# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global loop_ _publ_author_name 'Wei-Yin Sun' 'Jian Fan' 'Taka-aki Okamura' 'Xing-Mei Ouyang' 'Norikazu Ueyama' 'Shuang-Yi Wan' 'Hui-Fang Zhu' _publ_contact_author_name 'Prof Wei-Yin Sun' _publ_contact_author_address ; Coordination Chemistry Institute Nanjing University Nanjing 210093 CHINA ; _publ_contact_author_email SUNWY@NJU.EDU.CN data_shelxl _database_code_CSD 191433 _audit_creation_date 'Sat Sep 7 18:45:43 2002' _audit_creation_method SHELXL-97 _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; [Pb(timpt)(NO3)](NO3)-0.417(Et2O)-0.167(H2O) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34.67 H31.50 N11 O6.58 Pb ' _chemical_formula_sum 'C34.67 H31.50 N11 O6.58 Pb' _chemical_formula_weight 914.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pb' 'Pb' -3.3944 10.1111 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 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 33.6859(7) _cell_length_b 7.7447(2) _cell_length_c 30.8578(10) _cell_angle_alpha 90.00 _cell_angle_beta 116.0144(11) _cell_angle_gamma 90.00 _cell_volume 7234.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 200 _cell_measurement_reflns_used 21554 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 27.4 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3609 _exptl_absorpt_coefficient_mu 4.727 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.637 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _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 Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28746 _diffrn_reflns_av_R_equivalents 0.1331 _diffrn_reflns_av_sigmaI/netI 0.1731 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8120 _reflns_number_gt 3918 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare, 1994)' _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^)+(0.0351P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8120 _refine_ls_number_parameters 488 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1504 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.889 _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 Pb1 Pb 0.073835(9) -0.21845(4) 0.162811(12) 0.04933(12) Uani 1 1 d . . . O6 O 0.0000 -0.042(2) 0.2500 0.232(13) Uani 0.833(11) 2 d SPD . . O7 O 0.1000(14) -0.087(6) 0.3400(16) 0.115(19) Uiso 0.167(11) 1 d P . . O41 O 0.05176(18) -0.4860(7) 0.1097(2) 0.0651(17) Uani 1 1 d . . . O42 O -0.00648(19) -0.4107(9) 0.1159(2) 0.085(2) Uani 1 1 d . . . O43 O -0.0062(2) -0.6469(10) 0.0793(3) 0.102(3) Uani 1 1 d . . . O51 O 0.1662(2) -0.8361(8) 0.2614(2) 0.0763(19) Uani 1 1 d . . . O52 O 0.12288(18) -1.0547(8) 0.2491(2) 0.0698(17) Uani 1 1 d . . . O53 O 0.12538(19) -0.9257(7) 0.1897(2) 