# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2111969'
loop_
_audit_author_name
_audit_author_address
'guo-jun yuan'
;nanjing xiaozhuang university
China
;
_audit_update_record             
;
2022-03-10 deposited with the CCDC.	2022-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H28 I3 N O6 Pb'
_chemical_formula_weight         870.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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, 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                   8.3103(4)
_cell_length_b                   15.9036(9)
_cell_length_c                   18.3037(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2419.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18155
_cell_measurement_theta_min      2.225
_cell_measurement_theta_max      25.008

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.389
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   0.1872
_exptl_transmission_factor_max   0.7456
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    10.824
_shelx_estimated_absorpt_T_min   0.246
_shelx_estimated_absorpt_T_max   0.357
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18155
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.225
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_full        25.008
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2209
_reflns_number_gt                1489
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0546P)²+9.5659P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00242(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2209
_refine_ls_number_parameters     194
_refine_ls_number_restraints     433
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1215
_refine_ls_wR_factor_gt          0.1086
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      0.994
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001

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 0.16693(7) 0.750000 0.24915(3) 0.0675(3) Uani 1 2 d S T P . .
I1 I 0.41215(13) 0.750000 0.38853(6) 0.0984(4) Uani 1 2 d S T P . .
I2 I -0.07477(9) 0.61361(5) 0.31512(5) 0.0893(3) Uani 1 1 d . . . . .
N1 N 0.5685(15) 0.750000 0.5742(7) 0.089(4) Uani 1 2 d DS T P . .
H1C H 0.501727 0.750000 0.538058 0.106 Uiso 1 2 d DR U P . .
H1D H 0.575907 0.798430 0.595158 0.106 Uiso 1 1 d DR U . . .
H1E H 0.656007 0.750000 0.549808 0.106 Uiso 1 2 d DR U P . .
O2 O 0.611(3) 0.9238(15) 0.6086(15) 0.149(6) Uani 0.5 1 d D U P A 1
O3 O 0.374(3) 0.8348(14) 0.6811(13) 0.135(6) Uani 0.5 1 d D U P A 1
O1 O 0.868(3) 0.8361(15) 0.5597(14) 0.147(6) Uani 0.5 1 d D U P A 1
C1 C 0.985(4) 0.7964(6) 0.516(2) 0.151(8) Uani 0.5 1 d D U P A 1
H1A H 1.090296 0.815360 0.531395 0.181 Uiso 0.5 1 calc R U P A 1
H1B H 0.969968 0.815360 0.465788 0.181 Uiso 0.5 1 calc R U P A 1
C2 C 0.866(5) 0.9219(17) 0.542(2) 0.158(7) Uani 0.5 1 d D U P A 1
H2A H 0.838524 0.928103 0.490300 0.189 Uiso 0.5 1 calc R U P A 1
H2B H 0.972441 0.945552 0.548800 0.189 Uiso 0.5 1 calc R U P A 1
C3 C 0.749(4) 0.968(2) 0.586(2) 0.154(7) Uani 0.5 1 d D U P A 1
H3A H 0.804348 0.988733 0.629373 0.185 Uiso 0.5 1 calc R U P A 1
H3B H 0.714780 1.017301 0.558521 0.185 Uiso 0.5 1 calc R U P A 1
C4 C 0.484(4) 0.9743(19) 0.640(2) 0.145(7) Uani 0.5 1 d D U P A 1
H4A H 0.426925 1.003231 0.601560 0.174 Uiso 0.5 1 calc R U P A 1
H4B H 0.531597 1.016500 0.671853 0.174 Uiso 0.5 1 calc R U P A 1
C5 C 0.367(5) 0.9236(14) 0.684(2) 0.143(7) Uani 0.5 1 d D U P A 1
H5A H 0.377771 0.940212 0.734289 0.171 Uiso 0.5 1 calc R U P A 1
H5B H 0.259616 0.940153 0.668144 0.171 Uiso 0.5 1 calc R U P A 1
C6 C 0.265(5) 0.7960(6) 0.730(2) 0.146(8) Uani 0.5 1 d D U P A 1
H6A H 0.157329 0.815153 0.718520 0.175 Uiso 0.5 1 calc R U P A 1
H6B H 0.290039 0.815154 0.779076 0.175 Uiso 0.5 1 calc R U P A 1
O1A O 0.950(5) 0.750000 0.560(2) 0.172(9) Uani 0.5 2 d DS TU P B 2
O2A O 0.758(3) 0.9117(17) 0.5671(16) 0.175(6) Uani 0.5 1 d D U P B 2
O3A O 0.473(4) 0.9055(19) 0.6676(16) 0.175(7) Uani 0.5 1 d D U P B 2
O4A O 0.317(5) 0.750000 0.6874(17) 0.162(9) Uani 0.5 2 d DS TU P B 2
C1A C 0.941(6) 0.8354(13) 0.537(2) 0.171(8) Uani 0.5 1 d D U P B 2
H1AA H 0.849966 0.838256 0.503507 0.205 Uiso 0.5 1 calc R U P B 2
H1AB H 1.035945 0.845311 0.507557 0.205 Uiso 0.5 1 calc R U P B 2
C2A C 0.925(3) 0.910(3) 0.585(2) 0.164(7) Uani 0.5 1 d D U P B 2
H2AA H 0.946265 0.897894 0.636483 0.197 Uiso 0.5 1 calc R U P B 2
H2AB H 0.984868 0.958554 0.568923 0.197 Uiso 0.5 1 calc R U P B 2
C3A C 0.667(3) 0.9775(17) 0.600(2) 0.178(7) Uani 0.5 1 d D U P B 2
H3AA H 0.679300 1.028722 0.571969 0.214 Uiso 0.5 1 calc R U P B 2
H3AB H 0.707600 0.987952 0.649083 0.214 Uiso 0.5 1 calc R U P B 2
C4A C 0.495(3) 0.954(2) 0.6038(19) 0.177(8) Uani 0.5 1 d D U P B 2
H4AA H 0.428678 1.003910 0.605500 0.212 Uiso 0.5 1 calc R U P B 2
H4AB H 0.465599 0.921434 0.560984 0.212 Uiso 0.5 1 calc R U P B 2
C5A C 0.308(4) 0.885(4) 0.661(3) 0.26(3) Uani 0.5 1 d D U P B 2
H5AA H 0.283793 0.856088 0.615498 0.307 Uiso 0.5 1 calc R U P B 2
H5AB H 0.238138 0.932974 0.667206 0.307 Uiso 0.5 1 calc R U P B 2
C6A C 0.308(6) 0.8274(6) 0.725(2) 0.166(9) Uani 0.5 1 d D U P B 2
H6AA H 0.401038 0.836167 0.756582 0.199 Uiso 0.5 1 calc R U P B 2
H6AB H 0.210331 0.832324 0.753896 0.199 Uiso 0.5 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I2 3.1933(8) . ?
Pb1 I2 3.1933(8) 7_575 ?
Pb1 I1 3.2652(12) . ?
Pb1 I2 3.2705(8) 4_565 ?
Pb1 I2 3.2705(8) 6_656 ?
Pb1 I1 3.2915(13) 6_556 ?
N1 H1C 0.8632 . ?
N1 H1D 0.8629 . ?
N1 H1E 0.8528 . ?
N1 H1D 0.8629 7_575 ?
O2 C3 1.415(14) . ?
O2 C4 1.447(14) . ?
O3 C6 1.413(14) . ?
O3 C5 1.415(14) . ?
O1 C1 1.409(18) . ?
O1 C2 1.406(14) . ?
C1 C1 1.47(2) 7_575 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.466(19) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.491(19) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C6 1.46(2) 7_575 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
O1A C1A 1.424(14) 7_575 ?
O1A C1A 1.424(14) . ?
O2A C3A 1.425(14) . ?
O2A C2A 1.428(14) . ?
O3A C4A 1.412(19) . ?
O3A C5A 1.41(2) . ?
O4A C6A 1.415(14) . ?
O4A C6A 1.415(14) 7_575 ?
C1A C2A 1.484(14) . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C3A C4A 1.479(14) . ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C5A C6A 1.493(14) . ?
C5A H5AA 0.9700 . ?
C5A H5AB 0.9700 . ?
C6A H6AA 0.9700 . ?
C6A H6AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I2 Pb1 I2 85.57(3) . 7_575 ?
I2 Pb1 I1 95.57(3) . . ?
I2 Pb1 I1 95.57(3) 7_575 . ?
I2 Pb1 I2 177.90(3) . 4_565 ?
I2 Pb1 I2 95.64(2) 7_575 4_565 ?
I1 Pb1 I2 82.61(2) . 4_565 ?
I2 Pb1 I2 95.64(2) . 6_656 ?
I2 Pb1 I2 177.90(3) 7_575 6_656 ?
I1 Pb1 I2 82.61(2) . 6_656 ?
I2 Pb1 I2 83.09(3) 4_565 6_656 ?
I2 Pb1 I1 83.39(2) . 6_556 ?
I2 Pb1 I1 83.39(2) 7_575 6_556 ?
I1 Pb1 I1 178.58(3) . 6_556 ?
I2 Pb1 I1 98.44(3) 4_565 6_556 ?
I2 Pb1 I1 98.44(3) 6_656 6_556 ?
Pb1 I1 Pb1 78.65(3) . 6_656 ?
Pb1 I2 Pb1 80.000(17) . 6_556 ?
H1C N1 H1D 112.7 . . ?
H1C N1 H1E 98.5 . . ?
H1D N1 H1E 99.9 . . ?
H1C N1 H1D 112.7 . 7_575 ?
H1D N1 H1D 126.4 . 7_575 ?
H1E N1 H1D 99.9 . 7_575 ?
C3 O2 C4 116(2) . . ?
C6 O3 C5 112.9(15) . . ?
C1 O1 C2 108(2) . . ?
O1 C1 C1 116.6(12) . 7_575 ?
O1 C1 H1A 108.1 . . ?
C1 C1 H1A 108.1 7_575 . ?
O1 C1 H1B 108.1 . . ?
C1 C1 H1B 108.1 7_575 . ?
H1A C1 H1B 107.3 . . ?
O1 C2 C3 112(3) . . ?
O1 C2 H2A 109.3 . . ?
C3 C2 H2A 109.3 . . ?
O1 C2 H2B 109.3 . . ?
C3 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
O2 C3 C2 117(3) . . ?
O2 C3 H3A 108.2 . . ?
C2 C3 H3A 108.2 . . ?
O2 C3 H3B 108.2 . . ?
C2 C3 H3B 108.2 . . ?
H3A C3 H3B 107.3 . . ?
O2 C4 C5 113(3) . . ?
O2 C4 H4A 109.0 . . ?
C5 C4 H4A 109.0 . . ?
O2 C4 H4B 109.0 . . ?
C5 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
O3 C5 C4 120(3) . . ?
O3 C5 H5A 107.4 . . ?
C4 C5 H5A 107.4 . . ?
O3 C5 H5B 107.4 . . ?
C4 C5 H5B 107.4 . . ?
H5A C5 H5B 106.9 . . ?
O3 C6 C6 115.9(11) . 7_575 ?
O3 C6 H6A 108.3 . . ?
C6 C6 H6A 108.3 7_575 . ?
O3 C6 H6B 108.3 . . ?
C6 C6 H6B 108.3 7_575 . ?
H6A C6 H6B 107.4 . . ?
C1A O1A C1A 145(5) 7_575 . ?
C3A O2A C2A 115.5(17) . . ?
C4A O3A C5A 100(2) . . ?
O1A C1A C2A 126(4) . . ?
O1A C1A H1AA 105.8 . . ?
C2A C1A H1AA 105.8 . . ?
O1A C1A H1AB 105.8 . . ?
C2A C1A H1AB 105.8 . . ?
H1AA C1A H1AB 106.2 . . ?
O2A C2A C1A 88(3) . . ?
O2A C2A H2AA 114.0 . . ?
C1A C2A H2AA 114.0 . . ?
O2A C2A H2AB 114.0 . . ?
C1A C2A H2AB 114.0 . . ?
H2AA C2A H2AB 111.2 . . ?
O2A C3A C4A 110.1(17) . . ?
O2A C3A H3AA 109.6 . . ?
C4A C3A H3AA 109.6 . . ?
O2A C3A H3AB 109.6 . . ?
C4A C3A H3AB 109.6 . . ?
H3AA C3A H3AB 108.1 . . ?
O3A C4A C3A 107.6(18) . . ?
O3A C4A H4AA 110.2 . . ?
C3A C4A H4AA 110.2 . . ?
O3A C4A H4AB 110.2 . . ?
C3A C4A H4AB 110.2 . . ?
H4AA C4A H4AB 108.5 . . ?
O3A C5A C6A 94(3) . . ?
O3A C5A H5AA 112.9 . . ?
C6A C5A H5AA 112.9 . . ?
O3A C5A H5AB 112.9 . . ?
C6A C5A H5AB 112.9 . . ?
H5AA C5A H5AB 110.3 . . ?
O4A C6A C5A 98(3) . . ?
O4A C6A H6AA 112.1 . . ?
C5A C6A H6AA 112.1 . . ?
O4A C6A H6AB 112.1 . . ?
C5A C6A H6AB 112.1 . . ?
H6AA C6A H6AB 109.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 O1 C1 C1 -168(2) . . . 7_575 ?
C1 O1 C2 C3 -179(3) . . . . ?
C4 O2 C3 C2 -169(4) . . . . ?
O1 C2 C3 O2 -31(6) . . . . ?
C3 O2 C4 C5 -162(3) . . . . ?
C6 O3 C5 C4 174(4) . . . . ?
O2 C4 C5 O3 -9(6) . . . . ?
C5 O3 C6 C6 180(2) . . . 7_575 ?
C1A O1A C1A C2A 166(5) 7_575 . . . ?
C3A O2A C2A C1A -180(3) . . . . ?
O1A C1A C2A O2A -102(5) . . . . ?
C2A O2A C3A C4A -156(3) . . . . ?
C5A O3A C4A C3A -177(4) . . . . ?
O2A C3A C4A O3A 85(4) . . . . ?
C4A O3A C5A C6A 174(4) . . . . ?
C6A O4A C6A C5A -176(3) 7_575 . . . ?
O3A C5A C6A O4A -101(5) . . . . ?

