# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_t
_database_code_depnum_ccdc_archive 'CCDC 1413198'
_audit_update_record             
;
2015-07-16 deposited with the CCDC.
2015-09-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 N10 O4 Pb, 3(H2 O)'
_chemical_formula_sum            'C12 H22 N10 O7 Pb'
_chemical_formula_weight         625.59

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

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

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

_cell_length_a                   8.1250(16)
_cell_length_b                   10.772(2)
_cell_length_c                   12.866(3)
_cell_angle_alpha                70.45(3)
_cell_angle_beta                 76.89(3)
_cell_angle_gamma                89.02(3)
_cell_volume                     1031.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             604
_exptl_absorpt_coefficient_mu    8.237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2896
_exptl_absorpt_correction_T_max  0.3036
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      291(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            10658
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4695
_reflns_number_gt                4170
_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    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.1000P)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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4695
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.1089
_refine_ls_wR_factor_gt          0.1013
_refine_ls_goodness_of_fit_ref   0.786
_refine_ls_restrained_S_all      0.786
_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 0.94826(3) 0.29763(2) 0.231803(18) 0.02625(10) Uani 1 1 d . . .
N6 N 0.8013(7) 0.0978(5) 0.2085(5) 0.0331(12) Uani 1 1 d . . .
N7 N 0.5479(7) -0.2074(5) 0.0415(4) 0.0311(11) Uani 1 1 d . . .
N3 N 1.6486(7) 0.7527(5) 0.4334(5) 0.0322(12) Uani 1 1 d . . .
N1 N 1.1930(6) 0.3976(5) 0.2890(5) 0.0300(11) Uani 1 1 d . . .
N2 N 1.5021(7) 0.6954(5) 0.4337(5) 0.0317(12) Uani 1 1 d . . .
N8 N 0.4085(7) -0.2690(5) 0.0361(5) 0.0368(13) Uani 1 1 d . . .
N5 N 1.7152(7) 0.6325(5) 0.3255(4) 0.0319(12) Uani 1 1 d . . .
C6 C 1.5458(7) 0.6230(6) 0.3673(5) 0.0251(12) Uani 1 1 d . . .
C7 C 0.8701(8) 0.0258(7) 0.1453(6) 0.0354(15) Uani 1 1 d . . .
H7A H 0.9873 0.0309 0.1205 0.043 Uiso 1 1 calc R . .
N10 N 0.3252(7) -0.1682(5) 0.1581(5) 0.0333(12) Uani 1 1 d . . .
C9 C 0.6003(8) -0.0642(5) 0.1486(5) 0.0245(12) Uani 1 1 d . . .
N9 N 0.2758(7) -0.2473(6) 0.1076(5) 0.0381(13) Uani 1 1 d . . .
C3 C 1.4259(7) 0.5446(5) 0.3410(5) 0.0231(11) Uani 1 1 d . . .
N4 N 1.7730(7) 0.7139(6) 0.3706(5) 0.0359(13) Uani 1 1 d . . .
C1 C 1.1429(8) 0.4646(6) 0.3585(6) 0.0354(15) Uani 1 1 d . . .
H1A H 1.0275 0.4611 0.3905 0.043 Uiso 1 1 calc R . .
C11 C 0.6320(8) 0.0866(6) 0.2456(6) 0.0338(14) Uani 1 1 d . . .
H11A H 0.5819 0.1335 0.2922 0.041 Uiso 1 1 calc R . .
C12 C 0.4924(8) -0.1460(6) 0.1156(5) 0.0261(12) Uani 1 1 d . . .
C5 C 1.3611(8) 0.4028(6) 0.2454(6) 0.0350(14) Uani 1 1 d . . .
H5A H 1.3995 0.3562 0.1963 0.042 Uiso 1 1 calc R . .
C2 C 1.2505(8) 0.5401(6) 0.3873(5) 0.0319(13) Uani 1 1 d . . .
H2A H 1.2078 0.5864 0.4360 0.038 Uiso 1 1 calc R . .