0.0659(17) Uani 1 1 d . . . N1 N 0.21354(18) 0.3903(7) -0.0490(2) 0.0358(15) Uani 1 1 d . . . N2 N 0.28447(17) 0.5162(7) -0.0207(2) 0.0371(15) Uani 1 1 d . . . N3 N 0.24514(18) 0.5276(7) 0.0276(2) 0.0349(14) Uani 1 1 d . . . N4 N 0.0129(3) -0.5161(12) 0.1009(3) 0.066(2) Uani 1 1 d . . . N5 N 0.1393(3) -0.9395(10) 0.2346(3) 0.058(2) Uani 1 1 d . . . N11 N 0.05785(17) 0.1069(8) 0.0318(2) 0.0399(15) Uani 1 1 d . . . N12 N 0.07165(19) -0.0951(9) 0.0847(2) 0.0484(17) Uani 1 1 d . . . N21 N 0.20287(18) -0.4954(8) 0.1969(2) 0.0425(15) Uani 1 1 d . . . N22 N 0.14303(18) -0.3321(7) 0.1736(2) 0.0438(16) Uani 1 1 d . . . N31 N 0.0744(2) -0.5413(11) 0.2900(3) 0.064(2) Uani 1 1 d . . . N32 N 0.0821(2) -0.4600(10) 0.2247(3) 0.062(2) Uani 1 1 d . . . C1 C 0.2126(2) 0.4414(9) -0.0083(3) 0.0365(18) Uani 1 1 d . . . C2 C 0.2502(2) 0.4309(8) -0.0537(3) 0.0375(18) Uani 1 1 d . . . C3 C 0.2809(2) 0.5608(8) 0.0198(3) 0.0345(18) Uani 1 1 d . . . C11 C 0.1716(2) 0.4003(9) -0.0031(3) 0.0378(18) Uani 1 1 d . . . C12 C 0.1392(2) 0.3021(9) -0.0371(3) 0.0438(18) Uani 1 1 d . . . H1 H 0.1431 0.2590 -0.0638 0.053 Uiso 1 1 calc R . . C13 C 0.1008(2) 0.2648(9) -0.0332(3) 0.050(2) Uani 1 1 d . . . H2 H 0.0787 0.1952 -0.0568 0.060 Uiso 1 1 calc R . . C14 C 0.0948(2) 0.3294(9) 0.0056(3) 0.0389(18) Uani 1 1 d . . . C15 C 0.1271(2) 0.4271(9) 0.0393(3) 0.045(2) Uani 1 1 d . . . H3 H 0.1233 0.4695 0.0662 0.055 Uiso 1 1 calc R . . C16 C 0.1657(2) 0.4661(9) 0.0352(3) 0.046(2) Uani 1 1 d . . . H4 H 0.1877 0.5371 0.0585 0.055 Uiso 1 1 calc R . . C17 C 0.0535(2) 0.2782(10) 0.0106(3) 0.0468(19) Uani 1 1 d . . . H5 H 0.0479 0.3637 0.0311 0.056 Uiso 1 1 calc R . . H6 H 0.0278 0.2794 -0.0216 0.056 Uiso 1 1 calc R . . C18 C 0.0684(2) 0.0706(11) 0.0772(3) 0.052(2) Uani 1 1 d . . . H7 H 0.0731 0.1546 0.1014 0.062 Uiso 1 1 calc R . . C19 C 0.0626(2) -0.1685(11) 0.0416(3) 0.056(2) Uani 1 1 d . . . H8 H 0.0623 -0.2890 0.0357 0.067 Uiso 1 1 calc R . . C20 C 0.0541(2) -0.0440(11) 0.0087(3) 0.051(2) Uani 1 1 d . . . H9 H 0.0468 -0.0591 -0.0245 0.062 Uiso 1 1 calc R . . C21 C 0.2465(2) -0.8711(9) 0.0970(3) 0.0395(18) Uani 1 1 d . . . C22 C 0.2807(2) -0.7826(11) 0.1323(3) 0.068(3) Uani 1 1 d . . . H10 H 0.3074 -0.7691 0.1295 0.082 Uiso 1 1 calc R . . C23 C 0.2776(2) -0.7125(12) 0.1717(3) 0.066(2) Uani 1 1 d . . . H11 H 0.3019 -0.6522 0.1957 0.080 Uiso 1 1 calc R . . C24 C 0.2386(2) -0.7315(9) 0.1759(3) 0.0464(19) Uani 1 1 d . . . C25 C 0.2049(2) -0.8277(9) 0.1421(3) 0.045(2) Uani 1 1 d . . . H12 H 0.1787 -0.8477 0.1458 0.054 Uiso 1 1 calc R . . C26 C 0.2089(2) -0.8951(10) 0.1028(3) 0.048(2) Uani 1 1 d . . . H13 H 0.1851 -0.9592 0.0793 0.058 Uiso 1 1 calc R . . C27 C 0.2323(2) -0.6392(10) 0.2164(3) 0.052(2) Uani 1 1 d . . . H14 H 