# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Luo Yunjie' _publ_contact_author_email lyj@nit.net.cn _publ_author_name 'Yunjie Luo' data_[(SiMe3)2NC(NCy)2]Nd[N(SiMe3)2]2 _database_code_depnum_ccdc_archive 'CCDC 803565' #TrackingRef 'ccdc.doc' #TrackingRef 'ccdc.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H76 N5 Nd Si6' _chemical_formula_sum 'C31 H76 N5 Nd Si6' _chemical_formula_weight 831.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5611(10) _cell_length_b 24.392(3) _cell_length_c 20.327(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.353(3) _cell_angle_gamma 90.00 _cell_volume 4739.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9727 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1764 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.418 _exptl_absorpt_correction_T_max 0.602 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32618 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8536 _reflns_number_gt 6593 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0343P)^2^+3.8203P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8536 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _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 Nd1 Nd 0.25226(3) 0.393211(11) 0.747124(12) 0.04073(10) Uani 1 1 d . . . Si1 Si 0.3709(2) 0.18531(8) 0.68290(9) 0.0739(5) Uani 1 1 d . . . Si2 Si 0.0981(2) 0.18236(7) 0.76132(11) 0.0781(5) Uani 1 1 d . . . Si3 Si 0.49793(16) 0.43631(7) 0.63346(8) 0.0559(4) Uani 1 1 d . . . Si4 Si 0.21646(16) 0.49398(7) 0.63220(8) 0.0629(4) Uani 1 1 d . . . Si5 Si 0.30345(17) 0.47243(7) 0.88343(7) 0.0589(4) Uani 1 1 d . . . Si6 Si 0.01233(17) 0.42405(8) 0.86957(8) 0.0622(4) Uani 1 1 d . . . N1 N 0.1637(4) 0.31000(17) 0.69612(19) 0.0450(10) Uani 1 1 d . . . N2 N 0.3256(4) 0.30175(16) 0.77727(18) 0.0428(9) Uani 1 1 d . . . N3 N 0.2375(4) 0.21812(17) 0.7264(2) 0.0506(10) Uani 1 1 d . . . N4 N 0.3336(4) 0.44732(18) 0.6627(2) 0.0495(10) Uani 1 1 d . . . N5 N 0.1783(4) 0.43487(18) 0.84294(19) 0.0505(10) Uani 1 1 d . . . C1 C 0.2429(5) 0.2760(2) 0.7332(2) 0.0406(11) Uani 1 1 d . . . C2 C 0.0878(5) 0.2921(2) 0.6363(2) 0.0522(13) Uani 1 1 d . . . H2 H 0.0968 0.2522 0.6322 0.063 Uiso 1 1 calc R . . C3 C 0.1504(6) 0.3187(3) 0.5771(3) 0.0758(19) Uani 1 1 d . . . H3A H 0.2471 0.3073 0.5739 0.091 Uiso 1 1 calc R . . H3B H 0.1492 0.3582 0.5828 0.091 Uiso 1 1 calc R . . C4 C 0.0709(7) 0.3039(4) 0.5131(3) 0.100(3) Uani 1 1 d . . . H4A H 0.1107 0.3238 0.4767 0.120 Uiso 1 1 calc R . . H4B H 0.0812 0.2650 0.5046 0.120 Uiso 1 1 calc R . . C5 C -0.0817(7) 0.3177(4) 0.5176(3) 0.100(3) Uani 1 1 d . . . H5A H -0.0926 0.3572 0.5211 0.119 Uiso 1 1 calc R . . H5B H -0.1308 0.3057 0.4779 0.119 Uiso 1 1 calc R . . C6 C -0.1446(6) 0.2908(3) 0.5761(3) 0.091(2) Uani 1 1 d . . . H6A H -0.1416 0.2513 0.5706 0.109 Uiso 1 1 calc R . . H6B H -0.2418 0.3017 0.5791 0.109 Uiso 1 1 calc R . . C7 C -0.0657(5) 0.3066(3) 0.6392(3) 0.0677(17) Uani 1 1 d . . . H7A H -0.0752 0.3458 0.6464 0.081 Uiso 1 1 calc R . . H7B H -0.1068 0.2878 0.6761 0.081 Uiso 1 1 calc R . . C8 C 0.4009(5) 0.2717(2) 0.8297(2) 0.0515(13) Uani 1 1 d . . . H8 H 0.3934 0.2323 0.8213 0.062 Uiso 1 1 calc R . . C9 C 0.3371(6) 0.2848(3) 0.8954(3) 0.086(2) Uani 1 1 d . . . H9A H 0.2398 0.2734 0.8945 0.103 Uiso 1 1 calc R . . H9B H 0.3398 0.3241 0.9026 0.103 Uiso 1 1 calc R . . C10 C 0.4150(7) 0.2558(4) 0.9526(3) 0.121(4) Uani 1 1 d . . . H10A H 0.3739 0.2663 0.9939 0.145 Uiso 1 1 calc R . . H10B H 0.4054 0.2164 0.9478 0.145 Uiso 1 1 calc R . . C11 C 0.5667(7) 0.2709(4) 0.9538(3) 0.103(3) Uani 1 1 d . . . H11A H 0.5762 0.3094 0.9647 0.124 Uiso 1 1 calc R . . H11B H 0.6151 0.2499 0.9879 0.124 Uiso 1 1 calc R . . C12 C 0.6334(7) 0.2605(4) 0.8900(3) 0.096(3) Uani 1 1 d . . . H12A H 0.6369 0.2213 0.8822 0.115 Uiso 1 1 calc R . . H12B H 0.7288 0.2740 0.8920 0.115 Uiso 1 1 calc R . . C13 C 0.5549(6) 0.2880(3) 0.8328(3) 0.079(2) Uani 1 1 d . . . H13A H 0.5982 0.2779 0.7919 0.095 Uiso 1 1 calc R . . H13B H 0.5621 0.3275 0.8375 0.095 Uiso 1 1 calc R . . C14 C 0.4844(11) 0.1412(4) 0.7371(5) 0.174(6) Uani 1 1 d . . . H14A H 0.5005 0.1593 0.7786 0.261 Uiso 1 1 calc R . . H14B H 0.5722 0.1350 0.7164 0.261 Uiso 1 1 calc R . . H14C H 0.4388 0.1068 0.7443 0.261 Uiso 1 1 calc R . . C15 C 0.4877(7) 0.2363(3) 0.6458(3) 0.094(2) Uani 1 1 d . . . H15A H 0.4327 0.2641 0.6241 0.141 Uiso 1 1 calc R . . H15B H 0.5460 0.2185 0.6144 0.141 Uiso 1 1 calc R . . H15C H 0.5454 0.2528 0.6797 0.141 Uiso 1 1 calc R . . C16 C 0.2957(10) 0.1427(4) 0.6171(5) 0.162(5) Uani 1 1 d . . . H16A H 0.2391 0.1145 0.6359 0.242 Uiso 1 1 calc R . . H16B H 0.3695 0.1263 0.5927 0.242 Uiso 1 1 calc R . . H16C H 0.2388 0.1650 0.5882 0.242 Uiso 1 1 calc R . . C17 C -0.0217(10) 0.1515(4) 0.6972(5) 0.163(5) Uani 1 1 d . . . H17A H -0.0110 0.1705 0.6563 0.245 Uiso 1 1 calc R . . H17B H -0.1168 0.1547 0.7110 0.245 Uiso 1 1 calc R . . H17C H 0.0013 0.1135 0.6916 0.245 Uiso 1 1 calc R . . C18 C 0.1694(10) 0.1276(4) 0.8171(6) 0.166(5) Uani 1 1 d . . . H18A H 0.2030 0.0977 0.7912 0.249 Uiso 1 1 calc R . . H18B H 0.0968 0.1148 0.8451 0.249 Uiso 1 1 calc R . . H18C H 0.2450 0.1423 0.8436 0.249 Uiso 1 1 calc R . . C19 C -0.0065(7) 0.2284(3) 0.8122(4) 0.095(2) Uani 1 1 d . . . H19A H 0.0538 0.2469 0.8433 0.142 Uiso 1 1 calc R . . H19B H -0.0746 0.2073 0.8352 0.142 Uiso 1 1 calc R . . H19C H -0.0532 0.2548 0.7845 0.142 Uiso 1 1 calc R . . C20 C 0.5007(7) 0.4076(3) 0.5480(3) 0.094(2) Uani 1 1 d . . . H20A H 0.4651 0.3708 0.5482 0.141 Uiso 1 1 calc R . . H20B H 0.5950 0.4074 0.5328 0.141 Uiso 1 1 calc R . . H20C H 0.4433 0.4298 0.5192 0.141 Uiso 1 1 calc R . . C21 C 0.5852(7) 0.3849(3) 0.6889(3) 0.087(2) Uani 1 1 d . . . H21A H 0.5980 0.4003 0.7320 0.131 Uiso 1 1 calc R . . H21B H 0.6746 0.3752 0.6717 0.131 Uiso 1 1 calc R . . H21C H 0.5278 0.3527 0.6913 0.131 Uiso 1 1 calc R . . C22 C 0.6101(7) 0.4991(3) 0.6346(4) 0.098(2) Uani 1 1 d . . . H22A H 0.5637 0.5278 0.6102 0.146 Uiso 1 1 calc R . . H22B H 0.6979 0.4910 0.6149 0.146 Uiso 1 1 calc R . . H22C H 0.6262 0.5108 0.6792 0.146 Uiso 1 1 calc R . . C23 C 0.1864(8) 0.4913(4) 0.5419(3) 0.115(3) Uani 1 1 d . . . H23A H 0.2706 0.5016 0.5202 0.172 Uiso 1 1 calc R . . H23B H 0.1126 0.5163 0.5295 0.172 Uiso 1 1 calc R . . H23C H 0.1603 0.4548 0.5291 0.172 Uiso 1 1 calc R . . C24 C 0.2603(8) 0.5667(3) 0.6531(5) 0.116(3) Uani 1 1 d . . . H24A H 0.2634 0.5710 0.7001 0.174 Uiso 1 1 calc R . . H24B H 0.1901 0.5905 0.6344 0.174 Uiso 1 1 calc R . . H24C H 0.3497 0.5758 0.6357 0.174 Uiso 1 1 calc R . . C25 C 0.0444(6) 0.4788(3) 0.6721(4) 0.088(2) Uani 1 1 d . . . H25A H 0.0230 0.4405 0.6674 0.131 Uiso 1 1 calc R . . H25B H -0.0284 0.5001 0.6512 0.131 Uiso 1 1 calc R . . H25C H 0.0510 0.4880 0.7180 0.131 Uiso 1 1 calc R . . C26 C 0.4679(6) 0.4659(3) 0.8360(3) 0.088(2) Uani 1 1 d . . . H26A H 0.5005 0.4287 0.8382 0.132 Uiso 1 1 calc R . . H26B H 0.5380 0.4898 0.8546 0.132 Uiso 1 1 calc R . . H26C H 0.4495 0.4758 0.7909 0.132 Uiso 1 1 calc R . . C27 C 0.2658(8) 0.5473(3) 0.8898(4) 0.106(3) Uani 1 1 d . . . H27A H 0.2408 0.5614 0.8470 0.159 Uiso 1 1 calc R . . H27B H 0.3474 0.5660 0.9066 0.159 Uiso 1 1 calc R . . H27C H 0.1897 0.5529 0.9191 0.159 Uiso 1 1 calc R . . C28 C 0.3464(9) 0.4458(3) 0.9683(3) 0.107(3) Uani 1 1 d . . . H28A H 0.2729 0.4556 0.9974 0.161 Uiso 1 1 calc R . . H28B H 0.4329 0.4616 0.9839 0.161 Uiso 1 1 calc R . . H28C H 0.3553 0.4067 0.9669 0.161 Uiso 1 1 calc R . . C29 C -0.0896(8) 0.4881(4) 0.8822(5) 0.137(4) Uani 1 1 d . . . H29A H -0.0348 0.5133 0.9084 0.205 Uiso 1 1 calc R . . H29B H -0.1744 0.4795 0.9044 0.205 Uiso 1 1 calc R . . H29C H -0.1121 0.5045 0.8404 0.205 Uiso 1 1 calc R . . C30 C 0.0051(8) 0.3826(4) 0.9468(4) 0.124(3) Uani 1 1 d . . . H30A H 0.0505 0.3480 0.9403 0.186 Uiso 1 1 calc R . . H30B H -0.0908 0.3765 0.9578 0.186 Uiso 1 1 calc R . . H30C H 0.0518 0.4020 0.9820 0.186 Uiso 1 1 calc R . . C31 C -0.0850(7) 0.3839(3) 0.8048(3) 0.088(2) Uani 1 1 d . . . H31A H -0.1057 0.4072 0.7677 0.131 Uiso 1 1 calc R . . H31B H -0.1707 0.3704 0.8223 0.131 Uiso 1 1 calc R . . H31C H -0.0285 0.3536 0.7911 0.131 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.04106(16) 0.04076(15) 0.04030(15) -0.00084(12) -0.00092(10) -0.00061(12) Si1 0.0891(13) 0.0603(11) 0.0733(11) -0.0121(9) 0.0242(10) 0.0190(9) Si2 0.0730(12) 0.0522(10) 0.1101(15) 0.0003(10) 0.0240(11) -0.0166(9) Si3 0.0418(8) 0.0689(10) 0.0572(8) 0.0099(8) 0.0067(7) -0.0009(7) Si4 0.0472(9) 0.0701(11) 0.0711(10) 0.0209(9) -0.0023(8) 0.0049(8) Si5 0.0635(10) 0.0614(10) 0.0514(8) -0.0090(7) -0.0032(7) -0.0081(8) Si6 0.0515(10) 0.0734(11) 0.0622(9) -0.0171(8) 0.0111(8) -0.0004(8) N1 0.040(2) 0.048(2) 0.046(2) -0.0104(19) -0.0042(18) -0.0008(19) N2 0.040(2) 0.044(2) 0.044(2) 0.0037(18) -0.0039(18) 0.0052(18) N3 0.053(3) 0.042(2) 0.056(2) -0.005(2) 0.007(2) -0.0026(19) N4 0.039(2) 0.057(3) 0.053(2) 0.009(2) 0.0016(19) -0.0015(19) N5 0.050(3) 0.055(3) 0.047(2) -0.012(2) 0.005(2) 0.000(2) C1 0.035(3) 0.043(3) 0.044(2) -0.002(2) 0.011(2) 0.001(2) C2 0.050(3) 0.056(3) 0.050(3) -0.014(2) -0.006(2) -0.003(2) C3 0.051(4) 0.127(6) 0.049(3) -0.008(4) -0.001(3) -0.010(4) C4 0.077(5) 0.173(9) 0.049(3) -0.014(4) -0.007(3) -0.015(5) C5 0.078(5) 0.154(8) 0.064(4) -0.016(5) -0.034(4) 0.004(5) C6 0.044(4) 0.149(7) 0.078(4) -0.035(5) -0.017(3) -0.013(4) C7 0.042(3) 0.105(5) 0.057(3) -0.017(3) -0.003(3) -0.004(3) C8 0.053(3) 0.052(3) 0.049(3) 0.004(2) -0.001(2) 0.011(2) C9 0.056(4) 0.148(7) 0.054(3) 0.013(4) 0.007(3) 0.020(4) C10 0.075(5) 0.232(11) 0.055(4) 0.055(5) 0.002(4) 0.016(6) C11 0.068(5) 0.182(9) 0.059(4) 0.019(5) -0.015(3) 0.037(5) C12 0.058(4) 0.160(8) 0.069(4) 0.035(5) -0.005(3) 0.031(4) C13 0.044(4) 0.131(6) 0.061(3) 0.028(4) -0.004(3) 0.015(4) C14 0.212(11) 0.164(10) 0.149(9) 0.055(8) 0.080(8) 0.142(9) C15 0.074(5) 0.120(7) 0.091(5) -0.025(5) 0.035(4) 0.005(4) C16 0.156(9) 0.149(9) 0.183(10) -0.113(8) 0.068(8) -0.039(7) C17 0.133(8) 0.156(10) 0.203(11) -0.066(8) 0.039(8) -0.093(7) C18 0.137(8) 0.091(7) 0.272(14) 0.097(8) 0.066(9) 0.018(6) C19 0.075(5) 0.104(6) 0.107(6) 0.016(5) 0.036(4) -0.006(4) C20 0.079(5) 0.137(7) 0.067(4) -0.006(4) 0.018(4) 0.000(4) C21 0.065(4) 0.113(6) 0.084(4) 0.026(4) 0.013(3) 0.035(4) C22 0.061(4) 0.112(6) 0.121(6) 0.004(5) 0.025(4) -0.028(4) C23 0.108(6) 0.151(8) 0.085(5) 0.042(5) -0.014(5) 0.023(6) C24 0.090(6) 0.062(5) 0.196(10) 0.009(5) -0.003(6) 0.003(4) C25 0.051(4) 0.097(6) 0.115(6) 0.021(4) 0.009(4) 0.015(3) C26 0.053(4) 0.115(6) 0.096(5) -0.020(4) -0.009(4) -0.011(4) C27 0.109(6) 0.055(4) 0.153(8) -0.034(5) -0.003(5) -0.008(4) C28 0.145(7) 0.116(7) 0.060(4) 0.008(4) -0.037(4) -0.038(5) C29 0.070(5) 0.124(8) 0.217(11) -0.066(7) 0.027(6) 0.035(5) C30 0.095(6) 0.199(10) 0.079(5) 0.021(6) 0.031(4) -0.039(6) C31 0.070(4) 0.101(6) 0.091(5) -0.013(4) -0.001(4) -0.028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N4 2.314(4) . ? Nd1 N5 2.322(4) . ? Nd1 N2 2.413(4) . ? Nd1 N1 2.423(4) . ? Nd1 C1 2.874(5) . ? Nd1 Si4 3.4027(16) . ? Nd1 Si5 3.4040(15) . ? Si1 N3 1.761(4) . ? Si1 C16 1.828(8) . ? Si1 C15 1.845(7) . ? Si1 C14 1.869(8) . ? Si2 N3 1.757(4) . ? Si2 C19 1.837(7) . ? Si2 C18 1.869(9) . ? Si2 C17 1.872(9) . ? Si3 N4 1.715(4) . ? Si3 C22 1.870(7) . ? Si3 C21 1.870(6) . ? Si3 C20 1.874(6) . ? Si4 N4 1.703(4) . ? Si4 C23 1.853(7) . ? Si4 C24 1.868(7) . ? Si4 C25 1.888(6) . ? Si5 N5 1.704(4) . ? Si5 C27 1.866(7) . ? Si5 C26 1.870(6) . ? Si5 C28 1.879(6) . ? Si6 N5 1.709(4) . ? Si6 C29 1.862(7) . ? Si6 C30 1.870(8) . ? Si6 C31 1.871(6) . ? N1 C1 1.342(6) . ? N1 C2 1.468(6) . ? N2 C1 1.337(6) . ? N2 C8 1.468(6) . ? N3 C1 1.420(6) . ? C2 C3 1.504(7) . ? C2 C7 1.513(7) . ? C2 H2 0.9800 . ? C3 C4 1.534(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.503(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.496(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.523(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.515(7) . ? C8 C13 1.525(7) . ? C8 H8 0.9800 . ? C9 C10 1.538(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.496(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.480(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.525(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 Nd1 N5 119.13(16) . . ? N4 Nd1 N2 127.96(14) . . ? N5 Nd1 N2 106.49(14) . . ? N4 Nd1 N1 106.30(14) . . ? N5 Nd1 N1 127.98(14) . . ? N2 Nd1 N1 55.29(14) . . ? N4 Nd1 C1 120.29(14) . . ? N5 Nd1 C1 120.58(14) . . ? N2 Nd1 C1 27.58(13) . . ? N1 Nd1 C1 27.71(12) . . ? N4 Nd1 Si4 26.99(10) . . ? N5 Nd1 Si4 103.42(11) . . ? N2 Nd1 Si4 150.00(10) . . ? N1 Nd1 Si4 106.43(10) . . ? C1 Nd1 Si4 130.42(10) . . ? N4 Nd1 Si5 103.62(11) . . ? N5 Nd1 Si5 27.07(11) . . ? N2 Nd1 Si5 106.43(10) . . ? N1 Nd1 Si5 150.00(10) . . ? C1 Nd1 Si5 130.43(10) . . ? Si4 Nd1 Si5 99.15(5) . . ? N3 Si1 C16 110.4(3) . . ? N3 Si1 C15 110.6(3) . . ? C16 Si1 C15 108.4(4) . . ? N3 Si1 C14 112.5(3) . . ? C16 Si1 C14 108.5(5) . . ? C15 Si1 C14 106.3(4) . . ? N3 Si2 C19 110.6(3) . . ? N3 Si2 C18 109.3(3) . . ? C19 Si2 C18 106.9(4) . . ? N3 Si2 C17 112.1(3) . . ? C19 Si2 C17 107.7(4) . . ? C18 Si2 C17 110.1(5) . . ? N4 Si3 C22 113.4(3) . . ? N4 Si3 C21 107.2(2) . . ? C22 Si3 C21 107.2(4) . . ? N4 Si3 C20 114.4(3) . . ? C22 Si3 C20 107.3(3) . . ? C21 Si3 C20 107.0(3) . . ? N4 Si4 C23 115.0(3) . . ? N4 Si4 C24 114.2(3) . . ? C23 Si4 C24 106.7(4) . . ? N4 Si4 C25 106.5(3) . . ? C23 Si4 C25 107.6(3) . . ? C24 Si4 C25 106.3(4) . . ? N4 Si4 Nd1 38.06(14) . . ? C23 Si4 Nd1 131.8(3) . . ? C24 Si4 Nd1 120.7(3) . . ? C25 Si4 Nd1 68.8(2) . . ? N5 Si5 C27 115.2(3) . . ? N5 Si5 C26 107.1(2) . . ? C27 Si5 C26 106.6(3) . . ? N5 Si5 C28 113.2(3) . . ? C27 Si5 C28 108.2(4) . . ? C26 Si5 C28 106.0(4) . . ? N5 Si5 Nd1 38.32(13) . . ? C27 Si5 Nd1 126.0(3) . . ? C26 Si5 Nd1 68.8(2) . . ? C28 Si5 Nd1 125.1(3) . . ? N5 Si6 C29 114.0(3) . . ? N5 Si6 C30 113.7(3) . . ? C29 Si6 C30 107.9(4) . . ? N5 Si6 C31 107.9(3) . . ? C29 Si6 C31 106.4(4) . . ? C30 Si6 C31 106.3(4) . . ? C1 N1 C2 122.8(4) . . ? C1 N1 Nd1 95.2(3) . . ? C2 N1 Nd1 139.9(3) . . ? C1 N2 C8 121.7(4) . . ? C1 N2 Nd1 95.7(3) . . ? C8 N2 Nd1 141.3(3) . . ? C1 N3 Si2 118.7(3) . . ? C1 N3 Si1 118.4(3) . . ? Si2 N3 Si1 122.9(3) . . ? Si4 N4 Si3 125.3(2) . . ? Si4 N4 Nd1 115.0(2) . . ? Si3 N4 Nd1 119.6(2) . . ? Si5 N5 Si6 125.2(2) . . ? Si5 N5 Nd1 114.6(2) . . ? Si6 N5 Nd1 120.1(2) . . ? N2 C1 N1 113.8(4) . . ? N2 C1 N3 123.5(4) . . ? N1 C1 N3 122.7(4) . . ? N2 C1 Nd1 56.7(2) . . ? N1 C1 Nd1 57.1(2) . . ? N3 C1 Nd1 179.7(3) . . ? N1 C2 C3 109.6(4) . . ? N1 C2 C7 111.0(4) . . ? C3 C2 C7 109.5(5) . . ? N1 C2 H2 108.9 . . ? C3 C2 H2 108.9 . . ? C7 C2 H2 108.9 . . ? C2 C3 C4 112.2(5) . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 110.9(6) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 111.0(6) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 110.9(5) . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C2 C7 C6 111.6(5) . . ? C2 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? C2 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N2 C8 C9 109.5(4) . . ? N2 C8 C13 110.9(4) . . ? C9 C8 C13 108.5(5) . . ? N2 C8 H8 109.3 . . ? C9 C8 H8 109.3 . . ? C13 C8 H8 109.3 . . ? C8 C9 C10 111.9(5) . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 110.5(6) . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C10 112.5(6) . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C13 112.2(5) . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 C8 112.0(5) . . ? C12 C13 H13A 109.2 . . ? C8 C13 H13A 109.2 . . ? C12 C13 H13B 109.2 . . ? C8 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si4 C25 H25A 109.5 . . ? Si4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si5 C26 H26A 109.5 . . ? Si5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si5 C27 H27A 109.5 . . ? Si5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si5 C28 H28A 109.5 . . ? Si5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si6 C29 H29A 109.5 . . ? Si6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si6 C30 H30A 109.5 . . ? Si6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si6 C31 H31A 109.5 . . ? Si6 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si6 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Nd1 Si4 N4 129.4(3) . . . . ? N2 Nd1 Si4 N4 -46.3(3) . . . . ? N1 Nd1 Si4 N4 -93.8(3) . . . . ? C1 Nd1 Si4 N4 -77.8(3) . . . . ? Si5 Nd1 Si4 N4 102.1(2) . . . . ? N4 Nd1 Si4 C23 77.3(4) . . . . ? N5 Nd1 Si4 C23 -153.4(4) . . . . ? N2 Nd1 Si4 C23 30.9(4) . . . . ? N1 Nd1 Si4 C23 -16.5(4) . . . . ? C1 Nd1 Si4 C23 -0.5(4) . . . . ? Si5 Nd1 Si4 C23 179.4(3) . . . . ? N4 Nd1 Si4 C24 -90.8(4) . . . . ? N5 Nd1 Si4 C24 38.6(3) . . . . ? N2 Nd1 Si4 C24 -137.1(3) . . . . ? N1 Nd1 Si4 C24 175.5(3) . . . . ? C1 Nd1 Si4 C24 -168.5(3) . . . . ? Si5 Nd1 Si4 C24 11.3(3) . . . . ? N4 Nd1 Si4 C25 172.3(4) . . . . ? N5 Nd1 Si4 C25 -58.3(3) . . . . ? N2 Nd1 Si4 C25 126.0(3) . . . . ? N1 Nd1 Si4 C25 78.6(3) . . . . ? C1 Nd1 Si4 C25 94.6(3) . . . . ? Si5 Nd1 Si4 C25 -85.6(3) . . . . ? N4 Nd1 Si5 N5 128.8(3) . . . . ? N2 Nd1 Si5 N5 -94.2(3) . . . . ? N1 Nd1 Si5 N5 -46.8(3) . . . . ? C1 Nd1 Si5 N5 -78.5(3) . . . . ? Si4 Nd1 Si5 N5 101.6(2) . . . . ? N4 Nd1 Si5 C27 42.9(3) . . . . ? N5 Nd1 Si5 C27 -85.9(4) . . . . ? N2 Nd1 Si5 C27 179.9(3) . . . . ? N1 Nd1 Si5 C27 -132.7(4) . . . . ? C1 Nd1 Si5 C27 -164.4(3) . . . . ? Si4 Nd1 Si5 C27 15.7(3) . . . . ? N4 Nd1 Si5 C26 -52.7(3) . . . . ? N5 Nd1 Si5 C26 178.5(4) . . . . ? N2 Nd1 Si5 C26 84.3(3) . . . . ? N1 Nd1 Si5 C26 131.8(3) . . . . ? C1 Nd1 Si5 C26 100.0(3) . . . . ? Si4 Nd1 Si5 C26 -79.8(3) . . . . ? N4 Nd1 Si5 C28 -147.7(3) . . . . ? N5 Nd1 Si5 C28 83.5(4) . . . . ? N2 Nd1 Si5 C28 -10.8(3) . . . . ? N1 Nd1 Si5 C28 36.7(4) . . . . ? C1 Nd1 Si5 C28 4.9(4) . . . . ? Si4 Nd1 Si5 C28 -174.9(3) . . . . ? N4 Nd1 N1 C1 125.0(3) . . . . ? N5 Nd1 N1 C1 -84.4(3) . . . . ? N2 Nd1 N1 C1 -0.2(2) . . . . ? Si4 Nd1 N1 C1 153.1(2) . . . . ? Si5 Nd1 N1 C1 -59.5(3) . . . . ? N4 Nd1 N1 C2 -37.4(5) . . . . ? N5 Nd1 N1 C2 113.2(5) . . . . ? N2 Nd1 N1 C2 -162.7(5) . . . . ? C1 Nd1 N1 C2 -162.4(6) . . . . ? Si4 Nd1 N1 C2 -9.3(5) . . . . ? Si5 Nd1 N1 C2 138.1(4) . . . . ? N4 Nd1 N2 C1 -83.6(3) . . . . ? N5 Nd1 N2 C1 125.4(3) . . . . ? N1 Nd1 N2 C1 0.2(2) . . . . ? Si4 Nd1 N2 C1 -59.0(4) . . . . ? Si5 Nd1 N2 C1 153.6(2) . . . . ? N4 Nd1 N2 C8 110.8(5) . . . . ? N5 Nd1 N2 C8 -40.2(5) . . . . ? N1 Nd1 N2 C8 -165.3(5) . . . . ? C1 Nd1 N2 C8 -165.6(7) . . . . ? Si4 Nd1 N2 C8 135.4(4) . . . . ? Si5 Nd1 N2 C8 -11.9(5) . . . . ? C19 Si2 N3 C1 -8.1(5) . . . . ? C18 Si2 N3 C1 -125.5(5) . . . . ? C17 Si2 N3 C1 112.2(5) . . . . ? C19 Si2 N3 Si1 172.2(3) . . . . ? C18 Si2 N3 Si1 54.7(5) . . . . ? C17 Si2 N3 Si1 -67.6(5) . . . . ? C16 Si1 N3 C1 -125.9(5) . . . . ? C15 Si1 N3 C1 -6.0(5) . . . . ? C14 Si1 N3 C1 112.7(6) . . . . ? C16 Si1 N3 Si2 53.8(5) . . . . ? C15 Si1 N3 Si2 173.8(3) . . . . ? C14 Si1 N3 Si2 -67.6(5) . . . . ? C23 Si4 N4 Si3 50.3(5) . . . . ? C24 Si4 N4 Si3 -73.5(4) . . . . ? C25 Si4 N4 Si3 169.5(3) . . . . ? Nd1 Si4 N4 Si3 176.9(5) . . . . ? C23 Si4 N4 Nd1 -126.6(3) . . . . ? C24 Si4 N4 Nd1 109.6(4) . . . . ? C25 Si4 N4 Nd1 -7.5(4) . . . . ? C22 Si3 N4 Si4 57.6(4) . . . . ? C21 Si3 N4 Si4 175.7(4) . . . . ? C20 Si3 N4 Si4 -65.9(4) . . . . ? C22 Si3 N4 Nd1 -125.6(3) . . . . ? C21 Si3 N4 Nd1 -7.5(4) . . . . ? C20 Si3 N4 Nd1 110.9(3) . . . . ? N5 Nd1 N4 Si4 -59.4(3) . . . . ? N2 Nd1 N4 Si4 152.7(2) . . . . ? N1 Nd1 N4 Si4 94.3(2) . . . . ? C1 Nd1 N4 Si4 120.5(2) . . . . ? Si5 Nd1 N4 Si4 -83.4(2) . . . . ? N5 Nd1 N4 Si3 123.5(2) . . . . ? N2 Nd1 N4 Si3 -24.4(3) . . . . ? N1 Nd1 N4 Si3 -82.8(3) . . . . ? C1 Nd1 N4 Si3 -56.6(3) . . . . ? Si4 Nd1 N4 Si3 -177.1(4) . . . . ? Si5 Nd1 N4 Si3 99.5(2) . . . . ? C27 Si5 N5 Si6 -66.2(5) . . . . ? C26 Si5 N5 Si6 175.5(4) . . . . ? C28 Si5 N5 Si6 59.0(5) . . . . ? Nd1 Si5 N5 Si6 176.9(5) . . . . ? C27 Si5 N5 Nd1 116.9(3) . . . . ? C26 Si5 N5 Nd1 -1.4(4) . . . . ? C28 Si5 N5 Nd1 -117.9(3) . . . . ? C29 Si6 N5 Si5 58.6(5) . . . . ? C30 Si6 N5 Si5 -65.7(5) . . . . ? C31 Si6 N5 Si5 176.6(4) . . . . ? C29 Si6 N5 Nd1 -124.7(4) . . . . ? C30 Si6 N5 Nd1 111.0(4) . . . . ? C31 Si6 N5 Nd1 -6.7(4) . . . . ? N4 Nd1 N5 Si5 -60.1(3) . . . . ? N2 Nd1 N5 Si5 93.9(2) . . . . ? N1 Nd1 N5 Si5 152.5(2) . . . . ? C1 Nd1 N5 Si5 119.9(2) . . . . ? Si4 Nd1 N5 Si5 -83.8(2) . . . . ? N4 Nd1 N5 Si6 122.8(2) . . . . ? N2 Nd1 N5 Si6 -83.1(3) . . . . ? N1 Nd1 N5 Si6 -24.6(3) . . . . ? C1 Nd1 N5 Si6 -57.1(3) . . . . ? Si4 Nd1 N5 Si6 99.1(2) . . . . ? Si5 Nd1 N5 Si6 -177.1(5) . . . . ? C8 N2 C1 N1 169.1(4) . . . . ? Nd1 N2 C1 N1 -0.4(4) . . . . ? C8 N2 C1 N3 -10.2(7) . . . . ? Nd1 N2 C1 N3 -179.7(4) . . . . ? C8 N2 C1 Nd1 169.4(5) . . . . ? C2 N1 C1 N2 167.0(4) . . . . ? Nd1 N1 C1 N2 0.4(4) . . . . ? C2 N1 C1 N3 -13.7(7) . . . . ? Nd1 N1 C1 N3 179.7(4) . . . . ? C2 N1 C1 Nd1 166.6(5) . . . . ? Si2 N3 C1 N2 100.9(5) . . . . ? Si1 N3 C1 N2 -79.3(5) . . . . ? Si2 N3 C1 N1 -78.3(5) . . . . ? Si1 N3 C1 N1 101.5(5) . . . . ? Si2 N3 C1 Nd1 -16(62) . . . . ? Si1 N3 C1 Nd1 164(100) . . . . ? N4 Nd1 C1 N2 114.8(3) . . . . ? N5 Nd1 C1 N2 -65.2(3) . . . . ? N1 Nd1 C1 N2 -179.6(4) . . . . ? Si4 Nd1 C1 N2 145.7(2) . . . . ? Si5 Nd1 C1 N2 -34.0(3) . . . . ? N4 Nd1 C1 N1 -65.6(3) . . . . ? N5 Nd1 C1 N1 114.3(3) . . . . ? N2 Nd1 C1 N1 179.6(4) . . . . ? Si4 Nd1 C1 N1 -34.7(3) . . . . ? Si5 Nd1 C1 N1 145.5(2) . . . . ? N4 Nd1 C1 N3 -128(62) . . . . ? N5 Nd1 C1 N3 52(62) . . . . ? N2 Nd1 C1 N3 117(62) . . . . ? N1 Nd1 C1 N3 -62(62) . . . . ? Si4 Nd1 C1 N3 -97(62) . . . . ? Si5 Nd1 C1 N3 83(62) . . . . ? C1 N1 C2 C3 -112.6(6) . . . . ? Nd1 N1 C2 C3 46.4(7) . . . . ? C1 N1 C2 C7 126.2(5) . . . . ? Nd1 N1 C2 C7 -74.7(6) . . . . ? N1 C2 C3 C4 -177.2(5) . . . . ? C7 C2 C3 C4 -55.1(7) . . . . ? C2 C3 C4 C5 55.4(9) . . . . ? C3 C4 C5 C6 -55.2(9) . . . . ? C4 C5 C6 C7 56.5(9) . . . . ? N1 C2 C7 C6 177.2(5) . . . . ? C3 C2 C7 C6 56.0(7) . . . . ? C5 C6 C7 C2 -57.4(9) . . . . ? C1 N2 C8 C9 -109.7(6) . . . . ? Nd1 N2 C8 C9 53.4(7) . . . . ? C1 N2 C8 C13 130.6(5) . . . . ? Nd1 N2 C8 C13 -66.4(6) . . . . ? N2 C8 C9 C10 -178.2(6) . . . . ? C13 C8 C9 C10 -57.0(8) . . . . ? C8 C9 C10 C11 56.8(10) . . . . ? C9 C10 C11 C12 -54.1(10) . . . . ? C10 C11 C12 C13 53.6(10) . . . . ? C11 C12 C13 C8 -54.7(9) . . . . ? N2 C8 C13 C12 175.9(5) . . . . ? C9 C8 C13 C12 55.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.430 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.072 data_[(SiMe3)2NC(NCy)2]Lu[N(SiMe3)2]2 _database_code_depnum_ccdc_archive 'CCDC 803566' #TrackingRef 'ccdc.doc' #TrackingRef 'ccdc.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H76 Lu N5 Si6' _chemical_formula_sum 'C31 H76 Lu N5 Si6' _chemical_formula_weight 862.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6391(14) _cell_length_b 24.143(4) _cell_length_c 20.157(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.219(3) _cell_angle_gamma 90.00 _cell_volume 4689.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16249 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 2.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.295 _exptl_absorpt_correction_T_max 0.528 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43812 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.34 _reflns_number_total 8565 _reflns_number_gt 7403 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0293P)^2^+4.5082P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8565 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.173 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.248779(18) 0.391229(7) 0.746388(7) 0.03850(7) Uani 1 1 d . . . Si1 Si 0.37532(17) 0.18877(6) 0.68183(7) 0.0700(4) Uani 1 1 d . . . Si2 Si 0.10057(17) 0.18357(6) 0.75804(9) 0.0757(4) Uani 1 1 d . . . Si3 Si 0.49158(14) 0.43679(6) 0.63472(6) 0.0547(3) Uani 1 1 d . . . Si4 Si 0.21198(14) 0.49147(6) 0.63760(7) 0.0556(3) Uani 1 1 d . . . Si5 Si 0.30240(15) 0.47076(6) 0.87876(6) 0.0572(3) Uani 1 1 d . . . Si6 Si 0.01661(15) 0.42220(6) 0.86782(7) 0.0600(4) Uani 1 1 d . . . N1 N 0.1610(3) 0.31392(13) 0.69657(16) 0.0411(8) Uani 1 1 d . . . N2 N 0.3287(3) 0.30582(14) 0.77495(15) 0.0412(8) Uani 1 1 d . . . N3 N 0.2394(4) 0.22128(14) 0.72441(17) 0.0474(8) Uani 1 1 d . . . N4 N 0.3291(3) 0.44380(14) 0.66747(16) 0.0435(8) Uani 1 1 d . . . N5 N 0.1787(4) 0.43177(15) 0.83743(16) 0.0481(9) Uani 1 1 d . . . C1 C 0.2430(4) 0.27992(17) 0.73235(19) 0.0405(9) Uani 1 1 d . . . C2 C 0.0859(4) 0.29549(19) 0.6361(2) 0.0479(11) Uani 1 1 d . . . H2 H 0.0968 0.2553 0.6319 0.057 Uiso 1 1 calc R . . C3 C 0.1466(5) 0.3227(2) 0.5756(2) 0.0669(14) Uani 1 1 d . . . H3A H 0.2432 0.3120 0.5722 0.080 Uiso 1 1 calc R . . H3B H 0.1432 0.3626 0.5809 0.080 Uiso 1 1 calc R . . C4 C 0.0689(6) 0.3067(3) 0.5114(2) 0.092(2) Uani 1 1 d . . . H4A H 0.1075 0.3269 0.4744 0.110 Uiso 1 1 calc R . . H4B H 0.0809 0.2675 0.5032 0.110 Uiso 1 1 calc R . . C5 C -0.0833(6) 0.3197(3) 0.5159(3) 0.094(2) Uani 1 1 d . . . H5A H -0.0958 0.3595 0.5190 0.113 Uiso 1 1 calc R . . H5B H -0.1313 0.3070 0.4760 0.113 Uiso 1 1 calc R . . C6 C -0.1451(5) 0.2923(3) 0.5754(3) 0.0843(18) Uani 1 1 d . . . H6A H -0.1414 0.2524 0.5700 0.101 Uiso 1 1 calc R . . H6B H -0.2417 0.3030 0.5785 0.101 Uiso 1 1 calc R . . C7 C -0.0672(5) 0.3086(2) 0.6392(2) 0.0638(14) Uani 1 1 d . . . H7A H -0.0790 0.3479 0.6469 0.077 Uiso 1 1 calc R . . H7B H -0.1066 0.2889 0.6763 0.077 Uiso 1 1 calc R . . C8 C 0.4034(4) 0.27551(19) 0.82801(19) 0.0480(11) Uani 1 1 d . . . H8 H 0.3962 0.2357 0.8188 0.058 Uiso 1 1 calc R . . C9 C 0.3382(6) 0.2871(3) 0.8946(2) 0.0827(18) Uani 1 1 d . . . H9A H 0.2419 0.2755 0.8931 0.099 Uiso 1 1 calc R . . H9B H 0.3405 0.3267 0.9032 0.099 Uiso 1 1 calc R . . C10 C 0.4152(6) 0.2566(4) 0.9508(3) 0.115(3) Uani 1 1 d . . . H10A H 0.3742 0.2662 0.9928 0.137 Uiso 1 1 calc R . . H10B H 0.4051 0.2170 0.9444 0.137 Uiso 1 1 calc R . . C11 C 0.5660(6) 0.2713(3) 0.9529(3) 0.102(2) Uani 1 1 d . . . H11A H 0.6130 0.2493 0.9868 0.123 Uiso 1 1 calc R . . H11B H 0.5764 0.3100 0.9649 0.123 Uiso 1 1 calc R . . C12 C 0.6326(6) 0.2613(3) 0.8874(3) 0.094(2) Uani 1 1 d . . . H12A H 0.6337 0.2218 0.8783 0.113 Uiso 1 1 calc R . . H12B H 0.7279 0.2742 0.8896 0.113 Uiso 1 1 calc R . . C13 C 0.5547(5) 0.2913(3) 0.8310(2) 0.0738(16) Uani 1 1 d . . . H13A H 0.5629 0.3310 0.8374 0.089 Uiso 1 1 calc R . . H13B H 0.5969 0.2821 0.7891 0.089 Uiso 1 1 calc R . . C14 C 0.4932(8) 0.1466(3) 0.7372(4) 0.135(3) Uani 1 1 d . . . H14A H 0.5157 0.1673 0.7766 0.203 Uiso 1 1 calc R . . H14B H 0.5768 0.1381 0.7142 0.203 Uiso 1 1 calc R . . H14C H 0.4474 0.1128 0.7490 0.203 Uiso 1 1 calc R . . C15 C 0.4856(6) 0.2413(3) 0.6427(3) 0.0905(19) Uani 1 1 d . . . H15A H 0.4281 0.2675 0.6192 0.136 Uiso 1 1 calc R . . H15B H 0.5466 0.2236 0.6123 0.136 Uiso 1 1 calc R . . H15C H 0.5394 0.2602 0.6763 0.136 Uiso 1 1 calc R . . C16 C 0.3021(8) 0.1435(3) 0.6156(4) 0.138(3) Uani 1 1 d . . . H16A H 0.2487 0.1145 0.6353 0.207 Uiso 1 1 calc R . . H16B H 0.3763 0.1276 0.5910 0.207 Uiso 1 1 calc R . . H16C H 0.2435 0.1650 0.5864 0.207 Uiso 1 1 calc R . . C17 C -0.0209(8) 0.1553(3) 0.6931(4) 0.145(3) Uani 1 1 d . . . H17A H -0.0920 0.1820 0.6832 0.218 Uiso 1 1 calc R . . H17B H -0.0627 0.1219 0.7091 0.218 Uiso 1 1 calc R . . H17C H 0.0294 0.1473 0.6537 0.218 Uiso 1 1 calc R . . C18 C 0.1723(9) 0.1250(3) 0.8085(5) 0.169(4) Uani 1 1 d . . . H18A H 0.2099 0.0975 0.7796 0.253 Uiso 1 1 calc R . . H18B H 0.0996 0.1089 0.8340 0.253 Uiso 1 1 calc R . . H18C H 0.2441 0.1386 0.8380 0.253 Uiso 1 1 calc R . . C19 C -0.0033(6) 0.2276(3) 0.8125(3) 0.095(2) Uani 1 1 d . . . H19A H 0.0574 0.2494 0.8404 0.142 Uiso 1 1 calc R . . H19B H -0.0606 0.2047 0.8396 0.142 Uiso 1 1 calc R . . H19C H -0.0610 0.2517 0.7859 0.142 Uiso 1 1 calc R . . C20 C 0.4918(6) 0.4053(3) 0.5500(3) 0.0860(18) Uani 1 1 d . . . H20A H 0.4552 0.3683 0.5519 0.129 Uiso 1 1 calc R . . H20B H 0.5851 0.4041 0.5343 0.129 Uiso 1 1 calc R . . H20C H 0.4353 0.4272 0.5203 0.129 Uiso 1 1 calc R . . C21 C 0.5973(6) 0.3899(3) 0.6884(3) 0.092(2) Uani 1 1 d . . . H21A H 0.6264 0.4093 0.7279 0.137 Uiso 1 1 calc R . . H21B H 0.6774 0.3779 0.6649 0.137 Uiso 1 1 calc R . . H21C H 0.5427 0.3583 0.7003 0.137 Uiso 1 1 calc R . . C22 C 0.5890(7) 0.5036(3) 0.6312(3) 0.099(2) Uani 1 1 d . . . H22A H 0.5386 0.5294 0.6037 0.149 Uiso 1 1 calc R . . H22B H 0.6788 0.4972 0.6130 0.149 Uiso 1 1 calc R . . H22C H 0.5997 0.5185 0.6752 0.149 Uiso 1 1 calc R . . C23 C 0.1893(6) 0.4923(3) 0.5453(3) 0.092(2) Uani 1 1 d . . . H23A H 0.2735 0.5048 0.5255 0.139 Uiso 1 1 calc R . . H23B H 0.1147 0.5168 0.5330 0.139 Uiso 1 1 calc R . . H23C H 0.1680 0.4556 0.5298 0.139 Uiso 1 1 calc R . . C24 C 0.2516(7) 0.5646(2) 0.6630(4) 0.100(2) Uani 1 1 d . . . H24A H 0.2569 0.5669 0.7106 0.150 Uiso 1 1 calc R . . H24B H 0.1795 0.5886 0.6465 0.150 Uiso 1 1 calc R . . H24C H 0.3387 0.5756 0.6450 0.150 Uiso 1 1 calc R . . C25 C 0.0400(5) 0.4743(3) 0.6740(3) 0.0804(17) Uani 1 1 d . . . H25A H 0.0195 0.4358 0.6664 0.121 Uiso 1 1 calc R . . H25B H -0.0309 0.4967 0.6534 0.121 Uiso 1 1 calc R . . H25C H 0.0434 0.4814 0.7209 0.121 Uiso 1 1 calc R . . C26 C 0.4685(6) 0.4646(3) 0.8337(3) 0.098(2) Uani 1 1 d . . . H26A H 0.4899 0.4262 0.8271 0.148 Uiso 1 1 calc R . . H26B H 0.5418 0.4818 0.8594 0.148 Uiso 1 1 calc R . . H26C H 0.4595 0.4828 0.7915 0.148 Uiso 1 1 calc R . . C27 C 0.2618(7) 0.5461(2) 0.8836(4) 0.105(2) Uani 1 1 d . . . H27A H 0.2395 0.5598 0.8399 0.157 Uiso 1 1 calc R . . H27B H 0.3408 0.5656 0.9014 0.157 Uiso 1 1 calc R . . H27C H 0.1840 0.5516 0.9118 0.157 Uiso 1 1 calc R . . C28 C 0.3390(8) 0.4470(3) 0.9660(3) 0.113(3) Uani 1 1 d . . . H28A H 0.2706 0.4621 0.9948 0.170 Uiso 1 1 calc R . . H28B H 0.4295 0.4595 0.9801 0.170 Uiso 1 1 calc R . . H28C H 0.3357 0.4073 0.9677 0.170 Uiso 1 1 calc R . . C29 C -0.0775(7) 0.4877(3) 0.8825(4) 0.135(3) Uani 1 1 d . . . H29A H -0.0270 0.5095 0.9147 0.202 Uiso 1 1 calc R . . H29B H -0.1682 0.4796 0.8986 0.202 Uiso 1 1 calc R . . H29C H -0.0859 0.5080 0.8416 0.202 Uiso 1 1 calc R . . C30 C 0.0125(8) 0.3806(4) 0.9460(3) 0.124(3) Uani 1 1 d . . . H30A H 0.0537 0.3450 0.9386 0.186 Uiso 1 1 calc R . . H30B H -0.0820 0.3758 0.9591 0.186 Uiso 1 1 calc R . . H30C H 0.0635 0.3996 0.9805 0.186 Uiso 1 1 calc R . . C31 C -0.0904(7) 0.3827(3) 0.8069(3) 0.092(2) Uani 1 1 d . . . H31A H -0.1243 0.4072 0.7727 0.138 Uiso 1 1 calc R . . H31B H -0.1675 0.3662 0.8289 0.138 Uiso 1 1 calc R . . H31C H -0.0351 0.3542 0.7874 0.138 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.04625(12) 0.03715(11) 0.03209(11) -0.00020(7) 0.00028(8) -0.00126(8) Si1 0.0873(11) 0.0593(9) 0.0640(9) -0.0117(7) 0.0185(8) 0.0214(8) Si2 0.0757(10) 0.0516(9) 0.1004(12) 0.0051(8) 0.0176(9) -0.0162(8) Si3 0.0497(8) 0.0653(9) 0.0496(7) 0.0092(6) 0.0091(6) -0.0009(7) Si4 0.0519(8) 0.0563(8) 0.0583(8) 0.0138(6) -0.0025(6) 0.0028(6) Si5 0.0690(9) 0.0564(8) 0.0460(7) -0.0064(6) -0.0024(6) -0.0036(7) Si6 0.0574(8) 0.0704(9) 0.0526(8) -0.0144(7) 0.0115(6) 0.0032(7) N1 0.0433(19) 0.0390(19) 0.0409(18) -0.0087(15) -0.0024(15) -0.0001(16) N2 0.044(2) 0.0414(19) 0.0377(18) 0.0007(15) 0.0003(15) -0.0001(16) N3 0.052(2) 0.039(2) 0.051(2) -0.0017(16) 0.0076(17) 0.0009(17) N4 0.046(2) 0.044(2) 0.0412(18) 0.0079(15) 0.0057(15) -0.0041(16) N5 0.055(2) 0.049(2) 0.0406(19) -0.0066(16) 0.0037(16) 0.0051(18) C1 0.047(2) 0.039(2) 0.036(2) 0.0005(17) 0.0130(19) 0.0015(19) C2 0.048(3) 0.052(3) 0.043(2) -0.009(2) -0.006(2) -0.004(2) C3 0.052(3) 0.103(4) 0.045(3) -0.006(3) -0.002(2) -0.003(3) C4 0.078(4) 0.156(6) 0.041(3) -0.013(3) -0.005(3) -0.016(4) C5 0.078(4) 0.141(6) 0.062(4) -0.014(4) -0.027(3) -0.001(4) C6 0.052(3) 0.132(5) 0.069(4) -0.020(4) -0.013(3) -0.009(3) C7 0.048(3) 0.094(4) 0.049(3) -0.010(3) -0.005(2) -0.008(3) C8 0.051(3) 0.051(3) 0.041(2) 0.007(2) -0.001(2) 0.009(2) C9 0.067(4) 0.132(5) 0.049(3) 0.018(3) 0.009(3) 0.012(4) C10 0.082(4) 0.210(8) 0.052(3) 0.053(4) 0.005(3) 0.026(5) C11 0.084(4) 0.173(7) 0.049(3) 0.020(4) -0.013(3) 0.027(5) C12 0.062(3) 0.158(6) 0.062(3) 0.039(4) -0.004(3) 0.025(4) C13 0.050(3) 0.114(5) 0.057(3) 0.024(3) 0.000(2) 0.014(3) C14 0.156(7) 0.127(7) 0.125(6) 0.025(5) 0.035(6) 0.097(6) C15 0.078(4) 0.115(5) 0.079(4) -0.020(4) 0.029(3) -0.001(4) C16 0.150(7) 0.123(6) 0.142(7) -0.086(6) 0.040(6) -0.018(5) C17 0.125(7) 0.144(8) 0.167(8) -0.041(6) 0.010(6) -0.078(6) C18 0.143(8) 0.089(5) 0.276(12) 0.098(7) 0.050(8) 0.006(5) C19 0.074(4) 0.108(5) 0.104(5) 0.011(4) 0.042(4) -0.014(4) C20 0.082(4) 0.119(5) 0.058(3) -0.003(3) 0.023(3) 0.000(4) C21 0.077(4) 0.121(6) 0.078(4) 0.018(4) 0.013(3) 0.042(4) C22 0.086(4) 0.098(5) 0.115(5) 0.002(4) 0.026(4) -0.032(4) C23 0.093(4) 0.113(5) 0.070(4) 0.033(4) -0.012(3) 0.019(4) C24 0.099(5) 0.059(4) 0.141(6) 0.002(4) -0.011(4) 0.007(3) C25 0.050(3) 0.093(4) 0.098(4) 0.013(3) 0.011(3) 0.013(3) C26 0.064(4) 0.138(6) 0.093(5) -0.021(4) -0.008(3) 0.000(4) C27 0.116(5) 0.055(4) 0.144(6) -0.025(4) -0.001(5) -0.008(4) C28 0.158(7) 0.124(6) 0.056(3) 0.008(4) -0.038(4) -0.047(5) C29 0.074(5) 0.114(6) 0.217(9) -0.061(6) 0.036(5) 0.023(4) C30 0.099(5) 0.203(9) 0.072(4) 0.033(5) 0.029(4) -0.017(5) C31 0.093(5) 0.103(5) 0.081(4) -0.016(3) 0.010(4) -0.037(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 N4 2.189(3) . ? Lu1 N5 2.199(3) . ? Lu1 N2 2.271(3) . ? Lu1 N1 2.274(3) . ? Lu1 C1 2.703(4) . ? Lu1 Si4 3.2799(13) . ? Lu1 Si5 3.3189(13) . ? Si1 N3 1.765(4) . ? Si1 C15 1.842(6) . ? Si1 C16 1.853(7) . ? Si1 C14 1.876(6) . ? Si2 N3 1.766(4) . ? Si2 C19 1.840(6) . ? Si2 C18 1.866(7) . ? Si2 C17 1.867(7) . ? Si3 N4 1.721(4) . ? Si3 C21 1.856(6) . ? Si3 C22 1.868(6) . ? Si3 C20 1.869(6) . ? Si4 N4 1.713(4) . ? Si4 C23 1.870(5) . ? Si4 C25 1.873(5) . ? Si4 C24 1.875(6) . ? Si5 N5 1.720(4) . ? Si5 C27 1.863(6) . ? Si5 C26 1.863(6) . ? Si5 C28 1.875(5) . ? Si6 N5 1.706(4) . ? Si6 C29 1.850(6) . ? Si6 C31 1.852(6) . ? Si6 C30 1.870(6) . ? N1 C1 1.339(5) . ? N1 C2 1.474(5) . ? N2 C1 1.334(5) . ? N2 C8 1.472(5) . ? N3 C1 1.425(5) . ? C2 C7 1.511(6) . ? C2 C3 1.514(6) . ? C2 H2 0.9800 . ? C3 C4 1.530(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.505(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.503(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.528(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.508(6) . ? C8 C9 1.520(6) . ? C8 H8 0.9800 . ? C9 C10 1.529(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.496(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.500(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.531(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 Lu1 N5 117.91(14) . . ? N4 Lu1 N2 125.96(12) . . ? N5 Lu1 N2 107.53(12) . . ? N4 Lu1 N1 106.79(12) . . ? N5 Lu1 N1 128.01(13) . . ? N2 Lu1 N1 59.18(12) . . ? N4 Lu1 C1 120.48(12) . . ? N5 Lu1 C1 121.60(12) . . ? N2 Lu1 C1 29.52(12) . . ? N1 Lu1 C1 29.66(11) . . ? N4 Lu1 Si4 28.53(9) . . ? N5 Lu1 Si4 101.46(10) . . ? N2 Lu1 Si4 150.54(8) . . ? N1 Lu1 Si4 106.05(9) . . ? C1 Lu1 Si4 131.45(9) . . ? N4 Lu1 Si5 101.38(9) . . ? N5 Lu1 Si5 27.98(10) . . ? N2 Lu1 Si5 105.98(8) . . ? N1 Lu1 Si5 151.64(9) . . ? C1 Lu1 Si5 131.45(9) . . ? Si4 Lu1 Si5 97.09(4) . . ? N3 Si1 C15 110.0(2) . . ? N3 Si1 C16 109.7(3) . . ? C15 Si1 C16 108.2(3) . . ? N3 Si1 C14 113.5(3) . . ? C15 Si1 C14 106.3(3) . . ? C16 Si1 C14 108.9(4) . . ? N3 Si2 C19 111.0(2) . . ? N3 Si2 C18 109.0(3) . . ? C19 Si2 C18 108.2(4) . . ? N3 Si2 C17 112.9(3) . . ? C19 Si2 C17 106.8(4) . . ? C18 Si2 C17 108.9(4) . . ? N4 Si3 C21 109.2(2) . . ? N4 Si3 C22 113.1(2) . . ? C21 Si3 C22 106.2(3) . . ? N4 Si3 C20 114.2(2) . . ? C21 Si3 C20 105.9(3) . . ? C22 Si3 C20 107.8(3) . . ? N4 Si4 C23 114.8(2) . . ? N4 Si4 C25 107.2(2) . . ? C23 Si4 C25 107.8(3) . . ? N4 Si4 C24 114.1(2) . . ? C23 Si4 C24 106.3(3) . . ? C25 Si4 C24 106.2(3) . . ? N4 Si4 Lu1 37.63(11) . . ? C23 Si4 Lu1 133.0(2) . . ? C25 Si4 Lu1 70.03(18) . . ? C24 Si4 Lu1 119.6(2) . . ? N5 Si5 C27 114.5(3) . . ? N5 Si5 C26 108.4(2) . . ? C27 Si5 C26 106.6(3) . . ? N5 Si5 C28 113.7(2) . . ? C27 Si5 C28 106.6(3) . . ? C26 Si5 C28 106.6(3) . . ? N5 Si5 Lu1 36.84(12) . . ? C27 Si5 Lu1 125.2(2) . . ? C26 Si5 Lu1 71.5(2) . . ? C28 Si5 Lu1 126.8(2) . . ? N5 Si6 C29 113.4(3) . . ? N5 Si6 C31 109.5(2) . . ? C29 Si6 C31 106.1(3) . . ? N5 Si6 C30 114.3(3) . . ? C29 Si6 C30 107.8(4) . . ? C31 Si6 C30 105.1(3) . . ? C1 N1 C2 122.3(3) . . ? C1 N1 Lu1 93.2(2) . . ? C2 N1 Lu1 141.7(3) . . ? C1 N2 C8 121.4(4) . . ? C1 N2 Lu1 93.5(2) . . ? C8 N2 Lu1 142.5(3) . . ? C1 N3 Si1 118.7(3) . . ? C1 N3 Si2 119.0(3) . . ? Si1 N3 Si2 122.3(2) . . ? Si4 N4 Si3 122.00(19) . . ? Si4 N4 Lu1 113.84(17) . . ? Si3 N4 Lu1 124.10(18) . . ? Si6 N5 Si5 122.1(2) . . ? Si6 N5 Lu1 122.65(19) . . ? Si5 N5 Lu1 115.18(18) . . ? N2 C1 N1 114.2(4) . . ? N2 C1 N3 123.4(4) . . ? N1 C1 N3 122.4(4) . . ? N2 C1 Lu1 57.0(2) . . ? N1 C1 Lu1 57.2(2) . . ? N3 C1 Lu1 179.5(3) . . ? N1 C2 C7 111.4(3) . . ? N1 C2 C3 110.1(3) . . ? C7 C2 C3 109.7(4) . . ? N1 C2 H2 108.5 . . ? C7 C2 H2 108.5 . . ? C3 C2 H2 108.5 . . ? C2 C3 C4 112.4(4) . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 110.9(5) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C4 111.1(5) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 111.3(5) . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C2 C7 C6 111.9(4) . . ? C2 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? C2 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N2 C8 C13 111.2(4) . . ? N2 C8 C9 110.2(4) . . ? C13 C8 C9 109.6(4) . . ? N2 C8 H8 108.6 . . ? C13 C8 H8 108.6 . . ? C9 C8 H8 108.6 . . ? C8 C9 C10 111.2(5) . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 111.3(5) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 111.7(5) . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C11 C12 C13 111.5(5) . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C8 C13 C12 111.6(4) . . ? C8 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C8 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si4 C25 H25A 109.5 . . ? Si4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si5 C26 H26A 109.5 . . ? Si5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si5 C27 H27A 109.5 . . ? Si5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si5 C28 H28A 109.5 . . ? Si5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si6 C29 H29A 109.5 . . ? Si6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si6 C30 H30A 109.5 . . ? Si6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si6 C31 H31A 109.5 . . ? Si6 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si6 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Lu1 Si4 N4 128.8(2) . . . . ? N2 Lu1 Si4 N4 -40.8(3) . . . . ? N1 Lu1 Si4 N4 -95.8(2) . . . . ? C1 Lu1 Si4 N4 -78.0(2) . . . . ? Si5 Lu1 Si4 N4 100.81(19) . . . . ? N4 Lu1 Si4 C23 74.3(3) . . . . ? N5 Lu1 Si4 C23 -156.9(3) . . . . ? N2 Lu1 Si4 C23 33.5(3) . . . . ? N1 Lu1 Si4 C23 -21.5(3) . . . . ? C1 Lu1 Si4 C23 -3.7(3) . . . . ? Si5 Lu1 Si4 C23 175.1(3) . . . . ? N4 Lu1 Si4 C25 170.4(3) . . . . ? N5 Lu1 Si4 C25 -60.7(2) . . . . ? N2 Lu1 Si4 C25 129.6(3) . . . . ? N1 Lu1 Si4 C25 74.7(2) . . . . ? C1 Lu1 Si4 C25 92.4(2) . . . . ? Si5 Lu1 Si4 C25 -88.7(2) . . . . ? N4 Lu1 Si4 C24 -91.8(3) . . . . ? N5 Lu1 Si4 C24 37.0(3) . . . . ? N2 Lu1 Si4 C24 -132.7(3) . . . . ? N1 Lu1 Si4 C24 172.4(3) . . . . ? C1 Lu1 Si4 C24 -169.8(3) . . . . ? Si5 Lu1 Si4 C24 9.0(2) . . . . ? N4 Lu1 Si5 N5 129.7(2) . . . . ? N2 Lu1 Si5 N5 -97.4(2) . . . . ? N1 Lu1 Si5 N5 -43.6(3) . . . . ? C1 Lu1 Si5 N5 -80.1(2) . . . . ? Si4 Lu1 Si5 N5 101.1(2) . . . . ? N4 Lu1 Si5 C27 45.2(3) . . . . ? N5 Lu1 Si5 C27 -84.5(3) . . . . ? N2 Lu1 Si5 C27 178.1(3) . . . . ? N1 Lu1 Si5 C27 -128.1(3) . . . . ? C1 Lu1 Si5 C27 -164.5(3) . . . . ? Si4 Lu1 Si5 C27 16.6(3) . . . . ? N4 Lu1 Si5 C26 -52.5(3) . . . . ? N5 Lu1 Si5 C26 177.8(3) . . . . ? N2 Lu1 Si5 C26 80.4(3) . . . . ? N1 Lu1 Si5 C26 134.2(3) . . . . ? C1 Lu1 Si5 C26 97.8(3) . . . . ? Si4 Lu1 Si5 C26 -81.1(2) . . . . ? N4 Lu1 Si5 C28 -149.7(3) . . . . ? N5 Lu1 Si5 C28 80.6(4) . . . . ? N2 Lu1 Si5 C28 -16.8(3) . . . . ? N1 Lu1 Si5 C28 36.9(4) . . . . ? C1 Lu1 Si5 C28 0.5(3) . . . . ? Si4 Lu1 Si5 C28 -178.3(3) . . . . ? N4 Lu1 N1 C1 122.7(2) . . . . ? N5 Lu1 N1 C1 -88.4(3) . . . . ? N2 Lu1 N1 C1 0.4(2) . . . . ? Si4 Lu1 N1 C1 152.5(2) . . . . ? Si5 Lu1 N1 C1 -64.1(3) . . . . ? N4 Lu1 N1 C2 -36.4(4) . . . . ? N5 Lu1 N1 C2 112.6(4) . . . . ? N2 Lu1 N1 C2 -158.7(5) . . . . ? C1 Lu1 N1 C2 -159.1(6) . . . . ? Si4 Lu1 N1 C2 -6.6(4) . . . . ? Si5 Lu1 N1 C2 136.8(4) . . . . ? N4 Lu1 N2 C1 -89.5(3) . . . . ? N5 Lu1 N2 C1 123.9(2) . . . . ? N1 Lu1 N2 C1 -0.4(2) . . . . ? Si4 Lu1 N2 C1 -66.8(3) . . . . ? Si5 Lu1 N2 C1 153.1(2) . . . . ? N4 Lu1 N2 C8 110.8(4) . . . . ? N5 Lu1 N2 C8 -35.9(5) . . . . ? N1 Lu1 N2 C8 -160.2(5) . . . . ? C1 Lu1 N2 C8 -159.7(6) . . . . ? Si4 Lu1 N2 C8 133.5(4) . . . . ? Si5 Lu1 N2 C8 -6.7(4) . . . . ? C15 Si1 N3 C1 -9.5(4) . . . . ? C16 Si1 N3 C1 -128.4(4) . . . . ? C14 Si1 N3 C1 109.5(4) . . . . ? C15 Si1 N3 Si2 171.1(3) . . . . ? C16 Si1 N3 Si2 52.2(4) . . . . ? C14 Si1 N3 Si2 -69.9(4) . . . . ? C19 Si2 N3 C1 -10.5(4) . . . . ? C18 Si2 N3 C1 -129.5(5) . . . . ? C17 Si2 N3 C1 109.3(4) . . . . ? C19 Si2 N3 Si1 168.9(3) . . . . ? C18 Si2 N3 Si1 49.9(5) . . . . ? C17 Si2 N3 Si1 -71.3(4) . . . . ? C23 Si4 N4 Si3 48.0(3) . . . . ? C25 Si4 N4 Si3 167.8(3) . . . . ? C24 Si4 N4 Si3 -75.0(3) . . . . ? Lu1 Si4 N4 Si3 177.2(4) . . . . ? C23 Si4 N4 Lu1 -129.1(3) . . . . ? C25 Si4 N4 Lu1 -9.4(3) . . . . ? C24 Si4 N4 Lu1 107.8(3) . . . . ? C21 Si3 N4 Si4 170.7(3) . . . . ? C22 Si3 N4 Si4 52.7(4) . . . . ? C20 Si3 N4 Si4 -71.1(3) . . . . ? C21 Si3 N4 Lu1 -12.5(3) . . . . ? C22 Si3 N4 Lu1 -130.4(3) . . . . ? C20 Si3 N4 Lu1 105.8(3) . . . . ? N5 Lu1 N4 Si4 -59.8(2) . . . . ? N2 Lu1 N4 Si4 156.59(16) . . . . ? N1 Lu1 N4 Si4 92.83(19) . . . . ? C1 Lu1 N4 Si4 121.71(18) . . . . ? Si5 Lu1 N4 Si4 -83.87(18) . . . . ? N5 Lu1 N4 Si3 123.1(2) . . . . ? N2 Lu1 N4 Si3 -20.5(3) . . . . ? N1 Lu1 N4 Si3 -84.3(2) . . . . ? C1 Lu1 N4 Si3 -55.4(3) . . . . ? Si4 Lu1 N4 Si3 -177.1(4) . . . . ? Si5 Lu1 N4 Si3 99.0(2) . . . . ? C29 Si6 N5 Si5 57.4(4) . . . . ? C31 Si6 N5 Si5 175.7(3) . . . . ? C30 Si6 N5 Si5 -66.7(4) . . . . ? C29 Si6 N5 Lu1 -126.5(3) . . . . ? C31 Si6 N5 Lu1 -8.2(3) . . . . ? C30 Si6 N5 Lu1 109.4(3) . . . . ? C27 Si5 N5 Si6 -67.0(4) . . . . ? C26 Si5 N5 Si6 174.2(3) . . . . ? C28 Si5 N5 Si6 55.9(4) . . . . ? Lu1 Si5 N5 Si6 176.3(4) . . . . ? C27 Si5 N5 Lu1 116.7(3) . . . . ? C26 Si5 N5 Lu1 -2.2(3) . . . . ? C28 Si5 N5 Lu1 -120.5(3) . . . . ? N4 Lu1 N5 Si6 125.1(2) . . . . ? N2 Lu1 N5 Si6 -85.1(2) . . . . ? N1 Lu1 N5 Si6 -20.9(3) . . . . ? C1 Lu1 N5 Si6 -56.4(3) . . . . ? Si4 Lu1 N5 Si6 100.2(2) . . . . ? Si5 Lu1 N5 Si6 -176.3(4) . . . . ? N4 Lu1 N5 Si5 -58.6(2) . . . . ? N2 Lu1 N5 Si5 91.2(2) . . . . ? N1 Lu1 N5 Si5 155.41(16) . . . . ? C1 Lu1 N5 Si5 119.90(19) . . . . ? Si4 Lu1 N5 Si5 -83.50(18) . . . . ? C8 N2 C1 N1 166.4(3) . . . . ? Lu1 N2 C1 N1 0.7(3) . . . . ? C8 N2 C1 N3 -14.5(6) . . . . ? Lu1 N2 C1 N3 179.8(3) . . . . ? C8 N2 C1 Lu1 165.7(4) . . . . ? C2 N1 C1 N2 164.1(3) . . . . ? Lu1 N1 C1 N2 -0.7(3) . . . . ? C2 N1 C1 N3 -15.0(6) . . . . ? Lu1 N1 C1 N3 -179.8(3) . . . . ? C2 N1 C1 Lu1 164.8(4) . . . . ? Si1 N3 C1 N2 -74.2(5) . . . . ? Si2 N3 C1 N2 105.2(4) . . . . ? Si1 N3 C1 N1 104.8(4) . . . . ? Si2 N3 C1 N1 -75.8(4) . . . . ? Si1 N3 C1 Lu1 82(42) . . . . ? Si2 N3 C1 Lu1 -99(42) . . . . ? N4 Lu1 C1 N2 110.1(2) . . . . ? N5 Lu1 C1 N2 -68.4(3) . . . . ? N1 Lu1 C1 N2 179.2(4) . . . . ? Si4 Lu1 C1 N2 142.9(2) . . . . ? Si5 Lu1 C1 N2 -35.5(3) . . . . ? N4 Lu1 C1 N1 -69.1(3) . . . . ? N5 Lu1 C1 N1 112.4(2) . . . . ? N2 Lu1 C1 N1 -179.2(4) . . . . ? Si4 Lu1 C1 N1 -36.3(3) . . . . ? Si5 Lu1 C1 N1 145.2(2) . . . . ? N4 Lu1 C1 N3 -46(42) . . . . ? N5 Lu1 C1 N3 135(42) . . . . ? N2 Lu1 C1 N3 -156(100) . . . . ? N1 Lu1 C1 N3 23(42) . . . . ? Si4 Lu1 C1 N3 -13(42) . . . . ? Si5 Lu1 C1 N3 168(100) . . . . ? C1 N1 C2 C7 127.2(4) . . . . ? Lu1 N1 C2 C7 -77.8(5) . . . . ? C1 N1 C2 C3 -110.9(5) . . . . ? Lu1 N1 C2 C3 44.2(6) . . . . ? N1 C2 C3 C4 -177.9(4) . . . . ? C7 C2 C3 C4 -54.9(6) . . . . ? C2 C3 C4 C5 55.6(7) . . . . ? C3 C4 C5 C6 -55.3(7) . . . . ? C4 C5 C6 C7 55.8(7) . . . . ? N1 C2 C7 C6 177.2(4) . . . . ? C3 C2 C7 C6 55.0(6) . . . . ? C5 C6 C7 C2 -56.2(7) . . . . ? C1 N2 C8 C13 132.8(4) . . . . ? Lu1 N2 C8 C13 -71.1(6) . . . . ? C1 N2 C8 C9 -105.4(5) . . . . ? Lu1 N2 C8 C9 50.7(6) . . . . ? N2 C8 C9 C10 -179.3(5) . . . . ? C13 C8 C9 C10 -56.6(7) . . . . ? C8 C9 C10 C11 56.3(8) . . . . ? C9 C10 C11 C12 -54.8(9) . . . . ? C10 C11 C12 C13 54.2(8) . . . . ? N2 C8 C13 C12 178.3(5) . . . . ? C9 C8 C13 C12 56.2(6) . . . . ? C11 C12 C13 C8 -55.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.826 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.077 data_[(SiMe3)2NC(NCy)2]Y[N(SiMe3)2]2 _database_code_depnum_ccdc_archive 'CCDC 803567' #TrackingRef 'ccdc.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H76 N5 Si6 Y' _chemical_formula_weight 776.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5883(16) _cell_length_b 24.230(4) _cell_length_c 20.194(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.177(5) _cell_angle_gamma 90.00 _cell_volume 4690.