C8 C 0.7756(8) -0.0562(6) 0.1147(5) 0.0314(13) Uani 1 1 d . . .
H8A H 0.8296 -0.1057 0.0715 0.038 Uiso 1 1 calc R . .
C4 C 1.4789(8) 0.4725(6) 0.2688(6) 0.0337(14) Uani 1 1 d . . .
H4A H 1.5935 0.4717 0.2367 0.040 Uiso 1 1 calc R . .
C10 C 0.5284(8) 0.0078(6) 0.2171(6) 0.0324(14) Uani 1 1 d . . .
H10A H 0.4115 0.0035 0.2438 0.039 Uiso 1 1 calc R . .
O5 O 0.0427(6) 0.3902(5) 0.8585(4) 0.0386(11) Uani 1 1 d . . .
H5C H 0.0576 0.4646 0.8657 0.058 Uiso 1 1 d R . .
H5B H -0.0532 0.3851 0.8437 0.058 Uiso 1 1 d R . .
O6 O 0.0832(6) 0.8507(5) 0.3467(4) 0.0396(11) Uani 1 1 d . . .
H6A H 0.0171 0.8824 0.3030 0.059 Uiso 1 1 d R . .
H6B H 0.0265 0.8232 0.4152 0.059 Uiso 1 1 d R . .
O1 O 1.1529(6) 0.3126(5) 0.0511(4) 0.0379(11) Uani 1 1 d . . .
H1B H 1.2217 0.2521 0.0644 0.057 Uiso 1 1 d R . .
H1C H 1.0993 0.3027 0.0046 0.057 Uiso 1 1 d R . .
O4 O 0.7525(6) 0.4022(5) 0.0724(4) 0.0407(11) Uani 1 1 d . . .
H4B H 0.8082 0.4040 0.0074 0.061 Uiso 1 1 d R . .
H4C H 0.6616 0.3538 0.0915 0.061 Uiso 1 1 d R . .
O2 O 1.1063(6) 0.1157(5) 0.3059(5) 0.0458(13) Uani 1 1 d . . .
H2B H 1.1836 0.1161 0.2489 0.069 Uiso 1 1 d R . .
H2C H 1.1506 0.1293 0.3553 0.069 Uiso 1 1 d R . .
O3 O 0.7899(7) 0.2142(5) 0.4539(4) 0.0460(12) Uani 1 1 d . . .
H3B H 0.7953 0.2762 0.4803 0.069 Uiso 1 1 d R . .
H3A H 0.6868 0.1921 0.4615 0.069 Uiso 1 1 d R . .
O7 O 0.2990(8) 0.0777(5) 0.4544(5) 0.0585(16) Uani 1 1 d . . .
H7B H 0.3895 0.1262 0.4364 0.088 Uiso 1 1 d R . .
H7C H 0.2893 0.0210 0.5203 0.088 Uiso 1 1 d R . .


_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 O2 2.370(5) . ?
Pb1 O1 2.490(5) . ?
Pb1 N6 2.614(5) . ?
Pb1 N1 2.631(5) . ?
Pb1 O3 2.698(5) . ?
N6 C7 1.333(8) . ?
N6 C11 1.343(8) . ?
N7 C12 1.329(8) . ?
N7 N8 1.350(7) . ?
N3 N4 1.300(8) . ?
N3 N2 1.349(7) . ?
N1 C1 1.321(8) . ?
N1 C5 1.348(8) . ?
N2 C6 1.327(8) . ?
N8 N9 1.322(8) . ?
N5 N4 1.343(7) . ?
N5 C6 1.351(8) . ?
C6 C3 1.465(7) . ?
C7 C8 1.384(8) . ?
C7 H7A 0.9300 . ?
N10 C12 1.337(8) . ?
N10 N9 1.345(7) . ?
C9 C8 1.387(8) . ?
C9 C10 1.389(9) . ?
C9 C12 1.473(7) . ?
C3 C4 1.392(8) . ?
