# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_x

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H12 N28 O2 Pb2'
_chemical_formula_weight         994.88

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           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   13.8054(14)
_cell_length_b                   13.8054(14)
_cell_length_c                   27.530(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5246.8(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2765
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      26.62

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3680
_exptl_absorpt_coefficient_mu    12.893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.095
_exptl_absorpt_correction_T_max  0.275
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13609
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_sigmaI/netI    0.0648
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         26.16
_reflns_number_total             2598
_reflns_number_gt                2168
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00062(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2598
_refine_ls_number_parameters     207
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0633
_refine_ls_wR_factor_gt          0.0611
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_restrained_S_all      0.903
_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 0.23782(2) 0.51418(2) 0.105914(10) 0.02017(11) Uani 1 1 d . . .
O1 O 0.2466(3) 0.5171(4) 0.0071(2) 0.0357(14) Uani 1 1 d . . .
H1A H 0.2386 0.4684 -0.0113 0.054 Uiso 1 1 d R . .
H1B H 0.2586 0.5745 -0.0024 0.054 Uiso 1 1 d R . .
N1 N 0.2041(6) 0.3289(5) 0.0763(3) 0.0306(18) Uani 1 1 d . . .
N2 N 0.1643(6) 0.2865(5) 0.0374(3) 0.0345(19) Uani 1 1 d . . .
N3 N 0.1658(5) 0.1918(5) 0.0434(3) 0.0332(19) Uani 1 1 d . . .
N4 N 0.2106(5) 0.1712(5) 0.0856(2) 0.0285(17) Uani 1 1 d . . .
N5 N 0.3106(6) 0.1917(5) 0.1775(3) 0.0330(19) Uani 1 1 d . . .
N6 N 0.3524(6) 0.3278(5) 0.2094(3) 0.0294(17) Uani 1 1 d D . .
H6 H 0.382(6) 0.376(4) 0.225(3) 0.044 Uiso 1 1 d D . .
N7 N 0.3041(5) 0.3530(4) 0.1685(2) 0.0294(17) Uani 1 1 d . . .
N8 N 0.1959(6) 0.6751(5) 0.1641(3) 0.0321(18) Uani 1 1 d . . .
N9 N 0.1533(6) 0.6989(5) 0.2068(3) 0.037(2) Uani 1 1 d . . .
N10 N 0.1639(5) 0.7925(5) 0.2143(3) 0.0327(19) Uani 1 1 d . . .
N11 N 0.2133(5) 0.8322(4) 0.1772(3) 0.0295(17) Uani 1 1 d . . .
