# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1413675'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H16 N6 O6 Zn, 2(C6 H6)'
_chemical_formula_sum            'C36 H28 N6 O6 Zn'
_chemical_formula_weight         706.03

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'
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   17.9503(15)
_cell_length_b                   11.2846(6)
_cell_length_c                   9.2574(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.709(7)
_cell_angle_gamma                90.00
_cell_volume                     1628.71(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    1167
_cell_measurement_theta_min      3.6060
_cell_measurement_theta_max      25.0010

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             728
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7110
_exptl_absorpt_correction_T_max  0.8042
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.4692
_diffrn_standards_number         4363
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3674
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1514
_reflns_number_gt                1245
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_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)+(0.0333P)²+8.1070P] where P=(Fo²+2Fc²)/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         1514
_refine_ls_number_parameters     117
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_ref         0.1567
_refine_ls_wR_factor_gt          0.1461
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.004

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
Zn1 Zn 0.0000 0.5000 0.5000 0.02201(14) Uani 1 4 d S . .
O1 O 0.14047(16) 0.5000 0.6083(3) 0.0613(10) Uani 1 2 d S A .
O2 O 0.25707(15) 0.5927(2) 0.7525(3) 0.0929(10) Uani 1 1 d . A .
N2 N 0.21845(19) 0.5000 0.7049(3) 0.0395(9) Uani 1 2 d S . .
N1 N -0.0131(2) 0.3587(4) 0.3280(4) 0.0265(5) Uani 0.50 1 d PU A 1
C1 C -0.0827(3) 0.2902(4) 0.2646(5) 0.0265(5) Uani 0.50 1 d PU A 1
H1 H -0.1266 0.3113 0.2855 0.032 Uiso 0.50 1 calc PR A 1
C2 C -0.0941(3) 0.1919(4) 0.1718(5) 0.0265(5) Uani 0.50 1 d PU A 1
H2 H -0.1442 0.1476 0.1324 0.032 Uiso 0.50 1 calc PR A 1
C3 C -0.0306(3) 0.1574(4) 0.1356(5) 0.0265(5) Uani 0.50 1 d PU A 1
C4 C 0.0404(3) 0.2316(4) 0.1948(5) 0.0265(5) Uani 0.50 1 d PU A 1
H4 H 0.0854 0.2125 0.1763 0.032 Uiso 0.50 1 calc PR A 1
C5 C 0.0444(3) 0.3354(4) 0.2826(5) 0.0265(5) Uani 0.50 1 d PU A 1
H5 H 0.0887 0.3890 0.3094 0.032 Uiso 0.50 1 calc PR A 1
C6 C -0.0407(4) 0.0446(4) 0.0416(5) 0.0867(13) Uani 0.50 1 d PU . 1
N1A N 0.0027(3) 0.3631(4) 0.3458(5) 0.0282(5) Uani 0.50 1 d PU A 2
C1A C -0.0546(3) 0.2760(4) 0.2982(5) 0.0282(5) Uani 0.50 1 d PU A 2
H1A H -0.0993 0.2837 0.3211 0.034 Uiso 0.50 1 calc PR A 2
C2A C -0.0519(3) 0.1747(4) 0.2165(5) 0.0282(5) Uani 0.50 1 d PU A 2
H2A H -0.0954 0.1185 0.1805 0.034 Uiso 0.50 1 calc PR A 2
C3A C 0.0171(3) 0.1584(4) 0.1892(5) 0.0282(5) Uani 0.50 1 d PU A 2
C4A C 0.0763(3) 0.2459(4) 0.2422(5) 0.0282(5) Uani 0.50 1 d PU A 2
H4A H 0.1218 0.2407 0.2214 0.034 Uiso 0.50 1 calc PR A 2
C5A C 0.0705(3) 0.3392(4) 0.3234(5) 0.0282(5) Uani 0.50 1 d PU A 2
H5A H 0.1162 0.3921 0.3684 0.034 Uiso 0.50 1 calc PR A 2
C6A C 0.0346(3) 0.0449(4) 0.1244(5) 0.0282(11) Uiso 0.50 1 d P . 2
C7 C -0.3032(3) 0.0000 -0.9265(5) 0.0753(18) Uani 1 2 d S . .
H7 H -0.3358 0.0000 -1.0420 0.090 Uiso 1 2 calc SR . .
C8 C -0.2796(2) -0.1037(4) -0.8429(4) 0.0840(13) Uani 1 1 d . . .
H8 H -0.2943 -0.1751 -0.9008 0.101 Uiso 1 1 calc R . .
C9 C -0.2346(2) -0.1037(5) -0.6745(4) 0.0984(16) Uani 1 1 d . . .
H9 H -0.2188 -0.1749 -0.6164 0.118 Uiso 1 1 calc R . .
C10 C -0.2129(3) 0.0000 -0.5917(6) 0.103(3) Uani 1 2 d S . .
H10 H -0.1826 0.0000 -0.4760 0.124 Uiso 1 2 calc SR . .


_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
Zn1 N1A 2.120(5) 5_566 ?
Zn1 N1A 2.120(5) . ?
Zn1 N1A 2.120(5) 2_556 ?
Zn1 N1A 2.120(5) 6_565 ?
Zn1 N1 2.182(4) 5_566 ?
Zn1 N1 2.182(4) . ?
Zn1 N1 2.182(4) 2_556 ?
Zn1 N1 2.182(4) 6_565 ?
Zn1 O1 2.204(3) 5_566 ?
Zn1 O1 2.204(3) . ?
O1 N2 1.232(4) . ?
O2 N2 1.211(3) . ?
N2 O2 1.211(3) 6_565 ?
N1 C1 1.334(6) . ?
N1 C5 1.319(7) . ?
C1 C2 1.354(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.394(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.391(6) . ?
C3 C6 1.502(6) . ?
C4 C5 1.408(7) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C6 1.007(9) 6 ?
C6 C6 1.961(12) 2 ?
C6 C6 2.205(12) 5 ?
N1A C5A 1.360(7) . ?
N1A C1A 1.329(6) . ?
C1A C2A 1.385(7) . ?
C1A H1A 0.9300 . ?
C2A C3A 1.394(8) . ?
C2A H2A 0.9300 . ?
C3A C6A 1.512(7) . ?
C3A C4A 1.353(7) . ?
C4A C5A 1.327(7) . ?
C4A H4A 0.9300 . ?
C5A H5A 0.9300 . ?
C6A C6A 1.014(9) 6 ?
C6A C6A 2.003(8) 2 ?
C7 C8 1.351(5) 6 ?
C7 C8 1.351(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.354(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.347(5) . ?
C9 H9 0.9300 . ?
C10 C9 1.347(5) 6 ?
C10 H10 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
N1A Zn1 N1A 180.0 5_566 . ?
N1A Zn1 N1A 93.6(3) 5_566 2_556 ?
N1A Zn1 N1A 86.4(3) . 2_556 ?
N1A Zn1 N1A 86.4(3) 5_566 6_565 ?
N1A Zn1 N1A 93.6(3) . 6_565 ?
N1A Zn1 N1A 180.0(2) 2_556 6_565 ?
N1A Zn1 N1 6.50(16) 5_566 5_566 ?
N1A Zn1 N1 173.50(16) . 5_566 ?
N1A Zn1 N1 94.10(13) 2_556 5_566 ?
N1A Zn1 N1 85.90(13) 6_565 5_566 ?
N1A Zn1 N1 173.50(16) 5_566 . ?
N1A Zn1 N1 6.50(16) . . ?
N1A Zn1 N1 85.90(13) 2_556 . ?
N1A Zn1 N1 94.10(13) 6_565 . ?
N1 Zn1 N1 180.0 5_566 . ?
N1A Zn1 N1 94.10(13) 5_566 2_556 ?
N1A Zn1 N1 85.90(13) . 2_556 ?
N1A Zn1 N1 6.50(16) 2_556 2_556 ?
N1A Zn1 N1 173.50(16) 6_565 2_556 ?
N1 Zn1 N1 93.9(2) 5_566 2_556 ?
N1 Zn1 N1 86.1(2) . 2_556 ?
N1A Zn1 N1 85.90(13) 5_566 6_565 ?
N1A Zn1 N1 94.10(13) . 6_565 ?
N1A Zn1 N1 173.50(16) 2_556 6_565 ?
N1A Zn1 N1 6.50(16) 6_565 6_565 ?
N1 Zn1 N1 86.1(2) 5_566 6_565 ?
N1 Zn1 N1 93.9(2) . 6_565 ?
N1 Zn1 N1 180.00(15) 2_556 6_565 ?
N1A Zn1 O1 84.47(12) 5_566 5_566 ?
N1A Zn1 O1 95.53(12) . 5_566 ?
N1A Zn1 O1 84.47(12) 2_556 5_566 ?
N1A Zn1 O1 95.53(12) 6_565 5_566 ?
N1 Zn1 O1 90.97(11) 5_566 5_566 ?
N1 Zn1 O1 89.03(11) . 5_566 ?
N1 Zn1 O1 90.97(11) 2_556 5_566 ?
N1 Zn1 O1 89.03(11) 6_565 5_566 ?
N1A Zn1 O1 95.53(12) 5_566 . ?
N1A Zn1 O1 84.47(12) . . ?
N1A Zn1 O1 95.53(12) 2_556 . ?
N1A Zn1 O1 84.47(12) 6_565 . ?
N1 Zn1 O1 89.03(11) 5_566 . ?
N1 Zn1 O1 90.97(11) . . ?
N1 Zn1 O1 89.03(11) 2_556 . ?
N1 Zn1 O1 90.97(11) 6_565 . ?
O1 Zn1 O1 180.0 5_566 . ?
N2 O1 Zn1 164.2(3) . . ?
O2 N2 O2 119.5(3) . 6_565 ?
O2 N2 O1 120.23(16) . . ?
O2 N2 O1 120.23(16) 6_565 . ?
C1 N1 C5 117.1(4) . . ?
C1 N1 Zn1 118.9(4) . . ?
C5 N1 Zn1 124.0(3) . . ?
N1 C1 C2 124.6(5) . . ?
N1 C1 H1 117.7 . . ?
C2 C1 H1 117.7 . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 115.9(4) . . ?
C2 C3 C6 119.8(4) . . ?
C4 C3 C6 124.2(5) . . ?
C5 C4 C3 120.2(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 N1 121.7(4) . . ?
C4 C5 H5 119.1 . . ?
N1 C5 H5 119.1 . . ?
C6 C6 C3 148.0(2) 6 . ?
C6 C6 C6 90.0 6 2 ?
C3 C6 C6 109.1(3) . 2 ?
C6 C6 C6 62.8(3) 6 5 ?
C3 C6 C6 132.8(5) . 5 ?
C6 C6 C6 27.2(3) 2 5 ?
C5A N1A C1A 114.0(4) . . ?
C5A N1A Zn1 124.6(3) . . ?
C1A N1A Zn1 119.3(4) . . ?
C2A C1A N1A 124.1(5) . . ?
C2A C1A H1A 118.0 . . ?
N1A C1A H1A 118.0 . . ?
C1A C2A C3A 118.8(4) . . ?
C1A C2A H2A 120.6 . . ?
C3A C2A H2A 120.6 . . ?
C2A C3A C6A 124.2(4) . . ?
C2A C3A C4A 116.6(5) . . ?
C6A C3A C4A 118.8(5) . . ?
C5A C4A C3A 121.1(5) . . ?
C5A C4A H4A 119.4 . . ?
C3A C4A H4A 119.4 . . ?
N1A C5A C4A 124.8(5) . . ?
N1A C5A H5A 117.6 . . ?
C4A C5A H5A 117.6 . . ?
C6A C6A C3A 147.9(3) 6 . ?
C6A C6A C6A 90.0 6 2 ?
C3A C6A C6A 108.9(2) . 2 ?
C8 C7 C8 120.1(5) 6 . ?
C8 C7 H7 119.9 6 . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 119.9(4) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 119.7(5) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C9 C10 C9 120.7(5) . 6 ?
C9 C10 H10 119.7 . . ?
C9 C10 H10 119.7 6 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.094
####################################################################### 
# 
# 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 1413676'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H20 N6 O6 Zn, 2(C7 H8)'
_chemical_formula_sum            'C38 H36 N6 O6 Zn'
_chemical_formula_weight         738.12

