# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl #TrackingRef 'complexes 16 CIF.doc' #TrackingRef 'complexes 16 CIF.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 N Sc Si' _chemical_formula_sum 'C21 H36 N Sc Si' _chemical_formula_weight 375.56 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.037(3) _cell_length_b 16.030(4) _cell_length_c 14.767(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.640(7) _cell_angle_gamma 90.00 _cell_volume 2237.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6498 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.385 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 0.927 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16621 _diffrn_reflns_av_R_equivalents 0.1098 _diffrn_reflns_av_sigmaI/netI 0.0974 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3977 _reflns_number_gt 2376 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1122P)^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 3977 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1675 _refine_ls_R_factor_gt 0.1056 _refine_ls_wR_factor_ref 0.2775 _refine_ls_wR_factor_gt 0.2371 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _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 Sc1 Sc 1.01766(13) 0.75610(7) 0.77451(7) 0.0584(5) Uani 1 1 d . . . Si1 Si 0.68697(18) 0.72871(11) 0.84091(13) 0.0618(5) Uani 1 1 d . . . N1 N 0.6363(6) 0.6261(4) 0.8358(4) 0.0882(18) Uani 1 1 d . . . C1 C 0.8831(6) 0.7466(3) 0.8853(3) 0.0471(13) Uani 1 1 d . . . C2 C 0.9481(6) 0.8278(3) 0.8990(4) 0.0501(14) Uani 1 1 d . . . C3 C 1.0951(6) 0.8187(4) 0.9377(4) 0.0557(15) Uani 1 1 d . . . C4 C 1.1256(6) 0.7322(4) 0.9488(4) 0.0535(15) Uani 1 1 d . . . C5 C 0.9972(6) 0.6889(3) 0.9185(3) 0.0464(13) Uani 1 1 d . . . C6 C 0.8722(7) 0.9108(4) 0.8864(5) 0.0764(19) Uani 1 1 d . . . H6A H 0.8410 0.9207 0.9402 0.115 Uiso 1 1 calc R . . H6B H 0.7919 0.9099 0.8282 0.115 Uiso 1 1 calc R . . H6C H 0.9356 0.9546 0.8826 0.115 Uiso 1 1 calc R . . C7 C 1.2042(8) 0.8875(5) 0.9711(5) 0.092(2) Uani 1 1 d . . . H7A H 1.1797 0.9326 0.9258 0.138 Uiso 1 1 calc R . . H7B H 1.2956 0.8662 0.9758 0.138 Uiso 1 1 calc R . . H7C H 1.2065 0.9073 1.0330 0.138 Uiso 1 1 calc R . . C8 C 1.2701(7) 0.6940(5) 0.9932(5) 0.087(2) Uani 1 1 d . . . H8A H 1.3388 0.7276 0.9779 0.130 Uiso 1 1 calc R . . H8B H 1.2702 0.6387 0.9682 0.130 Uiso 1 1 calc R . . H8C H 1.2933 0.6914 1.0617 0.130 Uiso 1 1 calc R . . C9 C 0.9853(7) 0.5951(3) 0.9286(4) 0.0672(17) Uani 1 1 d . . . H9A H 1.0651 0.5682 0.9191 0.101 Uiso 1 1 calc R . . H9B H 0.8997 0.5755 0.8813 0.101 Uiso 1 1 calc R . . H9C H 0.9836 0.5824 0.9917 0.101 Uiso 1 1 calc R . . C10 C 0.6095(8) 0.7817(5) 0.9235(6) 0.095(2) Uani 1 1 d . . . H10A H 0.5086 0.7750 0.8998 0.142 Uiso 1 1 calc R . . H10B H 0.6325 0.8400 0.9269 0.142 Uiso 1 1 calc R . . H10C H 0.6474 0.7574 0.9864 0.142 Uiso 1 1 calc R . . C11 C 0.6054(8) 0.7712(5) 0.7170(5) 0.098(3) Uani 1 1 d . . . H11A H 0.6423 0.7420 0.6739 0.146 Uiso 1 1 calc R . . H11B H 0.6273 0.8295 0.7168 0.146 Uiso 1 1 calc R . . H11C H 0.5047 0.7640 0.6966 0.146 Uiso 1 1 calc R . . C12 C 0.6147(9) 0.5791(5) 0.9138(7) 0.117(3) Uani 1 1 d . . . H12A H 0.5691 0.6133 0.9490 0.141 Uiso 1 1 calc R . . H12B H 0.7041 0.5590 0.9580 0.141 Uiso 1 1 calc R . . C13 C 0.5223(13) 0.5083(6) 0.8658(9) 0.166(5) Uani 1 1 d . . . H13A H 0.5644 0.4561 0.8947 0.199 Uiso 1 1 calc R . . H13B H 0.4307 0.5137 0.8739 0.199 Uiso 1 1 calc R . . C14 C 0.5048(10) 0.5084(6) 0.7624(9) 0.145(4) Uani 1 1 d . . . H14A H 0.5291 0.4544 0.7427 0.174 Uiso 1 1 calc R . . H14B H 0.4081 0.5217 0.7238 0.174 Uiso 1 1 calc R . . C15 C 0.6027(10) 0.5731(5) 0.7524(7) 0.126(3) Uani 1 1 d . . . H15A H 0.6881 0.5477 0.7481 0.151 Uiso 1 1 calc R . . H15B H 0.5588 0.6054 0.6945 0.151 Uiso 1 1 calc R . . C16 C 1.1670(12) 0.8519(6) 0.7259(7) 0.122(3) Uani 1 1 d . . . H16A H 1.2500 0.8721 0.7766 0.147 Uiso 1 1 calc R . . H16B H 1.1859 0.8376 0.6675 0.147 Uiso 1 1 calc R . . C17 C 1.0461(14) 0.8936(5) 0.7140(7) 0.107(3) Uani 1 1 d . . . H17 H 1.0515 0.9409 0.7572 0.129 Uiso 1 1 calc R . . C18 C 0.9121(11) 0.8648(6) 0.6620(6) 0.112(3) Uani 1 1 d . . . H18A H 0.8955 0.8520 0.5949 0.134 Uiso 1 1 calc R . . H18B H 0.8339 0.8942 0.6722 0.134 Uiso 1 1 calc R . . C19 C 0.9048(11) 0.6392(5) 0.6718(5) 0.101(3) Uani 1 1 d . . . H19A H 0.8850 0.5904 0.7041 0.121 Uiso 1 1 calc R . . H19B H 0.8286 0.6530 0.6131 0.121 Uiso 1 1 calc R . . C20 C 1.0364(15) 0.6453(5) 0.6687(7) 0.117(3) Uani 1 1 d . . . H20 H 1.0448 0.6624 0.6072 0.140 Uiso 1 1 calc R . . C21 C 1.1562(10) 0.6423(5) 0.7437(6) 0.109(3) Uani 1 1 d . . . H21A H 1.2417 0.6579 0.7311 0.131 Uiso 1 1 calc R . . H21B H 1.1685 0.5939 0.7852 0.131 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.0825(9) 0.0478(7) 0.0524(7) 0.0026(5) 0.0327(6) 0.0020(6) Si1 0.0569(10) 0.0569(11) 0.0685(11) -0.0015(8) 0.0170(8) 0.0009(9) N1 0.090(4) 0.066(4) 0.098(4) -0.007(3) 0.017(3) -0.025(3) C1 0.063(3) 0.040(3) 0.042(3) 0.005(2) 0.021(3) 0.005(3) C2 0.066(4) 0.036(3) 0.053(3) 0.000(2) 0.026(3) 0.007(3) C3 0.064(4) 0.051(4) 0.058(3) -0.011(3) 0.028(3) -0.010(3) C4 0.046(3) 0.070(4) 0.049(3) 0.003(3) 0.022(3) 0.003(3) C5 0.051(3) 0.050(3) 0.046(3) 0.006(2) 0.026(2) 0.007(3) C6 0.103(5) 0.044(3) 0.093(5) -0.002(3) 0.048(4) 0.004(4) C7 0.095(5) 0.092(6) 0.100(5) -0.020(4) 0.049(4) -0.038(5) C8 0.063(4) 0.112(6) 0.090(5) 0.005(4) 0.033(4) 0.013(4) C9 0.093(5) 0.041(3) 0.078(4) 0.007(3) 0.043(4) 0.008(3) C10 0.072(5) 0.109(6) 0.114(6) -0.016(5) 0.046(4) 0.001(5) C11 0.086(5) 0.094(6) 0.088(5) -0.002(4) -0.004(4) 0.015(4) C12 0.102(6) 0.091(6) 0.157(8) 0.015(6) 0.040(6) -0.028(5) C13 0.157(10) 0.098(8) 0.191(11) 0.034(8) -0.008(9) -0.057(7) C14 0.099(7) 0.092(8) 0.232(13) -0.043(9) 0.039(9) -0.035(6) C15 0.129(8) 0.089(6) 0.151(8) -0.044(6) 0.035(6) -0.038(6) C16 0.144(9) 0.127(8) 0.120(7) 0.024(6) 0.076(7) -0.021(7) C17 0.172(10) 0.069(5) 0.096(6) 0.029(5) 0.066(7) -0.025(7) C18 0.148(9) 0.111(7) 0.084(5) 0.044(5) 0.048(6) 0.009(6) C19 0.155(9) 0.072(5) 0.082(5) -0.018(4) 0.046(6) -0.005(6) C20 0.188(11) 0.085(6) 0.115(7) -0.033(5) 0.099(8) -0.001(7) C21 0.122(7) 0.105(7) 0.099(6) -0.017(5) 0.034(6) 0.035(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 Sc1 C18 2.395(7) . ? Sc1 C20 2.414(7) . ? Sc1 C16 2.418(8) . ? Sc1 C21 2.428(8) . ? Sc1 C17 2.431(7) . ? Sc1 C19 2.438(7) . ? Sc1 C1 2.451(5) . ? Sc1 C5 2.453(5) . ? Sc1 C2 2.461(5) . ? Sc1 C4 2.464(5) . ? Sc1 C3 2.482(5) . ? Si1 N1 1.716(6) . ? Si1 C10 1.857(7) . ? Si1 C11 1.864(7) . ? Si1 C1 1.876(6) . ? N1 C15 1.440(9) . ? N1 C12 1.453(9) . ? C1 C5 1.425(7) . ? C1 C2 1.440(7) . ? C2 C3 1.399(8) . ? C2 C6 1.513(8) . ? C3 C4 1.418(8) . ? C3 C7 1.515(8) . ? C4 C5 1.398(7) . ? C4 C8 1.506(8) . ? C5 C9 1.518(8) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.486(12) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.477(13) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.470(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.344(12) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.384(11) . ? C17 H17 0.9800 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.341(12) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.334(12) . ? C20 H20 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 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 C18 Sc1 C20 101.5(4) . . ? C18 Sc1 C16 60.4(3) . . ? C20 Sc1 C16 94.8(4) . . ? C18 Sc1 C21 124.4(3) . . ? C20 Sc1 C21 32.0(3) . . ? C16 Sc1 C21 88.3(4) . . ? C18 Sc1 C17 33.3(3) . . ? C20 Sc1 C17 112.6(3) . . ? C16 Sc1 C17 32.2(3) . . ? C21 Sc1 C17 117.8(4) . . ? C18 Sc1 C19 97.1(4) . . ? C20 Sc1 C19 32.1(3) . . ? C16 Sc1 C19 120.6(3) . . ? C21 Sc1 C19 58.8(3) . . ? C17 Sc1 C19 123.8(3) . . ? C18 Sc1 C1 107.1(3) . . ? C20 Sc1 C1 124.5(3) . . ? C16 Sc1 C1 140.7(3) . . ? C21 Sc1 C1 123.9(3) . . ? C17 Sc1 C1 117.4(3) . . ? C19 Sc1 C1 97.0(3) . . ? C18 Sc1 C5 140.8(3) . . ? C20 Sc1 C5 106.6(3) . . ? C16 Sc1 C5 141.0(3) . . ? C21 Sc1 C5 93.0(3) . . ? C17 Sc1 C5 140.5(3) . . ? C19 Sc1 C5 92.6(2) . . ? C1 Sc1 C5 33.79(16) . . ? C18 Sc1 C2 90.4(3) . . ? C20 Sc1 C2 158.6(3) . . ? C16 Sc1 C2 106.6(3) . . ? C21 Sc1 C2 144.6(3) . . ? C17 Sc1 C2 87.1(3) . . ? C19 Sc1 C2 129.4(3) . . ? C1 Sc1 C2 34.10(17) . . ? C5 Sc1 C2 55.26(18) . . ? C18 Sc1 C4 140.7(3) . . ? C20 Sc1 C4 117.3(3) . . ? C16 Sc1 C4 108.1(3) . . ? C21 Sc1 C4 90.0(3) . . ? C17 Sc1 C4 117.4(3) . . ? C19 Sc1 C4 118.7(2) . . ? C1 Sc1 C4 55.99(18) . . ? C5 Sc1 C4 33.05(17) . . ? C2 Sc1 C4 55.07(18) . . ? C18 Sc1 C3 107.5(3) . . ? C20 Sc1 C3 149.2(3) . . ? C16 Sc1 C3 90.5(3) . . ? C21 Sc1 C3 118.3(3) . . ? C17 Sc1 C3 87.3(3) . . ? C19 Sc1 C3 147.5(2) . . ? C1 Sc1 C3 55.94(19) . . ? C5 Sc1 C3 54.98(19) . . ? C2 Sc1 C3 32.88(18) . . ? C4 Sc1 C3 33.31(18) . . ? N1 Si1 C10 106.5(4) . . ? N1 Si1 C11 106.3(3) . . ? C10 Si1 C11 109.5(4) . . ? N1 Si1 C1 115.0(3) . . ? C10 Si1 C1 108.8(3) . . ? C11 Si1 C1 110.5(3) . . ? C15 N1 C12 108.5(7) . . ? C15 N1 Si1 125.7(6) . . ? C12 N1 Si1 125.7(5) . . ? C5 C1 C2 105.4(5) . . ? C5 C1 Si1 130.4(4) . . ? C2 C1 Si1 124.1(4) . . ? C5 C1 Sc1 73.2(3) . . ? C2 C1 Sc1 73.3(3) . . ? Si1 C1 Sc1 121.7(2) . . ? C3 C2 C1 109.2(5) . . ? C3 C2 C6 124.1(5) . . ? C1 C2 C6 126.3(5) . . ? C3 C2 Sc1 74.4(3) . . ? C1 C2 Sc1 72.6(3) . . ? C6 C2 Sc1 125.2(4) . . ? C2 C3 C4 107.9(5) . . ? C2 C3 C7 127.2(6) . . ? C4 C3 C7 124.7(6) . . ? C2 C3 Sc1 72.7(3) . . ? C4 C3 Sc1 72.6(3) . . ? C7 C3 Sc1 124.5(4) . . ? C5 C4 C3 108.0(5) . . ? C5 C4 C8 125.9(6) . . ? C3 C4 C8 125.9(6) . . ? C5 C4 Sc1 73.1(3) . . ? C3 C4 Sc1 74.1(3) . . ? C8 C4 Sc1 122.6(4) . . ? C4 C5 C1 109.6(5) . . ? C4 C5 C9 123.7(5) . . ? C1 C5 C9 126.6(5) . . ? C4 C5 Sc1 73.9(3) . . ? C1 C5 Sc1 73.0(3) . . ? C9 C5 Sc1 123.5(4) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 104.6(8) . . ? N1 C12 H12A 110.8 . . ? C13 C12 H12A 110.8 . . ? N1 C12 H12B 110.8 . . ? C13 C12 H12B 110.8 . . ? H12A C12 H12B 108.9 . . ? C14 C13 C12 109.3(9) . . ? C14 C13 H13A 109.8 . . ? C12 C13 H13A 109.8 . . ? C14 C13 H13B 109.8 . . ? C12 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? C15 C14 C13 104.7(8) . . ? C15 C14 H14A 110.8 . . ? C13 C14 H14A 110.8 . . ? C15 C14 H14B 110.8 . . ? C13 C14 H14B 110.8 . . ? H14A C14 H14B 108.9 . . ? N1 C15 C14 107.6(8) . . ? N1 C15 H15A 110.2 . . ? C14 C15 H15A 110.2 . . ? N1 C15 H15B 110.2 . . ? C14 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? C17 C16 Sc1 74.5(5) . . ? C17 C16 H16A 116.1 . . ? Sc1 C16 H16A 116.1 . . ? C17 C16 H16B 116.1 . . ? Sc1 C16 H16B 116.1 . . ? H16A C16 H16B 113.0 . . ? C16 C17 C18 125.0(10) . . ? C16 C17 Sc1 73.4(5) . . ? C18 C17 Sc1 71.9(4) . . ? C16 C17 H17 116.7 . . ? C18 C17 H17 116.7 . . ? Sc1 C17 H17 116.7 . . ? C17 C18 Sc1 74.8(5) . . ? C17 C18 H18A 116.0 . . ? Sc1 C18 H18A 116.0 . . ? C17 C18 H18B 116.0 . . ? Sc1 C18 H18B 116.0 . . ? H18A C18 H18B 113.0 . . ? C20 C19 Sc1 73.0(5) . . ? C20 C19 H19A 116.3 . . ? Sc1 C19 H19A 116.3 . . ? C20 C19 H19B 116.3 . . ? Sc1 C19 H19B 116.3 . . ? H19A C19 H19B 113.2 . . ? C21 C20 C19 126.4(9) . . ? C21 C20 Sc1 74.6(5) . . ? C19 C20 Sc1 74.9(5) . . ? C21 C20 H20 116.4 . . ? C19 C20 H20 116.4 . . ? Sc1 C20 H20 116.4 . . ? C20 C21 Sc1 73.4(5) . . ? C20 C21 H21A 116.2 . . ? Sc1 C21 H21A 116.2 . . ? C20 C21 H21B 116.2 . . ? Sc1 C21 H21B 116.2 . . ? H21A C21 H21B 113.2 . . ? 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 C10 Si1 N1 C15 144.8(7) . . . . ? C11 Si1 N1 C15 28.0(8) . . . . ? C1 Si1 N1 C15 -94.6(7) . . . . ? C10 Si1 N1 C12 -32.6(7) . . . . ? C11 Si1 N1 C12 -149.4(7) . . . . ? C1 Si1 N1 C12 88.0(7) . . . . ? N1 Si1 C1 C5 -2.3(6) . . . . ? C10 Si1 C1 C5 117.0(5) . . . . ? C11 Si1 C1 C5 -122.7(5) . . . . ? N1 Si1 C1 C2 -177.2(4) . . . . ? C10 Si1 C1 C2 -57.9(5) . . . . ? C11 Si1 C1 C2 62.4(5) . . . . ? N1 Si1 C1 Sc1 92.2(3) . . . . ? C10 Si1 C1 Sc1 -148.4(4) . . . . ? C11 Si1 C1 Sc1 -28.1(4) . . . . ? C18 Sc1 C1 C5 -176.3(4) . . . . ? C20 Sc1 C1 C5 66.1(5) . . . . ? C16 Sc1 C1 C5 -112.5(5) . . . . ? C21 Sc1 C1 C5 27.2(5) . . . . ? C17 Sc1 C1 C5 -141.9(4) . . . . ? C19 Sc1 C1 C5 84.1(4) . . . . ? C2 Sc1 C1 C5 -112.3(5) . . . . ? C4 Sc1 C1 C5 -35.9(3) . . . . ? C3 Sc1 C1 C5 -76.4(3) . . . . ? C18 Sc1 C1 C2 -63.9(4) . . . . ? C20 Sc1 C1 C2 178.4(5) . . . . ? C16 Sc1 C1 C2 -0.1(6) . . . . ? C21 Sc1 C1 C2 139.5(4) . . . . ? C17 Sc1 C1 C2 -29.6(5) . . . . ? C19 Sc1 C1 C2 -163.6(4) . . . . ? C5 Sc1 C1 C2 112.3(5) . . . . ? C4 Sc1 C1 C2 76.4(3) . . . . ? C3 Sc1 C1 C2 35.9(3) . . . . ? C18 Sc1 C1 Si1 56.2(4) . . . . ? C20 Sc1 C1 Si1 -61.5(5) . . . . ? C16 Sc1 C1 Si1 120.0(5) . . . . ? C21 Sc1 C1 Si1 -100.3(4) . . . . ? C17 Sc1 C1 Si1 90.5(4) . . . . ? C19 Sc1 C1 Si1 -43.5(3) . . . . ? C5 Sc1 C1 Si1 -127.6(5) . . . . ? C2 Sc1 C1 Si1 120.1(4) . . . . ? C4 Sc1 C1 Si1 -163.5(4) . . . . ? C3 Sc1 C1 Si1 156.1(4) . . . . ? C5 C1 C2 C3 0.7(6) . . . . ? Si1 C1 C2 C3 176.7(4) . . . . ? Sc1 C1 C2 C3 -66.0(4) . . . . ? C5 C1 C2 C6 -172.1(5) . . . . ? Si1 C1 C2 C6 3.9(7) . . . . ? Sc1 C1 C2 C6 121.2(5) . . . . ? C5 C1 C2 Sc1 66.7(3) . . . . ? Si1 C1 C2 Sc1 -117.3(4) . . . . ? C18 Sc1 C2 C3 -122.7(4) . . . . ? C20 Sc1 C2 C3 112.9(10) . . . . ? C16 Sc1 C2 C3 -63.7(4) . . . . ? C21 Sc1 C2 C3 47.8(6) . . . . ? C17 Sc1 C2 C3 -89.6(4) . . . . ? C19 Sc1 C2 C3 137.7(4) . . . . ? C1 Sc1 C2 C3 116.4(4) . . . . ? C5 Sc1 C2 C3 77.7(3) . . . . ? C4 Sc1 C2 C3 37.1(3) . . . . ? C18 Sc1 C2 C1 120.8(4) . . . . ? C20 Sc1 C2 C1 -3.6(10) . . . . ? C16 Sc1 C2 C1 179.9(4) . . . . ? C21 Sc1 C2 C1 -68.6(6) . . . . ? C17 Sc1 C2 C1 154.0(4) . . . . ? C19 Sc1 C2 C1 21.2(4) . . . . ? C5 Sc1 C2 C1 -38.8(3) . . . . ? C4 Sc1 C2 C1 -79.3(3) . . . . ? C3 Sc1 C2 C1 -116.4(4) . . . . ? C18 Sc1 C2 C6 -1.8(6) . . . . ? C20 Sc1 C2 C6 -126.2(10) . . . . ? C16 Sc1 C2 C6 57.3(6) . . . . ? C21 Sc1 C2 C6 168.8(6) . . . . ? C17 Sc1 C2 C6 31.4(6) . . . . ? C19 Sc1 C2 C6 -101.3(5) . . . . ? C1 Sc1 C2 C6 -122.6(6) . . . . ? C5 Sc1 C2 C6 -161.4(6) . . . . ? C4 Sc1 C2 C6 158.1(6) . . . . ? C3 Sc1 C2 C6 121.0(6) . . . . ? C1 C2 C3 C4 0.2(6) . . . . ? C6 C2 C3 C4 173.2(5) . . . . ? Sc1 C2 C3 C4 -64.6(4) . . . . ? C1 C2 C3 C7 -174.7(5) . . . . ? C6 C2 C3 C7 -1.6(9) . . . . ? Sc1 C2 C3 C7 120.6(6) . . . . ? C1 C2 C3 Sc1 64.8(4) . . . . ? C6 C2 C3 Sc1 -122.2(5) . . . . ? C18 Sc1 C3 C2 61.9(4) . . . . ? C20 Sc1 C3 C2 -138.9(6) . . . . ? C16 Sc1 C3 C2 120.8(4) . . . . ? C21 Sc1 C3 C2 -150.9(4) . . . . ? C17 Sc1 C3 C2 88.8(4) . . . . ? C19 Sc1 C3 C2 -75.4(6) . . . . ? C1 Sc1 C3 C2 -37.3(3) . . . . ? C5 Sc1 C3 C2 -78.6(3) . . . . ? C4 Sc1 C3 C2 -115.7(5) . . . . ? C18 Sc1 C3 C4 177.6(4) . . . . ? C20 Sc1 C3 C4 -23.2(7) . . . . ? C16 Sc1 C3 C4 -123.5(4) . . . . ? C21 Sc1 C3 C4 -35.2(4) . . . . ? C17 Sc1 C3 C4 -155.5(4) . . . . ? C19 Sc1 C3 C4 40.3(6) . . . . ? C1 Sc1 C3 C4 78.4(3) . . . . ? C5 Sc1 C3 C4 37.1(3) . . . . ? C2 Sc1 C3 C4 115.7(5) . . . . ? C18 Sc1 C3 C7 -61.8(6) . . . . ? C20 Sc1 C3 C7 97.4(8) . . . . ? C16 Sc1 C3 C7 -2.9(6) . . . . ? C21 Sc1 C3 C7 85.4(6) . . . . ? C17 Sc1 C3 C7 -34.9(6) . . . . ? C19 Sc1 C3 C7 160.9(6) . . . . ? C1 Sc1 C3 C7 -161.0(6) . . . . ? C5 Sc1 C3 C7 157.7(6) . . . . ? C2 Sc1 C3 C7 -123.7(7) . . . . ? C4 Sc1 C3 C7 120.6(7) . . . . ? C2 C3 C4 C5 -1.0(6) . . . . ? C7 C3 C4 C5 173.9(5) . . . . ? Sc1 C3 C4 C5 -65.7(4) . . . . ? C2 C3 C4 C8 -176.3(5) . . . . ? C7 C3 C4 C8 -1.4(9) . . . . ? Sc1 C3 C4 C8 119.0(5) . . . . ? C2 C3 C4 Sc1 64.7(4) . . . . ? C7 C3 C4 Sc1 -120.4(5) . . . . ? C18 Sc1 C4 C5 111.3(5) . . . . ? C20 Sc1 C4 C5 -78.1(5) . . . . ? C16 Sc1 C4 C5 176.3(4) . . . . ? C21 Sc1 C4 C5 -95.5(4) . . . . ? C17 Sc1 C4 C5 142.8(4) . . . . ? C19 Sc1 C4 C5 -41.7(4) . . . . ? C1 Sc1 C4 C5 36.7(3) . . . . ? C2 Sc1 C4 C5 78.4(3) . . . . ? C3 Sc1 C4 C5 115.0(5) . . . . ? C18 Sc1 C4 C3 -3.7(6) . . . . ? C20 Sc1 C4 C3 166.9(5) . . . . ? C16 Sc1 C4 C3 61.3(4) . . . . ? C21 Sc1 C4 C3 149.5(4) . . . . ? C17 Sc1 C4 C3 27.8(5) . . . . ? C19 Sc1 C4 C3 -156.7(4) . . . . ? C1 Sc1 C4 C3 -78.3(3) . . . . ? C5 Sc1 C4 C3 -115.0(5) . . . . ? C2 Sc1 C4 C3 -36.6(3) . . . . ? C18 Sc1 C4 C8 -126.5(6) . . . . ? C20 Sc1 C4 C8 44.1(7) . . . . ? C16 Sc1 C4 C8 -61.5(6) . . . . ? C21 Sc1 C4 C8 26.7(6) . . . . ? C17 Sc1 C4 C8 -95.0(6) . . . . ? C19 Sc1 C4 C8 80.5(6) . . . . ? C1 Sc1 C4 C8 158.9(6) . . . . ? C5 Sc1 C4 C8 122.2(7) . . . . ? C2 Sc1 C4 C8 -159.4(6) . . . . ? C3 Sc1 C4 C8 -122.8(7) . . . . ? C3 C4 C5 C1 1.5(6) . . . . ? C8 C4 C5 C1 176.8(5) . . . . ? Sc1 C4 C5 C1 -64.8(3) . . . . ? C3 C4 C5 C9 -173.8(5) . . . . ? C8 C4 C5 C9 1.6(8) . . . . ? Sc1 C4 C5 C9 119.9(5) . . . . ? C3 C4 C5 Sc1 66.4(4) . . . . ? C8 C4 C5 Sc1 -118.3(5) . . . . ? C2 C1 C5 C4 -1.4(5) . . . . ? Si1 C1 C5 C4 -177.0(4) . . . . ? Sc1 C1 C5 C4 65.4(4) . . . . ? C2 C1 C5 C9 173.7(5) . . . . ? Si1 C1 C5 C9 -1.9(8) . . . . ? Sc1 C1 C5 C9 -119.5(5) . . . . ? C2 C1 C5 Sc1 -66.8(3) . . . . ? Si1 C1 C5 Sc1 117.6(4) . . . . ? C18 Sc1 C5 C4 -111.2(5) . . . . ? C20 Sc1 C5 C4 114.9(5) . . . . ? C16 Sc1 C5 C4 -5.6(6) . . . . ? C21 Sc1 C5 C4 85.4(4) . . . . ? C17 Sc1 C5 C4 -57.5(6) . . . . ? C19 Sc1 C5 C4 144.3(4) . . . . ? C1 Sc1 C5 C4 -116.9(5) . . . . ? C2 Sc1 C5 C4 -77.8(3) . . . . ? C3 Sc1 C5 C4 -37.4(3) . . . . ? C18 Sc1 C5 C1 5.7(6) . . . . ? C20 Sc1 C5 C1 -128.2(5) . . . . ? C16 Sc1 C5 C1 111.3(5) . . . . ? C21 Sc1 C5 C1 -157.6(4) . . . . ? C17 Sc1 C5 C1 59.4(6) . . . . ? C19 Sc1 C5 C1 -98.8(4) . . . . ? C2 Sc1 C5 C1 39.1(3) . . . . ? C4 Sc1 C5 C1 116.9(5) . . . . ? C3 Sc1 C5 C1 79.5(3) . . . . ? C18 Sc1 C5 C9 128.7(6) . . . . ? C20 Sc1 C5 C9 -5.2(6) . . . . ? C16 Sc1 C5 C9 -125.7(6) . . . . ? C21 Sc1 C5 C9 -34.6(5) . . . . ? C17 Sc1 C5 C9 -177.6(6) . . . . ? C19 Sc1 C5 C9 24.2(5) . . . . ? C1 Sc1 C5 C9 123.0(6) . . . . ? C2 Sc1 C5 C9 162.1(5) . . . . ? C4 Sc1 C5 C9 -120.1(6) . . . . ? C3 Sc1 C5 C9 -157.5(5) . . . . ? C15 N1 C12 C13 -18.8(10) . . . . ? Si1 N1 C12 C13 159.0(7) . . . . ? N1 C12 C13 C14 6.8(12) . . . . ? C12 C13 C14 C15 7.2(13) . . . . ? C12 N1 C15 C14 24.1(10) . . . . ? Si1 N1 C15 C14 -153.7(7) . . . . ? C13 C14 C15 N1 -18.8(11) . . . . ? C18 Sc1 C16 C17 25.7(6) . . . . ? C20 Sc1 C16 C17 126.2(7) . . . . ? C21 Sc1 C16 C17 157.5(7) . . . . ? C19 Sc1 C16 C17 105.9(7) . . . . ? C1 Sc1 C16 C17 -55.0(8) . . . . ? C5 Sc1 C16 C17 -109.8(7) . . . . ? C2 Sc1 C16 C17 -55.1(7) . . . . ? C4 Sc1 C16 C17 -113.0(6) . . . . ? C3 Sc1 C16 C17 -84.2(7) . . . . ? Sc1 C16 C17 C18 -52.8(8) . . . . ? C18 Sc1 C17 C16 -136.6(10) . . . . ? C20 Sc1 C17 C16 -60.6(8) . . . . ? C21 Sc1 C17 C16 -25.6(8) . . . . ? C19 Sc1 C17 C16 -95.0(7) . . . . ? C1 Sc1 C17 C16 144.2(6) . . . . ? C5 Sc1 C17 C16 111.5(7) . . . . ? C2 Sc1 C17 C16 128.1(7) . . . . ? C4 Sc1 C17 C16 80.3(7) . . . . ? C3 Sc1 C17 C16 95.2(7) . . . . ? C20 Sc1 C17 C18 76.0(8) . . . . ? C16 Sc1 C17 C18 136.6(10) . . . . ? C21 Sc1 C17 C18 111.0(6) . . . . ? C19 Sc1 C17 C18 41.7(8) . . . . ? C1 Sc1 C17 C18 -79.2(6) . . . . ? C5 Sc1 C17 C18 -111.8(6) . . . . ? C2 Sc1 C17 C18 -95.3(6) . . . . ? C4 Sc1 C17 C18 -143.0(5) . . . . ? C3 Sc1 C17 C18 -128.2(6) . . . . ? C16 C17 C18 Sc1 53.4(8) . . . . ? C20 Sc1 C18 C17 -113.9(7) . . . . ? C16 Sc1 C18 C17 -24.9(6) . . . . ? C21 Sc1 C18 C17 -89.4(7) . . . . ? C19 Sc1 C18 C17 -146.2(6) . . . . ? C1 Sc1 C18 C17 114.2(6) . . . . ? C5 Sc1 C18 C17 110.9(6) . . . . ? C2 Sc1 C18 C17 84.0(6) . . . . ? C4 Sc1 C18 C17 57.5(7) . . . . ? C3 Sc1 C18 C17 55.4(6) . . . . ? C18 Sc1 C19 C20 100.3(7) . . . . ? C16 Sc1 C19 C20 40.7(8) . . . . ? C21 Sc1 C19 C20 -25.8(6) . . . . ? C17 Sc1 C19 C20 78.7(7) . . . . ? C1 Sc1 C19 C20 -151.4(6) . . . . ? C5 Sc1 C19 C20 -117.8(6) . . . . ? C2 Sc1 C19 C20 -163.2(6) . . . . ? C4 Sc1 C19 C20 -96.5(6) . . . . ? C3 Sc1 C19 C20 -120.4(7) . . . . ? Sc1 C19 C20 C21 57.3(9) . . . . ? C18 Sc1 C20 C21 139.6(7) . . . . ? C16 Sc1 C20 C21 78.9(7) . . . . ? C17 Sc1 C20 C21 106.7(7) . . . . ? C19 Sc1 C20 C21 -135.3(10) . . . . ? C1 Sc1 C20 C21 -100.1(7) . . . . ? C5 Sc1 C20 C21 -68.1(7) . . . . ? C2 Sc1 C20 C21 -97.7(11) . . . . ? C4 Sc1 C20 C21 -34.3(7) . . . . ? C3 Sc1 C20 C21 -20.2(10) . . . . ? C18 Sc1 C20 C19 -85.0(7) . . . . ? C16 Sc1 C20 C19 -145.7(6) . . . . ? C21 Sc1 C20 C19 135.3(10) . . . . ? C17 Sc1 C20 C19 -118.0(6) . . . . ? C1 Sc1 C20 C19 35.2(8) . . . . ? C5 Sc1 C20 C19 67.2(7) . . . . ? C2 Sc1 C20 C19 37.6(13) . . . . ? C4 Sc1 C20 C19 101.1(6) . . . . ? C3 Sc1 C20 C19 115.2(8) . . . . ? C19 C20 C21 Sc1 -57.5(9) . . . . ? C18 Sc1 C21 C20 -50.2(8) . . . . ? C16 Sc1 C21 C20 -101.9(7) . . . . ? C17 Sc1 C21 C20 -88.6(7) . . . . ? C19 Sc1 C21 C20 25.9(6) . . . . ? C1 Sc1 C21 C20 102.3(7) . . . . ? C5 Sc1 C21 C20 117.0(6) . . . . ? C2 Sc1 C21 C20 141.2(6) . . . . ? C4 Sc1 C21 C20 150.0(6) . . . . ? C3 Sc1 C21 C20 168.