# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 886623' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H60 N12 O16 Pb2' _chemical_formula_weight 1859.78 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 P21/c 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 7.8908(7) _cell_length_b 16.1902(14) _cell_length_c 27.1562(19) _cell_angle_alpha 90.00 _cell_angle_beta 102.083(2) _cell_angle_gamma 90.00 _cell_volume 3392.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 5.041 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.441 _exptl_absorpt_correction_T_max 0.446 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18469 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6643 _reflns_number_gt 4784 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _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^)+(0.0290P)^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 6643 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _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 -0.56156(2) 0.461747(12) 0.237577(7) 0.03482(7) Uani 1 1 d . . . O1 O -0.8052(4) 0.4154(2) 0.27045(12) 0.0390(9) Uani 1 1 d . . . O2 O -0.5671(4) 0.3982(2) 0.32834(12) 0.0416(9) Uani 1 1 d . . . O3 O -1.4235(5) 0.4173(2) 0.71270(12) 0.0489(10) Uani 1 1 d . . . O4 O -1.6719(5) 0.4111(2) 0.65574(13) 0.0503(10) Uani 1 1 d . . . N1 N -0.7588(5) 0.3835(2) 0.15973(13) 0.0292(9) Uani 1 1 d . . . N2 N -0.8191(5) 0.5432(2) 0.18035(13) 0.0307(9) Uani 1 1 d . . . N3 N -1.5763(5) 0.4220(3) -0.15509(15) 0.0405(11) Uani 1 1 d . . . N4 N -1.6491(5) 0.5802(3) -0.13501(14) 0.0340(10) Uani 1 1 d . . . N5 N -1.2382(5) 0.5658(2) 0.02399(14) 0.0256(9) Uani 1 1 d . . . N6 N -1.1737(5) 0.4004(2) 0.00309(13) 0.0282(9) Uani 1 1 d . . . C1 C -0.7316(6) 0.3051(3) 0.15004(19) 0.0374(12) Uani 1 1 d . . . H1A H -0.6504 0.2762 0.1735 0.045 Uiso 1 1 calc R . . C2 C -0.8158(6) 0.2629(3) 0.10726(19) 0.0394(13) Uani 1 1 d . . . H2A H -0.7924 0.2075 0.1024 0.047 Uiso 1 1 calc R . . C3 C -0.9347(6) 0.3059(3) 0.07253(18) 0.0343(12) Uani 1 1 d . . . H3A H -0.9925 0.2799 0.0432 0.041 Uiso 1 1 calc R . . C4 C -0.9686(5) 0.3886(3) 0.08126(16) 0.0262(10) Uani 1 1 d . . . C5 C -1.0926(6) 0.4370(3) 0.04582(17) 0.0269(11) Uani 1 1 d . . . C6 C -1.1254(6) 0.5195(3) 0.05610(16) 0.0261(11) Uani 1 1 d . . . C7 C -1.0334(6) 0.5572(3) 0.10313(17) 0.0279(11) Uani 1 1 d . . . C8 C -1.0651(6) 0.6385(3) 0.11597(18) 0.0355(12) Uani 1 1 d . . . H8A H -1.1461 0.6707 0.0945 0.043 Uiso 1 1 calc R . . C9 C -0.9755(7) 0.6700(3) 0.16045(19) 0.0428(14) Uani 1 1 d . . . H9A H -0.9954 0.7238 0.1699 0.051 Uiso 1 1 calc R . . C10 C -0.8529(7) 0.6202(3) 0.19172(18) 0.0406(13) Uani 1 1 d . . . H10A H -0.7923 0.6422 0.2219 0.049 Uiso 1 1 calc R . . C11 C -0.9111(6) 0.5114(3) 0.13641(17) 0.0278(11) Uani 1 1 d . . . C12 C -0.8770(6) 0.4253(3) 0.12545(16) 0.0252(10) Uani 1 1 d . . . C13 C -1.2890(6) 0.4454(3) -0.02851(17) 0.0274(11) Uani 1 1 d . . . C14 C -1.3808(6) 0.4063(3) -0.07459(17) 0.0275(11) Uani 1 1 d . . . C15 C -1.3583(6) 0.3234(3) -0.08553(18) 0.0389(13) Uani 1 1 d . . . H15A H -1.2838 0.2904 -0.0626 0.047 Uiso 1 1 calc R . . C16 C -1.4469(7) 0.2905(3) -0.13039(19) 0.0465(14) Uani 1 1 d . . . H16A H -1.4360 0.2349 -0.1378 0.056 Uiso 1 1 calc R . . C17 C -1.5521(7) 0.3420(4) -0.1641(2) 0.0466(15) Uani 1 1 d . . . H17A H -1.6093 0.3200 -0.1947 0.056 Uiso 1 1 calc R . . C18 C -1.4959(6) 0.4531(3) -0.11033(17) 0.0318(11) Uani 1 1 d . . . C19 C -1.5320(6) 0.5394(3) -0.09991(17) 0.0306(11) Uani 1 1 d . . . C20 C -1.6832(7) 0.6578(3) -0.1252(2) 0.0417(14) Uani 1 1 d . . . H20A H -1.7633 0.6864 -0.1492 0.050 Uiso 1 1 calc R . . C21 C -1.6067(6) 0.6991(3) -0.08135(19) 0.0398(13) Uani 1 1 d . . . H21A H -1.6362 0.7535 -0.0761 0.048 Uiso 1 1 calc R . . C22 C -1.4871(6) 0.6582(3) -0.04599(19) 0.0354(12) Uani 1 1 d . . . H22A H -1.4334 0.6846 -0.0164 0.043 Uiso 1 1 calc R . . C23 C -1.4467(6) 0.5761(3) -0.05496(16) 0.0265(11) Uani 1 1 d . . . C24 C -1.3210(6) 0.5285(3) -0.01833(16) 0.0258(10) Uani 1 1 d . . . C25 C -0.7266(7) 0.4005(3) 0.31597(18) 0.0331(12) Uani 1 1 d . . . C26 C -0.8363(6) 0.3911(3) 0.35498(17) 0.0311(11) Uani 1 1 d . . . C27 C -1.0125(7) 0.4053(3) 0.3431(2) 0.0450(14) Uani 1 1 d . . . H27A H -1.0665 0.4164 0.3100 0.054 Uiso 1 1 calc R . . C28 C -1.1096(8) 0.4034(3) 0.3798(2) 0.0535(16) Uani 1 1 d . . . H28A H -1.2281 0.4135 0.3710 0.064 Uiso 1 1 calc R . . C29 C -1.0341(8) 0.3866(3) 0.4294(2) 0.0511(15) Uani 1 1 d . . . C30 C -0.8566(9) 0.3697(3) 0.4415(2) 0.0548(17) Uani 1 1 d . . . H30A H -0.8034 0.3566 0.4744 0.066 Uiso 1 1 calc R . . C31 C -0.7595(7) 0.3724(3) 0.40448(19) 0.0446(14) Uani 1 1 d . . . H31A H -0.6412 0.3615 0.4129 0.053 Uiso 1 1 calc R . . C32 C -1.5119(7) 0.4131(3) 0.66742(18) 0.0361(12) Uani 1 1 d . . . C33 C -1.4101(6) 0.4110(3) 0.62634(18) 0.0310(11) Uani 1 1 d . . . C34 C -1.2305(7) 0.4034(3) 0.6382(2) 0.0435(14) Uani 1 1 d . . . H34A H -1.1738 0.4004 0.6718 0.052 Uiso 1 1 calc R . . C35 C -1.1359(8) 0.4003(3) 0.6015(2) 0.0524(15) Uani 1 1 d . . . H35A H -1.0159 0.3957 0.6105 0.063 Uiso 1 1 calc R . . C36 C -1.2148(8) 0.4040(3) 0.5516(2) 0.0509(16) Uani 1 1 d . . . C37 C -1.3964(8) 0.4135(3) 0.53893(19) 0.0494(16) Uani 1 1 d . . . H37A H -1.4519 0.4175 0.5052 0.059 Uiso 1 1 calc R . . C38 C -1.4944(7) 0.4170(3) 0.57628(18) 0.0409(13) Uani 1 1 d . . . H38A H -1.6141 0.4233 0.5677 0.049 Uiso 1 1 calc R . . C39 C -1.1029(10) 0.3986(4) 0.5131(3) 0.072(2) Uani 1 1 d . . . H39A H -0.9839 0.4010 0.5255 0.086 Uiso 1 1 calc R . . C40 C -1.1495(10) 0.3914(4) 0.4678(3) 0.071(2) Uani 1 1 d . . . H40A H -1.2684 0.3887 0.4551 0.085 Uiso 1 1 calc R . . O1W O -0.3884(6) 0.2975(3) 0.24657(17) 0.0935(16) Uani 1 1 d . . . H1WA H -0.3864 0.2474 0.2374 0.112 Uiso 1 1 d R . . H1WB H -0.2960 0.3059 0.2359 0.112 Uiso 1 1 d R . . O2W O 0.1503(5) 0.1431(2) 0.22701(14) 0.0615(11) Uani 1 1 d . . . H2WA H 0.1595 0.0953 0.2403 0.074 Uiso 1 1 d R . . H2WB H 0.2040 0.1284 0.2044 0.074 Uiso 1 1 d R . . O3W O -0.0441(5) 0.2800(2) 0.23037(13) 0.0578(11) Uani 1 1 d . . . H3WA H 0.0040 0.2330 0.2303 0.069 Uiso 1 1 d R . . H3WB H 0.0287 0.3194 0.2345 0.069 Uiso 1 1 d R . . O4W O 0.8576(5) 0.4896(2) 0.22896(13) 0.0605(11) Uani 1 1 d . . . H4WA H 0.7876 0.4715 0.2031 0.073 Uiso 1 1 d R . . H4WB H 0.9412 0.4556 0.2319 0.073 Uiso 1 1 d 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 0.02892(11) 0.04962(13) 0.02549(10) -0.00228(10) 0.00474(7) -0.00178(11) O1 0.037(2) 0.056(2) 0.0258(19) 0.0057(16) 0.0108(16) -0.0040(18) O2 0.033(2) 0.054(2) 0.040(2) 0.0087(18) 0.0131(17) 0.0030(19) O3 0.058(3) 0.062(3) 0.0237(19) -0.0047(18) 0.0021(19) 0.002(2) O4 0.034(2) 0.079(3) 0.041(2) -0.003(2) 0.0142(19) -0.003(2) N1 0.028(2) 0.034(2) 0.023(2) 0.0068(18) -0.0009(17) 0.0008(19) N2 0.031(2) 0.036(2) 0.024(2) -0.0023(19) 0.0030(17) -0.002(2) N3 0.038(3) 0.047(3) 0.033(3) -0.006(2) 0.000(2) -0.001(2) N4 0.027(2) 0.043(3) 0.030(2) 0.0104(19) 0.0025(19) 0.005(2) N5 0.023(2) 0.027(2) 0.027(2) 0.0030(16) 0.0051(18) -0.0009(16) N6 0.025(2) 0.030(2) 0.028(2) 0.0019(18) 0.0013(18) 0.0011(18) C1 0.032(3) 0.038(3) 0.042(3) 0.008(2) 0.006(2) 0.007(2) C2 0.042(3) 0.029(3) 0.047(3) -0.001(2) 0.006(3) 0.003(2) C3 0.032(3) 0.033(3) 0.036(3) -0.002(2) 0.003(2) -0.002(2) C4 0.018(2) 0.032(3) 0.028(2) 0.006(2) 0.003(2) 0.002(2) C5 0.025(3) 0.031(3) 0.025(2) 0.002(2) 0.005(2) 0.001(2) C6 0.025(3) 0.032(3) 0.023(2) 0.003(2) 0.010(2) -0.001(2) C7 0.024(3) 0.035(3) 0.027(3) -0.002(2) 0.008(2) -0.003(2) C8 0.040(3) 0.032(3) 0.031(3) -0.001(2) -0.001(2) 0.005(2) C9 0.051(4) 0.030(3) 0.044(3) -0.006(2) 0.003(3) 0.005(3) C10 0.046(3) 0.045(3) 0.029(3) -0.007(2) 0.003(2) -0.006(3) C11 0.027(3) 0.036(3) 0.023(2) -0.001(2) 0.011(2) -0.003(2) C12 0.023(3) 0.033(3) 0.020(2) 0.003(2) 0.006(2) -0.005(2) C13 0.025(3) 0.034(3) 0.025(2) 0.005(2) 0.008(2) 0.000(2) C14 0.020(3) 0.035(3) 0.027(3) -0.001(2) 0.003(2) -0.001(2) C15 0.038(3) 0.044(3) 0.034(3) -0.001(2) 0.006(2) 0.000(3) C16 0.056(4) 0.038(3) 0.041(3) -0.014(3) -0.001(3) -0.005(3) C17 0.036(3) 0.066(4) 0.034(3) -0.009(3) -0.001(3) -0.010(3) C18 0.028(3) 0.040(3) 0.027(3) 0.003(2) 0.007(2) -0.002(2) C19 0.021(2) 0.041(3) 0.031(3) 0.008(2) 0.008(2) 0.002(2) C20 0.034(3) 0.045(4) 0.044(3) 0.018(3) 0.002(3) 0.001(3) C21 0.038(3) 0.035(3) 0.047(3) 0.015(3) 0.009(3) 0.005(2) C22 0.037(3) 0.034(3) 0.035(3) 0.005(2) 0.006(2) 0.002(2) C23 0.022(3) 0.034(3) 0.023(2) 0.007(2) 0.005(2) 0.001(2) C24 0.025(2) 0.031(3) 0.024(2) 0.003(2) 0.010(2) -0.002(2) C25 0.041(3) 0.025(3) 0.036(3) 0.003(2) 0.013(3) -0.001(2) C26 0.038(3) 0.026(3) 