# Supplementary Information (SI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2026

####################################################################### 
# 
# 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_x
_database_code_depnum_ccdc_archive 'CCDC 2513808'
loop_
_audit_author_name
_audit_author_address
'Xiao-Ying Huang'
;Fujian Institute of Research on the Structure of Matter
China
;
_audit_update_record             
;
2025-12-06 deposited with the CCDC.	2026-02-03 downloaded from the CCDC.
;
_audit_creation_date             2025-12-05
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H52 I4 N4 O16 Pb4 Sb4, 2(H2 O)'
_chemical_formula_sum            'C24 H56 I4 N4 O18 Pb4 Sb4'
_chemical_formula_weight         2512.08
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Sb Sb -0.5866 1.5461 '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           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   13.5517(17)
_cell_length_b                   26.077(3)
_cell_length_c                   31.062(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10977(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4053
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6003
_cell_measurement_theta_min      2.5959
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    16.469
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedron
_exptl_crystal_F_000             8928
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            13247
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.407
_diffrn_reflns_theta_max         24.407
_diffrn_reflns_theta_min         2.596
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3468
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1582
_reflns_number_total             2268
_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 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.233
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.236
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2268
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0431
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0402P)²+582.8323P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1088
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C5-C6 = C1-C2 = C3-C4
 1.55 with sigma of 0.02
 C6-O4 = C2-O2 = C4-O3
 1.2 with sigma of 0.01
 O1W-H1D = O1W-H1C
 0.82 with sigma of 0.01
 H1C-H1D
 1.39 with sigma of 0.01
 C5-C6 \\sim C5-C6B
 with sigma of 0.01
 C5-O4 \\sim C5-O4B
 with sigma of 0.01
 C6-O4 \\sim C6B-O4B
 with sigma of 0.001
2. Rigid bond restraints
 C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C6) = Uanis(C6B)
Uanis(O4) = Uanis(O4B)
4. Others
 Sof(H5C)=Sof(H5D)=Sof(O4B)=Sof(H4D)=Sof(C6B)=Sof(H6C)=Sof(H6D)=1-FVAR(1)
 Sof(H5A)=Sof(H5B)=Sof(O4)=Sof(H4C)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
 Fixed Sof: O1W(0.5) H1C(0.5) H1D(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C5(H5C,H5D),
 C6(H6A,H6B), C6B(H6C,H6D)
5.b Tetrahedral OH refined with riding coordinates:
 O4(H4C), O4B(H4D)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.47645(5) 0.42638(2) 0.41544(2) 0.0440(2) Uani 1 1 d . . . . .
Sb1 Sb 0.22983(8) 0.45271(4) 0.45625(3) 0.0511(3) Uani 1 1 d . . . . .
I1 I 0.375000 0.54091(6) 0.375000 0.0889(7) Uani 1 2 d S T P . .
I2 I 0.69623(13) 0.375000 0.375000 0.0885(6) Uani 1 2 d S T P . .
O1 O 0.3035(7) 0.4129(3) 0.4112(2) 0.038(2) Uani 1 1 d . . . . .
O2 O 0.3642(8) 0.4640(4) 0.4810(3) 0.062(3) Uani 1 1 d D . . . .
O3 O 0.2062(8) 0.3840(4) 0.4819(3) 0.063(3) Uani 1 1 d D . . . .
N1 N 0.2058(12) 0.4656(6) 0.5379(5) 0.070(4) Uani 1 1 d . . . . .
C1 C 0.3023(17) 0.4826(9) 0.5519(5) 0.095(7) Uani 1 1 d D . . . .
H1A H 0.317253 0.467601 0.579658 0.115 Uiso 1 1 calc R U . . .
H1B H 0.301829 0.519625 0.555164 0.115 Uiso 1 1 calc R U . . .
C2 C 0.3811(16) 0.4677(10) 0.5200(4) 0.124(10) Uani 1 1 d D . . . .
H2A H 0.434329 0.492251 0.523232 0.149 Uiso 1 1 calc R U . . .
H2B H 0.406805 0.434775 0.529292 0.149 Uiso 1 1 calc R U . . .
C3 C 0.184(2) 0.4149(8) 0.5540(5) 0.112(9) Uani 1 1 d D U . . .
H3A H 0.127968 0.416162 0.573092 0.134 Uiso 1 1 calc R U . . .
H3B H 0.240526 0.402034 0.570112 0.134 Uiso 1 1 calc R U . . .
C4 C 0.1630(18) 0.3797(9) 0.5168(5) 0.116(9) Uani 1 1 d D U . . .
H4A H 0.174411 0.345048 0.526889 0.140 Uiso 1 1 calc R U . . .
H4B H 0.092908 0.382522 0.510888 0.140 Uiso 1 1 calc R U . . .
C5 C 0.1255(19) 0.5017(9) 0.5510(7) 0.116(8) Uani 1 1 d D . . . .
