# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yaofeng Chen' _publ_contact_author_email YAOFCHEN@MAIL.SIOC.AC.CN _publ_section_title ; Single, double and triple deprotonation of a beta-diketimine bearing pendant pyridine group and the corresponding rare-earth metal complexes ; loop_ _publ_author_name 'Yaofeng Chen' 'Jie Sun' 'Xin Xu' 'Gang Zou' # Attachment 'CIF.cif' data_cd29139 _database_code_depnum_ccdc_archive 'CCDC 744083' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H52 N3 Sc Si2' _chemical_formula_weight 567.90 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6221(12) _cell_length_b 10.3910(12) _cell_length_c 18.515(2) _cell_angle_alpha 77.516(2) _cell_angle_beta 81.161(2) _cell_angle_gamma 72.257(2) _cell_volume 1713.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2547 _cell_measurement_theta_min 4.811 _cell_measurement_theta_max 47.854 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.347 _exptl_crystal_size_mid 0.311 _exptl_crystal_size_min 0.127 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.307 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.82807 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9448 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6612 _reflns_number_gt 4520 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6612 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc Sc 0.17037(5) 0.26228(5) 0.23184(3) 0.03533(15) Uani 1 1 d . . . Si1 Si 0.20383(9) 0.40362(9) 0.38648(4) 0.0497(2) Uani 1 1 d . . . Si2 Si 0.50234(8) 0.19753(9) 0.09191(4) 0.0508(2) Uani 1 1 d . . . N1 N 0.1511(2) 0.0615(2) 0.29350(11) 0.0363(5) Uani 1 1 d . . . N2 N -0.0683(2) 0.3264(2) 0.25910(12) 0.0444(6) Uani 1 1 d . . . N3 N 0.0762(2) 0.4586(2) 0.14800(12) 0.0497(6) Uani 1 1 d . . . C1 C 0.0618(4) -0.0937(3) 0.39829(16) 0.0667(9) Uani 1 1 d . . . H1A H 0.1200 -0.1650 0.3719 0.100 Uiso 1 1 calc R . . H1B H -0.0342 -0.1057 0.4128 0.100 Uiso 1 1 calc R . . H1C H 0.1075 -0.0983 0.4417 0.100 Uiso 1 1 calc R . . C2 C 0.0496(3) 0.0440(3) 0.34885(14) 0.0448(7) Uani 1 1 d . . . C3 C -0.0769(3) 0.1476(3) 0.36430(16) 0.0530(8) Uani 1 1 d . . . H3 H -0.1282 0.1297 0.4104 0.064 Uiso 1 1 calc R . . C4 C -0.1364(3) 0.2730(3) 0.32075(17) 0.0507(7) Uani 1 1 d . . . C5 C -0.2914(3) 0.3481(4) 0.3473(2) 0.0798(11) Uani 1 1 d . . . H5A H -0.2936 0.4371 0.3550 0.120 Uiso 1 1 calc R . . H5B H -0.3225 0.2963 0.3931 0.120 Uiso 1 1 calc R . . H5C H -0.3561 0.3582 0.3105 0.120 Uiso 1 1 calc R . . C6 C -0.1554(3) 0.4524(3) 0.21620(18) 0.0598(8) Uani 1 1 d . . . H6A H -0.1984 0.5191 0.2486 0.072 Uiso 1 1 calc R . . H6B H -0.2348 0.4327 0.1982 0.072 Uiso 1 1 calc R . . C7 C -0.0688(3) 0.5130(3) 0.15229(16) 0.0502(7) Uani 1 1 d . . . C8 C 0.1563(4) 0.5165(3) 0.09179(17) 0.0660(9) Uani 1 1 d . . . H8 H 0.2577 0.4806 0.0885 0.079 Uiso 1 1 calc R . . C9 C -0.1361(4) 0.6235(3) 0.1017(2) 0.0745(10) Uani 1 1 d . . . H9 H -0.2374 0.6603 0.1065 0.089 Uiso 1 1 calc R . . C10 C 0.2529(3) -0.0621(3) 0.27236(13) 0.0379(6) Uani 1 1 d . . . C11 C 0.2130(3) -0.1209(3) 0.22119(14) 0.0445(7) Uani 1 1 d . . . C12 C 0.3109(3) -0.2393(3) 0.19987(16) 0.0582(8) Uani 1 1 d . . . H12 H 0.2850 -0.2815 0.1666 0.070 Uiso 1 1 calc R . . C13 C 0.4449(4) -0.2938(3) 0.22740(19) 0.0678(9) Uani 1 1 d . . . H13 H 0.5098 -0.3723 0.2125 0.081 Uiso 1 1 calc R . . C14 C 0.4830(3) -0.2333(3) 0.27661(18) 0.0621(9) Uani 1 1 d . . . H14 H 0.5745 -0.2712 0.2946 0.074 Uiso 1 1 calc R . . C15 C 0.3894(3) -0.1168(3) 0.30065(15) 0.0468(7) Uani 1 1 d . . . C16 C 0.0662(3) -0.0619(3) 0.18808(17) 0.0623(9) Uani 1 1 d . . . H16 H 0.0179 0.0263 0.2041 0.075 Uiso 1 1 calc R . . C17 C -0.0335(4) -0.1543(5) 0.2165(2) 0.1114(16) Uani 1 1 d . . . H17A H -0.1287 -0.1093 0.1994 0.167 Uiso 1 1 calc R . . H17B H -0.0421 -0.1729 0.2698 0.167 Uiso 1 1 calc R . . H17C H 0.0072 -0.2391 0.1982 0.167 Uiso 1 1 calc R . . C18 C 0.0840(4) -0.0349(4) 0.10397(18) 0.0868(12) Uani 1 1 d . . . H18A H 0.1539 0.0166 0.0865 0.130 Uiso 1 1 calc R . . H18B H -0.0087 0.0165 0.0855 0.130 Uiso 1 1 calc R . . H18C H 0.1181 -0.1208 0.0865 0.130 Uiso 1 1 calc R . . C19 C 0.4350(3) -0.0565(3) 0.35698(17) 0.0615(8) Uani 1 1 d . . . H19 H 0.3569 0.0267 0.3650 0.074 Uiso 1 1 calc R . . C20 C 0.5750(4) -0.0152(4) 0.3308(2) 0.1025(14) Uani 1 1 d . . . H20A H 0.6555 -0.0958 0.3269 0.154 Uiso 1 1 calc R . . H20B H 0.5928 0.0326 0.3659 0.154 Uiso 1 1 calc R . . H20C H 0.5654 0.0440 0.2831 0.154 Uiso 1 1 calc R . . C21 C 0.4519(5) -0.1544(5) 0.4315(2) 0.1162(17) Uani 1 1 d . . . H21A H 0.3644 -0.1830 0.4472 0.174 Uiso 1 1 calc R . . H21B H 0.4680 -0.1084 0.4679 0.174 Uiso 1 1 calc R . . H21C H 0.5340 -0.2334 0.4264 0.174 Uiso 1 1 calc R . . C22 C 0.2783(3) 0.3516(3) 0.29656(14) 0.0484(7) Uani 1 1 d . . . H22A H 0.3736 0.2864 0.3044 0.058 Uiso 1 1 calc R . . H22B H 0.2967 0.4325 0.2639 0.058 Uiso 1 1 calc R . . C23 C 0.0142(4) 0.5196(4) 0.3804(2) 0.0937(13) Uani 1 1 d . . . H23A H 0.0149 0.5983 0.3421 0.141 Uiso 1 1 calc R . . H23B H -0.0223 0.5491 0.4271 0.141 Uiso 1 1 calc R . . H23C H -0.0478 0.4714 0.3688 0.141 Uiso 1 1 calc R . . C24 C 0.3105(4) 0.4959(4) 0.42225(18) 0.0760(10) Uani 1 1 d . . . H24A H 0.4020 0.4328 0.4368 0.114 Uiso 1 1 calc R . . H24B H 0.2553 0.5334 0.4644 0.114 Uiso 1 1 calc R . . H24C H 0.3291 0.5689 0.3839 0.114 Uiso 1 1 calc R . . C25 C 0.1976(4) 0.2492(4) 0.45773(17) 0.0806(11) Uani 1 1 d . . . H25A H 0.1320 0.2059 0.4450 0.121 Uiso 1 1 calc R . . H25B H 0.1635 0.2758 0.5053 0.121 Uiso 1 1 calc R . . H25C H 0.2940 0.1861 0.4598 0.121 Uiso 1 1 calc R . . C26 C 0.3211(3) 0.1849(3) 0.13495(14) 0.0455(7) Uani 1 1 d . . . H26A H 0.3329 0.0868 0.1461 0.055 Uiso 1 1 calc R . . H26B H 0.2603 0.2199 0.0939 0.055 Uiso 1 1 calc R . . C27 C 0.4963(4) 0.2957(4) -0.00543(16) 0.0757(10) Uani 1 1 d . . . H27A H 0.4645 0.2480 -0.0358 0.114 Uiso 1 1 calc R . . H27B H 0.5923 0.3038 -0.0247 0.114 Uiso 1 1 calc R . . H27C H 0.4291 0.3856 -0.0058 0.114 Uiso 1 1 calc R . . C28 C 0.6298(4) 0.0225(4) 0.0857(2) 0.0926(13) Uani 1 1 d . . . H28A H 0.6368 -0.0327 0.1345 0.139 Uiso 1 1 calc R . . H28B H 0.7251 0.0307 0.0648 0.139 Uiso 1 1 calc R . . H28C H 0.5928 -0.0200 0.0546 0.139 Uiso 1 1 calc R . . C29 C 0.5918(4) 0.2837(4) 0.14218(18) 0.0902(12) Uani 1 1 d . . . H29A H 0.5383 0.3791 0.1382 0.135 Uiso 1 1 calc R . . H29B H 0.6907 0.2756 0.1206 0.135 Uiso 1 1 calc R . . H29C H 0.5924 0.2408 0.1936 0.135 Uiso 1 1 calc R . . C8A C 0.0960(5) 0.6255(3) 0.03929(19) 0.0773(11) Uani 1 1 d . . . H8A H 0.1549 0.6627 0.0010 0.093 Uiso 1 1 calc R . . C9A C -0.0526(5) 0.6786(4) 0.0444(2) 0.0841(12) Uani 1 1 d . . . H9A H -0.0968 0.7520 0.0089 0.101 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 Sc 0.0309(3) 0.0344(3) 0.0358(3) -0.0042(2) 0.00351(19) -0.0066(2) Si1 0.0551(5) 0.0524(5) 0.0436(5) -0.0154(4) 0.0061(4) -0.0188(4) Si2 0.0434(4) 0.0676(6) 0.0406(5) -0.0125(4) 0.0068(3) -0.0181(4) N1 0.0356(11) 0.0314(12) 0.0365(12) -0.0039(9) 0.0018(9) -0.0056(9) N2 0.0324(11) 0.0378(13) 0.0573(14) -0.0062(11) -0.0010(10) -0.0046(10) N3 0.0498(14) 0.0413(14) 0.0481(14) -0.0013(11) -0.0019(11) -0.0041(11) C1 0.079(2) 0.057(2) 0.0486(18) 0.0043(15) 0.0189(16) -0.0182(17) C2 0.0481(16) 0.0444(17) 0.0397(15) -0.0065(12) 0.0041(12) -0.0143(13) C3 0.0464(16) 0.056(2) 0.0486(17) -0.0102(15) 0.0175(13) -0.0135(15) C4 0.0327(14) 0.0528(19) 0.0630(19) -0.0170(15) 0.0070(13) -0.0081(13) C5 0.0446(17) 0.081(3) 0.095(3) -0.020(2) 0.0226(17) -0.0013(18) C6 0.0387(15) 0.052(2) 0.081(2) -0.0048(17) -0.0117(15) -0.0044(14) C7 0.0519(17) 0.0398(17) 0.0597(19) -0.0072(14) -0.0186(15) -0.0085(14) C8 0.071(2) 0.050(2) 0.060(2) 0.0053(16) 0.0076(17) -0.0098(17) C9 0.071(2) 0.054(2) 0.093(3) 0.0061(19) -0.039(2) -0.0080(18) C10 0.0388(14) 0.0310(14) 0.0363(14) 0.0005(11) 0.0029(11) -0.0062(11) C11 0.0483(16) 0.0395(16) 0.0404(15) -0.0059(12) 0.0001(12) -0.0077(13) C12 0.071(2) 0.0467(19) 0.0555(19) -0.0187(15) 0.0015(16) -0.0116(16) C13 0.064(2) 0.046(2) 0.076(2) -0.0157(17) 0.0061(18) 0.0071(17) C14 0.0471(17) 0.052(2) 0.073(2) -0.0070(17) -0.0093(16) 0.0048(15) C15 0.0450(15) 0.0419(17) 0.0459(16) 0.0005(13) -0.0049(13) -0.0068(13) C16 0.0599(19) 0.064(2) 0.066(2) -0.0214(17) -0.0178(17) -0.0097(17) C17 0.070(2) 0.188(5) 0.079(3) 0.003(3) -0.008(2) -0.058(3) C18 0.104(3) 0.099(3) 0.070(2) 0.012(2) -0.032(2) -0.054(2) C19 0.0524(18) 0.060(2) 0.070(2) -0.0068(17) -0.0211(16) -0.0086(16) C20 0.075(3) 0.105(3) 0.140(4) -0.029(3) -0.021(3) -0.033(2) C21 0.151(4) 0.141(4) 0.070(3) 0.009(3) -0.047(3) -0.062(3) C22 0.0526(16) 0.0490(18) 0.0447(16) -0.0108(13) 0.0037(13) -0.0183(14) C23 0.078(2) 0.096(3) 0.104(3) -0.054(3) -0.005(2) 0.003(2) C24 0.088(2) 0.087(3) 0.068(2) -0.036(2) 0.0122(19) -0.041(2) C25 0.120(3) 0.085(3) 0.0474(19) -0.0135(18) 0.0071(19) -0.051(2) C26 0.0470(15) 0.0437(17) 0.0433(15) -0.0106(13) 0.0093(12) -0.0136(13) C27 0.072(2) 0.099(3) 0.053(2) -0.0042(18) 0.0118(17) -0.034(2) C28 0.060(2) 0.101(3) 0.097(3) -0.026(2) -0.006(2) 0.011(2) C29 0.089(3) 0.147(4) 0.063(2) -0.032(2) 0.0133(19) -0.075(3) C8A 0.113(3) 0.053(2) 0.057(2) 0.0064(17) -0.004(2) -0.024(2) C9A 0.112(3) 0.062(2) 0.076(3) 0.015(2) -0.048(3) -0.021(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc C22 2.197(3) . ? Sc N1 2.198(2) . ? Sc N2 2.198(2) . ? Sc C26 2.254(2) . ? Sc N3 2.308(2) . ? Si1 C22 1.834(3) . ? Si1 C25 1.854(3) . ? Si1 C23 1.860(3) . ? Si1 C24 1.870(3) . ? Si2 C26 1.833(3) . ? Si2 C29 1.867(3) . ? Si2 C27 1.869(3) . ? Si2 C28 1.874(3) . ? N1 C2 1.326(3) . ? N1 C10 1.448(3) . ? N2 C4 1.326(3) . ? N2 C6 1.461(3) . ? N3 C7 1.333(3) . ? N3 C8 1.344(4) . ? C1 C2 1.504(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.396(4) . ? C3 C4 1.381(4) . ? C3 H3 0.9300 . ? C4 C5 1.519(4) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.478(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C9 1.373(4) . ? C8 C8A 1.364(4) . ? C8 H8 0.9300 . ? C9 C9A 1.362(5) . ? C9 H9 0.9300 . ? C10 C11 1.387(4) . ? C10 C15 1.396(3) . ? C11 C12 1.394(4) . ? C11 C16 1.525(4) . ? C12 C13 1.369(4) . ? C12 H12 0.9300 . ? C13 C14 1.361(4) . ? C13 H13 0.9300 . ? C14 C15 1.385(4) . ? C14 H14 0.9300 . ? C15 C19 1.505(4) . ? C16 C18 1.514(4) . ? C16 C17 1.518(5) . ? C16 H16 0.9800 . ? 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 C20 1.515(5) . ? C19 C21 1.526(5) . ? C19 H19 0.9800 . ? 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 0.9700 . ? C22 H22B 0.9700 . ? 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 0.9700 . ? C26 H26B 0.9700 . ? 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 . ? C8A C9A 1.364(5) . ? C8A H8A 0.9300 . ? C9A H9A 0.9300 . ? 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 C22 Sc N1 109.82(9) . . ? C22 Sc N2 110.23(9) . . ? N1 Sc N2 83.41(8) . . ? C22 Sc C26 111.56(10) . . ? N1 Sc C26 96.97(9) . . ? N2 Sc C26 135.21(9) . . ? C22 Sc N3 98.12(10) . . ? N1 Sc N3 148.16(8) . . ? N2 Sc N3 72.55(8) . . ? C26 Sc N3 86.29(9) . . ? C22 Si1 C25 109.40(15) . . ? C22 Si1 C23 110.14(15) . . ? C25 Si1 C23 108.41(19) . . ? C22 Si1 C24 115.14(14) . . ? C25 Si1 C24 106.77(16) . . ? C23 Si1 C24 106.75(17) . . ? C26 Si2 C29 114.20(14) . . ? C26 Si2 C27 112.41(14) . . ? C29 Si2 C27 105.85(17) . . ? C26 Si2 C28 110.52(16) . . ? C29 Si2 C28 107.45(18) . . ? C27 Si2 C28 105.92(16) . . ? C2 N1 C10 116.4(2) . . ? C2 N1 Sc 124.60(17) . . ? C10 N1 Sc 119.04(15) . . ? C4 N2 C6 116.2(2) . . ? C4 N2 Sc 123.68(18) . . ? C6 N2 Sc 118.91(17) . . ? C7 N3 C8 117.4(3) . . ? C7 N3 Sc 117.86(19) . . ? C8 N3 Sc 124.54(19) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.6(3) . . ? N1 C2 C1 121.1(2) . . ? C3 C2 C1 115.2(2) . . ? C4 C3 C2 129.1(3) . . ? C4 C3 H3 115.5 . . ? C2 C3 H3 115.5 . . ? N2 C4 C3 124.3(2) . . ? N2 C4 C5 120.5(3) . . ? C3 C4 C5 115.1(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 113.1(2) . . ? N2 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? N2 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N3 C7 C9 122.3(3) . . ? N3 C7 C6 117.0(2) . . ? C9 C7 C6 120.7(3) . . ? N3 C8 C8A 123.2(3) . . ? N3 C8 H8 118.4 . . ? C8A C8 H8 118.4 . . ? C9A C9 C7 119.2(3) . . ? C9A C9 H9 120.4 . . ? C7 C9 H9 120.4 . . ? C11 C10 C15 121.3(2) . . ? C11 C10 N1 118.0(2) . . ? C15 C10 N1 120.6(2) . . ? C10 C11 C12 118.5(3) . . ? C10 C11 C16 122.5(2) . . ? C12 C11 C16 119.0(3) . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 120.0(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 122.0(3) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C14 C15 C10 117.6(3) . . ? C14 C15 C19 119.8(3) . . ? C10 C15 C19 122.5(2) . . ? C18 C16 C17 110.0(3) . . ? C18 C16 C11 112.2(3) . . ? C17 C16 C11 111.6(3) . . ? C18 C16 H16 107.6 . . ? C17 C16 H16 107.6 . . ? C11 C16 H16 107.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 C20 112.8(3) . . ? C15 C19 C21 111.6(3) . . ? C20 C19 C21 109.6(3) . . ? C15 C19 H19 107.5 . . ? C20 C19 H19 107.5 . . ? C21 C19 H19 107.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 Sc 125.28(14) . . ? Si1 C22 H22A 106.0 . . ? Sc C22 H22A 106.0 . . ? Si1 C22 H22B 106.0 . . ? Sc C22 H22B 106.0 . . ? H22A C22 H22B 106.3 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 Sc 134.85(15) . . ? Si2 C26 H26A 103.5 . . ? Sc C26 H26A 103.5 . . ? Si2 C26 H26B 103.5 . . ? Sc C26 H26B 103.5 . . ? H26A C26 H26B 105.3 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C9A C8A C8 118.4(4) . . ? C9A C8A H8A 120.8 . . ? C8 C8A H8A 120.8 . . ? C9 C9A C8A 119.6(3) . . ? C9 C9A H9A 120.2 . . ? C8A C9A H9A 120.2 . . ? 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 C22 Sc N1 C2 79.4(2) . . . . ? N2 Sc N1 C2 -29.7(2) . . . . ? C26 Sc N1 C2 -164.6(2) . . . . ? N3 Sc N1 C2 -70.4(3) . . . . ? C22 Sc N1 C10 -102.01(18) . . . . ? N2 Sc N1 C10 148.82(18) . . . . ? C26 Sc N1 C10 13.94(19) . . . . ? N3 Sc N1 C10 108.1(2) . . . . ? C22 Sc N2 C4 -76.9(2) . . . . ? N1 Sc N2 C4 31.9(2) . . . . ? C26 Sc N2 C4 125.1(2) . . . . ? N3 Sc N2 C4 -169.3(2) . . . . ? C22 Sc N2 C6 89.8(2) . . . . ? N1 Sc N2 C6 -161.4(2) . . . . ? C26 Sc N2 C6 -68.2(2) . . . . ? N3 Sc N2 C6 -2.57(19) . . . . ? C22 Sc N3 C7 -111.4(2) . . . . ? N1 Sc N3 C7 40.1(3) . . . . ? N2 Sc N3 C7 -2.61(19) . . . . ? C26 Sc N3 C7 137.4(2) . . . . ? C22 Sc N3 C8 73.6(3) . . . . ? N1 Sc N3 C8 -134.9(2) . . . . ? N2 Sc N3 C8 -177.7(3) . . . . ? C26 Sc N3 C8 -37.7(3) . . . . ? C10 N1 C2 C3 -163.6(3) . . . . ? Sc N1 C2 C3 15.0(4) . . . . ? C10 N1 C2 C1 14.2(4) . . . . ? Sc N1 C2 C1 -167.2(2) . . . . ? N1 C2 C3 C4 13.9(5) . . . . ? C1 C2 C3 C4 -164.0(3) . . . . ? C6 N2 C4 C3 173.2(3) . . . . ? Sc N2 C4 C3 -19.8(4) . . . . ? C6 N2 C4 C5 -5.3(4) . . . . ? Sc N2 C4 C5 161.7(2) . . . . ? C2 C3 C4 N2 -11.1(5) . . . . ? C2 C3 C4 C5 167.5(3) . . . . ? C4 N2 C6 C7 174.6(3) . . . . ? Sc N2 C6 C7 6.9(3) . . . . ? C8 N3 C7 C9 0.3(4) . . . . ? Sc N3 C7 C9 -175.2(2) . . . . ? C8 N3 C7 C6 -177.4(3) . . . . ? Sc N3 C7 C6 7.2(3) . . . . ? N2 C6 C7 N3 -9.1(4) . . . . ? N2 C6 C7 C9 173.3(3) . . . . ? C7 N3 C8 C8A -1.0(5) . . . . ? Sc N3 C8 C8A 174.1(2) . . . . ? N3 C7 C9 C9A 1.1(5) . . . . ? C6 C7 C9 C9A 178.6(3) . . . . ? C2 N1 C10 C11 86.6(3) . . . . ? Sc N1 C10 C11 -92.0(2) . . . . ? C2 N1 C10 C15 -95.9(3) . . . . ? Sc N1 C10 C15 85.5(3) . . . . ? C15 C10 C11 C12 1.9(4) . . . . ? N1 C10 C11 C12 179.3(2) . . . . ? C15 C10 C11 C16 -178.7(3) . . . . ? N1 C10 C11 C16 -1.2(4) . . . . ? C10 C11 C12 C13 -1.7(4) . . . . ? C16 C11 C12 C13 178.8(3) . . . . ? C11 C12 C13 C14 0.6(5) . . . . ? C12 C13 C14 C15 0.4(5) . . . . ? C13 C14 C15 C10 -0.2(5) . . . . ? C13 C14 C15 C19 178.1(3) . . . . ? C11 C10 C15 C14 -0.9(4) . . . . ? N1 C10 C15 C14 -178.3(2) . . . . ? C11 C10 C15 C19 -179.1(3) . . . . ? N1 C10 C15 C19 3.4(4) . . . . ? C10 C11 C16 C18 125.9(3) . . . . ? C12 C11 C16 C18 -54.6(4) . . . . ? C10 C11 C16 C17 -110.1(3) . . . . ? C12 C11 C16 C17 69.4(4) . . . . ? C14 C15 C19 C20 59.2(4) . . . . ? C10 C15 C19 C20 -122.7(3) . . . . ? C14 C15 C19 C21 -64.7(4) . . . . ? C10 C15 C19 C21 113.4(3) . . . . ? C25 Si1 C22 Sc 66.9(2) . . . . ? C23 Si1 C22 Sc -52.1(2) . . . . ? C24 Si1 C22 Sc -172.87(17) . . . . ? N1 Sc C22 Si1 -64.54(19) . . . . ? N2 Sc C22 Si1 25.6(2) . . . . ? C26 Sc C22 Si1 -170.86(16) . . . . ? N3 Sc C22 Si1 99.94(18) . . . . ? C29 Si2 C26 Sc 5.0(3) . . . . ? C27 Si2 C26 Sc -115.6(2) . . . . ? C28 Si2 C26 Sc 126.3(2) . . . . ? C22 Sc C26 Si2 -8.8(2) . . . . ? N1 Sc C26 Si2 -123.3(2) . . . . ? N2 Sc C26 Si2 149.04(16) . . . . ? N3 Sc C26 Si2 88.5(2) . . . . ? N3 C8 C8A C9A 0.3(5) . . . . ? C7 C9 C9A C8A -1.7(6) . . . . ? C8 C8A C9A C9 1.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.382 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.051 #===END data_cd29117 _database_code_depnum_ccdc_archive 'CCDC 744084' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H72 N6 O2 Y2' _chemical_formula_weight 1015.00 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2136(13) _cell_length_b 11.1187(14) _cell_length_c 13.3747(17) _cell_angle_alpha 68.788(2) _cell_angle_beta 84.920(2) _cell_angle_gamma 65.451(2) _cell_volume 1284.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1996 _cell_measurement_theta_min 4.720 _cell_measurement_theta_max 46.866 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.368 _exptl_crystal_size_mid 0.238 _exptl_crystal_size_min 0.189 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 2.293 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.60424 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7104 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0876 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4972 _reflns_number_gt 3457 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4972 _refine_ls_number_parameters 294 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1244 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.008 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 0.65868(5) 0.85419(4) 0.58786(4) 0.03790(16) Uani 1 1 d . . . N1 N 0.5633(4) 0.7098(4) 0.7086(3) 0.0438(9) Uani 1 1 d . . . N2 N 0.4737(4) 0.8833(3) 0.4783(3) 0.0386(8) Uani 1 1 d . . . N3 N 0.7418(4) 0.8519(4) 0.4152(3) 0.0475(10) Uani 1 1 d . . . O1 O 0.9053(3) 0.6826(3) 0.6474(3) 0.0549(9) Uani 1 1 d . . . C1 C 0.3522(5) 0.7015(5) 0.8145(4) 0.0614(14) Uani 1 1 d . . . H1A H 0.2515 0.7260 0.8025 0.092 Uiso 1 1 calc R . . H1B H 0.3637 0.7457 0.8609 0.092 Uiso 1 1 calc R . . H1C H 0.4026 0.6006 0.8475 0.092 Uiso 1 1 calc R . . C2 C 0.4138(5) 0.7528(5) 0.7072(4) 0.0477(12) Uani 1 1 d . . . C3 C 0.3201(5) 0.8340(4) 0.6216(4) 0.0446(11) Uani 1 1 d . . . H3 H 0.2237 0.8604 0.6370 0.054 Uiso 1 1 calc R . . C4 C 0.3421(5) 0.8874(4) 0.5100(4) 0.0435(11) Uani 1 1 d D . . C5 C 0.2237(5) 0.9616(5) 0.4336(4) 0.0559(13) Uani 1 1 d D . . H5A H 0.1293 0.9835 0.4620 0.067 Uiso 1 1 calc R . . H5B H 0.2321 0.9294 0.3740 0.067 Uiso 1 1 calc R . . C6 C 0.4925(5) 0.9283(4) 0.3651(4) 0.0446(11) Uani 1 1 d . . . H6 H 0.4383 0.9047 0.3238 0.054 Uiso 1 1 calc R . . C7 C 0.6339(5) 0.9022(5) 0.3362(4) 0.0492(12) Uani 1 1 d . . . C8 C 0.8748(5) 0.8394(5) 0.3835(4) 0.0619(14) Uani 1 1 d . . . H8 H 0.9463 0.8108 0.4361 0.074 Uiso 1 1 calc R . . C9 C 0.6669(6) 0.9282(5) 0.2271(4) 0.0677(16) Uani 1 1 d . . . H9 H 0.5957 0.9586 0.1738 0.081 Uiso 1 1 calc R . . C10 C 0.6509(5) 0.5865(5) 0.7929(4) 0.0455(11) Uani 1 1 d . . . C11 C 0.7155(6) 0.5943(5) 0.8763(4) 0.0553(13) Uani 1 1 d . . . C12 C 0.8195(6) 0.4673(6) 0.9497(4) 0.0730(16) Uani 1 1 d . . . H12 H 0.8687 0.4714 1.0028 0.088 Uiso 1 1 calc R . . C13 C 0.8473(6) 0.3408(6) 0.9429(5) 0.0743(17) Uani 1 1 d . . . H13 H 0.9147 0.2588 0.9923 0.089 Uiso 1 1 calc R . . C14 C 0.7795(6) 0.3306(5) 0.8661(5) 0.0658(15) Uani 1 1 d . . . H14 H 0.8001 0.2416 0.8646 0.079 Uiso 1 1 calc R . . C15 C 0.6791(5) 0.4508(5) 0.7889(4) 0.0538(13) Uani 1 1 d . . . C16 C 0.6715(6) 0.7334(5) 0.8932(4) 0.0652(15) Uani 1 1 d . . . H16 H 0.5963 0.8059 0.8366 0.078 Uiso 1 1 calc R . . C17 C 0.6039(8) 0.7269(7) 1.0003(5) 0.102(2) Uani 1 1 d . . . H17A H 0.6787 0.6830 1.0569 0.153 Uiso 1 1 calc R . . H17B H 0.5476 0.6724 1.0138 0.153 Uiso 1 1 calc R . . H17C H 0.5428 0.8211 0.9975 0.153 Uiso 1 1 calc R . . C18 C 0.7906(7) 0.7821(7) 0.8845(5) 0.096(2) Uani 1 1 d . . . H18A H 0.8699 0.7101 0.9351 0.144 Uiso 1 1 calc R . . H18B H 0.7554 0.8678 0.8997 0.144 Uiso 1 1 calc R . . H18C H 0.8224 0.7995 0.8130 0.144 Uiso 1 1 calc R . . C19 C 0.6008(6) 0.4402(5) 0.7043(5) 0.0637(15) Uani 1 1 d . . . H19 H 0.5048 0.5188 0.6878 0.076 Uiso 1 1 calc R . . C20 C 0.6771(7) 0.4519(8) 0.6007(5) 0.093(2) Uani 1 1 d . . . H20A H 0.6789 0.5438 0.5700 0.140 Uiso 1 1 calc R . . H20B H 0.6266 0.4392 0.5508 0.140 Uiso 1 1 calc R . . H20C H 0.7742 0.3803 0.6158 0.140 Uiso 1 1 calc R . . C21 C 0.5810(8) 0.3015(7) 0.7417(6) 0.116(3) Uani 1 1 d . . . H21A H 0.6680 0.2274 0.7334 0.173 Uiso 1 1 calc R . . H21B H 0.5025 0.3135 0.6991 0.173 Uiso 1 1 calc R . . H21C H 0.5602 0.2769 0.8160 0.173 Uiso 1 1 calc R . . C22 C 0.9586(5) 0.5384(5) 0.6480(5) 0.0650(15) Uani 1 1 d D . . H22A H 0.9228 0.4816 0.7074 0.078 Uiso 1 1 calc R . . H22B H 0.9270 0.5391 0.5813 0.078 Uiso 1 1 calc R . . C23 C 1.1103(6) 0.4828(6) 0.6592(7) 0.109(3) Uani 1 1 d D . . H23A H 1.1502 0.4724 0.5927 0.131 Uiso 1 1 calc R . . H23B H 1.1478 0.3901 0.7159 0.131 Uiso 1 1 calc R . . C24 C 1.1514(6) 0.5777(7) 0.6852(8) 0.126(3) Uani 1 1 d D . . H24A H 1.1942 0.5340 0.7584 0.151 Uiso 1 1 calc R . . H24B H 1.2218 0.5998 0.6371 0.151 Uiso 1 1 calc R . . C25 C 1.0305(6) 0.6979(6) 0.6741(6) 0.090(2) Uani 1 1 d D . . H25A H 1.0402 0.7777 0.6178 0.108 Uiso 1 1 calc R . . H25B H 1.0185 0.7162 0.7407 0.108 Uiso 1 1 calc R . . C8A C 0.9107(7) 0.8656(6) 0.2809(5) 0.0810(19) Uani 1 1 d . . . H8A H 1.0041 0.8555 0.2640 0.097 Uiso 1 1 calc R . . C9A C 0.8071(8) 0.9076(6) 0.2014(5) 0.084(2) Uani 1 1 d . . . H9A H 0.8312 0.9221 0.1306 0.101 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 0.0319(2) 0.0359(3) 0.0499(3) -0.01773(19) 0.00443(18) -0.01593(18) N1 0.046(2) 0.041(2) 0.047(2) -0.0152(19) 0.0047(18) -0.0206(19) N2 0.034(2) 0.034(2) 0.051(2) -0.0176(17) 0.0012(17) -0.0149(16) N3 0.040(2) 0.040(2) 0.060(3) -0.0204(19) 0.011(2) -0.0136(18) O1 0.0358(18) 0.053(2) 0.080(2) -0.0265(18) 0.0010(16) -0.0191(16) C1 0.052(3) 0.063(3) 0.069(3) -0.021(3) 0.018(3) -0.027(3) C2 0.047(3) 0.046(3) 0.063(3) -0.027(3) 0.017(3) -0.027(2) C3 0.028(2) 0.035(3) 0.066(3) -0.013(2) 0.004(2) -0.014(2) C4 0.035(3) 0.032(2) 0.065(3) -0.017(2) -0.002(2) -0.014(2) C5 0.045(3) 0.056(3) 0.078(4) -0.029(3) 0.005(3) -0.029(3) C6 0.047(3) 0.038(3) 0.055(3) -0.023(2) 0.001(2) -0.017(2) C7 0.057(3) 0.038(3) 0.056(3) -0.027(2) 0.011(3) -0.016(2) C8 0.041(3) 0.063(4) 0.073(4) -0.023(3) 0.018(3) -0.017(3) C9 0.078(4) 0.061(4) 0.059(4) -0.031(3) 0.017(3) -0.018(3) C10 0.040(3) 0.047(3) 0.048(3) -0.015(2) 0.012(2) -0.020(2) C11 0.059(3) 0.054(3) 0.048(3) -0.016(3) 0.006(3) -0.021(3) C12 0.073(4) 0.080(5) 0.053(3) -0.018(3) -0.002(3) -0.023(3) C13 0.066(4) 0.052(4) 0.066(4) -0.005(3) 0.000(3) -0.001(3) C14 0.061(4) 0.040(3) 0.078(4) -0.016(3) 0.010(3) -0.010(3) C15 0.050(3) 0.048(3) 0.063(3) -0.021(3) 0.020(3) -0.024(3) C16 0.084(4) 0.057(3) 0.051(3) -0.019(3) -0.006(3) -0.024(3) C17 0.140(7) 0.101(5) 0.078(5) -0.052(4) 0.023(4) -0.048(5) C18 0.102(6) 0.099(5) 0.107(5) -0.045(4) 0.002(4) -0.053(5) C19 0.050(3) 0.057(3) 0.097(4) -0.038(3) 0.011(3) -0.026(3) C20 0.097(5) 0.151(6) 0.073(4) -0.047(4) 0.009(4) -0.084(5) C21 0.167(8) 0.126(6) 0.131(6) -0.079(5) 0.070(6) -0.115(6) C22 0.044(3) 0.049(3) 0.104(4) -0.033(3) 0.007(3) -0.017(3) C23 0.049(4) 0.067(4) 0.218(9) -0.074(5) 0.001(5) -0.010(3) C24 0.041(4) 0.088(5) 0.252(10) -0.086(6) -0.041(5) 0.003(3) C25 0.047(4) 0.091(5) 0.147(6) -0.062(4) -0.019(4) -0.021(3) C8A 0.057(4) 0.077(4) 0.087(5) -0.023(4) 0.033(4) -0.017(3) C9A 0.099(6) 0.079(4) 0.058(4) -0.028(3) 0.036(4) -0.024(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 Y1 N1 2.298(3) . ? Y1 N2 2.336(3) . ? Y1 N3 2.394(4) . ? Y1 O1 2.425(3) . ? Y1 N2 2.488(3) 2_676 ? Y1 C6 2.540(4) 2_676 ? Y1 C4 2.688(4) 2_676 ? Y1 C5 2.698(4) 2_676 ? Y1 Y1 3.6939(9) 2_676 ? N1 C2 1.397(6) . ? N1 C10 1.410(6) . ? N2 C4 1.360(5) . ? N2 C6 1.435(5) . ? N2 Y1 2.488(3) 2_676 ? N3 C8 1.352(6) . ? N3 C7 1.383(6) . ? O1 C25 1.449(6) . ? O1 C22 1.461(5) . ? C1 C2 1.525(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.331(6) . ? C3 C4 1.428(6) . ? C3 H3 0.9300 . ? C4 C5 1.402(6) . ? C4 Y1 2.688(4) 2_676 ? C5 Y1 2.698(4) 2_676 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.397(6) . ? C6 Y1 2.540(4) 2_676 ? C6 H6 0.9800 . ? C7 C9 1.420(7) . ? C8 C8A 1.346(7) . ? C8 H8 0.9300 . ? C9 C9A 1.384(8) . ? C9 H9 0.9300 . ? C10 C11 1.391(6) . ? C10 C15 1.434(6) . ? C11 C12 1.422(7) . ? C11 C16 1.517(7) . ? C12 C13 1.350(8) . ? C12 H12 0.9300 . ? C13 C14 1.349(8) . ? C13 H13 0.9300 . ? C14 C15 1.398(7) . ? C14 H14 0.9300 . ? C15 C19 1.507(7) . ? C16 C18 1.505(8) . ? C16 C17 1.524(7) . ? C16 H16 0.9800 . ? 