# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# 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_10248
_database_code_depnum_ccdc_archive 'CCDC 1533510'
_audit_update_record             
;
2017-02-18 deposited with the CCDC.
2017-04-06 downloaded from the CCDC.
;
_audit_creation_date             2016-08-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C20 H22 N4 O16 Pb4, 2(H2 O)'
_chemical_formula_sum            'C20 H28 N4 O18 Pb4'
_chemical_formula_weight         1441.22
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z'
4 '-x, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x-1/2, y, -z-1/2'
7 '-x-1/2, y-1/2, z'
8 'x, -y-1/2, z-1/2'

_cell_length_a                   19.1011(5)
_cell_length_b                   9.06660(19)
_cell_length_c                   32.4789(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5624.8(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3847
_cell_measurement_temperature    175.6(8)
_cell_measurement_theta_max      27.2550
_cell_measurement_theta_min      3.6110
_exptl_absorpt_coefficient_mu    23.967
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.404
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5184
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.1117
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            46569
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.10
_diffrn_ambient_temperature      175.6(8)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -91.00    3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -57.0000 -120.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega  -42.00   52.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747   77.0000    0.0000 94

#__ type_ start__ end____ width___ exp.time_
  3 omega   -5.00   49.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747   63.0000  -89.0000 54

#__ type_ start__ end____ width___ exp.time_
  4 omega  -92.00   13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -77.0000  150.0000 105

#__ type_ start__ end____ width___ exp.time_
  5 omega  -81.00  -50.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747    0.0000 -150.0000 31

#__ type_ start__ end____ width___ exp.time_
  6 omega  -29.00   -4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747    0.0000 -150.0000 25

#__ type_ start__ end____ width___ exp.time_
  7 omega   23.00   52.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747    0.0000 -150.0000 29

#__ type_ start__ end____ width___ exp.time_
  8 omega  -67.00  -32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -57.0000 -180.0000 35

#__ type_ start__ end____ width___ exp.time_
  9 omega    5.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809  -99.0000   60.0000 60
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0252562000
_diffrn_orient_matrix_UB_12      -0.0209116000
_diffrn_orient_matrix_UB_13      0.0149055000
_diffrn_orient_matrix_UB_21      -0.0213661000
_diffrn_orient_matrix_UB_22      0.0603505000
_diffrn_orient_matrix_UB_23      -0.0059188000
_diffrn_orient_matrix_UB_31      -0.0168555000
_diffrn_orient_matrix_UB_32      -0.0451561000
_diffrn_orient_matrix_UB_33      -0.0148328000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4153
_reflns_number_total             5515
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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 (Sheldrick, 2008)'
_refine_diff_density_max         2.285
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.286
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5515
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0423
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0132P)²+0.3905P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0736
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.001
Uanis(O16) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.001
Uanis(C17) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.001
3.a Free rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C19(H19A,H19B), C10(H10A,H10B), C16(H16A,H16B), C20(H20A,H20B),
 C4(H4A,H4B), C12(H12A,H12B), C14(H14A,H14B), C2(H2A,H2B), C8(H8A,H8B),
 C18(H18A,H18B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Pb1 Pb 0.70700(2) 0.97547(4) 0.067176(12) 0.00956(10) Uani 1 d C . . .
Pb3 Pb 0.70685(2) 1.02337(4) -0.195152(12) 0.00951(10) Uani 1 d . . . .
Pb4 Pb 0.75389(2) 0.95440(4) -0.313696(13) 0.01065(10) Uani 1 d . . . .
Pb2 Pb 0.76746(2) 0.99779(4) -0.064369(12) 0.01207(10) Uani 1 d . . . .
O9 O 0.6665(4) 0.9680(7) -0.1217(2) 0.0136(17) Uani 1 d . . . .
O5 O 0.6570(4) 0.9210(7) 0.1383(2) 0.0107(16) Uani 1 d . . . .
O1 O 0.7205(4) 1.2041(7) 0.1149(2) 0.0122(17) Uani 1 d . . . .
O15 O 0.6625(4) 1.0805(7) -0.2660(2) 0.0119(17) Uani 1 d B . . .
O14 O 0.6412(4) 1.4265(8) -0.1171(2) 0.0209(19) Uani 1 d . . . .
N1 N 0.6076(5) 1.1576(9) 0.0606(3) 0.013(2) Uani 1 d . . . U
O12 O 0.6739(4) 0.5746(7) -0.2574(2) 0.0159(18) Uani 1 d . . . .
O16 O 0.6344(4) 1.2839(7) -0.3011(2) 0.0148(17) Uani 1 d . 1 . U
O11 O 0.7187(4) 0.7964(7) -0.2437(2) 0.0098(16) Uani 1 d E . . .
O4 O 0.6801(4) 1.2403(7) -0.0412(2) 0.0172(18) Uani 1 d . . . U
O3 O 0.6676(4) 1.0310(7) -0.0058(2) 0.0130(16) Uani 1 d C . . .
O13 O 0.7078(4) 1.2858(7) -0.1576(2) 0.0190(19) Uani 1 d B . . .
C6 C 0.5999(6) 0.7259(11) 0.1021(3) 0.010(2) Uani 1 d . . . .
H6A H 0.6291 0.6417 0.0931 0.012 Uiso 1 calc A . R .
H6B H 0.5527 0.6872 0.1087 0.012 Uiso 1 calc A . R .
N2 N 0.5937(4) 0.8324(9) 0.0675(3) 0.009(2) Uani 1 d C . . U
N3 N 0.5925(4) 1.1664(9) -0.1967(3) 0.009(2) Uani 1 d B . . .
O2W O 0.4668(4) 0.5174(9) -0.1798(3) 0.031(2) Uani 1 d . . . .
H2WA H 0.4345 0.5768 -0.1729 0.047 Uiso 1 d . . G .
H2WB H 0.5058 0.5486 -0.1708 0.047 Uiso 1 d . . G .
C19 C 0.5413(5) 0.9234(10) -0.1793(3) 0.011(2) Uani 1 d B 1 . U
H19A H 0.5410 0.9502 -0.1498 0.013 Uiso 1 calc B . R .
H19B H 0.5005 0.8589 -0.1846 0.013 Uiso 1 calc B . R .
C11 C 0.6588(6) 0.8271(11) -0.1181(3) 0.011(2) Uani 1 d . . . U
O1W O 0.5276(4) 0.5187(11) -0.0639(3) 0.038(2) Uani 1 d . . . .
H1WA H 0.5423 0.5073 -0.0884 0.056 Uiso 1 d . . G .
H1WB H 0.5620 0.5377 -0.0482 0.056 Uiso 1 d . . G .
C10 C 0.5344(5) 0.9380(10) 0.0752(3) 0.006(2) Uani 1 d C 1 . U
H10A H 0.5330 0.9631 0.1048 0.007 Uiso 1 calc . . R .
H10B H 0.4897 0.8893 0.0680 0.007 Uiso 1 calc . . R .
C16 C 0.5851(5) 1.2473(10) -0.1576(3) 0.007(2) Uani 1 d B 1 . U
H16A H 0.5704 1.1769 -0.1360 0.009 Uiso 1 calc B . R .
H16B H 0.5472 1.3210 -0.1607 0.009 Uiso 1 calc B . R .
C5 C 0.6313(5) 0.7905(10) 0.1406(3) 0.007(2) Uani 1 d D 1 . U
O2 O 0.6751(4) 1.4243(7) 0.1292(2) 0.0154(18) Uani 1 d . . . .
C20 C 0.5341(5) 1.0620(10) -0.2048(3) 0.007(2) Uani 1 d . . . .
H20A H 0.5337 1.0356 -0.2344 0.009 Uiso 1 calc B . R .
H20B H 0.4890 1.1105 -0.1983 0.009 Uiso 1 calc B . R .
C15 C 0.6505(6) 1.3257(10) -0.1433(3) 0.008(2) Uani 1 d B 1 . U
O10 O 0.6794(4) 0.7571(7) -0.0872(2) 0.0183(19) Uani 1 d . . . U
C7 C 0.6520(6) 0.6735(11) 0.0158(3) 0.012(2) Uani 1 d D 1 . U
O6 O 0.6310(4) 0.7139(7) 0.1722(2) 0.0149(18) Uani 1 d . . . .
C1 C 0.6708(6) 1.2940(11) 0.1157(3) 0.010(2) Uani 1 d D . . U
C13 C 0.6698(6) 0.7035(11) -0.2441(3) 0.010(2) Uani 1 d E 1 . U
O8 O 0.6429(4) 0.5720(7) -0.0112(2) 0.0175(18) Uani 1 d . . . .
O7 O 0.7083(4) 0.7125(7) 0.0302(2) 0.0169(18) Uani 1 d . . . .
N4 N 0.6068(4) 0.8397(8) -0.1886(3) 0.0071(19) Uani 1 d B 1 . U
C4 C 0.6262(6) 1.2549(10) 0.0258(3) 0.013(3) Uani 1 d D . . .
H4A H 0.6588 1.3322 0.0355 0.015 Uiso 1 calc . . R .
H4B H 0.5834 1.3042 0.0155 0.015 Uiso 1 calc . . R .
C12 C 0.6258(6) 0.7447(10) -0.1537(3) 0.012(3) Uani 1 d B . . .
H12A H 0.6590 0.6684 -0.1634 0.014 Uiso 1 calc F . R .
H12B H 0.5832 0.6937 -0.1438 0.014 Uiso 1 calc F . R .
C9 C 0.5418(5) 1.0809(11) 0.0498(3) 0.010(2) Uani 1 d C . . U
C14 C 0.5990(6) 0.7521(11) -0.2266(3) 0.009(2) Uani 1 d . . . .
H14A H 0.5740 0.8116 -0.2475 0.011 Uiso 1 calc E . R .
H14B H 0.5703 0.6637 -0.2206 0.011 Uiso 1 calc E . R .
C2 C 0.6005(6) 1.2479(11) 0.0985(3) 0.010(2) Uani 1 d D 1 . U
H2A H 0.5749 1.1903 0.1196 0.012 Uiso 1 calc . . R .
H2B H 0.5726 1.3371 0.0922 0.012 Uiso 1 calc . . R .
C8 C 0.5836(6) 0.7499(11) 0.0280(3) 0.010(2) Uani 1 d . . . U
H8A H 0.5693 0.8192 0.0060 0.012 Uiso 1 calc D . R .
H8B H 0.5461 0.6755 0.0314 0.012 Uiso 1 calc D . R .
C18 C 0.6006(6) 1.2741(10) -0.2307(3) 0.011(3) Uani 1 d . . . .
H18A H 0.6298 1.3575 -0.2211 0.013 Uiso 1 calc B . R .
H18B H 0.5540 1.3138 -0.2381 0.013 Uiso 1 calc . . R .
C17 C 0.6338(6) 1.2078(11) -0.2688(3) 0.011(2) Uani 1 d B . . U
C3 C 0.6604(5) 1.1693(11) -0.0095(3) 0.012(2) Uani 1 d . . . 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 O5 2.548(7) . ?
Pb1 O1 2.601(7) . ?
Pb1 N1 2.526(9) . ?
Pb1 O3 2.537(7) . ?
Pb1 N2 2.522(8) . ?
Pb1 O7 2.669(7) . ?
Pb3 O9 2.555(7) . ?
Pb3 O15 2.506(7) . ?
Pb3 O11 2.602(6) . ?
Pb3 O13 2.674(7) . ?
Pb3 N3 2.541(8) . ?
Pb3 N4 2.544(8) . ?
Pb4 O5 2.571(7) 2_674 ?
Pb4 O15 2.599(7) . ?
Pb4 O12 2.537(7) 7_765 ?
Pb4 O16 2.667(7) 7_755 ?
Pb4 O2 2.630(7) 8_585 ?
Pb2 O9 2.695(7) . ?
Pb2 O14 2.530(7) 7_755 ?
Pb2 O4 2.650(7) 7_755 ?
Pb2 O3 2.711(7) . ?
Pb2 O10 2.666(7) 7_765 ?
Pb2 O8 2.523(7) 7_765 ?
O9 C11 1.292(11) . ?
O5 Pb4 2.571(7) 2_675 ?
O5 C5 1.284(11) . ?
O1 C1 1.252(12) . ?
O15 C17 1.280(11) . ?
O14 Pb2 2.530(7) 7_765 ?
O14 C15 1.259(11) . ?
N1 C4 1.477(13) . ?
N1 C9 1.478(13) . ?
N1 C2 1.486(13) . ?
O12 Pb4 2.537(7) 7_755 ?
O12 C13 1.248(11) . ?
O16 Pb4 2.667(7) 7_765 ?
O16 C17 1.256(12) . ?
O11 C13 1.258(12) . ?
O4 Pb2 2.650(7) 7_765 ?
O4 C3 1.271(12) . ?
O3 C3 1.267(11) . ?
O13 C15 1.243(12) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 N2 1.485(13) . ?
C6 C5 1.505(15) . ?
N2 C10 1.504(12) . ?
N2 C8 1.500(12) . ?
N3 C16 1.472(13) . ?
N3 C20 1.487(12) . ?
N3 C18 1.484(13) . ?
O2W H2WA 0.8504 . ?
O2W H2WB 0.8487 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.510(13) . ?
C19 N4 1.493(12) . ?
C11 O10 1.249(12) . ?
C11 C12 1.515(14) . ?
O1W H1WA 0.8498 . ?
O1W H1WB 0.8501 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C9 1.541(13) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C15 1.511(14) . ?
C5 O6 1.240(12) . ?
O2 Pb4 2.630(7) 8_586 ?
O2 C1 1.262(11) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
O10 Pb2 2.666(7) 7_755 ?
C7 O8 1.284(12) . ?
C7 O7 1.224(12) . ?
C7 C8 1.530(14) . ?
C1 C2 1.512(14) . ?
C13 C14 1.532(14) . ?
O8 Pb2 2.523(7) 7_755 ?
N4 C12 1.468(12) . ?
N4 C14 1.475(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.529(14) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C17 1.513(15) . ?

