# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2003

data_global
_journal_name_full               'New J.Chem.(Nouv.J.Chim.)'

_journal_coden_Cambridge         0440

loop_
_publ_author_name
'Wei-Yin Sun'
'Jian Fan'
'Yi-Zhi Li'
'Taka-aki Okamura'
'Mou-Hai Shu'
'Wen-xia Tang'
;
N.Ueyama
;

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

_publ_contact_author_email       SWEIYIN@YAHOO.COM

_publ_section_title              
;
Solvent effect on structure and topology of
metal-organic frameworks with rigid tripodal tigand
1.3,5-Tris(1-immidazolyl)benzene and Lead(II) Nitrate
;

data_1
_database_code_CSD               206573

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         [Pb(tib)(DMF)(NO3)2]
_chemical_formula_sum            'C18 H19 N9 O7 Pb'
_chemical_formula_weight         680.61

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           monoclinic
_symmetry_space_group_name_H-M   P21/c

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                   8.5468(8)
_cell_length_b                   11.7744(11)
_cell_length_c                   23.277(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.143(2)
_cell_angle_gamma                90.00
_cell_volume                     2329.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5480
_cell_measurement_theta_min      2.4678
_cell_measurement_theta_max      26.9256

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    7.303
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.129
_exptl_absorpt_correction_T_max  0.482
_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            12999
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         27.06
_reflns_number_total             5034
_reflns_number_gt                4221
_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^)+(0.1360P)^2^] 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         5034
_refine_ls_number_parameters     316
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0536
_refine_ls_wR_factor_ref         0.1600
_refine_ls_wR_factor_gt          0.1486
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_restrained_S_all      0.888
_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 0.58004(3) 0.69830(2) 0.145256(10) 0.03410(15) Uani 1 1 d . . .
O11 O 0.7518(9) 0.5630(6) 0.0840(4) 0.099(3) Uani 1 1 d . . .
O12 O 0.9766(7) 0.5953(6) 0.0543(3) 0.0708(18) Uani 1 1 d . . .
O13 O 0.8283(11) 0.7320(7) 0.0769(5) 0.097(3) Uani 1 1 d . . .
O23 O 0.6809(13) 1.0484(6) 0.2075(4) 0.111(3) Uani 1 1 d . . .
O21 O 0.6865(8) 0.8712(5) 0.2219(3) 0.0634(16) Uani 1 1 d . . .
O22 O 0.6194(9) 0.9356(6) 0.1372(3) 0.0710(18) Uani 1 1 d . . .
O31 O 0.703(3) 0.6086(12) 0.2480(8) 0.293(15) Uani 1 1 d D . .
N11 N 0.3284(8) 0.7686(6) 0.1861(3) 0.0427(14) Uani 1 1 d . . .
N12 N 0.1797(7) 0.7925(4) 0.2564(3) 0.0367(13) Uani 1 1 d . . .
N1 N 0.8550(8) 0.6283(6) 0.0729(3) 0.0524(17) Uani 1 1 d . . .
N2 N 0.6621(8) 0.9531(6) 0.1892(4) 0.0575(18) Uani 1 1 d . . .
N3 N 0.8280(16) 0.5640(9) 0.3326(6) 0.136(6) Uani 1 1 d D . .
N51 N 0.4297(8) 0.7518(6) 0.0491(2) 0.0449(14) Uani 1 1 d . . .
N52 N 0.2949(7) 0.7525(5) -0.0369(2) 0.0353(12) Uani 1 1 d . . .
N31 N 0.4121(7) 0.5190(5) 0.1256(3) 0.0427(14) Uani 1 1 d . . .
N32 N 0.2061(6) 0.4061(5) 0.1157(2) 0.0358(12) Uani 1 1 d . . .
C11 C 0.3273(10) 0.7921(6) 0.2418(4) 0.0422(17) Uani 1 1 d . . .
H11A H 0.4166 0.8064 0.2672 0.051 Uiso 1 1 calc R . .
C12 C 0.1766(9) 0.7534(7) 0.1654(3) 0.0468(17) Uani 1 1 d . . .
H12A H 0.1421 0.7362 0.1272 0.056 Uiso 1 1 calc R . .
C13 C 0.0803(9) 0.7664(7) 0.2078(3) 0.0482(18) Uani 1 1 d . . .
H13A H -0.0286 0.7593 0.2046 0.058 Uiso 1 1 calc R . .
C1 C 0.1331(9) 0.8069(5) 0.3129(3) 0.0335(15) Uani 1 1 d . . .
C2 C -0.0112(8) 0.8487(6) 0.3197(3) 0.0367(14) Uani 1 1 d . . .
