# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'C Russell'
_publ_contact_author_email       CHRIS.RUSSELL@BRIS.AC.UK

_publ_section_title              
;
Syntheses and molecular structures of some saturated
N-heterocyclic plumbylenes
;
loop_
_publ_author_name
'C Russell'
'Jonathan Charmant'
R.Frohlich
'Mairi F Haddow'
'Ekkehardt Hahn'
'Dennis Heitmann'
;
S.M.Mansell
;
'Duncan Wass'

# Attachment 'plumbylenes.cif'

data_plumbylene-1
_database_code_depnum_ccdc_archive 'CCDC 689239'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H38 N2 Pb'
_chemical_formula_weight         585.77

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'
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   C2/c

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

_cell_length_a                   20.2881(5)
_cell_length_b                   6.5360(1)
_cell_length_c                   20.2042(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.915(1)
_cell_angle_gamma                90.00
_cell_volume                     2611.36(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    2864
_cell_measurement_theta_min      0.41
_cell_measurement_theta_max      27.88

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160
_exptl_absorpt_coefficient_mu    6.474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2103
_exptl_absorpt_correction_T_max  0.6974
_exptl_absorpt_process_details   
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9680
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.23
_diffrn_reflns_theta_max         28.26
_reflns_number_total             3178
_reflns_number_gt                2565
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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.
Core of the molecule Pb,N,C21,c22 is disordered with 0.5 occupancy.
ISOR for c21 and c22.
;

_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^)+(0.0103P)^2^+39.4163P] 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    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3178
_refine_ls_number_parameters     149
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1216
_refine_ls_wR_factor_gt          0.1145
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.068
_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
Pb Pb 0.24076(3) -1.43883(7) 0.44820(2) 0.04517(18) Uani 0.50 1 d P . 1
C21 C 0.2426(7) -1.027(2) 0.5147(8) 0.046(3) Uani 0.50 1 d PU . 2
H21A H 0.2664 -0.8958 0.5226 0.056 Uiso 0.50 1 calc PR . 2
H21B H 0.1943 -1.0017 0.5111 0.056 Uiso 0.50 1 calc PR . 2
C22 C 0.2690(9) -1.169(3) 0.5736(9) 0.069(4) Uani 0.50 1 d PU . 2
H22A H 0.3185 -1.1627 0.5866 0.082 Uiso 0.50 1 calc PR . 2
H22B H 0.2510 -1.1301 0.6129 0.082 Uiso 0.50 1 calc PR . 2
N1 N 0.2531(3) -1.1218(7) 0.4487(2) 0.0379(12) Uani 1 1 d . . .
C1 C 0.2475(3) -0.9780(8) 0.3940(2) 0.0302(11) Uani 1 1 d . . .
C2 C 0.3064(3) -0.8867(9) 0.3815(3) 0.0354(12) Uani 1 1 d . . .
C3 C 0.3003(3) -0.7496(9) 0.3275(3) 0.0425(14) Uani 1 1 d . . .
H3 H 0.3393 -0.6863 0.3190 0.051 Uiso 1 1 calc R . .
C4 C 0.2381(4) -0.7058(9) 0.2863(3) 0.0488(17) Uani 1 1 d . . .
H4 H 0.2351 -0.6190 0.2486 0.059 Uiso 1 1 calc R . .
C5 C 0.1811(4) -0.7874(10) 0.3000(3) 0.0467(16) Uani 1 1 d . . .
H5 H 0.1388 -0.7502 0.2730 0.056 Uiso 1 1 calc R . .
C6 C 0.1839(3) -0.9256(9) 0.3534(3) 0.0365(12) Uani 1 1 d . . .
C7 C 0.3762(3) -0.9451(13) 0.4231(3) 0.0564(18) Uani 1 1 d . . .
H7 H 0.3703 -0.9882 0.4684 0.068 Uiso 1 1 calc R . .
C8 C 0.4032(6) -1.127(2) 0.3920(6) 0.152(7) Uani 1 1 d . . .
H8A H 0.3685 -1.2313 0.3814 0.229 Uiso 1 1 calc R . .
H8B H 0.4422 -1.1814 0.4239 0.229 Uiso 1 1 calc R . .
H8C H 0.4164 -1.0852 0.3508 0.229 Uiso 1 1 calc R . .
C9 C 0.4256(5) -0.763(2) 0.4344(6) 0.119(5) Uani 1 1 d . . .
H9A H 0.4679 -0.8046 0.4642 0.179 Uiso 1 1 calc R . .
H9B H 0.4061 -0.6510 0.4550 0.179 Uiso 1 1 calc R . .
H9C H 0.4340 -0.7195 0.3911 0.179 Uiso 1 1 calc R . .
C10 C 0.1185(3) -1.0140(12) 0.3657(4) 0.0534(17) Uani 1 1 d . . .
H10 H 0.1294 -1.0856 0.4099 0.064 Uiso 1 1 calc R . .
C11 C 0.0663(5) -0.8535(18) 0.3695(6) 0.108(4) Uani 1 1 d . . .
H11A H 0.0883 -0.7354 0.3940 0.161 Uiso 1 1 calc R . .
H11B H 0.0335 -0.9089 0.3930 0.161 Uiso 1 1 calc R . .
H11C H 0.0436 -0.8129 0.3239 0.161 Uiso 1 1 calc R . .
C12 C 0.0886(4) -1.1736(17) 0.3110(4) 0.086(3) Uani 1 1 d . . .
H12A H 0.0504 -1.2409 0.3232 0.129 Uiso 1 1 calc R . .
H12B H 0.1229 -1.2744 0.3079 0.129 Uiso 1 1 calc R . .
H12C H 0.0738 -1.1059 0.2675 0.129 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
Pb 0.0889(4) 0.0243(2) 0.0248(3) -0.0007(2) 0.0180(2) 0.0053(2)
C21 0.059(5) 0.032(4) 0.042(4) -0.014(4) -0.002(4) 0.011(4)
C22 0.075(6) 0.069(6) 0.062(6) -0.012(5) 0.015(4) -0.003(5)
N1 0.065(3) 0.032(2) 0.0185(19) 0.0041(17) 0.013(2) 0.013(2)
C1 0.047(3) 0.023(2) 0.022(2) 0.0009(18) 0.010(2) 0.004(2)
C2 0.045(3) 0.035(3) 0.027(2) -0.003(2) 0.010(2) 0.000(2)
C3 0.064(4) 0.031(3) 0.039(3) -0.004(2) 0.026(3) -0.010(3)
C4 0.087(5) 0.029(3) 0.032(3) 0.009(2) 0.017(3) 0.006(3)
C5 0.064(4) 0.041(3) 0.033(3) 0.008(3) 0.005(3) 0.019(3)
C6 0.046(3) 0.035(3) 0.030(2) -0.001(2) 0.011(2) 0.009(3)
C7 0.045(4) 0.080(5) 0.043(3) -0.007(4) 0.008(3) 0.003(4)
C8 0.089(8) 0.220(16) 0.123(9) -0.083(10) -0.031(7) 0.100(9)
C9 0.071(7) 0.161(12) 0.110(8) 0.023(8) -0.014(6) -0.050(7)
C10 0.041(4) 0.071(5) 0.051(4) 0.000(3) 0.016(3) 0.004(3)
C11 0.068(6) 0.131(10) 0.134(9) -0.020(8) 0.044(6) 0.028(6)
C12 0.060(5) 0.124(8) 0.073(5) -0.008(6) 0.014(4) -0.034(6)

