# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm #TrackingRef '- new csl .txt' _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wei-Guang, Zhang' _publ_contact_author_email wgzhang@scnu.edu.cn _publ_section_title ; An unprecedented (3,4,14)-connected 3D metal Corganic framework based on planar octanuclear lead(II) cluster as a secondary building unit ; loop_ _publ_author_name 'Song-Liang Cai' 'Sheng-Run Zheng' 'Jing-Bo Tan' 'Jun Fan' data_csl-1 _database_code_depnum_ccdc_archive 'CCDC 847441' #TrackingRef '- new csl .txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H14 Cl N9 O12 Pb4' _chemical_formula_weight 1556.71 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/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 8.8709(18) _cell_length_b 30.672(6) _cell_length_c 13.972(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.065(10) _cell_angle_gamma 90.00 _cell_volume 3385.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2424 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 23.84 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 19.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0654 _exptl_absorpt_correction_T_max 0.1021 _exptl_absorpt_process_details 'Higashi, T. (1995)' _exptl_special_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 298(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 17428 _diffrn_reflns_av_R_equivalents 0.0794 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.25 _reflns_number_total 6116 _reflns_number_gt 4220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ISOR and SIMU restraints are used for C11 and C19 to made their U(eq) more resonable. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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 6116 _refine_ls_number_parameters 505 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 -0.19628(7) -0.341315(17) 0.18157(4) 0.02392(15) Uani 1 1 d . . . Pb2 Pb 0.41408(8) -0.192569(18) 0.12887(5) 0.02758(16) Uani 1 1 d . . . Pb3 Pb -0.35416(7) -0.490581(17) 0.17136(4) 0.02238(15) Uani 1 1 d . . . Pb4 Pb 0.22060(8) -0.435456(19) 0.51583(5) 0.02899(17) Uani 1 1 d . . . Cl1 Cl 0.1515(7) -0.36647(16) 0.3930(4) 0.0634(15) Uani 1 1 d . . . O1 O -0.0128(13) -0.3820(3) 0.1235(8) 0.034(3) Uani 1 1 d . . . O2 O 0.2270(14) -0.3882(3) 0.1121(9) 0.043(3) Uani 1 1 d . . . H2 H 0.2917 -0.3722 0.1014 0.065 Uiso 1 1 d R . . O3 O 0.4544(14) -0.3391(3) 0.1264(10) 0.045(3) Uani 1 1 d . . . O4 O 0.5256(13) -0.2686(3) 0.1501(9) 0.035(3) Uani 1 1 d . . . O5 O -0.3280(13) -0.4111(3) 0.1106(7) 0.028(2) Uani 1 1 d . . . O6 O -0.5094(17) -0.4484(3) -0.0254(8) 0.060(4) Uani 1 1 d . . . O7 O -0.6706(15) -0.4370(3) -0.2544(8) 0.042(3) Uani 1 1 d . . . O8 O -0.7275(12) -0.3757(3) -0.3483(7) 0.026(2) Uani 1 1 d . . . O9 O -0.1424(14) -0.4623(4) 0.3494(9) 0.048(3) Uani 1 1 d . . . O10 O -0.0858(14) -0.4289(4) 0.4995(8) 0.042(3) Uani 1 1 d . . . O11 O -0.2231(14) -0.4093(4) 0.6131(9) 0.050(3) Uani 1 