Supplementary material (ESI) for Journal of Materials Chemistry
This journal is © The Royal Society of Chemistry 2004


data_global

_journal_coden_Cambridge         1145

loop_
_publ_author_name
'Sun Wei-Yin'
'Jian Fan'
'Guohong Ma'
'Taka-aki Okamura'
'Bin Sui'
'Sing Hai Tang'
'Norikazu Ueyama'
'Wei Zhao'

_publ_contact_author_name        'Dr Sun Wei-Yin'
_publ_contact_author_address     
;
Coordination Chemistry Institute
Nanjing University
Nanjing
210093
CHINA
;

_publ_contact_author_email       SUNWY@NJU.EDU.CN

_publ_requested_journal          'Journal of Materials Chemistry'

_publ_section_title              
;
Novel Pb(II) Coordination Frameworks: Synthesis,
Crystal Structures and Unusual Third-Order Nonlinear Optical Properties
;

data_1
_database_code_depnum_ccdc_archive 'CCDC 227127'
_audit_creation_date             'Sat Mar  1 20:47:46 2003'
_audit_creation_method           SHELXL-97

_publ_section_references         
;
ENTER OTHER REFERENCES
Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan.
Single Crystal Structure Analysis Software. Version 1.11.
MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.
Rigaku, 3-9-12 Akishima, Tokyo, Japan.
;

