# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_x1
_database_code_depnum_ccdc_archive 'CCDC 1815922'
loop_
_audit_author_name
_audit_author_address
'Yangyang Dang' 'Tianjin University'
_audit_update_record             
;
2018-01-10 deposited with the CCDC.	2020-08-20 downloaded from the CCDC.
;
_audit_creation_date             2018-01-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        'C16 H24 I4 N2 Pb'
_chemical_formula_moiety         'I4 Pb, C16 N2'
_chemical_formula_sum            'C16 H24 I4 N2 Pb'
_chemical_formula_weight         959.16
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   32.824(6)
_cell_length_b                   6.1669(11)
_cell_length_c                   6.2114(11)
_cell_angle_alpha                90
_cell_angle_beta                 93.205(2)
_cell_angle_gamma                90
_cell_volume                     1255.4(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4187
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.49
_shelx_estimated_absorpt_T_max   0.389
_shelx_estimated_absorpt_T_min   0.184
_exptl_absorpt_coefficient_mu    11.639
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4336
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1370 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.5815.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.537
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7306
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_min         1.243
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1503
_reflns_number_total             1565
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.020
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.431
_refine_ls_extinction_coef       0.0142(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1565
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0328
_refine_ls_restrained_S_all      1.204
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0641P)²+2.8952P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1051
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: I2(0.25) I3(0.25) C3(0.5) C4(0.5) C5(0.5) C6(0.5) C7(0.5) C8(0.5)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.5000 0.5000 0.5000 0.0297(2) Uani 1 4 d S T P . .
I1 I 0.40202(2) 0.5000 0.45641(12) 0.0551(3) Uani 1 2 d S T P . .
I2 I 0.5000 0.3826(2) 0.0000 0.0418(3) Uani 0.5 2 d S T P . .
I3 I 0.49914(4) 0.0000 0.3804(2) 0.0424(3) Uani 0.5 2 d S T P . .
N1 N 0.4184(6) 0.0000 0.118(5) 0.159(10) Uani 1 2 d S T P . .
C1 C 0.3187(4) 0.0000 0.211(2) 0.080(4) Uani 1 2 d S T P . .
C2 C 0.4026(6) 0.0000 -0.077(3) 0.140(12) Uani 1 2 d S T P . .
C3 C 0.3302(4) 0.060(2) 0.014(2) 0.052(4) Uani 0.5 1 d . . . . .
C4 C 0.3579(5) 0.076(3) -0.114(3) 0.077(6) Uani 0.5 1 d . . . . .
C5 C 0.3159(7) 0.266(3) -0.068(4) 0.082(6) Uani 0.5 1 d . . . . .
C6 C 0.2936(7) 0.118(6) 0.327(4) 0.104(10) Uani 0.5 1 d . . . . .
C7 C 0.2909(8) 0.392(4) 0.051(6) 0.119(12) Uani 0.5 1 d . . . . .
C8 C 0.2797(7) 0.319(8) 0.253(7) 0.133(15) Uani 0.5 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.2125(9) . ?
Pb1 I1 3.2123(9) 5_666 ?
Pb1 I2 3.1890(6) 5_666 ?
Pb1 I2 3.1890(6) . ?
Pb1 I2 3.1890(6) 5_665 ?
Pb1 I2 3.1890(6) 1_556 ?
Pb1 I3 3.1714(6) . ?
Pb1 I3 3.1714(6) 5_656 ?
Pb1 I3 3.1714(6) 1_565 ?
Pb1 I3 3.1714(6) 5_666 ?
I2 Pb1 3.1890(6) 1_554 ?
I2 I2 1.449(3) 5_665 ?
I3 Pb1 3.1714(6) 1_545 ?
I3 I3 1.484(2) 5_656 ?
N1 C2 1.29(3) . ?
C1 C3 1.35(2) 6 ?
C1 C3 1.35(2) . ?
C1 C6 1.34(3) . ?
C1 C6 1.34(3) 6 ?
C2 C4 1.55(2) 6 ?
C2 C4 1.55(2) . ?
C3 C3 0.74(3) 6 ?
C3 C4 1.49(2) 6 ?
C3 C4 1.24(2) . ?
C3 C5 1.44(2) . ?
C4 C3 1.49(2) 6 ?
C4 C4 0.94(4) 6 ?
C4 C5 1.84(3) . ?
C5 C7 1.38(4) . ?
C6 C6 1.45(7) 6 ?
C6 C8 1.39(5) . ?
C7 C7 1.33(6) 6_565 ?
C7 C8 1.40(5) . ?

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 I1 180.0 5_666 . ?
I2 Pb1 I1 91.579(13) . 5_666 ?
I2 Pb1 I1 91.579(13) 1_556 . ?
I2 Pb1 I1 88.421(14) . . ?
I2 Pb1 I1 91.579(13) 5_666 . ?
I2 Pb1 I1 88.421(13) 1_556 5_666 ?
I2 Pb1 I1 88.421(14) 5_665 . ?
I2 Pb1 I1 91.579(13) 5_665 5_666 ?
I2 Pb1 I1 88.421(13) 5_666 5_666 ?
I2 Pb1 I2 153.75(5) 1_556 . ?
I2 Pb1 I2 26.25(5) 5_666 1_556 ?
I2 Pb1 I2 180.0 1_556 5_665 ?
I2 Pb1 I2 26.25(5) 5_665 . ?
I2 Pb1 I2 153.75(5) 5_666 5_665 ?
I2 Pb1 I2 180.0 5_666 . ?
I3 Pb1 I1 89.11(2) . . ?
I3 Pb1 I1 90.89(2) . 5_666 ?
I3 Pb1 I1 90.89(2) 5_656 . ?
I3 Pb1 I1 89.11(2) 5_666 5_666 ?
I3 Pb1 I1 90.89(2) 5_666 . ?
I3 Pb1 I1 89.11(2) 5_656 5_666 ?
I3 Pb1 I1 89.11(2) 1_565 . ?
I3 Pb1 I1 90.89(2) 1_565 5_666 ?
I3 Pb1 I2 116.64(3) . 5_666 ?
I3 Pb1 I2 63.36(3) . . ?
I3 Pb1 I2 116.64(3) 5_656 5_665 ?
I3 Pb1 I2 116.64(3) 5_666 . ?
I3 Pb1 I2 90.39(3) 5_666 5_665 ?
I3 Pb1 I2 89.61(3) . 5_665 ?
I3 Pb1 I2 90.39(3) 5_656 . ?
I3 Pb1 I2 90.39(3) 1_565 5_666 ?
I3 Pb1 I2 63.36(3) 5_666 5_666 ?
I3 Pb1 I2 89.61(3) 5_666 1_556 ?
I3 Pb1 I2 63.36(3) 1_565 5_665 ?
I3 Pb1 I2 63.36(3) 5_656 1_556 ?
I3 Pb1 I2 89.61(3) 5_656 5_666 ?
I3 Pb1 I2 116.64(3) 1_565 1_556 ?
I3 Pb1 I2 90.39(3) . 1_556 ?
I3 Pb1 I2 89.61(3) 1_565 . ?
I3 Pb1 I3 152.95(4) 5_666 5_656 ?
I3 Pb1 I3 27.05(4) 5_656 . ?
I3 Pb1 I3 152.95(4) 1_565 . ?
I3 Pb1 I3 27.05(4) 5_666 1_565 ?
I3 Pb1 I3 180.0 5_656 1_565 ?
I3 Pb1 I3 180.0 5_666 . ?
Pb1 I2 Pb1 153.75(5) . 1_554 ?
I2 I2 Pb1 76.87(2) 5_665 . ?
I2 I2 Pb1 76.87(2) 5_665 1_554 ?
Pb1 I3 Pb1 152.95(4) . 1_545 ?
I3 I3 Pb1 76.47(2) 5_656 . ?
I3 I3 Pb1 76.47(2) 5_656 1_545 ?
C3 C1 C3 31.6(13) . 6 ?
C6 C1 C3 148.0(17) 6 . ?
C6 C1 C3 148.0(17) . 6 ?
C6 C1 C3 123.6(16) . . ?
C6 C1 C3 123.6(16) 6 6 ?
C6 C1 C6 66(3) . 6 ?
N1 C2 C4 117.7(16) . . ?
N1 C2 C4 117.7(16) . 6 ?
C4 C2 C4 35.3(15) 6 . ?
C1 C3 C4 122.5(13) . 6 ?
C1 C3 C5 117.2(16) . . ?
C3 C3 C1 74.2(6) 6 . ?
C3 C3 C4 94.7(12) 6 . ?
C3 C3 C4 56.0(9) 6 6 ?