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.454 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.074 _database_code_depnum_ccdc_archive 'CCDC 917594' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_g120420b-mo #TrackingRef 'complexes 16 CIF.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 N Si Y' _chemical_formula_sum 'C21 H36 N Si Y' _chemical_formula_weight 419.51 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.0591(11) _cell_length_b 9.9549(3) _cell_length_c 17.3059(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.102(5) _cell_angle_gamma 90.00 _cell_volume 4319.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3427 _cell_measurement_theta_min 3.1163 _cell_measurement_theta_max 29.3268 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 2.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.307 _exptl_absorpt_correction_T_max 0.437 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10594 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4018 _reflns_number_gt 3204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+4.9722P] 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 4018 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Y1 Y 0.129146(9) 0.74092(3) 0.160680(16) 0.01817(10) Uani 1 1 d . . . Si1 Si 0.11554(3) 0.73589(8) -0.03836(5) 0.02260(19) Uani 1 1 d . . . N1 N 0.13653(8) 0.6011(2) 0.03641(14) 0.0209(5) Uani 1 1 d . . . C1 C 0.09405(10) 0.8634(3) 0.02006(16) 0.0188(6) Uani 1 1 d . . . C2 C 0.12708(10) 0.9655(3) 0.07372(18) 0.0234(6) Uani 1 1 d . . . C3 C 0.10301(11) 1.0080(3) 0.12881(18) 0.0288(7) Uani 1 1 d . . . C4 C 0.05485(11) 0.9347(3) 0.11065(18) 0.0259(7) Uani 1 1 d . . . C5 C 0.04901(10) 0.8473(3) 0.04426(17) 0.0207(6) Uani 1 1 d . . . C6 C 0.17642(12) 1.0293(3) 0.0679(2) 0.0401(8) Uani 1 1 d . . . H6A H 0.1862 1.1091 0.1035 0.060 Uiso 1 1 calc R . . H6B H 0.1690 1.0552 0.0099 0.060 Uiso 1 1 calc R . . H6C H 0.2059 0.9647 0.0863 0.060 Uiso 1 1 calc R . . C7 C 0.12067(14) 1.1232(3) 0.1900(2) 0.0471(10) Uani 1 1 d . . . H7A H 0.1597 1.1290 0.2126 0.071 Uiso 1 1 calc R . . H7B H 0.1082 1.1080 0.2356 0.071 Uiso 1 1 calc R . . H7C H 0.1056 1.2073 0.1615 0.071 Uiso 1 1 calc R . . C8 C 0.01472(13) 0.9582(4) 0.1510(2) 0.0415(9) Uani 1 1 d . . . H8A H 0.0336 0.9802 0.2101 0.062 Uiso 1 1 calc R . . H8B H -0.0066 0.8767 0.1461 0.062 Uiso 1 1 calc R . . H8C H -0.0088 1.0328 0.1229 0.062 Uiso 1 1 calc R . . C9 C 0.00118(11) 0.7565(3) 0.0046(2) 0.0305(7) Uani 1 1 d . . . H9A H 0.0125 0.6734 -0.0142 0.046 Uiso 1 1 calc R . . H9B H -0.0253 0.8023 -0.0432 0.046 Uiso 1 1 calc R . . H9C H -0.0146 0.7350 0.0456 0.046 Uiso 1 1 calc R . . C10 C 0.06168(13) 0.6834(4) -0.1385(2) 0.0433(9) Uani 1 1 d . . . H10A H 0.0764 0.6215 -0.1683 0.065 Uiso 1 1 calc R . . H10B H 0.0472 0.7628 -0.1731 0.065 Uiso 1 1 calc R . . H10C H 0.0331 0.6384 -0.1265 0.065 Uiso 1 1 calc R . . C11 C 0.17305(14) 0.7898(4) -0.0652(2) 0.0464(9) Uani 1 1 d . . . H11A H 0.2037 0.8094 -0.0139 0.070 Uiso 1 1 calc R . . H11B H 0.1633 0.8707 -0.1000 0.070 Uiso 1 1 calc R . . H11C H 0.1824 0.7178 -0.0959 0.070 Uiso 1 1 calc R . . C12 C 0.10258(13) 0.4778(3) 0.0147(2) 0.0350(8) Uani 1 1 d . . . H12A H 0.0651 0.5014 -0.0191 0.042 Uiso 1 1 calc R . . H12B H 0.1037 0.4313 0.0660 0.042 Uiso 1 1 calc R . . C13 C 0.12547(15) 0.3888(4) -0.0346(2) 0.0563(11) Uani 1 1 d . . . H13A H 0.1226 0.2929 -0.0217 0.068 Uiso 1 1 calc R . . H13B H 0.1064 0.4029 -0.0953 0.068 Uiso 1 1 calc R . . C14 C 0.18339(15) 0.4303(4) -0.0078(2) 0.0502(10) Uani 1 1 d . . . H14A H 0.1910 0.4648 -0.0558 0.060 Uiso 1 1 calc R . . H14B H 0.2073 0.3535 0.0170 0.060 Uiso 1 1 calc R . . C15 C 0.19060(11) 0.5400(3) 0.05644(19) 0.0311(7) Uani 1 1 d . . . H15A H 0.2042 0.5018 0.1134 0.037 Uiso 1 1 calc R . . H15B H 0.2162 0.6085 0.0529 0.037 Uiso 1 1 calc R . . C16 C 0.18712(14) 0.8391(4) 0.3077(2) 0.0486(10) Uani 1 1 d . . . H16A H 0.1733 0.9217 0.3245 0.058 Uiso 1 1 calc R . . H16B H 0.2013 0.7730 0.3536 0.058 Uiso 1 1 calc R . . C17 C 0.21690(12) 0.8576(4) 0.2592(2) 0.0424(9) Uani 1 1 d . . . H17 H 0.2225 0.9526 0.2455 0.051 Uiso 1 1 calc R . . C18 C 0.23256(12) 0.7586(3) 0.2173(2) 0.0401(9) Uani 1 1 d . . . H18A H 0.2524 0.6821 0.2516 0.048 Uiso 1 1 calc R . . H18B H 0.2481 0.7902 0.1770 0.048 Uiso 1 1 calc R . . C19 C 0.14387(12) 0.5055(3) 0.2383(2) 0.0348(8) Uani 1 1 d . . . H19A H 0.1553 0.4305 0.2112 0.042 Uiso 1 1 calc R . . H19B H 0.1631 0.5077 0.2995 0.042 Uiso 1 1 calc R . . C20 C 0.08967(13) 0.5298(4) 0.2096(2) 0.0387(8) Uani 1 1 d . . . H20 H 0.0668 0.4690 0.1642 0.046 Uiso 1 1 calc R . . C21 C 0.06496(14) 0.6446(4) 0.2232(2) 0.0485(10) Uani 1 1 d . . . H21A H 0.0730 0.6674 0.2824 0.058 Uiso 1 1 calc R . . H21B H 0.0266 0.6535 0.1883 0.058 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 0.02127(15) 0.01700(15) 0.01536(15) 0.00086(12) 0.00591(10) 0.00010(12) Si1 0.0235(4) 0.0283(5) 0.0172(4) 0.0026(4) 0.0090(3) 0.0049(3) N1 0.0196(12) 0.0207(13) 0.0231(13) -0.0001(10) 0.0086(10) 0.0004(10) C1 0.0188(13) 0.0191(14) 0.0158(15) 0.0048(12) 0.0033(11) 0.0004(11) C2 0.0253(14) 0.0169(14) 0.0238(16) 0.0049(13) 0.0045(12) -0.0002(12) C3 0.0343(17) 0.0152(15) 0.0275(17) -0.0011(13) 0.0010(13) 0.0068(13) C4 0.0310(16) 0.0245(16) 0.0235(16) 0.0050(13) 0.0115(13) 0.0144(14) C5 0.0192(13) 0.0230(15) 0.0199(15) 0.0036(12) 0.0073(11) 0.0032(12) C6 0.0344(18) 0.0297(18) 0.047(2) 0.0052(16) 0.0053(15) -0.0105(15) C7 0.059(2) 0.0280(19) 0.039(2) -0.0090(16) 0.0017(17) 0.0086(17) C8 0.0485(19) 0.048(2) 0.035(2) 0.0049(17) 0.0236(16) 0.0218(17) C9 0.0212(14) 0.0343(18) 0.0336(17) 0.0017(15) 0.0074(12) -0.0017(14) C10 0.053(2) 0.046(2) 0.0241(18) -0.0083(17) 0.0065(15) 0.0185(18) C11 0.052(2) 0.052(2) 0.050(2) 0.0202(19) 0.0360(18) 0.0124(18) C12 0.0422(18) 0.0270(17) 0.0307(18) -0.0032(15) 0.0079(14) -0.0089(15) C13 0.074(3) 0.033(2) 0.043(2) -0.0138(18) 0.0010(19) 0.010(2) C14 0.071(3) 0.045(2) 0.041(2) 0.0022(18) 0.0283(19) 0.023(2) C15 0.0286(16) 0.0365(19) 0.0293(18) 0.0050(15) 0.0122(13) 0.0128(14) C16 0.063(2) 0.035(2) 0.028(2) -0.0065(17) -0.0056(17) 0.0073(19) C17 0.0380(19) 0.0318(19) 0.033(2) -0.0025(16) -0.0146(15) -0.0084(16) C18 0.0246(16) 0.040(2) 0.041(2) 0.0045(17) -0.0048(14) -0.0011(15) C19 0.050(2) 0.0289(18) 0.0301(19) 0.0119(15) 0.0203(15) 0.0049(15) C20 0.047(2) 0.038(2) 0.039(2) 0.0146(17) 0.0254(16) -0.0075(17) C21 0.052(2) 0.061(3) 0.048(2) 0.027(2) 0.0363(19) 0.012(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 Y1 C21 2.554(3) . ? Y1 C1 2.564(3) . ? Y1 C5 2.568(3) . ? Y1 C18 2.600(3) . ? Y1 C17 2.617(3) . ? Y1 C16 2.625(3) . ? Y1 N1 2.631(2) . ? Y1 C20 2.637(3) . ? Y1 C19 2.656(3) . ? Y1 C2 2.684(3) . ? Y1 C4 2.684(3) . ? Y1 C3 2.753(3) . ? Si1 N1 1.801(2) . ? Si1 C1 1.848(3) . ? Si1 C11 1.863(3) . ? Si1 C10 1.870(3) . ? N1 C12 1.494(4) . ? N1 C15 1.500(3) . ? C1 C2 1.438(4) . ? C1 C5 1.439(4) . ? C2 C3 1.407(4) . ? C2 C6 1.516(4) . ? C3 C4 1.422(4) . ? C3 C7 1.512(4) . ? C4 C5 1.402(4) . ? C4 C8 1.514(4) . ? C5 C9 1.515(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.515(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.515(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.517(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.377(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.382(5) . ? C17 H17 1.0000 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.381(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.388(5) . ? C20 H20 1.0000 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Y1 C1 120.85(10) . . ? C21 Y1 C5 88.81(10) . . ? C1 Y1 C5 32.57(8) . . ? C21 Y1 C18 132.30(12) . . ? C1 Y1 C18 106.69(10) . . ? C5 Y1 C18 137.66(10) . . ? C21 Y1 C17 119.05(13) . . ? C1 Y1 C17 109.18(10) . . ? C5 Y1 C17 128.27(10) . . ? C18 Y1 C17 30.73(11) . . ? C21 Y1 C16 89.01(13) . . ? C1 Y1 C16 128.02(11) . . ? C5 Y1 C16 128.85(10) . . ? C18 Y1 C16 56.19(12) . . ? C17 Y1 C16 30.47(11) . . ? C21 Y1 N1 114.87(11) . . ? C1 Y1 N1 65.84(8) . . ? C5 Y1 N1 83.00(8) . . ? C18 Y1 N1 86.66(9) . . ? C17 Y1 N1 115.98(10) . . ? C16 Y1 N1 141.99(10) . . ? C21 Y1 C20 30.96(11) . . ? C1 Y1 C20 129.32(10) . . ? C5 Y1 C20 104.83(10) . . ? C18 Y1 C20 116.20(11) . . ? C17 Y1 C20 121.49(11) . . ? C16 Y1 C20 98.75(12) . . ? N1 Y1 C20 90.31(9) . . ? C21 Y1 C19 56.69(11) . . ? C1 Y1 C19 146.23(10) . . ? C5 Y1 C19 133.03(9) . . ? C18 Y1 C19 86.20(10) . . ? C17 Y1 C19 97.80(11) . . ? C16 Y1 C19 85.26(11) . . ? N1 Y1 C19 84.45(9) . . ? C20 Y1 C19 30.26(9) . . ? C21 Y1 C2 132.57(10) . . ? C1 Y1 C2 31.71(8) . . ? C5 Y1 C2 51.92(8) . . ? C18 Y1 C2 86.98(10) . . ? C17 Y1 C2 79.51(10) . . ? C16 Y1 C2 96.44(11) . . ? N1 Y1 C2 88.52(8) . . ? C20 Y1 C2 156.68(9) . . ? C19 Y1 C2 170.48(9) . . ? C21 Y1 C4 81.98(10) . . ? C1 Y1 C4 52.18(8) . . ? C5 Y1 C4 30.87(9) . . ? C18 Y1 C4 129.97(10) . . ? C17 Y1 C4 106.07(10) . . ? C16 Y1 C4 98.45(10) . . ? N1 Y1 C4 113.23(8) . . ? C20 Y1 C4 109.37(10) . . ? C19 Y1 C4 138.52(9) . . ? C2 Y1 C4 50.60(9) . . ? C21 Y1 C3 106.45(11) . . ? C1 Y1 C3 51.31(9) . . ? C5 Y1 C3 50.75(9) . . ? C18 Y1 C3 99.74(10) . . ? C17 Y1 C3 78.67(10) . . ? C16 Y1 C3 81.33(10) . . ? N1 Y1 C3 116.09(8) . . ? C20 Y1 C3 136.83(10) . . ? C19 Y1 C3 158.75(10) . . ? C2 Y1 C3 29.96(9) . . ? C4 Y1 C3 30.28(9) . . ? N1 Si1 C1 101.40(11) . . ? N1 Si1 C11 109.07(13) . . ? C1 Si1 C11 113.76(15) . . ? N1 Si1 C10 112.49(15) . . ? C1 Si1 C10 113.75(13) . . ? C11 Si1 C10 106.40(17) . . ? N1 Si1 Y1 52.02(7) . . ? C1 Si1 Y1 50.03(8) . . ? C11 Si1 Y1 118.49(12) . . ? C10 Si1 Y1 135.06(12) . . ? C12 N1 C15 100.3(2) . . ? C12 N1 Si1 115.71(18) . . ? C15 N1 Si1 118.99(18) . . ? C12 N1 Y1 114.28(17) . . ? C15 N1 Y1 113.15(16) . . ? Si1 N1 Y1 95.33(10) . . ? C2 C1 C5 106.2(2) . . ? C2 C1 Si1 126.3(2) . . ? C5 C1 Si1 123.9(2) . . ? C2 C1 Y1 78.74(16) . . ? C5 C1 Y1 73.88(15) . . ? Si1 C1 Y1 96.43(11) . . ? C3 C2 C1 108.4(2) . . ? C3 C2 C6 124.3(3) . . ? C1 C2 C6 127.0(3) . . ? C3 C2 Y1 77.75(17) . . ? C1 C2 Y1 69.55(15) . . ? C6 C2 Y1 123.60(19) . . ? C2 C3 C4 108.4(2) . . ? C2 C3 C7 126.7(3) . . ? C4 C3 C7 124.5(3) . . ? C2 C3 Y1 72.29(16) . . ? C4 C3 Y1 72.18(16) . . ? C7 C3 Y1 127.1(2) . . ? C5 C4 C3 108.1(2) . . ? C5 C4 C8 126.5(3) . . ? C3 C4 C8 125.2(3) . . ? C5 C4 Y1 69.98(15) . . ? C3 C4 Y1 77.54(16) . . ? C8 C4 Y1 122.8(2) . . ? C4 C5 C1 108.8(2) . . ? C4 C5 C9 123.7(3) . . ? C1 C5 C9 127.4(3) . . ? C4 C5 Y1 79.14(15) . . ? C1 C5 Y1 73.56(14) . . ? C9 C5 Y1 115.76(19) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 106.2(3) . . ? N1 C12 H12A 110.5 . . ? C13 C12 H12A 110.5 . . ? N1 C12 H12B 110.5 . . ? C13 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? C14 C13 C12 105.2(3) . . ? C14 C13 H13A 110.7 . . ? C12 C13 H13A 110.7 . . ? C14 C13 H13B 110.7 . . ? C12 C13 H13B 110.7 . . ? H13A C13 H13B 108.8 . . ? C13 C14 C15 104.7(3) . . ? C13 C14 H14A 110.8 . . ? C15 C14 H14A 110.8 . . ? C13 C14 H14B 110.8 . . ? C15 C14 H14B 110.8 . . ? H14A C14 H14B 108.9 . . ? N1 C15 C14 106.1(2) . . ? N1 C15 H15A 110.5 . . ? C14 C15 H15A 110.5 . . ? N1 C15 H15B 110.5 . . ? C14 C15 H15B 110.5 . . ? H15A C15 H15B 108.7 . . ? C17 C16 Y1 74.47(19) . . ? C17 C16 H16A 116.1 . . ? Y1 C16 H16A 116.1 . . ? C17 C16 H16B 116.1 . . ? Y1 C16 H16B 116.1 . . ? H16A C16 H16B 113.0 . . ? C16 C17 C18 126.2(3) . . ? C16 C17 Y1 75.06(19) . . ? C18 C17 Y1 73.93(18) . . ? C16 C17 H17 116.5 . . ? C18 C17 H17 116.5 . . ? Y1 C17 H17 116.5 . . ? C17 C18 Y1 75.34(18) . . ? C17 C18 H18A 115.9 . . ? Y1 C18 H18A 115.9 . . ? C17 C18 H18B 115.9 . . ? Y1 C18 H18B 115.9 . . ? H18A C18 H18B 112.9 . . ? C20 C19 Y1 74.14(18) . . ? C20 C19 H19A 116.1 . . ? Y1 C19 H19A 116.1 . . ? C20 C19 H19B 116.1 . . ? Y1 C19 H19B 116.1 . . ? H19A C19 H19B 113.1 . . ? C19 C20 C21 126.7(3) . . ? C19 C20 Y1 75.61(18) . . ? C21 C20 Y1 71.21(19) . . ? C19 C20 H20 115.8 . . ? C21 C20 H20 115.8 . . ? Y1 C20 H20 115.8 . . ? C20 C21 Y1 77.83(17) . . ? C20 C21 H21A 115.6 . . ? Y1 C21 H21A 115.6 . . ? C20 C21 H21B 115.6 . . ? Y1 C21 H21B 115.6 . . ? H21A C21 H21B 112.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Y1 Si1 N1 -77.98(14) . . . . ? C1 Y1 Si1 N1 -169.01(13) . . . . ? C5 Y1 Si1 N1 -136.82(12) . . . . ? C18 Y1 Si1 N1 76.93(11) . . . . ? C17 Y1 Si1 N1 101.68(12) . . . . ? C16 Y1 Si1 N1 110.33(16) . . . . ? C20 Y1 Si1 N1 -44.60(12) . . . . ? C19 Y1 Si1 N1 -10.98(12) . . . . ? C2 Y1 Si1 N1 160.55(11) . . . . ? C4 Y1 Si1 N1 -153.29(11) . . . . ? C3 Y1 Si1 N1 176.26(10) . . . . ? C21 Y1 Si1 C1 91.04(15) . . . . ? C5 Y1 Si1 C1 32.19(13) . . . . ? C18 Y1 Si1 C1 -114.05(13) . . . . ? C17 Y1 Si1 C1 -89.31(14) . . . . ? C16 Y1 Si1 C1 -80.65(18) . . . . ? N1 Y1 Si1 C1 169.01(13) . . . . ? C20 Y1 Si1 C1 124.41(13) . . . . ? C19 Y1 Si1 C1 158.04(13) . . . . ? C2 Y1 Si1 C1 -30.43(12) . . . . ? C4 Y1 Si1 C1 15.72(12) . . . . ? C3 Y1 Si1 C1 -14.72(12) . . . . ? C21 Y1 Si1 C11 -170.72(17) . . . . ? C1 Y1 Si1 C11 98.24(17) . . . . ? C5 Y1 Si1 C11 130.43(16) . . . . ? C18 Y1 Si1 C11 -15.82(16) . . . . ? C17 Y1 Si1 C11 8.93(16) . . . . ? C16 Y1 Si1 C11 17.6(2) . . . . ? N1 Y1 Si1 C11 -92.75(16) . . . . ? C20 Y1 Si1 C11 -137.35(16) . . . . ? C19 Y1 Si1 C11 -103.72(16) . . . . ? C2 Y1 Si1 C11 67.81(15) . . . . ? C4 Y1 Si1 C11 113.96(15) . . . . ? C3 Y1 Si1 C11 83.51(15) . . . . ? C21 Y1 Si1 C10 6.5(2) . . . . ? C1 Y1 Si1 C10 -84.49(19) . . . . ? C5 Y1 Si1 C10 -52.30(18) . . . . ? C18 Y1 Si1 C10 161.45(18) . . . . ? C17 Y1 Si1 C10 -173.80(18) . . . . ? C16 Y1 Si1 C10 -165.1(2) . . . . ? N1 Y1 Si1 C10 84.52(18) . . . . ? C20 Y1 Si1 C10 39.92(18) . . . . ? C19 Y1 Si1 C10 73.55(18) . . . . ? C2 Y1 Si1 C10 -114.92(17) . . . . ? C4 Y1 Si1 C10 -68.77(17) . . . . ? C3 Y1 Si1 C10 -99.22(17) . . . . ? C1 Si1 N1 C12 111.7(2) . . . . ? C11 Si1 N1 C12 -128.0(2) . . . . ? C10 Si1 N1 C12 -10.2(2) . . . . ? Y1 Si1 N1 C12 120.2(2) . . . . ? C1 Si1 N1 C15 -128.8(2) . . . . ? C11 Si1 N1 C15 -8.5(3) . . . . ? C10 Si1 N1 C15 109.3(2) . . . . ? Y1 Si1 N1 C15 -120.2(2) . . . . ? C1 Si1 N1 Y1 -8.57(10) . . . . ? C11 Si1 N1 Y1 111.74(15) . . . . ? C10 Si1 N1 Y1 -130.45(13) . . . . ? C21 Y1 N1 C12 -0.4(2) . . . . ? C1 Y1 N1 C12 -114.71(19) . . . . ? C5 Y1 N1 C12 -85.82(19) . . . . ? C18 Y1 N1 C12 135.3(2) . . . . ? C17 Y1 N1 C12 144.80(19) . . . . ? C16 Y1 N1 C12 123.8(2) . . . . ? C20 Y1 N1 C12 19.08(19) . . . . ? C19 Y1 N1 C12 48.81(19) . . . . ? C2 Y1 N1 C12 -137.63(19) . . . . ? C4 Y1 N1 C12 -92.22(19) . . . . ? C3 Y1 N1 C12 -125.48(19) . . . . ? C21 Y1 N1 C15 -114.4(2) . . . . ? C1 Y1 N1 C15 131.3(2) . . . . ? C5 Y1 N1 C15 160.22(19) . . . . ? C18 Y1 N1 C15 21.36(19) . . . . ? C17 Y1 N1 C15 30.8(2) . . . . ? C16 Y1 N1 C15 9.8(3) . . . . ? C20 Y1 N1 C15 -94.87(19) . . . . ? C19 Y1 N1 C15 -65.14(19) . . . . ? C2 Y1 N1 C15 108.42(19) . . . . ? C4 Y1 N1 C15 153.83(18) . . . . ? C3 Y1 N1 C15 120.57(19) . . . . ? C21 Y1 N1 Si1 120.93(11) . . . . ? C1 Y1 N1 Si1 6.63(8) . . . . ? C5 Y1 N1 Si1 35.52(9) . . . . ? C18 Y1 N1 Si1 -103.35(11) . . . . ? C17 Y1 N1 Si1 -93.86(12) . . . . ? C16 Y1 N1 Si1 -114.87(16) . . . . ? C20 Y1 N1 Si1 140.42(10) . . . . ? C19 Y1 N1 Si1 170.15(10) . . . . ? C2 Y1 N1 Si1 -16.29(9) . . . . ? C4 Y1 N1 Si1 29.12(12) . . . . ? C3 Y1 N1 Si1 -4.14(12) . . . . ? N1 Si1 C1 C2 89.6(2) . . . . ? C11 Si1 C1 C2 -27.4(3) . . . . ? C10 Si1 C1 C2 -149.4(3) . . . . ? Y1 Si1 C1 C2 80.7(2) . . . . ? N1 Si1 C1 C5 -66.1(2) . . . . ? C11 Si1 C1 C5 177.0(2) . . . . ? C10 Si1 C1 C5 54.9(3) . . . . ? Y1 Si1 C1 C5 -74.9(2) . . . . ? N1 Si1 C1 Y1 8.81(11) . . . . ? C11 Si1 C1 Y1 -108.13(14) . . . . ? C10 Si1 C1 Y1 129.81(15) . . . . ? C21 Y1 C1 C2 122.16(18) . . . . ? C5 Y1 C1 C2 110.8(2) . . . . ? C18 Y1 C1 C2 -53.84(18) . . . . ? C17 Y1 C1 C2 -21.61(19) . . . . ? C16 Y1 C1 C2 6.0(2) . . . . ? N1 Y1 C1 C2 -132.23(17) . . . . ? C20 Y1 C1 C2 158.85(16) . . . . ? C19 Y1 C1 C2 -162.75(17) . . . . ? C4 Y1 C1 C2 74.19(17) . . . . ? C3 Y1 C1 C2 35.36(16) . . . . ? C21 Y1 C1 C5 11.4(2) . . . . ? C18 Y1 C1 C5 -164.59(17) . . . . ? C17 Y1 C1 C5 -132.36(17) . . . . ? C16 Y1 C1 C5 -104.79(19) . . . . ? N1 Y1 C1 C5 117.02(17) . . . . ? C20 Y1 C1 C5 48.1(2) . . . . ? C19 Y1 C1 C5 86.5(2) . . . . ? C2 Y1 C1 C5 -110.8(2) . . . . ? C4 Y1 C1 C5 -36.56(16) . . . . ? C3 Y1 C1 C5 -75.39(17) . . . . ? C21 Y1 C1 Si1 -112.07(14) . . . . ? C5 Y1 C1 Si1 -123.5(2) . . . . ? C18 Y1 C1 Si1 71.92(13) . . . . ? C17 Y1 C1 Si1 104.16(13) . . . . ? C16 Y1 C1 Si1 131.73(13) . . . . ? N1 Y1 C1 Si1 -6.47(8) . . . . ? C20 Y1 C1 Si1 -75.38(15) . . . . ? C19 Y1 C1 Si1 -37.0(2) . . . . ? C2 Y1 C1 Si1 125.8(2) . . . . ? C4 Y1 C1 Si1 -160.04(16) . . . . ? C3 Y1 C1 Si1 161.12(15) . . . . ? C5 C1 C2 C3 0.6(3) . . . . ? Si1 C1 C2 C3 -158.5(2) . . . . ? Y1 C1 C2 C3 -68.7(2) . . . . ? C5 C1 C2 C6 -173.4(3) . . . . ? Si1 C1 C2 C6 27.5(4) . . . . ? Y1 C1 C2 C6 117.3(3) . . . . ? C5 C1 C2 Y1 69.34(18) . . . . ? Si1 C1 C2 Y1 -89.7(2) . . . . ? C21 Y1 C2 C3 34.6(2) . . . . ? C1 Y1 C2 C3 115.2(2) . . . . ? C5 Y1 C2 C3 75.50(17) . . . . ? C18 Y1 C2 C3 -115.51(18) . . . . ? C17 Y1 C2 C3 -85.47(18) . . . . ? C16 Y1 C2 C3 -60.03(18) . . . . ? N1 Y1 C2 C3 157.76(16) . . . . ? C20 Y1 C2 C3 70.4(3) . . . . ? C19 Y1 C2 C3 -159.8(5) . . . . ? C4 Y1 C2 C3 35.63(16) . . . . ? C21 Y1 C2 C1 -80.7(2) . . . . ? C5 Y1 C2 C1 -39.75(15) . . . . ? C18 Y1 C2 C1 129.25(17) . . . . ? C17 Y1 C2 C1 159.29(18) . . . . ? C16 Y1 C2 C1 -175.27(17) . . . . ? N1 Y1 C2 C1 42.52(16) . . . . ? C20 Y1 C2 C1 -44.8(3) . . . . ? C19 Y1 C2 C1 84.9(6) . . . . ? C4 Y1 C2 C1 -79.62(17) . . . . ? C3 Y1 C2 C1 -115.2(2) . . . . ? C21 Y1 C2 C6 157.8(2) . . . . ? C1 Y1 C2 C6 -121.5(3) . . . . ? C5 Y1 C2 C6 -161.3(3) . . . . ? C18 Y1 C2 C6 7.7(2) . . . . ? C17 Y1 C2 C6 37.8(2) . . . . ? C16 Y1 C2 C6 63.2(3) . . . . ? N1 Y1 C2 C6 -79.0(2) . . . . ? C20 Y1 C2 C6 -166.4(3) . . . . ? C19 Y1 C2 C6 -36.6(7) . . . . ? C4 Y1 C2 C6 158.9(3) . . . . ? C3 Y1 C2 C6 123.2(3) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C6 C2 C3 C4 173.9(3) . . . . ? Y1 C2 C3 C4 -63.6(2) . . . . ? C1 C2 C3 C7 -173.2(3) . . . . ? C6 C2 C3 C7 1.0(5) . . . . ? Y1 C2 C3 C7 123.5(3) . . . . ? C1 C2 C3 Y1 63.30(19) . . . . ? C6 C2 C3 Y1 -122.5(3) . . . . ? C21 Y1 C3 C2 -154.18(17) . . . . ? C1 Y1 C3 C2 -37.52(15) . . . . ? C5 Y1 C3 C2 -79.80(18) . . . . ? C18 