Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Luo, Yunjie' _publ_contact_author_email lyj@nit.zju.edu.cn _publ_section_title ; Rare earth metal bis(amide) complexes bearing amidinate ancillary ligands: Synthesis, characterization, and performance as catalyst precursors for cis-1,4 selective polymerization of isoprene ; _publ_author_name 'Yunjie Luo' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 792825' #TrackingRef 'data.doc' #TrackingRef 'data.doc' #TrackingRef 'data.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H65 N4 Si4 Y, 0.5(C6 H14)' _chemical_formula_sum 'C38 H72 N4 Si4 Y' _chemical_formula_weight 786.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 12.393(6) _cell_length_b 13.632(8) _cell_length_c 15.539(8) _cell_angle_alpha 104.788(14) _cell_angle_beta 108.411(6) _cell_angle_gamma 100.221(13) _cell_volume 2311(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8872 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.130 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 846 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4019 _exptl_absorpt_correction_T_max 0.6057 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21645 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8376 _reflns_number_gt 6520 _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^)+(0.0694P)^2^+2.4431P] 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 8376 _refine_ls_number_parameters 403 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.1781 _refine_ls_wR_factor_gt 0.1641 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.002 _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 0.53318(4) 0.23978(4) 0.27305(3) 0.03825(17) Uani 1 1 d . . . Si1 Si 0.29038(13) 0.00406(12) 0.18120(11) 0.0495(4) Uani 1 1 d . . . Si2 Si 0.27148(13) 0.21937(13) 0.27008(11) 0.0501(4) Uani 1 1 d . . . Si3 Si 0.65070(15) 0.50115(12) 0.27804(12) 0.0542(4) Uani 1 1 d . . . Si4 Si 0.51942(14) 0.32039(12) 0.09358(11) 0.0503(4) Uani 1 1 d . . . N1 N 0.6793(4) 0.1542(3) 0.3010(3) 0.0412(10) Uani 1 1 d . . . N2 N 0.6648(4) 0.2634(3) 0.4274(3) 0.0424(10) Uani 1 1 d . . . N3 N 0.3504(3) 0.1383(3) 0.2325(3) 0.0408(10) Uani 1 1 d . . . N4 N 0.5702(4) 0.3710(3) 0.2155(3) 0.0445(10) Uani 1 1 d . . . C1 C 0.7207(4) 0.1949(4) 0.3968(4) 0.0403(11) Uani 1 1 d . . . C2 C 0.7282(4) 0.0803(4) 0.2520(3) 0.0422(12) Uani 1 1 d . . . C3 C 0.8005(5) 0.1159(5) 0.2058(4) 0.0500(13) Uani 1 1 d . . . C4 C 0.8432(5) 0.0444(6) 0.1562(4) 0.0647(17) Uani 1 1 d . . . H4 H 0.8909 0.0673 0.1254 0.078 Uiso 1 1 calc R . . C5 C 0.8179(6) -0.0597(6) 0.1506(5) 0.075(2) Uani 1 1 d . . . H5 H 0.8487 -0.1063 0.1169 0.091 Uiso 1 1 calc R . . C6 C 0.7473(6) -0.0942(5) 0.1947(4) 