# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'S.LE GAC' ; Sciences Chimiques de Rennes UMR 6226 CNRS, Universit\'e de Rennes 1 Campus de Beaulieu, b\^at. 10C 263 Av G\'en\'eral Leclerc,CS 74205 35042 Rennes Cedex, France ; B.NAJJARI ; Sciences Chimiques de Rennes UMR 6226 CNRS, Universit\'e de Rennes 1 Campus de Beaulieu, b\^at. 10C 263 Av G\'en\'eral Leclerc,CS 74205 35042 Rennes Cedex, France ; L.FUSARO ; Laboratoire de RMN Haute R\'esolution Universit\'e Libre de Bruxelles CP160/08 50 Avenue F.-F. Roosevelt 1050 Bruxelles, Belgium ; T.ROISNEL ; Centre de Diffractom\'etrie X Sciences Chimiques de Rennes UMR 6226 CNRS Universit\'e de Rennes 1 263 Av G\'en\'eral Leclerc,CS 74205 35042 Rennes Cedex, France ; V.DORCET ; Centre de Diffractom\'etrie X Sciences Chimiques de Rennes UMR 6226 CNRS Universit\'e de Rennes 1 263 Av G\'en\'eral Leclerc, CS 74205 35042 Rennes Cedex, France ; M.LUHMER ; Laboratoire de RMN Haute R\'esolution Universit\'e Libre de Bruxelles CP160/08 50 Avenue F.-F. Roosevelt 1050 Bruxelles, Belgium ; ; E.FURET ; ; \'Ecole Nationale Sup\'erieure de Chimie de Rennes Sciences Chimiques de Rennes UMR 6226 CNRS Universit\'e de Rennes 1 Avenue du G\'en\'eral Leclerc CS 50837 35708 Rennes cedex 7, France ; J.-F.HALET ; Sciences Chimiques de Rennes UMR 6226 CNRS, Universit\'e de Rennes 1 Campus de Beaulieu, b\^at. 10C 263 Av G\'en\'eral Leclerc, CS 74205 35042 Rennes Cedex, France ; B.BOITREL ; Sciences Chimiques de Rennes UMR 6226 CNRS, Universit\'e de Rennes 1 Campus de Beaulieu, b\^at. 10C 263 Av G\'en\'eral Leclerc, CS 74205 35042 Rennes Cedex, France ; #----------------------------------------------------------------------------# # AUTHORS INFORMATION # #----------------------------------------------------------------------------# # Person making the deposition _publ_contact_author 'DORCET, Vincent' _publ_contact_author_address ; Centre de Diffractom\'etrie X Sciences Chimiques de Rennes UMR 6226 CNRS Universit\'e de Rennes 1 Avenue du General Leclerc 35042 Rennes, France ; _publ_contact_author_email vincent.dorcet@univ-rennes1.fr _publ_requested_category FM #----------------------------------------------------------------------------# # Compound #1 # #----------------------------------------------------------------------------# data_BN184 _database_code_depnum_ccdc_archive 'CCDC 845672' #TrackingRef 'BN184_CCDC845672_dec2011.cif' _audit_creation_date 2011-03-25T18:17:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C70 H58 N6 O11 Pb2 S' _chemical_formula_sum 'C70 H58 N6 O11 Pb2 S' _chemical_formula_weight 1605.66 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 13.0119(8) _cell_length_b 12.7579(7) _cell_length_c 41.322(2) _cell_angle_alpha 90 _cell_angle_beta 90.465(3) _cell_angle_gamma 90 _cell_volume 6859.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9874 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.46 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.495 _exptl_absorpt_correction_T_max 0.741 #----------------------------------------------------------------------------# # SQUEEZE RESULTS # #----------------------------------------------------------------------------# # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.290 0.000 0.500 508 156 ' ' 2 0.077 0.130 0.810 17 4 ' ' 3 0.926 0.500 0.000 508 157 ' ' 4 0.077 0.370 0.310 17 4 ' ' 5 0.923 0.630 0.690 17 4 ' ' 6 0.923 0.870 0.190 17 4 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_unetI/netI 0.0615 _diffrn_reflns_number 56791 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 15654 _reflns_number_gt 12855 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0000P)^2^+286.6864P] 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_number_reflns 15654 _refine_ls_number_parameters 691 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1069 _refine_ls_R_factor_gt 0.0912 _refine_ls_wR_factor_ref 0.1949 _refine_ls_wR_factor_gt 0.1894 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.01 _refine_ls_shift/su_mean 0 _refine_diff_density_max 7.299 _refine_diff_density_min -9.697 _refine_diff_density_rms 0.26 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.35554(3) 0.09920(3) 0.200975(10) 0.01755(11) Uani 1 1 d . . . Pb2 Pb 0.43694(4) 0.27663(4) 0.134265(12) 0.03122(14) Uani 1 1 d . . . N1 N 0.5372(7) 0.1119(7) 0.1915(2) 0.019(2) Uani 1 1 d . . . N2 N 0.3980(7) 0.2804(7) 0.2111(2) 0.0186(19) Uani 1 1 d . . . N3 N 0.2429(7) 0.1983(7) 0.1664(2) 0.0166(19) Uani 1 1 d . . . N4 N 0.3784(7) 0.0285(8) 0.1482(2) 0.020(2) Uani 1 1 d . . . C1 C 0.6053(8) 0.1665(9) 0.2095(3) 0.0193(5) Uani 1 1 d . . . C2 C 0.5821(8) 0.2585(9) 0.2280(3) 0.0193(5) Uani 1 1 d . . . C3 C 0.4863(8) 0.3112(9) 0.2279(3) 0.0193(5) Uani 1 1 d . . . C4 C 0.4704(8) 0.4151(9) 0.2413(3) 0.0193(5) Uani 1 1 d . . . H4 H 0.5178 0.4546 0.254 0.023 Uiso 1 1 calc R . . C5 C 0.3749(8) 0.4444(9) 0.2322(3) 0.0193(5) Uani 1 1 d . . . H5 H 0.3441 0.5098 0.2373 0.023 Uiso 1 1 calc R . . C6 C 0.3257(8) 0.3619(9) 0.2134(3) 0.0193(5) Uani 1 1 d . . . C7 C 0.2359(8) 0.3668(9) 0.1967(3) 0.0193(5) Uani 1 1 d . . . C8 C 0.1967(8) 0.2933(9) 0.1745(3) 0.0193(5) Uani 1 1 d . . . C9 C 0.1039(8) 0.3057(9) 0.1557(3) 0.0193(5) Uani 1 1 d . . . H9 H 0.0579 0.3635 0.1564 0.023 Uiso 1 1 calc R . . C10 C 0.0944(8) 0.2180(9) 0.1367(3) 0.0193(5) Uani 1 1 d . . . H10 H 0.0398 0.2027 0.122 0.023 Uiso 1 1 calc R . . C11 C 0.1829(8) 0.1539(9) 0.1432(3) 0.0193(5) Uani 1 1 d . . . C12 C 0.2019(8) 0.0586(9) 0.1269(3) 0.0193(5) Uani 1 1 d . . . C13 C 0.2953(8) 0.0017(9) 0.1287(3) 0.0193(5) Uani 1 1 d . . . C14 C 0.3190(8) -0.0904(9) 0.1102(3) 0.0193(5) Uani 1 1 d . . . H14 H 0.2755 -0.1232 0.0946 0.023 Uiso 1 1 calc R . . C15 C 0.4159(8) -0.1226(9) 0.1190(3) 0.0193(5) Uani 1 1 d . . . H15 H 0.4501 -0.1838 0.1117 0.023 Uiso 1 1 calc R . . C16 C 0.4567(8) -0.0457(9) 0.1418(3) 0.0193(5) Uani 1 1 d . . . C17 C 0.5526(8) -0.0468(9) 0.1565(3) 0.0193(5) Uani 1 1 d . . . C18 C 0.5927(8) 0.0287(9) 0.1770(3) 0.0193(5) Uani 1 1 d . . . C19 C 0.6988(8) 0.0392(9) 0.1872(3) 0.0193(5) Uani 1 1 d . . . H19 H 0.754 -0.0049 0.181 0.023 Uiso 1 1 calc R . . C20 C 0.7056(8) 0.1224(9) 0.2073(3) 0.0193(5) Uani 1 1 d . . . H20 H 0.7659 0.147 0.2179 0.023 Uiso 1 1 calc R . . C21 C 0.6655(9) 0.3061(9) 0.2486(3) 0.021(2) Uani 1 1 d . . . C22 C 0.6574(9) 0.2960(10) 0.2818(3) 0.024(3) Uani 1 1 d . . . H22 H 0.5985 0.2633 0.2908 0.029 Uiso 1 1 calc R . . C23 C 0.7356(10) 0.3339(10) 0.3027(3) 0.028(3) Uani 1 1 d . . . H23 H 0.7313 0.3241 0.3254 0.034 Uiso 1 1 calc R . . C24 C 0.8175(10) 0.3847(10) 0.2895(3) 0.029(3) Uani 1 1 d . . . H24 H 0.8694 0.4126 0.3033 0.035 Uiso 1 1 calc R . . C25 C 0.8263(9) 0.3963(10) 0.2567(3) 0.029(3) Uani 1 1 d . . . H25 H 0.8853 0.4298 0.2481 0.035 Uiso 1 1 calc R . . C26 C 0.7480(10) 0.3588(9) 0.2353(3) 0.025(3) Uani 1 1 d . . . N27 N 0.7548(7) 0.3685(7) 0.2013(3) 0.023(2) Uani 1 1 d . . . H27 H 0.6983 0.3556 0.1901 0.028 Uiso 1 1 calc R . . C28 C 0.8394(10) 0.3956(10) 0.1839(3) 0.030(3) Uani 1 1 d . . . O29 O 0.9189(7) 0.4293(8) 0.1964(3) 0.040(3) Uani 1 1 d . . . C30 C 0.8360(9) 0.3788(9) 0.1479(3) 0.026(3) Uani 1 1 d . . . C31 C 0.8921(9) 0.4522(11) 0.1292(4) 0.031(3) Uani 1 1 d . . . H31 H 0.9214 0.5125 0.1391 0.037 Uiso 1 1 calc R . . C32 C 0.9038(10) 0.4354(11) 0.0964(4) 0.033(3) Uani 1 1 d . . . H32 H 0.9401 0.4849 0.0837 0.04 Uiso 1 1 calc R . . C33 C 0.8629(11) 0.3466(12) 0.0821(4) 0.037(3) Uani 1 1 d . . . H33 H 0.8724 0.3358 0.0595 0.044 Uiso 1 1 calc R . . C34 C 0.8081(9) 0.2726(11) 0.0998(3) 0.028(3) Uani 1 1 d . . . C35 C 0.7946(8) 0.2922(9) 0.1333(3) 0.021(2) Uani 1 1 d . . . H35 H 0.7559 0.2441 0.1458 0.026 Uiso 1 1 calc R . . C36 C 0.7658(11) 0.1769(11) 0.0836(3) 0.032(3) Uani 1 1 d . . . H36A H 0.753 0.1227 0.1002 0.038 Uiso 1 1 calc R . . H36B H 0.8179 0.149 0.0685 0.038 Uiso 1 1 calc R . . C41 C 0.1201(9) 0.0211(9) 0.1048(3) 0.026(3) Uani 1 1 d . . . C42 C 0.0287(11) -0.0187(11) 0.1189(4) 0.036(3) Uani 1 1 d . . . H42 H 0.0248 -0.0253 0.1417 0.044 Uiso 1 1 calc R . . C43 C -0.0541(11) -0.0478(12) 0.1000(4) 0.042(4) Uani 1 1 d . . . H43 H -0.1146 -0.0739 0.1099 0.051 Uiso 1 1 calc R . . C44 C -0.0493(10) -0.0390(13) 0.0668(4) 0.042(4) Uani 1 1 d . . . H44 H -0.1067 -0.0586 0.0538 0.05 Uiso 1 1 calc R . . C45 C 0.0391(12) -0.0015(12) 0.0524(4) 0.042(4) Uani 1 1 d . . . H45 H 0.0415 0.0049 0.0295 0.05 Uiso 1 1 calc R . . C46 C 0.1252(10) 0.0272(11) 0.0711(3) 0.030(3) Uani 1 1 d . . . N47 N 0.2153(9) 0.0683(10) 0.0566(3) 0.034(3) Uani 1 1 d . . . H47 H 0.2564 0.1045 0.0694 0.041 Uiso 1 1 calc R . . C48 C 0.2449(12) 0.0586(13) 0.0257(4) 0.042(4) Uani 1 1 d . . . O49 O 0.1937(10) 0.0119(14) 0.0051(3) 0.081(5) Uani 1 1 d . . . C50 C 0.3503(12) 0.0996(13) 0.0178(3) 0.039(3) Uani 1 1 d . . . C51 C 0.3576(15) 0.1484(13) -0.0124(4) 0.051(5) Uani 1 1 d . . . H51 H 0.2986 0.156 -0.026 0.062 Uiso 1 1 calc R . . C52 C 0.4542(15) 0.1861(14) -0.0224(4) 0.053(5) Uani 1 1 d . . . H52 H 0.4603 0.2231 -0.0423 0.063 Uiso 1 1 calc R . . C53 C 0.5392(14) 0.1689(15) -0.0033(4) 0.050(4) Uani 1 1 d . . . H53 H 0.6041 0.1931 -0.0106 0.061 Uiso 1 1 calc R . . C54 C 0.5340(13) 0.1179(11) 0.0261(4) 0.038(3) Uani 1 1 d . . . C55 C 0.4350(12) 0.0869(11) 0.0367(3) 