#------------------------------------------------------------------------------ #$Date: 2017-04-21 05:23:32 +0300 (Fri, 21 Apr 2017) $ #$Revision: 195646 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042740.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_7042740 loop_ _publ_author_name 'Liberato, Andrea' 'Aguinaco, Almudena' 'Clares, Maria Paz' 'Delgado-Pinar, Estefania' 'Blasco, Salvador' 'Pitarch-Jarque, Javier' 'Basallote, Manuel G.' 'Garc\'ia-Espa\~na, Enrique' 'Verdejo, Bego\~na' _publ_section_title ; Pb2+ Complexes of Small-Cavity Azamacrocyclic Ligands. Thermodynamic and Kinetic Studies ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT00680B _journal_year 2017 _chemical_formula_moiety 'C11 H18 N4 Pb, 2(Cl O4)' _chemical_formula_sum 'C11 H18 Cl2 N4 O8 Pb' _chemical_formula_weight 612.38 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2016-12-14 _audit_creation_method ; Olex2 1.2 (compiled Nov 22 2016 12:06:14 for OlexSys, GUI svn.r5269) ; _audit_update_record ; 2017-01-24 deposited with the CCDC. 2017-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.1503(13) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.8925(3) _cell_length_b 15.1543(5) _cell_length_c 13.5209(5) _cell_measurement_reflns_used 4043 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 0.998 _cell_volume 1787.68(11) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SIR2011 (Burla et al., 2007)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.0476636 _diffrn_orient_matrix_UB_12 0.0023027 _diffrn_orient_matrix_UB_13 0.0732740 _diffrn_orient_matrix_UB_21 -0.1035306 _diffrn_orient_matrix_UB_22 -0.0066205 _diffrn_orient_matrix_UB_23 0.0176872 _diffrn_orient_matrix_UB_31 0.0121190 _diffrn_orient_matrix_UB_32 -0.0656145 _diffrn_orient_matrix_UB_33 0.0007869 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_unetI/netI 0.0747 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 7721 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.507 _diffrn_reflns_theta_min 3.071 _exptl_absorpt_coefficient_mu 9.785 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.275 _exptl_crystal_description prism _exptl_crystal_F_000 1168 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.722 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.164 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 235 _refine_ls_number_reflns 4065 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.891 _refine_ls_R_factor_all 0.1083 _refine_ls_R_factor_gt 0.0460 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1238 _refine_ls_wR_factor_ref 0.1630 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2212 _reflns_number_total 4065 