C3 C2 1.410(8) . ?
C1 C2 1.391(8) . ?
C1 H1A 0.9300 . ?
C11 C10 1.391(8) . ?
C11 H11A 0.9300 . ?
C5 C4 1.370(8) . ?
C5 H5A 0.9300 . ?
C2 H2A 0.9300 . ?
C8 H8A 0.9300 . ?
C4 H4A 0.9300 . ?
C10 H10A 0.9300 . ?
O5 H5C 0.8502 . ?
O5 H5B 0.8499 . ?
O6 H6A 0.8499 . ?
O6 H6B 0.8500 . ?
O1 H1B 0.8501 . ?
O1 H1C 0.8505 . ?
O4 H4B 0.8502 . ?
O4 H4C 0.8500 . ?
O2 H2B 0.8500 . ?
O2 H2C 0.8500 . ?
O3 H3B 0.8499 . ?
O3 H3A 0.8501 . ?
O7 H7B 0.8501 . ?
O7 H7C 0.8501 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Pb1 O1 82.13(18) . . ?
O2 Pb1 N6 75.45(17) . . ?
O1 Pb1 N6 85.82(17) . . ?
O2 Pb1 N1 75.04(16) . . ?
O1 Pb1 N1 87.92(16) . . ?
N6 Pb1 N1 150.40(17) . . ?
O2 Pb1 O3 78.71(19) . . ?
O1 Pb1 O3 160.84(17) . . ?
N6 Pb1 O3 89.79(17) . . ?
N1 Pb1 O3 86.73(17) . . ?
C7 N6 C11 117.4(5) . . ?
C7 N6 Pb1 126.8(4) . . ?
C11 N6 Pb1 114.3(4) . . ?
C12 N7 N8 105.1(5) . . ?
N4 N3 N2 108.8(5) . . ?
C1 N1 C5 116.4(5) . . ?
C1 N1 Pb1 115.2(4) . . ?
C5 N1 Pb1 127.9(4) . . ?
C6 N2 N3 105.3(5) . . ?
N9 N8 N7 109.0(5) . . ?
N4 N5 C6 103.8(5) . . ?
N2 C6 N5 111.3(5) . . ?
N2 C6 C3 124.5(5) . . ?
N5 C6 C3 124.2(5) . . ?
N6 C7 C8 123.3(6) . . ?
N6 C7 H7A 118.4 . . ?
C8 C7 H7A 118.4 . . ?
C12 N10 N9 104.9(5) . . ?
C8 C9 C10 117.1(5) . . ?
C8 C9 C12 122.5(6) . . ?
C10 C9 C12 120.5(5) . . ?
N8 N9 N10 109.3(5) . . ?
C4 C3 C2 117.1(5) . . ?
C4 C3 C6 122.0(5) . . ?
C2 C3 C6 121.0(5) . . ?
N3 N4 N5 110.8(5) . . ?
N1 C1 C2 124.6(6) . . ?
N1 C1 H1A 117.7 . . ?
C2 C1 H1A 117.7 . . ?
N6 C11 C10 122.7(6) . . ?
N6 C11 H11A 118.7 . . ?
C10 C11 H11A 118.7 . . ?
N7 C12 N10 111.7(5) . . ?
N7 C12 C9 124.7(6) . . ?
N10 C12 C9 123.5(6) . . ?
N1 C5 C4 124.1(6) . . ?
N1 C5 H5A 118.0 . . ?
C4 C5 H5A 118.0 . . ?
C1 C2 C3 118.3(6) . . ?
C1 C2 H2A 120.8 . . ?
C3 C2 H2A 120.8 . . ?
C7 C8 C9 119.8(6) . . ?
C7 C8 H8A 120.1 . . ?
C9 C8 H8A 120.1 . . ?
C5 C4 C3 119.6(6) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C9 C10 C11 119.7(6) . . ?
C9 C10 H10A 120.1 . . ?
C11 C10 H10A 120.1 . . ?
H5C O5 H5B 109.5 . . ?