C3 C3 C5 152.2(10) 6 . ?
C4 C3 C1 148.4(15) . . ?
C4 C3 C4 38.7(17) . 6 ?
C4 C3 C5 86.5(17) . . ?
C5 C3 C4 120.2(17) . 6 ?
C2 C4 C5 151.9(16) . . ?
C3 C4 C2 127.1(15) . . ?
C3 C4 C2 110.6(12) 6 . ?
C3 C4 C3 29.4(12) . 6 ?
C3 C4 C5 77.9(12) 6 . ?
C3 C4 C5 51.1(12) . . ?
C4 C4 C2 72.4(8) 6 . ?
C4 C4 C3 56.0(9) 6 6 ?
C4 C4 C3 85.4(12) 6 . ?
C4 C4 C5 129.4(9) 6 . ?
C3 C5 C4 42.4(10) . . ?
C7 C5 C3 120(2) . . ?
C7 C5 C4 157(2) . . ?
C1 C6 C6 57.2(14) . 6 ?
C1 C6 C8 120(2) . . ?
C8 C6 C6 153.2(16) . 6 ?
C5 C7 C8 119(3) . . ?
C7 C7 C5 124.5(17) 6_565 . ?
C7 C7 C8 109(2) 6_565 . ?
C6 C8 C7 119(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C4 C3 -57.9(17) . . . 6 ?
N1 C2 C4 C3 -30(2) . . . . ?
N1 C2 C4 C4 -99.6(8) . . . 6 ?
N1 C2 C4 C5 45(3) . . . . ?
C1 C3 C4 C2 3(4) . . . . ?
C1 C3 C4 C3 67(3) . . . 6 ?
C1 C3 C4 C4 67(3) . . . 6 ?
C1 C3 C4 C5 -141(3) . . . . ?
C1 C3 C5 C4 158(2) . . . . ?
C1 C3 C5 C7 -1(3) . . . . ?
C1 C6 C8 C7 3(4) . . . . ?
C2 C4 C5 C3 -98(3) . . . . ?
C2 C4 C5 C7 -48(7) . . . . ?
C3 C1 C3 C4 -29.6(14) 6 . . 6 ?
C3 C1 C3 C4 -73(3) 6 . . . ?
C3 C1 C3 C5 152.6(13) 6 . . . ?
C3 C1 C6 C6 115(3) 6 . . 6 ?
C3 C1 C6 C6 144.7(19) . . . 6 ?
C3 C1 C6 C8 -4(3) . . . . ?
C3 C1 C6 C8 -34(4) 6 . . . ?
C3 C3 C4 C2 -63.7(19) 6 . . . ?
C3 C3 C4 C4 -0.003(5) 6 . . 6 ?
C3 C3 C4 C5 152.1(10) 6 . . . ?
C3 C3 C5 C4 -93(3) 6 . . . ?
C3 C3 C5 C7 107(2) 6 . . . ?
C3 C4 C5 C3 13.6(7) 6 . . . ?
C3 C4 C5 C7 64(5) 6 . . . ?
C3 C4 C5 C7 50(5) . . . . ?
C3 C5 C7 C7 147.2(14) . . . 6_565 ?
C3 C5 C7 C8 0(3) . . . . ?
C4 C2 C4 C3 70(2) 6 . . . ?
C4 C2 C4 C3 41.7(15) 6 . . 6 ?
C4 C2 C4 C5 145(3) 6 . . . ?
C4 C3 C4 C2 -63.7(19) 6 . . . ?
C4 C3 C4 C3 0.003(5) 6 . . 6 ?
C4 C3 C4 C5 152.1(10) 6 . . . ?
C4 C3 C5 C4 -19.8(11) 6 . . . ?
C4 C3 C5 C7 -159(2) . . . . ?
C4 C3 C5 C7 -179.1(18) 6 . . . ?
C4 C4 C5 C3 37.1(13) 6 . . . ?
C4 C4 C5 C7 87(5) 6 . . . ?
C4 C5 C7 C7 111(5) . . . 6_565 ?
C4 C5 C7 C8 -36(6) . . . . ?
C5 C3 C4 C2 144(2) . . . . ?
C5 C3 C4 C3 -152.1(10) . . . 6 ?
C5 C3 C4 C4 -152.1(10) . . . 6 ?
C5 C7 C8 C6 -1(4) . . . . ?
C6 C1 C3 C3 -149.7(18) . . . 6 ?
C6 C1 C3 C3 -52(3) 6 . . 6 ?
C6 C1 C3 C4 -125(4) 6 . . . ?
C6 C1 C3 C4 -179.3(17) . . . 6 ?
C6 C1 C3 C4 -82(3) 6 . . 6 ?
C6 C1 C3 C4 138(3) . . . . ?
C6 C1 C3 C5 100(3) 6 . . . ?
C6 C1 C3 C5 3(2) . . . . ?
C6 C1 C6 C8 -149(2) 6 . . . ?
C6 C6 C8 C7 -74(5) 6 . . . ?
C7 C7 C8 C6 -153(2) 6_565 . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_x1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1815924'
loop_
_audit_author_name
_audit_author_address
'Yangyang Dang' 'Tianjin University'
_audit_update_record             
;
2018-01-10 deposited with the CCDC.	2020-08-20 downloaded from the CCDC.
;
_audit_creation_date             2018-01-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        C18H36N4I10Pb3
_chemical_formula_moiety         'I10 Pb3, 2(C8), C7 N, C2 N'
_chemical_formula_sum            'C18 H36 I10 N4 Pb3'
_chemical_formula_weight         2199.08
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8201(14)
_cell_length_b                   8.8198(14)
_cell_length_c                   29.038(5)
_cell_angle_alpha                93.198(2)
_cell_angle_beta                 95.495(2)
_cell_angle_gamma                90.123(2)
_cell_volume                     2245.0(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4868
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.82
_shelx_estimated_absorpt_T_max   0.265
_shelx_estimated_absorpt_T_min   0.122
_exptl_absorpt_coefficient_mu    18.112
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3368
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1515 before and 0.0631 after correction.
The Ratio of minimum to maximum transmission is 0.4517.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.253
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            22001
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.411
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5720
_reflns_number_total             7904
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         2.354
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.372
_refine_ls_extinction_coef       0.00106(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         7904
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0607
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          1.623
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0568P)²+37.1913P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1734
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Sof(I5B)=Sof(I8B)=Sof(I10B)=Sof(I2B)=Sof(I6B)=Sof(I9B)=1-FVAR(1)
 Sof(I2A)=Sof(I5A)=Sof(I6A)=Sof(I8A)=Sof(I9A)=Sof(I10A)=FVAR(1)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.07049(6) 0.53967(6) 0.72421(2) 0.0279(2) Uani 1 1 d . . . . .
Pb2 Pb 0.0000 0.5000 0.5000 0.0297(2) Uani 1 2 d S T P . .
Pb3 Pb 0.57265(6) 0.04173(6) 0.72418(2) 0.0275(2) Uani 1 1 d . . . . .
Pb4 Pb 0.5000 0.0000 0.5000 0.0294(2) Uani 1 2 d S T P . .
I1 I 0.46395(16) -0.02130(16) 0.38959(4) 0.0563(4) Uani 1 1 d . . . . .
I2A I 0.20149(19) 0.20125(19) 0.50002(6) 0.0553(5) Uani 0.839(2) 1 d . . . . .
I3 I 0.03344(15) 0.51975(15) 0.61044(4) 0.0532(4) Uani 1 1 d . . . . .
I4 I 0.60647(17) 0.04486(15) 0.83208(4) 0.0547(4) Uani 1 1 d . . . . .
I5A I 0.70061(18) 0.29948(19) 0.49955(6) 0.0552(5) Uani 0.839(2) 1 d . . . . .
I6A I 0.27203(15) 0.83792(15) 0.71998(5) 0.0402(4) Uani 0.839(2) 1 d . . . . .
I7 I 0.12084(15) 0.56006(17) 0.83219(4) 0.0548(4) Uani 1 1 d . . . . .
I8A I 0.36909(16) 0.34005(16) 0.72070(6) 0.0463(4) Uani 0.839(2) 1 d . . . . .
I9A I -0.22949(16) 0.74161(16) 0.72070(6) 0.0466(4) Uani 0.839(2) 1 d . . . . .
I10A I 0.87185(18) 0.23933(18) 0.72164(6) 0.0546(5) Uani 0.839(2) 1 d . . . . .
I5B I 0.8008(12) 0.2013(10) 0.5008(4) 0.068(3) Uani 0.161(2) 1 d . . . . .
I8B I 0.7731(11) 0.3399(11) 0.7198(3) 0.065(3) Uani 0.161(2) 1 d . . . . .
