0.32098 0.044 Uiso calc U . R 1 . .
C C23 0.2315(9) 0.5795(9) 0.3559(3) 0.040(2) Uani d . . . 1 . .
H H23A 0.154614 0.572741 0.344946 0.049 Uiso calc U . R 1 . .
H H23B 0.265491 0.506269 0.354947 0.049 Uiso calc U . R 1 . .
C C24 0.2363(9) 0.6194(5) 0.4005(3) 0.0256(19) Uani d . . . 1 . .
H H24A 0.202154 0.692615 0.401462 0.031 Uiso calc U . R 1 . .
H H24B 0.195014 0.568745 0.417358 0.031 Uiso calc U . R 1 . .
C C25 0.7882(8) 0.6616(8) 0.3278(3) 0.0325(19) Uani d . . . 1 . .
C C26 0.7572(8) 0.7626(8) 0.3114(3) 0.0357(19) Uani d . . . 1 . .
H H26 0.68884 0.793471 0.316602 0.043 Uiso calc U . R 1 . .
C C27 0.8279(13) 0.8180(10) 0.2872(4) 0.060(4) Uani d . . . 1 . .
H H27 0.808968 0.887746 0.275859 0.072 Uiso calc U . R 1 . .
C C28 0.9270(10) 0.7697(12) 0.2799(3) 0.053(3) Uani d . . . 1 . .
H H28 0.977341 0.807082 0.264034 0.063 Uiso calc U . R 1 . .
C C29 0.9495(12) 0.6751(14) 0.2945(4) 0.059(4) Uani d . . . 1 . .
H H29 1.016412 0.643375 0.287991 0.071 Uiso calc U . R 1 . .
C C30 0.8874(12) 0.6172(9) 0.3181(5) 0.035(3) Uani d . . . 1 . .
H H30 0.909921 0.547112 0.328192 0.042 Uiso calc U . R 1 . .
C C31 0.7118(9) 0.5968(9) 0.3551(4) 0.040(2) Uani d . . . 1 . .
H H31A 0.638076 0.629295 0.352235 0.048 Uiso calc U . R 1 . .
H H31B 0.706386 0.51996 0.345443 0.048 Uiso calc U . R 1 . .
C C32 0.7553(11) 0.6000(11) 0.4001(4) 0.044(3) Uani d . . . 1 . .
H H32A 0.705279 0.557503 0.416556 0.053 Uiso calc U . R 1 . .
H H32B 0.826389 0.562001 0.402465 0.053 Uiso calc U . R 1 . .
I I1 0.00182(7) 0.87715(4) 0.40040(3) 0.0303(2) Uani d . . . 1 . .
I I2 0.06909(7) 0.87102(5) 0.59950(3) 0.0298(2) Uani d . . . 1 . .
I I3 0.28488(7) 0.81384(4) 0.49907(3) 0.03059(12) Uani d . . . 1 . .
I I4 0.52028(6) 0.86124(6) 0.40069(3) 0.02997(17) Uani d . . . 1 . .
I I5 0.55063(7) 0.88856(6) 0.59987(3) 0.03065(18) Uani d . . . 1 . .
I I6 0.78553(7) 0.93482(4) 0.50097(4) 0.03061(12) Uani d . . . 1 . .
I I7 0.47210(7) 1.12412(3) 0.49907(4) 0.03125(14) Uani d . . . 1 . .
I I8 0.59787(7) 0.62450(4) 0.50123(4) 0.03086(14) Uani d . . . 1 . .
N N1 0.3015(6) 0.0433(6) 0.5827(2) 0.0321(14) Uani d . . . 1 . .
H H1A 0.365183 0.006395 0.58781 0.048 Uiso calc U . R 1 . .
H H1B 0.284214 0.046446 0.554832 0.048 Uiso calc U . R 1 . .
H H1C 0.247758 0.008083 0.595259 0.048 Uiso calc U . R 1 . .
N N2 0.7201(7) 0.1238(5) 0.5812(3) 0.0314(17) Uani d . . . 1 . .
H H2A 0.684032 0.075924 0.596847 0.047 Uiso calc U . R 1 . .
H H2B 0.723907 0.09624 0.555163 0.047 Uiso calc U . R 1 . .
H H2C 0.684064 0.188841 0.579741 0.047 Uiso calc U . R 1 . .
N N3 0.3503(7) 0.6259(5) 0.4182(3) 0.0325(17) Uani d . . . 1 . .
H H3A 0.383459 0.560173 0.415166 0.049 Uiso calc U . R 1 . .
H H3B 0.351381 0.642874 0.445746 0.049 Uiso calc U . R 1 . .
H H3C 0.386057 0.678523 0.404701 0.049 Uiso calc U . R 1 . .
N N4 0.7695(6) 0.7049(6) 0.4187(2) 0.0311(14) Uani d . . . 1 . .
H H4A 0.809839 0.747617 0.402546 0.047 Uiso calc U . R 1 . .
H H4B 0.804403 0.697859 0.444399 0.047 Uiso calc U . R 1 . .
H H4C 0.7034 0.736501 0.420888 0.047 Uiso calc U . R 1 . .
Pb Pb1 0.03649(5) 0.87393(3) 0.50032(2) 0.02657(8) Uani d . . . 1 . .
Pb Pb2 0.53650(5) 0.87412(3) 0.50051(2) 0.02648(8) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.343(16) ?
C1 C6 . 1.38(2) ?
C1 C7 . 1.491(15) ?
C2 C3 . 1.463(18) ?
C2 H2 . 0.95 ?
C3 C4 . 1.32(2) ?
C3 H3 . 0.95 ?
C4 C5 . 1.424(17) ?
C4 H4 . 0.95 ?
C5 C6 . 1.465(19) ?
C5 H5 . 0.95 ?
C6 H6 . 0.95 ?
C7 C8 . 1.498(17) ?
C7 H7 . 0.95 ?
C8 N1 . 1.539(12) ?
C8 H8A . 0.99 ?
C8 H8B . 0.99 ?
C9 C10 . 1.392(15) ?
C9 C14 . 1.41(3) ?
C9 C15 . 1.499(15) ?
C10 C11 . 1.398(15) ?
C10 H10 . 0.95 ?
C11 C12 . 1.32(2) ?
C11 H11 . 0.95 ?
C12 C13 . 1.44(2) ?
C12 H12 . 0.95 ?
C13 C14 . 1.33(3) ?
C13 H13 . 0.95 ?
C14 H14 . 0.95 ?
C15 C16 . 1.43(2) ?
C15 H15 . 0.95 ?
C16 N2 . 1.522(17) ?
C16 H16 . 0.95 ?
C17 C18 . 1.381(17) ?
C17 C22 . 1.398(13) ?
C17 C23 . 1.562(15) ?
C18 C19 . 1.407(19) ?
C18 H18 . 0.95 ?
C19 C20 . 1.323(19) ?
C19 H19 . 0.95 ?
C20 C21 . 1.441(19) ?
C20 H20 . 0.95 ?
C21 C22 . 1.304(17) ?
C21 H21 . 0.95 ?
C22 H22 . 0.95 ?
C23 C24 . 1.515(15) ?
C23 H23A . 0.99 ?
C23 H23B . 0.99 ?
C24 N3 . 1.479(14) ?
C24 H24A . 0.99 ?
C24 H24B . 0.99 ?
C25 C26 . 1.386(14) ?
C25 C30 . 1.396(17) ?
C25 C31 . 1.551(15) ?
C26 C27 . 1.388(18) ?
C26 H26 . 0.95 ?
C27 C28 . 1.39(2) ?
C27 H27 . 0.95 ?
C28 C29 . 1.27(2) ?
C28 H28 . 0.95 ?
C29 C30 . 1.32(2) ?
C29 H29 . 0.95 ?
C30 H30 . 0.95 ?
C31 C32 . 1.511(17) ?
C31 H31A . 0.99 ?
C31 H31B . 0.99 ?
C32 N4 . 1.420(14) ?
C32 H32A . 0.99 ?
C32 H32B . 0.99 ?
I1 Pb1 . 3.2174(12) ?
I2 Pb1 . 3.1928(12) ?
I3 Pb1 . 3.1539(13) ?
I3 Pb2 . 3.1870(13) ?
I4 Pb2 . 3.2129(12) ?
I5 Pb2 . 3.1997(12) ?
