# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_v-4-66-cu-ac_auto
_database_code_depnum_ccdc_archive 'CCDC 2244486'
loop_
_audit_author_name
_audit_author_address
'Xinsong Lin'
;Florida State University
United States of America
;
_audit_update_record             
;
2023-02-24 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;
_audit_creation_date             2023-02-24
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl11 Pb3, H2 O, C8 H28 N5'
_chemical_formula_sum            'C8 H30 Cl11 N5 O Pb3'
_chemical_formula_weight         1223.89
_chemical_melting_point          ?
_chemical_oxdiff_formula         C8H30Cl11N5OPb3
_chemical_oxdiff_usercomment     150K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 '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           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   11.36620(10)
_cell_length_b                   15.87190(10)
_cell_length_c                   32.1657(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5802.80(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    112230
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      77.3160
_cell_measurement_theta_min      3.8500
_shelx_estimated_absorpt_T_max   0.174
_shelx_estimated_absorpt_T_min   0.041
_exptl_absorpt_coefficient_mu    42.731
_exptl_absorpt_correction_T_max  0.292
_exptl_absorpt_correction_T_min  0.016
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.802
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4432
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0354
0 1 0 0.0334
0 0 -1 0.0343
0 0 1 0.0283
-1 0 0 0.1047
1 0 0 0.1047
-2 0 -5 0.0731
2 0 -5 0.0818

_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.063
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0000 -0.9993 0.0000 -0.0019 -0.0177 0.0955
-0.0000 0.9993 -0.0000 0.0019 0.0177 -0.0955
0.0001 -0.0001 -0.9993 -0.0105 0.0460 0.0083
-0.0001 0.0001 0.9993 0.0105 -0.0460 -0.0083
-0.9992 0.0001 -0.0009 0.1322 0.0288 0.0079
0.9992 -0.0001 0.0009 -0.1322 -0.0288 -0.0079
-1.9977 -0.0001 -4.9983 0.2118 0.2876 0.0573
1.9990 -0.0005 -4.9946 -0.3170 0.1723 0.0257

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            70033
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.237
_diffrn_reflns_theta_min         4.764
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -120.00 -76.00   0.50    0.33    --  -48.09-143.00 -15.00   88
  2  ω     67.00  96.00   0.50    0.33    --   48.09-127.00 154.00   58
  3  ω     37.00  74.00   0.50    1.32    --  107.75-127.00 154.00   74
  4  ω    103.00 178.00   0.50    1.32    --  107.75  14.00 170.00  150
  5  ω    130.00 156.00   0.50    1.32    --  107.75 114.00 -31.00   52
  6  ω      1.00  26.00   0.50    0.33    --  -48.09  19.00-180.00   50
  7  ω    -17.00  18.00   0.50    0.33    --  -48.09  37.00-150.00   70
  8  ω   -119.00 -85.00   0.50    0.33    --  -48.09 -57.00 150.00   68
  9  ω    -17.00  25.00   0.50    0.33    --  -48.09  37.00-120.00   84
 10  ω     35.00 105.00   0.50    1.32    --  107.75 -94.00-150.00  140
 11  ω     67.00 125.00   0.50    1.32    --  107.75-143.00 -15.00  116
 12  ω     40.00  66.00   0.50    1.32    --  107.75 -45.00-150.00   52
 13  ω     39.00  70.00   0.50    1.32    --  107.75 -45.00 150.00   62
 14  ω     36.00  70.00   0.50    1.32    --  107.75 -45.00  60.00   68
 15  ω     41.00  93.00   0.50    1.32    --  107.75-125.00 -60.00  104
 16  ω     35.00  98.00   0.50    1.32    --  107.75 -94.00-180.00  126
