# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dongmei Cui' _publ_contact_author_email DMCUI@CIAC.JL.CN _publ_section_title ; Rare-Earth Metal Complexes Stabilized by Amino-Phosphine Ligand. Reaction with Mesityl Azide and Catalysis on Cycloadditon of Organic Azides and Aromatic Alkynes ; loop_ _publ_author_name 'Dongmei Cui.' 'Bo Liu.' #===========END============= data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 670207' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H104 Lu2 N8 P2' _chemical_formula_weight 2021.95 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' P P 0.1023 0.0942 '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 13.6136(10) _cell_length_b 14.4341(11) _cell_length_c 27.0624(19) _cell_angle_alpha 79.4710(10) _cell_angle_beta 76.8340(10) _cell_angle_gamma 73.9160(10) _cell_volume 4934.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 2.074 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7889 _exptl_absorpt_correction_T_max 0.8194 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 27957 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0831 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.05 _reflns_number_total 19026 _reflns_number_gt 13680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^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 19026 _refine_ls_number_parameters 1132 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.059 _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 0.881118(18) 0.658179(17) 0.679959(8) 0.02354(7) Uani 1 1 d . . . Lu2 Lu 0.901428(18) 0.720774(17) 0.806469(8) 0.02332(7) Uani 1 1 d . . . P1 P 1.03022(11) 0.73597(11) 0.54882(5) 0.0260(3) Uani 1 1 d . . . P2 P 0.74518(11) 0.64215(10) 0.93625(5) 0.0250(3) Uani 1 1 d . . . N1 N 0.9691(3) 0.5267(3) 0.64722(16) 0.0260(10) Uani 1 1 d . . . N2 N 0.9543(3) 0.7418(3) 0.60504(16) 0.0275(11) Uani 1 1 d . . . N3 N 0.9057(3) 0.8377(3) 0.60984(16) 0.0264(11) Uani 1 1 d . . . N4 N 0.8417(3) 0.8431(3) 0.65257(17) 0.0258(10) Uani 1 1 d . . . N5 N 1.0130(3) 0.6223(3) 0.84855(16) 0.0270(11) Uani 1 1 d . . . N6 N 0.7719(3) 0.7020(3) 0.87955(16) 0.0232(10) Uani 1 1 d . . . N7 N 0.6844(3) 0.7730(3) 0.87074(17) 0.0275(11) Uani 1 1 d . . . N8 N 0.7024(4) 0.8235(3) 0.82754(16) 0.0293(11) Uani 1 1 d . . . C1 C 0.8043(4) 0.6333(4) 0.7716(2) 0.0289(13) Uani 1 1 d . . . C2 C 0.7652(4) 0.5663(4) 0.7739(2) 0.0281(13) Uani 1 1 d . . . C3 C 0.7148(4) 0.4873(4) 0.7808(2) 0.0308(14) Uani 1 1 d . . . C4 C 0.7555(5) 0.3979(5) 0.8070(2) 0.0414(16) Uani 1 1 d . . . H4 H 0.8168 0.3878 0.8192 0.050 Uiso 1 1 calc R . . C5 C 0.7055(6) 0.3238(5) 0.8151(3) 0.057(2) Uani 1 1 d . . . H5A H 0.7324 0.2642 0.8330 0.068 Uiso 1 1 calc R . . C6 C 0.6152(6) 0.3386(6) 0.7963(3) 0.057(2) Uani 1 1 d . . . H6 H 0.5812 0.2889 0.8018 0.068 Uiso 1 1 calc R . . C7 C 0.5754(5) 0.4265(5) 0.7695(2) 0.0466(18) Uani 1 1 d . . . H7 H 0.5155 0.4354 0.7564 0.056 Uiso 1 1 calc R . . C8 C 0.6241(4) 0.5017(5) 0.7621(2) 0.0367(15) Uani 1 1 d . . . H8 H 0.5963 0.5616 0.7446 0.044 Uiso 1 1 calc R . . C9 C 1.0012(4) 0.7125(4) 0.7180(2) 0.0310(14) Uani 1 1 d . . . C10 C 1.0783(5) 0.7363(4) 0.72163(19) 0.0321(14) Uani 1 1 d U . . C11 C 1.1719(5) 0.7651(5) 0.7212(2) 0.0384(15) Uani 1 1 d U . . C12 C 1.2680(5) 0.7011(6) 0.7084(2) 0.0503(18) Uani 1 1 d U . . H12 H 1.2719 0.6392 0.7015 0.060 Uiso 1 1 calc R . . C13 C 1.3586(5) 0.7302(7) 0.7059(3) 0.070(2) Uani 1 1 d U . . H13 H 1.4234 0.6880 0.6973 0.083 Uiso 1 1 calc R . . C14 C 1.3515(7) 0.8220(8) 0.7165(3) 0.078(3) Uani 1 1 d U . . H14 H 1.4118 0.8415 0.7151 0.094 Uiso 1 1 calc R . . C15 C 1.2586(7) 0.8833(7) 0.7286(3) 0.071(2) Uani 1 1 d U . . H15 H 1.2558 0.9450 0.7353 0.085 Uiso 1 1 calc R . . C16 C 1.1667(6) 0.8577(6) 0.7316(2) 0.053(2) Uani 1 1 d . . . H16 H 1.1029 0.9012 0.7404 0.064 Uiso 1 1 calc R . . C17 C 0.7325(5) 0.6644(4) 0.6464(2) 0.0342(14) Uani 1 1 d . . . C18 C 0.6655(5) 0.6455(4) 0.6301(2) 0.0336(14) Uani 1 1 d . . . C19 C 0.5862(4) 0.6151(4) 0.6135(2) 0.0313(14) Uani 1 1 d . . . C20 C 0.5668(5) 0.5250(5) 0.6328(2) 0.0403(16) Uani 1 1 d . . . H20 H 0.6067 0.4834 0.6553 0.048 Uiso 1 1 calc R . . C21 C 0.4894(5) 0.4956(6) 0.6192(3) 0.056(2) Uani 1 1 d . . . H21 H 0.4762 0.4354 0.6331 0.067 Uiso 1 1 calc R . . C22 C 0.4320(5) 0.5563(6) 0.5849(3) 0.058(2) Uani 1 1 d . . . H22 H 0.3797 0.5370 0.5757 0.070 Uiso 1 1 calc R . . C23 C 0.4514(5) 0.6446(6) 0.5643(3) 0.0551(19) Uani 1 1 d . . . H23 H 0.4132 0.6847 0.5406 0.066 Uiso 1 1 calc R . . C24 C 0.5284(5) 0.6748(5) 0.5789(2) 0.0448(17) Uani 1 1 d . . . H24 H 0.5409 0.7353 0.5652 0.054 Uiso 1 1 calc R . . C25 C 0.9302(4) 0.8577(4) 0.8304(2) 0.0360(15) Uani 1 1 d . . . C26 C 0.9540(5) 0.9200(4) 0.8473(2) 0.0344(14) Uani 1 1 d . . . C27 C 0.9821(5) 0.9960(5) 0.8647(3) 0.0440(16) Uani 1 1 d U . . C28 C 0.9659(6) 1.0877(5) 0.8378(3) 0.059(2) Uani 1 1 d U . . H28 H 0.9373 1.0995 0.8084 0.071 Uiso 1 1 calc R . . C29 C 0.9913(6) 1.1629(6) 0.8534(3) 0.074(2) Uani 1 1 d U . . H29 H 0.9787 1.2248 0.8351 0.089 Uiso 1 1 calc R . . C30 C 1.0345(7) 1.1455(7) 0.8956(4) 0.087(3) Uani 1 1 d U . . H30 H 1.0537 1.1952 0.9057 0.104 Uiso 1 1 calc R . . C31 C 1.0498(8) 1.0565(7) 0.9230(4) 0.111(4) Uani 1 1 d U . . H31 H 1.0785 1.0455 0.9523 0.133 Uiso 1 1 calc R . . C32 C 1.0231(7) 0.9811(6) 0.9080(4) 0.090(3) Uani 1 1 d U . . H32 H 1.0332 0.9202 0.9275 0.108 Uiso 1 1 calc R . . C33 C 0.6078(5) 0.8961(4) 0.8178(2) 0.0322(14) Uani 1 1 d . . . C34 C 0.6096(5) 0.9935(4) 0.8089(2) 0.0391(16) Uani 1 1 d . . . C35 C 0.5181(6) 1.0627(5) 0.8014(3) 0.056(2) Uani 1 1 d . . . H35 H 0.5188 1.1281 0.7954 0.067 Uiso 1 1 calc R . . C36 C 0.4266(6) 1.0382(5) 0.8025(2) 0.0508(18) Uani 1 1 d . . . C37 C 0.4280(5) 0.9401(5) 0.8108(2) 0.0471(18) Uani 1 1 d . . . H37 H 0.3672 0.9221 0.8114 0.056 Uiso 1 1 calc R . . C38 C 0.5176(5) 0.8673(4) 0.8184(2) 0.0365(15) Uani 1 1 d . . . C39 C 0.5136(5) 0.7619(5) 0.8260(3) 0.0506(18) Uani 1 1 d . . . H39A H 0.5789 0.7236 0.8101 0.076 Uiso 1 1 calc R . . H39B H 0.4588 0.7560 0.8107 0.076 Uiso 1 1 calc R . . H39C H 0.5005 0.7392 0.8619 0.076 Uiso 1 1 calc R . . C40 C 0.7077(5) 1.0239(5) 0.8062(3) 0.063(2) Uani 1 1 d . . . H40A H 0.7600 0.9965 0.7789 0.094 Uiso 1 1 calc R . . H40B H 0.7318 1.0013 0.8381 0.094 Uiso 1 1 calc R . . H40C H 0.6941 1.0936 0.8000 0.094 Uiso 1 1 calc R . . C41 C 0.3289(6) 1.1148(6) 0.7940(3) 0.077(3) Uani 1 1 d . . . H41A H 0.3200 1.1671 0.8133 0.116 Uiso 1 1 calc R . . H41B H 0.2701 1.0867 0.8051 0.116 Uiso 1 1 calc R . . H41C H 0.3345 1.1391 0.7583 0.116 Uiso 1 1 calc R . . C42 C 0.7923(4) 0.9427(4) 0.6598(2) 0.0264(13) Uani 1 1 d . . . C43 C 0.8497(5) 1.0114(4) 0.6552(2) 0.0346(14) Uani 1 1 d . . . C44 C 0.7954(5) 1.1070(4) 0.6594(2) 0.0406(16) Uani 1 1 d . . . H44 H 0.8330 1.1534 0.6559 0.049 Uiso 1 1 calc R . . C45 C 0.6885(5) 1.1367(5) 0.6684(3) 0.0446(17) Uani 1 1 d . . . C46 C 0.6345(5) 1.0649(5) 0.6760(2) 0.0427(16) Uani 1 1 d . . . H46 H 0.5622 1.0827 0.6835 0.051 Uiso 1 1 calc R . . C47 C 0.6841(4) 0.9678(4) 0.6729(2) 0.0328(14) Uani 1 1 d . . . C48 C 0.9677(4) 0.9842(4) 0.6468(2) 0.0428(16) Uani 1 1 d . . . H48A H 0.9915 0.9186 0.6622 0.064 Uiso 1 1 calc R . . H48B H 0.9907 1.0275 0.6621 0.064 Uiso 1 1 calc R . . H48C H 0.9955 0.9892 0.6107 0.064 Uiso 1 1 calc R . . C49 C 0.6310(5) 1.2423(5) 0.6712(3) 0.070(2) Uani 1 1 d . . . H49A H 0.6606 1.2696 0.6924 0.105 Uiso 1 1 calc R . . H49B H 0.5589 1.2464 0.6857 0.105 Uiso 1 1 calc R . . H49C H 0.6371 1.2777 0.6375 0.105 Uiso 1 1 calc R . . C50 C 0.6224(5) 0.8919(5) 0.6820(3) 0.0534(19) Uani 1 1 d . . . H50A H 0.6298 0.8667 0.6505 0.080 Uiso 1 1 calc R . . H50B H 0.5504 0.9209 0.6941 0.080 Uiso 1 1 calc R . . H50C H 0.6480 0.8400 0.7071 0.080 Uiso 1 1 calc R . . C51 C 1.1133(4) 0.8172(4) 0.5416(2) 0.0273(13) Uani 1 1 d . . . C52 C 1.1735(4) 0.8007(4) 0.5795(2) 0.0341(14) Uani 1 1 d . . . H52 H 1.1720 0.7482 0.6051 0.041 Uiso 1 1 calc R . . C53 C 1.2353(5) 0.8632(5) 0.5787(3) 0.0438(17) Uani 1 1 d . . . H53 H 1.2749 0.8533 0.6039 0.053 Uiso 1 1 calc R . . C54 C 1.2373(5) 0.9401(5) 0.5403(3) 0.0508(19) Uani 1 1 d . . . H54 H 1.2785 0.9821 0.5399 0.061 Uiso 1 1 calc R . . C55 C 1.1801(5) 0.9559(5) 0.5029(3) 0.0543(19) Uani 1 1 d . . . H55 H 1.1827 1.0080 0.4772 0.065 Uiso 1 1 calc R . . C56 C 1.1179(5) 0.8940(4) 0.5033(2) 0.0398(16) Uani 1 1 d . . . H56 H 1.0792 0.9045 0.4777 0.048 Uiso 1 1 calc R . . C57 C 0.9557(5) 0.7689(4) 0.4986(2) 0.0277(13) Uani 1 1 d . . . C58 C 0.8484(5) 0.7856(4) 0.5107(2) 0.0364(15) Uani 1 1 d . . . H58 H 0.8140 0.7816 0.5446 0.044 Uiso 1 1 calc R . . C59 C 0.7929(6) 0.8085(5) 0.4708(3) 0.0516(19) Uani 1 1 d . . . H59 H 0.7207 0.8201 0.4780 0.062 Uiso 1 1 calc R . . C60 C 0.8448(7) 0.8140(5) 0.4204(3) 0.057(2) Uani 1 1 d . . . H60 H 0.8070 0.8297 0.3942 0.068 Uiso 1 1 calc R . . C61 C 0.9516(6) 0.7966(5) 0.4087(3) 0.0525(19) Uani 1 1 d . . . H61 H 0.9859 0.8003 0.3747 0.063 Uiso 1 1 calc R . . C62 C 1.0067(5) 0.7739(4) 0.4476(2) 0.0426(16) Uani 1 1 d . . . H62 H 1.0790 0.7617 0.4400 0.051 Uiso 1 1 calc R . . C63 C 1.1085(4) 0.6147(4) 0.5419(2) 0.0281(13) Uani 1 1 d . . . C64 C 1.2079(5) 0.6079(4) 0.5115(2) 0.0365(15) Uani 1 1 d . . . H64 H 1.2336 0.6631 0.5011 0.044 Uiso 1 1 calc R . . C65 C 1.2677(5) 0.5198(4) 0.4968(2) 0.0377(15) Uani 1 1 d . . . H65 H 1.3334 0.5157 0.4765 0.045 Uiso 1 1 calc R . . C66 C 1.2302(5) 0.4386(5) 0.5123(2) 0.0442(17) Uani 1 1 d . . . H66 H 1.2704 0.3792 0.5024 0.053 Uiso 1 1 calc R . . C67 C 1.1323(5) 0.4443(4) 0.5428(2) 0.0386(15) Uani 1 1 d . . . H67 H 1.1085 0.3881 0.5531 0.046 Uiso 1 1 calc R . . C68 C 1.0687(4) 0.5316(4) 0.55826(19) 0.0269(13) Uani 1 1 d . . . C69 C 0.9647(4) 0.5315(4) 0.5929(2) 0.0294(13) Uani 1 1 d . . . H69A H 0.9139 0.5901 0.5831 0.035 Uiso 1 1 calc R . . H69B H 0.9417 0.4762 0.5884 0.035 Uiso 1 1 calc R . . C70 C 1.0116(4) 0.4324(4) 0.6703(2) 0.0298(13) Uani 1 1 d . . . C71 C 1.1129(5) 0.4062(4) 0.6809(2) 0.0330(14) Uani 1 1 d . . . C72 C 1.1513(5) 0.3133(5) 0.7047(2) 0.0434(17) Uani 1 1 d . . . H72 H 1.2190 0.2961 0.7107 0.052 Uiso 1 1 calc R . . C73 C 1.0925(5) 0.2465(4) 0.7195(2) 0.0429(17) Uani 1 1 d . . . H73 H 1.1197 0.1850 0.7357 0.051 Uiso 1 1 calc R . . C74 C 0.9935(5) 0.2713(4) 0.7102(2) 0.0424(17) Uani 1 1 d . . . H74 H 0.9527 0.2266 0.7212 0.051 Uiso 1 1 calc R . . C75 C 0.9516(5) 0.3621(4) 0.6846(2) 0.0327(14) Uani 1 1 d . . . C76 C 0.8434(4) 0.3841(4) 0.6724(2) 0.0391(15) Uani 1 1 d . . . H76A H 0.8481 0.3641 0.6398 0.059 Uiso 1 1 calc R . . H76B H 0.8125 0.4527 0.6712 0.059 Uiso 1 1 calc R . . H76C H 0.8012 0.3496 0.6984 0.059 Uiso 1 1 calc R . . C77 C 1.1792(5) 0.4787(5) 0.6676(2) 0.0483(18) Uani 1 1 d . . . H77A H 1.1851 0.5029 0.6318 0.072 Uiso 1 1 calc R . . H77B H 1.2473 0.4475 0.6750 0.072 Uiso 1 1 calc R . . H77C H 1.1476 0.5317 0.6874 0.072 Uiso 1 1 calc R . . C78 C 0.6257(4) 0.6060(4) 0.9420(2) 0.0279(13) Uani 1 1 d . . . C79 C 0.6258(5) 0.5448(4) 0.9083(2) 0.0359(15) Uani 1 1 d . . . H79 H 0.6876 0.5179 0.8872 0.043 Uiso 1 1 calc R . . C80 C 0.5335(5) 0.5232(5) 0.9056(2) 0.0459(17) Uani 1 1 d . . . H80 H 0.5332 0.4813 0.8833 0.055 Uiso 1 1 calc R . . C81 C 0.4424(5) 0.5653(5) 0.9369(3) 0.0441(17) Uani 1 1 d . . . H81 H 0.3803 0.5520 0.9352 0.053 Uiso 1 1 calc R . . C82 C 0.4418(5) 0.6251(5) 0.9698(2) 0.0420(16) Uani 1 1 d . . . H82 H 0.3797 0.6523 0.9906 0.050 Uiso 1 1 calc R . . C83 C 0.5336(4) 0.6466(4) 0.9730(2) 0.0351(14) Uani 1 1 d . . . H83 H 0.5330 0.6879 0.9958 0.042 Uiso 1 1 calc R . . C84 C 0.7312(4) 0.7171(4) 0.9854(2) 0.0283(13) Uani 1 1 d . . . C85 C 0.7052(5) 0.6824(5) 1.0369(2) 0.0384(15) Uani 1 1 d . . . H85 H 0.6929 0.6208 1.0465 0.046 Uiso 1 1 calc R . . C86 C 0.6976(5) 0.7402(5) 1.0737(2) 0.0517(19) Uani 1 1 d . . . H86 H 0.6801 0.7178 1.1082 0.062 Uiso 1 1 calc R . . C87 C 0.7162(5) 0.8314(5) 1.0589(3) 0.055(2) Uani 1 1 d . . . H87 H 0.7100 0.8704 1.0838 0.066 Uiso 1 1 calc R . . C88 C 0.7436(5) 0.8657(5) 1.0086(3) 0.0484(18) Uani 1 1 d . . . H88 H 0.7569 0.9269 0.9993 0.058 Uiso 1 1 calc R . . C89 C 0.7511(4) 0.8078(4) 0.9719(2) 0.0329(14) Uani 1 1 d . . . H89 H 0.7698 0.8304 0.9375 0.039 Uiso 1 1 calc R . . C90 C 0.8489(4) 0.5348(4) 0.94464(19) 0.0265(13) Uani 1 1 d . . . C91 C 0.8213(5) 0.4487(4) 0.9681(2) 0.0338(14) Uani 1 1 d . . . H91 H 0.7515 0.4475 0.9766 0.041 Uiso 1 1 calc R . . C92 C 0.8962(5) 0.3658(4) 0.9788(2) 0.0403(16) Uani 1 1 d . . . H92 H 0.8770 0.3088 0.9943 0.048 Uiso 1 1 calc R . . C93 C 1.0007(5) 0.3671(4) 0.9665(2) 0.0382(15) Uani 1 1 d . . . H93 H 1.0518 0.3110 0.9733 0.046 Uiso 1 1 calc R . . C94 C 1.0278(5) 0.4528(4) 0.9440(2) 0.0333(14) Uani 1 1 d . . . H94 H 1.0978 0.4534 0.9362 0.040 Uiso 1 1 calc R . . C95 C 0.9536(4) 0.5387(4) 0.93260(19) 0.0248(12) Uani 1 1 d . . . C96 C 0.9904(4) 0.6258(4) 0.9043(2) 0.0273(13) Uani 1 1 d . . . H96A H 0.9373 0.6844 0.9122 0.033 Uiso 1 1 calc R . . H96B H 1.0527 0.6278 0.9153 0.033 Uiso 1 1 calc R . . C97 C 1.1108(4) 0.5569(4) 0.83347(19) 0.0261(13) Uani 1 1 d . . . C98 C 1.2040(5) 0.5804(4) 0.8348(2) 0.0336(14) Uani 1 1 d . . . C99 C 1.2986(5) 0.5134(5) 0.8217(2) 0.0416(16) Uani 1 1 d . . . H99 H 1.3601 0.5285 0.8228 0.050 Uiso 1 1 calc R . . C100 C 1.3032(5) 0.4251(5) 0.8071(2) 0.0461(17) Uani 1 1 d . . . H100 H 1.3669 0.3810 0.7987 0.055 Uiso 1 1 calc R . . C101 C 1.2110(5) 0.4034(5) 0.8051(2) 0.0382(15) Uani 1 1 d . . . H101 H 1.2134 0.3445 0.7949 0.046 Uiso 1 1 calc R . . C102 C 1.1158(4) 0.4678(4) 0.8179(2) 0.0298(13) Uani 1 1 d . . . C103 C 1.0186(4) 0.4406(4) 0.8148(2) 0.0396(16) Uani 1 1 d . . . H10A H 1.0363 0.3752 0.8068 0.059 Uiso 1 1 calc R . . H10B H 0.9860 0.4841 0.7886 0.059 Uiso 1 1 calc R . . H10C H 0.9715 0.4451 0.8471 0.059 Uiso 1 1 calc R . . C104 C 1.2039(5) 0.6766(5) 0.8491(2) 0.0428(16) Uani 1 1 d . . . H10D H 1.2069 0.6693 0.8848 0.064 Uiso 1 1 calc R . . H10E H 1.1414 0.7238 0.8427 0.064 Uiso 1 1 calc R . . H10F H 1.2633 0.6979 0.8290 0.064 Uiso 1 1 calc R . . C105 C 0.5340(5) 0.7824(5) 0.42927(16) 0.109(4) Uani 1 1 d G . . H105 H 0.5232 0.7208 0.4417 0.131 Uiso 1 1 calc R . . C106 C 0.6068(4) 0.7954(5) 0.38503(17) 0.127(5) Uani 1 1 d G . . H106 H 0.6448 0.7426 0.3679 0.153 Uiso 1 1 calc R . . C107 C 0.6229(3) 0.8874(5) 0.36637(17) 0.157(7) Uani 1 1 d G . . H107 H 0.6716 0.8961 0.3368 0.188 Uiso 1 1 calc R . . C108 C 0.5662(5) 0.9664(5) 0.39196(18) 0.131(5) Uani 1 1 d G . . H108 H 0.5769 1.0279 0.3795 0.157 Uiso 1 1 calc R . . C109 C 0.4934(4) 0.9533(5) 0.43621(17) 0.134(5) Uani 1 1 d G . . H109 H 0.4554 1.0062 0.4533 0.161 Uiso 1 1 calc R . . C110 C 0.4773(4) 0.8613(6) 0.45486(15) 0.129(5) Uani 1 1 d G . . H110 H 0.4285 0.8526 0.4845 0.155 Uiso 1 1 calc R . . C111 C 0.3705(3) 0.8767(2) 0.04871(14) 0.122(5) Uani 1 1 d G . . H111 H 0.3881 0.8718 0.0805 0.146 Uiso 1 1 calc R . . C112 C 0.4417(4) 0.8931(3) 0.00575(14) 0.096(3) Uani 1 1 d G . . H112 H 0.5059 0.9016 0.0076 0.115 Uiso 1 1 calc R . . C113 C 0.4143(4) 0.8964(3) -0.03955(14) 0.091(3) Uani 1 1 d G . . H113 H 0.4609 0.9073 -0.0697 0.109 Uiso 1 1 calc R . . C114 C 0.3233(4) 0.8847(3) -0.04188(15) 0.100(4) Uani 1 1 d G . . H114 H 0.3064 0.8868 -0.0736 0.121 Uiso 1 1 calc R . . C115 C 0.2557(4) 0.8698(4) 0.00028(15) 0.115(4) Uani 1 1 d G . . H115 H 0.1921 0.8609 -0.0024 0.139 Uiso 1 1 calc R . . C116 C 0.2754(4) 0.8671(4) 0.04687(15) 0.137(6) Uani 1 1 d G . . H116 H 0.2263 0.8590 0.0764 