0.036(3) Uani 1 1 d . . . H55 H 0.428 0.0565 0.0576 0.043 Uiso 1 1 calc R . . C56 C 0.6301(12) 0.0988(12) 0.0460(4) 0.041(3) Uani 1 1 d . . . H56A H 0.6858 0.0758 0.0314 0.049 Uiso 1 1 calc R . . H56B H 0.617 0.0415 0.0615 0.049 Uiso 1 1 calc R . . C61 C 0.6657(10) 0.1971(11) 0.0647(3) 0.030(3) Uani 1 1 d . . . H61 H 0.6768 0.2558 0.049 0.036 Uiso 1 1 calc R . . C62 C 0.5827(10) 0.2281(12) 0.0883(3) 0.033(3) Uani 1 1 d . . . O63 O 0.5557(8) 0.1617(9) 0.1089(2) 0.043(3) Uani 1 1 d . . . O64 O 0.5447(8) 0.3186(8) 0.0877(2) 0.038(2) Uani 1 1 d . . . C71 C 0.2876(14) 0.3407(15) 0.0859(4) 0.050(4) Uani 1 1 d . . . O72 O 0.3260(10) 0.4122(9) 0.1032(3) 0.057(3) Uani 1 1 d . . . O73 O 0.3165(8) 0.2467(7) 0.0899(2) 0.039(2) Uani 1 1 d . . . S8 S 0.5704(4) 0.5307(4) 0.15524(13) 0.0596(13) Uani 1 1 d . . . C81 C 0.5899(16) 0.5458(16) 0.1131(5) 0.070(6) Uani 1 1 d . . . H81A H 0.658 0.5188 0.1074 0.105 Uiso 1 1 calc R . . H81B H 0.5856 0.6203 0.1074 0.105 Uiso 1 1 calc R . . H81C H 0.537 0.5067 0.1011 0.105 Uiso 1 1 calc R . . O82 O 0.5605(8) 0.4134(9) 0.1601(3) 0.046(3) Uani 1 1 d . . . C83 C 0.4430(18) 0.5858(16) 0.1571(5) 0.076(6) Uani 1 1 d . . . H83A H 0.4188 0.584 0.1795 0.114 Uiso 1 1 calc R . . H83B H 0.3963 0.5448 0.1433 0.114 Uiso 1 1 calc R . . H83C H 0.4446 0.6585 0.1495 0.114 Uiso 1 1 calc R . . C101 C 0.1727(9) 0.4622(10) 0.2026(3) 0.026(3) Uani 1 1 d . . . C102 C 0.1324(9) 0.4801(10) 0.2336(3) 0.028(3) Uani 1 1 d . . . H102 H 0.1451 0.4314 0.2505 0.034 Uiso 1 1 calc R . . C103 C 0.0746(9) 0.5680(12) 0.2393(4) 0.036(3) Uani 1 1 d . . . C104 C 0.0546(10) 0.6407(10) 0.2151(4) 0.038(4) Uani 1 1 d . . . H104 H 0.0144 0.7013 0.2193 0.046 Uiso 1 1 calc R . . C105 C 0.0949(11) 0.6226(10) 0.1844(4) 0.036(3) Uani 1 1 d . . . C106 C 0.1544(9) 0.5353(11) 0.1778(3) 0.030(3) Uani 1 1 d . . . H106 H 0.1824 0.5251 0.1569 0.036 Uiso 1 1 calc R . . O107 O 0.0371(8) 0.5770(9) 0.2704(3) 0.051(3) Uani 1 1 d . . . C108 C -0.0199(14) 0.6692(17) 0.2777(6) 0.079(7) Uani 1 1 d . . . H10A H -0.0421 0.6666 0.3003 0.119 Uiso 1 1 calc R . . H10B H -0.0803 0.6734 0.2635 0.119 Uiso 1 1 calc R . . H10C H 0.0235 0.731 0.2745 0.119 Uiso 1 1 calc R . . O109 O 0.0700(9) 0.6980(8) 0.1614(3) 0.051(3) Uani 1 1 d . . . C110 C 0.1112(15) 0.6870(12) 0.1296(5) 0.058(5) Uani 1 1 d . . . H11A H 0.0872 0.7451 0.116 0.087 Uiso 1 1 calc R . . H11B H 0.0882 0.6204 0.1202 0.087 Uiso 1 1 calc R . . H11C H 0.1865 0.688 0.1308 0.087 Uiso 1 1 calc R . . C111 C 0.6263(9) -0.1321(8) 0.1469(3) 0.019(2) Uani 1 1 d . . . C112 C 0.6606(9) -0.1411(10) 0.1157(3) 0.023(3) Uani 1 1 d . . . H112 H 0.6338 -0.0965 0.0993 0.028 Uiso 1 1 calc R . . C113 C 0.7366(10) -0.2173(9) 0.1080(3) 0.026(3) Uani 1 1 d . . . C114 C 0.7752(10) -0.2813(11) 0.1322(3) 0.031(3) Uani 1 1 d . . . H114 H 0.826 -0.3321 0.1272 0.037 Uiso 1 1 calc R . . C115 C 0.7403(10) -0.2718(11) 0.1633(3) 0.032(3) Uani 1 1 d . . . C116 C 0.6654(9) -0.1988(9) 0.1711(3) 0.025(3) Uani 1 1 d . . . H116 H 0.6408 -0.194 0.1927 0.029 Uiso 1 1 calc R . . O117 O 0.7638(8) -0.2213(8) 0.0766(2) 0.040(3) Uani 1 1 d . . . C118 C 0.8370(14) -0.2981(13) 0.0673(4) 0.052(3) Uani 1 1 d . . . H11D H 0.8498 -0.2923 0.044 0.078 Uiso 1 1 calc R . . H11E H 0.8104 -0.3682 0.0721 0.078 Uiso 1 1 calc R . . H11F H 0.9014 -0.2868 0.0793 0.078 Uiso 1 1 calc R . . O119 O 0.7828(8) -0.3403(8) 0.1853(2) 0.041(3) Uani 1 1 d . . . C120 C 0.7421(14) -0.3411(13) 0.2175(4) 0.052(3) Uani 1 1 d . . . H12A H 0.779 -0.3932 0.2306 0.078 Uiso 1 1 calc R . . H12B H 0.6689 -0.359 0.2167 0.078 Uiso 1 1 calc R . . H12C H 0.7507 -0.2716 0.2273 0.078 Uiso 1 1 calc R . . C74 C 0.2095(18) 0.3579(18) 0.0608(5) 0.079(7) Uani 1 1 d . . . H74A H 0.193 0.4327 0.0596 0.119 Uiso 1 1 calc R . . H74B H 0.1474 0.3183 0.0661 0.119 Uiso 1 1 calc R . . H74C H 0.2358 0.3342 0.0399 0.119 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.01566(19) 0.01537(19) 0.0216(2) 0.00044(17) -0.00293(14) -0.00078(17) Pb2 0.0283(3) 0.0374(3) 0.0280(3) -0.0029(2) 0.00258(19) -0.0072(2) N1 0.018(5) 0.011(5) 0.028(5) -0.004(4) -0.003(4) 0.004(4) N2 0.017(5) 0.015(5) 0.024(5) -0.003(4) -0.002(4) -0.006(4) N3 0.013(4) 0.020(5) 0.017(4) 0.000(4) 0.001(3) 0.003(4) N4 0.019(5) 0.017(5) 0.024(5) 0.000(4) -0.010(4) 0.003(4) C1 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C2 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C3 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C4 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C5 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C6 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C7 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C8 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C9 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C10 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C11 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C12 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C13 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C14 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C15 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C16 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C17 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C18 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C19 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C20 0.0145(12) 0.0154(12) 0.0280(14) -0.0020(11) -0.0020(10) 0.0017(10) C21 0.021(6) 0.014(5) 0.029(6) -0.002(5) -0.003(5) 0.004(4) C22 0.021(6) 0.027(7) 0.024(6) 0.002(5) -0.003(5) -0.002(5) C23 0.024(6) 0.023(6) 0.038(7) -0.009(6) -0.010(5) 0.015(5) C24 0.030(7) 0.018(6) 0.039(7) -0.012(5) -0.020(6) 0.003(5) C25 0.021(6) 0.018(6) 0.047(8) -0.011(6) -0.013(5) 0.005(5) C26 0.029(7) 0.011(5) 0.033(7) -0.004(5) -0.004(5) -0.005(5) N27 0.014(5) 0.014(5) 0.042(6) 0.004(4) -0.010(4) -0.005(4) C28 0.024(6) 0.022(6) 0.045(8) -0.003(6) -0.006(5) -0.009(5) O29 0.019(5) 0.047(6) 0.054(6) -0.011(5) -0.005(4) -0.007(4) C30 0.014(5) 0.017(6) 0.046(8) 0.002(5) -0.008(5) 0.002(4) C31 0.018(6) 0.025(7) 0.049(8) 0.005(6) -0.007(6) -0.010(5) C32 0.024(7) 0.026(7) 0.051(9) 0.009(6) 0.001(6) -0.005(5) C33 0.031(7) 0.046(9) 0.034(7) 0.005(7) 0.004(6) 0.007(7) C34 0.017(6) 0.028(7) 0.039(7) 0.000(6) 0.000(5) 0.007(5) C35 0.014(5) 0.015(6) 0.035(7) 0.002(5) 0.000(5) 0.003(4) C36 0.032(7) 0.029(7) 0.034(7) 0.002(6) 0.000(6) 0.005(6) C41 0.019(6) 0.015(6) 0.044(8) -0.007(5) -0.014(5) -0.002(5) C42 0.035(8) 0.025(7) 0.049(9) -0.009(6) -0.024(7) -0.007(6) C43 0.025(7) 0.042(9) 0.060(10) -0.015(8) -0.017(7) 0.007(6) C44 0.020(7) 0.050(10) 0.055(10) -0.021(8) -0.011(6) 0.006(6) C45 0.047(9) 0.040(9) 0.038(8) -0.013(7) -0.019(7) -0.001(7) C46 0.028(7) 0.028(7) 0.033(7) -0.015(6) -0.011(5) 0.012(6) N47 0.034(6) 0.041(7) 0.027(6) -0.006(5) -0.014(5) -0.004(5) C48 0.040(8) 0.053(10) 0.033(8) -0.018(7) -0.010(6) 0.007(7) O49 0.047(7) 0.149(15) 0.046(7) -0.052(9) -0.004(6) -0.013(8) C50 0.044(8) 0.047(9) 0.025(7) -0.015(7) -0.005(6) -0.001(7) C51 0.074(12) 0.045(10) 0.036(8) -0.009(7) -0.021(8) 0.018(9) C52 0.079(13) 0.051(11) 0.028(8) 0.004(7) -0.007(8) -0.006(9) C53 0.056(11) 0.060(11) 0.035(8) 0.002(8) -0.005(7) -0.004(9) C54 0.054(9) 0.027(8) 0.035(8) -0.012(6) 0.003(7) -0.002(7) C55 0.055(9) 0.032(8) 0.020(6) -0.006(6) -0.005(6) 0.005(7) C56 0.051(9) 0.035(8) 0.037(8) -0.009(7) -0.005(7) -0.008(7) C61 0.030(7) 0.033(7) 0.027(6) -0.001(6) -0.001(5) -0.006(6) C62 0.028(7) 0.039(8) 0.031(7) -0.003(6) 0.001(5) -0.004(6) O63 0.050(7) 0.043(6) 0.037(6) 0.007(5) 0.008(5) 0.000(5) O64 0.046(6) 0.027(5) 0.041(6) 0.008(4) 0.007(5) 0.009(4) C71 0.051(10) 0.056(11) 0.043(9) 0.005(8) 0.000(8) -0.016(9) O72 0.066(8) 0.037(7) 0.066(8) 0.001(6) -0.008(6) 0.004(6) O73 0.054(7) 0.022(5) 0.041(6) 0.002(4) -0.002(5) 0.001(5) S8 0.073(3) 0.036(2) 0.070(3) 0.007(2) -0.019(3) -0.022(2) C81 0.068(13) 0.051(12) 0.092(16) 0.021(11) -0.001(11) -0.019(10) O82 0.048(6) 0.039(6) 0.052(7) -0.005(5) -0.005(5) -0.012(5) C83 0.104(18) 0.042(11) 0.081(15) -0.003(10) 0.001(13) 0.022(11) C101 0.016(6) 0.021(6) 0.043(8) 0.003(6) -0.004(5) -0.010(5) C102 0.020(6) 0.025(7) 0.040(7) -0.015(6) -0.008(5) 0.012(5) C103 0.009(5) 0.040(8) 0.057(9) -0.024(7) -0.005(6) 0.000(5) C104 0.018(6) 0.015(6) 0.082(12) -0.022(7) -0.007(7) 0.002(5) C105 0.031(7) 0.014(6) 0.062(10) -0.002(6) -0.015(7) 0.001(5) C106 0.017(6) 0.031(7) 0.042(8) -0.002(6) -0.005(5) 0.007(5) O107 0.026(5) 0.057(8) 0.071(8) -0.035(6) 0.008(5) 0.006(5) C108 0.040(10) 0.074(14) 0.124(19) -0.057(14) 0.025(11) 0.002(10) O109 0.047(7) 0.022(5) 0.083(9) 0.008(6) -0.017(6) 0.005(5) C110 0.071(12) 0.015(7) 0.087(14) 0.017(8) -0.026(11) -0.005(7) C111 0.018(5) 0.007(5) 0.032(6) -0.003(4) -0.004(5) 0.003(4) C112 0.023(6) 0.023(6) 0.024(6) 0.002(5) -0.003(5) 0.009(5) C113 0.026(6) 0.014(6) 0.039(7) -0.001(5) -0.002(5) 0.012(5) C114 0.030(7) 0.024(7) 0.040(8) -0.002(6) 0.003(6) 0.005(6) C115 0.029(7) 0.027(7) 0.040(8) 0.004(6) -0.007(6) 0.006(6) C116 0.025(6) 0.017(6) 0.031(7) -0.005(5) -0.004(5) 0.003(5) O117 0.044(6) 0.042(6) 0.035(5) -0.003(5) 0.002(4) 0.025(5) C118 0.067(8) 0.035(6) 0.054(7) 0.011(5) -0.008(6) 0.029(6) O119 0.049(6) 0.033(6) 0.042(6) 0.008(5) -0.006(5) 0.017(5) C120 0.067(8) 0.035(6) 0.054(7) 0.011(5) -0.008(6) 