 17  ω     43.00  69.00   0.50    1.32    --  107.75 -45.00  90.00   52
 18  ω     36.00  63.00   0.50    1.32    --  107.75 -45.00  30.00   54
 19  ω     70.00 103.00   0.50    1.32    --  107.75 -94.00-120.00   66
 20  ω    -44.00   9.00   0.50    0.33    --  -48.09  57.00  30.00  106
 21  ω   -115.00 -82.00   0.50    0.33    --  -48.09 -57.00-120.00   66
 22  ω     57.00  94.00   0.50    0.33    --   48.09-125.00 -90.00   74
 23  ω     35.00  87.00   0.50    0.33    --   48.09  56.00 -80.98  104
 24  ω     34.00  61.00   0.50    0.33    --   48.09  56.00  89.65   54
 25  ω     93.00 119.00   0.50    0.33    --   48.09  56.00  67.02   52
 26  ω     76.00 118.00   0.50    0.33    --   48.09  19.00-120.00   84
 27  ω     34.00  67.00   0.50    0.33    --   48.09  54.00 150.52   66
 28  ω     38.00  72.00   0.50    0.33    --   48.09  19.00-120.00   68
 29  ω     91.00 120.00   0.50    0.33    --   48.09  56.00-153.39   58
 30  ω     34.00  65.00   0.50    0.33    --   48.09  56.00  42.44   62
 31  ω     78.00 121.00   0.50    0.33    --   48.09  55.00 173.90   86
 32  ω     76.00 121.00   0.50    0.33    --   48.09  56.00 -23.03   90
 33  ω     36.00 119.00   0.50    0.33    --   48.09  19.00 120.00  166
 34  ω     78.00 104.00   0.50    0.33    --   48.09  56.00-126.75   52
 35  ω     34.00  65.00   0.50    0.33    --   48.09  55.00 173.90   62
 36  ω     34.00  60.00   0.50    0.33    --   48.09  56.00-105.07   52
 37  ω     34.00  75.00   0.50    0.33    --   48.09  56.00 -44.50   82
 38  ω     36.00  63.00   0.50    0.33    --   48.09  56.00 108.32   54
 39  ω     83.00 119.00   0.50    0.33    --   48.09  56.00  15.70   72
 40  ω     34.00  60.00   0.50    0.33    --   48.09  56.00  15.70   52
 41  ω     34.00  63.00   0.50    0.33    --   48.09  56.00-153.39   58
 42  ω     35.00  72.00   0.50    0.33    --   48.09  56.00 -23.03   74
 43  ω     34.00  60.00   0.50    0.33    --   48.09  56.00-126.75   52
 44  ω     35.00  61.00   0.50    0.33    --   48.09  56.00  67.02   52
 45  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -51.00   2.66   52
 46  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00-155.04   52
 47  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00-177.70   52
 48  ω   -113.00 -72.00   0.50    1.32    --  -86.25 -55.00  18.37   82
 49  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -53.00-126.31   52
 50  ω   -120.00 -72.00   0.50    1.32    --  -86.25 -55.00 -70.28   96
 51  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00 -91.63   52
 52  ω    -98.00 -73.00   0.50    1.32    --  -86.25 -50.00  47.07   50
 53  ω   -102.00 -72.00   0.50    1.32    --  -86.25 -51.00 -46.74   60
 54  ω    -97.00 -72.00   0.50    1.32    --  -86.25 -55.00  65.58   50
 55  ω    -97.00 -72.00   0.50    1.32    --  -86.25 -54.00 127.00   50
 56  ω    -97.00 -72.00   0.50    1.32    --  -86.25 -53.00  -9.08   50
 57  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -54.00  75.24   52
 58  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00 105.93   52
 59  ω    -97.00 -72.00   0.50    1.32    --  -86.25 -55.00  87.41   50
 60  ω    -97.00 -72.00   0.50    1.32    --  -86.25 -54.00-115.67   50
 61  ω   -100.00 -74.00   0.50    1.32    --  -86.25 -53.00  29.93   52
 62  ω    -49.00 -23.00   0.50    1.32    --  -86.25  61.00  60.00   52
 63  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -54.00 143.76   52