Y1 C3 C2 66.12(18) . . . . ? C17 Y1 C3 C2 88.62(18) . . . . ? C16 Y1 C3 C2 119.45(19) . . . . ? N1 Y1 C3 C2 -24.92(18) . . . . ? C20 Y1 C3 C2 -146.97(17) . . . . ? C19 Y1 C3 C2 170.9(2) . . . . ? C4 Y1 C3 C2 -116.8(2) . . . . ? C21 Y1 C3 C4 -37.4(2) . . . . ? C1 Y1 C3 C4 79.26(17) . . . . ? C5 Y1 C3 C4 36.98(16) . . . . ? C18 Y1 C3 C4 -177.10(18) . . . . ? C17 Y1 C3 C4 -154.60(19) . . . . ? C16 Y1 C3 C4 -123.77(19) . . . . ? N1 Y1 C3 C4 91.86(17) . . . . ? C20 Y1 C3 C4 -30.2(2) . . . . ? C19 Y1 C3 C4 -72.3(3) . . . . ? C2 Y1 C3 C4 116.8(2) . . . . ? C21 Y1 C3 C7 82.8(3) . . . . ? C1 Y1 C3 C7 -160.6(3) . . . . ? C5 Y1 C3 C7 157.1(3) . . . . ? C18 Y1 C3 C7 -56.9(3) . . . . ? C17 Y1 C3 C7 -34.4(3) . . . . ? C16 Y1 C3 C7 -3.6(3) . . . . ? N1 Y1 C3 C7 -148.0(3) . . . . ? C20 Y1 C3 C7 90.0(3) . . . . ? C19 Y1 C3 C7 47.9(4) . . . . ? C2 Y1 C3 C7 -123.1(4) . . . . ? C4 Y1 C3 C7 120.2(4) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C7 C3 C4 C5 173.0(3) . . . . ? Y1 C3 C4 C5 -63.83(19) . . . . ? C2 C3 C4 C8 -174.8(3) . . . . ? C7 C3 C4 C8 -1.6(5) . . . . ? Y1 C3 C4 C8 121.6(3) . . . . ? C2 C3 C4 Y1 63.7(2) . . . . ? C7 C3 C4 Y1 -123.2(3) . . . . ? C21 Y1 C4 C5 -101.24(19) . . . . ? C1 Y1 C4 C5 38.67(15) . . . . ? C18 Y1 C4 C5 118.52(19) . . . . ? C17 Y1 C4 C5 140.74(18) . . . . ? C16 Y1 C4 C5 170.97(18) . . . . ? N1 Y1 C4 C5 12.44(18) . . . . ? C20 Y1 C4 C5 -86.60(18) . . . . ? C19 Y1 C4 C5 -96.6(2) . . . . ? C2 Y1 C4 C5 79.55(18) . . . . ? C3 Y1 C4 C5 114.8(2) . . . . ? C21 Y1 C4 C3 143.97(19) . . . . ? C1 Y1 C4 C3 -76.12(18) . . . . ? C5 Y1 C4 C3 -114.8(2) . . . . ? C18 Y1 C4 C3 3.7(2) . . . . ? C17 Y1 C4 C3 26.0(2) . . . . ? C16 Y1 C4 C3 56.18(19) . . . . ? N1 Y1 C4 C3 -102.35(17) . . . . ? C20 Y1 C4 C3 158.61(17) . . . . ? C19 Y1 C4 C3 148.58(18) . . . . ? C2 Y1 C4 C3 -35.24(16) . . . . ? C21 Y1 C4 C8 20.0(3) . . . . ? C1 Y1 C4 C8 159.9(3) . . . . ? C5 Y1 C4 C8 121.2(3) . . . . ? C18 Y1 C4 C8 -120.3(3) . . . . ? C17 Y1 C4 C8 -98.1(3) . . . . ? C16 Y1 C4 C8 -67.8(3) . . . . ? N1 Y1 C4 C8 133.6(2) . . . . ? C20 Y1 C4 C8 34.6(3) . . . . ? C19 Y1 C4 C8 24.6(3) . . . . ? C2 Y1 C4 C8 -159.3(3) . . . . ? C3 Y1 C4 C8 -124.0(3) . . . . ? C3 C4 C5 C1 0.6(3) . . . . ? C8 C4 C5 C1 175.1(3) . . . . ? Y1 C4 C5 C1 -68.29(18) . . . . ? C3 C4 C5 C9 -177.3(3) . . . . ? C8 C4 C5 C9 -2.8(5) . . . . ? Y1 C4 C5 C9 113.8(3) . . . . ? C3 C4 C5 Y1 68.9(2) . . . . ? C8 C4 C5 Y1 -116.6(3) . . . . ? C2 C1 C5 C4 -0.7(3) . . . . ? Si1 C1 C5 C4 159.0(2) . . . . ? Y1 C1 C5 C4 72.06(19) . . . . ? C2 C1 C5 C9 177.0(3) . . . . ? Si1 C1 C5 C9 -23.2(4) . . . . ? Y1 C1 C5 C9 -110.2(3) . . . . ? C2 C1 C5 Y1 -72.79(18) . . . . ? Si1 C1 C5 Y1 86.92(18) . . . . ? C21 Y1 C5 C4 76.27(18) . . . . ? C1 Y1 C5 C4 -113.5(2) . . . . ? C18 Y1 C5 C4 -91.3(2) . . . . ? C17 Y1 C5 C4 -50.8(2) . . . . ? C16 Y1 C5 C4 -11.5(2) . . . . ? N1 Y1 C5 C4 -168.49(17) . . . . ? C20 Y1 C5 C4 103.05(18) . . . . ? C19 Y1 C5 C4 115.85(18) . . . . ? C2 Y1 C5 C4 -74.87(18) . . . . ? C3 Y1 C5 C4 -36.24(16) . . . . ? C21 Y1 C5 C1 -170.22(18) . . . . ? C18 Y1 C5 C1 22.2(2) . . . . ? C17 Y1 C5 C1 62.8(2) . . . . ? C16 Y1 C5 C1 102.0(2) . . . . ? N1 Y1 C5 C1 -54.98(16) . . . . ? C20 Y1 C5 C1 -143.44(16) . . . . ? C19 Y1 C5 C1 -130.63(17) . . . . ? C2 Y1 C5 C1 38.64(16) . . . . ? C4 Y1 C5 C1 113.5(2) . . . . ? C3 Y1 C5 C1 77.28(18) . . . . ? C21 Y1 C5 C9 -46.1(2) . . . . ? C1 Y1 C5 C9 124.1(3) . . . . ? C18 Y1 C5 C9 146.3(2) . . . . ? C17 Y1 C5 C9 -173.1(2) . . . . ? C16 Y1 C5 C9 -133.8(2) . . . . ? N1 Y1 C5 C9 69.2(2) . . . . ? C20 Y1 C5 C9 -19.3(2) . . . . ? C19 Y1 C5 C9 -6.5(3) . . . . ? C2 Y1 C5 C9 162.8(3) . . . . ? C4 Y1 C5 C9 -122.3(3) . . . . ? C3 Y1 C5 C9 -158.6(3) . . . . ? C15 N1 C12 C13 -39.7(3) . . . . ? Si1 N1 C12 C13 89.6(3) . . . . ? Y1 N1 C12 C13 -161.1(2) . . . . ? N1 C12 C13 C14 24.7(4) . . . . ? C12 C13 C14 C15 0.7(4) . . . . ? C12 N1 C15 C14 40.2(3) . . . . ? Si1 N1 C15 C14 -87.0(3) . . . . ? Y1 N1 C15 C14 162.3(2) . . . . ? C13 C14 C15 N1 -25.7(4) . . . . ? C21 Y1 C16 C17 170.8(2) . . . . ? C1 Y1 C16 C17 -59.6(3) . . . . ? C5 Y1 C16 C17 -101.5(2) . . . . ? C18 Y1 C16 C17 25.6(2) . . . . ? N1 Y1 C16 C17 39.5(3) . . . . ? C20 Y1 C16 C17 141.3(2) . . . . ? C19 Y1 C16 C17 114.2(2) . . . . ? C2 Y1 C16 C17 -56.4(2) . . . . ? C4 Y1 C16 C17 -107.4(2) . . . . ? C3 Y1 C16 C17 -82.4(2) . . . . ? Y1 C16 C17 C18 -56.7(3) . . . . ? C21 Y1 C17 C16 -10.5(3) . . . . ? C1 Y1 C17 C16 134.0(2) . . . . ? C5 Y1 C17 C16 103.6(2) . . . . ? C18 Y1 C17 C16 -135.4(3) . . . . ? N1 Y1 C17 C16 -154.2(2) . . . . ? C20 Y1 C17 C16 -46.4(3) . . . . ? C19 Y1 C17 C16 -66.6(2) . . . . ? C2 Y1 C17 C16 122.7(2) . . . . ? C4 Y1 C17 C16 79.1(2) . . . . ? C3 Y1 C17 C16 92.2(2) . . . . ? C21 Y1 C17 C18 124.9(2) . . . . ? C1 Y1 C17 C18 -90.6(2) . . . . ? C5 Y1 C17 C18 -121.0(2) . . . . ? C16 Y1 C17 C18 135.4(3) . . . . ? N1 Y1 C17 C18 -18.8(2) . . . . ? C20 Y1 C17 C18 89.0(2) . . . . ? C19 Y1 C17 C18 68.8(2) . . . . ? C2 Y1 C17 C18 -101.9(2) . . . . ? C4 Y1 C17 C18 -145.4(2) . . . . ? C3 Y1 C17 C18 -132.4(2) . . . . ? C16 C17 C18 Y1 57.1(3) . . . . ? C21 Y1 C18 C17 -75.8(3) . . . . ? C1 Y1 C18 C17 99.6(2) . . . . ? C5 Y1 C18 C17 87.3(3) . . . . ? C16 Y1 C18 C17 -25.4(2) . . . . ? N1 Y1 C18 C17 163.1(2) . . . . ? C20 Y1 C18 C17 -108.2(2) . . . . ? C19 Y1 C18 C17 -112.2(2) . . . . ? C2 Y1 C18 C17 74.5(2) . . . . ? C4 Y1 C18 C17 45.3(3) . . . . ? C3 Y1 C18 C17 47.2(2) . . . . ? C21 Y1 C19 C20 24.5(2) . . . . ? C1 Y1 C19 C20 -72.5(3) . . . . ? C5 Y1 C19 C20 -25.2(3) . . . . ? C18 Y1 C19 C20 172.8(2) . . . . ? C17 Y1 C19 C20 144.3(2) . . . . ? C16 Y1 C19 C20 116.4(2) . . . . ? N1 Y1 C19 C20 -100.2(2) . . . . ? C2 Y1 C19 C20 -142.8(5) . . . . ? C4 Y1 C19 C20 19.0(3) . . . . ? C3 Y1 C19 C20 65.5(3) . . . . ? Y1 C19 C20 C21 -52.7(3) . . . . ? C21 Y1 C20 C19 -137.6(3) . . . . ? C1 Y1 C20 C19 136.76(19) . . . . ? C5 Y1 C20 C19 161.24(19) . . . . ? C18 Y1 C20 C19 -8.0(2) . . . . ? C17 Y1 C20 C19 -42.7(2) . . . . ? C16 Y1 C20 C19 -64.5(2) . . . . ? N1 Y1 C20 C19 78.4(2) . . . . ? C2 Y1 C20 C19 165.4(2) . . . . ? C4 Y1 C20 C19 -166.76(19) . . . . ? C3 Y1 C20 C19 -151.17(18) . . . . ? C1 Y1 C20 C21 -85.6(2) . . . . ? C5 Y1 C20 C21 -61.1(2) . . . . ? C18 Y1 C20 C21 129.6(2) . . . . ? C17 Y1 C20 C21 94.9(2) . . . . ? C16 Y1 C20 C21 73.1(2) . . . . ? N1 Y1 C20 C21 -144.0(2) . . . . ? C19 Y1 C20 C21 137.6(3) . . . . ? C2 Y1 C20 C21 -57.0(4) . . . . ? C4 Y1 C20 C21 -29.1(2) . . . . ? C3 Y1 C20 C21 -13.5(3) . . . . ? C19 C20 C21 Y1 54.5(3) . . . . ? C1 Y1 C21 C20 116.0(2) . . . . ? C5 Y1 C21 C20 122.2(2) . . . . ? C18 Y1 C21 C20 -69.1(3) . . . . ? C17 Y1 C21 C20 -103.6(2) . . . . ? C16 Y1 C21 C20 -108.9(2) . . . . ? N1 Y1 C21 C20 40.4(2) . . . . ? C19 Y1 C21 C20 -23.97(19) . . . . ? C2 Y1 C21 C20 153.21(19) . . . . ? C4 Y1 C21 C20 152.4(2) . . . . ? C3 Y1 C21 C20 170.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.414 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.068 _database_code_depnum_ccdc_archive 'CCDC 917595' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_g120420a-mo #TrackingRef 'complexes 16 CIF.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Lu N Si' _chemical_formula_sum 'C21 H36 Lu N Si' _chemical_formula_weight 505.57 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' Lu Lu -0.4720 5.8584 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.9928(9) _cell_length_b 9.9102(2) _cell_length_c 17.1932(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.218(4) _cell_angle_gamma 90.00 _cell_volume 4257.8(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5032 _cell_measurement_theta_min 3.0723 _cell_measurement_theta_max 29.3285 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 4.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.211 _exptl_absorpt_correction_T_max 0.391 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11010 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.49 _reflns_number_total 3959 _reflns_number_gt 3209 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+2.5641P] 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 3959 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0509 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 Lu1 Lu 0.129124(7) 0.742773(15) 0.159668(9) 0.01750(7) Uani 1 1 d . . . Si1 Si 0.11601(5) 0.73450(11) -0.03796(7) 0.0214(3) Uani 1 1 d . . . N1 N 0.13681(13) 0.6001(3) 0.03902(19) 0.0199(8) Uani 1 1 d . . . C1 C 0.09407(16) 0.8638(4) 0.0202(2) 0.0165(9) Uani 1 1 d . . . C2 C 0.12743(17) 0.9654(4) 0.0747(2) 0.0225(10) Uani 1 1 d . . . C3 C 0.10364(18) 1.0092(4) 0.1297(3) 0.0263(10) Uani 1 1 d . . . C4 C 0.05590(18) 0.9356(4) 0.1124(2) 0.0255(10) Uani 1 1 d . . . C5 C 0.04923(16) 0.8463(4) 0.0447(2) 0.0181(9) Uani 1 1 d . . . C6 C 0.17694(19) 1.0298(4) 0.0687(3) 0.0362(12) Uani 1 1 d . . . H6A H 0.1854 1.1112 0.1014 0.054 Uiso 1 1 calc R . . H6B H 0.1702 1.0508 0.0110 0.054 Uiso 1 1 calc R . . H6C H 0.2065 0.9682 0.0897 0.054 Uiso 1 1 calc R . . C7 C 0.1212(2) 1.1238(4) 0.1918(3) 0.0435(13) Uani 1 1 d . . . H7A H 0.1588 1.1396 0.2070 0.065 Uiso 1 1 calc R . . H7B H 0.1144 1.1011 0.2411 0.065 Uiso 1 1 calc R . . H7C H 0.1017 1.2039 0.1668 0.065 Uiso 1 1 calc R . . C8 C 0.0156(2) 0.9593(5) 0.1527(3) 0.0414(13) Uani 1 1 d . . . H8A H 0.0341 0.9735 0.2119 0.062 Uiso 1 1 calc R . . H8B H -0.0073 0.8819 0.1437 0.062 Uiso 1 1 calc R . . H8C H -0.0056 1.0374 0.1281 0.062 Uiso 1 1 calc R . . C9 C 0.00117(17) 0.7568(4) 0.0044(3) 0.0298(10) Uani 1 1 d . . . H9A H 0.0076 0.6707 0.0321 0.045 Uiso 1 1 calc R . . H9B H -0.0050 0.7446 -0.0539 0.045 Uiso 1 1 calc R . . H9C H -0.0297 0.7980 0.0094 0.045 Uiso 1 1 calc R . . C10 C 0.0624(2) 0.6808(5) -0.1389(3) 0.0407(13) Uani 1 1 d . . . H10A H 0.0767 0.6162 -0.1664 0.061 Uiso 1 1 calc R . . H10B H 0.0495 0.7580 -0.1746 0.061 Uiso 1 1 calc R . . H10C H 0.0335 0.6406 -0.1275 0.061 Uiso 1 1 calc R . . C11 C 0.1739(2) 0.7874(5) -0.0639(3) 0.0434(13) Uani 1 1 d . . . H11A H 0.2042 0.8043 -0.0129 0.065 Uiso 1 1 calc R . . H11B H 0.1649 0.8683 -0.0971 0.065 Uiso 1 1 calc R . . H11C H 0.1825 0.7171 -0.0951 0.065 Uiso 1 1 calc R . . C12 C 0.1015(2) 0.4773(4) 0.0164(3) 0.0333(11) Uani 1 1 d . . . H12A H 0.0648 0.5021 -0.0169 0.040 Uiso 1 1 calc R . . H12B H 0.1024 0.4309 0.0666 0.040 Uiso 1 1 calc R . . C13 C 0.1245(2) 0.3879(5) -0.0342(3) 0.0535(16) Uani 1 1 d . . . H13A H 0.1216 0.2934 -0.0219 0.064 Uiso 1 1 calc R . . H13B H 0.1055 0.4024 -0.0940 0.064 Uiso 1 1 calc R . . C14 C 0.1830(2) 0.4294(5) -0.0073(3) 0.0471(14) Uani 1 1 d . . . H14A H 0.1903 0.4643 -0.0547 0.056 Uiso 1 1 calc R . . H14B H 0.2065 0.3534 0.0166 0.056 Uiso 1 1 calc R . . C15 C 0.19054(18) 0.5394(4) 0.0587(3) 0.0300(11) Uani 1 1 d . . . H15A H 0.2039 0.5008 0.1147 0.036 Uiso 1 1 calc R . . H15B H 0.2157 0.6070 0.0557 0.036 Uiso 1 1 calc R . . C16 C 0.1859(2) 0.8383(5) 0.3072(3) 0.0470(14) Uani 1 1 d . . . H16A H 0.1723 0.9193 0.3239 0.056 Uiso 1 1 calc R . . H16B H 0.1998 0.7728 0.3521 0.056 Uiso 1 1 calc R . . C17 C 0.2153(2) 0.8572(5) 0.2579(3) 0.0413(14) Uani 1 1 d . . . H17 H 0.2205 0.9509 0.2446 0.050 Uiso 1 1 calc R . . C18 C 0.23047(18) 0.7588(4) 0.2141(3) 0.0369(12) Uani 1 1 d . . . H18A H 0.2500 0.6826 0.2469 0.044 Uiso 1 1 calc R . . H18B H 0.2454 0.7912 0.1743 0.044 Uiso 1 1 calc R . . C19 C 0.1452(2) 0.5092(4) 0.2384(3) 0.0337(12) Uani 1 1 d . . . H19A H 0.1563 0.4352 0.2117 0.040 Uiso 1 1 calc R . . H19B H 0.1643 0.5121 0.2988 0.040 Uiso 1 1 calc R . . C20 C 0.0907(2) 0.5349(5) 0.2093(3) 0.0381(12) Uani 1 1 d . . . H20 H 0.0681 0.4749 0.1647 0.046 Uiso 1 1 calc R . . C21 C 0.0661(2) 0.6505(5) 0.2224(3) 0.0422(13) Uani 1 1 d . . . H21A H 0.0742 0.6740 0.2807 0.051 Uiso 1 1 calc R . . H21B H 0.0283 0.6591 0.1879 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.01984(11) 0.01657(10) 0.01481(10) 0.00106(7) 0.00509(7) -0.00023(8) Si1 0.0222(7) 0.0266(6) 0.0163(6) 0.0028(4) 0.0085(5) 0.0046(5) N1 0.020(2) 0.0202(18) 0.0186(18) 0.0004(13) 0.0069(16) 0.0028(15) C1 0.018(2) 0.015(2) 0.014(2) 0.0025(15) 0.0034(18) 0.0023(16) C2 0.021(3) 0.018(2) 0.023(2) 0.0060(17) 0.002(2) 0.0029(18) C3 0.033(3) 0.016(2) 0.022(2) 0.0022(17) 0.001(2) 0.0093(19) C4 0.029(3) 0.025(2) 0.019(2) 0.0030(17) 0.006(2) 0.012(2) C5 0.019(2) 0.018(2) 0.018(2) 0.0039(15) 0.0069(19) 0.0035(17) C6 0.033(3) 0.025(3) 0.045(3) 0.005(2) 0.008(2) -0.007(2) C7 0.052(4) 0.022(3) 0.041(3) -0.006(2) 0.000(3) 0.005(2) C8 0.049(4) 0.048(3) 0.037(3) 0.002(2) 0.027(3) 0.020(3) C9 0.019(2) 0.033(3) 0.036(3) 0.0001(19) 0.009(2) -0.003(2) C10 0.048(3) 0.043(3) 0.022(2) -0.006(2) 0.003(2) 0.017(2) C11 0.047(3) 0.053(3) 0.047(3) 0.018(2) 0.037(3) 0.012(3) C12 0.040(3) 0.022(2) 0.031(3) -0.0048(19) 0.006(2) -0.010(2) C13 0.071(5) 0.033(3) 0.042(3) -0.011(2) 0.005(3) 0.014(3) C14 0.068(4) 0.044(3) 0.040(3) -0.001(2) 0.032(3) 0.017(3) C15 0.031(3) 0.031(3) 0.030(2) 0.0067(19) 0.014(2) 0.009(2) C16 0.061(4) 0.040(3) 0.023(3) -0.006(2) -0.002(3) 0.010(3) C17 0.039(3) 0.028(3) 0.030(3) -0.002(2) -0.018(3) -0.003(2) C18 0.029(3) 0.030(3) 0.040(3) 0.005(2) -0.001(2) 0.001(2) C19 0.047(4) 0.030(3) 0.029(3) 0.0090(19) 0.020(3) 0.004(2) C20 0.050(4) 0.033(3) 0.042(3) 0.015(2) 0.029(3) -0.005(2) C21 0.050(4) 0.045(3) 0.044(3) 0.021(2) 0.032(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 C21 2.506(4) . ? Lu1 C1 2.523(4) . ? Lu1 C5 2.528(4) . ? Lu1 C18 2.539(5) . ? Lu1 C17 2.564(4) . ? Lu1 N1 2.583(3) . ? Lu1 C20 2.592(4) . ? Lu1 C16 2.596(4) . ? Lu1 C19 2.633(4) . ? Lu1 C2 2.637(4) . ? Lu1 C4 2.647(4) . ? Lu1 C3 2.728(4) . ? Si1 N1 1.811(3) . ? Si1 C11 1.855(5) . ? Si1 C1 1.855(4) . ? Si1 C10 1.868(4) . ? N1 C15 1.486(5) . ? N1 C12 1.503(5) . ? C1 C5 1.434(5) . ? C1 C2 1.436(5) . ? C2 C3 1.399(6) . ? C2 C6 1.520(6) . ? C3 C4 1.411(6) . ? C3 C7 1.507(6) . ? C4 C5 1.418(5) . ? C4 C8 1.514(6) . ? C5 C9 1.507(5) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.529(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.525(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.531(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.374(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.386(6) . ? C17 H17 0.9800 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.387(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.384(6) . ? C20 H20 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 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 C21 Lu1 C1 120.71(15) . . ? C21 Lu1 C5 88.15(15) . . ? C1 Lu1 C5 32.98(12) . . ? C21 Lu1 C18 132.55(16) . . ? C1 Lu1 C18 106.56(14) . . ? C5 Lu1 C18 138.11(14) . . ? C21 Lu1 C17 118.15(18) . . ? C1 Lu1 C17 109.68(14) . . ? C5 Lu1 C17 128.96(13) . . ? C18 Lu1 C17 31.52(15) . . ? C21 Lu1 N1 114.79(14) . . ? C1 Lu1 N1 67.19(11) . . ? C5 Lu1 N1 84.14(11) . . ? C18 Lu1 N1 85.85(13) . . ? C17 Lu1 N1 116.30(15) . . ? C21 Lu1 C20 31.46(15) . . ? C1 Lu1 C20 129.63(15) . . ? C5 Lu1 C20 104.55(15) . . ? C18 Lu1 C20 115.96(16) . . ? C17 Lu1 C20 120.69(16) . . ? N1 Lu1 C20 89.59(13) . . ? C21 Lu1 C16 87.63(18) . . ? C1 Lu1 C16 128.73(14) . . ? C5 Lu1 C16 129.05(14) . . ? C18 Lu1 C16 57.43(16) . . ? C17 Lu1 C16 30.88(15) . . ? N1 Lu1 C16 141.95(15) . . ? C20 Lu1 C16 97.47(16) . . ? C21 Lu1 C19 57.65(15) . . ? C1 Lu1 C19 146.73(13) . . ? C5 Lu1 C19 133.25(14) . . ? C18 Lu1 C19 85.42(15) . . ? C17 Lu1 C19 96.76(15) . . ? N1 Lu1 C19 83.33(12) . . ? C20 Lu1 C19 30.77(14) . . ? C16 Lu1 C19 84.07(15) . . ? C21 Lu1 C2 132.18(14) . . ? C1 Lu1 C2 32.22(12) . . ? C5 Lu1 C2 52.84(12) . . ? C18 Lu1 C2 86.70(14) . . ? C17 Lu1 C2 79.44(14) . . ? N1 Lu1 C2 90.16(11) . . ? C20 Lu1 C2 157.26(15) . . ? C16 Lu1 C2 96.69(14) . . ? C19 Lu1 C2 170.11(14) . . ? C21 Lu1 C4 81.16(14) . . ? C1 Lu1 C4 52.88(12) . . ? C5 Lu1 C4 31.71(12) . . ? C18 Lu1 C4 130.05(14) . . ? C17 Lu1 C4 105.61(14) . . ? N1 Lu1 C4 115.21(11) . . ? C20 Lu1 C4 109.27(15) . . ? C16 Lu1 C4 97.65(14) . . ? C19 Lu1 C4 138.73(14) . . ? C2 Lu1 C4 51.04(13) . . ? C21 Lu1 C3 105.71(15) . . ? C1 Lu1 C3 51.93(12) . . ? C5 Lu1 C3 51.66(12) . . ? C18 Lu1 C3 99.72(14) . . ? C17 Lu1 C3 78.32(14) . . ? N1 Lu1 C3 118.00(11) . . ? C20 Lu1 C3 136.70(15) . . ? C16 Lu1 C3 81.07(14) . . ? C19 Lu1 C3 158.21(13) . . ? C2 Lu1 C3 30.17(13) . . ? C4 Lu1 C3 30.39(13) . . ? N1 Si1 C11 109.10(19) . . ? N1 Si1 C1 100.82(16) . . ? C11 Si1 C1 113.8(2) . . ? N1 Si1 C10 112.74(19) . . ? C11 Si1 C10 106.5(2) . . ? C1 Si1 C10 113.87(19) . . ? N1 Si1 Lu1 51.63(10) . . ? C11 Si1 Lu1 118.09(17) . . ? C1 Si1 Lu1 49.89(11) . . ? C10 Si1 Lu1 135.34(17) . . ? C15 N1 C12 101.5(3) . . ? C15 N1 Si1 118.1(3) . . ? C12 N1 Si1 114.6(3) . . ? C15 N1 Lu1 114.0(2) . . ? C12 N1 Lu1 114.5(2) . . ? Si1 N1 Lu1 95.02(13) . . ? C5 C1 C2 106.5(3) . . ? C5 C1 Si1 123.5(3) . . ? C2 C1 Si1 125.9(3) . . ? C5 C1 Lu1 73.7(2) . . ? C2 C1 Lu1 78.3(2) . . ? Si1 C1 Lu1 95.89(15) . . ? C3 C2 C1 108.9(4) . . ? C3 C2 C6 123.8(4) . . ? C1 C2 C6 126.9(4) . . ? C3 C2 Lu1 78.5(2) . . ? C1 C2 Lu1 69.5(2) . . ? C6 C2 Lu1 123.9(3) . . ? C2 C3 C4 108.2(4) . . ? C2 C3 C7 127.6(4) . . ? C4 C3 C7 123.9(4) . . ? C2 C3 Lu1 71.3(2) . . ? C4 C3 Lu1 71.6(2) . . ? C7 C3 Lu1 127.4(3) . . ? C3 C4 C5 108.6(4) . . ? C3 C4 C8 125.5(4) . . ? C5 C4 C8 125.6(4) . . ? C3 C4 Lu1 78.0(2) . . ? C5 C4 Lu1 69.5(2) . . ? C8 C4 Lu1 123.6(3) . . ? C4 C5 C1 107.8(4) . . ? C4 C5 C9 124.4(4) . . ? C1 C5 C9 127.7(3) . . ? C4 C5 Lu1 78.8(2) . . ? C1 C5 Lu1 73.3(2) . . ? C9 C5 Lu1 116.9(2) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 105.2(4) . . ? N1 C12 H12A 110.7 . . ? C13 C12 H12A 110.7 . . ? N1 C12 H12B 110.7 . . ? C13 C12 H12B 110.7 . . ? H12A C12 H12B 108.8 . . ? C14 C13 C12 105.5(4) . . ? C14 C13 H13A 110.6 . . ? C12 C13 H13A 110.6 . . ? C14 C13 H13B 110.6 . . ? C12 C13 H13B 110.6 . . ? H13A C13 H13B 108.8 . . ? C13 C14 C15 104.4(4) . . ? C13 C14 H14A 110.9 . . ? C15 C14 H14A 110.9 . . ? C13 C14 H14B 110.9 . . ? C15 C14 H14B 110.9 . . ? H14A C14 H14B 108.9 . . ? N1 C15 C14 105.9(4) . . ? N1 C15 H15A 110.5 . . ? C14 C15 H15A 110.5 . . ? N1 C15 H15B 110.5 . . ? C14 C15 H15B 110.5 . . ? H15A C15 H15B 108.7 . . ? C17 C16 Lu1 73.3(3) . . ? C17 C16 H16A 116.2 . . ? Lu1 C16 H16A 116.2 . . ? C17 C16 H16B 116.2 . . ? Lu1 C16 H16B 116.2 . . ? H16A C16 H16B 113.2 . . ? C16 C17 C18 126.7(5) . . ? C16 C17 Lu1 75.8(3) . . ? C18 C17 Lu1 73.3(3) . . ? C16 C17 H17 116.2 . . ? C18 C17 H17 116.2 . . ? Lu1 C17 H17 116.2 . . ? C17 C18 Lu1 75.2(3) . . ? C17 C18 H18A 115.9 . . ? Lu1 C18 H18A 115.9 . . ? C17 C18 H18B 115.9 . . ? Lu1 C18 H18B 115.9 . . ? H18A C18 H18B 112.9 . . ? C20 C19 Lu1 73.0(2) . . ? C20 C19 H19A 116.3 . . ? Lu1 C19 H19A 116.3 . . ? C20 C19 H19B 116.3 . . ? Lu1 C19 H19B 116.3 . . ? H19A C19 H19B 113.2 . . ? C21 C20 C19 127.0(5) . . ? C21 C20 Lu1 70.8(3) . . ? C19 C20 Lu1 76.3(3) . . ? C21 C20 H20 115.7 . . ? C19 C20 H20 115.7 . . ? Lu1 C20 H20 115.7 . . ? C20 C21 Lu1 77.7(3) . . ? C20 C21 H21A 115.6 . . ? Lu1 C21 H21A 115.6 . . ? C20 C21 H21B 115.6 . . ? Lu1 C21 H21B 115.6 . . ? H21A C21 H21B 112.