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17962 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 1.421 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.396 _exptl_absorpt_correction_T_max 0.492 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44680 _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8574 _reflns_number_gt 6616 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0368P)^2^+7.8849P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8574 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1394 _refine_ls_R_factor_gt 0.1070 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1692 _refine_ls_goodness_of_fit_ref 1.272 _refine_ls_restrained_S_all 1.272 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.25004(6) 0.39212(2) 0.24648(3) 0.04750(19) Uani 1 1 d . . . Si1 Si 0.3737(2) 0.18813(9) 0.18146(11) 0.0791(6) Uani 1 1 d . . . Si2 Si 0.0992(2) 0.18354(9) 0.25803(13) 0.0842(7) Uani 1 1 d . . . Si3 Si 0.49337(19) 0.43715(8) 0.13450(9) 0.0623(5) Uani 1 1 d . . . Si4 Si 0.2132(2) 0.49275(8) 0.13593(10) 0.0655(5) Uani 1 1 d . . . Si5 Si 0.3036(2) 0.47118(8) 0.38037(9) 0.0653(5) Uani 1 1 d . . . Si6 Si 0.0153(2) 0.42275(9) 0.36832(10) 0.0694(6) Uani 1 1 d . . . N1 N 0.1628(5) 0.31324(19) 0.1960(2) 0.0476(12) Uani 1 1 d . . . N2 N 0.3263(5) 0.30472(19) 0.2757(2) 0.0492(12) Uani 1 1 d . . . N3 N 0.2385(5) 0.22076(19) 0.2246(2) 0.0524(12) Uani 1 1 d . . . N4 N 0.3299(5) 0.44507(19) 0.1656(2) 0.0510(12) Uani 1 1 d . . . N5 N 0.1794(5) 0.4328(2) 0.3394(2) 0.0557(13) Uani 1 1 d . . . C1 C 0.2417(6) 0.2793(2) 0.2323(3) 0.0474(14) Uani 1 1 d . . . C2 C 0.0884(6) 0.2951(3) 0.1356(3) 0.0561(16) Uani 1 1 d . . . H2 H 0.0994 0.2550 0.1315 0.067 Uiso 1 1 calc R . . C3 C 0.1482(7) 0.3221(3) 0.0751(3) 0.076(2) Uani 1 1 d . . . H3A H 0.2457 0.3119 0.0718 0.091 Uiso 1 1 calc R . . H3B H 0.1435 0.3619 0.0800 0.091 Uiso 1 1 calc R . . C4 C 0.0711(8) 0.3054(4) 0.0115(3) 0.100(3) Uani 1 1 d . . . H4A H 0.1112 0.3245 -0.0259 0.120 Uiso 1 1 calc R . . H4B H 0.0813 0.2660 0.0044 0.120 Uiso 1 1 calc R . . C5 C -0.0816(8) 0.3198(4) 0.0158(4) 0.101(3) Uani 1 1 d . . . H5A H -0.0919 0.3595 0.0195 0.122 Uiso 1 1 calc R . . H5B H -0.1302 0.3079 -0.0243 0.122 Uiso 1 1 calc R . . C6 C -0.1452(7) 0.2924(4) 0.0745(4) 0.098(3) Uani 1 1 d . . . H6A H -0.1430 0.2527 0.0688 0.118 Uiso 1 1 calc R . . H6B H -0.2420 0.3037 0.0777 0.118 Uiso 1 1 calc R . . C7 C -0.0660(7) 0.3080(3) 0.1386(3) 0.075(2) Uani 1 1 d . . . H7A H -0.0778 0.3472 0.1468 0.090 Uiso 1 1 calc R . . H7B H -0.1057 0.2881 0.1754 0.090 Uiso 1 1 calc R . . C8 C 0.4022(6) 0.2742(3) 0.3283(3) 0.0577(16) Uani 1 1 d . . . H8 H 0.3947 0.2346 0.3190 0.069 Uiso 1 1 calc R . . C9 C 0.5537(7) 0.2896(4) 0.3324(4) 0.083(2) Uani 1 1 d . . . H9A H 0.5615 0.3292 0.3390 0.100 Uiso 1 1 calc R . . H9B H 0.5967 0.2808 0.2906 0.100 Uiso 1 1 calc R . . C10 C 0.6323(8) 0.2605(4) 0.3876(4) 0.102(3) Uani 1 1 d . . . H10A H 0.6334 0.2211 0.3788 0.123 Uiso 1 1 calc R . . H10B H 0.7281 0.2734 0.3892 0.123 Uiso 1 1 calc R . . C11 C 0.5672(8) 0.2707(4) 0.4526(4) 0.110(3) Uani 1 1 d . . . H11A H 0.5772 0.3094 0.4641 0.132 Uiso 1 1 calc R . . H11B H 0.6154 0.2492 0.4865 0.132 Uiso 1 1 calc R . . C12 C 0.4158(9) 0.2557(5) 0.4512(4) 0.120(4) Uani 1 1 d . . . H12A H 0.3750 0.2655 0.4932 0.145 Uiso 1 1 calc R . . H12B H 0.4062 0.2162 0.4453 0.145 Uiso 1 1 calc R . . C13 C 0.3369(7) 0.2858(4) 0.3945(3) 0.090(3) Uani 1 1 d . . . H13A H 0.2403 0.2739 0.3932 0.109 Uiso 1 1 calc R . . H13B H 0.3383 0.3253 0.4029 0.109 Uiso 1 1 calc R . . C14 C 0.4866(8) 0.2402(4) 0.1437(4) 0.099(3) Uani 1 1 d . . . H14A H 0.4321 0.2627 0.1138 0.148 Uiso 1 1 calc R . . H14B H 0.5590 0.2221 0.1198 0.148 Uiso 1 1 calc R . . H14C H 0.5275 0.2630 0.1778 0.148 Uiso 1 1 calc R . . C15 C 0.2991(11) 0.1439(4) 0.1158(5) 0.152(5) Uani 1 1 d . . . H15A H 0.2543 0.1127 0.1354 0.228 Uiso 1 1 calc R . . H15B H 0.3722 0.1314 0.0877 0.228 Uiso 1 1 calc R . . H15C H 0.2320 0.1646 0.0901 0.228 Uiso 1 1 calc R . . C16 C 0.4894(12) 0.1446(4) 0.2365(5) 0.157(5) Uani 1 1 d . . . H16A H 0.5167 0.1655 0.2751 0.236 Uiso 1 1 calc R . . H16B H 0.5709 0.1340 0.2128 0.236 Uiso 1 1 calc R . . H16C H 0.4396 0.1122 0.2497 0.236 Uiso 1 1 calc R . . C17 C -0.0225(11) 0.1547(4) 0.1933(5) 0.153(5) Uani 1 1 d . . . H17A H -0.0960 0.1807 0.1842 0.230 Uiso 1 1 calc R . . H17B H -0.0617 0.1208 0.2089 0.230 Uiso 1 1 calc R . . H17C H 0.0278 0.1479 0.1535 0.230 Uiso 1 1 calc R . . C18 C -0.0046(8) 0.2280(4) 0.3118(4) 0.108(3) Uani 1 1 d . . . H18A H 0.0551 0.2443 0.3452 0.162 Uiso 1 1 calc R . . H18B H -0.0752 0.2064 0.3326 0.162 Uiso 1 1 calc R . . H18C H -0.0480 0.2567 0.2858 0.162 Uiso 1 1 calc R . . C19 C 0.1678(12) 0.1258(4) 0.3087(7) 0.176(6) Uani 1 1 d . . . H19A H 0.2114 0.0993 0.2806 0.264 Uiso 1 1 calc R . . H19B H 0.0925 0.1085 0.3315 0.264 Uiso 1 1 calc R . . H19C H 0.2351 0.1396 0.3405 0.264 Uiso 1 1 calc R . . C20 C 0.5935(9) 0.3885(4) 0.1891(4) 0.105(3) Uani 1 1 d . . . H20A H 0.6208 0.4070 0.2293 0.158 Uiso 1 1 calc R . . H20B H 0.6753 0.3762 0.1667 0.158 Uiso 1 1 calc R . . H20C H 0.5361 0.3573 0.1993 0.158 Uiso 1 1 calc R . . C21 C 0.5955(8) 0.5029(4) 0.1327(5) 0.111(3) Uani 1 1 d . . . H21A H 0.5447 0.5300 0.1073 0.166 Uiso 1 1 calc R . . H21B H 0.6840 0.4963 0.1128 0.166 Uiso 1 1 calc R . . H21C H 0.6101 0.5162 0.1771 0.166 Uiso 1 1 calc R . . C22 C 0.4945(8) 0.4064(4) 0.0494(3) 0.096(3) Uani 1 1 d . . . H22A H 0.4505 0.3708 0.0500 0.144 Uiso 1 1 calc R . . H22B H 0.5890 0.4024 0.0353 0.144 Uiso 1 1 calc R . . H22C H 0.4445 0.4301 0.0191 0.144 Uiso 1 1 calc R . . C23 C 0.1876(9) 0.4921(4) 0.0447(4) 0.109(3) Uani 1 1 d . . . H23A H 0.2708 0.5050 0.0241 0.163 Uiso 1 1 calc R . . H23B H 0.1109 0.5158 0.0326 0.163 Uiso 1 1 calc R . . H23C H 0.1678 0.4551 0.0302 0.163 Uiso 1 1 calc R . . C24 C 0.2540(9) 0.5655(3) 0.1598(5) 0.111(3) Uani 1 1 d . . . H24A H 0.2458 0.5697 0.2068 0.166 Uiso 1 1 calc R . . H24B H 0.1898 0.5900 0.1375 0.166 Uiso 1 1 calc R . . H24C H 0.3475 0.5743 0.1473 0.166 Uiso 1 1 calc R . . C25 C 0.0408(7) 0.4766(3) 0.1729(4) 0.091(2) Uani 1 1 d . . . H25A H 0.0186 0.4384 0.1655 0.136 Uiso 1 1 calc R . . H25B H -0.0301 0.4993 0.1527 0.136 Uiso 1 1 calc R . . H25C H 0.0453 0.4837 0.2197 0.136 Uiso 1 1 calc R . . C26 C 0.3422(10) 0.4465(4) 0.4665(4) 0.116(3) Uani 1 1 d . . . H26A H 0.2664 0.4562 0.4946 0.174 Uiso 1 1 calc R . . H26B H 0.4264 0.4635 0.4829 0.174 Uiso 1 1 calc R . . H26C H 0.3535 0.4072 0.4663 0.174 Uiso 1 1 calc R . . C27 C 0.2644(9) 0.5462(3) 0.3857(5) 0.111(3) Uani 1 1 d . . . H27A H 0.2387 0.5598 0.3426 0.166 Uiso 1 1 calc R . . H27B H 0.3455 0.5655 0.4020 0.166 Uiso 1 1 calc R . . H27C H 0.1888 0.5519 0.4154 0.166 Uiso 1 1 calc R . . C28 C 0.4688(8) 0.4650(4) 0.3340(4) 0.103(3) Uani 1 1 d . . . H28A H 0.4965 0.4269 0.3325 0.155 Uiso 1 1 calc R . . H28B H 0.5405 0.4862 0.3560 0.155 Uiso 1 1 calc R . . H28C H 0.4545 0.4786 0.2898 0.155 Uiso 1 1 calc R . . C29 C -0.0873(9) 0.3833(3) 0.3062(4) 0.098(3) Uani 1 1 d . . . H29A H -0.1162 0.4074 0.2708 0.147 Uiso 1 1 calc R . . H29B H -0.1680 0.3679 0.3267 0.147 Uiso 1 1 calc R . . H29C H -0.0310 0.3541 0.2889 0.147 Uiso 1 1 calc R . . C30 C -0.0819(9) 0.4881(4) 0.3825(6) 0.144(4) Uani 1 1 d . . . H30A H -0.0368 0.5086 0.4175 0.215 Uiso 1 1 calc R . . H30B H -0.1758 0.4797 0.3945 0.215 Uiso 1 1 calc R . . H30C H -0.0831 0.5097 0.3426 0.215 Uiso 1 1 calc R . . C31 C 0.0090(10) 0.3817(5) 0.4468(4) 0.132(4) Uani 1 1 d . . . H31A H 0.0603 0.3480 0.4416 0.199 Uiso 1 1 calc R . . H31B H -0.0863 0.3733 0.4565 0.199 Uiso 1 1 calc R . . H31C H 0.0496 0.4028 0.4825 0.199 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0524(3) 0.0479(3) 0.0422(3) -0.0004(3) -0.0002(2) -0.0014(3) Si1 0.0934(16) 0.0707(13) 0.0740(14) -0.0118(11) 0.0182(12) 0.0217(12) Si2 0.0843(15) 0.0596(13) 0.1094(18) 0.0041(12) 0.0184(13) -0.0162(11) Si3 0.0552(11) 0.0726(12) 0.0595(11) 0.0089(10) 0.0086(9) -0.0004(10) Si4 0.0592(11) 0.0660(12) 0.0711(12) 0.0160(10) -0.0031(10) 0.0018(10) Si5 0.0749(13) 0.0657(12) 0.0551(11) -0.0080(9) -0.0028(10) -0.0033(10) Si6 0.0671(13) 0.0792(14) 0.0624(12) -0.0151(10) 0.0112(10) 0.0003(11) N1 0.048(3) 0.053(3) 0.042(3) -0.006(2) -0.004(2) 0.002(2) N2 0.049(3) 0.055(3) 0.044(3) 0.001(2) -0.003(2) 0.003(2) N3 0.056(3) 0.044(3) 0.056(3) -0.004(2) 0.002(2) -0.001(2) N4 0.052(3) 0.054(3) 0.047(3) 0.004(2) 0.003(2) 0.001(2) N5 0.059(3) 0.055(3) 0.053(3) -0.006(2) 0.000(3) 0.002(3) C1 0.045(3) 0.045(3) 0.052(4) -0.005(3) 0.014(3) -0.005(3) C2 0.056(4) 0.055(4) 0.056(4) -0.010(3) -0.005(3) -0.001(3) C3 0.066(4) 0.110(6) 0.051(4) -0.004(4) -0.004(3) -0.012(4) C4 0.077(6) 0.175(9) 0.047(4) -0.014(5) -0.005(4) -0.010(6) C5 0.088(6) 0.151(8) 0.064(5) -0.015(5) -0.021(5) 0.001(6) C6 0.050(4) 0.155(8) 0.089(6) -0.027(6) -0.018(4) -0.010(5) C7 0.063(4) 0.107(6) 0.055(4) -0.011(4) -0.007(3) -0.011(4) C8 0.058(4) 0.057(4) 0.058(4) 0.003(3) 0.001(3) 0.008(3) C9 0.057(4) 0.122(7) 0.071(5) 0.016(5) -0.005(4) 0.016(4) C10 0.057(5) 0.173(9) 0.077(5) 0.040(6) -0.002(4) 0.031(5) C11 0.076(6) 0.186(10) 0.066(5) 0.016(6) -0.014(4) 0.035(6) C12 0.091(6) 0.209(11) 0.061(5) 0.049(6) 0.001(5) 0.027(7) C13 0.064(5) 0.146(8) 0.062(5) 0.016(5) 0.010(4) 0.015(5) C14 0.080(6) 0.130(7) 0.087(6) -0.018(5) 0.032(5) 0.006(5) C15 0.160(10) 0.141(9) 0.157(10) -0.093(8) 0.044(8) -0.025(8) C16 0.186(11) 0.153(10) 0.135(9) 0.041(8) 0.053(8) 0.121(9) C17 0.135(9) 0.155(10) 0.170(11) -0.054(8) 0.017(8) -0.074(8) C18 0.083(6) 0.119(7) 0.123(7) 0.011(6) 0.044(5) -0.016(5) C19 0.150(10) 0.099(8) 0.280(16) 0.103(9) 0.057(10) 0.006(7) C20 0.092(6) 0.131(8) 0.094(6) 0.025(5) 0.006(5) 0.051(6) C21 0.081(6) 0.119(7) 0.135(8) 0.005(6) 0.034(5) -0.031(5) C22 0.088(6) 0.138(8) 0.063(5) 0.003(5) 0.022(4) 0.003(5) C23 0.116(7) 0.132(8) 0.077(6) 0.030(5) -0.018(5) 0.017(6) C24 0.107(7) 0.064(5) 0.161(9) -0.003(5) -0.003(6) 0.001(5) C25 0.066(5) 0.095(6) 0.111(6) 0.011(5) 0.009(5) 0.011(4) C26 0.158(9) 0.125(7) 0.064(5) 0.019(5) -0.028(5) -0.050(7) C27 0.113(7) 0.067(5) 0.152(9) -0.026(5) -0.003(6) -0.018(5) C28 0.067(5) 0.138(8) 0.103(6) -0.024(6) -0.002(5) -0.009(5) C29 0.101(6) 0.108(7) 0.085(6) -0.016(5) 0.015(5) -0.039(5) C30 0.080(6) 0.107(7) 0.244(13) -0.059(8) 0.040(7) 0.025(6) C31 0.112(7) 0.210(12) 0.077(6) 0.032(7) 0.024(5) -0.019(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N4 2.225(5) . ? Y1 N5 2.237(5) . ? Y1 N2 2.313(5) . ? Y1 N1 2.314(4) . ? Y1 C1 2.749(6) . ? Y1 Si4 3.320(2) . ? Y1 Si5 3.3446(19) . ? Y1 Si6 3.449(2) . ? Si1 N3 1.764(5) . ? Si1 C14 1.837(8) . ? Si1 C15 1.838(9) . ? Si1 C16 1.877(9) . ? Si2 N3 1.758(5) . ? Si2 C18 1.838(8) . ? Si2 C19 1.847(10) . ? Si2 C17 1.870(10) . ? Si3 N4 1.711(5) . ? Si3 C20 1.866(7) . ? Si3 C21 1.872(8) . ? Si3 C22 1.875(7) . ? Si4 N4 1.708(5) . ? Si4 C23 1.854(8) . ? Si4 C24 1.867(8) . ? Si4 C25 1.870(7) . ? Si5 N5 1.710(5) . ? Si5 C27 1.859(8) . ? Si5 C28 1.862(8) . ? Si5 C26 1.869(7) . ? Si6 N5 1.707(5) . ? Si6 C29 1.844(7) . ? Si6 C30 1.862(8) . ? Si6 C31 1.873(8) . ? N1 C1 1.328(7) . ? N1 C2 1.468(7) . ? N2 C1 1.332(7) . ? N2 C8 1.473(7) . ? N3 C1 1.427(7) . ? C2 C3 1.511(8) . ? C2 C7 1.515(8) . ? C2 H2 0.9800 . ? C3 C4 1.523(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.509(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.499(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.534(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.501(9) . ? C8 C13 1.515(9) . ? C8 H8 0.9800 . ? C9 C10 1.509(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.487(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.496(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.544(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 Y1 N5 118.44(18) . . ? N4 Y1 N2 127.12(17) . . ? N5 Y1 N2 106.82(17) . . ? N4 Y1 N1 106.24(17) . . ? N5 Y1 N1 128.34(17) . . ? N2 Y1 N1 57.70(17) . . ? N4 Y1 C1 120.43(17) . . ? N5 Y1 C1 121.13(17) . . ? N2 Y1 C1 28.90(16) . . ? N1 Y1 C1 28.79(16) . . ? N4 Y1 Si4 27.92(12) . . ? N5 Y1 Si4 102.13(13) . . ? N2 Y1 Si4 150.78(12) . . ? N1 Y1 Si4 106.15(12) . . ? C1 Y1 Si4 131.13(13) . . ? N4 Y1 Si5 102.36(13) . . ? N5 Y1 Si5 27.57(13) . . ? N2 Y1 Si5 106.00(12) . . ? N1 Y1 Si5 151.27(12) . . ? C1 Y1 Si5 131.08(13) . . ? Si4 Y1 Si5 97.79(5) . . ? N4 Y1 Si6 129.71(13) . . ? N5 Y1 Si6 24.98(13) . . ? N2 Y1 Si6 102.85(12) . . ? N1 Y1 Si6 104.85(12) . . ? C1 Y1 Si6 105.67(12) . . ? Si4 Y1 Si6 105.05(5) . . ? Si5 Y1 Si6 52.53(5) . . ? N3 Si1 C14 110.0(3) . . ? N3 Si1 C15 109.8(4) . . ? C14 Si1 C15 108.9(4) . . ? N3 Si1 C16 113.0(3) . . ? C14 Si1 C16 106.6(5) . . ? C15 Si1 C16 108.4(5) . . ? N3 Si2 C18 110.6(3) . . ? N3 Si2 C19 109.7(4) . . ? C18 Si2 C19 107.9(5) . . ? N3 Si2 C17 113.0(4) . . ? C18 Si2 C17 107.1(5) . . ? C19 Si2 C17 108.4(6) . . ? N4 Si3 C20 108.6(3) . . ? N4 Si3 C21 113.3(3) . . ? C20 Si3 C21 106.6(4) . . ? N4 Si3 C22 113.8(3) . . ? C20 Si3 C22 106.2(4) . . ? C21 Si3 C22 108.0(4) . . ? N4 Si4 C23 114.5(3) . . ? N4 Si4 C24 114.6(3) . . ? C23 Si4 C24 106.7(4) . . ? N4 Si4 C25 107.2(3) . . ? C23 Si4 C25 107.2(4) . . ? C24 Si4 C25 106.1(4) . . ? N4 Si4 Y1 37.59(16) . . ? C23 Si4 Y1 132.2(3) . . ? C24 Si4 Y1 120.1(3) . . ? C25 Si4 Y1 70.1(2) . . ? N5 Si5 C27 114.8(3) . . ? N5 Si5 C28 107.7(3) . . ? C27 Si5 C28 106.5(4) . . ? N5 Si5 C26 113.5(3) . . ? C27 Si5 C26 107.1(4) . . ? C28 Si5 C26 106.7(4) . . ? N5 Si5 Y1 37.26(17) . . ? C27 Si5 Y1 125.4(3) . . ? C28 Si5 Y1 70.5(3) . . ? C26 Si5 Y1 126.4(3) . . ? N5 Si6 C29 108.9(3) . . ? N5 Si6 C30 113.5(4) . . ? C29 Si6 C30 106.4(5) . . ? N5 Si6 C31 114.3(4) . . ? C29 Si6 C31 105.9(4) . . ? C30 Si6 C31 107.3(5) . . ? N5 Si6 Y1 33.62(16) . . ? C29 Si6 Y1 75.5(3) . . ? C30 Si6 Y1 128.9(4) . . ? C31 Si6 Y1 121.5(3) . . ? C1 N1 C2 122.3(5) . . ? C1 N1 Y1 94.1(3) . . ? C2 N1 Y1 141.1(4) . . ? C1 N2 C8 121.8(5) . . ? C1 N2 Y1 94.0(4) . . ? C8 N2 Y1 142.4(4) . . ? C1 N3 Si2 118.9(4) . . ? C1 N3 Si1 119.0(4) . . ? Si2 N3 Si1 122.1(3) . . ? Si4 N4 Si3 123.1(3) . . ? Si4 N4 Y1 114.5(2) . . ? Si3 N4 Y1 122.4(2) . . ? Si6 N5 Si5 123.3(3) . . ? Si6 N5 Y1 121.4(3) . . ? Si5 N5 Y1 115.2(3) . . ? N1 C1 N2 114.1(5) . . ? N1 C1 N3 123.0(5) . . ? N2 C1 N3 122.9(5) . . ? N1 C1 Y1 57.1(3) . . ? N2 C1 Y1 57.1(3) . . ? N3 C1 Y1 179.5(4) . . ? N1 C2 C3 110.9(5) . . ? N1 C2 C7 111.3(5) . . ? C3 C2 C7 109.3(6) . . ? N1 C2 H2 108.4 . . ? C3 C2 H2 108.4 . . ? C7 C2 H2 108.4 . . ? C2 C3 C4 112.4(6) . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 110.2(6) . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C4 110.8(7) . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C5 C6 C7 110.8(6) . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C2 C7 C6 112.5(6) . . ? C2 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? C2 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N2 C8 C9 112.2(5) . . ? N2 C8 C13 109.6(5) . . ? C9 C8 C13 108.8(6) . . ? N2 C8 H8 108.7 . . ? C9 C8 H8 108.7 . . ? C13 C8 H8 108.7 . . ? C8 C9 C10 113.1(6) . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C9 111.2(7) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 111.6(7) . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 111.1(7) . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C8 C13 C12 111.2(6) . . ? C8 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C8 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si4 C25 H25A 109.5 . . ? Si4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si5 C26 H26A 109.5 . . ? Si5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si5 C27 H27A 109.5 . . ? Si5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si5 C28 H28A 109.5 . . ? Si5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si6 C29 H29A 109.5 . . ? Si6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si6 C30 H30A 109.5 . . ? Si6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si6 C31 H31A 109.5 . . ? Si6 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si6 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Y1 Si4 N4 129.4(3) . . . . ? N2 Y1 Si4 N4 -42.8(4) . . . . ? N1 Y1 Si4 N4 -94.3(3) . . . . ? C1 Y1 Si4 N4 -77.7(3) . . . . ? Si5 Y1 Si4 N4 101.7(3) . . . . ? Si6 Y1 Si4 N4 154.9(3) . . . . ? N4 Y1 Si4 C23 74.9(5) . . . . ? N5 Y1 Si4 C23 -155.7(4) . . . . ? N2 Y1 Si4 C23 32.1(5) . . . . ? N1 Y1 Si4 C23 -19.4(4) . . . . ? C1 Y1 Si4 C23 -2.9(4) . . . . ? Si5 Y1 Si4 C23 176.6(4) . . . . ? Si6 Y1 Si4 C23 -130.2(4) . . . . ? N4 Y1 Si4 C24 -92.0(4) . . . . ? N5 Y1 Si4 C24 37.4(4) . . . . ? N2 Y1 Si4 C24 -134.8(4) . . . . ? N1 Y1 Si4 C24 173.6(4) . . . . ? C1 Y1 Si4 C24 -169.8(4) . . . . ? Si5 Y1 Si4 C24 9.7(3) . . . . ? Si6 Y1 Si4 C24 62.9(3) . . . . ? N4 Y1 Si4 C25 170.4(4) . . . . ? N5 Y1 Si4 C25 -60.2(3) . . . . ? N2 Y1 Si4 C25 127.6(4) . . . . ? N1 Y1 Si4 C25 76.1(3) . . . . ? C1 Y1 Si4 C25 92.7(3) . . . . ? Si5 Y1 Si4 C25 -87.8(3) . . . . ? Si6 Y1 Si4 C25 -34.7(3) . . . . ? N4 Y1 Si5 N5 129.3(3) . . . . ? N2 Y1 Si5 N5 -95.8(3) . . . . ? N1 Y1 Si5 N5 -45.1(4) . . . . ? C1 Y1 Si5 N5 -79.2(3) . . . . ? Si4 Y1 Si5 N5 101.3(3) . . . . ? Si6 Y1 Si5 N5 -1.7(3) . . . . ? N4 Y1 Si5 C27 44.1(4) . . . . ? N5 Y1 Si5 C27 -85.2(5) . . . . ? N2 Y1 Si5 C27 179.0(4) . . . . ? N1 Y1 Si5 C27 -130.3(4) . . . . ? C1 Y1 Si5 C27 -164.4(4) . . . . ? Si4 Y1 Si5 C27 16.1(4) . . . . ? Si6 Y1 Si5 C27 -86.9(4) . . . . ? N4 Y1 Si5 C28 -52.6(3) . . . . ? N5 Y1 Si5 C28 178.1(4) . . . . ? N2 Y1 Si5 C28 82.3(3) . . . . ? N1 Y1 Si5 C28 133.0(4) . . . . ? C1 Y1 Si5 C28 98.9(4) . . . . ? Si4 Y1 Si5 C28 -80.6(3) . . . . ? Si6 Y1 Si5 C28 176.4(3) . . . . ? N4 Y1 Si5 C26 -149.3(4) . . . . ? N5 Y1 Si5 C26 81.4(5) . . . . ? N2 Y1 Si5 C26 -14.4(4) . . . . ? N1 Y1 Si5 C26 36.3(5) . . . . ? C1 Y1 Si5 C26 2.2(4) . . . . ? Si4 Y1 Si5 C26 -177.3(4) . . . . ? Si6 Y1 Si5 C26 79.7(4) . . . . ? N4 Y1 Si6 N5 -71.5(3) . . . . ? N2 Y1 Si6 N5 102.3(3) . . . . ? N1 Y1 Si6 N5 161.9(3) . . . . ? C1 Y1 Si6 N5 132.0(3) . . . . ? Si4 Y1 Si6 N5 -86.5(3) . . . . ? Si5 Y1 Si6 N5 1.9(3) . . . . ? N4 Y1 Si6 C29 101.3(3) . . . . ? N5 Y1 Si6 C29 172.8(4) . . . . ? N2 Y1 Si6 C29 -84.9(3) . . . . ? N1 Y1 Si6 C29 -25.3(3) . . . . ? C1 Y1 Si6 C29 -55.2(3) . . . . ? Si4 Y1 Si6 C29 86.3(3) . . . . ? Si5 Y1 Si6 C29 174.7(3) . . . . ? N4 Y1 Si6 C30 1.6(5) . . . . ? N5 Y1 Si6 C30 73.1(5) . . . . ? N2 Y1 Si6 C30 175.4(4) . . . . ? N1 Y1 Si6 C30 -125.0(4) . . . . ? C1 Y1 Si6 C30 -154.8(5) . . . . ? Si4 Y1 Si6 C30 -13.3(4) . . . . ? Si5 Y1 Si6 C30 75.0(4) . . . . ? N4 Y1 Si6 C31 -158.7(4) . . . . ? N5 Y1 Si6 C31 -87.2(5) . . . . ? N2 Y1 Si6 C31 15.1(4) . . . . ? N1 Y1 Si6 C31 74.7(4) . . . . ? C1 Y1 Si6 C31 44.8(4) . . . . ? Si4 Y1 Si6 C31 -173.7(4) . . . . ? Si5 Y1 Si6 C31 -85.3(4) . . . . ? N4 Y1 N1 C1 124.4(3) . . . . ? N5 Y1 N1 C1 -86.0(4) . . . . ? N2 Y1 N1 C1 0.4(3) . . . . ? Si4 Y1 N1 C1 153.5(3) . . . . ? Si5 Y1 N1 C1 -61.3(4) . . . . ? Si6 Y1 N1 C1 -95.6(3) . . . . ? N4 Y1 N1 C2 -36.2(6) . . . . ? N5 Y1 N1 C2 113.4(6) . . . . ? N2 Y1 N1 C2 -160.2(6) . . . . ? C1 Y1 N1 C2 -160.6(8) . . . . ? Si4 Y1 N1 C2 -7.1(6) . . . . ? Si5 Y1 N1 C2 138.1(5) . . . . ? Si6 Y1 N1 C2 103.8(6) . . . . ? N4 Y1 N2 C1 -86.7(4) . . . . ? N5 Y1 N2 C1 124.8(3) . . . . ? N1 Y1 N2 C1 -0.4(3) . . . . ? Si4 Y1 N2 C1 -63.2(4) . . . . ? Si5 Y1 N2 C1 153.5(3) . . . . ? Si6 Y1 N2 C1 99.2(3) . . . . ? N4 Y1 N2 C8 110.2(6) . . . . ? N5 Y1 N2 C8 -38.3(6) . . . . ? N1 Y1 N2 C8 -163.4(7) . . . . ? C1 Y1 N2 C8 -163.1(8) . . . . ? Si4 Y1 N2 C8 133.7(5) . . . . ? Si5 Y1 N2 C8 -9.6(6) . . . . ? Si6 Y1 N2 C8 -63.8(6) . . . . ? C18 Si2 N3 C1 -10.5(6) . . . . ? C19 Si2 N3 C1 -129.4(6) . . . . ? C17 Si2 N3 C1 109.6(6) . . . . ? C18 Si2 N3 Si1 169.9(4) . . . . ? C19 Si2 N3 Si1 51.0(6) . . . . ? C17 Si2 N3 Si1 -70.0(5) . . . . ? C14 Si1 N3 C1 -7.6(6) . . . . ? C15 Si1 N3 C1 -127.5(6) . . . . ? C16 Si1 N3 C1 111.3(6) . . . . ? C14 Si1 N3 Si2 172.0(4) . . . . ? C15 Si1 N3 Si2 52.1(5) . . . . ? C16 Si1 N3 Si2 -69.1(6) . . . . ? C23 Si4 N4 Si3 50.2(5) . . . . ? C24 Si4 N4 Si3 -73.6(5) . . . . ? C25 Si4 N4 Si3 169.0(4) . . . . ? Y1 Si4 N4 Si3 178.4(5) . . . . ? C23 Si4 N4 Y1 -128.2(4) . . . . ? C24 Si4 N4 Y1 108.0(4) . . . . ? C25 Si4 N4 Y1 -9.4(4) . . . . ? C20 Si3 N4 Si4 171.6(4) . . . . ? C21 Si3 N4 Si4 53.3(5) . . . . ? C22 Si3 N4 Si4 -70.5(5) . . . . ? C20 Si3 N4 Y1 -10.1(5) . . . . ? C21 Si3 N4 Y1 -128.4(4) . . . . ? C22 Si3 N4 Y1 107.8(4) . . . . ? N5 Y1 N4 Si4 -59.2(3) . . . . ? N2 Y1 N4 Si4 155.4(2) . . . . ? N1 Y1 N4 Si4 94.0(3) . . . . ? C1 Y1 N4 Si4 121.4(3) . . . . ? Si5 Y1 N4 Si4 -83.3(2) . . . . ? Si6 Y1 N4 Si4 -32.1(3) . . . . ? N5 Y1 N4 Si3 122.3(3) . . . . ? N2 Y1 N4 Si3 -23.0(4) . . . . ? N1 Y1 N4 Si3 -84.5(3) . . . . ? C1 Y1 N4 Si3 -57.0(4) . . . . ? Si4 Y1 N4 Si3 -178.4(5) . . . . ? Si5 Y1 N4 Si3 98.3(3) . . . . ? Si6 Y1 N4 Si3 149.4(2) . . . . ? C29 Si6 N5 Si5 176.1(4) . . . . ? C30 Si6 N5 Si5 57.7(6) . . . . ? C31 Si6 N5 Si5 -65.7(5) . . . . ? Y1 Si6 N5 Si5 -176.5(6) . . . . ? C29 Si6 N5 Y1 -7.4(4) . . . . ? C30 Si6 N5 Y1 -125.7(5) . . . . ? C31 Si6 N5 Y1 110.8(5) . . . . ? C27 Si5 N5 Si6 -66.8(5) . . . . ? C28 Si5 N5 Si6 174.9(4) . . . . ? C26 Si5 N5 Si6 57.0(5) . . . . ? Y1 Si5 N5 Si6 176.7(5) . . . . ? C27 Si5 N5 Y1 116.5(4) . . . . ? C28 Si5 N5 Y1 -1.9(4) . . . . ? C26 Si5 N5 Y1 -119.8(4) . . . . ? N4 Y1 N5 Si6 123.9(3) . . . . ? N2 Y1 N5 Si6 -84.3(3) . . . . ? N1 Y1 N5 Si6 -22.5(4) . . . . ? C1 Y1 N5 Si6 -56.7(4) . . . . ? Si4 Y1 N5 Si6 99.6(3) . . . . ? Si5 Y1 N5 Si6 -176.8(5) . . . . ? N4 Y1 N5 Si5 -59.3(3) . . . . ? N2 Y1 N5 Si5 92.5(3) . . . . ? N1 Y1 N5 Si5 154.3(2) . . . . ? C1 Y1 N5 Si5 120.1(3) . . . . ? Si4 Y1 N5 Si5 -83.5(3) . . . . ? Si6 Y1 N5 Si5 176.8(5) . . . . ? C2 N1 C1 N2 165.1(5) . . . . ? Y1 N1 C1 N2 -0.6(5) . . . . ? C2 N1 C1 N3 -13.7(8) . . . . ? Y1 N1 C1 N3 -179.4(5) . . . . ? C2 N1 C1 Y1 165.7(6) . . . . ? C8 N2 C1 N1 168.5(5) . . . . ? Y1 N2 C1 N1 0.6(5) . . . . ? C8 N2 C1 N3 -12.7(8) . . . . ? Y1 N2 C1 N3 179.4(5) . . . . ? C8 N2 C1 Y1 167.9(6) . . . . ? Si2 N3 C1 N1 -77.2(6) . . . . ? Si1 N3 C1 N1 102.4(6) . . . . ? Si2 N3 C1 N2 104.1(6) . . . . ? Si1 N3 C1 N2 -76.3(6) . . . . ? Si2 N3 C1 Y1 -175(100) . . . . ? Si1 N3 C1 Y1 4(61) . . . . ? N4 Y1 C1 N1 -66.7(4) . . . . ? N5 Y1 C1 N1 113.9(3) . . . . ? N2 Y1 C1 N1 -179.3(5) . . . . ? Si4 Y1 C1 N1 -34.7(4) . . . . ? Si5 Y1 C1 N1 146.0(3) . . . . ? Si6 Y1 C1 N1 92.4(3) . . . . ? N4 Y1 C1 N2 112.6(3) . . . . ? N5 Y1 C1 N2 -66.8(4) . . . . ? N1 Y1 C1 N2 179.3(5) . . . . ? Si4 Y1 C1 N2 144.6(3) . . . . ? Si5 Y1 C1 N2 -34.7(4) . . . . ? Si6 Y1 C1 N2 -88.3(3) . . . . ? N4 Y1 C1 N3 32(61) . . . . ? N5 Y1 C1 N3 -148(60) . . . . ? N2 Y1 C1 N3 -81(60) . . . . ? N1 Y1 C1 N3 98(60) . . . . ? Si4 Y1 C1 N3 64(60) . . . . ? Si5 Y1 C1 N3 -116(60) . . . . ? Si6 Y1 C1 N3 -169(100) . . . . ? C1 N1 C2 C3 -112.5(6) . . . . ? Y1 N1 C2 C3 44.4(8) . . . . ? C1 N1 C2 C7 125.6(6) . . . . ? Y1 N1 C2 C7 -77.5(7) . . . . ? N1 C2 C3 C4 -178.5(6) . . . . ? C7 C2 C3 C4 -55.4(8) . . . . ? C2 C3 C4 C5 57.7(10) . . . . ? C3 C4 C5 C6 -57.3(10) . . . . ? C4 C5 C6 C7 56.2(10) . . . . ? N1 C2 C7 C6 176.8(6) . . . . ? C3 C2 C7 C6 54.0(8) . . . . ? C5 C6 C7 C2 -55.4(10) . . . . ? C1 N2 C8 C9 132.1(6) . . . . ? Y1 N2 C8 C9 -67.9(8) . . . . ? C1 N2 C8 C13 -106.9(7) . . . . ? Y1 N2 C8 C13 53.1(9) . . . . ? N2 C8 C9 C10 177.8(6) . . . . ? C13 C8 C9 C10 56.3(9) . . . . ? C8 C9 C10 C11 -56.3(11) . . . . ? C9 C10 C11 C12 54.5(11) . . . . ? C10 C11 C12 C13 -54.8(12) . . . . ? N2 C8 C13 C12 -178.6(7) . . . . ? C9 C8 C13 C12 -55.5(9) . . . . ? C11 C12 C13 C8 56.0(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.355 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.060 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 816943' #TrackingRef '4601_web_deposit_cif_file_0_luoyunjie_1299825581.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H76 N5 O Si6 Y' _chemical_formula_sum 'C31 H76 N5 O Si6 Y' _chemical_formula_weight 792.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0258(13) _cell_length_b 19.1155(19) _cell_length_c 20.642(2) _cell_angle_alpha 75.965(5) _cell_angle_beta 87.006(6) _cell_angle_gamma 85.555(6) _cell_volume 4587.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 20348 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 1.456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_T_max 0.770 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39101 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.1005 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.50 _reflns_number_total 16946 _reflns_number_gt 12758 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0309P)^2^+2.2612P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16946 _refine_ls_number_parameters 854 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1048 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1266 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.13038(4) 0.28542(2) 0.35134(2) 0.03219(12) Uani 1 1 d . . . Y2 Y 0.57261(4) 0.20133(2) 0.80270(2) 0.03347(13) Uani 1 1 d . . . Si1 Si 0.08733(13) 0.15113(9) 0.16658(8) 0.0517(4) Uani 1 1 d . . . Si2 Si -0.13453(12) 0.24561(9) 0.16331(8) 0.0508(4) Uani 1 1 d . . . Si3 Si 0.42591(12) 0.26256(8) 0.32967(8) 0.0455(4) Uani 1 1 d . . . H3 H 0.405(3) 0.333(2) 0.289(2) 0.051(13) Uiso 1 1 d . . . Si4 Si 0.29440(12) 0.15834(8) 0.43280(8) 0.0462(4) Uani 1 1 d . . . H4 H 0.179(4) 0.160(2) 0.451(2) 0.066(15) Uiso 1 1 d . . . Si5 Si 0.06787(12) 0.28318(8) 0.51679(7) 0.0440(4) Uani 1 1 d . . . H5 H 0.188(4) 0.268(2) 0.512(2) 0.067(15) Uiso 1 1 d . . . Si6 Si -0.10257(13) 0.35609(8) 0.41697(7) 0.0482(4) Uani 1 1 d . . . H6 H -0.110(4) 0.363(3) 0.349(3) 0.078(17) Uiso 1 1 d . . . Si7 Si 0.22834(12) 0.37178(8) 0.82560(8) 0.0475(4) Uani 1 1 d . . . Si8 Si 0.42371(13) 0.47420(8) 0.80019(8) 0.0488(4) Uani 1 1 d . . . Si9 Si 0.45493(13) 0.06389(8) 0.88397(8) 0.0505(4) Uani 1 1 d . . . H9 H 0.529(3) 0.108(2) 0.913(2) 0.046(13) Uiso 1 1 d . . . Si10 Si 0.39479(14) 0.09468(8) 0.73818(9) 0.0559(4) Uani 1 1 d . . . H10 H 0.443(4) 0.141(3) 0.676(3) 0.079(17) Uiso 1 1 d . . . Si11 Si 0.80489(12) 0.11344(8) 0.90611(7) 0.0463(4) Uani 1 1 d . . . H11 H 0.760(3) 0.0479(19) 0.8976(18) 0.029(11) Uiso 1 1 d . . . Si12 Si 0.80769(12) 0.25810(8) 0.80691(8) 0.0470(4) Uani 1 1 d . . . H12 H 0.720(3) 0.300(2) 0.771(2) 0.047(13) Uiso 1 1 d . . . O1 O 0.1944(3) 0.40491(16) 0.33192(16) 0.0415(8) Uani 1 1 d . . . O2 O 0.6675(3) 0.16776(17) 0.70718(17) 0.0486(9) Uani 1 1 d . . . N1 N 0.0898(3) 0.30424(19) 0.23772(18) 0.0344(9) Uani 1 1 d . . . N2 N 0.0228(3) 0.20895(19) 0.31252(18) 0.0345(9) Uani 1 1 d . . . N3 N -0.0021(3) 0.2164(2) 0.19436(18) 0.0366(9) Uani 1 1 d . . . N4 N 0.3036(3) 0.2349(2) 0.37062(19) 0.0378(9) Uani 1 1 d . . . N5 N 0.0225(3) 0.3122(2) 0.43730(19) 0.0402(10) Uani 1 1 d . . . N6 N 0.4773(3) 0.31047(19) 0.74954(18) 0.0349(9) Uani 1 1 d . . . N7 N 0.4843(3) 0.28194(19) 0.86124(18) 0.0362(9) Uani 1 1 d . . . N8 N 0.3700(3) 0.38945(19) 0.80996(19) 0.0368(9) Uani 1 1 d . . . N9 N 0.4609(3) 0.1116(2) 0.8032(2) 0.0433(10) Uani 1 1 d . . . N10 N 0.7454(3) 0.1826(2) 0.84734(19) 0.0385(9) Uani 1 1 d . . . C1 C 0.0363(4) 0.2431(2) 0.2481(2) 0.0345(11) Uani 1 1 d . . . C2 C 0.1180(4) 0.3460(2) 0.1703(2) 0.0376(11) Uani 1 1 d . . . H2 H 0.1106 0.3154 0.1386 0.045 Uiso 1 1 calc R . . C3 C 0.2388(4) 0.3672(3) 0.1664(2) 0.0428(12) Uani 1 1 d . . . H3A H 0.2490 0.3924 0.2015 0.051 Uiso 1 1 calc R . . H3B H 0.2889 0.3232 0.1749 0.051 Uiso 1 1 calc R . . C4 C 0.2712(5) 0.4155(3) 0.0989(3) 0.0552(15) Uani 1 1 d . . . H4A H 0.3471 0.4302 0.1005 0.066 Uiso 1 1 calc R . . H4B H 0.2711 0.3880 0.0645 0.066 Uiso 1 1 calc R . . C5 C 0.1927(5) 0.4820(3) 0.0799(3) 0.0651(17) Uani 1 1 d . . . H5A H 0.2126 0.5096 0.0348 0.078 Uiso 1 1 calc R . . H5B H 0.1993 0.5129 0.1109 0.078 Uiso 1 1 calc R . . C6 C 0.0738(5) 0.4606(3) 0.0821(3) 0.0621(16) Uani 1 1 d . . . H6A H 0.0660 0.4340 0.0477 0.075 Uiso 1 1 calc R . . H6B H 0.0233 0.5043 0.0720 0.075 Uiso 1 1 calc R . . C7 C 0.0405(4) 0.4140(3) 0.1498(2) 0.0473(13) Uani 1 1 d . . . H7A H -0.0359 0.4001 0.1484 0.057 Uiso 1 1 calc R . . H7B H 0.0415 0.4423 0.1835 0.057 Uiso 1 1 calc R . . C8 C -0.0460(4) 0.1472(2) 0.3340(2) 0.0382(12) Uani 1 1 d . . . H8 H -0.0806 0.1388 0.2943 0.046 Uiso 1 1 calc R . . C9 C -0.1387(4) 0.1624(3) 0.3834(3) 0.0507(14) Uani 1 1 d . . . H9A H -0.1053 0.1722 0.4223 0.061 Uiso 1 1 calc R . . H9B H -0.1849 0.2055 0.3620 0.061 Uiso 1 1 calc R . . C10 C -0.2122(5) 0.0988(3) 0.4064(3) 0.0716(19) Uani 1 1 d . . . H10A H -0.2673 0.1093 0.4401 0.086 Uiso 1 1 calc R . . H10B H -0.2527 0.0928 0.3684 0.086 Uiso 1 1 calc R . . C11 C -0.1445(6) 0.0293(3) 0.4358(3) 0.080(2) Uani 1 1 d . . . H11A H -0.1933 -0.0109 0.4454 0.095 Uiso 1 1 calc R . . H11B H -0.1142 0.0325 0.4781 0.095 Uiso 1 1 calc R . . C12 C -0.0492(5) 0.0143(3) 0.3889(3) 0.077(2) Uani 1 1 d . . . H12A H -0.0795 0.0037 0.3494 0.092 Uiso 1 1 calc R . . H12B H -0.0029 -0.0282 0.4114 0.092 Uiso 1 1 calc R . . C13 C 0.0225(5) 0.0791(3) 0.3672(3) 0.0583(16) Uani 1 1 d . . . H13A H 0.0577 0.0870 0.4063 0.070 Uiso 1 1 calc R . . H13B H 0.0819 0.0686 0.3359 0.070 Uiso 1 1 calc R . . C14 C 0.2263(4) 0.1496(3) 0.2017(3) 0.0559(15) Uani 1 1 d . . . H14A H 0.2576 0.1961 0.1843 0.084 Uiso 1 1 calc R . . H14B H 0.2753 0.1120 0.1892 0.084 Uiso 1 1 calc R . . H14C H 0.2188 0.1402 0.2500 0.084 Uiso 1 1 calc R . . C15 C 0.1000(5) 0.1748(4) 0.0736(3) 0.089(2) Uani 1 1 d . . . H15A H 0.0290 0.1699 0.0554 0.133 Uiso 1 1 calc R . . H15B H 0.1567 0.1425 0.0591 0.133 Uiso 1 1 calc R . . H15C H 0.1208 0.2242 0.0580 0.133 Uiso 1 1 calc R . . C16 C 0.0373(5) 0.0585(3) 0.1919(4) 0.085(2) Uani 1 1 d . . . H16A H 0.0173 0.0471 0.2393 0.128 Uiso 1 1 calc R . . H16B H 0.0960 0.0240 0.1830 0.128 Uiso 1 1 calc R . . H16C H -0.0276 0.0561 0.1667 0.128 Uiso 1 1 calc R . . C17 C -0.1273(5) 0.3015(3) 0.0752(3) 0.0761(19) Uani 1 1 d . . . H17A H -0.0691 0.3350 0.0706 0.114 Uiso 1 1 calc R . . H17B H -0.1985 0.3284 0.0645 0.114 Uiso 1 1 calc R . . H17C H -0.1106 0.2702 0.0449 0.114 Uiso 1 1 calc R . . C18 C -0.2102(4) 0.2995(3) 0.2176(3) 0.0664(17) Uani 1 1 d . . . H18A H -0.2312 0.2676 0.2599 0.100 Uiso 1 1 calc R . . H18B H -0.2767 0.3242 0.1958 0.100 Uiso 1 1 calc R . . H18C H -0.1621 0.3349 0.2255 0.100 Uiso 1 1 calc R . . C19 