Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Dalton Trans. _journal_coden_cambridge 0182 _publ_section_title ;High Tacticity Control in Organolanthanide Polymerization Catalysis: Formation of Isotactic Poly(alpha-alkenes) with a Chiral C3-Symmetric Thulium Complex ; _publ_contact_author_name 'Prof. Lutz Gade' _publ_contact_author_email LUTZ.GADE@UNI-HD.DE loop_ _publ_author_name 'Lutz Gade' 'Stephane Bellemin-Laponnaz' 'Lenka Lukesova' 'Hubert Wadepohl' 'Benjamin D. Ward' # Attachment 'ga_ml4-ga_ml3.cif' data_ga_ml4 _database_code_depnum_ccdc_archive 'CCDC 627376' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H66 N3 O3 Si3 Tm' _chemical_formula_weight 794.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_int_tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.2419(7) _cell_length_b 19.1519(13) _cell_length_c 10.3873(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.0530(10) _cell_angle_gamma 90.00 _cell_volume 1992.6(2) _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 plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 2.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7196 _exptl_absorpt_correction_T_max 0.7196 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19507 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 32.03 _reflns_number_total 10696 _reflns_number_gt 9802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0392P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(6) _refine_ls_number_reflns 10696 _refine_ls_number_parameters 395 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0769 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Tm1 Tm 0.112895(11) 0.502526(10) 0.241538(11) 0.01060(4) Uani 1 1 d . . . Si1 Si -0.12068(10) 0.48122(6) -0.09675(10) 0.0154(2) Uani 1 1 d . . . Si2 Si -0.16986(10) 0.60850(6) 0.35042(11) 0.0153(2) Uani 1 1 d . . . Si3 Si 0.25661(12) 0.66877(6) 0.12055(11) 0.0160(2) Uani 1 1 d . . . O1 O 0.3335(4) 0.2889(2) 0.2607(3) 0.0189(7) Uani 1 1 d . . . O2 O 0.1425(3) 0.33101(16) 0.5653(2) 0.0164(5) Uani 1 1 d . . . O3 O 0.4909(3) 0.43781(15) 0.5496(3) 0.0167(5) Uani 1 1 d . . . N1 N 0.2490(3) 0.39557(18) 0.2028(3) 0.0139(6) Uani 1 1 d . . . N2 N 0.0705(3) 0.40479(17) 0.3966(3) 0.0134(6) Uani 1 1 d . . . N3 N 0.3135(3) 0.4953(2) 0.4321(3) 0.0134(7) Uani 1 1 d . . . C1 C 0.2946(3) 0.3523(2) 0.2925(4) 0.0135(6) Uani 1 1 d . . . C2 C 0.2968(5) 0.2862(2) 0.1159(4) 0.0218(8) Uani 1 1 d . . . H2A H 0.2205 0.2542 0.0862 0.026 Uiso 1 1 calc R . . H2B H 0.3731 0.2704 0.0785 0.026 Uiso 1 1 calc R . . C3 C 0.2584(4) 0.3619(2) 0.0755(4) 0.0156(7) Uani 1 1 d . . . H3 H 0.1683 0.3623 0.0154 0.019 Uiso 1 1 calc R . . C4 C 0.3581(4) 0.4004(2) 0.0085(3) 0.0165(7) Uani 1 1 d . . . H4 H 0.3257 0.4496 -0.0067 0.020 Uiso 1 1 calc R . . C5 C 0.4975(4) 0.4037(3) 0.0932(4) 0.0262(9) Uani 1 1 d . . . H5A H 0.4949 0.4278 0.1759 0.039 Uiso 1 1 calc R . . H5B H 0.5562 0.4291 0.0463 0.039 Uiso 1 1 calc R . . H5C H 0.5316 0.3562 0.1125 0.039 Uiso 1 1 calc R . . C6 C 0.3571(4) 0.3685(2) -0.1259(4) 0.0205(8) Uani 1 1 d . . . H6A H 0.4105 0.3975 -0.1731 0.031 Uiso 1 1 calc R . . H6B H 0.2650 0.3661 -0.1766 0.031 Uiso 1 1 calc R . . H6C H 0.3949 0.3214 -0.1146 0.031 Uiso 1 1 calc R . . C7 C 0.1644(4) 0.3686(2) 0.4633(3) 0.0126(6) Uani 1 1 d . . . C8 C 0.0063(4) 0.3481(2) 0.5768(3) 0.0185(8) Uani 1 1 d . . . H8A H 0.0063 0.3771 0.6557 0.022 Uiso 1 1 calc R . . H8B H -0.0463 0.3052 0.5820 0.022 Uiso 1 1 calc R . . C9 C -0.0505(4) 0.3891(2) 0.4500(3) 0.0143(7) Uani 1 1 d . . . H9 H -0.0905 0.4338 0.4732 0.017 Uiso 1 1 calc R . . C10 C -0.1552(4) 0.3487(2) 0.3496(4) 0.0162(7) Uani 1 1 d . . . H10 H -0.1807 0.3782 0.2688 0.019 Uiso 1 1 calc R . . C11 C -0.1007(5) 0.2792(3) 0.3091(5) 0.0284(10) Uani 1 1 d . . . H11A H -0.0734 0.2496 0.3870 0.043 Uiso 1 1 calc R . . H11B H -0.0236 0.2882 0.2694 0.043 Uiso 1 1 calc R . . H11C H -0.1704 0.2554 0.2451 0.043 Uiso 1 1 calc R . . C12 C -0.2804(4) 0.3369(2) 0.4048(4) 0.0219(8) Uani 1 1 d . . . H12A H -0.2575 0.3092 0.4858 0.033 Uiso 1 1 calc R . . H12B H -0.3471 0.3118 0.3398 0.033 Uiso 1 1 calc R . . H12C H -0.3169 0.3820 0.4243 0.033 Uiso 1 1 calc R . . C13 C 0.3693(4) 0.4376(2) 0.4718(4) 0.0104(7) Uani 1 1 d . . . C14 C 0.5323(3) 0.5103(3) 0.5577(4) 0.0191(8) Uani 1 1 d . . . H14A H 0.6046 0.5181 0.5092 0.023 Uiso 1 1 calc R . . H14B H 0.5644 0.5246 0.6505 0.023 Uiso 1 1 calc R . . C15 C 0.4060(4) 0.5512(2) 0.4940(4) 0.0126(7) Uani 1 1 d . . . H15 H 0.4267 0.5825 0.4240 0.015 Uiso 1 1 calc R . . C16 C 0.3452(4) 0.5947(2) 0.5920(4) 0.0158(7) Uani 1 1 d . . . H16 H 0.2603 0.6157 0.5419 0.019 Uiso 1 1 calc R . . C17 C 0.3109(5) 0.5510(3) 0.7018(5) 0.0319(11) Uani 1 1 d . . . H17A H 0.3931 0.5323 0.7565 0.048 Uiso 1 1 calc R . . H17B H 0.2525 0.5124 0.6641 0.048 Uiso 1 1 calc R . . H17C H 0.2650 0.5802 0.7560 0.048 Uiso 1 1 calc R . . C18 C 0.4394(4) 0.6547(2) 0.6470(4) 0.0191(8) Uani 1 1 d . . . H18A H 0.3956 0.6853 0.7007 0.029 Uiso 1 1 calc R . . H18B H 0.4614 0.6816 0.5740 0.029 Uiso 1 1 calc R . . H18C H 0.5215 0.6357 0.7014 0.029 Uiso 1 1 calc R . . C19 C 0.3068(3) 0.36522(19) 0.4398(3) 0.0115(6) Uani 1 1 d . . . C20 C 0.3894(4) 0.3085(2) 0.5234(4) 0.0160(7) Uani 1 1 d . . . H20A H 0.3444 0.2634 0.5048 0.024 Uiso 1 1 calc R . . H20B H 0.3986 0.3198 0.6169 0.024 Uiso 1 1 calc R . . H20C H 0.4780 0.3062 0.5020 0.024 Uiso 1 1 calc R . . C21 C -0.0583(4) 0.4526(2) 0.0744(4) 0.0165(7) Uani 1 1 d . . . H21A H -0.0308 0.4034 0.0672 0.020 Uiso 1 1 calc R . . H21B H -0.1383 0.4509 0.1137 0.020 Uiso 1 1 calc R . . C22 C -0.2257(4) 0.5625(2) -0.1022(4) 0.0240(9) Uani 1 1 d . . . H22A H -0.3078 0.5514 -0.0722 0.036 Uiso 1 1 calc R . . H22B H -0.2483 0.5802 -0.1927 0.036 Uiso 1 1 calc R . . H22C H -0.1754 0.5982 -0.0446 0.036 Uiso 1 1 calc R . . C23 C -0.2235(4) 0.4125(3) -0.2010(4) 0.0243(9) Uani 1 1 d . . . H23A H -0.1729 0.3687 -0.1942 0.036 