I6 Pb2 . 3.1591(13) ?
I6 Pb1 1_655 3.1853(13) ?
I7 Pb1 3 3.1539(6) ?
I7 Pb2 . 3.1563(6) ?
I8 Pb2 . 3.1427(7) ?
I8 Pb1 3_545 3.1539(7) ?
N1 H1A . 0.91 ?
N1 H1B . 0.91 ?
N1 H1C . 0.91 ?
N2 H2A . 0.91 ?
N2 H2B . 0.91 ?
N2 H2C . 0.91 ?
N3 H3A . 0.91 ?
N3 H3B . 0.91 ?
N3 H3C . 0.91 ?
N4 H4A . 0.91 ?
N4 H4B . 0.91 ?
N4 H4C . 0.91 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 121.3(11) ?
C2 C1 C7 . . 121.0(11) ?
C6 C1 C7 . . 117.5(11) ?
C1 C2 C3 . . 119.6(12) ?
C1 C2 H2 . . 120.2 ?
C3 C2 H2 . . 120.2 ?
C4 C3 C2 . . 120.2(11) ?
C4 C3 H3 . . 119.9 ?
C2 C3 H3 . . 119.9 ?
C3 C4 C5 . . 122.5(11) ?
C3 C4 H4 . . 118.8 ?
C5 C4 H4 . . 118.8 ?
C4 C5 C6 . . 116.1(11) ?
C4 C5 H5 . . 121.9 ?
C6 C5 H5 . . 121.9 ?
C1 C6 C5 . . 120.3(11) ?
C1 C6 H6 . . 119.9 ?
C5 C6 H6 . . 119.9 ?
C1 C7 C8 . . 115.1(9) ?
C1 C7 H7 . . 122.5 ?
C8 C7 H7 . . 122.5 ?
C7 C8 N1 . . 108.3(9) ?
C7 C8 H8A . . 110.0 ?
N1 C8 H8A . . 110.0 ?
C7 C8 H8B . . 110.0 ?
N1 C8 H8B . . 110.0 ?
H8A C8 H8B . . 108.4 ?
C10 C9 C14 . . 115.8(12) ?
C10 C9 C15 . . 121.5(10) ?
C14 C9 C15 . . 122.2(13) ?
C9 C10 C11 . . 118.3(10) ?
C9 C10 H10 . . 120.9 ?
C11 C10 H10 . . 120.9 ?
C12 C11 C10 . . 122.7(12) ?
C12 C11 H11 . . 118.6 ?
C10 C11 H11 . . 118.6 ?
C11 C12 C13 . . 121.3(12) ?
C11 C12 H12 . . 119.3 ?
C13 C12 H12 . . 119.3 ?
C14 C13 C12 . . 114.3(12) ?
C14 C13 H13 . . 122.9 ?
C12 C13 H13 . . 122.9 ?
C13 C14 C9 . . 127.0(15) ?
C13 C14 H14 . . 116.5 ?
C9 C14 H14 . . 116.5 ?
C16 C15 C9 . . 116.8(10) ?
C16 C15 H15 . . 121.6 ?
C9 C15 H15 . . 121.6 ?
C15 C16 N2 . . 115.0(13) ?
C15 C16 H16 . . 122.5 ?
N2 C16 H16 . . 122.5 ?
C18 C17 C22 . . 118.3(10) ?
C18 C17 C23 . . 119.8(9) ?
C22 C17 C23 . . 121.8(10) ?
C17 C18 C19 . . 115.0(10) ?
C17 C18 H18 . . 122.5 ?
C19 C18 H18 . . 122.5 ?
C20 C19 C18 . . 127.1(12) ?
C20 C19 H19 . . 116.4 ?
C18 C19 H19 . . 116.4 ?
C19 C20 C21 . . 115.7(11) ?
C19 C20 H20 . . 122.1 ?
C21 C20 H20 . . 122.1 ?
C22 C21 C20 . . 118.5(11) ?
C22 C21 H21 . . 120.7 ?
C20 C21 H21 . . 120.7 ?
C21 C22 C17 . . 124.9(11) ?
C21 C22 H22 . . 117.5 ?
C17 C22 H22 . . 117.5 ?
C24 C23 C17 . . 110.7(8) ?
C24 C23 H23A . . 109.5 ?
C17 C23 H23A . . 109.5 ?
C24 C23 H23B . . 109.5 ?
C17 C23 H23B . . 109.5 ?
H23A C23 H23B . . 108.1 ?
N3 C24 C23 . . 110.6(9) ?
N3 C24 H24A . . 109.5 ?
C23 C24 H24A . . 109.5 ?
N3 C24 H24B . . 109.5 ?
C23 C24 H24B . . 109.5 ?
H24A C24 H24B . . 108.1 ?
C26 C25 C30 . . 118.8(10) ?
C26 C25 C31 . . 120.6(9) ?
C30 C25 C31 . . 120.6(10) ?
C25 C26 C27 . . 118.8(11) ?
C25 C26 H26 . . 120.6 ?
C27 C26 H26 . . 120.6 ?
C26 C27 C28 . . 119.0(11) ?
C26 C27 H27 . . 120.5 ?
C28 C27 H27 . . 120.5 ?
C29 C28 C27 . . 119.4(12) ?
C29 C28 H28 . . 120.3 ?
C27 C28 H28 . . 120.3 ?
C28 C29 C30 . . 125.5(15) ?
C28 C29 H29 . . 117.3 ?
C30 C29 H29 . . 117.3 ?
C29 C30 C25 . . 118.4(12) ?
C29 C30 H30 . . 120.8 ?
C25 C30 H30 . . 120.8 ?
C32 C31 C25 . . 110.1(8) ?
C32 C31 H31A . . 109.6 ?
C25 C31 H31A . . 109.6 ?
C32 C31 H31B . . 109.6 ?
C25 C31 H31B . . 109.6 ?
H31A C31 H31B . . 108.2 ?
N4 C32 C31 . . 116.8(11) ?
N4 C32 H32A . . 108.1 ?
C31 C32 H32A . . 108.1 ?
N4 C32 H32B . . 108.1 ?
C31 C32 H32B . . 108.1 ?
H32A C32 H32B . . 107.3 ?
Pb1 I3 Pb2 . . 153.13(2) ?
Pb2 I6 Pb1 . 1_655 152.90(2) ?
Pb1 I7 Pb2 3 . 150.92(5) ?
Pb2 I8 Pb1 . 3_545 152.23(5) ?
C8 N1 H1A . . 109.5 ?
C8 N1 H1B . . 109.5 ?
H1A N1 H1B . . 109.5 ?
C8 N1 H1C . . 109.5 ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
C16 N2 H2A . . 109.5 ?
C16 N2 H2B . . 109.5 ?
H2A N2 H2B . . 109.5 ?
C16 N2 H2C . . 109.5 ?
H2A N2 H2C . . 109.5 ?
H2B N2 H2C . . 109.5 ?
C24 N3 H3A . . 109.5 ?
C24 N3 H3B . . 109.5 ?
H3A N3 H3B . . 109.5 ?
C24 N3 H3C . . 109.5 ?
H3A N3 H3C . . 109.5 ?
H3B N3 H3C . . 109.5 ?
C32 N4 H4A . . 109.5 ?
C32 N4 H4B . . 109.5 ?
H4A N4 H4B . . 109.5 ?
C32 N4 H4C . . 109.5 ?
H4A N4 H4C . . 109.5 ?
H4B N4 H4C . . 109.5 ?
I7 Pb1 I3 3_445 . 91.05(2) ?
I7 Pb1 I8 3_445 3_455 179.30(5) ?
I3 Pb1 I8 . 3_455 89.62(3) ?
I7 Pb1 I6 3_445 1_455 88.98(3) ?
I3 Pb1 I6 . 1_455 179.65(6) ?
I8 Pb1 I6 3_455 1_455 90.34(2) ?
I7 Pb1 I2 3_445 . 90.84(3) ?
I3 Pb1 I2 . . 87.74(3) ?
I8 Pb1 I2 3_455 . 89.38(3) ?
I6 Pb1 I2 1_455 . 92.61(4) ?
I7 Pb1 I1 3_445 . 89.12(3) ?
I3 Pb1 I1 . . 92.66(4) ?
I8 Pb1 I1 3_455 . 90.65(3) ?
I6 Pb1 I1 1_455 . 86.99(3) ?
I2 Pb1 I1 . . 179.60(4) ?
I8 Pb2 I7 . . 179.27(5) ?
I8 Pb2 I6 . . 89.67(3) ?
I7 Pb2 I6 . . 90.94(2) ?
I8 Pb2 I3 . . 90.55(2) ?
I7 Pb2 I3 . . 88.84(3) ?
I6 Pb2 I3 . . 179.40(6) ?
I8 Pb2 I5 . . 92.93(4) ?
I7 Pb2 I5 . . 87.48(3) ?
I6 Pb2 I5 . . 90.13(3) ?
I3 Pb2 I5 . . 90.42(4) ?
I8 Pb2 I4 . . 87.52(3) ?
I7 Pb2 I4 . . 92.06(3) ?
I6 Pb2 I4 . . 90.22(4) ?
I3 Pb2 I4 . . 89.23(3) ?
I5 Pb2 I4 . . 179.43(4) ?