N12 N 0.3187(5) 0.8477(5) 0.0854(3) 0.0294(17) Uani 1 1 d . . .
N13 N 0.3614(5) 0.8209(5) 0.0436(3) 0.0294(17) Uani 1 1 d D . .
H13 H 0.391(6) 0.862(5) 0.023(3) 0.044 Uiso 1 1 d D . .
N14 N 0.3012(6) 0.6886(5) 0.0742(3) 0.0307(18) Uani 1 1 d . . .
C1 C 0.2309(6) 0.2559(5) 0.1042(3) 0.0176(17) Uani 1 1 d . . .
C2 C 0.2815(6) 0.2678(5) 0.1507(3) 0.0228(19) Uani 1 1 d . . .
C3 C 0.3561(7) 0.2331(6) 0.2146(3) 0.030(2) Uani 1 1 d . . .
H3A H 0.3857 0.2004 0.2401 0.036 Uiso 1 1 calc R . .
C4 C 0.2307(6) 0.7593(5) 0.1476(3) 0.0199(18) Uani 1 1 d . . .
C5 C 0.2825(6) 0.7660(5) 0.1022(3) 0.0208(18) Uani 1 1 d . . .
C6 C 0.3504(7) 0.7263(6) 0.0374(3) 0.033(2) Uani 1 1 d . . .
H6A H 0.3738 0.6914 0.0110 0.040 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 0.01881(18) 0.01819(17) 0.02352(16) -0.00066(11) -0.00009(10) -0.00030(9)
O1 0.045(4) 0.034(3) 0.028(3) -0.005(2) -0.001(2) 0.000(3)
N1 0.048(5) 0.018(4) 0.026(4) 0.003(3) -0.019(4) -0.003(3)
N2 0.045(5) 0.034(5) 0.024(5) 0.000(3) -0.020(4) -0.004(4)
N3 0.046(5) 0.029(4) 0.025(5) -0.003(3) -0.020(4) -0.002(4)
N4 0.043(5) 0.020(4) 0.023(4) -0.001(3) -0.011(4) 0.000(3)
N5 0.058(5) 0.017(4) 0.024(5) 0.002(3) -0.020(4) -0.003(3)
N6 0.042(5) 0.026(4) 0.020(4) -0.007(3) -0.016(3) -0.003(3)
N7 0.050(5) 0.019(4) 0.020(4) -0.004(3) -0.014(3) 0.001(3)
N8 0.047(5) 0.025(4) 0.025(4) -0.001(3) 0.017(4) -0.002(3)
N9 0.055(5) 0.030(4) 0.026(5) 0.002(4) 0.019(4) -0.002(4)
N10 0.043(5) 0.030(4) 0.025(5) -0.002(3) 0.023(4) -0.001(4)
N11 0.041(5) 0.016(3) 0.032(5) -0.003(3) 0.014(4) -0.002(3)
N12 0.039(4) 0.025(4) 0.024(4) 0.001(3) 0.017(3) 0.000(3)
N13 0.034(4) 0.031(4) 0.023(5) 0.007(3) 0.014(3) 0.000(3)
N14 0.050(5) 0.016(4) 0.026(5) -0.004(3) 0.015(4) -0.001(3)
C1 0.033(5) 0.007(3) 0.013(4) 0.001(3) -0.007(4) -0.004(3)
C2 0.031(5) 0.018(4) 0.019(5) 0.000(3) -0.009(4) -0.002(4)
C3 0.049(6) 0.024(5) 0.018(5) 0.013(4) -0.016(4) -0.002(4)
C4 0.028(4) 0.015(4) 0.016(5) -0.002(3) 0.009(4) 0.008(4)
C5 0.030(5) 0.009(4) 0.024(5) -0.001(3) 0.006(4) 0.001(3)
C6 0.046(6) 0.027(5) 0.026(6) -0.001(4) 0.024(4) 0.002(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 N14 2.707(7) . ?
Pb1 N5 2.721(7) 12_666 ?
Pb1 O1 2.722(6) . ?
Pb1 N1 2.724(6) . ?
Pb1 N11 2.738(6) 12_766 ?
Pb1 N8 2.800(7) . ?
O1 H1A 0.8502 . ?
O1 H1B 0.8500 . ?
N1 C1 1.320(9) . ?
N1 N2 1.340(9) . ?
N2 N3 1.318(9) . ?
N3 N4 1.346(9) . ?
N4 C1 1.307(9) . ?
N5 C3 1.327(10) . ?
N5 C2 1.345(10) . ?