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Lu1 Si1 N1 -77.9(2) . . . . ? C1 Lu1 Si1 N1 -168.5(2) . . . . ? C5 Lu1 Si1 N1 -136.15(17) . . . . ? C18 Lu1 Si1 N1 76.88(17) . . . . ? C17 Lu1 Si1 N1 101.65(18) . . . . ? C20 Lu1 Si1 N1 -43.95(19) . . . . ? C16 Lu1 Si1 N1 109.7(2) . . . . ? C19 Lu1 Si1 N1 -9.77(18) . . . . ? C2 Lu1 Si1 N1 160.78(18) . . . . ? C4 Lu1 Si1 N1 -153.19(17) . . . . ? C3 Lu1 Si1 N1 176.33(17) . . . . ? C21 Lu1 Si1 C11 -170.8(2) . . . . ? C1 Lu1 Si1 C11 98.6(2) . . . . ? C5 Lu1 Si1 C11 131.0(2) . . . . ? C18 Lu1 Si1 C11 -16.0(2) . . . . ? C17 Lu1 Si1 C11 8.8(2) . . . . ? N1 Lu1 Si1 C11 -92.9(2) . . . . ? C20 Lu1 Si1 C11 -136.8(2) . . . . ? C16 Lu1 Si1 C11 16.8(3) . . . . ? C19 Lu1 Si1 C11 -102.7(2) . . . . ? C2 Lu1 Si1 C11 67.9(2) . . . . ? C4 Lu1 Si1 C11 113.9(2) . . . . ? C3 Lu1 Si1 C11 83.4(2) . . . . ? C21 Lu1 Si1 C1 90.7(2) . . . . ? C5 Lu1 Si1 C1 32.38(19) . . . . ? C18 Lu1 Si1 C1 -114.58(19) . . . . ? C17 Lu1 Si1 C1 -89.8(2) . . . . ? N1 Lu1 Si1 C1 168.5(2) . . . . ? C20 Lu1 Si1 C1 124.6(2) . . . . ? C16 Lu1 Si1 C1 -81.7(3) . . . . ? C19 Lu1 Si1 C1 158.8(2) . . . . ? C2 Lu1 Si1 C1 -30.69(19) . . . . ? C4 Lu1 Si1 C1 15.35(19) . . . . ? C3 Lu1 Si1 C1 -15.14(19) . . . . ? C21 Lu1 Si1 C10 6.4(3) . . . . ? C1 Lu1 Si1 C10 -84.3(3) . . . . ? C5 Lu1 Si1 C10 -51.9(2) . . . . ? C18 Lu1 Si1 C10 161.1(2) . . . . ? C17 Lu1 Si1 C10 -174.1(2) . . . . ? N1 Lu1 Si1 C10 84.3(3) . . . . ? C20 Lu1 Si1 C10 40.3(2) . . . . ? C16 Lu1 Si1 C10 -166.0(3) . . . . ? C19 Lu1 Si1 C10 74.5(2) . . . . ? C2 Lu1 Si1 C10 -115.0(2) . . . . ? C4 Lu1 Si1 C10 -68.9(2) . . . . ? C3 Lu1 Si1 C10 -99.4(2) . . . . ? C11 Si1 N1 C15 -9.4(3) . . . . ? C1 Si1 N1 C15 -129.5(3) . . . . ? C10 Si1 N1 C15 108.7(3) . . . . ? Lu1 Si1 N1 C15 -120.6(3) . . . . ? C11 Si1 N1 C12 -128.9(3) . . . . ? C1 Si1 N1 C12 111.0(3) . . . . ? C10 Si1 N1 C12 -10.8(3) . . . . ? Lu1 Si1 N1 C12 119.9(3) . . . . ? C11 Si1 N1 Lu1 111.2(2) . . . . ? C1 Si1 N1 Lu1 -8.90(17) . . . . ? C10 Si1 N1 Lu1 -130.69(18) . . . . ? C21 Lu1 N1 C15 -114.7(3) . . . . ? C1 Lu1 N1 C15 130.7(3) . . . . ? C5 Lu1 N1 C15 160.1(3) . . . . ? C18 Lu1 N1 C15 20.8(3) . . . . ? C17 Lu1 N1 C15 29.2(3) . . . . ? C20 Lu1 N1 C15 -95.2(3) . . . . ? C16 Lu1 N1 C15 6.4(4) . . . . ? C19 Lu1 N1 C15 -65.0(3) . . . . ? C2 Lu1 N1 C15 107.5(3) . . . . ? C4 Lu1 N1 C15 153.6(3) . . . . ? C3 Lu1 N1 C15 119.6(3) . . . . ? C21 Lu1 N1 C12 1.6(3) . . . . ? C1 Lu1 N1 C12 -113.0(3) . . . . ? C5 Lu1 N1 C12 -83.6(3) . . . . ? C18 Lu1 N1 C12 137.1(3) . . . . ? C17 Lu1 N1 C12 145.5(3) . . . . ? C20 Lu1 N1 C12 21.1(3) . . . . ? C16 Lu1 N1 C12 122.7(3) . . . . ? C19 Lu1 N1 C12 51.3(3) . . . . ? C2 Lu1 N1 C12 -136.2(3) . . . . ? C4 Lu1 N1 C12 -90.1(3) . . . . ? C3 Lu1 N1 C12 -124.1(3) . . . . ? C21 Lu1 N1 Si1 121.54(16) . . . . ? C1 Lu1 N1 Si1 6.96(13) . . . . ? C5 Lu1 N1 Si1 36.32(14) . . . . ? C18 Lu1 N1 Si1 -102.95(16) . . . . ? C17 Lu1 N1 Si1 -94.55(17) . . . . ? C20 Lu1 N1 Si1 140.99(17) . . . . ? C16 Lu1 N1 Si1 -117.4(2) . . . . ? C19 Lu1 N1 Si1 171.19(16) . . . . ? C2 Lu1 N1 Si1 -16.27(15) . . . . ? C4 Lu1 N1 Si1 29.81(18) . . . . ? C3 Lu1 N1 Si1 -4.15(19) . . . . ? N1 Si1 C1 C5 -65.2(3) . . . . ? C11 Si1 C1 C5 178.2(3) . . . . ? C10 Si1 C1 C5 55.8(4) . . . . ? Lu1 Si1 C1 C5 -74.3(3) . . . . ? N1 Si1 C1 C2 88.9(3) . . . . ? C11 Si1 C1 C2 -27.8(4) . . . . ? C10 Si1 C1 C2 -150.1(3) . . . . ? Lu1 Si1 C1 C2 79.8(3) . . . . ? N1 Si1 C1 Lu1 9.13(17) . . . . ? C11 Si1 C1 Lu1 -107.5(2) . . . . ? C10 Si1 C1 Lu1 130.1(2) . . . . ? C21 Lu1 C1 C5 10.2(3) . . . . ? C18 Lu1 C1 C5 -165.6(2) . . . . ? C17 Lu1 C1 C5 -132.5(2) . . . . ? N1 Lu1 C1 C5 116.4(2) . . . . ? C20 Lu1 C1 C5 47.4(3) . . . . ? C16 Lu1 C1 C5 -104.3(3) . . . . ? C19 Lu1 C1 C5 86.9(3) . . . . ? C2 Lu1 C1 C5 -111.3(3) . . . . ? C4 Lu1 C1 C5 -37.5(2) . . . . ? C3 Lu1 C1 C5 -76.1(2) . . . . ? C21 Lu1 C1 C2 121.5(3) . . . . ? C5 Lu1 C1 C2 111.3(3) . . . . ? C18 Lu1 C1 C2 -54.2(3) . . . . ? C17 Lu1 C1 C2 -21.2(3) . . . . ? N1 Lu1 C1 C2 -132.3(3) . . . . ? C20 Lu1 C1 C2 158.7(2) . . . . ? C16 Lu1 C1 C2 7.0(3) . . . . ? C19 Lu1 C1 C2 -161.8(3) . . . . ? C4 Lu1 C1 C2 73.9(3) . . . . ? C3 Lu1 C1 C2 35.2(2) . . . . ? C21 Lu1 C1 Si1 -113.03(19) . . . . ? C5 Lu1 C1 Si1 -123.2(3) . . . . ? C18 Lu1 C1 Si1 71.25(18) . . . . ? C17 Lu1 C1 Si1 104.30(18) . . . . ? N1 Lu1 C1 Si1 -6.81(13) . . . . ? C20 Lu1 C1 Si1 -75.8(2) . . . . ? C16 Lu1 C1 Si1 132.47(19) . . . . ? C19 Lu1 C1 Si1 -36.3(3) . . . . ? C2 Lu1 C1 Si1 125.5(3) . . . . ? C4 Lu1 C1 Si1 -160.7(2) . . . . ? C3 Lu1 C1 Si1 160.7(2) . . . . ? C5 C1 C2 C3 -0.5(4) . . . . ? Si1 C1 C2 C3 -158.2(3) . . . . ? Lu1 C1 C2 C3 -69.4(3) . . . . ? C5 C1 C2 C6 -173.5(4) . . . . ? Si1 C1 C2 C6 28.9(6) . . . . ? Lu1 C1 C2 C6 117.7(4) . . . . ? C5 C1 C2 Lu1 68.8(2) . . . . ? Si1 C1 C2 Lu1 -88.8(3) . . . . ? C21 Lu1 C2 C3 33.7(3) . . . . ? C1 Lu1 C2 C3 115.3(4) . . . . ? C5 Lu1 C2 C3 75.8(3) . . . . ? C18 Lu1 C2 C3 -115.8(3) . . . . ? C17 Lu1 C2 C3 -84.9(3) . . . . ? N1 Lu1 C2 C3 158.3(3) . . . . ? C20 Lu1 C2 C3 69.0(4) . . . . ? C16 Lu1 C2 C3 -59.2(3) . . . . ? C19 Lu1 C2 C3 -153.0(7) . . . . ? C4 Lu1 C2 C3 35.3(2) . . . . ? C21 Lu1 C2 C1 -81.6(3) . . . . ? C5 Lu1 C2 C1 -39.5(2) . . . . ? C18 Lu1 C2 C1 128.8(3) . . . . ? C17 Lu1 C2 C1 159.8(3) . . . . ? N1 Lu1 C2 C1 43.0(2) . . . . ? C20 Lu1 C2 C1 -46.3(5) . . . . ? C16 Lu1 C2 C1 -174.5(3) . . . . ? C19 Lu1 C2 C1 91.7(8) . . . . ? C4 Lu1 C2 C1 -80.1(3) . . . . ? C3 Lu1 C2 C1 -115.3(4) . . . . ? C21 Lu1 C2 C6 156.9(3) . . . . ? C1 Lu1 C2 C6 -121.5(4) . . . . ? C5 Lu1 C2 C6 -161.0(4) . . . . ? C18 Lu1 C2 C6 7.4(3) . . . . ? C17 Lu1 C2 C6 38.3(3) . . . . ? N1 Lu1 C2 C6 -78.5(3) . . . . ? C20 Lu1 C2 C6 -167.8(4) . . . . ? C16 Lu1 C2 C6 64.0(4) . . . . ? C19 Lu1 C2 C6 -29.8(9) . . . . ? C4 Lu1 C2 C6 158.5(4) . . . . ? C3 Lu1 C2 C6 123.2(5) . . . . ? C1 C2 C3 C4 0.9(4) . . . . ? C6 C2 C3 C4 174.2(4) . . . . ? Lu1 C2 C3 C4 -62.5(3) . . . . ? C1 C2 C3 C7 -173.3(4) . . . . ? C6 C2 C3 C7 -0.1(7) . . . . ? Lu1 C2 C3 C7 123.3(4) . . . . ? C1 C2 C3 Lu1 63.5(3) . . . . ? C6 C2 C3 Lu1 -123.3(4) . . . . ? C21 Lu1 C3 C2 -154.7(3) . . . . ? C1 Lu1 C3 C2 -37.7(2) . . . . ? C5 Lu1 C3 C2 -80.1(3) . . . . ? C18 Lu1 C3 C2 65.8(3) . . . . ? C17 Lu1 C3 C2 89.0(3) . . . . ? N1 Lu1 C3 C2 -24.7(3) . . . . ? C20 Lu1 C3 C2 -148.2(3) . . . . ? C16 Lu1 C3 C2 120.3(3) . . . . ? C19 Lu1 C3 C2 167.9(3) . . . . ? C4 Lu1 C3 C2 -117.4(4) . . . . ? C21 Lu1 C3 C4 -37.3(3) . . . . ? C1 Lu1 C3 C4 79.6(3) . . . . ? C5 Lu1 C3 C4 37.3(2) . . . . ? C18 Lu1 C3 C4 -176.9(2) . . . . ? C17 Lu1 C3 C4 -153.6(3) . . . . ? N1 Lu1 C3 C4 92.7(2) . . . . ? C20 Lu1 C3 C4 -30.9(3) . . . . ? C16 Lu1 C3 C4 -122.3(3) . . . . ? C19 Lu1 C3 C4 -74.8(5) . . . . ? C2 Lu1 C3 C4 117.4(4) . . . . ? C21 Lu1 C3 C7 81.7(4) . . . . ? C1 Lu1 C3 C7 -161.3(5) . . . . ? C5 Lu1 C3 C7 156.4(5) . . . . ? C18 Lu1 C3 C7 -57.8(4) . . . . ? C17 Lu1 C3 C7 -34.5(4) . . . . ? N1 Lu1 C3 C7 -148.3(4) . . . . ? C20 Lu1 C3 C7 88.2(5) . . . . ? C16 Lu1 C3 C7 -3.2(4) . . . . ? C19 Lu1 C3 C7 44.3(7) . . . . ? C2 Lu1 C3 C7 -123.6(5) . . . . ? C4 Lu1 C3 C7 119.1(5) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? C7 C3 C4 C5 173.5(4) . . . . ? Lu1 C3 C4 C5 -63.3(3) . . . . ? C2 C3 C4 C8 -174.8(4) . . . . ? C7 C3 C4 C8 -0.3(6) . . . . ? Lu1 C3 C4 C8 122.9(4) . . . . ? C2 C3 C4 Lu1 62.3(3) . . . . ? C7 C3 C4 Lu1 -123.2(4) . . . . ? C21 Lu1 C4 C3 143.8(3) . . . . ? C1 Lu1 C4 C3 -76.2(3) . . . . ? C5 Lu1 C4 C3 -115.3(4) . . . . ? C18 Lu1 C4 C3 4.0(3) . . . . ? C17 Lu1 C4 C3 26.9(3) . . . . ? N1 Lu1 C4 C3 -102.9(2) . . . . ? C20 Lu1 C4 C3 158.1(2) . . . . ? C16 Lu1 C4 C3 57.4(3) . . . . ? C19 Lu1 C4 C3 147.1(2) . . . . ? C2 Lu1 C4 C3 -35.0(2) . . . . ? C21 Lu1 C4 C5 -100.9(3) . . . . ? C1 Lu1 C4 C5 39.1(2) . . . . ? C18 Lu1 C4 C5 119.3(3) . . . . ? C17 Lu1 C4 C5 142.2(3) . . . . ? N1 Lu1 C4 C5 12.4(3) . . . . ? C20 Lu1 C4 C5 -86.6(3) . . . . ? C16 Lu1 C4 C5 172.7(3) . . . . ? C19 Lu1 C4 C5 -97.6(3) . . . . ? C2 Lu1 C4 C5 80.3(3) . . . . ? C3 Lu1 C4 C5 115.3(4) . . . . ? C21 Lu1 C4 C8 19.0(4) . . . . ? C1 Lu1 C4 C8 159.0(4) . . . . ? C5 Lu1 C4 C8 119.9(5) . . . . ? C18 Lu1 C4 C8 -120.8(4) . . . . ? C17 Lu1 C4 C8 -97.9(4) . . . . ? N1 Lu1 C4 C8 132.3(3) . . . . ? C20 Lu1 C4 C8 33.3(4) . . . . ? C16 Lu1 C4 C8 -67.4(4) . . . . ? C19 Lu1 C4 C8 22.3(4) . . . . ? C2 Lu1 C4 C8 -159.8(4) . . . . ? C3 Lu1 C4 C8 -124.8(5) . . . . ? C3 C4 C5 C1 0.7(4) . . . . ? C8 C4 C5 C1 174.4(4) . . . . ? Lu1 C4 C5 C1 -68.2(3) . . . . ? C3 C4 C5 C9 -176.1(4) . . . . ? C8 C4 C5 C9 -2.4(6) . . . . ? Lu1 C4 C5 C9 115.0(4) . . . . ? C3 C4 C5 Lu1 68.9(3) . . . . ? C8 C4 C5 Lu1 -117.4(4) . . . . ? C2 C1 C5 C4 -0.1(4) . . . . ? Si1 C1 C5 C4 158.2(3) . . . . ? Lu1 C1 C5 C4 72.0(3) . . . . ? C2 C1 C5 C9 176.6(4) . . . . ? Si1 C1 C5 C9 -25.1(5) . . . . ? Lu1 C1 C5 C9 -111.4(4) . . . . ? C2 C1 C5 Lu1 -72.1(3) . . . . ? Si1 C1 C5 Lu1 86.3(3) . . . . ? C21 Lu1 C5 C4 76.1(3) . . . . ? C1 Lu1 C5 C4 -112.6(3) . . . . ? C18 Lu1 C5 C4 -91.7(3) . . . . ? C17 Lu1 C5 C4 -49.4(3) . . . . ? N1 Lu1 C5 C4 -168.7(3) . . . . ? C20 Lu1 C5 C4 103.2(3) . . . . ? C16 Lu1 C5 C4 -9.3(3) . . . . ? C19 Lu1 C5 C4 116.1(3) . . . . ? C2 Lu1 C5 C4 -74.1(3) . . . . ? C3 Lu1 C5 C4 -35.7(2) . . . . ? C21 Lu1 C5 C1 -171.3(2) . . . . ? C18 Lu1 C5 C1 21.0(3) . . . . ? C17 Lu1 C5 C1 63.2(3) . . . . ? N1 Lu1 C5 C1 -56.1(2) . . . . ? C20 Lu1 C5 C1 -144.2(2) . . . . ? C16 Lu1 C5 C1 103.3(3) . . . . ? C19 Lu1 C5 C1 -131.2(2) . . . . ? C2 Lu1 C5 C1 38.6(2) . . . . ? C4 Lu1 C5 C1 112.6(3) . . . . ? C3 Lu1 C5 C1 77.0(2) . . . . ? C21 Lu1 C5 C9 -46.9(3) . . . . ? C1 Lu1 C5 C9 124.4(4) . . . . ? C18 Lu1 C5 C9 145.4(3) . . . . ? C17 Lu1 C5 C9 -172.4(3) . . . . ? N1 Lu1 C5 C9 68.3(3) . . . . ? C20 Lu1 C5 C9 -19.8(3) . . . . ? C16 Lu1 C5 C9 -132.3(3) . . . . ? C19 Lu1 C5 C9 -6.8(4) . . . . ? C2 Lu1 C5 C9 162.9(3) . . . . ? C4 Lu1 C5 C9 -123.0(4) . . . . ? C3 Lu1 C5 C9 -158.7(4) . . . . ? C15 N1 C12 C13 -39.6(4) . . . . ? Si1 N1 C12 C13 88.8(4) . . . . ? Lu1 N1 C12 C13 -162.9(3) . . . . ? N1 C12 C13 C14 24.0(5) . . . . ? C12 C13 C14 C15 0.9(5) . . . . ? C12 N1 C15 C14 40.5(4) . . . . ? Si1 N1 C15 C14 -85.6(4) . . . . ? Lu1 N1 C15 C14 164.2(3) . . . . ? C13 C14 C15 N1 -25.9(5) . . . . ? C21 Lu1 C16 C17 171.5(3) . . . . ? C1 Lu1 C16 C17 -60.0(3) . . . . ? C5 Lu1 C16 C17 -102.8(3) . . . . ? C18 Lu1 C16 C17 25.5(3) . . . . ? N1 Lu1 C16 C17 42.6(4) . . . . ? C20 Lu1 C16 C17 141.6(3) . . . . ? C19 Lu1 C16 C17 113.8(3) . . . . ? C2 Lu1 C16 C17 -56.2(3) . . . . ? C4 Lu1 C16 C17 -107.7(3) . . . . ? C3 Lu1 C16 C17 -82.1(3) . . . . ? Lu1 C16 C17 C18 -56.0(4) . . . . ? C21 Lu1 C17 C16 -9.6(3) . . . . ? C1 Lu1 C17 C16 134.2(3) . . . . ? C5 Lu1 C17 C16 103.1(3) . . . . ? C18 Lu1 C17 C16 -136.1(4) . . . . ? N1 Lu1 C17 C16 -152.3(3) . . . . ? C20 Lu1 C17 C16 -45.7(3) . . . . ? C19 Lu1 C17 C16 -66.4(3) . . . . ? C2 Lu1 C17 C16 122.9(3) . . . . ? C4 Lu1 C17 C16 78.6(3) . . . . ? C3 Lu1 C17 C16 92.1(3) . . . . ? C21 Lu1 C17 C18 126.5(3) . . . . ? C1 Lu1 C17 C18 -89.8(3) . . . . ? C5 Lu1 C17 C18 -120.8(3) . . . . ? N1 Lu1 C17 C18 -16.2(3) . . . . ? C20 Lu1 C17 C18 90.3(3) . . . . ? C16 Lu1 C17 C18 136.1(4) . . . . ? C19 Lu1 C17 C18 69.7(3) . . . . ? C2 Lu1 C17 C18 -101.1(3) . . . . ? C4 Lu1 C17 C18 -145.3(3) . . . . ? C3 Lu1 C17 C18 -131.8(3) . . . . ? C16 C17 C18 Lu1 57.1(5) . . . . ? C21 Lu1 C18 C17 -74.2(3) . . . . ? C1 Lu1 C18 C17 100.8(3) . . . . ? C5 Lu1 C18 C17 89.0(3) . . . . ? N1 Lu1 C18 C17 165.5(3) . . . . ? C20 Lu1 C18 C17 -107.0(3) . . . . ? C16 Lu1 C18 C17 -25.0(3) . . . . ? C19 Lu1 C18 C17 -110.9(3) . . . . ? C2 Lu1 C18 C17 75.1(3) . . . . ? C4 Lu1 C18 C17 45.7(4) . . . . ? C3 Lu1 C18 C17 47.8(3) . . . . ? C21 Lu1 C19 C20 24.5(3) . . . . ? C1 Lu1 C19 C20 -73.3(4) . . . . ? C5 Lu1 C19 C20 -25.1(4) . . . . ? C18 Lu1 C19 C20 173.1(3) . . . . ? C17 Lu1 C19 C20 143.7(3) . . . . ? N1 Lu1 C19 C20 -100.5(3) . . . . ? C16 Lu1 C19 C20 115.5(3) . . . . ? C2 Lu1 C19 C20 -149.6(7) . . . . ? C4 Lu1 C19 C20 20.6(4) . . . . ? C3 Lu1 C19 C20 68.3(5) . . . . ? Lu1 C19 C20 C21 -52.6(4) . . . . ? C1 Lu1 C20 C21 -85.2(3) . . . . ? C5 Lu1 C20 C21 -60.8(3) . . . . ? C18 Lu1 C20 C21 130.2(3) . . . . ? C17 Lu1 C20 C21 94.7(3) . . . . ? N1 Lu1 C20 C21 -144.6(3) . . . . ? C16 Lu1 C20 C21 72.9(3) . . . . ? C19 Lu1 C20 C21 137.8(5) . . . . ? C2 Lu1 C20 C21 -55.2(5) . . . . ? C4 Lu1 C20 C21 -28.0(3) . . . . ? C3 Lu1 C20 C21 -12.0(4) . . . . ? C21 Lu1 C20 C19 -137.8(5) . . . . ? C1 Lu1 C20 C19 137.0(3) . . . . ? C5 Lu1 C20 C19 161.4(3) . . . . ? C18 Lu1 C20 C19 -7.6(3) . . . . ? C17 Lu1 C20 C19 -43.2(3) . . . . ? N1 Lu1 C20 C19 77.6(3) . . . . ? C16 Lu1 C20 C19 -64.9(3) . . . . ? C2 Lu1 C20 C19 167.0(3) . . . . ? C4 Lu1 C20 C19 -165.8(3) . . . . ? C3 Lu1 C20 C19 -149.8(3) . . . . ? C19 C20 C21 Lu1 54.8(4) . . . . ? C1 Lu1 C21 C20 116.8(3) . . . . ? C5 Lu1 C21 C20 122.3(3) . . . . ? C18 Lu1 C21 C20 -68.8(4) . . . . ? C17 Lu1 C21 C20 -103.6(3) . . . . ? N1 Lu1 C21 C20 39.6(3) . . . . ? C16 Lu1 C21 C20 -108.5(3) . . . . ? C19 Lu1 C21 C20 -24.0(3) . . . . ? C2 Lu1 C21 C20 154.6(3) . . . . ? C4 Lu1 C21 C20 153.4(3) . . . . ? C3 Lu1 C21 C20 171.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.509 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.106 _database_code_depnum_ccdc_archive 'CCDC 917596' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl2 #TrackingRef 'complexes 16 CIF.doc' #TrackingRef 'complexes 16 CIF.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H54 N3 Sc Si5' _chemical_formula_sum 'C23 H54 N3 Sc Si5' _chemical_formula_weight 558.10 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7456(16) _cell_length_b 10.7843(13) _cell_length_c 16.231(2) _cell_angle_alpha 108.818(6) _cell_angle_beta 93.485(8) _cell_angle_gamma 94.941(10) _cell_volume 1766.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4927 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 0.895 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14209 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6501 _reflns_number_gt 4245 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1361P)^2^+0.4044P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6501 _refine_ls_number_parameters 323 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1150 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.2485 _refine_ls_wR_factor_gt 0.2222 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.108 _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 Sc1 Sc 0.23408(7) 0.34931(8) 0.24815(5) 0.0563(3) Uani 1 1 d . A . Si1A Si 0.2723(5) 0.0469(6) 0.3363(4) 0.0697(7) Uiso 0.33 1 d PD A 1 Si1B Si 0.2308(5) 0.0398(5) 0.3333(3) 0.0697(7) Uiso 0.33 1 d PD A 2 Si1C Si 0.2880(5) 0.0426(5) 0.3120(3) 0.0697(7) Uiso 0.33 1 d PD A 3 Si2 Si -0.00462(14) 0.24075(16) 0.15576(11) 0.0882(5) Uani 1 1 d . . . H2 H 0.105(4) 0.172(5) 0.179(3) 0.089(15) Uiso 1 1 d . . . Si3 Si -0.01511(14) 0.53445(15) 0.24854(10) 0.0794(4) Uani 1 1 d . . . H3 H 0.086(4) 0.632(5) 0.288(3) 0.090(15) Uiso 1 1 d . . . Si4 Si 0.36187(13) 0.50224(15) 0.15847(9) 0.0752(4) Uani 1 1 d . A . H4 H 0.314(4) 0.560(4) 0.241(3) 0.075(13) Uiso 1 1 d . . . Si5A Si 0.3935(8) 0.1939(6) 0.0730(4) 0.0749(8) Uiso 0.33 1 d PD B 1 Si5B Si 0.3600(5) 0.2060(7) 0.0541(3) 0.0749(8) Uiso 0.33 1 d PD B 2 Si5C Si 0.4019(7) 0.2266(6) 0.0694(4) 0.0749(8) Uiso 0.33 1 d PD B 3 N1A N 0.2626(14) 0.0380(16) 0.4385(8) 0.0710(18) Uiso 0.33 1 d PD A 1 N1B N 0.2239(13) 0.0425(15) 0.4384(8) 0.0710(18) Uiso 0.33 1 d PD A 2 N1C N 0.2794(13) 0.0215(13) 0.4097(7) 0.0710(18) Uiso 0.33 1 d PD A 3 N2 N 0.0542(3) 0.3932(4) 0.2205(2) 0.0653(9) Uani 1 1 d . . . N3 N 0.3383(4) 0.3385(4) 0.1432(2) 0.0727(10) Uani 1 1 d D . . C1 C 0.2893(5) 0.2251(4) 0.3441(3) 0.0695(12) Uani 1 1 d . . . C2 C 0.2050(4) 0.3137(4) 0.3886(3) 0.0625(11) Uani 1 1 d . A . C3 C 0.2631(4) 0.4415(4) 0.4105(3) 0.0618(11) Uani 1 1 d . . . C4 C 0.3847(4) 0.4381(5) 0.3829(3) 0.0692(12) Uani 1 1 d . A . C5 C 0.4014(4) 0.3043(5) 0.3426(3) 0.0727(12) Uani 1 1 d . A . C6 C 0.0776(5) 0.2778(6) 0.4135(4) 0.0938(16) Uani 1 1 d . . . H6A H 0.0847 0.2802 0.4738 0.141 Uiso 1 1 calc R A . H6B H 0.0447 0.1898 0.3758 0.141 Uiso 1 1 calc R . . H6C H 0.0214 0.3404 0.4068 0.141 Uiso 1 1 calc R . . C7 C 0.2097(7) 0.5652(5) 0.4603(4) 0.0993(18) Uani 1 1 d . A . H7A H 0.1195 0.5469 0.4591 0.149 Uiso 1 1 calc R . . H7B H 0.2284 0.6324 0.4336 0.149 Uiso 1 1 calc R . . H7C H 0.2467 0.5963 0.5204 0.149 Uiso 1 1 calc R . . C8 C 0.4825(6) 0.5543(6) 0.4001(4) 0.103(2) Uani 1 1 d . . . H8A H 0.4426 0.6297 0.3960 0.155 Uiso 1 1 calc R A . H8B H 0.5432 0.5328 0.3572 0.155 Uiso 1 1 calc R . . H8C H 0.5249 0.5752 0.4582 0.155 Uiso 1 1 calc R . . C9 C 0.5235(5) 0.2576(9) 0.3086(4) 0.126(3) Uani 1 1 d . . . H9A H 0.5624 0.3185 0.2825 0.189 Uiso 1 1 calc R A . H9B H 0.5065 0.1706 0.2650 0.189 Uiso 1 1 calc R . . H9C H 0.5796 0.2537 0.3566 0.189 Uiso 1 1 calc R . . C10A C 0.1252(15) -0.044(2) 0.2631(12) 0.089(3) Uiso 0.33 1 d PD A 1 C10B C 0.0733(14) -0.0322(19) 0.2762(12) 0.089(3) Uiso 0.33 1 d PD A 2 C10C C 0.1484(16) -0.052(2) 0.2381(11) 0.089(3) Uiso 0.33 1 d PD A 3 C11A C 0.378(2) -0.053(2) 0.2555(13) 0.106(4) Uiso 0.33 1 d PD A 1 C11B C 0.3710(19) -0.058(2) 0.2954(15) 0.106(4) Uiso 0.33 1 d PD A 2 C11C C 0.4414(17) -0.025(2) 0.2866(15) 0.106(4) Uiso 0.33 1 d PD A 3 C12A C 0.3254(19) 0.129(2) 0.5191(12) 0.081(3) Uiso 0.33 1 d PD A 1 C12B C 0.2960(19) 0.136(2) 0.5169(12) 0.081(3) Uiso 0.33 1 d PD A 2 C12C C 0.3516(17) 0.1072(17) 0.4915(10) 0.081(3) Uiso 0.33 1 d PD A 3 C13A C 0.239(2) 0.089(3) 0.5791(17) 0.111(4) Uiso 0.33 1 d PD A 1 C13B C 0.272(2) 0.090(3) 0.5924(17) 0.111(4) Uiso 0.33 1 d PD A 2 C13C C 0.318(2) 0.073(2) 0.5706(13) 0.111(4) Uiso 0.33 1 d PD A 3 C14A C 0.179(2) -0.047(3) 0.5427(15) 0.123(4) Uiso 0.33 1 d PD A 1 C14B C 0.227(2) -0.053(3) 0.5505(15) 0.123(4) Uiso 0.33 1 d PD A 2 C14C C 0.266(2) -0.069(2) 0.5295(13) 0.123(4) Uiso 0.33 1 d PD A 3 C15A C 0.207(2) -0.086(2) 0.4471(15) 0.111(3) Uiso 0.33 1 d PD A 1 C15B C 0.165(2) -0.066(2) 0.4623(14) 0.111(3) Uiso 0.33 1 d PD A 2 C15C C 0.259(2) -0.1012(19) 0.4325(13) 0.111(3) Uiso 0.33 1 d PD A 3 C16 C -0.1376(6) 0.1613(7) 0.1948(6) 0.140(3) Uani 1 1 d . . . H16A H -0.1117 0.1540 0.2512 0.210 Uiso 1 1 calc R . . H16B H -0.1636 0.0740 0.1533 0.210 Uiso 1 1 calc R . . H16C H -0.2072 0.2141 0.2005 0.210 Uiso 1 1 calc R . . C17 C -0.0345(8) 0.2141(8) 0.0383(4) 0.139(3) Uani 1 1 d . . . H17A H -0.1168 0.2387 0.0266 0.209 Uiso 1 1 calc R . . H17B H -0.0313 0.1219 0.0055 0.209 Uiso 1 1 calc R . . H17C H 0.0288 0.2678 0.0207 0.209 Uiso 1 1 calc R . . C18 C -0.1452(7) 0.5303(9) 0.3197(5) 0.138(3) Uani 1 1 d . . . H18A H -0.2156 0.4695 0.2854 0.207 Uiso 1 1 calc R . . H18B H -0.1713 0.6178 0.3430 0.207 Uiso 1 1 calc R . . H18C H -0.1159 0.5015 0.3675 0.207 Uiso 1 1 calc R . . C19 C -0.0823(7) 0.5767(8) 0.1547(5) 0.126(2) Uani 1 1 d . . . H19A H -0.0161 0.5886 0.1190 0.188 Uiso 1 1 calc R . . H19B H -0.1210 0.6577 0.1760 0.188 Uiso 1 1 calc R . . H19C H -0.1449 0.5060 0.1200 0.188 Uiso 1 1 calc R . . C20 C 0.2765(7) 0.5604(7) 0.0790(4) 0.113(2) Uani 1 1 d . . . H20A H 0.3075 0.5246 0.0221 0.169 Uiso 1 1 calc R B . H20B H 0.2892 0.6559 0.0978 0.169 Uiso 1 1 calc R . . H20C H 0.1877 0.5314 0.0750 0.169 Uiso 1 1 calc R . . C21 C 0.5291(6) 0.5798(7) 0.1786(5) 0.116(2) Uani 1 1 d . . . H21A H 0.5778 0.5384 0.2127 0.174 Uiso 1 1 calc R B . H21B H 0.5320 0.6732 0.2105 0.174 Uiso 1 1 calc R . . H21C H 0.5638 0.5676 0.1231 0.174 Uiso 1 1 calc R . . C22A C 0.5540(17) 0.231(3) 0.0491(18) 0.116(4) Uiso 0.33 1 d PD B 1 C22B C 0.330(2) 0.0486(17) 0.0767(14) 0.116(4) Uiso 0.33 1 d PD B 2 C22C C 0.5637(17) 0.204(3) 0.0668(18) 0.116(4) Uiso 0.33 1 d PD B 3 C23A C 0.315(2) 0.164(2) -0.0410(11) 0.100(4) Uiso 0.33 1 d PD B 1 C23B C 0.289(2) 0.208(2) -0.0539(11) 0.100(4) Uiso 0.33 1 d PD B 2 C23C C 0.359(2) 0.204(2) -0.0482(10) 0.100(4) Uiso 0.33 1 d PD B 3 