I10B I 0.2735(11) 0.2359(11) 0.7204(4) 0.067(3) Uani 0.161(2) 1 d . . . . .
I2B I 0.2969(15) 0.2965(13) 0.5003(4) 0.083(3) Uani 0.161(2) 1 d . . . . .
I6B I 0.3714(12) 0.7409(12) 0.7210(5) 0.085(4) Uani 0.161(2) 1 d . . . . .
I9B I -0.1279(12) 0.8388(11) 0.7204(4) 0.070(3) Uani 0.161(2) 1 d . . . . .
C2 C 1.007(3) 0.208(3) 0.9229(8) 0.075(7) Uani 1 1 d . . . . .
C1 C 0.510(3) 0.704(3) 0.9260(8) 0.079(8) Uani 1 1 d . . . . .
N2 N 0.534(2) 0.631(2) 0.8123(8) 0.081(7) Uani 1 1 d . . . . .
C4 C 1.163(5) 0.035(6) 0.8842(17) 0.18(2) Uani 1 1 d . . . . .
C5 C 0.157(3) 1.110(4) 0.8178(12) 0.114(13) Uani 1 1 d . . . . .
C3 C 0.602(4) 0.607(5) 0.9097(8) 0.141(17) Uani 1 1 d . . . . .
C6 C 0.455(11) 0.432(6) 0.938(3) 0.41(8) Uani 1 1 d . . . . .
C8 C 0.048(5) 1.001(3) 0.8168(14) 0.136(16) Uani 1 1 d . . . . .
C9 C 0.358(9) 0.632(13) 0.9632(13) 0.48(9) Uani 1 1 d . . . . .
C10 C 0.847(6) 0.083(14) 0.9642(16) 0.37(7) Uani 1 1 d . . . . .
C7 C 0.661(6) 0.538(6) 0.8786(10) 0.21(3) Uani 1 1 d . . . . .
C12 C 1.033(10) 0.966(18) 0.926(3) 0.76(16) Uani 1 1 d . . . . .
C11 C 0.629(4) 0.521(4) 0.8278(13) 0.123(13) Uani 1 1 d . . . . .
C14 C 0.487(4) 0.413(7) 0.3827(17) 0.19(3) Uani 1 1 d . . . . .
C15 C 0.564(8) 0.859(6) 0.9564(18) 0.28(5) Uani 1 1 d . . . . .
C16 C 0.965(7) 0.062(6) 0.611(2) 0.21(3) Uani 1 1 d . . . . .
C17 C 0.712(6) 0.68(2) 1.039(7) 1.1(3) Uani 1 1 d . . . . .
N13 N 0.554(18) 0.428(11) 0.607(4) 0.74(14) Uani 1 1 d . . . . .
C20 C 1.055(9) 0.050(15) 0.609(4) 0.58(13) Uani 1 1 d . . . . .
C21 C 1.155(13) 0.367(6) 0.9631(17) 0.29(5) Uani 1 1 d . . . . .
C22 C 1.090(6) 0.957(6) 0.5959(16) 0.18(2) Uani 1 1 d . . . . .
C23 C 0.82(2) 0.919(6) 0.961(4) 0.67(16) Uani 1 1 d . . . . .
C25 C 0.556(12) 0.512(11) 0.599(2) 0.50(10) Uani 1 1 d . . . . .
C26 C 0.789(5) 0.748(10) 0.937(2) 0.31(5) Uani 1 1 d . . . . .
C27 C 1.199(15) 0.157(8) 0.920(2) 0.55(11) Uani 1 1 d . . . . .
C28 C 0.049(10) 0.690(12) 1.0490(13) 0.37(7) Uani 1 1 d . . . . .
C19 C 0.514(18) 0.063(18) 0.990(6) 1.81(17) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I3 3.2832(14) . ?
Pb1 I6A 3.1863(14) . ?
Pb1 I7 3.1194(15) . ?
Pb1 I8A 3.1777(14) . ?
Pb1 I9A 3.1893(14) . ?
Pb1 I10A 3.1662(15) 1_455 ?
Pb1 I8B 3.145(9) 1_455 ?
Pb1 I10B 3.228(9) . ?
Pb1 I6B 3.202(10) . ?
Pb1 I9B 3.170(10) . ?
Pb2 I2A 3.1814(14) 2_566 ?
Pb2 I2A 3.1814(14) . ?
Pb2 I3 3.1874(13) 2_566 ?
Pb2 I3 3.1873(13) . ?
Pb2 I5A 3.1736(14) 2_666 ?
Pb2 I5A 3.1736(13) 1_455 ?
Pb2 I5B 3.166(8) 1_455 ?
Pb2 I5B 3.166(8) 2_666 ?
Pb2 I2B 3.177(11) . ?
Pb2 I2B 3.177(11) 2_566 ?
Pb3 I1 3.2831(14) 2_656 ?
Pb3 I4 3.1174(15) . ?
Pb3 I6A 3.1890(13) 1_545 ?
Pb3 I8A 3.1893(14) . ?
Pb3 I9A 3.1759(14) 1_645 ?
Pb3 I10A 3.1684(15) . ?
Pb3 I8B 3.181(9) . ?
Pb3 I10B 3.145(9) . ?
Pb3 I6B 3.181(10) 1_545 ?
Pb3 I9B 3.201(10) 1_645 ?
Pb4 I1 3.1864(13) . ?
Pb4 I1 3.1865(13) 2_656 ?
Pb4 I2A 3.1785(14) 2_656 ?
Pb4 I2A 3.1785(14) . ?
Pb4 I5A 3.1774(14) 2_656 ?
Pb4 I5A 3.1774(14) . ?
Pb4 I5B 3.187(8) 2_656 ?
Pb4 I5B 3.187(8) . ?
Pb4 I2B 3.173(10) . ?
Pb4 I2B 3.173(10) 2_656 ?
I1 Pb3 3.2832(14) 2_656 ?
I2A I2B 1.187(14) . ?
I5A Pb2 3.1736(13) 1_655 ?
I5A I5B 1.238(11) . ?
I6A Pb3 3.1890(13) 1_565 ?
I6A I6B 1.226(11) . ?
I8A I10B 1.244(11) . ?
I9A Pb3 3.1759(14) 1_465 ?
I9A I9B 1.239(10) . ?
I10A Pb1 3.1662(14) 1_655 ?
I10A I8B 1.244(11) . ?
I5B Pb2 3.166(8) 1_655 ?
I8B Pb1 3.145(9) 1_655 ?
I6B Pb3 3.181(9) 1_565 ?
I9B Pb3 3.201(10) 1_465 ?
C2 C27 1.76(11) . ?
C2 C28 1.31(6) 2_667 ?
C1 C3 1.28(3) . ?
C1 C9 1.93(11) . ?
C1 C15 1.63(8) . ?
N2 C11 1.35(4) . ?
C4 C12 1.86(16) 1_545 ?
C4 C27 1.47(10) . ?
C5 C8 1.35(5) . ?
C3 C7 1.22(4) . ?
C6 C17 1.97(11) 2_667 ?
C10 C23 1.46(13) 1_545 ?
C7 C11 1.48(4) . ?
C12 C4 1.86(15) 1_565 ?
C14 N13 1.47(13) 2_666 ?
C14 C25 0.92(6) 2_666 ?
C15 C19 1.86(12) 2_667 ?
C16 C20 0.81(9) . ?
C16 C22 1.52(7) 1_545 ?
C17 C6 1.97(12) 2_667 ?
C17 C21 1.25(13) 2_767 ?
C17 C27 1.9(2) 2_767 ?
N13 C14 1.47(13) 2_666 ?
N13 C25 0.79(14) . ?
C20 C22 0.96(9) 1_545 ?
C21 C17 1.25(13) 2_767 ?
C21 C28 1.86(11) 2_667 ?
C22 C16 1.52(7) 1_565 ?
C22 C20 0.96(9) 1_565 ?
C23 C10 1.46(13) 1_565 ?
C23 C26 1.63(11) . ?
C25 C14 0.92(6) 2_666 ?
C27 C17 1.9(2) 2_767 ?
C28 C2 1.31(6) 2_667 ?
C28 C21 1.86(11) 2_667 ?
C19 C15 1.86(12) 2_667 ?
C19 C19 1.3(2) 2_657 ?

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
I6A Pb1 I3 87.77(4) . . ?
I6A Pb1 I9A 89.91(4) . . ?
I6A Pb1 I10B 111.75(19) . . ?
I6A Pb1 I6B 22.1(2) . . ?
I7 Pb1 I3 177.53(4) . . ?
I7 Pb1 I6A 90.65(4) . . ?
