data_am155 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34.50 H43.50 N6 O4.75 Pb S2' _chemical_formula_weight 889.56 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' 'S' 'S' 0.1246 0.1234 '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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.593(3) _cell_length_b 12.366(3) _cell_length_c 14.880(4) _cell_angle_alpha 67.814(4) _cell_angle_beta 67.952(4) _cell_angle_gamma 88.071(4) _cell_volume 1816.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 889 _exptl_absorpt_coefficient_mu 4.808 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4464 _exptl_absorpt_correction_T_max 0.4464 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15029 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11357 _reflns_number_gt 10369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0150P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.025(7) _refine_ls_number_reflns 11357 _refine_ls_number_parameters 869 _refine_ls_number_restraints 561 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0769 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 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 Pb1A Pb 0.000005(17) 0.000008(16) -0.000007(15) 0.01985(11) Uani 1 1 d . . . O1A O 0.0535(6) -0.0847(6) -0.1220(5) 0.0239(15) Uani 1 1 d U . . O2A O -0.0471(7) -0.1968(6) 0.1084(6) 0.0211(15) Uani 1 1 d U . . N1A N -0.1440(9) 0.0600(8) -0.0955(8) 0.0236(17) Uani 1 1 d U . . N2A N -0.2218(9) -0.0306(8) 0.1132(7) 0.0225(17) Uani 1 1 d U . . N3A N 0.0770(7) -0.3739(6) 0.0908(6) 0.0193(15) Uani 1 1 d U . . N4A N 0.1887(6) -0.2490(6) -0.1297(6) 0.0250(15) Uani 1 1 d U . . C1A C 0.0287(8) -0.0861(9) -0.1981(8) 0.0227(17) Uani 1 1 d U . . C2A C -0.0570(9) -0.0151(9) -0.2349(8) 0.0194(17) Uani 1 1 d U . . C3A C -0.0715(8) -0.0151(9) -0.3250(7) 0.0212(18) Uani 1 1 d U . . H3AB H -0.1224 0.0382 -0.3525 0.025 Uiso 1 1 calc R . . C4A C -0.0143(9) -0.0902(9) -0.3764(8) 0.0225(18) Uani 1 1 d U . . C5A C 0.0641(8) -0.1605(9) -0.3364(8) 0.0222(18) Uani 1 1 d U . . H5AA H 0.1065 -0.2099 -0.3707 0.027 Uiso 1 1 calc R . . C6A C 0.0856(8) -0.1643(9) -0.2490(7) 0.0207(16) Uani 1 1 d U . . C7A C -0.0358(10) -0.0865(10) -0.4682(9) 0.026(2) Uani 1 1 d U . . H7AA H 0.0112 -0.1433 -0.4940 0.040 Uiso 1 1 calc R . . H7AB H -0.0074 -0.0072 -0.5239 0.040 Uiso 1 1 calc R . . H7AC H -0.1255 -0.1064 -0.4481 0.040 Uiso 1 1 calc R . . C8A C -0.1411(10) 0.0474(9) -0.1781(8) 0.0198(17) Uani 1 1 d U . . H8AA H -0.2014 0.0835 -0.2051 0.024 Uiso 1 1 calc R . . C9A C -0.2561(8) 0.1059(7) -0.0401(6) 0.0222(15) Uani 1 1 d U . . H9AA H -0.3315 0.0588 -0.0305 0.027 Uiso 1 1 calc R . . C10A C -0.2622(8) 0.0840(7) 0.0722(7) 0.0245(16) Uani 1 1 d U . . H10A H -0.1975 0.1437 0.0621 0.029 Uiso 1 1 calc R . . C11A C -0.3882(10) 0.1104(9) 0.1355(9) 0.031(2) Uani 1 1 d U . . H11A H -0.3939 0.0963 0.2072 0.038 Uiso 1 1 calc R . . H11B H -0.4567 0.0585 0.1421 0.038 Uiso 1 1 calc R . . C12A C -0.4009(9) 0.2419(8) 0.0772(8) 0.0318(19) Uani 1 1 d U . . H12A H -0.4838 0.2596 0.1171 0.038 Uiso 1 1 calc R . . H12B H -0.3358 0.2927 0.0761 0.038 Uiso 1 1 calc R . . C13A C -0.3879(9) 0.2712(9) -0.0340(8) 0.033(2) Uani 1 1 d U . . H13A H -0.3871 0.3570 -0.0696 0.039 Uiso 1 1 calc R . . H13B H -0.4607 0.2306 -0.0331 0.039 Uiso 1 1 calc R . . C14A C -0.2660(9) 0.2331(10) -0.0957(8) 0.0275(19) Uani 1 1 d U . . H14A H -0.2044 0.2841 -0.1612 0.033 Uiso 1 1 calc R . . C15A C -0.2955(10) -0.1171(9) 0.1912(8) 0.0203(18) Uani 1 1 d U . . H15A H -0.3785 -0.1037 0.2260 0.024 Uiso 1 1 calc R . . C16A C -0.2622(10) -0.2384(10) 0.2326(8) 0.0202(17) Uani 1 1 d U . . C17A C -0.1441(10) -0.2705(9) 0.1849(8) 0.0193(16) Uani 1 1 d U . . C18A C -0.1322(9) -0.3938(9) 0.2214(7) 0.0192(16) Uani 1 1 d U . . C19A C -0.2338(9) -0.4753(9) 0.3080(8) 0.0210(17) Uani 1 1 d U . . H19A H -0.2222 -0.5561 0.3333 0.025 Uiso 1 1 calc R . . C20A C -0.3458(9) -0.4444(10) 0.3564(9) 0.0242(18) Uani 1 1 d U . . C21A C -0.3595(9) -0.3212(8) 0.3170(8) 0.0204(18) Uani 1 1 d U . . H21A H -0.4366 -0.2958 0.3493 0.024 Uiso 1 1 calc R . . C22A C -0.4542(9) -0.5303(9) 0.4472(8) 