# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email hroesky@gwdg.de _publ_contact_author_name 'Roesky, Herbert' loop_ _publ_author_name A.Jana S.P.Sarish D.Leusser I.Objartel H.W.Roesky D.Stalke data_PbF _database_code_depnum_ccdc_archive 'CCDC 808034' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H41 F N2 Pb' _chemical_formula_weight 643.83 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7697(16) _cell_length_b 20.465(3) _cell_length_c 11.7727(16) _cell_angle_alpha 90.00 _cell_angle_beta 95.906(2) _cell_angle_gamma 90.00 _cell_volume 2820.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9918 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 30.54 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 6.006 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5022 _exptl_absorpt_correction_T_max 0.7589 _exptl_absorpt_process_details SADABS-2008/2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS-Mo rotating anode' _diffrn_radiation_monochromator 'INCOATEC Helios Mirror optics' _diffrn_measurement_device_type 'Bruker TXS-Mo rotating anode' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 90262 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 30.62 _reflns_number_total 8667 _reflns_number_gt 7652 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 v2010.11-0' _computing_cell_refinement 'SAINT V7.68A' _computing_data_reduction 'SAINT V7.68A' _computing_structure_solution 'SHELXS in SHELXTL Version 2008/4' _computing_structure_refinement 'SHELXL in SHELXTL Version 2008/4' _computing_molecular_graphics 'XSHELL vers. 4.01' _computing_publication_material 'XSHELL vers. 4.01' _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^)+(0.0180P)^2^+3.7248P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8667 _refine_ls_number_parameters 350 _refine_ls_number_restraints 715 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0503 _refine_ls_wR_factor_gt 0.0491 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.147 _refine_ls_shift/su_mean 0.011 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 0.53693(5) 0.40213(4) 0.48651(6) 0.01197(13) Uani 0.4425(17) 1 d PDU A 1 F1 F 0.3689(12) 0.3726(10) 0.440(3) 0.032(2) Uani 0.4425(17) 1 d PDU A 1 N2 N 0.611(2) 0.3016(8) 0.4374(8) 0.0163(9) Uani 0.4425(17) 1 d PDU A 1 C3 C 0.625(3) 0.2778(8) 0.3350(9) 0.0180(10) Uani 0.4425(17) 1 d PDU A 1 C5 C 0.6818(8) 0.2117(5) 0.3284(8) 0.0227(10) Uani 0.4425(17) 1 d PDU A 1 H5A H 0.7007 0.1944 0.4057 0.034 Uiso 0.4425(17) 1 calc PR A 1 H5B H 0.7520 0.2165 0.2909 0.034 Uiso 0.4425(17) 1 calc PR A 1 H5C H 0.6299 0.1815 0.2843 0.034 Uiso 0.4425(17) 1 calc PR A 1 C2 C 0.593(2) 0.3094(7) 0.2314(11) 0.0200(15) Uani 0.4425(17) 1 d PDU A 1 H2 H 0.5945 0.2830 0.1652 0.024 Uiso 0.4425(17) 1 calc PR A 1 C1 C 0.5591(14) 0.3745(7) 0.2108(12) 0.0185(16) Uani 0.4425(17) 1 d PDU A 1 C4 C 0.5474(9) 0.3944(8) 0.0865(11) 0.0259(13) Uani 0.4425(17) 1 d PDU A 1 H4A H 0.5272 0.4408 0.0800 0.039 Uiso 0.4425(17) 1 calc PR A 1 H4B H 0.4873 0.3683 0.0442 0.039 Uiso 0.4425(17) 1 calc PR A 1 H4C H 0.6200 0.3871 0.0546 0.039 Uiso 0.4425(17) 1 calc PR A 1 N1 N 0.548(3) 0.4192(8) 0.2904(15) 0.0225(15) Uani 0.4425(17) 1 d PDU A 1 C6 C 0.5266(14) 0.4866(7) 0.264(3) 0.0205(11) Uani 0.4425(17) 1 d PGDU A 1 C7 C 0.6154(13) 0.5311(10) 0.285(3) 0.0220(10) Uani 0.4425(17) 1 d PGDU A 1 C8 C 0.5963(18) 0.5972(9) 0.264(4) 0.0252(14) Uani 0.4425(17) 1 d PGDU A 1 H8 H 0.6570 0.6276 0.2786 0.030 Uiso 0.4425(17) 1 calc PR A 1 C9 C 0.488(2) 0.6188(8) 0.221(4) 0.0267(18) Uani 0.4425(17) 1 d PGDU A 1 H9 H 0.4753 0.6640 0.2065 0.032 Uiso 0.4425(17) 1 calc PR A 1 C10 C 0.3995(16) 0.5743(10) 0.200(3) 0.0265(16) Uani 0.4425(17) 1 d PGDU A 1 H10 H 0.3257 0.5891 0.1704 0.032 Uiso 0.4425(17) 1 calc PR A 1 C11 C 0.4186(13) 0.5082(9) 0.221(2) 0.0244(12) Uani 0.4425(17) 1 d PGDU A 1 C12 C 0.7367(17) 0.5074(17) 0.330(3) 0.0269(11) Uani 0.4425(17) 1 d PDU A 1 H12 H 0.7263 0.4706 0.3841 0.032 Uiso 0.4425(17) 1 calc PR A 1 C13 C 0.803(3) 0.479(4) 0.236(5) 0.045(3) Uani 0.4425(17) 1 d PDU A 1 H13A H 0.8809 0.4688 0.2672 0.067 Uiso 0.4425(17) 1 calc PR A 1 H13B H 0.8051 0.5119 0.1747 0.067 Uiso 0.4425(17) 1 calc PR A 1 H13C H 0.7647 0.4398 0.2044 0.067 Uiso 0.4425(17) 1 calc PR A 1 C14 C 0.810(4) 0.559(3) 0.398(6) 0.0322(11) Uani 0.4425(17) 1 d PDU A 1 H14A H 0.7687 0.5760 0.4593 0.048 Uiso 0.4425(17) 1 calc PR A 1 H14B H 0.8275 0.5943 0.3468 0.048 Uiso 0.4425(17) 1 calc PR A 1 H14C H 0.8817 0.5385 0.4308 0.048 Uiso 0.4425(17) 1 calc PR A 1 C15 C 0.3129(11) 0.4626(10) 0.2062(11) 0.0263(15) Uani 0.4425(17) 1 d PDU A 1 H15 H 0.3402 0.4169 0.2216 0.032 Uiso 0.4425(17) 1 calc PR A 1 C16 C 0.2277(14) 0.4786(10) 0.2911(10) 0.0331(14) Uani 0.4425(17) 1 d PDU A 1 H16A H 0.1624 0.4488 0.2794 0.050 Uiso 0.4425(17) 1 calc PR A 1 H16B H 0.2011 0.5237 0.2795 0.050 Uiso 0.4425(17) 1 calc PR A 1 H16C H 0.2647 0.4736 0.3691 0.050 Uiso 0.4425(17) 1 calc PR A 1 C17 C 0.2551(9) 0.4650(6) 0.0826(8) 0.0374(14) Uani 0.4425(17) 1 d PDU A 1 H17A H 0.3113 0.4543 0.0295 0.056 Uiso 0.4425(17) 1 calc PR A 1 H17B H 0.2249 0.5090 0.0660 0.056 Uiso 0.4425(17) 1 calc PR A 1 H17C H 0.1924 0.4333 0.0737 0.056 Uiso 0.4425(17) 1 calc PR A 1 C18 C 0.6569(2) 0.26817(19) 0.5384(2) 0.0174(7) Uani 0.4425(17) 1 d PGDU A 1 C19 C 0.7680(2) 0.28180(12) 0.5841(2) 0.0249(6) Uani 0.4425(17) 1 d PGDU A 1 C20 C 0.8108(2) 0.25430(16) 0.6877(2) 0.0323(7) Uani 0.4425(17) 1 d PGDU A 1 H20 H 0.8867 0.2636 0.7189 0.039 Uiso 0.4425(17) 1 calc PR A 1 C21 C 0.7425(3) 0.21318(18) 0.7456(2) 0.0357(8) Uani 0.4425(17) 1 d PGDU A 1 H21 H 0.7718 0.1944 0.8164 0.043 Uiso 0.4425(17) 1 calc PR A 1 C22 C 0.6314(3) 0.19955(17) 0.6999(3) 0.0311(7) Uani 0.4425(17) 1 d PGDU A 1 H22 H 0.5847 0.1715 0.7395 0.037 Uiso 0.4425(17) 1 calc PR A 1 C23 C 0.5886(2) 0.2271(2) 0.5963(3) 0.0218(7) Uani 0.4425(17) 1 d PGDU A 1 C24 C 0.8461(3) 0.32791(18) 0.5220(3) 0.0302(7) Uani 0.4425(17) 1 d PGDU A 1 H24 H 0.8048 0.3380 0.4454 0.036 Uiso 0.4425(17) 1 calc PR A 1 C25 C 0.9610(5) 0.2968(4) 0.5009(5) 0.0418(9) Uani 0.4425(17) 1 d PDU A 1 H25A H 0.9471 0.2552 0.4607 0.063 Uiso 0.4425(17) 1 calc PR A 1 H25B H 1.0063 0.2890 0.5742 0.063 Uiso 0.4425(17) 1 calc PR A 1 H25C H 1.0026 0.3263 0.4544 0.063 Uiso 0.4425(17) 1 calc PR A 1 C26 C 0.8651(5) 0.3921(3) 0.5846(6) 0.0416(9) Uani 0.4425(17) 1 d PDU A 1 H26A H 0.7912 0.4114 0.5970 0.062 Uiso 0.4425(17) 1 calc PR A 1 H26B H 0.9068 0.4221 0.5389 0.062 Uiso 0.4425(17) 1 calc PR A 1 H26C H 0.9096 0.3846 0.6584 0.062 Uiso 0.4425(17) 1 calc PR A 1 C27 C 0.4673(5) 0.2067(4) 0.5450(6) 0.0245(8) Uani 0.4425(17) 1 d PDU A 1 H27 H 0.4532 0.2282 0.4685 0.029 Uiso 0.4425(17) 1 calc PR A 1 C28 C 0.4567(7) 0.1330(4) 0.5251(7) 0.0390(12) Uani 0.4425(17) 1 d PDU A 1 H28A H 0.5169 0.1184 0.4794 0.059 Uiso 0.4425(17) 1 calc PR A 1 H28B H 0.3818 0.1231 0.4845 0.059 Uiso 0.4425(17) 1 calc PR A 1 H28C H 0.4647 0.1103 0.5988 0.059 Uiso 0.4425(17) 1 calc PR A 1 C29 C 0.3741(5) 0.2303(4) 0.6162(6) 0.0371(9) Uani 0.4425(17) 1 d PDU A 1 H29A H 0.3814 0.2775 0.6280 0.056 Uiso 0.4425(17) 1 calc PR A 1 H29B H 0.3822 0.2080 0.6903 0.056 Uiso 0.4425(17) 1 calc PR A 1 H29C H 0.2990 0.2204 0.5760 0.056 Uiso 0.4425(17) 1 calc PR A 1 Pb1' Pb 0.53046(6) 0.40168(4) 0.48305(6) 0.0341(2) Uani 0.5575(17) 1 d PDU A 2 F1' F 0.3700(9) 0.3594(8) 0.442(3) 0.032(2) Uani 0.5575(17) 1 d PDU A 2 N2' N 0.6093(15) 0.3026(6) 0.4577(6) 0.0163(9) Uani 0.5575(17) 1 d PDU A 2 C3' C 0.624(2) 0.2754(6) 0.3579(7) 0.0180(10) Uani 0.5575(17) 1 d PDU A 2 C5' C 0.6598(6) 0.2044(4) 0.3531(6) 0.0227(10) Uani 0.5575(17) 1 d PDU A 2 H5'1 H 0.6676 0.1860 0.4304 0.034 Uiso 0.5575(17) 1 calc PR A 2 H5'2 H 0.7331 0.2014 0.3209 0.034 Uiso 0.5575(17) 1 calc PR A 2 H5'3 H 0.6018 0.1798 0.3050 0.034 Uiso 0.5575(17) 1 calc PR A 2 C2' C 0.6089(16) 0.3072(6) 0.2515(8) 0.0200(15) Uani 0.5575(17) 1 d PDU A 2 H2' H 0.6176 0.2795 0.1882 0.024 Uiso 0.5575(17) 1 calc PR A 2 C1' C 0.5836(9) 0.3724(5) 0.2219(9) 0.0185(16) Uani 0.5575(17) 1 d PDU A 2 C4' C 0.5789(6) 0.3884(6) 0.0956(8) 0.0259(13) Uani 0.5575(17) 1 d PDU A 2 H4'1 H 0.5581 0.4344 0.0835 0.039 Uiso 0.5575(17) 1 calc PR A 2 H4'2 H 0.5217 0.3606 0.0528 0.039 Uiso 0.5575(17) 1 calc PR A 2 H4'3 H 0.6539 0.3804 0.0691 0.039 Uiso 0.5575(17) 