0.031(3) -0.001(2) 0.010(2) -0.003(2) C27 0.047(4) 0.056(4) 0.035(3) 0.001(3) 0.015(3) -0.001(3) C28 0.055(4) 0.055(4) 0.058(4) 0.002(3) 0.030(3) -0.001(3) C29 0.071(5) 0.042(3) 0.050(4) 0.001(3) 0.033(3) -0.009(3) C30 0.083(5) 0.057(4) 0.028(3) 0.004(3) 0.018(3) -0.006(4) C31 0.046(3) 0.051(4) 0.036(3) 0.007(3) 0.007(3) 0.003(3) C32 0.053(4) 0.024(3) 0.032(3) 0.000(2) 0.011(3) -0.002(2) C33 0.037(3) 0.023(3) 0.033(3) -0.002(2) 0.007(2) -0.004(2) C34 0.043(3) 0.039(3) 0.049(3) -0.003(3) 0.012(3) 0.001(3) C35 0.049(4) 0.046(4) 0.065(4) -0.002(3) 0.019(3) 0.003(3) C36 0.062(4) 0.030(3) 0.074(5) 0.000(3) 0.043(4) -0.002(3) C37 0.086(5) 0.040(3) 0.024(3) 0.005(2) 0.015(3) 0.001(3) C38 0.044(3) 0.045(3) 0.032(3) 0.003(2) 0.005(3) -0.002(3) C39 0.103(6) 0.045(4) 0.074(5) 0.010(4) 0.031(5) -0.008(4) C40 0.112(6) 0.050(4) 0.058(4) 0.004(4) 0.032(4) -0.018(4) O1W 0.070(3) 0.119(4) 0.096(4) 0.041(3) 0.026(3) 0.020(3) O2W 0.066(3) 0.066(3) 0.056(3) 0.002(2) 0.019(2) 0.019(2) O3W 0.054(3) 0.050(2) 0.066(3) 0.004(2) 0.003(2) 0.000(2) O4W 0.051(3) 0.078(3) 0.046(2) -0.006(2) -0.005(2) 0.016(2) _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 O3 2.395(4) 3_366 ? Pb1 O1 2.403(3) . ? Pb1 N2 2.639(4) . ? Pb1 N1 2.668(4) . ? Pb1 O2 2.680(3) . ? O1 C25 1.285(5) . ? O2 C25 1.233(5) . ? O3 C32 1.282(6) . ? O3 Pb1 2.395(3) 3_366 ? O4 C32 1.236(6) . ? N1 C1 1.322(6) . ? N1 C12 1.354(5) . ? N2 C10 1.324(6) . ? N2 C11 1.361(6) . ? N3 C17 1.338(6) . ? N3 C18 1.346(6) . ? N4 C20 1.323(6) . ? N4 C19 1.353(6) . ? N5 C6 1.338(5) . ? N5 C24 1.341(5) . ? N6 C13 1.329(5) . ? N6 C5 1.340(5) . ? C1 C2 1.392(7) . ? C1 H1A 0.9300 . ? C2 C3 1.372(6) . ? C2 H2A 0.9300 . ? C3 C4 1.396(6) . ? C3 H3A 0.9300 . ? C4 C12 1.397(6) . ? C4 C5 1.451(6) . ? C5 C6 1.400(6) . ? C6 C7 1.463(6) . ? C7 C11 1.391(6) . ? C7 C8 1.398(6) . ? C8 C9 1.365(6) . ? C8 H8A 0.9300 . ? C9 C10 1.402(7) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.461(6) . ? C13 C24 1.407(6) . ? C13 C14 1.453(6) . ? C14 C15 1.394(6) . ? C14 C18 1.404(6) . ? C15 C16 1.378(6) . ? C15 H15A 0.9300 . ? C16 C17 1.380(7) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.465(7) . ? C19 C23 1.397(6) . ? C20 C21 1.389(7) . ? C20 H20A 0.9300 . ? C21 C22 1.368(6) . ? C21 H21A 0.9300 . ? C22 C23 1.399(6) . ? C22 H22A 0.9300 . ? C23 C24 1.468(6) . ? C25 C26 1.510(6) . ? C26 C27 1.379(7) . ? C26 C31 1.387(6) . ? C27 C28 1.378(7) . ? C27 H27A 0.9300 . ? C28 C29 1.380(8) . ? C28 H28A 0.9300 . ? C29 C30 1.397(8) . ? C29 C40 1.522(8) . ? C30 C31 1.386(7) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 C33 1.505(7) . ? C33 C38 1.386(6) . ? C33 C34 1.392(7) . ? C34 C35 1.367(7) . ? C34 H34A 0.9300 . ? C35 C36 1.369(8) . ? C35 H35A 0.9300 . ? C36 C37 1.410(8) . ? C36 C39 1.504(8) . ? C37 C38 1.400(7) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 C40 1.215(8) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? O1W H1WA 0.8499 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8501 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? 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 O3 Pb1 O1 84.72(12) 3_366 . ? O3 Pb1 N2 78.51(12) 3_366 . ? O1 Pb1 N2 78.30(11) . . ? O3 Pb1 N1 138.20(12) 3_366 . ? O1 Pb1 N1 76.52(11) . . ? N2 Pb1 N1 61.39(12) . . ? O3 Pb1 O2 77.48(11) 3_366 . ? O1 Pb1 O2 50.95(10) . . ? N2 Pb1 O2 125.08(11) . . ? N1 Pb1 O2 115.29(11) . . ? C25 O1 Pb1 98.8(3) . . ? C25 O2 Pb1 87.1(3) . . ? C32 O3 Pb1 120.2(3) . 3_366 ? C1 N1 C12 117.4(4) . . ? C1 N1 Pb1 121.4(3) . . ? C12 N1 Pb1 120.7(3) . . ? C10 N2 C11 117.7(4) . . ? C10 N2 Pb1 120.1(3) . . ? C11 N2 Pb1 122.0(3) . . ? C17 N3 C18 118.0(5) . . ? C20 N4 C19 117.4(5) . . ? C6 N5 C24 116.4(4) . . ? C13 N6 C5 117.1(4) . . ? N1 C1 C2 124.7(5) . . ? N1 C1 H1A 117.7 . . ? C2 C1 H1A 117.7 . . ? C3 C2 C1 117.5(5) . . ? C3 C2 H2A 121.2 . . ? C1 C2 H2A 121.2 . . ? C2 C3 C4 119.9(5) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C12 118.1(4) . . ? C3 C4 C5 122.2(4) . . ? C12 C4 C5 119.7(4) . . ? N6 C5 C6 121.3(4) . . ? N6 C5 C4 118.0(4) . . ? C6 C5 C4 120.7(4) . . ? N5 C6 C5 122.0(4) . . ? N5 C6 C7 118.4(4) . . ? C5 C6 C7 119.6(4) . . ? C11 C7 C8 118.5(4) . . ? C11 C7 C6 119.6(4) . . ? C8 C7 C6 121.9(4) . . ? C9 C8 C7 119.1(5) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C8 C9 C10 119.0(5) . . ? C8 C9 H9A 120.5 . . ? C10 C9 H9A 120.5 . . ? N2 C10 C9 123.2(5) . . ? N2 C10 H10A 118.4 . . ? C9 C10 H10A 118.4 . . ? N2 C11 C7 122.5(4) . . ? N2 C11 C12 116.9(4) . . ? C7 C11 C12 120.6(4) . . ? N1 C12 C4 122.4(4) . . ? N1 C12 C11 117.8(4) . . ? C4 C12 C11 119.8(4) . . ? N6 C13 C24 121.6(4) . . ? N6 C13 C14 117.9(4) . . ? C24 C13 C14 120.5(4) . . ? C15 C14 C18 117.7(4) . . ? C15 C14 C13 122.7(4) . . ? C18 C14 C13 119.6(4) . . ? C16 C15 C14 119.8(5) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C15 C16 C17 118.4(5) . . ? C15 C16 H16A 120.8 . . ? C17 C16 H16A 120.8 . . ? N3 C17 C16 123.6(5) . . ? N3 C17 H17A 118.2 . . ? C16 C17 H17A 118.2 . . ? N3 C18 C14 122.4(5) . . ? N3 C18 C19 117.3(4) . . ? C14 C18 C19 120.3(4) . . ? N4 C19 C23 122.7(5) . . ? N4 C19 C18 117.5(4) . . ? C23 C19 C18 119.8(4) . . ? N4 C20 C21 124.0(5) . . ? N4 C20 H20A 118.0 . . ? C21 C20 H20A 118.0 . . ? C22 C21 C20 118.8(5) . . ? C22 C21 H21A 120.6 . . ? C20 C21 H21A 120.6 . . ? C21 C22 C23 119.1(5) . . ? C21 C22 H22A 120.5 . . ? C23 C22 H22A 120.5 . . ? C19 C23 C22 118.1(4) . . ? C19 C23 C24 120.1(4) . . ? C22 C23 C24 121.8(4) . . ? N5 C24 C13 121.6(4) . . ? N5 C24 C23 118.9(4) . . ? C13 C24 C23 119.5(4) . . ? O2 C25 O1 121.9(5) . . ? O2 C25 C26 120.5(4) . . ? O1 C25 C26 117.5(4) . . ? C27 C26 C31 118.5(5) . . ? C27 C26 C25 121.2(4) . . ? C31 C26 C25 120.2(5) . . ? C28 C27 C26 120.9(5) . . ? C28 C27 H27A 119.6 . . ? C26 C27 H27A 119.6 . . ? C27 C28 C29 121.2(6) . . ? C27 C28 H28A 119.4 . . ? C29 C28 H28A 119.4 . . ? C28 C29 C30 118.3(5) . . ? C28 C29 C40 117.3(6) . . ? C30 C29 C40 124.3(6) . . ? C31 C30 C29 120.2(5) . . ? C31 C30 H30A 119.9 . . ? C29 C30 H30A 119.9 . . ? C26 C31 C30 120.9(5) . . ? C26 C31 H31A 119.6 . . ? C30 C31 H31A 119.6 . . ? O4 C32 O3 124.6(5) . . ? O4 C32 C33 118.9(5) . . ? O3 C32 C33 116.4(5) . . ? C38 C33 C34 119.4(5) . . ? C38 C33 C32 120.3(5) . . ? C34 C33 C32 120.3(5) . . ? C35 C34 C33 121.3(5) . . ? C35 C34 H34A 119.4 . . ? C33 C34 H34A 119.4 . . ? C34 C35 C36 121.1(6) . . ? C34 C35 H35A 119.4 . . ? C36 C35 H35A 119.4 . . ? C35 C36 C37 118.3(5) . . ? C35 C36 C39 118.3(6) . . ? C37 C36 C39 123.5(6) . . ? C38 C37 C36 121.0(5) . . ? C38 C37 H37A 119.5 . . ? C36 C37 H37A 119.5 . . ? C33 C38 C37 118.9(5) . . ? C33 C38 H38A 120.5 . . ? C37 C38 H38A 120.5 . . ? C40 C39 C36 127.8(8) . . ? C40 C39 H39A 116.1 . . ? C36 C39 H39A 116.1 . . ? C39 C40 C29 127.0(8) . . ? C39 C40 H40A 116.5 . . ? C29 C40 H40A 116.5 . . ? H1WA O1W H1WB 89.0 . . ? H2WA O2W H2WB 92.2 . . ? H3WA O3W H3WB 112.5 . . ? H4WA O4W H4WB 102.2 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.066 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.109 data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 886624' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H28 N10 O6 Pb' _chemical_formula_weight 963.93 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.589(5) _cell_length_b 22.803(5) _cell_length_c 14.703(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.504(5) _cell_angle_gamma 90.00 _cell_volume 3520(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 27.60 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1659 _exptl_absorpt_coefficient_mu 4.846 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.325 _exptl_absorpt_correction_T_max 0.418 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31836 _diffrn_reflns_av_R_equivalents 0.0935 _diffrn_reflns_av_sigmaI/netI 0.0989 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.60 _reflns_number_total 8124 _reflns_number_gt 4380 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _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^)+(0.0543P)^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 8124 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1255 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _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 O1W O 0.3999(14) 0.3199(6) -0.2465(9) 0.237(7) Uani 1 1 d . . . H1WA H 0.4324 0.3304 -0.1872 0.285 Uiso 1 1 d R . . H1WB H 0.3527 0.3092 -0.2004 0.285 Uiso 1 1 d R . . Pb1 Pb 0.48085(3) 0.295621(14) 0.36248(2) 0.05299(12) Uani 1 1 d . . . O1 O 0.6923(5) 0.3291(2) 0.4276(3) 0.0589(14) Uani 1 1 d . . . N1 N 0.4185(6) 0.3224(3) 0.1819(4) 0.0543(16) Uani 1 1 d . . . C1 C 0.7400(7) 0.3217(4) 0.3545(6) 