# 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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# 
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#  data retrieval see:
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#
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H32 N6 O13 Pb2 S2'
_chemical_formula_weight         1259.20

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'
S S 0.1246 0.1234 '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           TRICLINIC
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6177(15)
_cell_length_b                   13.490(2)
_cell_length_c                   15.996(2)
_cell_angle_alpha                90.087(2)
_cell_angle_beta                 96.643(2)
_cell_angle_gamma                105.861(2)
_cell_volume                     1981.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4086
_cell_measurement_theta_min      2.2176
_cell_measurement_theta_max      25.3664

_exptl_crystal_description       NEEDLE
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1204
_exptl_absorpt_coefficient_mu    8.665
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.085
_exptl_absorpt_correction_T_max  0.273
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean 8.3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17376
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0774
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.28
_diffrn_reflns_theta_max         27.58
_reflns_number_total             8952
_reflns_number_gt                6014
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond (CRYSTAL IMPACT, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0642P)²+0.0000P] where P=(Fo²+2Fc²)/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         8952
_refine_ls_number_parameters     550
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1297
_refine_ls_wR_factor_gt          0.1038
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.5576(12) 0.1664(9) 0.4751(7) 0.059(3) Uani 1 1 d . . .
H1 H 0.5338 0.1062 0.4418 0.071 Uiso 1 1 calc R . .
C2 C 0.7005(11) 0.2034(10) 0.5183(7) 0.060(3) Uani 1 1 d . . .
H2 H 0.7682 0.1664 0.5142 0.072 Uiso 1 1 calc R . .
C3 C 0.7391(11) 0.2933(10) 0.5659(7) 0.062(3) Uani 1 1 d . . .
H3 H 0.8326 0.3180 0.5941 0.074 Uiso 1 1 calc R . .
C4 C 0.6373(11) 0.3460(9) 0.5711(6) 0.051(3) Uani 1 1 d . . .
C5 C 0.6687(14) 0.4403(11) 0.6196(7) 0.070(4) Uani 1 1 d . . .
H5A H 0.7625 0.4676 0.6467 0.084 Uiso 1 1 calc R . .
C6 C 0.5690(15) 0.4909(9) 0.6276(7) 0.069(4) Uani 1 1 d . . .
H6 H 0.5948 0.5537 0.6575 0.083 Uiso 1 1 calc R . .
C7 C 0.4211(14) 0.4474(8) 0.5895(6) 0.055(3) Uani 1 1 d . . .
C8 C 0.3816(11) 0.3555(7) 0.5413(6) 0.042(2) Uani 1 1 d . . .
C9 C 0.4938(10) 0.3049(7) 0.5305(6) 0.037(2) Uani 1 1 d . . .
C10 C 0.1438(11) 0.3551(8) 0.5180(6) 0.048(3) Uani 1 1 d . . .
H10 H 0.0490 0.3246 0.4937 0.057 Uiso 1 1 calc R . .
C11 C 0.1719(15) 0.4483(8) 0.5658(8) 0.064(3) Uani 1 1 d . . .
H11 H 0.0973 0.4778 0.5737 0.077 Uiso 1 1 calc R . .
C12 C 0.3122(15) 0.4938(9) 0.6002(8) 0.067(3) Uani 1 1 d . . .
H12 H 0.3343 0.5560 0.6308 0.080 Uiso 1 1 calc R . .
C13 C 0.0541(10) 0.2600(7) 0.3138(5) 0.035(2) Uani 1 1 d . . .
C14 C -0.0034(9) 0.3326(6) 0.2602(5) 0.0286(19) Uani 1 1 d . . .
C15 C 0.0861(10) 0.3961(7) 0.2089(6) 0.041(2) Uani 1 1 d . . .
H15 H 0.1812 0.3917 0.2105 0.049 Uiso 1 1 calc R . .
C16 C -0.1474(10) 0.3386(7) 0.2583(6) 0.037(2) Uani 1 1 d . . .
C17 C -0.1906(10) 0.4109(7) 0.2054(6) 0.039(2) Uani 1 1 d . . .
H17 H -0.2850 0.4168 0.2039 0.047 Uiso 1 1 calc R . .
C18 C -0.0993(9) 0.4720(6) 0.1566(5) 0.033(2) Uani 1 1 d . . .
C19 C 0.0431(10) 0.4664(7) 0.1547(6) 0.037(2) Uani 1 1 d . . .
H19 H 0.1052 0.5067 0.1198 0.044 Uiso 1 1 calc R . .
C20 C 0.4870(8) 0.8218(6) 0.2720(5) 0.0288(19) Uani 1 1 d . . .
C21 C 0.5544(9) 0.7460(7) 0.2518(5) 0.034(2) Uani 1 1 d . . .
C22 C 0.7048(10) 0.7646(7) 0.2806(5) 0.034(2) Uani 1 1 d . . .
H22 H 0.7532 0.7167 0.2675 0.041 Uiso 1 1 calc R . .
C23 C 0.7788(9) 0.8510(7) 0.3268(5) 0.0316(19) Uani 1 1 d . . .
C24 C 0.7139(10) 0.9255(7) 0.3495(6) 0.039(2) Uani 1 1 d . . .
H24 H 0.7660 0.9834 0.3826 0.047 Uiso 1 1 calc R . .
C25 C 0.5675(10) 0.9093(7) 0.3206(5) 0.040(2) Uani 1 1 d . . .
H25 H 0.5213 0.9583 0.3341 0.048 Uiso 1 1 calc R . .
C26 C 0.3346(10) 0.8134(8) 0.2373(6) 0.037(2) Uani 1 1 d . . .
C27 C 0.2553(12) 0.7595(8) 0.0128(7) 0.054(3) Uani 1 1 d . . .
H27 H 0.2324 0.6962 0.0385 0.065 Uiso 1 1 calc R . .
C28 C 0.3381(14) 0.7705(11) -0.0540(8) 0.075(4) Uani 1 1 d . . .
H28 H 0.3646 0.7145 -0.0742 0.090 Uiso 1 1 calc R . .
C29 C 0.3791(15) 0.8613(13) -0.0886(8) 0.084(5) Uani 1 1 d . . .
H29 H 0.4400 0.8701 -0.1307 0.101 Uiso 1 1 calc R . .
C30 C 0.3319(14) 0.9434(11) -0.0627(8) 0.066(3) Uani 1 1 d . . .
C31 C 0.2491(11) 0.9301(7) 0.0055(6) 0.045(3) Uani 1 1 d . . .
C32 C 0.3705(17) 1.0431(14) -0.0971(9) 0.101(6) Uani 1 1 d . . .
H32 H 0.4309 1.0555 -0.1395 0.121 Uiso 1 1 calc R . .
C33 C 0.3199(18) 1.1214(12) -0.0686(9) 0.096(6) Uani 1 1 d . . .
H33 H 0.3412 1.1842 -0.0950 0.115 Uiso 1 1 calc R . .
C34 C 0.1992(11) 1.0130(7) 0.0371(6) 0.045(3) Uani 1 1 d . . .
C35 C 0.1866(18) 1.1880(9) 0.0306(9) 0.092(6) Uani 1 1 d . . .
H35 H 0.2100 1.2529 0.0076 0.110 Uiso 1 1 calc R . .
C36 C 0.2373(15) 1.1093(9) -0.0009(7) 0.069(4) Uani 1 1 d . . .
C37 C 0.1046(18) 1.1696(10) 0.0936(10) 0.084(5) Uani 1 1 d . . .
H37 H 0.0698 1.2219 0.1135 0.101 Uiso 1 1 calc R . .
C38 C 0.0687(13) 1.0706(8) 0.1312(7) 0.062(3) Uani 1 1 d . . .
H38 H 0.0123 1.0593 0.1756 0.074 Uiso 1 1 calc R . .
N1 N -0.2502(9) 0.2748(7) 0.3047(6) 0.061(3) Uani 1 1 d . . .
H1A H -0.2262 0.2291 0.3363 0.074 Uiso 1 1 calc R . .
H1B H -0.3371 0.2813 0.3014 0.074 Uiso 1 1 calc R . .
N2 N 0.2441(8) 0.3096(5) 0.5060(4) 0.0335(17) Uani 1 1 d . . .
N3 N 0.4575(8) 0.2161(6) 0.4813(5) 0.0393(19) Uani 1 1 d . . .
N4 N 0.4870(9) 0.6603(6) 0.2020(6) 0.054(2) Uani 1 1 d . . .
H4A H 0.3977 0.6500 0.1807 0.065 Uiso 1 1 calc R . .
H4B H 0.5338 0.6165 0.1918 0.065 Uiso 1 1 calc R . .
N5 N 0.2060(8) 0.8363(6) 0.0425(5) 0.0379(18) Uani 1 1 d . . .
N6 N 0.1165(9) 0.9958(6) 0.1024(5) 0.048(2) Uani 1 1 d . . .
O1 O 0.1855(7) 0.2584(5) 0.3132(4) 0.0455(17) Uani 1 1 d . . .
O2 O -0.0253(7) 0.2016(5) 0.3625(4) 0.0439(16) Uani 1 1 d . . .
O3 O -0.2565(8) 0.4942(5) 0.0195(5) 0.059(2) Uani 1 1 d . . .
O4 O -0.0434(7) 0.6324(5) 0.0643(5) 0.0516(19) Uani 1 1 d . . .
O5 O 1.0374(7) 0.9606(5) 0.3080(4) 0.0500(18) Uani 1 1 d . . .
O6 O 0.9988(7) 0.8992(5) 0.4471(4) 0.0449(16) Uani 1 1 d . . .
O7 O 1.0071(7) 0.7809(5) 0.3334(4) 0.0420(16) Uani 1 1 d . . .
O8 O 0.2916(7) 0.8956(5) 0.2341(4) 0.0395(15) Uani 1 1 d . . .
O9 O 0.2465(7) 0.7286(5) 0.2101(4) 0.0399(15) Uani 1 1 d . . .
O10 O -0.2526(8) 0.6042(6) 0.1386(5) 0.065(2) Uani 1 1 d . . .
O1W O 0.3527(8) 0.0911(5) 0.3101(5) 0.058(2) Uani 1 1 d . . .
H1WA H 0.3782 0.1417 0.2781 0.087 Uiso 1 1 d R . .
H1WB H 0.3326 0.0350 0.2808 0.087 Uiso 1 1 d R . .
O2W O 0.4354(8) 0.2874(6) 0.2311(5) 0.065(2) Uani 1 1 d . . .
H2WA H 0.4493 0.3189 0.1853 0.098 Uiso 1 1 d R . .
H2WB H 0.3451 0.2717 0.2366 0.098 Uiso 1 1 d R . .
O3W O 0.4483(9) 0.4302(7) 0.1002(5) 0.079(3) Uani 1 1 d . . .
H3WA H 0.4612 0.3896 0.0628 0.119 Uiso 1 1 d R . .
H3WB H 0.3770 0.4533 0.0823 0.119 Uiso 1 1 d R . .
Pb1 Pb 0.18261(3) 0.13358(2) 0.42495(2) 0.03397(11) Uani 1 1 d . . .
Pb2 Pb 0.05582(3) 0.81201(3) 0.16217(2) 0.03478(11) Uani 1 1 d . . .
S1 S 0.9697(2) 0.87335(18) 0.35688(14) 0.0344(5) Uani 1 1 d . . .
S2 S -0.1677(3) 0.55774(17) 0.08949(15) 0.0369(5) Uani 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
C1 N3 1.327(13) . ?
C1 C2 1.421(15) . ?
C1 H1 0.9300 . ?
C2 C3 1.369(17) . ?
C2 H2 0.9300 . ?
C3 C4 1.368(16) . ?
C3 H3 0.9300 . ?
C4 C9 1.417(12) . ?
C4 C5 1.429(16) . ?
C5 C6 1.337(18) . ?
C5 H5A 0.9300 . ?
C6 C7 1.442(16) . ?
C6 H6 0.9300 . ?
C7 C12 1.385(16) . ?
C7 C8 1.396(14) . ?
C8 N2 1.353(11) . ?
C8 C9 1.451(13) . ?
C9 N3 1.372(12) . ?
C10 N2 1.307(12) . ?
C10 C11 1.416(15) . ?
C10 H10 0.9300 . ?
C11 C12 1.369(17) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 O1 1.271(10) . ?
C13 O2 1.274(10) . ?
C13 C14 1.480(11) . ?
C14 C15 1.382(12) . ?
C14 C16 1.406(11) . ?
C15 C19 1.398(11) . ?
C15 H15 0.9300 . ?
C16 N1 1.406(11) . ?
C16 C17 1.409(11) . ?
C17 C18 1.351(12) . ?
C17 H17 0.9300 . ?
C18 C19 1.396(12) . ?
C18 S2 1.782(8) . ?
C19 H19 0.9300 . ?
C20 C25 1.398(12) . ?
C20 C21 1.408(12) . ?
C20 C26 1.480(11) . ?
C21 N4 1.363(12) . ?
C21 C22 1.419(12) . ?
C22 C23 1.355(12) . ?
C22 H22 0.9300 . ?
C23 C24 1.387(12) . ?
C23 S1 1.784(9) . ?
C24 C25 1.387(13) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 O9 1.265(11) . ?
C26 O8 1.284(10) . ?
C26 Pb2 2.804(9) . ?
C27 N5 1.357(13) . ?
C27 C28 1.390(16) . ?
C27 H27 0.9300 . ?
C28 C29 1.323(18) . ?
C28 H28 0.9300 . ?
C29 C30 1.385(19) . ?
C29 H29 0.9300 . ?
C30 C31 1.408(15) . ?
C30 C32 1.423(19) . ?
C31 N5 1.376(11) . ?
C31 C34 1.445(14) . ?
C32 C33 1.37(2) . ?
C32 H32 0.9300 . ?
C33 C36 1.40(2) . ?
C33 H33 0.9300 . ?
C34 N6 1.367(13) . ?
C34 C36 1.409(13) . ?
C35 C37 1.33(2) . ?
C35 C36 1.40(2) . ?
C35 H35 0.9300 . ?
C37 C38 1.437(17) . ?
C37 H37 0.9300 . ?
C38 N6 1.321(12) . ?
C38 H38 0.9300 . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N2 Pb1 2.591(7) . ?
N3 Pb1 2.623(8) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N5 Pb2 2.499(7) . ?
N6 Pb2 2.597(8) . ?
O1 Pb1 2.455(6) . ?
O2 Pb1 2.527(6) . ?
O3 S2 1.447(7) . ?
O4 S2 1.435(7) . ?
O4 Pb2 2.759(7) . ?
O5 S1 1.457(6) . ?
O6 S1 1.460(7) . ?
O7 S1 1.450(6) . ?
O8 Pb2 2.394(6) . ?
O9 Pb2 2.455(6) . ?
O10 S2 1.450(7) . ?
O1W Pb1 2.754(8) . ?
O1W H1WA 0.8529 . ?
O1W H1WB 0.8533 . ?
O2W H2WA 0.8528 . ?
O2W H2WB 0.8513 . ?
O3W H3WA 0.8516 . ?
O3W H3WB 0.8499 . ?