1 d . . . H11 H -0.1743 -0.4164 0.5777 0.076 Uiso 1 1 d R . . O12 O -0.4794(13) -0.4104(4) 0.5981(8) 0.041(3) Uani 1 1 d . . . N1 N 0.0288(15) -0.2934(3) 0.1646(9) 0.022(3) Uani 1 1 d . . . N2 N 0.2356(15) -0.2489(4) 0.1743(10) 0.025(3) Uani 1 1 d . . . N3 N -0.2430(16) -0.1880(4) 0.2120(10) 0.029(3) Uani 1 1 d . . . N4 N -0.3508(15) -0.3398(3) -0.0128(9) 0.023(3) Uani 1 1 d . . . N5 N -0.4976(17) -0.3285(3) -0.1885(10) 0.029(3) Uani 1 1 d . . . N6 N -0.124(3) -0.2131(6) -0.0631(13) 0.072(6) Uani 1 1 d . . . N7 N -0.4740(17) -0.4763(4) 0.3095(9) 0.035(3) Uani 1 1 d . . . N8 N -0.6082(15) -0.4559(4) 0.4064(9) 0.027(3) Uani 1 1 d . . . N9 N -1.0758(17) -0.5047(4) 0.1604(10) 0.033(3) Uani 1 1 d . . . C1 C 0.116(2) -0.3644(5) 0.1267(12) 0.030(4) Uani 1 1 d . . . C2 C 0.1403(19) -0.3171(5) 0.1454(12) 0.027(4) Uani 1 1 d . . . C3 C 0.2681(18) -0.2898(4) 0.1506(11) 0.021(3) Uani 1 1 d . . . C4 C 0.424(2) -0.2989(5) 0.1412(12) 0.031(4) Uani 1 1 d . . . C5 C 0.0906(18) -0.2524(4) 0.1843(11) 0.020(3) Uani 1 1 d . . . C6 C 0.010(2) -0.2172(5) 0.2172(12) 0.028(4) Uani 1 1 d . . . C7 C 0.104(2) -0.1860(5) 0.2858(13) 0.035(4) Uani 1 1 d . . . H7 H 0.2206 -0.1853 0.3122 0.042 Uiso 1 1 calc R . . C8 C 0.021(2) -0.1547(5) 0.3163(13) 0.037(4) Uani 1 1 d . . . H8 H 0.0815 -0.1322 0.3623 0.045 Uiso 1 1 calc R . . C9 C -0.1442(19) -0.1570(4) 0.2801(13) 0.025(4) Uani 1 1 d . . . H9 H -0.1961 -0.1358 0.3028 0.030 Uiso 1 1 calc R . . C10 C -0.157(2) -0.2177(4) 0.1851(12) 0.027(4) Uani 1 1 d . . . H10 H -0.2193 -0.2405 0.1408 0.033 Uiso 1 1 calc R . . C11 C -0.425(2) -0.4155(4) 0.0120(10) 0.025(3) Uani 1 1 d U . . C12 C -0.4359(18) -0.3775(4) -0.0582(10) 0.020(3) Uani 1 1 d . . . C13 C -0.5284(19) -0.3708(4) -0.1691(11) 0.024(3) Uani 1 1 d . . . C14 C -0.6555(19) -0.3969(4) -0.2611(11) 0.021(3) Uani 1 1 d . . . C15 C -0.3942(19) -0.3118(4) -0.0947(11) 0.024(3) Uani 1 1 d . . . C16 C -0.336(2) -0.2653(4) -0.0830(11) 0.026(4) Uani 1 1 d . . . C17 C -0.449(3) -0.2329(5) -0.0908(12) 0.052(5) Uani 1 1 d . . . H17 H -0.5586 -0.2396 -0.1023 0.062 Uiso 1 1 calc R . . C18 C -0.393(3) -0.1882(6) -0.0804(14) 0.062(6) Uani 1 1 d . . . H18A H -0.4607 -0.1649 -0.0816 0.074 Uiso 1 1 calc R . . C19 C -0.233(4) -0.1826(7) -0.0689(15) 0.068(6) Uani 1 1 d U . . H19 H -0.1962 -0.1539 -0.0646 0.082 Uiso 1 1 calc R . . C20 C -0.178(2) -0.2555(5) -0.0698(13) 0.045(5) Uani 1 1 d . . . H20 H -0.1047 -0.2781 -0.0653 0.054 Uiso 1 1 calc R . . C21 C -0.187(2) -0.4490(5) 0.4136(13) 0.032(4) Uani 1 1 d . . . C22 C -0.3635(19) -0.4549(4) 0.3972(11) 0.025(3) Uani 1 1 d . . . C23 C -0.4467(19) -0.4430(5) 0.4568(12) 0.026(4) Uani 1 1 d . . . C24 C -0.382(2) -0.4196(6) 0.5606(14) 0.041(4) Uani 1 1 d . . . C25 C -0.6195(19) -0.4762(5) 0.3196(11) 0.025(4) Uani 1 1 d . . . C26 C -0.780(2) -0.4967(4) 0.2351(11) 0.025(4) Uani 1 1 d . . . C27 C -0.775(2) -0.5281(5) 0.1661(13) 0.042(5) Uani 1 1 d . . . H27 H -0.6719 -0.5370 0.1706 0.050 Uiso 1 1 calc R . . C28 C -0.923(2) -0.5465(5) 0.0908(13) 0.040(4) Uani 1 1 d . . . H28 H -0.9244 -0.5657 0.0388 0.048 Uiso 1 1 calc R . . C29 C -1.070(2) -0.5349(5) 0.0965(13) 0.035(4) Uani 1 1 d . . . H29 H -1.1697 -0.5495 0.0524 0.042 Uiso 1 1 calc R . . C30 C -0.927(2) -0.4870(5) 0.2307(12) 0.034(4) Uani 1 1 d . . . H30 H -0.9294 -0.4666 0.2794 0.041 Uiso 1 1 calc R . . 