H5A H 0.127274 0.505603 0.582074 0.140 Uiso 0.759(18) 1 calc R U P A 1
H5B H 0.062400 0.486496 0.543601 0.140 Uiso 0.759(18) 1 calc R U P A 1
H5C H 0.161710 0.530298 0.538813 0.140 Uiso 0.241(18) 1 calc R U P A 2
H5D H 0.148610 0.500881 0.580568 0.140 Uiso 0.241(18) 1 calc R U P A 2
O4 O 0.113(3) 0.5515(13) 0.4926(7) 0.219(15) Uani 0.759(18) 1 d D U P A 1
H4C H 0.118132 0.579792 0.481370 0.329 Uiso 0.759(18) 1 calc R U P A 1
C6 C 0.131(2) 0.5548(9) 0.5305(6) 0.096(9) Uani 0.759(18) 1 d D U P A 1
H6A H 0.084731 0.577648 0.544391 0.116 Uiso 0.759(18) 1 calc R U P A 1
H6B H 0.197140 0.568760 0.534372 0.116 Uiso 0.759(18) 1 calc R U P A 1
O4B O 0.036(5) 0.5723(15) 0.5382(15) 0.219(15) Uani 0.241(18) 1 d D . P A 2
H4D H -0.002940 0.564565 0.519065 0.329 Uiso 0.241(18) 1 calc R U P A 2
C6B C 0.042(4) 0.5375(14) 0.5638(14) 0.096(9) Uani 0.241(18) 1 d D . P A 2
H6C H -0.020146 0.518712 0.564405 0.116 Uiso 0.241(18) 1 calc R U P A 2
H6D H 0.053575 0.551162 0.592392 0.116 Uiso 0.241(18) 1 calc R U P A 2
O1W O 0.152(4) 0.618(4) 0.4139(19) 0.26(3) Uani 0.5 1 d D . P . .
H1C H 0.12(3) 0.640(11) 0.427(12) 0.391 Uiso 0.5 1 d D U P . .
H1D H 0.12(3) 0.598(11) 0.400(11) 0.391 Uiso 0.5 1 d D U 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
Pb1 Pb1 3.6733(11) 4 ?
Pb1 I1 3.5195(15) . ?
Pb1 I2 3.4992(16) . ?
Pb1 O1 2.439(8) 3 ?
Pb1 O1 2.374(9) . ?
Pb1 O1 2.368(9) 2 ?
Pb1 O2 2.726(10) . ?
Pb1 O3 2.751(10) 2 ?
Sb1 O1 2.008(8) . ?
Sb1 O2 1.999(11) . ?
Sb1 O3 1.988(11) . ?
Sb1 N1 2.578(13) . ?
O2 C2 1.236(9) . ?
O3 C4 1.238(9) . ?
N1 C1 1.45(2) . ?
N1 C3 1.44(2) . ?
N1 C5 1.50(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.506(17) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.502(16) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C5 C6 1.525(17) . ?
C5 C6B 1.52(2) . ?
O4 H4C 0.8200 . ?
O4 C6 1.208(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
O4B H4D 0.8200 . ?
O4B C6B 1.208(10) . ?
C6B H6C 0.9700 . ?
C6B H6D 0.9700 . ?
O1W O1W 0.80(7) 14_455 ?
O1W H1C 0.5(4) 14_455 ?
O1W H1C 0.820(10) . ?
O1W H1D 0.820(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
I1 Pb1 Pb1 112.02(2) . 4 ?
I2 Pb1 Pb1 58.341(18) . 4 ?
I2 Pb1 I1 121.958(16) . . ?
O1 Pb1 Pb1 39.5(2) 3 4 ?
O1 Pb1 Pb1 81.6(2) . 4 ?
O1 Pb1 Pb1 40.90(19) 2 4 ?
O1 Pb1 I1 138.4(2) 2 . ?
O1 Pb1 I1 73.7(2) . . ?
O1 Pb1 I1 73.1(2) 3 . ?
O1 Pb1 I2 139.8(2) . . ?
O1 Pb1 I2 75.5(2) 2 . ?
O1 Pb1 I2 74.7(2) 3 . ?
O1 Pb1 O1 76.1(3) . 3 ?
O1 Pb1 O1 77.0(3) 2 3 ?
O1 Pb1 O1 71.5(4) 2 . ?
O1 Pb1 O2 107.5(3) 2 . ?
O1 Pb1 O2 62.9(3) . . ?
O1 Pb1 O2 133.5(3) 3 . ?
O1 Pb1 O3 134.8(3) 3 2 ?
O1 Pb1 O3 106.6(3) . 2 ?
O1 Pb1 O3 62.4(3) 2 2 ?
O2 Pb1 Pb1 140.7(2) . 4 ?
O2 Pb1 I1 75.1(2) . . ?
O2 Pb1 I2 151.8(2) . . ?
O2 Pb1 O3 80.2(3) . 2 ?
O3 Pb1 Pb1 95.5(2) 2 4 ?
O3 Pb1 I1 152.0(2) 2 . ?
O3 Pb1 I2 76.6(2) 2 . ?
O1 Sb1 N1 144.7(4) . . ?
O2 Sb1 O1 83.8(4) . . ?
O2 Sb1 N1 73.6(5) . . ?
O3 Sb1 O1 83.9(4) . . ?
O3 Sb1 O2 97.2(5) . . ?
O3 Sb1 N1 72.8(4) . . ?
Pb1 O1 Pb1 101.4(3) . 3 ?
Pb1 O1 Pb1 108.1(4) 2 . ?
Pb1 O1 Pb1 99.6(3) 2 3 ?
Sb1 O1 Pb1 121.6(4) . 3 ?
Sb1 O1 Pb1 112.6(4) . 2 ?
