# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C63 H46 N6 O48 Pb10'
_chemical_formula_weight         3726.96

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           HEXAGONAL
_symmetry_space_group_name_H-M   P3(1)21

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'

_cell_length_a                   15.729(2)
_cell_length_b                   15.729(2)
_cell_length_c                   30.451(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6524.6(18)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    19643
_cell_measurement_theta_min      2.5024
_cell_measurement_theta_max      27.4779

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5010
_exptl_absorpt_coefficient_mu    19.377
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4668
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            55798
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         27.49
_reflns_number_total             9961
_reflns_number_gt                9735
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0786P)²+329.0575P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_number_reflns         9961
_refine_ls_number_parameters     569
_refine_ls_number_restraints     94
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0679
_refine_ls_wR_factor_ref         0.1789
_refine_ls_wR_factor_gt          0.1777
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.977
_refine_ls_shift/su_max          0.165
_refine_ls_shift/su_mean         0.005

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
Pb1 Pb -0.15123(6) -0.59684(6) 0.00650(2) 0.03596(18) Uani 1 1 d . . .
Pb2 Pb 0.46297(6) -0.38129(6) 0.00441(3) 0.03808(18) Uani 1 1 d . . .
Pb3 Pb 0.16945(7) -0.43747(7) 0.00608(3) 0.0414(2) Uani 1 1 d . . .
Pb4 Pb -0.14944(7) -0.36128(7) 0.07982(3) 0.0468(2) Uani 1 1 d . . .
Pb5 Pb 0.16864(7) -0.19967(7) 0.07932(3) 0.0476(2) Uani 1 1 d . . .
O12 O 0.5295(11) -0.4781(12) 0.0477(5) 0.038(3) Uani 1 1 d . . .
O6 O -0.2518(14) -0.8019(13) -0.0026(5) 0.050(4) Uani 1 1 d . . .
O8 O -0.4417(12) -1.1768(12) -0.0022(5) 0.043(4) Uani 1 1 d . . .
O14 O 0.0129(11) -0.4916(11) 0.0495(4) 0.038(3) Uani 1 1 d . . .
O13 O 0.0073(9) -0.3689(10) 0.0840(5) 0.033(3) Uani 1 1 d . . .
O4 O 0.1907(11) -0.3635(17) 0.2493(4) 0.057(5) Uani 1 1 d . . .
O3 O 0.3225(12) -0.3329(14) 0.2871(5) 0.048(4) Uani 1 1 d . . .
O11 O 0.6555(11) -0.4659(12) 0.0819(5) 0.041(3) Uani 1 1 d . . .
O20 O 0.007(3) -0.186(3) 0.0624(14) 0.139(6) Uani 1 1 d U . .
O2 O 0.3564(16) -0.3171(17) 0.0520(5) 0.061(5) Uani 1 1 d . . .
O9 O 0.6480(15) -0.4610(16) 0.2520(7) 0.070(6) Uani 1 1 d . . .
O7 O -0.4001(13) -1.2514(12) 0.0489(6) 0.052(4) Uani 1 1 d . . .
O5 O -0.1522(14) -0.7279(13) 0.0510(7) 0.059(5) Uani 1 1 d . . .
O23 O -0.191(2) -0.2446(19) 0.1272(8) 0.095(9) Uani 1 1 d . . .
C29 C 0.0000 -0.4514(19) 0.1667 0.033(6) Uani 1 2 d S . .
H29A H 0.0000 -0.3923 0.1667 0.049 Uiso 1 2 calc SR . .
C15 C -0.3009(16) -0.9930(17) 0.0310(6) 0.038(5) Uani 1 1 d . . .
H15A H -0.3441 -0.9948 0.0097 0.046 Uiso 1 1 calc R . .
C28 C 0.0024(14) -0.4982(14) 0.1286(5) 0.026(4) Uani 1 1 d . . .
C23 C 0.4997(15) -0.243(2) 0.1740(7) 0.044(5) Uani 1 1 d . . .
C12 C -0.2096(16) -0.8076(14) 0.0308(7) 0.037(5) Uani 1 1 d . . .
C4 C 0.5188(15) -0.4836(17) 0.1262(6) 0.036(4) Uani 1 1 d . . .
C2 C 0.5191(17) -0.4770(18) 0.2053(7) 0.039(5) Uani 1 1 d . . .
C5 C 0.4212(19) -0.5117(19) 0.1244(7) 0.045(5) Uani 1 1 d . . .
H5A H 0.3893 -0.5233 0.0976 0.053 Uiso 1 1 calc R . .
C33 C 0.0095(13) -0.4493(16) 0.0849(5) 0.032(4) Uani 1 1 d . . .
C6 C 0.3708(19) -0.523(2) 0.1632(6) 0.051(7) Uani 1 1 d . . .
O22 O -0.145(2) -0.331(2) 0.1677(9) 0.097(9) Uani 1 1 d . . .
C3 C 0.5668(15) -0.4729(17) 0.1663(6) 0.035(4) Uani 1 1 d . . .
H3A H 0.6302 -0.4630 0.1668 0.042 Uiso 1 1 calc R . .
C11 C -0.3857(15) -1.1713(17) 0.0304(8) 0.040(5) Uani 1 1 d . . .
C26 C 0.2948(16) -0.3245(15) 0.1686(6) 0.034(4) Uani 1 1 d . . .
H26A H 0.2274 -0.3491 0.1668 0.041 Uiso 1 1 calc R . .
C27 C 0.3519(15) -0.3031(17) 0.1299(5) 0.031(4) Uani 1 1 d . . .
C25 C 0.3403(14) -0.3083(15) 0.2089(6) 0.031(4) Uani 1 1 d . . .
C14 C -0.2251(16) -0.9030(15) 0.0474(8) 0.042(5) Uani 1 1 d . . .
C30 C 0.0037(15) -0.5870(15) 0.1289(6) 0.032(4) Uani 1 1 d . . .
H30A H 0.0072 -0.6154 0.1027 0.039 Uiso 1 1 calc R . .
C24 C 0.4446(15) -0.2651(19) 0.2116(7) 0.043(5) Uani 1 1 d . . .
H24A H 0.4752 -0.2522 0.2389 0.052 Uiso 1 1 calc R . .
C21 C 0.298(2) -0.3299(19) 0.0865(7) 0.052(7) Uani 1 1 d . . .
O10 O 0.528(3) -0.459(3) 0.2834(6) 0.130(14) Uani 1 1 d . . .
C20 C 0.2818(15) -0.3377(18) 0.2521(7) 0.041(5) Uani 1 1 d . . .
C16 C -0.3092(17) -1.0788(15) 0.0476(8) 0.039(5) Uani 1 1 d . . .
O1 O 0.2093(17) -0.3629(18) 0.0824(6) 0.098(10) Uani 1 1 d . . .
C9 C 0.569(2) -0.4710(16) 0.2473(7) 0.042(5) Uani 1 1 d . . .
C8 C 0.242(4) -0.564(3) 0.1592(11) 0.110(18) Uani 1 1 d . . .
H8A H 0.2233 -0.5729 0.1289 0.166 Uiso 1 1 calc R . .
H8B H 0.2292 -0.5164 0.1722 0.166 Uiso 1 1 calc R . .