1 calc PR A 2 N1' N 0.559(3) 0.4177(7) 0.2964(12) 0.0225(15) Uani 0.5575(17) 1 d PDU A 2 C6' C 0.5402(11) 0.4844(6) 0.262(2) 0.0205(11) Uani 0.5575(17) 1 d PGDU A 2 C7' C 0.6285(10) 0.5292(8) 0.284(3) 0.0220(10) Uani 0.5575(17) 1 d PGDU A 2 C8' C 0.6092(14) 0.5951(7) 0.261(3) 0.0252(14) Uani 0.5575(17) 1 d PGDU A 2 H8' H 0.6695 0.6257 0.2762 0.030 Uiso 0.5575(17) 1 calc PR A 2 C9' C 0.5015(16) 0.6163(6) 0.217(3) 0.0267(18) Uani 0.5575(17) 1 d PGDU A 2 H9' H 0.4883 0.6613 0.2010 0.032 Uiso 0.5575(17) 1 calc PR A 2 C10' C 0.4132(13) 0.5715(8) 0.195(2) 0.0265(16) Uani 0.5575(17) 1 d PGDU A 2 H10' H 0.3396 0.5859 0.1643 0.032 Uiso 0.5575(17) 1 calc PR A 2 C11' C 0.4325(10) 0.5056(7) 0.2176(19) 0.0244(12) Uani 0.5575(17) 1 d PGDU A 2 C12' C 0.7477(13) 0.5069(13) 0.339(2) 0.0269(11) Uani 0.5575(17) 1 d PDU A 2 H12' H 0.7353 0.4712 0.3943 0.032 Uiso 0.5575(17) 1 calc PR A 2 C13' C 0.818(3) 0.478(3) 0.248(3) 0.045(3) Uani 0.5575(17) 1 d PDU A 2 H13D H 0.8940 0.4663 0.2829 0.067 Uiso 0.5575(17) 1 calc PR A 2 H13E H 0.8242 0.5104 0.1874 0.067 Uiso 0.5575(17) 1 calc PR A 2 H13F H 0.7792 0.4389 0.2147 0.067 Uiso 0.5575(17) 1 calc PR A 2 C14' C 0.816(3) 0.561(3) 0.405(5) 0.0322(11) Uani 0.5575(17) 1 d PDU A 2 H14D H 0.7699 0.5803 0.4606 0.048 Uiso 0.5575(17) 1 calc PR A 2 H14E H 0.8360 0.5947 0.3511 0.048 Uiso 0.5575(17) 1 calc PR A 2 H14F H 0.8861 0.5424 0.4441 0.048 Uiso 0.5575(17) 1 calc PR A 2 C15' C 0.3323(8) 0.4572(7) 0.1893(8) 0.0263(15) Uani 0.5575(17) 1 d PDU A 2 H15' H 0.3605 0.4123 0.2105 0.032 Uiso 0.5575(17) 1 calc PR A 2 C16' C 0.2326(11) 0.4725(8) 0.2590(7) 0.0331(14) Uani 0.5575(17) 1 d PDU A 2 H16D H 0.1708 0.4410 0.2399 0.050 Uiso 0.5575(17) 1 calc PR A 2 H16E H 0.2045 0.5168 0.2411 0.050 Uiso 0.5575(17) 1 calc PR A 2 H16F H 0.2586 0.4695 0.3407 0.050 Uiso 0.5575(17) 1 calc PR A 2 C17' C 0.2895(7) 0.4568(5) 0.0609(7) 0.0374(14) Uani 0.5575(17) 1 d PDU A 2 H17D H 0.3531 0.4464 0.0164 0.056 Uiso 0.5575(17) 1 calc PR A 2 H17E H 0.2587 0.5000 0.0385 0.056 Uiso 0.5575(17) 1 calc PR A 2 H17F H 0.2294 0.4238 0.0462 0.056 Uiso 0.5575(17) 1 calc PR A 2 C18' C 0.62925(18) 0.26492(14) 0.56065(17) 0.0174(7) Uani 0.5575(17) 1 d PGDU A 2 C19' C 0.73031(15) 0.27434(10) 0.63080(17) 0.0249(6) Uani 0.5575(17) 1 d PGDU A 2 C20' C 0.7491(2) 0.24098(12) 0.73387(18) 0.0323(7) Uani 0.5575(17) 1 d PGDU A 2 H20' H 0.8182 0.2474 0.7818 0.039 Uiso 0.5575(17) 1 calc PR A 2 C21' C 0.6668(2) 0.19820(13) 0.76679(19) 0.0357(8) Uani 0.5575(17) 1 d PGDU A 2 H21' H 0.6796 0.1754 0.8372 0.043 Uiso 0.5575(17) 1 calc PR A 2 C22' C 0.5657(2) 0.18878(12) 0.6966(2) 0.0311(7) Uani 0.5575(17) 1 d PGDU A 2 H22' H 0.5095 0.1595 0.7191 0.037 Uiso 0.5575(17) 1 calc PR A 2 C23' C 0.54695(18) 0.22214(15) 0.5936(2) 0.0218(7) Uani 0.5575(17) 1 d PGDU A 2 C24' C 0.8218(2) 0.32381(14) 0.5970(3) 0.0302(7) Uani 0.5575(17) 1 d PGDU A 2 H24' H 0.7800 0.3626 0.5621 0.036 Uiso 0.5575(17) 1 calc PR A 2 C25' C 0.8936(4) 0.2953(3) 0.5063(4) 0.0418(9) Uani 0.5575(17) 1 d PDU A 2 H25D H 0.8427 0.2796 0.4409 0.063 Uiso 0.5575(17) 1 calc PR A 2 H25E H 0.9398 0.2588 0.5395 0.063 Uiso 0.5575(17) 1 calc PR A 2 H25F H 0.9440 0.3292 0.4810 0.063 Uiso 0.5575(17) 1 calc PR A 2 C26' C 0.9018(4) 0.3482(3) 0.6978(5) 0.0416(9) Uani 0.5575(17) 1 d PDU A 2 H26D H 0.8568 0.3667 0.7556 0.062 Uiso 0.5575(17) 1 calc PR A 2 H26E H 0.9522 0.3820 0.6718 0.062 Uiso 0.5575(17) 1 calc PR A 2 H26F H 0.9479 0.3118 0.7310 0.062 Uiso 0.5575(17) 1 calc PR A 2 C27' C 0.4342(4) 0.2098(3) 0.5172(5) 0.0245(8) Uani 0.5575(17) 1 d PDU A 2 H27' H 0.4388 0.2331 0.4432 0.029 Uiso 0.5575(17) 1 calc PR A 2 C28' C 0.4143(5) 0.1365(3) 0.4907(6) 0.0390(12) Uani 0.5575(17) 1 d PDU A 2 H28D H 0.4797 0.1189 0.4554 0.059 Uiso 0.5575(17) 1 calc PR A 2 H28E H 0.3447 0.1312 0.4382 0.059 Uiso 0.5575(17) 1 calc PR A 2 H28F H 0.4060 0.1129 0.5618 0.059 Uiso 0.5575(17) 1 calc PR A 2 C29' C 0.3320(4) 0.2374(3) 0.5726(5) 0.0371(9) Uani 0.5575(17) 1 d PDU A 2 H29D H 0.3450 0.2838 0.5901 0.056 Uiso 0.5575(17) 1 calc PR A 2 H29E H 0.3231 0.2134 0.6432 0.056 Uiso 0.5575(17) 1 calc PR A 2 H29F H 0.2625 0.2325 0.5198 0.056 Uiso 0.5575(17) 1 calc PR A 2 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 0.01189(15) 0.0146(2) 0.0087(2) 0.00051(16) -0.00207(12) 0.00407(15) F1 0.0246(7) 0.041(6) 0.0294(9) 0.005(5) 0.0023(6) 0.010(2) N2 0.0163(9) 0.0177(8) 0.015(2) -0.0003(19) 0.004(3) 0.0004(6) C3 0.0144(9) 0.0198(12) 0.020(3) -0.004(2) 0.004(4) -0.0002(10) C5 0.020(3) 0.026(2) 0.024(3) -0.0043(19) 0.0099(16) 0.0065(19) C2 0.020(5) 0.0241(12) 0.016(3) -0.0059(18) 0.001(3) 0.0003(15) C1 0.013(5) 0.0259(12) 0.017(2) -0.0011(12) 0.002(2) -0.001(2) C4 0.029(4) 0.033(2) 0.0169(18) -0.0013(14) 0.005(3) 0.006(3) N1 0.032(5) 0.0191(9) 0.0172(14) 0.0024(9) 0.0065(18) -0.0003(11) C6 0.028(3) 0.0210(11) 0.0128(9) 0.0021(9) 0.006(2) -0.0007(14) C7 0.026(2) 0.0231(12) 0.0185(9) 0.0015(10) 0.009(3) -0.0007(16) C8 0.030(3) 0.0237(12) 0.0234(14) 0.0040(12) 0.009(3) -0.0045(17) C9 0.038(4) 0.0215(12) 0.021(2) 0.0054(15) 0.005(3) -0.0014(16) C10 0.033(3) 0.0252(15) 0.020(2) 0.0061(15) -0.002(3) -0.0014(17) C11 0.033(3) 0.0237(13) 0.0160(14) 0.0035(11) -0.001(2) -0.0031(17) C12 0.028(3) 0.0278(11) 0.026(3) 0.0028(18) 0.008(2) 0.000(2) C13 0.030(7) 0.063(3) 0.043(7) -0.017(6) 0.009(5) 0.005(6) C14 0.029(3) 0.036(3) 0.031(6) 0.002(2) 0.003(2) -0.002(2) C15 0.031(3) 0.022(2) 0.025(3) 0.002(2) -0.003(2) -0.003(3) C16 0.0322(17) 0.029(3) 0.037(5) 0.004(4) 0.002(3) -0.0035(16) C17 0.044(4) 0.036(3) 0.030(3) -0.002(2) -0.010(2) -0.002(3) C18 0.0170(16) 0.0183(10) 0.0176(14) -0.0008(10) 0.0048(13) 0.0052(11) C19 0.0243(16) 0.0232(13) 0.0262(17) 0.0017(12) -0.0013(10) 0.0022(12) C20 0.0357(19) 0.0315(18) 0.0270(17) 0.0021(14) -0.0098(12) 0.0066(15) C21 0.053(2) 0.0277(17) 0.0246(16) 0.0076(13) -0.0046(15) 0.0065(17) C22 0.045(2) 0.0216(15) 0.0268(14) 0.0065(12) 0.0073(17) -0.0008(16) C23 0.025(2) 0.0186(12) 0.0225(11) 0.0005(9) 0.0048(14) 0.0016(15) C24 0.0182(14) 0.0340(16) 0.0369(17) 0.0047(15) -0.0050(13) -0.0014(12) C25 0.0228(15) 0.061(2) 0.0414(19) -0.0007(18) 0.0010(16) 0.000(2) C26 0.0259(16) 0.040(2) 0.057(2) -0.0102(17) -0.0064(16) -0.0027(14) C27 0.024(3) 0.0231(13) 0.026(3) 0.0021(17) 0.0036(16) -0.0027(19) C28 0.044(4) 0.0276(15) 0.046(4) -0.007(2) 0.007(2) -0.010(2) C29 0.028(2) 0.0380(19) 0.047(3) -0.002(2) 0.0125(17) -0.004(2) Pb1' 0.0553(4) 0.0245(3) 0.0256(3) 0.0063(2) 0.0192(2) 0.0100(2) F1' 0.0246(7) 0.041(6) 0.0294(9) 0.005(5) 0.0023(6) 0.010(2) N2' 0.0163(9) 0.0177(8) 0.015(2) -0.0003(19) 0.004(3) 0.0004(6) C3' 0.0144(9) 0.0198(12) 0.020(3) -0.004(2) 0.004(4) -0.0002(10) C5' 0.020(3) 0.026(2) 0.024(3) -0.0043(19) 0.0099(16) 0.0065(19) C2' 0.020(5) 0.0241(12) 0.016(3) -0.0059(18) 0.001(3) 0.0003(15) C1' 0.013(5) 0.0259(12) 0.017(2) -0.0011(12) 0.002(2) -0.001(2) C4' 0.029(4) 0.033(2) 0.0169(18) -0.0013(14) 0.005(3) 0.006(3) N1' 0.032(5) 0.0191(9) 0.0172(14) 0.0024(9) 0.0065(18) -0.0003(11) C6' 0.028(3) 0.0210(11) 0.0128(9) 0.0021(9) 0.006(2) -0.0007(14) C7' 0.026(2) 0.0231(12) 0.0185(9) 0.0015(10) 0.009(3) -0.0007(16) C8' 0.030(3) 0.0237(12) 0.0234(14) 0.0040(12) 0.009(3) -0.0045(17) C9' 0.038(4) 0.0215(12) 0.021(2) 0.0054(15) 0.005(3) -0.0014(16) C10' 0.033(3) 0.0252(15) 0.020(2) 0.0061(15) -0.002(3) -0.0014(17) C11' 0.033(3) 0.0237(13) 0.0160(14) 0.0035(11) -0.001(2) -0.0031(17) C12' 0.028(3) 0.0278(11) 0.026(3) 0.0028(18) 0.008(2) 0.000(2) C13' 0.030(7) 0.063(3) 0.043(7) -0.017(6) 0.009(5) 0.005(6) C14' 0.029(3) 0.036(3) 0.031(6) 0.002(2) 0.003(2) -0.002(2) C15' 0.031(3) 0.022(2) 0.025(3) 0.002(2) -0.003(2) -0.003(3) C16' 0.0322(17) 0.029(3) 0.037(5) 0.004(4) 0.002(3) -0.0035(16) C17' 0.044(4) 0.036(3) 0.030(3) -0.002(2) -0.010(2) -0.002(3) C18' 0.0170(16) 0.0183(10) 0.0176(14) -0.0008(10) 0.0048(13) 0.0052(11) C19' 0.0243(16) 0.0232(13) 0.0262(17) 0.0017(12) -0.0013(10) 0.0022(12) C20' 0.0357(19) 0.0315(18) 0.0270(17) 0.0021(14) -0.0098(12) 0.0066(15) C21' 0.053(2) 0.0277(17) 0.0246(16) 0.0076(13) -0.0046(15) 0.0065(17) C22' 0.045(2) 0.0216(15) 0.0268(14) 0.0065(12) 0.0073(17) -0.0008(16) C23' 0.025(2) 0.0186(12) 0.0225(11) 0.0005(9) 0.0048(14) 0.0016(15) C24' 0.0182(14) 0.0340(16) 0.0369(17) 0.0047(15) -0.0050(13) -0.0014(12) C25' 0.0228(15) 