# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address Yu.Chapurina ;Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay UMR 8182, Univ Paris-11 d'Orsay, CNRS, 91405 Orsay, FRANCE. ; R.Guillot ;Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay UMR 8182, Univ Paris-11 d'Orsay, CNRS, 91405 Orsay, FRANCE. ; D.Lyubov ;G. A. Razuvaev Institute of Organometallic Chemistry of Russian Academy of Sciences, Tropinia 49, 603600 Nizhny Novgorod GSP-445, Russia. ; A.Trifonov ;G. A. Razuvaev Institute of Organometallic Chemistry of Russian Academy of Sciences, Tropinia 49, 603600 Nizhny Novgorod GSP-445, Russia. ; J.Hannedouche ;Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay UMR 8182, Univ Paris-11 d'Orsay, CNRS, 91405 Orsay, FRANCE. ; ; E.Schulz ; ;Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay UMR 8182, Univ Paris-11 d'Orsay, CNRS, 91405 Orsay, FRANCE. ; _publ_contact_author_address ;Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay UMR 8182, Univ Paris-11 d'Orsay, CNRS, 91405 Orsay, FRANCE. ; _publ_contact_author_email jerome.hannedouche@u-psud.fr _publ_contact_author_name 'Jerome Hannedouche' data_1270GuillotICMMO _database_code_depnum_ccdc_archive 'CCDC 855071' #TrackingRef _database_code_CSD 'CCDC 855071' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety '(C38 H46 Cl N2 O2 Y), 0.5(C4 H8 O)' _chemical_formula_sum 'C40 H50 Cl1 N2 O2.5 Y1 ' _chemical_properties_physical air-sensitive _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 100(1) _chemical_formula_weight 723.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7960 3.5670 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' _symmetry_int_tables_number 92 _chemical_absolute_configuration ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 10.2349(4) _cell_length_b 10.2349(4) _cell_length_c 68.165(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7140.5(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 8059 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 23.88 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 1.747 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7139 _exptl_absorpt_correction_T_max 0.9189 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'kappa X8 APEX II Bruker ICMMO' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32206 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -77 _diffrn_reflns_limit_l_max 77 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.21 _reflns_number_total 5736 _reflns_number_gt 4926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'Ortep-3 for Windows (L. J. Farrugia, J. Appl. Cryst (1997), 30, 565)' ; _computing_publication_material ; 'WINGX (Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838)' ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+8.1175P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(7) _refine_ls_number_reflns 5736 _refine_ls_number_parameters 404 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1071 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; SIMU 0.040 0.080 1.700 C4 C12 C11 C6 C5 C10 C9 C7 C3 C8 ; 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 C39 C 0.7604(6) 0.6653(7) 0.01435(9) 0.0485(10) Uani 1 1 d D . . H39A H 0.7283 0.6955 0.0270 0.058 Uiso 1 1 calc R . . H39B H 0.8062 0.5833 0.0163 0.058 Uiso 1 1 calc R . . C40 C 0.8474(6) 0.7628(6) 0.00560(9) 0.0485(10) Uani 1 1 d D . . H40A H 0.8929 0.8116 0.0157 0.058 Uiso 1 1 calc R . . H40B H 0.9114 0.7213 -0.0028 0.058 Uiso 1 1 calc R . . O3 O 0.6475(4) 0.6475(4) 0.0000 0.0485(10) Uani 1 2 d SD . . C1 C 0.3547(4) 0.0882(4) 0.91367(7) 0.0152(11) Uani 1 1 d . . . C2 C 0.3554(4) 0.1088(5) 0.93425(7) 0.0152(11) Uani 1 1 d . . . C3 C 0.2680(5) 0.0312(5) 0.94790(7) 0.0149(11) Uani 1 1 d U . . C4 C 0.1671(5) 0.0937(5) 0.95864(7) 0.0171(11) Uani 1 1 d U . . C5 C 0.1067(5) 0.0209(5) 0.97427(7) 0.0181(12) Uani 1 1 d U . . H5 H 0.0407 0.0599 0.9816 0.022 Uiso 1 1 calc R . . C6 C 0.1435(5) -0.1028(5) 0.97858(7) 0.0222(12) Uani 1 1 d U . . H6 H 0.1027 -0.1464 0.9889 0.027 Uiso 1 1 calc R . . C7 C 0.2432(5) -0.1679(5) 0.96775(7) 0.0167(8) Uani 1 1 d U . . C8 C 0.2822(5) -0.2978(5) 0.97235(9) 0.0282(14) Uani 1 1 d U . . H8 H 0.2408 -0.3419 0.9825 0.034 Uiso 1 1 calc R . . C9 C 0.3792(5) -0.3590(5) 0.96215(8) 0.0288(14) Uani 1 1 d U . . H9 H 0.4042 -0.4436 0.9654 0.035 Uiso 1 1 calc R . . C10 C 0.4411(5) -0.2925(5) 0.94661(8) 0.0265(13) Uani 1 1 d U . . H10 H 0.5062 -0.3340 0.9394 0.032 Uiso 1 1 calc R . . C11 C 0.4053(5) -0.1657(5) 0.94199(7) 0.0220(12) Uani 1 1 d U . . H11 H 0.4486 -0.1227 0.9319 0.026 Uiso 1 1 calc R . . C12 C 0.3052(4) -0.0999(5) 0.95219(7) 0.0167(8) Uani 1 1 d U . . C13 C 0.4601(4) 0.1450(5) 0.90250(7) 0.0161(12) Uani 1 1 d . . . H13 H 0.4647 0.1288 0.8891 0.019 Uiso 1 1 calc R . . C14 C 0.5521(5) 0.2208(5) 0.91089(8) 0.0191(12) Uani 1 1 d . . . H14 H 0.6193 0.2542 0.9032 0.023 Uiso 1 1 calc R . . C15 C 0.5488(5) 0.2509(5) 0.93116(8) 0.0178(12) Uani 1 1 d . . . C16 C 0.6416(5) 0.3347(5) 0.93988(7) 0.0223(13) Uani 1 1 d . . . H16 H 0.7057 0.3729 0.9321 0.027 Uiso 1 1 calc R . . C17 C 0.6393(5) 0.3610(5) 0.95954(8) 0.0272(14) Uani 1 1 d . . . H17 H 0.7001 0.4177 0.9650 0.033 Uiso 1 1 calc R . . C18 C 0.5446(5) 0.3017(5) 0.97133(8) 0.0246(13) Uani 1 1 d . . . H18 H 0.5431 0.3185 0.9847 0.030 Uiso 1 1 calc R . . C19 C 0.4541(5) 0.2191(5) 0.96334(7) 0.0174(12) Uani 1 1 d . . . H19 H 0.3928 0.1796 0.9715 0.021 Uiso 1 1 calc R . . C20 C 0.4517(4) 0.1925(4) 0.94296(7) 0.0145(11) Uani 1 1 d . . . C21 C 0.0445(5) 0.2937(5) 0.96577(7) 0.0171(12) Uani 1 1 d . . . H21 H -0.0306 0.2412 0.9699 0.020 Uiso 1 1 calc R . . C22 C -0.0048(5) 0.4176(5) 0.95542(8) 0.0249(13) Uani 1 1 d . . . H22A H 0.0607 0.4501 0.9464 0.030 Uiso 1 1 calc R . . H22B H -0.0840 0.3991 0.9481 0.030 Uiso 1 1 calc R . . C23 C -0.0318(5) 0.5188(5) 0.97149(8) 0.0226(13) Uani 1 1 d . . . H23A H -0.1245 0.5377 0.9723 0.027 Uiso 1 1 calc R . . H23B H 0.0148 0.5994 0.9688 0.027 Uiso 1 1 calc R . . C24 C 0.0174(5) 0.4557(5) 0.99078(8) 0.0276(14) Uani 1 1 d . . . H24A H 0.0620 0.5194 0.9989 0.033 Uiso 1 1 calc R . . H24B H -0.0545 0.4184 0.9982 0.033 Uiso 1 1 calc R . . C25 C 0.1120(5) 0.3489(5) 0.98383(7) 0.0206(12) Uani 1 1 d . . . H25A H 0.1966 0.3854 0.9805 0.025 Uiso 1 1 calc R . . H25B H 0.1233 0.2822 0.9938 0.025 Uiso 1 1 calc R . . C26 C 0.2469(5) 0.0028(5) 0.88441(7) 0.0199(12) Uani 1 1 d . . . H26 H 0.2762 0.0808 0.8773 0.024 Uiso 1 1 calc R . . C27 C 0.1122(6) -0.0352(6) 0.87716(7) 0.0317(14) Uani 1 1 d . . . H27A H 0.0571 0.0414 0.8759 0.038 Uiso 1 1 calc R . . H27B H 0.0710 -0.0957 0.8862 0.038 Uiso 1 1 calc R . . C28 C 0.1337(6) -0.0999(6) 0.85718(8) 0.0362(15) Uani 1 1 d . . . H28A H 0.1174 -0.0386 0.8466 0.043 Uiso 1 1 calc R . . H28B H 0.0768 -0.1749 0.8556 0.043 Uiso 1 1 calc R . . C29 C 0.2779(6) -0.1420(6) 0.85747(8) 0.0397(17) Uani 1 1 d . . . H29A H 0.2855 -0.2344 0.8546 0.048 Uiso 1 1 calc R . . H29B H 0.3273 -0.0933 0.8478 0.048 Uiso 1 1 calc R . . C30 C 0.3291(6) -0.1132(6) 0.87805(8) 0.0342(14) Uani 1 1 d . . . H30A H 0.3161 -0.1873 0.8867 0.041 Uiso 1 1 calc R . . H30B H 0.4212 -0.0911 0.8778 0.041 Uiso 1 1 calc R . . C31 C 0.2835(5) 0.4576(5) 0.91958(8) 0.0224(12) Uani 1 1 d . . . H31A H 0.3777 0.4573 0.9179 0.027 Uiso 1 1 calc R . . H31B H 0.2629 0.4531 0.9335 0.027 Uiso 1 1 calc R . . C32 C 0.2236(6) 0.5747(6) 0.91030(8) 0.0356(16) Uani 1 1 d . . . H32A H 0.2753 0.6524 0.9128 0.043 Uiso 1 1 calc R . . H32B H 0.1354 0.5888 0.9150 0.043 Uiso 1 1 calc R . . C33 C 0.2241(7) 0.5390(6) 0.88840(9) 0.0456(18) Uani 1 1 d . . . H33A H 0.1474 0.5737 0.8819 0.055 Uiso 1 1 calc R . . H33B H 0.3017 0.5726 0.8820 0.055 Uiso 1 1 calc R . . C34 C 0.2230(5) 0.3925(5) 0.88830(7) 0.0261(13) Uani 1 1 d . . . H34A H 0.1456 0.3602 0.8817 0.031 Uiso 1 1 calc R . . H34B H 0.2996 0.3591 0.8816 0.031 Uiso 1 1 calc R . . C35 C -0.0185(5) -0.1386(4) 0.92864(8) 0.0219(13) Uani 1 1 d . . . H35A H 0.0646 -0.1557 0.9350 0.026 Uiso 1 1 calc R . . H35B H -0.0179 -0.1785 0.9157 0.026 Uiso 1 1 calc R . . C36 C -0.1301(5) -0.1918(5) 0.94083(8) 0.0309(14) Uani 1 1 d . . . H36A H -0.1539 -0.2792 0.9367 0.037 Uiso 1 1 calc R . . H36B H -0.1076 -0.1934 0.9547 0.037 Uiso 1 1 calc R . . C37 C -0.2392(5) -0.0960(6) 0.93685(9) 0.0326(15) Uani 1 1 d . . . H37A H -0.3035 -0.0970 0.9473 0.039 Uiso 1 1 calc R . . H37B H -0.2823 -0.1149 0.9245 0.039 Uiso 1 1 calc R . . C38 C -0.1681(6) 0.0333(5) 0.93605(9) 0.0324(14) Uani 1 1 d . . . H38A H -0.2158 0.0959 0.9281 0.039 Uiso 1 1 calc R . . H38B H -0.1565 0.0690 0.9491 0.039 Uiso 1 1 calc R . . N1 N 0.2465(4) 0.0307(4) 0.90565(6) 0.0153(9) Uani 1 1 d . . . N2 N 0.1265(4) 0.2159(4) 0.95280(5) 0.0152(10) Uani 1 1 d . . . O1 O 0.2235(3) 0.3514(3) 0.90890(5) 0.0214(9) Uani 1 1 d . . . O2 O -0.0421(3) 0.0026(3) 0.92714(5) 0.0202(8) Uani 1 1 d . . . Cl Cl -0.08225(12) 0.27746(13) 0.902436(19) 0.0257(3) Uani 1 1 d . . . Y Y 0.10938(5) 0.16957(5) 0.920974(7) 0.01443(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C39 0.056(3) 0.049(3) 0.040(3) -0.011(2) 0.003(2) -0.0201(19) C40 0.056(3) 0.049(3) 0.040(3) -0.011(2) 0.003(2) -0.0201(19) O3 0.056(3) 0.049(3) 0.040(3) -0.011(2) 0.003(2) -0.0201(19) C1 0.011(3) 0.012(3) 0.023(3) 0.000(2) 0.004(2) 0.0037(19) C2 0.013(3) 0.019(3) 0.014(3) 0.001(2) 0.000(2) 0.006(2) C3 0.015(3) 0.017(3) 0.013(3) -0.001(2) -0.004(2) -0.003(2) C4 0.022(3) 0.024(3) 0.006(3) -0.004(2) -0.006(2) -0.006(2) C5 0.015(3) 0.028(3) 0.012(3) -0.001(2) 0.002(2) -0.005(2) C6 0.023(3) 0.030(3) 0.013(3) 0.005(2) 0.000(2) -0.009(2) C7 0.0136(19) 0.022(2) 0.015(2) 0.0001(16) -0.0101(14) -0.0026(15) C8 0.024(3) 0.029(3) 0.032(4) 0.000(3) -0.007(3) -0.007(2) C9 0.034(3) 0.021(3) 0.031(3) 0.007(2) -0.010(3) -0.005(2) C10 0.021(3) 0.025(3) 0.033(4) 0.001(3) -0.005(3) 0.005(2) C11 0.014(3) 0.029(3) 0.023(3) 0.003(3) -0.004(2) -0.002(2) C12 0.0136(19) 0.022(2) 0.015(2) 0.0001(16) -0.0101(14) -0.0026(15) C13 0.016(3) 0.023(3) 0.009(3) 0.003(2) 0.002(2) 0.007(2) C14 0.013(3) 0.025(3) 0.020(3) 0.006(2) 0.006(2) 0.002(2) C15 0.013(3) 0.019(3) 0.021(3) -0.004(2) -0.002(2) 0.005(2) C16 0.021(3) 0.023(3) 0.023(3) 0.005(2) -0.002(2) -0.005(2) C17 0.017(3) 0.026(3) 0.038(4) -0.006(3) -0.005(3) -0.008(2) C18 0.026(3) 0.031(3) 0.016(3) -0.002(2) 0.000(2) -0.004(3) C19 0.017(3) 0.022(3) 0.013(3) 0.001(2) -0.002(2) -0.003(2) C20 0.014(3) 0.012(3) 0.018(3) 0.002(2) 0.000(2) 0.0032(19) C21 0.015(3) 0.021(3) 0.015(3) 0.000(2) 0.005(2) -0.004(2) C22 0.028(3) 0.032(4) 0.014(3) 0.002(3) -0.003(2) 0.006(3) C23 0.021(3) 0.013(3) 0.034(4) -0.001(3) -0.006(3) 0.000(2) C24 0.033(4) 0.026(3) 0.024(4) -0.007(3) 0.002(3) 0.002(3) C25 0.032(3) 0.016(3) 0.014(3) -0.005(2) -0.003(2) 0.004(2) C26 0.032(3) 0.013(3) 0.015(3) -0.003(2) 0.007(2) -0.001(2) C27 0.030(3) 0.050(4) 0.015(3) -0.011(3) -0.002(3) -0.012(3) C28 0.050(4) 0.039(4) 0.019(3) -0.013(3) -0.003(3) -0.010(3) C29 0.066(5) 0.036(4) 0.017(4) -0.012(3) 0.016(3) -0.014(3) C30 0.040(3) 0.031(3) 0.032(4) -0.007(3) 0.000(3) 0.009(3) C31 0.022(3) 0.026(3) 0.019(3) 0.001(3) -0.006(2) -0.004(2) C32 0.045(4) 0.029(4) 0.033(4) 0.000(3) -0.003(3) 0.003(3) C33 0.062(5) 0.037(4) 0.037(4) 0.009(3) -0.010(3) -0.004(3) C34 0.030(3) 0.033(3) 0.015(3) 0.005(3) -0.002(2) -0.012(3) C35 0.035(3) 0.008(3) 0.022(3) 0.001(2) -0.005(2) 0.001(2) C36 0.035(4) 0.029(3) 0.028(3) 0.001(3) -0.004(3) -0.009(3) C37 0.022(3) 0.043(4) 0.033(4) 0.009(3) -0.001(3) -0.011(3) C38 0.024(3) 0.033(3) 0.040(4) 0.003(3) 0.007(3) 0.000(3) N1 0.019(2) 0.017(2) 0.010(2) -0.0006(18) -0.0004(19) -0.0045(17) N2 0.016(2) 0.017(2) 0.013(2) 0.0000(17) 0.0005(18) -0.0010(17) O1 0.028(2) 0.019(2) 0.017(2) 0.0016(16) -0.0041(16) -0.0045(15) O2 0.0116(19) 0.020(2) 0.029(2) -0.0009(16) 0.0013(16) -0.0003(14) Cl 0.0205(7) 0.0376(8) 0.0189(8) 0.0081(6) -0.0025(6) 0.0040(6) Y 0.0151(3) 0.0173(3) 0.0108(2) 0.0001(2) 0.0000(2) -0.0007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C39 C40 1.464(8) . ? C39 O3 1.525(6) . ? C40 C40 1.444(13) 7 ? O3 C39 1.525(6) 7 ? C1 N1 1.369(6) . ? C1 C2 1.419(6) . ? C1 C13 1.443(6) . ? C1 Y 2.692(5) . ? C2 C20 1.434(6) . ? C2 C3 1.516(7) . ? C2 Y 2.747(4) . ? C3 C4 1.418(7) . ? C3 C12 1.425(7) . ? C3 Y 2.830(5) . ? C4 N2 1.377(6) . ? C4 C5 1.439(7) . ? C4 Y 2.747(5) . ? C5 C6 1.353(7) . ? C6 C7 1.425(7) . ? C7 C12 1.419(7) . ? C7 C8 1.424(7) . ? C8 C9 1.364(7) . ? C9 C10 1.409(7) . ? C10 C11 1.385(7) . ? C11 C12 1.409(7) . ? C13 C14 1.347(7) . ? C14 C15 1.416(7) . ? C15 C20 1.412(7) . ? C15 C16 1.412(7) . ? C16 C17 1.367(7) . ? C17 C18 1.398(7) . ? C18 C19 1.367(7) . ? C19 C20 1.415(7) . ? C21 N2 1.456(6) . ? C21 C25 1.520(7) . ? C21 C22 1.537(7) . ? C22 C23 1.532(7) . ? C23 C24 1.549(7) . ? C24 C25 1.535(7) . ? C26 N1 1.476(6) . ? C26 C27 1.515(7) . ? C26 C30 1.518(7) . ? C27 C28 1.531(7) . ? C28 C29 1.537(8) . ? C29 C30 1.526(8) . ? C31 O1 1.445(6) . ? C31 C32 1.488(7) . ? C32 C33 1.537(8) . ? C33 C34 1.499(8) . ? C34 O1 1.466(6) . ? C35 O2 1.469(6) . ? C35 C36 1.513(7) . ? C36 C37 1.511(8) . ? C37 C38 1.511(8) . ? C38 O2 1.460(6) . ? N1 Y 2.254(4) . ? N2 Y 2.227(4) . ? O1 Y 2.346(3) . ? O2 Y 2.345(3) . ? Cl Y 2.5813(13) . ? 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 C40 C39 O3 106.3(5) . . ? C40 C40 C39 105.0(4) 7 . ? C39 O3 C39 103.3(6) . 7 ? N1 C1 C2 117.5(4) . . ? N1 C1 C13 124.6(4) . . ? C2 C1 C13 117.3(4) . . ? N1 C1 Y 56.8(2) . . ? C2 C1 Y 77.0(3) . . ? C13 C1 Y 132.1(3) . . ? C1 C2 C20 120.1(4) . . ? C1 C2 C3 121.8(4) . . ? C20 C2 C3 117.7(4) . . ? C1 C2 Y 72.8(3) . . ? C20 C2 Y 129.1(3) . . ? C3 C2 Y 77.3(2) . . ? C4 C3 C12 120.9(4) . . ? C4 C3 C2 120.7(4) . . ? C12 C3 C2 117.5(4) . . ? C4 C3 Y 72.0(3) . . ? C12 C3 Y 139.2(3) . . ? C2 C3 Y 71.2(2) . . ? N2 C4 C3 118.7(4) . . ? N2 C4 C5 123.7(5) . . ? C3 C4 C5 117.5(5) . . ? N2 C4 Y 53.7(2) . . ? C3 C4 Y 78.5(3) . . ? C5 C4 Y 138.2(3) . . ? C6 C5 C4 121.7(5) . . ? C5 C6 C7 121.6(5) . . ? C12 C7 C8 119.8(5) . . ? C12 C7 C6 118.6(5) . . ? C8 C7 C6 121.6(5) . . ? C9 C8 C7 121.4(5) . . ? C8 C9 C10 119.3(5) . . ? C11 C10 C9 120.3(5) . . ? C10 C11 C12 121.9(5) . . ? C11 C12 C7 117.4(5) . . ? C11 C12 C3 122.9(5) . . ? C7 C12 C3 119.7(5) . . ? C14 C13 C1 122.0(5) . . ? C13 C14 C15 121.5(5) . . ? C20 C15 C16 119.5(5) . . ? C20 C15 C14 118.7(5) . . ? C16 C15 C14 121.8(5) . . ? C17 C16 C15 121.3(5) . . ? C16 C17 C18 119.4(5) . . ? C19 C18 C17 120.6(5) . . ? C18 C19 C20 121.5(5) . . ? C15 C20 C19 117.7(4) . . ? C15 C20 C2 120.0(4) . . ? C19 C20 C2 122.2(4) . . ? N2 C21 C25 115.7(4) . . ? N2 C21 C22 111.2(4) . . ? C25 C21 C22 102.4(4) . . ? C23 C22 C21 106.8(4) . . ? C22 C23 C24 105.5(4) . . ? C25 C24 C23 103.9(4) . . ? C21 C25 C24 103.2(4) . . ? N1 C26 C27 111.5(4) . . ? N1 C26 C30 115.6(4) . . ? C27 C26 C30 102.2(4) . . ? C26 C27 C28 105.7(5) . . ? C27 C28 C29 104.4(4) . . ? C30 C29 C28 106.7(4) . . ? C26 C30 C29 102.9(5) . . ? O1 C31 C32 102.5(4) . . ? C31 C32 C33 102.7(5) . . ? C34 C33 C32 104.0(5) . . ? O1 C34 C33 106.4(4) . . ? O2 C35 C36 105.6(4) . . ? C37 C36 C35 103.1(4) . . ? C36 C37 C38 102.6(4) . . ? O2 C38 C37 104.6(4) . . ? C1 N1 C26 118.2(4) . . ? C1 N1 Y 92.7(3) . . ? C26 N1 Y 125.3(3) . . ? C4 N2 C21 119.7(4) . . ? C4 N2 Y 96.4(3) . . ? C21 N2 Y 131.5(3) . . ? C31 O1 C34 105.5(4) . . ? C31 O1 Y 129.2(3) . . ? C34 O1 Y 124.2(3) . . ? C38 O2 C35 109.1(4) . . ? C38 O2 Y 120.1(3) . . ? C35 O2 Y 128.4(3) . . ? N2 Y N1 122.45(14) . . ? N2 Y O2 91.88(13) . . ? N1 Y O2 91.99(14) . . ? N2 Y O1 97.67(13) . . ? N1 Y O1 91.60(14) . . ? O2 Y O1 165.90(12) . . ? N2 Y Cl 116.45(11) . . ? N1 Y Cl 121.06(10) . . ? O2 Y Cl 84.10(9) . . ? O1 Y Cl 82.37(9) . . ? N2 Y C1 99.94(15) . . ? N1 Y C1 30.53(14) . . ? O2 Y C1 115.11(13) . . ? O1 Y C1 73.50(13) . . ? Cl Y C1 138.63(11) . . ? N2 Y C2 69.83(14) . . ? N1 Y C2 55.90(14) . . ? O2 Y C2 112.46(13) . . ? O1 Y C2 80.72(13) . . ? Cl Y C2 162.66(11) . . ? C1 Y C2 30.22(14) . . ? N2 Y C4 29.88(14) . . ? N1 Y C4 96.94(14) . . ? O2 Y C4 76.63(13) . . ? O1 Y C4 116.43(13) . . ? Cl Y C4 137.90(11) . . ? C1 Y C4 83.39(15) . . ? C2 Y C4 55.31(14) . . ? N2 Y C3 55.24(14) . . ? N1 Y C3 68.15(14) . . ? O2 Y C3 84.16(13) . . ? O1 Y C3 109.81(13) . . ? Cl Y C3 165.33(11) . . ? C1 Y C3 55.27(14) . . ? C2 Y C3 31.50(14) . . ? C4 Y C3 29.41(14) . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.914 _refine_diff_density_max 1.061 _refine_diff_density_min -1.587 _refine_diff_density_rms 0.077 # Attachment '2a.cif' data_1299GuillotICMMO _database_code_depnum_ccdc_archive 'CCDC 855072' #TrackingRef '2a.cif'_database_code_CSD 'CCDC 855072' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C38 H57 N2 O2 Si3 Y, C6 H14' _chemical_formula_sum 'C44 H71 N2 O2 Si3 Y ' _chemical_melting_point ? _exptl_crystal_description plate _exptl_crystal_colour colorless _diffrn_ambient_temperature 100(1) _chemical_formula_weight 833.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0826 0.0707 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7960 3.5670 '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_int_tables_number 1 _chemical_absolute_configuration ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.5117(3) _cell_length_b 13.7159(4) _cell_length_c 17.3224(4) _cell_angle_alpha 78.1130(10) _cell_angle_beta 76.9110(10) _cell_angle_gamma 89.7390(10) _cell_volume 2378.13(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 9986 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.10 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 1.336 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7612 _exptl_absorpt_correction_T_max 0.9742 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'kappa X8 APEX II Bruker ICMMO' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40949 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14886 _reflns_number_gt 12982 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'Ortep-3 for Windows (L. J. Farrugia, J. Appl. Cryst (1997), 30, 565)' ; _computing_publication_material ; 'WINGX (Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838)' ; _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. Restraints were used to correct the geometry of hexane molecules. ; _iucr_refine_instructions_details ; DFIX 2.500 0.002 C88 C86 DFIX 2.500 0.002 C87 C85 DFIX 2.500 0.002 C86 C84 DFIX 2.500 0.002 C83 C85 DFIX 1.500 0.002 C84 C85 DFIX 1.500 0.002 C83 C84 DFIX 1.500 0.002 C85 C86 DFIX 1.500 0.002 C86 C87 DFIX 1.500 0.002 C88 C87 EADP C83 C84 C85 C86 C87 C88 EADP C77 C78 C79 C80 C81 C82 ; _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^)+(0.0575P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(4) _refine_ls_number_reflns 14886 _refine_ls_number_parameters 899 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.004 _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 C35 C 0.7416(6) 0.8661(4) 0.7811(3) 0.0559(15) Uani 1 1 d . . . H35A H 0.6641 0.8332 0.7765 0.084 Uiso 1 1 calc R . . H35B H 0.8124 0.8216 0.7770 0.084 Uiso 1 1 calc R . . H35C H 0.7637 0.9244 0.7383 0.084 Uiso 1 1 calc R . . C36 C 0.6772(6) 0.7823(4) 0.9580(4) 0.0603(16) Uani 1 1 d . . . H36A H 0.6708 0.7951 1.0111 0.090 Uiso 1 1 calc R . . H36B H 0.7469 0.7382 0.9463 0.090 Uiso 1 1 calc R . . H36C H 0.5963 0.7518 0.9560 0.090 Uiso 1 1 calc R . . C37 C 0.8692(5) 0.9573(5) 0.8889(4) 0.0654(18) Uani 1 1 d . . . H37A H 0.8907 1.0194 0.8502 0.098 Uiso 1 1 calc R . . H37B H 0.9372 0.9117 0.8780 0.098 Uiso 1 1 calc R . . H37C H 0.8608 0.9688 0.9426 0.098 Uiso 1 1 calc R . . C38 C 0.5809(4) 0.9927(3) 0.8881(3) 0.0278(9) Uani 1 1 d . . . H38A H 0.5682 1.0049 0.9425 0.033 Uiso 1 1 calc R . . H38B H 0.5030 0.9552 0.8878 0.033 Uiso 1 1 calc R . . C46 C 0.2112(5) 0.7124(4) 0.7063(3) 0.0374(11) Uani 1 1 d . . . H46 H 0.2369 0.6779 0.7520 0.045 Uiso 1 1 calc R . . C59 C 0.5797(4) 0.8725(3) 0.5242(3) 0.0265(8) Uani 1 1 d . . . H59A H 0.4899 0.8476 0.5468 0.032 Uiso 1 1 calc R . . H59B H 0.5837 0.9439 0.5207 0.032 Uiso 1 1 calc R . . C60 C 0.6688(4) 0.8209(3) 0.5766(3) 0.0330(10) Uani 1 1 d . . . H60A H 0.6780 0.8577 0.6174 0.040 Uiso 1 1 calc R . . H60B H 0.6365 0.7533 0.6030 0.040 Uiso 1 1 calc R . . C61 C 0.7963(4) 0.8218(3) 0.5150(3) 0.0331(10) Uani 1 1 d . . . H61A H 0.8523 0.7708 0.5346 0.040 Uiso 1 1 calc R . . H61B H 0.8425 0.8863 0.5018 0.040 Uiso 1 1 calc R . . C62 C 0.7528(4) 0.8001(3) 0.4419(3) 0.0310(9) Uani 1 1 d . . . H62A H 0.8162 0.8276 0.3920 0.037 Uiso 1 1 calc R . . H62B H 0.7410 0.7289 0.4464 0.037 Uiso 1 1 calc R . . C63 C 0.3861(4) 0.7432(3) 0.2053(3) 0.0310(9) Uani 1 1 d . . . H63A H 0.3133 0.7148 0.2497 0.037 Uiso 1 1 calc R . . H63B H 0.4487 0.6920 0.1973 0.037 Uiso 1 1 calc R . . C64 C 0.3392(6) 0.7790(4) 0.1306(3) 0.0520(14) Uani 1 1 d . . . H64A H 0.2489 0.7568 0.1382 0.062 Uiso 1 1 calc R . . H64B H 0.3920 0.7542 0.0857 0.062 Uiso 1 1 calc R . . C65 C 0.3518(5) 0.8917(4) 0.1143(3) 0.0371(11) Uani 1 1 d . . . H65A H 0.3786 0.9196 0.0566 0.045 Uiso 1 1 calc R . . H65B H 0.2697 0.9194 0.1361 0.045 Uiso 1 1 calc R . . C66 C 0.4548(5) 0.9123(3) 0.1569(3) 0.0390(11) Uani 1 1 d . . . H66A H 0.5407 0.9190 0.1204 0.047 Uiso 1 1 calc R . . H66B H 0.4383 0.9733 0.1769 0.047 Uiso 1 1 calc R . . C67 C 0.1767(5) 1.0766(4) 0.4653(3) 0.0440(12) Uani 1 1 d . . . H67A H 0.1016 1.0506 0.4519 0.066 Uiso 1 1 calc R . . H67B H 0.1653 1.1453 0.4681 0.066 Uiso 1 1 calc R . . H67C H 0.1864 1.0391 0.5168 0.066 Uiso 1 1 calc R . . C68 C 0.4731(4) 1.1126(3) 0.4133(3) 0.0327(10) Uani 1 1 d . . . H68A H 0.4695 1.0850 0.4695 0.049 Uiso 1 1 calc R . . H68B H 0.4740 1.1840 0.4046 0.049 Uiso 1 1 calc R . . H68C H 0.5511 1.0926 0.3805 0.049 Uiso 1 1 calc R . . C69 C 0.3093(5) 1.1530(3) 0.2899(3) 0.0383(11) Uani 1 1 d . . . H69A H 0.3771 1.1424 0.2453 0.057 Uiso 1 1 calc R . . H69B H 0.3161 1.2206 0.2960 0.057 Uiso 1 1 calc R . . H69C H 0.2255 1.1404 0.2796 0.057 Uiso 1 1 calc R . . C70 C 0.6417(4) 0.4906(3) 0.4323(3) 0.0340(10) Uani 1 1 d . . . H70A H 0.7044 0.5314 0.4454 0.051 Uiso 1 1 calc R . . H70B H 0.6861 0.4412 0.4055 0.051 Uiso 1 1 calc R . . H70C H 0.5813 0.4582 0.4812 0.051 Uiso 1 1 calc R . . C71 C 0.4210(5) 0.4845(3) 0.3521(3) 0.0347(11) Uani 1 1 d . . . H71A H 0.3634 0.4596 0.4041 0.052 Uiso 1 1 calc R . . H71B H 0.4617 0.4297 0.3309 0.052 Uiso 1 1 calc R . . H71C H 0.3718 0.5198 0.3156 0.052 Uiso 1 1 calc R . . C72 C 0.6674(4) 0.6153(3) 0.2642(3) 0.0319(9) Uani 1 1 d . . . H72A H 0.6213 0.6487 0.2251 0.048 Uiso 1 1 calc R . . H72B H 0.7098 0.5593 0.2459 0.048 Uiso 1 1 calc R . . H72C H 0.7318 0.6607 0.2703 0.048 Uiso 1 1 calc R . . C73 C 0.8386(5) 1.0558(4) 0.3199(3) 0.0419(12) Uani 1 1 d . . . H73A H 0.7644 1.0398 0.3651 0.063 Uiso 1 1 calc R . . H73B H 0.8635 1.1252 0.3106 0.063 Uiso 1 1 calc R . . H73C H 0.9102 1.0163 0.3316 0.063 Uiso 1 1 calc R . . C74 C 0.6839(5) 1.1252(4) 0.1895(4) 0.0552(15) Uani 1 1 d . . . H74A H 0.6663 1.1127 0.1403 0.083 Uiso 