Uiso 1 1 calc R . . H23B H -0.2445 0.4279 -0.2930 0.036 Uiso 1 1 calc R . . H23C H -0.3065 0.4050 -0.1702 0.036 Uiso 1 1 calc R . . C24 C 0.0182(3) 0.5031(4) -0.1827(3) 0.0222(6) Uani 1 1 d . . . H24A H 0.0645 0.5452 -0.1432 0.033 Uiso 1 1 calc R . . H24B H -0.0189 0.5116 -0.2762 0.033 Uiso 1 1 calc R . . H24C H 0.0813 0.4641 -0.1735 0.033 Uiso 1 1 calc R . . C25 C 0.0040(4) 0.5799(2) 0.3664(4) 0.0173(7) Uani 1 1 d . . . H25A H 0.0283 0.5612 0.4571 0.021 Uiso 1 1 calc R . . H25B H 0.0545 0.6241 0.3682 0.021 Uiso 1 1 calc R . . C26 C -0.2121(4) 0.6859(2) 0.2376(4) 0.0243(9) Uani 1 1 d . . . H26A H -0.1478 0.7235 0.2669 0.037 Uiso 1 1 calc R . . H26B H -0.3023 0.7022 0.2397 0.037 Uiso 1 1 calc R . . H26C H -0.2081 0.6722 0.1476 0.037 Uiso 1 1 calc R . . C27 C -0.2974(4) 0.5404(2) 0.2788(4) 0.0225(8) Uani 1 1 d . . . H27A H -0.2909 0.5304 0.1879 0.034 Uiso 1 1 calc R . . H27B H -0.3871 0.5578 0.2802 0.034 Uiso 1 1 calc R . . H27C H -0.2806 0.4975 0.3313 0.034 Uiso 1 1 calc R . . C28 C -0.2080(4) 0.6325(2) 0.5153(4) 0.0218(8) Uani 1 1 d . . . H28A H -0.1841 0.5935 0.5767 0.033 Uiso 1 1 calc R . . H28B H -0.3034 0.6427 0.5044 0.033 Uiso 1 1 calc R . . H28C H -0.1561 0.6739 0.5502 0.033 Uiso 1 1 calc R . . C29 C 0.2535(4) 0.5734(2) 0.1373(4) 0.0157(7) Uani 1 1 d . . . H29A H 0.3458 0.5604 0.1807 0.019 Uiso 1 1 calc R . . H29B H 0.2404 0.5553 0.0463 0.019 Uiso 1 1 calc R . . C30 C 0.0853(5) 0.7030(3) 0.0458(5) 0.0287(9) Uani 1 1 d . . . H30A H 0.0524 0.6804 -0.0394 0.043 Uiso 1 1 calc R . . H30B H 0.0899 0.7536 0.0332 0.043 Uiso 1 1 calc R . . H30C H 0.0245 0.6929 0.1048 0.043 Uiso 1 1 calc R . . C31 C 0.3149(6) 0.7125(3) 0.2827(5) 0.0277(12) Uani 1 1 d . . . H31A H 0.2574 0.6987 0.3428 0.042 Uiso 1 1 calc R . . H31B H 0.3109 0.7632 0.2707 0.042 Uiso 1 1 calc R . . H31C H 0.4071 0.6985 0.3199 0.042 Uiso 1 1 calc R . . C32 C 0.3717(5) 0.7014(3) 0.0142(4) 0.0280(10) Uani 1 1 d . . . H32A H 0.4631 0.6862 0.0514 0.042 Uiso 1 1 calc R . . H32B H 0.3685 0.7526 0.0108 0.042 Uiso 1 1 calc R . . H32C H 0.3433 0.6826 -0.0750 0.042 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 Tm1 0.01037(5) 0.00940(6) 0.01150(5) 0.00077(9) 0.00105(4) 0.00078(8) Si1 0.0140(4) 0.0181(5) 0.0130(4) -0.0007(3) 0.0007(3) -0.0003(4) Si2 0.0141(5) 0.0121(5) 0.0198(5) -0.0017(4) 0.0039(4) 0.0010(4) Si3 0.0195(5) 0.0132(6) 0.0147(5) 0.0007(4) 0.0017(4) -0.0031(4) O1 0.0252(16) 0.0126(16) 0.0206(15) -0.0029(12) 0.0086(12) 0.0044(13) O2 0.0143(12) 0.0216(15) 0.0138(11) 0.0051(10) 0.0043(9) 0.0013(11) O3 0.0111(12) 0.0148(14) 0.0226(13) -0.0004(11) -0.0004(10) -0.0004(10) N1 0.0145(14) 0.0135(15) 0.0139(13) -0.0030(12) 0.0035(11) 0.0009(12) N2 0.0115(13) 0.0118(15) 0.0173(14) 0.0004(12) 0.0041(11) -0.0011(12) N3 0.0132(11) 0.012(2) 0.0150(11) -0.0022(13) 0.0025(9) -0.0048(13) C1 0.0116(15) 0.0113(17) 0.0181(16) -0.0036(13) 0.0043(12) -0.0008(12) C2 0.032(2) 0.016(2) 0.0180(18) -0.0048(15) 0.0078(16) -0.0043(17) C3 0.0163(17) 0.017(2) 0.0120(16) -0.0062(14) -0.0003(13) 0.0015(15) C4 0.0222(18) 0.0150(18) 0.0138(15) -0.0004(13) 0.0074(14) 0.0018(14) C5 0.022(2) 0.035(3) 0.0234(19) -0.0125(18) 0.0081(16) -0.0094(18) C6 0.026(2) 0.023(2) 0.0138(16) -0.0013(15) 0.0068(15) -0.0009(16) C7 0.0136(15) 0.0108(16) 0.0132(15) -0.0010(12) 0.0025(12) -0.0018(12) C8 0.0150(16) 0.028(2) 0.0139(16) -0.0001(15) 0.0055(13) -0.0012(15) C9 0.0123(15) 0.0150(18) 0.0165(16) -0.0007(13) 0.0054(12) 0.0012(13) C10 0.0134(16) 0.020(2) 0.0152(16) 0.0027(14) 0.0030(13) -0.0033(14) C11 0.026(2) 0.027(2) 0.033(2) -0.013(2) 0.0073(18) -0.0029(18) C12 0.0166(17) 0.023(2) 0.0266(19) 0.0043(17) 0.0053(15) -0.0022(16) C13 0.0093(16) 0.0117(19) 0.0095(15) -0.0032(13) 0.0004(12) -0.0010(13) C14 0.0129(13) 0.013(2) 0.0290(16) -0.0050(19) -0.0009(11) -0.0055(17) C15 0.0142(18) 0.0083(18) 0.0136(17) 0.0028(13) -0.0007(14) -0.0009(14) C16 0.0127(15) 0.0150(18) 0.0193(17) -0.0003(14) 0.0020(13) -0.0025(13) C17 0.044(3) 0.026(2) 0.032(2) -0.0080(19) 0.023(2) -0.019(2) C18 0.0223(19) 0.0167(19) 0.0186(17) -0.0031(14) 0.0052(14) -0.0027(15) C19 0.0124(15) 0.0094(16) 0.0123(14) -0.0023(12) 0.0018(12) -0.0025(12) C20 0.0175(17) 0.0120(17) 0.0181(16) 0.0005(13) 0.0027(13) 0.0041(14) C21 0.0138(16) 0.0179(19) 0.0165(16) -0.0013(14) 0.0003(13) -0.0026(14) C22 0.026(2) 0.023(2) 0.0209(19) -0.0005(16) 0.0019(16) 0.0037(17) C23 0.023(2) 0.027(2) 0.0213(19) -0.0048(17) 0.0003(15) -0.0014(17) C24 0.0194(14) 0.0304(18) 0.0171(13) 0.003(3) 0.0044(11) 0.000(3) C25 0.0130(16) 0.0149(18) 0.0234(18) 0.0009(15) 0.0025(14) 0.0014(14) C26 0.028(2) 0.021(2) 0.024(2) 0.0013(17) 0.0047(17) 0.0029(17) C27 0.0172(18) 0.019(2) 0.032(2) -0.0045(17) 0.0066(16) -0.0021(15) C28 0.0236(19) 0.019(2) 0.026(2) 0.0006(16) 0.0123(16) 0.0031(16) C29 0.0142(16) 0.0146(18) 0.0187(16) 0.0011(14) 0.0044(13) -0.0025(13) C30 0.028(2) 0.022(2) 0.035(2) 0.0065(19) 0.0033(18) 0.0016(18) C31 0.045(3) 0.014(2) 0.021(2) -0.0013(18) 0.000(2) -0.007(2) C32 0.030(2) 0.027(2) 0.027(2) 0.0069(18) 0.0077(18) -0.0083(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tm1 C25 2.393(4) . ? Tm1 C21 2.394(4) . ? Tm1 C29 2.395(4) . ? Tm1 N3 2.542(3) . ? Tm1 N1 2.557(3) . ? Tm1 N2 2.565(3) . ? Si1 C21 1.842(4) . ? Si1 C24 1.878(4) . ? Si1 C23 1.881(4) . ? Si1 C22 1.887(5) . ? Si2 C25 1.837(4) . ? Si2 C26 1.882(5) . ? Si2 C27 1.886(4) . ? Si2 C28 1.891(4) . ? Si3 C29 1.837(4) . ? Si3 C31 1.864(5) . ? Si3 C30 1.882(5) . ? Si3 C32 1.883(4) . ? O1 C1 1.340(5) . ? O1 C2 1.473(5) . ? O2 C7 1.338(4) . ? O2 C8 1.462(4) . ? O3 C13 1.335(4) . ? O3 C14 1.448(6) . ? N1 C1 1.262(5) . ? N1 C3 1.492(5) . ? N2 C7 1.268(5) . ? N2 C9 1.490(5) . ? N3 C13 1.274(6) . ? N3 C15 1.483(5) . ? C1 C19 1.529(5) . ? C2 C3 1.538(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.539(6) . ? C3 H3 1.0000 . ? C4 C5 1.514(6) . ? C4 C6 1.522(5) . ? C4 H4 1.0000 . ? 