0.029(6) C74 0.093(17) 0.068(14) 0.076(14) 0.025(12) -0.039(13) -0.017(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 N4 2.381(10) . ? Pb1 N3 2.397(9) . ? Pb1 N1 2.404(9) . ? Pb1 N2 2.412(9) . ? Pb2 O63 2.379(11) . ? Pb2 O73 2.431(10) . ? Pb2 O64 2.450(10) . ? Pb2 O72 2.587(12) . ? Pb2 O82 2.597(10) . ? Pb2 C62 2.766(14) . ? N1 C1 1.347(14) . ? N1 C18 1.420(14) . ? N2 C3 1.393(14) . ? N2 C6 1.406(14) . ? N3 C11 1.357(14) . ? N3 C8 1.395(14) . ? N4 C13 1.387(14) . ? N4 C16 1.417(14) . ? C1 C20 1.425(15) . ? C1 C2 1.433(16) . ? C2 C3 1.416(15) . ? C2 C21 1.505(16) . ? C3 C4 1.453(15) . ? C4 C5 1.348(15) . ? C4 H4 0.95 . ? C5 C6 1.454(16) . ? C5 H5 0.95 . ? C6 C7 1.352(15) . ? C7 C8 1.406(16) . ? C7 C101 1.489(17) . ? C8 C9 1.439(15) . ? C9 C10 1.372(16) . ? C9 H9 0.95 . ? C10 C11 1.436(15) . ? C10 H10 0.95 . ? C11 C12 1.411(16) . ? C12 C13 1.418(15) . ? C12 C41 1.477(15) . ? C13 C14 1.436(16) . ? C14 C15 1.373(15) . ? C14 H14 0.95 . ? C15 C16 1.456(16) . ? C15 H15 0.95 . ? C16 C17 1.382(15) . ? C17 C18 1.383(16) . ? C17 C111 1.505(15) . ? C18 C19 1.447(15) . ? C19 C20 1.349(16) . ? C19 H19 0.95 . ? C20 H20 0.95 . ? C21 C22 1.383(17) . ? C21 C26 1.384(17) . ? C22 C23 1.413(17) . ? C22 H22 0.95 . ? C23 C24 1.364(19) . ? C23 H23 0.95 . ? C24 C25 1.369(19) . ? C24 H24 0.95 . ? C25 C26 1.427(16) . ? C25 H25 0.95 . ? C26 N27 1.415(16) . ? N27 C28 1.363(16) . ? N27 H27 0.88 . ? C28 O29 1.231(15) . ? C28 C30 1.502(19) . ? C30 C35 1.369(17) . ? C30 C31 1.421(18) . ? C31 C32 1.38(2) . ? C31 H31 0.95 . ? C32 C33 1.38(2) . ? C32 H32 0.95 . ? C33 C34 1.39(2) . ? C33 H33 0.95 . ? C34 C35 1.420(18) . ? C34 C36 1.495(19) . ? C35 H35 0.95 . ? C36 C61 1.535(18) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? C41 C46 1.396(19) . ? C41 C42 1.42(2) . ? C42 C43 1.375(17) . ? C42 H42 0.95 . ? C43 C44 1.38(2) . ? C43 H43 0.95 . ? C44 C45 1.38(2) . ? C44 H44 0.95 . ? C45 C46 1.404(18) . ? C45 H45 0.95 . ? C46 N47 1.421(18) . ? N47 C48 1.342(18) . ? N47 H47 0.88 . ? C48 O49 1.233(18) . ? C48 C50 1.51(2) . ? C50 C55 1.358(19) . ? C50 C51 1.40(2) . ? C51 C52 1.41(3) . ? C51 H51 0.95 . ? C52 C53 1.37(2) . ? C52 H52 0.95 . ? C53 C54 1.38(2) . ? C53 H53 0.95 . ? C54 C55 1.42(2) . ? C54 C56 1.51(2) . ? C55 H55 0.95 . ? C56 C61 1.543(19) . ? C56 H56A 0.99 . ? C56 H56B 0.99 . ? C61 C62 1.514(18) . ? C61 H61 1 . ? C62 O63 1.255(17) . ? C62 O64 1.256(17) . ? C71 O72 1.26(2) . ? C71 O73 1.27(2) . ? C71 C74 1.46(2) . ? S8 O82 1.516(12) . ? S8 C81 1.77(2) . ? S8 C83 1.80(2) . ? C81 H81A 0.98 . ? C81 H81B 0.98 . ? C81 H81C 0.98 . ? C83 H83A 0.98 . ? C83 H83B 0.98 . ? C83 H83C 0.98 . ? C101 C106 1.404(18) . ? C101 C102 1.405(19) . ? C102 C103 1.372(17) . ? C102 H102 0.95 . ? C103 O107 1.382(18) . ? C103 C104 1.39(2) . ? C104 C105 1.39(2) . ? C104 H104 0.95 . ? C105 C106 1.384(18) . ? C105 O109 1.389(17) . ? C106 H106 0.95 . ? O107 C108 1.42(2) . ? C108 H10A 0.98 . ? C108 H10B 0.98 . ? C108 H10C 0.98 . ? O109 C110 1.43(2) . ? C110 H11A 0.98 . ? C110 H11B 0.98 . ? C110 H11C 0.98 . ? C111 C112 1.374(17) . ? C111 C116 1.406(16) . ? C112 C113 1.425(16) . ? C112 H112 0.95 . ? C113 O117 1.349(16) . ? C113 C114 1.380(18) . ? C114 C115 1.372(19) . ? C114 H114 0.95 . ? C115 O119 1.376(16) . ? C115 C116 1.388(17) . ? C116 H116 0.95 . ? O117 C118 1.423(17) . ? C118 H11D 0.98 . ? C118 H11E 0.98 . ? C118 H11F 0.98 . ? O119 C120 1.436(19) . ? C120 H12A 0.98 . ? C120 H12B 0.98 . ? C120 H12C 0.98 . ? C74 H74A 0.98 . ? C74 H74B 0.98 . ? C74 H74C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Pb1 N3 74.6(3) . . ? N4 Pb1 N1 75.3(3) . . ? N3 Pb1 N1 117.7(3) . . ? N4 Pb1 N2 119.4(3) . . ? N3 Pb1 N2 74.7(3) . . ? N1 Pb1 N2 74.9(3) . . ? O63 Pb2 O73 89.3(4) . . ? O63 Pb2 O64 53.9(3) . . ? O73 Pb2 O64 79.2(4) . . ? O63 Pb2 O72 123.7(4) . . ? O73 Pb2 O72 51.5(4) . . ? O64 Pb2 O72 77.6(4) . . ? O63 Pb2 O82 101.1(4) . . ? O73 Pb2 O82 144.0(3) . . ? O64 Pb2 O82 79.6(4) . . ? O72 Pb2 O82 95.5(4) . . ? O63 Pb2 C62 26.9(4) . . ? O73 Pb2 C62 83.6(4) . . ? O64 Pb2 C62 27.0(4) . . ? O72 Pb2 C62 101.0(4) . . ? O82 Pb2 C62 90.4(4) . . ? C1 N1 C18 106.6(9) . . ? C1 N1 Pb1 126.0(7) . . ? C18 N1 Pb1 121.5(7) . . ? C3 N2 C6 107.9(9) . . ? C3 N2 Pb1 122.9(7) . . ? C6 N2 Pb1 124.6(7) . . ? C11 N3 C8 106.5(9) . . ? C11 N3 Pb1 123.2(7) . . ? C8 N3 Pb1 125.4(7) . . ? C13 N4 C16 106.6(9) . . ? C13 N4 Pb1 121.6(8) . . ? C16 N4 Pb1 121.3(7) . . ? N1 C1 C20 111.0(10) . . ? N1 C1 C2 125.3(10) . . ? C20 C1 C2 123.7(10) . . ? C3 C2 C1 125.2(10) . . ? C3 C2 C21 116.2(10) . . ? C1 C2 C21 118.6(10) . . ? N2 C3 C2 126.1(10) . . ? N2 C3 C4 109.2(9) . . ? C2 C3 C4 124.0(10) . . ? C5 C4 C3 106.2(10) . . ? C5 C4 H4 126.9 . . ? C3 C4 H4 126.9 . . ? C4 C5 C6 110.5(10) . . ? C4 C5 H5 124.8 . . ? C6 C5 H5 124.8 . . ? C7 C6 N2 125.2(11) . . ? C7 C6 C5 127.8(11) . . ? N2 C6 C5 106.2(9) . . ? C6 C7 C8 127.5(11) . . ? C6 C7 C101 115.5(10) . . ? C8 C7 C101 117.0(10) . . ? N3 C8 C7 125.5(10) . . ? N3 C8 C9 109.2(10) . . ? C7 C8 C9 125.3(10) . . ? C10 C9 C8 106.9(10) . . ? C10 C9 H9 126.5 . . ? C8 C9 H9 126.5 . . ? C9 C10 C11 106.8(10) . . ? C9 C10 H10 126.6 . . ? C11 C10 H10 126.6 . . ? N3 C11 C12 126.5(10) . . ? N3 C11 C10 110.5(10) . . ? C12 C11 C10 123.0(10) . . ? C11 C12 C13 124.8(10) . . ? C11 C12 C41 116.5(10) . . ? C13 C12 C41 118.6(10) . . ? N4 C13 C12 124.5(10) . . ? N4 C13 C14 110.0(9) . . ? C12 C13 C14 125.5(10) . . ? C15 C14 C13 107.7(10) . . ? C15 C14 H14 126.2 . . ? C13 C14 H14 126.2 . . ? C14 C15 C16 107.4(10) . . ? C14 C15 H15 126.3 . . ? C16 C15 H15 126.3 . . ? C17 C16 N4 125.0(10) . . ? C17 C16 C15 126.8(10) . . ? N4 C16 C15 108.1(9) . . ? C16 C17 C18 126.6(11) . . ? C16 C17 C111 117.9(10) . . ? C18 C17 C111 115.2(10) . . ? C17 C18 N1 126.1(10) . . ? C17 C18 C19 126.8(10) . . ? N1 C18 C19 107.1(9) . . ? C20 C19 C18 108.1(10) . . ? C20 C19 H19 126 . . ? C18 C19 H19 126 . . ? C19 C20 C1 107.2(10) . . ? C19 C20 H20 126.4 . . ? C1 C20 H20 126.4 . . ? C22 C21 C26 120.4(11) . . ? C22 C21 C2 117.8(11) . . ? C26 C21 C2 121.8(11) . . ? C21 C22 C23 120.8(12) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 118.7(12) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C25 121.2(11) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C24 C25 C26 120.8(13) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C21 C26 N27 119.6(11) . . ? C21 C26 C25 117.9(12) . . ? N27 C26 C25 122.4(11) . . ? C28 N27 C26 127.0(10) . . ? C28 N27 H27 116.5 . . ? C26 N27 H27 116.5 . . ? O29 C28 N27 123.2(13) . . ? O29 C28 C30 118.9(12) . . ? N27 C28 C30 117.9(10) . . ? C35 C30 C31 119.5(13) . . ? C35 C30 C28 124.1(12) . . ? C31 C30 C28 115.8(11) . . ? C32 C31 C30 119.6(12) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 120.1(13) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C34 121.9(14) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C33 C34 C35 117.3(12) . . ? C33 C34 C36 120.5(13) . . ? C35 C34 C36 122.2(12) . . ? C30 C35 C34 121.5(12) . . ? C30 C35 H35 119.2 . . ? C34 C35 H35 119.2 . . ? C34 C36 C61 113.5(11) . . ? C34 C36 H36A 108.9 . . ? C61 C36 H36A 108.9 . . ? C34 C36 H36B 108.9 . . ? C61 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? C46 C41 C42 118.3(11) . . ? C46 C41 C12 124.1(12) . . ? C42 C41 C12 117.5(12) . . ? C43 C42 C41 121.2(15) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C42 C43 C44 120.1(16) . . ? C42 C43 H43 120 . . ? C44 C43 H43 120 . . ? C43 C44 C45 120.0(13) . . ? C43 C44 H44 120 . . ? C45 C44 H44 120 . . ? C44 C45 C46 121.0(14) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C41 C46 C45 119.4(14) . . ? C41 C46 N47 119.1(11) . . ? C45 C46 N47 121.5(13) . . ? C48 N47 C46 127.6(12) . . ? C48 N47 H47 116.2 . . ? C46 N47 H47 116.2 . . ? O49 C48 N47 123.1(16) . . ? O49 C48 C50 120.3(14) . . ? N47 C48 C50 116.4(12) . . ? C55 C50 C51 120.5(15) . . ? C55 C50 C48 124.7(14) . . ? C51 C50 C48 114.7(14) . . ? C50 C51 C52 118.7(15) . . ? C50 C51 H51 120.6 . . ? C52 C51 H51 120.6 . . ? C53 C52 C51 119.5(16) . . ? C53 C52 H52 120.2 . . ? C51 C52 H52 120.2 . . ? C52 C53 C54 122.5(17) . . ? C52 C53 H53 118.7 . . ? C54 C53 H53 118.7 . . ? C53 C54 C55 117.0(15) . . ? C53 C54 C56 120.5(15) . . ? C55 C54 C56 122.5(13) . . ? C50 C55 C54 121.5(14) . . ? C50 C55 H55 119.2 . . ? C54 C55 H55 119.2 . . ? C54 C56 C61 112.7(13) . . ? C54 C56 H56A 109.1 . . ? C61 C56 H56A 109.1 . . ? C54 C56 H56B 109.1 . . ? C61 C56 H56B 109.1 . . ? H56A C56 H56B 107.8 . . ? C62 C61 C36 108.9(11) . . ? C62 C61 C56 108.8(11) . . ? C36 C61 C56 111.6(12) . . ? C62 C61 H61 109.2 . . ? C36 C61 H61 109.2 . . ? C56 C61 H61 109.2 . . ? O63 C62 O64 121.4(13) . . ? O63 C62 C61 117.8(13) . . ? O64 C62 C61 120.7(13) . . ? O63 C62 Pb2 59.1(7) . . ? O64 C62 Pb2 62.3(7) . . ? C61 C62 Pb2 176.4(10) . . ? C62 O63 Pb2 94.0(9) . . ? C62 O64 Pb2 90.7(8) . . ? O72 C71 O73 119.6(16) . . ? O72 C71 C74 124.3(18) . . ? O73 C71 C74 116.1(17) . . ? C71 O72 Pb2 90.8(11) . . ? C71 O73 Pb2 98.0(10) . . ? O82 S8 C81 104.6(8) . . ? O82 S8 C83 107.5(9) . . ? C81 S8 C83 98.0(10) . . ? S8 C81 H81A 109.5 . . ? S8 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? S8 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? S8 O82 Pb2 131.4(6) . . ? S8 C83 H83A 109.5 . . ? S8 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? S8 