# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Thomas Cameron' 'John Gordon' 'Brian L. Scott' 'William Tumas' _publ_contact_author_name 'Dr Thomas Cameron' _publ_contact_author_address ; Chemistry Division Los Alamos National Lab MS J514 Los Alamos NM 87544 UNITED STATES OF AMERICA ; _publ_contact_author_email TCAMERON@LANL.GOV _publ_requested_journal 'Chemical Communications' _publ_section_title ; C-H activation of a 2,2'-bipyridine ligand within (mono)pentamethylcyclopentadienyl lutetium complexes ; data_ccd780 _database_code_depnum_ccdc_archive 'CCDC 235857' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H52 Lu N3 O Si' _chemical_formula_weight 757.88 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.390(4) _cell_length_b 19.073(6) _cell_length_c 17.675(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.877(6) _cell_angle_gamma 90.00 _cell_volume 3674.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Octahedron _exptl_crystal_colour orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 2.750 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4549 _exptl_absorpt_correction_T_max 0.6093 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4/CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 2' _diffrn_reflns_number 22928 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0164 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6369 _reflns_number_gt 5783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (v. 4.202, Siemens 1996)' _computing_cell_refinement 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_data_reduction 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHEXTL (v. 5.10)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All hydrogen atom positions, except for HN3, were idealized and refined using the riding model. The postion of atom HN3 was found on the difference map, and refined with isotropic temperature factor fixed at 0.08 \%A^2^. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6369 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.793 _refine_ls_restrained_S_all 1.793 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.729753(13) 0.170688(7) 0.398701(9) 0.02564(7) Uani 1 1 d . . . Si1 Si 1.03717(12) 0.37690(7) 0.38063(8) 0.0458(3) Uani 1 1 d . . . O1 O 0.8704(2) 0.24447(14) 0.40464(17) 0.0336(6) Uani 1 1 d . . . N1 N 0.5513(3) 0.17557(16) 0.4500(2) 0.0327(8) Uani 1 1 d . . . N2 N 0.7566(3) 0.24181(16) 0.5118(2) 0.0309(7) Uani 1 1 d . . . N3 N 0.5943(3) 0.17581(17) 0.2784(2) 0.0333(8) Uani 1 1 d . . . HN3 H 0.597(6) 0.142(3) 0.261(4) 0.080 Uiso 1 1 d . . . C1 C 0.8934(4) 0.0742(2) 0.4052(3) 0.0379(10) Uani 1 1 d . . . C2 C 0.7795(4) 0.0434(2) 0.3602(3) 0.0369(10) Uani 1 1 d . . . C3 C 0.7080(4) 0.03320(19) 0.4127(3) 0.0339(9) Uani 1 1 d . . . C4 C 0.7748(4) 0.0576(2) 0.4887(3) 0.0334(9) Uani 1 1 d . . . C5 C 0.8899(4) 0.0823(2) 0.4839(3) 0.0362(10) Uani 1 1 d . . . C6 C 1.0011(4) 0.0900(3) 0.3758(4) 0.0612(15) Uani 1 1 d . . . H6A H 0.9802 0.0806 0.3202 0.092 Uiso 1 1 calc R . . H6B H 1.0692 0.0612 0.4033 0.092 Uiso 1 1 calc R . . H6C H 1.0231 0.1385 0.3852 0.092 Uiso 1 1 calc R . . C7 C 0.7486(5) 0.0186(2) 0.2770(3) 0.0528(12) Uani 1 1 d . . . H7A H 0.6669 -0.0001 0.2614 0.079 Uiso 1 1 calc R . . H7B H 0.8055 -0.0172 0.2727 0.079 Uiso 1 1 calc R . . H7C H 0.7536 0.0572 0.2432 0.079 Uiso 1 1 calc R . . C8 C 0.5846(4) -0.0035(2) 0.3923(3) 0.0500(12) Uani 1 1 d . . . H8A H 0.5594 -0.0154 0.3372 0.075 Uiso 1 1 calc R . . H8B H 0.5249 0.0271 0.4035 0.075 Uiso 1 1 calc R . . H8C H 0.5914 -0.0454 0.4233 0.075 Uiso 1 1 calc R . . C9 C 0.7369(5) 0.0531(2) 0.5636(3) 0.0503(12) Uani 1 1 d . . . H9A H 0.6542 0.0359 0.5514 0.075 Uiso 1 1 calc R . . H9B H 0.7414 0.0988 0.5870 0.075 Uiso 1 1 calc R . . H9C H 0.7909 0.0217 0.6001 0.075 Uiso 1 1 calc R . . C10 C 0.9948(4) 0.1080(3) 0.5510(3) 0.0565(14) Uani 1 1 d . . . H10A H 0.9708 0.1086 0.5988 0.085 Uiso 1 1 calc R . . H10B H 1.0168 0.1546 0.5396 0.085 Uiso 1 1 calc R . . H10C H 1.0639 0.0774 0.5576 0.085 Uiso 1 1 calc R . . C11 C 0.4422(4) 0.1493(2) 0.4101(3) 0.0384(10) Uani 1 1 d . . . H11 H 0.4330 0.1313 0.3598 0.046 Uiso 1 1 calc R . . C12 C 0.3429(4) 0.1473(3) 0.4391(3) 0.0490(12) Uani 1 1 d . . . H12 H 0.2687 0.1282 0.4094 0.059 Uiso 1 1 calc R . . C13 C 0.3559(5) 0.1745(2) 0.5131(4) 0.0518(13) Uani 1 1 d . . . H13 H 0.2905 0.1735 0.5347 0.062 Uiso 1 1 calc R . . C14 C 0.4667(4) 0.2033(2) 0.5551(3) 0.0451(11) Uani 1 1 d . . . H14 H 0.4768 0.2220 0.6052 0.054 Uiso 1 1 calc R . . C15 C 0.5630(4) 0.2040(2) 0.5218(3) 0.0353(9) Uani 1 1 d . . . C16 C 0.6827(4) 0.23829(19) 0.5594(3) 0.0335(9) Uani 1 1 d . . . C17 C 0.7163(4) 