#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/69/2016921.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2016921
loop_
_publ_author_name
'Blake, Alexander J.'
'Caltagirone, Claudia'
'Lippolis, Vito'
'Shamsipur, Mojtaba'
_publ_section_title
;A new polymorph of
 poly[bis(μ₂-perchlorato-κ²O:O')(2,2':6',2''-terpyridine-κ³N,N',N'')lead(II)]
 with a greatly extended chain repeat distance
;
_journal_coeditor_code           FG3072
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m33
_journal_page_last               m36
_journal_paper_doi               10.1107/S0108270108042236
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Pb (Cl O4)2 (C15 H11 N3)]'
_chemical_formula_moiety         'C15 H11 Cl2 N3 O8 Pb'
_chemical_formula_sum            'C15 H11 Cl2 N3 O8 Pb'
_chemical_formula_weight         639.36
_chemical_name_systematic
;
poly[bis(μ₂-perchlorato-κ²O:O')(2,2':6',2''-terpyridine-
κ³N,N',N'')lead(II)]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 98.671(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            20
_cell_length_a                   25.440(4)
_cell_length_b                   16.333(3)
_cell_length_c                   21.916(4)
_cell_measurement_reflns_used    2817
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.5
_cell_volume                     9002(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction
'SAINT (Bruker, 2001), SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
enCIFer (Allen et al.,  2004), PLATON (Spek, 2003),
publCIF (Westrip,
2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_av_sigmaI/netI    0.074
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27358
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.721
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.359
_exptl_crystal_description       column
_exptl_crystal_F_000             6040
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.07
_refine_diff_density_min         -2.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         8832
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ\^2\^(Fo\^2\^)+(0.027P)\^2\^+69.73P] where P=(Fo\^2\^+2Fc\^2\^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.126
_reflns_number_gt                4705
_reflns_number_total             8832
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fg3072.cif
_cod_data_source_block           I
_cod_original_cell_volume        9002(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2016921
_cod_database_fobs_code          2016921
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Pb Pb1 0.29584(2) 0.58101(3) 0.14318(2) 0.02740(10) Uani . . 1.000
Pb Pb2 0.10584(2) 0.41745(3) 0.05993(2) 0.02040(10) Uani . . 1.000
Pb Pb3 0.50000 0.41658(5) 0.25000 0.0265(2) Uani . . 1.000
Cl Cl1 0.36484(14) 0.4067(2) 0.26047(12) 0.0301(10) Uani . . 1.000
Cl Cl2 0.23748(13) 0.4117(3) 0.03496(12) 0.0300(9) Uani . . 1.000
Cl Cl3 0.16410(13) 0.5837(3) 0.16825(11) 0.0300(10) Uani . . 1.000
Cl Cl4 0.43245(12) 0.5844(2) 0.13279(11) 0.0257(9) Uani . . 1.000