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 Sc1 0.0508(5) 0.0599(5) 0.0560(5) 0.0186(4) -0.0014(3) 0.0008(3) Si2 0.0685(9) 0.0782(10) 0.1019(11) 0.0172(8) -0.0240(8) -0.0060(7) Si3 0.0697(9) 0.0821(10) 0.0843(9) 0.0259(7) -0.0093(7) 0.0154(7) Si4 0.0750(9) 0.0894(10) 0.0661(8) 0.0336(7) 0.0097(6) 0.0022(7) N2 0.0507(19) 0.073(2) 0.069(2) 0.0222(18) -0.0061(16) 0.0023(17) N3 0.071(2) 0.084(3) 0.063(2) 0.0223(19) 0.0114(18) 0.011(2) C1 0.080(3) 0.058(3) 0.071(3) 0.023(2) -0.004(2) 0.011(2) C2 0.066(3) 0.063(3) 0.063(2) 0.030(2) 0.002(2) 0.000(2) C3 0.079(3) 0.054(2) 0.055(2) 0.0233(19) 0.000(2) 0.005(2) C4 0.071(3) 0.078(3) 0.057(2) 0.030(2) -0.016(2) -0.016(2) C5 0.061(3) 0.093(4) 0.065(3) 0.028(2) -0.003(2) 0.012(3) C6 0.085(4) 0.110(4) 0.098(4) 0.051(3) 0.017(3) -0.003(3) C7 0.144(5) 0.075(3) 0.077(3) 0.021(3) 0.000(3) 0.024(4) C8 0.100(4) 0.120(5) 0.084(4) 0.048(3) -0.029(3) -0.054(4) C9 0.072(4) 0.204(8) 0.114(5) 0.058(5) 0.009(3) 0.052(4) C16 0.078(4) 0.124(6) 0.209(9) 0.061(6) -0.023(5) -0.038(4) C17 0.145(7) 0.136(6) 0.099(5) 0.002(4) -0.050(4) 0.002(5) C18 0.119(6) 0.178(8) 0.137(6) 0.062(6) 0.038(5) 0.067(6) C19 0.121(5) 0.148(6) 0.134(6) 0.077(5) 0.001(4) 0.047(5) C20 0.138(6) 0.123(5) 0.085(4) 0.049(4) -0.003(4) 0.010(4) C21 0.096(4) 0.128(5) 0.123(5) 0.046(4) 0.020(4) -0.020(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 Sc1 N3 2.073(4) . ? Sc1 N2 2.086(3) . ? Sc1 C1 2.437(4) . ? Sc1 C2 2.464(4) . ? Sc1 C5 2.473(4) . ? Sc1 C3 2.488(4) . ? Sc1 C4 2.504(4) . ? Sc1 Si2 2.8427(16) . ? Sc1 Si4 2.8506(16) . ? Sc1 H2 2.19(5) . ? Sc1 H4 2.40(4) . ? Si1A N1A 1.700(12) . ? Si1A C1 1.877(8) . ? Si1A C10A 1.903(15) . ? Si1A C11A 1.913(15) . ? Si1B N1B 1.702(12) . ? Si1B C10B 1.856(14) . ? Si1B C11B 1.930(15) . ? Si1B C1 1.991(7) . ? Si1C N1C 1.681(11) . ? Si1C C10C 1.861(15) . ? Si1C C1 1.865(7) . ? Si1C C11C 1.875(15) . ? Si2 N2 1.683(4) . ? Si2 C17 1.838(7) . ? Si2 C16 1.852(7) . ? Si2 H2 1.53(5) . ? Si3 N2 1.694(4) . ? Si3 C19 1.849(6) . ? Si3 C18 1.873(7) . ? Si3 H3 1.41(5) . ? Si4 N3 1.696(4) . ? Si4 C20 1.838(6) . ? Si4 C21 1.878(6) . ? Si4 H4 1.43(4) . ? Si5A N3 1.782(7) . ? Si5A C22A 1.830(16) . ? Si5A C23A 1.901(15) . ? Si5B N3 1.718(6) . ? Si5B C22B 1.855(15) . ? Si5B C23B 1.875(15) . ? Si5C N3 1.633(7) . ? Si5C C22C 1.777(16) . ? Si5C C23C 1.867(15) . ? N1A C12A 1.445(16) . ? N1A C15A 1.472(17) . ? N1B C15B 1.455(16) . ? N1B C12B 1.471(15) . ? N1C C12C 1.476(15) . ? N1C C15C 1.486(16) . ? C1 C5 1.422(7) . ? C1 C2 1.427(6) . ? C2 C3 1.387(6) . ? C2 C6 1.505(7) . ? C3 C4 1.407(7) . ? C3 C7 1.502(7) . ? C4 C5 1.412(7) . ? C4 C8 1.504(6) . ? C5 C9 1.517(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C12A C13A 1.523(18) . ? C12B C13B 1.496(18) . ? C12C C13C 1.500(17) . ? C13A C14A 1.468(17) . ? C13B C14B 1.488(18) . ? C13C C14C 1.505(18) . ? C14A C15A 1.528(18) . ? C14B C15B 1.498(18) . ? C14C C15C 1.495(18) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? 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 N3 Sc1 N2 109.57(15) . . ? N3 Sc1 C1 118.61(16) . . ? N2 Sc1 C1 125.58(17) . . ? N3 Sc1 C2 150.99(15) . . ? N2 Sc1 C2 98.91(15) . . ? C1 Sc1 C2 33.85(15) . . ? N3 Sc1 C5 96.76(16) . . ? N2 Sc1 C5 153.66(16) . . ? C1 Sc1 C5 33.66(16) . . ? C2 Sc1 C5 55.02(15) . . ? N3 Sc1 C3 138.31(16) . . ? N2 Sc1 C3 102.26(15) . . ? C1 Sc1 C3 55.23(15) . . ? C2 Sc1 C3 32.53(14) . . ? C5 Sc1 C3 54.38(16) . . ? N3 Sc1 C4 106.48(16) . . ? N2 Sc1 C4 131.44(16) . . ? C1 Sc1 C4 55.56(15) . . ? C2 Sc1 C4 54.60(15) . . ? C5 Sc1 C4 32.94(15) . . ? C3 Sc1 C4 32.73(15) . . ? N3 Sc1 Si2 99.35(12) . . ? N2 Sc1 Si2 35.97(11) . . ? C1 Sc1 Si2 109.27(13) . . ? C2 Sc1 Si2 100.55(11) . . ? C5 Sc1 Si2 141.77(14) . . ? C3 Sc1 Si2 122.03(12) . . ? C4 Sc1 Si2 154.04(12) . . ? N3 Sc1 Si4 36.13(11) . . ? N2 Sc1 Si4 96.52(11) . . ? C1 Sc1 Si4 137.49(13) . . ? C2 Sc1 Si4 147.15(11) . . ? C5 Sc1 Si4 104.57(13) . . ? C3 Sc1 Si4 115.54(11) . . ? C4 Sc1 Si4 93.82(11) . . ? Si2 Sc1 Si4 108.88(5) . . ? N3 Sc1 H2 95.1(12) . . ? N2 Sc1 H2 67.5(12) . . ? C1 Sc1 H2 83.9(12) . . ? C2 Sc1 H2 90.6(12) . . ? C5 Sc1 H2 112.0(12) . . ? C3 Sc1 H2 122.1(12) . . ? C4 Sc1 H2 139.3(12) . . ? Si2 Sc1 H2 32.3(12) . . ? Si4 Sc1 H2 122.2(12) . . ? N3 Sc1 H4 66.0(10) . . ? N2 Sc1 H4 88.1(10) . . ? C1 Sc1 H4 133.1(10) . . ? C2 Sc1 H4 121.9(10) . . ? C5 Sc1 H4 102.3(10) . . ? C3 Sc1 H4 89.5(10) . . ? C4 Sc1 H4 77.9(10) . . ? Si2 Sc1 H4 116.0(10) . . ? Si4 Sc1 H4 30.1(10) . . ? H2 Sc1 H4 142.8(16) . . ? N1A Si1A C1 108.6(7) . . ? N1A Si1A C10A 109.8(9) . . ? C1 Si1A C10A 110.3(8) . . ? N1A Si1A C11A 123.1(9) . . ? C1 Si1A C11A 112.0(8) . . ? C10A Si1A C11A 91.6(10) . . ? N1B Si1B C10B 106.0(8) . . ? N1B Si1B C11B 103.6(8) . . ? C10B Si1B C11B 117.6(10) . . ? N1B Si1B C1 104.4(6) . . ? C10B Si1B C1 118.2(7) . . ? C11B Si1B C1 105.2(8) . . ? N1C Si1C C10C 108.5(8) . . ? N1C Si1C C1 100.6(5) . . ? C10C Si1C C1 114.2(8) . . ? N1C Si1C C11C 97.9(9) . . ? C10C Si1C C11C 115.8(10) . . ? C1 Si1C C11C 116.7(8) . . ? N2 Si2 C17 117.2(3) . . ? N2 Si2 C16 116.2(3) . . ? C17 Si2 C16 110.4(4) . . ? N2 Si2 Sc1 46.69(12) . . ? C17 Si2 Sc1 121.6(3) . . ? C16 Si2 Sc1 127.1(3) . . ? N2 Si2 H2 95.3(18) . . ? C17 Si2 H2 114.1(18) . . ? C16 Si2 H2 101.7(18) . . ? Sc1 Si2 H2 49.7(18) . . ? N2 Si3 C19 114.4(3) . . ? N2 Si3 C18 112.4(3) . . ? C19 Si3 C18 106.6(3) . . ? N2 Si3 H3 103.1(18) . . ? C19 Si3 H3 105.8(19) . . ? C18 Si3 H3 114.5(19) . . ? N3 Si4 C20 116.7(3) . . ? N3 Si4 C21 116.8(3) . . ? C20 Si4 C21 109.2(3) . . ? N3 Si4 Sc1 46.10(13) . . ? C20 Si4 Sc1 121.2(2) . . ? C21 Si4 Sc1 128.9(2) . . ? N3 Si4 H4 102.8(17) . . ? C20 Si4 H4 107.0(17) . . ? C21 Si4 H4 102.6(18) . . ? Sc1 Si4 H4 57.2(17) . . ? N3 Si5A C22A 110.4(10) . . ? N3 Si5A C23A 106.6(8) . . ? C22A Si5A C23A 96.7(12) . . ? N3 Si5B C22B 111.4(8) . . ? N3 Si5B C23B 115.7(7) . . ? C22B Si5B C23B 115.9(10) . . ? N3 Si5C C22C 126.9(11) . . ? N3 Si5C C23C 118.2(9) . . ? C22C Si5C C23C 100.2(11) . . ? C12A N1A C15A 113.5(16) . . ? C12A N1A Si1A 126.9(14) . . ? C15A N1A Si1A 118.4(13) . . ? C15B N1B C12B 108.0(14) . . ? C15B N1B Si1B 123.8(12) . . ? C12B N1B Si1B 127.0(12) . . ? C12C N1C C15C 98.8(12) . . ? C12C N1C Si1C 124.4(10) . . ? C15C N1C Si1C 130.4(12) . . ? Si2 N2 Si3 129.3(2) . . ? Si2 N2 Sc1 97.33(18) . . ? Si3 N2 Sc1 133.3(2) . . ? Si5C N3 Si4 123.9(3) . . ? Si5C N3 Si5B 16.8(3) . . ? Si4 N3 Si5B 129.9(3) . . ? Si5C N3 Si5A 11.8(3) . . ? Si4 N3 Si5A 135.6(3) . . ? Si5B N3 Si5A 16.7(3) . . ? Si5C N3 Sc1 138.0(3) . . ? Si4 N3 Sc1 97.77(17) . . ? Si5B N3 Sc1 130.5(3) . . ? Si5A N3 Sc1 126.2(3) . . ? C5 C1 C2 106.3(4) . . ? C5 C1 Si1C 119.7(4) . . ? C2 C1 Si1C 132.7(4) . . ? C5 C1 Si1A 127.3(4) . . ? C2 C1 Si1A 121.8(4) . . ? Si1C C1 Si1A 13.2(3) . . ? C5 C1 Si1B 139.8(4) . . ? C2 C1 Si1B 111.4(4) . . ? Si1C C1 Si1B 21.39(18) . . ? Si1A C1 Si1B 12.7(2) . . ? C5 C1 Sc1 74.5(2) . . ? C2 C1 Sc1 74.1(2) . . ? Si1C C1 Sc1 126.4(3) . . ? Si1A C1 Sc1 135.8(3) . . ? Si1B C1 Sc1 129.0(3) . . ? C3 C2 C1 108.4(4) . . ? C3 C2 C6 124.5(5) . . ? C1 C2 C6 127.0(4) . . ? C3 C2 Sc1 74.7(2) . . ? C1 C2 Sc1 72.1(2) . . ? C6 C2 Sc1 122.2(3) . . ? C2 C3 C4 109.3(4) . . ? C2 C3 C7 126.3(5) . . ? C4 C3 C7 124.3(5) . . ? C2 C3 Sc1 72.8(2) . . ? C4 C3 Sc1 74.3(2) . . ? C7 C3 Sc1 121.9(3) . . ? C3 C4 C5 107.1(4) . . ? C3 C4 C8 126.4(5) . . ? C5 C4 C8 126.3(5) . . ? C3 C4 Sc1 73.0(2) . . ? C5 C4 Sc1 72.3(2) . . ? C8 C4 Sc1 124.1(3) . . ? C4 C5 C1 108.8(4) . . ? C4 C5 C9 123.7(5) . . ? C1 C5 C9 127.4(5) . . ? C4 C5 Sc1 74.7(2) . . ? C1 C5 Sc1 71.8(2) . . ? C9 C5 Sc1 122.1(3) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1A C12A C13A 96.0(17) . . ? N1B C12B C13B 107.9(17) . . ? N1C C12C C13C 113.4(15) . . ? C14A C13A C12A 114(2) . . ? C14B C13B C12B 104(2) . . ? C12C C13C C14C 101.1(17) . . ? C13A C14A C15A 103(2) . . ? C13B C14B C15B 106(2) . . ? C15C C14C C13C 107.6(19) . . ? N1A C15A C14A 103.6(17) . . ? N1B C15B C14B 106.1(18) . . ? N1C C15C C14C 110.5(17) . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si4 C20 H20A 109.5 . . ? Si4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si4 C21 H21A 109.5 . . ? Si4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Sc1 Si2 N2 -110.5(2) . . . . ? C1 Sc1 Si2 N2 124.6(2) . . . . ? C2 Sc1 Si2 N2 90.7(2) . . . . ? C5 Sc1 Si2 N2 135.8(3) . . . . ? C3 Sc1 Si2 N2 64.2(2) . . . . ? C4 Sc1 Si2 N2 75.2(3) . . . . ? Si4 Sc1 Si2 N2 -74.53(19) . . . . ? N3 Sc1 Si2 C17 -11.4(3) . . . . ? N2 Sc1 Si2 C17 99.1(4) . . . . ? C1 Sc1 Si2 C17 -136.3(3) . . . . ? C2 Sc1 Si2 C17 -170.2(3) . . . . ? C5 Sc1 Si2 C17 -125.1(4) . . . . ? C3 Sc1 Si2 C17 163.3(3) . . . . ? C4 Sc1 Si2 C17 174.3(4) . . . . ? Si4 Sc1 Si2 C17 24.6(3) . . . . ? N3 Sc1 Si2 C16 156.8(4) . . . . ? N2 Sc1 Si2 C16 -92.7(4) . . . . ? C1 Sc1 Si2 C16 31.9(4) . . . . ? C2 Sc1 Si2 C16 -2.0(4) . . . . ? C5 Sc1 Si2 C16 43.1(4) . . . . ? C3 Sc1 Si2 C16 -28.5(4) . . . . ? C4 Sc1 Si2 C16 -17.5(5) . . . . ? Si4 Sc1 Si2 C16 -167.2(3) . . . . ? N2 Sc1 Si4 N3 -114.5(2) . . . . ? C1 Sc1 Si4 N3 73.0(3) . . . . ? C2 Sc1 Si4 N3 127.8(3) . . . . ? C5 Sc1 Si4 N3 81.4(2) . . . . ? C3 Sc1 Si4 N3 138.5(2) . . . . ? C4 Sc1 Si4 N3 113.0(2) . . . . ? Si2 Sc1 Si4 N3 -79.80(18) . . . . ? N3 Sc1 Si4 C20 98.3(3) . . . . ? N2 Sc1 Si4 C20 -16.2(3) . . . . ? C1 Sc1 Si4 C20 171.3(3) . . . . ? C2 Sc1 Si4 C20 -133.9(3) . . . . ? C5 Sc1 Si4 C20 179.7(3) . . . . ? C3 Sc1 Si4 C20 -123.1(3) . . . . ? C4 Sc1 Si4 C20 -148.7(3) . . . . ? Si2 Sc1 Si4 C20 18.5(3) . . . . ? N3 Sc1 Si4 C21 -91.5(4) . . . . ? N2 Sc1 Si4 C21 154.0(3) . . . . ? C1 Sc1 Si4 C21 -18.5(4) . . . . ? C2 Sc1 Si4 C21 36.3(4) . . . . ? C5 Sc1 Si4 C21 -10.1(3) . . . . ? C3 Sc1 Si4 C21 47.0(3) . . . . ? C4 Sc1 Si4 C21 21.5(3) . . . . ? Si2 Sc1 Si4 C21 -171.3(3) . . . . ? C1 Si1A N1A C12A -34.1(16) . . . . ? C10A Si1A N1A C12A -154.7(16) . . . . ? C11A Si1A N1A C12A 99.6(18) . . . . ? C1 Si1A N1A C15A 159.7(13) . . . . ? C10A Si1A N1A C15A 39.1(16) . . . . ? C11A Si1A N1A C15A -66.6(18) . . . . ? C10B Si1B N1B C15B 43.2(17) . . . . ? C11B Si1B N1B C15B -81.2(17) . . . . ? C1 Si1B N1B C15B 168.8(14) . . . . ? C10B Si1B N1B C12B -150.8(16) . . . . ? C11B Si1B N1B C12B 84.7(17) . . . . ? C1 Si1B N1B C12B -25.2(17) . . . . ? C10C Si1C N1C C12C -162.5(14) . . . . ? C1 Si1C N1C C12C -42.3(14) . . . . ? C11C Si1C N1C C12C 76.9(15) . . . . ? C10C Si1C N1C C15C 51.5(19) . . . . ? C1 Si1C N1C C15C 171.7(16) . . . . ? C11C Si1C N1C C15C -69.1(18) . . . . ? C17 Si2 N2 Si3 69.1(4) . . . . ? C16 Si2 N2 Si3 -64.5(4) . . . . ? Sc1 Si2 N2 Si3 178.1(4) . . . . ? C17 Si2 N2 Sc1 -108.9(3) . . . . ? C16 Si2 N2 Sc1 117.5(3) . . . . ? C19 Si3 N2 Si2 -54.0(4) . . . . ? C18 Si3 N2 Si2 67.7(4) . . . . ? C19 Si3 N2 Sc1 123.4(4) . . . . ? C18 Si3 N2 Sc1 -114.9(4) . . . . ? N3 Sc1 N2 Si2 78.7(2) . . . . ? C1 Sc1 N2 Si2 -72.9(2) . . . . ? C2 Sc1 N2 Si2 -95.71(19) . . . . ? C5 Sc1 N2 Si2 -103.4(4) . . . . ? C3 Sc1 N2 Si2 -128.65(17) . . . . ? C4 Sc1 N2 Si2 -145.64(18) . . . . ? Si4 Sc1 N2 Si2 113.38(16) . . . . ? N3 Sc1 N2 Si3 -99.3(3) . . . . ? C1 Sc1 N2 Si3 109.2(3) . . . . ? C2 Sc1 N2 Si3 86.3(3) . . . . ? C5 Sc1 N2 Si3 78.7(5) . . . . ? C3 Sc1 N2 Si3 53.4(3) . . . . ? C4 Sc1 N2 Si3 36.4(4) . . . . ? Si2 Sc1 N2 Si3 -178.0(4) . . . . ? Si4 Sc1 N2 Si3 -64.6(3) . . . . ? C22C Si5C N3 Si4 67.2(11) . . . . ? C23C Si5C N3 Si4 -63.6(10) . . . . ? C22C Si5C N3 Si5B -176(2) . . . . ? C23C Si5C N3 Si5B 53.0(16) . . . . ? C22C Si5C N3 Si5A -107(3) . . . . ? C23C Si5C N3 Si5A 122(3) . . . . ? C22C Si5C N3 Sc1 -104.5(11) . . . . ? C23C Si5C N3 Sc1 124.6(9) . . . . ? C20 Si4 N3 Si5C 76.8(5) . . . . ? C21 Si4 N3 Si5C -55.0(5) . . . . ? Sc1 Si4 N3 Si5C -174.5(5) . . . . ? C20 Si4 N3 Si5B 57.1(5) . . . . ? C21 Si4 N3 Si5B -74.7(4) . . . . ? Sc1 Si4 N3 Si5B 165.8(5) . . . . ? C20 Si4 N3 Si5A 78.5(6) . . . . ? C21 Si4 N3 Si5A -53.3(6) . . . . ? Sc1 Si4 N3 Si5A -172.7(6) . . . . ? C20 Si4 N3 Sc1 -108.8(3) . . . . ? C21 Si4 N3 Sc1 119.4(3) . . . . ? C22B Si5B N3 Si5C 100.5(16) . . . . ? C23B Si5B N3 Si5C -124.3(18) . . . . ? C22B Si5B N3 Si4 175.8(7) . . . . ? C23B Si5B N3 Si4 -49.0(10) . . . . ? C22B Si5B N3 Si5A 58.9(15) . . . . ? C23B Si5B N3 Si5A -166.0(18) . . . . ? C22B Si5B N3 Sc1 -22.8(9) . . . . ? C23B Si5B N3 Sc1 112.4(9) . . . . ? C22A Si5A N3 Si5C 40(2) . . . . ? C23A Si5A N3 Si5C -64(2) . . . . ? C22A Si5A N3 Si4 32.3(10) . . . . ? C23A Si5A N3 Si4 -71.6(10) . . . . ? C22A Si5A N3 Si5B 110.1(15) . . . . ? C23A Si5A N3 Si5B 6.1(14) . . . . ? C22A Si5A N3 Sc1 -138.7(8) . . . . ? C23A Si5A N3 Sc1 117.4(8) . . . . ? N2 Sc1 N3 Si5C -113.3(5) . . . . ? C1 Sc1 N3 Si5C 40.5(6) . . . . ? C2 Sc1 N3 Si5C 55.2(7) . . . . ? C5 Sc1 N3 Si5C 67.6(5) . . . . ? C3 Sc1 N3 Si5C 109.1(5) . . . . ? C4 Sc1 N3 Si5C 99.8(5) . . . . ? Si2 Sc1 N3 Si5C -77.6(5) . . . . ? Si4 Sc1 N3 Si5C 173.1(6) . . . . ? N2 Sc1 N3 Si4 73.6(2) . . . . ? C1 Sc1 N3 Si4 -132.61(18) . . . . ? C2 Sc1 N3 Si4 -117.9(3) . . . . ? C5 Sc1 N3 Si4 -105.50(19) . . . . ? C3 Sc1 N3 Si4 -64.0(3) . . . . ? C4 Sc1 N3 Si4 -73.3(2) . . . . ? Si2 Sc1 N3 Si4 109.30(15) . . . . ? N2 Sc1 N3 Si5B -92.1(4) . . . . ? C1 Sc1 N3 Si5B 61.7(4) . . . . ? C2 Sc1 N3 Si5B 76.4(5) . . . . ? C5 Sc1 N3 Si5B 88.8(4) . . . . ? C3 Sc1 N3 Si5B 130.3(3) . . . . ? C4 Sc1 N3 Si5B 121.0(4) . . . . ? Si2 Sc1 N3 Si5B -56.4(4) . . . . ? Si4 Sc1 N3 Si5B -165.7(5) . . . . ? N2 Sc1 N3 Si5A -112.7(4) . . . . ? C1 Sc1 N3 Si5A 41.1(4) . . . . ? C2 Sc1 N3 Si5A 55.8(6) . . . . ? C5 Sc1 N3 Si5A 68.2(4) . . . . ? C3 Sc1 N3 Si5A 109.7(4) . . . . ? C4 Sc1 N3 Si5A 100.4(4) . . . . ? Si2 Sc1 N3 Si5A -77.0(4) . . . . ? Si4 Sc1 N3 Si5A 173.7(5) . . . . ? N1C Si1C C1 C5 108.6(6) . . . . ? C10C Si1C C1 C5 -135.3(8) . . . . ? C11C Si1C C1 C5 4.1(10) . . . . ? N1C Si1C C1 C2 -56.5(7) . . . . ? C10C Si1C C1 C2 59.5(8) . . . . ? C11C Si1C C1 C2 -161.0(9) . . . . ? N1C Si1C C1 Si1A -20.0(13) . . . . ? C10C Si1C C1 Si1A 96.0(15) . . . . ? C11C Si1C C1 Si1A -124.5(17) . . . . ? N1C Si1C C1 Si1B -54.0(7) . . . . ? C10C Si1C C1 Si1B 62.0(9) . . . . ? C11C Si1C C1 Si1B -158.5(11) . . . . ? N1C Si1C C1 Sc1 -159.1(6) . . . . ? C10C Si1C C1 Sc1 -43.1(8) . . . . ? C11C Si1C C1 Sc1 96.4(9) . . . . ? N1A Si1A C1 C5 100.8(7) . . . . ? C10A Si1A C1 C5 -138.8(7) . . . . ? C11A Si1A C1 C5 -38.4(10) . . . . ? N1A Si1A C1 C2 -51.6(7) . . . . ? C10A Si1A C1 C2 68.7(7) . . . . ? C11A Si1A C1 C2 169.2(8) . . . . ? N1A Si1A C1 Si1C 159.3(17) . . . . ? C10A Si1A C1 Si1C -80.3(14) . . . . ? C11A Si1A C1 Si1C 20.1(14) . . . . ? N1A Si1A C1 Si1B -88.7(14) . . . . ? C10A Si1A C1 Si1B 31.7(13) . . . . ? C11A Si1A C1 Si1B 132.1(17) . . . . ? N1A Si1A C1 Sc1 -151.6(6) . . . . ? C10A Si1A C1 Sc1 -31.3(8) . . . . ? C11A Si1A C1 Sc1 69.2(9) . . . . ? N1B Si1B C1 C5 99.1(8) . . . . ? C10B Si1B C1 C5 -143.5(8) . . . . ? C11B Si1B C1 C5 -9.7(10) . . . . ? N1B Si1B C1 C2 -59.3(6) . . . . ? C10B Si1B C1 C2 58.2(8) . . . . ? C11B Si1B C1 C2 -168.1(8) . . . . ? N1B Si1B C1 Si1C 122.8(8) . . . . ? C10B Si1B C1 Si1C -119.8(10) . . . . ? C11B Si1B C1 Si1C 14.0(8) . . . . ? N1B Si1B C1 Si1A 87.4(14) . . . . ? C10B Si1B C1 Si1A -155.2(17) . . . . ? C11B Si1B C1 Si1A -21.4(13) . . . . ? N1B Si1B C1 Sc1 -145.7(6) . . . . ? C10B Si1B C1 Sc1 -28.2(9) . . . . ? C11B Si1B C1 Sc1 105.5(8) . . . . ? N3 Sc1 C1 C5 54.7(3) . . . . ? N2 Sc1 C1 C5 -156.0(3) . . . . ? C2 Sc1 C1 C5 -112.5(4) . . . . ? C3 Sc1 C1 C5 -76.3(3) . . . . ? C4 Sc1 C1 C5 -36.3(3) . . . . ? Si2 Sc1 C1 C5 167.5(3) . . . . ? Si4 Sc1 C1 C5 14.8(4) . . . . ? N3 Sc1 C1 C2 167.2(3) . . . . ? N2 Sc1 C1 C2 -43.5(3) . . . . ? C5 Sc1 C1 C2 112.5(4) . . . . ? C3 Sc1 C1 C2 36.2(3) . . . . ? C4 Sc1 C1 C2 76.2(3) . . . . ? Si2 Sc1 C1 C2 -80.0(3) . . . . ? Si4 Sc1 C1 C2 127.3(2) . . . . ? N3 Sc1 C1 Si1C -61.0(4) . . . . ? N2 Sc1 C1 Si1C 88.3(4) . . . . ? C2 Sc1 C1 Si1C 131.8(5) . . . . ? C5 Sc1 C1 Si1C -115.7(5) . . . . ? C3 Sc1 C1 Si1C 168.0(4) . . . . ? C4 Sc1 C1 Si1C -152.0(4) . . . . ? Si2 Sc1 C1 Si1C 51.8(4) . . . . ? Si4 Sc1 C1 Si1C -100.9(4) . . . . ? N3 Sc1 C1 Si1A -73.3(5) . . . . ? N2 Sc1 C1 Si1A 75.9(5) . . . . ? C2 Sc1 C1 Si1A 119.5(6) . . . . ? C5 Sc1 C1 Si1A -128.1(6) . . . . ? C3 Sc1 C1 Si1A 155.6(5) . . . . ? C4 Sc1 C1 Si1A -164.4(5) . . . . ? Si2 Sc1 C1 Si1A 39.4(4) . . . . ? Si4 Sc1 C1 Si1A -113.3(4) . . . . ? N3 Sc1 C1 Si1B -87.9(4) . . . . ? N2 Sc1 C1 Si1B 61.3(4) . . . . ? C2 Sc1 C1 Si1B 104.9(5) . . . . ? C5 Sc1 C1 Si1B -142.7(5) . . . . ? C3 Sc1 C1 Si1B 141.0(4) . . . . ? C4 Sc1 C1 Si1B -178.9(4) . . . . ? Si2 Sc1 C1 Si1B 24.8(4) . . . . ? Si4 Sc1 C1 Si1B -127.9(3) . . . . ? C5 C1 C2 C3 1.8(5) . . . . ? Si1C C1 C2 C3 168.4(4) . . . . ? Si1A C1 C2 C3 159.2(4) . . . . ? Si1B C1 C2 C3 167.4(3) . . . . ? Sc1 C1 C2 C3 -66.4(3) . . . . ? C5 C1 C2 C6 -174.7(4) . . . . ? Si1C C1 C2 C6 -8.1(7) . . . . ? Si1A C1 C2 C6 -17.3(7) . . . . ? Si1B C1 C2 C6 -9.1(6) . . . . ? Sc1 C1 C2 C6 117.2(4) . . . . ? C5 C1 C2 Sc1 68.1(3) . . . . ? Si1C C1 C2 Sc1 -125.3(5) . . . . ? Si1A C1 C2 Sc1 -134.4(4) . . . . ? Si1B C1 C2 Sc1 -126.3(3) . . . . ? N3 Sc1 C2 C3 92.1(4) . . . . ? N2 Sc1 C2 C3 -98.9(3) . . . . ? C1 Sc1 C2 C3 115.7(4) . . . . ? C5 Sc1 C2 C3 77.0(3) . . . . ? C4 Sc1 C2 C3 36.4(3) . . . . ? Si2 Sc1 C2 C3 -135.3(3) . . . . ? Si4 Sc1 C2 C3 18.2(4) . . . . ? N3 Sc1 C2 C1 -23.6(5) . . . . ? N2 Sc1 C2 C1 145.4(3) . . . . ? C5 Sc1 C2 C1 -38.7(3) . . . . ? C3 Sc1 C2 C1 -115.7(4) . . . . ? C4 Sc1 C2 C1 -79.3(3) . . . . ? Si2 Sc1 C2 C1 109.0(3) . . . . ? Si4 Sc1 C2 C1 -97.5(3) . . . . ? N3 Sc1 C2 C6 -146.5(4) . . . . ? N2 Sc1 C2 C6 22.5(4) . . . . ? C1 Sc1 C2 C6 -122.9(5) . . . . ? C5 Sc1 C2 C6 -161.6(5) . . . . ? C3 Sc1 C2 C6 121.4(5) . . . . ? C4 Sc1 C2 C6 157.8(5) . . . . ? Si2 Sc1 C2 C6 -13.9(4) . . . . ? Si4 Sc1 C2 C6 139.6(3) . . . . ? C1 C2 C3 C4 -1.2(5) . . . . ? C6 C2 C3 C4 175.4(4) . . . . ? Sc1 C2 C3 C4 -65.9(3) . . . . ? C1 C2 C3 C7 -178.0(4) . . . . ? C6 C2 C3 C7 -1.5(7) . . . . ? Sc1 C2 C3 C7 117.3(4) . . . . ? C1 C2 C3 Sc1 64.7(3) . . . . ? C6 C2 C3 Sc1 -118.8(4) . . . . ? N3 Sc1 C3 C2 -133.2(3) . . . . ? N2 Sc1 C3 C2 87.4(3) . . . . ? C1 Sc1 C3 C2 -37.7(3) . . . . ? C5 Sc1 C3 C2 -79.2(3) . . . . ? C4 Sc1 C3 C2 -116.5(4) . . . . ? Si2 Sc1 C3 C2 54.6(3) . . . . ? Si4 Sc1 C3 C2 -169.2(2) . . . . ? N3 Sc1 C3 C4 -16.7(4) . . . . ? N2 Sc1 C3 C4 -156.1(3) . . . . ? C1 Sc1 C3 C4 78.9(3) . . . . ? C2 Sc1 C3 C4 116.5(4) . . . . ? C5 Sc1 C3 C4 37.4(3) . . . . ? Si2 Sc1 C3 C4 171.1(2) . . . . ? Si4 Sc1 C3 C4 -52.7(3) . . . . ? N3 Sc1 C3 C7 104.3(5) . . . . ? N2 Sc1 C3 C7 -35.1(5) . . . . ? C1 Sc1 C3 C7 -160.2(5) . . . . ? C2 Sc1 C3 C7 -122.5(6) . . . . ? C5 Sc1 C3 C7 158.3(5) . . . . ? C4 Sc1 C3 C7 121.0(5) . . . . ? Si2 Sc1 C3 C7 -67.9(4) . . . . ? Si4 Sc1 C3 C7 68.3(4) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C7 C3 C4 C5 177.1(4) . . . . ? Sc1 C3 C4 C5 -64.8(3) . . . . ? C2 C3 C4 C8 -174.9(4) . . . . ? C7 C3 C4 C8 2.1(7) . . . . ? Sc1 C3 C4 C8 120.2(4) . . . . ? C2 C3 C4 Sc1 64.9(3) . . . . ? C7 C3 C4 Sc1 -118.2(4) . . . . ? N3 Sc1 C4 C3 168.5(3) . . . . ? N2 Sc1 C4 C3 31.9(3) . . . . ? C1 Sc1 C4 C3 -77.7(3) . . . . ? C2 Sc1 C4 C3 -36.2(2) . . . . ? C5 Sc1 C4 C3 -114.8(4) . . . . ? Si2 Sc1 C4 C3 -17.4(5) . . . . ? Si4 Sc1 C4 C3 134.0(2) . . . . ? N3 Sc1 C4 C5 -76.7(3) . . . . ? N2 Sc1 C4 C5 146.7(3) . . . . ? C1 Sc1 C4 C5 37.1(3) . . . . ? C2 Sc1 C4 C5 78.7(3) . . . . ? C3 Sc1 C4 C5 114.8(4) . . . . ? Si2 Sc1 C4 C5 97.5(4) . . . . ? Si4 Sc1 C4 C5 -111.1(3) . . . . ? N3 Sc1 C4 C8 45.7(5) . . . . ? N2 Sc1 C4 C8 -91.0(5) . . . . ? C1 Sc1 C4 C8 159.4(6) . . . . ? C2 Sc1 C4 C8 -159.0(6) . . . . ? C5 Sc1 C4 C8 122.3(6) . . . . ? C3 Sc1 C4 C8 -122.8(6) . . . . ? Si2 Sc1 C4 C8 -140.2(4) . . . . ? Si4 Sc1 C4 C8 11.2(5) . . . . ? C3 C4 C5 C1 1.0(5) . . . . ? C8 C4 C5 C1 176.0(4) . . . . ? Sc1 C4 C5 C1 -64.2(3) . . . . ? C3 C4 C5 C9 -176.1(4) . . . . ? C8 C4 C5 C9 -1.1(7) . . . . ? Sc1 C4 C5 C9 118.7(5) . . . . ? C3 C4 C5 Sc1 65.2(3) . . . . ? C8 C4 C5 Sc1 -119.8(4) . . . . ? C2 C1 C5 C4 -1.7(5) . . . . ? Si1C C1 C5 C4 -170.4(3) . . . . ? Si1A C1 C5 C4 -157.5(4) . . . . ? Si1B C1 C5 C4 -160.7(5) . . . . ? Sc1 C1 C5 C4 66.1(3) . . . . ? C2 C1 C5 C9 175.3(5) . . . . ? Si1C C1 C5 C9 6.6(7) . . . . ? Si1A C1 C5 C9 19.5(8) . . . . ? Si1B C1 C5 C9 16.3(9) . . . . ? Sc1 C1 C5 C9 -116.9(5) . . . . ? C2 C1 C5 Sc1 -67.8(3) . . . . ? Si1C C1 C5 Sc1 123.5(4) . . . . ? Si1A C1 C5 Sc1 136.4(4) . . . . ? Si1B C1 C5 Sc1 133.2(5) . . . . ? N3 Sc1 C5 C4 110.0(3) . . . . ? N2 Sc1 C5 C4 -68.0(5) . . . . ? C1 Sc1 C5 C4 -116.2(4) . . . . ? C2 Sc1 C5 C4 -77.3(3) . . . . ? C3 Sc1 C5 C4 -37.1(3) . . . . ? Si2 Sc1 C5 C4 -135.5(3) . . . . ? Si4 Sc1 C5 C4 74.1(3) . . . . ? N3 Sc1 C5 C1 -133.8(3) . . . . ? N2 Sc1 C5 C1 48.1(5) . . . . ? C2 Sc1 C5 C1 38.9(3) . . . . ? C3 Sc1 C5 C1 79.0(3) . . . . ? C4 Sc1 C5 C1 116.2(4) . . . . ? Si2 Sc1 C5 C1 -19.3(4) . . . . ? Si4 Sc1 C5 C1 -169.7(3) . . . . ? N3 Sc1 C5 C9 -10.5(5) . . . . ? N2 Sc1 C5 C9 171.4(5) . . . . ? C1 Sc1 C5 C9 123.3(6) . . . . ? C2 Sc1 C5 C9 162.2(6) . . . . ? C3 Sc1 C5 C9 -157.7(6) . . . . ? C4 Sc1 C5 C9 -120.6(6) . . . . ? Si2 Sc1 C5 C9 104.0(5) . . . . ? Si4 Sc1 C5 C9 -46.5(5) . . . . ? C15A N1A C12A C13A -33(2) . . . . ? Si1A N1A C12A C13A 160.6(15) . . . . ? C15B N1B C12B C13B -5(2) . . . . ? Si1B N1B C12B C13B -172.5(15) . . . . ? C15C N1C C12C C13C -30(2) . . . . ? Si1C N1C C12C C13C 175.1(14) . . . . ? N1A C12A C13A C14A 27(2) . . . . ? N1B C12B C13B C14B 21(2) . . . . ? N1C C12C C13C C14C 24(2) . . . . ? C12A C13A C14A C15A -12(3) . . . . ? C12B C13B C14B C15B -28(3) . . . . ? C12C C13C C14C C15C -6(2) . . . . ? C12A N1A C15A C14A 28(2) . . . . ? Si1A N1A C15A C14A -164.1(14) . . . . ? C13A C14A C15A N1A -8(2) . . . . ? C12B N1B C15B C14B -13(2) . . . . ? Si1B N1B C15B C14B 155.1(15) . . . . ? C13B C14B C15B N1B 26(3) . . . . ? C12C N1C C15C C14C 25(2) . . . . ? Si1C N1C C15C C14C 177.1(15) . . . . ? C13C C14C C15C N1C -12(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.517 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.062 _database_code_depnum_ccdc_archive 'CCDC 917597' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_g120725b #TrackingRef 'complexes 16 CIF.