H2A H -0.0801 0.8704 0.2880 0.044 Uiso 1 1 calc R . .
C3 C -0.0538(7) 0.8585(6) 0.3762(3) 0.0337(14) Uani 1 1 d . . .
C4 C 0.0439(8) 0.8261(5) 0.4230(3) 0.0344(14) Uani 1 1 d . . .
H4A H 0.0135 0.8334 0.4600 0.041 Uiso 1 1 calc R . .
C5 C 0.1890(9) 0.7821(5) 0.4148(3) 0.0342(14) Uani 1 1 d . . .
C6 C 0.2381(8) 0.7727(6) 0.3601(3) 0.0349(14) Uani 1 1 d . . .
H6A H 0.3374 0.7447 0.3549 0.042 Uiso 1 1 calc R . .
C71 C 0.810(3) 0.5732(19) 0.2718(7) 0.62(7) Uani 1 1 d D . .
H71A H 0.8908 0.5485 0.2512 0.741 Uiso 1 1 calc R . .
C72 C 0.957(2) 0.5274(12) 0.3730(11) 0.28(2) Uani 1 1 d D . .
H72A H 1.0395 0.4982 0.3524 0.418 Uiso 1 1 calc R . .
H72B H 0.9213 0.4690 0.3973 0.418 Uiso 1 1 calc R . .
H72C H 0.9956 0.5906 0.3964 0.418 Uiso 1 1 calc R . .
C73 C 0.724(4) 0.571(3) 0.3773(13) 0.41(4) Uani 1 1 d D . .
H73A H 0.6232 0.5981 0.3612 0.620 Uiso 1 1 calc R . .
H73B H 0.7676 0.6214 0.4070 0.620 Uiso 1 1 calc R . .
H73C H 0.7124 0.4964 0.3934 0.620 Uiso 1 1 calc R . .
C51 C 0.3176(9) 0.7001(5) 0.0155(4) 0.0424(18) Uani 1 1 d . . .
H51A H 0.2620 0.6369 0.0260 0.051 Uiso 1 1 calc R . .
C53 C 0.3994(9) 0.8418(7) -0.0357(3) 0.0442(16) Uani 1 1 d . . .
H53A H 0.4106 0.8932 -0.0654 0.053 Uiso 1 1 calc R . .
C52 C 0.4813(10) 0.8399(7) 0.0163(4) 0.0490(19) Uani 1 1 d . . .
H52A H 0.5614 0.8904 0.0289 0.059 Uiso 1 1 calc R . .
C33 C 0.2962(8) 0.3796(6) 0.0718(3) 0.0421(16) Uani 1 1 d . . .
H33A H 0.2747 0.3249 0.0432 0.051 Uiso 1 1 calc R . .
C31 C 0.2804(8) 0.4892(5) 0.1467(3) 0.0373(14) Uani 1 1 d . . .
H31A H 0.2440 0.5221 0.1791 0.045 Uiso 1 1 calc R . .
C32 C 0.4210(8) 0.4487(6) 0.0788(3) 0.0455(17) Uani 1 1 d . . .
H32A H 0.5025 0.4492 0.0553 0.055 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 0.0277(2) 0.0451(2) 0.0298(2) -0.00291(9) 0.00418(12) -0.00355(8)
O11 0.082(5) 0.067(4) 0.162(8) -0.034(5) 0.077(6) -0.025(4)
O12 0.046(3) 0.108(5) 0.065(4) 0.009(3) 0.032(3) 0.015(3)
O13 0.078(6) 0.070(5) 0.148(9) 0.019(5) 0.037(6) 0.007(4)
O23 0.181(10) 0.060(4) 0.098(7) -0.023(4) 0.038(6) -0.040(5)
O21 0.075(4) 0.059(3) 0.052(4) 0.004(3) -0.013(3) -0.004(3)
O22 0.091(5) 0.071(4) 0.046(4) 0.005(3) -0.013(3) -0.015(4)
O31 0.58(5) 0.099(13) 0.181(17) 0.021(10) -0.03(2) 0.015(16)
N11 0.042(4) 0.054(3) 0.034(4) -0.006(3) 0.011(3) 0.010(3)
N12 0.037(3) 0.049(3) 0.026(3) -0.001(2) 0.008(2) 0.013(2)
N1 0.045(4) 0.065(4) 0.050(4) 0.001(3) 0.016(3) 0.002(3)
N2 0.053(4) 0.057(4) 0.062(5) -0.017(4) 0.007(3) -0.015(3)
N3 0.167(14) 0.060(6) 0.171(14) -0.001(8) -0.023(11) -0.020(7)
N51 0.053(4) 0.058(4) 0.024(3) 0.001(3) 0.004(3) -0.015(3)
N52 0.041(3) 0.041(3) 0.024(3) 0.004(2) 0.004(2) -0.008(2)
N31 0.039(3) 0.045(3) 0.045(4) -0.005(3) 0.012(3) -0.007(2)
N32 0.030(3) 0.047(3) 0.032(3) -0.002(2) 0.010(2) -0.008(2)
C11 0.037(4) 0.057(4) 0.034(5) -0.001(3) 0.008(3) 0.008(3)
C12 0.040(4) 0.068(5) 0.033(4) -0.009(4) 0.007(3) 0.009(4)
C13 0.042(4) 0.065(4) 0.037(4) -0.016(4) 0.003(3) 0.014(4)
C1 0.035(4) 0.044(4) 0.022(4) -0.003(2) 0.003(3) 0.002(2)
C2 0.034(4) 0.048(4) 0.028(4) -0.002(3) -0.001(3) 0.012(3)
C3 0.021(3) 0.041(3) 0.040(4) -0.002(3) 0.007(3) 0.005(2)
C4 0.037(4) 0.042(3) 0.027(4) -0.006(3) 0.013(3) 0.003(3)
C5 0.037(4) 0.035(3) 0.032(4) -0.004(3) 0.008(3) 0.002(3)
C6 0.031(3) 0.046(3) 0.029(4) -0.006(3) 0.007(3) 0.008(3)
C71 1.23(15) 0.042(11) 0.74(10) 0.01(3) 0.83(12) -0.03(3)
C72 0.105(14) 0.061(9) 0.63(6) -0.060(17) -0.14(2) -0.005(8)
C73 0.36(5) 0.31(4) 0.65(8) -0.31(5) 0.41(6) -0.20(4)
C51 0.037(4) 0.049(4) 0.040(5) 0.006(3) 0.000(3) -0.012(3)
C53 0.047(4) 0.048(4) 0.038(4) -0.002(3) 0.004(3) -0.017(3)
C52 0.054(5) 0.053(4) 0.040(5) 0.004(4) 0.007(4) -0.024(4)
C33 0.043(4) 0.046(4) 0.040(4) -0.010(3) 0.018(3) -0.001(3)
C31 0.033(3) 0.044(3) 0.036(4) -0.004(3) 0.010(3) -0.013(3)
C32 0.032(4) 0.057(4) 0.050(5) -0.007(3) 0.018(3) -0.005(3)