0.027(2) Uani 1 1 d U . . H22A H -0.4278 -0.6090 0.4687 0.041 Uiso 1 1 calc R . . H22B H -0.5238 -0.5321 0.4255 0.041 Uiso 1 1 calc R . . H22C H -0.4815 -0.5058 0.5067 0.041 Uiso 1 1 calc R . . C23A C -0.0259(8) -0.4376(8) 0.1664(7) 0.0214(17) Uani 1 1 d U . . H23A H -0.0301 -0.5205 0.1866 0.026 Uiso 1 1 calc R . . C24A C 0.1744(7) -0.4256(7) 0.0260(6) 0.0220(14) Uani 1 1 d U . . H24A H 0.1326 -0.4838 0.0124 0.026 Uiso 1 1 calc R . . C25A C 0.2613(7) -0.3317(6) -0.0792(6) 0.0219(13) Uani 1 1 d U . . H25A H 0.3144 -0.2856 -0.0631 0.026 Uiso 1 1 calc R . . C26A C 0.3480(9) -0.3892(9) -0.1462(9) 0.0256(18) Uani 1 1 d U . . H26A H 0.4009 -0.3288 -0.2160 0.031 Uiso 1 1 calc R . . H26B H 0.2989 -0.4437 -0.1571 0.031 Uiso 1 1 calc R . . C27A C 0.4331(7) -0.4593(7) -0.0879(6) 0.0297(16) Uani 1 1 d U . . H27A H 0.4902 -0.4994 -0.1301 0.036 Uiso 1 1 calc R . . H27B H 0.4848 -0.4039 -0.0801 0.036 Uiso 1 1 calc R . . C28A C 0.3502(8) -0.5503(7) 0.0209(7) 0.0307(18) Uani 1 1 d U . . H28A H 0.4036 -0.5928 0.0581 0.037 Uiso 1 1 calc R . . H28B H 0.3026 -0.6084 0.0127 0.037 Uiso 1 1 calc R . . C29A C 0.2581(11) -0.4896(10) 0.0867(10) 0.028(2) Uani 1 1 d U . . H29A H 0.3049 -0.4319 0.0961 0.034 Uiso 1 1 calc R . . H29B H 0.2051 -0.5487 0.1573 0.034 Uiso 1 1 calc R . . C30A C 0.1619(7) -0.2473(8) -0.2090(7) 0.0229(17) Uani 1 1 d U . . H30A H 0.1937 -0.3020 -0.2402 0.027 Uiso 1 1 calc R . . Pb1B Pb -0.324360(18) -0.348515(17) -0.454250(16) 0.02189(12) Uani 1 1 d . . . O1B O -0.3480(6) -0.2407(6) -0.3527(5) 0.0230(14) Uani 1 1 d U . . O2B O -0.2861(7) -0.1546(7) -0.5753(6) 0.0295(17) Uani 1 1 d U . . N1B N -0.1835(9) -0.4166(8) -0.3607(7) 0.0229(17) Uani 1 1 d U . . N2B N -0.0923(9) -0.3080(8) -0.5722(8) 0.0240(17) Uani 1 1 d U . . N3B N -0.4247(7) 0.0047(7) -0.5521(6) 0.0235(16) Uani 1 1 d U . . N4B N -0.4711(6) -0.0653(6) -0.3384(5) 0.0181(13) Uani 1 1 d U . . C1B C -0.3257(8) -0.2531(9) -0.2682(8) 0.0211(16) Uani 1 1 d U . . C2B C -0.2469(9) -0.3348(10) -0.2289(8) 0.0232(18) Uani 1 1 d U . . C3B C -0.2292(8) -0.3335(9) -0.1417(8) 0.0223(18) Uani 1 1 d U . . H3BB H -0.1722 -0.3826 -0.1192 0.027 Uiso 1 1 calc R . . C4B C -0.2876(9) -0.2670(9) -0.0854(8) 0.0218(18) Uani 1 1 d U . . C5B C -0.3600(8) -0.1835(9) -0.1251(8) 0.0220(18) Uani 1 1 d U . . H5BA H -0.3962 -0.1319 -0.0914 0.026 Uiso 1 1 calc R . . C6B C -0.3786(8) -0.1768(9) -0.2135(8) 0.0213(16) Uani 1 1 d U . . C7B C -0.2624(10) -0.2715(11) 0.0107(9) 0.031(3) Uani 1 1 d U . . H7BA H -0.2102 -0.3338 0.0278 0.046 Uiso 1 1 calc R . . H7BB H -0.3422 -0.2879 0.0714 0.046 Uiso 1 1 calc R . . H7BC H -0.2186 -0.1956 -0.0060 0.046 Uiso 1 1 calc R . . C8B C -0.1760(10) -0.4076(9) -0.2825(9) 0.0239(19) Uani 1 1 d U . . H8BA H -0.1192 -0.4519 -0.2555 0.029 Uiso 1 1 calc R . . C9B C -0.1031(8) -0.4845(7) -0.4190(6) 0.0253(16) Uani 1 1 d U . . H9BA H -0.1605 -0.5342 -0.4282 0.030 Uiso 1 1 calc R . . C10B C -0.0191(8) -0.4010(7) -0.5275(7) 0.0251(16) Uani 1 1 d U . . H10B H 0.0490 -0.3609 -0.5208 0.030 Uiso 1 1 calc R . . C11B C 0.0423(10) -0.4683(9) -0.5965(8) 0.031(2) Uani 1 1 d U . . H11C H 0.0969 -0.4125 -0.6681 0.037 Uiso 1 1 calc R . . H11D H -0.0231 -0.5112 -0.6026 0.037 Uiso 1 1 calc R . . C12B C 0.1200(9) -0.5551(8) -0.5482(7) 0.0322(19) Uani 1 1 d U . . H12C H 0.1532 -0.6039 -0.5897 0.039 Uiso 1 1 calc R . . H12D H 0.1922 -0.5113 -0.5512 0.039 Uiso 1 1 calc R . . C13B C 0.0413(9) -0.6348(9) -0.4339(8) 0.034(2) Uani 1 1 d U . . H13C H 0.0349 -0.7182 -0.4083 0.041 Uiso 1 1 calc R . . C14B C -0.0268(9) -0.5692(9) -0.3634(9) 0.031(2) Uani 1 1 d U . . H14B H 0.0346 -0.5243 -0.3547 0.037 Uiso 1 1 calc R . . H14C H -0.0834 -0.6256 -0.2928 0.037 Uiso 1 1 calc R . . C15B C -0.0244(11) -0.2112(9) -0.6501(9) 0.0239(19) Uani 1 1 d U . . H15B H 0.0627 -0.2154 -0.6821 0.029 Uiso 1 1 calc R . . C16B C -0.0660(11) -0.1013(10) -0.6918(9) 0.0225(17) Uani 1 1 d U . . C17B C -0.1924(10) -0.0738(10) -0.6457(9) 0.0246(17) Uani 1 1 d U . . C18B C -0.2123(9) 0.0474(9) -0.6830(8) 0.0218(16) Uani 1 1 d U . . C19B C -0.1181(8) 0.1346(9) -0.7638(8) 0.0214(17) Uani 1 1 d U . . H19B H -0.1341 0.2144 -0.7858 0.026 