# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dr. Qi Shen' _publ_contact_author_email qshen@suda.edu.cn loop_ _publ_author_name 'Wenbo Li' 'Mingqiang Xue' 'Yong Zhang' 'Qi Shen' # Attachment '- shelxl 2.cif' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 862443' #TrackingRef '- shelxl 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H62 N5 O2 Pr Si2' _chemical_formula_sum 'C39 H62 N5 O2 Pr Si2' _chemical_formula_weight 830.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 48.194(5) _cell_length_b 9.0139(9) _cell_length_c 19.816(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.281(3) _cell_angle_gamma 90.00 _cell_volume 8556.6(16) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 17016 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3472 _exptl_absorpt_coefficient_mu 1.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.552 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21163 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 58 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7915 _reflns_number_gt 6567 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+18.0923P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7915 _refine_ls_number_parameters 468 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 Pr1 Pr 0.868944(6) 0.49150(3) 0.690740(14) 0.02997(11) Uani 1 1 d . A . Si1 Si 0.79478(3) 0.3137(2) 0.71887(9) 0.0470(4) Uani 1 1 d . . . Si2 Si 0.94925(3) 0.36737(17) 0.66444(8) 0.0369(4) Uani 1 1 d . A . O1 O 0.86400(8) 0.2161(4) 0.65213(18) 0.0407(9) Uani 1 1 d . . . O2 O 0.88231(8) 0.2874(4) 0.77862(17) 0.0369(9) Uani 1 1 d . . . N1 N 0.81678(9) 0.4472(5) 0.6917(2) 0.0375(11) Uani 1 1 d . . . N2 N 0.83133(9) 0.6431(5) 0.6330(2) 0.0395(11) Uani 1 1 d D . . N3 N 0.91654(9) 0.4420(5) 0.6430(2) 0.0340(11) Uani 1 1 d . . . N4 N 0.88183(10) 0.5651(7) 0.5805(2) 0.0634(17) Uani 1 1 d D . . N5 N 0.89366(9) 0.6521(5) 0.7688(2) 0.0379(11) Uani 1 1 d D . . H5 H 0.9097(5) 0.637(6) 0.754(2) 0.034(16) Uiso 1 1 d D . . C1 C 0.81144(11) 0.5458(6) 0.6412(3) 0.0374(13) Uani 1 1 d . A . C2 C 0.90826(12) 0.5278(6) 0.5898(3) 0.0412(14) Uani 1 1 d . A . C3 C 0.8291(6) 0.747(4) 0.5762(14) 0.0464(19) Uani 0.50 1 d PD A 1 H3A H 0.8213 0.8405 0.5910 0.056 Uiso 0.50 1 calc PR A 1 H3B H 0.8160 0.7068 0.5396 0.056 Uiso 0.50 1 calc PR A 1 C3' C 0.8265(6) 0.753(4) 0.5784(13) 0.0464(19) Uani 0.50 1 d PD A 2 H3'1 H 0.8324 0.8517 0.5955 0.056 Uiso 0.50 1 calc PR A 2 H3'2 H 0.8066 0.7578 0.5621 0.056 Uiso 0.50 1 calc PR A 2 C4 C 0.8564(3) 0.7808(14) 0.5479(7) 0.047(2) Uani 0.50 1 d PD A 1 H4A H 0.8532 0.8550 0.5117 0.056 Uiso 0.50 1 calc PR A 1 H4B H 0.8698 0.8220 0.5838 0.056 Uiso 0.50 1 calc PR A 1 C4' C 0.8431(3) 0.7092(14) 0.5207(6) 0.047(2) Uani 0.50 1 d PD A 2 H4'1 H 0.8351 0.6160 0.5018 0.056 Uiso 0.50 1 calc PR A 2 H4'2 H 0.8396 0.7845 0.4852 0.056 Uiso 0.50 1 calc PR A 2 C5 C 0.8682(5) 0.642(2) 0.5202(11) 0.068(7) Uani 0.50 1 d PD A 1 H5A H 0.8534 0.5810 0.4967 0.081 Uiso 0.50 1 calc PR A 1 H5B H 0.8818 0.6664 0.4885 0.081 Uiso 0.50 1 calc PR A 1 C5' C 0.8741(5) 0.688(3) 0.5329(13) 0.068(7) Uani 0.50 1 d PD A 2 H5'1 H 0.8814 0.6677 0.4896 0.081 Uiso 0.50 1 calc PR A 2 H5'2 H 0.8828 0.7800 0.5514 0.081 Uiso 0.50 1 calc PR A 2 C6 C 0.78469(11) 0.5419(6) 0.5944(3) 0.0380(13) Uani 1 1 d . . . C7 C 0.78220(13) 0.4442(7) 0.5411(3) 0.0524(17) Uani 1 1 d . A . H7 H 0.7972 0.3807 0.5347 0.063 Uiso 1 1 calc R . . C8 C 0.75807(16) 0.4375(8) 0.4965(4) 0.072(2) Uani 1 1 d . . . H8 H 0.7568 0.3705 0.4599 0.087 Uiso 1 1 calc R A . C9 C 0.73615(14) 0.5284(8) 0.5057(4) 0.068(2) Uani 1 1 d . A . H9 H 0.7196 0.5229 0.4758 0.082 Uiso 1 1 calc R . . C10 C 0.73810(13) 0.6274(9) 0.5583(4) 0.065(2) Uani 1 1 d . . . H10 H 0.7229 0.6896 0.5647 0.078 Uiso 1 1 calc R A . C11 C 0.76273(13) 0.6359(7) 0.6027(3) 0.0551(17) Uani 1 1 d . A . H11 H 0.7643 0.7056 0.6382 0.066 Uiso 1 1 calc R . . C12 C 0.92872(11) 0.5843(7) 0.5419(3) 0.0385(14) Uani 1 1 d . . . C13 C 0.94001(13) 0.7244(7) 0.5509(3) 0.0507(16) Uani 1 1 d . A . H13 H 0.9344 0.7863 0.5851 0.061 Uiso 1 1 calc R . . C14 C 0.95966(13) 0.7746(8) 0.5097(3) 0.0601(19) Uani 1 1 d . . . H14 H 0.9676 0.8693 0.5165 0.072 Uiso 1 1 calc R A . C15 C 0.96733(14) 0.6836(9) 0.4585(4) 0.070(2) Uani 1 1 d . A . H15 H 0.9806 0.7160 0.4302 0.084 Uiso 1 1 calc R . . C16 C 0.95533(14) 0.5447(9) 0.4492(3) 0.065(2) Uani 1 1 d . . . H16 H 0.9604 0.4832 0.4143 0.079 Uiso 1 1 calc R A . C17 C 0.93606(12) 0.4950(7) 0.4905(3) 0.0475(15) Uani 1 1 d . A . H17 H 0.9280 0.4006 0.4835 0.057 Uiso 1 1 calc R . . C18 C 0.80788(14) 0.2733(7) 0.8092(3) 0.0623(19) Uani 1 1 d . . . H18A H 0.8280 0.2620 0.8134 0.093 Uiso 1 1 calc R . . H18B H 0.7995 0.1823 0.8233 0.093 Uiso 1 1 calc R . . H18C H 0.8030 0.3545 0.8377 0.093 Uiso 1 1 calc R . . C19 C 0.79537(14) 0.1389(7) 0.6688(3) 0.0630(19) Uani 1 1 d . . . H19A H 0.7877 0.1575 0.6223 0.094 Uiso 1 1 calc R . . H19B H 0.7843 0.0639 0.6885 0.094 Uiso 1 1 calc R . . H19C H 0.8145 0.1042 0.6697 0.094 Uiso 1 1 calc R . . C20 C 0.75751(13) 0.3707(9) 0.7187(4) 0.088(3) Uani 1 1 d . . . H20A H 0.7566 0.4664 0.7407 0.132 Uiso 1 1 calc R . . H20B H 0.7477 0.2976 0.7431 0.132 Uiso 1 1 calc R . . H20C H 0.7489 0.3777 0.6723 0.132 Uiso 1 1 calc R . . C21 C 0.97902(11) 0.4955(7) 0.6576(3) 0.0519(17) Uani 1 1 d . . . H21A H 0.9809 0.5139 0.6101 0.078 Uiso 1 1 calc R A . H21B H 0.9961 0.4509 0.6792 0.078 Uiso 1 1 calc R . . H21C H 0.9756 0.5885 0.6799 0.078 Uiso 1 1 calc R . . C22 C 0.95543(13) 0.1979(7) 0.6134(3) 0.0537(17) Uani 1 1 d . . . H22A H 0.9401 0.1290 0.6153 0.081 Uiso 1 1 calc R A . H22B H 0.9727 0.1510 0.6318 0.081 Uiso 1 1 calc R . . H22C H 0.9567 0.2261 0.5665 0.081 Uiso 1 1 calc R . . C23 C 0.95086(11) 0.3125(6) 0.7561(3) 0.0425(14) Uani 1 1 d . . . H23A H 0.9488 0.4000 0.7836 0.064 Uiso 1 1 calc R A . H23B H 0.9687 0.2661 0.7702 0.064 Uiso 1 1 calc R . . H23C H 0.9359 0.2431 0.7620 0.064 Uiso 1 1 calc R . . C24 C 0.89599(12) 0.7482(6) 0.8237(3) 0.0370(14) Uani 1 1 d . A . C25 C 0.92169(12) 0.8187(6) 0.8483(3) 0.0396(14) Uani 1 1 d . . . C26 C 0.92210(13) 0.9142(6) 0.9037(3) 0.0464(15) Uani 1 1 d . A . H26 H 0.9391 0.9585 0.9205 0.056 Uiso 1 1 calc R . . C27 C 0.89833(13) 0.9470(7) 0.9355(3) 0.0513(17) Uani 1 1 d . . . H27 H 0.8990 1.0144 0.9718 0.062 Uiso 1 1 calc R A . C28 C 0.87411(13) 0.8773(6) 0.9116(3) 0.0470(15) Uani 1 1 d . A . H28 H 0.8580 0.8973 0.9330 0.056 Uiso 1 1 calc R . . C29 C 0.87185(12) 0.7785(6) 0.8575(3) 0.0374(13) Uani 1 1 d . . . C30 C 0.94765(12) 0.7926(6) 0.8127(3) 0.0468(16) Uani 1 1 d . A . H30 H 0.9487 0.6849 0.8034 0.056 Uiso 1 1 calc R . . C31 C 0.94564(13) 0.8728(7) 0.7445(3) 0.0574(18) Uani 1 1 d . . . H31A H 0.9288 0.8415 0.7167 0.086 Uiso 1 1 calc R A . H31B H 0.9618 0.8488 0.7216 0.086 Uiso 1 1 calc R . . H31C H 0.9450 0.9790 0.7519 0.086 Uiso 1 1 calc R . . C32 C 0.97513(13) 0.8372(8) 0.8548(4) 0.076(2) Uani 1 1 d . . . H32A H 0.9755 0.9439 0.8612 0.114 Uiso 1 1 calc R A . H32B H 0.9908 0.8073 0.8311 0.114 Uiso 1 1 calc R . . H32C H 0.9764 0.7886 0.8987 0.114 Uiso 1 1 calc R . . C33 C 0.84384(12) 0.7099(6) 0.8323(3) 0.0454(15) Uani 1 1 d . A . H33 H 0.8475 0.6173 0.8079 0.054 Uiso 1 1 calc R . . C34 C 0.82716(13) 0.8125(7) 0.7819(3) 0.0619(19) Uani 1 1 d . . . H34A H 0.8232 0.9043 0.8045 0.093 Uiso 1 1 calc R A . H34B H 0.8098 0.7647 0.7648 0.093 Uiso 1 1 calc R . . H34C H 0.8379 0.8338 0.7445 0.093 Uiso 1 1 calc R . . C35 C 0.82608(15) 0.6692(8) 0.8891(4) 0.079(2) Uani 1 1 d . . . H35A H 0.8375 0.6171 0.9249 0.118 Uiso 1 1 calc R A . H35B H 0.8108 0.6059 0.8711 0.118 Uiso 1 1 calc R . . H35C H 0.8187 0.7590 0.9075 0.118 Uiso 1 1 calc R . . C36 C 0.88093(12) 0.1111(6) 0.6903(3) 0.0455(15) Uani 1 1 d . . . H36A H 0.9005 0.1243 0.6824 0.055 Uiso 1 1 calc R . . H36B H 0.8752 0.0103 0.6764 0.055 Uiso 1 1 calc R . . C37 C 0.87782(12) 0.1330(6) 0.7640(3) 0.0426(14) Uani 1 1 d . . . H37A H 0.8591 0.1035 0.7736 0.051 Uiso 1 1 calc R . . H37B H 0.8915 0.0728 0.7921 0.051 Uiso 1 1 calc R . . C38 C 0.86334(14) 0.1944(7) 0.5796(3) 0.0574(18) Uani 1 1 d . . . H38A H 0.8823 0.1944 0.5672 0.086 Uiso 1 1 calc R . . H38B H 0.8528 0.2741 0.5560 0.086 Uiso 1 1 calc R . . H38C H 0.8545 0.1002 0.5671 0.086 Uiso 1 1 calc R . . C39 C 0.88807(13) 0.3128(7) 0.8508(3) 0.0519(17) Uani 1 1 d . . . H39A H 0.8726 0.2761 0.8736 0.078 Uiso 1 1 calc R . . H39B H 0.8904 0.4183 0.8593 0.078 Uiso 1 1 calc R . . H39C H 0.9050 0.2611 0.8679 0.078 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 Pr1 0.03192(18) 0.03187(17) 0.02572(17) 0.00184(13) 0.00131(13) -0.00169(14) Si1 0.0362(9) 0.0501(10) 0.0556(11) 0.0101(9) 0.0093(8) -0.0046(8) Si2 0.0366(9) 0.0373(9) 0.0371(9) 0.0037(7) 0.0050(7) 0.0031(7) O1 0.052(2) 0.042(2) 0.027(2) -0.0060(18) -0.0005(18) 0.0008(19) O2 0.056(2) 0.030(2) 0.024(2) 0.0014(16) -0.0006(18) -0.0018(18) N1 0.035(3) 0.038(3) 0.041(3) 0.011(2) 0.007(2) 0.000(2) N2 0.036(3) 0.034(3) 0.048(3) 0.007(2) 0.001(2) 0.000(2) N3 0.032(2) 0.041(3) 0.029(2) 0.004(2) 0.005(2) 0.001(2) N4 0.042(3) 0.110(5) 0.040(3) 0.042(3) 0.014(3) 0.021(3) N5 0.035(3) 0.038(3) 0.041(3) -0.004(2) 0.007(2) -0.001(2) C1 0.037(3) 0.040(3) 0.036(3) -0.008(3) 0.003(3) 0.006(3) C2 0.039(3) 0.051(4) 0.034(3) 0.005(3) 0.008(3) 0.008(3) C3 0.044(5) 0.043(4) 0.052(4) 0.010(3) 0.004(4) 0.007(4) C3' 0.044(5) 0.043(4) 0.052(4) 0.010(3) 0.004(4) 0.007(4) C4 0.052(7) 0.044(6) 0.043(6) 0.019(5) -0.002(5) 0.003(4) C4' 0.052(7) 0.044(6) 0.043(6) 0.019(5) -0.002(5) 0.003(4) C5 0.039(10) 0.118(14) 0.046(9) 0.048(10) 0.005(6) 0.020(10) C5' 0.039(10) 0.118(14) 0.046(9) 0.048(10) 0.005(6) 0.020(10) C6 0.036(3) 0.038(3) 0.040(3) 0.006(3) 0.004(3) 0.000(3) C7 0.052(4) 0.045(4) 0.057(4) -0.002(3) -0.010(3) 0.005(3) C8 0.081(6) 0.056(5) 0.073(5) -0.012(4) -0.026(4) 0.005(4) C9 0.051(4) 0.069(5) 0.079(5) 0.005(4) -0.020(4) 0.000(4) C10 0.041(4) 0.087(6) 0.067(5) 0.018(4) 0.002(4) 0.019(4) C11 0.049(4) 0.065(4) 0.052(4) -0.001(3) 0.008(3) 0.014(4) C12 0.037(3) 0.052(4) 0.027(3) 0.009(3) 0.006(3) 0.010(3) C13 0.056(4) 0.055(4) 0.040(4) 0.010(3) 0.002(3) 0.008(3) C14 0.051(4) 0.065(5) 0.062(5) 0.025(4) -0.002(4) -0.003(4) C15 0.057(5) 0.094(6) 0.062(5) 0.034(5) 0.021(4) 0.007(4) C16 0.065(5) 0.086(6) 0.050(4) 0.012(4) 0.028(4) 0.015(4) C17 0.051(4) 0.056(4) 0.037(3) 0.005(3) 0.011(3) 0.004(3) C18 0.078(5) 0.061(4) 0.050(4) 0.008(3) 0.015(4) -0.009(4) C19 0.070(5) 0.046(4) 0.070(5) 0.005(4) -0.006(4) -0.019(4) C20 0.039(4) 0.099(6) 0.130(7) 0.056(6) 0.028(4) 0.006(4) C21 0.032(3) 0.061(4) 0.063(4) 0.017(4) 0.006(3) -0.001(3) C22 0.058(4) 0.052(4) 0.051(4) 0.001(3) 0.009(3) 0.017(3) C23 0.040(3) 0.044(3) 0.042(4) 0.004(3) -0.003(3) 0.002(3) C24 0.058(4) 0.022(3) 0.031(3) 0.007(2) 0.006(3) 0.005(3) C25 0.049(4) 0.032(3) 0.036(3) 0.003(3) -0.006(3) -0.001(3) C26 0.057(4) 0.039(3) 0.038(4) 0.000(3) -0.016(3) -0.009(3) C27 0.061(4) 0.055(4) 0.038(4) -0.019(3) 0.008(3) -0.015(3) C28 0.064(4) 0.045(4) 0.032(3) -0.002(3) 0.005(3) 0.004(3) C29 0.052(4) 0.035(3) 0.025(3) 0.002(2) 0.002(3) 0.001(3) C30 0.041(4) 0.036(3) 0.062(4) -0.004(3) 0.000(3) 0.000(3) C31 0.046(4) 0.054(4) 0.075(5) -0.006(4) 0.020(4) 0.000(3) C32 0.042(4) 0.068(5) 0.113(7) -0.018(5) -0.017(4) 0.004(4) C33 0.052(4) 0.039(3) 0.046(4) -0.010(3) 0.011(3) -0.006(3) C34 0.052(4) 0.064(5) 0.067(5) -0.005(4) -0.008(4) -0.002(4) C35 0.082(5) 0.082(5) 0.079(6) 0.005(4) 0.039(5) -0.024(5) C36 0.050(4) 0.035(3) 0.051(4) -0.001(3) -0.001(3) 0.000(3) C37 0.049(4) 0.037(3) 0.040(4) 0.003(3) -0.002(3) -0.009(3) C38 0.084(5) 0.055(4) 0.031(4) -0.014(3) -0.003(3) -0.005(4) C39 0.071(5) 0.052(4) 0.030(3) 0.002(3) -0.005(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 N5 2.347(5) . ? Pr1 N4 2.429(4) . ? Pr1 N2 2.451(4) . ? Pr1 N1 2.547(4) . ? Pr1 O2 2.566(3) . ? Pr1 O1 2.601(4) . ? Pr1 N3 2.614(4) . ? Pr1 C1 2.879(5) . ? Pr1 C2 2.921(5) . ? Pr1 H5 2.57(5) . ? Si1 N1 1.729(4) . ? Si1 C19 1.864(6) . ? Si1 C18 1.867(6) . ? Si1 C20 1.868(6) . ? Si2 N3 1.724(4) . ? Si2 C21 1.858(6) . ? Si2 C22 1.874(6) . ? Si2 C23 1.876(5) . ? O1 C36 1.414(6) . ? O1 C38 1.447(6) . ? O2 C37 1.433(6) . ? O2 C39 1.444(6) . ? N1 C1 1.342(7) . ? N2 C1 1.322(6) . ? N2 C3 1.461(15) . ? N2 C3' 1.469(16) . ? N3 C2 1.333(6) . ? N4 C2 1.311(7) . ? N4 C5 1.473(16) . ? N4 C5' 1.476(16) . ? N5 C24 1.384(7) . ? N5 H5 0.868(10) . ? C1 C6 1.504(7) . ? C2 C12 1.529(7) . ? C3 C4 1.515(19) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3' C4' 1.518(19) . ? C3' H3'1 0.9800 . ? C3' H3'2 0.9800 . ? C4 C5 1.501(19) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4' C5' 1.500(18) . ? C4' H4'1 0.9800 . ? C4' H4'2 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5' H5'1 0.9800 . ? C5' H5'2 0.9800 . ? C6 C7 1.371(8) . ? C6 C11 1.379(7) . ? C7 C8 1.383(8) . ? C7 H7 0.9400 . ? C8 C9 1.365(9) . ? C8 H8 0.9400 . ? C9 C10 1.369(9) . ? C9 H9 0.9400 . ? C10 C11 1.400(8) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C17 1.374(7) . ? C12 C13 1.379(8) . ? C13 C14 1.392(8) . ? C13 H13 0.9400 . ? C14 C15 1.386(9) . ? C14 H14 0.9400 . ? C15 C16 1.383(10) . ? C15 H15 0.9400 . ? C16 C17 1.377(8) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.430(7) . ? C24 C29 1.431(7) . ? C25 C26 1.394(7) . ? C25 C30 1.520(8) . ? C26 C27 1.398(8) . ? C26 H26 0.9400 . ? C27 C28 1.363(8) . ? C27 H27 0.9400 . ? C28 C29 1.390(7) . ? C28 H28 0.9400 . ? C29 C33 1.519(8) . ? C30 C31 1.526(8) . ? C30 C32 1.540(8) . ? C30 H30 0.9900 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.524(8) . ? C33 C35 1.532(8) . ? C33 H33 0.9900 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 C37 1.498(7) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Pr1 N4 105.29(19) . . ? N5 Pr1 N2 105.07(16) . . ? N4 Pr1 N2 71.13(15) . . ? N5 Pr1 N1 121.47(15) . . ? N4 Pr1 N1 113.51(16) . . ? N2 Pr1 N1 53.90(14) . . ? N5 Pr1 O2 85.60(14) . . ? N4 Pr1 O2 137.43(15) . . ? N2 Pr1 O2 146.53(13) . . ? N1 Pr1 O2 93.29(13) . . ? N5 Pr1 O1 143.75(14) . . ? N4 Pr1 O1 91.15(17) . . ? N2 Pr1 O1 110.82(14) . . ? N1 Pr1 O1 78.10(13) . . ? O2 Pr1 O1 61.55(11) . . ? N5 Pr1 N3 86.68(15) . . ? N4 Pr1 N3 53.12(14) . . ? N2 Pr1 N3 124.02(14) . . ? N1 Pr1 N3 151.84(14) . . ? O2 Pr1 N3 87.61(12) . . ? O1 Pr1 N3 77.66(12) . . ? N5 Pr1 C1 121.35(15) . . ? N4 Pr1 C1 88.74(16) . . ? N2 Pr1 C1 27.24(14) . . ? N1 Pr1 C1 27.78(14) . . ? O2 Pr1 C1 120.93(14) . . ? O1 Pr1 C1 90.46(14) . . ? N3 Pr1 C1 139.08(14) . . ? N5 Pr1 C2 93.57(16) . . ? N4 Pr1 C2 26.37(15) . . ? N2 Pr1 C2 96.88(15) . . ? N1 Pr1 C2 137.49(15) . . ? O2 Pr1 C2 114.31(14) . . ? O1 Pr1 C2 87.17(14) . . ? N3 Pr1 C2 27.15(13) . . ? C1 Pr1 C2 114.82(16) . . ? N5 Pr1 H5 19.6(5) . . ? N4 Pr1 H5 92.4(9) . . ? N2 Pr1 H5 115.5(10) . . ? N1 Pr1 H5 141.1(5) . . ? O2 Pr1 H5 85.0(11) . . ? O1 Pr1 H5 132.1(9) . . ? N3 Pr1 H5 67.0(5) . . ? C1 Pr1 H5 137.3(9) . . ? C2 Pr1 H5 76.0(7) . . ? N1 Si1 C19 112.1(3) . . ? N1 Si1 C18 106.3(3) . . ? C19 Si1 C18 108.8(3) . . ? N1 Si1 C20 115.5(3) . . ? C19 Si1 C20 107.6(4) . . ? C18 Si1 C20 106.2(3) . . ? N3 Si2 C21 115.6(2) . . ? N3 Si2 C22 112.3(3) . . ? C21 Si2 C22 107.3(3) . . ? N3 Si2 C23 106.4(2) . . ? C21 Si2 C23 106.5(3) . . ? C22 Si2 C23 108.4(3) . . ? C36 O1 C38 112.9(4) . . ? C36 O1 Pr1 116.9(3) . . ? C38 O1 Pr1 114.4(3) . . ? C37 O2 C39 111.2(4) . . ? C37 O2 Pr1 122.6(3) . . ? C39 O2 Pr1 124.4(3) . . ? C1 N1 Si1 128.3(4) . . ? C1 N1 Pr1 90.0(3) . . ? Si1 N1 Pr1 138.7(2) . . ? C1 N2 C3 121.9(15) . . ? C1 N2 C3' 118.8(16) . . ? C3 N2 C3' 5.8(16) . . ? C1 N2 Pr1 94.7(3) . . ? C3 N2 Pr1 134.9(9) . . ? C3' N2 Pr1 140.4(10) . . ? C2 N3 Si2 127.4(4) . . ? C2 N3 Pr1 89.4(3) . . ? Si2 N3 Pr1 142.4(2) . . ? C2 N4 C5 125.1(11) . . ? C2 N4 C5' 117.1(10) . . ? C5 N4 C5' 21.4(19) . . ? C2 N4 Pr1 98.3(3) . . ? C5 N4 Pr1 136.4(11) . . ? C5' N4 Pr1 135.1(11) . . ? C24 N5 Pr1 153.6(4) . . ? C24 N5 H5 111(3) . . ? Pr1 N5 H5 95(3) . . ? N2 C1 N1 116.6(5) . . ? N2 C1 C6 121.6(5) . . ? N1 C1 C6 121.7(5) . . ? N2 C1 Pr1 58.1(3) . . ? N1 C1 Pr1 62.2(3) . . ? C6 C1 Pr1 159.2(4) . . ? N4 C2 N3 117.5(5) . . ? N4 C2 C12 120.6(5) . . ? N3 C2 C12 121.8(5) . . ? N4 C2 Pr1 55.4(3) . . ? N3 C2 Pr1 63.5(3) . . ? C12 C2 Pr1 166.8(4) . . ? N2 C3 C4 114.9(16) . . ? N2 C3 H3A 108.5 . . ? C4 C3 H3A 108.5 . . ? N2 C3 H3B 108.5 . . ? C4 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? N2 C3' C4' 108.8(15) . . ? N2 C3' H3'1 109.9 . . ? C4' C3' H3'1 109.9 . . ? N2 C3' H3'2 109.9 . . ? C4' C3' H3'2 109.9 . . ? H3'1 C3' H3'2 108.3 . . ? C5 C4 C3 110.4(19) . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C5' C4' C3' 121(2) . . ? C5' C4' H4'1 107.2 . . ? C3' C4' H4'1 107.2 . . ? C5' C4' H4'2 107.2 . . ? C3' C4' H4'2 107.2 . . ? H4'1 C4' H4'2 106.8 . . ? N4 C5 C4 104.5(15) . . ? N4 C5 H5A 110.9 . . ? C4 C5 H5A 110.9 . . ? N4 C5 H5B 110.9 . . ? C4 C5 H5B 110.9 . . ? H5A C5 H5B 108.9 . . ? N4 C5' C4' 112.0(16) . . ? N4 C5' H5'1 109.2 . . ? C4' C5' H5'1 109.2 . . ? N4 C5' H5'2 109.2 . . ? C4' C5' H5'2 109.2 . . ? H5'1 C5' H5'2 107.9 . . ? C7 C6 C11 118.9(6) . . ? C7 C6 C1 119.1(5) . . ? C11 C6 C1 122.0(5) . . ? C6 C7 C8 121.1(6) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 119.8(7) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 120.3(7) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 119.8(7) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C6 C11 C10 120.0(6) . . ? C6 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C17 C12 C13 120.2(5) . . ? C17 C12 C2 120.0(5) . . ? C13 C12 C2 119.8(5) . . ? C12 C13 C14 120.4(6) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 119.4(7) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C16 C15 C14 119.4(6) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 121.0(7) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C12 C17 C16 119.6(6) . . ? C12 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 C25 122.6(5) . . ? N5 C24 C29 119.1(5) . . ? C25 C24 C29 118.3(5) . . ? C26 C25 C24 118.7(5) . . ? C26 C25 C30 121.3(5) . . ? C24 C25 C30 119.9(5) . . ? C25 C26 C27 122.9(6) . . ? C25 C26 H26 118.5 . . ? C27 C26 H26 118.5 . . ? C28 C27 C26 117.3(5) . . ? C28 C27 H27 121.3 . . ? C26 C27 H27 121.3 . . ? C27 C28 C29 123.7(6) . . ? C27 C28 H28 118.2 . . ? C29 C28 H28 118.2 . . ? C28 C29 C24 119.0(5) . . ? C28 C29 C33 120.4(5) . . ? C24 C29 C33 120.5(5) . . ? C25 C30 C31 111.2(5) . . ? C25 C30 C32 114.2(5) . . ? C31 C30 C32 108.9(5) . . ? C25 C30 H30 107.4 . . ? C31 C30 H30 107.4 . . ? C32 C30 H30 107.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C34 110.8(5) . . ? C29 C33 C35 113.8(5) . . ? C34 C33 C35 109.2(5) . . ? C29 C33 H33 107.6 . . ? C34 C33 H33 107.6 . . ? C35 C33 H33 107.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O1 C36 C37 108.7(5) . . ? O1 C36 H36A 110.0 . . ? C37 C36 H36A 110.0 . . ? O1 C36 H36B 110.0 . . ? C37 C36 H36B 110.0 . . ? H36A C36 H36B 108.3 . . ? O2 C37 C36 107.2(4) . . ? O2 C37 H37A 110.3 . . ? C36 C37 H37A 110.3 . . ? O2 C37 H37B 110.3 . . ? C36 C37 H37B 110.3 . . ? H37A C37 H37B 108.5 . . ? O1 C38 H38A 109.5 . . ? O1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O2 C39 H39A 109.5 . . ? O2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Pr1 O1 C36 3.2(5) . . . . ? N4 Pr1 O1 C36 121.5(4) . . . . ? N2 Pr1 O1 C36 -168.3(3) . . . . ? N1 Pr1 O1 C36 -124.7(4) . . . . ? O2 Pr1 O1 C36 -24.3(3) . . . . ? N3 Pr1 O1 C36 69.7(4) . . . . ? C1 Pr1 O1 C36 -149.8(4) . . . . ? C2 Pr1 O1 C36 95.4(4) . . . . ? N5 Pr1 O1 C38 -132.0(4) . . . . ? N4 Pr1 O1 C38 -13.7(4) . . . . ? N2 Pr1 O1 C38 56.5(4) . . . . ? N1 Pr1 O1 C38 100.1(4) . . . . ? O2 Pr1 O1 C38 -159.5(4) . . . . ? N3 Pr1 O1 C38 -65.5(4) . . . . ? C1 Pr1 O1 C38 75.1(4) . . . . ? C2 Pr1 O1 C38 -39.8(4) . . . . ? N5 Pr1 O2 C37 -170.2(4) . . . . ? N4 Pr1 O2 C37 -62.3(5) . . . . ? N2 Pr1 O2 C37 78.9(4) . . . . ? N1 Pr1 O2 C37 68.5(4) . . . . ? O1 Pr1 O2 C37 -6.1(4) . . . . ? N3 Pr1 O2 C37 -83.3(4) . . . . ? C1 Pr1 O2 C37 65.6(4) . . . . ? C2 Pr1 O2 C37 -78.3(4) . . . . ? N5 Pr1 O2 C39 26.6(4) . . . . ? N4 Pr1 O2 C39 134.5(4) . . . . ? N2 Pr1 O2 C39 -84.3(5) . . . . ? N1 Pr1 O2 C39 -94.8(4) . . . . ? O1 Pr1 O2 C39 -169.3(4) . . . . ? N3 Pr1 O2 C39 113.4(4) . . . . ? C1 Pr1 O2 C39 -97.6(4) . . . . ? C2 Pr1 O2 C39 118.5(4) . . . . ? C19 Si1 N1 C1 85.5(5) . . . . ? C18 Si1 N1 C1 -155.8(5) . . . . ? C20 Si1 N1 C1 -38.3(6) . . . . ? C19 Si1 N1 Pr1 -68.2(4) . . . . ? C18 Si1 N1 Pr1 50.5(4) . . . . ? C20 Si1 N1 Pr1 168.0(4) . . . . ? N5 Pr1 N1 C1 98.4(3) . . . . ? N4 Pr1 N1 C1 -28.7(4) . . . . ? N2 Pr1 N1 C1 12.4(3) . . . . ? O2 Pr1 N1 C1 -174.7(3) . . . . ? O1 Pr1 N1 C1 -114.7(3) . . . . ? N3 Pr1 N1 C1 -83.6(4) . . . . ? C2 Pr1 N1 C1 -42.4(4) . . . . ? N5 Pr1 N1 Si1 -101.9(4) . . . . ? N4 Pr1 N1 Si1 131.0(4) . . . . ? N2 Pr1 N1 Si1 172.0(4) . . . . ? O2 Pr1 N1 Si1 -15.1(4) . . . . ? O1 Pr1 N1 Si1 45.0(4) . . . . ? N3 Pr1 N1 Si1 76.0(5) . . . . ? C1 Pr1 N1 Si1 159.6(6) . . . . ? C2 Pr1 N1 Si1 117.2(4) . . . . ? N5 Pr1 N2 C1 -130.8(3) . . . . ? N4 Pr1 N2 C1 127.8(4) . . . . ? N1 Pr1 N2 C1 -12.6(3) . . . . ? O2 Pr1 N2 C1 -25.6(5) . . . . ? O1 Pr1 N2 C1 44.0(3) . . . . ? N3 Pr1 N2 C1 132.9(3) . . . . ? C2 Pr1 N2 C1 133.6(3) . . . . ? N5 Pr1 N2 C3 83(2) . . . . ? N4 Pr1 N2 C3 -18(2) . . . . ? N1 Pr1 N2 C3 -159(2) . . . . ? O2 Pr1 N2 C3 -172(2) . . . . ? O1 Pr1 N2 C3 -102(2) . . . . ? N3 Pr1 N2 C3 -13(2) . . . . ? C1 Pr1 N2 C3 -146(2) . . . . ? C2 Pr1 N2 C3 -13(2) . . . . ? N5 Pr1 N2 C3' 80(3) . . . . ? N4 Pr1 N2 C3' -21(3) . . . . ? N1 Pr1 N2 C3' -162(3) . . . . ? O2 Pr1 N2 C3' -175(2) . . . . ? O1 Pr1 N2 C3' -105(3) . . . . ? N3 Pr1 N2 C3' -16(3) . . . . ? C1 Pr1 N2 C3' -149(3) . . . . ? C2 Pr1 N2 C3' -15(3) . . . . ? C21 Si2 N3 C2 44.1(6) . . . . ? C22 Si2 N3 C2 -79.5(5) . . . . ? C23 Si2 N3 C2 162.0(5) . . . . ? C21 Si2 N3 Pr1 -122.2(4) . . . . ? C22 Si2 N3 Pr1 114.2(4) . . . . ? C23 Si2 N3 Pr1 -4.2(4) . . . . ? N5 Pr1 N3 C2 -104.5(3) . . . . ? N4 Pr1 N3 C2 7.5(3) . . . . ? N2 Pr1 N3 C2 1.5(4) . . . . ? N1 Pr1 N3 C2 77.3(4) . . . . ? O2 Pr1 N3 C2 169.8(3) . . . . ? O1 Pr1 N3 C2 108.4(3) . . . . ? C1 Pr1 N3 C2 32.3(4) . . . . ? N5 Pr1 N3 Si2 64.7(4) . . . . ? N4 Pr1 N3 Si2 176.6(5) . . . . ? N2 Pr1 N3 Si2 170.6(3) . . . . ? N1 Pr1 N3 Si2 -113.6(4) . . . . ? O2 Pr1 N3 Si2 -21.0(4) . . . . ? O1 Pr1 N3 Si2 -82.4(4) . . . . ? C1 Pr1 N3 Si2 -158.5(3) . . . . ? C2 Pr1 N3 Si2 169.2(6) . . . . ? N5 Pr1 N4 C2 66.0(4) . . . . ? N2 Pr1 N4 C2 167.1(5) . . . . ? N1 Pr1 N4 C2 -158.8(4) . . . . ? O2 Pr1 N4 C2 -34.3(5) . . . . ? O1 Pr1 N4 C2 -81.3(4) . . . . ? N3 Pr1 N4 C2 -7.7(4) . . . . ? C1 Pr1 N4 C2 -171.7(4) . . . . ? N5 Pr1 N4 C5 -107.6(16) . . . . ? N2 Pr1 N4 C5 -6.6(16) . . . . ? N1 Pr1 N4 C5 27.6(16) . . . . ? O2 Pr1 N4 C5 152.0(15) . . . . ? O1 Pr1 N4 C5 105.1(16) . . . . ? N3 Pr1 N4 C5 178.7(16) . . . . ? C1 Pr1 N4 C5 14.7(16) . . . . ? C2 Pr1 N4 C5 -173.6(17) . . . . ? N5 Pr1 N4 C5' -76.8(15) . . . . ? N2 Pr1 N4 C5' 24.2(15) . . . . ? N1 Pr1 N4 C5' 58.4(16) . . . . ? O2 Pr1 N4 C5' -177.2(15) . . . . ? O1 Pr1 N4 C5' 135.9(15) . . . . ? N3 Pr1 N4 C5' -150.5(16) . . . . ? C1 Pr1 N4 C5' 45.4(15) . . . . ? C2 Pr1 N4 C5' -142.9(17) . . . . ? N4 Pr1 N5 C24 133.0(8) . . . . ? N2 Pr1 N5 C24 58.9(8) . . . . ? N1 Pr1 N5 C24 2.3(9) . . . . ? O2 Pr1 N5 C24 -88.9(8) . . . . ? O1 Pr1 N5 C24 -112.9(8) . . . . ? N3 Pr1 N5 C24 -176.8(8) . . . . ? C1 Pr1 N5 C24 34.9(9) . . . . ? C2 Pr1 N5 C24 157.0(8) . . . . ? C3 N2 C1 N1 174.3(15) . . . . ? C3' N2 C1 N1 180.0(13) . . . . ? Pr1 N2 C1 N1 22.1(5) . . . . ? C3 N2 C1 C6 -3.2(16) . . . . ? C3' N2 C1 C6 2.5(15) . . . . ? Pr1 N2 C1 C6 -155.5(4) . . . . ? C3 N2 C1 Pr1 152.3(15) . . . . ? C3' N2 C1 Pr1 158.0(14) . . . . ? Si1 N1 C1 N2 175.9(4) . . . . ? Pr1 N1 C1 N2 -21.1(5) . . . . ? Si1 N1 C1 C6 -6.6(8) . . . . ? Pr1 N1 C1 C6 156.4(4) . . . . ? Si1 N1 C1 Pr1 -163.0(5) . . . . ? N5 Pr1 C1 N2 58.8(4) . . . . ? N4 Pr1 C1 N2 -48.4(3) . . . . ? N1 Pr1 C1 N2 157.7(5) . . . . ? O2 Pr1 C1 N2 163.9(3) . . . . ? O1 Pr1 C1 N2 -139.5(3) . . . . ? N3 Pr1 C1 N2 -68.0(4) . . . . ? C2 Pr1 C1 N2 -52.4(4) . . . . ? N5 Pr1 C1 N1 -98.9(3) . . . . ? N4 Pr1 C1 N1 153.9(3) . . . . ? N2 Pr1 C1 N1 -157.7(5) . . . . ? O2 Pr1 C1 N1 6.2(3) . . . . ? O1 Pr1 C1 N1 62.8(3) . . . . ? N3 Pr1 C1 N1 134.3(3) . . . . ? C2 Pr1 C1 N1 149.9(3) . . . . ? N5 Pr1 C1 C6 154.3(10) . . . . ? N4 Pr1 C1 C6 47.1(11) . . . . ? N2 Pr1 C1 C6 95.5(12) . . . . ? N1 Pr1 C1 C6 -106.8(12) . . . . ? O2 Pr1 C1 C6 -100.6(11) . . . . ? O1 Pr1 C1 C6 -44.0(11) . . . . ? N3 Pr1 C1 C6 27.5(12) . . . . ? C2 Pr1 C1 C6 43.1(11) . . . . ? C5 N4 C2 N3 -171.7(13) . . . . ? C5' N4 C2 N3 165.1(14) . . . . ? Pr1 N4 C2 N3 13.7(6) . . . . ? C5 N4 C2 C12 9.7(15) . . . . ? C5' N4 C2 C12 -13.6(15) . . . . ? Pr1 N4 C2 C12 -165.0(5) . . . . ? C5 N4 C2 Pr1 174.6(14) . . . . ? C5' N4 C2 Pr1 151.4(14) . . . . ? Si2 N3 C2 N4 175.8(5) . . . . ? Pr1 N3 C2 N4 -12.6(6) . . . . ? Si2 N3 C2 C12 -5.6(8) . . . . ? Pr1 N3 C2 C12 166.1(5) . . . . ? Si2 N3 C2 Pr1 -171.7(5) . . . . ? N5 Pr1 C2 N4 -118.0(4) . . . . ? N2 Pr1 C2 N4 -12.3(4) . . . . ? N1 Pr1 C2 N4 29.4(5) . . . . ? O2 Pr1 C2 N4 155.3(4) . . . . ? O1 Pr1 C2 N4 98.3(4) . . . . ? N3 Pr1 C2 N4 166.4(6) . . . . ? C1 Pr1 C2 N4 9.1(5) . . . . ? N5 Pr1 C2 N3 75.6(3) . . . . ? N4 Pr1 C2 N3 -166.4(6) . . . . ? N2 Pr1 C2 N3 -178.8(3) . . . . ? N1 Pr1 C2 N3 -137.1(3) . . . . ? O2 Pr1 C2 N3 -11.2(4) . . . . ? O1 Pr1 C2 N3 -68.1(3) . . . . ? C1 Pr1 C2 N3 -157.3(3) . . . . ? N5 Pr1 C2 C12 -41.2(17) . . . . ? N4 Pr1 C2 C12 76.7(17) . . . . ? N2 Pr1 C2 C12 64.4(17) . . . . ? N1 Pr1 C2 C12 106.1(17) . . . . ? O2 Pr1 C2 C12 -128.0(16) . . . . ? O1 Pr1 C2 C12 175.1(17) . . . . ? N3 Pr1 C2 C12 -116.8(18) . . . . ? C1 Pr1 C2 C12 85.9(17) . . . . ? C1 N2 C3 C4 -144.3(19) . . . . ? C3' N2 C3 C4 157(36) . . . . ? Pr1 N2 C3 C4 -5(4) . . . . ? C1 N2 C3' C4' -105(2) . . . . ? C3 N2 C3' C4' 19(31) . . . . ? Pr1 N2 C3' C4' 39(4) . . . . ? N2 C3 C4 C5 62(3) . . . . ? N2 C3' C4' C5' -57(3) . . . . ? C2 N4 C5 C4 -122.0(14) . . . . ? C5' N4 C5 C4 -48(4) . . . . ? Pr1 N4 C5 C4 50(2) . . . . ? C3 C4 C5 N4 -80(2) . . . . ? C2 N4 C5' C4' 173.7(13) . . . . ? C5 N4 C5' C4' 56(4) . . . . ? Pr1 N4 C5' C4' -48(3) . . . . ? C3' C4' C5' N4 63(3) . . . . ? N2 C1 C6 C7 96.2(7) . . . . ? N1 C1 C6 C7 -81.2(7) . . . . ? Pr1 C1 C6 C7 13.7(14) . . . . ? N2 C1 C6 C11 -82.6(7) . . . . ? N1 C1 C6 C11 100.0(7) . . . . ? Pr1 C1 C6 C11 -165.0(9) . . . . ? C11 C6 C7 C8 -0.8(9) . . . . ? C1 C6 C7 C8 -179.6(6) . . . . ? C6 C7 C8 C9 -0.6(11) . . . . ? C7 C8 C9 C10 0.9(11) . . . . ? C8 C9 C10 C11 0.3(11) . . . . ? C7 C6 C11 C10 1.9(9) . . . . ? C1 C6 C11 C10 -179.3(6) . . . . ? C9 C10 C11 C6 -1.7(10) . . . . ? N4 C2 C12 C17 -98.9(7) . . . . ? N3 C2 C12 C17 82.5(7) . . . . ? Pr1 C2 C12 C17 -167.5(14) . . . . ? N4 C2 C12 C13 81.8(8) . . . . ? N3 C2 C12 C13 -96.8(7) . . . . ? Pr1 C2 C12 C13 13(2) . . . . ? C17 C12 C13 C14 -2.3(9) . . . . ? C2 C12 C13 C14 177.0(5) . . . . ? C12 C13 C14 C15 1.4(9) . . . . ? C13 C14 C15 C16 0.0(10) . . . . ? C14 C15 C16 C17 -0.5(11) . . . . ? C13 C12 C17 C16 1.8(9) . . . . ? C2 C12 C17 C16 -177.5(6) . . . . ? C15 C16 C17 C12 -0.4(10) . . . . ? Pr1 N5 C24 C25 180.0(6) . . . . ? Pr1 N5 C24 C29 0.1(11) . . . . ? N5 C24 C25 C26 179.8(5) . . . . ? C29 C24 C25 C26 -0.3(8) . . . . ? N5 C24 C25 C30 1.7(8) . . . . ? C29 C24 C25 C30 -178.4(5) . . . . ? C24 C25 C26 C27 -1.6(8) . . . . ? C30 C25 C26 C27 176.5(6) . . . . ? C25 C26 C27 C28 2.2(9) . . . . ? C26 C27 C28 C29 -1.0(9) . . . . ? C27 C28 C29 C24 -0.8(9) . . . . ? C27 C28 C29 C33 -177.7(6) . . . . ? N5 C24 C29 C28 -178.7(5) . . . . ? C25 C24 C29 C28 1.5(8) . . . . ? N5 C24 C29 C33 -1.8(8) . . . . ? C25 C24 C29 C33 178.3(5) . . . . ? C26 C25 C30 C31 -105.4(6) . . . . ? C24 C25 C30 C31 72.7(7) . . . . ? C26 C25 C30 C32 18.3(8) . . . . ? C24 C25 C30 C32 -163.6(5) . . . . ? C28 C29 C33 C34 84.9(6) . . . . ? C24 C29 C33 C34 -91.9(6) . . . . ? C28 C29 C33 C35 -38.6(8) . . . . ? C24 C29 C33 C35 144.5(6) . . . . ? C38 O1 C36 C37 -174.1(5) . . . . ? Pr1 O1 C36 C37 50.1(5) . . . . ? C39 O2 C37 C36 -162.7(5) . . . . ? Pr1 O2 C37 C36 32.1(6) . . . . ? O1 C36 C37 O2 -50.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.507 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.083 # Attachment '- shelxl 3.cif' data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 862444' #TrackingRef '- shelxl 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H62 N5 Nd O2 Si2' _chemical_formula_sum 'C39 H62 N5 Nd O2 Si2' _chemical_formula_weight 833.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 48.267(8) _cell_length_b 9.0251(13) _cell_length_c 19.805(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.408(5) _cell_angle_gamma 90.00 _cell_volume 8573(2) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 18425 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.7 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3480 _exptl_absorpt_coefficient_mu 1.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.410 _exptl_absorpt_correction_T_max 0.771 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20771 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -58 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7902 _reflns_number_gt 6234 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+72.9663P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7902 _refine_ls_number_parameters 468 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.1857 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.869016(9) 0.49121(4) 0.68975(2) 0.03213(16) Uani 1 1 d . A . Si1 Si 0.79518(5) 0.3140(3) 0.71938(15) 0.0502(7) Uani 1 1 d . . . Si2 Si 0.94917(5) 0.3669(2) 0.66434(12) 0.0386(5) Uani 1 1 d . A . O1 O 0.86380(12) 0.2187(6) 0.6502(3) 0.0441(14) Uani 1 1 d . . . O2 O 0.88239(12) 0.2889(6) 0.7775(3) 0.0392(13) Uani 1 1 d . . . N1 N 0.81724(14) 0.4456(7) 0.6913(3) 0.0399(16) Uani 1 1 d . . . N2 N 0.83178(14) 0.6419(7) 0.6330(4) 0.0425(17) Uani 1 1 d D . . N3 N 0.91646(14) 0.4421(7) 0.6428(3) 0.0389(16) Uani 1 1 d . . . N4 N 0.88152(16) 0.5613(11) 0.5795(4) 0.064(2) Uani 1 1 d D . . N5 N 0.89357(15) 0.6524(8) 0.7675(4) 0.0420(17) Uani 1 1 d D . . H5 H 0.9088(8) 0.639(8) 0.749(3) 0.02(2) Uiso 1 1 d D . . C1 C 0.81159(17) 0.5453(9) 0.6421(5) 0.042(2) Uani 1 1 d . A . C2 C 0.90807(18) 0.5288(10) 0.5887(4) 0.046(2) Uani 1 1 d . A . C3 C 0.8292(7) 0.746(4) 0.5763(18) 0.046(3) Uani 0.50 1 d PD A 1 H3A H 0.8212 0.8386 0.5913 0.055 Uiso 0.50 1 calc PR A 1 H3B H 0.8160 0.7051 0.5397 0.055 Uiso 0.50 1 calc PR A 1 C3' C 0.8267(8) 0.755(4) 0.5804(16) 0.046(3) Uani 0.50 1 d PD A 2 H3'1 H 0.8334 0.8512 0.5978 0.055 Uiso 0.50 1 calc PR A 2 H3'2 H 0.8067 0.7622 0.5653 0.055 Uiso 0.50 1 calc PR A 2 C4 C 0.8560(4) 0.7809(19) 0.5480(10) 0.047(3) Uani 0.50 1 d PD A 1 H4A H 0.8693 0.8239 0.5837 0.057 Uiso 0.50 1 calc PR A 1 H4B H 0.8525 0.8539 0.5114 0.057 Uiso 0.50 1 calc PR A 1 C4' C 0.8422(4) 0.7079(19) 0.5225(10) 0.047(3) Uani 0.50 1 d PD A 2 H4'1 H 0.8390 0.7857 0.4879 0.057 Uiso 0.50 1 calc PR A 2 H4'2 H 0.8328 0.6191 0.5030 0.057 Uiso 0.50 1 calc PR A 2 C5 C 0.8681(8) 0.642(4) 0.5210(13) 0.080(8) Uani 0.50 1 d PD A 1 H5A H 0.8534 0.5822 0.4964 0.096 Uiso 0.50 1 calc PR A 1 H5B H 0.8818 0.6677 0.4898 0.096 Uiso 0.50 1 calc PR A 1 C5' C 0.8729(6) 0.674(4) 0.5288(16) 0.080(8) Uani 0.50 1 d PD A 2 H5'1 H 0.8779 0.6412 0.4846 0.096 Uiso 0.50 1 calc PR A 2 H5'2 H 0.8833 0.7657 0.5408 0.096 Uiso 0.50 1 calc PR A 2 C6 C 0.78507(17) 0.5431(9) 0.5952(5) 0.043(2) Uani 1 1 d . . . C7 C 0.7821(2) 0.4457(10) 0.5413(5) 0.059(3) Uani 1 1 d . A . H7 H 0.7969 0.3817 0.5347 0.071 Uiso 1 1 calc R . . C8 C 0.7579(2) 0.4395(12) 0.4967(6) 0.073(3) Uani 1 1 d . . . H8 H 0.7569 0.3734 0.4598 0.087 Uiso 1 1 calc R A . C9 C 0.7361(2) 0.5254(12) 0.5050(6) 0.071(3) Uani 1 1 d . A . H9 H 0.7196 0.5176 0.4754 0.085 Uiso 1 1 calc R . . C10 C 0.73826(19) 0.6269(13) 0.5583(5) 0.063(3) Uani 1 1 d . . . H10 H 0.7231 0.6890 0.5644 0.076 Uiso 1 1 calc R A . C11 C 0.7631(2) 0.6373(12) 0.6034(5) 0.061(3) Uani 1 1 d . A . H11 H 0.7646 0.7075 0.6387 0.073 Uiso 1 1 calc R . . C12 C 0.92846(18) 0.5831(9) 0.5422(4) 0.040(2) Uani 1 1 d . . . C13 C 0.9397(2) 0.7233(11) 0.5511(5) 0.053(2) Uani 1 1 d . A . H13 H 0.9342 0.7852 0.5853 0.064 Uiso 1 1 calc R . . C14 C 0.9594(2) 0.7738(12) 0.5091(5) 0.063(3) Uani 1 1 d . . . H14 H 0.9673 0.8686 0.5159 0.075 Uiso 1 1 calc R A . C15 C 0.9672(2) 0.6839(14) 0.4574(6) 0.072(3) Uani 1 1 d . A . H15 H 0.9802 0.7167 0.4288 0.086 Uiso 1 1 calc R . . C16 C 0.9553(2) 0.5448(14) 0.4494(5) 0.073(3) Uani 1 1 d . . . H16 H 0.9607 0.4821 0.4153 0.087 Uiso 1 1 calc R A . C17 C 0.93607(19) 0.4958(10) 0.4893(5) 0.048(2) Uani 1 1 d . A . H17 H 0.9278 0.4022 0.4811 0.058 Uiso 1 1 calc R . . C18 C 0.8083(2) 0.2723(11) 0.8095(5) 0.066(3) Uani 1 1 d . . . H18A H 0.8283 0.2598 0.8137 0.099 Uiso 1 1 calc R . . H18B H 0.7997 0.1818 0.8235 0.099 Uiso 1 1 calc R . . H18C H 0.8036 0.3535 0.8382 0.099 Uiso 1 1 calc R . . C19 C 0.7955(2) 0.1379(11) 0.6682(6) 0.069(3) Uani 1 1 d . . . H19A H 0.7877 0.1571 0.6218 0.103 Uiso 1 1 calc R . . H19B H 0.7845 0.0629 0.6879 0.103 Uiso 1 1 calc R . . H19C H 0.8145 0.1031 0.6685 0.103 Uiso 1 1 calc R . . C20 C 0.7583(2) 0.3730(17) 0.7189(8) 0.105(5) Uani 1 1 d . . . H20A H 0.7576 0.4705 0.7393 0.157 Uiso 1 1 calc R . . H20B H 0.7485 0.3027 0.7448 0.157 Uiso 1 1 calc R . . H20C H 0.7494 0.3765 0.6725 0.157 Uiso 1 1 calc R . . C21 C 0.97899(18) 0.4953(10) 0.6570(5) 0.053(2) Uani 1 1 d . . . H21A H 0.9791 0.5249 0.6100 0.079 Uiso 1 1 calc R A . H21B H 0.9963 0.4453 0.6725 0.079 Uiso 1 1 calc R . . H21C H 0.9770 0.5823 0.6848 0.079 Uiso 1 1 calc R . . C22 C 0.9556(2) 0.1972(10) 0.6136(5) 0.058(3) Uani 1 1 d . . . H22A H 0.9408 0.1259 0.6173 0.087 Uiso 1 1 calc R A . H22B H 0.9734 0.1537 0.6310 0.087 Uiso 1 1 calc R . . H22C H 0.9560 0.2243 0.5663 0.087 Uiso 1 1 calc R . . C23 C 0.95052(18) 0.3107(9) 0.7542(4) 0.048(2) Uani 1 1 d . . . H23A H 0.9512 0.3983 0.7828 0.071 Uiso 1 1 calc R A . H23B H 0.9670 0.2510 0.7665 0.071 Uiso 1 1 calc R . . H23C H 0.9340 0.2533 0.7607 0.071 Uiso 1 1 calc R . . C24 C 0.89579(18) 0.7481(8) 0.8221(4) 0.0379(19) Uani 1 1 d . A . C25 C 0.92162(18) 0.8183(8) 0.8461(4) 0.041(2) Uani 1 1 d . . . C26 C 0.9217(2) 0.9153(9) 0.9024(5) 0.051(2) Uani 1 1 d . A . H26 H 0.9386 0.9597 0.9195 0.062 Uiso 1 1 calc R . . C27 C 0.89792(19) 0.9485(11) 0.9339(5) 0.053(2) Uani 1 1 d . . . H27 H 0.8983 1.0171 0.9697 0.063 Uiso 1 1 calc R A . C28 C 0.8745(2) 0.8770(10) 0.9100(5) 0.054(2) Uani 1 1 d . A . H28 H 0.8586 0.8957 0.9318 0.065 Uiso 1 1 calc R . . C29 C 0.87176(19) 0.7781(9) 0.8562(4) 0.044(2) Uani 1 1 d . . . C30 C 0.94734(17) 0.7926(9) 0.8114(5) 0.047(2) Uani 1 1 d . A . H30 H 0.9482 0.6853 0.8015 0.056 Uiso 1 1 calc R . . C31 C 0.9450(2) 0.8742(10) 0.7434(5) 0.058(3) Uani 1 1 d . . . H31A H 0.9281 0.8432 0.7157 0.087 Uiso 1 1 calc R A . H31B H 0.9611 0.8511 0.7200 0.087 Uiso 1 1 calc R . . H31C H 0.9443 0.9801 0.7513 0.087 Uiso 1 1 calc R . . C32 C 0.9747(2) 0.8349(12) 0.8536(7) 0.078(4) Uani 1 1 d . . . H32A H 0.9758 0.9418 0.8579 0.117 Uiso 1 1 calc R A . H32B H 0.9903 0.7990 0.8313 0.117 Uiso 1 1 calc R . . H32C H 0.9753 0.7907 0.8984 0.117 Uiso 1 1 calc R . . C33 C 0.84370(18) 0.7108(10) 0.8316(5) 0.047(2) Uani 1 1 d . A . H33 H 0.8473 0.6180 0.8075 0.056 Uiso 1 1 calc R . . C34 C 0.8268(2) 0.8127(11) 0.7801(5) 0.058(3) Uani 1 1 d . . . H34A H 0.8207 0.8993 0.8033 0.087 Uiso 1 1 calc R A . H34B H 0.8107 0.7596 0.7587 0.087 Uiso 1 1 calc R . . H34C H 0.8384 0.8435 0.7457 0.087 Uiso 1 1 calc R . . C35 C 0.8260(3) 0.6701(14) 0.8885(6) 0.084(4) Uani 1 1 d . . . H35A H 0.8370 0.6103 0.9222 0.126 Uiso 1 1 calc R A . H35B H 0.8098 0.6144 0.8696 0.126 Uiso 1 1 calc R . . H35C H 0.8201 0.7598 0.9096 0.126 Uiso 1 1 calc R . . C36 C 0.8811(2) 0.1145(9) 0.6894(5) 0.052(2) Uani 1 1 d . . . H36A H 0.9006 0.1299 0.6820 0.063 Uiso 1 1 calc R . . H36B H 0.8758 0.0135 0.6751 0.063 Uiso 1 1 calc R . . C37 C 0.87790(19) 0.1332(9) 0.7625(5) 0.048(2) Uani 1 1 d . . . H37A H 0.8592 0.1032 0.7717 0.057 Uiso 1 1 calc R . . H37B H 0.8916 0.0726 0.7903 0.057 Uiso 1 1 calc R . . C38 C 0.8626(2) 0.1939(10) 0.5785(5) 0.059(3) Uani 1 1 d . . . H38A H 0.8813 0.1994 0.5649 0.089 Uiso 1 1 calc R . . H38B H 0.8510 0.2689 0.5545 0.089 Uiso 1 1 calc R . . H38C H 0.8549 0.0966 0.5676 0.089 Uiso 1 1 calc R . . C39 C 0.8881(2) 0.3160(10) 0.8503(4) 0.057(3) Uani 1 1 d . . . H39A H 0.8730 0.2770 0.8733 0.086 Uiso 1 1 calc R . . H39B H 0.8899 