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
O5 Pb1 O1 69.6(2) . . ?
O5 Pb1 O7 103.8(2) . . ?
O1 Pb1 O7 168.2(2) . . ?
N1 Pb1 O5 85.5(3) . . ?
N1 Pb1 O1 66.7(2) . . ?
N1 Pb1 O3 64.4(2) . . ?
N1 Pb1 O7 123.6(3) . . ?
O3 Pb1 O5 140.7(2) . . ?
O3 Pb1 O1 115.3(2) . . ?
O3 Pb1 O7 76.1(2) . . ?
N2 Pb1 O5 64.8(2) . . ?
N2 Pb1 O1 119.5(2) . . ?
N2 Pb1 N1 72.1(3) . . ?
N2 Pb1 O3 81.5(2) . . ?
N2 Pb1 O7 63.3(2) . . ?
O9 Pb3 O11 115.9(2) . . ?
O9 Pb3 O13 75.6(2) . . ?
O15 Pb3 O9 142.7(2) . . ?
O15 Pb3 O11 68.7(2) . . ?
O15 Pb3 O13 103.7(2) . . ?
O15 Pb3 N3 65.5(2) . . ?
O15 Pb3 N4 87.6(2) . . ?
O11 Pb3 O13 168.4(2) . . ?
N3 Pb3 O9 81.9(3) . . ?
N3 Pb3 O11 117.8(2) . . ?
N3 Pb3 O13 63.9(3) . . ?
N3 Pb3 N4 71.9(2) . . ?
N4 Pb3 O9 64.3(2) . . ?
N4 Pb3 O11 66.3(2) . . ?
N4 Pb3 O13 123.3(3) . . ?
O5 Pb4 O15 127.8(2) 2_674 . ?
O5 Pb4 O16 79.5(2) 2_674 7_755 ?
O5 Pb4 O2 76.6(2) 2_674 8_585 ?
O15 Pb4 O16 134.5(2) . 7_755 ?
O15 Pb4 O2 81.5(2) . 8_585 ?
O12 Pb4 O5 83.6(2) 7_765 2_674 ?
O12 Pb4 O15 75.3(2) 7_765 . ?
O12 Pb4 O16 72.7(2) 7_765 7_755 ?
O12 Pb4 O2 129.8(2) 7_765 8_585 ?
O2 Pb4 O16 144.0(2) 8_585 7_755 ?
O9 Pb2 O3 89.6(2) . . ?
O14 Pb2 O9 90.0(2) 7_755 . ?
O14 Pb2 O4 72.9(2) 7_755 7_755 ?
O14 Pb2 O3 171.6(2) 7_755 . ?
O14 Pb2 O10 77.0(2) 7_755 7_765 ?
O4 Pb2 O9 112.3(2) 7_755 . ?
O4 Pb2 O3 99.5(2) 7_755 . ?
O4 Pb2 O10 135.4(2) 7_755 7_765 ?
O10 Pb2 O9 99.7(2) 7_765 . ?
O10 Pb2 O3 111.4(2) 7_765 . ?
O8 Pb2 O9 170.2(2) 7_765 . ?
O8 Pb2 O14 93.6(2) 7_765 7_755 ?
O8 Pb2 O4 77.5(2) 7_765 7_755 ?
O8 Pb2 O3 88.2(2) 7_765 . ?
O8 Pb2 O10 72.4(2) 7_765 7_765 ?
Pb3 O9 Pb2 114.2(3) . . ?
C11 O9 Pb3 108.3(6) . . ?
C11 O9 Pb2 96.7(6) . . ?
Pb1 O5 Pb4 102.5(2) . 2_675 ?
C5 O5 Pb1 112.0(6) . . ?
C5 O5 Pb4 128.5(6) . 2_675 ?
C1 O1 Pb1 117.1(7) . . ?
Pb3 O15 Pb4 103.2(2) . . ?
C17 O15 Pb3 113.3(6) . . ?
C17 O15 Pb4 129.9(7) . . ?
C15 O14 Pb2 123.0(7) . 7_765 ?
C4 N1 Pb1 105.9(6) . . ?
C4 N1 C9 107.7(8) . . ?
C4 N1 C2 109.2(8) . . ?
C9 N1 Pb1 110.6(6) . . ?
C9 N1 C2 112.2(8) . . ?
C2 N1 Pb1 111.0(6) . . ?
C13 O12 Pb4 133.3(7) . 7_755 ?
C17 O16 Pb4 117.0(7) . 7_765 ?
C13 O11 Pb3 118.1(6) . . ?
C3 O4 Pb2 142.0(7) . 7_765 ?
Pb1 O3 Pb2 115.1(3) . . ?
C3 O3 Pb1 108.4(6) . . ?
C3 O3 Pb2 96.9(6) . . ?
C15 O13 Pb3 115.1(6) . . ?
H6A C6 H6B 107.7 . . ?
N2 C6 H6A 108.8 . . ?
N2 C6 H6B 108.8 . . ?
N2 C6 C5 114.0(8) . . ?
C5 C6 H6A 108.8 . . ?
C5 C6 H6B 108.8 . . ?
C6 N2 Pb1 105.7(6) . . ?
C6 N2 C10 110.4(8) . . ?
C6 N2 C8 109.5(8) . . ?
C10 N2 Pb1 108.6(5) . . ?
C8 N2 Pb1 111.3(6) . . ?
C8 N2 C10 111.2(8) . . ?
C16 N3 Pb3 108.7(6) . . ?
C16 N3 C20 113.5(8) . . ?
C16 N3 C18 109.0(8) . . ?
C20 N3 Pb3 108.8(5) . . ?
C18 N3 Pb3 105.1(6) . . ?
C18 N3 C20 111.4(8) . . ?
H2WA O2W H2WB 109.5 . . ?
H19A C19 H19B 107.8 . . ?
C20 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
N4 C19 H19A 109.0 . . ?
N4 C19 H19B 109.0 . . ?
N4 C19 C20 112.9(8) . . ?
O9 C11 C12 117.7(9) . . ?
O10 C11 O9 122.7(9) . . ?
O10 C11 C12 119.6(9) . . ?
H1WA O1W H1WB 109.5 . . ?
N2 C10 H10A 109.2 . . ?
N2 C10 H10B 109.2 . . ?
N2 C10 C9 112.2(8) . . ?
H10A C10 H10B 107.9 . . ?
C9 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
N3 C16 H16A 108.6 . . ?
N3 C16 H16B 108.6 . . ?
N3 C16 C15 114.9(9) . . ?
H16A C16 H16B 107.5 . . ?
C15 C16 H16A 108.6 . . ?
C15 C16 H16B 108.6 . . ?
O5 C5 C6 117.5(9) . . ?
O6 C5 O5 124.5(10) . . ?
O6 C5 C6 118.0(9) . . ?
C1 O2 Pb4 132.3(7) . 8_586 ?
N3 C20 C19 111.3(8) . . ?
N3 C20 H20A 109.4 . . ?
N3 C20 H20B 109.4 . . ?
C19 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
O14 C15 C16 115.6(9) . . ?
O13 C15 O14 126.0(10) . . ?
O13 C15 C16 118.4(9) . . ?
C11 O10 Pb2 142.3(7) . 7_755 ?
O8 C7 C8 112.6(9) . . ?
O7 C7 O8 126.0(10) . . ?
O7 C7 C8 121.4(10) . . ?
O1 C1 O2 124.5(10) . . ?
O1 C1 C2 119.1(9) . . ?
O2 C1 C2 116.4(9) . . ?
O12 C13 O11 125.8(10) . . ?
O12 C13 C14 116.9(9) . . ?
O11 C13 C14 117.3(9) . . ?
C7 O8 Pb2 124.5(7) . 7_755 ?
C7 O7 Pb1 114.9(7) . . ?
C19 N4 Pb3 108.3(5) . . ?
C12 N4 Pb3 105.2(6) . . ?
C12 N4 C19 110.5(8) . . ?
C12 N4 C14 110.8(7) . . ?
C14 N4 Pb3 111.0(6) . . ?
C14 N4 C19 110.9(8) . . ?
N1 C4 H4A 109.2 . . ?
N1 C4 H4B 109.2 . . ?
N1 C4 C3 111.9(8) . . ?
H4A C4 H4B 107.9 . . ?
C3 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
C11 C12 H12A 108.8 . . ?
C11 C12 H12B 108.8 . . ?
N4 C12 C11 113.8(8) . . ?
N4 C12 H12A 108.8 . . ?
N4 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
N1 C9 C10 110.3(8) . . ?
C13 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
N4 C14 C13 112.2(9) . . ?
N4 C14 H14A 109.2 . . ?
N4 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
N1 C2 C1 112.2(9) . . ?
N1 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N2 C8 C7 109.7(9) . . ?
N2 C8 H8A 109.7 . . ?
N2 C8 H8B 109.7 . . ?
C7 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
N3 C18 H18A 109.0 . . ?
N3 C18 H18B 109.0 . . ?
N3 C18 C17 113.0(8) . . ?
H18A C18 H18B 107.8 . . ?
C17 C18 H18A 109.0 . . ?
C17 C18 H18B 109.0 . . ?
O15 C17 C18 118.7(9) . . ?
O16 C17 O15 123.4(10) . . ?
O16 C17 C18 117.8(9) . . ?
O4 C3 C4 118.4(9) . . ?
O3 C3 O4 123.0(10) . . ?
O3 C3 C4 118.5(9) . . ?

