# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_exp_562_v-3pypbi-dark-hemi
_database_code_depnum_ccdc_archive 'CCDC 2081449'
loop_
_audit_author_name
_audit_author_address
'Wenzhe Li'
;Jinan University
China
;
_audit_update_record             
;
2021-05-03 deposited with the CCDC.	2021-07-05 downloaded from the CCDC.
;
_audit_creation_date             2021-04-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I6 Pb, 2(C15 H14 N3)'
_chemical_formula_sum            'C30 H28 I6 N6 Pb'
_chemical_formula_weight         1441.17
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb I C N'
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                   13.0069(3)
_cell_length_b                   14.6783(3)
_cell_length_c                   10.1587(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.854(3)
_cell_angle_gamma                90
_cell_volume                     1846.09(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14265
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1020
_cell_measurement_theta_min      2.0960
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.616
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.593
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18696
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.309
_diffrn_reflns_theta_min         2.106
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00  72.00   0.50    4.49    --    8.42  37.00  30.00  144
  2  ω     47.00  78.00   0.50    4.49    --    8.42  19.00 -60.00   62
  3  ω     22.00  77.00   0.50    4.49    --    8.42  19.00-180.00  110
  4  ω     16.00  62.00   0.50    4.49    --    8.42  37.00-180.00   92
  5  ω      3.00  62.00   0.50    4.49    --    8.42  77.00-120.00  118
  6  ω      0.00  44.00   0.50    4.49    --    8.42  19.00 -60.00   88
  7  ω     -7.00  44.00   0.50    4.49    --   -9.59  37.00 -60.00  102
  8  ω    -13.00  51.00   0.50    4.49    --    8.42  77.00-180.00  128
  9  ω    -33.00  -8.00   0.50    4.49    --    8.42 -19.00 -60.00   50
 10  ω    -60.00 -13.00   0.50    4.49    --    8.42 -19.00   0.00   94
 11  ω    -46.00  26.00   0.50    4.49    --    8.42 -57.00  60.00  144
 12  ω      5.00  31.00   0.50    4.49    --    8.42 -99.00  30.00   52
 13  ω    -14.00  20.00   0.50    4.49    --   -9.59 -99.00 -30.00   68
 14  ω     16.00  41.00   0.50    4.49    --    8.42 -99.00 -90.00   50
 15  ω    -12.00  13.00   0.50    4.49    --   -9.59 -99.00-180.00   50
 16  ω    -22.00   3.00   0.50    4.49    --    8.42 -99.00 -90.00   50
 17  ω    -22.00   4.00   0.50    4.49    --   -9.59 -99.00 -60.00   52
 18  ω    -23.00  37.00   0.50    4.49    --    8.42 -99.00 -30.00  120
 19  ω    -21.00  17.00   0.50    4.49    --   -9.59 -99.00  30.00   76
 20  ω    -12.00  13.00   0.50    4.49    --    8.42 -99.00  90.00   50
 21  ω      4.00  30.00   0.50    4.49    --   -9.59  37.00 120.00   52
 22  ω    -16.00  10.00   0.50    4.49    --   -9.59 -99.00  90.00   52
 23  ω    -41.00  -2.00   0.50    4.49    --    8.42 -19.00 150.00   78
 24  ω    -61.00 -36.00   0.50    4.49    --    8.42 -19.00 -60.00   50
 25  ω    -44.00 -19.00   0.50    4.49    --   -9.59 125.00 150.00   50
 26  ω    -37.00 -12.00   0.50    4.49    --   -9.59 125.00   0.00   50
 27  ω    -52.00 -26.00   0.50    4.49    --   -9.59 125.00 -60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0423740000
_diffrn_orient_matrix_UB_12      -0.0028939000
_diffrn_orient_matrix_UB_13      -0.0634380000
_diffrn_orient_matrix_UB_21      -0.0385229000
_diffrn_orient_matrix_UB_22      0.0054142000
_diffrn_orient_matrix_UB_23      0.0359732000
_diffrn_orient_matrix_UB_31      0.0017966000
_diffrn_orient_matrix_UB_32      0.0479282000
_diffrn_orient_matrix_UB_33      -0.0078788000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1842
_reflns_number_total             2095
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2095
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0295
_refine_ls_restrained_S_all      1.069
_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)+(0.0342P)²+4.0489P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0722
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N005(H005), N006(H006), C009(H009), C00A(H00A), C00B(H00B), C00C(H00C),
 C00D(H00D), C00E(H00E)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.500000 0.500000 0.500000 0.03979(12) Uani 1 4 d S T P . .
I002 I 0.75978(4) 0.500000 0.52833(4) 0.04605(14) Uani 1 2 d S T P . .
I003 I 0.43368(4) 0.500000 0.17670(4) 0.05429(15) Uani 1 2 d S T P . .
I004 I 0.500000 0.72502(4) 0.500000 0.06300(17) Uani 1 2 d S T P . .
N005 N 0.8617(4) 0.500000 0.9655(5) 0.0386(13) Uani 1 2 d S T P . .
H005 H 0.841716 0.500001 0.876585 0.046 Uiso 1 2 calc R U P . .
N006 N 0.8164(3) 0.6495(3) 0.8115(4) 0.0497(10) Uani 1 1 d . . . . .
H006 H 0.802701 0.594679 0.781224 0.060 Uiso 1 1 calc R U . . .
C007 C 0.8773(3) 0.5789(4) 1.0355(5) 0.0422(11) Uani 1 1 d . . . . .
C008 C 0.8562(3) 0.6617(4) 0.9493(5) 0.0442(11) Uani 1 1 d . . . . .
C009 C 0.8769(4) 0.7498(4) 0.9954(6) 0.0564(15) Uani 1 1 d . . . . .
H009 H 0.903701 0.761451 1.089720 0.068 Uiso 1 1 calc R U . . .
C00A C 0.8581(4) 0.8211(4) 0.9022(7) 0.0633(16) Uani 1 1 d . . . . .
H00A H 0.872632 0.880484 0.934468 0.076 Uiso 1 1 calc R U . . .
C00B C 0.9277(7) 0.500000 1.2475(8) 0.068(3) Uani 1 2 d S T P . .
H00B H 0.950755 0.499999 1.343693 0.082 Uiso 1 2 calc R U P . .
C00C C 0.9112(4) 0.5816(5) 1.1785(5) 0.0578(14) Uani 1 1 d . . . . .
H00C H 0.922249 0.636694 1.226079 0.069 Uiso 1 1 calc R U . . .
C00D C 0.8181(5) 0.8052(4) 0.7624(7) 0.0652(16) Uani 1 1 d . . . . .
H00D H 0.805714 0.852905 0.699224 0.078 Uiso 1 1 calc R U . . .
C00E C 0.7969(5) 0.7169(4) 0.7191(6) 0.0632(15) Uani 1 1 d . . . . .
H00E H 0.769020 0.703977 0.625241 0.076 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 I002 3.3021(5) . ?
Pb01 I002 3.3021(5) 5_666 ?
Pb01 I003 3.1294(4) . ?
Pb01 I003 3.1295(4) 5_666 ?
Pb01 I004 3.3030(5) 5_666 ?
