# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dongtao Liu' _publ_contact_author_email liudt@ciac.jl.cn _publ_author_name 'Dongtao Liu' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 780668' #TrackingRef '- cif of complexes 1,2,3,5.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H53 N2 O Si2 Y' _chemical_formula_weight 638.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.4555(12) _cell_length_b 16.8260(18) _cell_length_c 18.987(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.752(2) _cell_angle_gamma 90.00 _cell_volume 3607.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7263 _exptl_absorpt_correction_T_max 0.8085 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19968 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0845 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.07 _reflns_number_total 7105 _reflns_number_gt 4435 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0984P)^2^+1.4058P] 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 7105 _refine_ls_number_parameters 344 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1159 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.1898 _refine_ls_wR_factor_gt 0.1655 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.14241(4) 0.27407(3) 0.34180(3) 0.03299(18) Uani 1 1 d . . . N1 N 0.0593(3) 0.2353(2) 0.4472(2) 0.0312(9) Uani 1 1 d . . . N2 N 0.2350(3) 0.1617(2) 0.3948(2) 0.0309(9) Uani 1 1 d . . . O1 O 0.2760(3) 0.2945(2) 0.26322(19) 0.0465(10) Uani 1 1 d . . . Si1 Si -0.16898(13) 0.21023(10) 0.26028(8) 0.0421(4) Uani 1 1 d . . . Si2 Si 0.25689(17) 0.44969(10) 0.44839(10) 0.0559(5) Uani 1 1 d . . . C1 C -0.0272(5) 0.2741(3) 0.4722(3) 0.0406(13) Uani 1 1 d . . . H1 H -0.0521 0.3230 0.4522 0.049 Uiso 1 1 calc R . . C2 C -0.0814(5) 0.2443(4) 0.5267(3) 0.0468(15) Uani 1 1 d . . . H2 H -0.1409 0.2729 0.5430 0.056 Uiso 1 1 calc R . . C3 C -0.0455(5) 0.1718(3) 0.5562(3) 0.0416(14) Uani 1 1 d . . . H3 H -0.0820 0.1508 0.5922 0.050 Uiso 1 1 calc R . . C4 C 0.0460(4) 0.1294(3) 0.5322(2) 0.0322(11) Uani 1 1 d . . . C5 C 0.0875(5) 0.0557(3) 0.5610(3) 0.0401(13) Uani 1 1 d . . . H5 H 0.0551 0.0328 0.5979 0.048 Uiso 1 1 calc R . . C6 C 0.1768(4) 0.0178(3) 0.5340(3) 0.0398(13) Uani 1 1 d . . . H6 H 0.2037 -0.0313 0.5526 0.048 Uiso 1 1 calc R . . C7 C 0.2279(5) 0.0514(4) 0.4790(3) 0.0482(10) Uani 1 1 d . . . H7 H 0.2884 0.0243 0.4622 0.058 Uiso 1 1 calc R . . C8 C 0.1905(5) 0.1244(4) 0.4489(3) 0.0604(13) Uani 1 1 d . . . C9 C 0.0963(5) 0.1638(4) 0.4765(3) 0.0494(11) Uani 1 1 d . . . C10 C 0.3282(4) 0.1222(3) 0.3680(3) 0.0314(11) Uani 1 1 d . . . C11 C 0.4463(4) 0.1311(3) 0.4037(3) 0.0374(13) Uani 1 1 d . . . C12 C 0.5371(5) 0.0984(4) 0.3712(3) 0.0459(14) Uani 1 1 d . . . H12 H 0.6154 0.1044 0.3934 0.055 Uiso 1 1 calc R . . C13 C 0.5131(5) 0.0580(4) 0.3078(3) 0.0549(17) Uani 1 1 d . . . H13 H 0.5748 0.0380 0.2870 0.066 Uiso 1 1 calc R . . C14 C 0.3968(5) 0.0469(4) 0.2748(3) 0.0508(16) Uani 1 1 d . . . H14 H 0.3813 0.0181 0.2324 0.061 Uiso 1 1 calc R . . C15 C 0.3032(4) 0.0781(3) 0.3038(3) 0.0394(13) Uani 1 1 d . . . C16 C 0.4791(5) 0.1744(3) 0.4744(3) 0.0400(13) Uani 1 1 d . . . H16 H 0.4052 0.1888 0.4907 0.048 Uiso 1 1 calc R . . C17 C 0.5461(6) 0.2506(4) 0.4669(4) 0.0621(18) Uani 1 1 d . . . H17A H 0.6227 0.2382 0.4556 0.093 Uiso 1 1 calc R . . H17B H 0.5555 0.2797 0.5110 0.093 Uiso 1 1 calc R . . H17C H 0.5027 0.2823 0.4293 0.093 Uiso 1 1 calc R . . C18 C 0.5500(5) 0.1215(4) 0.5320(3) 0.0561(17) Uani 1 1 d . . . H18A H 0.5080 0.0727 0.5354 0.084 Uiso 1 1 calc R . . H18B H 0.5605 0.1485 0.5772 0.084 Uiso 1 1 calc R . . H18C H 0.6261 0.1102 0.5195 0.084 Uiso 1 1 calc R . . C19 C 0.1766(5) 0.0620(3) 0.2682(3) 0.0446(14) Uani 1 1 d . . . H19 H 0.1259 0.1001 0.2878 0.054 Uiso 1 1 calc R . . C20 C 0.1393(6) -0.0209(4) 0.2878(4) 0.070(2) Uani 1 1 d . . . H20A H 0.1869 -0.0599 0.2688 0.104 Uiso 1 1 calc R . . H20B H 0.0574 -0.0292 0.2680 0.104 Uiso 1 1 calc R . . H20C H 0.1502 -0.0260 0.3388 0.104 Uiso 1 1 calc R . . C21 C 0.1571(6) 0.0743(5) 0.1873(3) 0.083(2) Uani 1 1 d . . . H21A H 0.1937 0.1232 0.1766 0.125 Uiso 1 1 calc R . . H21B H 0.0737 0.0766 0.1691 0.125 Uiso 1 1 calc R . . H21C H 0.1917 0.0308 0.1653 0.125 Uiso 1 1 calc R . . C22 C 0.1426(5) 0.4107(4) 0.3783(3) 0.0513(15) Uani 1 1 d . . . H22A H 0.1442 0.4427 0.3360 0.062 Uiso 1 1 calc R . . H22B H 0.0669 0.4206 0.3931 0.062 Uiso 1 1 calc R . . C23 C -0.0262(4) 0.2561(3) 0.2510(3) 0.0405(13) Uani 1 1 d . . . H23A H -0.0458 0.3087 0.2316 0.049 Uiso 1 1 calc R . . H23B H 0.0021 0.2264 0.2135 0.049 Uiso 1 1 calc R . . C24 C 0.2969(6) 0.3737(4) 0.5213(3) 0.0679(19) Uani 1 1 d . . . H24A H 0.2274 0.3596 0.5406 0.102 Uiso 1 1 calc R . . H24B H 0.3552 0.3956 0.5586 0.102 Uiso 1 1 calc R . . H24C H 0.3285 0.3272 0.5021 0.102 Uiso 1 1 calc R . . C25 C 0.2130(9) 0.5408(4) 0.4948(4) 0.105(3) Uani 1 1 d . . . H25A H 0.1805 0.5795 0.4598 0.157 Uiso 1 1 calc R . . H25B H 0.2814 0.5626 0.5248 0.157 Uiso 1 1 calc R . . H25C H 0.1547 0.5268 0.5235 0.157 Uiso 1 1 calc R . . C26 C 0.3918(7) 0.4723(5) 0.4081(4) 0.083(2) Uani 1 1 d . . . H26A H 0.4208 0.4242 0.3900 0.124 Uiso 1 1 calc R . . H26B H 0.4521 0.4946 0.4439 0.124 Uiso 1 1 calc R . . H26C H 0.3717 0.5096 0.3697 0.124 Uiso 1 1 calc R . . C27 C -0.1436(5) 0.1129(4) 0.3073(4) 0.068(2) Uani 1 1 d . . . H27A H -0.1009 0.0782 0.2806 0.103 Uiso 1 1 calc R . . H27B H -0.2185 0.0893 0.3115 0.103 Uiso 1 1 calc R . . H27C H -0.0984 0.1211 0.3542 0.103 Uiso 1 1 calc R . . C28 C -0.2689(5) 0.1914(4) 0.1737(3) 0.0482(10) Uani 1 1 d . . . H28A H -0.2837 0.2405 0.1479 0.072 Uiso 1 1 calc R . . H28B H -0.3425 0.1698 0.1827 0.072 Uiso 1 1 calc R . . H28C H -0.2320 0.1544 0.1459 0.072 Uiso 1 1 calc R . . C29 C -0.2559(6) 0.2760(4) 0.3121(4) 0.070(2) Uani 1 1 d . . . H29A H -0.2106 0.2859 0.3586 0.105 Uiso 1 1 calc R . . H29B H -0.3289 0.2503 0.3170 0.105 Uiso 1 1 calc R . . H29C H -0.2726 0.3255 0.2873 0.105 Uiso 1 1 calc R . . C30 C 0.2368(5) 0.3424(4) 0.2003(3) 0.0494(11) Uani 1 1 d . . . H30A H 0.2362 0.3982 0.2128 0.059 Uiso 1 1 calc R . . H30B H 0.1575 0.3270 0.1779 0.059 Uiso 1 1 calc R . . C31 C 0.3213(7) 0.3275(6) 0.1522(4) 0.099(3) Uani 1 1 d . . . H31A H 0.2870 0.2924 0.1137 0.119 Uiso 1 1 calc R . . H31B H 0.3431 0.3770 0.1316 0.119 Uiso 1 1 calc R . . C32 C 0.4223(5) 0.2917(4) 0.1937(3) 0.0604(13) Uani 1 1 d U . . H32A H 0.4901 0.3267 0.1957 0.073 Uiso 1 1 calc R . . H32B H 0.4401 0.2422 0.1716 0.073 Uiso 1 1 calc R . . C33 C 0.4004(5) 0.2766(4) 0.2649(3) 0.0636(19) Uani 1 1 d . . . H33A H 0.4498 0.3103 0.2992 0.076 Uiso 1 1 calc R . . H33B H 0.4168 0.2215 0.2779 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0305(3) 0.0370(3) 0.0332(3) 0.0075(2) 0.01013(19) 0.0051(2) N1 0.027(2) 0.035(2) 