# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Reiner Anwander' _publ_contact_author_email REINER.ANWANDER@UNI-TUEBINGEN.DE _publ_section_title ; Amido-Stabilized Rare-Earth Metal Mixed Methyl Methylidene Complexes ; loop_ _publ_author_name 'Reiner Anwander' 'Klaus Eichele' 'Dorothea Rauschmaier' 'Karl W Tornroos' 'Melanie Zimmermann' # Attachment 'Compound4a.cif' # Compound 4a #=================================================================== data_zm79r _database_code_depnum_ccdc_archive 'CCDC 765379' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H116 N3 O3 Si3 Y3, C6 H14' _chemical_formula_sum 'C68 H130 N3 O3 Si3 Y3' _chemical_formula_weight 1388.75 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' Y Y -2.7962 3.5667 '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/n' _symmetry_space_group_name_HALL '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.4354(4) _cell_length_b 25.9885(8) _cell_length_c 26.3748(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.957(1) _cell_angle_gamma 90.00 _cell_volume 7762.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16044 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.04 _exptl_crystal_description 'thin prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 2.311 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3630 _exptl_absorpt_correction_T_max 0.8932 _exptl_absorpt_process_details ; SADABS version 2008/1, G.M Sheldrick, University of G\"ttingen, Germany, 2008. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'TXS Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 88796 _diffrn_reflns_av_R_equivalents 0.0907 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.07 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 13744 _reflns_number_gt 9165 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Bruker (1999). SMART, version 5.054, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_cell_refinement ; Bruker (2008). SAINT, version 6.45A, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_data_reduction ; Bruker (2004). SAINT, version 6.45a, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_structure_solution ; Sheldrick, G. M. (2008). Acta Crystallographica, A64, 112-122. ; _computing_structure_refinement ; Sheldrick, G. M. (2008). Acta Crystallographica, A64, 112-122. ; _computing_molecular_graphics ; Brandenburg, K. (2007). DIAMOND. Version 3.1. Crystal Impact GbR, Bonn, Germany. ; _computing_publication_material ; Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. ; _refine_special_details ; Refinement of F^2^ against ALL reflections except 0 0 1 and 0 0 2 which were evidently shadowed. 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. H atoms belonging to coordinating methyl groups were refined as pyramidal groups (DFIX C-H = 0.98 \%A) and the H---H distances set be 1.60 within 0.01 \%A and H(U~iso~) refined as a common group to the three H-atoms. The methylidene group H-atoms were restrained to C-H = 0.98 \%A and the H---H distance set be 1.60 within 0.01 \%A. H(U~iso~) were refined as a common group to the two H-atoms. All other methyl groups were refined as rigid pyramidal groups (AFIX 137) rotating around the C-C bond vector with U~iso~ set to be 1.5 times that of the parent carbon atom. Remaining groups, CH and CH2, were geometrically positioned, AFIX 13 and 23, respectively. The largest positive residual density (1.47 e/\%A^3^) is located 0.04 \%A from atom C2. The largest negative residual density (-0.89 e/\%A^3^) is located 0.07 \%A from atom C1. Atoms C52/C52A and C57/C57A in coordinated thf's were refined anisotropically in split positions. All C-C distances in the two half hexane molecules were restrained to 1.54 \%A. Comments on checkCIF alerts: PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.08 Ratio stems from disordered thf atoms C57/C57a. PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of 39.00 A**3 This a volume that represents the approx. volume of a water molecule. The warning is not applicable in this structure, the warning is hoax reflecting the loose packing and likely a hydrophobic pocket. ; _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^)+(0.0417P)^2^+29.5152P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13744 _refine_ls_number_parameters 786 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.474 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.093 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 Y1 Y 0.09978(5) 0.84740(2) 0.190399(18) 0.02801(13) Uani 1 1 d . . . C1 C -0.0232(4) 0.88877(18) 0.24441(16) 0.0171(7) Uani 1 1 d D . . H1A H -0.087(4) 0.8644(15) 0.232(2) 0.062(14) Uiso 1 1 d D . . H1B H -0.058(4) 0.9232(10) 0.246(2) 0.062(14) Uiso 1 1 d D . . Si1 Si -0.14450(15) 0.87198(7) 0.09323(6) 0.0442(4) Uani 1 1 d . . . O1 O 0.2811(3) 0.81079(15) 0.16755(15) 0.0402(10) Uani 1 1 d . B . N1 N -0.0240(4) 0.83466(18) 0.11625(16) 0.0343(11) Uani 1 1 d . . . C1S C 0.9495(10) 0.5102(5) 0.0150(4) 0.183(8) Uani 1 1 d D . . H1S1 H 0.8858 0.4841 0.0115 0.219 Uiso 1 1 calc R . . H1S2 H 0.9820 0.5120 0.0518 0.219 Uiso 1 1 calc R . . Y2 Y 0.05939(5) 0.83516(2) 0.315696(19) 0.03147(14) Uani 1 1 d . . . C2 C 0.2671(4) 0.85852(18) 0.27691(16) 0.0171(7) Uani 1 1 d D . . H2A H 0.275(6) 0.8263(11) 0.2623(19) 0.083(14) Uiso 1 1 d D . . H2B H 0.276(6) 0.859(2) 0.3131(7) 0.083(14) Uiso 1 1 d D . . H2C H 0.310(5) 0.8854(16) 0.2633(19) 0.083(14) Uiso 1 1 d D . . Si2 Si -0.24603(17) 0.80119(8) 0.31562(7) 0.0545(5) Uani 1 1 d . . . O2 O 0.2119(3) 0.79178(15) 0.37464(13) 0.0367(9) Uani 1 1 d . D . N2 N -0.1048(4) 0.8068(2) 0.34698(17) 0.0430(12) Uani 1 1 d . . . C2S C 0.8932(16) 0.5622(5) -0.0003(6) 0.214(10) Uani 1 1 d DU . . H2S1 H 0.8542 0.5615 -0.0362 0.257 Uiso 1 1 calc R . . H2S2 H 0.9535 0.5898 0.0034 0.257 Uiso 1 1 calc R . . Y3 Y 0.12933(5) 0.94820(2) 0.267311(19) 0.03000(14) Uani 1 1 d . . . Si3 Si -0.11805(17) 1.03379(8) 0.27217(7) 0.0541(5) Uani 1 1 d . . . O3 O 0.3307(3) 0.97872(15) 0.29137(15) 0.0427(10) Uani 1 1 d . . . N3 N 0.0268(4) 1.02367(17) 0.26547(16) 0.0361(11) Uani 1 1 d . . . C3 C 0.0715(5) 0.7689(2) 0.2469(2) 0.0337(13) Uani 1 1 d D . . H3A H 0.084(5) 0.753(2) 0.2141(12) 0.092(11) Uiso 1 1 d D . . H3B H 0.127(4) 0.753(2) 0.2742(16) 0.092(11) Uiso 1 1 d D . . H3C H -0.009(2) 0.759(3) 0.253(2) 0.092(11) Uiso 1 1 d D . . C3S C 0.8012(12) 0.5712(4) 0.0368(5) 0.134(4) Uani 1 1 d D . . H3SA H 0.7553 0.6022 0.0266 0.201 Uiso 1 1 calc R . . H3SB H 0.8421 0.5755 0.0718 0.201 Uiso 1 1 calc R . . H3SC H 0.7481 0.5415 0.0357 0.201 Uiso 1 1 calc R . . C4 C 0.1265(6) 0.9198(2) 0.3601(2) 0.0438(15) Uani 1 1 d D . . H4A H 0.193(4) 0.944(2) 0.368(3) 0.12(2) Uiso 1 1 d D . . H4B H 0.054(4) 0.938(2) 0.364(3) 0.12(2) Uiso 1 1 d D . . H4C H 0.137(6) 0.892(2) 0.385(2) 0.12(2) Uiso 1 1 d D . . C4S C 0.5104(11) -0.0054(5) 0.0291(3) 0.136(5) Uani 1 1 d D . . H4S1 H 0.4952 -0.0425 0.0338 0.163 Uiso 1 1 calc R . . H4S2 H 0.5952 0.0004 0.0411 0.163 Uiso 1 1 calc R . . C5 C 0.1861(5) 0.9354(2) 0.1774(2) 0.0341(13) Uani 1 1 d D . . H5A H 0.140(4) 0.930(2) 0.1430(14) 0.092(11) Uiso 1 1 d D . . H5B H 0.185(5) 0.9728(10) 0.184(2) 0.092(11) Uiso 1 1 d D . . H5C H 0.269(2) 0.926(2) 0.173(2) 0.092(11) Uiso 1 1 d D . . C5S C 0.4437(14) 0.0229(6) 0.0632(5) 0.179(7) Uani 1 1 d D . . H5S1 H 0.3580 0.0178 0.0525 0.214 Uiso 1 1 calc R . . H5S2 H 0.4608 0.0602 0.0612 0.214 Uiso 1 1 calc R . . C6 C -0.1062(6) 0.9418(3) 0.0947(3) 0.0588(19) Uani 1 1 d . . . H6A H -0.0745 0.9518 0.1298 0.088 Uiso 1 1 calc R . . H6B H -0.1772 0.9620 0.0832 0.088 Uiso 1 1 calc R . . H6C H -0.0468 0.9482 0.0720 0.088 Uiso 1 1 calc R . . C6S C 0.4769(10) 0.0043(6) 0.1180(4) 0.155(6) Uani 1 1 d D . . H6SA H 0.4199 0.0176 0.1393 0.233 Uiso 1 1 calc R . . H6SB H 0.5561 0.0168 0.1314 0.233 Uiso 1 1 calc R . . H6SC H 0.4762 -0.0334 0.1187 0.233 Uiso 1 1 calc R . . C7 C -0.2073(7) 0.8551(3) 0.0257(2) 0.064(2) Uani 1 1 d . . . H7A H -0.2670 0.8281 0.0261 0.096 Uiso 1 1 calc R . . H7B H -0.1439 0.8427 0.0073 0.096 Uiso 1 1 calc R . . H7C H -0.2437 0.8857 0.0084 0.096 Uiso 1 1 calc R . . C8 C -0.2679(6) 0.8644(3) 0.1326(3) 0.068(2) Uani 1 1 d . . . H8A H -0.2428 0.8775 0.1672 0.103 Uiso 1 1 calc R . . H8B H -0.2885 0.8279 0.1344 0.103 Uiso 1 1 calc R . . H8C H -0.3369 0.8838 0.1167 0.103 Uiso 1 1 calc R . . C9 C 0.0171(5) 0.7937(2) 0.08784(19) 0.0357(14) Uani 1 1 d . . . C10 C 0.0984(5) 0.8032(3) 0.0521(2) 0.0453(16) Uani 1 1 d . . . C11 C 0.1432(6) 0.7617(3) 0.0281(3) 0.061(2) Uani 1 1 d . . . H11A H 0.1967 0.7680 0.0043 0.073 Uiso 1 1 calc R . . C12 C 0.1134(7) 0.7116(3) 0.0374(3) 0.068(2) Uani 1 1 d . . . H12A H 0.1481 0.6839 0.0212 0.082 Uiso 1 1 calc R . . C13 C 0.0324(6) 0.7021(3) 0.0704(3) 0.0601(19) Uani 1 1 d . . . H13A H 0.0104 0.6676 0.0764 0.072 Uiso 1 1 calc R . . C14 C -0.0181(5) 0.7424(3) 0.0955(2) 0.0443(16) Uani 1 1 d . . . C15 C 0.1355(6) 0.8571(3) 0.0400(2) 0.0517(17) Uani 1 1 d . . . H15A H 0.1005 0.8810 0.0635 0.062 Uiso 1 1 calc R . . C16 C 0.2682(7) 0.8663(4) 0.0477(4) 0.096(3) Uani 1 1 d . . . H16A H 0.2994 0.8622 0.0840 0.144 Uiso 1 1 calc R . . H16B H 0.2845 0.9012 0.0365 0.144 Uiso 1 1 calc R . . H16C H 0.3062 0.8413 0.0274 0.144 Uiso 1 1 calc R . . C17 C 0.0906(9) 0.8731(4) -0.0137(3) 0.120(4) Uani 1 1 d . . . H17A H 0.0041 0.8713 -0.0192 0.180 Uiso 1 1 calc R . . H17B H 0.1225 0.8501 -0.0378 0.180 Uiso 1 1 calc R . . H17C H 0.1157 0.9085 -0.0192 0.180 Uiso 1 1 calc R . . C18 C -0.1129(5) 0.7292(2) 0.1285(2) 0.0450(15) Uani 1 1 d . . . H18A H -0.1157 0.7580 0.1535 0.054 Uiso 1 1 calc R . . C19 C -0.0903(7) 0.6792(3) 0.1593(3) 0.0574(18) Uani 1 1 d . . . H19A H -0.0092 0.6792 0.1771 0.086 Uiso 1 1 calc R . . H19B H -0.1017 0.6497 0.1361 0.086 Uiso 1 1 calc R . . H19C H -0.1457 0.6769 0.1845 0.086 Uiso 1 1 calc R . . C20 C -0.2348(6) 0.7262(3) 0.0957(3) 0.0604(19) Uani 1 1 d . . . H20A H -0.2531 0.7592 0.0785 0.091 Uiso 1 1 calc R . . H20B H -0.2949 0.7184 0.1177 0.091 Uiso 1 1 calc R . . H20C H -0.2342 0.6990 0.0700 0.091 Uiso 1 1 calc R . . C21 C -0.3488(7) 0.7688(4) 0.3561(3) 0.087(3) Uani 1 1 d . . . H21A H -0.3324 0.7317 0.3578 0.131 Uiso 1 1 calc R . . H21B H -0.4308 0.7745 0.3408 0.131 Uiso 1 1 calc R . . H21C H -0.3364 0.7833 0.3908 0.131 Uiso 1 1 calc R . . C22 C -0.3140(6) 0.8648(3) 0.2962(3) 0.069(2) Uani 1 1 d . . . H22A H -0.2669 0.8821 0.2729 0.104 Uiso 1 1 calc R . . H22B H -0.3162 0.8862 0.3267 0.104 Uiso 1 1 calc R . . H22C H -0.3946 0.8596 0.2788 0.104 Uiso 1 1 calc R . . C23 C -0.2519(7) 0.7623(3) 0.2556(3) 0.064(2) Uani 1 1 d . . . H23A H -0.2159 0.7286 0.2638 0.097 Uiso 1 1 calc R . . H23B H -0.2085 0.7802 0.2314 0.097 Uiso 1 1 calc R . . H23C H -0.3344 0.7578 0.2403 0.097 Uiso 1 1 calc R . . C24 C -0.0815(6) 0.7906(3) 0.3991(2) 0.0470(16) Uani 1 1 d . . . C25 C -0.0540(5) 0.7385(3) 0.4116(2) 0.0467(16) Uani 1 1 d . . . C26 C -0.0248(6) 0.7237(3) 0.4622(2) 0.0550(18) Uani 1 1 d . . . H26A H -0.0066 0.6887 0.4703 0.066 Uiso 1 1 calc R . . C27 C -0.0220(7) 0.7601(4) 0.5016(3) 0.068(2) Uani 1 1 d . . . H27A H -0.0004 0.7499 0.5362 0.081 Uiso 1 1 calc R . . C28 C -0.0504(7) 0.8100(3) 0.4900(3) 0.062(2) Uani 1 1 d . . . H28A H -0.0488 0.8343 0.5170 0.074 Uiso 1 1 calc R . . C29 C -0.0816(6) 0.8263(3) 0.4398(2) 0.0536(18) Uani 1 1 d . . . C30 C -0.0585(6) 0.6966(3) 0.3708(3) 0.0515(17) Uani 1 1 d . . . H30A H -0.0853 0.7131 0.3370 0.062 Uiso 1 1 calc R . . C31 C -0.1457(8) 0.6538(4) 0.3780(4) 0.098(3) Uani 1 1 d . . . H31A H -0.1482 0.6291 0.3498 0.147 Uiso 1 1 calc R . . H31B H -0.2244 0.6686 0.3784 0.147 Uiso 1 1 calc R . . H31C H -0.1206 0.6361 0.4106 0.147 Uiso 1 1 calc R . . C32 C 0.0612(7) 0.6725(3) 0.3679(3) 0.0613(19) Uani 1 1 d . . . H32A H 0.1177 0.6994 0.3619 0.092 Uiso 1 1 calc R . . H32B H 0.0545 0.6476 0.3398 0.092 Uiso 1 1 calc R . . H32C H 0.0889 0.6549 0.4003 0.092 Uiso 1 1 calc R . . C33 C -0.1200(8) 0.8813(3) 0.4306(3) 0.074(3) Uani 1 1 d . . . H33A H -0.1137 0.8891 0.3939 0.089 Uiso 1 1 calc R . . C34 C -0.0431(10) 0.9209(4) 0.4631(3) 0.112(4) Uani 1 1 d . . . H34A H 0.0405 0.9135 0.4618 0.168 Uiso 1 1 calc R . . H34B H -0.0588 0.9190 0.4987 0.168 Uiso 1 1 calc R . . H34C H -0.0619 0.9555 0.4496 0.168 Uiso 1 1 calc R . . C35 C -0.2500(9) 0.8888(3) 0.4377(4) 0.098(3) Uani 1 1 d . . . H35A H -0.2995 0.8653 0.4149 0.147 Uiso 1 1 calc R . . H35B H -0.2735 0.9244 0.4294 0.147 Uiso 1 1 calc R . . H35C H -0.2598 0.8814 0.4733 0.147 Uiso 1 1 calc R . . C36 C -0.2220(6) 1.0064(3) 0.2174(3) 0.072(2) Uani 1 1 d . . . H36A H -0.2142 0.9689 0.2172 0.107 Uiso 1 1 calc R . . H36B H -0.2028 1.0205 0.1851 0.107 Uiso 1 1 calc R . . H36C H -0.3033 1.0157 0.2215 0.107 Uiso 1 1 calc R . . C37 C -0.1524(7) 1.0018(3) 0.3327(3) 0.077(2) Uani 1 1 d . . . H37A H -0.1472 0.9644 0.3291 0.116 Uiso 1 1 calc R . . H37B H -0.2323 1.0112 0.3387 0.116 Uiso 1 1 calc R . . H37C H -0.0953 1.0132 0.3617 0.116 Uiso 1 1 calc R . . C38 C -0.1562(8) 1.1044(3) 0.2765(3) 0.079(3) Uani 1 1 d . . . H38A H -0.2207 1.1130 0.2494 0.118 Uiso 1 1 calc R . . H38B H -0.0868 1.1253 0.2725 0.118 