_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
Pb N1 2.087(5) . ?
Pb N1 2.096(4) 7_526 ?
Pb Pb 3.2038(9) 7_526 ?
C21 C22 1.51(3) . ?
C21 N1 1.528(14) . ?
C22 N1 1.476(19) 7_526 ?
N1 C1 1.436(6) . ?
N1 C22 1.476(19) 7_526 ?
N1 Pb 2.096(4) 7_526 ?
C1 C6 1.407(8) . ?
C1 C2 1.408(8) . ?
C2 C3 1.396(8) . ?
C2 C7 1.525(9) . ?
C3 C4 1.377(9) . ?
C4 C5 1.357(9) . ?
C5 C6 1.398(8) . ?
C6 C10 1.518(9) . ?
C7 C8 1.504(12) . ?
C7 C9 1.539(12) . ?
C10 C11 1.505(11) . ?
C10 C12 1.541(11) . ?

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 Pb N1 80.05(18) . 7_526 ?
N1 Pb Pb 40.13(11) . 7_526 ?
N1 Pb Pb 39.92(13) 7_526 7_526 ?
C22 C21 N1 110.1(10) . . ?
N1 C22 C21 107.4(12) 7_526 . ?
C1 N1 C22 113.8(9) . 7_526 ?
C1 N1 C21 113.9(7) . . ?
C22 N1 C21 123.3(10) 7_526 . ?
C1 N1 Pb 131.1(3) . . ?
C22 N1 Pb 18.6(8) 7_526 . ?
C21 N1 Pb 111.5(6) . . ?
C1 N1 Pb 128.2(3) . 7_526 ?
C22 N1 Pb 115.1(8) 7_526 7_526 ?
C21 N1 Pb 17.3(6) . 7_526 ?
Pb N1 Pb 99.95(18) . 7_526 ?
C6 C1 C2 119.7(5) . . ?
C6 C1 N1 120.9(5) . . ?
C2 C1 N1 119.4(5) . . ?
C3 C2 C1 118.9(5) . . ?
C3 C2 C7 120.0(6) . . ?
C1 C2 C7 121.0(5) . . ?
C4 C3 C2 120.9(6) . . ?
C5 C4 C3 120.2(5) . . ?
C4 C5 C6 121.4(6) . . ?
C5 C6 C1 118.8(6) . . ?
C5 C6 C10 119.0(6) . . ?
C1 C6 C10 122.2(5) . . ?
C8 C7 C2 110.4(6) . . ?
C8 C7 C9 112.7(9) . . ?
C2 C7 C9 112.5(7) . . ?
C11 C10 C6 113.2(7) . . ?
C11 C10 C12 109.9(7) . . ?
C6 C10 C12 111.0(6) . . ?