I7 Pb1 I8A 89.67(4) . . ?
I7 Pb1 I9A 93.96(4) . . ?
I7 Pb1 I10A 92.85(4) . 1_455 ?
I7 Pb1 I8B 94.53(19) . 1_455 ?
I7 Pb1 I10B 90.54(19) . . ?
I7 Pb1 I6B 89.4(2) . . ?
I7 Pb1 I9B 93.4(2) . . ?
I8A Pb1 I3 88.41(4) . . ?
I8A Pb1 I6A 89.40(4) . . ?
I8A Pb1 I9A 176.31(5) . . ?
I8A Pb1 I10B 22.38(19) . . ?
I8A Pb1 I6B 67.3(2) . . ?
I9A Pb1 I3 87.94(4) . . ?
I9A Pb1 I10B 157.8(2) . . ?
I9A Pb1 I6B 112.0(2) . . ?
I10A Pb1 I3 88.70(4) 1_455 . ?
I10A Pb1 I6A 176.38(5) 1_455 . ?
I10A Pb1 I8A 89.75(5) 1_455 . ?
I10A Pb1 I9A 90.72(5) 1_455 . ?
I10A Pb1 I10B 67.37(19) 1_455 . ?
I10A Pb1 I6B 156.9(2) 1_455 . ?
I10A Pb1 I9B 113.17(19) 1_455 . ?
I8B Pb1 I3 87.65(19) 1_455 . ?
I8B Pb1 I6A 157.6(2) 1_455 . ?
I8B Pb1 I8A 112.4(2) 1_455 . ?
I8B Pb1 I9A 68.0(2) 1_455 . ?
I8B Pb1 I10A 22.7(2) 1_455 1_455 ?
I8B Pb1 I10B 90.1(3) 1_455 . ?
I8B Pb1 I6B 176.0(3) 1_455 . ?
I8B Pb1 I9B 90.4(3) 1_455 . ?
I10B Pb1 I3 88.28(19) . . ?
I6B Pb1 I3 88.4(2) . . ?
I6B Pb1 I10B 89.7(3) . . ?
I9B Pb1 I3 87.8(2) . . ?
I9B Pb1 I6A 67.44(19) . . ?
I9B Pb1 I8A 156.7(2) . . ?
I9B Pb1 I9A 22.47(19) . . ?
I9B Pb1 I10B 176.0(3) . . ?
I9B Pb1 I6B 89.6(3) . . ?
I2A Pb2 I2A 180.0 . 2_566 ?
I2A Pb2 I3 89.96(4) . 2_566 ?
I2A Pb2 I3 89.96(4) 2_566 . ?
I2A Pb2 I3 90.04(4) . . ?
I2A Pb2 I3 90.04(4) 2_566 2_566 ?
I3 Pb2 I3 180.0 . 2_566 ?
I5A Pb2 I2A 90.23(5) 1_455 . ?
I5A Pb2 I2A 89.77(5) 1_455 2_566 ?
I5A Pb2 I2A 89.77(5) 2_666 . ?
I5A Pb2 I2A 90.23(5) 2_666 2_566 ?
I5A Pb2 I3 90.01(4) 1_455 2_566 ?
I5A Pb2 I3 89.99(4) 2_666 2_566 ?
I5A Pb2 I3 89.99(4) 1_455 . ?
I5A Pb2 I3 90.01(4) 2_666 . ?
I5A Pb2 I5A 180.0 2_666 1_455 ?
I5A Pb2 I2B 68.3(3) 2_666 . ?
I5A Pb2 I2B 111.7(3) 1_455 . ?
I5A Pb2 I2B 111.7(3) 2_666 2_566 ?
I5A Pb2 I2B 68.3(3) 1_455 2_566 ?
I5B Pb2 I2A 67.7(2) 2_666 2_566 ?
I5B Pb2 I2A 112.3(2) 2_666 . ?
I5B Pb2 I2A 112.3(2) 1_455 2_566 ?
I5B Pb2 I2A 67.7(2) 1_455 . ?
I5B Pb2 I3 89.4(2) 1_455 . ?
I5B Pb2 I3 90.6(2) 1_455 2_566 ?
I5B Pb2 I3 90.6(2) 2_666 . ?
I5B Pb2 I3 89.4(2) 2_666 2_566 ?
I5B Pb2 I5A 157.5(2) 1_455 2_666 ?
I5B Pb2 I5A 22.5(2) 2_666 2_666 ?
I5B Pb2 I5A 157.5(2) 2_666 1_455 ?
I5B Pb2 I5A 22.5(2) 1_455 1_455 ?
I5B Pb2 I5B 180.0 2_666 1_455 ?
I5B Pb2 I2B 89.2(3) 1_455 . ?
I5B Pb2 I2B 89.2(3) 2_666 2_566 ?
I5B Pb2 I2B 90.8(3) 1_455 2_566 ?
I5B Pb2 I2B 90.8(3) 2_666 . ?
I2B Pb2 I2A 158.5(3) . 2_566 ?
I2B Pb2 I2A 21.5(3) 2_566 2_566 ?
I2B Pb2 I2A 158.5(3) 2_566 . ?
I2B Pb2 I2A 21.5(3) . . ?
I2B Pb2 I3 90.0(2) 2_566 . ?
I2B Pb2 I3 90.0(2) 2_566 2_566 ?
I2B Pb2 I3 90.0(2) . . ?
I2B Pb2 I3 90.0(2) . 2_566 ?
I2B Pb2 I2B 180.0 2_566 . ?
I4 Pb3 I1 177.36(4) . 2_656 ?
I4 Pb3 I6A 90.62(4) . 1_545 ?
I4 Pb3 I8A 94.03(4) . . ?
I4 Pb3 I9A 89.57(4) . 1_645 ?
I4 Pb3 I10A 92.85(4) . . ?
I4 Pb3 I8B 94.53(19) . . ?
I4 Pb3 I10B 93.44(19) . . ?
I4 Pb3 I6B 89.4(3) . 1_545 ?
I4 Pb3 I9B 90.5(2) . 1_645 ?
I6A Pb3 I1 87.78(4) 1_545 2_656 ?
I6A Pb3 I8A 89.93(4) 1_545 . ?
I6A Pb3 I9B 111.81(18) 1_545 1_645 ?
I8A Pb3 I1 88.07(4) . 2_656 ?
I8A Pb3 I9B 157.77(19) . 1_645 ?
I9A Pb3 I1 88.32(4) 1_645 2_656 ?
I9A Pb3 I6A 89.43(4) 1_645 1_545 ?
I9A Pb3 I8A 176.35(4) 1_645 . ?
I9A Pb3 I8B 112.3(2) 1_645 . ?
I9A Pb3 I6B 67.3(2) 1_645 1_545 ?
I9A Pb3 I9B 22.41(18) 1_645 1_645 ?
I10A Pb3 I1 88.72(4) . 2_656 ?
I10A Pb3 I6A 176.43(5) . 1_545 ?
I10A Pb3 I8A 90.68(5) . . ?
I10A Pb3 I9A 89.74(5) . 1_645 ?
I10A Pb3 I8B 22.61(19) . . ?
I10A Pb3 I6B 156.9(2) . 1_545 ?
I10A Pb3 I9B 67.34(18) . 1_645 ?
I8B Pb3 I1 87.73(18) . 2_656 ?
I8B Pb3 I6A 157.7(2) . 1_545 ?
I8B Pb3 I8A 68.1(2) . . ?
I8B Pb3 I6B 176.1(3) . 1_545 ?
I8B Pb3 I9B 89.9(3) . 1_645 ?
I10B Pb3 I1 87.88(19) . 2_656 ?
I10B Pb3 I6A 67.3(2) . 1_545 ?
I10B Pb3 I8A 22.64(19) . . ?
I10B Pb3 I9A 156.5(2) . 1_645 ?
I10B Pb3 I10A 113.3(2) . . ?
I10B Pb3 I8B 90.7(3) . . ?
I10B Pb3 I6B 89.5(3) . 1_545 ?
I10B Pb3 I9B 176.0(3) . 1_645 ?
I6B Pb3 I1 88.4(3) 1_545 2_656 ?
I6B Pb3 I6A 22.2(2) 1_545 1_545 ?
I6B Pb3 I8A 112.1(2) 1_545 . ?
I6B Pb3 I9B 89.7(3) 1_545 1_645 ?
I9B Pb3 I1 88.2(2) 1_645 2_656 ?
I1 Pb4 I1 180.0 . 2_656 ?
I1 Pb4 I5B 90.6(2) 2_656 2_656 ?
I1 Pb4 I5B 89.4(2) . 2_656 ?