Uiso 1 1 calc R . . H38C H -0.1810 1.1114 0.3100 0.118 Uiso 1 1 calc R . . C39 C 0.1048(5) 1.0652(2) 0.2622(2) 0.0399(14) Uani 1 1 d . . . C40 C 0.1705(6) 1.0873(2) 0.3069(2) 0.0472(16) Uani 1 1 d . . . C41 C 0.2520(7) 1.1258(3) 0.3018(3) 0.061(2) Uani 1 1 d . . . H41A H 0.2946 1.1404 0.3319 0.073 Uiso 1 1 calc R . . C42 C 0.2733(8) 1.1433(3) 0.2551(3) 0.065(2) Uani 1 1 d . . . H42A H 0.3323 1.1685 0.2526 0.079 Uiso 1 1 calc R . . C43 C 0.2083(7) 1.1238(2) 0.2119(3) 0.0583(19) Uani 1 1 d . . . H43A H 0.2207 1.1371 0.1795 0.070 Uiso 1 1 calc R . . C44 C 0.1249(6) 1.0855(2) 0.2138(2) 0.0419(15) Uani 1 1 d . . . C45 C 0.1485(7) 1.0704(3) 0.3603(2) 0.0561(19) Uani 1 1 d . . . H45A H 0.1019 1.0378 0.3565 0.067 Uiso 1 1 calc R . . C46 C 0.2609(8) 1.0599(4) 0.3963(3) 0.085(3) Uani 1 1 d . . . H46A H 0.3092 1.0349 0.3805 0.128 Uiso 1 1 calc R . . H46B H 0.2412 1.0459 0.4285 0.128 Uiso 1 1 calc R . . H46C H 0.3053 1.0920 0.4031 0.128 Uiso 1 1 calc R . . C47 C 0.0768(10) 1.1097(4) 0.3847(3) 0.107(4) Uani 1 1 d . . . H47A H 0.0118 1.1218 0.3594 0.161 Uiso 1 1 calc R . . H47B H 0.1274 1.1389 0.3969 0.161 Uiso 1 1 calc R . . H47C H 0.0448 1.0940 0.4136 0.161 Uiso 1 1 calc R . . C48 C 0.0519(6) 1.0670(2) 0.1644(2) 0.0465(16) Uani 1 1 d . . . H48A H 0.0216 1.0319 0.1710 0.056 Uiso 1 1 calc R . . C49 C -0.0556(7) 1.1021(3) 0.1499(3) 0.067(2) Uani 1 1 d . . . H49A H -0.1016 1.1039 0.1786 0.101 Uiso 1 1 calc R . . H49B H -0.1051 1.0881 0.1198 0.101 Uiso 1 1 calc R . . H49C H -0.0288 1.1367 0.1422 0.101 Uiso 1 1 calc R . . C50 C 0.1220(6) 1.0628(3) 0.1192(2) 0.0523(17) Uani 1 1 d . . . H50A H 0.1966 1.0448 0.1302 0.078 Uiso 1 1 calc R . . H50B H 0.1386 1.0973 0.1071 0.078 Uiso 1 1 calc R . . H50C H 0.0759 1.0434 0.0914 0.078 Uiso 1 1 calc R . . C51 C 0.2922(5) 0.7561(2) 0.1611(3) 0.0469(16) Uani 1 1 d D . . H51A H 0.2691 0.7455 0.1250 0.056 Uiso 1 1 calc R A 1 H51B H 0.2455 0.7365 0.1834 0.056 Uiso 1 1 calc R A 1 C52 C 0.4219(12) 0.7504(7) 0.1774(10) 0.067(4) Uani 0.364(15) 1 d PD B 1 H52A H 0.4504 0.7167 0.1668 0.080 Uiso 0.364(15) 1 calc PR B 1 H52B H 0.4415 0.7539 0.2150 0.080 Uiso 0.364(15) 1 calc PR B 1 C52A C 0.4062(6) 0.7439(3) 0.1449(4) 0.067(4) Uani 0.636(15) 1 d PD B 2 H52C H 0.3958 0.7316 0.1091 0.080 Uiso 0.636(15) 1 calc PR B 2 H52D H 0.4478 0.7171 0.1672 0.080 Uiso 0.636(15) 1 calc PR B 2 C53 C 0.4746(6) 0.7941(3) 0.1499(4) 0.091(3) Uani 1 1 d RD . . H53A H 0.5608 0.7983 0.1598 0.109 Uiso 1 1 calc R B 1 H53B H 0.4535 0.7932 0.1123 0.109 Uiso 1 1 calc R B 1 C54 C 0.4021(6) 0.8306(3) 0.1761(3) 0.075(3) Uani 1 1 d . B . H54A H 0.4314 0.8323 0.2132 0.090 Uiso 1 1 calc R . . H54B H 0.4055 0.8656 0.1615 0.090 Uiso 1 1 calc R . . C55 C 0.3131(5) 0.7624(3) 0.3624(2) 0.0489(16) Uani 1 1 d . D . H55A H 0.3703 0.7853 0.3486 0.059 Uiso 1 1 calc R . . H55B H 0.2872 0.7356 0.3365 0.059 Uiso 1 1 calc R . . C56 C 0.3686(6) 0.7379(3) 0.4120(2) 0.0573(18) Uani 1 1 d D . . H56A H 0.3322 0.7041 0.4175 0.069 Uiso 1 1 calc R C 3 H56B H 0.4548 0.7333 0.4127 0.069 Uiso 1 1 calc R C 3 C57 C 0.342(3) 0.7756(10) 0.4496(5) 0.121(5) Uani 0.86(16) 1 d PD D 3 H57A H 0.4053 0.8020 0.4547 0.146 Uiso 0.86(16) 1 calc PR D 3 H57B H 0.3378 0.7586 0.4829 0.146 Uiso 0.86(16) 1 calc PR D 3 C57A C 0.3264(6) 0.7711(3) 0.4517(2) 0.121(5) Uani 0.14(16) 1 d PD D 4 H57C H 0.3047 0.7495 0.4798 0.146 Uiso 0.14(16) 1 calc PR D 4 H57D H 0.3904 0.7948 0.4662 0.146 Uiso 0.14(16) 1 calc PR D 4 C58 C 0.2291(6) 0.7994(3) 0.4301(2) 0.0495(17) Uani 1 1 d RD . . H58A H 0.1644 0.7830 0.4456 0.059 Uiso 1 1 calc R D 3 H58B H 0.2304 0.8366 0.4384 0.059 Uiso 1 1 calc R D 3 C59 C 0.4202(7) 0.9594(3) 0.3323(3) 0.071(2) Uani 1 1 d . . . H59A H 0.3889 0.9596 0.3655 0.085 Uiso 1 1 calc R . . H59B H 0.4428 0.9237 0.3248 0.085 Uiso 1 1 calc R . . C60 C 0.5228(8) 0.9938(4) 0.3345(4) 0.102(3) Uani 1 1 d . . . H60A H 0.5405 1.0093 0.3689 0.122 Uiso 1 1 calc R . . H60B H 0.5929 0.9742 0.3273 0.122 Uiso 1 1 calc R . . C61 C 0.4951(7) 1.0332(4) 0.2968(4) 0.094(3) Uani 1 1 d . . . H61A H 0.5635 1.0400 0.2785 0.112 Uiso 1 1 calc R . . H61B H 0.4734 1.0655 0.3130 0.112 Uiso 1 1 calc R . . C62 C 0.3916(6) 1.0126(3) 0.2603(3) 0.0546(18) Uani 1 1 d . . . H62A H 0.3393 1.0410 0.2460 0.066 Uiso 1 1 calc R . . H62B H 0.4193 0.9935 0.2317 0.066 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 Y1 0.0302(3) 0.0330(3) 0.0204(2) -0.0006(2) 0.0021(2) 0.0009(2) C1 0.0193(17) 0.0219(18) 0.0100(15) 0.0011(14) 0.0013(13) -0.0002(14) Si1 0.0354(9) 0.0598(11) 0.0347(9) -0.0029(8) -0.0049(7) 0.0090(8) O1 0.034(2) 0.038(2) 0.050(2) -0.0073(19) 0.0095(19) -0.0049(18) N1 0.034(3) 0.047(3) 0.021(2) -0.005(2) 0.0005(19) 0.005(2) C1S 0.241(19) 0.247(19) 0.060(7) -0.020(10) 0.018(8) -0.133(16) Y2 0.0370(3) 0.0361(3) 0.0228(3) -0.0006(2) 0.0094(2) -0.0032(2) C2 0.0193(17) 0.0219(18) 0.0100(15) 0.0011(14) 0.0013(13) -0.0002(14) Si2 0.0427(10) 0.0698(13) 0.0546(11) 0.0004(10) 0.0199(9) -0.0143(10) O2 0.038(2) 0.047(2) 0.0260(19) 0.0034(18) 0.0060(17) 0.0013(19) N2 0.048(3) 0.053(3) 0.031(3) -0.002(2) 0.016(2) -0.009(3) C2S 0.34(2) 0.130(12) 0.190(16) 0.083(11) 0.086(16) 0.148(15) Y3 0.0365(3) 0.0300(3) 0.0240(3) -0.0005(2) 0.0061(2) 0.0024(2) Si3 0.0520(11) 0.0602(12) 0.0536(11) -0.0051(10) 0.0188(9) 0.0192(10) O3 0.042(2) 0.043(2) 0.043(2) -0.003(2) 0.0039(19) -0.006(2) N3 0.048(3) 0.032(3) 0.029(2) -0.003(2) 0.008(2) 0.008(2) C3 0.040(3) 0.037(3) 0.024(3) -0.002(2) 0.005(2) -0.005(3) C3S 0.172(13) 0.094(8) 0.135(11) -0.009(8) 0.017(9) 0.000(8) C4 0.066(4) 0.040(4) 0.028(3) -0.002(3) 0.015(3) -0.007(3) C4S 0.142(11) 0.157(12) 0.121(9) -0.035(10) 0.058(9) -0.040(9) C5 0.041(3) 0.035(3) 0.027(3) 0.002(2) 0.008(2) 0.003(3) C5S 0.206(16) 0.211(17) 0.123(12) -0.039(12) 0.036(11) -0.059(14) C6 0.050(4) 0.058(4) 0.064(5) -0.001(4) -0.007(3) 0.015(4) C6S 0.107(9) 0.303(19) 0.053(6) 0.020(9) 0.001(6) -0.006(11) C7 0.067(5) 0.071(5) 0.045(4) -0.005(4) -0.021(3) 0.016(4) C8 0.040(4) 0.097(6) 0.067(5) 0.001(4) 0.005(4) 0.013(4) C9 0.032(3) 0.052(4) 0.020(3) -0.005(3) -0.005(2) 0.002(3) C10 0.041(4) 0.071(5) 0.023(3) -0.004(3) -0.001(3) 0.005(3) C11 0.050(4) 0.095(6) 0.040(4) -0.020(4) 0.013(3) 0.010(4) C12 0.067(5) 0.083(6) 0.053(4) -0.036(4) 0.005(4) 0.017(5) C13 0.064(5) 0.063(5) 0.050(4) -0.014(4) 0.000(4) 0.002(4) C14 0.045(4) 0.059(4) 0.025(3) -0.013(3) -0.006(3) 0.006(3) C15 0.052(4) 0.076(5) 0.029(3) 0.003(3) 0.011(3) -0.001(4) C16 0.067(6) 0.124(8) 0.096(7) 0.051(6) 0.007(5) -0.012(5) C17 0.120(9) 0.144(10) 0.083(7) 0.053(7) -0.036(6) -0.031(7) C18 0.047(4) 0.049(4) 0.037(3) -0.008(3) -0.001(3) -0.009(3) C19 0.071(5) 0.051(4) 0.047(4) -0.008(3) -0.002(4) -0.009(4) C20 0.048(4) 0.077(5) 0.053(4) -0.009(4) -0.005(3) -0.004(4) C21 0.052(5) 0.119(8) 0.095(6) 0.031(6) 0.027(5) -0.019(5) C22 0.053(4) 0.086(6) 0.072(5) -0.005(4) 0.020(4) 0.009(4) C23 0.056(4) 0.070(5) 0.064(5) -0.002(4) -0.002(4) -0.021(4) C24 0.045(4) 0.061(4) 0.038(3) -0.006(3) 0.018(3) -0.020(3) C25 0.040(4) 0.064(5) 0.038(3) -0.004(3) 0.013(3) -0.018(3) C26 0.048(4) 0.075(5) 0.044(4) 0.006(4) 0.013(3) -0.012(4) C27 0.062(5) 0.111(7) 0.032(4) -0.005(4) 0.017(3) -0.019(5) C28 0.074(5) 0.073(5) 0.043(4) -0.014(4) 0.029(4) -0.019(4) C29 0.067(5) 0.060(4) 0.040(4) -0.014(3) 0.031(3) -0.022(4) C30 0.057(4) 0.050(4) 0.047(4) -0.005(3) 0.006(3) -0.011(3) C31 0.075(6) 0.095(7) 0.129(8) -0.039(6) 0.029(6) -0.032(5) C32 0.074(5) 0.057(4) 0.056(4) -0.004(4) 0.017(4) -0.012(4) C33 0.111(7) 0.065(5) 0.059(5) -0.017(4) 0.059(5) -0.029(5) C34 0.212(12) 0.088(7) 0.053(5) -0.032(5) 0.078(6) -0.066(7) C35 0.128(8) 0.072(6) 0.115(7) 0.015(5) 0.091(7) 0.021(6) C36 0.046(4) 0.087(6) 0.082(6) -0.005(5) 0.009(4) 0.021(4) C37 0.065(5) 0.098(6) 0.077(5) 0.001(5) 0.042(4) 0.015(5) C38 0.092(6) 0.079(6) 0.069(5) -0.010(4) 0.023(5) 0.041(5) C39 0.056(4) 0.026(3) 0.039(3) 0.000(3) 0.011(3) 0.008(3) C40 0.069(5) 0.035(3) 0.037(3) -0.011(3) 0.006(3) 0.006(3) C41 0.081(5) 0.041(4) 0.061(5) -0.014(4) 0.007(4) -0.006(4) C42 0.096(6) 0.040(4) 0.061(5) -0.003(4) 0.015(4) -0.019(4) C43 0.093(6) 0.037(4) 0.046(4) 0.008(3) 0.016(4) -0.003(4) C44 0.057(4) 0.027(3) 0.041(3) 0.005(3) 0.006(3) 0.010(3) C45 0.088(5) 0.043(4) 0.036(3) -0.013(3) 0.004(4) 0.007(4) C46 0.119(8) 0.092(7) 0.040(4) -0.005(4) -0.004(5) -0.001(6) C47 0.174(11) 0.110(8) 0.045(5) -0.004(5) 0.038(6) 0.049(7) C48 0.065(4) 0.038(3) 0.036(3) 0.011(3) 0.006(3) 0.012(3) C49 0.085(6) 0.067(5) 0.052(4) 0.010(4) 0.014(4) 0.031(4) C50 0.075(5) 0.048(4) 0.035(3) 0.008(3) 0.013(3) 0.012(4) C51 0.040(4) 0.043(4) 0.060(4) -0.010(3) 0.015(3) 0.003(3) C52 0.056(6) 0.051(6) 0.096(11) -0.006(8) 0.020(8) 0.008(5) C52A 0.056(6) 0.051(6) 0.096(11) -0.006(8) 0.020(8) 0.008(5) C53 0.052(5) 0.085(6) 0.139(9) -0.010(6) 0.026(5) -0.001(5) C54 0.056(5) 0.091(6) 0.085(6) -0.037(5) 0.031(4) -0.040(4) C55 0.042(4) 0.063(4) 0.043(4) 0.009(3) 0.009(3) 0.011(3) C56 0.062(5) 0.064(5) 0.046(4) 0.013(4) 0.005(3) 0.008(4) C57 0.204(14) 0.110(8) 0.038(5) 0.005(5) -0.023(6) 0.077(9) C57A 0.204(14) 0.110(8) 0.038(5) 0.005(5) -0.023(6) 0.077(9) C58 0.055(4) 0.069(5) 0.025(3) -0.006(3) 0.006(3) -0.008(4) C59 0.062(5) 0.090(6) 0.053(4) 0.012(4) -0.020(4) -0.014(4) C60 0.083(7) 0.120(9) 0.093(7) 0.011(6) -0.019(5) -0.047(6) C61 0.052(5) 0.081(6) 0.147(9) 0.001(6) 0.009(6) -0.020(5) C62 0.057(4) 0.048(4) 0.063(4) -0.001(3) 0.021(4) -0.009(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 Y1 N1 2.274(4) . ? Y1 C1 2.391(5) . ? Y1 O1 2.432(4) . ? Y1 C5 2.533(6) . ? Y1 C3 2.574(5) . ? Y1 C2 2.782(4) . ? Y1 Y3 3.3017(7) . ? Y1 Y2 3.4144(7) . ? Y1 H1A 2.57(5) . ? Y1 H3A 2.54(7) . ? Y1 H5A 2.56(7) . ? C1 Y3 2.345(5) . ? C1 Y2 2.424(4) . ? C1 H1A 0.983(19) . ? C1 H1B 0.984(19) . ? Si1 N1 1.725(5) . ? Si1 C6 1.866(7) . ? Si1 C8 1.875(7) . ? Si1 C7 1.878(6) . ? O1 C51 1.439(7) . ? O1 C54 1.465(7) . ? N1 C9 1.420(7) . ? C1S C2S 1.527(13) . ? C1S C1S 1.579(16) 3_765 ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? Y2 N2 2.276(5) . ? Y2 O2 2.445(4) . ? Y2 C3 2.519(5) . ? Y2 C4 2.559(6) . ? Y2 C2 2.780(5) . ? Y2 Y3 3.3438(7) . ? Y2 H2B 2.57(6) . ? Y2 H3B 2.58(6) . ? Y2 H4C 2.43(8) . ? C2 Y3 2.805(5) . ? C2 H2A 0.932(18) . ? C2 H2B 0.947(18) . ? C2 H2C 0.955(18) . ? Si2 N2 1.715(5) . ? Si2 C22 1.869(8) . ? Si2 C23 1.870(7) . ? Si2 C21 1.892(7) . ? O2 C55 1.459(7) . ? O2 C58 1.463(6) . ? N2 C24 1.428(8) . ? C2S C3S 1.551(13) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? Y3 N3 2.282(4) . ? Y3 O3 2.435(4) . ? Y3 C4 2.561(6) . ? Y3 C5 2.565(5) . ? Y3 H1B 2.24(5) . ? Y3 H5B 2.45(7) . ? Si3 N3 1.711(5) . ? Si3 C36 1.878(8) . ? Si3 C37 1.889(8) . ? Si3 C38 1.894(8) . ? O3 C62 1.446(7) . ? O3 C59 1.470(8) . ? N3 C39 1.409(7) . ? C3 H3A 0.985(19) . ? C3 H3B 0.989(19) . ? C3 H3C 0.991(19) . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? C4 H4A 0.99(2) . ? C4 H4B 0.982(19) . ? C4 H4C 0.982(19) . ? C4S C5S 1.458(13) . ? C4S C4S 1.546(15) 3_655 ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5 H5A 0.997(19) . ? C5 H5B 0.987(19) . ? C5 H5C 0.997(19) . ? C5S C6S 1.522(13) . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C6S H6SA 0.9800 . ? C6S H6SB 0.9800 . ? C6S H6SC 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 C14 1.415(9) . ? C9 C10 1.434(8) . ? C10 C11 1.385(9) . ? C10 C15 1.510(9) . ? C11 C12 1.376(11) . ? C11 H11A 0.9500 . ? C12 C13 1.379(10) . ? C12 H12A 0.9500 . ? C13 C14 1.404(9) . ? C13 H13A 0.9500 . ? C14 C18 1.519(9) . ? C15 C17 1.498(10) . ? C15 C16 1.522(10) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.536(9) . ? C18 C20 1.537(8) . ? C18 H18A 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.419(9) . ? C24 C29 1.419(9) . ? C25 C26 1.385(9) . ? C25 C30 1.527(9) . ? C26 C27 1.400(10) . ? C26 H26A 0.9500 . ? C27 C28 1.362(11) . ? C27 H27A 0.9500 . ? C28 C29 1.389(10) . ? C28 H28A 0.9500 . ? C29 C33 1.504(11) . ? C30 C32 1.517(10) . ? C30 C31 1.523(10) . ? C30 H30A 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.536(11) . ? C33 C34 1.537(11) . ? C33 H33A 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? 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 C40 1.429(8) . ? C39 C44 1.430(8) . ? C40 C41 1.385(9) . ? C40 C45 1.531(9) . ? C41 C42 1.368(10) . ? C41 H41A 0.9500 . ? C42 C43 1.367(10) . ? C42 H42A 0.9500 . ? C43 C44 1.384(9) . ? C43 H43A 0.9500 . ? C44 C48 1.524(9) . ? C45 C47 1.508(10) . ? C45 C46 1.513(10) . ? C45 H45A 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C50 1.530(8) . ? C48 C49 1.536(9) . ? C48 H48A 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52A 1.461(8) . ? C51 C52 1.493(14) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.515(15) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C52A C53 1.5151 . ? C52A H52C 0.9900 . ? C52A H52D 0.9900 . ? C53 C54 1.492(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.513(8) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.456(10) . ? C56 C57A 1.489(9) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.464(15) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C57A C58 1.3885 . ? C57A H57C 0.9900 . ? C57A H57D 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.470(11) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.431(12) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.517(10) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? 