Pb01 I004 3.3029(5) . ?
N005 H005 0.8600 . ?
N005 C007 1.342(6) 6_565 ?
N005 C007 1.342(6) . ?
N006 H006 0.8600 . ?
N006 C008 1.347(6) . ?
N006 C00E 1.334(7) . ?
C007 C008 1.473(8) . ?
C007 C00C 1.384(7) . ?
C008 C009 1.373(7) . ?
C009 H009 0.9300 . ?
C009 C00A 1.382(8) . ?
C00A H00A 0.9300 . ?
C00A C00D 1.375(9) . ?
C00B H00B 0.9300 . ?
C00B C00C 1.371(7) . ?
C00B C00C 1.371(7) 6_565 ?
C00C H00C 0.9300 . ?
C00D H00D 0.9300 . ?
C00D C00E 1.369(8) . ?
C00E H00E 0.9300 . ?

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
I002 Pb01 I002 180.0 . 5_666 ?
I002 Pb01 I004 90.0 5_666 . ?
I002 Pb01 I004 90.0 . . ?
I002 Pb01 I004 90.0 . 5_666 ?
I002 Pb01 I004 90.0 5_666 5_666 ?
I003 Pb01 I002 92.116(12) 5_666 5_666 ?
I003 Pb01 I002 92.116(12) . . ?
I003 Pb01 I002 87.883(12) 5_666 . ?
I003 Pb01 I002 87.884(12) . 5_666 ?
I003 Pb01 I003 180.0 . 5_666 ?
I003 Pb01 I004 90.0 5_666 5_666 ?
I003 Pb01 I004 90.0 5_666 . ?
I003 Pb01 I004 90.0 . . ?
I003 Pb01 I004 90.0 . 5_666 ?
I004 Pb01 I004 180.0 . 5_666 ?
C007 N005 H005 120.3 . . ?
C007 N005 H005 120.3 6_565 . ?
C007 N005 C007 119.4(6) . 6_565 ?
C008 N006 H006 117.9 . . ?
C00E N006 H006 117.9 . . ?
C00E N006 C008 124.2(5) . . ?
N005 C007 C008 115.3(4) . . ?
N005 C007 C00C 121.9(5) . . ?
C00C C007 C008 122.8(5) . . ?
N006 C008 C007 116.7(4) . . ?
N006 C008 C009 116.9(5) . . ?
C009 C008 C007 126.3(5) . . ?
C008 C009 H009 119.8 . . ?
C008 C009 C00A 120.3(5) . . ?
C00A C009 H009 119.8 . . ?
C009 C00A H00A 119.7 . . ?
C00D C00A C009 120.7(5) . . ?
C00D C00A H00A 119.7 . . ?
C00C C00B H00B 119.1 6_565 . ?
C00C C00B H00B 119.1 . . ?
C00C C00B C00C 121.8(7) 6_565 . ?
C007 C00C H00C 121.3 . . ?
C00B C00C C007 117.5(6) . . ?
C00B C00C H00C 121.3 . . ?
C00A C00D H00D 121.0 . . ?
C00E C00D C00A 117.9(6) . . ?
C00E C00D H00D 121.0 . . ?
N006 C00E C00D 120.0(6) . . ?
N006 C00E H00E 120.0 . . ?
C00D C00E H00E 120.0 . . ?

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
N005 C007 C008 N006 4.6(6) . . . . ?
N005 C007 C008 C009 -172.8(5) . . . . ?
N005 C007 C00C C00B -0.4(8) . . . . ?
N006 C008 C009 C00A -0.7(7) . . . . ?
C007 N005 C007 C008 -179.0(3) 6_565 . . . ?
C007 N005 C007 C00C 1.1(8) 6_565 . . . ?
C007 C008 C009 C00A 176.7(4) . . . . ?
C008 N006 C00E C00D 0.3(9) . . . . ?
C008 C007 C00C C00B 179.7(5) . . . . ?
C008 C009 C00A C00D 0.3(8) . . . . ?
C009 C00A C00D C00E 0.5(9) . . . . ?
C00A C00D C00E N006 -0.8(9) . . . . ?
C00C C007 C008 N006 -175.5(4) . . . . ?
C00C C007 C008 C009 7.1(7) . . . . ?
C00C C00B C00C C007 -0.3(11) 6_565 . . . ?
C00E N006 C008 C007 -177.3(5) . . . . ?
C00E N006 C008 C009 0.4(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 1.759
_oxdiff_exptl_absorpt_empirical_full_min 0.668
####################################################################### 
# 
# 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_exp_566_3pypbi3-180c
_database_code_depnum_ccdc_archive 'CCDC 2081450'
loop_
_audit_author_name
_audit_author_address
'Wenzhe Li'
;Jinan University
China
;
_audit_update_record             
;
2021-05-03 deposited with the CCDC.	2021-07-05 downloaded from the CCDC.
;
_audit_creation_date             2021-03-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H22 I6 N6 Pb3'
_chemical_formula_sum            'C30 H22 I6 N6 Pb3'
_chemical_formula_weight         1849.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb I C N'
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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   22.4598(5)
_cell_length_b                   12.1864(2)
_cell_length_c                   14.4057(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3942.90(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14514
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1960
_cell_measurement_theta_min      1.8170
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    17.506
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    3.116
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30343
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.331
_diffrn_reflns_theta_min         1.813
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00   9.00   0.50    5.20    --   -9.59  19.00 -30.00   54
  2  ω     22.00  60.00   0.50    5.20    --   -9.59  19.00 -30.00   76
  3  ω     -3.00  23.00   0.50    5.20    --    8.42 -92.00 120.00   52
  4  ω    -23.00  16.00   0.50    5.20    --   -9.59 -99.00   0.00   78
  5  ω    -36.00  -8.00   0.50    5.20    --   -9.59 -30.00 -86.00   56
  6  ω    -59.00  -1.00   0.50    5.20    --    8.42 -19.00-150.00  116
  7  ω    -12.00  36.00   0.50    5.20    --    8.42 -99.00-120.00   96
  8  ω    -14.00  13.00   0.50    5.20    --   -9.59 -99.00-150.00   54
  9  ω    -40.00   2.00   0.50    5.20    --    8.42 -19.00 -60.00   84
 10  ω    -36.00 -11.00   0.50    5.20    --    8.42 -92.00 120.00   50
 11  ω    -55.00 -29.00   0.50    5.20    --   -9.59 125.00 120.00   52
 12  ω    -54.00 -29.00   0.50    5.20    --   -9.59 132.00 120.00   50
 13  ω    -44.00 -19.00   0.50    5.20    --    8.42 -19.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0289227000
_diffrn_orient_matrix_UB_12      0.0226428000
_diffrn_orient_matrix_UB_13      -0.0049344000
_diffrn_orient_matrix_UB_21      0.0029387000
_diffrn_orient_matrix_UB_22      -0.0021397000
_diffrn_orient_matrix_UB_23      -0.0489886000
_diffrn_orient_matrix_UB_31      -0.0123435000
_diffrn_orient_matrix_UB_32      -0.0535726000
_diffrn_orient_matrix_UB_33      -0.0001365000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3312
_reflns_number_total             4243
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.116
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       0.000465(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4243
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0273
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0181P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0489
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C16(H16), C8(H8), C13(H13), C15(H15), C20(H20), C21(H21),
 C1(H1), C2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.58940(2) 0.34888(2) 0.45787(2) 0.03180(7) Uani 1 1 d . . . . .