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 C20 1.519(7) . ? C19 C21 1.533(7) . ? C19 H19 0.9800 . ? 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 C23 1.409(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.438(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.361(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C8A C9A 1.378(8) . ? C8A H8A 0.9300 . ? C9A H9A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y1 N2 79.50(12) . . ? N1 Y1 N3 128.52(12) . . ? N2 Y1 N3 69.88(13) . . ? N1 Y1 O1 93.06(12) . . ? N2 Y1 O1 135.80(11) . . ? N3 Y1 O1 82.28(12) . . ? N1 Y1 N2 121.35(12) . 2_676 ? N2 Y1 N2 80.11(11) . 2_676 ? N3 Y1 N2 93.40(12) . 2_676 ? O1 Y1 N2 136.73(10) . 2_676 ? N1 Y1 C6 95.30(13) . 2_676 ? N2 Y1 C6 94.24(13) . 2_676 ? N3 Y1 C6 126.50(13) . 2_676 ? O1 Y1 C6 129.93(13) . 2_676 ? N2 Y1 C6 33.14(12) 2_676 2_676 ? N1 Y1 C4 149.54(13) . 2_676 ? N2 Y1 C4 97.76(13) . 2_676 ? N3 Y1 C4 76.78(13) . 2_676 ? O1 Y1 C4 108.72(12) . 2_676 ? N2 Y1 C4 30.16(11) 2_676 2_676 ? C6 Y1 C4 54.43(14) 2_676 2_676 ? N1 Y1 C5 143.64(14) . 2_676 ? N2 Y1 C5 127.73(13) . 2_676 ? N3 Y1 C5 86.75(14) . 2_676 ? O1 Y1 C5 82.19(12) . 2_676 ? N2 Y1 C5 54.55(12) 2_676 2_676 ? C6 Y1 C5 62.81(15) 2_676 2_676 ? C4 Y1 C5 30.18(13) 2_676 2_676 ? N1 Y1 Y1 103.61(10) . 2_676 ? N2 Y1 Y1 41.58(8) . 2_676 ? N3 Y1 Y1 79.77(9) . 2_676 ? O1 Y1 Y1 160.71(8) . 2_676 ? N2 Y1 Y1 38.53(8) 2_676 2_676 ? C6 Y1 Y1 58.85(10) 2_676 2_676 ? C4 Y1 Y1 60.19(9) 2_676 2_676 ? C5 Y1 Y1 89.79(10) 2_676 2_676 ? C2 N1 C10 118.6(4) . . ? C2 N1 Y1 119.6(3) . . ? C10 N1 Y1 121.3(3) . . ? C4 N2 C6 117.9(4) . . ? C4 N2 Y1 125.5(3) . . ? C6 N2 Y1 115.4(3) . . ? C4 N2 Y1 83.1(2) . 2_676 ? C6 N2 Y1 75.4(2) . 2_676 ? Y1 N2 Y1 99.89(11) . 2_676 ? C8 N3 C7 117.6(4) . . ? C8 N3 Y1 125.6(3) . . ? C7 N3 Y1 114.8(3) . . ? C25 O1 C22 105.8(4) . . ? C25 O1 Y1 131.3(3) . . ? C22 O1 Y1 122.4(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 N1 126.5(4) . . ? C3 C2 C1 116.9(4) . . ? N1 C2 C1 116.7(4) . . ? C2 C3 C4 131.0(4) . . ? C2 C3 H3 114.5 . . ? C4 C3 H3 114.5 . . ? N2 C4 C5 119.3(4) . . ? N2 C4 C3 120.4(4) . . ? C5 C4 C3 119.8(4) . . ? N2 C4 Y1 66.8(2) . 2_676 ? C5 C4 Y1 75.3(2) . 2_676 ? C3 C4 Y1 122.6(3) . 2_676 ? C4 C5 Y1 74.5(2) . 2_676 ? C4 C5 H5A 116.0 . . ? Y1 C5 H5A 116.0 2_676 . ? C4 C5 H5B 116.1 . . ? Y1 C5 H5B 116.0 2_676 . ? H5A C5 H5B 113.0 . . ? C7 C6 N2 116.1(4) . . ? C7 C6 Y1 120.6(3) . 2_676 ? N2 C6 Y1 71.4(2) . 2_676 ? C7 C6 H6 114.0 . . ? N2 C6 H6 114.0 . . ? Y1 C6 H6 114.0 2_676 . ? N3 C7 C6 119.2(4) . . ? N3 C7 C9 120.0(5) . . ? C6 C7 C9 120.8(5) . . ? C8A C8 N3 124.4(6) . . ? C8A C8 H8 117.8 . . ? N3 C8 H8 117.8 . . ? C9A C9 C7 118.9(6) . . ? C9A C9 H9 120.6 . . ? C7 C9 H9 120.6 . . ? C11 C10 N1 121.4(4) . . ? C11 C10 C15 119.7(4) . . ? N1 C10 C15 118.9(4) . . ? C10 C11 C12 118.6(5) . . ? C10 C11 C16 121.3(4) . . ? C12 C11 C16 120.0(5) . . ? C13 C12 C11 120.5(6) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 121.5(5) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C13 C14 C15 121.5(5) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C14 C15 C10 117.9(5) . . ? C14 C15 C19 121.8(5) . . ? C10 C15 C19 120.3(5) . . ? C18 C16 C11 114.7(5) . . ? C18 C16 C17 110.2(5) . . ? C11 C16 C17 110.7(4) . . ? C18 C16 H16 106.9 . . ? C11 C16 H16 107.0 . . ? C17 C16 H16 106.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 C20 112.4(4) . . ? C15 C19 C21 112.8(5) . . ? C20 C19 C21 107.7(5) . . ? C15 C19 H19 108.0 . . ? C20 C19 H19 107.9 . . ? C21 C19 H19 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.4 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.4 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 O1 106.4(4) . . ? C23 C22 H22A 110.4 . . ? O1 C22 H22A 110.5 . . ? C23 C22 H22B 110.4 . . ? O1 C22 H22B 110.4 . . ? H22A C22 H22B 108.6 . . ? C22 C23 C24 108.9(5) . . ? C22 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? C22 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? C25 C24 C23 107.9(5) . . ? C25 C24 H24A 110.1 . . ? C23 C24 H24A 110.1 . . ? C25 C24 H24B 110.1 . . ? C23 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? C24 C25 O1 110.0(5) . . ? C24 C25 H25A 109.7 . . ? O1 C25 H25A 109.7 . . ? C24 C25 H25B 109.6 . . ? O1 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C8 C8A C9A 119.1(6) . . ? C8 C8A H8A 120.5 . . ? C9A C8A H8A 120.5 . . ? C8A C9A C9 119.8(5) . . ? C8A C9A H9A 120.1 . . ? C9 C9A H9A 120.1 . . ? 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 N2 Y1 N1 C2 -40.0(3) . . . . ? N3 Y1 N1 C2 -93.5(3) . . . . ? O1 Y1 N1 C2 -176.1(3) . . . . ? N2 Y1 N1 C2 31.5(3) 2_676 . . . ? C6 Y1 N1 C2 53.4(3) 2_676 . . . ? C4 Y1 N1 C2 47.5(4) 2_676 . . . ? C5 Y1 N1 C2 103.0(4) 2_676 . . . ? Y1 Y1 N1 C2 -5.8(3) 2_676 . . . ? N2 Y1 N1 C10 147.9(3) . . . . ? N3 Y1 N1 C10 94.4(3) . . . . ? O1 Y1 N1 C10 11.8(3) . . . . ? N2 Y1 N1 C10 -140.6(3) 2_676 . . . ? C6 Y1 N1 C10 -118.8(3) 2_676 . . . ? C4 Y1 N1 C10 -124.7(4) 2_676 . . . ? C5 Y1 N1 C10 -69.2(4) 2_676 . . . ? Y1 Y1 N1 C10 -178.0(3) 2_676 . . . ? N1 Y1 N2 C4 36.2(3) . . . . ? N3 Y1 N2 C4 174.1(3) . . . . ? O1 Y1 N2 C4 119.7(3) . . . . ? N2 Y1 N2 C4 -88.5(3) 2_676 . . . ? C6 Y1 N2 C4 -58.4(3) 2_676 . . . ? C4 Y1 N2 C4 -113.1(3) 2_676 . . . ? C5 Y1 N2 C4 -117.0(3) 2_676 . . . ? Y1 Y1 N2 C4 -88.5(3) 2_676 . . . ? N1 Y1 N2 C6 -156.8(3) . . . . ? N3 Y1 N2 C6 -18.9(3) . . . . ? O1 Y1 N2 C6 -73.3(3) . . . . ? N2 Y1 N2 C6 78.4(3) 2_676 . . . ? C6 Y1 N2 C6 108.5(3) 2_676 . . . ? C4 Y1 N2 C6 53.9(3) 2_676 . . . ? C5 Y1 N2 C6 50.0(3) 2_676 . . . ? Y1 Y1 N2 C6 78.4(3) 2_676 . . . ? N1 Y1 N2 Y1 124.71(14) . . . 2_676 ? N3 Y1 N2 Y1 -97.36(14) . . . 2_676 ? O1 Y1 N2 Y1 -151.76(12) . . . 2_676 ? N2 Y1 N2 Y1 0.0 2_676 . . 2_676 ? C6 Y1 N2 Y1 30.09(14) 2_676 . . 2_676 ? C4 Y1 N2 Y1 -24.56(14) 2_676 . . 2_676 ? C5 Y1 N2 Y1 -28.4(2) 2_676 . . 2_676 ? N1 Y1 N3 C8 -124.2(4) . . . . ? N2 Y1 N3 C8 178.4(4) . . . . ? O1 Y1 N3 C8 -36.5(4) . . . . ? N2 Y1 N3 C8 100.2(4) 2_676 . . . ? C6 Y1 N3 C8 98.4(4) 2_676 . . . ? C4 Y1 N3 C8 74.9(4) 2_676 . . . ? C5 Y1 N3 C8 46.1(4) 2_676 . . . ? Y1 Y1 N3 C8 136.4(4) 2_676 . . . ? N1 Y1 N3 C7 72.4(3) . . . . ? N2 Y1 N3 C7 15.1(3) . . . . ? O1 Y1 N3 C7 160.2(3) . . . . ? N2 Y1 N3 C7 -63.1(3) 2_676 . . . ? C6 Y1 N3 C7 -65.0(3) 2_676 . . . ? C4 Y1 N3 C7 -88.4(3) 2_676 . . . ? C5 Y1 N3 C7 -117.3(3) 2_676 . . . ? Y1 Y1 N3 C7 -26.9(3) 2_676 . . . ? N1 Y1 O1 C25 -132.9(5) . . . . ? N2 Y1 O1 C25 149.0(5) . . . . ? N3 Y1 O1 C25 98.6(5) . . . . ? N2 Y1 O1 C25 11.8(5) 2_676 . . . ? C6 Y1 O1 C25 -33.4(5) 2_676 . . . ? C4 Y1 O1 C25 25.4(5) 2_676 . . . ? C5 Y1 O1 C25 10.8(5) 2_676 . . . ? Y1 Y1 O1 C25 77.0(5) 2_676 . . . ? N1 Y1 O1 C22 56.2(4) . . . . ? N2 Y1 O1 C22 -21.9(4) . . . . ? N3 Y1 O1 C22 -72.3(4) . . . . ? N2 Y1 O1 C22 -159.0(3) 2_676 . . . ? C6 Y1 O1 C22 155.7(3) 2_676 . . . ? C4 Y1 O1 C22 -145.4(3) 2_676 . . . ? C5 Y1 O1 C22 -160.0(4) 2_676 . . . ? Y1 Y1 O1 C22 -93.8(4) 2_676 . . . ? C10 N1 C2 C3 -156.8(5) . . . . ? Y1 N1 C2 C3 30.8(6) . . . . ? C10 N1 C2 C1 23.1(6) . . . . ? Y1 N1 C2 C1 -149.2(3) . . . . ? N1 C2 C3 C4 6.7(8) . . . . ? C1 C2 C3 C4 -173.2(4) . . . . ? C6 N2 C4 C5 -13.4(5) . . . . ? Y1 N2 C4 C5 153.3(3) . . . . ? Y1 N2 C4 C5 56.1(4) 2_676 . . . ? C6 N2 C4 C3 175.2(4) . . . . ? Y1 N2 C4 C3 -18.1(5) . . . . ? Y1 N2 C4 C3 -115.3(4) 2_676 . . . ? C6 N2 C4 Y1 -69.4(3) . . . 2_676 ? Y1 N2 C4 Y1 97.2(2) . . . 2_676 ? C2 C3 C4 N2 -14.3(7) . . . . ? C2 C3 C4 C5 174.4(5) . . . . ? C2 C3 C4 Y1 -94.6(5) . . . 2_676 ? N2 C4 C5 Y1 -52.0(3) . . . 2_676 ? C3 C4 C5 Y1 119.4(4) . . . 2_676 ? C4 N2 C6 C7 -170.4(4) . . . . ? Y1 N2 C6 C7 21.5(4) . . . . ? Y1 N2 C6 C7 115.7(4) 2_676 . . . ? C4 N2 C6 Y1 73.8(3) . . . 2_676 ? Y1 N2 C6 Y1 -94.18(18) . . . 2_676 ? C8 N3 C7 C6 -174.4(4) . . . . ? Y1 N3 C7 C6 -9.7(5) . . . . ? C8 N3 C7 C9 4.8(6) . . . . ? Y1 N3 C7 C9 169.6(3) . . . . ? N2 C6 C7 N3 -7.6(6) . . . . ? Y1 C6 C7 N3 75.4(5) 2_676 . . . ? N2 C6 C7 C9 173.1(4) . . . . ? Y1 C6 C7 C9 -103.8(4) 2_676 . . . ? C7 N3 C8 C8A -3.6(7) . . . . ? Y1 N3 C8 C8A -166.5(4) . . . . ? N3 C7 C9 C9A -2.5(7) . . . . ? C6 C7 C9 C9A 176.8(5) . . . . ? C2 N1 C10 C11 -105.3(5) . . . . ? Y1 N1 C10 C11 66.9(5) . . . . ? C2 N1 C10 C15 77.8(5) . . . . ? Y1 N1 C10 C15 -110.0(4) . . . . ? N1 C10 C11 C12 -170.6(4) . . . . ? C15 C10 C11 C12 6.3(7) . . . . ? N1 C10 C11 C16 12.6(7) . . . . ? C15 C10 C11 C16 -170.6(4) . . . . ? C10 C11 C12 C13 -4.6(8) . . . . ? C16 C11 C12 C13 172.3(5) . . . . ? C11 C12 C13 C14 0.9(9) . . . . ? C12 C13 C14 C15 1.1(9) . . . . ? C13 C14 C15 C10 0.6(8) . . . . ? C13 C14 C15 C19 -178.8(5) . . . . ? C11 C10 C15 C14 -4.3(7) . . . . ? N1 C10 C15 C14 172.6(4) . . . . ? C11 C10 C15 C19 175.0(4) . . . . ? N1 C10 C15 C19 -8.1(6) . . . . ? C10 C11 C16 C18 -118.9(6) . . . . ? C12 C11 C16 C18 64.3(7) . . . . ? C10 C11 C16 C17 115.7(6) . . . . ? C12 C11 C16 C17 -61.2(7) . . . . ? C14 C15 C19 C20 -93.2(6) . . . . ? C10 C15 C19 C20 87.5(6) . . . . ? C14 C15 C19 C21 28.8(7) . . . . ? C10 C15 C19 C21 -150.5(5) . . . . ? C25 O1 C22 C23 -8.0(7) . . . . ? Y1 O1 C22 C23 164.9(5) . . . . ? O1 C22 C23 C24 10.4(9) . . . . ? C22 C23 C24 C25 -8.9(11) . . . . ? C23 C24 C25 O1 3.6(10) . . . . ? C22 O1 C25 C24 2.7(8) . . . . ? Y1 O1 C25 C24 -169.3(5) . . . . ? N3 C8 C8A C9A -0.3(9) . . . . ? C8 C8A C9A C9 2.8(9) . . . . ? C7 C9 C9A C8A -1.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.466 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.081 #===END data_cd2989 _database_code_depnum_ccdc_archive 'CCDC 744085' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H56 N3 O2 Si Y' _chemical_formula_weight 667.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6283(18) _cell_length_b 18.118(3) _cell_length_c 21.637(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.217(4) _cell_angle_gamma 90.00 _cell_volume 3714.