# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2012


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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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data_d:\determination\solution\c175\khc175
_database_code_depnum_ccdc_archive 'CCDC 869337'
#TrackingRef 'khc175.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H48 N20 O18 Pb3'
_chemical_formula_weight         1790.64

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'

_symmetry_cell_setting           Monocl;inic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   30.9991(10)
_cell_length_b                   10.1021(4)
_cell_length_c                   20.4318(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.727(3)
_cell_angle_gamma                90.00
_cell_volume                     5984.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    20328
_cell_measurement_theta_min      2.10
_cell_measurement_theta_max      29.16

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3416
_exptl_absorpt_coefficient_mu    8.505
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.130
_exptl_absorpt_correction_T_max  0.220
_exptl_absorpt_process_details   'shape of crystal determined optically'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean '0.15 mm'
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20328
_diffrn_reflns_av_R_equivalents  0.1613
_diffrn_reflns_av_sigmaI/netI    0.1538
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         29.16
_reflns_number_total             8045
_reflns_number_gt                5075
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_cell_refinement       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_data_reduction        'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+380.8544P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8045
_refine_ls_number_parameters     394
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1702
_refine_ls_R_factor_gt           0.1076
_refine_ls_wR_factor_ref         0.2286
_refine_ls_wR_factor_gt          0.2029
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0749(6) 0.583(2) 0.1432(11) 0.040(5) Uani 1 1 d . . .
H1 H 0.0487 0.5330 0.1377 0.049 Uiso 1 1 calc R . .
C2 C 0.1154(7) 0.5226(18) 0.1442(12) 0.038(5) Uani 1 1 d . . .
H2 H 0.1149 0.4314 0.1378 0.045 Uiso 1 1 calc R . .
C3 C 0.1526(6) 0.719(2) 0.1588(9) 0.034(5) Uani 1 1 d . . .
H3 H 0.1792 0.7664 0.1633 0.041 Uiso 1 1 calc R . .
C4 C 0.1140(7) 0.789(2) 0.1577(9) 0.033(4) Uani 1 1 d . . .
H4 H 0.1150 0.8807 0.1615 0.040 Uiso 1 1 calc R . .
C5 C 0.0743(6) 0.7211(19) 0.1507(9) 0.028(4) Uani 1 1 d . . .
C6 C 0.0318(6) 0.7858(19) 0.1538(8) 0.028(4) Uani 1 1 d . . .
C7 C 0.0344(6) 0.928(2) 0.1753(9) 0.033(4) Uani 1 1 d . . .
H7A H 0.0434 0.9814 0.1432 0.039 Uiso 1 1 calc R . .
H7B H 0.0567 0.9382 0.2216 0.039 Uiso 1 1 calc R . .
H7C H 0.0047 0.9569 0.1748 0.039 Uiso 1 1 calc R . .
C8 C -0.0754(16) 0.552(4) 0.127(4) 0.23(4) Uani 1 1 d . . .
H8A H -0.0484 0.5112 0.1601 0.273 Uiso 1 1 calc R . .
H8B H -0.0757 0.5395 0.0807 0.273 Uiso 1 1 calc R . .
H8C H -0.1025 0.5127 0.1316 0.273 Uiso 1 1 calc R . .
C9 C -0.0748(8) 0.699(2) 0.1430(15) 0.050(6) Uani 1 1 d . . .
C10 C -0.1178(6) 0.751(2) 0.1477(8) 0.028(4) Uani 1 1 d . . .
C11 C -0.1525(7) 0.667(2) 0.1512(10) 0.038(5) Uani 1 1 d . . .
H11 H -0.1491 0.5758 0.1507 0.046 Uiso 1 1 calc R . .
C12 C -0.1933(9) 0.724(2) 0.1557(10) 0.042(5) Uani 1 1 d . . .
H12 H -0.2173 0.6690 0.1556 0.051 Uiso 1 1 calc R . .
C13 C -0.1653(7) 0.934(2) 0.1584(9) 0.034(5) Uani 1 1 d . . .
H13 H -0.1692 1.0240 0.1631 0.041 Uiso 1 1 calc R . .