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
N3 C1 C2 121.3(12) . . ?
N3 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
C3 C2 C1 120.3(10) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 118.6(10) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C9 119.8(11) . . ?
C3 C4 C5 122.1(11) . . ?
C9 C4 C5 118.0(11) . . ?
C6 C5 C4 122.8(11) . . ?
C6 C5 H5A 118.6 . . ?
C4 C5 H5A 118.6 . . ?
C5 C6 C7 119.6(12) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C12 C7 C8 117.3(11) . . ?
C12 C7 C6 121.7(11) . . ?
C8 C7 C6 121.1(12) . . ?
N2 C8 C7 123.7(10) . . ?
N2 C8 C9 118.2(9) . . ?
C7 C8 C9 118.0(10) . . ?
N3 C9 C4 120.9(9) . . ?
N3 C9 C8 118.7(8) . . ?
C4 C9 C8 120.4(9) . . ?
N2 C10 C11 123.6(11) . . ?
N2 C10 H10 118.2 . . ?
C11 C10 H10 118.2 . . ?
C12 C11 C10 118.0(11) . . ?
C12 C11 H11 121.0 . . ?
C10 C11 H11 121.0 . . ?
C11 C12 C7 120.1(11) . . ?
C11 C12 H12 120.0 . . ?
C7 C12 H12 120.0 . . ?
O1 C13 O2 119.7(8) . . ?
O1 C13 C14 119.7(8) . . ?
O2 C13 C14 120.6(8) . . ?
C15 C14 C16 118.3(7) . . ?
C15 C14 C13 119.3(7) . . ?
C16 C14 C13 122.4(8) . . ?
C14 C15 C19 124.4(8) . . ?
C14 C15 H15 117.8 . . ?
C19 C15 H15 117.8 . . ?
N1 C16 C14 123.4(8) . . ?
N1 C16 C17 118.9(8) . . ?
C14 C16 C17 117.7(8) . . ?
C18 C17 C16 122.1(8) . . ?
C18 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
C17 C18 C19 122.0(8) . . ?
C17 C18 S2 118.1(7) . . ?
C19 C18 S2 119.8(7) . . ?
C18 C19 C15 115.5(8) . . ?
C18 C19 H19 122.2 . . ?
C15 C19 H19 122.2 . . ?
C25 C20 C21 119.7(8) . . ?
C25 C20 C26 119.6(8) . . ?
C21 C20 C26 120.5(8) . . ?
N4 C21 C20 124.1(8) . . ?
N4 C21 C22 118.6(8) . . ?
C20 C21 C22 117.1(8) . . ?
C23 C22 C21 121.1(8) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C24 122.9(8) . . ?
C22 C23 S1 119.0(7) . . ?
C24 C23 S1 118.0(7) . . ?
C23 C24 C25 116.8(9) . . ?
C23 C24 H24 121.6 . . ?
C25 C24 H24 121.6 . . ?
C24 C25 C20 122.4(9) . . ?
C24 C25 H25 118.8 . . ?
C20 C25 H25 118.8 . . ?
O9 C26 O8 119.3(8) . . ?
O9 C26 C20 122.3(8) . . ?
O8 C26 C20 118.4(9) . . ?
O9 C26 Pb2 61.0(5) . . ?
O8 C26 Pb2 58.4(4) . . ?
C20 C26 Pb2 174.9(7) . . ?
N5 C27 C28 123.4(11) . . ?
N5 C27 H27 118.3 . . ?
C28 C27 H27 118.3 . . ?
C29 C28 C27 119.5(14) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 C30 120.7(13) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C29 C30 C31 118.3(12) . . ?
C29 C30 C32 124.0(14) . . ?
C31 C30 C32 117.5(14) . . ?
N5 C31 C30 121.6(10) . . ?
N5 C31 C34 116.9(9) . . ?
C30 C31 C34 121.4(10) . . ?
C33 C32 C30 121.1(13) . . ?
C33 C32 H32 119.4 . . ?
C30 C32 H32 119.4 . . ?
C32 C33 C36 121.9(12) . . ?
C32 C33 H33 119.0 . . ?
C36 C33 H33 119.0 . . ?
N6 C34 C36 122.2(11) . . ?
N6 C34 C31 119.2(8) . . ?
C36 C34 C31 118.6(11) . . ?
C37 C35 C36 119.8(12) . . ?
C37 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C33 123.3(13) . . ?
C35 C36 C34 117.4(13) . . ?
C33 C36 C34 119.3(13) . . ?
C35 C37 C38 121.3(13) . . ?
C35 C37 H37 119.3 . . ?
C38 C37 H37 119.3 . . ?
N6 C38 C37 119.5(13) . . ?
N6 C38 H38 120.3 . . ?
C37 C38 H38 120.3 . . ?
C16 N1 H1A 120.0 . . ?
C16 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C10 N2 C8 117.4(9) . . ?
C10 N2 Pb1 122.0(7) . . ?
C8 N2 Pb1 120.6(6) . . ?
C1 N3 C9 118.9(9) . . ?
C1 N3 Pb1 121.8(7) . . ?
C9 N3 Pb1 118.4(6) . . ?
C21 N4 H4A 120.0 . . ?
C21 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C27 N5 C31 116.2(9) . . ?
C27 N5 Pb2 122.1(6) . . ?
C31 N5 Pb2 121.6(7) . . ?
C38 N6 C34 119.9(9) . . ?
C38 N6 Pb2 122.9(8) . . ?
C34 N6 Pb2 117.3(6) . . ?
C13 O1 Pb1 95.6(5) . . ?
C13 O2 Pb1 92.2(5) . . ?
S2 O4 Pb2 115.8(4) . . ?
C26 O8 Pb2 94.5(5) . . ?
C26 O9 Pb2 92.2(5) . . ?
Pb1 O1W H1WA 110.8 . . ?
Pb1 O1W H1WB 124.5 . . ?
H1WA O1W H1WB 108.9 . . ?
H2WA O2W H2WB 109.0 . . ?
H3WA O3W H3WB 109.5 . . ?
O1 Pb1 O2 52.4(2) . . ?
O1 Pb1 N2 76.1(2) . . ?
O2 Pb1 N2 79.2(2) . . ?
O1 Pb1 N3 93.0(2) . . ?
O2 Pb1 N3 135.2(2) . . ?
N2 Pb1 N3 63.7(2) . . ?
O1 Pb1 O1W 73.1(2) . . ?
O2 Pb1 O1W 114.8(2) . . ?
N2 Pb1 O1W 122.7(2) . . ?
N3 Pb1 O1W 71.1(2) . . ?
O8 Pb2 O9 53.9(2) . . ?
O8 Pb2 N5 79.3(2) . . ?
O9 Pb2 N5 77.1(2) . . ?
O8 Pb2 N6 76.3(2) . . ?
O9 Pb2 N6 121.9(2) . . ?
N5 Pb2 N6 64.9(3) . . ?
O8 Pb2 O4 131.3(2) . . ?
O9 Pb2 O4 80.5(2) . . ?
N5 Pb2 O4 73.9(2) . . ?
N6 Pb2 O4 124.2(2) . . ?
O8 Pb2 C26 27.2(2) . . ?
O9 Pb2 C26 26.8(2) . . ?
N5 Pb2 C26 75.8(3) . . ?
N6 Pb2 C26 99.1(3) . . ?
O4 Pb2 C26 105.6(2) . . ?
O7 S1 O5 111.5(4) . . ?
O7 S1 O6 114.0(4) . . ?
O5 S1 O6 111.3(4) . . ?
O7 S1 C23 107.1(4) . . ?
O5 S1 C23 104.7(4) . . ?
O6 S1 C23 107.7(4) . . ?
O4 S2 O3 112.7(5) . . ?
O4 S2 O10 112.3(5) . . ?
O3 S2 O10 112.1(5) . . ?
O4 S2 C18 106.7(4) . . ?
O3 S2 C18 105.7(4) . . ?
O10 S2 C18 106.8(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
N3 C1 C2 C3 -1.6(17) . . . . ?
C1 C2 C3 C4 0.3(17) . . . . ?
C2 C3 C4 C9 2.6(16) . . . . ?
C2 C3 C4 C5 179.9(10) . . . . ?
C3 C4 C5 C6 -177.7(11) . . . . ?
C9 C4 C5 C6 -0.3(17) . . . . ?
C4 C5 C6 C7 3.0(18) . . . . ?
C5 C6 C7 C12 176.1(12) . . . . ?
C5 C6 C7 C8 -2.8(17) . . . . ?
C12 C7 C8 N2 -0.8(15) . . . . ?
C6 C7 C8 N2 178.1(9) . . . . ?
C12 C7 C8 C9 -179.0(9) . . . . ?
C6 C7 C8 C9 -0.1(14) . . . . ?
C3 C4 C9 N3 -4.3(14) . . . . ?
C5 C4 C9 N3 178.3(9) . . . . ?
C3 C4 C9 C8 174.8(9) . . . . ?
C5 C4 C9 C8 -2.6(14) . . . . ?
N2 C8 C9 N3 3.6(12) . . . . ?
C7 C8 C9 N3 -178.1(8) . . . . ?
N2 C8 C9 C4 -175.5(8) . . . . ?
C7 C8 C9 C4 2.8(13) . . . . ?
N2 C10 C11 C12 1.1(16) . . . . ?
C10 C11 C12 C7 -1.6(17) . . . . ?
C8 C7 C12 C11 1.4(17) . . . . ?
C6 C7 C12 C11 -177.5(11) . . . . ?
O1 C13 C14 C15 1.4(13) . . . . ?
O2 C13 C14 C15 179.1(9) . . . . ?
O1 C13 C14 C16 -179.7(9) . . . . ?
O2 C13 C14 C16 -2.0(14) . . . . ?
C16 C14 C15 C19 0.0(15) . . . . ?
C13 C14 C15 C19 178.9(9) . . . . ?
C15 C14 C16 N1 177.0(9) . . . . ?
C13 C14 C16 N1 -1.9(15) . . . . ?
C15 C14 C16 C17 -1.4(13) . . . . ?
C13 C14 C16 C17 179.7(9) . . . . ?
N1 C16 C17 C18 -177.4(9) . . . . ?
C14 C16 C17 C18 1.1(15) . . . . ?
C16 C17 C18 C19 0.8(15) . . . . ?
C16 C17 C18 S2 178.0(8) . . . . ?
C17 C18 C19 C15 -2.2(14) . . . . ?
S2 C18 C19 C15 -179.3(7) . . . . ?
C14 C15 C19 C18 1.8(15) . . . . ?
C25 C20 C21 N4 -177.2(9) . . . . ?
C26 C20 C21 N4 -1.5(13) . . . . ?
C25 C20 C21 C22 -1.8(12) . . . . ?
C26 C20 C21 C22 173.9(8) . . . . ?
N4 C21 C22 C23 176.8(8) . . . . ?
C20 C21 C22 C23 1.2(12) . . . . ?
C21 C22 C23 C24 0.6(13) . . . . ?
C21 C22 C23 S1 -177.0(6) . . . . ?
C22 C23 C24 C25 -1.7(13) . . . . ?
S1 C23 C24 C25 175.9(7) . . . . ?
C23 C24 C25 C20 1.0(13) . . . . ?
C21 C20 C25 C24 0.7(13) . . . . ?
C26 C20 C25 C24 -174.9(8) . . . . ?
C25 C20 C26 O9 -163.3(8) . . . . ?
C21 C20 C26 O9 21.0(13) . . . . ?
C25 C20 C26 O8 17.4(13) . . . . ?
C21 C20 C26 O8 -158.3(8) . . . . ?
N5 C27 C28 C29 3.8(19) . . . . ?
C27 C28 C29 C30 -4(2) . . . . ?
C28 C29 C30 C31 5(2) . . . . ?
C28 C29 C30 C32 -179.7(14) . . . . ?
C29 C30 C31 N5 -4.7(17) . . . . ?
C32 C30 C31 N5 179.6(11) . . . . ?
C29 C30 C31 C34 178.5(11) . . . . ?
C32 C30 C31 C34 2.8(16) . . . . ?
C29 C30 C32 C33 180.0(15) . . . . ?
C31 C30 C32 C33 -5(2) . . . . ?
C30 C32 C33 C36 5(2) . . . . ?
N5 C31 C34 N6 1.7(13) . . . . ?
C30 C31 C34 N6 178.6(9) . . . . ?
N5 C31 C34 C36 -178.0(9) . . . . ?
C30 C31 C34 C36 -1.1(14) . . . . ?
C37 C35 C36 C33 177.9(13) . . . . ?
C37 C35 C36 C34 -0.6(18) . . . . ?
C32 C33 C36 C35 178.8(14) . . . . ?
C32 C33 C36 C34 -3(2) . . . . ?
N6 C34 C36 C35 -0.2(15) . . . . ?
C31 C34 C36 C35 179.5(9) . . . . ?
N6 C34 C36 C33 -178.8(10) . . . . ?
C31 C34 C36 C33 0.9(15) . . . . ?
C36 C35 C37 C38 1(2) . . . . ?
C35 C37 C38 N6 -0.8(19) . . . . ?
C11 C10 N2 C8 -0.4(13) . . . . ?
C11 C10 N2 Pb1 176.4(7) . . . . ?
C7 C8 N2 C10 0.3(13) . . . . ?
C9 C8 N2 C10 178.5(8) . . . . ?
C7 C8 N2 Pb1 -176.5(7) . . . . ?
C9 C8 N2 Pb1 1.7(10) . . . . ?
C2 C1 N3 C9 0.0(15) . . . . ?
C2 C1 N3 Pb1 -168.9(8) . . . . ?
C4 C9 N3 C1 2.9(13) . . . . ?
C8 C9 N3 C1 -176.2(9) . . . . ?
C4 C9 N3 Pb1 172.2(6) . . . . ?
C8 C9 N3 Pb1 -6.9(10) . . . . ?
C28 C27 N5 C31 -3.4(15) . . . . ?
C28 C27 N5 Pb2 179.6(9) . . . . ?
C30 C31 N5 C27 3.9(14) . . . . ?
C34 C31 N5 C27 -179.2(8) . . . . ?
C30 C31 N5 Pb2 -179.1(8) . . . . ?
C34 C31 N5 Pb2 -2.1(11) . . . . ?
C37 C38 N6 C34 -0.1(15) . . . . ?
C37 C38 N6 Pb2 -178.7(8) . . . . ?
C36 C34 N6 C38 0.5(14) . . . . ?
C31 C34 N6 C38 -179.2(9) . . . . ?
C36 C34 N6 Pb2 179.2(7) . . . . ?
C31 C34 N6 Pb2 -0.5(11) . . . . ?
O2 C13 O1 Pb1 -2.6(9) . . . . ?
C14 C13 O1 Pb1 175.1(7) . . . . ?
O1 C13 O2 Pb1 2.5(9) . . . . ?
C14 C13 O2 Pb1 -175.1(7) . . . . ?
O9 C26 O8 Pb2 -4.0(9) . . . . ?
C20 C26 O8 Pb2 175.4(7) . . . . ?
O8 C26 O9 Pb2 3.8(9) . . . . ?
C20 C26 O9 Pb2 -175.4(8) . . . . ?
C13 O1 Pb1 O2 1.4(5) . . . . ?
C13 O1 Pb1 N2 -85.6(6) . . . . ?
C13 O1 Pb1 N3 -147.5(6) . . . . ?
C13 O1 Pb1 O1W 143.3(6) . . . . ?
C13 O2 Pb1 O1 -1.4(5) . . . . ?
C13 O2 Pb1 N2 79.2(6) . . . . ?
C13 O2 Pb1 N3 45.7(7) . . . . ?
C13 O2 Pb1 O1W -42.0(6) . . . . ?
C10 N2 Pb1 O1 79.2(7) . . . . ?
C8 N2 Pb1 O1 -104.1(6) . . . . ?
C10 N2 Pb1 O2 25.5(6) . . . . ?
C8 N2 Pb1 O2 -157.8(6) . . . . ?
C10 N2 Pb1 N3 179.8(7) . . . . ?
C8 N2 Pb1 N3 -3.6(6) . . . . ?
C10 N2 Pb1 O1W 138.2(6) . . . . ?
C8 N2 Pb1 O1W -45.1(7) . . . . ?
C1 N3 Pb1 O1 -112.9(8) . . . . ?
C9 N3 Pb1 O1 78.2(6) . . . . ?
C1 N3 Pb1 O2 -148.4(7) . . . . ?
C9 N3 Pb1 O2 42.7(7) . . . . ?
C1 N3 Pb1 N2 174.3(8) . . . . ?
C9 N3 Pb1 N2 5.3(6) . . . . ?
C1 N3 Pb1 O1W -41.9(7) . . . . ?
C9 N3 Pb1 O1W 149.2(7) . . . . ?
C26 O8 Pb2 O9 2.2(5) . . . . ?
C26 O8 Pb2 N5 -79.6(5) . . . . ?
C26 O8 Pb2 N6 -146.1(6) . . . . ?
C26 O8 Pb2 O4 -22.3(6) . . . . ?
C26 O9 Pb2 O8 -2.2(5) . . . . ?
C26 O9 Pb2 N5 83.9(5) . . . . ?
C26 O9 Pb2 N6 34.8(6) . . . . ?
C26 O9 Pb2 O4 159.4(6) . . . . ?
C27 N5 Pb2 O8 98.5(7) . . . . ?
C31 N5 Pb2 O8 -78.4(7) . . . . ?
C27 N5 Pb2 O9 43.3(7) . . . . ?
C31 N5 Pb2 O9 -133.6(7) . . . . ?
C27 N5 Pb2 N6 178.2(8) . . . . ?
C31 N5 Pb2 N6 1.3(6) . . . . ?
C27 N5 Pb2 O4 -40.4(7) . . . . ?
C31 N5 Pb2 O4 142.8(7) . . . . ?
C27 N5 Pb2 C26 70.9(7) . . . . ?
C31 N5 Pb2 C26 -106.0(7) . . . . ?
C38 N6 Pb2 O8 -97.3(8) . . . . ?
C34 N6 Pb2 O8 84.1(6) . . . . ?
C38 N6 Pb2 O9 -127.3(8) . . . . ?
C34 N6 Pb2 O9 54.1(7) . . . . ?
C38 N6 Pb2 N5 178.2(8) . . . . ?
C34 N6 Pb2 N5 -0.4(6) . . . . ?
C38 N6 Pb2 O4 131.8(7) . . . . ?
C34 N6 Pb2 O4 -46.8(7) . . . . ?
C38 N6 Pb2 C26 -112.2(8) . . . . ?
C34 N6 Pb2 C26 69.1(7) . . . . ?
S2 O4 Pb2 O8 125.5(4) . . . . ?
S2 O4 Pb2 O9 105.6(4) . . . . ?
S2 O4 Pb2 N5 -175.1(4) . . . . ?
S2 O4 Pb2 N6 -132.1(4) . . . . ?
S2 O4 Pb2 C26 115.1(4) . . . . ?
O9 C26 Pb2 O8 176.1(9) . . . . ?
O8 C26 Pb2 O9 -176.1(9) . . . . ?
O9 C26 Pb2 N5 -89.6(5) . . . . ?
O8 C26 Pb2 N5 94.4(5) . . . . ?
O9 C26 Pb2 N6 -150.7(5) . . . . ?
O8 C26 Pb2 N6 33.3(6) . . . . ?
O9 C26 Pb2 O4 -21.2(6) . . . . ?
O8 C26 Pb2 O4 162.8(5) . . . . ?
C22 C23 S1 O7 -7.9(8) . . . . ?
C24 C23 S1 O7 174.4(7) . . . . ?
C22 C23 S1 O5 110.6(7) . . . . ?
C24 C23 S1 O5 -67.1(8) . . . . ?
C22 C23 S1 O6 -130.9(7) . . . . ?
C24 C23 S1 O6 51.4(8) . . . . ?
Pb2 O4 S2 O3 151.0(4) . . . . ?
Pb2 O4 S2 O10 23.3(5) . . . . ?
Pb2 O4 S2 C18 -93.4(4) . . . . ?
C17 C18 S2 O4 163.6(8) . . . . ?
C19 C18 S2 O4 -19.2(9) . . . . ?
C17 C18 S2 O3 -76.2(9) . . . . ?
C19 C18 S2 O3 101.0(8) . . . . ?
C17 C18 S2 O10 43.4(9) . . . . ?
C19 C18 S2 O10 -139.4(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.842
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.211
_database_code_depnum_ccdc_archive 'CCDC 835434'
#######################################################################
#
#                 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_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H32 N6 O13 Pb2 S2'
_chemical_formula_weight         1211.20

