# 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 ? _publ_contact_author_name 'Cameron Jones' _publ_contact_author_email cameron.jones@monash.edu loop_ _publ_author_name C.Jones S.Choong C.Schenk A.Stasch D.Dange data_(MesNac)MgN(Mes)Ge(C3tBu2NMes) _database_code_depnum_ccdc_archive 'CCDC 859474' #TrackingRef '(MesNac)MgN(Mes)Ge(C3tBu2NMes).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H70 Ge Mg N4' _chemical_formula_weight 848.02 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 '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 20.546(4) _cell_length_b 12.171(2) _cell_length_c 19.870(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.60(3) _cell_angle_gamma 90.00 _cell_volume 4785.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9796 _exptl_absorpt_correction_T_max 0.9931 _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82740 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.62 _reflns_number_total 12014 _reflns_number_gt 10900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CifTAB _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^)+(0.0572P)^2^+3.6699P] 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 12014 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.685446(8) 0.137161(14) 0.371910(9) 0.01980(6) Uani 1 1 d . . . Mg1 Mg 0.79973(3) 0.03600(5) 0.48596(3) 0.02090(11) Uani 1 1 d . . . N1 N 0.68323(7) 0.13412(11) 0.26866(7) 0.0193(3) Uani 1 1 d . . . C1 C 0.58555(8) 0.15804(14) 0.33190(8) 0.0218(3) Uani 1 1 d . . . N2 N 0.72413(7) 0.00394(12) 0.40510(7) 0.0215(3) Uani 1 1 d . . . C2 C 0.57335(8) 0.18515(14) 0.26346(8) 0.0223(3) Uani 1 1 d . . . H2 H 0.5304 0.2131 0.2387 0.027 Uiso 1 1 calc R . . N3 N 0.87749(7) 0.13567(11) 0.53261(8) 0.0232(3) Uani 1 1 d . . . C3 C 0.62616(8) 0.17132(13) 0.22820(8) 0.0196(3) Uani 1 1 d . . . N4 N 0.81393(7) -0.06795(11) 0.56793(7) 0.0222(3) Uani 1 1 d . . . C4 C 0.53535(8) 0.19137(15) 0.37253(9) 0.0260(3) Uani 1 1 d . . . C5 C 0.54263(17) 0.3147(2) 0.38712(17) 0.0620(8) Uani 1 1 d . . . H5A H 0.5113 0.3373 0.4140 0.093 Uiso 1 1 calc R . . H5B H 0.5322 0.3549 0.3428 0.093 Uiso 1 1 calc R . . H5C H 0.5891 0.3310 0.4140 0.093 Uiso 1 1 calc R . . C6 C 0.46283(10) 0.1660(3) 0.33089(12) 0.0607(8) Uani 1 1 d . . . H6A H 0.4589 0.0878 0.3188 0.091 Uiso 1 1 calc R . . H6B H 0.4513 0.2100 0.2880 0.091 Uiso 1 1 calc R . . H6C H 0.4319 0.1840 0.3592 0.091 Uiso 1 1 calc R . . C7 C 0.54849(11) 0.1315(2) 0.44227(10) 0.0396(5) Uani 1 1 d . . . H7A H 0.5409 0.0526 0.4339 0.059 Uiso 1 1 calc R . . H7B H 0.5177 0.1594 0.4683 0.059 Uiso 1 1 calc R . . H7C H 0.5953 0.1441 0.4694 0.059 Uiso 1 1 calc R . . C8 C 0.61088(8) 0.21015(14) 0.15243(8) 0.0220(3) Uani 1 1 d . . . C9 C 0.54855(9) 0.14752(16) 0.10916(9) 0.0273(3) Uani 1 1 d . . . H9A H 0.5591 0.0690 0.1089 0.041 Uiso 1 1 calc R . . H9B H 0.5360 0.1755 0.0611 0.041 Uiso 1 1 calc R . . H9C H 0.5108 0.1582 0.1299 0.041 Uiso 1 1 calc R . . C10 C 0.59458(9) 0.33450(15) 0.15255(9) 0.0270(3) Uani 1 1 d . . . H10A H 0.5564 0.3457 0.1725 0.041 Uiso 1 1 calc R . . H10B H 0.5829 0.3624 0.1045 0.041 Uiso 1 1 calc R . . H10C H 0.6342 0.3740 0.1807 0.041 Uiso 1 1 calc R . . C11 C 0.66771(9) 0.19807(17) 0.11629(9) 0.0281(3) Uani 1 1 d . . . H11A H 0.7077 0.2383 0.1429 0.042 Uiso 1 1 calc R . . H11B H 0.6527 0.2280 0.0688 0.042 Uiso 1 1 calc R . . H11C H 0.6790 0.1202 0.1141 0.042 Uiso 1 1 calc R . . C12 C 0.74164(7) 0.10039(13) 0.24779(8) 0.0195(3) Uani 1 1 d . . . C13 C 0.79837(8) 0.16939(14) 0.26080(9) 0.0218(3) Uani 1 1 d . . . C14 C 0.85587(8) 0.13097(15) 0.24368(9) 0.0253(3) Uani 1 1 d . . . H14 H 0.8948 0.1765 0.2526 0.030 Uiso 1 1 calc R . . C15 C 0.85790(8) 0.02810(15) 0.21400(9) 0.0260(3) Uani 1 1 d . . . C16 C 0.80062(9) -0.03778(14) 0.20114(9) 0.0251(3) Uani 1 1 d . . . H16 H 0.8014 -0.1079 0.1803 0.030 Uiso 1 1 calc R . . C17 C 0.74197(8) -0.00398(14) 0.21792(8) 0.0215(3) Uani 1 1 d . . . C18 C 0.79683(9) 0.28393(14) 0.28890(10) 0.0276(3) Uani 1 1 d . . . H18A H 0.7996 0.2804 0.3389 0.041 Uiso 1 1 calc R . . H18B H 0.7546 0.3201 0.2640 0.041 Uiso 1 1 calc R . . H18C H 0.8353 0.3259 0.2821 0.041 Uiso 1 1 calc R . . C19 C 0.92005(10) -0.00924(19) 0.19377(11) 0.0365(4) Uani 1 1 d . . . H19A H 0.9268 -0.0881 0.2030 0.055 Uiso 1 1 calc R . . H19B H 0.9595 0.0312 0.2212 0.055 Uiso 1 1 calc R . . H19C H 0.9142 0.0049 0.1439 0.055 Uiso 1 1 calc R . . C20 C 0.68060(9) -0.07741(14) 0.20102(9) 0.0255(3) Uani 1 1 d . . . H20A H 0.6537 -0.0635 0.1530 0.038 Uiso 1 1 calc R . . H20B H 0.6532 -0.0620 0.2334 0.038 Uiso 1 1 calc R . . H20C H 0.6950 -0.1545 0.2057 0.038 Uiso 1 1 calc R . . C21 C 0.71856(8) -0.10255(14) 0.37659(8) 0.0215(3) Uani 1 1 d . . . C22 C 0.77651(9) -0.15358(14) 0.36484(9) 0.0244(3) Uani 1 1 d . . . C23 C 0.77376(10) -0.26135(16) 0.34056(9) 0.0299(4) Uani 1 1 d . . . H23 H 0.8132 -0.2932 0.3324 0.036 Uiso 1 1 calc R . . C24 C 0.71498(11) -0.32368(16) 0.32787(10) 0.0321(4) Uani 1 1 d . . . C25 C 0.65824(10) -0.27354(15) 0.33975(9) 0.0290(4) Uani 1 1 d . . . H25 H 0.6175 -0.3146 0.3315 0.035 Uiso 1 1 calc R . . C26 C 0.65867(8) -0.16598(14) 0.36313(9) 0.0242(3) Uani 1 1 d . . . C27 C 0.84252(8) -0.09153(16) 0.37957(10) 0.0288(4) Uani 1 1 d . . . H27A H 0.8626 -0.0874 0.4302 0.043 Uiso 1 1 calc R . . H27B H 0.8342 -0.0171 0.3604 0.043 Uiso 1 1 calc R . . H27C H 0.8735 -0.1298 0.3577 0.043 Uiso 1 1 calc R . . C28 C 0.71342(14) -0.44158(18) 0.30400(13) 0.0466(5) Uani 1 1 d . . . H28A H 0.7580 -0.4621 0.2988 0.070 Uiso 1 1 calc R . . H28B H 0.6795 -0.4498 0.2590 0.070 Uiso 1 1 calc R . . H28C H 0.7018 -0.4895 0.3387 0.070 Uiso 1 1 calc R . . C29 C 0.59612(9) -0.11742(16) 0.37620(11) 0.0308(4) Uani 1 1 d . . . H29A H 0.5781 -0.0606 0.3412 0.046 Uiso 1 1 calc R . . H29B H 0.6072 -0.0847 0.4230 0.046 Uiso 1 1 calc R . . H29C H 0.5622 -0.1752 0.3730 0.046 Uiso 1 1 calc R . . C30 C 0.96823(10) 0.20468(16) 0.63143(10) 0.0342(4) Uani 1 1 d . . . H30A H 1.0007 0.2085 0.6033 0.051 Uiso 1 1 calc R . . H30B H 0.9916 0.1815 0.6790 0.051 Uiso 1 1 calc R . . H30C H 0.9479 0.2772 0.6328 0.051 Uiso 1 1 calc R . . C31 C 0.91329(9) 0.12224(14) 0.59917(9) 0.0261(3) Uani 1 1 d . . . C32 C 0.90394(9) 0.03702(15) 0.64308(9) 0.0289(4) Uani 1 1 d . . . H32 H 0.9330 0.0393 0.6892 0.035 Uiso 1 1 calc R . . C33 C 0.85803(9) -0.05168(14) 0.62939(9) 0.0257(3) Uani 1 1 d . . . C34 C 0.86049(12) -0.13090(17) 0.68860(10) 0.0380(5) Uani 1 1 d . . . H34A H 0.8152 -0.1388 0.6952 0.057 Uiso 1 1 calc R . . H34B H 0.8914 -0.1026 0.7316 0.057 Uiso 1 1 calc R . . H34C H 0.8765 -0.2026 0.6773 0.057 Uiso 1 1 calc R . . C35 C 0.89150(8) 0.23194(13) 0.49697(9) 0.0217(3) Uani 1 1 d . . . C36 C 0.85636(8) 0.32930(14) 0.50097(9) 0.0222(3) Uani 1 1 d . . . C37 C 0.87086(8) 0.42266(14) 0.46714(9) 0.0240(3) Uani 1 1 d . . . H37 H 0.8471 0.4888 0.4698 0.029 Uiso 1 1 calc R . . C38 C 0.91915(8) 0.42222(14) 0.42950(9) 0.0238(3) Uani 1 1 d . . . C39 C 0.95160(8) 0.32387(14) 0.42436(9) 0.0247(3) Uani 1 1 d . . . H39 H 0.9838 0.3217 0.3978 0.030 Uiso 1 1 calc R . . C40 C 0.93840(8) 0.22811(14) 0.45694(9) 0.0245(3) Uani 1 1 d . . . C41 C 0.80340(9) 0.33272(15) 0.54083(10) 0.0286(3) Uani 1 1 d . . . H41A H 0.7899 0.4091 0.5452 0.043 Uiso 1 1 calc R . . H41B H 0.8220 0.3014 0.5875 0.043 Uiso 1 1 calc R . . H41C H 0.7639 0.2899 0.5157 0.043 Uiso 1 1 calc R . . C42 C 0.93593(10) 0.52553(16) 0.39586(11) 0.0325(4) Uani 1 1 d . . . H42A H 0.9766 0.5591 0.4263 0.049 Uiso 1 1 calc R . . H42B H 0.8981 0.5772 0.3887 0.049 Uiso 1 1 calc R . . H42C H 0.9439 0.5074 0.3507 0.049 Uiso 1 1 calc R . . C43 C 0.97508(9) 0.12317(15) 0.45026(13) 0.0348(4) Uani 1 1 d . . . H43A H 0.9985 0.1316 0.4136 0.052 Uiso 1 1 calc R . . H43B H 0.9425 0.0628 0.4380 0.052 Uiso 1 1 calc R . . H43C H 1.0081 0.1069 0.4948 0.052 Uiso 1 1 calc R . . C44 C 0.77017(8) -0.16207(13) 0.55685(8) 0.0206(3) Uani 1 1 d . . . C45 C 0.70320(9) -0.14912(14) 0.56037(9) 0.0242(3) Uani 1 1 d . . . C46 C 0.65846(8) -0.23660(15) 0.54102(9) 0.0258(3) Uani 1 1 d . . . H46 H 0.6132 -0.2280 0.5435 0.031 Uiso 1 1 calc R . . C47 C 0.67801(8) -0.33614(14) 0.51821(9) 0.0246(3) Uani 1 1 d . . . C48 C 0.74476(9) -0.34719(13) 0.51645(9) 0.0240(3) Uani 1 1 d . . . H48 H 0.7591 -0.4151 0.5016 0.029 Uiso 1 1 calc R . . C49 C 0.79149(8) -0.26243(13) 0.53567(9) 0.0224(3) Uani 1 1 d . . . C50 C 0.68004(10) -0.04119(16) 0.58316(11) 0.0337(4) Uani 1 1 d . . . H50A H 0.6327 -0.0474 0.5841 0.051 Uiso 1 1 calc R . . H50B H 0.6842 0.0166 0.5502 0.051 Uiso 1 1 calc R . . H50C H 0.7081 -0.0226 0.6300 0.051 Uiso 1 1 calc R . . C51 C 0.62816(9) -0.42822(16) 0.49357(11) 0.0326(4) Uani 1 1 d . . . H51A H 0.6124 -0.4272 0.4424 0.049 Uiso 1 1 calc R . . H51B H 0.5896 -0.4186 0.5132 0.049 Uiso 1 1 calc R . . H51C H 0.6501 -0.4987 0.5091 0.049 Uiso 1 1 calc R . . C52 C 0.86306(9) -0.27907(15) 0.53182(10) 0.0293(4) Uani 1 1 d . . . H52A H 0.8795 -0.3506 0.5519 0.044 Uiso 1 1 calc R . . H52B H 0.8919 -0.2208 0.5581 0.044 Uiso 1 1 calc R . . H52C H 0.8644 -0.2766 0.4829 0.044 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 Ge1 0.01728(9) 0.02204(9) 0.01988(9) -0.00156(6) 0.00466(6) 0.00086(6) Mg1 0.0196(2) 0.0203(3) 0.0212(3) 0.0015(2) 0.0027(2) -0.00359(19) N1 0.0170(6) 0.0205(6) 0.0210(6) -0.0005(5) 0.0059(5) 0.0000(5) C1 0.0190(7) 0.0245(7) 0.0226(7) -0.0026(6) 0.0071(6) 0.0014(6) N2 0.0185(6) 0.0232(6) 0.0222(6) 0.0000(5) 0.0044(5) -0.0001(5) C2 0.0161(6) 0.0282(8) 0.0233(7) 0.0004(6) 0.0064(6) 0.0025(6) N3 0.0209(6) 0.0195(6) 0.0270(7) 0.0026(5) 0.0024(5) -0.0036(5) C3 0.0182(7) 0.0206(7) 0.0205(7) -0.0009(6) 0.0062(5) -0.0007(5) N4 0.0248(6) 0.0188(6) 0.0221(6) 0.0005(5) 0.0047(5) -0.0027(5) C4 0.0226(7) 0.0340(9) 0.0231(7) 0.0000(7) 0.0094(6) 0.0060(6) C5 0.096(2) 0.0348(12) 0.0786(19) -0.0038(12) 0.0644(18) 0.0110(13) C6 0.0221(9) 0.134(3) 0.0287(10) -0.0089(13) 0.0118(8) -0.0004(12) C7 0.0414(11) 0.0567(13) 0.0258(9) 0.0047(9) 0.0176(8) 0.0172(9) C8 0.0191(7) 0.0276(8) 0.0199(7) 0.0018(6) 0.0063(5) 0.0012(6) C9 0.0232(8) 0.0342(9) 0.0231(8) -0.0016(7) 0.0041(6) -0.0012(6) C10 0.0265(8) 0.0272(8) 0.0279(8) 0.0049(7) 0.0082(6) 0.0010(6) C11 0.0226(7) 0.0408(10) 0.0229(7) 0.0049(7) 0.0097(6) 0.0038(7) C12 0.0174(6) 0.0222(7) 0.0193(7) 0.0007(6) 0.0057(5) 0.0022(5) C13 0.0187(7) 0.0236(7) 0.0234(7) 0.0004(6) 0.0061(6) 0.0003(6) C14 0.0183(7) 0.0305(9) 0.0279(8) 0.0030(7) 0.0077(6) 0.0010(6) C15 0.0219(7) 0.0325(9) 0.0256(8) 0.0041(7) 0.0098(6) 0.0076(6) C16 0.0294(8) 0.0244(8) 0.0232(7) 0.0001(6) 0.0098(6) 0.0057(6) C17 0.0219(7) 0.0228(7) 0.0198(7) 0.0007(6) 0.0057(6) 0.0010(6) C18 0.0231(7) 0.0251(8) 0.0352(9) -0.0038(7) 0.0090(7) -0.0039(6) C19 0.0285(9) 0.0445(11) 0.0412(10) 0.0021(9) 0.0175(8) 0.0109(8) C20 0.0279(8) 0.0248(8) 0.0233(7) -0.0031(6) 0.0056(6) -0.0029(6) C21 0.0226(7) 0.0213(7) 0.0195(7) 0.0012(6) 0.0042(6) 0.0008(6) C22 0.0235(7) 0.0269(8) 0.0222(7) 0.0016(6) 0.0053(6) 0.0035(6) C23 0.0344(9) 0.0293(9) 0.0257(8) -0.0008(7) 0.0076(7) 0.0087(7) C24 0.0452(11) 0.0244(8) 0.0250(8) -0.0011(7) 0.0065(7) 0.0015(7) C25 0.0335(9) 0.0258(8) 0.0250(8) 0.0011(7) 0.0034(7) -0.0055(7) C26 0.0233(7) 0.0252(8) 0.0229(7) 0.0026(6) 0.0042(6) -0.0018(6) C27 0.0203(7) 0.0360(9) 0.0304(8) 0.0002(7) 0.0074(6) 0.0039(7) C28 0.0646(15) 0.0273(10) 0.0456(12) -0.0092(9) 0.0108(11) 0.0014(10) C29 0.0219(8) 0.0302(9) 0.0403(10) 0.0030(8) 0.0083(7) -0.0048(7) C30 0.0313(9) 0.0289(9) 0.0345(9) 0.0024(8) -0.0046(7) -0.0092(7) C31 0.0241(8) 0.0221(8) 0.0285(8) 0.0001(6) 0.0010(6) -0.0023(6) C32 0.0318(9) 0.0255(8) 0.0240(8) 0.0013(7) -0.0018(6) -0.0047(7) C33 0.0310(8) 0.0224(8) 0.0215(7) 0.0018(6) 0.0030(6) -0.0018(6) C34 0.0515(12) 0.0318(10) 0.0248(9) 0.0068(7) 0.0004(8) -0.0115(8) C35 0.0181(7) 0.0194(7) 0.0260(7) 0.0011(6) 0.0031(6) -0.0038(5) C36 0.0211(7) 0.0214(7) 0.0246(7) -0.0012(6) 0.0072(6) -0.0028(6) C37 0.0245(7) 0.0203(7) 0.0287(8) 0.0005(6) 0.0096(6) 0.0003(6) C38 0.0206(7) 0.0234(8) 0.0275(8) 0.0030(6) 0.0066(6) -0.0016(6) C39 0.0178(7) 0.0254(8) 0.0323(8) 0.0030(7) 0.0090(6) -0.0009(6) C40 0.0164(7) 0.0214(7) 0.0349(9) 0.0013(7) 0.0054(6) -0.0001(6) C41 0.0319(9) 0.0257(8) 0.0326(9) -0.0010(7) 0.0165(7) -0.0014(7) C42 0.0321(9) 0.0280(9) 0.0413(10) 0.0079(8) 0.0165(8) 0.0009(7) C43 0.0247(8) 0.0231(8) 0.0598(13) 0.0021(8) 0.0165(8) 0.0029(6) C44 0.0240(7) 0.0179(7) 0.0202(7) 0.0019(6) 0.0063(6) -0.0022(6) C45 0.0277(8) 0.0235(8) 0.0245(8) 0.0020(6) 0.0124(6) 0.0009(6) C46 0.0224(7) 0.0291(8) 0.0288(8) 0.0039(7) 0.0117(6) -0.0015(6) C47 0.0236(7) 0.0231(8) 0.0263(8) 0.0044(6) 0.0056(6) -0.0043(6) C48 0.0251(8) 0.0188(7) 0.0275(8) 0.0010(6) 0.0060(6) 0.0001(6) C49 0.0210(7) 0.0205(7) 0.0254(7) 0.0025(6) 0.0057(6) 0.0001(6) C50 0.0376(10) 0.0306(9) 0.0390(10) -0.0040(8) 0.0206(8) 0.0034(7) C51 0.0279(8) 0.0287(9) 0.0386(10) 0.0041(8) 0.0047(7) -0.0087(7) C52 0.0216(8) 0.0256(8) 0.0405(10) 0.0023(7) 0.0079(7) 0.0013(6) _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 Ge1 N2 1.8477(14) . ? Ge1 C1 2.0079(17) . ? Ge1 N1 2.0402(14) . ? Mg1 N2 1.9504(16) . ? Mg1 N4 2.0206(15) . ? Mg1 N3 2.0216(15) . ? N1 C3 1.311(2) . ? N1 C12 1.4312(19) . ? C1 C2 1.356(2) . ? C1 C4 1.526(2) . ? N2 C21 1.407(2) . ? C2 C3 1.451(2) . ? C2 H2 0.9500 . ? N3 C31 1.339(2) . ? N3 C35 1.438(2) . ? C3 C8 1.528(2) . ? N4 C33 1.325(2) . ? N4 C44 1.436(2) . ? C4 C7 1.524(3) . ? C4 C5 1.528(3) . ? C4 C6 1.529(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C11 1.533(2) . ? C8 C9 1.539(2) . ? C8 C10 1.550(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.403(2) . ? C12 C13 1.403(2) . ? C13 C14 1.395(2) . ? C13 C18 1.505(2) . ? C14 C15 1.389(3) . ? C14 H14 0.9500 . ? C15 C16 1.390(3) . ? C15 C19 1.508(2) . ? C16 C17 1.396(2) . ? C16 H16 0.9500 . ? C17 C20 1.508(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 C26 1.416(2) . ? C21 C22 1.417(2) . ? C22 C23 1.394(2) . ? C22 C27 1.511(2) . ? C23 C24 1.391(3) . ? C23 H23 0.9500 . ? C24 C25 1.391(3) . ? C24 C28 1.509(3) . ? C25 C26 1.388(3) . ? C25 H25 0.9500 . ? C26 C29 