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 0.0271(4) 0.0220(3) 0.0197(3) -0.0053(2) 0.0081(3) -0.0059(2) Pb2 0.0343(4) 0.0246(3) 0.0210(3) -0.0039(2) 0.0101(3) 0.0025(3) Pb3 0.0249(3) 0.0188(3) 0.0189(3) -0.0020(2) 0.0060(3) -0.0045(2) Pb4 0.0239(4) 0.0336(4) 0.0249(3) -0.0079(3) 0.0072(3) -0.0040(3) Cl1 0.077(4) 0.069(3) 0.031(3) 0.016(2) 0.013(3) 0.027(3) O1 0.021(7) 0.034(6) 0.034(7) -0.017(5) 0.000(5) -0.001(5) O2 0.038(8) 0.018(6) 0.082(9) -0.010(6) 0.035(7) -0.005(5) O3 0.036(8) 0.021(6) 0.094(10) -0.014(6) 0.044(7) -0.001(5) O4 0.021(6) 0.023(6) 0.060(8) 0.000(5) 0.017(6) 0.000(5) O5 0.040(7) 0.025(6) 0.017(6) 0.006(4) 0.010(5) -0.004(5) O6 0.102(11) 0.034(7) 0.012(6) 0.001(5) -0.003(7) -0.038(7) O7 0.068(9) 0.025(6) 0.022(6) -0.002(5) 0.010(6) -0.006(6) O8 0.033(7) 0.013(5) 0.019(6) -0.002(4) 0.000(5) -0.002(4) O9 0.030(7) 0.082(9) 0.039(7) -0.039(6) 0.021(6) -0.008(6) O10 0.025(7) 0.073(8) 0.029(7) -0.031(6) 0.013(6) -0.009(6) O11 0.021(7) 0.093(10) 0.043(8) -0.039(7) 0.021(6) -0.025(6) O12 0.025(7) 0.063(8) 0.037(7) -0.023(6) 0.016(6) -0.019(6) N1 0.032(8) 0.016(7) 0.018(7) -0.010(5) 0.011(6) -0.001(6) N2 0.024(8) 0.023(7) 0.038(8) -0.007(6) 0.023(7) -0.008(5) N3 0.030(8) 0.025(7) 0.034(8) 0.002(6) 0.016(7) 0.003(6) N4 0.036(8) 0.014(6) 0.019(7) 0.005(5) 0.014(6) 0.003(6) N5 0.043(9) 0.014(6) 0.028(8) 0.003(5) 0.015(7) -0.010(6) N6 0.120(18) 0.045(11) 0.054(12) -0.008(9) 0.041(12) -0.030(11) N7 0.028(8) 0.055(9) 0.013(7) -0.021(6) 0.002(6) -0.015(7) N8 0.012(7) 0.035(8) 0.030(8) -0.013(6) 0.006(6) 0.003(6) N9 0.032(9) 0.019(7) 0.032(8) -0.008(6) 0.000(7) -0.007(6) C1 0.019(10) 0.026(9) 0.039(10) -0.009(7) 0.008(8) 0.005(7) C2 0.025(10) 0.024(9) 0.027(9) -0.005(6) 0.008(7) -0.007(7) C3 0.024(9) 0.021(8) 0.020(8) -0.014(6) 0.011(7) -0.001(7) C4 0.028(10) 0.026(9) 0.039(10) -0.015(7) 0.016(8) -0.013(8) C5 0.017(8) 0.017(8) 0.030(9) -0.012(6) 0.015(7) -0.002(6) C6 0.033(11) 0.027(9) 0.031(9) -0.010(7) 0.022(8) -0.009(7) C7 0.025(10) 0.032(10) 0.046(11) -0.017(8) 0.015(9) -0.003(7) C8 0.034(11) 0.032(10) 0.046(11) -0.023(8) 0.017(9) -0.022(8) C9 0.022(9) 0.014(8) 0.054(11) -0.006(7) 0.029(8) 0.000(7) C10 0.036(11) 0.016(8) 0.043(10) -0.001(7) 0.029(9) -0.005(7) C11 0.039(9) 0.023(8) 0.003(7) 0.000(6) 0.001(6) 0.002(7) C12 0.027(9) 0.018(8) 0.007(7) -0.002(6) 0.002(7) 0.008(6) C13 0.028(10) 0.026(9) 0.014(8) 0.007(6) 0.006(7) 0.009(7) C14 0.032(10) 0.015(8) 0.018(8) -0.012(6) 0.015(7) -0.007(7) C15 0.031(10) 0.020(8) 0.015(8) 0.004(6) 0.005(7) 0.000(7) C16 0.048(11) 0.009(7) 0.012(8) 0.004(6) 0.007(7) -0.005(7) C17 0.078(15) 0.040(11) 