# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_3Sc _database_code_depnum_ccdc_archive 'CCDC 767211' #TrackingRef '- DT-ART-02-2010-00006.cif' _database_code_depnum_ccdc_archive 'CCDC 767211' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H75 N6 Sc3 Si3' _chemical_formula_weight 811.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.587(2) _cell_length_b 13.134(2) _cell_length_c 14.841(3) _cell_angle_alpha 94.484(3) _cell_angle_beta 103.470(3) _cell_angle_gamma 104.442(3) _cell_volume 2286.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 15170 _cell_measurement_theta_min 1.43 _cell_measurement_theta_max 27.52 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8545 _exptl_absorpt_correction_T_max 0.9479 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 15170 _diffrn_reflns_av_R_equivalents 0.0953 _diffrn_reflns_av_sigmaI/netI 0.1553 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 27.52 _reflns_number_total 9934 _reflns_number_gt 5660 _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 'ORTEP-III (Farrugia, 1997)' _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^)+(0.1139P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9934 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1395 _refine_ls_R_factor_gt 0.0921 _refine_ls_wR_factor_ref 0.2347 _refine_ls_wR_factor_gt 0.2103 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.078 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.78617(8) 0.64052(8) 0.31055(6) 0.0206(2) Uani 1 1 d . . . Sc2 Sc 0.59571(8) 0.76488(8) 0.22889(6) 0.0201(2) Uani 1 1 d . . . Sc3 Sc 0.85230(8) 0.84419(8) 0.20046(7) 0.0217(2) Uani 1 1 d . . . Si1 Si 0.61927(13) 0.35836(12) 0.34278(10) 0.0280(4) Uani 1 1 d . . . Si2 Si 0.29858(12) 0.56717(13) 0.11900(11) 0.0309(4) Uani 1 1 d . . . Si3 Si 1.15841(15) 1.01433(16) 0.32549(13) 0.0475(5) Uani 1 1 d . . . N1 N 0.6162(3) 0.6013(3) 0.2098(3) 0.0224(9) Uani 1 1 d . . . H1A H 0.5622 0.5518 0.2278 0.027 Uiso 1 1 calc R . . H1B H 0.6175 0.5797 0.1497 0.027 Uiso 1 1 calc R . . N2 N 0.6790(4) 0.7271(3) 0.3683(3) 0.0255(10) Uani 1 1 d . . . H2A H 0.7214 0.7869 0.4101 0.031 Uiso 1 1 calc R . . H2B H 0.6283 0.6843 0.3945 0.031 Uiso 1 1 calc R . . N3 N 0.7411(3) 0.9111(3) 0.2696(3) 0.0256(10) Uani 1 1 d . . . H3A H 0.7236 0.9685 0.2442 0.031 Uiso 1 1 calc R . . H3B H 0.7703 0.9282 0.3334 0.031 Uiso 1 1 calc R . . N4 N 0.6743(3) 0.7837(3) 0.1099(3) 0.0242(9) Uani 1 1 d . . . H4A H 0.6523 0.8328 0.0741 0.029 Uiso 1 1 calc R . . H4B H 0.6619 0.7204 0.0726 0.029 Uiso 1 1 calc R . . N5 N 0.8459(4) 0.6723(3) 0.1826(3) 0.0253(10) Uani 1 1 d . . . H5A H 0.9160 0.6613 0.1861 0.030 Uiso 1 1 calc R . . H5B H 0.7942 0.6348 0.1284 0.030 Uiso 1 1 calc R . . N6 N 0.9091(3) 0.8004(3) 0.3410(3) 0.0260(10) Uani 1 1 d . . . H6A H 0.8983 0.8440 0.3876 0.031 Uiso 1 1 calc R . . H6B H 0.9835 0.7978 0.3548 0.031 Uiso 1 1 calc R . . C1 C 0.7561(4) 0.4653(4) 0.3642(3) 0.0243(11) Uani 1 1 d . . . C2 C 0.8080(4) 0.5428(4) 0.4488(3) 0.0251(11) Uani 1 1 d . . . C3 C 0.9195(4) 0.5917(4) 0.4468(4) 0.0287(12) Uani 1 1 d . . . C4 C 0.9388(4) 0.5483(4) 0.3639(4) 0.0297(12) Uani 1 1 d . . . C5 C 0.8397(5) 0.4698(4) 0.3138(4) 0.0290(12) Uani 1 1 d . . . C6 C 0.7560(5) 0.5633(5) 0.5277(4) 0.0357(14) Uani 1 1 d . . . H6C H 0.8094 0.6219 0.5741 0.054 Uiso 1 1 calc R . . H6D H 0.7395 0.4992 0.5573 0.054 Uiso 1 1 calc R . . H6E H 0.6854 0.5823 0.5030 0.054 Uiso 1 1 calc R . . C7 C 1.0082(5) 0.6733(5) 0.5233(4) 0.0414(16) Uani 1 1 d . . . H7A H 0.9728 0.6941 0.5714 0.062 Uiso 1 1 calc R . . H7B H 1.0400 0.7360 0.4963 0.062 Uiso 1 1 calc R . . H7C H 1.0691 0.6424 0.5517 0.062 Uiso 1 1 calc R . . C8 C 1.0509(5) 0.5774(5) 0.3375(5) 0.0484(18) Uani 1 1 d . . . H8A H 1.1046 0.5455 0.3762 0.073 Uiso 1 1 calc R . . H8B H 1.0820 0.6549 0.3481 0.073 Uiso 1 1 calc R . . H8C H 1.0384 0.5507 0.2713 0.073 Uiso 1 1 calc R . . C9 C 0.8278(6) 0.4012(5) 0.2239(4) 0.0424(15) Uani 1 1 d . . . H9A H 0.8894 0.4329 0.1960 0.064 Uiso 1 1 calc R . . H9B H 0.7544 0.3961 0.1803 0.064 Uiso 1 1 calc R . . H9C H 0.8318 0.3301 0.2369 0.064 Uiso 1 1 calc R . . C10 C 0.6513(5) 0.2422(5) 0.3973(4) 0.0408(15) Uani 1 1 d . . . H10A H 0.6908 0.2074 0.3603 0.061 Uiso 1 1 calc R . . H10B H 0.5801 0.1916 0.3989 0.061 Uiso 1 1 calc R . . H10C H 0.6996 0.2667 0.4613 0.061 Uiso 1 1 calc R . . C11 C 0.5462(5) 0.3094(5) 0.2150(4) 0.0406(15) Uani 1 1 d . . . H11A H 0.5454 0.3702 0.1809 0.061 Uiso 1 1 calc R . . H11B H 0.4679 0.2674 0.2085 0.061 Uiso 1 1 calc R . . H11C H 0.5872 0.2650 0.1891 0.061 Uiso 1 1 calc R . . C12 C 0.5134(5) 0.4017(5) 0.3956(4) 0.0381(14) Uani 1 1 d . . . H12A H 0.5379 0.4069 0.4640 0.057 Uiso 1 1 calc R . . H12B H 0.4389 0.3497 0.3720 0.057 Uiso 1 1 calc R . . H12C H 0.5082 0.4713 0.3787 0.057 Uiso 1 1 calc R . . C13 C 0.3842(4) 0.7039(4) 0.1781(3) 0.0228(11) Uani 1 1 d . . . C14 C 0.4149(4) 0.7917(4) 0.1289(4) 0.0277(12) Uani 1 1 d . . . C15 C 0.4658(4) 0.8845(4) 0.1947(4) 0.0288(12) Uani 1 1 d . . . C16 C 0.4670(4) 0.8571(4) 0.2852(4) 0.0259(12) Uani 1 1 d . . . C17 C 0.4152(4) 0.7472(4) 0.2749(3) 0.0236(11) Uani 1 1 d . . . C18 C 0.3928(5) 0.7875(6) 0.0244(4) 0.0453(16) Uani 1 1 d . . . H18A H 0.4303 0.8567 0.0098 0.068 Uiso 1 1 calc R . . H18B H 0.3108 0.7705 -0.0039 0.068 Uiso 1 1 calc R . . H18C H 0.4229 0.7328 -0.0007 0.068 Uiso 1 1 calc R . . C19 C 0.5062(5) 0.9947(5) 0.1715(5) 0.0434(16) Uani 1 1 d . . . H19A H 0.5381 0.9911 0.1174 0.065 Uiso 1 1 calc R . . H19B H 0.5648 1.0390 0.2254 0.065 Uiso 1 1 calc R . . H19C H 0.4421 1.0256 0.1565 0.065 Uiso 1 1 calc R . . C20 C 0.5151(5) 0.9324(5) 0.3756(4) 0.0393(15) Uani 1 1 d . . . H20A H 0.4632 0.9756 0.3819 0.059 Uiso 1 1 calc R . . H20B H 0.5893 0.9789 0.3756 0.059 Uiso 1 1 calc R . . H20C H 0.5240 0.8918 0.4282 0.059 Uiso 1 1 calc R . . C21 C 0.3936(5) 0.6886(5) 0.3544(4) 0.0324(13) Uani 1 1 d . . . H21A H 0.4425 0.7306 0.4137 0.049 Uiso 1 1 calc R . . H21B H 0.4103 0.6200 0.3466 0.049 Uiso 1 1 calc R . . H21C H 0.3137 0.6769 0.3549 0.049 Uiso 1 1 calc R . . C22 C 0.3623(5) 0.5139(6) 0.0295(4) 0.051(2) Uani 1 1 d . . . H22A H 0.3452 0.5466 -0.0273 0.077 Uiso 1 1 calc R . . H22B H 0.3301 0.4367 0.0144 0.077 Uiso 1 1 calc R . . H22C H 0.4448 0.5307 0.0548 0.077 Uiso 1 1 calc R . . C23 C 0.2806(6) 0.4663(5) 0.1996(5) 0.057(2) Uani 1 1 d . . . H23A H 0.3550 0.4579 0.2306 0.085 Uiso 1 1 calc R . . H23B H 0.2318 0.3981 0.1638 0.085 Uiso 1 1 calc R . . H23C H 0.2454 0.4897 0.2469 0.085 Uiso 1 1 calc R . . C24 C 0.1518(5) 0.5677(5) 0.0564(5) 0.053(2) Uani 1 1 d . . . H24A H 0.1116 0.5851 0.1020 0.079 Uiso 1 1 calc R . . H24B H 0.1107 0.4973 0.0206 0.079 Uiso 1 1 calc R . . H24C H 0.1559 0.6208 0.0136 0.079 Uiso 1 1 calc R . . C25 C 1.0387(5) 0.9716(4) 0.2150(4) 0.0277(12) Uani 1 1 d . . . C26 C 1.0267(5) 0.8905(4) 0.1412(4) 0.0282(12) Uani 1 1 d . . . C27 C 0.9351(5) 0.8927(5) 0.0663(4) 0.0381(15) Uani 1 1 d . . . C28 C 0.8937(5) 0.9787(5) 0.0927(5) 0.0441(17) Uani 1 1 d . . . C29 C 0.9569(5) 1.0278(5) 0.1831(5) 0.0385(15) Uani 1 1 d . . . C30 C 1.0969(6) 0.8134(5) 0.1404(5) 0.0482(17) Uani 1 1 d . . . H30A H 1.1749 0.8520 0.1420 0.072 Uiso 1 1 calc R . . H30B H 1.0642 0.7614 0.0833 0.072 Uiso 1 1 calc R . . H30C H 1.0973 0.7765 0.1953 0.072 Uiso 1 1 calc R . . C31 C 0.8905(7) 0.8217(7) -0.0263(4) 0.069(3) Uani 1 1 d . . . H31A H 0.9179 0.8597 -0.0743 0.103 Uiso 1 1 calc R . . H31B H 0.8073 0.8012 -0.0434 0.103 Uiso 1 1 calc R . . H31C H 0.9173 0.7579 -0.0216 0.103 Uiso 1 1 calc R . . C32 C 0.7999(6) 1.0133(7) 0.0305(6) 0.080(3) Uani 1 1 d . . . H32A H 0.7458 1.0239 0.0658 0.120 Uiso 1 1 calc R . . H32B H 0.7606 0.9584 -0.0238 0.120 Uiso 1 1 calc R . . H32C H 0.8325 1.0800 0.0093 0.120 Uiso 1 1 calc R . . C33 C 0.9440(7) 1.1264(5) 0.2335(6) 0.066(2) Uani 1 1 d . . . H33A H 1.0123 1.1852 0.2406 0.099 Uiso 1 1 calc R . . H33B H 0.9339 1.1132 0.2955 0.099 Uiso 1 1 calc R . . H33C H 0.8776 1.1449 0.1973 0.099 Uiso 1 1 calc R . . C34 C 1.2753(7) 1.1200(7) 0.3026(6) 0.087(3) Uani 1 1 d . . . H34A H 1.2983 1.0932 0.2488 0.130 Uiso 1 1 calc R . . H34B H 1.3405 1.1398 0.3579 0.130 Uiso 1 1 calc R . . H34C H 1.2485 1.1825 0.2892 0.130 Uiso 1 1 calc R . . C35 C 1.1126(8) 1.0658(7) 0.4272(5) 0.077(3) Uani 1 1 d . . . H35A H 1.0365 1.0222 0.4256 0.116 Uiso 1 1 calc R . . H35B H 1.1111 1.1396 0.4235 0.116 Uiso 1 1 calc R . . H35C H 1.1662 1.0624 0.4858 0.116 Uiso 1 1 calc R . . C36 C 1.2211(6) 0.9051(7) 0.3659(6) 0.070(2) Uani 1 1 d . . . H36A H 1.1628 0.8491 0.3807 0.105 Uiso 1 1 calc R . . H36B H 1.2844 0.9337 0.4219 0.105 Uiso 1 1 calc R . . H36C H 1.2489 0.8756 0.3162 0.105 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.0208(5) 0.0181(5) 0.0248(5) 0.0050(4) 0.0067(4) 0.0076(4) Sc2 0.0196(5) 0.0192(5) 0.0238(5) 0.0031(3) 0.0068(4) 0.0084(4) Sc3 0.0207(5) 0.0196(5) 0.0269(5) 0.0058(4) 0.0087(4) 0.0061(4) Si1 0.0322(8) 0.0187(8) 0.0328(9) 0.0034(6) 0.0093(6) 0.0056(6) Si2 0.0230(8) 0.0292(9) 0.0371(9) -0.0089(6) 0.0022(6) 0.0107(7) Si3 0.0370(10) 0.0502(12) 0.0432(11) 0.0009(8) 0.0099(8) -0.0072(9) N1 0.023(2) 0.021(2) 0.024(2) 0.0037(16) 0.0072(17) 0.0063(18) N2 0.028(2) 0.027(3) 0.022(2) 0.0047(17) 0.0066(17) 0.0083(19) N3 0.030(2) 0.022(2) 0.030(2) 0.0058(17) 0.0103(18) 0.0121(19) N4 0.030(2) 0.024(2) 0.020(2) 0.0021(16) 0.0077(17) 0.0104(19) N5 0.025(2) 0.025(3) 0.026(2) 0.0039(17) 0.0079(17) 0.0068(19) N6 0.025(2) 0.028(3) 0.028(2) 0.0032(18) 0.0084(18) 0.0117(19) C1 0.028(3) 0.018(3) 0.027(3) 0.008(2) 0.008(2) 0.006(2) C2 0.030(3) 0.021(3) 0.023(3) 0.007(2) 0.002(2) 0.009(2) C3 0.026(3) 0.026(3) 0.033(3) 0.010(2) 0.000(2) 0.010(2) C4 0.027(3) 0.027(3) 0.042(3) 0.016(2) 0.012(2) 0.016(2) C5 0.033(3) 0.025(3) 0.038(3) 0.010(2) 0.015(2) 0.019(2) C6 0.046(4) 0.033(3) 0.026(3) 0.007(2) 0.007(2) 0.007(3) C7 0.034(3) 0.039(4) 0.038(3) 0.008(3) -0.010(3) 0.004(3) C8 0.032(3) 0.045(4) 0.082(5) 0.026(3) 0.024(3) 0.023(3) C9 0.062(4) 0.033(4) 0.046(4) 0.007(3) 0.028(3) 0.025(3) C10 0.050(4) 0.023(3) 0.052(4) 0.009(3) 0.020(3) 0.007(3) C11 0.052(4) 0.028(3) 0.036(3) 0.000(2) 0.012(3) 0.002(3) C12 0.034(3) 0.036(4) 0.045(4) 0.007(3) 0.012(3) 0.010(3) C13 0.015(2) 0.022(3) 0.031(3) -0.002(2) 0.0032(19) 0.009(2) C14 0.021(3) 0.033(3) 0.033(3) 0.003(2) 0.007(2) 0.016(2) C15 0.020(3) 0.026(3) 0.045(3) 0.002(2) 0.006(2) 0.016(2) C16 0.020(3) 0.028(3) 0.032(3) -0.002(2) 0.010(2) 0.011(2) C17 0.019(2) 0.027(3) 0.028(3) 0.000(2) 0.009(2) 0.010(2) C18 0.035(3) 0.062(5) 0.042(4) 0.014(3) 0.008(3) 0.019(3) C19 0.046(4) 0.031(4) 0.058(4) 0.013(3) 0.013(3) 0.020(3) C20 0.036(3) 0.035(4) 0.045(4) -0.012(3) 0.008(3) 0.013(3) C21 0.031(3) 0.037(4) 0.030(3) 0.005(2) 0.012(2) 0.009(3) C22 0.038(4) 0.066(5) 0.043(4) -0.027(3) -0.004(3) 0.026(3) C23 0.061(5) 0.026(4) 0.071(5) -0.006(3) 0.008(4) 0.003(3) C24 0.025(3) 0.047(4) 0.077(5) -0.018(3) -0.004(3) 0.016(3) C25 0.031(3) 0.020(3) 0.036(3) 0.004(2) 0.019(2) 0.004(2) C26 0.033(3) 0.026(3) 0.030(3) 0.003(2) 0.017(2) 0.007(2) C27 0.045(4) 0.040(4) 0.025(3) 0.009(2) 0.017(3) -0.004(3) C28 0.035(3) 0.049(4) 0.059(4) 0.039(3) 0.019(3) 0.015(3) C29 0.037(3) 0.025(3) 0.066(4) 0.017(3) 0.031(3) 0.011(3) C30 0.052(4) 0.036(4) 0.071(5) 0.005(3) 0.040(4) 0.015(3) C31 0.071(5) 0.090(6) 0.025(4) -0.006(3) 0.017(3) -0.014(5) C32 0.051(5) 0.100(7) 0.105(7) 0.082(6) 0.023(4) 0.027(5) C33 0.071(5) 0.025(4) 0.120(7) 0.012(4) 0.047(5) 0.023(4) C34 0.053(5) 0.090(7) 0.085(7) 0.014(5) 0.006(4) -0.028(5) C35 0.104(7) 0.066(6) 0.048(5) -0.012(4) 0.014(4) 0.010(5) C36 0.036(4) 0.095(7) 0.079(6) 0.024(5) 0.008(4) 0.023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 N6 2.217(4) . ? Sc1 N1 2.217(4) . ? Sc1 N5 2.232(4) . ? Sc1 N2 2.236(4) . ? Sc1 C1 2.463(5) . ? Sc1 C5 2.499(5) . ? Sc1 C2 2.502(5) . ? Sc1 C4 2.527(5) . ? Sc1 C3 2.544(5) . ? Sc1 Sc3 3.2748(14) . ? Sc1 Sc2 3.2853(14) . ? Sc2 N4 2.218(4) . ? Sc2 N3 2.225(4) . ? Sc2 N1 2.231(4) . ? Sc2 N2 2.244(4) . ? Sc2 C17 2.483(5) . ? Sc2 C13 2.491(5) . ? Sc2 C16 2.498(5) . ? Sc2 C14 2.533(5) . ? Sc2 C15 2.535(5) . ? Sc2 Sc3 3.2741(14) . ? Sc3 N6 2.211(4) . ? Sc3 N3 2.219(4) . ? Sc3 N5 2.231(4) . ? Sc3 N4 2.236(4) . ? Sc3 C25 2.470(5) . ? Sc3 C29 2.507(6) . ? Sc3 C26 2.507(5) . ? Sc3 C27 2.508(6) . ? Sc3 C28 2.514(6) . ? Si1 C10 1.869(6) . ? Si1 C1 1.873(5) . ? Si1 C12 1.874(6) . ? Si1 C11 1.887(6) . ? Si2 C23 1.861(7) . ? Si2 C24 1.867(6) . ? Si2 C13 1.872(5) . ? Si2 C22 1.878(6) . ? Si3 C34 1.870(8) . ? Si3 C35 1.873(8) . ? Si3 C36 1.876(8) . ? Si3 C25 1.886(6) . ? C1 C5 1.420(7) . ? C1 C2 1.457(7) . ? C2 C3 1.399(7) . ? C2 C6 1.506(7) . ? C3 C4 1.413(8) . ? C3 C7 1.519(7) . ? C4 C5 1.407(8) . ? C4 C8 1.517(8) . ? C5 C9 1.504(7) . ? C13 C17 1.428(7) . ? C13 C14 1.433(8) . ? C14 C15 1.408(7) . ? C14 C18 1.505(8) . ? C15 C16 1.416(8) . ? C15 C19 1.504(8) . ? C16 C17 1.408(7) . ? C16 C20 1.504(7) . ? C17 C21 1.498(7) . ? C25 C26 1.422(7) . ? C25 C29 1.427(8) . ? C26 C27 1.411(8) . ? C26 C30 1.501(8) . ? C27 C28 1.421(9) . ? C27 C31 1.501(8) . ? C28 C29 1.401(9) . ? C28 C32 1.508(8) . ? C29 C33 1.508(9) . ? 