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C106 C101 C102 119.5(12) . . ? C106 C101 C7 121.0(12) . . ? C102 C101 C7 119.5(11) . . ? C103 C102 C101 120.0(14) . . ? C103 C102 H102 120 . . ? C101 C102 H102 120 . . ? C102 C103 O107 115.3(14) . . ? C102 C103 C104 121.4(14) . . ? O107 C103 C104 123.3(13) . . ? C103 C104 C105 118.4(12) . . ? C103 C104 H104 120.8 . . ? C105 C104 H104 120.8 . . ? C106 C105 O109 123.4(15) . . ? C106 C105 C104 121.8(14) . . ? O109 C105 C104 114.8(13) . . ? C105 C106 C101 119.0(14) . . ? C105 C106 H106 120.5 . . ? C101 C106 H106 120.5 . . ? C103 O107 C108 117.1(16) . . ? O107 C108 H10A 109.5 . . ? O107 C108 H10B 109.5 . . ? H10A C108 H10B 109.5 . . ? O107 C108 H10C 109.5 . . ? H10A C108 H10C 109.5 . . ? H10B C108 H10C 109.5 . . ? C105 O109 C110 118.3(12) . . ? O109 C110 H11A 109.5 . . ? O109 C110 H11B 109.5 . . ? H11A C110 H11B 109.5 . . ? O109 C110 H11C 109.5 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? C112 C111 C116 120.0(11) . . ? C112 C111 C17 121.2(10) . . ? C116 C111 C17 118.6(11) . . ? C111 C112 C113 119.8(11) . . ? C111 C112 H112 120.1 . . ? C113 C112 H112 120.1 . . ? O117 C113 C114 125.2(11) . . ? O117 C113 C112 115.3(11) . . ? C114 C113 C112 119.5(12) . . ? C115 C114 C113 120.2(12) . . ? C115 C114 H114 119.9 . . ? C113 C114 H114 119.9 . . ? C114 C115 O119 115.5(12) . . ? C114 C115 C116 121.1(12) . . ? O119 C115 C116 123.4(13) . . ? C115 C116 C111 119.4(12) . . ? C115 C116 H116 120.3 . . ? C111 C116 H116 120.3 . . ? C113 O117 C118 117.9(11) . . ? O117 C118 H11D 109.5 . . ? O117 C118 H11E 109.5 . . ? H11D C118 H11E 109.5 . . ? O117 C118 H11F 109.5 . . ? H11D C118 H11F 109.5 . . ? H11E C118 H11F 109.5 . . ? C115 O119 C120 118.0(11) . . ? O119 C120 H12A 109.5 . . ? O119 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? O119 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C71 C74 H74A 109.5 . . ? C71 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C71 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 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 N4 Pb1 N1 C1 168.0(10) . . . . ? N3 Pb1 N1 C1 104.5(9) . . . . ? N2 Pb1 N1 C1 41.3(9) . . . . ? N4 Pb1 N1 C18 -42.7(8) . . . . ? N3 Pb1 N1 C18 -106.2(8) . . . . ? N2 Pb1 N1 C18 -169.4(9) . . . . ? N4 Pb1 N2 C3 -104.8(9) . . . . ? N3 Pb1 N2 C3 -166.8(9) . . . . ? N1 Pb1 N2 C3 -41.9(9) . . . . ? N4 Pb1 N2 C6 102.2(9) . . . . ? N3 Pb1 N2 C6 40.3(9) . . . . ? N1 Pb1 N2 C6 165.2(9) . . . . ? N4 Pb1 N3 C11 43.5(8) . . . . ? N1 Pb1 N3 C11 107.3(9) . . . . ? N2 Pb1 N3 C11 170.6(9) . . . . ? N4 Pb1 N3 C8 -164.8(9) . . . . ? N1 Pb1 N3 C8 -101.0(9) . . . . ? N2 Pb1 N3 C8 -37.6(8) . . . . ? N3 Pb1 N4 C13 -48.2(8) . . . . ? N1 Pb1 N4 C13 -172.9(9) . . . . ? N2 Pb1 N4 C13 -110.2(9) . . . . ? N3 Pb1 N4 C16 171.8(9) . . . . ? N1 Pb1 N4 C16 47.1(8) . . . . ? N2 Pb1 N4 C16 109.8(8) . . . . ? C18 N1 C1 C20 0.4(13) . . . . ? Pb1 N1 C1 C20 153.4(8) . . . . ? C18 N1 C1 C2 178.8(11) . . . . ? Pb1 N1 C1 C2 -28.2(16) . . . . ? N1 C1 C2 C3 -6(2) . . . . ? C20 C1 C2 C3 172.5(12) . . . . ? N1 C1 C2 C21 175.9(11) . . . . ? C20 C1 C2 C21 -5.9(18) . . . . ? C6 N2 C3 C2 -171.0(12) . . . . ? Pb1 N2 C3 C2 32.2(16) . . . . ? C6 N2 C3 C4 -0.1(13) . . . . ? Pb1 N2 C3 C4 -156.9(7) . . . . ? C1 C2 C3 N2 3(2) . . . . ? C21 C2 C3 N2 -178.7(11) . . . . ? C1 C2 C3 C4 -166.8(12) . . . . ? C21 C2 C3 C4 11.6(17) . . . . ? N2 C3 C4 C5 -0.6(13) . . . . ? C2 C3 C4 C5 170.6(12) . . . . ? C3 C4 C5 C6 0.9(14) . . . . ? C3 N2 C6 C7 171.0(12) . . . . ? Pb1 N2 C6 C7 -32.7(16) . . . . ? C3 N2 C6 C5 0.6(13) . . . . ? Pb1 N2 C6 C5 156.9(7) . . . . ? C4 C5 C6 C7 -171.0(12) . . . . ? C4 C5 C6 N2 -1.0(14) . . . . ? N2 C6 C7 C8 0(2) . . . . ? C5 C6 C7 C8 168.7(12) . . . . ? N2 C6 C7 C101 -178.6(11) . . . . ? C5 C6 C7 C101 -10.4(19) . . . . ? C11 N3 C8 C7 -177.4(12) . . . . ? Pb1 N3 C8 C7 27.1(16) . . . . ? C11 N3 C8 C9 1.1(13) . . . . ? Pb1 N3 C8 C9 -154.5(8) . . . . ? C6 C7 C8 N3 3(2) . . . . ? C101 C7 C8 N3 -178.1(11) . . . . ? C6 C7 C8 C9 -175.5(12) . . . . ? C101 C7 C8 C9 3.6(18) . . . . ? N3 C8 C9 C10 0.4(13) . . . . ? C7 C8 C9 C10 178.8(12) . . . . ? C8 C9 C10 C11 -1.6(13) . . . . ? C8 N3 C11 C12 177.5(11) . . . . ? Pb1 N3 C11 C12 -26.2(16) . . . . ? C8 N3 C11 C10 -2.2(13) . . . . ? Pb1 N3 C11 C10 154.1(8) . . . . ? C9 C10 C11 N3 2.4(14) . . . . ? C9 C10 C11 C12 -177.2(11) . . . . ? N3 C11 C12 C13 -10(2) . . . . ? C10 C11 C12 C13 169.2(12) . . . . ? N3 C11 C12 C41 174.3(12) . . . . ? C10 C11 C12 C41 -6.1(17) . . . . ? C16 N4 C13 C12 -177.8(11) . . . . ? Pb1 N4 C13 C12 37.2(15) . . . . ? C16 N4 C13 C14 1.1(13) . . . . ? Pb1 N4 C13 C14 -143.9(8) . . . . ? C11 C12 C13 N4 4(2) . . . . ? C41 C12 C13 N4 179.6(11) . . . . ? C11 C12 C13 C14 -174.4(12) . . . . ? C41 C12 C13 C14 0.8(19) . . . . ? N4 C13 C14 C15 1.8(14) . . . . ? C12 C13 C14 C15 -179.3(12) . . . . ? C13 C14 C15 C16 -3.8(13) . . . . ? C13 N4 C16 C17 -179.9(12) . . . . ? Pb1 N4 C16 C17 -34.7(16) . . . . ? C13 N4 C16 C15 -3.4(13) . . . . ? Pb1 N4 C16 C15 141.7(8) . . . . ? C14 C15 C16 C17 -179.1(12) . . . . ? C14 C15 C16 N4 4.6(13) . . . . ? N4 C16 C17 C18 -7(2) . . . . ? C15 C16 C17 C18 177.0(12) . . . . ? N4 C16 C17 C111 179.5(11) . . . . ? C15 C16 C17 C111 3.8(19) . . . . ? C16 C17 C18 N1 12(2) . . . . ? C111 C17 C18 N1 -174.5(11) . . . . ? C16 C17 C18 C19 -166.8(12) . . . . ? C111 C17 C18 C19 6.6(18) . . . . ? C1 N1 C18 C17 179.9(12) . . . . ? Pb1 N1 C18 C17 25.5(16) . . . . ? C1 N1 C18 C19 -1.0(13) . . . . ? Pb1 N1 C18 C19 -155.4(7) . . . . ? C17 C18 C19 C20 -179.7(12) . . . . ? N1 C18 C19 C20 1.2(13) . . . . ? C18 C19 C20 C1 -1.0(13) . . . . ? N1 C1 C20 C19 0.4(14) . . . . ? C2 C1 C20 C19 -178.1(11) . . . . ? C3 C2 C21 C22 72.9(14) . . . . ? C1 C2 C21 C22 -108.5(13) . . . . ? C3 C2 C21 C26 -106.8(13) . . . . ? C1 C2 C21 C26 71.7(15) . . . . ? C26 C21 C22 C23 -3.6(18) . . . . ? C2 C21 C22 C23 176.6(11) . . . . ? C21 C22 C23 C24 2.8(18) . . . . ? C22 C23 C24 C25 -2.2(18) . . . . ? C23 C24 C25 C26 2.3(19) . . . . ? C22 C21 C26 N27 -179.8(11) . . . . ? C2 C21 C26 N27 -0.1(17) . . . . ? C22 C21 C26 C25 3.6(18) . . . . ? C2 C21 C26 C25 -176.6(10) . . . . ? C24 C25 C26 C21 -2.9(18) . . . . ? C24 C25 C26 N27 -179.4(11) . . . . ? C21 C26 N27 C28 -164.0(12) . . . . ? C25 C26 N27 C28 12.5(19) . . . . ? C26 N27 C28 O29 -10(2) . . . . ? C26 N27 C28 C30 167.0(11) . . . . ? O29 C28 C30 C35 136.2(13) . . . . ? N27 C28 C30 C35 -41.1(18) . . . . ? O29 C28 C30 C31 -35.2(18) . . . . ? N27 C28 C30 C31 147.5(12) . . . . ? C35 C30 C31 C32 0.2(18) . . . . ? C28 C30 C31 C32 172.0(12) . . . . ? C30 C31 C32 C33 -1(2) . . . . ? C31 C32 C33 C34 1(2) . . . . ? C32 C33 C34 C35 0.7(19) . . . . ? C32 C33 C34 C36 -179.4(12) . . . . ? C31 C30 C35 C34 1.3(17) . . . . ? C28 C30 C35 C34 -169.8(11) . . . . ? C33 C34 C35 C30 -1.8(17) . . . . ? C36 C34 C35 C30 178.3(11) . . . . ? C33 C34 C36 C61 -79.3(16) . . . . ? C35 C34 C36 C61 100.6(14) . . . . ? C11 C12 C41 C46 104.7(14) . . . . ? C13 C12 C41 C46 -71.0(16) . . . . ? C11 C12 C41 C42 -72.1(15) . . . . ? C13 C12 C41 C42 112.3(14) . . . . ? C46 C41 C42 C43 -2(2) . . . . ? C12 C41 C42 C43 175.1(13) . . . . ? C41 C42 C43 C44 0(2) . . . . ? C42 C43 C44 C45 0(2) . . . . ? C43 C44 C45 C46 1(2) . . . . ? C42 C41 C46 C45 2.8(19) . . . . ? C12 C41 C46 C45 -173.9(12) . . . . ? C42 C41 C46 N47 179.0(12) . . . . ? C12 C41 C46 N47 2.2(19) . . . . ? C44 C45 C46 C41 -2(2) . . . . ? C44 C45 C46 N47 -178.3(14) . . . . ? C41 C46 N47 C48 163.2(14) . . . . ? C45 C46 N47 C48 -21(2) . . . . ? C46 N47 C48 O49 2(3) . . . . ? C46 N47 C48 C50 -173.1(13) . . . . ? O49 C48 C50 C55 -133.4(18) . . . . ? N47 C48 C50 C55 41(2) . . . . ? O49 C48 C50 C51 43(2) . . . . ? N47 C48 C50 C51 -142.3(15) . . . . ? C55 C50 C51 C52 -1(2) . . . . ? C48 C50 C51 C52 -177.9(15) . . . . ? C50 C51 C52 C53 4(3) . . . . ? C51 C52 C53 C54 -2(3) . . . . ? C52 C53 C54 C55 -3(2) . . . . ? C52 C53 C54 C56 178.6(16) . . . . ? C51 C50 C55 C54 -3(2) . . . . ? C48 C50 C55 C54 173.2(14) . . . . ? C53 C54 C55 C50 5(2) . . . . ? C56 C54 C55 C50 -176.4(14) . . . . ? C53 C54 C56 C61 78.8(18) . . . . ? C55 C54 C56 C61 -100.0(16) . . . . ? C34 C36 C61 C62 -64.9(15) . . . . ? C34 C36 C61 C56 175.0(12) . . . . ? C54 C56 C61 C62 62.1(16) . . . . ? C54 C56 C61 C36 -177.8(12) . . . . ? C36 C61 C62 O63 -63.8(16) . . . . ? C56 C61 C62 O63 58.1(16) . . . . ? C36 C61 C62 O64 114.0(14) . . . . ? C56 C61 C62 O64 -124.1(14) . . . . ? O73 Pb2 C62 O63 -101.3(9) . . . . ? O64 Pb2 C62 O63 -180.0(14) . . . . ? O72 Pb2 C62 O63 -150.0(8) . . . . ? O82 Pb2 C62 O63 114.3(9) . . . . ? O63 Pb2 C62 O64 180.0(14) . . . . ? O73 Pb2 C62 O64 78.7(8) . . . . ? O72 Pb2 C62 O64 30.0(9) . . . . ? O82 Pb2 C62 O64 -65.7(8) . . . . ? C61 C62 O63 Pb2 177.7(10) . . . . ? O73 Pb2 O63 C62 77.0(9) . . . . ? O64 Pb2 O63 C62 0.0(8) . . . . ? O72 Pb2 O63 C62 36.2(10) . . . . ? O82 Pb2 O63 C62 -68.3(9) . . . . ? O63 C62 O64 Pb2 0.0(14) . . . . ? C61 C62 O64 Pb2 -177.7(11) . . . . ? O63 Pb2 O64 C62 0.0(8) . . . . ? O73 Pb2 O64 C62 -97.2(8) . . . . ? O72 Pb2 O64 C62 -149.8(9) . . . . ? O82 Pb2 O64 C62 112.1(9) . . . . ? O73 C71 O72 Pb2 -1.2(16) . . . . ? C74 C71 O72 Pb2 178.6(18) . . . . ? O63 Pb2 O72 C71 57.4(11) . . . . ? O73 Pb2 O72 C71 0.7(9) . . . . ? O64 