_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 N51 2.538(6) . ?
Pb1 N31 2.567(6) . ?
Pb1 N11 2.579(6) . ?
Pb1 O11 2.678(6) . ?
Pb1 O31 2.720(15) . ?
O11 N1 1.219(9) . ?
O12 N1 1.231(8) . ?
O13 N1 1.248(10) . ?
O23 N2 1.205(9) . ?
O21 N2 1.232(9) . ?
O22 N2 1.242(9) . ?
O31 C71 1.100(10) . ?
N11 C11 1.327(10) . ?
N11 C12 1.346(10) . ?
N12 C11 1.342(10) . ?
N12 C13 1.375(10) . ?
N12 C1 1.425(9) . ?
N3 C71 1.412(9) . ?
N3 C72 1.435(9) . ?
N3 C73 1.440(9) . ?
N51 C51 1.319(10) . ?
N51 C52 1.387(10) . ?
N52 C51 1.362(9) . ?
N52 C53 1.378(9) . ?
N52 C5 1.425(9) 4_575 ?
N31 C31 1.322(8) . ?
N31 C32 1.378(9) . ?
N32 C31 1.336(8) . ?
N32 C33 1.380(8) . ?
N32 C3 1.448(8) 2_545 ?
C11 H11A 0.9300 . ?
C12 C13 1.359(10) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C1 C2 1.352(10) . ?
C1 C6 1.400(10) . ?
C2 C3 1.406(9) . ?
C2 H2A 0.9300 . ?
C3 C4 1.354(10) . ?
C3 N32 1.448(8) 2 ?
C4 C5 1.376(10) . ?
C4 H4A 0.9300 . ?
C5 C6 1.387(9) . ?
C5 N52 1.425(9) 4_576 ?
C6 H6A 0.9300 . ?
C71 H71A 0.9300 . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C51 H51A 0.9300 . ?
C53 C52 1.334(11) . ?
C53 H53A 0.9300 . ?
C52 H52A 0.9300 . ?
C33 C32 1.337(10) . ?
C33 H33A 0.9300 . ?
C31 H31A 0.9300 . ?
C32 H32A 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
N51 Pb1 N31 80.0(2) . . ?
N51 Pb1 N11 83.2(2) . . ?
N31 Pb1 N11 81.8(2) . . ?
N51 Pb1 O11 86.1(3) . . ?
N31 Pb1 O11 75.16(19) . . ?
N11 Pb1 O11 156.0(2) . . ?
N51 Pb1 O31 169.4(5) . . ?
N31 Pb1 O31 89.6(4) . . ?
N11 Pb1 O31 93.4(6) . . ?
O11 Pb1 O31 93.2(5) . . ?
N1 O11 Pb1 100.8(5) . . ?
C71 O31 Pb1 144(2) . . ?
C11 N11 C12 105.6(6) . . ?
C11 N11 Pb1 121.4(5) . . ?
C12 N11 Pb1 129.5(5) . . ?
C11 N12 C13 107.7(6) . . ?
C11 N12 C1 126.8(7) . . ?
C13 N12 C1 125.3(6) . . ?
O11 N1 O12 122.2(8) . . ?
O11 N1 O13 117.4(7) . . ?
O12 N1 O13 120.2(7) . . ?
O23 N2 O21 120.2(9) . . ?
O23 N2 O22 120.9(9) . . ?
O21 N2 O22 119.0(7) . . ?
C71 N3 C72 132.4(15) . . ?
C71 N3 C73 135.2(17) . . ?
C72 N3 C73 91.8(19) . . ?
C51 N51 C52 105.8(6) . . ?
C51 N51 Pb1 132.5(5) . . ?
C52 N51 Pb1 120.6(5) . . ?
C51 N52 C53 107.4(6) . . ?
C51 N52 C5 126.5(5) . 4_575 ?
C53 N52 C5 126.1(5) . 4_575 ?
C31 N31 C32 104.9(6) . . ?
C31 N31 Pb1 129.3(5) . . ?
C32 N31 Pb1 123.9(4) . . ?
C31 N32 C33 107.2(6) . . ?
C31 N32 C3 126.5(6) . 2_545 ?
C33 N32 C3 126.2(6) . 2_545 ?
N11 C11 N12 110.8(7) . . ?
N11 C11 H11A 124.6 . . ?
N12 C11 H11A 124.6 . . ?
N11 C12 C13 111.2(7) . . ?
N11 C12 H12A 124.4 . . ?
C13 C12 H12A 124.4 . . ?
C12 C13 N12 104.7(7) . . ?
C12 C13 H13A 127.6 . . ?
N12 C13 H13A 127.6 . . ?
C2 C1 C6 121.9(7) . . ?
C2 C1 N12 120.0(6) . . ?
C6 C1 N12 118.0(6) . . ?
C1 C2 C3 118.0(6) . . ?
C1 C2 H2A 121.0 . . ?
C3 C2 H2A 121.0 . . ?
C4 C3 C2 122.0(6) . . ?
C4 C3 N32 119.3(6) . 2 ?
C2 C3 N32 118.7(6) . 2 ?
C3 C4 C5 118.8(6) . . ?
C3 C4 H4A 120.6 . . ?
C5 C4 H4A 120.6 . . ?
C4 C5 C6 121.5(7) . . ?
C4 C5 N52 120.2(6) . 4_576 ?
C6 C5 N52 118.2(6) . 4_576 ?
C5 C6 C1 117.7(6) . . ?
C5 C6 H6A 121.1 . . ?
C1 C6 H6A 121.1 . . ?
O31 C71 N3 122.0(18) . . ?
O31 C71 H71A 119.0 . . ?
N3 C71 H71A 119.0 . . ?
N3 C72 H72A 109.5 . . ?
N3 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
N3 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N3 C73 H73A 109.5 . . ?
N3 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
N3 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
N51 C51 N52 110.3(6) . . ?
N51 C51 H51A 124.8 . . ?
N52 C51 H51A 124.8 . . ?
C52 C53 N52 106.3(6) . . ?
C52 C53 H53A 126.8 . . ?
N52 C53 H53A 126.8 . . ?
C53 C52 N51 110.2(7) . . ?
C53 C52 H52A 124.9 . . ?
N51 C52 H52A 124.9 . . ?
C32 C33 N32 105.9(6) . . ?
C32 C33 H33A 127.1 . . ?
N32 C33 H33A 127.1 . . ?
N31 C31 N32 111.6(6) . . ?
N31 C31 H31A 124.2 . . ?
N32 C31 H31A 124.2 . . ?
C33 C32 N31 110.5(6) . . ?
C33 C32 H32A 124.7 . . ?
N31 C32 H32A 124.7 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.06
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         3.795
_refine_diff_density_min         -1.495
_refine_diff_density_rms         0.225