I1 Pb4 I5B 89.4(2) 2_656 . ?
I1 Pb4 I5B 90.6(2) . . ?
I2A Pb4 I1 90.06(4) . 2_656 ?
I2A Pb4 I1 89.94(4) . . ?
I2A Pb4 I1 89.93(4) 2_656 2_656 ?
I2A Pb4 I1 90.07(4) 2_656 . ?
I2A Pb4 I2A 180.0 2_656 . ?
I2A Pb4 I5B 112.2(2) 2_656 2_656 ?
I2A Pb4 I5B 67.8(2) 2_656 . ?
I2A Pb4 I5B 112.2(2) . . ?
I2A Pb4 I5B 67.8(2) . 2_656 ?
I5A Pb4 I1 90.01(4) 2_656 . ?
I5A Pb4 I1 89.99(4) 2_656 2_656 ?
I5A Pb4 I1 89.99(4) . . ?
I5A Pb4 I1 90.01(4) . 2_656 ?
I5A Pb4 I2A 89.80(5) . . ?
I5A Pb4 I2A 89.80(5) 2_656 2_656 ?
I5A Pb4 I2A 90.20(5) . 2_656 ?
I5A Pb4 I2A 90.20(5) 2_656 . ?
I5A Pb4 I5A 180.0 2_656 . ?
I5A Pb4 I5B 22.44(19) 2_656 2_656 ?
I5A Pb4 I5B 157.56(19) . 2_656 ?
I5A Pb4 I5B 22.44(19) . . ?
I5A Pb4 I5B 157.56(19) 2_656 . ?
I5B Pb4 I5B 180.0 . 2_656 ?
I2B Pb4 I1 90.2(2) 2_656 2_656 ?
I2B Pb4 I1 90.2(2) . . ?
I2B Pb4 I1 89.8(2) 2_656 . ?
I2B Pb4 I1 89.8(2) . 2_656 ?
I2B Pb4 I2A 21.5(3) . . ?
I2B Pb4 I2A 158.5(3) 2_656 . ?
I2B Pb4 I2A 21.5(3) 2_656 2_656 ?
I2B Pb4 I2A 158.5(3) . 2_656 ?
I2B Pb4 I5A 68.3(3) 2_656 2_656 ?
I2B Pb4 I5A 111.7(3) 2_656 . ?
I2B Pb4 I5A 68.3(3) . . ?
I2B Pb4 I5A 111.7(3) . 2_656 ?
I2B Pb4 I5B 90.7(3) . . ?
I2B Pb4 I5B 89.3(3) 2_656 . ?
I2B Pb4 I5B 89.3(3) . 2_656 ?
I2B Pb4 I5B 90.7(3) 2_656 2_656 ?
I2B Pb4 I2B 180.0 . 2_656 ?
Pb4 I1 Pb3 179.75(5) . 2_656 ?
Pb4 I2A Pb2 158.03(7) . . ?
I2B I2A Pb2 79.0(5) . . ?
I2B I2A Pb4 79.0(5) . . ?
Pb2 I3 Pb1 179.59(5) . . ?
Pb2 I5A Pb4 157.59(7) 1_655 . ?
I5B I5A Pb2 78.4(4) . 1_655 ?
I5B I5A Pb4 79.2(4) . . ?
Pb1 I6A Pb3 157.83(5) . 1_565 ?
I6B I6A Pb1 79.7(4) . . ?
I6B I6A Pb3 78.5(4) . 1_565 ?
Pb1 I8A Pb3 157.44(6) . . ?
I10B I8A Pb1 81.1(4) . . ?
I10B I8A Pb3 76.7(4) . . ?
Pb3 I9A Pb1 157.49(6) 1_465 . ?
I9B I9A Pb1 77.9(5) . . ?
I9B I9A Pb3 79.9(5) . 1_465 ?
Pb1 I10A Pb3 156.65(7) 1_655 . ?
I8B I10A Pb1 77.7(4) . 1_655 ?
I8B I10A Pb3 79.3(4) . . ?
Pb2 I5B Pb4 157.4(4) 1_655 . ?
I5A I5B Pb2 79.1(4) . 1_655 ?
I5A I5B Pb4 78.3(4) . . ?
Pb1 I8B Pb3 157.4(4) 1_655 . ?
I10A I8B Pb1 79.6(4) . 1_655 ?
I10A I8B Pb3 78.1(4) . . ?
Pb3 I10B Pb1 156.9(4) . . ?
I8A I10B Pb1 76.5(4) . . ?
I8A I10B Pb3 80.7(5) . . ?
Pb4 I2B Pb2 158.9(5) . . ?
I2A I2B Pb2 79.4(6) . . ?
I2A I2B Pb4 79.5(5) . . ?
Pb3 I6B Pb1 157.2(4) 1_565 . ?
I6A I6B Pb1 78.2(5) . . ?
I6A I6B Pb3 79.3(5) . 1_565 ?
Pb1 I9B Pb3 157.0(4) . 1_465 ?
I9A I9B Pb1 79.6(5) . . ?
I9A I9B Pb3 77.7(5) . 1_465 ?
C28 C2 C27 128(6) 2_667 . ?
C3 C1 C9 118(4) . . ?
C3 C1 C15 124(3) . . ?
C15 C1 C9 100(3) . . ?
C27 C4 C12 84(6) . 1_545 ?
C7 C3 C1 154(3) . . ?
C3 C7 C11 135(3) . . ?
N2 C11 C7 111(2) . . ?
C25 C14 N13 29(8) 2_666 2_666 ?
C1 C15 C19 127(8) . 2_667 ?
C20 C16 C22 33(9) . 1_545 ?
C21 C17 C6 125(8) 2_767 2_667 ?
C21 C17 C27 86(10) 2_767 2_767 ?
C27 C17 C6 116(10) 2_767 2_667 ?
C25 N13 C14 34(8) . 2_666 ?
C16 C20 C22 119(10) . 1_545 ?
C17 C21 C28 143(10) 2_767 2_667 ?
C20 C22 C16 28(8) 1_565 1_565 ?
C10 C23 C26 159(10) 1_565 . ?
N13 C25 C14 117(10) . 2_666 ?
C2 C27 C17 97(3) . 2_767 ?
C4 C27 C2 94(8) . . ?
C4 C27 C17 167(9) . 2_767 ?
C2 C28 C21 82(4) 2_667 2_667 ?
C19 C19 C15 80(9) 2_657 2_667 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 I6A I6B Pb3 -176.1(3) . . . 1_565 ?
Pb1 I8A I10B Pb3 -176.15(19) . . . . ?
Pb1 I9A I9B Pb3 -176.1(2) . . . 1_465 ?
Pb1 I10A I8B Pb3 -176.30(19) 1_655 . . . ?
Pb2 I2A I2B Pb4 -179.8(2) . . . . ?
Pb2 I5A I5B Pb4 -179.8(2) 1_655 . . . ?
Pb3 I6A I6B Pb1 176.1(3) 1_565 . . . ?
Pb3 I8A I10B Pb1 176.15(19) . . . . ?
Pb3 I9A I9B Pb1 176.1(2) 1_465 . . . ?
Pb3 I10A I8B Pb1 176.30(19) . . . 1_655 ?
Pb4 I2A I2B Pb2 179.8(2) . . . . ?
Pb4 I5A I5B Pb2 179.8(2) . . . 1_655 ?
C1 C3 C7 C11 -10(19) . . . . ?
C3 C1 C15 C19 -137(5) . . . 2_667 ?
C3 C7 C11 N2 16(10) . . . . ?
C9 C1 C3 C7 119(13) . . . . ?
C9 C1 C15 C19 -2(5) . . . 2_667 ?
C12 C4 C27 C2 -54(3) 1_545 . . . ?
C12 C4 C27 C17 155(21) 1_545 . . 2_767 ?
C15 C1 C3 C7 -114(12) . . . . ?
C28 C2 C27 C4 176(5) 2_667 . . . ?
C28 C2 C27 C17 -10(7) 2_667 . . 2_767 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_x1_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1815925'
loop_
_audit_author_name
_audit_author_address
'Yangyang Dang' 'Tianjin University'
_audit_update_record             
;
2018-01-10 deposited with the CCDC.	2020-08-20 downloaded from the CCDC.