0.033(2) -0.0026(19) 0.0065(17) 0.0041(19) N2 0.028(2) 0.034(2) 0.033(2) 0.0020(19) 0.0107(17) 0.0069(19) O1 0.033(2) 0.064(3) 0.045(2) 0.019(2) 0.0116(17) 0.0092(19) Si1 0.0319(8) 0.0560(11) 0.0390(8) 0.0113(8) 0.0076(6) 0.0007(7) Si2 0.0764(13) 0.0385(10) 0.0542(11) -0.0018(8) 0.0152(9) 0.0015(9) C1 0.039(3) 0.046(3) 0.040(3) 0.007(3) 0.013(2) 0.012(3) C2 0.048(3) 0.051(4) 0.047(3) -0.007(3) 0.025(3) 0.009(3) C3 0.041(3) 0.056(4) 0.032(3) 0.000(3) 0.017(2) -0.003(3) C4 0.031(3) 0.039(3) 0.026(2) -0.002(2) 0.004(2) -0.002(2) C5 0.041(3) 0.047(3) 0.033(3) 0.008(3) 0.008(2) -0.004(3) C6 0.037(3) 0.036(3) 0.045(3) 0.008(3) 0.006(2) 0.006(3) C7 0.042(2) 0.054(3) 0.049(2) -0.001(2) 0.0077(19) -0.001(2) C8 0.047(2) 0.080(3) 0.058(2) 0.016(2) 0.019(2) 0.015(2) C9 0.041(2) 0.064(3) 0.045(2) 0.018(2) 0.0122(19) 0.011(2) C10 0.028(3) 0.031(3) 0.039(3) 0.005(2) 0.015(2) 0.003(2) C11 0.036(3) 0.038(3) 0.041(3) 0.003(3) 0.012(2) 0.004(2) C12 0.032(3) 0.055(4) 0.052(3) -0.007(3) 0.012(3) 0.005(3) C13 0.038(3) 0.071(5) 0.059(4) -0.009(3) 0.020(3) 0.011(3) C14 0.051(4) 0.053(4) 0.052(4) -0.024(3) 0.021(3) -0.004(3) C15 0.035(3) 0.044(3) 0.042(3) 0.000(3) 0.014(2) 0.000(3) C16 0.029(3) 0.044(3) 0.048(3) -0.003(3) 0.011(2) 0.005(3) C17 0.064(4) 0.062(4) 0.062(4) -0.012(4) 0.014(3) -0.015(4) C18 0.057(4) 0.064(4) 0.045(3) -0.002(3) 0.002(3) 0.013(3) C19 0.044(3) 0.045(3) 0.045(3) -0.013(3) 0.010(3) 0.000(3) C20 0.056(4) 0.068(5) 0.085(5) -0.008(4) 0.012(4) -0.017(4) C21 0.065(5) 0.130(8) 0.052(4) -0.011(5) 0.002(4) -0.002(5) C22 0.058(4) 0.045(3) 0.053(4) 0.008(3) 0.015(3) 0.006(3) C23 0.034(3) 0.047(3) 0.042(3) 0.015(3) 0.010(2) 0.005(3) C24 0.086(5) 0.057(4) 0.058(4) 0.002(4) 0.004(4) 0.003(4) C25 0.181(9) 0.047(4) 0.094(6) -0.011(4) 0.045(6) 0.024(5) C26 0.089(6) 0.078(5) 0.080(5) 0.005(4) 0.013(4) -0.018(5) C27 0.043(4) 0.070(5) 0.093(5) 0.036(4) 0.013(3) -0.005(3) C28 0.042(2) 0.054(3) 0.049(2) -0.001(2) 0.0077(19) -0.001(2) C29 0.048(4) 0.099(6) 0.066(4) -0.004(4) 0.018(3) 0.001(4) C30 0.041(2) 0.064(3) 0.045(2) 0.018(2) 0.0122(19) 0.011(2) C31 0.089(6) 0.160(9) 0.058(4) 0.052(5) 0.041(4) 0.058(6) C32 0.047(2) 0.080(3) 0.058(2) 0.016(2) 0.019(2) 0.015(2) C33 0.044(4) 0.088(5) 0.061(4) 0.026(4) 0.015(3) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N2 2.314(4) . ? Y1 O1 2.336(3) . ? Y1 C23 2.380(5) . ? Y1 C22 2.400(6) . ? Y1 N1 2.445(4) . ? N1 C1 1.339(6) . ? N1 C9 1.364(7) . ? N2 C8 1.374(7) . ? N2 C10 1.422(6) . ? O1 C30 1.448(6) . ? O1 C33 1.452(7) . ? Si1 C23 1.844(5) . ? Si1 C28 1.864(6) . ? Si1 C27 1.865(6) . ? Si1 C29 1.875(7) . ? Si2 C22 1.824(6) . ? Si2 C26 1.876(7) . ? Si2 C25 1.878(7) . ? Si2 C24 1.884(6) . ? C1 C2 1.387(7) . ? C2 C3 1.376(8) . ? C3 C4 1.406(7) . ? C4 C5 1.405(7) . ? C4 C9 1.412(7) . ? C5 C6 1.376(7) . ? C6 C7 1.399(7) . ? C7 C8 1.391(8) . ? C8 C9 1.438(8) . ? C10 C15 1.415(7) . ? C10 C11 1.415(7) . ? C11 C12 1.406(7) . ? C11 C16 1.518(7) . ? C12 C13 1.369(8) . ? C13 C14 1.385(8) . ? C14 C15 1.389(7) . ? C15 C19 1.516(7) . ? C16 C17 1.513(8) . ? C16 C18 1.532(7) . ? C19 C20 1.524(8) . ? C19 C21 1.529(8) . ? C30 C31 1.461(8) . ? C31 C32 1.419(8) . ? C32 C33 1.439(8) . ? 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 O1 95.54(13) . . ? N2 Y1 C23 117.87(17) . . ? O1 Y1 C23 95.45(15) . . ? N2 Y1 C22 132.77(17) . . ? O1 Y1 C22 94.27(18) . . ? C23 Y1 C22 106.9(2) . . ? N2 Y1 N1 68.87(13) . . ? O1 Y1 N1 161.72(13) . . ? C23 Y1 N1 100.27(16) . . ? C22 Y1 N1 90.04(17) . . ? C1 N1 C9 118.9(4) . . ? C1 N1 Y1 125.1(3) . . ? C9 N1 Y1 115.6(3) . . ? C8 N2 C10 116.8(4) . . ? C8 N2 Y1 119.8(3) . . ? C10 N2 Y1 122.8(3) . . ? C30 O1 C33 107.4(4) . . ? C30 O1 Y1 117.6(3) . . ? C33 O1 Y1 134.6(3) . . ? C23 Si1 C28 114.1(3) . . ? C23 Si1 C27 110.2(3) . . ? C28 Si1 C27 107.2(3) . . ? C23 Si1 C29 111.2(3) . . ? C28 Si1 C29 105.2(3) . . ? C27 Si1 C29 108.7(3) . . ? C22 Si2 C26 108.3(3) . . ? C22 Si2 C25 114.8(4) . . ? C26 Si2 C25 109.3(4) . . ? C22 Si2 C24 110.3(3) . . ? C26 Si2 C24 108.8(3) . . ? C25 Si2 C24 105.1(3) . . ? N1 C1 C2 122.7(5) . . ? C3 C2 C1 118.9(5) . . ? C2 C3 C4 120.4(5) . . ? C5 C4 C3 123.0(5) . . ? C5 C4 C9 119.9(5) . . ? C3 C4 C9 117.1(5) . . ? C6 C5 C4 119.2(5) . . ? C5 C6 C7 121.4(5) . . ? C8 C7 C6 121.6(5) . . ? N2 C8 C7 125.7(5) . . ? N2 C8 C9 117.3(6) . . ? C7 C8 C9 117.1(6) . . ? N1 C9 C4 122.0(5) . . ? N1 C9 C8 117.3(5) . . ? C4 C9 C8 120.7(5) . . ? C15 C10 C11 120.3(4) . . ? C15 C10 N2 119.9(4) . . ? C11 C10 N2 119.6(4) . . ? C12 C11 C10 117.9(5) . . ? C12 C11 C16 119.0(5) . . ? C10 C11 C16 123.2(4) . . ? C13 C12 C11 121.7(5) . . ? C12 C13 C14 120.0(5) . . ? C13 C14 C15 121.1(5) . . ? C14 C15 C10 118.9(5) . . ? C14 C15 C19 120.0(5) . . ? C10 C15 C19 121.1(4) . . ? C17 C16 C11 112.1(5) . . ? C17 C16 C18 110.1(5) . . ? C11 C16 C18 112.0(5) . . ? C15 C19 C20 109.9(5) . . ? C15 C19 C21 112.9(5) . . ? C20 C19 C21 111.7(6) . . ? Si2 C22 Y1 121.4(3) . . ? Si1 C23 Y1 127.4(3) . . ? O1 C30 C31 106.0(5) . . ? C32 C31 C30 106.8(5) . . ? C31 C32 C33 110.0(5) . . ? C32 C33 O1 105.6(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.713 _refine_diff_density_min -1.695 _refine_diff_density_rms 0.096 #===========END============= data_complex2 _database_code_depnum_ccdc_archive 'CCDC 780669' #TrackingRef '- cif of complexes 1,2,3,5.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H53 Lu N2 O Si2' _chemical_formula_weight 724.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.3890(5) _cell_length_b 16.7980(8) _cell_length_c 18.8840(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.7520(10) _cell_angle_gamma 90.00 _cell_volume 3560.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 147(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 2.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6266 _exptl_absorpt_correction_T_max 0.8032 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 147(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19474 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.04 _reflns_number_total 7004 _reflns_number_gt 5410 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+5.7865P] 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 7004 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 0.358602(17) 0.726958(12) 0.158090(11) 0.02632(7) Uani 1 1 d . . . N1 N 0.4408(3) 0.7629(2) 0.0544(2) 0.0260(8) Uani 1 1 d . . . N2 N 0.2652(3) 0.8369(2) 0.1064(2) 0.0251(8) Uani 1 1 d . . . O1 O 0.2279(3) 0.7102(2) 0.23639(18) 0.0418(9) Uani 1 1 d . . . Si1 Si 0.66806(12) 0.79082(9) 0.23813(8) 0.0342(3) Uani 1 1 d . . . Si2 Si 0.24159(16) 0.55280(9) 0.05315(9) 0.0456(4) Uani 1 1 d . . . C1 C 0.5252(4) 0.7230(3) 0.0286(3) 0.0325(11) Uani 1 1 d . . . H1 H 0.5482 0.6722 0.0485 0.039 Uiso 1 1 calc R . . C2 C 0.5813(5) 0.7520(3) -0.0260(3) 