0.2198 -0.7207 0.2319 0.062 Uiso 1 1 calc R . . H15 H 0.2611 -0.5980 0.2412 0.062 Uiso 1 1 calc R . . C28 C 0.1637(2) -0.4724(10) 0.1973(3) 0.049(2) Uani 1 1 d . . . H16 H 0.1519 -0.5486 0.2129 0.059 Uiso 1 1 calc R . . C29 C 0.1717(2) -0.2577(9) 0.1579(3) 0.051(2) Uani 1 1 d . . . H17 H 0.1667 -0.1527 0.1404 0.062 Uiso 1 1 calc R . . C30 C 0.2073(3) -0.3572(10) 0.1714(3) 0.050(2) Uani 1 1 d . . . H18 H 0.2317 -0.3362 0.1645 0.061 Uiso 1 1 calc R . . C31 C 0.1813(2) -0.8498(9) 0.4424(3) 0.0398(18) Uani 1 1 d . . . C32 C 0.1836(2) -0.8019(10) 0.4003(3) 0.056(2) Uani 1 1 d . . . H19 H 0.2085 -0.8343 0.3953 0.067 Uiso 1 1 calc R . . C33 C 0.1494(3) -0.7057(11) 0.3649(3) 0.060(2) Uani 1 1 d . . . H20 H 0.1509 -0.6721 0.3361 0.072 Uiso 1 1 calc R . . C34 C 0.1131(2) -0.6606(10) 0.3729(3) 0.056(2) Uani 1 1 d . . . C35 C 0.1111(2) -0.7149(10) 0.4142(3) 0.055(2) Uani 1 1 d . . . H21 H 0.0856 -0.6888 0.4187 0.066 Uiso 1 1 calc R . . C36 C 0.1450(2) -0.8057(9) 0.4491(3) 0.0439(19) Uani 1 1 d . . . H22 H 0.1433 -0.8382 0.4780 0.053 Uiso 1 1 calc R . . C37 C 0.0767(3) -0.5448(13) 0.3369(3) 0.080(3) Uani 1 1 d . . . H23 H 0.0479 -0.5847 0.3346 0.096 Uiso 1 1 calc R . . H24 H 0.0814 -0.4256 0.3498 0.096 Uiso 1 1 calc R . . C38 C 0.0892(3) -0.4190(11) 0.2692(4) 0.066(3) Uani 1 1 d . . . H25 H 0.1031 -0.3150 0.2848 0.079 Uiso 1 1 calc R . . C39 C 0.0635(3) -0.6197(13) 0.2161(4) 0.072(3) Uani 1 1 d . . . H26 H 0.0552 -0.6847 0.1873 0.087 Uiso 1 1 calc R . . C40 C 0.0587(3) -0.6721(12) 0.2570(4) 0.073(3) Uani 1 1 d . . . H27 H 0.0467 -0.7786 0.2610 0.088 Uiso 1 1 calc R . . C61 C 0.0153(6) -0.119(2) 0.2942(3) 0.28(2) Uani 0.833(11) 1 d PD . . H28 H 0.0438 -0.1746 0.3010 0.334 Uiso 0.833(11) 1 calc PR . . H29 H -0.0057 -0.2114 0.2922 0.334 Uiso 0.833(11) 1 calc PR . . C62 C 0.0225(6) 0.0008(19) 0.3392(7) 0.38(3) Uani 0.833(11) 1 d PD . . H30 H 0.0380 -0.0649 0.3691 0.452 Uiso 0.833(11) 1 calc PR . . H31 H -0.0062 0.0388 0.3365 0.452 Uiso 0.833(11) 1 calc PR . . H32 H 0.0402 0.1018 0.3395 0.452 Uiso 0.833(11) 1 calc PR . . 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 0.05313(18) 0.04561(18) 0.0540(2) 0.01347(19) 0.02785(14) 0.00722(17) O6 0.107(12) 0.096(14) 0.36(3) 0.000 -0.021(15) 0.000 O41 0.054(4) 0.073(4) 0.081(5) -0.007(3) 0.040(4) -0.015(3) O42 0.061(4) 0.108(6) 0.085(5) -0.013(4) 0.030(4) 0.007(4) O43 0.068(5) 0.100(6) 0.146(7) -0.054(5) 0.055(5) -0.035(4) O51 0.077(4) 0.067(5) 0.074(5) -0.002(4) 0.024(4) -0.018(3) O52 0.074(4) 0.062(4) 0.077(5) 0.020(3) 0.036(4) -0.003(3) O53 0.087(4) 0.053(4) 0.074(5) 0.000(3) 0.050(4) -0.008(3) N1 0.042(4) 0.023(3) 0.039(4) -0.004(3) 0.015(3) -0.003(3) N2 0.039(4) 0.035(4) 0.041(4) 0.002(3) 0.021(3) 0.005(3) N3 0.044(4) 0.029(3) 0.035(4) 