# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 # SUBMISSION DETAILS _publ_contact_author_name 'Qing-Yan Liu' _publ_contact_author_address ; College of Chemistry and Chemical Engineering, Jiangxi Normal University, Nanchang, Jiangxi 330022, P. R. China ; _publ_contact_author_email qyliuchem@hotmail.com _publ_contact_author_fax +86-791-88120387 _publ_contact_author_phone +86-791-88120387 _publ_requested_coeditor_name ? _publ_author_name 'Qing-Yan Liu' ## Crystallographic Data for compound 1 data_Zn _database_code_depnum_ccdc_archive 'CCDC 887302' #TrackingRef '- Zn Pb NDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H54 N4 O18 Zn5' _chemical_formula_weight 1614.06 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.1492(14) _cell_length_b 15.1711(13) _cell_length_c 26.937(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6599.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2905 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 21.88 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 1.870 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6730 _exptl_absorpt_correction_T_max 0.8498 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 28407 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 23.76 _reflns_number_total 5029 _reflns_number_gt 3486 _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 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. The theta(max) is a bit low but the other parameters are in typical range and are reasonable. ; _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^)+(0.0453P)^2^+10.2224P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5029 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Zn1 Zn 0.09958(3) 0.46685(4) 0.11436(2) 0.03437(18) Uani 1 1 d . . . Zn2 Zn -0.09835(3) 0.49703(4) 0.10632(2) 0.03449(18) Uani 1 1 d . . . Zn3 Zn 0.0000 0.5000 0.0000 0.0242(2) Uani 1 2 d S . . N1 N -0.2088(2) 0.4355(2) 0.11480(14) 0.0308(9) Uani 1 1 d . . . N2 N -0.7820(3) 0.4209(3) 0.13147(16) 0.0418(11) Uani 1 1 d . . . O1 O -0.0731(2) 0.5217(2) 0.17731(12) 0.0384(9) Uani 1 1 d . . . O2 O 0.0629(2) 0.5442(3) 0.17029(13) 0.0497(10) Uani 1 1 d . . . O3 O -0.0670(3) 0.8471(3) 0.3523(2) 0.0935(19) Uani 1 1 d . . . O4 O 0.0393(3) 0.8019(3) 0.39164(19) 0.100(2) Uani 1 1 d . . . O5 O -0.1368(2) 0.6104(2) 0.08052(13) 0.0417(9) Uani 1 1 d . . . O6 O -0.0449(2) 0.6277(2) 0.01964(13) 0.0384(9) Uani 1 1 d . . . O7 O -0.3772(2) 0.9546(2) -0.00030(12) 0.0402(9) Uani 1 1 d . . . O8 O -0.3432(2) 0.9285(2) -0.07946(13) 0.0442(9) Uani 1 1 d . . . O9 O -0.00024(19) 0.4566(2) 0.07137(12) 0.0261(8) Uani 1 1 d . . . H9 H -0.009(3) 0.405(3) 0.0734(19) 0.039 Uiso 1 1 d . . . C1 C -0.0050(3) 0.5988(3) 0.24180(17) 0.0308(12) Uani 1 1 d . . . C2 C -0.0746(3) 0.6450(3) 0.25342(19) 0.0390(13) Uani 1 1 d . . . H2B H -0.1226 0.6364 0.2350 0.047 Uiso 1 1 calc R . . C3 C -0.0751(3) 0.7054(3) 0.2927(2) 0.0414(14) Uani 1 1 d . . . H3A H -0.1232 0.7369 0.2993 0.050 Uiso 1 1 calc R . . C4 C -0.0066(3) 0.7192(3) 0.32158(18) 0.0347(12) Uani 1 1 d . . . C5 C 0.0664(3) 0.6665(3) 0.31316(18) 0.0320(12) Uani 1 1 d . . . C6 C 0.1381(3) 0.6730(3) 0.34303(19) 0.0392(13) Uani 1 1 d . . . H6A H 0.1378 0.7108 0.3702 0.047 Uiso 1 1 calc R . . C7 C 0.2070(3) 0.6259(3) 0.3331(2) 0.0440(14) Uani 1 1 d . . . H7A H 0.2541 0.6333 0.3525 0.053 Uiso 1 1 calc R . . C8 C 0.2079(3) 0.5660(3) 0.29373(19) 0.0398(13) Uani 1 1 d . . . H8A H 0.2553 0.5331 0.2873 0.048 Uiso 1 1 calc R . . C9 C 0.1398(3) 0.5557(3) 0.26477(18) 0.0364(13) Uani 1 1 d . . . H9A H 0.1408 0.5143 0.2393 0.044 Uiso 1 1 calc R . . C10 C 0.0674(3) 0.6063(3) 0.27245(17) 0.0310(12) Uani 1 1 d . . . C11 C -0.0042(3) 0.5496(3) 0.19302(18) 0.0341(12) Uani 1 1 d . . . C12 C -0.0108(3) 0.7959(4) 0.3578(2) 0.0424(14) Uani 1 1 d . . . C13 C -0.1628(3) 0.7217(3) 0.02168(18) 0.0296(12) Uani 1 1 d . . . C14 C -0.2460(3) 0.7182(3) 0.03137(19) 0.0385(13) Uani 1 1 d . . . H14A H -0.2664 0.6721 0.0506 0.046 Uiso 1 1 calc R . . C15 C -0.3014(3) 0.7817(3) 0.01330(19) 0.0394(13) Uani 1 1 d . . . H15A H -0.3574 0.7777 0.0212 0.047 Uiso 1 1 calc R . . C16 C -0.2740(3) 0.8492(3) -0.01570(17) 0.0318(12) Uani 1 1 d . . . C17 C -0.1878(3) 0.8571(3) -0.02599(18) 0.0320(12) Uani 1 1 d . . . C18 C -0.1563(3) 0.9309(4) -0.0520(2) 0.0537(16) Uani 1 1 d . . . H18A H -0.1927 0.9728 -0.0647 0.064 Uiso 1 1 calc R . . C19 C -0.0739(4) 0.9413(4) -0.0587(3) 0.077(2) Uani 1 1 d . . . H19A H -0.0543 0.9899 -0.0761 0.092 Uiso 1 1 calc R . . C20 C -0.0179(3) 0.8801(4) -0.0398(3) 0.072(2) Uani 1 1 d . . . H20A H 0.0387 0.8883 -0.0444 0.086 Uiso 1 1 calc R . . C21 C -0.0458(3) 0.8084(4) -0.0147(2) 0.0474(15) Uani 1 1 d . . . H21A H -0.0078 0.7680 -0.0024 0.057 Uiso 1 1 calc R . . C22 C -0.1312(3) 0.7936(3) -0.00675(18) 0.0305(12) Uani 1 1 d . . . C23 C -0.1104(3) 0.6487(3) 0.04165(19) 0.0330(12) Uani 1 1 d . . . C24 C -0.3367(3) 0.9156(3) -0.0333(2) 0.0334(12) Uani 1 1 d . . . C25 C -0.2735(3) 0.4578(3) 0.08661(19) 0.0371(13) Uani 1 1 d . . . H25A H -0.2654 0.4976 0.0608 0.044 Uiso 1 1 calc R . . C26 C -0.3511(3) 0.4244(4) 0.0941(2) 0.0448(14) Uani 1 1 d . . . H26A H -0.3945 0.4423 0.0738 0.054 Uiso 1 1 calc R . . C27 C -0.3657(3) 0.3646(4) 0.1315(2) 0.0485(15) Uani 1 1 d . . . C28 C -0.2985(4) 0.3419(4) 0.1603(2) 0.0544(16) Uani 1 1 d . . . H28A H -0.3053 0.3016 0.1860 0.065 Uiso 1 1 calc R . . C29 C -0.2221(3) 0.3774(3) 0.1518(2) 0.0433(14) Uani 1 1 d . . . H29A H -0.1781 0.3611 0.1721 0.052 Uiso 1 1 calc R . . C30 C -0.4508(4) 0.3258(4) 0.1426(3) 0.0681(19) Uani 1 1 d . . . H30A H -0.4887 0.3412 0.1161 0.082 Uiso 1 1 calc R . . H30B H -0.4467 0.2621 0.1439 0.082 Uiso 1 1 calc R . . C31 C -0.4838(3) 0.3591(5) 0.1904(3) 0.071(2) Uani 1 1 d . . . H31A H -0.4913 0.4224 0.1882 0.086 Uiso 1 1 calc R . . H31B H -0.4437 0.3477 0.2165 0.086 Uiso 1 1 calc R . . C32 C -0.5667(4) 0.3161(5) 0.2047(3) 0.099(3) Uani 1 1 d . . . H32A H -0.5634 0.2533 0.1981 0.118 Uiso 1 1 calc R . . H32B H -0.5755 0.3236 0.2400 0.118 Uiso 1 1 calc R . . C33 C -0.7354(3) 0.4691(4) 0.1616(2) 0.0461(14) Uani 1 1 d . . . H33A H -0.7509 0.5272 0.1674 0.055 Uiso 1 1 calc R . . C34 C -0.6656(3) 0.4377(5) 0.1845(2) 0.0580(17) Uani 1 1 d . . . H34A H -0.6352 0.4744 0.2053 0.070 Uiso 1 1 calc R . . C35 C -0.6406(4) 0.3535(5) 0.1771(3) 0.0592(18) Uani 1 1 d . . . C36 C -0.6855(4) 0.3035(4) 0.1445(3) 0.074(2) Uani 1 1 d . . . H36A H -0.6690 0.2463 0.1371 0.089 Uiso 1 1 calc R . . C37 C -0.7559(4) 0.3385(4) 0.1225(2) 0.0614(18) Uani 1 1 d . . . H37A H -0.7860 0.3036 0.1006 0.074 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 Zn1 0.0266(3) 0.0502(4) 0.0263(3) 0.0032(3) -0.0037(3) -0.0037(3) Zn2 0.0228(3) 0.0561(4) 0.0245(3) -0.0013(3) 0.0011(2) -0.0013(3) Zn3 0.0227(4) 0.0296(4) 0.0205(4) 0.0003(3) 0.0007(3) 0.0017(3) N1 0.028(2) 0.032(2) 0.032(2) -0.002(2) 0.0016(19) 0.0029(18) N2 0.033(3) 0.048(3) 0.044(3) 0.002(2) 0.004(2) 0.000(2) O1 0.032(2) 0.054(2) 0.029(2) -0.0083(17) -0.0018(15) -0.0077(17) O2 0.038(2) 0.082(3) 0.029(2) -0.017(2) 0.0043(18) -0.010(2) O3 0.053(3) 0.090(4) 0.137(5) -0.080(3) -0.047(3) 0.037(3) O4 0.121(4) 0.084(4) 0.096(4) -0.058(3) -0.058(4) 0.051(3) O5 0.041(2) 0.050(2) 0.033(2) 0.0092(18) 0.0109(17) 0.0074(18) O6 0.038(2) 0.033(2) 0.045(2) 0.0032(17) 0.0151(18) 0.0085(16) O7 0.035(2) 0.052(2) 0.034(2) -0.0021(18) -0.0005(16) 0.0154(18) O8 0.043(2) 0.059(3) 0.031(2) 0.0085(18) 0.0024(17) 0.0129(18) O9 0.0285(18) 0.0253(18) 0.0244(18) 0.0026(15) -0.0002(14) 0.0010(16) C1 0.037(3) 0.035(3) 0.020(3) -0.003(2) 0.001(2) -0.005(2) C2 0.034(3) 0.045(3) 0.038(3) -0.011(3) -0.005(2) -0.006(2) C3 0.035(3) 0.045(3) 0.045(4) -0.013(3) -0.002(3) 0.001(2) C4 0.046(3) 0.032(3) 0.026(3) -0.006(2) 0.001(2) -0.005(2) C5 0.038(3) 0.028(3) 0.030(3) 0.003(2) -0.002(2) -0.001(2) C6 0.045(3) 0.040(3) 0.033(3) -0.004(2) -0.016(3) 0.001(3) C7 0.042(3) 0.047(4) 0.044(4) 0.002(3) -0.015(3) 0.001(3) C8 0.036(3) 0.042(3) 0.042(3) 0.001(3) -0.002(3) 0.006(2) C9 0.044(3) 0.036(3) 0.029(3) -0.006(2) -0.003(2) 0.006(2) C10 0.036(3) 0.031(3) 0.026(3) 0.001(2) 0.000(2) -0.003(2) C11 0.035(3) 0.041(3) 0.027(3) -0.002(2) 0.002(2) -0.006(2) C12 0.038(4) 0.044(3) 0.045(4) -0.014(3) -0.006(3) 0.004(3) C13 0.032(3) 0.026(3) 0.030(3) 0.000(2) 0.006(2) 0.010(2) C14 0.034(3) 0.038(3) 0.044(3) 0.011(3) 0.010(3) 0.002(2) C15 0.023(3) 0.046(3) 0.049(4) 0.005(3) 0.005(2) 0.003(2) C16 0.034(3) 0.034(3) 0.028(3) -0.001(2) 0.004(2) 0.007(2) C17 0.035(3) 0.030(3) 0.031(3) 0.001(2) 0.005(2) 0.003(2) C18 0.035(3) 0.054(4) 0.073(5) 0.022(3) 0.000(3) 0.005(3) C19 0.043(4) 0.068(5) 0.120(6) 0.050(4) 0.011(4) 0.000(3) C20 0.026(4) 0.063(5) 0.125(7) 0.036(4) 0.013(4) -0.001(3) C21 0.028(3) 0.042(3) 0.072(4) 0.013(3) 0.006(3) 0.006(3) C22 0.032(3) 0.029(3) 0.030(3) 0.000(2) 0.002(2) 0.002(2) C23 0.034(3) 0.028(3) 0.037(3) -0.007(2) 0.003(2) 0.001(2) C24 0.025(3) 0.036(3) 0.040(3) 0.008(3) -0.002(2) -0.002(2) C25 0.031(3) 0.043(3) 0.037(3) -0.005(3) 0.000(2) 0.000(2) C26 0.035(3) 0.049(4) 0.050(4) -0.005(3) -0.005(3) -0.001(3) C27 0.036(3) 0.051(4) 0.059(4) -0.006(3) 0.005(3) -0.002(3) C28 0.057(4) 0.043(4) 0.064(4) 0.013(3) 0.017(3) -0.005(3) C29 0.040(3) 0.043(4) 0.046(4) 0.005(3) -0.001(3) 0.002(3) C30 0.050(4) 0.068(5) 0.087(6) 0.001(4) 0.012(4) -0.013(3) C31 0.035(4) 0.091(5) 0.088(6) 0.027(4) -0.002(4) 0.007(3) C32 0.035(4) 0.131(7) 0.130(7) 0.080(6) 0.018(4) 0.024(4) C33 0.033(3) 0.049(4) 0.056(4) -0.005(3) -0.001(3) 0.001(3) C34 0.038(4) 0.078(5) 0.058(4) 0.001(3) -0.004(3) -0.002(3) C35 0.029(3) 0.065(5) 0.083(5) 0.029(4) 0.016(3) 0.001(3) C36 0.059(5) 0.043(4) 0.121(7) 0.019(4) 0.032(5) 0.019(4) C37 0.057(4) 0.050(4) 0.077(5) -0.013(4) 0.012(4) -0.002(3) _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 Zn1 O9 1.991(3) . ? Zn1 O2 2.000(4) . ? Zn1 O8 2.063(3) 4_565 ? Zn1 N2 2.088(4) 1_655 ? Zn1 O3 2.094(4) 3_545 ? Zn2 O9 1.942(3) . ? Zn2 O5 1.957(3) . ? Zn2 O1 1.991(3) . ? Zn2 N1 2.026(4) . ? Zn3 O9 2.032(3) 5_565 ? Zn3 O9 2.032(3) . ? Zn3 O7 2.099(3) 8 ? Zn3 O7 2.099(3) 4_565 ? Zn3 O6 2.135(3) 5_565 ? Zn3 O6 2.135(3) . ? N1 C25 1.335(6) . ? N1 C29 1.347(6) . ? N2 C33 1.325(7) . ? N2 C37 1.340(7) . ? N2 Zn1 2.088(4) 1_455 ? O1 C11 1.263(5) . ? O2 C11 1.247(5) . ? O3 C12 1.204(6) . ? O3 Zn1 2.094(4) 3 ? O4 C12 1.223(6) . ? O5 C23 1.271(6) . ? O6 C23 1.255(5) . ? O7 C24 1.253(6) . ? O7 Zn3 2.099(3) 4_465 ? O8 C24 1.263(6) . ? O8 Zn1 2.063(3) 4_465 ? O9 H9 0.80(5) . ? C1 C2 1.360(6) . ? C1 C10 1.437(6) . ? C1 C11 1.511(7) . ? C2 C3 1.399(7) . ? C2 H2B 0.9300 . ? C3 C4 1.369(7) . ? C3 H3A 0.9300 . ? C4 C5 1.442(7) . ? C4 C12 1.520(7) . ? C5 C6 1.414(6) . ? C5 C10 1.427(6) . ? C6 C7 1.350(7) . ? C6 H6A 0.9300 . ? C7 C8 1.395(7) . ? C7 H7A 0.9300 . ? C8 C9 1.357(7) . ? C8 H8A 0.9300 . ? C9 C10 1.414(6) . ? C9 H9A 0.9300 . ? C13 C14 1.370(6) . ? C13 C22 1.427(6) . ? C13 C23 1.494(6) . ? C14 C15 1.403(7) . ? C14 H14A 0.9300 . ? C15 C16 1.363(7) . ? C15 H15A 0.9300 . ? C16 C17 1.424(6) . ? C16 C24 1.504(6) . ? C17 C18 1.416(7) . ? C17 C22 1.425(6) . ? C18 C19 1.352(7) . ? C18 H18A 0.9300 . ? C19 C20 1.393(8) . ? C19 H19A 0.9300 . ? C20 C21 1.358(8) . ? C20 H20A 0.9300 . ? C21 C22 1.413(7) . ? C21 H21A 0.9300 . ? C25 C26 1.367(7) . ? C25 H25A 0.9300 . ? C26 C27 1.375(7) . ? C26 H26A 0.9300 . ? C27 C28 1.378(8) . ? C27 C30 1.525(8) . ? C28 C29 1.366(7) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 C31 1.483(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.538(8) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C35 1.515(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.372(7) . ? C33 H33A 0.9300 . ? C34 C35 1.354(8) . ? C34 H34A 0.9300 . ? C35 C36 1.370(9) . ? C36 C37 1.387(9) . ? C36 H36A 0.9300 . ? C37 H37A 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 O9 Zn1 O2 104.13(14) . . ? O9 Zn1 O8 99.10(13) . 