Pb2 Pb 0.500000 0.58256(2) 0.250000 0.04036(10) Uani 1 2 d S T P . .
I3 I 0.55724(2) 0.63250(3) 0.44941(2) 0.03538(10) Uani 1 1 d . . . . .
I4 I 0.60842(2) 0.25396(3) 0.66613(2) 0.03980(11) Uani 1 1 d . . . . .
I5 I 0.59790(2) 0.38786(3) 0.23840(3) 0.04955(12) Uani 1 1 d . . . . .
N17 N 0.69641(18) 0.4192(3) 0.4929(3) 0.0332(10) Uani 1 1 d . . . . .
N6 N 0.67482(17) 0.2178(3) 0.4171(3) 0.0299(10) Uani 1 1 d . . . . .
C12 C 0.7426(2) 0.3526(4) 0.4775(4) 0.0339(13) Uani 1 1 d . . . . .
C7 C 0.7316(2) 0.2550(4) 0.4201(4) 0.0367(13) Uani 1 1 d . . . . .
C11 C 0.6631(2) 0.1252(4) 0.3713(4) 0.0330(13) Uani 1 1 d . . . . .
C10 C 0.7072(3) 0.0691(4) 0.3233(4) 0.0500(16) Uani 1 1 d . . . . .
H10 H 0.698216 0.004618 0.291812 0.060 Uiso 1 1 calc R U . . .
N19 N 0.55889(19) 0.1580(3) 0.3996(3) 0.0355(11) Uani 1 1 d . . . . .
C9 C 0.7644(3) 0.1097(5) 0.3229(4) 0.0544(17) Uani 1 1 d . . . . .
H9 H 0.794200 0.074253 0.289654 0.065 Uiso 1 1 calc R U . . .
C16 C 0.7041(2) 0.5087(4) 0.5457(4) 0.0427(14) Uani 1 1 d . . . . .
H16 H 0.671717 0.554143 0.557417 0.051 Uiso 1 1 calc R U . . .
C8 C 0.7765(2) 0.2024(5) 0.3716(4) 0.0495(15) Uani 1 1 d . . . . .
H8 H 0.814958 0.230567 0.372454 0.059 Uiso 1 1 calc R U . . .
C13 C 0.7981(3) 0.3735(5) 0.5151(5) 0.0578(18) Uani 1 1 d . . . . .
H13 H 0.829713 0.325824 0.504629 0.069 Uiso 1 1 calc R U . . .
C15 C 0.7588(3) 0.5355(5) 0.5831(4) 0.0566(17) Uani 1 1 d . . . . .
H15 H 0.763802 0.599200 0.617727 0.068 Uiso 1 1 calc R U . . .
C18 C 0.6008(2) 0.0856(4) 0.3749(3) 0.0333(13) Uani 1 1 d . . . . .
C20 C 0.5020(2) 0.1249(5) 0.4008(4) 0.0514(17) Uani 1 1 d . . . . .
H20 H 0.472723 0.175669 0.416202 0.062 Uiso 1 1 calc R U . . .
C14 C 0.8055(3) 0.4652(7) 0.5676(5) 0.069(2) Uani 1 1 d . . . . .
H14 H 0.841(3) 0.483(5) 0.587(5) 0.083 Uiso 1 1 d . U . . .
C21 C 0.4851(3) 0.0191(5) 0.3804(4) 0.0576(18) Uani 1 1 d . . . . .
H21 H 0.445165 -0.001173 0.381940 0.069 Uiso 1 1 calc R U . . .
C1 C 0.5863(3) -0.0221(4) 0.3549(4) 0.0470(16) Uani 1 1 d . . . . .
H1 H 0.616002 -0.072003 0.339572 0.056 Uiso 1 1 calc R U . . .
C2 C 0.5279(3) -0.0553(5) 0.3578(4) 0.0561(17) Uani 1 1 d . . . . .
H2 H 0.517770 -0.127620 0.344461 0.067 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I4 3.2436(4) . ?
Pb1 I5 3.2028(4) . ?
Pb1 N17 2.601(4) . ?
Pb1 N6 2.565(4) . ?
Pb1 N19 2.566(4) . ?
Pb2 I3 3.2055(4) 3_655 ?
Pb2 I3 3.2055(4) . ?
Pb2 I4 3.3702(4) 7_565 ?
Pb2 I4 3.3702(4) 5_666 ?
Pb2 I5 3.2393(4) 3_655 ?
Pb2 I5 3.2393(4) . ?
N17 C12 1.336(6) . ?
N17 C16 1.341(6) . ?
N6 C7 1.354(6) . ?
N6 C11 1.334(6) . ?
C12 C7 1.469(7) . ?
C12 C13 1.382(7) . ?
C7 C8 1.384(7) . ?
C11 C10 1.387(7) . ?
C11 C18 1.482(7) . ?
C10 H10 0.9300 . ?
C10 C9 1.375(8) . ?
N19 C18 1.338(6) . ?
N19 C20 1.339(6) . ?
C9 H9 0.9300 . ?
C9 C8 1.358(8) . ?
C16 H16 0.9300 . ?
C16 C15 1.379(8) . ?
C8 H8 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.360(9) . ?
C15 H15 0.9300 . ?
C15 C14 1.372(9) . ?
C18 C1 1.383(7) . ?
C20 H20 0.9300 . ?
C20 C21 1.377(7) . ?
C14 H14 0.86(6) . ?
C21 H21 0.9300 . ?
C21 C2 1.362(8) . ?
C1 H1 0.9300 . ?
C1 C2 1.372(8) . ?
C2 H2 0.9300 . ?

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
I5 Pb1 I4 163.348(12) . . ?
N17 Pb1 I4 79.40(9) . . ?
N17 Pb1 I5 95.04(9) . . ?
N6 Pb1 I4 83.74(9) . . ?
N6 Pb1 I5 79.74(9) . . ?
N6 Pb1 N17 63.78(13) . . ?
N6 Pb1 N19 63.92(13) . . ?
N19 Pb1 I4 90.83(10) . . ?
N19 Pb1 I5 80.06(10) . . ?
N19 Pb1 N17 127.50(13) . . ?
I3 Pb2 I3 158.111(16) . 3_655 ?
I3 Pb2 I4 81.738(9) 3_655 7_565 ?
I3 Pb2 I4 85.369(10) . 7_565 ?
I3 Pb2 I4 85.368(10) 3_655 5_666 ?
I3 Pb2 I4 81.737(9) . 5_666 ?
I3 Pb2 I5 111.413(10) 3_655 . ?
I3 Pb2 I5 85.010(10) 3_655 3_655 ?
I3 Pb2 I5 85.012(10) . . ?
I3 Pb2 I5 111.414(10) . 3_655 ?
I4 Pb2 I4 107.526(14) 7_565 5_666 ?
I5 Pb2 I4 160.383(10) . 5_666 ?