####################################################################### 
# 
# 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_sumod25_0m_5
_database_code_depnum_ccdc_archive 'CCDC 2169957'
loop_
_audit_author_name
_audit_author_address
'Yongxin Li'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2022-05-02 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 I6 N4 Pb'
_chemical_formula_iupac          ?
_chemical_formula_weight         1245.01

_chemical_melting_point          ?

_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   10.9954(4)
_cell_length_b                   10.9954(4)
_cell_length_c                   25.0526(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3028.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9971
_cell_measurement_theta_min      2.6197
_cell_measurement_theta_max      28.8738
_cell_measurement_temperature    296.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    2.730
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2208

_exptl_absorpt_coefficient_mu    11.696
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_T_max  0.80

_exptl_special_details           
;
;

_diffrn_ambient_temperature      296.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker X8APEX'
_diffrn_source_power             ?
_diffrn_source_current           ?
_diffrn_source_voltage           ?

_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       'APEX II CCD'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            2190
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       34

_refine_special_details          
;

Refined as a 2-component twin.
;

_reflns_number_total             2190
_reflns_number_gt                1669
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0972
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.033
_refine_ls_number_reflns         2190
_refine_ls_number_parameters     100
_refine_ls_number_restraints     193
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0422P)²+11.4826P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.529
_refine_diff_density_min         -1.612
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'APEX3 (Ver 2019.11, Bruker AXS Inc., 2020)'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS Inc., 2020)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS Inc., 2020)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'APEX3 (Ver 2019.11,Bruker AXS Inc., 2020)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I I1 0.59748(4) 0.78208(5) 0.30393(2) 0.04216(15) Uani d . . . 1 . .
I I2 0.5 0.5 0.16833(4) 0.0407(2) Uani d T P S 1 . .
I I3 0.5 0.5 0.42468(5) 0.1070(6) Uani d T P S 1 . .
C C1 0.1824(12) 0.5887(10) 1.0995(3) 0.041(4) Uani d U P DG 0.5 A -1
C C2 0.2092(13) 0.4825(9) 1.0717(4) 0.067(4) Uani d U P G 0.5 A -1
H H2 0.238967 0.415021 1.089913 0.081 Uiso calc U P R 0.5 A -1
C C3 0.1916(13) 0.4772(11) 1.0168(4) 0.084(5) Uani d U P G 0.5 A -1
H H3 0.209561 0.406183 0.998293 0.101 Uiso calc U P R 0.5 A -1
C C4 0.1472(12) 0.5781(14) 0.9897(3) 0.091(4) Uani d U P DG 0.5 A -1
C C5 0.1204(12) 0.6843(11) 1.0174(4) 0.081(5) Uani d U P G 0.5 A -1
H H5 0.090665 0.751752 0.999222 0.098 Uiso calc U P R 0.5 A -1
C C6 0.1380(12) 0.6896(9) 1.0723(4) 0.054(4) Uani d U P G 0.5 A -1
H H6 0.12007 0.760592 1.090841 0.065 Uiso calc U P R 0.5 A -1
C C7 0.113(2) 0.569(3) 0.9308(7) 0.096(5) Uani d U P D 0.5 A -1
H H7A 0.103942 0.484251 0.921242 0.116 Uiso calc U P R 0.5 A -1
H H7B 0.035509 0.608983 0.925231 0.116 Uiso calc U P R 0.5 A -1
N N1 0.186(3) 0.601(4) 1.1582(6) 0.044(7) Uani d U P D 0.5 A -1
H H1A 0.210777 0.53166 1.1727 0.065 Uiso calc U P R 0.5 A -1
H H1B 0.112041 0.619358 1.170237 0.065 Uiso calc U P R 0.5 A -1
H H1C 0.237452 0.660479 1.167056 0.065 Uiso calc U P R 0.5 A -1
C C8 0.204(3) 0.625(2) 0.8958(8) 0.088(6) Uani d U P D 0.5 A -1
H H8A 0.196903 0.712436 0.898768 0.106 Uiso calc U P R 0.5 A -1
H H8B 0.284021 0.602231 0.90852 0.106 Uiso calc U P R 0.5 A -1
N N2 0.195(3) 0.592(4) 0.8394(8) 0.054(7) Uani d U P D 0.5 A -1
H H2A 0.269113 0.575757 0.826757 0.081 Uiso calc U P R 0.5 A -1
H H2B 0.163129 0.653709 0.821167 0.081 Uiso calc U P R 0.5 A -1
H H2C 0.148122 0.526692 0.835808 0.081 Uiso calc U P R 0.5 A -1
Pb Pb1 0.5 0.5 0.30711(2) 0.03681(15) Uani d T P S 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
I1 Pb1 . 3.2825(5) ?
I3 Pb1 . 2.9454(13) ?
C1 C2 . 1.39 ?
C1 C6 . 1.39 ?
C1 N1 . 1.479(15) ?
C2 C3 . 1.39 ?
C3 C4 . 1.39 ?
C4 C5 . 1.39 ?
C4 C7 . 1.525(17) ?
C5 C6 . 1.39 ?
C7 C8 . 1.46(2) ?
C8 N2 . 1.461(17) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 120.0 ?
C2 C1 N1 . . 124.8(17) ?
C6 C1 N1 . . 115.0(17) ?
C1 C2 C3 . . 120.0 ?
C4 C3 C2 . . 120.0 ?
C5 C4 C3 . . 120.0 ?
C5 C4 C7 . . 119.0(15) ?
C3 C4 C7 . . 120.6(15) ?
C4 C5 C6 . . 120.0 ?
C5 C6 C1 . . 120.0 ?
C8 C7 C4 . . 112.8(17) ?
N2 C8 C7 . . 116.(2) ?
I3 Pb1 I1 . . 91.391(11) ?
I3 Pb1 I1 . 2_665 91.392(11) ?
I1 Pb1 I1 . 2_665 177.22(2) ?
I3 Pb1 I1 . 4_565 91.392(11) ?
I1 Pb1 I1 . 4_565 89.9650(10) ?
I1 Pb1 I1 2_665 4_565 89.9660(10) ?
I3 Pb1 I1 . 3_655 91.392(11) ?
I1 Pb1 I1 . 3_655 89.9670(10) ?
I1 Pb1 I1 2_665 3_655 89.9660(10) ?
I1 Pb1 I1 4_565 3_655 177.22(2) ?

