#------------------------------------------------------------------------------ #$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/31/8103140.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_8103140 loop_ _publ_author_name 'Ji-Ku Wang' 'Hao Chen' 'Hong-Bin Xu' _publ_section_title ; Crystal structure of dipyrido[7,6-a:6',7'-c]-3-chloro-pyrido[2,3-b]-quinoxaline)-(naphthalene-1,4- dicarboxylato)lead(II), Pb(C17H8N4Cl)(C12H6O4) ; _journal_issue 3 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 361 _journal_volume 226 _journal_year 2011 _chemical_formula_moiety 'C29 H12 Cl N4 O4 Pb' _chemical_formula_sum 'C29 H12 Cl N4 O4 Pb' _chemical_formula_weight 737.08 _chemical_name_systematic ; [[dipyrido[7,6 -a:6',7'-c]-3-chloropyrido[2,3-b]quinoxaline)lead(II)]- naphthalene-1,4-dicarboxylato], [Pb(C~17~H~8~N~4~Cl)~2~(C~12~H~6~O~4~)] ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 80.808(5) _cell_angle_beta 81.973(5) _cell_angle_gamma 79.638(5) _cell_formula_units_Z 2 _cell_length_a 10.310(5) _cell_length_b 10.521(5) _cell_length_c 12.168(5) _cell_measurement_reflns_used 4456 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.08 _cell_measurement_theta_min 1.71 _cell_volume 1273.3(10) _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material 'SHELXTL (Bruker, 1998)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 6666 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.08 _diffrn_reflns_theta_min 1.71 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.777 _exptl_absorpt_correction_T_max 0.79 _exptl_absorpt_correction_T_min 0.52 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _refine_diff_density_max 1.395 _refine_diff_density_min -1.382 _refine_diff_density_rms 0.171 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 385 _refine_ls_number_reflns 4456 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0511 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+1.4783P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1311 _refine_ls_wR_factor_ref 0.1382 _reflns_number_gt 3850 _reflns_number_total 4456 _reflns_threshold_expression I>2\s(I) _cod_data_source_file 1267-3386.cff _cod_data_source_block 1 _cod_original_sg_symbol_Hall '- P1' _cod_database_code 8103140 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 C1 C 0.4456(10) 0.2012(10) -0.0108(9) 0.064(2) Uani 1 1 d . H1 H 0.4369 0.1788 0.0667 0.076 Uiso 1 1 calc R C2 C 0.3361(10) 0.2716(11) -0.0588(10) 0.070(3) Uani 1 1 d . H2 H 0.2571 0.2967 -0.0148 0.084 Uiso 1 1 calc R C3 C 0.3472(11) 0.3034(10) -0.1731(9) 0.067(3) Uani 1 1 d . H3 H 0.2754 0.3507 -0.2082 0.081 Uiso 1 1 calc R C4 C 0.4673(12) 