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
N1 C21 C22 N1 -43.4(16) . . . 7_526 ?
C22 C21 N1 C1 -163.4(10) . . . . ?
C22 C21 N1 C22 51.6(19) . . . 7_526 ?
C22 C21 N1 Pb 35.4(13) . . . . ?
C22 C21 N1 Pb -14.7(13) . . . 7_526 ?
N1 Pb N1 C1 -170.3(6) 7_526 . . . ?
Pb Pb N1 C1 -170.3(6) 7_526 . . . ?
N1 Pb N1 C22 -146(2) 7_526 . . 7_526 ?
Pb Pb N1 C22 -146(2) 7_526 . . 7_526 ?
N1 Pb N1 C21 -13.4(6) 7_526 . . . ?
Pb Pb N1 C21 -13.4(6) 7_526 . . . ?
N1 Pb N1 Pb 0.0 7_526 . . 7_526 ?
C22 N1 C1 C6 64.7(10) 7_526 . . . ?
C21 N1 C1 C6 -83.7(8) . . . . ?
Pb N1 C1 C6 72.8(7) . . . . ?
Pb N1 C1 C6 -95.0(6) 7_526 . . . ?
C22 N1 C1 C2 -116.2(9) 7_526 . . . ?
C21 N1 C1 C2 95.5(8) . . . . ?
Pb N1 C1 C2 -108.0(6) . . . . ?
Pb N1 C1 C2 84.1(6) 7_526 . . . ?
C6 C1 C2 C3 -1.8(8) . . . . ?
N1 C1 C2 C3 179.0(5) . . . . ?
C6 C1 C2 C7 -178.1(5) . . . . ?
N1 C1 C2 C7 2.8(8) . . . . ?
C1 C2 C3 C4 -0.9(8) . . . . ?
C7 C2 C3 C4 175.5(6) . . . . ?
C2 C3 C4 C5 3.5(9) . . . . ?
C3 C4 C5 C6 -3.5(9) . . . . ?
C4 C5 C6 C1 0.8(9) . . . . ?
C4 C5 C6 C10 -179.2(6) . . . . ?
C2 C1 C6 C5 1.8(8) . . . . ?
N1 C1 C6 C5 -179.0(5) . . . . ?
C2 C1 C6 C10 -178.2(5) . . . . ?
N1 C1 C6 C10 1.0(8) . . . . ?
C3 C2 C7 C8 -88.8(10) . . . . ?
C1 C2 C7 C8 87.4(9) . . . . ?
C3 C2 C7 C9 38.0(9) . . . . ?
C1 C2 C7 C9 -145.8(7) . . . . ?
C5 C6 C10 C11 -50.6(9) . . . . ?
C1 C6 C10 C11 129.4(7) . . . . ?
C5 C6 C10 C12 73.5(8) . . . . ?
C1 C6 C10 C12 -106.5(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        28.26
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.518
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.103

#===END

data_plumbylene-2
_database_code_depnum_ccdc_archive 'CCDC 689240'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H52 N4 Pb2'
_chemical_formula_weight         1003.24

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   8.7974(5)
_cell_length_b                   10.0046(6)
_cell_length_c                   11.9931(7)
_cell_angle_alpha                66.2800(10)
_cell_angle_beta                 74.3180(10)
_cell_angle_gamma                68.1540(10)
_cell_volume                     887.91(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    900
_cell_measurement_theta_min      1
_cell_measurement_theta_max      22.5

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             484
_exptl_absorpt_coefficient_mu    9.502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3298
_exptl_absorpt_correction_T_max  0.7024
_exptl_absorpt_process_details   
;
Corrections were done with the SADABS program, utilizing the none merged
raw data obtained from the integration process. Integration and final cell
refinement were done with SAINT.