Pb2 O72 C71 86.6(10) . . . . ? O82 Pb2 O72 C71 164.7(10) . . . . ? C62 Pb2 O72 C71 73.2(11) . . . . ? O72 C71 O73 Pb2 1.2(18) . . . . ? C74 C71 O73 Pb2 -178.5(15) . . . . ? O63 Pb2 O73 C71 -136.6(10) . . . . ? O64 Pb2 O73 C71 -83.3(10) . . . . ? O72 Pb2 O73 C71 -0.7(9) . . . . ? O82 Pb2 O73 C71 -28.4(13) . . . . ? C62 Pb2 O73 C71 -110.3(10) . . . . ? C81 S8 O82 Pb2 -56.2(11) . . . . ? C83 S8 O82 Pb2 47.3(12) . . . . ? O63 Pb2 O82 S8 119.8(9) . . . . ? O73 Pb2 O82 S8 15.3(13) . . . . ? O64 Pb2 O82 S8 70.1(9) . . . . ? O72 Pb2 O82 S8 -6.2(9) . . . . ? C62 Pb2 O82 S8 95.0(9) . . . . ? C6 C7 C101 C106 114.5(13) . . . . ? C8 C7 C101 C106 -64.7(15) . . . . ? C6 C7 C101 C102 -64.4(15) . . . . ? C8 C7 C101 C102 116.4(13) . . . . ? C106 C101 C102 C103 0.7(18) . . . . ? C7 C101 C102 C103 179.6(11) . . . . ? C101 C102 C103 O107 178.9(11) . . . . ? C101 C102 C103 C104 0.0(19) . . . . ? C102 C103 C104 C105 -0.1(19) . . . . ? O107 C103 C104 C105 -178.9(12) . . . . ? C103 C104 C105 C106 -0.6(19) . . . . ? C103 C104 C105 O109 178.9(11) . . . . ? O109 C105 C106 C101 -178.2(12) . . . . ? C104 C105 C106 C101 1.3(19) . . . . ? C102 C101 C106 C105 -1.3(18) . . . . ? C7 C101 C106 C105 179.8(11) . . . . ? C102 C103 O107 C108 177.6(13) . . . . ? C104 C103 O107 C108 -3.5(19) . . . . ? C106 C105 O109 C110 -3(2) . . . . ? C104 C105 O109 C110 177.9(13) . . . . ? C16 C17 C111 C112 62.1(16) . . . . ? C18 C17 C111 C112 -111.9(13) . . . . ? C16 C17 C111 C116 -122.2(12) . . . . ? C18 C17 C111 C116 63.8(15) . . . . ? C116 C111 C112 C113 -0.7(18) . . . . ? C17 C111 C112 C113 175.0(11) . . . . ? C111 C112 C113 O117 178.8(12) . . . . ? C111 C112 C113 C114 -0.2(19) . . . . ? O117 C113 C114 C115 -178.6(13) . . . . ? C112 C113 C114 C115 0(2) . . . . ? C113 C114 C115 O119 179.1(12) . . . . ? C113 C114 C115 C116 1(2) . . . . ? C114 C115 C116 C111 -1(2) . . . . ? O119 C115 C116 C111 -179.9(12) . . . . ? C112 C111 C116 C115 1.4(18) . . . . ? C17 C111 C116 C115 -174.3(11) . . . . ? C114 C113 O117 C118 1(2) . . . . ? C112 C113 O117 C118 -178.1(13) . . . . ? C114 C115 O119 C120 -174.0(14) . . . . ? C116 C115 O119 C120 5(2) . . . . ? data_BN327 _database_code_depnum_ccdc_archive 'CCDC 855999' #TrackingRef 'BN327_cif_deposit.cif' _audit_creation_date 2011-10-05T09:27:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C71 H58 N6 O10 Pb1' _chemical_formula_sum 'C71 H58 N6 O10 Pb1' _chemical_formula_weight 1362.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 51.1835(13) _cell_length_b 51.1835 _cell_length_c 16.2681(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 36908.6(13) _cell_formula_units_Z 18 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5653 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 22.81 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12384 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.464 _exptl_absorpt_correction_T_max 0.656 #----------------------------------------------------------------------------# # SQUEEZE RESULTS # #----------------------------------------------------------------------------# # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.009 3660 664 ' ' 2 0.000 0.333 0.401 491 100 ' ' 3 0.000 0.667 0.034 491 98 ' ' 4 0.333 0.667 0.164 3646 663 ' ' 5 0.333 1.000 0.478 491 100 ' ' 6 0.333 0.333 0.511 492 98 ' ' 7 0.666 0.333 0.830 3645 663 ' ' 8 0.667 0.667 0.144 492 100 ' ' 9 0.667 1.000 0.177 491 98 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_unetI/netI 0.0818 _diffrn_reflns_number 64886 _diffrn_reflns_limit_h_min -66 _diffrn_reflns_limit_h_max 58 _diffrn_reflns_limit_k_min -66 _diffrn_reflns_limit_k_max 65 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 18693 _reflns_number_gt 12472 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0479P)^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_number_reflns 18693 _refine_ls_number_parameters 799 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.578 _refine_diff_density_min -0.84 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.730759(3) 0.150478(3) 0.342231(9) 0.02842(5) Uani 1 1 d . . . N1 N 0.73681(7) 0.11562(7) 0.42429(17) 0.0295(7) Uani 1 1 d . . . N2 N 0.70788(7) 0.15021(7) 0.47088(18) 0.0325(8) Uani 1 1 d . . . N3 N 0.68157(7) 0.14101(7) 0.30813(18) 0.0316(7) Uani 1 1 d . . . N4 N 0.70957(7) 0.10515(7) 0.26181(17) 0.0278(7) Uani 1 1 d . . . C1 C 0.74501(8) 0.09580(8) 0.3944(2) 0.0278(8) Uani 1 1 d . . . C2 C 0.75874(9) 0.08758(9) 0.4600(2) 0.0345(9) Uani 1 1 d . . . H2 H 0.7669 0.0745 0.4557 0.041 Uiso 1 1 calc R . . C3 C 0.75776(9) 0.10196(9) 0.5282(2) 0.0380(10) Uani 1 1 d . . . H3 H 0.7648 0.1006 0.5811 0.046 Uiso 1 1 calc R . . C4 C 0.74414(8) 0.11980(8) 0.5070(2) 0.0322(9) Uani 1 1 d . . . C5 C 0.73817(9) 0.13714(8) 0.5624(2) 0.0329(9) Uani 1 1 d . . . C6 C 0.72131(9) 0.15107(9) 0.5451(2) 0.0346(10) Uani 1 1 d . . . C7 C 0.71445(9) 0.16824(9) 0.6030(2) 0.0398(10) Uani 1 1 d . . . H7 H 0.7209 0.1723 0.6587 0.048 Uiso 1 1 calc R . . C8 C 0.69733(9) 0.17748(10) 0.5638(2) 0.0422(11) Uani 1 1 d . . . H8 H 0.6897 0.1895 0.5865 0.051 Uiso 1 1 calc R . . C9 C 0.69269(9) 0.16590(9) 0.4814(2) 0.0360(10) Uani 1 1 d . . . C10 C 0.67606(9) 0.17067(9) 0.4203(2) 0.0377(10) Uani 1 1 d . . . C11 C 0.67058(8) 0.15848(9) 0.3402(2) 0.0349(9) Uani 1 1 d . . . C12 C 0.65184(9) 0.16184(9) 0.2798(2) 0.0387(10) Uani 1 1 d . . . H12 H 0.6416 0.1729 0.2862 0.046 Uiso 1 1 calc R . . C13 C 0.65151(8) 0.14615(9) 0.2116(2) 0.0366(10) Uani 1 1 d . . . H13 H 0.6409 0.1442 0.162 0.044 Uiso 1 1 calc R . . C14 C 0.67017(8) 0.13314(9) 0.2287(2) 0.0308(9) Uani 1 1 d . . . C15 C 0.67568(8) 0.11490(9) 0.1753(2) 0.0312(9) Uani 1 1 d . . . C16 C 0.69244(8) 0.10089(8) 0.1921(2) 0.0294(9) Uani 1 1 d . . . C17 C 0.69375(8) 0.07884(8) 0.1403(2) 0.0295(9) Uani 1 1 d . . . H17 H 0.684 0.0718 0.0887 0.035 Uiso 1 1 calc R . . C18 C 0.71144(9) 0.07002(8) 0.1791(2) 0.0321(9) Uani 1 1 d . . . H18 H 0.7165 0.0556 0.1596 0.039 Uiso 1 1 calc R . . C19 C 0.72111(8) 0.08642(8) 0.2552(2) 0.0281(8) Uani 1 1 d . . . C20 C 0.73911(8) 0.08300(8) 0.3161(2) 0.0286(9) Uani 1 1 d . . . C21 C 0.74977(9) 0.06105(8) 0.2982(2) 0.0303(9) Uani 1 1 d . . . C22 C 0.72918(10) 0.03029(9) 0.2939(2) 0.0390(10) Uani 1 1 d . . . H22 H 0.7083 0.0234 0.3009 0.047 Uiso 1 1 calc R . . C23 C 0.73838(11) 0.00955(9) 0.2799(2) 0.0451(11) Uani 1 1 d . . . H23 H 0.7239 -0.0113 0.2759 0.054 Uiso 1 1 calc R . . C24 C 0.76885(11) 0.01912(10) 0.2714(2) 0.0465(11) Uani 1 1 d . . . H24 H 0.7752 0.0048 0.2625 0.056 Uiso 1 1 calc R . . C25 C 0.78997(10) 0.04948(9) 0.2759(2) 0.0407(10) Uani 1 1 d . . . H25 H 0.8108 0.0561 0.2702 0.049 Uiso 1 1 calc R . . C26 C 0.78049(9) 0.07045(8) 0.2890(2) 0.0310(9) Uani 1 1 d . . . N27 N 0.80112(7) 0.10212(7) 0.28836(18) 0.0309(7) Uani 1 1 d . . . H27 H 0.7932 0.1137 0.2795 0.037 Uiso 1 1 calc R . . C28 C 0.83164(9) 0.11672(9) 0.2998(2) 0.0302(9) Uani 1 1 d . . . O29 O 0.84523(6) 0.10407(6) 0.32194(17) 0.0417(7) Uani 1 1 d . . . C30 C 0.84831(8) 0.15003(8) 0.2812(2) 0.0277(8) Uani 1 1 d . . . C31 C 0.87864(9) 0.16290(9) 0.2620(2) 0.0318(9) Uani 1 1 d . . . H31 H 0.8882 0.1511 0.2651 0.038 Uiso 1 1 calc R . . C32 C 0.89502(9) 0.19274(9) 0.2383(2) 0.0347(9) Uani 1 1 d . . . H32 H 0.9157 0.2014 0.2238 0.042 Uiso 1 1 calc R . . C33 C 0.88093(9) 0.21027(8) 0.2358(2) 0.0305(9) Uani 1 1 d . . . H33 H 0.8923 0.2309 0.22 0.037 Uiso 1 1 calc R . . C34 C 0.85094(9) 0.19810(8) 0.2560(2) 0.0296(9) Uani 1 1 d . . . C35 C 0.83442(8) 0.16784(8) 0.2786(2) 0.0285(8) Uani 1 1 d . . . H35 H 0.8137 0.1592 0.2924 0.034 Uiso 1 1 calc R . . C36 C 0.83597(9) 0.21688(8) 0.2467(2) 0.0303(9) Uani 1 1 d . . . H36A H 0.8145 0.203 0.2336 0.036 Uiso 1 1 calc R . . H36B H 0.8451 0.2301 0.1983 0.036 Uiso 1 1 calc R . . C37 C 0.83707(8) 0.23713(8) 0.3193(2) 0.0290(9) Uani 1 1 d . . . C38 C 0.82810(9) 0.26016(8) 0.2873(2) 0.0316(9) Uani 1 1 d . . . H38A H 0.8326 0.2755 0.3305 0.038 Uiso 1 1 calc R . . H38B H 0.8407 0.2707 0.2388 0.038 Uiso 1 1 calc R . . C39 C 0.86895(9) 0.25358(8) 0.3555(2) 0.0295(9) Uani 1 1 d . . . O40 O 0.87646(6) 0.24592(6) 0.41621(16) 0.0403(7) Uani 1 1 d . . . O41 O 0.88723(6) 0.27687(6) 0.30802(15) 0.0354(6) Uani 1 1 d . . . C42 C 0.91848(9) 0.29535(9) 0.3355(2) 0.0399(10) Uani 1 1 d . . . H42A H 0.9286 0.2832 0.3364 0.048 Uiso 1 1 calc R . . H42B H 0.9191 0.3031 0.3916 0.048 Uiso 1 1 calc R . . C43 C 0.93378(10) 0.32079(10) 0.2763(3) 0.0468(11) Uani 1 1 d . . . H43A H 0.9332 0.3128 0.2212 0.07 Uiso 1 1 calc R . . H43B H 0.9548 0.3338 0.2932 0.07 Uiso 1 1 calc R . . H43C H 0.9234 0.3325 0.2756 0.07 Uiso 1 1 calc R . . C44 C 0.81525(8) 0.21800(9) 0.3870(2) 0.0301(9) Uani 1 1 d . . . O45 O 0.80002(6) 0.19065(6) 0.38539(16) 0.0376(7) Uani 1 1 d . . . O46 O 0.81396(6) 0.23496(6) 0.44719(15) 0.0337(6) Uani 1 1 d . . . C47 C 0.79066(9) 0.21887(10) 0.5096(2) 0.0428(11) Uani 1 1 d . . . H47A H 0.7947 0.2044 0.5394 0.051 Uiso 1 1 calc R . . H47B H 0.7706 0.2075 0.4833 0.051 Uiso 1 1 calc R . . C48 C 0.79120(10) 0.24168(10) 0.5683(3) 0.0522(13) Uani 1 1 d . . . H48A H 0.811 0.2524 0.5952 0.078 Uiso 1 1 calc R . . H48B H 0.7755 0.2314 0.61 0.078 Uiso 1 1 calc R . . H48C H 0.7875 0.2561 0.5382 0.078 Uiso 1 1 calc R . . C51 C 0.66250(9) 0.18981(10) 0.4407(3) 0.0450(11) Uani 