#====END

data_2
_database_code_CSD               206574

_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(tib)](NO3)2
;
_chemical_name_common            (Pb(tib))(NO3)2
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N8 O6 Pb '
_chemical_formula_sum            'C15 H12 N8 O6 Pb'
_chemical_formula_weight         607.52

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                   8.6278(6)
_cell_length_b                   9.5870(7)
_cell_length_c                   11.5759(8)
_cell_angle_alpha                84.345(4)
_cell_angle_beta                 84.226(5)
_cell_angle_gamma                75.040(4)
_cell_volume                     917.73(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    200
_cell_measurement_reflns_used    2555
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      27.3

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_exptl_absorpt_coefficient_mu    9.247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_T_max  0.757
_exptl_absorpt_process_details   '(Higashi, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71069
_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            8649
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         27.38
_reflns_number_total             4112
_reflns_number_gt                3373
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_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^)+(0.0827P)^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         4112
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1386
_refine_ls_wR_factor_gt          0.1340
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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 0.01484(4) 0.24088(4) 0.31810(2) 0.03407(14) Uani 1 1 d . . .
O11 O 0.1371(8) -0.0290(7) 0.4035(6) 0.0487(17) Uani 1 1 d . . .
O12 O 0.0601(8) -0.2281(7) 0.4259(6) 0.0442(16) Uani 1 1 d . . .
O13 O -0.0604(10) -0.0500(9) 0.3092(6) 0.056(2) Uani 1 1 d . . .
O21 O -0.4387(9) 0.3719(8) 0.1426(6) 0.0505(17) Uani 1 1 d . . .
O22 O -0.2065(12) 0.2289(10) 0.1651(7) 0.074(3) Uani 1 1 d . . .
O23 O -0.2654(13) 0.4344(10) 0.2368(11) 0.100(4) Uani 1 1 d . . .
N1 N 0.0446(9) -0.1036(9) 0.3797(7) 0.0403(18) Uani 1 1 d . . .
N2 N -0.3066(10) 0.3482(9) 0.1817(7) 0.0419(18) Uani 1 1 d . . .
N11 N 0.2510(8) 0.6236(8) 0.1960(6) 0.0332(15) Uani 1 1 d . . .
N12 N 0.0976(10) 0.4728(9) 0.2385(7) 0.0427(18) Uani 1 1 d . . .
N31 N 0.3152(9) 0.1581(8) -0.0302(6) 0.0323(15) Uani 1 1 d . . .
N32 N 0.1767(9) 0.1629(9) 0.1405(7) 0.0376(17) Uani 1 1 d . . .
N51 N 0.4310(9) 0.2088(9) 0.5528(6) 0.0354(16) Uani 1 1 d . . .
N52 N 0.2838(10) 0.2124(9) 0.4054(7) 0.0397(18) Uani 1 1 d . . .
C1 C 0.3786(10) 0.6941(10) 0.2082(7) 0.0305(17) Uani 1 1 d . . .
C2 C 0.4655(10) 0.7383(10) 0.1107(7) 0.0338(19) Uani 1 1 d . . .
H1 H 0.4411 0.7281 0.0343 0.041 Uiso 1 1 calc R . .
C3 C 0.5896(11) 0.7981(10) 0.1298(8) 0.0349(19) Uani 1 1 d . . .
C4 C 0.6253(11) 0.8185(10) 0.2393(8) 0.0351(19) Uani 1 1 d . . .
H2 H 0.7095 0.8624 0.2493 0.042 Uiso 1 1 calc R . .