0.2640(10) -0.2362(9) 0.064(3) Uani 1 1 d . C5 C 0.5742(9) 0.1939(9) -0.1805(8) 0.054(2) Uani 1 1 d . C6 C 0.6970(11) 0.1542(12) -0.2434(9) 0.071(3) Uani 1 1 d . C7 C 0.9127(15) 0.045(2) -0.2412(14) 0.123(6) Uani 1 1 d . H7 H 0.9847 0.0053 -0.2029 0.148 Uiso 1 1 calc R C8 C 0.9286(19) 0.063(3) -0.3585(14) 0.166(10) Uani 1 1 d . H8 H 1.0046 0.0208 -0.3967 0.199 Uiso 1 1 calc R C9 C 0.8359(15) 0.140(2) -0.4171(13) 0.118(6) Uani 1 1 d . H9 H 0.8537 0.1665 -0.4937 0.141 Uiso 1 1 calc R C10 C 0.7143(13) 0.1800(13) -0.3605(10) 0.081(3) Uani 1 1 d . C11 C 0.6029(14) 0.2551(11) -0.4170(9) 0.075(3) Uani 1 1 d . C12 C 0.4815(12) 0.2962(10) -0.3573(9) 0.066(3) Uani 1 1 d . C13 C 0.3933(16) 0.3872(13) -0.5174(11) 0.087(4) Uani 1 1 d . C14 C 0.5098(14) 0.3532(11) -0.5781(10) 0.074(3) Uani 1 1 d . C15 C 0.5274(19) 0.3807(12) -0.7020(12) 0.104(5) Uani 1 1 d . H15 H 0.6070 0.3570 -0.7457 0.125 Uiso 1 1 calc R C16 C 0.299(2) 0.4796(18) -0.6740(16) 0.130(6) Uani 1 1 d . H16 H 0.2259 0.5258 -0.7085 0.156 Uiso 1 1 calc R C17 C 0.6393(9) 0.0269(10) 0.2729(8) 0.055(2) Uani 1 1 d . C18 C 0.5658(12) 0.0121(10) 0.3909(8) 0.064(3) Uani 1 1 d . C20 C 0.9004(10) 0.2545(9) 0.0216(10) 0.064(3) Uani 1 1 d . C21 C 0.9527(9) 0.3819(10) 0.0083(11) 0.065(3) Uani 1 1 d . C22 C 1.0025(10) 0.4393(10) -0.0996(12) 0.073(3) Uani 1 1 d . C23 C 1.0524(10) 0.5587(10) -0.1062(12) 0.075(3) Uani 1 1 d . C24 C 1.1010(18) 0.6161(17) -0.2269(16) 0.053(4) Uani 0.50 1 d P H24 H 1.1326 0.6950 -0.2363 0.064 Uiso 0.50 1 calc PR C25 C 1.101(2) 0.555(2) -0.330(2) 0.088(8) Uani 0.50 1 d P H25 H 1.1339 0.5951 -0.3994 0.105 Uiso 0.50 1 calc PR C26 C 1.057(2) 0.447(3) -0.324(2) 0.079(7) Uani 0.50 1 d P H26 H 1.0581 0.4092 -0.3882 0.095 Uiso 0.50 1 calc PR C27 C 0.4170(19) 0.4429(13) -0.7442(11) 0.091(4) Uani 1 1 d . C28 C 1.003(2) 0.382(2) -0.211(2) 0.068(6) Uani 0.50 1 d P H28 H 0.9689 0.3052 -0.2077 0.081 Uiso 0.50 1 calc PR C19 C 0.4272(8) 0.0668(8) 0.4083(6) 0.067(3) Uani 1 1 d G C29 C 0.3649(9) 0.0611(9) 0.5175(6) 0.068(3) Uani 1 1 d G C30 C 0.2345(9) 0.1223(14) 0.5384(8) 0.080(7) Uani 0.50 1 d PG H30 H 0.1927 0.1185 0.6115 0.096 Uiso 0.50 1 calc PR C31 C 0.1664(9) 0.1892(17) 0.4502(12) 0.089(8) Uani 0.50 1 d PG H31 H 0.0792 0.2302 0.4642 0.106 Uiso 0.50 1 calc PR C32 C 0.2288(12) 0.1950(17) 0.3410(10) 0.115(11) Uani 0.50 1 d PG H32 H 0.1833 0.2397 0.2819 0.139 Uiso 0.50 1 calc PR C33 C 0.3592(12) 0.1338(14) 0.3200(6) 0.083(7) Uani 0.50 1 d PG H33 H 0.4009 0.1376 0.2470 0.099 Uiso 0.50 1 calc PR N1 N 0.5634(7) 0.1630(7) -0.0676(6) 0.0536(18) Uani 1 1 d . N2 N 0.7984(10) 0.0821(12) -0.1843(8) 0.086(3) Uani 1 1 d . N3 N 0.6203(13) 