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 Y1 C1 103.31(15) . . ? N1 Y1 O1 100.40(15) . . ? C1 Y1 O1 156.28(14) . . ? N1 Y1 C5 102.91(17) . . ? C1 Y1 C5 86.96(17) . . ? O1 Y1 C5 87.60(16) . . ? N1 Y1 C3 105.61(17) . . ? C1 Y1 C3 83.10(17) . . ? O1 Y1 C3 90.76(16) . . ? C5 Y1 C3 151.25(17) . . ? N1 Y1 C2 174.78(15) . . ? C1 Y1 C2 81.90(14) . . ? O1 Y1 C2 74.38(13) . . ? C5 Y1 C2 77.30(16) . . ? C3 Y1 C2 74.62(15) . . ? N1 Y1 Y3 129.98(12) . . ? C1 Y1 Y3 45.24(11) . . ? O1 Y1 Y3 116.39(9) . . ? C5 Y1 Y3 50.05(12) . . ? C3 Y1 Y3 106.48(12) . . ? C2 Y1 Y3 54.09(10) . . ? N1 Y1 Y2 131.85(12) . . ? C1 Y1 Y2 45.23(10) . . ? O1 Y1 Y2 115.95(10) . . ? C5 Y1 Y2 108.80(12) . . ? C3 Y1 Y2 47.23(12) . . ? C2 Y1 Y2 52.10(9) . . ? Y3 Y1 Y2 59.691(15) . . ? N1 Y1 H1A 86.5(10) . . ? C1 Y1 H1A 22.5(6) . . ? O1 Y1 H1A 163.7(12) . . ? C5 Y1 H1A 105.4(8) . . ? C3 Y1 H1A 73.1(12) . . ? C2 Y1 H1A 98.5(11) . . ? Y3 Y1 H1A 67.7(6) . . ? Y2 Y1 H1A 50.9(12) . . ? N1 Y1 H3A 90.8(10) . . ? C1 Y1 H3A 102.6(7) . . ? O1 Y1 H3A 77.1(11) . . ? C5 Y1 H3A 161.2(13) . . ? C3 Y1 H3A 22.2(4) . . ? C2 Y1 H3A 87.9(10) . . ? Y3 Y1 H3A 128.2(5) . . ? Y2 Y1 H3A 69.4(4) . . ? H1A Y1 H3A 88.1(14) . . ? N1 Y1 H5A 80.4(5) . . ? C1 Y1 H5A 94.2(13) . . ? O1 Y1 H5A 89.5(13) . . ? C5 Y1 H5A 22.6(5) . . ? C3 Y1 H5A 173.8(5) . . ? C2 Y1 H5A 99.5(5) . . ? Y3 Y1 H5A 67.9(8) . . ? Y2 Y1 H5A 127.5(9) . . ? H1A Y1 H5A 106.3(17) . . ? H3A Y1 H5A 162.5(12) . . ? Y3 C1 Y1 88.38(15) . . ? Y3 C1 Y2 89.01(15) . . ? Y1 C1 Y2 90.32(16) . . ? Y3 C1 H1A 176(4) . . ? Y1 C1 H1A 89(3) . . ? Y2 C1 H1A 94(3) . . ? Y3 C1 H1B 72(3) . . ? Y1 C1 H1B 135(4) . . ? Y2 C1 H1B 128(4) . . ? H1A C1 H1B 108(3) . . ? N1 Si1 C6 111.4(3) . . ? N1 Si1 C8 111.8(3) . . ? C6 Si1 C8 106.5(4) . . ? N1 Si1 C7 112.6(3) . . ? C6 Si1 C7 107.8(3) . . ? C8 Si1 C7 106.4(4) . . ? C51 O1 C54 105.6(5) . . ? C51 O1 Y1 120.6(3) . . ? C54 O1 Y1 130.1(4) . . ? C9 N1 Si1 122.9(3) . . ? C9 N1 Y1 110.5(3) . . ? Si1 N1 Y1 126.3(2) . . ? C2S C1S C1S 118.3(14) . 3_765 ? C2S C1S H1S1 107.7 . . ? C1S C1S H1S1 107.7 3_765 . ? C2S C1S H1S2 107.7 . . ? C1S C1S H1S2 107.7 3_765 . ? H1S1 C1S H1S2 107.1 . . ? N2 Y2 C1 102.41(17) . . ? N2 Y2 O2 99.91(16) . . ? C1 Y2 O2 157.68(14) . . ? N2 Y2 C3 99.78(18) . . ? C1 Y2 C3 83.60(17) . . ? O2 Y2 C3 92.14(16) . . ? N2 Y2 C4 108.83(19) . . ? C1 Y2 C4 85.47(18) . . ? O2 Y2 C4 87.87(18) . . ? C3 Y2 C4 150.95(19) . . ? N2 Y2 C2 173.70(16) . . ? C1 Y2 C2 81.38(14) . . ? O2 Y2 C2 76.35(12) . . ? C3 Y2 C2 75.49(16) . . ? C4 Y2 C2 76.30(17) . . ? N2 Y2 Y3 132.53(13) . . ? C1 Y2 Y3 44.53(11) . . ? O2 Y2 Y3 117.41(9) . . ? C3 Y2 Y3 106.61(12) . . ? C4 Y2 Y3 49.24(13) . . ? C2 Y2 Y3 53.56(9) . . ? N2 Y2 Y1 127.59(12) . . ? C1 Y2 Y1 44.45(11) . . ? O2 Y2 Y1 118.56(9) . . ? C3 Y2 Y1 48.58(12) . . ? C4 Y2 Y1 106.89(13) . . ? C2 Y2 Y1 52.16(9) . . ? Y3 Y2 Y1 58.478(15) . . ? N2 Y2 H2B 159.6(6) . . ? C1 Y2 H2B 96.4(9) . . ? O2 Y2 H2B 61.6(10) . . ? C3 Y2 H2B 90.0(9) . . ? C4 Y2 H2B 64.6(11) . . ? C2 Y2 H2B 19.9(4) . . ? Y3 Y2 H2B 59.4(12) . . ? Y1 Y2 H2B 72.0(5) . . ? N2 Y2 H3B 101.4(14) . . ? C1 Y2 H3B 104.9(7) . . ? O2 Y2 H3B 69.9(5) . . ? C3 Y2 H3B 22.3(5) . . ? C4 Y2 H3B 145.1(12) . . ? C2 Y2 H3B 72.6(14) . . ? Y3 Y2 H3B 117.8(13) . . ? Y1 Y2 H3B 65.0(9) . . ? H2B Y2 H3B 81.0(17) . . ? N2 Y2 H4C 99.0(15) . . ? C1 Y2 H4C 107.5(6) . . ? O2 Y2 H4C 69.2(10) . . ? C3 Y2 H4C 155.5(16) . . ? C4 Y2 H4C 22.5(5) . . ? C2 Y2 H4C 84.5(16) . . ? Y3 Y2 H4C 71.0(6) . . ? Y1 Y2 H4C 126.3(10) . . ? H2B Y2 H4C 67.5(18) . . ? H3B Y2 H4C 136.6(16) . . ? Y2 C2 Y1 75.73(11) . . ? Y2 C2 Y3 73.55(11) . . ? Y1 C2 Y3 72.45(11) . . ? Y2 C2 H2A 96(4) . . ? Y1 C2 H2A 70(4) . . ? Y3 C2 H2A 143(4) . . ? Y2 C2 H2B 67(4) . . ? Y1 C2 H2B 143(4) . . ? Y3 C2 H2B 93(4) . . ? H2A C2 H2B 116(3) . . ? Y2 C2 H2C 144(4) . . ? Y1 C2 H2C 96(4) . . ? Y3 C2 H2C 71(4) . . ? H2A C2 H2C 114(3) . . ? H2B C2 H2C 112(3) . . ? N2 Si2 C22 112.6(3) . . ? N2 Si2 C23 112.0(3) . . ? C22 Si2 C23 106.4(4) . . ? N2 Si2 C21 112.5(3) . . ? C22 Si2 C21 106.4(4) . . ? C23 Si2 C21 106.5(4) . . ? C55 O2 C58 107.0(4) . . ? C55 O2 Y2 128.2(3) . . ? C58 O2 Y2 123.9(3) . . ? C24 N2 Si2 118.5(4) . . ? C24 N2 Y2 113.1(4) . . ? Si2 N2 Y2 128.4(3) . . ? C1S C2S C3S 105.3(10) . . ? C1S C2S H2S1 110.7 . . ? C3S C2S H2S1 110.7 . . ? C1S C2S H2S2 110.7 . . ? C3S C2S H2S2 110.7 . . ? H2S1 C2S H2S2 108.8 . . ? N3 Y3 C1 101.48(17) . . ? N3 Y3 O3 100.95(16) . . ? C1 Y3 O3 157.57(15) . . ? N3 Y3 C4 101.17(18) . . ? C1 Y3 C4 87.08(18) . . ? O3 Y3 C4 88.93(18) . . ? N3 Y3 C5 106.67(17) . . ? C1 Y3 C5 87.20(17) . . ? O3 Y3 C5 86.09(16) . . ? C4 Y3 C5 152.15(19) . . ? N3 Y3 C2 175.22(15) . . ? C1 Y3 C2 82.21(15) . . ? O3 Y3 C2 75.41(13) . . ? C4 Y3 C2 75.84(17) . . ? C5 Y3 C2 76.39(15) . . ? N3 Y3 Y1 131.32(12) . . ? C1 Y3 Y1 46.38(11) . . ? O3 Y3 Y1 115.55(10) . . ? C4 Y3 Y1 110.17(14) . . ? C5 Y3 Y1 49.21(13) . . ? C2 Y3 Y1 53.46(9) . . ? N3 Y3 Y2 127.88(12) . . ? C1 Y3 Y2 46.46(11) . . ? O3 Y3 Y2 117.02(10) . . ? C4 Y3 Y2 49.21(14) . . ? C5 Y3 Y2 110.08(13) . . ? C2 Y3 Y2 52.88(9) . . ? Y1 Y3 Y2 61.831(15) . . ? N3 Y3 H1B 76.8(5) . . ? C1 Y3 H1B 24.6(5) . . ? O3 Y3 H1B 177.8(6) . . ? C4 Y3 H1B 91.1(16) . . ? C5 Y3 H1B 94.9(15) . . ? C2 Y3 H1B 106.8(5) . . ? Y1 Y3 H1B 66.5(9) . . ? Y2 Y3 H1B 64.5(10) . . ? N3 Y3 H5B 87.4(8) . . ? C1 Y3 H5B 102.6(11) . . ? O3 Y3 H5B 78.1(13) . . ? C4 Y3 H5B 165.7(14) . . ? C5 Y3 H5B 22.6(4) . . ? C2 Y3 H5B 94.8(9) . . ? Y1 Y3 H5B 71.0(5) . . ? Y2 Y3 H5B 132.5(5) . . ? H1B Y3 H5B 102(2) . . ? N3 Si3 C36 112.4(3) . . ? N3 Si3 C37 109.7(3) . . ? C36 Si3 C37 107.4(4) . . ? N3 Si3 C38 112.9(3) . . ? C36 Si3 C38 106.7(4) . . ? C37 Si3 C38 107.4(4) . . ? C62 O3 C59 106.5(5) . . ? C62 O3 Y3 124.2(4) . . ? C59 O3 Y3 128.1(4) . . ? C39 N3 Si3 121.2(4) . . ? C39 N3 Y3 109.4(3) . . ? Si3 N3 Y3 129.2(3) . . ? Y2 C3 Y1 84.19(17) . . ? Y2 C3 H3A 161(4) . . ? Y1 C3 H3A 77(4) . . ? Y2 C3 H3B 82(4) . . ? Y1 C3 H3B 130(4) . . ? H3A C3 H3B 108(3) . . ? Y2 C3 H3C 85(4) . . ? Y1 C3 H3C 120(4) . . ? H3A C3 H3C 107(3) . . ? H3B C3 H3C 107(3) . . ? C2S C3S H3SA 109.5 . . ? C2S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? C2S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? Y2 C4 Y3 81.55(17) . . ? Y2 C4 H4A 145(5) . . ? Y3 C4 H4A 85(5) . . ? Y2 C4 H4B 106(4) . . ? Y3 C4 H4B 95(5) . . ? H4A C4 H4B 108(3) . . ? Y2 C4 H4C 71(5) . . ? Y3 C4 H4C 148(5) . . ? H4A C4 H4C 108(3) . . ? H4B C4 H4C 108(3) . . ? C5S C4S C4S 119.9(14) . 3_655 ? C5S C4S H4S1 107.3 . . ? C4S C4S H4S1 107.3 3_655 . ? C5S C4S H4S2 107.3 . . ? C4S C4S H4S2 107.3 3_655 . ? H4S1 C4S H4S2 106.9 . . ? Y1 C5 Y3 80.73(16) . . ? Y1 C5 H5A 80(4) . . ? Y3 C5 H5A 134(4) . . ? Y1 C5 H5B 148(4) . . ? Y3 C5 H5B 72(4) . . ? H5A C5 H5B 106(3) . . ? Y1 C5 H5C 102(4) . . ? Y3 C5 H5C 120(4) . . ? H5A C5 H5C 105(3) . . ? H5B C5 H5C 106(3) . . ? C4S C5S C6S 110.0(12) . . ? C4S C5S H5S1 109.7 . . ? C6S C5S H5S1 109.7 . . ? C4S C5S H5S2 109.7 . . ? C6S C5S H5S2 109.7 . . ? H5S1 C5S H5S2 108.2 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5S C6S H6SA 109.5 . . ? C5S C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? C5S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 N1 120.6(5) . . ? C14 C9 C10 118.7(5) . . ? N1 C9 C10 120.6(5) . . ? C11 C10 C9 118.7(7) . . ? C11 C10 C15 119.5(6) . . ? C9 C10 C15 121.8(6) . . ? C12 C11 C10 122.6(7) . . ? C12 C11 H11A 118.7 . . ? C10 C11 H11A 118.7 . . ? C11 C12 C13 119.1(7) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C12 C13 C14 121.4(7) . . ? C12 C13 H13A 119.3 . . ? C14 C13 H13A 119.3 . . ? C13 C14 C9 119.4(6) . . ? C13 C14 C18 118.3(6) . . ? C9 C14 C18 122.2(5) . . ? C17 C15 C10 112.8(6) . . ? C17 C15 C16 106.7(6) . . ? C10 C15 C16 115.0(6) . . ? C17 C15 H15A 107.3 . . ? C10 C15 H15A 107.3 . . ? C16 C15 H15A 107.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C19 114.4(6) . . ? C14 C18 C20 110.7(5) . . ? C19 C18 C20 109.1(5) . . ? C14 C18 H18A 107.5 . . ? C19 C18 H18A 107.5 . . ? C20 C18 H18A 107.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 118.2(6) . . ? C25 C24 N2 120.7(5) . . ? C29 C24 N2 121.1(6) . . ? C26 C25 C24 120.3(6) . . ? C26 C25 C30 117.5(6) . . ? C24 C25 C30 122.2(6) . . ? C25 C26 C27 120.3(7) . . ? C25 C26 H26A 119.8 . . ? C27 C26 H26A 119.8 . . ? C28 C27 C26 119.8(7) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? C27 C28 C29 121.7(7) . . ? C27 C28 H28A 119.2 . . ? C29 C28 H28A 119.2 . . ? C28 C29 C24 119.7(7) . . ? C28 C29 C33 118.4(6) . . ? C24 C29 C33 121.9(6) . . ? C32 C30 C31 108.4(6) . . ? C32 C30 C25 112.8(6) . . ? C31 C30 C25 113.1(6) . . ? C32 C30 H30A 107.4 . . ? C31 C30 H30A 107.4 . . ? C25 C30 H30A 107.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C35 111.5(6) . . ? C29 C33 C34 114.5(8) . . ? C35 C33 C34 109.6(7) . . ? C29 C33 H33A 107.0 . . ? C35 C33 H33A 107.0 . . ? C34 C33 H33A 107.0 . . ? 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 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si3 C36 H36A 109.5 . . ? Si3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si3 C37 H37A 109.5 . . ? Si3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si3 C38 H38A 109.5 . . ? Si3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N3 C39 C40 121.5(5) . . ? N3 C39 C44 121.3(5) . . ? C40 C39 C44 117.1(6) . . ? C41 C40 C39 119.7(6) . . ? C41 C40 C45 119.6(6) . . ? C39 C40 C45 120.7(6) . . ? C42 C41 C40 122.2(7) . . ? C42 C41 H41A 118.9 . . ? C40 C41 H41A 118.9 . . ? C43 C42 C41 118.9(7) . . ? C43 C42 H42A 120.5 . . ? C41 C42 H42A 120.5 . . ? C42 C43 C44 122.3(6) . . ? C42 C43 H43A 118.8 . . ? C44 C43 H43A 118.8 . . ? C43 C44 C39 119.6(6) . . ? C43 C44 C48 119.7(6) . . ? C39 C44 C48 120.6(6) . . ? C47 C45 C46 108.7(6) . . ? C47 C45 C40 111.5(6) . . ? C46 C45 C40 113.3(7) . . ? C47 C45 H45A 107.7 . . ? C46 C45 H45A 107.7 . . ? C40 C45 H45A 107.7 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 C50 113.8(6) . . ? C44 C48 C49 110.5(5) . . ? C50 C48 C49 109.7(5) . . ? C44 C48 H48A 107.5 . . ? C50 C48 H48A 107.5 . . ? C49 C48 H48A 107.5 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O1 C51 C52A 110.2(5) . . ? O1 C51 C52 99.5(9) . . ? O1 C51 H51A 111.9 . . ? C52A C51 H51A 77.9 . . ? C52 C51 H51A 111.9 . . ? O1 C51 H51B 111.9 . . ? C52A C51 H51B 129.7 . . ? C52 C51 H51B 111.9 . . ? H51A C51 H51B 109.6 . . ? C51 C52 C53 103.4(11) . . ? C51 C52 H52A 111.1 . . ? C53 C52 H52A 111.1 . . ? C51 C52 H52B 111.1 . . ? C53 C52 H52B 111.1 . . ? H52A C52 H52B 109.0 . . ? C51 C52A C53 105.0(4) . . ? C51 C52A H52C 110.8 . . ? C53 C52A H52C 110.8 . . ? C51 C52A H52D 110.8 . . ? C53 C52A H52D 110.8 . . ? H52C C52A H52D 108.8 . . ? C54 C53 C52A 106.0(4) . . ? C54 C53 C52 88.4(9) . . ? C54 C53 H53A 113.9 . . ? C52A C53 H53A 126.9 . . ? C52 C53 H53A 113.9 . . ? C54 C53 H53B 113.9 . . ? C52A C53 H53B 80.9 . . ? C52 C53 H53B 113.9 . . ? H53A C53 H53B 111.1 . . ? O1 C54 C53 106.1(6) . . ? O1 C54 H54A 110.5 . . ? C53 C54 H54A 110.5 . . ? O1 C54 H54B 110.5 . . ? C53 C54 H54B 110.5 . . ? H54A C54 H54B 108.7 . . ? O2 C55 C56 106.2(5) . . ? O2 C55 H55A 110.5 . . ? C56 C55 H55A 110.5 . . ? O2 C55 H55B 110.5 . . ? C56 C55 H55B 110.5 . . ? H55A C55 H55B 108.7 . . ? C57 C56 C55 101.8(7) . . ? C57A C56 C55 103.0(5) . . ? C57 C56 H56A 111.4 . . ? C57A C56 H56A 103.0 . . ? C55 C56 H56A 111.4 . . ? C57 C56 H56B 111.4 . . ? C57A C56 H56B 118.3 . . ? C55 C56 H56B 111.4 . . ? H56A C56 H56B 109.3 . . ? C56 C57 C58 107.5(10) . . ? C56 C57 H57A 110.2 . . ? C58 C57 H57A 110.2 . . ? C56 C57 H57B 110.2 . . ? C58 C57 H57B 110.2 . . ? H57A C57 H57B 108.5 . . ? C58 C57A C56 109.8(3) . . ? C58 C57A H57C 109.7 . . ? C56 C57A H57C 109.7 . . ? C58 C57A H57D 109.7 . . ? C56 C57A H57D 109.7 . . ? H57C C57A H57D 108.2 . . ? C57A C58 O2 109.1(3) . . ? O2 C58 C57 106.4(7) . . ? C57A C58 H58A 101.9 . . ? O2 C58 H58A 110.4 . . ? C57 C58 H58A 110.4 . . ? C57A C58 H58B 116.1 . . ? O2 C58 H58B 110.4 . . ? C57 C58 H58B 110.4 . . ? H58A C58 H58B 108.6 . . ? C60 C59 O3 106.9(6) . . ? C60 C59 H59A 110.3 . . ? O3 C59 H59A 110.3 . . ? C60 C59 H59B 110.3 . . ? O3 C59 H59B 110.3 . . ? H59A C59 H59B 108.6 . . ? C61 C60 C59 108.1(7) . . ? C61 C60 H60A 110.1 . . ? C59 C60 H60A 110.1 . . ? C61 C60 H60B 110.1 . . ? C59 C60 H60B 110.1 . . ? H60A C60 H60B 108.4 . . ? C60 C61 C62 105.5(7) . . ? C60 C61 H61A 110.6 . . ? C62 C61 H61A 110.6 . . ? C60 C61 H61B 110.6 . . ? C62 C61 H61B 110.6 . . ? H61A C61 H61B 108.8 . . ? O3 C62 C61 104.4(6) . . ? O3 C62 H62A 110.9 . . ? C61 C62 H62A 110.9 . . ? O3 C62 H62B 110.9 . . ? C61 C62 H62B 110.9 . . ? H62A C62 H62B 108.9 . . ? 