0.0379(12) Uani 1 1 d . . . H2 H 0.6424 0.7221 -0.0421 0.046 Uiso 1 1 calc R . . C3 C 0.5471(4) 0.8244(3) -0.0563(2) 0.0317(11) Uani 1 1 d . . . H3 H 0.5847 0.8451 -0.0936 0.038 Uiso 1 1 calc R . . C4 C 0.4560(4) 0.8681(3) -0.0319(2) 0.0246(10) Uani 1 1 d . . . C5 C 0.4140(4) 0.9424(3) -0.0611(3) 0.0316(11) Uani 1 1 d . . . H5 H 0.4471 0.9658 -0.0991 0.038 Uiso 1 1 calc R . . C6 C 0.3255(4) 0.9798(3) -0.0340(3) 0.0323(11) Uani 1 1 d . . . H6 H 0.2981 1.0300 -0.0532 0.039 Uiso 1 1 calc R . . C7 C 0.2737(4) 0.9470(3) 0.0212(2) 0.0294(11) Uani 1 1 d . . . H7 H 0.2118 0.9753 0.0382 0.035 Uiso 1 1 calc R . . C8 C 0.3102(4) 0.8737(3) 0.0522(2) 0.0235(10) Uani 1 1 d . . . C9 C 0.4039(5) 0.8342(4) 0.0238(3) 0.0576(13) Uani 1 1 d . . . C10 C 0.1707(4) 0.8771(3) 0.1326(2) 0.0243(10) Uani 1 1 d . . . C11 C 0.1961(4) 0.9221(3) 0.1965(3) 0.0299(11) Uani 1 1 d . . . C12 C 0.1011(5) 0.9544(3) 0.2252(3) 0.0417(13) Uani 1 1 d . . . H12 H 0.1168 0.9842 0.2685 0.050 Uiso 1 1 calc R . . C13 C -0.0144(5) 0.9437(3) 0.1917(3) 0.0435(14) Uani 1 1 d . . . H13 H -0.0780 0.9646 0.2127 0.052 Uiso 1 1 calc R . . C14 C -0.0386(4) 0.9029(3) 0.1279(3) 0.0339(12) Uani 1 1 d . . . H14 H -0.1189 0.8973 0.1047 0.041 Uiso 1 1 calc R . . C15 C 0.0522(4) 0.8694(3) 0.0962(3) 0.0294(11) Uani 1 1 d . . . C16 C 0.3233(4) 0.9388(3) 0.2327(3) 0.0379(12) Uani 1 1 d . . . H16 H 0.3759 0.9005 0.2123 0.046 Uiso 1 1 calc R . . C17 C 0.3434(6) 0.9255(5) 0.3139(3) 0.068(2) Uani 1 1 d . . . H17A H 0.3004 0.9663 0.3365 0.101 Uiso 1 1 calc R . . H17B H 0.4287 0.9291 0.3331 0.101 Uiso 1 1 calc R . . H17C H 0.3139 0.8727 0.3243 0.101 Uiso 1 1 calc R . . C18 C 0.3599(5) 1.0221(4) 0.2140(4) 0.0583(17) Uani 1 1 d . . . H18A H 0.3533 1.0269 0.1617 0.087 Uiso 1 1 calc R . . H18B H 0.4425 1.0319 0.2368 0.087 Uiso 1 1 calc R . . H18C H 0.3075 1.0612 0.2313 0.087 Uiso 1 1 calc R . . C19 C 0.0205(4) 0.8267(3) 0.0245(3) 0.0330(11) Uani 1 1 d . . . H19 H 0.0967 0.8115 0.0084 0.040 Uiso 1 1 calc R . . C20 C -0.0498(6) 0.7504(3) 0.0311(3) 0.0482(15) Uani 1 1 d . . . H20A H -0.0035 0.7153 0.0668 0.072 Uiso 1 1 calc R . . H20B H -0.0654 0.7234 -0.0156 0.072 Uiso 1 1 calc R . . H20C H -0.1256 0.7636 0.0463 0.072 Uiso 1 1 calc R . . C21 C -0.0491(5) 0.8801(3) -0.0333(3) 0.0458(14) Uani 1 1 d . . . H21A H -0.1288 0.8900 -0.0221 0.069 Uiso 1 1 calc R . . H21B H -0.0561 0.8538 -0.0801 0.069 Uiso 1 1 calc R . . H21C H -0.0070 0.9309 -0.0347 0.069 Uiso 1 1 calc R . . C22 C 0.5253(4) 0.7448(3) 0.2476(3) 0.0327(11) Uani 1 1 d . . . H22A H 0.4963 0.7752 0.2861 0.039 Uiso 1 1 calc R . . H22B H 0.5457 0.6911 0.2675 0.039 Uiso 1 1 calc R . . C23 C 0.3555(5) 0.5927(3) 0.1237(3) 0.0437(13) Uani 1 1 d . . . H23A H 0.4335 0.5813 0.1093 0.052 Uiso 1 1 calc R . . H23B H 0.3523 0.5608 0.1675 0.052 Uiso 1 1 calc R . . C24 C 0.7561(5) 0.7256(4) 0.1858(3) 0.0578(17) Uani 1 1 d . . . H24A H 0.7707 0.6741 0.2101 0.087 Uiso 1 1 calc R . . H24B H 0.8324 0.7512 0.1827 0.087 Uiso 1 1 calc R . . H24C H 0.7112 0.7175 0.1373 0.087 Uiso 1 1 calc R . . C25 C 0.6425(5) 0.8893(4) 0.1920(3) 0.0579(18) Uani 1 1 d . . . H25A H 0.5960 0.8817 0.1439 0.087 Uiso 1 1 calc R . . H25B H 0.7194 0.9136 0.1881 0.087 Uiso 1 1 calc R . . H25C H 0.5988 0.9243 0.2199 0.087 Uiso 1 1 calc R . . C26 C 0.7682(5) 0.8096(4) 0.3258(3) 0.0561(16) Uani 1 1 d . . . H26A H 0.7310 0.8486 0.3537 0.084 Uiso 1 1 calc R . . H26B H 0.8447 0.8304 0.3168 0.084 Uiso 1 1 calc R . . H26C H 0.7814 0.7597 0.3529 0.084 Uiso 1 1 calc R . . C27 C 0.2862(8) 0.4613(4) 0.0073(4) 0.088(3) Uani 1 1 d . . . H27A H 0.3527 0.4740 -0.0175 0.132 Uiso 1 1 calc R . . H27B H 0.2184 0.4423 -0.0276 0.132 Uiso 1 1 calc R . . H27C H 0.3107 0.4197 0.0432 0.132 Uiso 1 1 calc R . . C28 C 0.2016(6) 0.6277(3) -0.0204(3) 0.0527(16) Uani 1 1 d . . . H28A H 0.1684 0.6752 -0.0012 0.079 Uiso 1 1 calc R . . H28B H 0.1425 0.6047 -0.0587 0.079 Uiso 1 1 calc R . . H28C H 0.2732 0.6423 -0.0399 0.079 Uiso 1 1 calc R . . C29 C 0.1052(6) 0.5282(4) 0.0932(4) 0.0682(19) Uani 1 1 d . . . H29A H 0.1249 0.4868 0.1298 0.102 Uiso 1 1 calc R . . H29B H 0.0419 0.5091 0.0553 0.102 Uiso 1 1 calc R . . H29C H 0.0780 0.5761 0.1153 0.102 Uiso 1 1 calc R . . C30 C 0.2672(6) 0.6635(5) 0.3013(4) 0.083(3) Uani 1 1 d . . . H30A H 0.2745 0.6066 0.2890 0.100 Uiso 1 1 calc R . . H30B H 0.3457 0.6825 0.3261 0.100 Uiso 1 1 calc R . . C31 C 0.1783(6) 0.6735(5) 0.3470(3) 0.071(2) Uani 1 1 d . . . H31A H 0.1604 0.6220 0.3683 0.085 Uiso 1 1 calc R . . H31B H 0.2064 0.7115 0.3863 0.085 Uiso 1 1 calc R . . C32 C 0.0761(5) 0.7036(4) 0.3015(3) 0.0576(13) Uani 1 1 d . . . H32A H 0.0466 0.7510 0.3242 0.069 Uiso 1 1 calc R . . H32B H 0.0125 0.6628 0.2959 0.069 Uiso 1 1 calc R . . C33 C 0.1012(5) 0.7248(4) 0.2322(3) 0.0488(15) Uani 1 1 d . . . H33A H 0.0822 0.7816 0.2216 0.059 Uiso 1 1 calc R . . H33B H 0.0542 0.6917 0.1943 0.059 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 0.02398(11) 0.03054(12) 0.02600(11) 0.00672(9) 0.00869(8) 0.00412(9) N1 0.028(2) 0.025(2) 0.026(2) -0.0038(16) 0.0076(16) 0.0017(17) N2 0.022(2) 0.028(2) 0.027(2) 0.0016(16) 0.0098(16) 0.0022(16) O1 0.0254(19) 0.069(3) 0.034(2) 0.0216(18) 0.0121(15) 0.0085(17) Si1 0.0243(7) 0.0469(9) 0.0321(7) 0.0100(6) 0.0069(6) 0.0015(6) Si2 0.0626(11) 0.0295(8) 0.0466(10) -0.0020(7) 0.0145(8) 0.0000(7) C1 0.034(3) 0.035(3) 0.030(3) 0.003(2) 0.011(2) 0.010(2) C2 0.040(3) 0.043(3) 0.036(3) -0.005(2) 0.019(2) 0.009(2) C3 0.033(3) 0.040(3) 0.025(2) -0.001(2) 0.010(2) -0.002(2) C4 0.025(2) 0.029(2) 0.020(2) -0.0041(19) 0.0022(19) -0.0029(19) C5 0.028(3) 0.040(3) 0.027(3) 0.007(2) 0.004(2) -0.003(2) C6 0.027(3) 0.031(3) 0.038(3) 0.011(2) 0.005(2) 0.005(2) C7 0.028(3) 0.031(3) 0.031(3) 0.003(2) 0.009(2) 0.003(2) C8 0.022(2) 0.027(2) 0.021(2) -0.0014(19) 0.0037(18) -0.0027(19) C9 0.036(2) 0.094(4) 0.046(2) 0.031(2) 0.0179(19) 0.020(2) C10 0.022(2) 0.025(2) 0.028(2) 0.0041(19) 0.0113(19) 0.0036(19) C11 0.029(3) 0.032(3) 0.032(3) 0.001(2) 0.013(2) -0.001(2) C12 0.045(3) 0.042(3) 0.042(3) -0.016(3) 0.018(3) 0.000(3) C13 0.035(3) 0.049(3) 0.051(3) -0.014(3) 0.020(3) 0.009(3) C14 0.019(3) 0.039(3) 0.045(3) -0.006(2) 0.011(2) 0.002(2) C15 0.029(3) 0.027(2) 0.033(3) 0.003(2) 0.010(2) 0.005(2) C16 0.031(3) 0.047(3) 0.038(3) -0.013(2) 0.010(2) -0.003(2) C17 0.052(4) 0.102(6) 0.047(4) -0.006(4) 0.004(3) -0.005(4) C18 0.043(4) 0.052(4) 0.081(5) -0.006(3) 0.012(3) -0.011(3) C19 0.027(3) 0.035(3) 0.038(3) 0.002(2) 0.005(2) 0.008(2) C20 0.060(4) 0.044(3) 0.044(3) -0.007(3) 0.016(3) -0.016(3) C21 0.046(3) 0.055(4) 0.036(3) 0.003(3) 0.004(3) 0.011(3) C22 0.028(3) 0.043(3) 0.028(3) 0.007(2) 0.007(2) 0.003(2) C23 0.049(4) 0.035(3) 0.049(3) 0.011(3) 0.013(3) 0.006(3) C24 0.034(3) 0.089(5) 0.054(4) -0.003(4) 0.018(3) 0.006(3) C25 0.043(4) 0.063(4) 