# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_aa _database_code_depnum_ccdc_archive 'CCDC 857396' #TrackingRef 'Lu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H74 Lu N3 Si2' _chemical_formula_weight 984.30 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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3938(8) _cell_length_b 18.7363(12) _cell_length_c 20.5867(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.4890(10) _cell_angle_gamma 90.00 _cell_volume 5122.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9833 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.35 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 2.010 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4649 _exptl_absorpt_correction_T_max 0.4857 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24877 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8997 _reflns_number_gt 8511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+2.5289P] 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 8997 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.242326(8) 0.844955(6) 0.296364(5) 0.01234(7) Uani 1 1 d . . . N1 N 0.06881(16) 0.81597(12) 0.26881(11) 0.0162(5) Uani 1 1 d . . . N2 N 0.22438(17) 0.82411(13) 0.18842(11) 0.0154(4) Uani 1 1 d . . . N3 N 0.41085(18) 0.84514(10) 0.26771(12) 0.0148(5) Uani 1 1 d . . . Si1 Si 0.26797(6) 1.01308(4) 0.39637(4) 0.01857(17) Uani 1 1 d . . . Si2 Si 0.28349(6) 0.67608(5) 0.39244(4) 0.02131(17) Uani 1 1 d . . . C1 C 0.2179(2) 0.96461(15) 0.32133(14) 0.0199(6) Uani 1 1 d . . . H1A H 0.2403 0.9914 0.2856 0.024 Uiso 1 1 calc R . . H1B H 0.1454 0.9709 0.3172 0.024 Uiso 1 1 calc R . . C2 C 0.1673(3) 1.0262(2) 0.45005(17) 0.0360(8) Uani 1 1 d . . . H2A H 0.1124 1.0524 0.4266 0.054 Uiso 1 1 calc R . . H2B H 0.1941 1.0524 0.4885 0.054 Uiso 1 1 calc R . . H2C H 0.1435 0.9805 0.4627 0.054 Uiso 1 1 calc R . . C3 C 0.3733(2) 0.96554(17) 0.44715(15) 0.0280(7) Uani 1 1 d . . . H3A H 0.3513 0.9188 0.4580 0.042 Uiso 1 1 calc R . . H3B H 0.3932 0.9920 0.4866 0.042 Uiso 1 1 calc R . . H3C H 0.4296 0.9614 0.4228 0.042 Uiso 1 1 calc R . . C4 C 0.3220(3) 1.10256(17) 0.37788(17) 0.0360(8) Uani 1 1 d . . . H4A H 0.3829 1.0957 0.3587 0.054 Uiso 1 1 calc R . . H4B H 0.3364 1.1294 0.4177 0.054 Uiso 1 1 calc R . . H4C H 0.2741 1.1281 0.3478 0.054 Uiso 1 1 calc R . . C5 C 0.2698(2) 0.77359(15) 0.39056(14) 0.0197(6) Uani 1 1 d . . . H5A H 0.3302 0.7922 0.4160 0.024 Uiso 1 1 calc R . . H5B H 0.2148 0.7841 0.4154 0.024 Uiso 1 1 calc R . . C6 C 0.3195(3) 0.64292(18) 0.31275(19) 0.0372(9) Uani 1 1 d . . . H6A H 0.2688 0.6566 0.2776 0.056 Uiso 1 1 calc R . . H6B H 0.3252 0.5918 0.3141 0.056 Uiso 1 1 calc R . . H6C H 0.3830 0.6634 0.3057 0.056 Uiso 1 1 calc R . . C7 C 0.1623(2) 0.63258(18) 0.40686(16) 0.0291(7) Uani 1 1 d . . . H7A H 0.1499 0.6416 0.4510 0.044 Uiso 1 1 calc R . . H7B H 0.1669 0.5820 0.4001 0.044 Uiso 1 1 calc R . . H7C H 0.1081 0.6518 0.3768 0.044 Uiso 1 1 calc R . . C8 C 0.3841(3) 0.6415(2) 0.4569(2) 0.0398(9) Uani 1 1 d . . . H8A H 0.4491 0.6543 0.4457 0.060 Uiso 1 1 calc R . . H8B H 0.3791 0.5905 0.4594 0.060 Uiso 1 1 calc R . . H8C H 0.3754 0.6620 0.4985 0.060 Uiso 1 1 calc R . . C9 C 0.00525(19) 0.76608(15) 0.29853(13) 0.0179(6) Uani 1 1 d . . . C10 C -0.0171(2) 0.70082(16) 0.26631(15) 0.0238(6) Uani 1 1 d . . . C11 C -0.0836(3) 0.65493(15) 0.29261(19) 0.0292(8) Uani 1 1 d . . . H11 H -0.1017 0.6120 0.2716 0.035 Uiso 1 1 calc R . . C12 C -0.1227(2) 0.67236(18) 0.34938(17) 0.0299(7) Uani 1 1 d . . . H12 H -0.1677 0.6415 0.3658 0.036 Uiso 1 1 calc R . . C13 C -0.0955(2) 0.73493(17) 0.38171(15) 0.0266(7) Uani 1 1 d . . . H13 H -0.1210 0.7452 0.4206 0.032 Uiso 1 1 calc R . . C14 C -0.0303(2) 0.78367(15) 0.35744(14) 0.0199(6) Uani 1 1 d . . . C15 C 0.0304(2) 0.68007(18) 0.20594(16) 0.0302(7) Uani 1 1 d . . . H15 H 0.0923 0.7081 0.2063 0.036 Uiso 1 1 calc R . . C16 C -0.0381(3) 0.6981(2) 0.14267(17) 0.0421(9) Uani 1 1 d . . . H16A H -0.1015 0.6741 0.1424 0.063 Uiso 1 1 calc R . . H16B H -0.0068 0.6828 0.1057 0.063 Uiso 1 1 calc R . . H16C H -0.0490 0.7487 0.1402 0.063 Uiso 1 1 calc R . . C17 C 0.0601(3) 0.60071(19) 0.2068(2) 0.0429(9) Uani 1 1 d . . . H17A H 0.0978 0.5891 0.2483 0.064 Uiso 1 1 calc R . . H17B H 0.1006 0.5916 0.1725 0.064 Uiso 1 1 calc R . . H17C H 0.0004 0.5719 0.2000 0.064 Uiso 1 1 calc R . . C18 C -0.0009(2) 0.85312(16) 0.39297(15) 0.0218(6) Uani 1 1 d . . . H18 H 0.0641 0.8681 0.3806 0.026 Uiso 1 1 calc R . . C19 C -0.0769(2) 0.91230(18) 0.37277(16) 0.0309(7) Uani 1 1 d . . . H19A H -0.0837 0.9184 0.3261 0.046 Uiso 1 1 calc R . . H19B H -0.0537 0.9561 0.3938 0.046 Uiso 1 1 calc R . . H19C H -0.1409 0.8997 0.3857 0.046 Uiso 1 1 calc R . . C20 C 0.0120(3) 0.84380(17) 0.46734(17) 0.0311(8) Uani 1 1 d . . . H20A H -0.0524 0.8348 0.4814 0.047 Uiso 1 1 calc R . . H20B H 0.0405 0.8865 0.4879 0.047 Uiso 1 1 calc R . . H20C H 0.0561 0.8042 0.4794 0.047 Uiso 1 1 calc R . . C21 C 0.0225(2) 0.85412(14) 0.22221(14) 0.0173(6) Uani 1 1 d . . . H21 H -0.0474 0.8555 0.2187 0.021 Uiso 1 1 calc R . . C22 C 0.0697(2) 0.89511(15) 0.17462(13) 0.0181(6) Uani 1 1 d . . . C23 C 0.0141(2) 0.95135(16) 0.14238(15) 0.0227(6) Uani 1 1 d . . . H23 H -0.0459 0.9653 0.1568 0.027 Uiso 1 1 calc R . . C24 C 0.0461(2) 0.98624(17) 0.09026(15) 0.0262(6) Uani 1 1 d . . . H24 H 0.0101 1.0249 0.0709 0.031 Uiso 1 1 calc R . . C25 C 0.1337(2) 0.96260(16) 0.06669(15) 0.0256(6) Uani 1 1 d . . . H25 H 0.1543 0.9843 0.0301 0.031 Uiso 1 1 calc R . . C26 C 0.1899(2) 0.90737(15) 0.09714(14) 0.0212(6) Uani 1 1 d . . . H26 H 0.2477 0.8924 0.0806 0.025 Uiso 1 1 calc R . . C27 C 0.1614(2) 0.87341(14) 0.15262(13) 0.0162(5) Uani 1 1 d . . . C28 C 0.2777(2) 0.77642(14) 0.15437(13) 0.0164(5) Uani 1 1 d . . . C29 C 0.2318(2) 0.73865(15) 0.10004(13) 0.0199(6) Uani 1 1 d . . . H29 H 0.1653 0.7489 0.0837 0.024 Uiso 1 1 calc R . . C30 C 0.2825(2) 0.68633(16) 0.06979(14) 0.0228(6) Uani 1 1 d . . . H30 H 0.2492 0.6611 0.0346 0.027 Uiso 1 1 calc R . . C31 C 0.3834(2) 0.67134(16) 0.09188(15) 0.0226(6) Uani 1 1 d . . . H31 H 0.4174 0.6360 0.0718 0.027 Uiso 1 1 calc R . . C32 C 0.4313(2) 0.70919(15) 0.14323(14) 0.0206(6) Uani 1 1 d . . . H32 H 0.4991 0.7003 0.1570 0.025 Uiso 1 1 calc R . . C33 C 0.3810(2) 0.76155(14) 0.17626(13) 0.0164(5) Uani 1 1 d . . . C34 C 0.4416(2) 0.80519(15) 0.22372(13) 0.0172(6) Uani 1 1 d . . . H34 H 0.5107 0.8043 0.2223 0.021 Uiso 1 1 calc R . . C35 C 0.48610(19) 0.89487(14) 0.29849(13) 0.0169(5) Uani 1 1 d . . . C36 C 0.4897(2) 0.96267(15) 0.26911(15) 0.0210(6) Uani 1 1 d . . . C37 C 0.5616(2) 1.01055(17) 0.29808(16) 0.0268(7) Uani 1 1 d . . . H37 H 0.5646 1.0562 0.2808 0.032 Uiso 1 1 calc R . . C38 C 0.6284(2) 0.99149(17) 0.35197(16) 0.0272(7) Uani 1 1 d . . . H38 H 0.6769 1.0238 0.3700 0.033 Uiso 1 1 calc R . . C39 C 0.6234(2) 0.92462(17) 0.37921(15) 0.0242(6) Uani 1 1 d . . . H39 H 0.6690 0.9125 0.4155 0.029 Uiso 1 1 calc R . . C40 C 0.5519(2) 0.87487(16) 0.35370(14) 0.0190(6) Uani 1 1 d . . . C41 C 0.4206(2) 0.98132(16) 0.20675(15) 0.0249(6) Uani 1 1 d . . . H41 H 0.3598 0.9520 0.2056 0.030 Uiso 1 1 calc R . . C42 C 0.4710(3) 0.96259(19) 0.14627(16) 0.0335(8) Uani 1 1 d . . . H42A H 0.5301 0.9914 0.1457 0.050 Uiso 1 1 calc R . . H42B H 0.4248 0.9715 0.1074 0.050 Uiso 1 1 calc R . . H42C H 0.4896 0.9131 0.1479 0.050 Uiso 1 1 calc R . . C43 C 0.3876(3) 1.05970(18) 0.20230(19) 0.0364(8) Uani 1 1 d . . . H43A H 0.3602 1.0728 0.2415 0.055 Uiso 1 1 calc R . . H43B H 0.3372 1.0660 0.1651 0.055 Uiso 1 1 calc R . . H43C H 0.4446 1.0893 0.1976 0.055 Uiso 1 1 calc R . . C44 C 0.5462(2) 0.80143(16) 0.38425(14) 0.0221(6) Uani 1 1 d . . . H44 H 0.4778 0.7832 0.3720 0.026 Uiso 1 1 calc R . . C45 C 0.5663(3) 0.80387(19) 0.45914(15) 0.0318(7) Uani 1 1 d . . . H45A H 0.6357 0.8155 0.4726 0.048 Uiso 1 1 calc R . . H45B H 0.5516 0.7581 0.4766 0.048 Uiso 1 1 calc R . . H45C H 0.5241 0.8395 0.4752 0.048 Uiso 1 1 calc R . . C46 C 0.6190(3) 0.74907(17) 0.35851(16) 0.0314(7) Uani 1 1 d . . . H46A H 0.6004 0.7423 0.3123 0.047 Uiso 1 1 calc R . . H46B H 0.6162 0.7041 0.3806 0.047 Uiso 1 1 calc R . . H46C H 0.6862 0.7678 0.3664 0.047 Uiso 1 1 calc R . . C47 C 0.2736(4) 0.3721(2) 0.4058(2) 0.0527(11) Uani 1 1 d . . . C48 C 0.2785(3) 0.3050(2) 0.3766(2) 0.0495(10) Uani 1 1 d . . . H48 H 0.2850 0.2644 0.4028 0.059 Uiso 1 1 calc R . . C49 C 0.2737(3) 0.2978(2) 0.30988(18) 0.0370(8) Uani 1 1 d . . . H49 H 0.2772 0.2528 0.2913 0.044 Uiso 1 1 calc R . . C50 C 0.2638(3) 0.3569(2) 0.2710(2) 0.0403(9) Uani 1 1 d . . . H50 H 0.2607 0.3523 0.2258 0.048 Uiso 1 1 calc R . . C51 C 0.2586(3) 0.4239(2) 0.2987(2) 0.0423(10) Uani 1 1 d . . . H51 H 0.2516 0.4643 0.2721 0.051 Uiso 1 1 calc R . . C52 C 0.2636(3) 0.4307(2) 0.3651(2) 0.0466(10) Uani 1 1 d . . . H52 H 0.2602 0.4760 0.3833 0.056 Uiso 1 1 calc R . . C53 C 0.2778(6) 0.3785(4) 0.4777(3) 0.101(2) Uiso 1 1 d . . . H53A H 0.3135 0.4212 0.4923 0.152 Uiso 1 1 calc R . . H53B H 0.3121 0.3379 