H8C H 0.2059 -0.6255 0.1744 0.166 Uiso 1 1 calc R . .
C1 C 0.422(2) -0.5045(17) 0.2021(7) 0.045(6) Uani 1 1 d . . .
H1A H 0.3884 -0.5116 0.2281 0.054 Uiso 1 1 calc R . .
N1 N -0.170(2) -0.264(2) 0.1654(8) 0.067(7) Uani 1 1 d . . .
C32 C 0.0000 -0.7300(18) 0.1667 0.036(6) Uani 1 2 d SU . .
H32A H -0.0041 -0.7524 0.1963 0.053 Uiso 0.50 1 calc PR . .
H32B H 0.0595 -0.7206 0.1534 0.053 Uiso 0.50 1 calc PR . .
H32C H -0.0554 -0.7780 0.1502 0.053 Uiso 0.50 1 calc PR . .
C31 C 0.0000 -0.6297(18) 0.1667 0.040(7) Uani 1 2 d S . .
O21 O -0.192(2) -0.2442(19) 0.2023(9) 0.090(8) Uani 1 1 d . . .
C18 C -0.180(2) -0.995(2) 0.0991(11) 0.064(7) Uani 1 1 d U . .
C17 C -0.257(2) -1.074(2) 0.0825(12) 0.073(9) Uani 1 1 d . . .
H17A H -0.2772 -1.1322 0.0973 0.088 Uiso 1 1 calc R . .
C22 C 0.4532(19) -0.259(2) 0.1338(8) 0.058(8) Uani 1 1 d . . .
H22A H 0.4911 -0.2398 0.1084 0.069 Uiso 1 1 calc R . .
C13 C -0.164(2) -0.9033(18) 0.0806(10) 0.067(9) Uani 1 1 d . . .
H13A H -0.1125 -0.8441 0.0908 0.080 Uiso 1 1 calc R . .
C19 C 0.610(3) -0.198(5) 0.1766(11) 0.14(3) Uani 1 1 d . . .
H19A H 0.6366 -0.1860 0.1475 0.215 Uiso 1 1 calc R . .
H19B H 0.6252 -0.2418 0.1917 0.215 Uiso 1 1 calc R . .
H19C H 0.6372 -0.1366 0.1923 0.215 Uiso 1 1 calc R . .
C10 C -0.117(3) -0.988(3) 0.1382(11) 0.080(9) Uani 1 1 d U . .
H10A H -0.1299 -1.0520 0.1460 0.120 Uiso 1 1 calc R . .
H10B H -0.1328 -0.9592 0.1626 0.120 Uiso 1 1 calc R . .
H10C H -0.0490 -0.9471 0.1308 0.120 Uiso 1 1 calc R . .
O19 O -0.157(3) -0.235(3) 0.0400(13) 0.140(6) Uani 1 1 d DU . .
N2 N -0.079(3) -0.156(3) 0.0424(16) 0.140(6) Uani 1 1 d DU . .
O18 O -0.035(3) -0.076(3) 0.0232(12) 0.141(6) Uani 1 1 d DU . .
O17 O 0.127(5) -0.601(5) 0.021(2) 0.230(10) Uani 1 1 d U . .
O24 O 0.191(3) -0.062(3) 0.0385(12) 0.128(11) Uani 1 1 d U . .
O16 O 0.252(6) -0.560(6) -0.0123(18) 0.230(10) Uani 1 1 d DU . .
N3 N 0.243(6) -0.598(5) 0.024(2) 0.230(10) Uani 1 1 d DU . .
O15 O 0.293(5) -0.513(4) 0.012(3) 0.229(10) Uani 1 1 d DU . .
C7 C 0.5721(17) -0.4761(17) 0.0821(8) 0.041(5) Uiso 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O5 2.461(18) . ?
Pb1 O14 2.617(13) . ?
Pb1 O4 2.612(16) 6 ?
Pb1 O8 2.669(17) 4_655 ?
Pb1 O3 2.663(16) 6 ?
Pb2 O7 2.498(17) 1_665 ?
Pb2 O12 2.578(14) 4_645 ?
Pb2 O12 2.596(15) . ?
Pb2 O15 2.43(6) . ?
Pb3 O17 2.36(6) . ?
Pb3 O1 2.54(2) . ?
Pb3 O14 2.538(15) . ?
Pb3 O15 2.74(7) . ?
Pb3 O6 2.725(18) 4_655 ?
Pb4 O19 2.39(4) . ?
Pb4 O13 2.531(13) . ?
Pb4 O8 2.614(16) 4_655 ?
Pb4 O20 2.68(4) . ?
Pb4 O11 2.660(14) 1_455 ?
Pb4 O23 2.66(2) . ?
Pb4 O22 2.71(3) . ?
Pb4 O4 2.77(2) 6 ?
Pb4 N2 3.06(4) . ?
Pb5 O24 2.37(3) . ?
Pb5 O9 2.50(2) 6_665 ?
Pb5 O6 2.594(16) 4_655 ?
Pb5 O13 2.605(13) . ?
Pb5 O22 2.68(3) 6 ?
Pb5 O21 2.67(2) 6 ?
Pb5 O20 2.70(4) . ?
O12 C7 1.24(3) . ?
O12 Pb2 2.578(14) 4_645 ?
O6 C12 1.24(3) . ?
O6 Pb5 2.594(16) 4_545 ?
O6 Pb3 2.725(18) 4_545 ?
O8 C11 1.30(2) . ?
O8 Pb4 2.614(16) 4_545 ?
O8 Pb1 2.669(17) 4_545 ?
O14 C33 1.28(2) . ?
O13 C33 1.28(3) . ?
O4 C20 1.28(2) . ?
O4 Pb1 2.612(16) 6 ?
O4 Pb4 2.77(2) 6 ?
O3 C20 1.23(3) . ?
O3 Pb1 2.663(16) 6 ?
O11 C7 1.24(3) . ?
O11 Pb4 2.660(14) 1_655 ?
O20 N2 1.76(6) . ?
O2 C21 1.34(3) . ?
O9 C9 1.18(3) . ?
O9 Pb5 2.50(2) 6_655 ?
O7 C11 1.29(3) . ?
O7 Pb2 2.498(17) 1_445 ?
O5 C12 1.28(3) . ?
O23 N1 1.29(3) . ?
C29 C28 1.39(2) 6 ?
C29 C28 1.39(2) . ?
C29 H29A 0.9300 . ?
C15 C16 1.38(3) . ?
C15 C14 1.41(3) . ?
C15 H15A 0.9300 . ?
C28 C30 1.41(3) . ?
C28 C33 1.51(2) . ?
C23 C22 1.38(3) . ?
C23 C24 1.37(3) . ?
C23 C19 1.51(4) . ?
C12 C14 1.48(3) . ?
C4 C5 1.37(3) . ?
C4 C3 1.40(3) . ?
C4 C7 1.56(3) . ?
C2 C1 1.36(3) . ?
C2 C3 1.39(3) . ?
C2 C9 1.48(3) . ?
C5 C6 1.38(3) . ?
C5 H5A 0.9300 . ?
C6 C1 1.38(3) . ?
C6 C8 1.79(6) . ?
O22 N1 1.29(3) . ?
O22 Pb5 2.68(3) 6 ?