;
_audit_creation_date             2018-01-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        C17H30N3I7Pb2
_chemical_formula_moiety         'I7 Pb2, C4 N, 1.5(C2), N'
_chemical_formula_sum            'C17 H30 I7 N3 Pb2'
_chemical_formula_weight         1579.12
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 N1 Pb1 I1'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8092(5)
_cell_length_b                   8.8168(4)
_cell_length_c                   22.8196(12)
_cell_angle_alpha                97.072(4)
_cell_angle_beta                 93.983(4)
_cell_angle_gamma                90.199(4)
_cell_volume                     1754.52(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7002
_cell_measurement_temperature    296.00(10)
_cell_measurement_theta_max      28.8120
_cell_measurement_theta_min      4.1300
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    15.752
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.989
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23284
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.557
_diffrn_reflns_theta_min         3.266
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1975
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00  35.00   1.00    6.00    --   10.97 -37.00  60.00   98
  2  ω    -61.00  39.00   1.00    6.00    --   10.97 -57.00-180.00  100
  3  ω     34.00  98.00   1.00    6.00    --   10.97-178.00  90.00   64
  4  ω    -13.00  85.00   1.00    6.00    --   10.97  37.00-150.00   98
  5  ω    -20.00  29.00   1.00    6.00    --  -11.59 -99.00-150.00   49
  6  ω    -44.00  35.00   1.00    6.00    --  -11.59  77.00 -30.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0612121000
_diffrn_orient_matrix_UB_12      -0.0462145000
_diffrn_orient_matrix_UB_13      0.0064849000
_diffrn_orient_matrix_UB_21      0.0035839000
_diffrn_orient_matrix_UB_22      -0.0447712000
_diffrn_orient_matrix_UB_23      -0.0278980000
_diffrn_orient_matrix_UB_31      0.0524954000
_diffrn_orient_matrix_UB_32      -0.0493185000
_diffrn_orient_matrix_UB_33      0.0128667000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6355
_reflns_number_total             8472
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.705
_refine_diff_density_min         -1.896
_refine_diff_density_rms         0.315
_refine_ls_extinction_coef       0.00075(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         8472
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0546
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0754P)²+12.8276P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1592
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.22573(4) 0.20475(4) 0.35508(2) 0.02967(13) Uani 1 1 d . . . . .
Pb02 Pb 0.72271(4) 0.70167(4) 0.35505(2) 0.02963(13) Uani 1 1 d . . . . .
I003 I -0.07571(9) 0.00557(9) 0.35971(4) 0.0442(2) Uani 1 1 d . . . . .
I004 I 0.42250(9) 0.90278(9) 0.35857(4) 0.0493(2) Uani 1 1 d . . . . .
I005 I 0.02648(9) 0.50685(9) 0.35861(4) 0.0491(2) Uani 1 1 d . . . . .
I006 I 0.74772(9) 0.74744(10) 0.49998(3) 0.0507(2) Uani 1 1 d . . . . .
I007 I 0.19690(12) 0.14154(10) 0.21608(4) 0.0523(2) Uani 1 1 d . . . . .
I008 I 0.71675(10) 0.66080(12) 0.21603(4) 0.0523(2) Uani 1 1 d . . . . .
I009 I 0.52952(10) 0.39927(10) 0.35739(4) 0.0556(3) Uani 1 1 d . . . . .
N00A N 0.1296(12) 0.7437(12) 0.2465(5) 0.052(3) Uani 1 1 d . . . . .
C1 C 0.2381(18) 0.622(2) 0.2183(8) 0.070(4) Uani 1 1 d . . . . .
C0AA C 0.543(2) 0.259(2) 0.0986(8) 0.089(6) Uani 1 1 d . . . . .
C2 C 0.045(2) 0.755(2) 0.0944(8) 0.087(6) Uani 1 1 d . . . . .
C5 C 0.651(3) 0.152(3) 0.1169(7) 0.108(8) Uani 1 1 d . . . . .
C6 C 0.145(3) 0.653(4) 0.1142(8) 0.131(12) Uani 1 1 d . . . . .
N7 N 0.238(4) 0.757(3) 0.4976(10) 0.26(3) Uani 1 1 d . . . . .
C8 C 0.217(8) 0.622(9) 0.1495(17) 0.38(5) Uani 1 1 d . . . . .
C1AA C 0.703(5) 0.165(5) 0.2326(11) 0.28(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 I003 3.1936(8) . ?
Pb01 I004 3.1881(8) 1_545 ?
Pb01 I005 3.1908(8) . ?
Pb01 I006 3.2741(8) 2_666 ?
Pb01 I007 3.1447(9) . ?
Pb01 I009 3.1674(8) . ?
Pb02 I003 3.1960(8) 1_665 ?
Pb02 I004 3.1893(8) . ?
Pb02 I005 3.1865(8) 1_655 ?
Pb02 I006 3.2740(8) . ?
Pb02 I008 3.1451(9) . ?
Pb02 I009 3.1661(8) . ?
I003 Pb02 3.1960(8) 1_445 ?
I004 Pb01 3.1881(8) 1_565 ?
I005 Pb02 3.1865(8) 1_455 ?
I006 Pb01 3.2741(8) 2_666 ?
N00A C1 1.55(2) . ?
C1 C8 1.57(4) . ?
C0AA C5 1.42(3) . ?
C2 C6 1.36(3) . ?
C6 C8 1.05(5) . ?

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
I003 Pb01 I006 88.29(2) . 2_666 ?
I004 Pb01 I003 89.32(2) 1_545 . ?
I004 Pb01 I005 177.07(3) 1_545 . ?
I004 Pb01 I006 88.76(2) 1_545 2_666 ?
I005 Pb01 I003 89.91(2) . . ?
I005 Pb01 I006 88.40(2) . 2_666 ?
I007 Pb01 I003 89.72(3) . . ?
I007 Pb01 I004 89.19(3) . 1_545 ?
I007 Pb01 I005 93.63(3) . . ?
I007 Pb01 I006 177.16(2) . 2_666 ?
I007 Pb01 I009 93.06(3) . . ?
I009 Pb01 I003 177.01(3) . . ?
I009 Pb01 I004 89.60(3) . 1_545 ?
I009 Pb01 I005 91.03(3) . . ?
I009 Pb01 I006 88.89(3) . 2_666 ?
I003 Pb02 I006 88.28(2) 1_665 . ?
I004 Pb02 I003 89.79(2) . 1_665 ?
I004 Pb02 I006 88.45(2) . . ?
I005 Pb02 I003 89.38(2) 1_655 1_665 ?
I005 Pb02 I004 177.03(3) 1_655 . ?
I005 Pb02 I006 88.67(2) 1_655 . ?
I008 Pb02 I003 89.72(3) . 1_665 ?
I008 Pb02 I004 93.68(3) . . ?
I008 Pb02 I005 89.17(3) . 1_655 ?
I008 Pb02 I006 177.07(2) . . ?
I008 Pb02 I009 93.08(3) . . ?
I009 Pb02 I003 176.98(3) . 1_665 ?
I009 Pb02 I004 91.15(3) . . ?
I009 Pb02 I005 89.53(3) . 1_655 ?
I009 Pb02 I006 88.88(3) . . ?
Pb01 I003 Pb02 156.77(3) . 1_445 ?
Pb01 I004 Pb02 156.43(3) 1_565 . ?
Pb02 I005 Pb01 156.38(3) 1_455 . ?
Pb02 I006 Pb01 179.61(3) . 2_666 ?
Pb02 I009 Pb01 154.98(4) . . ?
N00A C1 C8 107(2) . . ?
C8 C6 C2 147(4) . . ?
C6 C8 C1 146(4) . . ?

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
N00A C1 C8 C6 -20(16) . . . . ?
C2 C6 C8 C1 36(23) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.025
_oxdiff_exptl_absorpt_empirical_full_min 0.559
####################################################################### 
# 
# 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_x1_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1815923'
loop_
_audit_author_name
_audit_author_address
'Yangyang Dang'
;Tianjin University
China
;
_audit_update_record             
;
2018-11-05 deposited with the CCDC.	2020-08-20 downloaded from the CCDC.
;
_audit_creation_date             2018-10-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        C16H24I4N2Pb
_chemical_formula_moiety         'I4 Pb, 1.8(C5), C6 N, C N'
_chemical_formula_sum            'C16 H24 I4 N2 Pb'
_chemical_formula_weight         959.16
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7497(8)
_cell_length_b                   8.7510(8)
_cell_length_c                   16.6830(15)
_cell_angle_alpha                99.7643(10)
_cell_angle_beta                 95.2258(10)
_cell_angle_gamma                90.3394(10)
_cell_volume                     1253.4(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6590
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.47
_shelx_estimated_absorpt_T_max   0.274
_shelx_estimated_absorpt_T_min   0.128
_exptl_absorpt_coefficient_mu    11.658
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.3551
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1549 before and 0.0472 after correction.