0.2842(11) -0.5325(9) 0.092(3) Uani 1 1 d . N4 N 0.3801(12) 0.3605(10) -0.4073(9) 0.091(3) Uani 1 1 d . N6 N 0.2836(17) 0.4539(14) -0.5657(12) 0.131(5) Uani 1 1 d . O1 O 0.7784(7) 0.2542(7) 0.0471(7) 0.073(2) Uani 1 1 d . O2 O 0.9787(8) 0.1549(7) 0.0017(9) 0.094(3) Uani 1 1 d . O3 O 0.7609(11) 0.0195(10) 0.2604(9) 0.100(3) Uani 1 1 d U O4 O 0.5772(7) 0.0533(8) 0.1913(6) 0.074(2) Uani 1 1 d . Cl1 Cl 0.3995(7) 0.4896(4) -0.8800(4) 0.154(2) Uani 1 1 d . Pb1 Pb 0.76337(3) 0.03798(3) 0.03963(3) 0.05062(16) Uani 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.051(6) 0.070(7) 0.065(6) -0.005(5) -0.001(5) -0.007(5) C2 0.044(6) 0.078(7) 0.087(8) -0.014(6) -0.004(5) -0.004(5) C3 0.060(6) 0.067(7) 0.076(7) -0.013(5) -0.020(5) -0.001(5) C4 0.082(7) 0.048(5) 0.068(6) -0.006(4) -0.025(5) -0.014(5) C5 0.051(5) 0.056(5) 0.058(5) -0.009(4) -0.006(4) -0.012(4) C6 0.063(7) 0.090(8) 0.061(6) -0.002(5) -0.015(5) -0.016(6) C7 0.068(9) 0.194(19) 0.089(10) -0.014(11) 0.008(7) 0.009(10) C8 0.101(13) 0.27(3) 0.079(11) 0.002(13) 0.017(9) 0.042(16) C9 0.076(9) 0.178(17) 0.079(9) 0.005(10) -0.009(7) 0.013(10) C10 0.082(8) 0.094(9) 0.067(7) -0.008(6) 0.005(6) -0.024(7) C11 0.109(10) 0.062(6) 0.056(6) 0.010(5) -0.028(6) -0.023(6) C12 0.076(7) 0.058(6) 0.068(6) -0.011(5) -0.021(6) -0.008(5) C13 0.111(11) 0.075(8) 0.083(9) -0.009(6) -0.042(8) -0.012(8) C14 0.098(9) 0.063(7) 0.070(7) 0.008(5) -0.042(7) -0.024(6) C15 0.164(15) 0.063(8) 0.097(10) -0.004(7) -0.035(10) -0.042(9) C16 0.162(18) 0.123(14) 0.107(13) -0.015(10) -0.065(13) 0.007(13) C17 0.038(5) 0.061(6) 0.062(6) 0.003(4) 0.001(4) -0.013(4) C18 0.083(7) 0.055(6) 0.051(5) -0.006(4) 0.017(5) -0.022(5) C20 0.055(6) 0.043(5) 0.091(8) 0.000(5) -0.010(5) -0.011(5) C21 0.033(5) 0.049(5) 0.108(9) -0.002(5) 0.001(5) -0.008(4) C22 0.036(5) 0.051(6) 0.130(10) -0.007(6) -0.005(6) -0.008(4) C23 0.039(5) 0.047(6) 0.129(10) 0.000(6) -0.005(6) 0.002(4) C24 0.039(9) 0.040(9) 0.071(12) 0.010(8) 0.000(8) -0.002(7) C25 0.066(15) 0.058(14) 0.11(2) 0.023(13) 0.020(13) 0.014(12) C26 0.050(12) 0.081(17) 0.11(2) -0.037(15) -0.020(12) 0.001(12) C27 0.145(14) 0.073(8) 0.063(7) -0.008(6) -0.047(8) -0.014(9) C28 0.042(11) 0.057(12) 0.102(17) -0.001(11) -0.019(11) -0.004(9) C19 0.073(7) 0.064(6) 0.062(6) -0.003(5) 0.005(5) -0.019(5) C29 0.076(7) 0.067(7) 0.057(6) -0.006(5) 0.019(5) -0.025(6) C30 0.066(15) 0.12(2) 0.054(12) -0.001(12) 0.010(10) -0.031(14) C31 0.044(12) 0.13(2) 0.082(16) 0.008(14) 0.025(11) -0.018(13) C32 0.11(2) 0.15(3) 0.059(15) 0.027(16) 0.002(15) -0.02(2) C33 0.081(17) 0.11(2) 0.047(12) -0.002(11) 0.014(11) -0.015(14) N1 0.051(4) 0.052(4) 0.057(5) -0.002(3) -0.008(3) -0.009(4) N2 