_chemical_name_systematic        
;
[Pb(dimb)(dmf)(NO3)2]
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H23 N7 O7 Pb '
_chemical_formula_sum            'C18 H23 N7 O7 Pb'
_chemical_formula_weight         656.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1         '
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.248(11)
_cell_length_b                   13.72(3)
_cell_length_c                   17.30(2)
_cell_angle_alpha                71.56(15)
_cell_angle_beta                 83.08(11)
_cell_angle_gamma                68.62(15)
_cell_volume                     2357(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    200
_cell_measurement_reflns_used    12621
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    7.210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.430
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_process_details   '(Higashi, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 10.00
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21828
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0883
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         27.48
_reflns_number_total             10304
_reflns_number_gt                6881
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10304
_refine_ls_number_parameters     601
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.0840
_refine_ls_wR_factor_gt          0.0785
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_restrained_S_all      0.866
_refine_ls_shift/su_max          0.002
_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
Pb1 Pb 0.62138(2) 0.68477(2) 1.142911(14) 0.03090(8) Uani 1 1 d . . .
Pb2 Pb 1.09816(2) 0.67578(2) 0.652515(14) 0.03517(8) Uani 1 1 d . . .
O11 O 0.9332(7) 0.5230(5) 1.3182(4) 0.082(2) Uani 1 1 d . . .
O12 O 0.7313(8) 0.5598(8) 1.3325(5) 0.101(3) Uani 1 1 d . . .
O13 O 0.8029(9) 0.6810(6) 1.2562(5) 0.112(3) Uani 1 1 d . . .
O21 O 0.8317(5) 0.4838(4) 1.1765(3) 0.0487(12) Uani 1 1 d . . .
O22 O 0.6726(5) 0.4979(4) 1.1109(3) 0.0584(15) Uani 1 1 d . . .
O23 O 0.7901(6) 0.3400(4) 1.1834(4) 0.0637(16) Uani 1 1 d . . .
O31 O 0.9736(5) 0.8809(5) 0.6072(4) 0.0690(18) Uani 1 1 d . . .
O32 O 1.1464(5) 0.8631(6) 0.6599(4) 0.0713(18) Uani 1 1 d . . .
O33 O 0.9876(6) 1.0158(5) 0.6399(4) 0.0651(17) Uani 1 1 d . . .
O41 O 0.5521(4) 0.9864(4) 0.8429(3) 0.0443(12) Uani 1 1 d . . .
O42 O 0.4167(5) 1.1011(5) 0.9022(3) 0.0539(14) Uani 1 1 d . . .
O43 O 0.5723(5) 1.1418(4) 0.8313(3) 0.0529(14) Uani 1 1 d . . .
O71 O 0.4405(6) 0.6046(5) 1.2226(4) 0.0695(17) Uani 1 1 d . . .
O81 O 0.8806(5) 0.6991(5) 0.7308(3) 0.0609(16) Uani 1 1 d . . .
N1 N 0.8219(9) 0.5886(7) 1.3023(5) 0.072(2) Uani 1 1 d . . .
N2 N 0.7646(6) 0.4402(5) 1.1573(4) 0.0419(14) Uani 1 1 d . . .
N3 N 1.0345(6) 0.9222(6) 0.6343(4) 0.0468(16) Uani 1 1 d . . .
N4 N 0.5135(5) 1.0751(5) 0.8595(3) 0.0345(13) Uani 1 1 d . . .
N7 N 0.2610(7) 0.6181(6) 1.2992(4) 0.0577(18) Uani 1 1 d . . .
N8 N 0.7521(6) 0.6258(6) 0.8210(4) 0.0515(17) Uani 1 1 d . . .
N11 N 0.8544(5) 0.8062(5) 0.9136(3) 0.0373(13) Uani 1 1 d . . .
N12 N 0.7794(5) 0.7200(5) 1.0273(3) 0.0351(13) Uani 1 1 d . . .
N31 N 0.3670(5) 0.8198(5) 0.9179(3) 0.0320(12) Uani 1 1 d . . .
N32 N 0.4777(5) 0.7331(4) 1.0313(3) 0.0313(12) Uani 1 1 d . . .
N111 N 0.8530(5) 0.7854(5) 0.4264(3) 0.0353(13) Uani 1 1 d . . .
N112 N 0.9624(5) 0.7068(5) 0.5404(3) 0.0409(14) Uani 1 1 d . . .
N131 N 1.3288(5) 0.7986(6) 0.4206(4) 0.0479(17) Uani 1 1 d . . .
N132 N 1.2533(6) 0.7110(6) 0.5331(4) 0.0474(16) Uani 1 1 d . . .
C1 C 0.9516(6) 0.9504(6) 0.8547(4) 0.0340(15) Uani 1 1 d . . .
C2 C 1.0819(6) 0.9095(5) 0.8418(4) 0.0309(14) Uani 1 1 d . . .
H1 H 1.1172 0.8473 0.8223 0.037 Uiso 1 1 calc R . .
C3 C 1.1621(6) 0.9581(6) 0.8570(4) 0.0332(15) Uani 1 1 d . . .
C4 C 1.1090(6) 1.0511(6) 0.8825(4) 0.0371(15) Uani 1 1 d . . .
H2 H 1.1635 1.0855 0.8916 0.045 Uiso 1 1 calc R . .
C5 C 0.9777(7) 1.0959(7) 0.8954(4) 0.0436(17) Uani 1 1 d . . .
C6 C 0.9008(6) 1.0426(6) 0.8821(4) 0.0404(17) Uani 1 1 d . . .
H3 H 0.8115 1.0700 0.8919 0.048 Uiso 1 1 calc R . .
C11 C 0.8663(7) 0.8935(6) 0.8409(4) 0.0413(17) Uani 1 1 d . . .
H4 H 0.7804 0.9483 0.8246 0.050 Uiso 1 1 calc R . .
H5 H 0.9018 0.8617 0.7954 0.050 Uiso 1 1 calc R . .
C12 C 0.7627(6) 0.8150(6) 0.9715(4) 0.0408(17) Uani 1 1 d . . .
H6 H 0.6949 0.8811 0.9719 0.049 Uiso 1 1 calc R . .
C13 C 0.8873(7) 0.6469(7) 1.0056(5) 0.0488(19) Uani 1 1 d . . .
H7 H 0.9240 0.5716 1.0350 0.059 Uiso 1 1 calc R . .
C14 C 0.9330(7) 0.6988(7) 0.9362(5) 0.051(2) Uani 1 1 d . . .
H8 H 1.0071 0.6668 0.9076 0.062 Uiso 1 1 calc R . .
C31 C 1.3043(6) 0.9091(6) 0.8455(4) 0.0386(17) Uani 1 1 d . . .
H9 H 1.3210 0.8803 0.7980 0.046 Uiso 1 1 calc R . .
H10 H 1.3420 0.9672 0.8336 0.046 Uiso 1 1 calc R . .
C32 C 0.4299(5) 0.8286(6) 0.9750(4) 0.0310(14) Uani 1 1 d . . .
H11 H 0.4391 0.8947 0.9751 0.037 Uiso 1 1 calc R . .
C33 C 0.4406(6) 0.6604(6) 1.0082(4) 0.0361(16) Uani 1 1 d . . .
H12 H 0.4598 0.5849 1.0371 0.043 Uiso 1 1 calc R . .
C34 C 0.3733(6) 0.7130(6) 0.9386(4) 0.0397(17) Uani 1 1 d . . .
H13 H 0.3373 0.6822 0.9096 0.048 Uiso 1 1 calc R . .
C51 C 0.9227(8) 1.1959(7) 0.9237(5) 0.063(2) Uani 1 1 d . . .
H14 H 0.9544 1.1795 0.9784 0.075 Uiso 1 1 calc R . .
H15 H 0.8294 1.2185 0.9253 0.075 Uiso 1 1 calc R . .
H16 H 0.9483 1.2552 0.8860 0.075 Uiso 1 1 calc R . .
C71 C 0.3365(8) 0.6591(8) 1.2432(5) 0.055(2) Uani 1 1 d . . .
H17 H 0.3073 0.7360 1.2178 0.067 Uiso 1 1 calc R . .
C72 C 0.3029(11) 0.5009(9) 1.3428(7) 0.100(4) Uani 1 1 d . . .
H18 H 0.3908 0.4652 1.3268 0.120 Uiso 1 1 calc R . .
H19 H 0.2469 0.4683 1.3291 0.120 Uiso 1 1 calc R . .
H20 H 0.2991 0.4905 1.4016 0.120 Uiso 1 1 calc R . .
C73 C 0.1385(9) 0.6863(10) 1.3205(7) 0.092(4) Uani 1 1 d . . .
H21 H 0.1351 0.6765 1.3793 0.110 Uiso 1 1 calc R . .
H22 H 0.0713 0.6658 1.3059 0.110 Uiso 1 1 calc R . .
H23 H 0.1255 0.7632 1.2908 0.110 Uiso 1 1 calc R . .
C81 C 0.8589(8) 0.6196(8) 0.7792(5) 0.053(2) Uani 1 1 d . . .
H24 H 0.9234 0.5495 0.7869 0.063 Uiso 1 1 calc R . .
C82 C 0.6500(8) 0.7289(8) 0.8127(6) 0.068(3) Uani 1 1 d . . .
H25 H 0.6715 0.7865 0.7697 0.082 Uiso 1 1 calc R . .
H26 H 0.6377 0.7467 0.8644 0.082 Uiso 1 1 calc R . .
H27 H 0.5711 0.7239 0.7984 0.082 Uiso 1 1 calc R . .
C83 C 0.7332(10) 0.5289(9) 0.8773(7) 0.092(4) Uani 1 1 d . . .
H28 H 0.8081 0.4643 0.8759 0.111 Uiso 1 1 calc R . .
H29 H 0.6573 0.5209 0.8615 0.111 Uiso 1 1 calc R . .
H30 H 0.7215 0.5361 0.9325 0.111 Uiso 1 1 calc R . .
C101 C 0.6533(6) 0.9277(6) 0.3618(4) 0.0374(16) Uani 1 1 d . . .
C102 C 0.5632(7) 0.8852(7) 0.3495(4) 0.0435(17) Uani 1 1 d . . .
H31 H 0.5903 0.8210 0.3324 0.052 Uiso 1 1 calc R . .
C103 C 0.4341(7) 0.9378(7) 0.3623(4) 0.0456(19) Uani 1 1 d . . .
C104 C 0.3953(7) 1.0320(7) 0.3841(4) 0.052(2) Uani 1 1 d . . .
H32 H 0.3069 1.0663 0.3931 0.062 Uiso 1 1 calc R . .
C105 C 0.4804(8) 1.0799(7) 0.3936(4) 0.0494(19) Uani 1 1 d . . .
C106 C 0.6108(7) 1.0236(7) 0.3833(4) 0.0467(19) Uani 1 1 d . . .
H33 H 0.6716 1.0527 0.3913 0.056 Uiso 1 1 calc R . .
C111 C 0.7940(6) 0.8704(6) 0.3499(4) 0.0412(17) Uani 1 1 d . . .
H34 H 0.8056 0.8355 0.3061 0.049 Uiso 1 1 calc R . .
H35 H 0.8376 0.9249 0.3328 0.049 Uiso 1 1 calc R . .
C112 C 0.9197(6) 0.7980(6) 0.4805(4) 0.0389(16) Uani 1 1 d . . .
H36 H 0.9338 0.8639 0.4758 0.047 Uiso 1 1 calc R . .
C113 C 0.9201(7) 0.6338(7) 0.5242(4) 0.0435(17) Uani 1 1 d . . .
H37 H 0.9370 0.5601 0.5570 0.052 Uiso 1 1 calc R . .
C114 C 0.8506(7) 0.6812(6) 0.4547(4) 0.0428(17) Uani 1 1 d . . .
H38 H 0.8090 0.6488 0.4308 0.051 Uiso 1 1 calc R . .