Uiso 1 1 calc R . . C20B C 0.0020(9) 0.1057(9) -0.8138(9) 0.0226(18) Uani 1 1 d U . . C21B C 0.0244(10) -0.0053(9) -0.7741(8) 0.0222(18) Uani 1 1 d U . . H21B H 0.1077 -0.0218 -0.8033 0.027 Uiso 1 1 calc R . . C22B C 0.1032(9) 0.2030(9) -0.9010(9) 0.030(2) Uani 1 1 d U . . H22D H 0.0695 0.2786 -0.9132 0.044 Uiso 1 1 calc R . . H22E H 0.1317 0.1884 -0.9658 0.044 Uiso 1 1 calc R . . H22F H 0.1740 0.2051 -0.8806 0.044 Uiso 1 1 calc R . . C23B C -0.3285(8) 0.0830(8) -0.6291(7) 0.0203(16) Uani 1 1 d U . . H23B H -0.3368 0.1645 -0.6490 0.024 Uiso 1 1 calc R . . C24B C -0.5398(8) 0.0336(7) -0.4841(6) 0.0266(15) Uani 1 1 d U . . H24B H -0.6073 -0.0330 -0.4553 0.032 Uiso 1 1 calc R . . C25B C -0.5214(7) 0.0423(7) -0.3910(6) 0.0239(14) Uani 1 1 d U . . H25B H -0.4591 0.1125 -0.4177 0.029 Uiso 1 1 calc R . . C26B C -0.6482(9) 0.0588(10) -0.3129(9) 0.030(2) Uani 1 1 d U . . H26C H -0.7097 -0.0118 -0.2836 0.036 Uiso 1 1 calc R . . H26D H -0.6352 0.0671 -0.2536 0.036 Uiso 1 1 calc R . . C27B C -0.6996(8) 0.1663(7) -0.3676(6) 0.0321(16) Uani 1 1 d U . . H27C H -0.6428 0.2378 -0.3896 0.039 Uiso 1 1 calc R . . H27D H -0.7828 0.1718 -0.3179 0.039 Uiso 1 1 calc R . . C28B C -0.7122(9) 0.1604(8) -0.4648(7) 0.0336(18) Uani 1 1 d U . . H28C H -0.7749 0.0931 -0.4421 0.040 Uiso 1 1 calc R . . H28D H -0.7421 0.2334 -0.5013 0.040 Uiso 1 1 calc R . . C29B C -0.5861(11) 0.1460(11) -0.5411(10) 0.031(2) Uani 1 1 d U . . H29C H -0.5960 0.1413 -0.6028 0.037 Uiso 1 1 calc R . . H29D H -0.5240 0.2149 -0.5666 0.037 Uiso 1 1 calc R . . C30B C -0.4445(7) -0.0829(8) -0.2567(7) 0.0201(16) Uani 1 1 d U . . H30B H -0.4705 -0.0297 -0.2228 0.024 Uiso 1 1 calc R . . S1T S 0.0296(3) 0.4537(4) -0.1254(3) 0.0502(10) Uani 1 1 d U . . N1T N -0.1413(10) 0.4271(9) 0.0741(8) 0.032(2) Uani 1 1 d U . . C1T C -0.0698(11) 0.4343(10) -0.0119(9) 0.029(2) Uani 1 1 d U . . S2T S -0.3350(4) 0.2122(4) -0.3286(4) 0.0663(12) Uani 1 1 d U . . N2T N -0.1940(9) 0.2161(9) -0.5349(7) 0.027(2) Uani 1 1 d U . . C2T C -0.2482(14) 0.2259(13) -0.4549(13) 0.052(3) Uani 1 1 d U . . S3T S -0.7328(4) -0.3676(5) -0.4492(5) 0.115(2) Uani 1 1 d U . . N3T N -0.5563(10) -0.2438(11) -0.4305(9) 0.044(3) Uani 1 1 d U . . C3T C -0.6287(12) -0.2905(14) -0.4376(13) 0.060(3) Uani 1 1 d U . . S4T S -0.5819(3) 0.0477(3) -0.0493(3) 0.0506(8) Uani 1 1 d U . . N4T N -0.7733(10) -0.1165(9) -0.0056(8) 0.034(2) Uani 1 1 d U . . C4T C -0.6959(10) -0.0509(9) -0.0189(8) 0.025(2) Uani 1 1 d U . . O1ME O -0.6913(18) -0.0557(14) -0.6677(17) 0.278(12) Uani 1 1 d U . . H1MD H -0.7088 -0.0237 -0.7210 0.417 Uiso 1 1 calc R . . C1ME C -0.749(3) -0.1897(17) -0.609(2) 0.275(13) Uani 1 1 d U . . H1MA H -0.7991 -0.2063 -0.6445 0.412 Uiso 1 1 calc R . . H1MB H -0.8034 -0.2063 -0.5357 0.412 Uiso 1 1 calc R . . H1MC H -0.6817 -0.2395 -0.6120 0.412 Uiso 1 1 calc R . . O2ME O -0.5965(13) -0.2421(17) 0.1836(10) 0.203(8) Uani 1 1 d U . . H2MD H -0.5784 -0.3089 0.2135 0.304 Uiso 1 1 calc R . . C2ME C -0.7308(16) -0.252(2) 0.1985(12) 0.157(7) Uani 1 1 d U . . H2MA H -0.7740 -0.3283 0.2544 0.236 Uiso 1 1 calc R . . H2MB H -0.7362 -0.2454 0.1325 0.236 Uiso 1 1 calc R . . H2MC H -0.7704 -0.1886 0.2184 0.236 Uiso 1 1 calc R . . O3ME O -0.3724(9) 0.3527(7) 0.2466(7) 0.036(2) Uani 1 1 d U . . H3MD H -0.3711 0.3492 0.3037 0.054 Uiso 1 1 calc R . . C3ME C -0.4618(12) 0.4272(10) 0.2217(10) 0.034(3) Uani 1 1 d U . . H3MA H -0.4990 0.4597 0.2755 0.052 Uiso 1 1 calc R . . H3MB H -0.5278 0.3816 0.2199 0.052 Uiso 1 1 calc R . . H3MC H -0.4201 0.4917 0.1526 0.052 Uiso 1 1 calc R . . O4ME O 0.0478(11) 0.3014(10) -0.6977(8) 0.066(3) Uani 1 1 d U . . H4MD H -0.0202 0.2905 -0.6460 0.099 Uiso 1 1 calc R . . C4ME C 0.1259(14) 0.2110(13) -0.6672(12) 0.065(4) Uani 1 1 d U . . H4MA H 0.1841 0.2000 -0.7299 0.097 Uiso 1 1 calc R . . H4MB H 0.0724 0.1367 -0.6167 0.097 Uiso 1 1 calc R . . H4MC H 0.1737 0.2357 -0.6345 0.097 Uiso 1 1 calc R . . C5ME C -0.5805(15) -0.6222(10) -0.2523(9) 0.091(4) Uani 1 1 d U . . H5MA H -0.6010 -0.7013 -0.1961 0.137 Uiso 1 1 calc R . . H5MB H -0.5951 -0.6252 -0.3122 0.137 Uiso 1 1 calc R . . H5MC H -0.6337 -0.5688 -0.2258 0.137 Uiso 1 1 calc