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 O5 C5 C6 -31.4(11) . . . . ?
Pb1 O5 C5 O6 148.1(9) . . . . ?
Pb1 O1 C1 O2 -162.8(8) . . . . ?
Pb1 O1 C1 C2 15.5(12) . . . . ?
Pb1 N1 C4 C3 39.2(10) . . . . ?
Pb1 N1 C9 C10 42.4(9) . . . . ?
Pb1 N1 C2 C1 40.9(9) . . . . ?
Pb1 O3 C3 O4 138.6(9) . . . . ?
Pb1 O3 C3 C4 -41.7(11) . . . . ?
Pb1 N2 C10 C9 43.7(9) . . . . ?
Pb1 N2 C8 C7 44.8(9) . . . . ?
Pb3 O9 C11 O10 136.9(9) . . . . ?
Pb3 O9 C11 C12 -40.7(10) . . . . ?
Pb3 O15 C17 O16 149.4(9) . . . . ?
Pb3 O15 C17 C18 -27.4(12) . . . . ?
Pb3 O11 C13 O12 -161.8(8) . . . . ?
Pb3 O11 C13 C14 17.8(12) . . . . ?
Pb3 O13 C15 O14 163.5(8) . . . . ?
Pb3 O13 C15 C16 -15.9(12) . . . . ?
Pb3 N3 C16 C15 44.7(9) . . . . ?
Pb3 N3 C20 C19 44.3(9) . . . . ?
Pb3 N3 C18 C17 43.0(10) . . . . ?
Pb3 N4 C12 C11 40.0(10) . . . . ?
Pb3 N4 C14 C13 42.2(9) . . . . ?
Pb4 O5 C5 C6 -159.8(6) 2_675 . . . ?
Pb4 O5 C5 O6 19.7(15) 2_675 . . . ?
Pb4 O15 C17 O16 16.2(16) . . . . ?
Pb4 O15 C17 C18 -160.7(7) . . . . ?
Pb4 O12 C13 O11 -30.6(17) 7_755 . . . ?
Pb4 O12 C13 C14 149.8(7) 7_755 . . . ?
Pb4 O16 C17 O15 -85.5(11) 7_765 . . . ?
Pb4 O16 C17 C18 91.4(10) 7_765 . . . ?
Pb4 O2 C1 O1 -29.7(16) 8_586 . . . ?
Pb4 O2 C1 C2 152.0(7) 8_586 . . . ?
Pb2 O9 C11 O10 18.6(11) . . . . ?
Pb2 O9 C11 C12 -159.0(8) . . . . ?
Pb2 O14 C15 O13 -28.0(15) 7_765 . . . ?
Pb2 O14 C15 C16 151.4(7) 7_765 . . . ?
Pb2 O4 C3 O3 -146.1(8) 7_765 . . . ?
Pb2 O4 C3 C4 34.2(16) 7_765 . . . ?
Pb2 O3 C3 O4 19.2(11) . . . . ?
Pb2 O3 C3 C4 -161.1(8) . . . . ?
O9 Pb3 O15 Pb4 -146.1(3) . . . . ?
O9 Pb3 O15 C17 68.9(8) . . . . ?
O9 Pb3 O11 C13 46.1(8) . . . . ?
O9 Pb3 O13 C15 -59.0(7) . . . . ?
O9 Pb3 N3 C16 42.6(6) . . . . ?
O9 Pb3 N3 C20 -81.4(6) . . . . ?
O9 Pb3 N3 C18 159.2(6) . . . . ?
O9 Pb3 N4 C19 76.2(6) . . . . ?
O9 Pb3 N4 C12 -42.0(6) . . . . ?
O9 Pb3 N4 C14 -161.8(7) . . . . ?
O9 Pb2 O3 Pb1 158.3(3) . . . . ?
O9 Pb2 O3 C3 -87.6(6) . . . . ?
O9 C11 O10 Pb2 -146.1(8) . . . 7_755 ?
O9 C11 C12 N4 0.1(14) . . . . ?
O5 Pb1 O1 C1 -88.7(7) . . . . ?
O5 Pb1 N1 C4 163.9(6) . . . . ?
O5 Pb1 N1 C9 -79.6(6) . . . . ?
O5 Pb1 N1 C2 45.6(6) . . . . ?
O5 Pb1 O3 Pb2 -163.6(2) . . . . ?
O5 Pb1 O3 C3 89.2(7) . . . . ?
O5 Pb1 N2 C6 -40.1(6) . . . . ?
O5 Pb1 N2 C10 78.4(6) . . . . ?
O5 Pb1 N2 C8 -158.9(6) . . . . ?
O5 Pb1 O7 C7 80.9(8) . . . . ?
O5 Pb4 O15 Pb3 -111.6(3) 2_674 . . . ?
O5 Pb4 O15 C17 25.0(10) 2_674 . . . ?
O1 Pb1 O5 Pb4 -39.9(2) . . . 2_675 ?
O1 Pb1 O5 C5 179.0(7) . . . . ?
O1 Pb1 N1 C4 94.3(6) . . . . ?
O1 Pb1 N1 C9 -149.3(7) . . . . ?
O1 Pb1 N1 C2 -24.1(6) . . . . ?
O1 Pb1 O3 Pb2 108.2(3) . . . . ?
O1 Pb1 O3 C3 1.0(7) . . . . ?
O1 Pb1 N2 C6 -85.0(6) . . . . ?
O1 Pb1 N2 C10 33.5(7) . . . . ?
O1 Pb1 N2 C8 156.3(5) . . . . ?
O1 Pb1 O7 C7 135.4(11) . . . . ?
O1 C1 C2 N1 -39.0(13) . . . . ?
O15 Pb3 O9 Pb2 -163.5(3) . . . . ?
O15 Pb3 O9 C11 90.0(7) . . . . ?
O15 Pb3 O11 C13 -93.4(7) . . . . ?
O15 Pb3 O13 C15 82.5(8) . . . . ?
O15 Pb3 N3 C16 -156.1(6) . . . . ?
O15 Pb3 N3 C20 79.8(6) . . . . ?
O15 Pb3 N3 C18 -39.5(6) . . . . ?
O15 Pb3 N4 C19 -78.4(6) . . . . ?
O15 Pb3 N4 C12 163.4(6) . . . . ?
O15 Pb3 N4 C14 43.6(6) . . . . ?
O14 Pb2 O9 Pb3 -30.0(3) 7_755 . . . ?
O14 Pb2 O9 C11 83.6(6) 7_755 . . . ?
O14 Pb2 O3 Pb1 71.3(16) 7_755 . . . ?
O14 Pb2 O3 C3 -174.6(14) 7_755 . . . ?
N1 Pb1 O5 Pb4 -106.7(3) . . . 2_675 ?
N1 Pb1 O5 C5 112.3(7) . . . . ?
N1 Pb1 O1 C1 5.3(7) . . . . ?
N1 Pb1 O3 Pb2 152.7(4) . . . . ?
N1 Pb1 O3 C3 45.5(6) . . . . ?
N1 Pb1 N2 C6 -133.6(6) . . . . ?
N1 Pb1 N2 C10 -15.1(6) . . . . ?
N1 Pb1 N2 C8 107.6(6) . . . . ?
N1 Pb1 O7 C7 -12.9(9) . . . . ?
N1 C4 C3 O4 -178.9(9) . . . . ?
N1 C4 C3 O3 1.4(14) . . . . ?
O12 Pb4 O15 Pb3 -42.1(2) 7_765 . . . ?
O12 Pb4 O15 C17 94.5(9) 7_765 . . . ?
O12 C13 C14 N4 138.3(9) . . . . ?
O16 Pb4 O15 Pb3 4.5(4) 7_755 . . . ?
O16 Pb4 O15 C17 141.1(8) 7_755 . . . ?
O11 Pb3 O9 Pb2 108.2(3) . . . . ?
O11 Pb3 O9 C11 1.7(7) . . . . ?
O11 Pb3 O15 Pb4 -41.0(2) . . . . ?
O11 Pb3 O15 C17 174.0(7) . . . . ?
O11 Pb3 O13 C15 130.5(11) . . . . ?
O11 Pb3 N3 C16 157.6(5) . . . . ?
O11 Pb3 N3 C20 33.6(7) . . . . ?
O11 Pb3 N3 C18 -85.8(6) . . . . ?
O11 Pb3 N4 C19 -146.2(7) . . . . ?
O11 Pb3 N4 C12 95.7(6) . . . . ?
O11 Pb3 N4 C14 -24.2(6) . . . . ?
O11 C13 C14 N4 -41.4(13) . . . . ?
O4 Pb2 O9 Pb3 -101.6(3) 7_755 . . . ?
O4 Pb2 O9 C11 12.0(6) 7_755 . . . ?
O4 Pb2 O3 Pb1 45.8(3) 7_755 . . . ?
O4 Pb2 O3 C3 159.9(6) 7_755 . . . ?
O3 Pb1 O5 Pb4 -145.4(3) . . . 2_675 ?
O3 Pb1 O5 C5 73.6(7) . . . . ?
O3 Pb1 O1 C1 48.8(8) . . . . ?
O3 Pb1 N1 C4 -42.1(6) . . . . ?
O3 Pb1 N1 C9 74.4(6) . . . . ?
O3 Pb1 N1 C2 -160.5(7) . . . . ?
O3 Pb1 N2 C6 160.6(6) . . . . ?
O3 Pb1 N2 C10 -80.9(6) . . . . ?
O3 Pb1 N2 C8 41.9(6) . . . . ?
O3 Pb1 O7 C7 -58.6(8) . . . . ?
O3 Pb2 O9 Pb3 158.4(3) . . . . ?
O3 Pb2 O9 C11 -88.0(6) . . . . ?
O13 Pb3 O9 Pb2 -69.7(3) . . . . ?
O13 Pb3 O9 C11 -176.1(7) . . . . ?
O13 Pb3 O15 Pb4 129.7(2) . . . . ?
O13 Pb3 O15 C17 -15.2(7) . . . . ?
O13 Pb3 O11 C13 -144.1(11) . . . . ?
O13 Pb3 N3 C16 -35.3(5) . . . . ?
O13 Pb3 N3 C20 -159.3(7) . . . . ?
O13 Pb3 N3 C18 81.3(6) . . . . ?
O13 Pb3 N4 C19 26.5(7) . . . . ?
O13 Pb3 N4 C12 -91.7(6) . . . . ?
O13 Pb3 N4 C14 148.4(6) . . . . ?
C6 N2 C10 C9 159.2(8) . . . . ?
C6 N2 C8 C7 -71.7(10) . . . . ?
N2 Pb1 O5 Pb4 -178.9(3) . . . 2_675 ?
N2 Pb1 O5 C5 40.0(6) . . . . ?
N2 Pb1 O1 C1 -45.8(8) . . . . ?
N2 Pb1 N1 C4 -131.1(7) . . . . ?
N2 Pb1 N1 C9 -14.6(6) . . . . ?
N2 Pb1 N1 C2 110.5(7) . . . . ?
N2 Pb1 O3 Pb2 -133.2(3) . . . . ?
N2 Pb1 O3 C3 119.6(7) . . . . ?
N2 Pb1 O7 C7 28.8(7) . . . . ?
N2 C6 C5 O5 -8.4(13) . . . . ?
N2 C6 C5 O6 172.1(9) . . . . ?
N2 C10 C9 N1 -60.0(10) . . . . ?
N3 Pb3 O9 Pb2 -134.7(3) . . . . ?
N3 Pb3 O9 C11 118.8(7) . . . . ?
N3 Pb3 O15 Pb4 -177.7(3) . . . . ?
N3 Pb3 O15 C17 37.3(7) . . . . ?
N3 Pb3 O11 C13 -48.5(8) . . . . ?
N3 Pb3 O13 C15 29.0(7) . . . . ?
N3 Pb3 N4 C19 -13.4(6) . . . . ?
N3 Pb3 N4 C12 -131.6(6) . . . . ?
N3 Pb3 N4 C14 108.6(6) . . . . ?
N3 C16 C15 O14 161.0(9) . . . . ?
N3 C16 C15 O13 -19.5(14) . . . . ?
N3 C18 C17 O15 -12.4(14) . . . . ?
N3 C18 C17 O16 170.6(9) . . . . ?
C19 N4 C12 C11 -76.7(11) . . . . ?
C19 N4 C14 C13 162.6(8) . . . . ?
C10 N2 C8 C7 166.0(8) . . . . ?
C16 N3 C20 C19 -76.9(10) . . . . ?
C16 N3 C18 C17 159.4(8) . . . . ?
C5 C6 N2 Pb1 42.6(9) . . . . ?
C5 C6 N2 C10 -74.7(10) . . . . ?
C5 C6 N2 C8 162.5(8) . . . . ?
O2 Pb4 O15 Pb3 -177.2(3) 8_585 . . . ?
O2 Pb4 O15 C17 -40.6(9) 8_585 . . . ?
O2 C1 C2 N1 139.3(9) . . . . ?
C20 N3 C16 C15 165.9(8) . . . . ?
C20 N3 C18 C17 -74.7(11) . . . . ?
C20 C19 N4 Pb3 42.6(9) . . . . ?
C20 C19 N4 C12 157.4(8) . . . . ?
C20 C19 N4 C14 -79.4(10) . . . . ?
O10 Pb2 O9 Pb3 46.7(3) 7_765 . . . ?
O10 Pb2 O9 C11 160.3(6) 7_765 . . . ?
O10 Pb2 O3 Pb1 -101.4(3) 7_765 . . . ?
O10 Pb2 O3 C3 12.7(7) 7_765 . . . ?
O10 C11 C12 N4 -177.5(9) . . . . ?
O8 Pb2 O9 Pb3 81.6(13) 7_765 . . . ?
O8 Pb2 O9 C11 -164.8(12) 7_765 . . . ?
O8 Pb2 O3 Pb1 -31.2(3) 7_765 . . . ?
O8 Pb2 O3 C3 82.9(6) 7_765 . . . ?
O8 C7 O7 Pb1 162.2(8) . . . . ?
O8 C7 C8 N2 163.1(8) . . . . ?
O7 Pb1 O5 Pb4 129.8(2) . . . 2_675 ?
O7 Pb1 O5 C5 -11.2(7) . . . . ?
O7 Pb1 O1 C1 -146.2(11) . . . . ?
O7 Pb1 N1 C4 -92.5(6) . . . . ?
O7 Pb1 N1 C9 24.0(7) . . . . ?
O7 Pb1 N1 C2 149.1(6) . . . . ?
O7 Pb1 O3 Pb2 -68.7(3) . . . . ?
O7 Pb1 O3 C3 -175.9(7) . . . . ?
O7 Pb1 N2 C6 82.0(6) . . . . ?
O7 Pb1 N2 C10 -159.5(7) . . . . ?
O7 Pb1 N2 C8 -36.8(6) . . . . ?
O7 C7 O8 Pb2 -27.6(15) . . . 7_755 ?
O7 C7 C8 N2 -19.1(14) . . . . ?
N4 Pb3 O9 Pb2 151.5(3) . . . . ?
N4 Pb3 O9 C11 45.0(6) . . . . ?
N4 Pb3 O15 Pb4 -106.5(3) . . . . ?
N4 Pb3 O15 C17 108.5(7) . . . . ?
N4 Pb3 O11 C13 3.6(7) . . . . ?
N4 Pb3 O13 C15 -13.7(8) . . . . ?
N4 Pb3 N3 C16 108.2(6) . . . . ?
N4 Pb3 N3 C20 -15.9(6) . . . . ?
N4 Pb3 N3 C18 -135.3(6) . . . . ?
N4 C19 C20 N3 -61.4(11) . . . . ?
C4 N1 C9 C10 157.7(8) . . . . ?
C4 N1 C2 C1 -75.5(11) . . . . ?
C12 C11 O10 Pb2 31.5(17) . . . 7_755 ?
C12 N4 C14 C13 -74.3(11) . . . . ?
C9 N1 C4 C3 -79.2(10) . . . . ?
C9 N1 C2 C1 165.2(8) . . . . ?
C14 N4 C12 C11 159.9(9) . . . . ?
C2 N1 C4 C3 158.7(8) . . . . ?
C2 N1 C9 C10 -82.1(10) . . . . ?
C8 N2 C10 C9 -79.1(10) . . . . ?
C8 C7 O8 Pb2 150.0(7) . . . 7_755 ?
C8 C7 O7 Pb1 -15.2(13) . . . . ?
C18 N3 C16 C15 -69.4(11) . . . . ?
C18 N3 C20 C19 159.7(8) . . . . ?