_refine_diff_density_max         1.259
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.146



####################################################################### 
# 
# 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_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2111967'
loop_
_audit_author_name
_audit_author_address
'guo-jun yuan'
;nanjing xiaozhuang university
China
;
_audit_update_record             
;
2022-03-10 deposited with the CCDC.	2022-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H28 I3 N O6 Pb'
_chemical_formula_weight         870.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   15.9408(9)
_cell_length_b                   8.4144(4)
_cell_length_c                   17.7939(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.858(2)
_cell_angle_gamma                90
_cell_volume                     2381.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    363(2)
_cell_measurement_reflns_used    17863
_cell_measurement_theta_min      2.294
_cell_measurement_theta_max      25.009

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.427
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    10.996
_shelx_estimated_absorpt_T_min   0.206
_shelx_estimated_absorpt_T_max   0.229
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      363(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17863
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.294
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_full        25.009
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4166
_reflns_number_gt                2893
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0313P)²+8.5108P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00254(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4166
_refine_ls_number_parameters     372
_refine_ls_number_restraints     540
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.0986
_refine_ls_wR_factor_gt          0.0880
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.75000(2) 0.63598(4) 0.25155(2) 0.05609(17) Uani 1 1 d . . . . .
I2 I 0.62413(4) 0.87775(8) 0.32237(5) 0.0821(3) Uani 1 1 d . . . . .
I1 I 0.76513(5) 0.40024(8) 0.39223(4) 0.0807(3) Uani 1 1 d . . . . .
I3 I 0.60722(4) 0.39755(7) 0.18709(4) 0.0696(2) Uani 1 1 d . . . . .
N1 N 0.7345(5) 0.6039(8) 0.5697(5) 0.077(2) Uani 1 1 d . . . . .
H1C H 0.735776 0.592700 0.524022 0.092 Uiso 1 1 d R U . . .
H1D H 0.719556 0.520750 0.587002 0.092 Uiso 1 1 d R U . . .
H1E H 0.780306 0.628350 0.587042 0.092 Uiso 1 1 d R U . . .
H1F H 0.700656 0.672760 0.577092 0.092 Uiso 1 1 d R U . . .
O1 O 0.5840(9) 0.5425(19) 0.6574(9) 0.091(4) Uani 0.537(9) 1 d D U P A 1
O2 O 0.5872(10) 0.8261(18) 0.5762(10) 0.095(5) Uani 0.537(9) 1 d D U P A 1
O3 O 0.7475(9) 0.9665(17) 0.5703(8) 0.089(4) Uani 0.537(9) 1 d D U P A 1
O4 O 0.8901(9) 0.7557(17) 0.5670(9) 0.097(4) Uani 0.537(9) 1 d D U P A 1
O5 O 0.8866(10) 0.4873(18) 0.6560(9) 0.103(5) Uani 0.537(9) 1 d D U P A 1
O6 O 0.7277(10) 0.3529(17) 0.6767(9) 0.093(4) Uani 0.537(9) 1 d D U P A 1
C1 C 0.5142(15) 0.606(3) 0.6130(16) 0.107(6) Uani 0.537(9) 1 d D U P A 1
H1A H 0.462086 0.567339 0.631481 0.128 Uiso 0.537(9) 1 calc R U P A 1
H1B H 0.516553 0.572454 0.560986 0.128 Uiso 0.537(9) 1 calc R U P A 1
C2 C 0.5179(14) 0.781(3) 0.6181(15) 0.098(6) Uani 0.537(9) 1 d D U P A 1
H2A H 0.466184 0.828098 0.596576 0.117 Uiso 0.537(9) 1 calc R U P A 1
H2B H 0.526747 0.814857 0.670152 0.117 Uiso 0.537(9) 1 calc R U P A 1
C3 C 0.6019(16) 0.992(2) 0.5872(15) 0.103(6) Uani 0.537(9) 1 d D U P A 1
H3A H 0.619168 1.014567 0.639332 0.123 Uiso 0.537(9) 1 calc R U P A 1
H3B H 0.551884 1.052881 0.572529 0.123 Uiso 0.537(9) 1 calc R U P A 1
C4 C 0.6699(13) 1.026(4) 0.5377(18) 0.104(6) Uani 0.537(9) 1 d D U P A 1
H4A H 0.657364 0.977367 0.488871 0.125 Uiso 0.537(9) 1 calc R U P A 1
H4B H 0.674171 1.140108 0.530483 0.125 Uiso 0.537(9) 1 calc R U P A 1
C5 C 0.8148(12) 0.982(3) 0.5229(14) 0.099(6) Uani 0.537(9) 1 d D U P A 1
H5A H 0.820047 1.092666 0.508666 0.119 Uiso 0.537(9) 1 calc R U P A 1
H5B H 0.802216 0.920924 0.477321 0.119 Uiso 0.537(9) 1 calc R U P A 1
C6 C 0.8963(14) 0.926(2) 0.5600(15) 0.091(6) Uani 0.537(9) 1 d D U P A 1
H6A H 0.942467 0.954402 0.529663 0.110 Uiso 0.537(9) 1 calc R U P A 1
H6B H 0.906067 0.975051 0.609236 0.110 Uiso 0.537(9) 1 calc R U P A 1
C7 C 0.9622(14) 0.686(3) 0.6025(17) 0.106(6) Uani 0.537(9) 1 d D U P A 1
H7A H 0.971013 0.725759 0.653587 0.127 Uiso 0.537(9) 1 calc R U P A 1
H7B H 1.011061 0.712885 0.575389 0.127 Uiso 0.537(9) 1 calc R U P A 1
C8 C 0.9502(15) 0.511(3) 0.6032(15) 0.107(6) Uani 0.537(9) 1 d D U P A 1
H8A H 0.931373 0.472557 0.553616 0.128 Uiso 0.537(9) 1 calc R U P A 1
H8B H 1.002004 0.457669 0.619841 0.128 Uiso 0.537(9) 1 calc R U P A 1
C9 C 0.8686(18) 0.324(2) 0.6720(17) 0.117(6) Uani 0.537(9) 1 d D U P A 1
H9A H 0.918944 0.273867 0.694663 0.140 Uiso 0.537(9) 1 calc R U P A 1
H9B H 0.853160 0.269174 0.625103 0.140 Uiso 0.537(9) 1 calc R U P A 1
C10 C 0.7993(14) 0.307(4) 0.7236(15) 0.101(6) Uani 0.537(9) 1 d D U P A 1
H10A H 0.794386 0.197672 0.740637 0.121 Uiso 0.537(9) 1 calc R U P A 1
H10B H 0.807653 0.375927 0.767008 0.121 Uiso 0.537(9) 1 calc R U P A 1
C11 C 0.6605(13) 0.328(3) 0.7244(15) 0.100(6) Uani 0.537(9) 1 d D U P A 1
H11A H 0.677276 0.368756 0.774241 0.120 Uiso 0.537(9) 1 calc R U P A 1
H11B H 0.650806 0.215177 0.728927 0.120 Uiso 0.537(9) 1 calc R U P A 1
C12 C 0.5822(15) 0.405(3) 0.6978(15) 0.092(6) Uani 0.537(9) 1 d D U P A 1
H12A H 0.550115 0.327651 0.667115 0.110 Uiso 0.537(9) 1 calc R U P A 1
H12B H 0.550706 0.425456 0.741543 0.110 Uiso 0.537(9) 1 calc R U P A 1
O1A O 0.5711(11) 0.650(2) 0.6293(11) 0.094(5) Uani 0.463(9) 1 d D U P A 2
O2A O 0.6488(11) 0.8884(19) 0.5565(10) 0.092(5) Uani 0.463(9) 1 d D U P A 2
O3A O 0.8277(11) 0.904(2) 0.5690(11) 0.100(5) Uani 0.463(9) 1 d D U P A 2
O4A O 0.9161(13) 0.622(2) 0.5959(13) 0.116(6) Uani 0.463(9) 1 d D U P A 2
O5A O 0.8358(11) 0.413(2) 0.6923(11) 0.100(5) Uani 0.463(9) 1 d D U P A 2
O6A O 0.6615(11) 0.3797(18) 0.6767(10) 0.082(5) Uani 0.463(9) 1 d D U P A 2
C1A C 0.5231(18) 0.756(3) 0.5811(17) 0.097(6) Uani 0.463(9) 1 d D U P A 2
H1AA H 0.467032 0.768960 0.598325 0.117 Uiso 0.463(9) 1 calc R U P A 2
H1AB H 0.518241 0.715250 0.530001 0.117 Uiso 0.463(9) 1 calc R U P A 2
C2A C 0.5687(14) 0.912(3) 0.5838(19) 0.096(6) Uani 0.463(9) 1 d D U P A 2
H2AA H 0.537490 0.989599 0.553028 0.115 Uiso 0.463(9) 1 calc R U P A 2
H2AB H 0.574452 0.950873 0.635190 0.115 Uiso 0.463(9) 1 calc R U P A 2
C3A C 0.6935(18) 1.042(3) 0.547(2) 0.103(7) Uani 0.463(9) 1 d D U P A 2
H3AA H 0.661191 1.111673 0.512659 0.124 Uiso 0.463(9) 1 calc R U P A 2
H3AB H 0.704180 1.095443 0.594911 0.124 Uiso 0.463(9) 1 calc R U P A 2
C4A C 0.7709(18) 0.995(4) 0.5161(17) 0.110(7) Uani 0.463(9) 1 d D U P A 2
H4AA H 0.799929 1.089288 0.500471 0.132 Uiso 0.463(9) 1 calc R U P A 2
H4AB H 0.757823 0.930487 0.471633 0.132 Uiso 0.463(9) 1 calc R U P A 2
C5A C 0.9034(16) 0.869(4) 0.5339(17) 0.108(7) Uani 0.463(9) 1 d D U P A 2
H5AA H 0.932468 0.966462 0.522678 0.129 Uiso 0.463(9) 1 calc R U P A 2
H5AB H 0.890500 0.812293 0.487027 0.129 Uiso 0.463(9) 1 calc R U P A 2
C6A C 0.9572(18) 0.769(3) 0.5862(19) 0.108(7) Uani 0.463(9) 1 d D U P A 2
H6AA H 1.011286 0.751819 0.565783 0.129 Uiso 0.463(9) 1 calc R U P A 2
H6AB H 0.966486 0.822752 0.634402 0.129 Uiso 0.463(9) 1 calc R U P A 2
C7A C 0.9616(17) 0.517(3) 0.6479(17) 0.105(7) Uani 0.463(9) 1 d D U P A 2