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'
Zn Zn 0.2839 1.4301 '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                   9.4863(9)
_cell_length_b                   9.8132(9)
_cell_length_c                   11.1496(11)
_cell_angle_alpha                68.615(9)
_cell_angle_beta                 89.254(8)
_cell_angle_gamma                63.457(10)
_cell_volume                     850.48(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2441
_cell_measurement_theta_min      3.7230
_cell_measurement_theta_max      26.9850

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             348
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6528
_exptl_absorpt_correction_T_max  0.8003
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      293(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  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.4692
_diffrn_standards_number         7414
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7397
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         29.43
_reflns_number_total             3948
_reflns_number_gt                3128
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_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)+(0.0809P)²+0.7092P] where P=(Fo²+2Fc²)/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         2992
_refine_ls_number_parameters     232
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1334
_refine_ls_wR_factor_gt          0.1267
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_restrained_S_all      0.921
_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
Zn1 Zn 1.5000 0.5000 0.5000 0.0260(2) Uani 1 2 d S . .
O1 O 1.6096(4) 0.2362(3) 0.6290(3) 0.0620(9) Uani 1 1 d . . .
O2 O 1.6485(7) 0.0538(5) 0.5609(4) 0.1054(16) Uani 1 1 d . . .
O3 O 1.7758(5) -0.0150(4) 0.7457(4) 0.0913(13) Uani 1 1 d . . .
N1 N 1.3582(3) 0.4816(3) 0.3598(2) 0.0274(6) Uani 1 1 d . . .
N3 N 1.6814(4) 0.0907(4) 0.6472(3) 0.0382(7) Uani 1 1 d . . .
C1 C 1.3277(4) 0.5817(5) 0.2335(3) 0.0388(9) Uani 1 1 d . . .
H1A H 1.3628 0.6610 0.2101 0.047 Uiso 1 1 calc R . .
C2 C 1.2477(4) 0.5749(5) 0.1363(3) 0.0381(8) Uani 1 1 d . . .
H2A H 1.2298 0.6485 0.0500 0.046 Uiso 1 1 calc R . .
C3 C 1.1933(4) 0.4585(4) 0.1661(3) 0.0278(7) Uani 1 1 d . . .
C4 C 1.2256(4) 0.3537(4) 0.2963(3) 0.0340(8) Uani 1 1 d . . .
H4A H 1.1920 0.2732 0.3222 0.041 Uiso 1 1 calc R . .
C5 C 1.3073(4) 0.3683(4) 0.3878(3) 0.0320(8) Uani 1 1 d . . .
H5A H 1.3286 0.2948 0.4747 0.038 Uiso 1 1 calc R . .
C6 C 1.1179(4) 0.4367(4) 0.0621(3) 0.0251(7) Uani 1 1 d . . .
H6 H 1.2006 0.3425 0.0470 0.030 Uiso 1 1 calc R . .
C7 C 0.7315(4) 0.3341(4) 0.3435(3) 0.0331(8) Uani 1 1 d . . .
H7A H 0.7032 0.2520 0.3877 0.040 Uiso 1 1 calc R . .
C8 C 0.8281(4) 0.3116(4) 0.2519(3) 0.0322(8) Uani 1 1 d . . .
H8A H 0.8646 0.2153 0.2368 0.039 Uiso 1 1 calc R . .
C9 C 0.8711(4) 0.4314(4) 0.1824(3) 0.0256(7) Uani 1 1 d . . .
C10 C 0.8154(4) 0.5692(4) 0.2140(3) 0.0330(8) Uani 1 1 d . . .
H10A H 0.8435 0.6521 0.1723 0.040 Uiso 1 1 calc R . .
C11 C 0.7188(4) 0.5833(4) 0.3067(3) 0.0322(8) Uani 1 1 d . . .
H11A H 0.6816 0.6779 0.3243 0.039 Uiso 1 1 calc R . .
C12 C 0.9629(4) 0.4153(4) 0.0726(3) 0.0248(7) Uani 1 1 d . . .
H12 H 0.9844 0.3120 0.0644 0.030 Uiso 1 1 calc R . .
C13 C 0.3753(9) -0.0768(8) 0.9528(6) 0.098(2) Uani 1 1 d . . .
H13A H 0.4478 -0.1284 1.0306 0.118 Uiso 1 1 calc R . .
C14 C 0.2150(9) -0.0071(7) 0.9526(6) 0.0812(17) Uani 1 1 d . . .
H14A H 0.1771 -0.0118 1.0306 0.097 Uiso 1 1 calc R . .
C15 C 0.1109(6) 0.0692(6) 0.8386(5) 0.0645(13) Uani 1 1 d . . .
H15A H 0.0015 0.1175 0.8395 0.077 Uiso 1 1 calc R . .
C16 C 0.1618(5) 0.0773(5) 0.7219(4) 0.0520(10) Uani 1 1 d . . .
C17 C 0.3236(5) 0.0044(5) 0.7226(5) 0.0586(12) Uani 1 1 d . . .
H17A H 0.3616 0.0058 0.6450 0.070 Uiso 1 1 calc R . .
C18 C 0.4287(7) -0.0702(7) 0.8374(7) 0.0870(19) Uani 1 1 d . . .
H18A H 0.5382 -0.1172 0.8371 0.104 Uiso 1 1 calc R . .
C19 C 0.0470(7) 0.1630(8) 0.5970(6) 0.0958(19) Uani 1 1 d . . .
H19A H 0.1049 0.1539 0.5266 0.144 Uiso 1 1 calc R . .
H19B H -0.0177 0.2783 0.5808 0.144 Uiso 1 1 calc R . .
H19C H -0.0206 0.1125 0.6027 0.144 Uiso 1 1 calc R . .
N2 N 0.6759(3) 0.4685(3) 0.3725(2) 0.0261(6) Uani 1 1 d . . .