1.499(2) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.517(2) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.402(2) . ? C32 C33 1.411(2) . ? C32 H32 0.9500 . ? C33 C34 1.511(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.401(2) . ? C35 C40 1.405(2) . ? C36 C37 1.393(2) . ? C36 C41 1.509(2) . ? C37 C38 1.394(2) . ? C37 H37 0.9500 . ? C38 C39 1.387(2) . ? C38 C42 1.507(2) . ? C39 C40 1.395(2) . ? C39 H39 0.9500 . ? C40 C43 1.507(2) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C49 1.400(2) . ? C44 C45 1.405(2) . ? C45 C46 1.392(2) . ? C45 C50 1.508(2) . ? C46 C47 1.390(2) . ? C46 H46 0.9500 . ? C47 C48 1.388(2) . ? C47 C51 1.508(2) . ? C48 C49 1.391(2) . ? C48 H48 0.9500 . ? C49 C52 1.507(2) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 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 N2 Ge1 C1 123.24(6) . . ? N2 Ge1 N1 103.54(6) . . ? C1 Ge1 N1 81.96(7) . . ? N2 Mg1 N4 116.69(6) . . ? N2 Mg1 N3 148.64(7) . . ? N4 Mg1 N3 94.65(6) . . ? C3 N1 C12 127.07(14) . . ? C3 N1 Ge1 112.63(11) . . ? C12 N1 Ge1 120.18(10) . . ? C2 C1 C4 119.81(14) . . ? C2 C1 Ge1 108.75(11) . . ? C4 C1 Ge1 126.06(12) . . ? C21 N2 Ge1 133.16(11) . . ? C21 N2 Mg1 118.47(11) . . ? Ge1 N2 Mg1 106.82(7) . . ? C1 C2 C3 119.71(14) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C31 N3 C35 117.15(14) . . ? C31 N3 Mg1 122.42(12) . . ? C35 N3 Mg1 120.09(11) . . ? N1 C3 C2 113.93(14) . . ? N1 C3 C8 128.60(14) . . ? C2 C3 C8 117.25(13) . . ? C33 N4 C44 120.34(14) . . ? C33 N4 Mg1 124.33(12) . . ? C44 N4 Mg1 115.28(10) . . ? C7 C4 C1 111.99(14) . . ? C7 C4 C5 108.20(18) . . ? C1 C4 C5 108.42(16) . . ? C7 C4 C6 107.71(18) . . ? C1 C4 C6 111.04(15) . . ? C5 C4 C6 109.4(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 C11 116.82(13) . . ? C3 C8 C9 108.48(13) . . ? C11 C8 C9 108.36(14) . . ? C3 C8 C10 106.72(13) . . ? C11 C8 C10 106.64(14) . . ? C9 C8 C10 109.68(14) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 121.44(14) . . ? C17 C12 N1 118.83(14) . . ? C13 C12 N1 119.65(14) . . ? C14 C13 C12 118.07(15) . . ? C14 C13 C18 120.30(15) . . ? C12 C13 C18 121.56(14) . . ? C15 C14 C13 121.97(16) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C14 C15 C16 118.52(15) . . ? C14 C15 C19 120.58(17) . . ? C16 C15 C19 120.86(17) . . ? C15 C16 C17 121.92(16) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C16 C17 C12 118.08(15) . . ? C16 C17 C20 119.73(15) . . ? C12 C17 C20 122.14(14) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 C26 123.43(15) . . ? N2 C21 C22 119.29(15) . . ? C26 C21 C22 117.13(16) . . ? C23 C22 C21 120.80(16) . . ? C23 C22 C27 119.23(16) . . ? C21 C22 C27 119.96(16) . . ? C24 C23 C22 121.91(17) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 117.16(17) . . ? C23 C24 C28 121.31(19) . . ? C25 C24 C28 121.51(19) . . ? C26 C25 C24 122.70(17) . . ? C26 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? C25 C26 C21 120.29(16) . . ? C25 C26 C29 120.07(16) . . ? C21 C26 C29 119.63(16) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 C32 125.05(16) . . ? N3 C31 C30 119.02(16) . . ? C32 C31 C30 115.93(16) . . ? C31 C32 C33 129.99(16) . . ? C31 C32 H32 115.0 . . ? C33 C32 H32 115.0 . . ? N4 C33 C32 123.22(16) . . ? N4 C33 C34 119.57(16) . . ? C32 C33 C34 117.21(16) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 120.16(15) . . ? C36 C35 N3 119.13(14) . . ? C40 C35 N3 120.69(15) . . ? C37 C36 C35 118.84(15) . . ? C37 C36 C41 120.59(15) . . ? C35 C36 C41 120.57(15) . . ? C36 C37 C38 122.09(15) . . ? C36 C37 H37 119.0 . . ? C38 C37 H37 119.0 . . ? C39 C38 C37 117.93(15) . . ? C39 C38 C42 121.03(15) . . ? C37 C38 C42 121.03(15) . . ? C38 C39 C40 121.97(15) . . ? C38 C39 H39 119.0 . . ? C40 C39 H39 119.0 . . ? C39 C40 C35 118.91(15) . . ? C39 C40 C43 120.20(16) . . ? C35 C40 C43 120.87(16) . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 H42A 109.5 . . ? C38 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C38 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C49 C44 C45 120.16(15) . . ? C49 C44 N4 120.56(14) . . ? C45 C44 N4 118.94(14) . . ? C46 C45 C44 118.91(15) . . ? C46 C45 C50 120.74(16) . . ? C44 C45 C50 120.33(16) . . ? C47 C46 C45 121.97(15) . . ? C47 C46 H46 119.0 . . ? C45 C46 H46 119.0 . . ? C48 C47 C46 117.83(15) . . ? C48 C47 C51 120.61(16) . . ? C46 C47 C51 121.52(16) . . ? C47 C48 C49 122.35(16) . . ? C47 C48 H48 118.8 . . ? C49 C48 H48 118.8 . . ? C48 C49 C44 118.75(15) . . ? C48 C49 C52 119.84(15) . . ? C44 C49 C52 121.40(15) . . ? C45 C50 H50A 109.5 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C47 C51 H51A 109.5 . . ? C47 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C47 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.539 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.066 # Attachment '(tBuMesNac)2Pb.CIF' data_(tBuMesNac)2Pb _database_code_depnum_ccdc_archive 'CCDC 859475' #TrackingRef '(tBuMesNac)2Pb.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H96 N4 Pb' _chemical_formula_weight 1128.64 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6557(4) _cell_length_b 12.1595(4) _cell_length_c 22.2271(8) _cell_angle_alpha 74.160(3) _cell_angle_beta 76.098(3) _cell_angle_gamma 86.034(2) _cell_volume 2941.78(18) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 2.908 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.756 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19383 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10856 _reflns_number_gt 9340 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One half of a molecule of hexane of crystallisation, sitting on an inversion centre, was located in the asymmetric unit and its carbon atoms refined isotropically. ; _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^)+(0.0295P)^2^+2.0039P] 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 10856 _refine_ls_number_parameters 618 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.232260(15) 0.244360(14) 0.233990(9) 0.01551(6) Uani 1 1 d . . . N1 N 0.1429(3) 0.2867(3) 0.13788(19) 0.0179(9) Uani 1 1 d . . . N2 N 0.2260(3) 0.0627(3) 0.21513(18) 0.0156(8) Uani 1 1 d . . . N3 N 0.2961(3) 0.2874(3) 0.33046(18) 0.0156(8) Uani 1 1 d . . . N4 N 0.4405(3) 0.2932(3) 0.19625(18) 0.0163(8) Uani 1 1 d . . . C1 C 0.1418(4) 0.2226(4) 0.0992(2) 0.0167(10) Uani 1 1 d . . . C2 C 0.2145(4) 0.1209(4) 0.1037(2) 0.0169(10) Uani 1 1 d . . . H2 H 0.2468 0.1040 0.0637 0.020 Uiso 1 1 calc R . . C3 C 0.2452(4) 0.0444(4) 0.1553(2) 0.0176(10) Uani 1 1 d . . . C4 C 0.0733(4) 0.2467(4) 0.0459(2) 0.0202(10) Uani 1 1 d . . . C5 C 0.0059(5) 0.1386(4) 0.0512(3) 0.0314(13) Uani 1 1 d . . . H5A H -0.0362 0.1537 0.0165 0.047 Uiso 1 1 calc R . . H5B H -0.0510 0.1177 0.0928 0.047 Uiso 1 1 calc R . . H5C H 0.0620 0.0756 0.0475 0.047 Uiso 1 1 calc R . . C6 C 0.1617(5) 0.2790(4) -0.0195(2) 0.0297(12) Uani 1 1 d . . . H6A H 0.2084 0.3448 -0.0219 0.045 Uiso 1 1 calc R . . H6B H 0.1187 0.2989 -0.0539 0.045 Uiso 1 1 calc R . . H6C H 0.2144 0.2141 -0.0243 0.045 Uiso 1 1 calc R . . C7 C -0.0191(5) 0.3425(4) 0.0476(3) 0.0313(13) Uani 1 1 d . . . H7A H 0.0202 0.4146 0.0416 0.047 Uiso 1 1 calc R . . H7B H -0.0763 0.3240 0.0892 0.047 Uiso 1 1 calc R . . H7C H -0.0602 0.3500 0.0130 0.047 Uiso 1 1 calc R . . C8 C 0.3073(4) -0.0700(4) 0.1435(2) 0.0207(11) Uani 1 1 d . . . C9 C 0.2155(4) -0.1636(4) 0.1566(3) 0.0331(13) Uani 1 1 d . . . H9A H 0.1559 -0.1345 0.1316 0.050 Uiso 1 1 calc R . . H9B H 0.1771 -0.1855 0.2025 0.050 Uiso 1 1 calc R . . H9C H 0.2550 -0.2304 0.1440 0.050 Uiso 1 1 calc R . . C10 C 0.3768(5) -0.0505(4) 0.0736(3) 0.0322(13) Uani 1 1 d . . . H10A H 0.4265 -0.1175 0.0691 0.048 Uiso 1 1 calc R . . H10B H 0.4269 0.0171 0.0616 0.048 Uiso 1 1 calc R . . H10C H 0.3216 -0.0388 0.0454 0.048 Uiso 1 1 calc R . . C11 C 0.3952(4) -0.1142(4) 0.1861(3) 0.0267(12) Uani 1 1 d . . . H11A H 0.3522 -0.1393 0.2311 0.040 Uiso 1 1 calc R . . H11B H 0.4499 -0.0528 0.1810 0.040 Uiso 1 1 calc R . . H11C H 0.4399 -0.1787 0.1733 0.040 Uiso 1 1 calc R . . C12 C 0.0747(4) 0.3859(4) 0.1468(2) 0.0172(10) Uani 1 1 d . . . C13 C -0.0274(4) 0.3746(4) 0.1956(2) 0.0195(10) Uani 1 1 d . . . C14 C -0.0803(4) 0.4731(4) 0.2105(2) 0.0236(11) Uani 1 1 d . . . H14 H -0.1509 0.4659 0.2433 0.028 Uiso 1 1 calc R . . C15 C -0.0337(4) 0.5817(4) 0.1791(3) 0.0247(12) Uani 1 1 d . . . C16 C 0.0690(4) 0.5893(4) 0.1314(2) 0.0230(11) Uani 1 1 d . . . H16 H 0.1017 0.6628 0.1092 0.028 Uiso 1 1 calc R . . C17 C 0.1260(4) 0.4948(4) 0.1147(2) 0.0195(10) Uani 1 1 d . . . C18 C -0.0823(4) 0.2600(4) 0.2314(2) 0.0259(12) Uani 1 1 d . . . H18A H -0.1128 0.2286 0.2021 0.039 Uiso 1 1 calc R . . H18B H -0.1473 0.2687 0.2670 0.039 Uiso 1 1 calc R . . H18C H -0.0226 0.2079 0.2482 0.039 Uiso 1 1 calc R . . C19 C -0.0907(5) 0.6868(5) 0.1981(3) 0.0397(15) Uani 1 1 d . . . H19A H -0.0557 0.7014 0.2311 0.060 Uiso 1 1 calc R . . H19B H -0.1758 0.6741 0.2152 0.060 Uiso 1 1 calc R . . H19C H -0.0774 0.7528 0.1604 0.060 Uiso 1 1 calc R . . C20 C 0.2401(4) 0.5078(4) 0.0646(3) 0.0293(12) Uani 1 1 d . . . H20A H 0.3038 0.4696 0.0844 0.044 Uiso 1 1 calc R . . H20B H 0.2585 0.5892 0.0458 0.044 Uiso 1 1 calc R . . H20C H 0.2323 0.4732 0.0308 0.044 Uiso 1 1 calc R . . C21 C 0.1803(4) -0.0239(4) 0.2727(2) 0.0167(10) Uani 1 1 d . . . C22 C 0.2393(4) -0.0551(4) 0.3233(2) 0.0183(10) Uani 1 1 d . . . C23 C 0.1889(4) -0.1333(4) 0.3799(2) 0.0242(11) Uani 1 1 d . . . H23 H 0.2306 -0.1540 0.4133 0.029 Uiso 1 1 calc R . . C24 C 0.0790(4) -0.1832(4) 0.3902(2) 0.0260(12) Uani 1 1 d . . . C25 C 0.0208(4) -0.1481(4) 0.3413(2) 0.0241(12) Uani 1 1 d . . . H25 H -0.0549 -0.1796 0.3476 0.029 Uiso 1 1 calc R . . C26 C 0.0661(4) -0.0692(4) 0.2832(2) 0.0205(11) Uani 1 1 d . . . C27 C 0.3560(4) -0.0015(4) 0.3171(3) 0.0247(11) Uani 1 1 d . . . H27A H 0.3422 0.0754 0.3234 0.037 Uiso 1 1 calc R . . H27B H 0.4060 0.0033 0.2741 0.037 Uiso 1 1 calc R . . H27C H 0.3956 -0.0485 0.3496 0.037 Uiso 1 1 calc R . . C28 C 0.0261(5) -0.2685(4) 0.4524(3) 0.0398(15) Uani 1 1 d . . . H28A H -0.0183 -0.2280 0.4833 0.060 Uiso 1 1 calc R . . H28B H 0.0894 -0.3136 0.4698 0.060 Uiso 1 1 calc R . . H28C H -0.0271 -0.3194 0.4447 0.060 Uiso 1 1 calc R . . C29 C -0.0095(4) -0.0312(4) 0.2349(3) 0.0276(12) Uani 1 1 d . . . H29A H -0.0054 -0.0885 0.2108 0.041 Uiso 1 1 calc R . . H29B H 0.0193 0.0422 0.2051 0.041 Uiso 1 1 calc R . . H29C H -0.0916 -0.0227 0.2574 0.041 Uiso 1 1 calc R . . C30 C 0.3000(4) 0.3988(4) 0.3050(2) 0.0172(10) Uani 1 1 d . . . C31 C 0.3585(4) 0.4462(4) 0.2401(2) 0.0178(10) Uani 1 1 d . . . H31 H 0.3326 0.5202 0.2205 0.021 Uiso 1 1 calc R . . C32 C 0.4513(4) 0.3976(3) 0.2003(2) 0.0135(9) Uani 1 1 d . . . C33 C 0.2335(4) 0.4878(4) 0.3409(2) 0.0216(11) Uani 1 1 d . . . C34 C 0.1736(4) 0.4361(4) 0.4110(2) 0.0266(12) Uani 1 1 d . . . H34A H 0.1301 0.4959 0.4292 0.040 Uiso 1 1 calc R . . H34B H 0.2335 0.4026 0.4350 0.040 Uiso 1 1 calc R . . H34C H 0.1185 0.3765 0.4139 0.040 Uiso 1 1 calc R . . C35 C 0.1356(4) 0.5410(4) 0.3058(3) 0.0307(13) Uani 1 1 d . . . H35A H 0.0815 0.4810 0.3082 0.046 Uiso 1 1 calc R . . H35B H 0.1714 0.5779 0.2607 0.046 Uiso 1 1 calc R . . H35C H 0.0917 0.5980 0.3263 0.046 Uiso 1 1 calc R . . C36 C 0.3175(5) 0.5831(4) 0.3377(3) 0.0346(14) Uani 1 1 d . . . H36A H 0.2746 0.6352 0.3622 0.052 Uiso 1 1 calc R . . H36B H 0.3471 0.6257 0.2928 0.052 Uiso 1 1 calc R . . H36C H 0.3842 0.5488 0.3562 0.052 Uiso 1 1 calc R . . C37 C 0.5583(4) 0.4783(4) 0.1641(2) 0.0189(10) Uani 1 1 d . . . C38 C 0.5965(4) 0.5319(4) 0.2118(3) 0.0305(13) Uani 1 1 d . . . H38A H 0.6158 0.4710 0.2471 0.046 Uiso 1 1 calc R . . H38B H 0.5317 0.5787 0.2290 0.046 Uiso 1 1 calc R . . H38C H 0.6662 0.5800 0.1894 0.046 Uiso 1 1 calc R . . C39 C 0.6687(4) 0.4245(4) 0.1307(2) 0.0226(11) Uani 1 1 d . . . H39A H 0.7315 0.4818 0.1119 0.034 Uiso 1 1 calc R . . H39B H 0.6505 0.3966 0.0966 0.034 Uiso 1 1 calc R . . H39C H 0.6951 0.3604 0.1620 0.034 Uiso 1 1 calc R . . C40 C 0.5173(4) 0.5752(4) 0.1125(3) 0.0305(13) Uani 1 1 d . . . H40A H 0.5821 0.6294 0.0904 0.046 Uiso 1 1 calc R . . H40B H 0.4496 0.6150 0.1331 0.046 Uiso 1 1 calc R . . H40C H 0.4941 0.5429 0.0814 0.046 Uiso 1 1 calc R . . C41 C 0.2825(4) 0.2225(4) 0.3949(2) 0.0183(10) Uani 1 1 d . . . C42 C 0.3723(4) 0.2183(4) 0.4279(3) 0.0260(12) Uani 1 1 d . . . C43 C 0.3655(5) 0.1367(5) 0.4869(3) 0.0339(13) Uani 1 1 d . . . H43 H 0.4273 0.1328 0.5085 0.041 Uiso 1 1 calc R . . C44 C 0.2720(5) 0.0619(4) 0.5146(3) 0.0371(14) Uani 1 1 d . . . C45 C 0.1821(5) 0.0703(4) 0.4829(3) 0.0304(12) Uani 1 1 d . . . H45 H 0.1163 0.0205 0.5021 0.036 Uiso 1 1 calc R . . C46 C 0.1842(4) 0.1486(4) 0.4242(2) 0.0218(11) Uani 1 1 d . . . C47 C 0.4744(4) 0.3004(5) 0.4018(3) 0.0315(13) Uani 1 1 d . . . H47A H 0.4861 0.3284 0.3550 0.047 Uiso 1 1 calc R . . H47B H 0.5461 0.2611 0.4123 0.047 Uiso 1 1 calc R . . H47C H 0.4573 0.3650 0.4210 0.047 Uiso 1 1 calc R . . C48 C 0.2671(7) -0.0248(5) 0.5788(3) 0.062(2) Uani 1 1 d . . . H48A H 0.2286 0.0097 0.6136 0.092 Uiso 1 1 calc R . . H48B H 0.3476 -0.0484 0.5829 0.092 Uiso 1 1 calc R . . H48C H 0.2220 -0.0917 0.5813 0.092 Uiso 1 1 calc R . . C49 C 0.0804(4) 0.1550(4) 0.3933(3) 0.0268(12) Uani 1 1 d . . . H49A H 0.0953 0.1051 0.3643 0.040 Uiso 1 1 calc R . . H49B H 0.0703 0.2339 0.3689 0.040 Uiso 1 1 calc R . . H49C H 0.0084 0.1302 0.4268 0.040 Uiso 1 1 calc R . . C50 C 0.5301(4) 0.2195(4) 0.1726(2) 0.0157(10) Uani 1 1 d . . . C51 C 0.5992(4) 0.1545(4) 0.2127(2) 0.0210(11) Uani 1 1 d . . . C52 C 0.6755(4) 0.0719(4) 0.1915(3) 0.0241(11) Uani 1 1 d . . . H52 H 0.7230 0.0276 0.2187 0.029 Uiso 1 1 calc R . . C53 C 0.6838(4) 0.0529(4) 0.1321(3) 0.0271(12) Uani 1 1 d . . . C54 C 0.6190(4) 0.1223(4) 0.0919(2) 0.0228(11) Uani 1 1 d . . . H54 H 0.6290 0.1142 0.0496 0.027 Uiso 1 1 calc R . . C55 C 0.5393(4) 0.2040(4) 0.1111(2) 0.0184(10) Uani 1 1 d . . . C56 C 0.5944(4) 0.1737(4) 0.2771(2) 0.0275(12) Uani 1 1 d . . . H56A H 0.6383 0.2431 0.2713 0.041 Uiso 1 1 calc R . . H56B H 0.6299 0.1081 0.3032 0.041 Uiso 1 1 calc R . . H56C H 0.5119 0.1824 0.2988 