0.070(4) 0.035(3) 0.016(3) 0.000(3) C26 0.037(3) 0.088(5) 0.042(3) 0.003(3) 0.003(3) -0.013(3) C27 0.152(8) 0.035(4) 0.083(6) -0.009(4) 0.037(5) 0.010(4) C28 0.063(4) 0.049(4) 0.046(4) -0.004(3) 0.007(3) 0.006(3) C29 0.076(5) 0.065(4) 0.065(5) -0.002(4) 0.014(4) -0.016(4) C30 0.058(4) 0.128(7) 0.070(5) 0.068(5) 0.028(4) 0.033(4) C31 0.056(4) 0.113(6) 0.048(4) 0.032(4) 0.020(3) 0.021(4) C32 0.036(2) 0.094(4) 0.046(2) 0.031(2) 0.0179(19) 0.020(2) C33 0.028(3) 0.069(4) 0.050(3) 0.022(3) 0.009(2) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 N2 2.267(4) . ? Lu1 O1 2.286(3) . ? Lu1 C22 2.338(5) . ? Lu1 C23 2.346(5) . ? Lu1 N1 2.387(4) . ? N1 C1 1.329(6) . ? N1 C9 1.365(7) . ? N2 C8 1.368(5) . ? N2 C10 1.428(5) . ? O1 C33 1.454(6) . ? O1 C30 1.461(6) . ? Si1 C22 1.836(5) . ? Si1 C25 1.870(6) . ? Si1 C26 1.872(6) . ? Si1 C24 1.875(6) . ? Si2 C23 1.822(6) . ? Si2 C28 1.872(6) . ? Si2 C27 1.876(6) . ? Si2 C29 1.885(7) . ? C1 C2 1.390(7) . ? C2 C3 1.372(7) . ? C3 C4 1.411(6) . ? C4 C9 1.411(7) . ? C4 C5 1.415(6) . ? C5 C6 1.359(7) . ? C6 C7 1.396(6) . ? C7 C8 1.395(6) . ? C8 C9 1.436(7) . ? C10 C11 1.412(6) . ? C10 C15 1.412(6) . ? C11 C12 1.399(7) . ? C11 C16 1.519(7) . ? C12 C13 1.371(7) . ? C13 C14 1.372(7) . ? C14 C15 1.397(6) . ? C15 C19 1.521(7) . ? C16 C18 1.519(8) . ? C16 C17 1.528(8) . ? C19 C21 1.527(7) . ? C19 C20 1.527(7) . ? C30 C31 1.447(8) . ? C31 C32 1.418(8) . ? C32 C33 1.431(7) . ? 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 O1 93.98(12) . . ? N2 Lu1 C22 118.09(15) . . ? O1 Lu1 C22 94.94(15) . . ? N2 Lu1 C23 132.84(16) . . ? O1 Lu1 C23 94.56(17) . . ? C22 Lu1 C23 107.22(18) . . ? N2 Lu1 N1 70.22(13) . . ? O1 Lu1 N1 161.94(12) . . ? C22 Lu1 N1 100.20(15) . . ? C23 Lu1 N1 90.33(16) . . ? C1 N1 C9 118.5(4) . . ? C1 N1 Lu1 125.5(3) . . ? C9 N1 Lu1 115.7(3) . . ? C8 N2 C10 116.4(4) . . ? C8 N2 Lu1 118.9(3) . . ? C10 N2 Lu1 124.3(3) . . ? C33 O1 C30 107.3(4) . . ? C33 O1 Lu1 133.9(3) . . ? C30 O1 Lu1 118.0(3) . . ? C22 Si1 C25 110.3(2) . . ? C22 Si1 C26 113.7(3) . . ? C25 Si1 C26 106.6(3) . . ? C22 Si1 C24 111.5(3) . . ? C25 Si1 C24 109.1(3) . . ? C26 Si1 C24 105.3(3) . . ? C23 Si2 C28 110.4(3) . . ? C23 Si2 C27 115.1(3) . . ? C28 Si2 C27 105.0(3) . . ? C23 Si2 C29 108.7(3) . . ? C28 Si2 C29 109.4(3) . . ? C27 Si2 C29 108.1(3) . . ? N1 C1 C2 123.1(5) . . ? C3 C2 C1 119.1(5) . . ? C2 C3 C4 119.8(4) . . ? C3 C4 C9 117.3(5) . . ? C3 C4 C5 123.4(4) . . ? C9 C4 C5 119.3(5) . . ? C6 C5 C4 119.0(4) . . ? C5 C6 C7 122.2(4) . . ? C8 C7 C6 121.9(4) . . ? N2 C8 C7 126.2(4) . . ? N2 C8 C9 117.8(4) . . ? C7 C8 C9 116.0(4) . . ? N1 C9 C4 122.1(5) . . ? N1 C9 C8 116.3(5) . . ? C4 C9 C8 121.6(5) . . ? C11 C10 C15 120.3(4) . . ? C11 C10 N2 119.5(4) . . ? C15 C10 N2 120.2(4) . . ? C12 C11 C10 118.6(4) . . ? C12 C11 C16 119.7(4) . . ? C10 C11 C16 121.7(4) . . ? C13 C12 C11 121.0(5) . . ? C12 C13 C14 120.3(5) . . ? C13 C14 C15 121.6(5) . . ? C14 C15 C10 118.1(4) . . ? C14 C15 C19 119.3(4) . . ? C10 C15 C19 122.6(4) . . ? C11 C16 C18 110.0(5) . . ? C11 C16 C17 113.3(4) . . ? C18 C16 C17 111.6(5) . . ? C15 C19 C21 112.1(4) . . ? C15 C19 C20 111.9(4) . . ? C21 C19 C20 109.6(4) . . ? Si1 C22 Lu1 127.4(2) . . ? Si2 C23 Lu1 122.1(3) . . ? C31 C30 O1 107.0(5) . . ? C32 C31 C30 105.4(5) . . ? C31 C32 C33 111.9(5) . . ? C32 C33 O1 104.9(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.608 _refine_diff_density_min -2.473 _refine_diff_density_rms 0.110 #===========END============= data_complex3 _database_code_depnum_ccdc_archive 'CCDC 780670' #TrackingRef '- cif of complexes 1,2,3,5.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H49 Lu N2 O Si2' _chemical_formula_weight 696.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7731(5) _cell_length_b 17.2591(9) _cell_length_c 20.0423(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.2090(10) _cell_angle_gamma 90.00 _cell_volume 3380.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 3.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5266 _exptl_absorpt_correction_T_max 0.7880 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18709 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.03 _reflns_number_total 6643 _reflns_number_gt 5341 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+26.1468P] 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 6643 _refine_ls_number_parameters 306 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1865 _refine_ls_wR_factor_gt 0.1738 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.053 _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 C1 C 0.6606(15) 0.7094(7) 0.8952(7) 0.081(3) Uani 1 1 d . . . H1 H 0.7072 0.7152 0.9354 0.098 Uiso 1 1 calc R . . C2 C 0.5371(9) 0.6697(6) 0.8954(5) 0.051(2) Uani 1 1 d . . . H2 H 0.5016 0.6494 0.9347 0.062 Uiso 1 1 calc R . . C3 C 0.4687(9) 0.6613(6) 0.8356(5) 0.051(2) Uani 1 1 d . . . H3 H 0.3861 0.6346 0.8345 0.061 Uiso 1 1 calc R . . C4 C 0.5213(9) 0.6924(5) 0.7764(5) 0.046(2) Uani 1 1 d . . . C5 C 0.4548(10) 0.6857(6) 0.7134(5) 0.055(2) Uani 1 1 d . . . H5 H 0.3723 0.6592 0.7095 0.066 Uiso 1 1 calc R . . C6 C 0.5137(11) 0.7187(7) 0.6589(6) 0.062(3) Uani 1 1 d . . . H6 H 0.4704 0.7145 0.6176 0.074 Uiso 1 1 calc R . . C7 C 0.6380(10) 0.7589(6) 0.6634(5) 0.054(2) Uani 1 1 d . . . H7 H 0.6740 0.7812 0.6251 0.065 Uiso 1 1 calc R . . C8 C 0.7086(13) 0.7665(8) 0.7225(7) 0.080(2) Uani 1 1 d . . . C9 C 0.6479(13) 0.7326(8) 0.7810(7) 0.081(2) Uani 1 1 d . . . C10 C 0.8954(9) 0.8390(6) 0.6758(4) 0.049(2) Uani 1 1 d . . . C11 C 0.8555(16) 0.9133(7) 0.6566(6) 0.084(4) Uani 1 1 d . . . C12 C 0.9270(19) 0.9501(8) 0.6043(6) 0.099(5) Uani 1 1 d . . . H12 H 0.9025 0.9998 0.5910 0.119 Uiso 1 1 calc R . . C13 C 1.0336(13) 0.9122(8) 0.5730(6) 0.076(3) Uani 1 1 d U . . H13 H 1.0805 0.9366 0.5386 0.091 Uiso 1 1 calc R . . C14 C 1.0687(13) 0.8424(9) 0.5912(6) 0.079(3) Uani 1 1 d U . . H14 H 1.1413 0.8186 0.5694 0.095 Uiso 1 1 calc R . . C15 C 1.0014(12) 0.8012(7) 0.6427(6) 0.065(3) Uani 1 1 d U . . C16 C 0.7285(14) 0.9478(7) 0.6891(7) 0.081(3) Uani 1 1 d DU . . H16A H 0.6552 0.9118 0.6787 0.098 Uiso 1 1 calc R . . H16B H 0.7445 0.9432 0.7367 0.098 Uiso 1 1 calc R . . C17 C 0.6730(13) 1.0193(7) 0.6806(7) 0.081(2) Uani 1 1 d DU . . H17A H 0.7330 1.0576 0.6994 0.121 Uiso 1 1 calc R . . H17B H 0.5860 1.0216 0.7025 0.121 Uiso 1 1 calc R . . H17C H 0.6608 1.0293 0.6338 0.121 Uiso 1 1 calc R . . C18 C 1.0496(16) 0.7238(10) 0.6621(7) 0.099(5) Uani 1 1 d U . . H18A H 1.1459 0.7195 0.6512 0.118 Uiso 1 1 calc R . . H18B H 1.0412 0.7185 0.7101 0.118 Uiso 1 1 calc R . . C19 C 0.9812(13) 0.6643(8) 0.6323(7) 0.080(2) Uani 1 1 d U . . H19A H 0.8874 0.6647 0.6464 0.120 Uiso 1 1 calc R . . H19B H 1.0228 0.6160 0.6448 0.120 Uiso 1 1 calc R . . H19C H 0.9852 0.6702 0.5847 0.120 