0.055(2) Uani 1 1 d . . . O2 O 0.6761(6) 0.3007(3) 0.2848(4) 0.0770(18) Uani 1 1 d . . . N2 N 0.4978(6) 0.4065(3) 0.3077(4) 0.0504(15) Uani 1 1 d . . . C2 C 0.8770(9) 0.3376(5) 0.3509(7) 0.094(3) Uani 1 1 d . . . H2A H 0.9237 0.3015 0.3454 0.113 Uiso 1 1 calc R . . H2B H 0.8808 0.3597 0.2949 0.113 Uiso 1 1 calc R . . O3 O 0.4353(8) 0.3601(3) 0.5078(5) 0.100(2) Uani 1 1 d . . . N3 N 0.5392(5) 0.5435(2) 0.0643(4) 0.0366(13) Uani 1 1 d . . . C3 C 0.9447(11) 0.3711(7) 0.4263(9) 0.121(4) Uani 1 1 d . . . H3B H 1.0348 0.3619 0.4303 0.145 Uiso 1 1 calc R . . H3A H 0.9158 0.3583 0.4830 0.145 Uiso 1 1 calc R . . N4 N 0.5632(6) 0.1797(3) 0.3428(4) 0.0546(16) Uani 1 1 d . . . O4 O 0.2658(10) 0.3674(6) 0.5702(8) 0.188(5) Uani 1 1 d . . . C4 C 0.9291(11) 0.4358(6) 0.4188(9) 0.111(4) Uani 1 1 d . . . H4A H 0.8396 0.4454 0.4171 0.133 Uiso 1 1 calc R . . H4B H 0.9560 0.4488 0.3615 0.133 Uiso 1 1 calc R . . N5 N 0.5404(5) 0.2195(2) 0.5137(4) 0.0461(15) Uani 1 1 d . . . O5 O 0.2657(9) 0.3676(5) 0.4174(8) 0.157(4) Uani 1 1 d . . . C5 C 1.0071(13) 0.4698(5) 0.4999(10) 0.120(4) Uani 1 1 d . . . H5A H 0.9832 0.4547 0.5570 0.144 Uiso 1 1 calc R . . H5B H 1.0966 0.4611 0.4995 0.144 Uiso 1 1 calc R . . N6 N 0.6633(5) 0.0315(3) 0.6419(4) 0.0452(14) Uani 1 1 d . . . C6 C 0.4490(6) 0.3756(3) 0.1499(5) 0.0409(16) Uani 1 1 d . . . N7 N 0.6723(5) -0.0132(3) 0.4664(4) 0.0439(14) Uani 1 1 d . . . C7 C 0.4899(6) 0.4207(3) 0.2166(5) 0.0436(17) Uani 1 1 d . . . N8 N 0.7917(7) -0.2011(3) 0.6025(5) 0.0668(19) Uani 1 1 d . . . C8 C 0.5338(8) 0.4494(4) 0.3672(5) 0.061(2) Uani 1 1 d . . . H8 H 0.5377 0.4405 0.4293 0.073 Uiso 1 1 calc R . . N9 N 0.7840(7) -0.1567(3) 0.7726(5) 0.0676(19) Uani 1 1 d . . . C9 C 0.5650(8) 0.5045(4) 0.3451(5) 0.058(2) Uani 1 1 d . . . H9 H 0.5917 0.5317 0.3907 0.070 Uiso 1 1 calc R . . C10 C 0.5565(7) 0.5195(3) 0.2550(5) 0.0509(19) Uani 1 1 d . . . H10 H 0.5759 0.5574 0.2379 0.061 Uiso 1 1 calc R . . C11 C 0.5182(6) 0.4770(3) 0.1885(5) 0.0402(16) Uani 1 1 d . . . N12 N 0.3221(12) 0.3661(5) 0.4989(10) 0.112(4) Uani 1 1 d . . . C12 C 0.5105(6) 0.4903(3) 0.0902(4) 0.0362(15) Uani 1 1 d . . . C13 C 0.4716(6) 0.4463(3) 0.0255(4) 0.0368(16) Uani 1 1 d . . . C14 C 0.4405(5) 0.3872(3) 0.0554(4) 0.0358(15) Uani 1 1 d . . . C15 C 0.4017(6) 0.3430(3) -0.0053(5) 0.0453(17) Uani 1 1 d . . . H15 H 0.3962 0.3494 -0.0682 0.054 Uiso 1 1 calc R . . C16 C 0.3711(7) 0.2895(3) 0.0278(6) 0.0541(19) Uani 1 1 d . . . H16 H 0.3437 0.2594 -0.0127 0.065 Uiso 1 1 calc R . . C17 C 0.3808(8) 0.2803(3) 0.1204(6) 0.059(2) Uani 1 1 d . . . H17 H 0.3606 0.2435 0.1416 0.070 Uiso 1 1 calc R . . C18 C 0.5824(6) 0.1403(3) 0.4123(5) 0.0431(17) Uani 1 1 d . . . C19 C 0.5725(6) 0.1627(3) 0.5042(5) 0.0409(16) Uani 1 1 d . . . C20 C 0.5389(7) 0.2412(4) 0.5972(6) 0.057(2) Uani 1 1 d . . . H20 H 0.5129 0.2799 0.6028 0.068 Uiso 1 1 calc R . . C21 C 0.5748(8) 0.2087(4) 0.6778(6) 0.062(2) Uani 1 1 d . . . H21 H 0.5785 0.2261 0.7352 0.074 Uiso 1 1 calc R . . C22 C 0.6043(7) 0.1502(4) 0.6694(5) 0.054(2) Uani 1 1 d . . . H22 H 0.6248 0.1270 0.7212 0.064 Uiso 1 1 calc R . . C23 C 0.6028(6) 0.1264(3) 0.5810(5) 0.0452(17) Uani 1 1 d . . . C24 C 0.6359(6) 0.0655(3) 0.5679(5) 0.0415(17) Uani 1 1 d . . . C25 C 0.6956(6) -0.0232(3) 0.6292(5) 0.0416(17) Uani 1 1 d . . . C26 C 0.6982(6) -0.0462(3) 0.5407(5) 0.0411(17) Uani 1 1 d . . . C27 C 0.6404(6) 0.0426(3) 0.4796(4) 0.0382(16) Uani 1 1 d . . . C28 C 0.6166(6) 0.0819(3) 0.3998(5) 0.0434(17) Uani 1 1 d . . . C29 C 0.6298(7) 0.0624(4) 0.3117(5) 0.054(2) Uani 1 1 d . . . H29 H 0.6496 0.0235 0.3009 0.064 Uiso 1 1 calc R . . C30 C 0.6127(8) 0.1025(4) 0.2412(5) 0.068(2) Uani 1 1 d . . . H30 H 0.6237 0.0915 0.1818 0.082 Uiso 1 1 calc R . . C31 C 0.5785(8) 0.1599(4) 0.2602(6) 0.063(2) Uani 1 1 d . . . H31 H 0.5655 0.1861 0.2114 0.076 Uiso 1 1 calc R . . C32 C 0.7329(6) -0.1084(3) 0.5313(5) 0.0471(18) Uani 1 1 d . . . C33 C 0.7600(7) -0.1442(3) 0.6086(5) 0.0516(19) Uani 1 1 d . . . C34 C 0.7965(8) -0.2230(4) 0.5187(7) 0.068(2) Uani 1 1 d . . . H34 H 0.8177 -0.2624 0.5143 0.082 Uiso 1 1 calc R . . C35 C 0.7725(8) -0.1915(4) 0.4385(7) 0.064(2) Uani 1 1 d . . . H35 H 0.7783 -0.2091 0.3822 0.076 Uiso 1 1 calc R . . C36 C 0.7397(7) -0.1336(4) 0.4440(5) 0.056(2) Uani 1 1 d . . . H36 H 0.7221 -0.1112 0.3911 0.067 Uiso 1 1 calc R . . C37 C 0.7568(7) -0.1198(4) 0.7003(5) 0.057(2) Uani 1 1 d . . . C38 C 0.7840(8) -0.1323(5) 0.8550(6) 0.074(3) Uani 1 1 d . . . H38 H 0.8031 -0.1568 0.9056 0.089 Uiso 1 1 calc R . . C39 C 0.7582(9) -0.0739(4) 0.8729(6) 0.070(2) Uani 1 1 d . . . H39 H 0.7616 -0.0599 0.9326 0.084 Uiso 1 1 calc R . . C40 C 0.7273(7) -0.0377(4) 0.7978(5) 0.062(2) Uani 1 1 d . . . H40 H 0.7082 0.0016 0.8058 0.075 Uiso 1 1 calc R . . C41 C 0.7252(6) -0.0611(4) 0.7098(5) 0.0492(19) 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 O1W 0.270(17) 0.269(15) 0.187(12) -0.052(11) 0.081(12) 0.045(12) Pb1 0.05136(17) 0.0565(2) 0.05217(19) 0.01611(17) 0.01096(12) 0.00434(17) O1 0.060(3) 0.068(4) 0.049(3) 0.013(3) 0.010(3) 0.006(3) N1 0.047(3) 0.045(4) 0.068(4) 0.019(4) 0.000(3) -0.003(3) C1 0.054(5) 0.061(5) 0.051(5) 0.017(4) 0.012(4) 0.014(4) O2 0.078(4) 0.099(5) 0.058(4) -0.006(4) 0.021(3) -0.001(4) N2 0.061(4) 0.047(4) 0.042(4) 0.007(3) 0.002(3) -0.001(3) C2 0.063(6) 0.123(9) 0.100(8) -0.010(7) 0.027(6) -0.020(6) O3 0.112(6) 0.086(5) 0.107(6) 0.015(4) 0.037(5) 0.007(5) N3 0.034(3) 0.023(3) 0.052(4) 0.001(3) 0.002(3) -0.002(2) C3 0.084(8) 0.147(13) 0.130(11) 0.028(10) 0.009(8) -0.014(8) N4 0.063(4) 0.059(4) 0.043(4) 0.020(3) 0.013(3) 0.004(3) O4 0.142(8) 0.258(14) 0.181(9) -0.091(9) 0.090(8) -0.026(9) C4 0.089(8) 0.127(11) 0.116(10) 0.024(9) 0.012(7) -0.004(8) N5 0.048(3) 0.040(4) 0.052(4) 0.007(3) 0.010(3) -0.001(3) O5 0.099(7) 0.224(12) 0.155(9) 0.068(9) 0.036(6) 0.051(7) C5 0.107(9) 0.116(10) 0.136(10) 0.034(11) 0.008(8) 0.003(10) N6 0.043(3) 0.050(4) 0.042(3) 0.012(3) 0.002(3) -0.002(3) C6 0.033(3) 0.033(4) 0.056(4) 0.005(4) 0.004(3) -0.004(3) N7 0.039(3) 0.044(4) 0.047(3) 0.010(3) 0.000(3) -0.007(3) C7 0.042(4) 0.040(4) 0.048(4) 0.007(4) 0.001(3) 0.003(3) N8 0.087(5) 0.051(5) 0.064(5) 0.008(4) 0.014(4) 0.007(4) C8 0.078(6) 0.064(6) 0.039(4) 0.011(4) 0.000(4) -0.002(5) N9 0.085(5) 0.061(5) 0.057(5) 0.021(4) 0.009(4) 0.008(4) C9 0.080(6) 0.054(6) 0.039(4) -0.004(4) 0.000(4) -0.009(4) C10 0.061(5) 0.037(4) 0.055(5) 0.000(4) 0.010(4) 0.005(4) C11 0.038(4) 0.037(4) 0.044(4) 0.008(3) 0.000(3) 0.005(3) N12 0.095(8) 0.090(7) 0.161(11) -0.014(8) 0.053(9) 0.005(6) C12 0.032(3) 0.037(4) 0.038(4) 0.005(3) 0.002(3) 0.001(3) C13 0.028(3) 0.043(4) 0.039(4) 0.007(3) 0.003(3) 0.005(3) C14 0.028(3) 0.031(4) 0.047(4) 0.008(3) 0.000(3) -0.002(3) C15 0.043(4) 0.039(4) 0.051(4) 0.005(4) -0.007(3) -0.001(3) C16 0.048(4) 0.043(5) 0.068(5) -0.001(4) -0.004(4) -0.003(4) C17 0.061(5) 0.029(4) 0.082(6) 0.016(4) -0.008(4) -0.007(4) C18 0.036(4) 0.048(5) 0.044(4) 0.011(4) 0.003(3) -0.004(3) C19 0.042(4) 0.040(4) 0.041(4) 0.006(3) 0.007(3) -0.010(3) C20 0.063(5) 0.046(5) 0.062(5) 0.005(4) 0.013(4) 0.002(4) C21 0.082(6) 0.056(6) 0.051(5) 0.002(4) 0.016(4) -0.003(5) C22 0.065(5) 0.054(5) 0.044(4) 0.007(4) 0.013(4) 0.000(4) C23 0.045(4) 0.044(5) 0.047(4) 0.005(4) 0.007(3) -0.006(3) C24 0.028(3) 0.050(5) 0.046(4) 0.004(4) 0.001(3) -0.007(3) C25 0.041(4) 0.043(5) 0.039(4) 0.007(4) 0.001(3) -0.007(3) C26 0.026(3) 0.044(4) 0.053(4) 0.003(4) 0.001(3) -0.011(3) C27 0.034(3) 0.038(4) 0.042(4) 0.009(3) 0.004(3) -0.010(3) C28 0.037(4) 0.055(5) 0.038(4) 0.007(4) 0.007(3) -0.004(3) C29 0.058(5) 0.056(5) 0.047(5) -0.002(4) 0.008(4) -0.013(4) C30 0.084(6) 0.087(7) 0.034(4) 0.010(5) 0.006(4) -0.003(5) C31 0.073(5) 0.064(6) 0.053(5) 0.027(5) 0.006(4) 0.014(5) C32 0.039(4) 0.050(5) 0.053(5) -0.002(4) 0.010(3) -0.013(4) C33 0.048(4) 0.048(5) 0.058(5) 0.004(4) 0.005(4) -0.007(4) C34 0.065(5) 0.049(5) 0.089(7) 0.008(5) 0.005(5) 0.001(4) C35 0.057(5) 0.061(6) 0.073(6) -0.005(5) 0.009(4) 0.001(4) C36 0.043(4) 0.068(6) 0.057(5) 0.000(4) 0.005(4) -0.008(4) C37 0.053(5) 0.058(6) 0.060(5) 0.010(4) 0.011(4) -0.003(4) C38 0.079(6) 0.090(8) 0.053(6) 0.030(5) 0.005(5) 0.007(5) C39 0.081(6) 0.071(7) 0.059(6) 0.009(5) 0.010(5) 0.009(5) C40 0.063(5) 0.068(6) 0.055(5) 0.007(5) 0.002(4) -0.003(4) C41 0.041(4) 0.057(5) 0.048(4) 0.012(4) 0.001(3) -0.006(4) _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 O1W H1WA 0.9261 . ? O1W H1WB 0.9266 . ? Pb1 O1 2.440(5) . ? Pb1 O2 2.492(6) . ? Pb1 N2 2.666(6) . ? Pb1 O3 2.688(7) . ? Pb1 N1 2.721(6) . ? Pb1 N4 2.811(7) . ? Pb1 C1 2.825(8) . ? Pb1 N5 2.826(6) . ? Pb1 O5 3.003(10) . ? O1 C1 1.257(9) . ? N1 C17 1.343(10) . ? N1 