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           TRICLINIC
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7272(10)
_cell_length_b                   13.4690(14)
_cell_length_c                   15.4478(16)
_cell_angle_alpha                89.2900(10)
_cell_angle_beta                 83.6170(10)
_cell_angle_gamma                70.4760(10)
_cell_volume                     1895.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6915
_cell_measurement_theta_min      2.2741
_cell_measurement_theta_max      27.5136

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1156
_exptl_absorpt_coefficient_mu    9.057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.154
_exptl_absorpt_correction_T_max  0.404
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean 8.3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16657
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         27.56
_reflns_number_total             8555
_reflns_number_gt                6879
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond (CRYSTAL IMPACT, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0616P)²+1.1077P] where P=(Fo²+2Fc²)/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         8555
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1294
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 -0.1442(8) 0.6643(6) 0.2778(5) 0.0300(15) Uani 1 1 d . . .
C2 C 0.0068(7) 0.6591(5) 0.2417(4) 0.0248(13) Uani 1 1 d . . .
C3 C 0.0662(7) 0.7375(6) 0.2613(5) 0.0325(15) Uani 1 1 d . . .
C4 C 0.2138(8) 0.7212(5) 0.2316(4) 0.0304(15) Uani 1 1 d . . .
H4 H 0.2550 0.7719 0.2437 0.036 Uiso 1 1 calc R . .
C5 C 0.2983(8) 0.6316(6) 0.1850(4) 0.0309(15) Uani 1 1 d . . .
C6 C 0.2409(8) 0.5525(6) 0.1651(5) 0.0391(17) Uani 1 1 d . . .
H6 H 0.2990 0.4914 0.1341 0.047 Uiso 1 1 calc R . .
C7 C 0.0950(8) 0.5692(6) 0.1935(5) 0.0328(16) Uani 1 1 d . . .
H7 H 0.0541 0.5188 0.1799 0.039 Uiso 1 1 calc R . .
C8 C 0.7669(9) 0.7266(7) 0.5066(6) 0.046(2) Uani 1 1 d . . .
H8 H 0.7327 0.7908 0.4794 0.056 Uiso 1 1 calc R . .
C9 C 0.8608(10) 0.7179(9) 0.5699(7) 0.062(3) Uani 1 1 d . . .
H9 H 0.8916 0.7734 0.5842 0.074 Uiso 1 1 calc R . .
C10 C 0.9057(11) 0.6222(10) 0.6104(7) 0.074(3) Uani 1 1 d . . .
H10 H 0.9662 0.6130 0.6545 0.088 Uiso 1 1 calc R . .
C11 C 0.8626(13) 0.5411(10) 0.5865(7) 0.071(3) Uani 1 1 d . . .
H11 H 0.8933 0.4771 0.6144 0.086 Uiso 1 1 calc R . .
C12 C 0.7732(8) 0.5541(6) 0.5207(5) 0.0384(17) Uani 1 1 d . . .
C13 C 0.7264(8) 0.4687(6) 0.4867(6) 0.043(2) Uani 1 1 d . . .
C14 C 0.7677(10) 0.3693(7) 0.5251(7) 0.065(3) Uani 1 1 d . . .
H14 H 0.8228 0.3554 0.5720 0.078 Uiso 1 1 calc R . .
C15 C 0.7214(13) 0.2912(7) 0.4890(8) 0.075(4) Uani 1 1 d . . .
H15 H 0.7472 0.2241 0.5118 0.091 Uiso 1 1 calc R . .
C16 C 0.6406(13) 0.3137(7) 0.4221(7) 0.069(3) Uani 1 1 d . . .
H16 H 0.6085 0.2633 0.3985 0.082 Uiso 1 1 calc R . .
C17 C 0.6063(12) 0.4128(8) 0.3892(7) 0.066(3) Uani 1 1 d . . .
H17 H 0.5524 0.4268 0.3417 0.079 Uiso 1 1 calc R . .
C18 C 0.4194(7) 1.0258(5) 0.3386(4) 0.0280(14) Uani 1 1 d . . .
C19 C 0.5643(8) 1.0233(6) 0.3386(5) 0.0350(16) Uani 1 1 d . . .
H19 H 0.6257 0.9788 0.3753 0.042 Uiso 1 1 calc R . .
C20 C 0.6143(8) 1.0879(6) 0.2834(5) 0.0360(16) Uani 1 1 d . . .
H20 H 0.7117 1.0844 0.2815 0.043 Uiso 1 1 calc R . .
C21 C 0.5225(8) 1.1589(5) 0.2301(4) 0.0295(14) Uani 1 1 d . . .
C22 C 0.3731(8) 1.1659(6) 0.2346(5) 0.0329(15) Uani 1 1 d . . .
C23 C 0.3263(8) 1.0963(6) 0.2885(4) 0.0316(15) Uani 1 1 d . . .
H23 H 0.2298 1.0978 0.2904 0.038 Uiso 1 1 calc R . .
C24 C 0.5825(8) 1.2290(6) 0.1736(5) 0.0372(17) Uani 1 1 d . . .
C25 C 0.6548(10) 0.1387(7) -0.0353(5) 0.0431(19) Uani 1 1 d . . .
H25 H 0.5594 0.1790 -0.0140 0.052 Uiso 1 1 calc R . .
C26 C 0.6789(13) 0.0408(8) -0.0741(7) 0.065(3) Uani 1 1 d . . .
H26 H 0.6029 0.0138 -0.0764 0.078 Uiso 1 1 calc R . .
C27 C 0.8186(13) -0.0137(8) -0.1087(7) 0.068(3) Uani 1 1 d . . .
H27 H 0.8380 -0.0786 -0.1364 0.082 Uiso 1 1 calc R . .
C28 C 0.8996(8) 0.1221(6) -0.0633(5) 0.0408(18) Uani 1 1 d . . .
C29 C 0.9306(11) 0.0246(7) -0.1037(6) 0.056(2) Uani 1 1 d . . .
H29 H 1.0259 -0.0138 -0.1269 0.068 Uiso 1 1 calc R . .
C30 C 1.0147(9) 0.1714(7) -0.0578(5) 0.0398(18) Uani 1 1 d . . .
C31 C 1.1535(9) 0.1325(9) -0.1075(6) 0.058(3) Uani 1 1 d . . .
H31 H 1.1770 0.0743 -0.1450 0.070 Uiso 1 1 calc R . .
C32 C 1.2532(10) 0.1831(10) -0.0990(7) 0.065(3) Uani 1 1 d . . .
H32 H 1.3458 0.1582 -0.1305 0.078 Uiso 1 1 calc R . .
C33 C 1.2179(10) 0.2682(10) -0.0455(7) 0.068(3) Uani 1 1 d . . .
H33 H 1.2843 0.3033 -0.0401 0.081 Uiso 1 1 calc R . .
C34 C 1.0786(9) 0.3023(9) 0.0017(6) 0.057(2) Uani 1 1 d . . .
H34 H 1.0537 0.3604 0.0395 0.068 Uiso 1 1 calc R . .
N1 N -0.0126(8) 0.8284(6) 0.3085(5) 0.058(2) Uani 1 1 d . . .
H1A H 0.0289 0.8735 0.3191 0.069 Uiso 1 1 d R . .
H1B H -0.1033 0.8402 0.3274 0.069 Uiso 1 1 d R . .
N2 N 0.6443(8) 0.4913(5) 0.4200(5) 0.0441(17) Uani 1 1 d . . .
N3 N 0.7225(7) 0.6480(5) 0.4822(4) 0.0364(14) Uani 1 1 d . . .
N4 N 0.2732(7) 1.2356(6) 0.1869(5) 0.054(2) Uani 1 1 d . . .
H4A H 0.1843 1.2357 0.1905 0.064 Uiso 1 1 d R . .
H4B H 0.2999 1.2790 0.1534 0.064 Uiso 1 1 d R . .
N5 N 0.9800(7) 0.2550(6) -0.0052(4) 0.0438(16) Uani 1 1 d . . .
N6 N 0.7625(7) 0.1773(5) -0.0272(4) 0.0385(14) Uani 1 1 d . . .
O1 O -0.2366(6) 0.7525(4) 0.3074(4) 0.0388(12) Uani 1 1 d . . .
O2 O -0.1818(5) 0.5829(4) 0.2785(3) 0.0346(11) Uani 1 1 d . . .
O3 O 0.5661(6) 0.5182(5) 0.1953(4) 0.0512(16) Uani 1 1 d . . .
O4 O 0.5141(6) 0.7056(4) 0.1786(3) 0.0401(13) Uani 1 1 d . . .
O5 O 0.5085(6) 0.5959(5) 0.0569(3) 0.0435(13) Uani 1 1 d . . .
O6 O 0.4710(6) 0.8664(4) 0.4392(4) 0.0442(13) Uani 1 1 d . . .
O7 O 0.2467(6) 1.0128(4) 0.4768(4) 0.0530(16) Uani 1 1 d . . .
O8 O 0.2686(8) 0.8990(5) 0.3539(4) 0.0606(18) Uani 1 1 d . . .
O9 O 0.7179(6) 1.2187(5) 0.1698(3) 0.0438(13) Uani 1 1 d . . .
O10 O 0.5015(6) 1.2957(5) 0.1264(4) 0.0445(14) Uani 1 1 d . . .
O1W O 0.9490(7) 0.1982(5) 0.2657(4) 0.0587(17) Uani 1 1 d . . .
H1WA H 0.8963 0.1833 0.2310 0.088 Uiso 1 1 d R . .
H1WB H 0.9611 0.1555 0.3075 0.088 Uiso 1 1 d R . .
O2W O 0.9487(7) 0.0503(6) 0.3968(4) 0.0667(19) Uani 1 1 d . . .
H2WB H 1.0121 0.0357 0.4326 0.100 Uiso 1 1 d R . .
H2WA H 0.8659 0.0521 0.4221 0.100 Uiso 1 1 d R . .
O3W O 0.8853(6) 0.3889(5) 0.1776(4) 0.0509(15) Uani 1 1 d . . .
H3WB H 0.8479 0.4517 0.1978 0.076 Uiso 1 1 d R . .
H3WA H 0.8962 0.3461 0.2193 0.076 Uiso 1 1 d R . .
Pb1 Pb 0.57463(3) 0.67657(2) 0.353808(17) 0.03014(9) Uani 1 1 d . . .
Pb2 Pb 0.70451(3) 0.35291(2) 0.057265(17) 0.03246(10) Uani 1 1 d . . .
S1 S 0.48658(18) 0.61176(16) 0.15115(12) 0.0331(4) Uani 1 1 d . . .
S2 S 0.3464(2) 0.94452(14) 0.40777(13) 0.0323(4) Uani 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
C1 O2 1.266(8) . ?
C1 O1 1.280(9) . ?
C1 C2 1.491(9) . ?
C1 Pb1 2.806(7) 1_455 ?
C2 C7 1.394(10) . ?
C2 C3 1.413(9) . ?
C3 N1 1.374(9) . ?
C3 C4 1.402(9) . ?
C4 C5 1.369(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.409(10) . ?
C5 S1 1.779(7) . ?
C6 C7 1.381(10) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 N3 1.342(10) . ?
C8 C9 1.388(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.382(16) . ?
C9 H9 0.9300 . ?
C10 C11 1.362(16) . ?
C10 H10 0.9300 . ?