The Ratio of minimum to maximum transmission is 0.4763.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12361
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.244
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4003
_reflns_number_total             4421
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         2.229
_refine_diff_density_min         -1.794
_refine_diff_density_rms         0.435
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4421
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0348
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0618P)²+2.8504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1064
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.0000 0.5000 0.5000 0.02681(13) Uani 1 2 d S T P . .
Pb2 Pb 0.5000 0.0000 0.5000 0.02676(13) Uani 1 2 d S T P . .
I3 I 0.69049(6) 0.31031(6) 0.50178(4) 0.04192(16) Uani 1 1 d . . . . .
I4 I 1.19137(6) 0.19130(6) 0.50002(4) 0.04107(16) Uani 1 1 d . . . . .
I5 I 0.96295(8) 0.42039(7) 0.30401(4) 0.04828(17) Uani 1 1 d . . . . .
I6 I 0.48151(7) -0.06079(8) 0.30401(4) 0.04830(17) Uani 1 1 d . . . . .
C17 C 0.3055(15) -0.4819(16) 0.1393(7) 0.072(3) Uani 1 1 d . . . . .
C1 C 1.0023(13) -0.0967(14) 0.3031(7) 0.068(3) Uani 1 1 d . . . . .
N3 N 0.4708(16) 0.500(2) 0.6769(10) 0.140(7) Uani 1 1 d . . . . .
C5 C 0.491(3) -0.637(3) 0.2148(11) 0.144(9) Uani 1 1 d . . . . .
C6 C 0.411(2) -0.578(2) 0.1609(8) 0.121(8) Uani 1 1 d . . . . .
N0AA N 0.8928(8) 0.0268(8) 0.3381(5) 0.0476(17) Uani 1 1 d . . . . .
C1AA C 0.5964(16) 0.6208(14) 0.6723(10) 0.100(5) Uani 1 1 d . . . . .
C4AA C 0.7996(17) 0.0098(17) 0.1324(8) 0.079(4) Uani 1 1 d . . . . .
C2AA C 0.911(3) -0.077(2) 0.1600(8) 0.132(9) Uani 1 1 d . . . . .
C3 C 0.983(3) -0.125(3) 0.2182(12) 0.198(15) Uani 1 1 d . . . . .
C6AA C 1.072(4) 0.060(6) 0.111(3) 0.41(5) Uani 1 1 d . . . . .
C2 C 0.762(7) -0.271(4) 0.117(3) 0.38(4) Uani 1 1 d . . . . .
C3AA C 0.562(4) -0.438(6) 0.105(3) 0.40(5) Uani 1 1 d . . . . .
C5AA C 1.255(7) 0.232(4) 0.110(3) 0.35(4) Uani 1 1 d . . . . .
C9 C 1.132(4) 0.425(9) 0.0669(17) 0.39(5) Uani 1 1 d . . . . .
C10 C 0.833(7) 0.132(5) 0.0745(19) 0.43(5) Uani 1 1 d . . . . .
C13 C 0.310(7) -0.367(5) 0.0803(18) 0.42(5) Uani 1 1 d . . . . .
C14 C 0.622(4) -0.100(10) 0.0645(18) 0.44(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I3 3.1730(5) 2_766 ?
Pb1 I3 3.1730(5) . ?
Pb1 I4 3.1867(5) . ?
Pb1 I4 3.1867(5) 2_766 ?
Pb1 I5 3.2113(6) . ?
Pb1 I5 3.2114(7) 2_766 ?
Pb2 I3 3.1723(5) 2_656 ?
Pb2 I3 3.1723(5) . ?
Pb2 I4 3.1856(5) 1_455 ?
Pb2 I4 3.1856(5) 2_756 ?
Pb2 I6 3.2114(6) . ?
Pb2 I6 3.2114(6) 2_656 ?
I4 Pb2 3.1856(5) 1_655 ?
C17 C6 1.317(18) . ?
C17 C9 1.94(6) 1_445 ?
C17 C13 1.53(5) . ?
C1 N0AA 1.526(12) . ?
C1 C3 1.39(2) . ?
N3 C1AA 1.54(2) . ?
C5 C6 1.27(2) . ?
C4AA C2AA 1.33(2) . ?
C4AA C10 1.60(6) . ?
C4AA C14 1.98(7) . ?
C2AA C3 1.24(2) . ?
C9 C17 1.94(6) 1_665 ?

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 I3 180.0 2_766 . ?
I3 Pb1 I4 89.615(15) . 2_766 ?
I3 Pb1 I4 90.385(15) . . ?
I3 Pb1 I4 90.385(15) 2_766 2_766 ?
I3 Pb1 I4 89.615(15) 2_766 . ?
I3 Pb1 I5 91.128(16) 2_766 . ?
I3 Pb1 I5 88.872(16) 2_766 2_766 ?
I3 Pb1 I5 88.873(16) . . ?
I3 Pb1 I5 91.127(16) . 2_766 ?
I4 Pb1 I4 180.0 2_766 . ?
I4 Pb1 I5 91.906(15) . 2_766 ?
I4 Pb1 I5 88.094(15) . . ?
I4 Pb1 I5 91.905(15) 2_766 . ?
I4 Pb1 I5 88.095(15) 2_766 2_766 ?
I5 Pb1 I5 180.00(2) . 2_766 ?
I3 Pb2 I3 180.0 2_656 . ?
I3 Pb2 I4 90.400(15) 2_656 1_455 ?
I3 Pb2 I4 89.599(15) . 1_455 ?
I3 Pb2 I4 90.401(15) . 2_756 ?
I3 Pb2 I4 89.600(15) 2_656 2_756 ?
I3 Pb2 I6 91.136(16) 2_656 . ?
I3 Pb2 I6 88.865(16) 2_656 2_656 ?
I3 Pb2 I6 91.135(16) . 2_656 ?
I3 Pb2 I6 88.865(16) . . ?
I4 Pb2 I4 180.0 2_756 1_455 ?
I4 Pb2 I6 88.108(15) 2_756 . ?
I4 Pb2 I6 88.108(15) 1_455 2_656 ?
I4 Pb2 I6 91.892(15) 1_455 . ?
I4 Pb2 I6 91.892(15) 2_756 2_656 ?
I6 Pb2 I6 180.0 . 2_656 ?
Pb2 I3 Pb1 152.931(19) . . ?
Pb2 I4 Pb1 153.737(19) 1_655 . ?
C6 C17 C9 116(2) . 1_445 ?
C6 C17 C13 130(2) . . ?
C13 C17 C9 85(2) . 1_445 ?
C3 C1 N0AA 111.1(10) . . ?
C5 C6 C17 151.4(14) . . ?
C2AA C4AA C10 121(2) . . ?
C2AA C4AA C14 118(2) . . ?
C10 C4AA C14 98(2) . . ?
C3 C2AA C4AA 149.5(14) . . ?
C2AA C3 C1 140.9(16) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_x1_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1815926'
loop_
_audit_author_name
_audit_author_address
'Yangyang Dang' 'Tianjin University'
_audit_update_record             
;
2018-01-10 deposited with the CCDC.	2020-08-20 downloaded from the CCDC.
;
_audit_creation_date             2018-01-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        C16H24N2I4Pb
_chemical_formula_moiety         'C I4 Pb, C7 N, C10 N, C'
_chemical_formula_sum            'C16 H24 I4 N2 Pb'
_chemical_formula_weight         959.16
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7350(16)
_cell_length_b                   8.7359(16)
_cell_length_c                   16.673(3)
_cell_angle_alpha                99.694(5)
_cell_angle_beta                 95.220(6)
_cell_angle_gamma                90.393(5)
_cell_volume                     1248.6(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   0.592
_shelx_estimated_absorpt_T_min   0.203
_exptl_absorpt_coefficient_mu    11.703
_exptl_absorpt_correction_T_max  0.5922
_exptl_absorpt_correction_T_min  0.2031
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.551
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43782
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.753
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3598
_reflns_number_total             4403
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         3.513
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.319
_refine_ls_extinction_coef       0.00005(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4403
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0525
_refine_ls_restrained_S_all      1.175
_refine_ls_shift/su_max          0.264
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0694P)²+20.0363P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1482
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.5000 0.5000 0.0000 0.0224(2) Uani 1 2 d S T P . .
Pb2 Pb 0.0000 1.0000 0.0000 0.0224(2) Uani 1 2 d S T P . .
I1 I 0.19135(10) 0.69141(11) 0.00004(7) 0.0375(3) Uani 1 1 d . . . . .
I2 I 0.30967(11) 0.18951(11) -0.00169(7) 0.0387(3) Uani 1 1 d . . . . .
I3 I 0.51889(12) 0.56122(13) 0.19594(6) 0.0447(3) Uani 1 1 d . . . . .