C -0.2157(5) 0.1664(3) 0.1651(3) 0.0717(18) Uani 1 1 d . . . H19A H -0.1787 0.1380 0.1361 0.108 Uiso 1 1 calc R . . H19B H -0.2902 0.1829 0.1497 0.108 Uiso 1 1 calc R . . H19C H -0.2205 0.1368 0.2104 0.108 Uiso 1 1 calc R . . C20 C 0.4885(5) 0.2033(4) 0.2758(3) 0.0736(19) Uani 1 1 d . . . H20A H 0.5148 0.1571 0.3036 0.110 Uiso 1 1 calc R . . H20B H 0.5507 0.2262 0.2493 0.110 Uiso 1 1 calc R . . H20C H 0.4326 0.1959 0.2463 0.110 Uiso 1 1 calc R . . C21 C 0.5363(4) 0.2717(3) 0.3860(3) 0.0706(18) Uani 1 1 d . . . H21A H 0.5078 0.3035 0.4141 0.106 Uiso 1 1 calc R . . H21B H 0.6004 0.2917 0.3596 0.106 Uiso 1 1 calc R . . H21C H 0.5582 0.2245 0.4139 0.106 Uiso 1 1 calc R . . C22 C 0.3356(5) 0.0721(3) 0.4076(3) 0.0695(18) Uani 1 1 d . . . H22A H 0.3028 0.0733 0.3654 0.104 Uiso 1 1 calc R . . H22B H 0.3090 0.0317 0.4416 0.104 Uiso 1 1 calc R . . H22C H 0.4162 0.0664 0.4028 0.104 Uiso 1 1 calc R . . C23 C 0.3678(5) 0.1530(3) 0.5117(3) 0.0700(17) Uani 1 1 d . . . H23A H 0.4468 0.1412 0.5050 0.105 Uiso 1 1 calc R . . H23B H 0.3373 0.1157 0.5473 0.105 Uiso 1 1 calc R . . H23C H 0.3573 0.1991 0.5236 0.105 Uiso 1 1 calc R . . C24 C 0.0131(5) 0.1967(3) 0.5648(3) 0.0621(16) Uani 1 1 d . . . H24A H -0.0676 0.2026 0.5693 0.093 Uiso 1 1 calc R . . H24B H 0.0445 0.1833 0.6088 0.093 Uiso 1 1 calc R . . H24C H 0.0337 0.1591 0.5414 0.093 Uiso 1 1 calc R . . C25 C 0.0380(5) 0.3500(3) 0.5700(3) 0.0627(16) Uani 1 1 d . . . H25A H 0.0687 0.3955 0.5478 0.094 Uiso 1 1 calc R . . H25B H 0.0719 0.3313 0.6129 0.094 Uiso 1 1 calc R . . H25C H -0.0420 0.3576 0.5767 0.094 Uiso 1 1 calc R . . C26 C -0.2245(4) 0.3137(3) 0.4672(3) 0.0686(18) Uani 1 1 d . . . H26A H -0.2249 0.2638 0.4644 0.103 Uiso 1 1 calc R . . H26B H -0.2931 0.3399 0.4497 0.103 Uiso 1 1 calc R . . H26C H -0.2187 0.3154 0.5135 0.103 Uiso 1 1 calc R . . C27 C -0.1180(5) 0.4524(3) 0.4241(3) 0.0655(17) Uani 1 1 d . . . H27A H -0.1060 0.4541 0.4698 0.098 Uiso 1 1 calc R . . H27B H -0.1926 0.4727 0.4119 0.098 Uiso 1 1 calc R . . H27C H -0.0636 0.4802 0.3944 0.098 Uiso 1 1 calc R . . C28 C 0.2640(4) 0.4182(3) 0.3825(3) 0.0531(14) Uani 1 1 d . . . H28A H 0.3388 0.4300 0.3640 0.064 Uiso 1 1 calc R . . H28B H 0.2707 0.3759 0.4204 0.064 Uiso 1 1 calc R . . C29 C 0.2047(5) 0.4808(3) 0.4036(3) 0.0608(16) Uani 1 1 d . . . H29A H 0.2562 0.5070 0.4228 0.073 Uiso 1 1 calc R . . H29B H 0.1443 0.4652 0.4364 0.073 Uiso 1 1 calc R . . C30 C 0.1592(5) 0.5271(3) 0.3389(3) 0.0547(15) Uani 1 1 d . . . H30A H 0.0907 0.5553 0.3472 0.066 Uiso 1 1 calc R . . H30B H 0.2142 0.5603 0.3150 0.066 Uiso 1 1 calc R . . C31 C 0.1361(4) 0.4726(3) 0.2997(3) 0.0485(13) Uani 1 1 d . . . H31A H 0.0558 0.4669 0.3001 0.058 Uiso 1 1 calc R . . H31B H 0.1632 0.4886 0.2533 0.058 Uiso 1 1 calc R . . C32 C 0.4450(4) 0.3277(2) 0.8071(2) 0.0353(11) Uani 1 1 d . . . C33 C 0.4447(4) 0.3555(3) 0.6850(2) 0.0407(12) Uani 1 1 d . . . H33 H 0.3996 0.3986 0.6926 0.049 Uiso 1 1 calc R . . C34 C 0.3749(4) 0.3163(3) 0.6472(3) 0.0512(14) Uani 1 1 d . . . H34A H 0.4151 0.2705 0.6442 0.061 Uiso 1 1 calc R . . H34B H 0.3046 0.3049 0.6724 0.061 Uiso 1 1 calc R . . C35 C 0.3490(5) 0.3603(3) 0.5770(3) 0.0621(16) Uani 1 1 d . . . H35A H 0.3071 0.3317 0.5545 0.075 Uiso 1 1 calc R . . H35B H 0.3021 0.4038 0.5800 0.075 Uiso 1 1 calc R . . C36 C 0.4534(5) 0.3820(3) 0.5366(3) 0.0616(16) Uani 1 1 d . . . H36A H 0.4337 0.4117 0.4924 0.074 Uiso 1 1 calc R . . H36B H 0.4977 0.3388 0.5304 0.074 Uiso 1 1 calc R . . C37 C 0.5215(5) 0.4244(3) 0.5714(3) 0.0656(17) Uani 1 1 d . . . H37A H 0.4797 0.4699 0.5739 0.079 Uiso 1 1 calc R . . H37B H 0.5911 0.4362 0.5456 0.079 Uiso 1 1 calc R . . C38 C 0.5482(4) 0.3812(3) 0.6415(3) 0.0558(15) Uani 1 1 d . . . H38A H 0.5887 0.4109 0.6635 0.067 Uiso 1 1 calc R . . H38B H 0.5977 0.3388 0.6382 0.067 Uiso 1 1 calc R . . C39 C 0.4639(4) 0.2951(3) 0.9283(2) 0.0398(12) Uani 1 1 d . . . H39 H 0.4060 0.3353 0.9258 0.048 Uiso 1 1 calc R . . C40 C 0.5698(4) 0.3161(4) 0.9534(3) 0.0690(18) Uani 1 1 d . . . H40A H 0.5956 0.3596 0.9224 0.083 Uiso 1 1 calc R . . H40B H 0.6283 0.2771 0.9552 0.083 Uiso 1 1 calc R . . C41 C 0.5484(5) 0.3303(5) 1.0232(3) 0.095(3) Uani 1 1 d . . . H41A H 0.6178 0.3428 1.0393 0.115 Uiso 1 1 calc R . . H41B H 0.4931 0.3712 1.0209 0.115 Uiso 1 1 calc R . . C42 C 0.5060(7) 0.2634(5) 1.0716(3) 0.109(3) Uani 1 1 d . . . H42A H 0.5645 0.2240 1.0772 0.131 Uiso 1 1 calc R . . H42B H 0.4889 0.2740 1.1153 0.131 Uiso 1 1 calc R . . C43 C 0.4047(6) 0.2403(3) 1.0472(3) 0.078(2) Uani 1 1 d . . . H43A H 0.3434 0.2771 1.0473 0.093 Uiso 1 1 calc R . . H43B H 0.3830 0.1952 1.0776 0.093 Uiso 1 1 calc R . . C44 C 0.4233(5) 0.2286(3) 0.9767(3) 0.0635(17) Uani 1 1 d . . . H44A H 0.4784 0.1878 0.9776 0.076 Uiso 1 1 calc R . . H44B H 0.3532 0.2164 0.9614 0.076 Uiso 1 1 calc R . . C45 C 0.2101(5) 0.2766(3) 0.8261(4) 0.086(2) Uani 1 1 d . . . H45A H 0.2597 0.2623 0.7924 0.129 Uiso 1 1 calc R . . H45B H 0.1334 0.2716 0.8165 0.129 Uiso 1 1 calc R . . H45C H 0.2275 0.2461 0.8697 0.129 Uiso 1 1 calc R . . C46 C 0.1418(5) 0.4311(4) 0.7602(4) 0.109(3) Uani 1 1 d . . . H46A H 0.1465 0.4811 0.7618 0.164 Uiso 1 1 calc R . . H46B H 0.0648 0.4186 0.7678 0.164 Uiso 1 1 calc R . . H46C H 0.1686 0.4249 0.7167 0.164 Uiso 1 1 calc R . . C47 C 0.1727(5) 0.3863(5) 0.9073(4) 0.111(3) Uani 1 1 d . . . H47A H 0.2202 0.3590 0.9426 0.166 Uiso 1 1 calc R . . H47B H 0.0976 0.3701 0.9155 0.166 Uiso 1 1 calc R . . H47C H 0.1713 0.4373 0.9066 0.166 Uiso 1 1 calc R . . C48 C 0.3730(6) 0.5403(3) 0.7241(3) 0.0776(19) Uani 1 1 d . . . H48A H 0.3969 0.5229 0.6849 0.116 Uiso 1 1 calc R . . H48B H 0.4034 0.5866 0.7212 0.116 Uiso 1 1 calc R . . H48C H 0.2921 0.5460 0.7267 0.116 Uiso 1 1 calc R . . C49 C 0.5783(4) 0.4655(3) 0.7920(3) 0.0709(18) Uani 1 1 d . . . H49A H 0.6094 0.4540 0.8361 0.106 Uiso 1 1 calc R . . H49B H 0.6052 0.5108 0.7660 0.106 Uiso 1 1 calc R . . H49C H 0.6011 0.4273 0.7698 0.106 Uiso 1 1 calc R . . C50 C 0.3832(6) 0.5129(3) 0.8736(3) 0.087(2) Uani 1 1 d . . . H50A H 0.3027 0.5213 0.8763 0.130 Uiso 1 1 calc R . . H50B H 0.4176 0.5583 0.8684 0.130 Uiso 1 1 calc R . . H50C H 0.4082 0.4792 0.9141 0.130 Uiso 1 1 calc R . . C51 C 0.3152(5) 0.0653(3) 0.9276(3) 0.0747(19) Uani 1 1 d . . . H51A H 0.2871 0.1150 0.9242 0.112 Uiso 1 1 calc R . . H51B H 0.3219 0.0405 0.9743 0.112 Uiso 1 1 calc R . . H51C H 0.2639 0.0412 0.9069 0.112 Uiso 1 1 calc R . . C52 C 0.5144(5) -0.0314(3) 0.8997(3) 0.0724(18) Uani 1 1 d . . . H52A H 0.4664 -0.0597 0.8814 0.109 Uiso 1 1 calc R . . H52B H 0.5196 -0.0514 0.9475 0.109 Uiso 1 1 calc R . . H52C H 0.5882 -0.0328 0.8785 0.109 Uiso 1 1 calc R . . C53 C 0.2408(5) 0.1110(4) 0.7405(4) 0.112(3) Uani 1 1 d . . . H53A H 0.2093 0.0782 0.7794 0.167 Uiso 1 1 calc R . . H53B H 0.2112 0.1027 0.7003 0.167 Uiso 1 1 calc R . . H53C H 0.2212 0.1605 0.7429 0.167 Uiso 1 1 calc R . . C54 C 0.4257(6) 0.0013(3) 0.7263(4) 0.096(2) Uani 1 1 d . . . H54A H 0.5057 -0.0100 0.7264 0.144 Uiso 1 1 calc R . . H54B H 0.3974 -0.0017 0.6840 0.144 Uiso 1 1 calc R . . H54C H 0.3900 -0.0329 0.7624 0.144 Uiso 1 1 calc R . . C55 C 0.9597(4) 0.1008(3) 0.8961(3) 0.0758(19) Uani 1 1 d . . . H55A H 0.9793 0.0954 0.8512 0.114 Uiso 1 1 calc R . . H55B H 0.9866 0.0578 0.9284 0.114 Uiso 1 1 calc R . . H55C H 0.9936 0.1425 0.9033 0.114 Uiso 1 1 calc R . . C56 C 0.7747(5) 0.1235(3) 0.9933(3) 0.0685(17) Uani 1 1 d . . . H56A H 0.7990 0.1695 0.9973 0.103 Uiso 1 1 calc R . . H56B H 0.8144 0.0845 1.0245 0.103 Uiso 1 1 calc R . . H56C H 0.6952 0.1218 1.0035 0.103 Uiso 1 1 calc R . . C57 C 0.9206(4) 0.2461(3) 0.7443(3) 0.0681(17) Uani 1 1 d . . . H57A H 0.9838 0.2180 0.7671 0.102 Uiso 1 1 calc R . . H57B H 0.9435 0.2930 0.7199 0.102 Uiso 1 1 calc R . . H57C H 0.8930 0.2210 0.7134 0.102 Uiso 1 1 calc R . . C58 C 0.8608(5) 0.3146(3) 0.8593(3) 0.0716(18) Uani 1 1 d . . . H58A H 0.8010 0.3269 0.8887 0.107 Uiso 1 1 calc R . . H58B H 0.8877 0.3585 0.8305 0.107 Uiso 1 1 calc R . . H58C H 0.9214 0.2877 0.8857 0.107 Uiso 1 1 calc R . . C59 C 0.7259(5) 0.0962(3) 0.7251(3) 0.0639(17) Uani 1 1 d . . . H59A H 0.6740 0.0599 0.7471 0.077 Uiso 1 1 calc R . . H59B H 0.7857 0.0959 0.7557 0.077 Uiso 1 1 calc R . . C60 C 0.7723(6) 0.0805(4) 0.6625(3) 0.077(2) Uani 1 1 d . . . H60A H 0.7697 0.0291 0.6637 0.092 Uiso 1 1 calc R . . H60B H 0.8499 0.0937 0.6545 0.092 Uiso 1 1 calc R . . C61 C 0.6998(6) 0.1257(3) 0.6098(3) 0.079(2) Uani 1 1 d . . . H61A H 0.6331 0.1011 0.6053 0.095 Uiso 1 1 calc R . . H61B H 0.7403 0.1375 0.5665 0.095 Uiso 1 1 calc R . . C62 C 0.6696(5) 0.1925(3) 0.6352(2) 0.0611(16) Uani 1 1 d . . . H62A H 0.7254 0.2282 0.6198 0.073 Uiso 1 1 calc R . . H62B H 0.5964 0.2144 0.6196 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0349(3) 0.0323(2) 0.0303(3) -0.0097(2) -0.0009(2) -0.0008(2) Y2 0.0360(3) 0.0304(2) 0.0329(3) -0.0069(2) 0.0010(2) 0.0012(2) Si1 0.0510(9) 0.0595(10) 0.0539(10) -0.0330(9) 0.0018(8) -0.0008(8) Si2 0.0439(9) 0.0657(10) 0.0467(9) -0.0198(8) -0.0126(7) -0.0010(8) Si3 0.0379(8) 0.0493(9) 0.0480(9) -0.0092(8) -0.0033(7) -0.0012(7) Si4 0.0453(9) 0.0456(8) 0.0475(9) -0.0122(7) -0.0002(7) 0.0009(7) Si5 0.0464(9) 0.0466(8) 0.0429(9) -0.0183(7) 0.0048(7) -0.0058(7) Si6 0.0576(10) 0.0488(9) 0.0392(9) -0.0149(7) 0.0023(7) 0.0021(8) Si7 0.0354(8) 0.0501(9) 0.0555(10) -0.0126(8) 0.0000(7) 0.0056(7) Si8 0.0559(9) 0.0342(8) 0.0577(10) -0.0147(7) 0.0001(8) -0.0003(7) Si9 0.0571(10) 0.0391(8) 0.0525(10) -0.0056(7) 0.0035(8) -0.0068(7) Si10 0.0646(11) 0.0477(9) 0.0587(10) -0.0161(8) -0.0078(9) -0.0106(8) Si11 0.0496(9) 0.0423(8) 0.0456(9) -0.0081(7) -0.0103(7) 0.0033(7) Si12 0.0382(8) 0.0501(9) 0.0494(9) -0.0052(8) 0.0015(7) -0.0049(7) O1 0.050(2) 0.0358(18) 0.0394(19) -0.0084(16) -0.0091(16) -0.0025(16) O2 0.055(2) 0.045(2) 0.043(2) -0.0098(18) 0.0067(18) 0.0071(18) N1 0.040(2) 0.035(2) 0.029(2) -0.0089(18) -0.0039(18) -0.0011(18) N2 0.041(2) 0.032(2) 0.032(2) -0.0086(18) -0.0040(18) -0.0060(18) N3 0.035(2) 0.045(2) 0.032(2) -0.016(2) -0.0044(18) 0.0001(19) N4 0.034(2) 0.043(2) 0.037(2) -0.011(2) -0.0024(18) -0.0002(19) N5 0.043(2) 0.042(2) 0.038(2) -0.015(2) 0.0047(19) -0.0030(19) N6 0.039(2) 0.034(2) 0.028(2) -0.0022(18) -0.0039(18) 0.0061(18) N7 0.046(2) 0.031(2) 0.029(2) -0.0057(18) -0.0003(19) 0.0065(18) N8 0.032(2) 0.035(2) 0.043(2) -0.012(2) -0.0014(18) 0.0053(18) N9 0.045(2) 0.038(2) 0.048(3) -0.012(2) 0.002(2) -0.008(2) N10 0.037(2) 0.038(2) 0.037(2) -0.0037(19) 0.0033(19) -0.0032(19) C1 0.032(3) 0.041(3) 0.033(3) -0.014(2) -0.002(2) 0.004(2) C2 0.047(3) 0.037(3) 0.028(3) -0.007(2) -0.003(2) 0.000(2) C3 0.046(3) 0.040(3) 0.041(3) -0.010(2) 0.004(2) 0.005(2) C4 0.069(4) 0.045(3) 0.050(3) -0.010(3) 0.020(3) -0.013(3) C5 0.096(5) 0.045(3) 0.047(4) -0.001(3) 0.017(3) -0.007(3) C6 0.083(5) 0.053(3) 0.042(3) 0.002(3) -0.010(3) 0.012(3) C7 0.049(3) 0.047(3) 0.040(3) -0.003(3) -0.007(3) 0.005(3) C8 0.041(3) 0.038(3) 0.040(3) -0.015(2) -0.005(2) -0.007(2) C9 0.048(3) 0.050(3) 0.054(3) -0.015(3) 0.007(3) -0.007(3) C10 0.064(4) 0.073(4) 0.079(5) -0.020(4) 0.027(4) -0.028(4) C11 0.091(5) 0.060(4) 0.084(5) -0.006(4) 0.025(4) -0.037(4) C12 0.092(5) 0.040(3) 0.096(5) -0.008(4) 0.012(4) -0.019(3) C13 0.062(4) 0.035(3) 0.075(4) -0.010(3) 0.007(3) -0.004(3) C14 0.050(3) 0.059(4) 0.062(4) -0.025(3) 0.006(3) 0.010(3) C15 0.081(5) 0.141(7) 0.058(4) -0.059(5) -0.005(4) 0.014(5) C16 0.085(5) 0.065(4) 0.122(6) -0.056(4) 0.007(4) -0.006(4) C17 0.076(4) 0.098(5) 0.055(4) -0.013(4) -0.028(3) -0.006(4) C18 0.047(3) 0.075(4) 0.078(5) -0.024(4) -0.010(3) 0.011(3) C19 0.053(4) 0.094(5) 0.077(5) -0.032(4) -0.015(3) -0.014(3) C20 0.054(4) 0.102(5) 0.073(4) -0.039(4) 0.020(3) -0.013(4) C21 0.050(4) 0.094(5) 0.074(4) -0.027(4) -0.006(3) -0.020(3) C22 0.076(4) 0.044(3) 0.086(5) -0.018(3) 0.016(4) 0.002(3) C23 0.081(4) 0.075(4) 0.044(4) 0.003(3) -0.009(3) 0.004(4) C24 0.075(4) 0.057(4) 0.051(4) -0.005(3) 0.004(3) -0.011(3) C25 0.085(4) 0.061(4) 0.049(4) -0.028(3) 0.005(3) -0.008(3) C26 0.050(4) 0.081(4) 0.082(5) -0.034(4) 0.003(3) -0.004(3) C27 0.070(4) 0.054(4) 0.073(4) -0.022(3) 0.010(3) 0.011(3) C28 0.062(4) 0.051(3) 0.049(3) -0.012(3) -0.014(3) -0.013(3) C29 0.071(4) 0.063(4) 0.056(4) -0.027(3) 0.001(3) -0.016(3) C30 0.061(4) 0.045(3) 0.063(4) -0.023(3) 0.007(3) -0.007(3) C31 0.051(3) 0.046(3) 0.049(3) -0.012(3) -0.005(3) 0.005(3) C32 0.036(3) 0.033(3) 0.037(3) -0.008(2) 0.004(2) -0.004(2) C33 0.046(3) 0.036(3) 0.042(3) -0.014(2) -0.009(2) 0.008(2) C34 0.050(3) 0.055(3) 0.048(3) -0.007(3) -0.006(3) -0.011(3) C35 0.069(4) 0.064(4) 0.056(4) -0.014(3) -0.026(3) -0.007(3) C36 0.083(4) 0.060(4) 0.041(3) -0.006(3) -0.015(3) -0.008(3) C37 0.082(4) 0.068(4) 0.040(3) 0.010(3) -0.014(3) -0.029(3) C38 0.060(4) 0.063(4) 0.041(3) 0.000(3) -0.007(3) -0.024(3) C39 0.041(3) 0.042(3) 0.035(3) -0.011(2) 0.002(2) 0.011(2) C40 0.045(3) 0.119(5) 0.053(4) -0.043(4) 0.002(3) 0.001(4) C41 0.059(4) 0.182(8) 0.064(5) -0.067(6) -0.008(4) 0.004(5) C42 0.107(6) 0.169(9) 0.039(4) -0.027(5) -0.007(4) 0.074(6) C43 0.109(6) 0.072(4) 0.039(4) 0.000(3) 0.023(4) 0.018(4) C44 0.096(5) 0.044(3) 0.044(3) -0.004(3) 0.022(3) 0.006(3) C45 0.049(4) 0.062(4) 0.147(7) -0.028(4) 0.024(4) -0.017(3) C46 0.043(4) 0.117(6) 0.135(7) 0.037(5) -0.025(4) -0.003(4) C47 0.047(4) 0.200(9) 0.114(6) -0.095(7) 0.030(4) -0.018(5) C48 0.109(5) 0.039(3) 0.078(5) 0.003(3) -0.019(4) -0.006(3) C49 0.063(4) 0.051(3) 0.104(5) -0.024(4) -0.001(4) -0.018(3) C50 0.123(6) 0.061(4) 0.085(5) -0.038(4) 0.015(4) -0.009(4) C51 0.075(4) 0.073(4) 0.071(4) -0.007(4) 0.018(4) -0.021(4) C52 0.089(5) 0.040(3) 0.079(5) -0.001(3) -0.002(4) 0.001(3) C53 0.070(5) 0.155(8) 0.132(7) -0.075(7) -0.027(5) -0.004(5) C54 0.130(6) 0.068(4) 0.105(6) -0.047(5) -0.019(5) -0.009(4) C55 0.053(4) 0.082(5) 0.091(5) -0.020(4) -0.021(4) 0.014(3) C56 0.098(5) 0.066(4) 0.040(3) -0.007(3) -0.014(3) -0.008(4) C57 0.051(4) 0.097(5) 0.057(4) -0.018(4) 0.009(3) -0.018(3) C58 0.058(4) 0.072(4) 0.092(5) -0.034(4) 0.010(4) -0.016(3) C59 0.078(4) 0.050(3) 0.060(4) -0.018(3) 0.009(3) 0.023(3) C60 0.086(5) 0.074(4) 0.076(5) -0.038(4) 0.008(4) 0.010(4) C61 0.106(5) 0.085(5) 0.053(4) -0.039(4) 0.004(4) 0.012(4) C62 0.081(4) 0.063(4) 0.034(3) -0.007(3) 0.007(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N4 2.241(4) . ? Y1 N5 2.278(4) . ? Y1 N2 2.328(3) . ? Y1 N1 2.356(4) . ? Y1 O1 2.401(3) . ? Y1 C1 2.776(4) . ? Y1 Si4 3.2003(16) . ? Y1 Si6 3.3783(15) . ? Y1 Si5 3.4491(15) . ? Y2 N9 2.256(4) . ? Y2 N10 2.284(4) . ? Y2 N7 2.340(3) . ? Y2 N6 2.349(4) . ? Y2 O2 2.422(3) . ? Y2 C32 2.777(5) . ? Y2 Si12 3.1184(15) . ? Y2 Si9 3.1480(15) . ? Y2 H9 2.59(4) . ? Si1 N3 1.765(4) . ? Si1 C14 1.852(5) . ? Si1 C16 1.859(6) . ? Si1 C15 1.862(6) . ? Si2 N3 1.748(4) . ? Si2 C19 1.856(5) . ? Si2 C18 1.858(5) . ? Si2 C17 1.875(6) . ? Si3 N4 1.712(4) . ? Si3 C21 1.855(5) . ? Si3 C20 1.865(5) . ? Si3 H3 1.42(4) . ? Si4 N4 1.703(4) . ? Si4 C23 1.869(6) . ? Si4 C22 1.870(5) . ? Si4 H4 1.42(5) . ? Si5 N5 1.704(4) . ? Si5 C24 1.859(5) . ? Si5 C25 1.879(5) . ? Si5 H5 1.46(5) . ? Si6 N5 1.686(4) . ? Si6 C26 1.871(6) . ? Si6 C27 1.876(5) . ? Si6 H6 1.38(5) . ? Si7 N8 1.761(4) . ? Si7 C45 1.846(5) . ? Si7 