R . . O5ME O -0.4467(14) -0.5791(7) -0.2870(7) 0.095(4) Uani 1 1 d U . . H1O5 H -0.4315 -0.5089 -0.3330 0.142 Uiso 1 1 d R . . O1W O 0.145(5) 0.244(4) -0.172(3) 0.22(2) Uiso 0.50 1 d P . . H1W1 H 0.0665 0.2319 -0.1541 0.333 Uiso 0.50 1 d PR . . H2W1 H 0.2207 0.2741 -0.1952 0.333 Uiso 0.50 1 d 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 Pb1A 0.0245(2) 0.0186(3) 0.0210(3) -0.0093(2) -0.0124(2) 0.00485(19) O1A 0.028(3) 0.034(3) 0.017(3) -0.014(2) -0.014(2) 0.014(2) O2A 0.022(3) 0.020(3) 0.020(3) -0.010(2) -0.005(2) 0.009(2) N1A 0.026(3) 0.024(3) 0.025(3) -0.013(3) -0.012(3) 0.011(3) N2A 0.030(3) 0.023(3) 0.022(3) -0.012(3) -0.015(3) 0.011(3) N3A 0.021(3) 0.016(3) 0.023(3) -0.008(2) -0.010(2) 0.008(2) N4A 0.019(3) 0.028(3) 0.026(3) -0.006(2) -0.012(2) 0.003(2) C1A 0.022(3) 0.028(3) 0.021(3) -0.011(2) -0.012(2) 0.007(2) C2A 0.021(3) 0.022(3) 0.019(3) -0.010(2) -0.010(2) 0.006(2) C3A 0.021(3) 0.024(3) 0.017(3) -0.005(3) -0.009(3) 0.002(3) C4A 0.029(3) 0.023(3) 0.016(3) -0.009(3) -0.008(3) 0.001(3) C5A 0.025(3) 0.025(3) 0.016(3) -0.009(3) -0.007(3) 0.004(3) C6A 0.020(3) 0.026(3) 0.020(3) -0.012(2) -0.010(2) 0.008(2) C7A 0.029(5) 0.025(5) 0.026(5) -0.006(4) -0.016(4) 0.002(4) C8A 0.023(3) 0.022(3) 0.021(3) -0.011(3) -0.014(3) 0.004(3) C9A 0.027(3) 0.026(3) 0.024(3) -0.015(2) -0.017(2) 0.012(2) C10A 0.030(3) 0.028(3) 0.026(3) -0.016(2) -0.018(2) 0.012(2) C11A 0.037(3) 0.033(3) 0.032(3) -0.019(3) -0.016(3) 0.013(3) C12A 0.034(3) 0.032(3) 0.037(4) -0.019(3) -0.017(3) 0.015(3) C13A 0.038(3) 0.034(3) 0.034(3) -0.016(3) -0.019(3) 0.014(3) C14A 0.032(3) 0.031(3) 0.026(3) -0.013(3) -0.017(3) 0.012(3) C15A 0.023(3) 0.024(3) 0.019(3) -0.010(3) -0.013(3) 0.006(3) C16A 0.026(3) 0.022(3) 0.019(3) -0.013(2) -0.009(2) 0.003(3) C17A 0.027(3) 0.020(3) 0.016(3) -0.009(2) -0.010(2) 0.005(2) C18A 0.025(3) 0.021(3) 0.019(3) -0.011(2) -0.013(2) 0.005(2) C19A 0.029(3) 0.020(3) 0.022(3) -0.012(3) -0.014(3) 0.005(3) C20A 0.029(3) 0.028(3) 0.022(3) -0.013(3) -0.013(3) 0.003(3) C21A 0.025(3) 0.022(3) 0.021(3) -0.014(3) -0.011(3) 0.005(3) C22A 0.034(5) 0.031(5) 0.025(4) -0.016(4) -0.016(4) 0.004(4) C23A 0.023(3) 0.020(3) 0.023(3) -0.005(2) -0.014(3) 0.003(3) C24A 0.022(3) 0.020(3) 0.027(3) -0.010(2) -0.013(2) 0.009(2) C25A 0.021(3) 0.024(3) 0.026(3) -0.008(2) -0.016(2) 0.007(2) C26A 0.026(3) 0.022(3) 0.027(3) -0.008(3) -0.012(3) 0.009(3) C27A 0.028(3) 0.026(3) 0.033(3) -0.011(3) -0.011(3) 0.010(3) C28A 0.028(3) 0.025(3) 0.035(3) -0.007(3) -0.014(3) 0.012(3) C29A 0.029(3) 0.024(3) 0.030(3) -0.008(3) -0.013(3) 0.010(3) C30A 0.019(3) 0.025(3) 0.025(3) -0.010(3) -0.010(3) 0.005(3) Pb1B 0.0300(3) 0.0196(3) 0.0208(3) -0.0098(2) -0.0133(2) 0.0068(2) O1B 0.031(3) 0.030(3) 0.021(3) -0.017(2) -0.018(2) 0.014(2) O2B 0.030(3) 0.027(3) 0.025(3) -0.007(3) -0.007(3) 0.005(3) N1B 0.029(3) 0.019(3) 0.025(3) -0.012(3) -0.012(3) 0.011(3) N2B 0.032(3) 0.024(3) 0.024(3) -0.013(3) -0.017(3) 0.015(3) N3B 0.025(3) 0.029(3) 0.020(3) -0.013(2) -0.010(2) 0.007(2) N4B 0.020(3) 0.023(3) 0.019(3) -0.012(2) -0.012(2) 0.009(2) C1B 0.024(3) 0.024(3) 0.022(3) -0.012(2) -0.012(2) 0.006(2) C2B 0.023(3) 0.024(3) 0.021(3) -0.006(3) -0.009(2) 0.005(3) C3B 0.022(3) 0.022(3) 0.022(3) -0.005(3) -0.011(3) 0.001(3) C4B 0.024(3) 0.022(3) 0.021(3) -0.007(3) -0.012(3) -0.003(3) C5B 0.026(3) 0.019(3) 0.021(3) -0.009(3) -0.008(3) -0.001(3) C6B 0.019(3) 0.024(3) 0.022(3) -0.008(2) -0.010(2) 0.005(2) C7B 0.030(5) 0.042(5) 0.022(5) -0.009(4) -0.013(4) -0.004(4) C8B 0.025(3) 0.020(3) 0.024(3) -0.007(3) -0.009(3) 0.007(3) C9B 0.033(3) 0.023(3) 0.026(3) -0.013(2) -0.015(2) 0.015(2) C10B 0.035(3) 0.024(3) 0.025(3) -0.013(2) -0.018(2) 0.015(2) C11B 0.039(3) 0.027(3) 0.028(3) -0.014(3) -0.015(3) 0.019(3) C12B 0.041(4) 0.027(3) 0.030(3) -0.013(3) -0.015(3) 0.023(3) C13B 0.039(4) 0.025(3) 0.037(4) -0.009(3) -0.018(3) 0.021(3) C14B 0.037(4) 0.025(3) 0.031(3) -0.009(3) -0.017(3) 0.018(3) C15B 0.031(3) 0.029(3) 0.019(3) -0.014(3) -0.014(3) 0.015(3) C16B 0.030(3) 0.026(3) 0.019(3) -0.012(2) -0.014(3) 0.012(3) C17B 0.028(3) 0.027(3) 0.021(3) -0.011(2) -0.011(2) 0.008(3) C18B 0.028(3) 0.025(3) 0.021(3) -0.013(2) -0.015(2) 