0.017(9) -0.006(8) 0.003(9) 0.006(10) C18 0.095(19) 0.041(12) 0.020(10) -0.004(8) 0.001(11) 0.014(12) C19 0.114(16) 0.044(11) 0.029(10) 0.005(8) 0.018(11) -0.025(12) C20 0.063(14) 0.038(11) 0.033(11) 0.004(8) 0.019(10) -0.023(9) C21 0.038(11) 0.036(10) 0.034(10) -0.001(8) 0.026(9) -0.005(8) C22 0.022(9) 0.022(8) 0.025(9) -0.003(6) 0.006(7) 0.000(7) C23 0.015(9) 0.030(9) 0.035(10) -0.011(7) 0.012(8) -0.001(7) C24 0.013(10) 0.064(12) 0.049(12) 0.002(9) 0.017(9) 0.006(9) C25 0.022(9) 0.029(9) 0.017(8) -0.008(6) 0.004(7) -0.001(7) C26 0.027(10) 0.017(8) 0.023(9) -0.005(6) 0.005(7) -0.011(7) C27 0.051(13) 0.028(10) 0.048(12) -0.015(8) 0.023(10) -0.012(8) C28 0.026(10) 0.039(10) 0.037(11) -0.022(8) 0.000(8) -0.004(8) C29 0.028(10) 0.031(10) 0.041(11) -0.006(8) 0.011(8) -0.013(8) C30 0.040(12) 0.027(9) 0.033(10) -0.009(7) 0.016(9) -0.023(8) _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 N4 2.423(11) . ? Pb1 O5 2.425(9) . ? Pb1 O1 2.463(10) . ? Pb1 N1 2.575(11) . ? Pb2 N5 2.393(12) 4_656 ? Pb2 O4 2.498(9) . ? Pb2 O8 2.534(9) 4_656 ? Pb2 N2 2.610(11) . ? Pb2 N3 2.721(13) 1_655 ? Pb3 O7 2.469(10) 3_445 ? Pb3 O9 2.493(10) . ? Pb3 N9 2.579(13) 1_655 ? Pb3 O6 2.623(10) 3_445 ? Pb3 O5 2.625(9) . ? Pb3 N7 2.630(12) . ? Pb4 O12 2.492(10) 1_655 ? Pb4 O8 2.527(9) 1_656 ? Pb4 Cl1 2.616(4) . ? Pb4 O10 2.629(10) . ? Pb4 N8 2.674(11) 1_655 ? O1 C1 1.245(17) . ? O2 C1 1.313(16) . ? O2 H2 0.8198 . ? O3 C4 1.299(16) . ? O4 C4 1.261(16) . ? O5 C11 1.256(15) . ? O6 C11 1.224(16) . ? O6 Pb3 2.623(10) 3_445 ? O7 C14 1.245(15) . ? O7 Pb3 2.469(10) 3_445 ? O8 C14 1.269(16) . ? O8 Pb4 2.527(9) 1_454 ? O8 Pb2 2.534(9) 4_455 ? O9 C21 1.207(16) . ? O10 C21 1.284(18) . ? O11 C24 1.299(18) . ? O11 H11 0.8201 . ? O12 C24 1.228(16) . ? O12 Pb4 2.492(10) 1_455 ? N1 C2 1.349(17) . ? N1 C5 1.349(15) . ? N2 C3 1.360(16) . ? N2 C5 1.360(16) . ? N3 C10 1.345(16) . ? N3 C9 1.349(18) . ? N3 Pb2 2.721(13) 1_455 ? N4 C15 1.340(16) . ? N4 C12 1.368(16) . ? N5 C15 1.315(17) . ? N5 C13 1.376(16) . ? N5 Pb2 2.393(12) 4_455 ? N6 C19 1.32(3) . ? N6 C20 1.37(2) . ? N7 C22 1.341(17) . ? N7 C25 1.361(18) . ? N8 C25 1.326(16) . ? N8 C23 1.337(17) . ? N8 Pb4 2.674(11) 1_455 ? N9 C29 1.305(18) . ? N9 C30 1.347(19) . ? N9 Pb3 2.579(13) 1_455 ? C1 C2 1.474(19) . ? C2 C3 1.385(19) . ? C3 C4 1.473(19) . ? C5 C6 1.480(18) . ? C6 C10 1.34(2) . ? C6 C7 1.341(19) . ? C7 C8 1.389(19) . ? C7 H7 0.9300 . ? C8 C9 1.31(2) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.498(18) . ? C12 C13 1.400(17) . ? C13 C14 1.498(19) . ? C15 C16 1.499(18) . ? C16 C20 1.37(2) . ? C16 C17 1.38(2) . ? C17 C18 1.44(2) . ? C17 H17 0.9300 . ? C18 C19 1.36(3) . ? C18 H18A 0.9300 . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.48(2) . ? C22 C23 1.390(19) . ? C23 C24 1.48(2) . ? C25 C26 1.510(19) . ? C26 C30 1.32(2) . ? C26 C27 1.377(19) . ? C27 C28 1.37(2) . ? C27 H27 0.9300 . ? C28 C29 1.39(2) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 H30 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 N4 Pb1 O5 68.7(3) . . ? N4 Pb1 O1 76.2(4) . . ? O5 Pb1 O1 71.7(3) . . ? N4 Pb1 N1 87.3(4) . . ? O5 Pb1 N1 135.7(3) . . ? O1 Pb1 N1 66.6(3) . . ? N5 Pb2 O4 101.9(4) 4_656 . ? N5 Pb2 O8 65.3(3) 4_656 4_656 ? O4 Pb2 O8 161.5(3) . 