0.041 Uiso 1 1 calc R . . C57 C 0.7590(5) -0.0437(4) 0.1125(3) 0.0401(15) Uani 1 1 d . . . H57A H 0.7105 -0.1124 0.1245 0.060 Uiso 1 1 calc R . . H57B H 0.8243 -0.0594 0.1344 0.060 Uiso 1 1 calc R . . H57C H 0.7909 -0.0218 0.0659 0.060 Uiso 1 1 calc R . . C58 C 0.4711(4) 0.2776(4) 0.0655(2) 0.0237(11) Uani 1 1 d . . . H58A H 0.4970 0.3571 0.0541 0.036 Uiso 1 1 calc R . . H58B H 0.3865 0.2727 0.0860 0.036 Uiso 1 1 calc R . . H58C H 0.4852 0.2511 0.0264 0.036 Uiso 1 1 calc R . . C59 C 0.5859(8) -0.2323(8) 0.3082(4) 0.108(3) Uiso 1 1 d DU . . H59A H 0.6193 -0.2879 0.2840 0.162 Uiso 1 1 calc R . . H59B H 0.5859 -0.1562 0.2784 0.162 Uiso 1 1 calc R . . H59C H 0.5047 -0.2539 0.3317 0.162 Uiso 1 1 calc R . . C60 C 0.6582(10) -0.2305(7) 0.3543(5) 0.139(4) Uiso 1 1 d DU . . H60A H 0.6317 -0.1658 0.3734 0.167 Uiso 1 1 calc R . . H60B H 0.7416 -0.2165 0.3306 0.167 Uiso 1 1 calc R . . C61 C 0.6517(11) -0.3395(8) 0.4080(5) 0.172(5) Uiso 1 1 d DU . . H61A H 0.6852 -0.3252 0.4420 0.206 Uiso 1 1 calc R . . H61B H 0.5678 -0.3609 0.4269 0.206 Uiso 1 1 calc R . . C62 C 0.7156(11) -0.4355(7) 0.3863(5) 0.141(4) Uiso 1 1 d DU . . H62A H 0.7927 -0.4071 0.3576 0.170 Uiso 1 1 calc R . . H62B H 0.6701 -0.4612 0.3603 0.170 Uiso 1 1 calc R . . C63 C 0.7382(10) -0.5382(8) 0.4387(5) 0.140(4) Uiso 1 1 d DU . . H63A H 0.7904 -0.5159 0.4625 0.167 Uiso 1 1 calc R . . H63B H 0.6624 -0.5649 0.4694 0.167 Uiso 1 1 calc R . . C64 C 0.7946(8) -0.6330(7) 0.4111(4) 0.096(3) Uiso 1 1 d DU . . H64A H 0.7517 -0.6444 0.3804 0.144 Uiso 1 1 calc R . . H64B H 0.7922 -0.7035 0.4458 0.144 Uiso 1 1 calc R . . H64C H 0.8769 -0.6134 0.3891 0.144 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 0.01530(10) 0.01533(9) 0.01695(10) -0.00525(7) -0.00479(7) 0.00061(6) N1 0.015(2) 0.0156(19) 0.022(2) -0.0054(17) -0.0014(17) 0.0017(15) N2 0.017(2) 0.0153(19) 0.012(2) 0.0004(16) -0.0033(17) 0.0010(15) N3 0.016(2) 0.0144(19) 0.017(2) -0.0017(17) -0.0068(17) -0.0001(15) N4 0.019(2) 0.019(2) 0.012(2) -0.0031(16) -0.0057(17) 0.0009(15) C1 0.019(3) 0.013(2) 0.017(3) -0.003(2) -0.004(2) -0.0016(18) C2 0.017(2) 0.017(2) 0.015(3) -0.005(2) 0.000(2) 0.0002(18) C3 0.017(2) 0.013(2) 0.023(3) -0.005(2) -0.005(2) -0.0031(18) C4 0.026(3) 0.021(2) 0.015(3) -0.003(2) -0.008(2) -0.0009(19) C5 0.036(3) 0.030(3) 0.034(3) -0.008(3) -0.019(3) -0.005(2) C6 0.038(3) 0.032(3) 0.019(3) -0.003(2) -0.011(2) -0.002(2) C7 0.034(3) 0.032(3) 0.036(3) -0.010(3) -0.025(3) 0.010(2) C8 0.023(3) 0.014(2) 0.024(3) -0.005(2) -0.007(2) 0.0043(19) C9 0.035(3) 0.017(3) 0.051(4) -0.015(3) -0.011(3) 0.001(2) C10 0.044(3) 0.029(3) 0.027(3) -0.014(2) -0.012(3) 0.017(2) C11 0.030(3) 0.024(3) 0.028(3) -0.011(2) -0.007(2) 0.009(2) C12 0.020(3) 0.016(2) 0.019(3) -0.007(2) -0.010(2) 0.0033(18) C13 0.013(2) 0.021(2) 0.027(3) -0.006(2) -0.009(2) -0.0011(18) C14 0.018(3) 0.027(3) 0.029(3) -0.012(2) -0.008(2) 0.004(2) C15 0.023(3) 0.025(3) 0.037(3) -0.016(2) -0.020(2) 0.009(2) C16 0.022(3) 0.018(2) 0.033(3) -0.007(2) -0.017(2) 0.0026(19) C17 0.020(3) 0.017(2) 0.026(3) -0.007(2) -0.013(2) 0.0019(18) C18 0.018(3) 0.030(3) 0.030(3) -0.010(2) -0.004(2) 0.004(2) C19 0.042(4) 0.031(3) 0.055(4) -0.025(3) -0.016(3) 0.009(2) C20 0.031(3) 0.017(2) 0.038(3) -0.002(2) -0.008(3) -0.004(2) C21 0.015(2) 0.013(2) 0.021(3) -0.007(2) -0.001(2) 0.0024(17) C22 0.024(3) 0.012(2) 0.019(3) -0.006(2) -0.004(2) 0.0057(18) C23 0.039(3) 0.016(2) 0.015(3) -0.004(2) -0.005(2) 0.009(2) C24 0.035(3) 0.016(2) 0.022(3) -0.003(2) 0.000(2) 0.003(2) C25 0.020(3) 0.017(2) 0.032(3) -0.008(2) 0.003(2) -0.0001(19) C26 0.021(3) 0.014(2) 0.025(3) -0.007(2) -0.003(2) 0.0035(18) C27 0.028(3) 0.022(3) 0.028(3) -0.008(2) -0.013(2) 0.006(2) C28 0.058(4) 0.023(3) 0.025(3) 0.003(2) 0.008(3) 0.000(2) C29 0.022(3) 0.023(3) 0.039(3) -0.010(2) -0.005(2) -0.001(2) C30 0.011(2) 0.018(2) 0.026(3) -0.009(2) -0.006(2) -0.0011(17) C31 0.018(2) 0.012(2) 0.021(3) -0.001(2) -0.003(2) 0.0014(17) C32 0.012(2) 0.013(2) 0.015(3) 0.0001(19) -0.0079(19) 0.0046(17) C33 0.021(3) 0.018(2) 0.025(3) -0.010(2) 0.002(2) -0.0025(19) C34 0.032(3) 0.023(3) 0.024(3) -0.012(2) 0.001(2) 0.004(2) C35 0.028(3) 0.030(3) 0.031(3) -0.009(2) -0.002(3) 0.009(2) C36 0.039(3) 0.025(3) 0.043(4) -0.021(3) 0.002(3) -0.006(2) C37 0.011(2) 0.023(2) 0.019(3) -0.003(2) -0.001(2) -0.0038(18) C38 0.018(3) 0.037(3) 0.039(4) -0.016(3) -0.001(2) -0.006(2) C39 0.017(3) 0.024(3) 0.024(3) -0.003(2) 0.000(2) -0.0040(19) C40 0.026(3) 0.023(3) 0.035(3) 0.002(2) -0.003(2) -0.003(2) C41 0.023(3) 0.019(2) 0.015(3) -0.009(2) -0.003(2) 0.0053(19) C42 0.027(3) 0.029(3) 0.027(3) -0.014(2) -0.011(2) 0.009(2) C43 0.043(4) 0.037(3) 0.027(3) -0.011(3) -0.021(3) 0.016(3) C44 0.058(4) 0.025(3) 0.023(3) 0.001(2) -0.012(3) 0.008(3) C45 0.040(3) 0.021(3) 0.025(3) -0.001(2) -0.002(3) 0.001(2) C46 0.028(3) 0.018(2) 0.017(3) -0.006(2) 0.001(2) 0.002(2) C47 0.027(3) 0.042(3) 0.031(3) -0.011(3) -0.016(3) 0.002(2) C48 0.091(6) 0.050(4) 0.036(4) 0.009(3) -0.025(4) 0.006(4) C49 0.022(3) 0.023(3) 0.034(3) -0.011(2) 0.004(2) -0.006(2) C50 0.015(2) 0.014(2) 0.016(3) -0.0010(19) -0.003(2) -0.0002(17) C51 0.014(2) 0.022(2) 0.025(3) -0.004(2) -0.004(2) -0.0007(19) C52 0.017(3) 0.016(2) 0.036(3) 0.002(2) -0.009(2) 0.0001(18) C53 0.014(3) 0.023(3) 0.045(4) -0.014(3) -0.002(2) -0.001(2) C54 0.019(3) 0.026(3) 0.025(3) -0.012(2) -0.001(2) 0.000(2) C55 0.017(2) 0.020(2) 0.018(3) -0.003(2) -0.005(2) -0.0023(18) C56 0.026(3) 0.033(3) 0.021(3) -0.003(2) -0.007(2) -0.001(2) C57 0.028(3) 0.022(3) 0.072(5) -0.021(3) -0.008(3) 0.008(2) C58 0.023(3) 0.033(3) 0.020(3) -0.009(2) -0.011(2) 0.002(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 N2 2.367(3) . ? Pb1 N4 2.428(4) . ? Pb1 N1 2.511(4) . ? Pb1 N3 2.619(4) . ? N1 C1 1.312(5) . ? N1 C12 1.431(5) . ? N2 C3 1.372(6) . ? N2 C21 1.429(6) . ? N3 C30 1.317(6) . ? N3 C41 1.411(6) . ? N4 C32 1.315(5) . ? N4 C50 1.426(5) . ? C1 C2 1.444(6) . ? C1 C4 1.536(7) . ? C2 C3 1.370(6) . ? C3 C8 1.579(6) . ? C4 C7 1.532(6) . ? C4 C6 1.533(7) . ? C4 C5 1.541(6) . ? C8 C10 1.532(7) . ? C8 C11 1.533(7) . ? C8 C9 1.537(6) . ? C12 C13 1.390(6) . ? C12 C17 1.418(6) . ? C13 C14 1.393(6) . ? C13 C18 1.502(6) . ? C14 C15 1.393(7) . ? C15 C16 1.384(7) . ? C15 C19 1.515(6) . ? C16 C17 1.382(6) . ? C17 C20 1.501(7) . ? C21 C22 1.409(7) . ? C21 C26 1.419(6) . ? C22 C23 1.379(7) . ? C22 C27 1.510(6) . ? C23 C24 1.397(7) . ? C24 C25 1.373(7) . ? C24 C28 1.505(7) . ? C25 C26 1.391(7) . ? C26 C29 1.506(7) . ? C30 C31 1.415(6) . ? C30 C33 1.571(6) . ? C31 C32 1.428(6) . ? C32 C37 1.557(6) . ? C33 C34 1.521(7) . ? C33 C35 1.542(7) . ? C33 C36 1.544(6) . ? C37 C39 1.525(6) . ? C37 C40 1.542(7) . ? C37 C38 1.545(6) . ? C41 C42 1.405(7) . ? C41 C46 1.418(6) . ? C42 C43 1.400(7) . ? C42 C47 1.504(7) . ? C43 C44 1.379(8) . ? C44 C45 1.379(8) . ? C44 C48 1.516(8) . ? C45 C46 1.386(7) . ? C46 C49 1.517(7) . ? C50 C51 1.393(7) . ? C50 C55 1.408(6) . ? C51 C52 1.398(6) . ? C51 C56 1.498(7) . ? C52 C53 1.380(7) . ? C53 C54 1.382(7) . ? C53 C57 1.513(6) . ? C54 C55 1.395(6) . ? C55 C58 1.503(7) . ? C59 C60 1.479(7) . ? C60 C61 1.515(7) . ? C61 C62 1.471(7) . ? C62 C63 1.515(7) . ? C63 C64 1.491(7) . ? 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 N2 Pb1 N4 103.08(12) . . ? N2 Pb1 N1 76.77(12) . . ? N4 Pb1 N1 108.01(12) . . ? N2 Pb1 N3 126.53(12) . . ? N4 Pb1 N3 73.90(11) . . ? N1 Pb1 N3 156.22(11) . . ? C1 N1 C12 130.5(4) . . ? C1 N1 Pb1 128.7(3) . . ? C12 N1 Pb1 99.6(3) . . ? C3 N2 C21 122.4(4) . . ? C3 N2 Pb1 124.3(3) . . ? C21 N2 Pb1 112.5(3) . . ? C30 N3 C41 130.8(4) . . ? C30 N3 Pb1 93.9(3) . . ? C41 N3 Pb1 130.8(3) . . ? C32 N4 C50 128.5(4) . . ? C32 N4 Pb1 107.4(3) . . ? C50 N4 Pb1 124.1(3) . . ? N1 C1 C2 118.9(4) . . ? N1 C1 C4 126.4(4) . . ? C2 C1 C4 114.7(4) . . ? C3 C2 C1 131.7(4) . . ? C2 C3 N2 123.7(4) . . ? C2 C3 C8 116.9(4) . . ? N2 C3 C8 119.4(4) . . ? C7 C4 C6 108.0(4) . . ? C7 C4 C1 115.0(4) . . ? C6 C4 C1 108.7(4) . . ? C7 C4 C5 106.2(4) . . ? C6 C4 C5 109.1(4) . . ? C1 C4 C5 109.7(4) . . ? C10 C8 C11 107.1(4) . . ? C10 C8 C9 107.6(4) . . ? C11 C8 C9 108.8(4) . . ? C10 C8 C3 110.6(4) . . ? C11 C8 C3 111.7(4) . . ? C9 C8 C3 111.0(4) . . ? C13 C12 C17 120.6(4) . . ? C13 C12 N1 119.8(4) . . ? C17 C12 N1 118.2(4) . . ? C12 C13 C14 118.5(4) . . ? C12 C13 C18 121.7(4) . . ? C14 C13 C18 119.8(4) . . ? C13 C14 C15 122.5(5) . . ? C16 C15 C14 117.4(4) . . ? C16 C15 C19 121.4(5) . . ? C14 C15 C19 121.2(5) . . ? C17 C16 C15 122.9(4) . . ? C16 C17 C12 118.2(4) . . ? C16 C17 C20 120.5(4) . . ? C12 C17 C20 121.3(4) . . ? C22 C21 C26 118.3(4) . . ? C22 C21 N2 121.4(4) . . ? C26 C21 N2 119.8(4) . . ? C23 C22 C21 120.0(4) . . ? C23 C22 C27 119.3(5) . . ? C21 C22 C27 120.7(4) . . ? C22 C23 C24 122.6(5) . . ? C25 C24 C23 116.6(5) . . ? C25 C24 C28 121.9(5) . . ? C23 C24 C28 121.5(5) . . ? C24 C25 C26 123.8(5) . . ? C25 C26 C21 118.6(5) . . ? C25 C26 C29 119.0(4) . . ? C21 C26 C29 122.3(4) . . ? N3 C30 C31 121.2(4) . . ? N3 C30 C33 123.8(4) . . ? C31 C30 C33 114.9(4) . . ? C30 C31 C32 128.6(4) . . ? N4 C32 C31 119.7(4) . . ? N4 C32 C37 125.8(4) . . ? C31 C32 C37 114.5(4) . . ? C34 C33 C35 107.2(4) . . ? C34 C33 C36 108.3(4) . . ? C35 C33 C36 109.2(4) . . ? C34 C33 C30 114.4(4) . . ? C35 C33 C30 106.3(4) . . ? C36 C33 C30 111.3(4) . . ? C39 C37 C40 107.6(4) . . ? C39 C37 C38 106.7(4) . . ? C40 C37 C38 108.4(4) . . ? C39 C37 C32 116.6(4) . . ? C40 C37 C32 107.8(4) . . ? C38 C37 C32 109.4(4) . . ? C42 C41 N3 121.1(4) . . ? C42 C41 C46 118.9(5) . . ? N3 C41 C46 119.5(4) . . ? C43 C42 C41 119.0(5) . . ? C43 C42 C47 119.4(5) . . ? C41 C42 C47 121.6(5) . . ? C44 C43 C42 122.2(5) . . ? C43 C44 C45 118.0(5) . . ? C43 C44 C48 120.8(6) . . ? C45 C44 C48 121.2(6) . . ? C44 C45 C46 122.4(5) . . ? C45 C46 C41 119.2(5) . . ? C45 C46 C49 119.4(4) . . ? C41 C46 C49 121.4(4) . . ? C51 C50 C55 120.4(4) . . ? C51 C50 N4 120.0(4) . . ? C55 C50 N4 119.3(4) . . ? C50 C51 C52 118.9(4) . . ? C50 C51 C56 121.0(4) . . ? C52 C51 C56 120.1(5) . . ? C53 C52 C51 121.9(5) . . ? C52 C53 C54 118.2(4) . . ? C52 C53 C57 120.9(5) . . ? C54 C53 C57 120.9(5) . . ? C53 C54 C55 122.3(5) . . ? C54 C55 C50 118.2(4) . . ? C54 C55 C58 120.2(4) . . ? C50 C55 C58 121.4(4) . . ? C59 C60 C61 114.0(7) . . ? C62 C61 C60 113.1(7) . . ? C61 C62 C63 116.0(7) . . ? C64 C63 C62 110.9(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.351 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.128 # Attachment '(tBuNac)PbCl.CIF' data_(tBuNac)PbCl _database_code_depnum_ccdc_archive 'CCDC 859476' #TrackingRef '(tBuNac)PbCl.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H53 Cl N2 Pb' _chemical_formula_weight 744.43 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' Cl Cl 0.1484 0.1585 '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 16.5359(4) _cell_length_b 10.6225(2) _cell_length_c 19.5757(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.726(2) _cell_angle_gamma 90.00 _cell_volume 3378.45(13) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 5.097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.427 _exptl_absorpt_correction_T_max 0.556 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22710 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7372 _reflns_number_gt 6211 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The methyl groups of one of the tert-butyl substituents of the Nacnac ligand were found to be disordered over two sites. This disorder was successfully modelled and the occupancies of each disordered set refined using a free variable to a ratio of ca. 62:38. The carbon atoms of the least occupied set were refined isotropically. ; _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^)+(0.0147P)^2^+3.1987P] 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 7372 _refine_ls_number_parameters 382 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0487 _refine_ls_wR_factor_gt 0.0443 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.073 _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 0.204794(7) 0.289546(10) 0.274312(6) 0.01976(4) Uani 1 1 d . . . Cl1 Cl 0.28213(6) 0.41281(7) 0.19396(4) 0.0343(2) Uani 1 1 d . . . N1 N 0.18235(14) 0.1163(2) 0.20203(11) 0.0165(5) Uani 1 1 d . . . N2 N 0.31814(15) 0.1877(2) 0.32688(12) 0.0175(5) Uani 1 1 d . . . C1 C 0.23942(19) 0.0323(3) 0.19668(14) 0.0196(6) Uani 1 1 d . . . C2 C 0.32289(19) 0.0524(3) 0.22907(15) 0.0221(6) Uani 1 1 d . . . H2 H 0.3610 0.0138 0.2048 0.027 Uiso 1 1 calc R . . C3 C 0.36084(18) 0.1163(3) 0.28871(14) 0.0195(6) Uani 1 1 d . A . C4 C 0.2256(2) -0.0966(3) 0.15714(16) 0.0247(7) Uani 1 1 d . . . C5 C 0.1375(2) -0.1279(3) 0.12110(17) 0.0305(8) Uani 1 1 d . . . H5A H 0.1361 -0.2124 0.1009 0.046 Uiso 1 1 calc R . . H5B H 0.1190 -0.0663 0.0842 0.046 Uiso 1 1 calc R . . H5C H 0.1010 -0.1249 0.1552 0.046 Uiso 1 1 calc R . . C6 C 0.2793(2) -0.1016(3) 0.10062(18) 0.0375(9) Uani 1 1 d . . . H6A H 0.2671 -0.1787 0.0732 0.056 Uiso 1 1 calc R . . H6B H 0.3376 -0.1009 0.1227 0.056 Uiso 1 1 calc R . . H6C H 0.2674 -0.0282 0.0700 0.056 Uiso 1 1 calc R . . C7 C 0.2527(2) -0.2010(3) 0.21150(19) 0.0377(9) Uani 1 1 d . . . H7A H 0.2183 -0.1977 0.2472 0.057 Uiso 1 1 calc R . . H7B H 0.3104 -0.1881 0.2333 0.057 Uiso 1 1 calc R . . H7C H 0.2465 -0.2833 0.1886 0.057 Uiso 1 1 calc R . . C8 C 0.45605(19) 0.1057(3) 0.30575(15) 0.0301(7) Uani 1 1 d D . . C9 C 0.4853(4) -0.0312(5) 0.3009(4) 0.069(3) Uani 0.623(7) 1 d PDU A 1 H9A H 0.5454 -0.0346 0.3139 0.104 Uiso 0.623(7) 1 calc PR A 1 H9B H 0.4683 -0.0617 0.2531 0.104 Uiso 0.623(7) 1 calc PR A 1 H9C H 0.4608 -0.0843 0.3325 0.104 Uiso 0.623(7) 1 calc PR A 1 C9A C 0.4854(6) -0.0064(7) 0.3521(4) 0.041(3) Uiso 0.377(7) 1 d PD A 2 H9A1 H 0.5457 -0.0079 0.3623 0.062 Uiso 0.377(7) 1 calc PR A 2 H9A2 H 0.4649 -0.0844 0.3283 0.062 Uiso 0.377(7) 1 calc PR A 2 H9A3 H 0.4646 0.0008 0.3957 0.062 Uiso 0.377(7) 1 calc PR A 2 C10 C 0.4997(3) 0.1583(6) 0.3734(2) 0.0327(16) Uani 0.623(7) 1 d PD A 1 H10A H 0.5592 0.1502 0.3763 0.049 Uiso 0.623(7) 1 calc PR A 1 H10B H 0.4830 0.1120 