 64  ω    -97.00 -72.00   0.50    1.32    --  -86.25 -53.00 155.20   50
 65  ω   -149.00-123.00   0.50    1.32    --  -86.25 -55.00 -29.99   52
 66  ω    -99.00 -73.00   0.50    1.32    --  -86.25 -53.00 -52.00   52
 67  ω    -97.00 -72.00   0.50    1.32    --  -86.25 -53.00-146.94   50
 68  ω   -135.00-109.00   0.50    1.32    --  -86.25 -53.00 155.20   52
 69  ω    -97.00 -72.00   0.50    1.32    --  -86.25 -55.00-102.97   50
 70  ω   -159.00-132.00   0.50    1.32    --  -86.25 -55.00-177.70   54
 71  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -53.00  39.96   52
 72  ω    -97.00 -72.00   0.50    1.32    --  -86.25 -54.00-170.76   50
 73  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00 119.61   52
 74  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -51.00 -25.02   52
 75  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -53.00-133.07   52
 76  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00 168.61   52
 77  ω    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00 -83.34   52
 78  ω    -99.00 -72.00   0.50    1.32    --  -86.25 -55.00 -29.99   54
 79  ω     77.00 104.00   0.50    1.32    --  107.75 -94.00  60.00   54
 80  ω     37.00  72.00   0.50    1.32    --  107.75 -94.00  60.00   70
 81  ω    125.00 158.00   0.50    1.32    --  107.75  61.00-120.00   66
 82  ω     91.00 120.00   0.50    1.32    --  107.75  61.00-120.00   58
 83  ω    131.00 163.00   0.50    1.32    --  107.75  45.00-180.00   64
 84  ω     96.00 121.00   0.50    1.32    --  107.75  45.00-180.00   50
 85  ω     36.00 105.00   0.50    1.32    --  107.75 -94.00 150.00  138
 86  ω    128.00 177.00   0.50    1.32    --  107.75  61.00 150.00   98
 87  ω     91.00 123.00   0.50    1.32    --  107.75  61.00 150.00   64
 88  ω    127.00 153.00   0.50    1.32    --  107.75  61.00   0.00   52
 89  ω     39.00  68.00   0.50    1.32    --  107.75-125.00  30.00   58
 90  ω     91.00 121.00   0.50    1.32    --  107.75  61.00   0.00   60
 91  ω     91.00 165.00   0.50    1.32    --  107.75  61.00 -90.00  148
 92  ω    100.00 157.00   0.50    1.32    --  107.75  45.00-150.00  114
 93  ω     96.00 122.00   0.50    1.32    --  107.75  45.00 120.00   52
 94  ω    142.00 168.00   0.50    1.32    --  107.75  45.00  90.00   52
 95  ω     44.00 106.00   0.50    1.32    --  107.75 -94.00 120.00  124
 96  ω     96.00 123.00   0.50    1.32    --  107.75  45.00  90.00   54
 97  ω     91.00 119.00   0.50    1.32    --  107.75  61.00 120.00   56
 98  ω    128.00 178.00   0.50    1.32    --  107.75  61.00  60.00  100
 99  ω     91.00 122.00   0.50    1.32    --  107.75  61.00  60.00   62
100  ω    100.00 154.00   0.50    1.32    --  107.75  45.00-120.00  108
101  ω     46.00  71.00   0.50    1.32    --  107.75 -45.00-180.00   50
102  ω     97.00 148.00   0.50    1.32    --  107.75  45.00 -90.00  102
103  ω     80.00 106.00   0.50    1.32    --  107.75 -94.00  90.00   52
104  ω    127.00 153.00   0.50    1.32    --  107.75  45.00 -30.00   52
105  ω     97.00 126.00   0.50    1.32    --  107.75  45.00 -30.00   58
106  ω     44.00  74.00   0.50    1.32    --  107.75 -94.00  90.00   60
107  ω    101.00 153.00   0.50    1.32    --  107.75  45.00  60.00  104
108  ω     40.00  68.00   0.50    1.32    --  107.75-125.00   0.00   56
109  ω     87.00 112.00   0.50    1.32    --  107.75-125.00   0.00   50
110  ω     81.00 107.00   0.50    1.32    --  107.75-102.00-113.87   52
111  ω     38.00  72.00   0.50    1.32    --  107.75-102.00-113.87   68