0.2682(2) 0.6332(3) 0.0452(11) Uani 1 1 d . . . H17 H 0.6649 0.2655 0.6655 0.054 Uiso 1 1 calc R . . C18 C 0.8287(5) 0.3026(3) 0.6590(3) 0.0511(12) Uani 1 1 d . . . H18 H 0.8545 0.3214 0.7097 0.061 Uiso 1 1 calc R . . C19 C 0.9018(5) 0.3088(2) 0.6092(3) 0.0449(11) Uani 1 1 d . . . H19 H 0.9760 0.3327 0.6255 0.054 Uiso 1 1 calc R . . C20 C 0.8625(4) 0.2786(2) 0.5345(3) 0.0363(10) Uani 1 1 d . . . C21 C 0.4801(4) 0.2070(2) 0.2454(3) 0.0343(9) Uani 1 1 d . . . C22 C 0.3818(4) 0.1712(2) 0.1907(3) 0.0423(11) Uani 1 1 d . . . C23 C 0.2696(4) 0.2060(3) 0.1604(3) 0.0521(13) Uani 1 1 d . . . H23 H 0.2055 0.1827 0.1244 0.063 Uiso 1 1 calc R . . C24 C 0.2507(5) 0.2736(3) 0.1821(3) 0.0606(15) Uani 1 1 d . . . H24 H 0.1753 0.2955 0.1610 0.073 Uiso 1 1 calc R . . C25 C 0.3454(5) 0.3079(3) 0.2353(3) 0.0554(13) Uani 1 1 d . . . H25 H 0.3328 0.3534 0.2504 0.066 Uiso 1 1 calc R . . C26 C 0.4598(4) 0.2768(2) 0.2674(3) 0.0418(10) Uani 1 1 d . . . C27 C 0.3965(4) 0.0973(3) 0.1642(3) 0.0546(13) Uani 1 1 d . . . H27 H 0.4500 0.0729 0.2101 0.065 Uiso 1 1 calc R . . C28 C 0.4605(6) 0.0947(3) 0.1003(4) 0.0724(17) Uani 1 1 d . . . H28A H 0.4680 0.0468 0.0857 0.109 Uiso 1 1 calc R . . H28B H 0.5407 0.1151 0.1198 0.109 Uiso 1 1 calc R . . H28C H 0.4135 0.1205 0.0550 0.109 Uiso 1 1 calc R . . C29 C 0.2776(5) 0.0554(3) 0.1381(4) 0.088(2) Uani 1 1 d . . . H29A H 0.2946 0.0091 0.1228 0.132 Uiso 1 1 calc R . . H29B H 0.2212 0.0783 0.0940 0.132 Uiso 1 1 calc R . . H29C H 0.2421 0.0524 0.1811 0.132 Uiso 1 1 calc R . . C30 C 0.5614(5) 0.3206(2) 0.3225(3) 0.0485(12) Uani 1 1 d . . . H30 H 0.6266 0.2878 0.3491 0.058 Uiso 1 1 calc R . . C31 C 0.5235(6) 0.3582(3) 0.3868(4) 0.0729(17) Uani 1 1 d . . . H31A H 0.5922 0.3839 0.4194 0.109 Uiso 1 1 calc R . . H31B H 0.4965 0.3246 0.4185 0.109 Uiso 1 1 calc R . . H31C H 0.4578 0.3901 0.3633 0.109 Uiso 1 1 calc R . . C32 C 0.6165(5) 0.3699(3) 0.2749(4) 0.0669(15) Uani 1 1 d . . . H32A H 0.6812 0.3966 0.3100 0.100 Uiso 1 1 calc R . . H32B H 0.5542 0.4012 0.2449 0.100 Uiso 1 1 calc R . . H32C H 0.6490 0.3433 0.2395 0.100 Uiso 1 1 calc R . . C33 C 0.9299(4) 0.2836(2) 0.4716(3) 0.0357(9) Uani 1 1 d . . . H33 H 1.0121 0.2638 0.4939 0.043 Uiso 1 1 calc R . . C34 C 0.9447(4) 0.3616(2) 0.4520(3) 0.0400(10) Uani 1 1 d . . . H34A H 0.9838 0.3863 0.5008 0.048 Uiso 1 1 calc R . . H34B H 0.8638 0.3817 0.4299 0.048 Uiso 1 1 calc R . . C35 C 1.0919(7) 0.4698(3) 0.3943(4) 0.093(2) Uani 1 1 d . . . H35A H 1.0226 0.5008 0.3811 0.139 Uiso 1 1 calc R . . H35B H 1.1425 0.4791 0.3605 0.139 Uiso 1 1 calc R . . H35C H 1.1387 0.4770 0.4484 0.139 Uiso 1 1 calc R . . C36 C 1.1694(6) 0.3160(4) 0.4043(4) 0.083(2) Uani 1 1 d . . . H36A H 1.2165 0.3219 0.4585 0.125 Uiso 1 1 calc R . . H36B H 1.2201 0.3259 0.3706 0.125 Uiso 1 1 calc R . . H36C H 1.1402 0.2686 0.3959 0.125 Uiso 1 1 calc R . . C37 C 0.9466(6) 0.3654(4) 0.2766(4) 0.0799(18) Uani 1 1 d . . . H37A H 0.8788 0.3975 0.2641 0.120 Uiso 1 1 calc R . . H37B H 0.9163 0.3182 0.2685 0.120 Uiso 1 1 calc R . . H37C H 0.9976 0.3745 0.2429 0.120 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 0.02486(10) 0.02743(10) 0.02419(12) 0.00028(7) 0.00643(7) 0.00087(6) Si1 0.0486(7) 0.0497(7) 0.0401(8) 0.0012(6) 0.0143(6) -0.0090(6) O1 0.0348(15) 0.0354(15) 0.0314(17) -0.0061(12) 0.0111(13) -0.0068(12) N1 0.0307(18) 0.0323(18) 0.037(2) 0.0053(14) 0.0123(16) 0.0023(14) N2 0.0328(17) 0.0313(17) 0.028(2) -0.0001(14) 0.0088(16) 0.0015(14) N3 0.0340(18) 0.0361(19) 0.027(2) 0.0013(15) 0.0045(16) 0.0036(16) C1 0.034(2) 0.0235(19) 0.058(3) 0.0059(18) 0.016(2) 0.0067(16) C2 0.039(2) 0.033(2) 0.037(3) -0.0011(18) 0.009(2) 0.0067(17) C3 0.031(2) 0.0244(19) 0.044(3) 0.0027(17) 0.007(2) -0.0006(15) C4 0.036(2) 0.029(2) 0.031(3) 0.0070(17) 0.0043(19) 0.0035(17) C5 0.032(2) 0.028(2) 0.040(3) 0.0055(17) -0.0018(19) 0.0034(16) C6 0.043(3) 0.057(3) 0.094(5) 0.011(3) 0.036(3) 0.013(2) C7 0.077(3) 0.034(2) 0.047(3) -0.008(2) 0.019(3) 0.009(2) C8 0.044(3) 0.036(2) 0.062(4) 0.000(2) 0.003(2) -0.011(2) C9 0.065(3) 0.044(3) 0.044(3) 0.015(2) 0.018(3) 0.011(2) C10 0.043(3) 0.049(3) 0.057(4) 0.002(2) -0.019(2) 0.002(2) C11 0.034(2) 0.040(2) 0.039(3) 0.0076(19) 0.009(2) 0.0018(18) C12 0.033(2) 0.052(3) 0.064(4) 0.007(2) 0.017(2) 0.000(2) C13 0.039(3) 0.056(3) 0.070(4) 0.010(3) 0.031(3) 0.005(2) C14 0.051(3) 0.051(3) 0.041(3) 0.005(2) 0.026(2) 0.009(2) C15 0.036(2) 0.036(2) 0.035(3) 0.0078(18) 0.013(2) 0.0087(18) C16 0.041(2) 0.029(2) 0.033(3) 0.0035(17) 0.013(2) 0.0051(17) C17 0.058(3) 0.045(3) 0.037(3) -0.002(2) 0.022(2) 0.004(2) C18 0.076(4) 0.047(3) 0.029(3) -0.010(2) 0.013(3) -0.001(2) C19 0.055(3) 0.041(2) 0.035(3) -0.0084(19) 