_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
Zn1 N2 2.168(2) 2_766 ?
Zn1 N2 2.168(2) 1_655 ?
Zn1 N1 2.183(3) . ?
Zn1 N1 2.183(3) 2_866 ?
Zn1 O1 2.184(3) . ?
Zn1 O1 2.184(3) 2_866 ?
O1 N3 1.211(4) . ?
O2 N3 1.232(5) . ?
O3 N3 1.204(4) . ?
N1 C5 1.338(4) . ?
N1 C1 1.334(4) . ?
C1 C2 1.369(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.388(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.379(5) . ?
C3 C6 1.498(4) . ?
C4 C5 1.375(5) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C12 1.548(4) 2_765 ?
C6 C12 1.572(4) . ?
C6 H6 0.9800 . ?
C7 C8 1.374(5) . ?
C7 N2 1.345(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.380(5) . ?
C8 H8A 0.9300 . ?
C9 C10 1.391(4) . ?
C9 C12 1.507(4) . ?
C10 C11 1.376(4) . ?
C10 H10A 0.9300 . ?
C11 N2 1.331(4) . ?
C11 H11A 0.9300 . ?
C12 C6 1.548(4) 2_765 ?
C12 H12 0.9800 . ?
C13 C14 1.360(9) . ?
C13 C18 1.366(9) . ?
C13 H13A 0.9300 . ?
C14 C15 1.353(8) . ?
C14 H14A 0.9300 . ?
C15 C16 1.369(6) . ?
C15 H15A 0.9300 . ?
C16 C17 1.372(6) . ?
C16 C19 1.483(7) . ?
C17 C18 1.367(8) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
N2 Zn1 2.168(2) 1_455 ?

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 Zn1 N2 180.000(1) 2_766 1_655 ?
N2 Zn1 N1 94.20(10) 2_766 . ?
N2 Zn1 N1 85.80(9) 1_655 . ?
N2 Zn1 N1 85.80(9) 2_766 2_866 ?
N2 Zn1 N1 94.20(9) 1_655 2_866 ?
N1 Zn1 N1 180.000(1) . 2_866 ?
N2 Zn1 O1 85.24(11) 2_766 . ?
N2 Zn1 O1 94.76(11) 1_655 . ?
N1 Zn1 O1 94.49(11) . . ?
N1 Zn1 O1 85.51(11) 2_866 . ?
N2 Zn1 O1 94.76(11) 2_766 2_866 ?
N2 Zn1 O1 85.24(11) 1_655 2_866 ?
N1 Zn1 O1 85.51(11) . 2_866 ?
N1 Zn1 O1 94.49(12) 2_866 2_866 ?
O1 Zn1 O1 180.00(16) . 2_866 ?
N3 O1 Zn1 151.3(2) . . ?
C5 N1 C1 115.6(3) . . ?
C5 N1 Zn1 125.3(2) . . ?
C1 N1 Zn1 119.0(2) . . ?
O3 N3 O1 122.8(4) . . ?
O3 N3 O2 120.8(4) . . ?
O1 N3 O2 116.4(4) . . ?
C2 C1 N1 124.0(3) . . ?
C2 C1 H1A 118.0 . . ?
N1 C1 H1A 118.0 . . ?
C1 C2 C3 120.3(3) . . ?
C1 C2 H2A 119.9 . . ?
C3 C2 H2A 119.9 . . ?
C2 C3 C4 116.1(3) . . ?
C2 C3 C6 122.1(3) . . ?
C4 C3 C6 121.5(3) . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
N1 C5 C4 124.1(3) . . ?
N1 C5 H5A 117.9 . . ?
C4 C5 H5A 117.9 . . ?
C3 C6 C12 118.8(3) . 2_765 ?
C3 C6 C12 122.6(2) . . ?
C12 C6 C12 90.7(2) 2_765 . ?
C3 C6 H6 107.7 . . ?
C12 C6 H6 107.7 2_765 . ?
C12 C6 H6 107.7 . . ?
C8 C7 N2 123.5(3) . . ?
C8 C7 H7A 118.3 . . ?
N2 C7 H7A 118.3 . . ?
C7 C8 C9 120.3(3) . . ?
C7 C8 H8A 119.8 . . ?
C9 C8 H8A 119.8 . . ?
C8 C9 C10 116.1(3) . . ?
C8 C9 C12 120.4(3) . . ?
C10 C9 C12 123.3(3) . . ?
C11 C10 C9 120.3(3) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
N2 C11 C10 123.4(3) . . ?
N2 C11 H11A 118.3 . . ?
C10 C11 H11A 118.3 . . ?
C9 C12 C6 115.2(2) . 2_765 ?
C9 C12 C6 122.1(3) . . ?
C6 C12 C6 89.3(2) 2_765 . ?
C9 C12 H12 109.5 . . ?
C6 C12 H12 109.5 2_765 . ?
C6 C12 H12 109.5 . . ?
C14 C13 C18 119.2(6) . . ?
C14 C13 H13A 120.4 . . ?
C18 C13 H13A 120.4 . . ?
C15 C14 C13 119.8(5) . . ?
C15 C14 H14A 120.1 . . ?
C13 C14 H14A 120.1 . . ?
C14 C15 C16 121.9(5) . . ?
C14 C15 H15A 119.0 . . ?
C16 C15 H15A 119.0 . . ?
C17 C16 C15 118.2(5) . . ?
C17 C16 C19 120.1(5) . . ?
C15 C16 C19 121.7(5) . . ?
C18 C17 C16 119.8(5) . . ?
C18 C17 H17A 120.1 . . ?
C16 C17 H17A 120.1 . . ?
C17 C18 C13 121.0(5) . . ?
C17 C18 H18A 119.5 . . ?
C13 C18 H18A 119.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C11 N2 C7 116.4(3) . . ?
C11 N2 Zn1 124.5(2) . 1_455 ?
C7 N2 Zn1 118.6(2) . 1_455 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.073
####################################################################### 
# 
# 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 1413677'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H13 N4 O7 Pb, C6 H6'
_chemical_formula_sum            'C19 H19 N4 O7 Pb'
_chemical_formula_weight         622.58

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/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   9.3515(6)
_cell_length_b                   26.1628(12)
_cell_length_c                   10.1410(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.673(7)
_cell_angle_gamma                90.00
_cell_volume                     2272.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    2959
_cell_measurement_theta_min      3.8030
_cell_measurement_theta_max      28.3590