Cl Cl5 -0.03225(12) 0.4109(2) 0.06172(11) 0.0243(9) Uani . . 1.000
O O1 0.4021(4) 0.3798(7) 0.2208(4) 0.052(3) Uani . . 1.000
O O2 0.3876(4) 0.4700(7) 0.2983(5) 0.062(4) Uani . . 1.000
O O3 0.3162(4) 0.4330(7) 0.2227(4) 0.041(3) Uani . . 1.000
O O4 0.3533(5) 0.3375(8) 0.2960(5) 0.083(5) Uani . . 1.000
O O5 0.2041(4) 0.3644(6) 0.0685(4) 0.044(3) Uani . . 1.000
O O6 0.2881(4) 0.4250(7) 0.0713(4) 0.044(3) Uani . . 1.000
O O7 0.2113(4) 0.4887(8) 0.0218(5) 0.069(4) Uani . . 1.000
O O8 0.2434(5) 0.3708(10) -0.0191(5) 0.105(5) Uani . . 1.000
O O9 0.1980(4) 0.6303(7) 0.1360(4) 0.047(3) Uani . . 1.000
O O10 0.1597(5) 0.6207(10) 0.2234(5) 0.109(6) Uani . . 1.000
O O11 0.1867(4) 0.5058(8) 0.1775(6) 0.077(4) Uani . . 1.000
O O12 0.1125(4) 0.5753(7) 0.1328(4) 0.040(3) Uani . . 1.000
O O13 0.3941(4) 0.6119(7) 0.1706(4) 0.051(3) Uani . . 1.000
O O14 0.4106(5) 0.5172(8) 0.0973(6) 0.081(5) Uani . . 1.000
O O15 0.4404(5) 0.6522(8) 0.0951(5) 0.085(5) Uani . . 1.000
O O16 0.4804(4) 0.5653(7) 0.1720(4) 0.045(3) Uani . . 1.000
O O17 -0.0441(4) 0.3410(6) 0.0940(4) 0.043(3) Uani . . 1.000
O O18 -0.0116(4) 0.4752(6) 0.1035(4) 0.036(3) Uani . . 1.000
O O19 0.0074(3) 0.3918(6) 0.0233(3) 0.034(2) Uani . . 1.000
O O20 -0.0793(3) 0.4383(6) 0.0218(4) 0.035(3) Uani . . 1.000
N N1 0.3101(4) 0.6465(7) 0.0433(4) 0.026(2) Uani . . 1.000
N N2 0.2996(5) 0.7336(5) 0.1448(5) 0.0292(19) Uani . . 1.000
N N3 0.2904(5) 0.6446(8) 0.2461(4) 0.033(2) Uani . . 1.000
N N4 0.0867(4) 0.3526(7) 0.1596(4) 0.027(2) Uani . . 1.000
N N5 0.1002(4) 0.2645(7) 0.0590(4) 0.023(2) Uani . . 1.000
N N6 0.1118(4) 0.3524(7) -0.0421(4) 0.026(2) Uani . . 1.000
N N7 0.50000 0.2636(9) 0.25000 0.025(3) Uani . . 1.000
N N8 0.4883(4) 0.3527(7) 0.3517(4) 0.025(2) Uani . . 1.000
C C1 0.3186(5) 0.5980(9) -0.0050(5) 0.032(4) Uani . . 1.000
C C2 0.3302(5) 0.6293(9) -0.0584(5) 0.032(4) Uani . . 1.000
C C3 0.3375(6) 0.7111(10) -0.0635(6) 0.040(4) Uani . . 1.000
C C4 0.3317(6) 0.7632(9) -0.0146(6) 0.033(3) Uani . . 1.000
C C5 0.3173(5) 0.7264(9) 0.0384(5) 0.027(3) Uani . . 1.000
C C6 0.3087(5) 0.7767(8) 0.0939(5) 0.026(3) Uani . . 1.000
C C7 0.3099(5) 0.8620(9) 0.0928(6) 0.031(4) Uani . . 1.000
C C8 0.3005(7) 0.9038(7) 0.1461(6) 0.034(3) Uani . . 1.000
C C9 0.2912(6) 0.8619(9) 0.1969(6) 0.037(4) Uani . . 1.000
C C10 0.2904(5) 0.7757(9) 0.1953(5) 0.028(3) Uani . . 1.000
C C11 0.2838(5) 0.7267(9) 0.2503(5) 0.026(3) Uani . . 1.000
C C12 0.2705(5) 0.7600(9) 0.3029(5) 0.030(3) Uani . . 1.000
C C13 0.2632(6) 0.7119(10) 0.3538(6) 0.034(4) Uani . . 1.000
C C14 0.2710(6) 0.6279(9) 0.3477(5) 0.037(4) Uani . . 1.000
C C15 0.2837(5) 0.5989(9) 0.2937(5) 0.031(4) Uani . . 1.000
C C16 0.1166(5) 0.4016(9) -0.0889(4) 0.032(4) Uani . . 1.000
C C17 0.1273(5) 0.3707(9) -0.1456(5) 0.029(3) Uani . . 1.000
C C18 0.1320(5) 0.2886(9) -0.1522(5) 0.031(4) Uani . . 1.000
C C19 0.1270(6) 0.2348(9) -0.1020(5) 0.035(4) Uani . . 1.000
C C20 0.1163(5) 0.2725(8) -0.0471(5) 0.025(3) Uani . . 1.000
C C21 0.1087(5) 0.2215(8) 0.0074(5) 0.023(3) Uani . . 1.000
C C22 0.1090(5) 0.1389(9) 0.0050(5) 0.029(3) Uani . . 1.000