C131 C 0.3387(7) 0.8892(7) 0.3496(4) 0.055(2) Uani 1 1 d . . .
H39 H 0.2537 0.9475 0.3384 0.066 Uiso 1 1 calc R . .
H40 H 0.3648 0.8622 0.3013 0.066 Uiso 1 1 calc R . .
C132 C 1.2411(7) 0.8050(8) 0.4797(4) 0.051(2) Uani 1 1 d . . .
H41 H 1.1762 0.8717 0.4824 0.061 Uiso 1 1 calc R . .
C133 C 1.3614(8) 0.6381(8) 0.5085(5) 0.062(2) Uani 1 1 d . . .
H42 H 1.3979 0.5620 0.5357 0.075 Uiso 1 1 calc R . .
C134 C 1.4061(8) 0.6937(9) 0.4391(6) 0.068(3) Uani 1 1 d . . .
H43 H 1.4791 0.6637 0.4089 0.082 Uiso 1 1 calc R . .
C151 C 0.4361(9) 1.1843(8) 0.4169(6) 0.072(3) Uani 1 1 d . . .
H44 H 0.4857 1.2302 0.3865 0.086 Uiso 1 1 calc R . .
H45 H 0.4483 1.1671 0.4755 0.086 Uiso 1 1 calc R . .
H46 H 0.3454 1.2237 0.4038 0.086 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.03483(14) 0.03010(15) 0.02790(13) -0.00869(11) -0.00050(11) -0.01119(12)
Pb2 0.03407(14) 0.03980(18) 0.02935(14) -0.00909(13) -0.00282(12) -0.01033(13)
O11 0.092(4) 0.052(4) 0.099(5) -0.033(4) -0.050(4) 0.002(4)
O12 0.088(5) 0.138(8) 0.087(5) -0.055(5) 0.035(5) -0.042(6)
O13 0.169(8) 0.046(5) 0.122(6) -0.022(4) -0.088(6) -0.015(5)
O21 0.047(3) 0.049(3) 0.051(3) -0.015(3) -0.011(2) -0.014(3)
O22 0.060(3) 0.037(3) 0.068(4) -0.012(3) -0.036(3) 0.004(3)
O23 0.087(4) 0.029(3) 0.073(4) -0.015(3) -0.035(3) -0.007(3)
O31 0.067(4) 0.056(4) 0.093(5) -0.024(4) -0.031(3) -0.020(3)
O32 0.053(3) 0.079(5) 0.087(5) -0.036(4) -0.003(3) -0.019(3)
O33 0.076(4) 0.042(4) 0.077(4) -0.003(3) -0.022(3) -0.025(3)
O41 0.045(3) 0.033(3) 0.056(3) -0.021(2) 0.002(2) -0.010(2)
O42 0.049(3) 0.048(3) 0.062(3) -0.023(3) 0.022(3) -0.016(3)
O43 0.053(3) 0.051(3) 0.068(3) -0.027(3) 0.022(3) -0.032(3)
O71 0.074(4) 0.066(4) 0.074(4) -0.020(3) 0.028(3) -0.040(4)
O81 0.045(3) 0.075(4) 0.053(3) -0.005(3) 0.008(3) -0.023(3)
N1 0.095(6) 0.058(6) 0.057(5) -0.028(4) -0.034(5) 0.000(5)
N2 0.052(4) 0.028(3) 0.041(3) -0.013(3) -0.009(3) -0.004(3)
N3 0.057(4) 0.045(4) 0.036(3) 0.000(3) 0.000(3) -0.026(4)
N4 0.038(3) 0.033(3) 0.029(3) -0.007(3) -0.002(3) -0.009(3)
N7 0.063(4) 0.060(5) 0.053(4) -0.012(4) 0.012(4) -0.031(4)
N8 0.047(3) 0.058(5) 0.054(4) -0.018(3) 0.014(3) -0.028(4)
N11 0.032(3) 0.044(4) 0.033(3) -0.008(3) -0.001(3) -0.013(3)
N12 0.040(3) 0.035(3) 0.033(3) -0.011(3) 0.011(3) -0.018(3)
N31 0.026(2) 0.032(3) 0.036(3) -0.008(2) 0.000(2) -0.009(2)
N32 0.034(3) 0.028(3) 0.032(3) -0.011(2) -0.003(2) -0.008(2)
N111 0.034(3) 0.047(4) 0.025(3) -0.007(3) -0.003(2) -0.016(3)
N112 0.039(3) 0.046(4) 0.036(3) -0.011(3) -0.006(3) -0.012(3)
N131 0.037(3) 0.073(5) 0.036(3) -0.015(3) 0.003(3) -0.023(4)
N132 0.047(3) 0.059(5) 0.037(3) -0.007(3) 0.005(3) -0.025(4)
C1 0.034(3) 0.041(4) 0.024(3) -0.006(3) -0.002(3) -0.013(3)
C2 0.037(3) 0.024(3) 0.027(3) -0.005(3) 0.001(3) -0.007(3)
C3 0.029(3) 0.039(4) 0.026(3) 0.001(3) -0.006(3) -0.012(3)
C4 0.047(4) 0.032(4) 0.033(3) -0.004(3) -0.008(3) -0.016(3)
C5 0.049(4) 0.044(5) 0.033(4) -0.011(3) -0.006(3) -0.010(4)
C6 0.031(3) 0.050(5) 0.034(4) -0.012(3) 0.003(3) -0.008(3)
C11 0.042(4) 0.055(5) 0.029(3) -0.007(3) 0.003(3) -0.025(4)
C12 0.031(3) 0.046(5) 0.037(4) -0.004(3) 0.001(3) -0.012(3)
C13 0.048(4) 0.039(5) 0.052(4) -0.017(4) 0.021(4) -0.010(4)
C14 0.051(4) 0.045(5) 0.056(5) -0.023(4) 0.022(4) -0.013(4)
C31 0.031(3) 0.049(4) 0.027(3) 0.004(3) -0.001(3) -0.015(3)
C32 0.025(3) 0.036(4) 0.030(3) -0.007(3) -0.003(3) -0.009(3)
C33 0.034(3) 0.038(4) 0.042(4) -0.009(3) -0.002(3) -0.021(3)
C34 0.032(3) 0.051(5) 0.043(4) -0.017(4) 0.002(3) -0.019(3)
C51 0.076(5) 0.052(6) 0.056(5) -0.022(4) -0.006(5) -0.012(5)
C71 0.056(5) 0.058(6) 0.056(5) -0.012(4) 0.003(4) -0.028(5)
C72 0.106(8) 0.075(8) 0.100(8) 0.006(7) 0.026(7) -0.046(7)
C73 0.058(5) 0.108(10) 0.105(9) -0.040(8) 0.017(6) -0.022(6)
C81 0.051(5) 0.059(6) 0.054(5) -0.023(4) 0.014(4) -0.024(4)
C82 0.058(5) 0.073(7) 0.064(6) -0.015(5) 0.011(5) -0.020(5)
C83 0.102(8) 0.061(7) 0.115(9) -0.032(6) 0.048(7) -0.040(6)
C101 0.039(4) 0.046(4) 0.024(3) -0.005(3) -0.002(3) -0.015(3)
C102 0.051(4) 0.052(5) 0.028(3) -0.009(3) -0.004(3) -0.018(4)
C103 0.043(4) 0.064(6) 0.024(3) -0.001(4) 0.002(3) -0.023(4)
C104 0.043(4) 0.063(6) 0.032(4) -0.007(4) 0.010(4) -0.007(4)
C105 0.060(5) 0.042(5) 0.036(4) -0.009(4) 0.003(4) -0.008(4)
C106 0.056(4) 0.052(5) 0.031(4) -0.005(3) -0.007(4) -0.022(4)
C111 0.041(4) 0.051(5) 0.027(3) -0.004(3) -0.007(3) -0.015(4)
C112 0.040(4) 0.036(4) 0.032(3) -0.003(3) -0.011(3) -0.007(3)
C113 0.052(4) 0.042(4) 0.034(4) -0.010(3) -0.007(3) -0.013(4)
C114 0.048(4) 0.044(5) 0.042(4) -0.014(3) -0.003(3) -0.020(4)
C131 0.051(4) 0.080(7) 0.030(4) -0.002(4) -0.003(4) -0.030(5)
C132 0.044(4) 0.068(6) 0.037(4) -0.013(4) 0.008(4) -0.020(4)
C133 0.057(5) 0.054(6) 0.072(6) -0.022(5) 0.025(5) -0.021(5)
C134 0.062(5) 0.076(7) 0.071(6) -0.036(6) 0.035(5) -0.026(5)
C151 0.089(6) 0.050(6) 0.064(6) -0.020(5) 0.002(5) -0.008(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N32 2.438(6) . ?
Pb1 N12 2.559(6) . ?
Pb1 O22 2.637(7) . ?
Pb1 O42 2.670(8) 2_677 ?
Pb1 O71 2.691(7) . ?
Pb1 O43 2.695(8) 2_677 ?
Pb2 N112 2.448(6) . ?
Pb2 O31 2.547(9) . ?
Pb2 N132 2.581(7) . ?
Pb2 O81 2.613(6) . ?
Pb2 O11 2.757(8) 2_767 ?
O11 N1 1.248(10) . ?
O11 Pb2 2.757(8) 2_767 ?
O12 N1 1.224(10) . ?
O13 N1 1.222(11) . ?
O21 N2 1.246(7) . ?
O22 N2 1.242(8) . ?
O23 N2 1.236(8) . ?
O31 N3 1.241(8) . ?
O32 N3 1.265(9) . ?
O33 N3 1.228(9) . ?
O41 N4 1.248(8) . ?
O42 N4 1.245(7) . ?
O42 Pb1 2.670(8) 2_677 ?
O43 N4 1.262(7) . ?
O43 Pb1 2.695(8) 2_677 ?
O71 C71 1.219(10) . ?
O81 C81 1.232(10) . ?
N7 C71 1.335(10) . ?
N7 C73 1.437(12) . ?
N7 C72 1.464(12) . ?
N8 C81 1.314(9) . ?
N8 C82 1.438(11) . ?
N8 C83 1.447(12) . ?
N11 C12 1.347(8) . ?
N11 C14 1.369(10) . ?
N11 C11 1.469(9) . ?
N12 C12 1.317(9) . ?
N12 C13 1.364(9) . ?
N31 C32 1.340(8) . ?
N31 C34 1.371(9) . ?
N31 C31 1.475(8) 1_455 ?
N32 C32 1.326(9) . ?
N32 C33 1.387(8) . ?
N111 C112 1.354(8) . ?
N111 C114 1.366(9) . ?
N111 C111 1.490(9) . ?
N112 C112 1.316(9) . ?
N112 C113 1.365(9) . ?
N131 C132 1.333(9) . ?
N131 C134 1.338(12) . ?
N131 C131 1.473(10) 1_655 ?
N132 C132 1.297(10) . ?
N132 C133 1.384(11) . ?
C1 C2 1.384(9) . ?
C1 C6 1.391(10) . ?
C1 C11 1.518(9) . ?
C2 C3 1.390(9) . ?
C2 H1 0.9500 . ?
C3 C4 1.385(10) . ?
C3 C31 1.508(9) . ?
C4 C5 1.398(10) . ?
C4 H2 0.9500 . ?
C5 C6 1.398(10) . ?
C5 C51 1.495(12) . ?
C6 H3 0.9500 . ?
C11 H4 0.9900 . ?
C11 H5 0.9900 . ?
C12 H6 0.9500 . ?
C13 C14 1.338(10) . ?
C13 H7 0.9500 . ?
C14 H8 0.9500 . ?
C31 N31 1.475(8) 1_655 ?
C31 H9 0.9900 . ?
C31 H10 0.9900 . ?
C32 H11 0.9500 . ?
C33 C34 1.348(9) . ?
C33 H12 0.9500 . ?
C34 H13 0.9500 . ?
C51 H14 0.9800 . ?
C51 H15 0.9800 . ?
C51 H16 0.9800 . ?
C71 H17 0.9500 . ?
C72 H18 0.9800 . ?
C72 H19 0.9800 . ?
C72 H20 0.9800 . ?
C73 H21 0.9800 . ?
C73 H22 0.9800 . ?
C73 H23 0.9800 . ?
C81 H24 0.9500 . ?
C82 H25 0.9800 . ?
C82 H26 0.9800 . ?
C82 H27 0.9800 . ?
C83 H28 0.9800 . ?
C83 H29 0.9800 . ?
C83 H30 0.9800 . ?
C101 C106 1.381(11) . ?
C101 C102 1.404(9) . ?
C101 C111 1.510(10) . ?
C102 C103 1.392(10) . ?
C102 H31 0.9500 . ?
C103 C104 1.364(12) . ?
C103 C131 1.521(10) . ?
C104 C105 1.392(11) . ?
C104 H32 0.9500 . ?
C105 C106 1.406(11) . ?
C105 C151 1.503(12) . ?
C106 H33 0.9500 . ?
C111 H34 0.9900 . ?
C111 H35 0.9900 . ?
C112 H36 0.9500 . ?
C113 C114 1.356(10) . ?
C113 H37 0.9500 . ?
C114 H38 0.9500 . ?
C131 N131 1.473(10) 1_455 ?
C131 H39 0.9900 . ?
C131 H40 0.9900 . ?
C132 H41 0.9500 . ?
C133 C134 1.352(12) . ?
C133 H42 0.9500 . ?
C134 H43 0.9500 . ?
C151 H44 0.9800 . ?
C151 H45 0.9800 . ?
C151 H46 0.9800 . ?