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2521 _cell_measurement_theta_min 4.438 _cell_measurement_theta_max 38.994 _exptl_crystal_description prismatic _exptl_crystal_colour black _exptl_crystal_size_max 0.482 _exptl_crystal_size_mid 0.403 _exptl_crystal_size_min 0.170 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.634 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4434 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18865 _diffrn_reflns_av_R_equivalents 0.1445 _diffrn_reflns_av_sigmaI/netI 0.1873 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6889 _reflns_number_gt 3109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6889 _refine_ls_number_parameters 378 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1444 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1512 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _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 Y Y 0.15896(6) 0.26057(3) 0.17507(2) 0.04169(19) Uani 1 1 d . . . Si1 Si 0.3163(2) 0.40111(9) 0.06123(9) 0.0690(5) Uani 1 1 d . . . N1 N 0.0105(4) 0.1670(2) 0.13138(19) 0.0419(11) Uani 1 1 d . . . N2 N 0.0956(5) 0.2072(2) 0.2689(2) 0.0443(11) Uani 1 1 d . . . N3 N 0.2639(5) 0.3312(3) 0.2618(2) 0.0524(13) Uani 1 1 d . . . O1 O -0.0345(4) 0.33984(19) 0.17832(19) 0.0636(12) Uani 1 1 d . . . O2 O 0.3701(4) 0.1907(2) 0.20987(17) 0.0560(10) Uani 1 1 d . . . C1 C -0.1661(6) 0.0654(3) 0.1153(3) 0.0715(19) Uani 1 1 d . . . H1A H -0.2013 0.0283 0.1403 0.107 Uiso 1 1 calc R . . H1B H -0.1117 0.0423 0.0876 0.107 Uiso 1 1 calc R . . H1C H -0.2439 0.0915 0.0911 0.107 Uiso 1 1 calc R . . C2 C -0.0725(6) 0.1196(3) 0.1585(3) 0.0446(14) Uani 1 1 d . . . C3 C -0.0752(6) 0.1159(3) 0.2207(3) 0.0489(15) Uani 1 1 d . . . H3 H -0.1412 0.0828 0.2311 0.059 Uiso 1 1 calc R . . C4 C 0.0048(6) 0.1535(3) 0.2736(3) 0.0453(14) Uani 1 1 d . . . C5 C -0.0190(6) 0.1280(3) 0.3372(3) 0.0651(18) Uani 1 1 d . . . H5A H 0.0638 0.1029 0.3583 0.098 Uiso 1 1 calc R . . H5B H -0.0981 0.0950 0.3321 0.098 Uiso 1 1 calc R . . H5C H -0.0377 0.1699 0.3616 0.098 Uiso 1 1 calc R . . C6 C 0.1750(6) 0.2379(3) 0.3229(3) 0.0519(15) Uani 1 1 d . . . H6 H 0.1711 0.2171 0.3619 0.062 Uiso 1 1 calc R . . C7 C 0.2591(6) 0.2984(3) 0.3194(3) 0.0505(15) Uani 1 1 d . . . C8 C 0.3448(7) 0.3915(3) 0.2610(3) 0.0673(19) Uani 1 1 d . . . H8 H 0.3464 0.4130 0.2221 0.081 Uiso 1 1 calc R . . C9 C 0.3454(6) 0.3294(4) 0.3746(3) 0.0620(17) Uani 1 1 d . . . H9 H 0.3480 0.3074 0.4136 0.074 Uiso 1 1 calc R . . C8A C 0.4234(7) 0.4234(4) 0.3113(3) 0.079(2) Uani 1 1 d . . . H8A H 0.4763 0.4656 0.3076 0.095 Uiso 1 1 calc R . . C9A C 0.4223(7) 0.3907(4) 0.3693(3) 0.076(2) Uani 1 1 d . . . H9A H 0.4756 0.4114 0.4052 0.091 Uiso 1 1 calc R . . C10 C 0.0098(6) 0.1619(3) 0.0649(3) 0.0456(14) Uani 1 1 d . . . C11 C -0.0884(6) 0.2003(3) 0.0221(3) 0.0492(15) Uani 1 1 d . . . C12 C -0.0783(7) 0.1970(3) -0.0409(3) 0.0626(17) Uani 1 1 d . . . H12 H -0.1446 0.2216 -0.0702 0.075 Uiso 1 1 calc R . . C13 C 0.0277(8) 0.1581(4) -0.0611(3) 0.072(2) Uani 1 1 d . . . H13 H 0.0343 0.1577 -0.1034 0.086 Uiso 1 1 calc R . . C14 C 0.1230(7) 0.1201(4) -0.0189(3) 0.0641(18) Uani 1 1 d . . . H14 H 0.1926 0.0928 -0.0333 0.077 Uiso 1 1 calc R . . C15 C 0.1192(6) 0.1208(3) 0.0447(3) 0.0485(15) Uani 1 1 d . . . C16 C -0.2055(6) 0.2456(3) 0.0398(3) 0.0655(17) Uani 1 1 d . . . H16 H -0.1986 0.2413 0.0854 0.079 Uiso 1 1 calc R . . C18 C -0.1906(8) 0.3276(4) 0.0252(3) 0.097(2) Uani 1 1 d . . . H18A H -0.1008 0.3453 0.0465 0.146 Uiso 1 1 calc R . . H18B H -0.2647 0.3550 0.0392 0.146 Uiso 1 1 calc R . . H18C H -0.1970 0.3341 -0.0193 0.146 Uiso 1 1 calc R . . C17 C -0.3531(7) 0.2186(4) 0.0098(4) 0.109(3) Uani 1 1 d . . . H17A H -0.3668 0.2259 -0.0348 0.164 Uiso 1 1 calc R . . H17B H -0.4230 0.2458 0.0268 0.164 Uiso 1 1 calc R . . H17C H -0.3617 0.1670 0.0186 0.164 Uiso 1 1 calc R . . C19 C 0.2272(6) 0.0775(3) 0.0878(3) 0.0568(16) Uani 1 1 d . . . H19 H 0.2227 0.0934 0.1307 0.068 Uiso 1 1 calc R . . C20 C 0.1949(7) -0.0059(3) 0.0842(4) 0.098(3) Uani 1 1 d . . . H20A H 0.0949 -0.0134 0.0796 0.147 Uiso 1 1 calc R . . H20B H 0.2415 -0.0295 0.1219 0.147 Uiso 1 1 calc R . . H20C H 0.2282 -0.0267 0.0487 0.147 Uiso 1 1 calc R . . C21 C 0.3796(6) 0.0907(4) 0.0776(3) 0.084(2) Uani 1 1 d . . . H21A H 0.3879 0.0758 0.0358 0.126 Uiso 1 1 calc R . . H21B H 0.4436 0.0623 0.1075 0.126 Uiso 1 1 calc R . . H21C H 0.4022 0.1421 0.0830 0.126 Uiso 1 1 calc R . . C22 C 0.2536(6) 0.3159(3) 0.0904(3) 0.0652(18) Uani 1 1 d . . . H22A H 0.3332 0.2836 0.0886 0.078 Uiso 1 1 calc R . . H22B H 0.1833 0.3012 0.0547 0.078 Uiso 1 1 calc R . . C23 C 0.3491(8) 0.3969(4) -0.0209(3) 0.115(3) Uani 1 1 d . . . H23A H 0.4079 0.3552 -0.0255 0.172 Uiso 1 1 calc R . . H23B H 0.3954 0.4413 -0.0304 0.172 Uiso 1 1 calc R . . H23C H 0.2608 0.3920 -0.0493 0.172 Uiso 1 1 calc R . . C24 C 0.4943(8) 0.4229(5) 0.1084(4) 0.133(3) Uani 1 1 d . . . H24A H 0.5271 0.3817 0.1350 0.200 Uiso 1 1 calc R . . H24B H 0.4875 0.4657 0.1339 0.200 Uiso 1 1 calc R . . H24C H 0.5596 0.4325 0.0806 0.200 Uiso 1 1 calc R . . C25 C 0.2126(10) 0.4826(5) 0.0739(5) 0.170(4) Uiso 1 1 d . . . H25A H 0.1190 0.4779 0.0500 0.256 Uiso 1 1 calc R . . H25B H 0.2566 0.5259 0.0606 0.256 Uiso 1 1 calc R . . H25C H 0.2079 0.4867 0.1177 0.256 Uiso 1 1 calc R . . C26 C -0.0243(7) 0.4202(3) 0.1866(4) 0.097(3) Uani 1 1 d . . . H26A H -0.0668 0.4458 0.1486 0.117 Uiso 1 1 calc R . . H26B H 0.0732 0.4358 0.1985 0.117 Uiso 1 1 calc R . . C27 C -0.1045(12) 0.4333(6) 0.2380(5) 0.151(4) Uiso 1 1 d . . . H27A H -0.0410 0.4510 0.2750 0.193 Uiso 1 1 calc R . . H27B H -0.1756 0.4708 0.2254 0.193 Uiso 1 1 calc R . . C28 C -0.1718(8) 0.3655(5) 0.2531(4) 0.122(3) Uani 1 1 d . . . H28A H -0.1235 0.3450 0.2925 0.147 Uiso 1 1 calc R . . H28B H -0.2699 0.3741 0.2559 0.147 Uiso 1 1 calc R . . C29 C -0.1599(6) 0.3168(4) 0.2011(3) 0.0686(19) Uani 1 1 d . . . H29A H -0.1513 0.2659 0.2151 0.082 Uiso 1 1 calc R . . H29B H -0.2423 0.3212 0.1683 0.082 Uiso 1 1 calc R . . C30 C 0.5088(6) 0.2226(4) 0.2144(4) 0.077(2) Uani 1 1 d . . . H30A H 0.5024 0.2756 0.2083 0.092 Uiso 1 1 calc R . . H30B H 0.5576 0.2015 0.1830 0.092 Uiso 1 1 calc R . . C31 C 0.5840(8) 0.2048(5) 0.2786(4) 0.114(3) Uani 1 1 d . . . H31A H 0.6836 0.1967 0.2786 0.136 Uiso 1 1 calc R . . H31B H 0.5741 0.2447 0.3074 0.136 Uiso 1 1 calc R . . C32 C 0.5187(9) 0.1385(5) 0.2963(4) 0.138(4) Uani 1 1 d . . . H32A H 0.4969 0.1440 0.3382 0.166 Uiso 1 1 calc R . . H32B H 0.5826 0.0971 0.2967 0.166 Uiso 1 1 calc R . . C33 C 0.3856(7) 0.1247(3) 0.2500(3) 0.076(2) Uani 1 1 d . . . H33A H 0.3941 0.0806 0.2255 0.091 Uiso 1 1 calc R . . H33B H 0.3054 0.1192 0.2712 0.091 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 Y 0.0461(3) 0.0331(3) 0.0473(3) 0.0013(3) 0.0122(2) -0.0071(3) Si1 0.0977(14) 0.0448(10) 0.0750(13) 0.0130(9) 0.0281(11) -0.0039(9) N1 0.042(3) 0.040(3) 0.044(3) -0.002(2) 0.009(2) -0.006(2) N2 0.052(3) 0.039(3) 0.045(3) 0.002(2) 0.014(2) -0.005(2) N3 0.058(3) 0.050(3) 0.051(3) -0.005(3) 0.014(3) -0.016(3) O1 0.051(3) 0.042(2) 0.102(3) 0.003(2) 0.023(2) 0.004(2) O2 0.046(3) 0.049(2) 0.075(3) 0.008(2) 0.013(2) 0.000(2) C1 0.076(5) 0.065(4) 0.073(5) -0.011(4) 0.014(4) -0.035(4) C2 0.049(4) 0.032(3) 0.054(4) 0.000(3) 0.015(3) -0.006(3) C3 0.051(4) 0.041(3) 0.059(4) 0.000(3) 0.020(3) -0.014(3) C4 0.057(4) 0.035(3) 0.048(4) 0.005(3) 0.021(3) 0.004(3) C5 0.083(5) 0.061(4) 0.056(4) 0.001(3) 0.025(4) -0.013(4) C6 0.059(4) 0.054(4) 0.044(3) 0.002(3) 0.012(3) -0.006(3) C7 0.057(4) 0.051(4) 0.045(4) -0.006(3) 0.017(3) 0.001(3) C8 0.086(5) 0.050(4) 0.068(5) -0.007(4) 0.019(4) -0.026(4) C9 0.065(4) 0.073(5) 0.046(4) -0.005(4) 0.005(3) -0.008(4) C8A 0.089(6) 0.076(5) 0.071(5) -0.010(4) 0.012(4) -0.036(4) C9A 0.071(5) 0.086(5) 0.068(5) -0.024(4) 0.003(4) -0.025(4) C10 0.060(4) 0.038(3) 0.040(3) -0.005(3) 0.012(3) -0.020(3) C11 0.055(4) 0.038(3) 0.052(4) -0.001(3) 0.002(3) -0.009(3) C12 0.068(5) 0.065(4) 0.050(4) 0.009(4) -0.001(4) -0.005(4) C13 0.095(6) 0.079(5) 0.045(4) -0.011(4) 0.024(4) -0.016(4) C14 0.073(5) 0.063(4) 0.058(4) -0.010(4) 0.015(4) -0.013(4) C15 0.056(4) 0.039(3) 0.051(4) -0.006(3) 0.012(3) -0.014(3) C16 0.065(4) 0.062(5) 0.065(4) 0.003(4) 0.000(3) -0.002(4) C18 0.107(6) 0.062(5) 0.120(6) 0.008(5) 0.010(5) 0.018(4) C17 0.062(5) 0.117(7) 0.147(7) 0.011(6) 0.014(5) -0.002(5) C19 0.052(4) 0.056(4) 0.064(4) -0.010(3) 0.014(3) -0.001(3) C20 0.088(5) 0.053(4) 0.144(7) 0.022(5) -0.002(5) -0.012(4) C21 0.049(4) 0.100(6) 0.106(6) 0.004(5) 0.019(4) 0.000(4) C22 0.084(5) 0.053(4) 0.060(4) 0.013(3) 0.019(4) -0.013(3) C23 0.150(8) 0.122(7) 0.071(5) 0.024(5) 0.019(5) -0.041(6) C24 0.126(7) 0.157(9) 0.113(7) 0.013(6) 0.012(6) -0.077(7) C26 0.100(6) 0.038(4) 0.165(8) -0.001(5) 0.053(6) -0.003(4) C28 0.114(7) 0.146(8) 0.118(7) -0.028(7) 0.052(6) -0.044(6) C29 0.054(4) 0.064(4) 0.091(5) -0.001(4) 0.025(4) 0.007(3) C30 0.049(4) 0.073(5) 0.111(6) 0.009(4) 0.022(4) -0.017(4) C31 0.065(6) 0.120(8) 0.150(9) 0.009(7) 0.003(6) -0.005(5) C32 0.108(7) 0.130(8) 0.151(8) 0.061(7) -0.043(7) 0.004(6) C33 0.084(5) 0.053(4) 0.094(5) 0.016(4) 0.024(5) 0.013(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 Y N1 2.310(4) . ? Y N3 2.346(4) . ? Y O1 2.363(4) . ? Y O2 2.400(4) . ? Y C22 2.406(5) . ? Y N2 2.423(4) . ? Si1 C22 1.811(5) . ? Si1 C25 1.830(9) . ? Si1 C23 1.861(7) . ? Si1 C24 1.875(7) . ? N1 C2 1.372(6) . ? N1 C10 1.440(6) . ? N2 C4 1.324(6) . ? N2 C6 1.393(6) . ? N3 C8 1.344(7) . ? N3 C7 1.390(6) . ? O1 C29 1.445(6) . ? O1 C26 1.468(6) . ? O2 C30 1.442(6) . ? O2 C33 1.469(6) . ? C1 C2 1.533(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.353(7) . ? C3 C4 1.433(7) . ? C3 H3 0.9300 . ? C4 C5 1.506(7) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.373(7) . ? C6 H6 0.9300 . ? C7 C9 1.441(7) . ? C8 C8A 1.343(8) . ? C8 H8 0.9300 . ? C9 C9A 1.351(8) . ? C9 H9 0.9300 . ? C8A C9A 1.389(8) . ? C8A H8A 0.9300 . ? C9A H9A 0.9300 . ? C10 C11 1.388(7) . ? C10 C15 1.420(7) . ? C11 C12 1.385(7) . ? C11 C16 1.499(8) . ? C12 C13 1.373(8) . ? C12 H12 0.9300 . ? C13 C14 1.361(8) . ? C13 H13 0.9300 . ? C14 C15 1.384(7) . ? C14 H14 0.9300 . ? C15 C19 1.491(7) . ? C16 C18 1.532(8) . ? C16 C17 1.534(8) . ? C16 H16 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C19 C21 1.541(7) . ? C19 C20 1.543(8) . ? C19 H19 0.9800 . ? 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 0.9700 . ? C22 H22B 0.9700 . ? 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 C27 1.482(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.452(11) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.451(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.484(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.439(10) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.502(9) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y N3 151.07(16) . . ? N1 Y O1 91.40(14) . . ? N3 Y O1 82.78(15) . . ? N1 Y O2 99.78(14) . . ? N3 Y O2 79.41(14) . . ? O1 Y O2 159.98(14) . . ? N1 Y C22 106.57(17) . . ? N3 Y C22 102.35(18) . . ? O1 Y C22 100.15(18) . . ? O2 Y C22 92.55(17) . . ? N1 Y N2 79.65(15) . . ? N3 Y N2 71.60(15) . . ? O1 Y N2 84.31(14) . . ? O2 Y N2 81.47(13) . . ? C22 Y N2 172.12(18) . . ? C22 Si1 C25 114.3(4) . . ? C22 Si1 C23 114.9(3) . . ? C25 Si1 C23 111.4(4) . . ? C22 Si1 C24 108.6(3) . . ? C25 Si1 C24 102.6(4) . . ? C23 Si1 C24 103.6(3) . . ? C2 N1 C10 119.2(4) . . ? C2 N1 Y 130.5(3) . . ? C10 N1 Y 110.4(3) . . ? C4 N2 C6 120.0(5) . . ? C4 N2 Y 128.7(4) . . ? C6 N2 Y 111.2(3) . . ? C8 N3 C7 118.1(5) . . ? C8 N3 Y 127.0(4) . . ? C7 N3 Y 114.0(3) . . ? C29 O1 C26 106.7(4) . . ? C29 O1 Y 123.1(3) . . ? C26 O1 Y 124.8(4) . . ? C30 O2 C33 106.9(5) . . ? C30 O2 Y 122.2(4) . . ? C33 O2 Y 127.3(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 N1 124.8(5) . . ? C3 C2 C1 117.5(5) . . ? N1 C2 C1 117.7(5) . . ? C2 C3 C4 132.0(5) . . ? C2 C3 H3 114.0 . . ? C4 C3 H3 114.0 . . ? N2 C4 C3 123.8(5) . . ? N2 C4 C5 120.3(5) . . ? C3 C4 C5 115.9(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 N2 120.9(5) . . ? C7 C6 H6 119.5 . . ? N2 C6 H6 119.5 . . ? C6 C7 N3 120.3(5) . . ? C6 C7 C9 121.6(5) . . ? N3 C7 C9 118.0(5) . . ? C8A C8 N3 125.7(6) . . ? C8A C8 H8 117.1 . . ? N3 C8 H8 117.1 . . ? C9A C9 C7 119.6(6) . . ? C9A C9 H9 120.2 . . ? C7 C9 H9 120.2 . . ? C8 C8A C9A 117.1(6) . . ? C8 C8A H8A 121.4 . . ? C9A C8A H8A 121.4 . . ? C9 C9A C8A 121.3(6) . . ? C9 C9A H9A 119.4 . . ? C8A C9A H9A 119.4 . . ? C11 C10 C15 120.8(5) . . ? C11 C10 N1 121.1(5) . . ? C15 C10 N1 117.9(5) . . ? C12 C11 C10 118.5(6) . . ? C12 C11 C16 117.6(6) . . ? C10 C11 C16 123.9(5) . . ? C13 C12 C11 121.4(6) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 119.8(6) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 121.9(6) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C14 C15 C10 117.6(6) . . ? C14 C15 C19 118.6(6) . . ? C10 C15 C19 123.8(5) . . ? C11 C16 C18 112.1(5) . . ? C11 C16 C17 113.5(5) . . ? C18 C16 C17 109.7(5) . . ? C11 C16 H16 107.1 . . ? C18 C16 H16 107.1 . . ? C17 C16 H16 107.1 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C19 C21 113.9(5) . . ? C15 C19 C20 111.8(5) . . ? C21 C19 C20 109.4(5) . . ? C15 C19 H19 107.1 . . ? C21 C19 H19 107.1 . . ? C20 C19 H19 107.