0.0670(18) Uani 1 1 d . . . H6 H 0.7298 -0.1649 0.1904 0.080 Uiso 1 1 calc R . . C7 C 0.7009(5) -0.0265(4) 0.2458(4) 0.0487(13) Uani 1 1 d . . . C8 C 0.8308(6) 0.2293(5) 0.2105(5) 0.0706(18) Uani 1 1 d . . . H8A H 0.8821 0.2392 0.1764 0.106 Uiso 1 1 calc R . . H8B H 0.8701 0.2742 0.2764 0.106 Uiso 1 1 calc R . . H8C H 0.7594 0.2469 0.1815 0.106 Uiso 1 1 calc R . . C9 C 0.6234(6) -0.0682(5) 0.2940(5) 0.0676(17) Uani 1 1 d . . . H9A H 0.5719 -0.1370 0.2527 0.101 Uiso 1 1 calc R . . H9B H 0.5766 -0.0211 0.3061 0.101 Uiso 1 1 calc R . . H9C H 0.6723 -0.0728 0.3537 0.101 Uiso 1 1 calc R . . C10 C 0.6868(7) 0.3128(6) 0.5250(5) 0.0813(10) Uani 1 1 d . . . C11 C 0.7752(7) 0.4079(6) 0.5825(5) 0.0813(10) Uani 1 1 d . . . C12 C 0.7906(7) 0.4539(6) 0.6791(5) 0.0813(10) Uani 1 1 d . . . H12 H 0.8499 0.5163 0.7182 0.098 Uiso 1 1 calc R . . C13 C 0.7182(7) 0.4063(6) 0.7138(5) 0.0813(10) Uani 1 1 d . . . H13 H 0.7304 0.4366 0.7782 0.098 Uiso 1 1 calc R . . C14 C 0.6284(7) 0.3170(6) 0.6608(5) 0.0813(10) Uani 1 1 d . . . H14 H 0.5786 0.2885 0.6876 0.098 Uiso 1 1 calc R . . C15 C 0.6122(7) 0.2688(6) 0.5662(5) 0.0813(10) Uani 1 1 d . . . C16 C 0.8531(6) 0.4610(5) 0.5415(6) 0.094(3) Uani 1 1 d . . . H16A H 0.8305 0.4205 0.4751 0.141 Uiso 1 1 calc R . . H16B H 0.9341 0.4659 0.5765 0.141 Uiso 1 1 calc R . . H16C H 0.8446 0.5307 0.5468 0.141 Uiso 1 1 calc R . . C17 C 0.5151(6) 0.1670(7) 0.5077(5) 0.090(2) Uani 1 1 d . . . H17A H 0.4699 0.1716 0.4467 0.135 Uiso 1 1 calc R . . H17B H 0.4640 0.1553 0.5416 0.135 Uiso 1 1 calc R . . H17C H 0.5494 0.1094 0.4974 0.135 Uiso 1 1 calc R . . C18 C 0.8227(4) 0.1646(4) 0.4592(4) 0.0430(12) Uani 1 1 d . . . H18 H 0.8196 0.0955 0.4181 0.052 Uiso 1 1 calc R . . C19 C 0.9426(5) 0.2347(5) 0.4781(5) 0.0607(16) Uani 1 1 d . . . H19A H 0.9560 0.3039 0.5231 0.073 Uiso 1 1 calc R . . H19B H 0.9446 0.2435 0.4186 0.073 Uiso 1 1 calc R . . C20 C 1.0396(5) 0.1858(6) 0.5195(5) 0.0675(17) Uani 1 1 d . . . H20A H 1.0328 0.1222 0.4701 0.081 Uiso 1 1 calc R . . H20B H 1.1162 0.2350 0.5372 0.081 Uiso 1 1 calc R . . C21 C 1.0343(5) 0.1584(6) 0.6056(5) 0.0735(19) Uani 1 1 d . . . H21A H 1.0903 0.1184 0.6227 0.088 Uiso 1 1 calc R . . H21B H 1.0578 0.2230 0.6595 0.088 Uiso 1 1 calc R . . C22 C 0.9142(6) 0.0955(6) 0.5888(5) 0.0711(18) Uani 1 1 d . . . H22A H 0.9131 0.0882 0.6491 0.085 Uiso 1 1 calc R . . H22B H 0.8973 0.0252 0.5442 0.085 Uiso 1 1 calc R . . C23 C 0.8171(5) 0.1452(6) 0.5486(5) 0.0679(18) Uani 1 1 d . . . H23A H 0.7402 0.0984 0.5339 0.082 Uiso 1 1 calc R . . H23B H 0.8273 0.2116 0.5963 0.082 Uiso 1 1 calc R . . C24 C 0.1300(5) -0.0351(5) 0.1019(5) 0.078(2) Uani 1 1 d . . . H24A H 0.0853 -0.0127 0.1397 0.117 Uiso 1 1 calc R . . H24B H 