1 1 calc R . . H74B H 0.7253 1.1904 0.1790 0.083 Uiso 1 1 calc R . . H74C H 0.6032 1.1219 0.2295 0.083 Uiso 1 1 calc R . . C75 C 0.9518(5) 1.0506(5) 0.1465(4) 0.0568(16) Uani 1 1 d . . . H75A H 1.0163 1.0064 0.1633 0.085 Uiso 1 1 calc R . . H75B H 0.9834 1.1184 0.1377 0.085 Uiso 1 1 calc R . . H75C H 0.9354 1.0379 0.0971 0.085 Uiso 1 1 calc R . . C76 C 0.7175(4) 0.9037(3) 0.2471(3) 0.0327(10) Uani 1 1 d . . . H76A H 0.7829 0.8575 0.2611 0.039 Uiso 1 1 calc R . . H76B H 0.7061 0.8948 0.1949 0.039 Uiso 1 1 calc R . . C77 C 0.4699(12) 0.4899(7) 0.1082(7) 0.1378(19) Uani 1 1 d . . . H77A H 0.4906 0.4216 0.1244 0.207 Uiso 1 1 calc R . . H77B H 0.5040 0.5297 0.1391 0.207 Uiso 1 1 calc R . . H77C H 0.5082 0.5136 0.0516 0.207 Uiso 1 1 calc R . . C78 C 0.3178(13) 0.4978(8) 0.1239(7) 0.1378(19) Uani 1 1 d . . . H78A H 0.2947 0.5569 0.1457 0.165 Uiso 1 1 calc R . . H78B H 0.2934 0.5075 0.0722 0.165 Uiso 1 1 calc R . . C79 C 0.2420(13) 0.4157(8) 0.1770(8) 0.1378(19) Uani 1 1 d . . . H79A H 0.2657 0.4064 0.2289 0.165 Uiso 1 1 calc R . . H79B H 0.2659 0.3564 0.1556 0.165 Uiso 1 1 calc R . . C80 C 0.0986(13) 0.4221(8) 0.1914(8) 0.1378(19) Uani 1 1 d . . . H80A H 0.0758 0.4829 0.2107 0.165 Uiso 1 1 calc R . . H80B H 0.0753 0.4295 0.1395 0.165 Uiso 1 1 calc R . . C81 C 0.0170(13) 0.3414(8) 0.2472(8) 0.1378(19) Uani 1 1 d . . . H81A H 0.0322 0.3367 0.3010 0.165 Uiso 1 1 calc R . . H81B H 0.0408 0.2791 0.2307 0.165 Uiso 1 1 calc R . . C82 C -0.1334(12) 0.3573(7) 0.2503(7) 0.1378(19) Uani 1 1 d . . . H82A H -0.1551 0.4220 0.2610 0.207 Uiso 1 1 calc R . . H82B H -0.1850 0.3070 0.2926 0.207 Uiso 1 1 calc R . . H82C H -0.1512 0.3525 0.1992 0.207 Uiso 1 1 calc R . . C83 C 0.9539(14) 0.8126(10) 0.0974(9) 0.306(9) Uani 1 1 d D . . H83A H 1.0189 0.8618 0.0970 0.460 Uiso 1 1 calc R . . H83B H 0.9176 0.7784 0.1523 0.460 Uiso 1 1 calc R . . H83C H 0.8858 0.8446 0.0743 0.460 Uiso 1 1 calc R . . C84 C 1.0155(13) 0.7390(8) 0.0487(9) 0.306(9) Uani 1 1 d D . . H84A H 0.9512 0.7147 0.0241 0.368 Uiso 1 1 calc R . . H84B H 1.0417 0.6825 0.0847 0.368 Uiso 1 1 calc R . . C85 C 1.1327(15) 0.7828(6) -0.0167(8) 0.306(9) Uani 1 1 d D . . H85A H 1.1035 0.8261 -0.0605 0.368 Uiso 1 1 calc R . . H85B H 1.1856 0.8232 0.0050 0.368 Uiso 1 1 calc R . . C86 C 1.2151(15) 0.7045(7) -0.0497(9) 0.306(9) Uani 1 1 d D . . H86A H 1.2432 0.6607 -0.0057 0.368 Uiso 1 1 calc R . . H86B H 1.1622 0.6645 -0.0718 0.368 Uiso 1 1 calc R . . C87 C 1.3330(15) 0.7474(8) -0.1144(9) 0.306(9) Uani 1 1 d D . . H87A H 1.3836 0.7899 -0.0931 0.368 Uiso 1 1 calc R . . H87B H 1.3048 0.7885 -0.1596 0.368 Uiso 1 1 calc R . . C88 C 1.4187(14) 0.6690(10) -0.1445(9) 0.306(9) Uani 1 1 d D . . H88A H 1.4992 0.6700 -0.1273 0.460 Uiso 1 1 calc R . . H88B H 1.4370 0.6821 -0.2026 0.460 Uiso 1 1 calc R . . H88C H 1.3749 0.6046 -0.1229 0.460 Uiso 1 1 calc R . . O4 O 0.4469(3) 0.8269(2) 0.22399(17) 0.0255(6) Uani 1 1 d . . . Si3 Si 0.71160(14) 0.90326(11) 0.88064(9) 0.0397(3) Uani 1 1 d . . . Si6 Si 0.79516(13) 1.02867(10) 0.22809(9) 0.0377(3) Uani 1 1 d . . . C1 C 0.5616(3) 1.2638(3) 0.6520(2) 0.0201(7) Uani 1 1 d . . . C2 C 0.4876(3) 1.3242(3) 0.7002(2) 0.0175(7) Uani 1 1 d . . . C3 C 0.5415(4) 1.3644(3) 0.7616(2) 0.0200(7) Uani 1 1 d . . . C4 C 0.4899(4) 1.3321(3) 0.8449(3) 0.0246(8) Uani 1 1 d . . . C5 C 0.5229(5) 1.3905(3) 0.8979(3) 0.0359(10) Uani 1 1 d . . . H5 H 0.4855 1.3725 0.9532 0.043 Uiso 1 1 calc R . . C6 C 0.6078(5) 1.4718(3) 0.8695(3) 0.0402(12) Uani 1 1 d . . . H6 H 0.6254 1.5088 0.9055 0.048 Uiso 1 1 calc R . . C7 C 0.6689(5) 1.5005(3) 0.7867(3) 0.0313(10) Uani 1 1 d . . . C8 C 0.7673(5) 1.5778(3) 0.7580(3) 0.0423(13) Uani 1 1 d . . . H8 H 0.7912 1.6112 0.7945 0.051 Uiso 1 1 calc R . . C9 C 0.8278(5) 1.6043(3) 0.6775(3) 0.0394(12) Uani 1 1 d . . . H9 H 0.8920 1.6555 0.6595 0.047 Uiso 1 1 calc R . . C10 C 0.7925(4) 1.5538(3) 0.6226(3) 0.0330(10) Uani 1 1 d . . . H10 H 0.8338 1.5718 0.5679 0.040 Uiso 1 1 calc R . . C11 C 0.6974(3) 1.4778(3) 0.6483(3) 0.0213(8) Uani 1 1 d . . . H11 H 0.6736 1.4461 0.6107 0.026 Uiso 1 1 calc R . . C12 C 0.6351(4) 1.4473(3) 0.7322(2) 0.0229(8) Uani 1 1 d . . . C13 C 0.5153(4) 1.2478(3) 0.5831(2) 0.0214(7) Uani 1 1 d . . . H13 H 0.5639 1.2100 0.5491 0.026 Uiso 1 1 calc R . . C14 C 0.4040(4) 1.2859(3) 0.5664(2) 0.0252(8) Uani 1 1 d . . . H14 H 0.3792 1.2752 0.5204 0.030 Uiso 1 1 calc R . . C15 C 0.3237(4) 1.3419(3) 0.6169(2) 0.0228(8) Uani 1 1 d . . . C16 C 0.2044(4) 1.3783(3) 0.6020(3) 0.0273(9) Uani 1 1 d . . . H16 H 0.1777 1.3663 0.5571 0.033 Uiso 1 1 calc R . . C17 C 0.1276(4) 1.4304(3) 0.6513(3) 0.0331(10) Uani 1 1 d . . . H17 H 0.0486 1.4533 0.6408 0.040 Uiso 1 1 calc R . . C18 C 0.1689(4) 1.4492(3) 0.7186(3) 0.0296(9) Uani 1 1 d . . . H18 H 0.1166 1.4857 0.7523 0.036 Uiso 1 1 calc R . . C19 C 0.2838(4) 1.4154(3) 0.7362(3) 0.0236(8) Uani 1 1 d . . . H19 H 0.3081 1.4283 0.7816 0.028 Uiso 1 1 calc R . . C20 C 0.3671(3) 1.3600(3) 0.6845(2) 0.0204(7) Uani 1 1 d . . . C21 C 0.3858(5) 1.1736(4) 1.0552(3) 0.0371(10) Uani 1 1 d . . . H21A H 0.4458 1.1216 1.0471 0.056 Uiso 1 1 calc R . . H21B H 0.3190 1.1508 1.1036 0.056 Uiso 1 1 calc R . . H21C H 0.4321 1.2312 1.0604 0.056 Uiso 1 1 calc R . . C22 C 0.1909(4) 1.3062(3) 0.9844(3) 0.0350(10) Uani 1 1 d . . . H22A H 0.2357 1.3625 0.9928 0.052 Uiso 1 1 calc R . . H22B H 0.1228 1.2808 1.0316 0.052 Uiso 1 1 calc R . . H22C H 0.1533 1.3263 0.9383 0.052 Uiso 1 1 calc R . . C23 C 0.2192(4) 1.0920(3) 0.9623(3) 0.0312(9) Uani 1 1 d . . . H23A H 0.1590 1.1090 0.9279 0.047 Uiso 1 1 calc R . . H23B H 0.1720 1.0611 1.0160 0.047 Uiso 1 1 calc R . . H23C H 0.2805 1.0466 0.9411 0.047 Uiso 1 1 calc R . . C24 C 0.9294(4) 1.1407(4) 0.6622(3) 0.0428(12) Uani 1 1 d . . . H24A H 0.9727 1.1948 0.6749 0.064 Uiso 1 1 calc R . . H24B H 0.9926 1.1057 0.6300 0.064 Uiso 1 1 calc R . . H24C H 0.8868 1.0958 0.7115 0.064 Uiso 1 1 calc R . . C25 C 0.8785(5) 1.3030(3) 0.5289(3) 0.0390(11) Uani 1 1 d . . . H25A H 0.8144 1.3316 0.5003 0.059 Uiso 1 1 calc R . . H25B H 0.9521 1.2852 0.4911 0.059 Uiso 1 1 calc R . . H25C H 0.9066 1.3507 0.5557 0.059 Uiso 1 1 calc R . . C26 C 0.7804(5) 1.0916(4) 0.5484(3) 0.0431(12) Uani 1 1 d . . . H26A H 0.7342 1.0347 0.5861 0.065 Uiso 1 1 calc R . . H26B H 0.8636 1.0723 0.5211 0.065 Uiso 1 1 calc R . . H26C H 0.7302 1.1173 0.5094 0.065 Uiso 1 1 calc R . . C27 C 0.4481(4) 0.9912(4) 0.7167(3) 0.0393(11) Uani 1 1 d . . . H27A H 0.4560 0.9311 0.7559 0.047 Uiso 1 1 calc R . . H27B H 0.5316 1.0072 0.6781 0.047 Uiso 1 1 calc R . . C28 C 0.3445(5) 0.9756(4) 0.6741(4) 0.0482(13) Uani 1 1 d . . . H28A H 0.3311 0.9056 0.6745 0.058 Uiso 1 1 calc R . . H28B H 0.3651 1.0132 0.6185 0.058 Uiso 1 1 calc R . . C29 C 0.2288(5) 1.0144(6) 0.7238(6) 0.0482(13) Uani 1 1 d . . . H29A H 0.1651 1.0362 0.6919 0.058 Uiso 1 1 calc R . . H29B H 0.1877 0.9634 0.7704 0.058 Uiso 1 1 calc R . . C30 C 0.2797(4) 1.0980(3) 0.7492(3) 0.0264(8) Uani 1 1 d . . . H30A H 0.2261 1.1067 0.8007 0.032 Uiso 1 1 calc R . . H30B H 0.2817 1.1592 0.7091 0.032 Uiso 1 1 calc R . . C31 C 0.7411(5) 1.1852(4) 0.9399(3) 0.0402(12) Uani 1 1 d . . . H31A H 0.7212 1.1149 0.9635 0.048 Uiso 1 1 calc R . . H31B H 0.6782 1.2239 0.9698 0.048 Uiso 1 1 calc R . . C32 C 0.8791(6) 1.2141(6) 0.9419(4) 0.082(3) Uani 1 1 d . . . H32A H 0.8785 1.2619 0.9761 0.099 Uiso 1 1 calc R . . H32B H 0.9244 1.1559 0.9620 0.099 Uiso 1 1 calc R . . C33 C 0.9428(10) 1.2593(11) 0.8555(6) 0.082(3) Uani 1 1 d . . . H33A H 0.9922 1.3202 0.8524 0.099 Uiso 1 1 calc R . . H33B H 1.0021 1.2133 0.8320 0.099 Uiso 1 1 calc R . . C34 C 0.8442(4) 1.2797(3) 0.8146(3) 0.0361(11) Uani 1 1 d . . . H34A H 0.8748 1.2743 0.7585 0.043 Uiso 1 1 calc R . . H34B H 0.8150 1.3467 0.8158 0.043 Uiso 1 1 calc R . . C39 C 0.2518(3) 0.8794(3) 0.3725(2) 0.0225(8) Uani 1 1 d . . . C40 C 0.2423(3) 0.7796(3) 0.4128(2) 0.0207(7) Uani 1 1 d . . . C41 C 0.3069(4) 0.7413(3) 0.4809(2) 0.0234(8) Uani 1 1 d . . . C42 C 0.4148(4) 0.6818(3) 0.4707(2) 0.0221(8) Uani 1 1 d . . . C43 C 0.4553(4) 0.6331(3) 0.5432(3) 0.0273(9) Uani 1 1 d . . . H43 H 0.5279 0.5939 0.5382 0.033 Uiso 1 1 calc R . . C44 C 0.3903(4) 0.6429(3) 0.6183(3) 0.0292(9) Uani 1 1 d . . . H44 H 0.4183 0.6090 0.6633 0.035 Uiso 1 1 calc R . . C45 C 0.2807(4) 0.7036(3) 0.6299(3) 0.0285(9) Uani 1 1 d . . . C47 C 0.1055(5) 0.7712(4) 0.7154(3) 0.0389(11) Uani 1 1 d . . . H47 H 0.0597 0.7767 0.7669 0.047 Uiso 1 1 calc R . . C48 C 0.0676(4) 0.8221(3) 0.6475(3) 0.0332(10) Uani 1 1 d . . . H48 H -0.0032 0.8631 0.6536 0.040 Uiso 1 1 calc R . . C49 C 0.1309(4) 0.8137(3) 0.5723(3) 0.0288(9) Uani 1 1 d . . . H49 H 0.1018 0.8482 0.5279 0.035 Uiso 1 1 calc R . . C50 C 0.2394(4) 0.7543(3) 0.5596(2) 0.0228(8) Uani 1 1 d . . . C51 C 0.1677(4) 0.9116(3) 0.3184(3) 0.0277(9) Uani 1 1 d . . . H51 H 0.1713 0.9783 0.2924 0.033 Uiso 1 1 calc R . . C52 C 0.0834(4) 0.8470(4) 0.3044(3) 0.0319(10) Uani 1 1 d . . . H52 H 0.0284 0.8709 0.2703 0.038 Uiso 1 1 calc R . . C53 C 0.0761(4) 0.7444(4) 0.3400(3) 0.0316(10) Uani 1 1 d . . . C54 C -0.0061(4) 0.6760(4) 0.3218(3) 0.0366(11) Uani 1 1 d . . . H54 H -0.0558 0.6980 0.2839 0.044 Uiso 1 1 calc R . . C55 C -0.0133(4) 0.5785(4) 0.3589(3) 0.0431(12) Uani 1 1 d . . . H55 H -0.0663 0.5337 0.3453 0.052 Uiso 1 1 calc R . . C56 C 0.0578(4) 0.5445(4) 0.4172(3) 0.0371(11) Uani 1 1 d . . . H56 H 0.0506 0.4775 0.4429 0.044 Uiso 1 1 calc R . . C57 C 0.1393(4) 0.6100(3) 0.4371(3) 0.0290(9) Uani 1 1 d . . . H57 H 0.1855 0.5868 0.4766 0.035 Uiso 1 1 calc R . . C58 C 0.1523(4) 0.7103(3) 0.3980(3) 0.0271(9) Uani 1 1 d . . . N1 N 0.4179(3) 1.2420(2) 0.8746(2) 0.0221(7) Uani 1 1 d . . . N2 N 0.6717(3) 1.2172(2) 0.6719(2) 0.0205(6) Uani 1 1 d . . . N3 N 0.3506(3) 0.9439(2) 0.3781(2) 0.0220(7) Uani 1 1 d . . . N4 N 0.4844(3) 0.6755(2) 0.3943(2) 0.0219(7) Uani 1 1 d . . . O1 O 0.4114(3) 1.0724(2) 0.75706(17) 0.0242(6) Uani 1 1 d . . . O2 O 0.7381(3) 1.2066(2) 0.85586(18) 0.0303(7) Uani 1 1 d . . . O3 O 0.6280(3) 0.8493(2) 0.44443(17) 0.0240(6) Uani 1 1 d . . . Si1 Si 0.30875(12) 1.20711(9) 0.96595(7) 0.0257(2) Uani 1 1 d . . . Si2 Si 0.80620(11) 1.19059(8) 0.60457(7) 0.0224(2) Uani 1 1 d . . . Si4 Si 0.32690(12) 1.06611(9) 0.38503(8) 0.0255(2) Uani 1 1 d . . . Si5 Si 0.55001(11) 0.57107(8) 0.36335(7) 0.0242(2) Uani 1 1 d . . . Y1 Y 0.56614(6) 1.15562(3) 0.80316(3) 0.02048(9) Uani 1 1 d . . . Y2 Y 0.51292(6) 0.84070(3) 0.34390(3) 0.02012(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C35 0.059(3) 0.050(3) 0.043(3) 0.011(3) 0.003(3) 0.027(3) C36 0.072(4) 0.049(3) 0.049(4) 0.010(3) -0.009(3) 0.022(3) C37 0.042(3) 0.081(4) 0.073(4) 0.002(4) -0.027(3) 0.021(3) C38 0.0228(18) 0.0259(19) 0.029(2) 0.0062(18) -0.0052(18) -0.0003(16) C46 0.053(3) 0.035(2) 0.021(2) -0.002(2) -0.007(2) -0.007(2) C59 0.0245(18) 0.0244(19) 0.029(2) -0.0006(18) -0.0064(18) -0.0016(15) C60 0.037(2) 0.033(2) 0.033(3) -0.003(2) -0.020(2) -0.0053(19) C61 0.027(2) 0.0231(19) 0.048(3) 0.009(2) -0.022(2) -0.0024(16) C62 0.0204(18) 0.032(2) 0.042(3) -0.007(2) -0.0109(19) 0.0050(16) C63 0.031(2) 0.031(2) 0.031(3) -0.001(2) -0.0132(19) 0.0025(18) C64 0.075(4) 0.048(3) 0.036(3) 0.000(3) -0.027(3) -0.017(3) C65 0.041(2) 0.046(3) 0.018(2) 0.011(2) -0.010(2) -0.006(2) C66 0.051(3) 0.036(2) 0.026(3) 0.011(2) -0.017(2) -0.011(2) C67 0.034(2) 0.039(3) 0.053(3) -0.010(2) 0.003(2) 0.014(2) C68 0.037(2) 0.025(2) 0.037(3) -0.004(2) -0.012(2) 0.0046(18) C69 0.040(2) 0.032(2) 0.042(3) 0.000(2) -0.015(2) 0.007(2) C70 0.032(2) 0.030(2) 0.040(3) -0.001(2) -0.017(2) 0.0095(18) C71 0.034(2) 0.026(2) 0.047(3) -0.009(2) -0.014(2) -0.0022(19) C72 0.0261(19) 0.040(2) 0.033(3) -0.009(2) -0.0129(19) 0.0107(18) C73 0.031(2) 0.037(2) 0.052(3) 0.008(2) -0.013(2) -0.0035(19) C74 0.044(3) 0.052(3) 0.054(4) 0.029(3) -0.016(3) -0.004(2) C75 0.027(2) 0.073(4) 0.052(4) 0.019(3) -0.003(2) -0.015(2) C76 0.0170(17) 0.045(3) 0.029(3) 0.006(2) -0.0020(17) -0.0030(17) C77 0.193(5) 0.087(3) 0.159(5) -0.039(3) -0.079(5) 0.015(4) C78 0.193(5) 0.087(3) 0.159(5) -0.039(3) -0.079(5) 0.015(4) C79 0.193(5) 0.087(3) 0.159(5) -0.039(3) -0.079(5) 0.015(4) C80 0.193(5) 0.087(3) 0.159(5) -0.039(3) -0.079(5) 0.015(4) C81 0.193(5) 0.087(3) 0.159(5) -0.039(3) -0.079(5) 0.015(4) C82 0.193(5) 0.087(3) 0.159(5) -0.039(3) -0.079(5) 0.015(4) C83 0.469(18) 0.167(8) 0.378(17) 0.021(9) -0.360(16) -0.077(11) C84 0.469(18) 0.167(8) 0.378(17) 0.021(9) -0.360(16) -0.077(11) C85 0.469(18) 0.167(8) 0.378(17) 0.021(9) -0.360(16) -0.077(11) C86 0.469(18) 0.167(8) 0.378(17) 0.021(9) -0.360(16) -0.077(11) C87 0.469(18) 0.167(8) 0.378(17) 0.021(9) -0.360(16) -0.077(11) C88 0.469(18) 0.167(8) 0.378(17) 0.021(9) -0.360(16) -0.077(11) O4 0.0252(13) 0.0261(14) 0.0233(16) 0.0027(12) -0.0090(12) -0.0017(11) Si3 0.0365(7) 0.0409(7) 0.0324(8) 0.0100(6) -0.0056(6) 0.0156(6) Si6 0.0209(5) 0.0454(7) 0.0344(8) 0.0149(6) -0.0020(5) -0.0062(5) C1 0.0182(16) 0.0179(16) 0.022(2) 0.0011(16) -0.0061(15) -0.0048(13) C2 0.0143(14) 0.0196(16) 0.0164(19) 0.0030(15) -0.0050(14) -0.0018(13) C3 0.0192(16) 0.0185(17) 0.023(2) -0.0028(16) -0.0080(16) -0.0020(14) C4 0.026(2) 0.0230(18) 0.024(2) -0.0006(17) -0.0084(18) -0.0025(16) C5 0.049(3) 0.033(2) 0.028(3) -0.006(2) -0.014(2) -0.011(2) C6 0.057(3) 0.034(2) 0.033(3) -0.002(2) -0.022(2) -0.015(2) C7 0.041(3) 0.020(2) 0.036(3) -0.002(2) -0.019(2) -0.0065(18) C8 0.054(3) 0.026(2) 0.054(3) 0.003(2) -0.036(3) -0.013(2) C9 0.041(3) 0.029(2) 0.049(3) 0.004(2) -0.023(2) -0.016(2) C10 0.027(2) 0.028(2) 0.042(3) 0.007(2) -0.017(2) -0.0036(17) C11 0.0174(16) 0.0178(17) 0.027(2) -0.0001(16) -0.0063(16) -0.0005(13) C12 0.0239(18) 0.0166(16) 0.028(2) 0.0040(16) -0.0131(17) -0.0031(14) C13 0.0251(18) 0.0217(17) 0.016(2) 0.0005(16) -0.0060(16) 0.0004(14) C14 0.0272(19) 0.0258(19) 0.026(2) -0.0041(17) -0.0145(17) -0.0006(16) C15 0.0217(17) 0.0176(17) 0.026(2) 0.0065(16) -0.0088(16) -0.0066(14) C16 0.0238(18) 0.027(2) 0.032(2) 0.0024(18) -0.0148(18) -0.0011(16) C17 0.0191(18) 0.031(2) 0.045(3) 0.005(2) -0.0111(19) 0.0039(16) C18 0.0228(18) 0.0236(19) 0.038(3) -0.0022(19) -0.0022(18) 0.0009(15) C19 0.0228(17) 0.0193(17) 0.025(2) 0.0023(16) -0.0039(16) -0.0034(14) C20 0.0182(16) 0.0147(15) 0.026(2) 0.0021(15) -0.0051(15) -0.0022(13) C21 0.039(2) 0.045(3) 0.024(2) -0.001(2) -0.007(2) -0.002(2) C22 0.029(2) 0.039(2) 0.036(3) -0.012(2) -0.002(2) 0.0048(19) C23 0.028(2) 0.037(2) 0.025(2) -0.004(2) -0.0013(18) -0.0032(18) C24 0.026(2) 0.065(3) 0.036(3) -0.004(3) -0.009(2) 0.020(2) C25 0.032(2) 0.036(2) 0.037(3) 0.004(2) 0.007(2) -0.0016(19) C26 0.029(2) 0.039(3) 0.058(3) -0.022(3) 0.007(2) -0.0035(19) C27 0.032(2) 0.040(2) 0.056(3) -0.023(2) -0.018(2) 0.0102(19) C28 0.048(3) 0.045(3) 0.066(4) -0.030(3) -0.026(3) 0.013(2) C29 0.048(3) 0.045(3) 0.066(4) -0.030(3) -0.026(3) 0.013(2) C30 0.0160(16) 0.030(2) 0.033(2) -0.0036(19) -0.0078(16) 0.0043(15) C31 0.035(2) 0.058(3) 0.023(2) 0.010(2) -0.014(2) -0.016(2) C32 0.059(4) 0.132(6) 0.046(4) 0.035(4) -0.036(3) -0.061(4) C33 0.059(4) 0.132(6) 0.046(4) 0.035(4) -0.036(3) -0.061(4) C34 0.035(2) 0.038(2) 0.030(3) 0.010(2) -0.011(2) -0.015(2) C39 0.0136(15) 0.0296(19) 0.023(2) -0.0037(17) -0.0037(15) 0.0035(14) C40 0.0111(14) 0.0286(19) 0.022(2) -0.0043(17) -0.0032(14) 0.0006(14) C41 0.0203(17) 0.0240(18) 0.024(2) 0.0047(17) -0.0088(16) -0.0045(15) C42 0.0213(17) 0.0211(17) 0.023(2) 0.0019(16) -0.0098(16) -0.0064(14) C43 0.030(2) 0.0197(18) 0.031(2) 0.0030(18) -0.0123(19) -0.0037(16) C44 0.039(2) 0.0230(19) 0.023(2) 0.0080(18) -0.0113(19) -0.0081(17) C45 0.038(2) 0.0215(19) 0.024(2) 0.0020(18) -0.0082(19) -0.0076(17) C47 0.045(3) 0.044(3) 0.026(3) -0.011(2) -0.001(2) -0.015(2) C48 0.027(2) 0.039(2) 0.031(3) -0.007(2) -0.0005(19) -0.0056(18) C49 0.0228(18) 0.032(2) 0.029(2) -0.0037(19) -0.0027(18) -0.0047(16) C50 0.0233(18) 0.0221(18) 0.018(2) 0.0049(17) -0.0032(16) -0.0087(15) C51 0.0193(17) 0.036(2) 0.026(2) 0.0003(19) -0.0084(17) 0.0050(16) C52 0.0153(17) 0.048(3) 0.033(3) -0.006(2) -0.0080(17) 0.0066(17) C53 0.0148(17) 0.046(3) 0.035(3) -0.007(2) -0.0109(18) 0.0021(17) C54 0.0173(18) 0.053(3) 0.046(3) -0.019(2) -0.0144(19) 0.0027(18) C55 0.023(2) 0.053(3) 0.060(4) -0.026(3) -0.011(2) -0.005(2) C56 0.024(2) 0.038(2) 0.046(3) -0.007(2) -0.004(2) -0.0121(18) C57 0.0216(18) 0.029(2) 0.033(3) -0.003(2) -0.0034(18) -0.0055(16) C58 0.0153(16) 0.040(2) 0.026(2) -0.0069(19) -0.0045(16) -0.0009(16) N1 0.0245(15) 0.0203(15) 0.0199(18) 0.0007(14) -0.0064(14) -0.0022(13) N2 0.0165(13) 0.0210(15) 0.0237(18) -0.0021(14) -0.0065(13) 0.0015(12) N3 0.0160(14) 0.0239(16) 0.0238(18) 0.0018(14) -0.0060(13) 0.0006(12) N4 0.0180(14) 0.0237(16) 0.0233(18) -0.0007(14) -0.0069(13) -0.0009(12) O1 0.0208(12) 0.0240(13) 0.0277(16) -0.0052(12) -0.0056(12) 0.0025(11) O2 0.0228(13) 0.0384(16) 0.0273(17) 0.0049(14) -0.0113(13) -0.0068(12) O3 0.0176(12) 0.0255(14) 0.0296(16) -0.0023(13) -0.0100(12) 0.0005(10) Si1 0.0248(5) 0.0301(6) 0.0210(6) -0.0026(5) -0.0053(5) -0.0004(4) Si2 0.0175(5) 0.0226(5) 0.0247(6) -0.0002(5) -0.0040(4) 0.0011(4) Si4 0.0221(5) 0.0241(5) 0.0274(6) 0.0004(5) -0.0052(5) 0.0052(4) Si5 0.0202(5) 0.0235(5) 0.0286(7) -0.0003(5) -0.0097(5) 0.0013(4) Y1 0.01650(17) 0.02301(19) 0.0203(2) 0.00119(16) -0.00620(15) 0.00015(14) Y2 0.01413(16) 0.02157(18) 0.0219(2) 0.00251(16) -0.00489(15) -0.00007(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C35 Si3 1.857(6) . ? C36 Si3 1.884(6) . ? C37 Si3 1.864(6) . ? C38 Si3 1.839(4) . ? C38 Y1 2.434(4) . ? C46 C47 1.369(7) . ? C46 C45 1.388(6) . ? C59 O3 1.460(5) . ? C59 C60 1.521(5) . ? C60 C61 1.511(7) . ? C61 C62 1.523(6) . ? C62 O3 1.469(4) . ? C63 O4 1.444(5) . ? C63 C64 1.477(6) . ? C64 C65 1.514(7) . ? C65 C66 1.498(6) . ? C66 O4 1.459(5) . ? C67 Si4 1.879(5) . ? C68 Si4 1.868(4) . ? C69 Si4 1.870(5) . ? C70 Si5 1.882(4) . ? C71 Si5 1.876(4) . ? C72 Si5 1.860(5) . ? C73 Si6 1.858(5) . ? C74 Si6 1.883(5) . ? C75 Si6 1.891(5) . ? C76 Si6 1.836(5) . ? C76 Y2 2.444(4) . ? C77 C78 1.567(15) . ? C78 C79 1.414(15) . ? C79 C80 1.477(15) . ? C80 C81 1.445(15) . ? C81 C82 1.585(14) . ? C83 C84 1.499(2) . ? C84 C85 1.502(2) . ? C85 C86 1.500(2) . ? C86 C87 1.498(2) . ? C87 C88 1.500(2) . ? O4 Y2 2.377(3) . ? C1 N2 1.397(4) . ? C1 C2 1.404(5) . ? C1 C13 1.443(5) . ? C1 Y1 2.741(4) . ? C2 C20 1.420(5) . ? C2 C3 1.508(5) . ? C2 Y1 2.857(3) . ? C3 C4 1.400(6) . ? C3 C12 1.437(5) . ? C3 Y1 2.831(4) . ? C4 N1 1.391(5) . ? C4 C5 1.433(5) . ? C4 Y1 2.733(4) . ? C5 C6 1.366(6) . ? C6 C7 1.406(7) . ? C7 C12 1.410(6) . ? C7 C8 1.414(6) . ? C8 C9 1.368(8) . ? C9 C10 1.399(6) . ? C10 C11 1.379(5) . ? C11 C12 1.427(6) . ? C13 C14 1.346(5) . ? C14 C15 1.416(6) . ? C15 C16 1.406(5) . ? C15 C20 1.416(5) . ? C16 C17 1.350(6) . ? C17 C18 1.403(6) . ? C18 C19 1.367(5) . ? C19 C20 1.437(5) . ? C21 Si1 1.878(4) . ? C22 Si1 1.862(4) . ? C23 Si1 1.861(4) . ? C24 Si2 1.854(4) . ? C25 Si2 1.844(5) . ? C26 Si2 1.878(5) . ? C27 O1 1.440(5) . ? C27 C28 1.486(6) . ? C28 C29 1.487(8) . ? C29 C30 1.455(7) . ? C30 O1 1.456(4) . ? C31 O2 1.433(5) . ? C31 C32 1.515(6) . ? C32 C33 1.496(10) . ? C33 C34 1.380(8) . ? C34 O2 1.454(5) . ? C39 C40 1.395(5) . ? C39 N3 1.399(5) . ? C39 C51 1.435(5) . ? C39 Y2 2.745(3) . ? C40 C58 1.442(5) . ? C40 C41 1.495(5) . ? C40 Y2 2.880(3) . ? C41 C42 1.394(5) . ? C41 C50 1.434(6) . ? C41 Y2 2.924(4) . ? C42 N4 1.379(5) . ? C42 C43 1.448(5) . ? C42 Y2 2.768(4) . ? C43 C44 1.359(6) . ? C44 C45 1.420(6) . ? C45 C50 1.429(6) . ? C47 C48 1.379(7) . ? C48 C49 1.349(6) . ? C49 C50 1.402(6) . ? C51 C52 1.349(6) . ? C52 C53 1.410(7) . ? C53 C54 1.407(6) . ? C53 C58 1.428(6) . ? C54 C55 1.354(7) . ? C55 C56 1.393(7) . ? C56 C57 1.389(6) . ? C57 C58 1.395(6) . ? N1 Si1 1.709(4) . ? N1 Y1 2.254(3) . ? N2 Si2 1.708(3) . ? N2 Y1 2.278(3) . ? N3 Si4 1.718(3) . ? N3 Y2 2.265(3) . ? N4 Si5 1.719(3) . ? N4 Y2 2.249(3) . ? O1 Y1 2.359(3) . ? O2 Y1 2.369(3) . ? O3 Y2 2.356(3) . ? 