C5 C 0.5343(11) 0.7731(10) 0.3344(7) 0.0343(18) Uani 1 1 d . . .
C6 C 0.4092(10) 0.7111(10) 0.3204(8) 0.0338(18) Uani 1 1 d . . .
H3 H 0.3465 0.6812 0.3858 0.041 Uiso 1 1 calc R . .
C11 C 0.2210(11) 0.5152(11) 0.2691(8) 0.038(2) Uani 1 1 d . . .
H4 H 0.2803 0.4740 0.3343 0.046 Uiso 1 1 calc R . .
C12 C 0.0449(12) 0.5622(11) 0.1421(8) 0.043(2) Uani 1 1 d . . .
H5 H -0.0449 0.5596 0.1018 0.051 Uiso 1 1 calc R . .
C13 C 0.1415(11) 0.6551(11) 0.1133(8) 0.038(2) Uani 1 1 d . . .
H6 H 0.1344 0.7262 0.0495 0.046 Uiso 1 1 calc R . .
C31 C 0.2771(12) 0.2222(11) 0.0716(8) 0.040(2) Uani 1 1 d . . .
H7 H 0.3175 0.2996 0.0908 0.048 Uiso 1 1 calc R . .
C32 C 0.1492(13) 0.0556(11) 0.0807(8) 0.045(2) Uani 1 1 d . . .
H8 H 0.0817 -0.0063 0.1097 0.054 Uiso 1 1 calc R . .
C33 C 0.2319(12) 0.0508(10) -0.0253(8) 0.040(2) Uani 1 1 d . . .
H9 H 0.2329 -0.0124 -0.0839 0.048 Uiso 1 1 calc R . .
C51 C 0.2801(12) 0.2380(11) 0.5151(8) 0.039(2) Uani 1 1 d . . .
H10 H 0.1840 0.2726 0.5626 0.047 Uiso 1 1 calc R . .
C52 C 0.4440(11) 0.1684(10) 0.3670(8) 0.038(2) Uani 1 1 d . . .
H11 H 0.4839 0.1434 0.2903 0.046 Uiso 1 1 calc R . .
C53 C 0.5376(11) 0.1664(10) 0.4577(7) 0.0364(19) Uani 1 1 d . . .
H12 H 0.6518 0.1411 0.4553 0.044 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 0.0300(2) 0.0437(2) 0.0305(2) -0.00443(14) -0.00275(12) -0.01202(14)
O11 0.034(4) 0.043(4) 0.072(5) -0.008(3) -0.010(3) -0.013(3)
O12 0.039(4) 0.042(4) 0.049(4) 0.002(3) 0.006(3) -0.011(3)
O13 0.056(5) 0.075(5) 0.041(4) 0.012(4) -0.027(3) -0.023(4)
O21 0.040(4) 0.060(5) 0.055(4) -0.012(4) -0.013(3) -0.012(3)
O22 0.075(6) 0.077(6) 0.055(5) -0.025(4) -0.023(4) 0.021(5)
O23 0.077(7) 0.058(5) 0.174(11) -0.040(6) -0.071(7) 0.003(5)
N1 0.033(4) 0.050(5) 0.039(4) -0.014(4) 0.010(3) -0.013(4)
N2 0.033(4) 0.044(5) 0.048(5) -0.004(4) -0.010(3) -0.004(4)
N11 0.026(4) 0.039(4) 0.038(4) -0.008(3) -0.002(3) -0.012(3)
N12 0.040(4) 0.042(4) 0.046(4) -0.004(4) -0.008(4) -0.007(4)
N31 0.031(4) 0.040(4) 0.028(3) -0.002(3) -0.004(3) -0.012(3)
N32 0.034(4) 0.044(4) 0.037(4) -0.006(3) 0.003(3) -0.016(3)
N51 0.029(4) 0.047(4) 0.033(4) -0.007(3) -0.001(3) -0.012(3)
N52 0.036(4) 0.049(5) 0.035(4) -0.001(3) -0.005(3) -0.012(4)
C1 0.027(4) 0.036(4) 0.029(4) -0.009(3) -0.004(3) -0.007(3)
C2 0.032(5) 0.047(5) 0.024(4) -0.007(4) -0.004(3) -0.011(4)
C3 0.030(4) 0.041(5) 0.034(4) -0.003(4) -0.002(3) -0.010(4)
C4 0.030(4) 0.045(5) 0.034(4) -0.006(4) -0.007(3) -0.014(4)
C5 0.036(5) 0.035(4) 0.028(4) 0.001(3) -0.008(3) -0.001(4)
C6 0.028(4) 0.039(5) 0.033(4) 0.003(4) -0.002(3) -0.008(4)
C11 0.033(5) 0.053(6) 0.033(5) -0.002(4) -0.008(4) -0.017(4)
C12 0.042(5) 0.050(6) 0.042(5) 0.001(4) -0.013(4) -0.019(5)
C13 0.039(5) 0.045(5) 0.034(5) 0.003(4) -0.012(4) -0.015(4)
C31 0.039(5) 0.048(5) 0.039(5) -0.009(4) -0.001(4) -0.018(4)
C32 0.044(6) 0.049(6) 0.043(5) -0.007(4) 0.004(4) -0.014(5)
C33 0.045(5) 0.033(5) 0.041(5) -0.011(4) 0.002(4) -0.006(4)
C51 0.034(5) 0.050(6) 0.036(5) -0.004(4) -0.002(4) -0.015(4)
C52 0.035(5) 0.041(5) 0.042(5) -0.011(4) -0.001(4) -0.013(4)
C53 0.027(4) 0.050(5) 0.033(4) -0.010(4) -0.006(3) -0.008(4)