112  ω     36.00  61.00   0.50    1.32    --  107.75 -45.00-120.00   50
113  ω     37.00 107.00   0.50    1.32    --  107.75-102.00  51.24  140
114  ω     76.00 106.00   0.50    1.32    --  107.75 -94.00   0.00   60
115  ω     35.00  73.00   0.50    1.32    --  107.75 -94.00   0.00   76
116  ω     95.00 178.00   0.50    1.32    --  107.75  58.00 -11.19  166
117  ω    128.00 176.00   0.50    1.32    --  107.75  61.00-150.00   96
118  ω     91.00 117.00   0.50    1.32    --  107.75  61.00-150.00   52
119  ω    124.00 162.00   0.50    1.32    --  107.75  56.00  26.52   76
120  ω    128.00 154.00   0.50    1.32    --  107.75  45.00 120.00   52
121  ω     96.00 155.00   0.50    1.32    --  107.75  45.00 150.00  118
122  ω    149.00 177.00   0.50    1.32    --  107.75  61.00-180.00   56
123  ω     91.00 120.00   0.50    1.32    --  107.75  61.00-180.00   58
124  ω     93.00 120.00   0.50    1.32    --  107.75  56.00  26.52   54
125  ω     84.00 111.00   0.50    1.32    --  107.75-125.00  30.00   54
126  ω    132.00 165.00   0.50    1.32    --  107.75  61.00 -30.00   66
127  ω     91.00 124.00   0.50    1.32    --  107.75  61.00 -30.00   66
128  ω     48.00  93.00   0.50    1.32    --  107.75 -61.00 -30.00   90
129  ω     70.00 106.00   0.50    1.32    --  107.75 -94.00 -60.00   72
130  ω    143.00 175.00   0.50    1.32    --  107.75  62.00 -77.09   64
131  ω    129.00 177.00   0.50    1.32    --  107.75  61.00  30.00   96
132  ω     92.00 121.00   0.50    1.32    --  107.75  61.00  30.00   58
133  ω     92.00 137.00   0.50    1.32    --  107.75  62.00 -77.09   90
134  ω    145.00 175.00   0.50    1.32    --  107.75  61.00  90.00   60
135  ω     91.00 140.00   0.50    1.32    --  107.75  61.00  90.00   98
136  ω     91.00 178.00   0.50    1.32    --  107.75  61.00 -60.00  174
137  ω     59.00  90.00   0.50    1.32    --  107.75 -61.00 -90.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1323197000
_diffrn_orient_matrix_UB_12      0.0018639000
_diffrn_orient_matrix_UB_13      0.0105034000
_diffrn_orient_matrix_UB_21      -0.0287951000
_diffrn_orient_matrix_UB_22      0.0176804000
_diffrn_orient_matrix_UB_23      -0.0460215000
_diffrn_orient_matrix_UB_31      -0.0079276000
_diffrn_orient_matrix_UB_32      -0.0955243000
_diffrn_orient_matrix_UB_33      -0.0083009000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5555
_reflns_number_total             6022
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.508
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       0.000047(2)
_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   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         6022
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0317
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0426P)²+23.1008P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0956
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, {H1A,H1B,H1C} of N1, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups, {H5A,H5B,H5C} of N5
2. Restrained distances
 H1G-H1B
 2.1 with sigma of 0.02
3.a Free rotating group:
 O1(H1F,H1G)
3.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), C1(H1D,H1E), C2(H2C,H2D), C3(H3C,H3D),
 C4(H4C,H4D), C5(H5D,H5E), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
3.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N5(H5A,H5B,H5C)
;
_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 0.51666(2) 0.65544(2) 0.74896(2) 0.02438(9) Uani 1 1 d . . . . .