0.1022 -0.1105 0.0719 0.117 Uiso 1 1 calc R . . H24C H 0.1201 -0.0022 0.0532 0.117 Uiso 1 1 calc R . . C25 C 0.3662(6) -0.0569(5) 0.1034(5) 0.0660(17) Uani 1 1 d . . . H25A H 0.3402 -0.0433 0.0436 0.099 Uiso 1 1 calc R . . H25B H 0.3469 -0.1318 0.0911 0.099 Uiso 1 1 calc R . . H25C H 0.4504 -0.0268 0.1358 0.099 Uiso 1 1 calc R . . C26 C 0.3021(6) -0.0622(5) 0.2734(5) 0.0758(19) Uani 1 1 d . . . H26A H 0.3841 -0.0523 0.3101 0.114 Uiso 1 1 calc R . . H26B H 0.2628 -0.1364 0.2422 0.114 Uiso 1 1 calc R . . H26C H 0.2654 -0.0321 0.3156 0.114 Uiso 1 1 calc R . . C27 C 0.1883(6) 0.1750(6) 0.3406(5) 0.077(2) Uani 1 1 d . . . H27A H 0.1269 0.1107 0.3003 0.115 Uiso 1 1 calc R . . H27B H 0.1536 0.2286 0.3636 0.115 Uiso 1 1 calc R . . H27C H 0.2415 0.1627 0.3943 0.115 Uiso 1 1 calc R . . C28 C 0.1649(5) 0.2485(5) 0.1701(5) 0.0727(18) Uani 1 1 d . . . H28A H 0.2082 0.2940 0.1469 0.109 Uiso 1 1 calc R . . H28B H 0.1137 0.2829 0.1937 0.109 Uiso 1 1 calc R . . H28C H 0.1183 0.1836 0.1187 0.109 Uiso 1 1 calc R . . C29 C 0.3847(5) 0.3492(5) 0.3515(4) 0.0601(15) Uani 1 1 d . . . H29A H 0.4423 0.3378 0.4032 0.090 Uiso 1 1 calc R . . H29B H 0.3459 0.3974 0.3772 0.090 Uiso 1 1 calc R . . H29C H 0.4235 0.3786 0.3154 0.090 Uiso 1 1 calc R . . C30 C 0.6045(8) 0.5952(5) 0.2148(5) 0.089(2) Uani 1 1 d . . . H30A H 0.6227 0.5823 0.1580 0.134 Uiso 1 1 calc R . . H30B H 0.6462 0.6665 0.2568 0.134 Uiso 1 1 calc R . . H30C H 0.5208 0.5853 0.1971 0.134 Uiso 1 1 calc R . . C31 C 0.8111(6) 0.5157(6) 0.3001(6) 0.090(2) Uani 1 1 d . . . H31A H 0.8401 0.4738 0.3384 0.136 Uiso 1 1 calc R . . H31B H 0.8555 0.5886 0.3334 0.136 Uiso 1 1 calc R . . H31C H 0.8201 0.4923 0.2396 0.136 Uiso 1 1 calc R . . C32 C 0.6340(6) 0.5502(5) 0.3961(4) 0.0672(17) Uani 1 1 d . . . H32A H 0.5564 0.5597 0.3849 0.101 Uiso 1 1 calc R . . H32B H 0.6928 0.6165 0.4350 0.101 Uiso 1 1 calc R . . H32C H 0.6443 0.4996 0.4289 0.101 Uiso 1 1 calc R . . C33 C 0.4818(5) 0.1737(4) 0.0634(4) 0.0579(15) Uani 1 1 d . . . H33A H 0.5502 0.1545 0.0963 0.087 Uiso 1 1 calc R . . H33B H 0.4573 0.1407 -0.0048 0.087 Uiso 1 1 calc R . . H33C H 0.4185 0.1504 0.0831 0.087 Uiso 1 1 calc R . . C34 C 0.6264(6) 0.3577(5) 0.0381(5) 0.0715(18) Uani 1 1 d . . . H34A H 0.6488 0.4331 0.0530 0.107 Uiso 1 1 calc R . . H34B H 0.5901 0.3240 -0.0305 0.107 Uiso 1 1 calc R . . H34C H 0.6956 0.3354 0.0630 0.107 Uiso 1 1 calc R . . C35 C 0.3818(6) 0.3530(6) 0.0337(5) 0.077(2) Uani 1 1 d . . . H35A H 0.3231 0.3309 0.0582 0.116 Uiso 1 1 calc R . . H35B H 0.3525 0.3171 -0.0345 0.116 Uiso 1 1 calc R . . H35C H 0.3988 0.4280 0.0463 0.116 Uiso 1 1 calc R . . C36 C 1.043(5) 0.334(4) 0.861(4) 0.220(7) Uiso 0.50 1 d PD . . C37 C 0.975(3) 0.356(3) 0.925(3) 