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 N6 Sc1 N1 123.62(16) . . ? N6 Sc1 N5 71.97(16) . . ? N1 Sc1 N5 82.77(16) . . ? N6 Sc1 N2 82.96(16) . . ? N1 Sc1 N2 71.45(15) . . ? N5 Sc1 N2 124.76(16) . . ? N6 Sc1 C1 141.45(16) . . ? N1 Sc1 C1 94.64(16) . . ? N5 Sc1 C1 122.63(17) . . ? N2 Sc1 C1 107.78(17) . . ? N6 Sc1 C5 124.65(17) . . ? N1 Sc1 C5 105.38(17) . . ? N5 Sc1 C5 92.22(17) . . ? N2 Sc1 C5 140.96(18) . . ? C1 Sc1 C5 33.25(17) . . ? N6 Sc1 C2 111.73(16) . . ? N1 Sc1 C2 117.85(17) . . ? N5 Sc1 C2 143.89(17) . . ? N2 Sc1 C2 90.92(17) . . ? C1 Sc1 C2 34.13(16) . . ? C5 Sc1 C2 55.14(18) . . ? N6 Sc1 C4 93.33(17) . . ? N1 Sc1 C4 137.25(17) . . ? N5 Sc1 C4 90.33(17) . . ? N2 Sc1 C4 140.62(17) . . ? C1 Sc1 C4 54.57(17) . . ? C5 Sc1 C4 32.50(18) . . ? C2 Sc1 C4 54.07(18) . . ? N6 Sc1 C3 86.76(17) . . ? N1 Sc1 C3 148.50(17) . . ? N5 Sc1 C3 118.10(18) . . ? N2 Sc1 C3 108.32(17) . . ? C1 Sc1 C3 54.69(17) . . ? C5 Sc1 C3 54.05(18) . . ? C2 Sc1 C3 32.17(17) . . ? C4 Sc1 C3 32.36(17) . . ? N6 Sc1 Sc3 42.24(11) . . ? N1 Sc1 Sc3 85.74(11) . . ? N5 Sc1 Sc3 42.78(11) . . ? N2 Sc1 Sc3 86.31(12) . . ? C1 Sc1 Sc3 165.29(13) . . ? C5 Sc1 Sc3 132.71(13) . . ? C2 Sc1 Sc3 153.96(12) . . ? C4 Sc1 Sc3 116.61(13) . . ? C3 Sc1 Sc3 125.73(13) . . ? N6 Sc1 Sc2 85.05(11) . . ? N1 Sc1 Sc2 42.57(11) . . ? N5 Sc1 Sc2 85.62(11) . . ? N2 Sc1 Sc2 42.92(11) . . ? C1 Sc1 Sc2 128.34(13) . . ? C5 Sc1 Sc2 147.92(13) . . ? C2 Sc1 Sc2 130.00(13) . . ? C4 Sc1 Sc2 175.93(13) . . ? C3 Sc1 Sc2 150.89(14) . . ? Sc3 Sc1 Sc2 59.88(3) . . ? N4 Sc2 N3 72.32(15) . . ? N4 Sc2 N1 82.85(16) . . ? N3 Sc2 N1 123.48(15) . . ? N4 Sc2 N2 124.74(16) . . ? N3 Sc2 N2 82.82(16) . . ? N1 Sc2 N2 71.05(15) . . ? N4 Sc2 C17 143.90(16) . . ? N3 Sc2 C17 123.63(16) . . ? N1 Sc2 C17 106.39(17) . . ? N2 Sc2 C17 90.85(16) . . ? N4 Sc2 C13 112.98(16) . . ? N3 Sc2 C13 142.17(17) . . ? N1 Sc2 C13 94.15(16) . . ? N2 Sc2 C13 116.63(17) . . ? C17 Sc2 C13 33.36(16) . . ? N4 Sc2 C16 131.69(17) . . ? N3 Sc2 C16 92.29(16) . . ? N1 Sc2 C16 138.77(17) . . ? N2 Sc2 C16 96.91(17) . . ? C17 Sc2 C16 32.83(17) . . ? C13 Sc2 C16 55.20(16) . . ? N4 Sc2 C14 90.08(16) . . ? N3 Sc2 C14 114.06(17) . . ? N1 Sc2 C14 115.91(16) . . ? N2 Sc2 C14 145.07(17) . . ? C17 Sc2 C14 54.23(17) . . ? C13 Sc2 C14 33.13(17) . . ? C16 Sc2 C14 54.16(17) . . ? N4 Sc2 C15 99.70(17) . . ? N3 Sc2 C15 87.64(16) . . ? N1 Sc2 C15 147.34(16) . . ? N2 Sc2 C15 128.24(17) . . ? C17 Sc2 C15 54.01(18) . . ? C13 Sc2 C15 54.63(17) . . ? C16 Sc2 C15 32.67(18) . . ? C14 Sc2 C15 32.27(16) . . ? N4 Sc2 Sc3 42.91(10) . . ? N3 Sc2 Sc3 42.48(11) . . ? N1 Sc2 Sc3 85.54(11) . . ? N2 Sc2 Sc3 86.20(12) . . ? C17 Sc2 Sc3 166.07(12) . . ? C13 Sc2 Sc3 155.79(13) . . ? C16 Sc2 Sc3 134.12(13) . . ? C14 Sc2 Sc3 127.32(13) . . ? C15 Sc2 Sc3 118.49(13) . . ? N4 Sc2 Sc1 85.76(11) . . ? N3 Sc2 Sc1 85.12(11) . . ? N1 Sc2 Sc1 42.23(10) . . ? N2 Sc2 Sc1 42.73(11) . . ? C17 Sc2 Sc1 124.81(13) . . ? C13 Sc2 Sc1 131.67(13) . . ? C16 Sc2 Sc1 139.60(13) . . ? C14 Sc2 Sc1 158.09(13) . . ? C15 Sc2 Sc1 169.17(13) . . ? Sc3 Sc2 Sc1 59.90(3) . . ? N6 Sc3 N3 81.95(16) . . ? N6 Sc3 N5 72.10(16) . . ? N3 Sc3 N5 124.17(16) . . ? N6 Sc3 N4 123.76(16) . . ? N3 Sc3 N4 72.07(15) . . ? N5 Sc3 N4 82.69(16) . . ? N6 Sc3 C25 92.45(17) . . ? N3 Sc3 C25 113.23(17) . . ? N5 Sc3 C25 116.36(17) . . ? N4 Sc3 C25 143.51(18) . . ? N6 Sc3 C29 113.65(19) . . ? N3 Sc3 C29 90.10(18) . . ? N5 Sc3 C29 145.50(18) . . ? N4 Sc3 C29 115.29(19) . . ? C25 Sc3 C29 33.31(18) . . ? N6 Sc3 C26 105.34(17) . . ? N3 Sc3 C26 144.19(17) . . ? N5 Sc3 C26 90.92(17) . . ? N4 Sc3 C26 124.91(17) . . ? C25 Sc3 C26 33.18(16) . . ? C29 Sc3 C26 54.58(18) . . ? N6 Sc3 C27 137.75(19) . . ? N3 Sc3 C27 132.5(2) . . ? N5 Sc3 C27 97.23(19) . . ? N4 Sc3 C27 93.80(18) . . ? C25 Sc3 C27 54.94(18) . . ? C29 Sc3 C27 54.6(2) . . ? C26 Sc3 C27 32.68(19) . . ? N6 Sc3 C28 145.2(2) . . ? N3 Sc3 C28 100.3(2) . . ? N5 Sc3 C28 128.8(2) . . ? N4 Sc3 C28 89.12(18) . . ? C25 Sc3 C28 54.48(19) . . ? C29 Sc3 C28 32.4(2) . . ? C26 Sc3 C28 54.04(19) . . ? C27 Sc3 C28 32.9(2) . . ? N6 Sc3 Sc2 85.42(11) . . ? N3 Sc3 Sc2 42.62(11) . . ? N5 Sc3 Sc2 85.91(11) . . ? N4 Sc3 Sc2 42.46(11) . . ? C25 Sc3 Sc2 155.83(13) . . ? C29 Sc3 Sc2 127.63(14) . . ? C26 Sc3 Sc2 167.28(13) . . ? C27 Sc3 Sc2 135.62(14) . . ? C28 Sc3 Sc2 119.72(14) . . ? N6 Sc3 Sc1 42.37(11) . . ? N3 Sc3 Sc1 85.47(12) . . ? N5 Sc3 Sc1 42.81(11) . . ? N4 Sc3 Sc1 85.73(12) . . ? C25 Sc3 Sc1 129.85(13) . . ? C29 Sc3 Sc1 156.00(16) . . ? C26 Sc3 Sc1 123.82(13) . . ? C27 Sc3 Sc1 139.84(16) . . ? C28 Sc3 Sc1 170.75(18) . . ? Sc2 Sc3 Sc1 60.22(3) . . ? C10 Si1 C1 108.0(3) . . ? C10 Si1 C12 108.3(3) . . ? C1 Si1 C12 112.4(3) . . ? C10 Si1 C11 107.2(3) . . ? C1 Si1 C11 114.1(3) . . ? C12 Si1 C11 106.6(3) . . ? C23 Si2 C24 105.8(3) . . ? C23 Si2 C13 114.5(3) . . ? C24 Si2 C13 110.6(3) . . ? C23 Si2 C22 106.4(3) . . ? C24 Si2 C22 107.0(3) . . ? C13 Si2 C22 112.1(3) . . ? C34 Si3 C35 109.7(4) . . ? C34 Si3 C36 107.0(4) . . ? C35 Si3 C36 105.1(4) . . ? C34 Si3 C25 108.3(3) . . ? C35 Si3 C25 112.5(3) . . ? C36 Si3 C25 114.0(3) . . ? Sc1 N1 Sc2 95.21(15) . . ? Sc1 N2 Sc2 94.35(16) . . ? Sc3 N3 Sc2 94.90(16) . . ? Sc2 N4 Sc3 94.63(15) . . ? Sc3 N5 Sc1 94.41(16) . . ? Sc3 N6 Sc1 95.39(16) . . ? C5 C1 C2 107.1(5) . . ? C5 C1 Si1 126.1(4) . . ? C2 C1 Si1 125.2(4) . . ? C5 C1 Sc1 74.8(3) . . ? C2 C1 Sc1 74.4(3) . . ? Si1 C1 Sc1 127.9(2) . . ? C3 C2 C1 107.3(5) . . ? C3 C2 C6 125.2(5) . . ? C1 C2 C6 127.4(5) . . ? C3 C2 Sc1 75.6(3) . . ? C1 C2 Sc1 71.5(3) . . ? C6 C2 Sc1 121.3(4) . . ? C2 C3 C4 108.8(5) . . ? C2 C3 C7 126.1(5) . . ? C4 C3 C7 125.1(5) . . ? C2 C3 Sc1 72.2(3) . . ? C4 C3 Sc1 73.1(3) . . ? C7 C3 Sc1 123.5(4) . . ? C5 C4 C3 108.7(5) . . ? C5 C4 C8 126.2(6) . . ? C3 C4 C8 125.0(5) . . ? C5 C4 Sc1 72.7(3) . . ? C3 C4 Sc1 74.5(3) . . ? C8 C4 Sc1 122.1(4) . . ? C4 C5 C1 108.1(5) . . ? C4 C5 C9 125.1(5) . . ? C1 C5 C9 126.8(5) . . ? C4 C5 Sc1 74.8(3) . . ? C1 C5 Sc1 72.0(3) . . ? C9 C5 Sc1 120.4(4) . . ? C17 C13 C14 106.1(4) . . ? C17 C13 Si2 129.3(4) . . ? C14 C13 Si2 123.8(4) . . ? C17 C13 Sc2 73.0(3) . . ? C14 C13 Sc2 75.0(3) . . ? Si2 C13 Sc2 124.9(2) . . ? C15 C14 C13 108.6(5) . . ? C15 C14 C18 125.1(5) . . ? C13 C14 C18 126.3(5) . . ? C15 C14 Sc2 73.9(3) . . ? C13 C14 Sc2 71.8(3) . . ? C18 C14 Sc2 122.1(4) . . ? C14 C15 C16 108.4(5) . . ? C14 C15 C19 125.4(5) . . ? C16 C15 C19 126.1(5) . . ? C14 C15 Sc2 73.8(3) . . ? C16 C15 Sc2 72.2(3) . . ? C19 C15 Sc2 122.3(4) . . ? C17 C16 C15 107.6(4) . . ? C17 C16 C20 126.6(5) . . ? C15 C16 C20 125.8(5) . . ? C17 C16 Sc2 73.0(3) . . ? C15 C16 Sc2 75.1(3) . . ? C20 C16 Sc2 117.8(3) . . ? C16 C17 C13 109.2(5) . . ? C16 C17 C21 123.9(5) . . ? C13 C17 C21 126.8(5) . . ? C16 C17 Sc2 74.2(3) . . ? C13 C17 Sc2 73.6(3) . . ? C21 C17 Sc2 120.4(4) . . ? C26 C25 C29 107.6(5) . . ? C26 C25 Si3 126.0(4) . . ? C29 C25 Si3 125.5(4) . . ? C26 C25 Sc3 74.8(3) . . ? C29 C25 Sc3 74.7(3) . . ? Si3 C25 Sc3 125.1(3) . . ? C27 C26 C25 108.4(5) . . ? C27 C26 C30 124.4(5) . . ? C25 C26 C30 127.3(5) . . ? C27 C26 Sc3 73.7(3) . . ? C25 C26 Sc3 72.0(3) . . ? C30 C26 Sc3 119.8(4) . . ? C26 C27 C28 107.3(5) . . ? C26 C27 C31 127.6(7) . . ? C28 C27 C31 125.1(6) . . ? C26 C27 Sc3 73.6(3) . . ? C28 C27 Sc3 73.8(3) . . ? C31 C27 Sc3 120.1(4) . . ? C29 C28 C27 109.0(5) . . ? C29 C28 C32 126.1(7) . . ? C27 C28 C32 124.8(7) . . ? C29 C28 Sc3 73.5(3) . . ? C27 C28 Sc3 73.3(3) . . ? C32 C28 Sc3 121.5(4) . . ? C28 C29 C25 107.6(5) . . ? C28 C29 C33 125.2(6) . . ? C25 C29 C33 127.1(6) . . ? C28 C29 Sc3 74.1(3) . . ? C25 C29 Sc3 71.9(3) . . ? C33 C29 Sc3 122.6(4) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.155 _refine_diff_density_min -1.102 _refine_diff_density_rms 0.137 data_3Lu _database_code_depnum_ccdc_archive 'CCDC 767212' #TrackingRef '- DT-ART-02-2010-00006.cif' _database_code_depnum_ccdc_archive 'CCDC 767212' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H75 Lu3 N6 Si3' _chemical_formula_weight 1201.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.9129(19) _cell_length_b 18.206(4) _cell_length_c 29.000(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4705.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 29385 _cell_measurement_theta_min 1.32 _cell_measurement_theta_max 27.51 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 6.350 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1434 _exptl_absorpt_correction_T_max 0.4493 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ; _diffrn_ambient_temperature 163(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 29385 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 27.51 _reflns_number_total 10575 _reflns_number_gt 9341 _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 'ORTEP-III (Farrugia, 1997)' _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^)+(0.0120P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.018(9) _refine_ls_number_reflns 10575 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0567 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _refine_ls_shift/su_max 0.024 _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 0.39503(3) 0.593133(14) 0.898447(10) 0.01998(7) Uani 1 1 d . . . Lu2 Lu 0.57664(3) 0.472864(15) 0.971921(10) 0.02178(7) Uani 1 1 d . . . Lu3 Lu 0.51350(3) 0.425474(15) 0.857568(10) 0.02084(7) Uani 1 1 d . . . N1 N 0.4502(7) 0.3816(3) 0.93049(18) 0.0279(15) Uani 1 1 d . . . H1A H 0.4880 0.3354 0.9360 0.033 Uiso 1 1 calc R . . H1B H 0.3484 0.3822 0.9357 0.033 Uiso 1 1 calc R . . N2 N 0.7174(6) 0.4455(3) 0.90711(19) 0.0285(15) Uani 1 1 d . . . H2A H 0.7754 0.4041 0.9110 0.034 Uiso 1 1 calc R . . H2B H 0.7764 0.4842 0.8978 0.034 Uiso 1 1 calc R . . N3 N 0.2844(6) 0.4868(3) 0.86706(18) 0.0246(14) Uani 1 1 d . . . H3A H 0.2211 0.4635 0.8874 0.030 Uiso 1 1 calc R . . H3B H 0.2360 0.4956 0.8396 0.030 Uiso 1 1 calc R . . N4 N 0.5514(6) 0.5484(3) 0.84173(18) 0.0261(14) Uani 1 1 d . . . H4A H 0.6496 0.5625 0.8459 0.031 Uiso 1 1 calc R . . H4B H 0.5200 0.5612 0.8126 0.031 Uiso 1 1 calc R . . N5 N 0.3435(6) 0.5309(3) 0.96668(18) 0.0260(14) Uani 1 1 d . . . H5A H 0.2655 0.4982 0.9637 0.031 Uiso 1 1 calc R . . H5B H 0.3256 0.5622 0.9910 0.031 Uiso 1 1 calc R . . N6 N 0.6130(7) 0.5915(3) 0.94406(17) 0.0261(13) Uani 1 1 d . . . H6A H 0.6993 0.5960 0.9269 0.031 Uiso 1 1 calc R . . H6B H 0.6113 0.6263 0.9670 0.031 Uiso 1 1 calc R . . Si1 Si 0.1020(3) 0.66323(11) 0.80673(7) 0.0309(5) Uani 1 1 d . . . Si2 Si 0.4891(3) 0.53134(11) 1.10107(7) 0.0321(5) Uani 1 1 d . . . Si3 Si 0.3712(2) 0.22580(11) 0.83677(7) 0.0283(5) Uani 1 1 d . . . C1 C 0.2188(8) 0.6850(3) 0.8581(2) 0.0214(15) Uani 1 1 d . . . C2 C 0.3655(8) 0.7189(3) 0.8547(3) 0.0250(16) Uani 1 1 d . . . C3 C 0.4122(9) 0.7384(3) 0.8989(3) 0.0262(16) Uani 1 1 d . . . C4 C 0.2977(9) 0.7182(4) 0.9310(3) 0.0288(18) Uani 1 1 d . . . C5 C 0.1801(8) 0.6853(3) 0.9062(2) 0.0236(17) Uani 1 1 d . . . C6 C 0.4528(8) 0.7362(4) 0.8112(2) 0.036(2) Uani 1 1 d . . . H6C H 0.5603 0.7298 0.8171 0.054 Uiso 1 1 calc R . . H6D H 0.4333 0.7871 0.8020 0.054 Uiso 1 1 calc R . . H6E H 0.4212 0.7030 0.7865 0.054 Uiso 1 1 calc R . . C7 C 0.5570(8) 0.7781(4) 0.9102(3) 0.039(2) Uani 1 1 d . . . H7A H 0.5541 0.8277 0.8970 0.058 Uiso 1 1 calc R . . H7B H 0.6418 0.7510 0.8970 0.058 Uiso 1 1 calc R . . H7C H 0.5688 0.7813 0.9437 0.058 Uiso 1 1 calc R . . C8 C 0.3009(10) 0.7325(4) 0.9822(2) 0.043(2) Uani 1 1 d . . . H8A H 0.2436 0.6942 0.9982 0.064 Uiso 1 1 calc R . . H8B H 0.2562 0.7806 0.9886 0.064 Uiso 1 1 calc R . . H8C H 0.4050 0.7319 0.9931 0.064 Uiso 1 1 calc R . . C9 C 0.0380(8) 0.6584(4) 0.9271(2) 0.037(2) Uani 1 1 d . . . H9A H 0.0496 0.6553 0.9607 0.056 Uiso 1 1 calc R . . H9B H 0.0143 0.6096 0.9148 0.056 Uiso 1 1 calc R . . H9C H -0.0436 0.6925 0.9197 0.056 Uiso 1 1 calc R . . C10 C -0.0754(10) 0.6169(4) 0.8220(3) 0.056(3) Uani 1 1 d . . . H10A H -0.1305 0.6046 0.7938 0.084 Uiso 1 1 calc R . . H10B H -0.1364 0.6496 0.8412 0.084 Uiso 1 1 calc R . . H10C H -0.0534 0.5718 0.8392 0.084 Uiso 1 1 calc R . . C11 C 0.0560(9) 0.7505(4) 0.7771(3) 0.048(2) Uani 1 1 d . . . H11A H 0.0041 0.7398 0.7480 0.072 Uiso 1 1 calc R . . H11B H 0.1487 0.7775 0.7706 0.072 Uiso 1 1 calc R . . H11C H -0.0092 0.7802 0.7968 0.072 Uiso 1 1 calc R . . C12 C 0.1965(10) 0.6040(5) 0.7624(3) 0.056(3) Uani 1 1 d . . . H12A H 0.2993 0.6214 0.7575 0.084 Uiso 1 1 calc R . . H12B H 0.1407 0.6067 0.7333 0.084 Uiso 1 1 calc R . . H12C H 0.1987 0.5530 0.7732 0.084 Uiso 1 1 calc R . . C13 C 0.6017(8) 0.4726(4) 1.0610(2) 0.0230(15) Uani 1 1 d . . . C14 C 0.5697(8) 0.3985(3) 1.0479(2) 0.0215(15) Uani 1 1 d . . . C15 C 0.6936(8) 0.3702(4) 1.0238(2) 0.0258(17) Uani 1 1 d . . . C16 C 0.8058(8) 0.4264(4) 1.0207(2) 0.0267(17) Uani 1 1 d . . . C17 C 0.7501(8) 0.4884(4) 1.0438(2) 0.0285(18) Uani 1 1 d . . . C18 C 0.4303(9) 0.3556(3) 1.0585(3) 0.035(2) Uani 1 1 d . . . H18A H 0.4418 0.3052 1.0472 0.053 Uiso 1 1 calc R . . H18B H 0.3443 0.3787 1.0432 0.053 Uiso 1 1 calc R . . H18C H 0.4136 0.3550 1.0919 0.053 Uiso 1 1 calc R . . C19 C 0.7145(9) 0.2929(4) 1.0054(3) 0.040(2) Uani 1 1 d . . . H19A H 0.7878 0.2668 1.0246 0.060 Uiso 1 1 calc R . . H19B H 0.7509 0.2951 0.9736 0.060 Uiso 1 1 calc R . . H19C H 0.6184 0.2668 1.0063 0.060 Uiso 1 1 calc R . . C20 C 0.9586(7) 0.4184(5) 1.0006(3) 0.045(2) Uani 1 1 d . . . H20A H 0.9622 0.3740 0.9815 0.067 Uiso 1 1 calc R . . H20B H 1.0325 0.4143 1.0255 0.067 Uiso 1 1 calc R . . H20C H 0.9816 0.4614 0.9816 0.067 Uiso 1 1 calc R . . C21 C 0.8440(9) 0.5571(4) 1.0527(3) 0.042(2) Uani 1 1 d . . . H21A H 0.9243 0.5602 1.0297 0.062 Uiso 1 1 calc R . . H21B H 0.8880 0.5544 1.0836 0.062 Uiso 1 1 calc R . . H21C H 0.7799 0.6007 1.0504 0.062 Uiso 1 1 calc R . . C22 C 0.5566(12) 0.5147(5) 1.1604(3) 0.085(4) Uani 1 1 d . . . H22A H 0.6563 0.5366 1.1642 0.127 Uiso 1 1 calc R . . H22B H 0.5624 0.4617 1.1660 0.127 Uiso 1 1 calc R . . H22C H 0.4869 0.5370 1.1824 0.127 Uiso 1 1 calc R . . C23 C 0.5036(12) 0.6316(4) 1.0882(3) 0.067(3) Uani 1 1 d . . . H23A H 0.4866 0.6398 1.0552 0.101 Uiso 1 1 calc R . . H23B H 0.6038 0.6492 1.0966 0.101 Uiso 1 1 calc R . . H23C H 0.4279 0.6584 1.1061 0.101 Uiso 1 1 calc R . . C24 C 0.2848(10) 0.5109(5) 1.1009(4) 0.074(3) Uani 1 1 d . . . H24A H 0.2675 0.4624 1.1147 0.111 Uiso 1 1 calc R . . H24B H 0.2475 0.5111 1.0691 0.111 Uiso 1 1 calc R . . H24C H 0.2316 0.5483 1.1189 0.111 Uiso 1 1 calc R . . C25 C 0.4921(8) 0.3022(3) 0.8146(2) 0.0194(15) Uani 1 1 d . . . C26 C 0.6478(8) 0.3148(4) 0.8200(2) 0.0240(17) Uani 1 1 d . . . C27 C 0.6899(8) 0.3754(4) 0.7928(2) 0.0226(16) Uani 1 1 d . . . C28 C 0.5625(8) 0.4000(3) 0.7692(2) 0.0239(16) Uani 1 1 d . . . C29 C 0.4384(8) 0.3565(3) 0.7818(2) 0.0200(15) Uani 1 1 d . . . C30 C 0.7571(8) 0.2706(4) 0.8492(3) 0.036(2) Uani 1 1 d . . . H30A H 0.7897 0.2272 0.8320 0.054 Uiso 1 1 calc R . . H30B H 0.7076 0.2553 0.8778 0.054 Uiso 1 1 calc R . . H30C H 0.8445 0.3011 0.8566 0.054 Uiso 1 1 calc R . . C31 C 0.8457(8) 0.4085(4) 0.7892(3) 0.042(2) Uani 1 1 d . . . H31A H 0.8991 0.3861 0.7632 0.063 Uiso 1 1 calc R . . H31B H 0.9010 0.3991 0.8178 0.063 Uiso 1 1 calc R . . H31C H 0.8375 0.4616 0.7843 0.063 Uiso 1 1 calc R . . C32 C 0.5597(10) 0.4601(3) 0.7327(2) 0.040(2) Uani 1 1 d . . . H32A H 0.4582 0.4805 0.7304 0.060 Uiso 1 1 calc R . . H32B H 0.5891 0.4394 0.7028 0.060 Uiso 1 1 calc R . . H32C H 0.6301 0.4992 0.7413 0.060 Uiso 1 1 calc R . . C33 C 0.2840(9) 0.3632(4) 0.7620(3) 0.037(2) Uani 1 1 d . . . H33A H 0.2750 0.3311 0.7350 0.056 Uiso 1 1 calc R . . H33B H 0.2658 0.4142 0.7528 0.056 Uiso 1 1 calc R . . H33C H 0.2100 0.3486 0.7853 0.056 Uiso 1 1 calc R . . C34 C 0.1911(8) 0.2596(4) 0.8621(3) 0.039(2) Uani 1 1 d . . . H34A H 0.2124 0.2889 0.8897 0.058 Uiso 1 1 calc R . . H34B H 0.1280 0.2176 0.8705 0.058 Uiso 1 1 calc R . . H34C H 0.1384 0.2901 0.8394 0.058 Uiso 1 1 calc R . . C35 C 0.3216(10) 0.1631(4) 0.7884(3) 0.044(2) Uani 1 1 d . . . H35A H 0.2551 0.1242 0.7998 0.066 Uiso 1 1 calc R . . H35B H 0.4132 0.1410 0.7759 0.066 Uiso 1 1 calc R . . H35C H 0.2705 0.1909 0.7642 0.066 Uiso 1 1 calc R . . C36 C 0.4648(9) 0.1682(4) 0.8818(3) 0.051(3) Uani 1 1 d . . . H36A H 0.5547 0.1452 0.8687 0.076 Uiso 1 1 calc R . . H36B H 0.3954 0.1299 0.8922 0.076 Uiso 1 1 calc R . . H36C H 0.4934 0.1992 0.9080 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 Lu1 0.02207(16) 0.01828(14) 0.01958(15) 0.00013(12) -0.00069(13) 0.00264(12) Lu2 0.02416(17) 0.02126(15) 0.01994(16) 0.00113(13) -0.00411(14) 0.00121(13) Lu3 0.02205(17) 0.01973(14) 0.02074(15) -0.00311(13) 0.00018(13) 0.00138(12) N1 0.030(4) 0.019(3) 0.034(4) 0.003(3) -0.005(3) 0.005(2) N2 0.025(4) 0.022(3) 0.039(4) -0.008(3) -0.003(3) 0.007(2) N3 0.023(4) 0.030(3) 0.021(3) 0.004(3) -0.002(3) 0.000(3) N4 0.025(4) 0.032(3) 0.021(3) -0.001(2) 0.001(3) -0.001(3) N5 0.020(3) 0.031(3) 0.026(3) 0.000(3) 0.002(3) 0.001(3) N6 0.033(4) 0.024(3) 0.022(3) -0.006(3) 0.000(3) 0.001(3) Si1 0.0291(13) 0.0297(11) 0.0339(13) 0.0056(9) -0.0109(11) -0.0006(10) Si2 0.0405(13) 0.0303(11) 0.0256(11) -0.0016(10) -0.0026(11) 0.0029(11) Si3 0.0316(13) 0.0248(11) 0.0284(12) 0.0004(9) 0.0046(10) -0.0041(9) C1 0.023(4) 0.015(3) 0.026(4) 0.001(3) 0.000(3) 0.003(3) C2 0.021(4) 0.024(4) 0.030(4) 0.005(3) 0.005(3) 0.008(3) C3 0.034(4) 0.008(3) 0.037(4) 0.002(3) -0.010(4) 0.003(3) C4 0.045(5) 0.016(4) 0.025(4) -0.006(3) -0.003(4) 0.011(3) C5 0.027(4) 0.016(3) 0.028(4) 0.002(3) 0.001(3) 0.006(3) C6 0.026(5) 0.044(5) 0.038(5) 0.006(4) 0.009(4) -0.007(4) C7 0.042(6) 0.028(4) 0.047(5) -0.008(4) -0.014(4) -0.002(4) C8 0.065(7) 0.033(5) 0.031(5) -0.007(4) 0.002(4) 