H7AA H 0.972260 0.569382 0.696201 0.126 Uiso 0.463(9) 1 calc R U P A 2
H7AB H 1.015211 0.489010 0.628781 0.126 Uiso 0.463(9) 1 calc R U P A 2
C8A C 0.9104(16) 0.373(3) 0.657(2) 0.112(7) Uani 0.463(9) 1 d D U P A 2
H8AA H 0.895688 0.326502 0.607692 0.134 Uiso 0.463(9) 1 calc R U P A 2
H8AB H 0.942440 0.295315 0.686914 0.134 Uiso 0.463(9) 1 calc R U P A 2
C9A C 0.7962(17) 0.268(3) 0.7064(19) 0.093(7) Uani 0.463(9) 1 d D U P A 2
H9AA H 0.829684 0.205481 0.743153 0.112 Uiso 0.463(9) 1 calc R U P A 2
H9AB H 0.786895 0.206502 0.660499 0.112 Uiso 0.463(9) 1 calc R U P A 2
C10A C 0.7152(16) 0.315(3) 0.7363(14) 0.096(6) Uani 0.463(9) 1 d D U P A 2
H10C H 0.688667 0.223731 0.757720 0.115 Uiso 0.463(9) 1 calc R U P A 2
H10D H 0.725088 0.394196 0.775673 0.115 Uiso 0.463(9) 1 calc R U P A 2
C11A C 0.5755(14) 0.380(3) 0.6692(19) 0.094(7) Uani 0.463(9) 1 d D U P A 2
H11C H 0.556265 0.380251 0.719754 0.113 Uiso 0.463(9) 1 calc R U P A 2
H11D H 0.558502 0.279465 0.646653 0.113 Uiso 0.463(9) 1 calc R U P A 2
C12A C 0.5278(16) 0.502(2) 0.6277(16) 0.091(6) Uani 0.463(9) 1 d D U P A 2
H12C H 0.517171 0.468322 0.575792 0.109 Uiso 0.463(9) 1 calc R U P A 2
H12D H 0.473959 0.515727 0.649201 0.109 Uiso 0.463(9) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I2 3.1769(7) . ?
Pb1 I3 3.1890(7) . ?
Pb1 I1 3.1903(8) . ?
Pb1 I2 3.2912(7) 2_645 ?
Pb1 I3 3.2987(7) 2_655 ?
Pb1 I1 3.3859(8) 2_655 ?
N1 H1C 0.8193 . ?
N1 H1D 0.8072 . ?
N1 H1E 0.7999 . ?
N1 H1F 0.8090 . ?
O1 C12 1.367(17) . ?
O1 C1 1.423(17) . ?
O2 C3 1.423(17) . ?
O2 C2 1.425(17) . ?
O3 C5 1.414(17) . ?
O3 C4 1.422(18) . ?
O4 C7 1.400(17) . ?
O4 C6 1.446(17) . ?
O5 C9 1.437(17) . ?
O5 C8 1.442(17) . ?
O6 C10 1.421(18) . ?
O6 C11 1.426(17) . ?
C1 C2 1.479(18) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.471(18) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.493(18) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.483(18) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.491(19) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.453(18) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
O1A C1A 1.423(18) . ?
O1A C12A 1.424(17) . ?
O2A C2A 1.410(18) . ?
O2A C3A 1.490(19) . ?
O3A C5A 1.427(18) . ?
O3A C4A 1.473(18) . ?
O4A C6A 1.420(18) . ?
O4A C7A 1.438(18) . ?
O5A C9A 1.407(18) . ?
O5A C8A 1.424(18) . ?
O6A C11A 1.368(18) . ?
O6A C10A 1.424(18) . ?
C1A C2A 1.497(18) . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C3A C4A 1.439(19) . ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C5A C6A 1.482(19) . ?
C5A H5AA 0.9700 . ?
C5A H5AB 0.9700 . ?
C6A H6AA 0.9700 . ?
C6A H6AB 0.9700 . ?
C7A C8A 1.477(19) . ?
C7A H7AA 0.9700 . ?
C7A H7AB 0.9700 . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C9A C10A 1.484(19) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C11A C12A 1.448(18) . ?
C11A H11C 0.9700 . ?
C11A H11D 0.9700 . ?
C12A H12C 0.9700 . ?
C12A H12D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I2 Pb1 I3 95.218(19) . . ?
I2 Pb1 I1 95.93(2) . . ?
I3 Pb1 I1 84.58(2) . . ?
I2 Pb1 I2 178.303(19) . 2_645 ?
I3 Pb1 I2 83.14(2) . 2_645 ?
I1 Pb1 I2 83.52(2) . 2_645 ?
I2 Pb1 I3 83.200(18) . 2_655 ?
I3 Pb1 I3 176.996(19) . 2_655 ?
I1 Pb1 I3 98.11(2) . 2_655 ?
I2 Pb1 I3 98.463(19) 2_645 2_655 ?
I2 Pb1 I1 82.21(2) . 2_655 ?
I3 Pb1 I1 97.39(2) . 2_655 ?
I1 Pb1 I1 177.39(2) . 2_655 ?
I2 Pb1 I1 98.39(2) 2_645 2_655 ?
I3 Pb1 I1 79.886(19) 2_655 2_655 ?
Pb1 I2 Pb1 81.139(16) . 2_655 ?
Pb1 I1 Pb1 79.494(17) . 2_645 ?
Pb1 I3 Pb1 80.843(14) . 2_645 ?
H1C N1 H1D 107.9 . . ?
H1C N1 H1E 109.3 . . ?
H1D N1 H1E 111.2 . . ?
H1C N1 H1F 107.8 . . ?
H1D N1 H1F 109.9 . . ?
H1E N1 H1F 110.8 . . ?
C12 O1 C1 124.5(19) . . ?
C3 O2 C2 108.3(18) . . ?
C5 O3 C4 113.4(19) . . ?
C7 O4 C6 113.2(17) . . ?
C9 O5 C8 114.9(18) . . ?
C10 O6 C11 102.5(19) . . ?
O1 C1 C2 108(2) . . ?
O1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
O1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
O2 C2 C1 105(2) . . ?
O2 C2 H2A 110.7 . . ?
C1 C2 H2A 110.7 . . ?
O2 C2 H2B 110.7 . . ?
C1 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
O2 C3 C4 103(2) . . ?
O2 C3 H3A 111.1 . . ?
C4 C3 H3A 111.1 . . ?
O2 C3 H3B 111.1 . . ?
C4 C3 H3B 111.1 . . ?
H3A C3 H3B 109.0 . . ?
O3 C4 C3 110(2) . . ?
O3 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
O3 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
O3 C5 C6 112(2) . . ?
O3 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
O3 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?
O4 C6 C5 106.7(18) . . ?
O4 C6 H6A 110.4 . . ?
C5 C6 H6A 110.4 . . ?
O4 C6 H6B 110.4 . . ?
C5 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
O4 C7 C8 108(2) . . ?
O4 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
O4 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
O5 C8 C7 104(2) . . ?
O5 C8 H8A 111.0 . . ?
C7 C8 H8A 111.0 . . ?
O5 C8 H8B 111.0 . . ?
C7 C8 H8B 111.0 . . ?
H8A C8 H8B 109.0 . . ?
O5 C9 C10 112(2) . . ?
O5 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
O5 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
O6 C10 C9 102(2) . . ?
O6 C10 H10A 111.3 . . ?
C9 C10 H10A 111.3 . . ?
O6 C10 H10B 111.3 . . ?
C9 C10 H10B 111.3 . . ?
H10A C10 H10B 109.2 . . ?
O6 C11 C12 114(2) . . ?
O6 C11 H11A 108.8 . . ?
C12 C11 H11A 108.8 . . ?
O6 C11 H11B 108.8 . . ?
C12 C11 H11B 108.8 . . ?
H11A C11 H11B 107.6 . . ?
O1 C12 C11 120(2) . . ?
O1 C12 H12A 107.4 . . ?
C11 C12 H12A 107.4 . . ?
O1 C12 H12B 107.4 . . ?
C11 C12 H12B 107.4 . . ?
H12A C12 H12B 106.9 . . ?
C1A O1A C12A 107(2) . . ?
C2A O2A C3A 112(2) . . ?
C5A O3A C4A 109(2) . . ?
C6A O4A C7A 113(2) . . ?
C9A O5A C8A 106(2) . . ?
C11A O6A C10A 128(2) . . ?
O1A C1A C2A 107(2) . . ?
O1A C1A H1AA 110.4 . . ?
C2A C1A H1AA 110.4 . . ?
O1A C1A H1AB 110.4 . . ?
C2A C1A H1AB 110.4 . . ?
H1AA C1A H1AB 108.6 . . ?
O2A C2A C1A 108(2) . . ?
O2A C2A H2AA 110.0 . . ?
C1A C2A H2AA 110.0 . . ?
O2A C2A H2AB 110.0 . . ?
C1A C2A H2AB 110.0 . . ?
H2AA C2A H2AB 108.4 . . ?
C4A C3A O2A 104(2) . . ?
C4A C3A H3AA 111.1 . . ?
O2A C3A H3AA 111.1 . . ?
C4A C3A H3AB 111.1 . . ?
O2A C3A H3AB 111.1 . . ?
H3AA C3A H3AB 109.0 . . ?
C3A C4A O3A 114(3) . . ?
C3A C4A H4AA 108.8 . . ?
O3A C4A H4AA 108.8 . . ?
C3A C4A H4AB 108.8 . . ?
O3A C4A H4AB 108.8 . . ?
H4AA C4A H4AB 107.7 . . ?
O3A C5A C6A 108(2) . . ?
O3A C5A H5AA 110.0 . . ?
C6A C5A H5AA 110.0 . . ?
O3A C5A H5AB 110.0 . . ?
C6A C5A H5AB 110.0 . . ?
H5AA C5A H5AB 108.4 . . ?
O4A C6A C5A 109(2) . . ?
O4A C6A H6AA 110.0 . . ?
C5A C6A H6AA 110.0 . . ?
O4A C6A H6AB 110.0 . . ?
C5A C6A H6AB 110.0 . . ?
H6AA C6A H6AB 108.4 . . ?
O4A C7A C8A 108(2) . . ?
O4A C7A H7AA 110.1 . . ?
C8A C7A H7AA 110.1 . . ?
O4A C7A H7AB 110.1 . . ?
C8A C7A H7AB 110.1 . . ?
H7AA C7A H7AB 108.4 . . ?
O5A C8A C7A 110(2) . . ?
O5A C8A H8AA 109.7 . . ?
C7A C8A H8AA 109.7 . . ?
O5A C8A H8AB 109.7 . . ?
C7A C8A H8AB 109.7 . . ?
H8AA C8A H8AB 108.2 . . ?
O5A C9A C10A 104(2) . . ?
O5A C9A H9AA 111.0 . . ?
C10A C9A H9AA 111.0 . . ?
O5A C9A H9AB 111.0 . . ?
C10A C9A H9AB 111.0 . . ?
H9AA C9A H9AB 109.0 . . ?
O6A C10A C9A 109(2) . . ?
O6A C10A H10C 109.8 . . ?
C9A C10A H10C 109.8 . . ?
O6A C10A H10D 109.8 . . ?
C9A C10A H10D 109.8 . . ?
H10C C10A H10D 108.3 . . ?
O6A C11A C12A 123(2) . . ?
O6A C11A H11C 106.6 . . ?
C12A C11A H11C 106.6 . . ?
O6A C11A H11D 106.6 . . ?
C12A C11A H11D 106.6 . . ?
H11C C11A H11D 106.6 . . ?
O1A C12A C11A 112(2) . . ?
O1A C12A H12C 109.2 . . ?
C11A C12A H12C 109.2 . . ?
O1A C12A H12D 109.2 . . ?
C11A C12A H12D 109.2 . . ?
H12C C12A H12D 107.9 . . ?