4_565 ? O2 Zn1 O8 91.41(15) . 4_565 ? O9 Zn1 N2 147.58(16) . 1_655 ? O2 Zn1 N2 107.55(16) . 1_655 ? O8 Zn1 N2 86.97(15) 4_565 1_655 ? O9 Zn1 O3 88.75(15) . 3_545 ? O2 Zn1 O3 96.4(2) . 3_545 ? O8 Zn1 O3 167.27(17) 4_565 3_545 ? N2 Zn1 O3 81.11(17) 1_655 3_545 ? O9 Zn2 O5 111.38(14) . . ? O9 Zn2 O1 110.96(13) . . ? O5 Zn2 O1 103.92(15) . . ? O9 Zn2 N1 128.86(14) . . ? O5 Zn2 N1 99.52(15) . . ? O1 Zn2 N1 99.14(15) . . ? O9 Zn3 O9 180.00(18) 5_565 . ? O9 Zn3 O7 96.00(13) 5_565 8 ? O9 Zn3 O7 84.00(13) . 8 ? O9 Zn3 O7 84.00(13) 5_565 4_565 ? O9 Zn3 O7 96.00(13) . 4_565 ? O7 Zn3 O7 180.00(19) 8 4_565 ? O9 Zn3 O6 93.39(13) 5_565 5_565 ? O9 Zn3 O6 86.61(13) . 5_565 ? O7 Zn3 O6 91.27(13) 8 5_565 ? O7 Zn3 O6 88.73(13) 4_565 5_565 ? O9 Zn3 O6 86.61(13) 5_565 . ? O9 Zn3 O6 93.39(13) . . ? O7 Zn3 O6 88.73(13) 8 . ? O7 Zn3 O6 91.27(13) 4_565 . ? O6 Zn3 O6 180.00(18) 5_565 . ? C25 N1 C29 117.5(4) . . ? C25 N1 Zn2 120.6(3) . . ? C29 N1 Zn2 121.6(3) . . ? C33 N2 C37 116.5(5) . . ? C33 N2 Zn1 118.0(4) . 1_455 ? C37 N2 Zn1 124.0(4) . 1_455 ? C11 O1 Zn2 124.4(3) . . ? C11 O2 Zn1 131.8(3) . . ? C12 O3 Zn1 134.1(4) . 3 ? C23 O5 Zn2 126.0(3) . . ? C23 O6 Zn3 129.4(3) . . ? C24 O7 Zn3 130.6(3) . 4_465 ? C24 O8 Zn1 127.3(3) . 4_465 ? Zn2 O9 Zn1 110.72(15) . . ? Zn2 O9 Zn3 110.95(15) . . ? Zn1 O9 Zn3 121.54(16) . . ? Zn2 O9 H9 98(4) . . ? Zn1 O9 H9 100(4) . . ? Zn3 O9 H9 112(4) . . ? C2 C1 C10 120.0(4) . . ? C2 C1 C11 117.5(4) . . ? C10 C1 C11 122.1(4) . . ? C1 C2 C3 121.1(5) . . ? C1 C2 H2B 119.5 . . ? C3 C2 H2B 119.5 . . ? C4 C3 C2 121.7(5) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 119.1(4) . . ? C3 C4 C12 116.5(5) . . ? C5 C4 C12 124.2(4) . . ? C6 C5 C10 118.2(5) . . ? C6 C5 C4 122.8(5) . . ? C10 C5 C4 119.1(4) . . ? C7 C6 C5 121.7(5) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C6 C7 C8 120.3(5) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C9 C8 C7 120.3(5) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C8 C9 C10 121.5(5) . . ? C8 C9 H9A 119.2 . . ? C10 C9 H9A 119.2 . . ? C9 C10 C5 118.0(4) . . ? C9 C10 C1 123.1(4) . . ? C5 C10 C1 118.8(4) . . ? O2 C11 O1 125.3(5) . . ? O2 C11 C1 117.8(4) . . ? O1 C11 C1 116.7(4) . . ? O3 C12 O4 122.9(5) . . ? O3 C12 C4 116.7(5) . . ? O4 C12 C4 120.4(5) . . ? C14 C13 C22 118.9(4) . . ? C14 C13 C23 117.2(4) . . ? C22 C13 C23 123.9(4) . . ? C13 C14 C15 122.2(5) . . ? C13 C14 H14A 118.9 . . ? C15 C14 H14A 118.9 . . ? C16 C15 C14 120.5(5) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 119.5(4) . . ? C15 C16 C24 117.7(4) . . ? C17 C16 C24 122.7(4) . . ? C18 C17 C16 120.9(5) . . ? C18 C17 C22 118.9(5) . . ? C16 C17 C22 120.0(4) . . ? C19 C18 C17 120.8(5) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C18 C19 C20 120.9(6) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C21 C20 C19 120.0(5) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C22 121.8(5) . . ? C20 C21 H21A 119.1 . . ? C22 C21 H21A 119.1 . . ? C21 C22 C17 117.6(5) . . ? C21 C22 C13 123.5(4) . . ? C17 C22 C13 118.8(4) . . ? O6 C23 O5 123.7(5) . . ? O6 C23 C13 119.8(5) . . ? O5 C23 C13 116.5(4) . . ? O7 C24 O8 125.5(5) . . ? O7 C24 C16 116.4(4) . . ? O8 C24 C16 118.1(5) . . ? N1 C25 C26 122.7(5) . . ? N1 C25 H25A 118.7 . . ? C26 C25 H25A 118.7 . . ? C25 C26 C27 120.6(5) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C26 C27 C28 116.3(5) . . ? C26 C27 C30 123.6(5) . . ? C28 C27 C30 120.1(6) . . ? C29 C28 C27 121.2(6) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? N1 C29 C28 121.7(5) . . ? N1 C29 H29A 119.1 . . ? C28 C29 H29A 119.1 . . ? C31 C30 C27 111.3(5) . . ? C31 C30 H30A 109.4 . . ? C27 C30 H30A 109.4 . . ? C31 C30 H30B 109.4 . . ? C27 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? C30 C31 C32 112.7(6) . . ? C30 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? C30 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C35 C32 C31 113.8(5) . . ? C35 C32 H32A 108.8 . . ? C31 C32 H32A 108.8 . . ? C35 C32 H32B 108.8 . . ? C31 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? N2 C33 C34 123.4(6) . . ? N2 C33 H33A 118.3 . . ? C34 C33 H33A 118.3 . . ? C35 C34 C33 120.4(6) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C36 117.3(6) . . ? C34 C35 C32 121.1(7) . . ? C36 C35 C32 121.6(7) . . ? C35 C36 C37 119.8(6) . . ? C35 C36 H36A 120.1 . . ? C37 C36 H36A 120.1 . . ? N2 C37 C36 122.5(6) . . ? N2 C37 H37A 118.8 . . ? C36 C37 H37A 118.