C3 H3A 0.9300 . ?
C11 C16 1.44(3) . ?
C26 C25 1.38(3) . ?
C26 C27 1.42(3) . ?
C26 H26A 0.9300 . ?
C27 C22 1.39(3) . ?
C27 C21 1.51(3) . ?
C25 C24 1.43(3) . ?
C25 C20 1.54(3) . ?
C14 C13 1.40(3) . ?
C30 C31 1.32(2) . ?
C30 H30A 0.9300 . ?
C24 H24A 0.9300 . ?
C21 O1 1.23(4) . ?
O10 C9 1.34(3) . ?
C16 C17 1.32(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C1 H1A 0.9300 . ?
N1 O21 1.27(3) . ?
C32 C31 1.58(4) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C31 C30 1.32(2) 6 ?
O21 Pb5 2.67(2) 6 ?
C18 C17 1.33(4) . ?
C18 C13 1.44(4) . ?
C18 C10 1.51(4) . ?
C17 H17A 0.9300 . ?
C22 H22A 0.9300 . ?
C13 H13A 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
O19 N2 1.232(5) . ?
N2 O18 1.235(5) . ?
O17 N3 1.81(9) . ?
O16 N3 1.230(6) . ?
N3 O15 1.230(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Pb1 O14 81.1(5) . . ?
O5 Pb1 O4 79.3(7) . 6 ?
O14 Pb1 O4 70.8(5) . 6 ?
O5 Pb1 O8 148.6(6) . 4_655 ?
O14 Pb1 O8 89.9(5) . 4_655 ?
O4 Pb1 O8 69.3(6) 6 4_655 ?
O5 Pb1 O3 83.0(6) . 6 ?
O14 Pb1 O3 119.9(5) . 6 ?
O4 Pb1 O3 49.4(5) 6 6 ?
O8 Pb1 O3 75.5(5) 4_655 6 ?
O7 Pb2 O12 112.4(6) 1_665 4_645 ?
O7 Pb2 O12 76.7(5) 1_665 . ?
O12 Pb2 O12 68.5(5) 4_645 . ?
O7 Pb2 O15 140.8(18) 1_665 . ?
O12 Pb2 O15 97.7(16) 4_645 . ?
O12 Pb2 O15 92.8(17) . . ?
O17 Pb3 O1 101.5(16) . . ?
O17 Pb3 O14 80.6(16) . . ?
O1 Pb3 O14 69.6(6) . . ?
O17 Pb3 O15 52.6(19) . . ?
O1 Pb3 O15 94.4(17) . . ?
O14 Pb3 O15 127.0(15) . . ?
O17 Pb3 O6 169.2(15) . 4_655 ?
O1 Pb3 O6 70.7(7) . 4_655 ?
O14 Pb3 O6 89.6(5) . 4_655 ?
O15 Pb3 O6 133.7(12) . 4_655 ?
O19 Pb4 O13 121.5(10) . . ?
O19 Pb4 O8 83.0(10) . 4_655 ?
O13 Pb4 O8 87.2(5) . 4_655 ?
O19 Pb4 O20 56.3(11) . . ?
O13 Pb4 O20 69.0(9) . . ?
O8 Pb4 O20 99.4(10) 4_655 . ?
O19 Pb4 O11 90.2(9) . 1_455 ?
O13 Pb4 O11 145.0(5) . 1_455 ?
O8 Pb4 O11 82.1(5) 4_655 1_455 ?
O20 Pb4 O11 145.6(9) . 1_455 ?
O19 Pb4 O23 64.3(11) . . ?
O13 Pb4 O23 126.1(7) . . ?
O8 Pb4 O23 141.7(7) 4_655 . ?
O20 Pb4 O23 79.4(11) . . ?
O11 Pb4 O23 78.8(8) 1_455 . ?
O19 Pb4 O22 111.3(11) . . ?
O13 Pb4 O22 90.9(6) . . ?
O8 Pb4 O22 164.0(7) 4_655 . ?
O20 Pb4 O22 94.7(11) . . ?
O11 Pb4 O22 90.4(7) 1_455 . ?
O23 Pb4 O22 48.7(7) . . ?
O19 Pb4 O4 148.8(9) . 6 ?
O13 Pb4 O4 69.3(5) . 6 ?
O8 Pb4 O4 67.7(5) 4_655 6 ?
O20 Pb4 O4 136.7(9) . 6 ?
O11 Pb4 O4 75.9(5) 1_455 6 ?
O23 Pb4 O4 136.6(7) . 6 ?
O22 Pb4 O4 96.8(6) . 6 ?
O19 Pb4 N2 22.0(8) . . ?
O13 Pb4 N2 102.9(9) . . ?
O8 Pb4 N2 93.3(10) 4_655 . ?
O20 Pb4 N2 34.9(11) . . ?
O11 Pb4 N2 110.9(9) 1_455 . ?
O23 Pb4 N2 63.7(12) . . ?
O22 Pb4 N2 102.5(11) . . ?
O4 Pb4 N2 159.3(10) 6 . ?
O24 Pb5 O9 83.5(11) . 6_665 ?
O24 Pb5 O6 81.3(10) . 4_655 ?
O9 Pb5 O6 82.2(6) 6_665 4_655 ?
O24 Pb5 O13 126.0(10) . . ?
O9 Pb5 O13 147.0(7) 6_665 . ?
O6 Pb5 O13 87.9(5) 4_655 . ?
O24 Pb5 O22 113.9(11) . 6 ?
O9 Pb5 O22 95.7(8) 6_665 6 ?
O6 Pb5 O22 164.5(7) 4_655 6 ?
O13 Pb5 O22 85.6(6) . 6 ?
O24 Pb5 O21 67.7(11) . 6 ?
O9 Pb5 O21 82.6(8) 6_665 6 ?
O6 Pb5 O21 146.8(8) 4_655 6 ?
O13 Pb5 O21 119.7(8) . 6 ?
O22 Pb5 O21 46.9(8) 6 6 ?
O24 Pb5 O20 62.9(12) . . ?
O9 Pb5 O20 145.2(10) 6_665 . ?
O6 Pb5 O20 100.2(10) 4_655 . ?
O13 Pb5 O20 67.6(9) . . ?
O22 Pb5 O20 90.3(11) 6 . ?
O21 Pb5 O20 76.7(10) 6 . ?
C7 O12 Pb2 98.3(13) . 4_645 ?
C7 O12 Pb2 142.0(15) . . ?
Pb2 O12 Pb2 110.5(5) 4_645 . ?
C12 O6 Pb5 119.8(15) . 4_545 ?
C12 O6 Pb3 126.0(16) . 4_545 ?
Pb5 O6 Pb3 110.1(5) 4_545 4_545 ?
C11 O8 Pb4 115.1(14) . 4_545 ?
C11 O8 Pb1 131.9(14) . 4_545 ?
Pb4 O8 Pb1 109.5(5) 4_545 4_545 ?
C33 O14 Pb3 123.3(11) . . ?
C33 O14 Pb1 117.8(12) . . ?
Pb3 O14 Pb1 115.8(5) . . ?
C33 O13 Pb4 123.7(11) . . ?
C33 O13 Pb5 121.0(11) . . ?
Pb4 O13 Pb5 115.0(5) . . ?