0.220(7) Uiso 0.50 1 d PD . . C38 C 1.035(3) 0.471(3) 0.936(2) 0.220(7) Uiso 0.50 1 d PD . . C39 C 1.006(4) 0.540(3) 1.011(3) 0.220(7) Uiso 0.50 1 d PD . . C40 C 0.938(3) 0.607(3) 1.053(3) 0.220(7) Uiso 0.50 1 d PD . . C41 C 0.970(5) 0.695(4) 1.143(4) 0.220(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 Y1 0.0340(3) 0.0419(3) 0.0414(3) 0.0191(2) 0.0126(2) 0.0123(2) Si1 0.0435(8) 0.0471(9) 0.0564(10) 0.0170(7) 0.0199(7) 0.0081(7) Si2 0.0418(8) 0.0561(9) 0.0564(10) 0.0176(8) 0.0236(7) 0.0160(7) Si3 0.0610(10) 0.0402(8) 0.0582(10) 0.0169(7) 0.0212(8) 0.0081(8) Si4 0.0589(10) 0.0514(9) 0.0441(9) 0.0225(7) 0.0192(7) 0.0152(8) N1 0.044(2) 0.041(2) 0.037(2) 0.0104(19) 0.0138(19) 0.014(2) N2 0.045(2) 0.043(2) 0.040(2) 0.0142(19) 0.014(2) 0.017(2) N3 0.036(2) 0.044(2) 0.042(2) 0.0122(19) 0.0168(19) 0.0112(19) N4 0.050(3) 0.039(2) 0.043(3) 0.0180(19) 0.015(2) 0.010(2) C1 0.037(3) 0.038(3) 0.050(3) 0.020(2) 0.018(2) 0.011(2) C2 0.035(3) 0.054(3) 0.033(3) 0.012(2) 0.007(2) 0.017(2) C3 0.039(3) 0.071(4) 0.047(3) 0.023(3) 0.017(3) 0.024(3) C4 0.054(4) 0.094(5) 0.054(4) 0.021(3) 0.027(3) 0.035(4) C5 0.076(5) 0.088(5) 0.060(4) 0.006(4) 0.024(4) 0.045(4) C6 0.072(4) 0.048(3) 0.062(4) 0.002(3) 0.009(3) 0.029(3) C7 0.043(3) 0.041(3) 0.047(3) 0.009(2) 0.003(2) 0.011(2) C8 0.064(4) 0.084(5) 0.085(5) 0.045(4) 0.038(4) 0.026(4) C9 0.069(4) 0.053(4) 0.079(5) 0.028(3) 0.023(4) 0.011(3) C10 0.101(3) 0.091(2) 0.0556(18) 0.0196(14) 0.0201(16) 0.061(2) C11 0.101(3) 0.091(2) 0.0556(18) 0.0196(14) 0.0201(16) 0.061(2) C12 0.101(3) 0.091(2) 0.0556(18) 0.0196(14) 0.0201(16) 0.061(2) C13 0.101(3) 0.091(2) 0.0556(18) 0.0196(14) 0.0201(16) 0.061(2) C14 0.101(3) 0.091(2) 0.0556(18) 0.0196(14) 0.0201(16) 0.061(2) C15 0.101(3) 0.091(2) 0.0556(18) 0.0196(14) 0.0201(16) 0.061(2) C16 0.073(5) 0.060(4) 0.113(6) 0.017(4) -0.008(4) 0.026(4) C17 0.077(5) 0.137(7) 0.092(6) 0.067(5) 0.046(4) 0.046(5) C18 0.042(3) 0.043(3) 0.046(3) 0.016(2) 0.014(2) 0.018(2) C19 0.047(3) 0.065(4) 0.071(4) 0.038(3) 0.011(3) 0.015(3) C20 0.045(3) 0.087(5) 0.076(4) 0.037(4) 0.018(3) 0.030(3) C21 0.057(4) 0.100(5) 0.070(4) 0.040(4) 0.013(3) 0.044(4) C22 0.071(4) 0.085(5) 0.079(5) 0.050(4) 0.030(4) 0.040(4) C23 0.057(4) 0.099(5) 0.080(5) 0.061(4) 0.033(3) 0.042(4) C24 0.048(4) 0.067(4) 0.089(5) 0.007(4) 0.009(3) 0.002(3) C25 0.074(4) 0.051(4) 0.074(4) 0.014(3) 0.035(4) 0.017(3) C26 0.081(5) 0.070(4) 0.093(5) 0.043(4) 0.043(4) 0.021(4) C27 0.070(4) 0.090(5) 0.084(5) 0.026(4) 0.050(4) 0.022(4) C28 0.058(4) 0.081(5) 0.081(5) 0.030(4) 0.019(3) 0.033(4) C29 0.053(3) 0.061(4) 0.067(4) 0.012(3) 0.029(3) 0.018(3) C30 0.135(7) 0.055(4) 0.090(5) 0.040(4) 0.045(5) 0.030(4) C31 0.061(4) 0.069(5) 0.104(6) 0.000(4) 