1 1 d . . . C52 C 0.63935(10) 0.18052(12) 0.4981(3) 0.0555(13) Uani 1 1 d . . . H52 H 0.6332 0.1626 0.5288 0.067 Uiso 1 1 calc R . . C53 C 0.62534(12) 0.19732(16) 0.5106(4) 0.0783(19) Uani 1 1 d . . . H53 H 0.609 0.1903 0.5483 0.094 Uiso 1 1 calc R . . C54 C 0.63433(14) 0.22324(17) 0.4705(4) 0.088(2) Uani 1 1 d . . . H54 H 0.6246 0.2346 0.4802 0.105 Uiso 1 1 calc R . . C55 C 0.65786(13) 0.23344(13) 0.4146(4) 0.0750(17) Uani 1 1 d . . . H55 H 0.6641 0.2517 0.3855 0.09 Uiso 1 1 calc R . . C56 C 0.67218(10) 0.21746(11) 0.4010(3) 0.0534(13) Uani 1 1 d . . . N57 N 0.69635(8) 0.22765(8) 0.3427(2) 0.0511(10) Uani 1 1 d . . . H57 H 0.6935 0.2313 0.2915 0.061 Uiso 1 1 calc R . . C58 C 0.72364(10) 0.23169(9) 0.3665(3) 0.0468(12) Uani 1 1 d . . . O59 O 0.73142(6) 0.23412(7) 0.4388(2) 0.0516(8) Uani 1 1 d . . . C60 C 0.74409(10) 0.23231(9) 0.2994(3) 0.0399(10) Uani 1 1 d . . . C61 C 0.73374(10) 0.21918(10) 0.2235(3) 0.0464(11) Uani 1 1 d . . . H61 H 0.7129 0.2098 0.2105 0.056 Uiso 1 1 calc R . . C62 C 0.75394(11) 0.21979(10) 0.1670(3) 0.0506(12) Uani 1 1 d . . . H62 H 0.747 0.2109 0.1145 0.061 Uiso 1 1 calc R . . C63 C 0.78456(11) 0.23335(10) 0.1859(3) 0.0456(11) Uani 1 1 d . . . H63 H 0.7984 0.234 0.1458 0.055 Uiso 1 1 calc R . . C64 C 0.79497(9) 0.24591(9) 0.2634(2) 0.0367(10) Uani 1 1 d . . . C65 C 0.77432(9) 0.24494(8) 0.3188(2) 0.0359(10) Uani 1 1 d . . . H65 H 0.781 0.2532 0.372 0.043 Uiso 1 1 calc R . . C71 C 0.66130(9) 0.10982(9) 0.0920(2) 0.0314(9) Uani 1 1 d . . . C72 C 0.67723(9) 0.12898(10) 0.0284(2) 0.0442(11) Uani 1 1 d . . . H72 H 0.697 0.1455 0.0377 0.053 Uiso 1 1 calc R . . C73 C 0.66425(10) 0.12410(11) -0.0497(3) 0.0496(12) Uani 1 1 d . . . C74 C 0.63572(10) 0.10046(10) -0.0641(2) 0.0414(11) Uani 1 1 d . . . H74 H 0.627 0.0972 -0.1174 0.05 Uiso 1 1 calc R . . C75 C 0.61973(9) 0.08131(9) 0.0008(2) 0.0336(9) Uani 1 1 d . . . C76 C 0.63218(8) 0.08539(9) 0.0782(2) 0.0315(9) Uani 1 1 d . . . H76 H 0.6212 0.0719 0.1215 0.038 Uiso 1 1 calc R . . O77 O 0.68210(8) 0.14478(9) -0.10796(19) 0.0739(11) Uani 1 1 d . . . C78 C 0.67084(14) 0.13942(17) -0.1909(3) 0.099(2) Uani 1 1 d . . . H78A H 0.6852 0.1558 -0.2265 0.149 Uiso 1 1 calc R . . H78B H 0.6513 0.1386 -0.1924 0.149 Uiso 1 1 calc R . . H78C H 0.6684 0.1202 -0.2105 0.149 Uiso 1 1 calc R . . O79 O 0.59143(6) 0.05866(7) -0.01999(16) 0.0463(8) Uani 1 1 d . . . C80 C 0.57291(10) 0.03912(10) 0.0434(3) 0.0500(12) Uani 1 1 d . . . H80A H 0.5809 0.0261 0.061 0.075 Uiso 1 1 calc R . . H80B H 0.5523 0.0266 0.0227 0.075 Uiso 1 1 calc R . . H80C H 0.5728 0.0511 0.0901 0.075 Uiso 1 1 calc R . . C81 C 0.74963(9) 0.13926(8) 0.6483(2) 0.0330(9) Uani 1 1 d . . . C82 C 0.78039(9) 0.15532(8) 0.6658(2) 0.0339(9) Uani 1 1 d . . . H82 H 0.7946 0.1659 0.6235 0.041 Uiso 1 1 calc R . . C83 C 0.79007(9) 0.15568(9) 0.7457(2) 0.0348(9) Uani 1 1 d . . . C84 C 0.76971(9) 0.14047(9) 0.8088(2) 0.0349(10) Uani 1 1 d . . . H84 H 0.7765 0.1412 0.8635 0.042 Uiso 1 1 calc R . . C85 C 0.73934(9) 0.12433(9) 0.7896(2) 0.0358(10) Uani 1 1 d . . . C86 C 0.72915(9) 0.12395(9) 0.7099(2) 0.0386(10) Uani 1 1 d . . . H86 H 0.7082 0.1132 0.6981 0.046 Uiso 1 1 calc R . . O87 O 0.82073(6) 0.17220(7) 0.75779(16) 0.0447(7) Uani 1 1 d . . . C88 C 0.83151(10) 0.17231(12) 0.8391(2) 0.0597(14) Uani 1 1 d . . . H88A H 0.8242 0.1822 0.8767 0.09 Uiso 1 1 calc R . . H88B H 0.8536 0.1833 0.839 0.09 Uiso 1 1 calc R . . H88C H 0.8241 0.1515 0.8571 0.09 Uiso 1 1 calc R . . O89 O 0.71740(7) 0.10774(7) 0.84637(16) 0.0516(8) Uani 1 1 d . . . C90 C 0.72734(11) 0.10933(12) 0.9299(2) 0.0647(15) Uani 1 1 d . . . H90A H 0.742 0.1024 0.9325 0.097 Uiso 1 1 calc R . . H90B H 0.71 0.0965 0.9649 0.097 Uiso 1 1 calc R . . H90C H 0.7368 0.1302 0.9493 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.02484(8) 0.02659(9) 0.02577(8) 0.00021(6) -0.00209(6) 0.00682(7) N1 0.0281(18) 0.0296(18) 0.0232(16) -0.0026(14) -0.0053(13) 0.0088(15) N2 0.0237(17) 0.0337(19) 0.0259(17) -0.0022(14) -0.0018(13) 0.0037(15) N3 0.0284(18) 0.0335(19) 0.0273(17) -0.0018(14) -0.0030(14) 0.0114(16) N4 0.0251(17) 0.0313(18) 0.0201(16) 0.0016(13) -0.0038(13) 0.0089(15) C1 0.023(2) 0.023(2) 0.0253(19) 0.0033(16) -0.0042(15) 0.0025(16) C2 0.039(2) 0.028(2) 0.029(2) 0.0047(17) -0.0030(18) 0.0114(19) C3 0.044(3) 0.034(2) 0.025(2) 0.0018(17) -0.0080(18) 0.011(2) C4 0.028(2) 0.028(2) 0.026(2) -0.0005(17) -0.0037(16) 0.0026(18) C5 0.032(2) 0.027(2) 0.023(2) 0.0012(16) -0.0002(17) 0.0028(18) C6 0.031(2) 0.033(2) 0.025(2) -0.0008(17) 0.0008(17) 0.0046(19) C7 0.035(2) 0.039(2) 0.030(2) -0.0073(18) 0.0006(18) 0.006(2) C8 0.038(3) 0.046(3) 0.038(2) -0.012(2) -0.001(2) 0.017(2) C9 0.025(2) 0.039(2) 0.035(2) -0.0046(19) 0.0011(18) 0.0097(19) C10 0.024(2) 0.038(2) 0.040(2) -0.0056(19) -0.0004(18) 0.0074(19) C11 0.019(2) 0.033(2) 0.043(2) -0.0040(19) 0.0015(17) 0.0061(18) C12 0.025(2) 0.044(3) 0.044(3) 0.000(2) 0.0009(19) 0.015(2) C13 0.025(2) 0.045(3) 0.033(2) 0.0023(19) -0.0039(17) 0.012(2) C14 0.023(2) 0.035(2) 0.026(2) 0.0033(17) 0.0021(16) 0.0076(18) C15 0.024(2) 0.032(2) 0.028(2) 0.0020(17) -0.0018(16) 0.0067(18) C16 0.028(2) 0.032(2) 0.0203(19) 0.0022(16) -0.0021(16) 0.0090(18) C17 0.034(2) 0.027(2) 0.0179(18) 0.0006(15) -0.0030(16) 0.0082(18) C18 0.037(2) 0.027(2) 0.027(2) -0.0003(16) -0.0027(17) 0.0118(19) C19 0.029(2) 0.024(2) 0.0251(19) 0.0040(16) -0.0003(16) 0.0082(17) C20 0.028(2) 0.0213(19) 0.027(2) 0.0029(16) -0.0026(16) 0.0048(17) C21 0.038(2) 0.028(2) 0.0207(19) 0.0031(16) -0.0048(17) 0.0136(19) C22 0.044(3) 0.032(2) 0.034(2) 0.0042(18) -0.0107(19) 0.014(2) C23 0.057(3) 0.024(2) 0.041(3) 0.0040(19) -0.015(2) 0.010(2) C24 0.064(3) 0.033(3) 0.042(3) -0.001(2) -0.010(2) 0.024(2) C25 0.051(3) 0.037(3) 0.032(2) 0.0045(19) -0.004(2) 0.021(2) C26 0.042(2) 0.024(2) 0.0227(19) 0.0011(16) -0.0033(17) 0.0139(19) N27 0.0281(18) 0.0246(17) 0.0396(19) 0.0027(14) 0.0006(14) 0.0130(15) C28 0.036(2) 0.035(2) 0.0206(19) -0.0001(16) -0.0017(16) 0.019(2) O29 0.0397(17) 0.0349(16) 0.0509(18) 0.0040(13) -0.0086(14) 0.0188(14) C30 0.034(2) 0.028(2) 0.0199(18) -0.0048(15) -0.0062(16) 0.0144(18) C31 0.034(2) 0.034(2) 0.028(2) -0.0065(17) -0.0039(17) 0.0177(19) C32 0.030(2) 0.036(2) 0.031(2) -0.0029(18) -0.0027(17) 0.0112(19) C33 0.035(2) 0.021(2) 0.028(2) -0.0036(16) -0.0044(17) 0.0081(18) C34 0.035(2) 0.032(2) 0.0191(18) -0.0041(16) -0.0067(16) 0.0149(19) C35 0.025(2) 0.032(2) 0.0231(19) -0.0062(16) -0.0041(15) 0.0103(18) C36 0.034(2) 0.025(2) 0.027(2) -0.0051(16) -0.0101(17) 0.0105(18) C37 0.033(2) 0.022(2) 0.028(2) -0.0063(16) -0.0046(17) 0.0108(17) C38 0.035(2) 0.026(2) 0.029(2) -0.0011(16) 0.0011(17) 0.0128(18) C39 0.034(2) 0.027(2) 0.025(2) -0.0063(17) -0.0007(17) 0.0128(18) O40 0.0353(16) 0.0446(18) 0.0310(15) 0.0031(13) -0.0059(13) 0.0123(14) O41 0.0319(15) 0.0295(15) 0.0325(15) 0.0022(12) -0.0023(12) 0.0059(13) C42 0.032(2) 0.036(2) 0.036(2) -0.0051(19) -0.0079(18) 0.005(2) C43 0.041(3) 0.038(3) 0.053(3) -0.002(2) 0.002(2) 0.014(2) C44 0.030(2) 0.025(2) 0.032(2) -0.0017(17) -0.0043(17) 0.0108(18) O45 0.0331(16) 0.0240(15) 0.0471(17) -0.0005(13) 0.0000(13) 0.0078(13) O46 0.0335(15) 0.0277(15) 0.0299(14) -0.0012(12) 0.0049(12) 0.0077(12) C47 0.036(2) 0.042(3) 0.038(2) 0.008(2) 0.0097(19) 0.010(2) C48 0.048(3) 0.052(3) 0.037(2) 0.000(2) 0.015(2) 0.009(2) C51 0.031(2) 0.046(3) 0.056(3) -0.018(2) -0.007(2) 0.018(2) C52 0.038(3) 0.063(3) 0.057(3) -0.019(3) -0.003(2) 0.019(3) C53 0.039(3) 0.100(5) 0.089(5) -0.044(4) -0.002(3) 0.030(4) C54 0.053(4) 0.101(6) 0.128(6) -0.047(5) -0.010(4) 0.052(4) C55 0.060(4) 0.071(4) 0.109(5) -0.029(3) -0.021(3) 0.044(3) C56 0.035(3) 0.057(3) 0.074(3) -0.021(3) -0.012(2) 0.027(3) N57 0.040(2) 0.040(2) 0.075(3) -0.001(2) -0.005(2) 0.0213(19) C58 0.031(3) 0.031(2) 0.071(3) -0.006(2) -0.007(2) 0.010(2) O59 0.0341(18) 0.051(2) 0.065(2) -0.0096(16) -0.0039(16) 0.0174(16) C60 0.039(3) 0.026(2) 0.051(3) 0.0023(19) -0.003(2) 0.013(2) C61 0.040(3) 0.040(3) 0.061(3) -0.007(2) -0.013(2) 0.022(2) C62 0.056(3) 0.050(3) 0.053(3) -0.009(2) -0.022(2) 0.031(3) C63 0.052(3) 0.045(3) 0.044(3) -0.008(2) -0.007(2) 0.028(2) C64 0.042(3) 0.029(2) 0.041(2) 0.0031(18) -0.005(2) 0.019(2) C65 0.038(2) 0.025(2) 0.041(2) 0.0026(18) -0.0025(19) 0.0133(19) C71 0.031(2) 0.041(2) 0.024(2) 0.0008(17) 0.0001(16) 0.019(2) C72 0.031(2) 0.048(3) 0.037(2) 0.011(2) -0.0008(19) 0.007(2) C73 0.045(3) 0.069(3) 0.033(2) 0.021(2) 0.008(2) 0.027(3) C74 0.044(3) 0.065(3) 0.020(2) -0.001(2) -0.0018(18) 0.031(2) C75 0.031(2) 0.043(2) 0.027(2) -0.0013(18) -0.0022(17) 0.019(2) C76 0.031(2) 0.036(2) 0.026(2) 0.0036(17) 0.0010(17) 0.0157(19) O77 0.066(2) 0.098(3) 0.0402(19) 0.0350(19) 0.0113(17) 0.027(2) C78 0.079(4) 0.159(7) 0.046(3) 0.046(4) 0.014(3) 0.048(5) O79 0.0395(18) 0.058(2) 0.0283(15) -0.0077(14) -0.0083(13) 0.0150(16) C80 0.037(3) 0.053(3) 0.043(3) -0.008(2) -0.008(2) 0.010(2) C81 0.037(2) 0.026(2) 0.025(2) -0.0061(16) -0.0047(17) 0.0069(18) C82 0.036(2) 0.028(2) 0.026(2) 0.0031(16) 0.0010(17) 0.0078(19) C83 0.033(2) 0.034(2) 0.026(2) -0.0027(17) -0.0052(17) 0.0080(19) C84 0.041(2) 0.036(2) 0.022(2) -0.0019(17) -0.0061(18) 0.015(2) C85 0.039(2) 0.033(2) 0.022(2) 0.0034(17) 0.0009(17) 0.008(2) C86 0.030(2) 0.037(2) 0.029(2) 0.0028(18) -0.0027(18) 0.0026(19) O87 0.0335(17) 