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H54 N3 Si5 Y' _chemical_formula_sum 'C23 H54 N3 Si5 Y' _chemical_formula_weight 602.05 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9340(4) _cell_length_b 19.5918(7) _cell_length_c 17.4660(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.036(5) _cell_angle_gamma 90.00 _cell_volume 3373.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 3335 _cell_measurement_theta_min 3.3081 _cell_measurement_theta_max 29.3736 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 1.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82037 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15282 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6249 _reflns_number_gt 4769 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6249 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 Y1 Y 0.36399(3) 0.860441(15) 0.190528(15) 0.02446(10) Uani 1 1 d . . . Si1 Si 0.54058(8) 1.00464(5) 0.17123(5) 0.0327(2) Uani 1 1 d . . . Si2 Si 0.33001(8) 0.81321(5) 0.35516(5) 0.0326(2) Uani 1 1 d . . . H2 H 0.459(2) 0.8122(14) 0.3223(15) 0.027(7) Uiso 1 1 d . . . Si3 Si 0.06751(9) 0.88114(6) 0.29669(7) 0.0475(3) Uani 1 1 d . . . H3 H 0.000(3) 0.8909(17) 0.2272(17) 0.044(9) Uiso 1 1 d . . . Si4 Si 0.26635(10) 0.68466(5) 0.14538(5) 0.0419(2) Uani 1 1 d . . . H4 H 0.279(3) 0.6354(16) 0.2060(18) 0.049(9) Uiso 1 1 d . . . Si5 Si 0.55385(9) 0.73758(5) 0.18055(5) 0.0420(3) Uani 1 1 d . . . H5 H 0.591(3) 0.8106(17) 0.1969(17) 0.050(9) Uiso 1 1 d . . . N1 N 0.5297(2) 0.95389(13) 0.25693(13) 0.0291(6) Uani 1 1 d . . . N2 N 0.2265(2) 0.85340(13) 0.28468(14) 0.0308(6) Uani 1 1 d . . . N3 N 0.3845(2) 0.74771(13) 0.16289(14) 0.0322(6) Uani 1 1 d . . . C1 C 0.4045(3) 0.96438(16) 0.10357(17) 0.0341(7) Uani 1 1 d . . . C2 C 0.2617(3) 0.96804(17) 0.11102(18) 0.0375(8) Uani 1 1 d . . . C3 C 0.1964(3) 0.91349(18) 0.06784(18) 0.0411(8) Uani 1 1 d . . . C4 C 0.2957(4) 0.87611(18) 0.03414(18) 0.0442(9) Uani 1 1 d . . . C5 C 0.4226(3) 0.90682(18) 0.05559(17) 0.0394(8) Uani 1 1 d . . . C6 C 0.1875(3) 1.02355(18) 0.1487(2) 0.0490(10) Uani 1 1 d . . . H6A H 0.1798 1.0637 0.1158 0.074 Uiso 1 1 calc R . . H6B H 0.2373 1.0351 0.1982 0.074 Uiso 1 1 calc R . . H6C H 0.0975 1.0076 0.1561 0.074 Uiso 1 1 calc R . . C7 C 0.0437(3) 0.9037(2) 0.0507(2) 0.0635(12) Uani 1 1 d . . . H7A H 0.0101 0.9291 0.0045 0.095 Uiso 1 1 calc R . . H7B H 0.0001 0.9203 0.0938 0.095 Uiso 1 1 calc R . . H7C H 0.0235 0.8556 0.0427 0.095 Uiso 1 1 calc R . . C8 C 0.2655(4) 0.8174(2) -0.0207(2) 0.0661(12) Uani 1 1 d . . . H8A H 0.2517 0.8344 -0.0732 0.099 Uiso 1 1 calc R . . H8B H 0.1841 0.7942 -0.0091 0.099 Uiso 1 1 calc R . . H8C H 0.3411 0.7857 -0.0150 0.099 Uiso 1 1 calc R . . C9 C 0.5538(4) 0.8833(2) 0.0273(2) 0.0570(10) Uani 1 1 d . . . H9A H 0.5354 0.8446 -0.0069 0.085 Uiso 1 1 calc R . . H9B H 0.6182 0.8701 0.0711 0.085 Uiso 1 1 calc R . . H9C H 0.5914 0.9203 -0.0003 0.085 Uiso 1 1 calc R . . C10 C 0.7137(3) 0.9973(2) 0.1412(2) 0.0534(10) Uani 1 1 d . . . H10A H 0.7779 1.0219 0.1775 0.080 Uiso 1 1 calc R . . H10B H 0.7137 1.0167 0.0901 0.080 Uiso 1 1 calc R . . H10C H 0.7395 0.9496 0.1404 0.080 Uiso 1 1 calc R . . C11 C 0.5162(3) 1.09715(18) 0.1900(2) 0.0463(9) Uani 1 1 d . . . H11A H 0.4231 1.1052 0.1989 0.070 Uiso 1 1 calc R . . H11B H 0.5360 1.1235 0.1456 0.070 Uiso 1 1 calc R . . H11C H 0.5768 1.1110 0.2351 0.070 Uiso 1 1 calc R . . C12 C 0.6593(3) 0.93298(19) 0.30357(18) 0.0399(8) Uani 1 1 d . . . H12A H 0.7305 0.9256 0.2703 0.048 Uiso 1 1 calc R . . H12B H 0.6468 0.8908 0.3321 0.048 Uiso 1 1 calc R . . C13 C 0.6958(3) 0.9918(2) 0.3586(2) 0.0574(11) Uani 1 1 d . . . H13A H 0.7519 0.9760 0.4053 0.069 Uiso 1 1 calc R . . H13B H 0.7454 1.0272 0.3340 0.069 Uiso 1 1 calc R . . C14 C 0.5616(3) 1.0186(2) 0.3776(2) 0.0553(10) Uani 1 1 d . . . H14A H 0.5602 1.0686 0.3760 0.066 Uiso 1 1 calc R . . H14B H 0.5448 1.0037 0.4291 0.066 Uiso 1 1 calc R . . C15 C 0.4547(3) 0.98906(17) 0.31589(17) 0.0363(8) Uani 1 1 d . . . H15A H 0.3969 0.9564 0.3391 0.044 Uiso 1 1 calc R . . H15B H 0.3972 1.0256 0.2915 0.044 Uiso 1 1 calc R . . C16 C 0.3606(4) 0.8562(2) 0.4514(2) 0.0631(12) Uani 1 1 d . . . H16A H 0.3972 0.9015 0.4452 0.095 Uiso 1 1 calc R . . H16B H 0.4247 0.8296 0.4856 0.095 Uiso 1 1 calc R . . H16C H 0.2757 0.8598 0.4733 0.095 Uiso 1 1 calc R . . C17 C 0.2942(3) 0.72215(18) 0.3742(2) 0.0486(9) Uani 1 1 d . . . H17A H 0.2103 0.7187 0.3970 0.073 Uiso 1 1 calc R . . H17B H 0.3680 0.7033 0.4093 0.073 Uiso 1 1 calc R . . H17C H 0.2857 0.6969 0.3260 0.073 Uiso 1 1 calc R . . C18 C -0.0301(3) 0.8174(2) 0.3479(3) 0.0716(13) Uani 1 1 d . . . H18A H -0.0294 0.7736 0.3220 0.107 Uiso 1 1 calc R . . H18B H -0.1229 0.8329 0.3474 0.107 Uiso 1 1 calc R . . H18C H 0.0116 0.8126 0.4008 0.107 Uiso 1 1 calc R . . C19 C 0.0692(4) 0.9633(2) 0.3501(3) 0.1020(19) Uani 1 1 d . . . H19A H 0.1011 0.9556 0.4041 0.153 Uiso 1 1 calc R . . H19B H -0.0218 0.9821 0.3453 0.153 Uiso 1 1 calc R . . H19C H 0.1292 0.9953 0.3287 0.153 Uiso 1 1 calc R . . C20 C 0.0919(3) 0.7204(2) 0.1431(2) 0.0587(11) Uani 1 1 d . . . H20A H 0.0825 0.7419 0.1922 0.088 Uiso 1 1 calc R . . H20B H 0.0259 0.6839 0.1338 0.088 Uiso 1 1 calc R . . H20C H 0.0763 0.7539 0.1021 0.088 Uiso 1 1 calc R . . C21 C 0.2763(4) 0.6345(2) 0.0548(2) 0.0648(11) Uani 1 1 d . . . H21A H 0.2572 0.6643 0.0105 0.097 Uiso 1 1 calc R . . H21B H 0.2102 0.5978 0.0515 0.097 Uiso 1 1 calc R . . H21C H 0.3666 0.6154 0.0557 0.097 Uiso 1 1 calc R . . C22 C 0.6157(4) 0.6844(3) 0.2664(2) 0.0741(14) Uani 1 1 d . . . H22A H 0.5688 0.6976 0.3096 0.111 Uiso 1 1 calc R . . H22B H 0.7125 0.6913 0.2797 0.111 Uiso 1 1 calc R . . H22C H 0.5982 0.6366 0.2545 0.111 Uiso 1 1 calc R . . C23 C 0.6452(4) 0.7090(2) 0.0992(2) 0.0728(13) Uani 1 1 d . . . H23A H 0.6299 0.6605 0.0904 0.109 Uiso 1 1 calc R . . H23B H 0.7416 0.7174 0.1120 0.109 Uiso 1 1 calc R . . H23C H 0.6117 0.7341 0.0529 0.109 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 0.03185(16) 0.02201(17) 0.01886(16) 0.00188(13) 0.00052(10) 0.00109(12) Si1 0.0374(5) 0.0276(5) 0.0326(5) 0.0043(4) 0.0025(4) -0.0037(4) Si2 0.0386(5) 0.0357(6) 0.0239(5) 0.0017(4) 0.0058(3) -0.0072(4) Si3 0.0334(5) 0.0430(7) 0.0681(7) 0.0022(6) 0.0137(4) 0.0030(4) Si4 0.0652(6) 0.0247(5) 0.0346(5) -0.0009(4) 0.0020(4) -0.0031(4) Si5 0.0478(5) 0.0429(6) 0.0362(6) -0.0023(5) 0.0084(4) 0.0160(5) N1 0.0300(13) 0.0272(15) 0.0292(14) 0.0033(12) 0.0002(10) 0.0020(11) N2 0.0309(13) 0.0259(15) 0.0363(15) -0.0018(12) 0.0066(10) -0.0004(11) N3 0.0450(14) 0.0257(16) 0.0257(14) -0.0016(12) 0.0035(11) 0.0063(11) C1 0.0516(19) 0.0236(18) 0.0251(17) 0.0046(15) -0.0030(13) -0.0055(14) C2 0.0482(19) 0.0274(19) 0.0329(19) 0.0078(16) -0.0104(14) -0.0027(15) C3 0.057(2) 0.029(2) 0.0315(19) 0.0106(16) -0.0171(15) -0.0060(16) C4 0.083(3) 0.029(2) 0.0165(16) 0.0035(15) -0.0083(16) -0.0088(18) C5 0.064(2) 0.032(2) 0.0210(17) 0.0087(16) 0.0029(14) -0.0049(17) C6 0.0461(19) 0.030(2) 0.066(3) 0.0025(19) -0.0130(17) 0.0045(16) C7 0.067(2) 0.048(3) 0.065(3) 0.010(2) -0.033(2) -0.012(2) C8 0.117(3) 0.050(3) 0.028(2) 0.000(2) -0.001(2) -0.021(2) C9 0.093(3) 0.049(3) 0.033(2) 0.000(2) 0.0234(19) -0.006(2) C10 0.051(2) 0.058(3) 0.053(2) 0.010(2) 0.0171(17) -0.0034(18) C11 0.053(2) 0.032(2) 0.053(2) 0.0030(19) 0.0008(16) -0.0080(16) C12 0.0339(17) 0.044(2) 0.040(2) 0.0117(17) -0.0051(14) -0.0011(15) C13 0.049(2) 0.068(3) 0.050(2) -0.001(2) -0.0139(17) -0.0086(19) C14 0.063(2) 0.057(3) 0.044(2) -0.015(2) -0.0007(17) -0.008(2) C15 0.0399(17) 0.036(2) 0.0331(19) -0.0015(16) 0.0044(14) 0.0002(15) C16 0.095(3) 0.066(3) 0.029(2) -0.004(2) 0.0099(19) -0.027(2) C17 0.060(2) 0.043(2) 0.043(2) 0.0106(19) 0.0043(16) -0.0070(18) C18 0.041(2) 0.072(3) 0.106(4) 0.017(3) 0.029(2) 0.000(2) C19 0.074(3) 0.063(3) 0.180(6) -0.044(4) 0.060(3) 0.001(3) C20 0.060(2) 0.054(3) 0.060(3) -0.009(2) -0.0015(18) -0.012(2) C21 0.098(3) 0.042(3) 0.054(3) -0.017(2) 0.008(2) -0.004(2) C22 0.074(3) 0.087(4) 0.059(3) 0.015(3) -0.001(2) 0.041(2) C23 0.087(3) 0.074(3) 0.064(3) -0.011(3) 0.036(2) 0.025(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 Y1 N2 2.267(2) . ? Y1 N3 2.275(3) . ? Y1 C1 2.601(3) . ? Y1 N1 2.634(2) . ? Y1 C5 2.656(3) . ? Y1 C2 2.657(3) . ? Y1 C4 2.750(3) . ? Y1 C3 2.751(3) . ? Y1 Si5 3.0760(10) . ? Y1 Si2 3.0783(9) . ? Y1 Si1 3.3641(9) . ? Y1 H2 2.56(3) . ? Y1 H5 2.45(3) . ? Si1 N1 1.811(3) . ? Si1 C1 1.859(3) . ? Si1 C11 1.863(4) . ? Si1 C10 1.864(3) . ? Si2 N2 1.698(3) . ? Si2 C17 1.857(4) . ? Si2 C16 1.871(4) . ? Si2 H2 1.47(2) . ? Si3 N2 1.707(2) . ? Si3 C19 1.860(5) . ? Si3 C18 1.874(4) . ? Si3 H3 1.33(3) . ? Si4 N3 1.706(3) . ? Si4 C20 1.865(4) . ? Si4 C21 1.875(4) . ? Si4 H4 1.43(3) . ? Si5 N3 1.684(2) . ? Si5 C23 1.863(4) . ? Si5 C22 1.868(4) . ? Si5 H5 1.50(3) . ? N1 C12 1.494(3) . ? N1 C15 1.510(4) . ? C1 C5 1.429(5) . ? C1 C2 1.442(4) . ? C2 C3 1.419(4) . ? C2 C6 1.509(5) . ? C3 C4 1.414(5) . ? C3 C7 1.522(4) . ? C4 C5 1.406(4) . ? C4 C8 1.503(5) . ? C5 C9 1.520(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 C13 1.516(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 C14 1.508(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.532(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? 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 Y1 N3 99.93(9) . . ? N2 Y1 C1 128.41(10) . . ? N3 Y1 C1 127.72(10) . . ? N2 Y1 N1 97.04(8) . . ? N3 Y1 N1 134.48(8) . . ? C1 Y1 N1 65.15(8) . . ? N2 Y1 C5 151.83(10) . . ? N3 Y1 C5 96.24(10) . . ? C1 Y1 C5 31.53(10) . . ? N1 Y1 C5 87.69(9) . . ? N2 Y1 C2 101.64(10) . . ? N3 Y1 C2 134.25(9) . . ? C1 Y1 C2 31.81(9) . . ? N1 Y1 C2 81.77(8) . . ? C5 Y1 C2 51.40(10) . . ? N2 Y1 C4 129.06(10) . . ? N3 Y1 C4 85.14(10) . . ? C1 Y1 C4 50.92(10) . . ? N1 Y1 C4 115.12(9) . . ? C5 Y1 C4 30.08(10) . . ? C2 Y1 C4 50.22(10) . . ? N2 Y1 C3 103.12(10) . . ? N3 Y1 C3 105.24(9) . . ? C1 Y1 C3 51.07(9) . . ? N1 Y1 C3 111.49(9) . . ? C5 Y1 C3 50.00(10) . . ? C2 Y1 C3 30.35(9) . . ? C4 Y1 C3 29.78(10) . . ? N2 Y1 Si5 114.93(7) . . ? N3 Y1 Si5 32.53(6) . . ? C1 Y1 Si5 116.09(7) . . ? N1 Y1 Si5 102.38(5) . . ? C5 Y1 Si5 90.85(8) . . ? C2 Y1 Si5 142.10(8) . . ? C4 Y1 Si5 96.29(8) . . ? C3 Y1 Si5 124.63(8) . . ? N2 Y1 Si2 32.79(6) . . ? N3 Y1 Si2 85.95(7) . . ? C1 Y1 Si2 145.41(7) . . ? N1 Y1 Si2 86.09(5) . . ? C5 Y1 Si2 173.06(7) . . ? C2 Y1 Si2 130.40(8) . . ? C4 Y1 Si2 156.85(8) . . ? C3 Y1 Si2 135.72(8) . . ? Si5 Y1 Si2 87.47(3) . . ? N2 Y1 Si1 119.45(7) . . ? N3 Y1 Si1 137.10(6) . . ? C1 Y1 Si1 33.29(6) . . ? N1 Y1 Si1 32.33(5) . . ? C5 Y1 Si1 56.64(8) . . ? C2 Y1 Si1 56.77(7) . . ? C4 Y1 Si1 82.82(7) . . ? C3 Y1 Si1 82.99(7) . . ? Si5 Y1 Si1 108.70(3) . . ? Si2 Y1 Si1 117.66(2) . . ? N2 Y1 H2 60.9(5) . . ? N3 Y1 H2 78.4(6) . . ? C1 Y1 H2 138.4(6) . . ? N1 Y1 H2 73.7(6) . . ? C5 Y1 H2 145.9(5) . . ? C2 Y1 H2 147.0(6) . . ? C4 Y1 H2 162.5(6) . . ? C3 Y1 H2 164.0(5) . . ? Si5 Y1 H2 66.5(6) . . ? Si2 Y1 H2 28.3(5) . . ? Si1 Y1 H2 105.2(6) . . ? N2 Y1 H5 125.2(7) . . ? N3 Y1 H5 61.1(8) . . ? C1 Y1 H5 97.5(8) . . ? N1 Y1 H5 74.6(8) . . ? C5 Y1 H5 82.9(7) . . ? C2 Y1 H5 129.1(7) . . ? C4 Y1 H5 101.7(7) . . ? C3 Y1 H5 130.7(7) . . ? Si5 Y1 H5 28.7(8) . . ? Si2 Y1 H5 92.5(7) . . ? Si1 Y1 H5 81.4(8) . . ? H2 Y1 H5 64.9(9) . . ? N1 Si1 C1 100.38(12) . . ? N1 Si1 C11 111.53(14) . . ? C1 Si1 C11 115.11(15) . . ? N1 Si1 C10 109.93(14) . . ? C1 Si1 C10 114.36(16) . . ? C11 Si1 C10 105.58(16) . . ? N1 Si1 Y1 51.07(8) . . ? C1 Si1 Y1 50.19(9) . . ? C11 Si1 Y1 135.96(11) . . ? C10 Si1 Y1 118.29(13) . . ? N2 Si2 C17 117.58(14) . . ? N2 Si2 C16 117.37(17) . . ? C17 Si2 C16 106.60(17) . . ? N2 Si2 Y1 46.31(8) . . ? C17 Si2 Y1 120.06(12) . . ? C16 Si2 Y1 132.79(13) . . ? N2 Si2 H2 101.7(10) . . ? C17 Si2 H2 104.6(11) . . ? C16 Si2 H2 107.7(10) . . ? Y1 Si2 H2 55.8(10) . . ? N2 Si3 C19 112.67(16) . . ? N2 Si3 C18 112.76(16) . . ? C19 Si3 C18 108.1(2) . . ? N2 Si3 H3 107.6(12) . . ? C19 Si3 H3 107.9(14) . . ? C18 Si3 H3 107.6(13) . . ? N3 Si4 C20 110.46(16) . . ? N3 Si4 C21 115.13(17) . . ? C20 Si4 C21 108.88(18) . . ? N3 Si4 H4 111.3(12) . . ? C20 Si4 H4 105.3(12) . . ? C21 Si4 H4 105.2(13) . . ? N3 Si5 C23 117.70(17) . . ? N3 Si5 C22 115.85(17) . . ? C23 Si5 C22 107.5(2) . . ? N3 Si5 Y1 46.58(9) . . ? C23 Si5 Y1 129.64(15) . . ? C22 Si5 Y1 122.36(14) . . ? N3 Si5 H5 98.2(11) . . ? C23 Si5 H5 107.4(11) . . ? C22 Si5 H5 109.3(12) . . ? Y1 Si5 H5 51.8(11) . . ? C12 N1 C15 102.6(2) . . ? C12 N1 Si1 117.81(19) . . ? C15 N1 Si1 113.4(2) . . ? C12 N1 Y1 119.99(19) . . ? C15 N1 Y1 106.46(16) . . ? Si1 N1 Y1 96.61(9) . . ? Si2 N2 Si3 123.07(15) . . ? Si2 N2 Y1 100.90(11) . . ? Si3 N2 Y1 135.92(14) . . ? Si5 N3 Si4 126.69(16) . . ? Si5 N3 Y1 100.89(12) . . ? Si4 N3 Y1 131.56(13) . . ? C5 C1 C2 106.7(3) . . ? C5 C1 Si1 125.0(2) . . ? C2 C1 Si1 124.6(2) . . ? C5 C1 Y1 76.37(18) . . ? C2 C1 Y1 76.23(17) . . ? Si1 C1 Y1 96.52(12) . . ? C3 C2 C1 107.8(3) . . ? C3 C2 C6 123.9(3) . . ? C1 C2 C6 127.9(3) . . ? C3 C2 Y1 78.52(18) . . ? C1 C2 Y1 71.97(16) . . ? C6 C2 Y1 121.3(2) . . ? C4 C3 C2 108.3(3) . . ? C4 C3 C7 125.6(3) . . ? C2 C3 C7 125.4(3) . . ? C4 C3 Y1 75.05(17) . . ? C2 C3 Y1 71.13(16) . . ? C7 C3 Y1 126.8(2) . . ? C5 C4 C3 108.4(3) . . ? C5 C4 C8 126.9(4) . . ? C3 C4 C8 124.5(3) . . ? C5 C4 Y1 71.27(17) . . ? C3 C4 Y1 75.17(18) . . ? C8 C4 Y1 123.6(2) . . ? C4 C5 C1 108.7(3) . . ? C4 C5 C9 124.1(3) . . ? C1 C5 C9 127.1(3) . . ? C4 C5 Y1 78.64(18) . . ? C1 C5 Y1 72.10(17) . . ? C9 C5 Y1 118.3(2) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 105.1(3) . . ? N1 C12 H12A 110.7 . . ? C13 C12 H12A 110.7 . . ? N1 C12 H12B 110.7 . . ? C13 C12 H12B 110.7 . . ? H12A C12 H12B 108.8 . . ? C14 C13 C12 104.8(3) . . ? C14 C13 H13A 110.8 . . ? C12 C13 H13A 110.8 . . ? C14 C13 H13B 110.8 . . ? C12 C13 H13B 110.8 . . ? H13A C13 H13B 108.9 . . ? C13 C14 C15 105.6(3) . . ? C13 C14 H14A 110.6 . . ? C15 C14 H14A 110.6 . . ? C13 C14 H14B 110.6 . . ? C15 C14 H14B 110.6 . . ? H14A C14 H14B 108.8 . . ? N1 C15 C14 107.2(2) . . ? N1 C15 H15A 110.3 . . ? C14 C15 H15A 110.3 . . ? N1 C15 H15B 110.3 . . ? C14 C15 H15B 110.3 . . ? H15A C15 H15B 108.