0.006(2) -0.008(2) C20 0.041(2) 0.033(2) 0.034(3) 0.0022(18) 0.010(2) 0.0038(18) C21 0.032(2) 0.042(2) 0.030(3) 0.0098(18) 0.0095(19) 0.0044(18) C22 0.037(2) 0.049(3) 0.035(3) 0.017(2) 0.002(2) -0.0005(19) C23 0.037(2) 0.065(3) 0.047(3) 0.015(2) 0.000(2) -0.001(2) C24 0.040(3) 0.082(4) 0.052(4) 0.022(3) 0.001(3) 0.020(3) C25 0.058(3) 0.056(3) 0.050(4) 0.011(2) 0.012(3) 0.023(3) C26 0.044(2) 0.046(2) 0.034(3) 0.010(2) 0.008(2) 0.009(2) C27 0.046(3) 0.048(3) 0.052(4) 0.011(2) -0.012(2) -0.009(2) C28 0.093(5) 0.060(3) 0.056(4) -0.013(3) 0.008(3) -0.002(3) C29 0.078(4) 0.061(4) 0.099(6) 0.007(4) -0.016(4) -0.026(3) C30 0.054(3) 0.040(3) 0.045(3) 0.005(2) 0.003(2) 0.016(2) C31 0.098(5) 0.066(4) 0.050(4) -0.005(3) 0.015(3) 0.009(3) C32 0.067(4) 0.074(4) 0.055(4) -0.003(3) 0.011(3) -0.013(3) C33 0.035(2) 0.034(2) 0.037(3) 0.0007(18) 0.009(2) -0.0011(17) C34 0.046(3) 0.030(2) 0.043(3) -0.0030(19) 0.011(2) -0.0062(19) C35 0.131(6) 0.076(4) 0.081(5) 0.002(3) 0.048(5) -0.044(4) C36 0.057(4) 0.118(5) 0.083(5) 0.016(4) 0.033(4) 0.017(4) C37 0.083(4) 0.108(5) 0.050(4) -0.006(3) 0.019(3) -0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 O1 2.112(3) . ? Lu1 N3 2.238(4) . ? Lu1 N2 2.360(3) . ? Lu1 N1 2.456(3) . ? Lu1 C1 2.598(4) . ? Lu1 C5 2.616(4) . ? Lu1 C2 2.628(4) . ? Lu1 C4 2.641(4) . ? Lu1 C3 2.652(4) . ? Si1 C37 1.842(6) . ? Si1 C36 1.851(6) . ? Si1 C35 1.870(6) . ? Si1 C34 1.886(4) . ? O1 C33 1.397(5) . ? N1 C11 1.336(6) . ? N1 C15 1.351(6) . ? N2 C20 1.351(5) . ? N2 C16 1.355(5) . ? N3 C21 1.395(5) . ? C1 C5 1.412(6) . ? C1 C2 1.436(6) . ? C1 C6 1.495(6) . ? C2 C3 1.413(6) . ? C2 C7 1.486(6) . ? C3 C4 1.417(6) . ? C3 C8 1.518(6) . ? C4 C5 1.419(6) . ? C4 C9 1.509(6) . ? C5 C10 1.501(6) . ? C11 C12 1.371(6) . ? C12 C13 1.376(8) . ? C13 C14 1.378(7) . ? C14 C15 1.388(6) . ? C15 C16 1.484(6) . ? C16 C17 1.373(6) . ? C17 C18 1.392(7) . ? C18 C19 1.380(7) . ? C19 C20 1.391(6) . ? C20 C33 1.526(6) . ? C21 C22 1.424(6) . ? C21 C26 1.423(6) . ? C22 C23 1.402(6) . ? C22 C27 1.509(7) . ? C23 C24 1.379(8) . ? C24 C25 1.374(8) . ? C25 C26 1.394(6) . ? C26 C30 1.527(7) . ? C27 C28 1.511(8) . ? C27 C29 1.525(7) . ? C30 C31 1.509(7) . ? C30 C32 1.515(7) . ? C33 C34 1.547(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Lu1 N3 108.78(12) . . ? O1 Lu1 N2 70.42(11) . . ? N3 Lu1 N2 131.58(12) . . ? O1 Lu1 N1 130.81(10) . . ? N3 Lu1 N1 86.16(13) . . ? N2 Lu1 N1 65.40(11) . . ? O1 Lu1 C1 86.88(12) . . ? N3 Lu1 C1 111.15(14) . . ? N2 Lu1 C1 117.03(13) . . ? N1 Lu1 C1 132.11(12) . . ? O1 Lu1 C5 90.51(12) . . ? N3 Lu1 C5 138.44(13) . . ? N2 Lu1 C5 89.18(13) . . ? N1 Lu1 C5 108.99(13) . . ? C1 Lu1 C5 31.41(14) . . ? O1 Lu1 C2 114.29(12) . . ? N3 Lu1 C2 86.29(13) . . ? N2 Lu1 C2 139.95(13) . . ? N1 Lu1 C2 113.22(12) . . ? C1 Lu1 C2 31.90(13) . . ? C5 Lu1 C2 52.16(14) . . ? O1 Lu1 C4 120.17(12) . . ? N3 Lu1 C4 124.61(13) . . ? N2 Lu1 C4 90.26(12) . . ? N1 Lu1 C4 81.10(11) . . ? C1 Lu1 C4 51.94(13) . . ? C5 Lu1 C4 31.31(12) . . ? C2 Lu1 C4 51.85(13) . . ? O1 Lu1 C3 138.08(11) . . ? N3 Lu1 C3 94.28(13) . . ? N2 Lu1 C3 118.81(13) . . ? N1 Lu1 C3 83.88(11) . . ? C1 Lu1 C3 51.74(12) . . ? C5 Lu1 C3 51.48(13) . . ? C2 Lu1 C3 31.05(13) . . ? C4 Lu1 C3 31.05(13) . . ? C37 Si1 C36 109.5(3) . . ? C37 Si1 C35 108.1(3) . . ? C36 Si1 C35 110.3(3) . . ? C37 Si1 C34 112.9(3) . . ? C36 Si1 C34 109.1(3) . . ? C35 Si1 C34 106.9(3) . . ? C33 O1 Lu1 125.0(2) . . ? C11 N1 C15 118.0(4) . . ? C11 N1 Lu1 122.3(3) . . ? C15 N1 Lu1 119.7(3) . . ? C20 N2 C16 120.2(4) . . ? C20 N2 Lu1 115.8(3) . . ? C16 N2 Lu1 123.1(3) . . ? C21 N3 Lu1 135.8(3) . . ? C5 C1 C2 108.1(4) . . ? C5 C1 C6 125.5(4) . . ? C2 C1 C6 126.2(5) . . ? C5 C1 Lu1 75.0(2) . . ? C2 C1 Lu1 75.2(2) . . ? C6 C1 Lu1 119.5(3) . . ? C3 C2 C1 107.0(4) . . ? C3 C2 C7 126.2(4) . . ? C1 C2 C7 126.4(4) . . ? C3 C2 Lu1 75.4(2) . . ? C1 C2 Lu1 72.9(2) . . ? C7 C2 Lu1 122.9(3) . . ? C2 C3 C4 109.0(4) . . ? C2 C3 C8 125.3(4) . . ? C4 C3 C8 125.6(4) . . ? C2 C3 Lu1 73.5(2) . . ? C4 C3 Lu1 74.0(2) . . ? C8 C3 Lu1 122.6(3) . . ? C3 C4 C5 107.6(4) . . ? C3 C4 C9 127.0(4) . . ? C5 C4 C9 125.2(4) . . ? C3 C4 Lu1 74.9(2) . . ? C5 C4 Lu1 73.4(2) . . ? C9 C4 Lu1 121.3(3) . . ? C1 C5 C4 108.3(4) . . ? C1 C5 C10 124.8(4) . . ? C4 C5 C10 126.8(4) . . ? C1 C5 Lu1 73.6(2) . . ? C4 C5 Lu1 75.3(2) . . ? C10 C5 Lu1 120.4(3) . . ? N1 C11 C12 123.7(5) . . ? C11 C12 C13 118.3(5) . . ? C12 C13 C14 119.4(4) . . ? C13 C14 C15 119.2(5) . . ? N1 C15 C14 121.4(4) . . ? N1 C15 C16 115.1(3) . . ? C14 C15 C16 123.4(4) . . ? N2 C16 C17 121.2(4) . . ? N2 C16 C15 113.6(4) . . ? C17 C16 C15 125.1(4) . . ? C16 C17 C18 118.9(4) . . ? C19 C18 C17 120.0(5) . . ? C18 C19 C20 