Sb1 O1 Pb1 112.1(4) . . ?
Sb1 O2 Pb1 99.6(3) . . ?
C2 O2 Pb1 131.1(13) . . ?
C2 O2 Sb1 123.9(13) . . ?
Sb1 O3 Pb1 99.4(3) . 2 ?
C4 O3 Pb1 139.8(12) . 2 ?
C4 O3 Sb1 120.5(13) . . ?
C1 N1 Sb1 102.7(10) . . ?
C1 N1 C5 112.5(16) . . ?
C3 N1 Sb1 104.3(9) . . ?
C3 N1 C1 111.0(18) . . ?
C3 N1 C5 109.7(16) . . ?
C5 N1 Sb1 116.2(13) . . ?
N1 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
N1 C1 C2 111.3(15) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
O2 C2 C1 122.1(18) . . ?
O2 C2 H2A 106.8 . . ?
O2 C2 H2B 106.8 . . ?
C1 C2 H2A 106.8 . . ?
C1 C2 H2B 106.8 . . ?
H2A C2 H2B 106.6 . . ?
N1 C3 H3A 109.8 . . ?
N1 C3 H3B 109.8 . . ?
N1 C3 C4 109.4(15) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
O3 C4 C3 121.9(16) . . ?
O3 C4 H4A 106.9 . . ?
O3 C4 H4B 106.9 . . ?
C3 C4 H4A 106.9 . . ?
C3 C4 H4B 106.9 . . ?
H4A C4 H4B 106.7 . . ?
N1 C5 H5A 108.6 . . ?
N1 C5 H5B 108.6 . . ?
N1 C5 H5C 90.5 . . ?
N1 C5 H5D 90.5 . . ?
N1 C5 C6 114.8(19) . . ?
N1 C5 C6B 178(3) . . ?
H5A C5 H5B 107.6 . . ?
H5C C5 H5D 102.9 . . ?
C6 C5 H5A 108.6 . . ?
C6 C5 H5B 108.6 . . ?
C6B C5 H5C 90.5 . . ?
C6B C5 H5D 90.5 . . ?
C6 O4 H4C 109.5 . . ?
C5 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
O4 C6 C5 109(3) . . ?
O4 C6 H6A 109.8 . . ?
O4 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
C6B O4B H4D 109.5 . . ?
C5 C6B H6C 109.7 . . ?
C5 C6B H6D 109.7 . . ?
O4B C6B C5 110(3) . . ?
O4B C6B H6C 109.7 . . ?
O4B C6B H6D 109.7 . . ?
H6C C6B H6D 108.2 . . ?
O1W O1W H1C 72(10) 14_455 14_455 ?
O1W O1W H1C 40(10) 14_455 . ?
O1W O1W H1D 79(10) 14_455 . ?
H1C O1W H1C 68(10) . 14_455 ?
H1C O1W H1D 116(2) . . ?
H1D O1W H1C 82(10) . 14_455 ?

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
C4 H4B O4B 0.97 2.60 3.43(6) 143.3 17_566 yes
O4 H4C O1W 0.82 2.37 3.05(7) 141.0 . yes
O4 H4C O1W 0.82 2.51 3.22(8) 146.2 14_455 yes
C6B H6D I2 0.97 2.62 3.24(3) 122.0 18_566 yes
O1W H1C O4 0.820(10) 2.6(3) 3.22(8) 139(38) 14_455 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
Pb1 O2 C2 C1 -170.6(15) . . . . ?
Pb1 O3 C4 C3 146.6(18) 2 . . . ?
Sb1 O2 C2 C1 -22(3) . . . . ?
Sb1 O3 C4 C3 -42(3) . . . . ?
Sb1 N1 C1 C2 -21(2) . . . . ?
Sb1 N1 C3 C4 -13(2) . . . . ?
Sb1 N1 C5 C6 -54(2) . . . . ?
N1 C1 C2 O2 31(3) . . . . ?
N1 C3 C4 O3 35(4) . . . . ?
N1 C5 C6 O4 70(4) . . . . ?
C1 N1 C3 C4 -123(2) . . . . ?
C1 N1 C5 C6 64(2) . . . . ?
C3 N1 C1 C2 90(2) . . . . ?
C3 N1 C5 C6 -171.4(19) . . . . ?
C5 N1 C1 C2 -146.6(18) . . . . ?
C5 N1 C3 C4 113(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT342_x                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.  
RESPONSE: This is due to the disorder of organic ligand and 
relatively low ratio of observed reflections and parameters.
;
_vrf_PLAT420_x                   
;
PROBLEM: D-H Bond Without Acceptor  O1W      --H1D      .     Please Check 
RESPONSE: This is due to that it was difficult to properly position the hydrogen
 atom of water molecule in the structure.
;
_vrf_PLAT973_x                   
;
PROBLEM: Check Calcd Positive Resid. Density on       Pb1       1.76 eA-3  
RESPONSE: This is due to the relatively poor quality of diffraction data. 
We have tried our best to recollect single crystal X-ray difftaction data
for this compound, but no better data set could be obtained. 
;
####################################################################### 
# 
# 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_x_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2513809'
loop_
_audit_author_name
_audit_author_address
'Xiao-Ying Huang'
;Fujian Institute of Research on the Structure of Matter
China
;
_audit_update_record             
;
2025-12-06 deposited with the CCDC.	2026-02-03 downloaded from the CCDC.