0.002(3) 0.020(3) 0.006(3) N4 0.061(6) 0.085(7) 0.054(6) -0.001(4) 0.026(5) 0.010(5) N5 0.076(6) 0.044(5) 0.057(6) 0.019(4) 0.031(5) 0.011(4) N11 0.041(4) 0.032(4) 0.047(5) 0.005(4) 0.021(3) -0.002(3) N12 0.054(4) 0.048(5) 0.041(5) 0.014(4) 0.018(3) 0.004(3) N21 0.044(4) 0.044(4) 0.037(4) -0.003(3) 0.015(3) -0.001(3) N22 0.050(4) 0.030(4) 0.056(4) 0.008(3) 0.027(3) 0.001(3) N31 0.059(5) 0.077(6) 0.054(6) 0.018(5) 0.025(4) 0.012(4) N32 0.064(5) 0.071(6) 0.062(6) 0.006(4) 0.037(4) -0.003(4) C1 0.038(5) 0.032(5) 0.034(5) 0.009(4) 0.011(4) 0.010(3) C2 0.037(5) 0.031(4) 0.042(5) -0.003(4) 0.014(4) 0.005(3) C3 0.042(5) 0.016(4) 0.043(5) 0.005(3) 0.015(4) 0.006(3) C11 0.031(4) 0.032(4) 0.047(5) 0.006(4) 0.014(4) 0.004(3) C12 0.036(4) 0.051(5) 0.036(4) -0.006(4) 0.008(3) -0.005(4) C13 0.043(4) 0.049(5) 0.051(5) -0.006(4) 0.015(4) -0.009(3) C14 0.036(4) 0.043(5) 0.038(5) 0.009(4) 0.017(4) 0.008(3) C15 0.053(5) 0.052(5) 0.039(5) 0.007(4) 0.027(4) 0.010(4) C16 0.039(5) 0.053(5) 0.046(6) 0.000(4) 0.020(4) 0.001(3) C17 0.038(4) 0.055(5) 0.042(5) 0.005(4) 0.013(4) 0.007(4) C18 0.060(5) 0.046(6) 0.048(6) 0.015(4) 0.022(5) 0.005(4) C19 0.048(5) 0.048(6) 0.072(7) -0.001(5) 0.026(5) 0.000(4) C20 0.058(5) 0.049(6) 0.054(6) 0.001(5) 0.030(5) -0.003(4) C21 0.036(5) 0.041(5) 0.039(5) -0.001(4) 0.014(4) 0.000(3) C22 0.037(5) 0.101(7) 0.063(6) -0.028(6) 0.020(4) -0.003(5) C23 0.036(5) 0.108(7) 0.056(6) -0.023(6) 0.021(4) -0.010(4) C24 0.053(5) 0.046(5) 0.037(5) -0.008(4) 0.016(4) 0.009(4) C25 0.051(5) 0.039(5) 0.060(6) 0.004(4) 0.037(4) -0.003(3) C26 0.058(5) 0.053(5) 0.036(5) -0.015(4) 0.023(4) -0.015(4) C27 0.049(5) 0.052(5) 0.043(5) 0.001(4) 0.009(4) 0.005(4) C28 0.051(5) 0.043(5) 0.065(6) -0.002(4) 0.037(5) -0.007(4) C29 0.053(5) 0.038(6) 0.063(6) 0.001(4) 0.026(4) -0.006(4) C30 0.055(5) 0.047(5) 0.064(6) -0.012(4) 0.040(5) -0.007(4) C31 0.052(5) 0.033(4) 0.037(5) 0.004(4) 0.022(4) 0.001(3) C32 0.051(5) 0.065(6) 0.054(5) 0.007(5) 0.026(4) 0.013(4) C33 0.076(6) 0.072(6) 0.045(5) 0.015(5) 0.037(5) 0.012(5) C34 0.053(5) 0.068(6) 0.045(6) 0.011(4) 0.021(5) 0.016(4) C35 0.044(5) 0.077(6) 0.045(5) 0.003(5) 0.021(4) 0.007(4) C36 0.045(5) 0.046(5) 0.041(5) -0.003(4) 0.019(4) 0.002(4) C37 0.103(8) 0.097(8) 0.053(7) 0.038(6) 0.046(6) 0.043(6) C38 0.073(6) 0.053(6) 0.074(8) 0.017(6) 0.034(6) 0.004(4) C39 0.061(6) 0.072(7) 0.074(8) 0.012(6) 0.020(5) 0.006(5) C40 0.064(6) 0.065(7) 0.074(8) 0.028(6) 0.015(5) -0.004(5) C61 0.36(4) 0.15(2) 0.55(6) 0.21(3) 0.41(4) 0.16(2) C62 0.26(3) 0.120(18) 0.39(4) 0.16(2) -0.18(2) -0.153(19) _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 N22 2.374(5) . ? Pb1 O41 2.543(6) . ? Pb1 N12 2.564(6) . ? Pb1 N32 2.600(7) . ? Pb1 O52 2.751(6) 1_565 ? Pb1 O53 2.753(5) 1_565 ? O6 C61 1.365(10) 2 ? O6 C61 1.365(10) . ? O41 N4 1.237(8) . ? O42 N4 1.254(8) . ? O43 N4 1.228(9) . ? O51 N5 1.221(8) . ? O52 N5 1.234(8) . ? O52 Pb1 2.751(6) 1_545 ? O53 N5 1.256(8) . ? O53 Pb1 2.753(5) 1_545 ? N1 C1 1.330(8) . ? N1 C2 1.343(8) . ? N2 C2 1.332(8) . ? N2 C3 1.355(8) . ? N3 C1 1.345(8) . ? N3 C3 1.350(8) . ? N11 C18 1.317(9) . ? N11 C20 1.345(9) . ? N11 C17 1.458(9) . ? N12 C18 1.300(9) . ? N12 C19 1.351(9) . ? N21 C28 1.338(8) . ? N21 C30 1.374(9) . ? N21 C27 1.436(9) . ? N22 C28 1.324(9) . ? N22 C29 1.381(9) . ? N31 C38 1.356(10) . ? N31 C40 1.368(11) . ? N31 C37 1.418(10) . ? N32 C38 1.322(10) . ? N32 C39 1.359(10) . ? C1 C11 1.495(9) . ? C2 C21 1.461(9) 7_545 ? C3 C31 1.469(9) 4_565 ? C11 C12 1.366(9) . ? C11 C16 1.378(9) . ? C12 C13 1.380(9) . ? C12 H1 0.9500 . ? C13 C14 1.391(10) . ? C13 H2 0.9500 . ? C14 C15 1.360(9) . ? C14 C17 1.519(9) . ? C15 C16 1.395(9) . ? C15 H3 0.9500 . ? C16 H4 0.9500 . ? C17 H5 0.9900 . ? C17 H6 0.9900 . ? C18 H7 0.9500 . ? C19 C20 1.338(10) . ? C19 H8 0.9500 . ? C20 H9 0.9500 . ? C21 C26 1.370(9) . ? C21 C22 1.372(10) . ? C21 C2 1.461(9) 7_545 ? C22 C23 1.375(11) . ? C22 H10 0.9500 . ? C23 C24 1.383(10) . ? C23 H11 0.9500 . ? C24 C25 1.378(10) . ? C24 C27 1.534(10) . ? C25 C26 1.380(9) . ? C25 H12 0.9500 . ? C26 H13 0.9500 . ? C27 H14 0.9900 . ? C27 H15 0.9900 . ? C28 H16 0.9500 . ? C29 C30 1.330(9) . ? C29 H17 0.9500 . ? C30 H18 0.9500 . ? C31 C36 1.373(9) . ? C31 C32 1.385(10) . ? C31 C3 1.469(9) 4_535 ? C32 C33 1.405(10) . ? C32 H19 0.9500 . ? C33 C34 1.392(10) . ? C33 H20 0.9500 . ? C34 C35 1.372(10) . ? C34 C37 1.532(10) . ? C35 C36 1.371(10) . ? C35 H21 0.9500 . ? C36 H22 0.9500 . ? C37 H23 0.9900 . ? C37 H24 0.9900 . ? C38 H25 0.9500 . ? C39 C40 1.400(12) . ? C39 H26 0.9500 . ? C40 H27 0.9500 . ? C61 C62 1.595(17) . ? C61 H28 0.9900 . ? C61 H29 0.9900 . ? C62 H30 0.9800 . ? C62 H31 0.9800 . ? C62 H32 0.9800 . ? 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 N22 Pb1 O41 77.28(19) . . ? N22 Pb1 N12 83.8(2) . . ? O41 Pb1 N12 79.5(2) . . ? N22 Pb1 N32 81.3(2) . . ? O41 Pb1 N32 78.1(2) . . ? N12 Pb1 N32 155.3(2) . . ? N22 Pb1 O52 84.21(19) . 1_565 ? O41 Pb1 O52 151.81(18) . 1_565 ? N12 Pb1 O52 119.7(2) . 1_565 ? N32 Pb1 O52 78.2(2) . 1_565 ? N22 Pb1 O53 79.19(17) . 1_565 ? O41 Pb1 O53 146.39(17) . 1_565 ? N12 Pb1 O53 74.4(2) . 1_565 ? N32 Pb1 O53 121.4(2) . 1_565 ? O52 Pb1 O53 45.33(17) 1_565 1_565 ? C61 O6 C61 128.3(18) 2 . ? N4 O41 Pb1 106.0(5) . . ? N5 O52 Pb1 99.0(5) . 1_545 ? N5 O53 Pb1 98.3(5) . 