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
N32 Pb1 N12 83.4(2) . . ?
N32 Pb1 O22 76.4(2) . . ?
N12 Pb1 O22 84.8(2) . . ?
N32 Pb1 O42 84.6(2) . 2_677 ?
N12 Pb1 O42 72.9(2) . 2_677 ?
O22 Pb1 O42 152.26(19) . 2_677 ?
N32 Pb1 O71 79.3(2) . . ?
N12 Pb1 O71 155.8(2) . . ?
O22 Pb1 O71 74.8(2) . . ?
O42 Pb1 O71 121.6(2) 2_677 . ?
N32 Pb1 O43 77.9(2) . 2_677 ?
N12 Pb1 O43 118.3(2) . 2_677 ?
O22 Pb1 O43 142.88(17) . 2_677 ?
O42 Pb1 O43 47.34(18) 2_677 2_677 ?
O71 Pb1 O43 74.4(2) . 2_677 ?
N112 Pb2 O31 74.1(3) . . ?
N112 Pb2 N132 81.4(2) . . ?
O31 Pb2 N132 87.3(3) . . ?
N112 Pb2 O81 81.0(2) . . ?
O31 Pb2 O81 75.0(3) . . ?
N132 Pb2 O81 157.9(2) . . ?
N112 Pb2 O11 76.4(3) . 2_767 ?
O31 Pb2 O11 141.2(2) . 2_767 ?
N132 Pb2 O11 112.5(3) . 2_767 ?
O81 Pb2 O11 76.0(3) . 2_767 ?
N1 O11 Pb2 101.8(6) . 2_767 ?
N2 O22 Pb1 99.1(4) . . ?
N3 O31 Pb2 104.9(5) . . ?
N4 O42 Pb1 96.5(4) . 2_677 ?
N4 O43 Pb1 94.9(4) . 2_677 ?
C71 O71 Pb1 125.0(6) . . ?
C81 O81 Pb2 121.0(6) . . ?
O13 N1 O12 119.9(10) . . ?
O13 N1 O11 120.3(11) . . ?
O12 N1 O11 119.9(9) . . ?
O23 N2 O22 119.9(6) . . ?
O23 N2 O21 120.4(6) . . ?
O22 N2 O21 119.7(6) . . ?
O33 N3 O31 122.0(7) . . ?
O33 N3 O32 120.0(7) . . ?
O31 N3 O32 117.9(8) . . ?
O42 N4 O41 121.9(6) . . ?
O42 N4 O43 118.5(6) . . ?
O41 N4 O43 119.7(6) . . ?
C71 N7 C73 122.0(9) . . ?
C71 N7 C72 120.3(8) . . ?
C73 N7 C72 117.7(8) . . ?
C81 N8 C82 121.3(7) . . ?
C81 N8 C83 121.2(8) . . ?
C82 N8 C83 117.6(7) . . ?
C12 N11 C14 105.7(6) . . ?
C12 N11 C11 127.1(6) . . ?
C14 N11 C11 127.2(6) . . ?
C12 N12 C13 106.5(6) . . ?
C12 N12 Pb1 124.4(5) . . ?
C13 N12 Pb1 128.9(5) . . ?
C32 N31 C34 107.5(6) . . ?
C32 N31 C31 125.9(6) . 1_455 ?
C34 N31 C31 126.6(6) . 1_455 ?
C32 N32 C33 105.2(5) . . ?
C32 N32 Pb1 128.8(4) . . ?
C33 N32 Pb1 125.6(4) . . ?
C112 N111 C114 107.5(6) . . ?
C112 N111 C111 125.7(6) . . ?
C114 N111 C111 126.8(6) . . ?
C112 N112 C113 105.6(6) . . ?
C112 N112 Pb2 126.1(5) . . ?
C113 N112 Pb2 128.2(5) . . ?
C132 N131 C134 106.3(7) . . ?
C132 N131 C131 126.6(8) . 1_655 ?
C134 N131 C131 127.1(7) . 1_655 ?
C132 N132 C133 104.6(7) . . ?
C132 N132 Pb2 125.5(6) . . ?
C133 N132 Pb2 129.9(6) . . ?
C2 C1 C6 119.0(6) . . ?
C2 C1 C11 120.2(7) . . ?
C6 C1 C11 120.8(6) . . ?
C1 C2 C3 121.0(7) . . ?
C1 C2 H1 119.5 . . ?
C3 C2 H1 119.5 . . ?
C4 C3 C2 118.9(6) . . ?
C4 C3 C31 121.3(6) . . ?
C2 C3 C31 119.8(7) . . ?
C3 C4 C5 121.9(6) . . ?
C3 C4 H2 119.0 . . ?
C5 C4 H2 119.0 . . ?
C6 C5 C4 117.4(7) . . ?
C6 C5 C51 121.6(7) . . ?
C4 C5 C51 121.0(7) . . ?
C1 C6 C5 121.7(6) . . ?
C1 C6 H3 119.2 . . ?
C5 C6 H3 119.2 . . ?
N11 C11 C1 112.6(6) . . ?
N11 C11 H4 109.1 . . ?
C1 C11 H4 109.1 . . ?
N11 C11 H5 109.1 . . ?
C1 C11 H5 109.1 . . ?
H4 C11 H5 107.8 . . ?
N12 C12 N11 111.1(7) . . ?
N12 C12 H6 124.4 . . ?
N11 C12 H6 124.4 . . ?
C14 C13 N12 108.7(7) . . ?
C14 C13 H7 125.7 . . ?
N12 C13 H7 125.7 . . ?
C13 C14 N11 108.0(7) . . ?
C13 C14 H8 126.0 . . ?
N11 C14 H8 126.0 . . ?
N31 C31 C3 112.5(5) 1_655 . ?
N31 C31 H9 109.1 1_655 . ?
C3 C31 H9 109.1 . . ?
N31 C31 H10 109.1 1_655 . ?
C3 C31 H10 109.1 . . ?
H9 C31 H10 107.8 . . ?
N32 C32 N31 111.3(6) . . ?
N32 C32 H11 124.4 . . ?
N31 C32 H11 124.4 . . ?
C34 C33 N32 109.6(6) . . ?
C34 C33 H12 125.2 . . ?
N32 C33 H12 125.2 . . ?
C33 C34 N31 106.4(6) . . ?
C33 C34 H13 126.8 . . ?
N31 C34 H13 126.8 . . ?
C5 C51 H14 109.5 . . ?
C5 C51 H15 109.5 . . ?
H14 C51 H15 109.5 . . ?
C5 C51 H16 109.5 . . ?
H14 C51 H16 109.5 . . ?
H15 C51 H16 109.5 . . ?
O71 C71 N7 124.4(9) . . ?
O71 C71 H17 117.8 . . ?
N7 C71 H17 117.8 . . ?
N7 C72 H18 109.5 . . ?
N7 C72 H19 109.5 . . ?
H18 C72 H19 109.5 . . ?
N7 C72 H20 109.5 . . ?
H18 C72 H20 109.5 . . ?
H19 C72 H20 109.5 . . ?
N7 C73 H21 109.5 . . ?
N7 C73 H22 109.5 . . ?
H21 C73 H22 109.5 . . ?
N7 C73 H23 109.5 . . ?
H21 C73 H23 109.5 . . ?
H22 C73 H23 109.5 . . ?
O81 C81 N8 124.0(9) . . ?
O81 C81 H24 118.0 . . ?
N8 C81 H24 118.0 . . ?
N8 C82 H25 109.5 . . ?
N8 C82 H26 109.5 . . ?
H25 C82 H26 109.5 . . ?
N8 C82 H27 109.5 . . ?
H25 C82 H27 109.5 . . ?
H26 C82 H27 109.5 . . ?
N8 C83 H28 109.5 . . ?
N8 C83 H29 109.5 . . ?
H28 C83 H29 109.5 . . ?
N8 C83 H30 109.5 . . ?
H28 C83 H30 109.5 . . ?
H29 C83 H30 109.5 . . ?
C106 C101 C102 118.9(7) . . ?
C106 C101 C111 120.8(6) . . ?
C102 C101 C111 120.4(7) . . ?
C103 C102 C101 119.7(8) . . ?
C103 C102 H31 120.2 . . ?
C101 C102 H31 120.2 . . ?
C104 C103 C102 120.0(7) . . ?
C104 C103 C131 121.4(7) . . ?
C102 C103 C131 118.6(8) . . ?
C103 C104 C105 122.5(7) . . ?
C103 C104 H32 118.8 . . ?
C105 C104 H32 118.8 . . ?
C104 C105 C106 116.8(8) . . ?
C104 C105 C151 121.9(8) . . ?
C106 C105 C151 121.3(8) . . ?
C101 C106 C105 122.2(7) . . ?
C101 C106 H33 118.9 . . ?
C105 C106 H33 118.9 . . ?
N111 C111 C101 111.2(5) . . ?
N111 C111 H34 109.4 . . ?
C101 C111 H34 109.4 . . ?
N111 C111 H35 109.4 . . ?
C101 C111 H35 109.4 . . ?
H34 C111 H35 108.0 . . ?
N112 C112 N111 110.9(7) . . ?
N112 C112 H36 124.6 . . ?
N111 C112 H36 124.6 . . ?
C114 C113 N112 110.5(7) . . ?
C114 C113 H37 124.7 . . ?
N112 C113 H37 124.7 . . ?
C113 C114 N111 105.5(6) . . ?
C113 C114 H38 127.3 . . ?
N111 C114 H38 127.3 . . ?
N131 C131 C103 112.7(6) 1_455 . ?
N131 C131 H39 109.1 1_455 . ?
C103 C131 H39 109.1 . . ?
N131 C131 H40 109.1 1_455 . ?
C103 C131 H40 109.1 . . ?
H39 C131 H40 107.8 . . ?
N132 C132 N131 113.1(8) . . ?
N132 C132 H41 123.5 . . ?
N131 C132 H41 123.5 . . ?
C134 C133 N132 108.4(8) . . ?
C134 C133 H42 125.8 . . ?
N132 C133 H42 125.8 . . ?
N131 C134 C133 107.7(8) . . ?
N131 C134 H43 126.2 . . ?
C133 C134 H43 126.2 . . ?
C105 C151 H44 109.5 . . ?
C105 C151 H45 109.5 . . ?
H44 C151 H45 109.5 . . ?
C105 C151 H46 109.5 . . ?
H44 C151 H46 109.5 . . ?
H45 C151 H46 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N32 Pb1 O22 N2 174.1(5) . . . . ?
N12 Pb1 O22 N2 89.6(4) . . . . ?
O42 Pb1 O22 N2 125.9(5) 2_677 . . . ?
O71 Pb1 O22 N2 -103.5(5) . . . . ?
O43 Pb1 O22 N2 -138.4(4) 2_677 . . . ?
N112 Pb2 O31 N3 -161.1(5) . . . . ?
N132 Pb2 O31 N3 -79.3(5) . . . . ?
O81 Pb2 O31 N3 114.1(5) . . . . ?
O11 Pb2 O31 N3 157.1(4) 2_767 . . . ?
N32 Pb1 O71 C71 -78.4(7) . . . . ?
N12 Pb1 O71 C71 -123.6(7) . . . . ?
O22 Pb1 O71 C71 -157.1(7) . . . . ?
O42 Pb1 O71 C71 -1.6(8) 2_677 . . . ?
O43 Pb1 O71 C71 1.9(7) 2_677 . . . ?
N112 Pb2 O81 C81 106.0(6) . . . . ?
O31 Pb2 O81 C81 -178.2(6) . . . . ?
N132 Pb2 O81 C81 143.6(6) . . . . ?
O11 Pb2 O81 C81 27.9(6) 2_767 . . . ?
Pb2 O11 N1 O13 -150.5(7) 2_767 . . . ?
Pb2 O11 N1 O12 29.0(9) 2_767 . . . ?
Pb1 O22 N2 O23 154.3(6) . . . . ?
Pb1 O22 N2 O21 -26.6(7) . . . . ?
Pb2 O31 N3 O33 -163.2(6) . . . . ?
Pb2 O31 N3 O32 13.8(8) . . . . ?
Pb1 O42 N4 O41 -161.9(5) 2_677 . . . ?
Pb1 O42 N4 O43 16.9(6) 2_677 . . . ?
Pb1 O43 N4 O42 -16.7(6) 2_677 . . . ?
Pb1 O43 N4 O41 162.1(5) 2_677 . . . ?
N32 Pb1 N12 C12 61.8(6) . . . . ?
O22 Pb1 N12 C12 138.7(6) . . . . ?
O42 Pb1 N12 C12 -24.6(5) 2_677 . . . ?
O71 Pb1 N12 C12 106.4(7) . . . . ?
O43 Pb1 N12 C12 -10.7(6) 2_677 . . . ?
N32 Pb1 N12 C13 -111.3(6) . . . . ?
O22 Pb1 N12 C13 -34.5(6) . . . . ?
O42 Pb1 N12 C13 162.3(6) 2_677 . . . ?
O71 Pb1 N12 C13 -66.8(8) . . . . ?
O43 Pb1 N12 C13 176.2(6) 2_677 . . . ?
N12 Pb1 N32 C32 -65.7(5) . . . . ?
O22 Pb1 N32 C32 -151.9(5) . . . . ?
O42 Pb1 N32 C32 7.7(5) 2_677 . . . ?
O71 Pb1 N32 C32 131.3(5) . . . . ?
O43 Pb1 N32 C32 55.1(5) 2_677 . . . ?
N12 Pb1 N32 C33 106.1(5) . . . . ?
O22 Pb1 N32 C33 19.9(5) . . . . ?
O42 Pb1 N32 C33 179.5(5) 2_677 . . . ?
O71 Pb1 N32 C33 -56.8(5) . . . . ?
O43 Pb1 N32 C33 -133.0(5) 2_677 . . . ?
O31 Pb2 N112 C112 27.0(6) . . . . ?
N132 Pb2 N112 C112 -62.7(6) . . . . ?
O81 Pb2 N112 C112 103.9(6) . . . . ?
O11 Pb2 N112 C112 -178.5(6) 2_767 . . . ?
O31 Pb2 N112 C113 -156.3(6) . . . . ?
N132 Pb2 N112 C113 114.0(6) . . . . ?
O81 Pb2 N112 C113 -79.5(6) . . . . ?
O11 Pb2 N112 C113 -1.8(6) 2_767 . . . ?
N112 Pb2 N132 C132 71.3(6) . . . . ?
O31 Pb2 N132 C132 -3.0(6) . . . . ?
O81 Pb2 N132 C132 33.7(10) . . . . ?
O11 Pb2 N132 C132 142.6(6) 2_767 . . . ?
N112 Pb2 N132 C133 -105.4(7) . . . . ?
O31 Pb2 N132 C133 -179.7(7) . . . . ?
O81 Pb2 N132 C133 -143.0(7) . . . . ?
O11 Pb2 N132 C133 -34.2(7) 2_767 . . . ?
C6 C1 C2 C3 1.0(9) . . . . ?
C11 C1 C2 C3 -177.7(6) . . . . ?
C1 C2 C3 C4 -2.3(9) . . . . ?
C1 C2 C3 C31 177.6(6) . . . . ?
C2 C3 C4 C5 1.5(10) . . . . ?
C31 C3 C4 C5 -178.3(6) . . . . ?
C3 C4 C5 C6 0.5(10) . . . . ?
C3 C4 C5 C51 179.5(7) . . . . ?
C2 C1 C6 C5 1.2(10) . . . . ?
C11 C1 C6 C5 179.8(6) . . . . ?
C4 C5 C6 C1 -1.9(10) . . . . ?
C51 C5 C6 C1 179.1(7) . . . . ?
C12 N11 C11 C1 93.4(8) . . . . ?
C14 N11 C11 C1 -87.4(9) . . . . ?
C2 C1 C11 N11 87.8(8) . . . . ?
C6 C1 C11 N11 -90.8(8) . . . . ?
C13 N12 C12 N11 1.0(8) . . . . ?
Pb1 N12 C12 N11 -173.4(4) . . . . ?
C14 N11 C12 N12 -0.7(8) . . . . ?
C11 N11 C12 N12 178.6(6) . . . . ?
C12 N12 C13 C14 -0.9(9) . . . . ?
Pb1 N12 C13 C14 173.2(5) . . . . ?
N12 C13 C14 N11 0.5(9) . . . . ?
C12 N11 C14 C13 0.1(9) . . . . ?
C11 N11 C14 C13 -179.2(6) . . . . ?
C4 C3 C31 N31 95.2(8) . . . 1_655 ?
C2 C3 C31 N31 -84.6(8) . . . 1_655 ?
C33 N32 C32 N31 -0.8(7) . . . . ?
Pb1 N32 C32 N31 172.4(4) . . . . ?
C34 N31 C32 N32 0.5(7) . . . . ?
C31 N31 C32 N32 -178.7(5) 1_455 . . . ?
C32 N32 C33 C34 0.7(7) . . . . ?
Pb1 N32 C33 C34 -172.7(4) . . . . ?
N32 C33 C34 N31 -0.4(7) . . . . ?
C32 N31 C34 C33 -0.1(7) . . . . ?
C31 N31 C34 C33 179.2(5) 1_455 . . . ?
Pb1 O71 C71 N7 -162.5(6) . . . . ?
C73 N7 C71 O71 -179.3(9) . . . . ?
C72 N7 C71 O71 2.4(14) . . . . ?
Pb2 O81 C81 N8 179.4(6) . . . . ?
C82 N8 C81 O81 0.1(13) . . . . ?
C83 N8 C81 O81 -179.7(9) . . . . ?
C106 C101 C102 C103 -2.7(10) . . . . ?
C111 C101 C102 C103 178.7(6) . . . . ?
C101 C102 C103 C104 2.3(10) . . . . ?
C101 C102 C103 C131 -179.2(6) . . . . ?
C102 C103 C104 C105 0.6(11) . . . . ?
C131 C103 C104 C105 -178.0(7) . . . . ?
C103 C104 C105 C106 -2.8(11) . . . . ?
C103 C104 C105 C151 179.4(7) . . . . ?
C102 C101 C106 C105 0.4(10) . . . . ?
C111 C101 C106 C105 179.0(6) . . . . ?
C104 C105 C106 C101 2.3(11) . . . . ?
C151 C105 C106 C101 -179.9(7) . . . . ?
C112 N111 C111 C101 -98.5(7) . . . . ?
C114 N111 C111 C101 81.9(9) . . . . ?
C106 C101 C111 N111 93.2(8) . . . . ?
C102 C101 C111 N111 -88.2(8) . . . . ?
C113 N112 C112 N111 -0.6(8) . . . . ?
Pb2 N112 C112 N111 176.7(4) . . . . ?
C114 N111 C112 N112 1.6(8) . . . . ?
C111 N111 C112 N112 -178.1(6) . . . . ?
C112 N112 C113 C114 -0.6(8) . . . . ?
Pb2 N112 C113 C114 -177.8(5) . . . . ?
N112 C113 C114 N111 1.5(8) . . . . ?
C112 N111 C114 C113 -1.8(8) . . . . ?
C111 N111 C114 C113 177.9(6) . . . . ?
C104 C103 C131 N131 -99.6(9) . . . 1_455 ?
C102 C103 C131 N131 81.8(9) . . . 1_455 ?
C133 N132 C132 N131 2.7(9) . . . . ?
Pb2 N132 C132 N131 -174.7(4) . . . . ?
C134 N131 C132 N132 -2.6(9) . . . . ?
C131 N131 C132 N132 177.7(7) 1_655 . . . ?
C132 N132 C133 C134 -1.7(10) . . . . ?
Pb2 N132 C133 C134 175.5(6) . . . . ?
C132 N131 C134 C133 1.3(10) . . . . ?
C131 N131 C134 C133 -179.0(7) 1_655 . . . ?
N132 C133 C134 N131 0.2(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.953
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.953
_refine_diff_density_max         2.855
_refine_diff_density_min         -1.545
_refine_diff_density_rms         0.143