0.4984 0.152 Uiso 1 1 calc R . . H53C H 0.2107 0.3806 0.4891 0.152 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 0.01131(9) 0.01438(9) 0.01138(9) -0.00169(3) 0.00171(5) 0.00014(4) N1 0.0146(11) 0.0193(12) 0.0152(11) -0.0032(9) 0.0046(9) -0.0020(9) N2 0.0124(11) 0.0209(11) 0.0125(11) -0.0001(9) -0.0004(9) 0.0016(10) N3 0.0111(12) 0.0148(12) 0.0185(13) 0.0001(8) 0.0013(10) -0.0002(8) Si1 0.0186(4) 0.0175(4) 0.0193(4) -0.0049(3) 0.0014(3) 0.0012(3) Si2 0.0207(4) 0.0198(4) 0.0240(4) 0.0048(3) 0.0049(3) 0.0021(3) C1 0.0185(14) 0.0199(14) 0.0214(14) -0.0004(11) 0.0030(11) 0.0006(11) C2 0.0275(17) 0.050(2) 0.0308(18) -0.0113(16) 0.0060(14) 0.0047(15) C3 0.0250(16) 0.0319(17) 0.0258(16) -0.0069(13) -0.0021(12) 0.0058(13) C4 0.048(2) 0.0214(16) 0.0369(19) -0.0038(14) -0.0003(15) -0.0074(15) C5 0.0181(14) 0.0210(14) 0.0202(14) 0.0007(11) 0.0027(11) 0.0021(11) C6 0.045(2) 0.0283(17) 0.042(2) -0.0028(15) 0.0203(18) 0.0001(16) C7 0.0277(17) 0.0289(16) 0.0315(17) 0.0078(14) 0.0066(13) -0.0006(14) C8 0.034(2) 0.0353(18) 0.048(2) 0.0157(17) -0.0048(17) 0.0036(16) C9 0.0108(12) 0.0234(14) 0.0194(14) 0.0018(11) 0.0017(10) -0.0013(11) C10 0.0179(14) 0.0274(15) 0.0264(15) -0.0014(12) 0.0041(12) -0.0018(12) C11 0.0242(18) 0.0264(18) 0.037(2) -0.0013(12) 0.0046(15) -0.0071(12) C12 0.0212(16) 0.0320(16) 0.0378(19) 0.0083(15) 0.0087(14) -0.0054(14) C13 0.0193(15) 0.0376(18) 0.0242(15) 0.0056(13) 0.0072(12) 0.0009(13) C14 0.0143(13) 0.0244(15) 0.0215(14) 0.0033(12) 0.0037(11) 0.0016(11) C15 0.0285(17) 0.0319(17) 0.0319(17) -0.0121(14) 0.0108(14) -0.0125(14) C16 0.044(2) 0.052(2) 0.0316(19) -0.0112(17) 0.0066(15) -0.0141(18) C17 0.044(2) 0.0330(19) 0.054(2) -0.0203(17) 0.0161(18) -0.0080(16) C18 0.0185(15) 0.0302(16) 0.0172(15) -0.0015(11) 0.0047(12) -0.0002(12) C19 0.0286(17) 0.0353(18) 0.0283(17) -0.0041(14) 0.0019(13) 0.0059(14) C20 0.033(2) 0.043(2) 0.0184(17) -0.0007(12) 0.0040(14) 0.0004(13) C21 0.0109(14) 0.0244(14) 0.0163(14) -0.0042(11) 0.0009(11) 0.0015(10) C22 0.0160(13) 0.0214(14) 0.0168(13) -0.0037(11) 0.0021(10) 0.0008(11) C23 0.0189(14) 0.0260(15) 0.0226(15) -0.0011(12) 0.0010(11) 0.0060(12) C24 0.0285(16) 0.0255(15) 0.0237(15) 0.0038(12) 0.0003(12) 0.0079(13) C25 0.0294(16) 0.0283(16) 0.0193(14) 0.0051(12) 0.0040(12) 0.0002(13) C26 0.0178(14) 0.0263(15) 0.0204(14) -0.0023(12) 0.0052(11) -0.0001(12) C27 0.0145(13) 0.0172(13) 0.0163(13) -0.0037(11) -0.0005(10) -0.0007(11) C28 0.0150(13) 0.0184(13) 0.0166(13) 0.0015(11) 0.0056(10) -0.0007(11) C29 0.0175(14) 0.0260(15) 0.0163(13) -0.0017(11) 0.0023(10) 0.0010(12) C30 0.0263(15) 0.0256(16) 0.0166(14) -0.0057(12) 0.0031(11) -0.0021(12) C31 0.0285(16) 0.0205(13) 0.0202(15) -0.0036(12) 0.0084(12) 0.0039(13) C32 0.0187(14) 0.0217(14) 0.0223(14) 0.0007(12) 0.0054(11) 0.0038(11) C33 0.0155(13) 0.0178(13) 0.0163(13) -0.0005(10) 0.0029(10) 0.0001(11) C34 0.0119(13) 0.0214(14) 0.0181(13) 0.0011(11) 0.0016(10) 0.0017(11) C35 0.0109(12) 0.0217(14) 0.0189(13) -0.0059(11) 0.0045(10) -0.0010(11) C36 0.0159(14) 0.0198(14) 0.0286(16) -0.0027(12) 0.0080(12) 0.0005(11) C37 0.0224(15) 0.0226(15) 0.0368(18) -0.0041(13) 0.0092(13) -0.0045(12) C38 0.0188(15) 0.0302(16) 0.0329(17) -0.0139(13) 0.0046(12) -0.0078(13) C39 0.0151(14) 0.0310(16) 0.0258(15) -0.0079(13) 0.0007(11) 0.0014(12) C40 0.0136(13) 0.0238(15) 0.0197(14) -0.0049(12) 0.0028(11) 0.0023(11) C41 0.0188(14) 0.0226(15) 0.0336(17) 0.0054(13) 0.0046(12) -0.0024(12) C42 0.0323(18) 0.0403(19) 0.0279(17) 0.0060(15) 0.0037(14) -0.0022(15) C43 0.0329(18) 0.0277(17) 0.049(2) 0.0122(15) 0.0054(15) 0.0036(14) C44 0.0163(14) 0.0261(15) 0.0226(15) -0.0011(12) -0.0023(11) 0.0003(12) C45 0.0346(18) 0.0375(18) 0.0226(16) 0.0009(13) 0.0007(13) 0.0075(15) C46 0.0376(19) 0.0267(16) 0.0294(17) -0.0019(13) 0.0030(14) 0.0073(14) C47 0.061(3) 0.047(2) 0.048(2) -0.003(2) 0.004(2) 0.026(2) C48 0.068(3) 0.036(2) 0.046(2) 0.0096(18) 0.011(2) 0.017(2) C49 0.0348(18) 0.0351(19) 0.041(2) -0.0037(16) 0.0061(15) 0.0016(16) C50 0.0205(18) 0.055(2) 0.047(2) 0.0087(18) 0.0102(16) 0.0054(16) C51 0.0287(18) 0.039(2) 0.061(3) 0.0203(18) 0.0114(17) 0.0014(16) C52 0.034(2) 0.0289(19) 0.076(3) -0.0054(19) 0.0026(18) 0.0046(16) _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 2.238(2) . ? Lu1 C1 2.333(3) . ? Lu1 C5 2.345(3) . ? Lu1 N1 2.382(2) . ? Lu1 N3 2.406(2) . ? N1 C21 1.289(4) . ? N1 C9 1.452(3) . ? N2 C28 1.390(3) . ? N2 C27 1.395(4) . ? N3 C34 1.283(4) . ? N3 C35 1.456(3) . ? Si1 C1 1.842(3) . ? Si1 C2 1.868(3) . ? Si1 C3 1.869(3) . ? Si1 C4 1.884(3) . ? Si2 C5 1.836(3) . ? Si2 C7 1.874(3) . ? Si2 C6 1.875(4) . ? Si2 C8 1.879(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? 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 C14 1.399(4) . ? C9 C10 1.405(4) . ? C10 C11 1.396(4) . ? C10 C15 1.519(4) . ? C11 C12 1.381(5) . ? C11 H11 0.9300 . ? C12 C13 1.374(5) . ? C12 H12 0.9300 . ? C13 C14 1.400(4) . ? C13 H13 0.9300 . ? C14 C18 1.519(4) . ? C15 C16 1.530(5) . ? C15 C17 1.539(5) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.525(4) . ? C18 C20 1.528(4) . ? C18 H18 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.453(4) . ? C21 H21 0.9300 . ? C22 C23 1.406(4) . ? C22 C27 1.422(4) . ? C23 C24 1.372(4) . ? C23 H23 0.9300 . ? C24 C25 1.399(4) . ? C24 H24 0.9300 . ? C25 C26 1.381(4) . ? C25 H25 0.9300 . ? C26 C27 1.403(4) . ? C26 H26 0.9300 . ? C28 C29 1.397(4) . ? C28 C33 1.425(4) . ? C29 C30 1.386(4) . ? C29 H29 0.9300 . ? C30 C31 1.397(4) . ? C30 H30 0.9300 . ? C31 C32 1.362(4) . ? C31 H31 0.9300 . ? C32 C33 1.414(4) . ? C32 H32 0.9300 . ? C33 C34 1.440(4) . ? C34 H34 0.9300 . ? C35 C40 1.396(4) . ? C35 C36 1.410(4) . ? C36 C37 1.392(4) . ? C36 C41 1.522(4) . ? C37 C38 1.378(5) . ? C37 H37 0.9300 . ? C38 C39 1.378(5) . ? C38 H38 0.9300 . ? C39 C40 1.389(4) . ? C39 H39 0.9300 . ? C40 C44 1.519(4) . ? C41 C42 1.533(4) . ? C41 C43 1.533(4) . ? C41 H41 0.9800 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C46 1.526(4) . ? C44 C45 1.531(4) . ? C44 H44 0.9800 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C52 1.376(6) . ? C47 C48 1.399(6) . ? C47 C53 1.479(8) . ? C48 C49 1.373(5) . ? C48 H48 0.9300 . ? C49 C50 1.363(5) . ? C49 H49 0.9300 . ? C50 C51 1.385(6) . ? C50 H50 0.9300 . ? C51 C52 1.366(6) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Lu1 C1 112.74(9) . . ? N2 Lu1 C5 134.96(9) . . ? C1 Lu1 C5 112.17(10) . . ? N2 Lu1 N1 75.44(8) . . ? C1 Lu1 N1 96.36(9) . . ? C5 Lu1 N1 96.31(9) . . ? N2 Lu1 N3 74.91(8) . . ? C1 Lu1 N3 102.47(8) . . ? C5 Lu1 N3 98.77(9) . . ? N1 Lu1 N3 149.23(8) . . ? C21 N1 C9 114.8(2) . . ? C21 N1 Lu1 114.24(18) . . ? C9 N1 Lu1 130.83(17) . . ? C28 N2 C27 118.3(2) . . ? C28 N2 Lu1 128.12(18) . . ? C27 N2 Lu1 112.84(17) . . ? C34 N3 C35 114.4(2) . . ? C34 N3 Lu1 124.71(19) . . ? C35 N3 Lu1 120.84(16) . . ? C1 Si1 C2 110.41(15) . . ? C1 Si1 C3 113.59(13) . . ? C2 Si1 C3 106.41(16) . . ? C1 Si1 C4 112.13(14) . . ? C2 Si1 C4 109.16(17) . . ? C3 Si1 C4 104.80(16) . . ? C5 Si2 C7 110.49(14) . . ? C5 Si2 C6 110.35(15) . . ? C7 Si2 C6 108.74(17) . . ? C5 Si2 C8 114.76(16) . . ? C7 Si2 C8 107.09(16) . . ? C6 Si2 C8 105.13(19) . . ? Si1 C1 Lu1 127.76(14) . . ? Si1 C1 H1A 105.4 . . ? Lu1 C1 H1A 105.4 . . ? Si1 C1 H1B 105.4 . . ? Lu1 C1 H1B 105.4 . . ? H1A C1 H1B 106.0 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 Lu1 126.11(14) . . ? Si2 C5 H5A 105.8 . . ? Lu1 C5 H5A 105.8 . . ? Si2 C5 H5B 105.8 . . ? Lu1 C5 H5B 105.8 . . ? H5A C5 H5B 106.2 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 122.6(3) . . ? C14 C9 N1 119.9(2) . . ? C10 C9 N1 117.5(2) . . ? C11 C10 C9 117.4(3) . . ? C11 C10 C15 121.1(3) . . ? C9 C10 C15 121.5(3) . . ? C12 C11 C10 120.9(3) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 121.5(3) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C9 C14 C13 117.0(3) . . ? C9 C14 C18 121.6(3) . . ? C13 C14 C18 121.4(3) . . ? C10 C15 C16 111.8(3) . . ? C10 C15 C17 111.9(3) . . ? C16 C15 C17 110.4(3) . . ? C10 C15 H15 107.5 . . ? C16 C15 H15 107.5 . . ? C17 C15 H15 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C19 111.7(3) . . ? C14 C18 C20 111.9(2) . . ? C19 C18 C20 109.9(3) . . ? C14 C18 H18 107.7 . . ? C19 C18 H18 107.7 . . ? C20 C18 H18 107.