SADABS reports ratio of Tmin/Tmax = 0.506270

;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean 80
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10817
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         31.59
_reflns_number_total             5519
_reflns_number_gt                5123
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_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^)+(0.0266P)^2^+0.7869P] 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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5519
_refine_ls_number_parameters     214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0201
_refine_ls_wR_factor_ref         0.0502
_refine_ls_wR_factor_gt          0.0490
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0781(3) -0.2913(3) 0.1398(2) 0.0181(5) Uani 1 1 d . . .
H1A H 0.0029 -0.3191 0.2177 0.022 Uiso 1 1 calc R . .
H1B H 0.1879 -0.3689 0.1496 0.022 Uiso 1 1 calc R . .
C2 C 0.1860(3) -0.1428(3) 0.2000(2) 0.0147(4) Uani 1 1 d . . .
C3 C 0.1056(3) -0.1159(3) 0.3114(2) 0.0162(5) Uani 1 1 d . . .
C4 C 0.1933(3) -0.1035(3) 0.3851(3) 0.0197(5) Uani 1 1 d . . .
H4 H 0.1362 -0.0821 0.4584 0.024 Uiso 1 1 calc R . .
C5 C 0.3619(3) -0.1214(3) 0.3552(3) 0.0205(5) Uani 1 1 d . . .
C6 C 0.4423(3) -0.1637(3) 0.2535(3) 0.0212(5) Uani 1 1 d . . .
H6 H 0.5591 -0.1849 0.2352 0.025 Uiso 1 1 calc R . .
C7 C 0.3594(3) -0.1766(3) 0.1764(2) 0.0188(5) Uani 1 1 d . . .
C8 C -0.0750(3) -0.1028(3) 0.3592(3) 0.0214(5) Uani 1 1 d . . .
H8A H -0.0906 -0.1424 0.4494 0.032 Uiso 1 1 calc R . .
H8B H -0.1103 -0.1622 0.3286 0.032 Uiso 1 1 calc R . .
H8C H -0.1413 0.0049 0.3307 0.032 Uiso 1 1 calc R . .
C9 C 0.4511(4) -0.0966(4) 0.4325(3) 0.0282(6) Uani 1 1 d . . .
H9A H 0.5708 -0.1347 0.4091 0.042 Uiso 1 1 calc R . .
H9B H 0.4211 -0.1519 0.5195 0.042 Uiso 1 1 calc R . .
H9C H 0.4196 0.0129 0.4193 0.042 Uiso 1 1 calc R . .
C10 C 0.4670(4) -0.2343(4) 0.0730(3) 0.0268(6) Uani 1 1 d . . .
H10A H 0.4914 -0.1482 0.0022 0.040 Uiso 1 1 calc R . .
H10B H 0.4085 -0.2828 0.0491 0.040 Uiso 1 1 calc R . .
H10C H 0.5707 -0.3092 0.1011 0.040 Uiso 1 1 calc R . .
C11 C -0.0111(3) 0.2909(3) -0.0355(2) 0.0178(5) Uani 1 1 d . . .
H11A H 0.1030 0.2204 -0.0305 0.021 Uiso 1 1 calc R . .
H11B H -0.0076 0.3948 -0.0514 0.021 Uiso 1 1 calc R . .
C12 C -0.1341(3) 0.2999(3) 0.1737(2) 0.0163(5) Uani 1 1 d . . .
C13 C -0.2945(3) 0.3520(3) 0.2345(3) 0.0189(5) Uani 1 1 d . . .
C14 C -0.3179(4) 0.4141(3) 0.3250(3) 0.0233(5) Uani 1 1 d . . .
H14 H -0.4271 0.4491 0.3640 0.028 Uiso 1 1 calc R . .
C15 C -0.1873(4) 0.4267(3) 0.3605(3) 0.0210(5) Uani 1 1 d . . .
C16 C -0.0306(4) 0.3722(3) 0.3028(3) 0.0191(5) Uani 1 1 d . . .
H16 H 0.0610 0.3774 0.3267 0.023 Uiso 1 1 calc R . .
C17 C -0.0003(3) 0.3097(3) 0.2110(2) 0.0171(5) Uani 1 1 d . . .
C18 C -0.4449(4) 0.3462(4) 0.2009(3) 0.0288(6) Uani 1 1 d . . .
H18A H -0.4461 0.2399 0.2306 0.043 Uiso 1 1 calc R . .
H18B H -0.4410 0.3883 0.1112 0.043 Uiso 1 1 calc R . .
H18C H -0.5452 0.4067 0.2389 0.043 Uiso 1 1 calc R . .
C19 C -0.2169(4) 0.4954(4) 0.4579(3) 0.0295(6) Uani 1 1 d . . .
H19A H -0.2268 0.4177 0.5394 0.044 Uiso 1 1 calc R . .
H19B H -0.3192 0.5811 0.4496 0.044 Uiso 1 1 calc R . .
H19C H -0.1238 0.5324 0.4484 0.044 Uiso 1 1 calc R . .
C20 C 0.1771(3) 0.2525(3) 0.1560(3) 0.0219(5) Uani 1 1 d . . .
H20A H 0.2005 0.3283 0.0761 0.033 Uiso 1 1 calc R . .
H20B H 0.1948 0.1557 0.1448 0.033 Uiso 1 1 calc R . .
H20C H 0.2513 0.2362 0.2113 0.033 Uiso 1 1 calc R . .
N1 N 0.0932(3) -0.1384(2) 0.1145(2) 0.0147(4) Uani 1 1 d . . .
N2 N -0.1163(3) 0.2423(3) 0.0799(2) 0.0172(4) Uani 1 1 d . . .
Pb1 Pb -0.187459(11) 0.045057(10) 0.096862(9) 0.01642(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0251(13) 0.0114(10) 0.0179(12) -0.0050(9) -0.0018(10) -0.0066(9)
C2 0.0169(11) 0.0123(10) 0.0153(11) -0.0047(8) -0.0032(9) -0.0042(9)
C3 0.0155(11) 0.0158(11) 0.0163(11) -0.0066(9) 0.0005(9) -0.0043(9)
C4 0.0230(13) 0.0193(12) 0.0187(12) -0.0100(10) -0.0008(10) -0.0062(10)
C5 0.0203(12) 0.0199(12) 0.0232(13) -0.0075(10) -0.0063(10) -0.0054(10)
C6 0.0168(12) 0.0240(13) 0.0240(13) -0.0088(11) -0.0022(10) -0.0071(10)
C7 0.0190(12) 0.0193(12) 0.0178(12) -0.0077(10) -0.0002(10) -0.0052(10)
C8 0.0180(12) 0.0275(14) 0.0195(12) -0.0103(11) 0.0026(10) -0.0086(10)
C9 0.0298(15) 0.0337(16) 0.0314(16) -0.0165(13) -0.0057(12) -0.0135(13)
C10 0.0183(13) 0.0359(16) 0.0239(14) -0.0163(12) -0.0012(11) 0.0000(11)
C11 0.0231(12) 0.0159(11) 0.0162(11) -0.0065(9) 0.0010(10) -0.0093(10)
C12 0.0178(11) 0.0139(10) 0.0171(11) -0.0070(9) 0.0000(9) -0.0047(9)
C13 0.0186(12) 0.0183(12) 0.0200(12) -0.0087(10) -0.0024(10) -0.0037(9)
C14 0.0231(13) 0.0235(13) 0.0221(13) -0.0127(11) 0.0017(11) -0.0037(11)
C15 0.0296(14) 0.0164(11) 0.0178(12) -0.0091(10) 0.0003(10) -0.0066(10)
C16 0.0245(13) 0.0166(11) 0.0189(12) -0.0066(9) -0.0014(10) -0.0094(10)
C17 0.0194(12) 0.0120(10) 0.0192(12) -0.0052(9) -0.0003(9) -0.0058(9)
C18 0.0185(13) 0.0358(17) 0.0359(17) -0.0218(14) -0.0027(12) -0.0025(12)
C19 0.0377(17) 0.0303(15) 0.0258(15) -0.0186(13) 0.0026(13) -0.0106(13)
C20 0.0171(12) 0.0236(13) 0.0272(14) -0.0114(11) -0.0008(10) -0.0068(10)
N1 0.0183(10) 0.0112(9) 0.0149(9) -0.0043(7) -0.0030(8) -0.0043(8)
N2 0.0215(11) 0.0172(10) 0.0156(10) -0.0089(8) 0.0030(8) -0.0090(8)
Pb1 0.01692(5) 0.01567(5) 0.01709(5) -0.00570(3) -0.00030(3) -0.00660(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
C1 N1 1.485(3) . ?
C1 C11 1.518(4) 2 ?
C2 C7 1.407(4) . ?
C2 C3 1.412(4) . ?
C2 N1 1.452(3) . ?
C3 C4 1.386(4) . ?
C3 C8 1.511(4) . ?
C4 C5 1.389(4) . ?
C5 C6 1.376(4) . ?
C5 C9 1.503(4) . ?
C6 C7 1.391(4) . ?
C7 C10 1.517(4) . ?
C11 N2 1.453(3) . ?
C11 C1 1.518(4) 2 ?
C12 N2 1.408(3) . ?
C12 C13 1.413(4) . ?
C12 C17 1.414(4) . ?
C13 C14 1.390(4) . ?
C13 C18 1.510(4) . ?
C14 C15 1.390(4) . ?
C15 C16 1.381(4) . ?
C15 C19 1.502(4) . ?
C16 C17 1.394(4) . ?
C17 C20 1.511(4) . ?
N1 Pb1 2.350(2) 2 ?
N1 Pb1 2.471(2) . ?
N2 Pb1 2.203(2) . ?
Pb1 N1 2.350(2) 2 ?
Pb1 Pb1 3.5241(2) 2 ?