0.016(4) C9 0.039(5) 0.041(5) 0.032(5) 0.005(4) 0.007(4) 0.001(4) C10 0.051(6) 0.054(5) 0.062(6) 0.010(5) -0.018(5) -0.025(5) C11 0.034(5) 0.057(5) 0.052(6) 0.021(4) -0.014(4) 0.001(4) C12 0.071(7) 0.066(6) 0.032(5) -0.010(5) -0.024(5) 0.017(5) C13 0.023(4) 0.028(4) 0.017(3) 0.004(3) -0.006(3) -0.009(4) C14 0.018(4) 0.030(4) 0.017(3) 0.003(3) 0.001(3) 0.000(3) C15 0.031(4) 0.024(4) 0.023(4) 0.004(3) -0.004(3) 0.007(3) C16 0.022(4) 0.035(4) 0.023(4) 0.006(3) -0.002(3) 0.010(3) C17 0.035(5) 0.026(4) 0.025(4) 0.009(3) -0.011(3) -0.004(3) C18 0.036(5) 0.023(4) 0.047(5) 0.004(4) -0.003(4) -0.002(4) C19 0.052(6) 0.036(5) 0.033(5) 0.008(4) -0.001(4) 0.010(4) C20 0.018(4) 0.074(6) 0.042(5) 0.008(5) -0.004(4) 0.011(4) C21 0.044(6) 0.036(5) 0.045(5) 0.004(4) -0.010(4) -0.016(4) C22 0.102(10) 0.125(9) 0.027(5) -0.012(5) -0.002(6) 0.054(8) C23 0.096(8) 0.032(5) 0.074(7) -0.005(4) 0.019(7) 0.004(5) C24 0.058(7) 0.082(8) 0.081(8) -0.018(7) 0.031(6) 0.010(6) C25 0.029(4) 0.010(3) 0.019(4) -0.005(3) 0.000(3) 0.002(3) C26 0.026(4) 0.021(4) 0.025(4) -0.002(3) 0.003(3) 0.007(3) C27 0.016(4) 0.027(4) 0.025(4) -0.016(3) 0.013(3) -0.003(3) C28 0.035(5) 0.014(3) 0.023(4) -0.001(3) 0.004(3) -0.001(3) C29 0.022(4) 0.017(3) 0.020(4) -0.008(3) -0.005(3) 0.000(3) C30 0.037(5) 0.029(4) 0.040(5) -0.004(4) 0.000(4) 0.005(4) C31 0.037(5) 0.038(5) 0.050(5) -0.017(4) 0.012(4) -0.003(4) C32 0.070(7) 0.024(4) 0.027(4) 0.003(3) 0.008(4) -0.006(4) C33 0.044(6) 0.029(4) 0.039(5) -0.004(4) -0.009(4) 0.001(4) C34 0.035(5) 0.041(5) 0.041(5) 0.001(4) 0.009(4) -0.003(4) C35 0.056(6) 0.028(4) 0.048(6) -0.005(4) 0.015(5) -0.015(4) C36 0.054(7) 0.040(5) 0.058(6) 0.026(4) 0.017(5) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 N4 2.305(5) . ? Lu1 N5 2.326(5) . ? Lu1 N6 2.350(5) . ? Lu1 N3 2.355(5) . ? Lu1 C5 2.557(7) . ? Lu1 C1 2.575(6) . ? Lu1 C4 2.613(6) . ? Lu1 C2 2.631(6) . ? Lu1 C3 2.649(6) . ? Lu1 Lu3 3.4406(7) . ? Lu1 Lu2 3.4576(6) . ? Lu2 N2 2.314(5) . ? Lu2 N6 2.329(5) . ? Lu2 N5 2.337(5) . ? Lu2 N1 2.340(5) . ? Lu2 C14 2.588(6) . ? Lu2 C13 2.592(6) . ? Lu2 C17 2.610(7) . ? Lu2 C15 2.616(6) . ? Lu2 C16 2.625(7) . ? Lu2 Lu3 3.4726(8) . ? Lu3 N4 2.310(5) . ? Lu3 N1 2.330(5) . ? Lu3 N3 2.344(5) . ? Lu3 N2 2.345(6) . ? Lu3 C25 2.573(6) . ? Lu3 C26 2.585(6) . ? Lu3 C27 2.614(6) . ? Lu3 C29 2.617(6) . ? Lu3 C28 2.640(6) . ? Si1 C10 1.846(9) . ? Si1 C11 1.853(7) . ? Si1 C1 1.860(7) . ? Si1 C12 1.878(8) . ? Si2 C22 1.847(8) . ? Si2 C24 1.859(9) . ? Si2 C23 1.867(7) . ? Si2 C13 1.872(7) . ? Si3 C35 1.861(7) . ? Si3 C34 1.870(7) . ? Si3 C36 1.871(7) . ? Si3 C25 1.873(7) . ? C1 C5 1.438(9) . ? C1 C2 1.449(9) . ? C2 C3 1.395(9) . ? C2 C6 1.514(9) . ? C3 C4 1.429(10) . ? C3 C7 1.514(9) . ? C4 C5 1.404(10) . ? C4 C8 1.509(9) . ? C5 C9 1.487(9) . ? C13 C14 1.430(8) . ? C13 C17 1.442(10) . ? C14 C15 1.406(9) . ? C14 C18 1.498(9) . ? C15 C16 1.433(9) . ? C15 C19 1.515(9) . ? C16 C17 1.403(9) . ? C16 C20 1.489(9) . ? C17 C21 1.527(9) . ? C25 C26 1.415(10) . ? C25 C29 1.454(8) . ? C26 C27 1.408(9) . ? C26 C30 1.519(9) . ? C27 C28 1.399(9) . ? C27 C31 1.517(9) . ? C28 C29 1.408(9) . ? C28 C32 1.524(8) . ? C29 C33 1.496(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Lu1 N5 123.70(18) . . ? N4 Lu1 N6 84.11(19) . . ? N5 Lu1 N6 71.24(18) . . ? N4 Lu1 N3 71.77(18) . . ? N5 Lu1 N3 81.14(18) . . ? N6 Lu1 N3 123.59(18) . . ? N4 Lu1 C5 138.4(2) . . ? N5 Lu1 C5 95.5(2) . . ? N6 Lu1 C5 125.3(2) . . ? N3 Lu1 C5 105.1(2) . . ? N4 Lu1 C1 105.9(2) . . ? N5 Lu1 C1 125.6(2) . . ? N6 Lu1 C1 140.16(19) . . ? N3 Lu1 C1 95.89(19) . . ? C5 Lu1 C1 32.5(2) . . ? N4 Lu1 C4 140.0(2) . . ? N5 Lu1 C4 92.9(2) . . ? N6 Lu1 C4 94.7(2) . . ? N3 Lu1 C4 135.8(2) . . ? C5 Lu1 C4 31.5(2) . . ? C1 Lu1 C4 52.8(2) . . ? N4 Lu1 C2 91.4(2) . . ? N5 Lu1 C2 144.5(2) . . ? N6 Lu1 C2 111.4(2) . . ? N3 Lu1 C2 119.1(2) . . ? C5 Lu1 C2 52.9(2) . . ? C1 Lu1 C2 32.3(2) . . ? C4 Lu1 C2 51.9(2) . . ? N4 Lu1 C3 108.7(2) . . ? N5 Lu1 C3 119.5(2) . . ? N6 Lu1 C3 87.8(2) . . ? N3 Lu1 C3 147.9(2) . . ? C5 Lu1 C3 52.2(2) . . ? C1 Lu1 C3 52.4(2) . . ? C4 Lu1 C3 31.5(2) . . ? C2 Lu1 C3 30.6(2) . . ? N4 Lu1 Lu3 41.85(12) . . ? N5 Lu1 Lu3 85.52(13) . . ? N6 Lu1 Lu3 85.94(12) . . ? N3 Lu1 Lu3 42.80(13) . . ? C5 Lu1 Lu3 147.43(16) . . ? C1 Lu1 Lu3 127.35(15) . . ? C4 Lu1 Lu3 178.05(18) . . ? C2 Lu1 Lu3 129.54(16) . . ? C3 Lu1 Lu3 150.43(17) . . ? N4 Lu1 Lu2 86.16(13) . . ? N5 Lu1 Lu2 42.26(13) . . ? N6 Lu1 Lu2 42.13(12) . . ? N3 Lu1 Lu2 85.05(13) . . ? C5 Lu1 Lu2 135.40(16) . . ? C1 Lu1 Lu2 167.61(16) . . ? C4 Lu1 Lu2 119.00(16) . . ? C2 Lu1 Lu2 153.54(16) . . ? C3 Lu1 Lu2 127.00(16) . . ? Lu3 Lu1 Lu2 60.450(14) . . ? N2 Lu2 N6 80.95(19) . . ? N2 Lu2 N5 121.79(19) . . ? N6 Lu2 N5 71.42(19) . . ? N2 Lu2 N1 71.99(19) . . ? N6 Lu2 N1 123.19(18) . . ? N5 Lu2 N1 81.93(19) . . ? N2 Lu2 C14 126.3(2) . . ? N6 Lu2 C14 141.66(19) . . ? N5 Lu2 C14 105.7(2) . . ? N1 Lu2 C14 93.1(2) . . ? N2 Lu2 C13 139.6(2) . . ? N6 Lu2 C13 109.61(19) . . ? N5 Lu2 C13 98.2(2) . . ? N1 Lu2 C13 123.48(19) . . ? C14 Lu2 C13 32.06(18) . . ? N2 Lu2 C17 110.5(2) . . ? N6 Lu2 C17 95.41(19) . . ? N5 Lu2 C17 122.0(2) . . ? N1 Lu2 C17 140.55(19) . . ? C14 Lu2 C17 52.5(2) . . ? C13 Lu2 C17 32.2(2) . . ? N2 Lu2 C15 95.5(2) . . ? N6 Lu2 C15 143.8(2) . . ? N5 Lu2 C15 135.7(2) . . ? N1 Lu2 C15 88.8(2) . . ? C14 Lu2 C15 31.3(2) . . ? C13 Lu2 C15 52.5(2) . . ? C17 Lu2 C15 51.9(2) . . ? N2 Lu2 C16 86.9(2) . . ? N6 Lu2 C16 112.2(2) . . ? N5 Lu2 C16 150.8(2) . . ? N1 Lu2 C16 115.0(2) . . ? C14 Lu2 C16 52.5(2) . . ? C13 Lu2 C16 52.8(2) . . ? C17 Lu2 C16 31.1(2) . . ? C15 Lu2 C16 31.7(2) . . ? N2 Lu2 Lu1 83.67(13) . . ? N6 Lu2 Lu1 42.60(14) . . ? N5 Lu2 Lu1 42.01(13) . . ? N1 Lu2 Lu1 84.71(13) . . ? C14 Lu2 Lu1 147.69(15) . . ? C13 Lu2 Lu1 130.96(15) . . ? C17 Lu2 Lu1 134.49(15) . . ? C15 Lu2 Lu1 173.42(16) . . ? C16 Lu2 Lu1 154.24(17) . . ? N2 Lu2 Lu3 42.16(14) . . ? N6 Lu2 Lu3 85.51(12) . . ? N5 Lu2 Lu3 84.62(13) . . ? N1 Lu2 Lu3 41.84(13) . . ? C14 Lu2 Lu3 132.80(15) . . ? C13 Lu2 Lu3 164.77(14) . . ? C17 Lu2 Lu3 152.31(17) . . ? C15 Lu2 Lu3 115.84(16) . . ? C16 Lu2 Lu3 124.12(15) . . ? Lu1 Lu2 Lu3 59.533(13) . . ? N4 Lu3 N1 123.24(17) . . ? N4 Lu3 N3 71.88(19) . . ? N1 Lu3 N3 81.14(19) . . ? N4 Lu3 N2 81.84(19) . . ? N1 Lu3 N2 71.6(2) . . ? N3 Lu3 N2 121.96(18) . . ? N4 Lu3 C25 139.44(19) . . ? N1 Lu3 C25 97.02(18) . . ? N3 Lu3 C25 114.1(2) . . ? N2 Lu3 C25 119.3(2) . . ? N4 Lu3 C26 127.2(2) . . ? N1 Lu3 C26 103.1(2) . . ? N3 Lu3 C26 145.5(2) . . ? N2 Lu3 C26 91.2(2) . . ? C25 Lu3 C26 31.8(2) . . ? N4 Lu3 C27 96.1(2) . . ? N1 Lu3 C27 132.7(2) . . ? N3 Lu3 C27 140.8(2) . . ? N2 Lu3 C27 91.6(2) . . ? C25 Lu3 C27 52.6(2) . . ? C26 Lu3 C27 31.4(2) . . ? N4 Lu3 C29 109.58(19) . . ? N1 Lu3 C29 122.39(19) . . ? N3 Lu3 C29 96.0(2) . . ? N2 Lu3 C29 141.9(2) . . ? C25 Lu3 C29 32.52(19) . . ? C26 Lu3 C29 52.5(2) . . ? C27 Lu3 C29 51.9(2) . . ? N4 Lu3 C28 87.31(18) . . ? N1 Lu3 C28 149.39(18) . . ? N3 Lu3 C28 110.0(2) . . ? N2 Lu3 C28 119.6(2) . . ? C25 Lu3 C28 52.38(19) . . ? C26 Lu3 C28 51.5(2) . . ? C27 Lu3 C28 30.9(2) . . ? C29 Lu3 C28 31.07(19) . . ? N4 Lu3 Lu1 41.73(13) . . ? N1 Lu3 Lu1 85.25(12) . . ? N3 Lu3 Lu1 43.06(13) . . ? N2 Lu3 Lu1 83.63(12) . . ? C25 Lu3 Lu1 156.58(16) . . ? C26 Lu3 Lu1 168.26(16) . . ? C27 Lu3 Lu1 137.86(15) . . ? C29 Lu3 Lu1 129.50(14) . . ? C28 Lu3 Lu1 122.75(14) . . ? N4 Lu3 Lu2 85.72(13) . . ? N1 Lu3 Lu2 42.06(13) . . ? N3 Lu3 Lu2 84.88(13) . . ? N2 Lu3 Lu2 41.48(13) . . ? C25 Lu3 Lu2 133.68(14) . . ? C26 Lu3 Lu2 121.40(16) . . ? C27 Lu3 Lu2 132.49(16) . . ? C29 Lu3 Lu2 164.20(14) . . ? C28 Lu3 Lu2 160.67(16) . . ? Lu1 Lu3 Lu2 60.017(8) . . ? Lu3 N1 Lu2 96.09(19) . . ? Lu2 N2 Lu3 96.4(2) . . ? Lu3 N3 Lu1 94.1(2) . . ? Lu1 N4 Lu3 96.42(19) . . ? Lu1 N5 Lu2 95.73(19) . . ? Lu2 N6 Lu1 95.28(19) . . ? C10 Si1 C11 108.3(4) . . ? C10 Si1 C1 112.6(4) . . ? C11 Si1 C1 108.3(3) . . ? C10 Si1 C12 106.6(4) . . ? C11 Si1 C12 105.8(4) . . ? C1 Si1 C12 114.8(3) . . ? C22 Si2 C24 106.7(5) . . ? C22 Si2 C23 108.9(4) . . ? C24 Si2 C23 105.3(4) . . ? C22 Si2 C13 108.1(4) . . ? C24 Si2 C13 114.2(4) . . ? C23 Si2 C13 113.4(4) . . ? C35 Si3 C34 107.1(4) . . ? C35 Si3 C36 106.7(4) . . ? C34 Si3 C36 107.1(4) . . ? C35 Si3 C25 109.5(3) . . ? C34 Si3 C25 112.6(3) . . ? C36 Si3 C25 113.5(4) . . ? C5 C1 C2 106.3(6) . . ? C5 C1 Si1 130.1(5) . . ? C2 C1 Si1 122.8(6) . . ? C5 C1 Lu1 73.0(4) . . ? C2 C1 Lu1 76.0(4) . . ? Si1 C1 Lu1 124.5(3) . . ? C3 C2 C1 108.4(7) . . ? C3 C2 C6 124.0(7) . . ? C1 C2 C6 127.5(7) . . ? C3 C2 Lu1 75.4(4) . . ? C1 C2 Lu1 71.7(4) . . ? C6 C2 Lu1 122.1(4) . . ? C2 C3 C4 108.6(7) . . ? C2 C3 C7 125.0(7) . . ? C4 C3 C7 126.3(7) . . ? C2 C3 Lu1 73.9(4) . . ? C4 C3 Lu1 72.8(4) . . ? C7 C3 Lu1 121.8(4) . . ? C5 C4 C3 108.1(6) . . ? C5 C4 C8 126.2(7) . . ? C3 C4 C8 125.6(7) . . ? C5 C4 Lu1 72.1(4) . . ? C3 C4 Lu1 75.7(4) . . ? C8 C4 Lu1 120.0(5) . . ? C4 C5 C1 108.6(6) . . ? C4 C5 C9 124.6(7) . . ? C1 C5 C9 126.7(7) . . ? C4 C5 Lu1 76.5(4) . . ? C1 C5 Lu1 74.4(4) . . ? C9 C5 Lu1 117.2(4) . . ? C14 C13 C17 106.3(6) . . ? C14 C13 Si2 126.6(5) . . ? C17 C13 Si2 126.3(5) . . ? C14 C13 Lu2 73.8(3) . . ? C17 C13 Lu2 74.6(4) . . ? Si2 C13 Lu2 124.9(3) . . ? C15 C14 C13 108.7(6) . . ? C15 C14 C18 124.2(6) . . ? C13 C14 C18 127.1(6) . . ? C15 C14 Lu2 75.4(4) . . ? C13 C14 Lu2 74.1(3) . . ? C18 C14 Lu2 117.8(4) . . ? C14 C15 C16 108.5(6) . . ? C14 C15 C19 127.7(7) . . ? C16 C15 C19 123.8(6) . . ? C14 C15 Lu2 73.2(4) . . ? C16 C15 Lu2 74.5(4) . . ? C19 C15 Lu2 120.7(5) . . ? C17 C16 C15 107.4(6) . . ? C17 C16 C20 126.2(7) . . ? C15 C16 C20 126.3(7) . . ? C17 C16 Lu2 73.9(4) . . ? C15 C16 Lu2 73.8(4) . . ? C20 C16 Lu2 122.1(5) . . ? C16 C17 C13 109.2(6) . . ? C16 C17 C21 123.0(7) . . ? C13 C17 C21 127.5(7) . . ? C16 C17 Lu2 75.0(4) . . ? C13 C17 Lu2 73.2(4) . . ? C21 C17 Lu2 123.2(4) . . ? C26 C25 C29 106.6(6) . . ? C26 C25 Si3 130.3(5) . . ? C29 C25 Si3 122.7(5) . . ? C26 C25 Lu3 74.5(4) . . ? C29 C25 Lu3 75.4(3) . . ? Si3 C25 Lu3 121.6(3) . . ? C27 C26 C25 109.0(6) . . ? C27 C26 C30 123.8(7) . . ? C25 C26 C30 127.2(7) . . ? C27 C26 Lu3 75.4(4) . . ? C25 C26 Lu3 73.6(4) . . ? C30 C26 Lu3 118.3(5) . . ? C28 C27 C26 108.0(6) . . ? C28 C27 C31 125.6(7) . . ? C26 C27 C31 126.4(7) . . ? C28 C27 Lu3 75.6(4) . . ? C26 C27 Lu3 73.2(4) . . ? C31 C27 Lu3 117.5(4) . . ? C27 C28 C29 109.4(6) . . ? C27 C28 C32 125.6(7) . . ? C29 C28 C32 124.8(7) . . ? C27 C28 Lu3 73.5(4) . . ? C29 C28 Lu3 73.6(4) . . ? C32 C28 Lu3 123.1(4) . . ? C28 C29 C25 107.0(6) . . ? C28 C29 C33 125.3(6) . . ? C25 C29 C33 127.5(6) . . ? C28 C29 Lu3 75.3(4) . . ? C25 C29 Lu3 72.1(3) . . ? C33 C29 Lu3 121.2(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.704 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.153 data_4Lu _database_code_depnum_ccdc_archive 'CCDC 767213' #TrackingRef '- DT-ART-02-2010-00006.cif' _database_code_depnum_ccdc_archive 'CCDC 767213' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H100 Lu4 N8 Si4' _chemical_formula_weight 1601.60 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0949(17) _cell_length_b 13.1788(17) _cell_length_c 18.228(2) _cell_angle_alpha 91.212(2) _cell_angle_beta 91.112(2) _cell_angle_gamma 99.820(2) _cell_volume 3098.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 20668 _cell_measurement_theta_min 1.58 _cell_measurement_theta_max 27.58 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 6.430 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2486 _exptl_absorpt_correction_T_max 0.3595 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 20668 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_sigmaI/netI 0.1042 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.58 _reflns_number_total 13508 _reflns_number_gt 9741 _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 'ORTEP-III (Farrugia, 1997)' _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^)+(0.0616P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13508 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1341 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.185 _refine_ls_shift/su_mean 0.002 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 0.76275(3) 0.81876(3) 0.35036(2) 0.02108(10) Uani 1 1 d . . . Lu2 Lu 0.74775(3) 0.83568(3) 0.16365(2) 0.02024(10) Uani 1 1 d . . . Lu3 Lu 0.68725(3) 0.53645(3) 0.23937(2) 0.02103(10) Uani 1 1 d . . . Lu4 Lu 0.48549(3) 0.67001(3) 0.25677(2) 0.02112(10) Uani 1 1 d . . . N1 N 0.7184(6) 0.9350(6) 0.2669(4) 0.0246(18) Uani 1 1 d . . . H1A H 0.7619 0.9977 0.2698 0.030 Uiso 1 1 calc R . . H1B H 0.6504 0.9439 0.2700 0.030 Uiso 1 1 calc R . . N2 N 0.8769(6) 0.8307(6) 0.2529(4) 0.0256(18) Uani 1 1 d . . . H2A H 0.9257 0.8899 0.2552 0.031 Uiso 1 1 calc R . . H2B H 0.9085 0.7738 0.2478 0.031 Uiso 1 1 calc R . . N3 N 0.7611(6) 0.6611(6) 0.1592(4) 0.0245(18) Uani 1 1 d . . . H3A H 0.7373 0.6374 0.1131 0.029 Uiso 1 1 calc R . . H3B H 0.8310 0.6591 0.1606 0.029 Uiso 1 1 calc R . . N4 N 0.5697(6) 0.7816(6) 0.1719(4) 0.0253(18) Uani 1 1 d . . . H4A H 0.5418 0.8410 0.1765 0.030 Uiso 1 1 calc R . . H4B H 0.5479 0.7531 0.1266 0.030 Uiso 1 1 calc R . . N5 N 0.7702(7) 0.6457(6) 0.3340(4) 0.0287(19) Uani 1 1 d . . . H5A H 0.7478 0.6151 0.3771 0.034 Uiso 1 1 calc R . . H5B H 0.8395 0.6417 0.3313 0.034 Uiso 1 1 calc R . . N6 N 0.5821(6) 0.7729(7) 0.3474(4) 0.0269(19) Uani 1 1 d . . . H6A H 0.5649 0.7414 0.3912 0.032 Uiso 1 1 calc R . . H6B H 0.5566 0.8337 0.3488 0.032 Uiso 1 1 calc R . . N7 N 0.5375(6) 0.5520(6) 0.1733(5) 0.0261(18) Uani 1 1 d . . . H7A H 0.4913 0.4911 0.1692 0.031 Uiso 1 1 calc R . . H7B H 0.5510 0.5790 0.1277 0.031 Uiso 1 1 calc R . . N8 N 0.5502(6) 0.5408(6) 0.3186(4) 0.0274(18) Uani 1 1 d . . . H8A H 0.5041 0.4797 0.3184 0.033 Uiso 1 1 calc R . . H8B H 0.5721 0.5603 0.3659 0.033 Uiso 1 1 calc R . . Si1 Si 0.6602(2) 0.8151(2) 0.55478(14) 0.0272(6) Uani 1 1 d . . . Si2 Si 0.7718(2) 0.7526(2) -0.04342(15) 0.0271(6) Uani 1 1 d . . . Si3 Si 0.9409(2) 0.4329(3) 0.3024(2) 0.0416(8) Uani 1 1 d . . . Si4 Si 0.2957(2) 0.8651(2) 0.19887(16) 0.0288(6) Uani 1 1 d . . . C1 C 0.7635(7) 0.8594(7) 0.4902(5) 0.0210(19) Uani 1 1 d . . . C2 C 0.7896(8) 0.9563(7) 0.4548(5) 0.024(2) Uani 1 1 d . . . C3 C 0.8879(8) 0.9641(9) 0.4229(5) 0.036(3) Uani 1 1 d . . . C4 C 0.9263(8) 0.8705(9) 0.4396(5) 0.030(2) Uani 1 1 d . . . C5 C 0.8532(7) 0.8077(8) 0.4799(5) 0.030(2) Uani 1 1 d . . . C6 C 0.7250(10) 1.0410(9) 0.4496(6) 0.043(3) Uani 1 1 d . . . H6C H 0.7486 1.0854 0.4087 0.065 Uiso 1 1 calc R . . H6D H 0.7326 1.0820 0.4954 0.065 Uiso 1 1 calc R . . H6E H 0.6520 1.0103 0.4413 0.065 Uiso 1 1 calc R . . C7 C 0.9466(9) 1.0541(10) 0.3852(6) 0.051(3) Uani 1 1 d . . . H7C H 0.9071 1.1110 0.3866 0.076 Uiso 1 1 calc R . . H7D H 0.9573 1.0349 0.3341 0.076 Uiso 1 1 calc R . . H7E H 1.0139 1.0759 0.4103 0.076 Uiso 1 1 calc R . . C8 C 1.0319(8) 0.8471(11) 0.4196(6) 0.052(4) Uani 1 1 d . . . H8C H 1.0753 0.8488 0.4642 0.078 Uiso 1 1 calc R . . H8D H 1.0649 0.8987 0.3857 0.078 Uiso 1 1 calc R . . H8E H 1.0237 0.7785 0.3961 0.078 Uiso 1 1 calc R . . C9 C 0.8668(9) 0.7076(9) 0.5128(6) 0.041(3) Uani 1 1 d . . . H9A H 0.9038 0.6692 0.4786 0.061 Uiso 1 1 calc R . . H9B H 0.7986 0.6669 0.5223 0.061 Uiso 1 1 calc R . . H9C H 0.9069 0.7210 0.5590 0.061 Uiso 1 1 calc R . . C10 C 0.5919(9) 0.6782(8) 0.5347(6) 0.040(3) Uani 