118.9(4) . . ? N2 C20 C19 120.6(4) . . ? N2 C20 C33 114.3(4) . . ? C19 C20 C33 125.1(4) . . ? N3 C21 C22 122.1(4) . . ? N3 C21 C26 119.4(4) . . ? C22 C21 C26 118.5(4) . . ? C23 C22 C21 118.7(4) . . ? C23 C22 C27 119.7(4) . . ? C21 C22 C27 121.6(4) . . ? C24 C23 C22 122.4(5) . . ? C23 C24 C25 118.8(5) . . ? C24 C25 C26 122.1(5) . . ? C25 C26 C21 119.6(5) . . ? C25 C26 C30 118.2(4) . . ? C21 C26 C30 122.2(4) . . ? C22 C27 C28 112.6(4) . . ? C22 C27 C29 114.5(5) . . ? C28 C27 C29 109.6(5) . . ? C31 C30 C32 112.2(5) . . ? C31 C30 C26 114.2(5) . . ? C32 C30 C26 110.2(4) . . ? O1 C33 C20 111.1(3) . . ? O1 C33 C34 112.4(3) . . ? C20 C33 C34 109.5(3) . . ? C33 C34 Si1 114.7(3) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.865 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.081 data_ccd788 _database_code_depnum_ccdc_archive 'CCDC 236211' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H45 Lu N2 O2 Si2' _chemical_formula_weight 696.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.367(2) _cell_length_b 20.140(5) _cell_length_c 14.186(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.178(4) _cell_angle_gamma 90.00 _cell_volume 3214.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 3.173 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4703 _exptl_absorpt_correction_T_max 0.8325 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4 with Smart 1K CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 2' _diffrn_reflns_number 22782 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.18 _reflns_number_total 7044 _reflns_number_gt 3971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (v. 4.202, Siemens 1996)' _computing_cell_refinement 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_data_reduction 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHEXTL (v. 5.10)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All hydrogen atom positions were idealized. The Cp ring was disordered and refined in two one-half occupancy positions. Each ring was refined as a rigid body, and the anisotropic temperature factors were constrained to be equal on corresponding atom postions in the ring, i.e.- C5 and C5'. ; _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^)+(0.0471P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7044 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1409 _refine_ls_R_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 1.256 _refine_ls_restrained_S_all 1.256 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.81334(2) -0.00004(2) 0.25030(2) 0.03864(12) Uani 1 1 d . . . Si1 Si 0.4427(2) 0.16346(13) 0.2710(2) 0.0539(7) Uani 1 1 d . . . Si2 Si 0.5314(2) -0.13151(12) 0.33208(19) 0.0472(6) Uani 1 1 d . . . O1 O 0.6757(4) 0.0688(3) 0.2575(4) 0.0451(15) Uani 1 1 d . . . O2 O 0.7485(5) -0.0850(3) 0.3055(4) 0.0461(15) Uani 1 1 d . . . N1 N 0.9999(6) -0.0170(3) 0.3566(5) 0.0384(18) Uani 1 1 d . . . N2 N 0.8860(3) 0.09735(19) 0.3373(2) 0.0357(15) Uani 1 1 d . . . C1 C 0.8230(3) 0.04714(19) 0.0751(2) 0.049(5) Uani 0.50 1 d PR . . C2 C 0.7746(3) -0.01798(19) 0.0687(2) 0.049(5) Uani 0.50 1 d PR . . C3 C 0.8674(3) -0.06322(19) 0.1013(2) 0.052(3) Uani 0.50 1 d PR . . C4 C 0.9731(3) -0.02607(19) 0.1277(2) 0.055(3) Uani 0.50 1 d PR . . C5 C 0.9457(3) 0.04213(19) 0.1116(2) 0.057(5) Uani 0.50 1 d PR . . C6 C 0.7559(3) 0.11054(19) 0.0479(2) 0.118(11) Uani 0.50 1 d PR . . C7 C 0.6470(3) -0.03595(19) 0.0336(2) 0.157(16) Uani 0.50 1 d PR . . C8 C 0.8557(3) -0.13773(19) 0.1068(2) 0.132(14) Uani 0.50 1 d PR . . C9 C 1.0935(3) -0.05415(19) 0.1663(2) 0.127(12) Uani 0.50 1 d PR . . C10 C 1.0318(3) 0.09929(19) 0.1299(2) 0.123(13) Uani 0.50 1 d PR . . C1' C 0.7778(3) 0.01882(19) 0.0734(2) 0.049(5) Uani 0.50 1 d PR . . C2' C 0.7824(3) -0.05129(19) 0.0838(2) 0.049(5) Uani 0.50 1 d PR . . C3' C 0.9017(3) -0.06933(19) 0.1178(2) 0.052(3) Uani 0.50 1 d PR . . C4' C 0.9708(3) -0.01036(19) 0.1284(2) 0.055(3) Uani 0.50 1 d PR . . C5' C 0.8942(3) 0.04412(19) 0.1009(2) 0.057(5) Uani 0.50 1 d PR . . C6' C 0.6684(3) 0.05934(19) 0.0391(2) 0.118(11) Uani 0.50 1 d PR . . C7' C 0.6787(3) -0.09838(19) 0.0625(2) 0.157(16) Uani 0.50 1 d PR . . C8' C 0.9470(3) -0.13896(19) 0.1390(2) 0.132(14) Uani 0.50 1 d PR . . C9' C 1.1025(3) -0.00631(19) 0.1628(2) 0.127(12) Uani 0.50 1 d PR . . C10' C 0.9303(3) 0.11625(19) 0.1010(2) 0.123(13) Uani 0.50 1 d PR . . C11 C 1.0477(7) -0.0760(5) 0.3712(6) 0.043(2) Uani 1 1 d . . . H11 H 1.0074 -0.1115 0.3394 0.052 Uiso 1 1 calc R . . C12 C 1.1526(7) -0.0902(5) 0.4297(6) 0.052(2) Uani 1 1 d . . . H12 H 1.1820 -0.1332 0.4375 0.063 Uiso 1 1 calc R . . C13 C 1.2118(7) -0.0363(6) 0.4762(6) 0.051(2) Uani 1 1 