H6A O6 H6B 109.5 . . ?
Pb1 O1 H1B 109.2 . . ?
Pb1 O1 H1C 109.4 . . ?
H1B O1 H1C 109.5 . . ?
H4B O4 H4C 109.5 . . ?
Pb1 O2 H2B 103.9 . . ?
Pb1 O2 H2C 109.3 . . ?
H2B O2 H2C 109.7 . . ?
Pb1 O3 H3B 109.5 . . ?
Pb1 O3 H3A 109.4 . . ?
H3B O3 H3A 109.5 . . ?
H7B O7 H7C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Pb1 N6 C7 -62.8(5) . . . . ?
O1 Pb1 N6 C7 20.2(5) . . . . ?
N1 Pb1 N6 C7 -58.2(7) . . . . ?
O3 Pb1 N6 C7 -141.2(6) . . . . ?
O2 Pb1 N6 C11 131.8(5) . . . . ?
O1 Pb1 N6 C11 -145.3(5) . . . . ?
N1 Pb1 N6 C11 136.4(5) . . . . ?
O3 Pb1 N6 C11 53.4(5) . . . . ?
O2 Pb1 N1 C1 -125.3(5) . . . . ?
O1 Pb1 N1 C1 152.3(5) . . . . ?
N6 Pb1 N1 C1 -129.9(5) . . . . ?
O3 Pb1 N1 C1 -46.1(5) . . . . ?
O2 Pb1 N1 C5 63.8(5) . . . . ?
O1 Pb1 N1 C5 -18.6(5) . . . . ?
N6 Pb1 N1 C5 59.2(7) . . . . ?
O3 Pb1 N1 C5 143.0(6) . . . . ?
N4 N3 N2 C6 -0.9(7) . . . . ?
C12 N7 N8 N9 -1.7(7) . . . . ?
N3 N2 C6 N5 0.3(7) . . . . ?
N3 N2 C6 C3 -178.9(5) . . . . ?
N4 N5 C6 N2 0.4(7) . . . . ?
N4 N5 C6 C3 179.5(5) . . . . ?
C11 N6 C7 C8 1.5(10) . . . . ?
Pb1 N6 C7 C8 -163.5(5) . . . . ?
N7 N8 N9 N10 1.8(7) . . . . ?
C12 N10 N9 N8 -1.2(7) . . . . ?
N2 C6 C3 C4 178.7(6) . . . . ?
N5 C6 C3 C4 -0.3(9) . . . . ?
N2 C6 C3 C2 -0.6(9) . . . . ?
N5 C6 C3 C2 -179.6(6) . . . . ?
N2 N3 N4 N5 1.2(7) . . . . ?
C6 N5 N4 N3 -1.0(7) . . . . ?
C5 N1 C1 C2 1.0(10) . . . . ?
Pb1 N1 C1 C2 -171.0(5) . . . . ?
C7 N6 C11 C10 -2.4(10) . . . . ?
Pb1 N6 C11 C10 164.5(5) . . . . ?
N8 N7 C12 N10 1.0(7) . . . . ?
N8 N7 C12 C9 -179.5(5) . . . . ?
N9 N10 C12 N7 0.1(7) . . . . ?
N9 N10 C12 C9 -179.4(5) . . . . ?
C8 C9 C12 N7 -7.8(9) . . . . ?
C10 C9 C12 N7 172.8(6) . . . . ?
C8 C9 C12 N10 171.6(6) . . . . ?
C10 C9 C12 N10 -7.8(9) . . . . ?
C1 N1 C5 C4 -0.2(10) . . . . ?
Pb1 N1 C5 C4 170.6(5) . . . . ?
N1 C1 C2 C3 -1.0(10) . . . . ?
C4 C3 C2 C1 0.1(9) . . . . ?
C6 C3 C2 C1 179.5(6) . . . . ?
N6 C7 C8 C9 1.1(11) . . . . ?
C10 C9 C8 C7 -2.8(9) . . . . ?