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 Si3 C38 Y1 130.2(2) . . ? C47 C46 C45 121.0(4) . . ? O3 C59 C60 105.8(3) . . ? C61 C60 C59 102.0(3) . . ? C60 C61 C62 103.2(3) . . ? O3 C62 C61 103.8(3) . . ? O4 C63 C64 108.2(4) . . ? C63 C64 C65 105.8(4) . . ? C66 C65 C64 104.1(4) . . ? O4 C66 C65 105.7(3) . . ? Si6 C76 Y2 126.8(2) . . ? C79 C78 C77 116.4(10) . . ? C78 C79 C80 116.7(11) . . ? C81 C80 C79 118.7(11) . . ? C80 C81 C82 111.7(10) . . ? C63 O4 C66 108.5(3) . . ? C63 O4 Y2 129.7(2) . . ? C66 O4 Y2 121.6(2) . . ? C38 Si3 C35 110.2(2) . . ? C38 Si3 C37 112.0(2) . . ? C35 Si3 C37 107.1(3) . . ? C38 Si3 C36 115.5(2) . . ? C35 Si3 C36 104.8(3) . . ? C37 Si3 C36 106.6(3) . . ? C76 Si6 C73 112.2(2) . . ? C76 Si6 C74 109.8(2) . . ? C73 Si6 C74 110.3(3) . . ? C76 Si6 C75 114.4(3) . . ? C73 Si6 C75 105.6(2) . . ? C74 Si6 C75 104.3(3) . . ? N2 C1 C2 121.6(3) . . ? N2 C1 C13 121.2(3) . . ? C2 C1 C13 117.1(3) . . ? N2 C1 Y1 56.04(18) . . ? C2 C1 Y1 80.1(2) . . ? C13 C1 Y1 136.7(3) . . ? C1 C2 C20 120.3(3) . . ? C1 C2 C3 121.3(3) . . ? C20 C2 C3 117.9(3) . . ? C1 C2 Y1 71.0(2) . . ? C20 C2 Y1 135.7(2) . . ? C3 C2 Y1 73.66(19) . . ? C4 C3 C12 120.1(3) . . ? C4 C3 C2 121.5(3) . . ? C12 C3 C2 117.8(3) . . ? C4 C3 Y1 71.6(2) . . ? C12 C3 Y1 133.1(2) . . ? C2 C3 Y1 75.58(19) . . ? N1 C4 C3 120.2(3) . . ? N1 C4 C5 121.8(4) . . ? C3 C4 C5 117.8(4) . . ? N1 C4 Y1 55.34(19) . . ? C3 C4 Y1 79.3(2) . . ? C5 C4 Y1 135.5(3) . . ? C6 C5 C4 121.8(4) . . ? C5 C6 C7 121.2(4) . . ? C6 C7 C12 118.7(4) . . ? C6 C7 C8 121.5(4) . . ? C12 C7 C8 119.8(5) . . ? C9 C8 C7 121.1(4) . . ? C8 C9 C10 119.6(4) . . ? C11 C10 C9 121.0(5) . . ? C10 C11 C12 120.4(4) . . ? C7 C12 C11 118.0(4) . . ? C7 C12 C3 120.2(4) . . ? C11 C12 C3 121.8(3) . . ? C14 C13 C1 122.1(4) . . ? C13 C14 C15 121.7(3) . . ? C16 C15 C20 120.2(4) . . ? C16 C15 C14 122.2(4) . . ? C20 C15 C14 117.6(3) . . ? C17 C16 C15 121.7(4) . . ? C16 C17 C18 119.0(4) . . ? C19 C18 C17 121.9(4) . . ? C18 C19 C20 120.1(4) . . ? C15 C20 C2 121.0(3) . . ? C15 C20 C19 117.1(3) . . ? C2 C20 C19 121.9(3) . . ? O1 C27 C28 107.6(3) . . ? C27 C28 C29 101.7(4) . . ? C30 C29 C28 105.2(4) . . ? C29 C30 O1 105.3(3) . . ? O2 C31 C32 105.3(4) . . ? C33 C32 C31 104.5(4) . . ? C34 C33 C32 107.0(7) . . ? C33 C34 O2 106.5(4) . . ? C40 C39 N3 120.6(3) . . ? C40 C39 C51 118.4(3) . . ? N3 C39 C51 120.6(4) . . ? C40 C39 Y2 81.1(2) . . ? N3 C39 Y2 55.39(17) . . ? C51 C39 Y2 131.6(3) . . ? C39 C40 C58 120.4(3) . . ? C39 C40 C41 123.2(3) . . ? C58 C40 C41 115.8(3) . . ? C39 C40 Y2 70.4(2) . . ? C58 C40 Y2 134.7(3) . . ? C41 C40 Y2 76.7(2) . . ? C42 C41 C50 121.5(3) . . ? C42 C41 C40 121.3(4) . . ? C50 C41 C40 116.3(3) . . ? C42 C41 Y2 69.7(2) . . ? C50 C41 Y2 139.4(3) . . ? C40 C41 Y2 73.5(2) . . ? N4 C42 C41 120.9(3) . . ? N4 C42 C43 121.9(3) . . ? C41 C42 C43 117.1(4) . . ? N4 C42 Y2 53.83(18) . . ? C41 C42 Y2 82.1(2) . . ? C43 C42 Y2 134.8(2) . . ? C44 C43 C42 122.0(4) . . ? C43 C44 C45 121.8(4) . . ? C46 C45 C44 122.5(4) . . ? C46 C45 C50 119.7(4) . . ? C44 C45 C50 117.8(4) . . ? C46 C47 C48 119.3(4) . . ? C49 C48 C47 121.4(4) . . ? C48 C49 C50 121.6(4) . . ? C49 C50 C45 117.0(4) . . ? C49 C50 C41 123.2(4) . . ? C45 C50 C41 119.8(4) . . ? C52 C51 C39 121.4(4) . . ? C51 C52 C53 122.0(4) . . ? C54 C53 C52 122.1(4) . . ? C54 C53 C58 119.6(4) . . ? C52 C53 C58 118.3(4) . . ? C55 C54 C53 120.4(4) . . ? C54 C55 C56 120.7(4) . . ? C57 C56 C55 120.4(4) . . ? C56 C57 C58 120.3(4) . . ? C57 C58 C53 118.5(4) . . ? C57 C58 C40 122.3(4) . . ? C53 C58 C40 119.2(4) . . ? C4 N1 Si1 126.8(3) . . ? C4 N1 Y1 94.1(2) . . ? Si1 N1 Y1 131.65(17) . . ? C1 N2 Si2 125.7(3) . . ? C1 N2 Y1 93.4(2) . . ? Si2 N2 Y1 137.40(17) . . ? C39 N3 Si4 123.3(2) . . ? C39 N3 Y2 94.1(2) . . ? Si4 N3 Y2 140.72(17) . . ? C42 N4 Si5 127.3(3) . . ? C42 N4 Y2 96.5(2) . . ? Si5 N4 Y2 134.93(18) . . ? C27 O1 C30 107.6(3) . . ? C27 O1 Y1 120.9(2) . . ? C30 O1 Y1 130.7(2) . . ? C31 O2 C34 106.6(3) . . ? C31 O2 Y1 124.8(2) . . ? C34 O2 Y1 127.6(2) . . ? C59 O3 C62 109.6(3) . . ? C59 O3 Y2 128.9(2) . . ? C62 O3 Y2 119.2(2) . . ? N1 Si1 C23 106.75(18) . . ? N1 Si1 C22 111.30(19) . . ? C23 Si1 C22 109.7(2) . . ? N1 Si1 C21 114.36(19) . . ? C23 Si1 C21 106.2(2) . . ? C22 Si1 C21 108.3(2) . . ? N2 Si2 C25 111.57(19) . . ? N2 Si2 C24 107.97(19) . . ? C25 Si2 C24 108.5(2) . . ? N2 Si2 C26 115.84(18) . . ? C25 Si2 C26 107.8(2) . . ? C24 Si2 C26 104.8(2) . . ? N3 Si4 C68 107.33(17) . . ? N3 Si4 C69 115.64(19) . . ? C68 Si4 C69 106.9(2) . . ? N3 Si4 C67 110.9(2) . . ? C68 Si4 C67 109.2(2) . . ? C69 Si4 C67 106.7(2) . . ? N4 Si5 C72 106.69(18) . . ? N4 Si5 C71 111.84(18) . . ? C72 Si5 C71 110.1(2) . . ? N4 Si5 C70 116.30(18) . . ? C72 Si5 C70 107.2(2) . . ? C71 Si5 C70 104.5(2) . . ? N1 Y1 N2 122.63(11) . . ? N1 Y1 O1 95.03(10) . . ? N2 Y1 O1 89.29(10) . . ? N1 Y1 O2 92.89(11) . . ? N2 Y1 O2 93.59(10) . . ? O1 Y1 O2 168.39(10) . . ? N1 Y1 C38 108.48(13) . . ? N2 Y1 C38 128.84(13) . . ? O1 Y1 C38 84.10(12) . . ? O2 Y1 C38 85.34(12) . . ? N1 Y1 C4 30.51(11) . . ? N2 Y1 C4 98.26(12) . . ? O1 Y1 C4 115.16(10) . . ? O2 Y1 C4 75.58(11) . . ? C38 Y1 C4 130.27(14) . . ? N1 Y1 C1 97.14(11) . . ? N2 Y1 C1 30.58(10) . . ? O1 Y1 C1 73.74(10) . . ? O2 Y1 C1 113.68(10) . . ? C38 Y1 C1 147.45(13) . . ? C4 Y1 C1 81.47(12) . . ? N1 Y1 C3 55.43(11) . . ? N2 Y1 C3 69.40(11) . . ? O1 Y1 C3 109.97(9) . . ? O2 Y1 C3 81.54(10) . . ? C38 Y1 C3 158.36(13) . . ? C4 Y1 C3 29.08(12) . . ? C1 Y1 C3 54.19(11) . . ? N1 Y1 C2 68.59(11) . . ? N2 Y1 C2 55.50(10) . . ? O1 Y1 C2 81.80(9) . . ? O2 Y1 C2 109.07(10) . . ? C38 Y1 C2 165.22(12) . . ? C4 Y1 C2 53.96(11) . . ? C1 Y1 C2 28.96(11) . . ? C3 Y1 C2 30.76(10) . . ? N4 Y2 N3 120.18(11) . . ? N4 Y2 O3 87.75(10) . . ? N3 Y2 O3 99.15(10) . . ? N4 Y2 O4 92.47(10) . . ? N3 Y2 O4 92.50(10) . . ? O3 Y2 O4 166.39(9) . . ? N4 Y2 C76 118.39(14) . . ? N3 Y2 C76 121.36(14) . . ? O3 Y2 C76 85.55(12) . . ? O4 Y2 C76 82.37(12) . . ? N4 Y2 C39 95.87(11) . . ? N3 Y2 C39 30.54(11) . . ? O3 Y2 C39 119.00(10) . . ? O4 Y2 C39 74.53(10) . . ? C76 Y2 C39 139.39(13) . . ? N4 Y2 C42 29.66(12) . . ? N3 Y2 C42 95.73(12) . . ? O3 Y2 C42 74.22(10) . . ? O4 Y2 C42 111.76(10) . . ? C76 Y2 C42 140.32(13) . . ? C39 Y2 C42 79.96(11) . . ? N4 Y2 C40 67.56(11) . . ? N3 Y2 C40 54.72(11) . . ? O3 Y2 C40 111.96(10) . . ? O4 Y2 C40 80.54(10) . . ? C76 Y2 C40 162.19(13) . . ? C39 Y2 C40 28.58(11) . . ? C42 Y2 C40 52.93(11) . . ? N4 Y2 C41 53.68(11) . . ? N3 Y2 C41 67.96(11) . . ? O3 Y2 C41 84.12(10) . . ? O4 Y2 C41 106.92(10) . . ? C76 Y2 C41 167.20(12) . . ? C39 Y2 C41 53.17(11) . . ? C42 Y2 C41 28.19(11) . . ? C40 Y2 C41 29.84(10) . . ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.073 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.103 # Attachment '2c.cif' data_1113GuillotICMMO _database_code_depnum_ccdc_archive 'CCDC 855073' #TrackingRef '2c.cif'_database_code_CSD 'CCDC 855073' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C52 H60 Li4 N4 Si4 ' _chemical_formula_sum 'C52 H60 Li4 N4 Si4 ' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 100(1) _chemical_formula_weight 881.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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' Li Li 0.0003 0.0001 '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' Si Si 0.0826 0.0707 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' _symmetry_int_tables_number 5 _chemical_absolute_configuration ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 23.2936(7) _cell_length_b 10.2146(3) _cell_length_c 22.5327(7) _cell_angle_alpha 90.00 _cell_angle_beta 111.3140(10) _cell_angle_gamma 90.00 _cell_volume 4994.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 4268 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 32.57 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.9742 _exptl_absorpt_correction_T_max 0.9950 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'kappa X8 APEX II Bruker ICMMO' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58845 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 30.57 _reflns_number_total 14912 _reflns_number_gt 13975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'Ortep-3 for Windows (L. J. Farrugia, J. Appl. Cryst (1997), 30, 565)' ; _computing_publication_material ; 'WINGX (Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838)' ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+0.2869P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(5) _refine_ls_number_reflns 14912 _refine_ls_number_parameters 589 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1149 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Li4 Li 0.91264(14) 0.5413(3) 0.93602(13) 0.0201(5) Uani 1 1 d . . . C1 C 0.97121(7) 0.11728(13) 0.40967(6) 0.0123(2) Uani 1 1 d . . . C2 C 0.99028(7) 0.03308(13) 0.60822(6) 0.0120(2) Uani 1 1 d . . . C3 C 0.99604(7) -0.11044(13) 0.38623(6) 0.0119(2) Uani 1 1 d . . . C4 C 1.03157(7) -0.19658(13) 0.43380(6) 0.0130(2) Uani 1 1 d . . . C5 C 1.01140(7) -0.33054(13) 0.42894(7) 0.0173(3) Uani 1 1 d . . . H5 H 1.0327 -0.3886 0.4612 0.021 Uiso 1 1 calc R . . C6 C 0.96223(7) -0.37585(14) 0.37880(8) 0.0207(3) Uani 1 1 d . . . H6 H 0.9504 -0.4630 0.3780 0.025 Uiso 1 1 calc R . . C7 C 0.92878(7) -0.29155(15) 0.32776(7) 0.0184(3) Uani 1 1 d . . . C8 C 0.87993(8) -0.33720(17) 0.27283(9) 0.0255(3) Uani 1 1 d . . . H8 H 0.8674 -0.4240 0.2708 0.031 Uiso 1 1 calc R . . C9 C 0.85116(8) -0.25486(19) 0.22293(8) 0.0281(4) Uani 1 1 d . . . H9 H 0.8205 -0.2868 0.1865 0.034 Uiso 1 1 calc R . . C10 C 0.86793(8) -0.12235(18) 0.22681(7) 0.0239(3) Uani 1 1 d . . . H10 H 0.8480 -0.0666 0.1930 0.029 Uiso 1 1 calc R . . C11 C 0.91355(7) -0.07420(16) 0.28018(7) 0.0179(3) Uani 1 1 d . . . H11 H 0.9234 0.0143 0.2824 0.022 Uiso 1 1 calc R . . C12 C 0.94576(7) -0.15737(14) 0.33188(6) 0.0144(3) Uani 1 1 d . . . C13 C 0.93923(7) 0.08280(14) 0.62239(6) 0.0134(2) Uani 1 1 d . . . C14 C 0.90278(7) 0.00047(15) 0.64594(7) 0.0175(3) Uani 1 1 d . . . H14 H 0.9108 -0.0889 0.6502 0.021 Uiso 1 1 calc R . . C15 C 0.85645(8) 0.05104(17) 0.66232(7) 0.0216(3) Uani 1 1 d . . . H15 H 0.8337 -0.0040 0.6782 0.026 Uiso 1 1 calc R . . C16 C 0.84267(8) 0.18590(17) 0.65548(8) 0.0227(3) Uani 1 1 d . . . H16 H 0.8111 0.2192 0.6670 0.027 Uiso 1 1 calc R . . C17 C 0.87569(7) 0.26779(16) 0.63194(7) 0.0194(3) Uani 1 1 d . . . H17 H 0.8660 0.3564 0.6269 0.023 Uiso 1 1 calc R . . C18 C 0.92451(7) 0.21873(14) 0.61516(6) 0.0150(3) Uani 1 1 d . . . C19 C 0.96139(7) 0.30129(14) 0.59282(7) 0.0170(3) Uani 1 1 d . . . H19 H 0.9517 0.3897 0.5861 0.020 Uiso 1 1 calc R . . C20 C 0.98915(7) 0.25313(14) 0.41895(6) 0.0150(2) Uani 1 1 d . . . H20 H 0.9661 0.3102 0.4335 0.018 Uiso 1 1 calc R . . C21 C 0.79027(8) 0.0229(2) 0.33681(8) 0.0276(4) Uani 1 1 d . . . H21A H 0.7495 0.0563 0.3284 0.041 Uiso 1 1 calc R . . H21B H 0.7960 -0.0561 0.3614 0.041 Uiso 1 1 calc R . . H21C H 0.7954 0.0047 0.2972 0.041 Uiso 1 1 calc R . . C22 C 0.82185(8) 0.22310(19) 0.44396(8) 0.0261(3) Uani 1 1 d . . . H22A H 0.8244 0.1595 0.4762 0.039 Uiso 1 1 calc R . . H22B H 0.7800 0.2520 0.4241 0.039 Uiso 1 1 calc R . . H22C H 0.8477 0.2965 0.4631 0.039 Uiso 1 1 calc R . . C23 C 0.84564(9) 0.2801(2) 0.32402(10) 0.0333(4) Uani 1 1 d . . . H23A H 0.8683 0.3548 0.3465 0.050 Uiso 1 1 calc R . . H23B H 0.8036 0.3046 0.3012 0.050 Uiso 1 1 calc R . . H23C H 0.8637 0.2489 0.2946 0.050 Uiso 1 1 calc R . . C24 C 0.84987(8) -0.34341(19) 0.57333(9) 0.0297(4) Uani 1 1 d . . . H24A H 0.8578 -0.2882 0.6099 0.045 Uiso 1 1 calc R . . H24B H 0.8818 -0.4080 0.5821 0.045 Uiso 1 1 calc R . . H24C H 0.8108 -0.3862 0.5637 0.045 Uiso 1 1 calc R . . C25 C 0.78327(8) -0.12257(17) 0.48722(8) 0.0219(3) Uani 1 1 d . . . H20A H 0.7895 -0.0708 0.5246 0.033 Uiso 1 1 calc R . . H20B H 0.7451 -0.1696 0.4762 0.033 Uiso 1 1 calc R . . H20C H 0.7818 -0.0663 0.4526 0.033 Uiso 1 1 calc R . . C26 C 0.82873(9) -0.3541(2) 0.43274(10) 0.0326(4) Uani 1 1 d . . . H26A H 0.8262 -0.3047 0.3956 0.049 Uiso 1 1 calc R . . H26B H 0.7898 -0.3956 0.4257 0.049 Uiso 1 1 calc R . . H26C H 0.8602 -0.4197 0.4409 0.049 Uiso 1 1 calc R . . C27 C 0.96077(7) 0.61565(13) 1.06040(6) 0.0124(2) Uani 1 1 d . . . C28 C 0.91038(7) 0.53004(13) 1.03687(6) 0.0121(2) Uani 1 1 d . . . C29 C 0.91996(6) 0.38703(13) 1.04956(6) 0.0114(2) Uani 1 1 d . . . C30 C 0.91927(7) 0.30142(13) 1.00049(6) 0.0116(2) Uani 1 1 d . . . C31 C 0.93523(7) 0.16706(13) 1.01795(6) 0.0133(2) Uani 1 1 d . . . H31 H 0.9366 0.1089 0.9867 0.016 Uiso 1 1 calc R . . C32 C 0.94849(7) 0.12117(13) 1.07851(6) 0.0149(3) Uani 1 1 d . . . H32 H 0.9589 0.0335 1.0875 0.018 Uiso 1 1 calc R . . C33 C 1.05338(7) 0.20555(13) 0.87209(6) 0.0134(2) Uani 1 1 d . . . C34 C 1.03974(7) 0.16020(15) 0.80892(6) 0.0172(3) Uani 1 1 d . . . H34 H 1.0291 0.0730 0.7990 0.021 Uiso 1 1 calc R . . C35 C 1.04215(7) 0.24392(16) 0.76241(6) 0.0187(3) Uani 1 1 d . . . H35 H 1.0327 0.2138 0.7210 0.022 Uiso 1 1 calc R . . C36 C 1.05901(8) 0.37597(15) 0.77745(7) 0.0189(3) Uani 1 1 d . . . H36 H 1.0614 0.4319 0.7459 0.023 Uiso 1 1 calc R . . C37 C 1.07192(7) 0.42301(14) 0.83802(7) 0.0164(3) Uani 1 1 d . . . H37 H 1.0829 0.5104 0.8470 0.020 Uiso 1 1 calc R . . C38 C 1.06868(7) 0.33942(13) 0.88720(6) 0.0121(2) Uani 1 1 d . . . C39 C 0.94948(7) 0.75103(14) 1.04195(6) 0.0159(3) Uani 1 1 d . . . H39 H 0.9825 0.8091 1.0547 0.019 Uiso 1 1 calc R . . C40 C 0.89229(8) 0.79772(14) 1.00648(7) 0.0179(3) Uani 1 1 d . . . H40 H 0.8874 0.8860 0.9958 0.022 Uiso 1 1 calc R . . C41 C 0.84026(7) 0.71383(14) 0.98564(7) 0.0156(3) Uani 1 1 d . . . C42 C 0.78016(7) 0.76002(16) 0.94986(7) 0.0199(3) Uani 1 1 d . . . H42 H 0.7742 0.8481 0.9390 0.024 Uiso 1 1 calc R . . C43 C 0.73083(8) 0.67638(16) 0.93117(8) 0.0225(3) Uani 1 1 d . . . H43 H 0.6916 0.7077 0.9077 0.027 Uiso 1 1 calc R . . C44 C 0.73957(8) 0.54253(16) 0.94764(8) 0.0205(3) Uani 1 1 d . . . H44 H 0.7059 0.4863 0.9355 0.025 Uiso 1 1 calc R . . C45 C 0.79734(7) 0.49450(14) 0.98140(7) 0.0166(3) Uani 1 1 d . . . H45 H 0.8023 0.4058 0.9914 0.020 Uiso 1 1 calc R . . C46 C 0.84963(7) 0.57841(14) 1.00134(6) 0.0134(2) Uani 1 1 d . . . C47 C 0.98172(11) 0.7833(2) 0.80692(9) 0.0358(5) Uani 1 1 d . . . H47A H 0.9827 0.8592 0.8324 0.054 Uiso 1 1 calc R . . H47B H 0.9608 0.8042 0.7627 0.054 Uiso 1 1 calc R . . H47C H 1.0231 0.7559 0.8138 0.054 Uiso 1 1 calc R . . C48 C 0.91759(9) 0.52819(18) 0.76201(7) 0.0252(3) Uani 1 1 d . . . H48A H 0.9490 0.5260 0.7438 0.038 Uiso 1 1 calc R . . H48B H 0.8792 0.5545 0.7301 0.038 Uiso 1 1 calc R . . H48C H 0.9132 0.4427 0.7775 0.038 Uiso 1 1 calc R . . C49 C 0.86644(9) 0.7193(2) 0.83263(9) 0.0328(4) Uani 1 1 d . . . H49A H 0.8439 0.6522 0.8446 0.049 Uiso 1 1 calc R . . H49B H 0.8419 0.7528 0.7914 0.049 Uiso 1 1 calc R . . H49C H 0.8760 0.7889 0.8633 0.049 Uiso 1 1 calc R . . C50 C 0.80039(8) 0.3676(2) 0.81736(8) 0.0296(4) Uani 1 1 d . . . H50A H 0.7763 0.4191 0.8354 0.044 Uiso 1 1 calc R . . H50B H 0.7734 0.3185 0.7818 0.044 Uiso 1 1 calc R . . H50C H 0.8257 0.4243 0.8032 0.044 Uiso 1 1 calc R . . C51 C 0.79898(8) 0.15156(18) 0.90813(7) 0.0239(3) Uani 1 1 d . . . H51A H 0.8238 0.0963 0.9423 0.036 Uiso 1 1 calc R . . H51B H 0.7726 0.0983 0.8740 0.036 Uiso 1 1 calc R . . H51C H 0.7743 0.2081 0.9232 0.036 Uiso 1 1 calc R . . C52 C 0.88550(9) 0.1376(2) 0.83656(9) 0.0344(4) Uani 1 1 d . . . H52A H 0.8534 0.0921 0.8037 0.052 Uiso 1 1 calc R . . H52B H 0.9111 0.0756 0.8665 0.052 Uiso 1 1 calc R . . H52C H 0.9100 0.1864 0.8180 0.052 Uiso 1 1 calc R . . Li1 Li 0.91703(13) 0.0424(3) 0.50741(12) 0.0172(5) Uani 1 1 d . . . Li2 Li 0.92121(13) -0.1247(3) 0.42952(13) 0.0190(5) Uani 1 1 d . . . Li3 Li 0.97452(13) 0.3753(3) 0.90715(13) 0.0193(5) Uani 1 1 d . . . N1 N 0.91895(6) 0.07223(11) 0.41889(5) 0.0136(2) Uani 1 1 d . . . N2 N 0.91540(6) -0.15471(12) 0.51623(5) 0.0135(2) Uani 1 1 d . . . N3 N 0.98070(6) 0.57229(12) 0.90121(6) 0.0143(2) Uani 1 1 d . . . N4 N 0.90430(6) 0.34346(12) 0.93781(5) 0.0129(2) Uani 1 1 d . . . Si1 Si 0.848393(19) 0.14735(4) 0.382374(17) 0.01496(8) Uani 1 1 d . . . Si2 Si 0.848176(19) -0.24117(4) 0.503291(19) 0.01599(8) Uani 1 1 d . . . Si3 Si 0.940013(19) 0.64848(4) 0.829859(17) 0.01588(8) Uani 1 1 d . . . Si4 Si 0.850246(19) 0.25288(4) 0.878645(17) 0.01558(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li4 0.0218(14) 0.0191(12) 0.0219(12) 0.0020(10) 0.0108(10) 0.0013(10) C1 0.0138(6) 0.0126(5) 0.0092(5) 0.0007(4) 0.0028(4) 0.0007(4) C2 0.0116(6) 0.0119(5) 0.0110(5) 0.0004(4) 0.0025(4) -0.0001(4) C3 0.0118(6) 0.0120(5) 0.0120(5) -0.0019(4) 0.0045(4) 0.0000(5) C4 0.0122(6) 0.0119(5) 0.0151(5) -0.0008(4) 0.0053(5) 0.0011(5) C5 0.0162(7) 0.0113(6) 0.0230(6) 0.0001(5) 0.0056(5) 0.0017(5) C6 0.0155(7) 0.0132(6) 0.0314(7) -0.0041(5) 0.0062(6) -0.0014(5) C7 0.0126(7) 0.0154(6) 0.0246(7) -0.0062(5) 0.0035(5) -0.0001(5) C8 0.0145(7) 0.0210(7) 0.0346(8) -0.0139(6) 0.0011(6) -0.0009(6) C9 0.0167(8) 0.0334(9) 0.0270(7) -0.0140(7) -0.0006(6) 0.0003(7) C10 0.0184(8) 0.0313(8) 0.0170(6) -0.0046(6) 0.0004(5) 0.0033(6) C11 0.0160(7) 0.0226(7) 0.0138(6) -0.0019(5) 0.0037(5) -0.0003(5) C12 0.0121(6) 0.0154(6) 0.0149(5) -0.0037(5) 0.0039(5) 0.0004(5) C13 0.0136(6) 0.0157(6) 0.0092(5) -0.0015(4) 0.0022(4) 0.0000(5) C14 0.0179(7) 0.0188(6) 0.0158(6) 0.0003(5) 0.0061(5) -0.0014(5) C15 0.0192(8) 0.0279(8) 0.0196(6) -0.0010(6) 0.0094(6) -0.0032(6) C16 0.0181(8) 0.0301(8) 0.0214(7) -0.0035(6) 0.0091(6) 0.0035(6) C17 0.0152(7) 0.0212(7) 0.0195(6) -0.0042(5) 0.0037(5) 0.0036(6) C18 0.0148(7) 0.0153(6) 0.0127(5) -0.0016(4) 0.0024(5) 0.0007(5) C19 0.0190(7) 0.0125(5) 0.0172(6) -0.0006(5) 0.0037(5) 0.0003(5) C20 0.0175(7) 0.0118(5) 0.0152(5) -0.0003(5) 0.0054(5) 0.0019(5) C21 0.0191(8) 0.0392(9) 0.0221(7) -0.0079(7) 0.0047(6) -0.0063(7) C22 0.0198(8) 0.0331(9) 0.0261(7) -0.0080(6) 0.0093(6) 0.0022(6) C23 0.0188(8) 0.0421(11) 0.0367(9) 0.0237(8) 0.0074(7) 0.0075(7) C24 0.0184(8) 0.0295(8) 0.0385(9) 0.0180(8) 0.0072(7) -0.0021(7) C25 0.0158(7) 0.0245(7) 0.0264(7) 0.0078(6) 0.0086(6) 0.0033(6) C26 0.0205(8) 0.0334(9) 0.0408(9) -0.0172(8) 0.0074(7) -0.0086(7) C27 0.0149(7) 0.0113(5) 0.0108(5) -0.0004(4) 0.0045(4) 0.0015(4) C28 0.0146(7) 0.0099(5) 0.0122(5) 0.0008(4) 0.0053(5) 0.0020(5) C29 0.0115(6) 0.0102(5) 0.0120(5) 0.0007(4) 0.0038(4) 0.0008(4) C30 0.0118(6) 0.0108(5) 0.0112(5) 0.0005(4) 0.0031(4) -0.0014(4) C31 0.0166(6) 0.0106(5) 0.0121(5) -0.0009(4) 0.0044(4) -0.0007(5) C32 0.0186(7) 0.0117(5) 0.0128(5) 0.0015(4) 0.0039(5) 0.0014(5) C33 0.0154(7) 0.0141(5) 0.0100(5) -0.0009(4) 0.0038(4) 0.0003(5) C34 0.0224(7) 0.0156(6) 0.0125(5) -0.0033(5) 0.0051(5) -0.0026(5) C35 0.0217(7) 0.0223(7) 0.0119(5) -0.0026(5) 0.0057(5) -0.0014(6) C36 0.0249(8) 0.0190(6) 0.0150(6) 0.0016(5) 0.0100(5) -0.0001(6) C37 0.0216(7) 0.0144(6) 0.0151(6) 0.0008(5) 0.0091(5) -0.0010(5) C38 0.0113(6) 0.0129(5) 0.0116(5) 0.0001(4) 0.0036(4) 0.0001(5) C39 0.0178(7) 0.0115(5) 0.0166(5) 0.0001(5) 0.0041(5) -0.0004(5) C40 0.0203(8) 0.0121(5) 0.0203(6) 0.0020(5) 0.0059(5) 0.0012(5) C41 0.0176(7) 0.0127(6) 0.0157(6) 0.0008(5) 0.0053(5) 0.0033(5) C42 0.0194(7) 0.0176(6) 0.0204(6) 0.0032(5) 0.0044(5) 0.0058(6) C43 0.0163(7) 0.0257(8) 0.0231(7) 0.0021(6) 0.0043(6) 0.0062(6) C44 0.0138(7) 0.0226(7) 0.0242(7) 0.0002(6) 0.0056(5) 0.0005(5) C45 0.0145(7) 0.0160(6) 0.0193(6) 0.0005(5) 0.0059(5) 0.0004(5) C46 0.0147(7) 0.0131(6) 0.0124(5) 0.0004(4) 0.0048(5) 0.0016(5) C47 0.0434(12) 0.0336(10) 0.0222(7) 0.0121(7) 0.0022(7) -0.0158(8) C48 0.0245(9) 0.0310(8) 0.0166(6) -0.0034(6) 0.0033(6) -0.0012(7) C49 0.0270(9) 0.0448(11) 0.0228(7) 0.0021(7) 0.0046(6) 0.0165(8) C50 0.0192(8) 0.0384(9) 0.0229(7) 0.0157(7) -0.0022(6) -0.0056(7) C51 0.0214(8) 0.0252(7) 0.0196(6) 0.0066(6) 0.0009(5) -0.0071(6) C52 0.0268(9) 0.0470(11) 0.0261(8) -0.0193(8) 0.0055(7) -0.0052(8) Li1 0.0175(13) 0.0172(11) 0.0159(10) 0.0022(9) 0.0050(9) 0.0011(9) Li2 0.0196(13) 0.0182(11) 0.0202(11) -0.0003(9) 0.0087(10) -0.0008(10) Li3 0.0193(13) 0.0184(12) 0.0201(11) 0.0000(9) 0.0070(10) 0.0001(10) N1 0.0133(6) 0.0140(5) 0.0141(5) 0.0012(4) 0.0056(4) 0.0008(4) N2 0.0121(6) 0.0130(5) 0.0141(5) 0.0005(4) 0.0031(4) -0.0022(4) N3 0.0144(6) 0.0138(5) 0.0133(5) 0.0020(4) 0.0035(4) -0.0015(4) N4 0.0140(6) 0.0143(5) 0.0095(4) 0.0012(4) 0.0032(4) -0.0011(4) Si1 0.01261(18) 0.01910(18) 0.01302(15) 0.00116(14) 0.00449(13) 0.00082(15) Si2 0.01177(18) 0.01515(17) 0.01990(17) 0.00107(14) 0.00438(14) -0.00175(14) Si3 0.01608(19) 0.01699(17) 0.01281(15) 0.00268(14) 0.00316(13) -0.00048(15) Si4 0.01402(19) 0.01908(18) 0.01083(15) 0.00113(14) 0.00116(13) -0.00266(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li4 N4 2.032(3) . ? Li4 N3 2.033(3) . ? Li4 C28 2.295(3) . ? Li4 C46 2.457(3) . ? Li4 Li3 2.461(4) . ? Li4 C27 2.721(3) . ? Li4 Si3 2.904(3) . ? C1 N1 1.3858(19) . ? C1 C2 1.4034(19) 2_756 ? C1 C20 1.4424(19) . ? C1 Li1 2.705(3) 2_756 ? C2 C1 1.4034(19) 2_756 ? C2 C13 1.432(2) . ? C2 C3 1.4958(18) 2_756 ? C2 Li1 2.294(3) . ? C3 C4 1.4012(19) . ? C3 C12 1.4347(18) . ? C3 C2 1.4958(18) 2_756 ? C3 Li2 2.291(3) . ? C4 N2 1.4020(18) 2_756 ? C4 C5 1.4379(19) . ? C4 Li2 2.641(3) . ? C5 C6 1.365(2) . ? C6 C7 1.421(2) . ? C7 C12 1.420(2) . ? C7 C8 1.421(2) . ? C8 C9 1.369(3) . ? C9 C10 1.403(3) . ? C10 C11 1.374(2) . ? C11 C12 1.416(2) . ? C12 Li2 2.489(3) . ? C13 C18 1.4253(19) . ? C13 C14 1.427(2) . ? C13 Li1 2.485(3) . ? C14 C15 1.363(2) . ? C15 C16 1.410(2) . ? C16 C17 1.367(2) . ? C17 C18 1.414(2) . ? C18 C19 1.420(2) . ? C19 C20 1.365(2) 2_756 ? C20 C19 1.365(2) 2_756 ? C21 Si1 1.8687(18) . ? C22 Si1 1.8790(17) . ? C23 Si1 1.8733(18) . ? C24 Si2 1.8809(17) . ? C25 Si2 1.8672(17) . ? C26 Si2 1.8816(18) . ? C27 N3 1.3950(18) 2_757 ? C27 C28 1.4041(19) . ? C27 C39 1.4403(19) . ? C28 C46 1.4365(19) . ? C28 C29 1.4896(18) . ? C29 C30 1.4052(18) . ? C29 C38 1.4363(18) 2_757 ? C29 Li3 2.294(3) 2_757 ? C30 N4 1.3938(16) . ? C30 C31 1.4389(18) . ? C30 Li3 2.698(3) 2_757 ? C31 C32 1.3678(18) . ? C32 C33 1.4208(19) 2_757 ? C33 C34 1.4189(18) . ? C33 C32 1.4208(19) 2_757 ? C33 C38 1.4229(18) . ? C34 C35 1.369(2) . ? C35 C36 1.411(2) . ? C36 C37 1.3733(19) . ? C37 C38 1.4225(19) . ? C38 C29 1.4363(18) 2_757 ? C38 Li3 2.421(3) . ? C39 C40 1.366(2) . ? C40 C41 1.418(2) . ? C41 C42 1.419(2) . ? C41 C46 1.4249(19) . ? C42 C43 1.370(2) . ? C43 C44 1.412(2) . ? C44 C45 1.373(2) . ? C45 C46 1.422(2) . ? C47 Si3 1.8632(18) . ? C48 Si3 1.8813(17) . ? C49 Si3 1.882(2) . ? C50 Si4 1.8608(17) . ? C51 Si4 1.8749(17) . ? C52 Si4 1.878(2) . ? Li1 N2 2.025(3) . ? Li1 N1 2.034(3) . ? Li1 Li2 2.476(4) . ? Li1 C1 2.705(3) 2_756 ? Li1 Si1 2.893(3) . ? Li2 N1 2.025(3) . ? Li2 N2 2.030(3) . ? Li2 Si2 3.021(3) . ? Li3 N4 2.020(3) . ? Li3 N3 2.025(3) . ? Li3 C29 2.294(3) 2_757 ? Li3 C30 2.698(3) 2_757 ? Li3 Si4 3.001(3) . ? N1 Si1 1.7274(13) . ? N2 C4 1.4020(18) 2_756 ? N2 Si2 1.7278(13) . ? N3 C27 1.3950(18) 2_757 ? N3 Si3 1.7265(12) . ? N4 Si4 1.7316(12) . ? 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 N4 Li4 N3 104.84(14) . . ? N4 Li4 C28 83.89(11) . . ? N3 Li4 C28 133.76(15) . . ? N4 Li4 C46 93.39(12) . . ? N3 Li4 C46 157.93(15) . . ? C28 Li4 C46 34.98(6) . . ? N4 Li4 Li3 52.38(10) . . ? N3 Li4 Li3 52.52(10) . . ? C28 Li4 Li3 116.97(13) . . ? C46 Li4 Li3 143.08(14) . . ? N4 Li4 C27 105.29(12) . . ? N3 Li4 C27 105.48(12) . . ? C28 Li4 C27 31.05(6) . . ? C46 Li4 C27 56.77(7) . . ? Li3 Li4 C27 113.76(13) . . ? N4 Li4 Si3 116.26(12) . . ? N3 Li4 Si3 35.72(6) . . ? C28 Li4 Si3 157.72(13) . . ? C46 Li4 Si3 142.48(12) . . ? Li3 Li4 Si3 73.56(10) . . ? C27 Li4 Si3 127.70(11) . . ? N1 C1 C2 121.84(12) . 2_756 ? N1 C1 C20 121.44(12) . . ? C2 C1 C20 116.71(13) 2_756 . ? N1 C1 Li1 118.68(10) . 2_756 ? C2 C1 Li1 58.00(9) 2_756 2_756 ? C20 C1 Li1 90.94(10) . 2_756 ? C1 C2 C13 121.07(12) 2_756 . ? C1 C2 C3 119.06(13) 2_756 2_756 ? C13 C2 C3 119.86(12) . 2_756 ? C1 C2 Li1 90.74(10) 2_756 . ? C13 C2 Li1 80.04(10) . . ? C3 C2 Li1 100.54(11) 2_756 . ? C4 C3 C12 121.00(13) . . ? C4 C3 C2 120.18(12) . 2_756 ? C12 C3 C2 118.81(12) . 2_756 ? C4 C3 Li2 87.91(11) . . ? C12 C3 Li2 80.26(11) . . ? C2 C3 Li2 101.46(11) 2_756 . ? C3 C4 N2 121.72(13) . 2_756 ? C3 C4 C5 116.97(13) . . ? N2 C4 C5 121.30(13) 2_756 . ? C3 C4 Li2 60.08(10) . . ? N2 C4 Li2 120.41(11) 2_756 . ? C5 C4 Li2 88.56(11) . . ? C6 C5 C4 122.58(14) . . ? C5 C6 C7 120.85(14) . . ? C12 C7 C6 118.30(13) . . ? C12 C7 C8 119.30(15) . . ? C6 C7 C8 122.40(15) . . ? C9 C8 C7 120.78(16) . . ? C8 C9 C10 119.98(15) . . ? C11 C10 C9 120.61(16) . . ? C10 C11 C12 121.00(15) . . ? C11 C12 C7 118.25(13) . . ? C11 C12 C3 121.71(13) . . ? C7 C12 C3 119.99(13) . . ? C11 C12 Li2 115.06(12) . . ? C7 C12 Li2 92.25(12) . . ? C3 C12 Li2 65.12(10) . . ? C18 C13 C14 117.76(14) . . ? C18 C13 C2 120.31(13) . . ? C14 C13 C2 121.90(13) . . ? C18 C13 Li1 95.28(10) . . ? C14 C13 Li1 111.31(11) . . ? C2 C13 Li1 65.39(9) . . ? C15 C14 C13 120.93(14) . . ? C14 C15 C16 120.79(16) . . ? C17 C16 C15 120.16(16) . . ? C16 C17 C18 120.49(15) . . ? C17 C18 C19 122.22(14) . . ? C17 C18 C13 119.86(14) . . ? C19 C18 C13 117.89(14) . . ? C20 C19 C18 121.14(13) 2_756 . ? C19 C20 C1 122.63(13) 2_756 . ? N3 C27 C28 122.07(12) 2_757 . ? N3 C27 C39 121.23(13) 2_757 . ? C28 C27 C39 116.69(12) . . ? N3 C27 Li4 119.61(11) 2_757 . ? C28 C27 Li4 57.48(9) . . ? C39 C27 Li4 90.40(10) . . ? C27 C28 C46 121.01(12) . . ? C27 C28 C29 119.46(12) . . ? C46 C28 C29 119.52(12) . . ? C27 C28 Li4 91.47(11) . . ? C46 C28 Li4 78.66(11) . . ? C29 C28 Li4 100.57(11) . . ? C30 C29 C38 121.01(12) . 2_757 ? C30 C29 C28 120.08(11) . . ? C38 C29 C28 118.89(11) 2_757 . ? C30 C29 Li3 90.36(11) . 2_757 ? C38 C29 Li3 77.17(11) 2_757 2_757 ? C28 C29 Li3 101.27(11) . 2_757 ? N4 C30 C29 122.18(12) . . ? N4 C30 C31 121.04(12) . . ? C29 C30 C31 116.77(11) . . ? N4 C30 Li3 121.13(11) . 2_757 ? C29 C30 Li3 58.25(10) . 2_757 ? C31 C30 Li3 88.99(10) . 2_757 ? C32 C31 C30 122.81(12) . . ? C31 C32 C33 120.90(12) . 2_757 ? C34 C33 C32 121.90(13) . 