C C23 0.0998(5) 0.0969(10) 0.0579(5) 0.031(4) Uani . . 1.000
C C24 0.0900(6) 0.1373(9) 0.1100(5) 0.030(4) Uani . . 1.000
C C25 0.0909(5) 0.2230(8) 0.1091(5) 0.025(3) Uani . . 1.000
C C26 0.0835(5) 0.2717(8) 0.1648(5) 0.021(3) Uani . . 1.000
C C27 0.0731(6) 0.2342(9) 0.2189(5) 0.033(4) Uani . . 1.000
C C28 0.0666(6) 0.2840(9) 0.2689(5) 0.032(4) Uani . . 1.000
C C29 0.0697(5) 0.3687(9) 0.2634(5) 0.028(3) Uani . . 1.000
C C30 0.0810(5) 0.3989(8) 0.2073(4) 0.025(3) Uani . . 1.000
C C31 0.4813(5) 0.3994(8) 0.3996(5) 0.029(3) Uani . . 1.000
C C32 0.4721(5) 0.3689(9) 0.4554(5) 0.031(4) Uani . . 1.000
C C33 0.4697(6) 0.2843(9) 0.4623(5) 0.032(4) Uani . . 1.000
C C34 0.4757(5) 0.2349(9) 0.4110(5) 0.028(3) Uani . . 1.000
C C35 0.4848(5) 0.2696(8) 0.3568(5) 0.026(3) Uani . . 1.000
C C36 0.4922(5) 0.2216(8) 0.3015(5) 0.027(3) Uani . . 1.000
C C37 0.4911(5) 0.1354(9) 0.3029(6) 0.033(4) Uani . . 1.000
C C38 0.50000 0.0928(13) 0.25000 0.033(5) Uani . . 1.000
H H1 0.31640 0.54020 -0.00090 0.0380 Uiso calc R 1.000
H H2 0.33320 0.59420 -0.09230 0.0380 Uiso calc R 1.000
H H3 0.34660 0.73300 -0.10060 0.0480 Uiso calc R 1.000
H H4 0.33730 0.82050 -0.01700 0.0400 Uiso calc R 1.000
H H7 0.31680 0.89090 0.05720 0.0370 Uiso calc R 1.000
H H8 0.30060 0.96200 0.14670 0.0410 Uiso calc R 1.000
H H9 0.28530 0.89040 0.23310 0.0440 Uiso calc R 1.000
H H12 0.26600 0.81760 0.30510 0.0360 Uiso calc R 1.000
H H13 0.25360 0.73500 0.39030 0.0420 Uiso calc R 1.000
H H14 0.26750 0.59160 0.38080 0.0440 Uiso calc R 1.000
H H15 0.28800 0.54140 0.29000 0.0370 Uiso calc R 1.000
H H16 0.11270 0.45900 -0.08410 0.0380 Uiso calc R 1.000
H H17 0.13120 0.40670 -0.17870 0.0350 Uiso calc R 1.000
H H18 0.13860 0.26670 -0.19050 0.0370 Uiso calc R 1.000
H H19 0.13060 0.17720 -0.10530 0.0430 Uiso calc R 1.000
H H22 0.11510 0.11060 -0.03110 0.0340 Uiso calc R 1.000
H H23 0.10040 0.03870 0.05790 0.0370 Uiso calc R 1.000
H H24 0.08290 0.10820 0.14540 0.0360 Uiso calc R 1.000
H H27 0.07050 0.17630 0.22150 0.0400 Uiso calc R 1.000
H H28 0.06000 0.26020 0.30660 0.0390 Uiso calc R 1.000
H H29 0.06440 0.40430 0.29620 0.0340 Uiso calc R 1.000
H H30 0.08480 0.45640 0.20330 0.0300 Uiso calc R 1.000
H H31 0.48290 0.45710 0.39490 0.0350 Uiso calc R 1.000
H H32 0.46750 0.40450 0.48840 0.0370 Uiso calc R 1.000
H H33 0.46410 0.26060 0.50040 0.0380 Uiso calc R 1.000
H H34 0.47330 0.17700 0.41420 0.0330 Uiso calc R 1.000
H H37 0.48450 0.10690 0.33880 0.0390 Uiso calc R 1.000
H H38 0.50000 0.03460 0.25000 0.0400 Uiso calc . 1.000
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'
Cl Cl 0.1484 0.1585 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Pb1 O6 . . . 66.9(3) ?
O3 Pb1 O9 . . . 111.6(3) ?
O3 Pb1 O13 . . . 86.8(3) ?
O3 Pb1 N1 . . . 145.1(3) ?
O3 Pb1 N2 . . . 143.1(3) ?
O3 Pb1 N3 . . . 80.7(3) ?
O6 Pb1 O9 . . . 104.2(3) ?
O6 Pb1 O13 . . . 106.2(3) ?
O6 Pb1 N1 . . . 84.9(3) ?
O6 Pb1 N2 . . . 149.3(3) ?
O6 Pb1 N3 . . . 145.1(3) ?
O9 Pb1 O13 . . . 148.8(4) yes
O9 Pb1 N1 . . . 94.5(3) ?
O9 Pb1 N2 . . . 74.1(4) ?
O9 Pb1 N3 . . . 75.2(3) ?
O13 Pb1 N1 . . . 81.7(3) ?
O13 Pb1 N2 . . . 76.3(4) ?