0.4217 0.8585 0.086 Uiso 1 1 calc R . . H39C H 0.9054 0.2672 0.8675 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0365(3) 0.0299(2) 0.0300(3) 0.00160(18) 0.00348(18) -0.00135(18) Si1 0.0418(14) 0.0473(14) 0.0631(18) 0.0130(13) 0.0132(12) -0.0027(11) Si2 0.0411(13) 0.0344(12) 0.0406(13) 0.0038(10) 0.0053(10) 0.0027(10) O1 0.056(4) 0.034(3) 0.042(3) -0.007(3) 0.005(3) -0.001(3) O2 0.056(4) 0.028(3) 0.031(3) 0.003(2) -0.003(3) -0.002(3) N1 0.045(4) 0.033(3) 0.042(4) 0.010(3) 0.005(3) 0.007(3) N2 0.041(4) 0.033(4) 0.053(5) 0.006(3) 0.006(3) 0.002(3) N3 0.039(4) 0.037(4) 0.042(4) 0.009(3) 0.011(3) 0.006(3) N4 0.049(5) 0.102(7) 0.044(5) 0.023(5) 0.016(4) 0.020(5) N5 0.044(4) 0.037(4) 0.046(4) -0.009(3) 0.012(4) -0.007(3) C1 0.039(5) 0.034(4) 0.054(6) 0.004(4) 0.014(4) 0.007(4) C2 0.046(5) 0.060(6) 0.032(5) 0.012(4) 0.011(4) 0.007(4) C3 0.042(6) 0.039(5) 0.058(7) 0.019(5) 0.011(5) 0.012(5) C3' 0.042(6) 0.039(5) 0.058(7) 0.019(5) 0.011(5) 0.012(5) C4 0.040(8) 0.034(7) 0.065(9) 0.027(7) -0.008(7) 0.000(5) C4' 0.040(8) 0.034(7) 0.065(9) 0.027(7) -0.008(7) 0.000(5) C5 0.056(12) 0.132(17) 0.051(9) 0.034(10) 0.006(7) 0.021(11) C5' 0.056(12) 0.132(17) 0.051(9) 0.034(10) 0.006(7) 0.021(11) C6 0.037(5) 0.039(4) 0.053(6) 0.008(4) 0.005(4) 0.005(4) C7 0.063(6) 0.041(5) 0.068(7) -0.007(5) -0.013(5) 0.001(5) C8 0.087(8) 0.048(6) 0.075(8) -0.014(6) -0.030(7) -0.005(6) C9 0.062(7) 0.060(7) 0.083(9) 0.009(6) -0.021(6) 0.001(6) C10 0.041(5) 0.077(7) 0.071(7) 0.029(6) 0.004(5) 0.025(5) C11 0.061(6) 0.062(6) 0.059(6) 0.004(5) 0.005(5) 0.012(5) C12 0.046(5) 0.043(5) 0.031(4) 0.009(4) -0.002(4) 0.007(4) C13 0.059(6) 0.053(6) 0.049(6) 0.010(5) 0.015(5) 0.010(5) C14 0.059(6) 0.062(6) 0.065(7) 0.020(6) -0.004(5) -0.001(5) C15 0.056(7) 0.089(9) 0.076(8) 0.032(7) 0.036(6) 0.004(6) C16 0.081(8) 0.094(9) 0.049(6) 0.017(6) 0.031(6) 0.034(7) C17 0.056(6) 0.052(5) 0.039(5) 0.009(4) 0.010(4) 0.012(4) C18 0.089(8) 0.055(6) 0.057(7) 0.013(5) 0.018(6) 0.001(6) C19 0.058(6) 0.057(6) 0.089(8) 0.016(6) 0.003(6) -0.016(5) C20 0.049(7) 0.124(12) 0.144(13) 0.058(10) 0.025(7) -0.003(7) C21 0.038(5) 0.053(6) 0.065(7) 0.013(5) -0.005(4) -0.003(4) C22 0.066(7) 0.043(5) 0.067(7) 0.003(5) 0.014(5) 0.011(5) C23 0.050(5) 0.037(5) 0.053(6) 0.015(4) -0.009(4) 0.008(4) C24 0.060(6) 0.019(4) 0.034(5) 0.001(3) 0.002(4) 0.000(4) C25 0.052(5) 0.026(4) 0.042(5) -0.001(4) -0.007(4) -0.007(4) C26 0.074(7) 0.032(4) 0.045(5) -0.006(4) -0.008(5) -0.013(4) C27 0.047(5) 0.055(6) 0.055(6) -0.012(5) 0.005(5) -0.027(5) C28 0.080(7) 0.041(5) 0.043(5) -0.003(4) 0.011(5) 0.005(5) C29 0.059(6) 0.028(4) 0.044(5) -0.002(4) 0.004(4) -0.005(4) C30 0.039(5) 0.028(4) 0.072(7) -0.006(4) -0.001(4) -0.004(4) C31 0.061(6) 0.040(5) 0.077(7) -0.013(5) 0.024(5) -0.005(5) C32 0.048(6) 0.063(7) 0.118(10) -0.030(7) -0.014(6) -0.007(5) C33 0.050(5) 0.038(5) 0.054(6) -0.002(4) 0.011(4) 0.001(4) C34 0.059(6) 0.050(6) 0.063(7) -0.004(5) -0.002(5) 0.001(5) C35 0.090(9) 0.082(8) 0.086(9) 0.014(7) 0.032(7) -0.006(7) C36 0.065(6) 0.032(4) 0.060(6) -0.002(4) 0.008(5) -0.004(4) C37 0.052(5) 0.031(4) 0.057(6) 0.010(4) -0.005(5) -0.004(4) C38 0.088(8) 0.042(5) 0.044(6) -0.012(4) -0.008(5) -0.007(5) C39 0.083(7) 0.044(5) 0.040(5) 0.006(4) -0.014(5) -0.023(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N5 2.342(7) . ? Nd1 N4 2.413(7) . ? Nd1 N2 2.427(6) . ? Nd1 N1 2.536(7) . ? Nd1 O2 2.554(5) . ? Nd1 O1 2.584(5) . ? Nd1 N3 2.604(7) . ? Nd1 C1 2.868(8) . ? Nd1 C2 2.919(8) . ? Nd1 H5 2.51(6) . ? Si1 N1 1.728(7) . ? Si1 C20 1.860(11) . ? Si1 C18 1.863(10) . ? Si1 C19 1.886(11) . ? Si2 N3 1.728(7) . ? Si2 C23 1.845(9) . ? Si2 C21 1.866(9) . ? Si2 C22 1.876(9) . ? O1 C36 1.428(10) . ? O1 C38 1.433(10) . ? O2 C37 1.448(9) . ? O2 C39 1.458(10) . ? N1 C1 1.332(10) . ? N2 C1 1.335(10) . ? N2 C3' 1.457(17) . ? N2 C3 1.459(16) . ? N3 C2 1.352(10) . ? N4 C2 1.307(11) . ? N4 C5' 1.460(18) . ? N4 C5 1.460(18) . ? N5 C24 1.379(10) . ? N5 H5 0.870(10) . ? C1 C6 1.496(12) . ? C2 C12 1.502(12) . ? C3 C4 1.50(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3' C4' 1.50(2) . ? C3' H3'1 0.9800 . ? C3' H3'2 0.9800 . ? C4 C5 1.50(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4' C5' 1.50(2) . ? C4' H4'1 0.9800 . ? C4' H4'2 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5' H5'1 0.9800 . ? C5' H5'2 0.9800 . ? C6 C7 1.377(13) . ? C6 C11 1.384(12) . ? C7 C8 1.385(13) . ? C7 H7 0.9400 . ? C8 C9 1.332(15) . ? C8 H8 0.9400 . ? C9 C10 1.393(15) . ? C9 H9 0.9400 . ? C10 C11 1.415(13) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C13 1.380(12) . ? C12 C17 1.393(12) . ? C13 C14 1.407(13) . ? C13 H13 0.9400 . ? C14 C15 1.391(15) . ? C14 H14 0.9400 . ? C15 C16 1.382(16) . ? C15 H15 0.9400 . ? C16 C17 1.359(14) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C29 1.431(12) . ? C24 C25 1.431(11) . ? C25 C26 1.417(12) . ? C25 C30 1.503(12) . ? C26 C27 1.398(13) . ? C26 H26 0.9400 . ? C27 C28 1.339(12) . ? C27 H27 0.9400 . ? C28 C29 1.385(12) . ? C28 H28 0.9400 . ? C29 C33 1.514(12) . ? C30 C31 1.528(13) . ? C30 C32 1.529(12) . ? C30 H30 0.9900 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C35 1.530(13) . ? C33 C34 1.538(12) . ? C33 H33 0.9900 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 C37 1.481(12) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Nd1 N4 105.8(3) . . ? N5 Nd1 N2 104.5(2) . . ? N4 Nd1 N2 71.4(2) . . ? N5 Nd1 N1 121.3(2) . . ? N4 Nd1 N1 113.6(2) . . ? N2 Nd1 N1 54.3(2) . . ? N5 Nd1 O2 85.7(2) . . ? N4 Nd1 O2 137.2(2) . . ? N2 Nd1 O2 146.5(2) . . ? N1 Nd1 O2 92.89(19) . . ? N5 Nd1 O1 144.6(2) . . ? N4 Nd1 O1 90.1(3) . . ? N2 Nd1 O1 110.5(2) . . ? N1 Nd1 O1 77.7(2) . . ? O2 Nd1 O1 62.25(17) . . ? N5 Nd1 N3 86.6(2) . . ? N4 Nd1 N3 53.3(2) . . ? N2 Nd1 N3 124.4(2) . . ? N1 Nd1 N3 152.1(2) . . ? O2 Nd1 N3 87.46(19) . . ? O1 Nd1 N3 77.9(2) . . ? N5 Nd1 C1 120.7(2) . . ? N4 Nd1 C1 89.3(3) . . ? N2 Nd1 C1 27.6(2) . . ? N1 Nd1 C1 27.7(2) . . ? O2 Nd1 C1 120.5(2) . . ? O1 Nd1 C1 90.2(2) . . ? N3 Nd1 C1 140.1(2) . . ? N5 Nd1 C2 93.5(3) . . ? N4 Nd1 C2 26.3(2) . . ? N2 Nd1 C2 96.8(2) . . ? N1 Nd1 C2 137.7(2) . . ? O2 Nd1 C2 114.6(2) . . ? O1 Nd1 C2 87.2(2) . . ? N3 Nd1 C2 27.6(2) . . ? C1 Nd1 C2 115.4(2) . . ? N5 Nd1 H5 20.2(6) . . ? N4 Nd1 H5 91.5(12) . . ? N2 Nd1 H5 114.0(15) . . ? N1 Nd1 H5 141.5(7) . . ? O2 Nd1 H5 86.6(16) . . ? O1 Nd1 H5 133.5(13) . . ? N3 Nd1 H5 66.4(7) . . ? C1 Nd1 H5 136.3(12) . . ? C2 Nd1 H5 74.8(9) . . ? N1 Si1 C20 115.2(5) . . ? N1 Si1 C18 107.0(4) . . ? C20 Si1 C18 106.5(6) . . ? N1 Si1 C19 111.4(4) . . ? C20 Si1 C19 107.7(6) . . ? C18 Si1 C19 108.8(5) . . ? N3 Si2 C23 106.2(4) . . ? N3 Si2 C21 115.4(4) . . ? C23 Si2 C21 107.5(4) . . ? N3 Si2 C22 112.9(4) . . ? C23 Si2 C22 107.6(4) . . ? C21 Si2 C22 106.8(5) . . ? C36 O1 C38 113.1(7) . . ? C36 O1 Nd1 115.5(5) . . ? C38 O1 Nd1 116.1(5) . . ? C37 O2 C39 112.0(6) . . ? C37 O2 Nd1 122.2(5) . . ? C39 O2 Nd1 124.0(5) . . ? C1 N1 Si1 128.1(6) . . ? C1 N1 Nd1 90.2(5) . . ? Si1 N1 Nd1 139.3(3) . . ? C1 N2 C3' 119.1(19) . . ? C1 N2 C3 121.6(18) . . ? C3' N2 C3 7(2) . . ? C1 N2 Nd1 94.9(5) . . ? C3' N2 Nd1 141.1(13) . . ? C3 N2 Nd1 135.4(11) . . ? C2 N3 Si2 127.4(6) . . ? C2 N3 Nd1 89.2(5) . . ? Si2 N3 Nd1 142.6(4) . . ? C2 N4 C5' 116.9(13) . . ? C2 N4 C5 124.2(16) . . ? C5' N4 C5 15(3) . . ? C2 N4 Nd1 99.0(5) . . ? C5' N4 Nd1 136.5(13) . . ? C5 N4 Nd1 135.8(14) . . ? C24 N5 Nd1 153.4(6) . . ? C24 N5 H5 116(5) . . ? Nd1 N5 H5 91(5) . . ? N1 C1 N2 116.5(8) . . ? N1 C1 C6 122.5(7) . . ? N2 C1 C6 120.8(7) . . ? N1 C1 Nd1 62.2(4) . . ? N2 C1 Nd1 57.5(4) . . ? C6 C1 Nd1 158.6(6) . . ? N4 C2 N3 116.2(8) . . ? N4 C2 C12 122.8(8) . . ? N3 C2 C12 121.0(7) . . ? N4 C2 Nd1 54.8(4) . . ? N3 C2 Nd1 63.2(4) . . ? C12 C2 Nd1 167.2(6) . . ? N2 C3 C4 114.8(19) . . ? N2 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? N2 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.5 . . ? N2 C3' C4' 107.1(18) . . ? N2 C3' H3'1 110.3 . . ? C4' C3' H3'1 110.3 . . ? N2 C3' H3'2 110.3 . . ? C4' C3' H3'2 110.3 . . ? H3'1 C3' H3'2 108.6 . . ? C3 C4 C5 110(2) . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C3' C4' C5' 124(2) . . ? C3' C4' H4'1 106.2 . . ? C5' C4' H4'1 106.2 . . ? C3' C4' H4'2 106.2 . . ? C5' C4' H4'2 106.2 . . ? H4'1 C4' H4'2 106.4 . . ? N4 C5 C4 106.9(18) . . ? N4 C5 H5A 110.3 . . ? C4 C5 H5A 110.3 . . ? N4 C5 H5B 110.3 . . ? C4 C5 H5B 110.3 . . ? H5A C5 H5B 108.6 . . ? N4 C5' C4' 114(2) . . ? N4 C5' H5'1 108.8 . . ? C4' C5' H5'1 108.8 . . ? N4 C5' H5'2 108.8 . . ? C4' C5' H5'2 108.8 . . ? H5'1 C5' H5'2 107.7 . . ? C7 C6 C11 118.0(9) . . ? C7 C6 C1 119.8(8) . . ? C11 C6 C1 122.3(9) . . ? C6 C7 C8 121.8(10) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? C9 C8 C7 121.3(10) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 118.9(10) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C9 C10 C11 120.5(9) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C6 C11 C10 119.4(10) . . ? C6 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C13 C12 C17 118.7(9) . . ? C13 C12 C2 119.8(8) . . ? C17 C12 C2 121.5(8) . . ? C12 C13 C14 120.3(9) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 120.2(10) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 118.1(10) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? C17 C16 C15 122.1(11) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C16 C17 C12 120.5(10) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 C29 119.5(7) . . ? N5 C24 C25 121.7(8) . . ? C29 C24 C25 118.8(7) . . ? C26 C25 C24 117.4(8) . . ? C26 C25 C30 121.7(8) . . ? C24 C25 C30 120.9(7) . . ? C27 C26 C25 123.6(9) . . ? C27 C26 H26 118.2 . . ? C25 C26 H26 118.2 . . ? C28 C27 C26 116.1(9) . . ? C28 C27 H27 121.9 . . ? C26 C27 H27 121.9 . . ? C27 C28 C29 126.0(10) . . ? C27 C28 H28 117.0 . . ? C29 C28 H28 117.0 . . ? C28 C29 C24 118.1(8) . . ? C28 C29 C33 120.8(9) . . ? C24 C29 C33 121.0(7) . . ? C25 C30 C31 110.2(7) . . ? C25 C30 C32 114.7(8) . . ? C31 C30 C32 109.6(8) . . ? C25 C30 H30 107.3 . . ? C31 C30 H30 107.3 . . ? C32 C30 H30 107.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C35 114.3(8) . . ? C29 C33 C34 111.2(7) . . ? C35 C33 C34 109.6(8) . . ? C29 C33 H33 107.1 . . ? C35 C33 H33 107.1 . . ? C34 C33 H33 107.1 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O1 C36 C37 109.8(7) . . ? O1 C36 H36A 109.7 . . ? C37 C36 H36A 109.7 . . ? O1 C36 H36B 109.7 . . ? C37 C36 H36B 109.7 . . ? H36A C36 H36B 108.2 . . ? O2 C37 C36 106.4(7) . . ? O2 C37 H37A 110.5 . . ? C36 C37 H37A 110.4 . . ? O2 C37 H37B 110.4 . . ? C36 C37 H37B 110.5 . . ? H37A C37 H37B 108.6 . . ? O1 C38 H38A 109.5 . . ? O1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O2 C39 H39A 109.5 . . ? O2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Nd1 O1 C36 3.5(8) . . . . ? N4 Nd1 O1 C36 121.7(6) . . . . ? N2 Nd1 O1 C36 -168.2(6) . . . . ? N1 Nd1 O1 C36 -124.2(6) . . . . ? O2 Nd1 O1 C36 -24.2(5) . . . . ? N3 Nd1 O1 C36 69.4(6) . . . . ? C1 Nd1 O1 C36 -149.0(6) . . . . ? C2 Nd1 O1 C36 95.6(6) . . . . ? N5 Nd1 O1 C38 -132.4(6) . . . . ? N4 Nd1 O1 C38 -14.2(6) . . . . ? N2 Nd1 O1 C38 55.9(6) . . . . ? N1 Nd1 O1 C38 99.9(6) . . . . ? O2 Nd1 O1 C38 -160.1(6) . . . . ? N3 Nd1 O1 C38 -66.5(6) . . . . ? C1 Nd1 O1 C38 75.1(6) . . . . ? C2 Nd1 O1 C38 -40.3(6) . . . . ? N5 Nd1 O2 C37 -170.1(6) . . . . ? N4 Nd1 O2 C37 -61.3(7) . . . . ? N2 Nd1 O2 C37 79.9(7) . . . . ? N1 Nd1 O2 C37 68.7(6) . . . . ? O1 Nd1 O2 C37 -5.7(6) . . . . ? N3 Nd1 O2 C37 -83.4(6) . . . . ? C1 Nd1 O2 C37 66.6(6) . . . . ? C2 Nd1 O2 C37 -78.2(6) . . . . ? N5 Nd1 O2 C39 26.6(6) . . . . ? N4 Nd1 O2 C39 135.4(7) . . . . ? N2 Nd1 O2 C39 -83.4(7) . . . . ? N1 Nd1 O2 C39 -94.6(6) . . . . ? O1 Nd1 O2 C39 -169.0(7) . . . . ? N3 Nd1 O2 C39 113.4(6) . . . . ? C1 Nd1 O2 C39 -96.7(6) . . . . ? C2 Nd1 O2 C39 118.5(6) . . . . ? C20 Si1 N1 C1 -35.8(10) . . . . ? C18 Si1 N1 C1 -154.0(8) . . . . ? C19 Si1 N1 C1 87.2(8) . . . . ? C20 Si1 N1 Nd1 167.5(7) . . . . ? C18 Si1 N1 Nd1 49.3(7) . . . . ? C19 Si1 N1 Nd1 -69.4(7) . . . . ? N5 Nd1 N1 C1 97.2(5) . . . . ? N4 Nd1 N1 C1 -30.6(6) . . . . ? N2 Nd1 N1 C1 11.6(5) . . . . ? O2 Nd1 N1 C1 -176.0(5) . . . . ? O1 Nd1 N1 C1 -115.2(5) . . . . ? N3 Nd1 N1 C1 -86.0(6) . . . . ? C2 Nd1 N1 C1 -43.5(6) . . . . ? N5 Nd1 N1 Si1 -101.0(6) . . . . ? N4 Nd1 N1 Si1 131.2(6) . . . . ? N2 Nd1 N1 Si1 173.4(7) . . . . ? O2 Nd1 N1 Si1 -14.2(6) . . . . ? O1 Nd1 N1 Si1 46.6(6) . . . . ? N3 Nd1 N1 Si1 75.8(8) . . . . ? C1 Nd1 N1 Si1 161.8(9) . . . . ? C2 Nd1 N1 Si1 118.3(6) . . . . ? N5 Nd1 N2 C1 -129.9(5) . . . . ? N4 Nd1 N2 C1 127.9(6) . . . . ? N1 Nd1 N2 C1 -11.6(5) . . . . ? O2 Nd1 N2 C1 -25.3(7) . . . . ? O1 Nd1 N2 C1 45.1(6) . . . . ? N3 Nd1 N2 C1 134.2(5) . . . . ? C2 Nd1 N2 C1 134.7(5) . . . . ? N5 Nd1 N2 C3' 78(3) . . . . ? N4 Nd1 N2 C3' -24(3) . . . . ? N1 Nd1 N2 C3' -164(3) . . . . ? O2 Nd1 N2 C3' -177(3) . . . . ? O1 Nd1 N2 C3' -107(3) . . . . ? N3 Nd1 N2 C3' -18(3) . . . . ? C1 Nd1 N2 C3' -152(3) . . . . ? C2 Nd1 N2 C3' -17(3) . . . . ? N5 Nd1 N2 C3 83(3) . . . . ? N4 Nd1 N2 C3 -19(3) . . . . ? N1 Nd1 N2 C3 -158(3) . . . . ? O2 Nd1 N2 C3 -172(3) . . . . ? O1 Nd1 N2 C3 -102(3) . . . . ? N3 Nd1 N2 C3 -13(3) . . . . ? C1 Nd1 N2 C3 -147(3) . . . . ? C2 Nd1 N2 C3 -12(3) . . . . ? C23 Si2 N3 C2 163.0(8) . . . . ? C21 Si2 N3 C2 44.0(9) . . . . ? C22 Si2 N3 C2 -79.3(9) . . . . ? C23 Si2 N3 Nd1 -3.9(7) . . . . ? C21 Si2 N3 Nd1 -122.9(6) . . . . ? C22 Si2 N3 Nd1 113.8(6) . . . . ? N5 Nd1 N3 C2 -104.2(5) . . . . ? N4 Nd1 N3 C2 8.4(5) . . . . ? N2 Nd1 N3 C2 1.0(6) . . . . ? N1 Nd1 N3 C2 78.5(7) . . . . ? O2 Nd1 N3 C2 169.9(5) . . . . ? O1 Nd1 N3 C2 107.7(5) . . . . ? C1 Nd1 N3 C2 32.3(7) . . . . ? N5 Nd1 N3 Si2 65.4(6) . . . . ? N4 Nd1 N3 Si2 178.1(8) . . . . ? N2 Nd1 N3 Si2 170.7(5) . . . . ? N1 Nd1 N3 Si2 -111.8(6) . . . . ? O2 Nd1 N3 Si2 -20.5(6) . . . . ? O1 Nd1 N3 Si2 -82.6(6) . . . . ? C1 Nd1 N3 Si2 -158.1(5) . . . . ? C2 Nd1 N3 Si2 169.6(10) . . . . ? N5 Nd1 N4 C2 64.4(7) . . . . ? N2 Nd1 N4 C2 164.7(7) . . . . ? N1 Nd1 N4 C2 -160.1(6) . . . . ? O2 Nd1 N4 C2 -36.7(9) . . . . ? O1 Nd1 N4 C2 -83.6(7) . . . . ? N3 Nd1 N4 C2 -8.8(6) . . . . ? C1 Nd1 N4 C2 -173.8(7) . . . . ? N5 Nd1 N4 C5' -82(3) . . . . ? N2 Nd1 N4 C5' 19(3) . . . . ? N1 Nd1 N4 C5' 54(3) . . . . ? O2 Nd1 N4 C5' 177(3) . . . . ? O1 Nd1 N4 C5' 130(3) . . . . ? N3 Nd1 N4 C5' -155(3) . . . . ? C1 Nd1 N4 C5' 40(3) . . . . ? C2 Nd1 N4 C5' -146(3) . . . . ? N5 Nd1 N4 C5 -104(2) . . . . ? N2 Nd1 N4 C5 -4(2) . . . . ? N1 Nd1 N4 C5 32(2) . . . . ? O2 Nd1 N4 C5 155(2) . . . . ? O1 Nd1 N4 C5 108(2) . . . . ? N3 Nd1 N4 C5 -177(2) . . . . ? C1 Nd1 N4 C5 18(2) . . . . ? C2 Nd1 N4 C5 -168(3) . . . . ? N4 Nd1 N5 C24 133.4(12) . . . . ? N2 Nd1 N5 C24 59.0(13) . . . . ? N1 Nd1 N5 C24 2.2(13) . . . . ? O2 Nd1 N5 C24 -88.6(12) . . . . ? O1 Nd1 N5 C24 -112.9(12) . . . . ? N3 Nd1 N5 C24 -176.3(13) . . . . ? C1 Nd1 N5 C24 34.6(13) . . . . ? C2 Nd1 N5 C24 157.0(12) . . . . ? Si1 N1 C1 N2 175.7(6) . . . . ? Nd1 N1 C1 N2 -19.3(8) . . . . ? Si1 N1 C1 C6 -9.3(12) . . . . ? Nd1 N1 C1 C6 155.7(7) . . . . ? Si1 N1 C1 Nd1 -165.0(8) . . . . ? C3' N2 C1 N1 -179.4(17) . . . . ? C3 N2 C1 N1 173.4(19) . . . . ? Nd1 N2 C1 N1 20.3(8) . . . . ? C3' N2 C1 C6 5.5(19) . . . . ? C3 N2 C1 C6 -2(2) . . . . ? Nd1 N2 C1 C6 -154.9(7) . . . . ? C3' N2 C1 Nd1 160.3(18) . . . . ? C3 N2 C1 Nd1 153.2(19) . . . . ? N5 Nd1 C1 N1 -99.8(5) . . . . ? N4 Nd1 C1 N1 152.2(5) . . . . ? N2 Nd1 C1 N1 -159.5(8) . . . . ? O2 Nd1 C1 N1 4.6(6) . . . . ? O1 Nd1 C1 N1 62.1(5) . . . . ? N3 Nd1 C1 N1 133.2(5) . . . . ? C2 Nd1 C1 N1 149.1(5) . . . . ? N5 Nd1 C1 N2 59.7(6) . . . . ? N4 Nd1 C1 N2 -48.4(6) . . . . ? N1 Nd1 C1 N2 159.5(8) . . . . ? O2 Nd1 C1 N2 164.1(5) . . . . ? O1 Nd1 C1 N2 -138.4(5) . . . . ? N3 Nd1 C1 N2 -67.3(6) . . . . ? C2 Nd1 C1 N2 -51.4(6) . . . . ? N5 Nd1 C1 C6 151.8(15) . . . . ? N4 Nd1 C1 C6 43.7(16) . . . . ? N2 Nd1 C1 C6 92.1(17) . . . . ? N1 Nd1 C1 C6 -108.5(17) . . . . ? O2 Nd1 C1 C6 -103.8(16) . . . . ? O1 Nd1 C1 C6 -46.4(16) . . . . ? N3 Nd1 C1 C6 24.8(17) . . . . ? C2 Nd1 C1 C6 40.7(16) . . . . ? C5' N4 C2 N3 170(2) . . . . ? C5 N4 C2 N3 -174.5(19) . . . . ? Nd1 N4 C2 N3 15.3(10) . . . . ? C5' N4 C2 C12 -10(2) . . . . ? C5 N4 C2 C12 5(2) . . . . ? Nd1 N4 C2 C12 -164.9(8) . . . . ? C5' N4 C2 Nd1 155(2) . . . . ? C5 N4 C2 Nd1 170(2) . . . . ? Si2 N3 C2 N4 173.9(7) . . . . ? Nd1 N3 C2 N4 -14.0(9) . . . . ? Si2 N3 C2 C12 -5.9(13) . . . . ? Nd1 N3 C2 C12 166.2(8) . . . . ? Si2 N3 C2 Nd1 -172.1(8) . . . . ? N5 Nd1 C2 N4 -119.6(7) . . . . ? N2 Nd1 C2 N4 -14.6(7) . . . . ? N1 Nd1 C2 N4 27.6(8) . . . . ? O2 Nd1 C2 N4 153.4(6) . . . . ? O1 Nd1 C2 N4 95.8(7) . . . . ? N3 Nd1 C2 N4 164.6(10) . . . . ? C1 Nd1 C2 N4 6.8(8) . . . . ? N5 Nd1 C2 N3 75.8(5) . . . . ? N4 Nd1 C2 N3 -164.6(10) . . . . ? N2 Nd1 C2 N3 -179.1(5) . . . . ? N1 Nd1 C2 N3 -137.0(5) . . . . ? O2 Nd1 C2 N3 -11.1(6) . . . . ? O1 Nd1 C2 N3 -68.8(5) . . . . ? C1 Nd1 C2 N3 -157.7(5) . . . . ? N5 Nd1 C2 C12 -37(3) . . . . ? N4 Nd1 C2 C12 83(3) . . . . ? N2 Nd1 C2 C12 69(3) . . . . ? N1 Nd1 C2 C12 111(3) . . . . ? O2 Nd1 C2 C12 -123(3) . . . . ? N3 Nd1 C2 C12 -112(3) . . . . ? C1 Nd1 C2 C12 90(3) . . . . ? C1 N2 C3 C4 -146(3) . . . . ? C3' N2 C3 C4 144(38) . . . . ? Nd1 N2 C3 C4 -6(5) . . . . ? C1 N2 C3' C4' -105(2) . . . . ? C3 N2 C3' C4' 9(32) . . . . ? Nd1 N2 C3' C4' 43(5) . . . . ? N2 C3 C4 C5 61(4) . . . . ? N2 C3' C4' C5' -55(4) . . . . ? C2 N4 C5 C4 -119(2) . . . . ? C5' N4 C5 C4 -54(7) . . . . ? Nd1 N4 C5 C4 47(4) . . . . ? C3 C4 C5 N4 -79(3) . . . . ? C2 N4 C5' C4' -179(2) . . . . ? C5 N4 C5' C4' 59(8) . . . . ? Nd1 N4 C5' C4' -37(5) . . . . ? C3' C4' C5' N4 55(4) . . . . ? N1 C1 C6 C7 -79.3(12) . . . . ? N2 C1 C6 C7 95.6(11) . . . . ? Nd1 C1 C6 C7 17(2) . . . . ? N1 C1 C6 C11 101.2(11) . . . . ? N2 C1 C6 C11 -83.9(12) . . . . ? Nd1 C1 C6 C11 -162.7(12) . . . . ? C11 C6 C7 C8 -0.7(15) . . . . ? C1 C6 C7 C8 179.8(9) . . . . ? C6 C7 C8 C9 -1.7(18) . . . . ? C7 C8 C9 C10 2.4(18) . . . . ? C8 C9 C10 C11 -0.8(17) . . . . ? C7 C6 C11 C10 2.2(14) . . . . ? C1 C6 C11 C10 -178.3(9) . . . . ? C9 C10 C11 C6 -1.5(16) . . . . ? N4 C2 C12 C13 82.9(12) . . . . ? N3 C2 C12 C13 -97.4(10) . . . . ? Nd1 C2 C12 C13 8(3) . . . . ? N4 C2 C12 C17 -96.1(12) . . . . ? N3 C2 C12 C17 83.6(11) . . . . ? Nd1 C2 C12 C17 -171(2) . . . . ? C17 C12 C13 C14 -2.7(13) . . . . ? C2 C12 C13 C14 178.3(8) . . . . ? C12 C13 C14 C15 1.3(14) . . . . ? C13 C14 C15 C16 -0.5(16) . . . . ? C14 C15 C16 C17 1.3(17) . . . . ? C15 C16 C17 C12 -2.8(16) . . . . ? C13 C12 C17 C16 3.4(13) . . . . ? C2 C12 C17 C16 -177.6(9) . . . . ? Nd1 N5 C24 C29 0.1(17) . . . . ? Nd1 N5 C24 C25 179.7(9) . . . . ? N5 C24 C25 C26 179.7(7) . . . . ? C29 C24 C25 C26 -0.6(11) . . . . ? N5 C24 C25 C30 1.3(12) . . . . ? C29 C24 C25 C30 -179.0(7) . . . . ? C24 C25 C26 C27 -1.9(13) . . . . ? C30 C25 C26 C27 176.5(9) . . . . ? C25 C26 C27 C28 3.2(14) . . . . ? C26 C27 C28 C29 -2.2(15) . . . . ? C27 C28 C29 C24 -0.2(14) . . . . ? C27 C28 C29 C33 -176.6(9) . . . . ? N5 C24 C29 C28 -178.7(8) . . . . ? C25 C24 C29 C28 1.6(12) . . . . ? N5 C24 C29 C33 -2.3(12) . . . . ? C25 C24 C29 C33 178.0(7) . . . . ? C26 C25 C30 C31 -105.1(9) . . . . ? C24 C25 C30 C31 73.2(9) . . . . ? C26 C25 C30 C32 19.2(12) . . . . ? C24 C25 C30 C32 -162.5(8) . . . . ? C28 C29 C33 C35 -39.1(12) . . . . ? C24 C29 C33 C35 144.6(9) . . . . ? C28 C29 C33 C34 85.6(10) . . . . ? C24 C29 C33 C34 -90.7(10) . . . . ? C38 O1 C36 C37 -171.6(7) . . . . ? Nd1 O1 C36 C37 51.2(8) . . . . ? C39 O2 C37 C36 -162.9(8) . . . . ? Nd1 O2 C37 C36 32.1(9) . . . . ? O1 C36 C37 O2 -51.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.427 _refine_diff_density_min -1.184 _refine_diff_density_rms 0.129 # Attachment '- shelxl 4.cif' data_shelxl4 _database_code_depnum_ccdc_archive 'CCDC 862445' #TrackingRef '- shelxl 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H62 Gd N5 O2 Si2' _chemical_formula_sum 'C39 H62 Gd N5 O2 Si2' _chemical_formula_weight 846.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.7140(18) _cell_length_b 8.9715(5) _cell_length_c 19.8141(13) _cell_angle_alpha 90.00 _cell_angle_beta 103.969(2) _cell_angle_gamma 90.00 _cell_volume 4263.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 16718 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1756 _exptl_absorpt_coefficient_mu 1.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.461 _exptl_absorpt_correction_T_max 0.778 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20979 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7854 _reflns_number_gt 6892 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+24.3924P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7854 _refine_ls_number_parameters 468 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_restrained_S_all 1.196 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.237548(13) 0.74059(3) 0.223581(15) 0.02808(10) Uani 1 1 d . A . Si1 Si 0.09180(8) 0.5635(2) 0.23322(12) 0.0464(5) Uani 1 1 d . . . Si2 Si 0.39750(8) 0.6158(2) 0.22560(10) 0.0374(4) Uani 1 1 d . A . O1 O 0.2286(2) 0.4765(5) 0.1808(2) 0.0419(11) Uani 1 1 d . . . O2 O 0.26298(19) 0.5434(5) 0.3141(2) 0.0366(11) Uani 1 1 d . . . N1 N 0.1360(2) 0.6945(6) 0.2127(3) 0.0352(13) Uani 1 1 d . . . N2 N 0.1641(2) 0.8939(6) 0.1592(3) 0.0367(13) Uani 1 1 d D . . N3 N 0.3327(2) 0.6971(6) 0.1954(3) 0.0341(13) Uani 1 1 d . . . N4 N 0.2625(3) 0.8154(9) 0.1207(3) 0.062(2) Uani 1 1 d D . . N5 N 0.2842(2) 0.9002(6) 0.3071(3) 0.0346(12) Uani 1 1 d D . . H5 H 0.3171(15) 0.883(9) 0.300(4) 0.07(3) Uiso 1 1 d D . . C1 C 0.1248(3) 0.7960(7) 0.1619(3) 0.0332(14) Uani 1 1 d . A . C2 C 0.3162(3) 0.7791(8) 0.1390(3) 0.0397(16) Uani 1 1 d . A . C3 C 0.1589(13) 1.001(4) 0.1026(18) 0.044(2) Uani 0.50 1 d PD A 1 H3A H 0.1452 1.0950 0.1170 0.053 Uiso 0.50 1 calc PR A 1 H3B H 0.1308 0.9637 0.0624 0.053 Uiso 0.50 1 calc PR A 1 C3' C 0.1541(15) 1.003(4) 0.1026(16) 0.044(2) Uani 0.50 1 d PD A 2 H3'1 H 0.1677 1.1012 0.1211 0.053 Uiso 0.50 1 calc PR A 2 H3'2 H 0.1140 1.0114 0.0820 0.053 Uiso 0.50 1 calc PR A 2 C4 C 0.2121(6) 1.0306(17) 0.0802(8) 0.045(3) Uani 0.50 1 d PD A 1 H4A H 0.2047 1.1042 0.0425 0.054 Uiso 0.50 1 calc PR A 1 H4B H 0.2398 1.0731 0.1194 0.054 Uiso 0.50 1 calc PR A 1 C4' C 0.1836(6) 0.9568(18) 0.0475(7) 0.045(3) Uani 0.50 1 d PD A 2 H4'1 H 0.1670 0.8630 0.0270 0.054 Uiso 0.50 1 calc PR A 2 H4'2 H 0.1759 1.0321 0.0106 0.054 Uiso 0.50 1 calc PR A 2 C5 C 0.2354(12) 0.892(3) 0.0557(11) 0.060(7) Uani 0.50 1 d PD A 1 H5A H 0.2057 0.8302 0.0274 0.072 Uiso 0.50 1 calc PR A 1 H5B H 0.2625 0.9161 0.0285 0.072 Uiso 0.50 1 calc PR A 1 C5' C 0.2453(10) 0.936(3) 0.0701(13) 0.060(7) Uani 0.50 1 d PD A 2 H5'1 H 0.2596 0.9146 0.0291 0.072 Uiso 0.50 1 calc PR A 2 H5'2 H 0.2624 1.0291 0.0906 0.072 Uiso 0.50 1 calc PR A 2 C6 C 0.0702(3) 0.7940(8) 0.1069(4) 0.0397(16) Uani 1 1 d . . . C7 C 0.0635(3) 0.6933(8) 0.0524(4) 0.054(2) Uani 1 1 d . A . H7 H 0.0926 0.6271 0.0508 0.064 Uiso 1 1 calc R . . C8 C 0.0151(4) 0.6884(10) 0.0006(5) 0.074(3) Uani 1 1 d . . . H8 H 0.0118 0.6216 -0.0367 0.089 Uiso 1 1 calc R A . C9 C -0.0277(4) 0.7802(12) 0.0037(5) 0.076(3) Uani 1 1 d . A . H9 H -0.0612 0.7744 -0.0309 0.092 Uiso 1 1 calc R . . C10 C -0.0229(3) 0.8823(12) 0.0570(5) 0.069(3) Uani 1 1 d . . . H10 H -0.0529 0.9448 0.0591 0.083 Uiso 1 1 calc R A . C11 C 0.0278(3) 0.8917(10) 0.1084(4) 0.056(2) Uani 1 1 d . A . H11 H 0.0325 0.9646 0.1434 0.067 Uiso 1 1 calc R . . C12 C 0.3555(3) 0.8304(8) 0.0960(3) 0.0388(16) Uani 1 1 d . . . C13 C 0.3654(3) 0.7385(10) 0.0436(3) 0.0486(18) Uani 1 1 d . A . H13 H 0.3478 0.6453 0.0348 0.058 Uiso 1 1 calc R . . C14 C 0.4018(4) 0.7864(12) 0.0047(4) 0.066(3) Uani 1 1 d . . . H14 H 0.4092 0.7246 -0.0303 0.079 Uiso 1 1 calc R A . C15 C 0.4270(4) 0.9230(13) 0.0168(5) 0.069(3) Uani 1 1 d . A . H15 H 0.4516 0.9541 -0.0100 0.083 Uiso 1 1 calc R . . C16 C 0.4166(4) 1.0158(11) 0.0681(5) 0.071(3) Uani 1 1 d . . . H16 H 0.4340 1.1094 0.0764 0.085 Uiso 1 1 calc R A . C17 C 0.3800(3) 0.9686(9) 0.1071(4) 0.055(2) Uani 1 1 d . A . H17 H 0.3721 1.0316 0.1414 0.066 Uiso 1 1 calc R . . C18 C 0.0172(3) 0.6219(11) 0.2214(6) 0.082(3) Uani 1 1 d . . . H18A H 0.0158 0.7212 0.2403 0.123 Uiso 1 1 calc R . . H18B H -0.0016 0.5525 0.2456 0.123 Uiso 1 1 calc R . . H18C H -0.0011 0.6221 0.1723 0.123 Uiso 1 1 calc R . . C19 C 0.0915(4) 0.3875(9) 0.1828(4) 0.064(2) Uani 1 1 d . . . H19A H 0.0854 0.4109 0.1337 0.096 Uiso 1 1 calc R . . H19B H 0.0619 0.3229 0.1899 0.096 Uiso 1 1 calc R . . H19C H 0.1271 0.3375 0.1986 0.096 Uiso 1 1 calc R . . C20 C 0.1175(4) 0.5203(10) 0.3273(4) 0.063(2) Uani 1 1 d . . . H20A H 0.1574 0.5016 0.3378 0.094 Uiso 1 1 calc R . . H20B H 0.0986 0.4325 0.3386 0.094 Uiso 1 1 calc R . . H20C H 0.1101 0.6041 0.3547 0.094 Uiso 1 1 calc R . . C21 C 0.4577(3) 0.7433(9) 0.2269(4) 0.054(2) Uani 1 1 d . . . H21A H 0.4604 0.7623 0.1796 0.082 Uiso 1 1 calc R A . H21B H 0.4919 0.6970 0.2528 0.082 Uiso 1 1 calc R . . H21C H 0.4521 0.8367 0.2489 0.082 Uiso 1 1 calc R . . C22 C 0.4057(3) 0.4463(9) 0.1733(4) 0.0501(19) Uani 1 1 d . . . H22A H 0.3733 0.3825 0.1687 0.075 Uiso 1 1 calc R A . H22B H 0.4389 0.3921 0.1967 0.075 Uiso 1 1 calc R . . H22C H 0.4091 0.4767 0.1275 0.075 Uiso 1 1 calc R . . C23 C 0.4030(3) 0.5613(9) 0.3181(3) 0.0471(18) Uani 1 1 d . . . H23A H 0.4001 0.6496 0.3453 0.071 Uiso 1 1 calc R A . H23B H 0.4386 0.5132 0.3367 0.071 Uiso 1 1 calc R . . H23C H 0.3731 0.4929 0.3203 0.071 Uiso 1 1 calc R . . C24 C 0.2900(3) 0.9964(7) 0.3624(3) 0.0329(14) Uani 1 1 d . A . C25 C 0.3422(3) 1.0647(7) 0.3933(3) 0.0368(15) Uani 1 1 d . . . C26 C 0.3451(3) 1.1631(8) 0.4490(4) 0.0443(17) Uani 1 1 d . A . H26 H 0.3794 1.2089 0.4694 0.053 Uiso 1 1 calc R . . C27 C 0.3000(4) 1.1949(8) 0.4747(4) 0.053(2) Uani 1 1 d . . . H27 H 0.3035 1.2606 0.5125 0.063 Uiso 1 1 calc R A . C28 C 0.2495(4) 1.1306(8) 0.4453(4) 0.0484(19) Uani 1 1 d . A . H28 H 0.2183 1.1547 0.4624 0.058 Uiso 1 1 calc R . . C29 C 0.2436(3) 1.0285(7) 0.3896(3) 0.0362(15) Uani 1 1 d . . . C30 C 0.3928(3) 1.0356(8) 0.3649(4) 0.0449(18) Uani 1 1 d . A . H30 H 0.3933 0.9277 0.3546 0.054 Uiso 1 1 calc R . . C31 C 0.3869(3) 1.1202(9) 0.2953(4) 0.0514(19) Uani 1 1 d . . . H31A H 0.3532 1.0880 0.2624 0.077 Uiso 1 1 calc R A . H31B H 0.4190 1.0992 0.2767 0.077 Uiso 1 1 calc R . . H31C H 0.3849 1.2265 0.3034 0.077 Uiso 1 1 calc R . . C32 C 0.4489(3) 1.0739(11) 0.4149(5) 0.071(3) Uani 1 1 d . . . H32A H 0.4530 1.1813 0.4186 0.106 Uiso 1 1 calc R A . H32B H 0.4790 1.0321 0.3974 0.106 Uiso 1 1 calc R . . H32C H 0.4500 1.0324 0.4605 0.106 Uiso 1 1 calc R . . C33 C 0.1865(3) 0.9625(8) 0.3577(4) 0.0399(16) Uani 1 1 d . A . H33 H 0.1925 0.8698 0.3334 0.048 Uiso 1 1 calc R . . C34 C 0.1523(3) 1.0662(9) 0.3036(4) 0.056(2) Uani 1 1 d . . . H34A H 0.1470 1.1604 0.3252 0.085 Uiso 1 1 calc R A . H34B H 0.1162 1.0213 0.2837 0.085 Uiso 1 1 calc R . . H34C H 0.1716 1.0834 0.2671 0.085 Uiso 1 1 calc R . . C35 C 0.1537(4) 0.9207(11) 0.4107(5) 0.077(3) Uani 1 1 d . . . H35A H 0.1763 0.8570 0.4460 0.116 Uiso 1 1 calc R A . H35B H 0.1200 0.8680 0.3875 0.116 Uiso 1 1 calc R . . H35C H 0.1438 1.0104 0.4322 0.116 Uiso 1 1 calc R . . C36 C 0.2606(3) 0.3670(8) 0.2253(4) 0.0456(18) Uani 1 1 d . . . H36A H 0.2999 0.3750 0.2240 0.055 Uiso 1 1 calc R . . H36B H 0.2475 0.2671 0.2093 0.055 Uiso 1 1 calc R . . C37 C 0.2551(3) 0.3899(7) 0.2975(4) 0.0447(18) Uani 1 1 d . . . H37A H 0.2180 0.3583 0.3015 0.054 Uiso 1 1 calc R . . H37B H 0.2830 0.3304 0.3299 0.054 Uiso 1 1 calc R . . C38 C 0.2256(4) 0.4498(9) 0.1093(4) 0.059(2) Uani 1 1 d . . . H38A H 0.2626 0.4583 0.1009 0.088 Uiso 1 1 calc R . . H38B H 0.2010 0.5224 0.0812 0.088 Uiso 1 1 calc R . . H38C H 0.2112 0.3503 0.0970 0.088 Uiso 1 1 calc R . . C39 C 0.2750(3) 0.5705(9) 0.3885(3) 0.0481(19) Uani 1 1 d . . . H39A H 0.2456 0.5275 0.4072 0.072 Uiso 1 1 calc R . . H39B H 0.2769 0.6770 0.3972 0.072 Uiso 1 1 calc R . . H39C H 0.3104 0.5251 0.4109 0.072 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 Gd1 0.02796(17) 0.03021(17) 0.02532(15) 0.00157(14) 0.00497(11) -0.00054(14) Si1 0.0311(11) 0.0502(12) 0.0593(13) 0.0115(10) 0.0138(9) -0.0016(9) Si2 0.0287(10) 0.0420(11) 0.0404(10) 0.0028(9) 0.0062(8) 0.0058(8) O1 0.047(3) 0.041(3) 0.035(2) -0.005(2) 0.006(2) 0.001(2) O2 0.046(3) 0.032(2) 0.029(2) 0.0029(19) 0.003(2) -0.001(2) N1 0.029(3) 0.038(3) 0.037(3) 0.000(2) 0.005(2) 0.000(2) N2 0.032(3) 0.037(3) 0.040(3) 0.010(3) 0.007(2) 0.004(3) N3 0.030(3) 0.040(3) 0.033(3) 0.007(2) 0.011(2) 0.008(2) N4 0.041(4) 0.105(6) 0.046(4) 0.040(4) 0.021(3) 0.032(4) N5 0.030(3) 0.035(3) 0.038(3) -0.007(2) 0.006(3) -0.004(3) C1 0.029(3) 0.036(4) 0.035(3) -0.002(3) 0.008(3) 0.004(3) C2 0.043(4) 0.045(4) 0.035(3) 0.007(3) 0.016(3) 0.009(3) C3 0.033(5) 0.043(4) 0.056(5) 0.016(4) 0.009(4) 0.009(4) C3' 0.033(5) 0.043(4) 0.056(5) 0.016(4) 0.009(4) 0.009(4) C4 0.051(8) 0.049(7) 0.034(6) 0.014(5) 0.007(5) 0.005(5) C4' 0.051(8) 0.049(7) 0.034(6) 0.014(5) 0.007(5) 0.005(5) C5 0.047(10) 0.101(15) 0.031(9) 0.025(10) 0.005(7) 0.015(10) C5' 0.047(10) 0.101(15) 0.031(9) 0.025(10) 0.005(7) 0.015(10) C6 0.028(4) 0.043(4) 0.045(4) 0.005(3) 0.003(3) 0.001(3) C7 0.047(5) 0.045(4) 0.056(5) -0.005(4) -0.011(4) 0.003(4) C8 0.076(7) 0.053(5) 0.074(6) -0.002(5) -0.020(5) 0.004(5) C9 0.054(6) 0.078(7) 0.081(7) 0.009(6) -0.017(5) -0.009(5) C10 0.034(5) 0.098(7) 0.075(6) 0.027(6) 0.011(4) 0.021(5) C11 0.045(5) 0.073(6) 0.050(5) 0.009(4) 0.010(4) 0.012(4) C12 0.038(4) 0.049(4) 0.033(4) 0.010(3) 0.014(3) 0.007(3) C13 0.048(4) 0.060(5) 0.042(4) 0.008(4) 0.019(3) 0.012(4) C14 0.064(6) 0.096(8) 0.045(5) 0.010(5) 0.029(4) 0.014(5) C15 0.046(5) 0.116(9) 0.051(5) 0.029(6) 0.022(4) 0.001(5) C16 0.064(6) 0.077(6) 0.068(6) 0.029(5) 0.011(5) -0.021(5) C17 0.064(6) 0.055(5) 0.047(5) 0.008(4) 0.014(4) 0.002(4) C18 0.038(5) 0.086(7) 0.128(9) 0.039(7) 0.034(5) 0.001(5) C19 0.067(6) 0.061(5) 0.055(5) 0.005(4) -0.001(4) -0.025(5) C20 0.076(6) 0.062(5) 0.058(5) 0.012(4) 0.030(5) -0.003(5) C21 0.047(4) 0.053(5) 0.063(5) 0.007(4) 0.012(4) -0.014(4) C22 0.041(4) 0.058(5) 0.049(4) 0.001(4) 0.007(3) 0.016(4) C23 0.033(4) 0.062(5) 0.040(4) 0.005(4) -0.005(3) 0.008(4) C24 0.040(4) 0.027(3) 0.030(3) 0.004(3) 0.004(3) 0.000(3) C25 0.041(4) 0.034(4) 0.031(3) 0.007(3) 0.000(3) 0.000(3) C26 0.051(5) 0.040(4) 0.036(4) -0.003(3) -0.001(3) -0.006(3) C27 0.081(6) 0.044(4) 0.029(4) -0.009(3) 0.004(4) -0.007(4) C28 0.067(5) 0.044(4) 0.040(4) -0.002(3) 0.023(4) -0.001(4) C29 0.047(4) 0.030(3) 0.032(3) 0.003(3) 0.008(3) -0.002(3) C30 0.035(4) 0.039(4) 0.053(4) -0.001(3) -0.005(3) -0.005(3) C31 0.047(5) 0.052(5) 0.060(5) 0.000(4) 0.022(4) -0.007(4) C32 0.041(5) 0.089(7) 0.075(6) -0.016(5) 0.000(4) -0.014(5) C33 0.036(4) 0.040(4) 0.044(4) -0.005(3) 0.011(3) 0.000(3) C34 0.045(5) 0.060(5) 0.061(5) -0.003(4) 0.007(4) 0.000(4) C35 0.079(7) 0.077(7) 0.086(7) -0.003(6) 0.039(6) -0.027(6) C36 0.055(5) 0.033(4) 0.043(4) -0.005(3) 0.002(4) 0.000(3) C37 0.058(5) 0.030(4) 0.044(4) 0.000(3) 0.009(4) -0.004(3) C38 0.080(6) 0.058(5) 0.035(4) -0.012(4) 0.009(4) 0.001(5) C39 0.060(5) 0.054(5) 0.026(3) 0.004(3) 0.001(3) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 N5 2.280(5) . ? Gd1 N4 2.364(6) . ? Gd1 N2 2.387(5) . ? Gd1 O2 2.490(4) . ? Gd1 N1 2.502(5) . ? Gd1 O1 2.508(5) . ? Gd1 N3 2.575(5) . ? Gd1 C1 2.804(6) . ? Gd1 C2 2.878(6) . ? Gd1 H5 2.52(8) . ? Si1 N1 1.718(6) . ? Si1 C20 1.860(8) . ? Si1 C19 1.867(9) . ? Si1 C18 1.876(8) . ? Si2 N3 1.729(5) . ? Si2 C23 1.870(7) . ? Si2 C21 1.873(7) . ? Si2 C22 1.878(8) . ? O1 C38 1.420(8) . ? O1 C36 1.427(8) . ? O2 C37 1.418(8) . ? O2 C39 1.452(7) . ? N1 C1 1.336(8) . ? N2 C1 1.320(8) . ? N2 C3 1.456(16) . ? N2 C3' 1.465(16) . ? N3 C2 1.319(8) . ? N4 C2 1.330(9) . ? N4 C5' 1.466(17) . ? N4 C5 1.470(17) . ? N5 C24 1.376(8) . ? N5 H5 0.868(10) . ? C1 C6 1.516(9) . ? C2 C12 1.509(9) . ? C3 C4 1.509(19) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3' C4' 1.511(19) . ? C3' H3'1 0.9800 . ? C3' H3'2 0.9800 . ? C4 C5 1.502(19) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4' C5' 1.495(19) . ? C4' H4'1 0.9800 . ? C4' H4'2 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5' H5'1 0.9800 . ? C5' H5'2 0.9800 . ? C6 C11 1.371(10) . ? C6 C7 1.387(10) . ? C7 C8 1.375(11) . ? C7 H7 0.9400 . ? C8 C9 1.354(13) . ? C8 H8 0.9400 . ? C9 C10 1.381(13) . ? C9 H9 0.9400 . ? C10 C11 1.413(11) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C17 1.375(11) . ? C12 C13 1.393(10) . ? C13 C14 1.386(10) . ? C13 H13 0.9400 . ? C14 C15 1.370(13) . ? C14 H14 0.9400 . ? C15 C16 1.385(13) . ? C15 H15 0.9400 . ? C16 C17 1.389(11) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C29 1.410(9) . ? C24 C25 1.426(9) . ? C25 C26 1.402(9) . ? C25 C30 1.513(10) . ? C26 C27 1.364(11) . ? C26 H26 0.9400 . ? C27 C28 1.370(11) . ? C27 H27 0.9400 . ? C28 C29 1.415(9) . ? C28 H28 0.9400 . ? C29 C33 1.519(9) . ? C30 C32 1.535(10) . ? C30 C31 1.550(10) . ? C30 H30 0.9900 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.514(10) . ? C33 C35 1.520(10) . ? C33 H33 0.9900 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 C37 1.485(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Gd1 N4 104.8(2) . . ? N5 Gd1 N2 102.3(2) . . ? N4 Gd1 N2 72.43(19) . . ? N5 Gd1 O2 85.84(17) . . ? N4 Gd1 O2 138.58(19) . . ? N2 Gd1 O2 145.28(17) . . ? N5 Gd1 N1 119.20(19) . . ? N4 Gd1 N1 115.9(2) . . ? N2 Gd1 N1 55.34(18) . . ? O2 Gd1 N1 91.05(16) . . ? N5 Gd1 O1 145.76(18) . . ? N4 Gd1 O1 89.8(2) . . ? N2 Gd1 O1 111.68(17) . . ? O2 Gd1 O1 63.84(14) . . ? N1 Gd1 O1 79.03(16) . . ? N5 Gd1 N3 85.62(19) . . ? N4 Gd1 N3 54.17(18) . . ? N2 Gd1 N3 126.02(17) . . ? O2 Gd1 N3 87.90(16) . . ? N1 Gd1 N3 155.02(17) . . ? O1 Gd1 N3 78.13(16) . . ? N5 Gd1 C1 118.72(19) . . ? N4 Gd1 C1 90.71(19) . . ? N2 Gd1 C1 28.02(18) . . ? O2 Gd1 C1 119.44(17) . . ? N1 Gd1 C1 28.44(17) . . ? O1 Gd1 C1 91.30(17) . . ? N3 Gd1 C1 142.78(17) . . ? N5 Gd1 C2 93.0(2) . . ? N4 Gd1 C2 27.21(19) . . ? N2 Gd1 C2 98.79(18) . . ? O2 Gd1 C2 114.61(17) . . ? N1 Gd1 C2 140.77(18) . . ? O1 Gd1 C2 86.17(18) . . ? N3 Gd1 C2 27.27(17) . . ? C1 Gd1 C2 117.71(18) . . ? N5 Gd1 H5 20.0(9) . . ? N4 Gd1 H5 92.8(16) . . ? N2 Gd1 H5 114.4(17) . . ? O2 Gd1 H5 84.3(19) . . ? N1 Gd1 H5 139.0(9) . . ? O1 Gd1 H5 132.4(14) . . ? N3 Gd1 H5 65.7(9) . . ? C1 Gd1 H5 136.1(13) . . ? C2 Gd1 H5 75.7(12) . . ? N1 Si1 C20 107.3(3) . . ? N1 Si1 C19 111.8(3) . . ? C20 Si1 C19 108.5(4) . . ? N1 Si1 C18 116.1(4) . . ? C20 Si1 C18 105.7(4) . . ? C19 Si1 C18 107.0(5) . . ? N3 Si2 C23 106.9(3) . . ? N3 Si2 C21 114.4(3) . . ? C23 Si2 C21 106.1(3) . . ? N3 Si2 C22 111.4(3) . . ? C23 Si2 C22 109.7(4) . . ? C21 Si2 C22 108.1(4) . . ? C38 O1 C36 112.8(5) . . ? C38 O1 Gd1 118.4(4) . . ? C36 O1 Gd1 116.8(4) . . ? C37 O2 C39 112.4(5) . . ? C37 O2 Gd1 121.7(4) . . ? C39 O2 Gd1 124.5(4) . . ? C1 N1 Si1 128.1(5) . . ? C1 N1 Gd1 88.4(4) . . ? Si1 N1 Gd1 140.7(3) . . ? C1 N2 C3 122.7(17) . . ? C1 N2 C3' 119.1(18) . . ? C3 N2 C3' 4.7(19) . . ? C1 N2 Gd1 93.9(4) . . ? C3 N2 Gd1 134.9(10) . . ? C3' N2 Gd1 139.6(11) . . ? C2 N3 Si2 126.8(5) . . ? C2 N3 Gd1 89.3(4) . . ? Si2 N3 Gd1 143.8(3) . . ? C2 N4 C5' 118.1(11) . . ? C2 N4 C5 124.5(13) . . ? C5' N4 C5 20(2) . . ? C2 N4 Gd1 98.5(4) . . ? C5' N4 Gd1 135.0(12) . . ? C5 N4 Gd1 136.8(12) . . ? C24 N5 Gd1 155.4(5) . . ? C24 N5 H5 108(6) . . ? Gd1 N5 H5 96(6) . . ? N2 C1 N1 117.7(6) . . ? N2 C1 C6 121.0(6) . . ? N1 C1 C6 121.3(6) . . ? N2 C1 Gd1 58.1(3) . . ? N1 C1 Gd1 63.1(3) . . ? C6 C1 Gd1 158.4(4) . . ? N3 C2 N4 116.9(6) . . ? N3 C2 C12 122.7(6) . . ? N4 C2 C12 120.5(6) . . ? N3 C2 Gd1 63.5(3) . . ? N4 C2 Gd1 54.3(3) . . ? C12 C2 Gd1 169.1(5) . . ? N2 C3 C4 115.0(17) . . ? N2 C3 H3A 108.5 . . ? C4 C3 H3A 108.5 . . ? N2 C3 H3B 108.5 . . ? C4 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? N2 C3' C4' 110.2(16) . . ? N2 C3' H3'1 109.6 . . ? C4' C3' H3'1 109.6 . . ? N2 C3' H3'2 109.6 . . ? C4' C3' H3'2 109.6 . . ? H3'1 C3' H3'2 108.1 . . ? C5 C4 C3 112(2) . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C5' C4' C3' 117(2) . . ? C5' C4' H4'1 108.1 . . ? C3' C4' H4'1 108.1 . . ? C5' C4' H4'2 108.1 . . ? C3' C4' H4'2 108.1 . . ? H4'1 C4' H4'2 107.3 . . ? N4 C5 C4 103.5(15) . . ? N4 C5 H5A 111.1 . . ? C4 C5 H5A 111.1 . . ? N4 C5 H5B 111.1 . . ? C4 C5 H5B 111.1 . . ? H5A C5 H5B 109.0 . . ? N4 C5' C4' 113.8(18) . . ? N4 C5' H5'1 108.8 . . ? C4' C5' H5'1 108.8 . . ? N4 C5' H5'2 108.8 . . ? C4' C5' H5'2 108.8 . . ? H5'1 C5' H5'2 107.7 . . ? C11 C6 C7 119.0(7) . . ? C11 C6 C1 121.9(7) . . ? C7 C6 C1 119.1(6) . . ? C8 C7 C6 121.4(8) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C9 C8 C7 119.7(9) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 120.9(8) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C9 C10 C11 119.2(8) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C6 C11 C10 119.7(8) . . ? C6 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C17 C12 C13 120.1(7) . . ? C17 C12 C2 120.3(7) . . ? C13 C12 C2 119.5(7) . . ? C14 C13 C12 119.1(8) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C15 C14 C13 120.6(8) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.5(8) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 119.1(9) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C12 C17 C16 120.5(8) . . ? C12 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 C29 119.7(6) . . ? N5 C24 C25 121.3(6) . . ? C29 C24 C25 119.0(6) . . ? C26 C25 C24 118.5(7) . . ? C26 C25 C30 120.8(6) . . ? C24 C25 C30 120.7(6) . . ? C27 C26 C25 122.3(7) . . ? C27 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C26 C27 C28 119.7(7) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C29 121.1(7) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C24 C29 C28 119.3(6) . . ? C24 C29 C33 121.4(6) . . ? C28 C29 C33 119.2(6) . . ? C25 C30 C32 114.8(6) . . ? C25 C30 C31 109.7(6) . . ? C32 C30 C31 110.0(6) . . ? C25 C30 H30 107.4 . . ? C32 C30 H30 107.4 . . ? C31 C30 H30 107.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C29 111.0(6) . . ? C34 C33 C35 109.9(7) . . ? C29 C33 C35 113.9(6) . . ? C34 C33 H33 107.2 . . ? C29 C33 H33 107.2 . . ? C35 C33 H33 107.2 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O1 C36 C37 109.5(6) . . ? O1 C36 H36A 109.8 . . ? C37 C36 H36A 109.8 . . ? O1 C36 H36B 109.8 . . ? C37 C36 H36B 109.8 . . ? H36A C36 H36B 108.2 . . ? O2 C37 C36 108.6(6) . . ? O2 C37 H37A 110.0 . . ? C36 C37 H37A 110.0 . . ? O2 C37 H37B 110.0 . . ? C36 C37 H37B 110.0 . . ? H37A C37 H37B 108.4 . . ? O1 C38 H38A 109.5 . . ? O1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O2 C39 H39A 109.5 . . ? O2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Gd1 O1 C38 -132.1(5) . . . . ? N4 Gd1 O1 C38 -15.3(5) . . . . ? N2 Gd1 O1 C38 55.6(5) . . . . ? O2 Gd1 O1 C38 -162.2(6) . . . . ? N1 Gd1 O1 C38 101.2(5) . . . . ? N3 Gd1 O1 C38 -68.6(5) . . . . ? C1 Gd1 O1 C38 75.4(5) . . . . ? C2 Gd1 O1 C38 -42.3(5) . . . . ? N5 Gd1 O1 C36 8.0(6) . . . . ? N4 Gd1 O1 C36 124.8(5) . . . . ? N2 Gd1 O1 C36 -164.3(4) . . . . ? O2 Gd1 O1 C36 -22.1(4) . . . . ? N1 Gd1 O1 C36 -118.7(5) . . . . ? N3 Gd1 O1 C36 71.4(5) . . . . ? C1 Gd1 O1 C36 -144.5(5) . . . . ? C2 Gd1 O1 C36 97.8(5) . . . . ? N5 Gd1 O2 C37 -169.2(5) . . . . ? N4 Gd1 O2 C37 -61.4(6) . . . . ? N2 Gd1 O2 C37 85.1(6) . . . . ? N1 Gd1 O2 C37 71.6(5) . . . . ? O1 Gd1 O2 C37 -5.7(5) . . . . ? N3 Gd1 O2 C37 -83.5(5) . . . . ? C1 Gd1 O2 C37 70.0(5) . . . . ? C2 Gd1 O2 C37 -77.8(5) . . . . ? N5 Gd1 O2 C39 25.1(5) . . . . ? N4 Gd1 O2 C39 132.9(5) . . . . ? N2 Gd1 O2 C39 -80.6(6) . . . . ? N1 Gd1 O2 C39 -94.1(5) . . . . ? O1 Gd1 O2 C39 -171.4(5) . . . . ? N3 Gd1 O2 C39 110.8(5) . . . . ? C1 Gd1 O2 C39 -95.7(5) . . . . ? C2 Gd1 O2 C39 116.5(5) . . . . ? C20 Si1 N1 C1 -153.5(6) . . . . ? C19 Si1 N1 C1 87.7(6) . . . . ? C18 Si1 N1 C1 -35.6(7) . . . . ? C20 Si1 N1 Gd1 51.7(5) . . . . ? C19 Si1 N1 Gd1 -67.1(5) . . . . ? C18 Si1 N1 Gd1 169.6(5) . . . . ? N5 Gd1 N1 C1 97.1(4) . . . . ? N4 Gd1 N1 C1 -29.6(4) . . . . ? N2 Gd1 N1 C1 12.3(3) . . . . ? O2 Gd1 N1 C1 -177.1(4) . . . . ? O1 Gd1 N1 C1 -114.0(4) . . . . ? N3 Gd1 N1 C1 -89.8(5) . . . . ? C2 Gd1 N1 C1 -44.1(5) . . . . ? N5 Gd1 N1 Si1 -102.5(5) . . . . ? N4 Gd1 N1 Si1 130.8(5) . . . . ? N2 Gd1 N1 Si1 172.7(5) . . . . ? O2 Gd1 N1 Si1 -16.6(5) . . . . ? O1 Gd1 N1 Si1 46.4(4) . . . . ? N3 Gd1 N1 Si1 70.6(6) . . . . ? C1 Gd1 N1 Si1 160.4(7) . . . . ? C2 Gd1 N1 Si1 116.3(5) . . . . ? N5 Gd1 N2 C1 -129.6(4) . . . . ? N4 Gd1 N2 C1 128.5(4) . . . . ? O2 Gd1 N2 C1 -29.0(5) . . . . ? N1 Gd1 N2 C1 -12.5(3) . . . . ? O1 Gd1 N2 C1 45.9(4) . . . . ? N3 Gd1 N2 C1 136.8(4) . . . . ? C2 Gd1 N2 C1 135.3(4) . . . . ? N5 Gd1 N2 C3 84(3) . . . . ? N4 Gd1 N2 C3 -18(3) . . . . ? O2 Gd1 N2 C3 -175(3) . . . . ? N1 Gd1 N2 C3 -159(3) . . . . ? O1 Gd1 N2 C3 -100(3) . . . . ? N3 Gd1 N2 C3 -9(3) . . . . ? C1 Gd1 N2 C3 -146(3) . . . . ? C2 Gd1 N2 C3 -11(3) . . . . ? N5 Gd1 N2 C3' 84(3) . . . . ? N4 Gd1 N2 C3' -18(3) . . . . ? O2 Gd1 N2 C3' -175(3) . . . . ? N1 Gd1 N2 C3' -159(3) . . . . ? O1 Gd1 N2 C3' -100(3) . . . . ? N3 Gd1 N2 C3' -9(3) . . . . ? C1 Gd1 N2 C3' -146(3) . . . . ? C2 Gd1 N2 C3' -11(3) . . . . ? C23 Si2 N3 C2 164.3(6) . . . . ? C21 Si2 N3 C2 47.2(7) . . . . ? C22 Si2 N3 C2 -75.8(7) . . . . ? C23 Si2 N3 Gd1 -11.5(6) . . . . ? C21 Si2 N3 Gd1 -128.6(5) . . . . ? C22 Si2 N3 Gd1 108.4(5) . . . . ? N5 Gd1 N3 C2 -105.3(4) . . . . ? N4 Gd1 N3 C2 6.5(4) . . . . ? N2 Gd1 N3 C2 -3.3(5) . . . . ? O2 Gd1 N3 C2 168.7(4) . . . . ? N1 Gd1 N3 C2 80.7(6) . . . . ? O1 Gd1 N3 C2 105.0(4) . . . . ? C1 Gd1 N3 C2 28.8(5) . . . . ? N5 Gd1 N3 Si2 71.3(5) . . . . ? N4 Gd1 N3 Si2 -176.8(6) . . . . ? N2 Gd1 N3 Si2 173.3(4) . . . . ? O2 Gd1 N3 Si2 -14.7(5) . . . . ? N1 Gd1 N3 Si2 -102.6(6) . . . . ? O1 Gd1 N3 Si2 -78.4(5) . . . . ? C1 Gd1 N3 Si2 -154.6(4) . . . . ? C2 Gd1 N3 Si2 176.6(8) . . . . ? N5 Gd1 N4 C2 66.7(5) . . . . ? N2 Gd1 N4 C2 165.1(6) . . . . ? O2 Gd1 N4 C2 -34.1(7) . . . . ? N1 Gd1 N4 C2 -159.7(5) . . . . ? O1 Gd1 N4 C2 -82.0(5) . . . . ? N3 Gd1 N4 C2 -6.5(4) . . . . ? C1 Gd1 N4 C2 -173.3(5) . . . . ? N5 Gd1 N4 C5' -78.6(17) . . . . ? N2 Gd1 N4 C5' 19.9(17) . . . . ? O2 Gd1 N4 C5' -179.4(16) . . . . ? N1 Gd1 N4 C5' 55.0(17) . . . . ? O1 Gd1 N4 C5' 132.7(17) . . . . ? N3 Gd1 N4 C5' -151.8(17) . . . . ? C1 Gd1 N4 C5' 41.4(17) . . . . ? C2 Gd1 N4 C5' -145.3(19) . . . . ? N5 Gd1 N4 C5 -107.6(17) . . . . ? N2 Gd1 N4 C5 -9.2(17) . . . . ? O2 Gd1 N4 C5 151.6(16) . . . . ? N1 Gd1 N4 C5 26.0(18) . . . . ? O1 Gd1 N4 C5 103.7(17) . . . . ? N3 Gd1 N4 C5 179.2(18) . . . . ? C1 Gd1 N4 C5 12.4(17) . . . . ? C2 Gd1 N4 C5 -174.3(19) . . . . ? N4 Gd1 N5 C24 133.7(11) . . . . ? N2 Gd1 N5 C24 58.9(11) . . . . ? O2 Gd1 N5 C24 -86.9(11) . . . . ? N1 Gd1 N5 C24 1.9(12) . . . . ? O1 Gd1 N5 C24 -113.8(11) . . . . ? N3 Gd1 N5 C24 -175.1(11) . . . . ? C1 Gd1 N5 C24 34.5(11) . . . . ? C2 Gd1 N5 C24 158.6(11) . . . . ? C3 N2 C1 N1 174.0(16) . . . . ? C3' N2 C1 N1 177.7(14) . . . . ? Gd1 N2 C1 N1 22.1(6) . . . . ? C3 N2 C1 C6 -2.6(18) . . . . ? C3' N2 C1 C6 1.1(16) . . . . ? Gd1 N2 C1 C6 -154.6(5) . . . . ? C3 N2 C1 Gd1 152.0(17) . . . . ? C3' N2 C1 Gd1 155.7(15) . . . . ? Si1 N1 C1 N2 174.7(5) . . . . ? Gd1 N1 C1 N2 -20.9(6) . . . . ? Si1 N1 C1 C6 -8.6(9) . . . . ? Gd1 N1 C1 C6 155.7(5) . . . . ? Si1 N1 C1 Gd1 -164.3(6) . . . . ? N5 Gd1 C1 N2 59.1(4) . . . . ? N4 Gd1 C1 N2 -48.3(4) . . . . ? O2 Gd1 C1 N2 161.5(4) . . . . ? N1 Gd1 C1 N2 158.1(6) . . . . ? O1 Gd1 C1 N2 -138.1(4) . . . . ? N3 Gd1 C1 N2 -66.2(5) . . . . ? C2 Gd1 C1 N2 -51.7(4) . . . . ? N5 Gd1 C1 N1 -99.0(4) . . . . ? N4 Gd1 C1 N1 153.6(4) . . . . ? N2 Gd1 C1 N1 -158.1(6) . . . . ? O2 Gd1 C1 N1 3.4(4) . . . . ? O1 Gd1 C1 N1 63.8(4) . . . . ? N3 Gd1 C1 N1 135.7(4) . . . . ? C2 Gd1 C1 N1 150.2(3) . . . . ? N5 Gd1 C1 C6 153.4(12) . . . . ? N4 Gd1 C1 C6 46.1(12) . . . . ? N2 Gd1 C1 C6 94.3(13) . . . . ? O2 Gd1 C1 C6 -104.2(12) . . . . ? N1 Gd1 C1 C6 -107.6(13) . . . . ? O1 Gd1 C1 C6 -43.8(12) . . . . ? N3 Gd1 C1 C6 28.2(14) . . . . ? C2 Gd1 C1 C6 42.6(13) . . . . ? Si2 N3 C2 N4 171.9(6) . . . . ? Gd1 N3 C2 N4 -10.6(7) . . . . ? Si2 N3 C2 C12 -7.9(10) . . . . ? Gd1 N3 C2 C12 169.6(6) . . . . ? Si2 N3 C2 Gd1 -177.5(6) . . . . ? C5' N4 C2 N3 164.5(15) . . . . ? C5 N4 C2 N3 -173.1(14) . . . . ? Gd1 N4 C2 N3 11.7(8) . . . . ? C5' N4 C2 C12 -15.7(17) . . . . ? C5 N4 C2 C12 6.7(17) . . . . ? Gd1 N4 C2 C12 -168.5(6) . . . . ? C5' N4 C2 Gd1 152.8(16) . . . . ? C5 N4 C2 Gd1 175.3(16) . . . . ? N5 Gd1 C2 N3 74.4(4) . . . . ? N4 Gd1 C2 N3 -168.4(8) . . . . ? N2 Gd1 C2 N3 177.3(4) . . . . ? O2 Gd1 C2 N3 -12.4(5) . . . . ? N1 Gd1 C2 N3 -138.8(4) . . . . ? O1 Gd1 C2 N3 -71.3(4) . . . . ? C1 Gd1 C2 N3 -160.8(4) . . . . ? N5 Gd1 C2 N4 -117.3(5) . . . . ? N2 Gd1 C2 N4 -14.3(6) . . . . ? O2 Gd1 C2 N4 155.9(5) . . . . ? N1 Gd1 C2 N4 29.6(7) . . . . ? O1 Gd1 C2 N4 97.0(5) . . . . ? N3 Gd1 C2 N4 168.4(8) . . . . ? C1 Gd1 C2 N4 7.6(6) . . . . ? N5 Gd1 C2 C12 -52(3) . . . . ? N4 Gd1 C2 C12 65(2) . . . . ? N2 Gd1 C2 C12 51(3) . . . . ? O2 Gd1 C2 C12 -139(2) . . . . ? N1 Gd1 C2 C12 95(3) . . . . ? O1 Gd1 C2 C12 162(3) . . . . ? N3 Gd1 C2 C12 -127(3) . . . . ? C1 Gd1 C2 C12 73(3) . . . . ? C1 N2 C3 C4 -142(2) . . . . ? Gd1 N2 C3 C4 -4(5) . . . . ? C1 N2 C3' C4' -102(2) . . . . ? Gd1 N2 C3' C4' 39(5) . . . . ? N2 C3 C4 C5 60(4) . . . . ? N2 C3' C4' C5' -58(3) . . . . ? C2 N4 C5 C4 -121.6(16) . . . . ? C5' N4 C5 C4 -44(5) . . . . ? Gd1 N4 C5 C4 52(3) . . . . ? C3 C4 C5 N4 -78(2) . . . . ? C2 N4 C5' C4' 173.8(15) . . . . ? C5 N4 C5' C4' 60(5) . . . . ? Gd1 N4 C5' C4' -46(3) . . . . ? C3' C4' C5' N4 63(3) . . . . ? N2 C1 C6 C11 -80.3(9) . . . . ? N1 C1 C6 C11 103.2(8) . . . . ? Gd1 C1 C6 C11 -161.2(10) . . . . ? N2 C1 C6 C7 97.8(8) . . . . ? N1 C1 C6 C7 -78.7(9) . . . . ? Gd1 C1 C6 C7 16.9(16) . . . . ? C11 C6 C7 C8 -0.9(12) . . . . ? C1 C6 C7 C8 -179.1(8) . . . . ? C6 C7 C8 C9 -2.1(14) . . . . ? C7 C8 C9 C10 2.1(15) . . . . ? C8 C9 C10 C11 0.8(15) . . . . ? C7 C6 C11 C10 3.8(12) . . . . ? C1 C6 C11 C10 -178.1(7) . . . . ? C9 C10 C11 C6 -3.8(13) . . . . ? N3 C2 C12 C17 -94.8(9) . . . . ? N4 C2 C12 C17 85.4(10) . . . . ? Gd1 C2 C12 C17 27(3) . . . . ? N3 C2 C12 C13 87.0(9) . . . . ? N4 C2 C12 C13 -92.8(9) . . . . ? Gd1 C2 C12 C13 -151(2) . . . . ? C17 C12 C13 C14 2.1(11) . . . . ? C2 C12 C13 C14 -179.7(7) . . . . ? C12 C13 C14 C15 -0.9(12) . . . . ? C13 C14 C15 C16 -0.1(14) . . . . ? C14 C15 C16 C17 -0.1(14) . . . . ? C13 C12 C17 C16 -2.4(12) . . . . ? C2 C12 C17 C16 179.4(7) . . . . ? C15 C16 C17 C12 1.4(13) . . . . ? Gd1 N5 C24 C29 -1.1(14) . . . . ? Gd1 N5 C24 C25 178.8(8) . . . . ? N5 C24 C25 C26 179.2(6) . . . . ? C29 C24 C25 C26 -0.9(9) . . . . ? N5 C24 C25 C30 1.3(9) . . . . ? C29 C24 C25 C30 -178.8(6) . . . . ? C24 C25 C26 C27 0.3(10) . . . . ? C30 C25 C26 C27 178.3(7) . . . . ? C25 C26 C27 C28 -0.7(11) . . . . ? C26 C27 C28 C29 1.6(11) . . . . ? N5 C24 C29 C28 -178.4(6) . . . . ? C25 C24 C29 C28 1.8(9) . . . . ? N5 C24 C29 C33 -1.8(9) . . . . ? C25 C24 C29 C33 178.3(6) . . . . ? C27 C28 C29 C24 -2.1(10) . . . . ? C27 C28 C29 C33 -178.8(7) . . . . ? C26 C25 C30 C32 20.4(10) . . . . ? C24 C25 C30 C32 -161.7(7) . . . . ? C26 C25 C30 C31 -104.0(7) . . . . ? C24 C25 C30 C31 73.9(8) . . . . ? C24 C29 C33 C34 -92.5(8) . . . . ? C28 C29 C33 C34 84.0(8) . . . . ? C24 C29 C33 C35 142.7(7) . . . . ? C28 C29 C33 C35 -40.7(9) . . . . ? C38 O1 C36 C37 -172.0(6) . . . . ? Gd1 O1 C36 C37 45.8(7) . . . . ? C39 O2 C37 C36 -162.7(6) . . . . ? Gd1 O2 C37 C36 30.0(8) . . . . ? O1 C36 C37 O2 -47.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.095 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.097 # Attachment '- shelxl 8.cif' data_shelxl8 _database_code_depnum_ccdc_archive 'CCDC 862446' #TrackingRef '- shelxl 8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H62 N7 Si2 Y' _chemical_formula_sum 'C49 H62 N7 Si2 Y' _chemical_formula_weight 894.15 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' Y Y -2.7962 3.5667 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9207(8) _cell_length_b 18.8194(10) _cell_length_c 20.0255(14) _cell_angle_alpha 76.526(5) _cell_angle_beta 89.145(7) _cell_angle_gamma 73.163(6) _cell_volume 4875.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 20615 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42285 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.1120 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.50 _reflns_number_total 18054 _reflns_number_gt 12351 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+2.4597P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18054 _refine_ls_number_parameters 1086 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.1548 _refine_ls_wR_factor_gt 0.1369 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.96649(3) 0.75904(2) 1.01511(2) 0.03702(13) Uani 1 1 d . . . Si1 Si 1.15122(11) 0.83447(8) 1.10470(8) 0.0539(4) Uani 1 1 d . . . Si2 Si 0.68866(10) 0.85780(8) 0.94022(7) 0.0475(3) Uani 1 1 d . . . N1 N 1.0981(3) 0.7673(2) 1.0897(2) 0.0452(10) Uani 1 1 d . . . N2 N 1.0643(3) 0.6561(2) 1.0994(2) 0.0585(12) Uani 1 1 d . . . N3 N 0.7911(3) 0.7822(2) 0.9761(2) 0.0440(10) Uani 1 1 d . . . N4 N 0.8848(3) 0.6653(2) 1.0322(2) 0.0592(12) Uani 1 1 d . . . N5 N 1.0464(3) 0.7338(2) 0.91399(18) 0.0380(9) Uani 1 1 d . . . N6 N 0.9897(3) 0.8554(2) 0.9219(2) 0.0444(10) Uani 1 1 d D . . H6 H 0.986(3) 0.8990(10) 0.9014(18) 0.025(11) Uiso 1 1 d D . . N7 N 0.8670(3) 0.8499(3) 1.0825(2) 0.0609(12) Uani 1 1 d . . . C1 C 1.1128(3) 0.6944(3) 1.1244(2) 0.0458(12) Uani 1 1 d . . . C2 C 0.7951(4) 0.7121(3) 1.0133(3) 0.0467(12) Uani 1 1 d . . . C3 C 1.0666(5) 0.5775(3) 1.1322(3) 0.0751(19) Uani 1 1 d . . . H3A H 1.0377 0.5757 1.1773 0.090 Uiso 1 1 calc R . . H3B H 1.1363 0.5446 1.1391 0.090 Uiso 1 1 calc R . . C4 C 1.0080(5) 0.5485(3) 1.0882(4) 0.100(3) Uani 1 1 d . . . H4A H 1.0400 0.5493 1.0442 0.120 Uiso 1 1 calc R . . H4B H 1.0151 0.4949 1.1104 0.120 Uiso 1 1 calc R . . C5 C 0.9022(4) 0.5875(3) 1.0734(4) 0.077(2) Uani 1 1 d . . . H5A H 0.8687 0.5888 1.1167 0.093 Uiso 1 1 calc R . . H5B H 0.8726 0.5590 1.0486 0.093 Uiso 1 1 calc R . . C6 C 1.1827(4) 0.6596(3) 1.1881(3) 0.0474(12) Uani 1 1 d . . . C7 C 1.2777(4) 0.6130(3) 1.1847(3) 0.0670(16) Uani 1 1 d . . . H7 H 1.2991 0.6008 1.1429 0.080 Uiso 1 1 calc R . . C8 C 1.3427(5) 0.5837(4) 1.2436(4) 0.084(2) Uani 1 1 d . . . H8 H 1.4078 0.5517 1.2411 0.101 Uiso 1 1 calc R . . C9 C 1.3135(5) 0.6007(4) 1.3041(4) 0.084(2) Uani 1 1 d . . . H9 H 1.3586 0.5819 1.3430 0.101 Uiso 1 1 calc R . . C10 C 1.2177(5) 0.6455(4) 1.3084(3) 0.082(2) Uani 1 1 d . . . H10 H 1.1961 0.6560 1.3508 0.098 Uiso 1 1 calc R . . C11 C 1.1528(4) 0.6753(4) 1.2505(3) 0.0683(17) Uani 1 1 d . . . H11 H 1.0875 0.7067 1.2536 0.082 Uiso 1 1 calc R . . C12 C 0.7013(3) 0.6895(3) 1.0348(3) 0.0454(12) Uani 1 1 d . . . C13 C 0.6697(4) 0.6889(3) 1.1004(3) 0.0645(15) Uani 1 1 d . . . H13A H 0.7066 0.7029 1.1314 0.077 Uiso 1 1 calc R . . C14 C 0.5845(5) 0.6679(3) 1.1215(3) 0.0710(17) Uani 1 1 d . . . H14 H 0.5631 0.6684 1.1662 0.085 Uiso 1 1 calc R . . C15 C 0.5315(4) 0.6464(3) 1.0762(4) 0.0724(18) Uani 1 1 d . . . H15 H 0.4738 0.6318 1.0899 0.087 Uiso 1 1 calc R . . C16 C 0.5631(4) 0.6464(3) 1.0116(3) 0.0697(17) Uani 1 1 d . . . H16 H 0.5264 0.6320 0.9808 0.084 Uiso 1 1 calc R . . C17 C 0.6484(4) 0.6673(3) 0.9905(3) 0.0587(14) Uani 1 1 d . . . H17 H 0.6698 0.6662 0.9460 0.070 Uiso 1 1 calc R . . C18 C 1.1057(7) 0.8705(5) 1.1830(4) 0.129(3) Uani 1 1 d . . . H18A H 1.0329 0.8845 1.1819 0.194 Uiso 1 1 calc R . . H18B H 1.1275 0.9150 1.1834 0.194 Uiso 1 1 calc R . . H18C H 1.1333 0.8307 1.2240 0.194 Uiso 1 1 calc R . . C19 C 1.1087(5) 0.9172(3) 1.0318(4) 0.095(2) Uani 1 1 d . . . H19A H 1.1348 0.9031 0.9900 0.142 Uiso 1 1 calc R . . H19B H 1.1328 0.9583 1.0391 0.142 Uiso 1 1 calc R . . H19C H 1.0358 0.9340 1.0274 0.142 Uiso 1 1 calc R . . C20 C 1.2895(5) 0.8031(4) 1.1113(5) 0.117(3) Uani 1 1 d . . . H20A H 1.3130 0.7594 1.1501 0.175 Uiso 1 1 calc R . . H20B H 1.3138 0.8445 1.1179 0.175 Uiso 1 1 calc R . . H20C H 1.3146 0.7889 1.0693 0.175 Uiso 1 1 calc R . . C21 C 0.6268(4) 0.8439(3) 0.8639(3) 0.0689(17) Uani 1 1 d . . . H21A H 0.6767 0.8305 0.8311 0.103 Uiso 1 1 calc R . . H21B H 0.5756 0.8908 0.8425 0.103 Uiso 1 1 calc R . . H21C H 0.5961 0.8031 0.8787 0.103 Uiso 1 1 calc R . . C22 C 0.7356(4) 0.9426(3) 0.9079(3) 0.0626(15) Uani 1 1 d . . . H22A H 0.7717 0.9506 0.9452 0.094 Uiso 1 1 calc R . . H22B H 0.6790 0.9876 0.8906 0.094 Uiso 1 1 calc R . . H22C H 0.7803 0.9335 0.8712 0.094 Uiso 1 1 calc R . . C23 C 0.5905(4) 0.8836(3) 1.0018(3) 0.0639(15) Uani 1 1 d . . . H23A H 0.5562 0.8446 1.0132 0.096 Uiso 1 1 calc R . . H23B H 0.5423 0.9324 0.9810 0.096 Uiso 1 1 calc R . . H23C H 0.6218 0.8872 1.0434 0.096 Uiso 1 1 calc R . . C24 C 1.0809(4) 0.6749(2) 0.8785(2) 0.0406(11) Uani 1 1 d . . . C25 C 1.1760(4) 0.6221(3) 0.8994(2) 0.0442(12) Uani 1 1 d . . . C26 C 1.2130(4) 0.5668(3) 0.8622(3) 0.0535(13) Uani 1 1 d . . . H26 H 1.2766 0.5311 0.8752 0.064 Uiso 1 1 calc R . . C27 C 1.1584(4) 0.5635(3) 0.8069(3) 0.0610(15) Uani 1 1 d . . . H27 H 1.1861 0.5275 0.7811 0.073 Uiso 1 1 calc R . . C28 C 1.0636(4) 0.6129(3) 0.7897(3) 0.0570(14) Uani 1 1 d . . . H28 H 1.0263 0.6092 0.7526 0.068 Uiso 1 1 calc R . . C29 C 1.0208(4) 0.6683(3) 0.8257(2) 0.0454(12) Uani 1 1 d . . . C30 C 1.2360(4) 0.6268(3) 0.9596(3) 0.0552(14) Uani 1 1 d . . . H30 H 1.1871 0.6414 0.9941 0.066 Uiso 1 1 calc R . . C31 C 1.2881(4) 0.6897(3) 0.9406(3) 0.0705(17) Uani 1 1 d . . . H31A H 1.3328 0.6801 0.9040 0.106 Uiso 1 1 calc R . . H31B H 1.3265 0.6898 0.9805 0.106 Uiso 1 1 calc R . . H31C H 1.2378 0.7389 0.9252 0.106 Uiso 1 1 calc R . . C32 C 1.3119(4) 0.5508(3) 0.9955(3) 0.0786(19) Uani 1 1 d . . . H32A H 1.2781 0.5114 1.0071 0.118 Uiso 1 1 calc R . . H32B H 1.3407 0.5563 1.0371 0.118 Uiso 1 1 calc R . . H32C H 1.3649 0.5364 0.9649 0.118 Uiso 1 1 calc R . . C33 C 0.9112(4) 0.7148(3) 0.8117(3) 0.0502(13) Uani 1 1 d . . . H33 H 0.8994 0.7572 0.8352 0.060 Uiso 1 1 calc R . . C34 C 0.8802(5) 0.7498(3) 0.7357(3) 0.0753(18) Uani 1 1 d . . . H34A H 0.9266 0.7773 0.7150 0.113 Uiso 1 1 calc R . . H34B H 0.8128 0.7848 0.7310 0.113 Uiso 1 1 calc R . . H34C H 0.8816 0.7095 0.7127 0.113 Uiso 1 1 calc R . . C35 C 0.8454(4) 0.6645(3) 0.8437(3) 0.0611(15) Uani 1 1 d . . . H35A H 0.8550 0.6227 0.8212 0.092 Uiso 1 1 calc R . . H35B H 0.7754 0.6948 0.8378 0.092 Uiso 1 1 calc R . . H35C H 0.8643 0.6440 0.8923 0.092 Uiso 1 1 calc R . . C36 C 1.0292(3) 0.8081(3) 0.8829(2) 0.0397(11) Uani 1 1 d . . . C37 C 1.0504(4) 0.8364(3) 0.8087(2) 0.0414(11) Uani 1 1 d . . . C38 C 0.9853(4) 0.9043(3) 0.7708(3) 0.0536(13) Uani 1 1 d . . . H38 H 0.9299 0.9311 0.7915 0.064 Uiso 1 1 calc R . . C39 C 1.0018(5) 0.9331(4) 0.7022(3) 0.0694(17) Uani 1 1 d . . . H39 H 0.9569 0.9787 0.6765 0.083 Uiso 1 1 calc R . . C40 C 1.0834(6) 0.8949(4) 0.6723(3) 0.0719(18) Uani 1 1 d . . . H40 H 1.0945 0.9143 0.6261 0.086 Uiso 1 1 calc R . . C41 C 1.1491(5) 0.8284(3) 0.7097(3) 0.0661(16) Uani 1 1 d . . . H41 H 1.2055 0.8026 0.6891 0.079 Uiso 1 1 calc R . . C42 C 1.1328(4) 0.7992(3) 0.7771(3) 0.0518(13) Uani 1 1 d . . . H42 H 1.1781 0.7534 0.8020 0.062 Uiso 1 1 calc R . . C43 C 0.8252(4) 0.9051(3) 1.0995(3) 0.0542(14) Uani 1 1 d . . . C44 C 0.7762(4) 0.9755(3) 1.1187(3) 0.0514(13) Uani 1 1 d . . . C45 C 0.8077(4) 0.9869(3) 1.1798(3) 0.0618(15) Uani 1 1 d . . . H45 H 0.8582 0.9484 1.2093 0.074 Uiso 1 1 calc R . . C46 C 0.7633(5) 1.0561(4) 1.1965(3) 0.0712(17) Uani 1 1 d . . . H46 H 0.7832 1.0647 1.2378 0.085 Uiso 1 1 calc R . . C47 C 0.6908(5) 1.1116(3) 1.1531(3) 0.0698(17) Uani 1 1 d . . . H47 H 0.6622 1.1587 1.1645 0.084 Uiso 1 1 calc R . . C48 C 0.6586(5) 1.1000(3) 1.0930(3) 0.0719(17) Uani 1 1 d . . . H48 H 0.6081 1.1386 1.0639 0.086 Uiso 1 1 calc R . . C49 C 0.7010(4) 1.0312(3) 1.0759(3) 0.0602(14) Uani 1 1 d . . . H49 H 0.6788 1.0223 1.0354 0.072 Uiso 1 1 calc R . . Y2 Y 0.28092(3) 0.24625(3) 0.47639(2) 0.04089(14) Uani 1 1 d . . . Si3 Si 0.53170(11) 0.17174(9) 0.38679(8) 0.0552(4) Uani 1 1 d . . . Si4 Si 0.07301(11) 0.15569(8) 0.55641(7) 0.0496(4) Uani 1 1 d . . . N8 N 0.4222(3) 0.2375(2) 0.3998(2) 0.0453(10) Uani 1 1 d . . . N9 N 0.2865(3) 0.3410(2) 0.3785(2) 0.0534(11) Uani 1 1 d . . . N10 N 0.1223(3) 0.2275(2) 0.5161(2) 0.0463(10) Uani 1 1 d . . . N11 N 0.1308(3) 0.3465(2) 0.4704(2) 0.0515(11) Uani 1 1 d . . . N12 N 0.3460(3) 0.2663(2) 0.5771(2) 0.0451(10) Uani 1 1 d . . . N13 N 0.3856(3) 0.1475(3) 0.5633(2) 0.0546(11) Uani 1 1 d D . . H13 H 0.413(3) 0.1020(9) 0.579(3) 0.060(17) Uiso 1 1 d D . . N14 N 0.2623(3) 0.1454(3) 0.4197(2) 0.0605(12) Uani 1 1 d . . . C50 C 0.3768(4) 0.3074(3) 0.3609(2) 0.0456(12) Uani 1 1 d . . . C51 C 0.0741(3) 0.3002(3) 0.4850(2) 0.0456(12) Uani 1 1 d . . . C52 C 0.2283(4) 0.4190(3) 0.3469(3) 0.0698(17) Uani 1 1 d . . . H52A H 0.1826 0.4187 0.3103 0.084 Uiso 1 1 calc R . . H52B H 0.2739 0.4479 0.3260 0.084 Uiso 1 1 calc R . . C53 C 0.1694(5) 0.4574(3) 0.3968(4) 0.080(2) Uani 1 1 d . . . H53A H 0.1381 0.5111 0.3735 0.096 Uiso 1 1 calc R . . H53B H 0.2161 0.4565 0.4334 0.096 Uiso 1 1 calc R . . C54 C 0.0889(4) 0.4256(3) 0.4298(3) 0.0675(17) Uani 1 1 d . . . H54A H 0.0529 0.4576 0.4599 0.081 Uiso 1 1 calc R . . H54B H 0.0406 0.4269 0.3942 0.081 Uiso 1 1 calc R . . C55 C 0.4260(4) 0.3461(3) 0.3015(3) 0.0482(12) Uani 1 1 d . . . C56 C 0.5138(4) 0.3635(3) 0.3115(3) 0.0551(14) Uani 1 1 d . . . H56 H 0.5418 0.3533 0.3563 0.066 Uiso 1 1 calc R . . C57 C 0.5612(5) 0.3960(3) 0.2563(4) 0.0739(18) Uani 1 1 d . . . H57 H 0.6216 0.4066 0.2637 0.089 Uiso 1 1 calc R . . C58 C 0.5200(6) 0.4121(4) 0.1922(4) 0.090(2) Uani 1 1 d . . . H58 H 0.5522 0.4340 0.1548 0.108 Uiso 1 1 calc R . . C59 C 0.4323(6) 0.3972(4) 0.1806(3) 0.091(2) Uani 1 1 d . . . H59 H 0.4042 0.4090 0.1355 0.110 Uiso 1 1 calc R . . C60 C 0.3843(5) 0.3640(3) 0.2361(3) 0.0697(17) Uani 1 1 d . . . H60 H 0.3235 0.3541 0.2284 0.084 Uiso 1 1 calc R . . C61 C -0.0361(3) 0.3271(3) 0.4645(2) 0.0464(12) Uani 1 1 d . . . C62 C -0.0711(4) 0.3057(3) 0.4111(3) 0.0555(14) Uani 1 1 d . . . H62 H -0.0264 0.2724 0.3884 0.067 Uiso 1 1 calc R . . C63 C -0.1731(5) 0.3331(3) 0.3902(3) 0.0694(16) Uani 1 1 d . . . H63 H -0.1963 0.3189 0.3529 0.083 Uiso 1 1 calc R . . C64 C -0.2387(5) 0.3796(4) 0.4228(4) 0.0732(18) Uani 1 1 d . . . H64 H -0.3074 0.3968 0.4089 0.088 Uiso 1 1 calc R . . C65 C -0.2047(4) 0.4017(4) 0.4763(4) 0.0796(19) Uani 1 1 d . . . H65 H -0.2504 0.4345 0.4989 0.096 Uiso 1 1 calc R . . C66 C -0.1033(4) 0.3760(3) 0.4975(3) 0.0662(16) Uani 1 1 d . . . H66 H -0.0804 0.3916 0.5340 0.079 Uiso 1 1 calc R . . C67 C 0.5543(5) 0.1714(4) 0.2948(3) 0.100(2) Uani 1 1 d . . . H67A H 0.4945 0.1689 0.2724 0.150 Uiso 1 1 calc R . . H67B H 0.6102 0.1273 0.2922 0.150 Uiso 1 1 calc R . . H67C H 0.5701 0.2177 0.2719 0.150 Uiso 1 1 calc R . . C68 C 0.5279(5) 0.0743(3) 0.4328(4) 0.105(3) Uani 1 1 d . . . H68A H 0.5089 0.0746 0.4796 0.157 Uiso 1 1 calc R . . H68B H 0.5938 0.0379 0.4337 0.157 Uiso 1 1 calc R . . H68C H 0.4791 0.0596 0.4092 0.157 Uiso 1 1 calc R . . C69 C 0.6451(4) 0.1844(4) 0.4250(3) 0.084(2) Uani 1 1 d . . . H69A H 0.6547 0.2326 0.4007 0.126 Uiso 1 1 calc R . . H69B H 0.7037 0.1428 0.4213 0.126 Uiso 1 1 calc R . . H69C H 0.6359 0.1845 0.4731 0.126 Uiso 1 1 calc R . . C70 C 0.0102(4) 0.1168(3) 0.4973(3) 0.0698(17) Uani 1 1 d . . . H70A H -0.0545 0.1532 0.4800 0.105 Uiso 1 1 calc R . . H70B H 0.0005 0.0688 0.5222 0.105 Uiso 1 1 calc R . . H70C H 0.0520 0.1083 0.4590 0.105 Uiso 1 1 calc R . . C71 C -0.0195(5) 0.1849(4) 0.6207(3) 0.090(2) Uani 1 1 d . . . H71A H 0.0106 0.2054 0.6523 0.135 Uiso 1 1 calc R . . H71B H -0.0382 0.1408 0.6461 0.135 Uiso 1 1 calc R . . H71C H -0.0788 0.2237 0.5971 0.135 Uiso 1 1 calc R . . C72 C 0.1792(5) 0.0761(3) 0.6038(4) 0.094(2) Uani 1 1 d . . . H72A H 0.2283 0.0589 0.5717 0.141 Uiso 1 1 calc R . . H72B H 0.1545 0.0342 0.6272 0.141 Uiso 1 1 calc R . . H72C H 0.2104 0.0936 0.6372 0.141 Uiso 1 1 calc R . . C73 C 0.3378(3) 0.3238(3) 0.6144(2) 0.0434(12) Uani 1 1 d . A . C74 C 0.2637(4) 0.3377(3) 0.6620(3) 0.0440(12) Uani 1 1 d . . . C75 C 0.2647(4) 0.3912(3) 0.6987(3) 0.0609(15) Uani 1 1 d . . . H75 H 0.2164 0.4004 0.7315 0.073 Uiso 1 1 calc R . . C76 C 0.3339(5) 0.4318(3) 0.6890(4) 0.0757(18) Uani 1 1 d . . . H76 H 0.3345 0.4664 0.7159 0.091 Uiso 1 1 calc R . . C77 C 0.4018(4) 0.4207(3) 0.6394(4) 0.0718(18) Uani 1 1 d . A . H77 H 0.4472 0.4499 0.6313 0.086 Uiso 1 1 calc R . . C78 C 0.4055(4) 0.3676(3) 0.6008(3) 0.0616(15) Uani 1 1 d D . . C79 C 0.1812(4) 0.2993(3) 0.6720(2) 0.0487(12) Uani 1 1 d . . . H79 H 0.1933 0.2630 0.6419 0.058 Uiso 1 1 calc R . . C80 C 0.1795(4) 0.2539(3) 0.7459(3) 0.0706(17) Uani 1 1 d . . . H80A H 0.2443 0.2161 0.7596 0.106 Uiso 1 1 calc R . . H80B H 0.1276 0.2285 0.7485 0.106 Uiso 1 1 calc R . . H80C H 0.1655 0.2885 0.7764 0.106 Uiso 1 1 calc R . . C81 C 0.0797(4) 0.3584(3) 0.6490(3) 0.0645(15) Uani 1 1 d . . . H81A H 0.0656 0.3946 0.6779 0.097 Uiso 1 1 calc R . . H81B H 0.0277 0.3329 0.6530 0.097 Uiso 1 1 calc R . . H81C H 0.0810 0.3853 0.6016 0.097 Uiso 1 1 calc R . . C82 C 0.4669(10) 0.3600(8) 0.5367(7) 0.0846(17) Uiso 0.50 1 d PD A 1 H82 H 0.4290 0.3402 0.5077 0.102 Uiso 0.50 1 calc PR A 1 C82' C 0.4911(9) 0.3556(9) 0.5541(6) 0.0846(17) Uiso 0.50 1 d PD A 2 H82' H 0.5104 0.4004 0.5604 0.102 Uiso 0.50 1 calc PR A 2 C83 C 0.5650(10) 0.2983(8) 0.5582(7) 0.0846(17) Uiso 0.50 1 d PD A 1 H83A H 0.6180 0.3215 0.5613 0.127 Uiso 0.50 1 calc PR A 1 H83B H 0.5806 0.2678 0.5244 0.127 Uiso 0.50 1 calc PR A 1 H83C H 0.5596 0.2660 0.6026 0.127 Uiso 0.50 1 calc PR A 1 C83' C 0.5910(10) 0.3001(8) 0.5822(7) 0.0846(17) Uiso 0.50 1 d PD A 2 H83D H 0.6357 0.2941 0.5449 0.127 Uiso 0.50 1 calc PR A 2 H83E H 0.5820 0.2510 0.6044 0.127 Uiso 0.50 1 calc PR A 2 H83F H 0.6200 0.3192 0.6155 0.127 Uiso 0.50 1 calc PR A 2 C84 C 0.4784(11) 0.4324(7) 0.4920(7) 0.0846(17) Uiso 0.50 1 d PD A 1 H84A H 0.5039 0.4595 0.5199 0.127 Uiso 0.50 1 calc PR A 1 H84B H 0.4137 0.4642 0.4701 0.127 Uiso 0.50 1 calc PR A 1 H84C H 0.5253 0.4203 0.4571 0.127 Uiso 0.50 1 calc PR A 1 C84' C 0.4527(10) 0.3925(8) 0.4809(6) 0.0846(17) Uiso 0.50 1 d PD A 2 H84D H 0.5079 0.4013 0.4533 0.127 Uiso 0.50 1 calc PR A 2 H84E H 0.4020 0.4410 0.4789 0.127 Uiso 0.50 1 calc PR A 2 H84F H 0.4234 0.3593 0.4632 0.127 Uiso 0.50 1 calc PR A 2 C85 C 0.3843(3) 0.1918(3) 0.6057(2) 0.0436(12) Uani 1 1 d . . . C86 C 0.4212(3) 0.1575(3) 0.6807(3) 0.0462(12) Uani 1 1 d . . . C87 C 0.4668(4) 0.1930(3) 0.7190(3) 0.0603(15) Uani 1 1 d . . . H87 H 0.4782 0.2399 0.6984 0.072 Uiso 1 1 calc R . . C88 C 0.4953(4) 0.1587(4) 0.7878(3) 0.0741(18) Uani 1 1 d . . . H88 H 0.5264 0.1826 0.8136 0.089 Uiso 1 1 calc R . . C89 C 0.4786(5) 0.0906(4) 0.8188(3) 0.078(2) Uani 1 1 d . . . H89 H 0.4971 0.0684 0.8657 0.094 Uiso 1 1 calc R . . C90 C 0.4352(4) 0.0554(4) 0.7812(3) 0.0738(18) Uani 1 1 d . . . H90 H 0.4249 0.0082 0.8020 0.089 Uiso 1 1 calc R . . C91 C 0.4062(4) 0.0884(3) 0.7127(3) 0.0583(15) Uani 1 1 d . . . H91 H 0.3757 0.0636 0.6874 0.070 Uiso 1 1 calc R . . C92 C 0.2631(4) 0.0920(3) 0.4009(3) 0.0544(14) Uani 1 1 d . . . C93 C 0.2641(4) 0.0248(3) 0.3773(3) 0.0507(13) Uani 1 1 d . . . C94 C 0.2956(4) 0.0183(3) 0.3127(3) 0.0696(16) Uani 1 1 d . . . H94 H 0.3167 0.0573 0.2838 0.084 Uiso 1 1 calc R . . C95 C 0.2956(5) -0.0460(4) 0.2909(3) 0.0803(19) Uani 1 1 d . . . H95 H 0.3163 -0.0505 0.2468 0.096 Uiso 1 1 calc R . . C96 C 0.2660(5) -0.1029(4) 0.3326(4) 0.0745(18) Uani 1 1 d . . . H96 H 0.2663 -0.1465 0.3173 0.089 Uiso 1 1 calc R . . C97 C 0.2357(5) -0.0971(3) 0.3970(4) 0.0747(18) Uani 1 1 d . . . H97 H 0.2163 -0.1371 0.4258 0.090 Uiso 1 1 calc R . . C98 C 0.2336(4) -0.0330(3) 0.4197(3) 0.0597(14) Uani 1 1 d . . . H98 H 0.2117 -0.0286 0.4636 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0390(3) 0.0343(2) 0.0378(3) -0.0094(2) 0.0043(2) -0.0103(2) Si1 0.0535(9) 0.0500(9) 0.0632(10) -0.0164(7) -0.0041(8) -0.0203(7) Si2 0.0421(8) 0.0485(8) 0.0486(8) -0.0139(7) -0.0001(7) -0.0065(7) N1 0.049(2) 0.035(2) 0.047(2) -0.0046(19) -0.006(2) -0.0106(19) N2 0.073(3) 0.039(2) 0.063(3) 0.002(2) -0.014(2) -0.025(2) N3 0.042(2) 0.041(2) 0.048(2) -0.0120(19) 0.0011(19) -0.0112(19) N4 0.045(3) 0.040(2) 0.085(3) 0.002(2) -0.004(2) -0.015(2) N5 0.043(2) 0.034(2) 0.037(2) -0.0132(17) 0.0077(18) -0.0093(17) N6 0.055(3) 0.029(2) 0.046(2) -0.004(2) 0.009(2) -0.012(2) N7 0.048(3) 0.075(3) 0.060(3) -0.029(3) 0.002(2) -0.008(2) C1 0.041(3) 0.042(3) 0.049(3) -0.006(2) 0.001(2) -0.006(2) C2 0.043(3) 0.043(3) 0.058(3) -0.019(2) 0.000(2) -0.013(2) C3 0.095(5) 0.043(3) 0.081(4) 0.009(3) -0.029(4) -0.028(3) C4 0.081(5) 0.041(3) 0.160(7) 0.016(4) -0.033(5) -0.021(3) C5 0.059(4) 0.043(3) 0.119(5) 0.009(3) -0.011(4) -0.020(3) C6 0.044(3) 0.044(3) 0.049(3) -0.005(2) -0.002(2) -0.011(2) C7 0.054(4) 0.072(4) 0.062(4) -0.012(3) -0.003(3) -0.001(3) C8 0.061(4) 0.078(5) 0.098(6) -0.016(4) -0.014(4) 0.002(3) C9 0.075(5) 0.091(5) 0.075(5) -0.006(4) -0.029(4) -0.017(4) C10 0.085(5) 0.119(6) 0.036(3) -0.011(3) 0.001(3) -0.028(4) C11 0.050(3) 0.098(5) 0.049(3) -0.016(3) 0.006(3) -0.011(3) C12 0.040(3) 0.046(3) 0.053(3) -0.012(2) 0.002(2) -0.015(2) C13 0.063(4) 0.075(4) 0.061(4) -0.017(3) 0.002(3) -0.029(3) C14 0.069(4) 0.078(4) 0.064(4) -0.019(3) 0.023(3) -0.019(3) C15 0.051(4) 0.075(4) 0.094(5) -0.017(4) 0.016(4) -0.026(3) C16 0.049(3) 0.090(4) 0.089(5) -0.041(4) 0.013(3) -0.035(3) C17 0.049(3) 0.067(4) 0.069(4) -0.028(3) 0.010(3) -0.021(3) C18 0.171(9) 0.152(8) 0.124(7) -0.091(6) 0.044(6) -0.094(7) C19 0.108(5) 0.059(4) 0.120(6) 0.001(4) -0.033(5) -0.044(4) C20 0.060(4) 0.089(5) 0.202(9) -0.026(5) -0.026(5) -0.028(4) C21 0.064(4) 0.068(4) 0.067(4) -0.022(3) -0.018(3) -0.001(3) C22 0.061(4) 0.047(3) 0.070(4) -0.004(3) -0.002(3) -0.010(3) C23 0.049(3) 0.066(4) 0.072(4) -0.024(3) 0.009(3) -0.004(3) C24 0.050(3) 0.034(3) 0.039(3) -0.009(2) 0.016(2) -0.014(2) C25 0.048(3) 0.033(3) 0.050(3) -0.011(2) 0.018(2) -0.010(2) C26 0.051(3) 0.045(3) 0.064(4) -0.016(3) 0.021(3) -0.012(3) C27 0.073(4) 0.050(3) 0.069(4) -0.032(3) 0.033(3) -0.020(3) C28 0.073(4) 0.056(3) 0.053(3) -0.024(3) 0.012(3) -0.028(3) C29 0.063(3) 0.040(3) 0.037(3) -0.012(2) 0.010(2) -0.018(2) C30 0.049(3) 0.054(3) 0.056(3) -0.017(3) 0.005(3) -0.002(3) C31 0.060(4) 0.073(4) 0.084(4) -0.025(3) 0.000(3) -0.021(3) C32 0.074(4) 0.067(4) 0.071(4) -0.009(3) 0.002(3) 0.011(3) C33 0.056(3) 0.048(3) 0.049(3) -0.017(2) -0.004(3) -0.015(3) C34 0.083(4) 0.073(4) 0.060(4) -0.006(3) -0.006(3) -0.015(3) C35 0.047(3) 0.065(4) 0.074(4) -0.020(3) 0.002(3) -0.019(3) C36 0.038(3) 0.040(3) 0.040(3) -0.009(2) 0.004(2) -0.009(2) C37 0.045(3) 0.043(3) 0.041(3) -0.008(2) 0.002(2) -0.022(2) C38 0.059(3) 0.052(3) 0.047(3) -0.006(3) 0.006(3) -0.016(3) C39 0.080(4) 0.076(4) 0.049(3) 0.009(3) -0.013(3) -0.036(4) C40 0.111(5) 0.089(5) 0.038(3) -0.014(3) 0.012(3) -0.063(4) C41 0.095(5) 0.070(4) 0.056(4) -0.030(3) 0.032(3) -0.047(4) C42 0.064(3) 0.053(3) 0.047(3) -0.017(3) 0.017(3) -0.026(3) C43 0.044(3) 0.069(4) 0.055(3) -0.025(3) 0.012(3) -0.017(3) C44 0.043(3) 0.058(3) 0.059(3) -0.024(3) 0.018(3) -0.016(3) C45 0.056(3) 0.068(4) 0.066(4) -0.028(3) 0.005(3) -0.015(3) C46 0.078(4) 0.075(4) 0.077(4) -0.043(4) 0.014(4) -0.029(4) C47 0.075(4) 0.056(4) 0.083(5) -0.028(3) 0.028(4) -0.018(3) C48 0.074(4) 0.066(4) 0.072(4) -0.021(3) 0.018(3) -0.011(3) C49 0.061(4) 0.067(4) 0.053(3) -0.022(3) 0.010(3) -0.013(3) Y2 0.0387(3) 0.0409(3) 0.0402(3) -0.0074(2) 0.0086(2) -0.0095(2) Si3 0.0473(8) 0.0549(9) 0.0600(10) -0.0175(8) 0.0173(7) -0.0075(7) Si4 0.0516(8) 0.0551(9) 0.0476(8) -0.0120(7) 0.0099(7) -0.0246(7) N8 0.042(2) 0.045(2) 0.050(2) -0.015(2) 0.0177(19) -0.0109(19) N9 0.050(3) 0.040(2) 0.058(3) 0.000(2) 0.021(2) -0.006(2) N10 0.043(2) 0.044(2) 0.050(2) -0.008(2) 0.0110(19) -0.013(2) N11 0.045(2) 0.042(2) 0.060(3) -0.004(2) 0.015(2) -0.007(2) N12 0.048(2) 0.039(2) 0.043(2) -0.0082(19) 0.0024(19) -0.0052(19) N13 0.064(3) 0.040(3) 0.054(3) -0.012(2) 0.000(2) -0.005(2) N14 0.058(3) 0.066(3) 0.059(3) -0.019(3) 0.010(2) -0.018(3) C50 0.048(3) 0.048(3) 0.045(3) -0.014(2) 0.013(2) -0.018(3) C51 0.039(3) 0.055(3) 0.041(3) -0.013(2) 0.013(2) -0.011(3) C52 0.073(4) 0.053(3) 0.068(4) 0.001(3) 0.029(3) -0.009(3) C53 0.075(4) 0.045(3) 0.103(5) 0.000(3) 0.024(4) -0.008(3) C54 0.054(3) 0.042(3) 0.092(4) 0.000(3) 0.024(3) -0.005(3) C55 0.050(3) 0.053(3) 0.044(3) -0.012(2) 0.014(2) -0.020(3) C56 0.055(3) 0.059(3) 0.056(3) -0.015(3) 0.010(3) -0.025(3) C57 0.063(4) 0.082(4) 0.087(5) -0.022(4) 0.026(4) -0.036(3) C58 0.094(5) 0.102(5) 0.080(5) -0.016(4) 0.046(4) -0.044(5) C59 0.119(6) 0.110(6) 0.045(4) -0.013(4) 0.022(4) -0.039(5) C60 0.074(4) 0.092(5) 0.053(4) -0.022(3) 0.010(3) -0.037(4) C61 0.039(3) 0.052(3) 0.044(3) -0.006(2) 0.013(2) -0.011(2) C62 0.056(3) 0.061(3) 0.046(3) -0.019(3) 0.008(3) -0.008(3) C63 0.069(4) 0.071(4) 0.064(4) -0.016(3) -0.010(3) -0.012(3) C64 0.048(3) 0.081(4) 0.086(5) -0.018(4) -0.006(3) -0.012(3) C65 0.039(3) 0.093(5) 0.104(5) -0.039(4) 0.015(3) -0.002(3) C66 0.046(3) 0.089(4) 0.063(4) -0.033(3) 0.007(3) -0.007(3) C67 0.098(5) 0.119(6) 0.074(5) -0.052(4) 0.017(4) 0.005(4) C68 0.071(4) 0.042(4) 0.181(8) -0.015(4) 0.046(5) 0.005(3) C69 0.057(4) 0.092(5) 0.089(5) -0.011(4) 0.001(3) -0.008(3) C70 0.078(4) 0.069(4) 0.078(4) -0.027(3) 0.006(3) -0.037(3) C71 0.113(5) 0.105(5) 0.090(5) -0.049(4) 0.063(4) -0.073(5) C72 0.086(5) 0.079(4) 0.103(5) 0.030(4) -0.022(4) -0.044(4) C73 0.044(3) 0.036(3) 0.046(3) -0.006(2) 0.002(2) -0.008(2) C74 0.043(3) 0.036(3) 0.052(3) -0.016(2) 0.004(2) -0.007(2) C75 0.054(3) 0.058(3) 0.072(4) -0.026(3) 0.011(3) -0.012(3) C76 0.071(4) 0.058(4) 0.110(5) -0.040(4) 0.001(4) -0.022(3) C77 0.057(4) 0.057(4) 0.109(5) -0.021(4) 0.008(4) -0.028(3) C78 0.054(3) 0.046(3) 0.085(4) -0.017(3) 0.020(3) -0.013(3) C79 0.052(3) 0.057(3) 0.044(3) -0.017(2) 0.015(2) -0.023(3) C80 0.071(4) 0.073(4) 0.063(4) -0.004(3) 0.018(3) -0.025(3) C81 0.049(3) 0.077(4) 0.069(4) -0.020(3) 0.005(3) -0.019(3) C85 0.037(3) 0.043(3) 0.045(3) -0.009(2) 0.003(2) -0.005(2) C86 0.037(3) 0.046(3) 0.049(3) -0.012(2) 0.001(2) -0.001(2) C87 0.050(3) 0.056(3) 0.067(4) -0.020(3) -0.009(3) 0.001(3) C88 0.066(4) 0.086(5) 0.061(4) -0.032(4) -0.019(3) 0.005(4) C89 0.065(4) 0.100(5) 0.043(4) -0.007(4) 0.002(3) 0.010(4) C90 0.058(4) 0.079(4) 0.062(4) 0.011(3) 0.005(3) -0.007(3) C91 0.051(3) 0.052(3) 0.063(4) 0.001(3) -0.007(3) -0.012(3) C92 0.049(3) 0.060(4) 0.051(3) -0.009(3) 0.008(3) -0.015(3) C93 0.052(3) 0.048(3) 0.054(3) -0.020(3) -0.003(3) -0.010(3) C94 0.077(4) 0.066(4) 0.066(4) -0.020(3) 0.018(3) -0.017(3) C95 0.097(5) 0.071(4) 0.070(4) -0.035(4) 0.010(4) -0.005(4) C96 0.079(4) 0.056(4) 0.081(5) -0.023(4) -0.019(4) -0.002(3) C97 0.078(4) 0.061(4) 0.083(5) -0.012(4) -0.009(4) -0.021(3) C98 0.065(4) 0.062(4) 0.051(3) -0.015(3) 0.003(3) -0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N4 2.321(4) . ? Y1 N2 2.339(4) . ? Y1 N6 2.372(4) . ? Y1 N5 2.375(4) . ? Y1 N1 2.443(4) . ? Y1 N3 2.458(4) . ? Y1 N7 2.514(5) . ? Y1 C2 2.777(5) . ? Y1 C1 2.806(5) . ? Y1 C36 2.808(5) . ? Si1 N1 1.721(4) . ? Si1 C19 1.828(6) . ? Si1 C20 1.840(6) . ? Si1 C18 1.880(7) . ? Si2 N3 1.719(4) . ? Si2 C23 1.863(5) . ? Si2 C21 1.871(5) . ? Si2 C22 1.871(5) . ? N1 C1 1.342(5) . ? N2 C1 1.299(6) . ? N2 C3 1.464(6) . ? N3 C2 1.341(6) . ? N4 C2 1.304(6) . ? N4 C5 1.457(6) . ? N5 C36 1.344(5) . ? N5 C24 1.417(6) . ? N6 C36 1.316(6) . ? N6 H6 0.814(10) . ? N7 C43 1.156(6) . ? C1 C6 1.511(6) . ? C2 C12 1.514(6) . ? C3 C4 1.495(8) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.443(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.371(7) . ? C6 C11 1.381(7) . ? C7 C8 1.398(8) . ? C7 H7 0.9400 . ? C8 C9 1.353(9) . ? C8 H8 0.9400 . ? C9 C10 1.369(9) . ? C9 H9 0.9400 . ? C10 C11 1.382(7) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C17 1.369(7) . ? C12 C13 1.378(7) . ? C13 C14 1.384(8) . ? C13 H13A 0.9400 . ? C14 C15 1.376(8) . ? C14 H14 0.9400 . ? C15 C16 1.360(8) . ? C15 H15 0.9400 . ? C16 C17 1.386(7) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.406(6) . ? C24 C29 1.409(6) . ? C25 C26 1.392(7) . ? C25 C30 1.511(7) . ? C26 C27 1.376(7) . ? C26 H26 0.9400 . ? C27 C28 1.371(7) . ? C27 H27 0.9400 . ? C28 C29 1.393(7) . ? C28 H28 0.9400 . ? C29 C33 1.516(7) . ? C30 C32 1.532(7) . ? C30 C31 1.532(7) . ? C30 H30 0.9900 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.525(7) . ? C33 C35 1.533(7) . ? C33 H33 0.9900 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 C37 1.512(6) . ? C37 C38 1.388(6) . ? C37 C42 1.389(7) . ? C38 C39 1.398(7) . ? C38 H38 0.9400 . ? C39 C40 1.368(8) . ? C39 H39 0.9400 . ? C40 C41 1.373(8) . ? C40 H40 0.9400 . ? C41 C42 1.375(7) . ? C41 H41 0.9400 . ? C42 H42 0.9400 . ? C43 C44 1.440(8) . ? C44 C49 1.378(7) . ? C44 C45 1.390(7) . ? C45 C46 1.386(8) . ? C45 H45 0.9400 . ? C46 C47 1.363(8) . ? C46 H46 0.9400 . ? C47 C48 1.375(8) . ? C47 H47 0.9400 . ? C48 C49 1.378(8) . ? C48 H48 0.9400 . ? C49 H49 0.9400 . ? Y2 N9 2.341(4) . ? Y2 N11 2.358(4) . ? Y2 N13 2.368(4) . ? Y2 N12 2.374(4) . ? Y2 N10 2.430(4) . ? Y2 N8 2.467(4) . ? Y2 N14 2.502(5) . ? Y2 C51 2.779(5) . ? Y2 C85 2.801(5) . ? Y2 C50 2.830(5) . ? Si3 N8 1.723(4) . ? Si3 C69 1.865(6) . ? Si3 C67 1.866(6) . ? Si3 C68 1.867(6) . ? Si4 N10 1.720(4) . ? Si4 C72 1.850(6) . ? Si4 C71 1.868(6) . ? Si4 C70 1.873(5) . ? N8 C50 1.338(6) . ? N9 C50 1.317(6) . ? N9 C52 1.451(6) . ? N10 C51 1.339(6) . ? N11 C51 1.318(6) . ? N11 C54 1.471(6) . ? N12 C85 1.334(5) . ? N12 C73 1.430(6) . ? N13 C85 1.317(6) . ? N13 H13 0.817(10) . ? N14 C92 1.149(6) . ? C50 C55 1.508(6) . ? C51 C61 1.501(6) . ? C52 C53 1.470(8) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.494(7) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C60 1.368(7) . ? C55 C56 1.382(6) . ? C56 C57 1.387(7) . ? C56 H56 0.9400 . ? C57 C58 1.344(9) . ? C57 H57 0.9400 . ? C58 C59 1.364(9) . ? C58 H58 0.9400 . ? C59 C60 1.404(8) . ? C59 H59 0.9400 . ? C60 H60 0.9400 . ? C61 C62 1.368(7) . ? C61 C66 1.387(7) . ? C62 C63 1.396(7) . ? C62 H62 0.9400 . ? C63 C64 1.345(8) . ? C63 H63 0.9400 . ? C64 C65 1.372(8) . ? C64 H64 0.9400 . ? C65 C66 1.391(7) . ? C65 H65 0.9400 . ? C66 H66 0.9400 . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C67 H67C 0.9700 . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C68 H68C 0.9700 . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C69 H69C 0.9700 . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C70 H70C 0.9700 . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C71 H71C 0.9700 . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C72 H72C 0.9700 . ? C73 C74 1.404(6) . ? C73 C78 1.407(7) . ? C74 C75 1.381(7) . ? C74 C79 1.512(6) . ? C75 C76 1.378(7) . ? C75 H75 0.9400 . ? C76 C77 1.370(8) . ? C76 H76 0.9400 . ? C77 C78 1.389(8) . ? C77 H77 0.9400 . ? C78 C82' 1.502(13) . ? C78 C82 1.542(13) . ? C79 C81 1.522(7) . ? C79 C80 1.530(6) . ? C79 H79 0.9900 . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C80 H80C 0.9700 . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C81 H81C 0.9700 . ? C82 C84 1.495(14) . ? C82 C83 1.505(14) . ? C82 H82 0.9900 . ? C82' C84' 1.499(14) . ? C82' C83' 1.500(14) . ? C82' H82' 0.9900 . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C83 H83C 0.9700 . ? C83' H83D 0.9700 . ? C83' H83E 0.9700 . ? C83' H83F 0.9700 . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C84 H84C 0.9700 . ? C84' H84D 0.9700 . ? C84' H84E 0.9700 . ? C84' H84F 0.9700 . ? C85 C86 1.522(6) . ? C86 C91 1.381(6) . ? C86 C87 1.392(7) . ? C87 C88 1.389(7) . ? C87 H87 0.9400 . ? C88 C89 1.370(8) . ? C88 H88 0.9400 . ? C89 C90 1.360(9) . ? C89 H89 0.9400 . ? C90 C91 1.381(7) . ? C90 H90 0.9400 . ? C91 H91 0.9400 . ? C92 C93 1.446(8) . ? C93 C94 1.381(7) . ? C93 C98 1.383(7) . ? C94 C95 1.379(8) . ? C94 H94 0.9400 . ? C95 C96 1.357(8) . ? C95 H95 0.9400 . ? C96 C97 1.369(8) . ? C96 H96 0.9400 . ? C97 C98 1.377(8) . ? C97 H97 0.9400 . ? C98 H98 0.9400 . ? 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 Y1 N2 73.76(14) . . ? N4 Y1 N6 136.93(15) . . ? N2 Y1 N6 138.66(15) . . ? N4 Y1 N5 97.23(15) . . ? N2 Y1 N5 101.21(15) . . ? N6 Y1 N5 56.26(13) . . ? N4 Y1 N1 127.49(13) . . ? N2 Y1 N1 55.81(13) . . ? N6 Y1 N1 94.14(13) . . ? N5 Y1 N1 105.32(13) . . ? N4 Y1 N3 55.88(13) . . ? N2 Y1 N3 127.46(13) . . ? N6 Y1 N3 92.34(13) . . ? N5 Y1 N3 99.10(13) . . ? N1 Y1 N3 154.13(13) . . ? N4 Y1 N7 102.73(16) . . ? N2 Y1 N7 103.91(16) . . ? N6 Y1 N7 95.41(15) . . ? N5 Y1 N7 151.39(14) . . ? N1 Y1 N7 78.35(14) . . ? N3 Y1 N7 76.12(13) . . ? N4 Y1 C2 27.83(13) . . ? N2 Y1 C2 98.85(14) . . ? N6 Y1 C2 119.13(14) . . ? N5 Y1 C2 104.24(14) . . ? N1 Y1 C2 144.21(14) . . ? N3 Y1 C2 28.87(12) . . ? N7 Y1 C2 85.27(15) . . ? N4 Y1 C1 99.60(14) . . ? N2 Y1 C1 27.37(13) . . ? N6 Y1 C1 119.42(14) . . ? N5 Y1 C1 107.05(14) . . ? N1 Y1 C1 28.58(12) . . ? N3 Y1 C1 146.53(13) . . ? N7 Y1 C1 89.71(14) . . ? C2 Y1 C1 121.44(14) . . ? N4 Y1 C36 118.03(15) . . ? N2 Y1 C36 123.97(15) . . ? N6 Y1 C36 27.85(12) . . ? N5 Y1 C36 28.53(12) . . ? N1 Y1 C36 102.74(13) . . ? N3 Y1 C36 94.60(13) . . ? N7 Y1 C36 122.92(14) . . ? C2 Y1 C36 112.86(14) . . ? C1 Y1 C36 118.29(13) . . ? N1 Si1 C19 106.0(2) . . ? N1 Si1 C20 114.3(3) . . ? C19 Si1 C20 108.7(4) . . ? N1 Si1 C18 113.7(3) . . ? C19 Si1 C18 105.6(4) . . ? C20 Si1 C18 108.1(4) . . ? N3 Si2 C23 114.1(2) . . ? N3 Si2 C21 113.6(2) . . ? C23 Si2 C21 108.2(3) . . ? N3 Si2 C22 107.0(2) . . ? C23 Si2 C22 107.4(3) . . ? C21 Si2 C22 106.2(3) . . ? C1 N1 Si1 129.7(3) . . ? C1 N1 Y1 90.9(3) . . ? Si1 N1 Y1 139.14(19) . . ? C1 N2 C3 123.8(4) . . ? C1 N2 Y1 96.7(3) . . ? C3 N2 Y1 138.2(3) . . ? C2 N3 Si2 129.7(3) . . ? C2 N3 Y1 88.9(3) . . ? Si2 N3 Y1 139.0(2) . . ? C2 N4 C5 122.8(4) . . ? C2 N4 Y1 95.9(3) . . ? C5 N4 Y1 137.2(3) . . ? C36 N5 C24 122.5(4) . . ? C36 N5 Y1 94.0(3) . . ? C24 N5 Y1 142.0(3) . . ? C36 N6 Y1 94.8(3) . . ? C36 N6 H6 110(3) . . ? Y1 N6 H6 155(3) . . ? C43 N7 Y1 162.8(4) . . ? N2 C1 N1 116.0(4) . . ? N2 C1 C6 122.6(4) . . ? N1 C1 C6 121.4(4) . . ? N2 C1 Y1 55.9(2) . . ? N1 C1 Y1 60.5(2) . . ? C6 C1 Y1 174.0(3) . . ? N4 C2 N3 116.0(4) . . ? N4 C2 C12 121.8(4) . . ? N3 C2 C12 122.2(4) . . ? N4 C2 Y1 56.2(2) . . ? N3 C2 Y1 62.2(2) . . ? C12 C2 Y1 162.2(4) . . ? N2 C3 C4 110.3(4) . . ? N2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 118.6(6) . . ? C5 C4 H4A 107.7 . . ? C3 C4 H4A 107.7 . . ? C5 C4 H4B 107.7 . . ? C3 C4 H4B 107.7 . . ? H4A C4 H4B 107.1 . . ? C4 C5 N4 111.6(5) . . ? C4 C5 H5A 109.3 . . ? N4 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? N4 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C11 118.8(5) . . ? C7 C6 C1 120.4(5) . . ? C11 C6 C1 120.8(5) . . ? C6 C7 C8 119.7(6) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 121.1(6) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.6(6) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 120.0(6) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C6 C11 C10 120.9(6) . . ? C6 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C17 C12 C13 119.0(5) . . ? C17 C12 C2 120.9(5) . . ? C13 C12 C2 120.0(5) . . ? C12 C13 C14 121.1(5) . . ? C12 C13 H13A 119.4 . . ? C14 C13 H13A 119.4 . . ? C15 C14 C13 119.2(6) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C16 C15 C14 119.7(6) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 121.1(6) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C12 C17 C16 119.8(6) . . ? C12 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 121.1(4) . . ? C25 C24 N5 117.6(4) . . ? C29 C24 N5 121.2(4) . . ? C26 C25 C24 118.0(5) . . ? C26 C25 C30 121.7(5) . . ? C24 C25 C30 120.3(4) . . ? C27 C26 C25 121.3(5) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C28 C27 C26 119.8(5) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 121.9(5) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C28 C29 C24 117.5(5) . . ? C28 C29 C33 120.5(5) . . ? C24 C29 C33 121.8(4) . . ? C25 C30 C32 114.0(4) . . ? C25 C30 C31 112.6(4) . . ? C32 C30 C31 110.3(5) . . ? C25 C30 H30 106.5 . . ? C32 C30 H30 106.5 . . ? C31 C30 H30 106.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C34 114.1(5) . . ? C29 C33 C35 109.0(4) . . ? C34 C33 C35 110.2(4) . . ? C29 C33 H33 107.8 . . ? C34 C33 H33 107.8 . . ? C35 C33 H33 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N6 C36 N5 114.5(4) . . ? N6 C36 C37 121.9(4) . . ? N5 C36 C37 123.6(4) . . ? N6 C36 Y1 57.3(2) . . ? N5 C36 Y1 57.5(2) . . ? C37 C36 Y1 173.4(3) . . ? C38 C37 C42 118.4(5) . . ? C38 C37 C36 118.1(4) . . ? C42 C37 C36 123.5(4) . . ? C37 C38 C39 120.4(5) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 119.9(6) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 120.1(5) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C40 C41 C42 120.3(6) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 120.9(5) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? N7 C43 C44 177.4(6) . . ? C49 C44 C45 120.8(5) . . ? C49 C44 C43 120.2(5) . . ? C45 C44 C43 118.9(5) . . ? C46 C45 C44 118.7(6) . . ? C46 C45 H45 120.7 . . ? C44 C45 H45 120.7 . . ? C47 C46 C45 120.1(6) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C46 C47 C48 121.2(6) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C47 C48 C49 119.5(6) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C44 C49 C48 119.6(6) . . ? C44 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? N9 Y2 N11 73.72(14) . . ? N9 Y2 N13 142.06(15) . . ? N11 Y2 N13 136.92(15) . . ? N9 Y2 N12 112.12(14) . . ? N11 Y2 N12 93.52(14) . . ? N13 Y2 N12 55.94(14) . . ? N9 Y2 N10 121.28(14) . . ? N11 Y2 N10 56.02(13) . . ? N13 Y2 N10 96.65(14) . . ? N12 Y2 N10 100.13(13) . . ? N9 Y2 N8 55.66(13) . . ? N11 Y2 N8 129.37(13) . . ? N13 Y2 N8 90.09(15) . . ? N12 Y2 N8 103.56(13) . . ? N10 Y2 N8 154.99(13) . . ? N9 Y2 N14 99.37(15) . . ? N11 Y2 N14 113.01(15) . . ? N13 Y2 N14 88.06(15) . . ? N12 Y2 N14 143.64(14) . . ? N10 Y2 N14 77.12(14) . . ? N8 Y2 N14 79.08(14) . . ? N9 Y2 C51 94.60(14) . . ? N11 Y2 C51 28.25(13) . . ? N13 Y2 C51 122.55(15) . . ? N12 Y2 C51 103.31(14) . . ? N10 Y2 C51 28.82(12) . . ? N8 Y2 C51 145.88(13) . . ? N14 Y2 C51 91.36(15) . . ? N9 Y2 C85 134.16(14) . . ? N11 Y2 C85 114.70(15) . . ? N13 Y2 C85 27.95(13) . . ? N12 Y2 C85 28.38(13) . . ? N10 Y2 C85 96.07(13) . . ? N8 Y2 C85 100.95(13) . . ? N14 Y2 C85 115.27(15) . . ? C51 Y2 C85 112.65(14) . . ? N9 Y2 C50 27.48(13) . . ? N11 Y2 C50 101.15(14) . . ? N13 Y2 C50 116.56(15) . . ? N12 Y2 C50 109.33(13) . . ? N10 Y2 C50 144.12(14) . . ? N8 Y2 C50 28.22(12) . . ? N14 Y2 C50 90.17(14) . . ? C51 Y2 C50 120.89(14) . . ? C85 Y2 C50 119.57(14) . . ? N8 Si3 C69 112.4(3) . . ? N8 Si3 C67 114.7(3) . . ? C69 Si3 C67 107.4(3) . . ? N8 Si3 C68 108.6(2) . . ? C69 Si3 C68 105.2(3) . . ? C67 Si3 C68 108.0(4) . . ? N10 Si4 C72 106.8(2) . . ? N10 Si4 C71 112.7(2) . . ? C72 Si4 C71 107.3(3) . . ? N10 Si4 C70 114.9(2) . . ? C72 Si4 C70 107.5(3) . . ? C71 Si4 C70 107.2(3) . . ? C50 N8 Si3 129.0(3) . . ? C50 N8 Y2 91.1(3) . . ? Si3 N8 Y2 139.5(2) . . ? C50 N9 C52 124.3(4) . . ? C50 N9 Y2 97.4(3) . . ? C52 N9 Y2 137.4(3) . . ? C51 N10 Si4 129.0(3) . . ? C51 N10 Y2 90.2(3) . . ? Si4 N10 Y2 140.3(2) . . ? C51 N11 C54 120.8(4) . . ? C51 N11 Y2 93.9(3) . . ? C54 N11 Y2 136.9(3) . . ? C85 N12 C73 122.7(4) . . ? C85 N12 Y2 93.9(3) . . ? C73 N12 Y2 141.7(3) . . ? C85 N13 Y2 94.6(3) . . ? C85 N13 H13 115(4) . . ? Y2 N13 H13 149(4) . . ? C92 N14 Y2 170.3(5) . . ? N9 C50 N8 115.7(4) . . ? N9 C50 C55 121.8(4) . . ? N8 C50 C55 122.5(4) . . ? N9 C50 Y2 55.1(2) . . ? N8 C50 Y2 60.7(2) . . ? C55 C50 Y2 175.1(3) . . ? N11 C51 N10 115.7(4) . . ? N11 C51 C61 121.7(4) . . ? N10 C51 C61 122.6(4) . . ? N11 C51 Y2 57.9(2) . . ? N10 C51 Y2 61.0(2) . . ? C61 C51 Y2 160.3(3) . . ? N9 C52 C53 112.2(5) . . ? N9 C52 H52A 109.2 . . ? C53 C52 H52A 109.2 . . ? N9 C52 H52B 109.2 . . ? C53 C52 H52B 109.2 . . ? H52A C52 H52B 107.9 . . ? C52 C53 C54 117.2(5) . . ? C52 C53 H53A 108.0 . . ? C54 C53 H53A 108.0 . . ? C52 C53 H53B 108.0 . . ? C54 C53 H53B 108.0 . . ? H53A C53 H53B 107.3 . . ? N11 C54 C53 111.5(4) . . ? N11 C54 H54A 109.3 . . ? C53 C54 H54A 109.3 . . ? N11 C54 H54B 109.3 . . ? C53 C54 H54B 109.3 . . ? H54A C54 H54B 108.0 . . ? C60 C55 C56 118.6(5) . . ? C60 C55 C50 120.0(5) . . ? C56 C55 C50 121.4(5) . . ? C55 C56 C57 121.1(5) . . ? C55 C56 H56 119.4 . . ? C57 C56 H56 119.4 . . ? C58 C57 C56 119.4(6) . . ? C58 C57 H57 120.3 . . ? C56 C57 H57 120.3 . . ? C57 C58 C59 121.0(6) . . ? C57 C58 H58 119.5 . . ? C59 C58 H58 119.5 . . ? C58 C59 C60 119.8(6) . . ? C58 C59 H59 120.1 . . ? C60 C59 H59 120.1 . . ? C55 C60 C59 119.9(6) . . ? C55 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C62 C61 C66 119.1(5) . . ? C62 C61 C51 120.1(5) . . ? C66 C61 C51 120.7(5) . . ? C61 C62 C63 120.2(5) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C64 C63 C62 120.8(6) . . ? C64 C63 H63 119.6 . . ? C62 C63 H63 119.6 . . ? C63 C64 C65 119.7(6) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? C64 C65 C66 120.6(6) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C61 C66 C65 119.6(6) . . ? C61 C66 H66 120.2 . . ? C65 C66 H66 120.2 . . ? Si3 C67 H67A 109.5 . . ? Si3 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? Si3 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? Si3 C68 H68A 109.5 . . ? Si3 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? Si3 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? Si3 C69 H69A 109.5 . . ? Si3 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? Si3 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? Si4 C70 H70A 109.5 . . ? Si4 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? Si4 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? Si4 C71 H71A 109.5 . . ? Si4 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? Si4 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? Si4 C72 H72A 109.5 . . ? Si4 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? Si4 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 C78 120.6(5) . . ? C74 C73 N12 121.7(4) . . ? C78 C73 N12 117.6(5) . . ? C75 C74 C73 117.9(4) . . ? C75 C74 C79 119.4(5) . . ? C73 C74 C79 122.7(4) . . ? C76 C75 C74 122.3(6) . . ? C76 C75 H75 118.8 . . ? C74 C75 H75 118.8 . . ? C77 C76 C75 118.9(6) . . ? C77 C76 H76 120.6 . . ? C75 C76 H76 120.6 . . ? C76 C77 C78 121.9(5) . . ? C76 C77 H77 119.1 . . ? C78 C77 H77 119.1 . . ? C77 C78 C73 118.1(5) . . ? C77 C78 C82' 115.8(8) . . ? C73 C78 C82' 125.6(8) . . ? C77 C78 C82 125.5(8) . . ? C73 C78 C82 115.8(7) . . ? C82' C78 C82 17.5(8) . . ? C74 C79 C81 110.0(4) . . ? C74 C79 C80 113.3(4) . . ? C81 C79 C80 110.3(4) . . ? C74 C79 H79 107.7 . . ? C81 C79 H79 107.7 . . ? C80 C79 H79 107.7 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C84 C82 C83 113.5(11) . . ? C84 C82 C78 116.5(11) . . ? C83 C82 C78 108.8(10) . . ? C84 C82 H82 105.7 . . ? C83 C82 H82 105.7 . . ? C78 C82 H82 105.7 . . ? C84' C82' C83' 129.8(12) . . ? C84' C82' C78 109.7(10) . . ? C83' C82' C78 119.3(10) . . ? C84' C82' H82' 93.6 . . ? C83' C82' H82' 93.6 . . ? C78 C82' H82' 93.6 . . ? C82' C83' H83D 109.5 . . ? C82' C83' H83E 109.5 . . ? H83D C83' H83E 109.5 . . ? C82' C83' H83F 109.5 . . ? H83D C83' H83F 109.5 . . ? H83E C83' H83F 109.5 . . ? C82' C84' H84D 109.5 . . ? C82' C84' H84E 109.5 . . ? H84D C84' H84E 109.5 . . ? C82' C84' H84F 109.5 . . ? H84D C84' H84F 109.5 . . ? H84E C84' H84F 109.5 . . ? N13 C85 N12 114.0(4) . . ? N13 C85 C86 120.7(4) . . ? N12 C85 C86 125.2(5) . . ? N13 C85 Y2 57.4(3) . . ? N12 C85 Y2 57.7(2) . . ? C86 C85 Y2 168.2(3) . . ? C91 C86 C87 118.5(5) . . ? C91 C86 C85 118.1(5) . . ? C87 C86 C85 123.4(5) . . ? C88 C87 C86 119.5(6) . . ? C88 C87 H87 120.2 . . ? C86 C87 H87 120.2 . . ? C89 C88 C87 121.0(6) . . ? C89 C88 H88 119.5 . . ? C87 C88 H88 119.5 . . ? C90 C89 C88 119.4(6) . . ? C90 C89 H89 120.3 . . ? C88 C89 H89 120.3 . . ? C89 C90 C91 120.6(6) . . ? C89 C90 H90 119.7 . . ? C91 C90 H90 119.7 . . ? C90 C91 C86 120.9(6) . . ? C90 C91 H91 119.6 . . ? C86 C91 H91 119.6 . . ? N14 C92 C93 180.0(7) . . ? C94 C93 C98 120.1(5) . . ? C94 C93 C92 120.2(5) . . ? C98 C93 C92 119.7(5) . . ? C95 C94 C93 119.4(6) . . ? C95 C94 H94 120.3 . . ? C93 C94 H94 120.3 . . ? C96 C95 C94 120.5(6) . . ? C96 C95 H95 119.7 . . ? C94 C95 H95 119.7 . . ? C95 C96 C97 120.3(6) . . ? C95 C96 H96 119.8 . . ? C97 C96 H96 119.8 . . ? C96 C97 C98 120.3(6) . . ? C96 C97 H97 119.8 . . ? C98 C97 H97 119.8 . . ? C97 C98 C93 119.3(6) . . ? C97 C98 H98 120.3 . . ? C93 C98 H98 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 Si1 N1 C1 173.3(5) . . . . ? C20 Si1 N1 C1 53.6(6) . . . . ? C18 Si1 N1 C1 -71.2(6) . . . . ? C19 Si1 N1 Y1 -14.1(5) . . . . ? C20 Si1 N1 Y1 -133.8(4) . . . . ? C18 Si1 N1 Y1 101.4(4) . . . . ? N4 Y1 N1 C1 14.4(4) . . . . ? N2 Y1 N1 C1 -4.3(3) . . . . ? N6 Y1 N1 C1 -153.7(3) . . . . ? N5 Y1 N1 C1 -97.6(3) . . . . ? N3 Y1 N1 C1 102.2(4) . . . . ? N7 Y1 N1 C1 111.6(3) . . . . ? C2 Y1 N1 C1 47.1(4) . . . . ? C36 Y1 N1 C1 -126.9(3) . . . . ? N4 Y1 N1 Si1 -159.9(3) . . . . ? N2 Y1 N1 Si1 -178.6(4) . . . . ? N6 Y1 N1 Si1 32.0(4) . . . . ? N5 Y1 N1 Si1 88.1(3) . . . . ? N3 Y1 N1 Si1 -72.1(5) . . . . ? N7 Y1 N1 Si1 -62.7(3) . . . . ? C2 Y1 N1 Si1 -127.3(3) . . . . ? C1 Y1 N1 Si1 -174.3(5) . . . . ? C36 Y1 N1 Si1 58.8(4) . . . . ? N4 Y1 N2 C1 -160.1(4) . . . . ? N6 Y1 N2 C1 54.7(4) . . . . ? N5 Y1 N2 C1 105.5(3) . . . . ? N1 Y1 N2 C1 4.5(3) . . . . ? N3 Y1 N2 C1 -143.7(3) . . . . ? N7 Y1 N2 C1 -60.7(4) . . . . ? C2 Y1 N2 C1 -148.0(3) . . . . ? C36 Y1 N2 C1 86.7(4) . . . . ? N4 Y1 N2 C3 6.1(6) . . . . ? N6 Y1 N2 C3 -139.1(6) . . . . ? N5 Y1 N2 C3 -88.3(6) . . . . ? N1 Y1 N2 C3 170.7(7) . . . . ? N3 Y1 N2 C3 22.5(7) . . . . ? N7 Y1 N2 C3 105.6(6) . . . . ? C2 Y1 N2 C3 18.3(6) . . . . ? C1 Y1 N2 C3 166.2(8) . . . . ? C36 Y1 N2 C3 -107.1(6) . . . . ? C23 Si2 N3 C2 52.4(5) . . . . ? C21 Si2 N3 C2 -72.2(5) . . . . ? C22 Si2 N3 C2 171.0(4) . . . . ? C23 Si2 N3 Y1 -104.1(3) . . . . ? C21 Si2 N3 Y1 131.3(3) . . . . ? C22 Si2 N3 Y1 14.5(4) . . . . ? N4 Y1 N3 C2 10.4(3) . . . . ? N2 Y1 N3 C2 -8.8(4) . . . . ? N6 Y1 N3 C2 159.2(3) . . . . ? N5 Y1 N3 C2 103.0(3) . . . . ? N1 Y1 N3 C2 -96.3(4) . . . . ? N7 Y1 N3 C2 -105.8(3) . . . . ? C1 Y1 N3 C2 -38.3(4) . . . . ? C36 Y1 N3 C2 131.4(3) . . . . ? N4 Y1 N3 Si2 172.5(4) . . . . ? N2 Y1 N3 Si2 153.4(3) . . . . ? N6 Y1 N3 Si2 -38.7(3) . . . . ? N5 Y1 N3 Si2 -94.9(3) . . . . ? N1 Y1 N3 Si2 65.8(5) . . . . ? N7 Y1 N3 Si2 56.3(3) . . . . ? C2 Y1 N3 Si2 162.1(5) . . . . ? C1 Y1 N3 Si2 123.8(3) . . . . ? C36 Y1 N3 Si2 -66.5(3) . . . . ? N2 Y1 N4 C2 153.5(4) . . . . ? N6 Y1 N4 C2 -60.0(4) . . . . ? N5 Y1 N4 C2 -106.9(3) . . . . ? N1 Y1 N4 C2 137.5(3) . . . . ? N3 Y1 N4 C2 -10.8(3) . . . . ? N7 Y1 N4 C2 52.5(4) . . . . ? C1 Y1 N4 C2 144.4(3) . . . . ? C36 Y1 N4 C2 -86.2(4) . . . . ? N2 Y1 N4 C5 -2.6(6) . . . . ? N6 Y1 N4 C5 143.9(5) . . . . ? N5 Y1 N4 C5 97.0(6) . . . . ? N1 Y1 N4 C5 -18.6(7) . . . . ? N3 Y1 N4 C5 -166.9(7) . . . . ? N7 Y1 N4 C5 -103.6(6) . . . . ? C2 Y1 N4 C5 -156.1(8) . . . . ? C1 Y1 N4 C5 -11.7(6) . . . . ? C36 Y1 N4 C5 117.7(6) . . . . ? N4 Y1 N5 C36 139.3(3) . . . . ? N2 Y1 N5 C36 -145.9(3) . . . . ? N6 Y1 N5 C36 -3.9(2) . . . . ? N1 Y1 N5 C36 -88.6(3) . . . . ? N3 Y1 N5 C36 82.8(3) . . . . ? N7 Y1 N5 C36 5.2(4) . . . . ? C2 Y1 N5 C36 111.9(3) . . . . ? C1 Y1 N5 C36 -118.3(3) . . . . ? N4 Y1 N5 C24 -24.7(5) . . . . ? N2 Y1 N5 C24 50.1(5) . . . . ? N6 Y1 N5 C24 -167.9(5) . . . . ? N1 Y1 N5 C24 107.5(5) . . . . ? N3 Y1 N5 C24 -81.1(5) . . . . ? N7 Y1 N5 C24 -158.8(4) . . . . ? C2 Y1 N5 C24 -52.1(5) . . . . ? C1 Y1 N5 C24 77.7(5) . . . . ? C36 Y1 N5 C24 -164.0(6) . . . . ? N4 Y1 N6 C36 -56.5(4) . . . . ? N2 Y1 N6 C36 70.1(4) . . . . ? N5 Y1 N6 C36 4.0(2) . . . . ? N1 Y1 N6 C36 109.7(3) . . . . ? N3 Y1 N6 C36 -95.4(3) . . . . ? N7 Y1 N6 C36 -171.7(3) . . . . ? C2 Y1 N6 C36 -84.1(3) . . . . ? C1 Y1 N6 C36 95.6(3) . . . . ? N4 Y1 N7 C43 -140.4(14) . . . . ? N2 Y1 N7 C43 143.4(14) . . . . ? N6 Y1 N7 C43 0.2(14) . . . . ? N5 Y1 N7 C43 -7.3(15) . . . . ? N1 Y1 N7 C43 93.4(14) . . . . ? N3 Y1 N7 C43 -90.8(14) . . . . ? C2 Y1 N7 C43 -118.6(14) . . . . ? C1 Y1 N7 C43 119.8(14) . . . . ? C36 Y1 N7 C43 -4.4(14) . . . . ? C3 N2 C1 N1 -176.5(5) . . . . ? Y1 N2 C1 N1 -7.5(5) . . . . ? C3 N2 C1 C6 4.1(8) . . . . ? Y1 N2 C1 C6 173.1(4) . . . . ? C3 N2 C1 Y1 -169.0(6) . . . . ? Si1 N1 C1 N2 -177.7(4) . . . . ? Y1 N1 C1 N2 7.2(5) . . . . ? Si1 N1 C1 C6 1.7(7) . . . . ? Y1 N1 C1 C6 -173.5(4) . . . . ? Si1 N1 C1 Y1 175.2(5) . . . . ? N4 Y1 C1 N2 19.3(4) . . . . ? N6 Y1 C1 N2 -141.8(3) . . . . ? N5 Y1 C1 N2 -81.4(3) . . . . ? N1 Y1 C1 N2 -172.2(5) . . . . ? N3 Y1 C1 N2 58.5(4) . . . . ? N7 Y1 C1 N2 122.2(4) . . . . ? C2 Y1 C1 N2 37.9(4) . . . . ? C36 Y1 C1 N2 -109.9(3) . . . . ? N4 Y1 C1 N1 -168.5(3) . . . . ? N2 Y1 C1 N1 172.2(5) . . . . ? N6 Y1 C1 N1 30.4(3) . . . . ? N5 Y1 C1 N1 90.8(3) . . . . ? N3 Y1 C1 N1 -129.3(3) . . . . ? N7 Y1 C1 N1 -65.6(3) . . . . ? C2 Y1 C1 N1 -149.9(3) . . . . ? C36 Y1 C1 N1 62.3(3) . . . . ? N4 Y1 C1 C6 -58(3) . . . . ? N2 Y1 C1 C6 -77(3) . . . . ? N6 Y1 C1 C6 141(3) . . . . ? N5 Y1 C1 C6 -158(3) . . . . ? N1 Y1 C1 C6 111(3) . . . . ? N3 Y1 C1 C6 -18(3) . . . . ? N7 Y1 C1 C6 45(3) . . . . ? C2 Y1 C1 C6 -39(3) . . . . ? C36 Y1 C1 C6 173(3) . . . . ? C5 N4 C2 N3 179.2(5) . . . . ? Y1 N4 C2 N3 18.4(5) . . . . ? C5 N4 C2 C12 1.9(8) . . . . ? Y1 N4 C2 C12 -159.0(4) . . . . ? C5 N4 C2 Y1 160.9(6) . . . . ? Si2 N3 C2 N4 177.9(4) . . . . ? Y1 N3 C2 N4 -17.2(5) . . . . ? Si2 N3 C2 C12 -4.7(7) . . . . ? Y1 N3 C2 C12 160.1(4) . . . . ? Si2 N3 C2 Y1 -164.8(4) . . . . ? N2 Y1 C2 N4 -25.7(4) . . . . ? N6 Y1 C2 N4 137.4(3) . . . . ? N5 Y1 C2 N4 78.3(3) . . . . ? N1 Y1 C2 N4 -66.5(4) . . . . ? N3 Y1 C2 N4 161.3(5) . . . . ? N7 Y1 C2 N4 -129.1(4) . . . . ? C1 Y1 C2 N4 -42.3(4) . . . . ? C36 Y1 C2 N4 107.1(3) . . . . ? N4 Y1 C2 N3 -161.3(5) . . . . ? N2 Y1 C2 N3 173.0(3) . . . . ? N6 Y1 C2 N3 -24.0(3) . . . . ? N5 Y1 C2 N3 -83.0(3) . . . . ? N1 Y1 C2 N3 132.1(3) . . . . ? N7 Y1 C2 N3 69.6(3) . . . . ? C1 Y1 C2 N3 156.4(3) . . . . ? C36 Y1 C2 N3 -54.2(3) . . . . ? N4 Y1 C2 C12 89.4(11) . . . . ? N2 Y1 C2 C12 63.7(11) . . . . ? N6 Y1 C2 C12 -133.2(11) . . . . ? N5 Y1 C2 C12 167.8(11) . . . . ? N1 Y1 C2 C12 22.9(12) . . . . ? N3 Y1 C2 C12 -109.2(12) . . . . ? N7 Y1 C2 C12 -39.6(11) . . . . ? C1 Y1 C2 C12 47.1(11) . . . . ? C36 Y1 C2 C12 -163.5(11) . . . . ? C1 N2 C3 C4 -176.6(6) . . . . ? Y1 N2 C3 C4 20.0(9) . . . . ? N2 C3 C4 C5 -61.2(8) . . . . ? C3 C4 C5 N4 65.1(9) . . . . ? C2 N4 C5 C4 -178.9(6) . . . . ? Y1 N4 C5 C4 -27.5(9) . . . . ? N2 C1 C6 C7 78.5(7) . . . . ? N1 C1 C6 C7 -100.9(6) . . . . ? Y1 C1 C6 C7 152(3) . . . . ? N2 C1 C6 C11 -102.8(7) . . . . ? N1 C1 C6 C11 77.8(6) . . . . ? Y1 C1 C6 C11 -30(4) . . . . ? C11 C6 C7 C8 -1.2(8) . . . . ? C1 C6 C7 C8 177.5(5) . . . . ? C6 C7 C8 C9 -0.2(10) . . . . ? C7 C8 C9 C10 2.0(11) . . . . ? C8 C9 C10 C11 -2.3(11) . . . . ? C7 C6 C11 C10 0.8(9) . . . . ? C1 C6 C11 C10 -177.9(5) . . . . ? C9 C10 C11 C6 1.0(10) . . . . ? N4 C2 C12 C17 -100.8(6) . . . . ? N3 C2 C12 C17 82.0(6) . . . . ? Y1 C2 C12 C17 -178.8(9) . . . . ? N4 C2 C12 C13 77.3(7) . . . . ? N3 C2 C12 C13 -99.9(6) . . . . ? Y1 C2 C12 C13 -0.7(14) . . . . ? C17 C12 C13 C14 -1.5(8) . . . . ? C2 C12 C13 C14 -179.6(5) . . . . ? C12 C13 C14 C15 0.9(9) . . . . ? C13 C14 C15 C16 -0.3(9) . . . . ? C14 C15 C16 C17 0.4(9) . . . . ? C13 C12 C17 C16 1.5(8) . . . . ? C2 C12 C17 C16 179.6(5) . . . . ? C15 C16 C17 C12 -1.0(9) . . . . ? C36 N5 C24 C25 116.3(5) . . . . ? Y1 N5 C24 C25 -82.7(6) . . . . ? C36 N5 C24 C29 -65.5(6) . . . . ? Y1 N5 C24 C29 95.5(5) . . . . ? C29 C24 C25 C26 5.5(6) . . . . ? N5 C24 C25 C26 -176.3(4) . . . . ? C29 C24 C25 C30 -175.5(4) . . . . ? N5 C24 C25 C30 2.7(6) . . . . ? C24 C25 C26 C27 -0.2(7) . . . . ? C30 C25 C26 C27 -179.2(4) . . . . ? C25 C26 C27 C28 -3.3(8) . . . . ? C26 C27 C28 C29 1.6(8) . . . . ? C27 C28 C29 C24 3.4(7) . . . . ? C27 C28 C29 C33 -171.7(5) . . . . ? C25 C24 C29 C28 -7.0(6) . . . . ? N5 C24 C29 C28 174.8(4) . . . . ? C25 C24 C29 C33 168.1(4) . . . . ? N5 C24 C29 C33 -10.1(6) . . . . ? C26 C25 C30 C32 -25.9(7) . . . . ? C24 C25 C30 C32 155.1(5) . . . . ? C26 C25 C30 C31 100.6(5) . . . . ? C24 C25 C30 C31 -78.3(6) . . . . ? C28 C29 C33 C34 -49.3(6) . . . . ? C24 C29 C33 C34 135.7(5) . . . . ? C28 C29 C33 C35 74.4(6) . . . . ? C24 C29 C33 C35 -100.6(5) . . . . ? Y1 N6 C36 N5 -6.4(4) . . . . ? Y1 N6 C36 C37 172.2(4) . . . . ? C24 N5 C36 N6 174.8(4) . . . . ? Y1 N5 C36 N6 6.4(4) . . . . ? C24 N5 C36 C37 -3.8(6) . . . . ? Y1 N5 C36 C37 -172.2(4) . . . . ? C24 N5 C36 Y1 168.4(4) . . . . ? N4 Y1 C36 N6 139.8(3) . . . . ? N2 Y1 C36 N6 -131.5(3) . . . . ? N5 Y1 C36 N6 -173.1(4) . . . . ? N1 Y1 C36 N6 -74.4(3) . . . . ? N3 Y1 C36 N6 86.3(3) . . . . ? N7 Y1 C36 N6 9.9(3) . . . . ? C2 Y1 C36 N6 109.5(3) . . . . ? C1 Y1 C36 N6 -100.1(3) . . . . ? N4 Y1 C36 N5 -47.1(3) . . . . ? N2 Y1 C36 N5 41.5(3) . . . . ? N6 Y1 C36 N5 173.1(4) . . . . ? N1 Y1 C36 N5 98.7(3) . . . . ? N3 Y1 C36 N5 -100.6(3) . . . . ? N7 Y1 C36 N5 -177.1(2) . . . . ? C2 Y1 C36 N5 -77.5(3) . . . . ? C1 Y1 C36 N5 73.0(3) . . . . ? N4 Y1 C36 C37 55(3) . . . . ? N2 Y1 C36 C37 143(3) . . . . ? N6 Y1 C36 C37 -85(3) . . . . ? N5 Y1 C36 C37 102(3) . . . . ? N1 Y1 C36 C37 -159(3) . . . . ? N3 Y1 C36 C37 1(3) . . . . ? N7 Y1 C36 C37 -75(3) . . . . ? C2 Y1 C36 C37 24(3) . . . . ? C1 Y1 C36 C37 175(3) . . . . ? N6 C36 C37 C38 -34.2(6) . . . . ? N5 C36 C37 C38 144.3(4) . . . . ? Y1 C36 C37 C38 47(3) . . . . ? N6 C36 C37 C42 144.2(5) . . . . ? N5 C36 C37 C42 -37.3(7) . . . . ? Y1 C36 C37 C42 -135(3) . . . . ? C42 C37 C38 C39 1.3(7) . . . . ? C36 C37 C38 C39 179.8(5) . . . . ? C37 C38 C39 C40 -1.1(8) . . . . ? C38 C39 C40 C41 0.0(9) . . . . ? C39 C40 C41 C42 0.7(8) . . . . ? C40 C41 C42 C37 -0.4(8) . . . . ? C38 C37 C42 C41 -0.6(7) . . . . ? C36 C37 C42 C41 -179.0(4) . . . . ? Y1 N7 C43 C44 -26(15) . . . . ? N7 C43 C44 C49 82(14) . . . . ? N7 C43 C44 C45 -96(14) . . . . ? C49 C44 C45 C46 -1.1(8) . . . . ? C43 C44 C45 C46 177.2(5) . . . . ? C44 C45 C46 C47 -0.6(9) . . . . ? C45 C46 C47 C48 1.4(9) . . . . ? C46 C47 C48 C49 -0.6(9) . . . . ? C45 C44 C49 C48 1.9(8) . . . . ? C43 C44 C49 C48 -176.3(5) . . . . ? C47 C48 C49 C44 -1.1(8) . . . . ? C69 Si3 N8 C50 88.6(5) . . . . ? C67 Si3 N8 C50 -34.5(5) . . . . ? C68 Si3 N8 C50 -155.4(5) . . . . ? C69 Si3 N8 Y2 -100.2(4) . . . . ? C67 Si3 N8 Y2 136.7(4) . . . . ? C68 Si3 N8 Y2 15.8(5) . . . . ? N9 Y2 N8 C50 2.0(3) . . . . ? N11 Y2 N8 C50 0.5(3) . . . . ? N13 Y2 N8 C50 -160.5(3) . . . . ? N12 Y2 N8 C50 -105.7(3) . . . . ? N10 Y2 N8 C50 93.4(4) . . . . ? N14 Y2 N8 C50 111.4(3) . . . . ? C51 Y2 N8 C50 35.4(4) . . . . ? C85 Y2 N8 C50 -134.6(3) . . . . ? N9 Y2 N8 Si3 -171.1(4) . . . . ? N11 Y2 N8 Si3 -172.6(3) . . . . ? N13 Y2 N8 Si3 26.3(3) . . . . ? N12 Y2 N8 Si3 81.1(3) . . . . ? N10 Y2 N8 Si3 -79.8(5) . . . . ? N14 Y2 N8 Si3 -61.7(3) . . . . ? C51 Y2 N8 Si3 -137.7(3) . . . . ? C85 Y2 N8 Si3 52.2(3) . . . . ? C50 Y2 N8 Si3 -173.2(5) . . . . ? N11 Y2 N9 C50 176.7(3) . . . . ? N13 Y2 N9 C50 27.1(4) . . . . ? N12 Y2 N9 C50 89.6(3) . . . . ? N10 Y2 N9 C50 -152.4(3) . . . . ? N8 Y2 N9 C50 -2.1(3) . . . . ? N14 Y2 N9 C50 -71.9(3) . . . . ? C51 Y2 N9 C50 -164.0(3) . . . . ? C85 Y2 N9 C50 67.9(4) . . . . ? N11 Y2 N9 C52 7.8(5) . . . . ? N13 Y2 N9 C52 -141.9(5) . . . . ? N12 Y2 N9 C52 -79.4(6) . . . . ? N10 Y2 N9 C52 38.6(6) . . . . ? N8 Y2 N9 C52 -171.1(6) . . . . ? N14 Y2 N9 C52 119.1(5) . . . . ? C51 Y2 N9 C52 27.0(6) . . . . ? C85 Y2 N9 C52 -101.1(6) . . . . ? C50 Y2 N9 C52 -169.0(7) . . . . ? C72 Si4 N10 C51 -168.5(5) . . . . ? C71 Si4 N10 C51 -50.8(5) . . . . ? C70 Si4 N10 C51 72.4(5) . . . . ? C72 Si4 N10 Y2 22.2(5) . . . . ? C71 Si4 N10 Y2 139.8(4) . . . . ? C70 Si4 N10 Y2 -97.0(4) . . . . ? N9 Y2 N10 C51 -24.6(3) . . . . ? N11 Y2 N10 C51 11.8(3) . . . . ? N13 Y2 N10 C51 155.7(3) . . . . ? N12 Y2 N10 C51 99.2(3) . . . . ? N8 Y2 N10 C51 -99.6(4) . . . . ? N14 Y2 N10 C51 -117.8(3) . . . . ? C85 Y2 N10 C51 127.6(3) . . . . ? C50 Y2 N10 C51 -45.9(4) . . . . ? N9 Y2 N10 Si4 147.2(3) . . . . ? N11 Y2 N10 Si4 -176.4(4) . . . . ? N13 Y2 N10 Si4 -32.5(4) . . . . ? N12 Y2 N10 Si4 -89.0(3) . . . . ? N8 Y2 N10 Si4 72.2(5) . . . . ? N14 Y2 N10 Si4 54.0(3) . . . . ? C51 Y2 N10 Si4 171.8(5) . . . . ? C85 Y2 N10 Si4 -60.6(3) . . . . ? C50 Y2 N10 Si4 125.8(3) . . . . ? N9 Y2 N11 C51 136.1(3) . . . . ? N13 Y2 N11 C51 -71.0(4) . . . . ? N12 Y2 N11 C51 -111.9(3) . . . . ? N10 Y2 N11 C51 -12.0(3) . . . . ? N8 Y2 N11 C51 137.3(3) . . . . ? N14 Y2 N11 C51 42.6(3) . . . . ? C85 Y2 N11 C51 -92.3(3) . . . . ? C50 Y2 N11 C51 137.6(3) . . . . ? N9 Y2 N11 C54 -9.3(5) . . . . ? N13 Y2 N11 C54 143.6(5) . . . . ? N12 Y2 N11 C54 102.7(5) . . . . ? N10 Y2 N11 C54 -157.5(6) . . . . ? N8 Y2 N11 C54 -8.1(6) . . . . ? N14 Y2 N11 C54 -102.8(5) . . . . ? C51 Y2 N11 C54 -145.4(7) . . . . ? C85 Y2 N11 C54 122.3(5) . . . . ? C50 Y2 N11 C54 -7.8(5) . . . . ? N9 Y2 N12 C85 -146.1(3) . . . . ? N11 Y2 N12 C85 140.1(3) . . . . ? N13 Y2 N12 C85 -7.2(3) . . . . ? N10 Y2 N12 C85 84.0(3) . . . . ? N8 Y2 N12 C85 -88.0(3) . . . . ? N14 Y2 N12 C85 2.0(4) . . . . ? C51 Y2 N12 C85 113.2(3) . . . . ? C50 Y2 N12 C85 -116.8(3) . . . . ? N9 Y2 N12 C73 50.3(5) . . . . ? N11 Y2 N12 C73 -23.6(5) . . . . ? N13 Y2 N12 C73 -170.9(5) . . . . ? N10 Y2 N12 C73 -79.7(5) . . . . ? N8 Y2 N12 C73 108.4(5) . . . . ? N14 Y2 N12 C73 -161.7(4) . . . . ? C51 Y2 N12 C73 -50.4(5) . . . . ? C85 Y2 N12 C73 -163.7(7) . . . . ? C50 Y2 N12 C73 79.5(5) . . . . ? N9 Y2 N13 C85 90.0(4) . . . . ? N11 Y2 N13 C85 -44.8(4) . . . . ? N12 Y2 N13 C85 7.3(3) . . . . ? N10 Y2 N13 C85 -90.4(3) . . . . ? N8 Y2 N13 C85 113.7(3) . . . . ? N14 Y2 N13 C85 -167.2(3) . . . . ? C51 Y2 N13 C85 -76.8(3) . . . . ? C50 Y2 N13 C85 103.6(3) . . . . ? N9 Y2 N14 C92 139(3) . . . . ? N11 Y2 N14 C92 -145(3) . . . . ? N13 Y2 N14 C92 -3(3) . . . . ? N12 Y2 N14 C92 -11(3) . . . . ? N10 Y2 N14 C92 -101(3) . . . . ? N8 Y2 N14 C92 87(3) . . . . ? C51 Y2 N14 C92 -126(3) . . . . ? C85 Y2 N14 C92 -10(3) . . . . ? C50 Y2 N14 C92 113(3) . . . . ? C52 N9 C50 N8 174.5(5) . . . . ? Y2 N9 C50 N8 3.5(5) . . . . ? C52 N9 C50 C55 -4.6(8) . . . . ? Y2 N9 C50 C55 -175.5(4) . . . . ? C52 N9 C50 Y2 171.0(6) . . . . ? Si3 N8 C50 N9 171.0(4) . . . . ? Y2 N8 C50 N9 -3.3(4) . . . . ? Si3 N8 C50 C55 -10.0(7) . . . . ? Y2 N8 C50 C55 175.7(4) . . . . ? Si3 N8 C50 Y2 174.3(4) . . . . ? N11 Y2 C50 N9 -3.2(3) . . . . ? N13 Y2 C50 N9 -161.8(3) . . . . ? N12 Y2 C50 N9 -101.0(3) . . . . ? N10 Y2 C50 N9 42.4(4) . . . . ? N8 Y2 C50 N9 176.4(5) . . . . ? N14 Y2 C50 N9 110.3(3) . . . . ? C51 Y2 C50 N9 18.6(4) . . . . ? C85 Y2 C50 N9 -130.2(3) . . . . ? N9 Y2 C50 N8 -176.4(5) . . . . ? N11 Y2 C50 N8 -179.6(3) . . . . ? N13 Y2 C50 N8 21.9(3) . . . . ? N12 Y2 C50 N8 82.6(3) . . . . ? N10 Y2 C50 N8 -133.9(3) . . . . ? N14 Y2 C50 N8 -66.0(3) . . . . ? C51 Y2 C50 N8 -157.7(3) . . . . ? C85 Y2 C50 N8 53.5(3) . . . . ? N9 Y2 C50 C55 51(4) . . . . ? N11 Y2 C50 C55 48(4) . . . . ? N13 Y2 C50 C55 -110(4) . . . . ? N12 Y2 C50 C55 -50(4) . . . . ? N10 Y2 C50 C55 94(4) . . . . ? N8 Y2 C50 C55 -132(4) . . . . ? N14 Y2 C50 C55 162(4) . . . . ? C51 Y2 C50 C55 70(4) . . . . ? C85 Y2 C50 C55 -79(4) . . . . ? C54 N11 C51 N10 173.5(4) . . . . ? Y2 N11 C51 N10 20.4(4) . . . . ? C54 N11 C51 C61 -3.6(7) . . . . ? Y2 N11 C51 C61 -156.7(4) . . . . ? C54 N11 C51 Y2 153.1(5) . . . . ? Si4 N10 C51 N11 167.1(4) . . . . ? Y2 N10 C51 N11 -19.7(4) . . . . ? Si4 N10 C51 C61 -15.8(7) . . . . ? Y2 N10 C51 C61 157.4(4) . . . . ? Si4 N10 C51 Y2 -173.2(4) . . . . ? N9 Y2 C51 N11 -41.9(3) . . . . ? N13 Y2 C51 N11 130.0(3) . . . . ? N12 Y2 C51 N11 72.1(3) . . . . ? N10 Y2 C51 N11 159.0(5) . . . . ? N8 Y2 C51 N11 -69.0(4) . . . . ? N14 Y2 C51 N11 -141.4(3) . . . . ? C85 Y2 C51 N11 100.4(3) . . . . ? C50 Y2 C51 N11 -50.4(3) . . . . ? N9 Y2 C51 N10 159.1(3) . . . . ? N11 Y2 C51 N10 -159.0(5) . . . . ? N13 Y2 C51 N10 -29.0(3) . . . . ? N12 Y2 C51 N10 -86.8(3) . . . . ? N8 Y2 C51 N10 132.0(3) . . . . ? N14 Y2 C51 N10 59.6(3) . . . . ? C85 Y2 C51 N10 -58.6(3) . . . . ? C50 Y2 C51 N10 150.6(3) . . . . ? N9 Y2 C51 C61 52.9(10) . . . . ? N11 Y2 C51 C61 94.8(11) . . . . ? N13 Y2 C51 C61 -135.2(10) . . . . ? N12 Y2 C51 C61 167.0(10) . . . . ? N10 Y2 C51 C61 -106.2(11) . . . . ? N8 Y2 C51 C61 25.8(11) . . . . ? N14 Y2 C51 C61 -46.6(10) . . . . ? C85 Y2 C51 C61 -164.8(10) . . . . ? C50 Y2 C51 C61 44.4(11) . . . . ? C50 N9 C52 C53 -143.9(6) . . . . ? Y2 N9 C52 C53 22.8(8) . . . . ? N9 C52 C53 C54 -64.1(7) . . . . ? C51 N11 C54 C53 -158.0(5) . . . . ? Y2 N11 C54 C53 -19.2(8) . . . . ? C52 C53 C54 N11 62.1(7) . . . . ? N9 C50 C55 C60 -63.8(7) . . . . ? N8 C50 C55 C60 117.2(6) . . . . ? Y2 C50 C55 C60 -113(4) . . . . ? N9 C50 C55 C56 116.8(6) . . . . ? N8 C50 C55 C56 -62.1(7) . . . . ? Y2 C50 C55 C56 68(4) . . . . ? C60 C55 C56 C57 -2.4(8) . . . . ? C50 C55 C56 C57 177.0(5) . . . . ? C55 C56 C57 C58 1.3(9) . . . . ? C56 C57 C58 C59 0.1(11) . . . . ? C57 C58 C59 C60 -0.4(12) . . . . ? C56 C55 C60 C59 2.0(9) . . . . ? C50 C55 C60 C59 -177.4(6) . . . . ? C58 C59 C60 C55 -0.7(11) . . . . ? N11 C51 C61 C62 105.9(6) . . . . ? N10 C51 C61 C62 -71.0(6) . . . . ? Y2 C51 C61 C62 23.5(13) . . . . ? N11 C51 C61 C66 -71.7(7) . . . . ? N10 C51 C61 C66 111.4(6) . . . . ? Y2 C51 C61 C66 -154.1(8) . . . . ? C66 C61 C62 C63 0.2(8) . . . . ? C51 C61 C62 C63 -177.4(5) . . . . ? C61 C62 C63 C64 -1.3(9) . . . . ? C62 C63 C64 C65 1.4(9) . . . . ? C63 C64 C65 C66 -0.5(10) . . . . ? C62 C61 C66 C65 0.6(8) . . . . ? C51 C61 C66 C65 178.3(5) . . . . ? C64 C65 C66 C61 -0.5(9) . . . . ? C85 N12 C73 C74 -75.2(6) . . . . ? Y2 N12 C73 C74 85.3(6) . . . . ? C85 N12 C73 C78 106.2(5) . . . . ? Y2 N12 C73 C78 -93.3(6) . . . . ? C78 C73 C74 C75 -5.1(7) . . . . ? N12 C73 C74 C75 176.4(4) . . . . ? C78 C73 C74 C79 172.1(5) . . . . ? N12 C73 C74 C79 -6.5(7) . . . . ? C73 C74 C75 C76 1.3(8) . . . . ? C79 C74 C75 C76 -175.9(5) . . . . ? C74 C75 C76 C77 2.5(9) . . . . ? C75 C76 C77 C78 -2.8(9) . . . . ? C76 C77 C78 C73 -0.9(9) . . . . ? C76 C77 C78 C82' -173.4(7) . . . . ? C76 C77 C78 C82 169.7(8) . . . . ? C74 C73 C78 C77 4.8(8) . . . . ? N12 C73 C78 C77 -176.5(5) . . . . ? C74 C73 C78 C82' 176.5(7) . . . . ? N12 C73 C78 C82' -4.8(9) . . . . ? C74 C73 C78 C82 -166.6(7) . . . . ? N12 C73 C78 C82 12.0(8) . . . . ? C75 C74 C79 C81 63.3(6) . . . . ? C73 C74 C79 C81 -113.8(5) . . . . ? C75 C74 C79 C80 -60.7(6) . . . . ? C73 C74 C79 C80 122.2(5) . . . . ? C77 C78 C82 C84 -33.3(15) . . . . ? C73 C78 C82 C84 137.4(10) . . . . ? C82' C78 C82 C84 -94(4) . . . . ? C77 C78 C82 C83 96.7(12) . . . . ? C73 C78 C82 C83 -92.6(11) . . . . ? C82' C78 C82 C83 36(3) . . . . ? C77 C78 C82' C84' -106.1(12) . . . . ? C73 C78 C82' C84' 82.0(13) . . . . ? C82 C78 C82' C84' 22(3) . . . . ? C77 C78 C82' C83' 85.0(14) . . . . ? C73 C78 C82' C83' -86.8(14) . . . . ? C82 C78 C82' C83' -147(4) . . . . ? Y2 N13 C85 N12 -11.9(4) . . . . ? Y2 N13 C85 C86 166.3(4) . . . . ? C73 N12 C85 N13 179.9(4) . . . . ? Y2 N12 C85 N13 11.9(4) . . . . ? C73 N12 C85 C86 1.8(7) . . . . ? Y2 N12 C85 C86 -166.2(4) . . . . ? C73 N12 C85 Y2 168.0(5) . . . . ? N9 Y2 C85 N13 -121.0(3) . . . . ? N11 Y2 C85 N13 148.0(3) . . . . ? N12 Y2 C85 N13 -167.1(5) . . . . ? N10 Y2 C85 N13 92.8(3) . . . . ? N8 Y2 C85 N13 -68.8(3) . . . . ? N14 Y2 C85 N13 14.2(3) . . . . ? C51 Y2 C85 N13 117.2(3) . . . . ? C50 Y2 C85 N13 -91.6(3) . . . . ? N9 Y2 C85 N12 46.1(4) . . . . ? N11 Y2 C85 N12 -44.8(3) . . . . ? N13 Y2 C85 N12 167.1(5) . . . . ? N10 Y2 C85 N12 -100.1(3) . . . . ? N8 Y2 C85 N12 98.3(3) . . . . ? N14 Y2 C85 N12 -178.7(3) . . . . ? C51 Y2 C85 N12 -75.7(3) . . . . ? C50 Y2 C85 N12 75.5(3) . . . . ? N9 Y2 C85 C86 154.4(16) . . . . ? N11 Y2 C85 C86 63.4(17) . . . . ? N13 Y2 C85 C86 -84.6(17) . . . . ? N12 Y2 C85 C86 108.3(18) . . . . ? N10 Y2 C85 C86 8.1(17) . . . . ? N8 Y2 C85 C86 -153.4(17) . . . . ? N14 Y2 C85 C86 -70.4(17) . . . . ? C51 Y2 C85 C86 32.6(18) . . . . ? C50 Y2 C85 C86 -176.2(17) . . . . ? N13 C85 C86 C91 -33.4(7) . . . . ? N12 C85 C86 C91 144.6(5) . . . . ? Y2 C85 C86 C91 44.0(19) . . . . ? N13 C85 C86 C87 148.3(5) . . . . ? N12 C85 C86 C87 -33.8(7) . . . . ? Y2 C85 C86 C87 -134.3(15) . . . . ? C91 C86 C87 C88 -0.4(8) . . . . ? C85 C86 C87 C88 177.9(5) . . . . ? C86 C87 C88 C89 -0.4(9) . . . . ? C87 C88 C89 C90 1.2(9) . . . . ? C88 C89 C90 C91 -1.3(9) . . . . ? C89 C90 C91 C86 0.5(9) . . . . ? C87 C86 C91 C90 0.3(8) . . . . ? C85 C86 C91 C90 -178.1(5) . . . . ? Y2 N14 C92 C93 -97(100) . . . . ? N14 C92 C93 C94 -22(100) . . . . ? N14 C92 C93 C98 158(100) . . . . ? C98 C93 C94 C95 0.4(9) . . . . ? C92 C93 C94 C95 -179.7(5) . . . . ? C93 C94 C95 C96 -0.6(10) . . . . ? C94 C95 C96 C97 0.0(10) . . . . ? C95 C96 C97 C98 0.9(10) . . . . ? C96 C97 C98 C93 -1.1(9) . . . . ? C94 C93 C98 C97 0.5(8) . . . . ? C92 C93 C98 C97 -179.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.673 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.066 # Attachment '- shelxl 9.cif' data_shelxl9 _database_code_depnum_ccdc_archive 'CCDC 862447' #TrackingRef '- shelxl 9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H62 N7 Si2 Yb, C7 H8' _chemical_formula_sum 'C56 H70 N7 Si2 Yb' _chemical_formula_weight 1070.41 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.0074(14) _cell_length_b 13.3464(7) _cell_length_c 17.8421(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.8920(10) _cell_angle_gamma 90.00 _cell_volume 5524.