;
_audit_creation_date             2025-11-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H39 I3 N3 O10 Pb Sb3, C H4 O'
_chemical_formula_sum            'C19 H43 I3 N3 O11 Pb Sb3'
_chemical_formula_weight         1442.70
_chemical_absolute_configuration unk
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.1178(3)
_cell_length_b                   15.5542(4)
_cell_length_c                   18.9473(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3571.24(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12152
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7892
_cell_measurement_theta_min      1.9949
_shelx_estimated_absorpt_T_max   0.646
_shelx_estimated_absorpt_T_min   0.646
_exptl_absorpt_coefficient_mu    9.589
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.683
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.789
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22557
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.750
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.789
_diffrn_reflns_theta_min         1.995
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.789
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.703
_reflns_number_gt                7850
_reflns_number_total             8403
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.101a 64-bit (release 13-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    ?
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.276(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         8403
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0272
_refine_ls_restrained_S_all      1.044
_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)+(0.0309P)²+0.4624P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0608
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.72419
 0.27581
2. Restrained distances
 O3-H3 = O6-H6 = O9-H9
 0.82 with sigma of 0.01
 O11-H11
 0.82 with sigma of 0.02
 H9-H11
 2.2 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B)
3.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.51305(5) 0.72674(3) 0.30098(3) 0.01657(12) Uani 1 1 d . . . . .
I2 I 0.13921(5) 0.63687(4) 0.37345(3) 0.02242(13) Uani 1 1 d . . . . .
I3 I 0.24908(5) 0.91622(3) 0.36152(3) 0.02024(12) Uani 1 1 d . . . . .
Pb1 Pb 0.26403(2) 0.75707(2) 0.26308(2) 0.01109(7) Uani 1 1 d . . . . .
Sb1 Sb 0.02646(4) 0.77215(3) 0.10359(3) 0.01115(11) Uani 1 1 d . . . . .
Sb2 Sb 0.29295(4) 0.85577(3) 0.06069(3) 0.01036(11) Uani 1 1 d . . . . .
Sb3 Sb 0.25929(5) 0.62478(3) 0.07342(3) 0.01034(11) Uani 1 1 d . . . . .
O1 O 0.1933(5) 0.7494(3) 0.0853(3) 0.0125(11) Uani 1 1 d . . . . .
O2 O 0.0316(5) 0.6415(3) 0.1087(3) 0.0139(11) Uani 1 1 d . . . . .
O3 O -0.1509(6) 0.9063(4) 0.1155(4) 0.0264(15) Uani 1 1 d D . . . .
H3 H -0.154(10) 0.956(3) 0.130(6) 0.040 Uiso 1 1 d D U . . .
O4 O 0.0714(5) 0.7974(3) 0.2030(3) 0.0154(12) Uani 1 1 d . . . . .
O5 O 0.1455(5) 0.9098(3) 0.0826(3) 0.0172(13) Uani 1 1 d . . . . .
O6 O 0.5221(6) 0.9068(4) 0.0326(3) 0.0194(13) Uani 1 1 d D . . . .
H6 H 0.512(10) 0.899(7) -0.0097(15) 0.029 Uiso 1 1 d D U . . .
O7 O 0.3453(5) 0.8448(3) 0.1597(3) 0.0121(11) Uani 1 1 d . . . . .
O8 O 0.3916(5) 0.7004(3) 0.0577(3) 0.0150(12) Uani 1 1 d . . . . .
O9 O 0.2079(6) 0.4361(4) 0.0881(4) 0.0248(15) Uani 1 1 d D . . . .
H9 H 0.164(7) 0.401(5) 0.103(6) 0.037 Uiso 1 1 d D U . . .
O10 O 0.2659(5) 0.6241(3) 0.1787(3) 0.0131(11) Uani 1 1 d . . . . .
N1 N -0.1360(6) 0.7343(5) 0.1774(4) 0.0165(15) Uani 1 1 d . . . . .
C1 C -0.1422(7) 0.6392(5) 0.1699(5) 0.0175(17) Uani 1 1 d . . . . .
H1A H -0.185334 0.624475 0.127200 0.021 Uiso 1 1 calc R U . . .
H1B H -0.180433 0.614389 0.211327 0.021 Uiso 1 1 calc R U . . .
N2 N 0.3400(6) 1.0023(4) 0.0944(4) 0.0123(14) Uani 1 1 d . . . . .
C2 C -0.0280(8) 0.6011(6) 0.1641(5) 0.0229(19) Uani 1 1 d . . . . .
H2A H 0.011863 0.608932 0.209242 0.028 Uiso 1 1 calc R U . . .
H2B H -0.033591 0.538609 0.154635 0.028 Uiso 1 1 calc R U . . .
N3 N 0.4130(6) 0.5299(4) 0.1005(4) 0.0139(14) Uani 1 1 d . . . . .
C3 C -0.2377(8) 0.7752(5) 0.1512(5) 0.0216(18) Uani 1 1 d . . . . .
H3A H -0.300833 0.752566 0.178662 0.026 Uiso 1 1 calc R U . . .
H3B H -0.248678 0.757723 0.101421 0.026 Uiso 1 1 calc R U . . .