O13 Pb1 N3 . . . 83.7(4) ?
N1 Pb1 N2 . . . 65.0(4) ?
N1 Pb1 N3 . . . 130.0(4) ?
N2 Pb1 N3 . . . 65.2(4) ?
O5 Pb2 O12 . . . 105.5(3) ?
O5 Pb2 O19 . . . 148.1(3) yes
O5 Pb2 O20 . . 3_565 115.6(3) ?
O5 Pb2 N4 . . . 96.0(3) ?
O5 Pb2 N5 . . . 74.0(3) ?
O5 Pb2 N6 . . . 74.8(3) ?
O12 Pb2 O19 . . . 106.3(3) ?
O12 Pb2 O20 . . 3_565 68.4(3) ?
O12 Pb2 N4 . . . 84.5(3) ?
O12 Pb2 N5 . . . 148.7(3) ?
O12 Pb2 N6 . . . 145.9(3) ?
O19 Pb2 O20 . . 3_565 79.5(3) ?
O19 Pb2 N4 . . . 84.0(3) ?
O19 Pb2 N5 . . . 77.3(3) ?
O19 Pb2 N6 . . . 80.7(3) ?
O20 Pb2 N4 3_565 . . 142.4(3) ?
O20 Pb2 N5 3_565 . . 141.1(3) ?
O20 Pb2 N6 3_565 . . 80.6(3) ?
N4 Pb2 N5 . . . 64.7(3) ?
N4 Pb2 N6 . . . 129.6(4) ?
N5 Pb2 N6 . . . 65.2(3) ?
O1 Pb3 O16 . . . 88.6(3) ?
O1 Pb3 N7 . . . 76.4(3) ?
O1 Pb3 N8 . . . 83.3(3) ?
O1 Pb3 O1 . . 2_655 152.7(4) yes
O1 Pb3 O16 . . 2_655 114.2(3) ?
O1 Pb3 N8 . . 2_655 85.5(3) ?
O16 Pb3 N7 . . . 144.9(2) ?
O16 Pb3 N8 . . . 144.7(3) ?
O16 Pb3 O16 . . 2_655 70.2(3) ?
O16 Pb3 N8 . . 2_655 82.0(3) ?
N7 Pb3 N8 . . . 65.5(3) ?
N8 Pb3 N8 . . 2_655 131.1(4) ?
O1 Cl1 O2 . . . 109.3(6) no
O1 Cl1 O3 . . . 109.1(5) no
O1 Cl1 O4 . . . 107.1(7) no
O2 Cl1 O3 . . . 111.3(7) no
O2 Cl1 O4 . . . 111.3(7) no
O3 Cl1 O4 . . . 108.6(7) no
O5 Cl2 O6 . . . 110.6(6) no
O5 Cl2 O7 . . . 106.5(6) no
O5 Cl2 O8 . . . 109.1(8) no
O6 Cl2 O7 . . . 109.4(7) no
O6 Cl2 O8 . . . 110.2(7) no
O7 Cl2 O8 . . . 111.0(8) no
O9 Cl3 O10 . . . 109.9(8) no
O9 Cl3 O11 . . . 107.1(7) no
O9 Cl3 O12 . . . 111.1(6) no
O10 Cl3 O11 . . . 111.1(8) no
O10 Cl3 O12 . . . 109.4(7) no
O11 Cl3 O12 . . . 108.4(7) no
O13 Cl4 O14 . . . 108.3(7) no
O13 Cl4 O15 . . . 105.1(7) no
O13 Cl4 O16 . . . 108.4(5) no
O14 Cl4 O15 . . . 111.5(7) no
O14 Cl4 O16 . . . 113.3(7) no
O15 Cl4 O16 . . . 109.9(7) no
O17 Cl5 O18 . . . 111.1(5) no
O17 Cl5 O19 . . . 110.0(6) no
O17 Cl5 O20 . . . 109.7(6) no
O18 Cl5 O19 . . . 108.0(6) no
O18 Cl5 O20 . . . 110.4(6) no
O19 Cl5 O20 . . . 107.6(5) no
Pb3 O1 Cl1 . . . 118.8(5) yes
Pb1 O3 Cl1 . . . 129.4(6) yes
Pb2 O5 Cl2 . . . 114.7(5) yes
Pb1 O6 Cl2 . . . 114.0(6) yes
Pb1 O9 Cl3 . . . 116.9(6) yes
Pb2 O12 Cl3 . . . 110.1(6) yes
Pb1 O13 Cl4 . . . 122.0(5) yes
Pb3 O16 Cl4 . . . 125.7(6) yes
Pb2 O19 Cl5 . . . 121.4(4) yes
Pb2 O20 Cl5 . 3_565 3_565 134.7(5) yes
Pb1 N1 C1 . . . 119.3(9) no
Pb1 N1 C5 . . . 122.0(7) no
C1 N1 C5 . . . 118.0(10) no
Pb1 N2 C6 . . . 120.9(8) no
Pb1 N2 C10 . . . 120.6(8) no
C6 N2 C10 . . . 118.5(10) no
Pb1 N3 C11 . . . 119.7(7) no
Pb1 N3 C15 . . . 120.7(10) no
C11 N3 C15 . . . 118.4(11) no
