# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_9414rrrp2c
_database_code_depnum_ccdc_archive 'CCDC 859172'
loop_
_audit_author_name
_audit_author_address
'Abdul Malik Abdul Malik Peedikakkal'
;King Fahd University of Petroleum and Minerals
Saudi Arabia
;
_audit_update_record             
;
2020-12-24 deposited with the CCDC.	2021-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H19 N2 O8 Pb2'
_chemical_formula_weight         817.74

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2/c

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

_cell_length_a                   13.6568(10)
_cell_length_b                   4.4427(3)
_cell_length_c                   18.6786(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.1950(10)
_cell_angle_gamma                90.00
_cell_volume                     1111.72(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    6780
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      27.53

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_diffrn    2.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             750
_exptl_absorpt_coefficient_mu    15.171
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.0543
_exptl_absorpt_correction_T_max  0.3123
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7342
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2552
_reflns_number_gt                2306
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0394P)²+14.7719P] 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         2552
_refine_ls_number_parameters     210
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1327
_refine_ls_wR_factor_gt          0.1291
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.129
_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 0.13788(3) 0.16396(11) 0.73343(2) 0.05005(18) Uani 1 1 d . . .
N1 N 0.2579(8) 0.110(2) 0.6452(6) 0.062(3) Uani 1 1 d D B .
C3 C 0.3884(8) 0.013(3) 0.5489(6) 0.059(3) Uani 1 1 d D . .
C6 C 0.4542(9) -0.050(3) 0.4973(7) 0.060(3) Uani 1 1 d . . .
H6 H 0.4286 -0.1717 0.4569 0.072 Uiso 1 1 calc R . .
C7 C -0.0130(8) 0.521(3) 0.6295(6) 0.049(2) Uani 1 1 d . . .
C8 C -0.0806(11) 0.681(5) 0.5711(9) 0.089(6) Uani 1 1 d . C .
H8A H -0.1031 0.8657 0.5902 0.107 Uiso 1 1 calc R . .
H8B H -0.1377 0.5542 0.5524 0.107 Uiso 1 1 calc R . .
H8C H -0.0456 0.7277 0.5320 0.107 Uiso 1 1 calc R . .
C9 C 0.2946(11) 0.528(4) 0.8202(10) 0.084(5) Uani 1 1 d . . .
O3 O 0.2356(6) 0.6061(18) 0.7644(5) 0.056(2) Uani 1 1 d . A .
O4A O 0.3163(15) 0.271(6) 0.8318(12) 0.061(6) Uani 0.50 1 d P A .
C10B C 0.384(4) 0.734(10) 0.829(4) 0.17(3) Uani 0.50 1 d P A 2
H10A H 0.4417 0.6202 0.8223 0.209 Uiso 0.50 1 calc PR A 2
H10B H 0.3957 0.8204 0.8777 0.209 Uiso 0.50 1 calc PR A 2
H10C H 0.3705 0.8935 0.7931 0.209 Uiso 0.50 1 calc PR A 2
O4B O 0.277(3) 0.313(7) 0.8605(16) 0.105(10) Uani 0.50 1 d P A 2
C1A C 0.2269(19) 0.017(4) 0.5802(16) 0.039(5) Uani 0.50 1 d PD B 1
H1A H 0.1577 -0.0113 0.5654 0.047 Uiso 0.50 1 calc PR B 1
C2A C 0.287(2) -0.050(6) 0.5278(15) 0.045(7) Uani 0.50 1 d PD B 1
H2A H 0.2601 -0.1311 0.4817 0.054 Uiso 0.50 1 calc PR B 1
C4A C 0.4313(18) 0.081(7) 0.6251(15) 0.057(7) Uani 0.50 1 d PD B 1
H4A H 0.5008 0.0934 0.6411 0.068 Uiso 0.50 1 calc PR B 1
C5A C 0.3686(18) 0.126(6) 0.6725(12) 0.048(6) Uani 0.50 1 d PD B 1
H5A H 0.3945 0.1673 0.7220 0.058 Uiso 0.50 1 calc PR B 1
C1B C 0.243(2) -0.099(5) 0.5988(14) 0.040(6) Uani 0.50 1 d PD B 2
H1B H 0.1867 -0.2221 0.5972 0.048 Uiso 0.50 1 calc PR B 2
C2B C 0.305(2) -0.159(8) 0.5504(15) 0.060(9) Uani 0.50 1 d PD B 2
H2B H 0.2894 -0.3209 0.5177 0.072 Uiso 0.50 1 calc PR B 2
C4B C 0.402(2) 0.240(6) 0.5979(15) 0.059(7) Uani 0.50 1 d PD B 2
H4B H 0.4579 0.3651 0.6007 0.070 Uiso 0.50 1 calc PR B 2