2_757 ? C34 C33 C38 119.94(12) . . ? C32 C33 C38 118.16(12) 2_757 . ? C35 C34 C33 120.48(14) . . ? C34 C35 C36 119.89(13) . . ? C37 C36 C35 120.95(13) . . ? C36 C37 C38 120.65(13) . . ? C37 C38 C33 118.03(12) . . ? C37 C38 C29 121.79(12) . 2_757 ? C33 C38 C29 120.17(12) . 2_757 ? C37 C38 Li3 111.21(12) . . ? C33 C38 Li3 91.43(11) . . ? C29 C38 Li3 67.49(10) 2_757 . ? C40 C39 C27 122.74(14) . . ? C39 C40 C41 121.14(13) . . ? C40 C41 C42 122.38(14) . . ? C40 C41 C46 117.98(13) . . ? C42 C41 C46 119.64(14) . . ? C43 C42 C41 120.78(14) . . ? C42 C43 C44 119.90(14) . . ? C45 C44 C43 120.68(15) . . ? C44 C45 C46 120.93(14) . . ? C45 C46 C41 118.05(13) . . ? C45 C46 C28 121.73(13) . . ? C41 C46 C28 120.21(13) . . ? C45 C46 Li4 110.33(12) . . ? C41 C46 Li4 94.13(11) . . ? C28 C46 Li4 66.35(10) . . ? N2 Li1 N1 104.64(13) . . ? N2 Li1 C2 83.98(10) . . ? N1 Li1 C2 134.72(15) . . ? N2 Li1 Li2 52.46(9) . . ? N1 Li1 Li2 52.23(9) . . ? C2 Li1 Li2 117.80(13) . . ? N2 Li1 C13 93.83(11) . . ? N1 Li1 C13 157.98(14) . . ? C2 Li1 C13 34.58(6) . . ? Li2 Li1 C13 143.76(13) . . ? N2 Li1 C1 105.12(11) . 2_756 ? N1 Li1 C1 106.05(12) . 2_756 ? C2 Li1 C1 31.25(6) . 2_756 ? Li2 Li1 C1 114.12(13) . 2_756 ? C13 Li1 C1 56.61(7) . 2_756 ? N2 Li1 Si1 116.13(11) . . ? N1 Li1 Si1 36.00(6) . . ? C2 Li1 Si1 158.24(12) . . ? Li2 Li1 Si1 73.46(9) . . ? C13 Li1 Si1 141.80(12) . . ? C1 Li1 Si1 128.36(10) 2_756 . ? N1 Li2 N2 104.82(13) . . ? N1 Li2 C3 82.95(11) . . ? N2 Li2 C3 138.31(15) . . ? N1 Li2 Li1 52.59(9) . . ? N2 Li2 Li1 52.29(9) . . ? C3 Li2 Li1 119.34(14) . . ? N1 Li2 C12 91.89(11) . . ? N2 Li2 C12 161.39(15) . . ? C3 Li2 C12 34.63(6) . . ? Li1 Li2 C12 143.12(14) . . ? N1 Li2 C4 105.28(12) . . ? N2 Li2 C4 109.11(12) . . ? C3 Li2 C4 32.02(6) . . ? Li1 Li2 C4 117.02(13) . . ? C12 Li2 C4 57.43(8) . . ? N1 Li2 Si2 117.44(12) . . ? N2 Li2 Si2 33.21(6) . . ? C3 Li2 Si2 158.01(12) . . ? Li1 Li2 Si2 72.93(9) . . ? C12 Li2 Si2 142.18(11) . . ? C4 Li2 Si2 127.28(10) . . ? N4 Li3 N3 105.57(14) . . ? N4 Li3 C29 137.60(14) . 2_757 ? N3 Li3 C29 83.42(11) . 2_757 ? N4 Li3 C38 160.02(15) . . ? N3 Li3 C38 92.71(12) . . ? C29 Li3 C38 35.33(6) 2_757 . ? N4 Li3 Li4 52.82(10) . . ? N3 Li3 Li4 52.80(10) . . ? C29 Li3 Li4 119.43(14) 2_757 . ? C38 Li3 Li4 144.13(14) . . ? N4 Li3 C30 108.70(12) . 2_757 ? N3 Li3 C30 105.17(12) . 2_757 ? C29 Li3 C30 31.39(6) 2_757 2_757 ? C38 Li3 C30 57.48(7) . 2_757 ? Li4 Li3 C30 116.73(12) . 2_757 ? N4 Li3 Si4 33.69(6) . . ? N3 Li3 Si4 119.08(12) . . ? C29 Li3 Si4 156.03(12) 2_757 . ? C38 Li3 Si4 139.96(11) . . ? Li4 Li3 Si4 74.43(10) . . ? C30 Li3 Si4 126.25(10) 2_757 . ? C1 N1 Si1 121.11(9) . . ? C1 N1 Li2 111.18(12) . . ? Si1 N1 Li2 118.50(11) . . ? C1 N1 Li1 122.01(12) . . ? Si1 N1 Li1 100.21(10) . . ? Li2 N1 Li1 75.18(12) . . ? C4 N2 Si2 117.35(9) 2_756 . ? C4 N2 Li1 109.86(12) 2_756 . ? Si2 N2 Li1 122.68(11) . . ? C4 N2 Li2 118.13(13) 2_756 . ? Si2 N2 Li2 106.74(10) . . ? Li1 N2 Li2 75.25(12) . . ? C27 N3 Si3 121.09(10) 2_757 . ? C27 N3 Li3 110.57(12) 2_757 . ? Si3 N3 Li3 118.77(10) . . ? C27 N3 Li4 122.25(12) 2_757 . ? Si3 N3 Li4 100.86(10) . . ? Li3 N3 Li4 74.68(12) . . ? C30 N4 Si4 117.36(10) . . ? C30 N4 Li3 117.44(12) . . ? Si4 N4 Li3 105.98(10) . . ? C30 N4 Li4 109.64(12) . . ? Si4 N4 Li4 124.34(10) . . ? Li3 N4 Li4 74.80(12) . . ? N1 Si1 C21 109.48(8) . . ? N1 Si1 C23 116.08(8) . . ? C21 Si1 C23 105.86(9) . . ? N1 Si1 C22 110.04(7) . . ? C21 Si1 C22 108.58(9) . . ? C23 Si1 C22 106.49(10) . . ? N1 Si1 Li1 43.80(7) . . ? C21 Si1 Li1 108.47(8) . . ? C23 Si1 Li1 144.83(9) . . ? C22 Si1 Li1 69.33(8) . . ? N2 Si2 C25 108.74(7) . . ? N2 Si2 C24 113.64(7) . . ? C25 Si2 C24 106.95(8) . . ? N2 Si2 C26 112.40(8) . . ? C25 Si2 C26 107.74(9) . . ? C24 Si2 C26 107.08(10) . . ? N2 Si2 Li2 40.05(7) . . ? C25 Si2 Li2 102.48(8) . . ? C24 Si2 Li2 146.72(8) . . ? C26 Si2 Li2 77.72(8) . . ? N3 Si3 C47 115.24(8) . . ? N3 Si3 C48 111.02(7) . . ? C47 Si3 C48 106.02(9) . . ? N3 Si3 C49 109.92(8) . . ? C47 Si3 C49 107.34(11) . . ? C48 Si3 C49 106.90(9) . . ? N3 Si3 Li4 43.42(7) . . ? C47 Si3 Li4 143.10(9) . . ? C48 Si3 Li4 110.12(8) . . ? C49 Si3 Li4 69.05(9) . . ? N4 Si4 C50 108.54(8) . . ? N4 Si4 C51 113.62(7) . . ? C50 Si4 C51 107.73(8) . . ? N4 Si4 C52 113.25(8) . . ? C50 Si4 C52 106.83(10) . . ? C51 Si4 C52 106.54(10) . . ? N4 Si4 Li3 40.33(7) . . ? C50 Si4 Li3 100.94(8) . . ? C51 Si4 Li3 147.49(7) . . ? C52 Si4 Li3 78.72(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 C12 C3 C4 N2 173.36(13) . . . 2_756 ? C2 C3 C4 N2 -7.3(2) 2_756 . . 2_756 ? Li2 C3 C4 N2 -109.32(15) . . . 2_756 ? C12 C3 C4 C5 -6.3(2) . . . . ? C2 C3 C4 C5 173.06(13) 2_756 . . . ? Li2 C3 C4 C5 71.01(15) . . . . ? C12 C3 C4 Li2 -77.32(14) . . . . ? C2 C3 C4 Li2 102.05(14) 2_756 . . . ? C3 C4 C5 C6 3.8(2) . . . . ? N2 C4 C5 C6 -175.85(15) 2_756 . . . ? Li2 C4 C5 C6 58.88(17) . . . . ? C4 C5 C6 C7 1.0(3) . . . . ? C5 C6 C7 C12 -3.3(3) . . . . ? C5 C6 C7 C8 175.78(16) . . . . ? C12 C7 C8 C9 3.0(3) . . . . ? C6 C7 C8 C9 -176.09(17) . . . . ? C7 C8 C9 C10 -2.9(3) . . . . ? C8 C9 C10 C11 0.6(3) . . . . ? C9 C10 C11 C12 1.5(3) . . . . ? C10 C11 C12 C7 -1.3(2) . . . . ? C10 C11 C12 C3 176.08(15) . . . . ? C10 C11 C12 Li2 -108.81(17) . . . . ? C6 C7 C12 C11 178.25(15) . . . . ? C8 C7 C12 C11 -0.9(2) . . . . ? C6 C7 C12 C3 0.8(2) . . . . ? C8 C7 C12 C3 -178.34(15) . . . . ? C6 C7 C12 Li2 -61.60(17) . . . . ? C8 C7 C12 Li2 119.27(16) . . . . ? C4 C3 C12 C11 -173.22(14) . . . . ? C2 C3 C12 C11 7.4(2) 2_756 . . . ? Li2 C3 C12 C11 105.20(15) . . . . ? C4 C3 C12 C7 4.2(2) . . . . ? C2 C3 C12 C7 -175.22(14) 2_756 . . . ? Li2 C3 C12 C7 -77.43(15) . . . . ? C4 C3 C12 Li2 81.58(15) . . . . ? C2 C3 C12 Li2 -97.80(14) 2_756 . . . ? C1 C2 C13 C18 3.47(19) 2_756 . . . ? C3 C2 C13 C18 -177.85(12) 2_756 . . . ? Li1 C2 C13 C18 -81.35(13) . . . . ? C1 C2 C13 C14 -174.49(13) 2_756 . . . ? C3 C2 C13 C14 4.19(19) 2_756 . . . ? Li1 C2 C13 C14 100.70(14) . . . . ? C1 C2 C13 Li1 84.81(13) 2_756 . . . ? C3 C2 C13 Li1 -96.51(13) 2_756 . . . ? C18 C13 C14 C15 -1.5(2) . . . . ? C2 C13 C14 C15 176.48(13) . . . . ? Li1 C13 C14 C15 -110.00(15) . . . . ? C13 C14 C15 C16 1.0(2) . . . . ? C14 C15 C16 C17 0.3(2) . . . . ? C15 C16 C17 C18 -1.0(2) . . . . ? C16 C17 C18 C19 -177.58(14) . . . . ? C16 C17 C18 C13 0.4(2) . . . . ? C14 C13 C18 C17 0.80(19) . . . . ? C2 C13 C18 C17 -177.24(12) . . . . ? Li1 C13 C18 C17 118.26(14) . . . . ? C14 C13 C18 C19 178.90(13) . . . . ? C2 C13 C18 C19 0.86(19) . . . . ? Li1 C13 C18 C19 -63.65(14) . . . . ? C17 C18 C19 C20 175.50(13) . . . 2_756 ? C13 C18 C19 C20 -2.6(2) . . . 2_756 ? N1 C1 C20 C19 -176.66(13) . . . 2_756 ? C2 C1 C20 C19 4.21(19) 2_756 . . 2_756 ? Li1 C1 C20 C19 58.40(14) 2_756 . . 2_756 ? N4 Li4 C27 N3 63.11(17) . . . 2_757 ? N3 Li4 C27 N3 -47.46(15) . . . 2_757 ? C28 Li4 C27 N3 111.22(14) . . . 2_757 ? C46 Li4 C27 N3 147.04(12) . . . 2_757 ? Li3 Li4 C27 N3 7.94(19) . . . 2_757 ? Si3 Li4 C27 N3 -79.17(16) . . . 2_757 ? N4 Li4 C27 C28 -48.11(12) . . . . ? N3 Li4 C27 C28 -158.67(16) . . . . ? C46 Li4 C27 C28 35.82(9) . . . . ? Li3 Li4 C27 C28 -103.28(15) . . . . ? Si3 Li4 C27 C28 169.62(17) . . . . ? N4 Li4 C27 C39 -169.99(14) . . . . ? N3 Li4 C27 C39 79.44(13) . . . . ? C28 Li4 C27 C39 -121.88(13) . . . . ? C46 Li4 C27 C39 -86.06(10) . . . . ? Li3 Li4 C27 C39 134.84(14) . . . . ? Si3 Li4 C27 C39 47.73(15) . . . . ? N3 C27 C28 C46 175.38(13) 2_757 . . . ? C39 C27 C28 C46 -5.78(19) . . . . ? Li4 C27 C28 C46 -77.64(13) . . . . ? N3 C27 C28 C29 -3.96(19) 2_757 . . . ? C39 C27 C28 C29 174.89(12) . . . . ? Li4 C27 C28 C29 103.02(14) . . . . ? N3 C27 C28 Li4 -106.98(14) 2_757 . . . ? C39 C27 C28 Li4 71.87(14) . . . . ? N4 Li4 C28 C27 133.76(11) . . . . ? N3 Li4 C28 C27 29.0(2) . . . . ? C46 Li4 C28 C27 -121.36(12) . . . . ? Li3 Li4 C28 C27 91.78(15) . . . . ? Si3 Li4 C28 C27 -22.1(4) . . . . ? N4 Li4 C28 C46 -104.87(12) . . . . ? N3 Li4 C28 C46 150.4(2) . . . . ? Li3 Li4 C28 C46 -146.86(16) . . . . ? C27 Li4 C28 C46 121.36(12) . . . . ? Si3 Li4 C28 C46 99.3(3) . . . . ? N4 Li4 C28 C29 13.41(12) . . . . ? N3 Li4 C28 C29 -91.3(2) . . . . ? C46 Li4 C28 C29 118.29(13) . . . . ? Li3 Li4 C28 C29 -28.57(17) . . . . ? C27 Li4 C28 C29 -120.35(13) . . . . ? Si3 Li4 C28 C29 -142.4(3) . . . . ? C27 C28 C29 C30 -105.96(16) . . . . ? C46 C28 C29 C30 74.69(18) . . . . ? Li4 C28 C29 C30 -8.18(17) . . . . ? C27 C28 C29 C38 72.55(17) . . . 2_757 ? C46 C28 C29 C38 -106.79(15) . . . 2_757 ? Li4 C28 C29 C38 170.33(13) . . . 2_757 ? C27 C28 C29 Li3 -8.90(15) . . . 2_757 ? C46 C28 C29 Li3 171.75(12) . . . 2_757 ? Li4 C28 C29 Li3 88.88(12) . . . 2_757 ? C38 C29 C30 N4 175.59(13) 2_757 . . . ? C28 C29 C30 N4 -5.9(2) . . . . ? Li3 C29 C30 N4 -109.20(15) 2_757 . . . ? C38 C29 C30 C31 -4.8(2) 2_757 . . . ? C28 C29 C30 C31 173.68(13) . . . . ? Li3 C29 C30 C31 70.41(14) 2_757 . . . ? C38 C29 C30 Li3 -75.21(14) 2_757 . . 2_757 ? C28 C29 C30 Li3 103.27(15) . . . 2_757 ? N4 C30 C31 C32 -178.09(14) . . . . ? C29 C30 C31 C32 2.3(2) . . . . ? Li3 C30 C31 C32 55.55(16) 2_757 . . . ? C30 C31 C32 C33 0.5(2) . . . 2_757 ? C32 C33 C34 C35 -179.78(16) 2_757 . . . ? C38 C33 C34 C35 1.1(2) . . . . ? C33 C34 C35 C36 0.7(2) . . . . ? C34 C35 C36 C37 -1.4(3) . . . . ? C35 C36 C37 C38 0.1(3) . . . . ? C36 C37 C38 C33 1.7(2) . . . . ? C36 C37 C38 C29 -177.99(15) . . . 2_757 ? C36 C37 C38 Li3 -102.03(17) . . . . ? C34 C33 C38 C37 -2.3(2) . . . . ? C32 C33 C38 C37 178.57(14) 2_757 . . . ? C34 C33 C38 C29 177.42(14) . . . 2_757 ? C32 C33 C38 C29 -1.8(2) 2_757 . . 2_757 ? C34 C33 C38 Li3 112.79(15) . . . . ? C32 C33 C38 Li3 -66.38(15) 2_757 . . . ? N3 C27 C39 C40 -177.39(14) 2_757 . . . ? C28 C27 C39 C40 3.8(2) . . . . ? Li4 C27 C39 C40 57.01(16) . . . . ? C27 C39 C40 C41 0.0(2) . . . . ? C39 C40 C41 C42 178.71(15) . . . . ? C39 C40 C41 C46 -1.7(2) . . . . ? C40 C41 C42 C43 -179.22(15) . . . . ? C46 C41 C42 C43 1.2(2) . . . . ? C41 C42 C43 C44 0.1(2) . . . . ? C42 C43 C44 C45 -1.1(2) . . . . ? C43 C44 C45 C46 0.8(2) . . . . ? C44 C45 C46 C41 0.4(2) . . . . ? C44 C45 C46 C28 179.79(14) . . . . ? C44 C45 C46 Li4 -106.11(16) . . . . ? C40 C41 C46 C45 178.97(13) . . . . ? C42 C41 C46 C45 -1.4(2) . . . . ? C40 C41 C46 C28 -0.4(2) . . . . ? C42 C41 C46 C28 179.22(13) . . . . ? C40 C41 C46 Li4 -65.37(15) . . . . ? C42 C41 C46 Li4 114.27(15) . . . . ? C27 C28 C46 C45 -175.08(13) . . . . ? C29 C28 C46 C45 4.3(2) . . . . ? Li4 C28 C46 C45 100.09(15) . . . . ? C27 C28 C46 C41 4.3(2) . . . . ? C29 C28 C46 C41 -176.38(12) . . . . ? Li4 C28 C46 C41 -80.55(14) . . . . ? C27 C28 C46 Li4 84.84(14) . . . . ? C29 C28 C46 Li4 -95.83(13) . . . . ? N4 Li4 C46 C45 -42.44(15) . . . . ? N3 Li4 C46 C45 171.5(4) . . . . ? C28 Li4 C46 C45 -116.74(14) . . . . ? Li3 Li4 C46 C45 -62.5(3) . . . . ? C27 Li4 C46 C45 -148.52(11) . . . . ? Si3 Li4 C46 C45 101.2(2) . . . . ? N4 Li4 C46 C41 -164.42(12) . . . . ? N3 Li4 C46 C41 49.6(4) . . . . ? C28 Li4 C46 C41 121.28(13) . . . . ? Li3 Li4 C46 C41 175.5(2) . . . . ? C27 Li4 C46 C41 89.51(9) . . . . ? Si3 Li4 C46 C41 -20.8(2) . . . . ? N4 Li4 C46 C28 74.30(12) . . . . ? N3 Li4 C46 C28 -71.7(4) . . . . ? Li3 Li4 C46 C28 54.2(2) . . . . ? C27 Li4 C46 C28 -31.77(8) . . . . ? Si3 Li4 C46 C28 -142.1(2) . . . . ? C1 C2 Li1 N2 132.80(11) 2_756 . . . ? C13 C2 Li1 N2 -105.75(11) . . . . ? C3 C2 Li1 N2 13.03(12) 2_756 . . . ? C1 C2 Li1 N1 28.1(2) 2_756 . . . ? C13 C2 Li1 N1 149.6(2) . . . . ? C3 C2 Li1 N1 -91.6(2) 2_756 . . . ? C1 C2 Li1 Li2 91.24(15) 2_756 . . . ? C13 C2 Li1 Li2 -147.31(15) . . . . ? C3 C2 Li1 Li2 -28.53(17) 2_756 . . . ? C1 C2 Li1 C13 -121.45(12) 2_756 . . . ? C3 C2 Li1 C13 118.78(13) 2_756 . . . ? C13 C2 Li1 C1 121.45(12) . . . 2_756 ? C3 C2 Li1 C1 -119.77(13) 2_756 . . 2_756 ? C1 C2 Li1 Si1 -25.7(4) 2_756 . . . ? C13 C2 Li1 Si1 95.8(4) . . . . ? C3 C2 Li1 Si1 -145.5(3) 2_756 . . . ? C18 C13 Li1 N2 -165.40(12) . . . . ? C14 C13 Li1 N2 -42.84(15) . . . . ? C2 C13 Li1 N2 73.60(12) . . . . ? C18 C13 Li1 N1 47.3(4) . . . . ? C14 C13 Li1 N1 169.9(4) . . . . ? C2 C13 Li1 N1 -73.7(4) . . . . ? C18 C13 Li1 C2 121.00(13) . . . . ? C14 C13 Li1 C2 -116.44(14) . . . . ? C18 C13 Li1 Li2 174.9(2) . . . . ? C14 C13 Li1 Li2 -62.5(3) . . . . ? C2 C13 Li1 Li2 53.9(2) . . . . ? C18 C13 Li1 C1 88.99(10) . . . 2_756 ? C14 C13 Li1 C1 -148.45(12) . . . 2_756 ? C2 C13 Li1 C1 -32.01(8) . . . 2_756 ? C18 C13 Li1 Si1 -22.4(2) . . . . ? C14 C13 Li1 Si1 100.2(2) . . . . ? C2 C13 Li1 Si1 -143.4(2) . . . . ? C4 C3 Li2 N1 134.31(11) . . . . ? C12 C3 Li2 N1 -103.73(11) . . . . ? C2 C3 Li2 N1 13.92(12) 2_756 . . . ? C4 C3 Li2 N2 29.9(2) . . . . ? C12 C3 Li2 N2 151.9(2) . . . . ? C2 C3 Li2 N2 -90.5(2) 2_756 . . . ? C4 C3 Li2 Li1 94.82(15) . . . . ? C12 C3 Li2 Li1 -143.22(15) . . . . ? C2 C3 Li2 Li1 -25.57(17) 2_756 . . . ? C4 C3 Li2 C12 -121.96(12) . . . . ? C2 C3 Li2 C12 117.65(12) 2_756 . . . ? C12 C3 Li2 C4 121.96(12) . . . . ? C2 C3 Li2 C4 -120.39(12) 2_756 . . . ? C4 C3 Li2 Si2 -24.7(3) . . . . ? C12 C3 Li2 Si2 97.3(3) . . . . ? C2 C3 Li2 Si2 -145.1(3) 2_756 . . . ? N2 Li1 Li2 N1 176.98(16) . . . . ? C2 Li1 Li2 N1 -126.71(16) . . . . ? C13 Li1 Li2 N1 -157.9(3) . . . . ? C1 Li1 Li2 N1 -92.08(13) 2_756 . . . ? Si1 Li1 Li2 N1 33.11(6) . . . . ? N1 Li1 Li2 N2 -176.98(16) . . . . ? C2 Li1 Li2 N2 56.31(13) . . . . ? C13 Li1 Li2 N2 25.1(2) . . . . ? C1 Li1 Li2 N2 90.94(13) 2_756 . . . ? Si1 Li1 Li2 N2 -143.86(12) . . . . ? N2 Li1 Li2 C3 -130.40(17) . . . . ? N1 Li1 Li2 C3 52.62(13) . . . . ? C2 Li1 Li2 C3 -74.09(18) . . . . ? C13 Li1 Li2 C3 -105.3(2) . . . . ? C1 Li1 Li2 C3 -39.46(18) 2_756 . . . ? Si1 Li1 Li2 C3 85.73(13) . . . . ? N2 Li1 Li2 C12 -164.9(3) . . . . ? N1 Li1 Li2 C12 18.1(2) . . . . ? C2 Li1 Li2 C12 -108.6(2) . . . . ? C13 Li1 Li2 C12 -139.9(2) . . . . ? C1 Li1 Li2 C12 -74.0(3) 2_756 . . . ? Si1 Li1 Li2 C12 51.2(2) . . . . ? N2 Li1 Li2 C4 -94.03(14) . . . . ? N1 Li1 Li2 C4 88.99(14) . . . . ? C2 Li1 Li2 C4 -37.72(19) . . . . ? C13 Li1 Li2 C4 -68.9(3) . . . . ? C1 Li1 Li2 C4 -3.09(18) 2_756 . . . ? Si1 Li1 Li2 C4 122.11(12) . . . . ? N2 Li1 Li2 Si2 29.66(6) . . . . ? N1 Li1 Li2 Si2 -147.32(12) . . . . ? C2 Li1 Li2 Si2 85.97(13) . . . . ? C13 Li1 Li2 Si2 54.7(2) . . . . ? C1 Li1 Li2 Si2 120.60(11) 2_756 . . . ? Si1 Li1 Li2 Si2 -114.20(7) . . . . ? C11 C12 Li2 N1 -40.30(16) . . . . ? C7 C12 Li2 N1 -163.07(12) . . . . ? C3 C12 Li2 N1 74.71(12) . . . . ? C11 C12 Li2 N2 165.5(4) . . . . ? C7 C12 Li2 N2 42.8(5) . . . . ? C3 C12 Li2 N2 -79.5(5) . . . . ? C11 C12 Li2 C3 -115.01(15) . . . . ? C7 C12 Li2 C3 122.22(13) . . . . ? C11 C12 Li2 Li1 -54.6(3) . . . . ? C7 C12 Li2 Li1 -177.4(2) . . . . ? C3 C12 Li2 Li1 60.4(2) . . . . ? C11 C12 Li2 C4 -147.27(13) . . . . ? C7 C12 Li2 C4 89.96(10) . . . . ? C3 C12 Li2 C4 -32.26(8) . . . . ? C11 C12 Li2 Si2 102.3(2) . . . . ? C7 C12 Li2 Si2 -20.5(2) . . . . ? C3 C12 Li2 Si2 -142.7(2) . . . . ? C3 C4 Li2 N1 -47.41(12) . . . . ? N2 C4 Li2 N1 64.04(16) 2_756 . . . ? C5 C4 Li2 N1 -169.95(13) . . . . ? C3 C4 Li2 N2 -159.45(16) . . . . ? N2 C4 Li2 N2 -48.01(16) 2_756 . . . ? C5 C4 Li2 N2 78.01(14) . . . . ? N2 C4 Li2 C3 111.45(15) 2_756 . . . ? C5 C4 Li2 C3 -122.54(13) . . . . ? C3 C4 Li2 Li1 -102.82(15) . . . . ? N2 C4 Li2 Li1 8.63(19) 2_756 . . . ? C5 C4 Li2 Li1 134.64(14) . . . . ? C3 C4 Li2 C12 34.89(8) . . . . ? N2 C4 Li2 C12 146.34(12) 2_756 . . . ? C5 C4 Li2 C12 -87.65(10) . . . . ? C3 C4 Li2 Si2 168.66(16) . . . . ? N2 C4 Li2 Si2 -79.89(16) 2_756 . . . ? C5 C4 Li2 Si2 46.12(15) . . . . ? C37 C38 Li3 N4 161.4(4) . . . . ? C33 C38 Li3 N4 40.5(4) . . . . ? C29 C38 Li3 N4 -81.8(4) 2_757 . . . ? C37 C38 Li3 N3 -42.18(14) . . . . ? C33 C38 Li3 N3 -163.11(11) . . . . ? C29 C38 Li3 N3 74.63(11) 2_757 . . . ? C37 C38 Li3 C29 -116.80(13) . . . 2_757 ? C33 C38 Li3 C29 122.27(12) . . . 2_757 ? C37 C38 Li3 Li4 -56.8(3) . . . . ? C33 C38 Li3 Li4 -177.8(2) . . . . ? C29 C38 Li3 Li4 60.0(2) 2_757 . . . ? C37 C38 Li3 C30 -148.47(11) . . . 2_757 ? C33 C38 Li3 C30 90.60(9) . . . 2_757 ? C29 C38 Li3 C30 -31.67(7) 2_757 . . 2_757 ? C37 C38 Li3 Si4 102.18(18) . . . . ? C33 C38 Li3 Si4 -18.75(18) . . . . ? C29 C38 Li3 Si4 -141.01(19) 2_757 . . . ? N3 Li4 Li3 N4 -176.89(15) . . . . ? C28 Li4 Li3 N4 57.11(13) . . . . ? C46 Li4 Li3 N4 25.7(2) . . . . ? C27 Li4 Li3 N4 91.40(13) . . . . ? Si3 Li4 Li3 N4 -144.08(12) . . . . ? N4 Li4 Li3 N3 176.89(15) . . . . ? C28 Li4 Li3 N3 -126.00(17) . . . . ? C46 Li4 Li3 N3 -157.5(3) . . . . ? C27 Li4 Li3 N3 -91.71(13) . . . . ? Si3 Li4 Li3 N3 32.81(6) . . . . ? N4 Li4 Li3 C29 -129.52(16) . . . 2_757 ? N3 Li4 Li3 C29 53.60(13) . . . 2_757 ? C28 Li4 Li3 C29 -72.40(19) . . . 2_757 ? C46 Li4 Li3 C29 -103.9(2) . . . 2_757 ? C27 Li4 Li3 C29 -38.12(19) . . . 2_757 ? Si3 Li4 Li3 C29 86.41(13) . . . 2_757 ? N4 Li4 Li3 C38 -164.6(3) . . . . ? N3 Li4 Li3 C38 18.5(2) . . . . ? C28 Li4 Li3 C38 -107.5(2) . . . . ? C46 Li4 Li3 C38 -139.0(2) . . . . ? C27 Li4 Li3 C38 -73.2(3) . . . . ? Si3 Li4 Li3 C38 51.3(2) . . . . ? N4 Li4 Li3 C30 -93.93(14) . . . 2_757 ? N3 Li4 Li3 C30 89.18(14) . . . 2_757 ? C28 Li4 Li3 C30 -36.8(2) . . . 2_757 ? C46 Li4 Li3 C30 -68.3(3) . . . 2_757 ? C27 Li4 Li3 C30 -2.54(19) . . . 2_757 ? Si3 Li4 Li3 C30 121.99(12) . . . 2_757 ? N4 Li4 Li3 Si4 29.23(6) . . . . ? N3 Li4 Li3 Si4 -147.66(11) . . . . ? C28 Li4 Li3 Si4 86.34(13) . . . . ? C46 Li4 Li3 Si4 54.9(2) . . . . ? C27 Li4 Li3 Si4 120.62(11) . . . . ? Si3 Li4 Li3 Si4 -114.85(7) . . . . ? C2 C1 N1 Si1 -129.20(12) 2_756 . . . ? C20 C1 N1 Si1 51.72(16) . . . . ? Li1 C1 N1 Si1 162.60(9) 2_756 . . . ? C2 C1 N1 Li2 17.05(17) 2_756 . . . ? C20 C1 N1 Li2 -162.04(13) . . . . ? Li1 C1 N1 Li2 -51.16(15) 2_756 . . . ? C2 C1 N1 Li1 102.38(16) 2_756 . . . ? C20 C1 N1 Li1 -76.70(17) . . . . ? Li1 C1 N1 Li1 34.18(15) 2_756 . . . ? N2 Li2 N1 C1 121.52(13) . . . . ? C3 Li2 N1 C1 -16.69(13) . . . . ? Li1 Li2 N1 C1 119.05(13) . . . . ? C12 Li2 N1 C1 -50.21(13) . . . . ? C4 Li2 N1 C1 6.47(15) . . . . ? Si2 Li2 N1 C1 154.61(10) . . . . ? N2 Li2 N1 Si1 -91.25(13) . . . . ? C3 Li2 N1 Si1 130.54(9) . . . . ? Li1 Li2 N1 Si1 -93.72(12) . . . . ? C12 Li2 N1 Si1 97.02(11) . . . . ? C4 Li2 N1 Si1 153.70(8) . . . . ? Si2 Li2 N1 Si1 -58.16(15) . . . . ? N2 Li2 N1 Li1 2.47(13) . . . . ? C3 Li2 N1 Li1 -135.74(12) . . . . ? C12 Li2 N1 Li1 -169.26(13) . . . . ? C4 Li2 N1 Li1 -112.58(13) . . . . ? Si2 Li2 N1 Li1 35.56(12) . . . . ? N2 Li1 N1 C1 -108.46(14) . . . . ? C2 Li1 N1 C1 -12.4(3) . . . . ? Li2 Li1 N1 C1 -105.98(15) . . . . ? C13 Li1 N1 C1 37.7(4) . . . . ? C1 Li1 N1 C1 2.39(16) 2_756 . . . ? Si1 Li1 N1 C1 137.03(15) . . . . ? N2 Li1 N1 Si1 114.51(11) . . . . ? C2 Li1 N1 Si1 -149.39(16) . . . . ? Li2 Li1 N1 Si1 116.99(11) . . . . ? C13 Li1 N1 Si1 -99.3(4) . . . . ? C1 Li1 N1 Si1 -134.65(9) 2_756 . . . ? N2 Li1 N1 Li2 -2.48(13) . . . . ? C2 Li1 N1 Li2 93.6(2) . . . . ? C13 Li1 N1 Li2 143.7(4) . . . . ? C1 Li1 N1 Li2 108.36(13) 2_756 . . . ? Si1 Li1 N1 Li2 -116.99(11) . . . . ? N1 Li1 N2 C4 117.51(13) . . . 2_756 ? C2 Li1 N2 C4 -17.22(13) . . . 2_756 ? Li2 Li1 N2 C4 115.04(14) . . . 2_756 ? C13 Li1 N2 C4 -50.41(14) . . . 2_756 ? C1 Li1 N2 C4 6.00(15) 2_756 . . 2_756 ? Si1 Li1 N2 C4 154.07(11) . . . 2_756 ? N1 Li1 N2 Si2 -98.19(14) . . . . ? C2 Li1 N2 Si2 127.08(10) . . . . ? Li2 Li1 N2 Si2 -100.66(13) . . . . ? C13 Li1 N2 Si2 93.89(11) . . . . ? C1 Li1 N2 Si2 150.30(8) 2_756 . . . ? Si1 Li1 N2 Si2 -61.64(16) . . . . ? N1 Li1 N2 Li2 2.47(13) . . . . ? C2 Li1 N2 Li2 -132.26(13) . . . . ? C13 Li1 N2 Li2 -165.45(13) . . . . ? C1 Li1 N2 Li2 -109.04(13) 2_756 . . . ? Si1 Li1 N2 Li2 39.03(13) . . . . ? N1 Li2 N2 C4 -107.41(14) . . . 2_756 ? C3 Li2 N2 C4 -11.3(3) . . . 2_756 ? Li1 Li2 N2 C4 -104.93(14) . . . 2_756 ? C12 Li2 N2 C4 45.8(5) . . . 2_756 ? C4 Li2 N2 C4 4.94(16) . . . 2_756 ? Si2 Li2 N2 C4 134.82(14) . . . 2_756 ? N1 Li2 N2 Si2 117.77(11) . . . . ? C3 Li2 N2 Si2 -146.13(18) . . . . ? Li1 Li2 N2 Si2 120.26(11) . . . . ? C12 Li2 N2 Si2 -89.0(5) . . . . ? C4 Li2 N2 Si2 -129.88(10) . . . . ? N1 Li2 N2 Li1 -2.48(13) . . . . ? C3 Li2 N2 Li1 93.6(2) . . . . ? C12 Li2 N2 Li1 150.7(5) . . . . ? C4 Li2 N2 Li1 109.86(14) . . . . ? Si2 Li2 N2 Li1 -120.26(11) . . . . ? N4 Li3 N3 C27 121.79(13) . . . 2_757 ? C29 Li3 N3 C27 -15.91(13) 2_757 . . 2_757 ? C38 Li3 N3 C27 -50.06(13) . . . 2_757 ? Li4 Li3 N3 C27 119.21(13) . . . 2_757 ? C30 Li3 N3 C27 6.93(16) 2_757 . . 2_757 ? Si4 Li3 N3 C27 155.34(11) . . . 2_757 ? N4 Li3 N3 Si3 -91.58(13) . . . . ? C29 Li3 N3 Si3 130.73(9) 2_757 . . . ? C38 Li3 N3 Si3 96.58(11) . . . . ? Li4 Li3 N3 Si3 -94.15(12) . . . . ? C30 Li3 N3 Si3 153.56(8) 2_757 . . . ? Si4 Li3 N3 Si3 -58.02(16) . . . . ? N4 Li3 N3 Li4 2.57(13) . . . . ? C29 Li3 N3 Li4 -135.12(12) 2_757 . . . ? C38 Li3 N3 Li4 -169.27(12) . . . . ? C30 Li3 N3 Li4 -112.29(13) 2_757 . . . ? Si4 Li3 N3 Li4 36.13(13) . . . . ? N4 Li4 N3 C27 -107.49(15) . . . 2_757 ? C28 Li4 N3 C27 -11.7(3) . . . 2_757 ? C46 Li4 N3 C27 37.3(4) . . . 2_757 ? Li3 Li4 N3 C27 -104.94(14) . . . 2_757 ? C27 Li4 N3 C27 3.39(17) . . . 2_757 ? Si3 Li4 N3 C27 137.96(15) . . . 