####################################################################### 
# 
# 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_je431m_0m_5
_database_code_depnum_ccdc_archive 'CCDC 2170085'
loop_
_audit_author_name
_audit_author_address
'Yongxin Li'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2022-05-02 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H12 I4 N2 Pb'
_chemical_formula_weight         838.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.3676(5)
_cell_length_b                   12.5920(7)
_cell_length_c                   20.5523(12)
_cell_angle_alpha                90
_cell_angle_beta                 96.257(4)
_cell_angle_gamma                90
_cell_volume                     1638.08(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    2109
_cell_measurement_theta_min      3.2357
_cell_measurement_theta_max      28.2603

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.402
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    17.813
_shelx_estimated_absorpt_T_min   0.224
_shelx_estimated_absorpt_T_max   0.717
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.35
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_process_details   
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            4139
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.567
_diffrn_reflns_theta_max         29.595
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measured_fraction_theta_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_point_group_measured_fraction_full 0.951
_reflns_number_total             4139
_reflns_number_gt                2879
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .


_computing_data_collection       'APEX3 (Bruker AXS Inc., 2017)'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2017)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2017)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0395P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4139
_refine_ls_number_parameters     129
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1017
_refine_ls_wR_factor_gt          0.0861
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.441(3) 0.6581(11) 0.5357(8) 0.055(4) Uani 1 1 d . . . . .
H1 H 0.313654 0.625109 0.520994 0.066 Uiso 1 1 calc R U . . .
C2 C 0.582(3) 0.6057(11) 0.5781(8) 0.058(4) Uani 1 1 d . . . . .
H2 H 0.553867 0.537227 0.591741 0.069 Uiso 1 1 calc R U . . .
C3 C 0.802(3) 0.7507(12) 0.5827(7) 0.062(5) Uani 1 1 d . . . . .
H3 H 0.926722 0.783144 0.600221 0.075 Uiso 1 1 calc R U . . .
C4 C 0.664(2) 0.8042(11) 0.5393(7) 0.053(4) Uani 1 1 d . . . . .
H4 H 0.695395 0.872895 0.526839 0.064 Uiso 1 1 calc R U . . .
C5 C 0.479(2) 0.7580(10) 0.5139(6) 0.036(3) Uani 1 1 d . . . . .
C6 C 0.332(2) 0.8109(12) 0.4632(6) 0.048(3) Uani 1 1 d . . . . .
H6A H 0.353378 0.887127 0.466141 0.058 Uiso 1 1 calc R U . . .
H6B H 0.187912 0.796046 0.471232 0.058 Uiso 1 1 calc R U . . .
C7 C 0.365(2) 0.7741(11) 0.3950(6) 0.043(3) Uani 1 1 d . . . . .
H7A H 0.501444 0.799400 0.384408 0.052 Uiso 1 1 calc R U . . .
H7B H 0.368417 0.697095 0.394299 0.052 Uiso 1 1 calc R U . . .
N1 N 0.760(2) 0.6538(10) 0.5997(7) 0.059(4) Uani 1 1 d . . . . .
H1A H 0.851293 0.620167 0.625840 0.071 Uiso 1 1 calc R U . . .
N2 N 0.202(2) 0.8112(10) 0.3452(6) 0.064(4) Uani 1 1 d . . . . .
H2A H 0.256212 0.818429 0.307345 0.096 Uiso 1 1 calc R U . . .
H2B H 0.153128 0.873533 0.357277 0.096 Uiso 1 1 calc R U . . .
H2C H 0.097042 0.764229 0.340635 0.096 Uiso 1 1 calc R U . . .
I1 I 0.2352(2) 0.69153(7) 0.72145(5) 0.0598(3) Uani 1 1 d . . . . .
I2 I 0.37852(15) 0.90811(7) 0.90550(5) 0.0425(2) Uani 1 1 d . . . . .
I3 I 0.76106(13) 0.94053(10) 0.74916(6) 0.0560(3) Uani 1 1 d . . . . .
I4 I 0.18660(17) 0.99699(8) 0.60005(5) 0.0482(3) Uani 1 1 d . . . . .
Pb1 Pb 0.26261(7) 0.94337(4) 0.74911(3) 0.03024(12) 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
C1 C2 1.35(2) . ?
C1 C5 1.365(18) . ?
C1 H1 0.9300 . ?
C2 N1 1.319(18) . ?
C2 H2 0.9300 . ?
C3 N1 1.304(17) . ?
C3 C4 1.363(18) . ?
C3 H3 0.9300 . ?
C4 C5 1.365(18) . ?
C4 H4 0.9300 . ?
C5 C6 1.479(17) . ?
C6 C7 1.513(18) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N2 1.453(15) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
N1 H1A 0.8600 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
I1 Pb1 3.1826(11) 2_546 ?
I1 Pb1 3.2230(11) . ?
I2 Pb1 3.2489(11) . ?
I3 Pb1 3.1740(10) . ?
I3 Pb1 3.1940(10) 1_655 ?
I4 Pb1 3.1228(11) . ?