1_545 ? C1 N1 C2 115.9(6) . . ? C2 N2 C3 115.7(6) . . ? C1 N3 C3 114.6(6) . . ? O43 N4 O41 121.7(8) . . ? O43 N4 O42 120.2(8) . . ? O41 N4 O42 118.1(8) . . ? O51 N5 O52 123.1(8) . . ? O51 N5 O53 119.9(8) . . ? O52 N5 O53 116.8(8) . . ? C18 N11 C20 107.3(7) . . ? C18 N11 C17 126.8(7) . . ? C20 N11 C17 125.8(7) . . ? C18 N12 C19 106.1(7) . . ? C18 N12 Pb1 120.0(6) . . ? C19 N12 Pb1 132.0(6) . . ? C28 N21 C30 104.9(6) . . ? C28 N21 C27 126.9(7) . . ? C30 N21 C27 128.1(6) . . ? C28 N22 C29 104.9(6) . . ? C28 N22 Pb1 128.9(5) . . ? C29 N22 Pb1 126.1(5) . . ? C38 N31 C40 105.5(8) . . ? C38 N31 C37 129.2(9) . . ? C40 N31 C37 125.2(9) . . ? C38 N32 C39 106.3(8) . . ? C38 N32 Pb1 120.1(6) . . ? C39 N32 Pb1 128.3(7) . . ? N1 C1 N3 125.2(6) . . ? N1 C1 C11 116.4(6) . . ? N3 C1 C11 118.4(7) . . ? N2 C2 N1 124.3(7) . . ? N2 C2 C21 117.9(6) . 7_545 ? N1 C2 C21 117.7(6) . 7_545 ? N3 C3 N2 124.2(6) . . ? N3 C3 C31 118.7(7) . 4_565 ? N2 C3 C31 117.1(6) . 4_565 ? C12 C11 C16 119.9(6) . . ? C12 C11 C1 120.0(7) . . ? C16 C11 C1 120.1(7) . . ? C11 C12 C13 120.8(7) . . ? C11 C12 H1 119.6 . . ? C13 C12 H1 119.6 . . ? C12 C13 C14 119.7(7) . . ? C12 C13 H2 120.1 . . ? C14 C13 H2 120.1 . . ? C15 C14 C13 119.3(7) . . ? C15 C14 C17 121.9(7) . . ? C13 C14 C17 118.7(6) . . ? C14 C15 C16 121.0(7) . . ? C14 C15 H3 119.5 . . ? C16 C15 H3 119.5 . . ? C11 C16 C15 119.2(7) . . ? C11 C16 H4 120.4 . . ? C15 C16 H4 120.4 . . ? N11 C17 C14 111.5(5) . . ? N11 C17 H5 109.3 . . ? C14 C17 H5 109.3 . . ? N11 C17 H6 109.3 . . ? C14 C17 H6 109.3 . . ? H5 C17 H6 108.0 . . ? N12 C18 N11 111.2(8) . . ? N12 C18 H7 124.4 . . ? N11 C18 H7 124.4 . . ? C20 C19 N12 108.9(7) . . ? C20 C19 H8 125.5 . . ? N12 C19 H8 125.5 . . ? C19 C20 N11 106.5(8) . . ? C19 C20 H9 126.7 . . ? N11 C20 H9 126.7 . . ? C26 C21 C22 117.7(7) . . ? C26 C21 C2 121.4(7) . 7_545 ? C22 C21 C2 120.9(7) . 7_545 ? C21 C22 C23 122.6(7) . . ? C21 C22 H10 118.7 . . ? C23 C22 H10 118.7 . . ? C22 C23 C24 118.8(7) . . ? C22 C23 H11 120.6 . . ? C24 C23 H11 120.6 . . ? C25 C24 C23 119.3(7) . . ? C25 C24 C27 120.3(7) . . ? C23 C24 C27 120.3(7) . . ? C24 C25 C26 120.3(7) . . ? C24 C25 H12 119.9 . . ? C26 C25 H12 119.9 . . ? C21 C26 C25 121.1(7) . . ? C21 C26 H13 119.4 . . ? C25 C26 H13 119.4 . . ? N21 C27 C24 109.7(6) . . ? N21 C27 H14 109.7 . . ? C24 C27 H14 109.7 . . ? N21 C27 H15 109.7 . . ? C24 C27 H15 109.7 . . ? H14 C27 H15 108.2 . . ? N22 C28 N21 112.7(7) . . ? N22 C28 H16 123.7 . . ? N21 C28 H16 123.7 . . ? C30 C29 N22 108.8(7) . . ? C30 C29 H17 125.6 . . ? N22 C29 H17 125.6 . . ? C29 C30 N21 108.7(7) . . ? C29 C30 H18 125.7 . . ? N21 C30 H18 125.7 . . ? C36 C31 C32 119.8(7) . . ? C36 C31 C3 121.2(7) . 4_535 ? C32 C31 C3 119.0(7) . 