C14 C -0.1246(6) 0.886(2) 0.1499(9) 0.030(4) Uani 1 1 d . . .
H14 H -0.1026 0.9446 0.1457 0.036 Uiso 1 1 calc R . .
C15 C 0.4055(7) 0.630(3) 0.0272(9) 0.045(6) Uani 1 1 d . . .
H15 H 0.4331 0.6767 0.0432 0.054 Uiso 1 1 calc R . .
C16 C 0.3657(7) 0.687(2) 0.0324(10) 0.039(5) Uani 1 1 d . . .
H16 H 0.3665 0.7717 0.0500 0.047 Uiso 1 1 calc R . .
C17 C 0.3245(6) 0.499(2) -0.0159(8) 0.038(5) Uani 1 1 d . . .
H17 H 0.2962 0.4550 -0.0325 0.046 Uiso 1 1 calc R . .
C18 C 0.3624(6) 0.433(2) -0.0223(8) 0.031(4) Uani 1 1 d . . .
H18 H 0.3600 0.3472 -0.0391 0.037 Uiso 1 1 calc R . .
C19 C 0.4038(6) 0.502(2) -0.0025(8) 0.028(4) Uani 1 1 d . . .
C20 C 0.4465(7) 0.447(3) -0.0110(9) 0.042(5) Uani 1 1 d . . .
C21 C 0.4442(7) 0.310(2) -0.0376(11) 0.042(5) Uani 1 1 d . . .
H21A H 0.4206 0.3045 -0.0831 0.050 Uiso 1 1 calc R . .
H21B H 0.4371 0.2507 -0.0062 0.050 Uiso 1 1 calc R . .
H21C H 0.4734 0.2866 -0.0407 0.050 Uiso 1 1 calc R . .
C22 C 0.5825(11) 0.742(4) 0.2583(17) 0.087(10) Uani 1 1 d . . .
H22B H 0.5862 0.6488 0.2668 0.104 Uiso 1 1 calc R . .
H22C H 0.5865 0.7875 0.3014 0.104 Uiso 1 1 calc R . .
H22A H 0.6052 0.7731 0.2398 0.104 Uiso 1 1 calc R . .
C23 C 0.5370(12) 0.769(4) 0.209(2) 0.110(16) Uani 1 1 d . . .
N1 N 0.1544(5) 0.5856(16) 0.1537(8) 0.031(4) Uani 1 1 d . . .
N2 N -0.0041(5) 0.7107(14) 0.1382(8) 0.028(3) Uani 1 1 d . . .
N3 N -0.0435(5) 0.7741(17) 0.1442(9) 0.033(4) Uani 1 1 d . . .
N4 N -0.1977(5) 0.849(2) 0.1598(8) 0.036(4) Uani 1 1 d . . .
N5 N 0.3254(6) 0.6149(19) 0.0112(8) 0.038(4) Uani 1 1 d . . .
N6 N 0.4806(5) 0.5269(17) 0.0049(8) 0.035(4) Uani 1 1 d . . .
N7 N 0.2102(6) 0.490(2) 0.0438(9) 0.039(4) Uani 1 1 d . . .
N8 N 0.2051(6) 0.3543(18) 0.3389(8) 0.033(4) Uani 1 1 d . . .
N9 N 0.1951(5) 0.1540(16) 0.2041(7) 0.028(3) Uani 1 1 d . . .
N10 N 0.5008(13) 0.782(4) 0.160(2) 0.118(12) Uani 1 1 d . . .
O1 O 0.1942(6) 0.3876(16) 0.0622(7) 0.048(4) Uani 1 1 d . . .
O2 O 0.2329(5) 0.5772(15) 0.0886(6) 0.042(4) Uani 1 1 d . . .
O3 O 0.2056(8) 0.515(2) -0.0193(7) 0.073(6) Uani 1 1 d . . .
O4 O 0.1814(5) 0.4065(16) 0.2819(7) 0.043(4) Uani 1 1 d . . .
O5 O 0.2467(5) 0.3821(17) 0.3682(7) 0.044(4) Uani 1 1 d . . .
O6 O 0.1855(5) 0.2794(16) 0.3689(7) 0.045(4) Uani 1 1 d . . .