0.022(4) -0.010(4) C32 0.070(4) 0.055(4) 0.058(4) 0.005(3) 0.017(3) 0.008(3) C33 0.072(4) 0.051(3) 0.049(3) 0.014(3) 0.024(3) 0.013(3) C34 0.090(5) 0.077(4) 0.070(4) 0.037(4) 0.047(4) 0.026(4) C35 0.082(5) 0.092(5) 0.060(4) 0.037(4) 0.015(4) 0.036(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 N3 2.232(4) . ? Y1 N4 2.235(4) . ? Y1 N1 2.311(4) . ? Y1 N2 2.338(4) . ? Y1 C1 2.785(5) . ? Y1 Si2 3.190(2) . ? Y1 Si4 3.216(2) . ? Si1 N3 1.714(4) . ? Si1 C26 1.862(6) . ? Si1 C24 1.870(6) . ? Si1 C25 1.875(6) . ? Si2 N3 1.712(4) . ? Si2 C27 1.860(6) . ? Si2 C28 1.876(6) . ? Si2 C29 1.886(6) . ? Si3 N4 1.722(4) . ? Si3 C30 1.867(6) . ? Si3 C31 1.872(7) . ? Si3 C32 1.876(6) . ? Si4 N4 1.699(4) . ? Si4 C35 1.857(6) . ? Si4 C34 1.863(6) . ? Si4 C33 1.868(6) . ? N1 C1 1.336(6) . ? N1 C2 1.441(6) . ? N2 C1 1.337(6) . ? N2 C10 1.407(8) . ? C1 C18 1.524(7) . ? C2 C7 1.406(7) . ? C2 C3 1.408(7) . ? C3 C4 1.371(8) . ? C3 C8 1.501(8) . ? C4 C5 1.372(9) . ? C4 H4 0.9300 . ? C5 C6 1.361(9) . ? C5 H5 0.9300 . ? C6 C7 1.384(8) . ? C6 H6 0.9300 . ? C7 C9 1.512(8) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.402(11) . ? C10 C15 1.413(11) . ? C11 C12 1.406(9) . ? C11 C16 1.496(11) . ? C12 C13 1.339(10) . ? C12 H12 0.9300 . ? C13 C14 1.352(10) . ? C13 H13 0.9300 . ? C14 C15 1.382(9) . ? C14 H14 0.9300 . ? C15 C17 1.507(10) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C23 1.499(7) . ? C18 C19 1.512(7) . ? C18 H18 0.9800 . ? C19 C20 1.523(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.497(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.485(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.526(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C41 0.38(10) 2_767 ? C36 C40 1.30(6) 2_767 ? C36 C37 1.51(2) . ? C37 C40 1.01(5) 2_767 ? C37 C39 1.43(5) 2_767 ? C37 C41 1.52(6) 2_767 ? C37 C38 1.549(19) . ? C38 C39 1.11(5) 2_767 ? C38 C40 1.20(5) 2_767 ? C38 C39 1.484(19) . ? C39 C39 1.03(7) 2_767 ? C39 C38 1.11(5) 2_767 ? C39 C37 1.43(5) 2_767 ? C39 C40 1.501(19) . ? C40 C37 1.01(5) 2_767 ? C40 C38 1.20(5) 2_767 ? C40 C36 1.30(6) 2_767 ? C40 C41 1.48(2) . ? C41 C36 0.38(10) 2_767 ? C41 C37 1.52(6) 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 N3 Y1 N4 122.70(15) . . ? N3 Y1 N1 114.64(15) . . ? N4 Y1 N1 114.46(15) . . ? N3 Y1 N2 114.71(15) . . ? N4 Y1 N2 115.80(15) . . ? N1 Y1 N2 57.07(14) . . ? N3 Y1 C1 117.67(15) . . ? N4 Y1 C1 119.61(15) . . ? N1 Y1 C1 28.50(14) . . ? N2 Y1 C1 28.59(14) . . ? N3 Y1 Si2 30.85(11) . . ? N4 Y1 Si2 105.00(11) . . ? N1 Y1 Si2 140.19(11) . . ? N2 Y1 Si2 110.15(11) . . ? C1 Y1 Si2 128.74(11) . . ? N3 Y1 Si4 104.64(11) . . ? N4 Y1 Si4 29.98(11) . . ? N1 Y1 Si4 109.84(11) . . ? N2 Y1 Si4 140.48(11) . . ? C1 