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si4 C20 H20A 109.5 . . ? Si4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si4 C21 H21A 109.5 . . ? Si4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si5 C22 H22A 109.5 . . ? Si5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si5 C23 H23A 109.5 . . ? Si5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Y1 Si1 N1 51.01(12) . . . . ? N3 Y1 Si1 N1 -102.96(13) . . . . ? C1 Y1 Si1 N1 167.12(17) . . . . ? C5 Y1 Si1 N1 -161.82(13) . . . . ? C2 Y1 Si1 N1 135.68(13) . . . . ? C4 Y1 Si1 N1 -177.83(12) . . . . ? C3 Y1 Si1 N1 152.16(12) . . . . ? Si5 Y1 Si1 N1 -83.59(10) . . . . ? Si2 Y1 Si1 N1 13.58(10) . . . . ? N2 Y1 Si1 C1 -116.11(15) . . . . ? N3 Y1 Si1 C1 89.92(16) . . . . ? N1 Y1 Si1 C1 -167.12(17) . . . . ? C5 Y1 Si1 C1 31.06(16) . . . . ? C2 Y1 Si1 C1 -31.44(15) . . . . ? C4 Y1 Si1 C1 15.05(16) . . . . ? C3 Y1 Si1 C1 -14.96(15) . . . . ? Si5 Y1 Si1 C1 109.29(13) . . . . ? Si2 Y1 Si1 C1 -153.54(13) . . . . ? N2 Y1 Si1 C11 -29.96(18) . . . . ? N3 Y1 Si1 C11 176.07(18) . . . . ? C1 Y1 Si1 C11 86.1(2) . . . . ? N1 Y1 Si1 C11 -80.97(19) . . . . ? C5 Y1 Si1 C11 117.21(19) . . . . ? C2 Y1 Si1 C11 54.71(18) . . . . ? C4 Y1 Si1 C11 101.20(18) . . . . ? C3 Y1 Si1 C11 71.19(18) . . . . ? Si5 Y1 Si1 C11 -164.56(16) . . . . ? Si2 Y1 Si1 C11 -67.39(17) . . . . ? N2 Y1 Si1 C10 144.62(15) . . . . ? N3 Y1 Si1 C10 -9.35(17) . . . . ? C1 Y1 Si1 C10 -99.28(19) . . . . ? N1 Y1 Si1 C10 93.60(17) . . . . ? C5 Y1 Si1 C10 -68.21(16) . . . . ? C2 Y1 Si1 C10 -130.72(16) . . . . ? C4 Y1 Si1 C10 -84.22(16) . . . . ? C3 Y1 Si1 C10 -114.23(16) . . . . ? Si5 Y1 Si1 C10 10.02(14) . . . . ? Si2 Y1 Si1 C10 107.18(14) . . . . ? N3 Y1 Si2 N2 -115.42(13) . . . . ? C1 Y1 Si2 N2 76.69(17) . . . . ? N1 Y1 Si2 N2 109.44(13) . . . . ? C5 Y1 Si2 N2 135.9(7) . . . . ? C2 Y1 Si2 N2 33.71(15) . . . . ? C4 Y1 Si2 N2 -47.9(2) . . . . ? C3 Y1 Si2 N2 -7.67(16) . . . . ? Si5 Y1 Si2 N2 -147.97(12) . . . . ? Si1 Y1 Si2 N2 102.21(12) . . . . ? N2 Y1 Si2 C17 100.76(18) . . . . ? N3 Y1 Si2 C17 -14.65(14) . . . . ? C1 Y1 Si2 C17 177.46(17) . . . . ? N1 Y1 Si2 C17 -149.80(14) . . . . ? C5 Y1 Si2 C17 -123.3(7) . . . . ? C2 Y1 Si2 C17 134.47(15) . . . . ? C4 Y1 Si2 C17 52.9(2) . . . . ? C3 Y1 Si2 C17 93.09(17) . . . . ? Si5 Y1 Si2 C17 -47.20(13) . . . . ? Si1 Y1 Si2 C17 -157.03(13) . . . . ? N2 Y1 Si2 C16 -89.0(2) . . . . ? N3 Y1 Si2 C16 155.6(2) . . . . ? C1 Y1 Si2 C16 -12.3(2) . . . . ? N1 Y1 Si2 C16 20.5(2) . . . . ? C5 Y1 Si2 C16 46.9(7) . . . . ? C2 Y1 Si2 C16 -55.3(2) . . . . ? C4 Y1 Si2 C16 -136.8(3) . . . . ? C3 Y1 Si2 C16 -96.6(2) . . . . ? Si5 Y1 Si2 C16 123.06(19) . . . . ? Si1 Y1 Si2 C16 13.2(2) . . . . ? N2 Y1 Si5 N3 67.96(14) . . . . ? C1 Y1 Si5 N3 -119.94(14) . . . . ? N1 Y1 Si5 N3 171.86(13) . . . . ? C5 Y1 Si5 N3 -100.31(14) . . . . ? C2 Y1 Si5 N3 -95.65(16) . . . . ? C4 Y1 Si5 N3 -70.65(14) . . . . ? C3 Y1 Si5 N3 -60.75(15) . . . . ? Si2 Y1 Si5 N3 86.43(12) . . . . ? Si1 Y1 Si5 N3 -155.17(12) . . . . ? N2 Y1 Si5 C23 160.6(2) . . . . ? N3 Y1 Si5 C23 92.7(2) . . . . ? C1 Y1 Si5 C23 -27.3(2) . . . . ? N1 Y1 Si5 C23 -95.4(2) . . . . ? C5 Y1 Si5 C23 -7.6(2) . . . . ? C2 Y1 Si5 C23 -3.0(2) . . . . ? C4 Y1 Si5 C23 22.0(2) . . . . ? C3 Y1 Si5 C23 31.9(2) . . . . ? Si2 Y1 Si5 C23 179.1(2) . . . . ? Si1 Y1 Si5 C23 -62.5(2) . . . . ? N2 Y1 Si5 C22 -28.4(2) . . . . ? N3 Y1 Si5 C22 -96.4(2) . . . . ? C1 Y1 Si5 C22 143.68(19) . . . . ? N1 Y1 Si5 C22 75.49(19) . . . . ? C5 Y1 Si5 C22 163.31(19) . . . . ? C2 Y1 Si5 C22 168.0(2) . . . . ? C4 Y1 Si5 C22 -167.03(19) . . . . ? C3 Y1 Si5 C22 -157.1(2) . . . . ? Si2 Y1 Si5 C22 -9.94(18) . . . . ? Si1 Y1 Si5 C22 108.45(18) . . . . ? C1 Si1 N1 C12 139.1(2) . . . . ? C11 Si1 N1 C12 -98.5(2) . . . . ? C10 Si1 N1 C12 18.2(3) . . . . ? Y1 Si1 N1 C12 129.0(2) . . . . ? C1 Si1 N1 C15 -101.1(2) . . . . ? C11 Si1 N1 C15 21.3(2) . . . . ? C10 Si1 N1 C15 138.0(2) . . . . ? Y1 Si1 N1 C15 -111.16(19) . . . . ? C1 Si1 N1 Y1 10.02(13) . . . . ? C11 Si1 N1 Y1 132.44(12) . . . . ? C10 Si1 N1 Y1 -110.81(14) . . . . ? N2 Y1 N1 C12 95.5(2) . . . . ? N3 Y1 N1 C12 -15.9(3) . . . . ? C1 Y1 N1 C12 -135.3(2) . . . . ? C5 Y1 N1 C12 -112.4(2) . . . . ? C2 Y1 N1 C12 -163.7(2) . . . . ? C4 Y1 N1 C12 -125.1(2) . . . . ? C3 Y1 N1 C12 -157.4(2) . . . . ? Si5 Y1 N1 C12 -22.0(2) . . . . ? Si2 Y1 N1 C12 64.5(2) . . . . ? Si1 Y1 N1 C12 -127.5(2) . . . . ? N2 Y1 N1 C15 -20.16(18) . . . . ? N3 Y1 N1 C15 -131.55(18) . . . . ? C1 Y1 N1 C15 109.09(19) . . . . ? C5 Y1 N1 C15 131.96(19) . . . . ? C2 Y1 N1 C15 80.65(18) . . . . ? C4 Y1 N1 C15 119.22(19) . . . . ? C3 Y1 N1 C15 86.97(19) . . . . ? Si5 Y1 N1 C15 -137.67(17) . . . . ? Si2 Y1 N1 C15 -51.13(17) . . . . ? Si1 Y1 N1 C15 116.8(2) . . . . ? N2 Y1 N1 Si1 -137.00(10) . . . . ? N3 Y1 N1 Si1 111.61(12) . . . . ? C1 Y1 N1 Si1 -7.75(10) . . . . ? C5 Y1 N1 Si1 15.12(11) . . . . ? C2 Y1 N1 Si1 -36.19(11) . . . . ? C4 Y1 N1 Si1 2.38(14) . . . . ? C3 Y1 N1 Si1 -29.88(13) . . . . ? Si5 Y1 N1 Si1 105.49(8) . . . . ? Si2 Y1 N1 Si1 -167.97(9) . . . . ? C17 Si2 N2 Si3 76.8(2) . . . . ? C16 Si2 N2 Si3 -52.4(2) . . . . ? Y1 Si2 N2 Si3 -176.7(2) . . . . ? C17 Si2 N2 Y1 -106.42(16) . . . . ? C16 Si2 N2 Y1 124.29(16) . . . . ? C19 Si3 N2 Si2 79.6(3) . . . . ? C18 Si3 N2 Si2 -43.2(3) . . . . ? C19 Si3 N2 Y1 -95.8(3) . . . . ? C18 Si3 N2 Y1 141.4(2) . . . . ? N3 Y1 N2 Si2 66.16(12) . . . . ? C1 Y1 N2 Si2 -135.17(11) . . . . ? N1 Y1 N2 Si2 -71.43(12) . . . . ? C5 Y1 N2 Si2 -169.74(16) . . . . ? C2 Y1 N2 Si2 -154.44(11) . . . . ? C4 Y1 N2 Si2 157.95(11) . . . . ? C3 Y1 N2 Si2 174.51(11) . . . . ? Si5 Y1 N2 Si2 35.76(13) . . . . ? Si1 Y1 N2 Si2 -96.19(11) . . . . ? N3 Y1 N2 Si3 -117.79(19) . . . . ? C1 Y1 N2 Si3 40.9(2) . . . . ? N1 Y1 N2 Si3 104.63(19) . . . . ? C5 Y1 N2 Si3 6.3(3) . . . . ? C2 Y1 N2 Si3 21.6(2) . . . . ? C4 Y1 N2 Si3 -26.0(3) . . . . ? C3 Y1 N2 Si3 -9.4(2) . . . . ? Si5 Y1 N2 Si3 -148.18(17) . . . . ? Si2 Y1 N2 Si3 176.1(3) . . . . ? Si1 Y1 N2 Si3 79.9(2) . . . . ? C23 Si5 N3 Si4 70.0(3) . . . . ? C22 Si5 N3 Si4 -59.2(3) . . . . ? Y1 Si5 N3 Si4 -170.4(2) . . . . ? C23 Si5 N3 Y1 -119.69(19) . . . . ? C22 Si5 N3 Y1 111.12(19) . . . . ? C20 Si4 N3 Si5 171.97(19) . . . . ? C21 Si4 N3 Si5 -64.2(2) . . . . ? C20 Si4 N3 Y1 4.7(2) . . . . ? C21 Si4 N3 Y1 128.5(2) . . . . ? N2 Y1 N3 Si5 -121.43(11) . . . . ? C1 Y1 N3 Si5 79.69(14) . . . . ? N1 Y1 N3 Si5 -11.17(18) . . . . ? C5 Y1 N3 Si5 81.73(12) . . . . ? C2 Y1 N3 Si5 121.41(13) . . . . ? C4 Y1 N3 Si5 109.74(13) . . . . ? C3 Y1 N3 Si5 131.92(12) . . . . ? Si2 Y1 N3 Si5 -91.65(10) . . . . ? Si1 Y1 N3 Si5 35.75(16) . . . . ? N2 Y1 N3 Si4 48.24(19) . . . . ? C1 Y1 N3 Si4 -110.65(18) . . . . ? N1 Y1 N3 Si4 158.49(14) . . . . ? C5 Y1 N3 Si4 -108.61(18) . . . . ? C2 Y1 N3 Si4 -68.9(2) . . . . ? C4 Y1 N3 Si4 -80.60(19) . . . . ? C3 Y1 N3 Si4 -58.4(2) . . . . ? Si5 Y1 N3 Si4 169.7(3) . . . . ? Si2 Y1 N3 Si4 78.01(17) . . . . ? Si1 Y1 N3 Si4 -154.59(12) . . . . ? N1 Si1 C1 C5 -88.0(3) . . . . ? C11 Si1 C1 C5 152.1(3) . . . . ? C10 Si1 C1 C5 29.6(3) . . . . ? Y1 Si1 C1 C5 -77.9(3) . . . . ? N1 Si1 C1 C2 67.6(3) . . . . ? C11 Si1 C1 C2 -52.3(3) . . . . ? C10 Si1 C1 C2 -174.8(3) . . . . ? Y1 Si1 C1 C2 77.7(2) . . . . ? N1 Si1 C1 Y1 -10.15(13) . . . . ? C11 Si1 C1 Y1 -130.01(14) . . . . ? C10 Si1 C1 Y1 107.46(16) . . . . ? N2 Y1 C1 C5 -149.19(17) . . . . ? N3 Y1 C1 C5 3.9(2) . . . . ? N1 Y1 C1 C5 132.0(2) . . . . ? C2 Y1 C1 C5 -111.4(2) . . . . ? C4 Y1 C1 C5 -36.11(18) . . . . ? C3 Y1 C1 C5 -74.7(2) . . . . ? Si5 Y1 C1 C5 39.97(19) . . . . ? Si2 Y1 C1 C5 168.54(14) . . . . ? Si1 Y1 C1 C5 124.5(2) . . . . ? N2 Y1 C1 C2 -37.8(2) . . . . ? N3 Y1 C1 C2 115.26(18) . . . . ? N1 Y1 C1 C2 -116.58(19) . . . . ? C5 Y1 C1 C2 111.4(2) . . . . ? C4 Y1 C1 C2 75.26(19) . . . . ? C3 Y1 C1 C2 36.65(17) . . . . ? Si5 Y1 C1 C2 151.34(15) . . . . ? Si2 Y1 C1 C2 -80.1(2) . . . . ? Si1 Y1 C1 C2 -124.1(2) . . . . ? N2 Y1 C1 Si1 86.31(15) . . . . ? N3 Y1 C1 Si1 -120.62(12) . . . . ? N1 Y1 C1 Si1 7.55(10) . . . . ? C5 Y1 C1 Si1 -124.5(2) . . . . ? C2 Y1 C1 Si1 124.1(2) . . . . ? C4 Y1 C1 Si1 -160.6(2) . . . . ? C3 Y1 C1 Si1 160.77(19) . . . . ? Si5 Y1 C1 Si1 -84.53(12) . . . . ? Si2 Y1 C1 Si1 44.0(2) . . . . ? C5 C1 C2 C3 -0.2(3) . . . . ? Si1 C1 C2 C3 -159.5(2) . . . . ? Y1 C1 C2 C3 -71.1(2) . . . . ? C5 C1 C2 C6 -173.0(3) . . . . ? Si1 C1 C2 C6 27.7(5) . . . . ? Y1 C1 C2 C6 116.1(3) . . . . ? C5 C1 C2 Y1 70.9(2) . . . . ? Si1 C1 C2 Y1 -88.4(2) . . . . ? N2 Y1 C2 C3 -96.1(2) . . . . ? N3 Y1 C2 C3 20.4(3) . . . . ? C1 Y1 C2 C3 113.2(3) . . . . ? N1 Y1 C2 C3 168.3(2) . . . . ? C5 Y1 C2 C3 74.7(2) . . . . ? C4 Y1 C2 C3 35.58(19) . . . . ? Si5 Y1 C2 C3 68.7(2) . . . . ? Si2 Y1 C2 C3 -114.02(19) . . . . ? Si1 Y1 C2 C3 146.1(2) . . . . ? N2 Y1 C2 C1 150.63(17) . . . . ? N3 Y1 C2 C1 -92.85(19) . . . . ? N1 Y1 C2 C1 55.08(17) . . . . ? C5 Y1 C2 C1 -38.55(17) . . . . ? C4 Y1 C2 C1 -77.6(2) . . . . ? C3 Y1 C2 C1 -113.2(3) . . . . ? Si5 Y1 C2 C1 -44.5(2) . . . . ? Si2 Y1 C2 C1 132.76(15) . . . . ? Si1 Y1 C2 C1 32.90(15) . . . . ? N2 Y1 C2 C6 26.7(2) . . . . ? N3 Y1 C2 C6 143.3(2) . . . . ? C1 Y1 C2 C6 -123.9(3) . . . . ? N1 Y1 C2 C6 -68.8(2) . . . . ? C5 Y1 C2 C6 -162.4(3) . . . . ? C4 Y1 C2 C6 158.5(3) . . . . ? C3 Y1 C2 C6 122.9(3) . . . . ? Si5 Y1 C2 C6 -168.41(18) . . . . ? Si2 Y1 C2 C6 8.9(3) . . . . ? Si1 Y1 C2 C6 -91.0(2) . . . . ? C1 C2 C3 C4 0.2(3) . . . . ? C6 C2 C3 C4 173.4(3) . . . . ? Y1 C2 C3 C4 -66.4(2) . . . . ? C1 C2 C3 C7 -171.1(3) . . . . ? C6 C2 C3 C7 2.1(5) . . . . ? Y1 C2 C3 C7 122.3(3) . . . . ? C1 C2 C3 Y1 66.6(2) . . . . ? C6 C2 C3 Y1 -120.2(3) . . . . ? N2 Y1 C3 C4 -153.53(19) . . . . ? N3 Y1 C3 C4 -49.2(2) . . . . ? C1 Y1 C3 C4 77.3(2) . . . . ? N1 Y1 C3 C4 103.3(2) . . . . ? C5 Y1 C3 C4 36.10(19) . . . . ? C2 Y1 C3 C4 115.8(3) . . . . ? Si5 Y1 C3 C4 -20.1(2) . . . . ? Si2 Y1 C3 C4 -149.28(16) . . . . ? Si1 Y1 C3 C4 87.78(19) . . . . ? N2 Y1 C3 C2 90.7(2) . . . . ? N3 Y1 C3 C2 -165.02(19) . . . . ? C1 Y1 C3 C2 -38.51(19) . . . . ? N1 Y1 C3 C2 -12.4(2) . . . . ? C5 Y1 C3 C2 -79.7(2) . . . . ? C4 Y1 C3 C2 -115.8(3) . . . . ? Si5 Y1 C3 C2 -135.93(18) . . . . ? Si2 Y1 C3 C2 94.9(2) . . . . ? Si1 Y1 C3 C2 -28.01(19) . . . . ? N2 Y1 C3 C7 -29.9(3) . . . . ? N3 Y1 C3 C7 74.4(3) . . . . ? C1 Y1 C3 C7 -159.1(4) . . . . ? N1 Y1 C3 C7 -133.1(3) . . . . ? C5 Y1 C3 C7 159.7(4) . . . . ? C2 Y1 C3 C7 -120.6(4) . . . . ? C4 Y1 C3 C7 123.6(4) . . . . ? Si5 Y1 C3 C7 103.4(3) . . . . ? Si2 Y1 C3 C7 -25.7(4) . . . . ? Si1 Y1 C3 C7 -148.6(3) . . . . ? C2 C3 C4 C5 -0.2(4) . . . . ? C7 C3 C4 C5 171.1(3) . . . . ? Y1 C3 C4 C5 -64.0(2) . . . . ? C2 C3 C4 C8 -175.4(3) . . . . ? C7 C3 C4 C8 -4.1(5) . . . . ? Y1 C3 C4 C8 120.8(3) . . . . ? C2 C3 C4 Y1 63.8(2) . . . . ? C7 C3 C4 Y1 -124.9(3) . . . . ? N2 Y1 C4 C5 149.77(19) . . . . ? N3 Y1 C4 C5 -111.4(2) . . . . ? C1 Y1 C4 C5 37.9(2) . . . . ? N1 Y1 C4 C5 26.1(2) . . . . ? C2 Y1 C4 C5 79.5(2) . . . . ? C3 Y1 C4 C5 115.8(3) . . . . ? Si5 Y1 C4 C5 -80.8(2) . . . . ? Si2 Y1 C4 C5 -179.09(17) . . . . ? Si1 Y1 C4 C5 27.4(2) . . . . ? N2 Y1 C4 C3 34.0(2) . . . . ? N3 Y1 C4 C3 132.8(2) . . . . ? C1 Y1 C4 C3 -77.8(2) . . . . ? N1 Y1 C4 C3 -89.7(2) . . . . ? C5 Y1 C4 C3 -115.8(3) . . . . ? C2 Y1 C4 C3 -36.30(18) . . . . ? Si5 Y1 C4 C3 163.44(19) . . . . ? Si2 Y1 C4 C3 65.1(3) . . . . ? Si1 Y1 C4 C3 -88.43(19) . . . . ? N2 Y1 C4 C8 -87.9(3) . . . . ? N3 Y1 C4 C8 11.0(3) . . . . ? C1 Y1 C4 C8 160.3(4) . . . . ? N1 Y1 C4 C8 148.4(3) . . . . ? C5 Y1 C4 C8 122.4(4) . . . . ? C2 Y1 C4 C8 -158.2(4) . . . . ? C3 Y1 C4 C8 -121.9(4) . . . . ? Si5 Y1 C4 C8 41.6(3) . . . . ? Si2 Y1 C4 C8 -56.7(4) . . . . ? Si1 Y1 C4 C8 149.7(3) . . . . ? C3 C4 C5 C1 0.1(4) . . . . ? C8 C4 C5 C1 175.1(3) . . . . ? Y1 C4 C5 C1 -66.5(2) . . . . ? C3 C4 C5 C9 -176.8(3) . . . . ? C8 C4 C5 C9 -1.8(5) . . . . ? Y1 C4 C5 C9 116.6(3) . . . . ? C3 C4 C5 Y1 66.6(2) . . . . ? C8 C4 C5 Y1 -118.4(3) . . . . ? C2 C1 C5 C4 0.1(3) . . . . ? Si1 C1 C5 C4 159.3(2) . . . . ? Y1 C1 C5 C4 70.9(2) . . . . ? C2 C1 C5 C9 176.8(3) . . . . ? Si1 C1 C5 C9 -24.0(5) . . . . ? Y1 C1 C5 C9 -112.4(3) . . . . ? C2 C1 C5 Y1 -70.8(2) . . . . ? Si1 C1 C5 Y1 88.4(2) . . . . ? N2 Y1 C5 C4 -55.9(3) . . . . ? N3 Y1 C5 C4 69.0(2) . . . . ? C1 Y1 C5 C4 -114.1(3) . . . . ? N1 Y1 C5 C4 -156.5(2) . . . . ? C2 Y1 C5 C4 -75.2(2) . . . . ? C3 Y1 C5 C4 -35.71(19) . . . . ? Si5 Y1 C5 C4 101.1(2) . . . . ? Si2 Y1 C5 C4 177.0(5) . . . . ? Si1 Y1 C5 C4 -146.9(2) . . . . ? N2 Y1 C5 C1 58.2(3) . . . . ? N3 Y1 C5 C1 -176.91(18) . . . . ? N1 Y1 C5 C1 -42.41(18) . . . . ? C2 Y1 C5 C1 38.91(17) . . . . ? C4 Y1 C5 C1 114.1(3) . . . . ? C3 Y1 C5 C1 78.4(2) . . . . ? Si5 Y1 C5 C1 -144.76(17) . . . . ? Si2 Y1 C5 C1 -68.8(7) . . . . ? Si1 Y1 C5 C1 -32.79(15) . . . . ? N2 Y1 C5 C9 -178.7(2) . . . . ? N3 Y1 C5 C9 -53.8(3) . . . . ? C1 Y1 C5 C9 123.1(3) . . . . ? N1 Y1 C5 C9 80.7(3) . . . . ? C2 Y1 C5 C9 162.0(3) . . . . ? C4 Y1 C5 C9 -122.8(4) . . . . ? C3 Y1 C5 C9 -158.5(3) . . . . ? Si5 Y1 C5 C9 -21.6(3) . . . . ? Si2 Y1 C5 C9 54.3(8) . . . . ? Si1 Y1 C5 C9 90.3(3) . . . . ? C15 N1 C12 C13 -38.6(3) . . . . ? Si1 N1 C12 C13 86.7(3) . . . . ? Y1 N1 C12 C13 -156.2(2) . . . . ? N1 C12 C13 C14 34.6(4) . . . . ? C12 C13 C14 C15 -16.3(4) . . . . ? C12 N1 C15 C14 28.3(3) . . . . ? Si1 N1 C15 C14 -99.9(3) . . . . ? Y1 N1 C15 C14 155.1(2) . . . . ? C13 C14 C15 N1 -7.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.319 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.074 _database_code_depnum_ccdc_archive 'CCDC 917598' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_g120727e #TrackingRef 'complexes 16 CIF.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H54 Lu N3 Si5' _chemical_formula_sum 'C23 H54 Lu N3 Si5' _chemical_formula_weight 688.11 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' Lu Lu -0.4720 5.8584 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9233(3) _cell_length_b 19.4249(5) _cell_length_c 17.3278(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.934(2) _cell_angle_gamma 90.00 _cell_volume 3315.66(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5744 _cell_measurement_theta_min 3.1398 _cell_measurement_theta_max 29.4654 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 3.174 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71940 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4692 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15664 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6148 _reflns_number_gt 5123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6148 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.365265(13) 0.860480(8) 0.188660(8) 0.01991(6) Uani 1 1 d . . . Si1 Si 0.54347(9) 1.00306(6) 0.17065(6) 0.0270(2) Uani 1 1 d . . . Si2 Si 0.33066(9) 0.81305(6) 0.35241(6) 0.0259(2) Uani 1 1 d . . . H2 H 0.460(3) 0.8116(18) 0.3197(18) 0.022(9) Uiso 1 1 d . . . Si3 Si 0.07010(10) 0.88308(6) 0.29395(8) 0.0380(3) Uani 1 1 d . . . H3 H -0.002(3) 0.894(2) 0.219(2) 0.043(11) Uiso 1 1 d . . . Si4 Si 0.26290(11) 0.68460(6) 0.14495(7) 0.0345(3) Uani 1 1 d . . . H4 H 0.276(4) 0.632(2) 0.209(2) 0.047(12) Uiso 1 1 d . . . Si5 Si 0.55041(10) 0.73786(6) 0.17910(7) 0.0338(3) Uani 1 1 d . . . H5 H 0.598(3) 0.810(2) 0.195(2) 0.048(11) Uiso 1 1 d . . . N1 N 0.5301(2) 0.95135(15) 0.25673(17) 0.0229(7) Uani 1 1 d . . . N2 N 0.2287(3) 0.85470(15) 0.28066(18) 0.0248(7) Uani 1 1 d . . . N3 N 0.3810(3) 0.74825(16) 0.16225(17) 0.0255(7) Uani 1 1 d . . . C1 C 0.4070(3) 0.9628(2) 0.1024(2) 0.0275(9) Uani 1 1 d . . . C2 C 0.2645(3) 0.9669(2) 0.1096(2) 0.0292(9) Uani 1 1 d . . . C3 C 0.1987(4) 0.9117(2) 0.0669(2) 0.0349(10) Uani 1 1 d . . . C4 C 0.2979(4) 0.8736(2) 0.0333(2) 0.0354(10) Uani 1 1 d . . . C5 C 0.4255(4) 0.9046(2) 0.0542(2) 0.0301(9) Uani 1 1 d . . . C6 C 0.1905(4) 1.0235(2) 0.1469(2) 0.0401(11) Uani 1 1 d . . . H6A H 0.1867 1.0648 0.1140 0.060 Uiso 1 1 calc R . . H6B H 0.2387 1.0342 0.1982 0.060 Uiso 1 1 calc R . . H6C H 0.0980 1.0084 0.1525 0.060 Uiso 1 1 calc R . . C7 C 0.0469(4) 0.9024(2) 0.0489(3) 0.0472(12) Uani 1 1 d . . . H7A H 0.0016 0.9229 0.0905 0.071 Uiso 1 1 calc R . . H7B H 0.0256 0.8531 0.0451 0.071 Uiso 1 1 calc R . . H7C H 0.0152 0.9249 -0.0005 0.071 Uiso 1 1 calc R . . C8 C 0.2690(5) 0.8146(2) -0.0225(2) 0.0471(12) Uani 1 1 d . . . H8A H 0.2528 0.8323 -0.0757 0.071 Uiso 1 1 calc R . . H8B H 0.1884 0.7897 -0.0101 0.071 Uiso 1 1 calc R . . H8C H 0.3470 0.7833 -0.0178 0.071 Uiso 1 1 calc R . . C9 C 0.5570(4) 0.8819(2) 0.0250(3) 0.0440(11) Uani 1 1 d . . . H9A H 0.5388 0.8428 -0.0106 0.066 Uiso 1 1 calc R . . H9B H 0.6224 0.8680 0.0692 0.066 Uiso 1 1 calc R . . H9C H 0.5945 0.9201 -0.0025 0.066 Uiso 1 1 calc R . . C10 C 0.7174(4) 0.9947(2) 0.1405(2) 0.0431(11) Uani 1 1 d . . . H10A H 0.7827 1.0192 0.1776 0.065 Uiso 1 1 calc R . . H10B H 0.7183 1.0147 0.0886 0.065 Uiso 1 1 calc R . . H10C H 0.7424 0.9460 0.1393 0.065 Uiso 1 1 calc R . . C11 C 0.5201(4) 1.0963(2) 0.1908(2) 0.0356(10) Uani 1 1 d . . . H11A H 0.4259 1.1047 0.1999 0.053 Uiso 1 1 calc R . . H11B H 0.5408 1.1236 0.1461 0.053 Uiso 1 1 calc R . . H11C H 0.5812 1.1098 0.2370 0.053 Uiso 1 1 calc R . . C12 C 0.6602(3) 0.9289(2) 0.3026(2) 0.0312(10) Uani 1 1 d . . . H12A H 0.7308 0.9203 0.2680 0.037 Uiso 1 1 calc R . . H12B H 0.6466 0.8864 0.3323 0.037 Uiso 1 1 calc R . . C13 C 0.6998(4) 0.9892(2) 0.3573(2) 0.0429(11) Uani 1 1 d . . . H13A H 0.7592 0.9736 0.4040 0.051 Uiso 1 1 calc R . . H13B H 0.7477 1.0253 0.3307 0.051 Uiso 1 1 calc R . . C14 C 0.5658(4) 1.0161(2) 0.3789(2) 0.0432(11) Uani 1 1 d . . . H14A H 0.5650 1.0670 0.3790 0.052 Uiso 1 1 calc R . . H14B H 0.5502 0.9994 0.4311 0.052 Uiso 1 1 calc R . . C15 C 0.4566(3) 0.9879(2) 0.3165(2) 0.0305(9) Uani 1 1 d . . . H15A H 0.3963 0.9554 0.3400 0.037 Uiso 1 1 calc R . . H15B H 0.4007 1.0260 0.2919 0.037 Uiso 1 1 calc R . . C16 C 0.3595(5) 0.8553(2) 0.4502(3) 0.0498(12) Uani 1 1 d . . . H16A H 0.3831 0.9038 0.4439 0.075 Uiso 1 1 calc R . . H16B H 0.4339 0.8320 0.4823 0.075 Uiso 1 1 calc R . . H16C H 0.2766 0.8522 0.4755 0.075 Uiso 1 1 calc R . . C17 C 0.2919(4) 0.7214(2) 0.3715(2) 0.0384(10) Uani 1 1 d . . . H17A H 0.2087 0.7187 0.3966 0.058 Uiso 1 1 calc R . . H17B H 0.3674 0.7011 0.4057 0.058 Uiso 1 1 calc R . . H17C H 0.2793 0.6961 0.3222 0.058 Uiso 1 1 calc R . . C18 C -0.0254(4) 0.8197(3) 0.3485(3) 0.0519(13) Uani 1 1 d . . . H18A H -0.0318 0.7756 0.3208 0.078 Uiso 1 1 calc R . . H18B H -0.1168 0.8374 0.3525 0.078 Uiso 1 1 calc R . . H18C H 0.0227 0.8131 0.4008 0.078 Uiso 1 1 calc R . . C19 C 0.0732(5) 0.9668(3) 0.3470(4) 0.0758(18) Uani 1 1 d . . . H19A H 0.1160 0.9603 0.4005 0.114 Uiso 1 1 calc R . . H19B H -0.0198 0.9834 0.3476 0.114 Uiso 1 1 calc R . . H19C H 0.1252 1.0006 0.3207 0.114 Uiso 1 1 calc R . . C20 C 0.0874(4) 0.7197(2) 0.1441(3) 0.0471(12) Uani 1 1 d . . . H20A H 0.0777 0.7403 0.1948 0.071 Uiso 1 1 calc R . . H20B H 0.0213 0.6824 0.1336 0.071 Uiso 1 1 calc R . . H20C H 0.0710 0.7549 0.1035 0.071 Uiso 1 1 calc R . . C21 C 0.2719(5) 0.6337(2) 0.0537(3) 0.0539(13) Uani 1 1 d . . . H21A H 0.2460 0.6630 0.0084 0.081 Uiso 1 1 calc R . . H21B H 0.2097 0.5944 0.0526 0.081 Uiso 1 1 calc R . . H21C H 0.3648 0.6169 0.0525 0.081 Uiso 1 1 calc R . . C22 C 0.6148(4) 0.6851(3) 0.2650(3) 0.0577(14) Uani 1 1 d . . . H22A H 0.5771 0.7025 0.3110 0.087 Uiso 1 1 calc R . . H22B H 0.7141 0.6879 0.2736 0.087 Uiso 1 1 calc R . . H22C H 0.5872 0.6370 0.2559 0.087 Uiso 1 1 calc R . . C23 C 0.6401(4) 0.7071(3) 0.0971(3) 0.0585(14) Uani 1 1 d . . . H23A H 0.6239 0.6577 0.0893 0.088 Uiso 1 1 calc R . . H23B H 0.7377 0.7155 0.1093 0.088 Uiso 1 1 calc R . . H23C H 0.6057 0.7320 0.0495 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.02465(9) 0.01795(9) 0.01668(10) 0.00142(7) 0.00067(6) 0.00099(6) Si1 0.0288(5) 0.0239(6) 0.0279(6) 0.0033(5) 0.0024(4) -0.0024(4) Si2 0.0302(5) 0.0279(6) 0.0200(6) 0.0015(5) 0.0050(4) -0.0050(5) Si3 0.0283(6) 0.0316(7) 0.0559(9) 0.0029(6) 0.0118(5) 0.0022(5) Si4 0.0538(7) 0.0211(6) 0.0278(7) -0.0009(5) 0.0016(5) -0.0019(5) Si5 0.0381(6) 0.0357(7) 0.0280(6) -0.0012(6) 0.0060(5) 0.0142(5) N1 0.0214(14) 0.0220(17) 0.0251(18) 0.0031(14) 0.0016(12) 0.0034(12) N2 0.0268(15) 0.0212(17) 0.0272(18) -0.0034(15) 0.0072(12) -0.0018(12) N3 0.0380(17) 0.0192(17) 0.0191(17) 0.0012(14) 0.0025(12) 0.0070(13) C1 0.035(2) 0.025(2) 0.021(2) 0.0072(18) -0.0034(15) -0.0023(17) C2 0.037(2) 0.022(2) 0.026(2) 0.0073(19) -0.0068(16) -0.0012(17) C3 0.045(2) 0.028(2) 0.028(2) 0.007(2) -0.0106(17) -0.0020(19) C4 0.055(3) 0.028(2) 0.020(2) 0.0058(19) -0.0070(18) -0.004(2) C5 0.050(2) 0.024(2) 0.015(2) 0.0087(18) 0.0011(16) -0.0025(18) C6 0.041(2) 0.025(2) 0.051(3) 0.003(2) -0.0075(19) 0.0022(18) C7 0.045(2) 0.039(3) 0.050(3) 0.008(2) -0.022(2) -0.009(2) C8 0.078(3) 0.039(3) 0.023(2) -0.001(2) -0.001(2) -0.014(2) C9 0.064(3) 0.037(3) 0.034(3) 0.001(2) 0.017(2) 0.000(2) C10 0.039(2) 0.048(3) 0.044(3) 0.005(2) 0.0113(19) -0.005(2) C11 0.042(2) 0.025(2) 0.039(3) 0.006(2) -0.0026(17) -0.0056(18) C12 0.0238(19) 0.037(3) 0.031(2) 0.005(2) -0.0036(15) 0.0007(17) C13 0.037(2) 0.047(3) 0.040(3) 0.003(2) -0.0116(18) -0.012(2) C14 0.049(2) 0.045(3) 0.033(3) -0.012(2) -0.0044(18) -0.007(2) C15 0.034(2) 0.030(2) 0.029(2) -0.0021(19) 0.0080(16) -0.0007(17) C16 0.069(3) 0.052(3) 0.029(3) 0.002(2) 0.010(2) -0.022(2) C17 0.045(2) 0.034(3) 0.036(3) 0.007(2) 0.0042(18) -0.0058(19) C18 0.034(2) 0.055(3) 0.069(4) 0.015(3) 0.019(2) 0.002(2) C19 0.061(3) 0.042(3) 0.133(6) -0.026(3) 0.050(3) 0.005(2) C20 0.050(3) 0.039(3) 0.050(3) -0.005(2) -0.004(2) -0.011(2) C21 0.079(3) 0.037(3) 0.043(3) -0.010(2) 0.001(2) -0.003(2) C22 0.059(3) 0.068(4) 0.045(3) 0.005(3) 0.000(2) 0.035(3) C23 0.064(3) 0.065(4) 0.050(3) -0.007(3) 0.023(2) 0.016(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 Lu1 N2 2.216(3) . ? Lu1 N3 2.237(3) . ? Lu1 C1 2.550(4) . ? Lu1 N1 2.592(3) . ? Lu1 C2 2.612(4) . ? Lu1 C5 2.618(4) . ? Lu1 C4 2.707(4) . ? Lu1 C3 2.708(4) . ? Lu1 Si5 3.0249(11) . ? Lu1 Si2 3.0419(10) . ? Lu1 Si1 3.3210(11) . ? Lu1 H2 2.53(3) . ? Lu1 H5 2.50(3) . ? Si1 N1 1.816(3) . ? Si1 C1 1.859(4) . ? Si1 C11 1.865(4) . ? Si1 C10 1.870(4) . ? Si2 N2 1.709(3) . ? Si2 C17 1.859(4) . ? Si2 C16 1.873(4) . ? Si2 H2 1.47(3) . ? Si3 N2 1.710(3) . ? Si3 C19 1.866(5) . ? Si3 C18 1.877(4) . ? Si3 H3 1.42(4) . ? Si4 N3 1.705(3) . ? Si4 C20 1.869(4) . ? Si4 C21 1.876(5) . ? Si4 H4 1.51(4) . ? Si5 N3 1.683(3) . ? Si5 C22 1.857(4) . ? Si5 C23 1.864(4) . ? Si5 H5 1.49(4) . ? N1 C12 1.497(4) . ? N1 C15 1.513(4) . ? C1 C5 1.430(5) . ? C1 C2 1.437(5) . ? C2 C3 1.416(5) . ? C2 C6 1.511(5) . ? C3 C4 1.412(6) . ? C3 C7 1.512(5) . ? C4 C5 1.409(5) . ? C4 C8 1.504(6) . ? C5 C9 1.522(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.528(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.517(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.537(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? 