0.4118 0.049 Uiso 0.623(7) 1 calc PR A 1 H10C H 0.4854 0.2474 0.3765 0.049 Uiso 0.623(7) 1 calc PR A 1 C10A C 0.4952(6) 0.2239(7) 0.3473(4) 0.034(2) Uiso 0.377(7) 1 d PD A 2 H10D H 0.4807 0.2242 0.3936 0.051 Uiso 0.377(7) 1 calc PR A 2 H10E H 0.4741 0.3006 0.3223 0.051 Uiso 0.377(7) 1 calc PR A 2 H10F H 0.5552 0.2208 0.3518 0.051 Uiso 0.377(7) 1 calc PR A 2 C11 C 0.4855(5) 0.1803(9) 0.2471(3) 0.078(3) Uani 0.623(7) 1 d PDU A 1 H11A H 0.4662 0.2676 0.2473 0.117 Uiso 0.623(7) 1 calc PR A 1 H11B H 0.4631 0.1415 0.2021 0.117 Uiso 0.623(7) 1 calc PR A 1 H11C H 0.5457 0.1792 0.2546 0.117 Uiso 0.623(7) 1 calc PR A 1 C11A C 0.4932(5) 0.1027(7) 0.2414(3) 0.0142(19) Uiso 0.377(7) 1 d PD A 2 H11D H 0.4727 0.1743 0.2116 0.021 Uiso 0.377(7) 1 calc PR A 2 H11E H 0.4778 0.0240 0.2161 0.021 Uiso 0.377(7) 1 calc PR A 2 H11F H 0.5532 0.1076 0.2544 0.021 Uiso 0.377(7) 1 calc PR A 2 C12 C 0.09728(18) 0.1140(2) 0.16942(14) 0.0178(6) Uani 1 1 d . . . C13 C 0.03779(19) 0.0748(2) 0.20754(15) 0.0193(6) Uani 1 1 d . . . C14 C -0.0447(2) 0.0752(3) 0.17516(16) 0.0246(7) Uani 1 1 d . . . H14 H -0.0856 0.0471 0.1999 0.029 Uiso 1 1 calc R . . C15 C -0.0679(2) 0.1165(3) 0.10680(16) 0.0266(7) Uani 1 1 d . . . H15 H -0.1240 0.1130 0.0844 0.032 Uiso 1 1 calc R . . C16 C -0.0093(2) 0.1623(3) 0.07199(15) 0.0236(7) Uani 1 1 d . . . H16 H -0.0261 0.1931 0.0260 0.028 Uiso 1 1 calc R . . C18 C 0.0607(2) 0.0328(3) 0.28340(15) 0.0237(7) Uani 1 1 d . . . H18 H 0.1217 0.0418 0.2981 0.028 Uiso 1 1 calc R . . C17 C 0.07353(19) 0.1651(3) 0.10186(14) 0.0201(6) Uani 1 1 d . . . C19 C 0.0196(2) 0.1160(3) 0.33140(16) 0.0339(8) Uani 1 1 d . . . H19A H -0.0403 0.1073 0.3188 0.051 Uiso 1 1 calc R . . H19B H 0.0349 0.2041 0.3262 0.051 Uiso 1 1 calc R . . H19C H 0.0380 0.0897 0.3798 0.051 Uiso 1 1 calc R . . C20 C 0.0390(2) -0.1050(3) 0.29264(18) 0.0344(8) Uani 1 1 d . . . H20A H -0.0205 -0.1168 0.2779 0.052 Uiso 1 1 calc R . . H20B H 0.0553 -0.1286 0.3417 0.052 Uiso 1 1 calc R . . H20C H 0.0682 -0.1581 0.2643 0.052 Uiso 1 1 calc R . . C21 C 0.1339(2) 0.2283(3) 0.06300(15) 0.0241(7) Uani 1 1 d . . . H21 H 0.1904 0.2199 0.0917 0.029 Uiso 1 1 calc R . . C22 C 0.1135(2) 0.3690(3) 0.05438(17) 0.0327(8) Uani 1 1 d . . . H22A H 0.0592 0.3795 0.0249 0.049 Uiso 1 1 calc R . . H22B H 0.1551 0.4110 0.0327 0.049 Uiso 1 1 calc R . . H22C H 0.1133 0.4065 0.1001 0.049 Uiso 1 1 calc R . . C23 C 0.1344(2) 0.1686(3) -0.00824(16) 0.0343(8) Uani 1 1 d . . . H23A H 0.1490 0.0794 -0.0022 0.051 Uiso 1 1 calc R . . H23B H 0.1748 0.2118 -0.0307 0.051 Uiso 1 1 calc R . . H23C H 0.0796 0.1764 -0.0373 0.051 Uiso 1 1 calc R . . C24 C 0.33746(17) 0.2051(3) 0.40077(14) 0.0178(6) Uani 1 1 d . . . C25 C 0.33230(19) 0.1018(3) 0.44567(15) 0.0211(6) Uani 1 1 d . . . C26 C 0.3432(2) 0.1228(3) 0.51682(15) 0.0264(7) Uani 1 1 d . . . H26 H 0.3391 0.0539 0.5469 0.032 Uiso 1 1 calc R . . C27 C 0.3598(2) 0.2417(3) 0.54497(16) 0.0275(7) Uani 1 1 d . . . H27 H 0.3676 0.2543 0.5938 0.033 Uiso 1 1 calc R . . C28 C 0.36484(19) 0.3415(3) 0.50085(15) 0.0237(7) Uani 1 1 d . . . H28 H 0.3763 0.4230 0.5201 0.028 Uiso 1 1 calc R . . C29 C 0.35367(18) 0.3266(3) 0.42920(15) 0.0184(6) Uani 1 1 d . . . C30 C 0.3121(2) -0.0318(3) 0.41896(17) 0.0295(8) Uani 1 1 d . . . H30 H 0.3139 -0.0344 0.3682 0.035 Uiso 1 1 calc R . . C31 C 0.3740(3) -0.1305(4) 0.4572(2) 0.0610(13) Uani 1 1 d . . . H31A H 0.3647 -0.1418 0.5048 0.092 Uiso 1 1 calc R . . H31B H 0.4304 -0.1009 0.4584 0.092 Uiso 1 1 calc R . . H31C H 0.3659 -0.2110 0.4324 0.092 Uiso 1 1 calc R . . C32 C 0.2270(2) -0.0710(3) 0.4287(2) 0.0418(9) Uani 1 1 d . . . H32A H 0.2265 -0.0801 0.4785 0.063 Uiso 1 1 calc R . . H32B H 0.2125 -0.1516 0.4053 0.063 Uiso 1 1 calc R . . H32C H 0.1869 -0.0068 0.4088 0.063 Uiso 1 1 calc R . . C33 C 0.35980(19) 0.4427(3) 0.38469(16) 0.0244(7) Uani 1 1 d . . . H33 H 0.3577 0.4146 0.3356 0.029 Uiso 1 1 calc R . . C34 C 0.4402(2) 0.5152(3) 0.40838(18) 0.0344(8) Uani 1 1 d . . . H34A H 0.4428 0.5862 0.3769 0.052 Uiso 1 1 calc R . . H34B H 0.4870 0.4590 0.4077 0.052 Uiso 1 1 calc R . . H34C H 0.4422 0.5469 0.4557 0.052 Uiso 1 1 calc R . . C35 C 0.2880(2) 0.5330(3) 0.38587(18) 0.0339(8) Uani 1 1 d . . . H35A H 0.2922 0.5682 0.4327 0.051 Uiso 1 1 calc R . . H35B H 0.2359 0.4873 0.3731 0.051 Uiso 1 1 calc R . . H35C H 0.2900 0.6014 0.3526 0.051 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 0.01582(6) 0.02177(6) 0.01987(6) -0.00662(4) -0.00142(4) 0.00345(5) Cl1 0.0462(6) 0.0294(4) 0.0250(4) 0.0025(3) 0.0003(4) -0.0068(4) N1 0.0168(13) 0.0171(12) 0.0145(12) -0.0003(9) 0.0003(10) 0.0003(9) N2 0.0156(13) 0.0217(12) 0.0145(12) -0.0007(9) 0.0008(10) 0.0002(9) C1 0.0261(18) 0.0197(14) 0.0135(14) 0.0000(10) 0.0053(13) 0.0000(12) C2 0.0221(17) 0.0276(16) 0.0170(15) -0.0029(11) 0.0044(13) 0.0071(12) C3 0.0181(16) 0.0256(15) 0.0142(14) 0.0025(11) 0.0015(12) 0.0034(12) C4 0.0286(19) 0.0205(15) 0.0246(17) -0.0028(11) 0.0041(14) 0.0023(12) C5 0.042(2) 0.0198(15) 0.0296(18) -0.0087(12) 0.0058(16) -0.0013(14) C6 0.045(2) 0.0346(19) 0.036(2) -0.0164(14) 0.0160(18) -0.0005(16) C7 0.045(2) 0.0238(17) 0.042(2) 0.0031(14) 0.0016(18) 0.0051(15) C8 0.0176(17) 0.047(2) 0.0251(17) -0.0007(14) 0.0022(14) 0.0087(14) C9 0.048(4) 0.081(4) 0.067(5) -0.047(3) -0.019(3) 0.038(3) C10 0.012(3) 0.051(4) 0.033(3) -0.006(3) -0.002(2) 0.003(2) C11 0.043(4) 0.131(6) 0.064(4) 0.026(4) 0.020(4) -0.004(4) C12 0.0200(16) 0.0146(13) 0.0172(15) -0.0054(10) -0.0006(12) -0.0013(11) C13 0.0223(17) 0.0148(14) 0.0195(15) -0.0031(11) 0.0006(13) -0.0033(11) C14 0.0227(18) 0.0231(15) 0.0282(17) -0.0025(12) 0.0053(14) -0.0051(12) C15 0.0196(17) 0.0274(16) 0.0290(18) -0.0062(13) -0.0053(14) -0.0031(13) C16 0.0261(18) 0.0243(15) 0.0173(15) -0.0029(11) -0.0043(13) 0.0004(12) C18 0.0283(18) 0.0229(15) 0.0196(16) 0.0035(11) 0.0041(13) -0.0049(13) C17 0.0239(17) 0.0187(14) 0.0166(15) -0.0054(11) 0.0009(13) -0.0005(11) C19 0.042(2) 0.0393(19) 0.0216(17) 0.0003(14) 0.0085(16) 0.0015(16) C20 0.039(2) 0.0313(18) 0.0330(19) 0.0050(14) 0.0058(16) -0.0087(15) C21 0.0275(18) 0.0278(17) 0.0157(15) 0.0002(11) 0.0008(13) 0.0002(13) C22 0.038(2) 0.0282(17) 0.0326(19) 0.0048(14) 0.0081(16) -0.0038(15) C23 0.042(2) 0.043(2) 0.0188(17) -0.0007(13) 0.0081(16) 0.0041(16) C24 0.0118(14) 0.0241(14) 0.0169(14) -0.0017(11) 0.0009(11) -0.0004(11) C25 0.0220(17) 0.0224(15) 0.0189(15) -0.0027(11) 0.0040(13) -0.0031(12) C26 0.0300(19) 0.0296(16) 0.0198(16) 0.0018(12) 0.0051(14) -0.0047(14) C27 0.030(2) 0.0357(17) 0.0166(15) -0.0064(12) 0.0045(14) -0.0063(14) C28 0.0223(18) 0.0246(15) 0.0240(16) -0.0070(12) 0.0034(13) -0.0048(12) C29 0.0107(15) 0.0218(14) 0.0222(15) -0.0019(11) 0.0018(12) -0.0014(11) C30 0.042(2) 0.0224(16) 0.0245(17) -0.0029(12) 0.0085(15) -0.0069(14) C31 0.057(3) 0.033(2) 0.085(3) -0.011(2) -0.009(3) 0.0111(19) C32 0.041(2) 0.041(2) 0.042(2) -0.0093(16) 0.0061(18) -0.0145(17) C33 0.0254(18) 0.0223(15) 0.0234(16) 0.0009(12) -0.0008(14) -0.0049(12) C34 0.032(2) 0.0329(18) 0.036(2) 0.0055(14) 0.0015(16) -0.0147(15) C35 0.036(2) 0.0239(17) 0.036(2) -0.0053(13) -0.0092(16) 0.0004(14) _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 N2 2.241(2) . ? Pb1 N1 2.309(2) . ? Pb1 Cl1 2.5637(9) . ? N1 C1 1.316(4) . ? N1 C12 1.433(4) . ? N2 C3 1.353(4) . ? N2 C24 1.434(3) . ? C1 C2 1.424(4) . ? C1 C4 1.568(4) . ? C2 C3 1.395(4) . ? C3 C8 1.551(4) . ? C4 C5 1.533(4) . ? C4 C6 1.543(4) . ? C4 C7 1.544(4) . ? C8 C10 1.494(5) . ? C8 C11A 1.502(5) . ? C8 C9A 1.522(6) . ? C8 C9 1.541(5) . ? C8 C11 1.547(5) . ? C8 C10A 1.569(6) . ? C12 C13 1.404(4) . ? C12 C17 1.416(4) . ? C13 C14 1.394(4) . ? C13 C18 1.529(4) . ? C14 C15 1.392(4) . ? C15 C16 1.373(4) . ? C16 C17 1.387(4) . ? C18 C20 1.525(4) . ? C18 C19 1.538(4) . ? C17 C21 1.520(4) . ? C21 C23 1.533(4) . ? C21 C22 1.535(4) . ? C24 C29 1.411(4) . ? C24 C25 1.418(4) . ? C25 C26 1.389(4) . ? C25 C30 1.528(4) . ? C26 C27 1.385(4) . ? C27 C28 1.380(4) . ? C28 C29 1.389(4) . ? C29 C33 1.524(4) . ? C30 C32 1.513(5) . ? C30 C31 1.556(5) . ? C33 C35 1.529(4) . ? C33 C34 1.532(4) . ? 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 N2 Pb1 N1 85.52(8) . . ? N2 Pb1 Cl1 93.34(6) . . ? N1 Pb1 Cl1 94.18(6) . . ? C1 N1 C12 127.7(2) . . ? C1 N1 Pb1 123.55(19) . . ? C12 N1 Pb1 108.61(16) . . ? C3 N2 C24 126.0(2) . . ? C3 N2 Pb1 119.68(18) . . ? C24 N2 Pb1 114.28(17) . . ? N1 C1 C2 120.9(2) . . ? N1 C1 C4 126.2(3) . . ? C2 C1 C4 113.0(2) . . ? C3 C2 C1 133.9(3) . . ? N2 C3 C2 122.4(3) . . ? N2 C3 C8 122.3(2) . . ? C2 C3 C8 115.2(3) . . ? C5 C4 C6 106.7(3) . . ? C5 C4 C7 106.9(3) . . ? C6 C4 C7 109.7(3) . . ? C5 C4 C1 117.0(3) . . ? C6 C4 C1 109.5(2) . . ? C7 C4 C1 106.9(2) . . ? C10 C8 C11A 123.2(4) . . ? C10 C8 C9A 73.5(4) . . ? C11A C8 C9A 110.4(4) . . ? C10 C8 C9 107.6(3) . . ? C11A C8 C9 75.3(4) . . ? C9A C8 C9 39.6(4) . . ? C10 C8 C11 107.5(4) . . ? C11A C8 C11 32.2(4) . . ? C9A C8 C11 137.3(5) . . ? C9 C8 C11 107.0(4) . . ? C10 C8 C3 117.8(3) . . ? C11A C8 C3 112.2(4) . . ? C9A C8 C3 112.5(4) . . ? C9 C8 C3 111.9(3) . . ? C11 C8 C3 104.5(4) . . ? C10 C8 C10A 32.5(3) . . ? C11A C8 C10A 105.0(4) . . ? C9A C8 C10A 105.2(4) . . ? C9 C8 C10A 133.1(5) . . ? C11 C8 C10A 79.5(4) . . ? C3 C8 C10A 111.0(4) . . ? C13 C12 C17 120.7(3) . . ? C13 C12 N1 119.7(2) . . ? C17 C12 N1 119.2(3) . . ? C14 C13 C12 118.8(3) . . ? C14 C13 C18 119.2(3) . . ? C12 C13 C18 122.1(3) . . ? C15 C14 C13 120.6(3) . . ? C16 C15 C14 119.7(3) . . ? C15 C16 C17 122.1(3) . . ? C20 C18 C13 112.0(2) . . ? C20 C18 C19 109.8(3) . . ? C13 C18 C19 111.5(3) . . ? C16 C17 C12 117.8(3) . . ? C16 C17 C21 119.2(3) . . ? C12 C17 C21 122.9(3) . . ? C17 C21 C23 112.8(3) . . ? C17 C21 C22 109.5(3) . . ? C23 C21 C22 109.9(2) . . ? C29 C24 C25 119.5(3) . . ? C29 C24 N2 120.4(2) . . ? C25 C24 N2 119.8(2) . . ? C26 C25 C24 119.1(3) . . ? C26 C25 C30 118.1(3) . . ? C24 C25 C30 122.8(3) . . ? C27 C26 C25 121.6(3) . . ? C28 C27 C26 118.8(3) . . ? C27 C28 C29 122.2(3) . . ? C28 C29 C24 118.8(3) . . ? C28 C29 C33 118.4(2) . . ? C24 C29 C33 122.8(3) . . ? C32 C30 C25 111.2(3) . . ? C32 C30 C31 107.3(3) . . ? C25 C30 C31 112.3(3) . . ? C29 C33 C35 111.4(3) . . ? C29 C33 C34 112.3(2) . . ? C35 C33 C34 108.2(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.966 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.095 # Attachment '{(MesNac)MgClPb(Cl)(tBuMesNac)}2.CIF' data_{(MesNac)MgClPb(Cl)(tBuMesNac)}2 _database_code_depnum_ccdc_archive 'CCDC 859477' #TrackingRef '{(MesNac)MgClPb(Cl)(tBuMesNac)}2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H154 Cl4 Mg2 N8 Pb2' _chemical_formula_weight 2193.21 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' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 14.0924(5) _cell_length_b 28.9325(9) _cell_length_c 27.2581(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.860(4) _cell_angle_gamma 90.00 _cell_volume 11055.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4504 _exptl_absorpt_coefficient_mu 3.197 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.778 _exptl_absorpt_correction_T_max 0.853 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65659 _diffrn_reflns_av_R_equivalents 0.1289 _diffrn_reflns_av_sigmaI/netI 0.1857 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19435 _reflns_number_gt 12455 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. one half molecule of hexane of crystallisation, sitting on an inversion centre, was located and its carbon atoms refined isotropically. Another molecule of hexame of crystallisation was located and found to be disordered over two sites. This disorder was successfully modelled and the carbon atoms of both disordered sets refined isotropically with a combined atomic site occupancy of 50%. The largest residual electron density peak (2.20 e/ang.3)in the final difference map is located close to Pb(2). ; _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^)+(0.0149P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19435 _refine_ls_number_parameters 1187 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.992 _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 0.02717(2) 0.659007(9) 0.109360(12) 0.02037(9) Uani 1 1 d . . . Cl1 Cl -0.00210(16) 0.63380(6) 0.20350(8) 0.0312(5) Uani 1 1 d . . . Mg1 Mg -0.02668(19) 0.70305(8) 0.24461(10) 0.0241(7) Uani 1 1 d . . . N1 N 0.1379(4) 0.60144(19) 0.1161(2) 0.0192(16) Uani 1 1 d . . . C1 C 0.1945(6) 0.5303(2) 0.1666(3) 0.022(2) Uani 1 1 d . . . C117 C 0.607(2) 1.0365(16) 0.1285(17) 0.030(12) Uiso 0.200(13) 1 d PD A 2 H11A H 0.6349 1.0087 0.1445 0.045 Uiso 0.200(13) 1 calc PR A 2 H11B H 0.6444 1.0636 0.1401 0.045 Uiso 0.200(13) 1 calc PR A 2 H11C H 0.6065 1.0337 0.0927 0.045 Uiso 0.200(13) 1 calc PR A 2 C118 C 0.505(2) 1.0421(19) 0.1416(11) 0.045(15) Uiso 0.200(13) 1 d PD A 2 H11D H 0.4830 1.0128 0.1553 0.055 Uiso 0.200(13) 1 calc PR A 2 H11E H 0.5028 1.0664 0.1670 0.055 Uiso 0.200(13) 1 calc PR A 2 C119 C 0.439(2) 1.0553(19) 0.0962(12) 0.030(13) Uiso 0.200(13) 1 d PD A 2 H11F H 0.4513 1.0878 0.0874 0.036 Uiso 0.200(13) 1 calc PR A 2 H11G H 0.4533 1.0355 0.0682 0.036 Uiso 0.200(13) 1 calc PR A 2 Pb2 Pb 0.12832(2) 0.819349(10) 0.150482(12) 0.02313(9) Uani 1 1 d . . . Cl2 Cl -0.02420(15) 0.75354(6) 0.17809(8) 0.0273(5) Uani 1 1 d . . . Mg2 Mg 0.41107(19) 0.85686(9) 0.15914(11) 0.0275(7) Uani 1 1 d . . . N2 N -0.0736(4) 0.59856(19) 0.0886(2) 0.0172(15) Uani 1 1 d . . . C2 C 0.1188(5) 0.5607(2) 0.1362(3) 0.0182(19) Uani 1 1 d . . . Cl3 Cl 0.26032(15) 0.89055(7) 0.13697(9) 0.0322(5) Uani 1 1 d . . . N3 N 0.0712(4) 0.82519(19) 0.0702(2) 0.0224(16) Uani 1 1 d . . . C3 C 0.0254(6) 0.5440(2) 0.1357(3) 0.024(2) Uani 1 1 d . . . H3 H 0.0206 0.5180 0.1566 0.029 Uiso 1 1 calc R . . Cl4 Cl 0.38251(16) 0.78102(7) 0.17627(9) 0.0379(6) Uani 1 1 d . . . N4 N 0.0248(4) 0.87984(19) 0.1592(2) 0.0217(16) Uani 1 1 d . . . C4 C -0.0624(6) 0.5573(2) 0.1111(3) 0.021(2) Uani 1 1 d . . . N5 N 0.0647(5) 0.7120(2) 0.3060(3) 0.0244(17) Uani 1 1 d . . . C5 C -0.1462(6) 0.5238(2) 0.1172(3) 0.024(2) Uani 1 1 d . . . N6 