_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_sad
_database_code_depnum_ccdc_archive 'CCDC 1533511'
_audit_update_record             
;
2017-02-18 deposited with the CCDC.
2017-04-06 downloaded from the CCDC.
;
_audit_creation_date             2016-08-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C20 H28 Cl2 N4 O18 Pb5, 2(H2 O)'
_chemical_formula_sum            'C20 H32 Cl2 N4 O20 Pb5'
_chemical_formula_weight         1755.34
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   7.5204(4)
_cell_length_b                   8.8464(4)
_cell_length_c                   13.5079(5)
_cell_angle_alpha                72.888(4)
_cell_angle_beta                 81.027(4)
_cell_angle_gamma                75.571(4)
_cell_volume                     828.46(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    98
_cell_measurement_temperature    173
_cell_measurement_theta_max      33.5373
_cell_measurement_theta_min      2.9949
_shelx_estimated_absorpt_T_max   0.234
_shelx_estimated_absorpt_T_min   0.114
_exptl_absorpt_coefficient_mu    25.570
_exptl_absorpt_correction_T_max  0.2342
_exptl_absorpt_correction_T_min  0.1141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.518
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9640
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.808
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -40.00  -14.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8810  135.0000  -57.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega  -94.00   -3.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8810  135.0000  122.0000 91

#__ type_ start__ end____ width___ exp.time_
  3 omega   45.00   79.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435 -135.0000   57.0000 34

#__ type_ start__ end____ width___ exp.time_
  4 omega   36.00   61.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435 -135.0000 -122.0000 25

#__ type_ start__ end____ width___ exp.time_
  5 omega  -98.00    4.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8810  -77.0000  120.0000 102

#__ type_ start__ end____ width___ exp.time_
  6 omega -101.00  -33.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8810  -38.0000 -150.0000 68

#__ type_ start__ end____ width___ exp.time_
  7 omega  -25.00    3.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8810  -38.0000 -150.0000 28

#__ type_ start__ end____ width___ exp.time_
  8 omega  -28.00   17.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435  -38.0000   30.0000 45

#__ type_ start__ end____ width___ exp.time_
  9 omega   59.00  110.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435  179.0000   30.0000 51

#__ type_ start__ end____ width___ exp.time_
 10 omega   81.00  110.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435  179.0000 -150.0000 29

#__ type_ start__ end____ width___ exp.time_
 11 omega  -42.00   25.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435  -38.0000  -30.0000 67

#__ type_ start__ end____ width___ exp.time_
 12 omega  -43.00   17.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       30.4435  -38.0000  120.0000 60
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0566527633
_diffrn_orient_matrix_UB_12      0.0537548651
_diffrn_orient_matrix_UB_13      0.0005578720
_diffrn_orient_matrix_UB_21      0.0066562722
_diffrn_orient_matrix_UB_22      0.0244469731
_diffrn_orient_matrix_UB_23      -0.0550665458
_diffrn_orient_matrix_UB_31      -0.0784539382
_diffrn_orient_matrix_UB_32      0.0618090237
_diffrn_orient_matrix_UB_33      -0.0001298519
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2903
_reflns_number_total             3244
_reflns_odcompleteness_completeness 75.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_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         2.011
_refine_diff_density_min         -2.515
_refine_diff_density_rms         0.264
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3244
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0258
_refine_ls_restrained_S_all      1.008
_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)+(0.0398P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0608
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups, {H1Wa,H1Wb} of C10
 At 1.2 times of:
  {H2a,H2b} of C2, {H4a,H4b} of C4, {H6a,H6b} of C6, {H9a,H9b} of C9, {H8a,
  H8b} of C8, {H10a,H10b} of C10
2. Restrained distances
 H1Wa-O1W = H1Wb-O1W
 0.85 with sigma of 0.01
 H1Wa-H1Wb
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4.a Free rotating group:
 O2W(H2Wa,H2Wb)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C4(H4a,H4b), C6(H6a,H6b), C9(H9a,H9b), C8(H8a,H8b), C10(H10a,H10b)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.22902(3) 0.37754(3) 0.66363(2) 0.00997(8) Uani 1 1 d . . . . .
Pb2 Pb 1.01440(3) -0.14311(3) 0.66587(2) 0.01212(8) Uani 1 1 d . . . . .
Pb3 Pb 0.5000 1.0000 0.5000 0.01403(10) Uani 1 2 d S T P . .
Cl1 Cl 0.8446(2) -0.2740(2) 0.53967(15) 0.0210(4) Uani 1 1 d . . . . .
O1 O 0.7739(6) 0.0937(5) 0.5782(4) 0.0128(10) Uani 1 1 d . . . . .
O4 O 0.3615(7) 0.6418(6) 0.6034(4) 0.0196(11) Uani 1 1 d . . . . .
O8 O 0.0803(6) 0.5583(5) 0.7823(4) 0.0157(10) Uani 1 1 d . . . . .
O5 O 0.0819(7) 0.1201(5) 0.7255(4) 0.0172(11) Uani 1 1 d . . . . .
O3 O 0.4422(7) 0.8044(5) 0.6782(4) 0.0169(11) Uani 1 1 d . . . . .
O2 O 0.4812(6) 0.1612(5) 0.6340(4) 0.0148(10) Uani 1 1 d . . . . .
O1W O 0.7246(6) -0.1553(5) 0.7767(4) 0.0154(10) Uani 1 1 d D . . . .
O7 O -0.1483(7) 0.5585(5) 0.9104(4) 0.0180(11) Uani 1 1 d . . . . .
O6 O 0.0857(7) -0.1200(5) 0.8381(4) 0.0173(10) Uani 1 1 d . . . . .
C1 C 0.6460(9) 0.1805(8) 0.6201(5) 0.0134(14) Uani 1 1 d . . . . .
N1 N 0.5388(7) 0.3649(6) 0.7329(4) 0.0093(11) Uani 1 1 d . . . . .
C3 C 0.4453(9) 0.6638(8) 0.6689(5) 0.0126(14) Uani 1 1 d . . . . .
O2W O 0.3723(7) -0.3449(6) 0.9528(4) 0.0233(12) Uani 1 1 d . . . . .
H2WA H 0.3319 -0.4128 1.0048 0.035 Uiso 1 1 d G . . . .
H2WB H 0.2837 -0.2872 0.9171 0.035 Uiso 1 1 d G . . . .
C2 C 0.6826(9) 0.3173(7) 0.6532(5) 0.0131(14) Uani 1 1 d . . . . .
H2A H 0.8044 0.2834 0.6816 0.016 Uiso 1 1 calc R . . . .
H2B H 0.6864 0.4116 0.5920 0.016 Uiso 1 1 calc R . . . .
N2 N 0.2275(7) 0.2311(6) 0.8590(4) 0.0106(11) Uani 1 1 d . . . . .
C4 C 0.5517(9) 0.5224(7) 0.7455(5) 0.0124(14) Uani 1 1 d . . . . .
H4A H 0.6828 0.5297 0.7358 0.015 Uiso 1 1 calc R . . . .
H4B H 0.5035 0.5283 0.8170 0.015 Uiso 1 1 calc R . . . .
C6 C 0.2391(9) 0.0550(7) 0.8779(5) 0.0109(13) Uani 1 1 d . . . . .
H6A H 0.1981 0.0098 0.9517 0.013 Uiso 1 1 calc R . . . .
H6B H 0.3695 0.0008 0.8656 0.013 Uiso 1 1 calc R . . . .
C7 C -0.0095(8) 0.4917(7) 0.8627(5) 0.0085(13) Uani 1 1 d . U . . .
C9 C 0.5543(9) 0.2408(7) 0.8342(6) 0.0134(14) Uani 1 1 d . . . . .
H9A H 0.6553 0.2511 0.8692 0.016 Uiso 1 1 calc R . . . .
H9B H 0.5856 0.1317 0.8223 0.016 Uiso 1 1 calc R . . . .
C5 C 0.1248(9) 0.0170(8) 0.8102(5) 0.0132(14) Uani 1 1 d . . . . .
C8 C 0.0470(9) 0.3050(7) 0.9061(5) 0.0130(14) Uani 1 1 d . . . . .
H8A H 0.0522 0.2787 0.9822 0.016 Uiso 1 1 calc R . . . .
H8B H -0.0495 0.2558 0.8938 0.016 Uiso 1 1 calc R . . . .
C10 C 0.3780(9) 0.2584(8) 0.9037(5) 0.0118(13) Uani 1 1 d . . . . .
H10A H 0.3964 0.1795 0.9725 0.014 Uiso 1 1 calc R . . . .
H10B H 0.3446 0.3685 0.9141 0.014 Uiso 1 1 calc R . . . .
H1WA H 0.626(6) -0.150(7) 0.751(5) 0.018 Uiso 1 1 d DR . . . .
H1WB H 0.746(9) -0.241(5) 0.826(4) 0.018 Uiso 1 1 d DR . . . .