C4 C -0.2403(8) 0.8719(5) 0.1548(5) 0.0224(18) Uani 1 1 d . . . . .
H4A H -0.310935 0.893345 0.135418 0.027 Uiso 1 1 calc R U . . .
H4B H -0.234756 0.890686 0.204611 0.027 Uiso 1 1 calc R U . . .
C5 C -0.1064(7) 0.7586(5) 0.2508(4) 0.0182(18) Uani 1 1 d . . . . .
H5A H -0.080597 0.707217 0.276796 0.022 Uiso 1 1 calc R U . . .
H5B H -0.172303 0.781530 0.275316 0.022 Uiso 1 1 calc R U . . .
C6 C -0.0154(8) 0.8268(6) 0.2499(5) 0.0214(19) Uani 1 1 d . . . . .
H6A H -0.045352 0.882322 0.233036 0.026 Uiso 1 1 calc R U . . .
H6B H 0.014295 0.835203 0.298104 0.026 Uiso 1 1 calc R U . . .
C7 C 0.2339(8) 1.0496(5) 0.0894(5) 0.0182(17) Uani 1 1 d . . . . .
H7A H 0.219130 1.065453 0.039678 0.022 Uiso 1 1 calc R U . . .
H7B H 0.237630 1.102999 0.117696 0.022 Uiso 1 1 calc R U . . .
C8 C 0.1410(8) 0.9916(5) 0.1172(5) 0.023(2) Uani 1 1 d . . . . .
H8A H 0.149322 0.983683 0.168766 0.028 Uiso 1 1 calc R U . . .
H8B H 0.068645 1.019032 0.108253 0.028 Uiso 1 1 calc R U . . .
C9 C 0.4232(8) 1.0434(5) 0.0468(5) 0.0189(19) Uani 1 1 d . . . . .
H9A H 0.434096 1.103872 0.061503 0.023 Uiso 1 1 calc R U . . .
H9B H 0.394002 1.043792 -0.002029 0.023 Uiso 1 1 calc R U . . .
C10 C 0.5326(8) 0.9983(5) 0.0473(5) 0.0184(18) Uani 1 1 d . . . . .
H10A H 0.581325 1.024770 0.011409 0.022 Uiso 1 1 calc R U . . .
H10B H 0.567697 1.006109 0.094022 0.022 Uiso 1 1 calc R U . . .
C11 C 0.3793(8) 0.9969(5) 0.1679(4) 0.0171(18) Uani 1 1 d . . . . .
H11A H 0.317620 1.009531 0.200526 0.021 Uiso 1 1 calc R U . . .
H11B H 0.437750 1.040364 0.175756 0.021 Uiso 1 1 calc R U . . .
C12 C 0.4248(8) 0.9077(5) 0.1832(4) 0.0155(17) Uani 1 1 d . . . . .
H12A H 0.495697 0.899332 0.158187 0.019 Uiso 1 1 calc R U . . .
H12B H 0.438165 0.901034 0.234507 0.019 Uiso 1 1 calc R U . . .
C13 C 0.5085(7) 0.5775(5) 0.0687(5) 0.0174(17) Uani 1 1 d . . . . .
H13A H 0.511020 0.566955 0.017143 0.021 Uiso 1 1 calc R U . . .
H13B H 0.578448 0.556551 0.089499 0.021 Uiso 1 1 calc R U . . .
C14 C 0.4959(7) 0.6726(5) 0.0827(4) 0.0155(17) Uani 1 1 d . . . . .
H14A H 0.501985 0.683893 0.133940 0.019 Uiso 1 1 calc R U . . .
H14B H 0.555281 0.704716 0.058329 0.019 Uiso 1 1 calc R U . . .
C15 C 0.4027(8) 0.4447(5) 0.0678(5) 0.0204(19) Uani 1 1 d . . . . .
H15A H 0.472678 0.413095 0.075021 0.025 Uiso 1 1 calc R U . . .
H15B H 0.392719 0.452365 0.016313 0.025 Uiso 1 1 calc R U . . .
C16 C 0.3093(8) 0.3902(5) 0.0952(6) 0.024(2) Uani 1 1 d . . . . .
H16A H 0.305520 0.335750 0.068256 0.029 Uiso 1 1 calc R U . . .
H16B H 0.322267 0.376009 0.145473 0.029 Uiso 1 1 calc R U . . .
C17 C 0.4208(8) 0.5266(5) 0.1782(4) 0.0176(18) Uani 1 1 d . . . . .
H17A H 0.476114 0.568825 0.194859 0.021 Uiso 1 1 calc R U . . .
H17B H 0.444767 0.468640 0.193301 0.021 Uiso 1 1 calc R U . . .
C18 C 0.3092(7) 0.5471(5) 0.2101(5) 0.0161(17) Uani 1 1 d . . . . .
H18A H 0.257791 0.498667 0.201771 0.019 Uiso 1 1 calc R U . . .
H18B H 0.316772 0.555156 0.261720 0.019 Uiso 1 1 calc R U . . .
O11 O 0.0572(8) 0.3072(6) 0.0642(4) 0.046(2) Uani 1 1 d D . . . .
H11 H 0.061(10) 0.284(5) 0.103(3) 0.055 Uiso 1 1 d D U . . .
C19 C 0.0898(11) 0.2553(6) 0.0069(6) 0.035(3) Uani 1 1 d . . . . .