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 C22 125.9(3) . . ? N1 C21 H21 117.1 . . ? C22 C21 H21 117.1 . . ? C23 C22 C27 119.3(3) . . ? C23 C22 C21 117.7(2) . . ? C27 C22 C21 122.2(2) . . ? C24 C23 C22 121.8(3) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 118.8(3) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C26 C25 C24 120.8(3) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 121.3(3) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? N2 C27 C26 121.3(2) . . ? N2 C27 C22 120.6(2) . . ? C26 C27 C22 117.9(2) . . ? N2 C28 C29 121.9(2) . . ? N2 C28 C33 120.5(2) . . ? C29 C28 C33 117.5(2) . . ? C30 C29 C28 121.8(3) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C29 C30 C31 120.4(3) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C32 C31 C30 119.1(3) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C33 121.9(3) . . ? C31 C32 H32 119.0 . . ? C33 C32 H32 119.0 . . ? C32 C33 C28 119.2(2) . . ? C32 C33 C34 117.3(2) . . ? C28 C33 C34 122.8(2) . . ? N3 C34 C33 127.3(3) . . ? N3 C34 H34 116.4 . . ? C33 C34 H34 116.4 . . ? C40 C35 C36 122.5(3) . . ? C40 C35 N3 120.7(2) . . ? C36 C35 N3 116.8(2) . . ? C37 C36 C35 117.2(3) . . ? C37 C36 C41 121.6(3) . . ? C35 C36 C41 121.2(3) . . ? C38 C37 C36 121.2(3) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C39 C38 C37 120.2(3) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 121.6(3) . . ? C38 C39 H39 119.2 . . ? C40 C39 H39 119.2 . . ? C39 C40 C35 117.3(3) . . ? C39 C40 C44 121.4(3) . . ? C35 C40 C44 121.3(3) . . ? C36 C41 C42 110.4(2) . . ? C36 C41 C43 114.2(3) . . ? C42 C41 C43 109.0(3) . . ? C36 C41 H41 107.7 . . ? C42 C41 H41 107.7 . . ? C43 C41 H41 107.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 C46 111.7(3) . . ? C40 C44 C45 112.2(3) . . ? C46 C44 C45 109.4(3) . . ? C40 C44 H44 107.8 . . ? C46 C44 H44 107.8 . . ? C45 C44 H44 107.8 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C52 C47 C48 117.6(4) . . ? C52 C47 C53 122.1(5) . . ? C48 C47 C53 120.3(5) . . ? C49 C48 C47 121.2(4) . . ? C49 C48 H48 119.4 . . ? C47 C48 H48 119.4 . . ? C50 C49 C48 119.8(4) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C49 C50 C51 120.1(4) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C52 C51 C50 119.9(4) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C51 C52 C47 121.5(4) . . ? C51 C52 H52 119.3 . . ? C47 C52 H52 119.3 . . ? C47 C53 H53A 109.5 . . ? C47 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C47 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 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 N1 C21 -54.05(19) . . . . ? C1 Lu1 N1 C21 57.8(2) . . . . ? C5 Lu1 N1 C21 171.1(2) . . . . ? N3 Lu1 N1 C21 -69.9(2) . . . . ? N2 Lu1 N1 C9 130.7(2) . . . . ? C1 Lu1 N1 C9 -117.4(2) . . . . ? C5 Lu1 N1 C9 -4.2(2) . . . . ? N3 Lu1 N1 C9 114.8(2) . . . . ? C1 Lu1 N2 C28 144.0(2) . . . . ? C5 Lu1 N2 C28 -40.8(3) . . . . ? N1 Lu1 N2 C28 -125.2(2) . . . . ? N3 Lu1 N2 C28 46.5(2) . . . . ? C1 Lu1 N2 C27 -26.2(2) . . . . ? C5 Lu1 N2 C27 149.01(18) . . . . ? N1 Lu1 N2 C27 64.69(18) . . . . ? N3 Lu1 N2 C27 -123.63(19) . . . . ? N2 Lu1 N3 C34 -34.8(2) . . . . ? C1 Lu1 N3 C34 -145.4(2) . . . . ? C5 Lu1 N3 C34 99.5(2) . . . . ? N1 Lu1 N3 C34 -19.0(3) . . . . ? N2 Lu1 N3 C35 142.3(2) . . . . ? C1 Lu1 N3 C35 31.8(2) . . . . ? C5 Lu1 N3 C35 -83.4(2) . . . . ? N1 Lu1 N3 C35 158.18(18) . . . . ? C2 Si1 C1 Lu1 -103.8(2) . . . . ? C3 Si1 C1 Lu1 15.7(2) . . . . ? C4 Si1 C1 Lu1 134.28(18) . . . . ? N2 Lu1 C1 Si1 -155.32(15) . . . . ? C5 Lu1 C1 Si1 28.3(2) . . . . ? N1 Lu1 C1 Si1 127.83(17) . . . . ? N3 Lu1 C1 Si1 -76.65(18) . . . . ? C7 Si2 C5 Lu1 -99.67(19) . . . . ? C6 Si2 C5 Lu1 20.6(2) . . . . ? C8 Si2 C5 Lu1 139.15(19) . . . . ? N2 Lu1 C5 Si2 0.2(2) . . . . ? C1 Lu1 C5 Si2 175.47(15) . . . . ? N1 Lu1 C5 Si2 75.95(17) . . . . ? N3 Lu1 C5 Si2 -77.15(17) . . . . ? C21 N1 C9 C14 -98.9(3) . . . . ? Lu1 N1 C9 C14 76.4(3) . . . . ? C21 N1 C9 C10 81.8(3) . . . . ? Lu1 N1 C9 C10 -102.9(3) . . . . ? C14 C9 C10 C11 4.8(4) . . . . ? N1 C9 C10 C11 -175.9(3) . . . . ? C14 C9 C10 C15 -174.1(3) . . . . ? N1 C9 C10 C15 5.2(4) . . . . ? C9 C10 C11 C12 -2.2(5) . . . . ? C15 C10 C11 C12 176.7(3) . . . . ? C10 C11 C12 C13 -1.1(5) . . . . ? C11 C12 C13 C14 1.9(5) . . . . ? C10 C9 C14 C13 -4.0(4) . . . . ? N1 C9 C14 C13 176.7(2) . . . . ? C10 C9 C14 C18 177.0(3) . . . . ? N1 C9 C14 C18 -2.2(4) . . . . ? C12 C13 C14 C9 0.6(4) . . . . ? C12 C13 C14 C18 179.5(3) . . . . ? C11 C10 C15 C16 85.1(4) . . . . ? C9 C10 C15 C16 -96.0(3) . . . . ? C11 C10 C15 C17 -39.3(4) . . . . ? C9 C10 C15 C17 139.6(3) . . . . ? C9 C14 C18 C19 92.3(3) . . . . ? C13 C14 C18 C19 -86.6(3) . . . . ? C9 C14 C18 C20 -144.0(3) . . . . ? C13 C14 C18 C20 37.1(4) . . . . ? C9 N1 C21 C22 -164.6(3) . . . . ? Lu1 N1 C21 C22 19.3(3) . . . . ? N1 C21 C22 C23 -158.8(3) . . . . ? N1 C21 C22 C27 31.4(4) . . . . ? C27 C22 C23 C24 -0.3(4) . . . . ? C21 C22 C23 C24 -170.4(3) . . . . ? C22 C23 C24 C25 3.3(5) . . . . ? C23 C24 C25 C26 -3.1(5) . . . . ? C24 C25 C26 C27 -0.2(5) . . . . ? C28 N2 C27 C26 -39.7(4) . . . . ? Lu1 N2 C27 C26 131.5(2) . . . . ? C28 N2 C27 C22 145.6(3) . . . . ? Lu1 N2 C27 C22 -43.2(3) . . . . ? C25 C26 C27 N2 -171.6(3) . . . . ? C25 C26 C27 C22 3.2(4) . . . . ? C23 C22 C27 N2 171.9(3) . . . . ? C21 C22 C27 N2 -18.4(4) . . . . ? C23 C22 C27 C26 -3.0(4) . . . . ? C21 C22 C27 C26 166.7(3) . . . . ? C27 N2 C28 C29 -46.9(4) . . . . ? Lu1 N2 C28 C29 143.4(2) . . . . ? C27 N2 C28 C33 136.6(3) . . . . ? Lu1 N2 C28 C33 -33.1(3) . . . . ? N2 C28 C29 C30 -173.9(3) . . . . ? C33 C28 C29 C30 2.7(4) . . . . ? C28 C29 C30 C31 -2.1(4) . . . . ? C29 C30 C31 C32 -0.5(4) . . . . ? C30 C31 C32 C33 2.2(4) . . . . ? C31 C32 C33 C28 -1.4(4) . . . . ? C31 C32 C33 C34 -171.6(3) . . . . ? N2 C28 C33 C32 175.7(2) . . . . ? C29 C28 C33 C32 -1.0(4) . . . . ? N2 C28 C33 C34 -14.7(4) . . . . ? C29 C28 C33 C34 168.6(3) . . . . ? C35 N3 C34 C33 -166.7(3) . . . . ? Lu1 N3 C34 C33 10.6(4) . . . . ? C32 C33 C34 N3 -165.1(3) . . . . ? C28 C33 C34 N3 25.1(4) . . . . ? C34 N3 C35 C40 -88.6(3) . . . . ? Lu1 N3 C35 C40 94.0(3) . . . . ? C34 N3 C35 C36 90.3(3) . . . . ? Lu1 N3 C35 C36 -87.1(3) . . . . ? C40 C35 C36 C37 -0.9(4) . . . . ? N3 C35 C36 C37 -179.8(2) . . . . ? C40 C35 C36 C41 176.6(3) . . . . ? N3 C35 C36 C41 -2.3(4) . . . . ? C35 C36 C37 C38 2.0(4) . . . . ? C41 C36 C37 C38 -175.6(3) . . . . ? C36 C37 C38 C39 -1.5(5) . . . . ? C37 C38 C39 C40 0.0(4) . . . . ? C38 C39 C40 C35 1.1(4) . . . . ? C38 C39 C40 C44 -179.5(3) . . . . ? C36 C35 C40 C39 -0.6(4) . . . . ? N3 C35 C40 C39 178.3(2) . . . . ? C36 C35 C40 C44 -180.0(3) . . . . ? N3 C35 C40 C44 -1.1(4) . . . . ? C37 C36 C41 C42 87.1(3) . . . . ? C35 C36 C41 C42 -90.4(3) . . . . ? C37 C36 C41 C43 -36.1(4) . . . . ? C35 C36 C41 C43 146.5(3) . . . . ? C39 C40 C44 C46 -84.9(3) . . . . ? C35 C40 C44 C46 94.5(3) . . . . ? C39 C40 C44 C45 38.4(4) . . . . ? C35 C40 C44 C45 -142.2(3) . . . . ? C52 C47 C48 C49 0.2(7) . . . . ? C53 C47 C48 C49 179.4(5) . . . . ? C47 C48 C49 C50 -0.2(6) . . . . ? C48 C49 C50 C51 -0.1(6) . . . . ? C49 C50 C51 C52 0.2(6) . . . . ? C50 C51 C52 C47 -0.2(6) . . . . ? C48 C47 C52 C51 0.0(6) . . . . ? C53 C47 C52 C51 -179.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.039 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.144 data_1 _database_code_depnum_ccdc_archive 'CCDC 857397' #TrackingRef 'Sc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H74 N3 Sc Si2' _chemical_formula_weight 854.29 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.661(2) _cell_length_b 18.871(3) _cell_length_c 20.672(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.225(5) _cell_angle_gamma 90.00 _cell_volume 5286.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9893 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 26.71 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9079 _exptl_absorpt_correction_T_max 0.9273 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58700 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.02 _reflns_number_total 9346 _reflns_number_gt 7138 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+3.0615P] 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 9346 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Sc1 Sc 0.24146(3) 0.65182(2) 0.293822(18) 0.03087(11) Uani 1 1 d . . . N1 N 0.40464(11) 0.65071(9) 0.27008(8) 0.0342(4) Uani 1 1 d . . . N2 N 0.22388(12) 0.66823(10) 0.19053(8) 0.0373(4) Uani 1 1 d . . . N3 N 0.07366(12) 0.67616(10) 0.27114(8) 0.0387(4) Uani 1 1 d . . . Si1 Si 0.27030(5) 0.48867(4) 0.39525(3) 0.04760(18) Uani 1 1 d . . . Si2 Si 0.28092(5) 0.81763(4) 0.38895(4) 0.05178(19) Uani 1 1 d . . . C1 C 0.22488(16) 0.53859(12) 0.32052(11) 0.0429(5) Uani 1 1 d . A . H1A H 0.1527 0.5305 0.3147 0.051 Uiso 1 1 calc R . . H1B H 0.2504 0.5119 0.2850 0.051 Uiso 1 1 calc R . . C2 C 0.3186(3) 0.39910(18) 0.37535(19) 0.1055(13) Uani 1 1 d . A . H2A H 0.3214 0.3684 0.4138 0.158 Uiso 1 1 calc R . . H2B H 0.3850 0.4042 0.3626 0.158 Uiso 1 1 calc R . . H2C H 0.2747 0.3780 0.3393 0.158 Uiso 1 1 calc R . . C3 C 0.3722(2) 0.53323(18) 0.44780(15) 0.0786(9) Uani 1 1 d . A . H3A H 0.3519 0.5814 0.4579 0.118 Uiso 1 1 calc R . . H3B H 0.4307 0.5355 0.4249 0.118 Uiso 1 1 calc R . . H3C H 0.3878 0.5064 0.4884 0.118 Uiso 1 1 calc R . . C4 C 0.1687(8) 0.4659(14) 0.4428(8) 0.075(3) Uani 0.69(6) 1 d P A 1 H4A H 0.1459 0.5088 0.4630 0.113 Uiso 0.69(6) 1 calc PR A 1 H4B H 0.1923 0.4316 0.4769 0.113 Uiso 0.69(6) 1 calc PR A 1 H4C H 0.1139 0.4451 0.4138 0.113 Uiso 0.69(6) 1 calc PR A 1 C4' C 0.175(2) 0.496(3) 0.458(2) 0.075(6) Uani 0.31(6) 1 d P A 2 H4'D H 0.1723 0.5452 0.4732 0.113 Uiso 0.31(6) 1 calc PR A 2 H4'E H 0.1961 0.4652 0.4957 0.113 