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 C1 C11 110.6(2) . 2 ?
C7 C2 C3 117.4(2) . . ?
C7 C2 N1 121.5(2) . . ?
C3 C2 N1 121.1(2) . . ?
C4 C3 C2 120.2(2) . . ?
C4 C3 C8 116.1(2) . . ?
C2 C3 C8 123.6(2) . . ?
C3 C4 C5 122.0(3) . . ?
C6 C5 C4 117.2(3) . . ?
C6 C5 C9 122.1(3) . . ?
C4 C5 C9 120.7(3) . . ?
C5 C6 C7 122.6(3) . . ?
C6 C7 C2 119.8(2) . . ?
C6 C7 C10 116.1(2) . . ?
C2 C7 C10 124.0(2) . . ?
N2 C11 C1 109.7(2) . 2 ?
N2 C12 C13 118.6(2) . . ?
N2 C12 C17 123.9(2) . . ?
C13 C12 C17 117.5(2) . . ?
C14 C13 C12 120.4(3) . . ?
C14 C13 C18 118.3(3) . . ?
C12 C13 C18 121.3(2) . . ?
C13 C14 C15 122.4(3) . . ?
C16 C15 C14 116.8(2) . . ?
C16 C15 C19 122.1(3) . . ?
C14 C15 C19 121.1(3) . . ?
C15 C16 C17 123.1(3) . . ?
C16 C17 C12 119.7(2) . . ?
C16 C17 C20 118.0(2) . . ?
C12 C17 C20 122.3(2) . . ?
C2 N1 C1 111.7(2) . . ?
C2 N1 Pb1 117.82(16) . 2 ?
C1 N1 Pb1 106.54(15) . 2 ?
C2 N1 Pb1 118.03(15) . . ?
C1 N1 Pb1 106.94(16) . . ?
Pb1 N1 Pb1 93.90(7) 2 . ?
C12 N2 C11 119.7(2) . . ?
C12 N2 Pb1 127.21(17) . . ?
C11 N2 Pb1 111.80(15) . . ?
N2 Pb1 N1 77.28(8) . 2 ?
N2 Pb1 N1 95.43(8) . . ?
N1 Pb1 N1 86.10(7) 2 . ?
N2 Pb1 Pb1 85.38(6) . 2 ?
N1 Pb1 Pb1 44.40(5) 2 2 ?
N1 Pb1 Pb1 41.70(5) . 2 ?

_diffrn_measured_fraction_theta_max 0.927
_diffrn_reflns_theta_full        31.59
_diffrn_measured_fraction_theta_full 0.927
_refine_diff_density_max         1.528
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.127

#===END

data_plumbylene-3
_database_code_depnum_ccdc_archive 'CCDC 689241'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H40 N2 Pb1'
_chemical_formula_sum            'C27 H40 N2 Pb1'
_chemical_formula_weight         599.81

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'
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 2(1)/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   12.9865(17)
_cell_length_b                   14.1072(18)
_cell_length_c                   14.7915(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.445(2)
_cell_angle_gamma                90.00
_cell_volume                     2697.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6830
_cell_measurement_theta_min      2.137
_cell_measurement_theta_max      25.2665