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 Y 144.6(3) . . ? Si1 C22 H22A 100.7 . . ? Y C22 H22A 100.7 . . ? Si1 C22 H22B 100.7 . . ? Y C22 H22B 100.7 . . ? H22A C22 H22B 104.4 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O1 C26 C27 102.6(6) . . ? O1 C26 H26A 111.3 . . ? C27 C26 H26A 111.3 . . ? O1 C26 H26B 111.3 . . ? C27 C26 H26B 111.3 . . ? H26A C26 H26B 109.2 . . ? C28 C27 C26 110.2(8) . . ? C28 C27 H27A 109.6 . . ? C26 C27 H27A 109.6 . . ? C28 C27 H27B 109.6 . . ? C26 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? C29 C28 C27 104.0(7) . . ? C29 C28 H28A 111.0 . . ? C27 C28 H28A 111.0 . . ? C29 C28 H28B 111.0 . . ? C27 C28 H28B 111.0 . . ? H28A C28 H28B 109.0 . . ? O1 C29 C28 105.9(6) . . ? O1 C29 H29A 110.6 . . ? C28 C29 H29A 110.6 . . ? O1 C29 H29B 110.6 . . ? C28 C29 H29B 110.6 . . ? H29A C29 H29B 108.7 . . ? O2 C30 C31 105.6(6) . . ? O2 C30 H30A 110.6 . . ? C31 C30 H30A 110.6 . . ? O2 C30 H30B 110.6 . . ? C31 C30 H30B 110.6 . . ? H30A C30 H30B 108.8 . . ? C32 C31 C30 105.5(7) . . ? C32 C31 H31A 110.6 . . ? C30 C31 H31A 110.6 . . ? C32 C31 H31B 110.6 . . ? C30 C31 H31B 110.6 . . ? H31A C31 H31B 108.8 . . ? C31 C32 C33 108.8(7) . . ? C31 C32 H32A 109.9 . . ? C33 C32 H32A 109.9 . . ? C31 C32 H32B 109.9 . . ? C33 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? O2 C33 C32 104.1(6) . . ? O2 C33 H33A 110.9 . . ? C32 C33 H33A 110.9 . . ? O2 C33 H33B 110.9 . . ? C32 C33 H33B 110.9 . . ? H33A C33 H33B 109.0 . . ? 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 N3 Y N1 C2 0.5(6) . . . . ? O1 Y N1 C2 -77.0(4) . . . . ? O2 Y N1 C2 86.3(4) . . . . ? C22 Y N1 C2 -178.1(4) . . . . ? N2 Y N1 C2 6.9(4) . . . . ? N3 Y N1 C10 179.6(4) . . . . ? O1 Y N1 C10 102.1(4) . . . . ? O2 Y N1 C10 -94.6(4) . . . . ? C22 Y N1 C10 1.1(4) . . . . ? N2 Y N1 C10 -174.0(4) . . . . ? N1 Y N2 C4 -4.6(4) . . . . ? N3 Y N2 C4 172.1(5) . . . . ? O1 Y N2 C4 87.8(4) . . . . ? O2 Y N2 C4 -106.3(4) . . . . ? C22 Y N2 C4 -147.3(12) . . . . ? N1 Y N2 C6 172.2(4) . . . . ? N3 Y N2 C6 -11.1(3) . . . . ? O1 Y N2 C6 -95.4(3) . . . . ? O2 Y N2 C6 70.5(3) . . . . ? C22 Y N2 C6 29.5(14) . . . . ? N1 Y N3 C8 -172.9(4) . . . . ? O1 Y N3 C8 -93.1(5) . . . . ? O2 Y N3 C8 96.0(5) . . . . ? C22 Y N3 C8 5.7(5) . . . . ? N2 Y N3 C8 -179.5(5) . . . . ? N1 Y N3 C7 18.7(6) . . . . ? O1 Y N3 C7 98.4(4) . . . . ? O2 Y N3 C7 -72.4(4) . . . . ? C22 Y N3 C7 -162.7(4) . . . . ? N2 Y N3 C7 12.0(4) . . . . ? N1 Y O1 C29 46.1(4) . . . . ? N3 Y O1 C29 -105.4(4) . . . . ? O2 Y O1 C29 -78.2(6) . . . . ? C22 Y O1 C29 153.3(4) . . . . ? N2 Y O1 C29 -33.3(4) . . . . ? N1 Y O1 C26 -163.5(5) . . . . ? N3 Y O1 C26 44.9(5) . . . . ? O2 Y O1 C26 72.2(7) . . . . ? C22 Y O1 C26 -56.4(5) . . . . ? N2 Y O1 C26 117.1(5) . . . . ? N1 Y O2 C30 151.1(4) . . . . ? N3 Y O2 C30 -58.3(4) . . . . ? O1 Y O2 C30 -85.9(6) . . . . ? C22 Y O2 C30 43.8(4) . . . . ? N2 Y O2 C30 -131.0(4) . . . . ? N1 Y O2 C33 -53.3(4) . . . . ? N3 Y O2 C33 97.3(4) . . . . ? O1 Y O2 C33 69.8(6) . . . . ? C22 Y O2 C33 -160.6(4) . . . . ? N2 Y O2 C33 24.6(4) . . . . ? C10 N1 C2 C3 176.0(5) . . . . ? Y N1 C2 C3 -4.9(8) . . . . ? C10 N1 C2 C1 -2.2(7) . . . . ? Y N1 C2 C1 176.9(4) . . . . ? N1 C2 C3 C4 -3.5(10) . . . . ? C1 C2 C3 C4 174.7(6) . . . . ? C6 N2 C4 C3 -176.3(5) . . . . ? Y N2 C4 C3 0.3(8) . . . . ? C6 N2 C4 C5 3.2(8) . . . . ? Y N2 C4 C5 179.7(4) . . . . ? C2 C3 C4 N2 5.8(10) . . . . ? C2 C3 C4 C5 -173.7(6) . . . . ? C4 N2 C6 C7 -173.3(5) . . . . ? Y N2 C6 C7 9.6(6) . . . . ? N2 C6 C7 N3 1.4(8) . . . . ? N2 C6 C7 C9 -178.0(5) . . . . ? C8 N3 C7 C6 178.2(5) . . . . ? Y N3 C7 C6 -12.2(7) . . . . ? C8 N3 C7 C9 -2.3(8) . . . . ? Y N3 C7 C9 167.2(4) . . . . ? C7 N3 C8 C8A 0.4(10) . . . . ? Y N3 C8 C8A -167.6(5) . . . . ? C6 C7 C9 C9A -177.5(6) . . . . ? N3 C7 C9 C9A 3.1(9) . . . . ? N3 C8 C8A C9A 0.8(11) . . . . ? C7 C9 C9A C8A -1.9(10) . . . . ? C8 C8A C9A C9 0.0(11) . . . . ? C2 N1 C10 C11 87.5(6) . . . . ? Y N1 C10 C11 -91.8(5) . . . . ? C2 N1 C10 C15 -97.1(6) . . . . ? Y N1 C10 C15 83.7(5) . . . . ? C15 C10 C11 C12 0.7(8) . . . . ? N1 C10 C11 C12 176.0(5) . . . . ? C15 C10 C11 C16 -179.2(5) . . . . ? N1 C10 C11 C16 -3.9(8) . . . . ? C10 C11 C12 C13 -1.3(9) . . . . ? C16 C11 C12 C13 178.5(5) . . . . ? C11 C12 C13 C14 1.9(10) . . . . ? C12 C13 C14 C15 -1.8(10) . . . . ? C13 C14 C15 C10 1.2(9) . . . . ? C13 C14 C15 C19 179.8(5) . . . . ? C11 C10 C15 C14 -0.6(8) . . . . ? N1 C10 C15 C14 -176.0(5) . . . . ? C11 C10 C15 C19 -179.2(5) . . . . ? N1 C10 C15 C19 5.4(7) . . . . ? C12 C11 C16 C18 -63.9(7) . . . . ? C10 C11 C16 C18 116.0(6) . . . . ? C12 C11 C16 C17 61.0(7) . . . . ? C10 C11 C16 C17 -119.1(6) . . . . ? C14 C15 C19 C21 48.7(7) . . . . ? C10 C15 C19 C21 -132.7(6) . . . . ? C14 C15 C19 C20 -75.9(7) . . . . ? C10 C15 C19 C20 102.7(6) . . . . ? C25 Si1 C22 Y -40.2(7) . . . . ? C23 Si1 C22 Y -170.8(5) . . . . ? C24 Si1 C22 Y 73.7(7) . . . . ? N1 Y C22 Si1 148.1(5) . . . . ? N3 Y C22 Si1 -31.2(6) . . . . ? O1 Y C22 Si1 53.6(6) . . . . ? O2 Y C22 Si1 -110.9(6) . . . . ? N2 Y C22 Si1 -70.4(15) . . . . ? C29 O1 C26 C27 24.5(8) . . . . ? Y O1 C26 C27 -129.9(5) . . . . ? O1 C26 C27 C28 -6.7(10) . . . . ? C26 C27 C28 C29 -13.2(11) . . . . ? C26 O1 C29 C28 -34.0(7) . . . . ? Y O1 C29 C28 121.0(5) . . . . ? C27 C28 C29 O1 28.5(9) . . . . ? C33 O2 C30 C31 -31.1(7) . . . . ? Y O2 C30 C31 128.8(5) . . . . ? O2 C30 C31 C32 26.4(9) . . . . ? C30 C31 C32 C33 -11.9(11) . . . . ? C30 O2 C33 C32 23.2(7) . . . . ? Y O2 C33 C32 -135.4(5) . . . . ? C31 C32 C33 O2 -6.6(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.753 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.074 #===END data_cd29199 _database_code_depnum_ccdc_archive 'CCDC 759490' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H66 N5 Si4 Y' _chemical_formula_weight 758.20 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.1051(19) _cell_length_b 12.0332(11) _cell_length_c 18.0092(18) _cell_angle_alpha 90.00 _cell_angle_beta 93.836(2) _cell_angle_gamma 90.00 _cell_volume 4347.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3094 _cell_measurement_theta_min 4.484 _cell_measurement_theta_max 39.915 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.398 _exptl_crystal_size_mid 0.357 _exptl_crystal_size_min 0.168 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 1.480 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6619 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25104 _diffrn_reflns_av_R_equivalents 0.1102 _diffrn_reflns_av_sigmaI/netI 0.1547 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9469 _reflns_number_gt 4561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 [0.00000+1.00000exp(2.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0393P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _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 9469 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1135 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1068 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 Y Y 0.274240(18) 0.48695(3) 0.70084(2) 0.03484(12) Uani 1 1 d . . . Si1 Si 0.44471(6) 0.49031(10) 0.77418(7) 0.0481(3) Uani 1 1 d . . . Si2 Si 0.34566(6) 0.57356(10) 0.87106(7) 0.0516(3) Uani 1 1 d . . . Si3 Si 0.18685(6) 0.27646(10) 0.60953(8) 0.0562(4) Uani 1 1 d . . . Si4 Si 0.24750(6) 0.20800(9) 0.75710(8) 0.0536(4) Uani 1 1 d . . . N1 N 0.17798(16) 0.6017(2) 0.69793(18) 0.0424(8) Uani 1 1 d . . . N2 N 0.29822(16) 0.6304(3) 0.62193(18) 0.0443(9) Uani 1 1 d . . . N3 N 0.34322(16) 0.4274(3) 0.59730(18) 0.0431(8) Uani 1 1 d . . . N4 N 0.36183(16) 0.5152(2) 0.78730(17) 0.0426(8) Uani 1 1 d . . . N5 N 0.23208(15) 0.3105(2) 0.69144(18) 0.0414(8) Uani 1 1 d . . . C1 C 0.1462(2) 0.7760(4) 0.7601(3) 0.0630(13) Uani 1 1 d . . . H1A H 0.1023 0.7449 0.7529 0.094 Uiso 1 1 calc R . . H1B H 0.1465 0.8492 0.7389 0.094 Uiso 1 1 calc R . . H1C H 0.1589 0.7800 0.8123 0.094 Uiso 1 1 calc R . . C2 C 0.1947(2) 0.7035(3) 0.7225(2) 0.0458(10) Uani 1 1 d . . . C3 C 0.2571(2) 0.7496(3) 0.7128(2) 0.0495(11) Uani 1 1 d . . . H3 H 0.2723 0.8017 0.7481 0.059 Uiso 1 1 calc R . . C4 C 0.2996(2) 0.7263(3) 0.6559(2) 0.0500(11) Uani 1 1 d . . . C5 C 0.3446(3) 0.8195(4) 0.6351(3) 0.0863(18) Uani 1 1 d . . . H5A H 0.3880 0.7905 0.6272 0.129 Uiso 1 1 calc R . . H5B H 0.3480 0.8734 0.6745 0.129 Uiso 1 1 calc R . . H5C H 0.3264 0.8542 0.5902 0.129 Uiso 1 1 calc R . . C6 C 0.3308(2) 0.6160(4) 0.5523(3) 0.0634(14) Uani 1 1 d . . . H6A H 0.3675 0.6682 0.5510 0.076 Uiso 1 1 calc R . . H6B H 0.2992 0.6326 0.5108 0.076 Uiso 1 1 calc R . . C7 C 0.3564(2) 0.5014(3) 0.5441(2) 0.0496(10) Uani 1 1 d . . . C8 C 0.3679(2) 0.3239(4) 0.5915(2) 0.0516(11) Uani 1 1 d . . . H8 H 0.3578 0.2714 0.6268 0.062 Uiso 1 1 calc R . . C9 C 0.3940(3) 0.4733(4) 0.4857(3) 0.0691(14) Uani 1 1 d . . . H9 H 0.4010 0.5251 0.4487 0.083 Uiso 1 1 calc R . . C10 C 0.1081(2) 0.5853(3) 0.6758(3) 0.0481(11) Uani 1 1 d . . . C11 C 0.0828(2) 0.6306(4) 0.6075(3) 0.0614(13) Uani 1 1 d . . . C12 C 0.0172(3) 0.6127(5) 0.5844(3) 0.0834(17) Uani 1 1 d . . . H12 H 0.0004 0.6411 0.5389 0.100 Uiso 1 1 calc R . . C13 C -0.0238(3) 0.5538(5) 0.6273(4) 0.0913(19) Uani 1 1 d . . . H13 H -0.0682 0.5429 0.6109 0.110 Uiso 1 1 calc R . . C14 C 0.0000(3) 0.5109(4) 0.6942(4) 0.0778(16) Uani 1 1 d . . . H14 H -0.0286 0.4710 0.7228 0.093 Uiso 1 1 calc R . . C15 C 0.0661(2) 0.5256(4) 0.7205(3) 0.0585(12) Uani 1 1 d . . . C16 C 0.1260(3) 0.7028(4) 0.5599(3) 0.0754(15) Uani 1 1 d . . . H16 H 0.1724 0.6959 0.5795 0.090 Uiso 1 1 calc R . . C17 C 0.1063(4) 0.8260(5) 0.5631(3) 0.115(2) Uani 1 1 d . . . H17A H 0.0616 0.8352 0.5416 0.172 Uiso 1 1 calc R . . H17B H 0.1363 0.8693 0.5356 0.172 Uiso 1 1 calc R . . H17C H 0.1087 0.8503 0.6139 0.172 Uiso 1 1 calc R . . C18 C 0.1222(3) 0.6687(5) 0.4775(3) 0.103(2) Uani 1 1 d . . . H18A H 0.1302 0.5903 0.4737 0.154 Uiso 1 1 calc R . . H18B H 0.1553 0.7086 0.4522 0.154 Uiso 1 1 calc R . . H18C H 0.0787 0.6859 0.4551 0.154 Uiso 1 1 calc R . . C19 C 0.0885(2) 0.4807(4) 0.7966(3) 0.0752(15) Uani 1 1 d . . . H19 H 0.1371 0.4891 0.8026 0.090 Uiso 1 1 calc R . . C20 C 0.0731(3) 0.3591(5) 0.8078(3) 0.113(2) Uani 1 1 d . . . H20A H 0.0257 0.3483 0.8041 0.169 Uiso 1 1 calc R . . H20B H 0.0910 0.3360 0.8561 0.169 Uiso 1 1 calc R . . H20C H 0.0929 0.3158 0.7703 0.169 Uiso 1 1 calc R . . C21 C 0.0591(4) 0.5454(5) 0.8596(4) 0.131(3) Uani 1 1 d . . . H21A H 0.0720 0.6220 0.8569 0.197 Uiso 1 1 calc R . . H21B H 0.0755 0.5149 0.9066 0.197 Uiso 1 1 calc R . . H21C H 0.0114 0.5398 0.8549 0.197 Uiso 1 1 calc R . . C22 C 0.4740(2) 0.5433(5) 0.6839(3) 0.0787(16) Uani 1 1 d . . . H22A H 0.4621 0.4911 0.6449 0.118 Uiso 1 1 calc R . . H22B H 0.5216 0.5521 0.6884 0.118 Uiso 1 1 calc R . . H22C H 0.4534 0.6137 0.6722 0.118 Uiso 1 1 calc R . . C23 C 0.5064(2) 0.5559(5) 0.8439(3) 0.0757(15) Uani 1 1 d . . . H23A H 0.4999 0.6349 0.8439 0.114 Uiso 1 1 calc R . . H23B H 0.5509 0.5394 0.8307 0.114 Uiso 1 1 calc R . . H23C H 0.5000 0.5268 0.8925 0.114 Uiso 1 1 calc R . . C24 C 0.4640(3) 0.3388(4) 0.7785(4) 0.0938(19) Uani 1 1 d . . . H24A H 0.4603 0.3124 0.8283 0.141 Uiso 1 1 calc R . . H24B H 0.5086 0.3266 0.7641 0.141 Uiso 1 1 calc R . . H24C H 0.4331 0.2993 0.7452 0.141 Uiso 1 1 calc R . . C25 C 0.3743(3) 0.7218(4) 0.8806(3) 0.0759(15) Uani 1 1 d . . . H25A H 0.4116 0.7261 0.9167 0.114 Uiso 1 1 calc R . . H25B H 0.3386 0.7670 0.8964 0.114 Uiso 1 1 calc R . . H25C H 0.3875 0.7481 0.8334 0.114 Uiso 1 1 calc R . . C26 C 0.3809(3) 0.4930(4) 0.9549(2) 0.0797(15) Uani 1 1 d . . . H26A H 0.3871 0.4168 0.9413 0.120 Uiso 1 1 calc R . . H26B H 0.3504 0.4968 0.9937 0.120 Uiso 1 1 calc R . . H26C H 0.4229 0.5245 0.9724 0.120 Uiso 1 1 calc R . . C27 C 0.2537(2) 0.5774(4) 0.8847(3) 0.0751(15) Uani 1 1 d . . . H27A H 0.2320 0.6265 0.8487 0.113 Uiso 1 1 calc R . . H27B H 0.2467 0.6035 0.9339 0.113 Uiso 1 1 calc R . . H27C H 0.2354 0.5040 0.8783 0.113 Uiso 1 1 calc R . . C28 C 0.2179(3) 0.1489(4) 0.5619(3) 0.0829(17) Uani 1 1 d . . . H28A H 0.2645 0.1573 0.5545 0.124 Uiso 1 1 calc R . . H28B H 0.1936 0.1396 0.5147 0.124 Uiso 1 1 calc R . . H28C H 0.2115 0.0848 0.5924 0.124 Uiso 1 1 calc R . . C29 C 0.1897(3) 0.3937(4) 0.5409(3) 0.0757(15) Uani 1 1 d . . . H29A H 0.1902 