H19A H 0.155537 0.280154 -0.015361 0.053 Uiso 1 1 calc R U . . .
H19B H 0.029846 0.252410 -0.027742 0.053 Uiso 1 1 calc R U . . .
H19C H 0.106862 0.197271 0.023822 0.053 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Pb1 3.1375(6) . ?
I2 Pb1 3.1869(6) . ?
I3 Pb1 3.1048(6) . ?
Pb1 O4 2.672(6) . ?
Pb1 O7 2.583(6) . ?
Pb1 O10 2.615(5) . ?
Sb1 O1 2.081(6) . ?
Sb1 O2 2.035(5) . ?
Sb1 O3 3.004(6) . ?
Sb1 O4 2.000(6) . ?
Sb1 N1 2.486(7) . ?
Sb2 O1 2.100(5) . ?
Sb2 O5 2.018(6) . ?
Sb2 O6 2.937(7) . ?
Sb2 O7 1.987(6) . ?
Sb2 N2 2.435(6) . ?
Sb3 O1 2.110(5) . ?
Sb3 O8 2.010(6) . ?
Sb3 O9 3.013(6) . ?
Sb3 O10 1.996(5) . ?
Sb3 N3 2.431(7) . ?
O2 C2 1.421(11) . ?
O3 H3 0.824(14) . ?
O3 C4 1.419(11) . ?
O4 C6 1.451(11) . ?
O5 C8 1.432(10) . ?
O6 H6 0.822(14) . ?
O6 C10 1.455(10) . ?
O7 C12 1.444(10) . ?
O8 C14 1.417(10) . ?
O9 H9 0.818(14) . ?
O9 C16 1.429(11) . ?
O10 C18 1.437(9) . ?
N1 C1 1.489(11) . ?
N1 C3 1.474(11) . ?
N1 C5 1.484(11) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.509(13) . ?
N2 C7 1.485(11) . ?
N2 C9 1.497(11) . ?
N2 C11 1.473(11) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N3 C13 1.500(11) . ?
N3 C15 1.468(10) . ?
N3 C17 1.477(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.506(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.531(12) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.535(12) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.500(13) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.522(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.511(11) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.506(13) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.515(13) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
O11 H11 0.82(3) . ?
O11 C19 1.411(13) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I2 102.594(17) . . ?
I3 Pb1 I1 92.208(17) . . ?
I3 Pb1 I2 92.628(17) . . ?
O4 Pb1 I1 166.70(13) . . ?
O4 Pb1 I2 90.14(13) . . ?
O4 Pb1 I3 91.02(12) . . ?
O7 Pb1 I1 83.48(13) . . ?
O7 Pb1 I2 171.38(12) . . ?
O7 Pb1 I3 93.26(11) . . ?
O7 Pb1 O4 83.46(18) . . ?
O7 Pb1 O10 87.16(16) . . ?
O10 Pb1 I1 90.74(13) . . ?
O10 Pb1 I2 86.64(12) . . ?
O10 Pb1 I3 177.05(13) . . ?
O10 Pb1 O4 86.12(17) . . ?
O1 Sb1 O3 145.63(19) . . ?
O1 Sb1 N1 145.4(2) . . ?
O2 Sb1 O1 79.0(2) . . ?
O2 Sb1 O3 135.4(2) . . ?
O2 Sb1 N1 76.2(2) . . ?
O4 Sb1 O1 85.7(2) . . ?
O4 Sb1 O2 98.2(2) . . ?
O4 Sb1 O3 89.3(2) . . ?
O4 Sb1 N1 74.4(2) . . ?
N1 Sb1 O3 63.6(2) . . ?
O1 Sb2 O6 142.83(19) . . ?
O1 Sb2 N2 144.4(2) . . ?
O5 Sb2 O1 76.9(2) . . ?
O5 Sb2 O6 139.6(2) . . ?
O5 Sb2 N2 76.3(2) . . ?
O7 Sb2 O1 84.6(2) . . ?
O7 Sb2 O5 97.2(2) . . ?
O7 Sb2 O6 83.8(2) . . ?
O7 Sb2 N2 76.0(2) . . ?
N2 Sb2 O6 64.7(2) . . ?
O1 Sb3 O9 143.8(2) . . ?
O1 Sb3 N3 145.7(2) . . ?
O8 Sb3 O1 77.3(2) . . ?
O8 Sb3 O9 138.4(2) . . ?
O8 Sb3 N3 77.0(2) . . ?
O10 Sb3 O1 85.0(2) . . ?
O10 Sb3 O8 96.8(2) . . ?
O10 Sb3 O9 84.9(2) . . ?
O10 Sb3 N3 75.9(2) . . ?
N3 Sb3 O9 63.1(2) . . ?
Sb1 O1 Sb2 117.5(2) . . ?
Sb1 O1 Sb3 122.8(2) . . ?
Sb2 O1 Sb3 118.8(3) . . ?
C2 O2 Sb1 117.5(5) . . ?
Sb1 O3 H3 135(9) . . ?
C4 O3 Sb1 108.9(5) . . ?
C4 O3 H3 99(9) . . ?
Sb1 O4 Pb1 126.4(3) . . ?
C6 O4 Pb1 116.5(5) . . ?
C6 O4 Sb1 116.2(5) . . ?