2_757 ? N4 Li4 N3 Si3 114.55(11) . . . . ? C28 Li4 N3 Si3 -149.63(17) . . . . ? C46 Li4 N3 Si3 -100.7(4) . . . . ? Li3 Li4 N3 Si3 117.10(10) . . . . ? C27 Li4 N3 Si3 -134.57(9) . . . . ? N4 Li4 N3 Li3 -2.55(12) . . . . ? C28 Li4 N3 Li3 93.3(2) . . . . ? C46 Li4 N3 Li3 142.2(4) . . . . ? C27 Li4 N3 Li3 108.33(13) . . . . ? Si3 Li4 N3 Li3 -117.10(11) . . . . ? C29 C30 N4 Si4 -130.76(13) . . . . ? C31 C30 N4 Si4 49.65(18) . . . . ? Li3 C30 N4 Si4 159.50(9) 2_757 . . . ? C29 C30 N4 Li3 101.08(17) . . . . ? C31 C30 N4 Li3 -78.51(17) . . . . ? Li3 C30 N4 Li3 31.33(15) 2_757 . . . ? C29 C30 N4 Li4 18.4(2) . . . . ? C31 C30 N4 Li4 -161.14(14) . . . . ? Li3 C30 N4 Li4 -51.30(17) 2_757 . . . ? N3 Li3 N4 C30 -107.13(14) . . . . ? C29 Li3 N4 C30 -9.7(3) 2_757 . . . ? C38 Li3 N4 C30 48.4(5) . . . . ? Li4 Li3 N4 C30 -104.56(14) . . . . ? C30 Li3 N4 C30 5.27(16) 2_757 . . . ? Si4 Li3 N4 C30 133.42(15) . . . . ? N3 Li3 N4 Si4 119.45(11) . . . . ? C29 Li3 N4 Si4 -143.16(18) 2_757 . . . ? C38 Li3 N4 Si4 -85.1(4) . . . . ? Li4 Li3 N4 Si4 122.02(11) . . . . ? C30 Li3 N4 Si4 -128.15(9) 2_757 . . . ? N3 Li3 N4 Li4 -2.57(13) . . . . ? C29 Li3 N4 Li4 94.8(2) 2_757 . . . ? C38 Li3 N4 Li4 152.9(4) . . . . ? C30 Li3 N4 Li4 109.83(13) 2_757 . . . ? Si4 Li3 N4 Li4 -122.02(11) . . . . ? N3 Li4 N4 C30 116.76(13) . . . . ? C28 Li4 N4 C30 -16.97(14) . . . . ? C46 Li4 N4 C30 -50.69(14) . . . . ? Li3 Li4 N4 C30 114.21(13) . . . . ? C27 Li4 N4 C30 5.75(16) . . . . ? Si3 Li4 N4 C30 153.07(12) . . . . ? N3 Li4 N4 Si4 -96.65(14) . . . . ? C28 Li4 N4 Si4 129.62(10) . . . . ? C46 Li4 N4 Si4 95.90(12) . . . . ? Li3 Li4 N4 Si4 -99.20(13) . . . . ? C27 Li4 N4 Si4 152.34(9) . . . . ? Si3 Li4 N4 Si4 -60.34(17) . . . . ? N3 Li4 N4 Li3 2.55(12) . . . . ? C28 Li4 N4 Li3 -131.18(12) . . . . ? C46 Li4 N4 Li3 -164.90(13) . . . . ? C27 Li4 N4 Li3 -108.46(13) . . . . ? Si3 Li4 N4 Li3 38.86(13) . . . . ? C1 N1 Si1 C21 125.76(11) . . . . ? Li2 N1 Si1 C21 -18.12(13) . . . . ? Li1 N1 Si1 C21 -96.70(11) . . . . ? C1 N1 Si1 C23 6.02(15) . . . . ? Li2 N1 Si1 C23 -137.85(13) . . . . ? Li1 N1 Si1 C23 143.57(12) . . . . ? C1 N1 Si1 C22 -114.97(12) . . . . ? Li2 N1 Si1 C22 101.15(13) . . . . ? Li1 N1 Si1 C22 22.57(12) . . . . ? C1 N1 Si1 Li1 -137.54(15) . . . . ? Li2 N1 Si1 Li1 78.58(14) . . . . ? N2 Li1 Si1 N1 -78.68(14) . . . . ? C2 Li1 Si1 N1 77.3(3) . . . . ? Li2 Li1 Si1 N1 -47.29(10) . . . . ? C13 Li1 Si1 N1 143.3(2) . . . . ? C1 Li1 Si1 N1 60.68(13) 2_756 . . . ? N2 Li1 Si1 C21 20.51(16) . . . . ? N1 Li1 Si1 C21 99.19(10) . . . . ? C2 Li1 Si1 C21 176.5(3) . . . . ? Li2 Li1 Si1 C21 51.90(12) . . . . ? C13 Li1 Si1 C21 -117.54(19) . . . . ? C1 Li1 Si1 C21 159.87(12) 2_756 . . . ? N2 Li1 Si1 C23 -146.52(15) . . . . ? N1 Li1 Si1 C23 -67.84(18) . . . . ? C2 Li1 Si1 C23 9.5(4) . . . . ? Li2 Li1 Si1 C23 -115.13(16) . . . . ? C13 Li1 Si1 C23 75.4(3) . . . . ? C1 Li1 Si1 C23 -7.2(2) 2_756 . . . ? N2 Li1 Si1 C22 123.98(15) . . . . ? N1 Li1 Si1 C22 -157.33(12) . . . . ? C2 Li1 Si1 C22 -80.0(3) . . . . ? Li2 Li1 Si1 C22 155.38(12) . . . . ? C13 Li1 Si1 C22 -14.07(18) . . . . ? C1 Li1 Si1 C22 -96.65(14) 2_756 . . . ? C4 N2 Si2 C25 137.59(11) 2_756 . . . ? Li1 N2 Si2 C25 -4.24(13) . . . . ? Li2 N2 Si2 C25 -87.19(11) . . . . ? C4 N2 Si2 C24 18.60(14) 2_756 . . . ? Li1 N2 Si2 C24 -123.23(13) . . . . ? Li2 N2 Si2 C24 153.83(12) . . . . ? C4 N2 Si2 C26 -103.21(13) 2_756 . . . ? Li1 N2 Si2 C26 114.96(13) . . . . ? Li2 N2 Si2 C26 32.02(13) . . . . ? C4 N2 Si2 Li2 -135.23(16) 2_756 . . . ? Li1 N2 Si2 Li2 82.94(14) . . . . ? N1 Li2 Si2 N2 -74.53(14) . . . . ? C3 Li2 Si2 N2 81.8(3) . . . . ? Li1 Li2 Si2 N2 -45.63(10) . . . . ? C12 Li2 Si2 N2 148.7(2) . . . . ? C4 Li2 Si2 N2 65.69(13) . . . . ? N1 Li2 Si2 C25 29.84(14) . . . . ? N2 Li2 Si2 C25 104.37(11) . . . . ? C3 Li2 Si2 C25 -173.8(3) . . . . ? Li1 Li2 Si2 C25 58.74(10) . . . . ? C12 Li2 Si2 C25 -106.98(19) . . . . ? C4 Li2 Si2 C25 170.06(12) . . . . ? N1 Li2 Si2 C24 -121.94(17) . . . . ? N2 Li2 Si2 C24 -47.41(19) . . . . ? C3 Li2 Si2 C24 34.4(4) . . . . ? Li1 Li2 Si2 C24 -93.04(17) . . . . ? C12 Li2 Si2 C24 101.2(2) . . . . ? C4 Li2 Si2 C24 18.3(2) . . . . ? N1 Li2 Si2 C26 135.59(15) . . . . ? N2 Li2 Si2 C26 -149.89(12) . . . . ? C3 Li2 Si2 C26 -68.0(3) . . . . ? Li1 Li2 Si2 C26 164.48(11) . . . . ? C12 Li2 Si2 C26 -1.24(19) . . . . ? C4 Li2 Si2 C26 -84.20(14) . . . . ? C27 N3 Si3 C47 3.41(16) 2_757 . . . ? Li3 N3 Si3 C47 -139.62(14) . . . . ? Li4 N3 Si3 C47 142.01(12) . . . . ? C27 N3 Si3 C48 123.93(12) 2_757 . . . ? Li3 N3 Si3 C48 -19.10(14) . . . . ? Li4 N3 Si3 C48 -97.47(11) . . . . ? C27 N3 Si3 C49 -118.00(13) 2_757 . . . ? Li3 N3 Si3 C49 98.96(14) . . . . ? Li4 N3 Si3 C49 20.59(13) . . . . ? C27 N3 Si3 Li4 -138.60(16) 2_757 . . . ? Li3 N3 Si3 Li4 78.37(14) . . . . ? N4 Li4 Si3 N3 -78.65(14) . . . . ? C28 Li4 Si3 N3 74.4(3) . . . . ? C46 Li4 Si3 N3 142.7(2) . . . . ? Li3 Li4 Si3 N3 -47.44(10) . . . . ? C27 Li4 Si3 N3 60.19(13) . . . . ? N4 Li4 Si3 C47 -146.67(15) . . . . ? N3 Li4 Si3 C47 -68.02(18) . . . . ? C28 Li4 Si3 C47 6.4(4) . . . . ? C46 Li4 Si3 C47 74.7(3) . . . . ? Li3 Li4 Si3 C47 -115.46(17) . . . . ? C27 Li4 Si3 C47 -7.8(2) . . . . ? N4 Li4 Si3 C48 21.06(16) . . . . ? N3 Li4 Si3 C48 99.71(11) . . . . ? C28 Li4 Si3 C48 174.1(3) . . . . ? C46 Li4 Si3 C48 -117.6(2) . . . . ? Li3 Li4 Si3 C48 52.27(11) . . . . ? C27 Li4 Si3 C48 159.90(12) . . . . ? N4 Li4 Si3 C49 122.09(16) . . . . ? N3 Li4 Si3 C49 -159.26(13) . . . . ? C28 Li4 Si3 C49 -84.9(3) . . . . ? C46 Li4 Si3 C49 -16.58(19) . . . . ? Li3 Li4 Si3 C49 153.30(12) . . . . ? C27 Li4 Si3 C49 -99.07(15) . . . . ? C30 N4 Si4 C50 141.46(12) . . . . ? Li3 N4 Si4 C50 -85.08(12) . . . . ? Li4 N4 Si4 C50 -2.81(15) . . . . ? C30 N4 Si4 C51 21.65(14) . . . . ? Li3 N4 Si4 C51 155.11(11) . . . . ? Li4 N4 Si4 C51 -122.62(13) . . . . ? C30 N4 Si4 C52 -100.09(13) . . . . ? Li3 N4 Si4 C52 33.37(13) . . . . ? Li4 N4 Si4 C52 115.64(15) . . . . ? C30 N4 Si4 Li3 -133.46(16) . . . . ? Li4 N4 Si4 Li3 82.27(15) . . . . ? N3 Li3 Si4 N4 -73.71(14) . . . . ? C29 Li3 Si4 N4 84.5(3) 2_757 . . . ? C38 Li3 Si4 N4 148.1(2) . . . . ? Li4 Li3 Si4 N4 -44.53(10) . . . . ? C30 Li3 Si4 N4 67.48(12) 2_757 . . . ? N4 Li3 Si4 C50 105.82(11) . . . . ? N3 Li3 Si4 C50 32.12(15) . . . . ? C29 Li3 Si4 C50 -169.7(3) 2_757 . . . ? C38 Li3 Si4 C50 -106.12(18) . . . . ? Li4 Li3 Si4 C50 61.30(11) . . . . ? C30 Li3 Si4 C50 173.30(13) 2_757 . . . ? N4 Li3 Si4 C51 -45.85(19) . . . . ? N3 Li3 Si4 C51 -119.56(16) . . . . ? C29 Li3 Si4 C51 38.6(4) 2_757 . . . ? C38 Li3 Si4 C51 102.2(2) . . . . ? Li4 Li3 Si4 C51 -90.38(17) . . . . ? C30 Li3 Si4 C51 21.6(2) 2_757 . . . ? N4 Li3 Si4 C52 -148.98(12) . . . . ? N3 Li3 Si4 C52 137.32(15) . . . . ? C29 Li3 Si4 C52 -64.5(3) 2_757 . . . ? C38 Li3 Si4 C52 -0.92(17) . . . . ? Li4 Li3 Si4 C52 166.49(11) . . . . ? C30 Li3 Si4 C52 -81.50(14) 2_757 . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.665 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.082 # Attachment '2d.cif' data_1217newintabs _database_code_depnum_ccdc_archive 'CCDC 855074' #TrackingRef '2d.cif'_database_code_CSD 'CCDC 855074' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C68 H92 Cl2 N4 O4 Si4 Y2' _chemical_formula_sum 'C68 H92 Cl2 N4 O4 Si4 Y2' _chemical_melting_point ? _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _diffrn_ambient_temperature 100(1) _chemical_formula_weight 1390.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0818 0.0705 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1485 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7963 3.5668 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_int_tables_number 4 _chemical_absolute_configuration ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.6878(9) _cell_length_b 29.465(3) _cell_length_c 20.484(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.581(2) _cell_angle_gamma 90.00 _cell_volume 6934.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 2979 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 19.16 _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 1.860 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8525 _exptl_absorpt_correction_T_max 0.9643 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'kappa X8 APEX II Bruker ICMMO' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67228 _diffrn_reflns_av_R_equivalents 0.1505 _diffrn_reflns_av_sigmaI/netI 0.2965 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 30.53 _reflns_number_total 25871 _reflns_number_gt 12984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'Ortep-3 for Windows (L. J. Farrugia, J. Appl. Cryst (1997), 30, 565)' ; _computing_publication_material ; 'WINGX (Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838)' ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1057P)^2^+18.0217P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(8) _refine_ls_number_reflns 25871 _refine_ls_number_parameters 1040 _refine_ls_number_restraints 182 _refine_ls_R_factor_all 0.1694 _refine_ls_R_factor_gt 0.0918 _refine_ls_wR_factor_ref 0.2552 _refine_ls_wR_factor_gt 0.2065 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; SIMU 0.040 0.080 1.700 C95 C96 C97 C98 O5 SIMU 0.040 0.080 1.700 C99 C100 C101 C102 O6 SIMU 0.040 0.080 1.700 C127 C128 C129 C130 O8 SIMU 0.040 0.080 1.700 C123 C124 C125 C126 O7 SIMU 0.040 0.080 1.700 C27 C28 C29 C30 O1 ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7783(12) 0.4616(5) 0.4839(8) 0.0232(12) Uani 1 1 d . . . C2 C 0.6745(12) 0.4548(5) 0.5127(8) 0.0232(12) Uani 1 1 d . . . C3 C 0.5643(13) 0.4757(5) 0.4829(8) 0.0261(11) Uani 1 1 d . . . C5 C 0.3894(13) 0.5178(5) 0.4954(8) 0.0261(11) Uani 1 1 d . . . H5 H 0.3524 0.5370 0.5209 0.031 Uiso 1 1 calc R . . C6 C 0.3296(13) 0.5005(5) 0.4389(7) 0.0261(11) Uani 1 1 d . . . H6 H 0.2522 0.5090 0.4255 0.031 Uiso 1 1 calc R . . C7 C 0.3798(13) 0.4691(5) 0.3975(8) 0.0261(11) Uani 1 1 d . . . C8 C 0.3211(13) 0.4538(5) 0.3378(7) 0.0261(11) Uani 1 1 d . . . H8 H 0.2428 0.4608 0.3240 0.031 Uiso 1 1 calc R . . C9 C 0.3790(13) 0.4278(5) 0.2979(8) 0.0261(11) Uani 1 1 d . . . H9 H 0.3411 0.4192 0.2557 0.031 Uiso 1 1 calc R . . C10 C 0.4931(12) 0.4146(5) 0.3203(7) 0.0261(11) Uani 1 1 d . . . H10 H 0.5289 0.3960 0.2935 0.031 Uiso 1 1 calc R . . C11 C 0.5558(13) 0.4280(5) 0.3810(7) 0.0261(11) Uani 1 1 d . . . H11 H 0.6324 0.4184 0.3943 0.031 Uiso 1 1 calc R . . C12 C 0.5018(13) 0.4571(5) 0.4244(8) 0.0261(11) Uani 1 1 d . . . C13 C 0.8819(12) 0.4359(5) 0.5076(8) 0.0232(12) Uani 1 1 d . . . H13 H 0.9480 0.4405 0.4892 0.028 Uiso 1 1 calc R . . C14 C 0.8839(12) 0.4039(5) 0.5582(7) 0.0232(12) Uani 1 1 d . . . H14 H 0.9513 0.3874 0.5735 0.028 Uiso 1 1 calc R . . C15 C 0.7815(12) 0.3963(5) 0.5869(8) 0.0232(12) Uani 1 1 d . . . C17 C 0.6815(12) 0.3515(5) 0.6587(8) 0.0232(12) Uani 1 1 d . . . H17 H 0.6833 0.3297 0.6917 0.028 Uiso 1 1 calc R . . C18 C 0.5764(13) 0.3744(5) 0.6301(8) 0.0232(12) Uani 1 1 d . . . H18 H 0.5065 0.3662 0.6424 0.028 Uiso 1 1 calc R . . C19 C 0.5786(12) 0.4076(5) 0.5856(8) 0.0232(12) Uani 1 1 d . . . H19 H 0.5096 0.4227 0.5689 0.028 Uiso 1 1 calc R . . C20 C 0.6783(12) 0.4204(5) 0.5637(8) 0.0232(12) Uani 1 1 d . . . C32 C 1.0049(12) 0.5059(6) 0.6792(8) 0.032(4) Uani 1 1 d U . . H32A H 1.0274 0.5306 0.7102 0.039 Uiso 1 1 calc R . . H32B H 1.0182 0.4773 0.7028 0.039 Uiso 1 1 calc R . . C35 C 0.9091(13) 0.7659(5) 0.5964(8) 0.0289(13) Uani 1 1 d . . . C37 C 0.9233(12) 0.7802(5) 0.4741(8) 0.0251(11) Uani 1 1 d . . . C38 C 0.9486(12) 0.7482(5) 0.4286(8) 0.0251(11) Uani 1 1 d . . . C39 C 0.9169(12) 0.7615(5) 0.3581(8) 0.0251(11) Uani 1 1 d . . . H39 H 0.9313 0.7414 0.3255 0.030 Uiso 1 1 calc R . . C40 C 0.8677(12) 0.8019(5) 0.3397(8) 0.0251(11) Uani 1 1 d . . . H40 H 0.8521 0.8092 0.2948 0.030 Uiso 1 1 calc R . . C41 C 0.8388(12) 0.8337(5) 0.3853(8) 0.0251(11) Uani 1 1 d . . . C42 C 0.7799(12) 0.8763(5) 0.3659(8) 0.0251(11) Uani 1 1 d . . . H42 H 0.7591 0.8834 0.3210 0.030 Uiso 1 1 calc R . . C43 C 0.7533(12) 0.9074(5) 0.4144(8) 0.0251(11) Uani 1 1 d . . . H43 H 0.7163 0.9349 0.4023 0.030 Uiso 1 1 calc R . . C44 C 0.7858(12) 0.8946(5) 0.4815(8) 0.0251(11) Uani 1 1 d . . . H44 H 0.7716 0.9148 0.5140 0.030 Uiso 1 1 calc R . . C45 C 0.8368(12) 0.8541(5) 0.5011(8) 0.0251(11) Uani 1 1 d . . . H45 H 0.8522 0.8469 0.5460 0.030 Uiso 1 1 calc R . . C46 C 0.8672(12) 0.8227(5) 0.4548(8) 0.0251(11) Uani 1 1 d . . . C47 C 0.9709(12) 0.7716(5) 0.6643(8) 0.0289(13) Uani 1 1 d . . . H47 H 0.9332 0.7640 0.6990 0.035 Uiso 1 1 calc R . . C48 C 1.0809(12) 0.7876(5) 0.6789(8) 0.0289(13) Uani 1 1 d . . . H48 H 1.1141 0.7927 0.7232 0.035 Uiso 1 1 calc R . . C49 C 1.1464(13) 0.7965(5) 0.6299(8) 0.0289(13) Uani 1 1 d . . . C50 C 1.2665(12) 0.8114(5) 0.6483(9) 0.0289(13) Uani 1 1 d . . . H50 H 1.3004 0.8163 0.6924 0.035 Uiso 1 1 calc R . . C51 C 1.3274(13) 0.8180(5) 0.5986(8) 0.0289(13) Uani 1 1 d . . . H51 H 1.4063 0.8248 0.6093 0.035 Uiso 1 1 calc R . . C52 C 1.2763(13) 0.8149(5) 0.5344(8) 0.0289(13) Uani 1 1 d . . . H52 H 1.3178 0.8228 0.5015 0.035 Uiso 1 1 calc R . . C53 C 1.1626(13) 0.8001(5) 0.5169(8) 0.0289(13) Uani 1 1 d . . . H53 H 1.1306 0.7962 0.4723 0.035 Uiso 1 1 calc R . . C54 C 1.0954(13) 0.7911(5) 0.5642(8) 0.0289(13) Uani 1 1 d . . . C58 C 1.1563(12) 0.6302(5) 0.4581(8) 0.026(4) Uani 1 1 d U . . H58A H 1.1787 0.6408 0.5030 0.039 Uiso 1 1 calc R . . H58B H 1.2240 0.6202 0.4419 0.039 Uiso 1 1 calc R . . H58C H 1.1026 0.6055 0.4569 0.039 Uiso 1 1 calc R . . C59 C 1.0088(12) 0.6489(5) 0.3243(7) 0.017(3) Uani 1 1 d U . . H59A H 0.9506 0.6284 0.3345 0.025 Uiso 1 1 calc R . . H59B H 1.0653 0.6322 0.3054 0.025 Uiso 1 1 calc R . . H59C H 0.9726 0.6712 0.2930 0.025 Uiso 1 1 calc R . . C60 C 1.1947(12) 0.7188(5) 0.3827(7) 0.018(3) Uani 1 1 d U . . H60A H 1.1572 0.7465 0.3659 0.027 Uiso 1 1 calc R . . H60B H 1.2326 0.7055 0.3495 0.027 Uiso 1 1 calc R . . H60C H 1.2514 0.7251 0.4218 0.027 Uiso 1 1 calc R . . C61 C 0.6928(12) 0.6850(5) 0.3568(6) 0.017(3) Uani 1 1 d . . . H61A H 0.6610 0.6546 0.3563 0.021 Uiso 1 1 calc R . . H61B H 0.7676 0.6838 0.3427 0.021 Uiso 1 1 calc R . . C62 C 0.6085(13) 0.7172(5) 0.3123(8) 0.025(4) Uani 1 1 d U . . H62A H 0.6508 0.7373 0.2878 0.030 Uiso 1 1 calc R . . H62B H 0.5525 0.7001 0.2810 0.030 Uiso 1 1 calc R . . C63 C 0.5477(15) 0.7440(6) 0.3594(9) 0.041(5) Uani 1 1 d U . . H63A H 0.5279 0.7743 0.3422 0.049 Uiso 1 1 calc R . . H63B H 0.4773 0.7288 0.3662 0.049 Uiso 1 1 calc R . . C64 C 0.6333(13) 0.7460(5) 0.4211(10) 0.041(5) Uani 1 1 d . . . H64A H 0.6813 0.7729 0.4217 0.050 Uiso 1 1 calc R . . H64B H 0.5942 0.7472 0.4589 0.050 Uiso 1 1 calc R . . C666 C 0.7805(13) 0.3635(5) 0.6346(8) 0.0232(12) Uani 1 1 d . . . H666 H 0.8498 0.3486 0.6515 0.028 Uiso 1 1 calc R . . N1 N 0.7782(11) 0.4973(4) 0.4379(6) 0.023(3) Uani 1 1 d . . . N2 N 0.5808(11) 0.5324(4) 0.5696(6) 0.0261(11) Uani 1 1 d . . . N3 N 0.8025(10) 0.7437(4) 0.5782(6) 0.020(3) Uani 1 1 d . . . N4 N 0.9957(10) 0.7071(4) 0.4470(7) 0.0251(11) Uani 1 1 d . . . O3 O 0.7038(7) 0.7060(3) 0.4245(5) 0.018(2) Uani 1 1 d U . . Si1 Si 0.8557(4) 0.49149(14) 0.3736(2) 0.0224(10) Uani 1 1 d . . . Si2 Si 0.5219(3) 0.55560(14) 0.6333(2) 0.0178(10) Uani 1 1 d . . . Si3 Si 0.6962(4) 0.75043(17) 0.6280(3) 0.0378(14) Uani 1 1 d . . . Si4 Si 1.0838(3) 0.67839(12) 0.4037(2) 0.0130(9) Uani 1 1 d . . . Cl1 Cl 0.8597(3) 0.60686(11) 0.45021(17) 0.0120(8) Uani 1 1 d . . . Cl2 Cl 0.7128(3) 0.63371(12) 0.56456(18) 0.0175(8) Uani 1 1 d . . . Y1 Y 0.71328(11) 0.55016(4) 0.50315(7) 0.0129(3) Uani 1 1 d . . . Y2 Y 0.86091(11) 0.68980(4) 0.51261(7) 0.0120(3) Uani 1 1 d . . . C4 C 0.5081(13) 0.5070(5) 0.5167(8) 0.0261(11) Uani 1 1 d . . . C21 C 0.7916(12) 0.5300(5) 0.3052(7) 0.022(4) Uani 1 1 d . . . H21A H 0.7150 0.5197 0.2859 0.033 Uiso 1 1 calc R . . H21B H 0.8397 0.5302 0.2719 0.033 Uiso 1 1 calc R . . H21C H 0.7869 0.5602 0.3223 0.033 Uiso 1 1 calc R . . C22 C 1.0115(11) 0.5062(5) 0.3957(8) 0.027(4) Uani 1 1 d . . . H22A H 1.0198 0.5351 0.4176 0.041 Uiso 1 1 calc R . . H22B H 1.0443 0.5077 0.3561 0.041 Uiso 1 1 calc R . . H22C H 1.0514 0.4834 0.4248 0.041 Uiso 1 1 calc R . . C23 C 0.8498(15) 0.4329(5) 0.3411(9) 0.039(5) Uani 1 1 d . . . H23A H 0.8660 0.4119 0.3775 0.059 Uiso 1 1 calc R . . H23B H 0.9067 0.4294 0.3131 0.059 Uiso 1 1 calc R . . H23C H 0.7737 0.4271 0.3158 0.059 Uiso 1 1 calc R . . C24 C 0.6382(12) 0.5698(5) 0.7038(8) 0.027(4) Uani 1 1 d . . . H24A H 0.6778 0.5426 0.7209 0.041 Uiso 1 1 calc R . . H24B H 0.6049 0.5841 0.7381 0.041 Uiso 1 1 calc R . . H24C H 0.6925 0.5902 0.6892 0.041 Uiso 1 1 calc R . . C25 C 0.4359(13) 0.6089(5) 0.6139(8) 0.032(4) Uani 1 1 d . . . H25A H 0.4832 0.6314 0.5978 0.049 Uiso 1 1 calc R . . H25B H 0.4118 0.6198 0.6534 0.049 Uiso 1 1 calc R . . H25C H 0.3686 0.6028 0.5805 0.049 Uiso 1 1 calc R . . C26 C 0.4237(13) 0.5140(6) 0.6611(8) 0.033(4) Uani 1 1 d . . . H26A H 0.3600 0.5078 0.6255 0.049 Uiso 1 1 calc R . . H26B H 0.3944 0.5261 0.6983 0.049 Uiso 1 1 calc R . . H26C H 0.4656 0.4865 0.6740 0.049 Uiso 1 1 calc R . . C27 C 0.4853(11) 0.6179(5) 0.4281(7) 0.022(4) Uani 1 1 d U . . H27A H 0.5261 0.6457 0.4431 0.027 Uiso 1 1 calc R . . H27B H 0.4382 0.6089 0.4603 0.027 Uiso 1 1 calc R . . C28 C 0.4111(11) 0.6242(4) 0.3606(7) 0.0170(17) Uani 1 1 d DU . . H28A H 0.4434 0.6472 0.3354 0.020 Uiso 1 1 calc R . . H28B H 0.3322 0.6326 0.3640 0.020 Uiso 1 1 calc R . . C29 C 0.4147(11) 0.5771(4) 0.3289(7) 0.0170(17) Uani 1 1 d DU . . H29A H 0.3616 0.5562 0.3445 0.020 Uiso 1 1 calc R . . H29B H 0.3961 0.5788 0.2808 0.020 Uiso 1 1 calc R . . C30 C 0.5400(13) 0.5634(5) 0.3527(8) 0.031(4) Uani 1 1 d U . . H30A H 0.5482 0.5306 0.3531 0.037 Uiso 1 1 calc R . . H30B H 0.5899 0.5763 0.3245 0.037 Uiso 1 1 calc R . . C31 C 0.8793(13) 0.5104(5) 0.6454(8) 0.028(4) Uani 1 1 d U . . H31A H 0.8451 0.4807 0.6347 0.034 Uiso 1 1 calc R . . H31B H 0.8347 0.5261 0.6740 0.034 Uiso 1 1 calc R . . C33 C 1.0715(13) 0.5079(6) 0.6228(8) 0.032(4) Uani 1 1 d U . . H33A H 1.0783 0.4779 0.6042 0.038 Uiso 1 1 calc R . . H33B H 1.1488 0.5202 0.6376 0.038 Uiso 1 1 calc R . . C34 C 0.9979(11) 0.5395(5) 0.5716(7) 0.020(4) Uani 1 1 d U . . H34A H 1.0262 0.5704 0.5769 0.023 Uiso 1 1 calc R . . H34B H 0.9998 0.5295 0.5266 0.023 Uiso 1 1 calc R . . C36 C 0.9792(13) 0.7741(5) 0.5482(8) 0.0289(13) Uani 1 1 d . . . C55 C 0.6859(14) 0.8102(6) 0.6551(11) 0.063(7) Uani 1 1 d . . . H55A H 0.7005 0.8115 0.7027 0.095 Uiso 1 1 calc R . . H55B H 0.6094 0.8217 0.6382 0.095 Uiso 1 1 calc R . . H55C H 0.7425 0.8283 0.6384 0.095 Uiso 1 1 calc R . . C56 C 0.7155(15) 0.7127(6) 0.7025(8) 0.039(5) Uani 1 1 d . . . H56A H 0.7246 0.6819 0.6891 0.059 Uiso 1 1 calc R . . H56B H 0.6483 0.7150 0.7231 0.059 Uiso 1 1 calc R . . H56C H 0.7835 0.7219 0.7334 0.059 Uiso 1 1 calc R . . C57 C 0.5537(14) 0.7373(6) 0.5761(10) 0.045(5) Uani 1 1 d . . . H57A H 0.5624 0.7128 0.5465 0.067 Uiso 1 1 calc R . . H57B H 0.5247 0.7636 0.5508 0.067 Uiso 1 1 calc R . . H57C H 0.5000 0.7285 0.6041 0.067 Uiso 1 1 calc R . . C65 C 0.9751(14) 0.6448(5) 0.6653(7) 0.027(4) Uani 1 1 d . . . H65A H 0.9266 0.6179 0.6582 0.032 Uiso 1 1 calc R . . H65B H 0.9364 0.6679 0.6871 0.032 Uiso 1 1 calc R . . C66 C 1.0998(15) 0.6337(6) 0.7055(9) 0.043(5) Uani 1 1 d U . . H66A H 1.1004 0.6341 0.7529 0.051 Uiso 1 1 calc R . . H66B H 1.1260 0.6042 0.6933 0.051 Uiso 1 1 calc R . . C67 C 1.1721(14) 0.6693(6) 0.6870(8) 0.035(4) Uani 1 1 d U . . H67A H 1.2537 0.6609 0.6968 0.042 Uiso 1 1 calc R . . H67B H 1.1612 0.6975 0.7096 0.042 Uiso 1 1 calc R . . C68 C 1.1283(13) 0.6732(6) 0.6126(7) 0.033(4) Uani 1 1 d . . . H68A H 1.1387 0.7039 0.5973 0.040 Uiso 1 1 calc R . . H68B H 1.1695 0.6524 0.5885 0.040 Uiso 1 1 calc R . . C69 C 0.7371(13) 0.1868(5) 0.9593(7) 0.0275(12) Uani 1 1 d . . . C70 C 0.6352(13) 0.1794(5) 0.9852(8) 0.0275(12) Uani 1 1 d . . . C71 C 0.5216(12) 0.2015(5) 0.9610(8) 0.0214(11) Uani 1 1 d . . . C72 C 0.4797(12) 0.2372(5) 0.9938(8) 0.0214(11) Uani 1 1 d . . . C73 C 0.3590(12) 0.2508(5) 0.9685(8) 0.0214(11) Uani 1 1 d . . . H73 H 0.3286 0.2761 0.9864 0.026 Uiso 1 1 calc R . . C74 C 0.2905(12) 0.2269(5) 0.9188(7) 0.0214(11) Uani 1 1 d . . . H74 H 0.2111 0.2331 0.9091 0.026 Uiso 1 1 calc R . . C75 C 0.3365(12) 0.1931(5) 0.8817(7) 0.0214(11) Uani 1 1 d . . . C76 C 0.2627(13) 0.1717(5) 0.8288(7) 0.0214(11) Uani 1 1 d . . . H76 H 0.1851 0.1803 0.8171 0.026 Uiso 1 1 calc R . . C77 C 0.3066(12) 0.1380(5) 0.7951(8) 0.0214(11) Uani 1 1 d . . . H77 H 0.2588 0.1233 0.7602 0.026 Uiso 1 1 calc R . . C78 C 0.4215(12) 0.1260(5) 0.8127(7) 0.0214(11) Uani 1 1 d . . . H78 H 0.4510 0.1040 0.7878 0.026 Uiso 1 1 calc R . . C79 C 0.4959(12) 0.1455(4) 0.8664(7) 0.0214(11) Uani 1 1 d . . . H79 H 0.5729 0.1362 0.8786 0.026 Uiso 1 1 calc R . . C80 C 0.4476(12) 0.1805(5) 0.9017(8) 0.0214(11) Uani 1 1 d . . . C81 C 0.8377(14) 0.1573(5) 0.9788(8) 0.0275(12) Uani 1 1 d . . . H81 H 0.9023 0.1602 0.9586 0.033 Uiso 1 1 calc R . . C82 C 0.8361(13) 0.1254(5) 1.0272(7) 0.0275(12) Uani 1 1 d . . . H82 H 0.9010 0.1069 1.0391 0.033 Uiso 1 1 calc R . . C83 C 0.7415(13) 0.1193(5) 1.0599(8) 0.0275(12) Uani 1 1 d . . . C84 C 0.7401(14) 0.0840(5) 1.1076(7) 0.0275(12) Uani 1 1 d . . . H84 H 0.8055 0.0659 1.1204 0.033 Uiso 1 1 calc R . . C85 C 0.6438(13) 0.0768(5) 1.1343(8) 0.0275(12) Uani 1 1 d . . . H85 H 0.6455 0.0550 1.1673 0.033 Uiso 1 1 calc R . . C86 C 0.5420(14) 0.1017(5) 1.1132(8) 0.0275(12) Uani 1 1 d . . . H86 H 0.4761 0.0951 1.1310 0.033 Uiso 1 1 calc R . . C87 C 0.5369(14) 0.1362(5) 1.0660(8) 0.0275(12) Uani 1 1 d . . . H87 H 0.4684 0.1525 1.0529 0.033 Uiso 1 1 calc R . . C88 C 0.6378(13) 0.1466(5) 1.0376(8) 0.0275(12) Uani 1 1 d . . . C89 C 0.7805(13) 0.1575(5) 0.8084(8) 0.025(4) Uani 1 1 d . . . H89A H 0.8181 0.1350 0.8389 0.038 Uiso 1 1 calc R . . H89B H 0.8107 0.1560 0.7679 0.038 Uiso 1 1 calc R . . H89C H 0.6982 0.1519 0.7991 0.038 Uiso 1 1 calc R . . C90 C 0.9702(12) 0.2233(5) 0.8670(8) 0.049(6) Uani 1 1 d . . . H90A H 0.9885 0.2506 0.8922 0.073 Uiso 1 1 calc R . . H90B H 1.0006 0.2253 0.8266 0.073 Uiso 1 1 calc R . . H90C H 1.0045 0.1978 0.8925 0.073 Uiso 1 1 calc R . . C91 C 0.7572(13) 0.2602(5) 0.7834(8) 0.025(4) Uani 1 1 d . . . H91A H 0.6809 0.2523 0.7599 0.038 Uiso 1 1 calc R . . H91B H 0.8098 0.2622 0.7526 0.038 Uiso 1 1 calc R . . H91C H 0.7540 0.2890 0.8050 0.038 Uiso 1 1 calc R . . C92 C 0.3992(18) 0.2441(7) 1.1402(9) 0.064(7) Uani 1 1 d . . . H92A H 0.3439 0.2317 1.1040 0.096 Uiso 1 1 calc R . . H92B H 0.3585 0.2590 1.1708 0.096 Uiso 1 1 calc R . . H92C H 0.4461 0.2200 1.1626 0.096 Uiso 1 1 calc R . . C93 C 0.6201(14) 0.2984(7) 1.1768(8) 0.049(6) Uani 1 1 d . . . H93A H 0.6483 0.2703 1.1973 0.073 Uiso 1 1 calc R . . H93B H 0.5934 0.3175 1.2090 0.073 Uiso 1 1 calc R . . H93C H 0.6818 0.3134 1.1602 0.073 Uiso 1 1 calc R . . C94 C 0.4175(14) 0.3419(5) 1.0870(8) 0.035(4) Uani 1 1 d . . . H94A H 0.4631 0.3618 1.0649 0.052 Uiso 1 1 calc R . . H94B H 0.4051 0.3558 1.1276 0.052 Uiso 1 1 calc R . . H94C H 0.3438 0.3363 1.0588 0.052 Uiso 1 1 calc R . . C95 C 0.4970(12) 0.2851(4) 0.8336(7) 0.031(4) Uani 1 1 d . . . H95A H 0.4315 0.2666 0.8401 0.037 Uiso 1 1 calc R . . H95B H 0.5546 0.2657 0.8192 0.037 Uiso 1 1 calc R . . C96 C 0.4591(13) 0.3204(5) 0.7845(8) 0.030(3) Uani 1 1 d . . . H96A H 0.4004 0.3091 0.7484 0.036 Uiso 1 1 calc R . . H96B H 0.5240 0.3324 0.7664 0.036 Uiso 1 1 calc R . . C97 C 0.4081(14) 0.3566(5) 0.8258(8) 0.030(3) Uani 1 1 d . . . H97A H 0.4159 0.3868 0.8084 0.036 Uiso 1 1 calc R . . H97B H 0.3267 0.3507 0.8264 0.036 Uiso 1 1 calc R . . C98 C 0.4792(12) 0.3513(4) 0.8917(7) 0.022(4) Uani 1 1 d U . . H98A H 0.4297 0.3506 0.9249 0.027 Uiso 1 1 calc R . . H98B H 0.5322 0.3767 0.9013 0.027 Uiso 1 1 calc R . . C99 C 0.8409(15) 0.2325(6) 1.1232(8) 0.0250(18) Uani 1 1 d . . . H99A H 0.7919 0.2061 1.1118 0.030 Uiso 1 1 calc R . . H99B H 0.8079 0.2511 1.1542 0.030 Uiso 1 1 calc R . . C100 C 0.9607(18) 0.2187(10) 1.1525(10) 0.088(10) Uani 1 1 d . . . H10A H 0.9776 0.2269 1.1991 0.105 Uiso 1 1 calc R . . H10B H 0.9685 0.1861 1.1490 0.105 Uiso 1 1 calc R . . C101 C 1.0405(18) 0.2407(8) 1.1184(12) 0.086(9) Uani 1 1 d . . . H10C H 1.0986 0.2194 1.1089 0.103 Uiso 1 1 calc R . . H10D H 1.0797 0.2653 1.1450 0.103 Uiso 1 1 calc R . . C102 C 0.9712(12) 0.2583(5) 1.0565(8) 0.022(4) Uani 1 1 d . . . H10E H 0.9962 0.2888 1.0481 0.027 Uiso 1 1 calc R . . H10F H 0.9813 0.2392 1.0194 0.027 Uiso 1 1 calc R . . C103 C 0.8885(12) 0.4812(5) 1.0833(8) 0.0233(11) Uani 1 1 d . . . C104 C 0.9677(12) 0.4952(5) 1.0430(8) 0.0233(11) Uani 1 1 d . . . C105 C 0.9369(13) 0.5067(5) 0.9698(8) 0.0297(12) Uani 1 1 d . . . C106 C 0.9596(13) 0.4790(5) 0.9207(8) 0.0297(12) Uani 1 1 d . . . C107 C 0.9418(12) 0.4977(5) 0.8532(8) 0.0297(12) Uani 1 1 d . . . H107 H 0.9558 0.4792 