O7 O 0.2365(4) 0.1807(12) 0.2398(7) 0.030(3) Uani 1 1 d . . .
O8 O 0.1726(5) 0.2395(15) 0.1615(6) 0.040(3) Uani 1 1 d . . .
O9 O 0.1801(5) 0.0429(15) 0.2089(7) 0.039(3) Uani 1 1 d . . .
Pb1 Pb 0.23125(2) 0.44599(7) 0.19736(3) 0.02505(17) Uani 1 1 d . . .
Pb2 Pb 0.2500 0.7500 0.0000 0.0318(3) Uani 1 2 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.021(9) 0.048(14) 0.051(11) -0.031(10) 0.012(8) -0.017(9)
C2 0.030(10) 0.014(9) 0.077(14) -0.005(9) 0.029(10) -0.003(7)
C3 0.024(9) 0.048(13) 0.031(9) -0.009(9) 0.009(7) -0.007(9)
C4 0.033(10) 0.035(11) 0.028(8) 0.009(8) 0.005(7) 0.006(8)
C5 0.029(9) 0.024(10) 0.029(8) 0.005(7) 0.008(7) 0.004(7)
C6 0.034(9) 0.029(10) 0.018(7) 0.003(7) 0.005(7) 0.019(8)
C7 0.017(8) 0.049(13) 0.033(9) 0.004(9) 0.010(7) -0.001(8)
C8 0.13(4) 0.037(19) 0.60(13) -0.02(4) 0.23(6) 0.02(2)
C9 0.044(12) 0.027(11) 0.099(19) -0.008(12) 0.049(13) 0.002(10)
C10 0.034(9) 0.032(10) 0.022(7) -0.009(7) 0.016(7) -0.009(9)
C11 0.048(12) 0.030(11) 0.043(10) -0.013(9) 0.025(9) -0.002(9)
C12 0.074(16) 0.026(11) 0.046(11) -0.013(9) 0.047(11) -0.014(11)
C13 0.038(10) 0.042(12) 0.026(8) 0.016(8) 0.016(7) 0.026(10)
C14 0.024(9) 0.034(11) 0.032(9) 0.004(8) 0.012(7) 0.007(8)
C15 0.023(9) 0.084(18) 0.030(9) 0.008(11) 0.010(8) 0.012(11)
C16 0.029(10) 0.046(13) 0.038(10) -0.023(9) 0.007(8) -0.001(9)
C17 0.022(9) 0.072(15) 0.014(7) 0.016(8) -0.003(6) 0.023(9)
C18 0.033(9) 0.035(11) 0.022(7) 0.001(8) 0.007(7) 0.005(9)
C19 0.020(8) 0.044(11) 0.015(7) -0.017(7) -0.001(6) 0.000(8)
C20 0.032(9) 0.068(15) 0.023(8) -0.029(10) 0.006(7) -0.008(11)
C21 0.033(10) 0.052(14) 0.043(11) 0.006(10) 0.017(9) 0.003(10)
C22 0.07(2) 0.09(2) 0.09(2) -0.03(2) 0.019(17) -0.01(2)
C23 0.06(2) 0.06(2) 0.17(4) 0.02(2) -0.01(2) -0.016(18)
N1 0.027(8) 0.029(9) 0.034(8) -0.007(6) 0.009(6) 0.001(6)
N2 0.022(7) 0.011(7) 0.053(9) -0.005(6) 0.018(7) 0.001(6)
N3 0.021(7) 0.031(9) 0.049(9) 0.002(7) 0.016(7) 0.005(7)
N4 0.017(7) 0.057(12) 0.036(8) -0.008(8) 0.012(6) 0.003(8)
N5 0.029(8) 0.049(11) 0.035(8) -0.009(8) 0.010(7) 0.003(8)
N6 0.032(8) 0.039(10) 0.034(8) -0.003(7) 0.013(7) 0.003(7)
N7 0.027(8) 0.055(12) 0.036(8) -0.014(8) 0.013(7) 0.004(8)
N8 0.047(10) 0.031(9) 0.032(8) -0.014(7) 0.026(7) -0.006(8)
N9 0.039(8) 0.030(8) 0.017(6) 0.004(6) 0.011(6) 0.006(7)
N10 0.10(3) 0.11(3) 0.14(3) -0.05(2) 0.04(2) -0.02(2)
O1 0.064(11) 0.038(9) 0.037(7) -0.001(7) 0.013(7) -0.009(8)