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 C19 1.529(5) . ? C8 C9 1.539(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.539(5) . ? C9 H9 1.0000 . ? C10 C12 1.527(5) . ? C10 C11 1.536(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C19 1.534(5) . ? C14 C15 1.539(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.543(5) . ? C15 H15 1.0000 . ? C16 C17 1.513(6) . ? C16 C18 1.533(5) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.530(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 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 C25 Tm1 C21 106.69(14) . . ? C25 Tm1 C29 106.64(14) . . ? C21 Tm1 C29 108.47(13) . . ? C25 Tm1 N3 90.22(12) . . ? C21 Tm1 N3 153.33(13) . . ? C29 Tm1 N3 85.29(12) . . ? C25 Tm1 N1 155.90(12) . . ? C21 Tm1 N1 84.63(12) . . ? C29 Tm1 N1 89.05(12) . . ? N3 Tm1 N1 72.58(11) . . ? C25 Tm1 N2 87.28(12) . . ? C21 Tm1 N2 88.25(12) . . ? C29 Tm1 N2 153.34(12) . . ? N3 Tm1 N2 71.75(11) . . ? N1 Tm1 N2 71.55(10) . . ? C21 Si1 C24 112.36(17) . . ? C21 Si1 C23 112.8(2) . . ? C24 Si1 C23 105.7(2) . . ? C21 Si1 C22 110.82(19) . . ? C24 Si1 C22 106.5(3) . . ? C23 Si1 C22 108.3(2) . . ? C25 Si2 C26 112.5(2) . . ? C25 Si2 C27 114.10(19) . . ? C26 Si2 C27 104.4(2) . . ? C25 Si2 C28 111.72(19) . . ? C26 Si2 C28 107.9(2) . . ? C27 Si2 C28 105.6(2) . . ? C29 Si3 C31 111.7(2) . . ? C29 Si3 C30 110.7(2) . . ? C31 Si3 C30 108.1(3) . . ? C29 Si3 C32 114.3(2) . . ? C31 Si3 C32 105.0(2) . . ? C30 Si3 C32 106.6(2) . . ? C1 O1 C2 105.0(3) . . ? C7 O2 C8 105.3(3) . . ? C13 O3 C14 105.3(3) . . ? C1 N1 C3 106.7(3) . . ? C1 N1 Tm1 122.7(2) . . ? C3 N1 Tm1 128.6(2) . . ? C7 N2 C9 106.4(3) . . ? C7 N2 Tm1 122.2(2) . . ? C9 N2 Tm1 130.1(2) . . ? C13 N3 C15 106.5(3) . . ? C13 N3 Tm1 122.3(3) . . ? C15 N3 Tm1 129.6(3) . . ? N1 C1 O1 119.7(3) . . ? N1 C1 C19 125.0(3) . . ? O1 C1 C19 115.3(3) . . ? O1 C2 C3 104.0(3) . . ? O1 C2 H2A 111.0 . . ? C3 C2 H2A 111.0 . . ? O1 C2 H2B 111.0 . . ? C3 C2 H2B 111.0 . . ? H2A C2 H2B 109.0 . . ? N1 C3 C2 103.0(3) . . ? N1 C3 C4 111.4(3) . . ? C2 C3 C4 114.9(3) . . ? N1 C3 H3 109.1 . . ? C2 C3 H3 109.1 . . ? C4 C3 H3 109.1 . . ? C5 C4 C6 112.0(3) . . ? C5 C4 C3 113.0(3) . . ? C6 C4 C3 110.1(3) . . ? C5 C4 H4 107.1 . . ? C6 C4 H4 107.1 . . ? C3 C4 H4 107.1 . . ? 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 . . ? N2 C7 O2 119.5(3) . . ? N2 C7 C19 125.2(3) . . ? O2 C7 C19 115.2(3) . . ? O2 C8 C9 104.0(3) . . ? O2 C8 H8A 111.0 . . ? C9 C8 H8A 111.0 . . ? O2 C8 H8B 111.0 . . ? C9 C8 H8B 111.0 . . ? H8A C8 H8B 109.0 . . ? N2 C9 C10 111.4(3) . . ? N2 C9 C8 103.1(3) . . ? C10 C9 C8 114.1(3) . . ? N2 C9 H9 109.3 . . ? C10 C9 H9 109.3 . . ? C8 C9 H9 109.3 . . ? C12 C10 C11 110.9(4) . . ? C12 C10 C9 109.9(3) . . ? C11 C10 C9 112.3(3) . . ? C12 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? C9 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 O3 119.4(4) . . ? N3 C13 C19 125.2(3) . . ? O3 C13 C19 115.4(3) . . ? O3 C14 C15 104.6(3) . . ? O3 C14 H14A 110.8 . . ? C15 C14 H14A 110.8 . . ? O3 C14 H14B 110.8 . . ? C15 C14 H14B 110.8 . . ? H14A C14 H14B 108.9 . . ? N3 C15 C14 102.9(3) . . ? N3 C15 C16 111.5(3) . . ? C14 C15 C16 114.2(3) . . ? N3 C15 H15 109.3 . . ? C14 C15 H15 109.3 . . ? C16 C15 H15 109.3 . . ? C17 C16 C18 111.1(3) . . ? C17 C16 C15 112.8(3) . . ? C18 C16 C15 110.0(3) . . ? C17 C16 H16 107.6 . . ? C18 C16 H16 107.6 . . ? C15 C16 H16 107.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C7 C19 C1 106.6(3) . . ? C7 C19 C20 111.9(3) . . ? C1 C19 C20 111.9(3) . . ? C7 C19 C13 107.2(3) . . ? C1 C19 C13 107.8(3) . . ? C20 C19 C13 111.2(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si1 C21 Tm1 129.4(2) . . ? Si1 C21 H21A 104.9 . . ? Tm1 C21 H21A 104.9 . . ? Si1 C21 H21B 104.9 . . ? Tm1 C21 H21B 104.9 . . ? H21A C21 H21B 105.8 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 Tm1 133.5(2) . . ? Si2 C25 H25A 103.8 . . ? Tm1 C25 H25A 103.8 . . ? Si2 C25 H25B 103.8 . . ? Tm1 C25 H25B 103.8 . . ? H25A C25 H25B 105.4 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si3 C29 Tm1 129.06(19) . . ? Si3 C29 H29A 105.0 . . ? Tm1 C29 H29A 105.0 . . ? Si3 C29 H29B 105.0 . . ? Tm1 C29 H29B 105.0 . . ? H29A C29 H29B 105.9 . . ? Si3 C30 H30A 109.5 . . ? Si3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C25 Tm1 N1 C1 -0.8(5) . . . . ? C21 Tm1 N1 C1 -120.5(3) . . . . ? C29 Tm1 N1 C1 130.8(3) . . . . ? N3 Tm1 N1 C1 45.4(3) . . . . ? N2 Tm1 N1 C1 -30.6(3) . . . . ? C25 Tm1 N1 C3 161.1(3) . . . . ? C21 Tm1 N1 C3 41.3(3) . . . . ? C29 Tm1 N1 C3 -67.3(3) . . . . ? N3 Tm1 N1 C3 -152.7(3) . . . . ? N2 Tm1 N1 C3 131.3(3) . . . . ? C25 Tm1 N2 C7 -122.5(3) . . . . ? C21 Tm1 N2 C7 130.7(3) . . . . ? C29 Tm1 N2 C7 0.5(5) . . . . ? N3 Tm1 N2 C7 -31.4(3) . . . . ? N1 Tm1 N2 C7 45.8(3) . . . . ? C25 Tm1 N2 C9 42.4(3) . . . . ? C21 Tm1 N2 C9 -64.4(3) . . . . ? C29 Tm1 N2 C9 165.4(3) . . . . ? N3 Tm1 N2 C9 133.5(3) . . . . ? N1 Tm1 N2 C9 -149.3(3) . . . . ? C25 Tm1 N3 C13 134.2(3) . . . . ? C21 Tm1 N3 C13 3.8(4) . . . . ? C29 Tm1 N3 C13 -119.1(3) . . . . ? N1 Tm1 N3 C13 -28.7(3) . . . . ? N2 Tm1 N3 C13 47.1(3) . . . . ? C25 Tm1 N3 C15 -62.4(3) . . . . ? C21 Tm1 N3 C15 167.2(3) . . . . ? C29 Tm1 N3 C15 44.2(3) . . . . ? N1 Tm1 N3 C15 134.7(3) . . . . ? N2 Tm1 N3 C15 -149.5(3) . . . . ? C3 N1 C1 O1 -2.9(5) . . . . ? Tm1 N1 C1 O1 162.4(3) . . . . ? C3 N1 C1 C19 178.8(3) . . . . ? Tm1 N1 C1 C19 -15.9(5) . . . . ? C2 O1 C1 N1 -5.4(5) . . . . ? C2 O1 C1 C19 173.1(3) . . . . ? C1 O1 C2 C3 10.7(4) . . . . ? C1 N1 C3 C2 9.4(4) . . . . ? Tm1 N1 C3 C2 -154.7(3) . . . . ? C1 N1 C3 C4 -114.2(4) . . . . ? Tm1 N1 C3 C4 81.6(4) . . . . ? O1 C2 C3 N1 -12.0(4) . . . . ? O1 C2 C3 C4 109.3(4) . . . . ? N1 C3 C4 C5 58.5(4) . . . . ? C2 C3 C4 C5 -58.1(4) . . . . ? N1 C3 C4 C6 -175.4(3) . . . . ? C2 C3 C4 C6 68.0(4) . . . . ? C9 N2 C7 O2 -4.6(5) . . . . ? Tm1 N2 C7 O2 163.4(2) . . . . ? C9 N2 C7 C19 177.2(3) . . . . ? Tm1 N2 C7 C19 -14.8(5) . . . . ? C8 O2 C7 N2 -4.3(5) . . . . ? C8 O2 C7 C19 174.1(3) . . . . ? C7 O2 C8 C9 10.6(4) . . . . ? C7 N2 C9 C10 -112.0(4) . . . . ? Tm1 N2 C9 C10 81.3(4) . . . . ? C7 N2 C9 C8 10.8(4) . . . . ? Tm1 N2 C9 C8 -155.9(3) . . . . ? O2 C8 C9 N2 -12.8(4) . . . . ? O2 C8 C9 C10 108.1(3) . . . . ? N2 C9 C10 C12 -177.1(3) . . . . ? C8 C9 C10 C12 66.7(4) . . . . ? N2 C9 C10 C11 59.0(4) . . . . ? C8 C9 C10 C11 -57.2(4) . . . . ? C15 N3 C13 O3 -2.5(4) . . . . ? Tm1 N3 C13 O3 164.2(2) . . . . ? C15 N3 C13 C19 176.2(4) . . . . ? Tm1 N3 C13 C19 -17.1(5) . . . . ? C14 O3 C13 N3 -5.2(4) . . . . ? C14 O3 C13 C19 176.0(3) . . . . ? C13 O3 C14 C15 10.0(4) . . . . ? C13 N3 C15 C14 8.5(3) . . . . ? Tm1 N3 C15 C14 -156.9(2) . . . . ? C13 N3 C15 C16 -114.3(4) . . . . ? Tm1 N3 C15 C16 80.3(4) . . . . ? O3 C14 C15 N3 -11.2(4) . . . . ? O3 C14 C15 C16 109.8(4) . . . . ? N3 C15 C16 C17 59.1(4) . . . . ? C14 C15 C16 C17 -57.0(5) . . . . ? N3 C15 C16 C18 -176.3(3) . . . . ? C14 C15 C16 C18 67.7(4) . . . . ? N2 C7 C19 C1 -48.7(5) . . . . ? O2 C7 C19 C1 133.0(3) . . . . ? N2 C7 C19 C20 -171.3(4) . . . . ? O2 C7 C19 C20 10.4(4) . . . . ? N2 C7 C19 C13 66.5(4) . . . . ? O2 C7 C19 C13 -111.7(3) . . . . ? N1 C1 C19 C7 68.2(4) . . . . ? O1 C1 C19 C7 -110.2(4) . . . . ? N1 C1 C19 C20 -169.2(4) . . . . ? O1 C1 C19 C20 12.4(4) . . . . ? N1 C1 C19 C13 -46.6(5) . . . . ? O1 C1 C19 C13 135.0(3) . . . . ? N3 C13 C19 C7 -46.8(5) . . . . ? O3 C13 C19 C7 131.9(3) . . . . ? N3 C13 C19 C1 67.6(4) . . . . ? O3 C13 C19 C1 -113.7(3) . . . . ? N3 C13 C19 C20 -169.4(3) . . . . ? O3 C13 C19 C20 9.3(4) . . . . ? C24 Si1 C21 Tm1 45.7(4) . . . . ? C23 Si1 C21 Tm1 165.1(2) . . . . ? C22 Si1 C21 Tm1 -73.3(3) . . . . ? C25 Tm1 C21 Si1 93.8(3) . . . . ? C29 Tm1 C21 Si1 -20.7(3) . . . . ? N3 Tm1 C21 Si1 -138.9(2) . . . . ? N1 Tm1 C21 Si1 -107.9(3) . . . . ? N2 Tm1 C21 Si1 -179.6(3) . . . . ? C26 Si2 C25 Tm1 -86.5(3) . . . . ? C27 Si2 C25 Tm1 32.2(4) . . . . ? C28 Si2 C25 Tm1 151.9(3) . . . . ? C21 Tm1 C25 Si2 -4.1(3) . . . . ? C29 Tm1 C25 Si2 111.7(3) . . . . ? N3 Tm1 C25 Si2 -163.2(3) . . . . ? N1 Tm1 C25 Si2 -119.6(3) . . . . ? N2 Tm1 C25 Si2 -91.5(3) . . . . ? C31 Si3 C29 Tm1 67.4(3) . . . . ? C30 Si3 C29 Tm1 -53.2(3) . . . . ? C32 Si3 C29 Tm1 -173.6(2) . . . . ? C25 Tm1 C29 Si3 -12.5(3) . . . . ? C21 Tm1 C29 Si3 102.0(3) . . . . ? N3 Tm1 C29 Si3 -101.4(3) . . . . ? N1 Tm1 C29 Si3 -174.0(2) . . . . ? N2 Tm1 C29 Si3 -131.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 32.03 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.841 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.136 _chemical_absolute_configuration ad #===end data_ga_ml3 _database_code_depnum_ccdc_archive 'CCDC 627377' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H72 N3 O3 Si3 Tm' _chemical_formula_weight 980.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_int_tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.1678(10) _cell_length_b 20.3453(18) _cell_length_c 22.558(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5125.6(8) _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 needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 1.840 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6563 _exptl_absorpt_correction_T_max 0.7099 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 104374 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 32.01 _reflns_number_total 17215 _reflns_number_gt 15962 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0252P)^2^+1.9422P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(4) _refine_ls_number_reflns 17215 _refine_ls_number_parameters 527 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0563 _refine_ls_wR_factor_gt 0.0537 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.003 _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 C1 C 0.3167(2) 0.01743(10) 0.24247(10) 0.0184(4) Uani 1 1 d . . . C2 C 0.4007(2) 0.04400(14) 0.15643(10) 0.0264(4) Uani 1 1 d . . . H2A H 0.4038 0.0915 0.1469 0.032 Uiso 1 1 calc R . . H2B H 0.4113 0.0185 0.1194 0.032 Uiso 1 1 calc R . . C3 C 0.4970(2) 0.02573(10) 0.20226(9) 0.0199(4) Uani 1 1 d . . . H3 H 0.5543 0.0632 0.2066 0.024 Uiso 1 1 calc R . . C4 C 0.5670(2) -0.03724(12) 0.18931(10) 0.0258(5) Uani 1 1 d . . . H4 H 0.6232 -0.0447 0.2232 0.031 Uiso 1 1 calc R . . C5 C 0.6430(3) -0.02783(14) 0.13329(13) 0.0388(6) Uani 1 1 d . . . H5A H 0.6903 -0.0676 0.1260 0.058 Uiso 1 1 calc R . . H5B H 0.6969 0.0097 0.1388 0.058 Uiso 1 1 calc R . . H5C H 0.5904 -0.0196 0.0993 0.058 Uiso 1 1 calc R . . C6 C 0.4874(3) -0.09796(12) 0.18413(13) 0.0379(6) Uani 1 1 d . . . H6A H 0.4438 -0.1045 0.2214 0.057 Uiso 1 1 calc R . . H6B H 0.5372 -0.1366 0.1760 0.057 Uiso 1 1 calc R . . H6C H 0.4302 -0.0918 0.1517 0.057 Uiso 1 1 calc R . . C7 C 0.19693(19) 0.06552(11) 0.32316(10) 0.0172(4) Uani 1 1 d . . . C8 C 0.0914(2) 0.13615(14) 0.37692(11) 0.0277(5) Uani 1 1 d . . . H8A H 0.0666 0.1209 0.4167 0.033 Uiso 1 1 calc R . . H8B H 0.0404 0.1737 0.3651 0.033 Uiso 1 1 calc R . . C9 C 0.2243(2) 0.15557(11) 0.37654(9) 0.0195(4) Uani 1 1 d . . . H9 H 0.2544 0.1590 0.4182 0.023 Uiso 1 1 calc R . . C10 C 0.2519(2) 0.21927(12) 0.34283(12) 0.0268(5) Uani 1 1 d . . . H10 H 0.3407 0.2254 0.3430 0.032 Uiso 1 1 calc R . . C11 C 0.2117(3) 0.21656(14) 0.27883(13) 0.0349(6) Uani 1 1 d . . . H11A H 0.1250 0.2092 0.2773 0.052 Uiso 1 1 calc R . . H11B H 0.2529 0.1805 0.2585 0.052 Uiso 1 1 calc R . . H11C H 0.2311 0.2582 0.2592 0.052 Uiso 1 1 calc R . . C12 C 0.1962(3) 0.27764(14) 0.37562(17) 0.0462(9) Uani 1 1 d . . . H12A H 0.2208 0.3187 0.3564 0.069 Uiso 1 1 calc R . . H12B H 0.2235 0.2776 0.4169 0.069 Uiso 1 1 calc R . . H12C H 0.1088 0.2740 0.3745 0.069 Uiso 1 1 calc R . . C13 C 0.25525(18) -0.04966(12) 0.32597(9) 0.0180(4) Uani 1 1 d . . . C14 C 0.2768(2) -0.15376(11) 0.35486(11) 0.0235(5) Uani 1 1 d . . . H14A H 0.3386 -0.1800 