0.008(2) C19B 0.025(3) 0.023(3) 0.025(3) -0.016(3) -0.013(3) 0.008(3) C20B 0.026(3) 0.027(3) 0.023(3) -0.015(3) -0.012(3) 0.004(3) C21B 0.023(3) 0.029(3) 0.021(3) -0.015(3) -0.010(3) 0.009(3) C22B 0.022(4) 0.022(4) 0.036(5) -0.010(4) -0.003(4) 0.009(3) C23B 0.030(3) 0.022(3) 0.019(3) -0.013(2) -0.016(3) 0.009(3) C24B 0.030(3) 0.028(3) 0.024(3) -0.011(2) -0.013(2) 0.014(2) C25B 0.027(3) 0.025(3) 0.022(3) -0.008(2) -0.013(2) 0.013(2) C26B 0.033(3) 0.032(3) 0.024(3) -0.011(3) -0.011(3) 0.012(3) C27B 0.031(3) 0.033(3) 0.031(3) -0.015(3) -0.011(3) 0.017(3) C28B 0.034(3) 0.035(3) 0.031(3) -0.012(3) -0.015(3) 0.021(3) C29B 0.034(3) 0.033(3) 0.028(3) -0.010(3) -0.017(3) 0.018(3) C30B 0.017(3) 0.026(3) 0.022(3) -0.013(3) -0.009(2) 0.005(3) S1T 0.0387(16) 0.073(2) 0.0264(16) -0.0012(15) -0.0174(13) -0.0058(15) N1T 0.039(5) 0.034(5) 0.029(5) -0.010(4) -0.022(4) 0.004(4) C1T 0.028(4) 0.027(4) 0.029(4) -0.002(4) -0.019(4) -0.002(4) S2T 0.071(3) 0.077(3) 0.066(3) -0.036(2) -0.035(2) 0.018(2) N2T 0.030(4) 0.054(5) 0.016(4) -0.026(4) -0.019(3) 0.011(4) C2T 0.048(5) 0.048(6) 0.063(6) -0.011(5) -0.037(5) 0.009(5) S3T 0.0399(19) 0.144(4) 0.228(6) -0.158(4) -0.040(3) 0.021(2) N3T 0.040(5) 0.066(6) 0.057(6) -0.043(5) -0.036(5) 0.023(5) C3T 0.027(5) 0.093(6) 0.111(7) -0.093(5) -0.029(5) 0.024(5) S4T 0.0367(15) 0.0560(17) 0.0670(18) -0.0388(14) -0.0135(13) -0.0001(12) N4T 0.032(5) 0.033(5) 0.031(4) -0.010(4) -0.010(4) 0.006(4) C4T 0.028(4) 0.022(4) 0.021(4) -0.006(3) -0.008(4) 0.012(4) O1ME 0.254(18) 0.123(10) 0.31(2) -0.143(12) 0.111(15) -0.082(11) C1ME 0.272(19) 0.110(11) 0.30(2) -0.153(13) 0.120(16) -0.067(12) O2ME 0.131(9) 0.337(18) 0.115(8) -0.077(10) -0.046(8) 0.165(12) C2ME 0.124(10) 0.300(18) 0.089(8) -0.104(10) -0.065(8) 0.149(12) O3ME 0.062(5) 0.025(4) 0.035(5) -0.018(4) -0.028(4) 0.018(4) C3ME 0.063(6) 0.021(5) 0.041(6) -0.021(4) -0.035(5) 0.009(4) O4ME 0.068(7) 0.057(6) 0.048(6) 0.000(5) -0.016(5) -0.006(5) C4ME 0.064(8) 0.063(8) 0.040(7) 0.000(6) -0.012(6) -0.010(6) C5ME 0.188(12) 0.036(5) 0.052(6) -0.012(5) -0.052(7) -0.007(6) O5ME 0.203(11) 0.027(4) 0.039(4) -0.004(3) -0.039(5) -0.009(5) _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 Pb1A O2A 2.300(7) . ? Pb1A O1A 2.307(7) . ? Pb1A N2A 2.434(9) . ? Pb1A N1A 2.502(10) . ? O1A C1A 1.275(12) . ? O2A C17A 1.309(12) . ? N1A C8A 1.284(14) . ? N1A C9A 1.480(12) . ? N2A C15A 1.265(13) . ? N2A C10A 1.456(12) . ? N3A C23A 1.302(11) . ? N3A C24A 1.488(10) . ? N4A C30A 1.321(12) . ? N4A C25A 1.468(9) . ? C1A C2A 1.430(14) . ? C1A C6A 1.442(14) . ? C2A C3A 1.413(15) . ? C2A C8A 1.444(13) . ? C3A C4A 1.415(13) . ? C4A C5A 1.378(14) . ? C4A C7A 1.460(16) . ? C5A C6A 1.398(14) . ? C6A C30A 1.435(12) . ? C9A C14A 1.499(13) . ? C9A C10A 1.563(12) . ? C10A C11A 1.515(13) . ? C11A C12A 1.559(14) . ? C12A C13A 1.502(13) . ? C13A C14A 1.539(14) . ? C15A C16A 1.490(14) . ? C16A C21A 1.394(14) . ? C16A C17A 1.409(14) . ? C17A C18A 1.435(14) . ? C18A C23A 1.418(12) . ? C18A C19A 1.423(13) . ? C19A C20A 1.350(13) . ? C20A C21A 1.438(14) . ? C20A C22A 1.505(14) . ? C24A C25A 1.528(10) . ? C24A C29A 1.565(13) . ? C25A C26A 1.499(13) . ? C26A C27A 1.579(13) . ? C27A C28A 1.530(11) . ? C28A C29A 1.543(14) . ? Pb1B O1B 2.307(7) . ? Pb1B O2B 2.325(8) . ? Pb1B N1B 2.459(10) . ? Pb1B N2B 2.540(9) . ? O1B C1B 1.329(12) . ? O2B C17B 1.305(13) . ? N1B C8B 1.245(14) . ? N1B C9B 1.488(11) . ? N2B C15B 1.314(14) . ? N2B C10B 1.505(12) . ? N3B C23B 1.330(11) . ? N3B C24B 1.470(10) . ? N4B C30B 1.304(11) . ? N4B C25B 1.492(9) . ? C1B C2B 1.446(14) . ? C1B C6B 1.448(14) . ? C2B C3B 1.393(15) . ? C2B C8B 1.457(14) . ? C3B C4B 1.376(14) . ? C4B C5B 1.404(14) . ? C4B C7B 1.545(15) . ? C5B C6B 1.382(14) . ? C6B C30B 1.445(12) . ? C9B C10B 1.500(12) . ? C9B C14B 1.548(13) . ? C10B C11B 1.520(13) . ? C11B C12B 1.523(13) . ? C12B C13B 1.526(13) . ? C13B C14B 1.536(15) . ? C15B C16B 1.418(14) . ? C16B C21B 1.424(15) . ? C16B C17B 1.457(15) . ? C17B C18B 1.432(15) . ? C18B C19B 1.384(13) . ? C18B C23B 1.438(12) . ? C19B C20B 1.418(13) . ? C20B C21B 1.334(14) . ? C20B C22B 1.510(14) . ? C24B C25B 1.520(11) . ? C24B C29B 1.530(13) . ? C25B C26B 1.559(12) . ? C26B C27B 1.510(13) . ? C27B C28B 1.536(13) . ? C28B C29B 1.532(14) . ? S1T C1T 1.578(13) . ? N1T C1T 1.206(15) . ? S2T C2T 1.711(18) . ? N2T C2T 1.170(18) . ? S3T C3T 1.659(14) . ? N3T C3T 1.093(16) . ? S4T C4T 1.637(12) . ? N4T C4T 1.139(15) . ? O1ME C1ME 1.58(2) . ? O2ME C2ME 1.49(2) . ? O3ME C3ME 1.424(13) . ? O4ME C4ME 1.460(17) . ? C5ME O5ME 1.48(2) . ? 