0.4634 0.5669 0.114 Uiso 1 1 calc R . . H29B H 0.1511 0.3904 0.5065 0.114 Uiso 1 1 calc R . . H29C H 0.2292 0.3873 0.5140 0.114 Uiso 1 1 calc R . . C30 C 0.0961(2) 0.2518(5) 0.6170(3) 0.0918(18) Uani 1 1 d . . . H30A H 0.0900 0.1940 0.6527 0.138 Uiso 1 1 calc R . . H30B H 0.0761 0.2297 0.5694 0.138 Uiso 1 1 calc R . . H30C H 0.0754 0.3189 0.6328 0.138 Uiso 1 1 calc R . . C31 C 0.3208(2) 0.1187(4) 0.7405(3) 0.0800(17) Uani 1 1 d . . . H31A H 0.3149 0.0859 0.6919 0.120 Uiso 1 1 calc R . . H31B H 0.3246 0.0610 0.7774 0.120 Uiso 1 1 calc R . . H31C H 0.3605 0.1631 0.7436 0.120 Uiso 1 1 calc R . . C32 C 0.2671(3) 0.2687(4) 0.8518(3) 0.0867(17) Uani 1 1 d . . . H32A H 0.3032 0.3205 0.8499 0.130 Uiso 1 1 calc R . . H32B H 0.2796 0.2103 0.8863 0.130 Uiso 1 1 calc R . . H32C H 0.2284 0.3064 0.8679 0.130 Uiso 1 1 calc R . . C33 C 0.1784(3) 0.1046(4) 0.7666(3) 0.092(2) Uani 1 1 d . . . H33A H 0.1379 0.1433 0.7752 0.137 Uiso 1 1 calc R . . H33B H 0.1898 0.0559 0.8077 0.137 Uiso 1 1 calc R . . H33C H 0.1722 0.0618 0.7217 0.137 Uiso 1 1 calc R . . C8A C 0.4076(2) 0.2923(4) 0.5354(3) 0.0657(14) Uani 1 1 d . . . H8A H 0.4250 0.2208 0.5337 0.079 Uiso 1 1 calc R . . C9A C 0.4207(3) 0.3700(5) 0.4821(3) 0.0770(16) Uani 1 1 d . . . H9A H 0.4476 0.3517 0.4439 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.0400(2) 0.0314(2) 0.0333(2) -0.00009(18) 0.00418(15) -0.00155(18) Si1 0.0434(7) 0.0492(7) 0.0513(7) -0.0042(6) -0.0003(5) -0.0031(6) Si2 0.0615(8) 0.0577(8) 0.0352(7) -0.0034(6) 0.0005(6) 0.0043(7) Si3 0.0551(8) 0.0531(8) 0.0603(9) -0.0146(6) 0.0027(7) -0.0078(6) Si4 0.0617(8) 0.0353(6) 0.0656(9) 0.0047(6) 0.0173(7) -0.0038(6) N1 0.049(2) 0.0380(19) 0.040(2) 0.0026(15) 0.0037(17) 0.0015(16) N2 0.057(2) 0.0356(19) 0.042(2) 0.0087(16) 0.0105(18) 0.0022(16) N3 0.049(2) 0.044(2) 0.038(2) -0.0012(16) 0.0078(17) -0.0045(17) N4 0.056(2) 0.0383(18) 0.0340(18) -0.0046(15) 0.0026(15) 0.0020(16) N5 0.046(2) 0.0354(18) 0.044(2) -0.0044(15) 0.0086(17) -0.0038(15) C1 0.072(3) 0.052(3) 0.065(3) -0.016(2) 0.007(3) 0.004(3) C2 0.057(3) 0.040(2) 0.041(3) 0.0031(19) 0.003(2) 0.005(2) C3 0.054(3) 0.040(2) 0.053(3) -0.006(2) -0.005(2) -0.004(2) C4 0.053(3) 0.038(2) 0.058(3) 0.011(2) -0.003(2) -0.003(2) C5 0.090(4) 0.055(3) 0.117(5) 0.009(3) 0.029(4) -0.016(3) C6 0.081(4) 0.055(3) 0.056(3) 0.011(2) 0.021(3) -0.001(3) C7 0.055(3) 0.054(3) 0.040(2) -0.002(2) 0.005(2) -0.005(2) C8 0.062(3) 0.048(3) 0.045(3) -0.007(2) 0.005(2) 0.000(2) C9 0.089(4) 0.075(3) 0.046(3) -0.002(3) 0.025(3) -0.001(3) C10 0.039(3) 0.044(2) 0.061(3) -0.014(2) -0.001(2) 0.005(2) C11 0.052(3) 0.069(3) 0.062(3) -0.007(3) -0.011(3) 0.010(3) C12 0.066(4) 0.104(4) 0.077(4) -0.002(3) -0.019(3) 0.015(3) C13 0.052(4) 0.110(5) 0.110(6) -0.027(4) -0.016(4) 0.005(3) C14 0.051(3) 0.077(4) 0.107(5) -0.015(4) 0.018(3) -0.001(3) C15 0.044(3) 0.058(3) 0.074(4) -0.009(3) 0.008(2) 0.003(2) C16 0.087(4) 0.086(4) 0.051(3) 0.009(3) -0.015(3) -0.002(3) C17 0.183(7) 0.079(4) 0.083(5) 0.007(3) 0.008(5) 0.002(5) C18 0.140(6) 0.107(5) 0.059(4) 0.003(3) -0.012(4) 0.023(4) C19 0.048(3) 0.090(4) 0.089(4) 0.019(3) 0.016(3) -0.011(3) C20 0.154(6) 0.078(4) 0.111(6) 0.016(4) 0.054(5) 0.019(4) C21 0.217(8) 0.095(5) 0.084(5) -0.013(4) 0.026(5) -0.008(5) C22 0.063(3) 0.111(4) 0.062(4) -0.006(3) 0.010(3) -0.028(3) C23 0.053(3) 0.105(4) 0.068(4) -0.008(3) -0.001(3) -0.015(3) C24 0.074(4) 0.060(3) 0.147(6) -0.007(4) 0.008(4) 0.010(3) C25 0.103(4) 0.063(3) 0.061(4) -0.024(3) -0.002(3) 0.007(3) C26 0.086(4) 0.110(4) 0.042(3) 0.010(3) -0.003(3) 0.016(3) C27 0.088(4) 0.089(4) 0.050(3) 0.006(3) 0.015(3) 0.018(3) C28 0.103(4) 0.071(3) 0.075(4) -0.031(3) 0.003(3) -0.008(3) C29 0.081(4) 0.079(4) 0.064(4) -0.010(3) -0.013(3) -0.001(3) C30 0.067(4) 0.108(5) 0.099(5) -0.020(4) -0.007(3) -0.017(3) C31 0.081(4) 0.062(3) 0.098(5) 0.015(3) 0.019(3) 0.011(3) C32 0.128(5) 0.070(3) 0.062(4) 0.013(3) 0.006(3) -0.007(3) C33 0.090(4) 0.055(3) 0.133(6) 0.023(3) 0.033(4) -0.019(3) C8A 0.074(3) 0.056(3) 0.068(4) -0.016(3) 0.013(3) 0.007(3) C9A 0.094(4) 0.087(4) 0.054(4) -0.013(3) 0.033(3) 0.004(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 Y N5 2.288(3) . ? Y N4 2.297(3) . ? Y N2 2.308(3) . ? Y N1 2.375(3) . ? Y N3 2.502(3) . ? Si1 N4 1.725(3) . ? Si1 C24 1.865(5) . ? Si1 C22 1.877(5) . ? Si1 C23 1.878(5) . ? Si2 N4 1.715(3) . ? Si2 C25 1.879(5) . ? Si2 C27 1.882(5) . ? Si2 C26 1.892(5) . ? Si3 N5 1.730(3) . ? Si3 C30 1.863(5) . ? Si3 C29 1.880(5) . ? Si3 C28 1.885(4) . ? Si4 N5 1.723(3) . ? Si4 C31 1.864(5) . ? Si4 C32 1.873(5) . ? Si4 C33 1.881(5) . ? N1 C2 1.338(5) . ? N1 C10 1.447(5) . ? N2 C4 1.305(5) . ? N2 C6 1.463(5) . ? N3 C7 1.346(5) . ? N3 C8 1.347(5) . ? C1 C2 1.503(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.392(5) . ? C3 C4 1.406(6) . ? C3 H3 0.9300 . ? C4 C5 1.505(5) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.484(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C9 1.378(6) . ? C8 C8A 1.382(5) . ? C8 H8 0.9300 . ? C9 C9A 1.357(6) . ? C9 H9 0.9300 . ? C10 C15 1.402(6) . ? C10 C11 1.410(6) . ? C11 C12 1.374(7) . ? C11 C16 1.531(6) . ? C12 C13 1.365(7) . ? C12 H12 0.9300 . ? C13 C14 1.369(8) . ? C13 H13 0.9300 . ? C14 C15 1.393(7) . ? C14 H14 0.9300 . ? C15 C19 1.513(7) . ? C16 C17 1.535(7) . ? C16 C18 1.537(6) . ? C16 H16 0.9800 . ? 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 C20 1.512(7) . ? C19 C21 1.527(7) . ? C19 H19 0.9800 . ? 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 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C8A C9A 1.377(6) . ? C8A H8A 0.9300 . ? C9A H9A 0.9300 . ? 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 N5 Y N4 116.81(11) . . ? N5 Y N2 137.76(12) . . ? N4 Y N2 97.14(12) . . ? N5 Y N1 103.91(11) . . ? N4 Y N1 121.04(11) . . ? N2 Y N1 75.82(11) . . ? N5 Y N3 84.28(10) . . ? N4 Y N3 96.29(11) . . ? N2 Y N3 66.81(11) . . ? N1 Y N3 129.91(11) . . ? N4 Si1 C24 111.4(2) . . ? N4 Si1 C22 115.0(2) . . ? C24 Si1 C22 106.9(2) . . ? N4 Si1 C23 115.88(19) . . ? C24 Si1 C23 104.9(3) . . ? C22 Si1 C23 101.8(2) . . ? N4 Si2 C25 113.18(19) . . ? N4 Si2 C27 111.7(2) . . ? C25 Si2 C27 105.3(2) . . ? N4 Si2 C26 114.19(19) . . ? C25 Si2 C26 108.5(2) . . ? C27 Si2 C26 103.1(2) . . ? N5 Si3 C30 116.0(2) . . ? N5 Si3 C29 110.24(19) . . ? C30 Si3 C29 103.9(2) . . ? N5 Si3 C28 114.2(2) . . ? C30 Si3 C28 105.0(2) . . ? C29 Si3 C28 106.7(2) . . ? N5 Si4 C31 114.24(19) . . ? N5 Si4 C32 111.29(19) . . ? C31 Si4 C32 104.6(3) . . ? N5 Si4 C33 115.8(2) . . ? C31 Si4 C33 103.3(2) . . ? C32 Si4 C33 106.6(2) . . ? C2 N1 C10 115.7(3) . . ? C2 N1 Y 109.8(3) . . ? C10 N1 Y 134.5(2) . . ? C4 N2 C6 120.7(3) . . ? C4 N2 Y 111.8(3) . . ? C6 N2 Y 124.2(2) . . ? C7 N3 C8 117.6(3) . . ? C7 N3 Y 119.1(3) . . ? C8 N3 Y 123.3(3) . . ? Si2 N4 Si1 115.69(19) . . ? Si2 N4 Y 118.37(16) . . ? Si1 N4 Y 125.83(16) . . ? Si4 N5 Si3 118.43(18) . . ? Si4 N5 Y 124.40(17) . . ? Si3 N5 Y 116.99(16) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 122.2(4) . . ? N1 C2 C1 121.6(4) . . ? C3 C2 C1 116.2(4) . . ? C2 C3 C4 127.4(4) . . ? C2 C3 H3 116.3 . . ? C4 C3 H3 116.3 . . ? N2 C4 C3 121.6(4) . . ? N2 C4 C5 122.4(4) . . ? C3 C4 C5 116.0(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 112.0(3) . . ? N2 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N3 C7 C9 121.7(4) . . ? N3 C7 C6 117.2(3) . . ? C9 C7 C6 121.0(4) . . ? N3 C8 C8A 123.0(4) . . ? N3 C8 H8 118.5 . . ? C8A C8 H8 118.5 . . ? C9A C9 C7 120.0(4) . . ? C9A C9 H9 120.0 . . ? C7 C9 H9 120.0 . . ? C15 C10 C11 120.2(4) . . ? C15 C10 N1 121.5(4) . . ? C11 C10 N1 118.3(4) . . ? C12 C11 C10 119.1(5) . . ? C12 C11 C16 119.2(5) . . ? C10 C11 C16 121.6(4) . . ? C13 C12 C11 120.9(6) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 120.4(5) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 121.4(5) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C14 C15 C10 117.9(5) . . ? C14 C15 C19 118.8(5) . . ? C10 C15 C19 123.3(4) . . ? C11 C16 C17 111.7(5) . . ? C11 C16 C18 113.3(5) . . ? C17 C16 C18 107.3(4) . . ? C11 C16 H16 108.1 . . ? C17 C16 H16 108.1 . . ? C18 C16 H16 108.1 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C15 114.6(5) . . ? C20 C19 C21 107.5(4) . . ? C15 C19 C21 112.6(5) . . ? C20 C19 H19 107.3 . . ? C15 C19 H19 107.3 . . ? C21 C19 H19 107.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si3 C28 H28A 109.5 . . ? Si3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si3 C29 H29A 109.5 . . ? Si3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si3 C30 H30A 109.5 . . ? Si3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si4 C31 H31A 109.5 . . ? Si4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si4 C32 H32A 109.5 . . ? Si4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si4 C33 H33A 109.5 . . ? Si4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C9A C8A C8 118.0(4) . . ? C9A C8A H8A 121.0 . . ? C8 C8A H8A 121.0 . . ? C9 C9A C8A 119.6(4) . . ? C9 C9A H9A 120.2 . . ? C8A C9A H9A 120.2 . . ? 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 Y N1 C2 163.7(3) . . . . ? N4 Y N1 C2 30.0(3) . . . . ? N2 Y N1 C2 -59.9(3) . . . . ? N3 Y N1 C2 -102.1(3) . . . . ? N5 Y N1 C10 -16.6(4) . . . . ? N4 Y N1 C10 -150.4(4) . . . . ? N2 Y N1 C10 119.8(4) . . . . ? N3 Y N1 C10 77.6(4) . . . . ? N5 Y N2 C4 157.3(3) . . . . ? N4 Y N2 C4 -58.1(3) . . . . ? N1 Y N2 C4 62.1(3) . . . . ? N3 Y N2 C4 -151.9(3) . . . . ? N5 Y N2 C6 -43.2(4) . . . . ? N4 Y N2 C6 101.4(3) . . . . ? N1 Y N2 C6 -138.3(4) . . . . ? N3 Y N2 C6 7.6(3) . . . . ? N5 Y N3 C7 143.5(3) . . . . ? N4 Y N3 C7 -100.1(3) . . . . ? N2 Y N3 C7 -5.0(3) . . . . ? N1 Y N3 C7 40.1(3) . . . . ? N5 Y N3 C8 -36.2(3) . . . . ? N4 Y N3 C8 80.3(3) . . . . ? N2 Y N3 C8 175.4(3) . . . . ? N1 Y N3 C8 -139.5(3) . . . . ? C25 Si2 N4 Si1 69.8(3) . . . . ? C27 Si2 N4 Si1 -171.6(2) . . . . ? C26 Si2 N4 Si1 -55.1(3) . . . . ? C25 Si2 N4 Y -106.7(2) . . . . ? C27 Si2 N4 Y 12.0(3) . . . . ? C26 Si2 N4 Y 128.5(2) . . . . ? C24 Si1 N4 Si2 107.8(3) . . . . ? C22 Si1 N4 Si2 -130.4(2) . . . . ? C23 Si1 N4 Si2 -11.9(3) . . . . ? C24 Si1 N4 Y -76.0(3) . . . . ? C22 Si1 N4 Y 45.8(3) . . . . ? C23 Si1 N4 Y 164.2(2) . . . . ? N5 Y N4 Si2 -100.23(18) . . . . ? N2 Y N4 Si2 105.69(18) . . . . ? N1 Y N4 Si2 28.0(2) . . . . ? N3 Y N4 Si2 173.02(17) . . . . ? N5 Y N4 Si1 83.7(2) . . . . ? N2 Y N4 Si1 -70.3(2) . . . . ? N1 Y N4 Si1 -148.06(17) . . . . ? N3 Y N4 Si1 -3.0(2) . . . . ? C31 Si4 N5 Si3 83.3(3) . . . . ? C32 Si4 N5 Si3 -158.5(2) . . . . ? C33 Si4 N5 Si3 -36.5(3) . . . . ? C31 Si4 N5 Y -91.7(3) . . . . ? C32 Si4 N5 Y 26.4(3) . . . . ? C33 Si4 N5 Y 148.4(2) . . . . ? C30 Si3 N5 Si4 72.3(3) . . . . ? C29 Si3 N5 Si4 -170.0(2) . . . . ? C28 Si3 N5 Si4 -50.0(3) . . . . ? C30 Si3 N5 Y -112.3(2) . . . . ? C29 Si3 N5 Y 5.4(2) . . . . ? C28 Si3 N5 Y 125.4(2) . . . . ? N4 Y N5 Si4 15.7(2) . . . . ? N2 Y N5 Si4 155.56(17) . . . . ? N1 Y N5 Si4 -120.34(19) . . . . ? N3 Y N5 Si4 109.91(19) . . . . ? N4 Y N5 Si3 -159.35(15) . . . . ? N2 Y N5 Si3 -19.5(3) . . . . ? N1 Y N5 Si3 64.57(18) . . . . ? N3 Y N5 Si3 -65.18(17) . . . . ? C10 N1 C2 C3 -149.1(4) . . . . ? Y N1 C2 C3 30.7(5) . . . . ? C10 N1 C2 C1 29.0(6) . . . . ? Y N1 C2 C1 -151.2(3) . . . . ? N1 C2 C3 C4 27.7(7) . . . . ? C1 C2 C3 C4 -150.5(4) . . . . ? C6 N2 C4 C3 165.6(4) . . . . ? Y N2 C4 C3 -34.0(5) . . . . ? C6 N2 C4 C5 -12.1(7) . . . . ? Y N2 C4 C5 148.3(4) . . . . ? C2 C3 C4 N2 -27.0(7) . . . . ? C2 C3 C4 C5 150.8(4) . . . . ? C4 N2 C6 C7 148.6(4) . . . . ? Y N2 C6 C7 -9.2(5) . . . . ? C8 N3 C7 C9 -0.2(6) . . . . ? Y N3 C7 C9 -179.8(3) . . . . ? C8 N3 C7 C6 -178.1(4) . . . . ? Y N3 C7 C6 2.2(5) . . . . ? N2 C6 C7 N3 3.9(6) . . . . ? N2 C6 C7 C9 -174.1(4) . . . . ? C7 N3 C8 C8A 2.3(6) . . . . ? Y N3 C8 C8A -178.1(3) . . . . ? N3 C7 C9 C9A -2.3(8) . . . . ? C6 C7 C9 C9A 175.6(5) . . . . ? C2 N1 C10 C15 -105.1(4) . . . . ? Y N1 C10 C15 75.2(5) . . . . ? C2 N1 C10 C11 75.1(5) . . . . ? Y N1 C10 C11 -104.5(4) . . . . ? C15 C10 C11 C12 -1.9(7) . . . . ? N1 C10 C11 C12 177.8(4) . . . . ? C15 C10 C11 C16 175.7(4) . . . . ? N1 C10 C11 C16 -4.5(6) . . . . ? C10 C11 C12 C13 1.3(8) . . . . ? C16 C11 C12 C13 -176.4(5) . . . . ? C11 C12 C13 C14 -0.4(9) . . . . ? C12 C13 C14 C15 0.0(9) . . . . ? C13 C14 C15 C10 -0.6(7) . . . . ? C13 C14 C15 C19 177.1(5) . . . . ? C11 C10 C15 C14 1.5(6) . . . . ? N1 C10 C15 C14 -178.2(4) . . . . ? C11 C10 C15 C19 -176.1(4) . . . . ? N1 C10 C15 C19 4.2(6) . . . . ? C12 C11 C16 C17 71.1(6) . . . . ? C10 C11 C16 C17 -106.5(5) . . . . ? C12 C11 C16 C18 -50.3(7) . . . . ? C10 C11 C16 C18 132.1(5) . . . . ? C14 C15 C19 C20 53.2(6) . . . . ? C10 C15 C19 C20 -129.2(5) . . . . ? C14 C15 C19 C21 -70.1(6) . . . . ? C10 C15 C19 C21 107.5(5) . . . . ? N3 C8 C8A C9A -1.8(7) . . . . ? C7 C9 C9A C8A 2.7(8) . . . . ? C8 C8A C9A C9 -0.