1 1 d . . . H10A H 0.5332 0.6791 0.5006 0.060 Uiso 1 1 calc R . . H10B H 0.5665 0.6466 0.5806 0.060 Uiso 1 1 calc R . . H10C H 0.6405 0.6383 0.5126 0.060 Uiso 1 1 calc R . . C11 C 0.7209(10) 0.8220(11) 0.6487(6) 0.051(3) Uani 1 1 d . . . H11A H 0.7732 0.7770 0.6503 0.077 Uiso 1 1 calc R . . H11B H 0.6674 0.7994 0.6845 0.077 Uiso 1 1 calc R . . H11C H 0.7538 0.8931 0.6605 0.077 Uiso 1 1 calc R . . C12 C 0.5561(9) 0.8958(10) 0.5586(7) 0.050(3) Uani 1 1 d . . . H12A H 0.5871 0.9675 0.5700 0.075 Uiso 1 1 calc R . . H12B H 0.5071 0.8704 0.5967 0.075 Uiso 1 1 calc R . . H12C H 0.5194 0.8917 0.5109 0.075 Uiso 1 1 calc R . . C13 C 0.7858(7) 0.8595(7) 0.0267(5) 0.0194(19) Uani 1 1 d . . . C14 C 0.8761(7) 0.9116(8) 0.0648(5) 0.029(2) Uani 1 1 d . . . C15 C 0.8526(8) 0.9977(8) 0.1017(6) 0.033(2) Uani 1 1 d . . . C16 C 0.7473(9) 1.0033(8) 0.0875(5) 0.032(2) Uani 1 1 d . . . C17 C 0.7059(8) 0.9206(8) 0.0402(5) 0.028(2) Uani 1 1 d . . . C18 C 0.9827(8) 0.8812(11) 0.0658(6) 0.048(3) Uani 1 1 d . . . H18A H 0.9769 0.8093 0.0803 0.072 Uiso 1 1 calc R . . H18B H 1.0281 0.9257 0.1011 0.072 Uiso 1 1 calc R . . H18C H 1.0119 0.8890 0.0168 0.072 Uiso 1 1 calc R . . C19 C 0.9272(10) 1.0753(10) 0.1474(6) 0.053(3) Uani 1 1 d . . . H19A H 0.9809 1.0413 0.1693 0.080 Uiso 1 1 calc R . . H19B H 0.8894 1.1042 0.1864 0.080 Uiso 1 1 calc R . . H19C H 0.9594 1.1308 0.1161 0.080 Uiso 1 1 calc R . . C20 C 0.6921(12) 1.0896(9) 0.1119(7) 0.059(4) Uani 1 1 d . . . H20A H 0.7122 1.1493 0.0809 0.089 Uiso 1 1 calc R . . H20B H 0.7113 1.1091 0.1631 0.089 Uiso 1 1 calc R . . H20C H 0.6170 1.0665 0.1075 0.089 Uiso 1 1 calc R . . C21 C 0.5992(8) 0.9047(10) 0.0054(6) 0.042(3) Uani 1 1 d . . . H21A H 0.5574 0.9493 0.0303 0.064 Uiso 1 1 calc R . . H21B H 0.5664 0.8325 0.0099 0.064 Uiso 1 1 calc R . . H21C H 0.6043 0.9217 -0.0466 0.064 Uiso 1 1 calc R . . C22 C 0.6523(8) 0.6522(9) -0.0295(6) 0.039(3) Uani 1 1 d . . . H22A H 0.6703 0.5980 0.0018 0.058 Uiso 1 1 calc R . . H22B H 0.6257 0.6220 -0.0772 0.058 Uiso 1 1 calc R . . H22C H 0.5989 0.6846 -0.0059 0.058 Uiso 1 1 calc R . . C23 C 0.8809(9) 0.6777(9) -0.0437(7) 0.045(3) Uani 1 1 d . . . H23A H 0.9442 0.7218 -0.0595 0.067 Uiso 1 1 calc R . . H23B H 0.8637 0.6182 -0.0776 0.067 Uiso 1 1 calc R . . H23C H 0.8921 0.6537 0.0059 0.067 Uiso 1 1 calc R . . C24 C 0.7623(9) 0.8073(8) -0.1365(5) 0.040(3) Uani 1 1 d . . . H24A H 0.6974 0.8345 -0.1412 0.060 Uiso 1 1 calc R . . H24B H 0.7632 0.7531 -0.1740 0.060 Uiso 1 1 calc R . . H24C H 0.8211 0.8629 -0.1431 0.060 Uiso 1 1 calc R . . C25 C 0.8126(7) 0.4053(8) 0.2537(5) 0.028(2) Uani 1 1 d . . . C26 C 0.7173(8) 0.3567(8) 0.2824(6) 0.030(2) Uani 1 1 d . . . C27 C 0.6435(8) 0.3342(7) 0.2215(6) 0.033(2) Uani 1 1 d . . . C28 C 0.6954(8) 0.3707(8) 0.1570(6) 0.036(3) Uani 1 1 d . . . C29 C 0.7973(8) 0.4115(8) 0.1767(6) 0.031(2) Uani 1 1 d . . . C30 C 0.6911(10) 0.3284(10) 0.3597(7) 0.055(4) Uani 1 1 d . . . H30A H 0.7050 0.2588 0.3685 0.082 Uiso 1 1 calc R . . H30B H 0.6176 0.3301 0.3675 0.082 Uiso 1 1 calc R . . H30C H 0.7335 0.3775 0.3937 0.082 Uiso 1 1 calc R . . C31 C 0.5342(9) 0.2797(10) 0.2244(10) 0.070(5) Uani 1 1 d . . . H31A H 0.4898 0.3151 0.1936 0.105 Uiso 1 1 calc R . . H31B H 0.5109 0.2798 0.2752 0.105 Uiso 1 1 calc R . . H31C H 0.5299 0.2085 0.2063 0.105 Uiso 1 1 calc R . . C32 C 0.6469(11) 0.3566(11) 0.0817(7) 0.061(4) Uani 1 1 d . . . H32A H 0.6910 0.3994 0.0474 0.092 Uiso 1 1 calc R . . H32B H 0.5784 0.3771 0.0823 0.092 Uiso 1 1 calc R . . H32C H 0.6396 0.2840 0.0661 0.092 Uiso 1 1 calc R . . C33 C 0.8809(10) 0.4475(9) 0.1206(7) 0.050(3) Uani 1 1 d . . . H33A H 0.9119 0.3887 0.1038 0.075 Uiso 1 1 calc R . . H33B H 0.9348 0.4999 0.1436 0.075 Uiso 1 1 calc R . . H33C H 0.8495 0.4769 0.0786 0.075 Uiso 1 1 calc R . . C34 C 1.0215(10) 0.5568(11) 0.2736(10) 0.079(5) Uani 1 1 d . . . H34A H 1.0206 0.5597 0.2199 0.118 Uiso 1 1 calc R . . H34B H 1.0930 0.5604 0.2918 0.118 Uiso 1 1 calc R . . H34C H 0.9929 0.6151 0.2941 0.118 Uiso 1 1 calc R . . C35 C 0.9349(12) 0.4406(13) 0.4050(7) 0.082(6) Uani 1 1 d . . . H35A H 0.8958 0.4947 0.4193 0.122 Uiso 1 1 calc R . . H35B H 1.0053 0.4569 0.4261 0.122 Uiso 1 1 calc R . . H35C H 0.9003 0.3743 0.4231 0.122 Uiso 1 1 calc R . . C36 C 1.0097(9) 0.3218(10) 0.2786(7) 0.051(3) Uani 1 1 d . . . H36A H 0.9653 0.2567 0.2903 0.076 Uiso 1 1 calc R . . H36B H 1.0748 0.3290 0.3072 0.076 Uiso 1 1 calc R . . H36C H 1.0244 0.3222 0.2261 0.076 Uiso 1 1 calc R . . C37 C 0.3127(7) 0.7403(7) 0.2374(5) 0.024(2) Uani 1 1 d . . . C38 C 0.3168(7) 0.7208(7) 0.3146(5) 0.023(2) Uani 1 1 d . . . C39 C 0.3109(7) 0.6153(8) 0.3265(6) 0.029(2) Uani 1 1 d . . . C40 C 0.2968(7) 0.5642(8) 0.2561(6) 0.033(2) Uani 1 1 d . . . C41 C 0.2993(8) 0.6392(8) 0.2019(5) 0.027(2) Uani 1 1 d . . . C42 C 0.3234(8) 0.8018(10) 0.3762(6) 0.040(3) Uani 1 1 d . . . H42A H 0.2536 0.8144 0.3871 0.060 Uiso 1 1 calc R . . H42B H 0.3661 0.8659 0.3609 0.060 Uiso 1 1 calc R . . H42C H 0.3547 0.7771 0.4202 0.060 Uiso 1 1 calc R . . C43 C 0.3049(10) 0.5642(11) 0.3999(7) 0.053(3) Uani 1 1 d . . . H43A H 0.3704 0.5855 0.4273 0.079 Uiso 1 1 calc R . . H43B H 0.2923 0.4892 0.3923 0.079 Uiso 1 1 calc R . . H43C H 0.2481 0.5847 0.4277 0.079 Uiso 1 1 calc R . . C44 C 0.2823(9) 0.4483(9) 0.2455(9) 0.063(4) Uani 1 1 d . . . H44A H 0.2128 0.4227 0.2248 0.095 Uiso 1 1 calc R . . H44B H 0.2904 0.4166 0.2929 0.095 Uiso 1 1 calc R . . H44C H 0.3344 0.4307 0.2118 0.095 Uiso 1 1 calc R . . C45 C 0.2860(9) 0.6120(9) 0.1214(6) 0.047(3) Uani 1 1 d . . . H45A H 0.3210 0.5537 0.1101 0.071 Uiso 1 1 calc R . . H45B H 0.3164 0.6714 0.0929 0.071 Uiso 1 1 calc R . . H45C H 0.2120 0.5932 0.1087 0.071 Uiso 1 1 calc R . . C46 C 0.1749(9) 0.9023(9) 0.2375(6) 0.042(3) Uani 1 1 d . . . H46A H 0.1146 0.8515 0.2215 0.062 Uiso 1 1 calc R . . H46B H 0.1669 0.9704 0.2200 0.062 Uiso 1 1 calc R . . H46C H 0.1803 0.9046 0.2913 0.062 Uiso 1 1 calc R . . C47 C 0.2797(10) 0.8600(10) 0.0975(6) 0.046(3) Uani 1 1 d . . . H47A H 0.3475 0.8618 0.0752 0.070 Uiso 1 1 calc R . . H47B H 0.2497 0.9193 0.0815 0.070 Uiso 1 1 calc R . . H47C H 0.2336 0.7962 0.0822 0.070 Uiso 1 1 calc R . . C48 C 0.4075(9) 0.9729(9) 0.2231(7) 0.047(3) Uani 1 1 d . . . H48A H 0.4399 0.9585 0.2698 0.070 Uiso 1 1 calc R . . H48B H 0.3816 1.0382 0.2277 0.070 Uiso 1 1 calc R . . H48C H 0.4589 0.9778 0.1844 0.070 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 0.0218(2) 0.0237(2) 0.01619(19) -0.00446(15) -0.00328(15) 0.00043(16) Lu2 0.0233(2) 0.0203(2) 0.01612(19) -0.00176(15) -0.00059(15) 0.00102(16) Lu3 0.0209(2) 0.0199(2) 0.0224(2) -0.00282(15) -0.00196(15) 0.00440(16) Lu4 0.01813(19) 0.0224(2) 0.0224(2) -0.00286(16) -0.00119(15) 0.00298(16) N1 0.025(4) 0.012(4) 0.034(5) -0.006(3) 0.003(3) -0.003(3) N2 0.029(4) 0.023(4) 0.025(4) -0.004(3) -0.004(3) 0.006(4) N3 0.025(4) 0.024(4) 0.024(4) -0.007(3) -0.004(3) 0.004(3) N4 0.023(4) 0.031(5) 0.022(4) -0.012(3) -0.005(3) 0.006(4) N5 0.043(5) 0.024(5) 0.022(4) -0.008(3) -0.006(4) 0.014(4) N6 0.018(4) 0.040(5) 0.023(4) -0.010(4) -0.003(3) 0.007(4) N7 0.020(4) 0.022(4) 0.036(5) -0.007(4) -0.006(3) 0.003(3) N8 0.029(4) 0.029(5) 0.019(4) 0.000(3) 0.002(3) -0.008(4) Si1 0.0303(15) 0.0334(16) 0.0181(13) 0.0004(11) 0.0026(11) 0.0059(12) Si2 0.0318(15) 0.0294(16) 0.0199(13) -0.0042(11) -0.0024(11) 0.0051(12) Si3 0.0290(16) 0.0358(18) 0.061(2) -0.0100(16) -0.0184(15) 0.0125(14) Si4 0.0256(14) 0.0307(16) 0.0315(16) 0.0029(12) -0.0006(12) 0.0090(12) C1 0.023(5) 0.026(5) 0.013(4) -0.006(4) 0.000(3) 0.004(4) C2 0.034(5) 0.023(5) 0.012(4) -0.003(4) -0.001(4) -0.005(4) C3 0.043(6) 0.042(7) 0.015(5) -0.013(4) 0.005(4) -0.016(5) C4 0.027(5) 0.042(6) 0.020(5) -0.002(4) -0.008(4) 0.004(5) C5 0.023(5) 0.044(7) 0.023(5) -0.002(5) -0.005(4) 0.004(5) C6 0.063(8) 0.036(7) 0.032(6) -0.002(5) 0.004(6) 0.015(6) C7 0.053(8) 0.060(9) 0.030(6) -0.011(6) -0.002(5) -0.018(6) C8 0.032(6) 0.094(11) 0.025(6) -0.023(6) -0.004(5) -0.001(6) C9 0.043(7) 0.052(8) 0.032(6) -0.002(5) -0.015(5) 0.022(6) C10 0.046(7) 0.038(7) 0.039(7) 0.010(5) -0.001(5) 0.013(5) C11 0.057(8) 0.070(9) 0.025(6) -0.002(6) 0.004(5) 0.004(7) C12 0.042(7) 0.050(8) 0.059(8) 0.000(6) 0.010(6) 0.012(6) C13 0.023(5) 0.016(5) 0.018(4) -0.002(3) -0.002(4) 0.001(4) C14 0.022(5) 0.043(6) 0.020(5) 0.006(4) 0.002(4) -0.002(4) C15 0.037(6) 0.030(6) 0.026(5) 0.000(4) 0.003(4) -0.009(5) C16 0.048(7) 0.025(6) 0.023(5) 0.003(4) 0.003(5) 0.006(5) C17 0.035(6) 0.030(6) 0.019(5) 0.007(4) -0.004(4) 0.009(5) C18 0.026(6) 0.089(10) 0.025(6) 0.001(6) -0.002(5) -0.001(6) C19 0.067(9) 0.048(8) 0.033(7) -0.003(6) -0.004(6) -0.021(7) C20 0.104(12) 0.036(7) 0.045(8) -0.007(6) 0.015(8) 0.032(8) C21 0.031(6) 0.069(9) 0.033(6) 0.004(6) -0.001(5) 0.023(6) C22 0.042(6) 0.036(6) 0.033(6) -0.004(5) -0.009(5) -0.008(5) C23 0.040(7) 0.035(7) 0.063(8) -0.008(6) 0.001(6) 0.019(5) C24 0.063(8) 0.028(6) 0.026(6) 0.001(5) -0.005(5) 0.002(6) C25 0.026(5) 0.027(6) 0.031(5) 0.001(4) -0.005(4) 0.007(4) C26 0.039(6) 0.023(5) 0.032(6) 0.002(4) 0.002(5) 0.014(5) C27 0.031(6) 0.011(5) 0.056(7) -0.007(4) -0.011(5) 0.003(4) C28 0.039(6) 0.030(6) 0.041(6) -0.014(5) -0.012(5) 0.011(5) C29 0.027(5) 0.024(5) 0.041(6) 0.003(4) -0.001(4) 0.008(4) C30 0.059(8) 0.051(8) 0.060(9) 0.023(7) 0.022(7) 0.022(7) C31 0.025(6) 0.031(7) 0.149(16) 0.001(8) -0.005(8) -0.005(5) C32 0.089(10) 0.060(9) 0.043(7) -0.026(7) -0.040(7) 0.041(8) C33 0.068(9) 0.037(7) 0.051(8) 0.005(6) 0.034(7) 0.022(6) C34 0.042(8) 0.046(9) 0.146(16) -0.013(9) -0.032(9) 0.010(7) C35 0.088(11) 0.110(13) 0.063(9) -0.036(9) -0.051(9) 0.073(11) C36 0.029(6) 0.053(8) 0.074(9) 0.000(7) -0.009(6) 0.019(6) C37 0.021(5) 0.020(5) 0.030(5) -0.007(4) -0.001(4) 0.004(4) C38 0.022(5) 0.028(5) 0.022(5) -0.004(4) -0.001(4) 0.011(4) C39 0.014(4) 0.035(6) 0.037(6) 0.011(5) 0.002(4) 0.005(4) C40 0.016(5) 0.035(6) 0.047(7) 0.004(5) -0.005(4) 0.007(4) C41 0.030(5) 0.026(5) 0.026(5) -0.009(4) -0.012(4) 0.008(4) C42 0.035(6) 0.066(8) 0.023(5) -0.015(5) -0.003(4) 0.021(6) C43 0.050(8) 0.060(9) 0.048(8) 0.023(6) 0.012(6) 0.005(7) C44 0.027(6) 0.032(7) 0.126(14) -0.007(8) 0.005(7) -0.008(5) C45 0.048(7) 0.046(8) 0.046(7) -0.026(6) -0.015(6) 0.010(6) C46 0.041(7) 0.043(7) 0.044(7) 0.011(5) 0.004(5) 0.016(6) C47 0.061(8) 0.046(7) 0.036(7) 0.012(5) -0.003(6) 0.018(6) C48 0.036(6) 0.032(7) 0.075(9) -0.004(6) 0.001(6) 0.012(5) _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 N5 2.313(7) . ? Lu1 N1 2.317(8) . ? Lu1 N2 2.335(8) . ? Lu1 N6 2.339(7) . ? Lu1 C2 2.578(8) . ? Lu1 C1 2.593(8) . ? Lu1 C3 2.615(9) . ? Lu1 C5 2.639(9) . ? Lu1 C4 2.649(9) . ? Lu1 Lu2 3.4195(7) . ? Lu2 N4 2.328(8) . ? Lu2 N2 2.333(7) . ? Lu2 N3 2.337(8) . ? Lu2 N1 2.344(7) . ? Lu2 C13 2.571(9) . ? Lu2 C14 2.586(10) . ? Lu2 C15 2.623(10) . ? Lu2 C17 2.624(9) . ? Lu2 C16 2.634(10) . ? Lu3 N3 2.320(8) . ? Lu3 N7 2.322(7) . ? Lu3 N8 2.334(8) . ? Lu3 N5 2.348(7) . ? Lu3 C25 2.592(9) . ? Lu3 C26 2.602(10) . ? Lu3 C29 2.625(10) . ? Lu3 C27 2.641(9) . ? Lu3 C28 2.643(10) . ? Lu3 Lu4 3.4314(6) . ? Lu4 N4 2.320(8) . ? Lu4 N6 2.325(7) . ? Lu4 N8 2.329(8) . ? Lu4 N7 2.346(7) . ? Lu4 C41 2.581(9) . ? Lu4 C37 2.608(9) . ? Lu4 C40 2.622(10) . ? Lu4 C39 2.637(10) . ? Lu4 C38 2.646(9) . ? Si1 C1 1.838(10) . ? Si1 C11 1.867(11) . ? Si1 C12 1.868(11) . ? Si1 C10 1.897(12) . ? Si2 C13 1.865(9) . ? Si2 C24 1.867(11) . ? Si2 C23 1.870(10) . ? Si2 C22 1.895(11) . ? Si3 C25 1.862(10) . ? Si3 C35 1.874(14) . ? Si3 C34 1.878(16) . ? Si3 C36 1.891(11) . ? Si4 C37 1.848(10) . ? Si4 C47 1.854(11) . ? Si4 C46 1.879(11) . ? Si4 C48 1.897(12) . ? C1 C2 1.435(13) . ? C1 C5 1.469(13) . ? C2 C3 1.412(14) . ? C2 C6 1.514(14) . ? C3 C4 1.446(15) . ? C3 C7 1.488(16) . ? C4 C5 1.388(15) . ? C4 C8 1.516(14) . ? C5 C9 1.497(15) . ? C13 C14 1.423(12) . ? C13 C17 1.447(12) . ? C14 C15 1.389(14) . ? C14 C18 1.516(14) . ? C15 C16 1.412(15) . ? C15 C19 1.511(14) . ? C16 C17 1.402(13) . ? C16 C20 1.513(14) . ? C17 C21 1.502(13) . ? C25 C26 1.417(14) . ? C25 C29 1.420(14) . ? C26 C27 1.450(14) . ? C26 C30 1.496(15) . ? C27 C28 1.422(16) . ? C27 C31 1.491(15) . ? C28 C29 1.389(14) . ? C28 C32 1.495(14) . ? C29 C33 1.534(15) . ? C37 C38 1.438(13) . ? C37 C41 1.450(12) . ? C38 C39 1.402(13) . ? C38 C42 1.524(13) . ? C39 C40 1.431(14) . ? C39 C43 1.507(15) . ? C40 C41 1.409(15) . ? C40 C44 1.513(15) . ? C41 C45 1.503(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Lu1 N1 129.5(3) . . ? N5 Lu1 N2 81.2(3) . . ? N1 Lu1 N2 70.7(3) . . ? N5 Lu1 N6 87.5(3) . . ? N1 Lu1 N6 79.4(3) . . ? N2 Lu1 N6 128.8(3) . . ? N5 Lu1 C2 138.4(3) . . ? N1 Lu1 C2 92.0(3) . . ? N2 Lu1 C2 120.2(3) . . ? N6 Lu1 C2 101.0(3) . . ? N5 Lu1 C1 108.1(3) . . ? N1 Lu1 C1 120.5(3) . . ? N2 Lu1 C1 139.9(3) . . ? N6 Lu1 C1 91.1(3) . . ? C2 Lu1 C1 32.2(3) . . ? N5 Lu1 C3 130.3(3) . . ? N1 Lu1 C3 91.8(3) . . ? N2 Lu1 C3 90.4(3) . . ? N6 Lu1 C3 131.9(3) . . ? C2 Lu1 C3 31.6(3) . . ? C1 Lu1 C3 53.2(3) . . ? N5 Lu1 C5 87.0(3) . . ? N1 Lu1 C5 142.5(3) . . ? N2 Lu1 C5 113.8(3) . . ? N6 Lu1 C5 115.3(3) . . ? C2 Lu1 C5 52.5(3) . . ? C1 Lu1 C5 32.6(3) . . ? C3 Lu1 C5 52.1(3) . . ? N5 Lu1 C4 98.6(3) . . ? N1 Lu1 C4 120.5(3) . . ? N2 Lu1 C4 87.8(3) . . ? N6 Lu1 C4 143.4(3) . . ? C2 Lu1 C4 52.0(3) . . ? C1 Lu1 C4 52.6(3) . . ? C3 Lu1 C4 31.9(3) . . ? C5 Lu1 C4 30.4(3) . . ? N5 Lu1 Lu2 88.18(19) . . ? N1 Lu1 Lu2 43.12(18) . . ? N2 Lu1 Lu2 42.88(18) . . ? N6 Lu1 Lu2 87.26(19) . . ? C2 Lu1 Lu2 132.4(2) . . ? C1 Lu1 Lu2 163.5(2) . . ? C3 Lu1 Lu2 117.6(2) . . ? C5 Lu1 Lu2 156.7(2) . . ? C4 Lu1 Lu2 128.8(2) . . ? N4 Lu2 N2 128.5(3) . . ? N4 Lu2 N3 86.6(3) . . ? N2 Lu2 N3 78.8(3) . . ? N4 Lu2 N1 81.2(3) . . ? N2 Lu2 N1 70.2(3) . . ? N3 Lu2 N1 127.5(3) . . ? N4 Lu2 C13 106.8(3) . . ? N2 Lu2 C13 123.1(3) . . ? N3 Lu2 C13 93.4(3) . . ? N1 Lu2 C13 139.0(3) . . ? N4 Lu2 C14 137.2(3) . . ? N2 Lu2 C14 94.3(3) . . ? N3 Lu2 C14 102.5(3) . . ? N1 Lu2 C14 120.7(3) . . ? C13 Lu2 C14 32.0(3) . . ? N4 Lu2 C15 130.4(3) . . ? N2 Lu2 C15 93.2(3) . . ? N3 Lu2 C15 132.6(3) . . ? N1 Lu2 C15 91.3(3) . . ? C13 Lu2 C15 52.4(3) . . ? C14 Lu2 C15 30.9(3) . . ? N4 Lu2 C17 86.4(3) . . ? N2 Lu2 C17 143.8(3) . . ? N3 Lu2 C17 117.6(3) . . ? N1 Lu2 C17 112.4(3) . . ? C13 Lu2 C17 32.3(3) . . ? C14 Lu2 C17 52.1(3) . . ? C15 Lu2 C17 51.4(3) . . ? N4 Lu2 C16 99.2(3) . . ? N2 Lu2 C16 120.1(3) . . ? N3 Lu2 C16 145.9(3) . . ? N1 Lu2 C16 86.6(3) . . ? C13 Lu2 C16 52.6(3) . . ? C14 Lu2 C16 51.7(3) . . ? C15 Lu2 C16 31.2(3) . . ? C17 Lu2 C16 30.9(3) . . ? N4 Lu2 Lu1 87.44(19) . . ? N2 Lu2 Lu1 42.91(19) . . ? N3 Lu2 Lu1 86.33(19) . . ? N1 Lu2 Lu1 42.5(2) . . ? C13 Lu2 Lu1 165.73(19) . . ? C14 Lu2 Lu1 134.3(2) . . ? C15 Lu2 Lu1 118.8(2) . . ? C17 Lu2 Lu1 154.8(2) . . ? C16 Lu2 Lu1 127.3(2) . . ? N3 Lu3 N7 82.2(3) . . ? N3 Lu3 N8 128.7(3) . . ? N7 Lu3 N8 69.7(3) . . ? N3 Lu3 N5 86.4(3) . . ? N7 Lu3 N5 127.9(3) . . ? N8 Lu3 N5 79.1(3) . . ? N3 Lu3 C25 107.7(3) . . ? N7 Lu3 C25 138.6(3) . . ? N8 Lu3 C25 121.9(3) . . ? N5 Lu3 C25 93.2(3) . . ? N3 Lu3 C26 137.9(3) . . ? N7 Lu3 C26 120.1(3) . . ? N8 Lu3 C26 93.3(3) . . ? N5 Lu3 C26 101.8(3) . . ? C25 Lu3 C26 31.7(3) . . ? N3 Lu3 C29 87.4(3) . . ? N7 Lu3 C29 113.5(3) . . ? N8 Lu3 C29 142.8(3) . . ? N5 Lu3 C29 116.5(3) . . ? C25 Lu3 C29 31.6(3) . . ? C26 Lu3 C29 51.8(3) . . ? N3 Lu3 C27 130.0(3) . . ? N7 Lu3 C27 89.9(3) . . ? N8 Lu3 C27 93.0(3) . . ? N5 Lu3 C27 133.3(3) . . ? C25 Lu3 