0.3340 0.028 Uiso 1 1 calc R . . H14B H 0.2201 -0.1840 0.3747 0.028 Uiso 1 1 calc R . . C15 C 0.3343(2) -0.10679(10) 0.39970(10) 0.0190(4) Uani 1 1 d . . . H15 H 0.4202 -0.1189 0.4057 0.023 Uiso 1 1 calc R . . C16 C 0.2706(2) -0.10272(11) 0.46000(10) 0.0206(4) Uani 1 1 d . . . H16 H 0.3117 -0.0680 0.4838 0.025 Uiso 1 1 calc R . . C17 C 0.1389(2) -0.08372(13) 0.45519(12) 0.0281(5) Uani 1 1 d . . . H17A H 0.1321 -0.0400 0.4372 0.042 Uiso 1 1 calc R . . H17B H 0.1030 -0.0830 0.4948 0.042 Uiso 1 1 calc R . . H17C H 0.0968 -0.1159 0.4305 0.042 Uiso 1 1 calc R . . C18 C 0.2853(3) -0.16797(13) 0.49309(13) 0.0314(6) Uani 1 1 d . . . H18A H 0.2556 -0.1632 0.5337 0.047 Uiso 1 1 calc R . . H18B H 0.3701 -0.1802 0.4940 0.047 Uiso 1 1 calc R . . H18C H 0.2395 -0.2023 0.4727 0.047 Uiso 1 1 calc R . . C19 C 0.2136(2) 0.00466(11) 0.28507(10) 0.0181(4) Uani 1 1 d . . . C20 C 0.0978(2) -0.01354(12) 0.25243(12) 0.0258(5) Uani 1 1 d . . . H20A H 0.1131 -0.0508 0.2259 0.039 Uiso 1 1 calc R . . H20B H 0.0702 0.0242 0.2292 0.039 Uiso 1 1 calc R . . H20C H 0.0362 -0.0257 0.2813 0.039 Uiso 1 1 calc R . . C21 C 0.4842(2) 0.06137(9) 0.46874(8) 0.0176(4) Uani 1 1 d . . . H21A H 0.4824 0.0155 0.4834 0.021 Uiso 1 1 calc R . . H21B H 0.5670 0.0766 0.4763 0.021 Uiso 1 1 calc R . . C22 C 0.2402(3) 0.07574(13) 0.52807(14) 0.0352(6) Uani 1 1 d . . . H22A H 0.2061 0.0775 0.4881 0.053 Uiso 1 1 calc R . . H22B H 0.1937 0.1041 0.5545 0.053 Uiso 1 1 calc R . . H22C H 0.2376 0.0304 0.5428 0.053 Uiso 1 1 calc R . . C23 C 0.4568(4) 0.09344(13) 0.60345(11) 0.0436(9) Uani 1 1 d . . . H23A H 0.4451 0.0477 0.6156 0.065 Uiso 1 1 calc R . . H23B H 0.4129 0.1225 0.6304 0.065 Uiso 1 1 calc R . . H23C H 0.5423 0.1042 0.6048 0.065 Uiso 1 1 calc R . . C24 C 0.4021(2) 0.19657(11) 0.51184(10) 0.0195(4) Uani 1 1 d . . . C25 C 0.4822(2) 0.22380(10) 0.47139(9) 0.0205(4) Uani 1 1 d . . . H25 H 0.5346 0.1955 0.4501 0.025 Uiso 1 1 calc R . . C26 C 0.4879(2) 0.29112(11) 0.46117(10) 0.0242(4) Uani 1 1 d . . . H26 H 0.5432 0.3082 0.4331 0.029 Uiso 1 1 calc R . . C27 C 0.4132(2) 0.33328(12) 0.49187(11) 0.0253(5) Uani 1 1 d . . . H27 H 0.4170 0.3793 0.4851 0.030 Uiso 1 1 calc R . . C28 C 0.3329(3) 0.30780(13) 0.53246(12) 0.0294(5) Uani 1 1 d . . . H28 H 0.2813 0.3365 0.5537 0.035 Uiso 1 1 calc R . . C29 C 0.3271(2) 0.24043(12) 0.54240(11) 0.0263(5) Uani 1 1 d . . . H29 H 0.2714 0.2237 0.5704 0.032 Uiso 1 1 calc R . . C30 C 0.62562(18) -0.04146(11) 0.35611(9) 0.0182(4) Uani 1 1 d . . . H30A H 0.5787 -0.0801 0.3430 0.022 Uiso 1 1 calc R . . H30B H 0.6781 -0.0297 0.3224 0.022 Uiso 1 1 calc R . . C31 C 0.8254(2) -0.00462(13) 0.44163(14) 0.0312(6) Uani 1 1 d . . . H31A H 0.8716 0.0137 0.4086 0.047 Uiso 1 1 calc R . . H31B H 0.8804 -0.0222 0.4716 0.047 Uiso 1 1 calc R . . H31C H 0.7761 0.0300 0.4594 0.047 Uiso 1 1 calc R . . C32 C 0.6471(3) -0.10960(14) 0.47938(12) 0.0299(6) Uani 1 1 d . . . H32A H 0.5923 -0.0771 0.4966 0.045 Uiso 1 1 calc R . . H32B H 0.7061 -0.1228 0.5092 0.045 Uiso 1 1 calc R . . H32C H 0.6014 -0.1482 0.4665 0.045 Uiso 1 1 calc R . . C33 C 0.83139(19) -0.13845(11) 0.38501(10) 0.0167(4) Uani 1 1 d . . . C34 C 0.8645(2) -0.19436(11) 0.41752(11) 0.0214(4) Uani 1 1 d . . . H34 H 0.8323 -0.2007 0.4561 0.026 Uiso 1 1 calc R . . C35 C 0.9437(2) -0.24067(12) 0.39452(12) 0.0267(5) Uani 1 1 d . . . H35 H 0.9645 -0.2781 0.4174 0.032 Uiso 1 1 calc R . . C36 C 0.9920(2) -0.23266(11) 0.33879(11) 0.0256(5) Uani 1 1 d . . . H36 H 1.0463 -0.2642 0.3233 0.031 Uiso 1 1 calc R . . C37 C 0.9603(2) -0.17788(12) 0.30539(11) 0.0234(5) Uani 1 1 d . . . H37 H 0.9932 -0.1719 0.2669 0.028 Uiso 1 1 calc R . . C38 C 0.8810(2) -0.13209(11) 0.32814(10) 0.0205(4) Uani 1 1 d . . . H38 H 0.8594 -0.0953 0.3045 0.025 Uiso 1 1 calc R . . C39 C 0.5956(2) 0.14120(11) 0.33323(9) 0.0177(4) Uani 1 1 d . . . H39A H 0.5331 0.1757 0.3329 0.021 Uiso 1 1 calc R . . H39B H 0.6441 0.1506 0.3690 0.021 Uiso 1 1 calc R . . C40 C 0.7785(2) 0.24664(13) 0.29140(11) 0.0268(5) Uani 1 1 d . . . H40A H 0.7214 0.2807 0.3036 0.040 Uiso 1 1 calc R . . H40B H 0.8221 0.2614 0.2561 0.040 Uiso 1 1 calc R . . H40C H 0.8353 0.2384 0.3237 0.040 Uiso 1 1 calc R . . C41 C 0.8099(2) 0.10466(13) 0.25514(12) 0.0281(5) Uani 1 1 d . . . H41A H 0.8560 0.0937 0.2908 0.042 Uiso 1 1 calc R . . H41B H 0.8640 0.1218 0.2246 0.042 Uiso 1 1 calc R . . H41C H 0.7699 0.0651 0.2403 0.042 Uiso 1 1 calc R . . C42 C 0.6076(2) 0.18844(11) 0.20404(10) 0.0187(4) Uani 1 1 d . . . C43 C 0.5006(2) 0.22398(11) 0.20734(10) 0.0254(5) Uani 1 1 d . . . H43 H 0.4708 0.2364 0.2452 0.030 Uiso 1 1 calc R . . C44 C 0.4363(3) 0.24170(14) 0.15684(13) 0.0331(6) Uani 1 1 d . . . H44 H 0.3642 0.2661 0.1604 0.040 Uiso 1 1 calc R . . C45 C 0.4783(3) 0.22351(14) 0.10145(12) 0.0373(6) Uani 1 1 d . . . H45 H 0.4349 0.2354 0.0669 0.045 Uiso 1 1 calc R . . C46 C 0.5833(3) 0.18815(14) 0.09648(12) 0.0343(6) Uani 1 1 d . . . H46 H 0.6117 0.1753 0.0585 0.041 Uiso 1 1 calc R . . C47 C 0.6475(2) 0.17143(12) 0.14700(10) 0.0267(5) Uani 1 1 d . . . H47 H 0.7204 0.1478 0.1429 0.032 Uiso 1 1 calc R . . N1 N 0.42580(18) 0.01914(9) 0.25777(8) 0.0176(4) Uani 1 1 d . . . N2 N 0.28158(17) 0.09854(9) 0.34636(8) 0.0166(3) Uani 1 1 d . . . N3 N 0.32644(15) -0.04197(9) 0.36920(9) 0.0178(3) Uani 1 1 d . . . O1 O 0.28721(17) 0.02706(8) 0.18543(7) 0.0252(4) Uani 1 1 d . . . O2 O 0.08338(15) 0.08295(9) 0.33371(8) 0.0230(3) Uani 1 1 d . . . O3 O 0.21393(16) -0.11000(8) 0.31345(8) 0.0236(3) Uani 1 1 d . . . Si1 Si 0.39971(6) 0.10483(3) 0.52590(3) 0.01880(12) Uani 1 1 d . . . Si2 Si 0.72642(5) -0.07234(3) 0.41370(3) 0.01668(11) Uani 1 1 d . . . Si3 Si 0.69497(6) 0.16845(3) 0.27375(3) 0.01667(11) Uani 1 1 d . . . Tm1 Tm 0.483991(7) 0.046395(4) 0.363715(4) 0.01265(2) Uani 1 1 d . . . 