0.062(6) 0.127(9) 0.064(6) -0.016(6) -0.003(5) -0.003(6) N3 0.120(9) 0.083(7) 0.077(7) -0.011(5) -0.005(6) -0.033(7) N4 0.124(9) 0.069(6) 0.091(7) -0.010(5) -0.060(7) -0.007(6) N6 0.153(12) 0.140(12) 0.097(9) -0.021(8) -0.071(9) 0.030(10) O1 0.049(4) 0.058(4) 0.109(6) -0.005(4) 0.007(4) -0.018(3) O2 0.054(4) 0.052(4) 0.171(9) -0.015(5) -0.002(5) -0.008(4) O3 0.099(3) 0.101(3) 0.099(3) -0.0135(11) -0.0110(11) -0.0160(11) O4 0.056(4) 0.096(6) 0.061(4) 0.006(4) -0.005(3) -0.004(4) Cl1 0.271(7) 0.107(3) 0.110(3) 0.017(2) -0.113(4) -0.055(4) Pb1 0.0457(2) 0.0493(2) 0.0546(2) -0.00106(14) -0.00019(15) -0.01150(15) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 N1 C1 C2 124.8(10) . . N1 C1 H1 117.6 . . C2 C1 H1 117.6 . . C3 C2 C1 118.1(10) . . C3 C2 H2 120.9 . . C1 C2 H2 120.9 . . C2 C3 C4 119.3(10) . . C2 C3 H3 120.4 . . C4 C3 H3 120.4 . . C3 C4 C5 118.9(10) . . C3 C4 C12 120.3(10) . . C5 C4 C12 120.7(10) . . N1 C5 C4 121.8(9) . . N1 C5 C6 118.7(9) . . C4 C5 C6 119.6(9) . . N2 C6 C10 121.1(11) . . N2 C6 C5 117.1(10) . . C10 C6 C5 121.7(10) . . N2 C7 C8 121.3(15) . . N2 C7 H7 119.3 . . C8 C7 H7 119.3 . . C9 C8 C7 121.2(16) . . C9 C8 H8 119.4 . . C7 C8 H8 119.4 . . C8 C9 C10 118.0(15) . . C8 C9 H9 121.0 . . C10 C9 H9 121.0 . . C9 C10 C6 119.3(13) . . C9 C10 C11 122.6(12) . . C6 C10 C11 118.0(11) . . N3 C11 C12 120.1(11) . . N3 C11 C10 118.4(12) . . C12 C11 C10 121.5(10) . . N4 C12 C11 122.0(11) . . N4 C12 C4 119.6(11) . . C11 C12 C4 118.5(10) . . N4 C13 C14 121.0(12) . . N4 C13 N6 116.8(15) . . C14 C13 N6 122.2(14) . . C13 C14 N3 123.6(12) . . C13 C14 C15 122.3(12) . . N3 C14 C15 114.1(14) . . C27 C15 C14 112.8(16) . . C27 C15 H15 123.6 . . C14 C15 H15 123.6 . . N6 C16 C27 125.2(16) . . N6 C16 H16 117.4 . . C27 C16 H16 117.4 . . O4 C17 O3 120.1(10) . . O4 C17 C18 120.1(9) . . O3 C17 C18 119.7(10) . . C19 C18 C29 121.2(8) . 2_656 C19 C18 C17 119.4(9) . . C29 C18 C17 119.4(10) 2_656 . O2 C20 O1 122.2(9) . . O2 C20 C21 118.7(9) . . O1 C20 C21 119.0(9) . . O2 C20 Pb1 69.2(5) . . O1 C20 Pb1 53.0(5) . . C21 C20 Pb1 171.2(7) . . C22 C21 C23 122.4(9) . 2_765 C22 C21 C20 120.0(10) . . C23 C21 C20 117.6(10) 2_765 . C21 C22 C23 117.2(11) . . C21 C22 C28 124.4(12) . . C23 C22 C28 118.3(14) . . C21 C23 C22 120.3(12) 2_765 . C21 C23 C24 125.8(11) 2_765 . C22 C23 C24 113.7(13) . . C25 C24 C23 125.2(16) . . C25 C24 H24 117.4 . . C23 C24 H24 117.4 . . C26 C25 C24 121(2) . . C26 C25 H25 119.5 . . C24 C25 H25 119.5 . . C25 C26 C28 119(2) . . C25 C26 H26 120.3 . . C28 C26 H26 120.3 . . C15 C27 C16 121.6(14) . . C15 C27 Cl1 126.2(15) . . C16 C27 Cl1 112.2(12) . . C26 C28 C22 122.4(18) . . C26 C28 H28 118.8 . . C22 C28 H28 118.8 . . C29 C19 C33 120.0 . . C29 C19 C18 118.3(7) . . C33 C19 C18 121.5(7) . . C19 C29 C30 120.0 . . C19 C29 C18 120.0(7) . 