O2 0.052(9) 0.048(10) 0.027(6) 0.010(6) 0.015(6) -0.007(7)
O3 0.106(16) 0.092(16) 0.021(7) -0.001(8) 0.022(8) -0.013(13)
O4 0.046(8) 0.050(10) 0.034(7) 0.006(6) 0.015(6) 0.002(7)
O5 0.031(7) 0.062(11) 0.037(7) -0.014(7) 0.008(6) -0.017(7)
O6 0.044(8) 0.046(10) 0.048(8) 0.001(7) 0.021(7) -0.008(7)
O7 0.011(5) 0.018(6) 0.057(8) -0.001(6) 0.006(5) -0.001(5)
O8 0.041(8) 0.037(8) 0.029(6) 0.004(6) -0.005(6) -0.001(7)
O9 0.037(7) 0.034(8) 0.043(7) 0.018(7) 0.008(6) -0.012(7)
Pb1 0.0199(3) 0.0268(3) 0.0276(3) -0.0018(3) 0.0074(2) -0.0003(3)
Pb2 0.0296(5) 0.0413(6) 0.0274(4) 0.0084(4) 0.0138(4) 0.0082(5)

_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
C1 C2 1.39(3) . ?
C1 C5 1.40(3) . ?
C1 H1 0.9300 . ?
C2 N1 1.32(2) . ?
C2 H2 0.9300 . ?
C3 N1 1.35(3) . ?
C3 C4 1.38(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.37(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.49(2) . ?
C6 N2 1.29(2) . ?
C6 C7 1.50(3) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.52(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N3 1.22(3) . ?
C9 C10 1.47(3) . ?
C10 C14 1.38(3) . ?
C10 C11 1.39(3) . ?
C11 C12 1.42(3) . ?
C11 H11 0.9300 . ?
C12 N4 1.28(3) . ?
C12 H12 0.9300 . ?
C13 N4 1.33(3) . ?
C13 C14 1.42(2) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.39(3) . ?
C15 C19 1.43(3) . ?
C15 H15 0.9300 . ?
C16 N5 1.38(3) . ?
C16 H16 0.9300 . ?
C17 N5 1.30(3) . ?
C17 C18 1.39(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.39(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.50(3) . ?
C20 N6 1.28(3) . ?
C20 C21 1.47(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.44(4) . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C22 H22A 0.9600 . ?
C23 N10 1.21(4) . ?
N1 Pb1 2.638(16) . ?
N2 N3 1.42(2) . ?
N4 Pb1 2.756(15) 3_455 ?
N5 Pb2 2.645(17) . ?
N6 N6 1.40(3) 5_665 ?
N7 O1 1.26(2) . ?
N7 O3 1.27(2) . ?
N7 O2 1.29(2) . ?
N8 O5 1.25(2) . ?
N8 O4 1.25(2) . ?
N8 O6 1.26(2) . ?
N9 O9 1.23(2) . ?
N9 O8 1.249(19) . ?
N9 O7 1.261(18) . ?
O1 Pb1 2.654(14) . ?
O2 Pb1 2.604(12) . ?
O2 Pb2 2.698(13) . ?
O3 Pb2 2.70(2) . ?
O4 Pb1 2.725(14) . ?
O6 Pb2 2.733(15) 4_545 ?
O7 Pb1 2.713(12) 4_545 ?
O8 Pb1 2.693(15) . ?
Pb1 O7 2.713(12) 4 ?
Pb1 N4 2.756(15) 3_545 ?
Pb2 N5 2.645(17) 7_565 ?
Pb2 O2 2.698(13) 7_565 ?
Pb2 O3 2.70(2) 7_565 ?
Pb2 O6 2.733(15) 6_565 ?
Pb2 O6 2.734(15) 4 ?

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
C2 C1 C5 118.9(18) . . ?
C2 C1 H1 120.5 . . ?
C5 C1 H1 120.5 . . ?