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
C2 C1 C5 122.1(15) . . ?
C2 C1 H1 119.0 . . ?
C5 C1 H1 119.0 . . ?
N1 C2 C1 118.6(14) . . ?
N1 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
N1 C3 C4 120.0(14) . . ?
N1 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 120.5(13) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C1 116.4(13) . . ?
C4 C5 C6 121.9(13) . . ?
C1 C5 C6 121.7(14) . . ?
C5 C6 C7 112.0(12) . . ?
C5 C6 H6A 109.2 . . ?
C7 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
C7 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N2 C7 C6 113.1(12) . . ?
N2 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
N2 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C3 N1 C2 122.3(14) . . ?
C3 N1 H1A 118.9 . . ?
C2 N1 H1A 118.9 . . ?
C7 N2 H2A 109.5 . . ?
C7 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C7 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
Pb1 I1 Pb1 158.99(4) 2_546 . ?
Pb1 I3 Pb1 178.71(5) . 1_655 ?
I4 Pb1 I3 92.91(3) . . ?
I4 Pb1 I1 88.35(3) . 2_556 ?
I3 Pb1 I1 91.57(4) . 2_556 ?
I4 Pb1 I3 87.40(3) . 1_455 ?
I3 Pb1 I3 178.71(5) . 1_455 ?
I1 Pb1 I3 89.69(4) 2_556 1_455 ?
I4 Pb1 I1 92.30(3) . . ?
I3 Pb1 I1 91.37(4) . . ?
I1 Pb1 I1 176.957(16) 2_556 . ?
I3 Pb1 I1 87.37(4) 1_455 . ?
I4 Pb1 I2 173.86(3) . . ?
I3 Pb1 I2 83.04(3) . . ?
I1 Pb1 I2 87.15(3) 2_556 . ?
I3 Pb1 I2 96.75(3) 1_455 . ?
I1 Pb1 I2 92.41(3) . . ?

_refine_diff_density_max         1.378
_refine_diff_density_min         -1.552
_refine_diff_density_rms         0.314

####################################################################### 
# 
# 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_je89
_audit_block_doi                 10.5517/ccdc.csd.cc238pz2
_database_code_depnum_ccdc_archive 'CCDC 1944784'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/cssc.202000028 2020
loop_
_audit_author_name
_audit_author_address
'Yongxin Li'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2019-08-01 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 I3 N Pb'
_chemical_formula_iupac          ?
_chemical_formula_weight         710.08

_chemical_melting_point          ?

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

_cell_length_a                   8.1205(4)
_cell_length_b                   9.2677(4)
_cell_length_c                   19.9344(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1500.23(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6472
_cell_measurement_theta_min      2.4235
_cell_measurement_theta_max      28.1438
_cell_measurement_temperature    253.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.160
_exptl_crystal_density_diffrn    3.144
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232

_exptl_absorpt_coefficient_mu    17.386
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_T_max  0.17

_exptl_special_details           
;
;

_diffrn_ambient_temperature      253.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker KappaCCD'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            35801
_diffrn_reflns_av_R_equivalents  0.1222
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         31.07
_diffrn_reflns_theta_full        31.07
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28

_refine_special_details          
;
;

_reflns_number_total             2530
_reflns_number_gt                1971
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1347
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.096
_refine_ls_number_reflns         2530
_refine_ls_number_parameters     72
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0506P)²+8.5448P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         3.158
_refine_diff_density_min         -2.473
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0048(3)

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'

_computing_data_collection       'APEX3 (Bruker AXS Inc., 2015)'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XS, VERSION 2013/1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2015)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.7361(13) 0.3743(11) 0.4430(6) 0.060(2) Uani d . . . 1 . .
H H1 0.7083 0.4616 0.423 0.072 Uiso calc U . R 1 . .
C C2 0.8220(16) 0.3729(14) 0.5026(6) 0.072(3) Uani d . . . 1 . .
H H2 0.8488 0.4596 0.5233 0.086 Uiso calc U . R 1 . .
C C3 0.867(2) 0.25 0.5304(9) 0.073(4) Uani d T P S 1 . .
H H3 0.9293 0.25 0.5694 0.087 Uiso calc U P R 1 . .
C C4 0.423(3) 0.25 0.3594(13) 0.144(14) Uani d T P S 1 . .
H H4A 0.3869 0.3334 0.334 0.173 Uiso calc U P R 0.5 . .
H H4B 0.3869 0.1666 0.334 0.173 Uiso calc U P R 0.5 . .
C C5 0.333(3) 0.25 0.4119(12) 0.162(16) Uani d T P S 1 . .
H H5A 0.284 0.1566 0.4175 0.242 Uiso calc U P R 0.5 . .
H H5B 0.2481 0.3213 0.4073 0.242 Uiso calc U P R 0.5 . .
H H5C 0.3994 0.2722 0.4504 0.242 Uiso calc U P R 0.5 . .
C C6 0.600(2) 0.25 0.3520(8) 0.080(5) Uani d T P S 1 . .
H H6A 0.6319 0.3344 0.3262 0.095 Uiso calc U P R 0.5 . .
H H6B 0.6319 0.1656 0.3262 0.095 Uiso calc U P R 0.5 . .
I I1 1.01412(8) 0.51023(7) 0.30862(3) 0.04809(19) Uani d . . . 1 . .
I I2 0.55239(11) 0.75 0.37762(4) 0.0468(2) Uani d T P S 1 . .
N N1 0.6927(14) 0.25 0.4141(5) 0.049(2) Uani d T P S 1 . .
Pb Pb1 0.78054(5) 0.75 0.24964(2) 0.04073(17) Uani d T P S 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.335(12) ?
C1 C2 . 1.376(16) ?
C2 C3 . 1.318(15) ?
C3 C2 7_565 1.318(15) ?
C4 C5 . 1.28(3) ?
C4 C6 . 1.44(3) ?
C6 N1 . 1.447(19) ?
I1 Pb1 . 3.1492(6) ?
I1 Pb1 6_656 3.3117(7) ?
I2 Pb1 . 3.1530(9) ?
I2 Pb1 6_556 3.3629(9) ?
N1 C1 7_565 1.335(12) ?
Pb1 I1 7_575 3.1492(7) ?
Pb1 I1 6_556 3.3116(7) ?
Pb1 I1 4_465 3.3116(7) ?
Pb1 I2 6_656 3.3629(9) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C1 C2 . . 119.9(10) ?
C3 C2 C1 . . 120.7(12) ?
C2 C3 C2 . 7_565 119.6(16) ?
C5 C4 C6 . . 131.(2) ?
C4 C6 N1 . . 115.4(15) ?
Pb1 I1 Pb1 . 6_656 77.826(13) ?
Pb1 I2 Pb1 . 6_556 77.015(17) ?
C1 N1 C1 . 7_565 119.2(13) ?
C1 N1 C6 . . 120.4(6) ?
C1 N1 C6 7_565 . 120.4(6) ?
I1 Pb1 I1 7_575 . 89.76(3) ?
I1 Pb1 I2 7_575 . 92.970(18) ?
I1 Pb1 I2 . . 92.970(18) ?
I1 Pb1 I1 7_575 6_556 176.24(2) ?
I1 Pb1 I1 . 6_556 92.920(19) ?
I2 Pb1 I1 . 6_556 84.253(18) ?
I1 Pb1 I1 7_575 4_465 92.919(19) ?
I1 Pb1 I1 . 4_465 176.24(2) ?
I2 Pb1 I1 . 4_465 84.253(18) ?
I1 Pb1 I1 6_556 4_465 84.29(2) ?
I1 Pb1 I2 7_575 6_656 83.469(18) ?
I1 Pb1 I2 . 6_656 83.469(18) ?
I2 Pb1 I2 . 6_656 174.96(3) ?
I1 Pb1 I2 6_556 6_656 99.458(18) ?
I1 Pb1 I2 4_465 6_656 99.458(18) ?