0.061(2) 0.0414(19) -0.0007(18) 0.0010(16) 0.000(2) C26' 0.0259(16) 0.040(2) 0.057(2) -0.0102(17) -0.0064(16) -0.0027(14) C27' 0.024(3) 0.0231(13) 0.026(3) 0.0021(17) 0.0036(16) -0.0027(19) C28' 0.044(4) 0.0276(15) 0.046(4) -0.007(2) 0.007(2) -0.010(2) C29' 0.028(2) 0.0380(19) 0.047(3) -0.002(2) 0.0125(17) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 F1 2.085(11) . ? Pb1 N2 2.332(14) . ? Pb1 N1 2.352(18) . ? N2 C3 1.324(9) . ? N2 C18 1.427(9) . ? C3 C2 1.398(9) . ? C3 C5 1.516(10) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C2 C1 1.405(10) . ? C2 H2 0.9500 . ? C1 N1 1.326(10) . ? C1 C4 1.512(10) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? N1 C6 1.430(9) . ? C6 C7 1.3900 . ? C6 C11 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.548(9) . ? C8 C9 1.3900 . ? C8 H8 0.9500 . ? C9 C10 1.3900 . ? C9 H9 0.9500 . ? C10 C11 1.3900 . ? C10 H10 0.9500 . ? C11 C15 1.551(9) . ? C12 C14 1.532(11) . ? C12 C13 1.533(11) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.522(10) . ? C15 C17 1.542(11) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C19 C24 1.5515 . ? C20 C21 1.3900 . ? C20 H20 0.9500 . ? C21 C22 1.3900 . ? C21 H21 0.9500 . ? C22 C23 1.3900 . ? C22 H22 0.9500 . ? C23 C27 1.549(6) . ? C24 C26 1.512(7) . ? C24 C25 1.538(7) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.525(9) . ? C27 C28 1.529(9) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? Pb1' F1' 2.089(8) . ? Pb1' N2' 2.263(11) . ? Pb1' N1' 2.282(15) . ? N2' C3' 1.327(7) . ? N2' C18' 1.435(7) . ? C3' C2' 1.406(8) . ? C3' C5' 1.517(8) . ? C5' H5'1 0.9800 . ? C5' H5'2 0.9800 . ? C5' H5'3 0.9800 . ? C2' C1' 1.403(8) . ? C2' H2' 0.9500 . ? C1' N1' 1.328(8) . ? C1' C4' 1.517(8) . ? C4' H4'1 0.9800 . ? C4' H4'2 0.9800 . ? C4' H4'3 0.9800 . ? N1' C6' 1.434(7) . ? C6' C7' 1.3900 . ? C6' C11' 1.3900 . ? C7' C8' 1.3900 . ? C7' C12' 1.551(8) . ? C8' C9' 1.3900 . ? C8' H8' 0.9500 . ? C9' C10' 1.3900 . ? C9' H9' 0.9500 . ? C10' C11' 1.3900 . ? C10' H10' 0.9500 . ? C11' C15' 1.549(7) . ? C12' C14' 1.531(9) . ? C12' C13' 1.535(9) . ? C12' H12' 1.0000 . ? C13' H13D 0.9800 . ? C13' H13E 0.9800 . ? C13' H13F 0.9800 . ? C14' H14D 0.9800 . ? C14' H14E 0.9800 . ? C14' H14F 0.9800 . ? C15' C16' 1.533(8) . ? C15' C17' 1.543(8) . ? C15' H15' 1.0000 . ? C16' H16D 0.9800 . ? C16' H16E 0.9800 . ? C16' H16F 0.9800 . ? C17' H17D 0.9800 . ? C17' H17E 0.9800 . ? C17' H17F 0.9800 . ? C18' C19' 1.3900 . ? C18' C23' 1.3900 . ? C19' C20' 1.3900 . ? C19' C24' 1.5594 . ? C20' C21' 1.3900 . ? C20' H20' 0.9500 . ? C21' C22' 1.3900 . ? C21' H21' 0.9500 . ? C22' C23' 1.3900 . ? C22' H22' 0.9500 . ? C23' C27' 1.545(5) . ? C24' C26' 1.522(5) . ? C24' C25' 1.543(6) . ? C24' H24' 1.0000 . ? C25' H25D 0.9800 . ? C25' H25E 0.9800 . ? C25' H25F 0.9800 . ? C26' H26D 0.9800 . ? C26' H26E 0.9800 . ? C26' H26F 0.9800 . ? C27' C29' 1.534(7) . ? C27' C28' 1.545(7) . ? C27' H27' 1.0000 . ? C28' H28D 0.9800 . ? C28' H28E 0.9800 . ? C28' H28F 0.9800 . ? C29' H29D 0.9800 . ? C29' H29E 0.9800 . ? C29' H29F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Pb1 N2 92.9(9) . . ? F1 Pb1 N1 86.2(15) . . ? N2 Pb1 N1 80.1(4) . . ? C3 N2 C18 120.8(11) . . ? C3 N2 Pb1 129.3(7) . . ? C18 N2 Pb1 109.6(7) . . ? N2 C3 C2 125.3(11) . . ? N2 C3 C5 118.0(9) . . ? C2 C3 C5 116.6(9) . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C2 C1 129.4(11) . . ? C3 C2 H2 115.3 . . ? C1 C2 H2 115.3 . . ? N1 C1 C2 125.5(11) . . ? N1 C1 C4 119.5(11) . . ? C2 C1 C4 114.7(10) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 N1 C6 122.6(15) . . ? C1 N1 Pb1 127.6(11) . . ? C6 N1 Pb1 109.4(15) . . ? C7 C6 C11 120.0 . . ? C7 C6 N1 118.6(12) . . ? C11 C6 N1 121.4(12) . . ? C8 C7 C6 120.0 . . ? C8 C7 C12 119.6(10) . . ? C6 C7 C12 120.4(10) . . ? C7 C8 C9 120.0 . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C6 120.0 . . ? C10 C11 C15 116.8(10) . . ? C6 C11 C15 122.9(10) . . ? C14 C12 C13 109.3(16) . . ? C14 C12 C7 114.5(15) . . ? C13 C12 C7 112.8(15) . . ? C14 C12 H12 106.5 . . ? C13 C12 H12 106.6 . . ? C7 C12 H12 106.5 . . ? C12 C13 H13A 109.4 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.4 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C17 110.9(9) . . ? C16 C15 C11 111.9(12) . . ? C17 C15 C11 111.0(12) . . ? C16 C15 H15 107.6 . . ? C17 C15 H15 107.6 . . ? C11 C15 H15 107.6 . . ? C15 C16 H16A 109.4 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.0 . . ? C19 C18 N2 119.0(10) . . ? C23 C18 N2 120.8(10) . . ? C20 C19 C18 120.0 . . ? C20 C19 C24 118.7 . . ? C18 C19 C24 121.2 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 C27 118.0(3) . . ? C18 C23 C27 121.9(3) . . ? C26 C24 C25 110.5(4) . . ? C26 C24 C19 111.4(3) . . ? C25 C24 C19 113.4(3) . . ? C26 C24 H24 107.1 . . ? C25 C24 H24 107.1 . . ? C19 C24 H24 107.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 110.1(7) . . ? C29 C27 C23 112.7(5) . . ? C28 C27 C23 112.4(5) . . ? C29 C27 H27 107.1 . . ? C28 C27 H27 107.1 . . ? C23 C27 H27 107.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? F1' Pb1' N2' 88.3(7) . . ? F1' Pb1' N1' 93.1(11) . . ? N2' Pb1' N1' 84.2(4) . . ? C3' N2' C18' 119.9(8) . . ? C3' N2' Pb1' 125.7(5) . . ? C18' N2' Pb1' 113.8(5) . . ? N2' C3' C2' 125.4(8) . . ? N2' C3' C5' 119.7(7) . . ? C2' C3' C5' 114.9(7) . . ? C3' C5' H5'1 109.5 . . ? C3' C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? C3' C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? C1' C2' C3' 131.7(9) . . ? C1' C2' H2' 114.1 . . ? C3' C2' H2' 114.1 . . ? N1' C1' C2' 123.7(9) . . ? N1' C1' C4' 120.5(8) . . ? C2' C1' C4' 115.7(8) . . ? C1' C4' H4'1 109.5 . . ? C1' C4' H4'2 109.5 . . ? H4'1 C4' H4'2 109.5 . . ? C1' C4' H4'3 109.5 . . ? H4'1 C4' H4'3 109.5 . . ? H4'2 C4' H4'3 109.5 . . ? C1' N1' C6' 121.2(12) . . ? C1' N1' Pb1' 126.8(8) . . ? C6' N1' Pb1' 111.9(12) . . ? C7' C6' C11' 120.0 . . ? C7' C6' N1' 118.9(9) . . ? C11' C6' N1' 120.8(9) . . ? C6' C7' C8' 120.0 . . ? C6' C7' C12' 120.6(8) . . ? C8' C7' C12' 119.3(8) . . ? C7' C8' C9' 120.0 . . ? C7' C8' H8' 120.0 . . ? C9' C8' H8' 120.0 . . ? C10' C9' C8' 120.0 . . ? C10' C9' H9' 120.0 . . ? C8' C9' H9' 120.0 . . ? C11' C10' C9' 120.0 . . ? C11' C10' H10' 120.0 . . ? C9' C10' H10' 120.0 . . ? C10' C11' C6' 120.0 . . ? C10' C11' C15' 118.2(8) . . ? C6' C11' C15' 121.8(8) . . ? C14' C12' C13' 109.9(12) . . ? C14' C12' C7' 113.8(13) . . ? C13' C12' C7' 110.5(11) . . ? C14' C12' H12' 107.5 . . ? C13' C12' H12' 107.4 . . ? C7' C12' H12' 107.5 . . ? C12' C13' H13D 109.5 . . ? C12' C13' H13E 109.4 . . ? H13D C13' H13E 109.5 . . ? C12' C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? C12' C14' H14D 109.5 . . ? C12' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C12' C14' H14F 109.4 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C16' C15' C17' 109.6(7) . . ? C16' C15' C11' 111.2(9) . . ? C17' C15' C11' 112.3(10) . . ? C16' C15' H15' 107.9 . . ? C17' C15' H15' 107.9 . . ? C11' C15' H15' 107.9 . . ? C15' C16' H16D 109.5 . . ? C15' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C15' C17' H17D 109.5 . . ? C15' C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C15' C17' H17F 109.4 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C19' C18' C23' 120.0 . . ? C19' C18' N2' 118.9(8) . . ? C23' C18' N2' 121.0(8) . . ? C20' C19' C18' 120.0 . . ? C20' C19' C24' 119.3 . . ? C18' C19' C24' 120.6 . . ? C19' C20' C21' 120.0 . . ? C19' C20' H20' 120.0 . . ? C21' C20' H20' 120.0 . . ? C22' C21' C20' 120.0 . . ? C22' C21' H21' 120.0 . . ? C20' C21' H21' 120.0 . . ? C21' C22' C23' 120.0 . . ? C21' C22' H22' 120.0 . . ? C23' C22' H22' 120.0 . . ? C22' C23' C18' 120.0 . . ? C22' C23' C27' 118.5(3) . . ? C18' C23' C27' 121.5(3) . . ? C26' C24' C25' 109.0(3) . . ? C26' C24' C19' 113.7(2) . . ? C25' C24' C19' 111.9(3) . . ? C26' C24' H24' 107.3 . . ? C25' C24' H24' 107.3 . . ? C19' C24' H24' 107.3 . . ? C24' C25' H25D 109.5 . . ? C24' C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C24' C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C24' C26' H26D 109.5 . . ? C24' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C24' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C29' C27' C28' 109.5(5) . . ? C29' C27' C23' 110.9(4) . . ? C28' C27' C23' 112.3(4) . . ? C29' C27' H27' 