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 N1 Y1 C1 Y3 -134.04(15) . . . . ? O1 Y1 C1 Y3 45.5(4) . . . . ? C5 Y1 C1 Y3 -31.48(16) . . . . ? C3 Y1 C1 Y3 121.48(17) . . . . ? C2 Y1 C1 Y3 46.12(13) . . . . ? Y2 Y1 C1 Y3 89.00(15) . . . . ? N1 Y1 C1 Y2 136.96(15) . . . . ? O1 Y1 C1 Y2 -43.5(4) . . . . ? C5 Y1 C1 Y2 -120.48(17) . . . . ? C3 Y1 C1 Y2 32.49(16) . . . . ? C2 Y1 C1 Y2 -42.88(14) . . . . ? Y3 Y1 C1 Y2 -89.00(15) . . . . ? N1 Y1 O1 C51 -70.5(4) . . . . ? C1 Y1 O1 C51 110.0(5) . . . . ? C5 Y1 O1 C51 -173.1(4) . . . . ? C3 Y1 O1 C51 35.6(4) . . . . ? C2 Y1 O1 C51 109.4(4) . . . . ? Y3 Y1 O1 C51 144.4(4) . . . . ? Y2 Y1 O1 C51 77.1(4) . . . . ? N1 Y1 O1 C54 134.8(6) . . . . ? C1 Y1 O1 C54 -44.8(7) . . . . ? C5 Y1 O1 C54 32.1(6) . . . . ? C3 Y1 O1 C54 -119.2(6) . . . . ? C2 Y1 O1 C54 -45.4(6) . . . . ? Y3 Y1 O1 C54 -10.3(6) . . . . ? Y2 Y1 O1 C54 -77.7(6) . . . . ? C6 Si1 N1 C9 -125.0(5) . . . . ? C8 Si1 N1 C9 116.0(5) . . . . ? C7 Si1 N1 C9 -3.8(6) . . . . ? C6 Si1 N1 Y1 48.9(4) . . . . ? C8 Si1 N1 Y1 -70.1(4) . . . . ? C7 Si1 N1 Y1 170.1(3) . . . . ? C1 Y1 N1 C9 -156.6(4) . . . . ? O1 Y1 N1 C9 23.6(4) . . . . ? C5 Y1 N1 C9 113.5(4) . . . . ? C3 Y1 N1 C9 -70.1(4) . . . . ? Y3 Y1 N1 C9 161.6(3) . . . . ? Y2 Y1 N1 C9 -116.0(3) . . . . ? C1 Y1 N1 Si1 28.9(3) . . . . ? O1 Y1 N1 Si1 -150.9(3) . . . . ? C5 Y1 N1 Si1 -61.0(3) . . . . ? C3 Y1 N1 Si1 115.3(3) . . . . ? Y3 Y1 N1 Si1 -12.9(4) . . . . ? Y2 Y1 N1 Si1 69.4(3) . . . . ? Y3 C1 Y2 N2 139.74(16) . . . . ? Y1 C1 Y2 N2 -131.89(16) . . . . ? Y3 C1 Y2 O2 -41.6(4) . . . . ? Y1 C1 Y2 O2 46.7(4) . . . . ? Y3 C1 Y2 C3 -121.61(17) . . . . ? Y1 C1 Y2 C3 -33.24(17) . . . . ? Y3 C1 Y2 C4 31.43(18) . . . . ? Y1 C1 Y2 C4 119.80(19) . . . . ? Y3 C1 Y2 C2 -45.38(14) . . . . ? Y1 C1 Y2 C2 43.00(14) . . . . ? Y1 C1 Y2 Y3 88.37(15) . . . . ? Y3 C1 Y2 Y1 -88.37(15) . . . . ? N1 Y1 Y2 N2 3.5(2) . . . . ? C1 Y1 Y2 N2 66.6(2) . . . . ? O1 Y1 Y2 N2 -131.4(2) . . . . ? C5 Y1 Y2 N2 132.0(2) . . . . ? C3 Y1 Y2 N2 -66.8(2) . . . . ? C2 Y1 Y2 N2 -172.0(2) . . . . ? Y3 Y1 Y2 N2 121.90(17) . . . . ? N1 Y1 Y2 C1 -63.1(2) . . . . ? O1 Y1 Y2 C1 162.07(19) . . . . ? C5 Y1 Y2 C1 65.4(2) . . . . ? C3 Y1 Y2 C1 -133.4(2) . . . . ? C2 Y1 Y2 C1 121.4(2) . . . . ? Y3 Y1 Y2 C1 55.33(16) . . . . ? N1 Y1 Y2 O2 135.29(19) . . . . ? C1 Y1 Y2 O2 -161.65(19) . . . . ? O1 Y1 Y2 O2 0.42(15) . . . . ? C5 Y1 Y2 O2 -96.27(17) . . . . ? C3 Y1 Y2 O2 64.9(2) . . . . ? C2 Y1 Y2 O2 -40.27(16) . . . . ? Y3 Y1 Y2 O2 -106.32(11) . . . . ? N1 Y1 Y2 C3 70.3(2) . . . . ? C1 Y1 Y2 C3 133.4(2) . . . . ? O1 Y1 Y2 C3 -64.5(2) . . . . ? C5 Y1 Y2 C3 -161.2(2) . . . . ? C2 Y1 Y2 C3 -105.2(2) . . . . ? Y3 Y1 Y2 C3 -171.26(18) . . . . ? N1 Y1 Y2 C4 -127.8(2) . . . . ? C1 Y1 Y2 C4 -64.7(2) . . . . ? O1 Y1 Y2 C4 97.37(19) . . . . ? C5 Y1 Y2 C4 0.7(2) . . . . ? C3 Y1 Y2 C4 161.9(2) . . . . ? C2 Y1 Y2 C4 56.7(2) . . . . ? Y3 Y1 Y2 C4 -9.37(17) . . . . ? N1 Y1 Y2 C2 175.6(2) . . . . ? C1 Y1 Y2 C2 -121.4(2) . . . . ? O1 Y1 Y2 C2 40.69(16) . . . . ? C5 Y1 Y2 C2 -56.00(18) . . . . ? C3 Y1 Y2 C2 105.2(2) . . . . ? Y3 Y1 Y2 C2 -66.05(12) . . . . ? N1 Y1 Y2 Y3 -118.39(16) . . . . ? C1 Y1 Y2 Y3 -55.33(16) . . . . ? O1 Y1 Y2 Y3 106.74(10) . . . . ? C5 Y1 Y2 Y3 10.05(14) . . . . ? C3 Y1 Y2 Y3 171.26(18) . . . . ? C2 Y1 Y2 Y3 66.05(12) . . . . ? C1 Y2 C2 Y1 -37.21(13) . . . . ? O2 Y2 C2 Y1 144.25(13) . . . . ? C3 Y2 C2 Y1 48.37(14) . . . . ? C4 Y2 C2 Y1 -124.61(17) . . . . ? Y3 Y2 C2 Y1 -75.56(8) . . . . ? C1 Y2 C2 Y3 38.35(12) . . . . ? O2 Y2 C2 Y3 -140.19(13) . . . . ? C3 Y2 C2 Y3 123.93(15) . . . . ? C4 Y2 C2 Y3 -49.05(16) . . . . ? Y1 Y2 C2 Y3 75.56(8) . . . . ? C1 Y1 C2 Y2 37.75(13) . . . . ? O1 Y1 C2 Y2 -142.51(14) . . . . ? C5 Y1 C2 Y2 126.44(16) . . . . ? C3 Y1 C2 Y2 -47.28(14) . . . . ? Y3 Y1 C2 Y2 76.94(9) . . . . ? C1 Y1 C2 Y3 -39.19(13) . . . . ? O1 Y1 C2 Y3 140.55(13) . . . . ? C5 Y1 C2 Y3 49.50(14) . . . . ? C3 Y1 C2 Y3 -124.22(16) . . . . ? Y2 Y1 C2 Y3 -76.94(9) . . . . ? N2 Y2 O2 C55 132.5(5) . . . . ? C1 Y2 O2 C55 -46.1(6) . . . . ? C3 Y2 O2 C55 32.2(5) . . . . ? C4 Y2 O2 C55 -118.8(5) . . . . ? C2 Y2 O2 C55 -42.3(5) . . . . ? Y3 Y2 O2 C55 -77.8(5) . . . . ? Y1 Y2 O2 C55 -10.6(5) . . . . ? N2 Y2 O2 C58 -59.7(4) . . . . ? C1 Y2 O2 C58 121.6(5) . . . . ? C3 Y2 O2 C58 -160.0(4) . . . . ? C4 Y2 O2 C58 49.0(4) . . . . ? C2 Y2 O2 C58 125.4(4) . . . . ? Y3 Y2 O2 C58 90.0(4) . . . . ? Y1 Y2 O2 C58 157.1(4) . . . . ? C22 Si2 N2 C24 116.0(5) . . . . ? C23 Si2 N2 C24 -124.1(5) . . . . ? C21 Si2 N2 C24 -4.1(6) . . . . ? C22 Si2 N2 Y2 -66.1(4) . . . . ? C23 Si2 N2 Y2 53.7(5) . . . . ? C21 Si2 N2 Y2 173.7(4) . . . . ? C1 Y2 N2 C24 -158.0(4) . . . . ? O2 Y2 N2 C24 22.6(4) . . . . ? C3 Y2 N2 C24 116.5(4) . . . . ? C4 Y2 N2 C24 -68.6(5) . . . . ? Y3 Y2 N2 C24 -120.0(4) . . . . ? Y1 Y2 N2 C24 160.9(4) . . . . ? C1 Y2 N2 Si2 24.1(4) . . . . ? O2 Y2 N2 Si2 -155.4(3) . . . . ? C3 Y2 N2 Si2 -61.4(4) . . . . ? C4 Y2 N2 Si2 113.5(4) . . . . ? Y3 Y2 N2 Si2 62.1(4) . . . . ? Y1 Y2 N2 Si2 -17.0(4) . . . . ? C1S C1S C2S C3S -178.6(14) 3_765 . . . ? Y1 C1 Y3 N3 137.49(14) . . . . ? Y2 C1 Y3 N3 -132.16(15) . . . . ? Y1 C1 Y3 O3 -41.6(4) . . . . ? Y2 C1 Y3 O3 48.7(4) . . . . ? Y1 C1 Y3 C4 -121.70(18) . . . . ? Y2 C1 Y3 C4 -31.35(18) . . . . ? Y1 C1 Y3 C5 31.04(16) . . . . ? Y2 C1 Y3 C5 121.39(17) . . . . ? Y1 C1 Y3 C2 -45.60(13) . . . . ? Y2 C1 Y3 C2 44.75(13) . . . . ? Y2 C1 Y3 Y1 90.35(15) . . . . ? Y1 C1 Y3 Y2 -90.35(15) . . . . ? Y2 C2 Y3 C1 -39.79(12) . . . . ? Y1 C2 Y3 C1 40.07(12) . . . . ? Y2 C2 Y3 O3 141.77(13) . . . . ? Y1 C2 Y3 O3 -138.37(13) . . . . ? Y2 C2 Y3 C4 49.15(16) . . . . ? Y1 C2 Y3 C4 129.01(17) . . . . ? Y2 C2 Y3 C5 -128.77(16) . . . . ? Y1 C2 Y3 C5 -48.92(15) . . . . ? Y2 C2 Y3 Y1 -79.86(9) . . . . ? Y1 C2 Y3 Y2 79.86(9) . . . . ? N1 Y1 Y3 N3 4.1(2) . . . . ? C1 Y1 Y3 N3 -61.9(2) . . . . ? O1 Y1 Y3 N3 136.83(19) . . . . ? C5 Y1 Y3 N3 75.3(2) . . . . ? C3 Y1 Y3 N3 -123.8(2) . . . . ? C2 Y1 Y3 N3 179.9(2) . . . . ? Y2 Y1 Y3 N3 -117.16(16) . . . . ? N1 Y1 Y3 C1 65.9(2) . . . . ? O1 Y1 Y3 C1 -161.32(18) . . . . ? C5 Y1 Y3 C1 137.1(2) . . . . ? C3 Y1 Y3 C1 -62.0(2) . . . . ? C2 Y1 Y3 C1 -118.24(19) . . . . ? Y2 Y1 Y3 C1 -55.31(15) . . . . ? N1 Y1 Y3 O3 -130.41(18) . . . . ? C1 Y1 Y3 O3 163.68(18) . . . . ? O1 Y1 Y3 O3 2.36(15) . . . . ? C5 Y1 Y3 O3 -59.2(2) . . . . ? C3 Y1 Y3 O3 101.69(17) . . . . ? C2 Y1 Y3 O3 45.45(15) . . . . ? Y2 Y1 Y3 O3 108.37(11) . . . . ? N1 Y1 Y3 C4 130.8(2) . . . . ? C1 Y1 Y3 C4 64.9(2) . . . . ? O1 Y1 Y3 C4 -96.5(2) . . . . ? C5 Y1 Y3 C4 -158.0(2) . . . . ? C3 Y1 Y3 C4 2.9(2) . . . . ? C2 Y1 Y3 C4 -53.4(2) . . . . ? Y2 Y1 Y3 C4 9.55(17) . . . . ? N1 Y1 Y3 C5 -71.2(2) . . . . ? C1 Y1 Y3 C5 -137.1(2) . . . . ? O1 Y1 Y3 C5 61.5(2) . . . . ? C3 Y1 Y3 C5 160.9(2) . . . . ? C2 Y1 Y3 C5 104.6(2) . . . . ? Y2 Y1 Y3 C5 167.55(17) . . . . ? N1 Y1 Y3 C2 -175.85(19) . . . . ? C1 Y1 Y3 C2 118.24(19) . . . . ? O1 Y1 Y3 C2 -43.09(16) . . . . ? C5 Y1 Y3 C2 -104.6(2) . . . . ? C3 Y1 Y3 C2 56.25(18) . . . . ? Y2 Y1 Y3 C2 62.93(11) . . . . ? N1 Y1 Y3 Y2 121.22(15) . . . . ? C1 Y1 Y3 Y2 55.31(15) . . . . ? O1 Y1 Y3 Y2 -106.01(11) . . . . ? C5 Y1 Y3 Y2 -167.55(17) . . . . ? C3 Y1 Y3 Y2 -6.68(14) . . . . ? C2 Y1 Y3 Y2 -62.93(11) . . . . ? N2 Y2 Y3 N3 8.0(2) . . . . ? C1 Y2 Y3 N3 67.0(2) . . . . ? O2 Y2 Y3 N3 -129.56(17) . . . . ? C3 Y2 Y3 N3 129.0(2) . . . . ? C4 Y2 Y3 N3 -69.7(3) . . . . ? C2 Y2 Y3 N3 -174.05(18) . . . . ? Y1 Y2 Y3 N3 122.17(15) . . . . ? N2 Y2 Y3 C1 -58.9(2) . . . . ? O2 Y2 Y3 C1 163.48(18) . . . . ? C3 Y2 Y3 C1 62.0(2) . . . . ? C4 Y2 Y3 C1 -136.7(3) . . . . ? C2 Y2 Y3 C1 118.99(19) . . . . ? Y1 Y2 Y3 C1 55.20(15) . . . . ? N2 Y2 Y3 O3 139.86(19) . . . . ? C1 Y2 Y3 O3 -161.23(19) . . . . ? O2 Y2 Y3 O3 2.26(15) . . . . ? C3 Y2 Y3 O3 -99.19(17) . . . . ? C4 Y2 Y3 O3 62.1(2) . . . . ? C2 Y2 Y3 O3 -42.24(15) . . . . ? Y1 Y2 Y3 O3 -106.02(11) . . . . ? N2 Y2 Y3 C4 77.7(3) . . . . ? C1 Y2 Y3 C4 136.7(3) . . . . ? O2 Y2 Y3 C4 -59.9(2) . . . . ? C3 Y2 Y3 C4 -161.3(2) . . . . ? C2 Y2 Y3 C4 -104.3(2) . . . . ? Y1 Y2 Y3 C4 -168.1(2) . . . . ? N2 Y2 Y3 C5 -124.1(2) . . . . ? C1 Y2 Y3 C5 -65.2(2) . . . . ? O2 Y2 Y3 C5 98.27(17) . . . . ? C3 Y2 Y3 C5 -3.2(2) . . . . ? C4 Y2 Y3 C5 158.1(2) . . . . ? C2 Y2 Y3 C5 53.78(18) . . . . ? Y1 Y2 Y3 C5 -10.01(14) . . . . ? N2 Y2 Y3 C2 -177.9(2) . . . . ? C1 Y2 Y3 C2 -118.99(19) . . . . ? O2 Y2 Y3 C2 44.49(15) . . . . ? C3 Y2 Y3 C2 -56.96(18) . . . . ? C4 Y2 Y3 C2 104.3(2) . . . . ? Y1 Y2 Y3 C2 -63.79(11) . . . . ? N2 Y2 Y3 Y1 -114.12(16) . . . . ? C1 Y2 Y3 Y1 -55.20(15) . . . . ? O2 Y2 Y3 Y1 108.28(10) . . . . ? C3 Y2 Y3 Y1 6.83(14) . . . . ? C4 Y2 Y3 Y1 168.1(2) . . . . ? C2 Y2 Y3 Y1 63.79(11) . . . . ? N3 Y3 O3 C62 -64.0(4) . . . . ? C1 Y3 O3 C62 115.1(5) . . . . ? C4 Y3 O3 C62 -165.2(5) . . . . ? C5 Y3 O3 C62 42.3(4) . . . . ? C2 Y3 O3 C62 119.2(4) . . . . ? Y1 Y3 O3 C62 82.9(4) . . . . ? Y2 Y3 O3 C62 152.8(4) . . . . ? N3 Y3 O3 C59 129.9(5) . . . . ? C1 Y3 O3 C59 -51.0(7) . . . . ? C4 Y3 O3 C59 28.7(5) . . . . ? C5 Y3 O3 C59 -123.9(5) . . . . ? C2 Y3 O3 C59 -46.9(5) . . . . ? Y1 Y3 O3 C59 -83.2(5) . . . . ? Y2 Y3 O3 C59 -13.3(6) . . . . ? C36 Si3 N3 C39 119.0(5) . . . . ? C37 Si3 N3 C39 -121.6(5) . . . . ? C38 Si3 N3 C39 -1.8(5) . . . . ? C36 Si3 N3 Y3 -66.9(4) . . . . ? C37 Si3 N3 Y3 52.6(4) . . . . ? C38 Si3 N3 Y3 172.4(3) . . . . ? C1 Y3 N3 C39 -161.4(3) . . . . ? O3 Y3 N3 C39 18.3(4) . . . . ? C4 Y3 N3 C39 109.4(4) . . . . ? C5 Y3 N3 C39 -70.9(4) . . . . ? Y1 Y3 N3 C39 -120.7(3) . . . . ? Y2 Y3 N3 C39 155.7(3) . . . . ? C1 Y3 N3 Si3 23.9(3) . . . . ? O3 Y3 N3 Si3 -156.4(3) . . . . ? C4 Y3 N3 Si3 -65.3(3) . . . . ? C5 Y3 N3 Si3 114.4(3) . . . . ? Y1 Y3 N3 Si3 64.6(3) . . . . ? Y2 Y3 N3 Si3 -19.0(4) . . . . ? N2 Y2 C3 Y1 132.33(17) . . . . ? C1 Y2 C3 Y1 30.79(15) . . . . ? O2 Y2 C3 Y1 -127.23(14) . . . . ? C4 Y2 C3 Y1 -37.8(5) . . . . ? C2 Y2 C3 Y1 -51.92(14) . . . . ? Y3 Y2 C3 Y1 -7.77(16) . . . . ? N1 Y1 C3 Y2 -133.24(15) . . . . ? C1 Y1 C3 Y2 -31.30(15) . . . . ? O1 Y1 C3 Y2 125.73(15) . . . . ? C5 Y1 C3 Y2 39.3(4) . . . . ? C2 Y1 C3 Y2 52.16(14) . . . . ? Y3 Y1 C3 Y2 7.86(16) . . . . ? N2 Y2 C4 Y3 -130.45(17) . . . . ? C1 Y2 C4 Y3 -28.87(16) . . . . ? O2 Y2 C4 Y3 129.81(16) . . . . ? C3 Y2 C4 Y3 39.2(5) . . . . ? C2 Y2 C4 Y3 53.34(15) . . . . ? Y1 Y2 C4 Y3 10.56(18) . . . . ? N3 Y3 C4 Y2 131.01(17) . . . . ? C1 Y3 C4 Y2 29.88(17) . . . . ? O3 Y3 C4 Y2 -128.04(17) . . . . ? C5 Y3 C4 Y2 -48.5(5) . . . . ? C2 Y3 C4 Y2 -52.82(15) . . . . ? Y1 Y3 C4 Y2 -11.13(19) . . . . ? N1 Y1 C5 Y3 131.89(15) . . . . ? C1 Y1 C5 Y3 28.93(15) . . . . ? O1 Y1 C5 Y3 -127.98(15) . . . . ? C3 Y1 C5 Y3 -40.8(4) . . . . ? C2 Y1 C5 Y3 -53.45(13) . . . . ? Y2 Y1 C5 Y3 -11.34(15) . . . . ? N3 Y3 C5 Y1 -130.69(16) . . . . ? C1 Y3 C5 Y1 -29.54(16) . . . . ? O3 Y3 C5 Y1 129.05(15) . . . . ? C4 Y3 C5 Y1 48.8(5) . . . . ? C2 Y3 C5 Y1 53.12(14) . . . . ? Y2 Y3 C5 Y1 11.67(16) . . . . ? C4S C4S C5S C6S 178.3(14) 3_655 . . . ? Si1 N1 C9 C14 -95.9(6) . . . . ? Y1 N1 C9 C14 89.4(5) . . . . ? Si1 N1 C9 C10 86.3(6) . . . . ? Y1 N1 C9 C10 -88.4(5) . . . . ? C14 C9 C10 C11 -2.7(8) . . . . ? N1 C9 C10 C11 175.1(5) . . . . ? C14 C9 C10 C15 177.0(5) . . . . ? N1 C9 C10 C15 -5.1(8) . . . . ? C9 C10 C11 C12 -0.4(10) . . . . ? C15 C10 C11 C12 179.9(6) . . . . ? C10 C11 C12 C13 2.4(11) . . . . ? C11 C12 C13 C14 -1.3(11) . . . . ? C12 C13 C14 C9 -1.8(10) . . . . ? C12 C13 C14 C18 175.8(6) . . . . ? N1 C9 C14 C13 -174.1(5) . . . . ? C10 C9 C14 C13 3.8(8) . . . . ? N1 C9 C14 C18 8.4(8) . . . . ? C10 C9 C14 C18 -173.8(5) . . . . ? C11 C10 C15 C17 67.5(9) . . . . ? C9 C10 C15 C17 -112.2(8) . . . . ? C11 C10 C15 C16 -55.1(8) . . . . ? C9 C10 C15 C16 125.1(7) . . . . ? C13 C14 C18 C19 38.6(8) . . . . ? C9 C14 C18 C19 -143.8(6) . . . . ? C13 C14 C18 C20 -85.1(7) . . . . ? C9 C14 C18 C20 92.5(7) . . . . ? Si2 N2 C24 C25 86.3(7) . . . . ? Y2 N2 C24 C25 -91.9(6) . . . . ? Si2 N2 C24 C29 -95.7(6) . . . . ? Y2 N2 C24 C29 86.2(6) . . . . ? C29 C24 C25 C26 -1.9(9) . . . . ? N2 C24 C25 C26 176.2(5) . . . . ? C29 C24 C25 C30 176.4(6) . . . . ? N2 C24 C25 C30 -5.5(9) . . . . ? C24 C25 C26 C27 -0.1(10) . . . . ? C30 C25 C26 C27 -178.4(6) . . . . ? C25 C26 C27 C28 1.3(10) . . . . ? C26 C27 C28 C29 -0.5(11) . . . . ? C27 C28 C29 C24 -1.5(11) . . . . ? C27 C28 C29 C33 175.8(7) . . . . ? C25 C24 C29 C28 2.6(9) . . . . ? N2 C24 C29 C28 -175.4(6) . . . . ? C25 C24 C29 C33 -174.6(6) . . . . ? N2 C24 C29 C33 7.4(10) . . . . ? C26 C25 C30 C32 -65.2(8) . . . . ? C24 C25 C30 C32 116.5(7) . . . . ? C26 C25 C30 C31 58.3(9) . . . . ? C24 C25 C30 C31 -120.0(7) . . . . ? C28 C29 C33 C35 -81.1(9) . . . . ? C24 C29 C33 C35 96.1(8) . . . . ? C28 C29 C33 C34 44.0(9) . . . . ? C24 C29 C33 C34 -138.8(7) . . . . ? Si3 N3 C39 C40 89.1(6) . . . . ? Y3 N3 C39 C40 -86.2(6) . . . . ? Si3 N3 C39 C44 -93.4(6) . . . . ? Y3 N3 C39 C44 91.3(5) . . . . ? N3 C39 C40 C41 175.7(6) . . . . ? C44 C39 C40 C41 -1.9(9) . . . . ? N3 C39 C40 C45 -6.5(9) . . . . ? C44 C39 C40 C45 175.9(6) . . . . ? C39 C40 C41 C42 -0.6(11) . . . . ? C45 C40 C41 C42 -178.5(7) . . . . ? C40 C41 C42 C43 3.0(12) . . . . ? C41 C42 C43 C44 -2.7(12) . . . . ? C42 C43 C44 C39 0.1(10) . . . . ? C42 C43 C44 C48 177.6(7) . . . . ? N3 C39 C44 C43 -175.4(6) . . . . ? C40 C39 C44 C43 2.2(9) . . . . ? N3 C39 C44 C48 7.1(8) . . . . ? C40 C39 C44 C48 -175.3(5) . . . . ? C41 