N -0.1423(5) 0.6966(2) 0.2820(3) 0.0253(17) Uani 1 1 d . . . C6 C 0.2974(6) 0.5456(3) 0.1667(3) 0.034(2) Uani 1 1 d . . . H6A H 0.3039 0.5775 0.1785 0.051 Uiso 1 1 calc R . . H6B H 0.3163 0.5438 0.1331 0.051 Uiso 1 1 calc R . . H6C H 0.3385 0.5254 0.1885 0.051 Uiso 1 1 calc R . . N7 N 0.5008(5) 0.8722(2) 0.1082(3) 0.0263(17) Uani 1 1 d . . . C7 C 0.1878(6) 0.4801(2) 0.1491(3) 0.034(2) Uani 1 1 d . . . H7A H 0.2016 0.4785 0.1146 0.051 Uiso 1 1 calc R . . H7B H 0.1234 0.4684 0.1518 0.051 Uiso 1 1 calc R . . H7C H 0.2343 0.4613 0.1695 0.051 Uiso 1 1 calc R . . N8 N 0.4904(5) 0.8887(2) 0.2150(3) 0.0303(18) Uani 1 1 d . . . C8 C 0.1698(6) 0.5336(3) 0.2196(3) 0.035(2) Uani 1 1 d . . . H8A H 0.2173 0.5166 0.2414 0.052 Uiso 1 1 calc R . . H8B H 0.1065 0.5202 0.2219 0.052 Uiso 1 1 calc R . . H8C H 0.1696 0.5661 0.2297 0.052 Uiso 1 1 calc R . . C9 C -0.1192(6) 0.4739(2) 0.1056(3) 0.032(2) Uani 1 1 d . . . H9A H -0.1722 0.4533 0.1110 0.049 Uiso 1 1 calc R . . H9B H -0.0624 0.4648 0.1272 0.049 Uiso 1 1 calc R . . H9C H -0.1056 0.4718 0.0711 0.049 Uiso 1 1 calc R . . C10 C -0.1615(6) 0.5270(3) 0.1728(3) 0.041(3) Uani 1 1 d . . . H1 H -0.1717 0.5594 0.1815 0.062 Uiso 1 1 calc R . . H2 H -0.1051 0.5150 0.1927 0.062 Uiso 1 1 calc R . . H4 H -0.2175 0.5087 0.1791 0.062 Uiso 1 1 calc R . . C11 C -0.2416(6) 0.5353(3) 0.0887(4) 0.037(2) Uani 1 1 d . . . H6 H -0.2619 0.5662 0.0981 0.056 Uiso 1 1 calc R . . H7 H -0.2894 0.5125 0.0965 0.056 Uiso 1 1 calc R . . H8 H -0.2352 0.5346 0.0533 0.056 Uiso 1 1 calc R . . C12 C 0.2266(5) 0.6153(2) 0.1002(3) 0.0208(19) Uani 1 1 d . . . C13 C 0.2602(5) 0.5950(2) 0.0598(3) 0.0204(19) Uani 1 1 d . . . C14 C 0.3433(5) 0.6113(2) 0.0430(3) 0.024(2) Uani 1 1 d . . . H14 H 0.3659 0.5977 0.0147 0.028 Uiso 1 1 calc R . . C15 C 0.3944(6) 0.6475(3) 0.0669(3) 0.028(2) Uani 1 1 d . . . C16 C 0.3595(6) 0.6680(2) 0.1061(3) 0.024(2) Uani 1 1 d . . . H16 H 0.3934 0.6932 0.1217 0.029 Uiso 1 1 calc R . . C17 C 0.2760(6) 0.6533(2) 0.1240(3) 0.025(2) Uani 1 1 d . . . C18 C 0.2099(6) 0.5549(2) 0.0328(3) 0.029(2) Uani 1 1 d . . . H18A H 0.2260 0.5262 0.0508 0.044 Uiso 1 1 calc R . . H18B H 0.2302 0.5528 -0.0005 0.044 Uiso 1 1 calc R . . H18C H 0.1408 0.5599 0.0305 0.044 Uiso 1 1 calc R . . C19 C 0.4873(6) 0.6633(3) 0.0484(4) 0.050(3) Uani 1 1 d . . . H19A H 0.5374 0.6406 0.0579 0.075 Uiso 1 1 calc R . . H19B H 0.5057 0.6933 0.0630 0.075 Uiso 1 1 calc R . . H19C H 0.4786 0.6661 0.0124 0.075 Uiso 1 1 calc R . . C20 C 0.2418(6) 0.6752(3) 0.1693(3) 0.030(2) Uani 1 1 d . . . H20A H 0.1924 0.6981 0.1593 0.045 Uiso 1 1 calc R . . H20B H 0.2955 0.6904 0.1886 0.045 Uiso 1 1 calc R . . H20C H 0.2153 0.6513 0.1895 0.045 Uiso 1 1 calc R . . C21 C -0.1462(5) 0.6120(2) 0.0507(3) 0.0210(19) Uani 1 1 d . . . C22 C -0.1454(6) 0.5932(3) 0.0034(3) 0.024(2) Uani 1 1 d . . . C23 C -0.2090(5) 0.6110(2) -0.0343(3) 0.024(2) Uani 1 1 d . . . H23 H -0.2103 0.5982 -0.0664 0.029 Uiso 1 1 calc R . . C24 C -0.2705(6) 0.6469(3) -0.0262(3) 0.025(2) Uani 1 1 d . . . C25 C -0.2684(5) 0.6646(3) 0.0204(3) 0.025(2) Uani 1 1 d . . . H25 H -0.3100 0.6894 0.0261 0.030 Uiso 1 1 calc R . . C26 C -0.2085(5) 0.6480(2) 0.0596(3) 0.023(2) Uani 1 1 d . . . C27 C -0.0797(5) 0.5546(2) -0.0075(3) 0.024(2) Uani 1 1 d . . . H27A H -0.0155 0.5609 0.0085 0.036 Uiso 1 1 calc R . . H27B H -0.0774 0.5521 -0.0432 0.036 Uiso 1 1 calc R . . H27C H -0.1031 0.5255 0.0051 0.036 Uiso 1 1 calc R . . C28 C -0.2128(6) 0.6664(2) 0.1104(3) 0.029(2) Uani 1 1 d . . . H28A H -0.1709 0.6934 0.1154 0.044 Uiso 1 1 calc R . . H28B H -0.1919 0.6424 0.1345 0.044 Uiso 1 1 calc R . . H28C H -0.2785 0.6755 0.1146 0.044 Uiso 1 1 calc R . . C29 C -0.3381(6) 0.6665(3) -0.0682(4) 0.047(3) Uani 1 1 d . . . H29A H -0.3449 0.6999 -0.0637 0.070 Uiso 1 1 calc R . . H29B H -0.4007 0.6517 -0.0683 0.070 Uiso 1 1 calc R . . H29C H -0.3124 0.6605 -0.0996 0.070 Uiso 1 1 calc R . . C30 C 0.0580(6) 0.8758(2) -0.0069(3) 0.026(2) Uani 1 1 d . . . C31 C 0.0531(5) 0.8666(2) 0.0491(3) 0.022(2) Uani 1 1 d . . . C32 C 0.0335(6) 0.9056(2) 0.0773(3) 0.027(2) Uani 1 1 d . . . H32 H 0.0376 0.9338 0.0598 0.032 Uiso 1 1 calc R . . C33 C 0.0094(5) 0.9122(2) 0.1253(3) 0.022(2) Uani 1 1 d . . . C34 C -0.0305(6) 0.9612(2) 0.1353(3) 0.028(2) Uani 1 1 d . . . C35 C 0.0575(7) 0.9267(3) -0.0208(4) 0.053(3) Uani 1 1 d . . . H35A H 0.0642 0.9298 -0.0560 0.079 Uiso 1 1 calc R . . H35B H 0.1107 0.9424 -0.0017 0.079 Uiso 1 1 calc R . . H35C H -0.0028 0.9407 -0.0135 0.079 Uiso 1 1 calc R . . C36 C 0.1537(7) 0.8577(3) -0.0218(4) 0.045(3) Uani 1 1 d . . . H36A H 0.1536 0.8238 -0.0213 0.068 Uiso 1 1 calc R . . H36B H 0.2058 0.8693 0.0015 0.068 Uiso 1 1 calc R . . H36C H 0.1625 0.8685 -0.0551 0.068 Uiso 1 1 calc R . . C37 C -0.0222(7) 0.8525(3) -0.0394(4) 0.048(3) Uani 1 1 d . . . H37A H -0.0837 0.8630 -0.0298 0.072 Uiso 1 1 calc R . . H37B H -0.0172 0.8189 -0.0353 0.072 Uiso 1 1 calc R . . H37C H -0.0173 0.8606 -0.0739 0.072 Uiso 1 1 calc R . . C38 C 0.0535(6) 0.9941(3) 0.1308(4) 0.046(3) Uani 1 1 d . . . H38A H 0.0756 0.9909 0.0980 0.069 Uiso 1 1 calc R . . H38B H 0.1057 0.9863 0.1560 0.069 Uiso 1 1 calc R . . H38C H 0.0330 1.0260 0.1356 0.069 Uiso 1 1 calc R . . C39 C -0.1103(6) 0.9738(3) 0.0960(4) 0.049(3) Uani 1 1 d . . . H39A H -0.1607 0.9504 0.0951 0.073 Uiso 1 1 calc R . . H39B H -0.0853 0.9752 0.0638 0.073 Uiso 1 1 calc R . . H39C H -0.1366 1.0040 0.1037 0.073 Uiso 1 1 calc R . . C40 C -0.0657(8) 0.9701(3) 0.1845(4) 0.053(3) Uani 1 1 d . . . H40A H -0.0809 1.0030 0.1873 0.080 Uiso 1 1 calc R . . H40B H -0.0162 0.9615 0.2107 0.080 Uiso 1 1 calc R . . H40C H -0.1232 0.9516 0.1875 0.080 Uiso 1 1 calc R . . C41 C 0.0688(6) 0.7815(2) 0.0443(3) 0.0216(19) Uani 1 1 d . . . C42 C -0.0188(6) 0.7605(2) 0.0296(3) 0.023(2) Uani 1 1 d . . . C43 C -0.0196(6) 0.7183(2) 0.0047(3) 0.022(2) Uani 1 1 d . . . H43 H -0.0788 0.7044 -0.0066 0.027 Uiso 1 1 calc R . . C44 C 0.0648(6) 0.6965(2) -0.0037(3) 0.022(2) Uani 1 1 d . . . C45 C 0.1496(6) 0.7162(2) 0.0157(3) 0.025(2) Uani 1 1 d . . . H45 H 0.2075 0.7002 0.0125 0.030 Uiso 1 1 calc R . . C46 C 0.1533(6) 0.7580(2) 0.0396(3) 0.022(2) Uani 1 1 d . . . C47 C -0.1114(6) 0.7817(3) 0.0412(3) 0.031(2) Uani 1 1 d . . . H47A H -0.1614 0.7748 0.0145 0.047 Uiso 1 1 calc R . . H47B H -0.1038 0.8152 0.0445 0.047 Uiso 1 1 calc R . . H47C H -0.1294 0.7688 0.0722 0.047 Uiso 1 1 calc R . . C48 C 0.0630(6) 0.6527(3) -0.0336(3) 0.038(2) Uani 1 1 d . . . H48A H 0.0685 0.6603 -0.0682 0.057 Uiso 1 1 calc R . . H48B H 0.0028 0.6364 -0.0309 0.057 Uiso 1 1 calc R . . H48C H 0.1165 0.6329 -0.0211 0.057 Uiso 1 1 calc R . . C49 C 0.2507(6) 0.7771(3) 0.0575(3) 0.033(2) Uani 1 1 d . . . H49A H 0.2742 0.7621 0.0887 0.049 Uiso 1 1 calc R . . H49B H 0.2459 0.8105 0.0627 0.049 Uiso 1 1 calc R . . H49C H 0.2951 0.7710 0.0328 0.049 Uiso 1 1 calc R . . C50 C -0.0187(5) 0.8764(2) 0.2046(3) 0.0184(19) Uani 1 1 d . . . C51 C -0.1134(6) 0.8619(2) 0.2031(3) 0.027(2) Uani 1 1 d . . . C52 C -0.1527(6) 0.8557(2) 0.2478(3) 0.028(2) Uani 1 1 d . . . H52 H -0.2174 0.8464 0.2472 0.033 Uiso 1 1 calc R . . C53 C -0.0998(7) 0.8627(3) 0.2926(4) 0.032(2) Uani 1 1 d . . . C54 C -0.0069(6) 0.8766(3) 0.2924(3) 0.032(2) Uani 1 1 d . . . H54 H 0.0302 0.8812 0.3231 0.039 Uiso 1 1 calc R . . C55 C 0.0352(6) 0.8841(2) 0.2494(3) 0.024(2) Uani 1 1 d . . . C56 C -0.1719(6) 0.8513(3) 0.1545(3) 0.036(2) Uani 1 1 d . . . H56A H -0.1747 0.8788 0.1334 0.053 Uiso 1 1 calc R . . H56B H -0.2367 0.8424 0.1608 0.053 Uiso 1 1 calc R . . H56C H -0.1421 0.8258 0.1380 0.053 Uiso 1 1 calc R . . C57 C -0.1443(7) 0.8540(3) 0.3396(4) 0.045(3) Uani 1 1 d . . . H57A H -0.1013 0.8651 0.3677 0.068 Uiso 1 1 calc R . . H57B H -0.1553 0.8208 0.3432 0.068 Uiso 1 1 calc R . . H57C H -0.2052 0.8705 0.3386 0.068 Uiso 1 1 calc R . . C58 C 0.1347(6) 0.9024(3) 0.2511(3) 0.036(2) Uani 1 1 d . . . H58A H 0.1331 0.9340 0.2379 0.053 Uiso 1 1 calc R . . H58B H 0.1723 0.8827 0.2312 0.053 Uiso 1 1 calc R . . H58C H 0.1639 0.9027 0.2853 0.053 Uiso 1 1 calc R . . C59 C 0.1070(7) 0.7392(3) 0.3900(3) 0.042(3) Uani 1 1 d . . . H59A H 0.1558 0.7150 0.3942 0.062 Uiso 1 1 calc R . . H59B H 0.0756 0.7421 0.4203 0.062 Uiso 1 1 calc R . . H59C H 0.1371 0.7687 0.3829 0.062 Uiso 1 1 calc R . . C60 C 0.0333(7) 0.7265(3) 0.3473(3) 0.030(2) Uani 1 1 d . . . C61 C -0.0620(6) 0.7305(3) 0.3560(3) 0.030(2) Uani 1 1 d . . . H61 H -0.0736 0.7468 0.3851 0.035 Uiso 1 1 calc R . . C62 C -0.1439(7) 0.7133(3) 0.3272(4) 0.034(2) Uani 1 1 d . . . C63 C -0.2353(6) 0.7131(3) 0.3513(4) 0.043(3) Uani 1 1 d . . . H63A H -0.2861 0.7275 0.3291 0.064 Uiso 1 1 calc R . . H63B H -0.2265 0.7304 0.3822 0.064 Uiso 1 1 calc R . . H63C H -0.2530 0.6811 0.3580 0.064 Uiso 1 1 calc R . . C64 C 0.1637(6) 0.7026(3) 0.3043(3) 0.023(2) Uani 1 1 d . . . C65 C 0.1973(6) 0.6578(3) 0.3129(3) 0.029(2) Uani 1 1 d . . . C66 C 0.2911(7) 0.6481(3) 0.3082(3) 0.039(2) Uani 1 1 d . . . H66 H 0.3132 0.6173 0.3138 0.047 Uiso 1 1 calc R . . C67 C 0.3554(7) 0.6817(4) 0.2957(3) 0.042(2) Uani 1 1 d . . . C68 C 0.3211(7) 0.7266(3) 0.2882(3) 0.037(2) Uani 1 1 d . . . H68 H 0.3639 0.7501 0.2802 0.044 Uiso 1 1 calc R . . C69 C 0.2281(7) 0.7378(3) 0.2921(3) 0.032(2) Uani 1 1 d . . . C70 C 0.1310(6) 0.6200(2) 0.3273(3) 0.031(2) Uani 1 1 d . . . H70A H 0.1680 0.5920 0.3362 0.046 Uiso 1 1 calc R . . H70B H 0.0834 0.6133 0.2994 0.046 Uiso 1 1 calc R . . H70C H 0.0986 0.6303 0.3555 0.046 Uiso 1 1 calc R . . C71 C 0.4573(7) 0.6705(4) 0.2901(4) 0.071(4) Uani 1 1 d . . . H71A H 0.4923 0.6664 0.3228 0.107 Uiso 1 1 calc R . . H71B H 0.4859 0.6959 0.2729 0.107 Uiso 1 1 calc R . . H71C H 0.4606 0.6419 0.2711 0.107 Uiso 1 1 calc R . . C72 C 0.1932(7) 0.7869(3) 0.2826(4) 0.046(3) Uani 1 1 d . . . H72A H 0.1851 0.8020 0.3141 0.069 Uiso 1 1 calc R . . H72B H 0.1319 0.7863 0.2620 0.069 Uiso 1 1 calc R . . H72C H 0.2400 0.8041 0.2655 0.069 Uiso 1 1 calc R . . C73 C -0.2245(6) 0.6720(3) 0.2600(3) 0.025(2) Uani 1 1 d . . . C74 C -0.2350(6) 0.6246(3) 0.2691(4) 0.033(2) Uani 1 1 d . . . C75 C -0.3101(6) 0.6012(3) 0.2447(4) 0.035(2) Uani 1 1 d . . . H75 H -0.3162 0.5691 0.2508 0.042 Uiso 1 1 calc R . . C76 C -0.3769(6) 0.6222(3) 0.2119(4) 0.036(2) Uani 1 1 d . . . C77 C -0.3665(6) 0.6684(3) 0.2038(3) 0.036(2) Uani 1 1 d . . . H77 H -0.4129 0.6834 0.1816 0.043 Uiso 1 1 calc R . . C78 C -0.2912(6) 0.6946(3) 0.2265(3) 0.029(2) Uani 1 1 d . . . C79 C -0.1614(6) 0.6000(3) 0.3040(4) 0.050(3) Uani 1 1 d . . . H79A H -0.1798 0.5676 0.3071 0.075 Uiso 1 1 calc R . . H79B H -0.1577 0.6148 0.3365 0.075 Uiso 1 1 calc R . . H79C H -0.0990 0.6017 0.2912 0.075 Uiso 1 1 calc R . . C80 C -0.4559(7) 0.5947(3) 0.1858(4) 0.059(3) Uani 1 1 d . . . H80A H -0.5093 0.6152 0.1750 0.088 Uiso 1 1 calc R . . H80B H -0.4771 0.5713 0.2082 0.088 Uiso 1 1 calc R . . H80C H -0.4333 0.5795 0.1570 0.088 Uiso 1 1 calc R . . C81 C -0.2802(6) 0.7454(3) 0.2159(4) 0.045(3) Uani 1 1 d . . . H81A H -0.2770 0.7628 0.2468 0.068 Uiso 1 1 calc R . . H81B H -0.3350 0.7559 0.1937 0.068 Uiso 1 1 calc R . . H81C H -0.2215 0.7503 0.2002 0.068 Uiso 1 1 calc R . . C82 C 0.6384(6) 0.9100(3) 0.0772(4) 0.044(3) Uani 1 1 d . . . H82A H 0.6711 0.8817 0.0687 0.066 Uiso 1 1 calc R . . H82B H 0.6857 0.9336 0.0884 0.066 Uiso 1 1 calc R . . H82C H 0.5987 0.9214 0.0481 0.066 Uiso 1 1 calc R . . C83 C 0.5759(6) 0.8999(3) 0.1180(4) 0.029(2) Uani 1 1 d . . . C84 C 0.6060(6) 0.9182(3) 0.1645(4) 0.040(3) Uani 1 1 d . . . H84 H 0.6604 0.9378 0.1655 0.047 Uiso 1 1 calc R . . C85 C 0.5688(6) 0.9123(3) 0.2099(4) 0.035(2) Uani 1 1 d . . . C86 C 0.6247(6) 0.9342(3) 0.2536(4) 0.046(3) Uani 1 1 d . . . H86A H 0.5880 0.9598 0.2657 0.068 Uiso 1 1 calc R . . H86B H 0.6853 0.9460 0.2438 0.068 Uiso 1 1 calc R . . H86C H 0.6375 0.9112 0.2797 0.068 Uiso 1 1 calc R . . C87 C 0.4857(6) 0.8527(3) 0.0601(3) 0.026(2) Uani 1 1 d . . . C88 C 0.4284(6) 0.8737(3) 0.0216(4) 0.034(2) Uani 1 1 d . . . C89 C 0.4095(7) 0.8511(3) -0.0225(4) 0.046(3) Uani 1 1 d . . . H89 H 0.3695 0.8655 -0.0482 0.055 Uiso 1 1 calc R . . C90 C 0.4475(7) 0.8072(3) -0.0311(4) 0.046(3) Uani 1 1 d . . . C91 C 0.5069(7) 0.7880(3) 0.0066(4) 0.040(2) Uani 1 1 d . . . H91 H 0.5361 0.7591 0.0010 0.048 Uiso 1 1 calc R . . C92 C 0.5261(6) 0.8086(3) 0.0521(3) 0.031(2) Uani 1 1 d . . . C93 C 0.3881(7) 0.9212(3) 0.0301(4) 0.047(3) Uani 1 1 d . . . H93A H 0.3593 0.9338 -0.0014 0.071 Uiso 1 1 calc R . . H93B H 0.4394 0.9417 0.0439 0.071 Uiso 1 1 calc R . . H93C H 0.3393 0.9189 0.0532 0.071 Uiso 1 1 calc R . . C94 C 0.4229(8) 0.7836(4) -0.0797(4) 0.076(4) Uani 1 1 d . . . H94A H 0.4099 0.7508 -0.0740 0.114 Uiso 1 1 calc R . . H94B H 0.4764 0.7864 -0.0998 0.114 Uiso 1 1 calc R . . H94C H 0.3661 0.7981 -0.0970 0.114 Uiso 1 1 calc R . . C95 C 0.5890(6) 0.7848(3) 0.0923(3) 0.036(2) Uani 1 1 d . . . H95A H 0.6126 0.7557 0.0797 0.054 Uiso 1 1 calc R . . H95B H 0.5522 0.7783 0.1202 0.054 Uiso 1 1 calc R . . H95C H 0.6431 0.8048 0.1033 0.054 Uiso 1 1 calc R . . C96 C 0.4597(6) 0.8845(3) 0.2632(3) 0.028(2) Uani 1 1 d . . . C97 C 0.3957(6) 0.9172(3) 0.2794(4) 0.034(2) Uani 1 1 d . . . C98 C 0.3581(6) 0.9096(3) 0.3240(4) 0.038(2) Uani 1 1 d . . . H98 H 0.3152 0.9317 0.3351 0.045 Uiso 1 1 calc R . . C99 C 0.3807(7) 0.8714(3) 0.3527(3) 0.038(2) Uani 1 1 d . . . C100 C 0.4453(6) 0.8406(3) 0.3373(3) 0.036(2) Uani 1 1 d . . . H100 H 0.4629 0.8145 0.3573 0.043 Uiso 1 1 calc R . . C101 C 0.4862(6) 0.8463(3) 0.2930(4) 0.033(2) Uani 1 1 d . . . C102 C 0.3695(6) 0.9597(3) 0.2480(4) 0.043(3) Uani 1 1 d . . . H5 H 0.3233 0.9784 0.2637 0.064 Uiso 1 1 calc R . . H10E H 0.3415 0.9500 0.2152 0.064 Uiso 1 1 calc R . . H10F H 0.4270 0.9780 0.2447 0.064 Uiso 1 1 calc R . . C103 C 0.3355(7) 0.8630(4) 0.4002(4) 0.062(3) Uani 1 1 d . . . H10G H 0.2882 0.8382 0.3950 0.093 Uiso 1 1 calc R . . H10H H 0.3041 0.8914 0.4097 0.093 Uiso 1 1 calc R . . H10I H 0.3849 0.8541 0.4263 0.093 Uiso 1 1 calc R . . C104 C 0.5571(6) 0.8126(3) 0.2780(3) 0.037(2) Uani 1 1 d . . . H10J H 0.5321 0.7977 0.2470 0.056 Uiso 1 1 calc R . . H10K H 0.5694 0.7891 0.3037 0.056 Uiso 1 1 calc R . . H10L