C20 O4 Pb1 92.9(13) . 6 ?
C20 O4 Pb4 115.5(17) . 6 ?
Pb1 O4 Pb4 106.5(6) 6 6 ?
C20 O3 Pb1 91.8(13) . 6 ?
C7 O11 Pb4 154.1(16) . 1_655 ?
N2 O20 Pb4 84.6(18) . . ?
N2 O20 Pb5 166(3) . . ?
Pb4 O20 Pb5 107.3(14) . . ?
C9 O9 Pb5 155.7(19) . 6_655 ?
C11 O7 Pb2 102.8(13) . 1_445 ?
C12 O5 Pb1 105.2(14) . . ?
N1 O23 Pb4 97.7(17) . . ?
C28 C29 C28 114(3) 6 . ?
C28 C29 H29A 123.1 6 . ?
C28 C29 H29A 123.1 . . ?
C16 C15 C14 118.1(19) . . ?
C16 C15 H15A 121.0 . . ?
C14 C15 H15A 121.0 . . ?
C29 C28 C30 122.6(18) . . ?
C29 C28 C33 118.7(18) . . ?
C30 C28 C33 118.6(17) . . ?
C22 C23 C24 119(2) . . ?
C22 C23 C19 121(2) . . ?
C24 C23 C19 120(2) . . ?
O6 C12 O5 118(2) . . ?
O6 C12 C14 121.9(18) . . ?
O5 C12 C14 120(2) . . ?
C5 C4 C3 121.5(18) . . ?
C5 C4 C7 117.6(18) . . ?
C3 C4 C7 120.5(18) . . ?
C1 C2 C3 116.4(19) . . ?
C1 C2 C9 124(2) . . ?
C3 C2 C9 119(2) . . ?
C6 C5 C4 119(2) . . ?
C6 C5 H5A 120.5 . . ?
C4 C5 H5A 120.5 . . ?
O14 C33 O13 121.5(18) . . ?
O14 C33 C28 119(2) . . ?
O13 C33 C28 119.3(16) . . ?
C5 C6 C1 118(2) . . ?
C5 C6 C8 117(2) . . ?
C1 C6 C8 125(2) . . ?
N1 O22 Pb5 99.6(18) . 6 ?
N1 O22 Pb4 95.5(18) . . ?
Pb5 O22 Pb4 160.1(12) 6 . ?
C2 C3 C4 119.6(18) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
O8 C11 O7 119(2) . . ?
O8 C11 C16 123(2) . . ?
O7 C11 C16 118.6(19) . . ?
C25 C26 C27 119.1(19) . . ?
C25 C26 H26A 120.4 . . ?
C27 C26 H26A 120.4 . . ?
C22 C27 C26 118.8(18) . . ?
C22 C27 C21 124(2) . . ?
C26 C27 C21 117.4(19) . . ?
C26 C25 C24 120.4(18) . . ?
C26 C25 C20 121.8(18) . . ?
C24 C25 C20 117.8(17) . . ?
C13 C14 C15 119(2) . . ?
C13 C14 C12 119.0(19) . . ?
C15 C14 C12 121.7(19) . . ?
C31 C30 C28 119.6(19) . . ?
C31 C30 H30A 120.2 . . ?
C28 C30 H30A 120.2 . . ?
C25 C24 C23 120.1(19) . . ?
C25 C24 H24A 120.0 . . ?
C23 C24 H24A 120.0 . . ?
O1 C21 O2 122(2) . . ?
O1 C21 C27 125(2) . . ?
O2 C21 C27 114(3) . . ?
O3 C20 O4 123(2) . . ?
O3 C20 C25 120.6(18) . . ?
O4 C20 C25 116.5(19) . . ?
C17 C16 C15 119(2) . . ?
C17 C16 C11 122(2) . . ?
C15 C16 C11 118(2) . . ?
C21 O1 Pb3 104.8(19) . . ?
O9 C9 O10 116(3) . . ?
O9 C9 C2 127(2) . . ?
O10 C9 C2 116(2) . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C1 C6 125(2) . . ?
C2 C1 H1A 117.4 . . ?
C6 C1 H1A 117.4 . . ?
O21 N1 O22 113(2) . . ?
O21 N1 O23 127(3) . . ?
O22 N1 O23 118(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C31 C30 122(3) 6 . ?
C30 C31 C32 119.2(14) 6 . ?
C30 C31 C32 119.2(14) . . ?
N1 O21 Pb5 100.6(17) . 6 ?
C17 C18 C13 113(3) . . ?
C17 C18 C10 129(3) . . ?
C13 C18 C10 117(3) . . ?
C16 C17 C18 128(3) . . ?
C16 C17 H17A 116.0 . . ?
C18 C17 H17A 116.0 . . ?
C23 C22 C27 122(2) . . ?
C23 C22 H22A 118.8 . . ?
C27 C22 H22A 118.8 . . ?
C14 C13 C18 121(2) . . ?
C14 C13 H13A 119.6 . . ?
C18 C13 H13A 119.6 . . ?
C23 C19 H19A 109.5 . . ?
C23 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C23 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C10 H10A 109.5 . . ?
C18 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C18 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 O19 Pb4 112(3) . . ?
O19 N2 O20 105(4) . . ?
O19 N2 O18 140(5) . . ?
O20 N2 O18 108(4) . . ?
O19 N2 Pb4 46(3) . . ?
O20 N2 Pb4 60.5(17) . . ?
O18 N2 Pb4 165(4) . . ?
N3 O17 Pb3 104(3) . . ?
O15 N3 O16 49(4) . . ?
O15 N3 O17 96(6) . . ?
O16 N3 O17 80(6) . . ?
N3 O15 Pb2 142(7) . . ?
N3 O15 Pb3 107(6) . . ?
Pb2 O15 Pb3 110(2) . . ?
O12 C7 O11 122(2) . . ?
O12 C7 C4 117.8(19) . . ?
O11 C7 C4 120(2) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.588
_refine_diff_density_min         -2.516
_refine_diff_density_rms         0.341
_database_code_depnum_ccdc_archive 'CCDC 988800'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C63 H46 N6 O48 Pb10'
_chemical_formula_weight         3726.96

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           HEXAGONAL
_symmetry_space_group_name_H-M   P3(2)21

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'

_cell_length_a                   15.6516(6)
_cell_length_b                   15.6516(6)
_cell_length_c                   30.325(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6433.5(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14636
_cell_measurement_theta_min      2.9292
_cell_measurement_theta_max      27.5750

_exptl_crystal_description       Prism
_exptl_crystal_colour            White
_exptl_crystal_size_max          0.7000
_exptl_crystal_size_mid          0.3000
_exptl_crystal_size_min          0.2500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5010
_exptl_absorpt_coefficient_mu    19.652
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5026
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Mercury70 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44742
_diffrn_reflns_av_R_equivalents  0.1067
_diffrn_reflns_av_sigmaI/netI    0.0853
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         27.50
_reflns_number_total             9845
_reflns_number_gt                9282
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0575P)²+512.6956P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(3)
_refine_ls_number_reflns         9845
_refine_ls_number_parameters     534
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0787
_refine_ls_wR_factor_ref         0.1880
_refine_ls_wR_factor_gt          0.1855
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.003

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
Pb1 Pb 1.15144(2) 0.59732(2) 0.493493(11) 0.02563(9) Uani 1 1 d . . .