C40 C45 C47 74.6(9) . . . . ? C39 C40 C45 C47 -103.2(8) . . . . ? C41 C40 C45 C46 -48.5(9) . . . . ? C39 C40 C45 C46 133.7(7) . . . . ? C43 C44 C48 C50 39.5(8) . . . . ? C39 C44 C48 C50 -143.1(6) . . . . ? C43 C44 C48 C49 -84.5(8) . . . . ? C39 C44 C48 C49 92.9(7) . . . . ? C54 O1 C51 C52A -22.7(8) . . . . ? Y1 O1 C51 C52A 177.1(5) . . . . ? C54 O1 C51 C52 10.9(11) . . . . ? Y1 O1 C51 C52 -149.3(10) . . . . ? O1 C51 C52 C53 -45.5(14) . . . . ? C52A C51 C52 C53 66.8(11) . . . . ? O1 C51 C52A C53 8.9(5) . . . . ? C52 C51 C52A C53 -67.7(12) . . . . ? C51 C52A C53 C54 8.1(5) . . . . ? C51 C52A C53 C52 68.8(12) . . . . ? C51 C52 C53 C54 58.0(13) . . . . ? C51 C52 C53 C52A -65.0(11) . . . . ? C51 O1 C54 C53 27.2(8) . . . . ? Y1 O1 C54 C53 -175.2(5) . . . . ? C52A C53 C54 O1 -21.8(7) . . . . ? C52 C53 C54 O1 -50.4(9) . . . . ? C58 O2 C55 C56 18.4(7) . . . . ? Y2 O2 C55 C56 -172.2(4) . . . . ? O2 C55 C56 C57 -31.0(19) . . . . ? O2 C55 C56 C57A -22.0(7) . . . . ? C57A C56 C57 C58 -67(2) . . . . ? C55 C56 C57 C58 32(3) . . . . ? C57 C56 C57A C58 101(3) . . . . ? C55 C56 C57A C58 18.3(6) . . . . ? C56 C57A C58 O2 -7.5(3) . . . . ? C56 C57A C58 C57 -81(3) . . . . ? C55 O2 C58 C57A -7.0(4) . . . . ? Y2 O2 C58 C57A -177.01(18) . . . . ? C55 O2 C58 C57 1.7(18) . . . . ? Y2 O2 C58 C57 -168.2(17) . . . . ? C56 C57 C58 C57A 87(4) . . . . ? C56 C57 C58 O2 -22(3) . . . . ? C62 O3 C59 C60 17.3(9) . . . . ? Y3 O3 C59 C60 -174.7(6) . . . . ? O3 C59 C60 C61 1.2(11) . . . . ? C59 C60 C61 C62 -18.3(12) . . . . ? C59 O3 C62 C61 -28.0(7) . . . . ? Y3 O3 C62 C61 163.4(5) . . . . ? C60 C61 C62 O3 28.8(10) . . . . ? # Attachment 'Compound4c.cif' # Compound 4c #=================================================================== data_zm118 _database_code_depnum_ccdc_archive 'CCDC 765380' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H116 Lu3 N3 O3 Si3, 2(C4 H8 O)' _chemical_formula_sum 'C70 H132 Lu3 N3 O5 Si3' _chemical_formula_weight 1704.97 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' Lu Lu -0.4720 5.8584 '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' _symmetry_space_group_name_HALL '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6347(7) _cell_length_b 13.0521(8) _cell_length_c 28.3440(16) _cell_angle_alpha 99.559(1) _cell_angle_beta 96.973(1) _cell_angle_gamma 105.926(1) _cell_volume 4017.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19596 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 30.87 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 3.745 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2835 _exptl_absorpt_correction_T_max 0.4545 _exptl_absorpt_process_details ; SADABS version 2008/1, G.M Sheldrick, University of G\"ttingen, Germany, 2008. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'TXS Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 47500 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 30.03 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.984 _reflns_number_total 23137 _reflns_number_gt 19572 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Bruker (1999). SMART, version 5.054, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_cell_refinement ; Bruker (2008). SAINT, version 6.45A, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_data_reduction ; Bruker (2004). SAINT, version 6.45a, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_structure_solution ; Sheldrick, G. M. (2008). Acta Crystallographica, A64, 112-122. ; _computing_structure_refinement ; Sheldrick, G. M. (2008). Acta Crystallographica, A64, 112-122. ; _computing_molecular_graphics ; Brandenburg, K. (2007). DIAMOND. Version 3.1. Crystal Impact GbR, Bonn, Germany. ; _computing_publication_material ; Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. ; _refine_special_details ; Refinement of F^2^ against ALL reflections except for six low-order reflections which were liekly shadowed. 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. Refinement of disorder in two coordinated thf molecules has been done. There are three solvent thf molecules in the structure. One of these, lying on a centre of inversion and partially occupied has been squeezed out. See PLATON/Squeeze details below. This accounts for the void (190 /\%A^3^ reported by checkCIF. The two remaining show large disorder and any disorder modelling is pointless with or without application of ADP's. neither does it improve on the magnitude of the residual peaks in the structures. The large residual peaks in this structure are not due to erroneous atomic assignments. Rather, this is due to the fact that the structure is rich on thf solvent molecules, some most likely only partially occupied. This means that the crystal develops defects, more so upon cooling when shrinking effects are significant, which demonstrates itself through the crystal developing small cracks. Effectively this leads to a set of micropscopic multiple sets of twins. Hence the occurence of spurious peaks, which actually can be even refined, but having no chemcial sense. H atoms belonging to coordinating methyl groups were refined as pyramidal groups (DFIX C-H = 0.98 \%A) and the H---H distances set be 1.60 within 0.01 \%A and H(U~iso~) refined as a common group to the three H-atoms. The methylidene group H-atoms were restrained to C-H = 0.98 \%A and the H---H distance set be 1.60 within 0.01 \%A. H(U~iso~) were refined as a common group to the two H-atoms. All other methyl groups were refined as rigid pyramidal groups (AFIX 137) rotating around the C-C bond vector with U~iso~ set to be 1.5 times that of the parent carbon atom. Remaining groups, CH and CH2, were geometrically positioned, AFIX 13 and 23, respectively. The largest positive residual density (5.01 e/\%A^3^) is located 0.71 \%A from atom H3C. The largest negative residual density (-6.16 e/\%A^3^) is located 1.59 \%A from atom C28. COMMENT on checkCIF alerts: The disordered thf's result in the A level Alert (PLAT220). ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.067 0.667 0.764 7 1 ' ' 2 0.500 0.000 1.000 194 60 ' ' 3 0.933 0.333 0.236 7 1 ' ' _platon_squeeze_details ; ; _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^)+(0.0001P)^2^+38.7001P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23137 _refine_ls_number_parameters 763 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1117 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 5.026 _refine_diff_density_min -6.160 _refine_diff_density_rms 0.190 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 Lu1 Lu 0.72100(2) 0.558039(18) 0.314512(8) 0.01966(5) Uani 1 1 d . . . Lu2 Lu 0.77870(2) 0.748906(18) 0.251110(8) 0.01908(5) Uani 1 1 d . . . Lu3 Lu 0.60003(2) 0.511976(18) 0.199311(8) 0.01987(5) Uani 1 1 d . C . Si1 Si 0.54347(15) 0.63842(13) 0.40003(6) 0.0230(3) Uani 1 1 d . . . O1 O 0.8830(4) 0.4838(4) 0.33830(16) 0.0288(9) Uani 1 1 d . . . N1 N 0.6310(4) 0.5577(4) 0.37975(16) 0.0203(8) Uani 1 1 d . . . C1 C 0.6014(5) 0.6387(4) 0.26695(18) 0.0196(9) Uani 1 1 d D . . H1A H 0.537(4) 0.575(3) 0.270(2) 0.024 Uiso 1 1 d D . . H1B H 0.576(5) 0.704(3) 0.275(2) 0.024 Uiso 1 1 d D . . Si2 Si 0.59957(15) 0.92952(13) 0.24958(7) 0.0276(3) Uani 1 1 d . . . N2 N 0.7409(4) 0.9098(3) 0.25965(17) 0.0211(9) Uani 1 1 d . . . C2 C 0.8402(4) 0.5597(4) 0.23641(17) 0.0143(8) Uani 1 1 d D . . H2A H 0.846(5) 0.498(3) 0.2507(16) 0.021 Uiso 1 1 d D . . H2B H 0.907(4) 0.624(3) 0.2519(15) 0.021 Uiso 1 1 d D . . H2C H 0.837(5) 0.543(4) 0.2016(7) 0.021 Uiso 1 1 d D . . O2 O 0.9802(4) 0.8062(4) 0.23205(17) 0.0322(9) Uani 1 1 d . B . Si3 Si 0.28167(15) 0.45330(15) 0.19526(6) 0.0291(3) Uani 1 1 d . . . N3 N 0.4018(4) 0.4492(4) 0.16526(17) 0.0253(10) Uani 1 1 d . . . O3 O 0.6624(4) 0.4073(4) 0.13539(15) 0.0334(10) Uani 1 1 d D . . C3 C 0.6081(6) 0.3830(4) 0.2549(2) 0.0254(11) Uani 1 1 d D . . H3A H 0.6666 0.3586 0.2745 0.038 Uiso 1 1 calc RD . . H3B H 0.5877 0.3392 0.2217 0.038 Uiso 1 1 calc RD . . H3C H 0.5344 0.3745 0.2692 0.038 Uiso 1 1 calc RD . . C4 C 0.8729(6) 0.7407(5) 0.3344(2) 0.0269(11) Uani 1 1 d D . . H4A H 0.9120 0.8106 0.3262 0.040 Uiso 1 1 calc RD C . H4B H 0.9348 0.7067 0.3442 0.040 Uiso 1 1 calc RD . . H4C H 0.8293 0.7530 0.3613 0.040 Uiso 1 1 calc RD . . C5 C 0.7007(5) 0.6709(5) 0.1625(2) 0.0248(11) Uani 1 1 d D . . H5A H 0.6179 0.6394 0.1440 0.037 Uiso 1 1 calc RD . . H5B H 0.7573 0.6459 0.1440 0.037 Uiso 1 1 calc RD . . H5C H 0.7227 0.7506 0.1684 0.037 Uiso 1 1 calc RD . . C6 C 0.3956(6) 0.6103(6) 0.3582(2) 0.0332(13) Uani 1 1 d . . . H6A H 0.4111 0.6355 0.3282 0.050 Uiso 1 1 calc R . . H6B H 0.3447 0.6490 0.3740 0.050 Uiso 1 1 calc R . . H6C H 0.3536 0.5319 0.3504 0.050 Uiso 1 1 calc R . . C7 C 0.5020(7) 0.6172(6) 0.4606(2) 0.0362(14) Uani 1 1 d . . . H7A H 0.5586 0.5852 0.4769 0.054 Uiso 1 1 calc R . . H7B H 0.4191 0.5680 0.4557 0.054 Uiso 1 1 calc R . . H7C H 0.5069 0.6874 0.4808 0.054 Uiso 1 1 calc R . . C8 C 0.6239(6) 0.7868(5) 0.4064(2) 0.0332(13) Uani 1 1 d . . . H8A H 0.6494 0.7996 0.3756 0.050 Uiso 1 1 calc R . . H8B H 0.6955 0.8090 0.4322 0.050 Uiso 1 1 calc R . . H8C H 0.5690 0.8293 0.4147 0.050 Uiso 1 1 calc R . . C9 C 0.6642(5) 0.4901(4) 0.41022(19) 0.0212(10) Uani 1 1 d . . . C10 C 0.5937(5) 0.3792(5) 0.40389(19) 0.0231(10) Uani 1 1 d . . . C11 C 0.6321(6) 0.3133(5) 0.4330(2) 0.0305(12) Uani 1 1 d . . . H11A H 0.5865 0.2387 0.4280 0.037 Uiso 1 1 calc R . . C12 C 0.7344(6) 0.3545(6) 0.4685(3) 0.0353(14) Uani 1 1 d . . . H12A H 0.7593 0.3084 0.4875 0.042 Uiso 1 1 calc R . . C13 C 0.8006(6) 0.4630(6) 0.4763(2) 0.0323(13) Uani 1 1 d . . . H13A H 0.8698 0.4915 0.5014 0.039 Uiso 1 1 calc R . . C14 C 0.7676(5) 0.5320(5) 0.4478(2) 0.0249(11) Uani 1 1 d . . . C15 C 0.4750(5) 0.3318(5) 0.3681(2) 0.0266(11) Uani 1 1 d . . . H15A H 0.4717 0.3824 0.3455 0.032 Uiso 1 1 calc R . . C16 C 0.4617(7) 0.2191(5) 0.3377(2) 0.0397(16) Uani 1 1 d . . . H16A H 0.5328 0.2226 0.3220 0.060 Uiso 1 1 calc R . . H16B H 0.3883 0.1965 0.3128 0.060 Uiso 1 1 calc R . . H16C H 0.4554 0.1663 0.3588 0.060 Uiso 1 1 calc R . . C17 C 0.3679(6) 0.3247(6) 0.3957(2) 0.0365(15) Uani 1 1 d . . . H17A H 0.3742 0.3974 0.4138 0.055 Uiso 1 1 calc R . . H17B H 0.3699 0.2759 0.4184 0.055 Uiso 1 1 calc R . . H17C H 0.2913 0.2962 0.3724 0.055 Uiso 1 1 calc R . . C18 C 0.8433(6) 0.6523(5) 0.4589(2) 0.0290(12) Uani 1 1 d . . . H18A H 0.8114 0.6868 0.4334 0.035 Uiso 1 1 calc R . . C19 C 0.8277(8) 0.7111(7) 0.5083(3) 0.051(2) Uani 1 1 d . . . H19A H 0.8726 0.7887 0.5138 0.076 Uiso 1 1 calc R . . H19B H 0.8591 0.6794 0.5341 0.076 Uiso 1 1 calc R . . H19C H 0.7413 0.7026 0.5083 0.076 Uiso 1 1 calc R . . C20 C 0.9778(6) 0.6695(6) 0.4577(3) 0.0440(17) Uani 1 1 d . . . H20A H 0.9877 0.6371 0.4252 0.066 Uiso 1 1 calc R . . H20B H 1.0113 0.6348 0.4818 0.066 Uiso 1 1 calc R . . H20C H 1.0209 0.7477 0.4652 0.066 Uiso 1 1 calc R . . C21 C 0.6115(7) 1.0753(6) 0.2470(3) 0.0421(16) Uani 1 1 d . . . H21A H 0.6631 1.1236 0.2767 0.063 Uiso 1 1 calc R . . H21B H 0.5303 1.0847 0.2442 0.063 Uiso 1 1 calc R . . H21C H 0.6471 1.0935 0.2187 0.063 Uiso 1 1 calc R . . C22 C 0.5070(6) 0.8429(6) 0.1902(3) 0.0379(15) Uani 1 1 d . . . H22A H 0.4984 0.7660 0.1902 0.057 Uiso 1 1 calc R . . H22B H 0.5479 0.8639 0.1635 0.057 Uiso 1 1 calc R . . H22C H 0.4265 0.8535 0.1859 0.057 Uiso 1 1 calc R . . C23 C 0.5053(7) 0.8953(6) 0.2974(3) 0.0401(15) Uani 1 1 d . . . H23A H 0.5441 0.9459 0.3284 0.060 Uiso 1 1 calc R . . H23B H 0.4983 0.8206 0.3010 0.060 Uiso 1 1 calc R . . H23C H 0.4241 0.9016 0.2877 0.060 Uiso 1 1 calc R . . C24 C 0.8471(5) 1.0031(4) 0.2711(2) 0.0238(11) Uani 1 1 d . . . C25 C 0.9033(6) 1.0465(5) 0.3202(2) 0.0276(12) Uani 1 1 d . . . C26 C 1.0161(6) 1.1291(5) 0.3304(2) 0.0359(14) Uani 1 1 d . . . H26A H 1.0565 1.1569 0.3631 0.043 Uiso 1 1 calc R . . C27 C 1.0685(7) 1.1700(6) 0.2940(3) 0.0410(16) Uani 1 1 d . . . H27A H 1.1458 1.2235 0.3014 0.049 Uiso 1 1 calc R . . C28 C 1.0088(6) 1.1333(5) 0.2469(2) 0.0343(14) Uani 1 1 d . . . H28A H 1.0435 1.1654 0.2222 0.041 Uiso 1 1 calc R . . C29 C 0.8986(5) 1.0502(5) 0.2342(2) 0.0265(11) Uani 1 1 d . . . C30 C 0.8453(6) 1.0117(5) 0.3624(2) 0.0317(13) Uani 1 1 d . . . H30A H 0.7872 0.9368 0.3503 0.038 Uiso 1 1 calc R . . C31 C 0.7721(8) 1.0886(6) 0.3800(3) 0.050(2) Uani 1 1 d . . . H31A H 0.7167 1.0941 0.3523 0.075 Uiso 1 1 calc R . . H31B H 0.8280 1.1610 0.3952 0.075 Uiso 1 1 calc R . . H31C H 0.7251 1.0594 0.4039 0.075 Uiso 1 1 calc R . . C32 C 0.9366(8) 1.0077(6) 0.4058(2) 0.0441(17) Uani 1 1 d . . . H32A H 0.9946 0.9721 0.3938 0.066 Uiso 1 1 calc R . . H32B H 0.8929 0.9664 0.4274 0.066 Uiso 1 1 calc R . . H32C H 0.9805 1.0820 0.4237 0.066 Uiso 1 1 calc R . . C33 C 0.8372(6) 1.0163(5) 0.1811(2) 0.0309(13) Uani 1 1 d . . . H33A H 0.7534 0.9672 0.1795 0.037 Uiso 1 1 calc R . . C34 C 0.8257(9) 1.1152(7) 0.1603(3) 0.054(2) Uani 1 1 d . . . H34A H 0.7978 1.1631 0.1836 0.081 Uiso 1 1 calc R . . H34B H 0.7671 1.0903 0.1298 0.081 Uiso 1 1 calc R . . H34C H 0.9050 1.1554 0.1541 0.081 Uiso 1 1 calc R . . C35 C 0.9009(7) 0.9551(6) 0.1484(3) 0.0422(16) Uani 