H 0.6166 0.8287 0.2733 0.056 Uiso 1 1 calc R . . C105 C 0.4352(9) 1.0418(4) 0.5999(3) 0.090(4) Uiso 1 1 d DU . . H10A H 0.3670 1.0445 0.5891 0.135 Uiso 1 1 calc R . . H10B H 0.4554 1.0681 0.6212 0.135 Uiso 1 1 calc R . . H10C H 0.4470 1.0130 0.6184 0.135 Uiso 1 1 calc R . . C106 C 0.4904(9) 1.0416(4) 0.5560(4) 0.116(5) Uiso 1 1 d DU . . H10D H 0.4745 1.0700 0.5367 0.139 Uiso 1 1 calc R . . H10M H 0.5592 1.0429 0.5677 0.139 Uiso 1 1 calc R . . C107 C 0.4744(8) 1.0017(4) 0.5228(3) 0.078(4) Uiso 1 1 d DU . . H10N H 0.4051 1.0003 0.5122 0.094 Uiso 1 1 calc R . . H10O H 0.4904 0.9735 0.5427 0.094 Uiso 1 1 calc R . . C111 C 0.6368(13) 1.0353(9) 0.1180(9) 0.012(7) Uiso 0.300(13) 1 d PDU A 1 H11H H 0.6364 1.0112 0.0928 0.018 Uiso 0.300(13) 1 calc PR A 1 H11I H 0.6845 1.0278 0.1456 0.018 Uiso 0.300(13) 1 calc PR A 1 H11J H 0.6526 1.0651 0.1038 0.018 Uiso 0.300(13) 1 calc PR A 1 C112 C 0.5385(14) 1.0383(11) 0.1366(7) 0.023(7) Uiso 0.300(13) 1 d PDU A 1 H11K H 0.5230 1.0084 0.1517 0.028 Uiso 0.300(13) 1 calc PR A 1 H11L H 0.5387 1.0626 0.1622 0.028 Uiso 0.300(13) 1 calc PR A 1 C113 C 0.4639(15) 1.0495(17) 0.0944(7) 0.064(13) Uiso 0.300(13) 1 d PDU A 1 H11M H 0.4823 1.0782 0.0780 0.077 Uiso 0.300(13) 1 calc PR A 1 H11N H 0.4616 1.0242 0.0699 0.077 Uiso 0.300(13) 1 calc PR A 1 C114 C 0.3662(13) 1.0557(10) 0.1114(8) 0.044(9) Uiso 0.300(13) 1 d PDU A 1 H11O H 0.3705 1.0768 0.1401 0.052 Uiso 0.300(13) 1 calc PR A 1 H11P H 0.3423 1.0255 0.1220 0.052 Uiso 0.300(13) 1 calc PR A 1 C115 C 0.2968(17) 1.0754(7) 0.0703(11) 0.073(12) Uiso 0.300(13) 1 d PDU A 1 H11Q H 0.2460 1.0928 0.0848 0.087 Uiso 0.300(13) 1 calc PR A 1 H11R H 0.3309 1.0972 0.0503 0.087 Uiso 0.300(13) 1 calc PR A 1 C116 C 0.2522(18) 1.0373(8) 0.0375(10) 0.036(9) Uiso 0.300(13) 1 d PDU A 1 H11S H 0.2985 1.0263 0.0156 0.054 Uiso 0.300(13) 1 calc PR A 1 H11T H 0.1957 1.0493 0.0176 0.054 Uiso 0.300(13) 1 calc PR A 1 H11U H 0.2336 1.0117 0.0579 0.054 Uiso 0.300(13) 1 calc PR A 1 C120 C 0.335(2) 1.0497(17) 0.1047(16) 0.076(16) Uiso 0.200(13) 1 d PDU A 2 H12A H 0.3225 1.0671 0.1346 0.091 Uiso 0.200(13) 1 calc PR A 2 H12B H 0.3215 1.0167 0.1101 0.091 Uiso 0.200(13) 1 calc PR A 2 C121 C 0.271(2) 1.0676(11) 0.0605(17) 0.054(14) Uiso 0.200(13) 1 d PDU A 2 H12C H 0.2751 1.0468 0.0320 0.065 Uiso 0.200(13) 1 calc PR A 2 H12D H 0.2040 1.0680 0.0684 0.065 Uiso 0.200(13) 1 calc PR A 2 C122 C 0.301(3) 1.1162(11) 0.0471(17) 0.048(15) Uiso 0.200(13) 1 d PDU A 2 H12E H 0.2579 1.1387 0.0602 0.072 Uiso 0.200(13) 1 calc PR A 2 H12F H 0.2970 1.1192 0.0112 0.072 Uiso 0.200(13) 1 calc PR A 2 H12G H 0.3663 1.1220 0.0614 0.072 Uiso 0.200(13) 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 0.02591(18) 0.01767(15) 0.01775(19) 0.00083(13) 0.00328(14) -0.00200(14) Cl1 0.0448(14) 0.0285(11) 0.0209(13) -0.0016(9) 0.0061(11) -0.0008(10) Mg1 0.0240(16) 0.0299(15) 0.0178(18) 0.0030(12) -0.0006(13) -0.0037(12) N1 0.023(4) 0.019(3) 0.017(4) -0.002(3) 0.005(3) -0.003(3) C1 0.025(5) 0.020(4) 0.020(5) 0.000(4) -0.001(4) -0.002(4) Pb2 0.02698(19) 0.02232(17) 0.0198(2) 0.00069(14) 0.00108(15) 0.00025(14) Cl2 0.0352(13) 0.0205(10) 0.0267(14) 0.0035(9) 0.0053(10) -0.0008(9) Mg2 0.0283(17) 0.0313(15) 0.0228(19) -0.0036(13) 0.0024(14) -0.0061(13) N2 0.014(4) 0.022(3) 0.016(4) -0.004(3) 0.006(3) -0.004(3) C2 0.028(5) 0.020(4) 0.006(5) -0.007(3) 0.001(4) -0.003(4) Cl3 0.0273(12) 0.0322(12) 0.0373(15) -0.0035(10) 0.0037(11) -0.0046(10) N3 0.027(4) 0.021(4) 0.018(4) 0.003(3) -0.002(3) -0.003(3) C3 0.034(5) 0.020(4) 0.019(5) 0.012(4) 0.008(4) 0.003(4) Cl4 0.0519(16) 0.0292(11) 0.0310(15) 0.0020(10) -0.0036(12) -0.0149(11) N4 0.028(4) 0.022(4) 0.015(4) 0.001(3) 0.002(3) 0.005(3) C4 0.027(5) 0.016(4) 0.023(5) -0.006(4) 0.015(4) 0.000(4) N5 0.032(4) 0.025(4) 0.016(4) 0.001(3) 0.000(3) -0.003(3) C5 0.027(5) 0.016(4) 0.033(6) -0.004(4) 0.017(4) -0.009(4) N6 0.029(4) 0.022(4) 0.026(5) 0.007(3) 0.007(4) 0.009(3) C6 0.035(6) 0.031(5) 0.032(6) 0.012(4) -0.010(5) 0.006(4) N7 0.031(4) 0.024(4) 0.024(5) 0.001(3) 0.000(4) -0.001(3) C7 0.033(5) 0.021(4) 0.045(7) -0.003(4) -0.004(5) 0.004(4) N8 0.027(4) 0.032(4) 0.032(5) -0.013(3) 0.004(4) -0.005(3) C8 0.042(6) 0.037(5) 0.023(6) -0.001(4) -0.006(5) 0.006(4) C9 0.029(5) 0.028(5) 0.040(7) -0.002(4) 0.005(5) -0.006(4) C10 0.037(6) 0.050(6) 0.039(7) 0.000(5) 0.015(5) -0.021(5) C11 0.028(5) 0.032(5) 0.052(7) 0.008(5) 0.010(5) -0.004(4) C12 0.020(5) 0.020(4) 0.021(5) -0.002(4) -0.008(4) 0.001(4) C13 0.022(5) 0.014(4) 0.026(6) -0.002(4) 0.005(4) -0.002(4) C14 0.024(5) 0.029(5) 0.018(5) -0.005(4) 0.004(4) 0.003(4) C15 0.024(5) 0.031(5) 0.029(6) 0.007(4) 0.006(4) -0.004(4) C16 0.027(5) 0.026(5) 0.019(5) -0.003(4) 0.001(4) -0.010(4) C17 0.033(5) 0.023(4) 0.017(5) 0.003(4) -0.002(4) 0.000(4) C18 0.029(5) 0.031(5) 0.026(6) -0.005(4) -0.003(4) -0.002(4) C19 0.042(6) 0.052(6) 0.060(8) -0.005(5) 0.020(6) -0.014(5) C20 0.027(5) 0.032(5) 0.030(6) -0.007(4) -0.001(4) -0.007(4) C21 0.023(5) 0.021(4) 0.020(5) -0.007(4) 0.004(4) 0.001(4) C22 0.024(5) 0.029(5) 0.018(5) 0.002(4) 0.005(4) -0.006(4) C23 0.024(5) 0.028(5) 0.021(5) -0.007(4) 0.007(4) -0.009(4) C24 0.022(5) 0.032(5) 0.021(6) 0.006(4) 0.002(4) 0.001(4) C25 0.021(5) 0.027(4) 0.028(6) 0.002(4) 0.001(4) 0.005(4) C26 0.021(5) 0.025(5) 0.023(6) 0.006(4) 0.005(4) -0.008(4) C27 0.028(5) 0.026(4) 0.019(5) -0.008(4) 0.009(4) -0.009(4) C28 0.028(5) 0.024(5) 0.035(6) 0.000(4) 0.004(4) 0.010(4) C29 0.041(6) 0.068(7) 0.030(7) 0.004(5) 0.000(5) 0.013(5) C30 0.040(6) 0.021(4) 0.019(5) 0.002(4) 0.005(4) -0.002(4) C31 0.015(4) 0.025(4) 0.025(6) 0.007(4) -0.006(4) -0.007(4) C32 0.039(6) 0.014(4) 0.027(6) 0.005(4) -0.004(5) 0.001(4) C33 0.021(5) 0.020(4) 0.026(6) 0.004(4) 0.002(4) -0.004(4) C34 0.040(6) 0.014(4) 0.033(6) 0.003(4) 0.013(5) -0.003(4) C35 0.079(8) 0.045(6) 0.034(7) 0.013(5) 0.008(6) -0.006(5) C36 0.063(7) 0.048(6) 0.025(6) 0.005(5) 0.009(5) -0.010(5) C37 0.051(7) 0.059(6) 0.032(7) 0.012(5) -0.002(5) -0.011(5) C38 0.060(7) 0.025(5) 0.053(8) 0.000(5) 0.006(6) 0.007(5) C39 0.037(6) 0.029(5) 0.080(9) 0.007(5) 0.001(6) -0.002(4) C40 0.083(8) 0.027(5) 0.054(8) 0.001(5) 0.032(7) 0.020(5) C41 0.034(5) 0.018(4) 0.013(5) 0.002(3) 0.005(4) 0.003(4) C42 0.027(5) 0.025(4) 0.016(5) 0.005(4) -0.003(4) 0.000(4) C43 0.028(5) 0.023(4) 0.014(5) 0.009(4) -0.004(4) -0.013(4) C44 0.029(5) 0.024(4) 0.011(5) 0.005(4) -0.004(4) -0.003(4) C45 0.031(5) 0.029(5) 0.014(5) 0.001(4) 0.003(4) 0.003(4) C46 0.024(5) 0.030(5) 0.010(5) -0.005(4) -0.004(4) 0.005(4) C47 0.030(5) 0.039(5) 0.024(6) 0.002(4) -0.001(4) -0.001(4) C48 0.048(6) 0.026(5) 0.040(7) 0.001(4) 0.007(5) 0.000(4) C49 0.031(5) 0.040(5) 0.026(6) -0.010(4) -0.001(4) -0.003(4) C50 0.024(5) 0.010(4) 0.022(5) -0.004(3) 0.010(4) 0.000(3) C51 0.019(5) 0.019(4) 0.041(7) 0.003(4) -0.001(4) 0.003(4) C52 0.032(5) 0.022(4) 0.031(6) -0.004(4) 0.011(5) 0.004(4) C53 0.046(6) 0.019(4) 0.033(7) 0.001(4) 0.013(5) 0.011(4) C54 0.043(6) 0.029(5) 0.025(6) -0.005(4) 0.000(5) 0.002(4) C55 0.027(5) 0.014(4) 0.031(6) -0.001(4) 0.009(4) 0.002(4) C56 0.024(5) 0.049(6) 0.033(6) 0.005(4) -0.001(5) -0.005(4) C57 0.064(7) 0.037(5) 0.037(7) 0.003(5) 0.020(6) 0.001(5) C58 0.040(6) 0.040(5) 0.027(6) -0.005(4) 0.003(5) -0.004(4) C59 0.061(7) 0.042(5) 0.021(6) -0.012(4) 0.005(5) -0.007(5) C60 0.054(7) 0.019(4) 0.019(6) 0.000(4) 0.005(5) 0.003(4) C61 0.039(6) 0.026(5) 0.025(6) -0.004(4) 0.007(5) 0.020(4) C62 0.044(6) 0.031(5) 0.028(6) 0.013(4) 0.010(5) 0.011(4) C63 0.050(7) 0.053(6) 0.029(6) -0.004(5) 0.022(5) 0.016(5) C64 0.038(6) 0.024(4) 0.006(5) -0.002(3) -0.005(4) 0.002(4) C65 0.034(5) 0.040(5) 0.012(5) -0.006(4) 0.002(4) 0.002(5) C66 0.049(7) 0.038(5) 0.030(6) -0.011(4) 0.009(5) 0.010(5) C67 0.036(6) 0.071(7) 0.018(6) -0.007(5) 0.006(5) -0.010(6) C68 0.037(6) 0.059(6) 0.014(6) -0.008(5) 0.003(5) -0.021(5) C69 0.040(6) 0.045(6) 0.010(5) -0.007(4) -0.006(4) -0.011(5) C70 0.046(6) 0.025(4) 0.022(6) 0.001(4) 0.007(5) 0.005(4) C71 0.044(7) 0.117(10) 0.057(9) -0.016(7) 0.025(6) -0.008(7) C72 0.073(8) 0.030(5) 0.031(7) 0.000(4) -0.015(6) -0.019(5) C73 0.021(5) 0.035(5) 0.021(5) 0.004(4) 0.013(4) 0.002(4) C74 0.035(6) 0.024(5) 0.043(7) 0.010(4) 0.020(5) 0.008(4) C75 0.034(6) 0.021(5) 0.050(7) -0.006(4) 0.005(5) -0.003(4) C76 0.028(6) 0.042(6) 0.043(7) -0.003(5) 0.020(5) 0.007(5) C77 0.025(5) 0.062(7) 0.023(6) 0.002(5) 0.011(4) 0.024(5) C78 0.026(5) 0.037(5) 0.024(6) 0.005(4) 0.007(4) 0.006(4) C79 0.045(6) 0.037(5) 0.068(9) 0.014(5) 0.006(6) 0.009(5) C80 0.044(7) 0.053(6) 0.077(10) -0.005(6) -0.002(6) 0.001(5) C81 0.039(6) 0.050(6) 0.048(8) 0.007(5) 0.011(5) 0.011(5) C82 0.034(6) 0.052(6) 0.047(7) 0.013(5) 0.006(5) -0.016(5) C83 0.026(5) 0.022(4) 0.039(7) 0.001(4) 0.003(5) -0.001(4) C84 0.026(5) 0.030(5) 0.061(8) -0.008(5) -0.006(5) -0.014(4) C85 0.027(5) 0.034(5) 0.042(7) -0.016(5) 0.000(5) -0.007(4) C86 0.039(6) 0.057(6) 0.040(7) -0.021(5) 0.000(5) -0.011(5) C87 0.022(5) 0.031(5) 0.023(6) 0.005(4) 0.001(4) -0.004(4) C88 0.030(5) 0.034(5) 0.041(7) 0.012(5) 0.013(5) 0.000(4) C89 0.046(7) 0.073(7) 0.019(6) 0.015(5) -0.001(5) -0.009(6) C90 0.064(7) 0.055(6) 0.022(7) -0.006(5) 0.020(6) -0.004(6) C91 0.047(6) 0.047(6) 0.026(7) 0.000(5) 0.002(5) 0.005(5) C92 0.042(6) 0.029(5) 0.022(6) 0.004(4) 0.001(5) -0.001(4) C93 0.043(6) 0.054(6) 0.044(7) 0.019(5) 0.003(5) 0.002(5) C94 0.103(10) 0.100(9) 0.024(7) -0.015(6) -0.001(7) 0.011(7) C95 0.027(5) 0.044(5) 0.036(7) 0.001(5) -0.004(5) -0.001(4) C96 0.020(5) 0.034(5) 0.028(6) -0.016(4) -0.003(4) -0.008(4) C97 0.034(6) 0.036(5) 0.032(7) -0.014(4) -0.003(5) -0.003(4) C98 0.030(6) 0.045(6) 0.039(7) -0.020(5) 0.004(5) 0.010(4) C99 0.037(6) 0.058(6) 0.017(6) -0.008(5) -0.010(5) 0.002(5) C100 0.038(6) 0.040(5) 0.027(6) -0.011(5) -0.008(5) 0.011(5) C101 0.030(5) 0.032(5) 0.035(7) -0.008(4) -0.010(5) 0.006(4) C102 0.040(6) 0.032(5) 0.056(8) -0.016(5) 0.000(5) 0.004(4) C103 0.062(8) 0.094(8) 0.031(7) -0.007(6) 0.011(6) 0.010(6) C104 0.038(6) 0.034(5) 0.038(7) -0.005(4) -0.005(5) 0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 N1 2.277(6) . ? Pb1 N2 2.287(6) . ? Pb1 Cl1 2.739(2) . ? Cl1 Mg1 2.339(3) . ? Mg1 N6 2.016(7) . ? Mg1 N5 2.022(7) . ? Mg1 Cl2 2.331(3) . ? N1 C2 1.339(9) . ? N1 C12 1.422(10) . ? C1 C6 1.516(10) . ? C1 C8 1.525(11) . ? C1 C7 1.528(9) . ? C1 C2 1.554(10) . ? C117 C118 1.522(7) . ? C118 C119 1.516(7) . ? C119 C120 1.513(7) . ? Pb2 N3 2.258(6) . ? Pb2 N4 2.306(6) . ? Pb2 Cl3 2.825(2) . ? Pb2 Cl2 3.023(2) . ? Mg2 N8 2.018(7) . ? Mg2 N7 2.020(8) . ? Mg2 Cl4 2.288(3) . ? Mg2 Cl3 2.359(3) . ? N2 C4 1.344(9) . ? N2 C21 1.432(9) . ? C2 C3 1.401(10) . ? N3 C31 1.342(9) . ? N3 C41 1.448(9) . ? C3 C4 1.399(11) . ? N4 C33 1.317(9) . ? N4 C50 1.440(10) . ? C4 C5 1.551(10) . ? N5 C60 1.319(10) . ? N5 C64 1.427(10) . ? C5 C11 1.520(11) . ? C5 C9 1.533(10) . ? C5 C10 1.554(12) . ? N6 C62 1.327(11) . ? N6 C73 1.436(10) . ? N7 C83 1.333(10) . ? N7 C87 1.423(10) . ? N8 C85 1.319(10) . ? N8 C96 1.430(11) . ? C12 C13 1.374(11) . ? C12 C17 1.421(10) . ? C13 C14 1.384(10) . ? C13 C18 1.511(10) . ? C14 C15 1.394(10) . ? C15 C16 1.356(11) . ? C15 C19 1.519(11) . ? C16 C17 1.387(11) . ? C17 C20 1.511(11) . ? C21 C26 1.398(10) . ? C21 C22 1.401(11) . ? C22 C23 1.391(11) . ? C22 C27 1.500(10) . ? C23 C24 1.386(10) . ? C24 C25 1.367(11) . ? C24 C29 1.522(11) . ? C25 C26 1.378(11) . ? C26 C28 1.490(11) . ? C30 C37 1.519(11) . ? C30 C35 1.521(10) . ? C30 C36 1.539(11) . ? C30 C31 1.559(11) . ? C31 C32 1.409(11) . ? C32 C33 1.398(11) . ? C33 C34 1.558(10) . ? C34 C40 1.499(12) . ? C34 C39 1.516(12) . ? C34 C38 1.534(11) . ? C41 C46 1.389(10) . ? C41 C42 1.397(10) . ? C42 C43 1.395(10) . ? C42 C47 1.505(10) . ? C43 C44 1.386(10) . ? C44 C45 1.379(10) . ? C44 C48 1.505(10) . ? C45 C46 1.371(10) . ? C46 C49 1.514(10) . ? C50 C55 1.388(11) . ? C50 C51 1.395(10) . ? C51 C52 1.402(12) . ? C51 C56 1.518(11) . ? C52 C53 1.380(12) . ? C53 C54 1.370(11) . ? C53 C57 1.504(12) . ? C54 C55 1.384(12) . ? C55 C58 1.496(11) . ? C59 C60 1.525(11) . ? C60 C61 1.392(11) . ? C61 C62 1.418(12) . ? C62 C63 1.504(12) . ? C64 C65 1.394(10) . ? C64 C69 1.425(11) . ? C65 C66 1.370(11) . ? C65 C70 1.515(11) . ? C66 C67 1.395(12) . ? C67 C68 1.394(12) . ? C67 C71 1.495(12) . ? C68 C69 1.365(11) . ? C69 C72 1.516(11) . ? C73 C78 1.403(11) . ? C73 C74 1.405(10) . ? C74 C75 1.368(11) . ? C74 C79 1.513(12) . ? C75 C76 1.374(12) . ? C76 C77 1.363(11) . ? C76 C80 1.489(12) . ? C77 C78 1.398(11) . ? C78 C81 1.507(10) . ? C82 C83 1.517(12) . ? C83 C84 1.400(12) . ? C84 C85 1.402(13) . ? C85 C86 1.500(11) . ? C87 C88 1.394(11) . ? C87 C92 1.426(11) . ? C88 C89 1.372(12) . ? C88 C93 1.514(11) . ? C89 C90 1.405(12) . ? C90 C91 1.375(13) . ? C90 C94 1.501(13) . ? C91 C92 1.378(12) . ? C92 C95 1.503(11) . ? C96 C101 1.400(11) . ? C96 C97 1.407(11) . ? C97 C98 1.393(13) . ? C97 C102 1.523(12) . ? C98 C99 1.373(12) . ? C99 C100 1.371(12) . ? C99 C103 1.518(13) . ? C100 C101 1.399(13) . ? C101 C104 1.483(11) . ? C105 C106 1.494(7) . ? C106 C107 1.469(6) . ? C107 C107 1.505(7) 3_676 ? C111 C112 1.525(7) . ? C112 C113 1.513(7) . ? C113 C114 1.507(7) . ? C114 C115 1.521(7) . ? C115 C116 1.516(7) . ? C120 C121 1.523(7) . ? C121 C122 1.521(7) . ? 