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9 O4 0.80(5) 1.89(5) 2.626(5) 153(5) 3_545 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.76 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.923 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.080 #===END OF 1 ## Crystallographic Data for compound 2 data_jyl126_0m _database_code_depnum_ccdc_archive 'CCDC 887303' #TrackingRef '- Zn Pb NDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H38 N2 O17 Pb5' _chemical_formula_weight 2106.88 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 C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.2764(6) _cell_length_b 12.1038(3) _cell_length_c 30.7311(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.3770(10) _cell_angle_gamma 90.00 _cell_volume 11192.0(4) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8258 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.25 _exptl_crystal_description bolck _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7712 _exptl_absorpt_coefficient_mu 15.069 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0796 _exptl_absorpt_correction_T_max 0.2650 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 49680 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.65 _reflns_number_total 12994 _reflns_number_gt 9611 _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 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. The O8, O15, and C56 have large thermal displacement parameters resulted from their freedom of libration. We tried to model some atoms (O8, O15, and C56) as disordered due to the large ADPs . However, this gave rise to some unreasonable bond distances (for example, the abnormal C--O = 1.56 A% is obtained using a disordered model). Collecting the data at lower temperature may improve the quality of the data. However, we were not able to obtain data at low temperature. ; _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^)+(0.0253P)^2^+10.6517P] 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 SHELXL _refine_ls_extinction_coef 0.000026(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12994 _refine_ls_number_parameters 767 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0674 _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 0.095818(8) -0.00541(2) 0.246779(9) 0.02844(7) Uani 1 1 d . . . Pb2 Pb 0.093968(9) -0.30162(2) 0.258833(10) 0.03536(8) Uani 1 1 d . . . Pb3 Pb 0.004465(8) -0.16029(2) 0.308609(8) 0.02369(7) Uani 1 1 d . . . Pb4 Pb 0.110176(9) 0.05945(2) 0.387724(9) 0.03375(8) Uani 1 1 d . . . Pb5 Pb 0.243092(10) 0.17048(3) 0.430382(9) 0.03712(8) Uani 1 1 d . . . N1 N 0.2679(3) -0.0247(6) 0.4570(2) 0.057(2) Uani 1 1 d . . . N2 N 0.5342(2) -0.4089(7) 0.4239(2) 0.059(2) Uani 1 1 d . . . C1 C 0.2153(2) -0.1906(7) 0.2190(2) 0.0400(19) Uani 1 1 d . . . C2 C 0.2026(2) -0.2800(7) 0.1933(2) 0.042(2) Uani 1 1 d . . . H2A H 0.1725 -0.2961 0.1871 0.051 Uiso 1 1 calc R . . C3 C 0.2340(2) -0.3478(7) 0.1760(2) 0.042(2) Uani 1 1 d . . . H3A H 0.2240 -0.4063 0.1579 0.051 Uiso 1 1 calc R . . C4 C 0.2790(2) -0.3307(7) 0.1850(2) 0.043(2) Uani 1 1 d . . . C5 C 0.2936(2) -0.2397(8) 0.2139(2) 0.048(2) Uani 1 1 d . . . C6 C 0.3394(3) -0.2144(10) 0.2245(3) 0.072(3) Uani 1 1 d . . . H6A H 0.3608 -0.2571 0.2129 0.086 Uiso 1 1 calc R . . C7 C 0.3519(3) -0.1309(11) 0.2507(3) 0.079(4) Uani 1 1 d . . . H7A H 0.3820 -0.1179 0.2582 0.095 Uiso 1 1 calc R . . C8 C 0.3210(3) -0.0618(11) 0.2675(3) 0.083(4) Uani 1 1 d . . . H8A H 0.3306 -0.0029 0.2856 0.099 Uiso 1 1 calc R . . C9 C 0.2764(3) -0.0812(9) 0.2571(3) 0.061(3) Uani 1 1 d . . . H9A H 0.2558 -0.0350 0.2682 0.073 Uiso 1 1 calc R . . C10 C 0.2615(2) -0.1704(8) 0.2298(2) 0.046(2) Uani 1 1 d . . . C11 C 0.1804(3) -0.1114(8) 0.2321(3) 0.0416(19) Uani 1 1 d . . . C12 C 0.3095(2) -0.4038(8) 0.1628(2) 0.048(2) Uani 1 1 d . . . C13 C 0.1158(2) -0.1631(6) 0.1134(2) 0.0317(16) Uani 1 1 d . . . C14 C 0.1462(3) -0.0854(7) 0.1052(3) 0.051(2) Uani 1 1 d . . . H14A H 0.1530 -0.0289 0.1253 0.061 Uiso 1 1 calc R . . C15 C 0.1675(3) -0.0891(8) 0.0668(3) 0.060(3) Uani 1 1 d . . . H15A H 0.1895 -0.0378 0.0628 0.072 Uiso 1 1 calc R . . C16 C 0.1562(3) -0.1670(8) 0.0355(2) 0.049(2) Uani 1 1 d . . . C17 C 0.1239(3) -0.2481(7) 0.0420(2) 0.0422(19) Uani 1 1 d . . . C18 C 0.1123(4) -0.3313(9) 0.0113(3) 0.070(3) Uani 1 1 d . . . H18A H 0.1265 -0.3346 -0.0140 0.084 Uiso 1 1 calc R . . C19 C 0.0809(5) -0.4072(10) 0.0178(3) 0.109(5) Uani 1 1 d . . . H19A H 0.0737 -0.4621 -0.0030 0.131 Uiso 1 1 calc R . . C20 C 0.0589(4) -0.4031(10) 0.0559(3) 0.096(4) Uani 1 1 d . . . H20A H 0.0371 -0.4548 0.0603 0.115 Uiso 1 1 calc R . . C21 C 0.0699(3) -0.3233(7) 0.0859(3) 0.057(3) Uani 1 1 d . . . H21A H 0.0547 -0.3200 0.1106 0.068 Uiso 1 1 calc R . . C22 C 0.1032(2) -0.2456(6) 0.0812(2) 0.0340(17) Uani 1 1 d . . . C23 C 0.0977(2) -0.1598(6) 0.1568(2) 0.0292(16) Uani 1 1 d . . . C24 C 0.1811(4) -0.1662(12) -0.0043(3) 0.079(4) Uani 1 1 d . . . C25 C 0.0114(2) 0.2211(5) 0.3161(2) 0.0247(15) Uani 1 1 d . . . C26 C 0.0458(2) 0.2846(5) 0.3051(3) 0.0360(18) Uani 1 1 d . . . H26A H 0.0721 0.2511 0.2989 0.043 Uiso 1 1 calc R . . C27 C 0.0419(2) 0.4002(6) 0.3031(3) 0.0373(18) Uani 1 1 d . . . H27A H 0.0655 0.4420 0.2953 0.045 Uiso 1 1 calc R . . C28 C 0.0047(2) 0.4513(5) 0.3121(2) 0.0282(15) Uani 1 1 d . . . C29 C -0.0309(2) 0.3894(5) 0.3270(2) 0.0253(15) Uani 1 1 d . . . C30 C -0.0683(3) 0.4404(7) 0.3424(3) 0.044(2) Uani 1 1 d . . . H30A H -0.0708 0.5170 0.3424 0.053 Uiso 1 1 calc R . . C31 C -0.1008(3) 0.3762(8) 0.3575(3) 0.057(2) Uani 1 1 d . . . H31A H -0.1253 0.4102 0.3675 0.069 Uiso 1 1 calc R . . C32 C -0.0981(3) 0.2623(8) 0.3579(3) 0.059(3) Uani 1 1 d . . . H32A H -0.1206 0.2205 0.3681 0.070 Uiso 1 1 calc R . . C33 C -0.0624(3) 0.2114(7) 0.3434(2) 0.0406(19) Uani 1 1 d . . . H33A H -0.0611 0.1346 0.3434 0.049 Uiso 1 1 calc R . . C34 C -0.0274(2) 0.2724(5) 0.3283(2) 0.0248(15) Uani 1 1 d . . . C35 C 0.0169(2) 0.0996(5) 0.3123(2) 0.0256(15) Uani 1 1 d . . . C36 C 