Uiso 1 1 calc R . . C20 C 1.0528(15) 0.6868(8) 0.8586(7) 0.084(3) Uani 1 1 d . . . H20A H 0.9965 0.6445 0.8422 0.100 Uiso 1 1 calc R . . H20B H 1.1351 0.6870 0.8316 0.100 Uiso 1 1 calc R . . C21 C 0.9547(14) 0.6523(9) 1.0027(8) 0.091(3) Uani 1 1 d . . . H21A H 0.9115 0.7020 1.0068 0.136 Uiso 1 1 calc R . . H21B H 0.9857 0.6353 1.0458 0.136 Uiso 1 1 calc R . . H21C H 0.8901 0.6156 0.9851 0.136 Uiso 1 1 calc R . . C22 C 1.2264(11) 0.7351(7) 0.9777(5) 0.066(3) Uani 1 1 d . . . H22A H 1.2888 0.7506 0.9433 0.099 Uiso 1 1 calc R . . H22B H 1.2769 0.7139 1.0146 0.099 Uiso 1 1 calc R . . H22C H 1.1751 0.7792 0.9924 0.099 Uiso 1 1 calc R . . C23 C 1.1946(12) 0.5633(7) 0.9495(7) 0.076(3) Uani 1 1 d . . . H23A H 1.1311 0.5230 0.9380 0.113 Uiso 1 1 calc R . . H23B H 1.2274 0.5553 0.9942 0.113 Uiso 1 1 calc R . . H23C H 1.2703 0.5623 0.9192 0.113 Uiso 1 1 calc R . . C24 C 0.8941(11) 0.8741(6) 0.9285(6) 0.067(3) Uani 1 1 d . . . H24A H 0.8732 0.8363 0.9628 0.081 Uiso 1 1 calc R . . H24B H 0.9825 0.8956 0.9405 0.081 Uiso 1 1 calc R . . C25 C 0.7577(14) 0.9816(8) 1.0302(7) 0.084(3) Uani 1 1 d U . . H25A H 0.7458 0.9364 1.0575 0.126 Uiso 1 1 calc R . . H25B H 0.6797 1.0149 1.0350 0.126 Uiso 1 1 calc R . . H25C H 0.8388 1.0087 1.0440 0.126 Uiso 1 1 calc R . . C26 C 0.6025(16) 0.9247(11) 0.9097(10) 0.115(5) Uani 1 1 d U . . H26A H 0.6072 0.9180 0.8622 0.172 Uiso 1 1 calc R . . H26B H 0.5378 0.9647 0.9200 0.172 Uiso 1 1 calc R . . H26C H 0.5739 0.8770 0.9300 0.172 Uiso 1 1 calc R . . C27 C 0.8419(15) 1.0423(8) 0.9007(7) 0.091(3) Uani 1 1 d U . . H27A H 0.9372 1.0483 0.9111 0.136 Uiso 1 1 calc R . . H27B H 0.7923 1.0867 0.9164 0.136 Uiso 1 1 calc R . . H27C H 0.8306 1.0377 0.8532 0.136 Uiso 1 1 calc R . . C28 C 1.1210(15) 0.9527(8) 0.7816(9) 0.094(4) Uani 1 1 d U . . H28A H 1.0973 0.9830 0.8207 0.113 Uiso 1 1 calc R . . H28B H 1.0557 0.9640 0.7464 0.113 Uiso 1 1 calc R . . C29 C 1.2613(16) 0.9711(10) 0.7597(9) 0.104(5) Uani 1 1 d U . . H29A H 1.2588 1.0017 0.7191 0.124 Uiso 1 1 calc R . . H29B H 1.3089 1.0005 0.7939 0.124 Uiso 1 1 calc R . . C30 C 1.3286(16) 0.9002(10) 0.7482(9) 0.106(5) Uani 1 1 d U . . H30A H 1.4229 0.9031 0.7633 0.127 Uiso 1 1 calc R . . H30B H 1.3279 0.8879 0.7010 0.127 Uiso 1 1 calc R . . C31 C 1.2542(14) 0.8413(9) 0.7858(9) 0.096(4) Uani 1 1 d U . . H31A H 1.2492 0.7934 0.7606 0.115 Uiso 1 1 calc R . . H31B H 1.3000 0.8309 0.8279 0.115 Uiso 1 1 calc R . . Lu1 Lu 0.93591(3) 0.80058(2) 0.833250(18) 0.04274(16) Uani 1 1 d . . . N1 N 0.7163(7) 0.7397(4) 0.8403(4) 0.0458(17) Uani 1 1 d . . . N2 N 0.8325(7) 0.8030(4) 0.7322(4) 0.0472(18) Uani 1 1 d . . . O1 O 1.1202(6) 0.8713(4) 0.7972(4) 0.0536(16) Uani 1 1 d . . . Si1 Si 1.1065(3) 0.66007(19) 0.94404(18) 0.0675(6) Uani 1 1 d . . . Si2 Si 0.7742(3) 0.95229(19) 0.94247(18) 0.0675(6) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.090(6) 0.083(5) 0.071(5) 0.016(4) 0.015(4) 0.017(4) C2 0.039(5) 0.062(6) 0.053(5) 0.017(5) 0.015(4) -0.003(4) C3 0.037(4) 0.053(5) 0.063(6) 0.013(4) 0.008(4) -0.005(4) C4 0.033(4) 0.049(5) 0.056(5) 0.006(4) 0.008(4) 0.007(4) C5 0.036(5) 0.066(6) 0.064(6) 0.003(5) 0.004(4) -0.009(4) C6 0.046(5) 0.080(7) 0.059(6) 0.011(5) -0.008(5) 0.000(5) C7 0.048(5) 0.070(6) 0.044(5) 0.009(5) 0.000(4) -0.007(5) C8 0.069(5) 0.088(5) 0.083(5) 0.010(5) 0.001(4) 0.005(4) C9 0.069(5) 0.086(5) 0.088(5) 0.018(5) 0.011(4) 0.009(4) C10 0.042(5) 0.064(6) 0.040(5) 0.001(4) 0.005(4) -0.011(4) C11 0.119(11) 0.073(8) 0.061(7) 0.021(6) 0.026(7) -0.003(7) C12 0.173(16) 0.070(8) 0.055(7) 0.004(6) 0.016(9) -0.048(9) C13 0.080(6) 0.093(7) 0.056(5) -0.002(5) 0.004(5) -0.043(6) C14 0.063(6) 0.112(8) 0.061(6) 0.001(6) 0.008(5) -0.010(6) C15 0.062(6) 0.081(6) 0.050(5) 0.003(5) 0.005(5) 0.002(5) C16 0.090(6) 0.083(5) 0.071(5) 0.016(4) 0.015(4) 0.017(4) C17 0.069(5) 0.086(5) 0.088(5) 0.018(5) 0.011(4) 0.009(4) C18 0.107(8) 0.105(8) 0.084(8) -0.008(6) 0.017(7) 0.016(7) C19 0.069(5) 0.088(5) 0.083(5) 0.010(5) 0.001(4) 0.005(4) C20 0.077(5) 0.085(5) 0.089(6) -0.021(4) 0.017(5) -0.005(4) C21 0.090(6) 0.087(5) 0.096(6) 0.008(5) 0.009(5) 0.005(5) C22 0.055(6) 0.090(8) 0.053(6) 0.004(6) 0.002(5) 0.000(6) C23 0.067(7) 0.070(7) 0.090(9) 0.033(6) 0.017(6) 0.019(6) C24 0.050(6) 0.063(6) 0.089(8) -0.013(6) 0.013(6) 0.002(5) C25 0.077(5) 0.085(5) 0.089(6) -0.021(4) 0.017(5) -0.005(4) C26 0.087(8) 0.119(9) 0.139(9) 0.001(8) 0.005(7) 0.031(7) C27 0.090(6) 0.087(5) 0.096(6) 0.008(5) 0.009(5) 0.005(5) C28 0.081(7) 0.078(7) 0.123(8) 0.007(6) 0.019(6) -0.006(6) C29 0.093(8) 0.095(8) 0.124(9) 0.014(7) 0.022(7) -0.013(7) C30 0.087(7) 0.107(8) 0.124(9) 0.004(7) 0.030(7) -0.009(7) C31 0.070(7) 0.093(7) 0.125(9) 0.016(7) 0.018(6) 0.003(6) Lu1 0.0330(2) 0.0505(2) 0.0447(2) 0.00256(16) 0.00543(15) 0.00110(15) N1 0.037(4) 0.057(4) 0.044(4) 0.013(3) 0.009(3) 0.003(3) N2 0.031(4) 0.065(5) 0.045(4) 0.011(3) 0.006(3) -0.007(3) O1 0.035(3) 0.057(4) 0.069(4) -0.002(3) 0.008(3) 0.000(3) Si1 0.0541(12) 0.0664(13) 0.0822(15) -0.0019(11) 0.0189(11) 0.0088(10) Si2 0.0541(12) 0.0664(13) 0.0822(15) -0.0019(11) 0.0189(11) 0.0088(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.336(14) . ? C1 C2 1.388(17) . ? C2 C3 1.379(14) . ? C3 C4 1.400(13) . ? C4 C9 1.421(16) . ? C4 C5 1.422(14) . ? C5 C6 1.363(15) . ? C6 C7 1.401(15) . ? C7 C8 1.375(16) . ? C8 N2 1.378(15) . ? C8 C9 1.440(18) . ? C9 N1 1.367(16) . ? C10 C15 1.394(15) . ? C10 C11 1.395(16) . ? C10 N2 1.431(11) . ? C11 C12 1.411(16) . ? C11 C16 1.524(18) . ? C12 C13 1.38(2) . ? C13 C14 1.304(19) . ? C14 C15 1.417(16) . ? C15 C18 1.47(2) . ? C16 C17 1.359(13) . ? C18 C19 1.36(2) . ? C20 Si1 1.848(16) . ? C20 Lu1 2.327(14) . ? C21 Si1 1.901(14) . ? C22 Si1 1.870(12) . ? C23 Si1 1.882(11) . ? C24 Si2 1.810(11) . ? C24 Lu1 2.329(11) . ? C25 Si2 1.838(13) . ? C26 Si2 1.862(17) . ? C27 Si2 1.886(14) . ? C28 O1 1.441(15) . ? C28 C29 1.475(18) . ? C29 C30 1.41(2) . ? C30 C31 1.46(2) . ? C31 O1 1.427(15) . ? Lu1 N2 2.260(8) . ? Lu1 O1 2.294(6) . ? Lu1 N1 2.394(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.6(13) . . ? C3 C2 C1 117.9(9) . . ? C2 C3 C4 121.2(9) . . ? C3 C4 C9 117.0(10) . . ? C3 C4 C5 123.5(9) . . ? C9 C4 C5 119.4(9) . . ? C6 C5 C4 119.0(9) . . ? C5 C6 C7 121.6(10) . . ? C8 C7 C6 122.4(10) . . ? C7 C8 N2 127.1(12) . . ? C7 C8 C9 117.1(12) . . ? N2 C8 C9 115.8(12) . . ? N1 C9 C4 121.5(11) . . ? N1 C9 C8 118.0(12) . . ? C4 C9 C8 120.5(12) . . ? C15 C10 C11 120.4(10) . . ? C15 C10 N2 119.7(9) . . ? C11 C10 N2 119.8(9) . . ? C10 C11 C12 118.7(13) . . ? C10 C11 C16 117.9(10) . . ? C12 C11 C16 123.2(13) . . ? C13 C12 C11 120.0(14) . . ? C14 C13 C12 120.5(12) . . ? C13 C14 C15 123.1(13) . . ? C10 C15 C14 117.3(11) . . ? C10 C15 C18 122.6(11) . . ? C14 C15 C18 120.0(12) . . ? C17 C16 C11 128.8(12) . . ? C19 C18 C15 