Pb2 Pb 0.50984(2) 0.65918(2) 0.61649(2) 0.02807(9) Uani 1 1 d . . . . .
Pb3 Pb 0.00802(2) 0.65729(2) 0.61902(2) 0.02601(9) Uani 1 1 d . . . . .
Cl1 Cl 0.51211(11) 0.52109(8) 0.81259(4) 0.0308(3) Uani 1 1 d . . . . .
Cl2 Cl 0.53462(12) 0.78072(8) 0.81115(4) 0.0310(3) Uani 1 1 d . . . . .
Cl3 Cl 0.76474(16) 0.65590(11) 0.74645(7) 0.0704(8) Uani 1 1 d . . . . .
Cl4 Cl 0.53676(13) 0.53212(8) 0.68330(4) 0.0323(3) Uani 1 1 d . . . . .
Cl5 Cl 0.50853(11) 0.78927(9) 0.68894(4) 0.0316(3) Uani 1 1 d . . . . .
Cl6 Cl 0.75664(11) 0.67085(10) 0.60282(6) 0.0492(4) Uani 1 1 d . . . . .
Cl7 Cl 0.51012(14) 0.53000(11) 0.56165(5) 0.0539(4) Uani 1 1 d . . . . .
Cl8 Cl 0.50090(15) 0.78649(11) 0.55684(6) 0.0608(5) Uani 1 1 d . . . . .
Cl9 Cl 0.25645(11) 0.64951(9) 0.61248(5) 0.0350(3) Uani 1 1 d . . . . .
Cl10 Cl 0.02279(12) 0.55159(9) 0.55210(4) 0.0393(3) Uani 1 1 d . . . . .
Cl11 Cl 0.02745(12) 0.79861(8) 0.57019(4) 0.0395(3) Uani 1 1 d . . . . .
O1 O 0.7886(6) 0.8706(3) 1.00292(17) 0.0703(15) Uani 1 1 d G . . . .
H1F H 0.766749 0.872547 1.028828 0.105 Uiso 1 1 d G U . . .
H1G H 0.853284 0.899818 1.002130 0.105 Uiso 1 1 d DG U . . .
N1 N 0.7448(4) 0.9392(3) 0.92088(14) 0.0384(10) Uani 1 1 d . . . . .
H1A H 0.776141 0.991899 0.920164 0.046 Uiso 1 1 calc R U . . .
H1B H 0.770869 0.911717 0.943944 0.046 Uiso 1 1 calc DR U . . .
H1C H 0.664899 0.942801 0.921653 0.046 Uiso 1 1 calc R U . . .
N2 N 0.7625(3) 0.8871(3) 0.80686(13) 0.0253(8) Uani 1 1 d . . . . .
H2A H 0.729427 0.834870 0.807207 0.030 Uiso 1 1 calc R U . . .
H2B H 0.842068 0.880539 0.806675 0.030 Uiso 1 1 calc R U . . .
N3 N 0.7349(3) 0.9279(3) 0.69156(12) 0.0259(8) Uani 1 1 d . . . . .
H3A H 0.655745 0.936362 0.691649 0.031 Uiso 1 1 calc R U . . .
H3B H 0.770642 0.979195 0.690693 0.031 Uiso 1 1 calc R U . . .
N4 N 0.7662(4) 0.8733(3) 0.57796(13) 0.0311(9) Uani 1 1 d . . . . .
H4A H 0.730140 0.822143 0.578698 0.037 Uiso 1 1 calc R U . . .
H4B H 0.845179 0.864543 0.579650 0.037 Uiso 1 1 calc R U . . .
N5 N 0.7194(6) 0.7990(5) 0.4873(2) 0.0730(19) Uani 1 1 d . . . . .