Pb2 Pb 1.53740(2) 1.38157(2) 0.495643(12) 0.02808(9) Uani 1 1 d . . .
Pb3 Pb 0.83068(2) 0.43774(3) 0.493952(12) 0.03077(9) Uani 1 1 d . . .
Pb4 Pb 1.36198(3) 1.14999(3) 0.579728(15) 0.03591(11) Uani 1 1 d . . .
Pb5 Pb 1.19977(3) 0.83142(3) 0.579269(15) 0.03682(11) Uani 1 1 d . . .
O4 O 1.0084(4) 0.5281(5) 0.7857(2) 0.0288(19) Uani 1 1 d . . .
O9 O 1.4425(5) 1.1767(4) 0.5023(2) 0.0298(19) Uani 1 1 d . . .
O13 O 0.9862(4) 0.4893(4) 0.4504(2) 0.0257(18) Uani 1 1 d . . .
O8 O 1.1916(4) 0.5501(5) 0.4160(2) 0.0301(4) Uani 1 1 d U . .
O12 O 1.2509(5) 0.8023(4) 0.5030(2) 0.0403(19) Uani 1 1 d . . .
O3 O 1.1204(5) 0.6539(4) 0.7519(2) 0.0312(19) Uani 1 1 d . . .
O7 O 1.3220(5) 0.6571(5) 0.4540(2) 0.036(2) Uani 1 1 d . . .
O15 O 0.9939(4) 0.3695(4) 0.4158(3) 0.0289(19) Uani 1 1 d . . .
O2 O 1.1128(6) 0.6524(5) 0.5834(3) 0.055(3) Uani 1 1 d . . .
O5 O 1.3549(6) 0.6708(5) 0.2184(3) 0.042(3) Uani 1 1 d . . .
O10 O 1.4012(5) 1.2518(4) 0.4502(3) 0.042(2) Uani 1 1 d . . .
O21 O 1.1880(7) 0.9973(7) 0.5621(5) 0.093(2) Uani 1 1 d U . .
O11 O 1.1504(5) 0.7296(5) 0.4484(3) 0.045(2) Uani 1 1 d . . .
O20 O 1.3326(6) 1.1458(6) 0.6664(3) 0.070(3) Uani 1 1 d . . .
C3 C 1.0043(6) 0.5202(6) 0.7069(3) 0.026(2) Uani 1 1 d . . .
C28 C 1.0000 0.4548(9) 0.3333 0.023(3) Uani 1 2 d S . .
H26A H 1.0000 0.3954 0.3333 0.027 Uiso 1 2 calc SR . .
C26 C 1.3027(5) 0.9944(7) 0.4699(3) 0.030(2) Uani 1 1 d . . .
H25A H 1.3438 0.9966 0.4925 0.036 Uiso 1 1 calc R . .
C10 C 0.9966(6) 0.5184(6) 0.6274(4) 0.032(3) Uani 1 1 d . . .
C6 C 0.8938(7) 0.3723(8) 0.6708(3) 0.034(3) Uani 1 1 d . . .
C30 C 0.9969(5) 0.4988(5) 0.3726(3) 0.017(2) Uani 1 1 d . . .
C2 C 1.0407(6) 0.5698(6) 0.6671(3) 0.026(3) Uani 1 1 d . . .
H21A H 1.0925 0.6346 0.6666 0.031 Uiso 1 1 calc R . .
C11 C 1.3402(5) 0.6488(6) 0.3762(3) 0.021(2) Uani 1 1 d . . .
C19 C 1.2094(6) 0.8062(5) 0.4689(3) 0.024(2) Uani 1 1 d . . .
C27 C 1.3859(5) 1.1722(6) 0.4703(3) 0.0244(19) Uani 1 1 d U . .
C9 C 1.2819(6) 0.6190(7) 0.4192(3) 0.030(2) Uani 1 1 d U . .
O18 O 1.2427(6) 1.1921(7) 0.7045(3) 0.065(3) Uani 1 1 d . . .
C5 C 0.9320(7) 0.4210(6) 0.7076(3) 0.031(3) Uani 1 1 d . . .
H16A H 0.9104 0.3886 0.7345 0.037 Uiso 1 1 calc R . .
C1 C 1.0406(6) 0.5717(8) 0.5867(3) 0.034(3) Uani 1 1 d . . .
C29 C 0.9899(5) 0.4490(6) 0.4160(3) 0.0188(18) Uani 1 1 d U . .
C12 C 1.2954(7) 0.6209(7) 0.3347(3) 0.0323(4) Uani 1 1 d U . .
H13A H 1.2276 0.5784 0.3328 0.039 Uiso 1 1 calc R . .
C14 C 1.2947(7) 0.6275(7) 0.2533(3) 0.032(2) Uani 1 1 d U . .
C25 C 1.3119(6) 1.0806(5) 0.4505(4) 0.029(3) Uani 1 1 d . . .
C8 C 0.9284(5) 0.4210(7) 0.6309(3) 0.031(3) Uani 1 1 d . . .
H10A H 0.9036 0.3848 0.6051 0.038 Uiso 1 1 calc R . .
C16 C 1.4997(7) 0.7438(8) 0.3393(4) 0.039(3) Uani 1 1 d . . .
C31 C 0.9958(5) 0.5850(6) 0.3717(3) 0.022(2) Uani 1 1 d . . .
H54A H 0.9921 0.6130 0.3982 0.026 Uiso 1 1 calc R . .
C13 C 1.3500(7) 0.6552(6) 0.2963(3) 0.028(3) Uani 1 1 d . . .
C20 C 1.2244(6) 0.9017(6) 0.4520(3) 0.030(3) Uani 1 1 d . . .
C33 C 1.0000 0.7279(7) 0.3333 0.025(3) Uani 1 2 d S . .
H51A H 1.0027 0.7497 0.3035 0.038 Uiso 0.50 1 calc PR . .
H51B H 1.0565 0.7766 0.3493 0.038 Uiso 0.50 1 calc PR . .
H51C H 0.9409 0.7188 0.3472 0.038 Uiso 0.50 1 calc PR . .
C7 C 0.8169(8) 0.2522(8) 0.6722(6) 0.063(5) Uani 1 1 d . . .
H50A H 0.8021 0.2308 0.7023 0.094 Uiso 1 1 calc R . .
H50B H 0.8468 0.2187 0.6581 0.094 Uiso 1 1 calc R . .
H50C H 0.7571 0.2371 0.6571 0.094 Uiso 1 1 calc R . .
O6 O 1.2081(5) 0.5656(8) 0.2497(3) 0.075(3) Uani 1 1 d . . .
O1 O 0.9879(10) 0.5239(10) 0.5493(5) 0.1039(4) Uani 1 1 d U . .
N1 N 1.2626(7) 1.1692(8) 0.6658(3) 0.060(3) Uani 1 1 d . . .
C32 C 1.0000 0.6318(8) 0.3333 0.0241(3) Uani 1 2 d SU . .
O14 O 0.7202(5) 0.5219(2) 0.49845(18) 0.197(3) Uani 1 1 d DU . .