_exptl_crystal_description       Needle
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_absorpt_coefficient_mu    6.268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.31017043
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_process_details   'SADABS v2.10 (BRUKER AXS, 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.2
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28092
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6184
_reflns_number_gt                4260
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.0399P)^2^+1.2145P] 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         6184
_refine_ls_number_parameters     279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.0960
_refine_ls_wR_factor_gt          0.0836
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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 0.579512(18) 0.569671(18) 0.110942(15) 0.03931(9) Uani 1 1 d . . .
N1 N 0.7036(4) 0.6041(3) 0.0318(3) 0.0336(11) Uani 1 1 d . . .
N2 N 0.6497(3) 0.6525(3) 0.2199(3) 0.0332(11) Uani 1 1 d . . .
C1 C 0.6936(4) 0.5799(5) -0.0615(4) 0.0393(15) Uani 1 1 d . . .
C2 C 0.7352(5) 0.4938(5) -0.0903(5) 0.0494(17) Uani 1 1 d . . .
C3 C 0.7118(6) 0.4669(6) -0.1795(6) 0.069(2) Uani 1 1 d . . .
H3 H 0.7372 0.4079 -0.1990 0.083 Uiso 1 1 calc R . .
C4 C 0.6536(7) 0.5212(8) -0.2409(5) 0.078(3) Uani 1 1 d . . .
H4 H 0.6367 0.4988 -0.3011 0.094 Uiso 1 1 calc R . .
C5 C 0.6194(6) 0.6093(7) -0.2152(5) 0.068(2) Uani 1 1 d . . .
H5 H 0.5827 0.6492 -0.2590 0.082 Uiso 1 1 calc R . .
C6 C 0.6385(5) 0.6400(5) -0.1252(4) 0.0484(17) Uani 1 1 d . . .
C7 C 0.8047(6) 0.4335(5) -0.0262(5) 0.0528(17) Uani 1 1 d . . .
H7 H 0.8227 0.4725 0.0296 0.063 Uiso 1 1 calc R . .
C8 C 0.7557(8) 0.3465(7) 0.0035(8) 0.108(4) Uani 1 1 d . . .
H8A H 0.7002 0.3631 0.0412 0.162 Uiso 1 1 calc R . .
H8B H 0.8074 0.3076 0.0390 0.162 Uiso 1 1 calc R . .
H8C H 0.7268 0.3108 -0.0498 0.162 Uiso 1 1 calc R . .
C9 C 0.9066(7) 0.4098(9) -0.0650(8) 0.123(5) Uani 1 1 d . . .
H9A H 0.9562 0.3856 -0.0165 0.185 Uiso 1 1 calc R . .
H9B H 0.9345 0.4671 -0.0911 0.185 Uiso 1 1 calc R . .
H9C H 0.8943 0.3615 -0.1124 0.185 Uiso 1 1 calc R . .
C10 C 0.6004(5) 0.7372(5) -0.0990(5) 0.059(2) Uani 1 1 d . . .
H10 H 0.6253 0.7471 -0.0336 0.070 Uiso 1 1 calc R . .
C11 C 0.4851(6) 0.7442(7) -0.1061(7) 0.096(3) Uani 1 1 d . . .
H11A H 0.4649 0.8102 -0.0970 0.144 Uiso 1 1 calc R . .
H11B H 0.4582 0.7042 -0.0595 0.144 Uiso 1 1 calc R . .
H11C H 0.4566 0.7229 -0.1664 0.144 Uiso 1 1 calc R . .
C12 C 0.6435(7) 0.8166(7) -0.1510(7) 0.095(3) Uani 1 1 d . . .
H12A H 0.6265 0.8062 -0.2162 0.143 Uiso 1 1 calc R . .
H12B H 0.7188 0.8189 -0.1374 0.143 Uiso 1 1 calc R . .
H12C H 0.6133 0.8768 -0.1334 0.143 Uiso 1 1 calc R . .
C13 C 0.5925(4) 0.6694(4) 0.2959(4) 0.0345(13) Uani 1 1 d . . .
C14 C 0.6089(5) 0.6106(4) 0.3725(4) 0.0366(14) Uani 1 1 d . . .
C15 C 0.5482(6) 0.6237(5) 0.4435(4) 0.0505(18) Uani 1 1 d . . .
H15 H 0.5582 0.5839 0.4954 0.061 Uiso 1 1 calc R . .
C16 C 0.4742(6) 0.6926(5) 0.4405(5) 0.064(2) Uani 1 1 d . . .
H16 H 0.4319 0.6992 0.4891 0.077 Uiso 1 1 calc R . .
C17 C 0.4609(6) 0.7521(5) 0.3674(5) 0.0559(19) Uani 1 1 d . . .
H17 H 0.4101 0.8007 0.3665 0.067 Uiso 1 1 calc R . .
C18 C 0.5199(5) 0.7433(4) 0.2945(4) 0.0432(15) Uani 1 1 d . . .
C19 C 0.6880(5) 0.5330(5) 0.3775(4) 0.0480(17) Uani 1 1 d . . .
H19 H 0.7342 0.5451 0.3283 0.058 Uiso 1 1 calc R . .
C20 C 0.6385(8) 0.4374(5) 0.3589(6) 0.083(3) Uani 1 1 d . . .
H20A H 0.5850 0.4271 0.4004 0.125 Uiso 1 1 calc R . .
H20B H 0.6913 0.3877 0.3683 0.125 Uiso 1 1 calc R . .
H20C H 0.6071 0.4351 0.2961 0.125 Uiso 1 1 calc R . .
C21 C 0.7560(8) 0.5320(8) 0.4670(6) 0.108(4) Uani 1 1 d . . .
H21A H 0.7160 0.5084 0.5152 0.163 Uiso 1 1 calc R . .
H21B H 0.7802 0.5965 0.4817 0.163 Uiso 1 1 calc R . .
H21C H 0.8156 0.4905 0.4616 0.163 Uiso 1 1 calc R . .
C22 C 0.5077(6) 0.8140(5) 0.2181(5) 0.0571(19) Uani 1 1 d . . .
H22 H 0.5478 0.7898 0.1685 0.069 Uiso 1 1 calc R . .
C23 C 0.3969(8) 0.8256(8) 0.1789(8) 0.128(5) Uani 1 1 d . . .
H23A H 0.3657 0.7631 0.1672 0.193 Uiso 1 1 calc R . .
H23B H 0.3949 0.8612 0.1218 0.193 Uiso 1 1 calc R . .
H23C H 0.3582 0.8602 0.2221 0.193 Uiso 1 1 calc R . .
C24 C 0.5527(8) 0.9098(5) 0.2473(6) 0.085(3) Uani 1 1 d . . .
H24A H 0.5070 0.9410 0.2872 0.128 Uiso 1 1 calc R . .
H24B H 0.5588 0.9492 0.1935 0.128 Uiso 1 1 calc R . .
H24C H 0.6212 0.9009 0.2800 0.128 Uiso 1 1 calc R . .
C25 C 0.7947(4) 0.6593(4) 0.0626(4) 0.0352(13) Uani 1 1 d . . .
H25A H 0.7821 0.7264 0.0456 0.042 Uiso 1 1 calc R . .
H25B H 0.8538 0.6367 0.0308 0.042 Uiso 1 1 calc R . .
C26 C 0.8236(5) 0.6534(5) 0.1636(4) 0.0445(16) Uani 1 1 d . . .
H26A H 0.8927 0.6826 0.1771 0.053 Uiso 1 1 calc R . .
H26B H 0.8300 0.5857 0.1807 0.053 Uiso 1 1 calc R . .
C27 C 0.7496(5) 0.7003(5) 0.2239(4) 0.0473(17) Uani 1 1 d . . .
H27A H 0.7813 0.7003 0.2875 0.057 Uiso 1 1 calc R . .
H27B H 0.7388 0.7671 0.2048 0.057 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 0.03532(14) 0.05272(16) 0.03117(12) -0.00815(12) 0.00987(9) -0.01660(12)
N1 0.029(3) 0.045(3) 0.027(2) -0.003(2) 0.005(2) -0.008(2)
N2 0.029(3) 0.041(3) 0.031(2) -0.010(2) 0.007(2) -0.009(2)
C1 0.027(3) 0.058(4) 0.033(3) 0.003(3) 0.007(3) -0.005(3)
C2 0.043(4) 0.061(5) 0.046(4) -0.007(3) 0.012(3) -0.004(3)
C3 0.063(5) 0.088(6) 0.057(5) -0.028(4) 0.016(4) -0.003(5)
C4 0.066(6) 0.134(9) 0.034(4) -0.017(5) 0.005(4) -0.004(6)
C5 0.055(5) 0.116(7) 0.033(4) 0.006(4) 0.002(4) 0.000(5)
C6 0.033(4) 0.079(5) 0.034(3) 0.004(3) 0.008(3) -0.004(3)
C7 0.055(4) 0.054(4) 0.052(4) -0.006(4) 0.016(3) -0.002(4)
C8 0.099(8) 0.086(7) 0.136(9) 0.038(7) -0.013(7) -0.023(6)
C9 0.077(7) 0.190(13) 0.111(9) 0.049(8) 0.051(6) 0.059(8)
C10 0.049(4) 0.076(5) 0.051(4) 0.019(4) 0.006(4) 0.007(4)
C11 0.038(5) 0.115(8) 0.134(9) 0.023(7) 0.010(5) 0.012(5)
C12 0.098(7) 0.088(7) 0.101(7) 0.035(6) 0.019(6) -0.002(6)
C13 0.035(3) 0.035(3) 0.034(3) -0.009(3) 0.011(3) -0.011(3)
C14 0.038(4) 0.034(3) 0.039(3) -0.001(3) 0.008(3) -0.004(3)
C15 0.068(5) 0.046(4) 0.042(4) 0.004(3) 0.029(4) 0.004(4)
C16 0.076(5) 0.055(5) 0.067(5) 0.002(4) 0.041(4) 0.012(4)
C17 0.062(5) 0.045(4) 0.064(5) -0.004(3) 0.023(4) 0.016(4)
C18 0.049(4) 0.035(4) 0.046(4) 0.001(3) 0.007(3) -0.001(3)
C19 0.053(4) 0.050(4) 0.042(4) 0.005(3) 0.009(3) 0.005(3)
C20 0.117(8) 0.046(5) 0.094(7) 0.005(4) 0.049(6) 0.018(5)
C21 0.101(8) 0.147(10) 0.071(6) -0.007(6) -0.023(6) 0.062(7)
C22 0.077(5) 0.049(4) 0.045(4) 0.001(3) 0.003(4) 0.016(4)
C23 0.115(9) 0.121(9) 0.136(10) 0.039(8) -0.057(8) -0.004(7)
C24 0.128(9) 0.048(5) 0.079(6) 0.014(4) 0.011(6) -0.004(5)
C25 0.024(3) 0.046(4) 0.037(3) -0.001(3) 0.011(3) -0.002(3)
C26 0.033(3) 0.062(4) 0.038(3) -0.007(3) -0.001(3) -0.008(3)
C27 0.041(4) 0.058(4) 0.044(4) -0.012(3) 0.015(3) -0.019(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 N2 2.125(4) . ?
Pb1 N1 2.136(5) . ?
N1 C1 1.416(7) . ?
N1 C25 1.453(7) . ?
N2 C13 1.426(7) . ?
N2 C27 1.458(7) . ?
C1 C6 1.411(9) . ?
C1 C2 1.412(9) . ?
C2 C3 1.379(10) . ?
C2 C7 1.509(10) . ?
C3 C4 1.361(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.400(9) . ?
C5 H5 0.9500 . ?
C6 C10 1.521(10) . ?
C7 C8 1.469(11) . ?
C7 C9 1.528(11) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.494(10) . ?
C10 C12 1.498(10) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.404(8) . ?
C13 C14 1.403(8) . ?
C14 C15 1.385(8) . ?
C14 C19 1.499(9) . ?
C15 C16 1.365(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.367(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(9) . ?
C17 H17 0.9500 . ?
C18 C22 1.504(9) . ?
C19 C20 1.508(10) . ?
C19 C21 1.520(10) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.508(11) . ?
C22 C24 1.519(10) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.508(8) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.523(8) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?