N1 C2 C1 124.5(17) . . ?
N1 C2 H2 117.8 . . ?
C1 C2 H2 117.8 . . ?
N1 C3 C4 124.5(19) . . ?
N1 C3 H3 117.7 . . ?
C4 C3 H3 117.7 . . ?
C5 C4 C3 119.0(19) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C1 117.4(18) . . ?
C4 C5 C6 123.4(18) . . ?
C1 C5 C6 119.2(18) . . ?
N2 C6 C5 115.4(16) . . ?
N2 C6 C7 126.1(16) . . ?
C5 C6 C7 118.5(17) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C10 121(2) . . ?
N3 C9 C8 124(2) . . ?
C10 C9 C8 115(2) . . ?
C14 C10 C11 118.0(18) . . ?
C14 C10 C9 120.4(18) . . ?
C11 C10 C9 121.5(19) . . ?
C10 C11 C12 118.6(19) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
N4 C12 C11 122(2) . . ?
N4 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
N4 C13 C14 119.7(19) . . ?
N4 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C10 C14 C13 119.5(19) . . ?
C10 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C16 C15 C19 120(2) . . ?
C16 C15 H15 119.9 . . ?
C19 C15 H15 119.9 . . ?
N5 C16 C15 119(2) . . ?
N5 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
N5 C17 C18 125(2) . . ?
N5 C17 H17 117.4 . . ?
C18 C17 H17 117.4 . . ?
C19 C18 C17 118(2) . . ?
C19 C18 H18 121.2 . . ?
C17 C18 H18 121.2 . . ?
C18 C19 C15 117.9(17) . . ?
C18 C19 C20 123.0(18) . . ?
C15 C19 C20 119.1(17) . . ?
N6 C20 C21 127.9(19) . . ?
N6 C20 C19 115(2) . . ?
C21 C20 C19 117.4(18) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C23 C22 H22A 109.4 . . ?
H22B C22 H22A 109.5 . . ?
H22C C22 H22A 109.5 . . ?
N10 C23 C22 171(5) . . ?
C2 N1 C3 115.6(17) . . ?
C2 N1 Pb1 117.6(12) . . ?
C3 N1 Pb1 124.2(13) . . ?
C6 N2 N3 114.0(14) . . ?
C9 N3 N2 114.8(17) . . ?
C12 N4 C13 122.5(18) . . ?
C12 N4 Pb1 119.0(14) . 3_455 ?
C13 N4 Pb1 117.5(14) . 3_455 ?
C17 N5 C16 119.4(18) . . ?
C17 N5 Pb2 123.1(13) . . ?
C16 N5 Pb2 115.7(14) . . ?
C20 N6 N6 113(2) . 5_665 ?
O1 N7 O3 123.3(18) . . ?
O1 N7 O2 121.6(16) . . ?
O3 N7 O2 115.1(19) . . ?
O5 N8 O4 121.3(17) . . ?
O5 N8 O6 119.8(17) . . ?
O4 N8 O6 118.7(17) . . ?
O9 N9 O8 123.6(16) . . ?
O9 N9 O7 118.9(15) . . ?
O8 N9 O7 117.3(16) . . ?
N7 O1 Pb1 93.3(11) . . ?
N7 O2 Pb1 95.0(11) . . ?
N7 O2 Pb2 98.8(11) . . ?
Pb1 O2 Pb2 165.9(6) . . ?
N7 O3 Pb2 99.0(13) . . ?
N8 O4 Pb1 111.9(11) . . ?
N8 O6 Pb2 103.3(11) . 4_545 ?
N9 O7 Pb1 102.5(10) . 4_545 ?
N9 O8 Pb1 100.9(10) . . ?
O2 Pb1 N1 74.2(5) . . ?
O2 Pb1 O1 50.0(5) . . ?
N1 Pb1 O1 76.1(5) . . ?
O2 Pb1 O8 112.2(4) . . ?
N1 Pb1 O8 83.1(5) . . ?
O1 Pb1 O8 62.8(4) . . ?
O2 Pb1 O7 81.0(4) . 4 ?
N1 Pb1 O7 80.2(4) . 4 ?
O1 Pb1 O7 129.6(4) . 4 ?