O19 O 1.2429(7) 1.1873(11) 0.6263(5) 0.134(5) Uani 1 1 d . . .
C4 C 1.0476(6) 0.5700(6) 0.7522(3) 0.035(3) Uani 1 1 d . . .
C22 C 1.1786(8) 0.9927(8) 0.4031(4) 0.047(3) Uani 1 1 d U . .
C15 C 1.4518(8) 0.7124(9) 0.3006(4) 0.047(4) Uani 1 1 d . . .
H43A H 1.4895 0.7302 0.2750 0.057 Uiso 1 1 calc R . .
C21 C 1.1641(8) 0.9019(8) 0.4206(4) 0.043(3) Uani 1 1 d U . .
H42A H 1.1127 0.8425 0.4101 0.052 Uiso 1 1 calc R . .
C24 C 1.2582(10) 1.0736(10) 0.4194(5) 0.0606(4) Uani 1 1 d U . .
H41A H 1.2749 1.1324 0.4051 0.073 Uiso 1 1 calc R . .
O24 O 1.089(2) 0.865(2) 0.5405(12) 0.3021(4) Uani 1 1 d U . .
C18 C 1.4445(6) 0.7126(9) 0.3787(4) 0.041(4) Uani 1 1 d . . .
H40A H 1.4756 0.7333 0.4059 0.050 Uiso 1 1 calc R . .
C23 C 1.1181(14) 0.9951(14) 0.3621(6) 0.094(6) Uiso 1 1 d . . .
H1A H 1.1389 1.0624 0.3546 0.141 Uiso 1 1 calc R . .
H1B H 1.0491 0.9609 0.3691 0.141 Uiso 1 1 calc R . .
H1C H 1.1296 0.9636 0.3374 0.141 Uiso 1 1 calc R . .
C17 C 1.6102(12) 0.8073(13) 0.3435(7) 0.088(6) Uiso 1 1 d . . .
H2A H 1.6394 0.8229 0.3147 0.132 Uiso 1 1 calc R . .
H2B H 1.6356 0.7723 0.3598 0.132 Uiso 1 1 calc R . .
H2C H 1.6258 0.8672 0.3587 0.132 Uiso 1 1 calc R . .
O16 O 0.85367(14) 0.5944(3) 0.4757(6) 0.225(4) Uiso 1 1 d DU . .
O17 O 0.73531(17) 0.64440(18) 0.4692(3) 0.252(7) Uiso 1 1 d DU . .
N3 N 0.77796(13) 0.59933(15) 0.47978(17) 0.217(2) Uiso 1 1 d DU . .
O23 O 1.2342(3) 1.1601(2) 0.5394(6) 0.137(3) Uiso 1 1 d DU . .
O22 O 1.07962(17) 1.0405(11) 0.52219(18) 0.144(4) Uiso 1 1 d DU . .
N2 N 1.16168(18) 1.0763(3) 0.5396(2) 0.1276(19) Uiso 1 1 d DU . .


_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 O11 2.487(8) . ?
Pb1 O13 2.623(5) . ?
Pb1 O8 2.632(7) . ?
Pb1 O7 2.634(7) . ?
Pb1 O9 2.645(8) 4_546 ?
Pb2 O10 2.498(7) . ?
Pb2 O4 2.559(6) 5_676 ?
Pb2 O14 2.595(6) 1_665 ?
Pb2 O4 2.598(6) 2_764 ?
Pb3 O16 2.359(6) . ?
Pb3 O13 2.520(6) . ?
Pb3 O6 2.576(10) 6_765 ?
Pb3 O14 2.649(9) . ?
Pb3 O1 2.714(14) . ?
Pb3 O12 2.731(7) 4_546 ?
Pb4 O23 2.415(11) . ?
Pb4 O15 2.508(7) 4_656 ?
Pb4 O9 2.597(7) . ?
Pb4 O19 2.626(15) . ?
Pb4 O21 2.627(9) . ?
Pb4 O20 2.662(10) . ?
Pb4 O3 2.660(6) 5_676 ?
Pb4 O8 2.683(7) 4_656 ?
Pb5 O24 2.36(4) . ?
Pb5 O2 2.430(7) . ?
Pb5 O12 2.562(8) . ?
Pb5 O15 2.605(5) 4_656 ?
Pb5 O18 2.644(11) 5_676 ?
Pb5 O20 2.704(10) 5_676 ?
Pb5 O21 2.743(12) . ?
O4 C4 1.196(11) . ?
O4 Pb2 2.559(6) 5_676 ?
O4 Pb2 2.598(6) 3_675 ?
O9 C27 1.293(11) . ?
O9 Pb1 2.645(8) 4_656 ?
O13 C29 1.237(11) . ?
O8 C9 1.283(9) . ?
O8 Pb4 2.683(7) 4_546 ?
O12 C19 1.237(12) . ?
O12 Pb3 2.731(7) 4_656 ?
O3 C4 1.235(9) . ?
O3 Pb4 2.660(6) 5_676 ?
O7 C9 1.219(11) . ?
O15 C29 1.277(12) . ?
O15 Pb4 2.508(7) 4_546 ?
O15 Pb5 2.605(5) 4_546 ?
O2 C1 1.206(11) . ?
O5 C14 1.353(12) . ?
O10 C27 1.297(12) . ?
O21 N2 1.635(13) . ?
O11 C19 1.253(10) . ?
O20 N1 1.317(17) . ?
O20 Pb5 2.704(10) 5_676 ?
C3 C2 1.393(13) . ?
C3 C5 1.391(11) . ?
C3 C4 1.559(12) . ?
C28 C30 1.389(11) 6_765 ?
C28 C30 1.389(11) . ?
C28 H26A 0.9300 . ?
C26 C25 1.410(14) . ?
C26 C20 1.457(11) . ?
C26 H25A 0.9300 . ?
C10 C8 1.360(12) . ?
C10 C2 1.421(13) . ?
C10 C1 1.456(14) . ?
C6 C5 1.314(13) . ?
C6 C8 1.388(13) . ?
C6 C7 1.651(14) . ?
C30 C31 1.359(13) . ?
C30 C29 1.504(12) . ?
C2 H21A 0.9300 . ?
C11 C12 1.401(13) . ?
C11 C18 1.428(10) . ?
C11 C9 1.526(13) . ?
C19 C20 1.484(13) . ?
C27 C25 1.449(11) . ?
O18 N1 1.308(15) . ?
O18 Pb5 2.644(11) 5_676 ?
C5 H16A 0.9300 . ?
C1 O1 1.382(16) . ?
C12 C13 1.384(13) . ?
C12 H13A 0.9300 . ?
C14 O6 1.215(11) . ?
C14 C13 1.501(13) . ?
C25 C24 1.232(19) . ?
C8 H10A 0.9300 . ?
C16 C15 1.346(15) . ?
C16 C18 1.412(15) . ?
C16 C17 1.508(18) . ?
C31 C32 1.358(11) . ?
C31 H54A 0.9300 . ?
C13 C15 1.390(14) . ?
C20 C21 1.343(17) . ?
C33 C32 1.505(17) . ?
C33 H51A 0.9600 . ?
C33 H51B 0.9600 . ?
C33 H51C 0.9600 . ?
C7 H50A 0.9600 . ?