H5A H 0.643301 0.806119 0.495357 0.110 Uiso 1 1 calc R U . . .
H5B H 0.748265 0.750693 0.498622 0.110 Uiso 1 1 calc R U . . .
H5C H 0.723044 0.795719 0.459108 0.110 Uiso 1 1 calc R U . . .
C1 C 0.7816(5) 0.8916(3) 0.88285(15) 0.0322(10) Uani 1 1 d . . . . .
H1D H 0.754854 0.832377 0.884760 0.039 Uiso 1 1 calc R U . . .
H1E H 0.868449 0.891859 0.880394 0.039 Uiso 1 1 calc R U . . .
C2 C 0.7272(4) 0.9336(3) 0.84531(14) 0.0281(10) Uani 1 1 d . . . . .
H2C H 0.640443 0.933518 0.847958 0.034 Uiso 1 1 calc R U . . .
H2D H 0.754071 0.992798 0.843531 0.034 Uiso 1 1 calc R U . . .
C3 C 0.7255(4) 0.9321(3) 0.76818(14) 0.0262(9) Uani 1 1 d . . . . .
H3C H 0.758542 0.989770 0.767936 0.031 Uiso 1 1 calc R U . . .
H3D H 0.638650 0.936322 0.767131 0.031 Uiso 1 1 calc R U . . .
C4 C 0.7703(4) 0.8828(3) 0.73070(15) 0.0282(10) Uani 1 1 d . . . . .
H4C H 0.857092 0.877917 0.732005 0.034 Uiso 1 1 calc R U . . .
H4D H 0.736593 0.825292 0.730846 0.034 Uiso 1 1 calc R U . . .
C5 C 0.7685(4) 0.8782(3) 0.65380(15) 0.0282(10) Uani 1 1 d . . . . .
H5D H 0.732001 0.821645 0.655078 0.034 Uiso 1 1 calc R U . . .
H5E H 0.855020 0.870934 0.652954 0.034 Uiso 1 1 calc R U . . .
C6 C 0.7273(5) 0.9240(3) 0.61459(15) 0.0314(10) Uani 1 1 d . . . . .
H6A H 0.640575 0.929559 0.614683 0.038 Uiso 1 1 calc R U . . .
H6B H 0.762142 0.981145 0.613404 0.038 Uiso 1 1 calc R U . . .
C7 C 0.7386(5) 0.9154(3) 0.53753(16) 0.0366(12) Uani 1 1 d . . . . .
H7A H 0.772362 0.972921 0.537625 0.044 Uiso 1 1 calc R U . . .
H7B H 0.652221 0.920672 0.534610 0.044 Uiso 1 1 calc R U . . .
C8 C 0.7866(8) 0.8675(5) 0.5010(2) 0.063(2) Uani 1 1 d . . . . .
H8A H 0.795727 0.907296 0.477486 0.075 Uiso 1 1 calc R U . . .
H8B H 0.866010 0.846732 0.508316 0.075 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 Cl1 2.9562(13) . ?
Pb1 Cl2 2.8280(12) . ?
Pb1 Cl3 2.8672(18) 6_557 ?
Pb1 Cl3 2.8209(18) . ?
Pb1 Cl4 2.8886(12) . ?
Pb1 Cl5 2.8720(13) . ?
Pb2 Cl4 2.9629(12) . ?
Pb2 Cl6 2.8455(13) . ?
Pb2 Cl7 2.7048(15) . ?
Pb2 Cl8 2.7881(16) . ?
Pb2 Cl9 2.8870(13) . ?
Pb3 Cl1 3.0843(13) 6_557 ?
Pb3 Cl2 2.9955(12) 6_557 ?
Pb3 Cl6 2.9123(14) 1_455 ?
Pb3 Cl9 2.8342(13) . ?
Pb3 Cl10 2.7342(13) . ?
Pb3 Cl11 2.7472(12) . ?