Uiso 0.31(6) 1 calc PR A 2 H4'F H 0.1100 0.4813 0.4377 0.113 Uiso 0.31(6) 1 calc PR A 2 C5 C 0.26555(16) 0.72080(12) 0.38159(11) 0.0437(5) Uani 1 1 d . . . H5A H 0.2098 0.7098 0.4062 0.052 Uiso 1 1 calc R . . H5B H 0.3249 0.7010 0.4078 0.052 Uiso 1 1 calc R . . C6 C 0.3189(3) 0.85474(17) 0.31196(18) 0.0881(10) Uani 1 1 d . . . H6A H 0.3825 0.8343 0.3044 0.132 Uiso 1 1 calc R . . H6B H 0.3253 0.9063 0.3158 0.132 Uiso 1 1 calc R . . H6C H 0.2689 0.8430 0.2753 0.132 Uiso 1 1 calc R . . C7 C 0.3787(3) 0.84699(18) 0.45558(18) 0.0911(11) Uani 1 1 d . . . H7A H 0.3661 0.8257 0.4970 0.137 Uiso 1 1 calc R . . H7B H 0.3774 0.8987 0.4593 0.137 Uiso 1 1 calc R . . H7C H 0.4435 0.8318 0.4453 0.137 Uiso 1 1 calc R . . C8 C 0.1641(2) 0.86155(16) 0.40613(16) 0.0739(9) Uani 1 1 d . . . H8A H 0.1107 0.8495 0.3717 0.111 Uiso 1 1 calc R . . H8B H 0.1734 0.9130 0.4075 0.111 Uiso 1 1 calc R . . H8C H 0.1470 0.8451 0.4483 0.111 Uiso 1 1 calc R . . C9 C 0.48057(14) 0.60128(12) 0.29853(11) 0.0384(5) Uani 1 1 d . . . C10 C 0.48573(17) 0.53539(13) 0.26775(12) 0.0490(6) Uani 1 1 d . . . C11 C 0.5589(2) 0.48854(14) 0.29397(15) 0.0625(7) Uani 1 1 d . . . H11 H 0.5633 0.4431 0.2749 0.075 Uiso 1 1 calc R . . C12 C 0.6253(2) 0.50706(16) 0.34732(15) 0.0660(8) Uani 1 1 d . . . H12 H 0.6752 0.4745 0.3642 0.079 Uiso 1 1 calc R . . C13 C 0.61946(17) 0.57196(15) 0.37599(13) 0.0571(7) Uani 1 1 d . . . H13 H 0.6661 0.5839 0.4124 0.069 Uiso 1 1 calc R . . C14 C 0.54661(15) 0.62128(13) 0.35310(11) 0.0434(5) Uani 1 1 d . . . C15 C 0.41874(19) 0.51715(14) 0.20484(13) 0.0576(7) Uani 1 1 d . . . H15 H 0.3582 0.5471 0.2037 0.069 Uiso 1 1 calc R . . C16 C 0.3852(3) 0.43984(17) 0.20001(19) 0.0897(11) Uani 1 1 d . . . H16A H 0.4422 0.4092 0.1963 0.135 Uiso 1 1 calc R . . H16B H 0.3364 0.4337 0.1614 0.135 Uiso 1 1 calc R . . H16C H 0.3556 0.4270 0.2392 0.135 Uiso 1 1 calc R . . C17 C 0.4690(2) 0.53655(19) 0.14478(15) 0.0796(9) Uani 1 1 d . . . H17A H 0.4863 0.5870 0.1464 0.119 Uiso 1 1 calc R . . H17B H 0.4237 0.5269 0.1051 0.119 Uiso 1 1 calc R . . H17C H 0.5289 0.5081 0.1445 0.119 Uiso 1 1 calc R . . C18 C 0.54307(17) 0.69327(13) 0.38504(12) 0.0499(6) Uani 1 1 d . . . H18 H 0.4752 0.7128 0.3728 0.060 Uiso 1 1 calc R . . C19 C 0.5613(2) 0.68969(18) 0.45935(14) 0.0773(9) Uani 1 1 d . . . H19A H 0.5157 0.6555 0.4751 0.116 Uiso 1 1 calc R . . H19B H 0.5505 0.7366 0.4776 0.116 Uiso 1 1 calc R . . H19C H 0.6294 0.6747 0.4731 0.116 Uiso 1 1 calc R . . C20 C 0.6159(2) 0.74502(16) 0.36020(16) 0.0784(9) Uani 1 1 d . . . H20A H 0.6831 0.7267 0.3705 0.118 Uiso 1 1 calc R . . H20B H 0.6109 0.7912 0.3813 0.118 Uiso 1 1 calc R . . H20C H 0.6003 0.7504 0.3129 0.118 Uiso 1 1 calc R . . C21 C 0.43434(15) 0.69176(12) 0.22676(11) 0.0394(5) Uani 1 1 d . . . H21 H 0.5036 0.6943 0.2260 0.047 Uiso 1 1 calc R . . C22 C 0.37426(15) 0.73440(11) 0.17916(10) 0.0378(5) Uani 1 1 d . . . C23 C 0.42238(18) 0.78719(13) 0.14634(12) 0.0507(6) Uani 1 1 d . . . H23 H 0.4896 0.7977 0.1607 0.061 Uiso 1 1 calc R . . C24 C 0.3749(2) 0.82344(14) 0.09472(13) 0.0581(7) Uani 1 1 d . . . H24 H 0.4075 0.8602 0.0745 0.070 Uiso 1 1 calc R . . C25 C 0.2778(2) 0.80564(15) 0.07211(12) 0.0594(7) Uani 1 1 d . . . H25 H 0.2445 0.8299 0.0355 0.071 Uiso 1 1 calc R . . C26 C 0.22922(18) 0.75360(14) 0.10182(11) 0.0513(6) Uani 1 1 d . . . H26 H 0.1634 0.7418 0.0847 0.062 Uiso 1 1 calc R . . C27 C 0.27477(15) 0.71739(12) 0.15711(10) 0.0375(5) Uani 1 1 d . . . C28 C 0.16249(15) 0.61928(12) 0.15522(10) 0.0395(5) Uani 1 1 d . . . C29 C 0.18887(18) 0.58651(14) 0.09862(11) 0.0525(6) Uani 1 1 d . . . H29 H 0.2461 0.6021 0.0810 0.063 Uiso 1 1 calc R . . C30 C 0.1335(2) 0.53245(16) 0.06848(13) 0.0646(7) Uani 1 1 d . . . H30 H 0.1540 0.5106 0.0310 0.077 Uiso 1 1 calc R . . C31 C 0.0480(2) 0.50913(16) 0.09161(14) 0.0666(8) Uani 1 1 d . . . H31 H 0.0113 0.4708 0.0710 0.080 Uiso 1 1 calc R . . C32 C 0.01763(19) 0.54202(15) 0.14425(13) 0.0575(7) Uani 1 1 d . . . H32 H -0.0423 0.5274 0.1590 0.069 Uiso 1 1 calc R . . C33 C 0.07293(15) 0.59730(12) 0.17746(11) 0.0416(5) Uani 1 1 d . . . C34 C 0.02816(15) 0.63756(13) 0.22565(11) 0.0437(5) Uani 1 1 d . . . H34 H -0.0417 0.6352 0.2234 0.052 Uiso 1 1 calc R . . C35 C 0.01017(15) 0.72550(13) 0.30033(12) 0.0456(6) Uani 1 1 d . . . C36 C -0.01310(18) 0.78980(15) 0.26758(14) 0.0597(7) Uani 1 1 d . . . C37 C -0.0793(2) 0.83504(17) 0.29278(18) 0.0781(9) Uani 1 1 d . . . H37 H -0.0971 0.8785 0.2712 0.094 Uiso 1 1 calc R . . C38 C -0.1193(2) 0.81792(19) 0.34823(18) 0.0825(10) Uani 1 1 d . . . H38 H -0.1656 0.8489 0.3641 0.099 Uiso 1 1 calc R . . C39 C -0.0928(2) 0.75610(18) 0.38110(15) 0.0706(8) Uani 1 1 d . . . H39 H -0.1197 0.7458 0.4202 0.085 Uiso 1 1 calc R . . C40 C -0.02688(16) 0.70794(14) 0.35821(12) 0.0509(6) Uani 1 1 d . . . C41 C 0.0315(2) 0.81027(17) 0.20682(16) 0.0769(9) Uani 1 1 d . . . H41 H 0.0938 0.7824 0.2068 0.092 Uiso 1 1 calc R . . C42 C -0.0362(3) 0.7906(2) 0.14463(18) 0.1100(14) Uani 1 1 d . . . H42A H -0.0471 0.7393 0.1435 0.165 Uiso 1 1 calc R . . H42B H -0.0052 0.8049 0.1064 0.165 Uiso 1 1 calc R . . H42C H -0.0996 0.8150 0.1442 0.165 Uiso 1 1 calc R . . C43 C 0.0595(3) 0.8893(2) 0.2057(2) 0.1168(15) Uani 1 1 d . . . H43A H -0.0005 0.9182 0.2027 0.175 Uiso 1 1 calc R . . H43B H 0.0942 0.8987 0.1679 0.175 Uiso 1 1 calc R . . H43C H 0.1025 0.9012 0.2458 0.175 Uiso 1 1 calc R . . C44 C -0.00033(18) 0.63973(15) 0.39416(12) 0.0555(7) Uani 1 1 d . . . H44 H 0.0637 0.6230 0.3809 0.067 Uiso 1 1 calc R . . C45 C -0.0773(2) 0.58178(18) 0.37515(16) 0.0815(9) Uani 1 1 d . . . H45A H -0.1419 0.5976 0.3855 0.122 Uiso 1 1 calc R . . H45B H -0.0580 0.5384 0.3995 0.122 Uiso 1 1 calc R . . H45C H -0.0812 0.5723 0.3283 0.122 Uiso 1 1 calc R . . C46 C 0.0148(3) 0.6491(2) 0.46831(14) 0.0849(10) Uani 1 1 d . . . H46A H 0.0590 0.6893 0.4798 0.127 Uiso 1 1 calc R . . H46B H 0.0440 0.6060 0.4888 0.127 Uiso 1 1 calc R . . H46C H -0.0490 0.6581 0.4838 0.127 Uiso 1 1 calc R . . C47 C 0.708(6) 0.620(3) 0.0918(7) 0.099(10) Uani 0.66(19) 1 d P B 1 C47' C 0.750(11) 0.641(5) 0.0912(14) 0.099(19) Uani 0.34(19) 1 d P B 2 C48 C 0.7112(4) 0.6913(3) 0.1208(3) 0.1241(16) Uani 1 1 d . . . H48 H 0.7073 0.7322 0.0938 0.149 Uiso 1 1 calc R B 1 C49 C 0.7200(3) 0.6979(2) 0.1867(3) 0.1061(12) Uani 1 1 d . B . H49 H 0.7148 0.7432 0.2060 0.127 Uiso 1 1 calc R . . C50 C 0.7360(3) 0.6410(3) 0.2239(2) 0.1003(12) Uani 1 1 d . . . H50 H 0.7413 0.6456 0.2700 0.120 Uiso 1 1 calc R B . C51 C 0.7447(3) 0.5771(3) 0.1971(3) 0.1028(13) Uani 1 1 d . B . H51 H 0.7571 0.5368 0.2245 0.123 Uiso 1 1 calc R . . C52 C 0.7363(3) 0.5690(2) 0.1321(3) 0.1095(13) Uani 1 1 d . . . H52 H 0.7516 0.5242 0.1148 0.131 Uiso 1 1 calc R B 1 C53 C 0.684(3) 0.6057(14) 0.0188(6) 0.160(9) Uani 0.60(4) 1 d P B 1 H53A H 0.7351 0.6261 -0.0044 0.240 Uiso 0.60(4) 1 calc PR B 1 H53B H 0.6198 0.6273 0.0027 0.240 Uiso 0.60(4) 1 calc PR B 1 H53C H 0.6801 0.5545 0.0113 0.240 Uiso 0.60(4) 1 calc PR B 1 C53' C 0.759(4) 0.641(2) 0.0195(8) 0.160(12) Uani 0.40(4) 1 d P B 2 H53D H 0.7024 0.6659 -0.0039 0.240 Uiso 0.40(4) 1 calc PR B 2 H53E H 0.7591 0.5916 0.0036 0.240 Uiso 0.40(4) 1 calc PR B 2 H53F H 0.8201 0.6641 0.0118 0.240 Uiso 0.40(4) 1 calc PR B 2 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 0.02922(19) 0.0329(2) 0.0305(2) 0.00320(16) 0.00369(15) -0.00119(16) N1 0.0294(8) 0.0367(10) 0.0362(9) 0.0028(8) 0.0028(7) 0.0002(7) N2 0.0305(9) 0.0487(11) 0.0326(9) 0.0048(8) 0.0035(7) -0.0044(8) N3 0.0326(9) 0.0472(11) 0.0371(10) 0.0045(8) 0.0074(8) 0.0013(8) Si1 0.0504(4) 0.0405(4) 0.0505(4) 0.0131(3) 0.0007(3) -0.0064(3) Si2 0.0523(4) 0.0431(4) 0.0619(5) -0.0112(3) 0.0148(3) -0.0061(3) C1 0.0459(12) 0.0378(12) 0.0446(13) 0.0039(10) 0.0043(10) -0.0016(10) C2 0.145(4) 0.067(2) 0.098(3) 0.016(2) -0.007(2) 0.025(2) C3 0.081(2) 0.083(2) 0.0658(19) 0.0199(17) -0.0145(16) -0.0216(17) C4 0.072(4) 0.087(9) 0.069(5) 0.015(5) 0.014(3) -0.017(5) C4' 0.072(8) 0.087(16) 0.069(12) 0.015(12) 0.014(8) -0.017(10) C5 0.0434(12) 0.0437(13) 0.0445(13) -0.0044(10) 0.0078(10) -0.0057(10) C6 0.112(3) 0.060(2) 0.101(3) 0.0051(18) 0.047(2) -0.0066(18) C7 0.082(2) 0.075(2) 0.111(3) -0.031(2) -0.008(2) -0.0133(18) C8 0.0709(19) 0.0629(19) 0.090(2) -0.0205(16) 0.0171(16) 0.0039(15) C9 0.0297(10) 0.0417(12) 0.0447(13) 0.0096(10) 0.0088(9) 0.0024(9) C10 0.0425(12) 0.0457(14) 0.0607(16) 0.0012(12) 0.0131(11) 0.0038(10) C11 0.0596(16) 0.0459(15) 0.084(2) 0.0068(14) 0.0176(15) 0.0140(12) C12 0.0511(15) 0.0625(19) 0.084(2) 0.0243(16) 0.0072(14) 0.0196(13) C13 0.0417(13) 0.0673(18) 0.0604(16) 0.0182(14) -0.0009(11) 0.0053(12) C14 0.0337(11) 0.0480(14) 0.0486(13) 0.0123(11) 0.0055(10) -0.0013(10) C15 0.0517(14) 0.0522(16) 0.0695(18) -0.0159(13) 0.0095(13) 0.0061(12) C16 0.092(2) 0.063(2) 0.114(3) -0.031(2) 0.013(2) -0.0056(17) C17 0.080(2) 0.095(2) 0.0649(19) -0.0132(18) 0.0152(16) 0.0080(18) C18 0.0384(12) 0.0553(15) 0.0535(15) 0.0024(12) -0.0038(10) -0.0024(11) C19 0.088(2) 0.086(2) 