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt00680b2.cif _cod_data_source_block import _cod_database_code 7042740 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups 2.a Ternary CH refined with riding coordinates: N2(H2), N3(H3), N4(H4) 2.b Secondary CH2 refined with riding coordinates: C6(H6A,H6B), C11(H11A,H11B), C8(H8A,H8B), C10(H10A,H10B), C7(H7A,H7B), C9(H9A, H9B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2A), C3(H3A), C4(H4A) ; _shelx_res_file ; import.res created by SHELXL-2014/7 TITL import REM Shelx file produced by Sir2014 on Wed Dec 14 2016 at 09:47:17 REM Structure name: import CELL 0.71073 8.8925 15.1543 13.5209 90 101.1503 90 ZERR 4 0.0003 0.0005 0.0005 0 0.0013 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O Pb UNIT 44 72 8 16 32 4 L.S. 20 PLAN 10 fmap 2 ACTA OMIT -1 2 1 OMIT 1 2 0 OMIT -1 0 2 OMIT 0 2 0 OMIT 1 1 2 OMIT -1 1 1 OMIT 0 1 1 OMIT 1 0 0 OMIT 1 0 2 OMIT 1 1 1 OMIT 0 1 2 OMIT 1 1 0 REM REM REM WGHT 0.100000 FVAR 0.08987 PB1 6 0.701121 0.497348 0.107360 11.00000 0.05661 0.04940 = 0.03731 0.00739 0.00664 -0.00123 CL1 3 0.354917 0.605929 0.174492 11.00000 0.06667 0.06510 = 0.05702 -0.00106 0.01992 0.00123 CL2 3 0.151574 0.239682 0.448128 11.00000 0.06384 0.06086 = 0.06024 0.00028 0.01452 0.00777 N1 4 0.676981 0.457313 0.275313 11.00000 0.05775 0.04359 = 0.04171 0.00695 0.01710 0.01087 C1 1 0.753850 0.505634 0.349740 11.00000 0.09980 0.06440 = 0.03213 -0.00515 0.01733 0.01109 C6 1 0.495667 0.345619 0.200742 11.00000 0.05389 0.06664 = 0.11586 0.02807 0.00500 -0.00370 AFIX 23 H6A 2 0.489171 0.284045 0.219059 11.00000 -1.20000 H6B 2 0.391890 0.368238 0.183092 11.00000 -1.20000 AFIX 0 N2 4 0.566877 0.350980 0.111577 11.00000 0.06315 0.06936 = 0.05346 0.00295 -0.00056 -0.01225 AFIX 13 H2 2 0.485139 0.347456 0.051624 11.00000 -1.20000 AFIX 0 N3 4 0.891240 0.382132 0.117271 11.00000 0.06185 0.09023 = 0.04285 -0.00650 0.01860 0.00790 AFIX 13 H3 2 0.902575 0.368342 0.048279 11.00000 -1.20000 AFIX 0 N4 4 0.928891 0.536909 0.239718 11.00000 0.06728 0.06581 = 0.06058 0.00852 0.00728 -0.02809 AFIX 13 H4 2 0.986633 0.584218 0.214603 11.00000 -1.20000 AFIX 0 C2 1 0.732248 0.493407 0.448179 11.00000 0.17128 0.07833 = 0.04028 -0.00247 0.04263 0.04107 AFIX 43 H2A 2 0.786851 0.526858 0.500774 11.00000 -1.20000 AFIX 0 O6 5 0.155259 0.245023 0.345955 11.00000 0.15569 0.15570 = 0.06769 0.02052 0.02567 0.03686 O8 5 0.030101 0.290581 0.472132 11.00000 0.09270 0.08581 = 0.13753 -0.03679 0.02955 0.02591 O2 5 0.358076 0.578312 0.274073 11.00000 0.23031 0.12436 = 0.05802 -0.00690 0.05845 -0.01697 C11 1 0.864192 0.570163 0.326557 11.00000 0.10423 0.05922 = 0.04826 -0.00632 -0.00254 -0.00829 AFIX 23 H11A 2 0.945751 0.578557 0.384769 11.00000 -1.20000 H11B 2 0.813906 0.626465 0.309589 11.00000 -1.20000 AFIX 0 O7 5 0.121557 0.151229 0.471095 11.00000 0.24891 0.07180 = 0.18807 -0.00072 0.13550 0.02739 C3 1 0.626144 0.429423 0.466443 11.00000 0.16203 0.09780 = 0.07599 0.03948 0.08217 0.06549 AFIX 43 H3A 2 0.607882 0.420909 0.531211 11.00000 -1.20000 AFIX 0 C8 1 0.834825 0.301700 0.159938 11.00000 0.09173 0.05893 = 0.06659 0.01255 0.02488 0.02018 AFIX 23 H8A 2 0.834451 0.311053 0.230861 11.00000 -1.20000 H8B 2 0.903503 0.252985 0.154474 11.00000 -1.20000 AFIX 0 O4 5 0.499071 0.644004 0.175963 11.00000 0.13824 0.10382 = 0.31762 -0.06673 0.08943 -0.06277 C10 1 1.027122 0.458952 0.262976 11.00000 0.06673 0.09529 = 0.06332 0.01482 -0.01459 -0.01038 AFIX 23 H10A 2 1.128276 0.476989 0.297697 11.00000 -1.20000 H10B 2 0.984332 0.419933 0.307252 11.00000 -1.20000 AFIX 0 O3 5 0.345613 0.532613 0.112644 11.00000 0.14842 0.11495 = 0.07400 -0.02992 0.02985 -0.02715 C7 1 0.676158 0.278516 0.106053 11.00000 0.08722 0.05439 = 0.07249 -0.00185 0.01193 0.00453 AFIX 23 H7A 2 0.677799 0.265855 0.035946 11.00000 -1.20000 H7B 2 0.642169 0.225749 0.135906 11.00000 -1.20000 AFIX 0 C5 1 0.578816 0.395188 0.290772 11.00000 0.05619 0.06070 = 0.06309 0.01154 0.03361 0.00146 C9 1 1.039359 0.412693 0.171860 11.00000 0.04446 0.09621 = 0.08843 -0.00369 0.02409 0.01079 AFIX 23 H9A 2 1.107006 0.362424 0.188647 11.00000 -1.20000 H9B 2 1.084633 0.451563 0.128677 11.00000 -1.20000 AFIX 0 C4 1 0.549720 0.379596 0.387322 11.00000 0.12560 0.07465 = 0.09808 0.03724 0.07451 0.03390 AFIX 43 H4A 2 0.480142 0.336434 0.397840 11.00000 -1.20000 AFIX 0 O5 5 0.289788 0.265815 0.503522 11.00000 0.06013 0.21204 = 0.14889 -0.00825 -0.01950 -0.00755 O1 5 0.245459 0.668006 0.147311 11.00000 0.15135 0.25811 = 0.16197 0.01049 -0.00789 0.13437 HKLF 4 REM import REM R1 = 0.0460 for 2212 Fo > 4sig(Fo) and 0.1083 for all 4065 data REM 235 parameters refined using 0 restraints END WGHT 0.0658 0.0000 REM Highest difference peak 0.722, deepest hole -1.024, 1-sigma level 0.164 Q1 1 0.3699 0.6626 0.0958 11.00000 0.05 0.72 Q2 1 0.6535 0.5654 0.1827 11.00000 0.05 0.67 Q3 1 0.6806 0.4403 0.1986 11.00000 0.05 0.59 Q4 1 0.4964 0.6459 0.1445 11.00000 0.05 0.59 Q5 1 0.1663 0.5426 0.0818 11.00000 0.05 0.56 Q6 1 0.3501 0.5142 0.1604 11.00000 0.05 0.55 Q7 1 0.5036 0.3528 0.1440 11.00000 0.05 0.55 Q8 1 0.1210 0.2213 0.5469 11.00000 0.05 0.54 Q9 1 0.5407 0.5003 0.2593 11.00000 0.05 0.54 Q10 1 0.6809 0.4483 0.0750 11.00000 0.05 0.54 ; _shelx_res_checksum 10767 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn Pb1 Pb 0.70112(4) 0.49735(3) 0.10736(3) 0.04810(18) Uani 1 1 d . Cl1 Cl 0.3549(3) 0.6059(2) 0.1745(2) 0.0619(7) Uani 1 1 d . Cl2 Cl 0.1516(3) 