O8 Pb1 O7 155.0(4) . 4 ?
O2 Pb1 O4 143.4(5) . . ?
N1 Pb1 O4 69.2(5) . . ?
O1 Pb1 O4 119.5(5) . . ?
O8 Pb1 O4 65.1(5) . . ?
O7 Pb1 O4 91.4(4) 4 . ?
O2 Pb1 N4 71.6(5) . 3_545 ?
N1 Pb1 N4 144.2(5) . 3_545 ?
O1 Pb1 N4 74.1(5) . 3_545 ?
O8 Pb1 N4 100.2(5) . 3_545 ?
O7 Pb1 N4 104.2(5) 4 3_545 ?
O4 Pb1 N4 144.4(5) . 3_545 ?
N5 Pb2 N5 179.999(1) . 7_565 ?
N5 Pb2 O2 90.8(5) . 7_565 ?
N5 Pb2 O2 89.2(5) 7_565 7_565 ?
N5 Pb2 O2 89.2(5) . . ?
N5 Pb2 O2 90.8(5) 7_565 . ?
O2 Pb2 O2 180.0(4) 7_565 . ?
N5 Pb2 O3 93.0(6) . 7_565 ?
N5 Pb2 O3 87.0(6) 7_565 7_565 ?
O2 Pb2 O3 47.1(4) 7_565 7_565 ?
O2 Pb2 O3 132.9(4) . 7_565 ?
N5 Pb2 O3 87.0(6) . . ?
N5 Pb2 O3 93.0(6) 7_565 . ?
O2 Pb2 O3 132.9(4) 7_565 . ?
O2 Pb2 O3 47.1(4) . . ?
O3 Pb2 O3 179.998(1) 7_565 . ?
N5 Pb2 O6 110.3(5) . 6_565 ?
N5 Pb2 O6 69.7(5) 7_565 6_565 ?
O2 Pb2 O6 70.3(4) 7_565 6_565 ?
O2 Pb2 O6 109.7(4) . 6_565 ?
O3 Pb2 O6 113.4(5) 7_565 6_565 ?
O3 Pb2 O6 66.6(5) . 6_565 ?
N5 Pb2 O6 69.7(5) . 4 ?
N5 Pb2 O6 110.3(5) 7_565 4 ?
O2 Pb2 O6 109.7(4) 7_565 4 ?
O2 Pb2 O6 70.3(4) . 4 ?
O3 Pb2 O6 66.6(5) 7_565 4 ?
O3 Pb2 O6 113.4(5) . 4 ?
O6 Pb2 O6 179.999(1) 6_565 4 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 N1 2(3) . . . . ?
N1 C3 C4 C5 0(3) . . . . ?
C3 C4 C5 C1 -2(3) . . . . ?
C3 C4 C5 C6 175.7(16) . . . . ?
C2 C1 C5 C4 1(3) . . . . ?
C2 C1 C5 C6 -176.6(18) . . . . ?
C4 C5 C6 N2 172.2(17) . . . . ?
C1 C5 C6 N2 -10(2) . . . . ?
C4 C5 C6 C7 -9(2) . . . . ?
C1 C5 C6 C7 168.5(17) . . . . ?
N3 C9 C10 C14 4(3) . . . . ?
C8 C9 C10 C14 -169(4) . . . . ?
N3 C9 C10 C11 -175(2) . . . . ?
C8 C9 C10 C11 12(5) . . . . ?
C14 C10 C11 C12 1(3) . . . . ?
C9 C10 C11 C12 -180(2) . . . . ?
C10 C11 C12 N4 -3(3) . . . . ?
C11 C10 C14 C13 3(3) . . . . ?
C9 C10 C14 C13 -176.4(18) . . . . ?
N4 C13 C14 C10 -4(3) . . . . ?
C19 C15 C16 N5 3(3) . . . . ?
N5 C17 C18 C19 -5(3) . . . . ?
C17 C18 C19 C15 4(2) . . . . ?
C17 C18 C19 C20 -175.9(17) . . . . ?
C16 C15 C19 C18 -3(3) . . . . ?
C16 C15 C19 C20 176.7(19) . . . . ?