0.8188 0.036 Uiso 1 1 calc R . . C108 C 0.9049(13) 0.5420(5) 0.8386(8) 0.0297(12) Uani 1 1 d . . . H108 H 0.9026 0.5537 0.7962 0.036 Uiso 1 1 calc R . . C109 C 0.8714(13) 0.5689(5) 0.8878(8) 0.0297(12) Uani 1 1 d . . . C110 C 0.8233(13) 0.6105(5) 0.8747(8) 0.0297(12) Uani 1 1 d . . . H110 H 0.8110 0.6211 0.8312 0.036 Uiso 1 1 calc R . . C111 C 0.7923(13) 0.6373(5) 0.9222(8) 0.0297(12) Uani 1 1 d . . . H111 H 0.7624 0.6662 0.9114 0.036 Uiso 1 1 calc R . . C112 C 0.8052(13) 0.6217(5) 0.9865(8) 0.0297(12) Uani 1 1 d . . . H112 H 0.7801 0.6395 1.0186 0.036 Uiso 1 1 calc R . . C113 C 0.8544(13) 0.5802(5) 1.0040(8) 0.0297(12) Uani 1 1 d . . . H113 H 0.8660 0.5709 1.0481 0.036 Uiso 1 1 calc R . . C114 C 0.8879(13) 0.5514(5) 0.9550(8) 0.0297(12) Uani 1 1 d . . . C115 C 0.9164(12) 0.4852(5) 1.1525(8) 0.0233(11) Uani 1 1 d . . . H115 H 0.8617 0.4779 1.1785 0.028 Uiso 1 1 calc R . . C116 C 1.0262(12) 0.5003(5) 1.1818(8) 0.0233(11) Uani 1 1 d . . . H116 H 1.0425 0.5051 1.2275 0.028 Uiso 1 1 calc R . . C117 C 1.1148(12) 0.5087(5) 1.1441(8) 0.0233(11) Uani 1 1 d . . . C118 C 1.2257(12) 0.5213(5) 1.1760(8) 0.0233(11) Uani 1 1 d . . . H118 H 1.2425 0.5239 1.2221 0.028 Uiso 1 1 calc R . . C119 C 1.3109(13) 0.5298(5) 1.1388(8) 0.0233(11) Uani 1 1 d . . . H119 H 1.3866 0.5366 1.1596 0.028 Uiso 1 1 calc R . . C120 C 1.2824(12) 0.5282(5) 1.0706(8) 0.0233(11) Uani 1 1 d . . . H120 H 1.3390 0.5348 1.0454 0.028 Uiso 1 1 calc R . . C121 C 1.1716(12) 0.5171(5) 1.0389(8) 0.0233(11) Uani 1 1 d . . . H121 H 1.1549 0.5159 0.9928 0.028 Uiso 1 1 calc R . . C122 C 1.0826(13) 0.5073(5) 1.0754(8) 0.0233(11) Uani 1 1 d . . . C123 C 0.7054(14) 0.4139(5) 0.8285(7) 0.030(4) Uani 1 1 d U . . H12A H 0.7803 0.4158 0.8146 0.036 Uiso 1 1 calc R . . H12B H 0.6826 0.3822 0.8283 0.036 Uiso 1 1 calc R . . C124 C 0.6181(15) 0.4401(6) 0.7836(9) 0.042(5) Uani 1 1 d U . . H12C H 0.5586 0.4203 0.7597 0.051 Uiso 1 1 calc R . . H12D H 0.6540 0.4566 0.7516 0.051 Uiso 1 1 calc R . . C125 C 0.5648(14) 0.4735(6) 0.8278(9) 0.042(5) Uani 1 1 d U . . H12E H 0.5423 0.5018 0.8050 0.051 Uiso 1 1 calc R . . H12F H 0.4979 0.4604 0.8427 0.051 Uiso 1 1 calc R . . C126 C 0.6636(13) 0.4799(5) 0.8837(8) 0.031(4) Uani 1 1 d U . . H12G H 0.6372 0.4914 0.9227 0.037 Uiso 1 1 calc R . . H12H H 0.7207 0.5007 0.8717 0.037 Uiso 1 1 calc R . . C127 C 0.9384(12) 0.3704(5) 1.1462(7) 0.0250(18) Uani 1 1 d . . . H12I H 0.9019 0.3407 1.1427 0.030 Uiso 1 1 calc R . . H12J H 0.8821 0.3924 1.1557 0.030 Uiso 1 1 calc R . . C128 C 1.0447(14) 0.3702(6) 1.2024(8) 0.041(5) Uani 1 1 d . . . H12K H 1.0430 0.3447 1.2321 0.049 Uiso 1 1 calc R . . H12L H 1.0504 0.3982 1.2277 0.049 Uiso 1 1 calc R . . C129 C 1.1451(18) 0.3658(10) 1.1629(10) 0.084(9) Uani 1 1 d . . . H12M H 1.2132 0.3823 1.1849 0.101 Uiso 1 1 calc R . . H12N H 1.1659 0.3342 1.1589 0.101 Uiso 1 1 calc R . . C130 C 1.1014(12) 0.3850(5) 1.0985(8) 0.0250(18) Uani 1 1 d . . . H13A H 1.1336 0.3688 1.0648 0.030 Uiso 1 1 calc R . . H13B H 1.1247 0.4166 1.0976 0.030 Uiso 1 1 calc R . . C131 C 0.5211(14) 0.4601(6) 1.0152(10) 0.055(6) Uani 1 1 d . . . H13C H 0.4965 0.4860 0.9878 0.083 Uiso 1 1 calc R . . H13D H 0.4585 0.4502 1.0362 0.083 Uiso 1 1 calc R . . H13E H 0.5426 0.4360 0.9883 0.083 Uiso 1 1 calc R . . C132 C 0.6324(14) 0.4410(7) 1.1561(9) 0.053(6) Uani 1 1 d . . . H13F H 0.5937 0.4129 1.1422 0.080 Uiso 1 1 calc R . . H13G H 0.5874 0.4577 1.1827 0.080 Uiso 1 1 calc R . . H13H H 0.7080 0.4347 1.1818 0.080 Uiso 1 1 calc R . . C133 C 0.6359(12) 0.5365(5) 1.0988(8) 0.0233(11) Uani 1 1 d . . . H13I H 0.6911 0.5440 1.1381 0.035 Uiso 1 1 calc R . . H13J H 0.5586 0.5427 1.1061 0.035 Uiso 1 1 calc R . . H13K H 0.6513 0.5543 1.0622 0.035 Uiso 1 1 calc R . . C134 C 1.2058(13) 0.4468(6) 0.8741(8) 0.035(5) Uani 1 1 d . . . H13L H 1.1733 0.4761 0.8613 0.052 Uiso 1 1 calc R . . H13M H 1.2436 0.4351 0.8398 0.052 Uiso 1 1 calc R . . H13N H 1.2614 0.4495 0.9147 0.052 Uiso 1 1 calc R . . C135 C 1.0092(14) 0.3841(6) 0.8050(8) 0.035(4) Uani 1 1 d . . . H13O H 0.9398 0.3686 0.8112 0.052 Uiso 1 1 calc R . . H13P H 1.0595 0.3634 0.7877 0.052 Uiso 1 1 calc R . . H13Q H 0.9891 0.4087 0.7744 0.052 Uiso 1 1 calc R . . C136 C 1.1611(15) 0.3558(5) 0.9355(8) 0.035(4) Uani 1 1 d . . . H13R H 1.1037 0.3373 0.9508 0.052 Uiso 1 1 calc R . . H13S H 1.2166 0.3663 0.9729 0.052 Uiso 1 1 calc R . . H13T H 1.2004 0.3381 0.9070 0.052 Uiso 1 1 calc R . . N5 N 0.7395(11) 0.2208(4) 0.9122(6) 0.0275(12) Uani 1 1 d . . . N6 N 0.5513(9) 0.2604(4) 1.0442(6) 0.020(3) Uani 1 1 d . . . N7 N 0.7790(10) 0.4669(4) 1.0508(7) 0.028(3) Uani 1 1 d . . . N8 N 0.9943(11) 0.4350(4) 0.9320(7) 0.0297(12) Uani 1 1 d . . . O1 O 0.5685(7) 0.5816(3) 0.4193(5) 0.0170(17) Uani 1 1 d U . . O2 O 0.8804(8) 0.5361(3) 0.5857(5) 0.024(3) Uani 1 1 d U . . O4 O 1.0044(8) 0.6616(3) 0.6029(5) 0.018(2) Uani 1 1 d U . . O5 O 0.5462(8) 0.3082(3) 0.8939(5) 0.023(3) Uani 1 1 d U . . O6 O 0.8502(9) 0.2586(3) 1.0634(5) 0.024(3) Uani 1 1 d U . . O7 O 0.7127(8) 0.4334(3) 0.8954(5) 0.026(3) Uani 1 1 d U . . O8 O 0.9739(8) 0.3817(3) 1.0843(5) 0.0250(18) Uani 1 1 d U . . Si5 Si 0.8091(3) 0.21594(14) 0.8467(2) 0.0189(10) Uani 1 1 d . . . Si6 Si 0.4967(4) 0.28684(17) 1.1064(2) 0.0332(13) Uani 1 1 d . . . Si7 Si 0.6485(4) 0.47593(16) 1.0799(3) 0.0387(14) Uani 1 1 d . . . Si8 Si 1.0864(3) 0.40702(14) 0.8869(2) 0.0219(10) Uani 1 1 d . . . Cl3 Cl 0.8501(3) 0.32994(12) 0.9296(2) 0.0222(9) Uani 1 1 d . . . Cl4 Cl 0.6901(3) 0.36008(13) 1.0361(2) 0.0255(10) Uani 1 1 d . . . Y3 Y 0.68816(12) 0.27664(5) 0.97930(7) 0.0178(4) Uani 1 1 d . . . Y4 Y 0.85233(11) 0.41349(5) 0.99079(8) 0.0201(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(3) 0.008(3) 0.036(3) 0.009(2) 0.002(2) 0.005(2) C2 0.025(3) 0.008(3) 0.036(3) 0.009(2) 0.002(2) 0.005(2) C3 0.034(3) 0.020(3) 0.022(3) 0.008(2) -0.002(2) -0.001(2) C5 0.034(3) 0.020(3) 0.022(3) 0.008(2) -0.002(2) -0.001(2) C6 0.034(3) 0.020(3) 0.022(3) 0.008(2) -0.002(2) -0.001(2) C7 0.034(3) 0.020(3) 0.022(3) 0.008(2) -0.002(2) -0.001(2) C8 0.034(3) 0.020(3) 0.022(3) 0.008(2) -0.002(2) -0.001(2) C9 0.034(3) 0.020(3) 0.022(3) 0.008(2) -0.002(2) -0.001(2) C10 0.034(3) 0.020(3) 0.022(3) 0.008(2) -0.002(2) -0.001(2) C11 0.034(3) 0.020(3) 0.022(3) 0.008(2) -0.002(2) -0.001(2) C12 0.034(3) 0.020(3) 0.022(3) 0.008(2) -0.002(2) -0.001(2) C13 0.025(3) 0.008(3) 0.036(3) 0.009(2) 0.002(2) 0.005(2) C14 0.025(3) 0.008(3) 0.036(3) 0.009(2) 0.002(2) 0.005(2) C15 0.025(3) 0.008(3) 0.036(3) 0.009(2) 0.002(2) 0.005(2) C17 0.025(3) 0.008(3) 0.036(3) 0.009(2) 0.002(2) 0.005(2) C18 0.025(3) 0.008(3) 0.036(3) 0.009(2) 0.002(2) 0.005(2) C19 0.025(3) 0.008(3) 0.036(3) 0.009(2) 0.002(2) 0.005(2) C20 0.025(3) 0.008(3) 0.036(3) 0.009(2) 0.002(2) 0.005(2) C32 0.022(9) 0.044(11) 0.030(10) 0.033(8) 0.002(7) 0.008(7) C35 0.026(3) 0.015(3) 0.041(4) -0.009(3) -0.005(2) 0.000(2) C37 0.018(2) 0.013(2) 0.041(3) 0.002(2) -0.002(2) -0.0013(18) C38 0.018(2) 0.013(2) 0.041(3) 0.002(2) -0.002(2) -0.0013(18) C39 0.018(2) 0.013(2) 0.041(3) 0.002(2) -0.002(2) -0.0013(18) C40 0.018(2) 0.013(2) 0.041(3) 0.002(2) -0.002(2) -0.0013(18) C41 0.018(2) 0.013(2) 0.041(3) 0.002(2) -0.002(2) -0.0013(18) C42 0.018(2) 0.013(2) 0.041(3) 0.002(2) -0.002(2) -0.0013(18) C43 0.018(2) 0.013(2) 0.041(3) 0.002(2) -0.002(2) -0.0013(18) C44 0.018(2) 0.013(2) 0.041(3) 0.002(2) -0.002(2) -0.0013(18) C45 0.018(2) 0.013(2) 0.041(3) 0.002(2) -0.002(2) -0.0013(18) C46 0.018(2) 0.013(2) 0.041(3) 0.002(2) -0.002(2) -0.0013(18) C47 0.026(3) 0.015(3) 0.041(4) -0.009(3) -0.005(2) 0.000(2) C48 0.026(3) 0.015(3) 0.041(4) -0.009(3) -0.005(2) 0.000(2) C49 0.026(3) 0.015(3) 0.041(4) -0.009(3) -0.005(2) 0.000(2) C50 0.026(3) 0.015(3) 0.041(4) -0.009(3) -0.005(2) 0.000(2) C51 0.026(3) 0.015(3) 0.041(4) -0.009(3) -0.005(2) 0.000(2) C52 0.026(3) 0.015(3) 0.041(4) -0.009(3) -0.005(2) 0.000(2) C53 0.026(3) 0.015(3) 0.041(4) -0.009(3) -0.005(2) 0.000(2) C54 0.026(3) 0.015(3) 0.041(4) -0.009(3) -0.005(2) 0.000(2) C58 0.019(7) 0.026(7) 0.038(8) -0.006(6) 0.016(6) -0.003(5) C59 0.023(7) 0.018(7) 0.012(7) -0.006(5) 0.009(5) 0.000(5) C60 0.024(7) 0.014(6) 0.017(7) 0.007(6) 0.008(5) 0.001(5) C61 0.020(8) 0.026(9) 0.005(8) 0.004(7) 0.000(6) 0.001(6) C62 0.028(9) 0.022(9) 0.025(10) -0.002(7) 0.004(7) 0.011(7) C63 0.041(11) 0.036(11) 0.039(12) -0.008(9) -0.009(9) 0.020(8) C64 0.015(9) 0.019(9) 0.077(15) -0.001(9) -0.024(9) 0.009(7) C666 0.025(3) 0.008(3) 0.036(3) 0.009(2) 0.002(2) 0.005(2) N1 0.041(8) 0.012(7) 0.017(8) 0.007(6) 0.011(6) -0.010(6) N2 0.034(3) 0.020(3) 0.022(3) 0.008(2) -0.002(2) -0.001(2) N3 0.022(7) 0.016(7) 0.023(8) -0.005(6) 0.008(6) 0.002(5) N4 0.018(2) 0.013(2) 0.041(3) 0.002(2) -0.002(2) -0.0013(18) O3 0.009(5) 0.024(5) 0.020(5) -0.001(4) 0.004(4) 0.009(4) Si1 0.024(2) 0.015(2) 0.029(3) 0.000(2) 0.009(2) 0.0010(18) Si2 0.014(2) 0.022(2) 0.018(3) 0.002(2) 0.0049(17) 0.0015(17) Si3 0.031(3) 0.033(3) 0.056(4) -0.022(3) 0.025(3) 0.000(2) Si4 0.017(2) 0.007(2) 0.015(2) 0.0001(17) 0.0058(17) -0.0024(15) Cl1 0.0177(19) 0.0077(18) 0.012(2) -0.0007(15) 0.0066(15) -0.0010(13) Cl2 0.021(2) 0.015(2) 0.018(2) 0.0000(16) 0.0100(16) 0.0019(15) Y1 0.0137(8) 0.0094(8) 0.0165(9) 0.0036(6) 0.0055(6) -0.0007(6) Y2 0.0150(8) 0.0101(8) 0.0111(8) -0.0027(6) 0.0032(6) 0.0012(6) C4 0.034(3) 0.020(3) 0.022(3) 0.008(2) -0.002(2) -0.001(2) C21 0.012(8) 0.034(10) 0.018(9) -0.008(7) 0.000(6) 0.005(6) C22 0.018(9) 0.016(9) 0.052(12) 0.000(8) 0.023(8) 0.009(6) C23 0.054(12) 0.001(8) 0.061(14) 0.007(8) 0.009(10) -0.001(7) C24 0.024(9) 0.025(9) 0.041(11) -0.001(8) 0.029(8) 0.003(7) C25 0.027(10) 0.043(11) 0.029(11) -0.001(9) 0.010(8) -0.014(8) C26 0.026(10) 0.051(12) 0.024(11) -0.006(9) 0.010(7) 0.002(8) C27 0.015(8) 0.021(9) 0.035(11) 0.006(7) 0.018(7) 0.005(6) C28 0.008(4) 0.022(4) 0.021(4) 0.000(3) 0.000(3) -0.004(3) C29 0.008(4) 0.022(4) 0.021(4) 0.000(3) 0.000(3) -0.004(3) C30 0.036(10) 0.018(9) 0.038(11) 0.009(8) 0.006(8) 0.000(7) C31 0.033(10) 0.007(8) 0.046(12) 0.017(8) 0.008(8) 0.001(6) C33 0.021(9) 0.040(10) 0.028(10) 0.021(8) -0.013(7) 0.005(7) C34 0.018(8) 0.033(10) 0.007(8) 0.005(7) 0.000(6) -0.016(6) C36 0.026(3) 0.015(3) 0.041(4) -0.009(3) -0.005(2) 0.000(2) C55 0.007(9) 0.061(14) 0.12(2) -0.055(13) 0.001(10) 0.013(8) C56 0.052(12) 0.039(11) 0.035(12) -0.020(9) 0.030(9) -0.008(9) C57 0.032(11) 0.031(11) 0.076(16) -0.012(10) 0.021(10) 0.004(8) C65 0.045(11) 0.019(9) 0.021(10) -0.002(7) 0.021(8) 0.005(7) C66 0.066(13) 0.038(11) 0.020(10) 0.016(9) -0.005(9) -0.005(9) C67 0.034(10) 0.038(11) 0.030(11) 0.004(8) -0.002(8) -0.001(8) C68 0.032(10) 0.054(12) 0.011(9) 0.019(8) -0.003(7) -0.010(8) C69 0.034(3) 0.028(3) 0.022(3) -0.002(2) 0.007(2) -0.010(2) C70 0.034(3) 0.028(3) 0.022(3) -0.002(2) 0.007(2) -0.010(2) C71 0.020(2) 0.011(2) 0.034(3) -0.002(2) 0.004(2) -0.0035(18) C72 0.020(2) 0.011(2) 0.034(3) -0.002(2) 0.004(2) -0.0035(18) C73 0.020(2) 0.011(2) 0.034(3) -0.002(2) 0.004(2) -0.0035(18) C74 0.020(2) 0.011(2) 0.034(3) -0.002(2) 0.004(2) -0.0035(18) C75 0.020(2) 0.011(2) 0.034(3) -0.002(2) 0.004(2) -0.0035(18) C76 0.020(2) 0.011(2) 0.034(3) -0.002(2) 0.004(2) -0.0035(18) C77 0.020(2) 0.011(2) 0.034(3) -0.002(2) 0.004(2) -0.0035(18) C78 0.020(2) 0.011(2) 0.034(3) -0.002(2) 0.004(2) -0.0035(18) C79 0.020(2) 0.011(2) 0.034(3) -0.002(2) 0.004(2) -0.0035(18) C80 0.020(2) 0.011(2) 0.034(3) -0.002(2) 0.004(2) -0.0035(18) C81 0.034(3) 0.028(3) 0.022(3) -0.002(2) 0.007(2) -0.010(2) C82 0.034(3) 0.028(3) 0.022(3) -0.002(2) 0.007(2) -0.010(2) C83 0.034(3) 0.028(3) 0.022(3) -0.002(2) 0.007(2) -0.010(2) C84 0.034(3) 0.028(3) 0.022(3) -0.002(2) 0.007(2) -0.010(2) C85 0.034(3) 0.028(3) 0.022(3) -0.002(2) 0.007(2) -0.010(2) C86 0.034(3) 0.028(3) 0.022(3) -0.002(2) 0.007(2) -0.010(2) C87 0.034(3) 0.028(3) 0.022(3) -0.002(2) 0.007(2) -0.010(2) C88 0.034(3) 0.028(3) 0.022(3) -0.002(2) 0.007(2) -0.010(2) C89 0.037(10) 0.015(8) 0.032(10) -0.010(7) 0.025(8) -0.006(7) C90 0.035(11) 0.088(16) 0.023(11) -0.034(10) 0.004(8) 0.004(10) C91 0.035(10) 0.014(9) 0.030(10) -0.006(7) 0.013(8) 0.006(7) C92 0.080(16) 0.097(18) 0.027(13) -0.030(12) 0.039(11) -0.024(13) C93 0.035(11) 0.088(16) 0.023(11) -0.034(10) 0.004(8) 0.004(10) C94 0.037(10) 0.044(11) 0.024(11) -0.023(9) 0.007(8) 0.008(8) C95 0.036(10) 0.018(9) 0.038(11) 0.009(8) 0.006(8) 0.000(7) C96 0.030(7) 0.027(7) 0.033(8) -0.020(6) 0.005(5) -0.005(5) C97 0.030(7) 0.027(7) 0.033(8) -0.020(6) 0.005(5) -0.005(5) C98 0.015(8) 0.021(9) 0.035(11) 0.006(7) 0.018(7) 0.005(6) C99 0.026(4) 0.016(4) 0.035(5) -0.010(3) 0.010(3) -0.001(3) C100 0.053(16) 0.18(3) 0.029(14) 0.030(15) 0.010(11) 0.066(17) C101 0.047(15) 0.10(2) 0.11(2) 0.049(17) -0.002(14) -0.028(13) C102 0.017(9) 0.020(9) 0.029(10) 0.003(7) 0.000(7) -0.006(6) C103 0.025(3) 0.018(3) 0.027(3) -0.009(2) 0.006(2) -0.005(2) C104 0.025(3) 0.018(3) 0.027(3) -0.009(2) 0.006(2) -0.005(2) C105 0.031(3) 0.026(3) 0.030(3) -0.006(2) 0.000(2) 0.006(2) C106 0.031(3) 0.026(3) 0.030(3) -0.006(2) 0.000(2) 0.006(2) C107 0.031(3) 0.026(3) 0.030(3) -0.006(2) 0.000(2) 0.006(2) C108 0.031(3) 0.026(3) 0.030(3) -0.006(2) 0.000(2) 0.006(2) C109 0.031(3) 0.026(3) 0.030(3) -0.006(2) 0.000(2) 0.006(2) C110 0.031(3) 0.026(3) 0.030(3) -0.006(2) 0.000(2) 0.006(2) C111 0.031(3) 0.026(3) 0.030(3) -0.006(2) 0.000(2) 0.006(2) C112 0.031(3) 0.026(3) 0.030(3) -0.006(2) 0.000(2) 0.006(2) C113 0.031(3) 0.026(3) 0.030(3) -0.006(2) 0.000(2) 0.006(2) C114 0.031(3) 0.026(3) 0.030(3) -0.006(2) 0.000(2) 0.006(2) C115 0.025(3) 0.018(3) 0.027(3) -0.009(2) 0.006(2) -0.005(2) C116 0.025(3) 0.018(3) 0.027(3) -0.009(2) 0.006(2) -0.005(2) C117 0.025(3) 0.018(3) 0.027(3) -0.009(2) 0.006(2) -0.005(2) C118 0.025(3) 0.018(3) 0.027(3) -0.009(2) 0.006(2) -0.005(2) C119 0.025(3) 0.018(3) 0.027(3) -0.009(2) 0.006(2) -0.005(2) C120 0.025(3) 0.018(3) 0.027(3) -0.009(2) 0.006(2) -0.005(2) C121 0.025(3) 0.018(3) 0.027(3) -0.009(2) 0.006(2) -0.005(2) C122 0.025(3) 0.018(3) 0.027(3) -0.009(2) 0.006(2) -0.005(2) C123 0.050(10) 0.010(8) 0.025(10) 0.006(7) -0.006(7) -0.003(7) C124 0.053(11) 0.034(10) 0.034(11) -0.019(8) -0.008(8) 0.014(8) C125 0.028(10) 0.026(10) 0.066(13) -0.006(9) -0.008(9) 0.005(7) C126 0.041(10) 0.014(8) 0.040(11) -0.016(8) 0.011(8) 0.000(7) C127 0.026(4) 0.016(4) 0.035(5) -0.010(3) 0.010(3) -0.001(3) C128 0.051(12) 0.040(12) 0.031(12) 0.003(9) 0.004(9) -0.012(9) C129 0.056(15) 0.16(3) 0.031(14) 0.024(15) 0.002(11) 0.042(15) C130 0.026(4) 0.016(4) 0.035(5) -0.010(3) 0.010(3) -0.001(3) C131 0.029(11) 0.019(10) 0.120(19) -0.029(11) 0.021(11) -0.018(8) C132 0.030(11) 0.084(16) 0.044(13) -0.038(12) 0.004(9) 0.005(10) C133 0.025(3) 0.018(3) 0.027(3) -0.009(2) 0.006(2) -0.005(2) C134 0.022(9) 0.070(14) 0.019(10) -0.013(9) 0.018(7) 0.001(8) C135 0.039(11) 0.042(11) 0.025(11) -0.012(9) 0.013(8) -0.010(8) C136 0.061(12) 0.022(10) 0.026(11) -0.005(8) 0.021(9) -0.018(8) N5 0.034(3) 0.028(3) 0.022(3) -0.002(2) 0.007(2) -0.010(2) N6 0.014(7) 0.019(7) 0.025(8) -0.012(6) 0.003(5) -0.007(5) N7 0.016(7) 0.020(8) 0.051(10) -0.026(7) 0.014(6) -0.006(5) N8 0.031(3) 0.026(3) 0.030(3) -0.006(2) 0.000(2) 0.006(2) O1 0.008(4) 0.022(4) 0.021(4) 0.000(3) 0.000(3) -0.004(3) O2 0.018(5) 0.025(5) 0.025(6) 0.014(4) -0.005(4) 0.003(4) O4 0.012(5) 0.026(5) 0.013(5) 0.005(4) -0.005(4) 0.005(4) O5 0.023(5) 0.009(5) 0.034(6) -0.012(4) -0.003(4) 0.000(4) O6 0.036(6) 0.016(5) 0.021(6) -0.001(4) 0.004(4) -0.009(4) O7 0.036(5) 0.015(5) 0.024(6) -0.014(4) -0.001(4) 0.009(4) O8 0.026(4) 0.016(4) 0.035(5) -0.010(3) 0.010(3) -0.001(3) Si5 0.022(2) 0.015(2) 0.021(3) -0.0076(19) 0.0090(19) -0.0055(17) Si6 0.026(3) 0.039(3) 0.038(3) -0.022(2) 0.015(2) -0.013(2) Si7 0.024(3) 0.026(3) 0.072(4) -0.032(3) 0.026(3) -0.006(2) Si8 0.021(2) 0.021(2) 0.025(3) -0.007(2) 0.0078(19) 0.0009(18) Cl3 0.019(2) 0.019(2) 0.030(2) -0.0135(18) 0.0066(17) -0.0054(15) Cl4 0.021(2) 0.022(2) 0.036(3) -0.0185(19) 0.0107(18) -0.0075(16) Y3 0.0161(8) 0.0199(9) 0.0181(9) -0.0136(7) 0.0049(6) -0.0070(6) Y4 0.0119(8) 0.0191(9) 0.0294(10) -0.0178(7) 0.0040(6) -0.0020(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.412(17) . ? C1 C13 1.436(19) . ? C1 C2 1.46(2) . ? C1 Y1 2.765(14) . ? C2 C20 1.451(19) . ? C2 C3 1.456(19) . ? C2 Y1 2.858(14) . ? C3 C4 1.39(2) . ? C3 C12 1.40(2) . ? C3 Y1 2.783(15) . ? C5 C6 1.34(2) . ? C5 C4 1.41(2) . ? C6 C7 1.45(2) . ? C7 C8 1.37(2) . ? C7 C12 1.47(2) . ? C8 C9 1.38(2) . ? C9 C10 1.38(2) . ? C10 C11 1.379(19) . ? C11 C12 1.46(2) . ? C13 C14 1.400(19) . ? C14 C15 1.44(2) . ? C15 C666 1.378(19) . ? C15 C20 1.404(19) . ? C17 C666 1.38(2) . ? C17 C18 1.429(19) . ? C18 C19 1.342(19) . ? C19 C20 1.376(19) . ? C32 C33 1.51(2) . ? C32 C31 1.51(2) . ? C35 N3 1.396(18) . ? C35 C36 1.42(2) . ? C35 C47 1.45(2) . ? C35 Y2 2.818(15) . ? C37 C38 1.39(2) . ? C37 C46 1.44(2) . ? C37 C36 1.55(2) . ? C37 Y2 2.908(15) . ? C38 N4 1.355(18) . ? C38 C39 1.48(2) . ? C38 Y2 2.760(15) . ? C39 C40 1.346(19) . ? C40 C41 1.41(2) . ? C41 C46 1.44(2) . ? C41 C42 1.452(19) . ? C42 C43 1.43(2) . ? C43 C44 1.41(2) . ? C44 C45 1.360(19) . ? C45 C46 1.42(2) . ? C47 C48 1.349(19) . ? C48 C49 1.40(2) . ? C49 C54 1.38(2) . ? C49 C50 1.45(2) . ? C50 C51 1.36(2) . ? C51 C52 1.34(2) . ? C52 C53 1.38(2) . ? C53 C54 1.38(2) . ? C54 C36 1.43(2) . ? C58 Si4 1.904(15) . ? C59 Si4 1.910(14) . ? C60 Si4 1.868(13) . ? C61 O3 1.501(16) . ? C61 C62 1.540(18) . ? C62 C63 1.52(2) . ? C63 C64 1.46(2) . ? C64 O3 1.432(16) . ? N1 Si1 1.738(13) . ? N1 Y1 2.272(13) . ? N2 C4 1.456(19) . ? N2 Si2 1.724(14) . ? N2 Y1 2.301(13) . ? N3 Si3 1.758(12) . ? N3 Y2 2.265(11) . ? N4 Si4 1.702(13) . ? N4 Y2 2.308(13) . ? O3 Y2 2.375(9) . ? Si1 C22 1.845(14) . ? Si1 C23 1.846(15) . ? Si1 C21 1.853(15) . ? Si2 C26 1.838(16) . ? Si2 C24 1.840(16) . ? Si2 C25 1.867(16) . ? Si3 C57 1.845(17) . ? Si3 C55 1.856(17) . ? Si3 C56 1.867(18) . ? Cl1 Y1 2.752(3) . ? Cl1 Y2 2.757(4) . ? Cl2 Y2 2.745(4) . ? Cl2 Y1 2.765(4) . ? Y1 O1 2.368(9) . ? Y1 O2 2.374(9) . ? Y1 C4 2.773(15) . ? Y2 O4 2.405(9) . ? Y2 C36 2.871(15) . ? C27 O1 1.478(16) . ? C27 C28 1.503(19) . ? C28 C29 1.536(14) . ? C29 C30 1.511(19) . ? C30 O1 1.446(17) . ? C31 O2 1.441(16) . ? C33 C34 1.542(18) . ? C34 O2 1.458(15) . ? C65 O4 1.468(17) . ? C65 C66 1.57(2) . ? C66 C67 1.44(2) . ? C67 C68 1.52(2) . ? C68 O4 1.465(17) . ? C69 N5 1.395(19) . ? C69 C70 1.41(2) . ? C69 C81 1.46(2) . ? C69 Y3 2.756(16) . ? C70 C88 1.44(2) . ? C70 C71 1.48(2) . ? C70 Y3 2.937(15) . ? C71 C72 1.387(19) . ? C71 C80 1.49(2) . ? C71 Y3 2.927(13) . ? C72 N6 1.385(18) . ? C72 C73 1.466(19) . ? C72 Y3 2.764(14) . ? C73 C74 1.368(19) . ? C74 C75 1.42(2) . ? C75 C80 1.340(19) . ? C75 C76 1.40(2) . ? C76 C77 1.362(19) . ? C77 C78 1.372(19) . ? C78 C79 1.393(19) . ? C79 C80 1.43(2) . ? C81 C82 1.37(2) . ? C82 C83 1.41(2) . ? C83 C84 1.43(2) . ? C83 C88 1.46(2) . ? C84 C85 1.36(2) . ? C85 C86 1.40(2) . ? C86 C87 1.40(2) . ? C87 C88 1.44(2) . ? C89 Si5 1.897(14) . ? C90 Si5 1.865(14) . ? C91 Si5 1.860(15) . ? C92 Si6 1.912(19) . ? C93 Si6 1.874(16) . ? C94 Si6 1.874(16) . ? C95 O5 1.435(16) . ? C95 C96 1.46(2) . ? C96 C97 1.55(2) . ? C97 C98 1.46(2) . ? C98 O5 1.488(15) . ? C99 O6 1.467(18) . ? C99 C100 1.48(2) . ? C100 C101 1.42(3) . ? C101 C102 1.47(2) . ? C102 O6 1.446(16) . ? C103 N7 1.394(18) . ? C103 C115 1.40(2) . ? C103 C104 1.41(2) . ? C103 Y4 2.729(14) . ? C104 C122 1.43(2) . ? C104 C105 1.52(2) . ? C104 Y4 2.869(14) . ? C105 C106 1.36(2) . ? C105 C114 1.44(2) . ? C105 Y4 2.977(16) . ? C106 N8 1.365(19) . ? C106 C107 1.47(2) . ? C106 Y4 2.832(17) . ? C107 C108 1.39(2) . ? C108 C109 1.39(2) . ? C109 C110 1.35(2) . ? C109 C114 1.45(2) . ? C110 C111 1.35(2) . ? C111 C112 1.38(2) . ? C112 C113 1.37(2) . ? C113 C114 1.42(2) . ? C115 C116 1.387(19) . ? C116 C117 1.42(2) . ? C117 C122 1.39(2) . ? C117 C118 1.39(2) . ? C118 C119 1.39(2) . ? C119 C120 1.377(19) . ? C120 C121 1.377(19) . ? C121 C122 1.42(2) . ? C123 C124 1.46(2) . ? C123 O7 1.475(17) . ? C124 C125 1.54(2) . ? C125 C126 1.48(2) . ? C126 O7 1.488(17) . ? C127 O8 1.443(17) . ? C127 C128 1.53(2) . ? C128 C129 1.55(2) . ? C129 C130 1.44(2) . ? C130 O8 1.468(17) . ? C131 Si7 1.862(18) . ? C132 Si7 1.91(2) . ? C133 Si7 1.837(14) . ? C134 Si8 1.877(16) . ? C135 Si8 1.878(16) . ? C136 Si8 1.928(16) . ? N5 Si5 1.699(13) . ? N5 Y3 2.294(13) . ? N6 Si6 1.713(13) . ? N6 Y3 2.309(12) . ? N7 Si7 1.757(12) . ? N7 Y4 2.259(11) . ? N8 Si8 1.748(13) . ? N8 Y4 2.311(13) . ? O5 Y3 2.369(10) . ? O6 Y3 2.375(10) . ? O7 Y4 2.377(10) . ? O8 Y4 2.359(11) . ? Cl3 Y4 2.761(4) . ? Cl3 Y3 2.792(4) . ? Cl4 Y3 2.718(4) . ? Cl4 Y4 2.753(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C13 121.1(13) . . ? N1 C1 C2 118.3(12) . . ? C13 C1 C2 120.3(13) . . ? N1 C1 Y1 55.0(7) . . ? C13 C1 Y1 133.4(10) . . ? C2 C1 Y1 78.5(8) . . ? C20 C2 C3 120.4(13) . . ? C20 C2 C1 118.0(12) . . ? C3 C2 C1 120.6(13) . . ? C20 C2 Y1 138.9(11) . . ? C3 C2 Y1 72.2(8) . . ? C1 C2 Y1 71.5(8) . . ? C4 C3 C12 117.9(14) . . ? C4 C3 C2 122.3(14) . . ? C12 C3 C2 118.5(14) . . ? C4 C3 Y1 75.1(9) . . ? C12 C3 Y1 130.7(11) . . ? C2 C3 Y1 77.9(8) . . ? C6 C5 C4 120.6(16) . . ? C5 C6 C7 123.0(15) . . ? C8 C7 C6 122.9(14) . . ? C8 C7 C12 123.3(15) . . ? C6 C7 C12 113.7(14) . . ? C7 C8 C9 119.5(15) . . ? C8 C9 C10 120.3(15) . . ? C11 C10 C9 122.6(15) . . ? C10 C11 C12 120.0(14) . . ? C3 C12 C11 122.5(14) . . ? C3 C12 C7 123.0(15) . . ? C11 C12 C7 114.2(14) . . ? C14 C13 C1 120.3(13) . . ? C13 C14 C15 120.2(12) . . ? C666 C15 C20 118.4(13) . . ? C666 C15 C14 120.8(12) . . ? C20 C15 C14 120.7(13) . . ? C666 C17 C18 116.5(14) . . ? C19 C18 C17 120.0(14) . . ? C18 C19 C20 123.0(13) . . ? C19 C20 C15 118.6(13) . . ? C19 C20 C2 120.7(12) . . ? C15 C20 C2 120.5(13) . . ? C33 C32 C31 104.0(13) . . ? N3 C35 C36 119.7(14) . . ? N3 C35 C47 125.0(15) . . ? C36 C35 C47 113.5(14) . . ? N3 C35 Y2 52.7(7) . . ? C36 C35 Y2 77.7(9) . . ? C47 C35 Y2 133.1(10) . . ? C38 C37 C46 123.3(15) . . ? C38 C37 C36 118.3(13) . . ? C46 C37 C36 117.3(13) . . ? C38 C37 Y2 69.9(9) . . ? C46 C37 Y2 138.5(10) . . ? C36 C37 Y2 73.1(8) . . ? N4 C38 C37 123.0(15) . . ? N4 C38 C39 121.6(14) . . ? C37 C38 C39 115.4(13) . . ? N4 C38 Y2 56.5(8) . . ? C37 C38 Y2 81.8(9) . . ? C39 C38 Y2 136.0(9) . . ? C40 C39 C38 121.7(15) . . ? C39 C40 C41 123.1(16) . . ? C40 C41 C46 117.9(13) . . ? C40 C41 C42 123.6(15) . . ? C46 C41 C42 118.5(14) . . ? C43 C42 C41 121.1(15) . . ? C44 C43 C42 117.0(14) . . ? C45 C44 C43 123.2(15) . . ? C44 C45 C46 121.7(16) . . ? C45 C46 C37 123.0(15) . . ? C45 C46 C41 118.4(13) . . ? C37 C46 C41 118.6(14) . . ? C48 C47 C35 122.6(16) . . ? C47 C48 C49 122.2(16) . . ? C54 C49 C48 119.1(15) . . ? C54 C49 C50 120.7(16) . . ? C48 C49 C50 120.2(15) . . ? C51 C50 C49 117.7(16) . . ? C52 C51 C50 121.5(16) . . ? C51 C52 C53 120.6(17) . . ? C54 C53 C52 121.5(16) . . ? C49 C54 C53 117.6(15) . . ? C49 C54 C36 119.1(16) . . ? C53 C54 C36 123.2(15) . . ? O3 C61 C62 103.3(11) . . ? C63 C62 C61 