_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 2.434(8) . ?
Pb1 N52 2.563(8) . ?
Pb1 N12 2.566(8) . ?
Pb1 O11 2.661(7) . ?
O11 N1 1.265(10) . ?
O12 N1 1.239(10) . ?
O13 N1 1.256(10) . ?
O21 N2 1.227(10) . ?
O22 N2 1.261(12) . ?
O23 N2 1.231(12) . ?
N11 C11 1.336(11) . ?
N11 C13 1.371(11) . ?
N11 C1 1.456(10) . ?
N12 C11 1.324(12) . ?
N12 C12 1.378(12) . ?
N31 C31 1.354(11) . ?
N31 C33 1.393(11) . ?
N31 C3 1.440(11) 2_665 ?
N32 C31 1.317(11) . ?
N32 C32 1.375(13) . ?
N51 C51 1.365(12) . ?
N51 C53 1.383(11) . ?
N51 C5 1.406(11) 2_666 ?
N52 C51 1.312(12) . ?
N52 C52 1.378(12) . ?
C1 C6 1.384(12) . ?
C1 C2 1.384(12) . ?
C2 C3 1.383(12) . ?
C2 H1 0.9500 . ?
C3 C4 1.377(12) . ?
C3 N31 1.440(11) 2_665 ?
C4 C5 1.388(12) . ?
C4 H2 0.9500 . ?
C5 C6 1.390(13) . ?
C5 N51 1.406(11) 2_666 ?
C6 H3 0.9500 . ?
C11 H4 0.9500 . ?
C12 C13 1.367(12) . ?
C12 H5 0.9500 . ?
C13 H6 0.9500 . ?
C31 H7 0.9500 . ?
C32 C33 1.355(13) . ?
C32 H8 0.9500 . ?
C33 H9 0.9500 . ?
C51 H10 0.9500 . ?
C52 C53 1.383(12) . ?
C52 H11 0.9500 . ?
C53 H12 0.9500 . ?