4_535 ? C31 C32 C33 120.4(7) . . ? C31 C32 H19 119.8 . . ? C33 C32 H19 119.8 . . ? C34 C33 C32 118.7(7) . . ? C34 C33 H20 120.6 . . ? C32 C33 H20 120.6 . . ? C35 C34 C33 119.4(7) . . ? C35 C34 C37 120.2(7) . . ? C33 C34 C37 120.4(8) . . ? C36 C35 C34 121.7(7) . . ? C36 C35 H21 119.1 . . ? C34 C35 H21 119.1 . . ? C35 C36 C31 119.9(7) . . ? C35 C36 H22 120.1 . . ? C31 C36 H22 120.1 . . ? N31 C37 C34 114.7(7) . . ? N31 C37 H23 108.6 . . ? C34 C37 H23 108.6 . . ? N31 C37 H24 108.6 . . ? C34 C37 H24 108.6 . . ? H23 C37 H24 107.6 . . ? N32 C38 N31 112.7(8) . . ? N32 C38 H25 123.6 . . ? N31 C38 H25 123.6 . . ? N32 C39 C40 108.2(9) . . ? N32 C39 H26 125.9 . . ? C40 C39 H26 125.9 . . ? N31 C40 C39 107.2(8) . . ? N31 C40 H27 126.4 . . ? C39 C40 H27 126.4 . . ? O6 C61 C62 117.6(15) . . ? O6 C61 H28 107.9 . . ? C62 C61 H28 107.9 . . ? O6 C61 H29 107.9 . . ? C62 C61 H29 107.9 . . ? H28 C61 H29 107.2 . . ? C61 C62 H30 109.5 . . ? C61 C62 H31 109.5 . . ? H30 C62 H31 109.5 . . ? C61 C62 H32 109.5 . . ? H30 C62 H32 109.5 . . ? H31 C62 H32 109.5 . . ? 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 N22 Pb1 O41 N4 164.0(5) . . . . ? N12 Pb1 O41 N4 -110.1(5) . . . . ? N32 Pb1 O41 N4 80.4(5) . . . . ? O52 Pb1 O41 N4 113.8(5) 1_565 . . . ? O53 Pb1 O41 N4 -149.4(5) 1_565 . . . ? Pb1 O41 N4 O43 -173.6(7) . . . . ? Pb1 O41 N4 O42 4.6(9) . . . . ? Pb1 O52 N5 O51 -176.2(7) 1_545 . . . ? Pb1 O52 N5 O53 7.6(7) 1_545 . . . ? Pb1 O53 N5 O51 176.1(6) 1_545 . . . ? Pb1 O53 N5 O52 -7.6(7) 1_545 . . . ? N22 Pb1 N12 C18 -121.1(5) . . . . ? O41 Pb1 N12 C18 160.7(6) . . . . ? N32 Pb1 N12 C18 -174.1(5) . . . . ? O52 Pb1 N12 C18 -41.4(6) 1_565 . . . ? O53 Pb1 N12 C18 -40.7(5) 1_565 . . . ? N22 Pb1 N12 C19 77.4(6) . . . . ? O41 Pb1 N12 C19 -0.8(6) . . . . ? N32 Pb1 N12 C19 24.5(9) . . . . ? O52 Pb1 N12 C19 157.1(6) 1_565 . . . ? O53 Pb1 N12 C19 157.9(7) 1_565 . . . ? O41 Pb1 N22 C28 -71.5(7) . . . . ? N12 Pb1 N22 C28 -152.1(7) . . . . ? N32 Pb1 N22 C28 8.2(7) . . . . ? O52 Pb1 N22 C28 87.1(7) 1_565 . . . ? O53 Pb1 N22 C28 132.7(7) 1_565 . . . ? O41 Pb1 N22 C29 112.0(6) . . . . ? N12 Pb1 N22 C29 31.4(6) . . . . ? N32 Pb1 N22 C29 -168.3(6) . . . . ? O52 Pb1 N22 C29 -89.4(6) 1_565 . . . ? O53 Pb1 N22 C29 -43.8(6) 1_565 . . . ? N22 Pb1 N32 C38 110.5(6) . . . . ? O41 Pb1 N32 C38 -170.8(6) . . . . ? N12 Pb1 N32 C38 163.9(5) . . . . ? O52 Pb1 N32 C38 24.6(6) 1_565 . . . ? O53 Pb1 N32 C38 38.9(7) 1_565 . . . ? N22 Pb1 N32 C39 -99.1(7) . . . . ? O41 Pb1 N32 C39 -20.4(7) . . . . ? N12 Pb1 N32 C39 -45.7(9) . . . . ? O52 Pb1 N32 C39 175.0(7) 1_565 . . . ? O53 Pb1 N32 C39 -170.7(6) 1_565 . . . ? C2 N1 C1 N3 -0.4(10) . . . . ? C2 N1 C1 C11 178.7(5) . . . . ? C3 N3 C1 N1 -0.3(9) . . . . ? C3 N3 C1 C11 -179.5(5) . . . . ? C3 N2 C2 N1 0.7(9) . . . . ? C3 N2 C2 C21 -176.6(6) . . . 7_545 ? C1 N1 C2 N2 0.2(10) . . . . ? C1 N1 C2 C21 177.5(6) . . . 7_545 ? C1 N3 C3 N2 1.3(9) . . . . ? C1 N3 C3 C31 -178.3(6) . . . 4_565 ? C2 N2 C3 N3 -1.5(9) . . . . ? C2 N2 C3 C31 178.1(6) . . . 