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1196
_exptl_absorpt_coefficient_mu    7.470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0196
_exptl_absorpt_correction_T_max  0.0548
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.4471
_diffrn_standards_number         13624
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10408
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3993
_reflns_number_gt                3151
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 '
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 '
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 '
_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)+(0.0728P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3993
_refine_ls_number_parameters     269
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1316
_refine_ls_wR_factor_gt          0.1198
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.13820(3) 0.201226(12) 0.83744(3) 0.03098(16) Uani 1 1 d . . .
N1 N -0.0827(8) 0.1396(3) 0.7001(7) 0.0348(17) Uani 1 1 d . . .
C6 C -0.4345(9) 0.0285(3) 0.4654(8) 0.0294(18) Uani 1 1 d . . .
H6 H -0.4499 0.0292 0.3630 0.035 Uiso 1 1 calc R . .
C8 C -0.6426(10) 0.0660(3) 0.5642(9) 0.033(2) Uani 1 1 d . . .
C7 C -0.5955(9) 0.0270(3) 0.4767(8) 0.0304(19) Uani 1 1 d . . .
H7 H -0.6782 0.0262 0.3779 0.037 Uiso 1 1 calc R . .
C12 C -0.6269(10) 0.1178(4) 0.5472(10) 0.040(2) Uani 1 1 d . . .
H12A H -0.5833 0.1296 0.4840 0.048 Uiso 1 1 calc R . .
C2 C -0.2600(9) 0.0732(3) 0.6962(8) 0.034(2) Uani 1 1 d . . .
H2A H -0.2993 0.0521 0.7489 0.041 Uiso 1 1 calc R . .
N4 N -0.0300(10) 0.2664(3) 0.5611(9) 0.047(2) Uani 1 1 d . . .
C3 C -0.3140(9) 0.0680(3) 0.5494(8) 0.0273(18) Uani 1 1 d . . .
C4 C -0.2500(10) 0.1000(4) 0.4780(9) 0.041(2) Uani 1 1 d . . .
H4A H -0.2834 0.0980 0.3775 0.049 Uiso 1 1 calc R . .
O5 O 0.0822(8) 0.2384(3) 0.5738(7) 0.0570(19) Uani 1 1 d . . .
C5 C -0.1348(11) 0.1351(4) 0.5579(10) 0.046(3) Uani 1 1 d . . .
H5A H -0.0922 0.1565 0.5086 0.055 Uiso 1 1 calc R . .
C11 C -0.6762(10) 0.1519(4) 0.6244(10) 0.044(2) Uani 1 1 d . . .
H11A H -0.6632 0.1870 0.6130 0.053 Uiso 1 1 calc R . .
O4 O -0.0848(10) 0.2645(3) 0.6520(9) 0.077(3) Uani 1 1 d . . .
C9 C -0.7105(11) 0.0509(4) 0.6572(11) 0.048(2) Uani 1 1 d . . .
H9A H -0.7251 0.0161 0.6703 0.058 Uiso 1 1 calc R . .
O6 O -0.0867(10) 0.2944(3) 0.4531(9) 0.069(2) Uani 1 1 d . . .
C1 C -0.1479(10) 0.1095(4) 0.7662(9) 0.037(2) Uani 1 1 d . . .
H1A H -0.1159 0.1132 0.8662 0.044 Uiso 1 1 calc R . .
N3 N 0.3072(11) 0.1333(4) 1.1161(9) 0.055(2) Uani 1 1 d . . .
O1 O 0.1981(10) 0.1195(3) 1.0036(7) 0.069(2) Uani 1 1 d . . .
O3 O 0.3632(10) 0.1043(4) 1.2173(9) 0.087(3) Uani 1 1 d . . .
O2 O 0.3603(11) 0.1776(4) 1.1203(10) 0.090(3) Uani 1 1 d . . .
C10 C -0.7562(12) 0.0872(4) 0.7296(10) 0.048(2) Uani 1 1 d . . .
H10A H -0.8002 0.0763 0.7934 0.058 Uiso 1 1 calc R . .
N2 N -0.7411(8) 0.1376(3) 0.7141(8) 0.0376(17) Uani 1 1 d . . .
O7 O 0.3890(8) 0.2613(3) 0.8577(9) 0.075(2) Uani 1 1 d . . .
C13 C -0.088(2) 0.3991(7) 0.6798(12) 0.125(7) Uani 1 1 d G . .
H13A H -0.0166 0.3740 0.7340 0.150 Uiso 1 1 calc R . .
C14 C -0.247(3) 0.3882(5) 0.6193(17) 0.119(7) Uani 1 1 d G . .
H14A H -0.2829 0.3559 0.6325 0.143 Uiso 1 1 calc R . .
C15 C -0.3529(13) 0.4253(8) 0.5392(13) 0.114(7) Uani 1 1 d G . .
H15A H -0.4603 0.4179 0.4983 0.137 Uiso 1 1 calc R . .
C16 C -0.300(2) 0.4731(6) 0.5197(12) 0.113(6) Uani 1 1 d G . .
H16A H -0.3714 0.4982 0.4655 0.135 Uiso 1 1 calc R . .
C17 C -0.141(2) 0.4839(5) 0.5802(17) 0.131(8) Uani 1 1 d G . .
H17A H -0.1051 0.5163 0.5670 0.157 Uiso 1 1 calc R . .
C18 C -0.0351(12) 0.4469(8) 0.6603(14) 0.137(9) Uani 1 1 d G . .
H18A H 0.0723 0.4542 0.7012 0.165 Uiso 1 1 calc R . .
C19 C 0.5467(15) 0.2526(6) 0.9404(18) 0.108(6) Uani 1 1 d . . .
H19A H 0.5950 0.2380 0.8804 0.162 Uiso 1 1 calc R . .
H19B H 0.5577 0.2290 1.0178 0.162 Uiso 1 1 calc R . .
H19C H 0.5974 0.2847 0.9808 0.162 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 N1 2.549(7) . ?
Pb1 N2 2.597(7) 1_655 ?
Pb1 O1 2.640(7) . ?
Pb1 O5 2.691(6) . ?
Pb1 O4 2.733(7) . ?
N1 C5 1.329(11) . ?
N1 C1 1.330(11) . ?
C6 C3 1.514(10) . ?
C6 C7 1.551(12) 3_456 ?
C6 C7 1.555(11) . ?
C6 H6 0.9900 . ?
C8 C12 1.379(13) . ?
C8 C9 1.390(13) . ?
C8 C7 1.528(12) . ?
C7 C6 1.551(12) 3_456 ?
C7 H7 0.9900 . ?
C12 C11 1.382(12) . ?
C12 H12A 0.9400 . ?
C2 C1 1.380(11) . ?
C2 C3 1.373(10) . ?
C2 H2A 0.9400 . ?
N4 O4 1.223(10) . ?
N4 O5 1.244(10) . ?
N4 O6 1.245(10) . ?
C3 C4 1.389(12) . ?
C4 C5 1.400(12) . ?
C4 H4A 0.9400 . ?
C5 H5A 0.9400 . ?
C11 N2 1.335(11) . ?
C11 H11A 0.9400 . ?
C9 C10 1.369(13) . ?
C9 H9A 0.9400 . ?
C1 H1A 0.9400 . ?
N3 O3 1.214(11) . ?
N3 O1 1.241(11) . ?
N3 O2 1.255(12) . ?
C10 N2 1.340(12) . ?
C10 H10A 0.9400 . ?
N2 Pb1 2.597(7) 1_455 ?
O7 C19 1.392(14) . ?
C13 C14 1.3900 . ?
C13 C18 1.3900 . ?
C13 H13A 0.9400 . ?
C14 C15 1.3900 . ?
C14 H14A 0.9400 . ?
C15 C16 1.3900 . ?
C15 H15A 0.9400 . ?
C16 C17 1.3900 . ?
C16 H16A 0.9400 . ?
C17 C18 1.3900 . ?
C17 H17A 0.9400 . ?
C18 H18A 0.9400 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pb1 N2 75.2(2) . 1_655 ?
N1 Pb1 O1 75.7(2) . . ?
N2 Pb1 O1 76.5(2) 1_655 . ?
N1 Pb1 O5 83.9(2) . . ?
N2 Pb1 O5 72.7(2) 1_655 . ?
O1 Pb1 O5 146.4(2) . . ?
N1 Pb1 O4 77.3(3) . . ?
N2 Pb1 O4 114.6(2) 1_655 . ?
O1 Pb1 O4 146.8(3) . . ?
O5 Pb1 O4 46.2(2) . . ?
C5 N1 C1 116.9(7) . . ?
C5 N1 Pb1 120.8(5) . . ?
C1 N1 Pb1 122.3(5) . . ?
C3 C6 C7 116.5(6) . 3_456 ?
C3 C6 C7 120.0(7) . . ?
C7 C6 C7 88.9(6) 3_456 . ?
C3 C6 H6 109.9 . . ?
C7 C6 H6 109.9 3_456 . ?
C7 C6 H6 109.9 . . ?
C12 C8 C9 117.6(8) . . ?
C12 C8 C7 120.9(8) . . ?
C9 C8 C7 121.4(8) . . ?
C8 C7 C6 117.2(7) . 3_456 ?
C8 C7 C6 122.6(7) . . ?
C6 C7 C6 91.1(6) 3_456 . ?
C8 C7 H7 108.2 . . ?
C6 C7 H7 108.2 3_456 . ?
C6 C7 H7 108.2 . . ?
C8 C12 C11 119.1(9) . . ?
C8 C12 H12A 120.4 . . ?
C11 C12 H12A 120.4 . . ?
C1 C2 C3 119.9(8) . . ?
C1 C2 H2A 120.0 . . ?
C3 C2 H2A 120.0 . . ?
O4 N4 O5 119.2(8) . . ?
O4 N4 O6 121.9(9) . . ?
O5 N4 O6 118.8(8) . . ?
C4 C3 C2 117.2(7) . . ?
C4 C3 C6 119.8(7) . . ?
C2 C3 C6 123.0(7) . . ?
C3 C4 C5 119.1(8) . . ?
C3 C4 H4A 120.5 . . ?
C5 C4 H4A 120.5 . . ?
N4 O5 Pb1 97.8(5) . . ?
N1 C5 C4 123.2(8) . . ?
N1 C5 H5A 118.4 . . ?
C4 C5 H5A 118.4 . . ?
N2 C11 C12 123.4(9) . . ?
N2 C11 H11A 118.3 . . ?
C12 C11 H11A 118.3 . . ?
N4 O4 Pb1 96.3(6) . . ?
C10 C9 C8 119.6(9) . . ?
C10 C9 H9A 120.2 . . ?
C8 C9 H9A 120.2 . . ?
N1 C1 C2 123.7(7) . . ?
N1 C1 H1A 118.2 . . ?
C2 C1 H1A 118.2 . . ?
O3 N3 O1 120.7(11) . . ?
O3 N3 O2 121.3(10) . . ?
O1 N3 O2 118.0(9) . . ?
N3 O1 Pb1 103.6(6) . . ?
N2 C10 C9 123.2(9) . . ?
N2 C10 H10A 118.4 . . ?
C9 C10 H10A 118.4 . . ?
C11 N2 C10 117.0(8) . . ?
C11 N2 Pb1 123.6(6) . 1_455 ?
C10 N2 Pb1 119.1(6) . 1_455 ?
C14 C13 C18 120.0 . . ?
C14 C13 H13A 120.0 . . ?
C18 C13 H13A 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15A 120.0 . . ?
C14 C15 H15A 120.0 . . ?
C17 C16 C15 120.0 . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C18 C17 C16 120.0 . . ?
C18 C17 H17A 120.0 . . ?
C16 C17 H17A 120.0 . . ?
C17 C18 C13 120.0 . . ?
C17 C18 H18A 120.0 . . ?
C13 C18 H18A 120.0 . . ?
O7 C19 H19A 109.5 . . ?
O7 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O7 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         4.093
_refine_diff_density_min         -2.209
_refine_diff_density_rms         0.196
####################################################################### 
# 
# 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 1413678'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H23 N6 O7 Pb'
_chemical_formula_sum            'C25 H23 N6 O7 Pb'
_chemical_formula_weight         726.69

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/c '
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   12.7971(9)
_cell_length_b                   11.8723(10)
_cell_length_c                   20.1498(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.569(6)
_cell_angle_gamma                90.00
_cell_volume                     2608.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    3596
_cell_measurement_theta_min      3.5020
_cell_measurement_theta_max      26.8040