0.164 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 0.02546(14) 0.02428(14) 0.02231(13) -0.00371(10) -0.00382(10) -0.00849(11) Lu2 0.02502(14) 0.02414(14) 0.02231(13) -0.00400(10) -0.00431(10) -0.00792(11) P1 0.0301(9) 0.0237(8) 0.0239(8) -0.0035(6) -0.0036(7) -0.0072(7) P2 0.0259(8) 0.0241(8) 0.0235(8) -0.0032(6) -0.0027(6) -0.0052(7) N1 0.031(3) 0.019(2) 0.027(3) -0.0007(19) -0.005(2) -0.007(2) N2 0.031(3) 0.022(3) 0.029(3) -0.005(2) -0.004(2) -0.007(2) N3 0.026(3) 0.028(3) 0.024(3) -0.003(2) -0.003(2) -0.007(2) N4 0.026(3) 0.025(3) 0.030(3) -0.004(2) -0.007(2) -0.010(2) N5 0.023(3) 0.036(3) 0.023(2) -0.006(2) -0.003(2) -0.008(2) N6 0.021(2) 0.020(2) 0.029(2) -0.0038(19) -0.008(2) -0.002(2) N7 0.026(3) 0.029(3) 0.029(3) -0.008(2) -0.008(2) -0.005(2) N8 0.038(3) 0.023(3) 0.027(3) -0.003(2) -0.008(2) -0.006(2) C1 0.028(3) 0.034(3) 0.024(3) -0.002(3) -0.002(3) -0.011(3) C2 0.030(3) 0.032(3) 0.023(3) -0.002(2) -0.003(2) -0.011(3) C3 0.029(3) 0.035(4) 0.034(3) -0.014(3) 0.003(3) -0.017(3) C4 0.045(4) 0.037(4) 0.046(4) -0.006(3) -0.010(3) -0.016(3) C5 0.067(5) 0.037(4) 0.066(5) 0.002(4) -0.012(4) -0.021(4) C6 0.068(5) 0.056(5) 0.061(5) -0.016(4) 0.003(4) -0.046(4) C7 0.039(4) 0.059(5) 0.049(4) -0.021(4) 0.006(3) -0.027(4) C8 0.034(4) 0.038(4) 0.039(4) -0.012(3) 0.002(3) -0.012(3) C9 0.034(4) 0.035(4) 0.026(3) -0.006(3) -0.007(3) -0.011(3) C10 0.037(3) 0.044(4) 0.018(3) -0.008(3) 0.000(3) -0.015(3) C11 0.034(3) 0.066(5) 0.024(3) -0.004(3) -0.008(3) -0.025(3) C12 0.036(4) 0.079(5) 0.041(4) -0.011(4) -0.006(3) -0.022(4) C13 0.030(4) 0.129(7) 0.052(5) -0.008(5) -0.003(3) -0.028(4) C14 0.058(5) 0.147(8) 0.056(5) -0.002(5) -0.008(4) -0.075(5) C15 0.077(5) 0.091(6) 0.068(5) -0.001(5) -0.019(5) -0.062(5) C16 0.055(5) 0.075(6) 0.047(4) -0.003(4) -0.014(4) -0.043(4) C17 0.035(4) 0.034(4) 0.033(3) -0.003(3) -0.007(3) -0.006(3) C18 0.032(4) 0.036(4) 0.032(3) -0.008(3) -0.005(3) -0.006(3) C19 0.026(3) 0.037(4) 0.029(3) -0.010(3) -0.004(3) -0.003(3) C20 0.040(4) 0.045(4) 0.041(4) -0.001(3) -0.016(3) -0.013(3) C21 0.049(5) 0.063(5) 0.068(5) -0.005(4) -0.015(4) -0.031(4) C22 0.036(4) 0.077(6) 0.070(5) -0.012(4) -0.017(4) -0.020(4) C23 0.043(4) 0.061(5) 0.061(5) -0.010(4) -0.021(4) -0.001(4) C24 0.039(4) 0.050(4) 0.047(4) -0.006(3) -0.015(3) -0.009(3) C25 0.028(3) 0.032(4) 0.046(4) -0.014(3) -0.003(3) -0.003(3) C26 0.037(4) 0.023(3) 0.045(4) -0.006(3) -0.011(3) -0.006(3) C27 0.049(4) 0.038(4) 0.052(4) -0.014(3) -0.013(3) -0.013(3) C28 0.084(6) 0.046(4) 0.057(5) -0.009(3) -0.010(4) -0.030(4) C29 0.086(6) 0.049(5) 0.093(6) -0.019(4) -0.003(5) -0.033(5) C30 0.093(7) 0.065(5) 0.127(8) -0.046(5) -0.031(6) -0.031(5) C31 0.147(9) 0.082(6) 0.142(9) -0.035(6) -0.094(7) -0.021(7) C32 0.132(8) 0.047(5) 0.114(7) -0.009(4) -0.087(6) -0.009(5) C33 0.039(4) 0.033(4) 0.024(3) -0.004(3) -0.011(3) -0.003(3) C34 0.053(4) 0.027(4) 0.039(4) -0.001(3) -0.018(3) -0.007(3) C35 0.070(5) 0.029(4) 0.068(5) -0.011(3) -0.030(4) 0.008(4) C36 0.058(5) 0.047(5) 0.044(4) -0.009(3) -0.029(4) 0.009(4) C37 0.038(4) 0.061(5) 0.039(4) -0.010(3) -0.013(3) 0.002(4) C38 0.034(4) 0.035(4) 0.039(4) -0.002(3) -0.013(3) -0.002(3) C39 0.038(4) 0.051(5) 0.066(5) -0.002(4) -0.017(4) -0.013(3) C40 0.074(6) 0.026(4) 0.090(6) 0.007(4) -0.033(5) -0.012(4) C41 0.074(6) 0.065(6) 0.083(6) -0.016(5) -0.040(5) 0.025(5) C42 0.026(3) 0.023(3) 0.029(3) -0.009(2) -0.001(3) -0.004(3) C43 0.037(4) 0.026(3) 0.040(4) -0.003(3) -0.008(3) -0.009(3) C44 0.044(4) 0.031(4) 0.051(4) -0.010(3) -0.002(3) -0.019(3) C45 0.037(4) 0.033(4) 0.064(5) -0.023(3) -0.005(3) -0.002(3) C46 0.025(3) 0.042(4) 0.061(4) -0.018(3) -0.006(3) -0.002(3) C47 0.032(4) 0.033(4) 0.037(3) -0.009(3) -0.005(3) -0.011(3) C48 0.031(4) 0.036(4) 0.064(5) -0.009(3) -0.006(3) -0.015(3) C49 0.049(5) 0.043(5) 0.121(7) -0.035(5) -0.015(5) -0.002(4) C50 0.035(4) 0.041(4) 0.083(5) -0.016(4) -0.001(4) -0.011(3) C51 0.027(3) 0.023(3) 0.030(3) -0.009(2) 0.004(3) -0.007(3) C52 0.035(4) 0.037(4) 0.032(3) -0.004(3) -0.003(3) -0.015(3) C53 0.035(4) 0.043(4) 0.056(4) -0.024(3) 0.002(3) -0.012(3) C54 0.034(4) 0.034(4) 0.086(6) -0.019(4) -0.001(4) -0.012(3) C55 0.055(5) 0.032(4) 0.073(5) 0.002(4) -0.004(4) -0.017(4) C56 0.044(4) 0.035(4) 0.043(4) -0.003(3) -0.006(3) -0.016(3) C57 0.040(4) 0.019(3) 0.028(3) -0.003(2) -0.009(3) -0.010(3) C58 0.044(4) 0.024(3) 0.043(4) -0.001(3) -0.019(3) -0.005(3) C59 0.056(5) 0.033(4) 0.075(5) -0.014(4) -0.033(4) -0.004(3) C60 0.094(7) 0.033(4) 0.056(5) -0.001(3) -0.048(5) -0.010(4) C61 0.088(6) 0.037(4) 0.037(4) -0.003(3) -0.021(4) -0.017(4) C62 0.058(5) 0.041(4) 0.030(3) -0.007(3) -0.008(3) -0.012(3) C63 0.029(3) 0.032(3) 0.025(3) -0.010(2) -0.004(3) -0.006(3) C64 0.041(4) 0.032(4) 0.037(4) -0.006(3) -0.002(3) -0.013(3) C65 0.034(4) 0.034(4) 0.041(4) -0.009(3) 0.000(3) -0.003(3) C66 0.045(4) 0.033(4) 0.049(4) -0.020(3) 0.006(3) -0.002(3) C67 0.050(4) 0.028(4) 0.040(4) -0.007(3) -0.006(3) -0.012(3) C68 0.033(3) 0.028(3) 0.022(3) -0.005(2) -0.004(2) -0.011(3) C69 0.030(3) 0.024(3) 0.035(3) -0.005(3) -0.005(3) -0.010(3) C70 0.034(3) 0.033(3) 0.020(3) -0.007(2) 0.003(3) -0.008(3) C71 0.037(4) 0.038(4) 0.025(3) -0.004(3) -0.010(3) -0.009(3) C72 0.046(4) 0.046(4) 0.034(4) -0.012(3) -0.013(3) 0.005(3) C73 0.068(5) 0.024(3) 0.033(4) 0.003(3) -0.019(3) -0.002(3) C74 0.069(5) 0.032(4) 0.025(3) -0.001(3) 0.000(3) -0.020(4) C75 0.040(4) 0.035(4) 0.022(3) -0.010(3) 0.002(3) -0.009(3) C76 0.040(4) 0.036(4) 0.041(4) -0.008(3) 0.002(3) -0.013(3) C77 0.029(4) 0.060(5) 0.056(4) -0.010(4) -0.007(3) -0.010(3) C78 0.029(3) 0.029(3) 0.026(3) -0.001(2) -0.005(3) -0.008(3) C79 0.032(4) 0.044(4) 0.033(3) -0.005(3) -0.006(3) -0.011(3) C80 0.054(5) 0.058(5) 0.034(4) -0.002(3) -0.011(3) -0.027(4) C81 0.035(4) 0.042(4) 0.058(4) 0.010(3) -0.021(3) -0.014(3) C82 0.025(4) 0.040(4) 0.056(4) 0.001(3) -0.003(3) -0.007(3) C83 0.034(4) 0.034(4) 0.034(3) -0.005(3) -0.001(3) -0.008(3) C84 0.027(3) 0.028(3) 0.029(3) -0.010(3) -0.005(3) -0.002(3) C85 0.042(4) 0.037(4) 0.029(3) -0.003(3) -0.005(3) -0.002(3) C86 0.068(5) 0.057(5) 0.027(4) -0.002(3) -0.009(3) -0.012(4) C87 0.069(5) 0.053(5) 0.047(4) -0.023(4) -0.024(4) 0.003(4) C88 0.061(5) 0.039(4) 0.054(4) -0.013(3) -0.028(4) -0.008(4) C89 0.035(4) 0.027(3) 0.036(3) -0.004(3) -0.012(3) -0.001(3) C90 0.034(3) 0.028(3) 0.017(3) -0.004(2) -0.003(2) -0.007(3) C91 0.033(4) 0.029(3) 0.036(3) -0.005(3) -0.003(3) -0.006(3) C92 0.055(5) 0.028(4) 0.035(4) -0.005(3) -0.001(3) -0.011(3) C93 0.050(4) 0.027(3) 0.035(3) -0.008(3) -0.018(3) 0.007(3) C94 0.032(3) 0.038(4) 0.025(3) -0.008(3) -0.010(3) 0.004(3) C95 0.028(3) 0.027(3) 0.018(3) -0.005(2) -0.005(2) -0.001(3) C96 0.024(3) 0.026(3) 0.033(3) -0.007(2) -0.007(3) -0.006(3) C97 0.025(3) 0.032(3) 0.020(3) -0.004(2) -0.002(2) -0.008(3) C98 0.031(4) 0.034(4) 0.036(3) -0.001(3) -0.004(3) -0.013(3) C99 0.021(3) 0.051(4) 0.051(4) -0.001(3) -0.008(3) -0.009(3) C100 0.029(4) 0.047(4) 0.049(4) -0.004(3) 0.001(3) 0.004(3) C101 0.037(4) 0.040(4) 0.034(3) -0.004(3) -0.002(3) -0.007(3) C102 0.023(3) 0.035(4) 0.026(3) 0.000(3) -0.003(3) -0.002(3) C103 0.039(4) 0.029(4) 0.051(4) -0.012(3) -0.011(3) -0.003(3) C104 0.037(4) 0.050(4) 0.046(4) -0.004(3) -0.009(3) -0.018(3) C105 0.061(7) 0.161(11) 0.087(8) -0.007(7) -0.008(6) -0.010(7) C106 0.069(8) 0.228(16) 0.081(8) -0.048(9) -0.015(6) -0.010(9) C107 0.069(8) 0.32(2) 0.075(8) -0.001(11) -0.025(6) -0.041(11) C108 0.104(10) 0.203(15) 0.093(9) 0.048(9) -0.055(7) -0.066(10) C109 0.123(11) 0.171(14) 0.081(8) 0.008(8) -0.025(8) -0.001(9) C110 0.102(9) 0.145(12) 0.088(8) -0.006(8) 0.016(7) 0.021(8) C111 0.144(11) 0.096(9) 0.080(8) -0.017(6) -0.020(8) 0.047(9) C112 0.059(6) 0.063(6) 0.162(11) -0.043(7) -0.025(7) 0.013(5) C113 0.112(9) 0.038(5) 0.097(8) -0.021(5) 0.028(7) -0.006(6) C114 0.145(11) 0.054(6) 0.108(9) -0.032(6) -0.032(8) -0.014(7) C115 0.094(8) 0.049(6) 0.182(13) 0.002(8) 0.011(9) -0.022(6) C116 0.131(11) 0.086(8) 0.106(9) 0.038(7) 0.046(8) 0.027(8) _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 N1 2.166(4) . ? Lu1 N2 2.327(4) . ? Lu1 C17 2.372(6) . ? Lu1 C1 2.465(5) . ? Lu1 C9 2.474(6) . ? Lu1 N4 2.575(4) . ? Lu2 N5 2.151(4) . ? Lu2 C25 2.344(6) . ? Lu2 N6 2.361(4) . ? Lu2 C9 2.474(5) . ? Lu2 C1 2.482(6) . ? Lu2 N8 2.691(5) . ? P1 N2 1.634(4) . ? P1 C57 1.795(5) . ? P1 C63 1.797(6) . ? P1 C51 1.801(5) . ? P2 N6 1.634(4) . ? P2 C90 1.803(6) . ? P2 C78 1.808(6) . ? P2 C84 1.809(5) . ? N1 C70 1.413(7) . ? N1 C69 1.473(6) . ? N2 N3 1.374(6) . ? N3 N4 1.280(5) . ? N4 C42 1.436(6) . ? N5 C97 1.424(7) . ? N5 C96 1.477(6) . ? N6 N7 1.375(6) . ? N7 N8 1.270(6) . ? N8 C33 1.460(7) . ? C1 C2 1.212(7) . ? C2 C3 1.450(7) . ? C3 C4 1.387(8) . ? C3 C8 1.389(8) . ? C4 C5 1.380(8) . ? C4 H4 0.9300 . ? C5 C6 1.384(9) . ? C5 H5A 0.9300 . ? C6 C7 1.374(9) . ? C6 H6 0.9300 . ? C7 C8 1.386(8) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.219(7) . ? C10 C11 1.442(8) . ? C11 C12 1.388(9) . ? C11 C16 1.396(9) . ? C12 C13 1.394(9) . ? C12 H12 0.9300 . ? C13 C14 1.379(11) . ? C13 H13 0.9300 . ? C14 C15 1.336(11) . ? C14 H14 0.9300 . ? C15 C16 1.381(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.211(7) . ? C18 C19 1.454(8) . ? C19 C24 1.381(8) . ? C19 C20 1.382(8) . ? C20 C21 1.381(8) . ? C20 H20 0.9300 . ? C21 C22 1.375(9) . ? C21 H21 0.9300 . ? C22 C23 1.366(9) . ? C22 H22 0.9300 . ? C23 C24 1.395(8) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.224(7) . ? C26 C27 1.441(8) . ? C27 C32 1.369(9) . ? C27 C28 1.375(9) . ? C28 C29 1.385(9) . ? C28 H28 0.9300 . ? C29 C30 1.354(11) . ? C29 H29 0.9300 . ? C30 C31 1.349(12) . ? C30 H30 0.9300 . ? C31 C32 1.389(11) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.388(8) . ? C33 C38 1.397(8) . ? C34 C35 1.394(8) . ? C34 C40 1.501(8) . ? C35 C36 1.378(9) . ? C35 H35 0.9300 . ? C36 C37 1.388(9) . ? C36 C41 1.508(9) . ? C37 C38 1.401(8) . ? C37 H37 0.9300 . ? C38 C39 1.511(8) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C47 1.392(7) . ? C42 C43 1.397(7) . ? C43 C44 1.384(8) . ? C43 C48 1.517(8) . ? C44 C45 1.375(8) . ? C44 H44 0.9300 . ? C45 C46 1.390(8) . ? C45 C49 1.515(8) . ? C46 C47 1.385(8) . ? C46 H46 0.9300 . ? C47 C50 1.510(8) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C56 1.376(7) . ? C51 C52 1.404(7) . ? C52 C53 1.388(7) . ? C52 H52 0.9300 . ? C53 C54 1.376(9) . ? C53 H53 0.9300 . ? C54 C55 1.365(9) . ? C54 H54 0.9300 . ? C55 C56 1.387(8) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 C58 1.385(8) . ? C57 C62 1.396(7) . ? C58 C59 1.396(8) . ? C58 H58 0.9300 . ? C59 C60 1.384(9) . ? C59 H59 0.9300 . ? C60 C61 1.377(9) . ? C60 H60 0.9300 . ? C61 C62 1.371(8) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 C64 1.402(7) . ? C63 C68 1.409(7) . ? C64 C65 1.378(8) . ? C64 H64 0.9300 . ? C65 C66 1.366(8) . ? C65 H65 0.9300 . ? C66 C67 1.387(8) . ? C66 H66 0.9300 . ? C67 C68 1.392(8) . ? C67 H67 0.9300 . ? C68 C69 1.510(7) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.406(8) . ? C70 C75 1.421(7) . ? C71 C72 1.391(8) . ? C71 C77 1.510(8) . ? C72 C73 1.368(8) . ? C72 H72 0.9300 . ? C73 C74 1.365(8) . ? C73 H73 0.9300 . ? C74 C75 1.399(8) . ? C74 H74 0.9300 . ? C75 C76 1.517(8) . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C78 C79 1.382(8) . ? C78 C83 1.382(7) . ? C79 C80 1.395(8) . ? C79 H79 0.9300 . ? C80 C81 1.385(8) . ? C80 H80 0.9300 . ? C81 C82 1.346(8) . ? C81 H81 0.9300 . ? C82 C83 1.392(8) . ? C82 H82 0.9300 . ? C83 H83 0.9300 . ? C84 C89 1.378(7) . ? C84 C85 1.391(7) . ? C85 C86 1.382(8) . ? C85 H85 0.9300 . ? C86 C87 1.380(9) . ? C86 H86 0.9300 . ? C87 C88 1.364(9) . ? C87 H87 0.9300 . ? C88 C89 1.381(8) . ? C88 H88 0.9300 . ? C89 H89 0.9300 . ? C90 C91 1.397(7) . ? C90 C95 1.403(7) . ? C91 C92 1.374(8) . ? C91 H91 0.9300 . ? C92 C93 1.389(8) . ? C92 H92 0.9300 . ? C93 C94 1.383(8) . ? C93 H93 0.9300 . ? C94 C95 1.401(7) . ? C94 H94 0.9300 . ? C95 C96 1.496(7) . ? C96 H96A 0.9700 . ? C96 H96B 0.9700 . ? C97 C102 1.405(7) . ? C97 C98 1.410(7) . ? C98 C99 1.395(8) . ? C98 C104 1.508(8) . ? C99 C100 1.383(8) . ? C99 H99 0.9300 . ? C100 C101 1.390(8) . ? C100 H100 0.9300 . ? C101 C102 1.382(8) . ? C101 H101 0.9300 . ? C102 C103 1.504(7) . ? C103 H10A 0.9600 . ? C103 H10B 0.9600 . ? C103 H10C 0.9600 . ? C104 H10D 0.9600 . ? C104 H10E 0.9600 . ? C104 H10F 0.9600 . ? C105 C106 1.3900 . ? C105 C110 1.3900 . ? C105 H105 0.9300 . ? C106 C107 1.3900 . ? C106 H106 0.9300 . ? C107 C108 1.3900 . ? C107 H107 0.9300 . ? C108 C109 1.3900 . ? C108 H108 0.9300 . ? C109 C110 1.3900 . ? C109 H109 0.9300 . ? C110 H110 0.9300 . ? C111 C116 1.3529 . ? C111 C112 1.3634 . ? C111 H111 0.9300 . ? C112 C113 1.3488 . ? C112 H112 0.9300 . ? C113 C114 1.3135 . ? C113 H113 0.9300 . ? C114 C115 1.3178 . ? C114 H114 0.9300 . ? C115 C116 1.3391 . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Lu1 N2 86.26(15) . . ? N1 Lu1 C17 92.61(18) . . ? N2 Lu1 C17 92.35(17) . . ? N1 Lu1 C1 114.96(17) . . ? N2 Lu1 C1 155.70(17) . . ? C17 Lu1 C1 98.04(18) . . ? N1 Lu1 C9 107.11(18) . . ? N2 Lu1 C9 83.35(16) . . ? C17 Lu1 C9 159.4(2) . . ? C1 Lu1 C9 79.22(18) . . ? N1 Lu1 N4 138.13(15) . . ? N2 Lu1 N4 52.14(14) . . ? C17 Lu1 N4 85.45(17) . . ? C1 Lu1 N4 106.70(17) . . ? C9 Lu1 N4 76.01(16) . . ? N5 Lu2 C25 92.61(19) . . ? N5 Lu2 N6 87.78(15) . . ? C25 Lu2 N6 93.54(17) . . ? N5 Lu2 C9 100.37(18) . . ? C25 Lu2 C9 104.1(2) . . ? N6 Lu2 C9 160.07(16) . . ? N5 Lu2 C1 111.85(17) . . ? C25 Lu2 C1 154.6(2) . . ? N6 Lu2 C1 81.19(15) . . ? C9 Lu2 C1 78.89(18) . . ? N5 Lu2 N8 136.92(15) . . ? C25 Lu2 N8 81.36(17) . . ? N6 Lu2 N8 50.51(14) . . ? C9 Lu2 N8 122.53(16) . . ? C1 Lu2 N8 76.13(16) . . ? N2 P1 C57 111.2(2) . . ? N2 P1 C63 111.7(2) . . ? C57 P1 C63 106.1(2) . . ? N2 P1 C51 108.1(2) . . ? C57 P1 C51 110.2(3) . . ? C63 P1 C51 109.6(3) . . ? N6 P2 C90 109.8(2) . . ? N6 P2 C78 109.2(2) . . ? C90 P2 C78 109.0(3) . . ? N6 P2 C84 110.4(2) . . ? C90 P2 C84 108.8(2) . . ? C78 P2 C84 109.7(3) . . ? C70 N1 C69 113.9(4) . . ? C70 N1 Lu1 131.4(3) . . ? C69 N1 Lu1 113.3(3) . . ? N3 N2 P1 108.5(3) . . ? N3 N2 Lu1 103.7(3) . . ? P1 N2 Lu1 147.5(3) . . ? N4 N3 N2 109.3(4) . . ? N3 N4 C42 110.8(4) . . ? N3 N4 Lu1 94.8(3) . . ? C42 N4 Lu1 154.3(3) . . ? C97 N5 C96 111.0(4) . . ? C97 N5 Lu2 133.1(3) . . ? C96 N5 Lu2 115.8(3) . . ? N7 N6 P2 108.4(3) . . ? N7 N6 Lu2 105.7(3) . . ? P2 N6 Lu2 145.8(2) . . ? N8 N7 N6 110.7(4) . . ? N7 N8 C33 110.1(4) . . ? N7 N8 Lu2 93.1(3) . . ? C33 N8 Lu2 156.7(3) . . ? C2 C1 Lu1 102.2(4) . . ? C2 C1 Lu2 151.9(4) . . ? Lu1 C1 Lu2 99.78(19) . . ? C1 C2 C3 175.4(6) . . ? C4 C3 C8 119.7(5) . . ? C4 C3 C2 120.4(5) . . ? C8 C3 C2 119.9(6) . . ? C5 C4 C3 120.3(6) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 119.7(7) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C7 C6 C5 120.3(6) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 120.3(6) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C3 119.7(6) . . ? C7 C8 H8 120.2 . . ? C3 C8 H8 120.2 . . ? C10 C9 Lu2 100.5(4) . . ? C10 C9 Lu1 159.7(4) . . ? Lu2 C9 Lu1 99.8(2) . . ? C9 C10 C11 175.1(6) . . ? C12 C11 C16 119.8(6) . . ? C12 C11 C10 119.4(6) . . ? C16 C11 C10 120.7(6) . . ? C11 C12 C13 119.5(7) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 119.5(8) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.6(7) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 122.0(8) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C15 C16 C11 118.5(8) . . ? C15 C16 H16 120.7 . . ? C11 C16 H16 120.7 . . ? C18 C17 Lu1 165.5(5) . . ? C17 C18 C19 175.1(6) . . ? C24 C19 C20 118.6(6) . . ? C24 C19 C18 121.4(6) . . ? C20 C19 C18 120.0(5) . . ? C21 C20 C19 121.4(6) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C22 C21 C20 119.3(7) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C23 C22 C21 120.5(7) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120.0(7) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C19 C24 C23 120.2(6) . . ? C19 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 Lu2 170.9(5) . . ? C25 C26 C27 177.2(6) . . ? C32 C27 C28 118.0(7) . . ? C32 C27 C26 122.4(7) . . ? C28 C27 C26 119.6(6) . . ? C27 C28 C29 121.4(7) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C30 C29 C28 119.4(8) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C31 C30 C29 120.3(8) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.6(9) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C27 C32 C31 120.2(8) . . ? C27 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C38 121.3(6) . . ? C34 C33 N8 118.5(5) . . ? C38 C33 N8 120.2(5) . . ? C33 C34 C35 118.3(6) . . ? C33 C34 C40 121.2(6) . . ? C35 C34 C40 120.5(6) . . ? C36 C35 C34 122.7(7) . . ? C36 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? C35 C36 C37 117.5(6) . . ? C35 C36 C41 121.5(7) . . ? C37 C36 C41 121.0(7) . . ? C36 C37 C38 122.4(6) . . ? C36 C37 H37 118.8 . . ? C38 C37 H37 118.8 . . ? C33 C38 C37 117.8(6) . . ? C33 C38 C39 123.0(5) . . ? C37 C38 C39 119.2(6) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34 C40 H40A 109.5 . . ? C34 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C34 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C47 C42 C43 121.0(5) . . ? C47 C42 N4 117.2(5) . . ? C43 C42 N4 121.8(5) . . ? C44 C43 C42 117.8(5) . . ? C44 C43 C48 119.9(5) . . ? C42 C43 C48 122.3(5) . . ? C45 C44 C43 123.2(6) . . ? C45 C44 H44 118.4 . . ? C43 C44 H44 118.4 . . ? C44 C45 C46 117.0(6) . . ? C44 C45 C49 122.1(6) . . ? C46 C45 C49 120.9(6) . . ? C47 C46 C45 122.7(6) . . ? C47 C46 H46 118.7 . . ? C45 C46 H46 118.7 . . ? C46 C47 C42 118.0(5) . . ? C46 C47 C50 120.9(5) . . ? C42 C47 C50 121.0(5) . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C45 C49 H49A 109.5 . . ? C45 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C45 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C56 C51 C52 119.6(5) . . ? C56 C51 P1 124.7(5) . . ? C52 C51 P1 115.6(4) . . ? C53 C52 C51 119.6(6) . . ? C53 C52 H52 120.2 . . ? C51 C52 H52 120.2 . . ? C54 C53 C52 119.4(6) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C55 C54 C53 121.3(6) . . ? C55 C54 H54 119.3 . . ? C53 C54 H54 119.3 . . ? C54 C55 C56 119.9(6) . . ? C54 C55 H55 120.1 . . ? C56 C55 H55 120.1 . . ? C51 C56 C55 120.2(6) . . ? C51 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C58 C57 C62 120.3(5) . . ? C58 C57 P1 119.9(4) . . ? C62 C57 P1 119.7(5) . . ? C57 C58 C59 118.6(6) . . ? C57 C58 H58 120.7 . . ? C59 C58 H58 120.7 . . ? C60 C59 C58 120.3(7) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C61 C60 C59 121.0(6) . . ? C61 C60 H60 119.5 . . ? C59 C60 H60 119.5 . . ? C62 C61 C60 119.2(7) . . ? C62 C61 H61 120.4 . . ? C60 C61 H61 120.4 . . ? C61 C62 C57 120.7(6) . . ? C61 C62 H62 119.6 . . ? C57 C62 H62 119.6 . . ? C64 C63 C68 120.5(5) . . ? C64 C63 P1 115.7(4) . . ? C68 C63 P1 122.9(4) . . ? C65 C64 C63 120.4(6) . . ? C65 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C66 C65 C64 119.8(6) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C65 C66 C67 120.3(6) . . ? C65 C66 H66 119.8 . . ? C67 C66 H66 119.8 . . ? C66 C67 C68 122.1(6) . . ? C66 C67 H67 119.0 . . ? C68 C67 H67 119.0 . . ? C67 C68 C63 116.9(5) . . ? C67 C68 C69 119.0(5) . . ? C63 C68 C69 124.1(5) . . ? N1 C69 C68 112.4(4) . . ? N1 C69 H69A 109.1 . . ? C68 C69 H69A 109.1 . . ? N1 C69 H69B 109.1 . . ? C68 C69 H69B 109.1 . . ? H69A C69 H69B 107.9 . . ? C71 C70 N1 121.3(5) . . ? C71 C70 C75 118.3(5) . . ? N1 C70 C75 120.4(5) . . ? C72 C71 C70 119.6(6) . . ? C72 C71 C77 119.9(6) . . ? C70 C71 C77 120.5(5) . . ? C73 C72 C71 122.0(6) . . ? C73 C72 H72 119.0 . . ? C71 C72 H72 119.0 . . ? C74 C73 C72 119.0(6) . . ? C74 C73 H73 120.5 . . ? C72 C73 H73 120.5 . . ? C73 C74 C75 121.8(6) . . ? C73 C74 H74 119.1 . . ? C75 C74 H74 119.1 . . ? C74 C75 C70 119.1(6) . . ? C74 C75 C76 119.8(5) . . ? C70 C75 C76 121.1(5) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C71 C77 H77A 109.5 . . ? C71 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C71 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C79 C78 C83 119.8(5) . . ? C79 C78 P2 116.5(4) . . ? C83 C78 P2 123.1(4) . . ? C78 C79 C80 120.3(6) . . ? C78 C79 H79 119.9 . . ? C80 C79 H79 119.9 . . ? C81 C80 C79 118.6(6) . . ? C81 C80 H80 120.7 . . ? C79 C80 H80 120.7 . . ? C82 C81 C80 121.4(6) . . ? C82 C81 H81 119.3 . . ? C80 C81 H81 119.3 . . ? C81 C82 C83 120.4(6) . . ? C81 C82 H82 119.8 . . ? C83 C82 H82 119.8 . . ? C78 C83 C82 119.5(6) . . ? C78 C83 H83 120.2 . . ? C82 C83 H83 120.2 . . ? C89 C84 C85 119.5(5) . . ? C89 C84 P2 119.7(4) . . ? C85 C84 P2 120.8(4) . . ? C86 C85 C84 119.6(6) . . ? C86 C85 H85 120.2 . . ? C84 C85 H85 120.2 . . ? C87 C86 C85 119.5(6) . . ? C87 C86 H86 120.2 . . ? C85 C86 H86 120.2 . . ? C88 C87 C86 121.6(6) . . ? C88 C87 H87 119.2 . . ? C86 C87 H87 119.2 . . ? C87 C88 C89 118.8(6) . . ? C87 C88 H88 120.6 . . ? C89 C88 H88 120.6 . . ? C84 C89 C88 121.0(6) . . ? C84 C89 H89 119.5 . . ? C88 C89 H89 119.5 . . ? C91 C90 C95 120.5(5) . . ? C91 C90 P2 117.6(4) . . ? C95 C90 P2 121.6(4) . . ? C92 C91 C90 120.7(6) . . ? C92 C91 H91 119.6 . . ? C90 C91 H91 119.6 . . ? C91 C92 C93 120.0(6) . . ? C91 C92 H92 120.0 . . ? C93 C92 H92 120.0 . . ? C94 C93 C92 119.2(6) . . ? C94 C93 H93 120.4 . . ? C92 C93 H93 120.4 . . ? C93 C94 C95 122.4(6) . . ? C93 C94 H94 118.8 . . ? C95 C94 H94 118.8 . . ? C94 C95 C90 117.2(5) . . ? C94 C95 C96 118.7(5) . . ? C90 C95 C96 123.9(5) . . ? N5 C96 C95 110.7(4) . . ? N5 C96 H96A 109.5 . . ? C95 C96 H96A 109.5 . . ? N5 C96 H96B 109.5 . . ? C95 C96 H96B 109.5 . . ? H96A C96 H96B 108.1 . . ? C102 C97 C98 119.2(5) . . ? C102 C97 N5 120.6(5) . . ? C98 C97 N5 120.2(5) . . ? C99 C98 C97 119.0(6) . . ? C99 C98 C104 119.4(5) . . ? C97 C98 C104 121.6(5) . . ? C100 C99 C98 121.7(6) . . ? C100 C99 H99 119.1 . . ? C98 C99 H99 119.1 . . ? C99 C100 C101 118.8(6) . . ? C99 C100 H100 120.6 . . ? C101 C100 H100 120.6 . . ? C102 C101 C100 121.2(6) . . ? C102 C101 H101 119.4 . . ? C100 C101 H101 119.4 . . ? C101 C102 C97 120.1(5) . . ? C101 C102 C103 118.8(5) . . ? C97 C102 C103 121.1(5) . . ? C102 C103 H10A 109.5 . . ? C102 C103 H10B 109.5 . . ? H10A C103 H10B 109.5 . . ? C102 C103 H10C 109.5 . . ? H10A C103 H10C 109.5 . . ? H10B C103 H10C 109.5 . . ? C98 C104 H10D 109.5 . . ? C98 C104 H10E 109.5 . . ? H10D C104 H10E 109.5 . . ? C98 C104 H10F 109.5 . . ? H10D C104 H10F 109.5 . . ? H10E C104 H10F 109.5 . . ? C106 C105 C110 120.0 . . ? C106 C105 H105 120.0 . . ? C110 C105 H105 120.0 . . ? C107 C106 C105 120.0 . . ? C107 C106 H106 120.0 . . ? C105 C106 H106 120.0 . . ? C106 C107 C108 120.0 . . ? C106 C107 H107 120.0 . . ? C108 C107 H107 120.0 . . ? C109 C108 C107 120.0 . . ? C109 C108 H108 120.0 . . ? C107 C108 H108 120.0 . . ? C108 C109 C110 120.0 . . ? C108 C109 H109 120.0 . . ? C110 C109 H109 120.0 . . ? C109 C110 C105 120.0 . . ? C109 C110 H110 120.0 . . ? C105 C110 H110 120.0 . . ? C116 C111 C112 122.5 . . ? C116 C111 H111 118.7 . . ? C112 C111 H111 118.7 . . ? C113 C112 C111 116.8 . . ? C113 C112 H112 121.6 . . ? C111 C112 H112 121.6 . . ? C114 C113 C112 121.3 . . ? C114 C113 H113 119.4 . . ? C112 C113 H113 119.4 . . ? C113 C114 C115 120.6 . . ? C113 C114 H114 119.7 . . ? C115 C114 H114 119.7 . . ? C114 C115 C116 122.3 . . ? C114 C115 H115 118.9 . . ? C116 C115 H115 118.9 . . ? C115 C116 C111 116.5 . . ? C115 C116 H116 121.8 . . ? C111 C116 H116 121.8 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.410 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.120 # Attachment 'cif_file_of_complex_.txt' data_complex_3a _database_code_depnum_ccdc_archive 'CCDC 670208' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H80 Lu N10 P Si2' _chemical_formula_weight 1227.48 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.1586(10) _cell_length_b 21.8677(17) _cell_length_c 12.8260(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.5040(10) _cell_angle_gamma 90.00 _cell_volume 3150.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 1.675 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6221 _exptl_absorpt_correction_T_max 0.9406 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 17814 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.1256 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.05 _reflns_number_total 11264 _reflns_number_gt 8638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^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 -0.021(8) _refine_ls_number_reflns 11264 _refine_ls_number_parameters 685 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7075(7) 0.1942(4) 0.3084(7) 0.0274(19) Uani 1 1 d . . . C2 C 0.7616(7) 0.1798(4) 0.2366(7) 0.039(2) Uani 1 1 d . . . H2 H 0.7545 0.1403 0.2082 0.046 Uiso 1 1 calc R . . C3 C 0.8270(10) 0.2222(6) 0.2046(10) 0.044(3) Uani 1 1 d . . . H3 H 0.8651 0.2111 0.1569 0.053 Uiso 1 1 calc R . . C4 C 0.8347(11) 0.2808(6) 0.2446(10) 0.051(3) Uani 1 1 d . . . H4 H 0.8760 0.3103 0.2219 0.061 Uiso 1 1 calc R . . C5 C 0.7817(9) 0.2962(4) 0.3179(9) 0.048(3) Uani 1 1 d . . . H5A H 0.7902 0.3359 0.3460 0.058 Uiso 1 1 calc R . . C6 C 0.7157(6) 0.2545(7) 0.3517(6) 0.0345(19) Uani 1 1 d . . . C7 C 0.6601(7) 0.2771(3) 0.4328(7) 0.0321(19) Uani 1 1 d . . . H7A H 0.6495 0.2428 0.4759 0.038 Uiso 1 1 calc R . . H7B H 0.7140 0.3058 0.4855 0.038 Uiso 1 1 calc R . . C8 C 0.5546(8) 0.3721(4) 0.3633(7) 0.0318(19) Uani 1 1 d . . . C9 C 0.5136(7) 0.3994(4) 0.2558(7) 0.039(2) Uani 1 1 d . . . C10 C 0.5189(9) 0.4627(4) 0.2457(9) 0.055(3) Uani 1 1 d . . . H10 H 0.4922 0.4803 0.1743 0.067 Uiso 1 1 calc R . . C11 C 0.5624(9) 0.4992(4) 0.3383(10) 0.055(3) Uani 1 1 d . . . H11 H 0.5646 0.5414 0.3295 0.066 Uiso 1 1 calc R . . C12 C 0.6027(8) 0.4746(4) 0.4435(9) 0.049(3) Uani 1 1 d . . . H12 H 0.6327 0.5001 0.5063 0.059 Uiso 1 1 calc R . . C13 C 0.5993(8) 0.4108(4) 0.4584(8) 0.040(2) Uani 1 1 d . . . C14 C 0.6375(9) 0.3865(4) 0.5763(8) 0.048(3) Uani 1 1 d . . . H14A H 0.5951 0.3494 0.5758 0.072 Uiso 1 1 calc R . . H14B H 0.6204 0.4163 0.6231 0.072 Uiso 1 1 calc R . . H14C H 0.7214 0.3784 0.6056 0.072 Uiso 1 1 calc R . . C15 C 0.4655(9) 0.3608(4) 0.1503(7) 0.055(3) Uani 1 1 d . . . H15A H 0.5291 0.3374 0.1433 0.083 Uiso 1 1 calc R . . H15B H 0.4314 0.3869 0.0856 0.083 Uiso 1 1 calc R . . H15C H 0.4055 0.3337 0.1549 0.083 Uiso 1 1 calc R . . C16 C 0.7188(7) 0.1166(3) 0.4966(6) 0.0297(19) Uani 1 1 d . . . C17 C 0.8377(7) 0.1299(4) 0.5474(7) 0.037(2) Uani 1 1 d . . . H17 H 0.8762 0.1501 0.5071 0.045 Uiso 1 1 calc R . . C18 C 0.8999(8) 0.1136(4) 0.6572(8) 0.051(3) Uani 1 1 d . . . H18 H 0.9801 0.1237 0.6914 0.061 Uiso 1 1 calc R . . C19 C 0.8461(9) 0.0823(4) 0.7180(7) 0.048(3) Uani 1 1 d . . . H19 H 0.8892 0.0713 0.7926 0.057 Uiso 1 1 calc R . . C20 C 0.7291(8) 0.0679(4) 0.6672(7) 0.041(2) Uani 1 1 d . . . H20 H 0.6928 0.0462 0.7076 0.049 Uiso 1 1 calc R . . C21 C 0.6626(8) 0.0845(4) 0.5575(8) 0.034(2) Uani 1 1 d . . . H21 H 0.5822 0.0748 0.5244 0.041 Uiso 1 1 calc R . . C22 C 0.6161(7) 0.0676(3) 0.2694(6) 0.0279(18) Uani 1 1 d . . . C23 C 0.6566(7) 0.0109(3) 0.3190(7) 0.0318(19) Uani 1 1 d . . . H23 H 0.6996 0.0080 0.3964 0.038 Uiso 1 1 calc R . . C24 C 0.6325(8) -0.0407(4) 0.2529(7) 0.040(2) Uani 1 1 d . . . H24 H 0.6573 -0.0787 0.2864 0.048 Uiso 1 1 calc R . . C25 C 0.5736(8) -0.0372(4) 0.1404(7) 0.043(2) Uani 1 1 d . . . H25 H 0.5597 -0.0725 0.0967 0.052 Uiso 1 1 calc R . . C26 C 0.5336(8) 0.0186(4) 0.0894(7) 0.045(2) Uani 1 1 d . . . H26 H 0.4926 0.0208 0.0116 0.054 Uiso 1 1 calc R . . C27 C 0.5544(8) 0.0714(4) 0.1539(6) 0.039(2) Uani 1 1 d . . . H27 H 0.5271 0.1090 0.1199 0.047 Uiso 1 1 calc R . . C28 C 0.2156(7) 0.3289(3) 0.5518(6) 0.0309(19) Uani 1 1 d . . . C29 C 0.2101(7) 0.3812(4) 0.4842(7) 0.033(2) Uani 1 1 d . . . C30 C 0.1095(8) 0.4195(4) 0.4562(7) 0.041(2) Uani 1 1 d . . . H30 H 0.1058 0.4538 0.4121 0.050 Uiso 1 1 calc R . . C31 C 0.0157(8) 0.4092(4) 0.4908(7) 0.044(2) Uani 1 1 d . . . C32 C 0.0269(8) 0.3577(4) 0.5586(7) 0.044(2) Uani 1 1 d . . . H32 H -0.0334 0.3495 0.5844 0.053 Uiso 1 1 calc R . . C33 C 0.1218(8) 0.3189(4) 0.5889(7) 0.038(2) Uani 1 1 d . . . C34 C 0.1302(8) 0.2647(4) 0.6672(7) 0.056(3) Uani 1 1 d . . . H34A H 0.0628 0.2650 0.6887 0.085 Uiso 1 1 calc R . . H34B H 0.2021 0.2679 0.7334 0.085 Uiso 1 1 calc R . . H34C H 0.1310 0.2272 0.6285 0.085 Uiso 1 1 calc R . . C35 C 0.3078(7) 0.4000(4) 0.4489(8) 0.044(2) Uani 1 1 d . . . H35A H 0.3830 0.3898 0.5073 0.065 Uiso 1 1 calc R . . H35B H 0.3038 0.4433 0.4359 0.065 Uiso 1 1 calc R . . H35C H 0.3000 0.3790 0.3807 0.065 Uiso 1 1 calc R . . C36 C -0.0904(8) 0.4516(4) 0.4602(8) 0.055(3) Uani 1 1 d . . . H36A H -0.0663 0.4925 0.4516 0.083 Uiso 1 1 calc R . . H36B H -0.1209 0.4509 0.5191 0.083 Uiso 1 1 calc R . . H36C H -0.1512 0.4384 0.3907 0.083 Uiso 1 1 calc R . . C37 C 0.4756(7) 0.1991(4) 0.6508(6) 0.035(2) Uani 1 1 d . . . H37A H 0.4986 0.1582 0.6380 0.042 Uiso 1 1 calc R . . H37B H 0.4044 0.1950 0.6672 0.042 Uiso 1 1 calc R . . C38 C 0.5508(10) 0.3017(4) 0.8318(8) 0.064(3) Uani 1 1 d . . . H38A H 0.6154 0.3164 0.8973 0.096 Uiso 1 1 calc R . . H38B H 0.4829 0.2939 0.8506 0.096 Uiso 1 1 calc R . . H38C H 0.5306 0.3319 0.7731 0.096 Uiso 1 1 calc R . . C39 C 0.6203(9) 0.1672(5) 0.8889(8) 0.060(3) Uani 1 1 d . . . H39A H 0.6539 0.1320 0.8674 0.090 Uiso 1 1 calc R . . H39B H 0.5455 0.1565 0.8929 0.090 Uiso 1 1 calc R . . H39C H 0.6739 0.1815 0.9614 0.090 Uiso 1 1 calc R . . C40 C 0.7357(7) 0.2410(7) 0.7574(7) 0.054(3) Uani 1 1 d . . . H40A H 0.7627 0.2026 0.7400 0.081 Uiso 1 1 calc R . . H40B H 0.7955 0.2579 0.8242 0.081 Uiso 1 1 calc R . . H40C H 0.7210 0.2688 0.6955 0.081 Uiso 1 1 calc R . . C41 C 0.1886(7) 0.1706(4) 0.0274(6) 0.0292(19) Uani 1 1 d . . . C42 C 0.1031(7) 0.1227(4) -0.0006(7) 0.033(2) Uani 1 1 d . . . C43 C 0.1199(7) 0.0722(4) -0.0585(7) 0.039(2) Uani 1 1 d . . . H43 H 0.0673 0.0394 -0.0728 0.047 Uiso 1 1 calc R . . C44 C 0.2133(8) 0.0693(4) -0.0957(7) 0.047(2) Uani 1 1 d . . . C45 C 0.2913(8) 0.1173(4) -0.0720(7) 0.045(2) Uani 1 1 d . . . H45 H 0.3531 0.1163 -0.0978 0.055 Uiso 1 1 calc R . . C46 C 0.2802(7) 0.1682(4) -0.0095(6) 0.034(2) Uani 1 1 d . . . C47 C -0.0047(8) 0.1264(4) 0.0313(8) 0.044(3) Uani 1 1 d . . . H47A H 0.0210 0.1334 0.1110 0.066 Uiso 1 1 calc R . . H47B H -0.0483 0.0888 0.0120 0.066 Uiso 1 1 calc R . . H47C H -0.0549 0.1595 -0.0089 0.066 Uiso 1 1 calc R . . C48 C 0.3691(8) 0.2197(4) 0.0105(8) 0.053(3) Uani 1 1 d . . . H48A H 0.3279 0.2582 -0.0030 0.079 Uiso 1 1 calc R . . H48B H 0.4101 0.2154 -0.0398 0.079 Uiso 1 1 calc R . . H48C H 0.4255 0.2183 0.0872 0.079 Uiso 1 1 calc R . . C49 C 0.2271(9) 0.0136(5) -0.1611(9) 0.074(4) Uani 1 1 d . . . H49A H 0.2699 0.0249 -0.2073 0.110 Uiso 1 1 calc R . . H49B H 0.1498 -0.0016 -0.2080 0.110 Uiso 1 1 calc R . . H49C H 0.2702 -0.0178 -0.1090 0.110 Uiso 1 1 calc R . . C50 C 0.1084(7) 