_refine_diff_density_max         0.948
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.150



####################################################################### 
# 
# 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_1_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2111965'
loop_
_audit_author_name
_audit_author_address
'guo-jun yuan'
;nanjing xiaozhuang university
China
;
_audit_update_record             
;
2022-03-10 deposited with the CCDC.	2022-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H28 I3 N O6 Pb'
_chemical_formula_weight         870.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   15.9339(7)
_cell_length_b                   8.5831(3)
_cell_length_c                   17.2046(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.483(2)
_cell_angle_gamma                90
_cell_volume                     2337.89(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    323(2)
_cell_measurement_reflns_used    17544
_cell_measurement_theta_min      2.383
_cell_measurement_theta_max      25.006

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.472
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    11.200
_shelx_estimated_absorpt_T_min   0.202
_shelx_estimated_absorpt_T_max   0.225
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      323(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17544
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.383
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_full        25.006
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             4086
_reflns_number_gt                3211
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0585P)²+4.0028P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00276(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4086
_refine_ls_number_parameters     209
_refine_ls_number_restraints     217
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.1115
_refine_ls_wR_factor_gt          0.1039
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.054
_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
Pb1 Pb 0.25007(2) 0.38350(3) 0.24870(2) 0.04382(16) Uani 1 1 d . . . . .
I1 I 0.22615(5) 0.59844(7) 0.10338(4) 0.0639(2) Uani 1 1 d . . . . .
I2 I 0.39516(3) 0.62850(6) 0.31409(4) 0.0557(2) Uani 1 1 d . . . . .
I3 I 0.37161(4) 0.15993(7) 0.17496(5) 0.0645(2) Uani 1 1 d . . . . .
O1 O 0.7130(6) 0.3764(8) 0.1749(5) 0.086(2) Uani 1 1 d . U . . .
O2 O 0.5786(5) 0.5857(10) 0.1564(5) 0.091(2) Uani 1 1 d . U . . .
O3 O 0.5900(6) 0.8680(9) 0.0762(5) 0.093(2) Uani 1 1 d . U . . .
O4 O 0.7548(5) 0.9842(8) 0.0701(5) 0.0829(19) Uani 1 1 d . U . . .
O5 O 0.8881(4) 0.7628(10) 0.0730(5) 0.089(2) Uani 1 1 d . U . . .
O6 O 0.8782(5) 0.4916(9) 0.1612(5) 0.092(2) Uani 1 1 d . U . . .
C1 C 0.6483(8) 0.3669(12) 0.2160(9) 0.088(3) Uani 1 1 d . U . . .
H1B H 0.661114 0.425536 0.264025 0.106 Uiso 1 1 calc R U . . .
H1A H 0.640589 0.258806 0.230047 0.106 Uiso 1 1 calc R U . . .
C2 C 0.5723(7) 0.4230(13) 0.1763(8) 0.084(3) Uani 1 1 d . U . . .
H2A H 0.527156 0.409383 0.209131 0.101 Uiso 1 1 calc R U . . .
H2B H 0.558160 0.362901 0.128906 0.101 Uiso 1 1 calc R U . . .
C3 C 0.5089(9) 0.6494(15) 0.1159(10) 0.105(3) Uani 1 1 d . U . . .
H3A H 0.459212 0.621180 0.140523 0.127 Uiso 1 1 calc R U . . .
H3B H 0.502167 0.609042 0.062918 0.127 Uiso 1 1 calc R U . . .
C4 C 0.5171(8) 0.8199(16) 0.1141(8) 0.097(3) Uani 1 1 d . U . . .
H4A H 0.466327 0.864190 0.086257 0.116 Uiso 1 1 calc R U . . .
H4B H 0.522560 0.859742 0.167196 0.116 Uiso 1 1 calc R U . . .
C5 C 0.6085(8) 1.0242(14) 0.0844(8) 0.096(3) Uani 1 1 d . U . . .
H5B H 0.623489 1.049120 0.139151 0.115 Uiso 1 1 calc R U . . .
H5A H 0.559428 1.085704 0.065032 0.115 Uiso 1 1 calc R U . . .
C6 C 0.6778(8) 1.0604(13) 0.0407(7) 0.082(3) Uani 1 1 d . U . . .
H6B H 0.662963 1.030053 -0.013444 0.098 Uiso 1 1 calc R U . . .
H6A H 0.686938 1.172140 0.041827 0.098 Uiso 1 1 calc R U . . .
C7 C 0.8153(8) 0.9907(15) 0.0205(8) 0.093(3) Uani 1 1 d . U . . .
H7A H 0.823722 1.098239 0.005810 0.112 Uiso 1 1 calc R U . . .
H7B H 0.796616 0.932694 -0.026646 0.112 Uiso 1 1 calc R U . . .
C8 C 0.8972(7) 0.9248(14) 0.0574(8) 0.088(3) Uani 1 1 d . U . . .
H8B H 0.940366 0.939315 0.022579 0.106 Uiso 1 1 calc R U . . .
H8A H 0.914798 0.979498 0.105812 0.106 Uiso 1 1 calc R U . . .
C9 C 0.9589(8) 0.6912(14) 0.1070(9) 0.098(3) Uani 1 1 d D U . . .
H9B H 0.975287 0.737942 0.157825 0.118 Uiso 1 1 calc R U . . .
H9A H 1.004464 0.707770 0.075080 0.118 Uiso 1 1 calc R U . . .
C10 C 0.9466(7) 0.5242(13) 0.1168(8) 0.094(3) Uani 1 1 d D U . . .
H10A H 0.935508 0.475779 0.065764 0.113 Uiso 1 1 calc R U . . .
H10B H 0.997971 0.479008 0.143046 0.113 Uiso 1 1 calc R U . . .
C11 C 0.8614(8) 0.3386(14) 0.1649(9) 0.094(3) Uani 1 1 d . U . . .
H11A H 0.911666 0.283499 0.186944 0.113 Uiso 1 1 calc R U . . .
H11B H 0.845186 0.298631 0.112651 0.113 Uiso 1 1 calc R U . . .
C12 C 0.7919(7) 0.3111(13) 0.2142(7) 0.084(3) Uani 1 1 d . U . . .
H12A H 0.785266 0.200214 0.222355 0.101 Uiso 1 1 calc R U . . .
H12B H 0.805448 0.360246 0.264837 0.101 Uiso 1 1 calc R U . . .
N1 N 0.7249(4) 0.6359(7) 0.0665(5) 0.0533(19) Uani 1 1 d . . . . .
H1C H 0.734064 0.617119 0.018877 0.064 Uiso 1 1 d R U . . .
H1D H 0.769664 0.620619 0.097197 0.064 Uiso 1 1 d R U . . .
H1E H 0.685284 0.579289 0.078707 0.064 Uiso 1 1 d R U . . .
H1F H 0.710724 0.730489 0.069617 0.064 Uiso 1 1 d 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
Pb1 I1 3.0958(7) . ?
Pb1 I3 3.0979(6) . ?
Pb1 I2 3.2319(6) . ?
Pb1 I2 3.2783(6) 2_545 ?
Pb1 I3 3.4188(7) 2 ?
O1 C1 1.316(14) . ?
O1 C12 1.470(14) . ?
O2 C3 1.357(16) . ?
O2 C2 1.444(13) . ?
O3 C5 1.377(13) . ?
O3 C4 1.455(15) . ?
O4 C7 1.360(13) . ?
O4 C6 1.431(13) . ?
O5 C9 1.357(13) . ?
O5 C8 1.427(13) . ?
O6 C11 1.343(13) . ?
O6 C10 1.426(14) . ?
C1 C2 1.406(17) . ?
C1 H1B 0.9700 . ?
C1 H1A 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.469(16) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.439(16) . ?
C5 H5B 0.9700 . ?
C5 H5A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6A 0.9700 . ?
C7 C8 1.495(16) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8A 0.9700 . ?
C9 C10 1.460(13) . ?
C9 H9B 0.9700 . ?
C9 H9A 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.487(16) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
N1 H1C 0.8638 . ?
N1 H1D 0.8484 . ?
N1 H1E 0.8417 . ?
N1 H1F 0.8458 . ?

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 I3 93.67(2) . . ?
I1 Pb1 I2 84.917(19) . . ?
I3 Pb1 I2 95.157(17) . . ?
I1 Pb1 I2 96.533(19) . 2_545 ?
I3 Pb1 I2 84.383(17) . 2_545 ?
I2 Pb1 I2 178.501(17) . 2_545 ?
I1 Pb1 I3 82.717(18) . 2 ?
I3 Pb1 I3 174.295(19) . 2 ?
I2 Pb1 I3 80.160(17) . 2 ?
I2 Pb1 I3 100.379(17) 2_545 2 ?
Pb1 I2 Pb1 82.480(13) . 2 ?
Pb1 I3 Pb1 82.225(14) . 2_545 ?
C1 O1 C12 114.3(10) . . ?
C3 O2 C2 115.9(10) . . ?
C5 O3 C4 113.8(10) . . ?
C7 O4 C6 113.5(9) . . ?
C9 O5 C8 115.2(8) . . ?
C11 O6 C10 112.7(9) . . ?
O1 C1 C2 113.7(13) . . ?
O1 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
O1 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
H1B C1 H1A 107.7 . . ?
C1 C2 O2 111.5(9) . . ?
C1 C2 H2A 109.3 . . ?
O2 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
O2 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
O2 C3 C4 110.0(12) . . ?
O2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
O2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
O3 C4 C3 111.7(11) . . ?
O3 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
O3 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
O3 C5 C6 109.0(11) . . ?
O3 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
O3 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
H5B C5 H5A 108.3 . . ?
O4 C6 C5 113.2(10) . . ?
O4 C6 H6B 108.9 . . ?
C5 C6 H6B 108.9 . . ?
O4 C6 H6A 108.9 . . ?
C5 C6 H6A 108.9 . . ?
H6B C6 H6A 107.7 . . ?
O4 C7 C8 111.4(11) . . ?
O4 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
O4 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
O5 C8 C7 110.3(9) . . ?
O5 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
O5 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
H8B C8 H8A 108.1 . . ?
O5 C9 C10 112.3(10) . . ?
O5 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
O5 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
H9B C9 H9A 107.9 . . ?
O6 C10 C9 112.0(10) . . ?
O6 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
O6 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
O6 C11 C12 110.4(11) . . ?
O6 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
O6 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
O1 C12 C11 109.3(10) . . ?
O1 C12 H12A 109.8 . . ?
C11 C12 H12A 109.8 . . ?
O1 C12 H12B 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
H1C N1 H1D 109.9 . . ?
H1C N1 H1E 109.9 . . ?
H1D N1 H1E 110.9 . . ?
H1C N1 H1F 108.3 . . ?
H1D N1 H1F 108.7 . . ?
H1E N1 H1F 109.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2A I3 0.97 3.28 3.912(10) 124.7 . yes
C3 H3A I2 0.97 3.26 4.042(16) 138.6 . yes
C6 H6B I3 0.97 3.22 4.159(13) 164.8 3_665 yes
C7 H7A I1 0.97 3.26 4.135(13) 151.5 3_675 yes
N1 H1C I1 0.86 2.92 3.703(8) 151.0 3_665 yes
N1 H1D O5 0.85 2.32 2.810(10) 116.8 . yes
N1 H1D O6 0.85 2.24 3.042(10) 158.8 . yes
N1 H1E O1 0.84 2.41 2.925(11) 120.3 . yes
N1 H1E O2 0.84 2.28 2.971(11) 139.7 . yes
N1 H1F O3 0.85 2.27 2.949(10) 137.4 . yes
N1 H1F O4 0.85 2.29 3.027(9) 146.1 . yes

_refine_diff_density_max         0.857
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.174



####################################################################### 
# 
# 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_1_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2111964'
loop_
_audit_author_name
_audit_author_address
'guo-jun yuan'
;nanjing xiaozhuang university
China
;
_audit_update_record             
;
2022-03-10 deposited with the CCDC.	2022-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H28 I3 N O6 Pb'
_chemical_formula_weight         870.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   15.9371(6)
_cell_length_b                   8.6190(3)
_cell_length_c                   17.0413(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.0200(10)
_cell_angle_gamma                90
_cell_volume                     2323.28(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16237
_cell_measurement_theta_min      2.691
_cell_measurement_theta_max      25.008

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.488
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    11.270
_shelx_estimated_absorpt_T_min   0.201
_shelx_estimated_absorpt_T_max   0.223
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16237
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.691
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_full        25.008
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             4050
_reflns_number_gt                3356
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0261P)²+8.0348P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00373(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4050
_refine_ls_number_parameters     209
_refine_ls_number_restraints     217
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0800
_refine_ls_wR_factor_gt          0.0760
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.24999(2) 0.38562(3) 0.24905(2) 0.03619(12) Uani 1 1 d . . . . .
I1 I 0.22389(4) 0.59708(6) 0.10221(3) 0.05404(19) Uani 1 1 d . . . . .
I2 I 0.39563(3) 0.63395(6) 0.31457(3) 0.04663(17) Uani 1 1 d . . . . .
I3 I 0.37066(3) 0.16685(6) 0.17408(4) 0.05310(19) Uani 1 1 d . . . . .
O1 O 0.7111(4) 0.3813(6) 0.1744(4) 0.0611(15) Uani 1 1 d . U . . .
O2 O 0.5779(4) 0.5927(7) 0.1571(4) 0.0668(16) Uani 1 1 d . U . . .
O3 O 0.5907(4) 0.8739(7) 0.0771(4) 0.0659(16) Uani 1 1 d . U . . .
O4 O 0.7564(4) 0.9887(6) 0.0711(3) 0.0600(15) Uani 1 1 d . U . . .
O5 O 0.8876(4) 0.7645(7) 0.0749(4) 0.0611(15) Uani 1 1 d . U . . .
O6 O 0.8781(4) 0.4942(7) 0.1620(4) 0.0663(16) Uani 1 1 d . U . . .
C1 C 0.6451(7) 0.3719(10) 0.2189(6) 0.068(2) Uani 1 1 d . U . . .
H1B H 0.657963 0.432056 0.267011 0.082 Uiso 1 1 calc R U . . .
H1A H 0.636668 0.264785 0.233591 0.082 Uiso 1 1 calc R U . . .
C2 C 0.5691(6) 0.4310(11) 0.1736(6) 0.071(2) Uani 1 1 d . U . . .
H2A H 0.558071 0.374049 0.124357 0.085 Uiso 1 1 calc R U . . .
H2B H 0.521374 0.415914 0.203131 0.085 Uiso 1 1 calc R U . . .
C3 C 0.5080(7) 0.6635(12) 0.1146(7) 0.075(2) Uani 1 1 d . U . . .
H3A H 0.457214 0.636356 0.137616 0.090 Uiso 1 1 calc R U . . .
H3B H 0.501689 0.627348 0.060350 0.090 Uiso 1 1 calc R U . . .
C4 C 0.5193(6) 0.8311(12) 0.1165(6) 0.071(2) Uani 1 1 d . U . . .
H4A H 0.468739 0.880885 0.090649 0.085 Uiso 1 1 calc R U . . .
H4B H 0.528142 0.866427 0.170937 0.085 Uiso 1 1 calc R U . . .
C5 C 0.6106(7) 1.0314(11) 0.0848(6) 0.072(2) Uani 1 1 d . U . . .
H5B H 0.627204 1.056787 0.139919 0.086 Uiso 1 1 calc R U . . .
H5A H 0.561637 1.093605 0.065561 0.086 Uiso 1 1 calc R U . . .
C6 C 0.6796(7) 1.0641(11) 0.0390(6) 0.067(2) Uani 1 1 d . U . . .
H6B H 0.664136 1.029476 -0.015035 0.081 Uiso 1 1 calc R U . . .
H6A H 0.688869 1.175237 0.037901 0.081 Uiso 1 1 calc R U . . .
C7 C 0.8193(6) 0.9919(11) 0.0196(6) 0.070(2) Uani 1 1 d . U . . .
H7A H 0.829045 1.098109 0.004202 0.084 Uiso 1 1 calc R U . . .
H7B H 0.800387 0.933066 -0.027797 0.084 Uiso 1 1 calc R U . . .
C8 C 0.8980(6) 0.9252(11) 0.0589(6) 0.066(2) Uani 1 1 d . U . . .
H8B H 0.942554 0.938020 0.025391 0.080 Uiso 1 1 calc R U . . .
H8A H 0.914752 0.979951 0.108080 0.080 Uiso 1 1 calc R U . . .
C9 C 0.9612(6) 0.6892(11) 0.1107(6) 0.074(2) Uani 1 1 d D U . . .
H9B H 0.977069 0.731024 0.163276 0.089 Uiso 1 1 calc R U . . .
H9A H 1.007501 0.707536 0.079790 0.089 Uiso 1 1 calc R U . . .
C10 C 0.9459(6) 0.5237(11) 0.1157(6) 0.075(2) Uani 1 1 d D U . . .
H10A H 0.931526 0.481686 0.063014 0.090 Uiso 1 1 calc R U . . .
H10B H 0.996810 0.472403 0.139751 0.090 Uiso 1 1 calc R U . . .
C11 C 0.8588(7) 0.3377(10) 0.1650(6) 0.070(2) Uani 1 1 d . U . . .
H11A H 0.908248 0.280300 0.187719 0.084 Uiso 1 1 calc R U . . .
H11B H 0.842147 0.298883 0.111965 0.084 Uiso 1 1 calc R U . . .
C12 C 0.7887(6) 0.3144(11) 0.2139(6) 0.068(2) Uani 1 1 d . U . . .
H12A H 0.780733 0.204398 0.222313 0.081 Uiso 1 1 calc R U . . .
H12B H 0.802975 0.363274 0.265061 0.081 Uiso 1 1 calc R U . . .
N1 N 0.7233(4) 0.6423(6) 0.0667(4) 0.0427(15) Uani 1 1 d . . . . .
H1C H 0.732473 0.623455 0.019103 0.051 Uiso 1 1 d R U . . .
H1D H 0.768073 0.626955 0.097423 0.051 Uiso 1 1 d R U . . .
H1E H 0.683693 0.585625 0.078933 0.051 Uiso 1 1 d R U . . .
H1F H 0.709133 0.736825 0.069843 0.051 Uiso 1 1 d 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
Pb1 I3 3.0801(6) . ?
Pb1 I1 3.0827(6) . ?
Pb1 I2 3.2530(6) . ?
Pb1 I2 3.2636(6) 2_545 ?
O1 C1 1.373(11) . ?
O1 C12 1.453(11) . ?
O2 C3 1.393(12) . ?
O2 C2 1.432(11) . ?
O3 C5 1.396(11) . ?
O3 C4 1.437(11) . ?
O4 C7 1.411(10) . ?
O4 C6 1.434(11) . ?
O5 C9 1.412(11) . ?
O5 C8 1.425(10) . ?
O6 C11 1.387(10) . ?
O6 C10 1.435(11) . ?
C1 C2 1.448(14) . ?
C1 H1B 0.9700 . ?
C1 H1A 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.455(13) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.452(13) . ?
C5 H5B 0.9700 . ?
C5 H5A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6A 0.9700 . ?
C7 C8 1.466(13) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8A 0.9700 . ?
C9 C10 1.452(11) . ?
C9 H9B 0.9700 . ?
C9 H9A 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.486(14) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
N1 H1C 0.8577 . ?
N1 H1D 0.8418 . ?
N1 H1E 0.8438 . ?
N1 H1F 0.8492 . ?