108.0 . . ? C28' C27' H27' 108.0 . . ? C23' C27' H27' 108.0 . . ? C27' C28' H28D 109.5 . . ? C27' C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? C27' C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? C27' C29' H29D 109.5 . . ? C27' C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? C27' C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 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 F1 Pb1 N2 C3 77(3) . . . . ? N1 Pb1 N2 C3 -9(3) . . . . ? F1 Pb1 N2 C18 -110.4(16) . . . . ? N1 Pb1 N2 C18 164.0(16) . . . . ? C18 N2 C3 C2 -174(2) . . . . ? Pb1 N2 C3 C2 -1(5) . . . . ? C18 N2 C3 C5 4(4) . . . . ? Pb1 N2 C3 C5 176.7(15) . . . . ? N2 C3 C2 C1 11(5) . . . . ? C5 C3 C2 C1 -167(2) . . . . ? C3 C2 C1 N1 -2(4) . . . . ? C3 C2 C1 C4 172(2) . . . . ? C2 C1 N1 C6 172(2) . . . . ? C4 C1 N1 C6 -1(4) . . . . ? C2 C1 N1 Pb1 -16(4) . . . . ? C4 C1 N1 Pb1 171.1(17) . . . . ? F1 Pb1 N1 C1 -76(3) . . . . ? N2 Pb1 N1 C1 17(3) . . . . ? F1 Pb1 N1 C6 96.2(18) . . . . ? N2 Pb1 N1 C6 -170.2(19) . . . . ? C1 N1 C6 C7 -105(3) . . . . ? Pb1 N1 C6 C7 81(2) . . . . ? C1 N1 C6 C11 77(4) . . . . ? Pb1 N1 C6 C11 -96(2) . . . . ? C11 C6 C7 C8 0.0 . . . . ? N1 C6 C7 C8 -178(3) . . . . ? C11 C6 C7 C12 -179(3) . . . . ? N1 C6 C7 C12 4(3) . . . . ? C6 C7 C8 C9 0.0 . . . . ? C12 C7 C8 C9 179(3) . . . . ? C7 C8 C9 C10 0.0 . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C6 0.0 . . . . ? C9 C10 C11 C15 174(2) . . . . ? C7 C6 C11 C10 0.0 . . . . ? N1 C6 C11 C10 178(3) . . . . ? C7 C6 C11 C15 -174(2) . . . . ? N1 C6 C11 C15 4(3) . . . . ? C8 C7 C12 C14 27(4) . . . . ? C6 C7 C12 C14 -155(4) . . . . ? C8 C7 C12 C13 -99(4) . . . . ? C6 C7 C12 C13 80(4) . . . . ? C10 C11 C15 C16 -64(2) . . . . ? C6 C11 C15 C16 110(2) . . . . ? C10 C11 C15 C17 60.5(19) . . . . ? C6 C11 C15 C17 -125.5(18) . . . . ? C3 N2 C18 C19 89(2) . . . . ? Pb1 N2 C18 C19 -84.9(11) . . . . ? C3 N2 C18 C23 -97(2) . . . . ? Pb1 N2 C18 C23 89.3(11) . . . . ? C23 C18 C19 C20 0.0 . . . . ? N2 C18 C19 C20 174.3(7) . . . . ? C23 C18 C19 C24 -179.5 . . . . ? N2 C18 C19 C24 -5.2(7) . . . . ? C18 C19 C20 C21 0.0 . . . . ? C24 C19 C20 C21 179.5 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C18 0.0 . . . . ? C21 C22 C23 C27 176.0(5) . . . . ? C19 C18 C23 C22 0.0 . . . . ? N2 C18 C23 C22 -174.2(7) . . . . ? C19 C18 C23 C27 -175.8(5) . . . . ? N2 C18 C23 C27 10.0(8) . . . . ? C20 C19 C24 C26 -70.5(4) . . . . ? C18 C19 C24 C26 109.1(4) . . . . ? C20 C19 C24 C25 54.9(4) . . . . ? C18 C19 C24 C25 -125.5(4) . . . . ? C22 C23 C27 C29 66.9(7) . . . . ? C18 C23 C27 C29 -117.3(5) . . . . ? C22 C23 C27 C28 -58.3(7) . . . . ? C18 C23 C27 C28 117.5(6) . . . . ? F1' Pb1' N2' C3' 78(2) . . . . ? N1' Pb1' N2' C3' -15(2) . . . . ? F1' Pb1' N2' C18' -93.3(13) . . . . ? N1' Pb1' N2' C18' 173.4(13) . . . . ? C18' N2' C3' C2' -178.9(18) . . . . ? Pb1' N2' C3' C2' 10(3) . . . . ? C18' N2' C3' C5' 1(3) . . . . ? Pb1' N2' C3' C5' -170.0(12) . . . . ? N2' C3' C2' C1' 4(4) . . . . ? C5' C3' C2' C1' -175.5(17) . . . . ? C3' C2' C1' N1' -6(3) . . . . ? C3' C2' C1' C4' 177.7(19) . . . . ? C2' C1' N1' C6' 176.5(15) . . . . ? C4' C1' N1' C6' -7(3) . . . . ? C2' C1' N1' Pb1' -8(3) . . . . ? C4' C1' N1' Pb1' 168.7(13) . . . . ? F1' Pb1' N1' C1' -74(2) . . . . ? N2' Pb1' N1' C1' 14(2) . . . . ? F1' Pb1' N1' C6' 102.3(14) . . . . ? N2' Pb1' N1' C6' -169.7(15) . . . . ? C1' N1' C6' C7' -99(2) . . . . ? Pb1' N1' C6' C7' 84.3(18) . . . . ? C1' N1' C6' C11' 86(3) . . . . ? Pb1' N1' C6' C11' -89.9(18) . . . . ? C11' C6' C7' C8' 0.0 . . . . ? N1' C6' C7' C8' -174(2) . . . . ? C11' C6' C7' C12' 177(2) . . . . ? N1' C6' C7' C12' 3(2) . . . . ? C6' C7' C8' C9' 0.0 . . . . ? C12' C7' C8' C9' -177(2) . . . . ? C7' C8' C9' C10' 0.0 . . . . ? C8' C9' C10' C11' 0.0 . . . . ? C9' C10' C11' C6' 0.0 . . . . ? C9' C10' C11' C15' -178.6(17) . . . . ? C7' C6' C11' C10' 0.0 . . . . ? N1' C6' C11' C10' 174(2) . . . . ? C7' C6' C11' C15' 178.5(18) . . . . ? N1' C6' C11' C15' -7(2) . . . . ? C6' C7' C12' C14' -154(3) . . . . ? C8' C7' C12' C14' 23(3) . . . . ? C6' C7' C12' C13' 82(3) . . . . ? C8' C7' C12' C13' -101(3) . . . . ? C10' C11' C15' C16' -62.0(15) . . . . ? C6' C11' C15' C16' 119.4(15) . . . . ? C10' C11' C15' C17' 61.1(15) . . . . ? C6' C11' C15' C17' -117.4(14) . . . . ? C3' N2' C18' C19' 102.4(18) . . . . ? Pb1' N2' C18' C19' -85.7(10) . . . . ? C3' N2' C18' C23' -81.0(19) . . . . ? Pb1' N2' C18' C23' 90.9(9) . . . . ? C23' C18' C19' C20' 0.0 . . . . ? N2' C18' C19' C20' 176.7(6) . . . . ? C23' C18' C19' C24' -178.0 . . . . ? N2' C18' C19' C24' -1.4(6) . . . . ? C18' C19' C20' C21' 0.0 . . . . ? C24' C19' C20' C21' 178.1 . . . . ? C19' C20' C21' C22' 0.0 . . . . ? C20' C21' C22' C23' 0.0 . . . . ? C21' C22' C23' C18' 0.0 . . . . ? C21' C22' C23' C27' 179.3(4) . . . . ? C19' C18' C23' C22' 0.0 . . . . ? N2' C18' C23' C22' -176.6(6) . . . . ? C19' C18' C23' C27' -179.3(4) . . . . ? N2' C18' C23' C27' 4.2(6) . . . . ? C20' C19' C24' C26' -20.7(3) . . . . ? C18' C19' C24' C26' 157.4(3) . . . . ? C20' C19' C24' C25' 103.3(3) . . . . ? C18' C19' C24' C25' -78.7(3) . . . . ? C22' C23' C27' C29' 68.6(5) . . . . ? C18' C23' C27' C29' -112.1(4) . . . . ? C22' C23' C27' C28' -54.3(5) . . . . ? C18' C23' C27' C28' 125.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.62 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.121 _refine_diff_density_min -1.411 _refine_diff_density_rms 0.085 # Attachment '- 6.cif' data_sq _database_code_depnum_ccdc_archive 'CCDC 808035' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H92 F6 N4 O2 Pb' _chemical_formula_weight 1390.71 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7060(15) _cell_length_b 18.9000(18) _cell_length_c 26.336(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.0930(10) _cell_angle_gamma 90.00 _cell_volume 7472.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9527 _cell_measurement_theta_min 2.547 _cell_measurement_theta_max 27.37 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2864 _exptl_absorpt_coefficient_mu 2.316 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6482 _exptl_absorpt_correction_T_max 0.7921 _exptl_absorpt_process_details SADABS-2008/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOTEC Mo micro source' _diffrn_radiation_monochromator 'INCOAZEC quazer mirror optics' _diffrn_measurement_device_type 'Bruker Smart ApexII with D8-Goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 166483 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 26.02 _reflns_number_total 14728 _reflns_number_gt 13062 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0' _computing_cell_refinement 'SAINT V7.68A' _computing_data_reduction 'SAINT V7.68A' _computing_structure_solution 'SHELXS in SHELXTL Version 2008/4' _computing_structure_refinement 'SHELXL in SHELXTL Version 2008/4' _computing_molecular_graphics 'XSHELL vers. 4.01' _computing_publication_material 'XSHELL vers. 4.01' _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. ; 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 -0.014 0.000 0.000 624 146 ' ' 2 -0.012 0.500 0.500 624 146 ' ' _platon_squeeze_details 'Highly disordered non-coordinating THF molecules' _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^)+(0.0280P)^2^+3.5678P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14728 _refine_ls_number_parameters 804 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0260 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0522 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.245822(5) 0.258838(4) 0.252838(3) 0.01744(3) Uani 1 1 d . . . O1 O 0.27655(9) 0.36927(7) 0.24449(5) 0.0190(3) Uani 1 1 d . . . O2 O 0.23810(9) 0.25058(7) 0.16939(6) 0.0191(3) Uani 1 1 d . . . N1 N 0.08923(10) 0.31838(8) 0.22837(6) 0.0175(3) Uani 1 1 d . . . N2 N 0.08928(10) 0.52686(8) 0.15888(6) 0.0167(3) Uani 1 1 d . . . N3 N 0.40790(10) 0.21663(9) 0.25814(7) 0.0188(3) Uani 1 1 d . . . N4 N 0.47944(11) 0.26023(8) 0.12161(7) 0.0186(3) Uani 1 1 d . . . F1 F 0.37795(8) 0.48446(6) 0.28923(5) 0.0278(3) Uani 1 1 d . . . F2 F 0.30589(8) 0.49400(6) 0.20660(5) 0.0240(3) Uani 1 1 d . . . F3 F 0.26328(8) 0.55269(6) 0.26517(5) 0.0257(3) Uani 1 1 d . . . F4 F 0.27366(9) 0.15797(7) 0.06083(5) 