####################################################################### 
# 
# 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_sumod42m
_database_code_depnum_ccdc_archive 'CCDC 2169958'
loop_
_audit_author_name
_audit_author_address
'Yongxin Li'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2022-05-02 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H24 I4 N2 O2 Pb'
_chemical_formula_iupac          ?
_chemical_formula_weight         991.16

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.703(3)
_cell_length_b                   8.698(3)
_cell_length_c                   17.123(7)
_cell_angle_alpha                92.942(14)
_cell_angle_beta                 101.643(13)
_cell_angle_gamma                90.504(13)
_cell_volume                     1267.6(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8985
_cell_measurement_theta_min      2.4324
_cell_measurement_theta_max      28.7770
_cell_measurement_temperature    300.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_exptl_crystal_density_diffrn    2.597
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888

_exptl_absorpt_coefficient_mu    11.537
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_T_max  0.89

_exptl_special_details           
;
;

_diffrn_ambient_temperature      300.(2)

_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'
_diffrn_source_power             0.07
_diffrn_source_current           1.4
_diffrn_source_voltage           50

_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Multilayer Mirror'

_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Photon II CMOS detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            23556
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         28.79
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23

_refine_special_details          
;
;

_reflns_number_total             6550
_reflns_number_gt                4571
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1178
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.019
_refine_ls_number_reflns         6550
_refine_ls_number_parameters     410
_refine_ls_number_restraints     737
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0288P)²+11.3096P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.497
_refine_diff_density_min         -0.943
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'APEX4 (Ver 2021.4-0, Bruker AXS Inc., 2021)'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'APEX4 (Ver 2021.4-0, Bruker AXS Inc., 2021)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.818(2) 0.6412(16) 0.0679(9) 0.091(4) Uani d U P DG 0.500000 A 1
C C2 0.9687(19) 0.7044(19) 0.0919(11) 0.086(3) Uani d U P DG 0.500000 A 1
H H2 1.052277 0.658776 0.073859 0.103000 Uiso calc U P R 0.500000 A 1
C C3 0.9942(16) 0.836(2) 0.1428(11) 0.081(3) Uani d U P DG 0.500000 A 1
H H3 1.094880 0.878181 0.158866 0.098000 Uiso calc U P R 0.500000 A 1
C C4 0.8694(19) 0.9041(17) 0.1698(9) 0.079(3) Uani d U P DG 0.500000 A 1
C C5 0.7190(16) 0.8408(19) 0.1458(10) 0.082(3) Uani d U P DG 0.500000 A 1
H H5 0.635401 0.886450 0.163844 0.099000 Uiso calc U P R 0.500000 A 1
C C6 0.6934(17) 0.7094(19) 0.0949(10) 0.087(4) Uani d U P DG 0.500000 A 1
H H6 0.592794 0.667045 0.078837 0.105000 Uiso calc U P R 0.500000 A 1
C C7 0.892(3) 1.047(2) 0.2218(11) 0.078(3) Uani d U P D 0.500000 A 1
H H7A 0.801837 1.110974 0.205787 0.094000 Uiso calc U P R 0.500000 A 1
H H7B 0.982946 1.102092 0.211659 0.094000 Uiso calc U P R 0.500000 A 1
C C8 0.915(4) 1.030(3) 0.3096(10) 0.076(4) Uani d U P D 0.500000 A 1
H H8A 0.970129 1.121122 0.336714 0.091000 Uiso calc U P R 0.500000 A 1
H H8B 0.812418 1.026810 0.323625 0.091000 Uiso calc U P R 0.500000 A 1
N N1 0.999(5) 0.897(4) 0.3395(19) 0.073(6) Uani d U P D 0.500000 A 1
H H1A 0.966449 0.815449 0.306771 0.110000 Uiso calc U P R 0.500000 A 1
H H1B 0.981985 0.880774 0.387889 0.110000 Uiso calc U P R 0.500000 A 1
H H1C 1.101331 0.913198 0.342311 0.110000 Uiso calc U P R 0.500000 A 1
O O1 0.792(3) 0.519(2) 0.0160(14) 0.115(6) Uani d U P D 0.500000 A 1
H H1O 0.872627 0.470445 0.018700 0.173000 Uiso calc U P R 0.500000 A 1
C C1A 1.140(3) 0.970(2) 0.0663(15) 0.088(4) Uani d U P D 0.500000 B 2
C C2A 1.094(3) 0.830(2) 0.0909(14) 0.085(3) Uani d U P D 0.500000 B 2
H H2A 1.134166 0.739084 0.073238 0.102000 Uiso calc U P R 0.500000 B 2
C C3A 0.989(3) 0.8267(19) 0.1421(16) 0.081(3) Uani d U P D 0.500000 B 2
H H3A 0.957942 0.733360 0.158819 0.097000 Uiso calc U P R 0.500000 B 2
C C4A 0.930(3) 0.9641(19) 0.1678(13) 0.078(3) Uani d U P D 0.500000 B 2