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
I3 Pb1 I1 93.116(18) . . ?
I3 Pb1 I2 95.145(15) . . ?
I1 Pb1 I2 84.803(16) . . ?
I3 Pb1 I2 84.836(15) . 2_545 ?
I1 Pb1 I2 95.931(17) . 2_545 ?
I2 Pb1 I2 179.266(14) . 2_545 ?
Pb1 I2 Pb1 82.804(12) . 2 ?
C1 O1 C12 112.8(7) . . ?
C3 O2 C2 115.9(7) . . ?
C5 O3 C4 112.9(7) . . ?
C7 O4 C6 113.0(7) . . ?
C9 O5 C8 114.8(7) . . ?
C11 O6 C10 112.2(7) . . ?
O1 C1 C2 109.4(8) . . ?
O1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
O1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
H1B C1 H1A 108.2 . . ?
O2 C2 C1 110.6(8) . . ?
O2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
O2 C3 C4 109.6(9) . . ?
O2 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
O2 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
O3 C4 C3 110.3(8) . . ?
O3 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
O3 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
O3 C5 C6 108.5(8) . . ?
O3 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
O3 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
H5B C5 H5A 108.4 . . ?
O4 C6 C5 111.9(8) . . ?
O4 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
O4 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
H6B C6 H6A 107.9 . . ?
O4 C7 C8 110.0(8) . . ?
O4 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
O4 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
O5 C8 C7 110.8(7) . . ?
O5 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
O5 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
H8B C8 H8A 108.1 . . ?
O5 C9 C10 109.9(8) . . ?
O5 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
O5 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
H9B C9 H9A 108.2 . . ?
O6 C10 C9 110.5(8) . . ?
O6 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 . . ?
O6 C10 H10B 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
O6 C11 C12 109.7(8) . . ?
O6 C11 H11A 109.7 . . ?
C12 C11 H11A 109.7 . . ?
O6 C11 H11B 109.7 . . ?
C12 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
O1 C12 C11 110.0(8) . . ?
O1 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
O1 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
H1C N1 H1D 109.2 . . ?
H1C N1 H1E 110.1 . . ?
H1D N1 H1E 111.1 . . ?
H1C N1 H1F 108.5 . . ?
H1D N1 H1F 108.9 . . ?
H1E N1 H1F 109.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2B I3 0.97 3.21 3.897(9) 128.9 . yes
C3 H3A I2 0.97 3.28 4.046(11) 136.9 . yes
C4 H4A I3 0.97 3.33 3.939(9) 122.7 1_565 yes
C6 H6B I3 0.97 3.19 4.132(10) 165.5 3_665 yes
C7 H7A I1 0.97 3.24 4.121(9) 151.1 3_675 yes
C7 H7B I2 0.97 3.29 3.988(10) 130.1 4_675 yes
N1 H1C I1 0.86 2.95 3.721(6) 150.0 3_665 yes
N1 H1D O5 0.84 2.32 2.811(8) 118.0 . yes
N1 H1D O6 0.84 2.26 3.061(9) 158.2 . yes
N1 H1E O1 0.84 2.40 2.924(8) 120.7 . yes
N1 H1E O2 0.84 2.27 2.966(9) 139.4 . yes
N1 H1F O3 0.85 2.24 2.929(8) 137.8 . yes
N1 H1F O4 0.85 2.30 3.032(8) 144.9 . yes

_refine_diff_density_max         0.940
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.157



####################################################################### 
# 
# 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_1_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2111963'
loop_
_audit_author_name
_audit_author_address
'guo-jun yuan'
;nanjing xiaozhuang university
China
;
_audit_update_record             
;
2022-03-10 deposited with the CCDC.	2022-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H28 I3 N O6 Pb'
_chemical_formula_weight         870.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   15.9434(6)
_cell_length_b                   8.6315(3)
_cell_length_c                   16.9273(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.4200(10)
_cell_angle_gamma                90
_cell_volume                     2309.95(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    16056
_cell_measurement_theta_min      2.427
_cell_measurement_theta_max      25.002

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.502
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    11.335
_shelx_estimated_absorpt_T_min   0.199
_shelx_estimated_absorpt_T_max   0.222
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16056
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.427
_diffrn_reflns_theta_max         25.002
_diffrn_reflns_theta_full        25.002
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             4022
_reflns_number_gt                3449
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0183P)²+10.5979P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00304(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4022
_refine_ls_number_parameters     209
_refine_ls_number_restraints     217
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0739
_refine_ls_wR_factor_gt          0.0707
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.002
_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
Pb1 Pb 0.24986(2) 0.38614(3) 0.24939(2) 0.03106(11) Uani 1 1 d . . . . .
I1 I 0.22237(4) 0.59600(6) 0.10150(3) 0.04666(17) Uani 1 1 d . . . . .
I2 I 0.39596(3) 0.63676(6) 0.31490(3) 0.04028(15) Uani 1 1 d . . . . .
I3 I 0.37011(3) 0.17049(6) 0.17342(3) 0.04497(17) Uani 1 1 d . . . . .
O1 O 0.7109(4) 0.3837(6) 0.1739(3) 0.0489(14) Uani 1 1 d . U . . .
O2 O 0.5777(4) 0.5975(6) 0.1581(4) 0.0523(14) Uani 1 1 d . U . . .
O3 O 0.5910(4) 0.8778(6) 0.0766(3) 0.0505(14) Uani 1 1 d . U . . .
O4 O 0.7576(4) 0.9916(6) 0.0716(3) 0.0480(13) Uani 1 1 d . U . . .
O5 O 0.8876(3) 0.7656(6) 0.0754(3) 0.0491(13) Uani 1 1 d . U . . .
O6 O 0.8783(4) 0.4949(6) 0.1633(3) 0.0517(14) Uani 1 1 d . U . . .
C1 C 0.6442(6) 0.3762(9) 0.2203(6) 0.054(2) Uani 1 1 d . U . . .
H1B H 0.657628 0.437475 0.268274 0.065 Uiso 1 1 calc R U . . .
H1A H 0.635260 0.269816 0.235661 0.065 Uiso 1 1 calc R U . . .
C2 C 0.5670(6) 0.4371(10) 0.1725(6) 0.056(2) Uani 1 1 d . U . . .
H2A H 0.556781 0.381860 0.122248 0.067 Uiso 1 1 calc R U . . .
H2B H 0.518623 0.421723 0.200923 0.067 Uiso 1 1 calc R U . . .
C3 C 0.5078(6) 0.6705(11) 0.1140(6) 0.059(2) Uani 1 1 d . U . . .
H3A H 0.456555 0.643642 0.136238 0.071 Uiso 1 1 calc R U . . .
H3B H 0.501861 0.634779 0.059256 0.071 Uiso 1 1 calc R U . . .
C4 C 0.5193(6) 0.8375(11) 0.1163(6) 0.057(2) Uani 1 1 d . U . . .
H4A H 0.468887 0.887971 0.090088 0.068 Uiso 1 1 calc R U . . .
H4B H 0.528634 0.872636 0.171169 0.068 Uiso 1 1 calc R U . . .
C5 C 0.6125(6) 1.0376(10) 0.0846(5) 0.057(2) Uani 1 1 d . U . . .
H5B H 0.630220 1.062507 0.140113 0.069 Uiso 1 1 calc R U . . .
H5A H 0.563856 1.101093 0.065630 0.069 Uiso 1 1 calc R U . . .
C6 C 0.6818(6) 1.0687(10) 0.0373(5) 0.054(2) Uani 1 1 d . U . . .
H6B H 0.666051 1.032609 -0.016851 0.065 Uiso 1 1 calc R U . . .
H6A H 0.691870 1.179371 0.035558 0.065 Uiso 1 1 calc R U . . .
C7 C 0.8207(5) 0.9925(10) 0.0187(5) 0.052(2) Uani 1 1 d . U . . .
H7A H 0.830961 1.097913 0.002488 0.062 Uiso 1 1 calc R U . . .
H7B H 0.801374 0.932590 -0.028657 0.062 Uiso 1 1 calc R U . . .
C8 C 0.8984(5) 0.9258(10) 0.0594(5) 0.0518(19) Uani 1 1 d . U . . .
H8B H 0.943510 0.938147 0.026508 0.062 Uiso 1 1 calc R U . . .
H8A H 0.914670 0.980520 0.109080 0.062 Uiso 1 1 calc R U . . .
C9 C 0.9617(6) 0.6895(10) 0.1123(6) 0.060(2) Uani 1 1 d D U . . .
H9B H 0.977391 0.730498 0.165495 0.071 Uiso 1 1 calc R U . . .
H9A H 1.008165 0.707820 0.081685 0.071 Uiso 1 1 calc R U . . .
C10 C 0.9453(6) 0.5235(10) 0.1164(6) 0.061(2) Uani 1 1 d D U . . .
H10A H 0.929891 0.482833 0.063119 0.074 Uiso 1 1 calc R U . . .
H10B H 0.996186 0.470711 0.140020 0.074 Uiso 1 1 calc R U . . .
C11 C 0.8567(6) 0.3363(9) 0.1654(6) 0.053(2) Uani 1 1 d . U . . .
H11A H 0.905573 0.276606 0.187899 0.064 Uiso 1 1 calc R U . . .
H11B H 0.839020 0.299164 0.111759 0.064 Uiso 1 1 calc R U . . .
C12 C 0.7878(6) 0.3166(10) 0.2141(5) 0.057(2) Uani 1 1 d . U . . .
H12A H 0.779105 0.207203 0.223430 0.068 Uiso 1 1 calc R U . . .
H12B H 0.802595 0.366637 0.265353 0.068 Uiso 1 1 calc R U . . .
N1 N 0.7228(4) 0.6461(6) 0.0662(4) 0.0377(15) Uani 1 1 d . . . . .
H1C H 0.731923 0.627274 0.018572 0.045 Uiso 1 1 d R U . . .
H1D H 0.767523 0.630774 0.096892 0.045 Uiso 1 1 d R U . . .
H1E H 0.683143 0.589445 0.078402 0.045 Uiso 1 1 d R U . . .
H1F H 0.708583 0.740644 0.069312 0.045 Uiso 1 1 d 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
Pb1 I3 3.0710(5) . ?
Pb1 I1 3.0753(6) . ?
Pb1 I2 3.2509(6) 2_545 ?
Pb1 I2 3.2661(6) . ?
O1 C1 1.402(10) . ?
O1 C12 1.445(11) . ?
O2 C2 1.420(10) . ?
O2 C3 1.407(11) . ?
O3 C5 1.424(10) . ?
O3 C4 1.441(10) . ?
O4 C6 1.435(10) . ?
O4 C7 1.430(9) . ?
O5 C9 1.423(10) . ?
O5 C8 1.424(10) . ?
O6 C11 1.412(10) . ?
O6 C10 1.432(10) . ?
C1 C2 1.479(13) . ?
C1 H1B 0.9700 . ?
C1 H1A 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.453(12) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.470(13) . ?
C5 H5B 0.9700 . ?
C5 H5A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6A 0.9700 . ?
C7 C8 1.457(12) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8A 0.9700 . ?
C9 C10 1.460(11) . ?
C9 H9B 0.9700 . ?
C9 H9A 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.467(13) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
N1 H1C 0.8535 . ?
N1 H1D 0.8372 . ?
N1 H1E 0.8450 . ?
N1 H1F 0.8504 . ?