0.0036(3) 0.5747(7) 0.3034(3) 0.050(2) Uani 1 1 d . . . C37 C 0.1408(3) 0.4476(9) 0.3890(3) 0.062(3) Uani 1 1 d . . . C38 C 0.1020(3) 0.4889(8) 0.4008(3) 0.062(3) Uani 1 1 d . . . H38A H 0.0817 0.4411 0.4115 0.074 Uiso 1 1 calc R . . C39 C 0.0919(3) 0.6021(9) 0.3972(3) 0.065(3) Uani 1 1 d . . . H39A H 0.0660 0.6280 0.4074 0.078 Uiso 1 1 calc R . . C40 C 0.1192(3) 0.6752(8) 0.3791(3) 0.055(3) Uani 1 1 d . . . C41 C 0.1596(3) 0.6354(8) 0.3664(2) 0.051(2) Uani 1 1 d . . . C42 C 0.1896(3) 0.7100(8) 0.3489(3) 0.053(2) Uani 1 1 d . . . H42A H 0.1824 0.7845 0.3460 0.063 Uiso 1 1 calc R . . C43 C 0.2290(3) 0.6730(10) 0.3363(3) 0.069(3) Uani 1 1 d . . . H43A H 0.2477 0.7207 0.3233 0.083 Uiso 1 1 calc R . . C44 C 0.2407(3) 0.5606(10) 0.3434(3) 0.075(3) Uani 1 1 d . . . H44A H 0.2683 0.5362 0.3367 0.090 Uiso 1 1 calc R . . C45 C 0.2128(3) 0.4879(10) 0.3596(3) 0.069(3) Uani 1 1 d . . . H45A H 0.2205 0.4136 0.3621 0.083 Uiso 1 1 calc R . . C46 C 0.1720(3) 0.5242(8) 0.3726(3) 0.054(2) Uani 1 1 d . . . C47 C 0.1479(5) 0.3220(11) 0.3941(4) 0.084(4) Uani 1 1 d . . . C48 C 0.1047(3) 0.7925(8) 0.3699(3) 0.054(2) Uani 1 1 d . . . C49 C 0.2896(4) -0.0321(8) 0.4961(3) 0.077(3) Uani 1 1 d . . . H49A H 0.2895 0.0281 0.5148 0.093 Uiso 1 1 calc R . . C50 C 0.3127(3) -0.1253(8) 0.5106(3) 0.062(3) Uani 1 1 d . . . H50A H 0.3274 -0.1261 0.5388 0.075 Uiso 1 1 calc R . . C51 C 0.3147(3) -0.2164(7) 0.4849(3) 0.049(2) Uani 1 1 d . . . C52 C 0.2900(4) -0.2090(9) 0.4447(3) 0.077(3) Uani 1 1 d . . . H52A H 0.2886 -0.2690 0.4256 0.093 Uiso 1 1 calc R . . C53 C 0.2676(4) -0.1138(9) 0.4325(3) 0.078(3) Uani 1 1 d . . . H53A H 0.2512 -0.1120 0.4051 0.093 Uiso 1 1 calc R . . C54 C 0.3415(3) -0.3160(7) 0.4997(3) 0.060(3) Uani 1 1 d . . . H54A H 0.3243 -0.3824 0.4925 0.073 Uiso 1 1 calc R . . H54B H 0.3490 -0.3136 0.5312 0.073 Uiso 1 1 calc R . . C55 C 0.3850(4) -0.3188(15) 0.4767(4) 0.141(7) Uani 1 1 d . . . H55A H 0.3767 -0.3451 0.4471 0.169 Uiso 1 1 calc R . . H55B H 0.3946 -0.2428 0.4742 0.169 Uiso 1 1 calc R . . C56 C 0.4189(4) -0.3741(19) 0.4921(5) 0.171(9) Uani 1 1 d . . . H56A H 0.4086 -0.4480 0.4979 0.205 Uiso 1 1 calc R . . H56B H 0.4294 -0.3418 0.5203 0.205 Uiso 1 1 calc R . . C57 C 0.5261(4) -0.3139(10) 0.4411(4) 0.087(4) Uani 1 1 d . . . H57A H 0.5454 -0.2553 0.4386 0.104 Uiso 1 1 calc R . . C58 C 0.4887(5) -0.2985(13) 0.4632(4) 0.119(5) Uani 1 1 d . . . H58A H 0.4834 -0.2303 0.4756 0.142 Uiso 1 1 calc R . . C59 C 0.4590(3) -0.3863(15) 0.4667(3) 0.096(5) Uani 1 1 d . . . C60 C 0.4681(4) -0.4812(14) 0.4473(4) 0.109(5) Uani 1 1 d . . . H60A H 0.4491 -0.5414 0.4479 0.131 Uiso 1 1 calc R . . C61 C 0.5053(4) -0.4890(11) 0.4267(3) 0.083(3) Uani 1 1 d . . . H61A H 0.5108 -0.5560 0.4135 0.099 Uiso 1 1 calc R . . O1 O 0.04794(13) -0.1571(3) 0.25225(14) 0.0209(9) Uani 1 1 d . . . O2 O 0.15005(16) -0.1525(4) 0.25266(16) 0.0386(13) Uani 1 1 d . . . O3 O 0.1816(2) -0.0139(6) 0.2211(2) 0.072(2) Uani 1 1 d . . . O4 O 0.34846(18) -0.4219(6) 0.18008(17) 0.0609(18) Uani 1 1 d . . . O5 O 0.29541(17) -0.4442(5) 0.12595(17) 0.0531(16) Uani 1 1 d . . . O6 O 0.08841(19) -0.0651(4) 0.17077(16) 0.0460(14) Uani 1 1 d . . . O7 O 0.09474(17) -0.2484(4) 0.17657(15) 0.0395(12) Uani 1 1 d . . . O8 O 0.2076(3) -0.2436(15) -0.0071(3) 0.225(9) Uani 1 1 d . . . O9 O 0.1762(4) -0.1035(6) -0.0320(2) 0.118(4) Uani 1 1 d . . . O10 O -0.01461(18) 0.0428(4) 0.29626(18) 0.0471(15) Uani 1 1 d . . . O11 O 0.05435(16) 0.0570(4) 0.32375(16) 0.0363(12) Uani 1 1 d . . . O12 O 0.0384(3) 0.6290(4) 0.3088(2) 0.074(2) Uani 1 1 d . . . O13 O -0.0339(3) 0.6166(6) 0.2930(3) 0.106(3) Uani 1 1 d . . . O14 O 0.1144(3) 0.2634(7) 0.3942(3) 0.095(3) Uani 1 1 d . . . O15 O 0.1864(3) 0.2928(9) 0.3989(4) 0.186(6) Uani 1 1 d . . . O16 O 0.0933(3) 0.8485(6) 0.4002(2) 0.083(2) Uani 1 1 d . . . O17 O 0.10143(19) 0.8246(5) 0.33067(19) 0.0613(18) 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 0.02248(14) 0.02815(14) 0.03513(15) -0.00309(11) 0.00509(11) -0.00451(11) Pb2 0.03220(16) 0.02656(14) 0.05026(18) 0.01138(13) 0.01761(13) 0.01228(12) Pb3 0.02301(14) 0.02391(12) 0.02516(13) 0.00183(10) 0.00717(10) 0.00099(10) Pb4 0.02600(15) 0.04788(18) 0.02865(15) 0.00057(13) 0.00879(11) -0.00424(13) Pb5 0.03481(17) 0.05086(18) 0.02678(15) 0.00642(13) 0.00830(12) 0.00112(13) N1 0.066(5) 0.053(5) 0.049(5) 0.001(4) -0.004(4) 0.002(4) N2 0.044(5) 0.082(6) 0.054(5) -0.002(4) 0.016(4) -0.008(4) C1 0.024(4) 0.066(5) 0.031(4) -0.002(4) 0.012(3) 0.006(4) C2 0.022(4) 0.071(6) 0.034(4) 0.005(4) 0.005(3) 0.009(4) C3 0.021(4) 0.081(6) 0.024(4) 0.001(4) -0.002(3) 0.014(4) C4 0.020(4) 0.090(6) 0.019(4) 0.001(4) 0.004(3) 0.013(4) C5 0.022(4) 0.100(7) 0.024(4) 0.005(4) 0.007(3) 0.011(4) C6 0.025(5) 0.144(10) 0.046(6) -0.021(6) 0.002(4) 0.009(6) C7 0.019(5) 0.164(11) 0.056(6) -0.018(7) 0.006(4) -0.005(6) C8 0.040(6) 0.151(11) 0.060(7) -0.036(7) 0.019(5) -0.018(7) C9 0.030(5) 0.103(8) 0.049(5) -0.012(5) 0.007(4) 0.006(5) C10 0.021(4) 0.090(7) 0.028(4) -0.013(4) 0.006(3) 0.001(4) C11 0.025(4) 0.066(6) 0.035(4) -0.011(4) 0.010(3) 0.004(4) C12 0.024(4) 0.096(7) 0.026(4) 0.008(4) 0.012(3) 0.026(4) C13 0.030(4) 0.036(4) 0.030(4) 0.005(3) 0.008(3) 0.003(3) C14 0.057(6) 0.056(5) 0.039(5) -0.002(4) 0.002(4) -0.013(5) C15 0.057(6) 0.072(6) 0.053(6) 0.019(5) 0.012(5) -0.016(5) C16 0.046(5) 0.080(6) 0.020(4) 0.017(4) 0.006(4) 0.008(5) C17 0.043(5) 0.055(5) 0.030(4) 0.007(4) 0.014(4) 0.007(4) C18 0.099(9) 0.079(7) 0.036(5) -0.013(5) 0.029(5) -0.008(6) C19 0.213(16) 0.075(8) 0.043(6) -0.019(6) 0.030(8) -0.053(9) C20 0.153(12) 0.088(8) 