0.2397(2) 0.4481(2) 0.0613(7) Uani 1 1 d . N1 N 0.6770(9) 0.4573(6) 0.2753(6) 0.0467(19) Uani 1 1 d . C1 C 0.7539(18) 0.5056(7) 0.3497(9) 0.065(3) Uani 1 1 d . C6 C 0.4957(13) 0.3456(9) 0.2007(11) 0.080(4) Uani 1 1 d . H6A H 0.4892 0.2840 0.2191 0.096 Uiso 1 1 calc R H6B H 0.3919 0.3682 0.1831 0.096 Uiso 1 1 calc R N2 N 0.5669(10) 0.3510(6) 0.1116(7) 0.064(3) Uani 1 1 d . H2 H 0.4851 0.3475 0.0516 0.076 Uiso 1 1 calc R N3 N 0.8912(10) 0.3821(7) 0.1173(7) 0.064(3) Uani 1 1 d . H3 H 0.9026 0.3683 0.0483 0.077 Uiso 1 1 calc R N4 N 0.9289(11) 0.5369(7) 0.2397(7) 0.065(3) Uani 1 1 d . H4 H 0.9866 0.5842 0.2146 0.078 Uiso 1 1 calc R C2 C 0.732(2) 0.4934(9) 0.4482(10) 0.094(6) Uani 1 1 d . H2A H 0.7869 0.5269 0.5008 0.112 Uiso 1 1 calc R O6 O 0.1553(14) 0.2450(9) 0.3460(7) 0.126(4) Uani 1 1 d . O8 O 0.0301(10) 0.2906(7) 0.4721(8) 0.104(3) Uani 1 1 d . O2 O 0.3581(15) 0.5783(7) 0.2741(7) 0.133(4) Uani 1 1 d . C11 C 0.8642(15) 0.5702(8) 0.3266(8) 0.073(3) Uani 1 1 d . H11A H 0.9458 0.5786 0.3848 0.087 Uiso 1 1 calc R H11B H 0.8139 0.6265 0.3096 0.087 Uiso 1 1 calc R O7 O 0.1216(18) 0.1512(8) 0.4711(11) 0.157(5) Uani 1 1 d . C3 C 0.626(2) 0.4294(12) 0.4664(11) 0.104(6) Uani 1 1 d . H3A H 0.6079 0.4209 0.5312 0.125 Uiso 1 1 calc R C8 C 0.8348(15) 0.3017(8) 0.1599(10) 0.071(3) Uani 1 1 d . H8A H 0.8345 0.3111 0.2309 0.085 Uiso 1 1 calc R H8B H 0.9035 0.2530 0.1545 0.085 Uiso 1 1 calc R O4 O 0.4991(15) 0.6440(9) 0.1760(16) 0.180(7) Uani 1 1 d . C10 C 1.0271(15) 0.4590(10) 0.2630(10) 0.079(4) Uani 1 1 d . H10A H 1.1283 0.4770 0.2977 0.095 Uiso 1 1 calc R H10B H 0.9843 0.4199 0.3073 0.095 Uiso 1 1 calc R O3 O 0.3456(15) 0.5326(8) 0.1126(8) 0.111(4) Uani 1 1 d . C7 C 0.6762(13) 0.2785(8) 0.1061(9) 0.072(3) Uani 1 1 d . H7A H 0.6778 0.2659 0.0359 0.086 Uiso 1 1 calc R H7B H 0.6422 0.2257 0.1359 0.086 Uiso 1 1 calc R C5 C 0.5788(12) 0.3952(7) 0.2908(8) 0.057(3) Uani 1 1 d . C9 C 1.0394(12) 0.4127(9) 0.1719(10) 0.075(4) Uani 1 1 d . H9A H 1.1070 0.3624 0.1886 0.090 Uiso 1 1 calc R H9B H 1.0846 0.4516 0.1287 0.090 Uiso 1 1 calc R C4 C 0.5497(17) 0.3796(10) 0.3873(12) 0.092(5) Uani 1 1 d . H4A H 0.4801 0.3364 0.3978 0.111 Uiso 1 1 calc R O5 O 0.2898(11) 0.2658(9) 0.5035(9) 0.146(5) Uani 1 1 d . O1 O 0.2455(15) 0.6680(11) 0.1473(10) 0.196(7) 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 Pb1 0.0566(3) 0.0494(3) 0.0373(2) 0.00739(18) 0.00664(16) -0.0012(2) Cl1 0.0667(17) 0.0651(19) 0.0570(16) -0.0011(14) 0.0199(13) 0.0012(15) Cl2 0.0638(16) 0.0609(18) 0.0602(16) 0.0003(14) 0.0145(13) 0.0078(14) N1 0.058(5) 0.044(5) 0.042(4) 0.007(4) 0.017(4) 0.011(4) C1 0.100(9) 0.064(8) 0.032(5) -0.005(5) 0.017(6) 0.011(7) C6 0.054(7) 0.067(9) 0.116(12) 0.028(8) 