0.0545(17) -0.0039(16) -0.0059(15) -0.0142(18) C20 0.086(2) 0.0631(19) 0.086(2) 0.0055(17) 0.0102(17) -0.0246(16) C21 0.0311(11) 0.0415(13) 0.0460(13) 0.0013(10) 0.0064(9) -0.0032(9) C22 0.0371(11) 0.0395(12) 0.0378(12) 0.0035(10) 0.0088(9) -0.0024(9) C23 0.0479(13) 0.0508(15) 0.0542(15) 0.0076(12) 0.0097(11) -0.0094(11) C24 0.0687(17) 0.0516(15) 0.0561(16) 0.0164(13) 0.0165(13) -0.0087(13) C25 0.0686(17) 0.0651(18) 0.0440(14) 0.0205(13) 0.0053(12) 0.0038(14) C26 0.0466(13) 0.0643(17) 0.0423(13) 0.0123(12) 0.0024(10) -0.0005(12) C27 0.0381(11) 0.0425(13) 0.0328(11) 0.0021(9) 0.0081(9) -0.0001(9) C28 0.0356(11) 0.0489(13) 0.0330(11) 0.0046(10) 0.0002(9) -0.0007(10) C29 0.0501(14) 0.0657(17) 0.0423(14) -0.0038(12) 0.0088(11) -0.0062(12) C30 0.0737(18) 0.0722(19) 0.0481(15) -0.0177(14) 0.0089(13) -0.0051(15) C31 0.0730(18) 0.0651(18) 0.0596(17) -0.0152(14) -0.0004(14) -0.0204(15) C32 0.0509(14) 0.0673(18) 0.0535(16) -0.0024(13) 0.0033(12) -0.0192(13) C33 0.0364(11) 0.0501(14) 0.0374(12) 0.0026(10) 0.0011(9) -0.0056(10) C34 0.0284(10) 0.0590(15) 0.0437(13) 0.0057(11) 0.0047(9) -0.0045(10) C35 0.0299(11) 0.0567(15) 0.0504(14) -0.0035(12) 0.0058(10) 0.0030(10) C36 0.0443(13) 0.0623(17) 0.0729(18) 0.0058(14) 0.0090(12) 0.0132(12) C37 0.0595(17) 0.073(2) 0.103(3) 0.0035(18) 0.0122(17) 0.0235(15) C38 0.0581(18) 0.084(2) 0.108(3) -0.020(2) 0.0231(18) 0.0173(16) C39 0.0512(15) 0.093(2) 0.0720(19) -0.0139(18) 0.0258(14) 0.0007(15) C40 0.0342(12) 0.0674(17) 0.0524(15) -0.0092(13) 0.0102(10) -0.0046(11) C41 0.0707(19) 0.076(2) 0.087(2) 0.0318(18) 0.0204(17) 0.0282(16) C42 0.121(3) 0.129(4) 0.080(3) 0.032(2) 0.014(2) 0.037(3) C43 0.117(3) 0.086(3) 0.153(4) 0.052(3) 0.038(3) 0.018(2) C44 0.0467(13) 0.0780(19) 0.0443(14) 0.0000(13) 0.0150(11) -0.0079(12) C45 0.081(2) 0.084(2) 0.079(2) 0.0061(18) 0.0072(17) -0.0231(18) C46 0.088(2) 0.119(3) 0.0492(17) 0.0007(18) 0.0135(15) -0.010(2) C47 0.10(2) 0.098(12) 0.099(6) 0.003(5) 0.012(6) 0.020(14) C47' 0.10(4) 0.10(2) 0.099(11) 0.003(10) 0.012(12) 0.02(3) C48 0.158(4) 0.094(3) 0.123(4) 0.020(3) 0.026(3) 0.030(3) C49 0.110(3) 0.091(3) 0.119(4) -0.005(3) 0.021(3) 0.004(2) C50 0.076(2) 0.125(4) 0.102(3) 0.010(3) 0.019(2) 0.010(2) C51 0.081(2) 0.097(3) 0.131(4) 0.032(3) 0.018(3) -0.001(2) C52 0.099(3) 0.087(3) 0.138(4) -0.006(3) 0.000(3) 0.022(2) C53 0.18(2) 0.176(14) 0.118(8) -0.021(8) 0.005(8) 0.046(15) C53' 0.18(3) 0.18(2) 0.118(12) -0.021(11) 0.005(13) 0.046(19) _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 N2 2.1411(17) . ? Sc1 C5 2.224(2) . ? Sc1 C1 2.226(2) . ? Sc1 N3 2.3270(17) . ? Sc1 N1 2.3421(17) . ? N1 C21 1.288(3) . ? N1 C9 1.462(3) . ? N2 C28 1.391(3) . ? N2 C27 1.394(3) . ? N3 C34 1.286(3) . ? N3 C35 1.454(3) . ? Si1 C1 1.849(2) . ? Si1 C4 1.850(11) . ? Si1 C3 1.856(3) . ? Si1 C2 1.879(4) . ? Si1 C4' 1.96(3) . ? Si2 C5 1.843(2) . ? Si2 C6 1.871(3) . ? Si2 C8 1.872(3) . ? Si2 C7 1.877(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C4' H4'D 0.9800 . ? C4' H4'E 0.9800 . ? C4' H4'F 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? 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 C10 1.403(3) . ? C9 C14 1.405(3) . ? C10 C11 1.392(3) . ? C10 C15 1.532(4) . ? C11 C12 1.382(4) . ? C11 H11 0.9500 . ? C12 C13 1.367(4) . ? C12 H12 0.9500 . ? C13 C14 1.401(3) . ? C13 H13 0.9500 . ? C14 C18 1.514(3) . ? C15 C16 1.529(4) . ? C15 C17 1.536(4) . ? C15 H15 1.0000 . ? 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 C19 1.526(4) . ? C18 C20 1.528(4) . ? C18 H18 1.0000 . ? 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 C22 1.444(3) . ? C21 H21 0.9500 . ? C22 C23 1.413(3) . ? C22 C27 1.415(3) . ? C23 C24 1.361(3) . ? C23 H23 0.9500 . ? C24 C25 1.391(4) . ? C24 H24 0.9500 . ? C25 C26 1.373(3) . ? C25 H25 0.9500 . ? C26 C27 1.408(3) . ? C26 H26 0.9500 . ? C28 C29 1.410(3) . ? C28 C33 1.422(3) . ? C29 C30 1.372(4) . ? C29 H29 0.9500 . ? C30 C31 1.388(4) . ? C30 H30 0.9500 . ? C31 C32 1.362(4) . ? C31 H31 0.9500 . ? C32 C33 1.414(3) . ? C32 H32 0.9500 . ? C33 C34 1.448(3) . ? C34 H34 0.9500 . ? C35 C40 1.396(3) . ? C35 C36 1.406(4) . ? C36 C37 1.392(4) . ? C36 C41 1.514(4) . ? C37 C38 1.369(5) . ? C37 H37 0.9500 . ? C38 C39 1.375(5) . ? C38 H38 0.9500 . ? C39 C40 1.403(4) . ? C39 H39 0.9500 . ? C40 C44 1.508(4) . ? C41 C42 1.532(5) . ? C41 C43 1.540(5) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C46 1.531(4) . ? C44 C45 1.534(4) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C52 1.30(3) . ? C47 C48 1.47(5) . ? C47 C53 1.53(2) . ? C47' C48 1.29(3) . ? C47' C53' 1.50(5) . ? C47' C52 1.62(11) . ? C48 C49 1.359(6) . ? C48 H48 0.9500 . ? C49 C50 1.323(5) . ? C49 H49 0.9500 . ? C50 C51 1.339(6) . ? C50 H50 0.9500 . ? C51 C52 1.343(6) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C53' H53D 0.9800 . ? C53' H53E 0.9800 . ? C53' H53F 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 Sc1 C5 135.69(8) . . ? N2 Sc1 C1 112.58(8) . . ? C5 Sc1 C1 111.65(9) . . ? N2 Sc1 N3 77.67(6) . . ? C5 Sc1 N3 95.15(8) . . ? C1 Sc1 N3 96.38(7) . . ? N2 Sc1 N1 77.45(6) . . ? C5 Sc1 N1 97.42(7) . . ? C1 Sc1 N1 99.94(7) . . ? N3 Sc1 N1 154.02(6) . . ? C21 N1 C9 113.19(17) . . ? C21 N1 Sc1 122.13(14) . . ? C9 N1 Sc1 124.54(12) . . ? C28 N2 C27 119.17(17) . . ? C28 N2 Sc1 114.32(13) . . ? C27 N2 Sc1 126.17(13) . . ? C34 N3 C35 114.04(18) . . ? C34 N3 Sc1 114.13(14) . . ? C35 N3 Sc1 131.80(14) . . ? C1 Si1 C4 111.5(4) . . ? C1 Si1 C3 113.98(12) . . ? C4 Si1 C3 110.6(7) . . ? C1 Si1 C2 111.46(14) . . ? C4 Si1 C2 102.4(9) . . ? C3 Si1 C2 106.10(18) . . ? C1 Si1 C4' 109.9(8) . . ? C4 Si1 C4' 19.5(9) . . ? C3 Si1 C4' 95.1(15) . . ? C2 Si1 C4' 119.4(14) . . ? C5 Si2 C6 109.98(13) . . ? C5 Si2 C8 111.32(13) . . ? C6 Si2 C8 109.28(16) . . ? C5 Si2 C7 114.59(14) . . ? C6 Si2 C7 105.42(18) . . ? C8 Si2 C7 105.95(15) . . ? Si1 C1 Sc1 131.49(12) . . ? Si1 C1 H1A 104.4 . . ? Sc1 C1 H1A 104.4 . . ? Si1 C1 H1B 104.4 . . ? Sc1 C1 H1B 104.4 . . ? H1A C1 H1B 105.6 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? Si1 C4' H4'D 109.5 . . ? Si1 C4' H4'E 109.5 . . ? H4'D C4' H4'E 109.5 . . ? Si1 C4' H4'F 109.5 . . ? H4'D C4' H4'F 109.5 . . ? H4'E C4' H4'F 109.5 . . ? Si2 C5 Sc1 130.64(12) . . ? Si2 C5 H5A 104.6 . . ? Sc1 C5 H5A 104.6 . . ? Si2 C5 H5B 104.6 . . ? Sc1 C5 H5B 104.6 . . ? H5A C5 H5B 105.7 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C14 122.6(2) . . ? C10 C9 N1 117.17(19) . . ? C14 C9 N1 120.2(2) . . ? C11 C10 C9 117.4(2) . . ? C11 C10 C15 120.7(2) . . ? C9 C10 C15 121.7(2) . . ? C12 C11 C10 121.1(3) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C13 C12 C11 120.3(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 121.8(2) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C9 116.7(2) . . ? C13 C14 C18 120.6(2) . . ? C9 C14 C18 122.6(2) . . ? C16 C15 C10 114.3(3) . . ? C16 C15 C17 109.6(2) . . ? C10 C15 C17 110.6(2) . . ? C16 C15 H15 107.3 . . ? C10 C15 H15 107.3 . . ? C17 C15 H15 107.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C19 112.9(2) . . ? C14 C18 C20 111.7(2) . . ? C19 C18 C20 109.6(2) . . ? C14 C18 H18 107.5 . . ? C19 C18 H18 107.5 . . ? C20 C18 H18 107.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 C22 127.38(19) . . ? N1 C21 H21 116.3 . . ? C22 C21 H21 116.3 . . ? C23 C22 C27 119.4(2) . . ? C23 C22 C21 117.45(19) . . ? C27 C22 C21 122.25(19) . . ? C24 C23 C22 121.7(2) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 118.9(2) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C26 C25 C24 121.1(2) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C27 121.4(2) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? N2 C27 C26 121.91(19) . . ? N2 C27 C22 120.67(18) . . ? C26 C27 C22 117.4(2) . . ? N2 C28 C29 121.8(2) . . ? N2 C28 C33 120.70(19) . . ? C29 C28 C33 117.4(2) . . ? C30 C29 C28 121.3(2) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 121.3(3) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C32 C31 C30 119.0(2) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C33 121.7(2) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C32 C33 C28 119.2(2) . . ? C32 C33 C34 118.4(2) . . ? C28 C33 C34 121.6(2) . . ? N3 C34 C33 126.37(19) . . ? N3 C34 H34 116.8 . . ? C33 C34 H34 116.8 . . ? C40 C35 C36 122.2(2) . . ? C40 C35 N3 120.2(2) . . ? C36 C35 N3 117.6(2) . . ? C37 C36 C35 117.9(3) . . ? C37 C36 C41 120.2(3) . . ? C35 C36 C41 122.0(2) . . ? C38 C37 C36 121.0(3) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 120.4(3) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C40 121.6(3) . . ? C38 C39 H39 119.2 . . ? C40 C39 H39 119.2 . . ? C35 C40 C39 116.9(3) . . ? C35 C40 C44 122.3(2) . . ? C39 C40 C44 120.8(2) . . ? C36 C41 C42 111.8(3) . . ? C36 C41 C43 112.7(3) . . ? C42 C41 C43 110.3(3) . . ? C36 C41 H41 107.3 . . ? C42 C41 H41 107.3 . . ? C43 C41 H41 107.3 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 C46 112.9(2) . . ? C40 C44 C45 111.6(2) . . ? C46 C44 C45 109.9(2) . . ? C40 C44 H44 107.4 . . ? C46 C44 H44 107.4 . . ? C45 C44 H44 107.4 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C52 C47 C48 115.3(19) . . ? C52 C47 C53 120(3) . . ? C48 C47 C53 124(3) . . ? C48 C47' C53' 124(3) . . ? C48 C47' C52 107(7) . . ? C53' C47' C52 123(6) . . ? C47' C48 C49 123.7(13) . . ? C47' C48 C47 28(5) . . ? C49 C48 C47 119.2(12) . . ? C47' C48 H48 108.8 . . ? C49 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? C50 C49 C48 119.8(5) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C49 C50 C51 120.5(5) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C50 C51 C52 121.1(4) . . ? C50 C51 H51 119.5 . . ? C52 C51 H51 119.5 . . ? C47 C52 C51 122.3(10) . . ? C47 C52 C47' 24.7(13) . . ? C51 C52 C47' 115(2) . . ? C47 C52 H52 118.8 . . ? C51 C52 H52 118.8 . . ? C47' C52 H52 119.9 . . ? C47' C53' H53D 109.5 . . ? C47' C53' H53E 109.5 . . ? H53D C53' H53E 109.5 . . ? C47' C53' H53F 109.5 . . ? H53D C53' H53F 109.5 . . ? H53E C53' H53F 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 Sc1 N1 C21 37.09(17) . . . . ? C5 Sc1 N1 C21 -98.17(17) . . . . ? C1 Sc1 N1 C21 148.22(17) . . . . ? N3 Sc1 N1 C21 20.1(3) . . . . ? N2 Sc1 N1 C9 -138.43(17) . . . . ? C5 Sc1 N1 C9 86.31(17) . . . . ? C1 Sc1 N1 C9 -27.31(17) . . . . ? N3 Sc1 N1 C9 -155.41(16) . . . . ? C5 Sc1 N2 C28 -147.98(15) . . . . ? C1 Sc1 N2 C28 28.56(17) . . . . ? N3 Sc1 N2 C28 -63.29(15) . . . . ? N1 Sc1 N2 C28 124.24(15) . . . . ? C5 Sc1 N2 C27 38.8(2) . . . . ? C1 Sc1 N2 C27 -144.68(17) . . . . ? N3 Sc1 N2 C27 123.47(18) . . . . ? N1 Sc1 N2 C27 -49.00(17) . . . . ? N2 Sc1 N3 C34 52.46(16) . . . . ? C5 Sc1 N3 C34 -171.84(16) . . . . ? C1 Sc1 N3 C34 -59.33(17) . . . . ? N1 Sc1 N3 C34 69.4(2) . . . . ? N2 Sc1 N3 C35 -129.7(2) . . . . ? C5 Sc1 N3 C35 6.0(2) . . . . ? C1 Sc1 N3 C35 118.5(2) . . . . ? N1 Sc1 N3 C35 -112.8(2) . . . . ? C4 Si1 C1 Sc1 108.3(10) . . . . ? C3 Si1 C1 Sc1 -17.9(2) . . . . ? C2 Si1 C1 Sc1 -137.9(2) . . . . ? C4' Si1 C1 Sc1 87.5(18) . . . . ? N2 Sc1 C1 Si1 156.95(14) . . . . ? C5 Sc1 C1 Si1 -25.64(19) . . . . ? N3 Sc1 C1 Si1 -123.78(16) . . . . ? N1 Sc1 C1 Si1 76.52(16) . . . . ? C6 Si2 C5 Sc1 -20.3(2) . . . . ? C8 Si2 C5 Sc1 101.02(18) . . . . ? C7 Si2 C5 Sc1 -138.78(18) . . . . ? N2 Sc1 C5 Si2 -1.8(2) . . . . ? C1 Sc1 C5 Si2 -178.41(14) . . . . ? N3 Sc1 C5 Si2 -79.44(15) . . . . ? N1 Sc1 C5 Si2 77.76(15) . . . . ? C21 N1 C9 C10 -90.0(2) . . . . ? Sc1 N1 C9 C10 85.9(2) . . . . ? C21 N1 C9 C14 88.0(2) . . . . ? Sc1 N1 C9 C14 -96.1(2) . . . . ? C14 C9 C10 C11 1.1(3) . . . . ? N1 C9 C10 C11 179.0(2) . . . . ? C14 C9 C10 C15 -174.6(2) . . . . ? N1 C9 C10 C15 3.3(3) . . . . ? C9 C10 C11 C12 -1.5(4) . . . . ? C15 C10 C11 C12 174.2(2) . . . . ? C10 C11 C12 C13 0.8(4) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? C12 C13 C14 C9 -1.0(4) . . . . ? C12 C13 C14 C18 -178.9(2) . . . . ? C10 C9 C14 C13 0.1(3) . . . . ? N1 C9 C14 C13 -177.71(19) . . . . ? C10 C9 C14 C18 178.0(2) . . . . ? N1 C9 C14 C18 0.2(3) . . . . ? C11 C10 C15 C16 40.4(3) . . . . ? C9 C10 C15 C16 -144.0(2) . . . . ? C11 C10 C15 C17 -83.9(3) . . . . ? C9 C10 C15 C17 91.7(3) . . . . ? C13 C14 C18 C19 -42.3(3) . . . . ? C9 C14 C18 C19 139.9(2) . . . . ? C13 C14 C18 C20 81.8(3) . . . . ? C9 C14 C18 C20 -96.0(3) . . . . ? C9 N1 C21 C22 164.5(2) . . . . ? Sc1 N1 C21 C22 -11.5(3) . . . . ? N1 C21 C22 C23 166.1(2) . . . . ? N1 C21 C22 C27 -24.7(4) . . . . ? C27 C22 C23 C24 1.5(4) . . . . ? C21 C22 C23 C24 171.0(2) . . . . ? C22 C23 C24 C25 -2.9(4) . . . . ? C23 C24 C25 C26 1.4(4) . . . . ? C24 C25 C26 C27 1.5(4) . . . . ? C28 N2 C27 C26 43.6(3) . . . . ? Sc1 N2 C27 C26 -143.48(19) . . . . ? C28 N2 C27 C22 -138.5(2) . . . . ? Sc1 N2 C27 C22 34.5(3) . . . . ? C25 C26 C27 N2 175.2(2) . . . . ? C25 C26 C27 C22 -2.9(4) . . . . ? C23 C22 C27 N2 -176.6(2) . . . . ? C21 C22 C27 N2 14.4(3) . . . . ? C23 C22 C27 C26 1.4(3) . . . . ? C21 C22 C27 C26 -167.6(2) . . . . ? C27 N2 C28 C29 39.6(3) . . . . ? Sc1 N2 C28 C29 -134.10(19) . . . . ? C27 N2 C28 C33 -144.2(2) . . . . ? Sc1 N2 C28 C33 42.1(2) . . . . ? N2 C28 C29 C30 172.4(2) . . . . ? C33 C28 C29 C30 -3.9(4) . . . . ? C28 C29 C30 C31 1.6(4) . . . . ? C29 C30 C31 C32 1.7(5) . . . . ? C30 C31 C32 C33 -2.6(4) . . . . ? C31 C32 C33 C28 0.2(4) . . . . ? C31 C32 C33 C34 169.7(3) . . . . ? N2 C28 C33 C32 -173.3(2) . . . . ? C29 C28 C33 C32 3.0(3) . . . . ? N2 C28 C33 C34 17.5(3) . . . . ? C29 C28 C33 C34 -166.1(2) . . . . ? C35 N3 C34 C33 163.6(2) . . . . ? Sc1 N3 C34 C33 -18.2(3) . . . . ? C32 C33 C34 N3 161.2(2) . . . . ? C28 C33 C34 N3 -29.6(4) . . . . ? C34 N3 C35 C40 96.8(3) . . . . ? Sc1 N3 C35 C40 -81.0(3) . . . . ? C34 N3 C35 C36 -82.1(3) . . . . ? Sc1 N3 C35 C36 100.1(2) . . . . ? C40 C35 C36 C37 -3.3(4) . . . . ? N3 C35 C36 C37 175.6(2) . . . . ? C40 C35 C36 C41 176.7(3) . . . . ? N3 C35 C36 C41 -4.4(4) . . . . ? C35 C36 C37 C38 1.0(5) . . . . ? C41 C36 C37 C38 -179.0(3) . . . . ? C36 C37 C38 C39 1.6(5) . . . . ? C37 C38 C39 C40 -1.9(5) . . . . ? C36 C35 C40 C39 2.9(4) . . . . ? N3 C35 C40 C39 -175.9(2) . . . . ? C36 C35 C40 C44 -178.7(2) . . . . ? N3 C35 C40 C44 2.5(3) . . . . ? C38 C39 C40 C35 -0.3(4) . . . . ? C38 C39 C40 C44 -178.7(3) . . . . ? C37 C36 C41 C42 -84.6(4) . . . . ? C35 C36 C41 C42 95.4(3) . . . . ? C37 C36 C41 C43 40.3(4) . . . . ? C35 C36 C41 C43 -139.7(3) . . . . ? C35 C40 C44 C46 141.0(2) . . . . ? C39 C40 C44 C46 -40.7(3) . . . . ? C35 C40 C44 C45 -94.7(3) . . . . ? C39 C40 C44 C45 83.7(3) . . . . ? C53' C47' C48 C49 -167(8) . . . . ? C52 C47' C48 C49 40(12) . . . . ? C53' C47' C48 C47 103(14) . . . . ? C52 C47' C48 C47 -50(7) . . . . ? C52 C47 C48 C47' 92(7) . . . . ? C53 C47 C48 C47' -81(7) . . . . ? C52 C47 C48 C49 -15(7) . . . . ? C53 C47 C48 C49 171(5) . . . . ? C47' C48 C49 C50 -26(10) . . . . ? C47 C48 C49 C50 7(4) . . . . ? C48 C49 C50 C51 0.8(7) . . . . ? C49 C50 C51 C52 -0.8(6) . . . . ? C48 C47 C52 C51 16(8) . . . . ? C53 C47 C52 C51 -170(4) . . . . ? C48 C47 C52 C47' -65(6) . . . . ? C53 C47 C52 C47' 109(7) . . . . ? C50 C51 C52 C47 -8(5) . . . . ? C50 C51 C52 C47' 19(5) . . . . ? C48 C47' C52 C47 76(8) . . . . ? C53' C47' C52 C47 -77(10) . . . . ? C48 C47' C52 C51 -36(10) . . . . ? C53' C47' C52 C51 170(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.302 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.040 data_mo_20100827_lxf_by_0m _database_code_depnum_ccdc_archive 'CCDC 857398' #TrackingRef 'Y.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H74 N3 Si2 Y' _chemical_formula_weight 898.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5064(8) _cell_length_b 18.8267(11) _cell_length_c 20.6945(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.3470(10) _cell_angle_gamma 90.00 _cell_volume 5219.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9508 _cell_measurement_theta_min 3.35 _cell_measurement_theta_max 28.49 _exptl_crystal_description Prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6146 _exptl_absorpt_correction_T_max 0.6791 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24387 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 25.02 _reflns_number_total 9178 _reflns_number_gt 7380 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+2.4685P] 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 9178 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0782 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.243558(14) 0.154587(10) 0.298174(9) 0.02332(6) Uani 1 1 d . . . N1 N 0.41321(11) 0.15406(9) 0.26719(8) 0.0259(4) Uani 1 1 d . . . N2 N 0.22649(12) 0.17629(9) 0.18881(8) 0.0272(4) Uani 1 1 d . . . N3 N 0.06951(12) 0.18695(9) 0.26879(8) 0.0277(4) Uani 1 1 d . . . Si1 Si 0.26664(5) -0.01326(3) 0.39911(3) 0.03512(15) Uani 1 1 d . . . Si2 Si 0.28508(5) 0.32469(4) 0.39335(3) 0.03939(17) Uani 1 1 d . . . C1 C 0.21623(16) 0.03342(11) 0.32408(11) 0.0337(5) Uani 1 1 d . . . H1A H 0.1444 0.0278 0.3206 0.040 Uiso 1 1 calc R . . H1B H 0.2376 0.0060 0.2887 0.040 Uiso 1 1 calc R . . C2 C 0.3164(3) -0.10349(15) 0.38244(16) 0.0718(9) Uani 1 1 d . . . H2A H 0.2676 -0.1289 0.3534 0.108 Uiso 1 1 calc R . . H2B H 0.3303 -0.1292 0.4226 0.108 Uiso 1 1 calc R . . H2C H 0.3766 -0.0986 0.3627 0.108 Uiso 1 1 calc R . . C3 C 0.37365(19) 0.03397(15) 0.44641(12) 0.0514(7) Uani 1 1 d . . . H3A H 0.4288 0.0354 0.4214 0.077 Uiso 1 1 calc R . . H3B H 0.3932 0.0093 0.4866 0.077 Uiso 1 1 calc R . . H3C H 0.3540 0.0816 0.4555 0.077 Uiso 1 1 calc R . . C4 C 0.1694(2) -0.02248(19) 0.45485(14) 0.0692(9) Uani 1 1 d . . . H4A H 0.1543 0.0234 0.4712 0.104 Uiso 1 1 calc R . . H4B H 0.1938 -0.0529 0.4906 0.104 Uiso 1 1 calc R . . H4C H 0.1101 -0.0427 0.4315 0.104 Uiso 1 1 calc R . . C5 C 0.27212(16) 0.22778(12) 0.39311(11) 0.0342(5) Uani 1 1 d . . . H5A H 0.2181 0.2175 0.4183 0.041 Uiso 1 1 calc R . . H5B H 0.3324 0.2097 0.4182 0.041 Uiso 1 1 calc R . . C6 C 0.3205(2) 0.35526(14) 0.31311(15) 0.0654(9) Uani 1 1 d . . . H6A H 0.3832 0.3343 0.3063 0.098 Uiso 1 1 calc R . . H6B H 0.3266 0.4061 0.3133 0.098 Uiso 1 1 calc