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 N2 82.2(2) . . ? N1 Pb1 Cl1 84.08(17) . . ? N2 Pb1 Cl1 83.05(17) . . ? Mg1 Cl1 Pb1 105.35(10) . . ? N6 Mg1 N5 94.2(3) . . ? N6 Mg1 Cl2 121.9(2) . . ? N5 Mg1 Cl2 120.3(2) . . ? N6 Mg1 Cl1 109.2(2) . . ? N5 Mg1 Cl1 113.2(2) . . ? Cl2 Mg1 Cl1 98.60(13) . . ? C2 N1 C12 126.4(6) . . ? C2 N1 Pb1 120.8(5) . . ? C12 N1 Pb1 112.7(4) . . ? C6 C1 C8 106.9(7) . . ? C6 C1 C7 107.8(6) . . ? C8 C1 C7 110.1(7) . . ? C6 C1 C2 116.1(6) . . ? C8 C1 C2 105.0(6) . . ? C7 C1 C2 110.7(6) . . ? C119 C118 C117 110.4(7) . . ? C120 C119 C118 111.6(7) . . ? N3 Pb2 N4 82.9(2) . . ? N3 Pb2 Cl3 89.63(16) . . ? N4 Pb2 Cl3 83.79(16) . . ? N3 Pb2 Cl2 95.51(16) . . ? N4 Pb2 Cl2 88.80(16) . . ? Cl3 Pb2 Cl2 170.41(6) . . ? Mg1 Cl2 Pb2 130.97(10) . . ? N8 Mg2 N7 94.7(3) . . ? N8 Mg2 Cl4 112.3(2) . . ? N7 Mg2 Cl4 119.1(2) . . ? N8 Mg2 Cl3 114.8(2) . . ? N7 Mg2 Cl3 110.1(2) . . ? Cl4 Mg2 Cl3 106.02(13) . . ? C4 N2 C21 127.8(6) . . ? C4 N2 Pb1 121.6(5) . . ? C21 N2 Pb1 110.5(4) . . ? N1 C2 C3 121.9(7) . . ? N1 C2 C1 124.0(7) . . ? C3 C2 C1 113.8(6) . . ? Mg2 Cl3 Pb2 104.66(9) . . ? C31 N3 C41 125.2(7) . . ? C31 N3 Pb2 121.0(5) . . ? C41 N3 Pb2 113.3(4) . . ? C4 C3 C2 133.9(7) . . ? C33 N4 C50 126.7(7) . . ? C33 N4 Pb2 121.9(6) . . ? C50 N4 Pb2 111.4(4) . . ? N2 C4 C3 121.3(7) . . ? N2 C4 C5 123.3(7) . . ? C3 C4 C5 115.0(7) . . ? C60 N5 C64 120.3(7) . . ? C60 N5 Mg1 120.4(6) . . ? C64 N5 Mg1 119.4(5) . . ? C11 C5 C9 109.0(6) . . ? C11 C5 C4 116.9(7) . . ? C9 C5 C4 111.0(6) . . ? C11 C5 C10 106.3(7) . . ? C9 C5 C10 108.7(7) . . ? C4 C5 C10 104.4(6) . . ? C62 N6 C73 118.6(7) . . ? C62 N6 Mg1 121.8(6) . . ? C73 N6 Mg1 119.6(5) . . ? C83 N7 C87 117.6(7) . . ? C83 N7 Mg2 122.2(6) . . ? C87 N7 Mg2 120.1(5) . . ? C85 N8 C96 118.5(7) . . ? C85 N8 Mg2 124.2(7) . . ? C96 N8 Mg2 117.3(5) . . ? C13 C12 C17 120.2(7) . . ? C13 C12 N1 120.6(6) . . ? C17 C12 N1 118.9(7) . . ? C12 C13 C14 119.4(7) . . ? C12 C13 C18 122.4(7) . . ? C14 C13 C18 118.2(7) . . ? C13 C14 C15 121.1(8) . . ? C16 C15 C14 118.9(8) . . ? C16 C15 C19 121.6(8) . . ? C14 C15 C19 119.5(8) . . ? C15 C16 C17 122.2(7) . . ? C16 C17 C12 118.0(8) . . ? C16 C17 C20 120.8(7) . . ? C12 C17 C20 121.0(7) . . ? C26 C21 C22 120.9(8) . . ? C26 C21 N2 119.5(7) . . ? C22 C21 N2 119.1(7) . . ? C23 C22 C21 118.1(7) . . ? C23 C22 C27 119.6(8) . . ? C21 C22 C27 122.3(7) . . ? C24 C23 C22 121.8(8) . . ? C25 C24 C23 118.3(8) . . ? C25 C24 C29 120.9(8) . . ? C23 C24 C29 120.8(8) . . ? C24 C25 C26 122.9(8) . . ? C25 C26 C21 118.1(8) . . ? C25 C26 C28 120.9(7) . . ? C21 C26 C28 120.9(7) . . ? C37 C30 C35 107.5(7) . . ? C37 C30 C36 108.4(7) . . ? C35 C30 C36 104.2(7) . . ? C37 C30 C31 113.0(7) . . ? C35 C30 C31 114.1(7) . . ? C36 C30 C31 109.2(7) . . ? N3 C31 C32 121.4(8) . . ? N3 C31 C30 123.1(7) . . ? C32 C31 C30 115.4(7) . . ? C33 C32 C31 134.4(8) . . ? N4 C33 C32 121.4(7) . . ? N4 C33 C34 124.1(8) . . ? C32 C33 C34 114.4(7) . . ? C40 C34 C39 107.5(8) . . ? C40 C34 C38 107.0(7) . . ? C39 C34 C38 108.5(7) . . ? C40 C34 C33 118.0(7) . . ? C39 C34 C33 110.6(7) . . ? C38 C34 C33 104.8(7) . . ? C46 C41 C42 120.1(7) . . ? C46 C41 N3 119.7(7) . . ? C42 C41 N3 119.8(7) . . ? C43 C42 C41 118.9(7) . . ? C43 C42 C47 119.6(7) . . ? C41 C42 C47 121.5(7) . . ? C44 C43 C42 120.9(7) . . ? C45 C44 C43 118.2(7) . . ? C45 C44 C48 121.5(7) . . ? C43 C44 C48 120.3(7) . . ? C46 C45 C44 122.4(8) . . ? C45 C46 C41 118.9(7) . . ? C45 C46 C49 117.7(7) . . ? C41 C46 C49 123.3(7) . . ? C55 C50 C51 120.7(8) . . ? C55 C50 N4 120.2(7) . . ? C51 C50 N4 118.9(7) . . ? C50 C51 C52 118.3(8) . . ? C50 C51 C56 121.4(8) . . ? C52 C51 C56 120.3(7) . . ? C53 C52 C51 121.7(8) . . ? C54 C53 C52 118.0(9) . . ? C54 C53 C57 122.3(9) . . ? C52 C53 C57 119.7(9) . . ? C53 C54 C55 122.8(9) . . ? C54 C55 C50 118.5(8) . . ? C54 C55 C58 120.8(8) . . ? C50 C55 C58 120.7(8) . . ? N5 C60 C61 125.9(8) . . ? N5 C60 C59 117.8(8) . . ? C61 C60 C59 116.3(8) . . ? C60 C61 C62 128.4(8) . . ? N6 C62 C61 123.6(8) . . ? N6 C62 C63 119.9(8) . . ? C61 C62 C63 116.5(9) . . ? C65 C64 C69 119.5(8) . . ? C65 C64 N5 119.2(7) . . ? C69 C64 N5 121.3(7) . . ? C66 C65 C64 119.3(8) . . ? C66 C65 C70 120.2(8) . . ? C64 C65 C70 120.5(8) . . ? C65 C66 C67 122.5(8) . . ? C68 C67 C66 117.5(9) . . ? C68 C67 C71 120.6(9) . . ? C66 C67 C71 122.0(9) . . ? C69 C68 C67 122.2(8) . . ? C68 C69 C64 119.1(8) . . ? C68 C69 C72 120.5(8) . . ? C64 C69 C72 120.4(8) . . ? C78 C73 C74 119.6(8) . . ? C78 C73 N6 119.9(7) . . ? C74 C73 N6 120.3(7) . . ? C75 C74 C73 119.2(8) . . ? C75 C74 C79 121.3(7) . . ? C73 C74 C79 119.5(8) . . ? C74 C75 C76 122.9(8) . . ? C77 C76 C75 117.4(8) . . ? C77 C76 C80 122.3(9) . . ? C75 C76 C80 120.3(8) . . ? C76 C77 C78 123.4(8) . . ? C77 C78 C73 117.5(7) . . ? C77 C78 C81 122.2(8) . . ? C73 C78 C81 120.3(8) . . ? N7 C83 C84 124.9(9) . . ? N7 C83 C82 118.5(8) . . ? C84 C83 C82 116.5(8) . . ? C83 C84 C85 130.2(8) . . ? N8 C85 C84 123.4(8) . . ? N8 C85 C86 120.8(9) . . ? C84 C85 C86 115.8(8) . . ? C88 C87 N7 122.8(8) . . ? C88 C87 C92 119.1(8) . . ? N7 C87 C92 118.0(7) . . ? C89 C88 C87 119.8(8) . . ? C89 C88 C93 121.6(9) . . ? C87 C88 C93 118.5(9) . . ? C88 C89 C90 122.2(9) . . ? C91 C90 C89 117.1(9) . . ? C91 C90 C94 122.9(9) . . ? C89 C90 C94 120.0(10) . . ? C90 C91 C92 123.2(9) . . ? C91 C92 C87 118.6(8) . . ? C91 C92 C95 120.4(8) . . ? C87 C92 C95 121.0(8) . . ? C101 C96 C97 119.4(9) . . ? C101 C96 N8 120.8(8) . . ? C97 C96 N8 119.6(8) . . ? C98 C97 C96 118.7(8) . . ? C98 C97 C102 121.8(8) . . ? C96 C97 C102 119.5(9) . . ? C99 C98 C97 122.5(9) . . ? C100 C99 C98 118.1(9) . . ? C100 C99 C103 120.5(9) . . ? C98 C99 C103 121.4(9) . . ? C99 C100 C101 122.2(9) . . ? C100 C101 C96 119.0(8) . . ? C100 C101 C104 120.6(8) . . ? C96 C101 C104 120.4(9) . . ? C107 C106 C105 115.9(7) . . ? C106 C107 C107 120.1(11) . 3_676 ? C113 C112 C111 110.1(7) . . ? C114 C113 C112 112.2(7) . . ? C113 C114 C115 111.0(7) . . ? C116 C115 C114 111.0(7) . . ? C119 C120 C121 110.5(7) . . ? C122 C121 C120 110.3(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.203 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.151 # Attachment '{(tBuMesNac)Sn}2.CIF' data_{(MesNac)Sn}2 _database_code_depnum_ccdc_archive 'CCDC 859478' #TrackingRef '{(tBuMesNac)Sn}2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H89 N4 Sn2' _chemical_formula_weight 1115.74 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.094(2) _cell_length_b 11.584(2) _cell_length_c 22.708(5) _cell_angle_alpha 94.78(3) _cell_angle_beta 98.11(3) _cell_angle_gamma 101.14(3) _cell_volume 2816.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1166 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9727 _exptl_absorpt_correction_T_max 0.9908 _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48811 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0154 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.60 _reflns_number_total 12819 _reflns_number_gt 11935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CifTAB _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. One half of a molecule of hexane of crystallisation, sitting on an inversion centre, was located in the asymmetric unit. Its carbon atoms were refined anisotropically. The low value (92.7%) for completeness of data to theta = 25 deg. arises from hardware constraints associated with the diffractometer used at the Australian Synchrotron and is common for triclinic data sets on that instrument. Its minimum crystal to detector distance is 72 mm and its goniometer only rotates about the phi axis. ; _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^)+(0.0487P)^2^+4.4626P] 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 12819 _refine_ls_number_parameters 629 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.157766(13) 0.977580(13) 0.237446(7) 0.01462(5) Uani 1 1 d . . . N1 N 0.27461(17) 0.99494(17) 0.32655(9) 0.0162(4) Uani 1 1 d . . . C1 C 0.3677(2) 1.1444(2) 0.41897(12) 0.0233(5) Uani 1 1 d . . . Sn2 Sn 0.271681(13) 1.236588(13) 0.226297(7) 0.01596(5) Uani 1 1 d . . . N2 N 0.00649(17) 0.97518(16) 0.29269(9) 0.0157(4) Uani 1 1 d . . . C2 C 0.2583(2) 1.0753(2) 0.36946(10) 0.0178(4) Uani 1 1 d . . . N3 N 0.13893(18) 1.35165(17) 0.20188(9) 0.0179(4) Uani 1 1 d . . . C3 C 0.1430(2) 1.1076(2) 0.37078(11) 0.0206(4) Uani 1 1 d . . . H3 H 0.1459 1.1824 0.3921 0.025 Uiso 1 1 calc R . . N4 N 0.26382(18) 1.20306(17) 0.12602(9) 0.0165(4) Uani 1 1 d . . . C4 C 0.0220(2) 1.0424(2) 0.34418(11) 0.0175(4) Uani 1 1 d . . . C5 C -0.0865(2) 1.0527(2) 0.37953(13) 0.0258(5) Uani 1 1 d . . . C6 C 0.3350(3) 1.1388(3) 0.48234(13) 0.0363(6) Uani 1 1 d . . . H6A H 0.3168 1.0561 0.4906 0.054 Uiso 1 1 calc R . . H6B H 0.2618 1.1734 0.4852 0.054 Uiso 1 1 calc R . . H6C H 0.4055 1.1834 0.5116 0.054 Uiso 1 1 calc R . . C7 C 0.4924(2) 1.1063(3) 0.41843(14) 0.0321(6) Uani 1 1 d . . . H7A H 0.5571 1.1605 0.4471 0.048 Uiso 1 1 calc R . . H7B H 0.5146 1.1084 0.3782 0.048 Uiso 1 1 calc R . . H7C H 0.4852 1.0256 0.4296 0.048 Uiso 1 1 calc R . . C8 C 0.3900(3) 1.2750(3) 0.40669(14) 0.0315(6) Uani 1 1 d . . . H8A H 0.3164 1.3071 0.4123 0.047 Uiso 1 1 calc R . . H8B H 0.4053 1.2803 0.3655 0.047 Uiso 1 1 calc R . . H8C H 0.4624 1.3205 0.4345 0.047 Uiso 1 1 calc R . . C9 C -0.0531(3) 1.1579(3) 0.42787(17) 0.0429(8) Uani 1 1 d . . . H9A H -0.1253 1.1628 0.4476 0.064 Uiso 1 1 calc R . . H9B H -0.0286 1.2309 0.4097 0.064 Uiso 1 1 calc R . . H9C H 0.0163 1.1478 0.4575 0.064 Uiso 1 1 calc R . . C10 C -0.1260(4) 0.9407(3) 0.40745(19) 0.0538(10) Uani 1 1 d . . . H10A H -0.0540 0.9240 0.4331 0.081 Uiso 1 1 calc R . . H10B H -0.1588 0.8746 0.3759 0.081 Uiso 1 1 calc R . . H10C H -0.1907 0.9507 0.4316 0.081 Uiso 1 1 calc R . . C11 C -0.2016(3) 1.0751(3) 0.33773(17) 0.0389(7) Uani 1 1 d . . . H11A H -0.2373 1.0046 0.3091 0.058 Uiso 1 1 calc R . . H11B H -0.1758 1.1428 0.3159 0.058 Uiso 1 1 calc R . . H11C H -0.2641 1.0919 0.3618 0.058 Uiso 1 1 calc R . . C12 C 0.3514(2) 0.9103(2) 0.33584(10) 0.0174(4) Uani 1 1 d . . . C13 C 0.3326(2) 0.8288(2) 0.37822(11) 0.0200(4) Uani 1 1 d . . . C14 C 0.4004(2) 0.7390(2) 0.38026(12) 0.0250(5) Uani 1 1 d . . . H14 H 0.3866 0.6835 0.4084 0.030 Uiso 1 1 calc R . . C15 C 0.4868(3) 0.7276(2) 0.34299(13) 0.0277(5) Uani 1 1 d . . . C16 C 0.5061(2) 0.8105(2) 0.30229(12) 0.0236(5) Uani 1 1 d . . . H16 H 0.5661 0.8051 0.2768 0.028 Uiso 1 1 calc R . . C17 C 0.4403(2) 0.9004(2) 0.29802(11) 0.0190(4) Uani 1 1 d . . . C18 C 0.2446(2) 0.8335(3) 0.42289(12) 0.0255(5) Uani 1 1 d . . . H18A H 0.1953 0.7539 0.4237 0.038 Uiso 1 1 calc R . . H18B H 0.1889 0.8867 0.4112 0.038 Uiso 1 1 calc R . . H18C H 0.2925 0.8630 0.4627 0.038 Uiso 1 1 calc R . . C19 C 0.5566(4) 0.6281(3) 0.34548(18) 0.0477(9) Uani 1 1 d . . . H19A H 0.5423 0.5874 0.3808 0.072 Uiso 1 1 calc R . . H19B H 0.6459 0.6604 0.3480 0.072 Uiso 1 1 calc R . . H19C H 0.5272 0.5718 0.3093 0.072 Uiso 1 1 calc R . . C20 C 0.4672(2) 0.9878(2) 0.25361(12) 0.0230(5) Uani 1 1 d . . . H20A H 0.5492 0.9864 0.2425 0.035 Uiso 1 1 calc R . . H20B H 0.4666 1.0675 0.2717 0.035 Uiso 1 1 calc R . . H20C H 0.4035 0.9664 0.2178 0.035 Uiso 1 1 calc R . . C21 C -0.0994(2) 0.88593(19) 0.26471(10) 0.0165(4) Uani 1 1 d . . . C22 C -0.1087(2) 0.7685(2) 0.27858(11) 0.0193(4) Uani 1 1 d . . . C23 C -0.2022(2) 0.6795(2) 0.24538(13) 0.0237(5) Uani 1 1 d . . . H23 H -0.2090 0.6006 0.2552 0.028 Uiso 1 1 calc R . . C24 C -0.2857(2) 0.7025(2) 0.19846(12) 0.0241(5) Uani 1 1 d . . . C25 C -0.2732(2) 0.8185(2) 0.18484(11) 0.0225(5) Uani 1 1 d . . . H25 H -0.3300 0.8359 0.1531 0.027 Uiso 1 1 calc R . . C26 C -0.1803(2) 0.9103(2) 0.21617(11) 0.0195(4) Uani 1 1 d . . . C27 C -0.0165(3) 0.7363(2) 0.32611(12) 0.0256(5) Uani 1 1 d . . . H27A H -0.0268 0.7709 0.3655 0.038 Uiso 1 1 calc R . . H27B H 0.0682 0.7669 0.3188 0.038 Uiso 1 1 calc R . . H27C H -0.0306 0.6499 0.3251 0.038 Uiso 1 1 calc R . . C28 C -0.3848(3) 0.6034(3) 0.16330(16) 0.0373(7) Uani 1 1 d . . . H28A H -0.3456 0.5422 0.1464 0.056 Uiso 1 1 calc R . . H28B H -0.4323 0.6346 0.1308 0.056 Uiso 1 1 calc R . . H28C H -0.4410 0.5690 0.1898 0.056 Uiso 1 1 calc R . . C29 C -0.1690(2) 1.0323(2) 0.19670(14) 0.0291(6) Uani 1 1 d . . . H29A H -0.2287 1.0721 0.2137 0.044 Uiso 1 1 calc R . . H29B H -0.1865 1.0263 0.1529 0.044 Uiso 1 1 calc R . . H29C H -0.0844 1.0781 0.2109 0.044 Uiso 1 1 calc R . . C30 C 0.1560(3) 1.5607(2) 0.16839(14) 0.0274(5) Uani 1 1 d . . . C31 C 0.1787(2) 1.4313(2) 0.16475(12) 0.0205(5) Uani 1 1 d . . . C32 C 0.2489(2) 1.4053(2) 0.12119(12) 0.0219(5) Uani 1 1 d . . . H32 H 0.2937 1.4726 0.1067 0.026 Uiso 1 1 calc R . . C33 C 0.2650(2) 1.2941(2) 0.09457(11) 0.0185(4) Uani 1 1 d . . . C34 C 0.2807(2) 1.2955(2) 0.02736(12) 0.0226(5) Uani 1 1 d . . . C35 C 0.0937(4) 1.5994(3) 0.2199(2) 0.0583(12) Uani 1 1 d . . . H35A H 0.1418 1.5883 0.2579 0.087 Uiso 1 1 calc R . . H35B H 0.0091 1.5517 0.2156 0.087 Uiso 1 1 calc R . . H35C H 0.0900 1.6832 0.2195 0.087 Uiso 1 1 calc R . . C36 C 0.2831(3) 1.6446(2) 0.17629(17) 0.0364(7) Uani 1 1 d . . . H36A H 0.2725 1.7267 0.1806 0.055 Uiso 1 1 calc R . . H36B H 0.3228 1.6309 0.1411 0.055 Uiso 1 1 calc R . . H36C H 0.3357 1.6298 0.2122 0.055 Uiso 1 1 calc R . . C37 C 0.0774(3) 1.5816(3) 0.10994(19) 0.0463(9) Uani 1 1 d . . . H37A H -0.0069 1.5335 0.1059 0.069 Uiso 1 1 calc R . . H37B H 0.1159 1.5590 0.0757 0.069 Uiso 1 1 calc R . . H37C H 0.0734 1.6655 0.1112 0.069 Uiso 1 1 calc R . . C38 C 0.1637(3) 1.3278(3) -0.00660(14) 0.0350(6) Uani 1 1 d . . . H38A H 0.1703 1.3275 -0.0492 0.053 Uiso 1 1 calc R . . H38B H 0.1565 1.4068 0.0097 0.053 Uiso 1 1 calc R . . H38C H 0.0898 1.2697 -0.0019 0.053 Uiso 1 1 calc R . . C39 C 0.3955(3) 1.3914(2) 0.02272(13) 0.0301(6) Uani 1 1 d . . . H39A H 0.4692 1.3752 0.0472 0.045 Uiso 1 1 calc R . . H39B H 0.3820 1.4693 0.0372 0.045 Uiso 1 1 calc R . . H39C H 0.4082 1.3907 -0.0191 0.045 Uiso 1 1 calc R . . C40 C 0.2975(3) 1.1811(2) -0.00680(12) 0.0287(5) Uani 1 1 d . . . H40A H 0.3030 1.1936 -0.0486 0.043 Uiso 1 1 calc R . . H40B H 0.2262 1.1172 -0.0054 0.043 Uiso 1 1 calc R . . H40C H 0.3741 1.1595 0.0118 0.043 Uiso 1 1 calc R . . C41 C 0.0268(2) 1.35206(19) 0.22574(12) 0.0196(4) Uani 1 1 d . . . C42 C 0.0306(2) 1.3775(2) 0.28763(12) 0.0231(5) Uani 1 1 d . . . C43 C -0.0794(3) 1.3824(2) 0.30967(13) 0.0277(5) Uani 1 1 d . . . H43 H -0.0762 1.4006 0.3515 0.033 Uiso 1 1 calc R . . C44 C -0.1938(3) 1.3613(2) 0.27236(15) 0.0305(6) Uani 1 1 d . . . C45 C -0.1955(2) 1.3340(2) 0.21177(15) 0.0305(6) Uani 1 1 d . . . H45 H -0.2728 1.3195 0.1856 0.037 Uiso 1 1 calc R . . C46 C -0.0875(2) 1.3268(2) 0.18754(13) 0.0244(5) Uani 1 1 d . . . C47 C 0.1514(3) 1.4043(3) 0.32960(14) 0.0344(6) Uani 1 1 d . . . H47A H 0.1368 1.4263 0.3702 0.052 Uiso 1 1 calc R . . H47B H 0.2081 1.4701 0.3170 0.052 Uiso 1 1 calc R . . H47C H 0.1886 1.3342 0.3292 0.052 Uiso 1 1 