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 N52 85.8(3) . . ?
N32 Pb1 N12 78.6(3) . . ?
N52 Pb1 N12 76.8(3) . . ?
N32 Pb1 O11 84.6(3) . . ?
N52 Pb1 O11 67.7(2) . . ?
N12 Pb1 O11 141.7(2) . . ?
N1 O11 Pb1 106.7(6) . . ?
O12 N1 O13 121.4(8) . . ?
O12 N1 O11 119.4(8) . . ?
O13 N1 O11 119.2(8) . . ?
O21 N2 O23 123.7(9) . . ?
O21 N2 O22 118.6(9) . . ?
O23 N2 O22 117.7(9) . . ?
C11 N11 C13 108.4(7) . . ?
C11 N11 C1 123.6(7) . . ?
C13 N11 C1 128.0(7) . . ?
C11 N12 C12 105.7(8) . . ?
C11 N12 Pb1 125.9(6) . . ?
C12 N12 Pb1 127.3(6) . . ?
C31 N31 C33 107.3(7) . . ?
C31 N31 C3 126.6(8) . 2_665 ?
C33 N31 C3 125.9(7) . 2_665 ?
C31 N32 C32 106.1(8) . . ?
C31 N32 Pb1 131.3(6) . . ?
C32 N32 Pb1 121.4(6) . . ?
C51 N51 C53 106.5(7) . . ?
C51 N51 C5 125.1(8) . 2_666 ?
C53 N51 C5 128.3(7) . 2_666 ?
C51 N52 C52 106.2(8) . . ?
C51 N52 Pb1 117.9(6) . . ?
C52 N52 Pb1 135.8(6) . . ?
C6 C1 C2 122.7(8) . . ?
C6 C1 N11 116.9(8) . . ?
C2 C1 N11 120.4(7) . . ?
C3 C2 C1 116.9(7) . . ?
C3 C2 H1 121.6 . . ?
C1 C2 H1 121.6 . . ?
C4 C3 C2 123.1(8) . . ?
C4 C3 N31 118.7(8) . 2_665 ?
C2 C3 N31 118.2(7) . 2_665 ?
C3 C4 C5 117.9(8) . . ?
C3 C4 H2 121.0 . . ?
C5 C4 H2 121.0 . . ?
C4 C5 C6 121.4(8) . . ?
C4 C5 N51 119.2(8) . 2_666 ?
C6 C5 N51 119.4(8) . 2_666 ?
C1 C6 C5 118.0(8) . . ?
C1 C6 H3 121.0 . . ?
C5 C6 H3 121.0 . . ?
N12 C11 N11 111.0(8) . . ?
N12 C11 H4 124.5 . . ?
N11 C11 H4 124.5 . . ?
C13 C12 N12 109.6(8) . . ?
C13 C12 H5 125.2 . . ?
N12 C12 H5 125.2 . . ?
C12 C13 N11 105.3(8) . . ?
C12 C13 H6 127.3 . . ?
N11 C13 H6 127.3 . . ?
N32 C31 N31 111.0(8) . . ?
N32 C31 H7 124.5 . . ?
N31 C31 H7 124.5 . . ?
C33 C32 N32 110.3(9) . . ?
C33 C32 H8 124.8 . . ?
N32 C32 H8 124.8 . . ?
C32 C33 N31 105.3(8) . . ?
C32 C33 H9 127.4 . . ?
N31 C33 H9 127.4 . . ?
N52 C51 N51 111.9(9) . . ?
N52 C51 H10 124.0 . . ?
N51 C51 H10 124.0 . . ?
N52 C52 C53 109.3(8) . . ?
N52 C52 H11 125.3 . . ?
C53 C52 H11 125.3 . . ?
N51 C53 C52 105.9(8) . . ?
N51 C53 H12 127.0 . . ?
C52 C53 H12 127.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N32 Pb1 O11 N1 -88.2(6) . . . . ?
N52 Pb1 O11 N1 -175.9(6) . . . . ?
N12 Pb1 O11 N1 -152.2(5) . . . . ?
Pb1 O11 N1 O12 -168.5(6) . . . . ?
Pb1 O11 N1 O13 11.9(9) . . . . ?
N32 Pb1 N12 C11 -95.7(8) . . . . ?
N52 Pb1 N12 C11 -7.5(8) . . . . ?