C18 C19 C20 N6 174.9(17) . . . . ?
C15 C19 C20 N6 -5(3) . . . . ?
C18 C19 C20 C21 -4(3) . . . . ?
C15 C19 C20 C21 176.0(18) . . . . ?
C1 C2 N1 C3 -4(3) . . . . ?
C1 C2 N1 Pb1 158.8(18) . . . . ?
C4 C3 N1 C2 3(3) . . . . ?
C4 C3 N1 Pb1 -158.3(14) . . . . ?
C5 C6 N2 N3 177.7(14) . . . . ?
C7 C6 N2 N3 -1(3) . . . . ?
C10 C9 N3 N2 -179.2(19) . . . . ?
C8 C9 N3 N2 -7(5) . . . . ?
C6 N2 N3 C9 -167(2) . . . . ?
C11 C12 N4 C13 2(3) . . . . ?
C11 C12 N4 Pb1 -166.5(14) . . . 3_455 ?
C14 C13 N4 C12 2(3) . . . . ?
C14 C13 N4 Pb1 170.5(12) . . . 3_455 ?
C18 C17 N5 C16 4(3) . . . . ?
C18 C17 N5 Pb2 168.1(13) . . . . ?
C15 C16 N5 C17 -3(3) . . . . ?
C15 C16 N5 Pb2 -168.1(15) . . . . ?
C21 C20 N6 N6 0(3) . . . 5_665 ?
C19 C20 N6 N6 -178.9(18) . . . 5_665 ?
O3 N7 O1 Pb1 176.1(18) . . . . ?
O2 N7 O1 Pb1 -3.6(19) . . . . ?
O1 N7 O2 Pb1 3.7(19) . . . . ?
O3 N7 O2 Pb1 -176.1(16) . . . . ?
O1 N7 O2 Pb2 -179.2(16) . . . . ?
O3 N7 O2 Pb2 1.1(19) . . . . ?
O1 N7 O3 Pb2 179.2(16) . . . . ?
O2 N7 O3 Pb2 -1.1(19) . . . . ?
O5 N8 O4 Pb1 36(2) . . . . ?
O6 N8 O4 Pb1 -149.2(13) . . . . ?
O5 N8 O6 Pb2 8(2) . . . 4_545 ?
O4 N8 O6 Pb2 -166.9(13) . . . 4_545 ?
O9 N9 O7 Pb1 3.9(17) . . . 4_545 ?
O8 N9 O7 Pb1 -170.6(12) . . . 4_545 ?
O9 N9 O8 Pb1 176.3(14) . . . . ?
O7 N9 O8 Pb1 -9.5(16) . . . . ?
N7 O2 Pb1 N1 -86.9(11) . . . . ?
Pb2 O2 Pb1 N1 105(3) . . . . ?
N7 O2 Pb1 O1 -1.9(10) . . . . ?
Pb2 O2 Pb1 O1 -170(3) . . . . ?
N7 O2 Pb1 O8 -11.4(12) . . . . ?
Pb2 O2 Pb1 O8 -180(100) . . . . ?
N7 O2 Pb1 O7 -169.2(11) . . . 4 ?
Pb2 O2 Pb1 O7 22(3) . . . 4 ?
N7 O2 Pb1 O4 -89.1(13) . . . . ?
Pb2 O2 Pb1 O4 102(3) . . . . ?
N7 O2 Pb1 N4 82.5(11) . . . 3_545 ?
Pb2 O2 Pb1 N4 -86(3) . . . 3_545 ?
C2 N1 Pb1 O2 129.3(15) . . . . ?
C3 N1 Pb1 O2 -69.8(15) . . . . ?
C2 N1 Pb1 O1 77.5(15) . . . . ?
C3 N1 Pb1 O1 -121.6(16) . . . . ?
C2 N1 Pb1 O8 13.9(15) . . . . ?
C3 N1 Pb1 O8 174.8(15) . . . . ?
C2 N1 Pb1 O7 -147.3(15) . . . 4 ?
C3 N1 Pb1 O7 13.6(15) . . . 4 ?
C2 N1 Pb1 O4 -52.0(15) . . . . ?
C3 N1 Pb1 O4 108.8(15) . . . . ?