C27 52.4(3) . . ? C26 Lu3 C27 32.1(3) . . ? C29 Lu3 C27 51.1(3) . . ? N3 Lu3 C28 98.9(3) . . ? N7 Lu3 C28 87.0(3) . . ? N8 Lu3 C28 120.6(3) . . ? N5 Lu3 C28 145.0(3) . . ? C25 Lu3 C28 52.1(3) . . ? C26 Lu3 C28 52.4(3) . . ? C29 Lu3 C28 30.6(3) . . ? C27 Lu3 C28 31.2(3) . . ? N3 Lu3 Lu4 87.94(18) . . ? N7 Lu3 Lu4 42.95(18) . . ? N8 Lu3 Lu4 42.6(2) . . ? N5 Lu3 Lu4 86.15(19) . . ? C25 Lu3 Lu4 164.3(2) . . ? C26 Lu3 Lu4 133.3(2) . . ? C29 Lu3 Lu4 156.5(2) . . ? C27 Lu3 Lu4 118.3(2) . . ? C28 Lu3 Lu4 128.3(2) . . ? N4 Lu4 N6 87.3(3) . . ? N4 Lu4 N8 127.6(3) . . ? N6 Lu4 N8 81.8(3) . . ? N4 Lu4 N7 79.6(3) . . ? N6 Lu4 N7 129.5(3) . . ? N8 Lu4 N7 69.4(3) . . ? N4 Lu4 C41 100.4(3) . . ? N6 Lu4 C41 138.4(3) . . ? N8 Lu4 C41 121.1(3) . . ? N7 Lu4 C41 92.0(3) . . ? N4 Lu4 C37 92.0(3) . . ? N6 Lu4 C37 107.3(3) . . ? N8 Lu4 C37 140.1(3) . . ? N7 Lu4 C37 121.5(3) . . ? C41 Lu4 C37 32.5(3) . . ? N4 Lu4 C40 131.0(3) . . ? N6 Lu4 C40 131.5(3) . . ? N8 Lu4 C40 91.5(3) . . ? N7 Lu4 C40 91.0(3) . . ? C41 Lu4 C40 31.4(3) . . ? C37 Lu4 C40 52.9(3) . . ? N4 Lu4 C39 144.8(3) . . ? N6 Lu4 C39 99.9(3) . . ? N8 Lu4 C39 87.6(3) . . ? N7 Lu4 C39 118.6(3) . . ? C41 Lu4 C39 52.4(3) . . ? C37 Lu4 C39 52.9(3) . . ? C40 Lu4 C39 31.6(3) . . ? N4 Lu4 C38 116.6(3) . . ? N6 Lu4 C38 88.0(3) . . ? N8 Lu4 C38 114.0(3) . . ? N7 Lu4 C38 141.2(3) . . ? C41 Lu4 C38 51.9(3) . . ? C37 Lu4 C38 31.7(3) . . ? C40 Lu4 C38 51.2(3) . . ? C39 Lu4 C38 30.8(3) . . ? N4 Lu4 Lu3 86.25(18) . . ? N6 Lu4 Lu3 88.60(18) . . ? N8 Lu4 Lu3 42.66(19) . . ? N7 Lu4 Lu3 42.41(18) . . ? C41 Lu4 Lu3 132.3(2) . . ? C37 Lu4 Lu3 163.87(19) . . ? C40 Lu4 Lu3 117.9(2) . . ? C39 Lu4 Lu3 128.0(2) . . ? C38 Lu4 Lu3 156.6(2) . . ? Lu1 N1 Lu2 94.4(3) . . ? Lu2 N2 Lu1 94.2(3) . . ? Lu3 N3 Lu2 126.5(3) . . ? Lu4 N4 Lu2 126.8(3) . . ? Lu1 N5 Lu3 126.1(3) . . ? Lu4 N6 Lu1 125.1(3) . . ? Lu3 N7 Lu4 94.6(3) . . ? Lu4 N8 Lu3 94.8(3) . . ? C1 Si1 C11 107.6(5) . . ? C1 Si1 C12 114.5(5) . . ? C11 Si1 C12 106.4(6) . . ? C1 Si1 C10 113.3(5) . . ? C11 Si1 C10 108.8(6) . . ? C12 Si1 C10 106.0(5) . . ? C13 Si2 C24 108.9(4) . . ? C13 Si2 C23 114.7(5) . . ? C24 Si2 C23 107.8(6) . . ? C13 Si2 C22 112.3(5) . . ? C24 Si2 C22 108.6(5) . . ? C23 Si2 C22 104.3(5) . . ? C25 Si3 C35 114.8(6) . . ? C25 Si3 C34 112.5(6) . . ? C35 Si3 C34 106.5(8) . . ? C25 Si3 C36 106.3(5) . . ? C35 Si3 C36 107.1(6) . . ? C34 Si3 C36 109.5(6) . . ? C37 Si4 C47 113.1(5) . . ? C37 Si4 C46 108.3(5) . . ? C47 Si4 C46 107.3(5) . . ? C37 Si4 C48 113.0(5) . . ? C47 Si4 C48 107.2(6) . . ? C46 Si4 C48 107.6(5) . . ? C2 C1 C5 105.2(9) . . ? C2 C1 Si1 130.2(7) . . ? C5 C1 Si1 122.9(8) . . ? C2 C1 Lu1 73.3(5) . . ? C5 C1 Lu1 75.4(5) . . ? Si1 C1 Lu1 127.3(4) . . ? C3 C2 C1 110.1(9) . . ? C3 C2 C6 122.3(10) . . ? C1 C2 C6 127.6(9) . . ? C3 C2 Lu1 75.7(5) . . ? C1 C2 Lu1 74.5(5) . . ? C6 C2 Lu1 116.3(6) . . ? C2 C3 C4 106.8(9) . . ? C2 C3 C7 127.4(11) . . ? C4 C3 C7 125.6(11) . . ? C2 C3 Lu1 72.8(5) . . ? C4 C3 Lu1 75.4(5) . . ? C7 C3 Lu1 121.6(7) . . ? C5 C4 C3 109.1(9) . . ? C5 C4 C8 125.4(11) . . ? C3 C4 C8 125.4(11) . . ? C5 C4 Lu1 74.4(5) . . ? C3 C4 Lu1 72.7(5) . . ? C8 C4 Lu1 121.5(6) . . ? C4 C5 C1 108.8(9) . . ? C4 C5 C9 125.6(9) . . ? C1 C5 C9 125.4(9) . . ? C4 C5 Lu1 75.2(6) . . ? C1 C5 Lu1 72.0(5) . . ? C9 C5 Lu1 122.7(7) . . ? C14 C13 C17 105.8(8) . . ? C14 C13 Si2 129.7(7) . . ? C17 C13 Si2 123.3(7) . . ? C14 C13 Lu2 74.6(5) . . ? C17 C13 Lu2 75.9(5) . . ? Si2 C13 Lu2 124.6(4) . . ? C15 C14 C13 109.2(9) . . ? C15 C14 C18 124.0(9) . . ? C13 C14 C18 126.8(9) . . ? C15 C14 Lu2 76.0(6) . . ? C13 C14 Lu2 73.4(5) . . ? C18 C14 Lu2 117.7(7) . . ? C14 C15 C16 108.6(9) . . ? C14 C15 C19 126.3(10) . . ? C16 C15 C19 125.1(10) . . ? C14 C15 Lu2 73.1(6) . . ? C16 C15 Lu2 74.8(6) . . ? C19 C15 Lu2 119.9(7) . . ? C17 C16 C15 108.0(9) . . ? C17 C16 C20 125.7(10) . . ? C15 C16 C20 126.0(10) . . ? C17 C16 Lu2 74.1(6) . . ? C15 C16 Lu2 74.0(6) . . ? C20 C16 Lu2 122.9(8) . . ? C16 C17 C13 108.3(8) . . ? C16 C17 C21 124.9(9) . . ? C13 C17 C21 126.6(9) . . ? C16 C17 Lu2 75.0(6) . . ? C13 C17 Lu2 71.8(5) . . ? C21 C17 Lu2 122.9(7) . . ? C26 C25 C29 107.2(8) . . ? C26 C25 Si3 127.1(8) . . ? C29 C25 Si3 124.7(8) . . ? C26 C25 Lu3 74.5(5) . . ? C29 C25 Lu3 75.5(5) . . ? Si3 C25 Lu3 124.7(5) . . ? C25 C26 C27 107.4(9) . . ? C25 C26 C30 129.6(10) . . ? C27 C26 C30 123.0(11) . . ? C25 C26 Lu3 73.8(6) . . ? C27 C26 Lu3 75.4(6) . . ? C30 C26 Lu3 117.8(7) . . ? C28 C27 C26 107.4(9) . . ? C28 C27 C31 125.5(11) . . ? C26 C27 C31 127.0(12) . . ? C28 C27 Lu3 74.5(6) . . ? C26 C27 Lu3 72.5(5) . . ? C31 C27 Lu3 120.3(7) . . ? C29 C28 C27 107.9(9) . . ? C29 C28 C32 128.1(12) . . ? C27 C28 C32 123.8(11) . . ? C29 C28 Lu3 74.0(6) . . ? C27 C28 Lu3 74.3(5) . . ? C32 C28 Lu3 121.8(7) . . ? C28 C29 C25 110.0(10) . . ? C28 C29 C33 123.3(10) . . ? C25 C29 C33 126.5(10) . . ? C28 C29 Lu3 75.4(6) . . ? C25 C29 Lu3 72.9(5) . . ? C33 C29 Lu3 122.8(7) . . ? C38 C37 C41 104.8(8) . . ? C38 C37 Si4 124.2(7) . . ? C41 C37 Si4 129.4(7) . . ? C38 C37 Lu4 75.6(5) . . ? C41 C37 Lu4 72.7(5) . . ? Si4 C37 Lu4 127.6(5) . . ? C39 C38 C37 110.7(8) . . ? C39 C38 C42 123.7(9) . . ? C37 C38 C42 125.6(9) . . ? C39 C38 Lu4 74.2(5) . . ? C37 C38 Lu4 72.7(5) . . ? C42 C38 Lu4 121.5(6) . . ? C38 C39 C40 106.9(9) . . ? C38 C39 C43 126.2(10) . . ? C40 C39 C43 126.3(10) . . ? C38 C39 Lu4 75.0(5) . . ? C40 C39 Lu4 73.7(6) . . ? C43 C39 Lu4 123.5(7) . . ? C41 C40 C39 108.5(9) . . ? C41 C40 C44 128.1(11) . . ? C39 C40 C44 123.4(11) . . ? C41 C40 Lu4 72.7(6) . . ? C39 C40 Lu4 74.8(6) . . ? C44 C40 Lu4 118.5(7) . . ? C40 C41 C37 109.0(9) . . ? C40 C41 C45 122.6(9) . . ? C37 C41 C45 128.4(10) . . ? C40 C41 Lu4 75.9(5) . . ? C37 C41 Lu4 74.8(5) . . ? C45 C41 Lu4 117.4(7) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 3.752 _refine_diff_density_min -2.989 _refine_diff_density_rms 0.286 data_5Y _database_code_depnum_ccdc_archive 'CCDC 767214' #TrackingRef '- DT-ART-02-2010-00006.cif' _database_code_depnum_ccdc_archive 'CCDC 767214' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H99 N7 Si4 Y4' _chemical_formula_weight 1242.34 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.297(4) _cell_length_b 12.839(2) _cell_length_c 41.586(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.606(4) _cell_angle_gamma 90.00 _cell_volume 12425(4) _cell_formula_units_Z 8 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 38523 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 27.59 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5184 _exptl_absorpt_coefficient_mu 3.811 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5161 _exptl_absorpt_correction_T_max 0.8942 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 38523 _diffrn_reflns_av_R_equivalents 0.2411 _diffrn_reflns_av_sigmaI/netI 0.5801 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.59 _reflns_number_total 14016 _reflns_number_gt 3196 _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 'ORTEP-III (Farrugia, 1997)' _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. Although there are solvent accessible voids in the structure, no lattice solvent was found. EADP was applied to C1-C5, C13-C17, C18-C21, and C25-C29. SADI was applied to the four Y-H1(mu4-H) bonds. Uiso of H1 is fixed. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0000P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14016 _refine_ls_number_parameters 509 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.3029 _refine_ls_R_factor_gt 0.0844 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.010 _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 H1 H 0.6099(5) 0.4951(9) 0.8848(3) 0.050 Uiso 1 1 d D . . Y1 Y 0.58894(6) 0.32496(10) 0.88315(4) 0.0332(4) Uani 1 1 d D . . Y2 Y 0.67448(6) 0.53676(11) 0.92412(3) 0.0301(4) Uani 1 1 d D . . Y3 Y 0.53437(6) 0.59658(10) 0.89387(4) 0.0327(4) Uani 1 1 d D . . Y4 Y 0.64704(6) 0.55718(11) 0.83993(4) 0.0372(4) Uani 1 1 d D . . N1 N 0.6323(5) 0.6844(9) 0.8876(3) 0.049(4) Uani 1 1 d . . . N2 N 0.5806(4) 0.5464(9) 0.9430(3) 0.051(4) Uani 1 1 d . . . H2A H 0.5678 0.4831 0.9501 0.062 Uiso 1 1 calc R . . H2B H 0.5774 0.5959 0.9588 0.062 Uiso 1 1 calc R . . N3 N 0.7209(5) 0.5069(8) 0.8764(2) 0.046(4) Uani 1 1 d . . . H3A H 0.7530 0.5479 0.8748 0.055 Uiso 1 1 calc R . . H3B H 0.7306 0.4380 0.8740 0.055 Uiso 1 1 calc R . . N4 N 0.5468(4) 0.5806(8) 0.8386(2) 0.043(3) Uani 1 1 d . . . H4A H 0.5356 0.6398 0.8275 0.051 Uiso 1 1 calc R . . H4B H 0.5275 0.5239 0.8299 0.051 Uiso 1 1 calc R . . N5 N 0.6579(5) 0.3539(8) 0.9247(3) 0.045(4) Uani 1 1 d . . . H5A H 0.6912 0.3179 0.9211 0.054 Uiso 1 1 calc R . . H5B H 0.6445 0.3333 0.9442 0.054 Uiso 1 1 calc R . . N6 N 0.6291(5) 0.3760(8) 0.8346(3) 0.045(4) Uani 1 1 d . . . H6E H 0.6039 0.3631 0.8174 0.053 Uiso 1 1 calc R . . H6D H 0.6627 0.3404 0.8316 0.053 Uiso 1 1 calc R . . N7 N 0.5059(4) 0.4202(8) 0.8927(3) 0.039(3) Uani 1 1 d . . . H7E H 0.4913 0.4012 0.9120 0.047 Uiso 1 1 calc R . . H7D H 0.4783 0.4090 0.8766 0.047 Uiso 1 1 calc R . . Si1 Si 0.5139(2) 0.1573(4) 0.81415(12) 0.0550(15) Uani 1 1 d . . . Si2 Si 0.83611(18) 0.4562(3) 0.95425(12) 0.0455(13) Uani 1 1 d . . . Si3 Si 0.3633(2) 0.5916(4) 0.87701(13) 0.0610(15) Uani 1 1 d . . . Si4 Si 0.7334(2) 0.4621(5) 0.76323(13) 0.0714(17) Uani 1 1 d . . . C1 C 0.5447(6) 0.1547(10) 0.8567(4) 0.043(2) Uani 1 1 d . . . C2 C 0.5129(7) 0.1712(10) 0.8845(4) 0.043(2) Uani 1 1 d . . . C3 C 0.5494(7) 0.1551(10) 0.9117(4) 0.043(2) Uani 1 1 d . . . C4 C 0.6032(7) 0.1271(10) 0.9013(4) 0.043(2) Uani 1 1 d . . . C5 C 0.6012(7) 0.1260(10) 0.8680(4) 0.043(2) Uani 1 1 d . . . C6 C 0.4487(6) 0.1903(11) 0.8841(4) 0.076(6) Uani 1 1 d . . . H6A H 0.4390 0.2487 0.8697 0.115 Uiso 1 1 calc R . . H6B H 0.4373 0.2067 0.9059 0.115 Uiso 1 1 calc R . . H6C H 0.4284 0.1276 0.8764 0.115 Uiso 1 1 calc R . . C7 C 0.5332(7) 0.1651(12) 0.9454(4) 0.090(7) Uani 1 1 d . . . H7A H 0.5606 0.2110 0.9570 0.135 Uiso 1 1 calc R . . H7B H 0.5338 0.0963 0.9556 0.135 Uiso 1 1 calc R . . H7C H 0.4945 0.1947 0.9460 0.135 Uiso 1 1 calc R . . C8 C 0.6533(6) 0.0901(12) 0.9235(4) 0.071(6) Uani 1 1 d . . . H8A H 0.6552 0.1326 0.9431 0.107 Uiso 1 1 calc R . . H8B H 0.6893 0.0970 0.9124 0.107 Uiso 1 1 calc R . . H8C H 0.6474 0.0169 0.9293 0.107 Uiso 1 1 calc R . . C9 C 0.6495(6) 0.0920(11) 0.8480(4) 0.057(5) Uani 1 1 d . . . H9A H 0.6578 0.1468 0.8325 0.086 Uiso 1 1 calc R . . H9B H 0.6387 0.0279 0.8365 0.086 Uiso 1 1 calc R . . H9C H 0.6837 0.0791 0.8620 0.086 Uiso 1 1 calc R . . C10 C 0.4790(6) 0.2830(11) 0.8040(4) 0.073(6) Uani 1 1 d . . . H10A H 0.5044 0.3402 0.8112 0.109 Uiso 1 1 calc R . . H10B H 0.4427 0.2881 0.8149 0.109 Uiso 1 1 calc R . . H10C H 0.4715 0.2875 0.7807 0.109 Uiso 1 1 calc R . . C11 C 0.5694(6) 0.1372(12) 0.7835(4) 0.077(6) Uani 1 1 d . . . H11A H 0.5989 0.1914 0.7859 0.115 Uiso 1 1 calc R . . H11B H 0.5511 0.1411 0.7618 0.115 Uiso 1 1 calc R . . H11C H 0.5873 0.0686 0.7866 0.115 Uiso 1 1 calc R . . C12 C 0.4594(6) 0.0521(12) 0.8085(4) 0.086(6) Uani 1 1 d . . . H12A H 0.4300 0.0600 0.8244 0.129 Uiso 1 1 calc R . . H12B H 0.4781 -0.0159 0.8113 0.129 Uiso 1 1 calc R . . H12C H 0.4414 0.0567 0.7868 0.129 Uiso 1 1 calc R . . C13 C 0.7729(5) 0.5423(10) 0.9579(3) 0.0282(16) Uani 1 1 d . . . C14 C 0.7668(5) 0.6438(10) 0.9439(3) 0.0282(16) Uani 1 1 d . . . C15 C 0.7212(5) 0.6959(10) 0.9576(3) 0.0282(16) Uani 1 1 d . . . C16 C 0.6996(5) 0.6307(10) 0.9811(3) 0.0282(16) Uani 1 1 d . . . C17 C 0.7301(5) 0.5357(10) 0.9809(3) 0.0282(16) Uani 1 1 d . . . C18 C 0.8053(5) 0.6924(10) 0.9197(3) 0.044(2) Uani 1 1 d . . . H18A H 0.8070 0.6470 0.9009 0.066 Uiso 1 1 calc R . . H18B H 0.8440 0.7013 0.9296 0.066 Uiso 1 1 calc R . . H18C H 0.7898 0.7605 0.9131 0.066 Uiso 1 1 calc R . . C19 C 0.7034(5) 0.8077(10) 0.9519(3) 0.044(2) Uani 1 1 d . . . H19A H 0.6615 0.8134 0.9525 0.066 Uiso 1 1 calc R . . H19B H 0.7158 0.8304 0.9308 0.066 Uiso 1 1 calc R . . H19C H 0.7214 0.8519 0.9687 0.066 Uiso 1 1 calc R . . C20 C 0.6544(5) 0.6599(10) 1.0042(3) 0.044(2) Uani 1 1 d . . . H20A H 0.6247 0.6058 1.0040 0.066 Uiso 1 1 calc R . . H20B H 0.6370 0.7265 0.9977 0.066 Uiso 1 1 calc R . . H20C H 0.6721 0.6662 1.0259 0.066 Uiso 1 1 calc R . . C21 C 0.7200(5) 0.4501(10) 1.0042(3) 0.044(2) Uani 1 1 d . . . H21A H 0.6805 0.4540 1.0112 0.066 Uiso 1 1 calc R . . H21B H 0.7468 0.4574 1.0230 0.066 Uiso 1 1 calc R . . H21C H 0.7262 0.3828 0.9939 0.066 Uiso 1 1 calc R . . C22 C 0.8247(6) 0.3216(11) 0.9688(4) 0.097(7) Uani 1 1 d . . . H22A H 0.8615 0.2849 0.9705 0.146 Uiso 1 1 calc R . . H22B H 0.7985 0.2848 0.9536 0.146 Uiso 1 1 calc R . . H22C H 0.8079 0.3240 0.9900 0.146 Uiso 1 1 calc R . . C23 C 0.8619(6) 0.4414(11) 0.9132(4) 0.070(6) Uani 1 1 d . . . H23A H 0.8914 0.3872 0.9131 0.104 Uiso 1 1 calc R . . H23B H 0.8782 0.5076 0.9062 0.104 Uiso 1 1 calc R . . H23C H 0.8297 0.4217 0.8984 0.104 Uiso 1 1 calc R . . C24 C 0.8959(6) 0.5128(12) 0.9794(4) 0.086(7) Uani 1 1 d . . . H24A H 0.9270 0.4616 0.9820 0.129 Uiso 1 1 calc R . . H24B H 0.8821 0.5315 1.0005 0.129 Uiso 1 1 calc R . . H24C H 0.9103 0.5753 0.9689 0.129 Uiso 1 1 calc R . . C25 C 0.4272(6) 0.6620(10) 0.8941(4) 0.041(2) Uani 1 1 d . . . C26 C 0.4558(6) 0.7401(11) 0.8784(4) 0.041(2) Uani 1 1 d . . . C27 C 0.4941(6) 0.7930(11) 0.8986(4) 0.041(2) Uani 1 1 d . . . C28 C 0.4891(6) 0.7470(11) 0.9292(4) 0.041(2) Uani 1 1 d . . . C29 C 0.4488(6) 0.6684(11) 0.9271(4) 0.041(2) Uani 1 1 d . . . C30 C 0.4414(7) 0.7729(13) 0.8424(4) 0.089(7) Uani 1 1 d . . . H30A H 0.4136 0.7238 0.8325 0.134 Uiso 1 1 calc R . . H30B H 0.4767 0.7721 0.8304 0.134 Uiso 1 1 calc R . . H30C H 0.4250 0.8432 0.8418 0.134 Uiso 1 1 calc R . . C31 C 0.5295(7) 0.8870(11) 0.8904(5) 0.091(7) Uani 1 1 d . . . H31A H 0.5671 0.8829 0.9018 0.136 Uiso 1 1 calc R . . H31B H 0.5096 0.9504 0.8970 0.136 Uiso 1 1 calc R . . H31C H 0.5346 0.8889 0.8672 0.136 Uiso 1 1 calc R . . C32 C 0.5206(6) 0.7883(14) 0.9585(4) 0.109(9) Uani 1 1 d . . . H32A H 0.5400 0.7310 0.9701 0.163 Uiso 1 1 calc R . . H32B H 0.4933 0.8217 0.9725 0.163 Uiso 1 1 calc R . . H32C H 0.5491 0.8395 0.9521 0.163 Uiso 1 1 calc R . . C33 C 0.4345(6) 0.6030(12) 0.9555(4) 0.074(6) Uani 1 1 d . . . H33A H 0.4336 0.5294 0.9493 0.111 Uiso 1 1 calc R . . H33B H 0.3968 0.6235 0.9630 0.111 Uiso 1 1 calc R . . H33C H 0.4638 0.6134 0.9729 0.111 Uiso 1 1 calc R . . C34 C 0.3759(6) 0.5281(14) 0.8382(4) 0.088(7) Uani 1 1 d . . . H34A H 0.3398 0.4987 0.8292 0.131 Uiso 1 1 calc R . . H34B H 0.4043 0.4723 0.8415 0.131 Uiso 1 1 calc R . . H34C H 0.3904 0.5796 0.8231 0.131 Uiso 1 1 calc R . . C35 C 0.3362(7) 0.4912(13) 0.9045(4) 0.100(7) Uani 1 1 d . . . H35A H 0.2972 0.4706 0.8972 0.150 Uiso 1 1 calc R . . H35B H 0.3356 0.5196 0.9264 0.150 Uiso 1 1 calc R . . H35C H 0.3615 0.4302 0.9045 0.150 Uiso 1 1 calc R . . C36 C 0.3053(6) 0.6892(14) 0.8672(4) 0.107(8) Uani 1 1 d . . . H36A H 0.3213 0.7475 0.8553 0.160 Uiso 1 1 calc R . . H36B H 0.2898 0.7150 0.8872 0.160 Uiso 1 1 calc R . . H36C H 0.2745 0.6561 0.8540 0.160 Uiso 1 1 calc R . . C37 C 0.7013(7) 0.5717(11) 0.7855(3) 0.040(4) Uani 1 1 d . . . C38 C 0.6480(7) 0.6232(15) 0.7809(4) 0.057(5) Uani 1 1 d . . . C39 C 0.6477(8) 0.7159(14) 0.7984(4) 0.054(5) Uani 1 1 d . . . C40 C 0.7007(8) 0.7231(13) 0.8151(4) 0.047(5) Uani 1 1 d . . . C41 C 0.7345(7) 0.6382(12) 0.8077(4) 