R . . H6C H 0.2700 0.3410 0.2787 0.098 Uiso 1 1 calc R . . C7 C 0.1654(2) 0.36838(15) 0.40685(14) 0.0544(7) Uani 1 1 d . . . H7A H 0.1127 0.3518 0.3748 0.082 Uiso 1 1 calc R . . H7B H 0.1720 0.4189 0.4030 0.082 Uiso 1 1 calc R . . H7C H 0.1499 0.3569 0.4496 0.082 Uiso 1 1 calc R . . C8 C 0.3840(2) 0.35994(16) 0.45709(17) 0.0719(10) Uani 1 1 d . . . H8A H 0.3745 0.3407 0.4988 0.108 Uiso 1 1 calc R . . H8B H 0.3796 0.4108 0.4585 0.108 Uiso 1 1 calc R . . H8C H 0.4486 0.3464 0.4466 0.108 Uiso 1 1 calc R . . C9 C 0.48766(14) 0.10470(11) 0.29744(10) 0.0286(5) Uani 1 1 d . . . C10 C 0.49023(16) 0.03687(12) 0.26946(12) 0.0358(5) Uani 1 1 d . . . C11 C 0.56166(18) -0.01022(13) 0.29826(13) 0.0457(6) Uani 1 1 d . . . H11 H 0.5648 -0.0558 0.2813 0.055 Uiso 1 1 calc R . . C12 C 0.62797(18) 0.00932(14) 0.35149(14) 0.0489(7) Uani 1 1 d . . . H12 H 0.6760 -0.0228 0.3697 0.059 Uiso 1 1 calc R . . C13 C 0.62332(17) 0.07582(14) 0.37760(12) 0.0422(6) Uani 1 1 d . . . H13 H 0.6688 0.0883 0.4134 0.051 Uiso 1 1 calc R . . C14 C 0.55224(15) 0.12545(12) 0.35193(11) 0.0318(5) Uani 1 1 d . . . C15 C 0.42131(17) 0.01717(13) 0.20813(13) 0.0439(6) Uani 1 1 d . . . H15 H 0.3613 0.0466 0.2071 0.053 Uiso 1 1 calc R . . C16 C 0.4689(2) 0.03437(17) 0.14698(13) 0.0595(8) Uani 1 1 d . . . H16A H 0.4873 0.0836 0.1474 0.089 Uiso 1 1 calc R . . H16B H 0.4220 0.0248 0.1091 0.089 Uiso 1 1 calc R . . H16C H 0.5273 0.0055 0.1459 0.089 Uiso 1 1 calc R . . C26 C 0.23409(17) 0.26164(12) 0.10138(10) 0.0356(5) Uani 1 1 d . . . H26 H 0.1679 0.2521 0.0856 0.043 Uiso 1 1 calc R . . C17 C 0.3877(2) -0.06021(15) 0.20602(17) 0.0681(9) Uani 1 1 d . . . H17A H 0.4443 -0.0905 0.2040 0.102 Uiso 1 1 calc R . . H17B H 0.3398 -0.0678 0.1682 0.102 Uiso 1 1 calc R . . H17C H 0.3578 -0.0710 0.2445 0.102 Uiso 1 1 calc R . . C18 C 0.54769(16) 0.19824(13) 0.38215(11) 0.0376(6) Uani 1 1 d . . . H18 H 0.4801 0.2168 0.3697 0.045 Uiso 1 1 calc R . . C19 C 0.6204(2) 0.25003(14) 0.35641(14) 0.0561(7) Uani 1 1 d . . . H19A H 0.6873 0.2326 0.3667 0.084 Uiso 1 1 calc R . . H19B H 0.6149 0.2957 0.3764 0.084 Uiso 1 1 calc R . . H19C H 0.6046 0.2544 0.3100 0.084 Uiso 1 1 calc R . . C20 C 0.5664(2) 0.19657(16) 0.45646(12) 0.0570(7) Uani 1 1 d . . . H20A H 0.5249 0.1609 0.4725 0.086 Uiso 1 1 calc R . . H20B H 0.5507 0.2421 0.4734 0.086 Uiso 1 1 calc R . . H20C H 0.6353 0.1857 0.4703 0.086 Uiso 1 1 calc R . . C21 C 0.44265(15) 0.19354(11) 0.22277(10) 0.0294(5) Uani 1 1 d . . . H21 H 0.5110 0.1941 0.2206 0.035 Uiso 1 1 calc R . . C22 C 0.38212(15) 0.23722(11) 0.17579(10) 0.0274(5) Uani 1 1 d . . . C23 C 0.43194(17) 0.28867(12) 0.14278(11) 0.0357(5) Uani 1 1 d . . . H23 H 0.4996 0.2966 0.1556 0.043 Uiso 1 1 calc R . . C24 C 0.38412(19) 0.32724(12) 0.09255(12) 0.0401(6) Uani 1 1 d . . . H24 H 0.4176 0.3627 0.0728 0.048 Uiso 1 1 calc R . . C25 C 0.28464(18) 0.31268(13) 0.07145(11) 0.0396(6) Uani 1 1 d . . . H25 H 0.2517 0.3379 0.0365 0.047 Uiso 1 1 calc R . . C27 C 0.27997(15) 0.22350(11) 0.15531(10) 0.0269(5) Uani 1 1 d . . . C28 C 0.16306(15) 0.12793(11) 0.15389(10) 0.0285(5) Uani 1 1 d . . . C29 C 0.18952(17) 0.09334(13) 0.09844(11) 0.0372(5) Uani 1 1 d . . . H29 H 0.2468 0.1076 0.0814 0.045 Uiso 1 1 calc R . . C30 C 0.13339(19) 0.03926(14) 0.06884(12) 0.0460(6) Uani 1 1 d . . . H30 H 0.1540 0.0168 0.0328 0.055 Uiso 1 1 calc R . . C31 C 0.04580(19) 0.01720(14) 0.09176(13) 0.0494(7) Uani 1 1 d . . . H31 H 0.0090 -0.0206 0.0723 0.059 Uiso 1 1 calc R . . C32 C 0.01511(18) 0.05223(13) 0.14330(12) 0.0425(6) Uani 1 1 d . . . H32 H -0.0449 0.0392 0.1575 0.051 Uiso 1 1 calc R . . C33 C 0.07134(15) 0.10756(12) 0.17579(10) 0.0306(5) Uani 1 1 d . . . C34 C 0.02468(15) 0.14885(12) 0.22241(10) 0.0313(5) Uani 1 1 d . . . H34 H -0.0447 0.1478 0.2185 0.038 Uiso 1 1 calc R . . C35 C 0.00604(15) 0.23650(12) 0.29790(11) 0.0320(5) Uani 1 1 d . . . C36 C -0.01526(17) 0.30149(13) 0.26586(12) 0.0407(6) Uani 1 1 d . . . C37 C -0.08078(19) 0.34736(15) 0.29169(14) 0.0533(7) Uani 1 1 d . . . H37 H -0.0976 0.3903 0.2710 0.064 Uiso 1 1 calc R . . C38 C -0.12081(19) 0.32996(15) 0.34727(14) 0.0547(7) Uani 1 1 d . . . H38 H -0.1662 0.3605 0.3631 0.066 Uiso 1 1 calc R . . C39 C -0.09438(18) 0.26780(15) 0.37980(13) 0.0480(7) Uani 1 1 d . . . H39 H -0.1201 0.2579 0.4184 0.058 Uiso 1 1 calc R . . C40 C -0.02998(15) 0.21939(13) 0.35623(11) 0.0349(5) Uani 1 1 d . . . C41 C 0.0326(2) 0.32219(14) 0.20600(13) 0.0524(7) Uani 1 1 d . . . H41 H 0.0934 0.2937 0.2063 0.063 Uiso 1 1 calc R . . C42 C -0.0345(2) 0.3049(2) 0.14340(15) 0.0785(10) Uani 1 1 d . . . H42A H -0.0472 0.2548 0.1413 0.118 Uiso 1 1 calc R . . H42B H -0.0022 0.3191 0.1067 0.118 Uiso 1 1 calc R . . H42C H -0.0965 0.3300 0.1426 0.118 Uiso 1 1 calc R . . C43 C 0.0639(3) 0.40054(16) 0.20714(18) 0.0816(11) Uani 1 1 d . . . H43A H 0.0055 0.4300 0.2010 0.122 Uiso 1 1 calc R . . H43B H 0.1039 0.4093 0.1728 0.122 Uiso 1 1 calc R . . H43C H 0.1020 0.4114 0.2484 0.122 Uiso 1 1 calc R . . C44 C -0.00220(17) 0.15092(13) 0.39195(11) 0.0385(5) Uani 1 1 d . . . H44 H 0.0623 0.1357 0.3798 0.046 Uiso 1 1 calc R . . C45 C -0.0774(2) 0.09192(15) 0.37143(14) 0.0554(7) Uani 1 1 d . . . H45A H -0.1421 0.1058 0.3815 0.083 Uiso 1 1 calc R . . H45B H -0.0569 0.0491 0.3945 0.083 Uiso 1 1 calc R . . H45C H -0.0804 0.0838 0.3254 0.083 Uiso 1 1 calc R . . C46 C 0.0109(2) 0.15979(17) 0.46572(12) 0.0573(7) Uani 1 1 d . . . H46A H 0.0560 0.1984 0.4778 0.086 Uiso 1 1 calc R . . H46B H 0.0376 0.1168 0.4859 0.086 Uiso 1 1 calc R . . H46C H -0.0526 0.1698 0.4799 0.086 Uiso 1 1 calc R . . C47 C 0.7264(3) 0.1274(2) 0.09244(19) 0.0876(11) Uani 1 1 d . . . C48 C 0.7238(3) 0.19337(19) 0.1211(2) 0.0864(11) Uani 1 1 d . A . H48 H 0.7189 0.2336 0.0948 0.104 Uiso 1 1 calc R . . C49 C 0.7282(2) 0.20115(19) 0.18659(18) 0.0725(9) Uani 1 1 d . . . H49 H 0.7253 0.2463 0.2045 0.087 Uiso 1 1 calc R A . C50 C 0.7368(2) 0.1437(2) 0.22560(18) 0.0726(10) Uani 1 1 d . A . H50 H 0.7403 0.1489 0.2705 0.087 Uiso 1 1 calc R . . C51 C 0.7404(2) 0.0782(2) 0.1988(2) 0.0808(11) Uani 1 1 d . . . H51 H 0.7467 0.0384 0.2257 0.097 Uiso 1 1 calc R A . C52 C 0.7348(3) 0.06967(19) 0.1335(2) 0.0830(11) Uani 1 1 d . A . H52 H 0.7368 0.0242 0.1162 0.100 Uiso 1 1 calc R . . C53 C 0.6940(10) 0.1072(6) 0.0218(4) 0.100(4) Uiso 0.520(17) 1 d P A 1 H53A H 0.7439 0.0774 0.0066 0.150 Uiso 0.520(17) 1 calc PR A 1 H53B H 0.6860 0.1494 -0.0044 0.150 Uiso 0.520(17) 1 calc PR A 1 H53C H 0.6317 0.0821 0.0184 0.150 Uiso 0.520(17) 1 calc PR A 1 C53' C 0.7505(11) 0.1322(6) 0.0172(4) 0.100(4) Uiso 0.480(17) 1 d P A 2 H53D H 0.8200 0.1224 0.0158 0.150 Uiso 0.480(17) 1 calc PR A 2 H53E H 0.7352 0.1791 0.0005 0.150 Uiso 0.480(17) 1 calc PR A 2 H53F H 0.7107 0.0980 -0.0089 0.150 Uiso 0.480(17) 1 calc PR A 2 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 0.02169(10) 0.02689(11) 0.02152(11) 0.00356(9) 0.00328(7) 0.00026(9) N1 0.0215(8) 0.0291(9) 0.0270(9) 0.0017(8) 0.0029(7) -0.0006(8) N2 0.0216(8) 0.0365(10) 0.0239(9) 0.0039(8) 0.0037(7) -0.0028(7) N3 0.0239(9) 0.0344(10) 0.0253(10) 0.0054(8) 0.0049(7) 0.0032(8) Si1 0.0350(3) 0.0316(3) 0.0378(4) 0.0104(3) 0.0009(3) -0.0033(3) Si2 0.0393(4) 0.0356(4) 0.0447(4) -0.0095(3) 0.0111(3) -0.0048(3) C1 0.0350(12) 0.0315(12) 0.0347(13) 0.0011(10) 0.0045(10) -0.0003(10) C2 0.093(2) 0.0429(16) 0.074(2) 0.0116(15) -0.0109(18) 0.0166(16) C3 0.0484(15) 0.0603(17) 0.0427(15) 0.0106(13) -0.0049(12) -0.0103(13) C4 0.0503(17) 0.105(3) 0.0534(18) 0.0302(18) 0.0096(14) -0.0068(17) C5 0.0318(12) 0.0388(13) 0.0327(13) -0.0010(10) 0.0068(10) -0.0045(10) C6 0.083(2) 0.0425(16) 0.078(2) 0.0080(15) 0.0363(18) -0.0011(15) C7 0.0519(16) 0.0503(16) 0.0629(19) -0.0140(14) 0.0142(14) 0.0028(13) C8 0.0547(18) 0.0573(19) 0.100(3) -0.0299(18) -0.0054(17) -0.0084(14) C9 0.0209(10) 0.0324(12) 0.0339(12) 0.0092(10) 0.0085(9) 0.0010(9) C10 0.0282(11) 0.0354(13) 0.0455(14) 0.0042(11) 0.0113(10) 0.0028(10) C11 0.0408(14) 0.0350(13) 0.0632(18) 0.0054(13) 0.0143(13) 0.0079(11) C12 0.0355(13) 0.0480(16) 0.0635(18) 0.0229(14) 0.0080(13) 0.0129(12) C13 0.0285(12) 0.0529(16) 0.0442(15) 0.0166(13) 0.0002(10) 0.0009(11) C14 0.0239(11) 0.0366(12) 0.0351(13) 0.0110(10) 0.0047(9) -0.0021(9) C15 0.0333(12) 0.0402(14) 0.0584(17) -0.0109(12) 0.0066(11) 0.0035(11) C16 0.0579(17) 0.070(2) 0.0510(17) -0.0132(15) 0.0088(14) 0.0059(15) C26 0.0321(12) 0.0466(14) 0.0273(12) 0.0058(11) 0.0012(9) 0.0009(10) C17 0.0599(18) 0.0485(17) 0.096(3) -0.0243(17) 0.0116(17) -0.0038(14) C18 0.0283(12) 0.0449(14) 0.0376(14) 0.0027(11) -0.0037(10) -0.0012(10) C19 0.0612(17) 0.0472(16) 0.0592(18) 0.0043(14) 0.0045(14) -0.0164(13) C20 0.0604(18) 0.0653(19) 0.0427(16) -0.0016(14) -0.0040(13) -0.0122(15) C21 0.0218(10) 0.0341(12) 0.0323(12) -0.0013(10) 0.0040(9) -0.0042(9) C22 0.0277(11) 0.0294(11) 0.0259(11) 0.0028(9) 0.0061(9) -0.0009(9) C23 0.0330(12) 0.0391(13) 0.0356(13) 0.0024(11) 0.0070(10) -0.0082(10) C24 0.0510(15) 0.0354(13) 0.0360(14) 0.0080(11) 0.0130(11) -0.0060(11) C25 