0.3124(4) 0.1873(7) 0.035(2) Uani 1 1 d . . . H50A H 0.0990 0.3335 0.2499 0.041 Uiso 1 1 calc R . . H50B H 0.0526 0.2785 0.1669 0.041 Uiso 1 1 calc R . . C51 C 0.1497(9) 0.4392(4) 0.1104(9) 0.068(3) Uani 1 1 d . . . H51A H 0.2318 0.4315 0.1241 0.103 Uiso 1 1 calc R . . H51B H 0.1430 0.4532 0.1787 0.103 Uiso 1 1 calc R . . H51C H 0.1190 0.4699 0.0529 0.103 Uiso 1 1 calc R . . C52 C -0.0996(10) 0.3817(5) 0.0258(10) 0.080(4) Uani 1 1 d . . . H52A H -0.1103 0.4029 0.0867 0.121 Uiso 1 1 calc R . . H52B H -0.1413 0.3434 0.0129 0.121 Uiso 1 1 calc R . . H52C H -0.1304 0.4062 -0.0414 0.121 Uiso 1 1 calc R . . C53 C 0.0823(11) 0.3390(5) -0.0656(9) 0.074(3) Uani 1 1 d . . . H53A H 0.0450 0.3669 -0.1269 0.111 Uiso 1 1 calc R . . H53B H 0.0465 0.2993 -0.0853 0.111 Uiso 1 1 calc R . . H53C H 0.1657 0.3362 -0.0511 0.111 Uiso 1 1 calc R . . C54 C 0.2289(7) 0.0962(3) 0.3129(6) 0.0284(18) Uani 1 1 d . . . C55 C 0.2154(7) 0.0415(4) 0.2532(6) 0.0299(19) Uani 1 1 d . . . C56 C 0.1109(7) 0.0082(4) 0.2320(7) 0.036(2) Uani 1 1 d . . . H56 H 0.1013 -0.0283 0.1925 0.044 Uiso 1 1 calc R . . C57 C 0.0216(7) 0.0261(4) 0.2659(7) 0.036(2) Uani 1 1 d . . . C58 C 0.0378(7) 0.0801(4) 0.3254(7) 0.035(2) Uani 1 1 d . . . H58 H -0.0208 0.0928 0.3505 0.042 Uiso 1 1 calc R . . C59 C 0.1386(7) 0.1162(3) 0.3491(6) 0.0297(19) Uani 1 1 d . . . C60 C 0.1488(8) 0.1766(4) 0.4120(8) 0.045(2) Uani 1 1 d . . . H60A H 0.0780 0.1831 0.4267 0.068 Uiso 1 1 calc R . . H60B H 0.1584 0.2096 0.3667 0.068 Uiso 1 1 calc R . . H60C H 0.2166 0.1752 0.4822 0.068 Uiso 1 1 calc R . . C61 C 0.3021(7) 0.0179(4) 0.2042(7) 0.039(2) Uani 1 1 d . . . H61A H 0.3733 0.0041 0.2641 0.058 Uiso 1 1 calc R . . H61B H 0.3216 0.0502 0.1634 0.058 Uiso 1 1 calc R . . H61C H 0.2667 -0.0155 0.1540 0.058 Uiso 1 1 calc R . . C62 C -0.0913(8) -0.0093(4) 0.2374(8) 0.052(3) Uani 1 1 d . . . H62A H -0.1297 0.0026 0.2872 0.078 Uiso 1 1 calc R . . H62B H -0.0737 -0.0522 0.2458 0.078 Uiso 1 1 calc R . . H62C H -0.1432 -0.0009 0.1608 0.078 Uiso 1 1 calc R . . Lu Lu 0.39550(2) 0.249439(17) 0.35825(2) 0.02513(8) Uani 1 1 d . . . N1 N 0.5443(6) 0.3071(3) 0.3738(6) 0.0346(18) Uani 1 1 d . . . N2 N 0.4994(6) 0.1617(3) 0.3377(5) 0.0242(15) Uani 1 1 d . . . N3 N 0.4209(5) 0.1151(3) 0.3314(5) 0.0255(14) Uani 1 1 d . . . N4 N 0.3241(5) 0.1380(3) 0.3335(5) 0.0237(14) Uani 1 1 d . . . N5 N 0.4423(6) 0.2325(3) 0.5445(5) 0.0258(18) Uani 1 1 d . . . N6 N 0.3581(6) 0.2741(3) 0.5186(6) 0.0340(17) Uani 1 1 d . . . N7 N 0.3103(6) 0.2877(3) 0.5909(5) 0.0335(16) Uani 1 1 d . . . N8 N 0.2290(5) 0.2868(3) 0.2281(5) 0.0255(14) Uani 1 1 d . . . N9 N 0.2490(5) 0.2406(4) 0.1710(5) 0.0268(17) Uani 1 1 d . . . N10 N 0.1604(6) 0.2215(3) 0.0826(5) 0.0333(17) Uani 1 1 d . . . P P 0.63103(19) 0.13573(9) 0.35276(17) 0.0264(5) Uani 1 1 d . . . Si1 Si 0.5965(2) 0.22927(10) 0.78154(19) 0.0405(7) Uani 1 1 d . . . Si2 Si 0.0626(3) 0.36724(12) 0.0628(2) 0.0415(7) Uani 1 1 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 C1 0.026(5) 0.030(5) 0.026(4) 0.001(4) 0.009(4) 0.003(4) C2 0.026(5) 0.049(6) 0.045(5) -0.001(5) 0.017(4) 0.000(4) C3 0.039(6) 0.051(7) 0.055(7) -0.003(5) 0.034(5) -0.004(5) C4 0.053(8) 0.049(7) 0.069(8) 0.003(6) 0.043(7) -0.010(6) C5 0.050(7) 0.029(5) 0.070(7) -0.003(5) 0.029(6) -0.007(5) C6 0.025(4) 0.038(6) 0.039(4) -0.004(6) 0.010(3) -0.004(6) C7 0.027(5) 0.025(4) 0.042(5) 0.002(4) 0.010(4) -0.002(3) C8 0.027(5) 0.034(5) 0.038(5) 0.001(4) 0.017(4) -0.002(4) C9 0.039(6) 0.038(5) 0.051(6) 0.005(4) 0.028(5) -0.003(4) C10 0.072(8) 0.043(6) 0.061(7) 0.017(5) 0.036(6) -0.001(5) C11 0.058(7) 0.022(5) 0.090(9) 0.003(5) 0.033(6) -0.004(5) C12 0.047(6) 0.031(6) 0.071(7) -0.012(5) 0.023(5) 0.002(4) C13 0.032(5) 0.031(5) 0.058(6) -0.005(4) 0.021(5) -0.007(4) C14 0.055(7) 0.039(7) 0.048(6) -0.011(5) 0.016(5) -0.001(5) C15 0.069(7) 0.056(7) 0.038(5) 0.007(5) 0.019(5) -0.007(5) C16 0.027(5) 0.026(5) 0.033(4) -0.009(4) 0.008(4) 0.002(3) C17 0.032(5) 0.033(5) 0.039(5) -0.002(4) 0.005(4) -0.003(4) C18 0.030(6) 0.060(7) 0.048(6) -0.006(5) -0.002(5) -0.002(5) C19 0.053(7) 0.038(6) 0.033(5) 0.005(4) -0.006(5) 0.009(5) C20 0.054(6) 0.033(5) 0.032(5) -0.004(4) 0.014(5) 0.003(4) C21 0.034(5) 0.026(6) 0.041(6) -0.006(4) 0.013(5) 0.005(4) C22 0.025(5) 0.025(5) 0.034(5) -0.001(4) 0.012(4) -0.001(3) C23 0.042(5) 0.025(5) 0.028(4) -0.001(4) 0.013(4) 0.000(4) C24 0.048(6) 0.025(5) 0.049(6) -0.006(4) 0.021(5) 0.002(4) C25 0.051(7) 0.030(5) 0.048(6) -0.016(5) 0.019(5) -0.001(4) C26 0.049(6) 0.053(6) 0.023(5) -0.014(4) 0.003(4) 0.005(5) C27 0.051(6) 0.037(5) 0.025(4) 0.000(4) 0.011(4) 0.007(4) C28 0.032(5) 0.025(5) 0.034(5) -0.008(4) 0.010(4) -0.003(4) C29 0.032(5) 0.035(5) 0.035(5) -0.010(4) 0.016(4) 0.001(4) C30 0.051(6) 0.033(5) 0.037(5) -0.010(4) 0.012(5) -0.001(4) C31 0.047(6) 0.042(6) 0.039(5) -0.009(4) 0.012(5) 0.008(5) C32 0.036(6) 0.053(6) 0.051(6) -0.012(5) 0.025(5) -0.003(4) C33 0.048(6) 0.043(6) 0.028(4) -0.005(4) 0.018(4) 0.002(4) C34 0.085(7) 0.050(9) 0.057(6) -0.002(5) 0.053(5) 0.000(5) C35 0.044(6) 0.033(5) 0.060(6) 0.000(4) 0.027(5) 0.003(4) C36 0.048(7) 0.054(7) 0.068(7) 0.000(5) 0.027(5) 0.009(5) C37 0.046(6) 0.026(5) 0.038(5) 0.002(4) 0.020(4) 0.007(4) C38 0.078(8) 0.056(7) 0.052(6) -0.022(5) 0.019(6) 0.007(6) C39 0.066(8) 0.065(8) 0.052(6) 0.017(6) 0.026(6) 0.014(6) C40 0.050(5) 0.057(8) 0.048(5) 0.004(7) 0.011(4) 0.008(7) C41 0.030(5) 0.030(5) 0.023(4) 0.008(3) 0.005(4) 0.007(4) C42 0.022(5) 0.049(6) 0.027(5) -0.003(4) 0.009(4) -0.002(4) C43 0.032(5) 0.037(5) 0.039(5) -0.013(4) 0.003(4) 0.003(4) C44 0.038(6) 0.060(7) 0.033(5) -0.015(5) 0.002(4) 0.009(5) C45 0.036(6) 0.060(7) 0.040(5) -0.011(5) 0.015(4) 0.006(5) C46 0.033(5) 0.042(5) 0.028(4) 0.006(4) 0.013(4) 0.003(4) C47 0.039(6) 0.051(7) 0.041(6) -0.008(5) 0.014(5) -0.002(5) C48 0.050(6) 0.063(7) 0.060(6) -0.016(5) 0.038(5) -0.003(5) C49 0.058(7) 0.084(9) 0.079(8) -0.052(7) 0.027(6) -0.003(6) C50 0.035(5) 0.037(5) 0.035(4) 0.000(4) 0.018(4) 0.003(4) C51 0.088(9) 0.029(6) 0.091(8) 0.008(6) 0.037(7) -0.001(5) C52 0.074(9) 0.072(8) 0.086(8) 0.049(7) 0.020(7) 0.030(7) C53 0.110(10) 0.062(8) 0.061(7) 0.022(6) 0.045(7) 0.024(7) C54 0.025(5) 0.030(5) 0.030(4) 0.000(4) 0.010(4) -0.002(4) C55 0.031(5) 0.026(5) 0.032(4) -0.003(4) 0.011(4) -0.002(4) C56 0.040(6) 0.030(5) 0.035(5) -0.010(4) 0.009(4) -0.009(4) C57 0.037(5) 0.031(5) 0.041(5) -0.001(4) 0.016(4) -0.010(4) C58 0.034(5) 0.036(5) 0.040(5) 0.001(4) 0.020(4) -0.001(4) C59 0.032(5) 0.023(5) 0.032(4) 0.004(4) 0.010(4) 0.005(4) C60 0.041(6) 0.045(6) 0.062(6) -0.012(5) 0.034(5) -0.004(4) C61 0.033(5) 0.035(5) 0.046(5) -0.013(4) 0.013(4) -0.003(4) C62 0.043(6) 0.049(6) 0.068(7) -0.020(5) 0.027(5) -0.012(5) Lu 0.02652(15) 0.02231(14) 0.02672(13) -0.0003(3) 0.01036(11) 0.0005(3) N1 0.039(5) 0.023(4) 0.041(4) 0.001(3) 0.014(4) -0.001(3) N2 0.025(4) 0.022(4) 0.028(4) -0.001(3) 0.012(3) 0.000(3) N3 0.025(4) 0.028(4) 0.022(3) -0.001(3) 0.007(3) -0.001(3) N4 0.025(4) 0.024(4) 0.021(3) 0.005(3) 0.008(3) 0.000(3) N5 0.027(4) 0.025(5) 0.024(3) -0.001(3) 0.008(3) 0.003(3) N6 0.031(4) 0.027(4) 0.047(4) -0.002(3) 0.018(4) -0.008(3) N7 0.039(4) 0.032(4) 0.036(4) -0.002(3) 0.021(4) -0.001(3) N8 0.026(4) 0.019(4) 0.033(4) 0.002(3) 0.013(3) 0.001(3) N9 0.031(3) 0.022(5) 0.029(3) 0.002(4) 0.013(3) 0.001(4) N10 0.043(4) 0.030(4) 0.025(3) -0.001(3) 0.011(3) 0.003(3) P 0.0254(12) 0.0252(12) 0.0278(11) -0.0012(9) 0.0091(10) 0.0025(9) Si1 0.0428(15) 0.0452(19) 0.0299(12) -0.0010(10) 0.0098(11) 0.0082(11) Si2 0.0454(18) 0.0328(15) 0.0439(17) 0.0085(12) 0.0145(15) 0.0087(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.357(11) . ? C1 C6 1.420(15) . ? C1 P 1.797(9) . ? C2 C3 1.381(13) . ? C3 C4 1.372(11) . ? C4 C5 1.369(15) . ? C5 C6 1.389(13) . ? C6 C7 1.523(11) . ? C7 N1 1.474(10) . ? C8 C9 1.406(11) . ? C8 C13 1.410(11) . ? C8 N1 1.438(10) . ? C9 C10 1.395(12) . ? C9 C15 1.510(11) . ? C10 C11 1.358(13) . ? C11 C12 1.358(13) . ? C12 C13 1.413(12) . ? C13 C14 1.499(12) . ? C16 C17 1.370(10) . ? C16 C21 1.407(12) . ? C16 P 1.792(8) . ? C17 C18 1.366(11) . ? C18 C19 1.377(13) . ? C19 C20 1.355(11) . ? C20 C21 1.376(11) . ? C22 C27 1.383(10) . ? C22 C23 1.395(10) . ? C22 P 1.802(8) . ? C23 C24 1.374(10) . ? C24 C25 1.345(11) . ? C25 C26 1.383(11) . ? C26 C27 1.385(10) . ? C28 N7 1.395(10) . ? C28 C33 1.411(11) . ? C28 C29 1.422(11) . ? C29 C30 1.411(11) . ? C29 C35 1.483(11) . ? C30 C31 1.392(12) . ? C31 C32 1.398(12) . ? C31 C36 1.512(11) . ? C32 C33 1.364(11) . ? C33 C34 1.531(12) . ? C37 N5 1.461(9) . ? C37 Si1 1.876(8) . ? C38 Si1 1.872(9) . ? C39 Si1 1.875(9) . ? C40 Si1 1.852(9) . ? C41 C46 1.368(11) . ? C41 C42 1.422(11) . ? C41 N10 1.429(9) . ? C42 C43 1.390(11) . ? C42 C47 1.517(12) . ? C43 C44 1.391(12) . ? C44 C45 1.369(12) . ? C44 C49 1.524(12) . ? C45 C46 1.407(11) . ? C46 C48 1.513(11) . ? C50 N8 1.467(9) . ? C50 Si2 1.902(8) . ? C51 Si2 1.864(9) . ? C52 Si2 1.870(11) . ? C53 Si2 1.859(11) . ? C54 C55 1.396(10) . ? C54 C59 1.415(10) . ? C54 N4 1.419(9) . ? C55 C56 1.397(10) . ? C55 C61 1.510(11) . ? C56 C57 1.372(11) . ? C57 C58 1.378(11) . ? C57 C62 1.494(11) . ? C58 C59 1.390(10) . ? C59 C60 1.529(10) . ? Lu N1 2.151(7) . ? Lu N8 2.228(6) . ? Lu N5 2.264(6) . ? Lu N6 2.332(7) . ? Lu N2 2.367(7) . ? Lu N9 2.388(6) . ? Lu N4 2.565(6) . ? N2 N3 1.377(8) . ? N2 P 1.638(7) . ? N3 N4 1.289(8) . ? N5 N6 1.313(8) . ? N6 N7 1.304(9) . ? N8 N9 1.323(9) . ? N9 N10 1.298(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.1(8) . . ? C2 C1 P 119.6(7) . . ? C6 C1 P 120.3(6) . . ? C1 C2 C3 122.0(10) . . ? C4 C3 C2 118.7(12) . . ? C5 C4 C3 120.3(12) . . ? C4 C5 C6 122.2(10) . . ? C5 C6 C1 116.7(8) . . ? C5 C6 C7 117.4(11) . . ? C1 C6 C7 125.9(9) . . ? N1 C7 C6 112.4(6) . . ? C9 C8 C13 117.9(8) . . ? C9 C8 N1 120.0(8) . . ? C13 C8 N1 122.0(7) . . ? C10 C9 C8 120.0(9) . . ? C10 C9 C15 119.2(9) . . ? C8 C9 C15 120.8(8) . . ? C11 C10 C9 121.2(9) . . ? C10 C11 C12 120.5(9) . . ? C11 C12 C13 120.5(9) . . ? C8 C13 C12 119.8(9) . . ? C8 C13 C14 121.9(8) . . ? C12 C13 C14 118.2(9) . . ? C17 C16 C21 119.3(7) . . ? C17 C16 P 123.0(6) . . ? C21 C16 P 117.6(6) . . ? C18 C17 C16 120.1(9) . . ? C17 C18 C19 121.3(9) . . ? C20 C19 C18 118.8(8) . . ? C19 C20 C21 121.9(9) . . ? C20 C21 C16 118.6(9) . . ? C27 C22 C23 119.6(7) . . ? C27 C22 P 118.5(6) . . ? C23 C22 P 121.8(6) . . ? C24 C23 C22 119.6(7) . . ? C25 C24 C23 121.0(8) . . ? C24 C25 C26 120.4(8) . . ? C25 C26 C27 120.1(7) . . ? C22 C27 C26 119.4(8) . . ? N7 C28 C33 116.2(7) . . ? N7 C28 C29 125.4(7) . . ? C33 C28 C29 118.4(7) . . ? C30 C29 C28 117.9(8) . . ? C30 C29 C35 118.4(8) . . ? C28 C29 C35 123.6(7) . . ? C31 C30 C29 124.0(8) . . ? C30 C31 C32 115.6(8) . . ? C30 C31 C36 122.7(9) . . ? C32 C31 C36 121.8(9) . . ? C33 C32 C31 123.4(8) . . ? C32 C33 C28 120.8(8) . . ? C32 C33 C34 120.4(8) . . ? C28 C33 C34 118.8(8) . . ? N5 C37 Si1 120.1(6) . . ? C46 C41 C42 119.9(8) . . ? C46 C41 N10 125.7(7) . . ? C42 C41 N10 114.0(7) . . ? C43 C42 C41 118.6(8) . . ? C43 C42 C47 120.3(8) . . ? C41 C42 C47 121.1(8) . . ? C42 C43 C44 121.7(8) . . ? C45 C44 C43 118.4(8) . . ? C45 C44 C49 121.5(9) . . ? C43 C44 C49 120.1(9) . . ? C44 C45 C46 121.6(8) . . ? C41 C46 C45 119.7(8) . . ? C41 C46 C48 122.4(8) . . ? C45 C46 C48 117.9(8) . . ? N8 C50 Si2 118.2(5) . . ? C55 C54 C59 120.1(7) . . ? C55 C54 N4 124.8(7) . . ? C59 C54 N4 114.8(7) . . ? C54 C55 C56 117.4(7) . . ? C54 C55 C61 124.5(7) . . ? C56 C55 C61 118.0(7) . . ? C57 C56 C55 124.1(8) . . ? C56 C57 C58 117.1(7) . . ? C56 C57 C62 122.7(8) . . ? C58 C57 C62 120.1(8) . . ? C57 C58 C59 122.3(8) . . ? C58 C59 C54 118.9(7) . . ? C58 C59 C60 119.6(7) . . ? C54 C59 C60 121.6(7) . . ? N1 Lu N8 110.2(2) . . ? N1 Lu N5 97.8(2) . . ? N8 Lu N5 129.8(2) . . ? N1 Lu N6 102.9(2) . . ? N8 Lu N6 98.5(2) . . ? N5 Lu N6 33.14(19) . . ? N1 Lu N2 91.1(3) . . ? N8 Lu N2 125.7(2) . . ? N5 Lu N2 93.2(2) . . ? N6 Lu N2 125.3(2) . . ? N1 Lu N9 114.7(3) . . ? N8 Lu N9 33.1(2) . . ? N5 Lu N9 146.8(2) . . ? N6 Lu N9 125.7(2) . . ? N2 Lu N9 92.7(3) . . ? N1 Lu N4 143.3(2) . . ? N8 Lu N4 95.0(2) . . ? N5 Lu N4 84.93(18) . . ? N6 Lu N4 99.07(19) . . ? N2 Lu N4 52.1(2) . . ? N9 Lu N4 73.2(2) . . ? C8 N1 C7 112.8(6) . . ? C8 N1 Lu 132.2(6) . . ? C7 N1 Lu 113.0(5) . . ? N3 N2 P 112.0(5) . . ? N3 N2 Lu 102.6(4) . . ? P N2 Lu 143.8(4) . . ? N4 N3 N2 109.2(6) . . ? N3 N4 C54 115.6(6) . . ? N3 N4 Lu 95.9(4) . . ? C54 N4 Lu 148.1(5) . . ? N6 N5 C37 119.6(6) . . ? N6 N5 Lu 76.3(4) . . ? C37 N5 Lu 159.1(5) . . ? N7 N6 N5 119.6(7) . . ? N7 N6 Lu 166.0(5) . . ? N5 N6 Lu 70.6(4) . . ? N6 N7 C28 115.0(6) . . ? N9 N8 C50 117.7(6) . . ? N9 N8 Lu 80.1(4) . . ? C50 N8 Lu 154.8(5) . . ? N10 N9 N8 117.5(6) . . ? N10 N9 Lu 162.7(6) . . ? N8 N9 Lu 66.8(3) . . ? N9 N10 C41 114.0(7) . . ? N2 P C16 111.9(4) . . ? N2 P C1 108.5(4) . . ? C16 P C1 108.4(4) . . ? N2 P C22 110.2(4) . . ? C16 P C22 107.7(4) . . ? C1 P C22 110.3(4) . . ? C40 Si1 C38 110.5(6) . . ? C40 Si1 C39 109.2(5) . . ? C38 Si1 C39 110.0(4) . . ? C40 Si1 C37 110.7(4) . . ? C38 Si1 C37 111.8(4) . . ? C39 Si1 C37 104.5(4) . . ? C53 Si2 C51 108.7(5) . . ? C53 Si2 C52 108.2(5) . . ? C51 Si2 C52 110.6(5) . . ? C53 Si2 C50 116.0(4) . . ? C51 Si2 C50 108.1(4) . . ? C52 Si2 C50 105.2(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.468 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.094 #===========END============= data_complex_3' _database_code_depnum_ccdc_archive 'CCDC 670209' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H89 Lu N10 P Si2' _chemical_formula_weight 1344.64 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' P P 0.1023 0.0942 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.5568(9) _cell_length_b 21.7750(13) _cell_length_c 22.0756(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.3220(10) _cell_angle_gamma 90.00 _cell_volume 6995.