N5 Pb1 2.721(7) 15 ?
N6 C3 1.316(10) . ?
N6 N7 1.355(9) . ?
N6 H6 0.888(10) . ?
N7 C2 1.311(9) . ?
N8 C4 1.337(10) . ?
N8 N9 1.354(9) . ?
N9 N10 1.316(9) . ?
N10 N11 1.345(9) . ?
N11 C4 1.316(10) . ?
N11 Pb1 2.738(6) 15_565 ?
N12 C5 1.317(9) . ?
N12 N13 1.345(9) . ?
N13 C6 1.326(11) . ?
N13 H13 0.892(10) . ?
N14 C6 1.325(10) . ?
N14 C5 1.344(9) . ?
C1 C2 1.468(10) . ?
C3 H3A 0.9300 . ?
C4 C5 1.443(10) . ?
C6 H6A 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
N14 Pb1 N5 88.6(2) . 12_666 ?
N14 Pb1 O1 69.50(19) . . ?
N5 Pb1 O1 72.49(18) 12_666 . ?
N14 Pb1 N1 142.6(2) . . ?
N5 Pb1 N1 88.0(2) 12_666 . ?
O1 Pb1 N1 73.93(18) . . ?
N14 Pb1 N11 80.1(2) . 12_766 ?
N5 Pb1 N11 140.8(2) 12_666 12_766 ?
O1 Pb1 N11 68.34(17) . 12_766 ?
N1 Pb1 N11 79.3(2) . 12_766 ?
N14 Pb1 N8 63.0(2) . . ?
N5 Pb1 N8 79.5(2) 12_666 . ?
O1 Pb1 N8 124.68(18) . . ?
N1 Pb1 N8 151.7(2) . . ?
N11 Pb1 N8 125.6(2) 12_766 . ?
Pb1 O1 H1A 125.4 . . ?
Pb1 O1 H1B 109.3 . . ?
H1A O1 H1B 125.3 . . ?
C1 N1 N2 104.3(6) . . ?
C1 N1 Pb1 119.7(5) . . ?
N2 N1 Pb1 136.0(5) . . ?
N3 N2 N1 109.0(7) . . ?
N2 N3 N4 109.0(6) . . ?
C1 N4 N3 104.3(6) . . ?
C3 N5 C2 103.1(7) . . ?
C3 N5 Pb1 139.8(5) . 15 ?
C2 N5 Pb1 117.1(5) . 15 ?
C3 N6 N7 111.4(7) . . ?
C3 N6 H6 132(6) . . ?
N7 N6 H6 116(6) . . ?
C2 N7 N6 101.3(6) . . ?
C4 N8 N9 103.9(7) . . ?
C4 N8 Pb1 114.9(5) . . ?
N9 N8 Pb1 141.1(5) . . ?
N10 N9 N8 109.0(7) . . ?
N9 N10 N11 109.7(7) . . ?
C4 N11 N10 104.5(6) . . ?
C4 N11 Pb1 116.2(5) . 15_565 ?
N10 N11 Pb1 138.8(5) . 15_565 ?
C5 N12 N13 103.4(6) . . ?
C6 N13 N12 109.3(7) . . ?
C6 N13 H13 127(6) . . ?
N12 N13 H13 124(6) . . ?
C6 N14 C5 103.0(7) . . ?
C6 N14 Pb1 139.6(6) . . ?
C5 N14 Pb1 117.4(5) . . ?
N4 C1 N1 113.3(7) . . ?
N4 C1 C2 122.9(7) . . ?
N1 C1 C2 123.7(7) . . ?
N7 C2 N5 115.2(7) . . ?
N7 C2 C1 122.6(7) . . ?
N5 C2 C1 122.2(7) . . ?
N6 C3 N5 109.0(7) . . ?
N6 C3 H3A 125.5 . . ?
N5 C3 H3A 125.5 . . ?
N11 C4 N8 112.9(7) . . ?
N11 C4 C5 125.2(7) . . ?
N8 C4 C5 121.8(7) . . ?
N12 C5 N14 113.9(7) . . ?
N12 C5 C4 123.2(7) . . ?
N14 C5 C4 122.8(7) . . ?
N14 C6 N13 110.3(7) . . ?
N14 C6 H6A 124.8 . . ?
N13 C6 H6A 124.8 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.16
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.859
_refine_diff_density_min         -1.400
_refine_diff_density_rms         0.178
_database_code_depnum_ccdc_archive 'CCDC 980107'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_x