Pb2 N4 C26 . . . 120.7(7) no
Pb2 N4 C30 . . . 120.1(8) no
C26 N4 C30 . . . 119.2(10) no
Pb2 N5 C21 . . . 120.0(8) no
Pb2 N5 C25 . . . 121.0(8) no
C21 N5 C25 . . . 118.9(11) no
Pb2 N6 C16 . . . 117.4(9) no
Pb2 N6 C20 . . . 120.9(7) no
C16 N6 C20 . . . 121.2(10) no
Pb3 N7 C36 . . . 120.3(8) no
Pb3 N7 C36 . . 2_655 120.3(8) no
C36 N7 C36 . . 2_655 119.5(13) no
Pb3 N8 C31 . . . 120.5(8) no
Pb3 N8 C35 . . . 120.1(7) no
C31 N8 C35 . . . 119.1(10) no
N1 C1 C2 . . . 122.2(13) no
C1 C2 C3 . . . 119.7(12) no
C2 C3 C4 . . . 120.4(13) no
C3 C4 C5 . . . 116.5(13) no
N1 C5 C4 . . . 123.0(12) no
N1 C5 C6 . . . 115.6(10) no
C4 C5 C6 . . . 121.4(13) no
N2 C6 C5 . . . 116.1(11) no
N2 C6 C7 . . . 122.4(11) no
C5 C6 C7 . . . 121.6(11) no
C6 C7 C8 . . . 117.7(12) no
C7 C8 C9 . . . 120.6(12) no
C8 C9 C10 . . . 119.2(12) no
N2 C10 C9 . . . 121.7(11) no
N2 C10 C11 . . . 116.6(12) no
C9 C10 C11 . . . 121.6(11) no
N3 C11 C10 . . . 116.7(10) no
N3 C11 C12 . . . 120.1(12) no
C10 C11 C12 . . . 123.2(13) no
C11 C12 C13 . . . 122.0(14) no
C12 C13 C14 . . . 116.0(12) no
C13 C14 C15 . . . 118.8(12) no
N3 C15 C14 . . . 124.7(14) no
N6 C16 C17 . . . 121.3(13) no
C16 C17 C18 . . . 118.8(12) no
C17 C18 C19 . . . 120.4(11) no
C18 C19 C20 . . . 116.0(13) no
N6 C20 C19 . . . 122.2(11) no
N6 C20 C21 . . . 117.6(10) no
C19 C20 C21 . . . 120.2(12) no
N5 C21 C20 . . . 115.4(11) no
N5 C21 C22 . . . 123.0(11) no
C20 C21 C22 . . . 121.6(10) no
C21 C22 C23 . . . 117.1(12) no
C22 C23 C24 . . . 121.9(14) no
C23 C24 C25 . . . 117.6(12) no
N5 C25 C24 . . . 121.5(11) no
N5 C25 C26 . . . 117.4(11) no
C24 C25 C26 . . . 121.1(10) no
N4 C26 C25 . . . 116.3(10) no
N4 C26 C27 . . . 122.1(11) no
C25 C26 C27 . . . 121.7(12) no
C26 C27 C28 . . . 118.2(13) no
C27 C28 C29 . . . 119.8(11) no
C28 C29 C30 . . . 116.7(11) no
N4 C30 C29 . . . 124.0(12) no
N8 C31 C32 . . . 123.8(12) no
C31 C32 C33 . . . 118.2(11) no
C32 C33 C34 . . . 118.0(11) no
C33 C34 C35 . . . 120.6(13) no
N8 C35 C34 . . . 120.3(11) no
N8 C35 C36 . . . 116.2(10) no
C34 C35 C36 . . . 123.5(12) no
N7 C36 C35 . . . 117.7(12) no
N7 C36 C37 . . . 121.9(11) no
C35 C36 C37 . . . 120.4(11) no
C36 C37 C38 . . . 118.2(13) no
C37 C38 C37 . . 2_655 120.4(17) no
N1 C1 H1 . . . 119.00 no
C2 C1 H1 . . . 119.00 no
C1 C2 H2 . . . 120.00 no
C3 C2 H2 . . . 120.00 no
C2 C3 H3 . . . 120.00 no
C4 C3 H3 . . . 120.00 no
C3 C4 H4 . . . 122.00 no
C5 C4 H4 . . . 122.00 no
C6 C7 H7 . . . 121.00 no
C8 C7 H7 . . . 121.00 no
C7 C8 H8 . . . 120.00 no
C9 C8 H8 . . . 120.00 no