0.052(6) -0.013(6) 0.033(7) -0.064(8) C21 0.082(7) 0.058(6) 0.034(5) -0.009(4) 0.021(5) -0.026(5) C22 0.040(5) 0.040(4) 0.022(4) 0.009(3) 0.007(3) 0.009(4) C23 0.025(4) 0.040(4) 0.022(4) 0.001(3) 0.002(3) 0.002(3) C24 0.054(7) 0.162(12) 0.024(5) 0.005(6) 0.014(5) -0.018(7) C25 0.021(4) 0.018(3) 0.035(4) -0.001(3) 0.005(3) 0.000(3) C26 0.024(4) 0.025(4) 0.061(5) -0.005(4) 0.014(4) 0.000(3) C27 0.028(4) 0.029(4) 0.057(5) 0.003(4) 0.016(4) -0.004(3) C28 0.036(4) 0.022(3) 0.028(4) 0.006(3) 0.009(3) 0.003(3) C29 0.023(4) 0.027(3) 0.027(4) 0.004(3) 0.007(3) 0.006(3) C30 0.045(5) 0.042(5) 0.045(5) 0.006(4) 0.008(4) 0.012(4) C31 0.039(5) 0.072(7) 0.065(6) 0.006(5) 0.021(5) 0.020(5) C32 0.036(5) 0.078(7) 0.066(6) 0.014(5) 0.023(5) -0.013(5) C33 0.038(5) 0.046(5) 0.040(5) 0.004(4) 0.012(4) -0.016(4) C34 0.023(4) 0.028(3) 0.024(3) 0.003(3) 0.004(3) -0.007(3) C35 0.035(4) 0.018(3) 0.025(3) -0.001(3) 0.004(3) -0.002(3) C36 0.074(7) 0.031(4) 0.051(5) 0.014(4) 0.036(5) 0.025(5) C37 0.065(7) 0.090(7) 0.032(5) 0.018(5) 0.011(4) 0.032(6) C38 0.060(6) 0.077(7) 0.050(6) 0.028(5) 0.018(5) 0.032(5) C39 0.058(6) 0.098(8) 0.043(5) 0.028(5) 0.019(5) 0.044(6) C40 0.060(6) 0.076(6) 0.030(4) 0.014(4) 0.008(4) 0.040(5) C41 0.045(5) 0.082(7) 0.024(4) 0.015(4) 0.000(4) 0.020(5) C42 0.040(5) 0.069(6) 0.047(5) -0.006(5) -0.004(4) 0.029(5) C43 0.046(6) 0.109(9) 0.054(6) 0.008(6) 0.010(5) 0.012(6) C44 0.049(6) 0.113(10) 0.066(7) 0.005(7) 0.015(5) 0.040(6) C45 0.067(7) 0.096(8) 0.047(6) 0.016(6) 0.018(5) 0.024(6) C46 0.040(5) 0.088(7) 0.035(5) 0.012(5) 0.009(4) 0.032(5) C47 0.090(10) 0.109(10) 0.059(7) 0.056(7) 0.038(7) 0.058(8) C48 0.047(5) 0.079(7) 0.036(5) 0.020(5) 0.008(4) 0.034(5) C49 0.124(10) 0.055(6) 0.046(6) -0.011(5) -0.019(6) 0.028(6) C50 0.075(7) 0.071(6) 0.035(5) -0.007(5) -0.017(5) 0.009(5) C51 0.042(5) 0.062(6) 0.044(5) -0.003(4) 0.007(4) 0.015(4) C52 0.095(8) 0.072(7) 0.056(6) -0.031(5) -0.024(6) 0.033(6) C53 0.096(9) 0.082(8) 0.048(6) -0.004(6) -0.027(6) 0.017(7) C54 0.050(6) 0.063(6) 0.068(6) -0.014(5) 0.000(5) 0.020(5) C55 0.086(10) 0.27(2) 0.069(8) -0.006(10) 0.020(7) 0.116(12) C56 0.052(8) 0.38(3) 0.082(10) -0.034(14) 0.032(8) 0.013(13) C57 0.064(8) 0.101(9) 0.102(10) -0.022(8) 0.042(7) -0.010(7) C58 0.096(11) 0.163(14) 0.106(11) -0.051(10) 0.054(9) 0.019(10) C59 0.031(6) 0.212(16) 0.046(6) -0.020(8) 0.012(5) -0.018(8) C60 0.076(9) 0.200(16) 0.057(7) -0.037(9) 0.025(6) -0.068(9) C61 0.066(8) 0.127(10) 0.058(7) -0.012(7) 0.016(6) -0.031(7) O1 0.018(2) 0.020(2) 0.025(2) 0.0012(18) 0.0043(18) 0.0023(18) O2 0.022(3) 0.059(3) 0.037(3) 0.004(3) 0.014(2) 0.006(2) O3 0.049(4) 0.071(5) 0.104(6) 0.007(4) 0.047(4) 0.002(3) O4 0.035(3) 0.120(5) 0.029(3) 0.011(3) 0.009(2) 0.034(3) O5 0.041(3) 0.091(5) 0.027(3) 0.001(3) 0.002(2) 0.032(3) O6 0.068(4) 0.040(3) 0.031(3) -0.004(2) 0.009(3) 0.016(3) O7 0.051(3) 0.043(3) 0.027(3) 0.003(2) 0.014(2) -0.005(3) O8 0.108(8) 0.51(2) 0.067(6) 0.131(10) 0.070(6) 0.162(12) O9 0.273(12) 0.056(4) 0.032(4) -0.002(3) 0.052(5) -0.034(6) O10 0.047(3) 0.024(3) 0.065(4) -0.009(3) -0.014(3) -0.007(2) O11 0.034(3) 0.027(3) 0.046(3) -0.008(2) -0.002(2) 0.008(2) O12 0.124(6) 0.024(3) 0.084(5) -0.004(3) 0.057(5) -0.020(4) O13 0.111(7) 0.086(5) 0.134(7) 0.072(5) 0.072(6) 0.067(5) O14 0.132(8) 0.077(6) 0.075(6) 0.007(4) 0.010(6) 0.035(5) O15 0.119(8) 0.176(10) 0.279(15) 0.180(10) 0.097(9) 0.102(8) O16 0.118(6) 0.087(5) 0.047(4) 0.012(4) 0.018(4) 0.058(5) O17 0.045(4) 0.092(5) 0.049(4) 0.027(3) 0.014(3) 0.032(3) _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 O1 2.357(4) . ? Pb1 O2 2.415(5) . ? Pb1 O6 2.432(5) . ? Pb1 O10 2.723(5) 2 ? Pb1 O3 2.798(6) . ? Pb1 O4 2.842(5) 4 ? Pb1 O11 2.899(5) . ? Pb1 Pb2 3.6054(4) . ? Pb2 O1 2.232(4) . ? Pb2 O13 2.487(8) 2_545 ? Pb2 O2 2.499(5) . ? Pb2 O12 2.541(7) 1_545 ? Pb2 O7 2.611(5) . ? Pb2 O17 2.674(6) 1_545 ? Pb2 Pb3 3.6784(4) . ? Pb3 O1 2.289(4) . ? Pb3 O1 2.315(4) 2 ? Pb3 O10 2.544(5) . ? Pb3 O12 2.750(6) 1_545 ? Pb3 O17 2.944(6) 1_545 ? Pb3 O13 2.957(9) 1_545 ? Pb3 Pb3 3.5823(5) 2 ? Pb4 O11 2.446(5) . ? Pb4 O14 2.478(8) . ? Pb4 O4 2.558(5) 4 ? Pb4 O16 2.640(7) 1_545 ? Pb4 N2 2.691(8) 3_455 ? Pb4 O5 2.936(5) 4 ? Pb5 O15 2.389(8) . ? Pb5 O5 2.415(5) 4 ? Pb5 O8 2.467(9) 6_556 ? Pb5 O9 2.571(10) 6_556 ? Pb5 N1 2.584(7) . ? Pb5 O8 2.845(8) 4 ? N1 C49 1.307(10) . ? N1 C53 1.315(12) . ? N2 C57 1.300(13) . ? N2 C61 1.315(12) . ? N2 Pb4 2.691(8) 3_545 ? C1 C2 1.370(11) . ? C1 C10 1.421(10) . ? C1 C11 1.516(11) . ? C2 C3 1.404(10) . ? C2 H2A 0.9300 . ? C3 C4 1.377(10) . ? C3 H3A 0.9300 . ? C4 C5 1.453(11) . ? C4 C12 1.495(11) . ? C5 C10 1.411(11) . ? C5 C6 1.423(11) . ? C6 C7 1.321(14) . ? C6 H6A 0.9300 . ? C7 C8 1.395(14) . ? C7 H7A 0.9300 . ? C8 C9 1.373(11) . ? C8 H8A 0.9300 . ? C9 C10 1.410(12) . ? C9 H9A 0.9300 . ? C11 O3 1.229(10) . ? C11 O2 1.272(9) . ? C12 O4 1.258(8) . ? C12 O5 1.264(9) . ? C13 C14 1.358(10) . ? C13 C22 1.427(10) . ? C13 C23 1.497(10) . ? C14 C15 1.406(12) . ? C14 H14A 0.9300 . ? C15 C16 1.365(12) . ? C15 H15A 0.9300 . ? C16 C17 1.416(11) . ? C16 C24 1.505(12) . ? C17 C18 1.398(12) . ? C17 C22 1.420(10) . ? C18 C19 1.353(14) . ? C18 H18A 0.9300 . ? C19 C20 1.411(15) . ? C19 H19A 0.9300 . ? C20 C21 1.352(12) . ? C20 H20A 0.9300 . ? C21 C22 1.398(11) . ? C21 H21A 0.9300 . ? C23 O7 1.241(8) . ? C23 O6 1.267(8) . ? C24 O9 1.138(12) . ? C24 O8 1.243(16) . ? C25 C26 1.366(9) . ? C25 C34 1.417(9) . ? C25 C35 1.486(8) . ? C26 C27 1.404(9) . ? C26 H26A 0.9300 . ? C27 C28 1.340(9) . ? C27 H27A 0.9300 . ? C28 C29 1.430(9) . ? C28 C36 1.516(10) . ? C29 C30 