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 C1 0.0268(11) 0.0108(9) 0.0176(9) -0.0018(7) -0.0045(8) 0.0001(8) C2 0.0336(12) 0.0259(11) 0.0196(9) 0.0025(10) -0.0028(8) 0.0008(12) C3 0.0274(13) 0.0167(8) 0.0158(8) -0.0026(7) 0.0018(8) -0.0014(8) C4 0.0364(13) 0.0206(12) 0.0205(10) -0.0030(8) 0.0033(9) 0.0043(10) C5 0.0529(17) 0.0355(14) 0.0281(12) -0.0069(12) 0.0157(14) 0.0083(12) C6 0.0560(19) 0.0191(11) 0.0386(13) -0.0072(10) 0.0061(14) 0.0020(13) C7 0.0149(9) 0.0173(9) 0.0192(9) 0.0042(7) -0.0034(7) 0.0007(7) C8 0.0190(10) 0.0340(13) 0.0300(13) -0.0086(10) 0.0023(8) 0.0021(10) C9 0.0159(9) 0.0226(10) 0.0202(10) -0.0053(8) -0.0022(7) 0.0039(8) C10 0.0218(12) 0.0178(11) 0.0406(14) -0.0048(9) -0.0038(10) 0.0040(9) C11 0.0362(15) 0.0273(13) 0.0413(16) 0.0137(12) -0.0070(12) -0.0004(11) C12 0.0315(14) 0.0250(13) 0.082(3) -0.0190(15) -0.0073(15) 0.0092(11) C13 0.0147(9) 0.0153(9) 0.0239(9) 0.0002(9) 0.0002(7) -0.0021(9) C14 0.0263(11) 0.0140(9) 0.0302(13) 0.0009(8) -0.0035(9) 0.0016(8) C15 0.0172(10) 0.0128(9) 0.0269(11) 0.0045(8) -0.0025(8) -0.0003(7) C16 0.0202(11) 0.0168(10) 0.0247(11) 0.0039(8) -0.0002(8) -0.0021(8) C17 0.0204(11) 0.0298(13) 0.0343(13) 0.0003(10) 0.0050(10) 0.0013(10) C18 0.0303(13) 0.0274(13) 0.0364(14) 0.0129(11) 0.0061(11) 0.0003(11) C19 0.0160(10) 0.0160(9) 0.0222(10) 0.0004(8) -0.0054(8) -0.0015(8) C20 0.0213(11) 0.0234(11) 0.0328(13) -0.0006(10) -0.0131(10) -0.0036(9) C21 0.0180(9) 0.0165(9) 0.0184(8) 0.0016(6) 0.0016(8) -0.0002(8) C22 0.0328(15) 0.0206(12) 0.0522(17) -0.0027(11) 0.0204(13) -0.0037(11) C23 0.089(3) 0.0256(12) 0.0167(10) 0.0043(9) -0.0050(13) -0.0082(15) C24 0.0246(11) 0.0182(10) 0.0158(9) -0.0022(8) 0.0013(8) -0.0031(8) C25 0.0250(10) 0.0176(9) 0.0190(9) -0.0014(7) 0.0052(9) -0.0013(9) C26 0.0300(12) 0.0183(9) 0.0241(10) 0.0021(8) 0.0042(9) -0.0031(9) C27 0.0323(13) 0.0155(10) 0.0280(12) -0.0028(9) -0.0013(10) -0.0019(9) C28 0.0325(14) 0.0203(11) 0.0353(13) -0.0106(10) 0.0080(11) -0.0011(10) C29 0.0312(13) 0.0215(11) 0.0263(12) -0.0049(9) 0.0111(10) -0.0055(10) C30 0.0178(9) 0.0176(9) 0.0193(10) 0.0004(9) -0.0001(7) 0.0019(8) C31 0.0233(12) 0.0227(12) 0.0477(16) -0.0103(11) -0.0100(11) 0.0018(10) C32 0.0300(13) 0.0317(13) 0.0280(12) 0.0089(10) 0.0046(10) 0.0129(11) C33 0.0144(9) 0.0139(9) 0.0217(9) -0.0010(8) -0.0043(7) 0.0007(8) C34 0.0221(11) 0.0171(10) 0.0252(11) 0.0001(8) -0.0015(9) 0.0034(8) C35 0.0289(12) 0.0173(10) 0.0338(13) 0.0006(9) -0.0026(10) 0.0060(9) C36 0.0230(12) 0.0184(9) 0.0354(11) -0.0049(8) 0.0039(10) 0.0015(9) C37 0.0207(12) 0.0234(11) 0.0260(11) -0.0030(9) 0.0035(8) -0.0014(9) C38 0.0178(10) 0.0180(10) 0.0256(11) 0.0015(8) 0.0012(8) 0.0000(8) C39 0.0176(10) 0.0182(10) 0.0174(9) 0.0022(8) -0.0007(7) -0.0045(8) C40 0.0289(13) 0.0278(12) 0.0237(11) 0.0013(9) 0.0003(9) -0.0125(10) C41 0.0194(11) 0.0331(13) 0.0318(13) 0.0005(10) 0.0005(9) 0.0057(10) C42 0.0225(11) 0.0162(9) 0.0175(9) 0.0011(8) -0.0004(8) -0.0043(8) C43 0.0266(14) 0.0246(10) 0.0248(10) 0.0027(8) -0.0030(9) 0.0021(9) C44 0.0308(14) 0.0318(14) 0.0367(14) 0.0111(11) -0.0117(11) 0.0012(11) C45 0.0455(16) 0.0374(14) 0.0291(12) 0.0134(10) -0.0172(12) -0.0171(14) C46 0.0495(18) 0.0363(14) 0.0171(11) 0.0045(10) -0.0008(11) -0.0134(13) C47 0.0337(13) 0.0252(11) 0.0211(12) 0.0020(9) 0.0028(9) -0.0038(10) N1 0.0229(10) 0.0145(8) 0.0155(8) -0.0019(6) -0.0011(7) -0.0007(7) N2 0.0167(9) 0.0136(8) 0.0195(8) -0.0017(6) -0.0032(6) 0.0016(7) N3 0.0164(7) 0.0135(7) 0.0233(9) 0.0055(8) -0.0023(7) -0.0022(7) O1 0.0314(9) 0.0255(8) 0.0186(7) 0.0029(6) -0.0078(7) -0.0025(7) O2 0.0148(8) 0.0251(8) 0.0291(9) -0.0028(7) -0.0010(6) 0.0010(6) O3 0.0271(9) 0.0141(7) 0.0297(9) -0.0001(6) -0.0065(7) -0.0029(6) Si1 0.0268(3) 0.0153(3) 0.0144(3) -0.0002(2) 0.0042(2) -0.0037(2) Si2 0.0150(3) 0.0152(3) 0.0198(3) -0.0002(2) -0.0013(2) 0.0025(2) Si3 0.0156(3) 0.0177(3) 0.0168(3) 0.0019(2) 0.0012(2) -0.0021(2) Tm1 0.01202(3) 0.01186(3) 0.01409(3) 0.00101(3) -0.00091(3) -0.00032(3) _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 C1 N1 1.267(3) . ? C1 O1 1.343(3) . ? C1 C19 1.522(3) . ? C2 O1 1.467(3) . ? C2 C3 1.537(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.489(3) . ? C3 C4 1.530(3) . ? C3 H3 1.0000 . ? C4 C6 1.527(4) . ? C4 C5 1.534(4) . ? C4 H4 1.0000 . ? 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 N2 1.272(3) . ? C7 O2 1.338(3) . ? C7 C19 1.519(3) . ? C8 O2 1.459(3) . ? C8 C9 1.535(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N2 1.490(3) . ? C9 C10 1.534(3) . ? C9 H9 1.0000 . ? C10 C11 1.513(4) . ? C10 C12 1.531(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N3 1.268(3) . ? C13 O3 1.342(3) . ? C13 C19 1.513(3) . ? C14 O3 1.469(3) . ? C14 C15 1.532(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N3 1.490(3) . ? C15 C16 1.537(3) . ? C15 H15 1.0000 . ? C16 C17 1.525(3) . ? C16 C18 1.532(3) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.533(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 Si1 1.826(2) . ? C21 Tm1 2.3888(19) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 Si1 1.878(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 Si1 1.876(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.393(3) . ? C24 C29 1.404(3) . ? C24 Si1 1.893(2) . ? C25 C26 1.390(3) . ? C25 H25 0.9500 . ? C26 C27 1.383(3) . ? C26 H26 0.9500 . ? C27 C28 1.383(4) . ? C27 H27 0.9500 . ? C28 C29 1.390(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 Si2 1.830(2) . ? C30 Tm1 2.393(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 Si2 1.876(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 Si2 1.886(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.403(3) . ? C33 C38 1.403(3) . ? C33 Si2 1.898(2) . ? C34 C35 1.392(3) . ? C34 H34 0.9500 . ? C35 C36 1.378(4) . ? C35 H35 0.9500 . ? C36 C37 1.391(3) . ? C36 H36 0.9500 . ? C37 C38 1.385(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 Si3 1.827(2) . ? C39 Tm1 2.397(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 Si3 1.886(2) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 Si3 1.873(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.399(3) . ? C42 C47 1.405(3) . ? C42 Si3 1.895(2) . ? C43 C44 1.394(3) . ? C43 H43 0.9500 . ? C44 C45 1.385(4) . ? C44 H44 0.9500 . ? C45 C46 1.380(5) . ? C45 H45 0.9500 . ? C46 C47 1.389(4) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? N1 Tm1 2.5380(18) . ? N2 Tm1 2.5276(18) . ? N3 Tm1 2.5187(17) . ? 