C5B C 0.339(2) 0.293(6) 0.6422(16) 0.068(9) Uani 0.50 1 d PD B 2
H5B H 0.3499 0.4626 0.6729 0.082 Uiso 0.50 1 calc PR B 2
O1A O 0.0696(10) 0.604(3) 0.6473(8) 0.036(3) Uani 0.50 1 d P C 3
O2A O -0.0533(15) 0.280(4) 0.6402(9) 0.058(4) Uani 0.50 1 d P C 3
O1B O 0.0697(11) 0.384(4) 0.6225(8) 0.052(4) Uani 0.50 1 d P C 4
O2B O -0.0235(9) 0.527(4) 0.7010(7) 0.049(4) Uani 0.50 1 d P . 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1B 2.317(14) . ?
Pb1 O3 2.382(8) . ?
Pb1 N1 2.551(9) . ?
Pb1 O1A 2.588(13) . ?
Pb1 O2B 2.700(14) 2_556 ?
Pb1 O2B 2.703(16) . ?
N1 C1B 1.26(3) . ?
N1 C1A 1.27(3) . ?
N1 C5B 1.38(3) . ?
N1 C5A 1.50(3) . ?
C3 C4B 1.35(3) . ?
C3 C2B 1.38(4) . ?
C3 C2A 1.39(3) . ?
C3 C4A 1.46(3) . ?
C3 C6 1.467(13) . ?
C6 C6 1.31(2) 3_656 ?
C7 O1A 1.172(17) . ?
C7 O2A 1.240(19) . ?
C7 O1B 1.31(2) . ?
C7 O2B 1.370(16) . ?
C7 C8 1.468(19) . ?
C9 O4A 1.19(3) . ?
C9 O3 1.237(16) . ?
C9 O4B 1.27(4) . ?
C9 C10B 1.50(5) . ?
O4A O4B 0.85(4) . ?
C1A C2A 1.43(4) . ?
C4A C5A 1.36(3) . ?
C1B C2B 1.37(4) . ?
C4B C5B 1.32(4) . ?
O2B O2B 1.82(3) 2_556 ?
O2B Pb1 2.700(14) 2_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
O1B Pb1 O3 88.8(5) . . ?
O1B Pb1 N1 70.0(5) . . ?
O3 Pb1 N1 80.4(3) . . ?
O1B Pb1 O1A 24.8(5) . . ?
O3 Pb1 O1A 69.2(4) . . ?
N1 Pb1 O1A 82.4(4) . . ?
O1B Pb1 O2B 89.2(5) . 2_556 ?
O3 Pb1 O2B 75.1(4) . 2_556 ?
N1 Pb1 O2B 148.2(5) . 2_556 ?
O1A Pb1 O2B 70.1(5) . 2_556 ?
O1B Pb1 O2B 51.6(5) . . ?
O3 Pb1 O2B 87.5(4) . . ?
N1 Pb1 O2B 120.6(4) . . ?
O1A Pb1 O2B 39.6(4) . . ?
O2B Pb1 O2B 39.4(6) 2_556 . ?
C1B N1 C1A 29.1(10) . . ?
C1B N1 C5B 115.3(18) . . ?
C1A N1 C5B 105.8(16) . . ?
C1B N1 C5A 106.5(15) . . ?
C1A N1 C5A 117.7(15) . . ?
C5B N1 C5A 39.2(13) . . ?
C1B N1 Pb1 118.4(14) . . ?
C1A N1 Pb1 120.6(13) . . ?
C5B N1 Pb1 126.3(12) . . ?
C5A N1 Pb1 120.5(9) . . ?
C4B C3 C2B 113.8(19) . . ?
C4B C3 C2A 109.8(19) . . ?
C2B C3 C2A 27.5(13) . . ?
C4B C3 C4A 37.8(14) . . ?
C2B C3 C4A 105.8(16) . . ?
C2A C3 C4A 120.5(16) . . ?
C4B C3 C6 124.6(15) . . ?
C2B C3 C6 121.7(16) . . ?
C2A C3 C6 118.6(16) . . ?
C4A C3 C6 119.9(12) . . ?
C6 C6 C3 125.6(13) 3_656 . ?
O1A C7 O2A 131.3(15) . . ?
O1A C7 O1B 51.4(10) . . ?
O2A C7 O1B 91.8(15) . . ?
O1A C7 O2B 89.7(12) . . ?
O2A C7 O2B 74.1(12) . . ?
O1B C7 O2B 111.2(12) . . ?
O1A C7 C8 119.4(12) . . ?
O2A C7 C8 107.6(14) . . ?
O1B C7 C8 125.4(12) . . ?
O2B C7 C8 123.1(13) . . ?
O4A C9 O3 121.4(17) . . ?
O4A C9 O4B 40.2(16) . . ?
O3 C9 O4B 123(2) . . ?
O4A C9 C10B 113(2) . . ?
O3 C9 C10B 108(3) . . ?
O4B C9 C10B 129(3) . . ?
C9 O3 Pb1 102.5(10) . . ?
O4B O4A C9 75(3) . . ?
O4A O4B C9 65(3) . . ?
N1 C1A C2A 126(2) . . ?
C3 C2A C1A 116(2) . . ?
C5A C4A C3 119(2) . . ?
C4A C5A N1 119.4(19) . . ?
N1 C1B C2B 124(3) . . ?
C1B C2B C3 121(3) . . ?
C5B C4B C3 123(2) . . ?
C4B C5B N1 123(2) . . ?
C7 O1A Pb1 98.6(9) . . ?
C7 O1B Pb1 108.1(10) . . ?
C7 O2B O2B 153.9(14) . 2_556 ?
C7 O2B Pb1 127.6(11) . 2_556 ?
O2B O2B Pb1 70.4(6) 2_556 2_556 ?
C7 O2B Pb1 88.4(9) . . ?
O2B O2B Pb1 70.2(6) 2_556 . ?
Pb1 O2B Pb1 93.4(5) 2_556 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         5.391
_refine_diff_density_min         -1.940
_refine_diff_density_rms         0.241
####################################################################### 
# 
# 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_9436n
_database_code_depnum_ccdc_archive 'CCDC 859173'
loop_
_audit_author_name
_audit_author_address
'Abdul Malik Abdul Malik Peedikakkal'
;King Fahd University of Petroleum and Minerals
Saudi Arabia
;
_audit_update_record             
;
2020-12-24 deposited with the CCDC.	2021-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H24 N4 O8 Pb2'
_chemical_formula_weight         958.89