114.4(13) . . ? Si1 C20 Lu1 123.4(6) . . ? Si2 C24 Lu1 130.5(7) . . ? O1 C28 C29 106.3(11) . . ? C30 C29 C28 107.3(14) . . ? C29 C30 C31 106.6(13) . . ? O1 C31 C30 106.8(12) . . ? N2 Lu1 O1 93.3(2) . . ? N2 Lu1 C20 115.4(4) . . ? O1 Lu1 C20 97.6(4) . . ? N2 Lu1 C24 130.1(4) . . ? O1 Lu1 C24 96.2(3) . . ? C20 Lu1 C24 111.6(5) . . ? N2 Lu1 N1 70.3(2) . . ? O1 Lu1 N1 163.1(2) . . ? C20 Lu1 N1 93.3(4) . . ? C24 Lu1 N1 91.8(3) . . ? C1 N1 C9 118.8(10) . . ? C1 N1 Lu1 126.0(8) . . ? C9 N1 Lu1 115.1(7) . . ? C8 N2 C10 117.8(9) . . ? C8 N2 Lu1 120.5(7) . . ? C10 N2 Lu1 121.6(6) . . ? C31 O1 C28 108.2(9) . . ? C31 O1 Lu1 125.4(7) . . ? C28 O1 Lu1 126.3(7) . . ? C20 Si1 C22 109.7(6) . . ? C20 Si1 C23 113.8(6) . . ? C22 Si1 C23 107.9(6) . . ? C20 Si1 C21 111.8(7) . . ? C22 Si1 C21 108.4(6) . . ? C23 Si1 C21 105.0(6) . . ? C24 Si2 C25 114.4(6) . . ? C24 Si2 C26 109.7(7) . . ? C25 Si2 C26 109.0(7) . . ? C24 Si2 C27 108.5(6) . . ? C25 Si2 C27 103.4(7) . . ? C26 Si2 C27 111.8(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.492 _refine_diff_density_min -3.373 _refine_diff_density_rms 0.168 #===========END============= data_complex5 _database_code_depnum_ccdc_archive 'CCDC 780671' #TrackingRef '- cif of complexes 1,2,3,5.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H65 N4 Nd O Si' _chemical_formula_weight 910.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0181(6) _cell_length_b 11.6008(7) _cell_length_c 18.1909(10) _cell_angle_alpha 89.2590(10) _cell_angle_beta 89.7830(10) _cell_angle_gamma 84.4310(10) _cell_volume 2314.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 950 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7972 _exptl_absorpt_correction_T_max 0.9007 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12109 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.04 _reflns_number_total 8032 _reflns_number_gt 6876 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.5073P] 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 8032 _refine_ls_number_parameters 525 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0854 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.308847(18) 0.274715(17) 0.271724(11) 0.03562(8) Uani 1 1 d . . . Si1 Si 0.40080(11) 0.23534(11) 0.47965(6) 0.0485(3) Uani 1 1 d . . . O1 O 0.4739(3) 0.4208(3) 0.27247(16) 0.0566(8) Uani 1 1 d . . . N1 N 0.3111(3) 0.3868(3) 0.14588(16) 0.0399(7) Uani 1 1 d . . . N2 N 0.3640(3) 0.1558(2) 0.16889(16) 0.0347(7) Uani 1 1 d . . . N3 N 0.1751(3) 0.1266(2) 0.32627(16) 0.0358(7) Uani 1 1 d . . . N4 N 0.0980(3) 0.3455(2) 0.28296(17) 0.0389(7) Uani 1 1 d . . . C1 C 0.2855(4) 0.4996(3) 0.1364(2) 0.0509(11) Uani 1 1 d . . . H1A H 0.2572 0.5433 0.1765 0.061 Uiso 1 1 calc R . . C2 C 0.2988(4) 0.5568(4) 0.0689(2) 0.0559(12) Uani 1 1 d . . . H2A H 0.2796 0.6364 0.0644 0.067 Uiso 1 1 calc R . . C3 C 0.3405(4) 0.4932(4) 0.0099(2) 0.0556(11) Uani 1 1 d . . . H3A H 0.3512 0.5299 -0.0351 0.067 Uiso 1 1 calc R . . C4 C 0.3674(4) 0.3728(3) 0.0164(2) 0.0443(9) Uani 1 1 d . . . C5 C 0.4110(4) 0.3013(4) -0.0420(2) 0.0569(12) Uani 1 1 d . . . H5 H 0.4238 0.3337 -0.0881 0.068 Uiso 1 1 calc R . . C6 C 0.4345(5) 0.1853(4) -0.0310(2) 0.0631(13) Uani 1 1 d . . . H6 H 0.4613 0.1387 -0.0702 0.076 Uiso 1 1 calc R . . C7 C 0.4190(4) 0.1345(4) 0.0383(2) 0.0534(11) Uani 1 1 d . . . H7 H 0.4362 0.0547 0.0437 0.064 Uiso 1 1 calc R . . C8 C 0.3788(3) 0.1985(3) 0.0993(2) 0.0394(9) Uani 1 1 d . . . C9 C 0.3526(3) 0.3211(3) 0.0872(2) 0.0377(8) Uani 1 1 d . . . C10 C 0.3804(3) 0.0324(3) 0.18033(19) 0.0353(8) Uani 1 1 d . . . C11 C 0.4876(3) -0.0193(3) 0.2143(2) 0.0396(9) Uani 1 1 d . . . C12 C 0.4956(4) -0.1366(4) 0.2320(2) 0.0482(10) Uani 1 1 d . . . H12 H 0.5661 -0.1707 0.2544 0.058 Uiso 1 1 calc R . . C13 C 0.4031(4) -0.2034(4) 0.2175(2) 0.0529(11) Uani 1 1 d . . . H13 H 0.4098 -0.2813 0.2312 0.064 Uiso 1 1 calc R . . C14 C 0.2999(4) -0.1541(3) 0.1824(2) 0.0475(10) Uani 1 1 d . . . H14 H 0.2380 -0.2001 0.1714 0.057 Uiso 1 1 calc R . . C15 C 0.2863(4) -0.0373(3) 0.1629(2) 0.0406(9) Uani 1 1 d . . . C16 C 0.5956(4) 0.0492(4) 0.2276(2) 0.0535(11) Uani 1 1 d . . . H16 H 0.5642 0.1287 0.2395 0.064 Uiso 1 1 calc R . . C17 C 0.6725(5) 0.0533(6) 0.1574(3) 0.102(2) Uani 1 1 d . . . H17A H 0.7073 -0.0235 0.1459 0.153 Uiso 1 1 calc R . . H17B H 0.7366 0.1023 0.1648 0.153 Uiso 1 1 calc R . . H17C H 0.6217 0.0836 0.1175 0.153 Uiso 1 1 calc R . . C18 C 0.6785(5) 0.0028(5) 0.2893(3) 0.0871(17) Uani 1 1 d . . . H18A H 0.6306 -0.0102 0.3323 0.131 Uiso 1 1 calc R . . H18B H 0.7353 0.0580 0.3001 0.131 Uiso 1 1 calc R . . H18C H 0.7224 -0.0688 0.2747 0.131 Uiso 1 1 calc R . . C19 C 0.1725(4) 0.0093(4) 0.1220(3) 0.0559(11) Uani 1 1 d . . . H19 H 0.1745 0.0931 0.1157 0.067 Uiso 1 1 calc R . . C20 C 0.1689(5) -0.0444(6) 0.0444(3) 0.0941(19) Uani 1 1 d . . . H20A H 0.2447 -0.0366 0.0195 0.141 Uiso 1 1 calc R . . H20B H 0.1032 -0.0047 0.0167 0.141 Uiso 1 1 calc R . . H20C H 0.1565 -0.1249 0.0491 0.141 Uiso 1 1 calc R . . C21 C 0.0566(4) -0.0116(5) 0.1644(3) 0.0747(15) Uani 1 1 d . . . H21A H 0.0555 -0.0930 0.1742 0.112 Uiso 1 1 calc R . . H21B H -0.0134 0.0158 0.1356 0.112 Uiso 1 1 calc R . . H21C H 0.0549 0.0293 0.2100 0.112 Uiso 1 1 calc R . . C22 C 0.2133(4) 0.0185(3) 0.3444(2) 0.0418(9) Uani 1 1 d . . . H22 H 0.2910 -0.0108 0.3297 0.050 Uiso 1 1 calc R . . C23 C 0.1424(4) -0.0541(3) 0.3848(2) 0.0471(10) Uani 1 1 d . . . H23 H 0.1724 -0.1299 0.3961 0.056 Uiso 1 1 calc R . . C24 C 0.0290(4) -0.0118(3) 0.4070(2) 0.0459(10) Uani 1 1 d . . . H24 H -0.0193 -0.0592 0.4334 0.055 Uiso 1 1 calc R . . C25 C -0.0156(3) 0.1030(3) 0.3904(2) 0.0394(9) Uani 1 1 d . . . C26 C -0.1317(4) 0.1532(4) 0.4133(2) 0.0489(10) Uani 1 1 d . . . H26 H -0.1824 0.1104 0.4415 0.059 Uiso 1 1 calc R . . C27 C -0.1679(4) 0.2642(4) 0.3937(2) 0.0528(11) Uani 1 1 d . . . H27 H -0.2435 0.2975 0.4096 0.063 Uiso 1 1 calc R . . C28 C -0.0947(4) 0.3304(4) 0.3500(2) 0.0476(10) Uani 1 1 d . . . H28 H -0.1242 0.4056 0.3367 0.057 Uiso 1 1 calc R . . C29 C 0.0207(3) 0.2869(3) 0.3260(2) 0.0385(9) Uani 1 1 d . . . C30 C 0.0608(3) 0.1705(3) 0.34805(19) 0.0355(8) Uani 1 1 d . . . C31 C 0.0430(4) 0.4491(3) 0.2477(2) 0.0440(10) Uani 1 1 d . . . C32 C 0.0357(4) 0.5564(4) 0.2832(3) 0.0531(11) Uani 1 1 d . . . C33 C -0.0136(5) 0.6558(4) 0.2461(3) 0.0682(14) Uani 1 1 d . . . H33 H -0.0170 0.7268 0.2695 0.082 Uiso 1 1 calc R . . C34 C -0.0567(5) 0.6513(4) 0.1763(3) 0.0729(15) Uani 1 1 d . . . H34 H -0.0902 0.7184 0.1526 0.088 Uiso 1 1 calc R . . C35 C -0.0504(4) 0.5467(4) 0.1410(3) 0.0610(12) Uani 1 1 d . . . H35 H -0.0800 0.5441 0.0933 0.073 Uiso 1 1 calc R . . C36 C -0.0003(4) 0.4436(3) 0.1752(2) 0.0481(10) Uani 1 1 d . . . C37 C 0.0837(4) 0.5658(4) 0.3601(3) 0.0629(13) Uani 1 1 d . . . H37 H 0.0977 0.4872 