calc R . . C48 C -0.3125(3) 1.3642(3) 0.29747(19) 0.0443(8) Uani 1 1 d . . . H48A H -0.3422 1.2879 0.3117 0.066 Uiso 1 1 calc R . . H48B H -0.3760 1.3793 0.2661 0.066 Uiso 1 1 calc R . . H48C H -0.2963 1.4273 0.3309 0.066 Uiso 1 1 calc R . . C49 C -0.0980(3) 1.2897(3) 0.12113(14) 0.0315(6) Uani 1 1 d . . . H49A H -0.1002 1.3588 0.0992 0.047 Uiso 1 1 calc R . . H49B H -0.1746 1.2299 0.1075 0.047 Uiso 1 1 calc R . . H49C H -0.0261 1.2564 0.1138 0.047 Uiso 1 1 calc R . . C50 C 0.2801(2) 1.0889(2) 0.10360(10) 0.0175(4) Uani 1 1 d . . . C51 C 0.4010(2) 1.0676(2) 0.10648(11) 0.0199(4) Uani 1 1 d . . . C52 C 0.4156(2) 0.9575(2) 0.08199(12) 0.0236(5) Uani 1 1 d . . . H52 H 0.4972 0.9430 0.0828 0.028 Uiso 1 1 calc R . . C53 C 0.3147(3) 0.8688(2) 0.05663(11) 0.0236(5) Uani 1 1 d . . . C54 C 0.1953(2) 0.8893(2) 0.05777(11) 0.0220(5) Uani 1 1 d . . . H54 H 0.1253 0.8281 0.0418 0.026 Uiso 1 1 calc R . . C55 C 0.1764(2) 0.9984(2) 0.08192(11) 0.0183(4) Uani 1 1 d . . . C56 C 0.5133(2) 1.1625(2) 0.13196(12) 0.0247(5) Uani 1 1 d . . . H56A H 0.5876 1.1280 0.1361 0.037 Uiso 1 1 calc R . . H56B H 0.5028 1.1970 0.1713 0.037 Uiso 1 1 calc R . . H56C H 0.5228 1.2244 0.1051 0.037 Uiso 1 1 calc R . . C57 C 0.3343(3) 0.7530(3) 0.02732(14) 0.0328(6) Uani 1 1 d . . . H57A H 0.3531 0.7634 -0.0130 0.049 Uiso 1 1 calc R . . H57B H 0.2586 0.6919 0.0248 0.049 Uiso 1 1 calc R . . H57C H 0.4039 0.7288 0.0513 0.049 Uiso 1 1 calc R . . C58 C 0.0470(2) 1.0197(2) 0.08183(12) 0.0226(5) Uani 1 1 d . . . H58A H 0.0424 1.0622 0.1204 0.034 Uiso 1 1 calc R . . H58B H -0.0125 0.9437 0.0755 0.034 Uiso 1 1 calc R . . H58C H 0.0267 1.0673 0.0495 0.034 Uiso 1 1 calc R . . C59 C 0.0667(3) 1.5279(3) 0.49751(15) 0.0355(6) Uani 1 1 d . . . H59A H 0.0708 1.5412 0.4553 0.043 Uiso 1 1 calc R . . H59B H 0.0899 1.6062 0.5218 0.043 Uiso 1 1 calc R . . C60 C 0.1609(3) 1.4551(3) 0.51761(16) 0.0391(7) Uani 1 1 d . . . H60A H 0.1398 1.3776 0.4925 0.047 Uiso 1 1 calc R . . H60B H 0.1559 1.4400 0.5596 0.047 Uiso 1 1 calc R . . C61 C 0.2934(3) 1.5156(3) 0.51349(19) 0.0489(8) Uani 1 1 d . . . H61A H 0.2989 1.5312 0.4721 0.073 Uiso 1 1 calc R . . H61B H 0.3504 1.4639 0.5259 0.073 Uiso 1 1 calc R . . H61C H 0.3163 1.5905 0.5398 0.073 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 Sn1 0.01407(7) 0.01641(8) 0.01474(8) 0.00327(6) 0.00331(6) 0.00508(5) N1 0.0149(8) 0.0202(9) 0.0143(9) 0.0036(7) 0.0004(7) 0.0068(7) C1 0.0192(11) 0.0278(12) 0.0224(13) -0.0004(10) 0.0003(10) 0.0069(9) Sn2 0.01503(8) 0.01679(8) 0.01677(9) 0.00242(6) 0.00239(6) 0.00495(5) N2 0.0132(8) 0.0162(8) 0.0182(10) 0.0027(7) 0.0038(7) 0.0033(7) C2 0.0194(10) 0.0209(10) 0.0134(10) 0.0034(9) 0.0020(9) 0.0051(8) N3 0.0173(9) 0.0161(8) 0.0222(10) 0.0042(8) 0.0054(8) 0.0059(7) C3 0.0206(11) 0.0196(10) 0.0228(12) 0.0017(9) 0.0050(9) 0.0059(9) N4 0.0159(8) 0.0172(8) 0.0163(9) 0.0020(7) 0.0024(7) 0.0033(7) C4 0.0163(10) 0.0180(10) 0.0197(11) 0.0026(9) 0.0047(9) 0.0058(8) C5 0.0210(11) 0.0285(12) 0.0292(14) -0.0018(11) 0.0112(11) 0.0055(9) C6 0.0355(15) 0.0510(18) 0.0201(14) -0.0005(13) 0.0003(12) 0.0085(13) C7 0.0201(12) 0.0388(15) 0.0344(16) -0.0046(13) -0.0039(11) 0.0082(11) C8 0.0272(13) 0.0299(13) 0.0334(16) -0.0001(12) -0.0042(12) 0.0042(10) C9 0.0427(17) 0.0386(16) 0.052(2) -0.0026(15) 0.0266(16) 0.0106(14) C10 0.072(3) 0.0401(17) 0.063(2) 0.0150(17) 0.047(2) 0.0169(17) C11 0.0257(13) 0.0390(16) 0.053(2) -0.0039(14) 0.0106(14) 0.0093(12) C12 0.0162(9) 0.0199(10) 0.0177(11) 0.0036(9) 0.0020(9) 0.0078(8) C13 0.0173(10) 0.0258(11) 0.0180(11) 0.0057(9) 0.0016(9) 0.0064(9) C14 0.0269(12) 0.0268(12) 0.0246(13) 0.0104(10) 0.0039(10) 0.0104(10) C15 0.0284(12) 0.0278(12) 0.0326(14) 0.0093(11) 0.0068(11) 0.0156(10) C16 0.0239(11) 0.0264(12) 0.0245(13) 0.0041(10) 0.0078(10) 0.0116(10) C17 0.0156(10) 0.0253(11) 0.0169(11) 0.0042(9) 0.0013(9) 0.0063(8) C18 0.0239(11) 0.0359(13) 0.0210(12) 0.0118(11) 0.0059(10) 0.0110(10) C19 0.057(2) 0.0459(18) 0.060(2) 0.0265(17) 0.0280(18) 0.0376(17) C20 0.0190(10) 0.0301(12) 0.0240(12) 0.0098(10) 0.0074(10) 0.0090(9) C21 0.0138(9) 0.0173(10) 0.0191(11) 0.0017(8) 0.0063(8) 0.0027(8) C22 0.0173(10) 0.0172(10) 0.0246(12) 0.0031(9) 0.0061(9) 0.0041(8) C23 0.0219(11) 0.0169(10) 0.0325(14) 0.0001(10) 0.0085(10) 0.0027(9) C24 0.0171(10) 0.0261(12) 0.0271(13) -0.0053(10) 0.0057(10) 0.0021(9) C25 0.0170(10) 0.0324(12) 0.0184(12) 0.0017(10) 0.0032(9) 0.0056(9) C26 0.0160(10) 0.0245(11) 0.0197(11) 0.0054(9) 0.0053(9) 0.0057(8) C27 0.0301(12) 0.0199(11) 0.0281(13) 0.0072(10) 0.0031(11) 0.0080(9) C28 0.0257(13) 0.0353(15) 0.0431(19) -0.0100(13) -0.0006(13) -0.0021(11) C29 0.0217(11) 0.0306(13) 0.0384(16) 0.0177(12) 0.0051(11) 0.0078(10) C30 0.0310(13) 0.0162(10) 0.0410(16) 0.0105(10) 0.0147(12) 0.0099(9) C31 0.0195(10) 0.0161(10) 0.0276(13) 0.0056(9) 0.0044(9) 0.0060(8) C32 0.0227(11) 0.0186(10) 0.0267(13) 0.0086(9) 0.0077(10) 0.0048(9) C33 0.0154(9) 0.0192(10) 0.0218(12) 0.0054(9) 0.0047(9) 0.0031(8) C34 0.0232(11) 0.0236(11) 0.0217(12) 0.0076(10) 0.0055(10) 0.0030(9) C35 0.089(3) 0.0222(14) 0.083(3) 0.0141(16) 0.060(3) 0.0225(16) C36 0.0333(14) 0.0198(12) 0.054(2) -0.0014(12) 0.0058(14) 0.0032(10) C37 0.0371(16) 0.0268(14) 0.072(3) 0.0168(16) -0.0085(16) 0.0071(12) C38 0.0340(14) 0.0446(16) 0.0277(15) 0.0111(13) -0.0002(12) 0.0118(13) C39 0.0327(13) 0.0267(12) 0.0332(15) 0.0073(11) 0.0174(12) 0.0010(10) C40 0.0404(15) 0.0267(12) 0.0188(12) 0.0039(10) 0.0082(11) 0.0036(11) C41 0.0185(10) 0.0141(9) 0.0276(13) 0.0037(9) 0.0067(9) 0.0043(8) C42 0.0242(11) 0.0195(10) 0.0289(13) 0.0044(10) 0.0096(10) 0.0080(9) C43 0.0319(13) 0.0219(11) 0.0346(15) 0.0054(10) 0.0167(12) 0.0098(10) C44 0.0245(12) 0.0174(10) 0.0538(19) 0.0061(11) 0.0170(12) 0.0064(9) C45 0.0175(11) 0.0200(11) 0.0526(19) 0.0006(12) 0.0030(12) 0.0037(9) C46 0.0197(11) 0.0175(10) 0.0359(15) 0.0017(10) 0.0018(10) 0.0061(8) C47 0.0332(14) 0.0456(16) 0.0273(15) 0.0008(13) 0.0044(12) 0.0168(13) C48 0.0323(15) 0.0319(15) 0.077(3) 0.0104(16) 0.0297(17) 0.0114(12) C49 0.0270(13) 0.0294(13) 0.0362(16) 0.0011(12) -0.0023(12) 0.0071(10) C50 0.0198(10) 0.0184(10) 0.0163(11) 0.0041(8) 0.0057(9) 0.0055(8) C51 0.0181(10) 0.0247(11) 0.0181(11) 0.0034(9) 0.0044(9) 0.0059(9) C52 0.0238(11) 0.0287(12) 0.0223(12) 0.0039(10) 0.0072(10) 0.0121(10) C53 0.0312(13) 0.0219(11) 0.0200(12) 0.0020(9) 0.0060(10) 0.0098(10) C54 0.0268(12) 0.0198(10) 0.0192(12) 0.0013(9) 0.0045(10) 0.0041(9) C55 0.0190(10) 0.0202(10) 0.0167(11) 0.0033(9) 0.0044(9) 0.0047(8) C56 0.0165(10) 0.0294(12) 0.0275(13) 0.0015(10) 0.0035(10) 0.0043(9) C57 0.0434(16) 0.0276(13) 0.0315(15) -0.0003(11) 0.0118(13) 0.0147(12) C58 0.0174(10) 0.0250(11) 0.0253(13) 0.0021(10) 0.0031(9) 0.0042(9) C59 0.0410(16) 0.0273(13) 0.0359(16) -0.0043(12) 0.0125(14) 0.0001(12) C60 0.0420(17) 0.0367(15) 0.0351(17) -0.0002(13) 0.0059(14) 0.0012(13) C61 0.0409(18) 0.050(2) 0.050(2) -0.0024(17) 0.0039(17) 0.0008(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 Sn1 N1 2.215(2) . ? Sn1 N2 2.2300(19) . ? Sn1 Sn2 3.0685(9) . ? N1 C2 1.346(3) . ? N1 C12 1.428(3) . ? C1 C7 1.532(3) . ? C1 C6 1.536(4) . ? C1 C8 1.540(4) . ? C1 C2 1.571(4) . ? Sn2 N3 2.215(2) . ? Sn2 N4 2.264(2) . ? N2 C4 1.320(3) . ? N2 C21 1.436(3) . ? C2 C3 1.403(3) . ? N3 C31 1.354(3) . ? N3 C41 1.426(3) . ? C3 C4 1.428(3) . ? C3 H3 0.9500 . ? N4 C33 1.321(3) . ? N4 C50 1.431(3) . ? C4 C5 1.556(3) . ? C5 C10 1.507(4) . ? C5 C9 1.522(4) . ? C5 C11 1.557(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.410(3) . ? C12 C13 1.412(3) . ? C13 C14 1.395(3) . ? C13 C18 1.509(3) . ? C14 C15 1.383(4) . ? C14 H14 0.9500 . ? C15 C16 1.395(4) . ? C15 C19 1.509(4) . ? C16 C17 1.385(3) . ? C16 H16 0.9500 . ? C17 C20 1.507(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 C26 1.404(3) . ? C21 C22 1.410(3) . ? C22 C23 1.394(3) . ? C22 C27 1.501(3) . ? C23 C24 1.389(4) . ? C23 H23 0.9500 . ? C24 C25 1.390(4) . ? C24 C28 1.509(4) . ? C25 C26 1.394(4) . ? C25 H25 0.9500 . ? C26 C29 1.504(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C35 1.519(4) . ? C30 C36 1.528(4) . ? C30 C37 1.545(4) . ? C30 C31 1.566(3) . ? C31 C32 1.391(3) . ? C32 C33 1.430(3) . ? C32 H32 0.9500 . ? C33 C34 1.562(3) . ? C34 C40 1.535(4) . ? C34 C38 1.541(4) . ? C34 C39 1.542(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? 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 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C46 1.397(4) . ? C41 C42 1.405(4) . ? C42 C43 1.393(3) . ? C42 C47 1.493(4) . ? C43 C44 1.389(4) . ? C43 H43 0.9500 . ? C44 C45 1.383(5) . ? C44 C48 1.512(4) . ? C45 C46 1.400(4) . ? C45 H45 0.9500 . ? C46 C49 1.515(4) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C55 1.398(3) . ? C50 C51 1.403(3) . ? C51 C52 1.397(3) . ? C51 C56 1.502(4) . ? C52 C53 1.384(4) . ? C52 H52 0.9500 . ? C53 C54 1.394(4) . ? C53 C57 1.514(4) . ? C54 C55 1.400(3) . ? C54 H54 0.9500 . ? C55 C58 1.503(3) . ? 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 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.511(5) . ? C59 C59 1.519(6) 2_586 ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.520(5) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 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 N1 Sn1 N2 82.29(7) . . ? N1 Sn1 Sn2 89.05(6) . . ? N2 Sn1 Sn2 108.23(5) . . ? C2 N1 C12 124.81(19) . . ? C2 N1 Sn1 117.96(14) . . ? C12 N1 Sn1 116.82(15) . . ? C7 C1 C6 108.1(2) . . ? C7 C1 C8 106.2(2) . . ? C6 C1 C8 107.9(2) . . ? C7 C1 C2 115.3(2) . . ? C6 C1 C2 112.4(2) . . ? C8 C1 C2 106.6(2) . . ? N3 Sn2 N4 83.81(8) . . ? N3 Sn2 Sn1 116.38(5) . . ? N4 Sn2 Sn1 93.39(6) . . ? C4 N2 C21 128.82(19) . . ? C4 N2 Sn1 122.38(15) . . ? C21 N2 Sn1 108.67(14) . . ? N1 C2 C3 121.8(2) . . ? N1 C2 C1 122.6(2) . . ? C3 C2 C1 115.5(2) . . ? C31 N3 C41 121.32(19) . . ? C31 N3 Sn2 113.39(15) . . ? C41 N3 Sn2 125.09(15) . . ? C2 C3 C4 128.4(2) . . ? C2 C3 H3 115.8 . . ? C4 C3 H3 115.8 . . ? C33 N4 C50 124.7(2) . . ? C33 N4 Sn2 118.05(16) . . ? C50 N4 Sn2 116.25(14) . . ? N2 C4 C3 120.2(2) . . ? N2 C4 C5 122.9(2) . . ? C3 C4 C5 116.8(2) . . ? C10 C5 C9 109.4(3) . . ? C10 C5 C4 110.7(2) . . ? C9 C5 C4 112.5(2) . . ? C10 C5 C11 108.3(3) . . ? C9 C5 C11 104.6(2) . . ? C4 C5 C11 111.1(2) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 C8 H8A 109.5 . . ? C1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 119.0(2) . . ? C17 C12 N1 119.2(2) . . ? C13 C12 N1 121.5(2) . . ? C14 C13 C12 118.9(2) . . ? C14 C13 C18 117.2(2) . . ? C12 C13 C18 124.0(2) . . ? C15 C14 C13 122.7(2) . . ? C15 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? C14 C15 C16 117.7(2) . . ? C14 C15 C19 121.3(2) . . ? C16 C15 C19 121.0(2) . . ? C17 C16 C15 121.9(2) . . ? C17 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C16 C17 C12 119.9(2) . . ? C16 C17 C20 119.0(2) . . ? C12 C17 C20 121.1(2) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 119.6(2) . . ? C26 C21 N2 119.9(2) . . ? C22 C21 N2 119.5(2) . . ? C23 C22 C21 119.1(2) . . ? C23 C22 C27 119.3(2) . . ? C21 C22 C27 121.5(2) . . ? C24 C23 C22 122.1(2) . . ? C24 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? C23 C24 C25 117.7(2) . . ? C23 C24 C28 120.4(2) . . ? C25 C24 C28 121.8(3) . . ? C24 C25 C26 122.3(2) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C21 119.1(2) . . ? C25 C26 C29 119.0(2) . . ? C21 C26 C29 121.9(2) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C36 106.0(3) . . ? C35 C30 C37 107.2(3) . . ? C36 C30 C37 108.4(2) . . ? C35 C30 C31 116.6(2) . . ? C36 C30 C31 107.4(2) . . ? C37 C30 C31 110.9(2) . . ? N3 C31 C32 122.0(2) . . ? N3 C31 C30 123.9(2) . . ? C32 C31 C30 114.1(2) . . ? C31 C32 C33 130.7(2) . . ? C31 C32 H32 114.6 . . ? C33 C32 H32 114.6 . . ? N4 C33 C32 120.6(2) . . ? N4 C33 C34 126.6(2) . . ? C32 C33 C34 112.8(2) . . ? C40 C34 C38 106.4(2) . . ? C40 C34 C39 106.3(2) . . ? C38 C34 C39 109.0(2) . . ? C40 C34 C33 118.2(2) . . ? C38 C34 C33 107.8(2) . . ? C39 C34 C33 108.9(2) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C30 C36 H36A 109.5 . . ? C30 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C30 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C30 C37 H37A 109.5 . . ? C30 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C30 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34 C40 H40A 109.5 . . ? C34 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C34 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C46 C41 C42 119.7(2) . . ? C46 C41 N3 120.0(2) . . ? C42 C41 N3 120.3(2) . . ? C43 C42 C41 119.3(2) . . ? C43 C42 C47 119.7(2) . . ? C41 C42 C47 120.9(2) . . ? C44 C43 C42 122.0(3) . . ? C44 C43 H43 119.0 . . ? C42 C43 H43 119.0 . . ? C45 C44 C43 117.5(2) . . ? C45 C44 C48 121.3(3) . . ? C43 C44 C48 121.1(3) . . ? C44 C45 C46 122.6(3) . . ? C44 C45 H45 118.7 . . ? C46 C45 H45 118.7 . . ? C41 C46 C45 118.8(3) . . ? C41 C46 C49 121.9(2) . . ? C45 C46 C49 119.3(2) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C55 C50 C51 120.7(2) . . ? C55 C50 N4 120.1(2) . . ? C51 C50 N4 119.2(2) . . ? C52 C51 C50 118.4(2) . . ? C52 C51 C56 120.1(2) . . ? C50 C51 C56 121.4(2) . . ? C53 C52 C51 122.0(2) . . ? C53 C52 H52 119.0 . . ? C51 C52 H52 119.0 . . ? C52 C53 C54 118.5(2) . . ? C52 C53 C57 120.5(2) . . ? C54 C53 C57 121.0(3) . . ? C53 C54 C55 121.3(2) . . ? C53 C54 H54 119.3 . . ? C55 C54 H54 119.3 . . ? C50 C55 C54 118.8(2) . . ? C50 C55 C58 120.5(2) . . ? C54 C55 C58 120.6(2) . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C53 C57 H57A 109.5 . . ? C53 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C53 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 C59 114.5(3) . 2_586 ? C60 C59 H59A 108.6 . . ? C59 C59 H59A 108.6 2_586 . ? C60 C59 H59B 108.6 . . ? C59 C59 H59B 108.6 2_586 . ? H59A C59 H59B 107.6 . . ? C59 C60 C61 112.7(3) . . ? C59 C60 H60A 109.0 . . ? C61 C60 H60A 109.0 . . ? C59 C60 H60B 109.0 . . ? C61 C60 H60B 109.0 . . ? H60A C60 H60B 107.8 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.436 _refine_diff_density_min -1.877 _refine_diff_density_rms 0.096