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 O2A Pb1A O1A 78.8(2) . . ? O2A Pb1A N2A 73.6(3) . . ? O1A Pb1A N2A 115.7(3) . . ? O2A Pb1A N1A 110.6(3) . . ? O1A Pb1A N1A 72.9(3) . . ? N2A Pb1A N1A 65.1(3) . . ? C1A O1A Pb1A 141.4(6) . . ? C17A O2A Pb1A 138.7(6) . . ? C8A N1A C9A 116.2(9) . . ? C8A N1A Pb1A 130.3(7) . . ? C9A N1A Pb1A 113.2(6) . . ? C15A N2A C10A 122.5(9) . . ? C15A N2A Pb1A 134.4(8) . . ? C10A N2A Pb1A 103.1(6) . . ? C23A N3A C24A 121.4(7) . . ? C30A N4A C25A 126.7(7) . . ? O1A C1A C2A 122.9(9) . . ? O1A C1A C6A 119.8(9) . . ? C2A C1A C6A 117.2(9) . . ? C3A C2A C1A 119.2(9) . . ? C3A C2A C8A 117.0(9) . . ? C1A C2A C8A 123.4(10) . . ? C4A C3A C2A 123.6(9) . . ? C5A C4A C3A 115.4(10) . . ? C5A C4A C7A 124.3(9) . . ? C3A C4A C7A 120.3(9) . . ? C4A C5A C6A 124.7(10) . . ? C5A C6A C30A 120.1(9) . . ? C5A C6A C1A 119.5(9) . . ? C30A C6A C1A 120.3(9) . . ? N1A C8A C2A 127.7(10) . . ? N1A C9A C14A 115.9(8) . . ? N1A C9A C10A 109.2(7) . . ? C14A C9A C10A 109.3(7) . . ? N2A C10A C11A 119.8(8) . . ? N2A C10A C9A 107.7(7) . . ? C11A C10A C9A 109.0(7) . . ? C10A C11A C12A 108.3(8) . . ? C13A C12A C11A 113.1(8) . . ? C12A C13A C14A 110.7(8) . . ? C9A C14A C13A 112.0(8) . . ? N2A C15A C16A 125.0(10) . . ? C21A C16A C17A 121.6(10) . . ? C21A C16A C15A 115.4(9) . . ? C17A C16A C15A 122.8(10) . . ? O2A C17A C16A 124.9(10) . . ? O2A C17A C18A 118.4(9) . . ? C16A C17A C18A 116.7(9) . . ? C23A C18A C19A 118.9(9) . . ? C23A C18A C17A 121.2(8) . . ? C19A C18A C17A 119.6(9) . . ? C20A C19A C18A 123.8(9) . . ? C19A C20A C21A 116.6(9) . . ? C19A C20A C22A 124.0(10) . . ? C21A C20A C22A 119.4(9) . . ? C16A C21A C20A 121.5(9) . . ? N3A C23A C18A 125.6(9) . . ? N3A C24A C25A 112.0(6) . . ? N3A C24A C29A 109.5(7) . . ? C25A C24A C29A 107.3(7) . . ? N4A C25A C26A 114.7(7) . . ? N4A C25A C24A 110.8(6) . . ? C26A C25A C24A 109.8(7) . . ? C25A C26A C27A 108.2(8) . . ? C28A C27A C26A 109.6(7) . . ? C27A C28A C29A 110.4(7) . . ? C28A C29A C24A 107.7(9) . . ? N4A C30A C6A 121.4(9) . . ? O1B Pb1B O2B 76.5(3) . . ? O1B Pb1B N1B 73.4(3) . . ? O2B Pb1B N1B 118.5(3) . . ? O1B Pb1B N2B 104.8(3) . . ? O2B Pb1B N2B 72.9(3) . . ? N1B Pb1B N2B 65.1(3) . . ? C1B O1B Pb1B 135.9(6) . . ? C17B O2B Pb1B 140.2(7) . . ? C8B N1B C9B 124.4(9) . . ? C8B N1B Pb1B 133.8(8) . . ? C9B N1B Pb1B 101.7(6) . . ? C15B N2B C10B 115.3(9) . . ? C15B N2B Pb1B 130.6(7) . . ? C10B N2B Pb1B 112.3(6) . . ? C23B N3B C24B 124.9(8) . . ? C30B N4B C25B 123.9(7) . . ? O1B C1B C2B 124.5(9) . . ? O1B C1B C6B 118.6(8) . . ? C2B C1B C6B 116.8(9) . . ? C3B C2B C1B 117.3(10) . . ? C3B C2B C8B 119.3(10) . . ? C1B C2B C8B 123.1(10) . . ? C4B C3B C2B 125.3(10) . . ? C3B C4B C5B 117.9(10) . . ? C3B C4B C7B 121.7(9) . . ? C5B C4B C7B 119.9(10) . . ? C6B C5B C4B 119.8(10) . . ? C5B C6B C30B 117.7(9) . . ? C5B C6B C1B 122.5(9) . . ? C30B C6B C1B 119.6(9) . . ? N1B C8B C2B 125.5(11) . . ? N1B C9B C10B 109.3(7) . . ? N1B C9B C14B 116.0(8) . . ? C10B C9B C14B 111.0(7) . . ? C9B C10B N2B 109.5(7) . . ? C9B C10B C11B 110.3(7) . . ? N2B C10B C11B 113.5(8) . . ? C10B C11B C12B 109.7(9) . . ? C13B C12B C11B 111.0(8) . . ? C12B C13B C14B 114.6(8) . . ? C13B C14B C9B 106.8(9) . . ? N2B C15B C16B 127.5(11) . . ? C15B C16B C21B 118.6(10) . . ? C15B C16B C17B 124.2(10) . . ? C21B C16B C17B 116.5(9) . . ? O2B C17B C18B 120.1(9) . . ? O2B C17B C16B 122.7(10) . . ? C18B C17B C16B 117.2(10) . . ? C19B C18B C23B 117.8(9) . . ? C19B C18B C17B 122.0(9) . . ? C23B C18B C17B 119.9(9) . . ? C18B C19B C20B 120.3(9) . . ? C21B C20B C19B 118.0(10) . . ? C21B C20B C22B 122.5(9) . . ? C19B C20B C22B 119.1(9) . . ? C20B C21B C16B 125.6(10) . . ? N3B C23B C18B 121.7(8) . . ? N3B C24B C25B 110.1(6) . . ? N3B C24B C29B 114.2(7) . . ? C25B C24B C29B 109.8(8) . . ? N4B C25B C24B 109.6(6) . . ? N4B C25B C26B 111.4(7) . . ? C24B C25B C26B 109.7(7) . . ? C27B C26B C25B 110.9(8) . . ? C26B C27B C28B 110.9(8) . . ? C29B C28B C27B 110.8(8) . . ? C24B C29B C28B 109.2(9) . . ? N4B C30B C6B 125.4(8) . . ? N1T C1T S1T 175.1(12) . . ? N2T C2T S2T 169.2(14) . . ? N3T C3T S3T 176.4(13) . . ? N4T C4T S4T 174.9(10) . . ? 