C11 C12 1.382(13) . ?
C11 H11 0.9300 . ?
C12 N3 1.352(9) . ?
C12 C13 1.491(12) . ?
C13 N2 1.344(11) . ?
C13 C14 1.406(11) . ?
C14 C15 1.416(16) . ?
C14 H14 0.9300 . ?
C15 C16 1.339(16) . ?
C15 H15 0.9300 . ?
C16 C17 1.369(14) . ?
C16 H16 0.9300 . ?
C17 N2 1.339(11) . ?
C17 H17 0.9300 . ?
C18 C23 1.372(10) . ?
C18 C19 1.398(9) . ?
C18 S2 1.780(6) . ?
C19 C20 1.375(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.402(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.418(10) . ?
C21 C24 1.493(9) . ?
C22 N4 1.379(9) . ?
C22 C23 1.400(9) . ?
C23 H23 0.9300 . ?
C24 O10 1.263(9) . ?
C24 O9 1.272(9) . ?
C24 Pb2 2.863(7) 1_565 ?
C25 N6 1.333(9) . ?
C25 C26 1.391(13) . ?
C25 H25 0.9300 . ?
C26 C27 1.361(15) . ?
C26 H26 0.9300 . ?
C27 C29 1.362(14) . ?
C27 H27 0.9300 . ?
C28 N6 1.350(10) . ?
C28 C29 1.385(12) . ?
C28 C30 1.491(11) . ?
C29 H29 0.9300 . ?
C30 N5 1.322(11) . ?
C30 C31 1.412(11) . ?
C31 C32 1.376(14) . ?
C31 H31 0.9300 . ?
C32 C33 1.346(16) . ?
C32 H32 0.9300 . ?
C33 C34 1.397(13) . ?
C33 H33 0.9300 . ?
C34 N5 1.331(10) . ?
C34 H34 0.9300 . ?
N1 H1A 0.8601 . ?
N1 H1B 0.8600 . ?
N2 Pb1 2.587(6) . ?
N3 Pb1 2.529(6) . ?
N4 H4A 0.8601 . ?
N4 H4B 0.8599 . ?
N5 Pb2 2.635(7) . ?
N6 Pb2 2.576(6) . ?
O1 Pb1 2.424(5) 1_455 ?
O2 Pb1 2.446(5) 1_455 ?
O3 S1 1.448(6) . ?
O3 Pb2 2.965(7) . ?
O4 S1 1.454(5) . ?
O4 Pb1 2.828(5) . ?
O5 S1 1.456(5) . ?
O5 Pb2 2.776(5) 2_665 ?
O6 S2 1.441(6) . ?
O6 Pb1 2.713(6) . ?
O7 S2 1.456(6) . ?
O8 S2 1.451(6) . ?
O9 Pb2 2.475(5) 1_565 ?
O10 Pb2 2.482(5) 1_565 ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8508 . ?
O2W H2WB 0.8480 . ?
O2W H2WA 0.8477 . ?
O3W Pb2 2.846(6) . ?
O3W H3WB 0.8497 . ?
O3W H3WA 0.8510 . ?
Pb1 O1 2.424(5) 1_655 ?
Pb1 O2 2.446(5) 1_655 ?
Pb1 C1 2.806(7) 1_655 ?
Pb2 O9 2.475(5) 1_545 ?
Pb2 O10 2.482(5) 1_545 ?
Pb2 O5 2.776(5) 2_665 ?
Pb2 C24 2.863(7) 1_545 ?

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
O2 C1 O1 120.0(6) . . ?
O2 C1 C2 120.8(6) . . ?
O1 C1 C2 119.2(6) . . ?
O2 C1 Pb1 60.5(3) . 1_455 ?
O1 C1 Pb1 59.6(3) . 1_455 ?
C2 C1 Pb1 177.2(5) . 1_455 ?
C7 C2 C3 119.6(6) . . ?
C7 C2 C1 118.1(6) . . ?
C3 C2 C1 122.0(6) . . ?
N1 C3 C4 118.3(7) . . ?
N1 C3 C2 123.5(6) . . ?
C4 C3 C2 118.1(6) . . ?
C5 C4 C3 121.0(6) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 121.6(6) . . ?
C4 C5 S1 119.8(5) . . ?
C6 C5 S1 118.6(6) . . ?
C7 C6 C5 117.4(7) . . ?
C7 C6 H6 121.3 . . ?
C5 C6 H6 121.3 . . ?
C6 C7 C2 122.2(7) . . ?
C6 C7 H7 118.9 . . ?
C2 C7 H7 118.9 . . ?
N3 C8 C9 124.1(9) . . ?
N3 C8 H8 118.0 . . ?
C9 C8 H8 118.0 . . ?
C10 C9 C8 116.1(10) . . ?
C10 C9 H9 121.9 . . ?
C8 C9 H9 121.9 . . ?
C11 C10 C9 120.9(9) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 119.8(9) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
N3 C12 C11 120.7(8) . . ?
N3 C12 C13 115.3(7) . . ?
C11 C12 C13 123.9(8) . . ?
N2 C13 C14 122.7(9) . . ?
N2 C13 C12 117.5(6) . . ?
C14 C13 C12 119.8(9) . . ?
C13 C14 C15 117.0(11) . . ?
C13 C14 H14 121.5 . . ?
C15 C14 H14 121.5 . . ?
C16 C15 C14 120.2(8) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C17 118.4(10) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
N2 C17 C16 125.1(11) . . ?
N2 C17 H17 117.4 . . ?
C16 C17 H17 117.4 . . ?
C23 C18 C19 120.4(6) . . ?
C23 C18 S2 117.8(5) . . ?
C19 C18 S2 121.7(5) . . ?
C20 C19 C18 118.8(7) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
C19 C20 C21 121.9(6) . . ?
C19 C20 H20 119.1 . . ?
C21 C20 H20 119.1 . . ?
C20 C21 C22 118.9(6) . . ?
C20 C21 C24 119.2(6) . . ?
C22 C21 C24 121.8(6) . . ?
N4 C22 C23 118.6(6) . . ?
N4 C22 C21 123.2(6) . . ?
C23 C22 C21 118.1(7) . . ?
C18 C23 C22 121.7(6) . . ?
C18 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
O10 C24 O9 119.4(6) . . ?
O10 C24 C21 120.6(6) . . ?
O9 C24 C21 119.9(7) . . ?
O10 C24 Pb2 59.9(4) . 1_565 ?
O9 C24 Pb2 59.6(4) . 1_565 ?
C21 C24 Pb2 176.4(5) . 1_565 ?
N6 C25 C26 123.0(9) . . ?
N6 C25 H25 118.5 . . ?
C26 C25 H25 118.5 . . ?
C27 C26 C25 117.0(10) . . ?
C27 C26 H26 121.5 . . ?
C25 C26 H26 121.5 . . ?
C26 C27 C29 121.6(10) . . ?
C26 C27 H27 119.2 . . ?
C29 C27 H27 119.2 . . ?
N6 C28 C29 121.3(8) . . ?
N6 C28 C30 116.8(7) . . ?
C29 C28 C30 121.9(8) . . ?
C27 C29 C28 118.5(9) . . ?
C27 C29 H29 120.8 . . ?
C28 C29 H29 120.8 . . ?
N5 C30 C31 121.3(8) . . ?
N5 C30 C28 116.8(7) . . ?
C31 C30 C28 121.9(8) . . ?
C32 C31 C30 118.2(10) . . ?
C32 C31 H31 120.9 . . ?
C30 C31 H31 120.9 . . ?
C33 C32 C31 120.6(9) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C32 C33 C34 118.1(10) . . ?
C32 C33 H33 121.0 . . ?
C34 C33 H33 121.0 . . ?
N5 C34 C33 122.6(10) . . ?
N5 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?
C3 N1 H1A 120.0 . . ?
C3 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C17 N2 C13 116.5(8) . . ?
C17 N2 Pb1 123.1(7) . . ?
C13 N2 Pb1 120.3(5) . . ?
C8 N3 C12 118.3(7) . . ?
C8 N3 Pb1 118.0(5) . . ?
C12 N3 Pb1 123.2(5) . . ?
C22 N4 H4A 120.0 . . ?
C22 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C30 N5 C34 119.2(7) . . ?
C30 N5 Pb2 120.5(5) . . ?
C34 N5 Pb2 118.9(6) . . ?
C25 N6 C28 118.5(7) . . ?
C25 N6 Pb2 119.4(5) . . ?
C28 N6 Pb2 122.0(5) . . ?
C1 O1 Pb1 93.4(4) . 1_455 ?
C1 O2 Pb1 92.7(4) . 1_455 ?
S1 O3 Pb2 106.0(3) . . ?
S1 O4 Pb1 106.6(3) . . ?
S1 O5 Pb2 127.5(3) . 2_665 ?
S2 O6 Pb1 116.7(3) . . ?
C24 O9 Pb2 94.1(4) . 1_565 ?
C24 O10 Pb2 94.0(4) . 1_565 ?
H1WA O1W H1WB 109.6 . . ?
H2WB O2W H2WA 110.3 . . ?
Pb2 O3W H3WB 109.2 . . ?
Pb2 O3W H3WA 112.4 . . ?
H3WB O3W H3WA 109.5 . . ?
O1 Pb1 O2 53.83(17) 1_655 1_655 ?
O1 Pb1 N3 76.79(19) 1_655 . ?
O2 Pb1 N3 80.82(19) 1_655 . ?
O1 Pb1 N2 120.2(2) 1_655 . ?
O2 Pb1 N2 76.24(19) 1_655 . ?
N3 Pb1 N2 63.5(2) . . ?
O1 Pb1 O6 77.84(17) 1_655 . ?
O2 Pb1 O6 130.16(16) 1_655 . ?
N3 Pb1 O6 76.63(19) . . ?
N2 Pb1 O6 127.97(19) . . ?
O1 Pb1 C1 27.08(19) 1_655 1_655 ?
O2 Pb1 C1 26.78(18) 1_655 1_655 ?
N3 Pb1 C1 76.5(2) . 1_655 ?
N2 Pb1 C1 97.9(2) . 1_655 ?
O6 Pb1 C1 104.02(18) . 1_655 ?
O1 Pb1 O4 83.68(17) 1_655 . ?
O2 Pb1 O4 79.87(17) 1_655 . ?
N3 Pb1 O4 158.21(17) . . ?
N2 Pb1 O4 120.8(2) . . ?
O6 Pb1 O4 108.82(16) . . ?
C1 Pb1 O4 81.71(17) 1_655 . ?
O9 Pb2 O10 52.42(18) 1_545 1_545 ?
O9 Pb2 N6 74.5(2) 1_545 . ?
O10 Pb2 N6 80.4(2) 1_545 . ?
O9 Pb2 N5 91.1(2) 1_545 . ?
O10 Pb2 N5 134.7(2) 1_545 . ?
N6 Pb2 N5 62.6(2) . . ?
O9 Pb2 O5 122.30(17) 1_545 2_665 ?
O10 Pb2 O5 73.79(17) 1_545 2_665 ?
N6 Pb2 O5 77.89(19) . 2_665 ?
N5 Pb2 O5 118.70(18) . 2_665 ?
O9 Pb2 O3W 74.54(18) 1_545 . ?
O10 Pb2 O3W 113.74(18) 1_545 . ?
N6 Pb2 O3W 123.80(19) . . ?
N5 Pb2 O3W 72.40(19) . . ?
O5 Pb2 O3W 157.24(18) 2_665 . ?
O9 Pb2 C24 26.30(19) 1_545 1_545 ?
O10 Pb2 C24 26.12(19) 1_545 1_545 ?
N6 Pb2 C24 75.7(2) . 1_545 ?
N5 Pb2 C24 113.7(2) . 1_545 ?
O5 Pb2 C24 98.00(19) 2_665 1_545 ?
O3W Pb2 C24 94.6(2) . 1_545 ?
O9 Pb2 O3 88.53(18) 1_545 . ?
O10 Pb2 O3 78.41(18) 1_545 . ?
N6 Pb2 O3 158.23(17) . . ?
N5 Pb2 O3 132.67(19) . . ?
O5 Pb2 O3 100.82(16) 2_665 . ?
O3W Pb2 O3 61.96(16) . . ?
C24 Pb2 O3 82.99(19) 1_545 . ?
O3 S1 O4 113.0(4) . . ?
O3 S1 O5 112.1(4) . . ?
O4 S1 O5 112.7(3) . . ?
O3 S1 C5 104.8(3) . . ?
O4 S1 C5 106.6(3) . . ?
O5 S1 C5 107.0(3) . . ?
O6 S2 O8 112.6(4) . . ?
O6 S2 O7 113.2(4) . . ?
O8 S2 O7 111.4(4) . . ?
O6 S2 C18 105.9(3) . . ?
O8 S2 C18 106.2(3) . . ?
O7 S2 C18 107.0(3) . . ?