105.6(12) . . ? C64 C63 C62 104.1(14) . . ? O3 C64 C63 107.8(13) . . ? C15 C666 C17 123.3(13) . . ? C1 N1 Si1 119.7(10) . . ? C1 N1 Y1 94.4(9) . . ? Si1 N1 Y1 142.2(7) . . ? C4 N2 Si2 120.5(10) . . ? C4 N2 Y1 92.3(9) . . ? Si2 N2 Y1 139.8(7) . . ? C35 N3 Si3 118.8(10) . . ? C35 N3 Y2 97.9(8) . . ? Si3 N3 Y2 138.2(6) . . ? C38 N4 Si4 123.6(12) . . ? C38 N4 Y2 94.2(9) . . ? Si4 N4 Y2 137.4(7) . . ? C64 O3 C61 110.1(11) . . ? C64 O3 Y2 124.0(9) . . ? C61 O3 Y2 122.8(7) . . ? N1 Si1 C22 114.8(7) . . ? N1 Si1 C23 112.0(7) . . ? C22 Si1 C23 106.1(7) . . ? N1 Si1 C21 108.5(6) . . ? C22 Si1 C21 106.6(7) . . ? C23 Si1 C21 108.5(7) . . ? N2 Si2 C26 109.3(7) . . ? N2 Si2 C24 110.1(6) . . ? C26 Si2 C24 108.7(7) . . ? N2 Si2 C25 116.5(7) . . ? C26 Si2 C25 106.5(7) . . ? C24 Si2 C25 105.5(7) . . ? N3 Si3 C57 107.5(7) . . ? N3 Si3 C55 111.8(8) . . ? C57 Si3 C55 105.7(8) . . ? N3 Si3 C56 114.5(7) . . ? C57 Si3 C56 107.8(8) . . ? C55 Si3 C56 108.9(9) . . ? N4 Si4 C60 108.4(6) . . ? N4 Si4 C58 108.2(6) . . ? C60 Si4 C58 110.9(6) . . ? N4 Si4 C59 116.3(6) . . ? C60 Si4 C59 108.9(6) . . ? C58 Si4 C59 104.2(7) . . ? Y1 Cl1 Y2 107.82(12) . . ? Y2 Cl2 Y1 107.80(12) . . ? N1 Y1 N2 121.7(4) . . ? N1 Y1 O1 96.5(4) . . ? N2 Y1 O1 92.8(4) . . ? N1 Y1 O2 88.9(4) . . ? N2 Y1 O2 95.4(4) . . ? O1 Y1 O2 166.0(3) . . ? N1 Y1 Cl1 83.4(3) . . ? N2 Y1 Cl1 154.8(3) . . ? O1 Y1 Cl1 83.7(2) . . ? O2 Y1 Cl1 84.1(2) . . ? N1 Y1 Cl2 155.1(3) . . ? N2 Y1 Cl2 82.8(3) . . ? O1 Y1 Cl2 85.5(2) . . ? O2 Y1 Cl2 84.3(3) . . ? Cl1 Y1 Cl2 72.07(10) . . ? N1 Y1 C1 30.6(4) . . ? N2 Y1 C1 95.9(4) . . ? O1 Y1 C1 116.4(4) . . ? O2 Y1 C1 74.1(4) . . ? Cl1 Y1 C1 108.0(3) . . ? Cl2 Y1 C1 158.2(3) . . ? N1 Y1 C4 97.6(4) . . ? N2 Y1 C4 31.6(4) . . ? O1 Y1 C4 74.7(4) . . ? O2 Y1 C4 117.5(4) . . ? Cl1 Y1 C4 158.3(3) . . ? Cl2 Y1 C4 106.8(3) . . ? C1 Y1 C4 81.2(4) . . ? N1 Y1 C3 68.9(4) . . ? N2 Y1 C3 55.9(5) . . ? O1 Y1 C3 81.7(4) . . ? O2 Y1 C3 112.3(4) . . ? Cl1 Y1 C3 146.8(3) . . ? Cl2 Y1 C3 135.7(3) . . ? C1 Y1 C3 54.3(4) . . ? C4 Y1 C3 28.9(4) . . ? N1 Y1 C2 56.0(4) . . ? N2 Y1 C2 66.7(4) . . ? O1 Y1 C2 109.5(4) . . ? O2 Y1 C2 84.3(4) . . ? Cl1 Y1 C2 137.9(3) . . ? Cl2 Y1 C2 146.1(3) . . ? C1 Y1 C2 30.0(4) . . ? C4 Y1 C2 52.5(4) . . ? C3 Y1 C2 29.9(4) . . ? N3 Y2 N4 120.2(4) . . ? N3 Y2 O3 92.0(4) . . ? N4 Y2 O3 91.6(4) . . ? N3 Y2 O4 91.7(4) . . ? N4 Y2 O4 94.0(4) . . ? O3 Y2 O4 170.6(3) . . ? N3 Y2 Cl2 85.0(3) . . ? N4 Y2 Cl2 154.9(3) . . ? O3 Y2 Cl2 87.8(2) . . ? O4 Y2 Cl2 83.9(2) . . ? N3 Y2 Cl1 157.0(3) . . ? N4 Y2 Cl1 82.6(3) . . ? O3 Y2 Cl1 83.6(2) . . ? O4 Y2 Cl1 89.7(2) . . ? Cl2 Y2 Cl1 72.30(10) . . ? N3 Y2 C38 96.8(4) . . ? N4 Y2 C38 29.3(4) . . ? O3 Y2 C38 74.0(4) . . ? O4 Y2 C38 114.1(4) . . ? Cl2 Y2 C38 161.7(3) . . ? Cl1 Y2 C38 103.6(3) . . ? N3 Y2 C35 29.4(4) . . ? N4 Y2 C35 95.6(5) . . ? O3 Y2 C35 110.1(4) . . ? O4 Y2 C35 76.9(4) . . ? Cl2 Y2 C35 108.2(4) . . ? Cl1 Y2 C35 166.3(3) . . ? C38 Y2 C35 80.1(5) . . ? N3 Y2 C36 55.0(4) . . ? N4 Y2 C36 67.0(4) . . ? O3 Y2 C36 106.7(4) . . ? O4 Y2 C36 82.4(4) . . ? Cl2 Y2 C36 137.0(3) . . ? Cl1 Y2 C36 147.8(3) . . ? C38 Y2 C36 53.3(5) . . ? C35 Y2 C36 28.8(4) . . ? N3 Y2 C37 68.7(4) . . ? N4 Y2 C37 53.7(4) . . ? O3 Y2 C37 78.9(4) . . ? O4 Y2 C37 110.5(4) . . ? Cl2 Y2 C37 149.8(3) . . ? Cl1 Y2 C37 131.8(3) . . ? C38 Y2 C37 28.3(4) . . ? C35 Y2 C37 53.5(5) . . ? C36 Y2 C37 31.1(4) . . ? C3 C4 C5 121.5(15) . . ? C3 C4 N2 116.6(14) . . ? C5 C4 N2 121.4(14) . . ? C3 C4 Y1 75.9(9) . . ? C5 C4 Y1 133.3(10) . . ? N2 C4 Y1 56.0(7) . . ? O1 C27 C28 104.9(11) . . ? C27 C28 C29 102.9(11) . . ? C30 C29 C28 101.8(11) . . ? O1 C30 C29 104.3(12) . . ? O2 C31 C32 106.0(11) . . ? C32 C33 C34 104.1(12) . . ? O2 C34 C33 104.6(11) . . ? C35 C36 C54 123.3(15) . . ? C35 C36 C37 120.7(13) . . ? C54 C36 C37 113.3(14) . . ? C35 C36 Y2 73.5(8) . . ? C54 C36 Y2 139.0(10) . . ? C37 C36 Y2 75.8(8) . . ? O4 C65 C66 100.6(11) . . ? C67 C66 C65 104.1(13) . . ? C66 C67 C68 102.3(13) . . ? O4 C68 C67 105.1(12) . . ? N5 C69 C70 119.8(14) . . ? N5 C69 C81 120.0(13) . . ? C70 C69 C81 120.1(14) . . ? N5 C69 Y3 56.2(8) . . ? C70 C69 Y3 83.0(9) . . ? C81 C69 Y3 135.2(10) . . ? C69 C70 C88 118.7(14) . . ? C69 C70 C71 125.2(14) . . ? C88 C70 C71 116.0(13) . . ? C69 C70 Y3 68.6(9) . . ? C88 C70 Y3 135.2(10) . . ? C71 C70 Y3 75.0(8) . . ? C72 C71 C70 123.1(14) . . ? C72 C71 C80 120.4(13) . . ? C70 C71 C80 116.3(12) . . ? C72 C71 Y3 69.4(8) . . ? C70 C71 Y3 75.8(8) . . ? C80 C71 Y3 133.7(10) . . ? N6 C72 C71 121.2(13) . . ? N6 C72 C73 122.7(13) . . ? C71 C72 C73 116.0(13) . . ? N6 C72 Y3 56.5(7) . . ? C71 C72 Y3 82.5(9) . . ? C73 C72 Y3 131.0(10) . . ? C74 C73 C72 121.1(14) . . ? C73 C74 C75 122.1(14) . . ? C80 C75 C76 122.3(14) . . ? C80 C75 C74 118.2(14) . . ? C76 C75 C74 119.3(13) . . ? C77 C76 C75 118.9(14) . . ? C76 C77 C78 119.7(14) . . ? C77 C78 C79 122.7(14) . . ? C78 C79 C80 116.6(14) . . ? C75 C80 C79 119.6(14) . . ? C75 C80 C71 121.3(13) . . ? C79 C80 C71 119.1(13) . . ? C82 C81 C69 119.4(14) . . ? C81 C82 C83 123.3(15) . . ? C82 C83 C84 121.8(15) . . ? C82 C83 C88 117.6(14) . . ? C84 C83 C88 120.2(14) . . ? C85 C84 C83 120.2(15) . . ? C84 C85 C86 121.2(15) . . ? C85 C86 C87 121.4(15) . . ? C86 C87 C88 120.1(15) . . ? C87 C88 C70 122.5(14) . . ? C87 C88 C83 116.9(14) . . ? C70 C88 C83 120.4(13) . . ? O5 C95 C96 106.2(11) . . ? C95 C96 C97 102.3(13) . . ? C98 C97 C96 102.8(13) . . ? C97 C98 O5 109.1(11) . . ? O6 C99 C100 105.9(14) . . ? C101 C100 C99 109.6(19) . . ? C100 C101 C102 106.1(17) . . ? O6 C102 C101 108.2(14) . . ? N7 C103 C115 122.1(13) . . ? N7 C103 C104 117.0(14) . . ? C115 C103 C104 120.7(13) . . ? N7 C103 Y4 55.7(7) . . ? C115 C103 Y4 137.9(11) . . ? C104 C103 Y4 81.0(9) . . ? C103 C104 C122 117.7(14) . . ? C103 C104 C105 125.6(13) . . ? C122 C104 C105 115.8(13) . . ? C103 C104 Y4 70.0(8) . . ? C122 C104 Y4 136.0(10) . . ? C105 C104 Y4 78.9(8) . . ? C106 C105 C114 121.0(15) . . ? C106 C105 C104 123.7(14) . . ? C114 C105 C104 115.1(13) . . ? C106 C105 Y4 70.6(10) . . ? C114 C105 Y4 137.9(11) . . ? C104 C105 Y4 71.1(8) . . ? C105 C106 N8 122.4(16) . . ? C105 C106 C107 117.3(15) . . ? N8 C106 C107 120.3(14) . . ? C105 C106 Y4 82.5(10) . . ? N8 C106 Y4 54.0(8) . . ? C107 C106 Y4 137.3(10) . . ? C108 C107 C106 122.7(15) . . ? C107 C108 C109 119.7(16) . . ? C110 C109 C108 122.2(16) . . ? C110 C109 C114 119.2(15) . . ? C108 C109 C114 118.6(14) . . ? C111 C110 C109 122.9(17) . . ? C110 C111 C112 119.7(15) . . ? C113 C112 C111 121.0(15) . . ? C112 C113 C114 120.3(16) . . ? C113 C114 C105 123.1(15) . . ? C113 C114 C109 116.8(14) . . ? C105 C114 C109 120.1(14) . . ? C116 C115 C103 119.4(14) . . ? C115 C116 C117 121.9(14) . . ? C122 C117 C118 122.6(14) . . ? C122 C117 C116 117.2(13) . . ? C118 C117 C116 119.9(14) . . ? C119 C118 C117 119.5(15) . . ? C120 C119 C118 119.2(14) . . ? C119 C120 C121 121.1(14) . . ? C120 C121 C122 121.2(15) . . ? C117 C122 C121 116.1(13) . . ? C117 C122 C104 122.2(14) . . ? C121 C122 C104 121.6(14) . . ? C124 C123 O7 107.0(12) . . ? C123 C124 C125 106.1(14) . . ? C126 C125 C124 101.2(13) . . ? C125 C126 O7 103.3(12) . . ? O8 C127 C128 109.7(12) . . ? C127 C128 C129 101.3(14) . . ? C130 C129 C128 105.7(15) . . ? C129 C130 O8 109.3(14) . . ? C69 N5 Si5 124.0(11) . . ? C69 N5 Y3 93.5(9) . . ? Si5 N5 Y3 138.6(7) . . ? C72 N6 Si6 121.4(10) . . ? C72 N6 Y3 93.5(9) . . ? Si6 N6 Y3 136.6(6) . . ? C103 N7 Si7 124.7(10) . . ? C103 N7 Y4 93.7(8) . . ? Si7 N7 Y4 136.9(6) . . ? C106 N8 Si8 123.4(12) . . ? C106 N8 Y4 97.5(10) . . ? Si8 N8 Y4 135.8(7) . . ? C30 O1 C27 109.9(10) . . ? C30 O1 Y1 123.3(8) . . ? C27 O1 Y1 126.3(8) . . ? C31 O2 C34 111.1(10) . . ? C31 O2 Y1 124.2(8) . . ? C34 O2 Y1 121.9(7) . . ? C68 O4 C65 110.2(10) . . ? C68 O4 Y2 123.7(8) . . ? C65 O4 Y2 123.0(8) . . ? C95 O5 C98 104.6(10) . . ? C95 O5 Y3 124.4(8) . . ? C98 O5 Y3 130.6(8) . . ? C102 O6 C99 107.6(11) . . ? C102 O6 Y3 126.4(8) . . ? C99 O6 Y3 123.5(9) . . ? C123 O7 C126 104.7(11) . . ? C123 O7 Y4 125.6(8) . . ? C126 O7 Y4 123.1(8) . . ? C127 O8 C130 106.7(11) . . ? C127 O8 Y4 125.3(8) . . ? C130 O8 Y4 124.9(8) . . ? N5 Si5 C91 110.4(7) . . ? N5 Si5 C90 115.1(7) . . ? C91 Si5 C90 105.1(7) . . ? N5 Si5 C89 109.2(6) . . ? C91 Si5 C89 109.8(7) . . ? C90 Si5 C89 107.0(6) . . ? N6 Si6 C94 118.2(7) . . ? N6 Si6 C93 108.4(7) . . ? C94 Si6 C93 106.6(8) . . ? N6 Si6 C92 107.4(7) . . ? C94 Si6 C92 110.1(9) . . ? C93 Si6 C92 105.5(9) . . ? N7 Si7 C133 109.1(6) . . ? N7 Si7 C131 110.6(7) . . ? C133 Si7 C131 107.9(7) . . ? N7 Si7 C132 114.7(7) . . ? C133 Si7 C132 109.2(8) . . ? C131 Si7 C132 105.1(8) . . ? N8 Si8 C134 108.9(7) . . ? N8 Si8 C135 113.6(7) . . ? C134 Si8 C135 110.3(7) . . ? N8 Si8 C136 111.2(7) . . ? C134 Si8 C136 106.4(7) . . ? C135 Si8 C136 106.1(7) . . ? Y4 Cl3 Y3 106.64(13) . . ? Y3 Cl4 Y4 108.96(13) . . ? N5 Y3 N6 118.8(4) . . ? N5 Y3 O5 93.7(4) . . ? N6 Y3 O5 92.4(4) . . ? N5 Y3 O6 90.7(4) . . ? N6 Y3 O6 94.6(4) . . ? O5 Y3 O6 168.7(3) . . ? N5 Y3 Cl4 157.4(3) . . ? N6 Y3 Cl4 83.8(3) . . ? O5 Y3 Cl4 84.9(2) . . ? O6 Y3 Cl4 87.1(3) . . ? N5 Y3 C69 30.4(4) . . ? N6 Y3 C69 94.1(4) . . ? O5 Y3 C69 113.8(4) . . ? O6 Y3 C69 74.6(4) . . ? Cl4 Y3 C69 161.3(3) . . ? N5 Y3 C72 95.5(4) . . ? N6 Y3 C72 30.0(4) . . ? O5 Y3 C72 74.5(4) . . ? O6 Y3 C72 115.4(4) . . ? Cl4 Y3 C72 105.8(3) . . ? C69 Y3 C72 79.8(4) . . ? N5 Y3 Cl3 85.2(3) . . ? N6 Y3 Cl3 156.0(3) . . ? O5 Y3 Cl3 86.5(3) . . ? O6 Y3 Cl3 83.5(3) . . ? Cl4 Y3 Cl3 72.20(11) . . ? C69 Y3 Cl3 108.3(3) . . ? C72 Y3 Cl3 161.0(3) . . ? N5 Y3 C71 67.8(4) . . ? N6 Y3 C71 53.3(4) . . ? O5 Y3 C71 81.0(4) . . ? O6 Y3 C71 110.3(4) . . ? Cl4 Y3 C71 133.8(3) . . ? C69 Y3 C71 53.5(4) . . ? C72 Y3 C71 28.0(4) . . ? Cl3 Y3 C71 149.1(3) . . ? N5 Y3 C70 53.5(4) . . ? N6 Y3 C70 66.5(4) . . ? O5 Y3 C70 106.8(4) . . ? O6 Y3 C70 84.2(4) . . ? Cl4 Y3 C70 148.2(3) . . ? C69 Y3 C70 28.4(4) . . ? C72 Y3 C70 52.4(4) . . ? Cl3 Y3 C70 136.5(3) . . ? C71 Y3 C70 29.2(4) . . ? N7 Y4 N8 118.2(4) . . ? N7 Y4 O8 93.8(4) . . ? N8 Y4 O8 98.6(4) . . ? N7 Y4 O7 90.2(4) . . ? N8 Y4 O7 87.4(4) . . ? O8 Y4 O7 170.1(3) . . ? N7 Y4 C103 30.6(4) . . ? N8 Y4 C103 97.3(4) . . ? O8 Y4 C103 74.5(4) . . ? O7 Y4 C103 112.7(4) . . ? N7 Y4 Cl4 82.0(3) . . ? N8 Y4 Cl4 159.6(3) . . ? O8 Y4 Cl4 81.3(3) . . ? O7 Y4 Cl4 90.4(3) . . ? C103 Y4 Cl4 102.2(3) . . ? N7 Y4 Cl3 153.5(3) . . ? N8 Y4 Cl3 87.5(3) . . ? O8 Y4 Cl3 88.2(2) . . ? O7 Y4 Cl3 84.2(2) . . ? C103 Y4 Cl3 162.6(3) . . ? Cl4 Y4 Cl3 72.17(11) . . ? N7 Y4 C106 92.8(5) . . ? N8 Y4 C106 28.6(4) . . ? O8 Y4 C106 115.2(4) . . ? O7 Y4 C106 73.5(4) . . ? C103 Y4 C106 80.1(5) . . ? Cl4 Y4 C106 163.1(3) . . ? Cl3 Y4 C106 110.2(3) . . ? N7 Y4 C104 54.0(4) . . ? N8 Y4 C104 68.3(4) . . ? O8 Y4 C104 81.9(4) . . ? O7 Y4 C104 107.7(4) . . ? C103 Y4 C104 29.0(4) . . ? Cl4 Y4 C104 131.3(3) . . ? Cl3 Y4 C104 151.9(3) . . ? C106 Y4 C104 52.8(4) . . ? N7 Y4 C105 66.8(4) . . ? N8 Y4 C105 51.9(4) . . ? O8 Y4 C105 108.5(4) . . ? O7 Y4 C105 81.4(4) . . ? C103 Y4 C105 54.1(5) . . ? Cl4 Y4 C105 147.5(3) . . ? Cl3 Y4 C105 137.1(3) . . ? C106 Y4 C105 26.9(4) . . ? C104 Y4 C105 30.0(4) . . ? _diffrn_measured_fraction_theta_max 0.888 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 2.299 _refine_diff_density_min -1.089 _refine_diff_density_rms 0.177 # Attachment '3c.cif' data_683GuillotICMMO _database_code_depnum_ccdc_archive 'CCDC 870819' #TrackingRef '3c.cif'_database_code_CSD 'CCDC 870819' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H58 Li2 N2 O2 Si2' _chemical_formula_sum 'C40 H58 Li2 N2 O2 Si2' _chemical_formula_weight 668.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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' Si Si 0.0826 0.0707 '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' O O 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li 0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 31' _symmetry_int_tables_number 144 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 11.4765(2) _cell_length_b 11.4765(2) _cell_length_c 26.9628(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3075.49(11) _cell_formula_units_Z 3 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 7452 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 38.90 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.310 _exptl_crystal_size_min 0.300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1086 _exptl_absorpt_coefficient_mu 0.119 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.968 _exptl_absorpt_correction_T_max 0.974 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'kappa X8 APEX II Bruker ICMMO' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70534 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 44.20 _reflns_number_total 29744 _reflns_number_gt 21428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'Ortep-3 for Windows (L. J. Farrugia, J. Appl. Cryst (1997), 30, 565)' ; _computing_publication_material ; 'WINGX (Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838)' ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+0.1529P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _chemical_absolute_configuration ad _refine_ls_number_reflns 29744 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1235 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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 Si2 Si 0.98256(2) 0.63219(2) 0.884023(9) 0.01403(4) Uani 1 1 d . . . Si1 Si 0.75601(2) 0.10055(2) 0.805597(9) 0.01513(4) Uani 1 1 d . . . N1 N 0.89195(7) 0.21430(7) 0.83915(3) 0.01461(11) Uani 1 1 d . . . C2 C 1.11449(8) 0.31545(8) 0.87572(3) 0.01296(11) Uani 1 1 d . . . C1 C 1.02132(8) 0.23573(8) 0.83875(3) 0.01401(12) Uani 1 1 d . . . C4 C 1.03368(8) 0.44461(8) 0.92927(3) 0.01352(11) Uani 1 1 d . . . C20 C 1.25504(8) 0.36049(9) 0.86925(3) 0.01503(12) Uani 1 1 d . . . C12 C 1.08647(8) 0.28137(8) 0.96754(3) 0.01444(12) Uani 1 1 d . . . C3 C 1.07328(8) 0.34686(8) 0.92434(3) 0.01276(11) Uani 1 1 d . . . C15 C 1.30002(9) 0.31507(10) 0.82841(4) 0.01831(14) Uani 1 1 d . . . C7 C 1.06846(9) 0.31994(9) 1.01586(3) 0.01777(14) Uani 1 1 d . . . C19 C 1.35445(9) 0.45429(9) 0.90218(4) 0.01923(15) Uani 1 1 d . . . H19 H 1.3279 0.4844 0.9296 0.023 Uiso 1 1 calc R . . C13 C 1.07046(9) 0.18776(10) 0.79903(3) 0.01899(14) Uani 1 1 d . . . H13 H 1.0095 0.1301 0.7756 0.023 Uiso 1 1 calc R . . C11 C 1.11616(10) 0.17520(9) 0.96413(4) 0.01975(15) Uani 1 1 d . . . H11 H 1.1294 0.1483 0.9331 0.024 Uiso 1 1 calc R . . C18 C 1.48938(10) 0.50146(11) 0.89429(5) 0.02507(18) Uani 1 1 d . . . H18 H 1.5525 0.5639 0.9161 0.030 Uiso 1 1 calc R . . C14 C 1.20244(10) 0.22330(10) 0.79443(4) 0.02127(16) Uani 1 1 d . . . H14 H 1.2289 0.1873 0.7689 0.026 Uiso 1 1 calc R . . C5 C 1.01898(10) 0.48203(10) 0.97897(3) 0.01916(14) Uani 1 1 d . . . H5 H 0.9956 0.5482 0.9831 0.023 Uiso 1 1 calc R . . C16 C 1.43896(10) 0.36324(12) 0.82169(4) 0.02504(18) Uani 1 1 d . . . H16 H 1.4674 0.3315 0.7953 0.030 Uiso 1 1 calc R . . C6 C 1.03781(11) 0.42471(11) 1.02011(4) 0.02122(16) Uani 1 1 d . . . H6 H 1.0305 0.4547 1.0514 0.025 Uiso 1 1 calc R . . C8 C 1.07964(12) 0.25287(11) 1.05815(4) 0.02453(18) Uani 1 1 d . . . H8 H 1.0679 0.2789 1.0896 0.029 Uiso 1 1 calc R . . C17 C 1.53253(10) 0.45609(12) 0.85359(5) 0.0283(2) Uani 1 1 d . . . H17 H 1.6238 0.4888 0.8483 0.034 Uiso 1 1 calc R . . C10 C 1.12566(12) 0.11165(11) 1.00594(4) 0.02640(19) Uani 1 1 d . . . H10 H 1.1444 0.0420 1.0027 0.032 Uiso 1 1 calc R . . C9 C 1.10741(13) 0.15046(11) 1.05350(4) 0.0288(2) Uani 1 1 d . . . H9 H 1.1142 0.1069 1.0815 0.035 Uiso 1 1 calc R . . O2 O 0.69314(8) 0.22789(8) 0.94076(3) 0.02374(13) Uani 1 1 d . . . C28 C 0.57078(13) 0.23325(15) 0.94027(6) 0.0342(2) Uani 1 1 d . . . H28A H 0.4950 0.1466 0.9312 0.041 Uiso 1 1 calc R . . H28B H 0.5771 0.3003 0.9168 0.041 Uiso 1 1 calc R . . C25 C 0.69370(15) 0.16603(16) 0.98693(5) 0.0375(3) Uani 1 1 d . . . H25A H 0.7848 0.1915 0.9966 0.045 Uiso 1 1 calc R . . H25B H 0.6411 0.0688 0.9844 0.045 Uiso 1 1 calc R . . C26 C 0.6313(3) 0.2179(3) 1.02406(7) 0.0691(7) Uani 1 1 d . . . H26A H 0.7002 0.2899 1.0439 0.083 Uiso 1 1 calc R . . H26B H 0.5699 0.1463 1.0460 0.083 Uiso 1 1 calc R . . C27 C 0.5548(3) 0.2705(3) 0.99209(8) 0.0622(6) Uani 1 1 d . . . H27B H 0.4606 0.2272 1.0014 0.075 Uiso 1 1 calc R . . H27A H 0.5944 0.3671 0.9955 0.075 Uiso 1 1 calc R . . N2 N 1.00169(7) 0.49393(7) 0.88821(3) 0.01452(11) Uani 1 1 d . . . C31 C 1.14663(9) 0.79790(9) 0.89261(4) 0.02100(16) Uani 1 1 d . . . C37 C 0.68142(9) -0.07719(9) 0.83092(4) 0.01979(15) Uani 1 1 d . . . C29 C 0.92079(10) 0.62464(10) 0.81883(4) 0.02046(15) Uani 1 1 d . . . H29C H 0.8477 0.5357 0.8121 0.031 Uiso 1 1 calc R . . H29B H 0.9928 0.6460 0.7959 0.031 Uiso 1 1 calc R . . H29A H 0.8903 0.6883 0.8152 0.031 Uiso 1 1 calc R . . C30 C 0.85289(10) 0.63519(11) 0.92653(4) 0.02119(16) Uani 1 1 d . . . H30C H 0.8911 0.6649 0.9589 0.032 Uiso 1 1 calc R . . H30B H 0.7760 0.5464 0.9288 0.032 Uiso 1 1 calc R . . H30A H 0.8258 0.6958 0.9134 0.032 Uiso 1 1 calc R . . C36 C 0.62860(11) 0.15723(12) 0.81185(4) 0.02520(19) Uani 1 1 d . . . H36A H 0.6652 0.2464 0.7986 0.038 Uiso 1 1 calc R . . H36B H 0.6071 0.1575 0.8462 0.038 Uiso 1 1 calc R . . H36C H 0.5485 0.0967 0.7939 0.038 Uiso 1 1 calc R . . C32 C 1.25469(11) 0.80161(12) 0.85801(6) 0.0311(2) Uani 1 1 d . . . H32C H 1.2688 0.7279 0.8657 0.047 Uiso 1 1 calc R . . H32B H 1.3373 0.8850 0.8625 0.047 Uiso 1 1 calc R . . H32A H 1.2256 0.7943 0.8242 0.047 Uiso 1 1 calc R . . C39 C 0.55584(11) -0.17508(12) 0.80128(5) 0.0293(2) Uani 1 1 d . . . H39C H 0.5129 -0.2615 0.8171 0.044 Uiso 1 1 calc R . . H39A H 0.5817 -0.1836 0.7682 0.044 Uiso 1 1 calc R . . H39B H 0.4945 -0.1412 0.8000 0.044 Uiso 1 1 calc R . . C35 C 0.77864(13) 0.09236(14) 0.73654(4) 0.0305(2) Uani 1 1 d . . . H35C H 0.8201 0.0390 0.7301 0.046 Uiso 1 1 calc R . . H35A H 0.8349 0.1816 0.7239 0.046 Uiso 1 1 calc R . . H35B H 0.6925 0.0523 0.7205 0.046 Uiso 1 1 calc R . . C34 C 1.12523(12) 0.91589(10) 0.87932(5) 0.0286(2) Uani 1 1 d . . . H34A H 1.2078 0.9991 0.8841 0.043 Uiso 1 1 calc R . . H34B H 1.0567 0.9140 0.9003 0.043 Uiso 1 1 calc R . . H34C H 1.0978 0.9083 0.8453 0.043 Uiso 1 1 calc R . . C33 C 1.19885(13) 0.81572(13) 0.94614(6) 0.0345(3) Uani 1 1 d . . . H33C H 1.1320 0.8122 0.9685 0.052 Uiso 1 1 calc R . . H33B H 1.2799 0.9011 0.9493 0.052 Uiso 1 1 calc R . . H33A H 1.2172 0.7449 0.9541 0.052 Uiso 1 1 calc R . . C38 C 0.78358(12) -0.12564(12) 0.82734(7) 0.0367(3) Uani 1 1 d . . . H38C H 0.7444 -0.2154 0.8403 0.055 Uiso 1 1 calc R . . H38A H 0.8623 -0.0668 0.8462 0.055 Uiso 1 1 calc R . . H38B H 0.8081 -0.1251 0.7933 0.055 Uiso 1 1 calc R . . C40 C 0.64263(14) -0.08018(13) 0.88545(5) 0.0314(2) Uani 1 1 d . . . H40A H 0.7222 -0.0263 0.9047 0.047 Uiso 1 1 calc R . . H40C H 0.5987 -0.1712 0.8973 0.047 Uiso 1 1 calc R . . H40B H 0.5827 -0.0449 0.8885 0.047 Uiso 1 1 calc R . . O1 O 1.10556(7) 0.49874(8) 0.76159(3) 0.02317(13) Uani 1 1 d . . . C21 C 1.25002(12) 0.56557(14) 0.76119(5) 0.0319(2) Uani 1 1 d . . . H21A H 1.2828 0.5398 0.7899 0.038 Uiso 1 1 calc R . . H21B H 1.2882 0.6624 0.7615 0.038 Uiso 1 1 calc R . . C24 C 1.06572(16) 0.49282(18) 0.71093(5) 0.0402(3) Uani 1 1 d . . . H24B H 1.0743 0.5777 0.7006 0.048 Uiso 1 1 calc R . . H24A H 0.9733 0.4219 0.7061 0.048 Uiso 1 1 calc R . . C22 C 1.2877(2) 0.5214(2) 0.71405(7) 0.0516(4) Uani 1 1 d . . . H22A H 1.3125 0.4536 0.7209 0.062 Uiso 1 1 calc R . . H22B H 1.3622 0.5971 0.6976 0.062 Uiso 1 1 calc R . . C23 C 1.1610(3) 0.4637(3) 0.68252(7) 0.0760(8) Uani 1 1 d . . . H23B H 1.1805 0.5066 0.6502 0.091 Uiso 1 1 calc R . . H23A H 1.1230 0.3676 0.6780 0.091 Uiso 1 1 calc R . . Li2 Li 0.84072(18) 0.29358(18) 0.89385(7) 0.0201(3) Uani 1 1 d . . . Li1 Li 1.01151(18) 0.42249(18) 0.82266(7) 0.0201(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si2 0.01295(9) 0.01419(9) 0.01727(9) 0.00018(7) 0.00036(7) 0.00852(8) Si1 0.01369(9) 0.01656(10) 0.01552(9) -0.00286(8) -0.00355(7) 0.00785(8) N1 0.0117(2) 0.0151(3) 0.0163(3) -0.0024(2) -0.0015(2) 0.0062(2) C2 0.0121(3) 0.0135(3) 0.0145(3) -0.0012(2) -0.0001(2) 0.0073(2) C1 0.0132(3) 0.0145(3) 0.0146(3) -0.0018(2) 0.0006(2) 0.0071(2) C4 0.0140(3) 0.0140(3) 0.0136(3) -0.0012(2) -0.0003(2) 0.0078(2) C20 0.0127(3) 0.0157(3) 0.0182(3) -0.0006(2) 0.0005(2) 0.0083(2) C12 0.0148(3) 0.0132(3) 0.0151(3) 0.0004(2) -0.0016(2) 0.0068(2) C3 0.0130(3) 0.0132(3) 0.0130(3) -0.0008(2) -0.0005(2) 0.0072(2) C15 0.0157(3) 0.0203(4) 0.0219(4) 0.0002(3) 0.0034(3) 0.0112(3) C7 0.0204(4) 0.0186(3) 0.0142(3) 0.0000(3) -0.0020(3) 0.0097(3) C19 0.0129(3) 0.0192(4) 0.0251(4) -0.0025(3) -0.0013(3) 0.0076(3) C13 0.0179(3) 0.0212(4) 0.0183(3) -0.0058(3) -0.0001(3) 0.0101(3) C11 0.0238(4) 0.0164(3) 0.0218(4) 0.0014(3) -0.0023(3) 0.0121(3) C18 0.0122(3) 0.0241(4) 0.0361(5) -0.0014(4) -0.0015(3) 0.0069(3) C14 0.0207(4) 0.0244(4) 0.0217(4) -0.0044(3) 0.0035(3) 0.0135(3) C5 0.0263(4) 0.0222(4) 0.0149(3) -0.0027(3) -0.0003(3) 0.0166(3) C16 0.0183(4) 0.0315(5) 0.0292(5) 0.0012(4) 0.0072(3) 0.0153(4) C6 0.0278(4) 0.0255(4) 0.0143(3) -0.0029(3) -0.0007(3) 0.0163(4) C8 0.0313(5) 0.0244(4) 0.0164(4) 0.0028(3) -0.0041(3) 0.0128(4) C17 0.0135(3) 0.0325(5) 0.0390(6) 0.0029(4) 0.0039(4) 0.0116(4) C10 0.0343(5) 0.0198(4) 0.0285(5) 0.0039(3) -0.0047(4) 0.0161(4) C9 0.0383(6) 0.0246(4) 0.0234(4) 0.0067(4) -0.0062(4) 0.0156(4) O2 0.0205(3) 0.0279(3) 0.0225(3) 0.0046(3) 0.0061(2) 0.0119(3) C28 0.0267(5) 0.0415(6) 0.0397(6) 0.0064(5) 0.0089(4) 0.0211(5) C25 0.0342(6) 0.0437(7) 0.0263(5) 0.0109(5) 0.0022(4) 0.0133(5) C26 0.0687(13) 0.0925(16) 0.0268(7) -0.0082(8) 0.0122(7) 0.0258(12) C27 0.0800(14) 0.0773(14) 0.0485(10) 0.0047(9) 0.0295(10) 0.0536(12) N2 0.0160(3) 0.0149(3) 0.0155(3) 0.0002(2) -0.0008(2) 0.0098(2) C31 0.0157(3) 0.0155(3) 0.0311(4) -0.0001(3) 0.0006(3) 0.0072(3) C37 0.0142(3) 0.0156(3) 0.0293(4) -0.0011(3) -0.0006(3) 0.0073(3) C29 0.0221(4) 0.0251(4) 0.0201(4) 0.0029(3) -0.0001(3) 0.0163(3) C30 0.0195(4) 0.0267(4) 0.0224(4) -0.0012(3) 0.0022(3) 0.0152(3) C36 0.0230(4) 0.0284(5) 0.0309(5) -0.0072(4) -0.0099(4) 0.0179(4) C32 0.0174(4) 0.0251(5) 0.0503(7) 0.0027(4) 0.0081(4) 0.0102(4) C39 0.0175(4) 0.0218(4) 0.0406(6) -0.0106(4) -0.0026(4) 0.0039(3) C35 0.0303(5) 0.0408(6) 0.0171(4) -0.0045(4) -0.0047(3) 0.0154(5) C34 0.0266(5) 0.0157(4) 0.0445(6) 0.0010(4) 0.0035(4) 0.0113(3) C33 0.0280(5) 0.0255(5) 0.0396(6) -0.0047(4) -0.0114(5) 0.0056(4) C38 0.0222(4) 0.0239(5) 0.0692(9) 0.0086(5) 0.0064(5) 0.0155(4) C40 0.0351(6) 0.0261(5) 0.0274(5) 0.0056(4) 0.0032(4) 0.0110(4) O1 0.0192(3) 0.0284(3) 0.0170(3) 0.0035(2) 0.0020(2) 0.0082(3) C21 0.0210(4) 0.0374(6) 0.0288(5) 0.0027(4) 0.0027(4) 0.0083(4) C24 0.0374(6) 0.0560(8) 0.0226(5) 0.0052(5) -0.0056(4) 0.0199(6) C22 0.0520(9) 0.0767(12) 0.0388(8) 0.0187(8) 0.0241(7) 0.0417(9) C23 0.1030(19) 0.124(2) 0.0267(7) -0.0163(10) -0.0036(9) 0.0763(18) Li2 0.0194(7) 0.0209(7) 