C6 1.355(9) . ? C1 O2 1.248(10) . ? C1 C2 1.503(11) . ? N2 C8 1.335(10) . ? N2 C7 1.370(8) . ? C2 C3 1.456(15) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? O3 N12 1.197(11) . ? N3 C12 1.320(8) . ? N3 C13 1.330(8) 3_665 ? C3 C4 1.488(16) . ? C3 H3B 0.9700 . ? C3 H3A 0.9700 . ? N4 C31 1.325(10) . ? N4 C18 1.356(8) . ? O4 N12 1.271(13) . ? C4 C5 1.565(16) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? N5 C20 1.327(9) . ? N5 C19 1.350(9) . ? O5 N12 1.269(13) . ? C5 C5 1.38(2) 3_766 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? N6 C25 1.313(9) . ? N6 C24 1.337(8) . ? C6 C14 1.405(9) . ? C6 C7 1.449(9) . ? N7 C26 1.325(8) . ? N7 C27 1.338(8) . ? C7 C11 1.392(9) . ? N8 C34 1.336(11) . ? N8 C33 1.348(9) . ? C8 C9 1.349(11) . ? C8 H8 0.9300 . ? N9 C38 1.333(11) . ? N9 C37 1.357(10) . ? C9 C10 1.360(10) . ? C9 H9 0.9300 . ? C10 C11 1.399(10) . ? C10 H10 0.9300 . ? C11 C12 1.470(9) . ? C12 C13 1.406(9) . ? C13 N3 1.330(8) 3_665 ? C13 C14 1.469(9) . ? C14 C15 1.374(9) . ? C15 C16 1.367(9) . ? C15 H15 0.9300 . ? C16 C17 1.368(11) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C28 1.398(10) . ? C18 C19 1.461(9) . ? C19 C23 1.403(9) . ? C20 C21 1.408(11) . ? C20 H20 0.9300 . ? C21 C22 1.378(10) . ? C21 H21 0.9300 . ? C22 C23 1.407(10) . ? C22 H22 0.9300 . ? C23 C24 1.451(10) . ? C24 C27 1.407(9) . ? C25 C26 1.407(9) . ? C25 C41 1.467(9) . ? C26 C32 1.477(10) . ? C27 C28 1.471(9) . ? C28 C29 1.394(10) . ? C29 C30 1.376(11) . ? C29 H29 0.9300 . ? C30 C31 1.396(12) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.397(10) . ? C32 C36 1.416(10) . ? C33 C37 1.463(11) . ? C34 C35 1.375(12) . ? C34 H34 0.9300 . ? C35 C36 1.370(10) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C41 1.390(11) . ? C38 C39 1.392(12) . ? C38 H38 0.9300 . ? C39 C40 1.384(11) . ? C39 H39 0.9300 . ? C40 C41 1.398(11) . ? C40 H40 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 H1WA O1W H1WB 63.2 . . ? O1 Pb1 O2 52.53(19) . . ? O1 Pb1 N2 74.18(18) . . ? O2 Pb1 N2 74.04(19) . . ? O1 Pb1 O3 76.6(2) . . ? O2 Pb1 O3 125.8(2) . . ? N2 Pb1 O3 75.39(19) . . ? O1 Pb1 N1 113.95(17) . . ? O2 Pb1 N1 69.6(2) . . ? N2 Pb1 N1 60.64(19) . . ? O3 Pb1 N1 127.4(2) . . ? O1 Pb1 N4 93.09(19) . . ? O2 Pb1 N4 73.10(19) . . ? N2 Pb1 N4 145.76(18) . . ? O3 Pb1 N4 133.4(2) . . ? N1 Pb1 N4 98.59(19) . . ? O1 Pb1 C1 26.3(2) . . ? O2 Pb1 C1 26.2(2) . . ? N2 Pb1 C1 71.6(2) . . ? O3 Pb1 C1 101.2(3) . . ? N1 Pb1 C1 91.5(2) . . ? N4 Pb1 C1 83.0(2) . . ? O1 Pb1 N5 77.58(16) . . ? O2 Pb1 N5 106.02(19) . . ? N2 Pb1 N5 143.45(18) . . ? O3 Pb1 N5 75.9(2) . . ? N1 Pb1 N5 154.99(19) . . ? N4 Pb1 N5 57.51(17) . . ? C1 Pb1 N5 92.51(19) . . ? O1 Pb1 O5 114.4(3) . . ? O2 Pb1 O5 143.3(3) . . ? N2 Pb1 O5 69.3(2) . . ? O3 Pb1 O5 42.8(3) . . ? N1 Pb1 O5 92.5(3) . . ? N4 Pb1 O5 143.0(3) . . ? C1 Pb1 O5 132.2(3) . . ? N5 Pb1 O5 102.9(2) . . ? C1 O1 Pb1 94.2(5) . . ? C17 N1 C6 118.0(7) . . ? C17 N1 Pb1 120.6(5) . . ? C6 N1 Pb1 120.1(5) . . ? O2 C1 O1 121.2(7) . . ? O2 C1 C2 119.1(8) . . ? O1 C1 C2 119.7(8) . . ? O2 C1 Pb1 61.8(4) . . ? O1 C1 Pb1 59.4(4) . . ? C2 C1 Pb1 178.1(7) . . ? C1 O2 Pb1 92.0(4) . . ? C8 N2 C7 116.3(6) . . ? C8 N2 Pb1 121.4(5) . . ? C7 N2 Pb1 121.5(5) . . ? C3 C2 C1 118.8(9) . . ? C3 C2 H2A 107.6 . . ? C1 C2 H2A 107.6 . . ? C3 C2 H2B 107.6 . . ? C1 C2 H2B 107.6 . . ? H2A C2 H2B 107.0 . . ? N12 O3 Pb1 104.9(8) . . ? C12 N3 C13 117.0(6) . 3_665 ? C2 C3 C4 115.2(11) . . ? C2 C3 H3B 108.5 . . ? C4 C3 H3B 108.5 . . ? C2 C3 H3A 108.5 . . ? C4 C3 H3A 108.5 . . ? H3B C3 H3A 107.5 . . ? C31 N4 C18 116.2(7) . . ? C31 N4 Pb1 119.4(5) . . ? C18 N4 Pb1 124.3(5) . . ? C3 C4 C5 113.1(10) . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.8 . . ? C20 N5 C19 119.2(6) . . ? C20 N5 Pb1 118.0(5) . . ? C19 N5 Pb1 122.8(4) . . ? N12 O5 Pb1 87.6(7) . . ? C5 C5 C4 116.6(15) 3_766 . ? C5 C5 H5A 108.1 3_766 . ? C4 C5 H5A 108.1 . . ? C5 C5 H5B 108.1 3_766 . ? C4 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? C25 N6 C24 118.0(6) . . ? N1 C6 C14 121.6(7) . . ? N1 C6 C7 117.7(6) . . ? C14 C6 C7 120.6(6) . . ? C26 N7 C27 116.7(6) . . ? N2 C7 C11 121.3(7) . . ? N2 C7 C6 117.9(6) . . ? C11 C7 C6 120.8(6) . . ? C34 N8 C33 117.4(7) . . ? N2 C8 C9 125.6(7) . . ? N2 C8 H8 117.2 . . ? C9 C8 H8 117.2 . . ? C38 N9 C37 115.4(7) . . ? C8 C9 C10 118.8(7) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C9 C10 C11 118.8(7) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C7 C11 C10 119.1(6) . . ? C7 C11 C12 119.7(6) . . ? C10 C11 C12 121.3(6) . . ? O3 N12 O5 116.6(12) . . ? O3 N12 O4 119.0(15) . . ? O5 N12 O4 124.4(13) . . ? N3 C12 C13 121.3(6) . . ? N3 C12 C11 119.2(6) . . ? C13 C12 C11 119.5(6) . . ? N3 C13 C12 121.7(6) 3_665 . ? N3 C13 C14 117.7(6) 3_665 . ? C12 C13 C14 120.6(6) . . ? C15 C14 C6 118.6(6) . . ? C15 C14 C13 122.5(6) . . ? C6 C14 C13 118.8(6) . . ? C16 C15 C14 119.2(7) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 120.0(7) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? N1 C17 C16 122.5(7) . . ? N1 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? N4 C18 C28 123.2(7) . . ? N4 C18 C19 116.3(6) . . ? C28 C18 C19 120.4(6) . . ? N5 C19 C23 121.1(6) . . ? N5 C19 C18 118.7(6) . . ? C23 C19 C18 120.1(6) . . ? N5 C20 C21 123.2(7) . . ? N5 C20 H20 118.4 . . ? C21 C20 H20 118.4 . . ? C22 C21 C20 118.3(8) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C21 C22 C23 118.8(7) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C19 C23 C22 119.3(7) . . ? C19 C23 C24 119.5(6) . . ? C22 C23 C24 121.2(7) . . ? N6 C24 C27 120.4(6) . . ? N6 C24 C23 118.6(6) . . ? C27 C24 C23 121.0(6) . . ? N6 C25 C26 121.5(6) . . ? N6 C25 C41 118.5(6) . . ? C26 C25 C41 120.0(7) . . ? N7 C26 C25 121.7(7) . . ? N7 C26 C32 119.7(6) . . ? C25 C26 C32 118.6(6) . . ? N7 C27 C24 121.8(6) . . ? N7 C27 C28 119.0(6) . . ? C24 C27 C28 119.1(6) . . ? C29 C28 C18 118.9(7) . . ? C29 C28 C27 121.3(7) . . ? C18 C28 C27 119.7(6) . . ? C30 C29 C28 118.0(8) . . ? C30 C29 H29 121.0 . . ? C28 C29 H29 121.0 . . ? C29 C30 C31 118.9(7) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? N4 C31 C30 124.7(7) . . ? N4 C31 H31 117.7 . . ? C30 C31 H31 117.7 . . ? C33 C32 C36 118.1(7) . . ? C33 C32 C26 120.8(7) . . ? C36 C32 C26 121.2(7) . . ? N8 C33 C32 122.3(7) . . ? N8 C33 C37 117.6(7) . . ? C32 C33 C37 120.1(7) . . ? N8 C34 C35 124.8(8) . . ? N8 C34 H34 117.6 . . ? C35 C34 H34 117.6 . . ? C36 C35 C34 118.2(9) . . ? C36 C35 H35 120.9 . . ? C34 C35 H35 120.9 . . ? C35 C36 C32 119.2(8) . . ? C35 C36 H36 120.4 . . ? C32 C36 H36 120.4 . . ? N9 C37 C41 123.1(7) . . ? N9 C37 C33 117.3(8) . . ? C41 C37 C33 119.5(7) . . ? N9 C38 C39 126.4(8) . . ? N9 C38 H38 116.8 . . ? C39 C38 H38 116.8 . . ? C40 C39 C38 116.9(8) . . ? C40 C39 H39 121.6 . . ? C38 C39 H39 121.6 . . ? C39 C40 C41 118.9(8) . . ? C39 C40 H40 120.5 . . ? C41 C40 H40 120.5 . . ? C37 C41 C40 119.1(7) . . ? C37 C41 C25 121.0(7) . . ? C40 C41 C25 119.9(7) . . ? 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 O2 Pb1 O1 C1 1.4(4) . . . . ? N2 Pb1 O1 C1 -80.4(5) . . . . ? O3 Pb1 O1 C1 -158.7(5) . . . . ? N1 Pb1 O1 C1 -33.5(5) . . . . ? N4 Pb1 O1 C1 67.3(5) . . . . ? N5 Pb1 O1 C1 123.1(5) . . . . ? O5 Pb1 O1 C1 -138.2(5) . . . . ? O1 Pb1 N1 C17 125.6(5) . . . . ? O2 Pb1 N1 C17 96.6(6) . . . . ? N2 Pb1 N1 C17 179.3(6) . . . . ? O3 Pb1 N1 C17 -143.3(6) . . . . ? N4 Pb1 N1 C17 28.3(6) . . . . ? C1 Pb1 N1 C17 111.4(6) . . . . ? N5 Pb1 N1 C17 12.3(8) . . . . ? O5 Pb1 N1 C17 -116.2(6) . . . . ? O1 Pb1 N1 C6 -41.1(5) . . . . ? O2 Pb1 N1 C6 -70.1(5) . . . . ? N2 Pb1 N1 C6 12.5(5) . . . . ? O3 Pb1 N1 C6 50.0(6) . . . . ? N4 Pb1 N1 C6 -138.4(5) . . . . ? C1 Pb1 N1 C6 -55.3(5) . . . . ? N5 Pb1 N1 C6 -154.4(5) . . . . ? O5 Pb1 N1 C6 77.0(5) . . . . ? Pb1 O1 C1 O2 -2.6(8) . . . . ? Pb1 O1 C1 C2 178.1(8) . . . . ? O1 Pb1 C1 O2 177.5(8) . . . . ? N2 Pb1 C1 O2 -91.1(5) . . . . ? O3 Pb1 C1 O2 -161.5(5) . . . . ? N1 Pb1 C1 O2 -32.8(5) . . . . ? N4 Pb1 C1 O2 65.6(5) . . . . ? N5 Pb1 C1 O2 122.5(5) . . . . ? O5 Pb1 C1 O2 -127.6(5) . . . . ? O2 Pb1 C1 O1 -177.5(8) . . . . ? N2 Pb1 C1 O1 91.4(5) . . . . ? O3 Pb1 C1 O1 21.1(5) . . . . ? N1 Pb1 C1 O1 149.7(5) . . . . ? N4 Pb1 C1 O1 -111.8(5) . . . . ? N5 Pb1 C1 O1 -55.0(5) . . . . ? O5 Pb1 C1 O1 55.0(6) . . . . ? O1 Pb1 C1 C2 -64(20) . . . . ? O2 Pb1 C1 C2 119(21) . . . . ? N2 Pb1 C1 C2 27(20) . . . . ? O3 Pb1 C1 C2 -43(21) . . . . ? N1 Pb1 C1 C2 86(21) . . . . ? N4 Pb1 C1 C2 -176(100) . . . . ? N5 Pb1 C1 C2 -119(21) . . . . ? O5 Pb1 C1 C2 -9(21) . . . . ? O1 C1 O2 Pb1 2.6(8) . . . . ? C2 C1 O2 Pb1 -178.1(8) . . . . ? O1 Pb1 O2 C1 -1.4(4) . . . . ? N2 Pb1 O2 C1 