d . . . H13 H 1.2821 -0.0427 0.5176 0.061 Uiso 1 1 calc R . . C14 C 1.1654(7) 0.0262(5) 0.4606(6) 0.047(2) Uani 1 1 d . . . H14 H 1.2046 0.0627 0.4904 0.056 Uiso 1 1 calc R . . C15 C 1.0603(7) 0.0343(4) 0.4003(5) 0.0354(18) Uani 1 1 d . . . C16 C 0.9993(7) 0.0995(4) 0.3854(5) 0.038(2) Uani 1 1 d . . . C17 C 1.0454(7) 0.1590(4) 0.4226(6) 0.049(2) Uani 1 1 d . . . H17 H 1.1219 0.1613 0.4560 0.059 Uiso 1 1 calc R . . C18 C 0.9747(8) 0.2151(5) 0.4087(7) 0.057(3) Uani 1 1 d . . . H18 H 1.0045 0.2559 0.4317 0.068 Uiso 1 1 calc R . . C19 C 0.8617(8) 0.2109(4) 0.3617(6) 0.050(2) Uani 1 1 d . . . H19 H 0.8137 0.2484 0.3536 0.061 Uiso 1 1 calc R . . C20 C 0.8194(7) 0.1500(4) 0.3262(6) 0.041(2) Uani 1 1 d . . . C21 C 0.6930(7) 0.1360(5) 0.2762(6) 0.046(2) Uani 1 1 d . . . H21 H 0.6843 0.1588 0.2146 0.055 Uiso 1 1 calc R . . C22 C 0.5998(7) 0.1663(4) 0.3338(6) 0.049(2) Uani 1 1 d . . . H22A H 0.6209 0.2122 0.3484 0.059 Uiso 1 1 calc R . . H22B H 0.6035 0.1427 0.3937 0.059 Uiso 1 1 calc R . . C23 C 0.3834(9) 0.0782(5) 0.2507(10) 0.104(5) Uani 1 1 d . . . H23A H 0.3876 0.0554 0.3105 0.155 Uiso 1 1 calc R . . H23B H 0.4297 0.0546 0.2100 0.155 Uiso 1 1 calc R . . H23C H 0.3022 0.0803 0.2210 0.155 Uiso 1 1 calc R . . C24 C 0.3469(9) 0.2081(7) 0.3473(9) 0.106(5) Uani 1 1 d . . . H24A H 0.3499 0.1854 0.4072 0.160 Uiso 1 1 calc R . . H24B H 0.2664 0.2089 0.3158 0.160 Uiso 1 1 calc R . . H24C H 0.3752 0.2527 0.3582 0.160 Uiso 1 1 calc R . . C25 C 0.4342(9) 0.2077(6) 0.1562(8) 0.087(4) Uani 1 1 d . . . H25A H 0.3543 0.2058 0.1235 0.131 Uiso 1 1 calc R . . H25B H 0.4869 0.1870 0.1177 0.131 Uiso 1 1 calc R . . H25C H 0.4570 0.2532 0.1675 0.131 Uiso 1 1 calc R . . C26 C 0.6951(7) -0.1406(4) 0.3305(6) 0.040(2) Uani 1 1 d . . . C27 C 0.7529(8) -0.1962(5) 0.3560(6) 0.060(3) Uani 1 1 d . . . H27A H 0.8348 -0.1983 0.3572 0.072 Uiso 1 1 calc R . . H27B H 0.7116 -0.2333 0.3727 0.072 Uiso 1 1 calc R . . C28 C 0.4556(9) -0.1087(5) 0.2106(7) 0.079(3) Uani 1 1 d . . . H28A H 0.4651 -0.1441 0.1669 0.119 Uiso 1 1 calc R . . H28B H 0.4902 -0.0688 0.1898 0.119 Uiso 1 1 calc R . . H28C H 0.3725 -0.1016 0.2128 0.119 Uiso 1 1 calc R . . C29 C 0.4639(9) -0.2097(5) 0.3704(8) 0.079(3) Uani 1 1 d . . . H29A H 0.4742 -0.2446 0.3261 0.118 Uiso 1 1 calc R . . H29B H 0.3807 -0.2029 0.3720 0.118 Uiso 1 1 calc R . . H29C H 0.5022 -0.2220 0.4327 0.118 Uiso 1 1 calc R . . C30 C 0.5126(8) -0.0628(4) 0.4156(7) 0.062(3) Uani 1 1 d . . . H30A H 0.4295 -0.0559 0.4179 0.092 Uiso 1 1 calc R . . H30B H 0.5466 -0.0229 0.3941 0.092 Uiso 1 1 calc R . . H30C H 0.5519 -0.0740 0.4780 0.092 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 0.02641(15) 0.0572(2) 0.03149(17) -0.0071(2) 0.00124(11) 0.0004(2) Si1 0.0334(12) 0.0628(17) 0.0645(19) 0.0138(15) 0.0036(13) 0.0042(12) Si2 0.0348(13) 0.0489(15) 0.0559(17) -0.0082(13) -0.0003(12) -0.0028(11) O1 0.028(3) 0.053(4) 0.053(4) -0.015(3) -0.002(3) 0.002(3) O2 0.033(3) 0.056(4) 0.049(4) -0.003(3) 0.005(3) -0.003(3) N1 0.032(3) 0.053(5) 0.031(4) -0.001(3) 0.004(3) 0.008(3) N2 0.024(3) 0.053(4) 0.028(4) -0.005(3) 0.000(3) -0.007(3) C1 0.049(10) 0.061(13) 0.045(8) 0.034(8) 0.037(8) 0.016(8) C2 0.049(7) 0.081(17) 0.016(6) 0.012(8) -0.002(6) -0.016(8) C3 0.057(9) 0.072(8) 0.031(7) 0.002(6) 0.020(7) 0.008(7) C4 0.038(5) 0.101(10) 0.028(5) 0.005(5) 0.010(4) -0.006(5) C5 0.083(15) 0.052(7) 0.045(7) -0.017(6) 0.039(9) -0.040(8) C6 0.15(2) 0.16(2) 0.046(9) 0.040(14) 0.024(14) 0.093(18) C7 0.088(15) 0.31(5) 0.078(15) -0.06(2) 0.010(13) -0.08(2) C8 0.28(4) 0.046(8) 0.088(15) -0.005(9) 0.08(2) 0.006(15) C9 0.037(7) 0.29(4) 0.063(9) 0.037(15) 0.027(7) 0.004(14) C10 0.22(3) 0.093(13) 0.067(13) -0.024(10) 0.046(18) -0.093(19) C1' 0.049(10) 0.061(13) 0.045(8) 0.034(8) 0.037(8) 0.016(8) C2' 0.049(7) 0.081(17) 0.016(6) 0.012(8) -0.002(6) -0.016(8) C3' 0.057(9) 0.072(8) 0.031(7) 0.002(6) 0.020(7) 0.008(7) C4' 0.038(5) 0.101(10) 0.028(5) 0.005(5) 0.010(4) -0.006(5) C5' 0.083(15) 0.052(7) 0.045(7) -0.017(6) 0.039(9) -0.040(8) C6' 0.15(2) 0.16(2) 0.046(9) 0.040(14) 0.024(14) 0.093(18) C7' 0.088(15) 0.31(5) 0.078(15) -0.06(2) 0.010(13) -0.08(2) C8' 0.28(4) 0.046(8) 0.088(15) -0.005(9) 0.08(2) 0.006(15) C9' 0.037(7) 0.29(4) 0.063(9) 0.037(15) 0.027(7) 0.004(14) C10' 0.22(3) 0.093(13) 0.067(13) -0.024(10) 0.046(18) -0.093(19) C11 0.032(5) 0.061(6) 0.038(5) -0.002(5) 0.006(4) -0.001(4) C12 0.037(5) 0.079(7) 0.042(5) 0.010(5) 0.012(4) 0.014(5) C13 0.018(4) 0.095(7) 0.039(6) 0.011(5) 0.002(4) 0.010(5) C14 0.019(4) 0.082(6) 0.039(5) 0.001(4) 0.003(4) -0.008(4) C15 0.026(4) 0.058(5) 0.023(4) 0.003(4) 0.007(4) -0.006(4) C16 0.033(4) 0.063(6) 0.021(4) 0.002(4) 0.009(4) -0.003(4) C17 