#====END

data_2
_database_code_depnum_ccdc_archive 'CCDC 227128'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
[Pb(dimb)(SCN)2]
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H32 N12 O0 Pb2 S4'
_chemical_formula_sum            'C34 H32 N12 O0 Pb2 S4'
_chemical_formula_weight         1151.34

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 1 21/c 1'

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                   11.968(2)
_cell_length_b                   10.0376(18)
_cell_length_c                   16.579(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.804(3)
_cell_angle_gamma                90.00
_cell_volume                     1989.3(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    777
_cell_measurement_theta_min      2.373
_cell_measurement_theta_max      20.110

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_absorpt_coefficient_mu    8.704
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.436
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_process_details   'SADABS (BRUKER 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11717
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         28.05
_reflns_number_total             4671
_reflns_number_gt                2496
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4671
_refine_ls_number_parameters     235
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.0909
_refine_ls_wR_factor_gt          0.0836
_refine_ls_goodness_of_fit_ref   0.847
_refine_ls_restrained_S_all      0.848
_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
Pb1 Pb 0.56716(2) 0.42641(3) -0.123084(16) 0.06645(13) Uani 1 1 d . . .
S1 S 0.34106(19) 0.2004(2) -0.32676(15) 0.0939(7) Uani 1 1 d . . .
S2 S 0.7354(3) 0.5401(4) 0.1617(2) 0.1737(15) Uani 1 1 d . . .
N11 N 0.6399(4) 0.0580(6) 0.0303(4) 0.0632(16) Uani 1 1 d . . .
N31 N 0.9055(5) 0.2834(6) -0.1968(3) 0.0611(15) Uani 1 1 d . . .
N12 N 0.5863(5) 0.2023(7) -0.0610(4) 0.0687(17) Uani 1 1 d . . .
N32 N 0.7580(5) 0.3780(6) -0.1501(4) 0.0643(16) Uani 1 1 d . . .
N1 N 0.5375(6) 0.2930(7) -0.2550(4) 0.0853(16) Uani 1 1 d U . .
N2 N 0.6608(7) 0.5281(12) 0.0179(5) 0.146(3) Uani 1 1 d U . .
C13 C 0.6058(6) 0.0858(9) -0.0967(5) 0.066(2) Uani 1 1 d . . .
H13A H 0.5959 0.0697 -0.1518 0.079 Uiso 1 1 calc R . .
C5 C 0.9868(6) 0.0974(6) 0.0923(4) 0.0509(17) Uani 1 1 d . . .
C33 C 0.8520(6) 0.4333(7) -0.1121(5) 0.069(2) Uani 1 1 d . . .
H33A H 0.8522 0.4998 -0.0730 0.083 Uiso 1 1 calc R . .
C4 C 1.0363(6) 0.0049(7) 0.1446(4) 0.0548(17) Uani 1 1 d . . .
H4A H 1.1136 0.0042 0.1535 0.066 Uiso 1 1 calc R . .
C2 C 0.8587(6) -0.0874(7) 0.1702(4) 0.0571(18) Uani 1 1 d . . .
H2A H 0.8158 -0.1507 0.1956 0.069 Uiso 1 1 calc R . .
C1 C 0.8069(6) 0.0053(7) 0.1192(4) 0.0550(17) Uani 1 1 d . . .
C6 C 0.8727(6) 0.0959(6) 0.0809(4) 0.0543(18) Uani 1 1 d . . .
H6A H 0.8385 0.1581 0.0462 0.065 Uiso 1 1 calc R . .
C32 C 0.7939(6) 0.2895(7) -0.1997(4) 0.066(2) Uani 1 1 d . . .
H32A H 0.7476 0.2367 -0.2332 0.079 Uiso 1 1 calc R . .
C3 C 0.9713(6) -0.0869(7) 0.1837(4) 0.0556(17) Uani 1 1 d . . .
C11 C 0.6814(6) 0.0013(8) 0.1081(4) 0.072(2) Uani 1 1 d . . .
H11A H 0.6564 -0.0903 0.1116 0.086 Uiso 1 1 calc R . .
H11B H 0.6493 0.0506 0.1517 0.086 Uiso 1 1 calc R . .
C34 C 0.9429(7) 0.3755(8) -0.1408(5) 0.071(2) Uani 1 1 d . . .
H34A H 1.0171 0.3943 -0.1255 0.085 Uiso 1 1 calc R . .
C14 C 0.6414(6) -0.0035(8) -0.0425(6) 0.073(2) Uani 1 1 d . . .
H14A H 0.6630 -0.0907 -0.0523 0.088 Uiso 1 1 calc R . .
C12 C 0.6053(6) 0.1804(8) 0.0160(5) 0.069(2) Uani 1 1 d . . .
H12A H 0.5956 0.2438 0.0559 0.082 Uiso 1 1 calc R . .
C31 C 0.9738(6) 0.1899(7) -0.2395(4) 0.069(2) Uani 1 1 d . . .
H31A H 1.0314 0.2385 -0.2664 0.083 Uiso 1 1 calc R . .
H31B H 0.9274 0.1448 -0.2807 0.083 Uiso 1 1 calc R . .
C51 C 1.0568(6) 0.1974(7) 0.0502(4) 0.0651(19) Uani 1 1 d . . .
H51A H 1.0091 0.2542 0.0170 0.098 Uiso 1 1 calc R . .
H51B H 1.1080 0.1517 0.0170 0.098 Uiso 1 1 calc R . .
H51C H 1.0980 0.2504 0.0896 0.098 Uiso 1 1 calc R . .
C71 C 0.4555(7) 0.2536(9) -0.2838(5) 0.0812(17) Uani 1 1 d U . .
C91 C 0.6958(9) 0.5105(16) 0.0738(7) 0.144(3) Uani 1 1 d U . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.05204(19) 0.0786(2) 0.0690(2) 0.00023(17) 0.00548(13) 0.01209(16)
S1 0.0724(16) 0.0917(16) 0.1169(18) -0.0088(14) -0.0024(13) -0.0149(12)
S2 0.118(3) 0.254(5) 0.147(3) -0.021(3) -0.018(2) -0.024(3)
N11 0.034(3) 0.075(5) 0.081(5) 0.018(4) 0.002(3) 0.007(3)
N31 0.053(4) 0.063(4) 0.067(4) 0.017(3) 0.009(3) 0.014(3)
N12 0.062(4) 0.078(5) 0.067(4) 0.008(4) 0.006(3) -0.002(3)
N32 0.045(4) 0.070(4) 0.078(4) 0.002(3) 0.008(3) 0.007(3)
N1 0.074(5) 0.103(4) 0.079(4) -0.003(3) 0.001(3) 0.002(4)
N2 0.066(5) 0.288(8) 0.084(6) 0.055(7) 0.017(4) 0.029(5)
C13 0.050(5) 0.081(6) 0.067(5) -0.012(5) -0.002(4) -0.003(4)
C5 0.047(4) 0.054(4) 0.052(4) -0.004(3) 0.011(3) 0.000(3)
C33 0.051(5) 0.061(5) 0.095(6) 0.002(4) 0.002(4) -0.005(4)
C4 0.041(4) 0.072(5) 0.052(4) -0.006(4) 0.008(3) 0.000(4)
C2 0.048(4) 0.069(5) 0.056(4) 0.013(4) 0.019(3) 0.005(4)
C1 0.048(5) 0.056(4) 0.061(4) 0.005(4) 0.009(3) 0.005(3)
C6 0.053(5) 0.053(5) 0.057(4) 0.006(3) 0.004(3) 0.008(3)
C32 0.050(5) 0.076(5) 0.072(5) 0.007(4) 0.006(4) 0.010(4)
C3 0.051(5) 0.071(5) 0.046(4) -0.001(4) 0.011(3) 0.008(4)
C11 0.045(5) 0.097(6) 0.074(5) 0.013(5) 0.009(4) -0.002(4)
C34 0.049(5) 0.077(5) 0.086(6) 0.012(5) -0.002(4) -0.006(4)
C14 0.054(5) 0.067(5) 0.099(7) -0.009(6) 0.011(5) -0.006(4)
C12 0.053(5) 0.080(6) 0.075(6) -0.002(5) 0.017(4) 0.009(4)
C31 0.060(5) 0.091(6) 0.057(4) 0.019(4) 0.018(4) 0.015(4)
C51 0.060(5) 0.067(5) 0.068(5) 0.004(4) 0.005(4) -0.003(4)
C71 0.070(5) 0.098(4) 0.075(4) -0.003(3) 0.002(3) 0.000(4)
C91 0.065(5) 0.285(8) 0.084(6) 0.052(7) 0.017(5) 0.029(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N32 2.399(6) . ?
Pb1 N12 2.480(6) . ?
Pb1 N1 2.575(7) . ?
Pb1 N2 2.740(10) . ?
Pb1 S1 3.090(2) 2_654 ?
S1 C71 1.605(9) . ?
S1 Pb1 3.090(2) 2_644 ?
S2 C91 1.540(13) . ?
N11 C12 1.314(8) . ?
N11 C14 1.356(9) . ?
N11 C11 1.473(8) . ?
N31 C32 1.336(8) . ?
N31 C34 1.370(9) . ?
N31 C31 1.452(8) . ?
N12 C12 1.305(8) . ?
N12 C13 1.336(8) . ?
N32 C32 1.299(8) . ?
N32 C33 1.378(9) . ?
N1 C71 1.140(9) . ?
N2 C91 1.013(10) . ?
C13 C14 1.325(10) . ?
C13 H13A 0.9300 . ?
C5 C6 1.369(9) . ?
C5 C4 1.384(9) . ?
C5 C51 1.501(8) . ?
C33 C34 1.341(10) . ?
C33 H33A 0.9300 . ?
C4 C3 1.386(9) . ?
C4 H4A 0.9300 . ?
C2 C3 1.356(9) . ?
C2 C1 1.384(9) . ?
C2 H2A 0.9300 . ?
C1 C6 1.378(8) . ?
C1 C11 1.505(9) . ?
C6 H6A 0.9300 . ?
C32 H32A 0.9300 . ?
C3 C31 1.515(8) 3_755 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C34 H34A 0.9300 . ?
C14 H14A 0.9300 . ?
C12 H12A 0.9300 . ?
C31 C3 1.515(8) 3_755 ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?