C46 1.847(6) . ? Si7 C47 1.858(6) . ? Si8 N8 1.753(4) . ? Si8 C49 1.856(6) . ? Si8 C48 1.858(6) . ? Si8 C50 1.868(6) . ? Si9 N9 1.697(4) . ? Si9 C52 1.863(5) . ? Si9 C51 1.866(6) . ? Si9 H9 1.51(4) . ? Si10 N9 1.703(4) . ? Si10 C53 1.854(7) . ? Si10 C54 1.867(6) . ? Si10 H10 1.49(5) . ? Si11 N10 1.703(4) . ? Si11 C55 1.866(6) . ? Si11 C56 1.871(5) . ? Si11 H11 1.46(4) . ? Si12 N10 1.690(4) . ? Si12 C57 1.865(5) . ? Si12 C58 1.867(5) . ? Si12 H12 1.40(4) . ? O1 C31 1.448(6) . ? O1 C28 1.453(5) . ? O2 C62 1.446(6) . ? O2 C59 1.460(6) . ? N1 C1 1.344(5) . ? N1 C2 1.463(5) . ? N2 C1 1.339(5) . ? N2 C8 1.461(5) . ? N3 C1 1.438(5) . ? N6 C32 1.339(5) . ? N6 C33 1.454(6) . ? N7 C32 1.324(6) . ? N7 C39 1.470(5) . ? N8 C32 1.440(5) . ? C2 C7 1.524(6) . ? C2 C3 1.532(6) . ? C2 H2 0.9900 . ? C3 C4 1.524(6) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.507(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.513(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.516(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C13 1.518(7) . ? C8 C9 1.530(6) . ? C8 H8 0.9900 . ? C9 C10 1.524(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C11 1.513(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.517(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.528(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 C29 1.489(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.515(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 C31 1.515(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C33 C34 1.527(6) . ? C33 C38 1.537(7) . ? C33 H33 0.9900 . ? C34 C35 1.522(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C35 C36 1.499(7) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 C37 1.515(7) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.518(7) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 C44 1.511(7) . ? C39 C40 1.516(7) . ? C39 H39 0.9900 . ? C40 C41 1.536(7) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 C42 1.524(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 C43 1.480(9) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 C44 1.526(7) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C49 H49C 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 H50C 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C55 H55C 0.9700 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C56 H56C 0.9700 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C57 H57C 0.9700 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C58 H58C 0.9700 . ? C59 C60 1.471(7) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 C61 1.488(8) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C61 C62 1.506(7) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Y1 N5 119.47(14) . . ? N4 Y1 N2 110.26(13) . . ? N5 Y1 N2 102.97(13) . . ? N4 Y1 N1 110.90(13) . . ? N5 Y1 N1 129.62(13) . . ? N2 Y1 N1 57.54(12) . . ? N4 Y1 O1 91.76(12) . . ? N5 Y1 O1 86.95(12) . . ? N2 Y1 O1 146.02(12) . . ? N1 Y1 O1 90.98(12) . . ? N4 Y1 C1 111.72(13) . . ? N5 Y1 C1 121.09(13) . . ? N2 Y1 C1 28.75(12) . . ? N1 Y1 C1 28.91(12) . . ? O1 Y1 C1 119.44(13) . . ? N4 Y1 Si4 30.45(10) . . ? N5 Y1 Si4 99.98(11) . . ? N2 Y1 Si4 94.99(10) . . ? N1 Y1 Si4 125.60(9) . . ? O1 Y1 Si4 115.48(8) . . ? C1 Y1 Si4 110.79(10) . . ? N4 Y1 Si6 145.97(10) . . ? N5 Y1 Si6 26.63(10) . . ? N2 Y1 Si6 89.79(9) . . ? N1 Y1 Si6 103.04(9) . . ? O1 Y1 Si6 85.04(8) . . ? C1 Y1 Si6 99.12(9) . . ? Si4 Y1 Si6 124.67(4) . . ? N4 Y1 Si5 94.19(10) . . ? N5 Y1 Si5 25.50(10) . . ? N2 Y1 Si5 112.05(9) . . ? N1 Y1 Si5 154.76(9) . . ? O1 Y1 Si5 90.92(8) . . ? C1 Y1 Si5 137.94(10) . . ? Si4 Y1 Si5 75.55(4) . . ? Si6 Y1 Si5 52.10(4) . . ? N9 Y2 N10 123.64(14) . . ? N9 Y2 N7 110.02(13) . . ? N10 Y2 N7 101.28(13) . . ? N9 Y2 N6 107.29(14) . . ? N10 Y2 N6 129.07(13) . . ? N7 Y2 N6 57.10(13) . . ? N9 Y2 O2 85.57(12) . . ? N10 Y2 O2 84.65(12) . . ? N7 Y2 O2 155.00(12) . . ? N6 Y2 O2 100.28(12) . . ? N9 Y2 C32 110.20(13) . . ? N10 Y2 C32 118.93(13) . . ? N7 Y2 C32 28.39(12) . . ? N6 Y2 C32 28.76(12) . . ? O2 Y2 C32 128.59(13) . . ? N9 Y2 Si12 151.50(10) . . ? N10 Y2 Si12 31.97(9) . . ? N7 Y2 Si12 93.55(10) . . ? N6 Y2 Si12 98.81(10) . . ? O2 Y2 Si12 78.59(9) . . ? C32 Y2 Si12 98.17(10) . . ? N9 Y2 Si9 31.43(11) . . ? N10 Y2 Si9 101.70(10) . . ? N7 Y2 Si9 96.21(10) . . ? N6 Y2 Si9 124.30(10) . . ? O2 Y2 Si9 106.43(8) . . ? C32 Y2 Si9 111.39(10) . . ? Si12 Y2 Si9 133.63(4) . . ? N9 Y2 H9 59.9(9) . . ? N10 Y2 H9 80.4(9) . . ? N7 Y2 H9 82.2(9) . . ? N6 Y2 H9 131.4(9) . . ? O2 Y2 H9 122.8(9) . . ? C32 Y2 H9 106.7(9) . . ? Si12 Y2 H9 110.1(9) . . ? Si9 Y2 H9 28.4(9) . . ? N3 Si1 C14 108.3(2) . . ? N3 Si1 C16 113.5(2) . . ? C14 Si1 C16 108.6(3) . . ? N3 Si1 C15 110.1(3) . . ? C14 Si1 C15 109.7(3) . . ? C16 Si1 C15 106.6(3) . . ? N3 Si2 C19 109.8(2) . . ? N3 Si2 C18 109.2(2) . . ? C19 Si2 C18 108.0(3) . . ? N3 Si2 C17 112.1(2) . . ? C19 Si2 C17 108.3(3) . . ? C18 Si2 C17 109.4(3) . . ? N4 Si3 C21 113.7(2) . . ? N4 Si3 C20 114.4(2) . . ? C21 Si3 C20 106.8(3) . . ? N4 Si3 H3 108.2(17) . . ? C21 Si3 H3 104.9(17) . . ? C20 Si3 H3 108.3(17) . . ? N4 Si4 C23 117.8(2) . . ? N4 Si4 C22 115.2(2) . . ? C23 Si4 C22 106.2(3) . . ? N4 Si4 Y1 41.83(13) . . ? C23 Si4 Y1 129.3(2) . . ? C22 Si4 Y1 124.5(2) . . ? N4 Si4 H4 102.7(19) . . ? C23 Si4 H4 105.1(19) . . ? C22 Si4 H4 109.2(18) . . ? Y1 Si4 H4 60.9(19) . . ? N5 Si5 C24 114.7(2) . . ? N5 Si5 C25 114.5(2) . . ? C24 Si5 C25 106.5(2) . . ? N5 Si5 Y1 35.15(12) . . ? C24 Si5 Y1 113.07(18) . . ? C25 Si5 Y1 138.18(19) . . ? N5 Si5 H5 107.0(19) . . ? C24 Si5 H5 105.1(18) . . ? C25 Si5 H5 108.4(18) . . ? Y1 Si5 H5 74.0(18) . . ? N5 Si6 C26 115.0(2) . . ? N5 Si6 C27 115.7(2) . . ? C26 Si6 C27 104.0(3) . . ? N5 Si6 Y1 37.27(13) . . ? C26 Si6 Y1 132.36(19) . . ? C27 Si6 Y1 122.51(19) . . ? N5 Si6 H6 106(2) . . ? C26 Si6 H6 113(2) . . ? C27 Si6 H6 103(2) . . ? Y1 Si6 H6 69(2) . . ? N8 Si7 C45 109.6(2) . . ? N8 Si7 C46 110.4(3) . . ? C45 Si7 C46 109.0(4) . . ? N8 Si7 C47 113.3(2) . . ? C45 Si7 C47 107.2(4) . . ? C46 Si7 C47 107.3(4) . . ? N8 Si8 C49 109.9(2) . . ? N8 Si8 C48 112.2(2) . . ? C49 Si8 C48 107.3(3) . . ? N8 Si8 C50 110.9(2) . . ? C49 Si8 C50 108.7(3) . . ? C48 Si8 C50 107.7(3) . . ? N9 Si9 C52 115.6(2) . . ? N9 Si9 C51 115.8(3) . . ? C52 Si9 C51 108.6(3) . . ? N9 Si9 Y2 43.90(13) . . ? C52 Si9 Y2 126.2(2) . . ? C51 Si9 Y2 125.1(2) . . ? N9 Si9 H9 98.8(16) . . ? C52 Si9 H9 109.7(16) . . ? C51 Si9 H9 107.6(15) . . ? Y2 Si9 H9 54.9(16) . . ? N9 Si10 C53 115.5(3) . . ? N9 Si10 C54 114.1(3) . . ? C53 Si10 C54 106.9(3) . . ? N9 Si10 H10 106.5(19) . . ? C53 Si10 H10 110(2) . . ? C54 Si10 H10 103.4(19) . . ? N10 Si11 C55 114.2(3) . . ? N10 Si11 C56 112.9(2) . . ? C55 Si11 C56 106.6(3) . . ? N10 Si11 H11 106.1(15) . . ? C55 Si11 H11 106.6(14) . . ? C56 Si11 H11 110.1(14) . . ? N10 Si12 C57 116.1(2) . . ? N10 Si12 C58 117.2(2) . . ? C57 Si12 C58 107.4(3) . . ? N10 Si12 Y2 45.70(14) . . ? C57 Si12 Y2 121.18(18) . . ? C58 Si12 Y2 131.16(18) . . ? N10 Si12 H12 102.6(17) . . ? C57 Si12 H12 106.6(17) . . ? C58 Si12 H12 105.8(16) . . ? Y2 Si12 H12 57.2(17) . . ? C31 O1 C28 108.4(3) . . ? C31 O1 Y1 127.7(3) . . ? C28 O1 Y1 116.3(3) . . ? C62 O2 C59 108.6(4) . . ? C62 O2 Y2 138.2(3) . . ? C59 O2 Y2 112.2(3) . . ? C1 N1 C2 121.6(4) . . ? C1 N1 Y1 93.2(3) . . ? C2 N1 Y1 143.8(3) . . ? C1 N2 C8 122.1(4) . . ? C1 N2 Y1 94.5(3) . . ? C8 N2 Y1 143.4(3) . . ? C1 N3 Si2 119.6(3) . . ? C1 N3 Si1 116.6(3) . . ? Si2 N3 Si1 123.7(2) . . ? Si4 N4 Si3 123.9(2) . . ? Si4 N4 Y1 107.72(18) . . ? Si3 N4 Y1 128.3(2) . . ? Si6 N5 Si5 124.4(2) . . ? Si6 N5 Y1 116.1(2) . . ? Si5 N5 Y1 119.3(2) . . ? C32 N6 C33 122.2(4) . . ? C32 N6 Y2 93.7(3) . . ? C33 N6 Y2 144.1(3) . . ? C32 N7 C39 122.0(4) . . ? C32 N7 Y2 94.4(3) . . ? C39 N7 Y2 143.5(3) . . ? C32 N8 Si8 119.5(3) . . ? C32 N8 Si7 115.5(3) . . ? Si8 N8 Si7 125.0(2) . . ? Si9 N9 Si10 126.6(2) . . ? Si9 N9 Y2 104.67(19) . . ? Si10 N9 Y2 128.7(2) . . ? Si12 N10 Si11 125.5(2) . . ? Si12 N10 Y2 102.33(19) . . ? Si11 N10 Y2 132.1(2) . . ? N2 C1 N1 114.3(4) . . ? N2 C1 N3 123.0(4) . . ? N1 C1 N3 122.7(4) . . ? N2 C1 Y1 56.7(2) . . ? N1 C1 Y1 57.9(2) . . ? N3 C1 Y1 174.1(3) . . ? N1 C2 C7 111.8(4) . . ? N1 C2 C3 110.1(4) . . ? C7 C2 C3 109.3(4) . . ? N1 C2 H2 108.5 . . ? C7 C2 H2 108.5 . . ? C3 C2 H2 108.5 . . ? C4 C3 C2 112.9(4) . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 112.2(4) . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 C6 110.0(4) . . ? C4 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? C4 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? C5 C6 C7 112.0(5) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 C2 112.4(4) . . ? C6 C7 H7A 109.1 . . ? C2 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? C2 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? N2 C8 C13 111.7(4) . . ? N2 C8 C9 110.6(4) . . ? C13 C8 C9 108.5(4) . . ? N2 C8 H8 108.6 . . ? C13 C8 H8 108.6 . . ? C9 C8 H8 108.6 . . ? C10 C9 C8 111.7(4) . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 111.8(5) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 111.9(5) . . ? C10 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? C10 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C12 C13 110.9(5) . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.0 . . ? C8 C13 C12 111.7(5) . . ? C8 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C8 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si4 C22 H22A 109.5 . . ? Si4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si5 C24 H24A 109.5 . . ? Si5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si5 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si5 C25 H25A 109.5 . . ? Si5 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si5 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si6 C26 H26A 109.5 . . ? Si6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si6 C27 H27A 109.5 . . ? Si6 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si6 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O1 C28 C29 104.3(4) . . ? O1 C28 H28A 110.9 . . ? C29 C28 H28A 110.9 . . ? O1 C28 H28B 110.9 . . ? C29 C28 H28B 110.9 . . ? H28A C28 H28B 108.9 . . ? C28 C29 C30 103.2(4) . . ? C28 C29 H29A 111.1 . . ? C30 C29 H29A 111.1 . . ? C28 C29 H29B 111.1 . . ? C30 C29 H29B 111.1 . . ? H29A C29 H29B 109.1 . . ? C31 C30 C29 103.6(4) . . ? C31 C30 H30A 111.0 . . ? C29 C30 H30A 111.0 . . ? C31 C30 H30B 111.0 . . ? C29 C30 H30B 111.0 . . ? H30A C30 H30B 109.0 . . ? O1 C31 C30 106.8(4) . . ? O1 C31 H31A 110.4 . . ? C30 C31 H31A 110.4 . . ? O1 C31 H31B 110.4 . . ? C30 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? N7 C32 N6 114.6(4) . . ? N7 C32 N8 122.7(4) . . ? N6 C32 N8 122.6(4) . . ? N7 C32 Y2 57.2(2) . . ? N6 C32 Y2 57.6(2) . . ? N8 C32 Y2 174.8(3) . . ? N6 C33 C34 112.4(4) . . ? N6 C33 C38 110.6(4) . . ? C34 C33 C38 108.8(4) . . ? N6 C33 H33 108.3 . . ? C34 C33 H33 108.3 . . ? C38 C33 H33 108.3 . . ? C35 C34 C33 112.9(4) . . ? C35 C34 H34A 109.0 . . ? C33 C34 H34A 109.0 . . ? C35 C34 H34B 109.0 . . ? C33 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? C36 C35 C34 111.7(5) . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35B 109.3 . . ? C34 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? C35 C36 C37 110.3(5) . . ? C35 C36 H36A 109.6 . . ? C37 C36 H36A 109.6 . . ? C35 C36 H36B 109.6 . . ? C37 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? C36 C37 C38 110.8(4) . . ? C36 C37 H37A 109.5 . . ? C38 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C37 C38 C33 113.8(5) . . ? C37 C38 H38A 108.8 . . ? C33 C38 H38A 108.8 . . ? C37 C38 H38B 108.8 . . ? C33 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? N7 C39 C44 110.7(4) . . ? N7 C39 C40 110.3(4) . . ? C44 C39 C40 109.5(5) . . ? N7 C39 H39 108.8 . . ? C44 C39 H39 108.8 . . ? C40 C39 H39 108.8 . . ? C39 C40 C41 110.4(4) . . ? C39 C40 H40A 109.6 . . ? C41 C40 H40A 109.6 . . ? C39 C40 H40B 109.6 . . ? C41 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? C42 C41 C40 110.1(6) . . ? C42 C41 H41A 109.6 . . ? C40 C41 H41A 109.6 . . ? C42 C41 H41B 109.6 . . ? C40 C41 H41B 109.6 . . ? H41A C41 H41B 108.2 . . ? C43 C42 C41 111.3(6) . . ? C43 C42 H42A 109.4 . . ? C41 C42 H42A 109.4 . . ? C43 C42 H42B 109.4 . . ? C41 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C42 C43 C44 111.9(5) . . ? C42 C43 H43A 109.2 . . ? C44 C43 H43A 109.2 . . ? C42 C43 H43B 109.2 . . ? C44 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? C39 C44 C43 111.6(5) . . ? C39 C44 H44A 109.3 . . ? C43 C44 H44A 109.3 . . ? C39 C44 H44B 109.3 . . ? C43 C44 H44B 109.3 . . ? H44A C44 H44B 108.0 . . ? Si7 C45 H45A 109.5 . . ? Si7 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si7 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si7 C46 H46A 109.5 . . ? Si7 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si7 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si7 C47 H47A 109.5 . . ? Si7 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si7 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si8 C48 H48A 109.5 . . ? Si8 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si8 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Si8 C49 H49A 109.5 . . ? Si8 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? Si8 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? Si8 C50 H50A 109.5 . . ? Si8 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si8 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Si9 C51 H51A 109.5 . . ? Si9 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si9 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si9 C52 H52A 109.5 . . ? Si9 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si9 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si10 C53 H53A 109.5 . . ? Si10 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si10 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? Si10 C54 H54A 109.5 . . ? Si10 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? Si10 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Si11 C55 H55A 109.5 . . ? Si11 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? Si11 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? Si11 C56 H56A 109.5 . . ? Si11 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? Si11 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? Si12 C57 H57A 109.5 . . ? Si12 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? Si12 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? Si12 C58 H58A 109.5 . . ? Si12 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? Si12 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O2 C59 C60 106.6(5) . . ? O2 C59 H59A 110.4 . . ? C60 C59 H59A 110.4 . . ? O2 C59 H59B 110.4 . . ? C60 C59 H59B 110.4 . . ? H59A C59 H59B 108.6 . . ? C59 C60 C61 104.6(5) . . ? C59 C60 H60A 110.8 . . ? C61 C60 H60A 110.8 . . ? C59 C60 H60B 110.8 . . ? C61 C60 H60B 110.8 . . ? H60A C60 H60B 108.9 . . ? C60 C61 C62 103.1(5) . . ? C60 C61 H61A 111.1 . . ? C62 C61 H61A 111.1 . . ? C60 C61 H61B 111.1 . . ? C62 C61 H61B 111.1 . . ? H61A C61 H61B 109.1 . . ? O2 C62 C61 105.1(4) . . ? O2 C62 H62A 110.7 . . ? C61 C62 H62A 110.7 . . ? O2 C62 H62B 110.7 . . ? C61 C62 H62B 110.7 . . ? H62A C62 H62B 108.8 . . ? 