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2796 _exptl_absorpt_coefficient_mu 1.515 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6592 _exptl_absorpt_correction_T_max 0.8391 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 38977 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.07 _reflns_number_total 13767 _reflns_number_gt 10545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^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 13767 _refine_ls_number_parameters 761 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N8 N 0.7762(2) 0.59375(15) 0.69554(14) 0.0293(8) Uani 1 1 d . . . Lu1 Lu 0.669387(11) 0.651056(7) 0.755335(7) 0.02336(6) Uani 1 1 d . . . P1 P 0.88600(7) 0.73678(5) 0.81480(4) 0.0258(2) Uani 1 1 d . . . Si1 Si 0.89349(9) 0.52013(6) 0.61963(6) 0.0456(3) Uani 1 1 d . . . Si2 Si 0.48577(9) 0.77600(6) 0.92145(6) 0.0438(3) Uani 1 1 d . . . N1 N 0.6681(2) 0.73799(15) 0.70697(13) 0.0279(8) Uani 1 1 d . . . N2 N 0.8110(2) 0.68123(14) 0.80700(13) 0.0256(7) Uani 1 1 d . . . N3 N 0.8173(2) 0.63698(14) 0.85105(14) 0.0291(8) Uani 1 1 d . . . N4 N 0.7523(2) 0.59881(14) 0.84398(13) 0.0249(7) Uani 1 1 d . . . N5 N 0.5943(2) 0.70407(14) 0.83798(14) 0.0277(7) Uani 1 1 d . . . N6 N 0.5150(2) 0.67765(15) 0.83145(14) 0.0292(8) Uani 1 1 d . . . N7 N 0.5188(2) 0.63460(15) 0.78906(15) 0.0335(8) Uani 1 1 d . . . N9 N 0.7171(2) 0.55764(15) 0.66841(14) 0.0313(8) Uani 1 1 d . . . N10 N 0.6336(2) 0.57153(15) 0.68633(14) 0.0322(8) Uani 1 1 d . . . C1 C 0.8872(3) 0.77779(17) 0.74396(16) 0.0254(9) Uani 1 1 d . . . C2 C 0.9709(3) 0.78620(19) 0.71650(18) 0.0361(10) Uani 1 1 d . . . H2 H 1.0240 0.7700 0.7345 0.043 Uiso 1 1 calc R . . C3 C 0.9767(3) 0.8186(2) 0.66247(19) 0.0438(12) Uani 1 1 d . . . H3 H 1.0329 0.8232 0.6438 0.053 Uiso 1 1 calc R . . C4 C 0.8985(3) 0.84358(19) 0.63708(18) 0.0385(11) Uani 1 1 d . . . H4 H 0.9018 0.8660 0.6013 0.046 Uiso 1 1 calc R . . C5 C 0.8151(3) 0.83583(17) 0.66404(18) 0.0334(10) Uani 1 1 d . . . H5 H 0.7630 0.8537 0.6464 0.040 Uiso 1 1 calc R . . C6 C 0.8067(3) 0.80192(17) 0.71718(17) 0.0259(9) Uani 1 1 d . . . C7 C 0.7115(3) 0.78936(17) 0.74030(17) 0.0292(9) Uani 1 1 d . . . H7A H 0.7155 0.7795 0.7831 0.035 Uiso 1 1 calc R . . H7B H 0.6739 0.8259 0.7355 0.035 Uiso 1 1 calc R . . C8 C 0.6250(3) 0.75746(18) 0.65138(19) 0.0333(10) Uani 1 1 d . . . C9 C 0.6605(3) 0.7399(2) 0.59548(19) 0.0411(11) Uani 1 1 d . . . C10 C 0.6158(4) 0.7581(2) 0.5421(2) 0.0630(16) Uani 1 1 d . . . H10 H 0.6393 0.7461 0.5051 0.076 Uiso 1 1 calc R . . C11 C 0.5379(4) 0.7933(3) 0.5431(3) 0.0711(18) Uani 1 1 d . . . H11 H 0.5096 0.8059 0.5069 0.085 Uiso 1 1 calc R . . C12 C 0.5018(4) 0.8100(2) 0.5974(3) 0.0641(16) Uani 1 1 d . . . H12 H 0.4483 0.8333 0.5977 0.077 Uiso 1 1 calc R . . C13 C 0.5438(3) 0.7929(2) 0.6524(2) 0.0413(11) Uani 1 1 d . . . C14 C 0.7476(3) 0.7026(2) 0.59119(19) 0.0512(13) Uani 1 1 d . . . H14A H 0.7884 0.7127 0.6245 0.077 Uiso 1 1 calc R . . H14B H 0.7769 0.7116 0.5537 0.077 Uiso 1 1 calc R . . H14C H 0.7329 0.6596 0.5927 0.077 Uiso 1 1 calc R . . C15 C 0.5012(3) 0.8110(2) 0.7108(2) 0.0546(14) Uani 1 1 d . . . H15A H 0.5247 0.8503 0.7234 0.082 Uiso 1 1 calc R . . H15B H 0.5158 0.7809 0.7413 0.082 Uiso 1 1 calc R . . H15C H 0.4357 0.8136 0.7052 0.082 Uiso 1 1 calc R . . C16 C 1.0005(3) 0.70838(19) 0.83070(17) 0.0317(10) Uani 1 1 d . . . C17 C 1.0275(3) 0.6528(2) 0.8082(2) 0.0489(12) Uani 1 1 d . . . H17 H 0.9850 0.6281 0.7877 0.059 Uiso 1 1 calc R . . C18 C 1.1176(3) 0.6331(2) 0.8156(3) 0.0624(16) Uani 1 1 d . . . H18 H 1.1351 0.5952 0.8002 0.075 Uiso 1 1 calc R . . C19 C 1.1803(3) 0.6690(3) 0.8453(2) 0.0605(16) Uani 1 1 d . . . H19 H 1.2412 0.6564 0.8490 0.073 Uiso 1 1 calc R . . C20 C 1.1536(3) 0.7234(3) 0.8696(2) 0.0610(16) Uani 1 1 d . . . H20 H 1.1960 0.7472 0.8912 0.073 Uiso 1 1 calc R . . C21 C 1.0640(3) 0.7437(2) 0.86242(19) 0.0477(12) Uani 1 1 d . . . H21 H 1.0465 0.7811 0.8789 0.057 Uiso 1 1 calc R . . C22 C 0.8617(3) 0.78891(18) 0.87550(17) 0.0277(9) Uani 1 1 d . . . C23 C 0.8553(3) 0.8515(2) 0.8666(2) 0.0424(11) Uani 1 1 d . . . H23 H 0.8601 0.8678 0.8279 0.051 Uiso 1 1 calc R . . C24 C 0.8419(4) 0.8900(2) 0.9156(2) 0.0580(14) Uani 1 1 d . . . H24 H 0.8373 0.9322 0.9096 0.070 Uiso 1 1 calc R . . C25 C 0.8353(3) 0.8664(2) 0.9725(2) 0.0533(14) Uani 1 1 d . . . H25 H 0.8265 0.8925 1.0051 0.064 Uiso 1 1 calc R . . C26 C 0.8416(3) 0.8043(2) 0.9819(2) 0.0488(13) Uani 1 1 d . . . H26 H 0.8368 0.7886 1.0209 0.059 Uiso 1 1 calc R . . C27 C 0.8549(3) 0.7653(2) 0.93419(18) 0.0394(11) Uani 1 1 d . . . H27 H 0.8595 0.7232 0.9408 0.047 Uiso 1 1 calc R . . C28 C 0.5649(3) 0.52992(18) 0.66300(18) 0.0312(10) Uani 1 1 d . . . C29 C 0.5348(3) 0.48249(18) 0.69961(18) 0.0340(10) Uani 1 1 d . . . C30 C 0.4629(3) 0.4453(2) 0.6793(2) 0.0400(11) Uani 1 1 d . . . H30 H 0.4426 0.4140 0.7043 0.048 Uiso 1 1 calc R . . C31 C 0.4204(3) 0.4535(2) 0.6228(2) 0.0408(11) Uani 1 1 d . . . C32 C 0.4533(3) 0.4999(2) 0.5865(2) 0.0441(12) Uani 1 1 d . . . H32 H 0.4267 0.5055 0.5482 0.053 Uiso 1 1 calc R . . C33 C 0.5254(3) 0.53909(19) 0.60513(18) 0.0371(10) Uani 1 1 d . . . C34 C 0.5578(3) 0.5893(2) 0.56377(19) 0.0480(12) Uani 1 1 d . . . H34A H 0.5542 0.6281 0.5842 0.072 Uiso 1 1 calc R . . H34B H 0.5196 0.5902 0.5277 0.072 Uiso 1 1 calc R . . H34C H 0.6203 0.5816 0.5530 0.072 Uiso 1 1 calc R . . C35 C 0.5805(3) 0.4706(2) 0.76056(19) 0.0449(12) Uani 1 1 d . . . H35A H 0.6398 0.4525 0.7549 0.067 Uiso 1 1 calc R . . H35B H 0.5432 0.4431 0.7834 0.067 Uiso 1 1 calc R . . H35C H 0.5875 0.5086 0.7821 0.067 Uiso 1 1 calc R . . C36 C 0.3424(3) 0.4130(2) 0.6012(2) 0.0644(15) Uani 1 1 d . . . H36A H 0.2930 0.4380 0.5857 0.097 Uiso 1 1 calc R . . H36B H 0.3213 0.3887 0.6344 0.097 Uiso 1 1 calc R . . H36C H 0.3634 0.3864 0.5697 0.097 Uiso 1 1 calc R . . C37 C 0.8693(3) 0.5842(2) 0.67407(18) 0.0375(11) Uani 1 1 d . . . H37A H 0.9090 0.5781 0.7095 0.045 Uiso 1 1 calc R . . H37B H 0.8886 0.6221 0.6552 0.045 Uiso 1 1 calc R . . C38 C 1.0187(3) 0.5274(3) 0.6038(2) 0.0737(18) Uani 1 1 d . . . H38A H 1.0379 0.4930 0.5800 0.111 Uiso 1 1 calc R . . H38B H 1.0533 0.5282 0.6413 0.111 Uiso 1 1 calc R . . H38C H 1.0292 0.5647 0.5818 0.111 Uiso 1 1 calc R . . C39 C 0.8293(3) 0.5262(2) 0.54573(19) 0.0557(14) Uani 1 1 d . . . H39A H 0.8379 0.5665 0.5291 0.084 Uiso 1 1 calc R . . H39B H 0.7651 0.5193 0.5519 0.084 Uiso 1 1 calc R . . H39C H 0.8520 0.4960 0.5181 0.084 Uiso 1 1 calc R . . C40 C 0.8734(4) 0.4439(2) 0.6565(2) 0.0655(16) Uani 1 1 d . . . H40A H 0.8123 0.4427 0.6719 0.098 Uiso 1 1 calc R . . H40B H 0.9171 0.4382 0.6892 0.098 Uiso 1 1 calc R . . H40C H 0.8804 0.4117 0.6272 0.098 Uiso 1 1 calc R . . C41 C 0.4355(3) 0.60073(19) 0.78063(19) 0.0356(10) Uani 1 1 d . . . C42 C 0.3857(3) 0.6077(2) 0.7261(2) 0.0392(11) Uani 1 1 d . . . C43 C 0.3100(3) 0.5705(2) 0.7149(2) 0.0513(13) Uani 1 1 d . . . H43 H 0.2768 0.5752 0.6787 0.062 Uiso 1 1 calc R . . C44 C 0.2820(3) 0.5266(2) 0.7558(3) 0.0533(13) Uani 1 1 d . . . C45 C 0.3302(3) 0.5214(2) 0.8103(2) 0.0534(13) Uani 1 1 d . . . H45 H 0.3106 0.4934 0.8391 0.064 Uiso 1 1 calc R . . C46 C 0.4078(3) 0.5574(2) 0.8229(2) 0.0418(11) Uani 1 1 d . . . C47 C 0.4616(3) 0.5467(2) 0.8815(2) 0.0533(13) Uani 1 1 d . . . H47A H 0.5262 0.5465 0.8736 0.080 Uiso 1 1 calc R . . H47B H 0.4443 0.5079 0.8985 0.080 Uiso 1 1 calc R . . H47C H 0.4484 0.5790 0.9097 0.080 Uiso 1 1 calc R . . C48 C 0.4136(3) 0.6546(2) 0.6804(2) 0.0488(12) Uani 1 1 d . . . H48A H 0.3825 0.6465 0.6424 0.073 Uiso 1 1 calc R . . H48B H 0.4788 0.6526 0.6751 0.073 Uiso 1 1 calc R . . H48C H 0.3973 0.6949 0.6943 0.073 Uiso 1 1 calc R . . C49 C 0.2001(4) 0.4844(3) 0.7415(3) 0.088(2) Uani 1 1 d . . . H49A H 0.1554 0.5062 0.7171 0.132 Uiso 1 1 calc R . . H49B H 0.1728 0.4717 0.7786 0.132 Uiso 1 1 calc R . . H49C H 0.2208 0.4490 0.7198 0.132 Uiso 1 1 calc R . . C50 C 0.5945(3) 0.75463(18) 0.88161(18) 0.0336(10) Uani 1 1 d . . . H50A H 0.6155 0.7910 0.8607 0.040 Uiso 1 1 calc R . . H50B H 0.6406 0.7452 0.9127 0.040 Uiso 1 1 calc R . . C51 C 0.3983(3) 0.8068(3) 0.8674(3) 0.0781(18) Uani 1 1 d . . . H51A H 0.3791 0.7749 0.8398 0.117 Uiso 1 1 calc R . . H51B H 0.4243 0.8401 0.8450 0.117 Uiso 1 1 calc R . . H51C H 0.3464 0.8213 0.8892 0.117 Uiso 1 1 calc R . . C52 C 0.4371(4) 0.7125(2) 0.9673(2) 0.0772(19) Uani 1 1 d . . . H52A H 0.3892 0.7284 0.9921 0.116 Uiso 1 1 calc R . . H52B H 0.4847 0.6951 0.9927 0.116 Uiso 1 1 calc R . . H52C H 0.4123 0.6815 0.9407 0.116 Uiso 1 1 calc R . . C53 C 0.5206(4) 0.8384(2) 0.9754(2) 0.0650(16) Uani 1 1 d . . . H53A H 0.5372 0.8744 0.9530 0.098 Uiso 1 1 calc R . . H53B H 0.5722 0.8250 0.9998 0.098 Uiso 1 1 calc R . . H53C H 0.4702 0.8479 1.0011 0.098 Uiso 1 1 calc R . . C54 C 0.7561(3) 0.54910(18) 0.88784(16) 0.0271(9) Uani 1 1 d . . . C55 C 0.7092(3) 0.55500(19) 0.94164(18) 0.0323(10) Uani 1 1 d . . . C56 C 0.7109(3) 0.5057(2) 0.98127(19) 0.0406(11) Uani 1 1 d . . . H56 H 0.6781 0.5085 1.0168 0.049 Uiso 1 1 calc R . . C57 C 0.7589(3) 0.4526(2) 0.97020(19) 0.0384(11) Uani 1 1 d . . . C58 C 0.8075(3) 0.44897(18) 0.91716(18) 0.0351(10) Uani 1 1 d . . . H58 H 0.8423 0.4141 0.9097 0.042 Uiso 1 1 calc R . . C59 C 0.8055(3) 0.49632(19) 0.87454(18) 0.0316(10) Uani 1 1 d . . . C60 C 0.8581(3) 0.4901(2) 0.81700(19) 0.0469(12) Uani 1 1 d . . . H60A H 0.8191 0.5012 0.7831 0.070 Uiso 1 1 calc R . . H60B H 0.8780 0.4483 0.8125 0.070 Uiso 1 1 calc R . . H60C H 0.9106 0.5167 0.8187 0.070 Uiso 1 1 calc R . . C61 C 0.6606(3) 0.6137(2) 0.95715(19) 0.0470(12) Uani 1 1 d . . . H61A H 0.7051 0.6451 0.9659 0.070 Uiso 1 1 calc R . . H61B H 0.6235 0.6072 0.9920 0.070 Uiso 1 1 calc R . . H61C H 0.6220 0.6261 0.9235 0.070 Uiso 1 1 calc R . . C62 C 0.7621(3) 0.3999(2) 1.0152(2) 0.0582(14) Uani 1 1 d . . . H62A H 0.7344 0.4126 1.0522 0.087 Uiso 1 1 calc R . . H62B H 0.8249 0.3884 1.0232 0.087 Uiso 1 1 calc R . . H62C H 0.7291 0.3655 0.9985 0.087 Uiso 1 1 calc R . . C63 C 0.6956(2) 0.72540(16) 0.08526(15) 0.091(2) Uani 1 1 d G . . H63 H 0.6861 0.7281 0.0435 0.109 Uiso 1 1 calc R . . C64 C 0.72403(15) 0.67027(14) 0.11131(14) 0.098(3) Uani 1 1 d G . . H64 H 0.7335 0.6361 0.0870 0.118 Uiso 1 1 calc R . . C65 C 0.7383(2) 0.66627(19) 0.17366(14) 0.128(3) Uani 1 1 d G . . H65 H 0.7573 0.6294 0.1911 0.154 Uiso 1 1 calc R . . C66 C 0.7241(2) 0.7174(2) 0.20996(15) 0.115(3) Uani 1 1 d G . . H66 H 0.7336 0.7147 0.2517 0.138 Uiso 1 1 calc R . . C67 C 0.69567(19) 0.77253(19) 0.18391(19) 0.107(3) Uani 1 1 d G . . H67 H 0.6862 0.8067 0.2082 0.129 Uiso 1 1 calc R . . C68 C 0.6814(2) 0.77653(16) 0.12156(19) 0.110(3) Uani 1 1 d G . . H68 H 0.6624 0.8134 0.1041 0.133 Uiso 1 1 calc R . . C69 C 0.9495(3) 0.50424(18) 0.0533(3) 0.126(3) Uani 1 1 d G . . H69 H 0.9160 0.5071 0.0886 0.151 Uiso 1 1 calc R . . C70 C 0.9453(2) 0.54849(18) 0.0091(2) 0.111(3) Uani 1 1 d G . . H70 H 0.9077 0.5825 0.0147 0.133 Uiso 1 1 calc R . . C71 C 0.9933(3) 0.5447(2) -0.0421(2) 0.115(3) Uani 1 1 d G . . H71 H 0.9878 0.5759 -0.0707 0.138 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 N8 0.0300(19) 0.032(2) 0.0256(18) 0.0007(15) 0.0001(15) 0.0023(16) Lu1 0.02394(9) 0.02288(9) 0.02322(9) -0.00087(8) -0.00038(6) 0.00209(8) P1 0.0238(5) 0.0274(6) 0.0262(5) 0.0040(4) -0.0015(4) -0.0004(4) Si1 0.0543(9) 0.0484(9) 0.0347(7) 0.0003(6) 0.0128(6) 0.0175(7) Si2 0.0431(8) 0.0355(8) 0.0538(8) -0.0102(6) 0.0194(6) 0.0000(6) N1 0.0282(18) 0.0280(19) 0.0272(18) 0.0039(15) -0.0033(14) -0.0018(15) N2 0.0304(18) 0.0208(17) 0.0254(17) 0.0067(14) -0.0021(14) 0.0023(14) N3 0.0319(19) 0.026(2) 0.0294(18) 0.0018(14) 0.0020(15) 0.0015(15) N4 0.0298(19) 0.0222(18) 0.0227(17) 0.0001(14) 0.0000(14) 0.0004(15) N5 0.0266(18) 0.0259(19) 0.0305(18) -0.0016(15) 0.0017(14) -0.0026(15) N6 0.0295(19) 0.0291(19) 0.0290(18) -0.0015(15) 0.0042(15) 0.0017(16) N7 0.030(2) 0.030(2) 0.040(2) -0.0091(16) 0.0049(16) -0.0004(15) N9 0.037(2) 0.031(2) 0.0264(18) -0.0016(15) 0.0004(15) 0.0036(16) N10 0.031(2) 0.031(2) 0.0342(19) -0.0082(16) 0.0011(16) 0.0015(16) C1 0.027(2) 0.023(2) 0.027(2) -0.0001(17) 0.0018(17) 0.0026(17) C2 0.030(2) 0.040(3) 0.038(2) 0.009(2) 0.0062(19) 0.006(2) C3 0.039(3) 0.055(3) 0.039(3) 0.013(2) 0.012(2) 0.000(2) C4 0.053(3) 0.037(3) 0.025(2) 0.005(2) 0.004(2) -0.006(2) C5 0.040(3) 0.026(2) 0.034(2) 0.0043(18) -0.0078(19) -0.0033(19) C6 0.030(2) 0.020(2) 0.028(2) -0.0010(17) -0.0005(17) -0.0009(17) C7 0.028(2) 0.025(2) 0.034(2) 0.0011(18) -0.0039(18) 0.0076(18) C8 0.035(2) 0.025(2) 0.039(3) 0.0068(19) -0.011(2) -0.0056(19) C9 0.057(3) 0.029(3) 0.037(3) 0.010(2) -0.008(2) -0.014(2) C10 0.102(5) 0.051(4) 0.035(3) 0.012(2) -0.019(3) -0.024(3) C11 0.090(5) 0.061(4) 0.060(4) 0.027(3) -0.039(4) -0.021(3) C12 0.051(3) 0.053(4) 0.087(4) 0.025(3) -0.034(3) -0.007(3) C13 0.037(3) 0.034(3) 0.053(3) 0.013(2) -0.013(2) -0.005(2) C14 0.077(4) 0.043(3) 0.034(3) 0.002(2) 0.018(2) -0.006(3) C15 0.029(3) 0.046(3) 0.088(4) 0.015(3) -0.002(3) 0.006(2) C16 0.031(2) 0.036(3) 0.028(2) 0.0082(19) -0.0008(18) 0.003(2) C17 0.040(3) 0.044(3) 0.063(3) 0.005(3) 0.000(2) 0.005(2) C18 0.042(3) 0.051(3) 0.094(4) 0.018(3) 0.006(3) 0.019(3) C19 0.032(3) 0.095(5) 0.055(3) 0.039(3) 0.002(2) 0.014(3) C20 0.030(3) 0.110(5) 0.042(3) 0.008(3) -0.010(2) -0.006(3) C21 0.034(3) 0.072(4) 0.038(3) -0.003(2) -0.003(2) 0.001(2) C22 0.024(2) 0.028(2) 0.031(2) -0.0011(18) -0.0048(17) -0.0034(17) C23 0.056(3) 0.037(3) 0.034(2) 0.002(2) 0.002(2) -0.012(2) C24 0.080(4) 0.032(3) 0.062(4) -0.011(3) 0.006(3) -0.009(3) C25 0.071(4) 0.050(3) 0.040(3) -0.015(2) 0.012(3) -0.012(3) C26 0.062(3) 0.055(3) 0.029(2) 0.002(2) 0.007(2) -0.009(3) C27 0.047(3) 0.038(3) 0.033(2) 0.002(2) 0.003(2) -0.001(2) C28 0.032(2) 0.027(2) 0.034(2) -0.0060(19) -0.0019(19) 0.0015(19) C29 0.045(3) 0.024(2) 0.033(2) -0.0060(19) 0.000(2) 0.008(2) C30 0.047(3) 0.026(2) 0.047(3) 0.000(2) 0.004(2) -0.001(2) C31 0.040(3) 0.034(3) 0.048(3) -0.005(2) -0.004(2) -0.005(2) C32 0.050(3) 0.044(3) 0.038(3) -0.005(2) -0.015(2) -0.001(2) C33 0.045(3) 0.031(3) 0.035(2) -0.003(2) -0.002(2) -0.005(2) C34 0.058(3) 0.051(3) 0.035(3) 0.002(2) -0.010(2) -0.017(3) C35 0.056(3) 0.033(3) 0.045(3) 0.002(2) -0.008(2) 0.003(2) C36 0.062(4) 0.057(4) 0.074(4) -0.006(3) -0.012(3) -0.020(3) C37 0.034(2) 0.046(3) 0.032(2) 0.001(2) 0.0018(19) 0.003(2) C38 0.061(4) 0.102(5) 0.058(4) 0.007(3) 0.020(3) 0.034(3) C39 0.072(4) 0.061(4) 0.035(3) -0.002(2) 0.014(2) 0.005(3) C40 0.102(5) 0.050(3) 0.045(3) -0.001(3) 0.014(3) 0.023(3) C41 0.032(2) 0.028(2) 0.046(3) -0.009(2) 0.007(2) -0.0006(19) C42 0.040(3) 0.030(3) 0.049(3) -0.007(2) 0.000(2) 0.006(2) C43 0.037(3) 0.045(3) 0.072(4) -0.009(3) -0.015(2) 0.003(2) C44 0.038(3) 0.045(3) 0.077(4) -0.011(3) -0.003(3) -0.008(2) C45 0.047(3) 0.050(3) 0.063(3) -0.004(3) 0.010(3) -0.017(3) C46 0.040(3) 0.040(3) 0.046(3) -0.009(2) 0.009(2) -0.004(2) C47 0.061(3) 0.050(3) 0.050(3) -0.007(3) 0.012(3) -0.018(3) C48 0.043(3) 0.043(3) 0.060(3) 0.001(3) -0.013(2) 0.007(2) C49 0.062(4) 0.072(4) 0.129(6) 0.004(4) -0.027(4) -0.029(3) C50 0.039(3) 0.030(2) 0.032(2) -0.0045(19) 0.0073(19) -0.0022(19) C51 0.049(3) 0.088(5) 0.098(5) -0.020(4) 0.005(3) 0.020(3) C52 0.093(4) 0.055(4) 0.086(4) -0.011(3) 0.060(4) -0.012(3) C53 0.089(4) 0.040(3) 0.068(4) -0.018(3) 0.029(3) -0.001(3) C54 0.033(2) 0.023(2) 0.025(2) 0.0052(17) -0.0073(17) -0.0062(18) C55 0.037(2) 0.029(2) 0.031(2) 0.0029(18) -0.0033(19) -0.0006(19) C56 0.037(3) 0.051(3) 0.034(2) 0.009(2) 0.003(2) -0.005(2) C57 0.039(3) 0.037(3) 0.039(3) 0.015(2) -0.009(2) -0.012(2) C58 0.041(3) 0.019(2) 0.045(3) 0.0013(19) -0.014(2) -0.0058(19) C59 0.033(2) 0.032(2) 0.029(2) -0.0002(19) -0.0073(18) -0.0046(19) C60 0.060(3) 0.041(3) 0.040(3) 0.001(2) 0.005(2) 0.013(2) C61 0.060(3) 0.051(3) 0.030(2) 0.002(2) 0.011(2) 0.007(3) C62 0.061(3) 0.054(3) 0.059(3) 0.029(3) -0.004(3) -0.008(3) C63 0.087(5) 0.115(6) 0.072(4) -0.033(4) 0.033(4) -0.037(4) C64 0.054(4) 0.145(7) 0.094(5) -0.051(5) -0.007(4) 0.010(4) C65 0.080(5) 0.179(9) 0.124(7) -0.025(6) -0.041(5) 0.029(5) C66 0.047(4) 0.219(11) 0.080(5) -0.040(6) -0.009(4) -0.027(6) C67 0.076(5) 0.162(8) 0.086(5) -0.070(5) 0.037(4) -0.065(5) C68 0.131(6) 0.110(6) 0.092(5) -0.027(5) 0.037(5) -0.065(5) C69 0.095(6) 0.142(9) 0.138(7) -0.036(6) -0.044(5) -0.043(6) C70 0.099(6) 0.074(5) 0.157(8) -0.023(6) -0.055(6) -0.021(4) C71 0.113(7) 0.116(7) 0.113(6) 0.023(6) -0.065(5) -0.061(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N8 N9 1.302(4) . ? N8 C37 1.461(5) . ? N8 Lu1 2.411(3) . ? Lu1 N1 2.173(3) . ? Lu1 N10 2.357(3) . ? Lu1 N7 2.359(3) . ? Lu1 N2 2.424(3) . ? Lu1 N5 2.439(3) . ? Lu1 N4 2.544(3) . ? P1 N2 1.636(3) . ? P1 C22 1.798(4) . ? P1 C1 1.801(4) . ? P1 C16 1.805(4) . ? Si1 C39 1.866(5) . ? Si1 C38 1.871(5) . ? Si1 C40 1.875(5) . ? Si1 C37 1.879(4) . ? Si2 C51 1.850(5) . ? Si2 C52 1.863(5) . ? Si2 C53 1.869(5) . ? Si2 C50 1.887(4) . ? N1 C8 1.430(5) . ? N1 C7 1.473(5) . ? N2 N3 1.371(4) . ? N3 N4 1.266(4) . ? N4 C54 1.452(4) . ? N5 N6 1.294(4) . ? N5 C50 1.463(5) . ? N6 N7 1.327(4) . ? N7 C41 1.427(5) . ? N9 N10 1.322(4) . ? N10 C28 1.436(5) . ? C1 C2 1.386(5) . ? C1 C6 1.402(5) . ? C2 C3 1.390(5) . ? C3 C4 1.370(6) . ? C4 C5 1.374(6) . ? C5 C6 1.394(5) . ? C6 C7 1.513(5) . ? C8 C9 1.402(6) . ? C8 C13 1.412(6) . ? C9 C10 1.390(6) . ? C9 C14 1.511(6) . ? C10 C11 1.371(8) . ? C11 C12 1.370(7) . ? C12 C13 1.397(6) . ? C13 C15 1.497(6) . ? C16 C17 1.369(6) . ? C16 C21 1.380(6) . ? C17 C18 1.385(6) . ? C18 C19 1.359(7) . ? C19 C20 1.362(7) . ? C20 C21 1.382(6) . ? C22 C23 1.380(5) . ? C22 C27 1.400(5) . ? C23 C24 1.386(6) . ? C24 C25 1.362(6) . ? C25 C26 1.370(6) . ? C26 C27 1.370(6) . ? C28 C29 1.388(5) . ? C28 C33 1.403(5) . ? C29 C30 1.389(6) . ? C29 C35 1.509(5) . ? C30 C31 1.391(6) . ? C31 C32 1.382(6) . ? C31 C36 1.506(6) . ? C32 C33 1.406(6) . ? C33 C34 1.508(6) . ? C41 C46 1.393(6) . ? C41 C42 1.398(6) . ? C42 C43 1.386(6) . ? C42 C48 1.500(6) . ? C43 C44 1.382(7) . ? C44 C45 1.384(7) . ? C44 C49 1.532(6) . ? C45 C46 1.399(6) . ? C46 C47 1.515(6) . ? C54 C55 1.390(5) . ? C54 C59 1.391(5) . ? C55 C56 1.385(5) . ? C55 C61 1.504(6) . ? C56 C57 1.375(6) . ? C57 C58 1.384(6) . ? C57 C62 1.518(6) . ? C58 C59 1.396(5) . ? C59 C60 1.504(5) . ? C63 C64 1.3900 . ? C63 C68 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C66 C67 1.3900 . ? C67 C68 1.3900 . ? C69 C70 1.3727 . ? C69 C71 1.378(6) 3_765 ? C70 C71 1.3447 . ? C71 C69 1.378(7) 3_765 ? 