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
O2 C1 C2 C7 12.7(10) . . . . ?
O1 C1 C2 C7 -166.5(7) . . . . ?
O2 C1 C2 C3 -161.8(7) . . . . ?
O1 C1 C2 C3 19.0(10) . . . . ?
C7 C2 C3 N1 -179.9(7) . . . . ?
C1 C2 C3 N1 -5.6(11) . . . . ?
C7 C2 C3 C4 -0.5(10) . . . . ?
C1 C2 C3 C4 173.8(6) . . . . ?
N1 C3 C4 C5 179.3(7) . . . . ?
C2 C3 C4 C5 -0.1(11) . . . . ?
C3 C4 C5 C6 0.0(11) . . . . ?
C3 C4 C5 S1 -178.1(5) . . . . ?
C4 C5 C6 C7 0.8(11) . . . . ?
S1 C5 C6 C7 178.9(6) . . . . ?
C5 C6 C7 C2 -1.5(11) . . . . ?
C3 C2 C7 C6 1.3(11) . . . . ?
C1 C2 C7 C6 -173.2(7) . . . . ?
N3 C8 C9 C10 -1.8(14) . . . . ?
C8 C9 C10 C11 2.0(16) . . . . ?
C9 C10 C11 C12 0.3(17) . . . . ?
C10 C11 C12 N3 -2.9(15) . . . . ?
C10 C11 C12 C13 176.7(9) . . . . ?
N3 C12 C13 N2 2.4(10) . . . . ?
C11 C12 C13 N2 -177.2(8) . . . . ?
N3 C12 C13 C14 -177.1(7) . . . . ?
C11 C12 C13 C14 3.2(12) . . . . ?
N2 C13 C14 C15 1.3(12) . . . . ?
C12 C13 C14 C15 -179.2(8) . . . . ?
C13 C14 C15 C16 -0.8(13) . . . . ?
C14 C15 C16 C17 0.9(14) . . . . ?
C15 C16 C17 N2 -1.7(15) . . . . ?
C23 C18 C19 C20 -4.1(11) . . . . ?
S2 C18 C19 C20 179.8(6) . . . . ?
C18 C19 C20 C21 2.7(12) . . . . ?
C19 C20 C21 C22 1.4(11) . . . . ?
C19 C20 C21 C24 178.2(7) . . . . ?
C20 C21 C22 N4 177.9(8) . . . . ?
C24 C21 C22 N4 1.1(12) . . . . ?
C20 C21 C22 C23 -4.0(10) . . . . ?
C24 C21 C22 C23 179.2(7) . . . . ?
C19 C18 C23 C22 1.5(11) . . . . ?
S2 C18 C23 C22 177.7(6) . . . . ?
N4 C22 C23 C18 -179.2(7) . . . . ?
C21 C22 C23 C18 2.6(11) . . . . ?
C20 C21 C24 O10 -178.2(7) . . . . ?
C22 C21 C24 O10 -1.4(11) . . . . ?
C20 C21 C24 O9 4.8(11) . . . . ?
C22 C21 C24 O9 -178.4(7) . . . . ?
N6 C25 C26 C27 -3.4(14) . . . . ?
C25 C26 C27 C29 1.5(16) . . . . ?
C26 C27 C29 C28 -0.8(16) . . . . ?
N6 C28 C29 C27 1.9(13) . . . . ?
C30 C28 C29 C27 -177.8(8) . . . . ?
N6 C28 C30 N5 11.8(11) . . . . ?
C29 C28 C30 N5 -168.5(8) . . . . ?
N6 C28 C30 C31 -167.0(8) . . . . ?
C29 C28 C30 C31 12.7(12) . . . . ?
N5 C30 C31 C32 0.9(13) . . . . ?
C28 C30 C31 C32 179.5(8) . . . . ?
C30 C31 C32 C33 -0.9(14) . . . . ?
C31 C32 C33 C34 0.9(15) . . . . ?
C32 C33 C34 N5 -0.9(15) . . . . ?
C16 C17 N2 C13 2.2(13) . . . . ?
C16 C17 N2 Pb1 -180.0(7) . . . . ?
C14 C13 N2 C17 -2.0(11) . . . . ?
C12 C13 N2 C17 178.5(7) . . . . ?
C14 C13 N2 Pb1 -179.9(6) . . . . ?
C12 C13 N2 Pb1 0.6(9) . . . . ?
C9 C8 N3 C12 -0.7(12) . . . . ?
C9 C8 N3 Pb1 -173.2(7) . . . . ?
C11 C12 N3 C8 3.1(11) . . . . ?
C13 C12 N3 C8 -176.5(7) . . . . ?
C11 C12 N3 Pb1 175.2(7) . . . . ?
C13 C12 N3 Pb1 -4.5(9) . . . . ?
C31 C30 N5 C34 -0.9(12) . . . . ?
C28 C30 N5 C34 -179.6(7) . . . . ?
C31 C30 N5 Pb2 165.3(6) . . . . ?
C28 C30 N5 Pb2 -13.5(9) . . . . ?
C33 C34 N5 C30 0.9(14) . . . . ?
C33 C34 N5 Pb2 -165.4(7) . . . . ?
C26 C25 N6 C28 4.4(12) . . . . ?
C26 C25 N6 Pb2 -175.1(7) . . . . ?
C29 C28 N6 C25 -3.6(12) . . . . ?
C30 C28 N6 C25 176.1(7) . . . . ?
C29 C28 N6 Pb2 175.8(6) . . . . ?
C30 C28 N6 Pb2 -4.4(9) . . . . ?
O2 C1 O1 Pb1 3.8(7) . . . 1_455 ?
C2 C1 O1 Pb1 -177.0(5) . . . 1_455 ?
O1 C1 O2 Pb1 -3.7(7) . . . 1_455 ?
C2 C1 O2 Pb1 177.1(6) . . . 1_455 ?
O10 C24 O9 Pb2 -1.1(8) . . . 1_565 ?
C21 C24 O9 Pb2 175.9(6) . . . 1_565 ?
O9 C24 O10 Pb2 1.1(8) . . . 1_565 ?
C21 C24 O10 Pb2 -175.9(6) . . . 1_565 ?
C8 N3 Pb1 O1 41.6(6) . . . 1_655 ?
C12 N3 Pb1 O1 -130.5(6) . . . 1_655 ?
C8 N3 Pb1 O2 96.4(6) . . . 1_655 ?
C12 N3 Pb1 O2 -75.7(6) . . . 1_655 ?
C8 N3 Pb1 N2 175.5(6) . . . . ?
C12 N3 Pb1 N2 3.4(5) . . . . ?
C8 N3 Pb1 O6 -38.8(5) . . . . ?
C12 N3 Pb1 O6 149.1(6) . . . . ?
C8 N3 Pb1 C1 69.4(6) . . . 1_655 ?
C12 N3 Pb1 C1 -102.7(6) . . . 1_655 ?
C8 N3 Pb1 O4 68.5(8) . . . . ?
C12 N3 Pb1 O4 -103.6(7) . . . . ?
C17 N2 Pb1 O1 -125.5(7) . . . 1_655 ?
C13 N2 Pb1 O1 52.3(6) . . . 1_655 ?
C17 N2 Pb1 O2 -93.2(7) . . . 1_655 ?
C13 N2 Pb1 O2 84.6(6) . . . 1_655 ?
C17 N2 Pb1 N3 -179.7(7) . . . . ?
C13 N2 Pb1 N3 -1.9(5) . . . . ?
C17 N2 Pb1 O6 136.2(6) . . . . ?
C13 N2 Pb1 O6 -46.0(6) . . . . ?
C17 N2 Pb1 C1 -109.1(7) . . . 1_655 ?
C13 N2 Pb1 C1 68.7(6) . . . 1_655 ?
C17 N2 Pb1 O4 -24.1(7) . . . . ?
C13 N2 Pb1 O4 153.7(5) . . . . ?
S2 O6 Pb1 O1 107.5(3) . . . 1_655 ?
S2 O6 Pb1 O2 121.2(3) . . . 1_655 ?
S2 O6 Pb1 N3 -173.4(3) . . . . ?
S2 O6 Pb1 N2 -133.6(3) . . . . ?
S2 O6 Pb1 C1 114.5(3) . . . 1_655 ?
S2 O6 Pb1 O4 28.6(3) . . . . ?
S1 O4 Pb1 O1 138.6(3) . . . 1_655 ?
S1 O4 Pb1 O2 84.2(3) . . . 1_655 ?
S1 O4 Pb1 N3 112.2(5) . . . . ?
S1 O4 Pb1 N2 17.1(4) . . . . ?
S1 O4 Pb1 O6 -146.6(3) . . . . ?
S1 O4 Pb1 C1 111.3(3) . . . 1_655 ?
C25 N6 Pb2 O9 78.5(6) . . . 1_545 ?
C28 N6 Pb2 O9 -100.9(6) . . . 1_545 ?
C25 N6 Pb2 O10 25.0(5) . . . 1_545 ?
C28 N6 Pb2 O10 -154.4(6) . . . 1_545 ?
C25 N6 Pb2 N5 178.1(6) . . . . ?
C28 N6 Pb2 N5 -1.4(6) . . . . ?
C25 N6 Pb2 O5 -50.3(5) . . . 2_665 ?
C28 N6 Pb2 O5 130.3(6) . . . 2_665 ?
C25 N6 Pb2 O3W 137.3(5) . . . . ?
C28 N6 Pb2 O3W -42.2(7) . . . . ?
C25 N6 Pb2 C24 51.3(6) . . . 1_545 ?
C28 N6 Pb2 C24 -128.1(6) . . . 1_545 ?
C25 N6 Pb2 O3 38.6(9) . . . . ?
C28 N6 Pb2 O3 -140.8(6) . . . . ?
C30 N5 Pb2 O9 80.0(6) . . . 1_545 ?
C34 N5 Pb2 O9 -113.9(6) . . . 1_545 ?
C30 N5 Pb2 O10 47.1(7) . . . 1_545 ?
C34 N5 Pb2 O10 -146.7(6) . . . 1_545 ?
C30 N5 Pb2 N6 8.1(5) . . . . ?
C34 N5 Pb2 N6 174.3(7) . . . . ?
C30 N5 Pb2 O5 -48.3(6) . . . 2_665 ?
C34 N5 Pb2 O5 117.8(6) . . . 2_665 ?
C30 N5 Pb2 O3W 153.4(6) . . . . ?
C34 N5 Pb2 O3W -40.5(6) . . . . ?
C30 N5 Pb2 C24 66.1(6) . . . 1_545 ?
C34 N5 Pb2 C24 -127.8(6) . . . 1_545 ?
C30 N5 Pb2 O3 169.0(5) . . . . ?
C34 N5 Pb2 O3 -24.9(7) . . . . ?
S1 O3 Pb2 O9 -157.7(3) . . . 1_545 ?
S1 O3 Pb2 O10 -105.8(3) . . . 1_545 ?
S1 O3 Pb2 N6 -119.4(5) . . . . ?
S1 O3 Pb2 N5 112.2(3) . . . . ?
S1 O3 Pb2 O5 -35.0(3) . . . 2_665 ?
S1 O3 Pb2 O3W 129.1(3) . . . . ?
S1 O3 Pb2 C24 -131.9(3) . . . 1_545 ?
Pb2 O3 S1 O4 -132.4(3) . . . . ?
Pb2 O3 S1 O5 -3.7(4) . . . . ?
Pb2 O3 S1 C5 112.0(3) . . . . ?
Pb1 O4 S1 O3 -29.9(4) . . . . ?
Pb1 O4 S1 O5 -158.2(3) . . . . ?
Pb1 O4 S1 C5 84.7(3) . . . . ?
Pb2 O5 S1 O3 132.0(4) 2_665 . . . ?
Pb2 O5 S1 O4 -99.2(4) 2_665 . . . ?
Pb2 O5 S1 C5 17.7(5) 2_665 . . . ?
C4 C5 S1 O3 117.1(6) . . . . ?
C6 C5 S1 O3 -61.1(7) . . . . ?
C4 C5 S1 O4 -2.9(7) . . . . ?
C6 C5 S1 O4 178.9(6) . . . . ?
C4 C5 S1 O5 -123.8(6) . . . . ?
C6 C5 S1 O5 58.1(7) . . . . ?
Pb1 O6 S2 O8 18.4(4) . . . . ?
Pb1 O6 S2 O7 145.8(3) . . . . ?
Pb1 O6 S2 C18 -97.3(3) . . . . ?
C23 C18 S2 O6 169.5(6) . . . . ?
C19 C18 S2 O6 -14.4(7) . . . . ?
C23 C18 S2 O8 49.5(7) . . . . ?
C19 C18 S2 O8 -134.3(6) . . . . ?
C23 C18 S2 O7 -69.5(6) . . . . ?
C19 C18 S2 O7 106.6(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         1.634
_refine_diff_density_min         -2.285
_refine_diff_density_rms         0.203
_database_code_depnum_ccdc_archive 'CCDC 834929'
#######################################################################
#
#                 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_6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H28 N6 O12 Pb2 S2'
_chemical_formula_weight         1119.06