C12 C9 C8 C7 177.8(6) . . . . ?
N1 C5 C4 C3 -0.6(11) . . . . ?
C2 C3 C4 C5 0.6(9) . . . . ?
C6 C3 C4 C5 -178.7(6) . . . . ?
C8 C9 C10 C11 1.9(9) . . . . ?
C12 C9 C10 C11 -178.7(6) . . . . ?
N6 C11 C10 C9 0.7(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.819
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.171
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_t
_database_code_depnum_ccdc_archive 'CCDC 1413199'
_audit_update_record             
;
2015-07-16 deposited with the CCDC.
2015-09-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H12 N10 O4 Pb'
_chemical_formula_sum            'C16 H12 N10 O4 Pb'
_chemical_formula_weight         615.55

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   'P 21/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                   12.9920(15)
_cell_length_b                   4.9834(6)
_cell_length_c                   15.3611(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.3490(17)
_cell_angle_gamma                90.00
_cell_volume                     938.37(19)
_cell_formula_units_Z            2
_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          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_absorpt_coefficient_mu    9.041
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.2202
_exptl_absorpt_correction_T_max  0.2650
_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6275
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.57
_diffrn_reflns_theta_max         26.37
_reflns_number_total             1908
_reflns_number_gt                1698
_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)+(0.0570P)²+29.0643P] 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         1908
_refine_ls_number_parameters     142
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0715
_refine_ls_wR_factor_ref         0.1856
_refine_ls_wR_factor_gt          0.1827
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_restrained_S_all      1.197
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.003

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 1.0000 0.5000 0.0000 0.03640(13) Uani 1 2 d SU . .
N1 N 0.9727(6) 0.9186(15) 0.3036(5) 0.0291(16) Uani 1 1 d U . .
N5 N 0.6640(7) 1.0880(18) 0.4356(6) 0.0384(19) Uani 1 1 d U . .
C3 C 0.9532(7) 1.0888(19) 0.3636(5) 0.0284(17) Uani 1 1 d U . .
O1 O 1.1077(6) 0.8925(19) 0.0896(6) 0.0582(19) Uani 1 1 d U . .
N2 N 1.0733(7) 0.9860(16) 0.3080(6) 0.0390(18) Uani 1 1 d U . .
C8 C 0.8404(8) 1.272(2) 0.4509(7) 0.039(2) Uani 1 1 d U . .
H8 H 0.8953 1.3933 0.4798 0.047 Uiso 1 1 calc R . .
O2 O 1.0729(8) 1.2602(17) 0.1557(6) 0.059(2) Uani 1 1 d U . .
C5 C 0.7704(8) 0.907(2) 0.3482(7) 0.038(2) Uani 1 1 d U . .
H5 H 0.7774 0.7801 0.3061 0.045 Uiso 1 1 calc R . .
N4 N 1.0397(8) 1.255(2) 0.4016(6) 0.052(2) Uani 1 1 d U . .
C7 C 0.7435(9) 1.263(2) 0.4706(7) 0.047(2) Uani 1 1 d U . .
H7 H 0.7337 1.3907 0.5114 0.057 Uiso 1 1 calc R . .
C2 C 1.1284(8) 0.875(2) 0.2497(8) 0.041(2) Uani 1 1 d U . .
H2A H 1.1091 0.6866 0.2387 0.050 Uiso 1 1 calc R . .
H2B H 1.2066 0.8852 0.2809 0.050 Uiso 1 1 calc R . .
N3 N 1.1143(7) 1.188(2) 0.3641(6) 0.046(2) Uani 1 1 d U . .
C1 C 1.0987(8) 1.023(2) 0.1564(7) 0.039(2) Uani 1 1 d U . .
C4 C 0.8515(8) 1.0903(19) 0.3862(6) 0.0305(17) Uani 1 1 d U . .
C6 C 0.6774(10) 0.914(3) 0.3740(8) 0.050(3) Uani 1 1 d U . .