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 23044 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.6 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2212 _exptl_absorpt_coefficient_mu 1.777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.510 _exptl_absorpt_correction_T_max 0.701 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27958 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10202 _reflns_number_gt 9102 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+2.4192P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10202 _refine_ls_number_parameters 611 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.178 _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 Yb1 Yb 0.756046(8) 0.045470(12) 0.572270(10) 0.03564(7) Uani 1 1 d . . . Si1 Si 0.85321(6) -0.11490(9) 0.72923(7) 0.0458(3) Uani 1 1 d . . . Si2 Si 0.61043(6) 0.15022(10) 0.57972(8) 0.0547(4) Uani 1 1 d . . . N1 N 0.83023(15) -0.0683(2) 0.63703(19) 0.0413(8) Uani 1 1 d . . . N2 N 0.80877(16) -0.0468(3) 0.5076(2) 0.0446(9) Uani 1 1 d . . . N3 N 0.65909(15) 0.1089(3) 0.5318(2) 0.0444(9) Uani 1 1 d . . . H3 H 0.774(2) 0.162(3) 0.725(3) 0.053(15) Uiso 1 1 d . . . N4 N 0.70332(17) 0.0473(3) 0.4455(2) 0.0479(9) Uani 1 1 d . . . N5 N 0.80790(15) 0.1958(2) 0.57835(18) 0.0358(8) Uani 1 1 d . . . N6 N 0.77494(16) 0.1502(2) 0.6798(2) 0.0406(9) Uani 1 1 d . . . N7 N 0.70203(18) -0.1074(3) 0.5925(2) 0.0570(11) Uani 1 1 d . . . C1 C 0.83448(19) -0.1015(3) 0.5677(3) 0.0421(10) Uani 1 1 d . . . C2 C 0.6566(2) 0.0893(3) 0.4575(3) 0.0434(11) Uani 1 1 d . . . C3 C 0.8067(2) -0.0697(4) 0.4269(3) 0.0542(12) Uani 1 1 d . . . H3A H 0.7862 -0.1330 0.4118 0.065 Uiso 1 1 calc R . . H3B H 0.8459 -0.0772 0.4209 0.065 Uiso 1 1 calc R . . C4 C 0.7760(2) 0.0142(4) 0.3748(3) 0.0585(13) Uani 1 1 d . . . H4A H 0.7952 0.0775 0.3938 0.070 Uiso 1 1 calc R . . H4B H 0.7808 0.0032 0.3226 0.070 Uiso 1 1 calc R . . C5 C 0.7125(2) 0.0257(4) 0.3689(3) 0.0522(12) Uani 1 1 d . . . H5A H 0.6967 0.0804 0.3331 0.063 Uiso 1 1 calc R . . H5B H 0.6923 -0.0361 0.3483 0.063 Uiso 1 1 calc R . . C6 C 0.8663(2) -0.1975(3) 0.5604(2) 0.0445(11) Uani 1 1 d . . . C7 C 0.9248(2) -0.2048(3) 0.5902(3) 0.0539(12) Uani 1 1 d . . . H7 H 0.9461 -0.1482 0.6122 0.065 Uiso 1 1 calc R . . C8 C 0.9529(2) -0.2961(4) 0.5879(3) 0.0647(14) Uani 1 1 d . . . H8 H 0.9930 -0.3005 0.6080 0.078 Uiso 1 1 calc R . . C9 C 0.9222(3) -0.3789(4) 0.5565(3) 0.0703(16) Uani 1 1 d . . . H9 H 0.9410 -0.4406 0.5561 0.084 Uiso 1 1 calc R . . C10 C 0.8640(3) -0.3713(4) 0.5257(3) 0.0686(16) Uani 1 1 d . . . H10 H 0.8430 -0.4280 0.5033 0.082 Uiso 1 1 calc R . . C11 C 0.8355(2) -0.2816(3) 0.5270(3) 0.0571(13) Uani 1 1 d . . . H11 H 0.7955 -0.2774 0.5053 0.068 Uiso 1 1 calc R . . C12 C 0.60554(19) 0.1163(4) 0.3923(3) 0.0483(11) Uani 1 1 d . . . C13 C 0.5707(2) 0.0440(4) 0.3493(4) 0.0779(18) Uani 1 1 d . . . H13 H 0.5783 -0.0243 0.3600 0.093 Uiso 1 1 calc R . . C14 C 0.5231(3) 0.0741(6) 0.2886(4) 0.090(2) Uani 1 1 d . . . H14 H 0.4989 0.0253 0.2590 0.107 Uiso 1 1 calc R . . C15 C 0.5119(3) 0.1728(6) 0.2727(4) 0.091(2) Uani 1 1 d . . . H15 H 0.4805 0.1917 0.2317 0.109 Uiso 1 1 calc R . . C16 C 0.5460(3) 0.2443(5) 0.3159(4) 0.090(2) Uani 1 1 d . . . H16 H 0.5381 0.3125 0.3050 0.108 Uiso 1 1 calc R . . C17 C 0.5924(2) 0.2163(4) 0.3760(3) 0.0717(16) Uani 1 1 d . . . H17 H 0.6153 0.2660 0.4064 0.086 Uiso 1 1 calc R . . C18 C 0.8599(2) -0.2542(3) 0.7378(3) 0.0570(13) Uani 1 1 d . . . H18A H 0.8246 -0.2851 0.7078 0.086 Uiso 1 1 calc R . . H18B H 0.8665 -0.2734 0.7918 0.086 Uiso 1 1 calc R . . H18C H 0.8920 -0.2763 0.7183 0.086 Uiso 1 1 calc R . . C19 C 0.7973(2) -0.0808(4) 0.7808(3) 0.0651(15) Uani 1 1 d . . . H19A H 0.7897 -0.0094 0.7756 0.098 Uiso 1 1 calc R . . H19B H 0.8111 -0.0978 0.8353 0.098 Uiso 1 1 calc R . . H19C H 0.7621 -0.1175 0.7583 0.098 Uiso 1 1 calc R . . C20 C 0.9222(3) -0.0533(4) 0.7812(3) 0.0727(16) Uani 1 1 d . . . H20A H 0.9527 -0.0735 0.7577 0.109 Uiso 1 1 calc R . . H20B H 0.9322 -0.0733 0.8353 0.109 Uiso 1 1 calc R . . H20C H 0.9177 0.0189 0.7777 0.109 Uiso 1 1 calc R . . C21 C 0.5333(3) 0.1445(6) 0.5258(4) 0.099(2) Uani 1 1 d . . . H21A H 0.5248 0.1984 0.4880 0.149 Uiso 1 1 calc R . . H21B H 0.5094 0.1516 0.5618 0.149 Uiso 1 1 calc R . . H21C H 0.5253 0.0806 0.4993 0.149 Uiso 1 1 calc R . . C22 C 0.6282(3) 0.2800(4) 0.6151(4) 0.100(2) Uani 1 1 d . . . H22A H 0.6691 0.2848 0.6398 0.150 Uiso 1 1 calc R . . H22B H 0.6065 0.2969 0.6524 0.150 Uiso 1 1 calc R . . H22C H 0.6182 0.3262 0.5718 0.150 Uiso 1 1 calc R . . C23 C 0.6186(3) 0.0698(5) 0.6674(3) 0.0867(19) Uani 1 1 d . . . H23A H 0.6074 0.0016 0.6515 0.130 Uiso 1 1 calc R . . H23B H 0.5941 0.0952 0.6987 0.130 Uiso 1 1 calc R . . H23C H 0.6584 0.0707 0.6975 0.130 Uiso 1 1 calc R . . C24 C 0.84333(18) 0.2497(3) 0.5403(2) 0.0352(9) Uani 1 1 d . . . C25 C 0.90387(18) 0.2378(3) 0.5614(2) 0.0382(10) Uani 1 1 d . . . C26 C 0.9362(2) 0.2982(3) 0.5252(3) 0.0459(11) Uani 1 1 d . . . H26 H 0.9765 0.2927 0.5400 0.055 Uiso 1 1 calc R . . C27 C 0.9110(2) 0.3661(3) 0.4682(3) 0.0468(11) Uani 1 1 d . . . H27 H 0.9339 0.4083 0.4463 0.056 Uiso 1 1 calc R . . C28 C 0.8519(2) 0.3711(3) 0.4441(2) 0.0410(10) Uani 1 1 d . . . H28 H 0.8345 0.4147 0.4034 0.049 Uiso 1 1 calc R . . C29 C 0.81705(19) 0.3132(3) 0.4785(2) 0.0368(9) Uani 1 1 d . . . C30 C 0.9335(2) 0.1575(3) 0.6176(3) 0.0500(12) Uani 1 1 d . . . H30 H 0.9042 0.1267 0.6406 0.060 Uiso 1 1 calc R . . C31 C 0.9817(2) 0.1990(4) 0.6840(3) 0.0743(16) Uani 1 1 d . . . H31A H 1.0131 0.2226 0.6636 0.111 Uiso 1 1 calc R . . H31B H 0.9956 0.1465 0.7218 0.111 Uiso 1 1 calc R . . H31C H 0.9669 0.2540 0.7087 0.111 Uiso 1 1 calc R . . C32 C 0.9564(2) 0.0760(4) 0.5737(3) 0.0729(16) Uani 1 1 d . . . H32A H 0.9250 0.0490 0.5333 0.109 Uiso 1 1 calc R . . H32B H 0.9736 0.0229 0.6093 0.109 Uiso 1 1 calc R . . H32C H 0.9853 0.1043 0.5506 0.109 Uiso 1 1 calc R . . C33 C 0.75202(19) 0.3191(3) 0.4513(2) 0.0439(11) Uani 1 1 d . . . H33 H 0.7365 0.2554 0.4659 0.053 Uiso 1 1 calc R . . C34 C 0.7281(2) 0.4035(4) 0.4913(3) 0.0716(16) Uani 1 1 d . . . H34A H 0.7397 0.3933 0.5470 0.107 Uiso 1 1 calc R . . H34B H 0.6863 0.4037 0.4737 0.107 Uiso 1 1 calc R . . H34C H 0.7429 0.4672 0.4787 0.107 Uiso 1 1 calc R . . C35 C 0.7307(2) 0.3293(4) 0.3638(3) 0.0626(14) Uani 1 1 d . . . H35A H 0.7430 0.3934 0.3478 0.094 Uiso 1 1 calc R . . H35B H 0.6890 0.3256 0.3486 0.094 Uiso 1 1 calc R . . H35C H 0.7466 0.2756 0.3390 0.094 Uiso 1 1 calc R . . C36 C 0.80782(18) 0.2129(3) 0.6522(2) 0.0351(9) Uani 1 1 d . . . C37 C 0.84160(18) 0.2941(3) 0.7021(2) 0.0363(9) Uani 1 1 d . . . C38 C 0.8658(2) 0.2738(3) 0.7801(2) 0.0464(11) Uani 1 1 d . . . H38 H 0.8615 0.2097 0.7996 0.056 Uiso 1 1 calc R . . C39 C 0.8963(2) 0.3465(4) 0.8295(3) 0.0561(13) Uani 1 1 d . . . H39 H 0.9125 0.3316 0.8820 0.067 Uiso 1 1 calc R . . C40 C 0.9027(2) 0.4410(4) 0.8012(3) 0.0577(13) Uani 1 1 d . . . H40 H 0.9227 0.4910 0.8347 0.069 Uiso 1 1 calc R . . C41 C 0.8797(2) 0.4616(3) 0.7240(3) 0.0556(13) Uani 1 1 d . . . H41 H 0.8846 0.5256 0.7046 0.067 Uiso 1 1 calc R . . C42 C 0.8494(2) 0.3894(3) 0.6744(3) 0.0470(11) Uani 1 1 d . . . H42 H 0.8341 0.4046 0.6217 0.056 Uiso 1 1 calc R . . C43 C 0.6854(2) -0.1814(4) 0.6103(3) 0.0527(12) Uani 1 1 d . . . C44 C 0.6657(2) -0.2762(3) 0.6332(3) 0.0503(12) Uani 1 1 d . . . C45 C 0.6970(2) -0.3613(4) 0.6305(3) 0.0666(15) Uani 1 1 d . . . H45 H 0.7312 -0.3587 0.6142 0.080 Uiso 1 1 calc R . . C46 C 0.6770(3) -0.4512(4) 0.6521(3) 0.0750(17) Uani 1 1 d . . . H46 H 0.6973 -0.5106 0.6492 0.090 Uiso 1 1 calc R . . C47 C 0.6287(3) -0.4546(4) 0.6772(3) 0.0726(17) Uani 1 1 d . . . H47 H 0.6163 -0.5162 0.6927 0.087 Uiso 1 1 calc R . . C48 C 0.5974(3) -0.3699(4) 0.6806(4) 0.0795(18) Uani 1 1 d . . . H48 H 0.5636 -0.3731 0.6980 0.095 Uiso 1 1 calc R . . C49 C 0.6161(3) -0.2791(4) 0.6581(3) 0.0706(15) Uani 1 1 d . . . H49 H 0.5951 -0.2201 0.6599 0.085 Uiso 1 1 calc R . . C50 C 0.5885(3) 0.6124(6) 0.4164(4) 0.086(2) Uani 1 1 d . . . C51 C 0.6023(3) 0.7153(7) 0.4354(4) 0.099(2) Uani 1 1 d . . . H51 H 0.5828 0.7514 0.4661 0.119 Uiso 1 1 calc R . . C52 C 0.6451(3) 0.7604(5) 0.4077(4) 0.089(2) Uani 1 1 d . . . H52 H 0.6560 0.8269 0.4216 0.107 Uiso 1 1 calc R . . C53 C 0.6707(3) 0.7098(6) 0.3615(4) 0.097(2) Uani 1 1 d . . . H53 H 0.6994 0.7416 0.3428 0.116 Uiso 1 1 calc R . . C54 C 0.6564(3) 0.6139(6) 0.3409(5) 0.102(2) Uani 1 1 d . . . H54 H 0.6746 0.5808 0.3072 0.123 Uiso 1 1 calc R . . C55 C 0.6168(3) 0.5656(5) 0.3679(4) 0.0832(18) Uani 1 1 d . . . H55 H 0.6081 0.4985 0.3536 0.100 Uiso 1 1 calc R . . C56 C 0.5453(4) 0.5580(8) 0.4450(5) 0.166(5) Uani 1 1 d . . . H56A H 0.5101 0.5972 0.4353 0.248 Uiso 1 1 calc R . . H56B H 0.5598 0.5466 0.5003 0.248 Uiso 1 1 calc R . . H56C H 0.5374 0.4942 0.4184 0.248 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 Yb1 0.03913(12) 0.03157(11) 0.03625(12) -0.00254(7) 0.00975(8) -0.00007(7) Si1 0.0535(8) 0.0372(6) 0.0425(7) -0.0013(5) 0.0050(6) 0.0068(6) Si2 0.0519(9) 0.0531(8) 0.0639(9) -0.0045(7) 0.0233(7) 0.0064(6) N1 0.045(2) 0.0410(19) 0.036(2) -0.0024(16) 0.0076(17) 0.0095(16) N2 0.048(2) 0.052(2) 0.035(2) -0.0039(17) 0.0122(17) 0.0080(17) N3 0.038(2) 0.049(2) 0.045(2) -0.0044(17) 0.0102(17) 0.0035(16) N4 0.047(2) 0.061(2) 0.036(2) -0.0026(17) 0.0101(18) 0.0058(19) N5 0.045(2) 0.0346(17) 0.0293(18) -0.0009(14) 0.0127(16) -0.0060(15) N6 0.058(3) 0.0349(19) 0.034(2) -0.0037(16) 0.0213(19) -0.0074(16) N7 0.056(3) 0.042(2) 0.072(3) 0.001(2) 0.014(2) -0.0117(19) C1 0.042(3) 0.038(2) 0.046(3) -0.008(2) 0.011(2) -0.0008(19) C2 0.045(3) 0.037(2) 0.046(3) -0.001(2) 0.006(2) -0.002(2) C3 0.060(3) 0.060(3) 0.046(3) -0.002(2) 0.021(2) 0.007(2) C4 0.059(3) 0.076(3) 0.047(3) -0.005(3) 0.024(3) 0.000(3) C5 0.056(3) 0.054(3) 0.045(3) -0.005(2) 0.011(2) 0.001(2) C6 0.049(3) 0.045(2) 0.043(3) -0.007(2) 0.018(2) 0.003(2) C7 0.049(3) 0.046(3) 0.070(3) -0.007(2) 0.021(3) 0.002(2) C8 0.057(3) 0.057(3) 0.083(4) 0.002(3) 0.024(3) 0.021(3) C9 0.094(5) 0.051(3) 0.076(4) -0.010(3) 0.040(4) 0.016(3) C10 0.093(5) 0.041(3) 0.071(4) -0.015(3) 0.020(3) 0.001(3) C11 0.059(3) 0.051(3) 0.060(3) -0.010(2) 0.013(3) 0.001(2) C12 0.036(3) 0.062(3) 0.045(3) -0.006(2) 0.008(2) -0.007(2) C13 0.050(3) 0.079(4) 0.096(5) -0.039(3) 0.002(3) 0.003(3) C14 0.051(4) 0.119(6) 0.080(4) -0.046(4) -0.016(3) 0.007(4) C15 0.069(5) 0.130(6) 0.062(4) -0.005(4) -0.004(3) 0.019(4) C16 0.063(4) 0.107(5) 0.092(5) 0.034(4) 0.006(4) 0.015(4) C17 0.053(3) 0.074(4) 0.081(4) 0.013(3) 0.003(3) -0.007(3) C18 0.063(3) 0.044(3) 0.062(3) 0.002(2) 0.012(3) 0.006(2) C19 0.083(4) 0.069(3) 0.048(3) 0.006(3) 0.026(3) 0.021(3) C20 0.078(4) 0.065(3) 0.061(3) -0.001(3) -0.007(3) -0.005(3) C21 0.063(4) 0.138(6) 0.102(5) -0.003(4) 0.031(4) 0.016(4) C22 0.121(6) 0.067(4) 0.133(6) -0.026(4) 0.073(5) -0.007(4) C23 0.094(5) 0.100(5) 0.083(4) 0.010(4) 0.054(4) 0.012(4) C24 0.046(3) 0.029(2) 0.033(2) -0.0042(17) 0.0135(19) -0.0048(18) C25 0.042(3) 0.038(2) 0.034(2) 0.0033(18) 0.0084(19) -0.0015(19) C26 0.043(3) 0.046(2) 0.051(3) -0.002(2) 0.016(2) -0.005(2) C27 0.057(3) 0.043(2) 0.048(3) -0.002(2) 0.026(2) -0.007(2) C28 0.055(3) 0.035(2) 0.038(2) 0.0024(19) 0.022(2) 0.002(2) C29 0.046(3) 0.035(2) 0.033(2) 0.0013(18) 0.017(2) 0.0034(19) C30 0.038(3) 0.054(3) 0.055(3) 0.013(2) 0.007(2) -0.004(2) C31 0.060(4) 0.087(4) 0.064(4) 0.013(3) -0.008(3) -0.011(3) C32 0.062(4) 0.053(3) 0.099(4) 0.013(3) 0.010(3) 0.012(3) C33 0.048(3) 0.043(2) 0.044(3) 0.012(2) 0.019(2) 0.005(2) C34 0.056(4) 0.086(4) 0.070(4) -0.010(3) 0.011(3) 0.023(3) C35 0.051(3) 0.089(4) 0.047(3) 0.010(3) 0.011(2) -0.011(3) C36 0.043(3) 0.030(2) 0.032(2) -0.0001(17) 0.0103(19) -0.0017(18) C37 0.045(3) 0.031(2) 0.035(2) -0.0032(17) 0.0128(19) -0.0027(18) C38 0.060(3) 0.041(2) 0.039(2) -0.005(2) 0.015(2) -0.008(2) C39 0.058(3) 0.063(3) 0.045(3) -0.011(2) 0.009(2) -0.006(3) C40 0.058(3) 0.059(3) 0.057(3) -0.025(3) 0.017(3) -0.022(2) C41 0.071(4) 0.035(2) 0.064(3) -0.010(2) 0.022(3) -0.013(2) C42 0.067(3) 0.036(2) 0.041(2) -0.005(2) 0.019(2) -0.006(2) C43 0.053(3) 0.052(3) 0.051(3) -0.001(2) 0.010(2) -0.003(2) C44 0.058(3) 0.044(3) 0.047(3) 0.001(2) 0.009(2) -0.012(2) C45 0.067(4) 0.051(3) 0.086(4) 0.003(3) 0.027(3) -0.003(3) C46 0.098(5) 0.050(3) 0.082(4) -0.004(3) 0.031(4) -0.003(3) C47 0.103(5) 0.054(3) 0.060(4) 0.001(3) 0.022(3) -0.022(3) C48 0.079(4) 0.073(4) 0.098(5) 0.004(3) 0.045(4) -0.021(3) C49 0.075(4) 0.060(3) 0.084(4) -0.003(3) 0.033(3) -0.009(3) C50 0.053(4) 0.135(6) 0.058(4) 0.031(4) -0.007(3) 0.004(4) C51 0.099(6) 0.141(7) 0.051(4) -0.004(4) 0.006(4) 0.047(5) C52 0.116(6) 0.075(4) 0.071(4) -0.005(3) 0.015(4) 0.009(4) C53 0.097(6) 0.106(6) 0.086(5) -0.014(4) 0.022(4) -0.014(4) C54 0.087(6) 0.095(5) 0.120(6) -0.017(5) 0.018(5) 0.009(4) C55 0.068(4) 0.088(4) 0.085(5) 0.003(4) 0.003(4) 0.009(4) C56 0.102(7) 0.278(13) 0.109(7) 0.051(7) 0.012(6) -0.049(7) _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 Yb1 N2 2.280(3) . ? Yb1 N4 2.291(4) . ? Yb1 N6 2.322(4) . ? Yb1 N5 2.349(3) . ? Yb1 N1 2.399(3) . ? Yb1 N3 2.407(3) . ? Yb1 N7 2.494(4) . ? Yb1 C1 2.734(4) . ? Yb1 C36 2.768(4) . ? Yb1 C2 2.779(4) . ? Si1 N1 1.712(3) . ? Si1 C19 1.868(5) . ? Si1 C18 1.869(4) . ? Si1 C20 1.869(5) . ? Si2 N3 1.707(4) . ? Si2 C22 1.856(6) . ? Si2 C21 1.857(6) . ? Si2 C23 1.866(6) . ? N1 C1 1.342(5) . ? N2 C1 1.313(5) . ? N2 C3 1.462(5) . ? N3 C2 1.337(5) . ? N4 C2 1.320(6) . ? N4 C5 1.467(6) . ? N5 C36 1.338(5) . ? N5 C24 1.414(5) . ? N6 C36 1.329(5) . ? N6 H3 0.82(4) . ? N7 C43 1.140(5) . ? C1 C6 1.515(6) . ? C2 C12 1.501(6) . ? C3 C4 1.519(6) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.508(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.371(6) . ? C6 C11 1.391(6) . ? C7 C8 1.399(6) . ? C7 H7 0.9400 . ? C8 C9 1.365(7) . ? C8 H8 0.9400 . ? C9 C10 1.368(8) . ? C9 H9 0.9400 . ? C10 C11 1.381(7) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C13 1.376(6) . ? C12 C17 1.385(7) . ? C13 C14 1.415(8) . ? C13 H13 0.9400 . ? C14 C15 1.360(9) . ? C14 H14 0.9400 . ? C15 C16 1.360(9) . ? C15 H15 0.9400 . ? C16 C17 1.385(7) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C29 1.405(5) . ? C24 C25 1.414(6) . ? C25 C26 1.388(6) . ? C25 C30 1.515(6) . ? C26 C27 1.381(6) . ? C26 H26 0.9400 . ? C27 C28 1.375(6) . ? C27 H27 0.9400 . ? C28 C29 1.391(5) . ? C28 H28 0.9400 . ? C29 C33 1.513(6) . ? C30 C32 1.524(7) . ? C30 C31 1.531(6) . ? C30 H30 0.9900 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C35 1.519(6) . ? C33 C34 1.524(6) . ? C33 H33 0.9900 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 C37 1.502(5) . ? C37 C38 1.389(6) . ? C37 C42 1.395(5) . ? C38 C39 1.387(6) . ? C38 H38 0.9400 . ? C39 C40 1.381(6) . ? C39 H39 0.9400 . ? C40 C41 1.374(7) . ? C40 H40 0.9400 . ? C41 C42 1.381(6) . ? C41 H41 0.9400 . ? C42 H42 0.9400 . ? C43 C44 1.446(6) . ? C44 C45 1.369(7) . ? C44 C49 1.374(7) . ? C45 C46 1.383(7) . ? C45 H45 0.9400 . ? C46 C47 1.346(8) . ? C46 H46 0.9400 . ? C47 C48 1.367(8) . ? C47 H47 0.9400 . ? C48 C49 1.387(7) . ? C48 H48 0.9400 . ? C49 H49 0.9400 . ? C50 C55 1.380(9) . ? C50 C51 1.432(10) . ? C50 C56 1.461(10) . ? C51 C52 1.386(10) . ? C51 H51 0.9400 . ? C52 C53 1.332(9) . ? C52 H52 0.9400 . ? C53 C54 1.351(9) . ? C53 H53 0.9400 . ? C54 C55 1.336(9) . ? C54 H54 0.9400 . ? C55 H55 0.9400 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C56 H56C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Yb1 N4 75.16(13) . . ? N2 Yb1 N6 136.63(13) . . ? N4 Yb1 N6 138.63(13) . . ? N2 Yb1 N5 97.36(12) . . ? N4 Yb1 N5 100.85(12) . . ? N6 Yb1 N5 57.25(11) . . ? N2 Yb1 N1 57.45(12) . . ? N4 Yb1 N1 129.48(12) . . ? N6 Yb1 N1 91.12(12) . . ? N5 Yb1 N1 101.49(12) . . ? N2 Yb1 N3 131.15(12) . . ? N4 Yb1 N3 56.89(13) . . ? N6 Yb1 N3 90.27(13) . . ? N5 Yb1 N3 99.99(12) . . ? N1 Yb1 N3 155.27(12) . . ? N2 Yb1 N7 90.48(13) . . ? N4 Yb1 N7 88.62(13) . . ? N6 Yb1 N7 111.80(13) . . ? N5 Yb1 N7 168.98(12) . . ? N1 Yb1 N7 76.22(13) . . ? N3 Yb1 N7 80.36(13) . . ? N2 Yb1 C1 28.57(12) . . ? N4 Yb1 C1 100.86(13) . . ? N6 Yb1 C1 117.79(13) . . ? N5 Yb1 C1 104.68(12) . . ? N1 Yb1 C1 29.38(11) . . ? N3 Yb1 C1 149.74(12) . . ? N7 Yb1 C1 78.75(13) . . ? N2 Yb1 C36 117.55(13) . . ? N4 Yb1 C36 124.14(12) . . ? N6 Yb1 C36 28.58(11) . . ? N5 Yb1 C36 28.86(11) . . ? N1 Yb1 C36 94.77(12) . . ? N3 Yb1 C36 98.17(12) . . ? N7 Yb1 C36 140.13(12) . . ? C1 Yb1 C36 111.89(12) . . ? N2 Yb1 C2 102.98(13) . . ? N4 Yb1 C2 28.15(12) . . ? N6 Yb1 C2 115.49(13) . . ? N5 Yb1 C2 101.48(12) . . ? N1 Yb1 C2 151.54(12) . . ? N3 Yb1 C2 28.75(12) . . ? N7 Yb1 C2 84.18(13) . . ? C1 Yb1 C2 126.66(13) . . ? C36 Yb1 C2 113.38(12) . . ? N1 Si1 C19 106.8(2) . . ? N1 Si1 C18 116.1(2) . . ? C19 Si1 C18 105.0(2) . . ? N1 Si1 C20 110.0(2) . . ? C19 Si1 C20 107.8(3) . . ? C18 Si1 C20 110.5(2) . . ? N3 Si2 C22 110.2(2) . . ? N3 Si2 C21 116.6(3) . . ? C22 Si2 C21 109.0(3) . . ? N3 Si2 C23 107.2(2) . . ? C22 Si2 C23 106.6(3) . . ? C21 Si2 C23 106.7(3) . . ? C1 N1 Si1 133.1(3) . . ? C1 N1 Yb1 89.3(2) . . ? Si1 N1 Yb1 135.14(18) . . ? C1 N2 C3 125.4(4) . . ? C1 N2 Yb1 95.3(3) . . ? C3 N2 Yb1 136.8(3) . . ? C2 N3 Si2 134.2(3) . . ? C2 N3 Yb1 91.3(3) . . ? Si2 N3 Yb1 134.20(19) . . ? C2 N4 C5 125.0(4) . . ? C2 N4 Yb1 96.9(3) . . ? C5 N4 Yb1 137.7(3) . . ? C36 N5 C24 122.7(3) . . ? C36 N5 Yb1 93.2(2) . . ? C24 N5 Yb1 142.1(2) . . ? C36 N6 Yb1 94.7(3) . . ? C36 N6 H3 114(3) . . ? Yb1 N6 H3 151(3) . . ? C43 N7 Yb1 168.9(4) . . ? N2 C1 N1 116.0(4) . . ? N2 C1 C6 122.8(4) . . ? N1 C1 C6 121.2(4) . . ? N2 C1 Yb1 56.1(2) . . ? N1 C1 Yb1 61.3(2) . . ? C6 C1 Yb1 167.4(3) . . ? N4 C2 N3 114.9(4) . . ? N4 C2 C12 122.3(4) . . ? N3 C2 C12 122.8(4) . . ? N4 C2 Yb1 54.9(2) . . ? N3 C2 Yb1 60.0(2) . . ? C12 C2 Yb1 175.9(3) . . ? N2 C3 C4 109.6(4) . . ? N2 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C3 116.1(4) . . ? C5 C4 H4A 108.3 . . ? C3 C4 H4A 108.3 . . ? C5 C4 H4B 108.3 . . ? C3 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? N4 C5 C4 110.2(4) . . ? N4 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? N4 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C7 C6 C11 119.1(4) . . ? C7 C6 C1 121.0(4) . . ? C11 C6 C1 119.7(4) . . ? C6 C7 C8 120.3(5) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 120.3(5) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.5(5) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 121.0(5) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C6 119.8(5) . . ? C10 C11 H11 120.1 . . ? C6 C11 H11 120.1 . . ? C13 C12 C17 119.0(5) . . ? C13 C12 C2 121.5(5) . . ? C17 C12 C2 119.4(4) . . ? C12 C13 C14 118.9(6) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C15 C14 C13 120.8(6) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 120.3(6) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.8(6) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C12 121.2(6) . . ? C16 C17 H17 119.4 . . ? C12 C17 H17 119.4 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 N5 118.6(4) . . ? C29 C24 C25 120.1(4) . . ? N5 C24 C25 121.2(4) . . ? C26 C25 C24 118.0(4) . . ? C26 C25 C30 119.7(4) . . ? C24 C25 C30 122.2(4) . . ? C27 C26 C25 122.2(4) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C28 C27 C26 118.9(4) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 121.6(4) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C28 C29 C24 118.8(4) . . ? C28 C29 C33 121.1(4) . . ? C24 C29 C33 120.1(4) . . ? C25 C30 C32 109.6(4) . . ? C25 C30 C31 112.9(4) . . ? C32 C30 C31 110.8(4) . . ? C25 C30 H30 107.8 . . ? C32 C30 H30 107.8 . . ? C31 C30 H30 107.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C35 112.5(4) . . ? C29 C33 C34 111.7(4) . . ? C35 C33 C34 110.4(4) . . ? C29 C33 H33 107.3 . . ? C35 C33 H33 107.3 . . ? C34 C33 H33 107.3 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N6 C36 N5 114.1(4) . . ? N6 C36 C37 121.1(4) . . ? N5 C36 C37 124.8(4) . . ? N6 C36 Yb1 56.7(2) . . ? N5 C36 Yb1 57.92(19) . . ? C37 C36 Yb1 172.3(3) . . ? C38 C37 C42 118.3(4) . . ? C38 C37 C36 118.4(3) . . ? C42 C37 C36 123.3(4) . . ? C39 C38 C37 121.0(4) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C40 C39 C38 119.8(4) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 C40 C39 119.7(4) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C40 C41 C42 120.8(4) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C41 C42 C37 120.4(4) . . ? C41 C42 H42 119.8 . . ? C37 C42 H42 119.8 . . ? N7 C43 C44 178.6(5) . . ? C45 C44 C49 121.1(5) . . ? C45 C44 C43 119.6(5) . . ? C49 C44 C43 119.3(5) . . ? C44 C45 C46 118.5(5) . . ? C44 C45 H45 120.8 . . ? C46 C45 H45 120.8 . . ? C47 C46 C45 120.8(5) . . ? C47 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C46 C47 C48 121.1(5) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C47 C48 C49 119.1(6) . . ? C47 C48 H48 120.4 . . ? C49 C48 H48 120.4 . . ? C44 C49 C48 119.3(5) . . ? C44 C49 H49 120.3 . . ? C48 C49 H49 120.3 . . ? C55 C50 C51 117.5(7) . . ? C55 C50 C56 120.1(9) . . ? C51 C50 C56 122.4(9) . . ? C52 C51 C50 118.7(6) . . ? C52 C51 H51 120.7 . . ? C50 C51 H51 120.7 . . ? C53 C52 C51 120.1(7) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C52 C53 C54 121.6(8) . . ? C52 C53 H53 119.2 . . ? C54 C53 H53 119.2 . . ? C55 C54 C53 120.9(8) . . ? C55 C54 H54 119.5 . . ? C53 C54 H54 119.5 . . ? C54 C55 C50 121.1(7) . . ? C54 C55 H55 119.4 . . ? C50 C55 H55 119.4 . . ? C50 C56 H56A 109.5 . . ? C50 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C50 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 Si1 N1 C1 -144.7(4) . . . . ? C18 Si1 N1 C1 -28.0(5) . . . . ? C20 Si1 N1 C1 98.5(5) . . . . ? C19 Si1 N1 Yb1 11.8(3) . . . . ? C18 Si1 N1 Yb1 128.5(3) . . . . ? C20 Si1 N1 Yb1 -105.0(3) . . . . ? N2 Yb1 N1 C1 -8.1(2) . . . . ? N4 Yb1 N1 C1 15.1(3) . . . . ? N6 Yb1 N1 C1 -156.3(3) . . . . ? N5 Yb1 N1 C1 -99.5(3) . . . . ? N3 Yb1 N1 C1 110.6(3) . . . . ? N7 Yb1 N1 C1 91.5(3) . . . . ? C36 Yb1 N1 C1 -127.9(3) . . . . ? C2 Yb1 N1 C1 43.7(4) . . . . ? N2 Yb1 N1 Si1 -171.2(3) . . . . ? N4 Yb1 N1 Si1 -148.0(2) . . . . ? N6 Yb1 N1 Si1 40.6(3) . . . . ? N5 Yb1 N1 Si1 97.4(3) . . . . ? N3 Yb1 N1 Si1 -52.5(4) . . . . ? N7 Yb1 N1 Si1 -71.6(3) . . . . ? C1 Yb1 N1 Si1 -163.1(4) . . . . ? C36 Yb1 N1 Si1 69.0(3) . . . . ? C2 Yb1 N1 Si1 -119.3(3) . . . . ? N4 Yb1 N2 C1 -153.4(3) . . . . ? N6 Yb1 N2 C1 58.4(3) . . . . ? N5 Yb1 N2 C1 107.3(3) . . . . ? N1 Yb1 N2 C1 8.3(2) . . . . ? N3 Yb1 N2 C1 -142.5(2) . . . . ? N7 Yb1 N2 C1 -65.0(3) . . . . ? C36 Yb1 N2 C1 85.5(3) . . . . ? C2 Yb1 N2 C1 -149.1(3) . . . . ? N4 Yb1 N2 C3 8.1(4) . . . . ? N6 Yb1 N2 C3 -140.1(4) . . . . ? N5 Yb1 N2 C3 -91.2(4) . . . . ? N1 Yb1 N2 C3 169.8(5) . . . . ? N3 Yb1 N2 C3 19.0(5) . . . . ? N7 Yb1 N2 C3 96.5(4) . . . . ? C1 Yb1 N2 C3 161.5(6) . . . . ? C36 Yb1 N2 C3 -113.0(4) . . . . ? C2 Yb1 N2 C3 12.4(5) . . . . ? C22 Si2 N3 C2 -109.8(5) . . . . ? C21 Si2 N3 C2 15.1(5) . . . . ? C23 Si2 N3 C2 134.5(5) . . . . ? C22 Si2 N3 Yb1 78.5(4) . . . . ? C21 Si2 N3 Yb1 -156.6(3) . . . . ? C23 Si2 N3 Yb1 -37.2(4) . . . . ? N2 Yb1 N3 C2 -13.4(3) . . . . ? N4 Yb1 N3 C2 -0.8(2) . . . . ? N6 Yb1 N3 C2 152.4(3) . . . . ? N5 Yb1 N3 C2 95.7(2) . . . . ? N1 Yb1 N3 C2 -114.3(3) . . . . ? N7 Yb1 N3 C2 -95.5(3) . . . . ? C1 Yb1 N3 C2 -48.6(4) . . . . ? C36 Yb1 N3 C2 124.9(2) . . . . ? N2 Yb1 N3 Si2 160.7(2) . . . . ? N4 Yb1 N3 Si2 173.3(3) . . . . ? N6 Yb1 N3 Si2 -33.5(3) . . . . ? N5 Yb1 N3 Si2 -90.2(3) . . . . ? N1 Yb1 N3 Si2 59.8(4) . . . . ? N7 Yb1 N3 Si2 78.6(3) . . . . ? C1 Yb1 N3 Si2 125.5(3) . . . . ? C36 Yb1 N3 Si2 -61.0(3) . . . . ? C2 Yb1 N3 Si2 174.1(4) . . . . ? N2 Yb1 N4 C2 171.1(3) . . . . ? N6 Yb1 N4 C2 -42.1(4) . . . . ? N5 Yb1 N4 C2 -94.1(3) . . . . ? N1 Yb1 N4 C2 151.0(2) . . . . ? N3 Yb1 N4 C2 0.8(2) . . . . ? N7 Yb1 N4 C2 80.2(3) . . . . ? C1 Yb1 N4 C2 158.5(3) . . . . ? C36 Yb1 N4 C2 -75.5(3) . . . . ? N2 Yb1 N4 C5 -16.4(4) . . . . ? N6 Yb1 N4 C5 130.4(4) . . . . ? N5 Yb1 N4 C5 78.4(4) . . . . ? N1 Yb1 N4 C5 -36.5(5) . . . . ? N3 Yb1 N4 C5 173.3(5) . . . . ? N7 Yb1 N4 C5 -107.3(4) . . . . ? C1 Yb1 N4 C5 -29.0(4) . . . . ? C36 Yb1 N4 C5 97.0(4) . . . . ? C2 Yb1 N4 C5 172.5(6) . . . . ? N2 Yb1 N5 C36 -137.0(2) . . . . ? N4 Yb1 N5 C36 146.7(2) . . . . ? N6 Yb1 N5 C36 5.0(2) . . . . ? N1 Yb1 N5 C36 -78.9(2) . . . . ? N3 Yb1 N5 C36 88.8(2) . . . . ? N7 Yb1 N5 C36 -2.0(8) . . . . ? C1 Yb1 N5 C36 -108.9(2) . . . . ? C2 Yb1 N5 C36 118.1(2) . . . . ? N2 Yb1 N5 C24 25.3(4) . . . . ? N4 Yb1 N5 C24 -50.9(4) . . . . ? N6 Yb1 N5 C24 167.4(5) . . . . ? N1 Yb1 N5 C24 83.5(4) . . . . ? N3 Yb1 N5 C24 -108.8(4) . . . . ? N7 Yb1 N5 C24 160.4(6) . . . . ? C1 Yb1 N5 C24 53.5(4) . . . . ? C36 Yb1 N5 C24 162.4(6) . . . . ? C2 Yb1 N5 C24 -79.6(4) . . . . ? N2 Yb1 N6 C36 57.6(3) . . . . ? N4 Yb1 N6 C36 -72.0(3) . . . . ? N5 Yb1 N6 C36 -5.0(2) . . . . ? N1 Yb1 N6 C36 97.9(3) . . . . ? N3 Yb1 N6 C36 -106.8(3) . . . . ? N7 Yb1 N6 C36 173.5(2) . . . . ? C1 Yb1 N6 C36 85.0(3) . . . . ? C2 Yb1 N6 C36 -92.5(3) . . . . ? N2 Yb1 N7 C43 73(2) . . . . ? N4 Yb1 N7 C43 149(2) . . . . ? N6 Yb1 N7 C43 -68(2) . . . . ? N5 Yb1 N7 C43 -62(2) . . . . ? N1 Yb1 N7 C43 17(2) . . . . ? N3 Yb1 N7 C43 -155(2) . . . . ? C1 Yb1 N7 C43 47(2) . . . . ? C36 Yb1 N7 C43 -64(2) . . . . ? C2 Yb1 N7 C43 176(2) . . . . ? C3 N2 C1 N1 -178.6(4) . . . . ? Yb1 N2 C1 N1 -14.0(4) . . . . ? C3 N2 C1 C6 0.4(7) . . . . ? Yb1 N2 C1 C6 164.9(4) . . . . ? C3 N2 C1 Yb1 -164.6(5) . . . . ? Si1 N1 C1 N2 176.9(3) . . . . ? Yb1 N1 C1 N2 13.2(4) . . . . ? Si1 N1 C1 C6 -2.0(7) . . . . ? Yb1 N1 C1 C6 -165.7(4) . . . . ? Si1 N1 C1 Yb1 163.7(4) . . . . ? N4 Yb1 C1 N2 26.1(3) . . . . ? N6 Yb1 C1 N2 -138.6(3) . . . . ? N5 Yb1 C1 N2 -78.2(3) . . . . ? N1 Yb1 C1 N2 -165.6(4) . . . . ? N3 Yb1 C1 N2 65.4(4) . . . . ? N7 Yb1 C1 N2 112.5(3) . . . . ? C36 Yb1 C1 N2 -107.7(3) . . . . ? C2 Yb1 C1 N2 38.6(3) . . . . ? N2 Yb1 C1 N1 165.6(4) . . . . ? N4 Yb1 C1 N1 -168.2(2) . . . . ? N6 Yb1 C1 N1 27.0(3) . . . . ? N5 Yb1 C1 N1 87.4(3) . . . . ? N3 Yb1 C1 N1 -129.0(3) . . . . ? N7 Yb1 C1 N1 -81.8(3) . . . . ? C36 Yb1 C1 N1 57.9(3) . . . . ? C2 Yb1 C1 N1 -155.8(2) . . . . ? N2 Yb1 C1 C6 -89.3(14) . . . . ? N4 Yb1 C1 C6 -63.2(14) . . . . ? N6 Yb1 C1 C6 132.1(14) . . . . ? N5 Yb1 C1 C6 -167.5(14) . . . . ? N1 Yb1 C1 C6 105.0(15) . . . . ? N3 Yb1 C1 C6 -24.0(15) . . . . ? N7 Yb1 C1 C6 23.2(14) . . . . ? C36 Yb1 C1 C6 163.0(14) . . . . ? C2 Yb1 C1 C6 -50.7(14) . . . . ? C5 N4 C2 N3 -175.2(4) . . . . ? Yb1 N4 C2 N3 -1.4(4) . . . . ? C5 N4 C2 C12 2.6(7) . . . . ? Yb1 N4 C2 C12 176.4(3) . . . . ? C5 N4 C2 Yb1 -173.8(5) . . . . ? Si2 N3 C2 N4 -172.8(3) . . . . ? Yb1 N3 C2 N4 1.3(4) . . . . ? Si2 N3 C2 C12 9.4(7) . . . . ? Yb1 N3 C2 C12 -176.5(4) . . . . ? Si2 N3 C2 Yb1 -174.1(4) . . . . ? N2 Yb1 C2 N4 -8.9(3) . . . . ? N6 Yb1 C2 N4 150.6(3) . . . . ? N5 Yb1 C2 N4 91.6(3) . . . . ? N1 Yb1 C2 N4 -51.7(4) . . . . ? N3 Yb1 C2 N4 -178.6(4) . . . . ? N7 Yb1 C2 N4 -98.0(3) . . . . ? C1 Yb1 C2 N4 -26.7(3) . . . . ? C36 Yb1 C2 N4 119.2(3) . . . . ? N2 Yb1 C2 N3 169.7(2) . . . . ? N4 Yb1 C2 N3 178.6(4) . . . . ? N6 Yb1 C2 N3 -30.9(3) . . . . ? N5 Yb1 C2 N3 -89.9(3) . . . . ? N1 Yb1 C2 N3 126.9(3) . . . . ? N7 Yb1 C2 N3 80.5(3) . . . . ? C1 Yb1 C2 N3 151.9(2) . . . . ? C36 Yb1 C2 N3 -62.2(3) . . . . ? N2 Yb1 C2 C12 -57(4) . . . . ? N4 Yb1 C2 C12 -48(4) . . . . ? N6 Yb1 C2 C12 102(4) . . . . ? N5 Yb1 C2 C12 43(4) . . . . ? N1 Yb1 C2 C12 -100(4) . . . . ? N3 Yb1 C2 C12 133(4) . . . . ? N7 Yb1 C2 C12 -146(4) . . . . ? C1 Yb1 C2 C12 -75(4) . . . . ? C36 Yb1 C2 C12 71(4) . . . . ? C1 N2 C3 C4 -176.8(4) . . . . ? Yb1 N2 C3 C4 26.0(6) . . . . ? N2 C3 C4 C5 -67.6(6) . . . . ? C2 N4 C5 C4 159.3(4) . . . . ? Yb1 N4 C5 C4 -11.6(6) . . . . ? C3 C4 C5 N4 60.8(5) . . . . ? N2 C1 C6 C7 114.2(5) . . . . ? N1 C1 C6 C7 -66.9(6) . . . . ? Yb1 C1 C6 C7 -164.8(12) . . . . ? N2 C1 C6 C11 -69.4(6) . . . . ? N1 C1 C6 C11 109.5(5) . . . . ? Yb1 C1 C6 C11 11.6(16) . . . . ? C11 C6 C7 C8 -1.0(7) . . . . ? C1 C6 C7 C8 175.4(4) . . . . ? C6 C7 C8 C9 -0.5(8) . . . . ? C7 C8 C9 C10 1.5(8) . . . . ? C8 C9 C10 C11 -1.1(9) . . . . ? C9 C10 C11 C6 -0.4(8) . . . . ? C7 C6 C11 C10 1.4(7) . . . . ? C1 C6 C11 C10 -175.0(4) . . . . ? N4 C2 C12 C13 69.9(6) . . . . ? N3 C2 C12 C13 -112.5(6) . . . . ? Yb1 C2 C12 C13 116(4) . . . . ? N4 C2 C12 C17 -111.5(5) . . . . ? N3 C2 C12 C17 66.1(6) . . . . ? Yb1 C2 C12 C17 -65(5) . . . . ? C17 C12 C13 C14 1.3(8) . . . . ? C2 C12 C13 C14 179.8(5) . . . . ? C12 C13 C14 C15 0.2(10) . . . . ? C13 C14 C15 C16 -1.0(11) . . . . ? C14 C15 C16 C17 0.3(11) . . . . ? C15 C16 C17 C12 1.3(10) . . . . ? C13 C12 C17 C16 -2.1(9) . . . . ? C2 C12 C17 C16 179.4(5) . . . . ? C36 N5 C24 C29 -113.7(4) . . . . ? Yb1 N5 C24 C29 87.3(5) . . . . ? C36 N5 C24 C25 68.6(5) . . . . ? Yb1 N5 C24 C25 -90.3(5) . . . . ? C29 C24 C25 C26 6.7(6) . . . . ? N5 C24 C25 C26 -175.6(4) . . . . ? C29 C24 C25 C30 -169.1(4) . . . . ? N5 C24 C25 C30 8.5(6) . . . . ? C24 C25 C26 C27 -2.2(6) . . . . ? C30 C25 C26 C27 173.8(4) . . . . ? C25 C26 C27 C28 -2.9(6) . . . . ? C26 C27 C28 C29 3.4(6) . . . . ? C27 C28 C29 C24 1.2(6) . . . . ? C27 C28 C29 C33 -179.8(4) . . . . ? N5 C24 C29 C28 176.0(3) . . . . ? C25 C24 C29 C28 -6.3(6) . . . . ? N5 C24 C29 C33 -3.1(5) . . . . ? C25 C24 C29 C33 174.6(4) . . . . ? C26 C25 C30 C32 -67.8(5) . . . . ? C24 C25 C30 C32 108.1(5) . . . . ? C26 C25 C30 C31 56.2(6) . . . . ? C24 C25 C30 C31 -127.9(5) . . . . ? C28 C29 C33 C35 38.6(5) . . . . ? C24 C29 C33 C35 -142.4(4) . . . . ? C28 C29 C33 C34 -86.2(5) . . . . ? C24 C29 C33 C34 92.8(5) . . . . ? Yb1 N6 C36 N5 8.2(4) . . . . ? Yb1 N6 C36 C37 -171.3(3) . . . . ? C24 N5 C36 N6 -175.3(4) . . . . ? Yb1 N5 C36 N6 -8.1(4) . . . . ? C24 N5 C36 C37 4.1(6) . . . . ? Yb1 N5 C36 C37 171.4(4) . . . . ? C24 N5 C36 Yb1 -167.2(4) . . . . ? N2 Yb1 C36 N6 -139.1(3) . . . . ? N4 Yb1 C36 N6 130.6(3) . . . . ? N5 Yb1 C36 N6 171.2(4) . . . . ? N1 Yb1 C36 N6 -83.6(3) . . . . ? N3 Yb1 C36 N6 75.3(3) . . . . ? N7 Yb1 C36 N6 -9.4(4) . . . . ? C1 Yb1 C36 N6 -108.2(3) . . . . ? C2 Yb1 C36 N6 100.8(3) . . . . ? N2 Yb1 C36 N5 49.7(3) . . . . ? N4 Yb1 C36 N5 -40.6(3) . . . . ? N6 Yb1 C36 N5 -171.2(4) . . . . ? N1 Yb1 C36 N5 105.2(2) . . . . ? N3 Yb1 C36 N5 -95.9(2) . . . . ? N7 Yb1 C36 N5 179.4(2) . . . . ? C1 Yb1 C36 N5 80.6(3) . . . . ? C2 Yb1 C36 N5 -70.4(3) . . . . ? N2 Yb1 C36 C37 -63(2) . . . . ? N4 Yb1 C36 C37 -153(2) . . . . ? N6 Yb1 C36 C37 76(2) . . . . ? N5 Yb1 C36 C37 -113(2) . . . . ? N1 Yb1 C36 C37 -7(2) . . . . ? N3 Yb1 C36 C37 151(2) . . . . ? N7 Yb1 C36 C37 67(2) . . . . ? C1 Yb1 C36 C37 -32(2) . . . . ? C2 Yb1 C36 C37 177(2) . . . . ? N6 C36 C37 C38 36.6(6) . . . . ? N5 C36 C37 C38 -142.8(4) . . . . ? Yb1 C36 C37 C38 -35(2) . . . . ? N6 C36 C37 C42 -142.7(4) . . . . ? N5 C36 C37 C42 37.9(6) . . . . ? Yb1 C36 C37 C42 145.8(19) . . . . ? C42 C37 C38 C39 0.9(7) . . . . ? C36 C37 C38 C39 -178.4(4) . . . . ? C37 C38 C39 C40 0.2(7) . . . . ? C38 C39 C40 C41 -1.2(8) . . . . ? C39 C40 C41 C42 1.0(8) . . . . ? C40 C41 C42 C37 0.2(8) . . . . ? C38 C37 C42 C41 -1.1(7) . . . . ? C36 C37 C42 C41 178.2(4) . . . . ? Yb1 N7 C43 C44 -34(24) . . . . ? N7 C43 C44 C45 -20(22) . . . . ? N7 C43 C44 C49 160(22) . . . . ? C49 C44 C45 C46 1.1(8) . . . . ? C43 C44 C45 C46 -179.5(5) . . . . ? C44 C45 C46 C47 -1.7(9) . . . . ? C45 C46 C47 C48 1.3(9) . . . . ? C46 C47 C48 C49 -0.3(9) . . . . ? C45 C44 C49 C48 -0.2(8) . . . . ? C43 C44 C49 C48 -179.5(5) . . . . ? C47 C48 C49 C44 -0.2(9) . . . . ? C55 C50 C51 C52 -3.2(9) . . . . ? C56 C50 C51 C52 178.1(6) . . . . ? C50 C51 C52 C53 3.0(10) . . . . ? C51 C52 C53 C54 -0.6(11) . . . . ? C52 C53 C54 C55 -1.6(12) . . . . ? C53 C54 C55 C50 1.2(11) . . . . ? C51 C50 C55 C54 1.2(9) . . . . ? C56 C50 C55 C54 179.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.789 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.078 # Attachment '- shelxl 10.cif' data_shelxl10 _database_code_depnum_ccdc_archive 'CCDC 862448' #TrackingRef '- shelxl 10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H66 N7 O2 Si2 Yb, 2(0.5(C7 H8))' _chemical_formula_sum 'C58 H74 N7 O2 Si2 Yb' _chemical_formula_weight 1130.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8432(9) _cell_length_b 20.1542(13) _cell_length_c 22.7598(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.886(2) _cell_angle_gamma 90.00 _cell_volume 5835.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 24983 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2340 _exptl_absorpt_coefficient_mu 1.