4_656 ? N5 Pb2 N2 82.0(4) 4_656 . ? O4 Pb2 N2 66.7(3) . . ? O8 Pb2 N2 97.3(3) 4_656 . ? N5 Pb2 N3 76.7(4) 4_656 1_655 ? O4 Pb2 N3 72.1(3) . 1_655 ? O8 Pb2 N3 115.2(3) 4_656 1_655 ? N2 Pb2 N3 127.9(4) . 1_655 ? O7 Pb3 O9 88.7(4) 3_445 . ? O7 Pb3 N9 89.7(4) 3_445 1_655 ? O9 Pb3 N9 79.1(4) . 1_655 ? O7 Pb3 O6 68.6(3) 3_445 3_445 ? O9 Pb3 O6 153.6(4) . 3_445 ? N9 Pb3 O6 87.1(4) 1_655 3_445 ? O7 Pb3 O5 170.0(3) 3_445 . ? O9 Pb3 O5 82.1(4) . . ? N9 Pb3 O5 84.7(3) 1_655 . ? O6 Pb3 O5 119.2(3) 3_445 . ? O7 Pb3 N7 77.5(4) 3_445 . ? O9 Pb3 N7 65.3(4) . . ? N9 Pb3 N7 142.1(4) 1_655 . ? O6 Pb3 N7 119.5(4) 3_445 . ? O5 Pb3 N7 102.0(3) . . ? O12 Pb4 O8 68.8(3) 1_655 1_656 ? O12 Pb4 Cl1 86.3(3) 1_655 . ? O8 Pb4 Cl1 79.3(2) 1_656 . ? O12 Pb4 O10 149.4(3) 1_655 . ? O8 Pb4 O10 80.6(3) 1_656 . ? Cl1 Pb4 O10 87.5(3) . . ? O12 Pb4 N8 64.6(3) 1_655 1_655 ? O8 Pb4 N8 130.0(3) 1_656 1_655 ? Cl1 Pb4 N8 80.7(3) . 1_655 ? O10 Pb4 N8 143.3(3) . 1_655 ? C1 O1 Pb1 120.2(9) . . ? C1 O2 H2 109.4 . . ? C4 O4 Pb2 116.7(9) . . ? C11 O5 Pb1 120.3(8) . . ? C11 O5 Pb3 98.0(8) . . ? Pb1 O5 Pb3 141.7(4) . . ? C11 O6 Pb3 153.8(10) . 3_445 ? C14 O7 Pb3 159.1(9) . 3_445 ? C14 O8 Pb4 100.9(7) . 1_454 ? C14 O8 Pb2 118.9(8) . 4_455 ? Pb4 O8 Pb2 115.9(4) 1_454 4_455 ? C21 O9 Pb3 120.4(11) . . ? C21 O10 Pb4 107.6(9) . . ? C24 O11 H11 109.4 . . ? C24 O12 Pb4 122.8(10) . 1_455 ? C2 N1 C5 106.0(11) . . ? C2 N1 Pb1 112.4(8) . . ? C5 N1 Pb1 140.6(9) . . ? C3 N2 C5 105.5(11) . . ? C3 N2 Pb2 109.4(8) . . ? C5 N2 Pb2 141.7(9) . . ? C10 N3 C9 114.1(13) . . ? C10 N3 Pb2 120.6(10) . 1_455 ? C9 N3 Pb2 125.4(9) . 1_455 ? C15 N4 C12 105.2(12) . . ? C15 N4 Pb1 140.0(9) . . ? C12 N4 Pb1 114.5(8) . . ? C15 N5 C13 106.5(11) . . ? C15 N5 Pb2 134.3(9) . 4_455 ? C13 N5 Pb2 117.8(9) . 4_455 ? C19 N6 C20 116(2) . . ? C22 N7 C25 103.7(12) . . ? C22 N7 Pb3 112.4(10) . . ? C25 N7 Pb3 142.7(9) . . ? C25 N8 C23 103.8(12) . . ? C25 N8 Pb4 143.8(10) . 1_455 ? C23 N8 Pb4 112.3(9) . 1_455 ? C29 N9 C30 117.1(15) . . ? C29 N9 Pb3 119.7(10) . 1_455 ? C30 N9 Pb3 122.3(10) . 1_455 ? O1 C1 O2 119.7(13) . . ? O1 C1 C2 119.3(13) . . ? O2 C1 C2 121.0(14) . . ? N1 C2 C3 108.7(12) . . ? N1 C2 C1 120.3(13) . . ? C3 C2 C1 131.0(14) . . ? N2 C3 C2 108.1(12) . . ? N2 C3 C4 120.5(12) . . ? C2 C3 C4 131.3(13) . . ? O4 C4 O3 121.5(14) . . ? O4 C4 C3 120.7(13) . . ? O3 C4 C3 117.8(13) . . ? N1 C5 N2 111.6(11) . . ? N1 C5 C6 122.4(12) . . ? N2 C5 C6 125.9(12) . . ? C10 C6 C7 118.6(14) . . ? C10 C6 C5 120.2(13) . . ? C7 C6 C5 120.9(14) . . ? C6 C7 C8 118.0(15) . . ? C6 C7 H7 121.0 . . ? C8 C7 H7 121.0 . . ? C9 C8 C7 119.9(14) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 N3 124.1(13) . . ? C8 C9 H9 118.0 . . ? N3 C9 H9 118.0 . . ? N3 C10 C6 125.3(14) . . ? N3 C10 H10 117.4 . . ? C6 C10 H10 117.4 . . ? O6 C11 O5 122.4(13) . . ? O6 C11 C12 121.2(12) . . ? O5 C11 C12 116.4(12) . . ? N4 C12 C13 108.2(12) . . ? N4 C12 C11 119.7(11) . . ? C13 C12 C11 132.1(13) . . ? N5 C13 C12 106.7(12) . . ? N5 C13 C14 118.3(12) . . ? C12 C13 C14 134.8(13) . . ? O7 C14 O8 123.7(12) . . ? O7 C14 C13 121.9(13) . . ? O8 C14 C13 113.7(11) . . ? N5 C15 N4 113.5(12) . . ? N5 C15 C16 122.0(12) . . ? N4 C15 C16 124.5(13) . . ? C20 C16 C17 121.2(15) . . ? C20 C16 C15 120.2(14) . . ? C17 C16 C15 118.5(16) . . ? C16 C17 C18 118.0(19) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? C19 C18 C17 115.4(19) . . ? C19 C18 H18A 122.3 . . ? C17 C18 H18A 122.3 . . ? N6 C19 C18 128(2) . . ? N6 C19 H19 116.2 . . ? C18 C19 H19 116.2 . . ? C16 C20 N6 121.5(18) . . ? C16 C20 H20 119.3 . . ? N6 C20 H20 119.3 . . ? O9 C21 O10 121.9(15) . . ? O9 C21 C22 121.6(15) . . ? O10 C21 C22 116.5(13) . . ? N7 C22 C23 108.1(13) . . ? N7 C22 C21 118.8(13) . . ? C23 C22 C21 133.1(13) . . ? N8 C23 C22 109.8(13) . . ? N8 C23 C24 120.3(12) . . ? C22 C23 C24 129.9(14) . . ? O12 C24 O11 119.8(16) . . ? O12 C24 C23 119.8(14) . . ? O11 C24 C23 120.4(13) . . ? N8 C25 N7 114.5(13) . . ? N8 C25 C26 124.3(13) . . ? N7 C25 C26 121.2(12) . . ? C30 C26 C27 118.0(15) . . ? C30 C26 C25 120.3(13) . . ? C27 C26 C25 121.4(15) . . ? C28 C27 C26 120.1(17) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 116.4(15) . . ? C27 C28 H28 121.8 . . ? C29 C28 H28 121.8 . . ? N9 C29 C28 123.5(15) . . ? N9 C29 H29 118.3 . . ? C28 C29 H29 118.3 . . ? C26 C30 N9 124.4(15) . . ? C26 C30 H30 117.8 . . ? N9 C30 H30 117.8 . . ? 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 N4 Pb1 O1 C1 103.3(12) . . . . ? O5 Pb1 O1 C1 175.1(12) . . . . ? N1 Pb1 O1 C1 10.3(11) . . . . ? N5 Pb2 O4 C4 95.5(11) 4_656 . . . ? O8 Pb2 O4 C4 51.0(17) 4_656 . . . ? N2 Pb2 O4 C4 19.8(10) . . . . ? N3 Pb2 O4 C4 167.2(11) 1_655 . . . ? N4 Pb1 O5 C11 -5.9(11) . . . . ? O1 Pb1 O5 C11 -87.8(11) . . . . ? N1 Pb1 O5 C11 -67.7(12) . . . . ? N4 Pb1 O5 Pb3 177.0(8) . . . . ? O1 Pb1 O5 Pb3 95.0(7) . . . . ? N1 Pb1 O5 Pb3 115.2(7) . . . . ? O7 Pb3 O5 C11 153.5(17) 3_445 . . . ? O9 Pb3 O5 C11 177.0(9) . . . . ? N9 Pb3 O5 C11 97.4(9) 1_655 . . . ? O6 Pb3 O5 C11 13.6(10) 3_445 . . . ? N7 Pb3 O5 C11 -120.4(9) . . . . ? O7 Pb3 O5 Pb1 -29(2) 3_445 . . . ? O9 Pb3 O5 Pb1 -5.5(7) . . . . ? N9 Pb3 O5 Pb1 -85.1(7) 1_655 . . . ? O6 Pb3 O5 Pb1 -168.9(6) 3_445 . . . ? N7 Pb3 O5 Pb1 57.1(7) . . . . ? O7 Pb3 O9 C21 -87.1(13) 3_445 . . . ? N9 Pb3 O9 C21 -177.1(13) 1_655 . . . ? O6 Pb3 O9 C21 -117.2(13) 3_445 . . . ? O5 Pb3 O9 C21 96.8(13) . . . . ? N7 Pb3 O9 C21 -10.3(12) . . . . ? O12 Pb4 O10 C21 164.3(9) 1_655 . . . ? O8 Pb4 O10 C21 165.5(10) 1_656 . . . ? Cl1 Pb4 O10 C21 85.9(10) . . . . ? N8 Pb4 O10 C21 15.1(13) 1_655 . . . ? N4 Pb1 N1 C2 -83.6(9) . . . . ? O5 Pb1 N1 C2 -28.3(11) . . . . ? O1 Pb1 N1 C2 -7.5(9) . . . . ? N4 Pb1 N1 C5 110.2(15) . . . . ? O5 