H6 H 0.6219 0.7913 0.3472 0.060 Uiso 1 1 calc R . .


_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 2.530(8) 3_765 ?
Pb1 O1 2.530(8) . ?
Pb1 O2 2.558(8) 3_775 ?
Pb1 O2 2.558(8) 1_545 ?
Pb1 N5 2.666(9) 4_675 ?
Pb1 N5 2.666(9) 2_645 ?
N1 N2 1.329(12) . ?
N1 C3 1.337(12) . ?
N5 C7 1.323(14) . ?
N5 C6 1.337(16) . ?
N5 Pb1 2.666(9) 2_655 ?
C3 N4 1.362(12) . ?
C3 C4 1.474(14) . ?
O1 C1 1.254(14) . ?
N2 N3 1.318(12) . ?
N2 C2 1.431(14) . ?
C8 C4 1.385(14) . ?
C8 C7 1.389(16) . ?
C8 H8 0.9300 . ?
O2 C1 1.226(13) . ?
O2 Pb1 2.558(8) 1_565 ?
C5 C4 1.371(14) . ?
C5 C6 1.391(17) . ?
C5 H5 0.9300 . ?
N4 N3 1.324(14) . ?
C7 H7 0.9300 . ?
C2 C1 1.545(15) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C6 H6 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
O1 Pb1 O1 180.0(5) 3_765 . ?
O1 Pb1 O2 83.4(3) 3_765 3_775 ?
O1 Pb1 O2 96.6(3) . 3_775 ?
O1 Pb1 O2 96.6(3) 3_765 1_545 ?
O1 Pb1 O2 83.4(3) . 1_545 ?
O2 Pb1 O2 180.0(3) 3_775 1_545 ?
O1 Pb1 N5 92.1(3) 3_765 4_675 ?
O1 Pb1 N5 87.9(3) . 4_675 ?
O2 Pb1 N5 79.8(3) 3_775 4_675 ?
O2 Pb1 N5 100.2(3) 1_545 4_675 ?
O1 Pb1 N5 87.9(3) 3_765 2_645 ?
O1 Pb1 N5 92.1(3) . 2_645 ?
O2 Pb1 N5 100.2(3) 3_775 2_645 ?
O2 Pb1 N5 79.8(3) 1_545 2_645 ?
N5 Pb1 N5 180.0(5) 4_675 2_645 ?
N2 N1 C3 102.2(7) . . ?
C7 N5 C6 116.7(10) . . ?
C7 N5 Pb1 124.7(7) . 2_655 ?
C6 N5 Pb1 117.6(7) . 2_655 ?
N1 C3 N4 111.4(9) . . ?
N1 C3 C4 123.7(8) . . ?
N4 C3 C4 124.9(9) . . ?
C1 O1 Pb1 131.5(7) . . ?
N1 N2 N3 113.8(9) . . ?
N1 N2 C2 123.9(8) . . ?
N3 N2 C2 121.9(9) . . ?
C4 C8 C7 117.0(9) . . ?
C4 C8 H8 121.5 . . ?
C7 C8 H8 121.5 . . ?
C1 O2 Pb1 118.2(7) . 1_565 ?
C4 C5 C6 118.7(10) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
N3 N4 C3 106.1(8) . . ?
N5 C7 C8 124.9(10) . . ?
N5 C7 H7 117.5 . . ?
C8 C7 H7 117.5 . . ?
N2 C2 C1 111.8(8) . . ?
N2 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
N2 N3 N4 106.4(8) . . ?
O2 C1 O1 126.4(11) . . ?
O2 C1 C2 117.0(10) . . ?
O1 C1 C2 116.6(9) . . ?
C5 C4 C8 119.5(10) . . ?
C5 C4 C3 121.3(9) . . ?
C8 C4 C3 119.1(8) . . ?
N5 C6 C5 123.1(10) . . ?
N5 C6 H6 118.5 . . ?
C5 C6 H6 118.5 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         2.001
_refine_diff_density_min         -2.138
_refine_diff_density_rms         0.260