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.497 _exptl_absorpt_correction_T_max 0.780 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29811 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_sigmaI/netI 0.0896 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10830 _reflns_number_gt 8632 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+5.9940P] 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 10830 _refine_ls_number_parameters 607 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.1505 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.195 _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 Yb1 Yb 0.46821(2) 0.203522(14) 0.316058(14) 0.04118(12) Uani 1 1 d . A . Si1 Si 0.76774(18) 0.17142(12) 0.35552(11) 0.0566(6) Uani 1 1 d . . . Si2 Si 0.2478(2) 0.08255(11) 0.26039(11) 0.0619(6) Uani 1 1 d D . . O1 O 0.6209(5) 0.0871(3) 0.4935(3) 0.0670(16) Uani 1 1 d . A . O2 O 0.4916(5) 0.0157(3) 0.1297(3) 0.0761(17) Uani 1 1 d . . . N1 N 0.6571(5) 0.2188(3) 0.3351(3) 0.0510(16) Uani 1 1 d . . . N2 N 0.5492(5) 0.3021(3) 0.3018(3) 0.0559(17) Uani 1 1 d . . . N3 N 0.3031(5) 0.1594(3) 0.2688(3) 0.0467(15) Uani 1 1 d . A . N4 N 0.3458(5) 0.2661(3) 0.2584(3) 0.0499(16) Uani 1 1 d . A . N5 N 0.4244(4) 0.2173(3) 0.4121(2) 0.0366(13) Uani 1 1 d . A . N6 N 0.4814(5) 0.1179(3) 0.3860(3) 0.0503(16) Uani 1 1 d . A . H6 H 0.4985 0.0763 0.3842 0.060 Uiso 1 1 calc R . . N7 N 0.5299(6) 0.1455(4) 0.2300(3) 0.0648(19) Uani 1 1 d . . . C1 C 0.6450(6) 0.2788(4) 0.3100(3) 0.0467(18) Uani 1 1 d . . . C2 C 0.2814(6) 0.2170(4) 0.2406(3) 0.0444(17) Uani 1 1 d . . . C3 C 0.5214(6) 0.3655(4) 0.2709(4) 0.056(2) Uani 1 1 d . . . H3A H 0.5385 0.3630 0.2304 0.067 Uiso 1 1 calc R . . H3B H 0.5629 0.4014 0.2915 0.067 Uiso 1 1 calc R . . C4 C 0.4066(6) 0.3805(4) 0.2692(4) 0.058(2) Uani 1 1 d . A . H4A H 0.3932 0.4254 0.2534 0.069 Uiso 1 1 calc R . . H4B H 0.3896 0.3801 0.3098 0.069 Uiso 1 1 calc R . . C5 C 0.3339(6) 0.3328(3) 0.2322(4) 0.057(2) Uani 1 1 d . . . H5A H 0.2609 0.3476 0.2308 0.068 Uiso 1 1 calc R A . H5B H 0.3509 0.3317 0.1915 0.068 Uiso 1 1 calc R . . C6 C 0.7350(6) 0.3171(4) 0.2895(4) 0.0505(19) Uani 1 1 d . . . C7 C 0.8060(6) 0.3485(4) 0.3313(4) 0.066(2) Uani 1 1 d . . . H7 H 0.7978 0.3473 0.3717 0.079 Uiso 1 1 calc R . . C8 C 0.8902(7) 0.3821(4) 0.3124(6) 0.084(3) Uani 1 1 d . . . H8 H 0.9395 0.4036 0.3403 0.101 Uiso 1 1 calc R . . C9 C 0.9018(8) 0.3840(5) 0.2536(7) 0.088(3) Uani 1 1 d . . . H9 H 0.9594 0.4065 0.2415 0.106 Uiso 1 1 calc R . . C10 C 0.8304(9) 0.3536(5) 0.2122(5) 0.087(3) Uani 1 1 d . . . H10 H 0.8385 0.3555 0.1718 0.105 Uiso 1 1 calc R . . C11 C 0.7449(7) 0.3194(4) 0.2302(4) 0.068(2) Uani 1 1 d . . . H11 H 0.6952 0.2984 0.2021 0.081 Uiso 1 1 calc R . . C12 C 0.1891(6) 0.2265(3) 0.1927(3) 0.0453(18) Uani 1 1 d . A . C13 C 0.0880(7) 0.2263(4) 0.2061(4) 0.061(2) Uani 1 1 d . . . H13 H 0.0755 0.2197 0.2454 0.073 Uiso 1 1 calc R A . C14 C 0.0039(8) 0.2359(5) 0.1610(5) 0.083(3) Uani 1 1 d . A . H14 H -0.0653 0.2363 0.1701 0.100 Uiso 1 1 calc R . . C15 C 0.0222(9) 0.2447(5) 0.1040(5) 0.084(3) Uani 1 1 d . . . H15 H -0.0344 0.2514 0.0737 0.101 Uiso 1 1 calc R A . C16 C 0.1225(9) 0.2438(5) 0.0907(4) 0.080(3) Uani 1 1 d . A . H16 H 0.1345 0.2494 0.0511 0.096 Uiso 1 1 calc R . . C17 C 0.2066(7) 0.2347(4) 0.1345(3) 0.055(2) Uani 1 1 d . . . H17 H 0.2755 0.2341 0.1250 0.066 Uiso 1 1 calc R A . C18 C 0.8747(7) 0.1821(5) 0.3076(4) 0.080(3) Uani 1 1 d . . . H18A H 0.8448 0.1791 0.2661 0.120 Uiso 1 1 calc R . . H18B H 0.9270 0.1475 0.3167 0.120 Uiso 1 1 calc R . . H18C H 0.9076 0.2251 0.3152 0.120 Uiso 1 1 calc R . . C19 C 0.7273(7) 0.0828(4) 0.3517(4) 0.074(3) Uani 1 1 d . . . H19A H 0.6734 0.0756 0.3770 0.110 Uiso 1 1 calc R . . H19B H 0.7877 0.0550 0.3650 0.110 Uiso 1 1 calc R . . H19C H 0.6998 0.0715 0.3111 0.110 Uiso 1 1 calc R . . C20 C 0.8275(8) 0.1901(4) 0.4333(4) 0.075(3) Uani 1 1 d . . . H20A H 0.8498 0.2361 0.4361 0.113 Uiso 1 1 calc R . . H20B H 0.8877 0.1615 0.4443 0.113 Uiso 1 1 calc R . . H20C H 0.7759 0.1824 0.4600 0.113 Uiso 1 1 calc R . . C21 C 0.1247(18) 0.0734(10) 0.2106(12) 0.108(4) Uani 0.50 1 d P A 1 H21A H 0.0789 0.1106 0.2159 0.163 Uiso 0.50 1 calc PR A 1 H21B H 0.0907 0.0324 0.2195 0.163 Uiso 0.50 1 calc PR A 1 H21C H 0.1391 0.0725 0.1699 0.163 Uiso 0.50 1 calc PR A 1 C21' C 0.2011(19) 0.0620(10) 0.1805(11) 0.108(4) Uani 0.50 1 d P A 2 H21D H 0.1640 0.0998 0.1613 0.163 Uiso 0.50 1 calc PR A 2 H21E H 0.1542 0.0241 0.1784 0.163 Uiso 0.50 1 calc PR A 2 H21F H 0.2611 0.0515 0.1605 0.163 Uiso 0.50 1 calc PR A 2 C22 C 0.1948(18) 0.0683(11) 0.3338(8) 0.108(4) Uani 0.50 1 d PD A 1 H22A H 0.2530 0.0645 0.3656 0.163 Uiso 0.50 1 calc PR A 1 H22B H 0.1537 0.0277 0.3314 0.163 Uiso 0.50 1 calc PR A 1 H22C H 0.1506 0.1054 0.3417 0.163 Uiso 0.50 1 calc PR A 1 C22' C 0.1407(15) 0.0701(11) 0.3037(10) 0.108(4) Uani 0.50 1 d PD A 2 H22D H 0.1470 0.1017 0.3362 0.163 Uiso 0.50 1 calc PR A 2 H22E H 0.1438 0.0253 0.3195 0.163 Uiso 0.50 1 calc PR A 2 H22F H 0.0741 0.0767 0.2787 0.163 Uiso 0.50 1 calc PR A 2 C23 C 0.351(3) 0.0197(18) 0.264(2) 0.108(4) Uani 0.50 1 d PD A 1 H23A H 0.3686 0.0115 0.2251 0.163 Uiso 0.50 1 calc PR A 1 H23B H 0.3255 -0.0211 0.2803 0.163 Uiso 0.50 1 calc PR A 1 H23C H 0.4123 0.0351 0.2902 0.163 Uiso 0.50 1 calc PR A 1 C23' C 0.351(3) 0.0202(18) 0.280(2) 0.108(4) Uani 0.50 1 d PD A 2 H23D H 0.4156 0.0348 0.2660 0.163 Uiso 0.50 1 calc PR A 2 H23E H 0.3293 -0.0218 0.2613 0.163 Uiso 0.50 1 calc PR A 2 H23F H 0.3636 0.0147 0.3226 0.163 Uiso 0.50 1 calc PR A 2 C24 C 0.3983(6) 0.2663(3) 0.4527(3) 0.0417(16) Uani 1 1 d . . . C25 C 0.2972(6) 0.2943(3) 0.4428(3) 0.0460(18) Uani 1 1 d . . . C26 C 0.2715(6) 0.3423(4) 0.4829(4) 0.055(2) Uani 1 1 d . . . H26 H 0.2035 0.3606 0.4776 0.066 Uiso 1 1 calc R . . C27 C 0.3424(7) 0.3634(4) 0.5297(4) 0.060(2) Uani 1 1 d . . . H27 H 0.3229 0.3953 0.5562 0.072 Uiso 1 1 calc R . . C28 C 0.4416(7) 0.3377(4) 0.5373(4) 0.062(2) Uani 1 1 d . . . H28 H 0.4905 0.3531 0.5689 0.074 Uiso 1 1 calc R . . C29 C 0.4727(6) 0.2893(3) 0.4995(3) 0.0501(19) Uani 1 1 d . . . C30 C 0.2162(6) 0.2732(4) 0.3920(3) 0.055(2) Uani 1 1 d . . . H30 H 0.2527 0.2463 0.3647 0.065 Uiso 1 1 calc R . . C31 C 0.1303(9) 0.2299(7) 0.4123(6) 0.127(5) Uani 1 1 d . . . H31A H 0.1595 0.1871 0.4251 0.191 Uiso 1 1 calc R . . H31B H 0.0741 0.2238 0.3796 0.191 Uiso 1 1 calc R . . H31C H 0.1026 0.2514 0.4450 0.191 Uiso 1 1 calc R . . C32 C 0.1665(8) 0.3312(5) 0.3573(4) 0.087(3) Uani 1 1 d . . . H32A H 0.1254 0.3567 0.3820 0.130 Uiso 1 1 calc R . . H32B H 0.1210 0.3152 0.3227 0.130 Uiso 1 1 calc R . . H32C H 0.2209 0.3592 0.3449 0.130 Uiso 1 1 calc R . . C33 C 0.5867(6) 0.2664(4) 0.5092(4) 0.054(2) Uani 1 1 d . . . H33 H 0.5919 0.2274 0.4833 0.065 Uiso 1 1 calc R . . C34 C 0.6231(8) 0.2442(4) 0.5730(4) 0.077(3) Uani 1 1 d . . . H34A H 0.6270 0.2824 0.5991 0.115 Uiso 1 1 calc R . . H34B H 0.6920 0.2238 0.5753 0.115 Uiso 1 1 calc R . . H34C H 0.5735 0.2124 0.5850 0.115 Uiso 1 1 calc R . . C35 C 0.6568(6) 0.3198(4) 0.4893(4) 0.070(3) Uani 1 1 d . . . H35A H 0.6324 0.3314 0.4484 0.106 Uiso 1 1 calc R . . H35B H 0.7284 0.3035 0.4926 0.106 Uiso 1 1 calc R . . H35C H 0.6544 0.3587 0.5142 0.106 Uiso 1 1 calc R . . C36 C 0.4541(6) 0.1548(3) 0.4290(3) 0.0440(17) Uani 1 1 d . . . C37 C 0.4483(6) 0.1275(3) 0.4899(3) 0.0491(19) Uani 1 1 d . A . C38 C 0.5330(7) 0.0917(4) 0.5204(4) 0.058(2) Uani 1 1 d . . . C39 C 0.5243(9) 0.0639(4) 0.5755(4) 0.073(3) Uani 1 1 d . A . H39 H 0.5808 0.0401 0.5961 0.088 Uiso 1 1 calc R . . C40 C 0.4329(10) 0.0714(4) 0.5994(4) 0.084(3) Uani 1 1 d . . . H40 H 0.4272 0.0520 0.6364 0.101 Uiso 1 1 calc R A . C41 C 0.3487(9) 0.1066(5) 0.5708(4) 0.082(3) Uani 1 1 d . A . H41 H 0.2866 0.1114 0.5880 0.098 Uiso 1 1 calc R . . C42 C 0.3574(7) 0.1348(4) 0.5163(4) 0.061(2) Uani 1 1 d . . . H42 H 0.3008 0.1594 0.4966 0.074 Uiso 1 1 calc R A . C43 C 0.7079(7) 0.0490(5) 0.5231(4) 0.087(3) Uani 1 1 d . . . H43A H 0.7355 0.0706 0.5601 0.131 Uiso 1 1 calc R A . H43B H 0.7627 0.0461 0.4978 0.131 Uiso 1 1 calc R . . H43C H 0.6840 0.0048 0.5313 0.131 Uiso 1 1 calc R . . C44 C 0.5733(7) 0.1144(4) 0.1991(4) 0.059(2) Uani 1 1 d . . . C45 C 0.6391(9) 0.0781(5) 0.1622(4) 0.0833(13) Uani 1 1 d . . . C46 C 0.5977(9) 0.0275(5) 0.1271(4) 0.0833(13) Uani 1 1 d . . . C47 C 0.6545(8) -0.0072(5) 0.0917(4) 0.0833(13) Uani 1 1 d . . . H47 H 0.6251 -0.0421 0.0674 0.100 Uiso 1 1 calc R . . C48 C 0.7596(8) 0.0119(5) 0.0933(4) 0.0833(13) Uani 1 1 d . . . H48 H 0.8018 -0.0113 0.0696 0.100 Uiso 1 1 calc R . . C49 C 0.8049(9) 0.0644(5) 0.1289(4) 0.0833(13) Uani 1 1 d . . . H49 H 0.8752 0.0773 0.1287 0.100 Uiso 1 1 calc R . . C50 C 0.7426(8) 0.0950(5) 0.1631(4) 0.0833(13) Uani 1 1 d . . . H50 H 0.7709 0.1292 0.1886 0.100 Uiso 1 1 calc R . . C51 C 0.4470(10) -0.0372(5) 0.0914(5) 0.109(4) Uani 1 1 d . . . H51A H 0.4487 -0.0249 0.0503 0.163 Uiso 1 1 calc R . . H51B H 0.3749 -0.0448 0.0978 0.163 Uiso 1 1 calc R . . H51C H 0.4876 -0.0774 0.1003 0.163 Uiso 1 1 calc R . . C52 C -0.0197(15) 1.0455(9) 0.9966(9) 0.073(5) Uiso 0.50 1 d PD . . C53 C -0.073(2) 0.9946(12) 0.9617(13) 0.094(10) Uiso 0.50 1 d PD . . C54 C -0.0338(17) 0.9289(11) 0.9665(9) 0.083(6) Uiso 0.50 1 d PD . . C55 C 0.058(2) 0.9106(15) 1.0052(13) 0.102(9) Uiso 0.50 1 d PD . . C56 C 0.109(2) 0.9624(12) 1.0400(12) 0.117(9) Uiso 0.50 1 d PD . . C57 C 0.0672(17) 1.0275(13) 1.0360(10) 0.068(7) Uiso 0.50 1 d PD . . C58 C -0.061(3) 1.1154(12) 0.9902(16) 0.130(13) Uiso 0.50 1 d PD . . C59 C 1.011(4) 1.0237(19) 0.5607(13) 0.169(14) Uiso 0.50 1 d PD . . C60 C 1.030(3) 1.0432(16) 0.5039(15) 0.169(14) Uiso 0.50 1 d PD . . C61 C 1.002(3) 1.0043(13) 0.4533(13) 0.124(10) Uiso 0.50 1 d PD . . C62 C 0.967(2) 0.9367(11) 0.4409(10) 0.096(7) Uiso 0.50 1 d PD . . C63 C 0.939(3) 0.9194(15) 0.4963(12) 0.180(15) Uiso 0.50 1 d PD . . C64 C 0.961(2) 0.9592(13) 0.5505(10) 0.116(9) Uiso 0.50 1 d PD . . C65 C 1.0455(18) 1.0641(11) 0.6167(10) 0.104(7) Uiso 0.50 1 d PD . . 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 Yb1 0.0467(2) 0.04040(19) 0.0369(2) -0.00014(14) 0.00763(14) 0.00137(15) Si1 0.0488(13) 0.0591(14) 0.0621(15) 0.0027(11) 0.0081(11) 0.0074(11) Si2 0.0659(15) 0.0484(13) 0.0688(17) 0.0073(11) 0.0000(13) -0.0082(12) O1 0.064(4) 0.067(4) 0.068(4) 0.014(3) 0.002(3) 0.011(3) O2 0.104(5) 0.059(4) 0.064(4) -0.005(3) 0.006(4) -0.004(4) N1 0.055(4) 0.048(4) 0.049(4) 0.008(3) 0.008(3) 0.007(3) N2 0.051(4) 0.055(4) 0.062(4) 0.006(3) 0.009(3) 0.001(3) N3 0.062(4) 0.038(3) 0.039(3) 0.002(3) 0.003(3) -0.005(3) N4 0.058(4) 0.039(3) 0.050(4) 0.005(3) -0.001(3) 0.001(3) N5 0.046(3) 0.034(3) 0.031(3) -0.002(2) 0.011(3) 0.003(3) N6 0.070(4) 0.034(3) 0.047(4) -0.010(3) 0.008(3) 0.004(3) N7 0.078(5) 0.069(5) 0.050(4) -0.005(4) 0.017(4) 0.003(4) C1 0.043(4) 0.056(5) 0.043(4) -0.005(4) 0.010(3) -0.004(4) C2 0.050(4) 0.050(4) 0.035(4) -0.004(3) 0.012(3) 0.004(4) C3 0.070(5) 0.043(4) 0.056(5) 0.006(4) 0.014(4) 0.008(4) C4 0.058(5) 0.039(4) 0.073(6) -0.003(4) 0.000(4) 0.008(4) C5 0.061(5) 0.042(4) 0.066(6) 0.006(4) 0.000(4) 0.007(4) C6 0.053(5) 0.045(4) 0.055(5) 0.004(4) 0.015(4) -0.006(4) C7 0.054(5) 0.052(5) 0.091(7) -0.004(5) 0.011(5) 0.001(4) C8 0.053(6) 0.053(6) 0.144(11) 0.006(6) 0.009(6) 0.001(5) C9 0.064(6) 0.067(7) 0.141(11) 0.026(7) 0.042(7) -0.003(5) C10 0.102(8) 0.083(7) 0.090(8) 0.027(6) 0.061(7) 0.021(7) C11 0.074(6) 0.065(5) 0.070(6) 0.010(5) 0.032(5) 0.010(5) C12 0.051(5) 0.041(4) 0.045(5) -0.001(3) 0.011(4) 0.004(3) C13 0.062(5) 0.067(5) 0.055(5) -0.011(4) 0.012(4) -0.004(4) C14 0.065(6) 0.089(7) 0.090(8) -0.027(6) -0.009(6) 0.011(5) C15 0.086(8) 0.071(7) 0.083(8) -0.009(6) -0.033(6) 0.015(6) C16 0.110(9) 0.080(7) 0.042(5) 0.006(5) -0.018(6) -0.005(6) C17 0.064(5) 0.058(5) 0.042(5) 0.000(4) 0.006(4) 0.000(4) C18 0.054(5) 0.095(7) 0.094(8) -0.005(6) 0.025(5) 0.004(5) C19 0.062(6) 0.052(5) 0.108(8) 0.006(5) 0.014(5) 0.015(4) C20 0.084(7) 0.077(6) 0.062(6) 0.003(5) -0.003(5) 0.022(5) C21 0.110(7) 0.053(4) 0.156(12) -0.011(6) -0.005(7) -0.018(5) C21' 0.110(7) 0.053(4) 0.156(12) -0.011(6) -0.005(7) -0.018(5) C22 0.110(7) 0.053(4) 0.156(12) -0.011(6) -0.005(7) -0.018(5) C22' 0.110(7) 0.053(4) 0.156(12) -0.011(6) -0.005(7) -0.018(5) C23 0.110(7) 0.053(4) 0.156(12) -0.011(6) -0.005(7) -0.018(5) C23' 0.110(7) 0.053(4) 0.156(12) -0.011(6) -0.005(7) -0.018(5) C24 0.046(4) 0.041(4) 0.037(4) -0.002(3) 0.002(3) -0.003(3) C25 0.051(4) 0.042(4) 0.046(5) 0.003(3) 0.009(4) -0.002(4) C26 0.060(5) 0.052(5) 0.057(5) -0.015(4) 0.021(4) 0.002(4) C27 0.076(6) 0.055(5) 0.053(5) -0.021(4) 0.019(5) -0.003(5) C28 0.071(6) 0.060(5) 0.052(5) -0.013(4) 0.000(4) -0.004(5) C29 0.061(5) 0.041(4) 0.050(5) 0.001(4) 0.014(4) -0.008(4) C30 0.051(5) 0.064(5) 0.047(5) -0.012(4) 0.001(4) 0.006(4) C31 0.108(9) 0.155(12) 0.109(10) 0.014(9) -0.021(8) -0.068(9) C32 0.081(7) 0.103(8) 0.071(7) -0.008(6) -0.010(5) 0.015(6) C33 0.057(5) 0.041(4) 0.062(5) -0.002(4) -0.001(4) 0.003(4) C34 0.098(7) 0.053(5) 0.068(6) 0.001(4) -0.023(5) 0.009(5) C35 0.053(5) 0.048(5) 0.108(8) -0.006(5) 0.003(5) -0.002(4) C36 0.049(4) 0.040(4) 0.043(4) 0.003(3) 0.011(3) -0.006(4) C37 0.069(5) 0.040(4) 0.040(4) 0.002(3) 0.014(4) -0.006(4) C38 0.082(6) 0.036(4) 0.052(5) 0.004(4) 0.002(5) -0.006(4) C39 0.120(9) 0.052(5) 0.045(5) 0.003(4) 0.003(5) 0.009(5) C40 0.159(11) 0.045(5) 0.052(6) 0.011(4) 0.026(7) -0.003(6) C41 0.115(8) 0.073(6) 0.066(6) 0.005(5) 0.047(6) -0.010(6) C42 0.084(6) 0.046(4) 0.057(5) 0.001(4) 0.023(5) -0.007(4) C43 0.084(7) 0.078(7) 0.093(8) 0.014(6) -0.011(6) 0.024(6) C44 0.077(6) 0.053(5) 0.046(5) -0.001(4) 0.013(4) 0.005(5) C45 0.102(3) 0.084(3) 0.068(3) -0.001(2) 0.024(3) 0.021(3) C46 0.102(3) 0.084(3) 0.068(3) -0.001(2) 0.024(3) 0.021(3) C47 0.102(3) 0.084(3) 0.068(3) -0.001(2) 0.024(3) 0.021(3) C48 0.102(3) 0.084(3) 0.068(3) -0.001(2) 0.024(3) 0.021(3) C49 0.102(3) 0.084(3) 0.068(3) -0.001(2) 0.024(3) 0.021(3) C50 0.102(3) 0.084(3) 0.068(3) -0.001(2) 0.024(3) 0.021(3) C51 0.152(11) 0.079(7) 0.083(8) -0.015(6) -0.026(7) -0.015(7) _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 Yb1 N4 2.284(6) . ? Yb1 N2 2.287(6) . ? Yb1 N6 2.337(6) . ? Yb1 N5 2.348(5) . ? Yb1 N3 2.412(6) . ? Yb1 N1 2.425(6) . ? Yb1 N7 2.500(7) . ? Yb1 C1 2.750(7) . ? Yb1 C2 2.765(7) . ? Yb1 C36 2.780(7) . ? Si1 N1 1.722(6) . ? Si1 C19 1.859(8) . ? Si1 C20 1.869(9) . ? Si1 C18 1.881(9) . ? Si2 N3 1.704(6) . ? Si2 C23 1.822(17) . ? Si2 C22' 1.817(16) . ? Si2 C21 1.82(2) . ? Si2 C23' 1.838(17) . ? Si2 C21' 1.88(2) . ? Si2 C22 1.910(16) . ? O1 C38 1.360(10) . ? O1 C43 1.444(9) . ? O2 C46 1.392(12) . ? O2 C51 1.445(10) . ? N1 C1 1.338(9) . ? N2 C1 1.306(9) . ? N2 C3 1.477(9) . ? N3 C2 1.336(9) . ? N4 C2 1.318(9) . ? N4 C5 1.470(9) . ? N5 C36 1.356(8) . ? N5 C24 1.424(8) . ? N6 C36 1.314(8) . ? N6 H6 0.8700 . ? N7 C44 1.144(9) . ? C1 C6 1.515(10) . ? C2 C12 1.509(10) . ? C3 C4 1.499(10) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.513(10) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C11 1.375(11) . ? C6 C7 1.378(11) . ? C7 C8 1.392(12) . ? C7 H7 0.9400 . ? C8 C9 1.367(14) . ? C8 H8 0.9400 . ? C9 C10 1.367(14) . ? C9 H9 0.9400 . ? C10 C11 1.404(12) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C13 1.374(10) . ? C12 C17 1.383(10) . ? C13 C14 1.397(12) . ? C13 H13 0.9400 . ? C14 C15 1.363(14) . ? C14 H14 0.9400 . ? C15 C16 1.363(13) . ? C15 H15 0.9400 . ? C16 C17 1.379(11) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21' H21D 0.9700 . ? C21' H21E 0.9700 . ? C21' H21F 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C22' H22D 0.9700 . ? C22' H22E 0.9700 . ? C22' H22F 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C23' H23D 0.9700 . ? C23' H23E 0.9700 . ? C23' H23F 0.9700 . ? C24 C25 1.405(10) . ? C24 C29 1.409(10) . ? C25 C26 1.400(10) . ? C25 C30 1.506(10) . ? C26 C27 1.370(11) . ? C26 H26 0.9400 . ? C27 C28 1.364(11) . ? C27 H27 0.9400 . ? C28 C29 1.394(10) . ? C28 H28 0.9400 . ? C29 C33 1.522(10) . ? C30 C32 1.504(12) . ? C30 C31 1.527(12) . ? C30 H30 0.9900 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C35 1.510(11) . ? C33 C34 1.531(11) . ? C33 H33 0.9900 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 C37 1.504(9) . ? C37 C42 1.391(10) . ? C37 C38 1.406(11) . ? C38 C39 1.392(11) . ? C39 C40 1.368(13) . ? C39 H39 0.9400 . ? C40 C41 1.380(13) . ? C40 H40 0.9400 . ? C41 C42 1.383(11) . ? C41 H41 0.9400 . ? C42 H42 0.9400 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 C45 1.465(12) . ? C45 C46 1.360(13) . ? C45 C50 1.370(13) . ? C46 C47 1.354(12) . ? C47 C48 1.399(13) . ? C47 H47 0.9400 . ? C48 C49 1.409(13) . ? C48 H48 0.9400 . ? C49 C50 1.342(12) . ? C49 H49 0.9400 . ? C50 H50 0.9400 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C52 C55 1.01(3) 3_577 ? C52 C54 1.13(3) 3_577 ? C52 C56 1.33(3) 3_577 ? C52 C57 1.379(16) . ? C52 C53 1.413(17) . ? C52 C58 1.506(18) . ? C52 C53 1.63(3) 3_577 ? C52 C57 1.72(3) 3_577 ? C52 C52 1.90(3) 3_577 ? C53 C57 0.45(3) 3_577 ? C53 C56 0.98(3) 3_577 ? C53 C54 1.414(18) . ? C53 C52 1.63(3) 3_577 ? C54 C57 0.97(2) 3_577 ? C54 C52 1.13(3) 3_577 ? C54 C55 1.421(18) . ? C54 C58 1.71(4) 3_577 ? C55 C58 0.53(4) 3_577 ? C55 C52 1.01(3) 3_577 ? C55 C56 1.414(18) . ? C56 C53 0.98(3) 3_577 ? C56 C52 1.33(3) 3_577 ? C56 C57 1.416(18) . ? C56 C58 1.78(4) 3_577 ? C57 C53 0.45(3) 3_577 ? C57 C54 0.97(2) 3_577 ? C57 C52 1.72(3) 3_577 ? C58 C55 0.53(4) 3_577 ? C58 C54 1.71(4) 3_577 ? C58 C56 1.78(4) 3_577 ? C59 C61 0.66(3) 3_776 ? C59 C62 0.85(3) 3_776 ? C59 C60 1.403(18) . ? C59 C64 1.455(19) . ? C59 C65 1.526(18) . ? C59 C63 1.91(4) 3_776 ? C59 C60 2.01(4) 3_776 ? C60 C63 0.86(4) 3_776 ? C60 C64 1.26(4) 3_776 ? C60 C62 1.31(4) 3_776 ? C60 C61 1.398(18) . ? C60 C61 1.46(4) 3_776 ? C60 C60 1.90(6) 3_776 ? C60 C59 2.01(4) 3_776 ? C61 C59 0.66(3) 3_776 ? C61 C64 0.89(3) 3_776 ? C61 C62 1.453(19) . ? C61 C60 1.46(4) 3_776 ? C61 C63 2.01(4) 3_776 ? C62 C59 0.85(3) 3_776 ? C62 C65 1.30(3) 3_776 ? C62 C60 1.31(4) 3_776 ? C62 C63 1.400(18) . ? C63 C60 0.86(4) 3_776 ? C63 C64 1.466(19) . ? C63 C59 1.91(4) 3_776 ? C63 C61 2.01(4) 3_776 ? C64 C61 0.89(3) 3_776 ? C64 C60 1.26(4) 3_776 ? C65 C62 1.30(3) 3_776 ? 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 Yb1 N2 74.3(2) . . ? N4 Yb1 N6 141.1(2) . . ? N2 Yb1 N6 138.3(2) . . ? N4 Yb1 N5 103.6(2) . . ? N2 Yb1 N5 101.6(2) . . ? N6 Yb1 N5 57.14(18) . . ? N4 Yb1 N3 56.9(2) . . ? N2 Yb1 N3 130.2(2) . . ? N6 Yb1 N3 90.5(2) . . ? N5 Yb1 N3 98.63(19) . . ? N4 Yb1 N1 128.7(2) . . ? N2 Yb1 N1 56.8(2) . . ? N6 Yb1 N1 89.7(2) . . ? N5 Yb1 N1 100.4(2) . . ? N3 Yb1 N1 157.4(2) . . ? N4 Yb1 N7 94.3(2) . . ? N2 Yb1 N7 95.5(2) . . ? N6 Yb1 N7 100.8(2) . . ? N5 Yb1 N7 157.9(2) . . ? N3 Yb1 N7 80.4(2) . . ? N1 Yb1 N7 77.4(2) . . ? N4 Yb1 C1 100.0(2) . . ? N2 Yb1 C1 28.2(2) . . ? N6 Yb1 C1 117.3(2) . . ? N5 Yb1 C1 106.7(2) . . ? N3 Yb1 C1 149.6(2) . . ? N1 Yb1 C1 29.11(19) . . ? N7 Yb1 C1 82.3(2) . . ? N4 Yb1 C2 28.3(2) . . ? N2 Yb1 C2 101.5(2) . . ? N6 Yb1 C2 118.1(2) . . ? N5 Yb1 C2 105.53(19) . . ? N3 Yb1 C2 28.89(19) . . ? N1 Yb1 C2 149.3(2) . . ? N7 Yb1 C2 84.3(2) . . ? C1 Yb1 C2 124.5(2) . . ? N4 Yb1 C36 126.8(2) . . ? N2 Yb1 C36 121.8(2) . . ? N6 Yb1 C36 28.09(19) . . ? N5 Yb1 C36 29.14(18) . . ? N3 Yb1 C36 96.7(2) . . ? N1 Yb1 C36 94.0(2) . . ? N7 Yb1 C36 128.8(2) . . ? C1 Yb1 C36 113.6(2) . . ? C2 Yb1 C36 116.6(2) . . ? N1 Si1 C19 107.8(4) . . ? N1 Si1 C20 111.1(4) . . ? C19 Si1 C20 108.3(4) . . ? N1 Si1 C18 114.9(4) . . ? C19 Si1 C18 107.7(4) . . ? C20 Si1 C18 106.8(5) . . ? N3 Si2 C23 109.8(15) . . ? N3 Si2 C22' 113.5(7) . . ? C23 Si2 C22' 118.2(18) . . ? N3 Si2 C21 118.3(7) . . ? C23 Si2 C21 121.4(15) . . ? C22' Si2 C21 70.6(11) . . ? N3 Si2 C23' 108.6(15) . . ? C23 Si2 C23' 11(3) . . ? C22' Si2 C23' 110.5(17) . . ? C21 Si2 C23' 128.1(15) . . ? N3 Si2 C21' 112.4(7) . . ? C23 Si2 C21' 91.7(15) . . ? C22' Si2 C21' 109.3(11) . . ? C21 Si2 C21' 40.8(9) . . ? C23' Si2 C21' 101.9(15) . . ? N3 Si2 C22 103.4(7) . . ? C23 Si2 C22 101.1(17) . . ? C22' Si2 C22 28.0(9) . . ? C21 Si2 C22 98.4(11) . . ? C23' Si2 C22 91.1(17) . . ? C21' Si2 C22 135.0(10) . . ? C38 O1 C43 117.6(7) . . ? C46 O2 C51 114.2(8) . . ? C1 N1 Si1 131.3(5) . . ? C1 N1 Yb1 89.0(4) . . ? Si1 N1 Yb1 138.3(3) . . ? C1 N2 C3 122.8(7) . . ? C1 N2 Yb1 96.0(5) . . ? C3 N2 Yb1 137.2(5) . . ? C2 N3 Si2 132.8(5) . . ? C2 N3 Yb1 90.4(4) . . ? Si2 N3 Yb1 135.4(3) . . ? C2 N4 C5 122.4(6) . . ? C2 N4 Yb1 96.6(4) . . ? C5 N4 Yb1 139.8(5) . . ? C36 N5 C24 122.9(6) . . ? C36 N5 Yb1 93.4(4) . . ? C24 N5 Yb1 142.6(4) . . ? C36 N6 Yb1 95.0(4) . . ? C36 N6 H6 132.5 . . ? Yb1 N6 H6 132.5 . . ? C44 N7 Yb1 166.5(7) . . ? N2 C1 N1 116.0(7) . . ? N2 C1 C6 121.0(7) . . ? N1 C1 C6 122.9(7) . . ? N2 C1 Yb1 55.8(4) . . ? N1 C1 Yb1 61.9(4) . . ? C6 C1 Yb1 165.1(5) . . ? N4 C2 N3 115.1(7) . . ? N4 C2 C12 121.6(6) . . ? N3 C2 C12 123.3(7) . . ? N4 C2 Yb1 55.1(4) . . ? N3 C2 Yb1 60.7(4) . . ? C12 C2 Yb1 171.8(5) . . ? N2 C3 C4 111.1(6) . . ? N2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 114.6(7) . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? N4 C5 C4 109.4(6) . . ? N4 C5 H5A 109.8 . . ? C4 C5 H5A 109.8 . . ? N4 C5 H5B 109.8 . . ? C4 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? C11 C6 C7 121.3(8) . . ? C11 C6 C1 119.8(7) . . ? C7 C6 C1 118.9(7) . . ? C6 C7 C8 118.6(9) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C9 C8 C7 120.7(10) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 120.6(9) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C11 119.8(10) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C6 C11 C10 119.0(10) . . ? C6 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C13 C12 C17 119.7(8) . . ? C13 C12 C2 120.7(7) . . ? C17 C12 C2 119.5(7) . . ? C12 C13 C14 119.7(9) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 120.1(10) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.1(9) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 120.7(9) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C12 119.7(8) . . ? C16 C17 H17 120.2 . . ? C12 C17 H17 120.2 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? Si2 C21' H21D 109.5 . . ? Si2 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? Si2 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? Si2 C22' H22D 109.5 . . ? Si2 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? Si2 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? Si2 C23' H23D 109.5 . . ? Si2 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? Si2 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? C25 C24 C29 120.4(7) . . ? C25 C24 N5 117.9(6) . . ? C29 C24 N5 121.6(6) . . ? C26 C25 C24 117.9(7) . . ? C26 C25 C30 119.7(7) . . ? C24 C25 C30 122.4(6) . . ? C27 C26 C25 122.0(8) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C28 C27 C26 119.4(7) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 121.9(8) . . ? C27 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C28 C29 C24 118.3(7) . . ? C28 C29 C33 118.3(7) . . ? C24 C29 C33 123.3(7) . . ? C32 C30 C25 112.5(7) . . ? C32 C30 C31 109.3(8) . . ? C25 C30 C31 112.4(7) . . ? C32 C30 H30 107.5 . . ? C25 C30 H30 107.5 . . ? C31 C30 H30 107.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C33 C29 110.0(6) . . ? C35 C33 C34 112.0(7) . . ? C29 C33 C34 112.8(7) . . ? C35 C33 H33 107.2 . . ? C29 C33 H33 107.2 . . ? C34 C33 H33 107.2 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N6 C36 N5 114.1(6) . . ? N6 C36 C37 122.1(6) . . ? N5 C36 C37 123.6(6) . . ? N6 C36 Yb1 56.9(4) . . ? N5 C36 Yb1 57.4(3) . . ? C37 C36 Yb1 178.8(5) . . ? C42 C37 C38 118.7(7) . . ? C42 C37 C36 120.6(7) . . ? C38 C37 C36 120.7(7) . . ? O1 C38 C39 123.5(8) . . ? O1 C38 C37 116.5(7) . . ? C39 C38 C37 119.9(9) . . ? C40 C39 C38 119.5(9) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 121.9(9) . . ? C39 C40 H40 119.0 . . ? C41 C40 H40 119.0 . . ? C40 C41 C42 118.7(9) . . ? C40 C41 H41 120.6 . . ? C42 C41 H41 120.6 . . ? C41 C42 C37 121.2(9) . . ? C41 C42 H42 119.4 . . ? C37 C42 H42 119.4 . . ? O1 C43 H43A 109.5 . . ? O1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N7 C44 C45 173.9(10) . . ? C46 C45 C50 119.7(10) . . ? C46 C45 C44 120.1(10) . . ? C50 C45 C44 120.2(10) . . ? C47 C46 C45 122.6(11) . . ? C47 C46 O2 123.2(10) . . ? C45 C46 O2 114.1(9) . . ? C46 C47 C48 116.0(11) . . ? C46 C47 H47 122.0 . . ? C48 C47 H47 122.0 . . ? C47 C48 C49 122.9(10) . . ? C47 C48 H48 118.5 . . ? C49 C48 H48 118.5 . . ? C50 C49 C48 116.6(10) . . ? C50 C49 H49 121.7 . . ? C48 C49 H49 121.7 . . ? C49 C50 C45 122.1(11) . . ? C49 C50 H50 118.9 . . ? C45 C50 H50 118.9 . . ? O2 C51 H51A 109.5 . . ? O2 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O2 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C55 C52 C54 82.8(19) 3_577 3_577 ? C55 C52 C56 72.9(17) 3_577 3_577 ? C54 C52 C56 154(2) 3_577 3_577 ? C55 C52 C57 127(2) 3_577 . ? C54 C52 C57 44.3(11) 3_577 . ? C56 C52 C57 157.8(17) 3_577 . ? C55 C52 C53 115(2) 3_577 . ? C54 C52 C53 160.6(18) 3_577 . ? C56 C52 C53 41.8(11) 3_577 . ? C57 C52 C53 117.3(16) . . ? C55 C52 C58 9(3) 3_577 . ? C54 C52 C58 79(2) 3_577 . ? C56 C52 C58 78(2) 3_577 . ? C57 C52 C58 124(2) . . ? C53 C52 C58 119(2) . . ? C55 C52 C53 140(3) 3_577 3_577 ? C54 C52 C53 58.4(14) 3_577 3_577 ? C56 C52 C53 143(2) 3_577 3_577 ? C57 C52 C53 14.6(13) . 3_577 ? C53 C52 C53 102.9(18) . 3_577 ? C58 C52 C53 138(2) . 3_577 ? C55 C52 C57 126(2) 3_577 3_577 ? C54 C52 C57 148.4(19) 3_577 3_577 ? C56 C52 C57 53.4(12) 3_577 3_577 ? C57 C52 C57 105.2(15) . 3_577 ? C53 C52 C57 12.2(13) . 3_577 ? C58 C52 C57 131(2) . 3_577 ? C53 C52 C57 90.8(13) 3_577 3_577 ? C55 C52 C52 166(3) 3_577 3_577 ? C54 C52 C52 104.6(18) 3_577 3_577 ? C56 C52 C52 97.6(17) 3_577 3_577 ? C57 C52 C52 60.8(14) . 3_577 ? C53 C52 C52 56.5(15) . 3_577 ? C58 C52 C52 175(2) . 3_577 ? C53 C52 C52 46.4(9) 3_577 3_577 ? C57 C52 C52 44.4(8) 3_577 3_577 ? C57 C53 C56 160(8) 3_577 3_577 ? C57 C53 C52 126(6) 3_577 . ? C56 C53 C52 65(2) 3_577 . ? C57 C53 C54 12(5) 3_577 . ? C56 C53 C54 172(4) 3_577 . ? C52 C53 C54 120(2) . . ? C57 C53 C52 50(5) 3_577 3_577 ? C56 C53 C52 140(3) 3_577 3_577 ? C52 C53 C52 77.1(18) . 3_577 ? C54 C53 C52 43.0(12) . 3_577 ? C57 C54 C52 81.4(19) 3_577 3_577 ? C57 C54 C53 6(3) 3_577 . ? C52 C54 C53 78.6(19) 3_577 . ? C57 C54 C55 126(3) 3_577 . ? C52 C54 C55 45.0(15) 3_577 . ? C53 C54 C55 123(2) . . ? C57 C54 C58 141(3) 3_577 3_577 ? C52 C54 C58 59.9(16) 3_577 3_577 ? C53 C54 C58 139(2) . 3_577 ? C55 C54 C58 16.5(18) . 3_577 ? C58 C55 C52 152(8) 3_577 3_577 ? C58 C55 C56 127(6) 3_577 . ? C52 C55 C56 64(2) 3_577 . ? C58 C55 C54 114(6) 3_577 . ? C52 C55 C54 52.2(17) 3_577 . ? C56 C55 C54 116(3) . . ? C53 C56 C52 74(2) 3_577 3_577 ? C53 C56 C55 117(3) 3_577 . ? C52 C56 C55 43.2(15) 3_577 . ? C53 C56 C57 6(3) 3_577 . ? C52 C56 C57 77.6(18) 3_577 . ? C55 C56 C57 120(2) . . ? C53 C56 C58 129(3) 3_577 3_577 ? C52 C56 C58 55.6(15) 3_577 3_577 ? C55 C56 C58 13.9(17) . 3_577 ? C57 C56 C58 133(2) . 3_577 ? C53 C57 C54 162(8) 3_577 3_577 ? C53 C57 C52 116(6) 3_577 . ? C54 C57 C52 54.3(17) 3_577 . ? C53 C57 C56 14(6) 3_577 . ? C54 C57 C56 176(3) 3_577 . ? C52 C57 C56 123(2) . . ? C53 C57 C52 41(5) 3_577 3_577 ? C54 C57 C52 128(2) 3_577 3_577 ? C52 C57 C52 74.8(15) . 3_577 ? C56 C57 C52 49.0(14) . 3_577 ? C55 C58 C52 18(5) 3_577 . ? C55 C58 C54 49(5) 3_577 3_577 ? C52 C58 C54 40.6(12) . 3_577 ? C55 C58 C56 40(5) 3_577 3_577 ? C52 C58 C56 46.7(14) . 3_577 ? C54 C58 C56 86.7(15) 3_577 3_577 ? C61 C59 C62 148(6) 3_776 3_776 ? C61 C59 C60 82(4) 3_776 . ? C62 C59 C60 66(3) 3_776 . ? C61 C59 C64 23(4) 3_776 . ? C62 C59 C64 168(4) 3_776 . ? C60 C59 C64 103(2) . . ? C61 C59 C65 153(6) 3_776 . ? C62 C59 C65 58(2) 3_776 . ? C60 C59 C65 123(3) . . ? C64 C59 C65 133(3) . . ? C61 C59 C63 106(4) 3_776 3_776 ? C62 C59 C63 42(2) 3_776 3_776 ? C60 C59 C63 24.4(16) . 3_776 ? C64 C59 C63 127.8(18) . 3_776 ? C65 C59 C63 99(2) . 3_776 ? C61 C59 C60 18(4) 3_776 3_776 ? C62 C59 C60 131(4) 3_776 3_776 ? C60 C59 C60 65(2) . 3_776 ? C64 C59 C60 38.7(12) . 3_776 ? C65 C59 C60 170(3) . 3_776 ? C63 C59 C60 89(2) 3_776 3_776 ? C63 C60 C64 85(3) 3_776 3_776 ? C63 C60 C62 77(3) 3_776 3_776 ? C64 C60 C62 162(3) 3_776 3_776 ? C63 C60 C61 124(3) 3_776 . ? C64 C60 C61 38.7(14) 3_776 . ? C62 C60 C61 159(3) 3_776 . ? C63 C60 C59 113(3) 3_776 . ? C64 C60 C59 161(3) 3_776 . ? C62 C60 C59 36.4(15) 3_776 . ? C61 C60 C59 123(2) . . ? C63 C60 C61 139(4) 3_776 3_776 ? C64 C60 C61 135(3) 3_776 3_776 ? C62 C60 C61 63(2) 3_776 3_776 ? C61 C60 C61 97(3) . 3_776 ? C59 C60 C61 26.4(15) . 3_776 ? C63 C60 C60 172(5) 3_776 3_776 ? C64 C60 C60 88(2) 3_776 3_776 ? C62 C60 C60 110(3) 3_776 3_776 ? C61 C60 C60 49.8(18) . 3_776 ? C59 C60 C60 73.2(19) . 3_776 ? C61 C60 C60 47.0(15) 3_776 3_776 ? C63 C60 C59 131(4) 3_776 3_776 ? C64 C60 C59 46.2(15) 3_776 3_776 ? C62 C60 C59 151(3) 3_776 3_776 ? C61 C60 C59 8.3(16) . 3_776 ? C59 C60 C59 115(2) . 3_776 ? C61 C60 C59 89(2) 3_776 3_776 ? C60 C60 C59 42.0(10) 3_776 3_776 ? C59 C61 C64 140(6) 3_776 3_776 ? C59 C61 C60 154(5) 3_776 . ? C64 C61 C60 62(3) 3_776 . ? C59 C61 C62 18(4) 3_776 . ? C64 C61 C62 156(4) 3_776 . ? C60 C61 C62 136(2) . . ? C59 C61 C60 72(3) 3_776 3_776 ? C64 C61 C60 144(5) 3_776 3_776 ? C60 C61 C60 83(3) . 3_776 ? C62 C61 C60 53.6(17) . 3_776 ? C59 C61 C63 170(8) 3_776 3_776 ? C64 C61 C63 42(2) 3_776 3_776 ? C60 C61 C63 20.8(14) . 3_776 ? C62 C61 C63 156(2) . 3_776 ? C60 C61 C63 104(3) 3_776 3_776 ? C59 C62 C65 88(2) 3_776 3_776 ? C59 C62 C60 77(3) 3_776 3_776 ? C65 C62 C60 162(3) 3_776 3_776 ? C59 C62 C63 114(3) 3_776 . ? C65 C62 C63 154(3) 3_776 . ? C60 C62 C63 36.6(18) 3_776 . ? C59 C62 C61 14(3) 3_776 . ? C65 C62 C61 101(2) 3_776 . ? C60 C62 C61 63.5(17) 3_776 . ? C63 C62 C61 100(2) . . ? C60 C63 C62 66(3) 3_776 . ? C60 C63 C64 59(3) 3_776 . ? C62 C63 C64 125(2) . . ? C60 C63 C59 42(2) 3_776 3_776 ? C62 C63 C59 24.2(12) . 3_776 ? C64 C63 C59 101.5(19) . 3_776 ? C60 C63 C61 35(2) 3_776 3_776 ? C62 C63 C61 102(2) . 3_776 ? C64 C63 C61 23.8(13) . 3_776 ? C59 C63 C61 77.9(15) 3_776 3_776 ? C61 C64 C60 79(3) 3_776 3_776 ? C61 C64 C59 17(3) 3_776 . ? C60 C64 C59 95(2) 3_776 . ? C61 C64 C63 114(3) 3_776 . ? C60 C64 C63 35.6(18) 3_776 . ? C59 C64 C63 131(2) . . ? C62 C65 C59 34.0(14) 3_776 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 Si1 N1 C1 -152.1(7) . . . . ? C20 Si1 N1 C1 89.5(8) . . . . ? C18 Si1 N1 C1 -32.0(8) . . . . ? C19 Si1 N1 Yb1 10.1(6) . . . . ? C20 Si1 N1 Yb1 -108.4(6) . . . . ? C18 Si1 N1 Yb1 130.2(5) . . . . ? N4 Yb1 N1 C1 11.4(5) . . . . ? N2 Yb1 N1 C1 -8.5(4) . . . . ? N6 Yb1 N1 C1 -162.1(4) . . . . ? N5 Yb1 N1 C1 -105.6(4) . . . . ? N3 Yb1 N1 C1 107.3(6) . . . . ? N7 Yb1 N1 C1 96.8(4) . . . . ? C2 Yb1 N1 C1 41.9(6) . . . . ? C36 Yb1 N1 C1 -134.3(4) . . . . ? N4 Yb1 N1 Si1 -155.3(4) . . . . ? N2 Yb1 N1 Si1 -175.2(6) . . . . ? N6 Yb1 N1 Si1 31.2(5) . . . . ? N5 Yb1 N1 Si1 87.7(5) . . . . ? N3 Yb1 N1 Si1 -59.4(8) . . . . ? N7 Yb1 N1 Si1 -69.9(5) . . . . ? C1 Yb1 N1 Si1 -166.7(8) . . . . ? C2 Yb1 N1 Si1 -124.8(5) . . . . ? C36 Yb1 N1 Si1 59.0(5) . . . . ? N4 Yb1 N2 C1 -155.3(5) . . . . ? N6 Yb1 N2 C1 50.6(6) . . . . ? N5 Yb1 N2 C1 103.7(5) . . . . ? N3 Yb1 N2 C1 -144.3(4) . . . . ? N1 Yb1 N2 C1 8.7(4) . . . . ? N7 Yb1 N2 C1 -62.3(5) . . . . ? C2 Yb1 N2 C1 -147.6(5) . . . . ? C36 Yb1 N2 C1 80.8(5) . . . . ? N4 Yb1 N2 C3 0.8(7) . . . . ? N6 Yb1 N2 C3 -153.3(6) . . . . ? N5 Yb1 N2 C3 -100.3(7) . . . . ? N3 Yb1 N2 C3 11.7(9) . . . . ? N1 Yb1 N2 C3 164.8(8) . . . . ? N7 Yb1 N2 C3 93.8(7) . . . . ? C1 Yb1 N2 C3 156.1(10) . . . . ? C2 Yb1 N2 C3 8.4(8) . . . . ? C36 Yb1 N2 C3 -123.1(7) . . . . ? C23 Si2 N3 C2 136.3(17) . . . . ? C22' Si2 N3 C2 -88.8(11) . . . . ? C21 Si2 N3 C2 -9.1(13) . . . . ? C23' Si2 N3 C2 147.8(17) . . . . ? C21' Si2 N3 C2 35.9(11) . . . . ? C22 Si2 N3 C2 -116.4(10) . . . . ? C23 Si2 N3 Yb1 -25.8(16) . . . . ? C22' Si2 N3 Yb1 109.0(9) . . . . ? C21 Si2 N3 Yb1 -171.3(10) . . . . ? C23' Si2 N3 Yb1 -14.3(16) . . . . ? C21' Si2 N3 Yb1 -126.3(9) . . . . ? C22 Si2 N3 Yb1 81.4(9) . . . . ? N4 Yb1 N3 C2 5.9(4) . . . . ? N2 Yb1 N3 C2 -6.7(5) . . . . ? N6 Yb1 N3 C2 163.4(4) . . . . ? N5 Yb1 N3 C2 106.6(4) . . . . ? N1 Yb1 N3 C2 -106.2(6) . . . . ? N7 Yb1 N3 C2 -95.7(4) . . . . ? C1 Yb1 N3 C2 -39.7(6) . . . . ? C36 Yb1 N3 C2 135.9(4) . . . . ? N4 Yb1 N3 Si2 172.9(6) . . . . ? N2 Yb1 N3 Si2 160.3(4) . . . . ? N6 Yb1 N3 Si2 -29.6(5) . . . . ? N5 Yb1 N3 Si2 -86.4(5) . . . . ? N1 Yb1 N3 Si2 60.8(7) . . . . ? N7 Yb1 N3 Si2 71.3(5) . . . . ? C1 Yb1 N3 Si2 127.3(5) . . . . ? C2 Yb1 N3 Si2 167.0(7) . . . . ? C36 Yb1 N3 Si2 -57.0(5) . . . . ? N2 Yb1 N4 C2 164.0(5) . . . . ? N6 Yb1 N4 C2 -43.6(6) . . . . ? N5 Yb1 N4 C2 -97.5(4) . . . . ? N3 Yb1 N4 C2 -6.0(4) . . . . ? N1 Yb1 N4 C2 146.8(4) . . . . ? N7 Yb1 N4 C2 69.5(5) . . . . ? C1 Yb1 N4 C2 152.4(4) . . . . ? C36 Yb1 N4 C2 -77.8(5) . . . . ? N2 Yb1 N4 C5 -2.5(7) . . . . ? N6 Yb1 N4 C5 149.9(7) . . . . ? N5 Yb1 N4 C5 95.9(8) . . . . ? N3 Yb1 N4 C5 -172.6(8) . . . . ? N1 Yb1 N4 C5 -19.7(9) . . . . ? N7 Yb1 N4 C5 -97.0(8) . . . . ? C1 Yb1 N4 C5 -14.1(8) . . . . ? C2 Yb1 N4 C5 -166.5(10) . . . . ? C36 Yb1 N4 C5 115.7(8) . . . . ? N4 Yb1 N5 C36 146.2(4) . . . . ? N2 Yb1 N5 C36 -137.4(4) . . . . ? N6 Yb1 N5 C36 3.3(4) . . . . ? N3 Yb1 N5 C36 88.3(4) . . . . ? N1 Yb1 N5 C36 -79.4(4) . . . . ? N7 Yb1 N5 C36 2.7(8) . . . . ? C1 Yb1 N5 C36 -108.7(4) . . . . ? C2 Yb1 N5 C36 117.1(4) . . . . ? N4 Yb1 N5 C24 -47.1(8) . . . . ? N2 Yb1 N5 C24 29.3(8) . . . . ? N6 Yb1 N5 C24 170.0(8) . . . . ? N3 Yb1 N5 C24 -105.0(7) . . . . ? N1 Yb1 N5 C24 87.2(7) . . . . ? N7 Yb1 N5 C24 169.4(7) . . . . ? C1 Yb1 N5 C24 58.0(8) . . . . ? C2 Yb1 N5 C24 -76.3(7) . . . . ? C36 Yb1 N5 C24 166.7(10) . . . . ? N4 Yb1 N6 C36 -72.7(5) . . . . ? N2 Yb1 N6 C36 65.2(6) . . . . ? N5 Yb1 N6 C36 -3.5(4) . . . . ? N3 Yb1 N6 C36 -103.4(5) . . . . ? N1 Yb1 N6 C36 99.2(5) . . . . ? N7 Yb1 N6 C36 176.3(4) . . . . ? C1 Yb1 N6 C36 89.5(5) . . . . ? C2 Yb1 N6 C36 -94.4(5) . . . . ? N4 Yb1 N7 C44 171(3) . . . . ? N2 Yb1 N7 C44 97(3) . . . . ? N6 Yb1 N7 C44 -45(3) . . . . ? N5 Yb1 N7 C44 -44(3) . . . . ? N3 Yb1 N7 C44 -133(3) . . . . ? N1 Yb1 N7 C44 42(3) . . . . ? C1 Yb1 N7 C44 72(3) . . . . ? C2 Yb1 N7 C44 -162(3) . . . . ? C36 Yb1 N7 C44 -43(3) . . . . ? C3 N2 C1 N1 -175.7(7) . . . . ? Yb1 N2 C1 N1 -14.9(7) . . . . ? C3 N2 C1 C6 1.9(11) . . . . ? Yb1 N2 C1 C6 162.7(6) . . . . ? C3 N2 C1 Yb1 -160.8(8) . . . . ? Si1 N1 C1 N2 -177.8(6) . . . . ? Yb1 N1 C1 N2 13.9(7) . . . . ? Si1 N1 C1 C6 4.6(11) . . . . ? Yb1 N1 C1 C6 -163.6(7) . . . . ? Si1 N1 C1 Yb1 168.2(7) . . . . ? N4 Yb1 C1 N2 24.2(5) . . . . ? N6 Yb1 C1 N2 -144.6(5) . . . . ? N5 Yb1 C1 N2 -83.5(5) . . . . ? N3 Yb1 C1 N2 61.6(6) . . . . ? N1 Yb1 C1 N2 -164.8(7) . . . . ? N7 Yb1 C1 N2 117.2(5) . . . . ? C2 Yb1 C1 N2 39.6(5) . . . . ? C36 Yb1 C1 N2 -113.7(5) . . . . ? N4 Yb1 C1 N1 -171.0(4) . . . . ? N2 Yb1 C1 N1 164.8(7) . . . . ? N6 Yb1 C1 N1 20.2(5) . . . . ? N5 Yb1 C1 N1 81.4(4) . . . . ? N3 Yb1 C1 N1 -133.6(5) . . . . ? N7 Yb1 C1 N1 -77.9(4) . . . . ? C2 Yb1 C1 N1 -155.6(4) . . . . ? C36 Yb1 C1 N1 51.2(5) . . . . ? N4 Yb1 C1 C6 -58(2) . . . . ? N2 Yb1 C1 C6 -83(2) . . . . ? N6 Yb1 C1 C6 133(2) . . . . ? N5 Yb1 C1 C6 -166(2) . . . . ? N3 Yb1 C1 C6 -21(2) . . . . ? N1 Yb1 C1 C6 113(2) . . . . ? N7 Yb1 C1 C6 35(2) . . . . ? C2 Yb1 C1 C6 -43(2) . . . . ? C36 Yb1 C1 C6 164(2) . . . . ? C5 N4 C2 N3 179.8(6) . . . . ? Yb1 N4 C2 N3 10.1(7) . . . . ? C5 N4 C2 C12 -1.3(11) . . . . ? Yb1 N4 C2 C12 -171.0(6) . . . . ? C5 N4 C2 Yb1 169.7(8) . . . . ? Si2 N3 C2 N4 -177.1(5) . . . . ? Yb1 N3 C2 N4 -9.5(6) . . . . ? Si2 N3 C2 C12 4.1(11) . . . . ? Yb1 N3 C2 C12 171.6(6) . . . . ? Si2 N3 C2 Yb1 -167.6(7) . . . . ? N2 Yb1 C2 N4 -15.7(5) . . . . ? N6 Yb1 C2 N4 150.6(4) . . . . ? N5 Yb1 C2 N4 90.0(5) . . . . ? N3 Yb1 C2 N4 169.5(7) . . . . ? N1 Yb1 C2 N4 -56.8(6) . . . . ? N7 Yb1 C2 N4 -110.2(5) . . . . ? C1 Yb1 C2 N4 -33.6(5) . . . . ? C36 Yb1 C2 N4 119.0(4) . . . . ? N4 Yb1 C2 N3 -169.5(7) . . . . ? N2 Yb1 C2 N3 174.8(4) . . . . ? N6 Yb1 C2 N3 -18.9(5) . . . . ? N5 Yb1 C2 N3 -79.5(4) . . . . ? N1 Yb1 C2 N3 133.7(5) . . . . ? N7 Yb1 C2 N3 80.3(4) . . . . ? C1 Yb1 C2 N3 156.9(4) . . . . ? C36 Yb1 C2 N3 -50.5(5) . . . . ? N4 Yb1 C2 C12 69(4) . . . . ? N2 Yb1 C2 C12 53(4) . . . . ? N6 Yb1 C2 C12 -140(4) . . . . ? N5 Yb1 C2 C12 159(4) . . . . ? N3 Yb1 C2 C12 -122(4) . . . . ? N1 Yb1 C2 C12 12(4) . . . . ? N7 Yb1 C2 C12 -41(4) . . . . ? C1 Yb1 C2 C12 35(4) . . . . ? C36 Yb1 C2 C12 -172(4) . . . . ? C1 N2 C3 C4 -178.8(7) . . . . ? Yb1 N2 C3 C4 29.9(10) . . . . ? N2 C3 C4 C5 -66.1(9) . . . . ? C2 N4 C5 C4 169.7(7) . . . . ? Yb1 N4 C5 C4 -26.2(11) . . . . ? C3 C4 C5 N4 63.6(9) . . . . ? N2 C1 C6 C11 -74.7(10) . . . . ? N1 C1 C6 C11 102.7(9) . . . . ? Yb1 C1 C6 C11 -2(2) . . . . ? N2 C1 C6 C7 105.9(9) . . . . ? N1 C1 C6 C7 -76.7(10) . . . . ? Yb1 C1 C6 C7 179.1(17) . . . . ? C11 C6 C7 C8 -1.2(12) . . . . ? C1 C6 C7 C8 178.2(7) . . . . ? C6 C7 C8 C9 0.3(13) . . . . ? C7 C8 C9 C10 0.6(15) . . . . ? C8 C9 C10 C11 -0.6(15) . . . . ? C7 C6 C11 C10 1.1(12) . . . . ? C1 C6 C11 C10 -178.3(7) . . . . ? C9 C10 C11 C6 -0.2(13) . . . . ? N4 C2 C12 C13 -109.1(9) . . . . ? N3 C2 C12 C13 69.7(10) . . . . ? Yb1 C2 C12 C13 -173(3) . . . . ? N4 C2 C12 C17 71.7(9) . . . . ? N3 C2 C12 C17 -109.5(8) . . . . ? Yb1 C2 C12 C17 8(4) . . . . ? C17 C12 C13 C14 -1.5(12) . . . . ? C2 C12 C13 C14 179.4(7) . . . . ? C12 C13 C14 C15 0.7(14) . . . . ? C13 C14 C15 C16 0.4(15) . . . . ? C14 C15 C16 C17 -0.7(16) . . . . ? C15 C16 C17 C12 0.0(14) . . . . ? C13 C12 C17 C16 1.1(12) . . . . ? C2 C12 C17 C16 -179.7(8) . . . . ? C36 N5 C24 C25 -121.0(7) . . . . ? Yb1 N5 C24 C25 74.9(9) . . . . ? C36 N5 C24 C29 62.7(9) . . . . ? Yb1 N5 C24 C29 -101.4(8) . . . . ? C29 C24 C25 C26 -3.9(10) . . . . ? N5 C24 C25 C26 179.7(6) . . . . ? C29 C24 C25 C30 177.7(7) . . . . ? N5 C24 C25 C30 1.3(10) . . . . ? C24 C25 C26 C27 1.9(11) . . . . ? C30 C25 C26 C27 -179.7(7) . . . . ? C25 C26 C27 C28 0.8(13) . . . . ? C26 C27 C28 C29 -1.4(13) . . . . ? C27 C28 C29 C24 -0.6(12) . . . . ? C27 C28 C29 C33 176.5(8) . . . . ? C25 C24 C29 C28 3.3(11) . . . . ? N5 C24 C29 C28 179.6(7) . . . . ? C25 C24 C29 C33 -173.6(7) . . . . ? N5 C24 C29 C33 2.6(11) . . . . ? C26 C25 C30 C32 51.0(10) . . . . ? C24 C25 C30 C32 -130.6(8) . . . . ? C26 C25 C30 C31 -72.9(10) . . . . ? C24 C25 C30 C31 105.4(10) . . . . ? C28 C29 C33 C35 -72.9(9) . . . . ? C24 C29 C33 C35 104.0(8) . . . . ? C28 C29 C33 C34 53.0(9) . . . . ? C24 C29 C33 C34 -130.1(8) . . . . ? Yb1 N6 C36 N5 5.5(6) . . . . ? Yb1 N6 C36 C37 -179.2(6) . . . . ? C24 N5 C36 N6 -175.9(6) . . . . ? Yb1 N5 C36 N6 -5.5(6) . . . . ? C24 N5 C36 C37 8.9(10) . . . . ? Yb1 N5 C36 C37 179.3(6) . . . . ? C24 N5 C36 Yb1 -170.4(7) . . . . ? N4 Yb1 C36 N6 131.6(4) . . . . ? N2 Yb1 C36 N6 -134.7(4) . . . . ? N5 Yb1 C36 N6 174.0(7) . . . . ? N3 Yb1 C36 N6 78.4(5) . . . . ? N1 Yb1 C36 N6 -81.7(5) . . . . ? N7 Yb1 C36 N6 -4.7(6) . . . . ? C1 Yb1 C36 N6 -104.1(5) . . . . ? C2 Yb1 C36 N6 100.4(5) . . . . ? N4 Yb1 C36 N5 -42.5(5) . . . . ? N2 Yb1 C36 N5 51.3(5) . . . . ? N6 Yb1 C36 N5 -174.0(7) . . . . ? N3 Yb1 C36 N5 -95.7(4) . . . . ? N1 Yb1 C36 N5 104.2(4) . . . . ? N7 Yb1 C36 N5 -178.7(4) . . . . ? C1 Yb1 C36 N5 81.9(4) . . . . ? C2 Yb1 C36 N5 -73.6(4) . . . . ? N4 Yb1 C36 C37 165(27) . . . . ? N2 Yb1 C36 C37 -101(27) . . . . ? N6 Yb1 C36 C37 33(27) . . . . ? N5 Yb1 C36 C37 -153(27) . . . . ? N3 Yb1 C36 C37 112(27) . . . . ? N1 Yb1 C36 C37 -48(27) . . . . ? N7 Yb1 C36 C37 29(27) . . . . ? C1 Yb1 C36 C37 -71(27) . . . . ? C2 Yb1 C36 C37 134(27) . . . . ? N6 C36 C37 C42 -126.7(8) . . . . ? N5 C36 C37 C42 48.1(10) . . . . ? Yb1 C36 C37 C42 -160(26) . . . . ? N6 C36 C37 C38 50.6(10) . . . . ? N5 C36 C37 C38 -134.6(7) . . . . ? Yb1 C36 C37 C38 18(27) . . . . ? C43 O1 C38 C39 2.4(11) . . . . ? C43 O1 C38 C37 -178.3(7) . . . . ? C42 C37 C38 O1 -178.7(7) . . . . ? C36 C37 C38 O1 4.0(10) . . . . ? C42 C37 C38 C39 0.6(11) . . . . ? C36 C37 C38 C39 -176.7(7) . . . . ? O1 C38 C39 C40 179.6(8) . . . . ? C37 C38 C39 C40 0.4(12) . . . . ? C38 C39 C40 C41 -0.8(14) . . . . ? C39 C40 C41 C42 0.2(14) . . . . ? C40 C41 C42 C37 0.8(13) . . . . ? C38 C37 C42 C41 -1.2(12) . . . . ? C36 C37 C42 C41 176.1(7) . . . . ? Yb1 N7 C44 C45 -51(11) . . . . ? N7 C44 C45 C46 172(8) . . . . ? N7 C44 C45 C50 -7(9) . . . . ? C50 C45 C46 C47 -0.9(16) . . . . ? C44 C45 C46 C47 179.2(9) . . . . ? C50 C45 C46 O2 -179.3(9) . . . . ? C44 C45 C46 O2 0.8(14) . . . . ? C51 O2 C46 C47 0.3(14) . . . . ? C51 O2 C46 C45 178.8(8) . . . . ? C45 C46 C47 C48 0.2(15) . . . . ? O2 C46 C47 C48 178.5(9) . . . . ? C46 C47 C48 C49 -0.6(15) . . . . ? C47 C48 C49 C50 1.6(15) . . . . ? C48 C49 C50 C45 -2.3(15) . . . . ? C46 C45 C50 C49 2.0(16) . . . . ? C44 C45 C50 C49 -178.1(9) . . . . ? C55 C52 C53 C57 -159(9) 3_577 . . 