_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 O4 2.628(5) . ?
Pb1 O8 2.537(4) . ?
Pb1 O5 2.638(5) . ?
Pb1 O2 2.413(4) . ?
Pb1 N1 2.608(5) . ?
Pb1 N2 2.575(5) . ?
Pb2 Cl1 2.9078(17) . ?
Pb2 O1 2.526(4) . ?
Pb2 O8 2.616(4) 1_645 ?
Pb2 O1W 2.451(5) . ?
Pb2 O6 2.542(5) 1_655 ?
Pb3 Cl1 3.0684(18) 2_666 ?
Pb3 Cl1 3.0684(18) 1_565 ?
Pb3 O3 2.564(5) 2_676 ?
Pb3 O3 2.564(5) . ?
Pb3 O2 2.582(5) 1_565 ?
Pb3 O2 2.582(5) 2_666 ?
Cl1 Pb3 3.0685(18) 1_545 ?
O1 C1 1.247(8) . ?
O4 C3 1.246(8) . ?
O8 Pb2 2.616(4) 1_465 ?
O8 C7 1.255(8) . ?
O5 C5 1.264(8) . ?
O3 C3 1.281(8) . ?
O2 Pb3 2.583(5) 1_545 ?
O2 C1 1.270(8) . ?
O1W H1WA 0.849(10) . ?
O1W H1WB 0.852(10) . ?
O7 C7 1.249(8) . ?
O6 Pb2 2.542(5) 1_455 ?
O6 C5 1.254(8) . ?
C1 C2 1.504(9) . ?
N1 C2 1.477(8) . ?
N1 C4 1.480(8) . ?
N1 C9 1.481(9) . ?
C3 C4 1.508(9) . ?
O2W H2WA 0.8499 . ?
O2W H2WB 0.8501 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N2 C6 1.485(7) . ?
N2 C8 1.486(8) . ?
N2 C10 1.462(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.504(9) . ?
C7 C8 1.552(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.503(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 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
O4 Pb1 O5 177.53(15) . . ?
O8 Pb1 O4 70.95(16) . . ?
O8 Pb1 O5 107.15(15) . . ?
O8 Pb1 N1 85.82(16) . . ?
O8 Pb1 N2 65.62(15) . . ?
O2 Pb1 O4 106.01(15) . . ?
O2 Pb1 O8 146.08(15) . . ?
O2 Pb1 O5 76.45(15) . . ?
O2 Pb1 N1 64.49(15) . . ?
O2 Pb1 N2 87.76(16) . . ?
N1 Pb1 O4 62.66(15) . . ?
N1 Pb1 O5 119.08(15) . . ?
N2 Pb1 O4 116.10(16) . . ?
N2 Pb1 O5 63.89(16) . . ?
N2 Pb1 N1 69.52(17) . . ?
O1 Pb2 Cl1 75.59(11) . . ?
O1 Pb2 O8 146.16(15) . 1_645 ?
O1 Pb2 O6 112.93(14) . 1_655 ?
O8 Pb2 Cl1 84.07(11) 1_645 . ?
O1W Pb2 Cl1 83.20(12) . . ?
O1W Pb2 O1 73.17(15) . . ?
O1W Pb2 O8 77.85(15) . 1_645 ?
O1W Pb2 O6 75.90(17) . 1_655 ?
O6 Pb2 Cl1 153.35(11) 1_655 . ?
O6 Pb2 O8 75.58(14) 1_655 1_645 ?
Cl1 Pb3 Cl1 180.0 2_666 1_565 ?
O3 Pb3 Cl1 71.86(11) 2_676 2_666 ?
O3 Pb3 Cl1 108.14(11) 2_676 1_565 ?
O3 Pb3 Cl1 108.14(11) . 2_666 ?
O3 Pb3 Cl1 71.86(11) . 1_565 ?
O3 Pb3 O3 180.0 . 2_676 ?
O3 Pb3 O2 74.49(14) . 1_565 ?
O3 Pb3 O2 105.51(14) 2_676 1_565 ?
O3 Pb3 O2 74.49(14) 2_676 2_666 ?
O3 Pb3 O2 105.51(14) . 2_666 ?
O2 Pb3 Cl1 73.94(10) 2_666 1_565 ?
O2 Pb3 Cl1 73.94(10) 1_565 2_666 ?
O2 Pb3 Cl1 106.06(10) 1_565 1_565 ?
O2 Pb3 Cl1 106.06(10) 2_666 2_666 ?
O2 Pb3 O2 180.00(12) 2_666 1_565 ?
Pb2 Cl1 Pb3 97.44(5) . 1_545 ?
C1 O1 Pb2 127.8(4) . . ?
C3 O4 Pb1 115.3(4) . . ?
Pb1 O8 Pb2 107.35(17) . 1_465 ?
C7 O8 Pb1 114.6(4) . . ?
C7 O8 Pb2 129.8(4) . 1_465 ?
C5 O5 Pb1 118.7(4) . . ?
C3 O3 Pb3 110.7(4) . . ?
Pb1 O2 Pb3 125.54(19) . 1_545 ?
C1 O2 Pb1 120.2(4) . . ?
C1 O2 Pb3 99.3(4) . 1_545 ?
Pb2 O1W H1WA 121(5) . . ?
Pb2 O1W H1WB 107(5) . . ?
H1WA O1W H1WB 109.7(18) . . ?
C5 O6 Pb2 100.6(4) . 1_455 ?
O1 C1 O2 122.3(6) . . ?
O1 C1 C2 120.1(6) . . ?
O2 C1 C2 117.6(6) . . ?
C2 N1 Pb1 104.6(4) . . ?
C2 N1 C4 110.0(5) . . ?
C2 N1 C9 111.5(5) . . ?
C4 N1 Pb1 112.7(4) . . ?
C4 N1 C9 109.8(5) . . ?
C9 N1 Pb1 108.1(4) . . ?
O4 C3 O3 123.2(6) . . ?
O4 C3 C4 120.9(6) . . ?
O3 C3 C4 115.9(6) . . ?
H2WA O2W H2WB 109.5 . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
N1 C2 C1 111.2(5) . . ?
N1 C2 H2A 109.4 . . ?
N1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C6 N2 Pb1 111.4(4) . . ?
C6 N2 C8 109.1(5) . . ?
C8 N2 Pb1 105.0(4) . . ?
C10 N2 Pb1 110.6(4) . . ?
C10 N2 C6 110.5(5) . . ?
C10 N2 C8 110.1(5) . . ?
N1 C4 C3 112.2(5) . . ?
N1 C4 H4A 109.2 . . ?
N1 C4 H4B 109.2 . . ?
C3 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N2 C6 H6A 108.9 . . ?
N2 C6 H6B 108.9 . . ?
N2 C6 C5 113.5(5) . . ?
H6A C6 H6B 107.7 . . ?
C5 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
O8 C7 C8 118.1(5) . . ?
O7 C7 O8 127.0(6) . . ?
O7 C7 C8 114.8(6) . . ?
N1 C9 H9A 109.3 . . ?
N1 C9 H9B 109.3 . . ?
N1 C9 C10 111.6(5) . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
O5 C5 C6 118.8(6) . . ?
O6 C5 O5 123.2(6) . . ?
O6 C5 C6 117.8(6) . . ?
N2 C8 C7 113.9(5) . . ?
N2 C8 H8A 108.8 . . ?
N2 C8 H8B 108.8 . . ?
C7 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
N2 C10 C9 111.3(6) . . ?
N2 C10 H10A 109.4 . . ?
N2 C10 H10B 109.4 . . ?
C9 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?

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
Pb1 O4 C3 O3 -145.6(5) . . . . ?
Pb1 O4 C3 C4 32.0(8) . . . . ?
Pb1 O8 C7 O7 -149.3(6) . . . . ?
Pb1 O8 C7 C8 26.8(7) . . . . ?
Pb1 O5 C5 O6 -168.5(5) . . . . ?
Pb1 O5 C5 C6 7.2(8) . . . . ?
Pb1 O2 C1 O1 -160.6(5) . . . . ?
Pb1 O2 C1 C2 17.6(8) . . . . ?
Pb1 N1 C2 C1 -45.0(5) . . . . ?
Pb1 N1 C4 C3 -29.9(6) . . . . ?
Pb1 N1 C9 C10 -46.3(6) . . . . ?
Pb1 N2 C6 C5 -40.4(6) . . . . ?
Pb1 N2 C8 C7 -41.7(6) . . . . ?
Pb1 N2 C10 C9 -44.0(6) . . . . ?
Pb2 O1 C1 O2 -100.5(7) . . . . ?
Pb2 O1 C1 C2 81.5(7) . . . . ?
Pb2 O8 C7 O7 -5.3(10) 1_465 . . . ?
Pb2 O8 C7 C8 170.7(4) 1_465 . . . ?
Pb2 O6 C5 O5 17.3(7) 1_455 . . . ?
Pb2 O6 C5 C6 -158.5(5) 1_455 . . . ?
Pb3 O3 C3 O4 -46.9(8) . . . . ?
Pb3 O3 C3 C4 135.4(5) . . . . ?
Pb3 O2 C1 O1 -19.7(7) 1_545 . . . ?
Pb3 O2 C1 C2 158.5(5) 1_545 . . . ?
O1 C1 C2 N1 -159.1(6) . . . . ?
O4 C3 C4 N1 -1.1(9) . . . . ?
O8 C7 C8 N2 12.3(8) . . . . ?
O3 C3 C4 N1 176.7(5) . . . . ?
O2 C1 C2 N1 22.7(8) . . . . ?
O7 C7 C8 N2 -171.2(6) . . . . ?
N1 C9 C10 N2 63.6(6) . . . . ?
C2 N1 C4 C3 86.4(6) . . . . ?
C2 N1 C9 C10 -160.8(5) . . . . ?
N2 C6 C5 O5 22.7(9) . . . . ?
N2 C6 C5 O6 -161.3(6) . . . . ?
C4 N1 C2 C1 -166.3(5) . . . . ?
C4 N1 C9 C10 77.0(7) . . . . ?
C6 N2 C8 C7 -161.2(5) . . . . ?
C6 N2 C10 C9 79.8(6) . . . . ?
C9 N1 C2 C1 71.6(7) . . . . ?
C9 N1 C4 C3 -150.5(5) . . . . ?
C8 N2 C6 C5 75.0(7) . . . . ?
C8 N2 C10 C9 -159.5(5) . . . . ?
C10 N2 C6 C5 -163.8(6) . . . . ?
C10 N2 C8 C7 77.3(7) . . . . ?

_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_exp_14372
_database_code_depnum_ccdc_archive 'CCDC 1533509'
_audit_update_record             
;
2017-02-18 deposited with the CCDC.
2017-04-06 downloaded from the CCDC.
;
_audit_creation_date             2017-02-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelxl_version_number           2014-7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H24 N4 O16 Pb4, 2(H2 O)'
_chemical_formula_sum            'C20 H28 N4 O18 Pb4'
_chemical_formula_weight         1441.22
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   8.4173(5)
_cell_length_b                   8.4523(6)
_cell_length_c                   11.0350(8)
_cell_angle_alpha                71.442(7)
_cell_angle_beta                 89.744(5)
_cell_angle_gamma                76.903(6)
_cell_volume                     722.96(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2111
_cell_measurement_temperature    178.7(7)
_cell_measurement_theta_max      27.9920
_cell_measurement_theta_min      3.7350
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.309
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.310
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5225
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.717
_diffrn_reflns_theta_min         3.051
_diffrn_ambient_temperature      178.7(7)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -88.00    2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -57.0000  -90.0000 90

#__ type_ start__ end____ width___ exp.time_
  2 omega  -44.00   50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747   57.0000   60.0000 94

#__ type_ start__ end____ width___ exp.time_
  3 omega    4.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747   57.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
  4 omega  -91.00    3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -57.0000  120.0000 94

#__ type_ start__ end____ width___ exp.time_
  5 omega   67.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809 -178.0000    0.0000 35