1.417(10) . ? C29 C34 1.421(9) . ? C30 C31 1.374(12) . ? C30 H30A 0.9300 . ? C31 C32 1.381(12) . ? C31 H31A 0.9300 . ? C32 C33 1.362(11) . ? C32 H32A 0.9300 . ? C33 C34 1.410(9) . ? C33 H33A 0.9300 . ? C35 O10 1.234(7) . ? C35 O11 1.259(8) . ? C36 O12 1.237(11) . ? C36 O13 1.253(10) . ? C37 C38 1.363(12) . ? C37 C46 1.454(13) . ? C37 C47 1.542(15) . ? C38 C39 1.405(13) . ? C38 H38A 0.9300 . ? C39 C40 1.370(13) . ? C39 H39A 0.9300 . ? C40 C41 1.409(12) . ? C40 C48 1.504(12) . ? C41 C46 1.405(12) . ? C41 C42 1.430(13) . ? C42 C43 1.368(12) . ? C42 H42A 0.9300 . ? C43 C44 1.417(14) . ? C43 H43A 0.9300 . ? C44 C45 1.353(14) . ? C44 H44A 0.9300 . ? C45 C46 1.410(12) . ? C45 H45A 0.9300 . ? C47 O15 1.212(13) . ? C47 O14 1.238(14) . ? C48 O16 1.231(10) . ? C48 O17 1.260(9) . ? C49 C50 1.375(12) . ? C49 H49A 0.9300 . ? C50 C51 1.362(12) . ? C50 H50A 0.9300 . ? C51 C52 1.375(11) . ? C51 C54 1.495(11) . ? C52 C53 1.367(13) . ? C52 H52A 0.9300 . ? C53 H53A 0.9300 . ? C54 C55 1.562(15) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.272(17) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C59 1.523(15) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.396(15) . ? C57 H57A 0.9300 . ? C58 C59 1.402(18) . ? C58 H58A 0.9300 . ? C59 C60 1.338(18) . ? C60 C61 1.355(15) . ? C60 H60A 0.9300 . ? C61 H61A 0.9300 . ? O1 Pb3 2.315(4) 2 ? O4 Pb4 2.558(5) 4_545 ? O5 Pb5 2.415(5) 4_545 ? O8 Pb5 2.467(9) 6 ? O9 Pb5 2.571(10) 6 ? O10 Pb1 2.723(5) 2 ? O12 Pb2 2.541(7) 1_565 ? O12 Pb3 2.750(6) 1_565 ? O13 Pb2 2.487(8) 2_565 ? O16 Pb4 2.640(7) 1_565 ? O17 Pb2 2.674(6) 1_565 ? 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 O1 Pb1 O2 80.72(15) . . ? O1 Pb1 O6 81.09(17) . . ? O2 Pb1 O6 80.91(17) . . ? O1 Pb1 O10 70.87(14) . 2 ? O2 Pb1 O10 139.83(16) . 2 ? O6 Pb1 O10 67.37(18) . 2 ? O1 Pb1 O3 126.08(17) . . ? O2 Pb1 O3 49.42(18) . . ? O6 Pb1 O3 73.0(2) . . ? O10 Pb1 O3 133.4(2) 2 . ? O1 Pb1 O4 122.45(16) . 4 ? O2 Pb1 O4 82.19(18) . 4 ? O6 Pb1 O4 148.07(17) . 4 ? O10 Pb1 O4 137.10(17) 2 4 ? O3 Pb1 O4 75.39(19) . 4 ? O1 Pb1 O11 79.59(14) . . ? O2 Pb1 O11 118.92(15) . . ? O6 Pb1 O11 149.24(16) . . ? O10 Pb1 O11 83.73(16) 2 . ? O3 Pb1 O11 137.64(18) . . ? O4 Pb1 O11 62.28(14) 4 . ? O1 Pb1 Pb2 36.99(9) . . ? O2 Pb1 Pb2 43.73(12) . . ? O6 Pb1 Pb2 78.59(12) . . ? O10 Pb1 Pb2 103.87(10) 2 . ? O3 Pb1 Pb2 91.02(14) . . ? O4 Pb1 Pb2 106.68(14) 4 . ? O11 Pb1 Pb2 99.34(9) . . ? O1 Pb2 O13 81.3(2) . 2_545 ? O1 Pb2 O2 81.35(15) . . ? O13 Pb2 O2 133.9(2) 2_545 . ? O1 Pb2 O12 82.27(18) . 1_545 ? O13 Pb2 O12 76.7(2) 2_545 1_545 ? O2 Pb2 O12 141.71(18) . 1_545 ? O1 Pb2 O7 77.97(16) . . ? O13 Pb2 O7 64.0(2) 2_545 . ? O2 Pb2 O7 70.69(16) . . ? O12 Pb2 O7 138.0(2) 1_545 . ? O1 Pb2 O17 67.76(15) . 1_545 ? O13 Pb2 O17 138.2(2) 2_545 1_545 ? O2 Pb2 O17 69.77(18) . 1_545 ? O12 Pb2 O17 72.0(2) 1_545 1_545 ? O7 Pb2 O17 130.50(17) . 1_545 ? O1 Pb2 Pb1 39.45(10) . . ? O13 Pb2 Pb1 110.4(2) 2_545 . ? O2 Pb2 Pb1 41.91(11) . . ? O12 Pb2 Pb1 114.17(13) 1_545 . ? O7 Pb2 Pb1 69.73(11) . . ? O17 Pb2 Pb1 61.03(12) 1_545 . ? O1 Pb2 Pb3 36.07(11) . . ? O13 Pb2 Pb3 86.06(17) 2_545 . ? O2 Pb2 Pb3 103.52(11) . . ? O12 Pb2 Pb3 48.34(13) 1_545 . ? O7 Pb2 Pb3 111.97(11) . . ? O17 Pb2 Pb3 52.37(12) 1_545 . ? Pb1 Pb2 Pb3 66.474(7) . . ? O1 Pb3 O1 77.80(16) . 2 ? O1 Pb3 O10 90.62(17) . . ? O1 Pb3 O10 74.90(15) 2 . ? O1 Pb3 O12 76.73(17) . 1_545 ? O1 Pb3 O12 103.87(19) 2 1_545 ? O10 Pb3 O12 167.19(19) . 1_545 ? O1 Pb3 O17 62.15(15) . 1_545 ? O1 Pb3 O17 139.78(16) 2 1_545 ? O10 Pb3 O17 107.35(17) . 1_545 ? O12 Pb3 O17 65.1(2) 1_545 1_545 ? O1 Pb3 O13 98.12(18) . 1_545 ? O1 Pb3 O13 70.30(18) 2 1_545 ? O10 Pb3 O13 141.24(18) . 1_545 ? O12 Pb3 O13 45.0(2) 1_545 1_545 ? O17 Pb3 O13 110.12(19) 1_545 1_545 ? O1 Pb3 Pb3 39.17(10) . 2 ? O1 Pb3 Pb3 38.66(10) 2 2 ? O10 Pb3 Pb3 81.92(13) . 2 ? O12 Pb3 Pb3 89.32(14) 1_545 2 ? O17 Pb3 Pb3 101.15(12) 1_545 2 ? O13 Pb3 Pb3 81.53(16) 1_545 2 ? O1 Pb3 Pb2 35.03(10) . . ? O1 Pb3 Pb2 98.18(10) 2 . ? O10 Pb3 Pb2 123.56(14) . . ? O12 Pb3 Pb2 43.66(14) 1_545 . ? O17 Pb3 Pb2 45.98(12) 1_545 . ? O13 Pb3 Pb2 78.58(14) 1_545 . ? Pb3 Pb3 Pb2 63.809(8) 2 . ? O11 Pb4 O14 95.8(2) . . ? O11 Pb4 O4 72.75(17) . 4 ? O14 Pb4 O4 87.3(3) . 4 ? O11 Pb4 O16 88.71(19) . 1_545 ? O14 Pb4 O16 163.8(3) . 1_545 ? O4 Pb4 O16 108.9(2) 4 1_545 ? O11 Pb4 N2 77.8(2) . 3_455 ? O14 Pb4 N2 82.1(3) . 3_455 ? O4 Pb4 N2 147.4(2) 4 3_455 ? O16 Pb4 N2 83.7(2) 1_545 3_455 ? O11 Pb4 O5 118.79(16) . 4 ? O14 Pb4 O5 89.1(3) . 4 ? O4 Pb4 O5 46.52(16) 4 4 ? O16 Pb4 O5 102.3(2) 1_545 4 ? N2 Pb4 O5 162.1(2) 3_455 4 ? O15 Pb5 O5 78.3(4) . 4 ? O15 Pb5 O8 74.8(5) . 6_556 ? O5 Pb5 O8 123.1(3) 4 6_556 ? O15 Pb5 O9 79.1(3) . 6_556 ? O5 Pb5 O9 78.4(2) 4 6_556 ? O8 Pb5 O9 48.0(3) 6_556 6_556 ? O15 Pb5 N1 149.9(4) . . ? O5 Pb5 N1 78.6(2) 4 . ? O8 Pb5 N1 102.6(5) 6_556 . ? O9 Pb5 N1 77.6(2) 6_556 . ? O15 Pb5 O8 113.4(5) . 4 ? O5 Pb5 O8 166.3(4) 4 4 ? O8 Pb5 O8 57.2(4) 6_556 4 ? O9 Pb5 O8 96.3(3) 6_556 4 ? N1 Pb5 O8 88.0(4) . 4 ? C49 N1 C53 116.1(8) . . ? C49 N1 Pb5 116.9(6) . . ? C53 N1 Pb5 125.9(6) . . ? C57 N2 C61 117.9(10) . . ? C57 N2 Pb4 120.3(7) . 3_545 ? C61 N2 Pb4 121.8(8) . 