0.005(7) -0.004(6) N2 0.063(5) 0.069(7) 0.053(5) 0.003(5) -0.001(5) -0.012(5) N3 0.062(5) 0.090(8) 0.043(5) -0.006(5) 0.019(4) 0.008(5) N4 0.067(6) 0.066(6) 0.061(6) 0.009(5) 0.007(5) -0.028(5) C2 0.171(17) 0.078(11) 0.040(6) -0.002(6) 0.043(9) 0.041(10) O6 0.156(9) 0.156(12) 0.068(6) 0.021(7) 0.026(6) 0.037(8) O8 0.093(6) 0.086(7) 0.138(8) -0.037(6) 0.030(6) 0.026(5) O2 0.230(13) 0.124(10) 0.058(6) -0.007(6) 0.058(7) -0.017(9) C11 0.104(9) 0.059(8) 0.048(6) -0.006(6) -0.003(6) -0.008(7) O7 0.249(14) 0.072(8) 0.188(13) -0.001(8) 0.136(11) 0.027(9) C3 0.162(14) 0.098(12) 0.076(10) 0.039(10) 0.082(10) 0.065(12) C8 0.092(9) 0.059(8) 0.067(8) 0.013(6) 0.025(7) 0.020(7) O4 0.138(10) 0.104(10) 0.32(2) -0.067(12) 0.089(12) -0.063(9) C10 0.067(8) 0.095(10) 0.063(8) 0.015(8) -0.015(7) -0.010(8) O3 0.148(10) 0.115(8) 0.074(7) -0.030(7) 0.030(7) -0.027(8) C7 0.087(9) 0.054(8) 0.072(8) -0.002(6) 0.012(7) 0.005(6) C5 0.056(6) 0.061(7) 0.063(7) 0.012(6) 0.034(5) 0.001(6) C9 0.044(6) 0.096(10) 0.088(9) -0.004(8) 0.024(6) 0.011(6) C4 0.126(12) 0.075(10) 0.098(11) 0.037(9) 0.075(10) 0.034(9) O5 0.060(5) 0.212(14) 0.149(9) -0.008(9) -0.020(6) -0.008(7) O1 0.151(11) 0.258(18) 0.162(12) 0.010(12) -0.008(9) 0.134(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' Cl Cl 0.1484 0.1585 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 Pb1 N2 68.1(3) N1 Pb1 N3 87.4(3) N1 Pb1 N4 65.9(3) N3 Pb1 N2 72.1(3) N3 Pb1 N4 70.9(3) N4 Pb1 N2 121.0(3) O2 Cl1 O4 105.1(10) O2 Cl1 O3 109.1(7) O3 Cl1 O4 106.7(8) O1 Cl1 O2 110.3(8) O1 Cl1 O4 109.0(11) O1 Cl1 O3 116.0(9) O6 Cl2 O8 111.2(7) O7 Cl2 O6 108.4(8) O7 Cl2 O8 106.4(8) O5 Cl2 O6 109.6(8) O5 Cl2 O8 111.2(7) O5 Cl2 O7 110.0(9) C1 N1 Pb1 116.9(8) C1 N1 C5 122.1(10) C5 N1 Pb1 120.7(7) N1 C1 C2 120.4(13) N1 C1 C11 118.5(10) C2 C1 C11 121.1(13) N2 C6 C5 114.6(9) C6 N2 Pb1 110.4(7) C6 N2 C7 113.1(9) C7 N2 Pb1 109.5(7) C8 N3 Pb1 109.3(7) C8 N3 C9 114.0(10) C9 N3 Pb1 110.7(7) C11 N4 Pb1 105.2(6) C11 N4 C10 114.1(9) C10 N4 Pb1 109.1(8) C1 C2 C3 118.7(15) C1 C11 N4 108.7(9) C4 C3 C2 119.2(13) N3 C8 C7 111.2(10) C9 C10 N4 110.4(10) N2 C7 C8 111.6(10) N1 C5 C6 117.6(10) N1 C5 C4 120.8(12) C4 C5 C6 121.5(12) C10 C9 N3 112.2(9) C5 C4 C3 118.7(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pb1 N1 2.400(8) Pb1 N2 2.525(9) Pb1 N3 2.416(9) Pb1 N4 2.503(8) Cl1 O2 1.405(9) Cl1 O4 1.402(12) Cl1 O3 1.383(11) Cl1 O1 1.352(11) Cl2 O6 1.391(10) Cl2 O8 1.415(9) Cl2 O7 1.413(12) Cl2 O5 1.368(9) N1 C1 1.323(15) N1 C5 1.328(12) C1 C2 1.393(17) C1 C11 1.462(17) C6 N2 1.468(16) C6 C5 1.498(18) N2 C7 1.478(14) N3 C8 1.477(15) N3 C9 1.455(13) N4 C11 1.492(15) N4 C10 1.467(17) C2 C3 1.41(2) C3 C4 1.38(2) C8 C7 1.499(16) C10 C9 1.440(16) C5 C4 1.399(15)