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
I3 Pb1 I1 92.703(17) . . ?
I3 Pb1 I2 85.217(15) . 2_545 ?
I1 Pb1 I2 95.563(16) . 2_545 ?
I3 Pb1 I2 95.000(15) . . ?
I1 Pb1 I2 84.643(16) . . ?
I2 Pb1 I2 179.694(9) 2_545 . ?
Pb1 I2 Pb1 82.940(12) 2 . ?
C1 O1 C12 112.1(7) . . ?
C2 O2 C3 115.0(7) . . ?
C5 O3 C4 112.7(7) . . ?
C6 O4 C7 111.6(6) . . ?
C9 O5 C8 114.6(6) . . ?
C11 O6 C10 112.5(6) . . ?
O1 C1 C2 108.3(7) . . ?
O1 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 . . ?
O1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
H1B C1 H1A 108.4 . . ?
O2 C2 C1 109.3(7) . . ?
O2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
O2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
O2 C3 C4 109.9(8) . . ?
O2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
O2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
O3 C4 C3 109.4(7) . . ?
O3 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
O3 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
O3 C5 C6 108.3(7) . . ?
O3 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
O3 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
H5B C5 H5A 108.4 . . ?
O4 C6 C5 110.4(7) . . ?
O4 C6 H6B 109.6 . . ?
C5 C6 H6B 109.6 . . ?
O4 C6 H6A 109.6 . . ?
C5 C6 H6A 109.6 . . ?
H6B C6 H6A 108.1 . . ?
O4 C7 C8 109.0(7) . . ?
O4 C7 H7A 109.9 . . ?
C8 C7 H7A 109.9 . . ?
O4 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
O5 C8 C7 110.9(7) . . ?
O5 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
O5 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
H8B C8 H8A 108.0 . . ?
O5 C9 C10 109.3(7) . . ?
O5 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
O5 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
H9B C9 H9A 108.3 . . ?
O6 C10 C9 110.3(7) . . ?
O6 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
O6 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
O6 C11 C12 109.2(7) . . ?
O6 C11 H11A 109.8 . . ?
C12 C11 H11A 109.8 . . ?
O6 C11 H11B 109.8 . . ?
C12 C11 H11B 109.8 . . ?
H11A C11 H11B 108.3 . . ?
O1 C12 C11 109.9(7) . . ?
O1 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
O1 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
H1C N1 H1D 108.6 . . ?
H1C N1 H1E 110.2 . . ?
H1D N1 H1E 111.2 . . ?
H1C N1 H1F 108.7 . . ?
H1D N1 H1F 109.0 . . ?
H1E N1 H1F 109.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2B I3 0.97 3.20 3.894(8) 129.9 . yes
C3 H3A I2 0.97 3.29 4.048(9) 136.2 . yes
C4 H4A I3 0.97 3.32 3.930(8) 123.2 1_565 yes
C6 H6B I3 0.97 3.17 4.112(9) 164.8 3_665 yes
C7 H7A I1 0.97 3.23 4.106(8) 151.6 3_675 yes
C7 H7B I2 0.97 3.27 3.956(8) 129.5 4_675 yes
N1 H1C I1 0.85 2.96 3.719(6) 149.3 3_665 yes
N1 H1D O5 0.84 2.31 2.809(8) 118.7 . yes
N1 H1D O6 0.84 2.29 3.082(8) 157.9 . yes
N1 H1E O1 0.84 2.40 2.928(8) 120.9 . yes
N1 H1E O2 0.84 2.29 2.978(8) 139.1 . yes
N1 H1F O3 0.85 2.23 2.922(8) 138.0 . yes
N1 H1F O4 0.85 2.30 3.033(8) 144.3 . yes

_refine_diff_density_max         1.021
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.154



####################################################################### 
# 
# 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_1_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 2111962'
loop_
_audit_author_name
_audit_author_address
'guo-jun yuan'
;nanjing xiaozhuang university
China
;
_audit_update_record             
;
2022-03-10 deposited with the CCDC.	2022-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H28 I3 N O6 Pb'
_chemical_formula_weight         870.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   15.9465(6)
_cell_length_b                   8.6266(3)
_cell_length_c                   16.7569(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.9190(10)
_cell_angle_gamma                90
_cell_volume                     2283.17(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    15778
_cell_measurement_theta_min      2.454
_cell_measurement_theta_max      25.004

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.532
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    11.468
_shelx_estimated_absorpt_T_min   0.197
_shelx_estimated_absorpt_T_max   0.219
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15778
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.454
_diffrn_reflns_theta_max         25.004
_diffrn_reflns_theta_full        25.004
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             3982
_reflns_number_gt                3602
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0212P)²+14.4712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00385(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3982
_refine_ls_number_parameters     209
_refine_ls_number_restraints     217
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0760
_refine_ls_wR_factor_gt          0.0740
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.108
_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
Pb1 Pb 0.24964(2) 0.38573(3) 0.25013(2) 0.02079(11) Uani 1 1 d . . . . .
I1 I 0.21992(4) 0.59428(6) 0.10055(3) 0.03152(16) Uani 1 1 d . . . . .
I2 I 0.39636(3) 0.63917(6) 0.31517(3) 0.02701(14) Uani 1 1 d . . . . .
I3 I 0.36930(3) 0.17408(6) 0.17212(3) 0.02979(15) Uani 1 1 d . . . . .
O1 O 0.7096(3) 0.3866(6) 0.1749(3) 0.0300(12) Uani 1 1 d . U . . .
O2 O 0.5770(3) 0.6039(6) 0.1592(3) 0.0322(12) Uani 1 1 d . U . . .
O3 O 0.5918(3) 0.8833(6) 0.0772(3) 0.0308(12) Uani 1 1 d . U . . .
O4 O 0.7588(3) 0.9970(6) 0.0724(3) 0.0291(11) Uani 1 1 d . U . . .
O5 O 0.8877(3) 0.7664(6) 0.0764(3) 0.0296(11) Uani 1 1 d . U . . .
O6 O 0.8783(3) 0.4953(6) 0.1653(3) 0.0309(12) Uani 1 1 d . U . . .
C1 C 0.6415(6) 0.3797(9) 0.2217(5) 0.0346(18) Uani 1 1 d . U . . .
H1B H 0.655406 0.441220 0.271638 0.042 Uiso 1 1 calc R U . . .
H1A H 0.631477 0.271000 0.236902 0.042 Uiso 1 1 calc R U . . .
C2 C 0.5653(5) 0.4429(10) 0.1727(5) 0.0377(18) Uani 1 1 d . U . . .
H2A H 0.554903 0.387645 0.120524 0.045 Uiso 1 1 calc R U . . .
H2B H 0.515410 0.427530 0.201124 0.045 Uiso 1 1 calc R U . . .
C3 C 0.5064(5) 0.6771(10) 0.1136(5) 0.0368(18) Uani 1 1 d . U . . .
H3A H 0.453960 0.651099 0.136086 0.044 Uiso 1 1 calc R U . . .
H3B H 0.500262 0.640853 0.057003 0.044 Uiso 1 1 calc R U . . .
C4 C 0.5206(5) 0.8463(10) 0.1169(5) 0.0347(17) Uani 1 1 d . U . . .
H4A H 0.469682 0.900695 0.090214 0.042 Uiso 1 1 calc R U . . .
H4B H 0.531308 0.880894 0.173726 0.042 Uiso 1 1 calc R U . . .
C5 C 0.6132(5) 1.0428(9) 0.0838(5) 0.0336(17) Uani 1 1 d . U . . .
H5B H 0.630508 1.069901 0.141102 0.040 Uiso 1 1 calc R U . . .
H5A H 0.563213 1.106427 0.063100 0.040 Uiso 1 1 calc R U . . .
C6 C 0.6838(5) 1.0760(9) 0.0366(5) 0.0335(17) Uani 1 1 d . U . . .
H6B H 0.668274 1.040935 -0.019692 0.040 Uiso 1 1 calc R U . . .
H6A H 0.694472 1.189079 0.036070 0.040 Uiso 1 1 calc R U . . .
C7 C 0.8218(5) 0.9937(9) 0.0185(5) 0.0321(17) Uani 1 1 d . U . . .
H7A H 0.832990 1.100380 0.000805 0.039 Uiso 1 1 calc R U . . .
H7B H 0.800944 0.931568 -0.029867 0.039 Uiso 1 1 calc R U . . .
C8 C 0.9005(5) 0.9251(9) 0.0601(5) 0.0330(17) Uani 1 1 d . U . . .
H8B H 0.946161 0.935563 0.025951 0.040 Uiso 1 1 calc R U . . .
H8A H 0.918170 0.981130 0.111216 0.040 Uiso 1 1 calc R U . . .
C9 C 0.9624(5) 0.6888(9) 0.1146(5) 0.0360(17) Uani 1 1 d D U . . .
H9B H 0.978510 0.729824 0.169762 0.043 Uiso 1 1 calc R U . . .
H9A H 1.010031 0.706676 0.083582 0.043 Uiso 1 1 calc R U . . .
C10 C 0.9440(5) 0.5208(9) 0.1179(5) 0.0381(18) Uani 1 1 d D U . . .
H10A H 0.926732 0.480776 0.062724 0.046 Uiso 1 1 calc R U . . .
H10B H 0.995598 0.464493 0.141590 0.046 Uiso 1 1 calc R U . . .
C11 C 0.8554(5) 0.3356(9) 0.1653(5) 0.0333(17) Uani 1 1 d . U . . .
H11A H 0.904885 0.272382 0.187627 0.040 Uiso 1 1 calc R U . . .
H11B H 0.836260 0.300553 0.109462 0.040 Uiso 1 1 calc R U . . .
C12 C 0.7850(5) 0.3159(9) 0.2159(5) 0.0365(18) Uani 1 1 d . U . . .
H12A H 0.774961 0.204315 0.224568 0.044 Uiso 1 1 calc R U . . .
H12B H 0.800913 0.365483 0.269123 0.044 Uiso 1 1 calc R U . . .
N1 N 0.7221(4) 0.6501(7) 0.0661(4) 0.0239(14) Uani 1 1 d . . . . .
H1C H 0.731287 0.631311 0.018414 0.029 Uiso 1 1 d R U . . .
H1D H 0.766887 0.634811 0.096734 0.029 Uiso 1 1 d R U . . .
H1E H 0.682507 0.593484 0.078244 0.029 Uiso 1 1 d R U . . .
H1F H 0.707947 0.744681 0.069154 0.029 Uiso 1 1 d 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
Pb1 I3 3.0612(5) . ?
Pb1 I1 3.0687(5) . ?
Pb1 I2 3.2310(5) 2_545 ?
Pb1 I2 3.2770(6) . ?
O1 C1 1.426(9) . ?
O1 C12 1.436(10) . ?
O2 C3 1.418(10) . ?
O2 C2 1.424(10) . ?
O3 C5 1.418(9) . ?
O3 C4 1.428(9) . ?
O4 C6 1.434(9) . ?
O4 C7 1.442(9) . ?
O5 C8 1.417(9) . ?
O5 C9 1.437(9) . ?
O6 C10 1.417(9) . ?
O6 C11 1.425(9) . ?
C1 C2 1.474(12) . ?
C1 H1B 0.9900 . ?
C1 H1A 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.477(12) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.491(12) . ?
C5 H5B 0.9900 . ?
C5 H5A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 H6A 0.9900 . ?
C7 C8 1.473(11) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8B 0.9900 . ?
C8 H8A 0.9900 . ?
C9 C10 1.481(10) . ?
C9 H9B 0.9900 . ?
C9 H9A 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.506(12) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N1 H1C 0.8468 . ?
N1 H1D 0.8308 . ?
N1 H1E 0.8455 . ?
N1 H1F 0.8500 . ?