3_577 ? C54 C52 C53 C57 -7(14) 3_577 . . 3_577 ? C56 C52 C53 C57 -160(11) 3_577 . . 3_577 ? C57 C52 C53 C57 10(11) . . . 3_577 ? C58 C52 C53 C57 -169(9) . . . 3_577 ? C53 C52 C53 C57 8(9) 3_577 . . 3_577 ? C52 C52 C53 C57 8(9) 3_577 . . 3_577 ? C55 C52 C53 C56 1(4) 3_577 . . 3_577 ? C54 C52 C53 C56 153(7) 3_577 . . 3_577 ? C57 C52 C53 C56 170(3) . . . 3_577 ? C58 C52 C53 C56 -9(4) . . . 3_577 ? C53 C52 C53 C56 168(4) 3_577 . . 3_577 ? C57 C52 C53 C56 160(11) 3_577 . . 3_577 ? C52 C52 C53 C56 168(4) 3_577 . . 3_577 ? C55 C52 C53 C54 -172(3) 3_577 . . . ? C54 C52 C53 C54 -19(9) 3_577 . . . ? C56 C52 C53 C54 -172(5) 3_577 . . . ? C57 C52 C53 C54 -2(4) . . . . ? C58 C52 C53 C54 179(2) . . . . ? C53 C52 C53 C54 -4(2) 3_577 . . . ? C57 C52 C53 C54 -12(7) 3_577 . . . ? C52 C52 C53 C54 -4(2) 3_577 . . . ? C55 C52 C53 C52 -167(3) 3_577 . . 3_577 ? C54 C52 C53 C52 -15(7) 3_577 . . 3_577 ? C56 C52 C53 C52 -168(4) 3_577 . . 3_577 ? C57 C52 C53 C52 2(3) . . . 3_577 ? C58 C52 C53 C52 -177(3) . . . 3_577 ? C53 C52 C53 C52 0.000(2) 3_577 . . 3_577 ? C57 C52 C53 C52 -8(9) 3_577 . . 3_577 ? C56 C53 C54 C57 4(19) 3_577 . . 3_577 ? C52 C53 C54 C57 126(25) . . . 3_577 ? C52 C53 C54 C57 119(23) 3_577 . . 3_577 ? C57 C53 C54 C52 -119(24) 3_577 . . 3_577 ? C56 C53 C54 C52 -115(25) 3_577 . . 3_577 ? C52 C53 C54 C52 6(3) . . . 3_577 ? C57 C53 C54 C55 -126(23) 3_577 . . . ? C56 C53 C54 C55 -122(25) 3_577 . . . ? C52 C53 C54 C55 0(4) . . . . ? C52 C53 C54 C55 -7(2) 3_577 . . . ? C57 C53 C54 C58 -118(23) 3_577 . . 3_577 ? C56 C53 C54 C58 -114(25) 3_577 . . 3_577 ? C52 C53 C54 C58 7(5) . . . 3_577 ? C52 C53 C54 C58 1(3) 3_577 . . 3_577 ? C57 C54 C55 C58 156(8) 3_577 . . 3_577 ? C52 C54 C55 C58 152(9) 3_577 . . 3_577 ? C53 C54 C55 C58 161(7) . . . 3_577 ? C57 C54 C55 C52 4(4) 3_577 . . 3_577 ? C53 C54 C55 C52 10(3) . . . 3_577 ? C58 C54 C55 C52 -152(9) 3_577 . . 3_577 ? C57 C54 C55 C56 -5(5) 3_577 . . . ? C52 C54 C55 C56 -8(2) 3_577 . . . ? C53 C54 C55 C56 1(4) . . . . ? C58 C54 C55 C56 -160(10) 3_577 . . . ? C58 C55 C56 C53 -151(9) 3_577 . . 3_577 ? C52 C55 C56 C53 -1(4) 3_577 . . 3_577 ? C54 C55 C56 C53 7(5) . . . 3_577 ? C58 C55 C56 C52 -150(11) 3_577 . . 3_577 ? C54 C55 C56 C52 7(2) . . . 3_577 ? C58 C55 C56 C57 -157(8) 3_577 . . . ? C52 C55 C56 C57 -7(3) 3_577 . . . ? C54 C55 C56 C57 1(4) . . . . ? C52 C55 C56 C58 150(11) 3_577 . . 3_577 ? C54 C55 C56 C58 158(11) . . . 3_577 ? C55 C52 C57 C53 159(8) 3_577 . . 3_577 ? C54 C52 C57 C53 163(9) 3_577 . . 3_577 ? C56 C52 C57 C53 8(11) 3_577 . . 3_577 ? C53 C52 C57 C53 -9(10) . . . 3_577 ? C58 C52 C57 C53 170(7) . . . 3_577 ? C57 C52 C57 C53 -7(7) 3_577 . . 3_577 ? C52 C52 C57 C53 -7(7) 3_577 . . 3_577 ? C55 C52 C57 C54 -4(4) 3_577 . . 3_577 ? C56 C52 C57 C54 -155(6) 3_577 . . 3_577 ? C53 C52 C57 C54 -172(3) . . . 3_577 ? C58 C52 C57 C54 7(3) . . . 3_577 ? C53 C52 C57 C54 -163(9) 3_577 . . 3_577 ? C57 C52 C57 C54 -170(3) 3_577 . . 3_577 ? C52 C52 C57 C54 -170(3) 3_577 . . 3_577 ? C55 C52 C57 C56 172(3) 3_577 . . . ? C54 C52 C57 C56 176(4) 3_577 . . . ? C56 C52 C57 C56 22(8) 3_577 . . . ? C53 C52 C57 C56 4(4) . . . . ? C58 C52 C57 C56 -177(2) . . . . ? C53 C52 C57 C56 13(7) 3_577 . . . ? C57 C52 C57 C56 6(2) 3_577 . . . ? C52 C52 C57 C56 6(2) 3_577 . . . ? C55 C52 C57 C52 166(4) 3_577 . . 3_577 ? C54 C52 C57 C52 170(3) 3_577 . . 3_577 ? C56 C52 C57 C52 15(5) 3_577 . . 3_577 ? C53 C52 C57 C52 -2(2) . . . 3_577 ? C58 C52 C57 C52 177(3) . . . 3_577 ? C53 C52 C57 C52 7(7) 3_577 . . 3_577 ? C57 C52 C57 C52 0.000(2) 3_577 . . 3_577 ? C52 C56 C57 C53 51(22) 3_577 . . 3_577 ? C55 C56 C57 C53 56(22) . . . 3_577 ? C58 C56 C57 C53 48(22) 3_577 . . 3_577 ? C53 C56 C57 C54 -7(35) 3_577 . . 3_577 ? C52 C56 C57 C54 44(41) 3_577 . . 3_577 ? C55 C56 C57 C54 48(42) . . . 3_577 ? C58 C56 C57 C54 41(42) 3_577 . . 3_577 ? C53 C56 C57 C52 -59(21) 3_577 . . . ? C52 C56 C57 C52 -8(3) 3_577 . . . ? C55 C56 C57 C52 -4(4) . . . . ? C58 C56 C57 C52 -11(4) 3_577 . . . ? C53 C56 C57 C52 -51(22) 3_577 . . 3_577 ? C55 C56 C57 C52 5(2) . . . 3_577 ? C58 C56 C57 C52 -3(2) 3_577 . . 3_577 ? C54 C52 C58 C55 -110(16) 3_577 . . 3_577 ? C56 C52 C58 C55 58(15) 3_577 . . 3_577 ? C57 C52 C58 C55 -115(15) . . . 3_577 ? C53 C52 C58 C55 64(16) . . . 3_577 ? C53 C52 C58 C55 -111(15) 3_577 . . 3_577 ? C57 C52 C58 C55 61(16) 3_577 . . 3_577 ? C52 C52 C58 C55 31(34) 3_577 . . 3_577 ? C55 C52 C58 C54 110(16) 3_577 . . 3_577 ? C56 C52 C58 C54 168(2) 3_577 . . 3_577 ? C57 C52 C58 C54 -5(2) . . . 3_577 ? C53 C52 C58 C54 174(3) . . . 3_577 ? C53 C52 C58 C54 -1(3) 3_577 . . 3_577 ? C57 C52 C58 C54 171(3) 3_577 . . 3_577 ? C52 C52 C58 C54 141(26) 3_577 . . 3_577 ? C55 C52 C58 C56 -58(15) 3_577 . . 3_577 ? C54 C52 C58 C56 -168(2) 3_577 . . 3_577 ? C57 C52 C58 C56 -173(3) . . . 3_577 ? C53 C52 C58 C56 6(2) . . . 3_577 ? C53 C52 C58 C56 -169(4) 3_577 . . 3_577 ? C57 C52 C58 C56 3(2) 3_577 . . 3_577 ? C52 C52 C58 C56 -27(25) 3_577 . . 3_577 ? C61 C59 C60 C63 -170(8) 3_776 . . 3_776 ? C62 C59 C60 C63 9(7) 3_776 . . 3_776 ? C64 C59 C60 C63 -178(6) . . . 3_776 ? C65 C59 C60 C63 -1(9) . . . 3_776 ? C60 C59 C60 C63 -175(8) 3_776 . . 3_776 ? C61 C59 C60 C64 -5(17) 3_776 . . 3_776 ? C62 C59 C60 C64 174(13) 3_776 . . 3_776 ? C64 C59 C60 C64 -13(15) . . . 3_776 ? C65 C59 C60 C64 164(11) . . . 3_776 ? C63 C59 C60 C64 165(18) 3_776 . . 3_776 ? C60 C59 C60 C64 -10(12) 3_776 . . 3_776 ? C61 C59 C60 C62 -179(10) 3_776 . . 3_776 ? C64 C59 C60 C62 173(6) . . . 3_776 ? C65 C59 C60 C62 -10(3) . . . 3_776 ? C63 C59 C60 C62 -9(7) 3_776 . . 3_776 ? C60 C59 C60 C62 176(5) 3_776 . . 3_776 ? C61 C59 C60 C61 9(10) 3_776 . . . ? C62 C59 C60 C61 -173(4) 3_776 . . . ? C64 C59 C60 C61 0(7) . . . . ? C65 C59 C60 C61 177(3) . . . . ? C63 C59 C60 C61 178(10) 3_776 . . . ? C60 C59 C60 C61 3(4) 3_776 . . . ? C62 C59 C60 C61 179(10) 3_776 . . 3_776 ? C64 C59 C60 C61 -9(5) . . . 3_776 ? C65 C59 C60 C61 168(10) . . . 3_776 ? C63 C59 C60 C61 170(8) 3_776 . . 3_776 ? C60 C59 C60 C61 -6(7) 3_776 . . 3_776 ? C61 C59 C60 C60 6(7) 3_776 . . 3_776 ? C62 C59 C60 C60 -176(5) 3_776 . . 3_776 ? C64 C59 C60 C60 -3(4) . . . 3_776 ? C65 C59 C60 C60 174(4) . . . 3_776 ? C63 C59 C60 C60 175(8) 3_776 . . 3_776 ? C61 C59 C60 C59 6(7) 3_776 . . 3_776 ? C62 C59 C60 C59 -176(5) 3_776 . . 3_776 ? C64 C59 C60 C59 -3(3) . . . 3_776 ? C65 C59 C60 C59 174(4) . . . 3_776 ? C63 C59 C60 C59 175(8) 3_776 . . 3_776 ? C60 C59 C60 C59 0.000(2) 3_776 . . 3_776 ? C63 C60 C61 C59 158(17) 3_776 . . 3_776 ? C64 C60 C61 C59 153(20) 3_776 . . 3_776 ? C62 C60 C61 C59 -32(25) 3_776 . . 3_776 ? C59 C60 C61 C59 -20(22) . . . 3_776 ? C61 C60 C61 C59 -16(18) 3_776 . . 3_776 ? C60 C60 C61 C59 -16(18) 3_776 . . 3_776 ? C63 C60 C61 C64 5(7) 3_776 . . 3_776 ? C62 C60 C61 C64 175(11) 3_776 . . 3_776 ? C59 C60 C61 C64 -173(5) . . . 3_776 ? C61 C60 C61 C64 -169(5) 3_776 . . 3_776 ? C60 C60 C61 C64 -169(5) 3_776 . . 3_776 ? C59 C60 C61 C64 -153(20) 3_776 . . 3_776 ? C63 C60 C61 C62 167(6) 3_776 . . . ? C64 C60 C61 C62 162(7) 3_776 . . . ? C62 C60 C61 C62 -24(14) 3_776 . . . ? C59 C60 C61 C62 -11(8) . . . . ? C61 C60 C61 C62 -8(4) 3_776 . . . ? C60 C60 C61 C62 -8(4) 3_776 . . . ? C59 C60 C61 C62 9(15) 3_776 . . . ? C63 C60 C61 C60 174(8) 3_776 . . 3_776 ? C64 C60 C61 C60 169(5) 3_776 . . 3_776 ? C62 C60 C61 C60 -16(9) 3_776 . . 3_776 ? C59 C60 C61 C60 -4(5) . . . 3_776 ? C61 C60 C61 C60 0.000(5) 3_776 . . 3_776 ? C59 C60 C61 C60 16(18) 3_776 . . 3_776 ? C64 C60 C61 C63 -5(7) 3_776 . . 3_776 ? C62 C60 C61 C63 170(17) 3_776 . . 3_776 ? C59 C60 C61 C63 -178(11) . . . 3_776 ? C61 C60 C61 C63 -174(8) 3_776 . . 3_776 ? C60 C60 C61 C63 -174(8) 3_776 . . 3_776 ? C59 C60 C61 C63 -158(17) 3_776 . . 3_776 ? C64 C61 C62 C59 -32(16) 3_776 . . 3_776 ? C60 C61 C62 C59 -168(23) . . . 3_776 ? C60 C61 C62 C59 -177(21) 3_776 . . 3_776 ? C63 C61 C62 C59 -156(23) 3_776 . . 3_776 ? C59 C61 C62 C65 -13(19) 3_776 . . 3_776 ? C64 C61 C62 C65 -45(11) 3_776 . . 3_776 ? C60 C61 C62 C65 179(5) . . . 3_776 ? C60 C61 C62 C65 170(3) 3_776 . . 3_776 ? C63 C61 C62 C65 -169(6) 3_776 . . 3_776 ? C59 C61 C62 C60 177(21) 3_776 . . 3_776 ? C64 C61 C62 C60 145(12) 3_776 . . 3_776 ? C60 C61 C62 C60 9(6) . . . 3_776 ? C63 C61 C62 C60 21(6) 3_776 . . 3_776 ? C59 C61 C62 C63 -177(20) 3_776 . . . ? C64 C61 C62 C63 151(11) 3_776 . . . ? C60 C61 C62 C63 15(5) . . . . ? C60 C61 C62 C63 6(3) 3_776 . . . ? C63 C61 C62 C63 27(7) 3_776 . . . ? C59 C62 C63 C60 -9(7) 3_776 . . 3_776 ? C65 C62 C63 C60 -151(6) 3_776 . . 3_776 ? C61 C62 C63 C60 -8(5) . . . 3_776 ? C59 C62 C63 C64 -10(7) 3_776 . . . ? C65 C62 C63 C64 -152(5) 3_776 . . . ? C60 C62 C63 C64 -1(3) 3_776 . . . ? C61 C62 C63 C64 -9(4) . . . . ? C65 C62 C63 C59 -142(10) 3_776 . . 3_776 ? C60 C62 C63 C59 9(7) 3_776 . . 3_776 ? C61 C62 C63 C59 1(5) . . . 3_776 ? C59 C62 C63 C61 -11(5) 3_776 . . 3_776 ? C65 C62 C63 C61 -154(6) 3_776 . . 3_776 ? C60 C62 C63 C61 -2(4) 3_776 . . 3_776 ? C61 C62 C63 C61 -11(3) . . . 3_776 ? C62 C59 C64 C61 54(20) 3_776 . . 3_776 ? C60 C59 C64 C61 22(12) . . . 3_776 ? C65 C59 C64 C61 -154(17) . . . 3_776 ? C63 C59 C64 C61 21(12) 3_776 . . 3_776 ? C60 C59 C64 C61 18(14) 3_776 . . 3_776 ? C61 C59 C64 C60 -18(14) 3_776 . . 3_776 ? C62 C59 C64 C60 36(26) 3_776 . . 3_776 ? C60 C59 C64 C60 4(5) . . . 3_776 ? C65 C59 C64 C60 -172(5) . . . 3_776 ? C63 C59 C64 C60 3(5) 3_776 . . 3_776 ? C61 C59 C64 C63 -18(15) 3_776 . . . ? C62 C59 C64 C63 36(27) 3_776 . . . ? C60 C59 C64 C63 4(5) . . . . ? C65 C59 C64 C63 -173(4) . . . . ? C63 C59 C64 C63 3(7) 3_776 . . . ? C60 C59 C64 C63 -1(4) 3_776 . . . ? C60 C63 C64 C61 -5(7) 3_776 . . 3_776 ? C62 C63 C64 C61 -4(7) . . . 3_776 ? C59 C63 C64 C61 -8(5) 3_776 . . 3_776 ? C62 C63 C64 C60 1(4) . . . 3_776 ? C59 C63 C64 C60 -3(4) 3_776 . . 3_776 ? C61 C63 C64 C60 5(7) 3_776 . . 3_776 ? C60 C63 C64 C59 1(6) 3_776 . . . ? C62 C63 C64 C59 2(6) . . . . ? C59 C63 C64 C59 -2(5) 3_776 . . . ? C61 C63 C64 C59 6(5) 3_776 . . . ? C61 C59 C65 C62 165(21) 3_776 . . 3_776 ? C60 C59 C65 C62 11(3) . . . 3_776 ? C64 C59 C65 C62 -173(8) . . . 3_776 ? C63 C59 C65 C62 11(3) 3_776 . . 3_776 ? C60 C59 C65 C62 157(22) 3_776 . . 3_776 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.719 _refine_diff_density_min -0.946 _refine_diff_density_rms 0.097 # Attachment '- shelxl 7.cif' data_shelxl7 _database_code_depnum_ccdc_archive 'CCDC 862449' #TrackingRef '- shelxl 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H84 N10 O2 Si4 Yb2, 2(C7 H8)' _chemical_formula_sum 'C74 H100 N10 O2 Si4 Yb2' _chemical_formula_weight 1620.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1228(6) _cell_length_b 12.7576(7) _cell_length_c 13.5956(6) _cell_angle_alpha 80.150(5) _cell_angle_beta 68.709(4) _cell_angle_gamma 84.206(5) _cell_volume 1928.55(17) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8055 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 826 _exptl_absorpt_coefficient_mu 2.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.425 _exptl_absorpt_correction_T_max 0.638 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16590 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0766 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.49 _reflns_number_total 7150 _reflns_number_gt 6227 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.3688P] 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 7150 _refine_ls_number_parameters 404 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.127 _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 Yb1 Yb 0.56835(2) 0.90005(2) 0.57314(2) 0.03115(10) Uani 1 1 d . . . Si1 Si 0.4569(2) 0.66363(16) 0.80052(16) 0.0547(6) Uani 1 1 d . . . Si2 Si 0.68890(16) 0.67338(14) 0.39702(14) 0.0396(4) Uani 1 1 d . . . O1 O 0.3609(4) 0.9765(3) 0.6706(3) 0.0396(10) Uani 1 1 d . . . N1 N 0.5178(5) 0.7858(4) 0.7386(4) 0.0395(13) Uani 1 1 d . . . N2 N 0.6041(4) 0.9409(4) 0.7190(4) 0.0344(12) Uani 1 1 d . . . N3 N 0.6940(4) 0.7791(4) 0.4605(4) 0.0359(12) Uani 1 1 d . . . N4 N 0.7685(4) 0.8952(4) 0.5233(4) 0.0367(12) Uani 1 1 d . . . N5 N 0.4277(4) 0.9110(4) 0.4891(4) 0.0313(11) Uani 1 1 d . . . H5 H 0.4538 0.8726 0.4327 0.038 Uiso 1 1 calc R . . C1 C 0.5743(6) 0.8475(5) 0.7749(5) 0.0364(14) Uani 1 1 d . . . C2 C 0.7897(5) 0.8139(4) 0.4700(5) 0.0334(14) Uani 1 1 d . . . C3 C 0.7027(6) 0.9939(5) 0.7242(5) 0.0437(16) Uani 1 1 d . . . H3A H 0.6919 0.9939 0.7992 0.052 Uiso 1 1 calc R . . H3B H 0.7014 1.0682 0.6907 0.052 Uiso 1 1 calc R . . C4 C 0.8232(6) 0.9413(5) 0.6692(5) 0.0484(18) Uani 1 1 d . . . H4A H 0.8838 0.9769 0.6817 0.058 Uiso 1 1 calc R . . H4B H 0.8236 0.8670 0.7029 0.058 Uiso 1 1 calc R . . C5 C 0.8577(6) 0.9430(5) 0.5498(5) 0.0444(16) Uani 1 1 d . . . H5A H 0.8677 1.0168 0.5142 0.053 Uiso 1 1 calc R . . H5B H 0.9340 0.9040 0.5228 0.053 Uiso 1 1 calc R . . C6 C 0.5968(6) 0.8121(5) 0.8789(5) 0.0427(16) Uani 1 1 d . . . C7 C 0.5261(7) 0.8586(6) 0.9686(5) 0.0553(19) Uani 1 1 d . . . H7 H 0.4688 0.9124 0.9632 0.066 Uiso 1 1 calc R . . C8 C 0.5411(9) 0.8248(7) 1.0644(6) 0.075(3) Uani 1 1 d . . . H8 H 0.4939 0.8559 1.1248 0.090 Uiso 1 1 calc R . . C9 C 0.6248(9) 0.7458(8) 1.0729(7) 0.079(3) Uani 1 1 d . . . H9 H 0.6340 0.7229 1.1391 0.095 Uiso 1 1 calc R . . C10 C 0.6944(8) 0.7008(7) 0.9852(7) 0.071(2) Uani 1 1 d . . . H10 H 0.7518 0.6472 0.9911 0.085 Uiso 1 1 calc R . . C11 C 0.6807(7) 0.7339(6) 0.8880(6) 0.0556(19) Uani 1 1 d . . . H11 H 0.7288 0.7029 0.8278 0.067 Uiso 1 1 calc R . . C12 C 0.9120(5) 0.7637(5) 0.4291(5) 0.0406(15) Uani 1 1 d . . . C13 C 0.9449(7) 0.6738(5) 0.4829(7) 0.060(2) Uani 1 1 d . . . H13 H 0.8896 0.6409 0.5465 0.072 Uiso 1 1 calc R . . C14 C 1.0573(9) 0.6307(7) 0.4458(10) 0.094(3) Uani 1 1 d . . . H14 H 1.0793 0.5697 0.4853 0.113 Uiso 1 1 calc R . . C15 C 1.1386(8) 0.6751(9) 0.3518(11) 0.103(4) Uani 1 1 d . . . H15 H 1.2151 0.6432 0.3262 0.123 Uiso 1 1 calc R . . C16 C 1.1089(8) 0.7661(9) 0.2946(9) 0.090(3) Uani 1 1 d . . . H16 H 1.1641 0.7974 0.2302 0.108 Uiso 1 1 calc R . . C17 C 0.9945(7) 0.8107(6) 0.3352(6) 0.062(2) Uani 1 1 d . . . H17 H 0.9729 0.8737 0.2982 0.074 Uiso 1 1 calc R . . C18 C 0.3563(11) 0.6668(9) 0.9403(7) 0.122(5) Uani 1 1 d . . . H18A H 0.4022 0.6747 0.9838 0.183 Uiso 1 1 calc R . . H18B H 0.3146 0.6010 0.9673 0.183 Uiso 1 1 calc R . . H18C H 0.2995 0.7265 0.9429 0.183 Uiso 1 1 calc R . . C19 C 0.5711(10) 0.5521(6) 0.7989(9) 0.107(4) Uani 1 1 d . . . H19A H 0.6340 0.5588 0.7296 0.161 Uiso 1 1 calc R . . H19B H 0.5344 0.4844 0.8127 0.161 Uiso 1 1 calc R . . H19C H 0.6038 0.5556 0.8536 0.161 Uiso 1 1 calc R . . C20 C 0.3717(7) 0.6301(6) 0.7219(5) 0.0537(19) Uani 1 1 d . . . H20A H 0.3108 0.6853 0.7208 0.081 Uiso 1 1 calc R . . H20B H 0.3350 0.5625 0.7543 0.081 Uiso 1 1 calc R . . H20C H 0.4247 0.6249 0.6495 0.081 Uiso 1 1 calc R . . C21 C 0.8064(7) 0.6727(6) 0.2625(6) 0.065(2) Uani 1 1 d . . . H21A H 0.8102 0.7434 0.2217 0.098 Uiso 1 1 calc R . . H21B H 0.7877 0.6223 0.2255 0.098 Uiso 1 1 calc R . . H21C H 0.8823 0.6521 0.2705 0.098 Uiso 1 1 calc R . . C22 C 0.5413(6) 0.6843(5) 0.3791(5) 0.0475(17) Uani 1 1 d . . . H22A H 0.4784 0.6886 0.4474 0.071 Uiso 1 1 calc R . . H22B H 0.5320 0.6221 0.3511 0.071 Uiso 1 1 calc R . . H22C H 0.5373 0.7478 0.3297 0.071 Uiso 1 1 calc R . . C23 C 0.6962(8) 0.5422(5) 0.4783(7) 0.067(2) Uani 1 1 d . . . H23A H 0.7729 0.5312 0.4865 0.101 Uiso 1 1 calc R . . H23B H 0.6851 0.4864 0.4429 0.101 Uiso 1 1 calc R . . H23C H 0.6343 0.5405 0.5480 0.101 Uiso 1 1 calc R . . C24 C 0.3176(5) 0.8765(5) 0.5629(5) 0.0360(14) Uani 1 1 d . . . C25 C 0.2781(5) 0.9140(5) 0.6610(5) 0.0378(15) Uani 1 1 d . . . C26 C 0.1697(6) 0.8921(6) 0.7370(6) 0.0514(18) Uani 1 1 d . . . H26 H 0.1444 0.9208 0.8013 0.062 Uiso 1 1 calc R . . C27 C 0.0969(6) 0.8259(6) 0.7173(7) 0.067(2) Uani 1 1 d . . . H27 H 0.0223 0.8090 0.7689 0.080 Uiso 1 1 calc R . . C28 C 0.1348(7) 0.7859(6) 0.6229(6) 0.057(2) Uani 1 1 d . . . H28 H 0.0863 0.7405 0.6105 0.068 Uiso 1 1 calc R . . C29 C 0.2418(6) 0.8110(5) 0.5463(5) 0.0431(16) Uani 1 1 d . . . H29 H 0.2651 0.7839 0.4813 0.052 Uiso 1 1 calc R . . C30 C 0.3275(6) 1.0205(6) 0.7677(5) 0.0505(18) Uani 1 1 d . . . H30A H 0.2567 1.0661 0.7759 0.076 Uiso 1 1 calc R . . H30B H 0.3914 1.0619 0.7657 0.076 Uiso 1 1 calc R . . H30C H 0.3119 0.9634 0.8275 0.076 Uiso 1 1 calc R . . C31 C 1.0594(16) 1.0055(15) 0.0160(16) 0.089(2) Uiso 0.50 1 d PD . . C32 C 0.996(2) 1.0856(18) -0.023(2) 0.089(2) Uiso 0.50 1 d PD . . C33 C 0.9028(17) 1.0556(15) -0.0487(16) 0.089(2) Uiso 0.50 1 d PD . . C34 C 0.8661(19) 0.9501(14) -0.0362(17) 0.089(2) Uiso 0.50 1 d PD . . C35 C 0.9320(17) 0.8786(15) 0.0031(15) 0.089(2) Uiso 0.50 1 d PD . . C36 C 1.027(2) 0.8976(17) 0.033(3) 0.089(2) Uiso 0.50 1 d PD . . C37 C 1.1591(17) 1.0008(16) 0.0596(17) 0.089(2) Uiso 0.50 1 d PD . . C38 C 0.967(2) 0.5192(19) 0.8870(17) 0.112(3) Uiso 0.50 1 d PD . . C39 C 0.929(2) 0.4228(18) 0.9413(18) 0.112(3) Uiso 0.50 1 d PD . . C40 C 0.930(2) 0.3989(19) 1.0457(18) 0.112(3) Uiso 0.50 1 d PD . . C41 C 0.982(3) 0.452(2) 1.100(2) 0.112(3) Uiso 0.50 1 d PD . . C42 C 1.031(2) 0.5439(19) 1.0354(19) 0.112(3) Uiso 0.50 1 d PD . . C43 C 1.032(3) 0.569(2) 0.930(2) 0.112(3) Uiso 0.50 1 d PD . . C44 C 0.972(2) 0.5499(18) 0.7759(16) 0.112(3) Uiso 0.50 1 d PD . . 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 Yb1 0.02935(17) 0.03599(17) 0.03310(16) -0.00750(11) -0.01626(12) 0.00037(11) Si1 0.0783(16) 0.0470(12) 0.0460(12) 0.0041(9) -0.0312(11) -0.0179(11) Si2 0.0393(11) 0.0389(10) 0.0459(11) -0.0143(8) -0.0187(9) 0.0025(8) O1 0.035(3) 0.046(3) 0.038(2) -0.0147(19) -0.011(2) 0.001(2) N1 0.048(3) 0.041(3) 0.036(3) -0.008(2) -0.021(3) -0.005(2) N2 0.042(3) 0.030(3) 0.041(3) -0.009(2) -0.025(3) -0.002(2) N3 0.030(3) 0.042(3) 0.039(3) -0.008(2) -0.015(2) 0.000(2) N4 0.024(3) 0.038(3) 0.055(3) -0.015(2) -0.021(3) 0.005(2) N5 0.025(3) 0.042(3) 0.029(3) -0.013(2) -0.010(2) -0.001(2) C1 0.043(4) 0.032(3) 0.038(4) -0.008(3) -0.020(3) 0.008(3) C2 0.032(4) 0.030(3) 0.036(3) 0.000(3) -0.012(3) 0.001(3) C3 0.041(4) 0.047(4) 0.052(4) -0.009(3) -0.025(3) -0.004(3) C4 0.054(5) 0.045(4) 0.065(5) -0.006(3) -0.042(4) -0.007(3) C5 0.036(4) 0.043(4) 0.066(5) -0.014(3) -0.030(4) 0.003(3) C6 0.052(4) 0.045(4) 0.037(4) -0.002(3) -0.023(3) -0.007(3) C7 0.068(5) 0.065(5) 0.042(4) -0.018(4) -0.028(4) 0.002(4) C8 0.099(7) 0.093(7) 0.044(5) -0.018(4) -0.034(5) -0.005(6) C9 0.101(8) 0.100(7) 0.048(5) 0.004(5) -0.046(5) -0.007(6) C10 0.089(7) 0.069(5) 0.065(6) 0.004(4) -0.047(5) 0.006(5) C11 0.071(5) 0.060(5) 0.051(4) -0.007(4) -0.042(4) 0.011(4) C12 0.030(4) 0.044(4) 0.052(4) -0.017(3) -0.016(3) 0.003(3) C13 0.045(5) 0.043(4) 0.096(6) -0.007(4) -0.034(5) 0.004(3) C14 0.060(7) 0.066(6) 0.169(11) -0.028(6) -0.058(7) 0.020(5) C15 0.038(6) 0.086(8) 0.193(13) -0.072(8) -0.039(7) 0.036(5) C16 0.038(5) 0.111(8) 0.116(8) -0.051(7) -0.005(5) 0.001(5) C17 0.043(5) 0.071(5) 0.069(5) -0.009(4) -0.015(4) -0.006(4) C18 0.170(12) 0.136(10) 0.050(6) 0.000(6) -0.010(6) -0.094(9) C19 0.152(10) 0.048(5) 0.171(11) -0.001(6) -0.125(9) 0.004(6) C20 0.066(5) 0.051(4) 0.052(4) -0.007(3) -0.029(4) -0.008(4) C21 0.055(5) 0.071(5) 0.068(5) -0.030(4) -0.012(4) -0.004(4) C22 0.048(4) 0.054(4) 0.049(4) -0.023(3) -0.020(3) -0.002(3) C23 0.080(6) 0.042(4) 0.098(6) -0.010(4) -0.054(5) 0.002(4) C24 0.027(3) 0.035(3) 0.049(4) 0.000(3) -0.020(3) -0.001(3) C25 0.028(4) 0.044(4) 0.041(4) -0.004(3) -0.012(3) -0.004(3) C26 0.033(4) 0.067(5) 0.045(4) 0.004(3) -0.009(3) -0.002(3) C27 0.024(4) 0.081(6) 0.084(6) 0.010(5) -0.012(4) -0.015(4) C28 0.054(5) 0.059(5) 0.066(5) 0.006(4) -0.036(4) -0.018(4) C29 0.041(4) 0.048(4) 0.047(4) -0.003(3) -0.022(3) -0.013(3) C30 0.050(4) 0.059(4) 0.040(4) -0.023(3) -0.007(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N4 2.267(5) . ? Yb1 N2 2.327(4) . ? Yb1 N5 2.354(4) . ? Yb1 N1 2.370(5) . ? Yb1 N3 2.384(5) . ? Yb1 N5 2.414(5) 2_676 ? Yb1 O1 2.561(4) . ? Yb1 C1 2.735(6) . ? Yb1 C2 2.752(6) . ? Yb1 C24 3.139(6) . ? Yb1 Yb1 3.6068(5) 2_676 ? Si1 N1 1.736(5) . ? Si1 C18 1.852(9) . ? Si1 C20 1.854(6) . ? Si1 C19 1.879(9) . ? Si2 N3 1.738(5) . ? Si2 C23 1.854(7) . ? Si2 C21 1.866(7) . ? Si2 C22 1.880(7) . ? O1 C25 1.397(7) . ? O1 C30 1.429(7) . ? N1 C1 1.349(7) . ? N2 C1 1.305(7) . ? N2 C3 1.460(7) . ? N3 C2 1.338(7) . ? N4 C2 1.317(7) . ? N4 C5 1.472(7) . ? N5 C24 1.407(7) . ? N5 Yb1 2.414(5) 2_676 ? N5 H5 0.9200 . ? C1 C6 1.521(8) . ? C2 C12 1.500(9) . ? C3 C4 1.524(9) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.519(9) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C11 1.373(9) . ? C6 C7 1.400(9) . ? C7 C8 1.371(10) . ? C7 H7 0.9400 . ? C8 C9 1.377(12) . ? C8 H8 0.9400 . ? C9 C10 1.367(12) . ? C9 H9 0.9400 . ? C10 C11 1.382(9) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C13 1.358(9) . ? C12 C17 1.385(9) . ? C13 C14 1.363(12) . ? C13 H13 0.9400 . ? C14 C15 1.370(14) . ? C14 H14 0.9400 . ? C15 C16 1.375(14) . ? C15 H15 0.9400 . ? C16 C17 1.395(11) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.395(8) . ? C24 C29 1.402(8) . ? C25 C26 1.365(9) . ? C26 C27 1.400(10) . ? C26 H26 0.9400 . ? C27 C28 1.367(11) . ? C27 H27 0.9400 . ? C28 C29 1.363(9) . ? C28 H28 0.9400 . ? C29 H29 0.9400 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 C33 0.99(2) 2_775 ? C31 C34 1.24(2) 2_775 ? C31 C32 1.363(16) . ? C31 C32 1.38(3) 2_775 ? C31 C36 1.429(16) . ? C31 C35 1.46(2) 2_775 ? C31 C37 1.520(16) . ? C31 C31 1.67(3) 2_775 ? C31 C36 1.74(3) 2_775 ? C32 C36 0.39(3) 2_775 ? C32 C35 1.15(2) 2_775 ? C32 C31 1.38(3) 2_775 ? C32 C33 1.407(16) . ? C33 C31 0.99(2) 2_775 ? C33 C37 1.15(2) 2_775 ? C33 C36 1.19(2) 2_775 ? C33 C34 1.423(16) . ? C34 C37 0.74(2) 2_775 ? C34 C31 1.24(2) 2_775 ? C34 C35 1.323(16) . ? C35 C32 1.15(2) 2_775 ? C35 C36 1.404(16) . ? C35 C31 1.46(2) 2_775 ? C36 C32 0.39(3) 2_775 ? C36 C33 1.19(2) 2_775 ? C36 C31 1.74(3) 2_775 ? C37 C34 0.74(2) 2_775 ? C37 C33 1.15(2) 2_775 ? C38 C41 0.83(3) 2_767 ? C38 C42 1.22(3) 2_767 ? C38 C39 1.352(17) . ? C38 C43 1.389(17) . ? C38 C44 1.472(17) . ? C39 C42 0.85(3) 2_767 ? C39 C40 1.405(17) . ? C39 C41 1.90(3) 2_767 ? C39 C43 2.00(3) 2_767 ? C40 C43 0.83(2) 2_767 ? C40 C42 1.18(3) 2_767 ? C40 C41 1.418(17) . ? C41 C43 0.60(3) 2_767 ? C41 C38 0.83(3) 2_767 ? C41 C42 1.379(17) . ? C41 C42 1.90(3) 2_767 ? C41 C39 1.90(3) 2_767 ? C41 C44 1.95(3) 2_767 ? C42 C39 0.85(3) 2_767 ? C42 C40 1.18(3) 2_767 ? C42 C38 1.22(3) 2_767 ? C42 C43 1.416(17) . ? C42 C43 1.62(4) 2_767 ? C42 C41 1.90(3) 2_767 ? C42 C42 1.96(4) 2_767 ? C43 C41 0.60(3) 2_767 ? C43 C40 0.83(2) 2_767 ? C43 C42 1.62(4) 2_767 ? C43 C39 2.00(3) 2_767 ? C44 C41 1.95(3) 2_767 ? 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 Yb1 N2 75.08(18) . . ? N4 Yb1 N5 137.18(17) . . ? N2 Yb1 N5 144.83(17) . . ? N4 Yb1 N1 100.69(18) . . ? N2 Yb1 N1 57.57(16) . . ? N5 Yb1 N1 114.18(16) . . ? N4 Yb1 N3 57.38(16) . . ? N2 Yb1 N3 122.37(17) . . ? N5 Yb1 N3 91.97(16) . . ? N1 Yb1 N3 98.99(17) . . ? N4 Yb1 N5 88.94(16) . 2_676 ? N2 Yb1 N5 86.43(15) . 2_676 ? N5 Yb1 N5 81.71(15) . 2_676 ? N1 Yb1 N5 137.78(16) . 2_676 ? N3 Yb1 N5 120.17(16) . 2_676 ? N4 Yb1 O1 152.46(15) . . ? N2 Yb1 O1 82.28(15) . . ? N5 Yb1 O1 62.65(14) . . ? N1 Yb1 O1 79.51(16) . . ? N3 Yb1 O1 150.14(14) . . ? N5 Yb1 O1 74.00(14) 2_676 . ? N4 Yb1 C1 84.09(18) . . ? N2 Yb1 C1 28.44(16) . . ? N5 Yb1 C1 137.73(17) . . ? N1 Yb1 C1 29.56(16) . . ? N3 Yb1 C1 110.10(17) . . ? N5 Yb1 C1 113.80(16) 2_676 . ? O1 Yb1 C1 83.34(16) . . ? N4 Yb1 C2 28.36(16) . . ? N2 Yb1 C2 97.93(17) . . ? N5 Yb1 C2 117.19(16) . . ? N1 Yb1 C2 99.65(18) . . ? N3 Yb1 C2 29.10(15) . . ? N5 Yb1 C2 107.13(16) 2_676 . ? O1 Yb1 C2 178.86(14) . . ? C1 Yb1 C2 96.30(18) . . ? N4 Yb1 C24 159.22(17) . . ? N2 Yb1 C24 125.56(17) . . ? N5 Yb1 C24 24.79(15) . . ? N1 Yb1 C24 90.60(16) . . ? N3 Yb1 C24 103.89(16) . . ? N5 Yb1 C24 94.36(15) 2_676 . ? O1 Yb1 C24 46.65(15) . . ? C1 Yb1 C24 112.97(17) . . ? C2 Yb1 C24 132.74(17) . . ? N4 Yb1 Yb1 117.81(13) . 2_676 ? N2 Yb1 Yb1 119.47(12) . 2_676 ? N5 Yb1 Yb1 41.47(11) . 2_676 ? N1 Yb1 Yb1 139.73(13) . 2_676 ? N3 Yb1 Yb1 111.03(11) . 2_676 ? N5 Yb1 Yb1 40.24(10) 2_676 2_676 ? O1 Yb1 Yb1 61.03(9) . 2_676 ? C1 Yb1 Yb1 138.86(13) . 2_676 ? C2 Yb1 Yb1 119.69(12) . 2_676 ? C24 Yb1 Yb1 57.20(10) . 2_676 ? N1 Si1 C18 112.7(4) . . ? N1 Si1 C20 106.6(3) . . ? C18 Si1 C20 109.1(4) . . ? N1 Si1 C19 113.4(4) . . ? C18 Si1 C19 108.5(6) . . ? C20 Si1 C19 106.3(4) . . ? N3 Si2 C23 112.5(3) . . ? N3 Si2 C21 114.1(3) . . ? C23 Si2 C21 108.3(4) . . ? N3 Si2 C22 107.4(3) . . ? C23 Si2 C22 106.4(3) . . ? C21 Si2 C22 107.7(3) . . ? C25 O1 C30 116.6(5) . . ? C25 O1 Yb1 108.1(3) . . ? C30 O1 Yb1 124.6(4) . . ? C1 N1 Si1 127.5(4) . . ? C1 N1 Yb1 90.4(3) . . ? Si1 N1 Yb1 141.6(2) . . ? C1 N2 C3 120.2(5) . . ? C1 N2 Yb1 93.5(3) . . ? C3 N2 Yb1 130.6(4) . . ? C2 N3 Si2 127.1(4) . . ? C2 N3 Yb1 90.9(4) . . ? Si2 N3 Yb1 141.6(3) . . ? C2 N4 C5 124.7(5) . . ? C2 N4 Yb1 96.8(3) . . ? C5 N4 Yb1 137.6(4) . . ? C24 N5 Yb1 110.6(3) . . ? C24 N5 Yb1 114.3(4) . 2_676 ? Yb1 N5 Yb1 98.29(15) . 2_676 ? C24 N5 H5 111.0 . . ? Yb1 N5 H5 111.0 . . ? Yb1 N5 H5 111.0 2_676 . ? N2 C1 N1 116.8(5) . . ? N2 C1 C6 121.6(5) . . ? N1 C1 C6 121.5(5) . . ? N2 C1 Yb1 58.1(3) . . ? N1 C1 Yb1 60.0(3) . . ? C6 C1 Yb1 171.3(5) . . ? N4 C2 N3 114.7(5) . . ? N4 C2 C12 120.8(5) . . ? N3 C2 C12 124.4(5) . . ? N4 C2 Yb1 54.9(3) . . ? N3 C2 Yb1 60.0(3) . . ? C12 C2 Yb1 171.8(4) . . ? N2 C3 C4 113.2(5) . . ? N2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 115.4(5) . . ? C5 C4 H4A 108.4 . . ? C3 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? C3 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? N4 C5 C4 112.1(5) . . ? N4 C5 H5A 109.2 . . ? C4 C5 H5A 109.2 . . ? N4 C5 H5B 109.2 . . ? C4 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C11 C6 C7 119.6(6) . . ? C11 C6 C1 122.2(6) . . ? C7 C6 C1 118.2(6) . . ? C8 C7 C6 119.4(8) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 120.6(8) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 120.1(7) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.2(8) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C6 C11 C10 120.2(7) . . ? C6 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C13 C12 C17 118.9(7) . . ? C13 C12 C2 121.5(6) . . ? C17 C12 C2 119.7(6) . . ? C12 C13 C14 120.7(8) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 120.9(9) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C16 120.3(9) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 118.0(9) . . ? C15 C16 H16 121.0 . . ? C17 C16 H16 121.0 . . ? C12 C17 C16 121.2(8) . . ? C12 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 116.8(6) . . ? C25 C24 N5 116.8(5) . . ? C29 C24 N5 126.4(6) . . ? C25 C24 Yb1 83.0(3) . . ? C29 C24 Yb1 147.0(4) . . ? N5 C24 Yb1 44.6(2) . . ? C26 C25 C24 122.7(6) . . ? C26 C25 O1 125.0(6) . . ? C24 C25 O1 112.3(5) . . ? C25 C26 C27 118.6(7) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? C28 C27 C26 119.8(7) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 121.0(7) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C28 C29 C24 121.1(6) . . ? C28 C29 H29 119.5 . . ? C24 C29 H29 119.5 . . ? O1 C30 H30A 109.5 . . ? O1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C34 78.4(15) 2_775 2_775 ? C33 C31 C32 174(2) 2_775 . ? C34 C31 C32 105.8(15) 2_775 . ? C33 C31 C32 70.9(17) 2_775 2_775 ? C34 C31 C32 149(2) 2_775 2_775 ? C32 C31 C32 104.7(18) . 2_775 ? C33 C31 C36 55.4(13) 2_775 . ? C34 C31 C36 133.7(16) 2_775 . ? C32 C31 C36 120.3(16) . . ? C32 C31 C36 15.6(14) 2_775 . ? C33 C31 C35 136.0(18) 2_775 2_775 ? C34 C31 C35 57.8(10) 2_775 2_775 ? C32 C31 C35 47.9(10) . 2_775 ? C32 C31 C35 152(2) 2_775 2_775 ? C36 C31 C35 167.8(16) . 2_775 ? C33 C31 C37 49.4(13) 2_775 . ? C34 C31 C37 29.0(10) 2_775 . ? C32 C31 C37 134.7(16) . . ? C32 C31 C37 120(2) 2_775 . ? C36 C31 C37 104.7(14) . . ? C35 C31 C37 86.8(13) 2_775 . ? C33 C31 C31 123(2) 2_775 2_775 ? C34 C31 C31 158(2) 2_775 2_775 ? C32 C31 C31 52.7(14) . 2_775 ? C32 C31 C31 52.0(10) 2_775 2_775 ? C36 C31 C31 67.6(15) . 2_775 ? C35 C31 C31 100.5(17) 2_775 2_775 ? C37 C31 C31 171(2) . 2_775 ? C33 C31 C36 171(2) 2_775 2_775 ? C34 C31 C36 108.9(17) 2_775 2_775 ? C32 C31 C36 3.2(12) . 2_775 ? C32 C31 C36 101.5(15) 2_775 2_775 ? C36 C31 C36 117.1(14) . 2_775 ? C35 C31 C36 51.1(11) 2_775 2_775 ? C37 C31 C36 137.8(17) . 2_775 ? C31 C31 C36 49.5(9) 2_775 2_775 ? C36 C32 C35 124(6) 2_775 2_775 ? C36 C32 C31 165(6) 2_775 . ? C35 C32 C31 70.6(15) 2_775 . ? C36 C32 C31 90(5) 2_775 2_775 ? C35 C32 C31 146(3) 2_775 2_775 ? C31 C32 C31 75.3(18) . 2_775 ? C36 C32 C33 49(4) 2_775 . ? C35 C32 C33 172(3) 2_775 . ? C31 C32 C33 116.7(19) . . ? C31 C32 C33 41.5(11) 2_775 . ? C31 C33 C37 90.2(17) 2_775 2_775 ? C31 C33 C36 81.5(17) 2_775 2_775 ? C37 C33 C36 172(2) 2_775 2_775 ? C31 C33 C32 67.6(18) 2_775 . ? C37 C33 C32 158(2) 2_775 . ? C36 C33 C32 14.1(17) 2_775 . ? C31 C33 C34 58.9(15) 2_775 . ? C37 C33 C34 31.3(11) 2_775 . ? C36 C33 C34 140(2) 2_775 . ? C32 C33 C34 126(2) . . ? C37 C34 C31 97(2) 2_775 2_775 ? C37 C34 C35 166(3) 2_775 . ? C31 C34 C35 69.5(16) 2_775 . ? C37 C34 C33 53.9(18) 2_775 . ? C31 C34 C33 42.8(11) 2_775 . ? C35 C34 C33 112.2(19) . . ? C32 C35 C34 114(2) 2_775 . ? C32 C35 C36 13.2(18) 2_775 . ? C34 C35 C36 127(2) . . ? C32 C35 C31 61.4(13) 2_775 2_775 ? C34 C35 C31 52.7(13) . 2_775 ? C36 C35 C31 74.6(15) . 2_775 ? C32 C36 C33 117(5) 2_775 2_775 ? C32 C36 C35 43(4) 2_775 . ? C33 C36 C35 160(2) 2_775 . ? C32 C36 C31 74(5) 2_775 . ? C33 C36 C31 43.1(12) 2_775 . ? C35 C36 C31 117.1(17) . . ? C32 C36 C31 12(5) 2_775 2_775 ? C33 C36 C31 105.8(18) 2_775 2_775 ? C35 C36 C31 54.3(11) . 2_775 ? C31 C36 C31 62.9(14) . 2_775 ? C34 C37 C33 95(2) 2_775 2_775 ? C34 C37 C31 54.4(19) 2_775 . ? C33 C37 C31 40.5(12) 2_775 . ? C41 C38 C42 82(2) 2_767 2_767 ? C41 C38 C39 119(3) 2_767 . ? C42 C38 C39 38.0(14) 2_767 . ? C41 C38 C43 12(3) 2_767 . ? C42 C38 C43 76.3(19) 2_767 . ? C39 C38 C43 114(2) . . ? C41 C38 C44 113(3) 2_767 . ? C42 C38 C44 154(3) 2_767 . ? C39 C38 C44 121(2) . . ? C43 C38 C44 122(2) . . ? C42 C39 C38 62(2) 2_767 . ? C42 C39 C40 57(2) 2_767 . ? C38 C39 C40 117(2) . . ? C42 C39 C41 40.8(17) 2_767 2_767 ? C38 C39 C41 22.4(13) . 2_767 ? C40 C39 C41 97.0(16) . 2_767 ? C42 C39 C43 36.8(17) 2_767 2_767 ? C38 C39 C43 97.6(16) . 2_767 ? C40 C39 C43 19.9(12) . 2_767 ? C41 C39 C43 77.2(12) 2_767 2_767 ? C43 C40 C42 88(3) 2_767 2_767 ? C43 C40 C39 125(3) 2_767 . ? C42 C40 C39 36.9(14) 2_767 . ? C43 C40 C41 7(3) 2_767 . ? C42 C40 C41 94(2) 2_767 . ? C39 C40 C41 130(2) . . ? C43 C41 C38 150(7) 2_767 2_767 ? C43 C41 C42 102(4) 2_767 . ? C38 C41 C42 61(2) 2_767 . ? C43 C41 C40 10(4) 2_767 . ? C38 C41 C40 160(4) 2_767 . ? C42 C41 C40 109(2) . . ? C43 C41 C42 31(4) 2_767 2_767 ? C38 C41 C42 127(3) 2_767 2_767 ? C42 C41 C42 71.3(19) . 2_767 ? C40 C41 C42 38.2(11) . 2_767 ? C43 C41 C39 125(5) 2_767 2_767 ? C38 C41 C39 38(2) 2_767 2_767 ? C42 C41 C39 23.6(11) . 2_767 ? C40 C41 C39 132.6(19) . 2_767 ? C42 C41 C39 94.5(18) 2_767 2_767 ? C43 C41 C44 153(5) 2_767 2_767 ? C38 C41 C44 44(2) 2_767 2_767 ? C42 C41 C44 102.7(19) . 2_767 ? C40 C41 C44 148(2) . 2_767 ? C42 C41 C44 169(2) 2_767 2_767 ? C39 C41 C44 79.1(15) 2_767 2_767 ? C39 C42 C40 86(2) 2_767 2_767 ? C39 C42 C38 80(2) 2_767 2_767 ? C40 C42 C38 157(3) 2_767 2_767 ? C39 C42 C41 116(3) 2_767 . ? C40 C42 C41 156(2) 2_767 . ? C38 C42 C41 36.7(13) 2_767 . ? C39 C42 C43 122(3) 2_767 . ? C40 C42 C43 35.9(12) 2_767 . ? C38 C42 C43 152(2) 2_767 . ? C41 C42 C43 121(2) . . ? C39 C42 C43 136(3) 2_767 2_767 ? C40 C42 C43 135(2) 2_767 2_767 ? C38 C42 C43 56.6(15) 2_767 2_767 ? C41 C42 C43 21.4(13) . 2_767 ? C43 C42 C43 100(2) . 2_767 ? C39 C42 C41 134(3) 2_767 2_767 ? C40 C42 C41 48.2(14) 2_767 2_767 ? C38 C42 C41 141(2) 2_767 2_767 ? C41 C42 C41 108.7(19) . 2_767 ? C43 C42 C41 12.6(13) . 2_767 ? C43 C42 C41 87.3(15) 2_767 2_767 ? C39 C42 C42 169(4) 2_767 2_767 ? C40 C42 C42 89.8(19) 2_767 2_767 ? C38 C42 C42 101(2) 2_767 2_767 ? C41 C42 C42 66.8(16) . 2_767 ? C43 C42 C42 54.5(16) . 2_767 ? C43 C42 C42 45.4(10) 2_767 2_767 ? C41 C42 C42 41.9(8) 2_767 2_767 ? C41 C43 C40 163(7) 2_767 2_767 ? C41 C43 C38 17(4) 2_767 . ? C40 C43 C38 177(4) 2_767 . ? C41 C43 C42 137(5) 2_767 . ? C40 C43 C42 56(2) 2_767 . ? C38 C43 C42 125(2) . . ? C41 C43 C42 56(4) 2_767 2_767 ? C40 C43 C42 135(4) 2_767 2_767 ? C38 C43 C42 47.1(13) . 2_767 ? C42 C43 C42 80(2) . 2_767 ? C41 C43 C39 156(5) 2_767 2_767 ? C40 C43 C39 35(2) 2_767 2_767 ? C38 C43 C39 146(2) . 2_767 ? C42 C43 C39 21.0(11) . 2_767 ? C42 C43 C39 101(2) 2_767 2_767 ? C38 C44 C41 23.2(12) . 2_767 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Yb1 O1 C25 -175.1(4) . . . . ? N2 Yb1 O1 C25 -140.3(4) . . . . ? N5 Yb1 O1 C25 42.4(3) . . . . ? N1 Yb1 O1 C25 -82.0(3) . . . . ? N3 Yb1 O1 C25 7.8(5) . . . . ? N5 Yb1 O1 C25 131.2(4) 2_676 . . . ? C1 Yb1 O1 C25 -111.7(4) . . . . ? C2 Yb1 O1 C25 -40(8) . . . . ? C24 Yb1 O1 C25 18.9(3) . . . . ? Yb1 Yb1 O1 C25 89.7(3) 2_676 . . . ? N4 Yb1 O1 C30 -32.2(6) . . . . ? N2 Yb1 O1 C30 2.5(5) . . . . ? N5 Yb1 O1 C30 -174.8(5) . . . . ? N1 Yb1 O1 C30 60.8(5) . . . . ? N3 Yb1 O1 C30 150.6(4) . . . . ? N5 Yb1 O1 C30 -85.9(5) 2_676 . . . ? C1 Yb1 O1 C30 31.2(5) . . . . ? C2 Yb1 O1 C30 103(7) . . . . ? C24 Yb1 O1 C30 161.8(5) . . . . ? Yb1 Yb1 O1 C30 -127.4(5) 2_676 . . . ? C18 Si1 N1 C1 51.4(7) . . . . ? C20 Si1 N1 C1 171.1(6) . . . . ? C19 Si1 N1 C1 -72.4(7) . . . . ? C18 Si1 N1 Yb1 -140.1(6) . . . . ? C20 Si1 N1 Yb1 -20.4(6) . . . . ? C19 Si1 N1 Yb1 96.1(6) . . . . ? N4 Yb1 N1 C1 56.9(4) . . . . ? N2 Yb1 N1 C1 -7.6(3) . . . . ? N5 Yb1 N1 C1 -148.5(3) . . . . ? N3 Yb1 N1 C1 115.2(4) . . . . ? N5 Yb1 N1 C1 -43.4(5) 2_676 . . . ? O1 Yb1 N1 C1 -95.0(4) . . . . ? C2 Yb1 N1 C1 85.8(4) . . . . ? C24 Yb1 N1 C1 -140.6(4) . . . . ? Yb1 Yb1 N1 C1 -106.3(3) 2_676 . . . ? N4 Yb1 N1 Si1 -113.9(5) . . . . ? N2 Yb1 N1 Si1 -178.4(6) . . . . ? N5 Yb1 N1 Si1 40.6(5) . . . . ? N3 Yb1 N1 Si1 -55.6(5) . . . . ? N5 Yb1 N1 Si1 145.7(4) 2_676 . . . ? O1 Yb1 N1 Si1 94.1(5) . . . . ? C1 Yb1 N1 Si1 -170.9(7) . . . . ? C2 Yb1 N1 Si1 -85.1(5) . . . . ? C24 Yb1 N1 Si1 48.5(5) . . . . ? Yb1 Yb1 N1 Si1 82.8(5) 2_676 . . . ? N4 Yb1 N2 C1 -105.6(4) . . . . ? N5 Yb1 N2 C1 94.4(4) . . . . ? N1 Yb1 N2 C1 7.8(3) . . . . ? N3 Yb1 N2 C1 -71.6(4) . . . . ? N5 Yb1 N2 C1 164.6(4) 2_676 . . . ? O1 Yb1 N2 C1 90.3(4) . . . . ? C2 Yb1 N2 C1 -88.6(4) . . . . ? C24 Yb1 N2 C1 71.8(4) . . . . ? Yb1 Yb1 N2 C1 140.6(3) 2_676 . . . ? N4 Yb1 N2 C3 30.1(5) . . . . ? N5 Yb1 N2 C3 -129.9(5) . . . . ? N1 Yb1 N2 C3 143.5(6) . . . . ? N3 Yb1 N2 C3 64.0(5) . . . . ? N5 Yb1 N2 C3 -59.8(5) 2_676 . . . ? O1 Yb1 N2 C3 -134.1(5) . . . . ? C1 Yb1 N2 C3 135.6(7) . . . . ? C2 Yb1 N2 C3 47.0(5) . . . . ? C24 Yb1 N2 C3 -152.6(5) . . . . ? Yb1 Yb1 N2 C3 -83.8(5) 2_676 . . . ? C23 Si2 N3 C2 77.4(6) . . . . ? C21 Si2 N3 C2 -46.6(6) . . . . ? C22 Si2 N3 C2 -165.8(5) . . . . ? C23 Si2 N3 Yb1 -93.0(5) . . . . ? C21 Si2 N3 Yb1 143.0(4) . . . . ? C22 Si2 N3 Yb1 23.7(5) . . . . ? N4 Yb1 N3 C2 3.3(3) . . . . ? N2 Yb1 N3 C2 -36.6(4) . . . . ? N5 Yb1 N3 C2 151.4(3) . . . . ? N1 Yb1 N3 C2 -93.7(3) . . . . ? N5 Yb1 N3 C2 69.9(4) 2_676 . . . ? O1 Yb1 N3 C2 -178.3(3) . . . . ? C1 Yb1 N3 C2 -65.3(4) . . . . ? C24 Yb1 N3 C2 173.4(3) . . . . ? Yb1 Yb1 N3 C2 113.6(3) 2_676 . . . ? N4 Yb1 N3 Si2 175.7(5) . . . . ? N2 Yb1 N3 Si2 135.8(4) . . . . ? N5 Yb1 N3 Si2 -36.2(4) . . . . ? N1 Yb1 N3 Si2 78.7(4) . . . . ? N5 Yb1 N3 Si2 -117.8(4) 2_676 . . . ? O1 Yb1 N3 Si2 -5.9(6) . . . . ? C1 Yb1 N3 Si2 107.0(4) . . . . ? C2 Yb1 N3 Si2 172.4(7) . . . . ? C24 Yb1 N3 Si2 -14.2(4) . . . . ? Yb1 Yb1 N3 Si2 -74.0(4) 2_676 . . . ? N2 Yb1 N4 C2 142.6(4) . . . . ? N5 Yb1 N4 C2 -54.3(4) . . . . ? N1 Yb1 N4 C2 90.5(4) . . . . ? N3 Yb1 N4 C2 -3.4(3) . . . . ? N5 Yb1 N4 C2 -130.9(4) 2_676 . . . ? O1 Yb1 N4 C2 178.3(3) . . . . ? C1 Yb1 N4 C2 115.1(4) . . . . ? C24 Yb1 N4 C2 -31.3(7) . . . . ? Yb1 Yb1 N4 C2 -101.6(3) 2_676 . . . ? N2 Yb1 N4 C5 -25.8(6) . . . . ? N5 Yb1 N4 C5 137.4(5) . . . . ? N1 Yb1 N4 C5 -77.8(6) . . . . ? N3 Yb1 N4 C5 -171.7(6) . . . . ? N5 Yb1 N4 C5 60.8(6) 2_676 . . . ? O1 Yb1 N4 C5 9.9(8) . . . . ? C1 Yb1 N4 C5 -53.3(6) . . . . ? C2 Yb1 N4 C5 -168.4(8) . . . . ? C24 Yb1 N4 C5 160.3(5) . . . . ? Yb1 Yb1 N4 C5 90.0(6) 2_676 . . . ? N4 Yb1 N5 C24 160.7(3) . . . . ? N2 Yb1 N5 C24 -48.3(5) . . . . ? N1 Yb1 N5 C24 19.1(4) . . . . ? N3 Yb1 N5 C24 119.9(4) . . . . ? N5 Yb1 N5 C24 -119.9(4) 2_676 . . . ? O1 Yb1 N5 C24 -43.7(4) . . . . ? C1 Yb1 N5 C24 -3.4(5) . . . . ? C2 Yb1 N5 C24 135.0(4) . . . . ? Yb1 Yb1 N5 C24 -119.9(4) 2_676 . . . ? N4 Yb1 N5 Yb1 -79.4(3) . . . 