C8 O5 Sb2 119.8(5) . . ?
Sb2 O6 H6 90(8) . . ?
C10 O6 Sb2 108.2(5) . . ?
C10 O6 H6 110(7) . . ?
Sb2 O7 Pb1 129.8(3) . . ?
C12 O7 Pb1 112.2(4) . . ?
C12 O7 Sb2 116.5(5) . . ?
C14 O8 Sb3 118.9(5) . . ?
Sb3 O9 H9 145(8) . . ?
C16 O9 Sb3 108.5(5) . . ?
C16 O9 H9 101(8) . . ?
Sb3 O10 Pb1 127.4(2) . . ?
C18 O10 Pb1 114.1(4) . . ?
C18 O10 Sb3 115.7(4) . . ?
C1 N1 Sb1 102.8(5) . . ?
C3 N1 Sb1 111.7(5) . . ?
C3 N1 C1 110.8(7) . . ?
C3 N1 C5 114.1(7) . . ?
C5 N1 Sb1 106.0(5) . . ?
C5 N1 C1 110.8(7) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 C2 110.6(7) . . ?
H1A C1 H1B 108.1 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C7 N2 Sb2 104.1(5) . . ?
C7 N2 C9 109.5(6) . . ?
C9 N2 Sb2 113.5(5) . . ?
C11 N2 Sb2 105.7(4) . . ?
C11 N2 C7 111.7(7) . . ?
C11 N2 C9 112.1(7) . . ?
O2 C2 C1 110.2(7) . . ?
O2 C2 H2A 109.6 . . ?
O2 C2 H2B 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C13 N3 Sb3 102.0(4) . . ?
C15 N3 Sb3 113.2(5) . . ?
C15 N3 C13 110.0(7) . . ?
C15 N3 C17 113.2(7) . . ?
C17 N3 Sb3 106.3(5) . . ?
C17 N3 C13 111.6(7) . . ?
N1 C3 H3A 108.4 . . ?
N1 C3 H3B 108.4 . . ?
N1 C3 C4 115.6(8) . . ?
H3A C3 H3B 107.4 . . ?
C4 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
O3 C4 C3 109.7(7) . . ?
O3 C4 H4A 109.7 . . ?
O3 C4 H4B 109.7 . . ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N1 C5 H5A 109.7 . . ?
N1 C5 H5B 109.7 . . ?
N1 C5 C6 109.9(7) . . ?
H5A C5 H5B 108.2 . . ?
C6 C5 H5A 109.7 . . ?
C6 C5 H5B 109.7 . . ?
O4 C6 C5 108.1(6) . . ?
O4 C6 H6A 110.1 . . ?
O4 C6 H6B 110.1 . . ?
C5 C6 H6A 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
N2 C7 H7A 109.9 . . ?
N2 C7 H7B 109.9 . . ?
N2 C7 C8 108.8(6) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
O5 C8 C7 109.7(7) . . ?
O5 C8 H8A 109.7 . . ?
O5 C8 H8B 109.7 . . ?
C7 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
N2 C9 H9A 109.0 . . ?
N2 C9 H9B 109.0 . . ?
N2 C9 C10 113.1(7) . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
O6 C10 C9 112.3(8) . . ?
O6 C10 H10A 109.1 . . ?
O6 C10 H10B 109.1 . . ?
C9 C10 H10A 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
N2 C11 H11A 109.6 . . ?
N2 C11 H11B 109.6 . . ?
N2 C11 C12 110.5(6) . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
O7 C12 C11 108.5(7) . . ?
O7 C12 H12A 110.0 . . ?
O7 C12 H12B 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
N3 C13 H13A 109.8 . . ?
N3 C13 H13B 109.8 . . ?
N3 C13 C14 109.5(7) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
O8 C14 C13 109.3(7) . . ?
O8 C14 H14A 109.8 . . ?
O8 C14 H14B 109.8 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.3 . . ?
N3 C15 H15A 108.5 . . ?
N3 C15 H15B 108.5 . . ?
N3 C15 C16 115.3(7) . . ?
H15A C15 H15B 107.5 . . ?
C16 C15 H15A 108.5 . . ?
C16 C15 H15B 108.5 . . ?
O9 C16 C15 109.4(7) . . ?
O9 C16 H16A 109.8 . . ?
O9 C16 H16B 109.8 . . ?
C15 C16 H16A 109.8 . . ?
C15 C16 H16B 109.8 . . ?
H16A C16 H16B 108.2 . . ?
N3 C17 H17A 109.8 . . ?
N3 C17 H17B 109.8 . . ?
N3 C17 C18 109.5(7) . . ?
H17A C17 H17B 108.2 . . ?
C18 C17 H17A 109.8 . . ?
C18 C17 H17B 109.8 . . ?
O10 C18 C17 109.6(6) . . ?
O10 C18 H18A 109.8 . . ?
O10 C18 H18B 109.8 . . ?
C17 C18 H18A 109.8 . . ?
C17 C18 H18B 109.8 . . ?
H18A C18 H18B 108.2 . . ?
C19 O11 H11 115(9) . . ?
O11 C19 H19A 109.5 . . ?
O11 C19 H19B 109.5 . . ?