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'
S S 0.1246 0.1234 '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           TRICLINIC
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.9314(7)
_cell_length_b                   11.0291(13)
_cell_length_c                   24.939(3)
_cell_angle_alpha                101.0520(10)
_cell_angle_beta                 92.705(2)
_cell_angle_gamma                93.508(2)
_cell_volume                     1595.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5028
_cell_measurement_theta_min      2.2061
_cell_measurement_theta_max      27.4362

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1060
_exptl_absorpt_coefficient_mu    10.745
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.1169
_exptl_absorpt_correction_T_max  0.2956
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean 8.3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14086
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         27.48
_reflns_number_total             7182
_reflns_number_gt                5774
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond (CRYSTAL IMPACT, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0335P)²+8.4058P] where P=(Fo²+2Fc²)/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         7182
_refine_ls_number_parameters     451
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.1085
_refine_ls_wR_factor_gt          0.0963
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.7160(13) 0.1780(7) 0.8239(3) 0.0272(17) Uani 1 1 d . . .
C2 C 0.9971(13) 0.3678(7) 0.8571(3) 0.0270(17) Uani 1 1 d . . .
C3 C 1.0507(13) 0.4933(7) 0.8573(3) 0.0292(17) Uani 1 1 d . . .
H3 H 1.1903 0.5304 0.8725 0.035 Uiso 1 1 calc R . .
C4 C 0.8982(12) 0.5623(7) 0.8354(3) 0.0213(15) Uani 1 1 d . . .
C5 C 0.6846(14) 0.5120(7) 0.8126(3) 0.0298(18) Uani 1 1 d . . .
H5 H 0.5801 0.5605 0.7995 0.036 Uiso 1 1 calc R . .
C6 C 0.6362(14) 0.3869(7) 0.8103(3) 0.0298(18) Uani 1 1 d . . .
H6 H 0.4980 0.3505 0.7939 0.036 Uiso 1 1 calc R . .
C7 C 0.7858(13) 0.3128(7) 0.8316(3) 0.0248(16) Uani 1 1 d . . .
C8 C 0.6883(15) 0.4388(9) 0.9833(4) 0.040(2) Uani 1 1 d . . .
H8 H 0.8143 0.3973 0.9715 0.048 Uiso 1 1 calc R . .
C9 C 0.3510(16) 0.4496(9) 1.0319(4) 0.041(2) Uani 1 1 d . . .
H9 H 0.2491 0.4153 1.0530 0.049 Uiso 1 1 calc R . .
C10 C 0.5408(15) 0.3890(8) 1.0158(3) 0.0329(18) Uani 1 1 d . . .
C11 C 0.5743(17) 0.2631(8) 1.0307(4) 0.041(2) Uani 1 1 d . . .
H11A H 0.7349 0.2540 1.0364 0.050 Uiso 1 1 calc R . .
H11B H 0.5043 0.2590 1.0648 0.050 Uiso 1 1 calc R . .
C12 C 0.5733(14) 0.1115(8) 0.9421(4) 0.0343(19) Uani 1 1 d . . .
H12 H 0.7211 0.1328 0.9346 0.041 Uiso 1 1 calc R . .
C13 C 0.2601(13) 0.1064(7) 0.9842(3) 0.0304(18) Uani 1 1 d . . .
H13 H 0.1522 0.1223 1.0100 0.037 Uiso 1 1 calc R . .
C14 C 0.2336(16) 0.0247(8) 0.9358(4) 0.038(2) Uani 1 1 d . . .
H14 H 0.1032 -0.0255 0.9227 0.046 Uiso 1 1 calc R . .
C15 C 0.6143(14) 0.7047(8) 0.6578(3) 0.0303(18) Uani 1 1 d . . .
C16 C 0.7499(14) 0.6136(8) 0.6350(4) 0.037(2) Uani 1 1 d . . .
H16 H 0.8777 0.6330 0.6173 0.044 Uiso 1 1 calc R . .
C17 C 0.6906(15) 0.4911(9) 0.6394(4) 0.039(2) Uani 1 1 d . . .
H17 H 0.7793 0.4283 0.6241 0.047 Uiso 1 1 calc R . .
C18 C 0.4983(15) 0.4624(7) 0.6665(4) 0.0326(18) Uani 1 1 d . . .
C19 C 0.3568(13) 0.5565(8) 0.6881(4) 0.0313(18) Uani 1 1 d . . .
C20 C 0.4206(14) 0.6774(8) 0.6823(3) 0.0323(18) Uani 1 1 d . . .
H20 H 0.3293 0.7409 0.6954 0.039 Uiso 1 1 calc R . .
C21 C 0.1960(16) 0.5509(9) 0.5301(4) 0.040(2) Uani 1 1 d . . .
H21 H 0.3296 0.5840 0.5500 0.048 Uiso 1 1 calc R . .
C22 C 0.1273(17) 0.4281(9) 0.5272(4) 0.045(2) Uani 1 1 d . . .
H22 H 0.2129 0.3805 0.5462 0.054 Uiso 1 1 calc R . .
C23 C -0.0673(15) 0.3736(8) 0.4964(3) 0.0341(19) Uani 1 1 d . . .
C24 C -0.1495(17) 0.2395(8) 0.4911(4) 0.042(2) Uani 1 1 d . . .
H24A H -0.2993 0.2348 0.5050 0.051 Uiso 1 1 calc R . .
H24B H -0.1614 0.1999 0.4527 0.051 Uiso 1 1 calc R . .
C25 C 0.2026(14) 0.1246(8) 0.5038(4) 0.0336(19) Uani 1 1 d . . .
H25 H 0.2601 0.1217 0.4695 0.040 Uiso 1 1 calc R . .
C26 C -0.0181(14) 0.1561(8) 0.5723(4) 0.0330(18) Uani 1 1 d . . .
H26 H -0.1396 0.1790 0.5933 0.040 Uiso 1 1 calc R . .
C27 C 0.2970(17) 0.0832(9) 0.5458(3) 0.040(2) Uani 1 1 d . . .
H27 H 0.4347 0.0472 0.5460 0.048 Uiso 1 1 calc R . .
C28 C 0.4527(14) 0.3318(7) 0.6725(3) 0.0297(18) Uani 1 1 d . . .
N1 N 0.4761(11) 0.1612(6) 0.9879(3) 0.0315(15) Uani 1 1 d . . .
N2 N 0.4344(11) 0.0282(6) 0.9086(3) 0.0298(15) Uani 1 1 d . . .
N3 N 1.1456(13) 0.3042(7) 0.8828(3) 0.044(2) Uani 1 1 d . . .
H3A H 1.2696 0.3414 0.8987 0.053 Uiso 1 1 calc R . .
H3B H 1.1150 0.2271 0.8830 0.053 Uiso 1 1 calc R . .
N4 N 0.0019(12) 0.1729(6) 0.5211(3) 0.0318(15) Uani 1 1 d . . .
N5 N 0.1579(13) 0.1024(7) 0.5891(3) 0.0357(17) Uani 1 1 d . . .
N6 N 0.1745(13) 0.5360(8) 0.7166(4) 0.049(2) Uani 1 1 d . . .
H6A H 0.0989 0.5969 0.7309 0.059 Uiso 1 1 calc R . .
H6B H 0.1341 0.4620 0.7204 0.059 Uiso 1 1 calc R . .
O1 O 0.8362(11) 0.7919(6) 0.8791(3) 0.0411(15) Uani 1 1 d . . .
O2 O 1.2133(9) 0.7448(5) 0.8491(2) 0.0317(13) Uani 1 1 d . . .
O3 O 0.8971(9) 0.7448(5) 0.7833(2) 0.0322(13) Uani 1 1 d . . .
O4 O 0.8507(10) 0.1041(5) 0.8409(3) 0.0355(14) Uani 1 1 d . . .
O5 O 0.5220(10) 0.1378(5) 0.8031(3) 0.0372(14) Uani 1 1 d . . .
O6 O 0.5917(11) 0.2515(6) 0.6571(3) 0.0435(16) Uani 1 1 d . . .
O7 O 0.2710(11) 0.3016(6) 0.6928(3) 0.0400(15) Uani 1 1 d . . .
O8 O 0.5421(11) 0.8977(6) 0.6154(3) 0.0435(16) Uani 1 1 d . . .
O9 O 0.6612(10) 0.9325(5) 0.7113(2) 0.0367(14) Uani 1 1 d . . .
O10 O 0.9281(10) 0.8701(6) 0.6428(3) 0.0439(16) Uani 1 1 d . . .
O1W O 0.1453(9) -0.0379(5) 0.7770(2) 0.0333(13) Uani 1 1 d D . .
H1WA H 0.0820 0.0211 0.7965 0.040 Uiso 1 1 d RD . .
H1WB H 0.0540 -0.1024 0.7705 0.040 Uiso 1 1 d RD . .
O2W O -0.0874(10) 0.1483(6) 0.7136(3) 0.0420(15) Uani 1 1 d D . .
H2WA H -0.1819 0.1925 0.7010 0.050 Uiso 1 1 d RD . .
H2WB H -0.1155 0.0728 0.6983 0.050 Uiso 1 1 d RD . .
Pb1 Pb 0.27223(5) 0.08053(3) 0.681053(13) 0.03061(10) Uani 1 1 d . . .
Pb2 Pb 0.52787(5) -0.07767(3) 0.816879(11) 0.02319(9) Uani 1 1 d . . .
S1 S 0.6941(3) 0.86158(19) 0.65565(8) 0.0286(4) Uani 1 1 d . . .
S2 S 0.9701(3) 0.72317(17) 0.83740(8) 0.0245(4) Uani 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
C1 O5 1.258(10) . ?
C1 O4 1.289(10) . ?
C1 C7 1.493(10) . ?
C2 N3 1.368(10) . ?
C2 C3 1.400(10) . ?
C2 C7 1.424(11) . ?
C3 C4 1.376(11) . ?
C4 C5 1.401(10) . ?
C4 S2 1.790(7) . ?
C5 C6 1.382(10) . ?
C6 C7 1.395(11) . ?
C8 C10 1.380(12) . ?
C8 C9 1.384(13) 2_667 ?
C9 C10 1.381(13) . ?
C9 C8 1.384(13) 2_667 ?
C10 C11 1.528(12) . ?
C11 N1 1.464(11) . ?
C12 N2 1.330(11) . ?
C12 N1 1.340(11) . ?
C13 C14 1.358(12) . ?
C13 N1 1.374(10) . ?
C14 N2 1.400(11) . ?
C15 C20 1.371(11) . ?
C15 C16 1.379(12) . ?
C15 S1 1.777(8) . ?
C16 C17 1.400(12) . ?
C17 C18 1.404(12) . ?
C18 C19 1.416(12) . ?
C18 C28 1.487(11) . ?
C19 N6 1.352(11) . ?
C19 C20 1.400(11) . ?
C21 C22 1.377(13) . ?
C21 C23 1.398(12) 2_566 ?
C22 C23 1.392(12) . ?
C23 C21 1.398(12) 2_566 ?
C23 C24 1.508(12) . ?
C24 N4 1.461(11) . ?
C25 C27 1.335(13) . ?
C25 N4 1.387(11) . ?
C26 N5 1.321(11) . ?
C26 N4 1.334(11) . ?
C27 N5 1.381(11) . ?
C28 O6 1.265(10) . ?
C28 O7 1.265(10) . ?
N2 Pb2 2.466(7) . ?
N5 Pb1 2.422(7) . ?
O1 S2 1.462(6) . ?
O2 S2 1.454(5) . ?
O3 S2 1.464(6) . ?
O4 Pb2 2.647(6) . ?
O5 Pb2 2.468(6) . ?
O6 Pb1 2.758(6) . ?
O7 Pb1 2.400(6) . ?
O8 S1 1.445(6) . ?
O9 S1 1.486(6) . ?
O10 S1 1.440(6) . ?
O1W Pb2 2.531(5) . ?
O2W Pb1 2.428(6) . ?