1 1 d . . . H35A H 0.9055 0.8894 0.1600 0.063 Uiso 1 1 calc R . . H35B H 0.9831 1.0019 0.1490 0.063 Uiso 1 1 calc R . . H35C H 0.8552 0.9344 0.1151 0.063 Uiso 1 1 calc R . . C36 C 0.1301(7) 0.3774(8) 0.1558(3) 0.054(2) Uani 1 1 d . . . H36A H 0.1308 0.3046 0.1405 0.081 Uiso 1 1 calc R . . H36B H 0.1141 0.4173 0.1306 0.081 Uiso 1 1 calc R . . H36C H 0.0663 0.3708 0.1757 0.081 Uiso 1 1 calc R . . C37 C 0.2879(6) 0.3903(5) 0.2500(2) 0.0349(14) Uani 1 1 d . . . H37A H 0.3639 0.4295 0.2727 0.052 Uiso 1 1 calc R . . H37B H 0.2842 0.3137 0.2399 0.052 Uiso 1 1 calc R . . H37C H 0.2190 0.3947 0.2661 0.052 Uiso 1 1 calc R . . C38 C 0.2720(6) 0.5946(6) 0.2168(3) 0.0387(15) Uani 1 1 d . . . H38A H 0.3490 0.6399 0.2375 0.058 Uiso 1 1 calc R . . H38B H 0.2061 0.5909 0.2356 0.058 Uiso 1 1 calc R . . H38C H 0.2560 0.6266 0.1887 0.058 Uiso 1 1 calc R . . C39 C 0.3703(5) 0.3948(5) 0.1154(2) 0.0293(12) Uani 1 1 d . . . C40 C 0.3578(6) 0.4546(6) 0.0779(2) 0.0330(13) Uani 1 1 d . . . C41 C 0.3303(7) 0.3996(7) 0.0290(2) 0.0442(18) Uani 1 1 d . . . H41A H 0.3234 0.4393 0.0041 0.053 Uiso 1 1 calc R . . C42 C 0.3131(7) 0.2880(7) 0.0164(2) 0.0472(19) Uani 1 1 d . . . H42A H 0.2951 0.2518 -0.0168 0.057 Uiso 1 1 calc R . . C43 C 0.3223(7) 0.2308(7) 0.0523(2) 0.0410(16) Uani 1 1 d . . . H43A H 0.3077 0.1543 0.0434 0.049 Uiso 1 1 calc R . . C44 C 0.3523(6) 0.2805(5) 0.1016(2) 0.0334(13) Uani 1 1 d . . . C45 C 0.3706(6) 0.5748(6) 0.0895(2) 0.0364(14) Uani 1 1 d . . . H45A H 0.4064 0.6033 0.1247 0.044 Uiso 1 1 calc R . . C46 C 0.2457(8) 0.5939(8) 0.0809(3) 0.0499(19) Uani 1 1 d . . . H46A H 0.1936 0.5561 0.1013 0.075 Uiso 1 1 calc R . . H46B H 0.2082 0.5656 0.0466 0.075 Uiso 1 1 calc R . . H46C H 0.2558 0.6721 0.0893 0.075 Uiso 1 1 calc R . . C47 C 0.4545(7) 0.6406(7) 0.0600(3) 0.0481(19) Uani 1 1 d . . . H47A H 0.5306 0.6217 0.0620 0.072 Uiso 1 1 calc R . . H47B H 0.4719 0.7187 0.0732 0.072 Uiso 1 1 calc R . . H47C H 0.4145 0.6234 0.0260 0.072 Uiso 1 1 calc R . . C48 C 0.3583(8) 0.2088(6) 0.1381(3) 0.049(2) Uani 1 1 d . . . H48A H 0.3904 0.2588 0.1706 0.059 Uiso 1 1 calc R . . C49 C 0.2407(12) 0.1348(10) 0.1416(5) 0.097(4) Uani 1 1 d . . . H49A H 0.1873 0.1774 0.1518 0.146 Uiso 1 1 calc R . . H49B H 0.2530 0.0907 0.1655 0.146 Uiso 1 1 calc R . . H49C H 0.2035 0.0868 0.1098 0.146 Uiso 1 1 calc R . . C50 C 0.4443(12) 0.1440(9) 0.1301(5) 0.080(3) Uani 1 1 d . . . H50A H 0.5239 0.1928 0.1286 0.120 Uiso 1 1 calc R . . H50B H 0.4133 0.0900 0.0995 0.120 Uiso 1 1 calc R . . H50C H 0.4523 0.1067 0.1571 0.120 Uiso 1 1 calc R . . C51 C 0.8610(6) 0.3768(5) 0.3507(2) 0.0301(12) Uani 1 1 d . . . H51A H 0.8502 0.3194 0.3214 0.036 Uiso 1 1 calc R . . H51B H 0.7880 0.3589 0.3660 0.036 Uiso 1 1 calc R . . C52 C 0.9752(6) 0.3879(6) 0.3863(3) 0.0357(14) Uani 1 1 d . . . H52A H 0.9696 0.4205 0.4198 0.043 Uiso 1 1 calc R . . H52B H 0.9889 0.3163 0.3861 0.043 Uiso 1 1 calc R . . C53 C 1.0759(6) 0.4633(6) 0.3674(3) 0.0406(16) Uani 1 1 d . . . H53A H 1.1220 0.4213 0.3495 0.049 Uiso 1 1 calc R . . H53B H 1.1329 0.5185 0.3945 0.049 Uiso 1 1 calc R . . C54 C 1.0107(6) 0.5178(7) 0.3333(3) 0.0412(17) Uani 1 1 d . . . H54A H 1.0450 0.5980 0.3428 0.049 Uiso 1 1 calc R . . H54B H 1.0197 0.4939 0.2993 0.049 Uiso 1 1 calc R . . C55 C 1.0833(6) 0.8831(6) 0.2669(3) 0.0401(16) Uani 1 1 d D . . H55A H 1.1191 0.8453 0.2896 0.048 Uiso 1 1 calc R A 3 H55B H 1.0580 0.9412 0.2860 0.048 Uiso 1 1 calc R A 3 C56 C 1.1733(9) 0.9299(9) 0.2358(4) 0.044(2) Uani 0.718(17) 1 d PD B 3 H56A H 1.2578 0.9491 0.2533 0.052 Uiso 0.718(17) 1 calc PR B 3 H56B H 1.1591 0.9958 0.2264 0.052 Uiso 0.718(17) 1 calc PR B 3 C56A C 1.1951(16) 0.883(2) 0.2443(6) 0.044(2) Uani 0.282(17) 1 d PD B 4 H56C H 1.2511 0.9581 0.2498 0.052 Uiso 0.282(17) 1 calc PR B 4 H56D H 1.2386 0.8369 0.2584 0.052 Uiso 0.282(17) 1 calc PR B 4 C57 C 1.1492(7) 0.8384(7) 0.1912(4) 0.056(2) Uani 1 1 d D . . H57A H 1.1437 0.8670 0.1610 0.068 Uiso 1 1 calc R B 3 H57B H 1.2155 0.8043 0.1922 0.068 Uiso 1 1 calc R B 3 C58 C 1.0294(7) 0.7557(6) 0.1927(3) 0.0436(17) Uani 1 1 d . B . H58A H 0.9730 0.7392 0.1614 0.052 Uiso 1 1 calc R . . H58B H 1.0426 0.6872 0.1991 0.052 Uiso 1 1 calc R . . C59 C 0.749(3) 0.346(3) 0.1368(10) 0.053(3) Uani 0.614(14) 1 d PD C 1 H59A H 0.7102 0.2682 0.1209 0.063 Uiso 0.614(14) 1 calc PR C 1 H59B H 0.7871 0.3505 0.1706 0.063 Uiso 0.614(14) 1 calc PR C 1 C60 C 0.8411(13) 0.4018(15) 0.1087(4) 0.055(3) Uani 0.614(14) 1 d PD C 1 H60A H 0.8854 0.3525 0.0949 0.066 Uiso 0.614(14) 1 calc PR C 1 H60B H 0.9002 0.4684 0.1295 0.066 Uiso 0.614(14) 1 calc PR C 1 C61 C 0.762(3) 0.429(2) 0.0688(7) 0.051(5) Uani 0.614(14) 1 d PD C 1 H61A H 0.7527 0.3789 0.0375 0.061 Uiso 0.614(14) 1 calc PR C 1 H61B H 0.7992 0.5048 0.0650 0.061 Uiso 0.614(14) 1 calc PR C 1 C62 C 0.637(4) 0.418(4) 0.0851(6) 0.029(4) Uani 0.614(14) 1 d PD C 1 H62A H 0.6104 0.4827 0.0828 0.035 Uiso 0.614(14) 1 calc PR C 1 H62B H 0.5743 0.3521 0.0652 0.035 Uiso 0.614(14) 1 calc PR C 1 C59A C 0.747(5) 0.346(5) 0.1445(14) 0.053(3) Uani 0.386(14) 1 d PD C 2 H59C H 0.7080 0.2834 0.1590 0.063 Uiso 0.386(14) 1 calc PR C 2 H59D H 0.8202 0.3926 0.1676 0.063 Uiso 0.386(14) 1 calc PR C 2 C60A C 0.781(2) 0.304(2) 0.0968(7) 0.055(3) Uani 0.386(14) 1 d PD C 2 H60C H 0.7260 0.2308 0.0809 0.066 Uiso 0.386(14) 1 calc PR C 2 H60D H 0.8657 0.3027 0.1011 0.066 Uiso 0.386(14) 1 calc PR C 2 C61A C 0.763(5) 0.389(4) 0.0683(13) 0.051(5) Uani 0.386(14) 1 d PD C 2 H61C H 0.8344 0.4554 0.0768 0.061 Uiso 0.386(14) 1 calc PR C 2 H61D H 0.7480 0.3599 0.0328 0.061 Uiso 0.386(14) 1 calc PR C 2 C62A C 0.659(6) 0.410(7) 0.0842(10) 0.029(4) Uani 0.386(14) 1 d PD C 2 H62C H 0.5845 0.3547 0.0648 0.035 Uiso 0.386(14) 1 calc PR C 2 H62D H 0.6555 0.4826 0.0790 0.035 Uiso 0.386(14) 1 calc PR C 2 O1S1 O 0.238(3) -0.128(2) 0.3975(9) 0.303(12) Uiso 1 1 d D . . C1S1 C 0.2915(19) -0.1525(16) 0.4410(7) 0.142(7) Uiso 1 1 d D . . H1S1 H 0.3764 -0.1528 0.4407 0.170 Uiso 1 1 calc R . . H1S2 H 0.2429 -0.2223 0.4475 0.170 Uiso 1 1 calc R . . C2S1 C 0.283(2) -0.0545(16) 0.4761(8) 0.165(8) Uiso 1 1 d D . . H2S1 H 0.3163 -0.0535 0.5102 0.198 Uiso 1 1 calc R . . H2S2 H 0.1991 -0.0505 0.4739 0.198 Uiso 1 1 calc R . . C3S1 C 0.365(3) 0.036(2) 0.4561(9) 0.223(12) Uiso 1 1 d D . . H3S1 H 0.3465 0.1063 0.4639 0.268 Uiso 1 1 calc R . . H3S2 H 0.4525 0.0473 0.4666 0.268 Uiso 1 1 calc R . . C4S1 C 0.320(3) -0.021(2) 0.4032(10) 0.224(13) Uiso 1 1 d D . . H4S1 H 0.2776 0.0228 0.3863 0.269 Uiso 1 1 calc R . . H4S2 H 0.3900 -0.0256 0.3875 0.269 Uiso 1 1 calc R . . O1S2 O -0.079(2) 0.153(2) -0.0561(10) 0.295(12) Uiso 1 1 d D . . C1S2 C 0.003(2) 0.263(2) -0.0484(8) 0.197(10) Uiso 1 1 d D . . H1S3 H -0.0244 0.3087 -0.0691 0.236 Uiso 1 1 calc R . . H1S4 H 0.0884 0.2656 -0.0502 0.236 Uiso 1 1 calc R . . C2S2 C -0.0216(18) 0.2857(15) 0.0042(7) 0.138(6) Uiso 1 1 d D . . H2S3 H 0.0519 0.3375 0.0258 0.165 Uiso 1 1 calc R . . H2S4 H -0.0883 0.3191 0.0050 0.165 Uiso 1 1 calc R . . C3S2 C -0.056(2) 0.1802(18) 0.0224(9) 0.189(10) Uiso 1 1 d D . . H3S3 H -0.0005 0.1846 0.0525 0.227 Uiso 1 1 calc R . . H3S4 H -0.1405 0.1621 0.0287 0.227 Uiso 1 1 calc R . . C4S2 C -0.043(3) 0.098(3) -0.0193(11) 0.279(17) Uiso 1 1 d D . . H4S3 H 0.0412 0.0946 -0.0182 0.334 Uiso 1 1 calc R . . H4S4 H -0.0997 0.0239 -0.0222 0.334 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 Lu1 0.01999(10) 0.02179(10) 0.01870(10) 0.00607(8) 0.00561(8) 0.00668(8) Lu2 0.01652(10) 0.01881(10) 0.02216(10) 0.00517(8) 0.00480(8) 0.00461(8) Lu3 0.02148(11) 0.02007(10) 0.01733(10) 0.00479(7) 0.00461(8) 0.00404(8) Si1 0.0239(7) 0.0260(7) 0.0195(7) 0.0048(6) 0.0063(6) 0.0069(6) O1 0.023(2) 0.032(2) 0.037(2) 0.0177(18) 0.0095(17) 0.0110(17) N1 0.021(2) 0.023(2) 0.018(2) 0.0054(16) 0.0036(16) 0.0061(17) C1 0.019(2) 0.021(2) 0.018(2) 0.0033(18) 0.0032(18) 0.0044(19) Si2 0.0236(8) 0.0238(7) 0.0377(9) 0.0079(6) 0.0076(7) 0.0093(6) N2 0.018(2) 0.0152(19) 0.027(2) 0.0027(16) 0.0032(17) 0.0015(16) C2 0.015(2) 0.016(2) 0.014(2) 0.0046(16) 0.0033(16) 0.0068(17) O2 0.021(2) 0.034(2) 0.045(3) 0.0111(19) 0.0145(18) 0.0081(17) Si3 0.0224(8) 0.0353(9) 0.0237(8) 0.0066(6) 0.0037(6) -0.0011(7) N3 0.024(2) 0.029(2) 0.017(2) 0.0039(18) 0.0030(17) 0.0002(19) O3 0.048(3) 0.037(2) 0.023(2) 0.0060(17) 0.0105(19) 0.023(2) C3 0.032(3) 0.020(2) 0.024(3) 0.011(2) 0.006(2) 0.004(2) C4 0.030(3) 0.025(3) 0.020(3) 0.002(2) -0.001(2) 0.005(2) C5 0.031(3) 0.024(3) 0.023(3) 0.011(2) 0.005(2) 0.010(2) C6 0.026(3) 0.044(4) 0.031(3) 0.006(3) 0.007(2) 0.011(3) C7 0.045(4) 0.045(4) 0.025(3) 0.009(3) 0.016(3) 0.020(3) C8 0.035(3) 0.029(3) 0.035(3) 0.005(2) 0.005(3) 0.010(3) C9 0.023(3) 0.025(2) 0.018(2) 0.0065(19) 0.0082(19) 0.010(2) C10 0.022(3) 0.027(3) 0.020(2) 0.006(2) 0.009(2) 0.005(2) C11 0.032(3) 0.027(3) 0.037(3) 0.013(2) 0.013(3) 0.009(2) C12 0.029(3) 0.048(4) 0.041(4) 0.026(3) 0.012(3) 0.018(3) C13 0.026(3) 0.043(4) 0.030(3) 0.016(3) 0.001(2) 0.011(3) C14 0.024(3) 0.031(3) 0.020(2) 0.006(2) 0.005(2) 0.008(2) C15 0.027(3) 0.028(3) 0.022(3) 0.006(2) 0.007(2) 0.000(2) C16 0.053(4) 0.027(3) 0.032(3) 0.000(2) 0.015(3) 0.000(3) C17 0.022(3) 0.051(4) 0.028(3) 0.001(3) 0.006(2) 0.001(3) C18 0.027(3) 0.026(3) 0.028(3) 0.003(2) -0.003(2) 0.003(2) C19 0.053(5) 0.041(4) 0.044(4) -0.009(3) 0.012(4) -0.002(3) C20 0.020(3) 0.039(4) 0.065(5) 0.012(3) -0.001(3) -0.002(3) C21 0.044(4) 0.034(3) 0.058(5) 0.015(3) 0.015(3) 0.021(3) C22 0.025(3) 0.042(4) 0.048(4) 0.011(3) 0.004(3) 0.012(3) C23 0.041(4) 0.038(4) 0.048(4) 0.013(3) 0.017(3) 0.017(3) C24 0.026(3) 0.021(2) 0.026(3) 0.009(2) 0.009(2) 0.007(2) C25 0.029(3) 0.021(3) 0.030(3) 0.007(2) 0.007(2) 0.002(2) C26 0.033(3) 0.034(3) 0.033(3) 0.007(3) 0.000(3) 0.000(3) C27 0.034(3) 0.036(3) 0.043(4) 0.007(3) 0.009(3) -0.006(3) C28 0.032(3) 0.029(3) 0.039(3) 0.016(3) 0.006(3) 0.000(2) C29 0.025(3) 0.023(3) 0.030(3) 0.006(2) 0.005(2) 0.003(2) C30 0.042(4) 0.022(3) 0.027(3) 0.005(2) 0.007(3) 0.003(2) C31 0.066(5) 0.036(4) 0.053(5) 0.012(3) 0.033(4) 0.012(4) C32 0.056(5) 0.039(4) 0.027(3) 0.003(3) -0.002(3) 0.003(3) C33 0.027(3) 0.029(3) 0.035(3) 0.011(2) 0.004(2) 0.002(2) C34 0.061(5) 0.060(5) 0.050(5) 0.029(4) 0.000(4) 0.025(4) C35 0.041(4) 0.045(4) 0.038(4) 0.012(3) 0.009(3) 0.008(3) C36 0.027(3) 0.080(6) 0.038(4) 0.003(4) 0.006(3) -0.004(4) C37 0.038(4) 0.034(3) 0.028(3) 0.007(2) 0.011(3) 0.001(3) C38 0.032(3) 0.048(4) 0.041(4) 0.014(3) 0.011(3) 0.016(3) C39 0.024(3) 0.038(3) 0.020(3) 0.003(2) 0.002(2) 0.003(2) C40 0.031(3) 0.044(4) 0.024(3) 0.008(3) 0.004(2) 0.012(3) C41 0.044(4) 0.069(5) 0.022(3) 0.010(3) 0.001(3) 0.023(4) C42 0.048(4) 0.069(5) 0.021(3) -0.004(3) 0.002(3) 0.021(4) C43 0.037(4) 0.050(4) 0.023(3) -0.006(3) -0.004(3) 0.004(3) C44 0.029(3) 0.036(3) 0.026(3) 0.002(2) 0.005(2) -0.002(3) C45 0.039(4) 0.048(4) 0.027(3) 0.015(3) 0.003(3) 0.018(3) C46 0.048(5) 0.065(5) 0.045(4) 0.019(4) 0.006(3) 0.027(4) C47 0.045(4) 0.064(5) 0.036(4) 0.023(4) 0.004(3) 0.011(4) C48 0.072(6) 0.035(4) 0.035(4) 0.013(3) 0.015(4) 0.002(4) C49 0.100(10) 0.063(7) 0.111(10) 0.031(7) 0.026(8) -0.012(7) C50 0.099(9) 0.064(6) 0.094(8) 0.041(6) 0.023(7) 0.033(6) C51 0.025(3) 0.031(3) 0.036(3) 0.012(2) 0.009(2) 0.008(2) C52 0.033(3) 0.034(3) 0.047(4) 0.019(3) 0.010(3) 0.013(3) C53 0.027(3) 0.043(4) 0.058(5) 0.021(3) 0.008(3) 0.014(3) C54 0.021(3) 0.054(4) 0.057(4) 0.031(4) 0.014(3) 0.011(3) C55 0.022(3) 0.046(4) 0.051(4) 0.014(3) 0.004(3) 0.007(3) C56 0.021(4) 0.049(6) 0.062(6) 0.027(5) 0.006(4) 0.004(4) C56A 0.021(4) 0.049(6) 0.062(6) 0.027(5) 0.006(4) 0.004(4) C57 0.039(4) 0.047(4) 0.094(7) 0.026(4) 0.043(5) 0.012(3) C58 0.036(4) 0.040(4) 0.061(5) 0.015(3) 0.025(3) 0.013(3) C59 0.079(7) 0.060(5) 0.034(9) 0.003(6) 0.007(6) 0.050(5) C60 0.048(7) 0.097(10) 0.034(5) 0.004(6) 0.007(5) 0.049(7) C61 0.044(5) 0.093(19) 0.033(4) 0.014(9) 0.016(4) 0.043(13) C62 0.029(15) 0.043(8) 0.023(3) 0.005(3) 0.010(3) 0.023(8) C59A 0.079(7) 0.060(5) 0.034(9) 0.003(6) 0.007(6) 0.050(5) C60A 0.048(7) 0.097(10) 0.034(5) 0.004(6) 0.007(5) 0.049(7) C61A 0.044(5) 0.093(19) 0.033(4) 0.014(9) 0.016(4) 0.043(13) C62A 0.029(15) 0.043(8) 0.023(3) 0.005(3) 0.010(3) 0.023(8) _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 Lu1 N1 2.233(4) . ? Lu1 C1 2.383(5) . ? Lu1 O1 2.420(4) . ? Lu1 C2 2.751(5) . ? Lu1 Lu2 3.2785(3) . ? Lu1 Lu3 3.2821(4) . ? Lu1 H1A 2.44(6) . ? Lu2 N2 2.241(4) . ? Lu2 O2 2.414(4) . ? Lu2 C2 2.736(5) . ? Lu2 Lu3 3.2036(3) . ? Lu2 H1B 2.48(5) . ? Lu2 H2B 2.50(6) . ? Lu3 N3 2.255(5) . ? Lu3 C1 2.310(5) . ? Lu3 O3 2.391(4) . ? Lu3 C2 2.723(5) . ? Lu3 H1A 2.31(6) . ? Si1 N1 1.734(5) . ? Si1 C8 1.872(7) . ? Si1 C6 1.876(6) . ? Si1 C7 1.883(6) . ? O1 C51 1.459(7) . ? O1 C54 1.461(7) . ? N1 C9 1.426(7) . ? C1 H1A 0.978(19) . ? C1 H1B 0.978(19) . ? Si2 N2 1.731(5) . ? Si2 C22 1.879(7) . ? Si2 C23 1.880(7) . ? Si2 C21 1.884(7) . ? N2 C24 1.435(7) . ? C2 H2A 0.972(18) . ? C2 H2B 0.968(18) . ? C2 H2C 0.967(18) . ? O2 C58 1.457(8) . ? O2 C55 1.465(8) . ? Si3 N3 1.730(5) . ? Si3 C37 1.876(7) . ? Si3 C36 1.881(7) . ? Si3 C38 1.883(8) . ? N3 C39 1.427(7) . ? O3 C62A 1.453(14) . ? O3 C59 1.454(11) . ? O3 C59A 1.456(14) . ? O3 C62 1.456(11) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? 