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1412
_exptl_absorpt_coefficient_mu    6.525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1113
_exptl_absorpt_correction_T_max  0.1573
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.4471
_diffrn_standards_number         17226
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13175
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_sigmaI/netI    0.0961
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4574
_reflns_number_gt                3250
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 '
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 '
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 '
_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)+(0.0605P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4574
_refine_ls_number_parameters     341
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1294
_refine_ls_wR_factor_gt          0.1161
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_restrained_S_all      0.931
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb -0.39676(3) 0.18110(3) -0.679700(19) 0.04090(17) Uani 1 1 d . . .
O1 O -0.1738(8) 0.2301(8) -0.6425(5) 0.0875(15) Uani 1 1 d . . .
O2 O -0.0696(8) 0.3819(7) -0.6088(5) 0.0875(15) Uani 1 1 d . . .
O3 O -0.2351(8) 0.3684(7) -0.6084(5) 0.0875(15) Uani 1 1 d . . .
O4 O -0.5937(7) 0.0924(7) -0.6756(5) 0.084(3) Uani 1 1 d . . .
O5 O -0.6748(10) -0.0686(8) -0.6984(7) 0.119(4) Uani 1 1 d . . .
O6 O -0.5301(8) -0.0358(8) -0.7176(5) 0.094(3) Uani 1 1 d . . .
O7 O -0.4048(6) 0.2853(5) -0.5574(4) 0.0539(17) Uani 1 1 d . . .
N1 N -0.2862(7) 0.0620(6) -0.5607(4) 0.0462(19) Uani 1 1 d . . .
N2 N -0.4235(9) -0.3278(6) -0.6510(5) 0.054(2) Uani 1 1 d . . .
N3 N 0.1784(9) -0.2241(8) -0.0794(5) 0.062(2) Uani 1 1 d . . .
N5 N -0.1573(8) 0.3298(7) -0.6189(5) 0.054(2) Uani 1 1 d . . .
N6 N -0.5988(9) -0.0049(10) -0.6973(6) 0.065(2) Uani 1 1 d . . .
C8 C -0.2266(9) -0.3497(7) -0.5346(5) 0.045(2) Uani 1 1 d U . .
H8A H -0.1424 -0.3634 -0.5127 0.054 Uiso 1 1 calc R . .
C18 C -0.1408(9) -0.1734(7) -0.3086(6) 0.042(2) Uani 1 1 d . . .
H18A H -0.1823 -0.1022 -0.3102 0.051 Uiso 1 1 calc R . .
C6 C -0.1163(9) -0.1796(7) -0.3764(5) 0.040(2) Uani 1 1 d . . .
H6A H -0.0278 -0.1883 -0.3567 0.048 Uiso 1 1 calc R . .
C12 C -0.1861(9) -0.2973(7) -0.4021(5) 0.044(2) Uani 1 1 d . . .
H12A H -0.1263 -0.3600 -0.3802 0.053 Uiso 1 1 calc R . .
C9 C -0.2747(9) -0.3147(7) -0.4897(6) 0.041(2) Uani 1 1 d . . .
C17 C 0.1610(9) -0.2799(9) -0.1415(6) 0.051(2) Uani 1 1 d . . .
H17A H 0.2230 -0.3306 -0.1335 0.062 Uiso 1 1 calc R . .
C15 C -0.0286(9) -0.1940(7) -0.2283(6) 0.043(2) Uani 1 1 d . . .
C16 C 0.0633(9) -0.2714(8) -0.2148(6) 0.049(2) Uani 1 1 d . . .
H16A H 0.0571 -0.3156 -0.2554 0.059 Uiso 1 1 calc R . .
C3 C -0.1726(8) -0.0875(7) -0.4358(5) 0.037(2) Uani 1 1 d . . .
C5 C -0.3359(9) 0.0370(7) -0.5180(5) 0.046(2) Uani 1 1 d . . .
H5A H -0.4111 0.0703 -0.5313 0.056 Uiso 1 1 calc R . .
C20 C -0.2830(10) -0.3333(8) -0.2502(6) 0.048(2) Uani 1 1 d . . .
H20A H -0.2898 -0.2569 -0.2409 0.058 Uiso 1 1 calc R . .
C24 C -0.2353(8) -0.2714(7) -0.3491(5) 0.040(2) Uani 1 1 d . . .
H24A H -0.3174 -0.2370 -0.3818 0.048 Uiso 1 1 calc R . .
C22 C -0.2323(8) -0.4749(8) -0.3094(5) 0.043(2) Uani 1 1 d . . .
H22A H -0.2054 -0.4983 -0.3426 0.052 Uiso 1 1 calc R . .
C19 C -0.3095(9) -0.4136(8) -0.2142(6) 0.054(3) Uani 1 1 d . . .
H19A H -0.3350 -0.3904 -0.1803 0.065 Uiso 1 1 calc R . .
C2 C -0.1218(8) -0.0603(8) -0.4796(5) 0.047(2) Uani 1 1 d . . .
H2B H -0.0479 -0.0940 -0.4686 0.056 Uiso 1 1 calc R . .
C4 C -0.2816(9) -0.0346(8) -0.4562(5) 0.046(2) Uani 1 1 d . . .
H4A H -0.3185 -0.0483 -0.4271 0.055 Uiso 1 1 calc R . .
C1 C -0.1785(10) 0.0146(8) -0.5383(6) 0.053(3) Uani 1 1 d . . .
H1A H -0.1393 0.0347 -0.5651 0.064 Uiso 1 1 calc R . .
C25 C -0.4341(10) 0.4022(9) -0.5639(7) 0.073(3) Uani 1 1 d . . .
H25A H -0.4518 0.4228 -0.5242 0.109 Uiso 1 1 calc R . .
H25B H -0.5053 0.4173 -0.6150 0.109 Uiso 1 1 calc R . .
H25C H -0.3650 0.4460 -0.5569 0.109 Uiso 1 1 calc R . .
C21 C -0.2461(8) -0.3629(8) -0.3003(5) 0.042(2) Uani 1 1 d . . .
C10 C -0.3951(10) -0.2813(8) -0.5266(6) 0.054(3) Uani 1 1 d . . .
H10A H -0.4286 -0.2524 -0.4983 0.065 Uiso 1 1 calc R . .
C14 C -0.0161(10) -0.1390(9) -0.1646(6) 0.055(3) Uani 1 1 d . . .
H14A H -0.0780 -0.0902 -0.1702 0.066 Uiso 1 1 calc R . .
C13 C 0.0888(11) -0.1559(9) -0.0917(6) 0.059(3) Uani 1 1 d . . .
H13A H 0.0961 -0.1167 -0.0490 0.071 Uiso 1 1 calc R . .
C23 C -0.2584(9) -0.5541(8) -0.2691(5) 0.048(2) Uani 1 1 d . . .
H23A H -0.2449 -0.6307 -0.2740 0.057 Uiso 1 1 calc R . .
C11 C -0.4663(11) -0.2917(8) -0.6080(6) 0.060(3) Uani 1 1 d . . .
H11A H -0.5496 -0.2716 -0.6333 0.072 Uiso 1 1 calc R . .
C7 C -0.3106(12) -0.3627(9) -0.6133(6) 0.058(3) Uani 1 1 d . . .
H7A H -0.2833 -0.4006 -0.6425 0.070 Uiso 1 1 calc R . .
N4 N -0.3020(7) -0.5256(6) -0.2236(4) 0.0461(19) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N1 2.490(7) . ?
Pb1 O1 2.608(8) . ?
Pb1 N4 2.605(7) 4 ?
O1 N5 1.251(10) . ?
O2 N5 1.202(10) . ?
O3 N5 1.211(10) . ?
O4 N6 1.225(11) . ?
O5 N6 1.223(11) . ?
O6 N6 1.205(10) . ?
O7 C25 1.426(12) . ?
N1 C1 1.330(11) . ?
N1 C5 1.344(10) . ?
N2 C7 1.300(13) . ?
N2 C11 1.316(13) . ?
N3 C13 1.317(13) . ?
N3 C17 1.327(13) . ?
C8 C7 1.381(13) . ?
C8 C9 1.398(12) . ?
C8 H8A 0.9400 . ?
C18 C15 1.519(14) . ?
C18 C24 1.565(12) . ?
C18 C6 1.556(12) . ?
C18 H18A 0.9900 . ?
C6 C3 1.499(12) . ?
C6 C12 1.592(11) . ?
C6 H6A 0.9900 . ?
C12 C9 1.534(13) . ?
C12 C24 1.528(11) . ?
C12 H12A 0.9900 . ?
C9 C10 1.372(14) . ?
C17 C16 1.351(14) . ?
C17 H17A 0.9400 . ?
C15 C14 1.373(13) . ?
C15 C16 1.402(12) . ?
C16 H16A 0.9400 . ?
C3 C4 1.381(12) . ?
C3 C2 1.381(11) . ?
C5 C4 1.360(12) . ?
C5 H5A 0.9400 . ?
C20 C21 1.365(12) . ?
C20 C19 1.345(12) . ?
C20 H20A 0.9400 . ?
C24 C21 1.519(12) . ?
C24 H24A 0.9900 . ?
C22 C21 1.367(12) . ?
C22 C23 1.392(11) . ?
C22 H22A 0.9400 . ?
C19 N4 1.354(11) . ?
C19 H19A 0.9400 . ?
C2 C1 1.348(12) . ?
C2 H2B 0.9400 . ?
C4 H4A 0.9400 . ?
C1 H1A 0.9400 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C10 C11 1.403(14) . ?
C10 H10A 0.9400 . ?
C14 C13 1.391(14) . ?
C14 H14A 0.9400 . ?
C13 H13A 0.9400 . ?
C23 N4 1.343(10) . ?
C23 H23A 0.9400 . ?
C11 H11A 0.9400 . ?
C7 H7A 0.9400 . ?
N4 Pb1 2.605(7) 4_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pb1 O1 82.3(3) . . ?
N1 Pb1 N4 78.1(2) . 4 ?
O1 Pb1 N4 67.8(3) . 4 ?
N5 O1 Pb1 105.1(6) . . ?
C1 N1 C5 116.3(8) . . ?
C1 N1 Pb1 122.1(6) . . ?
C5 N1 Pb1 121.4(6) . . ?
C7 N2 C11 116.0(9) . . ?
C13 N3 C17 115.5(9) . . ?
O3 N5 O2 123.7(10) . . ?
O3 N5 O1 115.7(9) . . ?
O2 N5 O1 120.5(9) . . ?
O6 N6 O4 119.7(11) . . ?
O6 N6 O5 121.4(12) . . ?
O4 N6 O5 118.9(10) . . ?
C7 C8 C9 115.7(9) . . ?
C7 C8 H8A 122.1 . . ?
C9 C8 H8A 122.1 . . ?
C15 C18 C24 118.5(7) . . ?
C15 C18 C6 114.5(8) . . ?
C24 C18 C6 87.9(6) . . ?
C15 C18 H18A 111.3 . . ?
C24 C18 H18A 111.3 . . ?
C6 C18 H18A 111.3 . . ?
C3 C6 C18 115.7(7) . . ?
C3 C6 C12 115.3(8) . . ?
C18 C6 C12 89.4(6) . . ?
C3 C6 H6A 111.6 . . ?
C18 C6 H6A 111.6 . . ?
C12 C6 H6A 111.6 . . ?
C9 C12 C24 120.3(8) . . ?
C9 C12 C6 116.3(7) . . ?
C24 C12 C6 87.9(6) . . ?
C9 C12 H12A 110.2 . . ?
C24 C12 H12A 110.2 . . ?
C6 C12 H12A 110.2 . . ?
C10 C9 C8 119.1(9) . . ?
C10 C9 C12 121.9(8) . . ?
C8 C9 C12 118.3(8) . . ?
N3 C17 C16 126.6(10) . . ?
N3 C17 H17A 116.7 . . ?
C16 C17 H17A 116.7 . . ?
C14 C15 C16 117.1(9) . . ?
C14 C15 C18 120.1(9) . . ?
C16 C15 C18 122.7(8) . . ?
C17 C16 C15 117.6(9) . . ?
C17 C16 H16A 121.2 . . ?
C15 C16 H16A 121.2 . . ?
C4 C3 C2 116.4(8) . . ?
C4 C3 C6 123.9(8) . . ?
C2 C3 C6 119.3(8) . . ?
N1 C5 C4 122.5(9) . . ?
N1 C5 H5A 118.8 . . ?
C4 C5 H5A 118.8 . . ?
C21 C20 C19 120.0(9) . . ?
C21 C20 H20A 120.0 . . ?
C19 C20 H20A 120.0 . . ?
C21 C24 C12 121.3(7) . . ?
C21 C24 C18 120.1(7) . . ?
C12 C24 C18 91.4(6) . . ?
C21 C24 H24A 107.5 . . ?
C12 C24 H24A 107.5 . . ?
C18 C24 H24A 107.5 . . ?
C21 C22 C23 119.4(8) . . ?
C21 C22 H22A 120.3 . . ?
C23 C22 H22A 120.3 . . ?
N4 C19 C20 124.3(9) . . ?
N4 C19 H19A 117.8 . . ?
C20 C19 H19A 117.8 . . ?
C1 C2 C3 119.8(9) . . ?
C1 C2 H2B 120.1 . . ?
C3 C2 H2B 120.1 . . ?
C5 C4 C3 120.6(8) . . ?
C5 C4 H4A 119.7 . . ?
C3 C4 H4A 119.7 . . ?
N1 C1 C2 124.3(8) . . ?
N1 C1 H1A 117.9 . . ?
C2 C1 H1A 117.9 . . ?
O7 C25 H25A 109.5 . . ?
O7 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O7 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C21 C20 118.0(8) . . ?
C22 C21 C24 123.1(8) . . ?
C20 C21 C24 118.6(8) . . ?
C9 C10 C11 117.7(9) . . ?
C9 C10 H10A 121.1 . . ?
C11 C10 H10A 121.1 . . ?
C15 C14 C13 119.7(10) . . ?
C15 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
N3 C13 C14 123.4(9) . . ?
N3 C13 H13A 118.3 . . ?
C14 C13 H13A 118.3 . . ?
N4 C23 C22 122.7(8) . . ?
N4 C23 H23A 118.7 . . ?
C22 C23 H23A 118.7 . . ?
N2 C11 C10 124.0(11) . . ?
N2 C11 H11A 118.0 . . ?
C10 C11 H11A 118.0 . . ?
N2 C7 C8 126.4(9) . . ?
N2 C7 H7A 116.8 . . ?
C8 C7 H7A 116.8 . . ?
C19 N4 C23 115.4(8) . . ?
C19 N4 Pb1 124.7(6) . 4_556 ?
C23 N4 Pb1 119.1(6) . 4_556 ?