I5 Pb2 I4 160.383(10) 3_655 7_565 ?
I5 Pb2 I4 85.643(10) 3_655 5_666 ?
I5 Pb2 I4 85.643(9) . 7_565 ?
I5 Pb2 I5 85.810(16) 3_655 . ?
Pb1 I4 Pb2 91.468(9) . 5_666 ?
Pb1 I5 Pb2 90.987(10) . . ?
C12 N17 Pb1 119.0(3) . . ?
C12 N17 C16 119.2(5) . . ?
C16 N17 Pb1 119.8(3) . . ?
C7 N6 Pb1 119.3(3) . . ?
C11 N6 Pb1 119.5(3) . . ?
C11 N6 C7 119.0(4) . . ?
N17 C12 C7 117.0(4) . . ?
N17 C12 C13 121.6(5) . . ?
C13 C12 C7 121.4(5) . . ?
N6 C7 C12 116.6(4) . . ?
N6 C7 C8 121.0(5) . . ?
C8 C7 C12 122.4(5) . . ?
N6 C11 C10 121.5(5) . . ?
N6 C11 C18 116.4(4) . . ?
C10 C11 C18 122.1(5) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 C11 119.4(5) . . ?
C9 C10 H10 120.3 . . ?
C18 N19 Pb1 119.8(3) . . ?
C18 N19 C20 118.4(4) . . ?
C20 N19 Pb1 121.5(3) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 C10 118.9(5) . . ?
C8 C9 H9 120.5 . . ?
N17 C16 H16 119.0 . . ?
N17 C16 C15 121.9(5) . . ?
C15 C16 H16 119.0 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.0(5) . . ?
C9 C8 H8 120.0 . . ?
C12 C13 H13 120.7 . . ?
C14 C13 C12 118.6(6) . . ?
C14 C13 H13 120.7 . . ?
C16 C15 H15 121.0 . . ?
C14 C15 C16 118.0(6) . . ?
C14 C15 H15 121.0 . . ?
N19 C18 C11 117.3(4) . . ?
N19 C18 C1 121.0(5) . . ?
C1 C18 C11 121.6(5) . . ?
N19 C20 H20 118.6 . . ?
N19 C20 C21 122.9(5) . . ?
C21 C20 H20 118.6 . . ?
C13 C14 C15 120.7(6) . . ?
C13 C14 H14 119(4) . . ?
C15 C14 H14 120(4) . . ?
C20 C21 H21 120.7 . . ?
C2 C21 C20 118.7(6) . . ?
C2 C21 H21 120.7 . . ?
C18 C1 H1 120.0 . . ?
C2 C1 C18 119.9(5) . . ?
C2 C1 H1 120.0 . . ?
C21 C2 C1 119.1(6) . . ?
C21 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?

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
Pb1 N17 C12 C7 15.1(6) . . . . ?
Pb1 N17 C12 C13 -163.9(4) . . . . ?
Pb1 N17 C16 C15 165.5(4) . . . . ?
Pb1 N6 C7 C12 21.6(6) . . . . ?
Pb1 N6 C7 C8 -158.8(4) . . . . ?
Pb1 N6 C11 C10 160.0(4) . . . . ?
Pb1 N6 C11 C18 -20.3(5) . . . . ?
Pb1 N19 C18 C11 -7.6(6) . . . . ?
Pb1 N19 C18 C1 171.4(4) . . . . ?
Pb1 N19 C20 C21 -172.2(5) . . . . ?
N17 C12 C7 N6 -24.3(7) . . . . ?
N17 C12 C7 C8 156.1(5) . . . . ?
N17 C12 C13 C14 -1.1(9) . . . . ?
N17 C16 C15 C14 -2.3(9) . . . . ?
N6 C7 C8 C9 -2.4(8) . . . . ?
N6 C11 C10 C9 0.0(8) . . . . ?
N6 C11 C18 N19 18.4(7) . . . . ?
N6 C11 C18 C1 -160.7(5) . . . . ?
C12 N17 C16 C15 1.3(8) . . . . ?
C12 C7 C8 C9 177.1(5) . . . . ?
C12 C13 C14 C15 0.1(11) . . . . ?
C7 N6 C11 C10 -2.9(7) . . . . ?
C7 N6 C11 C18 176.8(4) . . . . ?
C7 C12 C13 C14 180.0(6) . . . . ?
C11 N6 C7 C12 -175.4(4) . . . . ?
C11 N6 C7 C8 4.2(7) . . . . ?
C11 C10 C9 C8 1.8(9) . . . . ?
C11 C18 C1 C2 -179.1(5) . . . . ?
C10 C11 C18 N19 -161.9(5) . . . . ?
C10 C11 C18 C1 19.1(8) . . . . ?
C10 C9 C8 C7 -0.6(9) . . . . ?
N19 C18 C1 C2 1.8(8) . . . . ?
N19 C20 C21 C2 -0.1(10) . . . . ?
C16 N17 C12 C7 179.4(4) . . . . ?
C16 N17 C12 C13 0.4(8) . . . . ?
C16 C15 C14 C13 1.5(10) . . . . ?
C13 C12 C7 N6 154.7(5) . . . . ?
C13 C12 C7 C8 -24.9(8) . . . . ?
C18 C11 C10 C9 -179.7(5) . . . . ?
C18 N19 C20 C21 1.9(9) . . . . ?
C18 C1 C2 C21 0.0(9) . . . . ?
C20 N19 C18 C11 178.2(5) . . . . ?
C20 N19 C18 C1 -2.7(8) . . . . ?
C20 C21 C2 C1 -0.9(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.738
_oxdiff_exptl_absorpt_empirical_full_min 0.653
####################################################################### 
# 
# 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_exp_567_vpbi3py
_database_code_depnum_ccdc_archive 'CCDC 2081451'
loop_
_audit_author_name
_audit_author_address
'Wenzhe Li'
;Jinan University
China
;
_audit_update_record             
;
2021-05-03 deposited with the CCDC.	2021-07-05 downloaded from the CCDC.