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
N32 Pb1 N12 79.89(19) . . ?
N32 Pb1 N1 80.2(2) . . ?
N12 Pb1 N1 83.5(2) . . ?
N32 Pb1 N2 83.2(2) . . ?
N12 Pb1 N2 87.6(3) . . ?
N1 Pb1 N2 162.3(2) . . ?
N32 Pb1 S1 77.04(15) . 2_654 ?
N12 Pb1 S1 153.15(14) . 2_654 ?
N1 Pb1 S1 105.67(16) . 2_654 ?
N2 Pb1 S1 76.2(2) . 2_654 ?
C71 S1 Pb1 96.2(3) . 2_644 ?
C12 N11 C14 106.4(7) . . ?
C12 N11 C11 127.5(7) . . ?
C14 N11 C11 125.8(7) . . ?
C32 N31 C34 106.7(6) . . ?
C32 N31 C31 126.7(7) . . ?
C34 N31 C31 126.4(7) . . ?
C12 N12 C13 105.1(7) . . ?
C12 N12 Pb1 124.6(6) . . ?
C13 N12 Pb1 128.7(5) . . ?
C32 N32 C33 106.1(6) . . ?
C32 N32 Pb1 127.1(5) . . ?
C33 N32 Pb1 126.6(5) . . ?
C71 N1 Pb1 128.0(7) . . ?
C91 N2 Pb1 148.0(15) . . ?
C14 C13 N12 110.4(7) . . ?
C14 C13 H13A 124.8 . . ?
N12 C13 H13A 124.8 . . ?
C6 C5 C4 118.2(6) . . ?
C6 C5 C51 121.2(6) . . ?
C4 C5 C51 120.6(6) . . ?
C34 C33 N32 108.8(7) . . ?
C34 C33 H33A 125.6 . . ?
N32 C33 H33A 125.6 . . ?
C5 C4 C3 120.4(6) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C3 C2 C1 120.7(6) . . ?
C3 C2 H2A 119.7 . . ?
C1 C2 H2A 119.7 . . ?
C6 C1 C2 118.5(6) . . ?
C6 C1 C11 123.4(6) . . ?
C2 C1 C11 118.1(6) . . ?
C5 C6 C1 122.2(6) . . ?
C5 C6 H6A 118.9 . . ?
C1 C6 H6A 118.9 . . ?
N32 C32 N31 111.7(7) . . ?
N32 C32 H32A 124.2 . . ?
N31 C32 H32A 124.2 . . ?
C2 C3 C4 120.1(6) . . ?
C2 C3 C31 119.7(6) . 3_755 ?
C4 C3 C31 120.2(6) . 3_755 ?
N11 C11 C1 112.8(5) . . ?
N11 C11 H11A 109.0 . . ?
C1 C11 H11A 109.0 . . ?
N11 C11 H11B 109.0 . . ?
C1 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C33 C34 N31 106.7(7) . . ?
C33 C34 H34A 126.6 . . ?
N31 C34 H34A 126.6 . . ?
C13 C14 N11 106.2(7) . . ?
C13 C14 H14A 126.9 . . ?
N11 C14 H14A 126.9 . . ?
N12 C12 N11 111.9(7) . . ?
N12 C12 H12A 124.0 . . ?
N11 C12 H12A 124.0 . . ?
N31 C31 C3 112.4(5) . 3_755 ?
N31 C31 H31A 109.1 . . ?
C3 C31 H31A 109.1 3_755 . ?
N31 C31 H31B 109.1 . . ?
C3 C31 H31B 109.1 3_755 . ?
H31A C31 H31B 107.9 . . ?
C5 C51 H51A 109.5 . . ?
C5 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C5 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N1 C71 S1 178.2(9) . . ?
N2 C91 S2 157.8(18) . . ?

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
N32 Pb1 N12 C12 98.9(6) . . . . ?
N1 Pb1 N12 C12 -180.0(6) . . . . ?
N2 Pb1 N12 C12 15.4(6) . . . . ?
S1 Pb1 N12 C12 67.9(7) 2_654 . . . ?
N32 Pb1 N12 C13 -63.8(6) . . . . ?
N1 Pb1 N12 C13 17.3(6) . . . . ?
N2 Pb1 N12 C13 -147.3(6) . . . . ?
S1 Pb1 N12 C13 -94.9(7) 2_654 . . . ?
N12 Pb1 N32 C32 69.2(6) . . . . ?
N1 Pb1 N32 C32 -15.9(6) . . . . ?
N2 Pb1 N32 C32 158.0(6) . . . . ?
S1 Pb1 N32 C32 -124.6(6) 2_654 . . . ?
N12 Pb1 N32 C33 -106.5(6) . . . . ?
N1 Pb1 N32 C33 168.5(6) . . . . ?
N2 Pb1 N32 C33 -17.7(6) . . . . ?
S1 Pb1 N32 C33 59.7(5) 2_654 . . . ?
N32 Pb1 N1 C71 169.9(9) . . . . ?
N12 Pb1 N1 C71 89.1(9) . . . . ?
N2 Pb1 N1 C71 149.5(9) . . . . ?
S1 Pb1 N1 C71 -116.6(8) 2_654 . . . ?
N32 Pb1 N2 C91 -76.9(17) . . . . ?
N12 Pb1 N2 C91 3.2(17) . . . . ?
N1 Pb1 N2 C91 -57(2) . . . . ?
S1 Pb1 N2 C91 -155.1(18) 2_654 . . . ?
C12 N12 C13 C14 -3.0(8) . . . . ?
Pb1 N12 C13 C14 162.4(5) . . . . ?
C32 N32 C33 C34 0.2(8) . . . . ?
Pb1 N32 C33 C34 176.6(5) . . . . ?
C6 C5 C4 C3 0.4(9) . . . . ?
C51 C5 C4 C3 179.7(6) . . . . ?
C3 C2 C1 C6 1.5(10) . . . . ?
C3 C2 C1 C11 -178.7(6) . . . . ?
C4 C5 C6 C1 -0.5(9) . . . . ?
C51 C5 C6 C1 -179.8(6) . . . . ?
C2 C1 C6 C5 -0.4(10) . . . . ?
C11 C1 C6 C5 179.8(6) . . . . ?
C33 N32 C32 N31 -0.2(8) . . . . ?
Pb1 N32 C32 N31 -176.5(4) . . . . ?
C34 N31 C32 N32 0.1(8) . . . . ?
C31 N31 C32 N32 175.3(6) . . . . ?
C1 C2 C3 C4 -1.6(10) . . . . ?
C1 C2 C3 C31 -179.7(6) . . . 3_755 ?
C5 C4 C3 C2 0.7(10) . . . . ?
C5 C4 C3 C31 178.7(6) . . . 3_755 ?
C12 N11 C11 C1 -95.1(8) . . . . ?
C14 N11 C11 C1 77.4(9) . . . . ?
C6 C1 C11 N11 25.3(10) . . . . ?
C2 C1 C11 N11 -154.5(6) . . . . ?
N32 C33 C34 N31 -0.1(8) . . . . ?
C32 N31 C34 C33 0.0(8) . . . . ?
C31 N31 C34 C33 -175.2(6) . . . . ?
N12 C13 C14 N11 2.4(8) . . . . ?
C12 N11 C14 C13 -0.9(8) . . . . ?
C11 N11 C14 C13 -174.6(6) . . . . ?
C13 N12 C12 N11 2.4(8) . . . . ?
Pb1 N12 C12 N11 -163.7(4) . . . . ?
C14 N11 C12 N12 -1.0(8) . . . . ?
C11 N11 C12 N12 172.6(6) . . . . ?
C32 N31 C31 C3 -107.9(7) . . . 3_755 ?
C34 N31 C31 C3 66.4(9) . . . 3_755 ?
Pb1 N1 C71 S1 126(29) . . . . ?
Pb1 S1 C71 N1 95(29) 2_644 . . . ?
Pb1 N2 C91 S2 -160(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        28.05
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         1.179
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.110

#====END

data_3
_database_code_depnum_ccdc_archive 'CCDC 227129'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H27 N8 O6 Pb, C3 H7 N O'
_chemical_formula_sum            'C33 H34 N9 O7 Pb'
_chemical_formula_weight         875.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1 '
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.236(1)
_cell_length_b                   11.672(2)
_cell_length_c                   15.299(2)
_cell_angle_alpha                73.50(1)
_cell_angle_beta                 86.58(1)
_cell_angle_gamma                81.92(1)
_cell_volume                     1734.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    784
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      18.14