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
N2 Pb1 N1 89.94(17) . . ?
C1 N1 C25 115.6(4) . . ?
C1 N1 Pb1 118.4(3) . . ?
C25 N1 Pb1 125.7(3) . . ?
C13 N2 C27 114.7(4) . . ?
C13 N2 Pb1 118.2(3) . . ?
C27 N2 Pb1 127.0(4) . . ?
C6 C1 N1 120.0(6) . . ?
C6 C1 C2 120.0(6) . . ?
N1 C1 C2 120.0(6) . . ?
C3 C2 C1 118.0(7) . . ?
C3 C2 C7 120.8(7) . . ?
C1 C2 C7 121.2(6) . . ?
C4 C3 C2 122.8(8) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 119.7(7) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 120.4(7) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 118.8(7) . . ?
C5 C6 C10 119.3(7) . . ?
C1 C6 C10 121.9(6) . . ?
C8 C7 C2 114.1(7) . . ?
C8 C7 C9 110.2(8) . . ?
C2 C7 C9 112.0(7) . . ?
C8 C7 H7 106.7 . . ?
C2 C7 H7 106.7 . . ?
C9 C7 H7 106.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C12 109.6(7) . . ?
C11 C10 C6 113.0(7) . . ?
C12 C10 C6 113.4(6) . . ?
C11 C10 H10 106.8 . . ?
C12 C10 H10 106.8 . . ?
C6 C10 H10 106.8 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 120.1(5) . . ?
C18 C13 N2 120.8(5) . . ?
C14 C13 N2 119.2(5) . . ?
C15 C14 C13 118.7(6) . . ?
C15 C14 C19 119.8(6) . . ?
C13 C14 C19 121.5(5) . . ?
C16 C15 C14 121.3(6) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C15 C16 C17 119.9(7) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 121.5(6) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
C17 C18 C13 118.4(6) . . ?
C17 C18 C22 119.9(6) . . ?
C13 C18 C22 121.8(6) . . ?
C14 C19 C20 111.5(6) . . ?
C14 C19 C21 112.9(6) . . ?
C20 C19 C21 110.6(7) . . ?
C14 C19 H19 107.2 . . ?
C20 C19 H19 107.2 . . ?
C21 C19 H19 107.2 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C18 112.9(7) . . ?
C23 C22 C24 109.8(7) . . ?
C18 C22 C24 111.5(6) . . ?
C23 C22 H22 107.4 . . ?
C18 C22 H22 107.4 . . ?
C24 C22 H22 107.4 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N1 C25 C26 113.6(5) . . ?
N1 C25 H25A 108.8 . . ?
C26 C25 H25A 108.8 . . ?
N1 C25 H25B 108.8 . . ?
C26 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C25 C26 C27 116.4(5) . . ?
C25 C26 H26A 108.2 . . ?
C27 C26 H26A 108.2 . . ?
C25 C26 H26B 108.2 . . ?
C27 C26 H26B 108.2 . . ?
H26A C26 H26B 107.3 . . ?
N2 C27 C26 112.6(5) . . ?
N2 C27 H27A 109.1 . . ?
C26 C27 H27A 109.1 . . ?
N2 C27 H27B 109.1 . . ?
C26 C27 H27B 109.1 . . ?
H27A C27 H27B 107.8 . . ?