0.057(2) 0.0274(15) -0.0006(13) -0.0042(12) 0.0100(15) C88 0.038(3) 0.086(4) 0.028(2) -0.003(2) -0.011(2) 0.010(3) O89 0.0450(19) 0.062(2) 0.0230(15) 0.0105(14) 0.0012(13) 0.0081(16) C90 0.063(3) 0.082(4) 0.025(2) 0.016(2) 0.010(2) 0.018(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N1 2.369(3) . ? Pb1 N3 2.380(3) . ? Pb1 N2 2.395(3) . ? Pb1 N4 2.399(3) . ? N1 C1 1.366(5) . ? N1 C4 1.385(4) . ? N2 C6 1.379(5) . ? N2 C9 1.380(5) . ? N3 C11 1.375(5) . ? N3 C14 1.392(4) . ? N4 C19 1.358(5) . ? N4 C16 1.383(4) . ? C1 C20 1.396(5) . ? C1 C2 1.451(5) . ? C2 C3 1.346(5) . ? C2 H2 0.95 . ? C3 C4 1.440(6) . ? C3 H3 0.95 . ? C4 C5 1.401(5) . ? C5 C6 1.396(6) . ? C5 C81 1.499(5) . ? C6 C7 1.446(6) . ? C7 C8 1.347(6) . ? C7 H7 0.95 . ? C8 C9 1.437(5) . ? C8 H8 0.95 . ? C9 C10 1.407(6) . ? C10 C11 1.411(5) . ? C10 C51 1.494(6) . ? C11 C12 1.443(5) . ? C12 C13 1.364(5) . ? C12 H12 0.95 . ? C13 C14 1.438(5) . ? C13 H13 0.95 . ? C14 C15 1.404(5) . ? C15 C16 1.392(5) . ? C15 C71 1.501(5) . ? C16 C17 1.437(5) . ? C17 C18 1.353(5) . ? C17 H17 0.95 . ? C18 C19 1.438(5) . ? C18 H18 0.95 . ? C19 C20 1.421(5) . ? C20 C21 1.502(5) . ? C21 C22 1.391(5) . ? C21 C26 1.403(5) . ? C22 C23 1.379(6) . ? C22 H22 0.95 . ? C23 C24 1.388(6) . ? C23 H23 0.95 . ? C24 C25 1.382(6) . ? C24 H24 0.95 . ? C25 C26 1.398(5) . ? C25 H25 0.95 . ? C26 N27 1.425(5) . ? N27 C28 1.366(5) . ? N27 H27 0.88 . ? C28 O29 1.218(4) . ? C28 C30 1.507(5) . ? C30 C31 1.385(5) . ? C30 C35 1.409(5) . ? C31 C32 1.380(5) . ? C31 H31 0.95 . ? C32 C33 1.405(5) . ? C32 H32 0.95 . ? C33 C34 1.377(5) . ? C33 H33 0.95 . ? C34 C35 1.393(5) . ? C34 C36 1.506(5) . ? C35 H35 0.95 . ? C36 C37 1.553(5) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? C37 C44 1.525(5) . ? C37 C39 1.531(5) . ? C37 C38 1.554(5) . ? C38 C64 1.523(5) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 O40 1.195(4) . ? C39 O41 1.333(4) . ? O41 C42 1.463(4) . ? C42 C43 1.488(5) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 O45 1.215(4) . ? C44 O46 1.332(4) . ? O46 C47 1.466(4) . ? C47 C48 1.497(6) . ? C47 H47A 0.99 . ? C47 H47B 0.99 . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C51 C52 1.392(6) . ? C51 C56 1.401(6) . ? C52 C53 1.382(8) . ? C52 H52 0.95 . ? C53 C54 1.337(8) . ? C53 H53 0.95 . ? C54 C55 1.386(8) . ? C54 H54 0.95 . ? C55 C56 1.361(6) . ? C55 H55 0.95 . ? C56 N57 1.435(6) . ? N57 C58 1.362(5) . ? N57 H57 0.88 . ? C58 O59 1.228(5) . ? C58 C60 1.502(6) . ? C60 C61 1.379(6) . ? C60 C65 1.382(6) . ? C61 C62 1.372(6) . ? C61 H61 0.95 . ? C62 C63 1.395(6) . ? C62 H62 0.95 . ? C63 C64 1.395(5) . ? C63 H63 0.95 . ? C64 C65 1.370(6) . ? C65 H65 0.95 . ? C71 C72 1.377(5) . ? C71 C76 1.404(5) . ? C72 C73 1.398(6) . ? C72 H72 0.95 . ? C73 C74 1.373(6) . ? C73 O77 1.374(5) . ? C74 C75 1.395(5) . ? C74 H74 0.95 . ? C75 O79 1.370(5) . ? C75 C76 1.378(5) . ? C76 H76 0.95 . ? O77 C78 1.439(6) . ? C78 H78A 0.98 . ? C78 H78B 0.98 . ? C78 H78C 0.98 . ? O79 C80 1.419(5) . ? C80 H80A 0.98 . ? C80 H80B 0.98 . ? C80 H80C 0.98 . ? C81 C86 1.376(5) . ? C81 C82 1.394(5) . ? C82 C83 1.388(5) . ? C82 H82 0.95 . ? C83 O87 1.374(4) . ? C83 C84 1.390(5) . ? C84 C85 1.383(5) . ? C84 H84 0.95 . ? C85 O89 1.371(4) . ? C85 C86 1.395(5) . ? C86 H86 0.95 . ? O87 C88 1.431(4) . ? C88 H88A 0.98 . ? C88 H88B 0.98 . ? C88 H88C 0.98 . ? O89 C90 1.440(5) . ? C90 H90A 0.98 . ? C90 H90B 0.98 . ? C90 H90C 0.98 . ? 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 N1 Pb1 N3 120.10(10) . . ? N1 Pb1 N2 75.57(11) . . ? N3 Pb1 N2 74.81(10) . . ? N1 Pb1 N4 75.23(10) . . ? N3 Pb1 N4 75.84(10) . . ? N2 Pb1 N4 119.19(10) . . ? C1 N1 C4 107.4(3) . . ? C1 N1 Pb1 124.3(2) . . ? C4 N1 Pb1 124.0(2) . . ? C6 N2 C9 106.8(3) . . ? C6 N2 Pb1 122.0(3) . . ? C9 N2 Pb1 121.4(2) . . ? C11 N3 C14 107.0(3) . . ? C11 N3 Pb1 120.9(2) . . ? C14 N3 Pb1 121.5(2) . . ? C19 N4 C16 106.8(3) . . ? C19 N4 Pb1 125.4(2) . . ? C16 N4 Pb1 123.0(2) . . ? N1 C1 C20 126.8(3) . . ? N1 C1 C2 109.1(3) . . ? C20 C1 C2 123.9(4) . . ? C3 C2 C1 106.9(4) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? C2 C3 C4 108.2(3) . . ? C2 C3 H3 125.9 . . ? C4 C3 H3 125.9 . . ? N1 C4 C5 126.4(4) . . ? N1 C4 C3 108.3(3) . . ? C5 C4 C3 125.2(3) . . ? C6 C5 C4 125.5(3) . . ? C6 C5 C81 118.0(3) . . ? C4 C5 C81 116.4(4) . . ? N2 C6 C5 125.8(4) . . ? N2 C6 C7 108.7(4) . . ? C5 C6 C7 125.4(4) . . ? C8 C7 C6 107.7(4) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 107.4(4) . . ? C7 C8 H8 126.3 . . ? C9 C8 H8 126.3 . . ? N2 C9 C10 125.4(4) . . ? N2 C9 C8 109.3(4) . . ? C10 C9 C8 125.2(4) . . ? C9 C10 C11 125.4(4) . . ? C9 C10 C51 118.5(4) . . ? C11 C10 C51 116.1(4) . . ? N3 C11 C10 125.6(4) . . ? N3 C11 C12 109.3(3) . . ? C10 C11 C12 125.0(4) . . ? C13 C12 C11 107.3(4) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? C12 C13 C14 107.5(3) . . ? C12 C13 H13 126.3 . . ? C14 C13 H13 126.3 . . ? N3 C14 C15 124.9(3) . . ? N3 C14 C13 108.9(3) . . ? C15 C14 C13 126.1(3) . . ? C16 C15 C14 127.0(3) . . ? C16 C15 C71 117.6(3) . . ? C14 C15 C71 115.4(3) . . ? N4 C16 C15 125.8(3) . . ? N4 C16 C17 109.3(3) . . ? C15 C16 C17 124.9(3) . . ? C18 C17 C16 106.9(3) . . ? C18 C17 H17 126.6 . . ? C16 C17 H17 126.6 . . ? C17 C18 C19 107.4(3) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? N4 C19 C20 124.7(3) . . ? N4 C19 C18 109.6(3) . . ? C20 C19 C18 125.7(4) . . ? C1 C20 C19 125.4(4) . . ? C1 C20 C21 117.0(3) . . ? C19 C20 C21 117.2(3) . . ? C22 C21 C26 117.9(4) . . ? C22 C21 C20 120.2(4) . . ? C26 C21 C20 121.8(3) . . ? C23 C22 C21 121.5(4) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23 120 . . ? C24 C23 H23 120 . . ? C25 C24 C23 120.1(4) . . ? C25 C24 H24 120 . . ? C23 C24 H24 120 . . ? C24 C25 C26 119.7(4) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C21 120.8(4) . . ? C25 C26 N27 121.9(4) . . ? C21 C26 N27 117.2(3) . . ? C28 N27 C26 128.0(3) . . ? C28 N27 H27 116 . . ? C26 N27 H27 116 . . ? O29 C28 N27 123.4(4) . . ? O29 C28 C30 120.7(4) . . ? N27 C28 C30 115.9(3) . . ? C31 C30 C35 119.6(3) . . ? C31 C30 C28 116.7(3) . . ? C35 C30 C28 123.7(3) . . ? C32 C31 C30 120.4(4) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 119.5(4) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C34 C33 C32 121.1(4) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C35 119.0(4) . . ? C33 C34 C36 119.7(3) . . ? C35 C34 C36 121.1(3) . . ? C34 C35 C30 120.4(3) . . ? C34 C35 H35 119.8 . . ? C30 C35 H35 119.8 . . ? C34 C36 C37 119.3(3) . . ? C34 C36 H36A 107.5 . . ? C37 C36 H36A 107.5 . . ? C34 C36 H36B 107.5 . . ? C37 C36 H36B 107.5 . . ? H36A C36 H36B 107 . . ? C44 C37 C39 108.2(3) . . ? C44 C37 C36 110.5(3) . . ? C39 C37 C36 109.4(3) . . ? C44 C37 C38 109.2(3) . . ? C39 C37 C38 110.5(3) . . ? C36 C37 C38 109.0(3) . . ? C64 C38 C37 113.7(3) . . ? C64 C38 H38A 108.8 . . ? C37 C38 H38A 108.8 . . ? C64 C38 H38B 108.8 . . ? C37 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? O40 C39 O41 125.1(4) . . ? O40 C39 C37 124.5(4) . . ? O41 C39 C37 110.3(3) . . ? C39 O41 C42 116.9(3) . . ? O41 C42 C43 107.2(3) . . ? O41 C42 H42A 110.3 . . ? C43 C42 H42A 110.3 . . ? O41 C42 H42B 110.3 . . ? C43 C42 H42B 110.3 . . ? H42A C42 H42B 108.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O45 C44 O46 123.6(3) . . ? O45 C44 C37 124.5(3) . . ? O46 C44 C37 111.8(3) . . ? C44 O46 C47 115.8(3) . . ? O46 C47 C48 108.1(3) . . ? O46 C47 H47A 110.1 . . ? C48 C47 H47A 110.1 . . ? O46 C47 H47B 110.1 . . ? C48 C47 H47B 110.1 . . ? H47A C47 H47B 108.4 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C52 C51 C56 117.7(4) . . ? C52 C51 C10 121.4(4) . . ? C56 C51 C10 121.0(4) . . ? C53 C52 C51 120.3(5) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C54 C53 C52 121.2(6) . . ? C54 C53 H53 119.4 . . ? C52 C53 H53 119.4 . . ? C53 C54 C55 119.8(6) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C56 C55 C54 120.5(6) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? C55 C56 C51 120.5(5) . . ? C55 C56 N57 120.9(5) . . ? C51 C56 N57 118.5(4) . . ? C58 N57 C56 119.9(4) . . ? C58 N57 H57 120 . . ? C56 N57 H57 120 . . ? O59 C58 N57 123.0(4) . . ? O59 C58 C60 120.5(4) . . ? N57 C58 C60 116.6(4) . . ? C61 C60 C65 119.9(4) . . ? C61 C60 C58 123.2(4) . . ? C65 C60 C58 116.7(4) . . ? C62 C61 C60 119.2(4) . . ? C62 C61 H61 120.4 . . ? C60 C61 H61 120.4 . . ? C61 C62 C63 120.7(4) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 119.7 . . ? C62 C63 C64 120.3(4) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 119.9 . . ? C65 C64 C63 117.9(4) . . ? C65 C64 C38 120.3(4) . . ? C63 C64 C38 121.9(4) . . ? C64 C65 C60 122.0(4) . . ? C64 C65 H65 119 . . ? C60 C65 H65 119 . . ? C72 C71 C76 120.0(3) . . ? C72 C71 C15 119.3(3) . . ? C76 C71 C15 120.6(3) . . ? C71 C72 C73 119.8(4) . . ? C71 C72 H72 120.1 . . ? C73 C72 H72 120.1 . . ? C74 C73 O77 124.4(4) . . ? C74 C73 C72 121.0(4) . . ? O77 C73 C72 114.6(4) . . ? C73 C74 C75 118.8(4) . . ? C73 C74 H74 120.6 . . ? C75 C74 H74 120.6 . . ? O79 C75 C76 124.6(4) . . ? O79 C75 C74 114.1(3) . . ? C76 C75 C74 121.4(4) . . ? C75 C76 C71 119.1(4) . . ? C75 C76 H76 120.5 . . ? C71 C76 H76 120.5 . . ? C73 O77 C78 116.9(4) . . ? O77 C78 H78A 109.5 . . ? O77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? O77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C75 