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
I3 Pb1 I1 92.066(16) . . ?
I3 Pb1 I2 85.710(14) . 2_545 ?
I1 Pb1 I2 94.951(15) . 2_545 ?
I3 Pb1 I2 94.675(14) . . ?
I1 Pb1 I2 84.453(15) . . ?
I2 Pb1 I2 179.300(15) 2_545 . ?
Pb1 I2 Pb1 83.019(11) 2 . ?
C1 O1 C12 111.7(6) . . ?
C3 O2 C2 114.1(6) . . ?
C5 O3 C4 112.2(6) . . ?
C6 O4 C7 111.1(6) . . ?
C8 O5 C9 113.8(6) . . ?
C10 O6 C11 111.0(6) . . ?
O1 C1 C2 108.1(7) . . ?
O1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
O1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
H1B C1 H1A 108.4 . . ?
O2 C2 C1 109.5(6) . . ?
O2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
O2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
O2 C3 C4 108.3(7) . . ?
O2 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
O2 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
O3 C4 C3 109.3(6) . . ?
O3 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
O3 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
O3 C5 C6 109.7(6) . . ?
O3 C5 H5B 109.7 . . ?
C6 C5 H5B 109.7 . . ?
O3 C5 H5A 109.7 . . ?
C6 C5 H5A 109.7 . . ?
H5B C5 H5A 108.2 . . ?
O4 C6 C5 109.5(6) . . ?
O4 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
O4 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
H6B C6 H6A 108.2 . . ?
O4 C7 C8 109.5(6) . . ?
O4 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
O4 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
O5 C8 C7 110.1(6) . . ?
O5 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
O5 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
H8B C8 H8A 108.2 . . ?
O5 C9 C10 108.4(6) . . ?
O5 C9 H9B 110.0 . . ?
C10 C9 H9B 110.0 . . ?
O5 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
H9B C9 H9A 108.4 . . ?
O6 C10 C9 109.8(6) . . ?
O6 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
O6 C10 H10B 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
O6 C11 C12 108.6(6) . . ?
O6 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
O6 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.3 . . ?
O1 C12 C11 108.8(6) . . ?
O1 C12 H12A 109.9 . . ?
C11 C12 H12A 109.9 . . ?
O1 C12 H12B 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
H1C N1 H1D 107.9 . . ?
H1C N1 H1E 110.4 . . ?
H1D N1 H1E 111.4 . . ?
H1C N1 H1F 108.9 . . ?
H1D N1 H1F 109.1 . . ?
H1E N1 H1F 109.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2B I3 0.99 3.18 3.890(8) 129.6 . yes
C3 H3A I2 0.99 3.26 4.029(8) 135.9 . yes
C4 H4A I3 0.99 3.26 3.910(8) 125.0 1_565 yes
C6 H6B I3 0.99 3.15 4.098(8) 161.6 3_665 yes
C7 H7A I1 0.99 3.18 4.085(8) 152.0 3_675 yes
C7 H7B I2 0.99 3.24 3.930(7) 127.9 4_675 yes
C10 H10B I2 0.99 3.32 4.218(8) 151.6 2_645 yes
N1 H1C I1 0.85 2.97 3.715(6) 148.7 3_665 yes
N1 H1D O5 0.83 2.30 2.808(8) 119.7 . yes
N1 H1D O6 0.83 2.32 3.100(8) 157.6 . yes
N1 H1E O1 0.85 2.41 2.938(8) 121.3 . yes
N1 H1E O2 0.85 2.30 2.992(8) 138.6 . yes
N1 H1F O3 0.85 2.22 2.917(8) 138.6 . yes
N1 H1F O4 0.85 2.32 3.048(8) 143.8 . yes

_refine_diff_density_max         1.152
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.188



####################################################################### 
# 
# 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_1_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 2111960'
loop_
_audit_author_name
_audit_author_address
'guo-jun yuan'
;nanjing xiaozhuang university
China
;
_audit_update_record             
;
2022-03-10 deposited with the CCDC.	2022-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H28 I3 N O6 Pb'
_chemical_formula_weight         870.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   15.9485(6)
_cell_length_b                   8.6219(3)
_cell_length_c                   16.6746(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.1810(10)
_cell_angle_gamma                90
_cell_volume                     2269.53(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    15690
_cell_measurement_theta_min      2.692
_cell_measurement_theta_max      25.01

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.547
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    11.537
_shelx_estimated_absorpt_T_min   0.196
_shelx_estimated_absorpt_T_max   0.218
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15690
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.692
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_full        25.010
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             3958
_reflns_number_gt                3635
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0265P)²+9.7190P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00349(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3958
_refine_ls_number_parameters     209
_refine_ls_number_restraints     217
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0707
_refine_ls_wR_factor_gt          0.0686
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.24955(2) 0.38524(3) 0.25064(2) 0.01493(10) Uani 1 1 d . . . . .
I1 I 0.21854(3) 0.59328(5) 0.10014(2) 0.02267(13) Uani 1 1 d . . . . .
I2 I 0.39650(3) 0.64007(5) 0.31524(3) 0.01929(12) Uani 1 1 d . . . . .
I3 I 0.36887(3) 0.17574(5) 0.17137(3) 0.02145(13) Uani 1 1 d . . . . .
O1 O 0.7094(3) 0.3883(5) 0.1751(3) 0.0203(10) Uani 1 1 d . U . . .
O2 O 0.5772(3) 0.6065(5) 0.1598(3) 0.0219(10) Uani 1 1 d . U . . .
O3 O 0.5922(3) 0.8865(5) 0.0769(3) 0.0220(10) Uani 1 1 d . U . . .
O4 O 0.7594(3) 0.9995(5) 0.0726(2) 0.0198(9) Uani 1 1 d . U . . .
O5 O 0.8876(3) 0.7668(5) 0.0771(3) 0.0217(9) Uani 1 1 d . U . . .
O6 O 0.8783(3) 0.4950(5) 0.1664(3) 0.0210(9) Uani 1 1 d . U . . .
C1 C 0.6405(4) 0.3812(7) 0.2219(4) 0.0244(14) Uani 1 1 d . U . . .
H1B H 0.654837 0.441202 0.272583 0.029 Uiso 1 1 calc R U . . .
H1A H 0.630131 0.272235 0.236354 0.029 Uiso 1 1 calc R U . . .
C2 C 0.5639(4) 0.4461(8) 0.1739(4) 0.0257(14) Uani 1 1 d . U . . .
H2A H 0.551743 0.390566 0.121546 0.031 Uiso 1 1 calc R U . . .
H2B H 0.514825 0.432908 0.203470 0.031 Uiso 1 1 calc R U . . .
C3 C 0.5063(4) 0.6798(8) 0.1133(4) 0.0239(14) Uani 1 1 d . U . . .
H3A H 0.453731 0.653754 0.135532 0.029 Uiso 1 1 calc R U . . .
H3B H 0.500286 0.643546 0.056378 0.029 Uiso 1 1 calc R U . . .
C4 C 0.5210(4) 0.8516(8) 0.1169(4) 0.0240(14) Uani 1 1 d . U . . .
H4A H 0.470122 0.906608 0.089961 0.029 Uiso 1 1 calc R U . . .
H4B H 0.532005 0.886192 0.174057 0.029 Uiso 1 1 calc R U . . .
C5 C 0.6137(4) 1.0458(7) 0.0846(4) 0.0241(14) Uani 1 1 d . U . . .
H5B H 0.631384 1.072013 0.142312 0.029 Uiso 1 1 calc R U . . .
H5A H 0.563874 1.110243 0.063903 0.029 Uiso 1 1 calc R U . . .
C6 C 0.6850(4) 1.0779(8) 0.0367(4) 0.0244(14) Uani 1 1 d . U . . .
H6B H 0.669153 1.041997 -0.019858 0.029 Uiso 1 1 calc R U . . .
H6A H 0.695877 1.190882 0.035604 0.029 Uiso 1 1 calc R U . . .
C7 C 0.8224(4) 0.9952(8) 0.0184(4) 0.0235(14) Uani 1 1 d . U . . .
H7A H 0.833813 1.101776 0.000584 0.028 Uiso 1 1 calc R U . . .
H7B H 0.801053 0.933227 -0.030244 0.028 Uiso 1 1 calc R U . . .
C8 C 0.9017(4) 0.9254(7) 0.0603(4) 0.0224(13) Uani 1 1 d . U . . .
H8B H 0.946958 0.934126 0.025636 0.027 Uiso 1 1 calc R U . . .
H8A H 0.920224 0.981647 0.111490 0.027 Uiso 1 1 calc R U . . .
C9 C 0.9625(4) 0.6890(8) 0.1154(4) 0.0250(14) Uani 1 1 d D U . . .
H9B H 0.978971 0.730060 0.170878 0.030 Uiso 1 1 calc R U . . .
H9A H 1.009937 0.707178 0.084159 0.030 Uiso 1 1 calc R U . . .
C10 C 0.9445(4) 0.5203(8) 0.1188(4) 0.0264(14) Uani 1 1 d D U . . .
H10A H 0.927320 0.479931 0.063323 0.032 Uiso 1 1 calc R U . . .
H10B H 0.996172 0.464371 0.142990 0.032 Uiso 1 1 calc R U . . .
C11 C 0.8549(4) 0.3355(7) 0.1665(4) 0.0224(14) Uani 1 1 d . U . . .
H11A H 0.904116 0.272070 0.189856 0.027 Uiso 1 1 calc R U . . .
H11B H 0.836430 0.299961 0.110309 0.027 Uiso 1 1 calc R U . . .
C12 C 0.7839(4) 0.3159(8) 0.2160(4) 0.0241(14) Uani 1 1 d . U . . .
H12A H 0.773078 0.204192 0.223712 0.029 Uiso 1 1 calc R U . . .
H12B H 0.799651 0.363719 0.270025 0.029 Uiso 1 1 calc R U . . .
N1 N 0.7215(3) 0.6501(6) 0.0657(3) 0.0188(12) Uani 1 1 d . . . . .
H1C H 0.730647 0.631315 0.018031 0.023 Uiso 1 1 d R U . . .
H1D H 0.766247 0.634814 0.096351 0.023 Uiso 1 1 d R U . . .
H1E H 0.681867 0.593487 0.077861 0.023 Uiso 1 1 d R U . . .
H1F H 0.707306 0.744685 0.068771 0.023 Uiso 1 1 d 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
Pb1 I3 3.0573(4) . ?
Pb1 I1 3.0670(5) . ?
Pb1 I2 3.2205(5) 2_545 ?
Pb1 I2 3.2805(5) . ?
O1 C12 1.426(8) . ?
O1 C1 1.437(8) . ?
O2 C2 1.424(8) . ?
O2 C3 1.424(8) . ?
O3 C5 1.417(8) . ?
O3 C4 1.428(8) . ?
O4 C6 1.422(8) . ?
O4 C7 1.444(7) . ?
O5 C8 1.420(7) . ?
O5 C9 1.438(8) . ?
O6 C10 1.424(7) . ?
O6 C11 1.425(7) . ?
C1 C2 1.471(10) . ?
C1 H1B 0.9900 . ?
C1 H1A 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.500(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.506(9) . ?
C5 H5B 0.9900 . ?
C5 H5A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 H6A 0.9900 . ?
C7 C8 1.483(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8B 0.9900 . ?
C8 H8A 0.9900 . ?
C9 C10 1.485(9) . ?
C9 H9B 0.9900 . ?
C9 H9A 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.502(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N1 H1C 0.8437 . ?
N1 H1D 0.8276 . ?
N1 H1E 0.8458 . ?
N1 H1F 0.8497 . ?

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
I3 Pb1 I1 91.695(13) . . ?
I3 Pb1 I2 85.942(12) . 2_545 ?
I1 Pb1 I2 94.598(13) . 2_545 ?
I3 Pb1 I2 94.478(12) . . ?
I1 Pb1 I2 84.344(13) . . ?
I2 Pb1 I2 178.870(12) 2_545 . ?
Pb1 I2 Pb1 83.073(10) 2 . ?
C12 O1 C1 111.8(5) . . ?
C2 O2 C3 113.3(5) . . ?
C5 O3 C4 111.1(5) . . ?
C6 O4 C7 111.2(5) . . ?
C8 O5 C9 113.1(5) . . ?
C10 O6 C11 111.4(5) . . ?
O1 C1 C2 109.2(5) . . ?
O1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
O1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
H1B C1 H1A 108.3 . . ?
O2 C2 C1 109.2(5) . . ?
O2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
O2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
O2 C3 C4 108.0(5) . . ?
O2 C3 H3A 110.1 . . ?
C4 C3 H3A 110.1 . . ?
O2 C3 H3B 110.1 . . ?
C4 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
O3 C4 C3 108.6(5) . . ?
O3 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
O3 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
O3 C5 C6 108.7(5) . . ?
O3 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
O3 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
H5B C5 H5A 108.3 . . ?
O4 C6 C5 109.7(5) . . ?
O4 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
O4 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
H6B C6 H6A 108.2 . . ?
O4 C7 C8 109.7(5) . . ?
O4 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
O4 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
O5 C8 C7 109.6(5) . . ?
O5 C8 H8B 109.7 . . ?
C7 C8 H8B 109.7 . . ?
O5 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
H8B C8 H8A 108.2 . . ?
O5 C9 C10 108.7(5) . . ?
O5 C9 H9B 110.0 . . ?
C10 C9 H9B 110.0 . . ?
O5 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
H9B C9 H9A 108.3 . . ?
O6 C10 C9 109.5(5) . . ?
O6 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
O6 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
O6 C11 C12 109.1(5) . . ?
O6 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
O6 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
O1 C12 C11 109.2(5) . . ?
O1 C12 H12A 109.8 . . ?
C11 C12 H12A 109.8 . . ?
O1 C12 H12B 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
H1C N1 H1D 107.5 . . ?
H1C N1 H1E 110.5 . . ?
H1D N1 H1E 111.6 . . ?
H1C N1 H1F 109.0 . . ?
H1D N1 H1F 109.2 . . ?
H1E N1 H1F 109.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2B I3 0.99 3.20 3.883(6) 127.1 . yes
C3 H3A I2 0.99 3.26 4.026(7) 135.8 . yes
C4 H4A I3 0.99 3.23 3.891(6) 125.3 1_565 yes
C6 H6B I3 0.99 3.14 4.087(7) 161.4 3_665 yes
C7 H7A I1 0.99 3.17 4.068(6) 152.0 3_675 yes
C7 H7B I2 0.99 3.24 3.920(6) 127.7 4_675 yes
C8 H8A I2 0.99 3.30 4.024(7) 131.5 2_655 yes
C10 H10B I2 0.99 3.30 4.195(6) 151.1 2_645 yes
N1 H1C I1 0.84 2.96 3.704(5) 148.6 3_665 yes
N1 H1D O5 0.83 2.31 2.815(7) 120.2 . yes
N1 H1D O6 0.83 2.33 3.110(7) 157.8 . yes
N1 H1E O1 0.85 2.40 2.926(7) 121.1 . yes
N1 H1E O2 0.85 2.31 2.989(7) 138.0 . yes
N1 H1F O3 0.85 2.23 2.924(7) 139.4 . yes
N1 H1F O4 0.85 2.35 3.072(6) 143.5 . yes