0.0356(3) Uani 1 1 d . . . F5 F 0.24399(8) 0.26778(7) 0.06974(5) 0.0303(3) Uani 1 1 d . . . F6 F 0.14882(8) 0.18828(7) 0.07314(5) 0.0304(3) Uani 1 1 d . . . C1 C 0.23661(13) 0.42654(10) 0.26070(8) 0.0175(4) Uani 1 1 d . . . C2 C 0.29566(13) 0.48945(10) 0.25538(8) 0.0202(4) Uani 1 1 d . . . C3 C 0.24009(13) 0.42348(11) 0.32037(8) 0.0213(4) Uani 1 1 d . . . C4 C 0.29866(14) 0.37725(11) 0.35404(8) 0.0250(5) Uani 1 1 d . . . H4 H 0.3365 0.3486 0.3404 0.030 Uiso 1 1 calc R . . C5 C 0.30325(17) 0.37186(13) 0.40746(9) 0.0362(6) Uani 1 1 d . . . H5 H 0.3436 0.3395 0.4298 0.043 Uiso 1 1 calc R . . C6 C 0.24914(18) 0.41360(15) 0.42816(10) 0.0433(6) Uani 1 1 d . . . H6 H 0.2510 0.4093 0.4644 0.052 Uiso 1 1 calc R . . C7 C 0.19245(17) 0.46155(14) 0.39565(9) 0.0398(6) Uani 1 1 d . . . H7 H 0.1561 0.4911 0.4099 0.048 Uiso 1 1 calc R . . C8 C 0.18786(15) 0.46709(12) 0.34234(8) 0.0281(5) Uani 1 1 d . . . H8 H 0.1489 0.5008 0.3205 0.034 Uiso 1 1 calc R . . C9 C 0.13841(12) 0.44190(10) 0.22668(7) 0.0152(4) Uani 1 1 d . . . H9 H 0.1207 0.4841 0.2442 0.018 Uiso 1 1 calc R . . C10 C 0.07205(12) 0.38429(10) 0.23097(7) 0.0168(4) Uani 1 1 d . . . C11 C -0.01295(13) 0.41297(11) 0.23820(8) 0.0225(4) Uani 1 1 d . . . H11A H -0.0570 0.3749 0.2329 0.034 Uiso 1 1 calc R . . H11B H -0.0360 0.4506 0.2122 0.034 Uiso 1 1 calc R . . H11C H -0.0012 0.4321 0.2742 0.034 Uiso 1 1 calc R . . C12 C 0.02850(13) 0.26382(10) 0.23492(8) 0.0196(4) Uani 1 1 d . . . C13 C 0.02401(14) 0.24589(11) 0.28603(9) 0.0225(4) Uani 1 1 d . . . C14 C -0.02869(14) 0.18799(11) 0.29025(9) 0.0276(5) Uani 1 1 d . . . H14 H -0.0329 0.1749 0.3243 0.033 Uiso 1 1 calc R . . C15 C -0.07478(14) 0.14935(11) 0.24641(9) 0.0293(5) Uani 1 1 d . . . H15 H -0.1107 0.1105 0.2504 0.035 Uiso 1 1 calc R . . C16 C -0.06866(14) 0.16704(11) 0.19681(9) 0.0263(5) Uani 1 1 d . . . H16 H -0.1004 0.1399 0.1669 0.032 Uiso 1 1 calc R . . C17 C -0.01694(13) 0.22389(11) 0.18974(9) 0.0220(4) Uani 1 1 d . . . C18 C -0.01320(15) 0.24420(11) 0.13462(9) 0.0233(5) Uani 1 1 d . . . H18 H 0.0484 0.2612 0.1378 0.028 Uiso 1 1 calc R . . C19 C -0.03460(15) 0.18340(12) 0.09449(9) 0.0313(5) Uani 1 1 d . . . H19A H 0.0029 0.1425 0.1093 0.047 Uiso 1 1 calc R . . H19B H -0.0230 0.1985 0.0615 0.047 Uiso 1 1 calc R . . H19C H -0.0975 0.1703 0.0870 0.047 Uiso 1 1 calc R . . C20 C -0.07805(15) 0.30510(12) 0.11277(9) 0.0285(5) Uani 1 1 d . . . H20A H -0.1393 0.2888 0.1075 0.043 Uiso 1 1 calc R . . H20B H -0.0711 0.3210 0.0788 0.043 Uiso 1 1 calc R . . H20C H -0.0652 0.3445 0.1381 0.043 Uiso 1 1 calc R . . C21 C 0.07327(14) 0.28504(12) 0.33637(8) 0.0254(5) Uani 1 1 d . . . H21 H 0.1090 0.3238 0.3267 0.031 Uiso 1 1 calc R . . C22 C 0.13750(16) 0.23541(13) 0.37598(9) 0.0332(5) Uani 1 1 d . . . H22A H 0.1037 0.1969 0.3858 0.050 Uiso 1 1 calc R . . H22B H 0.1690 0.2621 0.4079 0.050 Uiso 1 1 calc R . . H22C H 0.1807 0.2157 0.3595 0.050 Uiso 1 1 calc R . . C23 C 0.00802(16) 0.31846(13) 0.36310(10) 0.0345(5) Uani 1 1 d . . . H23A H -0.0337 0.3494 0.3377 0.052 Uiso 1 1 calc R . . H23B H 0.0414 0.3463 0.3939 0.052 Uiso 1 1 calc R . . H23C H -0.0252 0.2810 0.3747 0.052 Uiso 1 1 calc R . . C24 C 0.12137(12) 0.46491(10) 0.16830(8) 0.0163(4) Uani 1 1 d . . . C25 C 0.13991(13) 0.41406(10) 0.12912(8) 0.0209(4) Uani 1 1 d . . . H25A H 0.0948 0.3766 0.1213 0.031 Uiso 1 1 calc R . . H25B H 0.1991 0.3931 0.1442 0.031 Uiso 1 1 calc R . . H25C H 0.1380 0.4393 0.0963 0.031 Uiso 1 1 calc R . . C26 C 0.06245(13) 0.56144(10) 0.10827(7) 0.0176(4) Uani 1 1 d . . . C27 C 0.11649(13) 0.61580(11) 0.09797(8) 0.0199(4) Uani 1 1 d . . . C28 C 0.08166(14) 0.65912(11) 0.05380(8) 0.0242(4) Uani 1 1 d . . . H28 H 0.1174 0.6960 0.0464 0.029 Uiso 1 1 calc R . . C29 C -0.00354(14) 0.64944(12) 0.02064(8) 0.0266(5) Uani 1 1 d . . . H29 H -0.0266 0.6801 -0.0088 0.032 Uiso 1 1 calc R . . C30 C -0.05528(14) 0.59487(11) 0.03041(8) 0.0243(4) Uani 1 1 d . . . H30 H -0.1133 0.5876 0.0069 0.029 Uiso 1 1 calc R . . C31 C -0.02397(13) 0.55030(10) 0.07414(8) 0.0195(4) Uani 1 1 d . . . C32 C -0.08435(13) 0.49451(11) 0.08688(8) 0.0215(4) Uani 1 1 d . . . H32 H -0.0454 0.4562 0.1076 0.026 Uiso 1 1 calc R . . C33 C -0.14726(14) 0.46066(12) 0.03750(9) 0.0302(5) Uani 1 1 d . . . H33A H -0.1900 0.4961 0.0180 0.045 Uiso 1 1 calc R . . H33B H -0.1794 0.4216 0.0481 0.045 Uiso 1 1 calc R . . H33C H -0.1128 0.4426 0.0147 0.045 Uiso 1 1 calc R . . C34 C -0.13606(14) 0.52641(11) 0.12248(9) 0.0259(5) Uani 1 1 d . . . H34A H -0.0941 0.5468 0.1543 0.039 Uiso 1 1 calc R . . H34B H -0.1711 0.4893 0.1330 0.039 Uiso 1 1 calc R . . H34C H -0.1761 0.5635 0.1030 0.039 Uiso 1 1 calc R . . C35 C 0.21097(14) 0.62555(11) 0.13307(8) 0.0245(4) Uani 1 1 d . . . H35 H 0.2154 0.6028 0.1680 0.029 Uiso 1 1 calc R . . C36 C 0.23868(17) 0.70266(13) 0.14379(10) 0.0393(6) Uani 1 1 d . . . H36A H 0.2397 0.7254 0.1105 0.059 Uiso 1 1 calc R . . H36B H 0.2982 0.7050 0.1694 0.059 Uiso 1 1 calc R . . H36C H 0.1960 0.7272 0.1583 0.059 Uiso 1 1 calc R . . C37 C 0.27577(15) 0.58698(13) 0.10907(10) 0.0342(5) Uani 1 1 d . . . H37A H 0.2597 0.5368 0.1045 0.051 Uiso 1 1 calc R . . H37B H 0.3365 0.5917 0.1329 0.051 Uiso 1 1 calc R . . H37C H 0.2725 0.6078 0.0745 0.051 Uiso 1 1 calc R . . C38 C 0.27784(13) 0.19684(10) 0.14898(8) 0.0196(4) Uani 1 1 d . . . C39 C 0.23643(14) 0.20268(12) 0.08805(9) 0.0252(5) Uani 1 1 d . . . C40 C 0.25182(13) 0.12197(11) 0.16369(8) 0.0221(4) Uani 1 1 d . . . C41 C 0.29797(15) 0.06065(11) 0.15842(10) 0.0301(5) Uani 1 1 d . . . H41 H 0.3486 0.0638 0.1458 0.036 Uiso 1 1 calc R . . C42 C 0.27038(16) -0.00502(12) 0.17148(11) 0.0379(6) Uani 1 1 d . . . H42 H 0.3026 -0.0463 0.1679 0.045 Uiso 1 1 calc R . . C43 C 0.19630(16) -0.01080(12) 0.18967(11) 0.0382(6) Uani 1 1 d . . . H43 H 0.1781 -0.0557 0.1990 0.046 Uiso 1 1 calc R . . C44 C 0.14949(15) 0.04912(12) 0.19412(10) 0.0314(5) Uani 1 1 d . . . H44 H 0.0984 0.0456 0.2063 0.038 Uiso 1 1 calc R . . C45 C 0.17637(14) 0.11479(11) 0.18092(8) 0.0240(4) Uani 1 1 d . . . H45 H 0.1427 0.1556 0.1837 0.029 Uiso 1 1 calc R . . C46 C 0.38194(13) 0.20273(10) 0.16222(8) 0.0187(4) Uani 1 1 d . . . H46 H 0.3999 0.1639 0.1417 0.022 Uiso 1 1 calc R . . C47 C 0.43216(13) 0.18827(10) 0.22060(8) 0.0188(4) Uani 1 1 d . . . C48 C 0.51305(14) 0.14238(11) 0.22818(9) 0.0244(5) Uani 1 1 d . . . H48A H 0.5521 0.1476 0.2646 0.037 Uiso 1 1 calc R . . H48B H 0.5452 0.1568 0.2031 0.037 Uiso 1 1 calc R . . H48C H 0.4946 0.0928 0.2217 0.037 Uiso 1 1 calc R . . C49 C 0.45588(13) 0.20359(11) 0.31314(8) 0.0205(4) Uani 1 1 d . . . C50 C 0.44870(13) 0.13785(11) 0.33676(8) 0.0229(4) Uani 1 1 d . . . C51 C 0.49329(14) 0.13022(12) 0.39088(9) 0.0277(5) Uani 1 1 d . . . H51 H 0.4901 0.0862 0.4076 0.033 Uiso 1 1 calc R . . C52 C 0.54142(15) 0.18435(12) 0.42047(9) 0.0297(5) Uani 1 1 d . . . H52 H 0.5714 0.1774 0.4571 0.036 Uiso 1 1 calc R . . C53 C 0.54631(15) 0.24922(12) 0.39699(9) 0.0276(5) Uani 1 1 d . . . H53 H 0.5796 0.2865 0.4178 0.033 Uiso 1 1 calc R . . C54 C 0.50308(14) 0.26062(11) 0.34327(9) 0.0226(4) Uani 1 1 d . . . C55 C 0.39321(14) 0.07703(11) 0.30741(9) 0.0250(5) Uani 1 1 d . . . H55 H 0.3712 0.0900 0.2689 0.030 Uiso 1 1 calc R . . C56 C 0.31169(15) 0.06477(12) 0.32741(10) 0.0302(5) Uani 1 1 d . . . H56A H 0.3317 0.0528 0.3653 0.045 Uiso 1 1 calc R . . H56B H 0.2759 0.0258 0.3075 0.045 Uiso 1 1 calc R . . H56C H 0.2755 0.1079 0.3222 0.045 Uiso 1 1 calc R . . C57 C 0.44694(16) 0.00796(11) 0.31218(10) 0.0337(5) Uani 1 1 d . . . H57A H 0.4984 0.0157 0.2990 0.051 Uiso 1 1 calc R . . H57B H 0.4090 -0.0291 0.2911 0.051 Uiso 1 1 calc R . . H57C H 0.4676 -0.0067 0.3495 0.051 Uiso 1 1 calc R . . C58 C 0.50940(14) 0.33163(11) 0.31737(9) 0.0241(4) Uani 1 1 d . . . H58 H 0.4496 0.3420 0.2919 0.029 Uiso 1 1 calc R . . C59 C 0.53374(15) 0.39336(12) 0.35666(9) 0.0303(5) Uani 1 1 d . . . H59A H 0.4926 0.3945 0.3783 0.045 Uiso 1 1 calc R . . H59B H 0.5294 0.4379 0.3370 0.045 Uiso 1 1 calc R . . H59C H 0.5948 0.3872 0.3798 0.045 Uiso 1 1 calc R . . C60 C 0.57666(14) 0.32814(12) 0.28543(9) 0.0280(5) Uani 1 1 d . . . H60A H 0.6368 0.3218 0.3098 0.042 Uiso 1 1 calc R . . H60B H 0.5742 0.3722 0.2654 0.042 Uiso 1 1 calc R . . H60C H 0.5620 0.2882 0.2607 0.042 Uiso 1 1 calc R . . C61 C 0.42199(13) 0.27122(11) 0.14657(8) 