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H3 N7 O Pb'

_chemical_formula_weight         360.31

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   'P2(1)/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                   3.9010(16)
_cell_length_b                   23.862(10)
_cell_length_c                   7.561(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.419(6)
_cell_angle_gamma                90.00
_cell_volume                     681.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_absorpt_coefficient_mu    24.710
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3402
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0910
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         27.43
_reflns_number_total             1502
_reflns_number_gt                1329
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1700P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1502
_refine_ls_number_parameters     110
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0731
_refine_ls_wR_factor_ref         0.2200
_refine_ls_wR_factor_gt          0.2065
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.034
_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 0.6334(3) 0.47395(4) 0.78042(12) 0.0208(4) Uani 1 1 d . . .
O1 O 0.239(5) 0.4559(6) 0.966(2) 0.015(3) Uani 1 1 d U . .
N3 N 0.395(7) 0.2794(10) 0.620(3) 0.029(6) Uani 1 1 d . . .
N1 N 0.592(6) 0.3602(9) 0.771(3) 0.021(4) Uani 1 1 d . . .
N2 N 0.660(8) 0.2686(11) 0.777(3) 0.034(6) Uani 1 1 d . . .
H2A H 0.7426 0.2358 0.8107 0.041 Uiso 1 1 calc R . .
N4 N 0.086(6) 0.4225(8) 0.495(3) 0.027(5) Uani 1 1 d U . .
N5 N -0.158(5) 0.4336(8) 0.329(3) 0.018(4) Uani 1 1 d . . .
N6 N -0.276(6) 0.3880(10) 0.249(4) 0.033(6) Uani 1 1 d . . .
H6A H -0.4423 0.3857 0.1505 0.040 Uiso 1 1 calc R . .
N7 N -0.106(8) 0.3446(9) 0.339(3) 0.028(5) Uani 1 1 d . . .
C1 C 0.770(7) 0.3155(11) 0.870(4) 0.027(6) Uani 1 1 d . . .
H1A H 0.9366 0.3179 0.9813 0.032 Uiso 1 1 calc R . .
C2 C 0.370(7) 0.3352(10) 0.629(3) 0.020(5) Uani 1 1 d . . .
C3 C 0.122(8) 0.3671(12) 0.485(5) 0.032(7) 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
Pb1 0.0156(5) 0.0228(5) 0.0209(5) -0.0022(3) -0.0012(5) -0.0007(5)
O1 0.016(5) 0.016(5) 0.013(4) -0.011(4) 0.003(4) -0.001(4)
N3 0.024(14) 0.030(12) 0.026(12) 0.002(10) -0.008(9) 0.003(9)
N1 0.024(12) 0.018(10) 0.022(10) -0.005(8) 0.004(9) 0.002(9)
N2 0.028(14) 0.033(13) 0.036(14) 0.006(10) -0.001(13) 0.010(12)
N4 0.029(7) 0.023(6) 0.027(6) -0.006(5) 0.004(4) 0.002(4)
N5 0.025(12) 0.019(10) 0.018(10) 0.007(8) 0.018(9) 0.009(8)
N6 0.026(12) 0.024(12) 0.036(14) 0.010(10) -0.021(10) -0.004(9)
N7 0.035(13) 0.031(11) 0.017(10) -0.001(9) 0.004(11) 0.000(12)
C1 0.027(14) 0.023(13) 0.026(15) 0.004(11) -0.003(10) 0.014(10)
C2 0.030(15) 0.021(12) 0.011(11) 0.003(8) 0.008(10) 0.008(11)
C3 0.024(13) 0.023(13) 0.043(18) -0.004(13) -0.004(11) -0.011(10)

_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 O1 2.363(17) . ?
Pb1 O1 2.466(17) 1_655 ?
Pb1 O1 2.502(13) 3_667 ?
Pb1 N1 2.72(2) . ?
O1 Pb1 2.466(17) 1_455 ?
O1 Pb1 2.502(13) 3_667 ?
N3 C2 1.34(3) . ?
N3 N2 1.39(3) . ?
N1 C2 1.34(3) . ?
N1 C1 1.39(3) . ?
N2 C1 1.33(4) . ?
N2 H2A 0.8600 . ?
N4 C3 1.33(3) . ?
N4 N5 1.40(3) . ?
N5 N6 1.27(3) . ?
N6 N7 1.32(3) . ?
N6 H6A 0.8600 . ?
N7 C3 1.35(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.48(4) . ?

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
O1 Pb1 O1 107.8(6) . 1_655 ?
O1 Pb1 O1 72.6(6) . 3_667 ?
O1 Pb1 O1 72.6(6) 1_655 3_667 ?
O1 Pb1 N1 77.9(6) . . ?
O1 Pb1 N1 83.3(6) 1_655 . ?
O1 Pb1 N1 133.4(6) 3_667 . ?
Pb1 O1 Pb1 107.8(6) . 1_455 ?
Pb1 O1 Pb1 107.4(6) . 3_667 ?
Pb1 O1 Pb1 107.4(6) 1_455 3_667 ?
C2 N3 N2 101(2) . . ?
C2 N1 C1 103(2) . . ?
C2 N1 Pb1 119.4(16) . . ?
C1 N1 Pb1 137.3(18) . . ?
C1 N2 N3 111(2) . . ?
C1 N2 H2A 124.3 . . ?
N3 N2 H2A 124.3 . . ?
C3 N4 N5 101(2) . . ?
N6 N5 N4 110.3(19) . . ?
N5 N6 N7 110(2) . . ?
N5 N6 H6A 124.8 . . ?
N7 N6 H6A 124.8 . . ?
N6 N7 C3 105(2) . . ?
N2 C1 N1 108(2) . . ?
N2 C1 H1A 125.9 . . ?
N1 C1 H1A 125.9 . . ?
N3 C2 N1 116(2) . . ?
N3 C2 C3 121(2) . . ?
N1 C2 C3 122(2) . . ?
N4 C3 N7 113(3) . . ?
N4 C3 C2 122(3) . . ?
N7 C3 C2 125(2) . . ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         4.202
_refine_diff_density_min         -5.859
_refine_diff_density_rms         0.707
_database_code_depnum_ccdc_archive 'CCDC 980108'