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
N2 Pb1 N1 C1 -169.7(4) . . . . ?
N2 Pb1 N1 C25 3.7(5) . . . . ?
N1 Pb1 N2 C13 171.5(4) . . . . ?
N1 Pb1 N2 C27 -4.4(5) . . . . ?
C25 N1 C1 C6 -91.4(7) . . . . ?
Pb1 N1 C1 C6 82.7(6) . . . . ?
C25 N1 C1 C2 91.2(7) . . . . ?
Pb1 N1 C1 C2 -94.7(6) . . . . ?
C6 C1 C2 C3 -6.1(10) . . . . ?
N1 C1 C2 C3 171.3(6) . . . . ?
C6 C1 C2 C7 172.9(6) . . . . ?
N1 C1 C2 C7 -9.6(9) . . . . ?
C1 C2 C3 C4 2.4(12) . . . . ?
C7 C2 C3 C4 -176.7(8) . . . . ?
C2 C3 C4 C5 2.8(13) . . . . ?
C3 C4 C5 C6 -4.2(13) . . . . ?
C4 C5 C6 C1 0.4(11) . . . . ?
C4 C5 C6 C10 179.8(7) . . . . ?
N1 C1 C6 C5 -172.7(6) . . . . ?
C2 C1 C6 C5 4.8(9) . . . . ?
N1 C1 C6 C10 8.0(9) . . . . ?
C2 C1 C6 C10 -174.6(6) . . . . ?
C3 C2 C7 C8 -74.0(10) . . . . ?
C1 C2 C7 C8 107.0(9) . . . . ?
C3 C2 C7 C9 52.0(10) . . . . ?
C1 C2 C7 C9 -127.0(8) . . . . ?
C5 C6 C10 C11 66.3(9) . . . . ?
C1 C6 C10 C11 -114.4(8) . . . . ?
C5 C6 C10 C12 -59.2(9) . . . . ?
C1 C6 C10 C12 120.2(7) . . . . ?
C27 N2 C13 C18 92.7(7) . . . . ?
Pb1 N2 C13 C18 -83.6(6) . . . . ?
C27 N2 C13 C14 -87.9(7) . . . . ?
Pb1 N2 C13 C14 95.8(5) . . . . ?
C18 C13 C14 C15 3.6(9) . . . . ?
N2 C13 C14 C15 -175.8(5) . . . . ?
C18 C13 C14 C19 -178.2(6) . . . . ?
N2 C13 C14 C19 2.4(9) . . . . ?
C13 C14 C15 C16 -0.5(10) . . . . ?
C19 C14 C15 C16 -178.8(7) . . . . ?
C14 C15 C16 C17 -1.9(12) . . . . ?
C15 C16 C17 C18 1.3(12) . . . . ?
C16 C17 C18 C13 1.7(11) . . . . ?
C16 C17 C18 C22 -176.1(7) . . . . ?
C14 C13 C18 C17 -4.2(9) . . . . ?
N2 C13 C18 C17 175.2(6) . . . . ?
C14 C13 C18 C22 173.6(6) . . . . ?
N2 C13 C18 C22 -7.0(9) . . . . ?
C15 C14 C19 C20 76.5(8) . . . . ?
C13 C14 C19 C20 -101.7(7) . . . . ?
C15 C14 C19 C21 -48.8(10) . . . . ?
C13 C14 C19 C21 133.0(8) . . . . ?
C17 C18 C22 C23 -52.9(10) . . . . ?
C13 C18 C22 C23 129.4(8) . . . . ?
C17 C18 C22 C24 71.4(9) . . . . ?
C13 C18 C22 C24 -106.4(8) . . . . ?
C1 N1 C25 C26 -158.9(5) . . . . ?
Pb1 N1 C25 C26 27.5(7) . . . . ?
N1 C25 C26 C27 -68.4(7) . . . . ?
C13 N2 C27 C26 158.3(5) . . . . ?
Pb1 N2 C27 C26 -25.8(8) . . . . ?
C25 C26 C27 N2 67.0(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.995
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.134