Pb1 N1 C5 165.5(13) . . . . ? O1 Pb1 N1 C5 -173.7(16) . . . . ? N5 Pb2 N2 C3 -126.2(10) 4_656 . . . ? O4 Pb2 N2 C3 -19.5(9) . . . . ? O8 Pb2 N2 C3 170.0(9) 4_656 . . . ? N3 Pb2 N2 C3 -60.0(10) 1_655 . . . ? N5 Pb2 N2 C5 79.4(15) 4_656 . . . ? O4 Pb2 N2 C5 -173.9(16) . . . . ? O8 Pb2 N2 C5 15.6(15) 4_656 . . . ? N3 Pb2 N2 C5 145.6(14) 1_655 . . . ? O5 Pb1 N4 C15 175.7(16) . . . . ? O1 Pb1 N4 C15 -108.9(15) . . . . ? N1 Pb1 N4 C15 -42.4(15) . . . . ? O5 Pb1 N4 C12 3.3(9) . . . . ? O1 Pb1 N4 C12 78.7(9) . . . . ? N1 Pb1 N4 C12 145.2(9) . . . . ? O7 Pb3 N7 C22 104.2(11) 3_445 . . . ? O9 Pb3 N7 C22 9.8(10) . . . . ? N9 Pb3 N7 C22 31.3(13) 1_655 . . . ? O6 Pb3 N7 C22 160.5(9) 3_445 . . . ? O5 Pb3 N7 C22 -65.6(11) . . . . ? O7 Pb3 N7 C25 -91.1(17) 3_445 . . . ? O9 Pb3 N7 C25 174.5(18) . . . . ? N9 Pb3 N7 C25 -164.0(15) 1_655 . . . ? O6 Pb3 N7 C25 -34.8(18) 3_445 . . . ? O5 Pb3 N7 C25 99.1(17) . . . . ? Pb1 O1 C1 O2 169.2(10) . . . . ? Pb1 O1 C1 C2 -11.6(19) . . . . ? C5 N1 C2 C3 -1.7(16) . . . . ? Pb1 N1 C2 C3 -172.7(9) . . . . ? C5 N1 C2 C1 176.5(13) . . . . ? Pb1 N1 C2 C1 5.5(16) . . . . ? O1 C1 C2 N1 4(2) . . . . ? O2 C1 C2 N1 -177.3(14) . . . . ? O1 C1 C2 C3 -178.7(15) . . . . ? O2 C1 C2 C3 0(3) . . . . ? C5 N2 C3 C2 0.8(16) . . . . ? Pb2 N2 C3 C2 -163.0(9) . . . . ? C5 N2 C3 C4 -175.8(13) . . . . ? Pb2 N2 C3 C4 20.3(16) . . . . ? N1 C2 C3 N2 0.6(17) . . . . ? C1 C2 C3 N2 -177.4(15) . . . . ? N1 C2 C3 C4 176.7(14) . . . . ? C1 C2 C3 C4 -1(3) . . . . ? Pb2 O4 C4 O3 164.1(12) . . . . ? Pb2 O4 C4 C3 -17.7(18) . . . . ? N2 C3 C4 O4 -3(2) . . . . ? C2 C3 C4 O4 -179.0(15) . . . . ? N2 C3 C4 O3 175.0(13) . . . . ? C2 C3 C4 O3 -1(2) . . . . ? C2 N1 C5 N2 2.3(16) . . . . ? Pb1 N1 C5 N2 169.1(10) . . . . ? C2 N1 C5 C6 -175.3(13) . . . . ? Pb1 N1 C5 C6 -9(2) . . . . ? C3 N2 C5 N1 -2.0(16) . . . . ? Pb2 N2 C5 N1 153.0(11) . . . . ? C3 N2 C5 C6 175.5(14) . . . . ? Pb2 N2 C5 C6 -30(2) . . . . ? N1 C5 C6 C10 -29(2) . . . . ? N2 C5 C6 C10 153.5(15) . . . . ? N1 C5 C6 C7 145.5(15) . . . . ? N2 C5 C6 C7 -32(2) . . . . ? C10 C6 C7 C8 -3(2) . . . . ? C5 C6 C7 C8 -177.7(14) . . . . ? C6 C7 C8 C9 2(2) . . . . ? C7 C8 C9 N3 -1(3) . . . . ? C10 N3 C9 C8 1(2) . . . . ? Pb2 N3 C9 C8 -177.7(12) 1_455 . . . ? C9 N3 C10 C6 -3(2) . . . . ? Pb2 N3 C10 C6 176.4(11) 1_455 . . . ? C7 C6 C10 N3 4(2) . . . . ? C5 C6 C10 N3 178.5(13) . . . . ? Pb3 O6 C11 O5 -141.3(19) 3_445 . . . ? Pb3 O6 C11 C12 40(3) 3_445 . . . ? Pb1 O5 C11 O6 -171.3(12) . . . . ? Pb3 O5 C11 O6 6.9(17) . . . . ? Pb1 O5 C11 C12 7.2(17) . . . . ? Pb3 O5 C11 C12 -174.5(10) . . . . ? C15 N4 C12 C13 0.8(15) . . . . ? Pb1 N4 C12 C13 175.8(9) . . . . ? C15 N4 C12 C11 -176.2(12) . . . . ? Pb1 N4 C12 C11 -1.2(16) . . . . ? O6 C11 C12 N4 174.6(15) . . . . ? O5 C11 C12 N4 -4(2) . . . . ? O6 C11 C12 C13 -2(3) . . . . ? O5 C11 C12 C13 179.9(14) . . . . ? C15 N5 C13 C12 -0.1(16) . . . . ? Pb2 N5 C13 C12 168.1(9) 4_455 . . . ? C15 N5 C13 C14 174.7(13) . . . . ? Pb2 N5 