C C5A 0.980(3) 1.1037(18) 0.1448(14) 0.081(3) Uani d U P D 0.500000 B 2
H H5A 0.941085 1.195284 0.162463 0.098000 Uiso calc U P R 0.500000 B 2
C C6A 1.089(3) 1.108(2) 0.0959(15) 0.085(4) Uani d U P D 0.500000 B 2
H H6A 1.126525 1.201520 0.082919 0.102000 Uiso calc U P R 0.500000 B 2
C C7A 0.815(2) 0.967(3) 0.2205(11) 0.078(3) Uani d U P D 0.500000 B 2
H H7AA 0.756251 0.869902 0.211053 0.094000 Uiso calc U P R 0.500000 B 2
H H7AB 0.741255 1.047614 0.204091 0.094000 Uiso calc U P R 0.500000 B 2
C C8A 0.875(3) 0.990(4) 0.3079(11) 0.077(4) Uani d U P D 0.500000 B 2
H H8AA 0.886593 1.100338 0.320920 0.092000 Uiso calc U P R 0.500000 B 2
H H8AB 0.796272 0.951551 0.335053 0.092000 Uiso calc U P R 0.500000 B 2
N N1A 1.020(4) 0.921(4) 0.3395(18) 0.069(6) Uani d U P D 0.500000 B 2
H H1A1 1.002638 0.824020 0.350722 0.103000 Uiso calc U P R 0.500000 B 2
H H1A2 1.068041 0.973337 0.383760 0.103000 Uiso calc U P R 0.500000 B 2
H H1A3 1.081546 0.920547 0.303552 0.103000 Uiso calc U P R 0.500000 B 2
O O1A 1.238(3) 0.975(3) 0.0156(15) 0.114(7) Uani d U P D 0.500000 B 2
H H1AO 1.286852 0.894277 0.016655 0.171000 Uiso calc U P R 0.500000 B 2
C C9 0.328(2) 0.1392(18) 0.0659(11) 0.098(4) Uani d U P DG 0.500000 C 1
C C10 0.478(2) 0.203(2) 0.0929(11) 0.090(3) Uani d U P DG 0.500000 C 1
H H10 0.563701 0.158234 0.076982 0.108000 Uiso calc U P R 0.500000 C 1
C C11 0.4985(17) 0.335(2) 0.1437(12) 0.082(3) Uani d U P DG 0.500000 C 1
H H11 0.598397 0.378000 0.161808 0.099000 Uiso calc U P R 0.500000 C 1
C C12 0.370(2) 0.4025(18) 0.1675(10) 0.080(3) Uani d U P DG 0.500000 C 1
C C13 0.2207(17) 0.338(2) 0.1405(10) 0.084(4) Uani d U P DG 0.500000 C 1
H H13 0.134764 0.383483 0.156408 0.101000 Uiso calc U P R 0.500000 C 1
C C14 0.1999(18) 0.207(2) 0.0897(11) 0.097(4) Uani d U P DG 0.500000 C 1
H H14 0.100065 0.163716 0.071581 0.116000 Uiso calc U P R 0.500000 C 1
C C15 0.391(3) 0.544(2) 0.2205(10) 0.081(3) Uani d U P D 0.500000 C 1
H H15A 0.292044 0.597485 0.211744 0.097000 Uiso calc U P R 0.500000 C 1
H H15B 0.467658 0.609667 0.204305 0.097000 Uiso calc U P R 0.500000 C 1
C C16 0.440(3) 0.524(3) 0.3074(10) 0.081(4) Uani d U P D 0.500000 C 1
H H16A 0.553171 0.510024 0.318916 0.097000 Uiso calc U P R 0.500000 C 1
H H16B 0.420162 0.618734 0.335349 0.097000 Uiso calc U P R 0.500000 C 1
N N2 0.370(3) 0.400(2) 0.3407(12) 0.078(5) Uani d U P D 0.500000 C 1
H H2B 0.289819 0.435094 0.360629 0.117000 Uiso calc U P R 0.500000 C 1
H H2C 0.441177 0.361598 0.379375 0.117000 Uiso calc U P R 0.500000 C 1
H H2D 0.336837 0.326812 0.302723 0.117000 Uiso calc U P R 0.500000 C 1
O O2 0.311(3) 0.008(3) 0.0210(17) 0.133(8) Uani d U P D 0.500000 C 1
H H2O 0.307381 0.027236 -0.025766 0.199000 Uiso calc U P R 0.500000 C 1
C C9A 0.644(3) 0.461(2) 0.0669(16) 0.094(4) Uani d U P D 0.500000 D 2
C C10A 0.592(3) 0.323(2) 0.0917(15) 0.089(3) Uani d U P D 0.500000 D 2
H H10A 0.628969 0.229608 0.074728 0.106000 Uiso calc U P R 0.500000 D 2
C C11A 0.485(3) 0.3267(19) 0.1422(17) 0.083(3) Uani d U P D 0.500000 D 2
H H11A 0.450691 0.235608 0.159618 0.099000 Uiso calc U P R 0.500000 D 2
C C12A 0.431(3) 0.4669(19) 0.1664(13) 0.080(3) Uani d U P D 0.500000 D 2
C C13A 0.480(3) 0.6039(19) 0.1400(14) 0.084(3) Uani d U P D 0.500000 D 2
H H13A 0.442655 0.697407 0.156221 0.101000 Uiso calc U P R 0.500000 D 2
C C14A 0.586(3) 0.601(2) 0.0893(15) 0.091(3) Uani d U P D 0.500000 D 2
H H14A 0.618143 0.691559 0.070538 0.109000 Uiso calc U P R 0.500000 D 2
C C15A 0.319(2) 0.472(3) 0.2207(10) 0.081(3) Uani d U P D 0.500000 D 2
H H15C 0.241588 0.389628 0.203533 0.098000 Uiso calc U P R 0.500000 D 2
H H15D 0.263549 0.568526 0.214638 0.098000 Uiso calc U P R 0.500000 D 2
C C16A 0.386(3) 0.458(3) 0.3068(10) 0.080(4) Uani d U P D 0.500000 D 2
H H16C 0.304632 0.480766 0.336427 0.097000 Uiso calc U P R 0.500000 D 2
H H16D 0.414582 0.351520 0.314661 0.097000 Uiso calc U P R 0.500000 D 2
N N2A 0.520(2) 0.552(3) 0.3414(12) 0.079(5) Uani d U P D 0.500000 D 2
H H2A1 0.489222 0.639918 0.362051 0.119000 Uiso calc U P R 0.500000 D 2
H H2A2 0.573820 0.573358 0.303919 0.119000 Uiso calc U P R 0.500000 D 2
H H2A3 0.581485 0.502907 0.379725 0.119000 Uiso calc U P R 0.500000 D 2
O O2A 0.746(3) 0.457(3) 0.0187(15) 0.113(5) Uani d U P D 0.500000 D 2
H H2AO 0.719706 0.389021 -0.016654 0.170000 Uiso calc U P R 0.500000 D 2
I I1 1.07650(10) 0.50790(8) 0.69205(4) 0.0568(2) Uani d . . . 1.000000 . .
I I2 0.68897(9) 0.31069(9) 0.49902(5) 0.0460(3) Uani d U P . 0.8010(19) E 1
I I3 0.58817(9) 0.01955(9) 0.69205(4) 0.0567(2) Uani d . . . 1.000000 . .
I I4 0.18972(9) 0.18970(9) 0.49993(5) 0.0440(3) Uani d U P . 0.7901(19) E 1