0.043(5) Uani 1 1 d . . . C42 C 0.5991(7) 0.5929(14) 0.7573(4) 0.084(7) Uani 1 1 d . . . H42A H 0.5637 0.6271 0.7634 0.126 Uiso 1 1 calc R . . H42B H 0.5939 0.5172 0.7577 0.126 Uiso 1 1 calc R . . H42C H 0.6083 0.6148 0.7355 0.126 Uiso 1 1 calc R . . C43 C 0.6019(7) 0.7978(12) 0.7979(4) 0.085(7) Uani 1 1 d . . . H43A H 0.5682 0.7730 0.7852 0.127 Uiso 1 1 calc R . . H43B H 0.6164 0.8616 0.7882 0.127 Uiso 1 1 calc R . . H43C H 0.5911 0.8124 0.8199 0.127 Uiso 1 1 calc R . . C44 C 0.7201(7) 0.8136(12) 0.8366(4) 0.085(7) Uani 1 1 d . . . H44A H 0.6885 0.8636 0.8380 0.127 Uiso 1 1 calc R . . H44B H 0.7531 0.8481 0.8275 0.127 Uiso 1 1 calc R . . H44C H 0.7310 0.7874 0.8581 0.127 Uiso 1 1 calc R . . C45 C 0.7964(6) 0.6244(12) 0.8180(4) 0.071(6) Uani 1 1 d . . . H45A H 0.8034 0.5515 0.8240 0.106 Uiso 1 1 calc R . . H45B H 0.8057 0.6693 0.8366 0.106 Uiso 1 1 calc R . . H45C H 0.8206 0.6433 0.8003 0.106 Uiso 1 1 calc R . . C46 C 0.7819(8) 0.3767(14) 0.7880(5) 0.128(9) Uani 1 1 d . . . H46A H 0.8096 0.4196 0.8005 0.192 Uiso 1 1 calc R . . H46B H 0.8026 0.3300 0.7739 0.192 Uiso 1 1 calc R . . H46C H 0.7593 0.3354 0.8026 0.192 Uiso 1 1 calc R . . C47 C 0.6794(7) 0.3742(13) 0.7442(4) 0.097(7) Uani 1 1 d . . . H47A H 0.6548 0.3465 0.7607 0.146 Uiso 1 1 calc R . . H47B H 0.6988 0.3166 0.7338 0.146 Uiso 1 1 calc R . . H47C H 0.6559 0.4128 0.7282 0.146 Uiso 1 1 calc R . . C48 C 0.7763(8) 0.5226(14) 0.7312(4) 0.128(9) Uani 1 1 d . . . H48A H 0.7506 0.5605 0.7161 0.192 Uiso 1 1 calc R . . H48B H 0.7965 0.4680 0.7197 0.192 Uiso 1 1 calc R . . H48C H 0.8045 0.5710 0.7412 0.192 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 0.0411(10) 0.0205(8) 0.0385(10) -0.0007(7) 0.0065(8) 0.0008(7) Y2 0.0333(9) 0.0230(8) 0.0344(10) -0.0034(7) 0.0043(7) 0.0008(7) Y3 0.0363(9) 0.0218(8) 0.0403(10) -0.0017(7) 0.0045(8) 0.0019(7) Y4 0.0478(10) 0.0288(9) 0.0357(10) -0.0012(7) 0.0109(8) -0.0012(8) N1 0.056(9) 0.058(9) 0.034(9) 0.004(7) 0.016(7) 0.014(7) N2 0.056(9) 0.035(8) 0.063(10) -0.019(7) 0.011(7) -0.005(7) N3 0.060(9) 0.027(8) 0.051(9) -0.010(6) 0.008(7) -0.008(6) N4 0.050(8) 0.024(8) 0.054(9) 0.004(6) 0.005(7) 0.003(6) N5 0.065(10) 0.033(8) 0.038(9) 0.005(6) 0.014(7) 0.000(7) N6 0.054(9) 0.046(9) 0.034(9) -0.002(6) 0.006(7) -0.003(7) N7 0.045(8) 0.040(8) 0.032(8) 0.002(6) 0.002(6) -0.005(6) Si1 0.060(4) 0.033(3) 0.071(4) -0.005(3) -0.016(3) -0.003(3) Si2 0.042(3) 0.028(3) 0.067(4) 0.001(2) 0.009(3) 0.011(2) Si3 0.061(4) 0.050(3) 0.072(4) -0.005(3) 0.000(3) -0.011(3) Si4 0.078(4) 0.076(4) 0.063(4) -0.024(3) 0.026(3) -0.005(4) C1 0.054(6) 0.016(4) 0.060(6) -0.003(4) 0.006(5) -0.007(4) C2 0.054(6) 0.016(4) 0.060(6) -0.003(4) 0.006(5) -0.007(4) C3 0.054(6) 0.016(4) 0.060(6) -0.003(4) 0.006(5) -0.007(4) C4 0.054(6) 0.016(4) 0.060(6) -0.003(4) 0.006(5) -0.007(4) C5 0.054(6) 0.016(4) 0.060(6) -0.003(4) 0.006(5) -0.007(4) C6 0.050(12) 0.048(12) 0.134(19) -0.017(12) 0.036(12) -0.011(10) C7 0.141(19) 0.049(13) 0.082(17) 0.008(11) 0.041(14) -0.023(13) C8 0.099(15) 0.045(12) 0.068(14) -0.006(10) -0.017(12) -0.010(11) C9 0.057(12) 0.030(10) 0.085(15) -0.022(9) -0.002(10) -0.003(9) C10 0.093(15) 0.047(12) 0.075(15) -0.017(10) -0.035(11) 0.017(10) C11 0.084(14) 0.076(15) 0.067(15) -0.019(11) -0.016(12) 0.018(11) C12 0.103(16) 0.063(14) 0.088(16) 0.008(12) -0.044(12) -0.030(12) C13 0.023(4) 0.025(4) 0.036(5) -0.009(3) 0.002(3) -0.008(3) C14 0.023(4) 0.025(4) 0.036(5) -0.009(3) 0.002(3) -0.008(3) C15 0.023(4) 0.025(4) 0.036(5) -0.009(3) 0.002(3) -0.008(3) C16 0.023(4) 0.025(4) 0.036(5) -0.009(3) 0.002(3) -0.008(3) C17 0.023(4) 0.025(4) 0.036(5) -0.009(3) 0.002(3) -0.008(3) C18 0.044(5) 0.039(5) 0.049(6) -0.006(4) 0.008(4) 0.001(4) C19 0.044(5) 0.039(5) 0.049(6) -0.006(4) 0.008(4) 0.001(4) C20 0.044(5) 0.039(5) 0.049(6) -0.006(4) 0.008(4) 0.001(4) C21 0.044(5) 0.039(5) 0.049(6) -0.006(4) 0.008(4) 0.001(4) C22 0.084(15) 0.029(11) 0.18(2) 0.031(13) 0.048(14) 0.031(11) C23 0.068(13) 0.054(13) 0.089(16) 0.002(11) 0.031(11) 0.018(10) C24 0.041(12) 0.071(15) 0.15(2) -0.011(13) 0.005(12) 0.023(10) C25 0.031(5) 0.021(4) 0.070(6) -0.007(4) 0.007(4) 0.008(3) C26 0.031(5) 0.021(4) 0.070(6) -0.007(4) 0.007(4) 0.008(3) C27 0.031(5) 0.021(4) 0.070(6) -0.007(4) 0.007(4) 0.008(3) C28 0.031(5) 0.021(4) 0.070(6) -0.007(4) 0.007(4) 0.008(3) C29 0.031(5) 0.021(4) 0.070(6) -0.007(4) 0.007(4) 0.008(3) C30 0.090(16) 0.066(15) 0.115(19) 0.031(13) 0.050(14) 0.034(12) C31 0.072(14) 0.038(12) 0.17(2) 0.001(13) 0.042(13) 0.003(11) C32 0.038(12) 0.13(2) 0.16(2) -0.108(16) -0.032(13) 0.029(12) C33 0.079(14) 0.077(14) 0.068(15) 0.029(11) 0.035(11) 0.044(11) C34 0.075(14) 0.127(19) 0.060(14) -0.028(13) 0.006(11) -0.032(13) C35 0.107(17) 0.087(17) 0.110(18) 0.018(13) 0.046(14) -0.038(13) C36 0.038(12) 0.107(18) 0.17(2) 0.014(16) -0.045(13) 0.021(12) C37 0.051(11) 0.047(11) 0.022(10) 0.020(8) 0.013(8) -0.014(9) C38 0.041(12) 0.087(16) 0.044(13) 0.009(11) 0.012(10) 0.012(11) C39 0.070(15) 0.053(13) 0.041(13) 0.036(10) 0.016(11) 0.013(11) C40 0.064(14) 0.035(11) 0.042(12) 0.013(9) 0.007(10) -0.020(10) C41 0.038(11) 0.037(10) 0.055(13) 0.019(9) 0.012(10) 0.019(9) C42 0.083(15) 0.14(2) 0.025(12) 0.007(12) 0.006(11) 0.012(14) C43 0.086(15) 0.069(14) 0.104(17) 0.051(12) 0.063(13) 0.043(12) C44 0.098(16) 0.038(12) 0.119(19) 0.031(12) 0.020(14) -0.001(11) C45 0.060(13) 0.087(16) 0.067(15) -0.002(11) 0.015(11) -0.017(11) C46 0.16(2) 0.10(2) 0.12(2) -0.002(16) 0.005(17) 0.039(17) C47 0.133(19) 0.078(16) 0.086(17) -0.022(12) 0.061(14) -0.024(13) C48 0.14(2) 0.12(2) 0.13(2) -0.055(16) 0.104(17) -0.056(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 Y1 N5 2.336(11) . ? Y1 N7 2.338(10) . ? Y1 N6 2.357(10) . ? Y1 C1 2.635(14) . ? Y1 C2 2.654(14) . ? Y1 C5 2.650(13) . ? Y1 C3 2.666(14) . ? Y1 C4 2.667(14) . ? Y1 Y2 3.736(2) . ? Y1 Y3 3.745(2) . ? Y1 Y4 3.765(2) . ? Y2 N3 2.335(10) . ? Y2 N2 2.360(10) . ? Y2 N5 2.380(10) . ? Y2 N1 2.595(12) . ? Y2 C13 2.635(12) . ? Y2 C17 2.641(13) . ? Y2 C14 2.651(12) . ? Y2 C15 2.676(12) . ? Y2 C16 2.698(13) . ? Y2 Y3 3.529(2) . ? Y2 Y4 3.540(2) . ? Y3 N4 2.340(10) . ? Y3 N2 2.354(11) . ? Y3 N7 2.359(10) . ? Y3 N1 2.568(11) . ? Y3 C25 2.635(13) . ? Y3 C29 2.641(14) . ? Y3 C26 2.656(14) . ? Y3 C28 2.672(14) . ? Y3 C27 2.700(13) . ? Y3 Y4 3.565(2) . ? Y4 N3 2.331(11) . ? Y4 N4 2.353(10) . ? Y4 N6 2.372(10) . ? Y4 N1 2.603(11) . ? Y4 C38 2.600(17) . ? Y4 C37 2.648(13) . ? Y4 C39 2.672(15) . ? Y4 C41 2.698(15) . ? Y4 C40 2.700(14) . ? Si1 C10 1.847(14) . ? Si1 C12 1.861(14) . ? Si1 C1 1.881(16) . ? Si1 C11 1.876(15) . ? Si2 C23 1.845(14) . ? Si2 C13 1.854(13) . ? Si2 C24 1.852(15) . ? Si2 C22 1.853(14) . ? Si3 C34 1.845(15) . ? Si3 C25 1.854(15) . ? Si3 C35 1.853(15) . ? Si3 C36 1.874(15) . ? Si4 C47 1.841(16) . ? Si4 C46 1.852(18) . ? Si4 C37 1.861(16) . ? Si4 C48 1.869(16) . ? C1 C2 1.417(18) . ? C1 C5 1.424(18) . ? C2 C3 1.397(19) . ? C2 C6 1.514(17) . ? C3 C4 1.388(18) . ? C3 C7 1.475(19) . ? C4 C5 1.387(19) . ? C4 C8 1.530(19) . ? C5 C9 1.493(17) . ? C13 C17 1.415(15) . ? C13 C14 1.431(16) . ? C14 C15 1.399(16) . ? C14 C18 1.513(16) . ? C15 C16 1.395(16) . ? C15 C19 1.510(16) . ? C16 C17 1.412(16) . ? C16 C20 1.505(16) . ? C17 C21 1.491(16) . ? C25 C26 1.383(18) . ? C25 C29 1.442(19) . ? C26 C27 1.375(18) . ? C26 C30 1.578(18) . ? C27 C28 1.414(19) . ? C27 C31 1.509(18) . ? C28 C29 1.377(17) . ? C28 C32 1.491(18) . ? C29 C33 1.502(18) . ? C37 C38 1.411(19) . ? C37 C41 1.453(19) . ? C38 C39 1.40(2) . ? C38 C42 1.52(2) . ? C39 C40 1.39(2) . ? C39 C43 1.498(19) . ? C40 C41 1.387(19) . ? C40 C44 1.52(2) . ? C41 C45 1.497(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Y1 N7 109.8(4) . . ? N5 Y1 N6 107.6(4) . . ? N7 Y1 N6 111.4(4) . . ? N5 Y1 C1 133.1(4) . . ? N7 Y1 C1 101.2(4) . . ? N6 Y1 C1 92.1(4) . . ? N5 Y1 C2 122.7(4) . . ? N7 Y1 C2 80.0(4) . . ? N6 Y1 C2 121.1(4) . . ? C1 Y1 C2 31.1(4) . . ? N5 Y1 C5 104.6(4) . . ? N7 Y1 C5 130.1(4) . . ? N6 Y1 C5 90.7(4) . . ? C1 Y1 C5 31.3(4) . . ? C2 Y1 C5 50.8(5) . . ? N5 Y1 C3 92.3(4) . . ? N7 Y1 C3 92.7(4) . . ? N6 Y1 C3 140.1(4) . . ? C1 Y1 C3 51.0(5) . . ? C2 Y1 C3 30.5(4) . . ? C5 Y1 C3 50.2(5) . . ? N5 Y1 C4 82.5(4) . . ? N7 Y1 C4 122.9(4) . . ? N6 Y1 C4 117.3(4) . . ? C1 Y1 C4 50.9(5) . . ? C2 Y1 C4 50.2(5) . . ? C5 Y1 C4 30.2(4) . . ? C3 Y1 C4 30.2(4) . . ? N5 Y1 Y2 38.0(2) . . ? N7 Y1 Y2 88.3(3) . . ? N6 Y1 Y2 87.9(3) . . ? C1 Y1 Y2 169.8(3) . . ? C2 Y1 Y2 150.9(4) . . ? C5 Y1 Y2 138.5(4) . . ? C3 Y1 Y2 125.5(4) . . ? C4 Y1 Y2 120.5(4) . . ? N5 Y1 Y3 89.4(3) . . ? N7 Y1 Y3 37.3(2) . . ? N6 Y1 Y3 89.6(3) . . ? C1 Y1 Y3 133.9(3) . . ? C2 Y1 Y3 117.3(3) . . ? C5 Y1 Y3 165.2(4) . . ? C3 Y1 Y3 125.7(3) . . ? C4 Y1 Y3 153.1(4) . . ? Y2 Y1 Y3 56.29(4) . . ? N5 Y1 Y4 88.7(3) . . ? N7 Y1 Y4 89.1(3) . . ? N6 Y1 Y4 37.4(3) . . ? C1 Y1 Y4 126.9(3) . . ? C2 Y1 Y4 148.6(4) . . ? C5 Y1 Y4 127.2(4) . . ? C3 Y1 Y4 177.4(4) . . ? C4 Y1 Y4 147.9(3) . . ? Y2 Y1 Y4 56.32(4) . . ? Y3 Y1 Y4 56.68(4) . . ? N3 Y2 N2 139.7(4) . . ? N3 Y2 N5 85.9(4) . . ? N2 Y2 N5 84.0(4) . . ? N3 Y2 N1 78.4(4) . . ? N2 Y2 N1 79.9(4) . . ? N5 Y2 N1 132.0(4) . . ? N3 Y2 C13 91.9(4) . . ? N2 Y2 C13 128.2(4) . . ? N5 Y2 C13 99.1(4) . . ? N1 Y2 C13 126.1(4) . . ? N3 Y2 C17 122.1(4) . . ? N2 Y2 C17 97.4(4) . . ? N5 Y2 C17 93.4(4) . . ? N1 Y2 C17 133.2(4) . . ? C13 Y2 C17 31.1(3) . . ? N3 Y2 C14 87.1(4) . . ? N2 Y2 C14 128.4(4) . . ? N5 Y2 C14 129.6(4) . . ? N1 Y2 C14 94.8(4) . . ? C13 Y2 C14 31.4(4) . . ? C17 Y2 C14 50.7(4) . . ? N3 Y2 C15 112.0(4) . . ? N2 Y2 C15 98.5(4) . . ? N5 Y2 C15 144.1(4) . . ? N1 Y2 C15 83.2(4) . . ? C13 Y2 C15 51.6(4) . . ? C17 Y2 C15 50.8(4) . . ? C14 Y2 C15 30.4(3) . . ? N3 Y2 C16 136.8(4) . . ? N2 Y2 C16 81.5(4) . . ? N5 Y2 C16 117.4(4) . . ? N1 Y2 C16 104.4(4) . . ? C13 Y2 C16 51.0(4) . . ? C17 Y2 C16 30.7(4) . . ? C14 Y2 C16 49.8(4) . . ? C15 Y2 C16 30.1(3) . . ? N3 Y2 Y3 100.9(3) . . ? N2 Y2 Y3 41.5(3) . . ? N5 Y2 Y3 94.1(3) . . ? N1 Y2 Y3 46.6(3) . . ? C13 Y2 Y3 162.3(3) . . ? C17 Y2 Y3 136.7(3) . . ? C14 Y2 Y3 136.2(3) . . ? C15 Y2 Y3 111.5(3) . . ? C16 Y2 Y3 112.1(3) . . ? N3 Y2 Y4 40.6(3) . . ? N2 Y2 Y4 101.3(3) . . ? N5 Y2 Y4 93.5(3) . . ? N1 Y2 Y4 47.2(3) . . ? C13 Y2 Y4 129.7(3) . . ? C17 Y2 Y4 160.7(3) . . ? C14 Y2 Y4 112.1(3) . . ? C15 Y2 Y4 120.6(3) . . ? C16 Y2 Y4 149.0(3) . . ? Y3 Y2 Y4 60.58(4) . . ? N3 Y2 Y1 75.6(3) . . ? N2 Y2 Y1 72.9(3) . . ? N5 Y2 Y1 37.2(3) . . ? N1 Y2 Y1 94.9(3) . . ? C13 Y2 Y1 134.1(3) . . ? C17 Y2 Y1 129.3(3) . . ? C14 Y2 Y1 158.0(3) . . ? C15 Y2 Y1 171.4(3) . . ? C16 Y2 Y1 144.6(3) . . ? Y3 Y2 Y1 61.98(4) . . ? Y4 Y2 Y1 62.25(4) . . ? N4 Y3 N2 139.1(3) . . ? N4 Y3 N7 86.7(4) . . ? N2 Y3 N7 82.7(4) . . ? N4 Y3 N1 77.8(4) . . ? N2 Y3 N1 80.5(4) . . ? N7 Y3 N1 132.0(4) . . ? N4 Y3 C25 101.0(4) . . ? N2 Y3 C25 118.7(4) . . ? N7 Y3 C25 92.3(4) . . ? N1 Y3 C25 135.0(4) . . ? N4 Y3 C29 132.4(4) . . ? N2 Y3 C29 88.2(4) . . ? N7 Y3 C29 97.3(4) . . ? N1 Y3 C29 126.5(4) . . ? C25 Y3 C29 31.7(4) . . ? N4 Y3 C26 86.4(4) . . ? N2 Y3 C26 133.1(4) . . ? N7 Y3 C26 118.1(4) . . ? N1 Y3 C26 106.0(4) . . ? C25 Y3 C26 30.3(4) . . ? C29 Y3 C26 49.9(5) . . ? N4 Y3 C28 132.3(4) . . ? N2 Y3 C28 84.1(4) . . ? N7 Y3 C28 126.0(4) . . ? N1 Y3 C28 96.5(4) . . ? C25 Y3 C28 50.9(4) . . ? C29 Y3 C28 30.0(4) . . ? C26 Y3 C28 49.2(5) . . ? N4 Y3 C27 102.2(4) . . ? N2 Y3 C27 109.9(4) . . ? N7 Y3 C27 143.1(4) . . ? N1 Y3 C27 84.9(4) . . ? C25 Y3 C27 50.9(4) . . ? C29 Y3 C27 50.5(4) . . ? C26 Y3 C27 29.7(4) . . ? C28 Y3 C27 30.5(4) . . ? N4 Y3 Y2 100.2(2) . . ? N2 Y3 Y2 41.6(2) . . ? N7 Y3 Y2 93.0(2) . . ? N1 Y3 Y2 47.2(3) . . ? C25 Y3 Y2 158.4(3) . . ? C29 Y3 Y2 126.7(4) . . ? C26 Y3 Y2 148.6(3) . . ? C28 Y3 Y2 110.1(3) . . ? C27 Y3 Y2 119.8(3) . . ? N4 Y3 Y4 40.7(2) . . ? N2 Y3 Y4 100.7(3) . . ? N7 Y3 Y4 93.7(2) . . ? N1 Y3 Y4 46.8(3) . . ? C25 Y3 Y4 140.6(4) . . ? C29 Y3 Y4 166.6(3) . . ? C26 Y3 Y4 117.7(3) . . ? C28 Y3 Y4 140.2(3) . . ? C27 Y3 Y4 116.5(3) . . ? Y2 Y3 Y4 59.86(4) . . ? N4 Y3 Y1 75.1(3) . . ? N2 Y3 Y1 72.8(3) . . ? N7 Y3 Y1 36.9(2) . . ? N1 Y3 Y1 95.1(3) . . ? C25 Y3 Y1 128.6(3) . . ? C29 Y3 Y1 130.9(3) . . ? C26 Y3 Y1 148.3(3) . . ? C28 Y3 Y1 152.0(4) . . ? C27 Y3 Y1 177.3(4) . . ? Y2 Y3 Y1 61.73(4) . . ? Y4 Y3 Y1 61.93(4) . . ? N3 Y4 N4 138.9(4) . . ? N3 Y4 N6 84.9(4) . . ? N4 Y4 N6 87.3(4) . . ? N3 Y4 N1 78.4(4) . . ? N4 Y4 N1 76.9(4) . . ? N6 Y4 N1 131.2(4) . . ? N3 Y4 C38 131.8(5) . . ? N4 Y4 C38 89.3(5) . . ? N6 Y4 C38 103.9(5) . . ? N1 Y4 C38 121.5(5) . . ? N3 Y4 C37 102.0(4) . . ? N4 Y4 C37 118.8(4) . . ? N6 Y4 C37 94.5(4) . . ? N1 Y4 C37 133.7(4) . . ? C38 Y4 C37 31.2(4) . . ? N3 Y4 C39 127.3(5) . . ? N4 Y4 C39 85.5(5) . . ? N6 Y4 C39 133.9(5) . . ? N1 Y4 C39 91.0(5) . . ? C38 Y4 C39 30.7(5) . . ? C37 Y4 C39 51.4(5) . . ? N3 Y4 C41 83.0(4) . . ? N4 Y4 C41 135.2(4) . . ? N6 Y4 C41 117.7(4) . . ? N1 Y4 C41 105.4(5) . . ? C38 Y4 C41 50.6(5) . . ? C37 Y4 C41 31.5(4) . . ? C39 Y4 C41 50.1(5) . . ? N3 Y4 C40 97.3(5) . . ? N4 Y4 C40 111.5(5) . . ? N6 Y4 C40 145.1(4) . . ? N1 Y4 C40 82.9(4) . . ? C38 Y4 C40 49.9(5) . . ? C37 Y4 C40 50.9(5) . . ? C39 Y4 C40 30.0(4) . . ? C41 Y4 C40 29.8(4) . . ? N3 Y4 Y2 40.7(3) . . ? N4 Y4 Y2 99.7(3) . . ? N6 Y4 Y2 92.5(3) . . ? N1 Y4 Y2 47.0(3) . . ? C38 Y4 Y2 161.7(4) . . ? C37 Y4 Y2 141.1(4) . . ? C39 Y4 Y2 133.6(5) . . ? C41 Y4 Y2 114.4(4) . . ? C40 Y4 Y2 111.8(4) . . ? N3 Y4 Y3 100.0(3) . . ? N4 Y4 Y3 40.4(3) . . ? N6 Y4 Y3 93.8(2) . . ? N1 Y4 Y3 46.0(2) . . ? C38 Y4 Y3 125.9(4) . . ? C37 Y4 Y3 157.1(4) . . ? C39 Y4 Y3 108.9(4) . . ? C41 Y4 Y3 148.4(3) . . ? C40 Y4 Y3 119.7(4) . . ? Y2 Y4 Y3 59.56(4) . . ? N3 Y4 Y1 75.0(3) . . ? N4 Y4 Y1 74.6(3) . . ? N6 Y4 Y1 37.1(2) . . ? N1 Y4 Y1 94.1(3) . . ? C38 Y4 Y1 136.7(4) . . ? C37 Y4 Y1 131.3(3) . . ? C39 Y4 Y1 157.7(4) . . ? C41 Y4 Y1 147.0(3) . . ? C40 Y4 Y1 172.1(4) . . ? Y2 Y4 Y1 61.44(4) . . ? Y3 Y4 Y1 61.38(4) . . ? Y3 N1 Y2 86.2(4) . . ? Y3 N1 Y4 87.2(4) . . ? Y2 N1 Y4 85.8(4) . . ? Y3 N2 Y2 96.9(4) . . ? Y4 N3 Y2 98.7(4) . . ? Y3 N4 Y4 98.9(4) . . ? Y1 N5 Y2 104.8(4) . . ? Y1 N6 Y4 105.5(4) . . ? Y1 N7 Y3 105.7(4) . . ? C10 Si1 C12 108.4(7) . . ? C10 Si1 C1 112.0(7) . . ? C12 Si1 C1 109.6(7) . . ? C10 Si1 C11 106.0(7) . . ? C12 Si1 C11 107.6(7) . . ? C1 Si1 C11 113.1(7) . . ? C23 Si2 C13 115.5(6) . . ? C23 Si2 C24 107.1(7) . . ? C13 Si2 C24 107.4(6) . . ? C23 Si2 C22 105.3(7) . . ? C13 Si2 C22 113.8(7) . . ? C24 Si2 C22 107.3(8) . . ? C34 Si3 C25 113.2(7) . . ? C34 Si3 C35 107.8(8) . . ? C25 Si3 C35 113.1(8) . . ? C34 Si3 C36 104.4(8) . . ? C25 Si3 C36 108.3(7) . . ? C35 Si3 C36 109.6(8) . . ? C47 Si4 C46 105.3(9) . . ? C47 Si4 C37 113.2(8) . . ? C46 Si4 C37 114.8(8) . . ? C47 Si4 C48 109.1(8) . . ? C46 Si4 C48 108.0(9) . . ? C37 Si4 C48 106.3(7) . . ? C2 C1 C5 106.3(15) . . ? C2 C1 Si1 125.0(12) . . ? C5 C1 Si1 128.4(13) . . ? C2 C1 Y1 75.2(8) . . ? C5 C1 Y1 75.0(8) . . ? Si1 C1 Y1 120.2(6) . . ? C3 C2 C1 108.3(15) . . ? C3 C2 C6 126.7(16) . . ? C1 C2 C6 124.6(16) . . ? C3 C2 Y1 75.2(9) . . ? C1 C2 Y1 73.7(8) . . ? C6 C2 Y1 122.6(9) . . ? C4 C3 C2 108.3(16) . . ? C4 C3 C7 126.1(17) . . ? C2 C3 C7 125.6(16) . . ? C4 C3 Y1 74.9(9) . . ? C2 C3 Y1 74.3(9) . . ? C7 C3 Y1 117.4(10) . . ? C3 C4 C5 108.8(17) . . ? C3 C4 C8 124.6(16) . . ? C5 C4 C8 126.2(16) . . ? C3 C4 Y1 74.9(9) . . ? C5 C4 Y1 74.2(8) . . ? C8 C4 Y1 123.3(10) . . ? C4 C5 C1 108.3(15) . . ? C4 C5 C9 