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2/c

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

_cell_length_a                   18.508(2)
_cell_length_b                   4.0982(5)
_cell_length_c                   18.984(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.680(2)
_cell_angle_gamma                90.00
_cell_volume                     1430.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3418
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      27.52

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    11.813
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.1078
_exptl_absorpt_correction_T_max  0.6494
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6387
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.11
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2511
_reflns_number_gt                1971
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0695P)²+13.3890P] 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         2511
_refine_ls_number_parameters     109
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1274
_refine_ls_wR_factor_gt          0.1202
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.056
_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 0.244920(19) 0.23489(8) 0.25507(2) 0.01681(18) Uani 1 1 d . . .
N1 N 0.3319(12) 0.269(8) 0.1605(13) 0.0273(17) Uani 0.50 1 d PG A 1
C1 C 0.4029(13) 0.163(6) 0.1795(10) 0.0273(17) Uani 0.50 1 d PG A 1
H1 H 0.4154 0.0550 0.2235 0.033 Uiso 0.50 1 calc PR A 1
C2 C 0.4555(10) 0.215(5) 0.1340(9) 0.0273(17) Uani 0.50 1 d PG A 1
H2 H 0.5039 0.1426 0.1470 0.033 Uiso 0.50 1 calc PR A 1
C3 C 0.4371(7) 0.373(4) 0.0696(8) 0.0273(17) Uani 0.50 1 d PG A 1
C4 C 0.3661(8) 0.479(5) 0.0507(10) 0.0273(17) Uani 0.50 1 d PG A 1
H4 H 0.3536 0.5864 0.0067 0.033 Uiso 0.50 1 calc PR A 1
C5 C 0.3135(7) 0.427(7) 0.0961(14) 0.0273(17) Uani 0.50 1 d PG A 1
H5 H 0.2651 0.4989 0.0832 0.033 Uiso 0.50 1 calc PR A 1
C6 C 0.5007(12) 0.403(5) 0.0279(9) 0.0273(17) Uani 0.50 1 d PD . 1
H6 H 0.5434 0.2792 0.0419 0.033 Uiso 0.50 1 calc PR . 1
N21 N 0.3283(13) 0.285(8) 0.1568(13) 0.0273(17) Uani 0.50 1 d PG A 2
C21 C 0.4028(13) 0.228(6) 0.1680(10) 0.0273(17) Uani 0.50 1 d PG A 2
H21 H 0.4238 0.1331 0.2112 0.033 Uiso 0.50 1 calc PR A 2
C22 C 0.4465(9) 0.309(5) 0.1158(9) 0.0273(17) Uani 0.50 1 d PG A 2
H22 H 0.4974 0.2702 0.1234 0.033 Uiso 0.50 1 calc PR A 2