0.3806 0.075 Uiso 1 1 calc R . . C38 C 0.2047(5) 0.6154(5) 0.3570(3) 0.0844(17) Uani 1 1 d . . . H38A H 0.2608 0.5664 0.3279 0.127 Uiso 1 1 calc R . . H38B H 0.2362 0.6200 0.4059 0.127 Uiso 1 1 calc R . . H38C H 0.1944 0.6915 0.3352 0.127 Uiso 1 1 calc R . . C39 C -0.0038(5) 0.6371(5) 0.4127(3) 0.0887(17) Uani 1 1 d . . . H39A H -0.0194 0.7148 0.3940 0.133 Uiso 1 1 calc R . . H39B H 0.0327 0.6385 0.4605 0.133 Uiso 1 1 calc R . . H39C H -0.0792 0.6022 0.4164 0.133 Uiso 1 1 calc R . . C40 C 0.0034(4) 0.3315(4) 0.1346(2) 0.0545(11) Uani 1 1 d . . . H40 H 0.0675 0.2780 0.1570 0.065 Uiso 1 1 calc R . . C41 C 0.0321(5) 0.3395(5) 0.0516(2) 0.0679(14) Uani 1 1 d . . . H41A H -0.0352 0.3820 0.0268 0.102 Uiso 1 1 calc R . . H41B H 0.0449 0.2629 0.0319 0.102 Uiso 1 1 calc R . . H41C H 0.1043 0.3784 0.0445 0.102 Uiso 1 1 calc R . . C42 C -0.1161(5) 0.2768(5) 0.1425(3) 0.0800(16) Uani 1 1 d . . . H42A H -0.1317 0.2621 0.1936 0.120 Uiso 1 1 calc R . . H42B H -0.1106 0.2051 0.1163 0.120 Uiso 1 1 calc R . . H42C H -0.1814 0.3285 0.1226 0.120 Uiso 1 1 calc R . . C43 C 0.4349(4) 0.2060(4) 0.3825(2) 0.0489(10) Uani 1 1 d . . . H43A H 0.4460 0.1223 0.3790 0.059 Uiso 1 1 calc R . . H43B H 0.5146 0.2325 0.3740 0.059 Uiso 1 1 calc R . . C44 C 0.2767(5) 0.1507(5) 0.5144(2) 0.0689(14) Uani 1 1 d . . . H44A H 0.2032 0.1731 0.4876 0.103 Uiso 1 1 calc R . . H44B H 0.2632 0.1658 0.5657 0.103 Uiso 1 1 calc R . . H44C H 0.2999 0.0695 0.5079 0.103 Uiso 1 1 calc R . . C45 C 0.5338(5) 0.2037(6) 0.5432(3) 0.0849(18) Uani 1 1 d . . . H45A H 0.5610 0.1226 0.5420 0.127 Uiso 1 1 calc R . . H45B H 0.5095 0.2246 0.5924 0.127 Uiso 1 1 calc R . . H45C H 0.5990 0.2478 0.5278 0.127 Uiso 1 1 calc R . . C46 C 0.3444(5) 0.3918(4) 0.4944(3) 0.0809(16) Uani 1 1 d . . . H46A H 0.4077 0.4398 0.4818 0.121 Uiso 1 1 calc R . . H46B H 0.3221 0.4029 0.5451 0.121 Uiso 1 1 calc R . . H46C H 0.2745 0.4125 0.4639 0.121 Uiso 1 1 calc R . . C47 C 0.5221(4) 0.4846(4) 0.3313(3) 0.0663(13) Uani 1 1 d . . . H47A H 0.5509 0.4324 0.3709 0.080 Uiso 1 1 calc R . . H47B H 0.4594 0.5408 0.3505 0.080 Uiso 1 1 calc R . . C48 C 0.6245(4) 0.5443(4) 0.3004(3) 0.0681(14) Uani 1 1 d . . . H48A H 0.6016 0.6268 0.2952 0.082 Uiso 1 1 calc R . . H48B H 0.6958 0.5320 0.3317 0.082 Uiso 1 1 calc R . . C49 C 0.6483(5) 0.4913(6) 0.2285(3) 0.096(2) Uani 1 1 d . . . H49A H 0.6311 0.5486 0.1897 0.115 Uiso 1 1 calc R . . H49B H 0.7332 0.4608 0.2248 0.115 Uiso 1 1 calc R . . C50 C 0.5726(5) 0.4015(5) 0.2214(4) 0.104(2) Uani 1 1 d . . . H50A H 0.6184 0.3274 0.2316 0.125 Uiso 1 1 calc R . . H50B H 0.5413 0.4006 0.1717 0.125 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.03726(13) 0.03987(12) 0.03106(12) -0.00296(8) 0.00571(8) -0.01039(8) Si1 0.0520(7) 0.0609(7) 0.0346(6) -0.0025(5) -0.0020(5) -0.0156(6) O1 0.0477(18) 0.069(2) 0.0565(19) -0.0124(15) 0.0094(14) -0.0236(15) N1 0.052(2) 0.0335(17) 0.0361(17) -0.0027(13) 0.0099(15) -0.0127(14) N2 0.0401(18) 0.0338(16) 0.0308(16) 0.0007(13) 0.0026(13) -0.0068(13) N3 0.0409(19) 0.0335(16) 0.0334(17) 0.0002(13) 0.0024(14) -0.0051(14) N4 0.0431(19) 0.0338(16) 0.0402(18) 0.0060(14) 0.0099(14) -0.0063(14) C1 0.066(3) 0.041(2) 0.047(2) -0.0018(19) 0.016(2) -0.011(2) C2 0.071(3) 0.034(2) 0.063(3) 0.005(2) 0.016(2) -0.008(2) C3 0.068(3) 0.050(3) 0.049(3) 0.011(2) 0.013(2) -0.012(2) C4 0.049(2) 0.045(2) 0.039(2) 0.0060(18) 0.0045(18) -0.0074(18) C5 0.087(3) 0.049(3) 0.035(2) 0.0045(19) 0.014(2) -0.007(2) C6 0.092(4) 0.057(3) 0.039(2) -0.003(2) 0.022(2) 0.000(3) C7 0.078(3) 0.045(2) 0.036(2) -0.0015(18) 0.009(2) -0.001(2) C8 0.042(2) 0.040(2) 0.037(2) -0.0027(17) 0.0025(17) -0.0058(17) C9 0.040(2) 0.037(2) 0.037(2) 0.0010(16) 0.0027(17) -0.0078(16) C10 0.045(2) 0.0334(19) 0.0280(19) -0.0010(15) 0.0034(16) -0.0038(17) C11 0.037(2) 0.049(2) 0.033(2) -0.0038(17) 0.0039(16) -0.0045(18) C12 0.047(3) 0.049(2) 0.046(2) 0.0113(19) -0.0017(19) 0.006(2) C13 0.062(3) 0.038(2) 0.057(3) 0.010(2) 0.006(2) -0.001(2) C14 0.047(2) 0.039(2) 0.058(3) -0.0015(19) 0.003(2) -0.0083(18) C15 0.043(2) 0.038(2) 0.041(2) -0.0053(17) 0.0022(17) -0.0018(17) C16 0.045(3) 0.060(3) 0.055(3) -0.007(2) -0.002(2) -0.009(2) C17 0.075(4) 0.154(6) 0.085(4) -0.008(4) 0.013(3) -0.056(4) C18 0.068(4) 0.109(5) 0.085(4) -0.014(3) -0.029(3) -0.007(3) C19 0.047(3) 0.046(2) 0.075(3) -0.001(2) -0.015(2) -0.006(2) C20 0.079(4) 0.142(6) 0.061(4) -0.007(3) -0.026(3) -0.009(4) C21 0.051(3) 0.076(3) 0.097(4) -0.012(3) -0.011(3) -0.003(3) C22 0.046(2) 0.038(2) 0.041(2) -0.0013(17) 0.0037(18) -0.0046(18) C23 0.065(3) 0.031(2) 0.045(2) 0.0042(17) -0.002(2) -0.0065(19) C24 0.058(3) 0.042(2) 0.041(2) 0.0030(18) 0.000(2) -0.017(2) C25 0.044(2) 0.044(2) 0.031(2) 0.0034(16) -0.0015(17) -0.0139(18) C26 0.042(2) 0.062(3) 0.045(2) 0.013(2) 0.0060(19) -0.019(2) C27 0.039(2) 0.064(3) 0.055(3) 0.012(2) 0.011(2) -0.004(2) C28 0.042(2) 0.049(2) 0.050(2) 0.0114(19) 0.0081(19) 0.0008(19) C29 0.041(2) 0.039(2) 0.036(2) 0.0016(16) 0.0041(17) -0.0053(17) C30 0.038(2) 0.039(2) 0.0310(19) 0.0007(16) -0.0026(16) -0.0109(16) C31 0.043(2) 0.038(2) 0.050(3) 0.0068(18) 0.0164(19) -0.0038(17) C32 0.055(3) 0.041(2) 0.064(3) 0.004(2) 0.008(2) -0.006(2) C33 0.076(4) 0.040(2) 0.088(4) 0.008(2) 0.015(3) -0.003(2) C34 0.081(4) 0.051(3) 0.085(4) 0.025(3) 0.006(3) -0.001(3) C35 0.059(3) 0.057(3) 0.066(3) 0.022(2) 0.009(2) -0.004(2) C36 0.043(2) 0.046(2) 0.054(3) 0.013(2) 0.013(2) -0.0021(18) C37 0.071(3) 0.037(2) 0.081(4) -0.007(2) 0.003(3) -0.006(2) C38 0.077(4) 0.070(4) 0.105(5) -0.014(3) -0.003(3) 0.001(3) C39 0.083(4) 0.084(4) 0.100(5) -0.019(3) 0.014(3) -0.008(3) C40 0.065(3) 0.050(3) 0.047(3) 0.008(2) 0.002(2) 0.001(2) C41 0.067(3) 0.086(4) 0.051(3) 0.012(3) 0.000(2) -0.005(3) C42 0.113(5) 0.066(3) 0.065(3) -0.003(3) 0.017(3) -0.030(3) C43 0.048(3) 0.060(3) 0.041(2) -0.0024(19) 0.0021(19) -0.015(2) C44 0.084(4) 0.085(4) 0.042(3) -0.004(2) 0.012(2) -0.030(3) C45 0.065(3) 0.139(5) 0.049(3) -0.012(3) -0.010(3) -0.004(3) C46 0.117(5) 0.068(3) 0.060(3) -0.005(3) 0.019(3) -0.018(3) C47 0.066(3) 0.076(3) 0.062(3) -0.014(3) 0.000(2) -0.027(3) C48 0.060(3) 0.048(3) 0.097(4) 0.002(3) -0.014(3) -0.012(2) C49 0.080(4) 0.154(6) 0.063(4) 0.010(4) 0.008(3) -0.055(4) C50 0.077(4) 0.108(5) 0.137(6) -0.068(4) 0.062(4) -0.057(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N2 2.381(3) . ? Nd1 N4 2.397(3) . ? Nd1 C43 2.528(4) . ? Nd1 N3 2.559(3) . ? Nd1 O1 2.603(3) . ? Nd1 N1 2.619(3) . ? Si1 C43 1.834(4) . ? Si1 C44 1.863(5) . ? Si1 C45 1.875(5) . ? Si1 C46 1.883(5) . ? O1 C50 1.430(5) . ? O1 C47 1.441(5) . ? N1 C1 1.321(5) . ? N1 C9 1.372(5) . ? N2 C8 1.369(4) . ? N2 C10 1.437(4) . ? N3 C22 1.321(4) . ? N3 C30 1.371(5) . ? N4 C29 1.376(4) . ? N4 C31 1.436(5) . ? C1 C2 1.403(6) . ? C1 H1A 0.9300 . ? C2 C3 1.363(6) . ? C2 H2A 