0.0178(4) Uani 1 1 d . . . C62 C 0.39654(13) 0.34137(10) 0.16421(8) 0.0211(4) Uani 1 1 d . . . H62A H 0.4379 0.3778 0.1594 0.032 Uiso 1 1 calc R . . H62B H 0.3992 0.3388 0.2018 0.032 Uiso 1 1 calc R . . H62C H 0.3358 0.3535 0.1430 0.032 Uiso 1 1 calc R . . C63 C 0.52692(13) 0.31635(10) 0.10553(8) 0.0185(4) Uani 1 1 d . . . C64 C 0.61907(13) 0.32255(10) 0.13117(8) 0.0199(4) Uani 1 1 d . . . C65 C 0.66769(14) 0.37204(11) 0.11208(8) 0.0239(4) Uani 1 1 d . . . H65 H 0.7297 0.3771 0.1293 0.029 Uiso 1 1 calc R . . C66 C 0.62806(14) 0.41390(11) 0.06874(9) 0.0263(5) Uani 1 1 d . . . H66 H 0.6624 0.4472 0.0561 0.032 Uiso 1 1 calc R . . C67 C 0.53784(15) 0.40691(11) 0.04379(8) 0.0250(5) Uani 1 1 d . . . H67 H 0.5106 0.4359 0.0140 0.030 Uiso 1 1 calc R . . C68 C 0.48575(13) 0.35833(11) 0.06123(8) 0.0210(4) Uani 1 1 d . . . C69 C 0.66471(14) 0.27402(12) 0.17697(9) 0.0271(5) Uani 1 1 d . . . H69 H 0.6213 0.2641 0.1973 0.033 Uiso 1 1 calc R . . C70 C 0.68723(16) 0.20309(13) 0.15546(11) 0.0394(6) Uani 1 1 d . . . H70A H 0.7285 0.2112 0.1344 0.059 Uiso 1 1 calc R . . H70B H 0.6325 0.1813 0.1330 0.059 Uiso 1 1 calc R . . H70C H 0.7151 0.1715 0.1852 0.059 Uiso 1 1 calc R . . C71 C 0.74801(15) 0.30614(15) 0.21581(10) 0.0401(6) Uani 1 1 d . . . H71A H 0.7953 0.3098 0.1986 0.060 Uiso 1 1 calc R . . H71B H 0.7681 0.2759 0.2473 0.060 Uiso 1 1 calc R . . H71C H 0.7340 0.3534 0.2265 0.060 Uiso 1 1 calc R . . C72 C 0.38769(14) 0.34899(12) 0.03168(9) 0.0290(5) Uani 1 1 d . . . H72 H 0.3555 0.3401 0.0587 0.035 Uiso 1 1 calc R . . C73 C 0.37472(18) 0.28340(18) -0.00459(11) 0.0555(8) Uani 1 1 d . . . H73A H 0.3109 0.2745 -0.0203 0.083 Uiso 1 1 calc R . . H73B H 0.4026 0.2422 0.0164 0.083 Uiso 1 1 calc R . . H73C H 0.4024 0.2918 -0.0329 0.083 Uiso 1 1 calc R . . C74 C 0.34520(19) 0.41245(18) -0.00066(13) 0.0608(9) Uani 1 1 d . . . H74A H 0.3496 0.4534 0.0228 0.091 Uiso 1 1 calc R . . H74B H 0.2823 0.4023 -0.0186 0.091 Uiso 1 1 calc R . . H74C H 0.3760 0.4229 -0.0272 0.091 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 0.01703(4) 0.01439(4) 0.02335(5) 0.00176(3) 0.00973(3) 0.00145(3) O1 0.0196(7) 0.0126(7) 0.0272(8) -0.0008(5) 0.0107(6) 0.0012(5) O2 0.0189(7) 0.0165(7) 0.0245(7) 0.0005(5) 0.0104(6) 0.0025(5) N1 0.0156(8) 0.0177(9) 0.0207(8) 0.0017(7) 0.0078(7) -0.0011(6) N2 0.0153(8) 0.0176(9) 0.0180(8) -0.0001(6) 0.0062(7) -0.0011(6) N3 0.0170(8) 0.0156(8) 0.0257(9) 0.0037(7) 0.0093(7) -0.0003(7) N4 0.0153(8) 0.0209(9) 0.0202(8) 0.0004(7) 0.0061(7) -0.0014(6) F1 0.0190(6) 0.0239(7) 0.0351(7) 0.0051(5) -0.0004(5) -0.0034(5) F2 0.0238(6) 0.0225(6) 0.0281(7) 0.0031(5) 0.0117(5) -0.0016(5) F3 0.0263(6) 0.0158(6) 0.0340(7) -0.0043(5) 0.0075(5) -0.0005(5) F4 0.0352(7) 0.0451(8) 0.0305(7) -0.0119(6) 0.0157(6) 0.0000(6) F5 0.0284(7) 0.0352(7) 0.0263(7) 0.0061(5) 0.0066(6) -0.0054(6) F6 0.0207(6) 0.0417(8) 0.0279(7) -0.0016(6) 0.0057(5) -0.0069(5) C1 0.0176(10) 0.0159(10) 0.0200(10) -0.0002(8) 0.0071(8) 0.0004(8) C2 0.0187(10) 0.0174(10) 0.0229(10) 0.0003(8) 0.0034(8) 0.0004(8) C3 0.0215(10) 0.0210(10) 0.0208(10) -0.0011(8) 0.0055(9) -0.0043(8) C4 0.0239(11) 0.0223(11) 0.0251(11) 0.0009(9) 0.0013(9) -0.0023(9) C5 0.0401(14) 0.0342(14) 0.0273(12) 0.0066(10) -0.0012(11) -0.0024(11) C6 0.0529(17) 0.0549(17) 0.0210(12) 0.0021(11) 0.0091(12) -0.0052(13) C7 0.0447(15) 0.0517(16) 0.0251(12) -0.0060(11) 0.0137(11) 0.0036(12) C8 0.0296(12) 0.0324(13) 0.0211(11) -0.0024(9) 0.0057(9) 0.0043(10) C9 0.0162(9) 0.0146(9) 0.0157(9) -0.0009(7) 0.0060(8) 0.0003(7) C10 0.0170(10) 0.0198(10) 0.0145(9) 0.0003(7) 0.0059(8) 0.0006(8) C11 0.0200(10) 0.0186(10) 0.0311(12) 0.0024(8) 0.0110(9) 0.0025(8) C12 0.0158(10) 0.0159(10) 0.0291(11) 0.0038(8) 0.0097(9) 0.0017(8) C13 0.0182(10) 0.0221(11) 0.0292(11) 0.0066(8) 0.0100(9) 0.0033(8) C14 0.0256(11) 0.0265(12) 0.0335(12) 0.0109(9) 0.0130(10) 0.0016(9) C15 0.0227(11) 0.0213(11) 0.0457(14) 0.0076(10) 0.0127(10) -0.0035(9) C16 0.0215(11) 0.0204(11) 0.0378(13) 0.0003(9) 0.0101(10) -0.0024(8) C17 0.0176(10) 0.0178(10) 0.0319(12) 0.0000(9) 0.0095(9) 0.0020(8) C18 0.0203(11) 0.0225(11) 0.0291(11) -0.0032(9) 0.0104(9) -0.0045(8) C19 0.0296(12) 0.0298(13) 0.0362(13) -0.0068(10) 0.0122(11) -0.0048(10) C20 0.0329(12) 0.0264(12) 0.0286(12) 0.0021(9) 0.0126(10) -0.0003(9) C21 0.0262(11) 0.0261(11) 0.0271(11) 0.0060(9) 0.0127(9) -0.0014(9) C22 0.0334(13) 0.0369(14) 0.0286(12) 0.0099(10) 0.0081(10) 0.0020(10) C23 0.0418(14) 0.0333(13) 0.0352(13) 0.0038(10) 0.0216(11) 0.0011(11) C24 0.0130(9) 0.0174(10) 0.0199(10) -0.0009(8) 0.0071(8) -0.0030(7) C25 0.0224(11) 0.0207(10) 0.0208(10) -0.0021(8) 0.0083(9) 0.0016(8) C26 0.0198(10) 0.0171(10) 0.0172(9) -0.0015(7) 0.0077(8) 0.0042(8) C27 0.0211(10) 0.0213(10) 0.0196(10) -0.0012(8) 0.0094(8) 0.0012(8) C28 0.0281(11) 0.0232(11) 0.0243(11) 0.0019(8) 0.0123(9) -0.0013(9) C29 0.0305(12) 0.0307(12) 0.0196(10) 0.0065(9) 0.0089(9) 0.0061(9) C30 0.0220(11) 0.0316(12) 0.0197(10) 0.0000(9) 0.0068(9) 0.0035(9) C31 0.0194(10) 0.0205(10) 0.0202(10) -0.0033(8) 0.0084(8) 0.0025(8) C32 0.0176(10) 0.0224(11) 0.0243(11) 0.0007(8) 0.0061(9) 0.0015(8) C33 0.0236(11) 0.0288(12) 0.0352(13) -0.0071(10) 0.0039(10) -0.0008(9) C34 0.0229(11) 0.0276(12) 0.0294(12) 0.0016(9) 0.0110(9) -0.0007(9) C35 0.0238(11) 0.0248(11) 0.0247(11) 0.0042(9) 0.0067(9) -0.0041(9) C36 0.0379(14) 0.0311(13) 0.0405(14) 0.0027(11) -0.0017(11) -0.0109(11) C37 0.0227(12) 0.0446(15) 0.0375(13) 0.0046(11) 0.0122(10) -0.0015(10) C38 0.0181(10) 0.0182(10) 0.0255(11) -0.0022(8) 0.0111(8) -0.0006(8) C39 0.0203(10) 0.0276(12) 0.0298(12) -0.0024(9) 0.0109(9) -0.0040(9) C40 0.0202(10) 0.0182(10) 0.0287(11) -0.0010(8) 0.0083(9) -0.0014(8) C41 0.0229(11) 0.0227(12) 0.0466(14) -0.0050(10) 0.0132(10) -0.0019(9) C42 0.0285(13) 0.0199(12) 0.0630(17) -0.0005(11) 0.0102(12) 0.0023(9) C43 0.0337(13) 0.0215(12) 0.0576(17) 0.0058(11) 0.0107(12) -0.0073(10) C44 0.0264(12) 0.0289(12) 0.0405(14) 0.0017(10) 0.0124(10) -0.0066(10) C45 0.0205(10) 0.0214(11) 0.0308(12) -0.0016(9) 0.0088(9) -0.0013(8) C46 0.0183(10) 0.0159(10) 0.0252(11) 0.0002(8) 0.0114(8) 0.0002(8) C47 0.0172(10) 0.0130(9) 0.0294(11) 0.0043(8) 0.0119(9) -0.0020(7) C48 0.0226(11) 0.0236(11) 0.0315(12) 0.0055(9) 0.0151(9) 0.0045(9) C49 0.0174(10) 0.0218(11) 0.0265(11) 0.0026(8) 0.0127(9) 0.0045(8) C50 0.0220(10) 0.0231(11) 0.0299(11) 0.0051(9) 0.0173(9) 0.0050(8) C51 0.0283(12) 0.0308(12) 0.0302(12) 0.0097(9) 0.0183(10) 0.0058(9) C52 0.0296(12) 0.0374(13) 0.0255(11) 0.0079(10) 0.0134(10) 0.0065(10) C53 0.0259(12) 0.0324(13) 0.0262(11) 0.0001(9) 0.0104(10) 0.0016(9) C54 0.0195(10) 0.0238(11) 0.0276(11) 0.0030(8) 0.0118(9) 0.0037(8) C55 0.0299(12) 0.0189(11) 0.0321(12) 0.0058(9) 0.0183(10) 0.0025(9) C56 0.0290(12) 0.0262(12) 0.0407(13) 0.0073(10) 0.0184(11) -0.0007(9) C57 0.0422(14) 0.0207(12) 0.0460(14) 0.0040(10) 0.0250(12) 0.0050(10) C58 0.0199(10) 0.0216(11) 0.0308(12) 0.0018(9) 0.0073(9) 0.0012(8) C59 0.0249(12) 0.0255(12) 0.0371(13) -0.0013(10) 0.0038(10) -0.0001(9) C60 0.0282(12) 0.0230(11) 0.0354(13) 0.0066(9) 0.0132(10) -0.0014(9) C61 0.0148(9) 0.0205(10) 0.0178(10) 0.0028(8) 0.0043(8) -0.0002(8) C62 0.0230(10) 0.0178(10) 0.0258(11) 0.0021(8) 0.0122(9) -0.0011(8) C63 0.0201(10) 0.0193(10) 0.0196(10) -0.0021(8) 0.0109(8) -0.0006(8) C64 0.0200(10) 0.0204(10) 0.0218(10) -0.0007(8) 0.0102(8) 0.0003(8) C65 0.0195(10) 0.0280(12) 0.0260(11) -0.0003(9) 0.0092(9) -0.0031(8) C66 0.0293(12) 0.0251(11) 0.0290(12) 0.0021(9) 0.0156(10) -0.0054(9) C67 0.0326(12) 0.0251(11) 0.0202(10) 0.0031(9) 0.0125(9) 0.0011(9) C68 0.0225(10) 0.0239(11) 0.0186(10) -0.0008(8) 0.0093(8) 0.0002(8) C69 0.0184(10) 0.0333(12) 0.0302(12) 0.0100(10) 0.0081(9) -0.0007(9) C70 0.0284(13) 0.0317(13) 0.0593(17) 0.0132(12) 0.0148(12) 0.0048(10) C71 0.0280(13) 0.0555(17) 0.0332(13) 0.0119(12) 0.0034(11) -0.0055(11) C72 0.0211(11) 0.0419(14) 0.0240(11) 0.0080(10) 0.0063(9) 0.0000(10) C73 0.0347(15) 0.092(2) 0.0409(16) -0.0248(16) 0.0127(13) -0.0203(15) C74 0.0365(16) 0.079(2) 0.062(2) 0.0350(17) 0.0062(14) 0.0061(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O1 2.1679(13) . ? Pb1 O2 2.1707(14) . ? Pb1 N1 2.6075(16) . ? Pb1 N3 2.6319(16) . ? O1 C1 1.380(2) . ? O2 C38 1.381(2) . ? N1 C10 1.281(2) . ? N1 C12 1.449(2) . ? N2 C24 1.270(2) . ? N2 C26 