;
_audit_creation_date             2021-05-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I17 Pb5, I, 4(C15 H13 N3)'
_chemical_formula_sum            'C60 H52 I18 N12 Pb5'
_chemical_formula_weight         4261.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'V Pb I C N'
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                   12.8492(2)
_cell_length_b                   12.89296(18)
_cell_length_c                   15.7151(2)
_cell_angle_alpha                86.4469(11)
_cell_angle_beta                 70.5166(13)
_cell_angle_gamma                72.3962(13)
_cell_volume                     2337.22(6)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    23472
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9030
_cell_measurement_theta_min      1.7560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    14.958
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    3.028
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44481
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.203
_diffrn_reflns_theta_min         1.659
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -36.00  22.00   0.50    2.51    --  -15.91  45.00 -60.00  116
  2  ω      8.00  49.00   0.50    2.51    --  -15.91  61.00 -30.00   82
  3  ω     -6.00  85.00   0.50    2.51    --   14.73  37.00-113.00  182
  4  ω     -7.00  84.00   0.50    2.51    --   14.73  61.00 -30.00  182
  5  ω     -2.00  42.00   0.50    2.51    --   14.73 -61.00  30.00   88
  6  ω     26.00  51.00   0.50    2.51    --   14.73 -94.00  60.00   50
  7  ω     12.00  59.00   0.50    2.51    --   14.73-125.00  30.00   94
  8  ω     15.00  69.00   0.50    2.51    --   14.73-125.00 150.00  108
  9  ω    -15.00  14.00   0.50    2.51    --   14.73 -30.00  90.00   58
 10  ω    -22.00   4.00   0.50    2.51    --  -15.91 -61.00  60.00   52
 11  ω    -35.00  30.00   0.50    2.51    --   14.73 -94.00  30.00  130
 12  ω    -23.00   2.00   0.50    2.51    --  -15.91 -15.00 -90.00   50
 13  ω    -33.00  54.00   0.50    2.51    --  -15.91  37.00-113.00  174
 14  ω    -16.00  81.00   0.50    2.51    --   14.73  77.00-120.00  194
 15  ω    -27.00  -2.00   0.50    2.51    --  -15.91  61.00 -30.00   50
 16  ω    -55.00   3.00   0.50    2.51    --   14.73 -15.00  30.00  116
 17  ω    -41.00 -16.00   0.50    2.51    --  -15.91 -37.00  90.00   50
 18  ω    -45.00  20.00   0.50    2.51    --   14.73 -37.00  90.00  130
 19  ω    -37.00   6.00   0.50    2.51    --   14.73 -30.00 -90.00   86
 20  ω    -30.00  -5.00   0.50    2.51    --  -15.91 -94.00-120.00   50
 21  ω     -7.00  21.00   0.50    2.51    --  -15.91 -94.00-150.00   56
 22  ω    -39.00 -13.00   0.50    2.51    --   14.73 -61.00  30.00   52
 23  ω     -7.00  19.00   0.50    2.51    --   14.73 -94.00  60.00   52
 24  ω    -28.00  11.00   0.50    2.51    --  -15.91 -94.00 150.00   78
 25  ω    -22.00   3.00   0.50    2.51    --  -15.91 -94.00  30.00   50
 26  ω    -70.00 -45.00   0.50    2.51    --  -15.91 -61.00  60.00   50
 27  ω    -72.00 -47.00   0.50    2.51    --  -15.91 -37.00  90.00   50
 28  ω     32.00  85.00   0.50    2.51    --   14.73  77.00 150.00  106
 29  ω    -44.00 -19.00   0.50    2.51    --   14.73 133.00 123.43   50
 30  ω    -70.00 -40.00   0.50    2.51    --  -15.91 125.00 -30.00   60
 31  ω    -59.00 -33.00   0.50    2.51    --  -15.91 125.00 -90.00   52
 32  ω    -81.00 -56.00   0.50    2.51    --  -15.91 -15.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0409551000
_diffrn_orient_matrix_UB_12      -0.0039361000
_diffrn_orient_matrix_UB_13      0.0220634000
_diffrn_orient_matrix_UB_21      -0.0071164000
_diffrn_orient_matrix_UB_22      0.0565724000
_diffrn_orient_matrix_UB_23      -0.0045908000
_diffrn_orient_matrix_UB_31      -0.0451490000
_diffrn_orient_matrix_UB_32      0.0110282000
_diffrn_orient_matrix_UB_33      0.0422918000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7322
_reflns_number_total             9900
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.694
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         9900
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0325
_refine_ls_restrained_S_all      0.971
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0261P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0645
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N00K(H00K), C00L(H00L), C00P(H00P), C00Q(H00Q), C00S(H00S), C00U(H00U),
 C00V(H00V), C00Y(H00Y), C5(H5), C7(H7), C13(H13), C14(H14), C15(H15), C17(H17),
  C18(H18), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28), C32(H32), C1(H1),
 C8(H8)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 1.000000 0.500000 1.000000 0.03815(9) Uani 1 2 d S . P . .
Pb02 Pb 0.83531(2) 0.09745(2) 0.70984(2) 0.04023(7) Uani 1 1 d . . . . .
Pb03 Pb 0.92663(2) 0.28449(2) 0.86229(2) 0.03890(7) Uani 1 1 d . . . . .
I004 I 0.94070(4) 0.30232(4) 0.65779(3) 0.04858(12) Uani 1 1 d . . . . .
I005 I 0.81481(4) 0.54811(3) 0.89303(3) 0.04383(11) Uani 1 1 d . . . . .
I006 I 1.08024(4) 0.71087(4) 0.92968(3) 0.05049(13) Uani 1 1 d . . . . .
I007 I 0.73933(4) -0.10167(3) 0.76272(3) 0.04876(12) Uani 1 1 d . . . . .
I008 I 0.62399(4) 0.19246(3) 0.63632(3) 0.04953(12) Uani 1 1 d . . . . .
I009 I 1.16719(4) 0.34309(4) 0.82240(3) 0.05289(13) Uani 1 1 d . . . . .
I00A I 1.02759(4) 0.02674(4) 0.81548(3) 0.05915(14) Uani 1 1 d . . . . .
I00B I 0.500000 0.500000 0.500000 0.0593(2) Uani 1 2 d S . P . .
I00C I 0.68163(4) 0.23724(4) 0.89877(3) 0.05927(14) Uani 1 1 d . . . . .
I00D I 1.000000 0.000000 0.500000 0.0655(2) Uani 1 2 d S . P . .
N00E N 0.7122(4) 0.4886(3) 0.5993(3) 0.0309(11) Uani 1 1 d . . . . .
N00F N 0.8053(5) 0.3364(4) 0.4672(4) 0.0387(14) Uani 1 1 d . . . . .
N00G N 0.4581(4) 0.9203(4) 0.7119(3) 0.0397(13) Uani 1 1 d . . . . .
N00H N 0.5218(5) 0.4738(4) 0.7210(4) 0.0493(15) Uani 1 1 d . . . . .
N00I N 0.4329(6) 1.0518(5) 0.8466(4) 0.069(2) Uani 1 1 d . . . . .
C00J C 0.6740(5) 0.5545(5) 0.6736(4) 0.0349(14) Uani 1 1 d . . . . .
N00K N 0.6383(5) 0.9175(4) 0.5632(3) 0.0564(16) Uani 1 1 d . . . . .
H00K H 0.626013 0.948430 0.613988 0.068 Uiso 1 1 calc R U . . .
C00L C 0.2616(6) 1.0235(6) 0.9384(4) 0.058(2) Uani 1 1 d . . . . .
H00L H 0.205429 0.987847 0.951613 0.069 Uiso 1 1 calc R U . . .
C00M C 0.8402(5) 0.4256(5) 0.4511(4) 0.0378(15) Uani 1 1 d . . . . .
C00O C 0.7985(5) 0.5047(5) 0.5288(4) 0.0351(14) Uani 1 1 d . . . . .
C00P C 0.7197(5) 0.6366(5) 0.6799(4) 0.0462(17) Uani 1 1 d . . . . .
H00P H 0.692689 0.679511 0.732713 0.055 Uiso 1 1 calc R U . . .
C00Q C 0.9101(6) 0.2622(6) 0.3220(4) 0.058(2) Uani 1 1 d . . . . .