80.6(5) . . . . ? O3 Pb1 O2 C1 22.6(6) . . . . ? N1 Pb1 O2 C1 144.7(5) . . . . ? N4 Pb1 O2 C1 -109.1(5) . . . . ? N5 Pb1 O2 C1 -61.3(5) . . . . ? O5 Pb1 O2 C1 79.5(7) . . . . ? O1 Pb1 N2 C8 -51.3(6) . . . . ? O2 Pb1 N2 C8 -106.0(6) . . . . ? O3 Pb1 N2 C8 28.6(6) . . . . ? N1 Pb1 N2 C8 178.7(6) . . . . ? N4 Pb1 N2 C8 -122.8(6) . . . . ? C1 Pb1 N2 C8 -78.7(6) . . . . ? N5 Pb1 N2 C8 -10.5(7) . . . . ? O5 Pb1 N2 C8 73.2(6) . . . . ? O1 Pb1 N2 C7 118.2(5) . . . . ? O2 Pb1 N2 C7 63.4(5) . . . . ? O3 Pb1 N2 C7 -162.0(6) . . . . ? N1 Pb1 N2 C7 -11.9(5) . . . . ? N4 Pb1 N2 C7 46.6(7) . . . . ? C1 Pb1 N2 C7 90.7(5) . . . . ? N5 Pb1 N2 C7 158.9(4) . . . . ? O5 Pb1 N2 C7 -117.4(6) . . . . ? O2 C1 C2 C3 169.6(10) . . . . ? O1 C1 C2 C3 -11.1(15) . . . . ? Pb1 C1 C2 C3 52(21) . . . . ? O1 Pb1 O3 N12 168.7(8) . . . . ? O2 Pb1 O3 N12 149.3(8) . . . . ? N2 Pb1 O3 N12 91.8(8) . . . . ? N1 Pb1 O3 N12 58.6(8) . . . . ? N4 Pb1 O3 N12 -109.9(8) . . . . ? C1 Pb1 O3 N12 159.2(8) . . . . ? N5 Pb1 O3 N12 -111.0(8) . . . . ? O5 Pb1 O3 N12 16.7(8) . . . . ? C1 C2 C3 C4 -85.6(13) . . . . ? O1 Pb1 N4 C31 -104.9(6) . . . . ? O2 Pb1 N4 C31 -55.7(6) . . . . ? N2 Pb1 N4 C31 -38.9(8) . . . . ? O3 Pb1 N4 C31 -179.3(6) . . . . ? N1 Pb1 N4 C31 9.8(6) . . . . ? C1 Pb1 N4 C31 -80.6(6) . . . . ? N5 Pb1 N4 C31 -178.1(7) . . . . ? O5 Pb1 N4 C31 115.7(7) . . . . ? O1 Pb1 N4 C18 78.9(5) . . . . ? O2 Pb1 N4 C18 128.2(6) . . . . ? N2 Pb1 N4 C18 145.0(5) . . . . ? O3 Pb1 N4 C18 4.6(7) . . . . ? N1 Pb1 N4 C18 -166.3(5) . . . . ? C1 Pb1 N4 C18 103.3(6) . . . . ? N5 Pb1 N4 C18 5.8(5) . . . . ? O5 Pb1 N4 C18 -60.4(7) . . . . ? C2 C3 C4 C5 -178.2(10) . . . . ? O1 Pb1 N5 C20 72.6(5) . . . . ? O2 Pb1 N5 C20 117.2(5) . . . . ? N2 Pb1 N5 C20 32.6(6) . . . . ? O3 Pb1 N5 C20 -6.5(5) . . . . ? N1 Pb1 N5 C20 -166.7(5) . . . . ? N4 Pb1 N5 C20 174.4(6) . . . . ? C1 Pb1 N5 C20 94.4(5) . . . . ? O5 Pb1 N5 C20 -40.0(6) . . . . ? O1 Pb1 N5 C19 -106.0(5) . . . . ? O2 Pb1 N5 C19 -61.3(5) . . . . ? N2 Pb1 N5 C19 -146.0(5) . . . . ? O3 Pb1 N5 C19 175.0(5) . . . . ? N1 Pb1 N5 C19 14.8(7) . . . . ? N4 Pb1 N5 C19 -4.1(4) . . . . ? C1 Pb1 N5 C19 -84.1(5) . . . . ? O5 Pb1 N5 C19 141.5(5) . . . . ? O1 Pb1 O5 N12 -45.3(8) . . . . ? O2 Pb1 O5 N12 -104.7(8) . . . . ? N2 Pb1 O5 N12 -105.8(8) . . . . ? O3 Pb1 O5 N12 -15.2(7) . . . . ? N1 Pb1 O5 N12 -163.1(8) . . . . ? N4 Pb1 O5 N12 89.1(9) . . . . ? C1 Pb1 O5 N12 -68.8(8) . . . . ? N5 Pb1 O5 N12 36.8(8) . . . . ? C3 C4 C5 C5 -177.2(15) . . . 3_766 ? C17 N1 C6 C14 0.7(10) . . . . ? Pb1 N1 C6 C14 167.8(4) . . . . ? C17 N1 C6 C7 -179.9(6) . . . . ? Pb1 N1 C6 C7 -12.8(8) . . . . ? C8 N2 C7 C11 0.0(10) . . . . ? Pb1 N2 C7 C11 -169.9(5) . . . . ? C8 N2 C7 C6 -179.0(7) . . . . ? Pb1 N2 C7 C6 11.1(8) . . . . ? N1 C6 C7 N2 1.4(9) . . . . ? C14 C6 C7 N2 -179.2(6) . . . . ? N1 C6 C7 C11 -177.6(6) . . . . ? C14 C6 C7 C11 1.8(10) . . . . ? C7 N2 C8 C9 -1.3(12) . . . . ? Pb1 N2 C8 C9 168.6(7) . . . . ? N2 C8 C9 C10 2.0(14) . . . . ? C8 C9 C10 C11 -1.2(12) . . . . ? N2 C7 C11 C10 0.6(10) . . . . ? C6 C7 C11 C10 179.6(6) . . . . ? N2 C7 C11 C12 179.1(6) . . . . ? C6 C7 C11 C12 -2.0(10) . . . . ? C9 C10 C11 C7 0.0(10) . . . . ? C9 C10 C11 C12 -178.4(7) . . . . ? Pb1 O3 N12 O5 -31.1(13) . . . . ? Pb1 O3 N12 O4 145.3(10) . . . . ? Pb1 O5 N12 O3 26.6(11) . . . . ? Pb1 O5 N12 O4 -149.7(12) . . . . ? C13 N3 C12 C13 0.7(10) 3_665 . . . ? C13 N3 C12 C11 -178.7(5) 3_665 . . . ? C7 C11 C12 N3 -179.1(6) . . . . ? C10 C11 C12 N3 -0.7(9) . . . . ? C7 C11 C12 C13 1.5(9) . . . . ? C10 C11 C12 C13 179.9(6) . . . . ? N3 C12 C13 N3 -0.7(10) . . . 3_665 ? C11 C12 C13 N3 178.7(5) . . . 3_665 ? N3 C12 C13 C14 179.8(5) . . . . ? C11 C12 C13 C14 -0.8(9) . . . . ? N1 C6 C14 C15 -0.8(9) . . . . ? C7 C6 C14 C15 179.8(6) . . . . ? N1 C6 C14 C13 178.3(6) . . . . ? C7 C6 C14 C13 -1.1(9) . . . . ? N3 C13 C14 C15 0.2(9) 3_665 . . . ? C12 C13 C14 C15 179.7(6) . . . . ? N3 C13 C14 C6 -178.9(5) 3_665 . . . ? C12 C13 C14 C6 0.6(9) . . . . ? C6 C14 C15 C16 0.8(9) . . . . ? C13 C14 C15 C16 -178.3(6) . . . . ? C14 C15 C16 C17 -0.8(11) . . . . ? C6 N1 C17 C16 -0.7(11) . . . . ? Pb1 N1 C17 C16 -167.7(6) . . . . ? C15 C16 C17 N1 0.8(12) . . . . ? C31 N4 C18 C28 0.1(10) . . . . ? Pb1 N4 C18 C28 176.3(5) . . . . ? C31 N4 C18 C19 176.7(6) . . . . ? Pb1 N4 C18 C19 -7.0(8) . . . . ? C20 N5 C19 C23 0.8(10) . . . . ? Pb1 N5 C19 C23 179.3(5) . . . . ? C20 N5 C19 C18 -175.8(6) . . . . ? Pb1 N5 C19 C18 2.7(8) . . . . ? N4 C18 C19 N5 2.7(9) . . . . ? C28 C18 C19 N5 179.4(6) . . . . ? N4 C18 C19 C23 -173.9(6) . . . . ? C28 C18 C19 C23 2.8(10) . . . . ? C19 N5 C20 C21 2.8(11) . . . . ? Pb1 N5 C20 C21 -175.8(6) . . . . ? N5 C20 C21 C22 -4.7(12) . . . . ? C20 C21 C22 C23 2.8(11) . . . . ? N5 C19 C23 C22 -2.4(10) . . . . ? C18 C19 C23 C22 174.1(6) . . . . ? N5 C19 C23 C24 179.5(6) . . . . ? C18 C19 C23 C24 -3.9(9) . . . . ? C21 C22 C23 C19 0.5(11) . . . . ? C21 C22 C23 C24 178.5(7) . . . . ? C25 N6 C24 C27 0.8(9) . . . . ? C25 N6 C24 C23 -178.7(6) . . . . ? C19 C23 C24 N6 -179.4(6) . . . . ? C22 C23 C24 N6 2.6(10) . . . . ? C19 C23 C24 C27 1.2(9) . . . . ? C22 C23 C24 C27 -176.8(6) . . . . ? C24 N6 C25 C26 -1.7(9) . . . . ? C24 N6 C25 C41 -179.7(6) . . . . ? C27 N7 C26 C25 -1.6(9) . . . . ? C27 N7 C26 C32 179.4(5) . . . . ? N6 C25 C26 N7 2.2(10) . . . . ? C41 C25 C26 N7 -179.8(6) . . . . ? N6 C25 C26 C32 -178.8(6) . . . . ? C41 C25 C26 C32 -0.8(9) . . . . ? C26 N7 C27 C24 0.7(9) . . . . ? C26 N7 C27 C28 177.2(5) . . . . ? N6 C24 C27 N7 -0.2(9) . . . . ? C23 C24 C27 N7 179.2(6) . . . . ? N6 C24 C27 C28 -176.7(6) . . . . ? C23 C24 C27 C28 2.7(9) . . . . ? N4 C18 C28 C29 -1.1(10) . . . . ? C19 C18 C28 C29 -177.6(6) . . . . ? N4 C18 C28 C27 177.6(6) . . . . ? C19 C18 C28 C27 1.1(9) . . . . ? N7 C27 C28 C29 -1.7(9) . . . . ? C24 C27 C28 C29 174.9(6) . . . . ? N7 C27 C28 C18 179.6(6) . . . . ? C24 C27 C28 C18 -3.8(9) . . . . ? C18 C28 C29 C30 2.2(10) . . . . ? C27 C28 C29 C30 -176.5(7) . . . . ? C28 C29 C30 C31 -2.3(12) . . . . ? C18 N4 C31 C30 -0.2(12) . . . . ? Pb1 N4 C31 C30 -176.7(7) . . . . ? C29 C30 C31 N4 1.4(14) . . . . ? N7 C26 C32 C33 -179.7(6) . . . . ? C25 C26 C32 C33 1.3(9) . . . . ? N7 C26 C32 C36 0.4(9) . . . . ? C25 C26 C32 C36 -178.7(6) . . . . ? C34 N8 C33 C32 -0.1(12) . . . . ? C34 N8 C33 C37 -179.0(7) . . . . ? C36 C32 C33 N8 -0.1(11) . . . . ? C26 C32 C33 N8 179.9(7) . . . . ? C36 C32 C33 C37 178.7(6) . . . . ? C26 C32 C33 C37 -1.3(10) . . . . ? C33 N8 C34 C35 0.5(13) . . . . ? N8 C34 C35 C36 -0.8(13) . . . . ? C34 C35 C36 C32 0.5(11) . . . . ? C33 C32 C36 C35 -0.1(10) . . . . ? C26 C32 C36 C35 179.9(6) . . . . ? C38 N9 C37 C41 -2.7(12) . . . . ? C38 N9 C37 C33 178.0(7) . . . . ? N8 C33 C37 N9 -1.0(10) . . . . ? C32 C33 C37 N9 -179.9(7) . . . . ? N8 C33 C37 C41 179.6(7) . . . . ? C32 C33 C37 C41 0.7(11) . . . . ? C37 N9 C38 C39 0.4(14) . . . . ? N9 C38 C39 C40 1.3(15) . . . . ? C38 C39 C40 C41 -0.8(13) . . . . ? N9 C37 C41 C40 3.2(12) . . . . ? C33 C37 C41 C40 -177.5(7) . . . . ? N9 C37 C41 C25 -179.5(7) . . . . ? C33 C37 C41 C25 -0.2(10) . . . . ? C39 C40 C41 C37 -1.3(12) . . . . ? C39 C40 C41 C25 -178.6(7) . . . . ? N6 C25 C41 C37 178.3(7) . . . . ? C26 C25 C41 C37 0.3(10) . . . . ? N6 C25 C41 C40 -4.4(10) . . . . ? C26 C25 C41 C40 177.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.467 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.120 data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 886625' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H64 N12 O14 Pb3' _chemical_formula_weight 1942.92 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.320(5) _cell_length_b 14.580(5) _cell_length_c 16.195(5) _cell_angle_alpha 86.729(5) _cell_angle_beta 84.156(5) _cell_angle_gamma 79.526(5) _cell_volume 3305.1(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.952 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1876 _exptl_absorpt_coefficient_mu 7.