2_656 C30 C29 C18 119.9(7) . 2_656 C31 C30 C29 120.0 . . C31 C30 H30 120.0 . . C29 C30 H30 120.0 . . C32 C31 C30 120.0 . . C32 C31 H31 120.0 . . C30 C31 H31 120.0 . . C33 C32 C31 120.0 . . C33 C32 H32 120.0 . . C31 C32 H32 120.0 . . C32 C33 C19 120.0 . . C32 C33 H33 120.0 . . C19 C33 H33 120.0 . . C1 N1 C5 117.1(8) . . C1 N1 Pb1 120.3(7) . . C5 N1 Pb1 122.6(6) . . C7 N2 C6 117.9(12) . . C7 N2 Pb1 121.7(10) . . C6 N2 Pb1 120.3(7) . . C14 N3 C11 114.2(12) . . C12 N4 C13 119.1(13) . . C16 N6 C13 115.9(18) . . C20 O1 Pb1 101.5(6) . . C20 O2 Pb1 85.2(6) . . C17 O3 Pb1 90.5(7) . . C17 O4 Pb1 99.8(6) . . O1 Pb1 O4 88.5(3) . . O1 Pb1 N1 78.3(2) . . O4 Pb1 N1 77.4(2) . . O1 Pb1 O3 82.4(3) . . O4 Pb1 O3 48.8(3) . . N1 Pb1 O3 123.0(3) . . O1 Pb1 N2 90.1(3) . . O4 Pb1 N2 137.9(3) . . N1 Pb1 N2 61.2(3) . . O3 Pb1 N2 170.1(3) . . O1 Pb1 O2 51.1(2) . . O4 Pb1 O2 129.7(3) . . N1 Pb1 O2 114.4(3) . . O3 Pb1 O2 92.0(3) . . N2 Pb1 O2 78.3(3) . . O1 Pb1 C20 25.5(3) . . O4 Pb1 C20 109.9(3) . . N1 Pb1 C20 96.5(3) . . O3 Pb1 C20 87.1(3) . . N2 Pb1 C20 83.4(3) . . O2 Pb1 C20 25.6(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 N1 1.339(12) . C1 C2 1.382(15) . C1 H1 0.9300 . C2 C3 1.371(16) . C2 H2 0.9300 . C3 C4 1.395(15) . C3 H3 0.9300 . C4 C5 1.405(14) . C4 C12 1.451(15) . C5 N1 1.354(12) . C5 C6 1.416(14) . C6 N2 1.391(15) . C6 C10 1.399(16) . C7 N2 1.310(17) . C7 C8 1.40(2) . C7 H7 0.9300 . C8 C9 1.35(2) . C8 H8 0.9300 . C9 C10 1.372(19) . C9 H9 0.9300 . C10 C11 1.461(17) . C11 N3 1.383(15) . C11 C12 1.390(17) . C12 N4 1.308(14) . C13 N4 1.317(17) . C13 C14 1.341(19) . C13 N6 1.374(17) . C14 N3 1.372(16) . C14 C15 1.481(18) . C15 C27 1.33(2) . C15 H15 0.9300 . C16 N6 1.30(2) . C16 C27 1.42(3) . C16 H16 0.9300 . C17 O4 1.224(12) . C17 O3 1.231(13) . C17 C18 1.525(13) . C18 C19 1.441(14) . C18 C29 1.449(18) 2_656 C20 O2 1.237(12) . C20 O1 1.253(12) . C20 C21 1.511(13) . C20 Pb1 2.854(10) . C21 C22 1.422(17) . C21 C23 1.421(17) 2_765 C22 C23 1.428(14) . C22 C28 1.57(3) . C23 C21 1.421(17) 2_765 C23 C24 1.55(2) . C24 C25 1.50(3) . C24 H24 0.9300 . C25 C26 1.28(3) . C25 H25 0.9300 . C26 C28 1.51(4) . C26 H26 0.9300 . C27 Cl1 1.672(13) . C28 H28 0.9300 . C19 C29 1.3900 . C19 C33 1.3900 . C29 C30 1.3900 . C29 C18 1.449(14) 2_656 C30 C31 1.3900 . C30 H30 0.9300 . C31 C32 1.3900 . C31 H31 0.9300 . C32 C33 1.3900 . C32 H32 0.9300 . C33 H33 0.9300 . N1 Pb1 2.629(7) . N2 Pb1 2.674(10) . O1 Pb1 2.325(7) . O2 Pb1 2.678(8) . O3 Pb1 2.659(10) . O4 Pb1 2.472(7) .