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 Pb1 O1 N5 -108.8(7) . . . . ?
N4 Pb1 O1 N5 170.9(7) 4 . . . ?
O1 Pb1 N1 C1 -31.5(8) . . . . ?
N4 Pb1 N1 C1 37.3(7) 4 . . . ?
O1 Pb1 N1 C5 152.3(7) . . . . ?
N4 Pb1 N1 C5 -138.9(7) 4 . . . ?
Pb1 O1 N5 O3 10.7(11) . . . . ?
Pb1 O1 N5 O2 -168.5(8) . . . . ?
C15 C18 C6 C3 -135.0(8) . . . . ?
C24 C18 C6 C3 104.5(8) . . . . ?
C15 C18 C6 C12 106.9(8) . . . . ?
C24 C18 C6 C12 -13.5(7) . . . . ?
C3 C6 C12 C9 18.6(11) . . . . ?
C18 C6 C12 C9 136.9(8) . . . . ?
C3 C6 C12 C24 -104.4(8) . . . . ?
C18 C6 C12 C24 13.9(7) . . . . ?
C7 C8 C9 C10 -9.0(13) . . . . ?
C7 C8 C9 C12 -179.3(8) . . . . ?
C24 C12 C9 C10 16.5(12) . . . . ?
C6 C12 C9 C10 -87.5(11) . . . . ?
C24 C12 C9 C8 -173.5(8) . . . . ?
C6 C12 C9 C8 82.5(10) . . . . ?
C13 N3 C17 C16 1.7(15) . . . . ?
C24 C18 C15 C14 -111.8(9) . . . . ?
C6 C18 C15 C14 146.6(8) . . . . ?
C24 C18 C15 C16 65.8(11) . . . . ?
C6 C18 C15 C16 -35.8(11) . . . . ?
N3 C17 C16 C15 1.7(14) . . . . ?
C14 C15 C16 C17 -4.6(13) . . . . ?
C18 C15 C16 C17 177.7(8) . . . . ?
C18 C6 C3 C4 -31.4(13) . . . . ?
C12 C6 C3 C4 71.0(11) . . . . ?
C18 C6 C3 C2 155.9(8) . . . . ?
C12 C6 C3 C2 -101.7(10) . . . . ?
C1 N1 C5 C4 -1.5(14) . . . . ?
Pb1 N1 C5 C4 174.9(7) . . . . ?
C9 C12 C24 C21 99.7(10) . . . . ?
C6 C12 C24 C21 -140.8(8) . . . . ?
C9 C12 C24 C18 -133.3(8) . . . . ?
C6 C12 C24 C18 -13.8(7) . . . . ?
C15 C18 C24 C21 25.1(11) . . . . ?
C6 C18 C24 C21 142.0(8) . . . . ?
C15 C18 C24 C12 -102.8(8) . . . . ?
C6 C18 C24 C12 14.1(7) . . . . ?
C21 C20 C19 N4 0.3(16) . . . . ?
C4 C3 C2 C1 0.3(14) . . . . ?
C6 C3 C2 C1 173.6(9) . . . . ?
N1 C5 C4 C3 -1.6(15) . . . . ?
C2 C3 C4 C5 2.1(13) . . . . ?
C6 C3 C4 C5 -170.8(9) . . . . ?
C5 N1 C1 C2 4.1(15) . . . . ?
Pb1 N1 C1 C2 -172.2(8) . . . . ?
C3 C2 C1 N1 -3.6(16) . . . . ?
C23 C22 C21 C20 1.3(14) . . . . ?
C23 C22 C21 C24 -172.2(9) . . . . ?
C19 C20 C21 C22 -2.8(15) . . . . ?
C19 C20 C21 C24 170.9(9) . . . . ?
C12 C24 C21 C22 -10.9(13) . . . . ?
C18 C24 C21 C22 -123.6(9) . . . . ?
C12 C24 C21 C20 175.7(9) . . . . ?
C18 C24 C21 C20 63.0(12) . . . . ?
C8 C9 C10 C11 4.5(13) . . . . ?
C12 C9 C10 C11 174.5(8) . . . . ?
C16 C15 C14 C13 4.2(13) . . . . ?
C18 C15 C14 C13 -178.0(8) . . . . ?
C17 N3 C13 C14 -2.2(15) . . . . ?
C15 C14 C13 N3 -0.8(16) . . . . ?
C21 C22 C23 N4 2.9(14) . . . . ?
C7 N2 C11 C10 5.1(14) . . . . ?
C9 C10 C11 N2 -2.4(15) . . . . ?
C11 N2 C7 C8 -10.7(15) . . . . ?
C9 C8 C7 N2 12.8(15) . . . . ?
C20 C19 N4 C23 3.7(15) . . . . ?
C20 C19 N4 Pb1 -166.0(8) . . . 4_556 ?
C22 C23 N4 C19 -5.3(14) . . . . ?
C22 C23 N4 Pb1 165.0(7) . . . 4_556 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.211
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.170
####################################################################### 
# 
# 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 1413679'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 N6 O7 Pb'
_chemical_formula_sum            'C24 H22 N6 O7 Pb'
_chemical_formula_weight         713.68