_refine_diff_density_max         1.141
_refine_diff_density_min         -2.265
_refine_diff_density_rms         0.192



####################################################################### 
# 
# 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_1_CCDC7
_database_code_depnum_ccdc_archive 'CCDC 2111959'
loop_
_audit_author_name
_audit_author_address
'guo-jun yuan'
;nanjing xiaozhuang university
China
;
_audit_update_record             
;
2022-03-10 deposited with the CCDC.	2022-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H28 I3 N O6 Pb'
_chemical_formula_weight         870.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   15.9602(7)
_cell_length_b                   8.6135(3)
_cell_length_c                   16.5827(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.3610(10)
_cell_angle_gamma                90
_cell_volume                     2255.45(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15502
_cell_measurement_theta_min      2.580
_cell_measurement_theta_max      24.999

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.563
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    11.609
_shelx_estimated_absorpt_T_min   0.194
_shelx_estimated_absorpt_T_max   0.216
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15502
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.580
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             3913
_reflns_number_gt                3674
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0213P)²+24.9709P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00335(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3913
_refine_ls_number_parameters     209
_refine_ls_number_restraints     217
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0765
_refine_ls_wR_factor_gt          0.0749
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.24943(2) 0.38491(3) 0.25108(2) 0.01133(11) Uani 1 1 d . . . . .
I1 I 0.21727(3) 0.59230(6) 0.09972(3) 0.01630(14) Uani 1 1 d . . . . .
I2 I 0.39669(3) 0.64101(5) 0.31522(3) 0.01411(14) Uani 1 1 d . . . . .
I3 I 0.36842(3) 0.17724(6) 0.17062(3) 0.01555(14) Uani 1 1 d . . . . .
O1 O 0.7086(3) 0.3885(6) 0.1748(3) 0.0154(11) Uani 1 1 d . U . . .
O2 O 0.5769(3) 0.6084(6) 0.1604(3) 0.0159(11) Uani 1 1 d . U . . .
O3 O 0.5922(3) 0.8886(6) 0.0766(3) 0.0163(11) Uani 1 1 d . U . . .
O4 O 0.7603(3) 1.0018(6) 0.0727(3) 0.0144(11) Uani 1 1 d . U . . .
O5 O 0.8876(3) 0.7670(6) 0.0774(3) 0.0162(11) Uani 1 1 d . U . . .
O6 O 0.8785(3) 0.4959(6) 0.1674(3) 0.0164(11) Uani 1 1 d . U . . .
C1 C 0.6404(5) 0.3821(9) 0.2224(5) 0.0186(16) Uani 1 1 d . U . . .
H1B H 0.655406 0.442471 0.273255 0.022 Uiso 1 1 calc R U . . .
H1A H 0.630218 0.273118 0.237335 0.022 Uiso 1 1 calc R U . . .
C2 C 0.5623(5) 0.4478(9) 0.1739(5) 0.0198(16) Uani 1 1 d . U . . .
H2A H 0.549522 0.392710 0.121113 0.024 Uiso 1 1 calc R U . . .
H2B H 0.513497 0.435189 0.203922 0.024 Uiso 1 1 calc R U . . .
C3 C 0.5064(5) 0.6833(9) 0.1129(5) 0.0184(15) Uani 1 1 d . U . . .
H3A H 0.453476 0.657123 0.134540 0.022 Uiso 1 1 calc R U . . .
H3B H 0.500820 0.647764 0.055606 0.022 Uiso 1 1 calc R U . . .
C4 C 0.5210(5) 0.8548(9) 0.1172(5) 0.0189(16) Uani 1 1 d . U . . .
H4A H 0.470153 0.910283 0.090316 0.023 Uiso 1 1 calc R U . . .
H4B H 0.532463 0.888775 0.174789 0.023 Uiso 1 1 calc R U . . .
C5 C 0.6152(5) 1.0481(9) 0.0841(5) 0.0177(15) Uani 1 1 d . U . . .
H5B H 0.633718 1.073641 0.142184 0.021 Uiso 1 1 calc R U . . .
H5A H 0.565531 1.113479 0.064039 0.021 Uiso 1 1 calc R U . . .
C6 C 0.6853(5) 1.0814(9) 0.0360(5) 0.0179(15) Uani 1 1 d . U . . .
H6B H 0.669246 1.045826 -0.020916 0.021 Uiso 1 1 calc R U . . .
H6A H 0.696008 1.194558 0.035267 0.021 Uiso 1 1 calc R U . . .
C7 C 0.8218(5) 0.9972(9) 0.0181(4) 0.0165(15) Uani 1 1 d . U . . .
H7A H 0.833202 1.103771 0.000066 0.020 Uiso 1 1 calc R U . . .
H7B H 0.799878 0.935153 -0.030714 0.020 Uiso 1 1 calc R U . . .
C8 C 0.9022(5) 0.9259(9) 0.0605(5) 0.0172(15) Uani 1 1 d . U . . .
H8B H 0.947203 0.934268 0.025501 0.021 Uiso 1 1 calc R U . . .
H8A H 0.921191 0.982047 0.112031 0.021 Uiso 1 1 calc R U . . .
C9 C 0.9625(5) 0.6883(9) 0.1153(5) 0.0185(15) Uani 1 1 d D U . . .
H9B H 0.979768 0.729876 0.170927 0.022 Uiso 1 1 calc R U . . .
H9A H 1.009378 0.705850 0.083359 0.022 Uiso 1 1 calc R U . . .
C10 C 0.9447(5) 0.5196(9) 0.1196(5) 0.0192(16) Uani 1 1 d D U . . .
H10A H 0.927605 0.477936 0.063986 0.023 Uiso 1 1 calc R U . . .
H10B H 0.996388 0.464099 0.144477 0.023 Uiso 1 1 calc R U . . .
C11 C 0.8545(5) 0.3357(9) 0.1666(5) 0.0161(15) Uani 1 1 d . U . . .
H11A H 0.903586 0.271404 0.189659 0.019 Uiso 1 1 calc R U . . .
H11B H 0.835575 0.301373 0.109939 0.019 Uiso 1 1 calc R U . . .
C12 C 0.7838(5) 0.3157(9) 0.2165(5) 0.0174(15) Uani 1 1 d . U . . .
H12A H 0.773187 0.203884 0.224327 0.021 Uiso 1 1 calc R U . . .
H12B H 0.799662 0.363799 0.270821 0.021 Uiso 1 1 calc R U . . .
N1 N 0.7213(4) 0.6520(7) 0.0664(4) 0.0153(13) Uani 1 1 d . . . . .
H1C H 0.730467 0.633236 0.018801 0.018 Uiso 1 1 d R U . . .
H1D H 0.766067 0.636735 0.097121 0.018 Uiso 1 1 d R U . . .
H1E H 0.681687 0.595407 0.078631 0.018 Uiso 1 1 d R U . . .
H1F H 0.707126 0.746604 0.069541 0.018 Uiso 1 1 d 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
Pb1 I3 3.0534(5) . ?
Pb1 I1 3.0627(5) . ?
Pb1 I2 3.2118(5) 2_545 ?
Pb1 I2 3.2855(5) . ?
O1 C1 1.436(9) . ?
O1 C12 1.439(9) . ?
O2 C2 1.426(9) . ?
O2 C3 1.430(9) . ?
O3 C5 1.423(9) . ?
O3 C4 1.433(10) . ?
O4 C7 1.431(9) . ?
O4 C6 1.436(9) . ?
O5 C8 1.423(9) . ?
O5 C9 1.437(9) . ?
O6 C10 1.425(9) . ?
O6 C11 1.432(9) . ?
C1 C2 1.493(11) . ?
C1 H1B 0.9900 . ?
C1 H1A 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.495(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.493(11) . ?
C5 H5B 0.9900 . ?
C5 H5A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 H6A 0.9900 . ?
C7 C8 1.502(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8B 0.9900 . ?
C8 H8A 0.9900 . ?
C9 C10 1.484(10) . ?
C9 H9B 0.9900 . ?
C9 H9A 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.502(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N1 H1C 0.8399 . ?
N1 H1D 0.8253 . ?
N1 H1E 0.8459 . ?
N1 H1F 0.8489 . ?

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
I3 Pb1 I1 91.394(15) . . ?
I3 Pb1 I2 86.219(14) . 2_545 ?
I1 Pb1 I2 94.253(14) . 2_545 ?
I3 Pb1 I2 94.225(14) . . ?
I1 Pb1 I2 84.286(14) . . ?
I2 Pb1 I2 178.480(14) 2_545 . ?
Pb1 I2 Pb1 83.033(11) 2 . ?
C1 O1 C12 111.4(5) . . ?
C2 O2 C3 113.0(6) . . ?
C5 O3 C4 111.6(6) . . ?
C7 O4 C6 110.5(5) . . ?
C8 O5 C9 113.0(5) . . ?
C10 O6 C11 110.7(5) . . ?
O1 C1 C2 109.2(6) . . ?
O1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
O1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
H1B C1 H1A 108.3 . . ?
O2 C2 C1 108.0(6) . . ?
O2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
O2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
O2 C3 C4 108.3(6) . . ?
O2 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
O2 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
O3 C4 C3 107.9(6) . . ?
O3 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 . . ?
O3 C4 H4B 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
O3 C5 C6 110.0(6) . . ?
O3 C5 H5B 109.7 . . ?
C6 C5 H5B 109.7 . . ?
O3 C5 H5A 109.7 . . ?
C6 C5 H5A 109.7 . . ?
H5B C5 H5A 108.2 . . ?
O4 C6 C5 108.9(6) . . ?
O4 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
O4 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
H6B C6 H6A 108.3 . . ?
O4 C7 C8 109.4(6) . . ?
O4 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
O4 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
O5 C8 C7 109.4(6) . . ?
O5 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
O5 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
H8B C8 H8A 108.2 . . ?
O5 C9 C10 109.3(6) . . ?
O5 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
O5 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
H9B C9 H9A 108.3 . . ?
O6 C10 C9 109.2(6) . . ?
O6 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
O6 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
O6 C11 C12 109.1(6) . . ?
O6 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
O6 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
O1 C12 C11 109.0(6) . . ?
O1 C12 H12A 109.9 . . ?
C11 C12 H12A 109.9 . . ?
O1 C12 H12B 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
H1C N1 H1D 107.2 . . ?
H1C N1 H1E 110.6 . . ?
H1D N1 H1E 111.8 . . ?
H1C N1 H1F 109.0 . . ?
H1D N1 H1F 109.3 . . ?
H1E N1 H1F 108.9 . . ?

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
N1 H1F O4 0.85 2.35 3.075(8) 143.0 . yes
N1 H1F O3 0.85 2.22 2.920(8) 139.5 . yes
N1 H1E O2 0.85 2.30 2.987(8) 138.1 . yes
N1 H1E O1 0.85 2.39 2.920(8) 121.4 . yes
N1 H1D O6 0.83 2.33 3.111(8) 157.7 . yes
N1 H1D O5 0.83 2.30 2.814(8) 120.4 . yes
N1 H1C I1 0.84 2.97 3.711(6) 148.6 3_665 yes
C10 H10B I2 0.99 3.28 4.173(7) 150.6 2_645 yes
C8 H8A I2 0.99 3.28 4.007(7) 131.7 2_655 yes
C7 H7B I2 0.99 3.24 3.915(7) 126.9 4_675 yes
C7 H7A I1 0.99 3.14 4.043(8) 152.6 3_675 yes
C6 H6B I3 0.99 3.13 4.072(8) 160.1 3_665 yes
C4 H4A I3 0.99 3.21 3.880(8) 126.1 1_565 yes
C3 H3A I2 0.99 3.26 4.020(8) 135.1 . yes
C2 H2B I3 0.99 3.20 3.868(8) 126.3 . yes

_refine_diff_density_max         1.066
_refine_diff_density_min         -2.519
_refine_diff_density_rms         0.215