0.033(4) 0.068(6) 0.045(5) -0.008(5) 0.000(4) -0.010(4) C18 0.064(6) 0.052(6) 0.053(6) -0.006(5) 0.005(5) -0.017(5) C19 0.049(6) 0.051(6) 0.050(6) 0.004(5) 0.005(5) -0.006(4) C20 0.034(4) 0.052(5) 0.036(5) 0.007(4) 0.005(4) 0.002(4) C21 0.032(4) 0.071(6) 0.031(5) 0.004(5) -0.009(4) 0.002(4) C22 0.036(5) 0.059(6) 0.051(6) 0.002(5) 0.004(4) 0.006(4) C23 0.054(7) 0.070(8) 0.183(14) 0.013(9) 0.002(8) -0.012(6) C24 0.052(7) 0.160(13) 0.109(10) 0.004(9) 0.015(7) 0.038(8) C25 0.057(7) 0.110(9) 0.086(9) 0.048(7) -0.015(6) -0.005(6) C26 0.039(5) 0.052(5) 0.028(5) -0.006(4) 0.000(4) -0.001(4) C27 0.054(6) 0.058(6) 0.065(7) -0.005(5) 0.001(5) 0.005(5) C28 0.076(8) 0.074(7) 0.077(8) -0.016(6) -0.023(7) 0.018(6) C29 0.060(7) 0.065(7) 0.109(10) 0.006(7) 0.003(7) -0.017(5) C30 0.050(6) 0.070(7) 0.068(7) -0.014(5) 0.018(5) 0.009(5) _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 O2 2.062(5) . ? Lu1 O1 2.104(5) . ? Lu1 N2 2.400(4) . ? Lu1 N1 2.445(7) . ? Lu1 C1' 2.513(3) . ? Lu1 C2' 2.555(3) . ? Lu1 C2 2.576(3) . ? Lu1 C5' 2.584(3) . ? Lu1 C3 2.615(3) . ? Lu1 C3' 2.651(3) . ? Lu1 C4' 2.668(3) . ? Lu1 C1 2.678(3) . ? Si1 C25 1.847(10) . ? Si1 C23 1.853(10) . ? Si1 C24 1.871(11) . ? Si1 C22 1.880(8) . ? Si2 C30 1.854(8) . ? Si2 C29 1.867(9) . ? Si2 C28 1.871(10) . ? Si2 C26 1.873(8) . ? O1 C21 1.387(10) . ? O2 C26 1.345(9) . ? N1 C11 1.311(10) . ? N1 C15 1.342(10) . ? N2 C20 1.299(9) . ? N2 C16 1.371(9) . ? C1 C1' 0.7659 . ? C1 C5' 0.8418 . ? C1 C5 1.4200 . ? C1 C2 1.4200 . ? C1 C6 1.5095 . ? C1 C6' 1.7767 . ? C1 C10' 1.8524 . ? C2 C2' 0.7060 . ? C2 C1' 0.7445 . ? C2 C3 1.4200 . ? C2 C7 1.5094 . ? C2 C3' 1.8313 . ? C2 C5' 1.8558 . ? C2 C7' 1.9472 . ? C2 C6' 1.9791 . ? C3 C2' 0.9920 . ? C3 C4 1.4200 . ? C3 C8 1.5095 . ? C3 C4' 1.5919 . ? C3 C8' 1.8151 . ? C3 C1' 1.9517 . ? C4 C3' 1.1855 . ? C4 C5 1.4200 . ? C4 C9 1.5094 . ? C4 C9' 1.5365 . ? C4 C5' 1.6881 . ? C5 C5' 0.5843 . ? C5 C4' 1.1122 . ? C5 C10' 1.5079 . ? C5 C10 1.5094 . ? C5 C1' 1.9650 . ? C6 C6' 1.4258 . ? C6 C1' 1.8920 . ? C6 C10' 2.0215 . ? C7 C7' 1.3557 . ? C7 C2' 1.6310 . ? C7 C1' 1.8727 . ? C7 C6' 1.9347 . ? C8 C8' 1.0738 . ? C8 C3' 1.4740 . ? C8 C2' 1.9372 . ? C9 C9' 0.9711 . ? C9 C4' 1.6729 . ? C10 C10' 1.2174 . ? C10 C5' 1.9147 . ? C1' C5' 1.4200 . ? C1' C2' 1.4200 . ? C1' C6' 1.5094 . ? C2' C3' 1.4200 . ? C2' C7' 1.5095 . ? C3' C4' 1.4200 . ? C3' C8' 1.5095 . ? C4' C5' 1.4200 . ? C4' C9' 1.5094 . ? C5' C10' 1.5095 . ? C11 C12 1.382(11) . ? C12 C13 1.393(12) . ? C13 C14 1.370(13) . ? C14 C15 1.376(11) . ? C15 C16 1.488(11) . ? C16 C17 1.382(11) . ? C17 C18 1.383(12) . ? C18 C19 1.362(12) . ? C19 C20 1.387(11) . ? C20 C21 1.536(10) . ? C21 C22 1.553(10) . ? C26 C27 1.322(11) . ? 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 O2 Lu1 O1 102.7(2) . . ? O2 Lu1 N2 126.78(17) . . ? O1 Lu1 N2 68.89(17) . . ? O2 Lu1 N1 88.6(2) . . ? O1 Lu1 N1 130.4(2) . . ? N2 Lu1 N1 65.94(17) . . ? O2 Lu1 C1' 119.28(18) . . ? O1 Lu1 C1' 86.22(17) . . ? N2 Lu1 C1' 112.61(14) . . ? N1 Lu1 C1' 129.71(16) . . ? O2 Lu1 C2' 90.33(17) . . ? O1 Lu1 C2' 107.82(17) . . ? N2 Lu1 C2' 142.87(14) . . ? N1 Lu1 C2' 120.44(16) . . ? C1' Lu1 C2' 32.5 . . ? O2 Lu1 C2 104.10(18) . . ? O1 Lu1 C2 96.83(17) . . ? N2 Lu1 C2 128.75(15) . . ? N1 Lu1 C2 127.35(16) . . ? C1' Lu1 C2 16.8 . . ? C2' Lu1 C2 15.8 . . ? O2 Lu1 C5' 141.72(17) . . ? O1 Lu1 C5' 99.60(17) . . ? N2 Lu1 C5' 90.22(12) . . ? N1 Lu1 C5' 100.07(16) . . ? C1' Lu1 C5' 32.3 . . ? C2' Lu1 C5' 53.10(5) . . ? C2 Lu1 C5' 42.2 . . ? O2 Lu1 C3 92.33(17) . . ? O1 Lu1 C3 128.48(17) . . ? N2 Lu1 C3 135.25(14) . . ? N1 Lu1 C3 98.49(16) . . ? C1' Lu1 C3 44.7 . . ? C2' Lu1 C3 22.1 . . ? C2 Lu1 C3 31.7 . . ? C5' Lu1 C3 49.7 . . ? O2 Lu1 C3' 91.37(16) . . ? O1 Lu1 C3' 137.82(17) . . ? N2 Lu1 C3' 131.11(14) . . ? N1 Lu1 C3' 88.90(16) . . ? C1' Lu1 C3' 52.76(5) . . ? C2' Lu1 C3' 31.6 . . ? C2 Lu1 C3' 41.0 . . ? C5' Lu1 C3' 52.0 . . ? C3 Lu1 C3' 9.6 . . ? O2 Lu1 C4' 119.37(16) . . ? O1 Lu1 C4' 130.92(17) . . ? N2 Lu1 C4' 100.58(12) . . ? N1 Lu1 C4' 77.63(16) . . ? C1' Lu1 C4' 52.55(5) . . ? C2' Lu1 C4' 52.14(5) . . ? C2 Lu1 C4' 51.4 . . ? C5' Lu1 C4' 31.3 . . ? C3 Lu1 C4' 35.1 . . ? C3' Lu1 C4' 31.0 . . ? O2 Lu1 C1 135.32(18) . . ? O1 Lu1 C1 86.59(17) . . ? N2 Lu1 C1 97.51(13) . . ? N1 Lu1 C1 118.37(16) . . ? C1' Lu1 C1 16.6 . . ? C2' Lu1 C1 45.9 . . ? C2 Lu1 C1 31.3 . . ? C5' Lu1 C1 18.3 . . ? C3 Lu1 C1 51.4 . . ? C3' Lu1 C1 57.24(5) . . ? C4' Lu1 C1 46.1 . . ? C25 Si1 C23 109.7(6) . . ? C25 Si1 C24 108.5(6) . . ? C23 Si1 C24 107.8(6) . . ? C25 Si1 C22 109.3(4) . . ? C23 Si1 C22 113.7(5) . . ? C24 Si1 C22 107.6(5) . . ? C30 Si2 C29 110.8(5) . . ? C30 Si2 C28 109.0(4) . . ? C29 