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 N5 Y1 Si4 N4 -133.4(2) . . . . ? N2 Y1 Si4 N4 122.5(2) . . . . ? N1 Y1 Si4 N4 69.4(2) . . . . ? O1 Y1 Si4 N4 -42.0(2) . . . . ? C1 Y1 Si4 N4 97.8(2) . . . . ? Si6 Y1 Si4 N4 -144.28(18) . . . . ? Si5 Y1 Si4 N4 -125.98(18) . . . . ? N4 Y1 Si4 C23 89.3(3) . . . . ? N5 Y1 Si4 C23 -44.0(3) . . . . ? N2 Y1 Si4 C23 -148.2(3) . . . . ? N1 Y1 Si4 C23 158.7(3) . . . . ? O1 Y1 Si4 C23 47.4(3) . . . . ? C1 Y1 Si4 C23 -172.9(3) . . . . ? Si6 Y1 Si4 C23 -54.9(3) . . . . ? Si5 Y1 Si4 C23 -36.6(3) . . . . ? N4 Y1 Si4 C22 -90.4(3) . . . . ? N5 Y1 Si4 C22 136.2(2) . . . . ? N2 Y1 Si4 C22 32.1(2) . . . . ? N1 Y1 Si4 C22 -21.0(3) . . . . ? O1 Y1 Si4 C22 -132.4(2) . . . . ? C1 Y1 Si4 C22 7.4(2) . . . . ? Si6 Y1 Si4 C22 125.3(2) . . . . ? Si5 Y1 Si4 C22 143.6(2) . . . . ? N4 Y1 Si5 N5 172.8(2) . . . . ? N2 Y1 Si5 N5 -73.4(2) . . . . ? N1 Y1 Si5 N5 -13.3(3) . . . . ? O1 Y1 Si5 N5 81.0(2) . . . . ? C1 Y1 Si5 N5 -57.8(3) . . . . ? Si4 Y1 Si5 N5 -162.9(2) . . . . ? Si6 Y1 Si5 N5 -2.0(2) . . . . ? N4 Y1 Si5 C24 -86.7(2) . . . . ? N5 Y1 Si5 C24 100.6(3) . . . . ? N2 Y1 Si5 C24 27.2(2) . . . . ? N1 Y1 Si5 C24 87.3(3) . . . . ? O1 Y1 Si5 C24 -178.5(2) . . . . ? C1 Y1 Si5 C24 42.8(3) . . . . ? Si4 Y1 Si5 C24 -62.4(2) . . . . ? Si6 Y1 Si5 C24 98.5(2) . . . . ? N4 Y1 Si5 C25 113.2(3) . . . . ? N5 Y1 Si5 C25 -59.6(4) . . . . ? N2 Y1 Si5 C25 -132.9(3) . . . . ? N1 Y1 Si5 C25 -72.8(4) . . . . ? O1 Y1 Si5 C25 21.4(3) . . . . ? C1 Y1 Si5 C25 -117.3(3) . . . . ? Si4 Y1 Si5 C25 137.5(3) . . . . ? Si6 Y1 Si5 C25 -61.6(3) . . . . ? N4 Y1 Si6 N5 -7.3(3) . . . . ? N2 Y1 Si6 N5 120.5(2) . . . . ? N1 Y1 Si6 N5 177.0(2) . . . . ? O1 Y1 Si6 N5 -93.1(2) . . . . ? C1 Y1 Si6 N5 147.8(2) . . . . ? Si4 Y1 Si6 N5 24.6(2) . . . . ? Si5 Y1 Si6 N5 1.9(2) . . . . ? N4 Y1 Si6 C26 -82.7(3) . . . . ? N5 Y1 Si6 C26 -75.3(3) . . . . ? N2 Y1 Si6 C26 45.2(3) . . . . ? N1 Y1 Si6 C26 101.7(3) . . . . ? O1 Y1 Si6 C26 -168.5(3) . . . . ? C1 Y1 Si6 C26 72.5(3) . . . . ? Si4 Y1 Si6 C26 -50.7(3) . . . . ? Si5 Y1 Si6 C26 -73.4(3) . . . . ? N4 Y1 Si6 C27 83.3(3) . . . . ? N5 Y1 Si6 C27 90.6(3) . . . . ? N2 Y1 Si6 C27 -148.8(3) . . . . ? N1 Y1 Si6 C27 -92.3(3) . . . . ? O1 Y1 Si6 C27 -2.5(2) . . . . ? C1 Y1 Si6 C27 -121.5(3) . . . . ? Si4 Y1 Si6 C27 115.2(2) . . . . ? Si5 Y1 Si6 C27 92.6(2) . . . . ? N10 Y2 Si9 N9 -138.3(2) . . . . ? N7 Y2 Si9 N9 118.8(2) . . . . ? N6 Y2 Si9 N9 64.8(2) . . . . ? O2 Y2 Si9 N9 -50.4(2) . . . . ? C32 Y2 Si9 N9 94.0(2) . . . . ? Si12 Y2 Si9 N9 -140.23(19) . . . . ? N9 Y2 Si9 C52 90.6(3) . . . . ? N10 Y2 Si9 C52 -47.6(3) . . . . ? N7 Y2 Si9 C52 -150.5(3) . . . . ? N6 Y2 Si9 C52 155.4(3) . . . . ? O2 Y2 Si9 C52 40.2(3) . . . . ? C32 Y2 Si9 C52 -175.3(3) . . . . ? Si12 Y2 Si9 C52 -49.6(3) . . . . ? N9 Y2 Si9 C51 -92.1(3) . . . . ? N10 Y2 Si9 C51 129.6(3) . . . . ? N7 Y2 Si9 C51 26.7(3) . . . . ? N6 Y2 Si9 C51 -27.3(3) . . . . ? O2 Y2 Si9 C51 -142.5(3) . . . . ? C32 Y2 Si9 C51 1.9(3) . . . . ? Si12 Y2 Si9 C51 127.7(3) . . . . ? N9 Y2 Si12 N10 -40.7(3) . . . . ? N7 Y2 Si12 N10 105.7(2) . . . . ? N6 Y2 Si12 N10 162.9(2) . . . . ? O2 Y2 Si12 N10 -98.26(19) . . . . ? C32 Y2 Si12 N10 133.9(2) . . . . ? Si9 Y2 Si12 N10 3.65(19) . . . . ? N9 Y2 Si12 C57 56.7(3) . . . . ? N10 Y2 Si12 C57 97.4(3) . . . . ? N7 Y2 Si12 C57 -156.9(3) . . . . ? N6 Y2 Si12 C57 -99.7(3) . . . . ? O2 Y2 Si12 C57 -0.9(3) . . . . ? C32 Y2 Si12 C57 -128.7(3) . . . . ? Si9 Y2 Si12 C57 101.0(2) . . . . ? N9 Y2 Si12 C58 -130.5(4) . . . . ? N10 Y2 Si12 C58 -89.7(3) . . . . ? N7 Y2 Si12 C58 16.0(3) . . . . ? N6 Y2 Si12 C58 73.2(3) . . . . ? O2 Y2 Si12 C58 172.0(3) . . . . ? C32 Y2 Si12 C58 44.1(3) . . . . ? Si9 Y2 Si12 C58 -86.1(3) . . . . ? N4 Y1 O1 C31 163.5(4) . . . . ? N5 Y1 O1 C31 -77.1(4) . . . . ? N2 Y1 O1 C31 31.7(4) . . . . ? N1 Y1 O1 C31 52.5(4) . . . . ? C1 Y1 O1 C31 47.2(4) . . . . ? Si4 Y1 O1 C31 -176.7(3) . . . . ? Si6 Y1 O1 C31 -50.5(3) . . . . ? Si5 Y1 O1 C31 -102.3(3) . . . . ? N4 Y1 O1 C28 -50.7(3) . . . . ? N5 Y1 O1 C28 68.8(3) . . . . ? N2 Y1 O1 C28 177.6(3) . . . . ? N1 Y1 O1 C28 -161.6(3) . . . . ? C1 Y1 O1 C28 -166.9(3) . . . . ? Si4 Y1 O1 C28 -30.9(3) . . . . ? Si6 Y1 O1 C28 95.4(3) . . . . ? Si5 Y1 O1 C28 43.6(3) . . . . ? N9 Y2 O2 C62 100.0(5) . . . . ? N10 Y2 O2 C62 -135.6(5) . . . . ? N7 Y2 O2 C62 -30.3(6) . . . . ? N6 Y2 O2 C62 -6.8(5) . . . . ? C32 Y2 O2 C62 -12.4(5) . . . . ? Si12 Y2 O2 C62 -103.8(5) . . . . ? Si9 Y2 O2 C62 123.8(5) . . . . ? N9 Y2 O2 C59 -67.3(3) . . . . ? N10 Y2 O2 C59 57.1(3) . . . . ? N7 Y2 O2 C59 162.5(4) . . . . ? N6 Y2 O2 C59 -174.1(3) . . . . ? C32 Y2 O2 C59 -179.7(3) . . . . ? Si12 Y2 O2 C59 88.9(3) . . . . ? Si9 Y2 O2 C59 -43.5(3) . . . . ? N4 Y1 N1 C1 97.4(3) . . . . ? N5 Y1 N1 C1 -83.5(3) . . . . ? N2 Y1 N1 C1 -4.0(2) . . . . ? O1 Y1 N1 C1 -170.4(3) . . . . ? Si4 Y1 N1 C1 66.8(3) . . . . ? Si6 Y1 N1 C1 -85.3(2) . . . . ? Si5 Y1 N1 C1 -76.2(3) . . . . ? N4 Y1 N1 C2 -67.7(5) . . . . ? N5 Y1 N1 C2 111.4(5) . . . . ? N2 Y1 N1 C2 -169.0(5) . . . . ? O1 Y1 N1 C2 24.6(5) . . . . ? C1 Y1 N1 C2 -165.0(6) . . . . ? Si4 Y1 N1 C2 -98.2(5) . . . . ? Si6 Y1 N1 C2 109.7(5) . . . . ? Si5 Y1 N1 C2 118.8(4) . . . . ? N4 Y1 N2 C1 -98.5(3) . . . . ? N5 Y1 N2 C1 133.0(3) . . . . ? N1 Y1 N2 C1 4.0(2) . . . . ? O1 Y1 N2 C1 28.9(4) . . . . ? Si4 Y1 N2 C1 -125.6(2) . . . . ? Si6 Y1 N2 C1 109.6(3) . . . . ? Si5 Y1 N2 C1 158.0(2) . . . . ? N4 Y1 N2 C8 84.1(5) . . . . ? N5 Y1 N2 C8 -44.4(5) . . . . ? N1 Y1 N2 C8 -173.4(5) . . . . ? O1 Y1 N2 C8 -148.6(4) . . . . ? C1 Y1 N2 C8 -177.4(6) . . . . ? Si4 Y1 N2 C8 57.0(5) . . . . ? Si6 Y1 N2 C8 -67.8(5) . . . . ? Si5 Y1 N2 C8 -19.4(5) . . . . ? C19 Si2 N3 C1 -126.1(4) . . . . ? C18 Si2 N3 C1 -7.9(4) . . . . ? C17 Si2 N3 C1 113.5(4) . . . . ? C19 Si2 N3 Si1 50.4(3) . . . . ? C18 Si2 N3 Si1 168.6(3) . . . . ? C17 Si2 N3 Si1 -70.0(3) . . . . ? C14 Si1 N3 C1 -13.5(4) . . . . ? C16 Si1 N3 C1 107.1(4) . . . . ? C15 Si1 N3 C1 -133.5(4) . . . . ? C14 Si1 N3 Si2 169.9(3) . . . . ? C16 Si1 N3 Si2 -69.5(4) . . . . ? C15 Si1 N3 Si2 50.0(4) . . . . ? C23 Si4 N4 Si3 63.7(3) . . . . ? C22 Si4 N4 Si3 -62.9(3) . . . . ? Y1 Si4 N4 Si3 -177.2(4) . . . . ? C23 Si4 N4 Y1 -119.0(2) . . . . ? C22 Si4 N4 Y1 114.3(3) . . . . ? C21 Si3 N4 Si4 -55.1(3) . . . . ? C20 Si3 N4 Si4 68.0(4) . . . . ? C21 Si3 N4 Y1 128.3(3) . . . . ? C20 Si3 N4 Y1 -108.7(3) . . . . ? N5 Y1 N4 Si4 55.3(2) . . . . ? N2 Y1 N4 Si4 -63.6(2) . . . . ? N1 Y1 N4 Si4 -125.44(17) . . . . ? O1 Y1 N4 Si4 142.83(17) . . . . ? C1 Y1 N4 Si4 -94.37(19) . . . . ? Si6 Y1 N4 Si4 59.1(3) . . . . ? Si5 Y1 N4 Si4 51.78(17) . . . . ? N5 Y1 N4 Si3 -127.6(2) . . . . ? N2 Y1 N4 Si3 113.5(2) . . . . ? N1 Y1 N4 Si3 51.6(3) . . . . ? O1 Y1 N4 Si3 -40.1(2) . . . . ? C1 Y1 N4 Si3 82.7(3) . . . . ? Si4 Y1 N4 Si3 177.1(4) . . . . ? Si6 Y1 N4 Si3 -123.8(2) . . . . ? Si5 Y1 N4 Si3 -131.1(2) . . . . ? C26 Si6 N5 Si5 -48.3(4) . . . . ? C27 Si6 N5 Si5 73.1(3) . . . . ? Y1 Si6 N5 Si5 -176.2(4) . . . . ? C26 Si6 N5 Y1 127.9(2) . . . . ? C27 Si6 N5 Y1 -110.7(3) . . . . ? C24 Si5 N5 Si6 80.6(3) . . . . ? C25 Si5 N5 Si6 -43.1(4) . . . . ? Y1 Si5 N5 Si6 176.1(4) . . . . ? C24 Si5 N5 Y1 -95.5(3) . . . . ? C25 Si5 N5 Y1 140.8(2) . . . . ? N4 Y1 N5 Si6 175.30(18) . . . . ? N2 Y1 N5 Si6 -62.1(2) . . . . ? N1 Y1 N5 Si6 -3.7(3) . . . . ? O1 Y1 N5 Si6 85.0(2) . . . . ? C1 Y1 N5 Si6 -37.9(3) . . . . ? Si4 Y1 N5 Si6 -159.66(18) . . . . ? Si5 Y1 N5 Si6 -176.4(4) . . . . ? N4 Y1 N5 Si5 -8.3(3) . . . . ? N2 Y1 N5 Si5 114.3(2) . . . . ? N1 Y1 N5 Si5 172.69(17) . . . . ? O1 Y1 N5 Si5 -98.6(2) . . . . ? C1 Y1 N5 Si5 138.6(2) . . . . ? Si4 Y1 N5 Si5 16.8(2) . . . . ? Si6 Y1 N5 Si5 176.4(4) . . . . ? N9 Y2 N6 C32 100.6(3) . . . . ? N10 Y2 N6 C32 -79.4(3) . . . . ? N7 Y2 N6 C32 -2.4(3) . . . . ? O2 Y2 N6 C32 -170.8(3) . . . . ? Si12 Y2 N6 C32 -90.9(3) . . . . ? Si9 Y2 N6 C32 71.0(3) . . . . ? N9 Y2 N6 C33 -76.2(5) . . . . ? N10 Y2 N6 C33 103.8(5) . . . . ? N7 Y2 N6 C33 -179.2(6) . . . . ? O2 Y2 N6 C33 12.4(5) . . . . ? C32 Y2 N6 C33 -176.8(7) . . . . ? Si12 Y2 N6 C33 92.3(5) . . . . ? Si9 Y2 N6 C33 -105.8(5) . . . . ? N9 Y2 N7 C32 -95.7(3) . . . . ? N10 Y2 N7 C32 131.9(3) . . . . ? N6 Y2 N7 C32 2.4(3) . . . . ? O2 Y2 N7 C32 30.2(5) . . . . ? Si12 Y2 N7 C32 100.6(3) . . . . ? Si9 Y2 N7 C32 -124.8(3) . . . . ? N9 Y2 N7 C39 85.0(5) . . . . ? N10 Y2 N7 C39 -47.3(5) . . . . ? N6 Y2 N7 C39 -176.8(6) . . . . ? O2 Y2 N7 C39 -149.0(4) . . . . ? C32 Y2 N7 C39 -179.3(7) . . . . ? Si12 Y2 N7 C39 -78.6(5) . . . . ? Si9 Y2 N7 C39 56.0(5) . . . . ? C49 Si8 N8 C32 -3.2(4) . . . . ? C48 Si8 N8 C32 116.1(4) . . . . ? C50 Si8 N8 C32 -123.4(4) . . . . ? C49 Si8 N8 Si7 175.0(3) . . . . ? C48 Si8 N8 Si7 -65.7(4) . . . . ? C50 Si8 N8 Si7 54.8(4) . . . . ? C45 Si7 N8 C32 -5.7(4) . . . . ? C46 Si7 N8 C32 -125.7(4) . . . . ? C47 Si7 N8 C32 113.9(4) . . . . ? C45 Si7 N8 Si8 176.0(3) . . . . ? C46 Si7 N8 Si8 55.9(4) . . . . ? C47 Si7 N8 Si8 -64.4(4) . . . . ? C52 Si9 N9 Si10 64.1(4) . . . . ? C51 Si9 N9 Si10 -64.5(4) . . . . ? Y2 Si9 N9 Si10 -179.3(4) . . . . ? C52 Si9 N9 Y2 -116.5(3) . . . . ? C51 Si9 N9 Y2 114.8(3) . . . . ? C53 Si10 N9 Si9 68.9(4) . . . . ? C54 Si10 N9 Si9 -55.5(4) . . . . ? C53 Si10 N9 Y2 -110.2(4) . . . . ? C54 Si10 N9 Y2 125.4(3) . . . . ? N10 Y2 N9 Si9 51.6(2) . . . . ? N7 Y2 N9 Si9 -68.0(2) . . . . ? N6 Y2 N9 Si9 -128.48(18) . . . . ? O2 Y2 N9 Si9 132.12(19) . . . . ? C32 Y2 N9 Si9 -98.2(2) . . . . ? Si12 Y2 N9 Si9 76.1(3) . . . . ? N10 Y2 N9 Si10 -129.1(2) . . . . ? N7 Y2 N9 Si10 111.4(3) . . . . ? N6 Y2 N9 Si10 50.8(3) . . . . ? O2 Y2 N9 Si10 -48.6(3) . . . . ? C32 Y2 N9 Si10 81.1(3) . . . . ? Si12 Y2 N9 Si10 -104.6(3) . . . . ? Si9 Y2 N9 Si10 179.3(4) . . . . ? C57 Si12 N10 Si11 71.1(4) . . . . ? C58 Si12 N10 Si11 -57.7(4) . . . . ? Y2 Si12 N10 Si11 -179.8(4) . . . . ? C57 Si12 N10 Y2 -109.1(2) . . . . ? C58 Si12 N10 Y2 122.2(2) . . . . ? C55 Si11 N10 Si12 -28.8(4) . . . . ? C56 Si11 N10 Si12 93.2(3) . . . . ? C55 Si11 N10 Y2 151.4(3) . . . . ? C56 Si11 N10 Y2 -86.6(3) . . . . ? N9 Y2 N10 Si12 158.04(16) . . . . ? N7 Y2 N10 Si12 -78.45(18) . . . . ? N6 Y2 N10 Si12 -21.9(2) . . . . ? O2 Y2 N10 Si12 76.99(17) . . . . ? C32 Y2 N10 Si12 -54.6(2) . . . . ? Si9 Y2 N10 Si12 -177.31(14) . . . . ? N9 Y2 N10 Si11 -22.1(3) . . . . ? N7 Y2 N10 Si11 101.4(3) . . . . ? N6 Y2 N10 Si11 157.9(2) . . . . ? O2 Y2 N10 Si11 -103.2(3) . . . . ? C32 Y2 N10 Si11 125.2(3) . . . . ? Si12 Y2 N10 Si11 179.8(4) . . . . ? Si9 Y2 N10 Si11 2.5(3) . . . . ? C8 N2 C1 N1 171.7(4) . . . . ? Y1 N2 C1 N1 -6.5(4) . . . . ? C8 N2 C1 N3 -8.9(6) . . . . ? Y1 N2 C1 N3 172.9(4) . . . . ? C8 N2 C1 Y1 178.2(4) . . . . ? C2 N1 C1 N2 176.1(4) . . . . ? Y1 N1 C1 N2 6.4(4) . . . . ? C2 N1 C1 N3 -3.3(6) . . . . ? Y1 N1 C1 N3 -173.0(4) . . . . ? C2 N1 C1 Y1 169.7(4) . . . . ? Si2 N3 C1 N2 92.7(5) . . . . ? Si1 N3 C1 N2 -84.1(5) . . . . ? Si2 N3 C1 N1 -88.0(5) . . . . ? Si1 N3 C1 N1 95.3(5) . . . . ? Si2 N3 C1 Y1 178(3) . . . . ? Si1 N3 C1 Y1 1(3) . . . . ? N4 Y1 C1 N2 92.8(3) . . . . ? N5 Y1 C1 N2 -56.4(3) . . . . ? N1 Y1 C1 N2 -173.0(4) . . . . ? O1 Y1 C1 N2 -162.0(2) . . . . ? Si4 Y1 C1 N2 60.1(3) . . . . ? Si6 Y1 C1 N2 -72.5(3) . . . . ? Si5 Y1 C1 N2 -31.2(3) . . . . ? N4 Y1 C1 N1 -94.2(3) . . . . ? N5 Y1 C1 N1 116.7(3) . . . . ? N2 Y1 C1 N1 173.0(4) . . . . ? O1 Y1 C1 N1 11.1(3) . . . . ? Si4 Y1 C1 N1 -126.9(2) . . . . ? Si6 Y1 C1 N1 100.5(2) . . . . ? Si5 Y1 C1 N1 141.8(2) . . . . ? N4 Y1 C1 N3 4(3) . . . . ? N5 Y1 C1 N3 -146(3) . . . . ? N2 Y1 C1 N3 -89(3) . . . . ? N1 Y1 C1 N3 98(3) . . . . ? O1 Y1 C1 N3 109(3) . . . . ? Si4 Y1 C1 N3 -29(3) . . . . ? Si6 Y1 C1 N3 -162(3) . . . . ? Si5 Y1 C1 N3 -120(3) . . . . ? C1 N1 C2 C7 104.3(5) . . . . ? Y1 N1 C2 C7 -93.3(5) . . . . ? C1 N1 C2 C3 -134.0(4) . . . . ? Y1 N1 C2 C3 28.3(6) . . . . ? N1 C2 C3 C4 -175.7(4) . . . . ? C7 C2 C3 C4 -52.6(5) . . . . ? C2 C3 C4 C5 54.6(6) . . . . ? C3 C4 C5 C6 -54.7(6) . . . . ? C4 C5 C6 C7 56.0(6) . . . . ? C5 C6 C7 C2 -56.9(6) . . . . ? N1 C2 C7 C6 175.8(4) . . . . ? C3 C2 C7 C6 53.7(5) . . . . ? C1 N2 C8 C13 116.9(5) . . . . ? Y1 N2 C8 C13 -66.1(6) . . . . ? C1 N2 C8 C9 -122.1(5) . . . . ? Y1 N2 C8 C9 54.9(6) . . . . ? N2 C8 C9 C10 179.8(5) . . . . ? C13 C8 C9 C10 -57.3(6) . . . . ? C8 C9 C10 C11 55.2(7) . . . . ? C9 C10 C11 C12 -52.7(7) . . . . ? C10 C11 C12 C13 53.3(8) . . . . ? N2 C8 C13 C12 -179.3(4) . . . . ? C9 C8 C13 C12 58.5(6) . . . . ? C11 C12 C13 C8 -57.2(7) . . . . ? C31 O1 C28 C29 28.5(5) . . . . ? Y1 O1 C28 C29 -123.7(3) . . . . ? O1 C28 C29 C30 -37.3(5) . . . . ? C28 C29 C30 C31 32.0(5) . . . . ? C28 O1 C31 C30 -7.9(5) . . . . ? Y1 O1 C31 C30 140.1(3) . . . . ? C29 C30 C31 O1 -15.3(5) . . . . ? C39 N7 C32 N6 175.5(4) . . . . ? Y2 N7 C32 N6 -3.9(4) . . . . ? C39 N7 C32 N8 -6.7(7) . . . . ? Y2 N7 C32 N8 173.9(4) . . . . ? C39 N7 C32 Y2 179.5(5) . . . . ? C33 N6 C32 N7 -178.3(4) . . . . ? Y2 N6 C32 N7 3.9(4) . . . . ? C33 N6 C32 N8 3.9(7) . . . . ? Y2 N6 C32 N8 -173.9(3) . . . . ? C33 N6 C32 Y2 177.8(5) . . . . ? Si8 N8 C32 N7 96.3(5) . . . . ? Si7 N8 C32 N7 -82.1(5) . . . . ? Si8 N8 C32 N6 -86.1(5) . . . . ? Si7 N8 C32 N6 95.5(4) . . . . ? Si8 N8 C32 Y2 -176(3) . . . . ? Si7 N8 C32 Y2 5(4) . . . . ? N9 Y2 C32 N7 94.9(3) . . . . ? N10 Y2 C32 N7 -56.4(3) . . . . ? N6 Y2 C32 N7 -175.8(4) . . . . ? O2 Y2 C32 N7 -164.2(2) . . . . ? Si12 Y2 C32 N7 -82.3(3) . . . . ? Si9 Y2 C32 N7 61.3(3) . . . . ? N9 Y2 C32 N6 -89.3(3) . . . . ? N10 Y2 C32 N6 119.3(3) . . . . ? N7 Y2 C32 N6 175.8(4) . . . . ? O2 Y2 C32 N6 11.6(3) . . . . ? Si12 Y2 C32 N6 93.4(3) . . . . ? Si9 Y2 C32 N6 -123.0(2) . . . . ? N9 Y2 C32 N8 4(4) . . . . ? N10 Y2 C32 N8 -147(4) . . . . ? N7 Y2 C32 N8 -91(4) . . . . ? N6 Y2 C32 N8 94(4) . . . . ? O2 Y2 C32 N8 105(4) . . . . ? Si12 Y2 C32 N8 -173(4) . . . . ? Si9 Y2 C32 N8 -29(4) . . . . ? C32 N6 C33 C34 -117.9(5) . . . . ? Y2 N6 C33 C34 58.4(7) . . . . ? C32 N6 C33 C38 120.4(5) . . . . ? Y2 N6 C33 C38 -63.4(6) . . . . ? N6 C33 C34 C35 -174.8(4) . . . . ? C38 C33 C34 C35 -52.0(6) . . . . ? C33 C34 C35 C36 56.5(6) . . . . ? C34 C35 C36 C37 -57.2(6) . . . . ? C35 C36 C37 C38 56.4(7) . . . . ? C36 C37 C38 C33 -55.4(7) . . . . ? N6 C33 C38 C37 176.1(4) . . . . ? C34 C33 C38 C37 52.3(6) . . . . ? C32 N7 C39 C44 131.3(5) . . . . ? Y2 N7 C39 C44 -49.5(7) . . . . ? C32 N7 C39 C40 -107.3(5) . . . . ? Y2 N7 C39 C40 71.8(6) . . . . ? N7 C39 C40 C41 179.6(5) . . . . ? C44 C39 C40 C41 -58.3(7) . . . . ? C39 C40 C41 C42 58.1(8) . . . . ? C40 C41 C42 C43 -56.1(7) . . . . ? C41 C42 C43 C44 54.6(7) . . . . ? N7 C39 C44 C43 178.4(5) . . . . ? C40 C39 C44 C43 56.6(6) . . . . ? C42 C43 C44 C39 -55.4(8) . . . . ? C62 O2 C59 C60 4.9(6) . . . . ? Y2 O2 C59 C60 175.9(4) . . . . ? O2 C59 C60 C61 -24.6(7) . . . . ? C59 C60 C61 C62 34.2(7) . . . . ? C59 O2 C62 C61 16.6(6) . . . . ? Y2 O2 C62 C61 -150.9(4) . . . . ? C60 C61 C62 O2 -31.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.645 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.071