H00Q H 0.933855 0.206191 0.278810 0.069 Uiso 1 1 calc R U . . .
C00R C 0.3773(5) 0.9156(5) 0.7908(4) 0.0412(16) Uani 1 1 d . . . . .
C00S C 0.3337(7) 1.1563(6) 0.9808(5) 0.073(2) Uani 1 1 d . . . . .
H00S H 0.327611 1.209280 1.021191 0.087 Uiso 1 1 calc R U . . .
C00U C 0.8058(6) 0.6531(5) 0.6062(5) 0.0562(19) Uani 1 1 d . . . . .
H00U H 0.836946 0.708975 0.608291 0.067 Uiso 1 1 calc R U . . .
C00V C 0.9131(6) 0.4347(6) 0.3669(4) 0.0540(19) Uani 1 1 d . . . . .
H00V H 0.939172 0.495581 0.353083 0.065 Uiso 1 1 calc R U . . .
C00W C 0.5762(5) 0.5340(5) 0.7449(4) 0.0374(15) Uani 1 1 d . . . . .
C00X C 0.4803(5) 0.8489(5) 0.6463(4) 0.0422(16) Uani 1 1 d . . . . .
C00Y C 0.4232(6) 0.7695(5) 0.6566(5) 0.0549(19) Uani 1 1 d . . . . .
H00Y H 0.441075 0.719660 0.609682 0.066 Uiso 1 1 calc R U . . .
C5 C 0.8469(6) 0.5873(5) 0.5287(4) 0.0503(18) Uani 1 1 d . . . . .
H5 H 0.905242 0.598093 0.478062 0.060 Uiso 1 1 calc R U . . .
C7 C 0.9480(6) 0.3506(6) 0.3014(4) 0.062(2) Uani 1 1 d . . . . .
H7 H 0.997462 0.355815 0.243656 0.075 Uiso 1 1 calc R U . . .
C9 C 0.3558(5) 0.9973(5) 0.8593(4) 0.0432(16) Uani 1 1 d . . . . .
C13 C 0.4302(6) 0.4468(6) 0.7766(5) 0.064(2) Uani 1 1 d . . . . .
H13 H 0.395922 0.404732 0.755414 0.076 Uiso 1 1 calc R U . . .
C14 C 0.7241(6) 0.9331(6) 0.4906(5) 0.074(2) Uani 1 1 d . . . . .
H14 H 0.769087 0.975573 0.495429 0.088 Uiso 1 1 calc R U . . .
C15 C 0.5910(7) 0.8061(6) 0.4812(5) 0.075(2) Uani 1 1 d . . . . .
H15 H 0.547757 0.760866 0.478518 0.090 Uiso 1 1 calc R U . . .
C17 C 0.3882(6) 0.4823(6) 0.8652(5) 0.061(2) Uani 1 1 d . . . . .
H17 H 0.324321 0.465101 0.905049 0.073 Uiso 1 1 calc R U . . .
C18 C 0.2525(7) 1.1045(7) 0.9980(5) 0.071(2) Uani 1 1 d . . . . .
H18 H 0.189068 1.123045 1.050722 0.085 Uiso 1 1 calc R U . . .
C21 C 0.5714(6) 0.8571(5) 0.5609(4) 0.0467(18) Uani 1 1 d . . . . .
C22 C 0.8366(6) 0.2558(5) 0.4069(4) 0.0487(18) Uani 1 1 d . . . . .
H22 H 0.808996 0.195888 0.421994 0.058 Uiso 1 1 calc R U . . .
C24 C 0.4239(7) 1.1291(7) 0.9032(5) 0.088(3) Uani 1 1 d . . . . .
H24 H 0.480349 1.164549 0.889155 0.106 Uiso 1 1 calc R U . . .
C25 C 0.5354(6) 0.5700(5) 0.8360(5) 0.0548(19) Uani 1 1 d . . . . .
H25 H 0.571501 0.611012 0.856254 0.066 Uiso 1 1 calc R U . . .
C27 C 0.6754(8) 0.8218(8) 0.4044(5) 0.096(3) Uani 1 1 d . . . . .
H27 H 0.686869 0.790188 0.349070 0.115 Uiso 1 1 calc R U . . .
C28 C 0.7425(7) 0.8846(7) 0.4102(5) 0.076(3) Uani 1 1 d . . . . .
H28 H 0.800752 0.894013 0.358937 0.091 Uiso 1 1 calc R U . . .
C32 C 0.4414(7) 0.5437(6) 0.8948(5) 0.066(2) Uani 1 1 d . . . . .
H32 H 0.413457 0.567719 0.955084 0.080 Uiso 1 1 calc R U . . .
C1 C 0.3180(6) 0.8399(6) 0.8066(5) 0.0565(19) Uani 1 1 d . . . . .
H1 H 0.263864 0.837781 0.862833 0.068 Uiso 1 1 calc R U . . .
C8 C 0.3403(6) 0.7679(6) 0.7381(6) 0.066(2) Uani 1 1 d . . . . .
H8 H 0.299121 0.717742 0.746728 0.079 Uiso 1 1 calc R U . . .
H00I H 0.489(4) 1.041(4) 0.796(3) 0.022(15) Uiso 1 1 d . . . . .
H00F H 0.762(5) 0.329(5) 0.513(4) 0.06(2) Uiso 1 1 d . . . . .
H00H H 0.545(6) 0.444(5) 0.658(4) 0.09(3) Uiso 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 I005 3.2433(4) 2_767 ?
Pb01 I005 3.2433(4) . ?
Pb01 I006 3.1998(4) . ?
Pb01 I006 3.1998(4) 2_767 ?
Pb01 I009 3.2510(4) . ?
Pb01 I009 3.2510(4) 2_767 ?
Pb02 I004 3.2615(5) . ?
Pb02 I007 3.1255(5) . ?
Pb02 I008 3.1802(5) . ?
Pb02 I00A 3.2980(5) . ?
Pb02 I00C 3.2501(5) . ?
Pb02 I00D 3.3438(2) . ?
Pb03 I004 3.1560(5) . ?
Pb03 I005 3.2613(5) . ?
Pb03 I006 3.2445(5) 2_767 ?
Pb03 I009 3.2526(5) . ?
Pb03 I00A 3.2135(5) . ?
Pb03 I00C 3.2438(5) . ?
N00E C00J 1.347(6) . ?
N00E C00O 1.339(6) . ?
N00F C00M 1.337(7) . ?
N00F C22 1.325(7) . ?
N00F H00F 0.76(5) . ?
N00G C00R 1.338(7) . ?
N00G C00X 1.325(7) . ?
N00H C00W 1.332(7) . ?
N00H C13 1.339(8) . ?
N00H H00H 0.99(6) . ?
N00I C9 1.337(8) . ?
N00I C24 1.330(8) . ?
N00I H00I 0.86(5) . ?
C00J C00P 1.380(7) . ?
C00J C00W 1.459(8) . ?
N00K H00K 0.8600 . ?
N00K C14 1.351(7) . ?
N00K C21 1.333(7) . ?
C00L H00L 0.9300 . ?
C00L C9 1.388(8) . ?