C23 C 0.4157(8) 0.447(5) 0.0525(8) 0.0273(17) Uani 0.50 1 d PG A 2
C24 C 0.3412(8) 0.504(5) 0.0413(10) 0.0273(17) Uani 0.50 1 d PG A 2
H24 H 0.3201 0.5990 -0.0019 0.033 Uiso 0.50 1 calc PR A 2
C25 C 0.2975(8) 0.423(7) 0.0935(14) 0.0273(17) Uani 0.50 1 d PG A 2
H25 H 0.2466 0.4619 0.0859 0.033 Uiso 0.50 1 calc PR A 2
C26 C 0.4653 0.5440 -0.0013 0.027 Uani 0.50 1 d PD . 2
H26 H 0.4457 0.6772 -0.0398 0.033 Uiso 0.50 1 calc PR . 2
N2 N 0.1599(11) 0.860(5) 0.3401(12) 0.0238(15) Uani 0.50 1 d PG B 1
C8 C 0.1004(13) 0.676(5) 0.3119(8) 0.0238(15) Uani 0.50 1 d PG B 1
H8 H 0.0930 0.6318 0.2625 0.029 Uiso 0.50 1 calc PR B 1
C9 C 0.0516(9) 0.557(4) 0.3560(8) 0.0238(15) Uani 0.50 1 d PG B 1
H9 H 0.0109 0.4310 0.3367 0.029 Uiso 0.50 1 calc PR B 1
C10 C 0.0623(7) 0.622(4) 0.4283(7) 0.0238(15) Uani 0.50 1 d PG B 1
C11 C 0.1218(8) 0.806(4) 0.4565(8) 0.0238(15) Uani 0.50 1 d PG B 1
H11 H 0.1291 0.8504 0.5060 0.029 Uiso 0.50 1 calc PR B 1
C12 C 0.1706(8) 0.925(5) 0.4124(13) 0.0238(15) Uani 0.50 1 d PG B 1
H12 H 0.2112 1.0511 0.4317 0.029 Uiso 0.50 1 calc PR B 1
C13 C 0.0044(12) 0.463(6) 0.4669(6) 0.0238(15) Uani 0.50 1 d PD . 1
H13 H -0.0267 0.3047 0.4427 0.029 Uiso 0.50 1 calc PR . 1
N22 N 0.1648(12) 0.846(6) 0.3444(12) 0.0238(15) Uani 0.50 1 d PG C 2
C28 C 0.0993(13) 0.683(5) 0.3265(8) 0.0238(15) Uani 0.50 1 d PG C 2
H28 H 0.0845 0.6259 0.2785 0.029 Uiso 0.50 1 calc PR C 2
C29 C 0.0554(9) 0.605(4) 0.3787(8) 0.0238(15) Uani 0.50 1 d PG C 2
H29 H 0.0106 0.4946 0.3665 0.029 Uiso 0.50 1 calc PR C 2
C30 C 0.0771(8) 0.690(4) 0.4489(7) 0.0238(15) Uani 0.50 1 d PG C 2
C31 C 0.1426(8) 0.852(5) 0.4669(9) 0.0238(15) Uani 0.50 1 d PG C 2
H31 H 0.1574 0.9097 0.5149 0.029 Uiso 0.50 1 calc PR C 2
C32 C 0.1864(8) 0.930(5) 0.4147(13) 0.0238(15) Uani 0.50 1 d PG C 2
H32 H 0.2312 1.0410 0.4269 0.029 Uiso 0.50 1 calc PR C 2
C33 C 0.0284(8) 0.599(5) 0.5039(13) 0.0238(15) Uani 0.50 1 d PD . 2
H33 H 0.0398 0.6943 0.5495 0.029 Uiso 0.50 1 calc PR . 2
C1S C 0.3574(6) -0.136(3) 0.3482(7) 0.032(3) Uani 1 1 d U . .
H1S H 0.3914 -0.2867 0.3711 0.038 Uiso 1 1 calc R A .
O1 O 0.3300(4) -0.2044(18) 0.2864(5) 0.0297(19) Uani 1 1 d . A .
O2 O 0.3439(5) 0.110(2) 0.3816(5) 0.048(3) Uani 1 1 d . A .
C2S C 0.1389(7) -0.105(3) 0.1510(6) 0.029(3) Uani 1 1 d U . .
H2S H 0.1131 -0.2431 0.1165 0.034 Uiso 1 1 calc R A .
O3 O 0.2012(5) -0.1934(19) 0.1764(4) 0.031(2) Uani 1 1 d . A .
O4 O 0.1082(5) 0.148(2) 0.1674(6) 0.050(3) Uani 1 1 d . A .