#__ type_ start__ end____ width___ exp.time_
  6 omega  -22.00    9.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809   99.0000  127.0000 31
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0143205000
_diffrn_orient_matrix_UB_12      -0.0763543000
_diffrn_orient_matrix_UB_13      -0.0164504000
_diffrn_orient_matrix_UB_21      -0.0187942000
_diffrn_orient_matrix_UB_22      -0.0456842000
_diffrn_orient_matrix_UB_23      0.0621881000
_diffrn_orient_matrix_UB_31      -0.0834710000
_diffrn_orient_matrix_UB_32      0.0196841000
_diffrn_orient_matrix_UB_33      -0.0220021000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2730
_reflns_number_total             3250
_reflns_odcompleteness_completeness 99.80
_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, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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         1.589
_refine_diff_density_min         -1.729
_refine_diff_density_rms         0.286
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3250
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0363
_refine_ls_restrained_S_all      1.040
_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)+(0.0081P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0721
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
3.a Free rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B), C8(H8A,H8B), C9(H9A,H9B), C6(H6A,H6B), C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.68833(4) 0.45508(4) 0.62452(3) 0.01350(10) Uani 1 1 d . . . . .
Pb2 Pb 0.18275(4) 0.04225(4) 0.65682(3) 0.01294(9) Uani 1 1 d . . . . .
O8 O 1.0651(8) 0.7878(8) 0.5615(6) 0.0230(15) Uani 1 1 d . . . . .
O4 O 0.9163(6) 0.1977(7) 0.7185(6) 0.0133(13) Uani 1 1 d . . . . .
O7 O 0.8658(7) 0.6747(8) 0.5244(6) 0.0206(14) Uani 1 1 d . . . . .
O2 O 0.4521(7) 0.2596(8) 0.6564(6) 0.0218(15) Uani 1 1 d . . . . .
O5 O 0.5006(7) 0.6519(8) 0.7003(6) 0.0212(15) Uani 1 1 d . . . . .
O1 O 0.2583(7) 0.1901(8) 0.7893(6) 0.0177(14) Uani 1 1 d . . . . .
O3 O 1.0006(7) -0.0697(8) 0.8503(6) 0.0182(14) Uani 1 1 d . . . . .
N1 N 0.6470(8) 0.2728(9) 0.8545(7) 0.0115(15) Uani 1 1 d . . . . .
C7 C 0.9758(10) 0.6886(11) 0.5947(8) 0.0147(19) Uani 1 1 d . . . . .
C4 C 0.7391(9) 0.0894(11) 0.8805(8) 0.0126(18) Uani 1 1 d . . . . .
H4A H 0.6692 0.0287 0.8528 0.015 Uiso 1 1 calc R . . . .
H4B H 0.7642 0.0352 0.9722 0.015 Uiso 1 1 calc R . . . .
N2 N 0.8372(8) 0.5390(8) 0.7836(6) 0.0092(14) Uani 1 1 d . . . . .
O6 O 0.4642(7) 0.8555(8) 0.7917(6) 0.0219(15) Uani 1 1 d . . . . .
C10 C 0.8597(10) 0.4037(11) 0.9086(8) 0.0131(18) Uani 1 1 d . . . . .
H10A H 0.8961 0.4460 0.9731 0.016 Uiso 1 1 calc R . . . .
H10B H 0.9442 0.3060 0.9056 0.016 Uiso 1 1 calc R . . . .
C3 C 0.8969(10) 0.0712(11) 0.8137(8) 0.0144(18) Uani 1 1 d . . . . .
C8 C 0.9963(10) 0.5706(11) 0.7338(8) 0.0135(18) Uani 1 1 d . . . . .
H8A H 1.0704 0.4617 0.7399 0.016 Uiso 1 1 calc R . . . .
H8B H 1.0449 0.6221 0.7866 0.016 Uiso 1 1 calc R . . . .
C9 C 0.7049(10) 0.3466(10) 0.9464(8) 0.0107(17) Uani 1 1 d . . . . .
H9A H 0.7239 0.2612 1.0312 0.013 Uiso 1 1 calc R . . . .
H9B H 0.6206 0.4441 0.9504 0.013 Uiso 1 1 calc R . . . .
C6 C 0.7369(9) 0.7033(10) 0.7929(8) 0.0100(17) Uani 1 1 d . U . . .
H6A H 0.7774 0.7971 0.7363 0.012 Uiso 1 1 calc R . . . .
H6B H 0.7526 0.7040 0.8798 0.012 Uiso 1 1 calc R . . . .
C1 C 0.3897(10) 0.2352(11) 0.7631(8) 0.0120(17) Uani 1 1 d . U . . .
C5 C 0.5524(10) 0.7376(11) 0.7593(9) 0.017(2) Uani 1 1 d . . . . .
C2 C 0.4701(9) 0.2750(11) 0.8692(9) 0.0131(18) Uani 1 1 d . . . . .
H2A H 0.4125 0.3874 0.8709 0.016 Uiso 1 1 calc R . . . .
H2B H 0.4593 0.1915 0.9507 0.016 Uiso 1 1 calc R . . . .
O1W O 0.3084(11) -0.0517(12) 0.4370(8) 0.050(2) Uani 1 1 d . . . . .
H1WA H 0.3984 -0.0317 0.4548 0.075 Uiso 1 1 d G . . . .
H1WB H 0.2820 -0.1241 0.5023 0.075 Uiso 1 1 d G . . . .


_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 O4 2.486(6) . ?
Pb1 O7 2.614(6) . ?
Pb1 O5 2.376(6) . ?
Pb1 N1 2.585(7) . ?
Pb1 N2 2.524(7) . ?
Pb2 O4 2.537(5) 1_455 ?
Pb2 O7 2.531(6) 2_666 ?
Pb2 O1 2.374(6) . ?
Pb2 O3 2.673(6) 1_455 ?
Pb2 O6 2.676(6) 1_545 ?
O8 C7 1.220(10) . ?
O4 Pb2 2.537(5) 1_655 ?
O4 C3 1.280(10) . ?
O7 Pb2 2.531(6) 2_666 ?
O7 C7 1.260(10) . ?
O2 C1 1.262(10) . ?
O5 C5 1.257(11) . ?
O1 C1 1.253(10) . ?
O3 Pb2 2.673(6) 1_655 ?
O3 C3 1.253(10) . ?
N1 C4 1.504(10) . ?
N1 C9 1.483(10) . ?
N1 C2 1.494(10) . ?
C7 C8 1.526(12) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.517(11) . ?
N2 C10 1.465(10) . ?
N2 C8 1.494(10) . ?
N2 C6 1.487(10) . ?
O6 Pb2 2.676(6) 1_565 ?
O6 C5 1.249(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.503(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.538(11) . ?
C1 C2 1.517(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O1W H1WA 0.8498 . ?
O1W H1WB 0.8498 . ?

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
O4 Pb1 O7 97.71(19) . . ?
O4 Pb1 N1 66.42(19) . . ?
O4 Pb1 N2 77.00(19) . . ?
O5 Pb1 O4 136.9(2) . . ?
O5 Pb1 O7 93.5(2) . . ?
O5 Pb1 N1 76.4(2) . . ?
O5 Pb1 N2 70.5(2) . . ?
N1 Pb1 O7 135.2(2) . . ?
N2 Pb1 O7 64.8(2) . . ?
N2 Pb1 N1 70.7(2) . . ?
O4 Pb2 O3 50.29(18) 1_455 1_455 ?
O4 Pb2 O6 132.59(19) 1_455 1_545 ?
O7 Pb2 O4 80.48(19) 2_666 1_455 ?
O7 Pb2 O3 130.70(18) 2_666 1_455 ?
O7 Pb2 O6 128.1(2) 2_666 1_545 ?
O1 Pb2 O4 74.26(18) . 1_455 ?
O1 Pb2 O7 86.7(2) . 2_666 ?
O1 Pb2 O3 82.8(2) . 1_455 ?
O1 Pb2 O6 71.37(19) . 1_545 ?
O3 Pb2 O6 93.44(18) 1_455 1_545 ?
Pb1 O4 Pb2 139.9(2) . 1_655 ?
C3 O4 Pb1 121.1(5) . . ?
C3 O4 Pb2 96.5(5) . 1_655 ?
Pb2 O7 Pb1 134.6(3) 2_666 . ?
C7 O7 Pb1 118.9(5) . . ?
C7 O7 Pb2 101.8(5) . 2_666 ?
C5 O5 Pb1 120.1(5) . . ?
C1 O1 Pb2 113.7(5) . . ?
C3 O3 Pb2 90.8(5) . 1_655 ?
C4 N1 Pb1 109.7(5) . . ?
C9 N1 Pb1 108.8(5) . . ?
C9 N1 C4 111.1(6) . . ?
C9 N1 C2 109.2(6) . . ?
C2 N1 Pb1 110.2(5) . . ?
C2 N1 C4 107.8(6) . . ?
O8 C7 O7 125.8(9) . . ?
O8 C7 C8 118.1(8) . . ?
O7 C7 C8 116.1(8) . . ?
N1 C4 H4A 108.9 . . ?
N1 C4 H4B 108.9 . . ?
N1 C4 C3 113.5(7) . . ?
H4A C4 H4B 107.7 . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
C10 N2 Pb1 109.5(5) . . ?
C10 N2 C8 112.0(6) . . ?
C10 N2 C6 110.4(6) . . ?
C8 N2 Pb1 109.0(5) . . ?
C6 N2 Pb1 108.0(4) . . ?
C6 N2 C8 107.8(6) . . ?
C5 O6 Pb2 120.7(6) . 1_565 ?
N2 C10 H10A 109.2 . . ?
N2 C10 H10B 109.2 . . ?
N2 C10 C9 112.0(7) . . ?
H10A C10 H10B 107.9 . . ?
C9 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
O4 C3 C4 118.9(7) . . ?
O3 C3 O4 122.2(8) . . ?
O3 C3 C4 118.8(8) . . ?
C7 C8 H8A 109.2 . . ?
C7 C8 H8B 109.2 . . ?
N2 C8 C7 112.1(6) . . ?
N2 C8 H8A 109.2 . . ?
N2 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
N1 C9 C10 111.8(7) . . ?
N1 C9 H9A 109.3 . . ?
N1 C9 H9B 109.3 . . ?
C10 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
N2 C6 H6A 108.4 . . ?
N2 C6 H6B 108.4 . . ?
N2 C6 C5 115.3(7) . . ?
H6A C6 H6B 107.5 . . ?
C5 C6 H6A 108.4 . . ?
C5 C6 H6B 108.4 . . ?
O2 C1 C2 119.1(7) . . ?
O1 C1 O2 126.0(8) . . ?
O1 C1 C2 114.8(7) . . ?
O5 C5 C6 119.9(8) . . ?
O6 C5 O5 124.7(8) . . ?
O6 C5 C6 115.4(8) . . ?
N1 C2 C1 113.6(7) . . ?
N1 C2 H2A 108.8 . . ?
N1 C2 H2B 108.8 . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
H1WA O1W H1WB 109.5 . . ?

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 O4 C3 O3 168.9(6) . . . . ?
Pb1 O4 C3 C4 -7.9(10) . . . . ?
Pb1 O7 C7 O8 -178.5(7) . . . . ?
Pb1 O7 C7 C8 1.1(9) . . . . ?
Pb1 O5 C5 O6 172.7(7) . . . . ?
Pb1 O5 C5 C6 -5.5(11) . . . . ?
Pb1 N1 C4 C3 33.5(8) . . . . ?
Pb1 N1 C9 C10 -40.3(7) . . . . ?
Pb1 N1 C2 C1 49.2(7) . . . . ?
Pb1 N2 C10 C9 -47.3(7) . . . . ?
Pb1 N2 C8 C7 48.9(8) . . . . ?
Pb1 N2 C6 C5 25.7(8) . . . . ?
Pb2 O4 C3 O3 3.4(9) 1_655 . . . ?
Pb2 O4 C3 C4 -173.4(7) 1_655 . . . ?
Pb2 O7 C7 O8 -19.4(10) 2_666 . . . ?
Pb2 O7 C7 C8 160.1(6) 2_666 . . . ?
Pb2 O1 C1 O2 24.0(11) . . . . ?
Pb2 O1 C1 C2 -160.6(5) . . . . ?
Pb2 O3 C3 O4 -3.2(9) 1_655 . . . ?
Pb2 O3 C3 C4 173.6(7) 1_655 . . . ?
Pb2 O6 C5 O5 -28.3(12) 1_565 . . . ?
Pb2 O6 C5 C6 150.0(5) 1_565 . . . ?
O8 C7 C8 N2 145.5(8) . . . . ?
O7 C7 C8 N2 -34.1(10) . . . . ?
O2 C1 C2 N1 -22.9(11) . . . . ?
O1 C1 C2 N1 161.4(7) . . . . ?
N1 C4 C3 O4 -19.0(11) . . . . ?
N1 C4 C3 O3 164.0(7) . . . . ?
C4 N1 C9 C10 80.6(8) . . . . ?
C4 N1 C2 C1 -70.6(9) . . . . ?
N2 C10 C9 N1 61.6(9) . . . . ?
N2 C6 C5 O5 -15.7(12) . . . . ?
N2 C6 C5 O6 165.9(7) . . . . ?
C10 N2 C8 C7 170.3(7) . . . . ?
C10 N2 C6 C5 -94.1(8) . . . . ?
C8 N2 C10 C9 -168.3(7) . . . . ?
C8 N2 C6 C5 143.3(7) . . . . ?
C9 N1 C4 C3 -86.8(8) . . . . ?
C9 N1 C2 C1 168.7(7) . . . . ?
C6 N2 C10 C9 71.5(8) . . . . ?
C6 N2 C8 C7 -68.0(8) . . . . ?
C2 N1 C4 C3 153.6(7) . . . . ?
C2 N1 C9 C10 -160.6(7) . . . . ?