4_565 ? N1 C1 C11 C12 5.5(9) . . . . ? N3 C1 C11 C12 -175.2(6) . . . . ? N1 C1 C11 C16 -172.4(6) . . . . ? N3 C1 C11 C16 6.9(9) . . . . ? C16 C11 C12 C13 -1.3(11) . . . . ? C1 C11 C12 C13 -179.2(6) . . . . ? C11 C12 C13 C14 0.8(11) . . . . ? C12 C13 C14 C15 -0.7(11) . . . . ? C12 C13 C14 C17 -176.6(6) . . . . ? C13 C14 C15 C16 1.2(11) . . . . ? C17 C14 C15 C16 177.0(6) . . . . ? C12 C11 C16 C15 1.8(11) . . . . ? C1 C11 C16 C15 179.6(6) . . . . ? C14 C15 C16 C11 -1.8(11) . . . . ? C18 N11 C17 C14 98.7(8) . . . . ? C20 N11 C17 C14 -77.5(8) . . . . ? C15 C14 C17 N11 -95.8(8) . . . . ? C13 C14 C17 N11 80.0(8) . . . . ? C19 N12 C18 N11 0.0(8) . . . . ? Pb1 N12 C18 N11 -165.8(4) . . . . ? C20 N11 C18 N12 -0.1(8) . . . . ? C17 N11 C18 N12 -176.8(6) . . . . ? C18 N12 C19 C20 0.1(8) . . . . ? Pb1 N12 C19 C20 163.5(5) . . . . ? N12 C19 C20 N11 -0.2(8) . . . . ? C18 N11 C20 C19 0.1(8) . . . . ? C17 N11 C20 C19 176.9(6) . . . . ? C26 C21 C22 C23 -2.6(13) . . . . ? C2 C21 C22 C23 174.8(8) 7_545 . . . ? C21 C22 C23 C24 -0.2(14) . . . . ? C22 C23 C24 C25 3.5(13) . . . . ? C22 C23 C24 C27 -173.5(8) . . . . ? C23 C24 C25 C26 -4.1(11) . . . . ? C27 C24 C25 C26 173.0(7) . . . . ? C22 C21 C26 C25 2.0(12) . . . . ? C2 C21 C26 C25 -175.4(7) 7_545 . . . ? C24 C25 C26 C21 1.3(12) . . . . ? C28 N21 C27 C24 118.5(8) . . . . ? C30 N21 C27 C24 -57.4(10) . . . . ? C25 C24 C27 N21 -71.5(9) . . . . ? C23 C24 C27 N21 105.5(8) . . . . ? C29 N22 C28 N21 -1.5(9) . . . . ? Pb1 N22 C28 N21 -178.6(4) . . . . ? C30 N21 C28 N22 0.7(9) . . . . ? C27 N21 C28 N22 -175.9(7) . . . . ? C28 N22 C29 C30 1.7(9) . . . . ? Pb1 N22 C29 C30 178.9(5) . . . . ? N22 C29 C30 N21 -1.3(9) . . . . ? C28 N21 C30 C29 0.4(8) . . . . ? C27 N21 C30 C29 176.9(7) . . . . ? C36 C31 C32 C33 1.2(11) . . . . ? C3 C31 C32 C33 -175.5(7) 4_535 . . . ? C31 C32 C33 C34 -0.4(12) . . . . ? C32 C33 C34 C35 -1.8(12) . . . . ? C32 C33 C34 C37 175.5(8) . . . . ? C33 C34 C35 C36 3.2(13) . . . . ? C37 C34 C35 C36 -174.2(8) . . . . ? C34 C35 C36 C31 -2.3(12) . . . . ? C32 C31 C36 C35 0.1(11) . . . . ? C3 C31 C36 C35 176.8(7) 4_535 . . . ? C38 N31 C37 C34 -101.9(10) . . . . ? C40 N31 C37 C34 73.6(11) . . . . ? C35 C34 C37 N31 -161.2(8) . . . . ? C33 C34 C37 N31 21.6(13) . . . . ? C39 N32 C38 N31 -2.7(10) . . . . ? Pb1 N32 C38 N31 153.5(5) . . . . ? C40 N31 C38 N32 2.8(10) . . . . ? C37 N31 C38 N32 178.9(7) . . . . ? C38 N32 C39 C40 1.4(9) . . . . ? Pb1 N32 C39 C40 -152.1(6) . . . . ? C38 N31 C40 C39 -1.8(9) . . . . ? C37 N31 C40 C39 -178.1(7) . . . . ? N32 C39 C40 N31 0.3(10) . . . . ? C61 O6 C61 C62 -168.6(19) 2 . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.018 _refine_diff_density_min -1.067 _refine_diff_density_rms 0.146