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             866
_exptl_absorpt_coefficient_mu    4.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_T_max  0.38
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9453
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6667
_reflns_number_gt                5037
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+1.5500P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6667
_refine_ls_number_parameters     451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1489
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
Pb1 Pb 0.59309(3) 0.18571(3) 0.97736(2) 0.05322(15) Uani 1 1 d . . .
N1 N 0.5895(7) 0.3536(7) 0.8379(5) 0.0557(19) Uani 1 1 d . . .
N2 N 0.4910(7) 0.5016(7) 0.7270(5) 0.0539(18) Uani 1 1 d . . .
N3 N 0.3485(7) 0.2912(7) 1.0080(5) 0.0573(19) Uani 1 1 d . . .
N4 N 0.1894(7) 0.3861(7) 1.0774(5) 0.0521(18) Uani 1 1 d . . .
N5 N 0.8103(7) 0.1100(7) 0.9046(5) 0.0555(18) Uani 1 1 d . . .
N6 N 0.9421(7) -0.0030(7) 0.8351(5) 0.0560(19) Uani 1 1 d . . .
N7 N 0.7321(9) 0.3336(8) 1.0733(6) 0.069(2) Uani 1 1 d . . .
N8 N 0.4443(11) 0.0474(10) 0.8438(7) 0.082(3) Uani 1 1 d . . .
N9 N 0.1585(9) 0.3682(8) 0.6354(6) 0.066(2) Uani 1 1 d . . .
O1 O 0.7888(7) 0.3945(7) 1.1092(5) 0.0693(18) Uani 1 1 d . . .
O2 O 0.6141(7) 0.3485(6) 1.0690(5) 0.0697(18) Uani 1 1 d . . .
O3 O 0.7959(7) 0.2716(6) 1.0309(5) 0.0680(18) Uani 1 1 d . . .
O4 O 0.4395(8) 0.0652(7) 0.9189(5) 0.082(2) Uani 1 1 d . . .
O5 O 0.5168(8) 0.0998(7) 0.7834(5) 0.083(2) Uani 1 1 d . . .
O6 O 0.3765(9) -0.0233(8) 0.8285(5) 0.083(2) Uani 1 1 d . . .
O7 O 0.2793(9) 0.4674(7) 0.5252(5) 0.082(2) Uani 1 1 d . . .
C1 C 0.6569(9) 0.3621(9) 0.7560(6) 0.058(2) Uani 1 1 d . . .
H1A H 0.7335 0.3120 0.7490 0.070 Uiso 1 1 calc R . .
C2 C 0.5997(9) 0.4506(8) 0.6879(6) 0.058(2) Uani 1 1 d . . .
H2A H 0.6275 0.4728 0.6271 0.070 Uiso 1 1 calc R . .
C3 C 0.4893(9) 0.4389(8) 0.8164(6) 0.055(2) Uani 1 1 d . . .
H3A H 0.4241 0.4548 0.8580 0.066 Uiso 1 1 calc R . .
C4 C 0.3858(9) 0.5908(8) 0.6816(7) 0.059(2) Uani 1 1 d . . .
H4A H 0.3204 0.6049 0.7272 0.071 Uiso 1 1 calc R . .
H4B H 0.3436 0.5576 0.6409 0.071 Uiso 1 1 calc R . .
C5 C 0.4264(9) 0.7100(8) 0.6275(6) 0.054(2) Uani 1 1 d . . .
C6 C 0.4375(9) 0.7417(9) 0.5359(7) 0.058(2) Uani 1 1 d . . .
H6A H 0.4238 0.6861 0.5053 0.070 Uiso 1 1 calc R . .
C7 C 0.4679(9) 0.8521(8) 0.4861(7) 0.057(2) Uani 1 1 d . . .
H7A H 0.4767 0.8683 0.4231 0.068 Uiso 1 1 calc R . .
C8 C 0.4857(8) 0.9398(8) 0.5263(6) 0.052(2) Uani 1 1 d . . .
C9 C 0.4749(9) 0.9061(8) 0.6204(6) 0.055(2) Uani 1 1 d . . .
H9A H 0.4878 0.9614 0.6514 0.066 Uiso 1 1 calc R . .
C10 C 0.4462(9) 0.7947(8) 0.6696(6) 0.056(2) Uani 1 1 d . . .
H10A H 0.4400 0.7762 0.7328 0.067 Uiso 1 1 calc R . .
C11 C 0.2291(9) 0.2560(8) 0.9971(6) 0.057(2) Uani 1 1 d . . .
H11A H 0.2163 0.2008 0.9659 0.069 Uiso 1 1 calc R . .
C12 C 0.1333(9) 0.3149(8) 1.0391(6) 0.056(2) Uani 1 1 d . . .
H12A H 0.0438 0.3074 1.0413 0.068 Uiso 1 1 calc R . .
C13 C 0.3203(9) 0.3726(9) 1.0564(6) 0.057(2) Uani 1 1 d . . .
H13A H 0.3821 0.4136 1.0729 0.068 Uiso 1 1 calc R . .
C14 C 0.1293(9) 0.4583(8) 1.1341(6) 0.054(2) Uani 1 1 d . . .
H14A H 0.0454 0.4999 1.1086 0.065 Uiso 1 1 calc R . .
H14B H 0.1853 0.5188 1.1340 0.065 Uiso 1 1 calc R . .
C15 C 0.1066(9) 0.3856(8) 1.2312(6) 0.051(2) Uani 1 1 d . . .
C16 C -0.0147(9) 0.3738(9) 1.2688(6) 0.059(2) Uani 1 1 d . . .
H16A H -0.0881 0.4142 1.2348 0.071 Uiso 1 1 calc R . .
C17 C -0.0326(9) 0.3042(9) 1.3556(6) 0.059(2) Uani 1 1 d . . .
H17A H -0.1185 0.3004 1.3788 0.071 Uiso 1 1 calc R . .
C18 C 0.0669(8) 0.2405(8) 1.4099(6) 0.051(2) Uani 1 1 d . . .
C19 C 0.1921(9) 0.2558(10) 1.3731(7) 0.066(3) Uani 1 1 d . . .
H19A H 0.2657 0.2188 1.4080 0.079 Uiso 1 1 calc R . .
C20 C 0.2080(10) 0.3268(10) 1.2837(7) 0.067(3) Uani 1 1 d . . .
H20A H 0.2932 0.3334 1.2597 0.080 Uiso 1 1 calc R . .
C21 C 0.0483(9) 0.1603(8) 1.5022(6) 0.053(2) Uani 1 1 d . . .
C22 C 0.1476(10) 0.0973(9) 1.5552(6) 0.060(2) Uani 1 1 d . . .
H22A H 0.2331 0.1057 1.5325 0.072 Uiso 1 1 calc R . .
C23 C 0.9362(9) 0.1293(9) 0.9117(6) 0.060(2) Uani 1 1 d . . .
H23A H 0.9623 0.1806 0.9421 0.072 Uiso 1 1 calc R . .
C24 C 1.0182(10) 0.0611(9) 0.8669(6) 0.059(2) Uani 1 1 d . . .
H24A H 1.1093 0.0592 0.8596 0.071 Uiso 1 1 calc R . .
C25 C 0.8189(9) 0.0333(8) 0.8572(6) 0.056(2) Uani 1 1 d . . .
H25A H 0.7457 0.0061 0.8403 0.067 Uiso 1 1 calc R . .
C26 C 0.9831(10) -0.0739(8) 0.7710(6) 0.060(2) Uani 1 1 d . . .
H26A H 0.9151 -0.1230 0.7688 0.071 Uiso 1 1 calc R . .
H26B H 1.0632 -0.1274 0.7922 0.071 Uiso 1 1 calc R . .
C27 C 1.0074(9) 0.0054(8) 0.6770(6) 0.054(2) Uani 1 1 d . . .
C28 C 0.9035(10) 0.0676(9) 0.6259(7) 0.063(3) Uani 1 1 d . . .
H28A H 0.8183 0.0591 0.6492 0.076 Uiso 1 1 calc R . .
C29 C 0.9217(9) 0.1441(9) 0.5390(6) 0.063(3) Uani 1 1 d . . .
H29A H 0.8485 0.1850 0.5050 0.076 Uiso 1 1 calc R . .
C30 C 0.1322(9) 0.0204(9) 1.6417(6) 0.061(2) Uani 1 1 d . . .
H30A H 0.2056 -0.0205 1.6754 0.073 Uiso 1 1 calc R . .
C31 C 0.2661(10) 0.2970(10) 0.6931(7) 0.070(3) Uani 1 1 d . . .
H31A H 0.3489 0.3187 0.6651 0.106 Uiso 1 1 calc R . .
H31B H 0.2631 0.2129 0.7006 0.106 Uiso 1 1 calc R . .
H31C H 0.2571 0.3126 0.7517 0.106 Uiso 1 1 calc R . .
C32 C 0.0254(11) 0.3441(10) 0.6681(8) 0.081(3) Uani 1 1 d . . .
H32A H -0.0379 0.3969 0.6262 0.121 Uiso 1 1 calc R . .
H32B H 0.0102 0.3578 0.7271 0.121 Uiso 1 1 calc R . .
H32C H 0.0162 0.2619 0.6725 0.121 Uiso 1 1 calc R . .
C33 C 0.1756(13) 0.4542(11) 0.5498(8) 0.076(3) Uani 1 1 d . . .
H33A H 0.1038 0.4982 0.5156 0.091 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0516(2) 0.0555(2) 0.0511(2) -0.01345(16) 0.00804(15) -0.00857(15)
N1 0.052(4) 0.059(5) 0.056(5) -0.018(4) 0.004(4) -0.006(4)
N2 0.051(4) 0.056(4) 0.053(4) -0.012(4) 0.001(3) -0.007(3)
N3 0.050(4) 0.069(5) 0.056(5) -0.022(4) 0.006(4) -0.012(4)
N4 0.046(4) 0.056(5) 0.054(4) -0.012(4) 0.000(3) -0.016(3)
N5 0.053(4) 0.059(5) 0.054(5) -0.017(4) 0.005(4) -0.004(4)
N6 0.054(5) 0.058(5) 0.055(5) -0.018(4) 0.004(4) -0.002(4)
N7 0.062(6) 0.078(6) 0.075(6) -0.032(5) -0.005(5) -0.006(5)
N8 0.093(8) 0.085(7) 0.064(7) -0.015(6) -0.005(6) -0.009(6)
N9 0.071(6) 0.067(5) 0.064(5) -0.021(4) -0.001(4) -0.012(4)
O1 0.062(4) 0.078(5) 0.075(5) -0.032(4) -0.005(4) -0.006(4)
O2 0.058(4) 0.069(5) 0.087(5) -0.030(4) -0.005(4) -0.007(3)
O3 0.062(4) 0.074(5) 0.077(5) -0.034(4) 0.004(4) -0.012(3)
O4 0.093(6) 0.085(5) 0.064(5) -0.015(4) -0.005(4) -0.009(4)
O5 0.095(6) 0.086(6) 0.064(5) -0.015(4) -0.005(4) -0.009(5)
O6 0.095(6) 0.086(6) 0.063(5) -0.014(4) -0.005(4) -0.009(5)
O7 0.093(6) 0.086(6) 0.063(5) -0.015(4) -0.004(4) -0.009(5)
C1 0.056(5) 0.058(6) 0.055(6) -0.010(5) 0.002(5) -0.003(4)
C2 0.063(6) 0.060(6) 0.048(5) -0.010(4) 0.006(4) -0.005(5)
C3 0.054(5) 0.053(5) 0.056(6) -0.013(4) 0.005(4) -0.008(4)
C4 0.051(5) 0.058(6) 0.064(6) -0.009(5) -0.005(4) -0.006(4)
C5 0.046(5) 0.054(5) 0.059(6) -0.010(4) 0.003(4) -0.008(4)
C6 0.059(6) 0.055(6) 0.060(6) -0.014(5) -0.003(5) -0.011(4)
C7 0.054(5) 0.057(6) 0.056(6) -0.011(5) -0.005(4) -0.003(4)
C8 0.044(5) 0.053(5) 0.056(6) -0.014(4) 0.002(4) -0.002(4)
C9 0.056(5) 0.055(5) 0.054(5) -0.014(4) 0.003(4) -0.007(4)
C10 0.055(5) 0.057(6) 0.053(5) -0.010(4) 0.001(4) -0.008(4)
C11 0.057(6) 0.057(6) 0.059(6) -0.020(5) 0.001(4) -0.007(4)
C12 0.049(5) 0.065(6) 0.053(5) -0.013(5) 0.001(4) -0.011(4)
C13 0.048(5) 0.067(6) 0.057(6) -0.019(5) 0.000(4) -0.011(4)
C14 0.052(5) 0.053(5) 0.054(5) -0.013(4) 0.004(4) -0.005(4)
C15 0.049(5) 0.056(5) 0.048(5) -0.015(4) 0.001(4) -0.005(4)
C16 0.043(5) 0.068(6) 0.061(6) -0.012(5) -0.002(4) -0.004(4)
C17 0.049(5) 0.069(6) 0.053(6) -0.011(5) 0.004(4) -0.004(4)
C18 0.045(5) 0.060(6) 0.048(5) -0.019(4) 0.001(4) -0.005(4)
C19 0.048(5) 0.082(7) 0.058(6) -0.003(5) -0.005(5) -0.009(5)
C20 0.048(5) 0.087(7) 0.059(6) -0.007(5) 0.003(5) -0.012(5)
C21 0.050(5) 0.059(6) 0.051(5) -0.019(4) 0.001(4) -0.005(4)
C22 0.054(6) 0.067(6) 0.054(6) -0.011(5) 0.005(4) -0.002(5)
C23 0.052(6) 0.074(7) 0.057(6) -0.023(5) 0.001(4) -0.007(5)
C24 0.054(5) 0.069(6) 0.055(6) -0.020(5) 0.004(4) -0.006(5)
C25 0.054(6) 0.055(6) 0.056(6) -0.012(4) -0.003(4) -0.002(4)
C26 0.069(6) 0.053(5) 0.055(6) -0.016(4) 0.003(5) 0.000(5)
C27 0.059(6) 0.053(5) 0.049(5) -0.016(4) 0.001(4) -0.002(4)
C28 0.055(6) 0.076(7) 0.055(6) -0.013(5) 0.000(5) -0.011(5)
C29 0.050(5) 0.081(7) 0.054(6) -0.010(5) -0.004(4) -0.005(5)
C30 0.053(6) 0.069(6) 0.053(6) -0.011(5) -0.001(4) 0.004(5)
C31 0.064(6) 0.078(7) 0.076(7) -0.032(6) -0.006(5) -0.007(5)
C32 0.084(8) 0.075(7) 0.082(8) -0.021(6) 0.005(6) -0.010(6)
C33 0.076(8) 0.083(8) 0.070(8) -0.019(6) 0.001(6) -0.021(7)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N1 2.451(8) . ?
Pb1 N5 2.584(7) . ?
Pb1 O4 2.599(8) . ?
Pb1 O3 2.691(7) . ?
Pb1 O2 2.700(7) . ?
Pb1 N3 2.707(7) . ?
N1 C3 1.311(11) . ?
N1 C1 1.379(12) . ?
N2 C3 1.356(11) . ?
N2 C2 1.373(11) . ?
N2 C4 1.445(11) . ?
N3 C13 1.353(11) . ?
N3 C11 1.377(12) . ?
N4 C12 1.347(11) . ?
N4 C13 1.357(11) . ?
N4 C14 1.431(11) . ?
N5 C25 1.293(11) . ?
N5 C23 1.355(12) . ?
N6 C25 1.328(11) . ?
N6 C24 1.349(12) . ?
N6 C26 1.462(11) . ?
N7 O2 1.199(10) . ?
N7 O3 1.205(10) . ?
N7 O1 1.233(10) . ?
N8 O4 1.222(12) . ?
N8 O5 1.226(12) . ?
N8 O6 1.228(13) . ?
N9 C33 1.424(14) . ?
N9 C31 1.459(13) . ?
N9 C32 1.460(13) . ?
O7 C33 1.121(13) . ?
C1 C2 1.338(12) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
C4 C5 1.504(13) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.347(13) . ?
C5 C10 1.365(13) . ?
C6 C7 1.365(13) . ?
C6 H6A 0.9300 . ?
C7 C8 1.372(13) . ?
C7 H7A 0.9300 . ?
C8 C9 1.382(12) . ?
C8 C8 1.468(17) 2_676 ?
C9 C10 1.368(12) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.355(13) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.510(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C20 1.334(12) . ?
C15 C16 1.346(12) . ?
C16 C17 1.363(13) . ?
C16 H16A 0.9300 . ?
C17 C18 1.347(12) . ?
C17 H17A 0.9300 . ?
C18 C19 1.383(13) . ?
C18 C21 1.475(13) . ?
C19 C20 1.398(14) . ?
C19 H19A 0.9300 . ?
C20 H20A 0.9300 . ?
C21 C22 1.334(12) . ?
C21 C29 1.397(13) 1_456 ?
C22 C30 1.386(13) . ?
C22 H22A 0.9300 . ?
C23 C24 1.365(13) . ?
C23 H23A 0.9300 . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 C27 1.500(13) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.353(13) . ?
C27 C30 1.371(13) 1_654 ?
C28 C29 1.394(13) . ?
C28 H28A 0.9300 . ?
C29 C21 1.397(13) 1_654 ?
C29 H29A 0.9300 . ?
C30 C27 1.371(13) 1_456 ?
C30 H30A 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9300 . ?