124.5(16) . . ? C1 C5 C9 127.0(16) . . ? C4 C5 Y1 75.5(8) . . ? C1 C5 Y1 73.8(8) . . ? C9 C5 Y1 120.4(9) . . ? C17 C13 C14 105.7(11) . . ? C17 C13 Si2 127.3(11) . . ? C14 C13 Si2 125.1(10) . . ? C17 C13 Y2 74.7(7) . . ? C14 C13 Y2 74.9(7) . . ? Si2 C13 Y2 128.0(6) . . ? C15 C14 C13 109.4(12) . . ? C15 C14 C18 123.9(13) . . ? C13 C14 C18 126.5(12) . . ? C15 C14 Y2 75.8(7) . . ? C13 C14 Y2 73.6(7) . . ? C18 C14 Y2 120.3(9) . . ? C16 C15 C14 107.6(13) . . ? C16 C15 C19 125.1(12) . . ? C14 C15 C19 126.7(13) . . ? C16 C15 Y2 75.8(8) . . ? C14 C15 Y2 73.8(7) . . ? C19 C15 Y2 122.8(9) . . ? C15 C16 C17 108.5(13) . . ? C15 C16 C20 125.6(13) . . ? C17 C16 C20 125.8(13) . . ? C15 C16 Y2 74.1(8) . . ? C17 C16 Y2 72.5(7) . . ? C20 C16 Y2 122.8(9) . . ? C16 C17 C13 108.7(12) . . ? C16 C17 C21 122.6(13) . . ? C13 C17 C21 128.4(12) . . ? C16 C17 Y2 76.9(8) . . ? C13 C17 Y2 74.2(7) . . ? C21 C17 Y2 120.0(9) . . ? C26 C25 C29 104.6(14) . . ? C26 C25 Si3 124.7(13) . . ? C29 C25 Si3 129.2(12) . . ? C26 C25 Y3 75.7(8) . . ? C29 C25 Y3 74.4(8) . . ? Si3 C25 Y3 126.0(6) . . ? C27 C26 C25 112.6(16) . . ? C27 C26 C30 123.4(15) . . ? C25 C26 C30 123.7(15) . . ? C27 C26 Y3 76.9(8) . . ? C25 C26 Y3 74.0(8) . . ? C30 C26 Y3 122.0(9) . . ? C26 C27 C28 105.3(14) . . ? C26 C27 C31 127.2(17) . . ? C28 C27 C31 127.2(15) . . ? C26 C27 Y3 73.3(8) . . ? C28 C27 Y3 73.7(8) . . ? C31 C27 Y3 122.4(9) . . ? C29 C28 C27 109.4(15) . . ? C29 C28 C32 128.5(17) . . ? C27 C28 C32 121.9(15) . . ? C29 C28 Y3 73.7(8) . . ? C27 C28 Y3 75.8(8) . . ? C32 C28 Y3 120.9(9) . . ? C28 C29 C25 108.1(15) . . ? C28 C29 C33 122.3(16) . . ? C25 C29 C33 129.6(15) . . ? C28 C29 Y3 76.2(8) . . ? C25 C29 Y3 73.9(8) . . ? C33 C29 Y3 114.7(9) . . ? C38 C37 C41 104.5(15) . . ? C38 C37 Si4 131.1(14) . . ? C41 C37 Si4 123.0(12) . . ? C38 C37 Y4 72.5(9) . . ? C41 C37 Y4 76.1(9) . . ? Si4 C37 Y4 126.2(7) . . ? C39 C38 C37 110.7(17) . . ? C39 C38 C42 122.3(18) . . ? C37 C38 C42 126.6(18) . . ? C39 C38 Y4 77.5(10) . . ? C37 C38 Y4 76.3(9) . . ? C42 C38 Y4 119.2(11) . . ? C38 C39 C40 106.9(17) . . ? C38 C39 C43 127.7(19) . . ? C40 C39 C43 125.2(19) . . ? C38 C39 Y4 71.8(10) . . ? C40 C39 Y4 76.1(9) . . ? C43 C39 Y4 121.3(10) . . ? C41 C40 C39 109.7(16) . . ? C41 C40 C44 125.1(18) . . ? C39 C40 C44 125.1(18) . . ? C41 C40 Y4 75.0(9) . . ? C39 C40 Y4 73.8(9) . . ? C44 C40 Y4 120.4(10) . . ? C40 C41 C37 108.2(15) . . ? C40 C41 C45 125.3(17) . . ? C37 C41 C45 126.2(15) . . ? C40 C41 Y4 75.2(9) . . ? C37 C41 Y4 72.4(8) . . ? C45 C41 Y4 123.4(10) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.890 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.091 data_5Lu _database_code_depnum_ccdc_archive 'CCDC 767215' #TrackingRef '- DT-ART-02-2010-00006.cif' _database_code_depnum_ccdc_archive 'CCDC 767215' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H99 Lu4 N7 Si4' _chemical_formula_weight 1586.58 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.316(3) _cell_length_b 12.7783(14) _cell_length_c 41.196(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.302(2) _cell_angle_gamma 90.00 _cell_volume 12264(2) _cell_formula_units_Z 8 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 37488 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 27.56 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6208 _exptl_absorpt_coefficient_mu 6.496 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1396 _exptl_absorpt_correction_T_max 0.3565 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 37488 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.56 _reflns_number_total 13816 _reflns_number_gt 11964 _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 'ORTEP-III (Farrugia, 1997)' _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. Although there are solvent accessible voids in the structure, no lattice solvent was found. EADP was applied to C46-C48. SADI was applied to the four Lu-H1(mu4-H) bonds. Uiso of H1 is fixed. ; _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^)+(0.0215P)^2^+142.0753P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13816 _refine_ls_number_parameters 587 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.229 _refine_ls_restrained_S_all 1.229 _refine_ls_shift/su_max 0.075 _refine_ls_shift/su_mean 0.002 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 0.410237(14) 0.66770(2) 0.116209(8) 0.02091(8) Uani 1 1 d D . . Lu2 Lu 0.462727(13) 0.39952(2) 0.105551(8) 0.02036(8) Uani 1 1 d D . . Lu3 Lu 0.326697(13) 0.46011(2) 0.076149(8) 0.01858(7) Uani 1 1 d D . . Lu4 Lu 0.352595(15) 0.43931(2) 0.158714(8) 0.02354(8) Uani 1 1 d D . . N1 N 0.4923(3) 0.5738(5) 0.10701(17) 0.0277(15) Uani 1 1 d . . . H1A H 0.5195 0.5845 0.1235 0.033 Uiso 1 1 calc R . . H1B H 0.5074 0.5930 0.0876 0.033 Uiso 1 1 calc R . . N2 N 0.3428(3) 0.6398(5) 0.07479(17) 0.0290(15) Uani 1 1 d . . . H2A H 0.3566 0.6599 0.0551 0.035 Uiso 1 1 calc R . . H2B H 0.3096 0.6763 0.0783 0.035 Uiso 1 1 calc R . . N3 N 0.3724(3) 0.6188(5) 0.16511(16) 0.0291(15) Uani 1 1 d . . . H3A H 0.3395 0.6557 0.1689 0.035 Uiso 1 1 calc R . . H3B H 0.3985 0.6300 0.1821 0.035 Uiso 1 1 calc R . . N4 N 0.4517(3) 0.4173(5) 0.16062(17) 0.0313(16) Uani 1 1 d . . . H4A H 0.4707 0.4749 0.1690 0.038 Uiso 1 1 calc R . . H4B H 0.4630 0.3584 0.1720 0.038 Uiso 1 1 calc R . . N5 N 0.4182(3) 0.4498(5) 0.05682(16) 0.0267(14) Uani 1 1 d . . . H5A H 0.4312 0.5132 0.0496 0.032 Uiso 1 1 calc R . . H5B H 0.4212 0.3999 0.0409 0.032 Uiso 1 1 calc R . . N6 N 0.2799(3) 0.4938(5) 0.12347(16) 0.0275(15) Uani 1 1 d . . . H6A H 0.2715 0.5636 0.1259 0.033 Uiso 1 1 calc R . . H6B H 0.2471 0.4543 0.1251 0.033 Uiso 1 1 calc R . . N7 N 0.3679(3) 0.3179(5) 0.11218(16) 0.0233(14) Uani 1 1 d . . . Si1 Si 0.48600(11) 0.83588(18) 0.18496(7) 0.0381(6) Uani 1 1 d . . . Si2 Si 0.63281(10) 0.40962(19) 0.12219(6) 0.0336(5) Uani 1 1 d . . . Si3 Si 0.16482(10) 0.54357(17) 0.04789(7) 0.0320(5) Uani 1 1 d . . . Si4 Si 0.26628(14) 0.5391(2) 0.23535(7) 0.0494(7) Uani 1 1 d . . . C1 C 0.4537(3) 0.8352(6) 0.1429(2) 0.0282(18) Uani 1 1 d . . . C2 C 0.3966(4) 0.8651(5) 0.1314(2) 0.0282(18) Uani 1 1 d . . . C3 C 0.3946(4) 0.8650(6) 0.0972(2) 0.035(2) Uani 1 1 d . . . C4 C 0.4487(4) 0.8344(6) 0.0868(2) 0.039(2) Uani 1 1 d . . . C5 C 0.4852(4) 0.8204(6) 0.1141(2) 0.034(2) Uani 1 1 d . . . C6 C 0.3488(4) 0.9006(7) 0.1522(2) 0.042(2) Uani 1 1 d . . . H6C H 0.3149 0.9172 0.1383 0.064 Uiso 1 1 calc R . . H6D H 0.3610 0.9631 0.1644 0.064 Uiso 1 1 calc R . . H6E H 0.3395 0.8446 0.1673 0.064 Uiso 1 1 calc R . . C7 C 0.3442(5) 0.9007(7) 0.0759(3) 0.051(3) Uani 1 1 d . . . H7A H 0.3435 0.9773 0.0752 0.076 Uiso 1 1 calc R . . H7B H 0.3085 0.8750 0.0849 0.076 Uiso 1 1 calc R . . H7C H 0.3478 0.8730 0.0539 0.076 Uiso 1 1 calc R . . C8 C 0.4651(6) 0.8275(9) 0.0514(3) 0.069(4) Uani 1 1 d . . . H8A H 0.4377 0.7823 0.0394 0.103 Uiso 1 1 calc R . . H8B H 0.5038 0.7980 0.0503 0.103 Uiso 1 1 calc R . . H8C H 0.4644 0.8976 0.0418 0.103 Uiso 1 1 calc R . . C9 C 0.5489(4) 0.8016(7) 0.1133(3) 0.055(3) Uani 1 1 d . . . H9A H 0.5573 0.7611 0.0938 0.082 Uiso 1 1 calc R . . H9B H 0.5619 0.7627 0.1327 0.082 Uiso 1 1 calc R . . H9C H 0.5690 0.8689 0.1127 0.082 Uiso 1 1 calc R . . C10 C 0.4314(5) 0.8601(9) 0.2162(3) 0.059(3) Uani 1 1 d . . . H10A H 0.4161 0.9312 0.2136 0.089 Uiso 1 1 calc R . . H10B H 0.4495 0.8526 0.2380 0.089 Uiso 1 1 calc R . . H10C H 0.4001 0.8094 0.2134 0.089 Uiso 1 1 calc R . . C11 C 0.5211(5) 0.7088(8) 0.1959(3) 0.059(3) Uani 1 1 d . . . H11A H 0.4919 0.6537 0.1965 0.088 Uiso 1 1 calc R . . H11B H 0.5407 0.7148 0.2173 0.088 Uiso 1 1 calc R . . H11C H 0.5490 0.6910 0.1796 0.088 Uiso 1 1 calc R . . C12 C 0.5405(5) 0.9425(8) 0.1892(3) 0.069(4) Uani 1 1 d . . . H12A H 0.5675 0.9369 0.1717 0.103 Uiso 1 1 calc R . . H12B H 0.5613 0.9361 0.2103 0.103 Uiso 1 1 calc R . . H12C H 0.5211 1.0106 0.1879 0.103 Uiso 1 1 calc R . . C13 C 0.5692(3) 0.3375(5) 0.1050(2) 0.0244(17) Uani 1 1 d . . . C14 C 0.5472(3) 0.3301(6) 0.0721(2) 0.0293(18) Uani 1 1 d . . . C15 C 0.5070(3) 0.2481(6) 0.0698(2) 0.032(2) Uani 1 1 d . . . C16 C 0.5028(3) 0.2041(6) 0.1009(2) 0.035(2) Uani 1 1 d . . . C17 C 0.5407(3) 0.2565(6) 0.1229(2) 0.0287(18) Uani 1 1 d . . . C18 C 0.5635(4) 0.3978(7) 0.0439(2) 0.041(2) Uani 1 1 d . . . H18A H 0.5364 0.3860 0.0255 0.062 Uiso 1 1 calc R . . H18B H 0.6024 0.3797 0.0376 0.062 Uiso 1 1 calc R . . H18C H 0.5624 0.4715 0.0503 0.062 Uiso 1 1 calc R . . C19 C 0.4773(4) 0.2075(8) 0.0395(3) 0.054(3) Uani 1 1 d . . . H19A H 0.4936 0.1394 0.0339 0.082 Uiso 1 1 calc R . . H19B H 0.4828 0.2568 0.0216 0.082 Uiso 1 1 calc R . . H19C H 0.4362 0.1996 0.0430 0.082 Uiso 1 1 calc R . . C20 C 0.4676(4) 0.1082(6) 0.1087(3) 0.049(3) Uani 1 1 d . . . H20A H 0.4310 0.1102 0.0962 0.073 Uiso 1 1 calc R . . H20B H 0.4603 0.1074 0.1320 0.073 Uiso 1 1 calc R . . H20C H 0.4888 0.0449 0.1031 0.073 Uiso 1 1 calc R . . C21 C 0.5539(4) 0.2251(7) 0.1575(2) 0.043(2) Uani 1 1 d . . . H21A H 0.5189 0.1994 0.1672 0.064 Uiso 1 1 calc R . . H21B H 0.5686 0.2858 0.1698 0.064 Uiso 1 1 calc R . . H21C H 0.5830 0.1696 0.1581 0.064 Uiso 1 1 calc R . . C22 C 0.6918(4) 0.3121(9) 0.1308(4) 0.076(4) Uani 1 1 d . . . H22A H 0.6786 0.2589 0.1459 0.114 Uiso 1 1 calc R . . H22B H 0.7254 0.3481 0.1405 0.114 Uiso 1 1 calc R . . H22C H 0.7022 0.2785 0.1105 0.114 Uiso 1 1 calc R . . C23 C 0.6609(5) 0.5115(9) 0.0945(3) 0.072(4) Uani 1 1 d . . . H23A H 0.6790 0.4776 0.0762 0.108 Uiso 1 1 calc R . . H23B H 0.6892 0.5549 0.1065 0.108 Uiso 1 1 calc R . . H23C H 0.6291 0.5556 0.0863 0.108 Uiso 1 1 calc R . . C24 C 0.6196(5) 0.4776(9) 0.1613(3) 0.062(3) Uani 1 1 d . . . H24A H 0.5806 0.5065 0.1606 0.093 Uiso 1 1 calc R . . H24B H 0.6474 0.5344 0.1646 0.093 Uiso 1 1 calc R . . H24C H 0.6237 0.4275 0.1793 0.093 Uiso 1 1 calc R . . C25 C 0.2291(3) 0.4568(5) 0.04384(19) 0.0213(15) Uani 1 1 d . . . C26 C 0.2344(3) 0.3542(5) 0.05739(19) 0.0209(15) Uani 1 1 d . . . C27 C 0.2794(3) 0.3019(6) 0.04235(19) 0.0227(16) Uani 1 1 d . . . C28 C 0.3020(3) 0.3700(6) 0.01869(19) 0.0233(16) Uani 1 1 d . . . C29 C 0.2711(3) 0.4648(6) 0.01965(19) 0.0236(16) Uani 1 1 d . . . C30 C 0.1961(4) 0.3055(6) 0.0816(2) 0.033(2) Uani 1 1 d . . . H30A H 0.1589 0.2884 0.0709 0.049 Uiso 1 1 calc R . . H30B H 0.1903 0.3548 0.0994 0.049 Uiso 1 1 calc R . . H30C H 0.2140 0.2414 0.0902 0.049 Uiso 1 1 calc R . . C31 C 0.2977(4) 0.1891(6) 0.0471(2) 0.033(2) Uani 1 1 d . . . H31A H 0.2767 0.1583 0.0649 0.049 Uiso 1 1 calc R . . H31B H 0.3390 0.1863 0.0525 0.049 Uiso 1 1 calc R . . H31C H 0.2892 0.1497 0.0271 0.049 Uiso 1 1 calc R . . C32 C 0.3456(4) 0.3415(7) -0.0058(2) 0.037(2) Uani 1 1 d . . . H32A H 0.3258 0.3221 -0.0264 0.055 Uiso 1 1 calc R . . H32B H 0.3687 0.2823 0.0023 0.055 Uiso 1 1 calc R . . H32C H 0.3707 0.4017 -0.0094 0.055 Uiso 1 1 calc R . . C33 C 0.2808(4) 0.5558(6) -0.0028(2) 0.035(2) Uani 1 1 d . . . H33A H 0.3204 0.5544 -0.0098 0.052 Uiso 1 1 calc R . . H33B H 0.2739 0.6215 0.0087 0.052 Uiso 1 1 calc R . . H33C H 0.2543 0.5507 -0.0218 0.052 Uiso 1 1 calc R . . C34 C 0.1760(5) 0.6807(7) 0.0335(3) 0.062(3) Uani 1 1 d . . . H34A H 0.1418 0.7225 0.0375 0.093 Uiso 1 1 calc R . . H34B H 0.1828 0.6801 0.0102 0.093 Uiso 1 1 calc R . . H34C H 0.2093 0.7112 0.0453 0.093 Uiso 1 1 calc R . . C35 C 0.1058(4) 0.4844(9) 0.0217(3) 0.073(4) Uani 1 1 d . . . H35A H 0.0726 0.5316 0.0208 0.110 Uiso 1 1 calc R . . H35B H 0.0946 0.4170 0.0308 0.110 Uiso 1 1 calc R . . H35C H 0.1193 0.4737 -0.0003 0.110 Uiso 1 1 calc R . . C36 C 0.1389(4) 0.5563(8) 0.0898(3) 0.053(3) Uani 1 1 d . . . H36A H 0.1286 0.4870 0.0980 0.080 Uiso 1 1 calc R . . H36B H 0.1052 0.6020 0.0896 0.080 Uiso 1 1 calc R . . H36C H 0.1694 0.5865 0.1040 0.080 Uiso 1 1 calc R . . C37 C 0.2988(4) 0.4286(7) 0.2126(2) 0.033(2) Uani 1 1 d . . . C38 C 0.2655(4) 0.3608(7) 0.1910(2) 0.036(2) Uani 1 1 d . . . C39 C 0.2991(4) 0.2734(7) 0.1837(2) 0.036(2) Uani 1 1 d . . . C40 C 0.3523(4) 0.2821(7) 0.2005(2) 0.039(2) Uani 1 1 d . . . C41 C 0.3519(4) 0.3764(7) 0.2188(2) 0.039(2) Uani 1 1 d . . . C42 C 0.2032(4) 0.3734(8) 0.1804(2) 0.046(2) Uani 1 1 d . . . H42A H 0.1940 0.3263 0.1622 0.069 Uiso 1 1 calc R . . H42B H 0.1960 0.4459 0.1736 0.069 Uiso 1 1 calc R . . H42C H 0.1790 0.3562 0.1986 0.069 Uiso 1 1 calc R . . C43 C 0.2792(5) 0.1807(7) 0.1626(3) 0.057(3) Uani 1 1 d . . . H43A H 0.3127 0.1405 0.1562 0.085 Uiso 1 1 calc R . . H43B H 0.2581 0.2066 0.1432 0.085 Uiso 1 1 calc R . . H43C H 0.2541 0.1357 0.1751 0.085 Uiso 1 1 calc R . . C44 C 0.3992(5) 0.2004(8) 0.2018(3) 0.059(3) Uani 1 1 d . . . H44A H 0.3900 0.1464 0.2177 0.089 Uiso 1 1 calc R . . H44B H 0.4358 0.2335 0.2083 0.089 Uiso 1 1 calc R . . H44C H 0.4021 0.1684 0.1803 0.089 Uiso 1 1 calc R . . C45 C 0.4003(5) 0.4111(11) 0.2413(3) 0.067(3) Uani 1 1 d . . . H45A H 0.3910 0.3952 0.2638 0.101 Uiso 1 1 calc R . . H45B H 0.4061 0.4867 0.2390 0.101 Uiso 1 1 calc R . . H45C H 0.4355 0.3742 0.2359 0.101 Uiso 1 1 calc R . . C46 C 0.3199(6) 0.6293(10) 0.2559(3) 0.082(2) Uani 1 1 d . . . H46A H 0.3441 0.5896 0.2715 0.123 Uiso 1 1 calc R . . H46B H 0.2996 0.6844 0.2674 0.123 Uiso 1 1 calc R . . H46C H 0.3439 0.6611 0.2396 0.123 Uiso 1 1 calc R . . C47 C 0.2196(6) 0.6261(10) 0.2091(3) 0.082(2) Uani 1 1 d . . . H47A H 0.2393 0.6433 0.1892 0.123 Uiso 1 1 calc R . . H47B H 0.2114 0.6906 0.2209 0.123 Uiso 1 1 calc R . . H47C H 0.1835 0.5900 0.2033 0.123 Uiso 1 1 calc R . . C48 C 0.2223(6) 0.4796(10) 0.2671(3) 0.082(2) Uani 1 1 d . . . H48A H 0.1913 0.4381 0.2567 0.123 Uiso 1 1 calc R . . H48B H 0.2058 0.5350 0.2803 0.123 Uiso 1 1 calc R . . H48C H 0.2465 0.4342 0.2811 0.123 Uiso 1 1 calc R . . H1 H 0.3896(5) 0.5010(9) 0.1148(3) 0.050 Uiso 1 1 d D . . 