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 Lu1 N3 99.30(11) . . ? N2 Lu1 C1 128.15(11) . . ? N3 Lu1 C1 128.27(11) . . ? N2 Lu1 N1 96.55(10) . . ? N3 Lu1 N1 134.52(9) . . ? C1 Lu1 N1 66.27(10) . . ? N2 Lu1 C2 100.90(11) . . ? N3 Lu1 C2 134.10(11) . . ? C1 Lu1 C2 32.29(11) . . ? N1 Lu1 C2 83.12(10) . . ? N2 Lu1 C5 151.84(11) . . ? N3 Lu1 C5 96.21(12) . . ? C1 Lu1 C5 32.09(12) . . ? N1 Lu1 C5 89.01(10) . . ? C2 Lu1 C5 52.25(12) . . ? N2 Lu1 C4 128.41(12) . . ? N3 Lu1 C4 84.45(11) . . ? C1 Lu1 C4 51.82(12) . . ? N1 Lu1 C4 117.07(11) . . ? C2 Lu1 C4 50.99(12) . . ? C5 Lu1 C4 30.64(11) . . ? N2 Lu1 C3 102.16(12) . . ? N3 Lu1 C3 104.48(11) . . ? C1 Lu1 C3 51.97(11) . . ? N1 Lu1 C3 113.36(10) . . ? C2 Lu1 C3 30.80(12) . . ? C5 Lu1 C3 50.92(12) . . ? C4 Lu1 C3 30.24(12) . . ? N2 Lu1 Si5 115.32(8) . . ? N3 Lu1 Si5 33.23(7) . . ? C1 Lu1 Si5 116.03(9) . . ? N1 Lu1 Si5 101.95(6) . . ? C2 Lu1 Si5 142.29(9) . . ? C5 Lu1 Si5 90.22(9) . . ? C4 Lu1 Si5 95.65(9) . . ? C3 Lu1 Si5 124.37(10) . . ? N2 Lu1 Si2 33.48(8) . . ? N3 Lu1 Si2 85.08(8) . . ? C1 Lu1 Si2 145.81(9) . . ? N1 Lu1 Si2 85.29(7) . . ? C2 Lu1 Si2 130.55(9) . . ? C5 Lu1 Si2 173.09(8) . . ? C4 Lu1 Si2 156.10(9) . . ? C3 Lu1 Si2 135.33(9) . . ? Si5 Lu1 Si2 87.15(3) . . ? N2 Lu1 Si1 119.25(8) . . ? N3 Lu1 Si1 137.94(8) . . ? C1 Lu1 Si1 33.79(8) . . ? N1 Lu1 Si1 32.94(7) . . ? C2 Lu1 Si1 57.65(8) . . ? C5 Lu1 Si1 57.45(9) . . ? C4 Lu1 Si1 84.17(9) . . ? C3 Lu1 Si1 84.37(9) . . ? Si5 Lu1 Si1 108.53(3) . . ? Si2 Lu1 Si1 117.49(3) . . ? N2 Lu1 H2 62.0(7) . . ? N3 Lu1 H2 77.9(8) . . ? C1 Lu1 H2 138.4(7) . . ? N1 Lu1 H2 72.7(7) . . ? C2 Lu1 H2 147.6(8) . . ? C5 Lu1 H2 145.0(7) . . ? C4 Lu1 H2 161.2(7) . . ? C3 Lu1 H2 164.0(7) . . ? Si5 Lu1 H2 65.9(7) . . ? Si2 Lu1 H2 28.7(6) . . ? Si1 Lu1 H2 104.6(7) . . ? N2 Lu1 H5 126.2(9) . . ? N3 Lu1 H5 62.5(9) . . ? C1 Lu1 H5 96.8(9) . . ? N1 Lu1 H5 73.7(9) . . ? C2 Lu1 H5 128.9(9) . . ? C5 Lu1 H5 81.9(9) . . ? C4 Lu1 H5 101.3(9) . . ? C3 Lu1 H5 130.7(9) . . ? Si5 Lu1 H5 29.4(9) . . ? Si2 Lu1 H5 92.7(9) . . ? Si1 Lu1 H5 80.4(9) . . ? H2 Lu1 H5 64.7(11) . . ? N1 Si1 C1 99.75(15) . . ? N1 Si1 C11 111.13(17) . . ? C1 Si1 C11 115.50(17) . . ? N1 Si1 C10 110.08(17) . . ? C1 Si1 C10 114.30(19) . . ? C11 Si1 C10 106.05(19) . . ? N1 Si1 Lu1 50.88(9) . . ? C1 Si1 Lu1 49.71(11) . . ? C11 Si1 Lu1 135.47(13) . . ? C10 Si1 Lu1 118.29(15) . . ? N2 Si2 C17 117.76(16) . . ? N2 Si2 C16 117.57(19) . . ? C17 Si2 C16 105.7(2) . . ? N2 Si2 Lu1 45.69(10) . . ? C17 Si2 Lu1 120.32(14) . . ? C16 Si2 Lu1 133.53(15) . . ? N2 Si2 H2 101.4(12) . . ? C17 Si2 H2 105.0(13) . . ? C16 Si2 H2 108.3(12) . . ? Lu1 Si2 H2 56.1(12) . . ? N2 Si3 C19 112.73(18) . . ? N2 Si3 C18 112.67(18) . . ? C19 Si3 C18 107.6(2) . . ? N2 Si3 H3 107.3(14) . . ? C19 Si3 H3 107.3(16) . . ? C18 Si3 H3 109.1(15) . . ? N3 Si4 C20 110.92(17) . . ? N3 Si4 C21 115.40(19) . . ? C20 Si4 C21 109.0(2) . . ? N3 Si4 H4 111.6(14) . . ? C20 Si4 H4 104.8(14) . . ? C21 Si4 H4 104.5(15) . . ? N3 Si5 C22 116.42(19) . . ? N3 Si5 C23 117.70(19) . . ? C22 Si5 C23 106.5(2) . . ? N3 Si5 Lu1 46.74(11) . . ? C22 Si5 Lu1 122.91(16) . . ? C23 Si5 Lu1 130.04(17) . . ? N3 Si5 H5 102.1(13) . . ? C22 Si5 H5 107.4(14) . . ? C23 Si5 H5 105.7(14) . . ? Lu1 Si5 H5 55.5(13) . . ? C12 N1 C15 103.3(3) . . ? C12 N1 Si1 117.0(2) . . ? C15 N1 Si1 113.1(2) . . ? C12 N1 Lu1 120.0(2) . . ? C15 N1 Lu1 107.50(19) . . ? Si1 N1 Lu1 96.18(12) . . ? Si2 N2 Si3 121.90(18) . . ? Si2 N2 Lu1 100.83(13) . . ? Si3 N2 Lu1 137.17(17) . . ? Si5 N3 Si4 126.47(19) . . ? Si5 N3 Lu1 100.04(14) . . ? Si4 N3 Lu1 132.78(15) . . ? C5 C1 C2 106.9(3) . . ? C5 C1 Si1 124.7(3) . . ? C2 C1 Si1 124.8(3) . . ? C5 C1 Lu1 76.6(2) . . ? C2 C1 Lu1 76.2(2) . . ? Si1 C1 Lu1 96.49(14) . . ? C3 C2 C1 108.0(3) . . ? C3 C2 C6 123.9(3) . . ? C1 C2 C6 127.7(3) . . ? C3 C2 Lu1 78.3(2) . . ? C1 C2 Lu1 71.48(19) . . ? C6 C2 Lu1 121.8(3) . . ? C4 C3 C2 108.2(3) . . ? C4 C3 C7 125.3(4) . . ? C2 C3 C7 125.7(4) . . ? C4 C3 Lu1 74.9(2) . . ? C2 C3 Lu1 70.9(2) . . ? C7 C3 Lu1 128.0(3) . . ? C5 C4 C3 108.6(4) . . ? C5 C4 C8 125.9(4) . . ? C3 C4 C8 125.2(4) . . ? C5 C4 Lu1 71.2(2) . . ? C3 C4 Lu1 74.9(2) . . ? C8 C4 Lu1 124.9(3) . . ? C4 C5 C1 108.3(3) . . ? C4 C5 C9 124.7(4) . . ? C1 C5 C9 126.8(3) . . ? C4 C5 Lu1 78.2(2) . . ? C1 C5 Lu1 71.3(2) . . ? C9 C5 Lu1 119.9(2) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 104.3(3) . . ? N1 C12 H12A 110.9 . . ? C13 C12 H12A 110.9 . . ? N1 C12 H12B 110.9 . . ? C13 C12 H12B 110.9 . . ? H12A C12 H12B 108.9 . . ? C14 C13 C12 104.4(3) . . ? C14 C13 H13A 110.9 . . ? C12 C13 H13A 110.9 . . ? C14 C13 H13B 110.9 . . ? C12 C13 H13B 110.9 . . ? H13A C13 H13B 108.9 . . ? C13 C14 C15 105.6(3) . . ? C13 C14 H14A 110.6 . . ? C15 C14 H14A 110.6 . . ? C13 C14 H14B 110.6 . . ? C15 C14 H14B 110.6 . . ? H14A C14 H14B 108.8 . . ? N1 C15 C14 106.9(3) . . ? N1 C15 H15A 110.3 . . ? C14 C15 H15A 110.3 . . ? N1 C15 H15B 110.3 . . ? C14 C15 H15B 110.3 . . ? H15A C15 H15B 108.6 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si4 C20 H20A 109.5 . . ? Si4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si4 C21 H21A 109.5 . . ? Si4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si5 C22 H22A 109.5 . . ? Si5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si5 C23 H23A 109.5 . . ? Si5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Lu1 Si1 N1 51.42(14) . . . . ? N3 Lu1 Si1 N1 -102.37(15) . . . . ? C1 Lu1 Si1 N1 167.3(2) . . . . ? C2 Lu1 Si1 N1 135.79(15) . . . . ? C5 Lu1 Si1 N1 -161.30(15) . . . . ? C4 Lu1 Si1 N1 -177.39(15) . . . . ? C3 Lu1 Si1 N1 152.21(14) . . . . ? Si5 Lu1 Si1 N1 -83.37(11) . . . . ? Si2 Lu1 Si1 N1 13.25(12) . . . . ? N2 Lu1 Si1 C1 -115.86(18) . . . . ? N3 Lu1 Si1 C1 90.35(19) . . . . ? N1 Lu1 Si1 C1 -167.3(2) . . . . ? C2 Lu1 Si1 C1 -31.49(18) . . . . ? C5 Lu1 Si1 C1 31.42(18) . . . . ? C4 Lu1 Si1 C1 15.32(18) . . . . ? C3 Lu1 Si1 C1 -15.07(18) . . . . ? Si5 Lu1 Si1 C1 109.35(16) . . . . ? Si2 Lu1 Si1 C1 -154.03(16) . . . . ? N2 Lu1 Si1 C11 -29.1(2) . . . . ? N3 Lu1 Si1 C11 177.1(2) . . . . ? C1 Lu1 Si1 C11 86.7(2) . . . . ? N1 Lu1 Si1 C11 -80.5(2) . . . . ? C2 Lu1 Si1 C11 55.2(2) . . . . ? C5 Lu1 Si1 C11 118.2(2) . . . . ? C4 Lu1 Si1 C11 102.1(2) . . . . ? C3 Lu1 Si1 C11 71.7(2) . . . . ? Si5 Lu1 Si1 C11 -163.92(18) . . . . ? Si2 Lu1 Si1 C11 -67.30(18) . . . . ? N2 Lu1 Si1 C10 145.13(18) . . . . ? N3 Lu1 Si1 C10 -8.65(19) . . . . ? C1 Lu1 Si1 C10 -99.0(2) . . . . ? N1 Lu1 Si1 C10 93.72(19) . . . . ? C2 Lu1 Si1 C10 -130.50(19) . . . . ? C5 Lu1 Si1 C10 -67.59(18) . . . . ? C4 Lu1 Si1 C10 -83.68(18) . . . . ? C3 Lu1 Si1 C10 -114.07(18) . . . . ? Si5 Lu1 Si1 C10 10.34(16) . . . . ? Si2 Lu1 Si1 C10 106.97(16) . . . . ? N3 Lu1 Si2 N2 -115.10(16) . . . . ? C1 Lu1 Si2 N2 76.5(2) . . . . ? N1 Lu1 Si2 N2 109.40(15) . . . . ? C2 Lu1 Si2 N2 32.62(17) . . . . ? C5 Lu1 Si2 N2 143.9(8) . . . . ? C4 Lu1 Si2 N2 -50.8(3) . . . . ? C3 Lu1 Si2 N2 -9.45(19) . . . . ? Si5 Lu1 Si2 N2 -148.35(14) . . . . ? Si1 Lu1 Si2 N2 102.22(14) . . . . ? N2 Lu1 Si2 C17 100.6(2) . . . . ? N3 Lu1 Si2 C17 -14.55(16) . . . . ? C1 Lu1 Si2 C17 177.09(19) . . . . ? N1 Lu1 Si2 C17 -150.05(16) . . . . ? C2 Lu1 Si2 C17 133.17(17) . . . . ? C5 Lu1 Si2 C17 -115.6(8) . . . . ? C4 Lu1 Si2 C17 49.7(3) . . . . ? C3 Lu1 Si2 C17 91.11(19) . . . . ? Si5 Lu1 Si2 C17 -47.79(14) . . . . ? Si1 Lu1 Si2 C17 -157.23(14) . . . . ? N2 Lu1 Si2 C16 -88.0(3) . . . . ? N3 Lu1 Si2 C16 156.9(2) . . . . ? C1 Lu1 Si2 C16 -11.4(3) . . . . ? N1 Lu1 Si2 C16 21.4(2) . . . . ? C2 Lu1 Si2 C16 -55.4(2) . . . . ? C5 Lu1 Si2 C16 55.9(8) . . . . ? C4 Lu1 Si2 C16 -138.8(3) . . . . ? C3 Lu1 Si2 C16 -97.4(2) . . . . ? Si5 Lu1 Si2 C16 123.7(2) . . . . ? Si1 Lu1 Si2 C16 14.2(2) . . . . ? N2 Lu1 Si5 N3 66.68(16) . . . . ? C1 Lu1 Si5 N3 -120.82(16) . . . . ? N1 Lu1 Si5 N3 169.93(15) . . . . ? C2 Lu1 Si5 N3 -95.84(19) . . . . ? C5 Lu1 Si5 N3 -101.04(16) . . . . ? C4 Lu1 Si5 N3 -70.83(16) . . . . ? C3 Lu1 Si5 N3 -60.59(17) . . . . ? Si2 Lu1 Si5 N3 85.36(14) . . . . ? Si1 Lu1 Si5 N3 -156.55(14) . . . . ? N2 Lu1 Si5 C22 -30.1(2) . . . . ? N3 Lu1 Si5 C22 -96.8(2) . . . . ? C1 Lu1 Si5 C22 142.4(2) . . . . ? N1 Lu1 Si5 C22 73.1(2) . . . . ? C2 Lu1 Si5 C22 167.3(2) . . . . ? C5 Lu1 Si5 C22 162.1(2) . . . . ? C4 Lu1 Si5 C22 -167.6(2) . . . . ? C3 Lu1 Si5 C22 -157.4(2) . . . . ? Si2 Lu1 Si5 C22 -11.5(2) . . . . ? Si1 Lu1 Si5 C22 106.6(2) . . . . ? N2 Lu1 Si5 C23 159.1(2) . . . . ? N3 Lu1 Si5 C23 92.5(3) . . . . ? C1 Lu1 Si5 C23 -28.4(2) . . . . ? N1 Lu1 Si5 C23 -97.6(2) . . . . ? C2 Lu1 Si5 C23 -3.4(3) . . . . ? C5 Lu1 Si5 C23 -8.6(2) . . . . ? C4 Lu1 Si5 C23 21.6(2) . . . . ? C3 Lu1 Si5 C23 31.9(2) . . . . ? Si2 Lu1 Si5 C23 177.8(2) . . . . ? Si1 Lu1 Si5 C23 -64.1(2) . . . . ? C1 Si1 N1 C12 138.0(3) . . . . ? C11 Si1 N1 C12 -99.6(3) . . . . ? C10 Si1 N1 C12 17.5(3) . . . . ? Lu1 Si1 N1 C12 128.2(3) . . . . ? C1 Si1 N1 C15 -102.2(2) . . . . ? C11 Si1 N1 C15 20.1(3) . . . . ? C10 Si1 N1 C15 137.3(2) . . . . ? Lu1 Si1 N1 C15 -112.0(2) . . . . ? C1 Si1 N1 Lu1 9.81(15) . . . . ? C11 Si1 N1 Lu1 132.14(14) . . . . ? C10 Si1 N1 Lu1 -110.68(17) . . . . ? N2 Lu1 N1 C12 97.3(2) . . . . ? N3 Lu1 N1 C12 -12.7(3) . . . . ? C1 Lu1 N1 C12 -133.8(3) . . . . ? C2 Lu1 N1 C12 -162.5(3) . . . . ? C5 Lu1 N1 C12 -110.4(3) . . . . ? C4 Lu1 N1 C12 -123.2(3) . . . . ? C3 Lu1 N1 C12 -156.4(2) . . . . ? Si5 Lu1 N1 C12 -20.4(2) . . . . ? Si2 Lu1 N1 C12 65.7(2) . . . . ? Si1 Lu1 N1 C12 -126.1(3) . . . . ? N2 Lu1 N1 C15 -20.1(2) . . . . ? N3 Lu1 N1 C15 -130.0(2) . . . . ? C1 Lu1 N1 C15 108.9(2) . . . . ? C2 Lu1 N1 C15 80.2(2) . . . . ? C5 Lu1 N1 C15 132.2(2) . . . . ? C4 Lu1 N1 C15 119.5(2) . . . . ? C3 Lu1 N1 C15 86.2(2) . . . . ? Si5 Lu1 N1 C15 -137.7(2) . . . . ? Si2 Lu1 N1 C15 -51.7(2) . . . . ? Si1 Lu1 N1 C15 116.6(3) . . . . ? N2 Lu1 N1 Si1 -136.64(12) . . . . ? N3 Lu1 N1 Si1 113.41(14) . . . . ? C1 Lu1 N1 Si1 -7.69(12) . . . . ? C2 Lu1 N1 Si1 -36.40(13) . . . . ? C5 Lu1 N1 Si1 15.68(13) . . . . ? C4 Lu1 N1 Si1 2.91(16) . . . . ? C3 Lu1 N1 Si1 -30.35(15) . . . . ? Si5 Lu1 N1 Si1 105.69(10) . . . . ? Si2 Lu1 N1 Si1 -168.23(10) . . . . ? C17 Si2 N2 Si3 76.5(3) . . . . ? C16 Si2 N2 Si3 -51.8(3) . . . . ? Lu1 Si2 N2 Si3 -177.0(3) . . . . ? C17 Si2 N2 Lu1 -106.46(18) . . . . ? C16 Si2 N2 Lu1 125.18(17) . . . . ? C19 Si3 N2 Si2 81.0(3) . . . . ? C18 Si3 N2 Si2 -41.1(3) . . . . ? C19 Si3 N2 Lu1 -94.7(3) . . . . ? C18 Si3 N2 Lu1 143.3(3) . . . . ? N3 Lu1 N2 Si2 66.09(14) . . . . ? C1 Lu1 N2 Si2 -135.98(13) . . . . ? N1 Lu1 N2 Si2 -71.12(14) . . . . ? C2 Lu1 N2 Si2 -155.35(13) . . . . ? C5 Lu1 N2 Si2 -171.35(19) . . . . ? C4 Lu1 N2 Si2 156.37(13) . . . . ? C3 Lu1 N2 Si2 173.22(14) . . . . ? Si5 Lu1 N2 Si2 35.44(15) . . . . ? Si1 Lu1 N2 Si2 -96.46(13) . . . . ? N3 Lu1 N2 Si3 -117.7(2) . . . . ? C1 Lu1 N2 Si3 40.3(3) . . . . ? N1 Lu1 N2 Si3 105.1(2) . . . . ? C2 Lu1 N2 Si3 20.9(3) . . . . ? C5 Lu1 N2 Si3 4.9(4) . . . . ? C4 Lu1 N2 Si3 -27.4(3) . . . . ? C3 Lu1 N2 Si3 -10.5(3) . . . . ? Si5 Lu1 N2 Si3 -148.3(2) . . . . ? Si2 Lu1 N2 Si3 176.2(3) . . . . ? Si1 Lu1 N2 Si3 79.8(2) . . . . ? C22 Si5 N3 Si4 -59.9(3) . . . . ? C23 Si5 N3 Si4 68.4(3) . . . . ? Lu1 Si5 N3 Si4 -171.3(3) . . . . ? C22 Si5 N3 Lu1 111.4(2) . . . . ? C23 Si5 N3 Lu1 -120.2(2) . . . . ? C20 Si4 N3 Si5 171.6(2) . . . . ? C21 Si4 N3 Si5 -63.8(3) . . . . ? C20 Si4 N3 Lu1 3.3(3) . . . . ? C21 Si4 N3 Lu1 127.8(2) . . . . ? N2 Lu1 N3 Si5 -122.73(14) . . . . ? C1 Lu1 N3 Si5 79.38(16) . . . . ? N1 Lu1 N3 Si5 -13.9(2) . . . . ? C2 Lu1 N3 Si5 122.09(15) . . . . ? C5 Lu1 N3 Si5 80.85(14) . . . . ? C4 Lu1 N3 Si5 109.20(15) . . . . ? C3 Lu1 N3 Si5 132.04(14) . . . . ? Si2 Lu1 N3 Si5 -92.32(12) . . . . ? Si1 Lu1 N3 Si5 34.28(19) . . . . ? N2 Lu1 N3 Si4 47.8(2) . . . . ? C1 Lu1 N3 Si4 -110.1(2) . . . . ? N1 Lu1 N3 Si4 156.61(17) . . . . ? C2 Lu1 N3 Si4 -67.4(3) . . . . ? C5 Lu1 N3 Si4 -108.7(2) . . . . ? C4 Lu1 N3 Si4 -80.3(2) . . . . ? C3 Lu1 N3 Si4 -57.5(2) . . . . ? Si5 Lu1 N3 Si4 170.5(3) . . . . ? Si2 Lu1 N3 Si4 78.2(2) . . . . ? Si1 Lu1 N3 Si4 -155.24(15) . . . . ? N1 Si1 C1 C5 -88.1(3) . . . . ? C11 Si1 C1 C5 152.7(3) . . . . ? C10 Si1 C1 C5 29.2(4) . . . . ? Lu1 Si1 C1 C5 -78.2(3) . . . . ? N1 Si1 C1 C2 67.7(3) . . . . ? C11 Si1 C1 C2 -51.4(4) . . . . ? C10 Si1 C1 C2 -174.9(3) . . . . ? Lu1 Si1 C1 C2 77.7(3) . . . . ? N1 Si1 C1 Lu1 -9.98(15) . . . . ? C11 Si1 C1 Lu1 -129.14(17) . . . . ? C10 Si1 C1 Lu1 107.40(19) . . . . ? N2 Lu1 C1 C5 -149.05(19) . . . . ? N3 Lu1 C1 C5 2.8(3) . . . . ? N1 Lu1 C1 C5 131.7(2) . . . . ? C2 Lu1 C1 C5 -111.5(3) . . . . ? C4 Lu1 C1 C5 -36.3(2) . . . . ? C3 Lu1 C1 C5 -75.0(2) . . . . ? Si5 Lu1 C1 C5 39.6(2) . . . . ? Si2 Lu1 C1 C5 167.93(15) . . . . ? Si1 Lu1 C1 C5 124.2(3) . . . . ? N2 Lu1 C1 C2 -37.5(3) . . . . ? N3 Lu1 C1 C2 114.3(2) . . . . ? N1 Lu1 C1 C2 -116.8(2) . . . . ? C5 Lu1 C1 C2 111.5(3) . . . . ? C4 Lu1 C1 C2 75.2(2) . . . . ? C3 Lu1 C1 C2 36.5(2) . . . . ? Si5 Lu1 C1 C2 151.08(19) . . . . ? Si2 Lu1 C1 C2 -80.6(2) . . . . ? Si1 Lu1 C1 C2 -124.3(3) . . . . ? N2 Lu1 C1 Si1 86.75(17) . . . . ? N3 Lu1 C1 Si1 -121.44(15) . . . . ? N1 Lu1 C1 Si1 7.51(12) . . . . ? C2 Lu1 C1 Si1 124.3(3) . . . . ? C5 Lu1 C1 Si1 -124.2(3) . . . . ? C4 Lu1 C1 Si1 -160.5(2) . . . . ? C3 Lu1 C1 Si1 160.8(2) . . . . ? Si5 Lu1 C1 Si1 -84.62(15) . . . . ? Si2 Lu1 C1 Si1 43.7(2) . . . . ? C5 C1 C2 C3 0.5(4) . . . . ? Si1 C1 C2 C3 -158.9(3) . . . . ? Lu1 C1 C2 C3 -70.5(3) . . . . ? C5 C1 C2 C6 -172.6(4) . . . . ? Si1 C1 C2 C6 28.0(5) . . . . ? Lu1 C1 C2 C6 116.3(4) . . . . ? C5 C1 C2 Lu1 71.1(2) . . . . ? Si1 C1 C2 Lu1 -88.4(3) . . . . ? N2 Lu1 C2 C3 -95.5(2) . . . . ? N3 Lu1 C2 C3 19.1(3) . . . . ? C1 Lu1 C2 C3 113.7(3) . . . . ? N1 Lu1 C2 C3 169.1(2) . . . . ? C5 Lu1 C2 C3 75.0(3) . . . . ? C4 Lu1 C2 C3 35.7(2) . . . . ? Si5 Lu1 C2 C3 68.5(3) . . . . ? Si2 Lu1 C2 C3 -113.1(2) . . . . ? Si1 Lu1 C2 C3 146.7(3) . . . . ? N2 Lu1 C2 C1 150.8(2) . . . . ? N3 Lu1 C2 C1 -94.6(2) . . . . ? N1 Lu1 C2 C1 55.4(2) . . . . ? C5 Lu1 C2 C1 -38.7(2) . . . . ? C4 Lu1 C2 C1 -78.0(2) . . . . ? C3 Lu1 C2 C1 -113.7(3) . . . . ? Si5 Lu1 C2 C1 -45.3(3) . . . . ? Si2 Lu1 C2 C1 133.16(19) . . . . ? Si1 Lu1 C2 C1 32.95(18) . . . . ? N2 Lu1 C2 C6 27.3(3) . . . . ? N3 Lu1 C2 C6 141.9(3) . . . . ? C1 Lu1 C2 C6 -123.5(4) . . . . ? N1 Lu1 C2 C6 -68.1(3) . . . . ? C5 Lu1 C2 C6 -162.2(3) . . . . ? C4 Lu1 C2 C6 158.5(3) . . . . ? C3 Lu1 C2 C6 122.8(4) . . . . ? Si5 Lu1 C2 C6 -168.8(2) . . . . ? Si2 Lu1 C2 C6 9.7(3) . . . . ? Si1 Lu1 C2 C6 -90.5(3) . . . . ? C1 C2 C3 C4 -0.2(4) . . . . ? C6 C2 C3 C4 173.2(4) . . . . ? Lu1 C2 C3 C4 -66.1(3) . . . . ? C1 C2 C3 C7 -170.5(4) . . . . ? C6 C2 C3 C7 2.9(6) . . . . ? Lu1 C2 C3 C7 123.5(4) . . . . ? C1 C2 C3 Lu1 65.9(2) . . . . ? C6 C2 C3 Lu1 -120.6(4) . . . . ? N2 Lu1 C3 C4 -153.2(2) . . . . ? N3 Lu1 C3 C4 -50.1(2) . . . . ? C1 Lu1 C3 C4 77.5(3) . . . . ? N1 Lu1 C3 C4 104.1(2) . . . . ? C2 Lu1 C3 C4 115.9(3) . . . . ? C5 Lu1 C3 C4 36.1(2) . . . . ? Si5 Lu1 C3 C4 -20.6(3) . . . . ? Si2 Lu1 C3 C4 -147.87(19) . . . . ? Si1 Lu1 C3 C4 88.1(2) . . . . ? N2 Lu1 C3 C2 90.9(2) . . . . ? N3 Lu1 C3 C2 -166.0(2) . . . . ? C1 Lu1 C3 C2 -38.4(2) . . . . ? N1 Lu1 C3 C2 -11.8(3) . . . . ? C5 Lu1 C3 C2 -79.8(3) . . . . ? C4 Lu1 C3 C2 -115.9(3) . . . . ? Si5 Lu1 C3 C2 -136.4(2) . . . . ? Si2 Lu1 C3 C2 96.3(2) . . . . ? Si1 Lu1 C3 C2 -27.8(2) . . . . ? N2 Lu1 C3 C7 -29.9(4) . . . . ? N3 Lu1 C3 C7 73.2(4) . . . . ? C1 Lu1 C3 C7 -159.3(4) . . . . ? N1 Lu1 C3 C7 -132.6(3) . . . . ? C2 Lu1 C3 C7 -120.9(5) . . . . ? C5 Lu1 C3 C7 159.4(4) . . . . ? C4 Lu1 C3 C7 123.3(5) . . . . ? Si5 Lu1 C3 C7 102.7(4) . . . . ? Si2 Lu1 C3 C7 -24.6(4) . . . . ? Si1 Lu1 C3 C7 -148.7(4) . . . . ? C2 C3 C4 C5 -0.2(4) . . . . ? C7 C3 C4 C5 170.2(4) . . . . ? Lu1 C3 C4 C5 -63.7(3) . . . . ? C2 C3 C4 C8 -174.2(4) . . . . ? C7 C3 C4 C8 -3.8(6) . . . . ? Lu1 C3 C4 C8 122.3(4) . . . . ? C2 C3 C4 Lu1 63.5(3) . . . . ? C7 C3 C4 Lu1 -126.1(4) . . . . ? N2 Lu1 C4 C5 150.4(2) . . . . ? N3 Lu1 C4 C5 -112.2(2) . . . . ? C1 Lu1 C4 C5 38.1(2) . . . . ? N1 Lu1 C4 C5 25.7(3) . . . . ? C2 Lu1 C4 C5 79.7(3) . . . . ? C3 Lu1 C4 C5 116.1(4) . . . . ? Si5 Lu1 C4 C5 -80.8(2) . . . . ? Si2 Lu1 C4 C5 -176.56(19) . . . . ? Si1 Lu1 C4 C5 27.3(2) . . . . ? N2 Lu1 C4 C3 34.2(3) . . . . ? N3 Lu1 C4 C3 131.7(2) . . . . ? C1 Lu1 C4 C3 -78.0(2) . . . . ? N1 Lu1 C4 C3 -90.4(2) . . . . ? C2 Lu1 C4 C3 -36.4(2) . . . . ? C5 Lu1 C4 C3 -116.1(4) . . . . ? Si5 Lu1 C4 C3 163.1(2) . . . . ? Si2 Lu1 C4 C3 67.3(3) . . . . ? Si1 Lu1 C4 C3 -88.8(2) . . . . ? N2 Lu1 C4 C8 -88.4(4) . . . . ? N3 Lu1 C4 C8 9.1(3) . . . . ? C1 Lu1 C4 C8 159.3(4) . . . . ? N1 Lu1 C4 C8 146.9(3) . . . . ? C2 Lu1 C4 C8 -159.0(4) . . . . ? C5 Lu1 C4 C8 121.2(5) . . . . ? C3 Lu1 C4 C8 -122.7(5) . . . . ? Si5 Lu1 C4 C8 40.4(3) . . . . ? Si2 Lu1 C4 C8 -55.3(5) . . . . ? Si1 Lu1 C4 C8 148.5(3) . . . . ? C3 C4 C5 C1 0.6(4) . . . . ? C8 C4 C5 C1 174.5(4) . . . . ? Lu1 C4 C5 C1 -65.6(2) . . . . ? C3 C4 C5 C9 -175.5(4) . . . . ? C8 C4 C5 C9 -1.6(6) . . . . ? Lu1 C4 C5 C9 118.3(4) . . . . ? C3 C4 C5 Lu1 66.1(3) . . . . ? C8 C4 C5 Lu1 -119.9(4) . . . . ? C2 C1 C5 C4 -0.7(4) . . . . ? Si1 C1 C5 C4 158.8(3) . . . . ? Lu1 C1 C5 C4 70.2(3) . . . . ? C2 C1 C5 C9 175.3(4) . . . . ? Si1 C1 C5 C9 -25.2(5) . . . . ? Lu1 C1 C5 C9 -113.8(4) . . . . ? C2 C1 C5 Lu1 -70.8(2) . . . . ? Si1 C1 C5 Lu1 88.6(3) . . . . ? N2 Lu1 C5 C4 -55.2(4) . . . . ? N3 Lu1 C5 C4 68.0(2) . . . . ? C1 Lu1 C5 C4 -114.2(3) . . . . ? N1 Lu1 C5 C4 -157.3(2) . . . . ? C2 Lu1 C5 C4 -75.2(2) . . . . ? C3 Lu1 C5 C4 -35.6(2) . . . . ? Si5 Lu1 C5 C4 100.8(2) . . . . ? Si2 Lu1 C5 C4 168.4(6) . . . . ? Si1 Lu1 C5 C4 -147.2(3) . . . . ? N2 Lu1 C5 C1 59.0(3) . . . . ? N3 Lu1 C5 C1 -177.8(2) . . . . ? N1 Lu1 C5 C1 -43.1(2) . . . . ? C2 Lu1 C5 C1 38.95(19) . . . . ? C4 Lu1 C5 C1 114.2(3) . . . . ? C3 Lu1 C5 C1 78.5(2) . . . . ? Si5 Lu1 C5 C1 -145.07(19) . . . . ? Si2 Lu1 C5 C1 -77.5(8) . . . . ? Si1 Lu1 C5 C1 -33.08(17) . . . . ? N2 Lu1 C5 C9 -178.6(3) . . . . ? N3 Lu1 C5 C9 -55.4(3) . . . . ? C1 Lu1 C5 C9 122.4(4) . . . . ? N1 Lu1 C5 C9 79.3(3) . . . . ? C2 Lu1 C5 C9 161.3(4) . . . . ? C4 Lu1 C5 C9 -123.5(4) . . . . ? C3 Lu1 C5 C9 -159.1(4) . . . . ? Si5 Lu1 C5 C9 -22.7(3) . . . . ? Si2 Lu1 C5 C9 44.9(9) . . . . ? Si1 Lu1 C5 C9 89.3(3) . . . . ? C15 N1 C12 C13 -39.2(4) . . . . ? Si1 N1 C12 C13 85.6(3) . . . . ? Lu1 N1 C12 C13 -158.7(2) . . . . ? N1 C12 C13 C14 36.4(4) . . . . ? C12 C13 C14 C15 -18.8(4) . . . . ? C12 N1 C15 C14 27.4(4) . . . . ? Si1 N1 C15 C14 -99.9(3) . . . . ? Lu1 N1 C15 C14 155.2(3) . . . . ? C13 C14 C15 N1 -5.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.244 _refine_diff_density_min -1.089 _refine_diff_density_rms 0.104 _database_code_depnum_ccdc_archive 'CCDC 917599'