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 C1 O4 120.3(7) . . ?
O5 C1 C7 119.8(7) . . ?
O4 C1 C7 119.9(7) . . ?
N3 C2 C3 119.0(7) . . ?
N3 C2 C7 122.7(7) . . ?
C3 C2 C7 118.3(7) . . ?
C4 C3 C2 120.5(7) . . ?
C3 C4 C5 122.3(7) . . ?
C3 C4 S2 119.3(6) . . ?
C5 C4 S2 118.3(6) . . ?
C6 C5 C4 117.0(7) . . ?
C5 C6 C7 122.8(7) . . ?
C6 C7 C2 119.0(7) . . ?
C6 C7 C1 117.0(7) . . ?
C2 C7 C1 123.9(7) . . ?
C10 C8 C9 120.1(8) . 2_667 ?
C10 C9 C8 120.4(8) . 2_667 ?
C8 C10 C9 119.5(8) . . ?
C8 C10 C11 121.0(9) . . ?
C9 C10 C11 119.3(8) . . ?
N1 C11 C10 111.7(7) . . ?
N2 C12 N1 112.3(7) . . ?
C14 C13 N1 107.2(7) . . ?
C13 C14 N2 108.9(8) . . ?
C20 C15 C16 121.7(8) . . ?
C20 C15 S1 119.2(7) . . ?
C16 C15 S1 119.1(6) . . ?
C15 C16 C17 118.4(8) . . ?
C16 C17 C18 120.6(8) . . ?
C17 C18 C19 120.3(8) . . ?
C17 C18 C28 117.8(8) . . ?
C19 C18 C28 121.9(8) . . ?
N6 C19 C20 119.4(8) . . ?
N6 C19 C18 123.3(8) . . ?
C20 C19 C18 117.2(7) . . ?
C15 C20 C19 121.7(8) . . ?
C22 C21 C23 120.8(8) . 2_566 ?
C21 C22 C23 121.6(8) . . ?
C22 C23 C21 117.6(8) . 2_566 ?
C22 C23 C24 124.0(8) . . ?
C21 C23 C24 118.4(8) 2_566 . ?
N4 C24 C23 112.0(7) . . ?
C27 C25 N4 106.6(8) . . ?
N5 C26 N4 110.9(7) . . ?
C25 C27 N5 109.2(9) . . ?
O6 C28 O7 120.4(8) . . ?
O6 C28 C18 120.7(8) . . ?
O7 C28 C18 118.9(7) . . ?
C12 N1 C13 106.8(7) . . ?
C12 N1 C11 126.2(8) . . ?
C13 N1 C11 126.7(7) . . ?
C12 N2 C14 104.8(7) . . ?
C12 N2 Pb2 124.2(6) . . ?
C14 N2 Pb2 130.9(5) . . ?
C26 N4 C25 107.1(7) . . ?
C26 N4 C24 126.0(8) . . ?
C25 N4 C24 126.7(8) . . ?
C26 N5 C27 106.2(7) . . ?
C26 N5 Pb1 128.8(6) . . ?
C27 N5 Pb1 123.7(6) . . ?
C1 O4 Pb2 89.7(5) . . ?
C1 O5 Pb2 98.9(5) . . ?
C28 O6 Pb1 86.3(5) . . ?
C28 O7 Pb1 103.3(5) . . ?
O7 Pb1 N5 79.2(2) . . ?
O7 Pb1 O2W 69.9(2) . . ?
N5 Pb1 O2W 90.8(2) . . ?
O7 Pb1 O6 49.8(2) . . ?
N5 Pb1 O6 75.8(2) . . ?
O2W Pb1 O6 119.5(2) . . ?
N2 Pb2 O5 79.4(2) . . ?
N2 Pb2 O1W 90.7(2) . . ?
O5 Pb2 O1W 69.01(18) . . ?
N2 Pb2 O4 77.8(2) . . ?
O5 Pb2 O4 51.02(18) . . ?
O1W Pb2 O4 119.99(18) . . ?
O10 S1 O8 113.4(4) . . ?
O10 S1 O9 111.3(4) . . ?
O8 S1 O9 110.8(4) . . ?
O10 S1 C15 108.3(4) . . ?
O8 S1 C15 107.1(4) . . ?
O9 S1 C15 105.4(4) . . ?
O2 S2 O1 114.0(4) . . ?
O2 S2 O3 112.9(3) . . ?
O1 S2 O3 109.9(4) . . ?
O2 S2 C4 107.4(3) . . ?
O1 S2 C4 106.6(3) . . ?
O3 S2 C4 105.4(3) . . ?

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
N3 C2 C3 C4 -175.4(8) . . . . ?
C7 C2 C3 C4 2.6(12) . . . . ?
C2 C3 C4 C5 0.7(12) . . . . ?
C2 C3 C4 S2 178.9(6) . . . . ?
C3 C4 C5 C6 -3.3(12) . . . . ?
S2 C4 C5 C6 178.4(6) . . . . ?
C4 C5 C6 C7 2.7(12) . . . . ?
C5 C6 C7 C2 0.5(13) . . . . ?
C5 C6 C7 C1 -177.1(8) . . . . ?
N3 C2 C7 C6 174.7(8) . . . . ?
C3 C2 C7 C6 -3.2(12) . . . . ?
N3 C2 C7 C1 -7.8(13) . . . . ?
C3 C2 C7 C1 174.3(7) . . . . ?
O5 C1 C7 C6 -5.6(11) . . . . ?
O4 C1 C7 C6 177.5(7) . . . . ?
O5 C1 C7 C2 176.9(8) . . . . ?
O4 C1 C7 C2 0.0(12) . . . . ?
C9 C8 C10 C9 1.7(15) 2_667 . . . ?
C9 C8 C10 C11 177.0(8) 2_667 . . . ?
C8 C9 C10 C8 -1.7(15) 2_667 . . . ?
C8 C9 C10 C11 -177.1(8) 2_667 . . . ?
C8 C10 C11 N1 -84.1(11) . . . . ?
C9 C10 C11 N1 91.2(10) . . . . ?
N1 C13 C14 N2 -0.1(10) . . . . ?
C20 C15 C16 C17 -2.5(14) . . . . ?
S1 C15 C16 C17 177.0(7) . . . . ?
C15 C16 C17 C18 -0.4(14) . . . . ?
C16 C17 C18 C19 2.5(14) . . . . ?
C16 C17 C18 C28 -176.4(8) . . . . ?
C17 C18 C19 N6 -177.3(9) . . . . ?
C28 C18 C19 N6 1.6(14) . . . . ?
C17 C18 C19 C20 -1.6(13) . . . . ?
C28 C18 C19 C20 177.3(8) . . . . ?
C16 C15 C20 C19 3.5(13) . . . . ?
S1 C15 C20 C19 -176.1(7) . . . . ?
N6 C19 C20 C15 174.6(8) . . . . ?
C18 C19 C20 C15 -1.3(12) . . . . ?
C23 C21 C22 C23 2.3(17) 2_566 . . . ?
C21 C22 C23 C21 -2.2(17) . . . 2_566 ?
C21 C22 C23 C24 179.3(10) . . . . ?
C22 C23 C24 N4 -1.4(14) . . . . ?
C21 C23 C24 N4 -179.8(8) 2_566 . . . ?
N4 C25 C27 N5 1.1(10) . . . . ?
C17 C18 C28 O6 5.0(12) . . . . ?
C19 C18 C28 O6 -173.9(8) . . . . ?
C17 C18 C28 O7 -174.3(8) . . . . ?
C19 C18 C28 O7 6.9(12) . . . . ?
N2 C12 N1 C13 0.3(10) . . . . ?
N2 C12 N1 C11 -174.1(8) . . . . ?
C14 C13 N1 C12 -0.1(9) . . . . ?
C14 C13 N1 C11 174.3(8) . . . . ?
C10 C11 N1 C12 82.3(11) . . . . ?
C10 C11 N1 C13 -91.0(10) . . . . ?
N1 C12 N2 C14 -0.4(10) . . . . ?
N1 C12 N2 Pb2 175.7(5) . . . . ?
C13 C14 N2 C12 0.3(9) . . . . ?
C13 C14 N2 Pb2 -175.4(6) . . . . ?
N5 C26 N4 C25 1.1(10) . . . . ?
N5 C26 N4 C24 -174.0(8) . . . . ?
C27 C25 N4 C26 -1.3(10) . . . . ?
C27 C25 N4 C24 173.7(8) . . . . ?
C23 C24 N4 C26 93.5(10) . . . . ?
C23 C24 N4 C25 -80.7(11) . . . . ?
N4 C26 N5 C27 -0.5(10) . . . . ?
N4 C26 N5 Pb1 166.7(5) . . . . ?
C25 C27 N5 C26 -0.4(10) . . . . ?
C25 C27 N5 Pb1 -168.4(6) . . . . ?
O5 C1 O4 Pb2 -3.8(8) . . . . ?
C7 C1 O4 Pb2 173.0(6) . . . . ?
O4 C1 O5 Pb2 4.1(8) . . . . ?
C7 C1 O5 Pb2 -172.7(6) . . . . ?
O7 C28 O6 Pb1 5.3(8) . . . . ?
C18 C28 O6 Pb1 -173.9(7) . . . . ?
O6 C28 O7 Pb1 -6.3(9) . . . . ?
C18 C28 O7 Pb1 173.0(6) . . . . ?
C28 O7 Pb1 N5 -77.3(5) . . . . ?
C28 O7 Pb1 O2W -172.2(6) . . . . ?
C28 O7 Pb1 O6 3.3(5) . . . . ?
C26 N5 Pb1 O7 -57.9(7) . . . . ?
C27 N5 Pb1 O7 107.2(7) . . . . ?
C26 N5 Pb1 O2W 11.4(8) . . . . ?
C27 N5 Pb1 O2W 176.5(7) . . . . ?
C26 N5 Pb1 O6 -108.9(8) . . . . ?
C27 N5 Pb1 O6 56.2(7) . . . . ?
C28 O6 Pb1 O7 -3.2(5) . . . . ?
C28 O6 Pb1 N5 84.5(5) . . . . ?
C28 O6 Pb1 O2W 1.8(6) . . . . ?
C12 N2 Pb2 O5 -65.6(7) . . . . ?
C14 N2 Pb2 O5 109.5(7) . . . . ?
C12 N2 Pb2 O1W -134.0(7) . . . . ?
C14 N2 Pb2 O1W 41.0(7) . . . . ?
C12 N2 Pb2 O4 -13.5(6) . . . . ?
C14 N2 Pb2 O4 161.6(7) . . . . ?
C1 O5 Pb2 N2 80.6(5) . . . . ?
C1 O5 Pb2 O1W 175.5(5) . . . . ?
C1 O5 Pb2 O4 -2.2(5) . . . . ?
C1 O4 Pb2 N2 -84.0(5) . . . . ?
C1 O4 Pb2 O5 2.1(4) . . . . ?
C1 O4 Pb2 O1W -0.3(5) . . . . ?
C20 C15 S1 O10 163.7(7) . . . . ?
C16 C15 S1 O10 -15.8(8) . . . . ?
C20 C15 S1 O8 -73.6(8) . . . . ?
C16 C15 S1 O8 106.9(8) . . . . ?
C20 C15 S1 O9 44.4(8) . . . . ?
C16 C15 S1 O9 -135.1(7) . . . . ?
C3 C4 S2 O2 16.2(7) . . . . ?
C5 C4 S2 O2 -165.5(6) . . . . ?
C3 C4 S2 O1 -106.4(7) . . . . ?
C5 C4 S2 O1 71.9(7) . . . . ?
C3 C4 S2 O3 136.9(6) . . . . ?
C5 C4 S2 O3 -44.8(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         1.826
_refine_diff_density_min         -1.643
_refine_diff_density_rms         0.211
_database_code_depnum_ccdc_archive 'CCDC 835435'
#######################################################################
#
#                 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_7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H7 N O6 Pb S'
_chemical_formula_weight         440.39

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'
S S 0.1246 0.1234 '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           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   6.6780(11)
_cell_length_b                   14.672(3)
_cell_length_c                   9.7183(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.169(2)
_cell_angle_gamma                90.00
_cell_volume                     948.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4645
_cell_measurement_theta_min      2.5210
_cell_measurement_theta_max      27.4940

_exptl_crystal_description       prism
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.084
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             808
_exptl_absorpt_coefficient_mu    18.024
_exptl_absorpt_correction_T_min  0.019
_exptl_absorpt_correction_T_max  0.067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean 8.3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8085
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         27.55
_reflns_number_total             2177
_reflns_number_gt                1983
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond (CRYSTAL IMPACT, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0384P)²+0.3359P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.0061(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2177
_refine_ls_number_parameters     148
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0705
_refine_ls_wR_factor_gt          0.0688
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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 -0.1954(7) 0.3801(3) 0.6591(5) 0.0168(9) Uani 1 1 d . . .
C2 C -0.0139(6) 0.3383(3) 0.6414(5) 0.0175(9) Uani 1 1 d . . .
H2 H 0.0557 0.3085 0.7155 0.021 Uiso 1 1 calc R . .
C3 C 0.0666(6) 0.3405(3) 0.5125(5) 0.0176(9) Uani 1 1 d . . .
C4 C -0.0384(7) 0.3887(3) 0.4027(5) 0.0168(9) Uani 1 1 d . . .
C5 C -0.2217(8) 0.4303(4) 0.4240(5) 0.0250(10) Uani 1 1 d . . .
H5 H -0.2914 0.4618 0.3516 0.030 Uiso 1 1 calc R . .
C6 C -0.3016(8) 0.4257(4) 0.5507(5) 0.0263(11) Uani 1 1 d . . .
H6 H -0.4246 0.4529 0.5629 0.032 Uiso 1 1 calc R . .
C7 C 0.0394(7) 0.3986(3) 0.2635(5) 0.0200(10) Uani 1 1 d . . .
N1 N 0.2458(5) 0.2902(3) 0.5011(4) 0.0224(10) Uani 1 1 d . . .
H1A H 0.3363 0.3089 0.5694 0.027 Uiso 1 1 calc R . .
H1B H 0.2936 0.3064 0.4209 0.027 Uiso 1 1 calc R . .
O1 O -0.4672(5) 0.3036(2) 0.7950(4) 0.0282(8) Uani 1 1 d . . .
O2 O -0.3819(5) 0.4581(2) 0.8537(4) 0.0266(8) Uani 1 1 d . . .
O3 O -0.1416(5) 0.3378(2) 0.9178(4) 0.0279(8) Uani 1 1 d . . .
O4 O -0.0484(6) 0.4503(3) 0.1742(4) 0.0328(9) Uani 1 1 d . . .
O5 O 0.1933(5) 0.3527(2) 0.2370(3) 0.0273(8) Uani 1 1 d . . .
O1W O 0.5642(5) 0.3470(2) 1.1262(4) 0.0289(8) Uani 1 1 d D . .
H1WB H 0.6802 0.3681 1.1150 0.12(4) Uiso 1 1 d RD . .
H1WA H 0.5702 0.3143 1.1985 0.10(3) Uiso 1 1 d RD . .
Pb1 Pb 0.23764(2) 0.398301(12) 1.009022(18) 0.02030(11) Uani 1 1 d . . .
S1 S -0.30230(16) 0.36930(7) 0.81860(11) 0.0166(2) Uani 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
C1 C2 1.383(6) . ?
C1 C6 1.388(7) . ?
C1 S1 1.771(5) . ?
C2 C3 1.407(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.413(6) . ?
C3 N1 1.419(5) . ?
C4 C5 1.400(6) . ?
C4 C7 1.499(7) . ?
C5 C6 1.387(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O4 1.258(5) . ?
C7 O5 1.275(6) . ?
N1 Pb1 2.767(5) 4_565 ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
O1 S1 1.466(3) . ?
O2 S1 1.460(3) . ?
O2 Pb1 2.629(3) 3_567 ?
O3 S1 1.452(4) . ?
O3 Pb1 2.754(3) . ?
O4 Pb1 2.713(4) 1_554 ?
O5 Pb1 2.358(3) 1_554 ?
O1W Pb1 2.485(3) . ?
O1W H1WB 0.8510 . ?
O1W H1WA 0.8490 . ?
Pb1 O5 2.358(3) 1_556 ?
Pb1 O2 2.629(3) 3_567 ?
Pb1 O4 2.713(4) 1_556 ?
Pb1 N1 2.767(5) 4_566 ?