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 O2A Pb1A O1A C1A 122.2(9) . . . . ? N2A Pb1A O1A C1A 56.7(10) . . . . ? N1A Pb1A O1A C1A 6.4(9) . . . . ? O1A Pb1A O2A C17A -121.6(10) . . . . ? N2A Pb1A O2A C17A -0.4(10) . . . . ? N1A Pb1A O2A C17A -54.9(10) . . . . ? O2A Pb1A N1A C8A -80.3(10) . . . . ? O1A Pb1A N1A C8A -9.7(9) . . . . ? N2A Pb1A N1A C8A -139.8(11) . . . . ? O2A Pb1A N1A C9A 92.8(6) . . . . ? O1A Pb1A N1A C9A 163.4(7) . . . . ? N2A Pb1A N1A C9A 33.3(6) . . . . ? O2A Pb1A N2A C15A 6.0(11) . . . . ? O1A Pb1A N2A C15A 74.5(12) . . . . ? N1A Pb1A N2A C15A 128.7(12) . . . . ? O2A Pb1A N2A C10A -175.2(6) . . . . ? O1A Pb1A N2A C10A -106.6(6) . . . . ? N1A Pb1A N2A C10A -52.4(6) . . . . ? Pb1A O1A C1A C2A 2.3(15) . . . . ? Pb1A O1A C1A C6A -176.0(6) . . . . ? O1A C1A C2A C3A 175.0(9) . . . . ? C6A C1A C2A C3A -6.7(13) . . . . ? O1A C1A C2A C8A -12.3(15) . . . . ? C6A C1A C2A C8A 166.1(9) . . . . ? C1A C2A C3A C4A 6.0(14) . . . . ? C8A C2A C3A C4A -167.2(9) . . . . ? C2A C3A C4A C5A -3.6(14) . . . . ? C2A C3A C4A C7A 178.9(9) . . . . ? C3A C4A C5A C6A 2.3(14) . . . . ? C7A C4A C5A C6A 179.7(9) . . . . ? C4A C5A C6A C30A 175.3(9) . . . . ? C4A C5A C6A C1A -3.5(14) . . . . ? O1A C1A C6A C5A -176.1(8) . . . . ? C2A C1A C6A C5A 5.5(12) . . . . ? O1A C1A C6A C30A 5.1(13) . . . . ? C2A C1A C6A C30A -173.3(8) . . . . ? C9A N1A C8A C2A -167.3(9) . . . . ? Pb1A N1A C8A C2A 5.6(17) . . . . ? C3A C2A C8A N1A -179.2(11) . . . . ? C1A C2A C8A N1A 7.9(17) . . . . ? C8A N1A C9A C14A -71.1(12) . . . . ? Pb1A N1A C9A C14A 114.8(7) . . . . ? C8A N1A C9A C10A 164.9(9) . . . . ? Pb1A N1A C9A C10A -9.2(9) . . . . ? C15A N2A C10A C11A 12.3(15) . . . . ? Pb1A N2A C10A C11A -166.7(7) . . . . ? C15A N2A C10A C9A -112.8(11) . . . . ? Pb1A N2A C10A C9A 68.1(7) . . . . ? N1A C9A C10A N2A -38.4(10) . . . . ? C14A C9A C10A N2A -166.2(8) . . . . ? N1A C9A C10A C11A -169.8(8) . . . . ? C14A C9A C10A C11A 62.4(10) . . . . ? N2A C10A C11A C12A 175.2(8) . . . . ? C9A C10A C11A C12A -60.2(10) . . . . ? C10A C11A C12A C13A 57.4(11) . . . . ? C11A C12A C13A C14A -52.8(12) . . . . ? N1A C9A C14A C13A 177.8(8) . . . . ? C10A C9A C14A C13A -58.2(10) . . . . ? C12A C13A C14A C9A 53.8(12) . . . . ? C10A N2A C15A C16A 175.9(9) . . . . ? Pb1A N2A C15A C16A -5.4(19) . . . . ? N2A C15A C16A C21A -177.8(11) . . . . ? N2A C15A C16A C17A -2.9(18) . . . . ? Pb1A O2A C17A C16A -5.8(17) . . . . ? Pb1A O2A C17A C18A 171.8(7) . . . . ? C21A C16A C17A O2A -177.1(10) . . . . ? C15A C16A C17A O2A 8.4(17) . . . . ? C21A C16A C17A C18A 5.3(15) . . . . ? C15A C16A C17A C18A -169.3(10) . . . . ? O2A C17A C18A C23A -9.5(14) . . . . ? C16A C17A C18A C23A 168.4(9) . . . . ? O2A C17A C18A C19A 176.8(9) . . . . ? C16A C17A C18A C19A -5.4(14) . . . . ? C23A C18A C19A C20A -170.5(10) . . . . ? C17A C18A C19A C20A 3.4(15) . . . . ? C18A C19A C20A C21A -0.8(16) . . . . ? C18A C19A C20A C22A 179.3(10) . . . . ? C17A C16A C21A C20A -2.9(17) . . . . ? C15A C16A C21A C20A 172.0(10) . . . . ? C19A C20A C21A C16A 0.5(16) . . . . ? C22A C20A C21A C16A -179.5(10) . . . . ? C24A N3A C23A C18A -169.5(8) . . . . ? C19A C18A C23A N3A -175.0(9) . . . . ? C17A C18A C23A N3A 11.2(14) . . . . ? C23A N3A C24A C25A 159.7(8) . . . . ? C23A N3A C24A C29A -81.4(10) . . . . ? C30A N4A C25A C26A 22.6(11) . . . . ? C30A N4A C25A C24A -102.4(9) . . . . ? N3A C24A C25A N4A -45.9(9) . . . . ? C29A C24A C25A N4A -166.2(7) . . . . ? N3A C24A C25A C26A -173.7(7) . . . . ? C29A C24A C25A C26A 66.1(9) . . . . ? N4A C25A C26A C27A 171.4(7) . . . . ? C24A C25A C26A C27A -63.1(9) . . . . ? C25A C26A C27A C28A 58.3(10) . . . . ? C26A C27A C28A C29A -57.9(11) . . . . ? C27A C28A C29A C24A 60.3(10) . . . . ? N3A C24A C29A C28A 