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 C1 O1 119.5(2) . . ? N1 C1 C19 124.1(2) . . ? O1 C1 C19 116.4(2) . . ? O1 C2 C3 104.33(17) . . ? O1 C2 H2A 110.9 . . ? C3 C2 H2A 110.9 . . ? O1 C2 H2B 110.9 . . ? C3 C2 H2B 110.9 . . ? H2A C2 H2B 108.9 . . ? N1 C3 C4 110.99(17) . . ? N1 C3 C2 102.36(18) . . ? C4 C3 C2 115.59(19) . . ? N1 C3 H3 109.2 . . ? C4 C3 H3 109.2 . . ? C2 C3 H3 109.2 . . ? C6 C4 C3 113.2(2) . . ? C6 C4 C5 111.1(2) . . ? C3 C4 C5 109.6(2) . . ? C6 C4 H4 107.5 . . ? C3 C4 H4 107.5 . . ? C5 C4 H4 107.5 . . ? 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 . . ? N2 C7 O2 119.4(2) . . ? N2 C7 C19 124.9(2) . . ? O2 C7 C19 115.64(19) . . ? O2 C8 C9 104.29(18) . . ? O2 C8 H8A 110.9 . . ? C9 C8 H8A 110.9 . . ? O2 C8 H8B 110.9 . . ? C9 C8 H8B 110.9 . . ? H8A C8 H8B 108.9 . . ? N2 C9 C10 110.17(18) . . ? N2 C9 C8 102.55(18) . . ? C10 C9 C8 114.5(2) . . ? N2 C9 H9 109.8 . . ? C10 C9 H9 109.8 . . ? C8 C9 H9 109.8 . . ? C11 C10 C12 111.6(2) . . ? C11 C10 C9 112.5(2) . . ? C12 C10 C9 109.5(2) . . ? C11 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? C9 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 O3 119.4(2) . . ? N3 C13 C19 124.9(2) . . ? O3 C13 C19 115.74(18) . . ? O3 C14 C15 104.00(17) . . ? O3 C14 H14A 111.0 . . ? C15 C14 H14A 111.0 . . ? O3 C14 H14B 111.0 . . ? C15 C14 H14B 111.0 . . ? H14A C14 H14B 109.0 . . ? N3 C15 C14 102.86(17) . . ? N3 C15 C16 109.51(18) . . ? C14 C15 C16 115.12(19) . . ? N3 C15 H15 109.7 . . ? C14 C15 H15 109.7 . . ? C16 C15 H15 109.7 . . ? C17 C16 C18 110.9(2) . . ? C17 C16 C15 113.4(2) . . ? C18 C16 C15 109.6(2) . . ? C17 C16 H16 107.6 . . ? C18 C16 H16 107.6 . . ? C15 C16 H16 107.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C19 C7 106.75(18) . . ? C13 C19 C1 106.08(18) . . ? C7 C19 C1 108.11(18) . . ? C13 C19 C20 112.08(19) . . ? C7 C19 C20 111.44(19) . . ? C1 C19 C20 112.06(19) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si1 C21 Tm1 139.62(11) . . ? Si1 C21 H21A 102.2 . . ? Tm1 C21 H21A 102.2 . . ? Si1 C21 H21B 102.2 . . ? Tm1 C21 H21B 102.2 . . ? H21A C21 H21B 104.8 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 116.9(2) . . ? C25 C24 Si1 120.70(17) . . ? C29 C24 Si1 122.40(18) . . ? C26 C25 C24 122.0(2) . . ? C26 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? C27 C26 C25 120.0(2) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 119.4(2) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C27 C28 C29 120.4(2) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C24 121.3(2) . . ? C28 C29 H29 119.3 . . ? C24 C29 H29 119.3 . . ? Si2 C30 Tm1 127.74(11) . . ? Si2 C30 H30A 105.4 . . ? Tm1 C30 H30A 105.4 . . ? Si2 C30 H30B 105.4 . . ? Tm1 C30 H30B 105.4 . . ? H30A C30 H30B 106.0 . . ? Si2 C31 H31A 109.5 . . ? Si2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si2 C32 H32A 109.5 . . ? Si2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C38 116.7(2) . . ? C34 C33 Si2 124.00(17) . . ? C38 C33 Si2 119.34(16) . . ? C35 C34 C33 121.4(2) . . ? C35 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? C36 C35 C34 120.6(2) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 119.3(2) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C38 C37 C36 120.1(2) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C33 122.0(2) . . ? C37 C38 H38 119.0 . . ? C33 C38 H38 119.0 . . ? Si3 C39 Tm1 140.40(12) . . ? Si3 C39 H39A 101.9 . . ? Tm1 C39 H39A 101.9 . . ? Si3 C39 H39B 101.9 . . ? Tm1 C39 H39B 101.9 . . ? H39A C39 H39B 104.7 . . ? Si3 C40 H40A 109.5 . . ? Si3 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si3 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si3 C41 H41A 109.5 . . ? Si3 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si3 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C47 116.5(2) . . ? C43 C42 Si3 120.44(17) . . ? C47 C42 Si3 122.97(19) . . ? C44 C43 C42 122.0(2) . . ? C44 C43 H43 119.0 . . ? C42 C43 H43 119.0 . . ? C45 C44 C43 119.6(3) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C46 C45 C44 120.0(2) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.0(3) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C42 121.9(3) . . ? C46 C47 H47 119.1 . . ? C42 C47 H47 119.1 . . ? C1 N1 C3 106.66(18) . . ? C1 N1 Tm1 120.59(15) . . ? C3 N1 Tm1 129.46(14) . . ? C7 N2 C9 106.25(18) . . ? C7 N2 Tm1 120.43(14) . . ? C9 N2 Tm1 129.82(13) . . ? C13 N3 C15 106.42(19) . . ? C13 N3 Tm1 119.23(15) . . ? C15 N3 Tm1 127.85(13) . . ? C1 O1 C2 104.48(18) . . ? C7 O2 C8 104.88(17) . . ? C13 O3 C14 104.85(17) . . ? C21 Si1 C23 115.02(14) . . ? C21 Si1 C22 110.84(12) . . ? C23 Si1 C22 105.02(16) . . ? C21 Si1 C24 110.61(10) . . ? C23 Si1 C24 105.86(11) . . ? C22 Si1 C24 109.17(12) . . ? C30 Si2 C31 110.42(12) . . ? C30 Si2 C32 114.00(11) . . ? C31 Si2 C32 107.97(14) . . ? C30 Si2 C33 112.40(10) . . ? C31 Si2 C33 105.72(11) . . ? C32 Si2 C33 105.86(11) . . ? C39 Si3 C41 111.75(12) . . ? C39 Si3 C40 113.65(11) . . ? C41 Si3 C40 107.02(13) . . ? C39 Si3 C42 111.21(10) . . ? C41 Si3 C42 108.40(11) . . ? C40 Si3 C42 104.40(11) . . ? C21 Tm1 C30 99.55(7) . . ? C21 Tm1 C39 100.46(7) . . ? C30 Tm1 C39 103.70(8) . . ? C21 Tm1 N3 92.46(7) . . ? C30 Tm1 N3 86.10(7) . . ? C39 Tm1 N3 162.11(6) . . ? C21 Tm1 N2 95.78(7) . . ? C30 Tm1 N2 153.33(7) . . ? C39 Tm1 N2 94.75(7) . . ? N3 Tm1 N2 71.49(6) . . ? C21 Tm1 N1 164.16(7) . . ? C30 Tm1 N1 86.48(7) . . ? C39 Tm1 N1 92.22(7) . . ? N3 Tm1 N1 73.23(6) . . ? N2 Tm1 N1 73.55(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C2 