C7 H50B 0.9600 . ?
C7 H50C 0.9600 . ?
O6 Pb3 2.576(10) 6_765 ?
N1 O19 1.305(18) . ?
C32 C31 1.358(11) 6_765 ?
O14 N3 1.229(4) . ?
O14 Pb2 2.595(6) 1_445 ?
C22 C24 1.350(16) . ?
C22 C21 1.424(18) . ?
C22 C23 1.58(2) . ?
C15 H43A 0.9300 . ?
C21 H42A 0.9300 . ?
C24 H41A 0.9300 . ?
C18 H40A 0.9300 . ?
C23 H1A 0.9600 . ?
C23 H1B 0.9600 . ?
C23 H1C 0.9600 . ?
C17 H2A 0.9600 . ?
C17 H2B 0.9600 . ?
C17 H2C 0.9600 . ?
O16 N3 1.232(3) . ?
O17 N3 1.232(4) . ?
O23 N2 1.232(3) . ?
O22 N2 1.234(4) . ?
O22 O22 1.714(19) 4_556 ?

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
O11 Pb1 O13 81.3(2) . . ?
O11 Pb1 O8 81.1(3) . . ?
O13 Pb1 O8 70.8(2) . . ?
O11 Pb1 O7 83.2(3) . . ?
O13 Pb1 O7 120.0(2) . . ?
O8 Pb1 O7 49.60(19) . . ?
O11 Pb1 O9 148.7(3) . 4_546 ?
O13 Pb1 O9 89.1(2) . 4_546 ?
O8 Pb1 O9 67.7(2) . 4_546 ?
O7 Pb1 O9 76.0(2) . 4_546 ?
O10 Pb2 O4 113.4(3) . 5_676 ?
O10 Pb2 O14 146.9(2) . 1_665 ?
O4 Pb2 O14 93.1(2) 5_676 1_665 ?
O10 Pb2 O4 77.0(3) . 2_764 ?
O4 Pb2 O4 68.4(2) 5_676 2_764 ?
O14 Pb2 O4 96.3(2) 1_665 2_764 ?
O16 Pb3 O13 85.6(3) . . ?
O16 Pb3 O6 99.8(5) . 6_765 ?
O13 Pb3 O6 68.7(2) . 6_765 ?
O16 Pb3 O14 45.07(16) . . ?
O13 Pb3 O14 129.31(19) . . ?
O6 Pb3 O14 103.7(3) 6_765 . ?
O16 Pb3 O1 90.0(4) . . ?
O13 Pb3 O1 71.0(3) . . ?
O6 Pb3 O1 137.4(4) 6_765 . ?
O14 Pb3 O1 112.1(4) . . ?
O16 Pb3 O12 168.4(5) . 4_546 ?
O13 Pb3 O12 88.5(2) . 4_546 ?
O6 Pb3 O12 68.7(3) 6_765 4_546 ?
O14 Pb3 O12 137.18(16) . 4_546 ?
O1 Pb3 O12 97.6(4) . 4_546 ?
O23 Pb4 O15 122.3(2) . 4_656 ?
O23 Pb4 O9 83.3(4) . . ?
O15 Pb4 O9 87.1(2) 4_656 . ?
O23 Pb4 O19 63.5(5) . . ?
O15 Pb4 O19 124.9(4) 4_656 . ?
O9 Pb4 O19 142.3(4) . . ?
O23 Pb4 O21 56.0(3) . . ?
O15 Pb4 O21 69.9(3) 4_656 . ?
O9 Pb4 O21 99.3(3) . . ?
O19 Pb4 O21 77.5(4) . . ?
O23 Pb4 O20 111.3(4) . . ?
O15 Pb4 O20 90.8(3) 4_656 . ?
O9 Pb4 O20 163.7(2) . . ?
O19 Pb4 O20 48.9(4) . . ?
O21 Pb4 O20 95.2(3) . . ?
O23 Pb4 O3 89.20(17) . 5_676 ?
O15 Pb4 O3 145.3(2) 4_656 5_676 ?
O9 Pb4 O3 82.1(2) . 5_676 ?
O19 Pb4 O3 80.1(3) . 5_676 ?
O21 Pb4 O3 144.4(3) . 5_676 ?
O20 Pb4 O3 90.5(2) . 5_676 ?
O23 Pb4 O8 148.6(4) . 4_656 ?
O15 Pb4 O8 69.72(19) 4_656 4_656 ?
O9 Pb4 O8 67.6(2) . 4_656 ?
O19 Pb4 O8 137.3(3) . 4_656 ?
O21 Pb4 O8 138.0(3) . 4_656 ?
O20 Pb4 O8 96.5(3) . 4_656 ?
O3 Pb4 O8 75.6(2) 5_676 4_656 ?
O24 Pb5 O2 103.4(8) . . ?
O24 Pb5 O12 85.3(9) . . ?
O2 Pb5 O12 83.5(3) . . ?
O24 Pb5 O15 108.4(7) . 4_656 ?
O2 Pb5 O15 146.3(3) . 4_656 ?
O12 Pb5 O15 88.2(2) . 4_656 ?
O24 Pb5 O18 67.6(9) . 5_676 ?
O2 Pb5 O18 82.2(3) . 5_676 ?
O12 Pb5 O18 145.2(3) . 5_676 ?
O15 Pb5 O18 120.1(3) 4_656 5_676 ?
O24 Pb5 O20 110.4(9) . 5_676 ?
O2 Pb5 O20 93.8(3) . 5_676 ?
O12 Pb5 O20 164.2(3) . 5_676 ?
O15 Pb5 O20 85.5(3) 4_656 5_676 ?
O18 Pb5 O20 48.7(3) 5_676 5_676 ?
O24 Pb5 O21 44.9(8) . . ?
O2 Pb5 O21 146.9(3) . . ?
O12 Pb5 O21 99.9(3) . . ?
O15 Pb5 O21 66.7(2) 4_656 . ?
O18 Pb5 O21 76.5(3) 5_676 . ?
O20 Pb5 O21 91.0(3) 5_676 . ?
C4 O4 Pb2 98.4(5) . 5_676 ?
C4 O4 Pb2 141.2(7) . 3_675 ?
Pb2 O4 Pb2 110.3(2) 5_676 3_675 ?
C27 O9 Pb4 113.9(6) . . ?
C27 O9 Pb1 133.0(6) . 4_656 ?
Pb4 O9 Pb1 109.9(3) . 4_656 ?
C29 O13 Pb3 124.2(4) . . ?
C29 O13 Pb1 117.8(5) . . ?
Pb3 O13 Pb1 115.4(2) . . ?
C9 O8 Pb1 90.8(6) . . ?
C9 O8 Pb4 118.6(7) . 4_546 ?
Pb1 O8 Pb4 107.7(2) . 4_546 ?
C19 O12 Pb5 121.8(7) . . ?
C19 O12 Pb3 124.5(6) . 4_656 ?
Pb5 O12 Pb3 110.2(3) . 4_656 ?
C4 O3 Pb4 154.8(8) . 5_676 ?
C9 O7 Pb1 92.1(5) . . ?
C29 O15 Pb4 124.7(4) . 4_546 ?
C29 O15 Pb5 119.7(5) . 4_546 ?