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 0.02430(17) 0.01433(14) 0.02418(18) -0.00146(12) 0.00219(13) -0.00189(12) Lu2 0.01971(16) 0.01665(14) 0.02479(18) -0.00223(12) 0.00162(12) 0.00055(11) Lu3 0.01947(15) 0.01648(14) 0.01988(17) -0.00179(12) 0.00188(12) -0.00111(11) Lu4 0.02964(18) 0.02085(15) 0.02053(17) -0.00014(12) 0.00593(13) -0.00160(13) N1 0.025(4) 0.022(3) 0.037(4) 0.002(3) 0.002(3) -0.006(3) N2 0.028(4) 0.022(3) 0.037(4) 0.000(3) 0.000(3) 0.003(3) N3 0.027(4) 0.033(4) 0.027(4) 0.002(3) -0.002(3) 0.008(3) N4 0.032(4) 0.024(3) 0.038(4) 0.002(3) 0.003(3) 0.005(3) N5 0.023(3) 0.029(3) 0.029(4) -0.005(3) 0.001(3) 0.000(3) N6 0.029(4) 0.022(3) 0.032(4) -0.005(3) 0.009(3) -0.004(3) N7 0.023(3) 0.020(3) 0.027(4) -0.002(3) 0.003(3) -0.004(2) Si1 0.0398(15) 0.0243(11) 0.0488(17) -0.0023(11) -0.0154(12) -0.0011(10) Si2 0.0279(13) 0.0334(12) 0.0395(15) -0.0018(10) -0.0001(11) -0.0068(10) Si3 0.0256(12) 0.0224(11) 0.0481(16) 0.0009(10) 0.0039(11) 0.0058(9) Si4 0.0601(19) 0.0482(16) 0.0412(17) -0.0108(13) 0.0198(14) 0.0013(14) C1 0.029(4) 0.019(4) 0.035(5) -0.003(3) -0.007(4) -0.005(3) C2 0.034(5) 0.013(3) 0.037(5) -0.008(3) -0.005(4) -0.003(3) C3 0.044(5) 0.016(4) 0.045(6) 0.002(3) -0.009(4) -0.006(3) C4 0.062(6) 0.021(4) 0.034(5) 0.003(4) 0.014(5) -0.018(4) C5 0.033(5) 0.020(4) 0.049(6) -0.006(4) 0.007(4) -0.008(3) C6 0.034(5) 0.035(5) 0.058(7) -0.018(4) 0.002(5) 0.005(4) C7 0.073(7) 0.019(4) 0.058(7) 0.005(4) -0.021(6) -0.004(4) C8 0.106(10) 0.054(7) 0.049(7) 0.000(6) 0.030(7) -0.022(7) C9 0.039(6) 0.029(5) 0.098(9) -0.017(5) 0.025(6) -0.017(4) C10 0.076(8) 0.067(7) 0.035(6) -0.005(5) -0.008(6) 0.006(6) C11 0.060(7) 0.043(6) 0.070(8) -0.002(5) -0.034(6) 0.008(5) C12 0.072(8) 0.053(7) 0.079(9) 0.006(6) -0.038(7) -0.034(6) C13 0.019(4) 0.019(3) 0.036(5) -0.003(3) 0.003(3) 0.000(3) C14 0.026(4) 0.026(4) 0.037(5) -0.003(3) 0.011(4) 0.009(3) C15 0.021(4) 0.027(4) 0.047(6) -0.012(4) -0.007(4) 0.008(3) C16 0.023(4) 0.019(4) 0.064(7) -0.004(4) 0.007(4) 0.001(3) C17 0.023(4) 0.021(4) 0.043(5) 0.002(3) 0.007(4) 0.007(3) C18 0.034(5) 0.052(6) 0.039(6) 0.001(4) 0.009(4) 0.006(4) C19 0.033(5) 0.059(6) 0.070(8) -0.037(6) -0.008(5) 0.016(5) C20 0.027(5) 0.019(4) 0.100(9) -0.005(5) 0.000(5) 0.001(3) C21 0.041(6) 0.040(5) 0.048(6) 0.024(4) 0.008(5) 0.004(4) C22 0.025(6) 0.070(8) 0.131(13) -0.001(8) -0.021(7) -0.003(5) C23 0.078(9) 0.063(7) 0.074(9) 0.010(6) 0.002(7) -0.044(7) C24 0.060(7) 0.084(8) 0.042(7) -0.021(6) -0.001(5) -0.018(6) C25 0.022(4) 0.013(3) 0.029(4) 0.002(3) -0.004(3) 0.002(3) C26 0.016(4) 0.018(3) 0.029(4) -0.002(3) -0.002(3) -0.003(3) C27 0.020(4) 0.024(4) 0.023(4) -0.005(3) -0.004(3) 0.001(3) C28 0.021(4) 0.029(4) 0.019(4) -0.005(3) -0.004(3) -0.002(3) C29 0.017(4) 0.029(4) 0.024(4) -0.003(3) -0.002(3) 0.000(3) C30 0.034(5) 0.023(4) 0.042(5) 0.002(4) 0.010(4) -0.005(3) C31 0.029(4) 0.020(4) 0.049(6) -0.006(4) -0.004(4) 0.002(3) C32 0.027(5) 0.047(5) 0.035(5) -0.018(4) 0.000(4) 0.002(4) C33 0.032(5) 0.035(5) 0.036(5) 0.009(4) 0.002(4) -0.003(4) C34 0.061(7) 0.036(5) 0.091(9) 0.014(6) 0.016(7) 0.022(5) C35 0.032(6) 0.067(8) 0.119(12) -0.020(7) -0.022(6) 0.015(5) C36 0.044(6) 0.045(6) 0.072(8) 0.001(5) 0.021(5) 0.019(5) C37 0.041(5) 0.038(5) 0.021(4) 0.006(4) 0.012(4) 0.002(4) C38 0.042(5) 0.035(5) 0.031(5) 0.008(4) 0.012(4) -0.011(4) C39 0.047(6) 0.033(5) 0.029(5) 0.001(4) 0.011(4) -0.005(4) C40 0.045(6) 0.040(5) 0.035(5) 0.022(4) 0.018(4) 0.006(4) C41 0.049(6) 0.051(6) 0.018(5) 0.009(4) 0.006(4) -0.004(4) C42 0.038(5) 0.058(6) 0.043(6) 0.007(5) 0.018(5) -0.010(5) C43 0.080(8) 0.034(5) 0.058(7) -0.001(5) 0.018(6) -0.022(5) C44 0.066(8) 0.047(6) 0.066(8) 0.023(5) 0.025(6) 0.019(5) C45 0.062(8) 0.111(10) 0.027(6) 0.011(6) -0.002(5) 0.001(7) C46 0.103(7) 0.068(5) 0.077(6) -0.016(4) 0.028(5) -0.008(4) C47 0.103(7) 0.068(5) 0.077(6) -0.016(4) 0.028(5) -0.008(4) C48 0.103(7) 0.068(5) 0.077(6) -0.016(4) 0.028(5) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 N2 2.302(7) . ? Lu1 N1 2.302(6) . ? Lu1 N3 2.317(7) . ? Lu1 C1 2.594(7) . ? Lu1 C2 2.621(7) . ? Lu1 C5 2.623(8) . ? Lu1 C4 2.627(8) . ? Lu1 C3 2.661(8) . ? Lu1 Lu3 3.6464(5) . ? Lu1 Lu2 3.6712(5) . ? Lu1 Lu4 3.6850(5) . ? Lu2 N4 2.305(7) . ? Lu2 N5 2.314(7) . ? Lu2 N1 2.332(6) . ? Lu2 N7 2.470(6) . ? Lu2 C14 2.604(7) . ? Lu2 C13 2.607(7) . ? Lu2 C17 2.655(8) . ? Lu2 C15 2.664(8) . ? Lu2 C16 2.676(8) . ? Lu2 Lu3 3.4377(6) . ? Lu2 Lu4 3.4786(5) . ? Lu3 N5 2.310(6) . ? Lu3 N6 2.312(6) . ? Lu3 N2 2.328(6) . ? Lu3 N7 2.513(6) . ? Lu3 C25 2.591(7) . ? Lu3 C29 2.619(8) . ? Lu3 C26 2.633(7) . ? Lu3 C27 2.668(7) . ? Lu3 C28 2.674(7) . ? Lu3 Lu4 3.4409(6) . ? Lu4 N6 2.295(7) . ? Lu4 N4 2.327(7) . ? Lu4 N3 2.353(7) . ? Lu4 N7 2.503(6) . ? Lu4 C37 2.598(8) . ? Lu4 C41 2.603(8) . ? Lu4 C40 2.646(8) . ? Lu4 C38 2.666(8) . ? Lu4 C39 2.685(8) . ? Si1 C1 1.861(9) . ? Si1 C12 1.866(10) . ? Si1 C11 1.865(10) . ? Si1 C10 1.871(11) . ? Si2 C13 1.861(8) . ? Si2 C23 1.867(10) . ? Si2 C24 1.867(10) . ? Si2 C22 1.879(11) . ? Si3 C36 1.861(10) . ? Si3 C34 1.871(10) . ? Si3 C35 1.874(11) . ? Si3 C25 1.876(7) . ? Si4 C48 1.857(12) . ? Si4 C37 1.870(9) . ? Si4 C46 1.878(13) . ? Si4 C47 1.871(14) . ? C1 C5 1.431(12) . ? C1 C2 1.447(11) . ? C2 C3 1.407(12) . ? C2 C6 1.503(11) . ? C3 C4 1.405(13) . ? C3 C7 1.507(13) . ? C4 C5 1.396(13) . ? C4 C8 1.524(13) . ? C5 C9 1.508(12) . ? C13 C14 1.434(12) . ? C13 C17 1.448(10) . ? C14 C15 1.406(11) . ? C14 C18 1.509(12) . ? C15 C16 1.404(13) . ? C15 C19 1.498(12) . ? C16 C17 1.412(12) . ? C16 C20 1.517(11) . ? C17 C21 1.500(12) . ? C25 C26 1.429(9) . ? C25 C29 1.429(10) . ? C26 C27 1.410(10) . ? C26 C30 1.499(10) . ? C27 C28 1.423(10) . ? C27 C31 1.513(10) . ? C28 C29 1.410(10) . ? C28 C32 1.506(10) . ? C29 C33 1.508(11) . ? C37 C41 1.421(13) . ? C37 C38 1.448(12) . ? C38 C39 1.402(12) . ? C38 C42 1.510(13) . ? C39 C40 1.400(13) . ? C39 C43 1.529(13) . ? C40 C41 1.420(13) . ? C40 C44 1.511(13) . ? C41 C45 1.500(14) . ? 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 N1 110.2(2) . . ? N2 Lu1 N3 109.3(2) . . ? N1 Lu1 N3 110.5(2) . . ? N2 Lu1 C1 133.3(2) . . ? N1 Lu1 C1 100.7(2) . . ? N3 Lu1 C1 90.5(3) . . ? N2 Lu1 C2 103.9(2) . . ? N1 Lu1 C2 130.5(2) . . ? N3 Lu1 C2 89.9(2) . . ? C1 Lu1 C2 32.2(2) . . ? N2 Lu1 C5 121.8(3) . . ? N1 Lu1 C5 79.8(2) . . ? N3 Lu1 C5 120.4(3) . . ? C1 Lu1 C5 31.8(3) . . ? C2 Lu1 C5 51.6(3) . . ? N2 Lu1 C4 91.1(3) . . ? N1 Lu1 C4 92.6(3) . . ? N3 Lu1 C4 140.3(3) . . ? C1 Lu1 C4 52.5(3) . . ? C2 Lu1 C4 51.4(3) . . ? C5 Lu1 C4 30.8(3) . . ? N2 Lu1 C3 81.2(2) . . ? N1 Lu1 C3 123.4(3) . . ? N3 Lu1 C3 117.3(3) . . ? C1 Lu1 C3 52.4(3) . . ? C2 Lu1 C3 30.9(3) . . ? C5 Lu1 C3 50.9(3) . . ? C4 Lu1 C3 30.8(3) . . ? N2 Lu1 Lu3 38.29(15) . . ? N1 Lu1 Lu3 88.78(16) . . ? N3 Lu1 Lu3 89.00(17) . . ? C1 Lu1 Lu3 169.98(18) . . ? C2 Lu1 Lu3 137.77(18) . . ? C5 Lu1 Lu3 150.6(2) . . ? C4 Lu1 Lu3 124.6(2) . . ? C3 Lu1 Lu3 119.44(19) . . ? N2 Lu1 Lu2 89.31(15) . . ? N1 Lu1 Lu2 37.88(15) . . ? N3 Lu1 Lu2 89.58(16) . . ? C1 Lu1 Lu2 133.97(18) . . ? C2 Lu1 Lu2 166.17(18) . . ? C5 Lu1 Lu2 117.70(18) . . ? C4 Lu1 Lu2 125.4(2) . . ? C3 Lu1 Lu2 153.1(2) . . ? Lu3 Lu1 Lu2 56.040(10) . . ? N2 Lu1 Lu4 88.76(16) . . ? N1 Lu1 Lu4 89.25(15) . . ? N3 Lu1 Lu4 38.24(16) . . ? C1 Lu1 Lu4 126.57(19) . . ? C2 Lu1 Lu4 126.81(19) . . ? C5 Lu1 Lu4 149.4(2) . . ? C4 Lu1 Lu4 178.1(2) . . ? C3 Lu1 Lu4 147.3(2) . . ? Lu3 Lu1 Lu4 55.979(11) . . ? Lu2 Lu1 Lu4 56.444(10) . . ? N4 Lu2 N5 139.7(2) . . ? N4 Lu2 N1 85.7(2) . . ? N5 Lu2 N1 83.1(2) . . ? N4 Lu2 N7 78.3(2) . . ? N5 Lu2 N7 80.8(2) . . ? N1 Lu2 N7 131.7(2) . . ? N4 Lu2 C14 132.2(3) . . ? N5 Lu2 C14 87.6(2) . . ? N1 Lu2 C14 96.3(2) . . ? N7 Lu2 C14 127.9(2) . . ? N4 Lu2 C13 100.5(2) . . ? N5 Lu2 C13 118.1(2) . . ? N1 Lu2 C13 90.6(2) . . ? N7 Lu2 C13 136.9(2) . . ? C14 Lu2 C13 31.9(3) . . ? N4 Lu2 C17 84.5(2) . . ? N5 Lu2 C17 134.7(2) . . ? N1 Lu2 C17 116.9(2) . . ? N7 Lu2 C17 106.6(2) . . ? C14 Lu2 C17 52.0(3) . . ? C13 Lu2 C17 31.9(2) . . ? N4 Lu2 C15 132.6(3) . . ? N5 Lu2 C15 83.8(2) . . ? N1 Lu2 C15 126.0(2) . . ? N7 Lu2 C15 97.1(2) . . ? C14 Lu2 C15 30.9(2) . . ? C13 Lu2 C15 52.0(2) . . ? C17 Lu2 C15 51.2(3) . . ? N4 Lu2 C16 102.5(3) . . ? N5 Lu2 C16 110.0(3) . . ? N1 Lu2 C16 142.2(2) . . ? N7 Lu2 C16 86.0(2) . . ? C14 Lu2 C16 51.0(3) . . ? C13 Lu2 C16 51.7(2) . . ? C17 Lu2 C16 30.7(3) . . ? C15 Lu2 C16 30.5(3) . . ? N4 Lu2 Lu3 100.78(17) . . ? N5 Lu2 Lu3 41.93(15) . . ? N1 Lu2 Lu3 93.52(16) . . ? N7 Lu2 Lu3 46.90(15) . . ? C14 Lu2 Lu3 126.6(2) . . ? C13 Lu2 Lu3 158.57(18) . . ? C17 Lu2 Lu3 149.53(18) . . ? C15 Lu2 Lu3 109.96(18) . . ? C16 Lu2 Lu3 120.29(19) . . ? N4 Lu2 Lu4 41.55(17) . . ? N5 Lu2 Lu4 100.87(15) . . ? N1 Lu2 Lu4 93.95(16) . . ? N7 Lu2 Lu4 46.00(14) . . ? C14 Lu2 Lu4 167.41(18) . . ? C13 Lu2 Lu4 141.00(18) . . ? C17 Lu2 Lu4 116.46(18) . . ? C15 Lu2 Lu4 140.01(19) . . ? C16 Lu2 Lu4 116.76(19) . . ? Lu3 Lu2 Lu4 59.666(12) . . ? N4 Lu2 Lu1 74.89(16) . . ? N5 Lu2 Lu1 72.81(16) . . ? N1 Lu2 Lu1 37.32(16) . . ? N7 Lu2 Lu1 94.40(14) . . ? C14 Lu2 Lu1 130.10(17) . . ? C13 Lu2 Lu1 127.36(16) . . ? C17 Lu2 Lu1 146.93(19) . . ? C15 Lu2 Lu1 151.9(2) . . ? C16 Lu2 Lu1 177.2(2) . . ? Lu3 Lu2 Lu1 61.616(9) . . ? Lu4 Lu2 Lu1 61.979(9) . . ? N5 Lu3 N6 140.8(2) . . ? N5 Lu3 N2 84.0(2) . . ? N6 Lu3 N2 85.3(2) . . ? N5 Lu3 N7 80.0(2) . . ? N6 Lu3 N7 79.5(2) . . ? N2 Lu3 N7 132.0(2) . . ? N5 Lu3 C25 128.8(2) . . ? N6 Lu3 C25 90.1(2) . . ? N2 Lu3 C25 98.2(2) . . ? N7 Lu3 C25 126.8(2) . . ? N5 Lu3 C29 97.2(2) . . ? N6 Lu3 C29 120.8(2) . . ? N2 Lu3 C29 91.7(2) . . ? N7 Lu3 C29 134.9(2) . . ? C25 Lu3 C29 31.8(2) . . ? N5 Lu3 C26 128.7(2) . . ? N6 Lu3 C26 86.3(2) . . ? N2 Lu3 C26 129.1(2) . . ? N7 Lu3 C26 95.2(2) . . ? C25 Lu3 C26 31.7(2) . . ? C29 Lu3 C26 51.8(2) . . ? N5 Lu3 C27 98.3(2) . . ? N6 Lu3 C27 112.5(2) . . ? N2 Lu3 C27 143.0(2) . . ? N7 Lu3 C27 84.3(2) . . ? C25 Lu3 C27 52.0(2) . . ? C29 Lu3 C27 51.3(2) . . ? C26 Lu3 C27 30.9(2) . . ? N5 Lu3 C28 80.8(2) . . ? N6 Lu3 C28 137.2(2) . . ? N2 Lu3 C28 115.6(2) . . ? N7 Lu3 C28 106.0(2) . . ? C25 Lu3 C28 52.0(2) . . ? C29 Lu3 C28 30.9(2) . . ? C26 Lu3 C28 51.3(2) . . ? C27 Lu3 C28 30.9(2) . . ? N5 Lu3 Lu2 42.02(17) . . ? N6 Lu3 Lu2 101.81(17) . . ? N2 Lu3 Lu2 94.78(16) . . ? N7 Lu3 Lu2 45.85(14) . . ? C25 Lu3 Lu2 163.06(15) . . ? C29 Lu3 Lu2 137.31(16) . . ? C26 Lu3 Lu2 136.04(15) . . ? C27 Lu3 Lu2 111.66(16) . . ? C28 Lu3 Lu2 112.20(16) . . ? N5 Lu3 Lu4 102.03(17) . . ? N6 Lu3 Lu4 41.49(17) . . ? N2 Lu3 Lu4 94.47(17) . . ? N7 Lu3 Lu4 46.56(14) . . ? C25 Lu3 Lu4 128.48(17) . . ? C29 Lu3 Lu4 160.25(16) . . ? C26 Lu3 Lu4 111.07(17) . . ? C27 Lu3 Lu4 120.65(17) . . ? C28 Lu3 Lu4 149.86(16) . . ? Lu2 Lu3 Lu4 60.758(10) . . ? N5 Lu3 Lu1 73.37(16) . . ? N6 Lu3 Lu1 75.21(16) . . ? N2 Lu3 Lu1 37.78(17) . . ? N7 Lu3 Lu1 94.25(14) . . ? C25 Lu3 Lu1 133.36(15) . . ? C29 Lu3 Lu1 128.46(16) . . ? C26 Lu3 Lu1 157.29(15) . . ? C27 Lu3 Lu1 171.67(16) . . ? C28 Lu3 Lu1 143.70(16) . . ? Lu2 Lu3 Lu1 62.344(10) . . ? Lu4 Lu3 Lu1 62.578(10) . . ? N6 Lu4 N4 139.9(2) . . ? N6 Lu4 N3 85.0(2) . . ? N4 Lu4 N3 85.6(2) . . ? N6 Lu4 N7 80.1(2) . . ? N4 Lu4 N7 77.2(2) . . ? N3 Lu4 N7 131.1(2) . . ? N6 Lu4 C37 100.8(3) . . ? N4 Lu4 C37 118.5(3) . . ? N3 Lu4 C37 93.1(2) . . ? N7 Lu4 C37 135.3(2) . . ? N6 Lu4 C41 131.5(3) . . ? N4 Lu4 C41 88.5(3) . . ? N3 Lu4 C41 101.7(3) . . ? N7 Lu4 C41 122.9(3) . . ? C37 Lu4 C41 31.7(3) . . ? N6 Lu4 C40 128.4(3) . . ? N4 Lu4 C40 85.1(3) . . ? N3 Lu4 C40 132.3(3) . . ? N7 Lu4 C40 91.8(3) . . ? C37 Lu4 C40 52.4(3) . . ? C41 Lu4 C40 31.4(3) . . ? N6 Lu4 C38 82.6(3) . . ? N4 Lu4 C38 135.5(3) . . ? N3 Lu4 C38 117.5(2) . . ? N7 Lu4 C38 106.5(2) . . ? C37 Lu4 C38 31.9(3) . . ? C41 Lu4 C38 51.4(3) . . ? C40 Lu4 C38 50.8(3) . . ? N6 Lu4 C39 98.0(3) . . ? N4 Lu4 C39 111.6(3) . . ? N3 Lu4 C39 145.0(2) . . ? N7 Lu4 C39 83.5(2) . . ? C37 Lu4 C39 51.9(3) . . ? C41 Lu4 C39 51.0(3) . . ? C40 Lu4 C39 30.4(3) . . ? C38 Lu4 C39 30.4(3) . . ? N6 Lu4 Lu3 41.88(15) . . ? N4 Lu4 Lu3 100.21(17) . . ? N3 Lu4 Lu3 93.52(16) . . ? N7 Lu4 Lu3 46.80(15) . . ? C37 Lu4 Lu3 141.1(2) . . ? C41 Lu4 Lu3 163.0(2) . . ? C40 Lu4 Lu3 134.2(2) . . ? C38 Lu4 Lu3 114.5(2) . . ? C39 Lu4 Lu3 112.0(2) . . ? N6 Lu4 Lu2 101.02(15) . . ? N4 Lu4 Lu2 41.07(17) . . ? N3 Lu4 Lu2 93.80(16) . . ? N7 Lu4 Lu2 45.22(14) . . ? C37 Lu4 Lu2 157.6(2) . . ? C41 Lu4 Lu2 125.9(2) . . ? C40 Lu4 Lu2 108.68(19) . . ? C38 Lu4 Lu2 148.73(19) . . ? C39 Lu4 Lu2 119.47(19) . . ? Lu3 Lu4 Lu2 59.576(11) . . ? N6 Lu4 Lu1 74.54(16) . . ? N4 Lu4 Lu1 74.38(16) . . ? N3 Lu4 Lu1 37.56(16) . . ? N7 Lu4 Lu1 93.50(14) . . ? C37 Lu4 Lu1 130.22(19) . . ? C41 Lu4 Lu1 135.5(2) . . ? C40 Lu4 Lu1 157.1(2) . . ? C38 Lu4 Lu1 146.5(2) . . ? C39 Lu4 Lu1 172.4(2) . . ? Lu3 Lu4 Lu1 61.443(9) . . ? Lu2 Lu4 Lu1 61.578(10) . . ? Lu1 N1 Lu2 104.8(2) . . ? Lu1 N2 Lu3 103.9(3) . . ? Lu1 N3 Lu4 104.2(3) . . ? Lu2 N4 Lu4 97.4(3) . . ? Lu3 N5 Lu2 96.1(2) . . ? Lu4 N6 Lu3 96.6(2) . . ? Lu2 N7 Lu4 88.79(19) . . ? Lu2 N7 Lu3 87.25(19) . . ? Lu4 N7 Lu3 86.64(19) . . ? C1 Si1 C12 109.8(5) . . ? C1 Si1 C11 112.2(4) . . ? C12 Si1 C11 108.9(5) . . ? C1 Si1 C10 112.3(4) . . ? C12 Si1 C10 107.1(6) . . ? C11 Si1 C10 106.3(5) . . ? C13 Si2 C23 114.0(5) . . ? C13 Si2 C24 113.7(4) . . ? C23 Si2 C24 106.1(6) . . ? C13 Si2 C22 108.1(4) . . ? C23 Si2 C22 107.8(6) . . ? C24 Si2 C22 106.9(6) . . ? C36 Si3 C34 105.5(5) . . ? C36 Si3 C35 108.2(6) . . ? C34 Si3 C35 107.7(6) . . ? C36 Si3 C25 115.1(4) . . ? C34 Si3 C25 113.8(4) . . ? C35 Si3 C25 106.3(4) . . ? C48 Si4 C37 106.9(5) . . ? C48 Si4 C46 108.1(6) . . ? C37 Si4 C46 114.4(5) . . ? C48 Si4 C47 109.0(6) . . ? C37 Si4 C47 113.4(5) . . ? C46 Si4 C47 104.9(6) . . ? C5 C1 C2 104.9(7) . . ? C5 C1 Si1 124.8(7) . . ? C2 C1 Si1 129.6(6) . . ? C5 C1 Lu1 75.2(4) . . ? C2 C1 Lu1 74.9(4) . . ? Si1 C1 Lu1 122.4(4) . . ? C3 C2 C1 108.8(7) . . ? C3 C2 C6 125.1(8) . . ? C1 C2 C6 125.8(8) . . ? C3 C2 Lu1 76.1(4) . . ? C1 C2 Lu1 72.8(4) . . ? C6 C2 Lu1 121.7(5) . . ? C4 C3 C2 108.1(8) . . ? C4 C3 C7 126.6(9) . . ? C2 C3 C7 125.1(9) . . ? C4 C3 Lu1 73.3(4) . . ? C2 C3 Lu1 73.0(4) . . ? C7 C3 Lu1 123.5(5) . . ? C5 C4 C3 108.3(8) . . ? C5 C4 C8 126.7(10) . . ? C3 C4 C8 124.8(10) . . ? C5 C4 Lu1 74.4(5) . . ? C3 C4 Lu1 75.9(4) . . ? C8 C4 Lu1 119.8(6) . . ? C4 C5 C1 109.6(8) . . ? C4 C5 C9 124.8(9) . . ? C1 C5 C9 125.4(9) . . ? C4 C5 Lu1 74.7(5) . . ? C1 C5 Lu1 72.9(4) . . ? C9 C5 Lu1 122.8(5) . . ? C14 C13 C17 106.3(7) . . ? C14 C13 Si2 130.0(6) . . ? C17 C13 Si2 122.3(6) . . ? C14 C13 Lu2 73.9(4) . . ? C17 C13 Lu2 75.9(4) . . ? Si2 C13 Lu2 126.2(3) . . ? C15 C14 C13 108.9(7) . . ? C15 C14 C18 124.4(8) . . ? C13 C14 C18 126.7(8) . . ? C15 C14 Lu2 76.9(4) . . ? C13 C14 Lu2 74.1(4) . . ? C18 C14 Lu2 115.6(5) . . ? C16 C15 C14 108.0(8) . . ? C16 C15 C19 125.1(8) . . ? C14 C15 C19 126.7(9) . . ? C16 C15 Lu2 75.2(5) . . ? C14 C15 Lu2 72.2(4) . . ? C19 C15 Lu2 122.5(5) . . ? C15 C16 C17 109.3(7) . . ? C15 C16 C20 125.2(9) . . ? C17 C16 C20 125.2(9) . . ? C15 C16 Lu2 74.3(4) . . ? C17 C16 Lu2 73.9(4) . . ? C20 C16 Lu2 123.1(5) . . ? C16 C17 C13 107.5(8) . . ? C16 C17 C21 125.7(8) . . ? C13 C17 C21 126.5(8) . . ? C16 C17 Lu2 75.4(5) . . ? C13 C17 Lu2 72.2(4) . . ? C21 C17 Lu2 123.5(5) . . ? C26 C25 C29 106.7(6) . . ? C26 C25 Si3 124.4(5) . . ? C29 C25 Si3 126.3(5) . . ? C26 C25 Lu3 75.7(4) . . ? C29 C25 Lu3 75.2(4) . . ? Si3 C25 Lu3 129.3(4) . . ? C27 C26 C25 108.5(7) . . ? C27 C26 C30 124.7(7) . . ? C25 C26 C30 126.6(7) . . ? C27 C26 Lu3 75.9(4) . . ? C25 C26 Lu3 72.5(4) . . ? C30 C26 Lu3 121.4(5) . . ? C26 C27 C28 108.3(6) . . ? C26 C27 C31 127.2(7) . . ? C28 C27 C31 124.2(7) . . ? C26 C27 Lu3 73.2(4) . . ? C28 C27 Lu3 74.8(4) . . ? C31 C27 Lu3 123.1(5) . . ? C29 C28 C27 107.6(6) . . ? C29 C28 C32 125.9(7) . . ? C27 C28 C32 126.1(7) . . ? C29 C28 Lu3 72.4(4) . . ? C27 C28 Lu3 74.3(4) . . ? C32 C28 Lu3 124.8(5) . . ? C28 C29 C25 108.9(7) . . ? C28 C29 C33 123.8(7) . . ? C25 C29 C33 127.3(7) . . ? C28 C29 Lu3 76.7(4) . . ? C25 C29 Lu3 73.0(4) . . ? C33 C29 Lu3 118.8(5) . . ? C41 C37 C38 105.6(8) . . ? C41 C37 Si4 129.3(7) . . ? C38 C37 Si4 122.9(7) . . ? C41 C37 Lu4 74.3(5) . . ? C38 C37 Lu4 76.6(5) . . ? Si4 C37 Lu4 127.4(4) . . ? C39 C38 C37 108.6(8) . . ? C39 C38 C42 124.2(9) . . ? C37 C38 C42 126.9(8) . . ? C39 C38 Lu4 75.6(5) . . ? C37 C38 Lu4 71.5(4) . . ? C42 C38 Lu4 124.1(6) . . ? C40 C39 C38 108.8(8) . . ? C40 C39 C43 125.8(9) . . ? C38 C39 C43 125.3(9) . . ? C40 C39 Lu4 73.2(5) . . ? C38 C39 Lu4 74.1(5) . . ? C43 C39 Lu4 122.0(6) . . ? C39 C40 C41 107.8(8) . . ? C39 C40 C44 126.0(10) . . ? C41 C40 C44 125.9(10) . . ? C39 C40 Lu4 76.3(5) . . ? C41 C40 Lu4 72.6(5) . . ? C44 C40 Lu4 121.8(6) . . ? C40 C41 C37 109.1(9) . . ? C40 C41 C45 124.0(10) . . ? C37 C41 C45 126.9(9) . . ? C40 C41 Lu4 76.0(5) . . ? C37 C41 Lu4 74.0(5) . . ? C45 C41 Lu4 117.7(6) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.675 _refine_diff_density_min -1.598 _refine_diff_density_rms 0.196 #===END