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 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C14 1.420(8) . ? C9 C10 1.423(8) . ? C10 C11 1.406(8) . ? C10 C15 1.517(8) . ? C11 C12 1.377(9) . ? C11 H11A 0.9500 . ? C12 C13 1.380(10) . ? C12 H12A 0.9500 . ? C13 C14 1.401(8) . ? C13 H13A 0.9500 . ? C14 C18 1.533(8) . ? C15 C16 1.534(9) . ? C15 C17 1.539(8) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.524(9) . ? C18 C19 1.537(10) . ? C18 H18A 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.414(8) . ? C24 C29 1.414(8) . ? C25 C26 1.413(8) . ? C25 C30 1.516(8) . ? C26 C27 1.369(9) . ? C26 H26A 0.9500 . ? C27 C28 1.369(10) . ? C27 H27A 0.9500 . ? C28 C29 1.394(8) . ? C28 H28A 0.9500 . ? C29 C33 1.520(9) . ? C30 C32 1.543(10) . ? C30 C31 1.547(10) . ? C30 H30A 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.513(10) . ? C33 C34 1.538(9) . ? C33 H33A 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? 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 C44 1.428(9) . ? C39 C40 1.433(9) . ? C40 C41 1.405(9) . ? C40 C45 1.510(10) . ? C41 C42 1.393(12) . ? C41 H41A 0.9500 . ? C42 C43 1.370(11) . ? C42 H42A 0.9500 . ? C43 C44 1.395(9) . ? C43 H43A 0.9500 . ? C44 C48 1.514(10) . ? C45 C46 1.538(10) . ? C45 C47 1.538(10) . ? C45 H45A 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.467(14) . ? C48 C50 1.492(14) . ? C48 H48A 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.526(9) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.525(9) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.536(9) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.517(10) . ? C55 C56A 1.519(15) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.528(12) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C56A C57 1.494(15) . ? C56A H56C 0.9900 . ? C56A H56D 0.9900 . ? C57 C58 1.522(10) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.51(2) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.522(18) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.55(4) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C59A C60A 1.51(2) . ? C59A H59C 0.9900 . ? C59A H59D 0.9900 . ? C60A C61A 1.51(2) . ? C60A H60C 0.9900 . ? C60A H60D 0.9900 . ? C61A C62A 1.43(6) . ? C61A H61C 0.9900 . ? C61A H61D 0.9900 . ? C62A H62C 0.9900 . ? C62A H62D 0.9900 . ? O1S1 C4S1 1.427(19) . ? O1S1 C1S1 1.434(18) . ? C1S1 C2S1 1.518(16) . ? C1S1 H1S1 0.9900 . ? C1S1 H1S2 0.9900 . ? C2S1 C3S1 1.538(17) . ? C2S1 H2S1 0.9900 . ? C2S1 H2S2 0.9900 . ? C3S1 C4S1 1.520(17) . ? C3S1 H3S1 0.9900 . ? C3S1 H3S2 0.9900 . ? C4S1 H4S1 0.9900 . ? C4S1 H4S2 0.9900 . ? O1S2 C4S2 1.45(2) . ? O1S2 C1S2 1.454(19) . ? C1S2 C2S2 1.549(16) . ? C1S2 H1S3 0.9900 . ? C1S2 H1S4 0.9900 . ? C2S2 C3S2 1.518(16) . ? C2S2 H2S3 0.9900 . ? C2S2 H2S4 0.9900 . ? C3S2 C4S2 1.513(17) . ? C3S2 H3S3 0.9900 . ? C3S2 H3S4 0.9900 . ? C4S2 H4S3 0.9900 . ? C4S2 H4S4 0.9900 . ? 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 Lu1 C1 99.99(17) . . ? N1 Lu1 O1 101.08(15) . . ? C1 Lu1 O1 158.81(16) . . ? N1 Lu1 C2 177.81(15) . . ? C1 Lu1 C2 81.85(16) . . ? O1 Lu1 C2 77.04(14) . . ? N1 Lu1 Lu2 127.58(12) . . ? C1 Lu1 Lu2 44.78(13) . . ? O1 Lu1 Lu2 117.65(10) . . ? C2 Lu1 Lu2 53.10(10) . . ? N1 Lu1 Lu3 129.42(12) . . ? C1 Lu1 Lu3 44.72(12) . . ? O1 Lu1 Lu3 119.66(11) . . ? C2 Lu1 Lu3 52.77(10) . . ? Lu2 Lu1 Lu3 58.460(7) . . ? N1 Lu1 C5 140.66(14) . . ? C1 Lu1 C5 40.71(14) . . ? O1 Lu1 C5 118.14(12) . . ? C2 Lu1 C5 41.15(12) . . ? Lu2 Lu1 C5 29.28(7) . . ? Lu3 Lu1 C5 30.01(7) . . ? N1 Lu1 H1A 87.8(13) . . ? C1 Lu1 H1A 23.4(5) . . ? O1 Lu1 H1A 160.4(11) . . ? C2 Lu1 H1A 94.3(12) . . ? Lu2 Lu1 H1A 67.6(6) . . ? Lu3 Lu1 H1A 44.7(14) . . ? C5 Lu1 H1A 56.2(11) . . ? N2 Lu2 O2 98.41(16) . . ? O2 Lu2 C2 76.93(15) . . ? N2 Lu2 Lu3 128.72(12) . . ? O2 Lu2 Lu3 119.34(11) . . ? C2 Lu2 Lu3 53.87(10) . . ? N2 Lu2 Lu1 131.05(12) . . ? O2 Lu2 Lu1 117.61(11) . . ? C2 Lu2 Lu1 53.52(10) . . ? Lu3 Lu2 Lu1 60.827(8) . . ? N2 Lu2 C3 142.92(14) . . ? O2 Lu2 C3 118.65(13) . . ? C2 Lu2 C3 41.73(13) . . ? Lu3 Lu2 C3 30.41(7) . . ? Lu1 Lu2 C3 31.13(7) . . ? N2 Lu2 H1B 78.1(6) . . ? O2 Lu2 H1B 175.5(9) . . ? C2 Lu2 H1B 106.7(6) . . ? Lu3 Lu2 H1B 65.2(9) . . ? Lu1 Lu2 H1B 63.8(10) . . ? C3 Lu2 H1B 65.0(6) . . ? N2 Lu2 H2B 156.2(5) . . ? O2 Lu2 H2B 60.7(8) . . ? Lu1 Lu2 H2B 60.8(10) . . ? C3 Lu2 H2B 59.4(7) . . ? H1B Lu2 H2B 122.1(11) . . ? N3 Lu3 C1 102.51(18) . . ? N3 Lu3 O3 94.19(17) . . ? C1 Lu3 O3 162.86(18) . . ? N3 Lu3 C2 172.23(16) . . ? C1 Lu3 C2 83.79(16) . . ? O3 Lu3 C2 79.90(15) . . ? N3 Lu3 Lu2 133.50(13) . . ? C1 Lu3 Lu2 46.10(13) . . ? O3 Lu3 Lu2 118.22(12) . . ? C2 Lu3 Lu2 54.26(10) . . ? N3 Lu3 Lu1 128.18(12) . . ? C1 Lu3 Lu1 46.55(13) . . ? O3 Lu3 Lu1 123.80(10) . . ? C2 Lu3 Lu1 53.55(10) . . ? Lu2 Lu3 Lu1 60.713(7) . . ? N3 Lu3 C4 143.27(15) . . ? C1 Lu3 C4 40.96(15) . . ? O3 Lu3 C4 122.53(14) . . ? C2 Lu3 C4 42.83(13) . . ? Lu2 Lu3 C4 30.72(7) . . ? Lu1 Lu3 C4 30.49(7) . . ? N3 Lu3 H1A 86.4(12) . . ? C1 Lu3 H1A 24.4(5) . . ? O3 Lu3 H1A 165.5(10) . . ? C2 Lu3 H1A 98.1(13) . . ? Lu2 Lu3 H1A 70.3(6) . . ? Lu1 Lu3 H1A 48.0(15) . . ? C4 Lu3 H1A 58.0(11) . . ? N1 Si1 C8 111.7(3) . . ? N1 Si1 C6 113.5(3) . . ? C8 Si1 C6 105.9(3) . . ? N1 Si1 C7 112.0(3) . . ? C8 Si1 C7 107.8(3) . . ? C6 Si1 C7 105.6(3) . . ? C51 O1 C54 105.6(5) . . ? C51 O1 Lu1 122.8(3) . . ? C54 O1 Lu1 130.2(4) . . ? C9 N1 Si1 118.3(3) . . ? C9 N1 Lu1 112.9(3) . . ? Si1 N1 Lu1 128.4(2) . . ? Lu3 C1 Lu1 88.73(18) . . ? Lu3 C1 H1A 78(3) . . ? Lu1 C1 H1A 82(4) . . ? Lu3 C1 H1B 140(4) . . ? Lu1 C1 H1B 131(4) . . ? H1A C1 H1B 109(3) . . ? N2 Si2 C22 111.1(3) . . ? N2 Si2 C23 114.2(3) . . ? C22 Si2 C23 106.2(3) . . ? N2 Si2 C21 111.9(3) . . ? C22 Si2 C21 107.0(3) . . ? C23 Si2 C21 106.1(3) . . ? C24 N2 Si2 118.7(4) . . ? C24 N2 Lu2 114.8(3) . . ? Si2 N2 Lu2 126.3(2) . . ? Lu3 C2 Lu2 71.87(11) . . ? Lu3 C2 Lu1 73.68(12) . . ? Lu2 C2 Lu1 73.38(12) . . ? Lu3 C2 H2A 105(3) . . ? Lu2 C2 H2A 144(3) . . ? Lu1 C2 H2A 71(3) . . ? Lu3 C2 H2B 138(3) . . ? Lu2 C2 H2B 66(3) . . ? Lu1 C2 H2B 95(3) . . ? H2A C2 H2B 110(3) . . ? Lu3 C2 H2C 76(3) . . ? Lu2 C2 H2C 103(3) . . ? Lu1 C2 H2C 149(3) . . ? H2A C2 H2C 111(3) . . ? H2B C2 H2C 111(3) . . ? C58 O2 C55 107.2(5) . . ? C58 O2 Lu2 128.6(4) . . ? C55 O2 Lu2 122.5(4) . . ? N3 Si3 C37 112.0(3) . . ? N3 Si3 C36 112.5(3) . . ? C37 Si3 C36 106.2(4) . . ? N3 Si3 C38 114.2(3) . . ? C37 Si3 C38 106.7(3) . . ? C36 Si3 C38 104.6(4) . . ? C39 N3 Si3 116.1(4) . . ? C39 N3 Lu3 118.1(4) . . ? Si3 N3 Lu3 125.7(2) . . ? C62A O3 C59 94(2) . . ? C62A O3 C59A 103(2) . . ? C59 O3 C62 105.8(12) . . ? C59A O3 C62 114.6(16) . . ? C62A O3 Lu3 132(2) . . ? C59 O3 Lu3 131.1(11) . . ? C59A O3 Lu3 122.7(15) . . ? C62 O3 Lu3 121.7(12) . . ? Lu2 C3 H3A 109.5 . . ? Lu2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Lu2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Lu3 C4 H4A 109.5 . . ? Lu3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Lu3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Lu1 C5 H5A 109.5 . . ? Lu1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Lu1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 118.5(5) . . ? C14 C9 N1 120.8(5) . . ? C10 C9 N1 120.7(5) . . ? C11 C10 C9 119.3(5) . . ? C11 C10 C15 119.1(5) . . ? C9 C10 C15 121.6(5) . . ? C12 C11 C10 121.4(6) . . ? C12 C11 H11A 119.3 . . ? C10 C11 H11A 119.3 . . ? C11 C12 C13 119.7(6) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? C12 C13 C14 121.2(6) . . ? C12 C13 H13A 119.4 . . ? C14 C13 H13A 119.4 . . ? C13 C14 C9 119.8(5) . . ? C13 C14 C18 118.8(5) . . ? C9 C14 C18 121.4(5) . . ? C10 C15 C16 113.2(6) . . ? C10 C15 C17 109.6(5) . . ? C16 C15 C17 109.5(5) . . ? C10 C15 H15A 108.1 . . ? C16 C15 H15A 108.1 . . ? C17 C15 H15A 108.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C14 113.5(5) . . ? C20 C18 C19 109.8(6) . . ? C14 C18 C19 110.6(5) . . ? C20 C18 H18A 107.5 . . ? C14 C18 H18A 107.5 . . ? C19 C18 H18A 107.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 119.5(5) . . ? C25 C24 N2 119.3(5) . . ? C29 C24 N2 121.2(5) . . ? C26 C25 C24 118.4(5) . . ? C26 C25 C30 118.7(6) . . ? C24 C25 C30 122.9(5) . . ? C27 C26 C25 121.4(6) . . ? C27 C26 H26A 119.3 . . ? C25 C26 H26A 119.3 . . ? C28 C27 C26 119.7(6) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C27 C28 C29 121.9(6) . . ? C27 C28 H28A 119.1 . . ? C29 C28 H28A 119.1 . . ? C28 C29 C24 118.8(6) . . ? C28 C29 C33 118.4(5) . . ? C24 C29 C33 122.7(5) . . ? C25 C30 C32 114.0(6) . . ? C25 C30 C31 109.9(5) . . ? C32 C30 C31 109.2(6) . . ? C25 C30 H30A 107.8 . . ? C32 C30 H30A 107.8 . . ? C31 C30 H30A 107.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C33 C29 114.1(6) . . ? C35 C33 C34 107.9(6) . . ? C29 C33 C34 111.4(6) . . ? C35 C33 H33A 107.7 . . ? C29 C33 H33A 107.7 . . ? C34 C33 H33A 107.7 . . ? 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 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si3 C36 H36A 109.5 . . ? Si3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si3 C37 H37A 109.5 . . ? Si3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si3 C38 H38A 109.5 . . ? Si3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N3 C39 C44 121.0(5) . . ? N3 C39 C40 120.5(6) . . ? C44 C39 C40 118.5(6) . . ? C41 C40 C39 119.3(7) . . ? C41 C40 C45 118.8(6) . . ? C39 C40 C45 121.9(6) . . ? C42 C41 C40 121.2(7) . . ? C42 C41 H41A 119.4 . . ? C40 C41 H41A 119.4 . . ? C43 C42 C41 119.3(6) . . ? C43 C42 H42A 120.4 . . ? C41 C42 H42A 120.4 . . ? C42 C43 C44 122.6(7) . . ? C42 C43 H43A 118.7 . . ? C44 C43 H43A 118.7 . . ? C43 C44 C39 119.0(6) . . ? C43 C44 C48 117.9(7) . . ? C39 C44 C48 123.0(6) . . ? C40 C45 C46 110.7(6) . . ? C40 C45 C47 113.1(6) . . ? C46 C45 C47 109.1(6) . . ? C40 C45 H45A 107.9 . . ? C46 C45 H45A 107.9 . . ? C47 C45 H45A 107.9 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C50 108.6(9) . . ? C49 C48 C44 114.8(9) . . ? C50 C48 C44 113.2(7) . . ? C49 C48 H48A 106.6 . . ? C50 C48 H48A 106.6 . . ? C44 C48 H48A 106.6 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O1 C51 C52 103.8(5) . . ? O1 C51 H51A 111.0 . . ? C52 C51 H51A 111.0 . . ? O1 C51 H51B 111.0 . . ? C52 C51 H51B 111.0 . . ? H51A C51 H51B 109.0 . . ? C53 C52 C51 103.5(5) . . ? C53 C52 H52A 111.1 . . ? C51 C52 H52A 111.1 . . ? C53 C52 H52B 111.1 . . ? C51 C52 H52B 111.1 . . ? H52A C52 H52B 109.0 . . ? C52 C53 C54 105.2(5) . . ? C52 C53 H53A 110.7 . . ? C54 C53 H53A 110.7 . . ? C52 C53 H53B 110.7 . . ? C54 C53 H53B 110.7 . . ? H53A C53 H53B 108.8 . . ? O1 C54 C53 106.2(5) . . ? O1 C54 H54A 110.5 . . ? C53 C54 H54A 110.5 . . ? O1 C54 H54B 110.5 . . ? C53 C54 H54B 110.5 . . ? H54A C54 H54B 108.7 . . ? O2 C55 C56 104.5(6) . . ? O2 C55 C56A 105.9(9) . . ? O2 C55 H55A 110.9 . . ? C56 C55 H55A 110.9 . . ? C56A C55 H55A 83.0 . . ? O2 C55 H55B 110.9 . . ? C56 C55 H55B 110.9 . . ? C56A C55 H55B 133.2 . . ? H55A C55 H55B 108.9 . . ? C55 C56 C57 104.1(7) . . ? C55 C56 H56A 110.9 . . ? C57 C56 H56A 110.9 . . ? C55 C56 H56B 110.9 . . ? C57 C56 H56B 110.9 . . ? H56A C56 H56B 108.9 . . ? C57 C56A C55 105.7(11) . . ? C57 C56A H56C 110.6 . . ? C55 C56A H56C 110.6 . . ? C57 C56A H56D 110.6 . . ? C55 C56A H56D 110.6 . . ? H56C C56A H56D 108.7 . . ? C56A C57 C58 100.4(10) . . ? C58 C57 C56 106.4(6) . . ? C56A C57 H57A 137.4 . . ? C58 C57 H57A 110.5 . . ? C56 C57 H57A 110.5 . . ? C56A C57 H57B 86.0 . . ? C58 C57 H57B 110.5 . . ? C56 C57 H57B 110.5 . . ? H57A C57 H57B 108.6 . . ? O2 C58 C57 105.8(6) . . ? O2 C58 H58A 110.6 . . ? C57 C58 H58A 110.6 . . ? O2 C58 H58B 110.6 . . ? C57 C58 H58B 110.6 . . ? H58A C58 H58B 108.7 . . ? O3 C59 C60 102.5(13) . . ? O3 C59 H59A 111.3 . . ? C60 C59 H59A 111.3 . . ? O3 C59 H59B 111.3 . . ? C60 C59 H59B 111.3 . . ? H59A C59 H59B 109.2 . . ? C59 C60 C61 102.6(17) . . ? C59 C60 H60A 111.2 . . ? C61 C60 H60A 111.2 . . ? C59 C60 H60B 111.2 . . ? C61 C60 H60B 111.2 . . ? H60A C60 H60B 109.2 . . ? C60 C61 C62 106.2(15) . . ? C60 C61 H61A 110.5 . . ? C62 C61 H61A 110.5 . . ? C60 C61 H61B 110.5 . . ? C62 C61 H61B 110.5 . . ? H61A C61 H61B 108.7 . . ? O3 C62 C61 102.6(18) . . ? O3 C62 H62A 111.3 . . ? C61 C62 H62A 111.3 . . ? O3 C62 H62B 111.3 . . ? C61 C62 H62B 111.3 . . ? H62A C62 H62B 109.2 . . ? O3 C59A C60A 108.4(18) . . ? O3 C59A H59C 110.0 . . ? C60A C59A H59C 110.0 . . ? O3 C59A H59D 110.0 . . ? C60A C59A H59D 110.0 . . ? H59C C59A H59D 108.4 . . ? C59A C60A C61A 101(3) . . ? C59A C60A H60C 111.5 . . ? C61A C60A H60C 111.5 . . ? C59A C60A H60D 111.5 . . ? C61A C60A H60D 111.5 . . ? H60C C60A H60D 109.3 . . ? C62A C61A C60A 101(4) . . ? C62A C61A H61C 111.6 . . ? C60A C61A H61C 111.6 . . ? C62A C61A H61D 111.6 . . ? C60A C61A H61D 111.6 . . ? H61C C61A H61D 109.4 . . ? C61A C62A O3 110(3) . . ? C61A C62A H62C 109.6 . . ? O3 C62A H62C 109.6 . . ? C61A C62A H62D 109.6 . . ? O3 C62A H62D 109.6 . . ? H62C C62A H62D 108.1 . . ? C4S1 O1S1 C1S1 97(2) . . ? O1S1 C1S1 C2S1 97.1(18) . . ? O1S1 C1S1 H1S1 112.3 . . ? C2S1 C1S1 H1S1 112.3 . . ? O1S1 C1S1 H1S2 112.3 . . ? C2S1 C1S1 H1S2 112.3 . . ? H1S1 C1S1 H1S2 109.9 . . ? C1S1 C2S1 C3S1 98.9(18) . . ? C1S1 C2S1 H2S1 112.0 . . ? C3S1 C2S1 H2S1 112.0 . . ? C1S1 C2S1 H2S2 112.0 . . ? C3S1 C2S1 H2S2 112.0 . . ? H2S1 C2S1 H2S2 109.7 . . ? C4S1 C3S1 C2S1 95(2) . . ? C4S1 C3S1 H3S1 112.8 . . ? C2S1 C3S1 H3S1 112.8 . . ? C4S1 C3S1 H3S2 112.8 . . ? C2S1 C3S1 H3S2 112.8 . . ? H3S1 C3S1 H3S2 110.2 . . ? O1S1 C4S1 C3S1 113(2) . . ? O1S1 C4S1 H4S1 109.0 . . ? C3S1 C4S1 H4S1 109.0 . . ? O1S1 C4S1 H4S2 109.0 . . ? C3S1 C4S1 H4S2 109.0 . . ? H4S1 C4S1 H4S2 107.8 . . ? C4S2 O1S2 C1S2 110(3) . . ? O1S2 C1S2 C2S2 89.4(18) . . ? O1S2 C1S2 H1S3 113.7 . . ? C2S2 C1S2 H1S3 113.7 . . ? O1S2 C1S2 H1S4 113.7 . . ? C2S2 C1S2 H1S4 113.7 . . ? H1S3 C1S2 H1S4 111.0 . . ? C3S2 C2S2 C1S2 110.1(18) . . ? C3S2 C2S2 H2S3 109.6 . . ? C1S2 C2S2 H2S3 109.6 . . ? C3S2 C2S2 H2S4 109.6 . . ? C1S2 C2S2 H2S4 109.6 . . ? H2S3 C2S2 H2S4 108.1 . . ? C4S2 C3S2 C2S2 103(2) . . ? C4S2 C3S2 H3S3 111.2 . . ? C2S2 C3S2 H3S3 111.2 . . ? C4S2 C3S2 H3S4 111.2 . . ? C2S2 C3S2 H3S4 111.2 . . ? H3S3 C3S2 H3S4 109.1 . . ? O1S2 C4S2 C3S2 94(2) . . ? O1S2 C4S2 H4S3 112.9 . . ? C3S2 C4S2 H4S3 112.9 . . ? O1S2 C4S2 H4S4 112.9 . . ? C3S2 C4S2 H4S4 112.9 . . ? H4S3 C4S2 H4S4 110.4 . . ? 