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.328 _exptl_absorpt_correction_T_max 0.340 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49449 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12860 _reflns_number_gt 9397 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _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^)+(0.0864P)^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 12860 _refine_ls_number_parameters 881 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.032 _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 -0.30211(3) 0.14365(3) 1.336706(19) 0.04912(11) Uani 1 1 d . . . Pb2 Pb -0.56825(2) 0.13660(2) 0.526663(18) 0.04364(11) Uani 1 1 d . . . Pb3 Pb 0.08524(2) 0.33925(2) 0.95157(2) 0.04163(10) Uani 1 1 d . . . O1 O -0.1481(5) 0.2192(7) 1.3263(5) 0.088(3) Uani 1 1 d . . . O2 O -0.2434(6) 0.2395(7) 1.4411(5) 0.095(3) Uani 1 1 d . . . O3 O -0.4571(5) 0.2326(5) 1.4072(4) 0.0618(17) Uani 1 1 d . . . O4 O -0.3838(6) 0.2908(5) 1.2946(4) 0.0677(19) Uani 1 1 d . . . O5 O -0.3134(7) 0.7292(7) 1.4454(6) 0.103(3) Uani 1 1 d . . . O6 O -0.2941(9) 0.7824(10) 1.5621(11) 0.175(7) Uani 1 1 d . . . O7 O -0.6122(6) -0.0074(5) 0.4231(4) 0.077(2) Uani 1 1 d . . . O8 O -0.6814(6) 0.0230(7) 0.5456(5) 0.092(3) Uani 1 1 d U . . O9 O -0.0394(4) 0.2582(5) 0.8963(4) 0.0583(16) Uani 1 1 d . . . O10 O 0.0789(4) 0.2922(5) 0.8089(4) 0.0637(18) Uani 1 1 d . . . O11 O -0.1532(5) -0.1767(5) 1.0270(4) 0.0647(18) Uani 1 1 d . . . O12 O -0.0625(4) -0.2300(4) 0.9180(3) 0.0480(14) Uani 1 1 d . . . C1 C -0.1743(5) 0.1653(6) 1.1453(5) 0.0400(18) Uani 1 1 d . . . H1A H -0.1301 0.1677 1.1832 0.048 Uiso 1 1 calc R . . C2 C -0.1465(5) 0.1793(6) 1.0609(5) 0.0396(18) Uani 1 1 d . . . H2A H -0.0858 0.1904 1.0424 0.048 Uiso 1 1 calc R . . C3 C -0.2147(5) 0.1757(5) 1.0057(5) 0.0342(17) Uani 1 1 d . . . H3A H -0.2008 0.1865 0.9490 0.041 Uiso 1 1 calc R . . C4 C -0.3035(5) 0.1560(5) 1.0362(4) 0.0315(15) Uani 1 1 d . . . C5 C -0.3772(5) 0.1508(5) 0.9814(4) 0.0353(17) Uani 1 1 d . . . C6 C -0.4633(5) 0.1279(5) 1.0110(4) 0.0304(15) Uani 1 1 d . . . C7 C -0.4850(5) 0.1122(5) 1.1007(4) 0.0323(16) Uani 1 1 d . . . C8 C -0.5691(5) 0.0890(6) 1.1359(5) 0.0405(18) Uani 1 1 d . . . H8A H -0.6152 0.0811 1.1017 0.049 Uiso 1 1 calc R . . C9 C -0.5872(5) 0.0770(6) 1.2205(5) 0.0431(19) Uani 1 1 d . . . H9A H -0.6446 0.0621 1.2445 0.052 Uiso 1 1 calc R . . C10 C -0.5147(5) 0.0884(6) 1.2684(5) 0.0435(19) Uani 1 1 d . . . H10A H -0.5259 0.0808 1.3257 0.052 Uiso 1 1 calc R . . C11 C -0.4151(5) 0.1206(5) 1.1538(4) 0.0352(17) Uani 1 1 d . . . C12 C -0.3241(5) 0.1416(5) 1.1213(4) 0.0350(16) Uani 1 1 d . . . C13 C -0.3875(5) 0.2426(6) 0.5979(5) 0.045(2) Uani 1 1 d . . . H13A H -0.3808 0.2604 0.5419 0.054 Uiso 1 1 calc R . . C14 C -0.3152(6) 0.2544(7) 0.6474(5) 0.052(2) Uani 1 1 d . . . H14A H -0.2612 0.2777 0.6253 0.063 Uiso 1 1 calc R . . C15 C -0.3294(5) 0.2295(6) 0.7299(5) 0.0404(19) Uani 1 1 d . . . H15A H -0.2850 0.2383 0.7654 0.048 Uiso 1 1 calc R . . C16 C -0.4084(5) 0.1914(6) 0.7623(4) 0.0370(17) Uani 1 1 d . . . C17 C -0.4245(5) 0.1653(5) 0.8511(4) 0.0308(15) Uani 1 1 d . . . C18 C -0.5122(5) 0.1396(5) 0.8799(4) 0.0320(16) Uani 1 1 d . . . C19 C -0.5821(5) 0.1322(5) 0.8238(4) 0.0349(16) Uani 1 1 d . . . C20 C -0.6696(5) 0.1100(6) 0.8530(5) 0.0394(18) Uani 1 1 d . . . H20A H -0.6856 0.1008 0.9096 0.047 Uiso 1 1 calc R . . C21 C -0.7329(5) 0.1020(6) 0.7958(5) 0.045(2) Uani 1 1 d . . . H21A H -0.7939 0.0911 0.8134 0.054 Uiso 1 1 calc R . . C22 C -0.7042(5) 0.1105(6) 0.7121(5) 0.044(2) Uani 1 1 d . . . H22A H -0.7452 0.1002 0.6740 0.053 Uiso 1 1 calc R . . C23 C -0.5610(5) 0.1465(5) 0.7393(4) 0.0314(16) Uani 1 1 d . . . C24 C -0.4747(5) 0.1810(5) 0.7081(4) 0.0349(17) Uani 1 1 d . . . C25 C 0.2648(5) 0.3616(6) 0.7868(5) 0.0434(19) Uani 1 1 d . . . H25A H 0.2113 0.3572 0.7601 0.052 Uiso 1 1 calc R . . C26 C 0.3479(6) 0.3781(6) 0.7390(5) 0.045(2) Uani 1 1 d . . . H26A H 0.3509 0.3798 0.6814 0.055 Uiso 1 1 calc R . . C27 C 0.4238(6) 0.3914(6) 0.7774(5) 0.0433(19) Uani 1 1 d . . . H27A H 0.4773 0.4069 0.7460 0.052 Uiso 1 1 calc R . . C28 C 0.4223(5) 0.3822(5) 0.8628(5) 0.0322(16) Uani 1 1 d . . . C29 C 0.5030(5) 0.3905(5) 0.9070(5) 0.0324(16) Uani 1 1 d . . . C30 C 0.4987(4) 0.3760(5) 0.9937(4) 0.0280(15) Uani 1 1 d . . . C31 C 0.4105(5) 0.3541(5) 1.0402(4) 0.0328(16) Uani 1 1 d . . . C32 C 0.4066(5) 0.3373(6) 1.1269(5) 0.0390(18) Uani 1 1 d . . . H32A H 0.4587 0.3395 1.1563 0.047 Uiso 1 1 calc R . . C33 C 0.3208(5) 0.3172(6) 1.1669(5) 0.0416(19) Uani 1 1 d . . . H33A H 0.3146 0.3051 1.2240 0.050 Uiso 1 1 calc R . . C34 C 0.2455(5) 0.3155(6) 1.1202(5) 0.045(2) Uani 1 1 d . . . H34A H 0.1885 0.3034 1.1477 0.054 Uiso 1 1 calc R . . C35 C 0.3335(5) 0.3494(5) 0.9980(5) 0.0326(16) Uani 1 1 d . . . C36 C 0.3370(5) 0.3620(5) 0.9072(5) 0.0333(16) Uani 1 1 d . . . C37 C 0.9051(6) 0.4908(8) 0.7873(6) 0.062(3) Uani 1 1 d . . . H37A H 0.9597 0.5095 0.7609 0.074 Uiso 1 1 calc R . . C38 C 0.8310(7) 0.4818(8) 0.7392(6) 0.064(3) Uani 1 1 d . . . H38A H 0.8392 0.4907 0.6818 0.076 Uiso 1 1 calc R . . C39 C 0.7452(6) 0.4597(6) 0.7766(5) 0.048(2) Uani 1 1 d . . . H39A H 0.6937 0.4579 0.7465 0.057 Uiso 1 1 calc R . . C40 C 0.7418(5) 0.4406(5) 0.8616(5) 0.0393(18) Uani 1 1 d . . . C41 C 0.6561(5) 0.4169(5) 0.9061(5) 0.0339(16) Uani 1 1 d . . . C42 C 0.6503(5) 0.4027(5) 0.9928(5) 0.0327(16) Uani 1 1 d . . . C43 C 0.7323(5) 0.4081(5) 1.0388(5) 0.0305(15) Uani 1 1 d . . . C44 C 0.7270(5) 0.3934(6) 1.1249(5) 0.0412(18) Uani 1 1 d . . . H44A H 0.6719 0.3805 1.1552 0.049 Uiso 1 1 calc R . . C45 C 0.8059(6) 0.3990(6) 1.1620(5) 0.0438(19) Uani 1 1 d . . . H45A H 0.8047 0.3905 1.2194 0.053 Uiso 1 1 calc R . . C46 C 0.8906(6) 0.4174(7) 1.1157(5) 0.051(2) Uani 1 1 d . . . H46A H 0.9445 0.4189 1.1428 0.061 Uiso 1 1 calc R . . C47 C 0.8168(5) 0.4289(5) 0.9955(5) 0.0367(17) Uani 1 1 d . . . C48 C 0.8196(5) 0.4472(6) 0.9058(5) 0.0426(19) Uani 1 1 d . . . C49 C -0.1702(10) 0.2462(11) 1.3974(7) 0.093(4) Uani 1 1 d . . . C50 C -0.0926(13) 0.2795(14) 1.4405(12) 0.137(6) Uiso 1 1 d . . . H50A H -0.0680 0.2302 1.4795 0.165 Uiso 1 1 calc R . . H50B H -0.0407 0.2868 1.3986 0.165 Uiso 1 1 calc R . . C51 C -0.117(2) 0.362(2) 1.4834(19) 0.226(12) Uiso 1 1 d . . . H51A H -0.0682 0.3693 1.5185 0.271 Uiso 1 1 calc R . . H51B H -0.1773 0.3642 1.5175 0.271 Uiso 1 1 calc R . . C52 C -0.126(3) 0.434(3) 1.419(2) 0.307(19) Uiso 1 1 d D . . H52A H -0.1728 0.4256 1.3823 0.369 Uiso 1 1 calc R . . H52B H -0.0650 0.4338 1.3860 0.369 Uiso 1 1 calc R . . C53 C -0.158(3) 0.529(2) 1.466(2) 0.270(16) Uiso 1 1 d D . . H53A H -0.2271 0.5397 1.4758 0.324 Uiso 1 1 calc R . . H53B H -0.1329 0.5202 1.5196 0.324 Uiso 1 1 calc R . . C54 C -0.1314(19) 0.6113(19) 1.4268(17) 0.198(10) Uiso 1 1 d . . . H54A H -0.1700 0.6326 1.3813 0.237 Uiso 1 1 calc R . . H54B H -0.0650 0.5989 1.4049 0.237 Uiso 1 1 calc R . . C55 C -0.147(2) 0.684(2) 1.490(2) 0.260(15) Uiso 1 1 d . . . H55A H -0.1069 0.7300 1.4739 0.312 Uiso 1 1 calc R . . H55B H -0.1292 0.6551 1.5434 0.312 Uiso 1 1 calc R . . C56 C -0.2629(13) 0.7347(15) 1.4985(17) 0.139(7) Uani 1 1 d . . . C57 C -0.4535(8) 0.2963(7) 1.3504(6) 0.060(3) Uani 1 1 d . . . C58 C -0.5322(11) 0.3816(8) 1.3523(7) 0.087(4) Uani 1 1 d . . . H58A H -0.5156 0.4260 1.3089 0.105 Uiso 1 1 calc R . . H58B H -0.5906 0.3628 1.3396 0.105 Uiso 1 1 calc R . . C59 C -0.5508(14) 0.4290(11) 1.4325(9) 0.126(6) Uani 1 1 d . . . H59A H -0.6095 0.4740 1.4301 0.152 Uiso 1 1 calc R . . H59B H -0.5631 0.3825 1.4755 0.152 Uiso 1 1 calc R . . C60 C -0.4840(11) 0.4748(11) 1.4587(7) 0.101(5) Uani 1 1 d . . . H60A H -0.4691 0.5205 1.4158 0.121 Uiso 1 1 calc R . . H60B H -0.4261 0.4301 1.4655 0.121 Uiso 1 1 calc R . . C61 C -0.6842(6) 0.0001(7) 0.4731(5) 0.051(2) Uani 1 1 d . . . C62 C -0.7765(6) -0.0186(8) 0.4481(6) 0.060(3) Uani 1 1 d . . . H62A H -0.7691 -0.0851 0.4405 0.073 Uiso 1 1 calc R . . H62B H -0.7862 0.0124 0.3942 0.073 Uiso 1 1 calc R . . C63 C -0.8683(7) 0.0103(8) 0.5054(6) 0.065(3) Uani 1 1 d . . . H63A H -0.8755 0.0762 0.5158 0.078 Uiso 1 1 calc R . . H63B H -0.8620 -0.0240 0.5583 0.078 Uiso 1 1 calc R . . C64 C -0.9588(7) -0.0074(10) 0.4697(6) 0.074(3) Uani 1 1 d . . . H64A H -0.9711 0.0341 0.4215 0.089 Uiso 1 1 calc R . . H64B H -0.9485 -0.0711 0.4517 0.089 Uiso 1 1 calc R . . C65 C -0.0027(6) 0.2653(7) 0.8250(6) 0.050(2) Uani 1 1 d . . . C66 C -0.0489(11) 0.2399(10) 0.7535(8) 0.098(5) Uani 1 1 d . . . H66A H -0.1139 0.2338 0.7731 0.118 Uiso 1 1 calc R . . H66B H -0.0524 0.2918 0.7129 0.118 Uiso 1 1 calc R . . C67 C -0.0074(10) 0.1604(11) 0.7132(10) 0.107(5) Uani 1 1 d . . . H67A H 0.0567 0.1665 0.6906 0.128 Uiso 1 1 calc R . . H67B H -0.0435 0.1535 0.6672 0.128 Uiso 1 1 calc R . . C68 C -0.0023(11) 0.0717(12) 0.7709(10) 0.108(5) Uani 1 1 d . B . H68A H 0.0384 0.0207 0.7419 0.130 Uiso 1 1 calc R . . H68B H 0.0287 0.0821 0.8193 0.130 Uiso 1 1 calc R . . C69 C -0.0912(12) 0.0422(12) 0.7996(10) 0.116(5) Uani 1 1 d . . . H69A H -0.1204 0.0231 0.7534 0.139 Uiso 1 1 calc R A 1 H69B H -0.1352 0.0925 0.8268 0.139 Uiso 1 1 calc R A 1 C70 C -0.0664(11) -0.0373(13) 0.8588(12) 0.069(3) Uani 0.603(15) 1 d P B 1 H70A H -0.0362 -0.0167 0.9036 0.083 Uiso 0.603(15) 1 calc PR B 1 H70B H -0.0207 -0.0856 0.8306 0.083 Uiso 0.603(15) 1 calc PR B 1 C71 C -0.1581(14) -0.0811(18) 