C13 C14 -17.2(17) 4_455 . . . ? N4 C12 C13 N5 -0.4(16) . . . . ? C11 C12 C13 N5 176.1(14) . . . . ? N4 C12 C13 C14 -174.0(15) . . . . ? C11 C12 C13 C14 3(3) . . . . ? Pb3 O7 C14 O8 -171(2) 3_445 . . . ? Pb3 O7 C14 C13 19(4) 3_445 . . . ? Pb4 O8 C14 O7 -22.5(16) 1_454 . . . ? Pb2 O8 C14 O7 -150.4(11) 4_455 . . . ? Pb4 O8 C14 C13 148.3(10) 1_454 . . . ? Pb2 O8 C14 C13 20.5(15) 4_455 . . . ? N5 C13 C14 O7 168.3(13) . . . . ? C12 C13 C14 O7 -19(3) . . . . ? N5 C13 C14 O8 -2.8(19) . . . . ? C12 C13 C14 O8 170.2(15) . . . . ? C13 N5 C15 N4 0.7(17) . . . . ? Pb2 N5 C15 N4 -164.7(10) 4_455 . . . ? C13 N5 C15 C16 -177.8(13) . . . . ? Pb2 N5 C15 C16 17(2) 4_455 . . . ? C12 N4 C15 N5 -0.9(17) . . . . ? Pb1 N4 C15 N5 -173.8(10) . . . . ? C12 N4 C15 C16 177.5(14) . . . . ? Pb1 N4 C15 C16 5(2) . . . . ? N5 C15 C16 C20 -102.8(18) . . . . ? N4 C15 C16 C20 78.9(19) . . . . ? N5 C15 C16 C17 74.3(19) . . . . ? N4 C15 C16 C17 -104.0(17) . . . . ? C20 C16 C17 C18 -2(2) . . . . ? C15 C16 C17 C18 -179.4(13) . . . . ? C16 C17 C18 C19 3(2) . . . . ? C20 N6 C19 C18 0(3) . . . . ? C17 C18 C19 N6 -2(3) . . . . ? C17 C16 C20 N6 0(2) . . . . ? C15 C16 C20 N6 177.4(14) . . . . ? C19 N6 C20 C16 1(2) . . . . ? Pb3 O9 C21 O10 -170.4(11) . . . . ? Pb3 O9 C21 C22 10(2) . . . . ? Pb4 O10 C21 O9 -8.7(19) . . . . ? Pb4 O10 C21 C22 171.2(10) . . . . ? C25 N7 C22 C23 0.3(17) . . . . ? Pb3 N7 C22 C23 170.8(9) . . . . ? C25 N7 C22 C21 179.6(13) . . . . ? Pb3 N7 C22 C21 -9.9(17) . . . . ? O9 C21 C22 N7 1(2) . . . . ? O10 C21 C22 N7 -178.9(14) . . . . ? O9 C21 C22 C23 -179.9(16) . . . . ? O10 C21 C22 C23 0(3) . . . . ? C25 N8 C23 C22 1.5(16) . . . . ? Pb4 N8 C23 C22 179.2(9) 1_455 . . . ? C25 N8 C23 C24 -178.5(14) . . . . ? Pb4 N8 C23 C24 -0.8(18) 1_455 . . . ? N7 C22 C23 N8 -1.2(18) . . . . ? C21 C22 C23 N8 179.6(15) . . . . ? N7 C22 C23 C24 178.8(16) . . . . ? C21 C22 C23 C24 0(3) . . . . ? Pb4 O12 C24 O11 -173.0(11) 1_455 . . . ? Pb4 O12 C24 C23 6(2) 1_455 . . . ? N8 C23 C24 O12 -3(2) . . . . ? C22 C23 C24 O12 176.8(16) . . . . ? N8 C23 C24 O11 175.8(15) . . . . ? C22 C23 C24 O11 -4(3) . . . . ? C23 N8 C25 N7 -1.4(17) . . . . ? Pb4 N8 C25 N7 -177.8(11) 1_455 . . . ? C23 N8 C25 C26 -179.5(13) . . . . ? Pb4 N8 C25 C26 4(3) 1_455 . . . ? C22 N7 C25 N8 0.7(18) . . . . ? Pb3 N7 C25 N8 -164.7(11) . . . . ? C22 N7 C25 C26 178.9(13) . . . . ? Pb3 N7 C25 C26 13(3) . . . . ? N8 C25 C26 C30 15(2) . . . . ? N7 C25 C26 C30 -162.6(14) . . . . ? N8 C25 C26 C27 -159.7(15) . . . . ? N7 C25 C26 C27 22(2) . . . . ? C30 C26 C27 C28 4(2) . . . . ? C25 C26 C27 C28 179.3(14) . . . . ? C26 C27 C28 C29 -6(2) . . . . ? C30 N9 C29 C28 -6(2) . . . . ? Pb3 N9 C29 C28 -175.7(12) 1_455 . . . ? C27 C28 C29 N9 8(2) . . . . ? C27 C26 C30 N9 -3(2) . . . . ? C25 C26 C30 N9 -177.8(14) . . . . ? C29 N9 C30 C26 4(2) . . . . ? Pb3 N9 C30 C26 172.8(11) 1_455 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.941 _refine_diff_density_min -2.240 _refine_diff_density_rms 0.300