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 N9 N8 C37 111.9(3) . . ? N9 N8 Lu1 97.8(2) . . ? C37 N8 Lu1 150.1(3) . . ? N1 Lu1 N10 108.86(12) . . ? N1 Lu1 N7 106.86(11) . . ? N10 Lu1 N7 84.22(11) . . ? N1 Lu1 N8 100.38(11) . . ? N10 Lu1 N8 53.24(11) . . ? N7 Lu1 N8 135.25(11) . . ? N1 Lu1 N2 89.57(11) . . ? N10 Lu1 N2 132.55(11) . . ? N7 Lu1 N2 132.79(11) . . ? N8 Lu1 N2 81.11(11) . . ? N1 Lu1 N5 87.50(11) . . ? N10 Lu1 N5 137.32(11) . . ? N7 Lu1 N5 53.12(11) . . ? N8 Lu1 N5 163.83(10) . . ? N2 Lu1 N5 84.88(10) . . ? N1 Lu1 N4 139.99(11) . . ? N10 Lu1 N4 105.22(10) . . ? N7 Lu1 N4 96.72(11) . . ? N8 Lu1 N4 83.63(10) . . ? N2 Lu1 N4 51.39(10) . . ? N5 Lu1 N4 81.32(10) . . ? N2 P1 C22 113.76(17) . . ? N2 P1 C1 107.15(16) . . ? C22 P1 C1 109.88(18) . . ? N2 P1 C16 112.22(18) . . ? C22 P1 C16 105.57(18) . . ? C1 P1 C16 108.15(18) . . ? C39 Si1 C38 107.5(2) . . ? C39 Si1 C40 111.3(2) . . ? C38 Si1 C40 108.6(3) . . ? C39 Si1 C37 114.1(2) . . ? C38 Si1 C37 104.7(2) . . ? C40 Si1 C37 110.2(2) . . ? C51 Si2 C52 110.8(3) . . ? C51 Si2 C53 108.6(3) . . ? C52 Si2 C53 107.1(2) . . ? C51 Si2 C50 111.1(2) . . ? C52 Si2 C50 113.8(2) . . ? C53 Si2 C50 105.0(2) . . ? C8 N1 C7 112.2(3) . . ? C8 N1 Lu1 132.7(2) . . ? C7 N1 Lu1 114.7(2) . . ? N3 N2 P1 114.3(2) . . ? N3 N2 Lu1 100.7(2) . . ? P1 N2 Lu1 143.93(17) . . ? N4 N3 N2 109.7(3) . . ? N3 N4 C54 113.0(3) . . ? N3 N4 Lu1 98.1(2) . . ? C54 N4 Lu1 148.9(2) . . ? N6 N5 C50 113.4(3) . . ? N6 N5 Lu1 96.9(2) . . ? C50 N5 Lu1 148.7(2) . . ? N5 N6 N7 110.0(3) . . ? N6 N7 C41 114.1(3) . . ? N6 N7 Lu1 99.7(2) . . ? C41 N7 Lu1 146.1(3) . . ? N8 N9 N10 109.1(3) . . ? N9 N10 C28 112.7(3) . . ? N9 N10 Lu1 99.8(2) . . ? C28 N10 Lu1 146.8(3) . . ? C2 C1 C6 120.0(3) . . ? C2 C1 P1 118.1(3) . . ? C6 C1 P1 121.8(3) . . ? C1 C2 C3 120.9(4) . . ? C4 C3 C2 119.1(4) . . ? C3 C4 C5 120.5(4) . . ? C4 C5 C6 121.7(4) . . ? C5 C6 C1 117.7(4) . . ? C5 C6 C7 118.6(3) . . ? C1 C6 C7 123.6(3) . . ? N1 C7 C6 110.7(3) . . ? C9 C8 C13 119.3(4) . . ? C9 C8 N1 120.7(4) . . ? C13 C8 N1 119.9(4) . . ? C10 C9 C8 119.5(5) . . ? C10 C9 C14 118.5(5) . . ? C8 C9 C14 121.9(4) . . ? C11 C10 C9 121.2(5) . . ? C12 C11 C10 119.7(5) . . ? C11 C12 C13 121.5(5) . . ? C12 C13 C8 118.7(5) . . ? C12 C13 C15 119.8(5) . . ? C8 C13 C15 121.5(4) . . ? C17 C16 C21 118.8(4) . . ? C17 C16 P1 120.3(3) . . ? C21 C16 P1 120.8(3) . . ? C16 C17 C18 120.7(5) . . ? C19 C18 C17 120.1(5) . . ? C18 C19 C20 119.7(5) . . ? C19 C20 C21 120.7(5) . . ? C16 C21 C20 119.9(5) . . ? C23 C22 C27 119.2(4) . . ? C23 C22 P1 122.1(3) . . ? C27 C22 P1 118.5(3) . . ? C22 C23 C24 119.8(4) . . ? C25 C24 C23 120.3(5) . . ? C24 C25 C26 120.5(4) . . ? C27 C26 C25 120.3(4) . . ? C26 C27 C22 119.9(4) . . ? C29 C28 C33 120.5(4) . . ? C29 C28 N10 119.2(4) . . ? C33 C28 N10 120.3(4) . . ? C28 C29 C30 119.4(4) . . ? C28 C29 C35 120.6(4) . . ? C30 C29 C35 120.0(4) . . ? C29 C30 C31 122.1(4) . . ? C32 C31 C30 117.4(4) . . ? C32 C31 C36 120.9(4) . . ? C30 C31 C36 121.7(4) . . ? C31 C32 C33 122.7(4) . . ? C28 C33 C32 117.8(4) . . ? C28 C33 C34 121.8(4) . . ? C32 C33 C34 120.3(4) . . ? N8 C37 Si1 120.1(3) . . ? C46 C41 C42 119.8(4) . . ? C46 C41 N7 121.4(4) . . ? C42 C41 N7 118.6(4) . . ? C43 C42 C41 119.1(4) . . ? C43 C42 C48 120.3(4) . . ? C41 C42 C48 120.7(4) . . ? C44 C43 C42 122.1(5) . . ? C43 C44 C45 118.3(4) . . ? C43 C44 C49 121.3(5) . . ? C45 C44 C49 120.4(5) . . ? C44 C45 C46 121.2(5) . . ? C41 C46 C45 119.5(4) . . ? C41 C46 C47 121.6(4) . . ? C45 C46 C47 118.9(4) . . ? N5 C50 Si2 120.2(3) . . ? C55 C54 C59 121.6(4) . . ? C55 C54 N4 119.3(3) . . ? C59 C54 N4 119.1(3) . . ? C56 C55 C54 117.8(4) . . ? C56 C55 C61 121.1(4) . . ? C54 C55 C61 121.1(4) . . ? C57 C56 C55 122.7(4) . . ? C56 C57 C58 118.1(4) . . ? C56 C57 C62 121.8(4) . . ? C58 C57 C62 120.1(4) . . ? C57 C58 C59 121.7(4) . . ? C54 C59 C58 118.1(4) . . ? C54 C59 C60 121.9(4) . . ? C58 C59 C60 120.0(4) . . ? C64 C63 C68 120.0 . . ? C63 C64 C65 120.0 . . ? C64 C65 C66 120.0 . . ? C67 C66 C65 120.0 . . ? C66 C67 C68 120.0 . . ? C67 C68 C63 120.0 . . ? C70 C69 C71 115.6(6) . 3_765 ? C71 C70 C69 122.6 . . ? C70 C71 C69 121.8(6) . 3_765 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.153 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.092 #===========END============= data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 670210' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H72 Lu N6 P' _chemical_formula_weight 1083.18 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' P P 0.1023 0.0942 '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 13.2430(19) _cell_length_b 13.321(2) _cell_length_c 19.106(3) _cell_angle_alpha 71.435(3) _cell_angle_beta 84.227(3) _cell_angle_gamma 83.052(3) _cell_volume 3164.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.622 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6769 _exptl_absorpt_correction_T_max 0.8329 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(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 17730 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.2415 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 26.02 _reflns_number_total 12117 _reflns_number_gt 6317 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^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 12117 _refine_ls_number_parameters 626 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1808 _refine_ls_R_factor_gt 0.0906 _refine_ls_wR_factor_ref 0.2072 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.044 _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 C1 C 0.7297(9) -0.1074(9) 0.1590(7) 0.038(3) Uani 1 1 d . . . C2 C 0.6739(9) -0.0110(9) 0.1188(7) 0.038(3) Uani 1 1 d . . . C3 C 0.5762(9) -0.0134(10) 0.0977(7) 0.046(3) Uani 1 1 d . . . H3 H 0.5390 0.0511 0.0717 0.055 Uiso 1 1 calc R . . C4 C 0.5342(9) -0.1066(11) 0.1139(7) 0.040(3) Uani 1 1 d . . . H4 H 0.4678 -0.1067 0.0992 0.048 Uiso 1 1 calc R . . C5 C 0.5863(9) -0.2010(11) 0.1515(7) 0.046(3) Uani 1 1 d . . . H5 H 0.5560 -0.2657 0.1617 0.055 Uiso 1 1 calc R . . C6 C 0.6828(8) -0.2029(9) 0.1748(6) 0.034(3) Uani 1 1 d . . . C7 C 0.7413(10) -0.3079(9) 0.2132(8) 0.049(4) Uani 1 1 d . . . H7 H 0.7895 -0.2936 0.2451 0.058 Uiso 1 1 calc R . . C8 C 0.6721(12) -0.3921(12) 0.2641(10) 0.089(6) Uani 1 1 d . . . H8A H 0.6292 -0.4141 0.2338 0.133 Uiso 1 1 calc R . . H8B H 0.6288 -0.3612 0.2982 0.133 Uiso 1 1 calc R . . H8C H 0.7148 -0.4541 0.2926 0.133 Uiso 1 1 calc R . . C9 C 0.8042(12) -0.3511(13) 0.1573(10) 0.093(6) Uani 1 1 d . . . H9A H 0.7591 -0.3653 0.1246 0.140 Uiso 1 1 calc R . . H9B H 0.8441 -0.4172 0.1830 0.140 Uiso 1 1 calc R . . H9C H 0.8505 -0.2988 0.1279 0.140 Uiso 1 1 calc R . . C10 C 0.7225(9) 0.0943(9) 0.0938(8) 0.045(3) Uani 1 1 d . . . H10 H 0.7831 0.0842 0.1234 0.053 Uiso 1 1 calc R . . C11 C 0.7594(15) 0.1176(15) 0.0173(11) 0.111(7) Uani 1 1 d . . . H11A H 0.7148 0.0904 -0.0090 0.167 Uiso 1 1 calc R . . H11B H 0.8288 0.0835 0.0141 0.167 Uiso 1 1 calc R . . H11C H 0.7597 0.1947 -0.0054 0.167 Uiso 1 1 calc R . . C12 C 0.6539(12) 0.1856(12) 0.1068(13) 0.116(8) Uani 1 1 d . . . H12A H 0.6900 0.2500 0.0899 0.173 Uiso 1 1 calc R . . H12B H 0.6341 0.1695 0.1597 0.173 Uiso 1 1 calc R . . H12C H 0.5928 0.1970 0.0792 0.173 Uiso 1 1 calc R . . C13 C 0.7446(9) 0.0846(9) 0.3623(7) 0.036(3) Uani 1 1 d . . . C14 C 0.7509(9) 0.1549(9) 0.4054(7) 0.041(3) Uani 1 1 d . . . C15 C 0.6664(10) 0.1787(10) 0.4490(8) 0.050(4) Uani 1 1 d . . . H15 H 0.6723 0.2222 0.4790 0.060 Uiso 1 1 calc R . . C16 C 0.5739(11) 0.1400(12) 0.4491(8) 0.062(4) Uani 1 1 d . . . H16 H 0.5156 0.1576 0.4777 0.074 Uiso 1 1 calc R . . C17 C 0.5697(10) 0.0750(12) 0.4064(8) 0.060(4) Uani 1 1 d . . . H17 H 0.5062 0.0480 0.4073 0.072 Uiso 1 1 calc R . . C18 C 0.6507(9) 0.0449(10) 0.3614(8) 0.048(3) Uani 1 1 d . . . C19 C 0.6430(9) -0.0296(11) 0.3183(8) 0.053(4) Uani 1 1 d . . . H19 H 0.6872 -0.0058 0.2716 0.064 Uiso 1 1 calc R . . C20 C 0.5361(9) -0.0329(14) 0.2966(9) 0.076(5) Uani 1 1 d . . . H20A H 0.4956 -0.0733 0.3399 0.115 Uiso 1 1 calc R . . H20B H 0.5404 -0.0673 0.2579 0.115 Uiso 1 1 calc R . . H20C H 0.5036 0.0398 0.2779 0.115 Uiso 1 1 calc R . . C21 C 0.6858(11) -0.1430(11) 0.3616(9) 0.066(4) Uani 1 1 d . . . H21A H 0.7598 -0.1451 0.3633 0.098 Uiso 1 1 calc R . . H21B H 0.6708 -0.1931 0.3368 0.098 Uiso 1 1 calc R . . H21C H 0.6541 -0.1628 0.4121 0.098 Uiso 1 1 calc R . . C22 C 0.8522(10) 0.1948(10) 0.4080(7) 0.048(3) Uani 1 1 d . . . H22 H 0.8856 0.2111 0.3569 0.058 Uiso 1 1 calc R . . C23 C 0.8454(13) 0.2965(11) 0.4291(9) 0.079(5) Uani 1 1 d . . . H23A H 0.8028 0.3525 0.3950 0.119 Uiso 1 1 calc R . . H23B H 0.9139 0.3190 0.4260 0.119 Uiso 1 1 calc R . . H23C H 0.8151 0.2835 0.4797 0.119 Uiso 1 1 calc R . . C24 C 0.9228(10) 0.1078(11) 0.4584(7) 0.058(4) Uani 1 1 d . . . H24A H 0.8948 0.0919 0.5098 0.087 Uiso 1 1 calc R . . H24B H 0.9906 0.1326 0.4541 0.087 Uiso 1 1 calc R . . H24C H 0.9283 0.0434 0.4434 0.087 Uiso 1 1 calc R . . C25 C 1.1932(8) 0.1009(9) 0.3218(7) 0.037(3) Uani 1 1 d . . . C26 C 1.1469(9) 0.2030(10) 0.3171(8) 0.050(4) Uani 1 1 d . . . H26 H 1.1045 0.2394 0.2778 0.060 Uiso 1 1 calc R . . C27 C 1.1618(12) 0.2512(12) 0.3683(9) 0.065(4) Uani 1 1 d . . . H27 H 1.1318 0.3213 0.3638 0.079 Uiso 1 1 calc R . . C28 C 1.2225(11) 0.1952(13) 0.4278(8) 0.061(4) Uani 1 1 d . . . H28 H 1.2341 0.2289 0.4628 0.073 Uiso 1 1 calc R . . C29 C 1.2645(10) 0.0949(11) 0.4360(8) 0.053(4) Uani 1 1 d . . . H29 H 1.3027 0.0569 0.4775 0.063 Uiso 1 1 calc R . . C30 C 1.2508(10) 0.0495(10) 0.3833(8) 0.047(3) Uani 1 1 d . . . H30 H 1.2818 -0.0204 0.3884 0.056 Uiso 1 1 calc R . . C31 C 1.2595(8) 0.1062(9) 0.1732(7) 0.035(3) Uani 1 1 d . . . C32 C 1.3156(8) 0.1899(9) 0.1724(8) 0.046(3) Uani 1 1 d . . . H32 H 1.3166 0.2096 0.2160 0.055 Uiso 1 1 calc R . . C33 C 1.3694(10) 0.2433(11) 0.1081(8) 0.057(4) Uani 1 1 d . . . H33 H 1.4077 0.2995 0.1074 0.068 Uiso 1 1 calc R . . C34 C 1.3674(9) 0.2152(10) 0.0455(8) 0.051(4) Uani 1 1 d . . . H34 H 1.4021 0.2538 0.0008 0.061 Uiso 1 1 calc R . . C35 C 1.3146(9) 0.1298(10) 0.0467(7) 0.047(3) Uani 1 1 d . . . H35 H 1.3165 0.1083 0.0037 0.056 Uiso 1 1 calc R . . C36 C 1.2609(8) 0.0779(9) 0.1089(7) 0.038(3) Uani 1 1 d . . . H36 H 1.2236 0.0214 0.1088 0.046 Uiso 1 1 calc R . . C37 C 1.2267(8) -0.0977(9) 0.2863(6) 0.032(3) Uani 1 1 d . . . C38 C 1.3250(8) -0.1260(9) 0.2626(7) 0.036(3) Uani 1 1 d . . . H38 H 1.3629 -0.0742 0.2272 0.044 Uiso 1 1 calc R . . C39 C 1.3681(10) -0.2290(11) 0.2901(8) 0.056(4) Uani 1 1 d . . . H39 H 1.4358 -0.2485 0.2742 0.067 Uiso 1 1 calc R . . C40 C 1.3114(11) -0.3042(11) 0.3415(8) 0.058(4) Uani 1 1 d . . . H40 H 1.3398 -0.3758 0.3603 0.069 Uiso 1 1 calc R . . C41 C 1.2117(9) -0.2738(10) 0.3656(7) 0.044(3) Uani 1 1 d . . . H41 H 1.1741 -0.3246 0.4020 0.053 Uiso 1 1 calc R . . C42 C 1.1684(8) -0.1721(9) 0.3372(6) 0.029(3) Uani 1 1 d . . . C43 C 1.0560(8) -0.1518(9) 0.3600(7) 0.038(3) Uani 1 1 d . . . H43A H 1.0404 -0.2017 0.4097 0.046 Uiso 1 1 calc R . . H43B H 1.0429 -0.0786 0.3633 0.046 Uiso 1 1 calc R . . C44 C 0.9980(10) -0.2700(10) 0.3058(9) 0.054(3) Uani 1 1 d U . . C45 C 1.0417(10) -0.2950(10) 0.2445(9) 0.056(3) Uani 1 1 d U . . C46 C 1.0476(14) -0.4012(12) 0.2430(10) 0.087(5) Uani 1 1 d U . . H46 H 1.0809 -0.4209 0.2023 0.104 Uiso 1 1 calc R . . C47 C 1.0019(17) -0.4771(13) 0.3044(13) 0.113(6) Uani 1 1 d U . . H47 H 1.0059 -0.5488 0.3045 0.136 Uiso 1 1 calc R . . C48 C 0.9521(16) -0.4508(13) 0.3639(12) 0.101(5) Uani 1 1 d U . . H48 H 0.9162 -0.5017 0.4016 0.121 Uiso 1 1 calc R . . C49 C 0.9548(13) -0.3512(11) 0.3679(11) 0.074(4) Uani 1 1 d U . . C50 C 0.9050(13) -0.3296(14) 0.4351(10) 0.096(6) Uani 1 1 d . . . H50A H 0.8432 -0.3670 0.4504 0.145 Uiso 1 1 calc R . . H50B H 0.8868 -0.2529 0.4244 0.145 Uiso 1 1 calc R . . H50C H 0.9519 -0.3545 0.4749 0.145 Uiso 1 1 calc R . . C51 C 1.0911(11) -0.2118(13) 0.1804(8) 0.072(5) Uani 1 1 d . . . H51A H 1.0391 -0.1552 0.1576 0.108 Uiso 1 1 calc R . . H51B H 1.1232 -0.2449 0.1437 0.108 Uiso 1 1 calc R . . H51C H 1.1430 -0.1817 0.1987 0.108 Uiso 1 1 calc R . . C52 C 0.9253(8) 0.2529(9) 0.0993(8) 0.040(3) Uani 1 1 d . . . C53 C 0.8616(10) 0.3356(9) 0.1167(8) 0.044(3) Uani 1 1 d . . . C54 C 0.8442(11) 0.4292(11) 0.0600(9) 0.062(4) Uani 1 1 d . . . H54 H 0.8044 0.4873 0.0710 0.075 Uiso 1 1 calc R . . C55 C 0.8822(10) 0.4422(10) -0.0121(9) 0.051(4) Uani 1 1 d . . . C56 C 0.9427(9) 0.3601(12) -0.0261(8) 0.056(4) Uani 1 1 d . . . H56 H 0.9715 0.3702 -0.0752 0.067 Uiso 1 1 calc R . . C57 C 0.9656(10) 0.2616(11) 0.0267(8) 0.049(3) Uani 1 1 d . . . C58 C 1.0276(10) 0.1720(11) 0.0079(8) 0.066(4) Uani 1 1 d . . . H58A H 1.0983 0.1698 0.0199 0.099 Uiso 1 1 calc R . . H58B H 1.0258 0.1822 -0.0451 0.099 Uiso 1 1 calc R . . H58C H 0.9998 0.1050 0.0365 0.099 Uiso 1 1 calc R . . C59 C 0.8225(13) 0.3224(12) 0.1944(9) 0.087(6) Uani 1 1 d . . . H59A H 0.8707 0.3474 0.2194 0.130 Uiso 1 1 calc R . . H59B H 0.8147 0.2470 0.2202 0.130 Uiso 1 1 calc R . . H59C H 0.7562 0.3639 0.1949 0.130 Uiso 1 1 calc R . . C60 C 0.8652(11) 0.5475(10) -0.0747(8) 0.071(5) Uani 1 1 d . . . H60A H 0.9310 0.5752 -0.0941 0.107 Uiso 1 1 calc R . . H60B H 0.8219 0.5991 -0.0554 0.107 Uiso 1 1 calc R . . H60C H 0.8318 0.5353 -0.1144 0.107 Uiso 1 1 calc R . . Lu Lu 0.90234(4) -0.02277(4) 0.24347(3) 0.03048(18) Uani 1 1 d . . . N1 N 0.9502(7) 0.1553(7) 0.1571(5) 0.033(2) Uani 1 1 d . . . N2 N 1.0398(7) 0.1505(7) 0.1757(5) 0.033(2) Uani 1 1 d . . . N3 N 1.0622(6) 0.0533(7) 0.2276(5) 0.034(2) Uani 1 1 d . . . N4 N 0.8257(6) -0.1008(7) 0.1825(5) 0.037(2) Uani 1 1 d . . . H4A H 0.8711 -0.1441 0.1668 0.045 Uiso 1 1 calc R . . N5 N 0.8298(6) 0.0537(8) 0.3209(5) 0.042(3) Uani 1 1 d . . . H5A H 0.8804 0.0799 0.3338 0.051 Uiso 1 1 calc R . . N6 N 0.9887(7) -0.1644(7) 0.3086(5) 0.037(2) Uani 1 1 d . . . P1 P 1.1813(2) 0.0414(2) 0.25262(17) 0.0316(7) Uani 1 1 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 