Pb4 O15 Pb5 115.2(3) 4_546 4_546 ?
C1 O2 Pb5 154.5(10) . . ?
C27 O10 Pb2 101.2(6) . . ?
N2 O21 Pb4 86.3(4) . . ?
N2 O21 Pb5 163.0(7) . . ?
Pb4 O21 Pb5 107.0(4) . . ?
C19 O11 Pb1 102.4(7) . . ?
N1 O20 Pb4 97.9(7) . . ?
N1 O20 Pb5 97.0(7) . 5_676 ?
Pb4 O20 Pb5 161.0(4) . 5_676 ?
C2 C3 C5 120.9(8) . . ?
C2 C3 C4 122.0(7) . . ?
C5 C3 C4 116.9(8) . . ?
C30 C28 C30 118.3(12) 6_765 . ?
C30 C28 H26A 120.8 6_765 . ?
C30 C28 H26A 120.8 . . ?
C25 C26 C20 115.5(9) . . ?
C25 C26 H25A 122.2 . . ?
C20 C26 H25A 122.2 . . ?
C8 C10 C2 117.1(9) . . ?
C8 C10 C1 126.1(9) . . ?
C2 C10 C1 116.0(7) . . ?
C5 C6 C8 118.9(8) . . ?
C5 C6 C7 119.9(10) . . ?
C8 C6 C7 120.7(9) . . ?
C31 C30 C28 119.7(8) . . ?
C31 C30 C29 119.9(8) . . ?
C28 C30 C29 120.3(9) . . ?
C3 C2 C10 118.1(7) . . ?
C3 C2 H21A 120.9 . . ?
C10 C2 H21A 120.9 . . ?
C12 C11 C18 119.0(8) . . ?
C12 C11 C9 123.0(7) . . ?
C18 C11 C9 117.9(8) . . ?
O12 C19 O11 121.4(9) . . ?
O12 C19 C20 121.0(7) . . ?
O11 C19 C20 117.5(9) . . ?
O9 C27 O10 120.6(7) . . ?
O9 C27 C25 123.5(9) . . ?
O10 C27 C25 115.4(8) . . ?
O7 C9 O8 124.0(9) . . ?
O7 C9 C11 120.5(7) . . ?
O8 C9 C11 115.5(8) . . ?
N1 O18 Pb5 100.1(8) . 5_676 ?
C6 C5 C3 121.0(9) . . ?
C6 C5 H16A 119.5 . . ?
C3 C5 H16A 119.5 . . ?
O2 C1 O1 119.6(10) . . ?
O2 C1 C10 126.6(9) . . ?
O1 C1 C10 113.7(8) . . ?
O13 C29 O15 122.6(8) . . ?
O13 C29 C30 119.0(9) . . ?
O15 C29 C30 118.3(8) . . ?
C13 C12 C11 121.3(8) . . ?
C13 C12 H13A 119.3 . . ?
C11 C12 H13A 119.3 . . ?
O6 C14 O5 123.2(9) . . ?
O6 C14 C13 124.2(9) . . ?
O5 C14 C13 112.2(8) . . ?
C24 C25 C26 119.7(9) . . ?
C24 C25 C27 125.3(10) . . ?
C26 C25 C27 115.0(9) . . ?
C10 C8 C6 123.7(9) . . ?
C10 C8 H10A 118.1 . . ?
C6 C8 H10A 118.1 . . ?
C15 C16 C18 118.6(9) . . ?
C15 C16 C17 124.1(12) . . ?
C18 C16 C17 117.3(11) . . ?
C30 C31 C32 122.1(9) . . ?
C30 C31 H54A 118.9 . . ?
C32 C31 H54A 118.9 . . ?
C12 C13 C15 117.1(9) . . ?
C12 C13 C14 117.5(8) . . ?
C15 C13 C14 125.3(9) . . ?
C21 C20 C26 120.2(9) . . ?
C21 C20 C19 119.4(8) . . ?
C26 C20 C19 120.4(9) . . ?
C32 C33 H51A 109.5 . . ?
C32 C33 H51B 109.5 . . ?
H51A C33 H51B 109.5 . . ?
C32 C33 H51C 109.5 . . ?
H51A C33 H51C 109.5 . . ?
H51B C33 H51C 109.5 . . ?
C6 C7 H50A 109.5 . . ?
C6 C7 H50B 109.5 . . ?
H50A C7 H50B 109.5 . . ?
C6 C7 H50C 109.5 . . ?
H50A C7 H50C 109.5 . . ?
H50B C7 H50C 109.5 . . ?
C14 O6 Pb3 101.0(7) . 6_765 ?
C1 O1 Pb3 157.5(11) . . ?
O19 N1 O20 113.1(11) . . ?
O19 N1 O18 130.4(14) . . ?
O20 N1 O18 114.2(10) . . ?
C31 C32 C31 118.1(13) 6_765 . ?
C31 C32 C33 121.0(6) 6_765 . ?
C31 C32 C33 121.0(6) . . ?
N3 O14 Pb2 140.8(5) . 1_445 ?
N3 O14 Pb3 97.2(5) . . ?
Pb2 O14 Pb3 107.15(14) 1_445 . ?
N1 O19 Pb4 100.0(10) . . ?
O4 C4 O3 122.5(9) . . ?
O4 C4 C3 119.8(7) . . ?
O3 C4 C3 117.6(8) . . ?
C24 C22 C21 114.3(13) . . ?
C24 C22 C23 123.3(13) . . ?
C21 C22 C23 121.3(11) . . ?
C16 C15 C13 124.7(10) . . ?
C16 C15 H43A 117.7 . . ?
C13 C15 H43A 117.7 . . ?
C20 C21 C22 120.3(9) . . ?
C20 C21 H42A 119.8 . . ?
C22 C21 H42A 119.8 . . ?
C25 C24 C22 129.2(14) . . ?
C25 C24 H41A 115.4 . . ?
C22 C24 H41A 115.4 . . ?
C16 C18 C11 119.0(9) . . ?
C16 C18 H40A 120.5 . . ?
C11 C18 H40A 120.5 . . ?
C22 C23 H1A 109.5 . . ?
C22 C23 H1B 109.5 . . ?
H1A C23 H1B 109.5 . . ?
C22 C23 H1C 109.5 . . ?
H1A C23 H1C 109.5 . . ?
H1B C23 H1C 109.5 . . ?
C16 C17 H2A 109.5 . . ?
C16 C17 H2B 109.5 . . ?
H2A C17 H2B 109.5 . . ?
C16 C17 H2C 109.5 . . ?
H2A C17 H2C 109.5 . . ?
H2B C17 H2C 109.5 . . ?
N3 O16 Pb3 113.0(4) . . ?
O14 N3 O17 110.1(5) . . ?
O14 N3 O16 103.9(6) . . ?
O17 N3 O16 145.4(7) . . ?
N2 O23 Pb4 106.3(6) . . ?
N2 O22 O22 130.6(4) . 4_556 ?
O23 N2 O22 132.6(9) . . ?
O23 N2 O21 111.1(6) . . ?
O22 N2 O21 115.7(8) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         3.223
_refine_diff_density_min         -3.548
_refine_diff_density_rms         0.420
_database_code_depnum_ccdc_archive 'CCDC 988801'