C00L C18 1.398(9) . ?
C00M C00O 1.484(8) . ?
C00M C00V 1.366(7) . ?
C00O C5 1.387(7) . ?
C00P H00P 0.9300 . ?
C00P C00U 1.366(8) . ?
C00Q H00Q 0.9300 . ?
C00Q C7 1.352(9) . ?
C00Q C22 1.369(8) . ?
C00R C9 1.452(8) . ?
C00R C1 1.374(8) . ?
C00S H00S 0.9300 . ?
C00S C18 1.348(10) . ?
C00S C24 1.348(9) . ?
C00U H00U 0.9300 . ?
C00U C5 1.383(8) . ?
C00V H00V 0.9300 . ?
C00V C7 1.404(8) . ?
C00W C25 1.405(8) . ?
C00X C00Y 1.402(8) . ?
C00X C21 1.480(8) . ?
C00Y H00Y 0.9300 . ?
C00Y C8 1.370(9) . ?
C5 H5 0.9300 . ?
C7 H7 0.9300 . ?
C13 H13 0.9300 . ?
C13 C17 1.365(8) . ?
C14 H14 0.9300 . ?
C14 C28 1.361(9) . ?
C15 H15 0.9300 . ?
C15 C21 1.362(8) . ?
C15 C27 1.380(10) . ?
C17 H17 0.9300 . ?
C17 C32 1.377(9) . ?
C18 H18 0.9300 . ?
C22 H22 0.9300 . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C25 C32 1.375(9) . ?
C27 H27 0.9300 . ?
C27 C28 1.375(10) . ?
C28 H28 0.9300 . ?
C32 H32 0.9300 . ?
C1 H1 0.9300 . ?
C1 C8 1.364(8) . ?
C8 H8 0.9300 . ?

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
I005 Pb01 I005 180.0 . 2_767 ?
I005 Pb01 I009 82.928(11) . . ?
I005 Pb01 I009 97.073(11) 2_767 . ?
I005 Pb01 I009 97.072(11) . 2_767 ?
I005 Pb01 I009 82.928(11) 2_767 2_767 ?
I006 Pb01 I005 93.865(11) 2_767 2_767 ?
I006 Pb01 I005 93.866(11) . . ?
I006 Pb01 I005 86.135(11) . 2_767 ?
I006 Pb01 I005 86.134(11) 2_767 . ?
I006 Pb01 I006 180.0 2_767 . ?
I006 Pb01 I009 83.660(11) . 2_767 ?
I006 Pb01 I009 83.659(11) 2_767 . ?
I006 Pb01 I009 96.340(11) 2_767 2_767 ?
I006 Pb01 I009 96.341(11) . . ?
I009 Pb01 I009 180.0 2_767 . ?
I004 Pb02 I00A 81.587(13) . . ?
I004 Pb02 I00D 85.386(9) . . ?
I007 Pb02 I004 178.352(14) . . ?
I007 Pb02 I008 85.009(13) . . ?
I007 Pb02 I00A 96.765(13) . . ?
I007 Pb02 I00C 95.715(13) . . ?
I007 Pb02 I00D 94.920(10) . . ?
I008 Pb02 I004 96.622(13) . . ?
I008 Pb02 I00A 170.465(14) . . ?
I008 Pb02 I00C 89.468(13) . . ?
I008 Pb02 I00D 88.108(10) . . ?
I00A Pb02 I00D 101.039(11) . . ?
I00C Pb02 I004 84.079(13) . . ?
I00C Pb02 I00A 81.039(13) . . ?
I00C Pb02 I00D 168.844(12) . . ?
I004 Pb03 I005 90.254(12) . . ?
I004 Pb03 I006 174.075(13) . 2_767 ?
I004 Pb03 I009 92.829(13) . . ?
I004 Pb03 I00A 84.568(13) . . ?
I004 Pb03 I00C 85.885(13) . . ?
I006 Pb03 I005 85.108(12) 2_767 . ?
I006 Pb03 I009 82.934(12) 2_767 . ?
I009 Pb03 I005 82.624(12) . . ?
I00A Pb03 I005 174.358(13) . . ?
I00A Pb03 I006 100.201(13) . 2_767 ?
I00A Pb03 I009 99.832(14) . . ?
I00A Pb03 I00C 82.425(13) . . ?
I00C Pb03 I005 94.995(13) . . ?
I00C Pb03 I006 98.172(13) . 2_767 ?
I00C Pb03 I009 177.297(14) . . ?
Pb03 I004 Pb02 80.601(11) . . ?
Pb01 I005 Pb03 78.626(10) . . ?
Pb01 I006 Pb03 79.505(10) . 2_767 ?
Pb01 I009 Pb03 78.641(10) . . ?
Pb03 I00A Pb02 79.210(12) . . ?
Pb03 I00C Pb02 79.479(11) . . ?
Pb02 I00D Pb02 180.0 2_756 . ?
C00O N00E C00J 117.7(5) . . ?
C00M N00F H00F 122(5) . . ?
C22 N00F C00M 124.5(6) . . ?
C22 N00F H00F 113(5) . . ?
C00X N00G C00R 117.8(5) . . ?
C00W N00H C13 125.0(6) . . ?
C00W N00H H00H 123(4) . . ?
C13 N00H H00H 112(4) . . ?
C9 N00I H00I 118(3) . . ?
C24 N00I C9 124.6(7) . . ?
C24 N00I H00I 117(3) . . ?
N00E C00J C00P 123.1(6) . . ?
N00E C00J C00W 113.5(5) . . ?
C00P C00J C00W 123.4(6) . . ?
C14 N00K H00K 118.0 . . ?
C21 N00K H00K 118.0 . . ?
C21 N00K C14 124.1(6) . . ?
C9 C00L H00L 120.5 . . ?
C9 C00L C18 118.9(7) . . ?
C18 C00L H00L 120.5 . . ?
N00F C00M C00O 116.2(5) . . ?
N00F C00M C00V 118.0(6) . . ?
C00V C00M C00O 125.8(6) . . ?
N00E C00O C00M 114.7(5) . . ?
N00E C00O C5 122.8(6) . . ?
C5 C00O C00M 122.5(6) . . ?
C00J C00P H00P 120.9 . . ?
C00U C00P C00J 118.2(6) . . ?
C00U C00P H00P 120.9 . . ?
C7 C00Q H00Q 120.3 . . ?
C7 C00Q C22 119.5(6) . . ?
C22 C00Q H00Q 120.3 . . ?
N00G C00R C9 115.0(6) . . ?
N00G C00R C1 123.0(6) . . ?
C1 C00R C9 122.0(6) . . ?
C18 C00S H00S 121.0 . . ?
C18 C00S C24 118.1(7) . . ?
C24 C00S H00S 121.0 . . ?
C00P C00U H00U 119.8 . . ?
C00P C00U C5 120.4(6) . . ?
C5 C00U H00U 119.8 . . ?
C00M C00V H00V 120.6 . . ?
C00M C00V C7 118.9(6) . . ?
C7 C00V H00V 120.6 . . ?
N00H C00W C00J 116.3(5) . . ?
N00H C00W C25 117.2(6) . . ?
C25 C00W C00J 126.5(6) . . ?