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
N1 Pb1 N5 82.6(2) . . ?
N1 Pb1 O4 95.9(2) . . ?
N5 Pb1 O4 97.2(2) . . ?
N1 Pb1 O3 87.5(2) . . ?
N5 Pb1 O3 70.5(2) . . ?
O4 Pb1 O3 166.8(2) . . ?
N1 Pb1 O2 86.8(2) . . ?
N5 Pb1 O2 115.3(2) . . ?
O4 Pb1 O2 147.4(2) . . ?
O3 Pb1 O2 45.3(2) . . ?
N1 Pb1 N3 84.5(2) . . ?
N5 Pb1 N3 165.2(2) . . ?
O4 Pb1 N3 76.9(2) . . ?
O3 Pb1 N3 116.2(2) . . ?
O2 Pb1 N3 71.1(2) . . ?
C3 N1 C1 103.3(8) . . ?
C3 N1 Pb1 123.0(6) . . ?
C1 N1 Pb1 130.4(6) . . ?
C3 N2 C2 106.5(7) . . ?
C3 N2 C4 125.0(8) . . ?
C2 N2 C4 127.8(8) . . ?
C13 N3 C11 105.3(7) . . ?
C13 N3 Pb1 125.4(6) . . ?
C11 N3 Pb1 127.8(6) . . ?
C12 N4 C13 106.9(8) . . ?
C12 N4 C14 128.6(8) . . ?
C13 N4 C14 124.4(8) . . ?
C25 N5 C23 105.1(8) . . ?
C25 N5 Pb1 123.9(6) . . ?
C23 N5 Pb1 130.7(6) . . ?
C25 N6 C24 105.5(8) . . ?
C25 N6 C26 126.5(8) . . ?
C24 N6 C26 126.4(8) . . ?
O2 N7 O3 119.4(9) . . ?
O2 N7 O1 120.3(9) . . ?
O3 N7 O1 119.4(9) . . ?
O4 N8 O5 120.3(12) . . ?
O4 N8 O6 120.0(11) . . ?
O5 N8 O6 119.7(11) . . ?
C33 N9 C31 124.6(9) . . ?
C33 N9 C32 119.3(9) . . ?
C31 N9 C32 116.1(9) . . ?
N7 O2 Pb1 97.2(6) . . ?
N7 O3 Pb1 97.5(6) . . ?
N8 O4 Pb1 126.6(8) . . ?
C2 C1 N1 112.3(8) . . ?
C2 C1 H1A 123.9 . . ?
N1 C1 H1A 123.9 . . ?
C1 C2 N2 105.2(8) . . ?
C1 C2 H2A 127.4 . . ?
N2 C2 H2A 127.4 . . ?
N1 C3 N2 112.7(8) . . ?
N1 C3 H3A 123.7 . . ?
N2 C3 H3A 123.7 . . ?
N2 C4 C5 115.7(8) . . ?
N2 C4 H4A 108.4 . . ?
C5 C4 H4A 108.4 . . ?
N2 C4 H4B 108.4 . . ?
C5 C4 H4B 108.4 . . ?
H4A C4 H4B 107.4 . . ?
C6 C5 C10 116.7(9) . . ?
C6 C5 C4 122.3(9) . . ?
C10 C5 C4 120.8(9) . . ?
C5 C6 C7 122.6(9) . . ?
C5 C6 H6A 118.7 . . ?
C7 C6 H6A 118.7 . . ?
C6 C7 C8 122.0(9) . . ?
C6 C7 H7A 119.0 . . ?
C8 C7 H7A 119.0 . . ?
C7 C8 C9 114.9(8) . . ?
C7 C8 C8 122.8(10) . 2_676 ?
C9 C8 C8 122.3(10) . 2_676 ?
C10 C9 C8 122.6(9) . . ?
C10 C9 H9A 118.7 . . ?
C8 C9 H9A 118.7 . . ?
C5 C10 C9 121.2(9) . . ?
C5 C10 H10A 119.4 . . ?
C9 C10 H10A 119.4 . . ?
C12 C11 N3 108.8(8) . . ?
C12 C11 H11A 125.6 . . ?
N3 C11 H11A 125.6 . . ?
N4 C12 C11 108.5(8) . . ?
N4 C12 H12A 125.8 . . ?
C11 C12 H12A 125.8 . . ?
N3 C13 N4 110.5(8) . . ?
N3 C13 H13A 124.8 . . ?
N4 C13 H13A 124.8 . . ?
N4 C14 C15 112.9(7) . . ?
N4 C14 H14A 109.0 . . ?
C15 C14 H14A 109.0 . . ?
N4 C14 H14B 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C20 C15 C16 116.4(9) . . ?
C20 C15 C14 120.8(8) . . ?
C16 C15 C14 122.7(8) . . ?
C15 C16 C17 121.6(9) . . ?
C15 C16 H16A 119.2 . . ?
C17 C16 H16A 119.2 . . ?
C18 C17 C16 123.8(9) . . ?
C18 C17 H17A 118.1 . . ?
C16 C17 H17A 118.1 . . ?
C17 C18 C19 115.0(9) . . ?
C17 C18 C21 124.2(8) . . ?
C19 C18 C21 120.8(8) . . ?
C18 C19 C20 120.0(9) . . ?
C18 C19 H19A 120.0 . . ?
C20 C19 H19A 120.0 . . ?
C15 C20 C19 123.0(9) . . ?
C15 C20 H20A 118.5 . . ?
C19 C20 H20A 118.5 . . ?
C22 C21 C29 115.6(9) . 1_456 ?
C22 C21 C18 123.7(8) . . ?
C29 C21 C18 120.7(8) 1_456 . ?
C21 C22 C30 124.6(9) . . ?
C21 C22 H22A 117.7 . . ?
C30 C22 H22A 117.7 . . ?
N5 C23 C24 108.7(9) . . ?
N5 C23 H23A 125.6 . . ?
C24 C23 H23A 125.6 . . ?
N6 C24 C23 106.9(8) . . ?
N6 C24 H24A 126.5 . . ?
C23 C24 H24A 126.5 . . ?
N5 C25 N6 113.6(9) . . ?
N5 C25 H25A 123.2 . . ?
N6 C25 H25A 123.2 . . ?
N6 C26 C27 111.5(8) . . ?
N6 C26 H26A 109.3 . . ?
C27 C26 H26A 109.3 . . ?
N6 C26 H26B 109.3 . . ?
C27 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 C30 118.3(9) . 1_654 ?
C28 C27 C26 119.4(9) . . ?
C30 C27 C26 122.3(8) 1_654 . ?
C27 C28 C29 121.3(9) . . ?
C27 C28 H28A 119.4 . . ?
C29 C28 H28A 119.4 . . ?
C28 C29 C21 121.0(9) . 1_654 ?
C28 C29 H29A 119.5 . . ?
C21 C29 H29A 119.5 1_654 . ?
C27 C30 C22 119.3(9) 1_456 . ?
C27 C30 H30A 120.4 1_456 . ?
C22 C30 H30A 120.4 . . ?
N9 C31 H31A 109.5 . . ?
N9 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N9 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N9 C32 H32A 109.5 . . ?
N9 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N9 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O7 C33 N9 117.4(12) . . ?
O7 C33 H33A 121.0 . . ?
N9 C33 H33A 121.5 . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.143
_refine_diff_density_min         -0.117
_refine_diff_density_rms         0.142

#====END