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                   12.0677(4)
_cell_length_b                   18.1490(4)
_cell_length_c                   12.1215(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.818(4)
_cell_angle_gamma                90.00
_cell_volume                     2481.49(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    7127
_cell_measurement_theta_min      3.1580
_cell_measurement_theta_max      30.0060

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1384
_exptl_absorpt_coefficient_mu    6.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0257
_exptl_absorpt_correction_T_max  0.0355
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.4471
_diffrn_standards_number         17805
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13856
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4364
_reflns_number_gt                3764
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 '
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 '
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 '
_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)+(0.0376P)²+0.7952P] 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         4364
_refine_ls_number_parameters     366
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0660
_refine_ls_wR_factor_gt          0.0634
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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 1.399277(15) -0.023679(8) 0.800359(14) 0.02190(8) Uani 1 1 d . . .
O7 O 1.2787(4) 0.07969(19) 0.8654(3) 0.0369(9) Uani 1 1 d . . .
N6 N 1.6777(4) -0.0322(2) 0.8410(4) 0.0366(11) Uani 1 1 d . . .
O1 O 1.6258(3) -0.07957(17) 0.8845(3) 0.0374(8) Uani 1 1 d . . .
N1 N 1.2992(4) 0.0614(2) 0.6028(4) 0.0414(11) Uani 1 1 d . A .
N5 N 1.4410(4) -0.1312(2) 1.0155(4) 0.0299(9) Uani 1 1 d . . .
C5 C 1.2628(6) 0.0437(3) 0.4895(5) 0.0471(15) Uani 1 1 d . . .
H5A H 1.2547 -0.0064 0.4690 0.056 Uiso 1 1 calc R . .
C13 C 1.5111(5) 0.3313(3) 0.1817(5) 0.0472(14) Uani 1 1 d . . .
H13A H 1.5603 0.3213 0.1383 0.057 Uiso 1 1 calc R . .
C10 C 1.3561(5) 0.2917(3) 0.2414(4) 0.0365(13) Uani 1 1 d . . .
C4 C 1.2356(5) 0.0961(3) 0.3986(5) 0.0442(14) Uani 1 1 d . A .
H4 H 1.2124 0.0810 0.3194 0.053 Uiso 1 1 calc R . .
C20 C 0.9993(5) 0.1712(3) 0.2336(5) 0.0397(13) Uani 1 1 d . . .
C12 C 1.4482(6) 0.4103(3) 0.2906(6) 0.0514(16) Uani 1 1 d . . .
H12A H 1.4516 0.4567 0.3264 0.062 Uiso 1 1 calc R A .
O3 O 1.7855(4) -0.0249(2) 0.8858(4) 0.0605(12) Uani 1 1 d . . .
C15 C 1.1296(5) 0.2741(3) 0.0429(4) 0.0381(12) Uani 1 1 d U . .
C19 C 1.1659(5) 0.2562(3) -0.0470(5) 0.0421(14) Uani 1 1 d . A .
H19A H 1.1997 0.2098 -0.0488 0.050 Uiso 1 1 calc R . .
N2 N 1.5262(4) 0.3958(2) 0.2380(4) 0.0470(12) Uani 1 1 d . A .
O4 O 1.4348(3) -0.06102(15) 1.0200(3) 0.0323(8) Uani 1 1 d . . .
C23 C 0.8794(5) 0.1173(3) 0.3286(5) 0.0378(12) Uani 1 1 d . . .
H23A H 0.8615 0.1129 0.3978 0.045 Uiso 1 1 calc R A .
C22 C 0.8470(5) 0.0814(3) 0.1397(5) 0.0401(13) Uani 1 1 d . . .
H22A H 0.8058 0.0530 0.0728 0.048 Uiso 1 1 calc R A .
C21 C 0.9396(5) 0.1269(3) 0.1372(5) 0.0454(14) Uani 1 1 d . A .
H21A H 0.9615 0.1275 0.0701 0.055 Uiso 1 1 calc R . .
C3 C 1.2436(4) 0.1704(3) 0.4273(5) 0.0369(12) Uani 1 1 d . . .
C2 C 1.2793(5) 0.1883(3) 0.5440(5) 0.0438(14) Uani 1 1 d . A .
H2B H 1.2847 0.2380 0.5675 0.053 Uiso 1 1 calc R . .
C14 C 1.4318(5) 0.2794(3) 0.1817(5) 0.0436(14) Uani 1 1 d . A .
H14A H 1.4281 0.2349 0.1409 0.052 Uiso 1 1 calc R . .
C18 C 1.1531(5) 0.3066(3) -0.1364(5) 0.0410(14) Uani 1 1 d . . .
H18A H 1.1797 0.2930 -0.1975 0.049 Uiso 1 1 calc R A .
C16 C 1.0777(5) 0.3434(3) 0.0392(5) 0.0428(12) Uani 1 1 d U A .
H16A H 1.0504 0.3579 0.0995 0.051 Uiso 1 1 calc R . .
C17 C 1.0669(5) 0.3907(3) -0.0546(5) 0.0395(13) Uani 1 1 d . . .
H17A H 1.0308 0.4368 -0.0565 0.047 Uiso 1 1 calc R A .
C1 C 1.3073(5) 0.1329(3) 0.6274(5) 0.0402(13) Uani 1 1 d . . .
H1A H 1.3340 0.1467 0.7073 0.048 Uiso 1 1 calc R A .
C11 C 1.3621(5) 0.3605(3) 0.2951(5) 0.0486(15) Uani 1 1 d . A .
H11A H 1.3093 0.3728 0.3335 0.058 Uiso 1 1 calc R . .
N4 N 0.8157(4) 0.0772(2) 0.2347(4) 0.0331(9) Uani 1 1 d . . .
O2 O 1.6160(4) 0.0040(2) 0.7544(4) 0.0496(10) Uani 1 1 d . . .
N3 N 1.1051(4) 0.3736(2) -0.1411(3) 0.0337(10) Uani 1 1 d . . .
O5 O 1.4137(4) -0.16029(17) 0.9167(3) 0.0476(10) Uani 1 1 d . . .
O6 O 1.4726(4) -0.1670(2) 1.1062(4) 0.0661(13) Uani 1 1 d . . .
C24 C 0.9678(5) 0.1639(3) 0.3305(5) 0.0398(13) Uani 1 1 d . A .
H24A H 1.0077 0.1914 0.3990 0.048 Uiso 1 1 calc R . .
C7 C 1.2773(5) 0.2275(3) 0.2469(4) 0.0247(15) Uani 0.845(8) 1 d P A 1
H7B H 1.3224 0.1808 0.2581 0.030 Uiso 0.845(8) 1 calc PR A 1
C9 C 1.0904(5) 0.2285(3) 0.2337(5) 0.0241(14) Uani 0.845(8) 1 d P A 1
H9A H 1.0530 0.2778 0.2230 0.029 Uiso 0.845(8) 1 calc PR A 1
C8 C 1.1544(5) 0.2189(3) 0.1426(5) 0.0242(14) Uani 0.845(8) 1 d P A 1
H8A H 1.1445 0.1680 0.1114 0.029 Uiso 0.845(8) 1 calc PR A 1
C6 C 1.2128(5) 0.2322(3) 0.3365(5) 0.0238(14) Uani 0.845(8) 1 d P A 1
H6A H 1.2249 0.2810 0.3754 0.029 Uiso 0.845(8) 1 calc PR A 1
C7A C 1.242(2) 0.2677(14) 0.286(2) 0.012(7) Uiso 0.155(8) 1 d P A 2
C9A C 1.121(2) 0.1761(14) 0.177(2) 0.014(7) Uiso 0.155(8) 1 d P A 2
C8A C 1.117(3) 0.2617(17) 0.175(3) 0.025(8) Uiso 0.155(8) 1 d P A 2
C6A C 1.245(2) 0.1796(13) 0.287(2) 0.015(7) Uiso 0.155(8) 1 d P A 2
HW1 H 1.196(4) 0.081(2) 0.825(4) 0.018 Uiso 1 1 d . . .
HW2 H 1.292(4) 0.083(2) 0.930(4) 0.018 Uiso 1 1 d . . .