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 C6 120.9(4) . . ?
C2 C1 S1 119.7(3) . . ?
C6 C1 S1 119.3(4) . . ?
C1 C2 C3 120.7(4) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C2 C3 C4 118.7(4) . . ?
C2 C3 N1 116.8(4) . . ?
C4 C3 N1 124.4(4) . . ?
C5 C4 C3 119.2(4) . . ?
C5 C4 C7 118.0(4) . . ?
C3 C4 C7 122.8(4) . . ?
C6 C5 C4 121.4(5) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C1 119.1(5) . . ?
C5 C6 H6 120.4 . . ?
C1 C6 H6 120.4 . . ?
O4 C7 O5 120.9(5) . . ?
O4 C7 C4 120.3(4) . . ?
O5 C7 C4 118.9(4) . . ?
C3 N1 Pb1 119.9(3) . 4_565 ?
C3 N1 H1A 107.3 . . ?
Pb1 N1 H1A 107.3 4_565 . ?
C3 N1 H1B 107.3 . . ?
Pb1 N1 H1B 107.3 4_565 . ?
H1A N1 H1B 106.9 . . ?
S1 O2 Pb1 135.2(2) . 3_567 ?
S1 O3 Pb1 135.6(2) . . ?
C7 O4 Pb1 86.0(3) . 1_554 ?
C7 O5 Pb1 102.2(3) . 1_554 ?
Pb1 O1W H1WB 127.0 . . ?
Pb1 O1W H1WA 121.7 . . ?
H1WB O1W H1WA 109.7 . . ?
O5 Pb1 O1W 70.28(12) 1_556 . ?
O5 Pb1 O2 79.73(11) 1_556 3_567 ?
O1W Pb1 O2 75.16(11) . 3_567 ?
O5 Pb1 O4 50.90(11) 1_556 1_556 ?
O1W Pb1 O4 116.73(11) . 1_556 ?
O2 Pb1 O4 73.72(11) 3_567 1_556 ?
O5 Pb1 O3 91.23(11) 1_556 . ?
O1W Pb1 O3 142.52(12) . . ?
O2 Pb1 O3 134.91(10) 3_567 . ?
O4 Pb1 O3 66.74(11) 1_556 . ?
O5 Pb1 N1 75.37(11) 1_556 4_566 ?
O1W Pb1 N1 72.02(11) . 4_566 ?
O2 Pb1 N1 143.86(10) 3_567 4_566 ?
O4 Pb1 N1 108.33(11) 1_556 4_566 ?
O3 Pb1 N1 71.85(10) . 4_566 ?
O3 S1 O2 113.1(2) . . ?
O3 S1 O1 113.2(2) . . ?
O2 S1 O1 109.8(2) . . ?
O3 S1 C1 106.1(2) . . ?
O2 S1 C1 108.0(2) . . ?
O1 S1 C1 106.1(2) . . ?

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
C6 C1 C2 C3 -0.6(7) . . . . ?
S1 C1 C2 C3 175.4(3) . . . . ?
C1 C2 C3 C4 2.0(6) . . . . ?
C1 C2 C3 N1 -175.4(4) . . . . ?
C2 C3 C4 C5 -1.9(6) . . . . ?
N1 C3 C4 C5 175.3(4) . . . . ?
C2 C3 C4 C7 177.2(4) . . . . ?
N1 C3 C4 C7 -5.6(6) . . . . ?
C3 C4 C5 C6 0.4(7) . . . . ?
C7 C4 C5 C6 -178.7(4) . . . . ?
C4 C5 C6 C1 1.1(7) . . . . ?
C2 C1 C6 C5 -1.0(7) . . . . ?
S1 C1 C6 C5 -177.0(4) . . . . ?
C5 C4 C7 O4 6.9(6) . . . . ?
C3 C4 C7 O4 -172.2(4) . . . . ?
C5 C4 C7 O5 -172.0(4) . . . . ?
C3 C4 C7 O5 8.9(6) . . . . ?
C2 C3 N1 Pb1 68.6(4) . . . 4_565 ?
C4 C3 N1 Pb1 -108.7(4) . . . 4_565 ?
O5 C7 O4 Pb1 -1.1(4) . . . 1_554 ?
C4 C7 O4 Pb1 180.0(4) . . . 1_554 ?
O4 C7 O5 Pb1 1.3(5) . . . 1_554 ?
C4 C7 O5 Pb1 -179.8(3) . . . 1_554 ?
S1 O3 Pb1 O5 141.9(3) . . . 1_556 ?
S1 O3 Pb1 O1W -159.8(2) . . . . ?
S1 O3 Pb1 O2 65.3(3) . . . 3_567 ?
S1 O3 Pb1 O4 96.0(3) . . . 1_556 ?
S1 O3 Pb1 N1 -143.9(3) . . . 4_566 ?
Pb1 O3 S1 O2 -62.3(3) . . . . ?
Pb1 O3 S1 O1 172.0(2) . . . . ?
Pb1 O3 S1 C1 55.9(3) . . . . ?
Pb1 O2 S1 O3 27.5(4) 3_567 . . . ?
Pb1 O2 S1 O1 155.1(2) 3_567 . . . ?
Pb1 O2 S1 C1 -89.6(3) 3_567 . . . ?
C2 C1 S1 O3 16.4(4) . . . . ?
C6 C1 S1 O3 -167.5(4) . . . . ?
C2 C1 S1 O2 138.0(3) . . . . ?
C6 C1 S1 O2 -46.0(4) . . . . ?
C2 C1 S1 O1 -104.3(4) . . . . ?
C6 C1 S1 O1 71.8(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.252
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.219
_database_code_depnum_ccdc_archive 'CCDC 835436'
#######################################################################
#
#                 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_zl05

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H16 N2 O11 S2'
_chemical_formula_weight         452.41

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.2881(12)
_cell_length_b                   8.0961(14)
_cell_length_c                   8.6404(14)
_cell_angle_alpha                93.554(5)
_cell_angle_beta                 97.654(6)
_cell_angle_gamma                102.178(6)
_cell_volume                     424.30(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3553
_cell_measurement_theta_min      2.5849
_cell_measurement_theta_max      27.0839

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             234
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean 8.3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8567
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.58
_diffrn_reflns_theta_max         27.56
_reflns_number_total             1955
_reflns_number_gt                1598
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond (CRYSTAL IMPACT, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0456P)²+0.2654P] where P=(Fo²+2Fc²)/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         1955
_refine_ls_number_parameters     135
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1002
_refine_ls_wR_factor_gt          0.0934
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.2192(3) 0.2832(2) 0.1568(2) 0.0232(4) Uani 1 1 d . . .
C2 C 0.0001(3) 0.2108(2) 0.1678(2) 0.0216(4) Uani 1 1 d . . .
C3 C -0.1588(3) 0.1726(2) 0.0358(2) 0.0224(4) Uani 1 1 d . . .
H3 H -0.3040 0.1241 0.0446 0.027 Uiso 1 1 calc R . .
C4 C -0.0995(3) 0.2072(2) -0.1091(2) 0.0223(4) Uani 1 1 d . . .
C5 C 0.1169(4) 0.2783(3) -0.1237(2) 0.0337(5) Uani 1 1 d . . .
H5 H 0.1561 0.3012 -0.2215 0.040 Uiso 1 1 calc R . .
C6 C 0.2737(4) 0.3146(3) 0.0095(3) 0.0315(5) Uani 1 1 d . . .
H6 H 0.4192 0.3612 -0.0001 0.038 Uiso 1 1 calc R . .
C7 C 0.4048(3) 0.3253(2) 0.2921(2) 0.0254(4) Uani 1 1 d . . .
N1 N -0.0697(3) 0.1665(3) 0.31747(19) 0.0304(4) Uani 1 1 d . . .
H1A H -0.2111 0.1138 0.3014 0.046 Uiso 1 1 calc R . .
H1B H -0.0510 0.2606 0.3814 0.046 Uiso 1 1 calc R . .
H1C H 0.0106 0.0983 0.3607 0.046 Uiso 1 1 calc R . .
O1 O 0.3405(2) 0.3080(2) 0.43029(16) 0.0311(4) Uani 1 1 d . . .
H1 H 0.4481 0.3149 0.4974 0.047 Uiso 1 1 calc R . .
O2 O 0.5939(2) 0.3719(2) 0.27298(19) 0.0379(4) Uani 1 1 d . . .
O3 O -0.4841(3) 0.0362(2) -0.23777(17) 0.0378(4) Uani 1 1 d . . .
O4 O -0.3511(3) 0.3122(2) -0.32488(18) 0.0392(4) Uani 1 1 d . . .
O5 O -0.1905(3) 0.0788(2) -0.39607(17) 0.0350(4) Uani 1 1 d . . .
O1W O 0.0000 0.5000 0.5000 0.0508(7) Uani 1 2 d SD . .
H1WA H 0.0469 0.5383 0.4171 0.061 Uiso 0.50 1 d PRD . .
H1WB H 0.1155 0.5003 0.5662 0.061 Uiso 0.50 1 d PRD . .
S1 S -0.30013(8) 0.15279(6) -0.28101(5) 0.02307(16) Uani 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
C1 C6 1.386(3) . ?
C1 C2 1.397(3) . ?
C1 C7 1.505(3) . ?
C2 C3 1.384(3) . ?
C2 N1 1.461(2) . ?
C3 C4 1.382(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(3) . ?
C4 S1 1.7824(19) . ?
C5 C6 1.384(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O2 1.206(2) . ?
C7 O1 1.317(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
O1 H1 0.8200 . ?
O3 S1 1.4374(16) . ?
O4 S1 1.4545(16) . ?
O5 S1 1.4511(16) . ?
O1W H1WA 0.8611 . ?
O1W H1WB 0.8622 . ?

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
C6 C1 C2 118.08(17) . . ?
C6 C1 C7 116.64(18) . . ?
C2 C1 C7 125.24(18) . . ?
C3 C2 C1 121.12(18) . . ?
C3 C2 N1 117.20(17) . . ?
C1 C2 N1 121.64(17) . . ?
C4 C3 C2 119.37(18) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.80(18) . . ?
C3 C4 S1 119.98(15) . . ?
C5 C4 S1 119.17(15) . . ?
C6 C5 C4 118.97(19) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C1 121.65(19) . . ?
C5 C6 H6 119.2 . . ?
C1 C6 H6 119.2 . . ?
O2 C7 O1 124.13(18) . . ?
O2 C7 C1 121.99(19) . . ?
O1 C7 C1 113.88(17) . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C7 O1 H1 109.5 . . ?
H1WA O1W H1WB 106.2 . . ?
O3 S1 O5 113.87(10) . . ?
O3 S1 O4 113.46(11) . . ?
O5 S1 O4 111.92(10) . . ?
O3 S1 C4 106.28(9) . . ?
O5 S1 C4 104.84(9) . . ?
O4 S1 C4 105.54(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
C6 C1 C2 C3 -0.5(3) . . . . ?
C7 C1 C2 C3 -178.38(18) . . . . ?
C6 C1 C2 N1 177.25(19) . . . . ?
C7 C1 C2 N1 -0.6(3) . . . . ?
C1 C2 C3 C4 -0.2(3) . . . . ?
N1 C2 C3 C4 -178.04(17) . . . . ?
C2 C3 C4 C5 0.5(3) . . . . ?
C2 C3 C4 S1 178.05(15) . . . . ?
C3 C4 C5 C6 -0.1(3) . . . . ?
S1 C4 C5 C6 -177.67(17) . . . . ?
C4 C5 C6 C1 -0.6(3) . . . . ?
C2 C1 C6 C5 0.9(3) . . . . ?
C7 C1 C6 C5 179.0(2) . . . . ?
C6 C1 C7 O2 -5.4(3) . . . . ?
C2 C1 C7 O2 172.5(2) . . . . ?
C6 C1 C7 O1 173.93(18) . . . . ?
C2 C1 C7 O1 -8.2(3) . . . . ?
C3 C4 S1 O3 -15.7(2) . . . . ?
C5 C4 S1 O3 161.94(17) . . . . ?
C3 C4 S1 O5 -136.56(17) . . . . ?
C5 C4 S1 O5 41.04(19) . . . . ?
C3 C4 S1 O4 105.11(18) . . . . ?
C5 C4 S1 O4 -77.29(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.067
_database_code_depnum_ccdc_archive 'CCDC 989589'