N00G C00X C00Y 122.8(6) . . ?
N00G C00X C21 115.5(6) . . ?
C00Y C00X C21 121.7(6) . . ?
C00X C00Y H00Y 121.2 . . ?
C8 C00Y C00X 117.6(6) . . ?
C8 C00Y H00Y 121.2 . . ?
C00O C5 H5 121.1 . . ?
C00U C5 C00O 117.9(6) . . ?
C00U C5 H5 121.1 . . ?
C00Q C7 C00V 120.2(6) . . ?
C00Q C7 H7 119.9 . . ?
C00V C7 H7 119.9 . . ?
N00I C9 C00L 116.4(6) . . ?
N00I C9 C00R 118.2(6) . . ?
C00L C9 C00R 125.5(6) . . ?
N00H C13 H13 120.6 . . ?
N00H C13 C17 118.7(7) . . ?
C17 C13 H13 120.6 . . ?
N00K C14 H14 121.2 . . ?
N00K C14 C28 117.7(7) . . ?
C28 C14 H14 121.2 . . ?
C21 C15 H15 120.2 . . ?
C21 C15 C27 119.7(8) . . ?
C27 C15 H15 120.2 . . ?
C13 C17 H17 120.3 . . ?
C13 C17 C32 119.3(7) . . ?
C32 C17 H17 120.3 . . ?
C00L C18 H18 119.2 . . ?
C00S C18 C00L 121.5(7) . . ?
C00S C18 H18 119.2 . . ?
N00K C21 C00X 117.4(5) . . ?
N00K C21 C15 118.6(7) . . ?
C15 C21 C00X 124.0(7) . . ?
N00F C22 C00Q 118.8(6) . . ?
N00F C22 H22 120.6 . . ?
C00Q C22 H22 120.6 . . ?
N00I C24 C00S 120.5(8) . . ?
N00I C24 H24 119.7 . . ?
C00S C24 H24 119.7 . . ?
C00W C25 H25 120.4 . . ?
C32 C25 C00W 119.2(7) . . ?
C32 C25 H25 120.4 . . ?
C15 C27 H27 120.3 . . ?
C28 C27 C15 119.5(7) . . ?
C28 C27 H27 120.3 . . ?
C14 C28 C27 120.4(7) . . ?
C14 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C17 C32 H32 119.7 . . ?
C25 C32 C17 120.6(7) . . ?
C25 C32 H32 119.7 . . ?
C00R C1 H1 120.7 . . ?
C8 C1 C00R 118.7(7) . . ?
C8 C1 H1 120.7 . . ?
C00Y C8 H8 120.0 . . ?
C1 C8 C00Y 120.0(7) . . ?
C1 C8 H8 120.0 . . ?

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
N00E C00J C00P C00U 1.6(10) . . . . ?
N00E C00J C00W N00H -15.0(8) . . . . ?
N00E C00J C00W C25 164.0(6) . . . . ?
N00E C00O C5 C00U 2.0(10) . . . . ?
N00F C00M C00O N00E -13.6(8) . . . . ?
N00F C00M C00O C5 165.2(6) . . . . ?
N00F C00M C00V C7 0.0(10) . . . . ?
N00G C00R C9 N00I -14.9(9) . . . . ?
N00G C00R C9 C00L 165.9(6) . . . . ?
N00G C00R C1 C8 -1.8(11) . . . . ?
N00G C00X C00Y C8 0.8(10) . . . . ?
N00G C00X C21 N00K 13.7(9) . . . . ?
N00G C00X C21 C15 -166.9(7) . . . . ?
N00H C00W C25 C32 -1.3(10) . . . . ?
N00H C13 C17 C32 -0.5(12) . . . . ?
C00J N00E C00O C00M 177.0(5) . . . . ?
C00J N00E C00O C5 -1.8(9) . . . . ?
C00J C00P C00U C5 -1.4(10) . . . . ?
C00J C00W C25 C32 179.8(6) . . . . ?
N00K C14 C28 C27 -0.2(13) . . . . ?
C00M N00F C22 C00Q 0.4(10) . . . . ?
C00M C00O C5 C00U -176.7(6) . . . . ?
C00M C00V C7 C00Q -0.2(11) . . . . ?
C00O N00E C00J C00P -0.1(9) . . . . ?
C00O N00E C00J C00W 177.1(5) . . . . ?
C00O C00M C00V C7 177.6(6) . . . . ?
C00P C00J C00W N00H 162.2(6) . . . . ?
C00P C00J C00W C25 -18.9(10) . . . . ?
C00P C00U C5 C00O -0.3(10) . . . . ?
C00R N00G C00X C00Y -0.2(9) . . . . ?
C00R N00G C00X C21 -179.3(5) . . . . ?
C00R C1 C8 C00Y 2.3(11) . . . . ?
C00V C00M C00O N00E 168.7(6) . . . . ?
C00V C00M C00O C5 -12.6(10) . . . . ?
C00W N00H C13 C17 -0.3(12) . . . . ?
C00W C00J C00P C00U -175.3(6) . . . . ?
C00W C25 C32 C17 0.5(11) . . . . ?
C00X N00G C00R C9 -179.0(5) . . . . ?
C00X N00G C00R C1 0.7(9) . . . . ?
C00X C00Y C8 C1 -1.9(11) . . . . ?
C00Y C00X C21 N00K -165.4(6) . . . . ?
C00Y C00X C21 C15 14.0(10) . . . . ?
C7 C00Q C22 N00F -0.7(11) . . . . ?
C9 N00I C24 C00S 1.4(14) . . . . ?
C9 C00L C18 C00S -0.9(12) . . . . ?
C9 C00R C1 C8 177.9(6) . . . . ?
C13 N00H C00W C00J -179.7(6) . . . . ?
C13 N00H C00W C25 1.2(10) . . . . ?
C13 C17 C32 C25 0.4(12) . . . . ?
C14 N00K C21 C00X -179.5(6) . . . . ?
C14 N00K C21 C15 1.1(11) . . . . ?
C15 C27 C28 C14 -1.6(15) . . . . ?
C18 C00L C9 N00I 0.9(10) . . . . ?
C18 C00L C9 C00R -179.9(6) . . . . ?
C18 C00S C24 N00I -1.2(14) . . . . ?
C21 N00K C14 C28 0.5(11) . . . . ?
C21 C00X C00Y C8 179.9(6) . . . . ?
C21 C15 C27 C28 3.2(14) . . . . ?
C22 N00F C00M C00O -178.0(6) . . . . ?
C22 N00F C00M C00V -0.1(10) . . . . ?
C22 C00Q C7 C00V 0.6(11) . . . . ?
C24 N00I C9 C00L -1.2(12) . . . . ?
C24 N00I C9 C00R 179.5(8) . . . . ?
C24 C00S C18 C00L 1.0(13) . . . . ?
C27 C15 C21 N00K -2.9(12) . . . . ?
C27 C15 C21 C00X 177.7(8) . . . . ?
C1 C00R C9 N00I 165.4(7) . . . . ?
C1 C00R C9 C00L -13.8(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.831
_oxdiff_exptl_absorpt_empirical_full_min 0.687