_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 O4 2.630(3) . ?
Pb1 N4 2.659(4) 3_756 ?
Pb1 O7 2.660(4) . ?
Pb1 N3 2.671(4) 2_745 ?
Pb1 N1 2.743(4) . ?
Pb1 O1 2.749(4) . ?
O7 HW1 0.94(5) . ?
O7 HW2 0.74(5) . ?
N6 O3 1.226(6) . ?
N6 O2 1.238(6) . ?
N6 O1 1.283(5) . ?
N1 C5 1.323(7) . ?
N1 C1 1.327(7) . ?
N5 O6 1.215(5) . ?
N5 O5 1.242(5) . ?
N5 O4 1.278(5) . ?
C5 C4 1.403(7) . ?
C5 H5A 0.9400 . ?
C13 N2 1.335(7) . ?
C13 C14 1.342(7) . ?
C13 H13A 0.9400 . ?
C10 C14 1.371(7) . ?
C10 C11 1.397(8) . ?
C10 C7 1.520(7) . ?
C10 C7A 1.70(3) . ?
C4 C3 1.388(7) . ?
C4 H4 0.9400 . ?
C20 C24 1.363(7) . ?
C20 C21 1.391(8) . ?
C20 C9 1.514(7) . ?
C20 C9A 1.83(3) . ?
C12 N2 1.337(7) . ?
C12 C11 1.394(8) . ?
C12 H12A 0.9400 . ?
C15 C19 1.350(7) . ?
C15 C16 1.399(8) . ?
C15 C8 1.515(7) . ?
C15 C8A 1.68(3) . ?
C19 C18 1.384(7) . ?
C19 H19A 0.9400 . ?
C23 N4 1.340(6) . ?
C23 C24 1.356(7) . ?
C23 H23A 0.9400 . ?
C22 N4 1.336(6) . ?
C22 C21 1.398(7) . ?
C22 H22A 0.9400 . ?
C21 H21A 0.9400 . ?
C3 C2 1.363(7) . ?
C3 C6 1.521(7) . ?
C3 C6A 1.72(3) . ?
C2 C1 1.380(7) . ?
C2 H2B 0.9400 . ?
C14 H14A 0.9400 . ?
C18 N3 1.339(6) . ?
C18 H18A 0.9400 . ?
C16 C17 1.393(7) . ?
C16 H16A 0.9400 . ?
C17 N3 1.323(6) . ?
C17 H17A 0.9400 . ?
C1 H1A 0.9400 . ?
C11 H11A 0.9400 . ?
N4 Pb1 2.659(4) 3_756 ?
N3 Pb1 2.671(4) 2_755 ?
C24 H24A 0.9400 . ?
C7 C6 1.547(7) . ?
C7 C8 1.577(7) . ?
C7 H7B 0.9900 . ?
C9 C6 1.559(7) . ?
C9 C8 1.566(8) . ?
C9 H9A 0.9900 . ?
C8 H8A 0.9900 . ?
C6 H6A 0.9900 . ?
C7A C6A 1.60(3) . ?
C7A C8A 1.63(4) . ?
C9A C8A 1.55(4) . ?
C9A C6A 1.61(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
O4 Pb1 N4 82.31(11) . 3_756 ?
O4 Pb1 O7 77.95(10) . . ?
N4 Pb1 O7 72.53(12) 3_756 . ?
O4 Pb1 N3 120.39(10) . 2_745 ?
N4 Pb1 N3 82.07(13) 3_756 2_745 ?
O7 Pb1 N3 146.55(13) . 2_745 ?
O4 Pb1 N1 153.07(12) . . ?
N4 Pb1 N1 87.96(13) 3_756 . ?
O7 Pb1 N1 75.18(12) . . ?
N3 Pb1 N1 82.67(13) 2_745 . ?
O4 Pb1 O1 75.32(10) . . ?
N4 Pb1 O1 135.18(11) 3_756 . ?
O7 Pb1 O1 136.61(11) . . ?
N3 Pb1 O1 76.83(11) 2_745 . ?
N1 Pb1 O1 127.07(12) . . ?
Pb1 O7 HW1 117(3) . . ?
Pb1 O7 HW2 115(4) . . ?
HW1 O7 HW2 110(5) . . ?
O3 N6 O2 122.9(5) . . ?
O3 N6 O1 119.1(5) . . ?
O2 N6 O1 118.0(4) . . ?
N6 O1 Pb1 99.6(3) . . ?
C5 N1 C1 116.2(4) . . ?
C5 N1 Pb1 130.6(3) . . ?
C1 N1 Pb1 112.3(3) . . ?
O6 N5 O5 122.4(4) . . ?
O6 N5 O4 119.9(4) . . ?
O5 N5 O4 117.7(4) . . ?
N1 C5 C4 123.3(5) . . ?
N1 C5 H5A 118.3 . . ?
C4 C5 H5A 118.3 . . ?
N2 C13 C14 125.6(6) . . ?
N2 C13 H13A 117.2 . . ?
C14 C13 H13A 117.2 . . ?
C14 C10 C11 117.2(5) . . ?
C14 C10 C7 116.3(5) . . ?
C11 C10 C7 126.4(5) . . ?
C14 C10 C7A 152.9(10) . . ?
C11 C10 C7A 89.8(10) . . ?
C7 C10 C7A 37.0(8) . . ?
C3 C4 C5 119.0(5) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C24 C20 C21 116.7(5) . . ?
C24 C20 C9 119.4(5) . . ?
C21 C20 C9 123.8(5) . . ?
C24 C20 C9A 146.5(9) . . ?
C21 C20 C9A 87.6(9) . . ?
C9 C20 C9A 44.5(8) . . ?
N2 C12 C11 123.4(5) . . ?
N2 C12 H12A 118.3 . . ?
C11 C12 H12A 118.3 . . ?
C19 C15 C16 117.4(5) . . ?
C19 C15 C8 117.1(5) . . ?
C16 C15 C8 125.4(5) . . ?
C19 C15 C8A 154.7(12) . . ?
C16 C15 C8A 87.7(11) . . ?
C8 C15 C8A 37.7(11) . . ?
C15 C19 C18 119.7(5) . . ?
C15 C19 H19A 120.2 . . ?
C18 C19 H19A 120.2 . . ?
C13 N2 C12 115.2(5) . . ?
N5 O4 Pb1 101.8(2) . . ?
N4 C23 C24 124.3(5) . . ?
N4 C23 H23A 117.8 . . ?
C24 C23 H23A 117.8 . . ?
N4 C22 C21 121.7(5) . . ?
N4 C22 H22A 119.2 . . ?
C21 C22 H22A 119.2 . . ?
C20 C21 C22 120.2(5) . . ?
C20 C21 H21A 119.9 . . ?
C22 C21 H21A 119.9 . . ?
C2 C3 C4 117.4(5) . . ?
C2 C3 C6 118.8(5) . . ?
C4 C3 C6 123.9(5) . . ?
C2 C3 C6A 153.6(10) . . ?
C4 C3 C6A 82.5(9) . . ?
C6 C3 C6A 45.3(8) . . ?
C3 C2 C1 119.4(5) . . ?
C3 C2 H2B 120.3 . . ?
C1 C2 H2B 120.3 . . ?
C13 C14 C10 119.7(5) . . ?
C13 C14 H14A 120.2 . . ?
C10 C14 H14A 120.2 . . ?
N3 C18 C19 124.0(5) . . ?
N3 C18 H18A 118.0 . . ?
C19 C18 H18A 118.0 . . ?
C17 C16 C15 119.4(5) . . ?
C17 C16 H16A 120.3 . . ?
C15 C16 H16A 120.3 . . ?
N3 C17 C16 123.0(5) . . ?
N3 C17 H17A 118.5 . . ?
C16 C17 H17A 118.5 . . ?
N1 C1 C2 124.6(5) . . ?
N1 C1 H1A 117.7 . . ?
C2 C1 H1A 117.7 . . ?
C12 C11 C10 118.6(6) . . ?
C12 C11 H11A 120.7 . . ?
C10 C11 H11A 120.7 . . ?
C22 N4 C23 116.7(4) . . ?
C22 N4 Pb1 116.2(3) . 3_756 ?
C23 N4 Pb1 124.5(3) . 3_756 ?
C17 N3 C18 116.5(4) . . ?
C17 N3 Pb1 119.1(3) . 2_755 ?
C18 N3 Pb1 124.2(3) . 2_755 ?
C23 C24 C20 120.3(5) . . ?
C23 C24 H24A 119.9 . . ?
C20 C24 H24A 119.9 . . ?
C10 C7 C6 117.8(4) . . ?
C10 C7 C8 117.7(4) . . ?
C6 C7 C8 90.2(4) . . ?
C10 C7 H7B 109.9 . . ?
C6 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
C20 C9 C6 120.8(4) . . ?
C20 C9 C8 117.7(4) . . ?
C6 C9 C8 90.2(4) . . ?
C20 C9 H9A 108.9 . . ?
C6 C9 H9A 108.9 . . ?
C8 C9 H9A 108.9 . . ?
C15 C8 C9 118.8(5) . . ?
C15 C8 C7 115.9(4) . . ?
C9 C8 C7 89.0(4) . . ?
C15 C8 H8A 110.5 . . ?
C9 C8 H8A 110.5 . . ?
C7 C8 H8A 110.5 . . ?
C3 C6 C7 114.4(4) . . ?
C3 C6 C9 117.8(4) . . ?
C7 C6 C9 90.3(4) . . ?
C3 C6 H6A 110.9 . . ?
C7 C6 H6A 110.9 . . ?
C9 C6 H6A 110.9 . . ?
C6A C7A C8A 87.0(19) . . ?
C6A C7A C10 104.2(17) . . ?
C8A C7A C10 112.1(19) . . ?
C8A C9A C6A 89.1(19) . . ?
C8A C9A C20 91.8(17) . . ?
C6A C9A C20 109.0(17) . . ?
C9A C8A C7A 92(2) . . ?
C9A C8A C15 98(2) . . ?
C7A C8A C15 114(2) . . ?
C7A C6A C9A 91.4(18) . . ?
C7A C6A C3 95.6(16) . . ?
C9A C6A C3 118.9(19) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.469
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.113