175.4(7) . . . . ? C25A C24A C29A C28A -62.8(10) . . . . ? C25A N4A C30A C6A 177.6(7) . . . . ? C5A C6A C30A N4A 176.7(8) . . . . ? C1A C6A C30A N4A -4.5(12) . . . . ? O2B Pb1B O1B C1B -146.2(8) . . . . ? N1B Pb1B O1B C1B -20.5(8) . . . . ? N2B Pb1B O1B C1B -78.3(8) . . . . ? O1B Pb1B O2B C17B 98.6(12) . . . . ? N1B Pb1B O2B C17B 36.2(12) . . . . ? N2B Pb1B O2B C17B -11.8(11) . . . . ? O1B Pb1B N1B C8B 17.0(10) . . . . ? O2B Pb1B N1B C8B 81.0(11) . . . . ? N2B Pb1B N1B C8B 132.6(11) . . . . ? O1B Pb1B N1B C9B -166.2(6) . . . . ? O2B Pb1B N1B C9B -102.2(6) . . . . ? N2B Pb1B N1B C9B -50.6(5) . . . . ? O1B Pb1B N2B C15B -68.3(11) . . . . ? O2B Pb1B N2B C15B 2.2(10) . . . . ? N1B Pb1B N2B C15B -131.7(11) . . . . ? O1B Pb1B N2B C10B 95.2(6) . . . . ? O2B Pb1B N2B C10B 165.7(7) . . . . ? N1B Pb1B N2B C10B 31.8(6) . . . . ? Pb1B O1B C1B C2B 16.0(13) . . . . ? Pb1B O1B C1B C6B -166.9(6) . . . . ? O1B C1B C2B C3B 177.5(8) . . . . ? C6B C1B C2B C3B 0.4(13) . . . . ? O1B C1B C2B C8B 4.2(15) . . . . ? C6B C1B C2B C8B -172.9(9) . . . . ? C1B C2B C3B C4B 4.9(15) . . . . ? C8B C2B C3B C4B 178.4(9) . . . . ? C2B C3B C4B C5B -7.7(14) . . . . ? C2B C3B C4B C7B 179.9(9) . . . . ? C3B C4B C5B C6B 5.0(13) . . . . ? C7B C4B C5B C6B 177.6(9) . . . . ? C4B C5B C6B C30B -174.7(8) . . . . ? C4B C5B C6B C1B -0.1(13) . . . . ? O1B C1B C6B C5B -179.9(8) . . . . ? C2B C1B C6B C5B -2.6(13) . . . . ? O1B C1B C6B C30B -5.4(12) . . . . ? C2B C1B C6B C30B 171.9(8) . . . . ? C9B N1B C8B C2B 175.1(9) . . . . ? Pb1B N1B C8B C2B -8.7(17) . . . . ? C3B C2B C8B N1B 179.8(11) . . . . ? C1B C2B C8B N1B -7.1(16) . . . . ? C8B N1B C9B C10B -112.9(11) . . . . ? Pb1B N1B C9B C10B 69.9(7) . . . . ? C8B N1B C9B C14B 13.6(14) . . . . ? Pb1B N1B C9B C14B -163.7(7) . . . . ? N1B C9B C10B N2B -41.7(10) . . . . ? C14B C9B C10B N2B -170.9(8) . . . . ? N1B C9B C10B C11B -167.3(8) . . . . ? C14B C9B C10B C11B 63.5(11) . . . . ? C15B N2B C10B C9B 159.8(9) . . . . ? Pb1B N2B C10B C9B -6.4(9) . . . . ? C15B N2B C10B C11B -76.4(12) . . . . ? Pb1B N2B C10B C11B 117.3(7) . . . . ? C9B C10B C11B C12B -59.9(11) . . . . ? N2B C10B C11B C12B 176.8(8) . . . . ? C10B C11B C12B C13B 53.8(12) . . . . ? C11B C12B C13B C14B -53.2(12) . . . . ? C12B C13B C14B C9B 53.6(11) . . . . ? N1B C9B C14B C13B 176.3(8) . . . . ? C10B C9B C14B C13B -58.1(11) . . . . ? C10B N2B C15B C16B -165.3(10) . . . . ? Pb1B N2B C15B C16B -2.1(19) . . . . ? N2B C15B C16B C21B 177.4(11) . . . . ? N2B C15B C16B C17B 7(2) . . . . ? Pb1B O2B C17B C18B -162.1(8) . . . . ? Pb1B O2B C17B C16B 19.8(18) . . . . ? C15B C16B C17B O2B -14.9(18) . . . . ? C21B C16B C17B O2B 174.7(10) . . . . ? C15B C16B C17B C18B 166.9(11) . . . . ? C21B C16B C17B C18B -3.4(15) . . . . ? O2B C17B C18B C19B -174.5(10) . . . . ? C16B C17B C18B C19B 3.7(15) . . . . ? O2B C17B C18B C23B 12.1(15) . . . . ? C16B C17B C18B C23B -169.7(9) . . . . ? C23B C18B C19B C20B 174.6(9) . . . . ? C17B C18B C19B C20B 1.1(15) . . . . ? C18B C19B C20B C21B -6.3(16) . . . . ? C18B C19B C20B C22B -179.4(10) . . . . ? C19B C20B C21B C16B 6.8(18) . . . . ? C22B C20B C21B C16B 179.7(11) . . . . ? C15B C16B C21B C20B -172.8(11) . . . . ? C17B C16B C21B C20B -1.9(17) . . . . ? C24B N3B C23B C18B 171.5(8) . . . . ? C19B C18B C23B N3B 178.6(8) . . . . ? C17B C18B C23B N3B -7.7(13) . . . . ? C23B N3B C24B C25B -85.9(9) . . . . ? C23B N3B C24B C29B 38.2(12) . . . . ? C30B N4B C25B C24B 179.3(7) . . . . ? C30B N4B C25B C26B -59.2(10) . . . . ? N3B C24B C25B N4B -51.0(9) . . . . ? C29B C24B C25B N4B -177.6(7) . . . . ? N3B C24B C25B C26B -173.6(7) . . . . ? C29B C24B C25B C26B 59.8(10) . . . . ? N4B C25B C26B C27B -178.7(8) . . . . ? C24B C25B C26B C27B -57.2(10) . . . . ? C25B C26B C27B C28B 55.2(11) . . . . ? C26B C27B C28B C29B -56.5(11) . . . . ? N3B C24B C29B C28B 174.8(8) . . . . ? C25B C24B C29B C28B -60.9(11) . . . . ? C27B C28B C29B C24B 58.7(12) . . . . ? C25B N4B C30B C6B -170.2(7) . . . . ? C5B C6B C30B N4B -179.0(8) . . . . ? C1B C6B C30B N4B 6.2(12) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.543 _refine_diff_density_min -1.264 _refine_diff_density_rms 0.130