Si2 C28 108.7(5) . . ? C30 Si2 C26 106.6(4) . . ? C29 Si2 C26 111.8(4) . . ? C28 Si2 C26 110.0(4) . . ? C21 O1 Lu1 124.5(4) . . ? C26 O2 Lu1 172.1(6) . . ? C11 N1 C15 116.8(8) . . ? C11 N1 Lu1 121.8(6) . . ? C15 N1 Lu1 121.3(5) . . ? C20 N2 C16 121.6(6) . . ? C20 N2 Lu1 116.9(4) . . ? C16 N2 Lu1 120.8(4) . . ? C1' C1 C5' 124.0 . . ? C1' C1 C5 125.3 . . ? C5' C1 C5 4.4 . . ? C1' C1 C2 19.6 . . ? C5' C1 C2 107.5 . . ? C5 C1 C2 108.0 . . ? C1' C1 C6 108.0 . . ? C5' C1 C6 126.3 . . ? C5 C1 C6 126.0 . . ? C2 C1 C6 126.0 . . ? C1' C1 C6' 57.4 . . ? C5' C1 C6' 170.4 . . ? C5 C1 C6' 174.1 . . ? C2 C1 C6' 75.6 . . ? C6 C1 C6' 50.6 . . ? C1' C1 C10' 170.3 . . ? C5' C1 C10' 53.4 . . ? C5 C1 C10' 52.9 . . ? C2 C1 C10' 160.8 . . ? C6 C1 C10' 73.1 . . ? C6' C1 C10' 123.3 . . ? C1' C1 Lu1 69.44(8) . . ? C5' C1 Lu1 74.57(8) . . ? C5 C1 Lu1 78.73(8) . . ? C2 C1 Lu1 70.40(8) . . ? C6 C1 Lu1 116.84(8) . . ? C6' C1 Lu1 98.41(8) . . ? C10' C1 Lu1 101.25(8) . . ? C2' C2 C1' 156.4 . . ? C2' C2 C1 145.9 . . ? C1' C2 C1 20.2 . . ? C2' C2 C3 40.2 . . ? C1' C2 C3 125.8 . . ? C1 C2 C3 108.0 . . ? C2' C2 C7 86.9 . . ? C1' C2 C7 107.5 . . ? C1 C2 C7 126.0 . . ? C3 C2 C7 126.0 . . ? C2' C2 C3' 44.8 . . ? C1' C2 C3' 120.2 . . ? C1 C2 C3' 102.7 . . ? C3 C2 C3' 5.8 . . ? C7 C2 C3' 131.2 . . ? C2' C2 C5' 120.7 . . ? C1' C2 C5' 44.2 . . ? C1 C2 C5' 25.6 . . ? C3 C2 C5' 82.4 . . ? C7 C2 C5' 151.5 . . ? C3' C2 C5' 77.1 . . ? C2' C2 C7' 43.0 . . ? C1' C2 C7' 148.4 . . ? C1 C2 C7' 168.6 . . ? C3 C2 C7' 82.3 . . ? C7 C2 C7' 44.0 . . ? C3' C2 C7' 87.3 . . ? C5' C2 C7' 163.2 . . ? C2' C2 C6' 149.1 . . ? C1' C2 C6' 41.9 . . ? C1 C2 C6' 60.4 . . ? C3 C2 C6' 167.6 . . ? C7 C2 C6' 65.8 . . ? C3' C2 C6' 161.7 . . ? C5' C2 C6' 85.7 . . ? C7' C2 C6' 108.9 . . ? C2' C2 Lu1 80.44(9) . . ? C1' C2 Lu1 76.83(9) . . ? C1 C2 Lu1 78.31(8) . . ? C3 C2 Lu1 75.63(9) . . ? C7 C2 Lu1 112.55(8) . . ? C3' C2 Lu1 71.69(9) . . ? C5' C2 Lu1 69.17(8) . . ? C7' C2 Lu1 100.18(8) . . ? C6' C2 Lu1 96.57(9) . . ? C2' C3 C4 134.1 . . ? C2' C3 C2 27.4 . . ? C4 C3 C2 108.0 . . ? C2' C3 C8 99.4 . . ? C4 C3 C8 126.0 . . ? C2 C3 C8 126.0 . . ? C2' C3 C4' 123.9 . . ? C4 C3 C4' 10.2 . . ? C2 C3 C4' 97.9 . . ? C8 C3 C4' 136.0 . . ? C2' C3 C8' 134.8 . . ? C4 C3 C8' 89.8 . . ? C2 C3 C8' 162.0 . . ? C8 C3 C8' 36.2 . . ? C4' C3 C8' 99.8 . . ? C2' C3 C1' 44.2 . . ? C4 C3 C1' 90.3 . . ? C2 C3 C1' 18.0 . . ? C8 C3 C1' 143.6 . . ? C4' C3 C1' 80.1 . . ? C8' C3 C1' 174.4 . . ? C2' C3 Lu1 75.60(9) . . ? C4 C3 Lu1 79.46(8) . . ? C2 C3 Lu1 72.63(9) . . ? C8 C3 Lu1 114.18(8) . . ? C4' C3 Lu1 74.30(8) . . ? C8' C3 Lu1 109.61(9) . . ? C1' C3 Lu1 64.90(9) . . ? C3' C4 C3 16.6 . . ? C3' C4 C5 124.1 . . ? C3 C4 C5 108.0 . . ? C3' C4 C9 109.7 . . ? C3 C4 C9 126.0 . . ? C5 C4 C9 126.0 . . ? C3' C4 C9' 146.8 . . ? C3 C4 C9' 163.2 . . ? C5 C4 C9' 88.8 . . ? C9 C4 C9' 37.2 . . ? C3' C4 C5' 104.8 . . ? C3 C4 C5' 88.8 . . ? C5 C4 C5' 19.3 . . ? C9 C4 C5' 145.1 . . ? C9' C4 C5' 108.0 . . ? C3' C4 Lu1 73.22(8) . . ? C3 C4 Lu1 69.88(8) . . ? C5 C4 Lu1 76.54(8) . . ? C9 C4 Lu1 119.38(8) . . ? C9' C4 Lu1 115.85(8) . . ? C5' C4 Lu1 66.64(8) . . ? C5' C5 C4' 109.7 . . ? C5' C5 C1 6.4 . . ? C4' C5 C1 110.7 . . ? C5' C5 C4 107.2 . . ? C4' C5 C4 3.6 . . ? C1 C5 C4 108.0 . . ? C5' C5 C10' 79.0 . . ? C4' C5 C10' 170.1 . . ? C1 C5 C10' 78.4 . . ? C4 C5 C10' 173.4 . . ? C5' C5 C10 126.4 . . ? C4' C5 C10 123.2 . . ? C1 C5 C10 126.0 . . ? C4 C5 C10 126.0 . . ? C10' C5 C10 47.6 . . ? C5' C5 C1' 17.8 . . ? C4' C5 C1' 92.4 . . ? C1 C5 C1' 18.5 . . ? C4 C5 C1' 89.7 . . ? C10' C5 C1' 96.6 . . ? C10 C5 C1' 144.1 . . ? C5' C5 Lu1 65.15(8) . . ? C4' C5 Lu1 72.86(8) . . ? C1 C5 Lu1 71.14(8) . . ? C4 C5 Lu1 73.62(8) . . ? C10' C5 Lu1 107.83(8) . . ? C10 C5 Lu1 120.99(7) . . ? C1' C5 Lu1 61.25(8) . . ? C6' C6 C1 74.4 . . ? C6' C6 C1' 51.8 . . ? C1 C6 C1' 22.6 . . ? C6' C6 C10' 135.1 . . ? C1 C6 C10' 61.3 . . ? C1' C6 C10' 83.6 . . ? C7' C7 C2 85.4 . . ? C7' C7 C2' 59.9 . . ? C2 C7 C2' 25.6 . . ? C7' C7 C1' 106.8 . . ? C2 C7 C1' 22.3 . . ? C2' C7 C1' 47.2 . . ? C7' C7 C6' 151.8 . . ? C2 C7 C6' 68.9 . . ? C2' C7 C6' 93.7 . . ? C1' C7 C6' 46.7 . . ? C8' C8 C3' 70.7 . . ? C8' C8 C3 87.6 . . ? C3' C8 C3 17.0 . . ? C8' C8 C2' 117.3 . . ? C3' C8 C2' 46.8 . . ? C3 C8 C2' 30.3 . . ? C9' C9 C4 72.9 . . ? C9' C9 C4' 63.2 . . ? C4 C9 C4' 9.8 . . ? C10' C10 C5 66.1 . . ? C10' C10 C5' 52.0 . . ? C5 C10 C5' 14.2 . . ? C2 C1' C1 140.1 . . ? C2 C1' C5' 114.4 . . ? C1 C1' C5' 29.4 . . ? C2 C1' C2' 11.5 . . ? C1 C1' C2' 136.3 . . ? C5' C1' C2' 108.0 . . ? C2 C1' C6' 118.8 . . ? C1 C1' C6' 97.3 . . ? C5' C1' C6' 126.0 . . ? C2' C1' C6' 126.0 . . ? C2 C1' C7 50.3 . . ? C1 C1' C7 161.5 . . ? C5' C1' C7 164.4 . . ? C2' C1' C7 57.4 . . ? C6' C1' C7 68.8 . . ? C2 C1' C6 162.1 . . ? C1 C1' C6 49.4 . . ? C5' C1' C6 78.1 . . ? C2' C1' C6 173.1 . . ? C6' C1' C6 48.0 . . ? C7 C1' C6 116.1 . . ? C2 C1' C3 36.1 . . ? C1 C1' C3 107.2 . . ? C5' C1' C3 79.0 . . ? C2' C1' C3 29.1 . . ? C6' C1' C3 154.9 . . ? C7 C1' C3 86.1 . . ? C6 C1' C3 156.4 . . ? C2 C1' C5 107.2 . . ? C1 C1' C5 36.1 . . ? C5' C1' C5 7.2 . . ? C2' C1' C5 100.9 . . ? C6' C1' C5 133.1 . . ? C7 C1' C5 157.2 . . ? C6 C1' C5 85.2 . . ? C3 C1' C5 71.8 . . ? C2 C1' Lu1 86.41(9) . . ? C1 C1' Lu1 93.99(9) . . ? C5' C1' Lu1 76.61(8) . . ? C2' C1' Lu1 75.37(9) . . ? C6' C1' Lu1 114.32(8) . . ? C7 C1' Lu1 102.73(8) . . ? C6 C1' Lu1 109.68(9) . . ? C3 C1' Lu1 70.41(9) . . ? C5 C1' Lu1 75.48(8) . . ? C2 C2' C3 112.4 . . ? C2 C2' C3' 114.7 . . ? C3 C2' C3' 5.5 . . ? C2 C2' C1' 12.1 . . ? C3 C2' C1' 106.7 . . ? C3' C2' C1' 108.0 . . ? C2 C2' C7' 118.4 . . ? C3 C2' C7' 127.1 . . ? C3' C2' C7' 126.0 . . ? C1' C2' C7' 126.0 . . ? C2 C2' C7 67.5 . . ? C3 C2' C7 168.4 . . ? C3' C2' C7 173.1 . . ? C1' C2' C7 75.4 . . ? C7' C2' C7 51.0 . . ? C2 C2' C8 159.6 . . ? C3 C2' C8 50.2 . . ? C3' C2' C8 49.2 . . ? C1' C2' C8 156.9 . . ? C7' C2' C8 76.9 . . ? C7 C2' C8 126.9 . . ? C2 C2' Lu1 83.75(9) . . ? C3 C2' Lu1 82.32(9) . . ? C3' C2' Lu1 77.90(9) . . ? C1' C2' Lu1 72.10(9) . . ? C7' C2' Lu1 116.08(8) . . ? C7 C2' Lu1 108.95(9) . . ? C8 C2' Lu1 102.04(9) . . ? C4 C3' C4' 9.5 . . ? C4 C3' C2' 117.2 . . ? C4' C3' C2' 108.0 . . ? C4 C3' C8 157.8 . . ? C4' C3' C8 167.3 . . ? C2' C3' C8 84.0 . . ? C4 C3' C8' 116.8 . . ? C4' C3' C8' 126.0 . . ? C2' C3' C8' 126.0 . . ? C8 C3' C8' 42.2 . . ? C4 C3' C2 96.9 . . ? C4' C3' C2 87.8 . . ? C2' C3' C2 20.5 . . ? C8 C3' C2 103.8 . . ? C8' C3' C2 146.0 . . ? C4 C3' Lu1 81.43(8) . . ? C4' C3' Lu1 75.19(8) . . ? C2' C3' Lu1 70.50(8) . . ? C8 C3' Lu1 113.77(8) . . ? C8' C3' Lu1 120.09(8) . . ? C2 C3' Lu1 67.32(8) . . ? C5 C4' C3' 130.6 . . ? C5 C4' C5' 22.8 . . ? C3' C4' C5' 108.0 . . ? C5 C4' C9' 103.3 . . ? C3' C4' C9' 126.0 . . ? C5' C4' C9' 126.0 . . ? C5 C4' C3 115.2 . . ? C3' C4' C3 15.6 . . ? C5' C4' C3 92.7 . . ? C9' C4' C3 141.1 . . ? C5 C4' C9 138.3 . . ? C3' C4' C9 90.9 . . ? C5' C4' C9 161.1 . . ? C9' C4' C9 35.1 . . ? C3 C4' C9 106.2 . . ? C5 C4' Lu1 83.67(8) . . ? C3' C4' Lu1 73.84(8) . . ? C5' C4' Lu1 71.09(8) . . ? C9' C4' Lu1 120.82(8) . . ? C3 C4' Lu1 70.64(8) . . ? C9 C4' Lu1 115.98(8) . . ? C5 C5' C1 169.2 . . ? C5 C5' C1' 155.0 . . ? C1 C5' C1' 26.6 . . ? C5 C5' C4' 47.5 . . ? C1 C5' C4' 133.5 . . ? C1' C5' C4' 108.0 . . ? C5 C5' C10' 78.7 . . ? C1 C5' C10' 100.1 . . ? C1' C5' C10' 126.0 . . ? C4' C5' C10' 126.0 . . ? C5 C5' C4 53.5 . . ? C1 C5' C4 127.3 . . ? C1' C5' C4 101.9 . . ? C4' C5' C4 6.3 . . ? C10' C5' C4 132.1 . . ? C5 C5' C2 133.5 . . ? C1 C5' C2 46.9 . . ? C1' C5' C2 21.4 . . ? C4' C5' C2 86.9 . . ? C10' C5' C2 146.9 . . ? C4 C5' C2 80.7 . . ? C5 C5' C10 39.4 . . ? C1 C5' C10 139.2 . . ? C1' C5' C10 165.5 . . ? C4' C5' C10 86.5 . . ? C10' C5' C10 39.5 . . ? C4 C5' C10 92.6 . . ? C2 C5' C10 172.4 . . ? C5 C5' Lu1 103.01(9) . . ? C1 C5' Lu1 87.13(9) . . ? C1' C5' Lu1 71.08(8) . . ? C4' C5' Lu1 77.59(9) . . ? C10' C5' Lu1 117.30(8) . . ? C4 C5' Lu1 76.51(9) . . ? C2 C5' Lu1 68.68(8) . . ? C10 C5' Lu1 113.50(8) . . ? C6 C6' C1' 80.2 . . ? C6 C6' C1 54.9 . . ? C1' C6' C1 25.3 . . ? C6 C6' C7 143.4 . . ? C1' C6' C7 64.5 . . ? C1 C6' C7 89.3 . . ? C6 C6' C2 98.8 . . ? C1' C6' C2 19.2 . . ? C1 C6' C2 44.0 . . ? C7 C6' C2 45.4 . . ? C7 C7' C2' 69.2 . . ? C7 C7' C2 50.6 . . ? C2' C7' C2 18.6 . . ? C8 C8' C3' 67.1 . . ? C8 C8' C3 56.2 . . ? C3' C8' C3 11.1 . . ? C9 C9' C4' 81.7 . . ? C9 C9' C4 69.9 . . ? C4' C9' C4 11.9 . . ? C10 C10' C5 66.3 . . ? C10 C10' C5' 88.5 . . ? C5 C10' C5' 22.3 . . ? C10 C10' C1 114.9 . . ? C5 C10' C1 48.7 . . ? C5' C10' C1 26.6 . . ? C10 C10' C6 160.4 . . ? C5 C10' C6 94.3 . . ? C5' C10' C6 72.1 . . ? C1 C10' C6 45.6 . . ? N1 C11 C12 125.8(9) . . ? C11 C12 C13 116.2(9) . . ? C14 C13 C12 119.3(8) . . ? C15 C14 C13 119.3(9) . . ? N1 C15 C14 122.6(9) . . ? N1 C15 C16 114.6(7) . . ? C14 C15 C16 122.6(8) . . ? N2 C16 C17 119.8(8) . . ? N2 C16 C15 115.4(7) . . ? C17 C16 C15 124.6(8) . . ? C16 C17 C18 118.2(8) . . ? C19 C18 C17 120.5(9) . . ? C18 C19 C20 119.1(9) . . ? N2 C20 C19 120.8(8) . . ? N2 C20 C21 113.4(7) . . ? C19 C20 C21 125.7(8) . . ? O1 C21 C20 111.4(7) . . ? O1 C21 C22 113.3(7) . . ? C20 C21 C22 110.4(7) . . ? C21 C22 Si1 114.3(6) . . ? C27 C26 O2 123.5(8) . . ? C27 C26 Si2 122.4(7) . . ? O2 C26 Si2 114.1(6) . . ? _refine_diff_density_max 1.054 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.128