C8 C9 H9 . . . 120.00 no
C10 C9 H9 . . . 120.00 no
C11 C12 H12 . . . 119.00 no
C13 C12 H12 . . . 119.00 no
C12 C13 H13 . . . 122.00 no
C14 C13 H13 . . . 122.00 no
C13 C14 H14 . . . 121.00 no
C15 C14 H14 . . . 121.00 no
N3 C15 H15 . . . 118.00 no
C14 C15 H15 . . . 118.00 no
N6 C16 H16 . . . 119.00 no
C17 C16 H16 . . . 119.00 no
C16 C17 H17 . . . 121.00 no
C18 C17 H17 . . . 121.00 no
C17 C18 H18 . . . 120.00 no
C19 C18 H18 . . . 120.00 no
C18 C19 H19 . . . 122.00 no
C20 C19 H19 . . . 122.00 no
C21 C22 H22 . . . 121.00 no
C23 C22 H22 . . . 121.00 no
C22 C23 H23 . . . 119.00 no
C24 C23 H23 . . . 119.00 no
C23 C24 H24 . . . 121.00 no
C25 C24 H24 . . . 121.00 no
C26 C27 H27 . . . 121.00 no
C28 C27 H27 . . . 121.00 no
C27 C28 H28 . . . 120.00 no
C29 C28 H28 . . . 120.00 no
C28 C29 H29 . . . 122.00 no
C30 C29 H29 . . . 121.00 no
N4 C30 H30 . . . 118.00 no
C29 C30 H30 . . . 118.00 no
N8 C31 H31 . . . 118.00 no
C32 C31 H31 . . . 118.00 no
C31 C32 H32 . . . 121.00 no
C33 C32 H32 . . . 121.00 no
C32 C33 H33 . . . 121.00 no
C34 C33 H33 . . . 121.00 no
C33 C34 H34 . . . 120.00 no
C35 C34 H34 . . . 120.00 no
C36 C37 H37 . . . 121.00 no
C38 C37 H37 . . . 121.00 no
C37 C38 H38 . . . 120.00 no
C37 C38 H38 2_655 . . 120.00 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 O3 . . 2.980(11) yes
Pb1 O6 . . 2.987(11) yes
Pb1 O9 . . 2.598(10) yes
Pb1 O13 . . 2.532(10) yes
Pb1 N1 . . 2.511(9) yes
Pb1 N2 . . 2.494(8) yes
Pb1 N3 . . 2.506(10) yes
Pb2 O5 . . 2.626(10) yes
Pb2 O12 . . 3.024(11) yes
Pb2 O19 . . 2.547(8) yes
Pb2 O20 . 3_565 2.975(9) yes
Pb2 N4 . . 2.540(9) yes
Pb2 N5 . . 2.502(11) yes
Pb2 N6 . . 2.501(9) yes
Pb3 O1 . . 2.548(10) yes
Pb3 O16 . . 2.969(11) yes
Pb3 N7 . . 2.499(15) yes
Pb3 N8 . . 2.519(9) yes
Cl1 O1 . . 1.448(10) no
Cl1 O2 . . 1.395(12) no
Cl1 O3 . . 1.446(10) no
Cl1 O4 . . 1.428(13) no
Cl2 O5 . . 1.431(10) no
Cl2 O6 . . 1.425(10) no
Cl2 O7 . . 1.432(13) no
Cl2 O8 . . 1.388(13) no
Cl3 O9 . . 1.417(11) no
Cl3 O10 . . 1.371(13) no
Cl3 O11 . . 1.398(14) no
Cl3 O12 . . 1.428(10) no
Cl4 O13 . . 1.444(10) no
Cl4 O14 . . 1.410(13) no
Cl4 O15 . . 1.414(13) no
Cl4 O16 . . 1.417(10) no
Cl5 O17 . . 1.400(10) no
Cl5 O18 . . 1.440(10) no
Cl5 O19 . . 1.442(8) no
Cl5 O20 . . 1.443(9) no
N1 C1 . . 1.365(16) no
N1 C5 . . 1.324(19) no
N2 C6 . . 1.368(16) no
N2 C10 . . 1.353(16) no
N3 C11 . . 1.36(2) no
N3 C15 . . 1.315(16) no
N4 C26 . . 1.330(17) no
N4 C30 . . 1.316(14) no
N5 C21 . . 1.376(15) no
N5 C25 . . 1.341(15) no
N6 C16 . . 1.323(15) no