1.432(2) . ? N3 C47 1.277(2) . ? N3 C49 1.444(3) . ? N4 C61 1.280(3) . ? N4 C63 1.430(2) . ? F1 C2 1.340(2) . ? F2 C2 1.343(2) . ? F3 C2 1.353(2) . ? F4 C39 1.348(2) . ? F5 C39 1.339(2) . ? F6 C39 1.343(2) . ? C1 C2 1.539(3) . ? C1 C3 1.557(3) . ? C1 C9 1.566(3) . ? C3 C4 1.384(3) . ? C3 C8 1.402(3) . ? C4 C5 1.391(3) . ? C4 H4 0.9500 . ? C5 C6 1.384(4) . ? C5 H5 0.9500 . ? C6 C7 1.378(4) . ? C6 H6 0.9500 . ? C7 C8 1.389(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.534(3) . ? C9 C24 1.544(3) . ? C9 H9 1.0000 . ? C10 C11 1.504(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.410(3) . ? C12 C17 1.413(3) . ? C13 C14 1.396(3) . ? C13 C21 1.517(3) . ? C14 C15 1.378(3) . ? C14 H14 0.9500 . ? C15 C16 1.379(3) . ? C15 H15 0.9500 . ? C16 C17 1.392(3) . ? C16 H16 0.9500 . ? C17 C18 1.519(3) . ? C18 C19 1.530(3) . ? C18 C20 1.533(3) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.539(3) . ? C21 C23 1.539(3) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.500(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C31 1.406(3) . ? C26 C27 1.409(3) . ? C27 C28 1.396(3) . ? C27 C35 1.511(3) . ? C28 C29 1.378(3) . ? C28 H28 0.9500 . ? C29 C30 1.383(3) . ? C29 H29 0.9500 . ? C30 C31 1.394(3) . ? C30 H30 0.9500 . ? C31 C32 1.520(3) . ? C32 C33 1.524(3) . ? C32 C34 1.533(3) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.523(3) . ? C35 C37 1.531(3) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.548(3) . ? C38 C40 1.553(3) . ? C38 C46 1.572(3) . ? C40 C45 1.394(3) . ? C40 C41 1.395(3) . ? C41 C42 1.391(3) . ? C41 H41 0.9500 . ? C42 C43 1.387(3) . ? C42 H42 0.9500 . ? C43 C44 1.374(3) . ? C43 H43 0.9500 . ? C44 C45 1.388(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.532(3) . ? C46 C61 1.547(3) . ? C46 H46 1.0000 . ? C47 C48 1.502(3) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.409(3) . ? C49 C54 1.412(3) . ? C50 C51 1.399(3) . ? C50 C55 1.511(3) . ? C51 C52 1.371(3) . ? C51 H51 0.9500 . ? C52 C53 1.385(3) . ? C52 H52 0.9500 . ? C53 C54 1.394(3) . ? C53 H53 0.9500 . ? C54 C58 1.522(3) . ? C55 C56 1.538(3) . ? C55 C57 1.539(3) . ? C55 H55 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.532(3) . ? C58 C60 1.533(3) . ? C58 H58 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.498(3) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C68 1.402(3) . ? C63 C64 1.411(3) . ? C64 C65 1.392(3) . ? C64 C69 1.517(3) . ? C65 C66 1.378(3) . ? C65 H65 0.9500 . ? C66 C67 1.382(3) . ? C66 H66 0.9500 . ? C67 C68 1.394(3) . ? C67 H67 0.9500 . ? C68 C72 1.518(3) . ? C69 C71 1.530(3) . ? C69 C70 1.536(3) . ? C69 H69 1.0000 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C74 1.509(3) . ? C72 C73 1.542(4) . ? C72 H72 1.0000 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 O2 85.09(5) . . ? O1 Pb1 N1 77.37(5) . . ? O2 Pb1 N1 90.74(5) . . ? O1 Pb1 N3 93.24(5) . . ? O2 Pb1 N3 78.30(5) . . ? N1 Pb1 N3 166.23(5) . . ? C1 O1 Pb1 126.07(11) . . ? C38 O2 Pb1 123.35(12) . . ? C10 N1 C12 121.96(16) . . ? C10 N1 Pb1 127.22(13) . . ? C12 N1 Pb1 105.63(11) . . ? C24 N2 C26 126.43(16) . . ? C47 N3 C49 121.22(17) . . ? C47 N3 Pb1 126.17(13) . . ? C49 N3 Pb1 108.44(11) . . ? C61 N4 C63 122.64(17) . . ? O1 C1 C2 103.70(15) . . ? O1 C1 C3 113.50(16) . . ? C2 C1 C3 106.09(15) . . ? O1 C1 C9 115.40(16) . . ? C2 C1 C9 108.85(15) . . ? C3 C1 C9 108.70(15) . . ? F1 C2 F2 106.11(16) . . ? F1 C2 F3 106.17(16) . . ? F2 C2 F3 106.44(15) . . ? F1 C2 C1 111.96(16) . . ? F2 C2 C1 112.39(16) . . ? F3 C2 C1 113.25(16) . . ? C4 C3 C8 117.77(19) . . ? C4 C3 C1 119.30(18) . . ? C8 C3 C1 122.90(18) . . ? C3 C4 C5 121.4(2) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 120.1(2) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C7 C6 C5 119.3(2) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 120.7(2) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C7 C8 C3 120.7(2) . . ? C7 C8 H8 119.7 . . ? C3 C8 H8 119.7 . . ? C10 C9 C24 110.54(15) . . ? C10 C9 C1 113.73(15) . . ? C24 C9 C1 118.37(15) . . ? C10 C9 H9 104.1 . . ? C24 C9 H9 104.1 . . ? C1 C9 H9 104.1 . . ? N1 C10 C11 124.49(17) . . ? N1 C10 C9 121.86(17) . . ? C11 C10 C9 113.65(16) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 121.42(18) . . ? C13 C12 N1 120.27(18) . . ? C17 C12 N1 117.85(18) . . ? C14 C13 C12 117.5(2) . . ? C14 C13 C21 118.36(19) . . ? C12 C13 C21 124.15(18) . . ? C15 C14 C13 121.8(2) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 120.0(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 121.3(2) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C12 118.0(2) . . ? C16 C17 C18 120.71(19) . . ? C12 C17 C18 121.20(18) . . ? C17 C18 C19 114.07(18) . . ? C17 C18 C20 109.90(17) . . ? C19 C18 C20 108.53(19) . . ? C17 C18 H18 108.1 . . ? C19 C18 H18 108.1 . . ? C20 C18 H18 108.1 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C21 C22 111.07(18) . . ? C13 C21 C23 111.27(18) . . ? C22 C21 C23 109.39(18) . . ? C13 C21 H21 108.3 . . ? C22 C21 H21 108.3 . . ? C23 C21 H21 108.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 C25 127.05(18) . . ? N2 C24 C9 113.39(16) . . ? C25 C24 C9 119.52(16) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C31 C26 C27 120.60(18) . . ? C31 C26 N2 119.43(17) . . ? C27 C26 N2 118.87(17) . . ? C28 C27 C26 118.51(19) . . ? C28 C27 C35 120.80(18) . . ? C26 C27 C35 120.66(18) . . ? C29 C28 C27 121.32(19) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C30 119.7(2) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C29 C30 C31 121.3(2) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C30 C31 C26 118.51(19) . . ? C30 C31 C32 120.66(18) . . ? C26 C31 C32 120.68(18) . . ? C31 C32 C33 113.14(17) . . ? C31 C32 C34 109.83(16) . . ? C33 C32 C34 111.10(17) . . ? C31 C32 H32 107.5 . . ? C33 C32 H32 107.5 . . ? C34 C32 H32 107.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C27 C35 C36 113.93(18) . . ? C27 C35 C37 109.98(18) . . ? C36 C35 C37 110.10(19) . . ? C27 C35 H35 107.5 . . ? C36 C35 H35 107.5 . . ? C37 C35 H35 107.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O2 C38 C39 104.53(16) . . ? O2 C38 C40 113.00(16) . . ? C39 C38 C40 105.21(16) . . ? O2 C38 C46 114.91(16) . . ? C39 C38 C46 108.50(15) . . ? C40 C38 C46 109.99(16) . . ? F5 C39 F6 105.81(17) . . ? F5 C39 F4 106.64(16) . . ? F6 C39 F4 106.55(17) . . ? F5 C39 C38 112.58(17) . . ? F6 C39 C38 111.76(16) . . ? F4 C39 C38 113.01(17) . . ? C45 C40 C41 117.86(19) . . ? C45 C40 C38 118.74(18) . . ? C41 C40 C38 123.33(18) . . ? C42 C41 C40 120.5(2) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C43 C42 C41 120.7(2) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C44 C43 C42 119.3(2) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C43 C44 C45 120.4(2) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C40 121.2(2) . . ? C44 C45 H45 119.4 . . ? C40 C45 H45 119.4 . . ? C47 C46 C61 106.67(15) . . ? C47 C46 C38 113.88(15) . . ? C61 C46 C38 118.54(16) . . ? C47 C46 H46 105.6 . . ? C61 C46 H46 105.6 . . ? C38 C46 H46 105.6 . . ? N3 C47 C48 124.93(19) . . ? N3 C47 C46 121.28(17) . . ? C48 C47 C46 113.69(17) . . ? 