I I2A 0.8119(4) 0.1893(4) 0.5011(3) 0.0564(12) Uani d U P . 0.1990(19) E 2
I I4A 0.3101(5) 0.3099(4) 0.4997(2) 0.0618(12) Uani d U P . 0.2099(19) E 2
Pb Pb1 1.000000 0.500000 0.500000 0.03698(13) Uani d . P S 1.000000 . .
Pb Pb2 0.500000 0.000000 0.500000 0.03703(13) Uani d . P S 1.000000 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 . 1.335(12) ?
C1 C2 . 1.390000 ?
C1 C6 . 1.390000 ?
C2 C3 . 1.390000 ?
C3 C4 . 1.390000 ?
C4 C5 . 1.390000 ?
C4 C7 . 1.479(12) ?
C5 C6 . 1.390000 ?
C7 C8 . 1.491(13) ?
C8 N1 . 1.434(13) ?
C1A O1A . 1.333(13) ?
C1A C6A . 1.389(8) ?
C1A C2A . 1.390(8) ?
C2A C3A . 1.393(8) ?
C3A C4A . 1.390(8) ?
C4A C5A . 1.391(8) ?
C4A C7A . 1.476(14) ?
C5A C6A . 1.383(8) ?
C7A C8A . 1.486(15) ?
C8A N1A . 1.427(15) ?
C9 O2 . 1.330(13) ?
C9 C10 . 1.390000 ?
C9 C14 . 1.390000 ?
C10 C11 . 1.390000 ?
C11 C12 . 1.390000 ?
C12 C13 . 1.390000 ?
C12 C15 . 1.475(13) ?
C13 C14 . 1.390000 ?
C15 C16 . 1.483(15) ?
C16 N2 . 1.428(15) ?
C9A O2A . 1.331(13) ?
C9A C14A . 1.385(8) ?
C9A C10A . 1.391(8) ?
C10A C11A . 1.392(8) ?
C11A C12A . 1.386(8) ?
C12A C13A . 1.391(8) ?
C12A C15A . 1.477(14) ?
C13A C14A . 1.385(8) ?
C15A C16A . 1.485(15) ?
C16A N2A . 1.428(15) ?
I1 Pb1 . 3.2179(14) ?
I2 Pb1 . 3.1528(11) ?
I2 Pb2 . 3.1536(11) ?
I3 Pb2 . 3.2177(14) ?
I4 Pb1 1_455 3.1764(11) ?
I4 Pb2 . 3.1768(11) ?
I2A Pb1 . 3.150(3) ?
I2A Pb2 . 3.159(3) ?
I4A Pb2 . 3.174(4) ?
I4A Pb1 1_455 3.178(4) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 C1 C2 . . 120.2(12) ?
O1 C1 C6 . . 119.7(12) ?
C2 C1 C6 . . 120.000000 ?
C1 C2 C3 . . 120.000000 ?
C4 C3 C2 . . 120.000000 ?
C3 C4 C5 . . 120.000000 ?
C3 C4 C7 . . 121.1(7) ?
C5 C4 C7 . . 118.8(7) ?
C6 C5 C4 . . 120.000000 ?
C5 C6 C1 . . 120.000000 ?
C4 C7 C8 . . 117.2(13) ?
N1 C8 C7 . . 116.0(13) ?
O1A C1A C6A . . 119.1(13) ?
O1A C1A C2A . . 120.5(13) ?
C6A C1A C2A . . 120.4(9) ?
C1A C2A C3A . . 120.1(10) ?
C4A C3A C2A . . 119.3(10) ?
C3A C4A C5A . . 120.1(9) ?
C3A C4A C7A . . 121.6(10) ?
C5A C4A C7A . . 118.3(9) ?
C6A C5A C4A . . 120.6(10) ?
C5A C6A C1A . . 119.2(10) ?
C4A C7A C8A . . 118.0(15) ?
N1A C8A C7A . . 116.5(14) ?
O2 C9 C10 . . 119.6(12) ?
O2 C9 C14 . . 120.3(12) ?
C10 C9 C14 . . 120.000000 ?
C9 C10 C11 . . 120.000000 ?
C12 C11 C10 . . 120.000000 ?
C11 C12 C13 . . 120.000000 ?
C11 C12 C15 . . 120.4(8) ?
C13 C12 C15 . . 119.6(7) ?
C12 C13 C14 . . 120.000000 ?
C13 C14 C9 . . 120.000000 ?
C12 C15 C16 . . 116.9(14) ?
N2 C16 C15 . . 118.0(14) ?
O2A C9A C14A . . 119.8(13) ?
O2A C9A C10A . . 119.1(13) ?
C14A C9A C10A . . 121.1(9) ?
C9A C10A C11A . . 119.2(10) ?
C12A C11A C10A . . 119.7(10) ?
C11A C12A C13A . . 120.7(9) ?
C11A C12A C15A . . 120.0(10) ?
C13A C12A C15A . . 119.2(10) ?
C14A C13A C12A . . 119.8(10) ?
C9A C14A C13A . . 119.4(10) ?
C12A C15A C16A . . 116.2(15) ?
N2A C16A C15A . . 117.6(14) ?
Pb1 I2 Pb2 . . 152.46(3) ?
Pb1 I4 Pb2 1_455 . 153.12(3) ?
Pb1 I2A Pb2 . . 152.27(13) ?
Pb2 I4A Pb1 . 1_455 153.20(13) ?
I2 Pb1 I2 . 2_766 180.000000 ?
I2 Pb1 I4 . 2_666 89.63(3) ?
I2 Pb1 I4 2_766 2_666 90.37(3) ?
I2 Pb1 I4 . 1_655 90.37(3) ?
I2 Pb1 I4 2_766 1_655 89.63(3) ?
I4 Pb1 I4 2_666 1_655 180.000000 ?
I2 Pb1 I4A . 2_666 62.81(7) ?
I2 Pb1 I4A 2_766 2_666 117.20(7) ?
I4 Pb1 I4A 2_666 2_666 26.83(7) ?
I4 Pb1 I4A 1_655 2_666 153.17(7) ?
I2 Pb1 I4A . 1_655 117.20(7) ?
I2 Pb1 I4A 2_766 1_655 62.80(7) ?
I4 Pb1 I4A 2_666 1_655 153.17(7) ?
I4 Pb1 I4A 1_655 1_655 26.83(7) ?
I2 Pb1 I1 . 2_766 90.66(3) ?
I2 Pb1 I1 2_766 2_766 89.34(3) ?
I4 Pb1 I1 2_666 2_766 88.40(2) ?
I4 Pb1 I1 1_655 2_766 91.60(2) ?
I2A Pb1 I1 . . 88.07(8) ?
I2A Pb1 I1 2_766 . 91.93(8) ?
I2 Pb1 I1 . . 89.34(3) ?
I2 Pb1 I1 2_766 . 90.66(3) ?
I4 Pb1 I1 2_666 . 91.60(3) ?
I4 Pb1 I1 1_655 . 88.40(3) ?
I4A Pb1 I1 2_666 . 90.91(8) ?
I4A Pb1 I1 1_655 . 89.09(8) ?
I1 Pb1 I1 2_766 . 180.00(4) ?
I2 Pb2 I2 2_656 . 180.000000 ?
I2 Pb2 I2A 2_656 2_656 27.61(7) ?
I2 Pb2 I2A . 2_656 152.39(7) ?
I2A Pb2 I2A 2_656 . 180.000000 ?
I2 Pb2 I4A 2_656 2_656 62.87(7) ?
I2 Pb2 I4A . 2_656 117.13(7) ?
I2A Pb2 I4A 2_656 . 89.53(10) ?
I2A Pb2 I4A . . 90.47(10) ?
I4A Pb2 I4A 2_656 . 180.000000 ?
I2 Pb2 I4 2_656 . 90.29(3) ?
I2 Pb2 I4 . . 89.71(3) ?
I2 Pb2 I4 2_656 2_656 89.71(3) ?
I2 Pb2 I4 . 2_656 90.29(3) ?
I4 Pb2 I4 . 2_656 180.000000 ?
I2 Pb2 I3 2_656 2_656 89.43(3) ?
I2 Pb2 I3 . 2_656 90.57(3) ?
I4 Pb2 I3 . 2_656 88.38(3) ?
I4 Pb2 I3 2_656 2_656 91.62(3) ?
I2 Pb2 I3 2_656 . 90.57(3) ?
I2 Pb2 I3 . . 89.43(3) ?
I2A Pb2 I3 2_656 . 91.84(8) ?
I2A Pb2 I3 . . 88.16(8) ?
I4A Pb2 I3 2_656 . 88.88(8) ?
I4A Pb2 I3 . . 91.12(8) ?
I4 Pb2 I3 . . 91.62(3) ?
I4 Pb2 I3 2_656 . 88.38(3) ?
I3 Pb2 I3 2_656 . 180.000000 ?