N6 C20 . . 1.316(17) no
N7 C36 . . 1.361(14) no
N7 C36 . 2_655 1.361(14) no
N8 C31 . . 1.331(15) no
N8 C35 . . 1.366(17) no
C1 C2 . . 1.350(17) no
C2 C3 . . 1.36(2) no
C3 C4 . . 1.39(2) no
C4 C5 . . 1.405(18) no
C5 C6 . . 1.511(17) no
C6 C7 . . 1.39(2) no
C7 C8 . . 1.404(19) no
C8 C9 . . 1.358(19) no
C9 C10 . . 1.41(2) no
C10 C11 . . 1.477(17) no
C11 C12 . . 1.363(17) no
C12 C13 . . 1.400(19) no
C13 C14 . . 1.40(2) no
C14 C15 . . 1.358(17) no
C16 C17 . . 1.405(15) no
C17 C18 . . 1.36(2) no
C18 C19 . . 1.429(18) no
C19 C20 . . 1.414(17) no
C20 C21 . . 1.493(17) no
C21 C22 . . 1.35(2) no
C22 C23 . . 1.397(17) no
C23 C24 . . 1.374(18) no
C24 C25 . . 1.40(2) no
C25 C26 . . 1.493(16) no
C26 C27 . . 1.395(17) no
C27 C28 . . 1.394(18) no
C28 C29 . . 1.39(2) no
C29 C30 . . 1.394(15) no
C31 C32 . . 1.373(16) no
C32 C33 . . 1.39(2) no
C33 C34 . . 1.411(18) no
C34 C35 . . 1.367(16) no
C35 C36 . . 1.479(16) no
C36 C37 . . 1.41(2) no
C37 C38 . . 1.400(17) no
C1 H1 . . 0.9500 no
C2 H2 . . 0.9500 no
C3 H3 . . 0.9500 no
C4 H4 . . 0.9500 no
C7 H7 . . 0.9500 no
C8 H8 . . 0.9500 no
C9 H9 . . 0.9500 no
C12 H12 . . 0.9500 no
C13 H13 . . 0.9500 no
C14 H14 . . 0.9500 no
C15 H15 . . 0.9500 no
C16 H16 . . 0.9500 no
C17 H17 . . 0.9500 no
C18 H18 . . 0.9500 no
C19 H19 . . 0.9500 no
C22 H22 . . 0.9500 no
C23 H23 . . 0.9500 no
C24 H24 . . 0.9500 no
C27 H27 . . 0.9500 no
C28 H28 . . 0.9500 no
C29 H29 . . 0.9500 no
C30 H30 . . 0.9500 no
C31 H31 . . 0.9500 no
C32 H32 . . 0.9500 no
C33 H33 . . 0.9500 no
C34 H34 . . 0.9500 no
C37 H37 . . 0.9500 no
C38 H38 . . 0.9500 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C3 H3 O4 4_564 0.95 2.57 3.263(17) 130 no
C3 H3 O9 7_565 0.95 2.57 3.101(19) 116 no
C13 H13 O5 6_555 0.95 2.48 3.061(18) 120 no
C14 H14 O8 4_565 0.95 2.44 3.104(16) 126 no
C15 H15 O3 . 0.95 2.48 3.292(17) 144 no
C16 H16 O20 3_565 0.95 2.40 3.213(16) 144 no
C17 H17 O10 4_564 0.95 2.41 3.107(16) 130 no
C22 H22 O14 7_555 0.95 2.57 3.382(19) 144 no
C31 H31 O16 2_655 0.95 2.56 3.349(17) 141 no
C37 H37 O18 6_545 0.95 2.54 3.317(17) 139 no
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C5 N1 C1 C2 . . . . -4.8(18) no
C1 N1 C5 C4 . . . . 1.9(19) no
C1 N1 C5 C6 . . . . -178.5(11) no
C10 N2 C6 C5 . . . . -178.5(11) no
C10 N2 C6 C7 . . . . 1.4(19) no
C6 N2 C10 C9 . . . . -1(2) no
C6 N2 C10 C11 . . . . -176.7(12) no
C15 N3 C11 C10 . . . . -178.6(12) no
C15 N3 C11 C12 . . . . -0.1(19) no
C11 N3 C15 C14 . . . . -1(2) no
C30 N4 C26 C25 . . . . -179.4(11) no
C30 N4 C26 C27 . . . . 1.5(19) no