_olex2_date_sample_data_collection 2016-08-07
_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_exp_13255
_database_code_depnum_ccdc_archive 'CCDC 1533512'
_audit_update_record             
;
2017-02-18 deposited with the CCDC.
2017-04-06 downloaded from the CCDC.
;
_audit_creation_date             2016-08-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C20 H28 Br2 N4 O18 Pb5, 2(H2 O)'
_chemical_formula_sum            'C20 H32 Br2 N4 O20 Pb5'
_chemical_formula_weight         1844.27
_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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   7.5998(10)
_cell_length_b                   8.8154(12)
_cell_length_c                   13.7290(18)
_cell_angle_alpha                72.365(12)
_cell_angle_beta                 80.702(11)
_cell_angle_gamma                75.351(11)
_cell_volume                     844.46(19)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1367
_cell_measurement_temperature    176.8(3)
_cell_measurement_theta_max      27.5690
_cell_measurement_theta_min      3.2190
_exptl_absorpt_coefficient_mu    27.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.627
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.1296
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5116
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.06
_diffrn_ambient_temperature      176.8(3)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -59.00    7.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -38.0000 -120.0000 66

#__ type_ start__ end____ width___ exp.time_
  2 omega  -44.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747   57.0000 -180.0000 87

#__ type_ start__ end____ width___ exp.time_
  3 omega  -12.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747   57.0000   90.0000 57

#__ type_ start__ end____ width___ exp.time_
  4 omega  -91.00   13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4747  -77.0000   30.0000 104

#__ type_ start__ end____ width___ exp.time_
  5 omega   -1.00   59.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809   57.0000  -90.0000 60

#__ type_ start__ end____ width___ exp.time_
  6 omega   39.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809  -99.0000  -60.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0387662000
_diffrn_orient_matrix_UB_12      0.0551913000
_diffrn_orient_matrix_UB_13      0.0300174000
_diffrn_orient_matrix_UB_21      -0.0069873000
_diffrn_orient_matrix_UB_22      -0.0665679000
_diffrn_orient_matrix_UB_23      0.0440350000
_diffrn_orient_matrix_UB_31      0.0885092000
_diffrn_orient_matrix_UB_32      -0.0016105000
_diffrn_orient_matrix_UB_33      0.0111334000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2380
_reflns_number_total             2969
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.863
_refine_diff_density_min         -4.158
_refine_diff_density_rms         0.549
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2969
_refine_ls_number_restraints     143
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0645
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0294P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1439
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H1WA-O1W = H1WB-O1W
 0.85 with sigma of 0.01
 H2WA-O2W = H2WB-O2W
 0.85 with sigma of 0.01
 H2WB-H2WA = H1WB-H1WA
 1.39 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
5.a Rotating group:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb1 Pb 0.27595(9) 0.61362(8) 0.33224(6) 0.0138(2) Uani 1 d . . 1 . U .
Pb2 Pb 0.48787(9) 1.13135(8) 0.32908(6) 0.0162(2) Uani 1 d . . 1 . U .
Pb3 Pb 0.0000 0.0000 0.5000 0.0178(3) Uani 1 d . . 2 S TU P
Br1 Br 0.6397(2) 1.2786(2) 0.46397(17) 0.0208(5) Uani 1 d . . 1 . U .
O1 O 0.1426(16) 0.3518(14) 0.3934(11) 0.019(3) Uani 1 d . . 1 . U .
O1W O 0.7727(16) 1.1509(15) 0.2188(12) 0.021(3) Uani 1 d . . 1 D U .
H1WA H 0.8622 1.1604 0.2520 0.031 Uiso 1 d . . 1 DGR . .
H1WB H 0.7575 1.2393 0.1631 0.031 Uiso 1 d . . 1 DGR . .
O2 O 0.0513(16) 0.1907(14) 0.3219(11) 0.019(3) Uani 1 d . . 1 . U .
O3 O 0.0323(16) 0.8287(15) 0.3706(12) 0.023(3) Uani 1 d . . 1 . U .
O4 O -0.2611(16) 0.9066(15) 0.4195(11) 0.018(3) Uani 1 d . . 1 . U .
O5 O 0.4283(17) 0.8735(14) 0.2677(12) 0.022(3) Uani 1 d . . 1 . U .
O6 O 0.4139(18) 1.1173(14) 0.1595(11) 0.023(3) Uani 1 d . . 1 . U .
O7 O 0.4210(16) 0.4375(14) 0.2149(11) 0.017(2) Uani 1 d . . 1 . U .
O8 O 0.6487(16) 0.4404(14) 0.0866(12) 0.022(3) Uani 1 d . . 1 . U .
N1 N -0.0326(18) 0.6302(16) 0.2686(13) 0.014(2) Uani 1 d . . 1 . U .
N2 N 0.2748(19) 0.7681(16) 0.1372(13) 0.012(2) Uani 1 d . . 1 . U .
C1 C 0.056(2) 0.330(2) 0.3295(18) 0.020(4) Uani 1 d . . 1 . U .
C2 C -0.050(2) 0.478(2) 0.2508(16) 0.015(3) Uani 1 d . . 1 . U .
H2A H -0.0002 0.4750 0.1816 0.017 Uiso 1 calc . . 1 R . .
H2B H -0.1774 0.4731 0.2585 0.017 Uiso 1 calc . . 1 R . .
C3 C -0.172(2) 0.686(2) 0.3441(16) 0.013(3) Uani 1 d . . 1 . U .
H3A H -0.1843 0.5934 0.4028 0.016 Uiso 1 calc . . 1 R . .
H3B H -0.2881 0.7258 0.3142 0.016 Uiso 1 calc . . 1 R . .
C4 C -0.136(2) 0.8160(19) 0.3805(15) 0.010(3) Uani 1 d . . 1 . U .
C5 C 0.382(2) 0.979(2) 0.1864(16) 0.014(3) Uani 1 d . . 1 . U .
C6 C 0.270(2) 0.945(2) 0.1172(16) 0.015(3) Uani 1 d . . 1 . U .
H6A H 0.1440 1.0020 0.1265 0.018 Uiso 1 calc . . 1 R . .
H6B H 0.3150 0.9870 0.0464 0.018 Uiso 1 calc . . 1 R . .
C7 C 0.508(3) 0.506(2) 0.1351(15) 0.016(4) Uani 1 d . . 1 . U .
C8 C 0.456(2) 0.688(2) 0.0921(16) 0.014(3) Uani 1 d . . 1 . U .
H8A H 0.4518 0.7132 0.0185 0.017 Uiso 1 calc . . 1 R . .
H8B H 0.5501 0.7356 0.1034 0.017 Uiso 1 calc . . 1 R . .
C9 C -0.048(2) 0.760(2) 0.1636(16) 0.016(3) Uani 1 d . . 1 . U .
H9A H -0.1486 0.7520 0.1311 0.019 Uiso 1 calc . . 1 R . .
H9B H -0.0763 0.8681 0.1744 0.019 Uiso 1 calc . . 1 R . .
C10 C 0.123(2) 0.741(2) 0.0937(17) 0.019(3) Uani 1 d . . 1 . U .
H10A H 0.1540 0.6327 0.0843 0.023 Uiso 1 calc . . 1 R . .
H10B H 0.1045 0.8194 0.0270 0.023 Uiso 1 calc . . 1 R . .
O2W O 0.126(2) 1.3491(17) 0.0437(13) 0.031(4) Uani 1 d . . 1 D U .
H2WA H 0.14(2) 1.28(2) 0.103(8) 0.047 Uiso 1 d . . 1 DR . .
H2WB H 0.222(15) 1.39(2) 0.018(14) 0.047 Uiso 1 d . . 1 DR . .