0.8976(16) 0.069(3) Uani 0.603(15) 1 d P B 1 H71A H -0.2027 -0.0357 0.9301 0.083 Uiso 0.603(15) 1 calc PR B 1 H71B H -0.1907 -0.1008 0.8538 0.083 Uiso 0.603(15) 1 calc PR B 1 C70' C -0.1308(17) -0.056(2) 0.8290(19) 0.069(3) Uani 0.397(15) 1 d P B 2 H70C H -0.1929 -0.0545 0.8096 0.083 Uiso 0.397(15) 1 calc PR B 2 H70D H -0.0873 -0.1091 0.8053 0.083 Uiso 0.397(15) 1 calc PR B 2 C71' C -0.137(2) -0.065(3) 0.917(2) 0.069(3) Uani 0.397(15) 1 d P B 2 H71C H -0.2007 -0.0362 0.9390 0.083 Uiso 0.397(15) 1 calc PR B 2 H71D H -0.0922 -0.0314 0.9373 0.083 Uiso 0.397(15) 1 calc PR B 2 C72 C -0.1178(7) -0.1662(7) 0.9535(6) 0.057(2) Uani 1 1 d . . . N1 N -0.2627(4) 0.1482(4) 1.1757(4) 0.0353(14) Uani 1 1 d . . . N2 N -0.4313(5) 0.1091(5) 1.2384(4) 0.0423(16) Uani 1 1 d . . . N3 N -0.4661(4) 0.2069(5) 0.6269(4) 0.0422(16) Uani 1 1 d . . . N4 N -0.6199(5) 0.1329(5) 0.6838(4) 0.0436(16) Uani 1 1 d . . . N5 N -0.3568(4) 0.1704(4) 0.8995(4) 0.0334(14) Uani 1 1 d . . . N6 N -0.5322(4) 0.1217(4) 0.9621(4) 0.0332(13) Uani 1 1 d . . . N7 N 0.2605(4) 0.3520(5) 0.8691(4) 0.0406(15) Uani 1 1 d . . . N8 N 0.2501(4) 0.3301(5) 1.0386(4) 0.0367(15) Uani 1 1 d . . . N9 N 0.9003(4) 0.4739(5) 0.8680(5) 0.0490(18) Uani 1 1 d . . . N10 N 0.8934(5) 0.4322(5) 1.0352(4) 0.0475(17) Uani 1 1 d . . . N11 N 0.5822(4) 0.4103(4) 0.8635(4) 0.0348(14) Uani 1 1 d . . . N12 N 0.5715(4) 0.3817(4) 1.0366(4) 0.0314(13) Uani 1 1 d . . . O1W O 0.0184(6) 0.2721(7) 1.2507(5) 0.093(3) Uani 1 1 d . . . O2W O -0.8042(9) 0.1888(13) 0.3018(7) 0.188(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 0.0609(2) 0.0612(2) 0.03033(17) 0.00598(14) -0.00831(14) -0.02440(17) Pb2 0.05290(19) 0.0512(2) 0.03066(17) -0.00057(13) -0.00759(13) -0.01761(15) Pb3 0.03156(15) 0.0494(2) 0.04535(19) -0.00219(14) 0.00143(12) -0.01357(13) O1 0.077(5) 0.152(8) 0.052(4) -0.019(5) 0.004(4) -0.062(5) O2 0.096(6) 0.153(8) 0.051(4) -0.031(5) 0.032(4) -0.077(6) O3 0.075(4) 0.075(5) 0.035(3) 0.006(3) 0.006(3) -0.022(4) O4 0.100(5) 0.057(4) 0.045(4) 0.002(3) 0.011(4) -0.024(4) O5 0.095(6) 0.110(7) 0.088(6) -0.004(5) -0.033(5) 0.033(6) O6 0.098(8) 0.172(13) 0.270(18) -0.067(12) -0.123(11) 0.013(8) O7 0.102(6) 0.083(5) 0.055(4) -0.007(4) -0.002(4) -0.044(5) O8 0.106(5) 0.140(6) 0.051(4) -0.011(4) 0.002(4) -0.076(5) O9 0.044(3) 0.073(5) 0.061(4) -0.002(3) 0.001(3) -0.022(3) O10 0.048(3) 0.096(5) 0.053(4) -0.010(4) -0.004(3) -0.028(4) O11 0.066(4) 0.054(4) 0.068(5) -0.011(3) 0.025(3) -0.008(3) O12 0.039(3) 0.065(4) 0.040(3) -0.004(3) 0.008(2) -0.013(3) C1 0.023(3) 0.058(5) 0.042(4) -0.004(4) -0.010(3) -0.011(3) C2 0.028(3) 0.053(5) 0.040(4) -0.001(4) -0.002(3) -0.011(3) C3 0.028(3) 0.043(5) 0.031(4) 0.001(3) 0.001(3) -0.007(3) C4 0.032(3) 0.031(4) 0.032(4) -0.003(3) 0.000(3) -0.009(3) C5 0.047(4) 0.028(4) 0.029(4) -0.003(3) -0.005(3) -0.002(3) C6 0.029(3) 0.032(4) 0.029(4) -0.002(3) -0.004(3) -0.004(3) C7 0.042(4) 0.028(4) 0.026(4) -0.004(3) -0.003(3) -0.005(3) C8 0.040(4) 0.045(5) 0.039(4) -0.006(4) -0.001(3) -0.016(4) C9 0.032(4) 0.053(5) 0.046(5) -0.002(4) -0.003(3) -0.012(4) C10 0.040(4) 0.059(6) 0.035(4) -0.006(4) 0.003(3) -0.020(4) C11 0.042(4) 0.033(4) 0.029(4) -0.001(3) 0.002(3) -0.002(3) C12 0.044(4) 0.034(4) 0.027(4) -0.002(3) -0.006(3) -0.005(3) C13 0.041(4) 0.069(6) 0.027(4) 0.005(4) -0.008(3) -0.015(4) C14 0.047(5) 0.079(7) 0.036(5) 0.000(4) 0.007(4) -0.033(5) C15 0.028(3) 0.062(5) 0.035(4) 0.001(4) -0.007(3) -0.016(4) C16 0.041(4) 0.041(5) 0.028(4) -0.001(3) 0.009(3) -0.012(3) C17 0.034(4) 0.033(4) 0.024(4) -0.004(3) 0.001(3) -0.004(3) C18 0.033(4) 0.028(4) 0.033(4) -0.001(3) -0.007(3) 0.003(3) C19 0.046(4) 0.031(4) 0.028(4) 0.000(3) 0.000(3) -0.011(3) C20 0.035(4) 0.053(5) 0.033(4) -0.006(4) 0.003(3) -0.014(4) C21 0.018(3) 0.063(6) 0.056(5) -0.008(4) -0.017(3) -0.002(3) C22 0.022(3) 0.066(6) 0.046(5) -0.007(4) -0.013(3) -0.007(3) C23 0.030(3) 0.036(4) 0.028(4) -0.003(3) -0.006(3) -0.003(3) C24 0.040(4) 0.037(4) 0.026(4) 0.000(3) -0.001(3) -0.003(3) C25 0.033(4) 0.054(5) 0.046(5) -0.005(4) -0.008(3) -0.012(4) C26 0.042(4) 0.056(5) 0.038(4) -0.003(4) -0.008(4) -0.005(4) C27 0.041(4) 0.041(5) 0.046(5) -0.003(4) 0.008(4) -0.010(4) C28 0.028(3) 0.030(4) 0.039(4) -0.003(3) -0.005(3) -0.004(3) C29 0.026(3) 0.033(4) 0.041(4) -0.006(3) 0.001(3) -0.014(3) C30 0.024(3) 0.028(4) 0.031(4) 0.002(3) 0.003(3) -0.006(3) C31 0.034(4) 0.033(4) 0.030(4) -0.005(3) 0.010(3) -0.007(3) C32 0.034(4) 0.047(5) 0.038(4) 0.006(4) 0.003(3) -0.019(3) C33 0.034(4) 0.047(5) 0.045(5) -0.004(4) -0.001(3) -0.010(4) C34 0.032(4) 0.053(5) 0.051(5) 0.004(4) 0.003(3) -0.022(4) C35 0.038(4) 0.022(4) 0.036(4) 0.001(3) 0.007(3) -0.007(3) C36 0.025(3) 0.035(4) 0.040(4) 0.001(3) 0.001(3) -0.007(3) C37 0.047(5) 0.087(8) 0.057(6) 0.004(5) 0.008(4) -0.035(5) C38 0.053(5) 0.106(9) 0.037(5) -0.001(5) 0.003(4) -0.031(6) C39 0.035(4) 0.060(6) 0.048(5) 0.002(4) -0.001(4) -0.009(4) C40 0.038(4) 0.033(4) 0.049(5) -0.014(4) -0.004(3) -0.007(3) C41 0.030(3) 0.023(4) 0.049(5) -0.001(3) -0.008(3) -0.003(3) C42 0.023(3) 0.032(4) 0.045(4) -0.003(3) -0.004(3) -0.009(3) C43 0.026(3) 0.029(4) 0.038(4) 0.000(3) -0.010(3) -0.006(3) C44 0.030(4) 0.052(5) 0.042(5) -0.004(4) 0.001(3) -0.012(3) C45 0.043(4) 0.047(5) 0.040(4) -0.004(4) -0.006(3) -0.003(4) C46 0.044(4) 0.067(6) 0.047(5) -0.013(4) -0.004(4) -0.020(4) C47 0.027(3) 0.035(4) 0.048(5) -0.005(3) 0.001(3) -0.008(3) C48 0.034(4) 0.040(5) 0.053(5) -0.008(4) 0.004(4) -0.007(3) C49 0.099(9) 0.154(13) 0.046(6) -0.015(7) -0.003(6) -0.078(9) C56 0.089(12) 0.129(16) 0.20(2) -0.038(15) -0.036(14) 0.000(11) C57 0.090(7) 0.069(7) 0.032(5) -0.008(5) -0.004(5) -0.043(6) C58 0.145(12) 0.056(7) 0.056(7) -0.019(5) -0.006(7) -0.004(7) C59 0.203(19) 0.088(11) 0.090(11) -0.028(9) 0.015(11) -0.039(12) C60 0.139(12) 0.123(12) 0.054(7) -0.014(7) 0.014(7) -0.067(10) C61 0.052(5) 0.073(7) 0.032(5) -0.003(4) -0.006(4) -0.024(5) C62 0.043(5) 0.086(7) 0.056(6) -0.008(5) -0.020(4) -0.010(5) C63 0.080(7) 0.064(7) 0.055(6) -0.016(5) 0.005(5) -0.026(6) C64 0.071(7) 0.108(9) 0.049(6) -0.012(6) 0.001(5) -0.028(7) C65 0.037(4) 0.061(6) 0.055(6) -0.012(5) 0.000(4) -0.013(4) C66 0.138(12) 0.093(10) 0.085(9) -0.019(8) -0.050(8) -0.051(9) C67 0.088(9) 0.116(12) 0.125(13) -0.009(11) -0.050(9) -0.022(9) C68 0.108(11) 0.117(13) 0.100(11) -0.037(10) 0.008(9) -0.017(10) C69 0.109(12) 0.122(13) 0.106(12) -0.005(10) -0.009(9) 0.005(10) C70 0.038(6) 0.076(8) 0.093(10) 0.013(7) -0.019(5) -0.008(5) C71 0.038(6) 0.076(8) 0.093(10) 0.013(7) -0.019(5) -0.008(5) C70' 0.038(6) 0.076(8) 0.093(10) 0.013(7) -0.019(5) -0.008(5) C71' 0.038(6) 0.076(8) 0.093(10) 0.013(7) -0.019(5) -0.008(5) C72 0.057(5) 0.044(5) 0.066(6) -0.002(5) 0.008(5) -0.010(4) N1 0.037(3) 0.042(4) 0.029(3) -0.003(3) -0.008(3) -0.011(3) N2 0.058(4) 0.044(4) 0.025(3) 0.002(3) -0.001(3) -0.014(3) N3 0.040(3) 0.060(5) 0.028(3) -0.004(3) 0.001(3) -0.015(3) N4 0.052(4) 0.054(4) 0.030(3) -0.003(3) -0.005(3) -0.022(3) N5 0.035(3) 0.040(4) 0.024(3) -0.003(3) 0.002(2) -0.008(3) N6 0.040(3) 0.030(3) 0.028(3) -0.001(3) -0.003(3) -0.004(3) N7 0.034(3) 0.049(4) 0.042(4) -0.006(3) -0.002(3) -0.014(3) N8 0.027(3) 0.046(4) 0.037(4) 0.001(3) 0.007(3) -0.011(3) N9 0.028(3) 0.067(5) 0.055(5) 0.003(4) -0.004(3) -0.021(3) N10 0.043(4) 0.056(5) 0.048(4) -0.007(3) -0.007(3) -0.017(3) N11 0.028(3) 0.031(3) 0.047(4) -0.006(3) -0.002(3) -0.007(3) N12 0.026(3) 0.034(3) 0.033(3) -0.003(3) 0.004(2) -0.005(2) O1W 0.081(5) 0.135(8) 0.066(5) -0.008(5) 0.000(4) -0.030(5) O2W 0.119(9) 0.32(2) 0.102(9) 0.057(11) 0.009(7) -0.013(11) _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 O4 2.349(7) . ? Pb1 O2 2.551(8) . ? Pb1 O3 2.553(7) . ? Pb1 N1 2.611(6) . ? Pb1 O1 2.625(7) . ? Pb1 N2 2.692(7) . ? Pb1 C57 2.812(12) . ? Pb2 O5 2.376(8) 2_467 ? Pb2 O8 2.506(8) . ? Pb2 N4 2.577(6) . ? Pb2 O6 2.623(11) 2_467 ? Pb2 N3 2.654(6) . ? Pb2 C56 2.828(19) 2_467 ? Pb3 O11 2.412(7) 2_557 ? Pb3 O10 2.462(6) . ? Pb3 O9 2.568(6) . ? Pb3 O12 2.602(6) 2_557 ? Pb3 N7 2.752(6) . ? Pb3 C65 2.867(9) . ? Pb3 C72 2.868(10) 2_557 ? O1 C49 1.231(13) . ? O2 C49 1.219(13) . ? O3 C57 1.272(11) . ? O4 C57 1.270(12) . ? O5 C56 1.19(2) . ? O5 Pb2 2.376(8) 2_467 ? O6 C56 1.27(2) . ? O6 Pb2 2.623(11) 2_467 ? O7 C61 1.237(11) . ? O8 C61 1.246(11) . ? O9 C65 1.226(10) . ? O10 C65 1.296(10) . ? O11 C72 1.258(11) . ? O11 Pb3 2.412(7) 2_557 ? O12 C72 1.235(10) . ? O12 Pb3 2.602(6) 2_557 ? C1 N1 1.371(9) . ? C1 C2 1.399(11) . ? C2 C3 1.400(10) . ? C3 C4 1.390(10) . ? C4 C12 1.393(10) . ? C4 C5 1.461(10) . ? C5 N5 1.355(9) . ? C5 C6 1.367(10) . ? C6 N6 1.346(9) . ? C6 C7 1.469(10) . ? C7 C8 1.370(10) . ? C7 