O11 Pb1 N12 C11 -29.9(10) . . . . ?
N32 Pb1 N12 C12 70.8(8) . . . . ?
N52 Pb1 N12 C12 159.0(9) . . . . ?
O11 Pb1 N12 C12 136.6(8) . . . . ?
N52 Pb1 N32 C31 -63.1(9) . . . . ?
N12 Pb1 N32 C31 14.3(9) . . . . ?
O11 Pb1 N32 C31 -131.1(9) . . . . ?
N52 Pb1 N32 C32 131.1(8) . . . . ?
N12 Pb1 N32 C32 -151.5(8) . . . . ?
O11 Pb1 N32 C32 63.1(8) . . . . ?
N32 Pb1 N52 C51 -178.2(7) . . . . ?
N12 Pb1 N52 C51 102.6(7) . . . . ?
O11 Pb1 N52 C51 -92.3(7) . . . . ?
N32 Pb1 N52 C52 -1.7(9) . . . . ?
N12 Pb1 N52 C52 -81.0(9) . . . . ?
O11 Pb1 N52 C52 84.2(9) . . . . ?
C11 N11 C1 C6 -36.0(12) . . . . ?
C13 N11 C1 C6 142.7(9) . . . . ?
C11 N11 C1 C2 142.7(9) . . . . ?
C13 N11 C1 C2 -38.6(14) . . . . ?
C6 C1 C2 C3 1.6(14) . . . . ?
N11 C1 C2 C3 -177.0(8) . . . . ?
C1 C2 C3 C4 -2.0(14) . . . . ?
C1 C2 C3 N31 178.5(8) . . . 2_665 ?
C2 C3 C4 C5 1.7(15) . . . . ?
N31 C3 C4 C5 -178.7(8) 2_665 . . . ?
C3 C4 C5 C6 -1.1(14) . . . . ?
C3 C4 C5 N51 179.4(8) . . . 2_666 ?
C2 C1 C6 C5 -1.1(14) . . . . ?
N11 C1 C6 C5 177.6(8) . . . . ?
C4 C5 C6 C1 0.8(14) . . . . ?
N51 C5 C6 C1 -179.7(8) 2_666 . . . ?
C12 N12 C11 N11 -1.4(11) . . . . ?
Pb1 N12 C11 N11 167.5(6) . . . . ?
C13 N11 C11 N12 0.3(11) . . . . ?
C1 N11 C11 N12 179.2(8) . . . . ?
C11 N12 C12 C13 2.0(12) . . . . ?
Pb1 N12 C12 C13 -166.7(7) . . . . ?
N12 C12 C13 N11 -1.8(12) . . . . ?
C11 N11 C13 C12 0.9(11) . . . . ?
C1 N11 C13 C12 -177.9(8) . . . . ?
C32 N32 C31 N31 0.2(11) . . . . ?
Pb1 N32 C31 N31 -167.1(6) . . . . ?
C33 N31 C31 N32 0.2(11) . . . . ?
C3 N31 C31 N32 174.4(8) 2_665 . . . ?
C31 N32 C32 C33 -0.7(12) . . . . ?
Pb1 N32 C32 C33 168.2(7) . . . . ?
N32 C32 C33 N31 0.8(11) . . . . ?
C31 N31 C33 C32 -0.6(11) . . . . ?
C3 N31 C33 C32 -174.9(8) 2_665 . . . ?
C52 N52 C51 N51 -1.8(11) . . . . ?
Pb1 N52 C51 N51 175.6(6) . . . . ?
C53 N51 C51 N52 2.2(11) . . . . ?
C5 N51 C51 N52 179.4(8) 2_666 . . . ?
C51 N52 C52 C53 0.7(11) . . . . ?
Pb1 N52 C52 C53 -176.0(7) . . . . ?
C51 N51 C53 C52 -1.6(10) . . . . ?
C5 N51 C53 C52 -178.7(9) 2_666 . . . ?
N52 C52 C53 N51 0.6(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.38
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         2.108
_refine_diff_density_min         -2.832
_refine_diff_density_rms         0.252

#====END