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.774 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.071 #===END data_cd29481 _database_code_depnum_ccdc_archive 'CCDC 759491' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H66 La N5 Si4' _chemical_formula_weight 808.20 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6794(18) _cell_length_b 11.7544(19) _cell_length_c 18.051(3) _cell_angle_alpha 85.938(3) _cell_angle_beta 86.272(3) _cell_angle_gamma 81.210(3) _cell_volume 2230.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4394 _cell_measurement_theta_min 4.577 _cell_measurement_theta_max 51.912 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.397 _exptl_crystal_size_mid 0.311 _exptl_crystal_size_min 0.169 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.092 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4599 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11582 _diffrn_reflns_av_R_equivalents 0.0836 _diffrn_reflns_av_sigmaI/netI 0.0878 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8145 _reflns_number_gt 6860 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0960P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8145 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1587 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.003 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 La La 0.20315(3) 0.25043(3) 0.271785(17) 0.03371(14) Uani 1 1 d . . . Si1 Si 0.2669(3) 0.4469(2) 0.41381(13) 0.0722(7) Uani 1 1 d . . . Si2 Si 0.3847(2) 0.2040(2) 0.42920(13) 0.0666(6) Uani 1 1 d . . . Si3 Si 0.43936(19) 0.35651(17) 0.14477(11) 0.0520(5) Uani 1 1 d . . . Si4 Si 0.2131(2) 0.30869(19) 0.07228(10) 0.0559(5) Uani 1 1 d . . . N1 N 0.1524(5) 0.0490(4) 0.2543(3) 0.0390(11) Uani 1 1 d . . . N2 N -0.0127(5) 0.2445(4) 0.3214(3) 0.0451(12) Uani 1 1 d . . . N3 N 0.0280(6) 0.4348(5) 0.2431(3) 0.0521(14) Uani 1 1 d . . . N4 N 0.2920(5) 0.3102(5) 0.3814(3) 0.0513(14) Uani 1 1 d . . . N5 N 0.2947(5) 0.3096(4) 0.1512(3) 0.0440(12) Uani 1 1 d . . . C1 C 0.1641(10) -0.1257(6) 0.3401(4) 0.078(3) Uani 1 1 d . . . H1A H 0.1996 -0.1631 0.2963 0.117 Uiso 1 1 calc R . . H1B H 0.0871 -0.1546 0.3568 0.117 Uiso 1 1 calc R . . H1C H 0.2237 -0.1412 0.3784 0.117 Uiso 1 1 calc R . . C2 C 0.1355(7) 0.0039(6) 0.3221(4) 0.0491(16) Uani 1 1 d . . . C3 C 0.0882(7) 0.0711(6) 0.3810(4) 0.0525(17) Uani 1 1 d . . . H3 H 0.1187 0.0442 0.4271 0.063 Uiso 1 1 calc R . . C4 C 0.0022(7) 0.1722(6) 0.3812(4) 0.0534(17) Uani 1 1 d . . . C5 C -0.0737(10) 0.1982(8) 0.4534(5) 0.090(3) Uani 1 1 d . . . H5A H -0.1603 0.1884 0.4485 0.135 Uiso 1 1 calc R . . H5B H -0.0704 0.2763 0.4646 0.135 Uiso 1 1 calc R . . H5C H -0.0386 0.1465 0.4929 0.135 Uiso 1 1 calc R . . C6 C -0.1223(7) 0.3338(7) 0.3171(5) 0.064(2) Uani 1 1 d . . . H6A H -0.1489 0.3585 0.3665 0.077 Uiso 1 1 calc R . . H6B H -0.1920 0.3030 0.2976 0.077 Uiso 1 1 calc R . . C7 C -0.0922(7) 0.4340(6) 0.2683(4) 0.0547(17) Uani 1 1 d . . . C8 C 0.0553(9) 0.5277(7) 0.2004(5) 0.080(3) Uani 1 1 d . . . H8 H 0.1390 0.5305 0.1837 0.096 Uiso 1 1 calc R . . C9 C -0.1876(9) 0.5233(8) 0.2498(6) 0.087(3) Uani 1 1 d . . . H9 H -0.2712 0.5196 0.2665 0.104 Uiso 1 1 calc R . . C10 C 0.1591(6) -0.0232(5) 0.1924(3) 0.0428(14) Uani 1 1 d . . . C11 C 0.0460(7) -0.0330(6) 0.1610(4) 0.0501(16) Uani 1 1 d . . . C12 C 0.0512(9) -0.1005(8) 0.0997(4) 0.073(2) Uani 1 1 d . . . H12 H -0.0231 -0.1074 0.0774 0.087 Uiso 1 1 calc R . . C13 C 0.1655(9) -0.1568(8) 0.0724(5) 0.077(2) Uani 1 1 d . . . H13 H 0.1674 -0.2025 0.0322 0.092 Uiso 1 1 calc R . . C14 C 0.2757(8) -0.1464(7) 0.1032(4) 0.069(2) Uani 1 1 d . . . H14 H 0.3520 -0.1840 0.0831 0.082 Uiso 1 1 calc R . . C15 C 0.2766(7) -0.0805(6) 0.1645(4) 0.0527(17) Uani 1 1 d . . . C16 C -0.0816(7) 0.0243(7) 0.1923(5) 0.066(2) Uani 1 1 d . . . H16 H -0.0654 0.0904 0.2185 0.079 Uiso 1 1 calc R . . C17 C -0.1416(10) -0.0546(11) 0.2494(6) 0.111(4) Uani 1 1 d . . . H17A H -0.0820 -0.0835 0.2864 0.167 Uiso 1 1 calc R . . H17B H -0.1647 -0.1180 0.2254 0.167 Uiso 1 1 calc R . . H17C H -0.2160 -0.0123 0.2728 0.167 Uiso 1 1 calc R . . C18 C -0.1740(8) 0.0713(10) 0.1333(6) 0.097(3) Uani 1 1 d . . . H18A H -0.2109 0.0092 0.1160 0.145 Uiso 1 1 calc R . . H18B H -0.1297 0.1075 0.0924 0.145 Uiso 1 1 calc R . . H18C H -0.2397 0.1269 0.1541 0.145 Uiso 1 1 calc R . . C19 C 0.4012(7) -0.0724(7) 0.1966(5) 0.065(2) Uani 1 1 d . . . H19 H 0.3818 -0.0332 0.2430 0.078 Uiso 1 1 calc R . . C20 C 0.4777(10) -0.1886(9) 0.2159(7) 0.109(4) Uani 1 1 d . . . H20A H 0.5007 -0.2288 0.1714 0.164 Uiso 1 1 calc R . . H20B H 0.4278 -0.2329 0.2495 0.164 Uiso 1 1 calc R . . H20C H 0.5531 -0.1780 0.2391 0.164 Uiso 1 1 calc R . . C21 C 0.4816(9) 0.0000(9) 0.1461(7) 0.103(4) Uani 1 1 d . . . H21A H 0.4337 0.0747 0.1353 0.154 Uiso 1 1 calc R . . H21B H 0.5053 -0.0373 0.1006 0.154 Uiso 1 1 calc R . . H21C H 0.5566 0.0085 0.1705 0.154 Uiso 1 1 calc R . . C22 C 0.1070(15) 0.5270(12) 0.3951(9) 0.192(10) Uani 1 1 d . . . H22A H 0.0435 0.4806 0.4130 0.289 Uiso 1 1 calc R . . H22B H 0.1011 0.5441 0.3426 0.289 Uiso 1 1 calc R . . H22C H 0.0939 0.5976 0.4201 0.289 Uiso 1 1 calc R . . C23 C 0.2809(11) 0.4517(10) 0.5160(5) 0.104(4) Uani 1 1 d . . . H23A H 0.3655 0.4196 0.5287 0.157 Uiso 1 1 calc R . . H23B H 0.2215 0.4077 0.5423 0.157 Uiso 1 1 calc R . . H23C H 0.2629 0.5302 0.5296 0.157 Uiso 1 1 calc R . . C24 C 0.3869(19) 0.5378(12) 0.3701(8) 0.131(8) Uani 1 1 d . . . H24A H 0.3675 0.5601 0.3194 0.217 Uiso 1 1 calc R . . H24B H 0.4704 0.4938 0.3712 0.217 Uiso 1 1 calc R . . H24C H 0.3838 0.6055 0.3973 0.217 Uiso 1 1 calc R . . C25 C 0.3080(11) 0.1501(10) 0.5177(5) 0.102(3) Uani 1 1 d . . . H25A H 0.2243 0.1358 0.5088 0.153 Uiso 1 1 calc R . . H25B H 0.3025 0.2069 0.5539 0.153 Uiso 1 1 calc R . . H25C H 0.3576 0.0799 0.5359 0.153 Uiso 1 1 calc R . . C26 C 0.5436(9) 0.2382(10) 0.4513(6) 0.103(4) Uani 1 1 d . . . H26A H 0.5322 0.3078 0.4773 0.155 Uiso 1 1 calc R . . H26B H 0.5938 0.2484 0.4059 0.155 Uiso 1 1 calc R . . H26C H 0.5860 0.1759 0.4819 0.155 Uiso 1 1 calc R . . C27 C 0.4255(9) 0.0769(8) 0.3707(5) 0.083(3) Uani 1 1 d . . . H27A H 0.4770 0.0972 0.3276 0.124 Uiso 1 1 calc R . . H27B H 0.3490 0.0545 0.3552 0.124 Uiso 1 1 calc R . . H27C H 0.4715 0.0139 0.3991 0.124 Uiso 1 1 calc R . . C28 C 0.4268(9) 0.5181(8) 0.1427(6) 0.086(3) Uani 1 1 d . . . H28A H 0.3722 0.5465 0.1839 0.129 Uiso 1 1 calc R . . H28B H 0.3922 0.5513 0.0970 0.129 Uiso 1 1 calc R . . H28C H 0.5095 0.5390 0.1463 0.129 Uiso 1 1 calc R . . C29 C 0.5323(7) 0.2999(8) 0.2276(5) 0.075(2) Uani 1 1 d . . . H29A H 0.5376 0.2175 0.2331 0.112 Uiso 1 1 calc R . . H29B H 0.4908 0.3332 0.2714 0.112 Uiso 1 1 calc R . . H29C H 0.6163 0.3202 0.2206 0.112 Uiso 1 1 calc R . . C30 C 0.5447(8) 0.3092(8) 0.0618(5) 0.077(2) Uani 1 1 d . . . H30A H 0.5044 0.3396 0.0171 0.116 Uiso 1 1 calc R . . H30B H 0.5594 0.2265 0.0626 0.116 Uiso 1 1 calc R . . H30C H 0.6242 0.3374 0.0632 0.116 Uiso 1 1 calc R . . C31 C 0.2017(10) 0.4480(9) 0.0125(5) 0.091(3) Uani 1 1 d . . . H31A H 0.2843 0.4578 -0.0089 0.136 Uiso 1 1 calc R . . H31B H 0.1696 0.5114 0.0425 0.136 Uiso 1 1 calc R . . H31C H 0.1453 0.4455 -0.0265 0.136 Uiso 1 1 calc R . . C32 C 0.2799(10) 0.1924(10) 0.0077(5) 0.097(3) Uani 1 1 d . . . H32A H 0.2788 0.1181 0.0333 0.146 Uiso 1 1 calc R . . H32B H 0.3656 0.2012 -0.0082 0.146 Uiso 1 1 calc R . . H32C H 0.2293 0.1987 -0.0349 0.146 Uiso 1 1 calc R . . C33 C 0.0471(8) 0.2810(9) 0.0971(5) 0.079(3) Uani 1 1 d . . . H33A H 0.0025 0.3427 0.1249 0.119 Uiso 1 1 calc R . . H33B H 0.0492 0.2095 0.1266 0.119 Uiso 1 1 calc R . . H33C H 0.0044 0.2764 0.0524 0.119 Uiso 1 1 calc R . . C8A C -0.0369(12) 0.6189(9) 0.1806(7) 0.112(4) Uani 1 1 d . . . H8A H -0.0155 0.6806 0.1497 0.134 Uiso 1 1 calc R . . C9A C -0.1575(12) 0.6174(9) 0.2065(7) 0.114(4) Uani 1 1 d . . . H9A H -0.2200 0.6793 0.1953 0.136 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 La 0.0388(2) 0.02700(19) 0.0349(2) -0.00478(12) -0.00285(13) -0.00198(12) Si1 0.0949(18) 0.0576(14) 0.0669(14) -0.0276(11) -0.0236(12) -0.0011(12) Si2 0.0702(14) 0.0675(15) 0.0622(13) -0.0121(10) -0.0295(11) 0.0044(11) Si3 0.0533(11) 0.0505(11) 0.0532(11) -0.0060(8) 0.0078(9) -0.0137(9) Si4 0.0695(13) 0.0578(12) 0.0409(10) -0.0008(8) -0.0060(9) -0.0111(10) N1 0.044(3) 0.032(3) 0.041(3) -0.010(2) 0.002(2) -0.003(2) N2 0.049(3) 0.030(3) 0.054(3) -0.005(2) 0.004(2) 0.001(2) N3 0.059(4) 0.034(3) 0.058(3) -0.002(2) -0.001(3) 0.007(2) N4 0.056(3) 0.052(4) 0.047(3) -0.015(2) -0.013(3) -0.002(3) N5 0.055(3) 0.035(3) 0.042(3) -0.006(2) 0.000(2) -0.005(2) C1 0.128(8) 0.034(4) 0.067(5) 0.002(3) 0.015(5) -0.001(4) C2 0.063(4) 0.035(3) 0.047(4) -0.001(3) 0.005(3) -0.005(3) C3 0.075(5) 0.039(4) 0.041(4) -0.002(3) 0.003(3) -0.003(3) C4 0.056(4) 0.056(4) 0.049(4) -0.011(3) 0.011(3) -0.016(3) C5 0.114(8) 0.075(6) 0.068(6) -0.010(5) 0.034(5) 0.011(5) C6 0.042(4) 0.064(5) 0.083(5) -0.003(4) 0.008(4) 0.002(3) C7 0.058(4) 0.044(4) 0.058(4) -0.012(3) -0.007(3) 0.011(3) C8 0.091(6) 0.043(5) 0.096(7) 0.008(4) 0.011(5) 0.008(4) C9 0.071(6) 0.063(6) 0.116(8) -0.006(5) -0.004(5) 0.023(5) C10 0.054(4) 0.034(3) 0.041(3) -0.006(2) 0.004(3) -0.010(3) C11 0.057(4) 0.043(4) 0.052(4) -0.009(3) -0.001(3) -0.013(3) C12 0.081(6) 0.082(6) 0.064(5) -0.024(4) -0.009(4) -0.030(5) C13 0.090(6) 0.079(6) 0.067(5) -0.037(4) 0.008(5) -0.021(5) C14 0.079(6) 0.062(5) 0.067(5) -0.030(4) 0.018(4) -0.013(4) C15 0.058(4) 0.043(4) 0.057(4) -0.014(3) 0.011(3) -0.009(3) C16 0.053(4) 0.068(5) 0.081(5) -0.023(4) -0.004(4) -0.013(4) C17 0.090(7) 0.125(10) 0.114(9) -0.005(7) 0.034(6) -0.018(7) C18 0.053(5) 0.106(8) 0.133(9) -0.005(7) -0.012(5) -0.014(5) C19 0.050(4) 0.062(5) 0.084(6) -0.031(4) 0.004(4) -0.003(4) C20 0.094(8) 0.075(7) 0.154(11) -0.006(7) -0.023(7) 0.010(6) C21 0.060(6) 0.080(7) 0.169(11) -0.017(7) 0.005(6) -0.014(5) C22 0.205(16) 0.123(11) 0.249(18) -0.135(12) -0.141(14) 0.090(11) C23 0.135(9) 0.093(8) 0.088(7) -0.051(6) -0.016(6) 0.000(7) C24 0.202(2) 0.084(11) 0.112(12) -0.043(9) 0.033(13) -0.082(14) C25 0.130(9) 0.100(8) 0.075(6) 0.013(5) -0.036(6) -0.012(7) C26 0.087(7) 0.105(8) 0.122(9) -0.035(7) -0.047(6) 0.006(6) C27 0.080(6) 0.070(6) 0.095(7) -0.016(5) -0.031(5) 0.017(5) C28 0.097(7) 0.055(5) 0.111(7) -0.008(5) 0.001(6) -0.030(5) C29 0.055(5) 0.092(7) 0.079(6) -0.015(5) -0.009(4) -0.008(4) C30 0.072(5) 0.089(7) 0.070(5) -0.012(5) 0.024(4) -0.018(5) C31 0.114(8) 0.090(7) 0.070(6) 0.033(5) -0.026(5) -0.030(6) C32 0.125(9) 0.110(9) 0.062(5) -0.037(5) -0.011(5) -0.015(7) C33 0.081(6) 0.106(8) 0.061(5) 0.001(5) -0.022(4) -0.041(5) C8A 0.128(10) 0.054(6) 0.132(9) 0.030(6) 0.007(8) 0.031(6) C9A 0.117(10) 0.052(6) 0.153(11) 0.012(6) -0.008(8) 0.037(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La N2 2.428(5) . ? La N5 2.428(5) . ? La N4 2.441(5) . ? La N1 2.553(5) . ? La N3 2.682(5) . ? La C4 3.024(7) . ? La C3 3.119(7) . ? La Si2 3.508(2) . ? Si1 N4 1.725(6) . ? Si1 C22 1.858(12) . ? Si1 C23 1.866(9) . ? Si1 C24 1.891(14) . ? Si2 N4 1.692(6) . ? Si2 C25 1.862(11) . ? Si2 C27 1.871(9) . ? Si2 C26 1.876(10) . ? Si3 N5 1.712(6) . ? Si3 C29 1.874(8) . ? Si3 C30 1.878(8) . ? Si3 C28 1.882(9) . ? Si4 N5 1.720(5) . ? Si4 C33 1.871(9) . ? Si4 C32 1.886(9) . ? Si4 C31 1.888(9) . ? N1 C2 1.311(8) . ? N1 C10 1.442(7) . ? N2 C4 1.329(9) . ? N2 C6 1.450(8) . ? N3 C7 1.335(9) . ? N3 C8 1.349(10) . ? C1 C2 1.524(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.392(9) . ? C3 C4 1.386(10) . ? C3 H3 0.9300 . ? C4 C5 1.514(10) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.482(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C9 1.385(10) . ? C8 C8A 1.384(12) . ? C8 H8 0.9300 . ? C9 C9A 1.375(15) . ? C9 H9 0.9300 . ? C10 C11 1.391(9) . ? C10 C15 1.411(9) . ? C11 C12 1.399(10) . ? C11 C16 1.518(10) . ? C12 C13 1.376(12) . ? C12 H12 0.9300 . ? C13 C14 1.359(12) . ? C13 H13 0.9300 . ? C14 C15 1.396(10) . ? C14 H14 0.9300 . ? C15 C19 1.504(10) . ? C16 C17 1.514(13) . ? C16 C18 1.517(12) . ? C16 H16 0.9800 . ? 