C3 N1 -15.9(2) . . . . ? O1 C2 C3 C4 104.8(2) . . . . ? N1 C3 C4 C6 57.5(3) . . . . ? C2 C3 C4 C6 -58.4(3) . . . . ? N1 C3 C4 C5 -177.8(2) . . . . ? C2 C3 C4 C5 66.2(3) . . . . ? O2 C8 C9 N2 -15.9(2) . . . . ? O2 C8 C9 C10 103.5(2) . . . . ? N2 C9 C10 C11 57.3(3) . . . . ? C8 C9 C10 C11 -57.7(3) . . . . ? N2 C9 C10 C12 -178.0(2) . . . . ? C8 C9 C10 C12 67.1(3) . . . . ? O3 C14 C15 N3 -15.5(2) . . . . ? O3 C14 C15 C16 103.6(2) . . . . ? N3 C15 C16 C17 59.0(2) . . . . ? C14 C15 C16 C17 -56.3(3) . . . . ? N3 C15 C16 C18 -176.50(19) . . . . ? C14 C15 C16 C18 68.2(3) . . . . ? N3 C13 C19 C7 -37.4(3) . . . . ? O3 C13 C19 C7 144.01(19) . . . . ? N3 C13 C19 C1 77.7(3) . . . . ? O3 C13 C19 C1 -100.9(2) . . . . ? N3 C13 C19 C20 -159.7(2) . . . . ? O3 C13 C19 C20 21.7(3) . . . . ? N2 C7 C19 C13 70.8(3) . . . . ? O2 C7 C19 C13 -107.0(2) . . . . ? N2 C7 C19 C1 -43.0(3) . . . . ? O2 C7 C19 C1 139.28(19) . . . . ? N2 C7 C19 C20 -166.6(2) . . . . ? O2 C7 C19 C20 15.7(3) . . . . ? N1 C1 C19 C13 -41.4(3) . . . . ? O1 C1 C19 C13 138.37(19) . . . . ? N1 C1 C19 C7 72.8(3) . . . . ? O1 C1 C19 C7 -107.4(2) . . . . ? N1 C1 C19 C20 -164.0(2) . . . . ? O1 C1 C19 C20 15.8(3) . . . . ? C29 C24 C25 C26 -0.4(4) . . . . ? Si1 C24 C25 C26 -178.47(19) . . . . ? C24 C25 C26 C27 0.5(4) . . . . ? C25 C26 C27 C28 -0.3(4) . . . . ? C26 C27 C28 C29 0.0(4) . . . . ? C27 C28 C29 C24 0.0(4) . . . . ? C25 C24 C29 C28 0.1(4) . . . . ? Si1 C24 C29 C28 178.2(2) . . . . ? C38 C33 C34 C35 0.7(3) . . . . ? Si2 C33 C34 C35 -178.85(19) . . . . ? C33 C34 C35 C36 0.1(4) . . . . ? C34 C35 C36 C37 -0.4(4) . . . . ? C35 C36 C37 C38 -0.1(4) . . . . ? C36 C37 C38 C33 0.9(4) . . . . ? C34 C33 C38 C37 -1.1(3) . . . . ? Si2 C33 C38 C37 178.38(18) . . . . ? C47 C42 C43 C44 0.0(3) . . . . ? Si3 C42 C43 C44 177.5(2) . . . . ? C42 C43 C44 C45 0.4(4) . . . . ? C43 C44 C45 C46 -0.1(4) . . . . ? C44 C45 C46 C47 -0.7(4) . . . . ? C45 C46 C47 C42 1.2(4) . . . . ? C43 C42 C47 C46 -0.9(3) . . . . ? Si3 C42 C47 C46 -178.3(2) . . . . ? O1 C1 N1 C3 -5.6(3) . . . . ? C19 C1 N1 C3 174.12(19) . . . . ? O1 C1 N1 Tm1 155.68(15) . . . . ? C19 C1 N1 Tm1 -24.5(3) . . . . ? C4 C3 N1 C1 -110.6(2) . . . . ? C2 C3 N1 C1 13.3(2) . . . . ? C4 C3 N1 Tm1 90.3(2) . . . . ? C2 C3 N1 Tm1 -145.77(16) . . . . ? O2 C7 N2 C9 -5.6(3) . . . . ? C19 C7 N2 C9 176.8(2) . . . . ? O2 C7 N2 Tm1 155.33(15) . . . . ? C19 C7 N2 Tm1 -22.3(3) . . . . ? C10 C9 N2 C7 -109.1(2) . . . . ? C8 C9 N2 C7 13.2(2) . . . . ? C10 C9 N2 Tm1 92.4(2) . . . . ? C8 C9 N2 Tm1 -145.27(16) . . . . ? O3 C13 N3 C15 -6.1(3) . . . . ? C19 C13 N3 C15 175.4(2) . . . . ? O3 C13 N3 Tm1 147.83(16) . . . . ? C19 C13 N3 Tm1 -30.7(3) . . . . ? C14 C15 N3 C13 13.3(2) . . . . ? C16 C15 N3 C13 -109.6(2) . . . . ? C14 C15 N3 Tm1 -137.61(16) . . . . ? C16 C15 N3 Tm1 99.51(19) . . . . ? N1 C1 O1 C2 -5.3(3) . . . . ? C19 C1 O1 C2 174.90(19) . . . . ? C3 C2 O1 C1 13.2(2) . . . . ? N2 C7 O2 C8 -5.3(3) . . . . ? C19 C7 O2 C8 172.57(19) . . . . ? C9 C8 O2 C7 13.2(2) . . . . ? N3 C13 O3 C14 -4.5(3) . . . . ? C19 C13 O3 C14 174.10(19) . . . . ? C15 C14 O3 C13 12.5(2) . . . . ? Tm1 C21 Si1 C23 -179.27(16) . . . . ? Tm1 C21 Si1 C22 61.8(2) . . . . ? Tm1 C21 Si1 C24 -59.42(19) . . . . ? C25 C24 Si1 C21 -13.8(2) . . . . ? C29 C24 Si1 C21 168.2(2) . . . . ? C25 C24 Si1 C23 111.4(2) . . . . ? C29 C24 Si1 C23 -66.6(3) . . . . ? C25 C24 Si1 C22 -136.0(2) . . . . ? C29 C24 Si1 C22 46.0(2) . . . . ? Tm1 C30 Si2 C31 -57.64(17) . . . . ? Tm1 C30 Si2 C32 64.10(17) . . . . ? Tm1 C30 Si2 C33 -175.43(12) . . . . ? C34 C33 Si2 C30 -141.33(19) . . . . ? C38 C33 Si2 C30 39.2(2) . . . . ? C34 C33 Si2 C31 98.1(2) . . . . ? C38 C33 Si2 C31 -81.4(2) . . . . ? C34 C33 Si2 C32 -16.3(2) . . . . ? C38 C33 Si2 C32 164.23(18) . . . . ? Tm1 C39 Si3 C41 -44.5(2) . . . . ? Tm1 C39 Si3 C40 -165.72(17) . . . . ? Tm1 C39 Si3 C42 76.8(2) . . . . ? C43 C42 Si3 C39 43.3(2) . . . . ? C47 C42 Si3 C39 -139.34(19) . . . . ? C43 C42 Si3 C41 166.56(19) . . . . ? C47 C42 Si3 C41 -16.1(2) . . . . ? C43 C42 Si3 C40 -79.6(2) . . . . ? C47 C42 Si3 C40 97.7(2) . . . . ? Si1 C21 Tm1 C30 -169.14(16) . . . . ? Si1 C21 Tm1 C39 84.89(17) . . . . ? Si1 C21 Tm1 N3 -82.68(17) . . . . ? Si1 C21 Tm1 N2 -11.04(17) . . . . ? Si1 C21 Tm1 N1 -57.8(3) . . . . ? Si2 C30 Tm1 C21 -12.20(15) . . . . ? Si2 C30 Tm1 C39 91.13(14) . . . . ? Si2 C30 Tm1 N3 -104.04(14) . . . . ? Si2 C30 Tm1 N2 -136.42(13) . . . . ? Si2 C30 Tm1 N1 -177.44(14) . . . . ? Si3 C39 Tm1 C21 151.17(18) . . . . ? Si3 C39 Tm1 C30 48.5(2) . . . . ? Si3 C39 Tm1 N3 -73.3(3) . . . . ? Si3 C39 Tm1 N2 -112.04(18) . . . . ? Si3 C39 Tm1 N1 -38.36(19) . . . . ? C13 N3 Tm1 C21 150.41(17) . . . . ? C15 N3 Tm1 C21 -61.91(18) . . . . ? C13 N3 Tm1 C30 -110.18(18) . . . . ? C15 N3 Tm1 C30 37.50(17) . . . . ? C13 N3 Tm1 C39 14.0(3) . . . . ? C15 N3 Tm1 C39 161.7(2) . . . . ? C13 N3 Tm1 N2 55.13(17) . . . . ? C15 N3 Tm1 N2 -157.19(19) . . . . ? C13 N3 Tm1 N1 -22.69(17) . . . . ? C15 N3 Tm1 N1 124.99(18) . . . . ? C7 N2 Tm1 C21 -119.69(17) . . . . ? C9 N2 Tm1 C21 36.18(18) . . . . ? C7 N2 Tm1 C30 5.3(3) . . . . ? C9 N2 Tm1 C30 161.14(17) . . . . ? C7 N2 Tm1 C39 139.28(17) . . . . ? C9 N2 Tm1 C39 -64.86(18) . . . . ? C7 N2 Tm1 N3 -29.02(16) . . . . ? C9 N2 Tm1 N3 126.84(19) . . . . ? C7 N2 Tm1 N1 48.36(17) . . . . ? C9 N2 Tm1 N1 -155.78(19) . . . . ? C1 N1 Tm1 C21 23.8(3) . . . . ? C3 N1 Tm1 C21 -179.6(2) . . . . ? C1 N1 Tm1 C30 136.85(18) . . . . ? C3 N1 Tm1 C30 -66.55(17) . . . . ? C1 N1 Tm1 C39 -119.55(18) . . . . ? C3 N1 Tm1 C39 37.04(17) . . . . ? C1 N1 Tm1 N3 49.86(17) . . . . ? C3 N1 Tm1 N3 -153.54(18) . . . . ? C1 N1 Tm1 N2 -25.26(17) . . . . ? C3 N1 Tm1 N2 131.34(18) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 32.01 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.418 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.090 _chemical_absolute_configuration ad