C11 1.410(10) . ? C8 C9 1.375(11) . ? C9 C10 1.395(11) . ? C10 N2 1.322(10) . ? C11 N2 1.372(9) . ? C11 C12 1.433(11) . ? C12 N1 1.325(9) . ? C13 N3 1.355(10) . ? C13 C14 1.413(11) . ? C14 C15 1.370(11) . ? C15 C16 1.391(10) . ? C16 C24 1.391(11) . ? C16 C17 1.471(10) . ? C17 N5 1.322(9) . ? C17 C18 1.402(10) . ? C18 N6 1.354(9) . ? C18 C19 1.440(10) . ? C19 C20 1.380(10) . ? C19 C23 1.384(10) . ? C20 C21 1.384(10) . ? C21 C22 1.380(11) . ? C22 N4 1.338(10) . ? C23 N4 1.338(9) . ? C23 C24 1.451(10) . ? C24 N3 1.348(9) . ? C25 N7 1.329(10) . ? C25 C26 1.403(11) . ? C26 C27 1.354(11) . ? C27 C28 1.381(11) . ? C28 C36 1.423(10) . ? C28 C29 1.446(9) . ? C29 N11 1.342(9) . ? C29 C30 1.405(10) . ? C30 N12 1.327(9) . ? C30 C31 1.480(9) . ? C31 C35 1.368(10) . ? C31 C32 1.410(10) . ? C32 C33 1.401(10) . ? C33 C34 1.383(11) . ? C34 N8 1.323(10) . ? C35 N8 1.372(9) . ? C35 C36 1.467(10) . ? C36 N7 1.346(9) . ? C37 N9 1.313(12) . ? C37 C38 1.408(13) . ? C38 C39 1.396(12) . ? C39 C40 1.386(12) . ? C40 C48 1.404(11) . ? C40 C41 1.447(11) . ? C41 N11 1.342(9) . ? C41 C42 1.404(11) . ? C42 N12 1.345(9) . ? C42 C43 1.469(9) . ? C43 C44 1.395(11) . ? C43 C47 1.409(10) . ? C44 C45 1.349(11) . ? C45 C46 1.420(12) . ? C46 N10 1.307(11) . ? C47 N10 1.336(10) . ? C47 C48 1.459(11) . ? C48 N9 1.362(10) . ? C49 C50 1.53(2) . ? C50 C51 1.40(3) . ? C51 C52 1.43(4) . ? C52 C53 1.588(19) . ? C53 C54 1.42(4) . ? C54 C55 1.48(3) . ? C55 C56 1.69(3) . ? C56 Pb2 2.828(19) 2_467 ? C57 C58 1.518(16) . ? C58 C59 1.483(16) . ? C59 C60 1.37(2) . ? C60 C60 1.55(2) 2_468 ? C61 C62 1.497(11) . ? C62 C63 1.537(13) . ? C63 C64 1.541(14) . ? C64 C64 1.45(2) 2_356 ? C65 C66 1.487(13) . ? C66 C67 1.371(18) . ? C67 C68 1.55(2) . ? C68 C69 1.44(2) . ? C69 C70 1.48(2) . ? C69 C70' 1.66(3) . ? C70 C71 1.62(3) . ? C71 C72 1.55(2) . ? C70' C71' 1.43(5) . ? C71' C72 1.54(4) . ? C72 Pb3 2.868(10) 2_557 ? 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 O4 Pb1 O2 82.4(3) . . ? O4 Pb1 O3 53.5(2) . . ? O2 Pb1 O3 77.2(2) . . ? O4 Pb1 N1 76.7(2) . . ? O2 Pb1 N1 127.1(2) . . ? O3 Pb1 N1 122.40(19) . . ? O4 Pb1 O1 87.0(3) . . ? O2 Pb1 O1 50.1(2) . . ? O3 Pb1 O1 118.8(3) . . ? N1 Pb1 O1 80.4(2) . . ? O4 Pb1 N2 74.4(2) . . ? O2 Pb1 N2 153.2(3) . . ? O3 Pb1 N2 78.3(2) . . ? N1 Pb1 N2 60.42(19) . . ? O1 Pb1 N2 139.3(2) . . ? O4 Pb1 C57 26.6(2) . . ? O2 Pb1 C57 79.3(3) . . ? O3 Pb1 C57 26.9(2) . . ? N1 Pb1 C57 99.4(2) . . ? O1 Pb1 C57 104.3(3) . . ? N2 Pb1 C57 74.0(2) . . ? O5 Pb2 O8 95.4(4) 2_467 . ? O5 Pb2 N4 72.3(3) 2_467 . ? O8 Pb2 N4 75.5(2) . . ? O5 Pb2 O6 50.5(4) 2_467 2_467 ? O8 Pb2 O6 77.9(4) . 2_467 ? N4 Pb2 O6 112.9(4) . 2_467 ? O5 Pb2 N3 85.8(3) 2_467 . ? O8 Pb2 N3 134.6(2) . . ? N4 Pb2 N3 61.7(2) . . ? O6 Pb2 N3 131.1(4) 2_467 . ? O5 Pb2 C56 24.6(5) 2_467 2_467 ? O8 Pb2 C56 82.5(5) . 2_467 ? N4 Pb2 C56 89.2(6) . 2_467 ? O6 Pb2 C56 26.7(5) 2_467 2_467 ? N3 Pb2 C56 109.7(5) . 2_467 ? O11 Pb3 O10 83.0(2) 2_557 . ? O11 Pb3 O9 78.3(2) 2_557 . ? O10 Pb3 O9 51.9(2) . . ? O11 Pb3 O12 51.2(2) 2_557 2_557 ? O10 Pb3 O12 123.2(2) . 2_557 ? O9 Pb3 O12 83.6(2) . 2_557 ? O11 Pb3 N7 84.5(2) 2_557 . ? O10 Pb3 N7 74.03(19) . . ? O9 Pb3 N7 124.55(19) . . ? O12 Pb3 N7 123.43(18) 2_557 . ? O11 Pb3 C65 81.9(3) 2_557 . ? O10 Pb3 C65 26.8(2) . . ? O9 Pb3 C65 25.3(2) . . ? O12 Pb3 C65 104.9(2) 2_557 . ? N7 Pb3 C65 100.6(2) . . ? O11 Pb3 C72 25.8(2) 2_557 2_557 ? O10 Pb3 C72 104.2(3) . 2_557 ? O9 Pb3 C72 80.6(3) . 2_557 ? O12 Pb3 C72 25.5(2) 2_557 2_557 ? N7 Pb3 C72 104.3(2) . 2_557 ? C65 Pb3 C72 94.3(3) . 2_557 ? C49 O1 Pb1 89.4(6) . . ? C49 O2 Pb1 93.2(7) . . ? C57 O3 Pb1 88.0(6) . . ? C57 O4 Pb1 97.4(6) . . ? C56 O5 Pb2 99.4(11) . 2_467 ? C56 O6 Pb2 85.7(12) . 2_467 ? C61 O8 Pb2 102.3(6) . . ? C65 O9 Pb3 91.1(5) . . ? C65 O10 Pb3 94.3(5) . . ? C72 O11 Pb3 97.8(6) . 2_557 ? C72 O12 Pb3 89.4(5) . 2_557 ? N1 C1 C2 123.9(6) . . ? C1 C2 C3 116.6(7) . . ? C4 C3 C2 119.6(7) . . ? C3 C4 C12 119.6(7) . . ? C3 C4 C5 121.9(7) . . ? C12 C4 C5 118.4(6) . . ? N5 C5 C6 121.2(7) . . ? N5 C5 C4 116.9(7) . . ? C6 C5 C4 121.9(7) . . ? N6 C6 C5 123.3(7) . . ? N6 C6 C7 116.9(6) . . ? C5 C6 C7 119.7(6) . . ? C8 C7 C11 118.0(7) . . ? C8 C7 C6 123.8(7) . . ? C11 C7 C6 118.2(7) . . ? C7 C8 C9 121.7(7) . . ? C8 C9 C10 116.4(7) . . ? N2 C10 C9 125.0(7) . . ? N2 C11 C7 121.4(7) . . ? N2 C11 C12 117.4(7) . . ? C7 C11 C12 121.2(7) . . ? N1 C12 C4 122.4(7) . . ? N1 C12 C11 117.2(7) . . ? C4 C12 C11 120.4(6) . . ? N3 C13 C14 124.2(7) . . ? C15 C14 C13 115.8(7) . . ? C14 C15 C16 122.1(7) . . ? C24 C16 C15 117.6(7) . . ? C24 C16 C17 120.0(7) . . ? C15 C16 C17 122.3(7) . . ? N5 C17 C18 123.8(6) . . ? N5 C17 C16 118.1(6) . . ? C18 C17 C16 118.1(6) . . ? N6 C18 C17 119.7(6) . . ? N6 C18 C19 118.9(7) . . ? C17 C18 C19 121.4(7) . . ? C20 C19 C23 119.4(7) . . ? C20 C19 C18 121.1(7) . . ? C23 C19 C18 119.5(7) . . ? C19 C20 C21 118.2(7) . . ? C22 C21 C20 119.1(7) . . ? N4 C22 C21 122.6(7) . . ? N4 C23 C19 122.2(7) . . ? N4 C23 C24 117.6(6) . . ? C19 C23 C24 120.2(6) . . ? N3 C24 C16 123.0(7) . . ? N3 C24 C23 116.8(6) . . ? C16 C24 C23 120.1(6) . . ? N7 C25 C26 121.7(7) . . ? C27 C26 C25 119.7(8) . . ? C26 C27 C28 120.3(7) . . ? C27 C28 C36 117.0(7) . . ? C27 C28 C29 122.9(7) . . ? C36 C28 C29 120.1(6) . . ? N11 C29 C30 120.9(6) . . ? N11 C29 C28 118.7(7) . . ? C30 C29 C28 120.3(6) . . ? N12 C30 C29 122.3(6) . . ? N12 C30 C31 117.9(6) . . ? C29 C30 C31 119.8(6) . . ? C35 C31 C32 120.6(6) . . ? C35 C31 C30 119.4(6) . . ? C32 C31 C30 120.0(6) . . ? C33 C32 C31 116.9(7) . . ? C34 C33 C32 119.1(8) . . ? N8 C34 C33 123.6(7) . . ? C31 C35 N8 121.3(7) . . ? C31 C35 C36 121.8(6) . . ? N8 C35 C36 116.9(6) . . ? N7 C36 C28 122.5(7) . . ? N7 C36 C35 118.9(6) . . ? C28 C36 C35 118.6(6) . . ? N9 C37 C38 122.7(8) . . ? C39 C38 C37 120.8(8) . . ? C40 C39 C38 115.7(8) . . ? C39 C40 C48 120.8(8) . . ? C39 C40 C41 119.9(7) . . ? C48 C40 C41 119.3(7) . . ? N11 C41 C42 120.9(7) . . ? N11 C41 C40 119.0(7) . . ? C42 C41 C40 120.1(6) . . ? N12 C42 C41 121.9(6) . . ? N12 C42 C43 117.5(7) . . ? C41 C42 C43 120.5(6) . . ? C44 C43 C47 119.8(6) . . ? C44 C43 C42 120.6(6) . . ? C47 C43 C42 119.6(7) . . ? C45 C44 C43 116.6(7) . . ? C44 C45 C46 121.8(8) . . ? N10 C46 C45 120.4(8) . . ? N10 C47 C43 121.1(7) . . ? N10 C47 C48 120.1(7) . . ? C43 C47 C48 118.8(7) . . ? N9 C48 C40 122.0(8) . . ? N9 C48 C47 116.4(7) . . ? C40 C48 C47 121.6(7) . . ? O2 C49 O1 127.0(10) . . ? O2 C49 C50 115.7(12) . . ? O1 C49 C50 116.7(12) . . ? C51 C50 C49 118(2) . . ? C50 C51 C52 104(3) . . ? C51 C52 C53 105(3) . . ? C54 C53 C52 118(3) . . ? C53 C54 C55 108(3) . . ? C54 C55 C56 109(3) . . ? O5 C56 O6 120.8(17) . . ? O5 C56 C55 121(2) . . ? O6 C56 C55 118(2) . . ? O5 C56 Pb2 56.0(9) . 2_467 ? O6 C56 Pb2 67.7(10) . 2_467 ? C55 C56 Pb2 160.4(18) . 2_467 ? O4 C57 O3 121.0(10) . . ? O4 C57 C58 120.1(10) . . ? O3 C57 C58 118.8(9) . . ? O4 C57 Pb1 55.9(6) . . ? O3 C57 Pb1 65.1(6) . . ? C58 C57 Pb1 176.0(8) . . ? C59 C58 C57 114.7(12) . . ? C60 C59 C58 120.2(15) . . ? C59 C60 C60 114.1(15) . 2_468 ? O7 C61 O8 120.7(9) . . ? O7 C61 C62 120.8(8) . . ? O8 C61 C62 118.5(8) . . ? C61 C62 C63 119.0(8) . . ? C62 C63 C64 113.6(8) . . ? C64 C64 C63 111.8(11) 2_356 . ? O9 C65 O10 121.8(8) . . ? O9 C65 C66 120.9(9) . . ? O10 C65 C66 117.2(10) . . ? O9 C65 Pb3 63.6(5) . . ? O10 C65 Pb3 58.9(4) . . ? C66 C65 Pb3 172.0(8) . . ? C67 C66 C65 117.9(13) . . ? C66 C67 C68 112.6(14) . . ? C69 C68 C67 117.1(14) . . ? C68 C69 C70 105.6(14) . . ? C68 C69 C70' 138.6(16) . . ? C70 C69 C70' 43.0(11) . . ? C69 C70 C71 112.9(14) . . ? C72 C71 C70 105.5(13) . . ? C71' C70' C69 109(2) . . ? C70' C71' C72 115(3) . . ? O12 C72 O11 121.5(9) . . ? O12 C72 C71' 123.3(17) . . ? O11 C72 C71' 114.7(17) . . ? O12 C72 C71 116.2(13) . . ? O11 C72 C71 121.0(12) . . ? C71' C72 C71 20.4(13) . . ? O12 C72 Pb3 65.1(5) . 2_557 ? O11 C72 Pb3 56.4(5) . 2_557 ? C71' C72 Pb3 170.0(16) . 2_557 ? C71 C72 Pb3 165.7(9) . 2_557 ? C12 N1 C1 117.8(6) . . ? C12 N1 Pb1 124.6(5) . . ? C1 N1 Pb1 117.4(4) . . ? C10 N2 C11 117.5(7) . . ? C10 N2 Pb1 122.5(5) . . ? C11 N2 Pb1 119.8(5) . . ? C24 N3 C13 117.2(7) . . ? C24 N3 Pb2 117.7(5) . . ? C13 N3 Pb2 121.9(5) . . ? C22 N4 C23 118.2(7) . . ? C22 N4 Pb2 120.2(5) . . ? C23 N4 Pb2 121.4(5) . . ? C17 N5 C5 115.8(6) . . ? C6 N6 C18 116.1(6) . . ? C25 N7 C36 118.6(6) . . ? C25 N7 Pb3 116.9(5) . . ? C36 N7 Pb3 123.8(5) . . ? C34 N8 C35 118.4(6) . . ? C37 N9 C48 117.9(7) . . ? C46 N10 C47 120.2(7) . . ? C29 N11 C41 117.4(6) . . ? C30 N12 C42 116.5(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.426 _refine_diff_density_min -1.151 _refine_diff_density_rms 0.203