O1 H1F 0.8700 . ?
O1 H1G 0.8700 . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.497(6) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 C2 1.495(6) . ?
N2 C3 1.495(6) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 C4 1.503(6) . ?
N3 C5 1.498(6) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 C6 1.494(6) . ?
N4 C7 1.495(6) . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 H5C 0.9100 . ?
N5 C8 1.399(11) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C1 C2 1.512(7) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C3 C4 1.525(7) . ?
C4 H4C 0.9900 . ?
C4 H4D 0.9900 . ?
C5 H5D 0.9900 . ?
C5 H5E 0.9900 . ?
C5 C6 1.529(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.502(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?

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
Cl2 Pb1 Cl1 91.07(4) . . ?
Cl2 Pb1 Cl3 91.94(4) . 6_557 ?
Cl2 Pb1 Cl4 171.09(5) . . ?
Cl2 Pb1 Cl5 87.58(4) . . ?
Cl3 Pb1 Cl1 92.24(4) . . ?
Cl3 Pb1 Cl1 87.06(5) 6_557 . ?
Cl3 Pb1 Cl2 86.92(6) . . ?
Cl3 Pb1 Cl3 178.655(19) . 6_557 ?
Cl3 Pb1 Cl4 84.36(6) . . ?
Cl3 Pb1 Cl4 96.80(5) 6_557 . ?
Cl3 Pb1 Cl5 90.03(5) 6_557 . ?
Cl3 Pb1 Cl5 90.63(4) . . ?
Cl4 Pb1 Cl1 91.08(4) . . ?
Cl5 Pb1 Cl1 176.75(4) . . ?
Cl5 Pb1 Cl4 90.70(4) . . ?
Cl6 Pb2 Cl4 93.13(5) . . ?
Cl6 Pb2 Cl9 168.53(6) . . ?
Cl7 Pb2 Cl4 87.53(5) . . ?
Cl7 Pb2 Cl6 86.99(5) . . ?
Cl7 Pb2 Cl8 95.78(6) . . ?
Cl7 Pb2 Cl9 86.09(4) . . ?
Cl8 Pb2 Cl4 174.94(5) . . ?
Cl8 Pb2 Cl6 83.25(5) . . ?
Cl8 Pb2 Cl9 88.36(5) . . ?
Cl9 Pb2 Cl4 95.70(4) . . ?
Cl2 Pb3 Cl1 85.54(3) 6_557 6_557 ?
Cl6 Pb3 Cl1 101.20(4) 1_455 6_557 ?
Cl6 Pb3 Cl2 100.65(4) 1_455 6_557 ?
Cl9 Pb3 Cl1 90.43(4) . 6_557 ?
Cl9 Pb3 Cl2 89.06(4) . 6_557 ?
Cl9 Pb3 Cl6 165.32(6) . 1_455 ?
Cl10 Pb3 Cl1 97.50(4) . 6_557 ?
Cl10 Pb3 Cl2 170.16(4) . 6_557 ?
Cl10 Pb3 Cl6 87.98(5) . 1_455 ?
Cl10 Pb3 Cl9 81.58(4) . . ?
Cl10 Pb3 Cl11 92.63(4) . . ?
Cl11 Pb3 Cl1 168.17(4) . 6_557 ?
Cl11 Pb3 Cl2 83.49(4) . 6_557 ?
Cl11 Pb3 Cl6 85.19(5) . 1_455 ?
Cl11 Pb3 Cl9 85.01(4) . . ?
Pb1 Cl1 Pb3 89.34(4) . 6_657 ?
Pb1 Cl2 Pb3 93.62(4) . 6_657 ?
Pb1 Cl3 Pb1 175.41(9) . 6_657 ?
Pb1 Cl4 Pb2 93.49(4) . . ?
Pb2 Cl6 Pb3 159.18(8) . 1_655 ?
Pb3 Cl9 Pb2 171.21(6) . . ?