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 C20 1.511(12) . ? C19 C21 1.517(13) . ? C19 H19 0.9800 . ? 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 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C8A C9A 1.344(15) . ? C8A H8A 0.9300 . ? C9A H9A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 La N5 133.67(18) . . ? N2 La N4 99.04(19) . . ? N5 La N4 117.14(19) . . ? N2 La N1 72.73(16) . . ? N5 La N1 103.97(16) . . ? N4 La N1 125.76(18) . . ? N2 La N3 61.94(18) . . ? N5 La N3 82.92(17) . . ? N4 La N3 100.19(18) . . ? N1 La N3 119.40(17) . . ? N2 La C4 25.30(19) . . ? N5 La C4 156.54(19) . . ? N4 La C4 84.73(19) . . ? N1 La C4 65.25(17) . . ? N3 La C4 84.91(19) . . ? N2 La C3 48.77(18) . . ? N5 La C3 151.97(17) . . ? N4 La C3 85.60(19) . . ? N1 La C3 48.03(16) . . ? N3 La C3 110.39(18) . . ? C4 La C3 26.02(19) . . ? N2 La Si2 104.13(13) . . ? N5 La Si2 121.21(14) . . ? N4 La Si2 25.94(14) . . ? N1 La Si2 102.35(12) . . ? N3 La Si2 125.31(13) . . ? C4 La Si2 82.13(15) . . ? C3 La Si2 72.05(14) . . ? N4 Si1 C22 113.1(4) . . ? N4 Si1 C23 114.8(4) . . ? C22 Si1 C23 105.1(6) . . ? N4 Si1 C24 111.5(5) . . ? C22 Si1 C24 107.1(9) . . ? C23 Si1 C24 104.6(6) . . ? N4 Si2 C25 114.3(4) . . ? N4 Si2 C27 109.1(3) . . ? C25 Si2 C27 106.2(5) . . ? N4 Si2 C26 115.5(4) . . ? C25 Si2 C26 107.3(5) . . ? C27 Si2 C26 103.5(5) . . ? N4 Si2 La 39.12(18) . . ? C25 Si2 La 117.7(3) . . ? C27 Si2 La 71.0(3) . . ? C26 Si2 La 134.5(4) . . ? N5 Si3 C29 110.6(3) . . ? N5 Si3 C30 115.0(3) . . ? C29 Si3 C30 105.3(4) . . ? N5 Si3 C28 113.0(4) . . ? C29 Si3 C28 105.8(4) . . ? C30 Si3 C28 106.5(4) . . ? N5 Si4 C33 110.6(3) . . ? N5 Si4 C32 115.1(4) . . ? C33 Si4 C32 104.2(5) . . ? N5 Si4 C31 113.9(4) . . ? C33 Si4 C31 107.1(4) . . ? C32 Si4 C31 105.2(5) . . ? C2 N1 C10 119.3(5) . . ? C2 N1 La 104.6(4) . . ? C10 N1 La 135.2(4) . . ? C4 N2 C6 120.7(6) . . ? C4 N2 La 103.3(4) . . ? C6 N2 La 128.9(4) . . ? C7 N3 C8 117.9(6) . . ? C7 N3 La 119.8(4) . . ? C8 N3 La 122.2(5) . . ? Si2 N4 Si1 118.8(3) . . ? Si2 N4 La 114.9(3) . . ? Si1 N4 La 126.3(3) . . ? Si3 N5 Si4 119.6(3) . . ? Si3 N5 La 120.0(3) . . ? Si4 N5 La 120.4(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 122.1(6) . . ? N1 C2 C1 121.5(6) . . ? C3 C2 C1 116.4(6) . . ? C4 C3 C2 129.6(7) . . ? C4 C3 La 73.2(4) . . ? C2 C3 La 78.4(4) . . ? C4 C3 H3 115.2 . . ? C2 C3 H3 115.2 . . ? La C3 H3 125.1 . . ? N2 C4 C3 122.0(6) . . ? N2 C4 C5 120.9(7) . . ? C3 C4 C5 117.0(7) . . ? N2 C4 La 51.4(3) . . ? C3 C4 La 80.8(4) . . ? C5 C4 La 144.3(6) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 110.8(6) . . ? N2 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N3 C7 C9 121.7(8) . . ? N3 C7 C6 118.2(6) . . ? C9 C7 C6 120.0(8) . . ? N3 C8 C8A 122.4(9) . . ? N3 C8 H8 118.8 . . ? C8A C8 H8 118.8 . . ? C9A C9 C7 119.4(9) . . ? C9A C9 H9 120.3 . . ? C7 C9 H9 120.3 . . ? C11 C10 C15 121.5(6) . . ? C11 C10 N1 117.6(6) . . ? C15 C10 N1 120.9(6) . . ? C10 C11 C12 118.3(7) . . ? C10 C11 C16 122.1(6) . . ? C12 C11 C16 119.6(7) . . ? C13 C12 C11 120.4(8) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 120.9(7) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 121.3(8) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C14 C15 C10 117.5(7) . . ? C14 C15 C19 119.1(7) . . ? C10 C15 C19 123.4(6) . . ? C17 C16 C18 110.5(8) . . ? C17 C16 C11 111.8(8) . . ? C18 C16 C11 113.7(7) . . ? C17 C16 H16 106.8 . . ? C18 C16 H16 106.8 . . ? C11 C16 H16 106.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 C20 113.3(7) . . ? C15 C19 C21 112.2(8) . . ? C20 C19 C21 109.7(7) . . ? C15 C19 H19 107.1 . . ? C20 C19 H19 107.1 . . ? C21 C19 H19 107.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si3 C28 H28A 109.5 . . ? Si3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si3 C29 H29A 109.5 . . ? Si3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si3 C30 H30A 109.5 . . ? Si3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si4 C31 H31A 109.5 . . ? Si4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si4 C32 H32A 109.5 . . ? Si4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si4 C33 H33A 109.5 . . ? Si4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C9A C8A C8 119.2(10) . . ? C9A C8A H8A 120.4 . . ? C8 C8A H8A 120.4 . . ? C8A C9A C9 119.3(9) . . ? C8A C9A H9A 120.3 . . ? C9 C9A H9A 120.3 . . ? 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 N2 La Si2 N4 -81.5(4) . . . . ? N5 La Si2 N4 88.5(4) . . . . ? N1 La Si2 N4 -156.6(3) . . . . ? N3 La Si2 N4 -16.1(4) . . . . ? C4 La Si2 N4 -94.1(4) . . . . ? C3 La Si2 N4 -118.8(4) . . . . ? N2 La Si2 C25 13.6(4) . . . . ? N5 La Si2 C25 -176.3(4) . . . . ? N4 La Si2 C25 95.2(5) . . . . ? N1 La Si2 C25 -61.4(4) . . . . ? N3 La Si2 C25 79.0(4) . . . . ? C4 La Si2 C25 1.0(4) . . . . ? C3 La Si2 C25 -23.6(4) . . . . ? N2 La Si2 C27 112.4(4) . . . . ? N5 La Si2 C27 -77.5(4) . . . . ? N4 La Si2 C27 -166.0(5) . . . . ? N1 La Si2 C27 37.4(4) . . . . ? N3 La Si2 C27 177.8(4) . . . . ? C4 La Si2 C27 99.8(4) . . . . ? C3 La Si2 C27 75.2(4) . . . . ? N2 La Si2 C26 -157.1(5) . . . . ? N5 La Si2 C26 13.0(5) . . . . ? N4 La Si2 C26 -75.5(6) . . . . ? N1 La Si2 C26 127.9(5) . . . . ? N3 La Si2 C26 -91.7(5) . . . . ? C4 La Si2 C26 -169.7(5) . . . . ? C3 La Si2 C26 165.7(5) . . . . ? N2 La N1 C2 -64.5(4) . . . . ? N5 La N1 C2 163.6(4) . . . . ? N4 La N1 C2 24.3(5) . . . . ? N3 La N1 C2 -106.7(4) . . . . ? C4 La N1 C2 -38.6(4) . . . . ? C3 La N1 C2 -15.0(4) . . . . ? Si2 La N1 C2 36.6(4) . . . . ? N2 La N1 C10 127.1(6) . . . . ? N5 La N1 C10 -4.8(6) . . . . ? N4 La N1 C10 -144.1(5) . . . . ? N3 La N1 C10 84.9(6) . . . . ? C4 La N1 C10 153.0(6) . . . . ? C3 La N1 C10 176.7(6) . . . . ? Si2 La N1 C10 -131.8(5) . . . . ? N5 La N2 C4 161.4(4) . . . . ? N4 La N2 C4 -56.4(4) . . . . ? N1 La N2 C4 68.4(4) . . . . ? N3 La N2 C4 -153.1(5) . . . . ? C3 La N2 C4 19.6(4) . . . . ? Si2 La N2 C4 -30.4(4) . . . . ? N5 La N2 C6 -48.8(7) . . . . ? N4 La N2 C6 93.4(6) . . . . ? N1 La N2 C6 -141.8(6) . . . . ? N3 La N2 C6 -3.3(6) . . . . ? C4 La N2 C6 149.8(8) . . . . ? C3 La N2 C6 169.4(7) . . . . ? Si2 La N2 C6 119.4(6) . . . . ? N2 La N3 C7 -1.2(5) . . . . ? N5 La N3 C7 147.6(5) . . . . ? N4 La N3 C7 -96.0(5) . . . . ? N1 La N3 C7 45.5(6) . . . . ? C4 La N3 C7 -12.3(5) . . . . ? C3 La N3 C7 -7.0(5) . . . . ? Si2 La N3 C7 -89.0(5) . . . . ? N2 La N3 C8 -177.7(7) . . . . ? N5 La N3 C8 -29.0(6) . . . . ? N4 La N3 C8 87.4(6) . . . . ? N1 La N3 C8 -131.1(6) . . . . ? C4 La N3 C8 171.1(7) . . . . ? C3 La N3 C8 176.5(6) . . . . ? Si2 La N3 C8 94.5(6) . . . . ? C25 Si2 N4 Si1 74.3(6) . . . . ? C27 Si2 N4 Si1 -167.0(5) . . . . ? C26 Si2 N4 Si1 -50.9(6) . . . . ? La Si2 N4 Si1 179.0(6) . . . . ? C25 Si2 N4 La -104.7(5) . . . . ? C27 Si2 N4 La 14.0(5) . . . . ? C26 Si2 N4 La 130.0(4) . . . . ? C22 Si1 N4 Si2 -146.9(8) . . . . ? C23 Si1 N4 Si2 -26.3(6) . . . . ? C24 Si1 N4 Si2 92.4(7) . . . . ? C22 Si1 N4 La 32.0(8) . . . . ? C23 Si1 N4 La 152.6(5) . . . . ? C24 Si1 N4 La -88.7(7) . . . . ? N2 La N4 Si2 103.8(3) . . . . ? N5 La N4 Si2 -106.1(3) . . . . ? N1 La N4 Si2 28.6(4) . . . . ? N3 La N4 Si2 166.7(3) . . . . ? C4 La N4 Si2 82.8(3) . . . . ? C3 La N4 Si2 56.7(3) . . . . ? N2 La N4 Si1 -75.2(4) . . . . ? N5 La N4 Si1 74.9(4) . . . . ? N1 La N4 Si1 -150.4(3) . . . . ? N3 La N4 Si1 -12.3(4) . . . . ? C4 La N4 Si1 -96.1(4) . . . . ? C3 La N4 Si1 -122.2(4) . . . . ? Si2 La N4 Si1 -179.0(7) . . . . ? C29 Si3 N5 Si4 -159.2(4) . . . . ? C30 Si3 N5 Si4 -40.2(5) . . . . ? C28 Si3 N5 Si4 82.4(5) . . . . ? C29 Si3 N5 La 22.6(4) . . . . ? C30 Si3 N5 La 141.6(4) . . . . ? C28 Si3 N5 La -95.8(4) . . . . ? C33 Si4 N5 Si3 -169.2(4) . . . . ? C32 Si4 N5 Si3 73.0(5) . . . . ? C31 Si4 N5 Si3 -48.6(5) . . . . ? C33 Si4 N5 La 8.9(5) . . . . ? C32 Si4 N5 La -108.8(5) . . . . ? C31 Si4 N5 La 129.6(4) . . . . ? N2 La N5 Si3 153.9(2) . . . . ? N4 La N5 Si3 16.7(4) . . . . ? N1 La N5 Si3 -126.8(3) . . . . ? N3 La N5 Si3 114.6(3) . . . . ? C4 La N5 Si3 173.8(4) . . . . ? C3 La N5 Si3 -124.5(4) . . . . ? Si2 La N5 Si3 -12.7(3) . . . . ? N2 La N5 Si4 -24.3(4) . . . . ? N4 La N5 Si4 -161.4(3) . . . . ? N1 La N5 Si4 55.0(3) . . . . ? N3 La N5 Si4 -63.6(3) . . . . ? C4 La N5 Si4 -4.3(6) . . . . ? C3 La N5 Si4 57.3(5) . . . . ? Si2 La N5 Si4 169.1(2) . . . . ? C10 N1 C2 C3 -158.9(7) . . . . ? La N1 C2 C3 30.5(8) . . . . ? C10 N1 C2 C1 19.7(10) . . . . ? La N1 C2 C1 -150.9(7) . . . . ? N1 C2 C3 C4 32.2(12) . . . . ? C1 C2 C3 C4 -146.4(8) . . . . ? N1 C2 C3 La -24.2(6) . . . . ? C1 C2 C3 La 157.1(7) . . . . ? N2 La C3 C4 -19.1(4) . . . . ? N5 La C3 C4 -127.0(5) . . . . ? N4 La C3 C4 87.0(4) . . . . ? N1 La C3 C4 -124.0(5) . . . . ? N3 La C3 C4 -12.3(5) . . . . ? Si2 La C3 C4 109.6(4) . . . . ? N2 La C3 C2 118.8(5) . . . . ? N5 La C3 C2 10.9(7) . . . . ? N4 La C3 C2 -135.1(4) . . . . ? N1 La C3 C2 13.9(4) . . . . ? N3 La C3 C2 125.6(4) . . . . ? C4 La C3 C2 137.9(7) . . . . ? Si2 La C3 C2 -112.5(4) . . . . ? C6 N2 C4 C3 165.0(7) . . . . ? La N2 C4 C3 -42.1(8) . . . . ? C6 N2 C4 C5 -15.8(11) . . . . ? La N2 C4 C5 137.2(7) . . . . ? C6 N2 C4 La -152.9(7) . . . . ? C2 C3 C4 N2 -26.5(12) . . . . ? La C3 C4 N2 32.0(6) . . . . ? C2 C3 C4 C5 154.2(8) . . . . ? La C3 C4 C5 -147.2(7) . . . . ? C2 C3 C4 La -58.5(8) . . . . ? N5 La C4 N2 -35.3(7) . . . . ? N4 La C4 N2 124.3(4) . . . . ? N1 La C4 N2 -102.1(4) . . . . ? N3 La C4 N2 23.6(4) . . . . ? C3 La C4 N2 -144.9(7) . . . . ? Si2 La C4 N2 150.3(4) . . . . ? N2 La C4 C3 144.9(7) . . . . ? N5 La C4 C3 109.5(6) . . . . ? N4 La C4 C3 -90.8(4) . . . . ? N1 La C4 C3 42.8(4) . . . . ? N3 La C4 C3 168.5(4) . . . . ? Si2 La C4 C3 -64.8(4) . . . . ? N2 La C4 C5 -90.8(11) . . . . ? N5 La C4 C5 -126.2(9) . . . . ? N4 La C4 C5 33.5(10) . . . . ? N1 La C4 C5 167.1(10) . . . . ? N3 La C4 C5 -67.2(10) . . . . ? C3 La C4 C5 124.3(12) . . . . ? Si2 La C4 C5 59.5(10) . . . . ? C4 N2 C6 C7 152.1(7) . . . . ? La N2 C6 C7 6.8(9) . . . . ? C8 N3 C7 C9 2.0(11) . . . . ? La N3 C7 C9 -174.7(6) . . . . ? C8 N3 C7 C6 -178.3(7) . . . . ? La N3 C7 C6 5.0(9) . . . . ? N2 C6 C7 N3 -7.1(10) . . . . ? N2 C6 C7 C9 172.6(7) . . . . ? C7 N3 C8 C8A -1.9(14) . . . . ? La N3 C8 C8A 174.7(8) . . . . ? N3 C7 C9 C9A -2.4(15) . . . . ? C6 C7 C9 C9A 177.9(10) . . . . ? C2 N1 C10 C11 89.1(8) . . . . ? La N1 C10 C11 -103.8(6) . . . . ? C2 N1 C10 C15 -91.6(8) . . . . ? La N1 C10 C15 75.5(8) . . . . ? C15 C10 C11 C12 -0.8(10) . . . . ? N1 C10 C11 C12 178.5(7) . . . . ? C15 C10 C11 C16 177.6(7) . . . . ? N1 C10 C11 C16 -3.2(10) . . . . ? C10 C11 C12 C13 1.0(13) . . . . ? C16 C11 C12 C13 -177.5(8) . . . . ? C11 C12 C13 C14 -1.2(15) . . . . ? C12 C13 C14 C15 1.3(14) . . . . ? C13 C14 C15 C10 -1.1(12) . . . . ? C13 C14 C15 C19 179.7(8) . . . . ? C11 C10 C15 C14 0.8(10) . . . . ? N1 C10 C15 C14 -178.4(6) . . . . ? C11 C10 C15 C19 180.0(7) . . . . ? N1 C10 C15 C19 0.8(10) . . . . ? C10 C11 C16 C17 -91.2(9) . . . . ? C12 C11 C16 C17 87.2(10) . . . . ? C10 C11 C16 C18 142.8(8) . . . . ? C12 C11 C16 C18 -38.9(11) . . . . ? C14 C15 C19 C20 -53.6(11) . . . . ? C10 C15 C19 C20 127.3(9) . . . . ? C14 C15 C19 C21 71.4(10) . . . . ? C10 C15 C19 C21 -107.7(8) . . . . ? N3 C8 C8A C9A 2.2(18) . . . . ? C8 C8A C9A C9 -2(2) . . . . ? C7 C9 C9A C8A 2.6(18) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 3.449 _refine_diff_density_min -1.292 _refine_diff_density_rms 0.149