C2 N1 Pb1 N4 111.9(16) . . . 3_545 ?
C3 N1 Pb1 N4 -87.2(17) . . . 3_545 ?
N7 O1 Pb1 O2 2.0(10) . . . . ?
N7 O1 Pb1 N1 82.8(12) . . . . ?
N7 O1 Pb1 O8 172.1(13) . . . . ?
N7 O1 Pb1 O7 18.4(14) . . . 4 ?
N7 O1 Pb1 O4 138.8(11) . . . . ?
N7 O1 Pb1 N4 -77.1(12) . . . 3_545 ?
N9 O8 Pb1 O2 140.4(10) . . . . ?
N9 O8 Pb1 N1 -149.8(11) . . . . ?
N9 O8 Pb1 O1 132.3(12) . . . . ?
N9 O8 Pb1 O7 -101.3(13) . . . 4 ?
N9 O8 Pb1 O4 -79.5(11) . . . . ?
N9 O8 Pb1 N4 66.3(11) . . . 3_545 ?
N8 O4 Pb1 O2 -161.9(11) . . . . ?
N8 O4 Pb1 N1 -164.1(14) . . . . ?
N8 O4 Pb1 O1 136.5(12) . . . . ?
N8 O4 Pb1 O8 103.9(13) . . . . ?
N8 O4 Pb1 O7 -85.2(13) . . . 4 ?
N8 O4 Pb1 N4 32.0(17) . . . 3_545 ?
C17 N5 Pb2 N5 98(6) . . . 7_565 ?
C16 N5 Pb2 N5 -98(6) . . . 7_565 ?
C17 N5 Pb2 O2 -109.0(15) . . . 7_565 ?
C16 N5 Pb2 O2 55.8(14) . . . 7_565 ?
C17 N5 Pb2 O2 71.0(15) . . . . ?
C16 N5 Pb2 O2 -124.2(14) . . . . ?
C17 N5 Pb2 O3 -156.0(15) . . . 7_565 ?
C16 N5 Pb2 O3 8.7(14) . . . 7_565 ?
C17 N5 Pb2 O3 24.0(15) . . . . ?
C16 N5 Pb2 O3 -171.3(14) . . . . ?
C17 N5 Pb2 O6 -39.7(17) . . . 6_565 ?
C16 N5 Pb2 O6 125.0(13) . . . 6_565 ?
C17 N5 Pb2 O6 140.3(17) . . . 4 ?
C16 N5 Pb2 O6 -55.0(13) . . . 4 ?
N7 O2 Pb2 N5 -87.4(11) . . . . ?
Pb1 O2 Pb2 N5 81(3) . . . . ?
N7 O2 Pb2 N5 92.6(11) . . . 7_565 ?
Pb1 O2 Pb2 N5 -99(3) . . . 7_565 ?
N7 O2 Pb2 O2 71(2) . . . 7_565 ?
Pb1 O2 Pb2 O2 -121(4) . . . 7_565 ?
N7 O2 Pb2 O3 179.4(11) . . . 7_565 ?
Pb1 O2 Pb2 O3 -12(3) . . . 7_565 ?
N7 O2 Pb2 O3 -0.6(11) . . . . ?
Pb1 O2 Pb2 O3 168(3) . . . . ?
N7 O2 Pb2 O6 23.9(12) . . . 6_565 ?
Pb1 O2 Pb2 O6 -168(3) . . . 6_565 ?
N7 O2 Pb2 O6 -156.1(12) . . . 4 ?
Pb1 O2 Pb2 O6 12(3) . . . 4 ?
N7 O3 Pb2 N5 92.3(14) . . . . ?
N7 O3 Pb2 N5 -87.7(14) . . . 7_565 ?
N7 O3 Pb2 O2 -179.3(11) . . . 7_565 ?
N7 O3 Pb2 O2 0.7(11) . . . . ?
N7 O3 Pb2 O3 -55(4) . . . 7_565 ?
N7 O3 Pb2 O6 -154.1(15) . . . 6_565 ?
N7 O3 Pb2 O6 25.9(15) . . . 4 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        29.16
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.978
_refine_diff_density_min         -1.862
_refine_diff_density_rms         0.336