C1 0.047(7) 0.039(7) 0.032(7) -0.014(6) -0.007(6) -0.003(6) C2 0.035(7) 0.046(7) 0.038(8) -0.017(6) -0.005(6) -0.006(6) C3 0.039(7) 0.045(8) 0.054(9) -0.015(7) -0.008(7) -0.002(6) C4 0.023(6) 0.064(9) 0.036(8) -0.023(7) 0.002(6) -0.004(6) C5 0.044(8) 0.060(9) 0.044(8) -0.026(7) -0.006(7) -0.017(7) C6 0.037(7) 0.037(7) 0.025(7) -0.004(6) 0.001(6) -0.013(5) C7 0.052(8) 0.033(7) 0.069(10) -0.020(7) -0.037(8) 0.000(6) C8 0.086(12) 0.054(10) 0.104(15) 0.012(10) -0.021(11) -0.007(8) C9 0.083(12) 0.092(13) 0.108(15) -0.046(12) -0.028(11) 0.034(10) C10 0.037(7) 0.038(7) 0.057(10) -0.009(7) -0.013(7) -0.002(6) C11 0.147(18) 0.113(15) 0.096(15) -0.046(13) 0.023(14) -0.088(13) C12 0.076(12) 0.063(11) 0.22(3) -0.062(14) 0.019(14) -0.019(9) C13 0.039(7) 0.037(7) 0.033(7) -0.012(6) -0.004(6) -0.003(5) C14 0.048(8) 0.030(7) 0.047(8) -0.012(6) -0.010(7) -0.006(6) C15 0.055(9) 0.052(8) 0.053(9) -0.036(8) 0.008(8) -0.001(7) C16 0.055(9) 0.080(11) 0.058(10) -0.036(9) 0.004(8) -0.004(8) C17 0.027(7) 0.086(11) 0.070(11) -0.028(10) -0.004(8) -0.008(7) C18 0.033(7) 0.056(8) 0.057(9) -0.016(7) -0.017(7) -0.005(6) C19 0.035(7) 0.084(11) 0.058(10) -0.040(9) 0.001(7) -0.021(7) C20 0.034(8) 0.143(15) 0.075(11) -0.061(11) 0.007(8) -0.033(9) C21 0.074(10) 0.063(10) 0.072(11) -0.038(9) 0.006(9) -0.014(8) C22 0.063(9) 0.059(9) 0.030(7) -0.017(7) -0.009(7) -0.022(7) C23 0.111(13) 0.060(10) 0.079(12) -0.029(9) 0.002(10) -0.037(9) C24 0.057(9) 0.080(10) 0.037(8) -0.007(8) -0.014(7) -0.028(8) C25 0.029(6) 0.040(7) 0.043(8) -0.017(6) 0.008(6) -0.001(5) C26 0.042(8) 0.061(9) 0.057(9) -0.034(8) -0.006(7) 0.002(7) C27 0.082(11) 0.058(9) 0.071(11) -0.041(9) 0.006(10) -0.012(8) C28 0.063(10) 0.093(12) 0.045(9) -0.038(9) 0.002(8) -0.033(9) C29 0.051(9) 0.055(9) 0.052(10) -0.014(8) -0.014(7) -0.004(7) C30 0.052(8) 0.034(7) 0.050(9) -0.007(7) -0.005(7) -0.009(6) C31 0.026(6) 0.034(7) 0.047(8) -0.017(6) 0.001(6) 0.004(5) C32 0.037(7) 0.042(7) 0.063(10) -0.022(7) 0.001(7) -0.006(6) C33 0.044(8) 0.060(9) 0.053(10) 0.003(8) 0.006(8) -0.019(7) C34 0.027(7) 0.057(9) 0.049(9) 0.008(8) 0.004(7) -0.003(6) C35 0.038(7) 0.063(9) 0.035(8) -0.011(7) 0.002(6) -0.001(7) C36 0.027(6) 0.040(7) 0.050(9) -0.019(7) -0.002(6) 0.000(5) C37 0.031(6) 0.038(7) 0.030(7) -0.014(6) -0.005(6) -0.007(5) C38 0.020(6) 0.042(7) 0.049(8) -0.018(6) -0.003(6) 0.003(5) C39 0.042(8) 0.058(9) 0.065(10) -0.021(8) 0.002(8) 0.006(7) C40 0.064(10) 0.053(9) 0.059(10) -0.021(8) -0.020(8) 0.004(8) C41 0.040(7) 0.043(8) 0.051(9) -0.015(7) -0.006(7) -0.001(6) C42 0.033(6) 0.032(6) 0.025(7) -0.013(6) -0.010(5) 0.005(5) C43 0.042(7) 0.031(7) 0.038(8) -0.002(6) -0.010(6) -0.005(5) C44 0.055(8) 0.037(7) 0.077(9) -0.023(6) -0.026(7) 0.004(6) C45 0.049(8) 0.044(6) 0.085(9) -0.034(7) -0.040(7) 0.017(6) C46 0.142(13) 0.056(8) 0.085(10) -0.046(8) -0.080(9) 0.025(8) C47 0.179(18) 0.036(8) 0.126(15) -0.017(8) -0.079(12) 0.017(9) C48 0.155(16) 0.042(8) 0.106(12) -0.004(8) -0.068(10) -0.017(9) C49 0.096(11) 0.037(7) 0.087(10) -0.003(7) -0.048(8) -0.006(7) C50 0.101(14) 0.110(15) 0.072(13) -0.002(12) -0.005(11) -0.057(11) C51 0.061(10) 0.113(13) 0.065(11) -0.062(11) -0.001(9) -0.005(9) C52 0.026(6) 0.041(7) 0.057(9) -0.017(7) -0.009(6) -0.008(5) C53 0.066(9) 0.020(6) 0.045(9) -0.010(6) -0.004(7) -0.001(6) C54 0.073(10) 0.046(9) 0.083(12) -0.045(9) 0.006(9) -0.001(7) C55 0.053(9) 0.036(8) 0.064(11) -0.011(8) -0.022(8) -0.002(6) C56 0.038(8) 0.072(10) 0.050(9) -0.003(8) -0.010(7) -0.008(7) C57 0.045(8) 0.062(9) 0.044(9) -0.016(8) -0.008(7) -0.017(7) C58 0.065(10) 0.071(10) 0.057(10) -0.024(9) -0.008(8) 0.025(8) C59 0.134(16) 0.055(10) 0.057(11) -0.011(9) -0.008(11) 0.032(10) C60 0.086(11) 0.052(9) 0.064(11) 0.009(8) -0.028(9) -0.010(8) Lu 0.0256(3) 0.0332(3) 0.0339(3) -0.0098(2) -0.0047(2) -0.00710(19) N1 0.026(5) 0.039(6) 0.036(6) -0.015(5) -0.006(5) -0.004(4) N2 0.043(6) 0.026(5) 0.034(6) -0.014(5) -0.011(5) 0.001(4) N3 0.031(5) 0.030(5) 0.041(6) -0.009(5) -0.008(5) -0.002(4) N4 0.026(5) 0.045(6) 0.048(7) -0.022(5) -0.017(5) -0.004(4) N5 0.019(5) 0.071(7) 0.044(7) -0.024(6) -0.005(5) -0.015(5) N6 0.032(5) 0.040(6) 0.042(6) -0.010(5) -0.012(5) -0.010(4) P1 0.0258(16) 0.0352(17) 0.0342(19) -0.0088(15) -0.0053(14) -0.0069(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N4 1.412(13) . ? C1 C6 1.415(15) . ? C1 C2 1.428(15) . ? C2 C3 1.401(15) . ? C2 C10 1.530(16) . ? C3 C4 1.354(16) . ? C4 C5 1.374(16) . ? C5 C6 1.390(15) . ? C6 C7 1.514(15) . ? C7 C9 1.503(19) . ? C7 C8 1.555(18) . ? C10 C11 1.44(2) . ? C10 C12 1.498(19) . ? C13 N5 1.408(14) . ? C13 C18 1.413(15) . ? C13 C14 1.444(16) . ? C14 C15 1.393(16) . ? C14 C22 1.512(16) . ? C15 C16 1.385(18) . ? C16 C17 1.375(19) . ? C17 C18 1.407(17) . ? C18 C19 1.495(18) . ? C19 C20 1.525(16) . ? C19 C21 1.541(18) . ? C22 C23 1.521(17) . ? C22 C24 1.533(16) . ? C25 C26 1.402(16) . ? C25 C30 1.405(17) . ? C25 P1 1.771(13) . ? C26 C27 1.371(18) . ? C27 C28 1.412(19) . ? C28 C29 1.350(18) . ? C29 C30 1.366(18) . ? C31 C36 1.393(16) . ? C31 C32 1.409(15) . ? C31 P1 1.785(12) . ? C32 C33 1.384(17) . ? C33 C34 1.367(19) . ? C34 C35 1.398(17) . ? C35 C36 1.349(16) . ? C37 C38 1.383(14) . ? C37 C42 1.396(14) . ? C37 P1 1.805(11) . ? C38 C39 1.377(16) . ? C39 C40 1.394(17) . ? C40 C41 1.409(16) . ? C41 C42 1.365(15) . ? C42 C43 1.524(14) . ? C43 N6 1.451(14) . ? C44 C45 1.373(19) . ? C44 N6 1.414(15) . ? C44 C49 1.45(2) . ? C45 C46 1.416(18) . ? C45 C51 1.519(19) . ? C46 C47 1.42(3) . ? C47 C48 1.38(3) . ? C48 C49 1.36(2) . ? C49 C50 1.48(2) . ? C52 C53 1.409(16) . ? C52 C57 1.410(17) . ? C52 N1 1.441(14) . ? C53 C54 1.379(18) . ? C53 C59 1.484(19) . ? C54 C55 1.383(19) . ? C55 C56 1.357(18) . ? C55 C60 1.535(17) . ? C56 C57 1.397(17) . ? C57 C58 1.484(18) . ? Lu N5 2.142(10) . ? Lu N6 2.165(9) . ? Lu N4 2.175(9) . ? Lu N3 2.407(9) . ? Lu N1 2.532(9) . ? N1 N2 1.261(11) . ? N2 N3 1.377(11) . ? N3 P1 1.669(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 C1 C6 124.5(10) . . ? N4 C1 C2 118.1(10) . . ? C6 C1 C2 117.4(10) . . ? C3 C2 C1 119.9(11) . . ? C3 C2 C10 119.2(11) . . ? C1 C2 C10 120.7(10) . . ? C4 C3 C2 120.7(12) . . ? C3 C4 C5 120.9(11) . . ? C4 C5 C6 120.7(11) . . ? C5 C6 C1 120.3(11) . . ? C5 C6 C7 120.2(10) . . ? C1 C6 C7 119.4(10) . . ? C9 C7 C6 110.4(11) . . ? C9 C7 C8 110.6(12) . . ? C6 C7 C8 113.4(11) . . ? C11 C10 C12 111.4(15) . . ? C11 C10 C2 109.6(12) . . ? C12 C10 C2 113.9(11) . . ? N5 C13 C18 118.6(11) . . ? N5 C13 C14 121.9(10) . . ? C18 C13 C14 119.5(11) . . ? C15 C14 C13 120.2(11) . . ? C15 C14 C22 120.1(12) . . ? C13 C14 C22 119.5(11) . . ? C16 C15 C14 121.0(13) . . ? C17 C16 C15 117.5(13) . . ? C16 C17 C18 126.0(13) . . ? C17 C18 C13 115.8(12) . . ? C17 C18 C19 123.8(12) . . ? C13 C18 C19 120.4(12) . . ? C18 C19 C20 115.0(11) . . ? C18 C19 C21 110.1(11) . . ? C20 C19 C21 109.3(12) . . ? C14 C22 C23 115.1(12) . . ? C14 C22 C24 111.2(10) . . ? C23 C22 C24 110.2(11) . . ? C26 C25 C30 116.5(12) . . ? C26 C25 P1 121.5(10) . . ? C30 C25 P1 122.0(9) . . ? C27 C26 C25 121.1(14) . . ? C26 C27 C28 119.0(14) . . ? C29 C28 C27 121.6(14) . . ? C28 C29 C30 118.4(14) . . ? C29 C30 C25 123.3(12) . . ? C36 C31 C32 118.8(11) . . ? C36 C31 P1 119.6(9) . . ? C32 C31 P1 121.5(10) . . ? C33 C32 C31 119.8(14) . . ? C34 C33 C32 119.9(13) . . ? C33 C34 C35 120.4(12) . . ? C36 C35 C34 120.2(13) . . ? C35 C36 C31 120.8(12) . . ? C38 C37 C42 121.4(10) . . ? C38 C37 P1 116.6(8) . . ? C42 C37 P1 121.9(8) . . ? C39 C38 C37 120.2(11) . . ? C38 C39 C40 119.3(12) . . ? C39 C40 C41 119.8(12) . . ? C42 C41 C40 120.8(12) . . ? C41 C42 C37 118.5(11) . . ? C41 C42 C43 116.2(10) . . ? C37 C42 C43 125.2(10) . . ? N6 C43 C42 112.8(10) . . ? C45 C44 N6 121.5(13) . . ? C45 C44 C49 120.1(13) . . ? N6 C44 C49 118.3(14) . . ? C44 C45 C46 119.9(16) . . ? C44 C45 C51 120.6(12) . . ? C46 C45 C51 119.3(16) . . ? C45 C46 C47 117.7(17) . . ? C48 C47 C46 122.5(17) . . ? C49 C48 C47 119(2) . . ? C48 C49 C44 120.0(19) . . ? C48 C49 C50 116.7(18) . . ? C44 C49 C50 123.1(14) . . ? C53 C52 C57 122.3(12) . . ? C53 C52 N1 119.6(12) . . ? C57 C52 N1 118.1(11) . . ? C54 C53 C52 117.1(13) . . ? C54 C53 C59 122.8(12) . . ? C52 C53 C59 119.9(12) . . ? C53 C54 C55 122.8(12) . . ? C56 C55 C54 117.8(13) . . ? C56 C55 C60 119.4(14) . . ? C54 C55 C60 122.6(13) . . ? C55 C56 C57 124.5(14) . . ? C56 C57 C52 115.3(13) . . ? C56 C57 C58 122.6(13) . . ? C52 C57 C58 122.1(12) . . ? N5 Lu N6 105.7(4) . . ? N5 Lu N4 125.7(3) . . ? N6 Lu N4 96.5(3) . . ? N5 Lu N3 96.5(3) . . ? N6 Lu N3 83.4(3) . . ? N4 Lu N3 135.5(3) . . ? N5 Lu N1 90.0(3) . . ? N6 Lu N1 133.9(3) . . ? N4 Lu N1 109.1(3) . . ? N3 Lu N1 51.4(3) . . ? N2 N1 C52 111.0(9) . . ? N2 N1 Lu 98.6(6) . . ? C52 N1 Lu 150.4(7) . . ? N1 N2 N3 108.8(8) . . ? N2 N3 P1 110.9(7) . . ? N2 N3 Lu 101.0(6) . . ? P1 N3 Lu 148.1(5) . . ? C1 N4 Lu 143.0(8) . . ? C13 N5 Lu 153.2(7) . . ? C44 N6 C43 111.8(9) . . ? C44 N6 Lu 130.5(8) . . ? C43 N6 Lu 117.4(7) . . ? N3 P1 C25 113.3(5) . . ? N3 P1 C31 108.3(5) . . ? C25 P1 C31 107.5(6) . . ? N3 P1 C37 109.4(5) . . ? C25 P1 C37 108.8(5) . . ? C31 P1 C37 109.5(5) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.571 _refine_diff_density_min -1.273 _refine_diff_density_rms 0.169 #===========END============= data_complex_3b _database_code_depnum_ccdc_archive 'CCDC 673960' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H80 N10 P Sc Si2' _chemical_formula_weight 1097.47 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.0822(10) _cell_length_b 21.7373(18) _cell_length_c 12.8265(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.7380(10) _cell_angle_gamma 90.00 _cell_volume 3106.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9665 _exptl_absorpt_correction_T_max 0.9820 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 17592 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0845 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.06 _reflns_number_total 11378 _reflns_number_gt 9196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0192P)^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 -0.03(2) _refine_ls_number_reflns 11378 _refine_ls_number_parameters 702 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 0.895 _refine_ls_restrained_S_all 0.895 _refine_ls_shift/su_max 0.003 _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 Sc Sc 0.10348(4) 0.44513(2) 0.64515(4) 0.02559(13) Uani 1 1 d . . . P P -0.12803(6) 0.55773(3) 0.64802(6) 0.02640(17) Uani 1 1 d . . . Si1 Si 0.43235(8) 0.32892(4) 0.93648(8) 0.0408(2) Uani 1 1 d . . . Si2 Si -0.09575(8) 0.46542(4) 0.22855(7) 0.0405(2) Uani 1 1 d . . . N1 N -0.0373(2) 0.38731(11) 0.63273(19) 0.0322(6) Uani 1 1 d . . . N2 N 0.00375(19) 0.53094(10) 0.66210(18) 0.0282(6) Uani 1 1 d . . . N3 N 0.0828(2) 0.57768(10) 0.66673(18) 0.0263(5) Uani 1 1 d . . . N4 N 0.17924(19) 0.55470(11) 0.66659(17) 0.0252(5) Uani 1 1 d . . . N5 N 0.2633(2) 0.40879(10) 0.76968(18) 0.0271(5) Uani 1 1 d . . . N6 N 0.24361(19) 0.45531(11) 0.82683(18) 0.0277(5) Uani 1 1 d . . . N7 N 0.3319(2) 0.47407(11) 0.91597(19) 0.0309(6) Uani 1 1 d . . . N8 N 0.0589(2) 0.46078(10) 0.46856(18) 0.0296(6) Uani 1 1 d . . . N9 N 0.1431(2) 0.41893(10) 0.49220(19) 0.0309(6) Uani 1 1 d . . . N10 N 0.1890(2) 0.40626(11) 0.41912(19) 0.0323(6) Uani 1 1 d . . . C1 C -0.2029(2) 0.49913(13) 0.6949(2) 0.0284(7) Uani 1 1 d . . . C2 C -0.2586(3) 0.51506(15) 0.7680(3) 0.0368(8) Uani 1 1 d . . . H2 H -0.2525 0.5551 0.7952 0.044 Uiso 1 1 calc R . . C3 C -0.3224(3) 0.47210(17) 0.8000(3) 0.0500(9) Uani 1 1 d . . . H3 H -0.3596 0.4831 0.8486 0.060 Uiso 1 1 calc R . . C4 C -0.3313(3) 0.41278(17) 0.7603(3) 0.0538(10) Uani 1 1 d . . . H4 H -0.3745 0.3837 0.7822 0.065 Uiso 1 1 calc R . . C5 C -0.2767(3) 0.39618(15) 0.6882(3) 0.0462(9) Uani 1 1 d . . . H5 H -0.2831 0.3558 0.6624 0.055 Uiso 1 1 calc R . . C6 C -0.2116(2) 0.43899(14) 0.6530(2) 0.0320(7) Uani 1 1 d . . . C7 C -0.1546(2) 0.41723(13) 0.5727(2) 0.0320(7) Uani 1 1 d . . . H7A H -0.2082 0.3884 0.5192 0.038 Uiso 1 1 calc R . . H7B H -0.1440 0.4522 0.5305 0.038 Uiso 1 1 calc R . . C8 C -0.0453(2) 0.32249(14) 0.6436(3) 0.0324(7) Uani 1 1 d . . . C9 C -0.0057(3) 0.29559(15) 0.7514(3) 0.0374(8) Uani 1 1 d . . . C10 C -0.0100(3) 0.23175(16) 0.7605(3) 0.0487(9) Uani 1 1 d . . . H10 H 0.0176 0.2139 0.8319 0.058 Uiso 1 1 calc R . . C11 C -0.0537(3) 0.19463(16) 0.6667(3) 0.0522(9) Uani 1 1 d . . . H11 H -0.0569 0.1522 0.6746 0.063 Uiso 1 1 calc R . . C12 C -0.0926(3) 0.22076(14) 0.5615(3) 0.0433(9) Uani 1 1 d . . . H12 H -0.1228 0.1956 0.4980 0.052 Uiso 1 1 calc R . . C13 C -0.0880(3) 0.28372(15) 0.5475(3) 0.0371(8) Uani 1 1 d . . . C14 C -0.1256(3) 0.30871(14) 0.4292(3) 0.0452(9) Uani 1 1 d . . . H14A H -0.1018 0.2805 0.3841 0.068 Uiso 1 1 calc R . . H14B H -0.0878 0.3478 0.4315 0.068 Uiso 1 1 calc R . . H14C H -0.2112 0.3137 0.3967 0.068 Uiso 1 1 calc R . . C15 C 0.0394(3) 0.33485(15) 0.8557(2) 0.0518(9) Uani 1 1 d . . . H15A H 0.0576 0.3093 0.9213 0.078 Uiso 1 1 calc R . . H15B H -0.0211 0.3642 0.8527 0.078 Uiso 1 1 calc R . . H15C H 0.1106 0.3562 0.8599 0.078 Uiso 1 1 calc R . . C16 C -0.2187(2) 0.57625(13) 0.5038(2) 0.0286(7) Uani 1 1 d . . . C17 C -0.3397(3) 0.56135(14) 0.4545(2) 0.0384(8) Uani 1 1 d . . . H17 H -0.3762 0.5402 0.4956 0.046 Uiso 1 1 calc R . . C18 C -0.4058(3) 0.57831(16) 0.3433(3) 0.0505(10) Uani 1 1 d . . . H18 H -0.4866 0.5679 0.3093 0.061 Uiso 1 1 calc R . . C19 C -0.3517(3) 0.61050(15) 0.2834(3) 0.0475(9) Uani 1 1 d . . . H19 H -0.3967 0.6223 0.2093 0.057 Uiso 1 1 calc R . . C20 C -0.2320(3) 0.62540(14) 0.3317(2) 0.0398(8) Uani 1 1 d . . . H20 H -0.1963 0.6467 0.2901 0.048 Uiso 1 1 calc R . . C21 C -0.1651(3) 0.60876(13) 0.4417(2) 0.0323(7) Uani 1 1 d . . . H21 H -0.0842 0.6191 0.4747 0.039 Uiso 1 1 calc R . . C22 C -0.1125(2) 0.62713(13) 0.7288(2) 0.0271(7) Uani 1 1 d . . . C23 C -0.1519(3) 0.68332(13) 0.6770(2) 0.0328(7) Uani 1 1 d . . . H23 H -0.1934 0.6852 0.5991 0.039 Uiso 1 1 calc R . . C24 C -0.1300(3) 0.73653(14) 0.7405(3) 0.0399(8) Uani 1 1 d . . . H24 H -0.1557 0.7743 0.7053 0.048 Uiso 1 1 calc R . . C25 C -0.0698(3) 0.73366(15) 0.8560(3) 0.0431(8) Uani 1 1 d . . . H25 H -0.0551 0.7695 0.8987 0.052 Uiso 1 1 calc R . . C26 C -0.0313(3) 0.67809(16) 0.9085(3) 0.0433(8) Uani 1 1 d . . . H26 H 0.0087 0.6765 0.9866 0.052 Uiso 1 1 calc R . . C27 C -0.0518(3) 0.62485(14) 0.8460(2) 0.0380(8) Uani 1 1 d . . . H27 H -0.0253 0.5873 0.8817 0.046 Uiso 1 1 calc R . . C28 C 0.3068(3) 0.52593(13) 0.9713(2) 0.0303(7) Uani 1 1 d . . . C29 C 0.3928(2) 0.57325(13) 0.9986(2) 0.0303(7) Uani 1 1 d . . . C30 C 0.3779(3) 0.62406(15) 1.0564(2) 0.0391(8) Uani 1 1 d . . . H30 H 0.4317 0.6565 1.0697 0.047 Uiso 1 1 calc R . . C31 C 0.2864(3) 0.62877(15) 1.0956(3) 0.0424(8) Uani 1 1 d . . . C32 C 0.2065(3) 0.57982(15) 1.0722(2) 0.0419(8) Uani 1 1 d . . . H32 H 0.1458 0.5811 1.0999 0.050 Uiso 1 1 calc R . . C33 C 0.2135(3) 0.52899(14) 1.0089(2) 0.0364(8) Uani 1 1 d . . . C34 C 0.5006(3) 0.56784(14) 0.9670(2) 0.0397(8) Uani 1 1 d . . . H34A H 0.5450 0.6057 0.9844 0.059 Uiso 1 1 calc R . . H34B H 0.4744 0.5595 0.8876 0.059 Uiso 1 1 calc R . . H34C H 0.5511 0.5349 1.0091 0.059 Uiso 1 1 calc R . . C35 C 0.1235(3) 0.47748(15) 0.9886(3) 0.0509(9) Uani 1 1 d . . . H35A H 0.0707 0.4769 0.9103 0.076 Uiso 1 1 calc R . . H35B H 0.0776 0.4840 1.0343 0.076 Uiso 1 1 calc R . . H35C H 0.1651 0.4389 1.0084 0.076 Uiso 1 1 