H1F O1 H1G 104.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H2A N2 H2B 107.9 . . ?
C2 N2 H2A 109.2 . . ?
C2 N2 H2B 109.2 . . ?
C2 N2 C3 112.2(4) . . ?
C3 N2 H2A 109.2 . . ?
C3 N2 H2B 109.2 . . ?
H3A N3 H3B 108.0 . . ?
C4 N3 H3A 109.4 . . ?
C4 N3 H3B 109.4 . . ?
C5 N3 H3A 109.4 . . ?
C5 N3 H3B 109.4 . . ?
C5 N3 C4 111.1(4) . . ?
H4A N4 H4B 107.8 . . ?
C6 N4 H4A 109.1 . . ?
C6 N4 H4B 109.1 . . ?
C6 N4 C7 112.5(4) . . ?
C7 N4 H4A 109.1 . . ?
C7 N4 H4B 109.1 . . ?
H5A N5 H5B 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C8 N5 H5A 109.5 . . ?
C8 N5 H5B 109.5 . . ?
C8 N5 H5C 109.5 . . ?
N1 C1 H1D 110.0 . . ?
N1 C1 H1E 110.0 . . ?
N1 C1 C2 108.4(4) . . ?
H1D C1 H1E 108.4 . . ?
C2 C1 H1D 110.0 . . ?
C2 C1 H1E 110.0 . . ?
N2 C2 C1 109.5(4) . . ?
N2 C2 H2C 109.8 . . ?
N2 C2 H2D 109.8 . . ?
C1 C2 H2C 109.8 . . ?
C1 C2 H2D 109.8 . . ?
H2C C2 H2D 108.2 . . ?
N2 C3 H3C 110.0 . . ?
N2 C3 H3D 110.0 . . ?
N2 C3 C4 108.6(4) . . ?
H3C C3 H3D 108.4 . . ?
C4 C3 H3C 110.0 . . ?
C4 C3 H3D 110.0 . . ?
N3 C4 C3 109.2(4) . . ?
N3 C4 H4C 109.8 . . ?
N3 C4 H4D 109.8 . . ?
C3 C4 H4C 109.8 . . ?
C3 C4 H4D 109.8 . . ?
H4C C4 H4D 108.3 . . ?
N3 C5 H5D 109.7 . . ?
N3 C5 H5E 109.7 . . ?
N3 C5 C6 109.9(4) . . ?
H5D C5 H5E 108.2 . . ?
C6 C5 H5D 109.7 . . ?
C6 C5 H5E 109.7 . . ?
N4 C6 C5 107.7(4) . . ?
N4 C6 H6A 110.2 . . ?
N4 C6 H6B 110.2 . . ?
C5 C6 H6A 110.2 . . ?
C5 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
N4 C7 H7A 109.2 . . ?
N4 C7 H7B 109.2 . . ?
N4 C7 C8 112.2(4) . . ?
H7A C7 H7B 107.9 . . ?
C8 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
N5 C8 C7 116.2(7) . . ?
N5 C8 H8A 108.2 . . ?
N5 C8 H8B 108.2 . . ?
C7 C8 H8A 108.2 . . ?
C7 C8 H8B 108.2 . . ?
H8A C8 H8B 107.4 . . ?

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
N1 C1 C2 N2 -179.9(4) . . . . ?
N2 C3 C4 N3 -179.3(3) . . . . ?
N3 C5 C6 N4 178.3(4) . . . . ?
N4 C7 C8 N5 81.2(7) . . . . ?
C2 N2 C3 C4 177.1(4) . . . . ?
C3 N2 C2 C1 -172.1(4) . . . . ?
C4 N3 C5 C6 177.9(4) . . . . ?
C5 N3 C4 C3 -175.4(4) . . . . ?
C6 N4 C7 C8 175.4(5) . . . . ?
C7 N4 C6 C5 -175.7(4) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.808
_oxdiff_exptl_absorpt_empirical_full_min 0.676