3_545 ? C2 C1 C10 118.6(7) . . ? C2 C1 C11 119.5(7) . . ? C10 C1 C11 121.7(7) . . ? C1 C2 C3 121.3(7) . . ? C1 C2 H2A 119.3 . . ? C3 C2 H2A 119.3 . . ? C4 C3 C2 122.2(8) . . ? C4 C3 H3A 118.9 . . ? C2 C3 H3A 118.9 . . ? C3 C4 C5 117.6(7) . . ? C3 C4 C12 117.8(7) . . ? C5 C4 C12 124.5(7) . . ? C10 C5 C6 118.9(8) . . ? C10 C5 C4 119.3(7) . . ? C6 C5 C4 121.7(8) . . ? C7 C6 C5 120.7(9) . . ? C7 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? C6 C7 C8 121.8(9) . . ? C6 C7 H7A 119.1 . . ? C8 C7 H7A 119.1 . . ? C9 C8 C7 119.5(10) . . ? C9 C8 H8A 120.3 . . ? C7 C8 H8A 120.3 . . ? C8 C9 C10 120.8(9) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C9 C10 C5 118.3(7) . . ? C9 C10 C1 120.9(7) . . ? C5 C10 C1 120.9(7) . . ? O3 C11 O2 123.8(7) . . ? O3 C11 C1 119.5(8) . . ? O2 C11 C1 116.6(8) . . ? O4 C12 O5 121.2(7) . . ? O4 C12 C4 120.6(7) . . ? O5 C12 C4 118.2(6) . . ? C14 C13 C22 119.4(7) . . ? C14 C13 C23 118.0(7) . . ? C22 C13 C23 122.6(6) . . ? C13 C14 C15 121.1(8) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C16 C15 C14 120.8(8) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 120.0(8) . . ? C15 C16 C24 117.4(9) . . ? C17 C16 C24 122.4(9) . . ? C18 C17 C16 121.9(8) . . ? C18 C17 C22 119.1(8) . . ? C16 C17 C22 118.9(7) . . ? C19 C18 C17 121.2(9) . . ? C19 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? C18 C19 C20 120.2(10) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C21 C20 C19 119.2(10) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C20 C21 C22 122.5(9) . . ? C20 C21 H21A 118.8 . . ? C22 C21 H21A 118.8 . . ? C21 C22 C17 117.7(7) . . ? C21 C22 C13 122.8(7) . . ? C17 C22 C13 119.5(7) . . ? O7 C23 O6 125.8(7) . . ? O7 C23 C13 117.8(6) . . ? O6 C23 C13 116.3(6) . . ? O9 C24 O8 118.8(11) . . ? O9 C24 C16 125.3(13) . . ? O8 C24 C16 115.9(10) . . ? C26 C25 C34 119.8(6) . . ? C26 C25 C35 116.3(6) . . ? C34 C25 C35 123.8(6) . . ? C25 C26 C27 120.5(7) . . ? C25 C26 H26A 119.8 . . ? C27 C26 H26A 119.8 . . ? C28 C27 C26 121.4(7) . . ? C28 C27 H27A 119.3 . . ? C26 C27 H27A 119.3 . . ? C27 C28 C29 120.3(6) . . ? C27 C28 C36 114.9(7) . . ? C29 C28 C36 124.8(7) . . ? C30 C29 C34 119.0(6) . . ? C30 C29 C28 122.5(6) . . ? C34 C29 C28 118.4(6) . . ? C31 C30 C29 119.7(8) . . ? C31 C30 H30A 120.2 . . ? C29 C30 H30A 120.2 . . ? C30 C31 C32 121.6(8) . . ? C30 C31 H31A 119.2 . . ? C32 C31 H31A 119.2 . . ? C33 C32 C31 119.8(8) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.1 . . ? C32 C33 C34 121.5(8) . . ? C32 C33 H33A 119.2 . . ? C34 C33 H33A 119.2 . . ? C33 C34 C25 122.3(6) . . ? C33 C34 C29 118.4(7) . . ? C25 C34 C29 119.3(6) . . ? O10 C35 O11 121.0(6) . . ? O10 C35 C25 119.6(6) . . ? O11 C35 C25 119.3(6) . . ? O12 C36 O13 123.6(8) . . ? O12 C36 C28 120.0(8) . . ? O13 C36 C28 116.4(9) . . ? C38 C37 C46 118.2(9) . . ? C38 C37 C47 116.7(10) . . ? C46 C37 C47 125.2(9) . . ? C37 C38 C39 121.5(10) . . ? C37 C38 H38A 119.2 . . ? C39 C38 H38A 119.2 . . ? C40 C39 C38 121.8(9) . . ? C40 C39 H39A 119.1 . . ? C38 C39 H39A 119.1 . . ? C39 C40 C41 118.1(9) . . ? C39 C40 C48 120.7(8) . . ? C41 C40 C48 121.0(9) . . ? C46 C41 C40 121.3(9) . . ? C46 C41 C42 118.9(8) . . ? C40 C41 C42 119.8(9) . . ? C43 C42 C41 120.7(9) . . ? C43 C42 H42A 119.7 . . ? C41 C42 H42A 119.7 . . ? C42 C43 C44 118.9(10) . . ? C42 C43 H43A 120.6 . . ? C44 C43 H43A 120.6 . . ? C45 C44 C43 121.6(10) . . ? C45 C44 H44A 119.2 . . ? C43 C44 H44A 119.2 . . ? C44 C45 C46 120.3(10) . . ? C44 C45 H45A 119.8 . . ? C46 C45 H45A 119.8 . . ? C41 C46 C45 119.4(9) . . ? C41 C46 C37 118.8(8) . . ? C45 C46 C37 121.5(9) . . ? O15 C47 O14 127.7(13) . . ? O15 C47 C37 114.9(13) . . ? O14 C47 C37 117.4(10) . . ? O16 C48 O17 123.7(8) . . ? O16 C48 C40 118.5(8) . . ? O17 C48 C40 117.5(8) . . ? N1 C49 C50 122.8(9) . . ? N1 C49 H49A 118.6 . . ? C50 C49 H49A 118.6 . . ? C51 C50 C49 122.0(8) . . ? C51 C50 H50A 119.0 . . ? C49 C50 H50A 119.0 . . ? C50 C51 C52 114.5(8) . . ? C50 C51 C54 122.3(8) . . ? C52 C51 C54 123.2(8) . . ? C53 C52 C51 120.3(9) . . ? C53 C52 H52A 119.9 . . ? C51 C52 H52A 119.9 . . ? N1 C53 C52 124.3(9) . . ? N1 C53 H53A 117.8 . . ? C52 C53 H53A 117.8 . . ? C51 C54 C55 109.7(9) . . ? C51 C54 H54A 109.7 . . ? C55 C54 H54A 109.7 . . ? C51 C54 H54B 109.7 . . ? C55 C54 H54B 109.7 . . ? H54A C54 H54B 108.2 . . ? C56 C55 C54 121.8(13) . . ? C56 C55 H55A 106.9 . . ? C54 C55 H55A 106.9 . . ? C56 C55 H55B 106.9 . . ? C54 C55 H55B 106.9 . . ? H55A C55 H55B 106.7 . . ? C55 C56 C59 121.1(15) . . ? C55 C56 H56A 107.1 . . ? C59 C56 H56A 107.1 . . ? C55 C56 H56B 107.1 . . ? C59 C56 H56B 107.1 . . ? H56A C56 H56B 106.8 . . ? N2 C57 C58 121.1(12) . . ? N2 C57 H57A 119.4 . . ? C58 C57 H57A 119.4 . . ? C57 C58 C59 119.8(13) . . ? C57 C58 H58A 120.1 . . ? C59 C58 H58A 120.1 . . ? C60 C59 C58 116.8(11) . . ? C60 C59 C56 121.9(15) . . ? C58 C59 C56 121.3(16) . . ? C59 C60 C61 119.5(12) . . ? C59 C60 H60A 120.3 . . ? C61 C60 H60A 120.3 . . ? N2 C61 C60 124.9(12) . . ? N2 C61 H61A 117.6 . . ? C60 C61 H61A 117.6 . . ? Pb2 O1 Pb3 108.89(16) . . ? Pb2 O1 Pb3 115.17(17) . 2 ? Pb3 O1 Pb3 102.17(16) . 2 ? Pb2 O1 Pb1 103.55(16) . . ? Pb3 O1 Pb1 118.49(17) . . ? Pb3 O1 Pb1 109.11(16) 2 . ? C11 O2 Pb1 101.3(5) . . ? C11 O2 Pb2 148.7(5) . . ? Pb1 O2 Pb2 94.37(16) . . ? C11 O3 Pb1 84.3(5) . . ? C12 O4 Pb4 101.2(4) . 4_545 ? C12 O5 Pb5 120.6(5) . 4_545 ? C23 O6 Pb1 126.5(4) . . ? C23 O7 Pb2 134.1(4) . . ? C24 O8 Pb5 97.1(8) . 6 ? C24 O9 Pb5 94.7(9) . 6 ? C35 O10 Pb3 109.0(4) . . ? C35 O10 Pb1 158.5(4) . 2 ? Pb3 O10 Pb1 92.46(14) . 2 ? C35 O11 Pb4 137.6(4) . . ? C35 O11 Pb1 109.8(4) . . ? Pb4 O11 Pb1 109.62(17) . . ? C36 O12 Pb2 134.9(6) . 1_565 ? C36 O12 Pb3 100.4(5) . 1_565 ? Pb2 O12 Pb3 88.00(17) 1_565 1_565 ? C36 O13 Pb2 154.5(6) . 2_565 ? C47 O14 Pb4 127.2(8) . . ? C47 O15 Pb5 150.2(8) . . ? C48 O16 Pb4 110.3(6) . 1_565 ? C48 O17 Pb2 127.2(6) . 1_565 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.581 _refine_diff_density_min -1.634 _refine_diff_density_rms 0.187 #===END OF 2