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 N1 Lu1 Lu2 N2 -0.3(2) . . . . ? C1 Lu1 Lu2 N2 62.0(2) . . . . ? O1 Lu1 Lu2 N2 -132.9(2) . . . . ? C2 Lu1 Lu2 N2 -177.6(2) . . . . ? Lu3 Lu1 Lu2 N2 117.63(15) . . . . ? C5 Lu1 Lu2 N2 128.3(2) . . . . ? N1 Lu1 Lu2 O2 132.15(19) . . . . ? C1 Lu1 Lu2 O2 -165.5(2) . . . . ? O1 Lu1 Lu2 O2 -0.45(18) . . . . ? C2 Lu1 Lu2 O2 -45.23(18) . . . . ? Lu3 Lu1 Lu2 O2 -109.96(13) . . . . ? C5 Lu1 Lu2 O2 -99.33(19) . . . . ? N1 Lu1 Lu2 C2 177.38(19) . . . . ? C1 Lu1 Lu2 C2 -120.3(2) . . . . ? O1 Lu1 Lu2 C2 44.78(18) . . . . ? Lu3 Lu1 Lu2 C2 -64.73(12) . . . . ? C5 Lu1 Lu2 C2 -54.10(19) . . . . ? N1 Lu1 Lu2 Lu3 -117.89(15) . . . . ? C1 Lu1 Lu2 Lu3 -55.58(18) . . . . ? O1 Lu1 Lu2 Lu3 109.51(12) . . . . ? C2 Lu1 Lu2 Lu3 64.73(12) . . . . ? C5 Lu1 Lu2 Lu3 10.63(15) . . . . ? N1 Lu1 Lu2 C3 -127.4(2) . . . . ? C1 Lu1 Lu2 C3 -65.1(2) . . . . ? O1 Lu1 Lu2 C3 99.97(19) . . . . ? C2 Lu1 Lu2 C3 55.18(19) . . . . ? Lu3 Lu1 Lu2 C3 -9.55(15) . . . . ? C5 Lu1 Lu2 C3 1.1(2) . . . . ? N2 Lu2 Lu3 N3 -4.7(2) . . . . ? O2 Lu2 Lu3 N3 -136.4(2) . . . . ? C2 Lu2 Lu3 N3 -179.4(2) . . . . ? Lu1 Lu2 Lu3 N3 116.41(16) . . . . ? C3 Lu2 Lu3 N3 126.2(2) . . . . ? N2 Lu2 Lu3 C1 -64.8(2) . . . . ? O2 Lu2 Lu3 C1 163.5(2) . . . . ? C2 Lu2 Lu3 C1 120.5(2) . . . . ? Lu1 Lu2 Lu3 C1 56.32(18) . . . . ? C3 Lu2 Lu3 C1 66.1(2) . . . . ? N2 Lu2 Lu3 O3 123.89(19) . . . . ? O2 Lu2 Lu3 O3 -7.86(17) . . . . ? C2 Lu2 Lu3 O3 -50.84(16) . . . . ? Lu1 Lu2 Lu3 O3 -115.02(11) . . . . ? C3 Lu2 Lu3 O3 -105.27(19) . . . . ? N2 Lu2 Lu3 C2 174.73(19) . . . . ? O2 Lu2 Lu3 C2 42.98(17) . . . . ? Lu1 Lu2 Lu3 C2 -64.18(12) . . . . ? C3 Lu2 Lu3 C2 -54.42(19) . . . . ? N2 Lu2 Lu3 Lu1 -121.09(15) . . . . ? O2 Lu2 Lu3 Lu1 107.16(13) . . . . ? C2 Lu2 Lu3 Lu1 64.18(12) . . . . ? C3 Lu2 Lu3 Lu1 9.75(15) . . . . ? N2 Lu2 Lu3 C4 -129.2(2) . . . . ? O2 Lu2 Lu3 C4 99.1(2) . . . . ? C2 Lu2 Lu3 C4 56.11(19) . . . . ? Lu1 Lu2 Lu3 C4 -8.06(15) . . . . ? C3 Lu2 Lu3 C4 1.7(2) . . . . ? N1 Lu1 Lu3 N3 -9.3(2) . . . . ? C1 Lu1 Lu3 N3 -68.6(2) . . . . ? O1 Lu1 Lu3 N3 129.7(2) . . . . ? C2 Lu1 Lu3 N3 170.5(2) . . . . ? Lu2 Lu1 Lu3 N3 -124.26(17) . . . . ? C5 Lu1 Lu3 N3 -134.7(2) . . . . ? N1 Lu1 Lu3 C1 59.3(2) . . . . ? O1 Lu1 Lu3 C1 -161.8(2) . . . . ? C2 Lu1 Lu3 C1 -121.0(2) . . . . ? Lu2 Lu1 Lu3 C1 -55.68(18) . . . . ? C5 Lu1 Lu3 C1 -66.1(2) . . . . ? N1 Lu1 Lu3 O3 -139.0(2) . . . . ? C1 Lu1 Lu3 O3 161.8(2) . . . . ? O1 Lu1 Lu3 O3 0.00(18) . . . . ? C2 Lu1 Lu3 O3 40.81(19) . . . . ? Lu2 Lu1 Lu3 O3 106.08(14) . . . . ? C5 Lu1 Lu3 O3 95.7(2) . . . . ? N1 Lu1 Lu3 C2 -179.78(19) . . . . ? C1 Lu1 Lu3 C2 121.0(2) . . . . ? O1 Lu1 Lu3 C2 -40.81(17) . . . . ? Lu2 Lu1 Lu3 C2 65.27(12) . . . . ? C5 Lu1 Lu3 C2 54.88(19) . . . . ? N1 Lu1 Lu3 Lu2 114.95(15) . . . . ? C1 Lu1 Lu3 Lu2 55.68(18) . . . . ? O1 Lu1 Lu3 Lu2 -106.08(11) . . . . ? C2 Lu1 Lu3 Lu2 -65.27(12) . . . . ? C5 Lu1 Lu3 Lu2 -10.39(14) . . . . ? N1 Lu1 Lu3 C4 123.1(2) . . . . ? C1 Lu1 Lu3 C4 63.8(2) . . . . ? O1 Lu1 Lu3 C4 -97.96(19) . . . . ? C2 Lu1 Lu3 C4 -57.2(2) . . . . ? Lu2 Lu1 Lu3 C4 8.12(15) . . . . ? C5 Lu1 Lu3 C4 -2.3(2) . . . . ? N1 Lu1 O1 C51 58.8(4) . . . . ? C1 Lu1 O1 C51 -127.6(5) . . . . ? C2 Lu1 O1 C51 -122.3(4) . . . . ? Lu2 Lu1 O1 C51 -157.7(4) . . . . ? Lu3 Lu1 O1 C51 -90.1(4) . . . . ? C5 Lu1 O1 C51 -124.4(4) . . . . ? N1 Lu1 O1 C54 -136.4(6) . . . . ? C1 Lu1 O1 C54 37.2(8) . . . . ? C2 Lu1 O1 C54 42.4(6) . . . . ? Lu2 Lu1 O1 C54 7.1(6) . . . . ? Lu3 Lu1 O1 C54 74.7(6) . . . . ? C5 Lu1 O1 C54 40.3(6) . . . . ? C8 Si1 N1 C9 119.0(4) . . . . ? C6 Si1 N1 C9 -121.4(4) . . . . ? C7 Si1 N1 C9 -2.0(5) . . . . ? C8 Si1 N1 Lu1 -52.9(4) . . . . ? C6 Si1 N1 Lu1 66.8(4) . . . . ? C7 Si1 N1 Lu1 -173.9(3) . . . . ? C1 Lu1 N1 C9 165.8(4) . . . . ? O1 Lu1 N1 C9 -16.6(4) . . . . ? Lu2 Lu1 N1 C9 -154.9(3) . . . . ? Lu3 Lu1 N1 C9 127.9(3) . . . . ? C5 Lu1 N1 C9 167.9(3) . . . . ? C1 Lu1 N1 Si1 -22.0(3) . . . . ? O1 Lu1 N1 Si1 155.7(3) . . . . ? Lu2 Lu1 N1 Si1 17.3(4) . . . . ? Lu3 Lu1 N1 Si1 -59.9(3) . . . . ? C5 Lu1 N1 Si1 -19.8(4) . . . . ? N3 Lu3 C1 Lu1 131.44(16) . . . . ? O3 Lu3 C1 Lu1 -61.9(6) . . . . ? C2 Lu3 C1 Lu1 -43.94(15) . . . . ? Lu2 Lu3 C1 Lu1 -88.65(17) . . . . ? C4 Lu3 C1 Lu1 -43.99(15) . . . . ? N1 Lu1 C1 Lu3 -137.60(16) . . . . ? O1 Lu1 C1 Lu3 48.8(5) . . . . ? C2 Lu1 C1 Lu3 43.61(15) . . . . ? Lu2 Lu1 C1 Lu3 87.83(17) . . . . ? C5 Lu1 C1 Lu3 44.50(15) . . . . ? C22 Si2 N2 C24 127.7(4) . . . . ? C23 Si2 N2 C24 -112.3(5) . . . . ? C21 Si2 N2 C24 8.2(5) . . . . ? C22 Si2 N2 Lu2 -47.3(4) . . . . ? C23 Si2 N2 Lu2 72.7(4) . . . . ? C21 Si2 N2 Lu2 -166.8(3) . . . . ? O2 Lu2 N2 C24 -23.1(4) . . . . ? Lu3 Lu2 N2 C24 -162.0(3) . . . . ? Lu1 Lu2 N2 C24 115.5(3) . . . . ? C3 Lu2 N2 C24 158.6(3) . . . . ? O2 Lu2 N2 Si2 152.1(3) . . . . ? Lu3 Lu2 N2 Si2 13.2(4) . . . . ? Lu1 Lu2 N2 Si2 -69.3(3) . . . . ? C3 Lu2 N2 Si2 -26.2(4) . . . . ? C1 Lu3 C2 Lu2 -38.65(14) . . . . ? O3 Lu3 C2 Lu2 136.05(14) . . . . ? Lu1 Lu3 C2 Lu2 -77.42(9) . . . . ? C4 Lu3 C2 Lu2 -38.60(13) . . . . ? C1 Lu3 C2 Lu1 38.78(14) . . . . ? O3 Lu3 C2 Lu1 -146.52(14) . . . . ? Lu2 Lu3 C2 Lu1 77.42(9) . . . . ? C4 Lu3 C2 Lu1 38.83(13) . . . . ? O2 Lu2 C2 Lu3 -142.40(15) . . . . ? Lu1 Lu2 C2 Lu3 77.83(9) . . . . ? C3 Lu2 C2 Lu3 38.21(13) . . . . ? O2 Lu2 C2 Lu1 139.77(15) . . . . ? Lu3 Lu2 C2 Lu1 -77.83(9) . . . . ? C3 Lu2 C2 Lu1 -39.62(13) . . . . ? C1 Lu1 C2 Lu3 -37.56(14) . . . . ? O1 Lu1 C2 Lu3 144.35(14) . . . . ? Lu2 Lu1 C2 Lu3 -75.46(9) . . . . ? C5 Lu1 C2 Lu3 -38.44(13) . . . . ? C1 Lu1 C2 Lu2 37.90(14) . . . . ? O1 Lu1 C2 Lu2 -140.18(14) . . . . ? Lu3 Lu1 C2 Lu2 75.46(9) . . . . ? C5 Lu1 C2 Lu2 37.02(13) . . . . ? N2 Lu2 O2 C58 -131.5(5) . . . . ? C2 Lu2 O2 C58 46.8(5) . . . . ? Lu3 Lu2 O2 C58 12.4(6) . . . . ? Lu1 Lu2 O2 C58 82.7(5) . . . . ? C3 Lu2 O2 C58 47.3(6) . . . . ? N2 Lu2 O2 C55 65.4(5) . . . . ? C2 Lu2 O2 C55 -116.3(5) . . . . ? Lu3 Lu2 O2 C55 -150.7(4) . . . . ? Lu1 Lu2 O2 C55 -80.4(5) . . . . ? C3 Lu2 O2 C55 -115.8(4) . . . . ? C37 Si3 N3 C39 122.4(5) . . . . ? C36 Si3 N3 C39 2.9(6) . . . . ? C38 Si3 N3 C39 -116.2(5) . . . . ? C37 Si3 N3 Lu3 -53.4(4) . . . . ? C36 Si3 N3 Lu3 -173.0(4) . . . . ? C38 Si3 N3 Lu3 68.0(4) . . . . ? C1 Lu3 N3 C39 160.9(4) . . . . ? O3 Lu3 N3 C39 -15.2(4) . . . . ? Lu2 Lu3 N3 C39 121.1(4) . . . . ? Lu1 Lu3 N3 C39 -155.3(4) . . . . ? C4 Lu3 N3 C39 165.9(4) . . . . ? C1 Lu3 N3 Si3 -23.3(4) . . . . ? O3 Lu3 N3 Si3 160.6(3) . . . . ? Lu2 Lu3 N3 Si3 -63.1(4) . . . . ? Lu1 Lu3 N3 Si3 20.5(4) . . . . ? C4 Lu3 N3 Si3 -18.3(5) . . . . ? N3 Lu3 O3 C62A 65(5) . . . . ? C1 Lu3 O3 C62A -102(5) . . . . ? C2 Lu3 O3 C62A -120(5) . . . . ? Lu2 Lu3 O3 C62A -81(5) . . . . ? Lu1 Lu3 O3 C62A -153(5) . . . . ? C4 Lu3 O3 C62A -116(5) . . . . ? N3 Lu3 O3 C59 -138(2) . . . . ? C1 Lu3 O3 C59 55(2) . . . . ? C2 Lu3 O3 C59 37(2) . . . . ? Lu2 Lu3 O3 C59 77(2) . . . . ? Lu1 Lu3 O3 C59 5(2) . . . . ? C4 Lu3 O3 C59 41(2) . . . . ? N3 Lu3 O3 C59A -134(3) . . . . ? C1 Lu3 O3 C59A 59(4) . . . . ? C2 Lu3 O3 C59A 41(3) . . . . ? Lu2 Lu3 O3 C59A 81(3) . . . . ? Lu1 Lu3 O3 C59A 9(3) . . . . ? C4 Lu3 O3 C59A 45(3) . . . . ? N3 Lu3 O3 C62 58(2) . . . . ? C1 Lu3 O3 C62 -109(2) . . . . ? C2 Lu3 O3 C62 -127(2) . . . . ? Lu2 Lu3 O3 C62 -87(2) . . . . ? Lu1 Lu3 O3 C62 -159(2) . . . . ? C4 Lu3 O3 C62 -123(2) . . . . ? Si1 N1 C9 C14 -84.6(6) . . . . ? Lu1 N1 C9 C14 88.5(5) . . . . ? Si1 N1 C9 C10 94.8(5) . . . . ? Lu1 N1 C9 C10 -92.0(5) . . . . ? C14 C9 C10 C11 -3.5(8) . . . . ? N1 C9 C10 C11 177.0(5) . . . . ? C14 C9 C10 C15 173.5(5) . . . . ? N1 C9 C10 C15 -6.0(8) . . . . ? C9 C10 C11 C12 2.0(9) . . . . ? C15 C10 C11 C12 -175.2(6) . . . . ? C10 C11 C12 C13 0.7(10) . . . . ? C11 C12 C13 C14 -1.7(10) . . . . ? C12 C13 C14 C9 0.1(9) . . . . ? C12 C13 C14 C18 178.8(6) . . . . ? C10 C9 C14 C13 2.5(8) . . . . ? N1 C9 C14 C13 -178.0(5) . . . . ? C10 C9 C14 C18 -176.1(5) . . . . ? N1 C9 C14 C18 3.4(8) . . . . ? C11 C10 C15 C16 -47.0(7) . . . . ? C9 C10 C15 C16 135.9(6) . . . . ? C11 C10 C15 C17 75.6(7) . . . . ? C9 C10 C15 C17 -101.5(6) . . . . ? C13 C14 C18 C20 56.1(8) . . . . ? C9 C14 C18 C20 -125.2(6) . . . . ? C13 C14 C18 C19 -67.8(8) . . . . ? C9 C14 C18 C19 110.9(7) . . . . ? Si2 N2 C24 C25 98.4(6) . . . . ? Lu2 N2 C24 C25 -86.0(6) . . . . ? Si2 N2 C24 C29 -83.7(6) . . . . ? Lu2 N2 C24 C29 91.9(6) . . . . ? C29 C24 C25 C26 -6.1(9) . . . . ? N2 C24 C25 C26 171.9(6) . . . . ? C29 C24 C25 C30 171.3(6) . . . . ? N2 C24 C25 C30 -10.8(9) . . . . ? C24 C25 C26 C27 2.6(10) . . . . ? C30 C25 C26 C27 -174.9(7) . . . . ? C25 C26 C27 C28 2.4(12) . . . . ? C26 C27 C28 C29 -3.9(12) . . . . ? C27 C28 C29 C24 0.3(10) . . . . ? C27 C28 C29 C33 178.7(7) . . . . ? C25 C24 C29 C28 4.7(9) . . . . ? N2 C24 C29 C28 -173.2(6) . . . . ? C25 C24 C29 C33 -173.5(6) . . . . ? N2 C24 C29 C33 8.5(9) . . . . ? C26 C25 C30 C32 -38.3(8) . . . . ? C24 C25 C30 C32 144.3(6) . . . . ? C26 C25 C30 C31 84.7(8) . . . . ? C24 C25 C30 C31 -92.7(7) . . . . ? C28 C29 C33 C35 71.2(8) . . . . ? C24 C29 C33 C35 -110.5(7) . . . . ? C28 C29 C33 C34 -51.2(8) . . . . ? C24 C29 C33 C34 127.0(7) . . . . ? Si3 N3 C39 C44 -88.9(6) . . . . ? Lu3 N3 C39 C44 87.3(6) . . . . ? Si3 N3 C39 C40 92.1(6) . . . . ? Lu3 N3 C39 C40 -91.8(6) . . . . ? N3 C39 C40 C41 178.1(6) . . . . ? C44 C39 C40 C41 -1.0(9) . . . . ? N3 C39 C40 C45 -3.3(9) . . . . ? C44 C39 C40 C45 177.6(6) . . . . ? C39 C40 C41 C42 1.1(11) . . . . ? C45 C40 C41 C42 -177.6(7) . . . . ? C40 C41 C42 C43 0.4(12) . . . . ? C41 C42 C43 C44 -2.1(12) . . . . ? C42 C43 C44 C39 2.2(11) . . . . ? C42 C43 C44 C48 179.2(7) . . . . ? N3 C39 C44 C43 -179.7(6) . . . . ? C40 C39 C44 C43 -0.6(9) . . . . ? N3 C39 C44 C48 3.5(10) . . . . ? C40 C39 C44 C48 -177.5(7) . . . . ? C41 C40 C45 C46 73.5(8) . . . . ? C39 C40 C45 C46 -105.1(7) . . . . ? C41 C40 C45 C47 -49.3(9) . . . . ? C39 C40 C45 C47 132.1(7) . . . . ? C43 C44 C48 C49 -68.9(11) . . . . ? C39 C44 C48 C49 108.0(10) . . . . ? C43 C44 C48 C50 56.5(10) . . . . ? C39 C44 C48 C50 -126.5(9) . . . . ? C54 O1 C51 C52 40.4(6) . . . . ? Lu1 O1 C51 C52 -151.7(4) . . . . ? O1 C51 C52 C53 -35.2(7) . . . . ? C51 C52 C53 C54 17.3(8) . . . . ? C51 O1 C54 C53 -29.2(7) . . . . ? Lu1 O1 C54 C53 164.1(4) . . . . ? C52 C53 C54 O1 6.5(8) . . . . ? C58 O2 C55 C56 35.8(8) . . . . ? Lu2 O2 C55 C56 -158.0(5) . . . . ? C58 O2 C55 C56A 4.8(13) . . . . ? Lu2 O2 C55 C56A 171.0(12) . . . . ? O2 C55 C56 C57 -29.5(9) . . . . ? C56A C55 C56 C57 67.3(14) . . . . ? O2 C55 C56A C57 20(2) . . . . ? C56 C55 C56A C57 -71.9(15) . . . . ? C55 C56A C57 C58 -34.6(19) . . . . ? C55 C56A C57 C56 70.2(14) . . . . ? C55 C56 C57 C56A -69.1(14) . . . . ? C55 C56 C57 C58 13.3(10) . . . . ? C55 O2 C58 C57 -27.1(8) . . . . ? Lu2 O2 C58 C57 167.8(5) . . . . ? C56A C57 C58 O2 38.1(13) . . . . ? C56 C57 C58 O2 7.8(9) . . . . ? C62A O3 C59 C60 44(4) . . . . ? C62 O3 C59 C60 47(3) . . . . ? Lu3 O3 C59 C60 -119.4(12) . . . . ? O3 C59 C60 C61 -37(3) . . . . ? C59 C60 C61 C62 16(3) . . . . ? C62A O3 C62 C61 -22(27) . . . . ? C59 O3 C62 C61 -36(4) . . . . ? C59A O3 C62 C61 -37(5) . . . . ? Lu3 O3 C62 C61 132.1(16) . . . . ? C60 C61 C62 O3 11(3) . . . . ? C62A O3 C59A C60A -5(6) . . . . ? C59 O3 C59A C60A -10(27) . . . . ? C62 O3 C59A C60A -2(6) . . . . ? Lu3 O3 C59A C60A -171(3) . . . . ? O3 C59A C60A C61A 27(6) . . . . ? C59A C60A C61A C62A -37(6) . . . . ? C60A C61A C62A O3 37(7) . . . . ? C59 O3 C62A C61A -20(7) . . . . ? C59A O3 C62A C61A -20(7) . . . . ? Lu3 O3 C62A C61A 144(3) . . . . ? C4S1 O1S1 C1S1 C2S1 55(2) . . . . ? O1S1 C1S1 C2S1 C3S1 -62(2) . . . . ? C1S1 C2S1 C3S1 C4S1 38(2) . . . . ? C1S1 O1S1 C4S1 C3S1 -32(3) . . . . ? C2S1 C3S1 C4S1 O1S1 -5(3) . . . . ? C4S2 O1S2 C1S2 C2S2 -55(3) . . . . ? O1S2 C1S2 C2S2 C3S2 27(3) . . . . ? C1S2 C2S2 C3S2 C4S2 3(3) . . . . ? C1S2 O1S2 C4S2 C3S2 60(3) . . . . ? C2S2 C3S2 C4S2 O1S2 -33(3) . . . . ?