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 . . ? C50 C49 C54 121.46(19) . . ? C50 C49 N3 120.49(18) . . ? C54 C49 N3 117.80(17) . . ? C51 C50 C49 117.4(2) . . ? C51 C50 C55 118.93(19) . . ? C49 C50 C55 123.66(19) . . ? C52 C51 C50 122.0(2) . . ? C52 C51 H51 119.0 . . ? C50 C51 H51 119.0 . . ? C51 C52 C53 120.0(2) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C52 C53 C54 121.0(2) . . ? C52 C53 H53 119.5 . . ? C54 C53 H53 119.5 . . ? C53 C54 C49 118.08(19) . . ? C53 C54 C58 121.0(2) . . ? C49 C54 C58 120.91(19) . . ? C50 C55 C56 110.64(17) . . ? C50 C55 C57 112.55(19) . . ? C56 C55 C57 109.62(17) . . ? C50 C55 H55 108.0 . . ? C56 C55 H55 108.0 . . ? C57 C55 H55 108.0 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C54 C58 C59 113.90(18) . . ? C54 C58 C60 110.75(17) . . ? C59 C58 C60 109.16(18) . . ? C54 C58 H58 107.6 . . ? C59 C58 H58 107.6 . . ? C60 C58 H58 107.6 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N4 C61 C62 126.56(18) . . ? N4 C61 C46 113.85(17) . . ? C62 C61 C46 119.45(16) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C68 C63 C64 120.59(18) . . ? C68 C63 N4 120.86(17) . . ? C64 C63 N4 118.07(17) . . ? C65 C64 C63 118.52(19) . . ? C65 C64 C69 120.82(18) . . ? C63 C64 C69 120.60(17) . . ? C66 C65 C64 121.5(2) . . ? C66 C65 H65 119.2 . . ? C64 C65 H65 119.2 . . ? C65 C66 C67 119.30(19) . . ? C65 C66 H66 120.3 . . ? C67 C66 H66 120.3 . . ? C66 C67 C68 121.7(2) . . ? C66 C67 H67 119.2 . . ? C68 C67 H67 119.2 . . ? C67 C68 C63 118.36(19) . . ? C67 C68 C72 120.85(19) . . ? C63 C68 C72 120.74(18) . . ? C64 C69 C71 113.78(18) . . ? C64 C69 C70 109.92(19) . . ? C71 C69 C70 110.39(19) . . ? C64 C69 H69 107.5 . . ? C71 C69 H69 107.5 . . ? C70 C69 H69 107.5 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C74 C72 C68 114.3(2) . . ? C74 C72 C73 109.5(2) . . ? C68 C72 C73 109.91(19) . . ? C74 C72 H72 107.7 . . ? C68 C72 H72 107.7 . . ? C73 C72 H72 107.7 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 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 O2 Pb1 O1 C1 130.67(14) . . . . ? N1 Pb1 O1 C1 38.81(14) . . . . ? N3 Pb1 O1 C1 -151.38(14) . . . . ? O1 Pb1 O2 C38 133.80(14) . . . . ? N1 Pb1 O2 C38 -148.94(14) . . . . ? N3 Pb1 O2 C38 39.46(13) . . . . ? O1 Pb1 N1 C10 -17.27(15) . . . . ? O2 Pb1 N1 C10 -102.06(16) . . . . ? N3 Pb1 N1 C10 -65.1(3) . . . . ? O1 Pb1 N1 C12 -171.81(13) . . . . ? O2 Pb1 N1 C12 103.39(12) . . . . ? N3 Pb1 N1 C12 140.3(2) . . . . ? O1 Pb1 N3 C47 -101.90(16) . . . . ? O2 Pb1 N3 C47 -17.60(15) . . . . ? N1 Pb1 N3 C47 -55.5(3) . . . . ? O1 Pb1 N3 C49 101.08(12) . . . . ? O2 Pb1 N3 C49 -174.62(13) . . . . ? N1 Pb1 N3 C49 147.53(19) . . . . ? Pb1 O1 C1 C2 169.19(11) . . . . ? Pb1 O1 C1 C3 54.5(2) . . . . ? Pb1 O1 C1 C9 -71.87(19) . . . . ? O1 C1 C2 F1 -65.41(19) . . . . ? C3 C1 C2 F1 54.4(2) . . . . ? C9 C1 C2 F1 171.25(15) . . . . ? O1 C1 C2 F2 53.9(2) . . . . ? C3 C1 C2 F2 173.76(15) . . . . ? C9 C1 C2 F2 -69.4(2) . . . . ? O1 C1 C2 F3 174.59(15) . . . . ? C3 C1 C2 F3 -65.6(2) . . . . ? C9 C1 C2 F3 51.2(2) . . . . ? O1 C1 C3 C4 16.0(3) . . . . ? C2 C1 C3 C4 -97.2(2) . . . . ? C9 C1 C3 C4 145.85(18) . . . . ? O1 C1 C3 C8 -165.75(19) . . . . ? C2 C1 C3 C8 81.0(2) . . . . ? C9 C1 C3 C8 -35.9(3) . . . . ? C8 C3 C4 C5 2.6(3) . . . . ? C1 C3 C4 C5 -179.04(19) . . . . ? C3 C4 C5 C6 -0.5(4) . . . . ? C4 C5 C6 C7 -1.5(4) . . . . ? C5 C6 C7 C8 1.4(4) . . . . ? C6 C7 C8 C3 0.7(4) . . . . ? C4 C3 C8 C7 -2.7(3) . . . . ? C1 C3 C8 C7 179.0(2) . . . . ? O1 C1 C9 C10 66.8(2) . . . . ? C2 C1 C9 C10 -177.17(15) . . . . ? C3 C1 C9 C10 -62.0(2) . . . . ? O1 C1 C9 C24 -65.5(2) . . . . ? C2 C1 C9 C24 50.5(2) . . . . ? C3 C1 C9 C24 165.68(16) . . . . ? C12 N1 C10 C11 -3.2(3) . . . . ? Pb1 N1 C10 C11 -153.95(15) . . . . ? C12 N1 C10 C9 177.03(17) . . . . ? Pb1 N1 C10 C9 26.2(3) . . . . ? C24 C9 C10 N1 90.9(2) . . . . ? C1 C9 C10 N1 -45.0(2) . . . . ? C24 C9 C10 C11 -88.89(19) . . . . ? C1 C9 C10 C11 135.14(17) . . . . ? C10 N1 C12 C13 -77.8(2) . . . . ? Pb1 N1 C12 C13 78.39(18) . . . . ? C10 N1 C12 C17 109.9(2) . . . . ? Pb1 N1 C12 C17 -93.91(17) . . . . ? C17 C12 C13 C14 -1.4(3) . . . . ? N1 C12 C13 C14 -173.39(18) . . . . ? C17 C12 C13 C21 178.08(19) . . . . ? N1 C12 C13 C21 6.1(3) . . . . ? C12 C13 C14 C15 0.1(3) . . . . ? C21 C13 C14 C15 -179.4(2) . . . . ? C13 C14 C15 C16 0.8(3) . . . . ? C14 C15 C16 C17 -0.4(3) . . . . ? C15 C16 C17 C12 -0.8(3) . . . . ? C15 C16 C17 C18 -178.03(19) . . . . ? C13 C12 C17 C16 1.7(3) . . . . ? N1 C12 C17 C16 173.92(17) . . . . ? C13 C12 C17 C18 178.92(18) . . . . ? N1 C12 C17 C18 -8.9(3) . . . . ? C16 C17 C18 C19 -24.6(3) . . . . ? C12 C17 C18 C19 158.31(19) . . . . ? C16 C17 C18 C20 97.6(2) . . . . ? C12 C17 C18 C20 -79.6(2) . . . . ? C14 C13 C21 C22 59.5(2) . . . . ? C12 C13 C21 C22 -119.9(2) . . . . ? C14 C13 C21 C23 -62.6(3) . . . . ? C12 C13 C21 C23 117.9(2) . . . . ? C26 N2 C24 C25 1.0(3) . . . . ? C26 N2 C24 C9 -176.70(16) . . . . ? C10 C9 C24 N2 109.73(18) . . . . ? C1 C9 C24 N2 -116.59(19) . . . . ? C10 C9 C24 C25 -68.1(2) . . . . ? C1 C9 C24 C25 65.5(2) . . . . ? C24 N2 C26 C31 85.8(2) . . . . ? C24 N2 C26 C27 -106.2(2) . . . . ? C31 C26 C27 C28 1.3(3) . . . . ? N2 C26 C27 C28 -166.67(17) . . . . ? C31 C26 C27 C35 -176.96(18) . . . . ? N2 C26 C27 C35 15.1(3) . . . . ? C26 C27 C28 C29 -0.1(3) . . . . ? C35 C27 C28 C29 178.14(19) . . . . ? C27 C28 C29 C30 -1.4(3) . . . . ? C28 C29 C30 C31 1.8(3) . . . . ? C29 C30 C31 C26 -0.6(3) . . . . ? C29 C30 C31 C32 174.90(19) . . . . ? C27 C26 C31 C30 -0.9(3) . . . . ? N2 C26 C31 C30 166.94(17) . . . . ? C27 C26 C31 C32 -176.43(17) . . . . ? N2 C26 C31 C32 -8.6(3) . . . . ? C30 C31 C32 C33 36.7(3) . . . . ? C26 C31 C32 C33 -147.90(18) . . . . ? C30 C31 C32 C34 -88.1(2) . . . . ? C26 C31 C32 C34 87.3(2) . . . . ? C28 C27 C35 C36 40.9(3) . . . . ? C26 C27 C35 C36 -140.9(2) . . . . ? C28 C27 C35 C37 -83.3(2) . . . . ? C26 C27 C35 C37 94.9(2) . . . . ? Pb1 O2 C38 C39 166.98(11) . . . . ? Pb1 O2 C38 C40 53.1(2) . . . . ? Pb1 O2 C38 C46 -74.21(19) . . . . ? O2 C38 C39 F5 53.3(2) . . . . ? C40 C38 C39 F5 172.59(16) . . . . ? C46 C38 C39 F5 -69.7(2) . . . . ? O2 C38 C39 F6 -65.6(2) . . . . ? C40 C38 C39 F6 53.7(2) . . . . ? C46 C38 C39 F6 171.35(16) . . . . ? O2 C38 C39 F4 174.23(15) . . . . ? C40 C38 C39 F4 -66.5(2) . . . . ? C46 C38 C39 F4 51.2(2) . . . . ? O2 C38 C40 C45 18.0(3) . . . . ? C39 C38 C40 C45 -95.4(2) . . . . ? C46 C38 C40 C45 147.91(19) . . . . ? O2 C38 C40 C41 -164.8(2) . . . . ? C39 C38 C40 C41 81.7(2) . . . . ? C46 C38 C40 C41 -34.9(3) . . . . ? C45 C40 C41 C42 -1.8(3) . . . . ? C38 C40 C41 C42 -178.9(2) . . . . ? C40 C41 C42 C43 0.4(4) . . . . ? C41 C42 C43 C44 0.8(4) . . . . ? C42 C43 C44 C45 -0.5(4) . . . . ? C43 C44 C45 C40 -1.0(4) . . . . ? C41 C40 C45 C44 2.1(3) . . . . ? C38 C40 C45 C44 179.4(2) . . . . ? O2 C38 C46 C47 70.9(2) . . . . ? C39 C38 C46 C47 -172.57(16) . . . . ? C40 C38 C46 C47 -58.0(2) . . . . ? O2 C38 C46 C61 -55.8(2) . . . . ? C39 C38 C46 C61 60.7(2) . . . . ? C40 C38 C46 C61 175.29(16) . . . . ? C49 N3 C47 C48 -3.1(3) . . . . ? Pb1 N3 C47 C48 -157.41(14) . . . . ? C49 N3 C47 C46 -179.29(17) . . . . ? Pb1 N3 C47 C46 26.4(2) . . . . ? C61 C46 C47 N3 86.0(2) . . . . ? C38 C46 C47 N3 -46.7(2) . . . . ? C61 C46 C47 C48 -90.59(19) . . . . ? C38 C46 C47 C48 136.73(17) . . . . ? C47 N3 C49 C50 -73.4(2) . . . . ? Pb1 N3 C49 C50 84.98(18) . . . . ? C47 N3 C49 C54 112.3(2) . . . . ? Pb1 N3 C49 C54 -89.36(17) . . . . ? C54 C49 C50 C51 -2.6(3) . . . . ? N3 C49 C50 C51 -176.74(17) . . . . ? C54 C49 C50 C55 175.05(18) . . . . ? N3 C49 C50 C55 0.9(3) . . . . ? C49 C50 C51 C52 0.8(3) . . . . ? C55 C50 C51 C52 -176.95(19) . . . . ? C50 C51 C52 C53 0.6(3) . . . . ? C51 C52 C53 C54 -0.2(3) . . . . ? C52 C53 C54 C49 -1.5(3) . . . . ? C52 C53 C54 C58 -179.28(19) . . . . ? C50 C49 C54 C53 2.9(3) . . . . ? N3 C49 C54 C53 177.23(18) . . . . ? C50 C49 C54 C58 -179.28(18) . . . . ? N3 C49 C54 C58 -5.0(3) . . . . ? C51 C50 C55 C56 67.2(2) . . . . ? C49 C50 C55 C56 -110.4(2) . . . . ? C51 C50 C55 C57 -55.8(2) . . . . ? C49 C50 C55 C57 126.6(2) . . . . ? C53 C54 C58 C59 -22.0(3) . . . . ? C49 C54 C58 C59 160.26(19) . . . . ? C53 C54 C58 C60 101.4(2) . . . . ? C49 C54 C58 C60 -76.3(2) . . . . ? C63 N4 C61 C62 -1.8(3) . . . . ? C63 N4 C61 C46 -177.38(17) . . . . ? C47 C46 C61 N4 99.06(19) . . . . ? C38 C46 C61 N4 -130.86(19) . . . . ? C47 C46 C61 C62 -76.9(2) . . . . ? C38 C46 C61 C62 53.2(2) . . . . ? C61 N4 C63 C68 -76.9(3) . . . . ? C61 N4 C63 C64 111.0(2) . . . . ? C68 C63 C64 C65 1.1(3) . . . . ? N4 C63 C64 C65 173.22(18) . . . . ? C68 C63 C64 C69 -176.20(19) . . . . ? N4 C63 C64 C69 -4.1(3) . . . . ? C63 C64 C65 C66 -0.8(3) . . . . ? C69 C64 C65 C66 176.5(2) . . . . ? C64 C65 C66 C67 0.3(3) . . . . ? C65 C66 C67 C68 -0.2(3) . . . . ? C66 C67 C68 C63 0.5(3) . . . . ? C66 C67 C68 C72 -177.0(2) . . . . ? C64 C63 C68 C67 -1.0(3) . . . . ? N4 C63 C68 C67 -172.88(18) . . . . ? C64 C63 C68 C72 176.60(19) . . . . ? N4 C63 C68 C72 4.7(3) . . . . ? C65 C64 C69 C71 29.5(3) . . . . ? C63 C64 C69 C71 -153.2(2) . . . . ? C65 C64 C69 C70 -94.9(2) . . . . ? C63 C64 C69 C70 82.4(2) . . . . ? C67 C68 C72 C74 -23.9(3) . . . . ? C63 C68 C72 C74 158.5(2) . . . . ? C67 C68 C72 C73 99.6(2) . . . . ? C63 C68 C72 C73 -78.0(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.717 _refine_diff_density_min -1.197 _refine_diff_density_rms 0.057