_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 O1 2.606(12) . ?
Pb1 O3 2.411(12) . ?
Pb1 O5 2.675(11) . ?
Pb1 O7 2.509(13) . ?
Pb1 N1 2.587(14) . ?
Pb1 N2 2.611(16) . ?
Pb2 Br1 3.058(2) . ?
Pb2 O1W 2.445(13) . ?
Pb2 O4 2.544(13) 1_655 ?
Pb2 O6 2.527(15) . ?
Pb2 O7 2.646(12) 1_565 ?
Pb3 Br1 3.1738(19) 1_445 ?
Pb3 Br1 3.1738(19) 2_666 ?
Pb3 O2 2.548(14) . ?
Pb3 O2 2.548(14) 2_556 ?
Pb3 O3 2.607(14) 1_545 ?
Pb3 O3 2.607(14) 2_566 ?
Br1 Pb3 3.1738(19) 1_665 ?
O1 C1 1.26(2) . ?
O1W H1WA 0.9108 . ?
O1W H1WB 0.9094 . ?
O2 C1 1.27(2) . ?
O3 Pb3 2.607(14) 1_565 ?
O3 C4 1.29(2) . ?
O4 Pb2 2.544(12) 1_455 ?
O4 C4 1.24(2) . ?
O5 C5 1.25(2) . ?
O6 C5 1.24(2) . ?
O7 Pb2 2.646(12) 1_545 ?
O7 C7 1.25(2) . ?
O8 C7 1.27(2) . ?
N1 C2 1.47(2) . ?
N1 C3 1.46(2) . ?
N1 C9 1.55(2) . ?
N2 C6 1.49(2) . ?
N2 C8 1.51(2) . ?
N2 C10 1.48(2) . ?
C1 C2 1.55(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.48(2) . ?
C5 C6 1.51(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.50(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.49(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O2W H2WA 0.850(10) . ?
O2W H2WB 0.851(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O5 177.3(4) . . ?
O1 Pb1 N2 116.8(4) . . ?
O3 Pb1 O1 105.6(4) . . ?
O3 Pb1 O5 77.1(4) . . ?
O3 Pb1 O7 148.8(5) . . ?
O3 Pb1 N1 65.9(4) . . ?
O3 Pb1 N2 89.8(5) . . ?
O7 Pb1 O1 72.1(4) . . ?
O7 Pb1 O5 105.8(4) . . ?
O7 Pb1 N1 86.9(4) . . ?
O7 Pb1 N2 65.7(4) . . ?
N1 Pb1 O1 62.5(4) . . ?
N1 Pb1 O5 119.4(4) . . ?
N1 Pb1 N2 70.2(5) . . ?
N2 Pb1 O5 63.2(4) . . ?
O1W Pb2 Br1 85.8(3) . . ?
O1W Pb2 O4 72.7(4) . 1_655 ?
O1W Pb2 O6 76.4(5) . . ?
O1W Pb2 O7 77.0(4) . 1_565 ?
O4 Pb2 Br1 73.9(3) 1_655 . ?
O4 Pb2 O7 142.4(4) 1_655 1_565 ?
O6 Pb2 Br1 153.7(3) . . ?
O6 Pb2 O4 117.6(4) . 1_655 ?
O6 Pb2 O7 75.1(4) . 1_565 ?
O7 Pb2 Br1 82.3(3) 1_565 . ?
Br1 Pb3 Br1 180.0 2_666 1_445 ?
O2 Pb3 Br1 73.3(3) . 1_445 ?
O2 Pb3 Br1 106.7(3) . 2_666 ?
O2 Pb3 Br1 106.7(3) 2_556 1_445 ?
O2 Pb3 Br1 73.3(3) 2_556 2_666 ?
O2 Pb3 O2 180.000(1) 2_556 . ?
O2 Pb3 O3 106.3(4) 2_556 1_545 ?
O2 Pb3 O3 106.3(4) . 2_566 ?
O2 Pb3 O3 73.7(4) . 1_545 ?
O2 Pb3 O3 73.7(4) 2_556 2_566 ?
O3 Pb3 Br1 71.5(3) 2_566 1_445 ?
O3 Pb3 Br1 108.5(3) 1_545 1_445 ?
O3 Pb3 Br1 71.5(3) 1_545 2_666 ?
O3 Pb3 Br1 108.5(3) 2_566 2_666 ?
O3 Pb3 O3 180.000(1) 2_566 1_545 ?
Pb2 Br1 Pb3 94.72(5) . 1_665 ?
C1 O1 Pb1 115.7(12) . . ?
Pb2 O1W H1WA 112.5 . . ?
Pb2 O1W H1WB 111.8 . . ?
H1WA O1W H1WB 106.5 . . ?
C1 O2 Pb3 109.7(14) . . ?
Pb1 O3 Pb3 131.1(6) . 1_565 ?
C4 O3 Pb1 120.4(10) . . ?
C4 O3 Pb3 97.9(11) . 1_565 ?
C4 O4 Pb2 127.4(12) . 1_455 ?
C5 O5 Pb1 118.4(11) . . ?
C5 O6 Pb2 99.4(13) . . ?
Pb1 O7 Pb2 107.5(5) . 1_545 ?
C7 O7 Pb1 114.7(10) . . ?
C7 O7 Pb2 130.0(11) . 1_545 ?
C2 N1 Pb1 114.3(10) . . ?
C2 N1 C9 106.2(15) . . ?
C3 N1 Pb1 105.3(11) . . ?
C3 N1 C2 113.8(13) . . ?
C3 N1 C9 109.4(13) . . ?
C9 N1 Pb1 107.8(9) . . ?
C6 N2 Pb1 112.4(12) . . ?
C6 N2 C8 108.8(13) . . ?
C8 N2 Pb1 103.0(10) . . ?
C10 N2 Pb1 110.3(11) . . ?
C10 N2 C6 111.8(14) . . ?
C10 N2 C8 110.3(14) . . ?
O1 C1 O2 124.4(17) . . ?
O1 C1 C2 120.3(15) . . ?
O2 C1 C2 115.3(18) . . ?
N1 C2 C1 109.4(16) . . ?
N1 C2 H2A 109.8 . . ?
N1 C2 H2B 109.8 . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
N1 C3 H3A 108.5 . . ?
N1 C3 H3B 108.5 . . ?
N1 C3 C4 114.9(14) . . ?
H3A C3 H3B 107.5 . . ?
C4 C3 H3A 108.5 . . ?
C4 C3 H3B 108.5 . . ?
O3 C4 C3 116.7(15) . . ?
O4 C4 O3 122.2(15) . . ?
O4 C4 C3 121.2(15) . . ?
O5 C5 C6 120.2(15) . . ?
O6 C5 O5 124.1(18) . . ?
O6 C5 C6 115.7(17) . . ?
N2 C6 C5 113.3(15) . . ?
N2 C6 H6A 108.9 . . ?
N2 C6 H6B 108.9 . . ?
C5 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
O7 C7 O8 127.1(16) . . ?
O7 C7 C8 119.7(16) . . ?
O8 C7 C8 113.1(15) . . ?
N2 C8 H8A 108.6 . . ?
N2 C8 H8B 108.6 . . ?
C7 C8 N2 114.7(15) . . ?
C7 C8 H8A 108.6 . . ?
C7 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
N1 C9 H9A 109.2 . . ?
N1 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 N1 112.1(15) . . ?
C10 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
N2 C10 C9 110.3(17) . . ?
N2 C10 H10A 109.6 . . ?
N2 C10 H10B 109.6 . . ?
C9 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
H2WA O2W H2WB 109.6(19) . . ?

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 O1 C1 O2 147.4(16) . . . . ?
Pb1 O1 C1 C2 -31(2) . . . . ?
Pb1 O3 C4 O4 165.5(13) . . . . ?
Pb1 O3 C4 C3 -14(2) . . . . ?
Pb1 O5 C5 O6 165.3(14) . . . . ?
Pb1 O5 C5 C6 -11(2) . . . . ?
Pb1 O7 C7 O8 148.3(16) . . . . ?
Pb1 O7 C7 C8 -27(2) . . . . ?
Pb1 N1 C2 C1 33.3(18) . . . . ?
Pb1 N1 C3 C4 41.2(17) . . . . ?
Pb1 N1 C9 C10 46.3(16) . . . . ?
Pb1 N2 C6 C5 37.3(17) . . . . ?
Pb1 N2 C8 C7 40.9(17) . . . . ?
Pb1 N2 C10 C9 45.0(16) . . . . ?
Pb2 O4 C4 O3 109.4(18) 1_455 . . . ?
Pb2 O4 C4 C3 -71(2) 1_455 . . . ?
Pb2 O6 C5 O5 -17(2) . . . . ?
Pb2 O6 C5 C6 159.6(13) . . . . ?
Pb2 O7 C7 O8 3(3) 1_545 . . . ?
Pb2 O7 C7 C8 -171.7(12) 1_545 . . . ?
Pb3 O2 C1 O1 45(2) . . . . ?
Pb3 O2 C1 C2 -137.2(14) . . . . ?
Pb3 O3 C4 O4 17.1(19) 1_565 . . . ?
Pb3 O3 C4 C3 -162.2(14) 1_565 . . . ?
Br1 Pb2 O6 C5 165.9(8) . . . . ?
Br1 Pb3 O2 C1 -114.1(10) 2_666 . . . ?
Br1 Pb3 O2 C1 65.9(10) 1_445 . . . ?
O1 Pb1 O3 Pb3 113.6(7) . . . 1_565 ?
O1 Pb1 O3 C4 -22.8(15) . . . . ?
O1 Pb1 O5 C5 113(9) . . . . ?
O1 Pb1 O7 Pb2 -39.7(4) . . . 1_545 ?
O1 Pb1 O7 C7 167.8(13) . . . . ?
O1 Pb1 N1 C2 -34.3(12) . . . . ?
O1 Pb1 N1 C3 91.3(11) . . . . ?
O1 Pb1 N1 C9 -152.0(12) . . . . ?
O1 Pb1 N2 C6 153.6(10) . . . . ?
O1 Pb1 N2 C8 -89.5(9) . . . . ?
O1 Pb1 N2 C10 28.2(12) . . . . ?
O1 C1 C2 N1 -2(2) . . . . ?
O1W Pb2 Br1 Pb3 -57.6(3) . . . 1_665 ?
O1W Pb2 O6 C5 117.2(11) . . . . ?
O2 Pb3 O2 C1 10(100) 2_556 . . . ?
O2 C1 C2 N1 180.0(15) . . . . ?
O3 Pb1 O1 C1 85.9(13) . . . . ?
O3 Pb1 O5 C5 -73.9(14) . . . . ?
O3 Pb1 O7 Pb2 -130.2(7) . . . 1_545 ?
O3 Pb1 O7 C7 77.2(15) . . . . ?
O3 Pb1 N1 C2 -158.6(14) . . . . ?
O3 Pb1 N1 C3 -33.1(10) . . . . ?
O3 Pb1 N1 C9 83.7(10) . . . . ?
O3 Pb1 N2 C6 46.3(10) . . . . ?
O3 Pb1 N2 C8 163.1(9) . . . . ?
O3 Pb1 N2 C10 -79.2(11) . . . . ?
O3 Pb3 O2 C1 -178.4(11) 1_545 . . . ?
O3 Pb3 O2 C1 1.6(11) 2_566 . . . ?
O4 Pb2 Br1 Pb3 15.7(3) 1_655 . . 1_665 ?
O4 Pb2 O6 C5 55.3(12) 1_655 . . . ?
O5 Pb1 O1 C1 -101(10) . . . . ?
O5 Pb1 O3 Pb3 -66.1(7) . . . 1_565 ?
O5 Pb1 O3 C4 157.5(15) . . . . ?
O5 Pb1 O7 Pb2 138.6(4) . . . 1_545 ?
O5 Pb1 O7 C7 -14.0(14) . . . . ?
O5 Pb1 N1 C2 143.5(12) . . . . ?
O5 Pb1 N1 C3 -90.9(11) . . . . ?
O5 Pb1 N1 C9 25.8(12) . . . . ?
O5 Pb1 N2 C6 -29.4(10) . . . . ?
O5 Pb1 N2 C8 87.5(9) . . . . ?
O5 Pb1 N2 C10 -154.9(12) . . . . ?
O5 C5 C6 N2 -18(2) . . . . ?
O6 Pb2 Br1 Pb3 -104.6(7) . . . 1_665 ?
O6 C5 C6 N2 165.3(16) . . . . ?
O7 Pb1 O1 C1 -61.6(13) . . . . ?
O7 Pb1 O3 Pb3 -165.4(6) . . . 1_565 ?
O7 Pb1 O3 C4 58.1(18) . . . . ?
O7 Pb1 O5 C5 74.0(14) . . . . ?
O7 Pb1 N1 C2 37.1(12) . . . . ?
O7 Pb1 N1 C3 162.7(10) . . . . ?
O7 Pb1 N1 C9 -80.6(10) . . . . ?
O7 Pb1 N2 C6 -153.7(11) . . . . ?
O7 Pb1 N2 C8 -36.8(9) . . . . ?
O7 Pb1 N2 C10 80.9(11) . . . . ?
O7 Pb2 Br1 Pb3 -135.0(3) 1_565 . . 1_665 ?
O7 Pb2 O6 C5 -162.8(12) 1_565 . . . ?
O7 C7 C8 N2 -13(3) . . . . ?
O8 C7 C8 N2 171.5(16) . . . . ?
N1 Pb1 O1 C1 34.4(12) . . . . ?
N1 Pb1 O3 Pb3 163.1(9) . . . 1_565 ?
N1 Pb1 O3 C4 26.7(14) . . . . ?
N1 Pb1 O5 C5 -21.5(15) . . . . ?
N1 Pb1 O7 Pb2 -101.8(5) . . . 1_545 ?
N1 Pb1 O7 C7 105.7(13) . . . . ?
N1 Pb1 N2 C6 110.6(11) . . . . ?
N1 Pb1 N2 C8 -132.5(10) . . . . ?
N1 Pb1 N2 C10 -14.9(10) . . . . ?
N1 C3 C4 O3 -22(2) . . . . ?
N1 C3 C4 O4 158.7(17) . . . . ?
N1 C9 C10 N2 -63.8(19) . . . . ?
N2 Pb1 O1 C1 -11.9(13) . . . . ?
N2 Pb1 O3 Pb3 -128.6(7) . . . 1_565 ?
N2 Pb1 O3 C4 95.0(14) . . . . ?
N2 Pb1 O5 C5 22.4(13) . . . . ?
N2 Pb1 O7 Pb2 -171.4(6) . . . 1_545 ?
N2 Pb1 O7 C7 36.0(13) . . . . ?
N2 Pb1 N1 C2 102.4(13) . . . . ?
N2 Pb1 N1 C3 -132.1(11) . . . . ?
N2 Pb1 N1 C9 -15.3(10) . . . . ?
C2 N1 C3 C4 167.0(15) . . . . ?
C2 N1 C9 C10 -76.6(18) . . . . ?
C3 N1 C2 C1 -87.7(18) . . . . ?
C3 N1 C9 C10 160.2(15) . . . . ?
C6 N2 C8 C7 160.3(17) . . . . ?
C6 N2 C10 C9 -80.7(19) . . . . ?
C8 N2 C6 C5 -76.0(19) . . . . ?
C8 N2 C10 C9 158.1(14) . . . . ?
C9 N1 C2 C1 151.9(14) . . . . ?
C9 N1 C3 C4 -74.4(19) . . . . ?
C10 N2 C6 C5 161.9(16) . . . . ?
C10 N2 C8 C7 -77(2) . . . . ?

_olex2_date_sample_data_collection 2016-05-14
_olex2_submission_special_instructions 'No special instructions were received'