_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 O3 2.384(8) . ?
Pb1 O1 2.420(8) . ?
Pb1 N1 2.551(13) . ?
Pb1 N21 2.563(13) . ?
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
C1 C2 1.3900 . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C3 C6 1.50(2) . ?
C4 C5 1.3900 . ?
C6 C6 1.321(18) 3_665 ?
N21 C21 1.3900 . ?
N21 C25 1.3900 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C23 C26 1.503(11) . ?
C24 C25 1.3900 . ?
C26 C26 1.3295 3_665 ?
N2 C8 1.3900 . ?
N2 C12 1.3900 . ?
C8 C9 1.3900 . ?
C9 C10 1.3900 . ?
C10 C11 1.3900 . ?
C10 C13 1.51(2) . ?
C11 C12 1.3900 . ?
C13 C13 1.322(18) 3_566 ?
N22 C28 1.3900 . ?
N22 C32 1.3900 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C30 C31 1.3900 . ?
C30 C33 1.50(2) . ?
C31 C32 1.3900 . ?
C33 C33 1.323(18) 3_566 ?
C1S O2 1.232(16) . ?
C1S O1 1.253(15) . ?
C2S O4 1.240(15) . ?
C2S O3 1.250(14) . ?

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
O3 Pb1 O1 76.7(3) . . ?
O3 Pb1 N1 78.2(7) . . ?
O1 Pb1 N1 76.6(7) . . ?
O3 Pb1 N21 78.0(7) . . ?
O1 Pb1 N21 79.0(7) . . ?
N1 Pb1 N21 2.5(13) . . ?
C1 N1 C5 120.0 . . ?
C1 N1 Pb1 117.1(12) . . ?
C5 N1 Pb1 122.3(12) . . ?
C2 C1 N1 120.0 . . ?
C3 C2 C1 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 C6 112.1(11) . . ?
C4 C3 C6 127.9(11) . . ?
C3 C4 C5 120.0 . . ?
C4 C5 N1 120.0 . . ?
C6 C6 C3 122(2) 3_665 . ?
C21 N21 C25 120.0 . . ?
C21 N21 Pb1 123.1(12) . . ?
C25 N21 Pb1 116.1(12) . . ?
C22 C21 N21 120.0 . . ?
C21 C22 C23 120.0 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 C26 118.2(9) . . ?
C24 C23 C26 121.7(9) . . ?
C25 C24 C23 120.0 . . ?
C24 C25 N21 120.0 . . ?
C26 C26 C23 124.6(6) 3_665 . ?
C8 N2 C12 120.0 . . ?
C9 C8 N2 120.0 . . ?
C10 C9 C8 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 C13 128.4(10) . . ?
C9 C10 C13 111.6(10) . . ?
C12 C11 C10 120.0 . . ?
C11 C12 N2 120.0 . . ?
C13 C13 C10 122(3) 3_566 . ?
C28 N22 C32 120.0 . . ?
C29 C28 N22 120.0 . . ?
C28 C29 C30 120.0 . . ?
C29 C30 C31 120.0 . . ?
C29 C30 C33 118.4(11) . . ?
C31 C30 C33 121.6(11) . . ?
C30 C31 C32 120.0 . . ?
C31 C32 N22 120.0 . . ?
C33 C33 C30 127(3) 3_566 . ?
O2 C1S O1 125.4(12) . . ?
C1S O1 Pb1 104.2(8) . . ?
O4 C2S O3 125.0(12) . . ?
C2S O3 Pb1 105.0(8) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         5.740
_refine_diff_density_min         -2.459
_refine_diff_density_rms         0.269