0.0486(14) 0.0431(14) 0.0269(12) 0.0097(11) 0.0044(11) 0.0026(12) C27 0.0277(11) 0.0324(12) 0.0215(11) 0.0000(9) 0.0067(9) 0.0010(9) C28 0.0261(11) 0.0357(12) 0.0225(11) 0.0045(9) -0.0012(9) 0.0015(9) C29 0.0348(12) 0.0472(14) 0.0310(13) 0.0003(11) 0.0092(10) -0.0014(11) C30 0.0534(15) 0.0505(15) 0.0347(14) -0.0121(12) 0.0075(12) -0.0026(13) C31 0.0546(16) 0.0487(16) 0.0444(16) -0.0107(13) 0.0037(13) -0.0166(13) C32 0.0363(13) 0.0514(15) 0.0395(14) -0.0010(12) 0.0046(11) -0.0132(11) C33 0.0261(11) 0.0382(13) 0.0271(12) 0.0035(10) 0.0016(9) -0.0021(9) C34 0.0222(10) 0.0420(13) 0.0302(12) 0.0092(11) 0.0052(9) -0.0032(10) C35 0.0219(10) 0.0401(13) 0.0342(13) -0.0009(10) 0.0042(9) 0.0036(9) C36 0.0304(12) 0.0449(14) 0.0472(15) 0.0063(12) 0.0067(11) 0.0096(11) C37 0.0416(14) 0.0487(15) 0.0696(19) 0.0060(15) 0.0081(13) 0.0162(13) C38 0.0389(14) 0.0595(18) 0.068(2) -0.0111(15) 0.0168(13) 0.0138(13) C39 0.0374(13) 0.0620(17) 0.0476(16) -0.0063(14) 0.0170(12) 0.0033(13) C40 0.0246(11) 0.0461(14) 0.0346(13) -0.0030(11) 0.0057(9) -0.0024(10) C41 0.0503(15) 0.0527(16) 0.0565(18) 0.0248(14) 0.0162(13) 0.0206(13) C42 0.077(2) 0.103(3) 0.056(2) 0.0285(19) 0.0110(17) 0.023(2) C43 0.085(2) 0.060(2) 0.106(3) 0.038(2) 0.036(2) 0.0164(18) C44 0.0310(11) 0.0545(15) 0.0317(12) 0.0036(12) 0.0109(10) 0.0002(11) C45 0.0536(16) 0.0590(18) 0.0529(18) 0.0073(14) 0.0038(13) -0.0119(14) C46 0.0582(17) 0.079(2) 0.0355(15) 0.0041(14) 0.0092(12) -0.0017(15) C47 0.102(3) 0.082(3) 0.077(3) -0.002(2) 0.001(2) 0.035(2) C48 0.115(3) 0.058(2) 0.088(3) 0.017(2) 0.020(2) 0.024(2) C49 0.069(2) 0.066(2) 0.084(3) -0.002(2) 0.0160(18) 0.0037(17) C50 0.0484(17) 0.098(3) 0.074(2) 0.014(2) 0.0185(16) 0.0135(18) C51 0.060(2) 0.074(3) 0.111(3) 0.035(2) 0.021(2) -0.0027(18) C52 0.069(2) 0.057(2) 0.120(3) -0.009(2) -0.001(2) 0.0072(17) _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 2.2823(17) . ? Y1 C1 2.383(2) . ? Y1 C5 2.390(2) . ? Y1 N3 2.4293(16) . ? Y1 N1 2.4572(16) . ? N1 C21 1.284(3) . ? N1 C9 1.451(3) . ? N2 C27 1.386(3) . ? N2 C28 1.388(3) . ? N3 C34 1.286(3) . ? N3 C35 1.449(3) . ? Si1 C1 1.837(2) . ? Si1 C4 1.863(3) . ? Si1 C3 1.864(2) . ? Si1 C2 1.875(3) . ? Si2 C5 1.833(2) . ? Si2 C7 1.866(3) . ? Si2 C8 1.875(3) . ? Si2 C6 1.877(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? 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 C14 1.390(3) . ? C9 C10 1.404(3) . ? C10 C11 1.387(3) . ? C10 C15 1.521(3) . ? C11 C12 1.378(4) . ? C11 H11 0.9300 . ? C12 C13 1.368(4) . ? C12 H12 0.9300 . ? C13 C14 1.395(3) . ? C13 H13 0.9300 . ? C14 C18 1.511(3) . ? C15 C17 1.525(4) . ? C15 C16 1.526(4) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C26 C25 1.372(3) . ? C26 C27 1.403(3) . ? C26 H26 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C20 1.527(3) . ? C18 C19 1.527(3) . ? C18 H18 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.444(3) . ? C21 H21 0.9300 . ? C22 C23 1.405(3) . ? C22 C27 1.414(3) . ? C23 C24 1.362(3) . ? C23 H23 0.9300 . ? C24 C25 1.386(3) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C28 C29 1.405(3) . ? C28 C33 1.425(3) . ? C29 C30 1.367(3) . ? C29 H29 0.9300 . ? C30 C31 1.393(3) . ? C30 H30 0.9300 . ? C31 C32 1.363(3) . ? C31 H31 0.9300 . ? C32 C33 1.408(3) . ? C32 H32 0.9300 . ? C33 C34 1.445(3) . ? C34 H34 0.9300 . ? C35 C40 1.396(3) . ? C35 C36 1.404(3) . ? C36 C37 1.391(3) . ? C36 C41 1.520(3) . ? C37 C38 1.372(4) . ? C37 H37 0.9300 . ? C38 C39 1.374(4) . ? C38 H38 0.9300 . ? C39 C40 1.391(3) . ? C39 H39 0.9300 . ? C40 C44 1.509(3) . ? C41 C42 1.518(4) . ? C41 C43 1.534(4) . ? C41 H41 0.9800 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C46 1.523(3) . ? C44 C45 1.528(3) . ? C44 H44 0.9800 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C52 1.375(5) . ? C47 C48 1.378(5) . ? C47 C53 1.520(9) . ? C47 C53' 1.633(10) . ? C48 C49 1.358(5) . ? C48 H48 0.9300 . ? C49 C50 1.345(5) . ? C49 H49 0.9300 . ? C50 C51 1.357(5) . ? C50 H50 0.9300 . ? C51 C52 1.352(5) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C53' H53D 0.9600 . ? C53' H53E 0.9600 . ? C53' H53F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Y1 C1 113.30(7) . . ? N2 Y1 C5 134.19(7) . . ? C1 Y1 C5 112.35(8) . . ? N2 Y1 N3 74.63(6) . . ? C1 Y1 N3 97.11(7) . . ? C5 Y1 N3 96.34(7) . . ? N2 Y1 N1 73.82(6) . . ? C1 Y1 N1 103.37(7) . . ? C5 Y1 N1 99.14(7) . . ? N3 Y1 N1 147.20(6) . . ? C21 N1 C9 114.75(16) . . ? C21 N1 Y1 124.68(13) . . ? C9 N1 Y1 120.52(12) . . ? C27 N2 C28 119.12(17) . . ? C27 N2 Y1 128.16(13) . . ? C28 N2 Y1 112.10(13) . . ? C34 N3 C35 114.98(17) . . ? C34 N3 Y1 113.27(14) . . ? C35 N3 Y1 131.47(13) . . ? C1 Si1 C4 110.70(12) . . ? C1 Si1 C3 113.22(11) . . ? C4 Si1 C3 106.24(14) . . ? C1 Si1 C2 112.37(12) . . ? C4 Si1 C2 109.07(16) . . ? C3 Si1 C2 104.88(14) . . ? C5 Si2 C7 110.78(12) . . ? C5 Si2 C8 114.43(13) . . ? C7 Si2 C8 106.97(13) . . ? C5 Si2 C6 109.75(12) . . ? C7 Si2 C6 108.74(14) . . ? C8 Si2 C6 105.92(16) . . ? Si1 C1 Y1 126.63(11) . . ? Si1 C1 H1A 105.7 . . ? Y1 C1 H1A 105.7 . . ? Si1 C1 H1B 105.7 . . ? Y1 C1 H1B 105.7 . . ? H1A C1 H1B 106.1 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 Y1 125.56(11) . . ? Si2 C5 H5A 105.9 . . ? Y1 C5 H5A 105.9 . . ? Si2 C5 H5B 105.9 . . ? Y1 C5 H5B 105.9 . . ? H5A C5 H5B 106.3 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 122.9(2) . . ? C14 C9 N1 119.87(19) . . ? C10 C9 N1 117.18(19) . . ? C11 C10 C9 117.2(2) . . ? C11 C10 C15 121.4(2) . . ? C9 C10 C15 121.4(2) . . ? C12 C11 C10 121.2(2) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C13 C12 C11 120.1(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 121.8(2) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C9 C14 C13 116.8(2) . . ? C9 C14 C18 122.42(19) . . ? C13 C14 C18 120.8(2) . . ? C10 C15 C17 113.9(2) . . ? C10 C15 C16 111.3(2) . . ? C17 C15 C16 109.5(2) . . ? C10 C15 H15 107.3 . . ? C17 C15 H15 107.3 . . ? C16 C15 H15 107.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C25 C26 C27 121.5(2) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C20 112.8(2) . . ? C14 C18 C19 111.9(2) . . ? C20 C18 C19 109.5(2) . . ? C14 C18 H18 107.5 . . ? C20 C18 H18 107.5 . . ? C19 C18 H18 107.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 C22 127.65(19) . . ? N1 C21 H21 116.2 . . ? C22 C21 H21 116.2 . . ? C23 C22 C27 119.31(19) . . ? C23 C22 C21 117.03(19) . . ? C27 C22 C21 122.97(18) . . ? C24 C23 C22 121.9(2) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 118.8(2) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C26 C25 C24 121.0(2) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? N2 C27 C26 121.38(18) . . ? N2 C27 C22 121.21(18) . . ? C26 C27 C22 117.37(19) . . ? N2 C28 C29 121.66(19) . . ? N2 C28 C33 120.98(19) . . ? C29 C28 C33 117.2(2) . . ? C30 C29 C28 121.8(2) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C29 C30 C31 121.1(2) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 118.6(2) . . ? C32 C31 H31 120.7 . . ? C30 C31 H31 120.7 . . ? C31 C32 C33 122.2(2) . . ? C31 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C32 C33 C28 119.0(2) . . ? C32 C33 C34 117.53(19) . . ? C28 C33 C34 122.59(19) . . ? N3 C34 C33 126.48(19) . . ? N3 C34 H34 116.8 . . ? C33 C34 H34 116.8 . . ? C40 C35 C36 122.5(2) . . ? C40 C35 N3 120.1(2) . . ? C36 C35 N3 117.45(19) . . ? C37 C36 C35 117.5(2) . . ? C37 C36 C41 120.8(2) . . ? C35 C36 C41 121.7(2) . . ? C38 C37 C36 120.8(2) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 120.6(2) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C40 121.4(2) . . ? C38 C39 H39 119.3 . . ? C40 C39 H39 119.3 . . ? C39 C40 C35 117.1(2) . . ? C39 C40 C44 121.0(2) . . ? C35 C40 C44 121.9(2) . . ? C42 C41 C36 111.7(2) . . ? C42 C41 C43 110.6(3) . . ? C36 C41 C43 112.3(2) . . ? C42 C41 H41 107.3 . . ? C36 C41 H41 107.3 . . ? C43 C41 H41 107.3 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 C46 112.8(2) . . ? C40 C44 C45 111.71(19) . . ? C46 C44 C45 110.2(2) . . ? C40 C44 H44 107.3 . . ? C46 C44 H44 107.3 . . ? C45 C44 H44 107.3 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C52 C47 C48 116.8(4) . . ? C52 C47 C53 112.8(5) . . ? C48 C47 C53 128.2(5) . . ? C52 C47 C53' 128.5(5) . . ? C48 C47 C53' 112.2(5) . . ? C53 C47 C53' 33.4(4) . . ? C49 C48 C47 121.7(4) . . ? C49 C48 H48 119.1 . . ? C47 C48 H48 119.1 . . ? C50 C49 C48 120.1(4) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C49 C50 C51 119.3(4) . . ? C49 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C52 C51 C50 121.1(3) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C51 C52 C47 120.9(4) . . ? C51 C52 H52 119.6 . . ? C47 C52 H52 119.6 . . ? C47 C53 H53A 109.5 . . ? C47 C53 H53B 109.5 . . ? C47 C53 H53C 109.5 . . ? C47 C53' H53D 109.5 . . ? C47 C53' H53E 109.5 . . ? H53D C53' H53E 109.5 . . ? C47 C53' H53F 109.5 . . ? H53D C53' H53F 109.5 . . ? H53E C53' H53F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.293 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.041