2_676 ? N2 Yb1 N5 Yb1 71.6(3) . . . 2_676 ? N1 Yb1 N5 Yb1 139.02(16) . . . 2_676 ? N3 Yb1 N5 Yb1 -120.21(17) . . . 2_676 ? N5 Yb1 N5 Yb1 0.0 2_676 . . 2_676 ? O1 Yb1 N5 Yb1 76.22(16) . . . 2_676 ? C1 Yb1 N5 Yb1 116.5(2) . . . 2_676 ? C2 Yb1 N5 Yb1 -105.05(18) . . . 2_676 ? C24 Yb1 N5 Yb1 119.9(4) . . . 2_676 ? C3 N2 C1 N1 -155.2(5) . . . . ? Yb1 N2 C1 N1 -13.1(6) . . . . ? C3 N2 C1 C6 27.6(9) . . . . ? Yb1 N2 C1 C6 169.7(5) . . . . ? C3 N2 C1 Yb1 -142.1(6) . . . . ? Si1 N1 C1 N2 -174.3(5) . . . . ? Yb1 N1 C1 N2 12.8(6) . . . . ? Si1 N1 C1 C6 2.9(9) . . . . ? Yb1 N1 C1 C6 -170.0(5) . . . . ? Si1 N1 C1 Yb1 172.9(6) . . . . ? N4 Yb1 C1 N2 69.4(4) . . . . ? N5 Yb1 C1 N2 -121.4(4) . . . . ? N1 Yb1 C1 N2 -166.5(6) . . . . ? N3 Yb1 C1 N2 121.4(4) . . . . ? N5 Yb1 C1 N2 -16.9(4) 2_676 . . . ? O1 Yb1 C1 N2 -86.1(4) . . . . ? C2 Yb1 C1 N2 95.0(4) . . . . ? C24 Yb1 C1 N2 -122.9(4) . . . . ? Yb1 Yb1 C1 N2 -57.1(4) 2_676 . . . ? N4 Yb1 C1 N1 -124.1(4) . . . . ? N2 Yb1 C1 N1 166.5(6) . . . . ? N5 Yb1 C1 N1 45.1(4) . . . . ? N3 Yb1 C1 N1 -72.1(4) . . . . ? N5 Yb1 C1 N1 149.7(3) 2_676 . . . ? O1 Yb1 C1 N1 80.5(4) . . . . ? C2 Yb1 C1 N1 -98.5(4) . . . . ? C24 Yb1 C1 N1 43.6(4) . . . . ? Yb1 Yb1 C1 N1 109.4(3) 2_676 . . . ? N4 Yb1 C1 C6 -22(3) . . . . ? N2 Yb1 C1 C6 -91(3) . . . . ? N5 Yb1 C1 C6 148(3) . . . . ? N1 Yb1 C1 C6 102(3) . . . . ? N3 Yb1 C1 C6 30(3) . . . . ? N5 Yb1 C1 C6 -108(3) 2_676 . . . ? O1 Yb1 C1 C6 -177(3) . . . . ? C2 Yb1 C1 C6 4(3) . . . . ? C24 Yb1 C1 C6 146(3) . . . . ? Yb1 Yb1 C1 C6 -148(3) 2_676 . . . ? C5 N4 C2 N3 176.0(5) . . . . ? Yb1 N4 C2 N3 5.6(5) . . . . ? C5 N4 C2 C12 -1.3(9) . . . . ? Yb1 N4 C2 C12 -171.7(5) . . . . ? C5 N4 C2 Yb1 170.5(7) . . . . ? Si2 N3 C2 N4 -179.3(4) . . . . ? Yb1 N3 C2 N4 -5.2(5) . . . . ? Si2 N3 C2 C12 -2.1(8) . . . . ? Yb1 N3 C2 C12 171.9(5) . . . . ? Si2 N3 C2 Yb1 -174.1(5) . . . . ? N2 Yb1 C2 N4 -36.4(4) . . . . ? N5 Yb1 C2 N4 141.7(3) . . . . ? N1 Yb1 C2 N4 -94.7(4) . . . . ? N3 Yb1 C2 N4 174.2(6) . . . . ? N5 Yb1 C2 N4 52.3(4) 2_676 . . . ? O1 Yb1 C2 N4 -137(7) . . . . ? C1 Yb1 C2 N4 -65.0(4) . . . . ? C24 Yb1 C2 N4 165.5(3) . . . . ? Yb1 Yb1 C2 N4 94.3(3) 2_676 . . . ? N4 Yb1 C2 N3 -174.2(6) . . . . ? N2 Yb1 C2 N3 149.5(3) . . . . ? N5 Yb1 C2 N3 -32.5(4) . . . . ? N1 Yb1 C2 N3 91.2(3) . . . . ? N5 Yb1 C2 N3 -121.9(3) 2_676 . . . ? O1 Yb1 C2 N3 49(8) . . . . ? C1 Yb1 C2 N3 120.8(3) . . . . ? C24 Yb1 C2 N3 -8.7(4) . . . . ? Yb1 Yb1 C2 N3 -79.9(3) 2_676 . . . ? N4 Yb1 C2 C12 61(3) . . . . ? N2 Yb1 C2 C12 24(3) . . . . ? N5 Yb1 C2 C12 -158(3) . . . . ? N1 Yb1 C2 C12 -34(3) . . . . ? N3 Yb1 C2 C12 -125(3) . . . . ? N5 Yb1 C2 C12 113(3) 2_676 . . . ? O1 Yb1 C2 C12 -76(8) . . . . ? C1 Yb1 C2 C12 -4(3) . . . . ? C24 Yb1 C2 C12 -134(3) . . . . ? Yb1 Yb1 C2 C12 155(3) 2_676 . . . ? C1 N2 C3 C4 71.1(7) . . . . ? Yb1 N2 C3 C4 -55.0(7) . . . . ? N2 C3 C4 C5 63.4(7) . . . . ? C2 N4 C5 C4 -122.2(6) . . . . ? Yb1 N4 C5 C4 43.7(8) . . . . ? C3 C4 C5 N4 -55.6(7) . . . . ? N2 C1 C6 C11 -109.7(7) . . . . ? N1 C1 C6 C11 73.2(9) . . . . ? Yb1 C1 C6 C11 -24(3) . . . . ? N2 C1 C6 C7 72.7(8) . . . . ? N1 C1 C6 C7 -104.4(7) . . . . ? Yb1 C1 C6 C7 158(2) . . . . ? C11 C6 C7 C8 -0.4(11) . . . . ? C1 C6 C7 C8 177.3(7) . . . . ? C6 C7 C8 C9 -0.1(12) . . . . ? C7 C8 C9 C10 0.5(14) . . . . ? C8 C9 C10 C11 -0.4(14) . . . . ? C7 C6 C11 C10 0.5(11) . . . . ? C1 C6 C11 C10 -177.0(6) . . . . ? C9 C10 C11 C6 -0.1(12) . . . . ? N4 C2 C12 C13 98.2(7) . . . . ? N3 C2 C12 C13 -78.8(8) . . . . ? Yb1 C2 C12 C13 42(3) . . . . ? N4 C2 C12 C17 -80.7(8) . . . . ? N3 C2 C12 C17 102.3(7) . . . . ? Yb1 C2 C12 C17 -137(3) . . . . ? C17 C12 C13 C14 0.4(11) . . . . ? C2 C12 C13 C14 -178.5(7) . . . . ? C12 C13 C14 C15 -2.0(14) . . . . ? C13 C14 C15 C16 1.9(16) . . . . ? C14 C15 C16 C17 -0.2(15) . . . . ? C13 C12 C17 C16 1.3(11) . . . . ? C2 C12 C17 C16 -179.8(7) . . . . ? C15 C16 C17 C12 -1.4(13) . . . . ? Yb1 N5 C24 C25 45.0(6) . . . . ? Yb1 N5 C24 C25 -64.8(6) 2_676 . . . ? Yb1 N5 C24 C29 -137.4(5) . . . . ? Yb1 N5 C24 C29 112.8(6) 2_676 . . . ? Yb1 N5 C24 Yb1 -109.8(4) 2_676 . . . ? N4 Yb1 C24 C25 -179.8(4) . . . . ? N2 Yb1 C24 C25 7.5(4) . . . . ? N5 Yb1 C24 C25 -140.6(6) . . . . ? N1 Yb1 C24 C25 56.8(4) . . . . ? N3 Yb1 C24 C25 156.2(4) . . . . ? N5 Yb1 C24 C25 -81.2(4) 2_676 . . . ? O1 Yb1 C24 C25 -18.1(3) . . . . ? C1 Yb1 C24 C25 36.9(4) . . . . ? C2 Yb1 C24 C25 160.6(3) . . . . ? Yb1 Yb1 C24 C25 -97.5(4) 2_676 . . . ? N4 Yb1 C24 C29 50.2(10) . . . . ? N2 Yb1 C24 C29 -122.5(8) . . . . ? N5 Yb1 C24 C29 89.4(9) . . . . ? N1 Yb1 C24 C29 -73.2(8) . . . . ? N3 Yb1 C24 C29 26.2(8) . . . . ? N5 Yb1 C24 C29 148.8(8) 2_676 . . . ? O1 Yb1 C24 C29 -148.1(9) . . . . ? C1 Yb1 C24 C29 -93.1(8) . . . . ? C2 Yb1 C24 C29 30.6(9) . . . . ? Yb1 Yb1 C24 C29 132.5(8) 2_676 . . . ? N4 Yb1 C24 N5 -39.2(7) . . . . ? N2 Yb1 C24 N5 148.1(4) . . . . ? N1 Yb1 C24 N5 -162.6(4) . . . . ? N3 Yb1 C24 N5 -63.2(4) . . . . ? N5 Yb1 C24 N5 59.3(4) 2_676 . . . ? O1 Yb1 C24 N5 122.5(4) . . . . ? C1 Yb1 C24 N5 177.5(4) . . . . ? C2 Yb1 C24 N5 -58.9(4) . . . . ? Yb1 Yb1 C24 N5 43.1(3) 2_676 . . . ? C29 C24 C25 C26 -2.1(9) . . . . ? N5 C24 C25 C26 175.8(6) . . . . ? Yb1 C24 C25 C26 -154.2(6) . . . . ? C29 C24 C25 O1 178.7(5) . . . . ? N5 C24 C25 O1 -3.4(8) . . . . ? Yb1 C24 C25 O1 26.6(4) . . . . ? C30 O1 C25 C26 -0.4(9) . . . . ? Yb1 O1 C25 C26 145.9(6) . . . . ? C30 O1 C25 C24 178.8(5) . . . . ? Yb1 O1 C25 C24 -34.9(6) . . . . ? C24 C25 C26 C27 2.5(10) . . . . ? O1 C25 C26 C27 -178.5(6) . . . . ? C25 C26 C27 C28 -0.8(11) . . . . ? C26 C27 C28 C29 -1.2(12) . . . . ? C27 C28 C29 C24 1.5(11) . . . . ? C25 C24 C29 C28 0.1(9) . . . . ? N5 C24 C29 C28 -177.6(6) . . . . ? Yb1 C24 C29 C28 121.8(8) . . . . ? C41 C38 C39 C42 13(5) 2_767 . . 2_767 ? C43 C38 C39 C42 0(3) . . . 2_767 ? C44 C38 C39 C42 161(4) . . . 2_767 ? C41 C38 C39 C40 30(6) 2_767 . . . ? C42 C38 C39 C40 17(3) 2_767 . . . ? C43 C38 C39 C40 17(3) . . . . ? C44 C38 C39 C40 178(2) . . . . ? C42 C38 C39 C41 -13(5) 2_767 . . 2_767 ? C43 C38 C39 C41 -13(4) . . . 2_767 ? C44 C38 C39 C41 148(6) . . . 2_767 ? C41 C38 C39 C43 24(4) 2_767 . . 2_767 ? C42 C38 C39 C43 11(2) 2_767 . . 2_767 ? C43 C38 C39 C43 12(3) . . . 2_767 ? C44 C38 C39 C43 172(2) . . . 2_767 ? C42 C39 C40 C43 1(5) 2_767 . . 2_767 ? C38 C39 C40 C43 -17(6) . . . 2_767 ? C41 C39 C40 C43 -6(5) 2_767 . . 2_767 ? C38 C39 C40 C42 -18(3) . . . 2_767 ? C41 C39 C40 C42 -7(3) 2_767 . . 2_767 ? C43 C39 C40 C42 -1(5) 2_767 . . 2_767 ? C42 C39 C40 C41 7(4) 2_767 . . . ? C38 C39 C40 C41 -11(4) . . . . ? C41 C39 C40 C41 0(4) 2_767 . . . ? C43 C39 C40 C41 6(4) 2_767 . . . ? C42 C40 C41 C43 -37(26) 2_767 . . 2_767 ? C39 C40 C41 C43 -41(26) . . . 2_767 ? C43 C40 C41 C38 -13(22) 2_767 . . 2_767 ? C42 C40 C41 C38 -50(11) 2_767 . . 2_767 ? C39 C40 C41 C38 -54(12) . . . 2_767 ? C43 C40 C41 C42 45(26) 2_767 . . . ? C42 C40 C41 C42 8(4) 2_767 . . . ? C39 C40 C41 C42 4(4) . . . . ? C43 C40 C41 C42 37(26) 2_767 . . 2_767 ? C39 C40 C41 C42 -4(2) . . . 2_767 ? C43 C40 C41 C39 41(26) 2_767 . . 2_767 ? C42 C40 C41 C39 4(4) 2_767 . . 2_767 ? C39 C40 C41 C39 0(5) . . . 2_767 ? C43 C40 C41 C44 -128(29) 2_767 . . 2_767 ? C42 C40 C41 C44 -165(4) 2_767 . . 2_767 ? C39 C40 C41 C44 -169(4) . . . 2_767 ? C43 C41 C42 C39 -166(6) 2_767 . . 2_767 ? C38 C41 C42 C39 -13(5) 2_767 . . 2_767 ? C40 C41 C42 C39 -173(3) . . . 2_767 ? C42 C41 C42 C39 -168(5) 2_767 . . 2_767 ? C44 C41 C42 C39 3(4) 2_767 . . 2_767 ? C43 C41 C42 C40 -13(10) 2_767 . . 2_767 ? C38 C41 C42 C40 141(7) 2_767 . . 2_767 ? C40 C41 C42 C40 -20(9) . . . 2_767 ? C42 C41 C42 C40 -14(6) 2_767 . . 2_767 ? C39 C41 C42 C40 154(10) 2_767 . . 2_767 ? C44 C41 C42 C40 156(6) 2_767 . . 2_767 ? C43 C41 C42 C38 -154(8) 2_767 . . 2_767 ? C40 C41 C42 C38 -161(5) . . . 2_767 ? C42 C41 C42 C38 -155(4) 2_767 . . 2_767 ? C39 C41 C42 C38 13(5) 2_767 . . 2_767 ? C44 C41 C42 C38 15(3) 2_767 . . 2_767 ? C43 C41 C42 C43 3(8) 2_767 . . . ? C38 C41 C42 C43 156(4) 2_767 . . . ? C40 C41 C42 C43 -4(4) . . . . ? C42 C41 C42 C43 1(3) 2_767 . . . ? C39 C41 C42 C43 169(6) 2_767 . . . ? C44 C41 C42 C43 172(2) 2_767 . . . ? C38 C41 C42 C43 154(8) 2_767 . . 2_767 ? C40 C41 C42 C43 -7(5) . . . 2_767 ? C42 C41 C42 C43 -2(6) 2_767 . . 2_767 ? C39 C41 C42 C43 166(6) 2_767 . . 2_767 ? C44 C41 C42 C43 169(7) 2_767 . . 2_767 ? C43 C41 C42 C41 2(6) 2_767 . . 2_767 ? C38 C41 C42 C41 155(4) 2_767 . . 2_767 ? C40 C41 C42 C41 -5(2) . . . 2_767 ? C42 C41 C42 C41 0.000(2) 2_767 . . 2_767 ? C39 C41 C42 C41 168(5) 2_767 . . 2_767 ? C44 C41 C42 C41 171(2) 2_767 . . 2_767 ? C43 C41 C42 C42 2(6) 2_767 . . 2_767 ? C38 C41 C42 C42 155(4) 2_767 . . 2_767 ? C40 C41 C42 C42 -5(2) . . . 2_767 ? C39 C41 C42 C42 168(5) 2_767 . . 2_767 ? C44 C41 C42 C42 171(2) 2_767 . . 2_767 ? C42 C38 C43 C41 117(15) 2_767 . . 2_767 ? C39 C38 C43 C41 116(15) . . . 2_767 ? C44 C38 C43 C41 -44(14) . . . 2_767 ? C41 C38 C43 C40 103(87) 2_767 . . 2_767 ? C42 C38 C43 C40 -140(86) 2_767 . . 2_767 ? C39 C38 C43 C40 -140(85) . . . 2_767 ? C44 C38 C43 C40 59(86) . . . 2_767 ? C41 C38 C43 C42 -136(16) 2_767 . . . ? C42 C38 C43 C42 -20(4) 2_767 . . . ? C39 C38 C43 C42 -20(4) . . . . ? C44 C38 C43 C42 180(3) . . . . ? C41 C38 C43 C42 -117(15) 2_767 . . 2_767 ? C39 C38 C43 C42 0(2) . . . 2_767 ? C44 C38 C43 C42 -161(3) . . . 2_767 ? C41 C38 C43 C39 -137(17) 2_767 . . 2_767 ? C42 C38 C43 C39 -21(4) 2_767 . . 2_767 ? C39 C38 C43 C39 -21(5) . . . 2_767 ? C44 C38 C43 C39 179(3) . . . 2_767 ? C39 C42 C43 C41 164(9) 2_767 . . 2_767 ? C40 C42 C43 C41 165(12) 2_767 . . 2_767 ? C38 C42 C43 C41 27(12) 2_767 . . 2_767 ? C41 C42 C43 C41 -4(12) . . . 2_767 ? C43 C42 C43 C41 -3(9) 2_767 . . 2_767 ? C42 C42 C43 C41 -3(9) 2_767 . . 2_767 ? C39 C42 C43 C40 -1(5) 2_767 . . 2_767 ? C38 C42 C43 C40 -138(6) 2_767 . . 2_767 ? C41 C42 C43 C40 -169(4) . . . 2_767 ? C43 C42 C43 C40 -168(5) 2_767 . . 2_767 ? C41 C42 C43 C40 -165(12) 2_767 . . 2_767 ? C42 C42 C43 C40 -168(5) 2_767 . . 2_767 ? C39 C42 C43 C38 -178(4) 2_767 . . . ? C40 C42 C43 C38 -177(6) 2_767 . . . ? C38 C42 C43 C38 44(7) 2_767 . . . ? C41 C42 C43 C38 13(5) . . . . ? C43 C42 C43 C38 14(3) 2_767 . . . ? C41 C42 C43 C38 17(8) 2_767 . . . ? C42 C42 C43 C38 14(3) 2_767 . . . ? C39 C42 C43 C42 167(5) 2_767 . . 2_767 ? C40 C42 C43 C42 168(5) 2_767 . . 2_767 ? C38 C42 C43 C42 30(5) 2_767 . . 2_767 ? C41 C42 C43 C42 -1(3) . . . 2_767 ? C43 C42 C43 C42 0.000(3) 2_767 . . 2_767 ? C41 C42 C43 C42 3(9) 2_767 . . 2_767 ? C40 C42 C43 C39 1(5) 2_767 . . 2_767 ? C38 C42 C43 C39 -137(8) 2_767 . . 2_767 ? C41 C42 C43 C39 -168(6) . . . 2_767 ? C43 C42 C43 C39 -167(5) 2_767 . . 2_767 ? C41 C42 C43 C39 -164(9) 2_767 . . 2_767 ? C42 C42 C43 C39 -167(5) 2_767 . . 2_767 ? C42 C38 C44 C41 -122(9) 2_767 . . 2_767 ? C39 C38 C44 C41 -150(6) . . . 2_767 ? C43 C38 C44 C41 9(4) . . . 2_767 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.171 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.123 data_shelxl1 _database_code_depnum_ccdc_archive 'CCDC 863200' #TrackingRef '- shelxl 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H62 N5 O2 Si2 Y' _chemical_formula_sum 'C39 H62 N5 O2 Si2 Y' _chemical_formula_weight 778.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.757(5) _cell_length_b 8.9687(16) _cell_length_c 19.765(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.382(3) _cell_angle_gamma 90.00 _cell_volume 4251.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 12776 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 1.465 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5163 _exptl_absorpt_correction_T_max 0.7784 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mo K\a' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26862 _diffrn_reflns_av_R_equivalents 0.0823 _diffrn_reflns_av_sigmaI/netI 0.0935 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7840 _reflns_number_gt 6310 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0284P)^2^+6.5499P] 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 7840 _refine_ls_number_parameters 464 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1083 _refine_ls_R_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.1554 _refine_ls_wR_factor_gt 0.1459 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.26170(2) 0.73951(5) 0.27794(3) 0.02936(14) Uani 1 1 d . . . Si1 Si 0.40614(7) 0.5645(2) 0.26519(10) 0.0502(5) Uani 1 1 d . . . Si2 Si 0.10246(6) 0.61525(18) 0.27345(9) 0.0396(4) Uani 1 1 d . . . O1 O 0.23684(16) 0.5485(4) 0.18851(18) 0.0379(9) Uani 1 1 d . . . O2 O 0.27157(16) 0.4816(4) 0.32196(19) 0.0425(10) Uani 1 1 d . . . N1 N 0.36142(18) 0.6940(5) 0.2869(2) 0.0362(11) Uani 1 1 d . . . N2 N 0.33445(18) 0.8925(5) 0.3408(2) 0.0399(11) Uani 1 1 d . . . N3 N 0.16712(18) 0.6964(5) 0.3033(2) 0.0364(11) Uani 1 1 d . . . N4 N 0.2379(2) 0.8097(6) 0.3804(3) 0.0573(16) Uani 1 1 d . . . N5 N 0.21657(18) 0.8970(5) 0.1953(2) 0.0383(11) Uani 1 1 d D . . H5 H 0.1830 0.8943 0.2013 0.046 Uiso 1 1 calc RD . . C1 C 0.3739(2) 0.7958(6) 0.3373(3) 0.0356(13) Uani 1 1 d . . . C2 C 0.1846(2) 0.7760(6) 0.3615(3) 0.0398(14) Uani 1 1 d . . . C3 C 0.3425(2) 1.0052(7) 0.3971(3) 0.0470(15) Uani 1 1 d D . . C4 C 0.2893(4) 1.0330(10) 0.4207(5) 0.053(3) Uani 0.65 1 d PD . . C4' C 0.3210(6) 0.947(2) 0.4572(7) 0.045(4) Uani 0.35 1 d PD . . C5 C 0.2597(3) 0.9051(10) 0.4414(4) 0.084(3) Uani 1 1 d D . . C6 C 0.4285(2) 0.7960(7) 0.3914(3) 0.0441(15) Uani 1 1 d . . . C7 C 0.4706(3) 0.8966(8) 0.3889(4) 0.0606(19) Uani 1 1 d . . . H7 H 0.4651 0.9692 0.3536 0.073 Uiso 1 1 calc R . . C8 C 0.5216(3) 0.8890(10) 0.4398(4) 0.073(2) Uani 1 1 d . . . H8 H 0.5510 0.9534 0.4374 0.088 Uiso 1 1 calc R . . C9 C 0.5281(3) 0.7862(10) 0.4930(5) 0.089(3) Uani 1 1 d . . . H9 H 0.5619 0.7822 0.5275 0.106 Uiso 1 1 calc R . . C10 C 0.4864(3) 0.6907(8) 0.4964(4) 0.086(3) Uani 1 1 d . . . H10 H 0.4913 0.6223 0.5335 0.103 Uiso 1 1 calc R . . C11 C 0.4370(3) 0.6934(7) 0.4460(4) 0.065(2) Uani 1 1 d . . . H11 H 0.4087 0.6254 0.4483 0.078 Uiso 1 1 calc R . . C12 C 0.1453(2) 0.8266(7) 0.4048(3) 0.0409(14) Uani 1 1 d . . . C13 C 0.1346(2) 0.7368(7) 0.4563(3) 0.0466(15) Uani 1 1 d . . . H13 H 0.1521 0.6434 0.4653 0.056 Uiso 1 1 calc R . . C14 C 0.0982(3) 0.7833(9) 0.4949(3) 0.062(2) Uani 1 1 d . . . H14 H 0.0906 0.7208 0.5297 0.075 Uiso 1 1 calc R . . C15 C 0.0731(3) 0.9199(10) 0.4828(4) 0.071(2) Uani 1 1 d . . . H15 H 0.0486 0.9511 0.5094 0.086 Uiso 1 1 calc R . . C16 C 0.0834(3) 1.0121(9) 0.4318(4) 0.067(2) Uani 1 1 d . . . H16 H 0.0659 1.1057 0.4233 0.081 Uiso 1 1 calc R . . C17 C 0.1202(3) 0.9649(7) 0.3930(3) 0.0543(17) Uani 1 1 d . . . H17 H 0.1280 1.0278 0.3586 0.065 Uiso 1 1 calc R . . C18 C 0.3788(3) 0.5178(8) 0.1706(3) 0.069(2) Uani 1 1 d . . . H18A H 0.3407 0.4827 0.1625 0.103 Uiso 1 1 calc R . . H18B H 0.4017 0.4403 0.1577 0.103 Uiso 1 1 calc R . . H18C H 0.3799 0.6060 0.1426 0.103 Uiso 1 1 calc R . . C19 C 0.4096(3) 0.3887(7) 0.3169(3) 0.070(2) Uani 1 1 d . . . H19A H 0.4270 0.4090 0.3656 0.104 Uiso 1 1 calc R . . H19B H 0.4314 0.3150 0.2993 0.104 Uiso 1 1 calc R . . H19C H 0.3721 0.3509 0.3124 0.104 Uiso 1 1 calc R . . C20 C 0.4798(3) 0.6279(10) 0.2763(5) 0.107(4) Uani 1 1 d . . . H20A H 0.4801 0.7214 0.2518 0.161 Uiso 1 1 calc R . . H20B H 0.5003 0.5533 0.2573 0.161 Uiso 1 1 calc R . . H20C H 0.4972 0.6419 0.3256 0.161 Uiso 1 1 calc R . . C21 C 0.0412(3) 0.7377(7) 0.2707(4) 0.0638(19) Uani 1 1 d . . . H21A H 0.0394 0.7616 0.3180 0.096 Uiso 1 1 calc R . . H21B H 0.0073 0.6864 0.2468 0.096 Uiso 1 1 calc R . . H21C H 0.0449 0.8290 0.2459 0.096 Uiso 1 1 calc R . . C22 C 0.0947(3) 0.4480(7) 0.3272(3) 0.0532(17) Uani 1 1 d . . . H22A H 0.1272 0.3846 0.3327 0.080 Uiso 1 1 calc R . . H22B H 0.0616 0.3928 0.3039 0.080 Uiso 1 1 calc R . . H22C H 0.0912 0.4802 0.3728 0.080 Uiso 1 1 calc R . . C23 C 0.0964(3) 0.5580(7) 0.1807(3) 0.0528(16) Uani 1 1 d . . . H23A H 0.1026 0.6440 0.1538 0.079 Uiso 1 1 calc R . . H23B H 0.0595 0.5182 0.1609 0.079 Uiso 1 1 calc R . . H23C H 0.1241 0.4823 0.1794 0.079 Uiso 1 1 calc R . . C24 C 0.2104(2) 0.9972(5) 0.1398(3) 0.0320(12) Uani 1 1 d . . . C25 C 0.1585(2) 1.0651(6) 0.1083(3) 0.0404(14) Uani 1 1 d . . . C26 C 0.1544(3) 1.1635(7) 0.0527(3) 0.0507(16) Uani 1 1 d . . . H26 H 0.1198 1.2075 0.0319 0.061 Uiso 1 1 calc R . . C27 C 0.2004(3) 1.1976(7) 0.0276(3) 0.0544(17) Uani 1 1 d . . . H27 H 0.1973 1.2645 -0.0098 0.065 Uiso 1 1 calc R . . C28 C 0.2509(3) 1.1315(7) 0.0584(3) 0.0510(16) Uani 1 1 d . . . H28 H 0.2822 1.1562 0.0419 0.061 Uiso 1 1 calc R . . C29 C 0.2571(2) 1.0306(6) 0.1126(3) 0.0389(13) Uani 1 1 d . . . C30 C 0.1078(2) 1.0357(7) 0.1367(3) 0.0442(14) Uani 1 1 d . . . H30 H 0.1075 0.9275 0.1466 0.053 Uiso 1 1 calc R . . C31 C 0.1128(3) 1.1168(7) 0.2064(3) 0.0545(17) Uani 1 1 d . . . H31A H 0.1485 1.0931 0.2381 0.082 Uiso 1 1 calc R . . H31B H 0.0829 1.0850 0.2268 0.082 Uiso 1 1 calc R . . H31C H 0.1103 1.2235 0.1984 0.082 Uiso 1 1 calc R . . C32 C 0.0513(3) 1.0735(8) 0.0868(4) 0.070(2) Uani 1 1 d . . . H32A H 0.0484 1.1805 0.0797 0.106 Uiso 1 1 calc R . . H32B H 0.0215 1.0395 0.1068 0.106 Uiso 1 1 calc R . . H32C H 0.0483 1.0243 0.0423 0.106 Uiso 1 1 calc R . . C33 C 0.3142(2) 0.9650(6) 0.1450(3) 0.0389(13) Uani 1 1 d . . . H33 H 0.3082 0.8729 0.1697 0.047 Uiso 1 1 calc R . . C34 C 0.3489(3) 1.0689(7) 0.1990(3) 0.0587(18) Uani 1 1 d . . . H34A H 0.3582 1.1574 0.1761 0.088 Uiso 1 1 calc R . . H34B H 0.3829 1.0187 0.2233 0.088 Uiso 1 1 calc R . . H34C H 0.3278 1.0973 0.2323 0.088 Uiso 1 1 calc R . . C35 C 0.3471(3) 0.9210(8) 0.0922(4) 0.078(2) Uani 1 1 d . . . H35A H 0.3569 1.0099 0.0700 0.117 Uiso 1 1 calc R . . H35B H 0.3245 0.8561 0.0571 0.117 Uiso 1 1 calc R . . H35C H 0.3809 0.8691 0.1161 0.117 Uiso 1 1 calc R . . C36 C 0.2446(3) 0.3929(6) 0.2052(3) 0.0475(15) Uani 1 1 d . . . H36A H 0.2814 0.3605 0.2009 0.057 Uiso 1 1 calc R . . H36B H 0.2162 0.3338 0.1728 0.057 Uiso 1 1 calc R . . C37 C 0.2399(3) 0.3705(6) 0.2776(3) 0.0490(16) Uani 1 1 d . . . H37A H 0.2007 0.3770 0.2791 0.059 Uiso 1 1 calc R . . H37B H 0.2537 0.2712 0.2940 0.059 Uiso 1 1 calc R . . C38 C 0.2241(3) 0.5742(7) 0.1145(3) 0.0506(16) Uani 1 1 d . . . H38A H 0.2528 0.5293 0.0954 0.076 Uiso 1 1 calc R . . H38B H 0.2227 0.6806 0.1055 0.076 Uiso 1 1 calc R . . H38C H 0.1883 0.5300 0.0926 0.076 Uiso 1 1 calc R . . C39 C 0.2755(3) 0.4545(7) 0.3944(3) 0.063(2) Uani 1 1 d . . . H39A H 0.2385 0.4567 0.4028 0.095 Uiso 1 1 calc R . . H39B H 0.2985 0.5309 0.4223 0.095 Uiso 1 1 calc R . . H39C H 0.2922 0.3574 0.4073 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0270(2) 0.0307(3) 0.0285(3) -0.0010(2) 0.00322(18) 0.0005(2) Si1 0.0311(9) 0.0508(10) 0.0691(13) -0.0131(9) 0.0128(9) 0.0022(8) Si2 0.0295(8) 0.0436(9) 0.0434(10) -0.0029(8) 0.0051(7) -0.0058(7) O1 0.049(2) 0.0307(19) 0.030(2) -0.0025(16) 0.0012(18) -0.0029(17) O2 0.046(2) 0.043(2) 0.034(2) 0.0089(18) 0.0017(18) -0.0031(19) N1 0.031(2) 0.036(2) 0.042(3) -0.005(2) 0.010(2) 0.001(2) N2 0.033(3) 0.041(3) 0.044(3) -0.010(2) 0.006(2) -0.004(2) N3 0.030(2) 0.044(3) 0.036(3) -0.008(2) 0.009(2) -0.009(2) N4 0.042(3) 0.093(4) 0.042(3) -0.034(3) 0.020(3) -0.024(3) N5 0.032(3) 0.034(2) 0.046(3) 0.001(2) 0.006(2) 0.000(2) C1 0.027(3) 0.037(3) 0.043(3) 0.005(3) 0.009(3) 0.001(2) C2 0.044(3) 0.045(3) 0.034(3) -0.006(3) 0.016(3) -0.011(3) C3 0.037(3) 0.049(4) 0.055(4) -0.022(3) 0.012(3) -0.007(3) C4 0.066(7) 0.044(6) 0.048(6) -0.028(5) 0.014(6) -0.014(5) C4' 0.046(10) 0.061(11) 0.023(9) -0.012(8) -0.001(8) -0.013(9) C5 0.064(5) 0.138(8) 0.052(4) -0.065(5) 0.018(4) -0.050(5) C6 0.030(3) 0.050(4) 0.049(4) -0.007(3) 0.003(3) -0.004(3) C7 0.043(4) 0.076(5) 0.060(4) -0.009(4) 0.008(3) -0.018(4) C8 0.034(4) 0.107(7) 0.077(6) -0.030(5) 0.009(4) -0.024(4) C9 0.049(5) 0.088(6) 0.107(7) -0.026(5) -0.021(5) 0.014(4) C10 0.081(6) 0.058(5) 0.087(6) 0.007(4) -0.040(5) 0.001(4) C11 0.058(5) 0.052(4) 0.069(5) 0.007(4) -0.015(4) 0.001(3) C12 0.039(3) 0.052(4) 0.030(3) -0.012(3) 0.005(3) -0.009(3) C13 0.044(3) 0.059(4) 0.040(3) -0.006(3) 0.015(3) -0.007(3) C14 0.057(4) 0.093(6) 0.042(4) -0.008(4) 0.021(3) -0.016(4) C15 0.053(5) 0.111(7) 0.053(5) -0.022(5) 0.019(4) 0.004(5) C16 0.057(5) 0.082(5) 0.057(5) -0.021(4) 0.003(4) 0.017(4) C17 0.066(5) 0.059(4) 0.040(4) -0.009(3) 0.017(3) -0.001(3) C18 0.078(5) 0.072(5) 0.062(5) -0.012(4) 0.027(4) 0.000(4) C19 0.073(5) 0.057(4) 0.065(5) -0.008(4) -0.009(4) 0.024(4) C20 0.047(5) 0.115(7) 0.171(9) -0.072(7) 0.050(6) -0.019(5) C21 0.038(4) 0.064(4) 0.085(5) -0.009(4) 0.007(3) 0.000(3) C22 0.051(4) 0.051(4) 0.058(4) -0.004(3) 0.014(3) -0.019(3) C23 0.045(4) 0.059(4) 0.046(4) -0.001(3) -0.004(3) -0.009(3) C24 0.039(3) 0.026(3) 0.029(3) -0.002(2) 0.004(2) 0.002(2) C25 0.045(3) 0.033(3) 0.037(3) -0.002(3) -0.003(3) 0.005(3) C26 0.054(4) 0.049(4) 0.041(4) 0.004(3) -0.003(3) 0.009(3) C27 0.074(5) 0.047(4) 0.037(4) 0.010(3) 0.006(3) 0.009(3) C28 0.069(5) 0.045(4) 0.042(4) 0.003(3) 0.020(3) 0.004(3) C29 0.045(3) 0.037(3) 0.032(3) -0.002(3) 0.006(3) 0.003(3) C30 0.031(3) 0.042(3) 0.053(4) 0.004(3) -0.002(3) -0.001(3) C31 0.052(4) 0.051(4) 0.064(4) -0.006(3) 0.020(3) 0.004(3) C32 0.036(4) 0.087(6) 0.076(5) 0.006(4) -0.009(3) 0.011(4) C33 0.041(3) 0.038(3) 0.040(3) 0.003(3) 0.014(3) 0.005(3) C34 0.051(4) 0.051(4) 0.067(5) 0.002(3) 0.002(3) -0.001(3) C35 0.078(6) 0.084(6) 0.078(5) 0.001(4) 0.029(5) 0.031(5) C36 0.058(4) 0.032(3) 0.051(4) -0.008(3) 0.011(3) 0.001(3) C37 0.059(4) 0.031(3) 0.055(4) 0.000(3) 0.010(3) -0.002(3) C38 0.067(4) 0.053(4) 0.026(3) -0.004(3) 0.000(3) -0.001(3) C39 0.083(5) 0.063(4) 0.038(4) 0.012(3) 0.004(4) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N5 2.237(4) . ? Y1 N4 2.332(4) . ? Y1 N2 2.358(4) . ? Y1 O1 2.428(3) . ? Y1 O2 2.462(4) . ? Y1 N1 2.465(4) . ? Y1 N3 2.543(4) . ? Y1 C1 2.780(5) . ? Y1 C2 2.836(5) . ? Si1 N1 1.730(4) . ? Si1 C19 1.869(7) . ? Si1 C20 1.870(7) . ? Si1 C18 1.871(7) . ? Si2 N3 1.724(4) . ? Si2 C21 1.862(6) . ? Si2 C23 1.873(6) . ? Si2 C22 1.875(6) . ? O1 C38 1.436(6) . ? O1 C36 1.436(6) . ? O2 C37 1.426(6) . ? O2 C39 1.432(6) . ? N1 C1 1.330(7) . ? N2 C1 1.321(6) . ? N2 C3 1.479(7) . ? N3 C2 1.331(6) . ? N4 C2 1.313(7) . ? N4 C5 1.467(7) . ? N5 C24 1.397(6) . ? N5 H5 0.8700 . ? C1 C6 1.502(7) . ? C2 C12 1.515(7) . ? C3 C4' 1.510(13) . ? C3 C4 1.523(10) . ? C4 C5 1.473(10) . ? C4' C5 1.519(13) . ? C6 C7 1.388(8) . ? C6 C11 1.393(8) . ? C7 C8 1.406(9) . ? C7 H7 0.9400 . ? C8 C9 1.378(11) . ? C8 H8 0.9400 . ? C9 C10 1.356(11) . ? C9 H9 0.9400 . ? C10 C11 1.372(9) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C13 1.375(8) . ? C12 C17 1.381(8) . ? C13 C14 1.384(8) . ? C13 H13 0.9400 . ? C14 C15 1.368(10) . ? C14 H14 0.9400 . ? C15 C16 1.375(10) . ? C15 H15 0.9400 . ? C16 C17 1.394(8) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.418(7) . ? C24 C29 1.424(7) . ? C25 C26 1.393(8) . ? C25 C30 1.518(8) . ? C26 C27 1.385(9) . ? C26 H26 0.9400 . ? C27 C28 1.381(8) . ? C27 H27 0.9400 . ? C28 C29 1.380(7) . ? C28 H28 0.9400 . ? C29 C33 1.519(7) . ? C30 C31 1.535(8) . ? C30 C32 1.537(7) . ? C30 H30 0.9900 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.514(8) . ? C33 C35 1.525(8) . ? C33 H33 0.9900 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 C37 1.480(7) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Y1 N4 105.99(19) . . ? N5 Y1 N2 101.22(16) . . ? N4 Y1 N2 73.16(16) . . ? N5 Y1 O1 85.62(14) . . ? N4 Y1 O1 138.55(15) . . ? N2 Y1 O1 144.72(14) . . ? N5 Y1 O2 147.03(14) . . ? N4 Y1 O2 88.34(17) . . ? N2 Y1 O2 111.41(15) . . ? O1 Y1 O2 65.13(12) . . ? N5 Y1 N1 117.79(15) . . ? N4 Y1 N1 116.58(17) . . ? N2 Y1 N1 55.83(15) . . ? O1 Y1 N1 90.20(14) . . ? O2 Y1 N1 79.02(13) . . ? N5 Y1 N3 85.57(16) . . ? N4 Y1 N3 54.95(15) . . ? N2 Y1 N3 127.21(14) . . ? O1 Y1 N3 87.55(13) . . ? O2 Y1 N3 78.63(14) . . ? N1 Y1 N3 156.29(15) . . ? N5 Y1 C1 117.31(16) . . ? N4 Y1 C1 91.51(17) . . ? N2 Y1 C1 28.30(15) . . ? O1 Y1 C1 118.76(14) . . ? O2 Y1 C1 91.17(14) . . ? N1 Y1 C1 28.58(14) . . ? N3 Y1 C1 144.76(15) . . ? N5 Y1 C2 93.78(17) . . ? N4 Y1 C2 27.28(16) . . ? N2 Y1 C2 99.35(15) . . ? O1 Y1 C2 114.83(14) . . ? O2 Y1 C2 85.69(15) . . ? N1 Y1 C2 141.67(16) . . ? N3 Y1 C2 27.98(14) . . ? C1 Y1 C2 118.67(16) . . ? N1 Si1 C19 112.1(3) . . ? N1 Si1 C20 115.6(3) . . ? C19 Si1 C20 106.4(4) . . ? N1 Si1 C18 107.6(3) . . ? C19 Si1 C18 108.2(3) . . ? C20 Si1 C18 106.6(4) . . ? N3 Si2 C21 116.2(3) . . ? N3 Si2 C23 107.0(2) . . ? C21 Si2 C23 105.5(3) . . ? N3 Si2 C22 111.1(3) . . ? C21 Si2 C22 106.9(3) . . ? C23 Si2 C22 109.9(3) . . ? C38 O1 C36 111.8(4) . . ? C38 O1 Y1 125.5(3) . . ? C36 O1 Y1 121.6(3) . . ? C37 O2 C39 112.7(4) . . ? C37 O2 Y1 116.6(3) . . ? C39 O2 Y1 119.3(3) . . ? C1 N1 Si1 127.0(4) . . ? C1 N1 Y1 89.0(3) . . ? Si1 N1 Y1 141.7(2) . . ? C1 N2 C3 121.6(5) . . ? C1 N2 Y1 93.9(3) . . ? C3 N2 Y1 137.5(3) . . ? C2 N3 Si2 126.7(4) . . ? C2 N3 Y1 88.3(3) . . ? Si2 N3 Y1 145.0(2) . . ? C2 N4 C5 120.5(5) . . ? C2 N4 Y1 98.2(3) . . ? C5 N4 Y1 138.5(4) . . ? C24 N5 Y1 156.5(4) . . ? C24 N5 H5 101.7 . . ? Y1 N5 H5 101.7 . . ? N2 C1 N1 117.0(5) . . ? N2 C1 C6 120.6(5) . . ? N1 C1 C6 122.4(5) . . ? N2 C1 Y1 57.8(3) . . ? N1 C1 Y1 62.5(3) . . ? C6 C1 Y1 158.4(4) . . ? N4 C2 N3 117.2(5) . . ? N4 C2 C12 120.7(5) . . ? N3 C2 C12 122.1(5) . . ? N4 C2 Y1 54.5(3) . . ? N3 C2 Y1 63.7(3) . . ? C12 C2 Y1 169.2(4) . . ? N2 C3 C4' 110.5(8) . . ? N2 C3 C4 112.1(5) . . ? C4' C3 C4 46.7(7) . . ? C5 C4 C3 119.0(7) . . ? C3 C4' C5 116.9(10) . . ? N4 C5 C4 109.5(6) . . ? N4 C5 C4' 117.5(8) . . ? C4 C5 C4' 47.3(7) . . ? C7 C6 C11 119.1(6) . . ? C7 C6 C1 121.8(6) . . ? C11 C6 C1 119.1(5) . . ? C6 C7 C8 119.4(7) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 119.4(7) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 121.0(7) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 120.2(8) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 120.7(7) . . ? C10 C11 H11 119.6 . . ? C6 C11 H11 119.6 . . ? C13 C12 C17 119.3(6) . . ? C13 C12 C2 120.8(6) . . ? C17 C12 C2 120.0(5) . . ? C12 C13 C14 120.3(6) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 120.2(7) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.6(7) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 119.1(7) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C12 C17 C16 120.6(6) . . ? C12 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 C25 122.1(5) . . ? N5 C24 C29 119.4(5) . . ? C25 C24 C29 118.5(5) . . ? C26 C25 C24 119.8(6) . . ? C26 C25 C30 119.9(5) . . ? C24 C25 C30 120.3(5) . . ? C27 C26 C25 121.3(6) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C28 C27 C26 118.7(6) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C29 C28 C27 122.6(6) . . ? C29 C28 H28 118.7 . . ? C27 C28 H28 118.7 . . ? C28 C29 C24 119.1(5) . . ? C28 C29 C33 119.6(5) . . ? C24 C29 C33 121.2(5) . . ? C25 C30 C31 111.1(5) . . ? C25 C30 C32 115.3(5) . . ? C31 C30 C32 109.2(5) . . ? C25 C30 H30 106.9 . . ? C31 C30 H30 106.9 . . ? C32 C30 H30 106.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C29 111.3(5) . . ? C34 C33 C35 109.7(5) . . ? C29 C33 C35 114.3(5) . . ? C34 C33 H33 107.1 . . ? C29 C33 H33 107.1 . . ? C35 C33 H33 107.1 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O1 C36 C37 108.4(4) . . ? O1 C36 H36A 110.0 . . ? C37 C36 H36A 110.0 . . ? O1 C36 H36B 110.0 . . ? C37 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? O2 C37 C36 109.6(5) . . ? O2 C37 H37A 109.7 . . ? C36 C37 H37A 109.7 . . ? O2 C37 H37B 109.7 . . ? C36 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? O1 C38 H38A 109.5 . . ? O1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O2 C39 H39A 109.5 . . ? O2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Y1 O1 C38 23.7(4) . . . . ? N4 Y1 O1 C38 133.0(4) . . . . ? N2 Y1 O1 C38 -79.6(5) . . . . ? O2 Y1 O1 C38 -172.0(4) . . . . ? N1 Y1 O1 C38 -94.2(4) . . . . ? N3 Y1 O1 C38 109.4(4) . . . . ? C1 Y1 O1 C38 -95.2(4) . . . . ? C2 Y1 O1 C38 115.8(4) . . . . ? N5 Y1 O1 C36 -169.5(4) . . . . ? N4 Y1 O1 C36 -60.2(5) . . . . ? N2 Y1 O1 C36 87.3(4) . . . . ? O2 Y1 O1 C36 -5.1(4) . . . . ? N1 Y1 O1 C36 72.7(4) . . . . ? N3 Y1 O1 C36 -83.7(4) . . . . ? C1 Y1 O1 C36 71.7(4) . . . . ? C2 Y1 O1 C36 -77.3(4) . . . . ? N5 Y1 O2 C37 7.7(5) . . . . ? N4 Y1 O2 C37 125.2(4) . . . . ? N2 Y1 O2 C37 -163.6(4) . . . . ? O1 Y1 O2 C37 -21.9(4) . . . . ? N1 Y1 O2 C37 -117.3(4) . . . . ? N3 Y1 O2 C37 70.7(4) . . . . ? C1 Y1 O2 C37 -143.3(4) . . . . ? C2 Y1 O2 C37 98.0(4) . . . . ? N5 Y1 O2 C39 -133.2(4) . . . . ? N4 Y1 O2 C39 -15.7(4) . . . . ? N2 Y1 O2 C39 55.5(4) . . . . ? O1 Y1 O2 C39 -162.8(4) . . . . ? N1 Y1 O2 C39 101.8(4) . . . . ? N3 Y1 O2 C39 -70.2(4) . . . . ? C1 Y1 O2 C39 75.8(4) . . . . ? C2 Y1 O2 C39 -42.9(4) . . . . ? C19 Si1 N1 C1 87.9(5) . . . . ? C20 Si1 N1 C1 -34.3(6) . . . . ? C18 Si1 N1 C1 -153.2(5) . . . . ? C19 Si1 N1 Y1 -68.8(5) . . . . ? C20 Si1 N1 Y1 169.1(4) . . . . ? C18 Si1 N1 Y1 50.1(5) . . . . ? N5 Y1 N1 C1 96.7(3) . . . . ? N4 Y1 N1 C1 -31.0(4) . . . . ? N2 Y1 N1 C1 12.0(3) . . . . ? O1 Y1 N1 C1 -178.2(3) . . . . ? O2 Y1 N1 C1 -113.6(3) . . . . ? N3 Y1 N1 C1 -93.8(4) . . . . ? C2 Y1 N1 C1 -45.2(4) . . . . ? N5 Y1 N1 Si1 -101.7(4) . . . . ? N4 Y1 N1 Si1 130.5(4) . . . . ? N2 Y1 N1 Si1 173.5(5) . . . . ? O1 Y1 N1 Si1 -16.6(4) . . . . ? O2 Y1 N1 Si1 48.0(4) . . . . ? N3 Y1 N1 Si1 67.8(6) . . . . ? C1 Y1 N1 Si1 161.6(6) . . . . ? C2 Y1 N1 Si1 116.4(4) . . . . ? N5 Y1 N2 C1 -128.2(3) . . . . ? N4 Y1 N2 C1 128.3(4) . . . . ? O1 Y1 N2 C1 -29.8(5) . . . . ? O2 Y1 N2 C1 47.0(3) . . . . ? N1 Y1 N2 C1 -12.1(3) . . . . ? N3 Y1 N2 C1 138.8(3) . . . . ? C2 Y1 N2 C1 136.0(3) . . . . ? N5 Y1 N2 C3 83.4(6) . . . . ? N4 Y1 N2 C3 -20.0(5) . . . . ? O1 Y1 N2 C3 -178.2(5) . . . . ? O2 Y1 N2 C3 -101.4(6) . . . . ? N1 Y1 N2 C3 -160.5(6) . . . . ? N3 Y1 N2 C3 -9.5(6) . . . . ? C1 Y1 N2 C3 -148.4(7) . . . . ? C2 Y1 N2 C3 -12.3(6) . . . . ? C21 Si2 N3 C2 49.5(6) . . . . ? C23 Si2 N3 C2 167.0(5) . . . . ? C22 Si2 N3 C2 -73.0(6) . . . . ? C21 Si2 N3 Y1 -129.3(4) . . . . ? C23 Si2 N3 Y1 -11.8(5) . . . . ? C22 Si2 N3 Y1 108.2(4) . . . . ? N5 Y1 N3 C2 -106.7(3) . . . . ? N4 Y1 N3 C2 6.4(4) . . . . ? N2 Y1 N3 C2 -5.9(4) . . . . ? O1 Y1 N3 C2 167.5(3) . . . . ? O2 Y1 N3 C2 102.4(3) . . . . ? N1 Y1 N3 C2 82.6(5) . . . . ? C1 Y1 N3 C2 26.8(5) . . . . ? N5 Y1 N3 Si2 72.4(4) . . . . ? N4 Y1 N3 Si2 -174.5(5) . . . . ? N2 Y1 N3 Si2 173.1(4) . . . . ? O1 Y1 N3 Si2 -13.4(4) . . . . ? O2 Y1 N3 Si2 -78.5(4) . . . . ? N1 Y1 N3 Si2 -98.3(5) . . . . ? C1 Y1 N3 Si2 -154.1(4) . . . . ? C2 Y1 N3 Si2 179.1(7) . . . . ? N5 Y1 N4 C2 66.1(4) . . . . ? N2 Y1 N4 C2 163.2(5) . . . . ? O1 Y1 N4 C2 -35.7(6) . . . . ? O2 Y1 N4 C2 -83.8(4) . . . . ? N1 Y1 N4 C2 -160.7(4) . . . . ? N3 Y1 N4 C2 -6.5(4) . . . . ? C1 Y1 N4 C2 -174.9(4) . . . . ? N5 Y1 N4 C5 -93.7(8) . . . . ? N2 Y1 N4 C5 3.5(8) . . . . ? O1 Y1 N4 C5 164.6(7) . . . . ? O2 Y1 N4 C5 116.5(8) . . . . ? N1 Y1 N4 C5 39.6(8) . . . . ? N3 Y1 N4 C5 -166.3(9) . . . . ? C1 Y1 N4 C5 25.4(8) . . . . ? C2 Y1 N4 C5 -159.7(11) . . . . ? N4 Y1 N5 C24 131.6(9) . . . . ? N2 Y1 N5 C24 56.1(9) . . . . ? O1 Y1 N5 C24 -89.0(9) . . . . ? O2 Y1 N5 C24 -115.7(9) . . . . ? N1 Y1 N5 C24 -1.1(9) . . . . ? N3 Y1 N5 C24 -176.9(9) . . . . ? C1 Y1 N5 C24 31.3(9) . . . . ? C2 Y1 N5 C24 156.4(9) . . . . ? C3 N2 C1 N1 176.5(5) . . . . ? Y1 N2 C1 N1 21.1(5) . . . . ? C3 N2 C1 C6 0.7(8) . . . . ? Y1 N2 C1 C6 -154.7(4) . . . . ? C3 N2 C1 Y1 155.4(6) . . . . ? Si1 N1 C1 N2 174.1(4) . . . . ? Y1 N1 C1 N2 -20.1(5) . . . . ? Si1 N1 C1 C6 -10.2(8) . . . . ? Y1 N1 C1 C6 155.6(5) . . . . ? Si1 N1 C1 Y1 -165.8(5) . . . . ? N5 Y1 C1 N2 60.2(4) . . . . ? N4 Y1 C1 N2 -48.7(4) . . . . ? O1 Y1 C1 N2 160.9(3) . . . . ? O2 Y1 C1 N2 -137.1(3) . . . . ? N1 Y1 C1 N2 158.8(5) . . . . ? N3 Y1 C1 N2 -65.3(4) . . . . ? C2 Y1 C1 N2 -51.3(4) . . . . ? N5 Y1 C1 N1 -98.6(3) . . . . ? N4 Y1 C1 N1 152.5(3) . . . . ? N2 Y1 C1 N1 -158.8(5) . . . . ? O1 Y1 C1 N1 2.1(4) . . . . ? O2 Y1 C1 N1 64.2(3) . . . . ? N3 Y1 C1 N1 135.9(3) . . . . ? C2 Y1 C1 N1 149.9(3) . . . . ? N5 Y1 C1 C6 152.6(10) . . . . ? N4 Y1 C1 C6 43.7(11) . . . . ? N2 Y1 C1 C6 92.4(11) . . . . ? O1 Y1 C1 C6 -106.7(10) . . . . ? O2 Y1 C1 C6 -44.6(10) . . . . ? N1 Y1 C1 C6 -108.8(11) . . . . ? N3 Y1 C1 C6 27.1(12) . . . . ? C2 Y1 C1 C6 41.1(11) . . . . ? C5 N4 C2 N3 176.1(6) . . . . ? Y1 N4 C2 N3 11.6(6) . . . . ? C5 N4 C2 C12 -3.9(10) . . . . ? Y1 N4 C2 C12 -168.5(5) . . . . ? C5 N4 C2 Y1 164.5(8) . . . . ? Si2 N3 C2 N4 170.2(5) . . . . ? Y1 N3 C2 N4 -10.5(6) . . . . ? Si2 N3 C2 C12 -9.8(8) . . . . ? Y1 N3 C2 C12 169.5(5) . . . . ? Si2 N3 C2 Y1 -179.3(5) . . . . ? N5 Y1 C2 N4 -118.3(4) . . . . ? N2 Y1 C2 N4 -16.3(4) . . . . ? O1 Y1 C2 N4 154.8(4) . . . . ? O2 Y1 C2 N4 94.8(4) . . . . ? N1 Y1 C2 N4 28.5(5) . . . . ? N3 Y1 C2 N4 168.5(6) . . . . ? C1 Y1 C2 N4 5.8(5) . . . . ? N5 Y1 C2 N3 73.2(3) . . . . ? N4 Y1 C2 N3 -168.5(6) . . . . ? N2 Y1 C2 N3 175.2(3) . . . . ? O1 Y1 C2 N3 -13.7(4) . . . . ? O2 Y1 C2 N3 -73.8(3) . . . . ? N1 Y1 C2 N3 -140.0(3) . . . . ? C1 Y1 C2 N3 -162.7(3) . . . . ? N5 Y1 C2 C12 -52(2) . . . . ? N4 Y1 C2 C12 67(2) . . . . ? N2 Y1 C2 C12 50(2) . . . . ? O1 Y1 C2 C12 -139(2) . . . . ? O2 Y1 C2 C12 161(2) . . . . ? N1 Y1 C2 C12 95(2) . . . . ? N3 Y1 C2 C12 -125(2) . . . . ? C1 Y1 C2 C12 72(2) . . . . ? C1 N2 C3 C4' -93.1(9) . . . . ? Y1 N2 C3 C4' 49.0(10) . . . . ? C1 N2 C3 C4 -143.4(6) . . . . ? Y1 N2 C3 C4 -1.3(9) . . . . ? N2 C3 C4 C5 52.8(10) . . . . ? C4' C3 C4 C5 -45.0(9) . . . . ? N2 C3 C4' C5 -59.3(14) . . . . ? C4 C3 C4' C5 42.2(9) . . . . ? C2 N4 C5 C4 -124.9(8) . . . . ? Y1 N4 C5 C4 31.7(12) . . . . ? C2 N4 C5 C4' -176.1(10) . . . . ? Y1 N4 C5 C4' -19.5(15) . . . . ? C3 C4 C5 N4 -65.8(10) . . . . ? C3 C4 C5 C4' 44.0(9) . . . . ? C3 C4' C5 N4 48.4(17) . . . . ? C3 C4' C5 C4 -43.5(9) . . . . ? N2 C1 C6 C7 -80.4(7) . . . . ? N1 C1 C6 C7 104.0(7) . . . . ? Y1 C1 C6 C7 -159.5(8) . . . . ? N2 C1 C6 C11 99.0(7) . . . . ? N1 C1 C6 C11 -76.6(8) . . . . ? Y1 C1 C6 C11 19.9(14) . . . . ? C11 C6 C7 C8 2.6(10) . . . . ? C1 C6 C7 C8 -178.0(6) . . . . ? C6 C7 C8 C9 -2.9(11) . . . . ? C7 C8 C9 C10 1.2(13) . . . . ? C8 C9 C10 C11 0.9(13) . . . . ? C9 C10 C11 C6 -1.3(12) . . . . ? C7 C6 C11 C10 -0.5(11) . . . . ? C1 C6 C11 C10 -179.9(7) . . . . ? N4 C2 C12 C13 -92.1(7) . . . . ? N3 C2 C12 C13 87.8(7) . . . . ? Y1 C2 C12 C13 -152.5(19) . . . . ? N4 C2 C12 C17 87.3(8) . . . . ? N3 C2 C12 C17 -92.8(7) . . . . ? Y1 C2 C12 C17 27(2) . . . . ? C17 C12 C13 C14 1.4(9) . . . . ? C2 C12 C13 C14 -179.2(5) . . . . ? C12 C13 C14 C15 -0.9(10) . . . . ? C13 C14 C15 C16 0.5(11) . . . . ? C14 C15 C16 C17 -0.5(11) . . . . ? C13 C12 C17 C16 -1.4(9) . . . . ? C2 C12 C17 C16 179.2(6) . . . . ? C15 C16 C17 C12 1.0(10) . . . . ? Y1 N5 C24 C25 179.9(6) . . . . ? Y1 N5 C24 C29 1.2(12) . . . . ? N5 C24 C25 C26 -179.6(5) . . . . ? C29 C24 C25 C26 -0.8(8) . . . . ? N5 C24 C25 C30 2.8(8) . . . . ? C29 C24 C25 C30 -178.5(5) . . . . ? C24 C25 C26 C27 -0.5(9) . . . . ? C30 C25 C26 C27 177.2(5) . . . . ? C25 C26 C27 C28 0.3(10) . . . . ? C26 C27 C28 C29 1.2(10) . . . . ? C27 C28 C29 C24 -2.5(9) . . . . ? C27 C28 C29 C33 -178.7(5) . . . . ? N5 C24 C29 C28 -178.9(5) . . . . ? C25 C24 C29 C28 2.3(8) . . . . ? N5 C24 C29 C33 -2.9(8) . . . . ? C25 C24 C29 C33 178.4(5) . . . . ? C26 C25 C30 C31 -104.5(6) . . . . ? C24 C25 C30 C31 73.2(7) . . . . ? C26 C25 C30 C32 20.5(8) . . . . ? C24 C25 C30 C32 -161.9(5) . . . . ? C28 C29 C33 C34 82.8(7) . . . . ? C24 C29 C33 C34 -93.3(6) . . . . ? C28 C29 C33 C35 -42.2(8) . . . . ? C24 C29 C33 C35 141.8(6) . . . . ? C38 O1 C36 C37 -162.6(5) . . . . ? Y1 O1 C36 C37 29.0(6) . . . . ? C39 O2 C37 C36 -171.6(5) . . . . ? Y1 O2 C37 C36 45.0(6) . . . . ? O1 C36 C37 O2 -45.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.522 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.071