C26 N4 C30 C29 . . . . -2.5(19) no
C25 N5 C21 C20 . . . . 177.4(11) no
C25 N5 C21 C22 . . . . -1.1(18) no
C21 N5 C25 C24 . . . . 0.4(18) no
C21 N5 C25 C26 . . . . 178.2(11) no
C20 N6 C16 C17 . . . . -0.7(19) no
C16 N6 C20 C19 . . . . 0.7(19) no
C16 N6 C20 C21 . . . . -178.2(11) no
C36 N7 C36 C35 2_655 . . . 179.0(10) no
C36 N7 C36 C37 2_655 . . . -1.0(15) no
C35 N8 C31 C32 . . . . 1.9(19) no
C31 N8 C35 C34 . . . . -1.8(18) no
C31 N8 C35 C36 . . . . 179.1(11) no
N1 C1 C2 C3 . . . . 5(2) no
C1 C2 C3 C4 . . . . -2(2) no
C2 C3 C4 C5 . . . . -1(2) no
C3 C4 C5 N1 . . . . 1(2) no
C3 C4 C5 C6 . . . . -178.7(12) no
N1 C5 C6 N2 . . . . 6.1(17) no
N1 C5 C6 C7 . . . . -173.7(12) no
C4 C5 C6 N2 . . . . -174.2(13) no
C4 C5 C6 C7 . . . . 6.0(19) no
N2 C6 C7 C8 . . . . -1(2) no
C5 C6 C7 C8 . . . . 178.8(13) no
C6 C7 C8 C9 . . . . 1(2) no
C7 C8 C9 C10 . . . . -1(2) no
C8 C9 C10 N2 . . . . 1(2) no
C8 C9 C10 C11 . . . . 176.2(14) no
N2 C10 C11 N3 . . . . 3.4(18) no
N2 C10 C11 C12 . . . . -175.0(12) no
C9 C10 C11 N3 . . . . -171.8(13) no
C9 C10 C11 C12 . . . . 10(2) no
N3 C11 C12 C13 . . . . 0(2) no
C10 C11 C12 C13 . . . . 178.4(13) no
C11 C12 C13 C14 . . . . 1(2) no
C12 C13 C14 C15 . . . . -1(2) no
C13 C14 C15 N3 . . . . 1(2) no
N6 C16 C17 C18 . . . . 0.9(19) no
C16 C17 C18 C19 . . . . -1.0(19) no
C17 C18 C19 C20 . . . . 1(2) no
C18 C19 C20 N6 . . . . -1(2) no
C18 C19 C20 C21 . . . . 178.1(12) no
N6 C20 C21 N5 . . . . -3.1(17) no
N6 C20 C21 C22 . . . . 175.4(12) no
C19 C20 C21 N5 . . . . 178.0(12) no
C19 C20 C21 C22 . . . . -3.5(19) no
N5 C21 C22 C23 . . . . 0.4(19) no
C20 C21 C22 C23 . . . . -178.0(12) no
C21 C22 C23 C24 . . . . 1.0(19) no
C22 C23 C24 C25 . . . . -2(2) no
C23 C24 C25 N5 . . . . 1(2) no
C23 C24 C25 C26 . . . . -176.8(12) no
N5 C25 C26 N4 . . . . 0.2(17) no
N5 C25 C26 C27 . . . . 179.3(12) no
C24 C25 C26 N4 . . . . 178.0(12) no
C24 C25 C26 C27 . . . . -3(2) no
N4 C26 C27 C28 . . . . -1(2) no
C25 C26 C27 C28 . . . . -179.9(13) no
C26 C27 C28 C29 . . . . 1(2) no
C27 C28 C29 C30 . . . . -2(2) no
C28 C29 C30 N4 . . . . 2.7(19) no
N8 C31 C32 C33 . . . . 0(2) no
C31 C32 C33 C34 . . . . -1(2) no
C32 C33 C34 C35 . . . . 2(2) no
C33 C34 C35 N8 . . . . 0.1(19) no
C33 C34 C35 C36 . . . . 179.1(12) no
N8 C35 C36 N7 . . . . -2.2(16) no
N8 C35 C36 C37 . . . . 177.8(11) no
C34 C35 C36 N7 . . . . 178.8(11) no
C34 C35 C36 C37 . . . . -1.2(19) no
N7 C36 C37 C38 . . . . 2.0(17) no
C35 C36 C37 C38 . . . . -178.0(10) no
C36 C37 C38 C37 . . . 2_655 -1.0(15) no