I4 I 0.03660(13) 1.07915(12) 0.19586(6) 0.0448(3) Uani 1 1 d . . . . .
N1 N 0.1062(17) 0.4753(17) 0.1620(9) 0.052(4) Uani 1 1 d . . . . .
C1 C -0.001(3) 0.599(3) 0.1928(13) 0.077(8) Uani 1 1 d . . . . .
C2 C 0.697(3) 0.986(3) 0.3619(16) 0.075(6) Uani 1 1 d . . . . .
C3 C 0.202(3) 0.483(3) 0.3680(15) 0.074(6) Uani 1 1 d . . . . .
N2 N 0.473(3) 0.994(4) 0.176(2) 0.151(14) Uani 1 1 d . . . . .
C6 C 0.591(5) 1.076(4) 0.3407(15) 0.114(12) Uani 1 1 d . . . . .
C7 C 0.093(4) 0.575(4) 0.3423(15) 0.123(14) Uani 1 1 d . . . . .
C8 C 0.412(7) 0.981(6) 0.378(3) 0.25(4) Uani 1 1 d . . . . .
C9 C -0.188(3) 0.685(4) -0.0026(13) 0.097(9) Uani 1 1 d . . . . .
C22 C 0.595(3) 1.113(3) 0.1774(19) 0.105(11) Uani 1 1 d . . . . .
C15 C -0.061(7) 0.436(11) 0.391(5) 0.42(8) Uani 1 1 d . . . . .
C18 C -0.286(6) 0.274(9) 0.380(3) 0.25(4) Uani 1 1 d . . . . .
C21 C 0.750(10) 0.899(9) 0.413(3) 0.40(7) Uani 1 1 d . . . . .
C17 C 0.173(12) 0.381(10) 0.423(3) 0.43(8) Uani 1 1 d . . . . .
C19 C 0.48(2) 1.172(18) 0.567(4) 0.8(2) Uani 1 1 d . . . . .
C16 C -0.126(6) 0.193(17) 0.434(3) 0.46(9) Uani 1 1 d . . . . .
C5 C 0.363(7) 0.568(15) 0.428(4) 0.34(6) Uani 1 1 d . . . . .
C13 C 0.310(15) 0.793(10) 0.403(5) 0.51(10) Uani 1 1 d . . . . .
C10 C -0.006(5) 0.607(7) 0.285(2) 0.18(2) Uani 1 1 d . . . . .
C12 C 0.507(5) 1.135(5) 0.2837(17) 0.161(19) Uani 1 1 d . . . . .
C11 C 0.114(13) 0.721(18) 0.308(12) 1.0(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.1822(9) 2_665 ?
Pb1 I1 3.1822(9) . ?
Pb1 I2 3.1663(10) . ?
Pb1 I2 3.1663(10) 2_665 ?
Pb1 I3 3.2089(12) . ?
Pb1 I3 3.2089(12) 2_665 ?
Pb2 I1 3.1817(9) 2_575 ?
Pb2 I1 3.1817(9) . ?
Pb2 I2 3.1665(10) 2_565 ?
Pb2 I2 3.1665(10) 1_565 ?
Pb2 I4 3.2079(12) . ?
Pb2 I4 3.2079(12) 2_575 ?
I2 Pb2 3.1665(10) 1_545 ?
I2 C9 1.53(4) 2_565 ?
N1 C1 1.49(3) . ?
C1 C10 1.53(5) . ?
C2 C6 1.28(4) . ?
C2 C21 1.29(5) . ?
C3 C7 1.34(3) . ?
C3 C17 1.42(12) . ?
C3 C5 1.74(10) . ?
N2 C22 1.48(4) . ?
C6 C8 1.96(8) . ?
C6 C18 2.01(9) 1_665 ?
C6 C12 1.32(4) . ?
C7 C10 1.30(4) . ?
C7 C11 1.50(8) . ?
C8 C19 1.96(10) 2_676 ?
C8 C13 1.99(13) . ?
C9 I2 1.53(4) 2_565 ?
C22 C12 1.98(5) . ?
C18 C6 2.01(8) 1_445 ?
C18 C16 1.80(9) . ?
C19 C8 1.96(10) 2_676 ?
C19 C13 1.9(2) 2_676 ?
C13 C19 1.9(2) 2_676 ?
C10 C11 1.4(2) . ?

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 I1 180.0 2_665 . ?
I1 Pb1 I3 88.09(3) 2_665 2_665 ?
I1 Pb1 I3 91.91(3) . 2_665 ?
I1 Pb1 I3 91.91(3) 2_665 . ?
I1 Pb1 I3 88.09(3) . . ?
I2 Pb1 I1 89.53(3) . 2_665 ?
I2 Pb1 I1 90.47(3) . . ?
I2 Pb1 I1 89.53(3) 2_665 . ?
I2 Pb1 I1 90.47(3) 2_665 2_665 ?
I2 Pb1 I2 180.0 . 2_665 ?
I2 Pb1 I3 91.02(3) 2_665 . ?
I2 Pb1 I3 88.98(3) 2_665 2_665 ?
I2 Pb1 I3 88.98(3) . . ?
I2 Pb1 I3 91.02(3) . 2_665 ?
I3 Pb1 I3 180.00(4) 2_665 . ?
I1 Pb2 I1 180.00(4) . 2_575 ?
I1 Pb2 I4 91.93(3) . . ?
I1 Pb2 I4 88.07(3) 2_575 . ?
I1 Pb2 I4 88.07(3) . 2_575 ?
I1 Pb2 I4 91.93(3) 2_575 2_575 ?
I2 Pb2 I1 90.46(3) 2_565 . ?
I2 Pb2 I1 89.54(3) 2_565 2_575 ?
I2 Pb2 I1 90.46(3) 1_565 2_575 ?
I2 Pb2 I1 89.54(3) 1_565 . ?
I2 Pb2 I2 180.00(4) 2_565 1_565 ?
I2 Pb2 I4 91.08(3) 1_565 2_575 ?
I2 Pb2 I4 88.92(3) 1_565 . ?
I2 Pb2 I4 88.92(3) 2_565 2_575 ?
I2 Pb2 I4 91.08(3) 2_565 . ?
I4 Pb2 I4 180.0 . 2_575 ?
Pb2 I1 Pb1 153.78(3) . . ?
Pb1 I2 Pb2 152.83(3) . 1_545 ?
C9 I2 Pb1 75.9(9) 2_565 . ?
C9 I2 Pb2 76.9(9) 2_565 1_545 ?
N1 C1 C10 109(2) . . ?
C6 C2 C21 148(4) . . ?
C7 C3 C17 121(4) . . ?
C7 C3 C5 119(4) . . ?
C17 C3 C5 93(4) . . ?
C2 C6 C8 100(3) . . ?
C2 C6 C18 95(3) . 1_665 ?
C2 C6 C12 151(3) . . ?
C8 C6 C18 133.9(19) . 1_665 ?
C12 C6 C8 93(4) . . ?
C12 C6 C18 94(3) . 1_665 ?
C3 C7 C11 128(5) . . ?
C10 C7 C3 150(3) . . ?
C10 C7 C11 61(8) . . ?
C6 C8 C19 98(8) . 2_676 ?
C6 C8 C13 149(3) . . ?
C19 C8 C13 57(8) 2_676 . ?
N2 C22 C12 69(3) . . ?
C16 C18 C6 98(5) . 1_445 ?
C13 C19 C8 62(5) 2_676 2_676 ?
C19 C13 C8 61(7) 2_676 . ?
C7 C10 C1 133(3) . . ?
C7 C10 C11 67(5) . . ?
C11 C10 C1 95(8) . . ?
C6 C12 C22 115(3) . . ?
C10 C11 C7 53(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C10 C7 28(8) . . . . ?
N1 C1 C10 C11 91(4) . . . . ?
C1 C10 C11 C7 -135(4) . . . . ?
C2 C6 C12 C22 -19(11) . . . . ?
C3 C7 C10 C1 -40(15) . . . . ?
C3 C7 C10 C11 -115(11) . . . . ?
C3 C7 C11 C10 145(5) . . . . ?
C8 C6 C12 C22 -137(3) . . . . ?
C18 C6 C12 C22 89(3) 1_665 . . . ?
C21 C2 C6 C8 -33(9) . . . . ?
C21 C2 C6 C18 104(9) . . . 1_665 ?
C21 C2 C6 C12 -149(10) . . . . ?
C17 C3 C7 C10 -106(10) . . . . ?
C17 C3 C7 C11 159(11) . . . . ?
C5 C3 C7 C10 139(9) . . . . ?
C5 C3 C7 C11 44(11) . . . . ?
C11 C7 C10 C1 75(9) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