0.9300 . ? C3 C4 1.403(6) . ? C3 H3A 0.9300 . ? C4 C5 1.409(6) . ? C4 C9 1.429(5) . ? C5 C6 1.359(6) . ? C5 H5 0.9300 . ? C6 C7 1.401(6) . ? C6 H6 0.9300 . ? C7 C8 1.390(5) . ? C7 H7 0.9300 . ? C8 C9 1.438(5) . ? C10 C11 1.412(5) . ? C10 C15 1.415(5) . ? C11 C12 1.389(5) . ? C11 C16 1.515(6) . ? C12 C13 1.368(6) . ? C12 H12 0.9300 . ? C13 C14 1.378(6) . ? C13 H13 0.9300 . ? C14 C15 1.390(5) . ? C14 H14 0.9300 . ? C15 C19 1.511(6) . ? C16 C18 1.510(6) . ? C16 C17 1.533(7) . ? C16 H16 0.9800 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C21 1.527(7) . ? C19 C20 1.551(7) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.402(5) . ? C22 H22 0.9300 . ? C23 C24 1.359(6) . ? C23 H23 0.9300 . ? C24 C25 1.403(5) . ? C24 H24 0.9300 . ? C25 C26 1.417(5) . ? C25 C30 1.422(5) . ? C26 C27 1.355(6) . ? C26 H26 0.9300 . ? C27 C28 1.404(5) . ? C27 H27 0.9300 . ? C28 C29 1.392(5) . ? C28 H28 0.9300 . ? C29 C30 1.433(5) . ? C31 C32 1.406(6) . ? C31 C36 1.409(6) . ? C32 C33 1.393(6) . ? C32 C37 1.506(7) . ? C33 C34 1.361(7) . ? C33 H33 0.9300 . ? C34 C35 1.376(7) . ? C34 H34 0.9300 . ? C35 C36 1.406(6) . ? C35 H35 0.9300 . ? C36 C40 1.501(6) . ? C37 C38 1.503(7) . ? C37 C39 1.545(7) . ? C37 H37 0.9800 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C42 1.522(7) . ? C40 C41 1.545(6) . ? C40 H40 0.9800 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? 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 C48 1.484(6) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.464(7) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.403(7) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Nd1 N4 116.81(11) . . ? N2 Nd1 C43 110.25(12) . . ? N4 Nd1 C43 121.61(12) . . ? N2 Nd1 N3 92.32(9) . . ? N4 Nd1 N3 66.13(9) . . ? C43 Nd1 N3 79.82(12) . . ? N2 Nd1 O1 103.60(9) . . ? N4 Nd1 O1 119.38(10) . . ? C43 Nd1 O1 78.18(12) . . ? N3 Nd1 O1 156.24(10) . . ? N2 Nd1 N1 65.56(9) . . ? N4 Nd1 N1 87.70(10) . . ? C43 Nd1 N1 144.60(12) . . ? N3 Nd1 N1 133.95(10) . . ? O1 Nd1 N1 69.53(10) . . ? C43 Si1 C44 111.6(2) . . ? C43 Si1 C45 114.7(2) . . ? C44 Si1 C45 107.0(3) . . ? C43 Si1 C46 111.7(2) . . ? C44 Si1 C46 105.5(2) . . ? C45 Si1 C46 105.8(3) . . ? C50 O1 C47 104.7(4) . . ? C50 O1 Nd1 117.2(3) . . ? C47 O1 Nd1 131.5(2) . . ? C1 N1 C9 119.0(3) . . ? C1 N1 Nd1 125.7(3) . . ? C9 N1 Nd1 115.1(2) . . ? C8 N2 C10 118.3(3) . . ? C8 N2 Nd1 123.5(2) . . ? C10 N2 Nd1 118.2(2) . . ? C22 N3 C30 118.7(3) . . ? C22 N3 Nd1 125.2(2) . . ? C30 N3 Nd1 115.4(2) . . ? C29 N4 C31 115.2(3) . . ? C29 N4 Nd1 120.3(2) . . ? C31 N4 Nd1 124.4(2) . . ? N1 C1 C2 123.3(4) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C3 C2 C1 118.6(4) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 120.6(4) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C3 C4 C5 123.9(4) . . ? C3 C4 C9 117.4(4) . . ? C5 C4 C9 118.7(4) . . ? C6 C5 C4 120.1(4) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 121.2(4) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 122.6(4) . . ? C8 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? N2 C8 C7 126.1(3) . . ? N2 C8 C9 117.9(3) . . ? C7 C8 C9 116.0(3) . . ? N1 C9 C4 121.0(3) . . ? N1 C9 C8 117.6(3) . . ? C4 C9 C8 121.4(3) . . ? C11 C10 C15 119.2(3) . . ? C11 C10 N2 120.0(3) . . ? C15 C10 N2 120.6(3) . . ? C12 C11 C10 118.9(4) . . ? C12 C11 C16 119.8(4) . . ? C10 C11 C16 121.2(3) . . ? C13 C12 C11 122.1(4) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C13 C14 119.3(4) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 121.6(4) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C10 119.0(4) . . ? C14 C15 C19 118.4(4) . . ? C10 C15 C19 122.6(3) . . ? C18 C16 C11 114.7(4) . . ? C18 C16 C17 108.0(4) . . ? C11 C16 C17 109.9(4) . . ? C18 C16 H16 108.0 . . ? C11 C16 H16 108.0 . . ? C17 C16 H16 108.0 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 C21 112.0(4) . . ? C15 C19 C20 111.0(4) . . ? C21 C19 C20 109.8(4) . . ? C15 C19 H19 107.9 . . ? C21 C19 H19 107.9 . . ? C20 C19 H19 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 C23 123.2(4) . . ? N3 C22 H22 118.4 . . ? C23 C22 H22 118.4 . . ? C24 C23 C22 118.8(4) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 120.5(4) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 123.3(3) . . ? C24 C25 C30 117.3(4) . . ? C26 C25 C30 119.4(3) . . ? C27 C26 C25 119.1(4) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 121.9(4) . . ? C26 C27 H27 119.0 . . ? C28 C27 H27 119.0 . . ? C29 C28 C27 122.0(4) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? N4 C29 C28 125.8(3) . . ? N4 C29 C30 117.9(3) . . ? C28 C29 C30 116.3(3) . . ? N3 C30 C25 121.4(3) . . ? N3 C30 C29 117.4(3) . . ? C25 C30 C29 121.2(3) . . ? C32 C31 C36 119.4(4) . . ? C32 C31 N4 121.2(4) . . ? C36 C31 N4 119.3(3) . . ? C33 C32 C31 119.6(5) . . ? C33 C32 C37 119.6(4) . . ? C31 C32 C37 120.8(4) . . ? C34 C33 C32 121.5(5) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C33 C34 C35 119.5(5) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C36 121.6(5) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C35 C36 C31 118.4(4) . . ? C35 C36 C40 119.6(4) . . ? C31 C36 C40 122.0(4) . . ? C38 C37 C32 109.3(4) . . ? C38 C37 C39 110.2(4) . . ? C32 C37 C39 114.5(4) . . ? C38 C37 H37 107.5 . . ? C32 C37 H37 107.5 . . ? C39 C37 H37 107.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 C42 111.5(4) . . ? C36 C40 C41 115.3(4) . . ? C42 C40 C41 107.4(4) . . ? C36 C40 H40 107.4 . . ? C42 C40 H40 107.4 . . ? C41 C40 H40 107.4 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si1 C43 Nd1 127.8(2) . . ? Si1 C43 H43A 105.4 . . ? Nd1 C43 H43A 105.4 . . ? Si1 C43 H43B 105.4 . . ? Nd1 C43 H43B 105.4 . . ? H43A C43 H43B 106.0 . . ? Si1 C44 H44A 109.5 . . ? Si1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si1 C45 H45A 109.5 . . ? Si1 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si1 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si1 C46 H46A 109.5 . . ? Si1 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si1 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O1 C47 C48 107.3(4) . . ? O1 C47 H47A 110.3 . . ? C48 C47 H47A 110.3 . . ? O1 C47 H47B 110.3 . . ? C48 C47 H47B 110.3 . . ? H47A C47 H47B 108.5 . . ? C49 C48 C47 104.4(4) . . ? C49 C48 H48A 110.9 . . ? C47 C48 H48A 110.9 . . ? C49 C48 H48B 110.9 . . ? C47 C48 H48B 110.9 . . ? H48A C48 H48B 108.9 . . ? C50 C49 C48 108.1(5) . . ? C50 C49 H49A 110.1 . . ? C48 C49 H49A 110.1 . . ? C50 C49 H49B 110.1 . . ? C48 C49 H49B 110.1 . . ? H49A C49 H49B 108.4 . . ? C49 C50 O1 108.3(5) . . ? C49 C50 H50A 110.0 . . ? O1 C50 H50A 110.0 . . ? C49 C50 H50B 110.0 . . ? O1 C50 H50B 110.0 . . ? H50A C50 H50B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.959 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.077