O79 C80 117.9(3) . . ? O79 C80 H80A 109.5 . . ? O79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? O79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C86 C81 C82 120.1(3) . . ? C86 C81 C5 118.6(3) . . ? C82 C81 C5 121.2(3) . . ? C83 C82 C81 119.3(4) . . ? C83 C82 H82 120.3 . . ? C81 C82 H82 120.3 . . ? O87 C83 C82 115.6(3) . . ? O87 C83 C84 123.0(3) . . ? C82 C83 C84 121.4(4) . . ? C85 C84 C83 118.2(3) . . ? C85 C84 H84 120.9 . . ? C83 C84 H84 120.9 . . ? O89 C85 C84 123.1(3) . . ? O89 C85 C86 115.6(4) . . ? C84 C85 C86 121.2(4) . . ? C81 C86 C85 119.7(4) . . ? C81 C86 H86 120.1 . . ? C85 C86 H86 120.1 . . ? C83 O87 C88 117.0(3) . . ? O87 C88 H88A 109.5 . . ? O87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? O87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C85 O89 C90 116.4(3) . . ? O89 C90 H90A 109.5 . . ? O89 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? O89 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 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 N3 Pb1 N1 C1 103.8(3) . . . . ? N2 Pb1 N1 C1 166.3(3) . . . . ? N4 Pb1 N1 C1 40.2(3) . . . . ? N3 Pb1 N1 C4 -102.5(3) . . . . ? N2 Pb1 N1 C4 -40.0(3) . . . . ? N4 Pb1 N1 C4 -166.1(3) . . . . ? N1 Pb1 N2 C6 44.3(3) . . . . ? N3 Pb1 N2 C6 171.6(3) . . . . ? N4 Pb1 N2 C6 107.8(3) . . . . ? N1 Pb1 N2 C9 -174.2(3) . . . . ? N3 Pb1 N2 C9 -46.9(3) . . . . ? N4 Pb1 N2 C9 -110.6(3) . . . . ? N1 Pb1 N3 C11 111.2(3) . . . . ? N2 Pb1 N3 C11 48.3(3) . . . . ? N4 Pb1 N3 C11 174.4(3) . . . . ? N1 Pb1 N3 C14 -108.7(3) . . . . ? N2 Pb1 N3 C14 -171.6(3) . . . . ? N4 Pb1 N3 C14 -45.5(3) . . . . ? N1 Pb1 N4 C19 -39.7(3) . . . . ? N3 Pb1 N4 C19 -166.7(3) . . . . ? N2 Pb1 N4 C19 -103.5(3) . . . . ? N1 Pb1 N4 C16 168.0(3) . . . . ? N3 Pb1 N4 C16 41.1(3) . . . . ? N2 Pb1 N4 C16 104.3(3) . . . . ? C4 N1 C1 C20 173.3(3) . . . . ? Pb1 N1 C1 C20 -29.3(5) . . . . ? C4 N1 C1 C2 -1.4(4) . . . . ? Pb1 N1 C1 C2 156.0(2) . . . . ? N1 C1 C2 C3 1.6(4) . . . . ? C20 C1 C2 C3 -173.3(4) . . . . ? C1 C2 C3 C4 -1.1(4) . . . . ? C1 N1 C4 C5 -176.4(4) . . . . ? Pb1 N1 C4 C5 26.1(5) . . . . ? C1 N1 C4 C3 0.7(4) . . . . ? Pb1 N1 C4 C3 -156.7(2) . . . . ? C2 C3 C4 N1 0.3(4) . . . . ? C2 C3 C4 C5 177.5(4) . . . . ? N1 C4 C5 C6 6.1(6) . . . . ? C3 C4 C5 C6 -170.5(4) . . . . ? N1 C4 C5 C81 -177.4(3) . . . . ? C3 C4 C5 C81 6.0(5) . . . . ? C9 N2 C6 C5 177.9(4) . . . . ? Pb1 N2 C6 C5 -35.8(5) . . . . ? C9 N2 C6 C7 -0.8(4) . . . . ? Pb1 N2 C6 C7 145.5(3) . . . . ? C4 C5 C6 N2 -0.3(6) . . . . ? C81 C5 C6 N2 -176.8(3) . . . . ? C4 C5 C6 C7 178.1(4) . . . . ? C81 C5 C6 C7 1.7(6) . . . . ? N2 C6 C7 C8 -0.2(4) . . . . ? C5 C6 C7 C8 -178.8(4) . . . . ? C6 C7 C8 C9 1.0(5) . . . . ? C6 N2 C9 C10 179.5(4) . . . . ? Pb1 N2 C9 C10 32.9(5) . . . . ? C6 N2 C9 C8 1.4(4) . . . . ? Pb1 N2 C9 C8 -145.2(3) . . . . ? C7 C8 C9 N2 -1.5(5) . . . . ? C7 C8 C9 C10 -179.6(4) . . . . ? N2 C9 C10 C11 4.5(6) . . . . ? C8 C9 C10 C11 -177.7(4) . . . . ? N2 C9 C10 C51 -176.4(4) . . . . ? C8 C9 C10 C51 1.5(6) . . . . ? C14 N3 C11 C10 178.4(4) . . . . ? Pb1 N3 C11 C10 -36.4(5) . . . . ? C14 N3 C11 C12 -0.1(4) . . . . ? Pb1 N3 C11 C12 145.0(3) . . . . ? C9 C10 C11 N3 -2.7(6) . . . . ? C51 C10 C11 N3 178.1(4) . . . . ? C9 C10 C11 C12 175.7(4) . . . . ? C51 C10 C11 C12 -3.5(6) . . . . ? N3 C11 C12 C13 0.4(4) . . . . ? C10 C11 C12 C13 -178.2(4) . . . . ? C11 C12 C13 C14 -0.5(4) . . . . ? C11 N3 C14 C15 -178.9(4) . . . . ? Pb1 N3 C14 C15 36.2(5) . . . . ? C11 N3 C14 C13 -0.2(4) . . . . ? Pb1 N3 C14 C13 -145.1(3) . . . . ? C12 C13 C14 N3 0.4(4) . . . . ? C12 C13 C14 C15 179.1(4) . . . . ? N3 C14 C15 C16 2.0(6) . . . . ? C13 C14 C15 C16 -176.6(4) . . . . ? N3 C14 C15 C71 -179.2(3) . . . . ? C13 C14 C15 C71 2.3(5) . . . . ? C19 N4 C16 C15 177.6(4) . . . . ? Pb1 N4 C16 C15 -25.8(5) . . . . ? C19 N4 C16 C17 -0.5(4) . . . . ? Pb1 N4 C16 C17 156.1(2) . . . . ? C14 C15 C16 N4 -7.7(6) . . . . ? C71 C15 C16 N4 173.5(3) . . . . ? C14 C15 C16 C17 170.1(4) . . . . ? C71 C15 C16 C17 -8.7(6) . . . . ? N4 C16 C17 C18 0.2(4) . . . . ? C15 C16 C17 C18 -177.9(4) . . . . ? C16 C17 C18 C19 0.2(4) . . . . ? C16 N4 C19 C20 -177.3(3) . . . . ? Pb1 N4 C19 C20 26.8(5) . . . . ? C16 N4 C19 C18 0.7(4) . . . . ? Pb1 N4 C19 C18 -155.2(2) . . . . ? C17 C18 C19 N4 -0.6(4) . . . . ? C17 C18 C19 C20 177.4(3) . . . . ? N1 C1 C20 C19 -5.7(6) . . . . ? C2 C1 C20 C19 168.3(4) . . . . ? N1 C1 C20 C21 -178.4(3) . . . . ? C2 C1 C20 C21 -4.4(5) . . . . ? N4 C19 C20 C1 7.0(6) . . . . ? C18 C19 C20 C1 -170.7(4) . . . . ? N4 C19 C20 C21 179.7(3) . . . . ? C18 C19 C20 C21 2.0(5) . . . . ? C1 C20 C21 C22 106.0(4) . . . . ? C19 C20 C21 C22 -67.3(4) . . . . ? C1 C20 C21 C26 -71.1(4) . . . . ? C19 C20 C21 C26 115.6(4) . . . . ? C26 C21 C22 C23 -1.0(5) . . . . ? C20 C21 C22 C23 -178.2(3) . . . . ? C21 C22 C23 C24 1.5(6) . . . . ? C22 C23 C24 C25 -0.9(6) . . . . ? C23 C24 C25 C26 0.0(6) . . . . ? C24 C25 C26 C21 0.4(5) . . . . ? C24 C25 C26 N27 -175.4(3) . . . . ? C22 C21 C26 C25 0.1(5) . . . . ? C20 C21 C26 C25 177.2(3) . . . . ? C22 C21 C26 N27 176.2(3) . . . . ? C20 C21 C26 N27 -6.7(5) . . . . ? C25 C26 N27 C28 -21.0(5) . . . . ? C21 C26 N27 C28 163.0(3) . . . . ? C26 N27 C28 O29 -8.7(6) . . . . ? C26 N27 C28 C30 169.7(3) . . . . ? O29 C28 C30 C31 22.1(5) . . . . ? N27 C28 C30 C31 -156.3(3) . . . . ? O29 C28 C30 C35 -161.0(3) . . . . ? N27 C28 C30 C35 20.5(5) . . . . ? C35 C30 C31 C32 -1.7(5) . . . . ? C28 C30 C31 C32 175.2(3) . . . . ? C30 C31 C32 C33 1.6(5) . . . . ? C31 C32 C33 C34 -0.5(5) . . . . ? C32 C33 C34 C35 -0.4(5) . . . . ? C32 C33 C34 C36 -175.6(3) . . . . ? C33 C34 C35 C30 0.3(5) . . . . ? C36 C34 C35 C30 175.4(3) . . . . ? C31 C30 C35 C34 0.8(5) . . . . ? C28 C30 C35 C34 -176.0(3) . . . . ? C33 C34 C36 C37 -88.2(4) . . . . ? C35 C34 C36 C37 96.7(4) . . . . ? C34 C36 C37 C44 -75.1(4) . . . . ? C34 C36 C37 C39 43.9(5) . . . . ? C34 C36 C37 C38 164.8(3) . . . . ? C44 C37 C38 C64 -51.4(4) . . . . ? C39 C37 C38 C64 -170.3(3) . . . . ? C36 C37 C38 C64 69.4(4) . . . . ? C44 C37 C39 O40 20.7(5) . . . . ? C36 C37 C39 O40 -99.7(4) . . . . ? C38 C37 C39 O40 140.3(4) . . . . ? C44 C37 C39 O41 -161.6(3) . . . . ? C36 C37 C39 O41 78.0(4) . . . . ? C38 C37 C39 O41 -42.0(4) . . . . ? O40 C39 O41 C42 -3.6(5) . . . . ? C37 C39 O41 C42 178.7(3) . . . . ? C39 O41 C42 C43 -176.4(3) . . . . ? C39 C37 C44 O45 -117.2(4) . . . . ? C36 C37 C44 O45 2.5(5) . . . . ? C38 C37 C44 O45 122.4(4) . . . . ? C39 C37 C44 O46 65.1(4) . . . . ? C36 C37 C44 O46 -175.1(3) . . . . ? C38 C37 C44 O46 -55.2(4) . . . . ? O45 C44 O46 C47 -5.5(5) . . . . ? C37 C44 O46 C47 172.2(3) . . . . ? C44 O46 C47 C48 -176.1(3) . . . . ? C9 C10 C51 C52 -66.8(5) . . . . ? C11 C10 C51 C52 112.4(5) . . . . ? C9 C10 C51 C56 114.8(5) . . . . ? C11 C10 C51 C56 -66.0(5) . . . . ? C56 C51 C52 C53 4.2(7) . . . . ? C10 C51 C52 C53 -174.2(4) . . . . ? C51 C52 C53 C54 -2.5(8) . . . . ? C52 C53 C54 C55 0.8(9) . . . . ? C53 C54 C55 C56 -0.9(9) . . . . ? C54 C55 C56 C51 2.8(8) . . . . ? C54 C55 C56 N57 179.3(5) . . . . ? C52 C51 C56 C55 -4.4(7) . . . . ? C10 C51 C56 C55 174.0(4) . . . . ? C52 C51 C56 N57 179.0(4) . . . . ? C10 C51 C56 N57 -2.6(6) . . . . ? C55 C56 N57 C58 124.9(5) . . . . ? C51 C56 N57 C58 -58.5(6) . . . . ? C56 N57 C58 O59 -18.0(6) . . . . ? C56 N57 C58 C60 160.5(4) . . . . ? O59 C58 C60 C61 155.4(4) . . . . ? N57 C58 C60 C61 -23.2(6) . . . . ? O59 C58 C60 C65 -19.9(6) . . . . ? N57 C58 C60 C65 161.5(4) . . . . ? C65 C60 C61 C62 -2.3(6) . . . . ? C58 C60 C61 C62 -177.4(4) . . . . ? C60 C61 C62 C63 0.4(7) . . . . ? C61 C62 C63 C64 1.4(7) . . . . ? C62 C63 C64 C65 -1.3(6) . . . . ? C62 C63 C64 C38 178.3(4) . . . . ? C37 C38 C64 C65 94.7(4) . . . . ? C37 C38 C64 C63 -84.9(5) . . . . ? C63 C64 C65 C60 -0.6(6) . . . . ? C38 C64 C65 C60 179.8(3) . . . . ? C61 C60 C65 C64 2.5(6) . . . . ? C58 C60 C65 C64 177.9(4) . . . . ? C16 C15 C71 C72 -89.2(5) . . . . ? C14 C15 C71 C72 91.8(5) . . . . ? C16 C15 C71 C76 89.3(5) . . . . ? C14 C15 C71 C76 -89.7(5) . . . . ? C76 C71 C72 C73 0.3(6) . . . . ? C15 C71 C72 C73 178.8(4) . . . . ? C71 C72 C73 C74 0.2(7) . . . . ? C71 C72 C73 O77 179.4(4) . . . . ? O77 C73 C74 C75 -178.9(4) . . . . ? C72 C73 C74 C75 0.2(7) . . . . ? C73 C74 C75 O79 179.4(4) . . . . ? C73 C74 C75 C76 -1.1(6) . . . . ? O79 C75 C76 C71 -179.0(4) . . . . ? C74 C75 C76 C71 1.6(6) . . . . ? C72 C71 C76 C75 -1.2(6) . . . . ? C15 C71 C76 C75 -179.6(4) . . . . ? C74 C73 O77 C78 -5.7(7) . . . . ? C72 C73 O77 C78 175.1(5) . . . . ? C76 C75 O79 C80 4.0(6) . . . . ? C74 C75 O79 C80 -176.5(4) . . . . ? C6 C5 C81 C86 69.1(5) . . . . ? C4 C5 C81 C86 -107.7(4) . . . . ? C6 C5 C81 C82 -113.5(4) . . . . ? C4 C5 C81 C82 69.7(5) . . . . ? C86 C81 C82 C83 0.0(6) . . . . ? C5 C81 C82 C83 -177.4(4) . . . . ? C81 C82 C83 O87 -179.6(4) . . . . ? C81 C82 C83 C84 -0.3(6) . . . . ? O87 C83 C84 C85 -179.5(4) . . . . ? C82 C83 C84 C85 1.3(6) . . . . ? C83 C84 C85 O89 177.9(4) . . . . ? C83 C84 C85 C86 -1.9(6) . . . . ? C82 C81 C86 C85 -0.6(6) . . . . ? C5 C81 C86 C85 176.9(4) . . . . ? O89 C85 C86 C81 -178.2(4) . . . . ? C84 C85 C86 C81 1.6(6) . . . . ? C82 C83 O87 C88 -178.2(4) . . . . ? C84 C83 O87 C88 2.5(6) . . . . ? C84 C85 O89 C90 3.8(6) . . . . ? C86 C85 O89 C90 -176.4(4) . . . . ?