0.0193(7) -0.0024(6) 0.0036(6) 0.0096(6) Li1 0.0199(7) 0.0198(7) 0.0187(7) 0.0007(6) 0.0017(6) 0.0084(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si2 N2 1.7108(7) . ? Si2 C29 1.8811(10) . ? Si2 C30 1.8922(10) . ? Si2 C31 1.9066(10) . ? Si2 Li1 3.0723(19) . ? Si1 N1 1.7087(8) . ? Si1 C36 1.8818(10) . ? Si1 C35 1.8887(12) . ? Si1 C37 1.9010(10) . ? Si1 Li2 3.0596(18) . ? N1 C1 1.3784(11) . ? N1 Li2 1.9707(19) . ? N1 Li1 2.124(2) . ? C2 C1 1.4127(11) . ? C2 C20 1.4373(11) . ? C2 C3 1.4975(11) . ? C2 Li1 2.531(2) . ? C1 C13 1.4417(12) . ? C1 Li1 2.244(2) . ? C4 N2 1.3744(11) . ? C4 C3 1.4117(11) . ? C4 C5 1.4424(12) . ? C4 Li2 2.232(2) . ? C20 C15 1.4210(12) . ? C20 C19 1.4215(13) . ? C12 C11 1.4228(12) . ? C12 C7 1.4240(12) . ? C12 C3 1.4347(11) . ? C3 Li2 2.558(2) . ? C15 C16 1.4141(13) . ? C15 C14 1.4225(14) . ? C7 C6 1.4160(13) . ? C7 C8 1.4170(13) . ? C19 C18 1.3776(13) . ? C19 H19 0.9300 . ? C13 C14 1.3631(13) . ? C13 H13 0.9300 . ? C11 C10 1.3763(14) . ? C11 H11 0.9300 . ? C18 C17 1.4066(17) . ? C18 H18 0.9300 . ? C14 H14 0.9300 . ? C5 C6 1.3609(14) . ? C5 H5 0.9300 . ? C16 C17 1.3726(18) . ? C16 H16 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.3686(17) . ? C8 H8 0.9300 . ? C17 H17 0.9300 . ? C10 C9 1.4071(18) . ? C10 H10 0.9300 . ? C9 H9 0.9300 . ? O2 C25 1.4346(15) . ? O2 C28 1.4360(14) . ? O2 Li2 1.9392(19) . ? C28 C27 1.499(2) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C25 C26 1.515(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.552(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27B 0.9700 . ? C27 H27A 0.9700 . ? N2 Li1 1.975(2) . ? N2 Li2 2.115(2) . ? C31 C34 1.5346(14) . ? C31 C32 1.5354(15) . ? C31 C33 1.5369(18) . ? C37 C40 1.5314(17) . ? C37 C38 1.5314(14) . ? C37 C39 1.5359(14) . ? C29 H29C 0.9600 . ? C29 H29B 0.9600 . ? C29 H29A 0.9600 . ? C30 H30C 0.9600 . ? C30 H30B 0.9600 . ? C30 H30A 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C32 H32C 0.9600 . ? C32 H32B 0.9600 . ? C32 H32A 0.9600 . ? C39 H39C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C35 H35C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C33 H33C 0.9600 . ? C33 H33B 0.9600 . ? C33 H33A 0.9600 . ? C38 H38C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C40 H40A 0.9600 . ? C40 H40C 0.9600 . ? C40 H40B 0.9600 . ? O1 C24 1.4310(15) . ? O1 C21 1.4371(14) . ? O1 Li1 1.923(2) . ? C21 C22 1.509(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C24 C23 1.503(3) . ? C24 H24B 0.9700 . ? C24 H24A 0.9700 . ? C22 C23 1.521(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23B 0.9700 . ? C23 H23A 0.9700 . ? Li2 Li1 2.610(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Si2 C29 103.83(4) . . ? N2 Si2 C30 116.34(4) . . ? C29 Si2 C30 106.57(4) . . ? N2 Si2 C31 113.36(4) . . ? C29 Si2 C31 108.71(5) . . ? C30 Si2 C31 107.56(5) . . ? N2 Si2 Li1 36.36(4) . . ? C29 Si2 Li1 69.30(5) . . ? C30 Si2 Li1 137.26(5) . . ? C31 Si2 Li1 114.02(5) . . ? N1 Si1 C36 105.01(4) . . ? N1 Si1 C35 117.66(5) . . ? C36 Si1 C35 104.80(6) . . ? N1 Si1 C37 112.27(4) . . ? C36 Si1 C37 109.14(5) . . ? C35 Si1 C37 107.46(6) . . ? N1 Si1 Li2 36.57(4) . . ? C36 Si1 Li2 72.58(5) . . ? C35 Si1 Li2 143.21(6) . . ? C37 Si1 Li2 107.89(5) . . ? C1 N1 Si1 128.52(6) . . ? C1 N1 Li2 117.83(8) . . ? Si1 N1 Li2 112.32(7) . . ? C1 N1 Li1 76.43(7) . . ? Si1 N1 Li1 125.33(7) . . ? Li2 N1 Li1 79.12(8) . . ? C1 C2 C20 119.81(7) . . ? C1 C2 C3 123.07(7) . . ? C20 C2 C3 116.90(7) . . ? C1 C2 Li1 61.94(6) . . ? C20 C2 Li1 117.99(7) . . ? C3 C2 Li1 95.61(6) . . ? N1 C1 C2 120.60(7) . . ? N1 C1 C13 121.98(8) . . ? C2 C1 C13 117.23(7) . . ? N1 C1 Li1 66.91(6) . . ? C2 C1 Li1 84.32(7) . . ? C13 C1 Li1 115.92(8) . . ? N2 C4 C3 120.65(7) . . ? N2 C4 C5 122.05(7) . . ? C3 C4 C5 117.14(7) . . ? N2 C4 Li2 67.01(7) . . ? C3 C4 Li2 86.05(7) . . ? C5 C4 Li2 114.23(8) . . ? C15 C20 C19 117.42(8) . . ? C15 C20 C2 120.69(8) . . ? C19 C20 C2 121.87(8) . . ? C11 C12 C7 117.35(8) . . ? C11 C12 C3 121.96(8) . . ? C7 C12 C3 120.68(7) . . ? C4 C3 C12 120.00(7) . . ? C4 C3 C2 122.66(7) . . ? C12 C3 C2 117.13(7) . . ? C4 C3 Li2 60.54(6) . . ? C12 C3 Li2 120.43(7) . . ? C2 C3 Li2 94.50(6) . . ? C16 C15 C20 120.09(9) . . ? C16 C15 C14 121.55(9) . . ? C20 C15 C14 118.34(8) . . ? C6 C7 C8 121.64(9) . . ? C6 C7 C12 118.31(8) . . ? C8 C7 C12 120.04(9) . . ? C18 C19 C20 121.33(9) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C14 C13 C1 122.79(8) . . ? C14 C13 H13 118.6 . . ? C1 C13 H13 118.6 . . ? C10 C11 C12 121.15(10) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C19 C18 C17 120.64(10) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C13 C14 C15 120.57(8) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C6 C5 C4 122.87(8) . . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C17 C16 C15 120.98(10) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C5 C6 C7 120.76(8) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C9 C8 C7 121.07(10) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C16 C17 C18 119.52(9) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C11 C10 C9 121.00(10) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C8 C9 C10 119.38(9) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C25 O2 C28 106.00(10) . . ? C25 O2 Li2 122.64(10) . . ? C28 O2 Li2 131.30(10) . . ? O2 C28 C27 105.39(14) . . ? O2 C28 H28A 110.7 . . ? C27 C28 H28A 110.7 . . ? O2 C28 H28B 110.7 . . ? C27 C28 H28B 110.7 . . ? H28A C28 H28B 108.8 . . ? O2 C25 C26 105.01(15) . . ? O2 C25 H25A 110.7 . . ? C26 C25 H25A 110.7 . . ? O2 C25 H25B 110.7 . . ? C26 C25 H25B 110.7 . . ? H25A C25 H25B 108.8 . . ? C25 C26 C27 104.84(14) . . ? C25 C26 H26A 110.8 . . ? C27 C26 H26A 110.8 . . ? C25 C26 H26B 110.8 . . ? C27 C26 H26B 110.8 . . ? H26A C26 H26B 108.9 . . ? C28 C27 C26 103.49(14) . . ? C28 C27 H27B 111.1 . . ? C26 C27 H27B 111.1 . . ? C28 C27 H27A 111.1 . . ? C26 C27 H27A 111.1 . . ? H27B C27 H27A 109.0 . . ? C4 N2 Si2 128.29(6) . . ? C4 N2 Li1 117.87(8) . . ? Si2 N2 Li1 112.73(7) . . ? C4 N2 Li2 76.26(7) . . ? Si2 N2 Li2 124.44(6) . . ? Li1 N2 Li2 79.23(8) . . ? C34 C31 C32 108.49(9) . . ? C34 C31 C33 109.01(10) . . ? C32 C31 C33 108.13(10) . . ? C34 C31 Si2 109.75(7) . . ? C32 C31 Si2 109.58(7) . . ? C33 C31 Si2 111.82(8) . . ? C40 C37 C38 108.62(11) . . ? C40 C37 C39 109.10(9) . . ? C38 C37 C39 108.08(9) . . ? C40 C37 Si1 109.80(7) . . ? C38 C37 Si1 110.56(7) . . ? C39 C37 Si1 110.63(8) . . ? Si2 C29 H29C 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29C C29 H29B 109.5 . . ? Si2 C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? Si2 C30 H30C 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30C C30 H30B 109.5 . . ? Si2 C30 H30A 109.5 . . ? H30C C30 H30A 109.5 . . ? H30B C30 H30A 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C31 C32 H32C 109.5 . . ? C31 C32 H32B 109.5 . . ? H32C C32 H32B 109.5 . . ? C31 C32 H32A 109.5 . . ? H32C C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? C37 C39 H39C 109.5 . . ? C37 C39 H39A 109.5 . . ? H39C C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39C C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si1 C35 H35C 109.5 . . ? Si1 C35 H35A 109.5 . . ? H35C C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35C C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C33 H33C 109.5 . . ? C31 C33 H33B 109.5 . . ? H33C C33 H33B 109.5 . . ? C31 C33 H33A 109.5 . . ? H33C C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? C37 C38 H38C 109.5 . . ? C37 C38 H38A 109.5 . . ? H38C C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38C C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? H40C C40 H40B 109.5 . . ? C24 O1 C21 105.91(9) . . ? C24 O1 Li1 134.62(10) . . ? C21 O1 Li1 118.98(9) . . ? O1 C21 C22 105.95(12) . . ? O1 C21 H21A 110.5 . . ? C22 C21 H21A 110.5 . . ? O1 C21 H21B 110.5 . . ? C22 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? O1 C24 C23 104.27(13) . . ? O1 C24 H24B 110.9 . . ? C23 C24 H24B 110.9 . . ? O1 C24 H24A 110.9 . . ? C23 C24 H24A 110.9 . . ? H24B C24 H24A 108.9 . . ? C21 C22 C23 104.18(13) . . ? C21 C22 H22A 110.9 . . ? C23 C22 H22A 110.9 . . ? C21 C22 H22B 110.9 . . ? C23 C22 H22B 110.9 . . ? H22A C22 H22B 108.9 . . ? C24 C23 C22 105.17(15) . . ? C24 C23 H23B 110.7 . . ? C22 C23 H23B 110.7 . . ? C24 C23 H23A 110.7 . . ? C22 C23 H23A 110.7 . . ? H23B C23 H23A 108.8 . . ? O2 Li2 N1 135.47(10) . . ? O2 Li2 N2 126.00(9) . . ? N1 Li2 N2 98.51(8) . . ? O2 Li2 C4 110.93(9) . . ? N1 Li2 C4 105.64(8) . . ? N2 Li2 C4 36.73(4) . . ? O2 Li2 C3 119.17(9) . . ? N1 Li2 C3 80.47(7) . . ? N2 Li2 C3 61.54(5) . . ? C4 Li2 C3 33.41(4) . . ? O2 Li2 Li1 164.22(11) . . ? N1 Li2 Li1 53.03(6) . . ? N2 Li2 Li1 48.01(6) . . ? C4 Li2 Li1 72.68(7) . . ? C3 Li2 Li1 72.71(6) . . ? O2 Li2 Si1 109.04(8) . . ? N1 Li2 Si1 31.11(4) . . ? N2 Li2 Si1 121.31(7) . . ? C4 Li2 Si1 136.70(7) . . ? C3 Li2 Si1 109.81(6) . . ? Li1 Li2 Si1 73.46(6) . . ? O1 Li1 N2 135.47(10) . . ? O1 Li1 N1 126.23(10) . . ? N2 Li1 N1 98.10(8) . . ? O1 Li1 C1 108.38(9) . . ? N2 Li1 C1 105.31(9) . . ? N1 Li1 C1 36.66(4) . . ? O1 Li1 C2 114.39(9) . . ? N2 Li1 C2 80.39(7) . . ? N1 Li1 C2 62.06(5) . . ? C1 Li1 C2 33.74(4) . . ? O1 Li1 Li2 168.25(11) . . ? N2 Li1 Li2 52.76(6) . . ? N1 Li1 Li2 47.85(6) . . ? C1 Li1 Li2 72.46(7) . . ? C2 Li1 Li2 73.13(7) . . ? O1 Li1 Si2 111.14(8) . . ? N2 Li1 Si2 30.90(4) . . ? N1 Li1 Si2 120.43(7) . . ? C1 Li1 Si2 136.12(8) . . ? C2 Li1 Si2 109.60(7) . . ? Li2 Li1 Si2 72.74(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C36 Si1 N1 C1 -165.51(8) . . . . ? C35 Si1 N1 C1 -49.47(10) . . . . ? C37 Si1 N1 C1 76.03(9) . . . . ? Li2 Si1 N1 C1 166.32(12) . . . . ? C36 Si1 N1 Li2 28.17(8) . . . . ? C35 Si1 N1 Li2 144.21(8) . . . . ? C37 Si1 N1 Li2 -90.29(8) . . . . ? C36 Si1 N1 Li1 -64.18(9) . . . . ? C35 Si1 N1 Li1 51.86(9) . . . . ? C37 Si1 N1 Li1 177.36(8) . . . . ? Li2 Si1 N1 Li1 -92.35(10) . . . . ? Si1 N1 C1 C2 -167.54(7) . . . . ? Li2 N1 C1 C2 -1.86(12) . . . . ? Li1 N1 C1 C2 67.84(9) . . . . ? Si1 N1 C1 C13 17.52(13) . . . . ? Li2 N1 C1 C13 -176.80(9) . . . . ? Li1 N1 C1 C13 -107.10(10) . . . . ? Si1 N1 C1 Li1 124.62(9) . . . . ? Li2 N1 C1 Li1 -69.70(9) . . . . ? C20 C2 C1 N1 -166.80(8) . . . . ? C3 C2 C1 N1 18.69(12) . . . . ? Li1 C2 C1 N1 -58.89(8) . . . . ? C20 C2 C1 C13 8.37(12) . . . . ? C3 C2 C1 C13 -166.13(8) . . . . ? Li1 C2 C1 C13 116.28(9) . . . . ? C20 C2 C1 Li1 -107.91(9) . . . . ? C3 C2 C1 Li1 77.58(9) . . . . ? C1 C2 C20 C15 -6.17(12) . . . . ? C3 C2 C20 C15 168.67(8) . . . . ? Li1 C2 C20 C15 -78.14(10) . . . . ? C1 C2 C20 C19 171.99(8) . . . . ? C3 C2 C20 C19 -13.17(12) . . . . ? Li1 C2 C20 C19 100.02(10) . . . . ? N2 C4 C3 C12 -170.49(8) . . . . ? C5 C4 C3 C12 5.05(12) . . . . ? Li2 C4 C3 C12 -110.22(8) . . . . ? N2 C4 C3 C2 14.95(12) . . . . ? C5 C4 C3 C2 -169.51(8) . . . . ? Li2 C4 C3 C2 75.22(9) . . . . ? N2 C4 C3 Li2 -60.27(8) . . . . ? C5 C4 C3 Li2 115.27(9) . . . . ? C11 C12 C3 C4 175.17(8) . . . . ? C7 C12 C3 C4 -4.08(12) . . . . ? C11 C12 C3 C2 -9.97(12) . . . . ? C7 C12 C3 C2 170.78(8) . . . . ? C11 C12 C3 Li2 103.80(10) . . . . ? C7 C12 C3 Li2 -75.44(10) . . . . ? C1 C2 C3 C4 -77.44(11) . . . . ? C20 C2 C3 C4 107.91(9) . . . . ? Li1 C2 C3 C4 -17.45(9) . . . . ? C1 C2 C3 C12 107.85(9) . . . . ? C20 C2 C3 C12 -66.80(10) . . . . ? Li1 C2 C3 C12 167.85(7) . . . . ? C1 C2 C3 Li2 -19.82(9) . . . . ? C20 C2 C3 Li2 165.53(7) . . . . ? Li1 C2 C3 Li2 40.17(7) . . . . ? C19 C20 C15 C16 -0.09(13) . . . . ? C2 C20 C15 C16 178.15(9) . . . . ? C19 C20 C15 C14 -178.73(9) . . . . ? C2 C20 C15 C14 -0.49(13) . . . . ? C11 C12 C7 C6 -179.53(9) . . . . ? C3 C12 C7 C6 -0.24(13) . . . . ? C11 C12 C7 C8 -0.30(13) . . . . ? C3 C12 C7 C8 178.98(9) . . . . ? C15 C20 C19 C18 1.27(14) . . . . ? C2 C20 C19 C18 -176.95(9) . . . . ? N1 C1 C13 C14 170.78(9) . . . . ? C2 C1 C13 C14 -4.32(14) . . . . ? Li1 C1 C13 C14 92.93(12) . . . . ? C7 C12 C11 C10 0.65(14) . . . . ? C3 C12 C11 C10 -178.62(9) . . . . ? C20 C19 C18 C17 -1.03(17) . . . . ? C1 C13 C14 C15 -2.30(16) . . . . ? C16 C15 C14 C13 -173.93(10) . . . . ? C20 C15 C14 C13 4.69(15) . . . . ? N2 C4 C5 C6 173.56(9) . . . . ? C3 C4 C5 C6 -1.92(14) . . . . ? Li2 C4 C5 C6 96.47(12) . . . . ? C20 C15 C16 C17 -1.36(16) . . . . ? C14 C15 C16 C17 177.23(11) . . . . ? C4 C5 C6 C7 -2.41(16) . . . . ? C8 C7 C6 C5 -175.75(10) . . . . ? C12 C7 C6 C5 3.46(15) . . . . ? C6 C7 C8 C9 179.05(11) . . . . ? C12 C7 C8 C9 -0.14(16) . . . . ? C15 C16 C17 C18 1.63(18) . . . . ? C19 C18 C17 C16 -0.44(18) . . . . ? C12 C11 C10 C9 -0.55(17) . . . . ? C7 C8 C9 C10 0.26(18) . . . . ? C11 C10 C9 C8 0.08(19) . . . . ? C25 O2 C28 C27 40.05(16) . . . . ? Li2 O2 C28 C27 -137.01(14) . . . . ? C28 O2 C25 C26 -36.50(16) . . . . ? Li2 O2 C25 C26 140.88(14) . . . . ? O2 C25 C26 C27 18.8(2) . . . . ? O2 C28 C27 C26 -26.5(2) . . . . ? C25 C26 C27 C28 4.6(2) . . . . ? C3 C4 N2 Si2 -166.50(6) . . . . ? C5 C4 N2 Si2 18.18(13) . . . . ? Li2 C4 N2 Si2 123.27(8) . . . . ? C3 C4 N2 Li1 0.53(12) . . . . ? C5 C4 N2 Li1 -174.79(9) . . . . ? Li2 C4 N2 Li1 -69.70(9) . . . . ? C3 C4 N2 Li2 70.23(9) . . . . ? C5 C4 N2 Li2 -105.09(10) . . . . ? C29 Si2 N2 C4 -173.92(8) . . . . ? C30 Si2 N2 C4 -57.21(9) . . . . ? C31 Si2 N2 C4 68.29(9) . . . . ? Li1 Si2 N2 C4 167.57(12) . . . . ? C29 Si2 N2 Li1 18.50(8) . . . . ? C30 Si2 N2 Li1 135.22(7) . . . . ? C31 Si2 N2 Li1 -99.29(8) . . . . ? C29 Si2 N2 Li2 -73.89(8) . . . . ? C30 Si2 N2 Li2 42.83(9) . . . . ? C31 Si2 N2 Li2 168.32(8) . . . . ? Li1 Si2 N2 Li2 -92.39(10) . . . . ? N2 Si2 C31 C34 170.10(8) . . . . ? C29 Si2 C31 C34 55.19(9) . . . . ? C30 Si2 C31 C34 -59.83(9) . . . . ? Li1 Si2 C31 C34 130.26(8) . . . . ? N2 Si2 C31 C32 51.07(9) . . . . ? C29 Si2 C31 C32 -63.84(9) . . . . ? C30 Si2 C31 C32 -178.86(8) . . . . ? Li1 Si2 C31 C32 11.23(10) . . . . ? N2 Si2 C31 C33 -68.80(9) . . . . ? C29 Si2 C31 C33 176.29(8) . . . . ? C30 Si2 C31 C33 61.27(9) . . . . ? Li1 Si2 C31 C33 -108.64(9) . . . . ? N1 Si1 C37 C40 56.91(8) . . . . ? C36 Si1 C37 C40 -59.08(9) . . . . ? C35 Si1 C37 C40 -172.20(8) . . . . ? Li2 Si1 C37 C40 18.15(9) . . . . ? N1 Si1 C37 C38 -62.92(10) . . . . ? C36 Si1 C37 C38 -178.91(9) . . . . ? C35 Si1 C37 C38 67.97(10) . . . . ? Li2 Si1 C37 C38 -101.68(10) . . . . ? N1 Si1 C37 C39 177.39(7) . . . . ? C36 Si1 C37 C39 61.40(8) . . . . ? C35 Si1 C37 C39 -51.72(8) . . . . ? Li2 Si1 C37 C39 138.63(7) . . . . ? C24 O1 C21 C22 -35.09(15) . . . . ? Li1 O1 C21 C22 137.99(12) . . . . ? C21 O1 C24 C23 38.83(19) . . . . ? Li1 O1 C24 C23 -132.66(18) . . . . ? O1 C21 C22 C23 16.9(2) . . . . ? O1 C24 C23 C22 -27.2(2) . . . . ? C21 C22 C23 C24 6.2(2) . . . . ? C25 O2 Li2 N1 86.14(18) . . . . ? C28 O2 Li2 N1 -97.22(18) . . . . ? C25 O2 Li2 N2 -95.54(15) . . . . ? C28 O2 Li2 N2 81.11(17) . . . . ? C25 O2 Li2 C4 -57.04(14) . . . . ? C28 O2 Li2 C4 119.60(13) . . . . ? C25 O2 Li2 C3 -21.14(15) . . . . ? C28 O2 Li2 C3 155.50(11) . . . . ? C25 O2 Li2 Li1 -157.5(4) . . . . ? C28 O2 Li2 Li1 19.1(5) . . . . ? C25 O2 Li2 Si1 105.96(11) . . . . ? C28 O2 Li2 Si1 -77.39(14) . . . . ? C1 N1 Li2 O2 -129.57(14) . . . . ? Si1 N1 Li2 O2 38.35(17) . . . . ? Li1 N1 Li2 O2 162.24(16) . . . . ? C1 N1 Li2 N2 51.80(11) . . . . ? Si1 N1 Li2 N2 -140.28(6) . . . . ? Li1 N1 Li2 N2 -16.38(8) . . . . ? C1 N1 Li2 C4 14.89(12) . . . . ? Si1 N1 Li2 C4 -177.19(6) . . . . ? Li1 N1 Li2 C4 -53.29(8) . . . . ? C1 N1 Li2 C3 -7.29(9) . . . . ? Si1 N1 Li2 C3 160.63(5) . . . . ? Li1 N1 Li2 C3 -75.47(6) . . . . ? C1 N1 Li2 Li1 68.18(9) . . . . ? Si1 N1 Li2 Li1 -123.89(7) . . . . ? C1 N1 Li2 Si1 -167.92(11) . . . . ? Li1 N1 Li2 Si1 123.89(7) . . . . ? C4 N2 Li2 O2 76.40(12) . . . . ? Si2 N2 Li2 O2 -50.88(15) . . . . ? Li1 N2 Li2 O2 -161.16(13) . . . . ? C4 N2 Li2 N1 -104.79(8) . . . . ? Si2 N2 Li2 N1 127.93(7) . . . . ? Li1 N2 Li2 N1 17.65(8) . . . . ? Si2 N2 Li2 C4 -127.28(8) . . . . ? Li1 N2 Li2 C4 122.44(8) . . . . ? C4 N2 Li2 C3 -30.55(4) . . . . ? Si2 N2 Li2 C3 -157.83(6) . . . . ? Li1 N2 Li2 C3 91.89(7) . . . . ? C4 N2 Li2 Li1 -122.44(8) . . . . ? Si2 N2 Li2 Li1 110.28(8) . . . . ? C4 N2 Li2 Si1 -127.52(9) . . . . ? Si2 N2 Li2 Si1 105.20(8) . . . . ? Li1 N2 Li2 Si1 -5.08(9) . . . . ? N2 C4 Li2 O2 -122.66(10) . . . . ? C3 C4 Li2 O2 111.59(10) . . . . ? C5 C4 Li2 O2 -6.48(12) . . . . ? N2 C4 Li2 N1 83.22(9) . . . . ? C3 C4 Li2 N1 -42.54(9) . . . . ? C5 C4 Li2 N1 -160.60(8) . . . . ? C3 C4 Li2 N2 -125.76(7) . . . . ? C5 C4 Li2 N2 116.18(8) . . . . ? N2 C4 Li2 C3 125.76(7) . . . . ? C5 C4 Li2 C3 -118.06(9) . . . . ? N2 C4 Li2 Li1 41.08(6) . . . . ? C3 C4 Li2 Li1 -84.68(7) . . . . ? C5 C4 Li2 Li1 157.26(8) . . . . ? N2 C4 Li2 Si1 81.10(12) . . . . ? C3 C4 Li2 Si1 -44.66(12) . . . . ? C5 C4 Li2 Si1 -162.72(10) . . . . ? C4 C3 Li2 O2 -84.08(10) . . . . ? C12 C3 Li2 O2 25.44(13) . . . . ? C2 C3 Li2 O2 150.66(9) . . . . ? C4 C3 Li2 N1 138.69(9) . . . . ? C12 C3 Li2 N1 -111.79(8) . . . . ? C2 C3 Li2 N1 13.42(7) . . . . ? C4 C3 Li2 N2 33.51(5) . . . . ? C12 C3 Li2 N2 143.03(7) . . . . ? C2 C3 Li2 N2 -91.75(6) . . . . ? C12 C3 Li2 C4 109.52(9) . . . . ? C2 C3 Li2 C4 -125.26(8) . . . . ? C4 C3 Li2 Li1 84.59(7) . . . . ? C12 C3 Li2 Li1 -165.89(8) . . . . ? C2 C3 Li2 Li1 -40.68(7) . . . . ? C4 C3 Li2 Si1 149.18(9) . . . . ? C12 C3 Li2 Si1 -101.30(8) . . . . ? C2 C3 Li2 Si1 23.91(7) . . . . ? N1 Si1 Li2 O2 -152.59(13) . . . . ? C36 Si1 Li2 O2 55.95(8) . . . . ? C35 Si1 Li2 O2 147.52(8) . . . . ? C37 Si1 Li2 O2 -49.10(9) . . . . ? C36 Si1 Li2 N1 -151.45(8) . . . . ? C35 Si1 Li2 N1 -59.89(12) . . . . ? C37 Si1 Li2 N1 103.49(7) . . . . ? N1 Si1 Li2 N2 47.71(8) . . . . ? C36 Si1 Li2 N2 -103.74(10) . . . . ? C35 Si1 Li2 N2 -12.18(15) . . . . ? C37 Si1 Li2 N2 151.20(8) . . . . ? N1 Si1 Li2 C4 3.95(8) . . . . ? C36 Si1 Li2 C4 -147.50(13) . . . . ? C35 Si1 Li2 C4 -55.94(16) . . . . ? C37 Si1 Li2 C4 107.44(12) . . . . ? N1 Si1 Li2 C3 -20.34(5) . . . . ? C36 Si1 Li2 C3 -171.79(8) . . . . ? C35 Si1 Li2 C3 -80.23(11) . . . . ? C37 Si1 Li2 C3 83.15(7) . . . . ? N1 Si1 Li2 Li1 43.77(7) . . . . ? C36 Si1 Li2 Li1 -107.68(7) . . . . ? C35 Si1 Li2 Li1 -16.12(11) . . . . ? C37 Si1 Li2 Li1 147.26(6) . . . . ? C24 O1 Li1 N2 -125.49(17) . . . . ? C21 O1 Li1 N2 63.87(18) . . . . ? C24 O1 Li1 N1 60.79(19) . . . . ? C21 O1 Li1 N1 -109.85(13) . . . . ? C24 O1 Li1 C1 97.23(15) . . . . ? C21 O1 Li1 C1 -73.41(12) . . . . ? C24 O1 Li1 C2 133.00(14) . . . . ? C21 O1 Li1 C2 -37.64(13) . . . . ? C24 O1 Li1 Li2 5.0(6) . . . . ? C21 O1 Li1 Li2 -165.6(5) . . . . ? C24 O1 Li1 Si2 -102.24(15) . . . . ? C21 O1 Li1 Si2 87.12(11) . . . . ? C4 N2 Li1 O1 -123.18(14) . . . . ? Si2 N2 Li1 O1 45.80(16) . . . . ? Li2 N2 Li1 O1 168.79(16) . . . . ? C4 N2 Li1 N1 51.70(10) . . . . ? Si2 N2 Li1 N1 -139.31(6) . . . . ? Li2 N2 Li1 N1 -16.32(8) . . . . ? C4 N2 Li1 C1 14.94(11) . . . . ? Si2 N2 Li1 C1 -176.07(6) . . . . ? Li2 N2 Li1 C1 -53.09(8) . . . . ? C4 N2 Li1 C2 -8.03(9) . . . . ? Si2 N2 Li1 C2 160.96(5) . . . . ? Li2 N2 Li1 C2 -76.05(7) . . . . ? C4 N2 Li1 Li2 68.03(9) . . . . ? Si2 N2 Li1 Li2 -122.99(7) . . . . ? C4 N2 Li1 Si2 -168.99(11) . . . . ? Li2 N2 Li1 Si2 122.99(7) . . . . ? C1 N1 Li1 O1 70.75(12) . . . . ? Si1 N1 Li1 O1 -57.13(14) . . . . ? Li2 N1 Li1 O1 -166.88(13) . . . . ? C1 N1 Li1 N2 -104.80(8) . . . . ? Si1 N1 Li1 N2 127.31(7) . . . . ? Li2 N1 Li1 N2 17.57(8) . . . . ? Si1 N1 Li1 C1 -127.89(8) . . . . ? Li2 N1 Li1 C1 122.37(8) . . . . ? C1 N1 Li1 C2 -30.25(5) . . . . ? Si1 N1 Li1 C2 -158.13(6) . . . . ? Li2 N1 Li1 C2 92.12(7) . . . . ? C1 N1 Li1 Li2 -122.37(8) . . . . ? Si1 N1 Li1 Li2 109.74(8) . . . . ? C1 N1 Li1 Si2 -127.65(9) . . . . ? Si1 N1 Li1 Si2 104.46(8) . . . . ? Li2 N1 Li1 Si2 -5.28(9) . . . . ? N1 C1 Li1 O1 -126.63(10) . . . . ? C2 C1 Li1 O1 106.61(9) . . . . ? C13 C1 Li1 O1 -10.97(12) . . . . ? N1 C1 Li1 N2 82.93(8) . . . . ? C2 C1 Li1 N2 -43.84(8) . . . . ? C13 C1 Li1 N2 -161.41(8) . . . . ? C2 C1 Li1 N1 -126.77(7) . . . . ? C13 C1 Li1 N1 115.66(9) . . . . ? N1 C1 Li1 C2 126.77(7) . . . . ? C13 C1 Li1 C2 -117.57(9) . . . . ? N1 C1 Li1 Li2 41.05(6) . . . . ? C2 C1 Li1 Li2 -85.72(7) . . . . ? C13 C1 Li1 Li2 156.71(8) . . . . ? N1 C1 Li1 Si2 80.02(11) . . . . ? C2 C1 Li1 Si2 -46.74(11) . . . . ? C13 C1 Li1 Si2 -164.32(9) . . . . ? C1 C2 Li1 O1 -86.83(10) . . . . ? C20 C2 Li1 O1 23.94(12) . . . . ? C3 C2 Li1 O1 148.48(9) . . . . ? C1 C2 Li1 N2 137.35(8) . . . . ? C20 C2 Li1 N2 -111.88(8) . . . . ? C3 C2 Li1 N2 12.67(7) . . . . ? C1 C2 Li1 N1 32.78(5) . . . . ? C20 C2 Li1 N1 143.55(7) . . . . ? C3 C2 Li1 N1 -91.90(6) . . . . ? C20 C2 Li1 C1 110.77(8) . . . . ? C3 C2 Li1 C1 -124.68(7) . . . . ? C1 C2 Li1 Li2 83.51(7) . . . . ? C20 C2 Li1 Li2 -165.72(8) . . . . ? C3 C2 Li1 Li2 -41.18(7) . . . . ? C1 C2 Li1 Si2 147.60(8) . . . . ? C20 C2 Li1 Si2 -101.63(8) . . . . ? C3 C2 Li1 Si2 22.91(7) . . . . ? O2 Li2 Li1 O1 -64.1(7) . . . . ? N1 Li2 Li1 O1 64.1(5) . . . . ? N2 Li2 Li1 O1 -138.0(5) . . . . ? C4 Li2 Li1 O1 -169.9(5) . . . . ? C3 Li2 Li1 O1 155.1(5) . . . . ? Si1 Li2 Li1 O1 37.5(5) . . . . ? O2 Li2 Li1 N2 73.9(4) . . . . ? N1 Li2 Li1 N2 -157.95(10) . . . . ? C4 Li2 Li1 N2 -31.92(5) . . . . ? C3 Li2 Li1 N2 -66.97(6) . . . . ? Si1 Li2 Li1 N2 175.47(8) . . . . ? O2 Li2 Li1 N1 -128.1(4) . . . . ? N2 Li2 Li1 N1 157.95(10) . . . . ? C4 Li2 Li1 N1 126.03(9) . . . . ? C3 Li2 Li1 N1 90.99(7) . . . . ? Si1 Li2 Li1 N1 -26.58(4) . . . . ? O2 Li2 Li1 C1 -160.1(4) . . . . ? N1 Li2 Li1 C1 -31.93(5) . . . . ? N2 Li2 Li1 C1 126.02(8) . . . . ? C4 Li2 Li1 C1 94.10(7) . . . . ? C3 Li2 Li1 C1 59.06(5) . . . . ? Si1 Li2 Li1 C1 -58.51(4) . . . . ? O2 Li2 Li1 C2 164.6(4) . . . . ? N1 Li2 Li1 C2 -67.30(6) . . . . ? N2 Li2 Li1 C2 90.66(7) . . . . ? C4 Li2 Li1 C2 58.73(5) . . . . ? C3 Li2 Li1 C2 23.69(4) . . . . ? Si1 Li2 Li1 C2 -93.87(5) . . . . ? O2 Li2 Li1 Si2 47.1(4) . . . . ? N1 Li2 Li1 Si2 175.23(8) . . . . ? N2 Li2 Li1 Si2 -26.81(4) . . . . ? C4 Li2 Li1 Si2 -58.74(4) . . . . ? C3 Li2 Li1 Si2 -93.78(5) . . . . ? Si1 Li2 Li1 Si2 148.66(5) . . . . ? N2 Si2 Li1 O1 -147.38(12) . . . . ? C29 Si2 Li1 O1 51.85(8) . . . . ? C30 Si2 Li1 O1 144.16(7) . . . . ? C31 Si2 Li1 O1 -50.10(9) . . . . ? C29 Si2 Li1 N2 -160.77(8) . . . . ? C30 Si2 Li1 N2 -68.46(10) . . . . ? C31 Si2 Li1 N2 97.28(7) . . . . ? N2 Si2 Li1 N1 48.46(8) . . . . ? C29 Si2 Li1 N1 -112.30(9) . . . . ? C30 Si2 Li1 N1 -20.00(13) . . . . ? C31 Si2 Li1 N1 145.74(8) . . . . ? N2 Si2 Li1 C1 5.47(8) . . . . ? C29 Si2 Li1 C1 -155.30(12) . . . . ? C30 Si2 Li1 C1 -63.00(14) . . . . ? C31 Si2 Li1 C1 102.74(11) . . . . ? N2 Si2 Li1 C2 -19.97(5) . . . . ? C29 Si2 Li1 C2 179.26(8) . . . . ? C30 Si2 Li1 C2 -88.43(9) . . . . ? C31 Si2 Li1 C2 77.31(7) . . . . ? N2 Si2 Li1 Li2 44.37(7) . . . . ? C29 Si2 Li1 Li2 -116.40(7) . . . . ? C30 Si2 Li1 Li2 -24.10(9) . . . . ? C31 Si2 Li1 Li2 141.64(6) . . . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.519 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.060