O11 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3 I2 0.824(14) 2.81(5) 3.595(6) 159(11) 3 yes
O6 H6 O2 0.822(14) 1.99(4) 2.784(8) 162(11) 4_565 yes
O9 H9 O11 0.818(14) 2.08(8) 2.750(10) 139(11) . yes
C2 H2B I3 0.99 3.25 3.960(9) 130.4 3_545 yes
C3 H3A I1 0.99 3.26 4.213(9) 162.3 1_455 yes
C6 H6A O3 0.99 2.60 3.273(12) 125.7 . yes
C8 H8B I2 0.99 3.13 4.083(9) 160.9 3 yes
C9 H9A I1 0.99 3.29 4.129(9) 143.2 3_655 yes
C9 H9B I3 0.99 3.17 4.132(9) 163.2 2_574 yes
C10 H10A O9 0.99 2.50 3.483(11) 169.3 4_565 yes
C11 H11B I1 0.99 2.99 3.850(8) 145.7 3_655 yes
C12 H12A O6 0.99 2.40 3.088(11) 125.7 . yes
C12 H12B I1 0.99 3.12 3.747(8) 122.2 . yes
C13 H13A O5 0.99 2.52 3.317(11) 137.3 4_565 yes
C13 H13B I3 0.99 3.16 4.083(8) 155.5 3_645 yes
C14 H14A I1 0.99 3.24 4.226(8) 177.5 . yes
C15 H15B I2 0.99 3.07 3.928(9) 146.1 2_564 yes
C16 H16B I1 0.99 3.23 3.868(9) 124.1 3_645 yes
C17 H17A I1 0.99 3.21 4.043(8) 143.4 . yes
C18 H18A O9 0.99 2.44 3.136(10) 126.9 . yes
C18 H18B I2 0.99 3.28 3.971(9) 128.8 . yes
C19 H19B I1 0.98 3.30 4.105(11) 140.3 2_564 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
Pb1 O4 C6 C5 -112.4(6) . . . . ?
Pb1 O7 C12 C11 -114.9(6) . . . . ?
Pb1 O10 C18 C17 -109.1(6) . . . . ?
Sb1 O2 C2 C1 46.2(9) . . . . ?
Sb1 O3 C4 C3 -22.9(8) . . . . ?
Sb1 O4 C6 C5 57.4(8) . . . . ?
Sb1 N1 C1 C2 34.6(8) . . . . ?
Sb1 N1 C3 C4 -64.9(8) . . . . ?
Sb1 N1 C5 C6 22.5(8) . . . . ?
Sb2 O5 C8 C7 38.1(9) . . . . ?
Sb2 O6 C10 C9 -19.9(8) . . . . ?
Sb2 O7 C12 C11 52.5(8) . . . . ?
Sb2 N2 C7 C8 39.4(7) . . . . ?
Sb2 N2 C9 C10 -62.8(8) . . . . ?
Sb2 N2 C11 C12 25.6(8) . . . . ?
Sb3 O8 C14 C13 40.7(8) . . . . ?
Sb3 O9 C16 C15 -19.9(8) . . . . ?
Sb3 O10 C18 C17 53.3(7) . . . . ?
Sb3 N3 C13 C14 40.2(7) . . . . ?
Sb3 N3 C15 C16 -66.7(8) . . . . ?
Sb3 N3 C17 C18 24.9(7) . . . . ?
N1 C1 C2 O2 -54.0(10) . . . . ?
N1 C3 C4 O3 58.5(10) . . . . ?
N1 C5 C6 O4 -49.1(9) . . . . ?
C1 N1 C3 C4 -178.9(8) . . . . ?
C1 N1 C5 C6 133.3(7) . . . . ?
N2 C7 C8 O5 -51.8(10) . . . . ?
N2 C9 C10 O6 53.2(10) . . . . ?
N2 C11 C12 O7 -49.2(9) . . . . ?
N3 C13 C14 O8 -54.7(9) . . . . ?
N3 C15 C16 O9 55.8(10) . . . . ?
N3 C17 C18 O10 -49.4(8) . . . . ?
C3 N1 C1 C2 154.1(7) . . . . ?
C3 N1 C5 C6 -100.8(8) . . . . ?
C5 N1 C1 C2 -78.3(9) . . . . ?
C5 N1 C3 C4 55.3(10) . . . . ?
C7 N2 C9 C10 -178.6(7) . . . . ?
C7 N2 C11 C12 138.2(7) . . . . ?
C9 N2 C7 C8 161.0(7) . . . . ?
C9 N2 C11 C12 -98.6(8) . . . . ?
C11 N2 C7 C8 -74.2(8) . . . . ?
C11 N2 C9 C10 56.9(9) . . . . ?
C13 N3 C15 C16 -180.0(7) . . . . ?
C13 N3 C17 C18 135.3(7) . . . . ?
C15 N3 C13 C14 160.6(7) . . . . ?
C15 N3 C17 C18 -100.0(8) . . . . ?
C17 N3 C13 C14 -72.9(8) . . . . ?
C17 N3 C15 C16 54.4(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.72419
2 0.27581

# start Validation Reply Form
_vrf_PLAT420_x                   
;
PROBLEM: D-H Bond Without Acceptor  O11      --H11      .     Please Check 
RESPONSE: This is due to that it was difficult to properly position the
 hydrogen atom attached to the solvent molecule of CH3OH.
;
# end Validation Reply Form