calc R . . C36 C 0.2738(3) 0.68459(17) 1.1603(3) 0.0663(11) Uani 1 1 d . . . H36A H 0.2292 0.7158 1.1081 0.099 Uiso 1 1 calc R . . H36B H 0.3520 0.7001 1.2061 0.099 Uiso 1 1 calc R . . H36C H 0.2323 0.6733 1.2080 0.099 Uiso 1 1 calc R . . C37 C 0.3852(2) 0.38354(14) 0.8118(2) 0.0323(7) Uani 1 1 d . . . H37A H 0.4408 0.4179 0.8322 0.039 Uiso 1 1 calc R . . H37B H 0.3954 0.3623 0.7496 0.039 Uiso 1 1 calc R . . C38 C 0.4115(4) 0.35745(17) 1.0635(3) 0.0647(11) Uani 1 1 d . . . H38A H 0.3273 0.3599 1.0482 0.097 Uiso 1 1 calc R . . H38B H 0.4468 0.3975 1.0828 0.097 Uiso 1 1 calc R . . H38C H 0.4494 0.3297 1.1254 0.097 Uiso 1 1 calc R . . C39 C 0.5968(3) 0.31618(17) 0.9754(3) 0.0691(12) Uani 1 1 d . . . H39A H 0.6265 0.2878 1.0375 0.104 Uiso 1 1 calc R . . H39B H 0.6385 0.3546 0.9970 0.104 Uiso 1 1 calc R . . H39C H 0.6097 0.2995 0.9116 0.104 Uiso 1 1 calc R . . C40 C 0.3509(3) 0.25596(15) 0.8884(3) 0.0606(10) Uani 1 1 d . . . H40A H 0.3762 0.2269 0.9495 0.091 Uiso 1 1 calc R . . H40B H 0.3678 0.2399 0.8264 0.091 Uiso 1 1 calc R . . H40C H 0.2662 0.2631 0.8643 0.091 Uiso 1 1 calc R . . C41 C 0.2882(3) 0.36464(13) 0.4575(2) 0.0301(7) Uani 1 1 d . . . C42 C 0.3765(3) 0.37642(14) 0.4146(2) 0.0363(8) Uani 1 1 d . . . C43 C 0.4739(3) 0.33753(15) 0.4425(3) 0.0427(9) Uani 1 1 d . . . H43 H 0.5327 0.3459 0.4144 0.051 Uiso 1 1 calc R . . C44 C 0.4872(3) 0.28626(15) 0.5109(3) 0.0407(8) Uani 1 1 d . . . C45 C 0.3978(3) 0.27455(14) 0.5501(2) 0.0393(8) Uani 1 1 d . . . H45 H 0.4048 0.2403 0.5956 0.047 Uiso 1 1 calc R . . C46 C 0.2971(3) 0.31235(13) 0.5236(2) 0.0337(7) Uani 1 1 d . . . C47 C 0.3652(3) 0.43000(15) 0.3359(3) 0.0518(10) Uani 1 1 d . . . H47A H 0.4349 0.4317 0.3174 0.078 Uiso 1 1 calc R . . H47B H 0.3585 0.4676 0.3724 0.078 Uiso 1 1 calc R . . H47C H 0.2949 0.4247 0.2680 0.078 Uiso 1 1 calc R . . C48 C 0.5941(3) 0.24350(17) 0.5377(3) 0.0577(10) Uani 1 1 d . . . H48A H 0.6544 0.2541 0.6099 0.087 Uiso 1 1 calc R . . H48B H 0.6265 0.2475 0.4805 0.087 Uiso 1 1 calc R . . H48C H 0.5688 0.2018 0.5396 0.087 Uiso 1 1 calc R . . C49 C 0.1986(3) 0.29233(14) 0.5610(3) 0.0398(8) Uani 1 1 d . . . H49A H 0.2084 0.2495 0.5810 0.060 Uiso 1 1 calc R . . H49B H 0.1220 0.2986 0.5004 0.060 Uiso 1 1 calc R . . H49C H 0.2026 0.3162 0.6254 0.060 Uiso 1 1 calc R . . C50 C 0.0241(3) 0.49515(14) 0.3623(2) 0.0360(7) Uani 1 1 d . . . H50A H 0.0961 0.5008 0.3471 0.043 Uiso 1 1 calc R . . H50B H -0.0010 0.5357 0.3760 0.043 Uiso 1 1 calc R . . C51 C -0.0495(3) 0.39393(16) 0.1755(3) 0.0592(10) Uani 1 1 d . . . H51A H -0.0442 0.3605 0.2262 0.089 Uiso 1 1 calc R . . H51B H 0.0273 0.4003 0.1713 0.089 Uiso 1 1 calc R . . H51C H -0.1078 0.3842 0.1017 0.089 Uiso 1 1 calc R . . C52 C -0.1201(3) 0.52924(16) 0.1244(3) 0.0567(10) Uani 1 1 d . . . H52A H -0.1679 0.5146 0.0499 0.085 Uiso 1 1 calc R . . H52B H -0.0440 0.5433 0.1263 0.085 Uiso 1 1 calc R . . H52C H -0.1609 0.5626 0.1434 0.085 Uiso 1 1 calc R . . C53 C -0.2386(3) 0.45152(17) 0.2476(3) 0.0532(9) Uani 1 1 d . . . H53A H -0.2266 0.4199 0.3032 0.080 Uiso 1 1 calc R . . H53B H -0.2993 0.4387 0.1771 0.080 Uiso 1 1 calc R . . H53C H -0.2636 0.4888 0.2724 0.080 Uiso 1 1 calc R . . C54 C 0.2756(2) 0.59693(13) 0.6861(2) 0.0257(6) Uani 1 1 d . . . C55 C 0.3661(2) 0.57694(13) 0.6517(2) 0.0287(7) Uani 1 1 d . . . C56 C 0.4667(3) 0.61355(14) 0.6742(2) 0.0341(7) Uani 1 1 d . . . H56 H 0.5256 0.6008 0.6491 0.041 Uiso 1 1 calc R . . C57 C 0.4824(3) 0.66851(15) 0.7329(2) 0.0368(8) Uani 1 1 d . . . C58 C 0.3912(3) 0.68731(14) 0.7657(2) 0.0367(8) Uani 1 1 d . . . H58 H 0.3996 0.7245 0.8037 0.044 Uiso 1 1 calc R . . C59 C 0.2873(2) 0.65290(13) 0.7441(2) 0.0298(7) Uani 1 1 d . . . C60 C 0.1979(2) 0.67764(14) 0.7905(2) 0.0361(8) Uani 1 1 d . . . H60A H 0.1252 0.6892 0.7290 0.054 Uiso 1 1 calc R . . H60B H 0.2314 0.7129 0.8370 0.054 Uiso 1 1 calc R . . H60C H 0.1806 0.6464 0.8349 0.054 Uiso 1 1 calc R . . C61 C 0.3568(3) 0.51681(14) 0.5907(3) 0.0422(8) Uani 1 1 d . . . H61A H 0.4288 0.5101 0.5774 0.063 Uiso 1 1 calc R . . H61B H 0.2892 0.5180 0.5198 0.063 Uiso 1 1 calc R . . H61C H 0.3466 0.4839 0.6361 0.063 Uiso 1 1 calc R . . C62 C 0.5972(3) 0.70513(15) 0.7629(3) 0.0537(10) Uani 1 1 d . . . H62A H 0.6533 0.6929 0.8362 0.081 Uiso 1 1 calc R . . H62B H 0.5799 0.7482 0.7638 0.081 Uiso 1 1 calc R . . H62C H 0.6312 0.6976 0.7077 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc 0.0254(3) 0.0249(3) 0.0274(3) -0.0004(2) 0.0112(2) 0.0007(2) P 0.0233(4) 0.0275(4) 0.0277(4) -0.0012(3) 0.0091(3) 0.0004(3) Si1 0.0404(6) 0.0368(6) 0.0424(5) 0.0088(4) 0.0131(4) 0.0082(4) Si2 0.0416(6) 0.0462(6) 0.0306(5) -0.0009(4) 0.0105(4) 0.0085(4) N1 0.0303(15) 0.0276(15) 0.0409(15) -0.0021(11) 0.0162(12) -0.0022(11) N2 0.0231(13) 0.0288(14) 0.0343(14) -0.0011(11) 0.0129(11) -0.0037(11) N3 0.0253(14) 0.0265(14) 0.0264(13) 0.0017(10) 0.0092(11) 0.0017(11) N4 0.0209(13) 0.0301(14) 0.0255(12) -0.0001(11) 0.0099(10) 0.0008(11) N5 0.0262(13) 0.0251(14) 0.0318(13) 0.0014(11) 0.0131(11) 0.0049(10) N6 0.0286(14) 0.0265(15) 0.0307(13) 0.0042(11) 0.0143(11) 0.0025(11) N7 0.0282(14) 0.0321(15) 0.0279(13) 0.0000(11) 0.0060(11) 0.0011(11) N8 0.0298(14) 0.0273(15) 0.0322(13) 0.0004(11) 0.0125(11) 0.0039(11) N9 0.0316(15) 0.0277(14) 0.0350(15) -0.0041(11) 0.0146(12) -0.0028(11) N10 0.0342(15) 0.0321(15) 0.0333(14) -0.0026(11) 0.0160(12) -0.0002(12) C1 0.0204(16) 0.0333(18) 0.0282(16) 0.0022(14) 0.0059(13) -0.0007(13) C2 0.0340(18) 0.039(2) 0.0426(19) -0.0034(15) 0.0212(15) 0.0001(15) C3 0.049(2) 0.060(3) 0.056(2) -0.003(2) 0.0375(19) 0.0002(19) C4 0.046(2) 0.052(3) 0.079(3) 0.013(2) 0.042(2) -0.0052(19) C5 0.040(2) 0.033(2) 0.070(2) -0.0038(18) 0.0260(19) -0.0042(16) C6 0.0244(16) 0.0328(19) 0.0387(17) 0.0004(15) 0.0123(13) 0.0013(14) C7 0.0274(17) 0.0292(17) 0.0395(18) -0.0030(14) 0.0128(14) -0.0044(13) C8 0.0259(17) 0.0304(19) 0.0449(19) 0.0000(15) 0.0181(15) -0.0022(14) C9 0.0342(19) 0.041(2) 0.046(2) 0.0012(16) 0.0250(16) -0.0048(15) C10 0.048(2) 0.043(2) 0.064(2) 0.0154(19) 0.0310(19) -0.0013(17) C11 0.053(2) 0.025(2) 0.086(3) 0.001(2) 0.036(2) -0.0013(16) C12 0.042(2) 0.028(2) 0.064(2) -0.0088(17) 0.0258(18) -0.0024(15) C13 0.0291(18) 0.036(2) 0.051(2) -0.0057(16) 0.0204(16) -0.0043(14) C14 0.047(2) 0.040(2) 0.048(2) -0.0129(16) 0.0190(17) -0.0046(16) C15 0.064(3) 0.053(2) 0.042(2) 0.0057(18) 0.0245(18) -0.0070(19) C16 0.0232(16) 0.0258(17) 0.0336(16) -0.0012(13) 0.0076(13) 0.0034(12) C17 0.0318(18) 0.039(2) 0.0406(18) 0.0038(16) 0.0097(15) -0.0017(15) C18 0.032(2) 0.058(3) 0.046(2) -0.0034(18) -0.0021(17) -0.0017(17) C19 0.051(2) 0.045(2) 0.0332(19) 0.0041(16) 0.0007(17) 0.0101(17) C20 0.044(2) 0.036(2) 0.0375(19) 0.0001(15) 0.0133(16) 0.0070(16) C21 0.0291(17) 0.0328(19) 0.0331(18) -0.0024(14) 0.0101(14) 0.0038(13) C22 0.0232(16) 0.0297(17) 0.0316(17) -0.0056(13) 0.0140(13) -0.0005(13) C23 0.0327(18) 0.0315(18) 0.0347(17) -0.0035(15) 0.0136(14) -0.0005(14) C24 0.041(2) 0.0314(19) 0.049(2) -0.0005(16) 0.0188(17) 0.0045(15) C25 0.045(2) 0.042(2) 0.045(2) -0.0137(17) 0.0199(17) -0.0040(17) C26 0.048(2) 0.050(2) 0.0329(18) -0.0104(17) 0.0164(16) 0.0013(17) C27 0.042(2) 0.0338(19) 0.0370(19) 0.0019(15) 0.0141(15) 0.0056(15) C28 0.0318(17) 0.0311(18) 0.0239(16) 0.0007(13) 0.0062(13) 0.0071(14) C29 0.0265(17) 0.0353(19) 0.0248(16) 0.0001(13) 0.0052(13) 0.0053(14) C30 0.0301(18) 0.043(2) 0.0380(19) -0.0019(16) 0.0058(15) 0.0025(15) C31 0.039(2) 0.049(2) 0.0336(18) -0.0115(16) 0.0073(15) 0.0020(16) C32 0.0334(19) 0.056(2) 0.0401(19) -0.0051(17) 0.0184(16) 0.0055(16) C33 0.0326(18) 0.041(2) 0.0351(18) -0.0019(15) 0.0126(15) 0.0003(15) C34 0.0349(18) 0.043(2) 0.0408(19) 0.0010(16) 0.0146(15) 0.0029(15) C35 0.053(2) 0.047(2) 0.066(2) -0.0063(18) 0.0376(19) -0.0020(18) C36 0.056(2) 0.071(3) 0.072(3) -0.037(2) 0.024(2) -0.008(2) C37 0.0300(17) 0.0338(18) 0.0332(17) -0.0038(14) 0.0123(14) 0.0038(14) C38 0.091(3) 0.054(3) 0.051(2) 0.0100(19) 0.029(2) 0.012(2) C39 0.050(3) 0.075(3) 0.071(3) 0.037(2) 0.011(2) 0.019(2) C40 0.070(3) 0.037(2) 0.070(3) 0.0079(19) 0.021(2) 0.0052(19) C41 0.0320(17) 0.0285(18) 0.0309(16) -0.0110(14) 0.0133(14) -0.0004(13) C42 0.0373(19) 0.038(2) 0.0370(18) -0.0061(15) 0.0185(16) 0.0002(15) C43 0.033(2) 0.055(2) 0.048(2) -0.0119(18) 0.0239(17) -0.0042(16) C44 0.0343(19) 0.043(2) 0.041(2) -0.0118(16) 0.0106(16) 0.0044(16) C45 0.043(2) 0.035(2) 0.0385(19) -0.0045(15) 0.0141(17) 0.0008(16) C46 0.0380(19) 0.0314(19) 0.0343(18) -0.0093(14) 0.0166(15) 0.0000(15) C47 0.062(2) 0.048(2) 0.062(2) -0.0009(18) 0.042(2) 0.0001(18) C48 0.044(2) 0.066(3) 0.064(2) -0.004(2) 0.0203(19) 0.0149(19) C49 0.047(2) 0.0307(19) 0.048(2) 0.0012(15) 0.0251(17) -0.0002(15) C50 0.0376(19) 0.0343(19) 0.0387(18) 0.0010(14) 0.0177(15) 0.0043(14) C51 0.063(3) 0.056(2) 0.050(2) -0.0160(19) 0.0126(19) 0.008(2) C52 0.061(2) 0.071(3) 0.039(2) 0.0059(19) 0.0200(18) 0.009(2) C53 0.047(2) 0.055(2) 0.052(2) -0.003(2) 0.0131(17) 0.0006(19) C54 0.0234(16) 0.0278(17) 0.0255(16) 0.0008(13) 0.0091(13) -0.0021(13) C55 0.0270(17) 0.0344(19) 0.0240(15) 0.0024(13) 0.0093(13) 0.0001(13) C56 0.0297(18) 0.042(2) 0.0375(18) -0.0002(15) 0.0207(15) 0.0024(15) C57 0.0296(18) 0.042(2) 0.0405(19) 0.0010(15) 0.0154(15) -0.0068(15) C58 0.0345(19) 0.0345(19) 0.0416(19) -0.0071(15) 0.0153(15) -0.0040(15) C59 0.0279(17) 0.0281(17) 0.0330(17) 0.0025(13) 0.0113(14) 0.0010(13) C60 0.0304(18) 0.0358(19) 0.0418(18) -0.0123(15) 0.0136(15) -0.0027(14) C61 0.0358(19) 0.048(2) 0.050(2) -0.0130(17) 0.0249(16) -0.0039(16) C62 0.043(2) 0.053(2) 0.074(3) -0.018(2) 0.0326(19) -0.0152(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc N1 2.071(2) . ? Sc N5 2.126(2) . ? Sc N8 2.143(2) . ? Sc N9 2.265(2) . ? Sc N2 2.276(2) . ? Sc N6 2.301(2) . ? Sc N4 2.528(2) . ? P N2 1.638(2) . ? P C16 1.794(3) . ? P C1 1.795(3) . ? P C22 1.798(3) . ? Si1 C40 1.842(3) . ? Si1 C38 1.849(3) . ? Si1 C39 1.873(3) . ? Si1 C37 1.894(3) . ? Si2 C53 1.859(3) . ? Si2 C51 1.867(3) . ? Si2 C52 1.869(3) . ? Si2 C50 1.881(3) . ? N1 C8 1.423(4) . ? N1 C7 1.477(3) . ? N2 N3 1.380(3) . ? N3 N4 1.269(3) . ? N4 C54 1.426(3) . ? N5 N6 1.323(3) . ? N5 C37 1.465(3) . ? N6 N7 1.292(3) . ? N7 C28 1.426(3) . ? N8 N9 1.310(3) . ? N8 C50 1.466(3) . ? N9 N10 1.289(3) . ? N10 C41 1.429(3) . ? C1 C2 1.393(4) . ? C1 C6 1.402(4) . ? C2 C3 1.371(4) . ? C3 C4 1.376(4) . ? C4 C5 1.374(4) . ? C5 C6 1.401(4) . ? C6 C7 1.518(4) . ? C8 C9 1.404(4) . ? C8 C13 1.416(4) . ? C9 C10 1.395(4) . ? C9 C15 1.500(4) . ? C10 C11 1.373(4) . ? C11 C12 1.369(4) . ? C12 C13 1.384(4) . ? C13 C14 1.507(4) . ? C16 C17 1.388(4) . ? C16 C21 1.398(4) . ? C17 C18 1.388(4) . ? C18 C19 1.377(4) . ? C19 C20 1.374(4) . ? C20 C21 1.376(4) . ? C22 C23 1.384(4) . ? C22 C27 1.395(4) . ? C23 C24 1.380(4) . ? C24 C25 1.376(4) . ? C25 C26 1.374(4) . ? C26 C27 1.375(4) . ? C28 C33 1.389(4) . ? C28 C29 1.407(4) . ? C29 C30 1.381(4) . ? C29 C34 1.511(4) . ? C30 C31 1.383(4) . ? C31 C32 1.390(4) . ? C31 C36 1.511(4) . ? C32 C33 1.393(4) . ? C33 C35 1.511(4) . ? C41 C46 1.397(4) . ? C41 C42 1.400(4) . ? C42 C43 1.380(4) . ? C42 C47 1.512(4) . ? C43 C44 1.389(4) . ? C44 C45 1.380(4) . ? C44 C48 1.518(4) . ? C45 C46 1.397(4) . ? C46 C49 1.509(4) . ? C54 C55 1.398(4) . ? C54 C59 1.405(4) . ? C55 C56 1.387(4) . ? C55 C61 1.505(4) . ? C56 C57 1.386(4) . ? C57 C58 1.384(4) . ? C57 C62 1.514(4) . ? C58 C59 1.395(4) . ? C59 C60 1.518(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sc N5 108.24(9) . . ? N1 Sc N8 98.74(9) . . ? N5 Sc N8 129.57(9) . . ? N1 Sc N9 102.91(9) . . ? N5 Sc N9 97.04(9) . . ? N8 Sc N9 34.44(8) . . ? N1 Sc N2 93.16(9) . . ? N5 Sc N2 126.39(9) . . ? N8 Sc N2 92.57(8) . . ? N9 Sc N2 125.86(9) . . ? N1 Sc N6 113.40(8) . . ? N5 Sc N6 34.50(8) . . ? N8 Sc N6 147.23(8) . . ? N9 Sc N6 125.60(8) . . ? N2 Sc N6 91.94(8) . . ? N1 Sc N4 146.31(8) . . ? N5 Sc N4 94.74(8) . . ? N8 Sc N4 84.14(8) . . ? N9 Sc N4 98.18(8) . . ? N2 Sc N4 53.16(7) . . ? N6 Sc N4 72.87(7) . . ? N2 P C16 111.95(13) . . ? N2 P C1 107.73(12) . . ? C16 P C1 108.59(13) . . ? N2 P C22 110.76(12) . . ? C16 P C22 106.97(13) . . ? C1 P C22 110.85(13) . . ? C40 Si1 C38 110.26(17) . . ? C40 Si1 C39 109.65(17) . . ? C38 Si1 C39 107.87(18) . . ? C40 Si1 C37 108.04(14) . . ? C38 Si1 C37 115.78(14) . . ? C39 Si1 C37 105.03(14) . . ? C53 Si2 C51 109.68(17) . . ? C53 Si2 C52 108.49(16) . . ? C51 Si2 C52 110.11(16) . . ? C53 Si2 C50 111.23(14) . . ? C51 Si2 C50 112.66(15) . . ? C52 Si2 C50 104.48(15) . . ? C8 N1 C7 113.6(2) . . ? C8 N1 Sc 132.68(18) . . ? C7 N1 Sc 111.54(18) . . ? N3 N2 P 111.69(17) . . ? N3 N2 Sc 102.98(15) . . ? P N2 Sc 143.96(13) . . ? N4 N3 N2 109.3(2) . . ? N3 N4 C54 115.7(2) . . ? N3 N4 Sc 94.41(16) . . ? C54 N4 Sc 149.53(18) . . ? N6 N5 C37 116.9(2) . . ? N6 N5 Sc 80.02(14) . . ? C37 N5 Sc 155.20(18) . . ? N7 N6 N5 117.9(2) . . ? N7 N6 Sc 163.60(18) . . ? N5 N6 Sc 65.49(13) . . ? N6 N7 C28 115.4(2) . . ? N9 N8 C50 119.2(2) . . ? N9 N8 Sc 77.86(15) . . ? C50 N8 Sc 158.11(19) . . ? N10 N9 N8 119.6(2) . . ? N10 N9 Sc 167.85(19) . . ? N8 N9 Sc 67.70(14) . . ? N9 N10 C41 115.1(2) . . ? C2 C1 C6 120.4(3) . . ? C2 C1 P 119.1(2) . . ? C6 C1 P 120.4(2) . . ? C3 C2 C1 120.4(3) . . ? C2 C3 C4 120.0(3) . . ? C5 C4 C3 120.4(3) . . ? C4 C5 C6 121.1(3) . . ? C5 C6 C1 117.7(3) . . ? C5 C6 C7 118.0(3) . . ? C1 C6 C7 124.3(3) . . ? N1 C7 C6 112.3(2) . . ? C9 C8 C13 118.7(3) . . ? C9 C8 N1 119.9(3) . . ? C13 C8 N1 121.3(3) . . ? C10 C9 C8 119.1(3) . . ? C10 C9 C15 120.2(3) . . ? C8 C9 C15 120.6(3) . . ? C11 C10 C9 121.7(3) . . ? C12 C11 C10 119.3(3) . . ? C11 C12 C13 121.5(3) . . ? C12 C13 C8 119.7(3) . . ? C12 C13 C14 118.4(3) . . ? C8 C13 C14 121.9(3) . . ? C17 C16 C21 119.8(3) . . ? C17 C16 P 122.3(2) . . ? C21 C16 P 117.9(2) . . ? C16 C17 C18 119.5(3) . . ? C19 C18 C17 120.0(3) . . ? C20 C19 C18 120.8(3) . . ? C19 C20 C21 120.0(3) . . ? C20 C21 C16 119.9(3) . . ? C23 C22 C27 119.2(3) . . ? C23 C22 P 121.6(2) . . ? C27 C22 P 119.0(2) . . ? C24 C23 C22 120.3(3) . . ? C25 C24 C23 119.9(3) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C27 120.2(3) . . ? C26 C27 C22 120.0(3) . . ? C33 C28 C29 120.0(3) . . ? C33 C28 N7 124.6(3) . . ? C29 C28 N7 115.0(3) . . ? C30 C29 C28 118.7(3) . . ? C30 C29 C34 120.8(3) . . ? C28 C29 C34 120.5(3) . . ? C29 C30 C31 122.9(3) . . ? C30 C31 C32 116.8(3) . . ? C30 C31 C36 121.6(3) . . ? C32 C31 C36 121.6(3) . . ? C31 C32 C33 122.6(3) . . ? C28 C33 C32 118.7(3) . . ? C28 C33 C35 122.1(3) . . ? C32 C33 C35 119.1(3) . . ? N5 C37 Si1 118.51(19) . . ? C46 C41 C42 119.7(3) . . ? C46 C41 N10 125.6(3) . . ? C42 C41 N10 114.5(3) . . ? C43 C42 C41 119.3(3) . . ? C43 C42 C47 119.6(3) . . ? C41 C42 C47 121.1(3) . . ? C42 C43 C44 122.3(3) . . ? C45 C44 C43 117.5(3) . . ? C45 C44 C48 121.5(3) . . ? C43 C44 C48 121.0(3) . . ? C44 C45 C46 122.3(3) . . ? C45 C46 C41 118.8(3) . . ? C45 C46 C49 118.2(3) . . ? C41 C46 C49 122.8(3) . . ? N8 C50 Si2 121.1(2) . . ? C55 C54 C59 120.4(3) . . ? C55 C54 N4 115.4(2) . . ? C59 C54 N4 124.0(2) . . ? C56 C55 C54 119.1(3) . . ? C56 C55 C61 119.3(3) . . ? C54 C55 C61 121.6(3) . . ? C57 C56 C55 122.2(3) . . ? C58 C57 C56 117.5(3) . . ? C58 C57 C62 121.7(3) . . ? C56 C57 C62 120.7(3) . . ? C57 C58 C59 122.9(3) . . ? C58 C59 C54 117.9(3) . . ? C58 C59 C60 117.1(3) . . ? C54 C59 C60 125.0(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.498 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.040