Y1 Si4 129.76(11) . . ? Si2 Y1 Si4 101.49(4) . . ? N3 Si1 C26 111.9(3) . . ? N3 Si1 C24 112.9(3) . . ? C26 Si1 C24 106.9(3) . . ? N3 Si1 C25 111.9(2) . . ? C26 Si1 C25 106.9(3) . . ? C24 Si1 C25 105.9(3) . . ? N3 Si2 C27 115.8(3) . . ? N3 Si2 C28 113.8(3) . . ? C27 Si2 C28 107.5(3) . . ? N3 Si2 C29 105.5(2) . . ? C27 Si2 C29 107.1(3) . . ? C28 Si2 C29 106.6(3) . . ? N3 Si2 Y1 41.94(14) . . ? C27 Si2 Y1 135.6(2) . . ? C28 Si2 Y1 116.7(2) . . ? C29 Si2 Y1 64.54(18) . . ? N4 Si3 C30 114.1(3) . . ? N4 Si3 C31 109.7(3) . . ? C30 Si3 C31 107.2(4) . . ? N4 Si3 C32 111.8(3) . . ? C30 Si3 C32 104.5(3) . . ? C31 Si3 C32 109.3(3) . . ? N4 Si4 C35 112.7(3) . . ? N4 Si4 C34 115.9(3) . . ? C35 Si4 C34 107.5(3) . . ? N4 Si4 C33 105.7(2) . . ? C35 Si4 C33 107.4(3) . . ? C34 Si4 C33 107.2(3) . . ? N4 Si4 Y1 41.09(14) . . ? C35 Si4 Y1 117.4(2) . . ? C34 Si4 Y1 134.8(2) . . ? C33 Si4 Y1 65.35(18) . . ? C1 N1 C2 122.0(4) . . ? C1 N1 Y1 95.9(3) . . ? C2 N1 Y1 142.1(3) . . ? C1 N2 C10 123.8(4) . . ? C1 N2 Y1 94.6(3) . . ? C10 N2 Y1 141.2(4) . . ? Si2 N3 Si1 121.7(2) . . ? Si2 N3 Y1 107.2(2) . . ? Si1 N3 Y1 130.9(2) . . ? Si4 N4 Si3 122.1(2) . . ? Si4 N4 Y1 108.9(2) . . ? Si3 N4 Y1 128.6(2) . . ? N1 C1 N2 112.4(4) . . ? N1 C1 C18 120.8(4) . . ? N2 C1 C18 126.8(5) . . ? N1 C1 Y1 55.6(2) . . ? N2 C1 Y1 56.8(2) . . ? C18 C1 Y1 176.4(4) . . ? C7 C2 C3 119.8(5) . . ? C7 C2 N1 121.5(5) . . ? C3 C2 N1 118.6(5) . . ? C4 C3 C2 118.4(6) . . ? C4 C3 C8 120.4(6) . . ? C2 C3 C8 121.2(5) . . ? C3 C4 C5 122.1(6) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 119.4(6) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 121.6(6) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C6 C7 C2 118.7(6) . . ? C6 C7 C9 119.7(6) . . ? C2 C7 C9 121.6(5) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 N2 123.1(7) . . ? C11 C10 C15 117.8(7) . . ? N2 C10 C15 119.0(7) . . ? C10 C11 C12 120.0(8) . . ? C10 C11 C16 120.3(6) . . ? C12 C11 C16 119.7(8) . . ? C13 C12 C11 118.8(8) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 123.9(7) . . ? C12 C13 H13 118.0 . . ? C14 C13 H13 118.0 . . ? C13 C14 C15 118.7(8) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C14 C15 C10 120.7(8) . . ? C14 C15 C17 119.0(8) . . ? C10 C15 C17 120.2(6) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 111.5(5) . . ? C23 C18 C1 118.8(4) . . ? C19 C18 C1 112.6(4) . . ? C23 C18 H18 104.1 . . ? C19 C18 H18 104.1 . . ? C1 C18 H18 104.1 . . ? C18 C19 C20 110.0(5) . . ? C18 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? C18 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C21 C20 C19 113.2(5) . . ? C21 C20 H20A 108.9 . . ? C19 C20 H20A 108.9 . . ? C21 C20 H20B 108.9 . . ? C19 C20 H20B 108.9 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C20 112.5(5) . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? C20 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C21 C22 C23 113.0(5) . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C18 C23 C22 110.0(5) . . ? C18 C23 H23A 109.7 . . ? C22 C23 H23A 109.7 . . ? C18 C23 H23B 109.7 . . ? C22 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si3 C30 H30A 109.5 . . ? Si3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si4 C33 H33A 109.5 . . ? Si4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si4 C34 H34A 109.5 . . ? Si4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si4 C35 H35A 109.5 . . ? Si4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C36 C40 111(10) 2_767 2_767 ? C41 C36 C37 85(10) 2_767 . ? C40 C36 C37 41(2) 2_767 . ? C40 C37 C39 74(3) 2_767 2_767 ? C40 C37 C36 58(4) 2_767 . ? C39 C37 C36 123(3) 2_767 . ? C40 C37 C41 68(3) 2_767 2_767 ? C39 C37 C41 137(4) 2_767 2_767 ? C36 C37 C41 14(4) . 2_767 ? C40 C37 C38 51(3) 2_767 . ? C39 C37 C38 44(2) 2_767 . ? C36 C37 C38 80(3) . . ? C41 C37 C38 95(4) 2_767 . ? C39 C38 C40 81(3) 2_767 2_767 ? C39 C38 C39 44(4) 2_767 . ? C40 C38 C39 120(4) 2_767 . ? C39 C38 C37 63(2) 2_767 . ? C40 C38 C37 41(2) 2_767 . ? C39 C38 C37 106(3) . . ? C39 C39 C38 88(4) 2_767 2_767 ? C39 C39 C37 159(6) 2_767 2_767 ? C38 C39 C37 74(3) 2_767 2_767 ? C39 C39 C38 48(3) 2_767 . ? C38 C39 C38 136(4) 2_767 . ? C37 C39 C38 149(4) 2_767 . ? C39 C39 C40 132(6) 2_767 . ? C38 C39 C40 52(3) 2_767 . ? C37 C39 C40 40(2) 2_767 . ? C38 C39 C40 158(4) . . ? C37 C40 C38 89(4) 2_767 2_767 ? C37 C40 C36 81(4) 2_767 2_767 ? C38 C40 C36 104(5) 2_767 2_767 ? C37 C40 C41 73(4) 2_767 . ? C38 C40 C41 115(4) 2_767 . ? C36 C40 C41 14(4) 2_767 . ? C37 C40 C39 66(3) 2_767 . ? C38 C40 C39 47(3) 2_767 . ? C36 C40 C39 134(5) 2_767 . ? C41 C40 C39 134(4) . . ? C36 C41 C40 55(10) 2_767 . ? C36 C41 C37 81(10) 2_767 2_767 ? C40 C41 C37 39(2) . 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 Y1 Si2 N3 130.0(2) . . . . ? N1 Y1 Si2 N3 -42.4(3) . . . . ? N2 Y1 Si2 N3 -104.7(2) . . . . ? C1 Y1 Si2 N3 -79.5(2) . . . . ? Si4 Y1 Si2 N3 99.3(2) . . . . ? N3 Y1 Si2 C27 78.1(4) . . . . ? N4 Y1 Si2 C27 -151.9(3) . . . . ? N1 Y1 Si2 C27 35.7(4) . . . . ? N2 Y1 Si2 C27 -26.6(3) . . . . ? C1 Y1 Si2 C27 -1.4(4) . . . . ? Si4 Y1 Si2 C27 177.4(3) . . . . ? N3 Y1 Si2 C28 -96.6(3) . . . . ? N4 Y1 Si2 C28 33.4(3) . . . . ? N1 Y1 Si2 C28 -138.9(3) . . . . ? N2 Y1 Si2 C28 158.7(3) . . . . ? C1 Y1 Si2 C28 -176.1(3) . . . . ? Si4 Y1 Si2 C28 2.8(2) . . . . ? N3 Y1 Si2 C29 166.9(3) . . . . ? N4 Y1 Si2 C29 -63.1(3) . . . . ? N1 Y1 Si2 C29 124.5(3) . . . . ? N2 Y1 Si2 C29 62.2(2) . . . . ? C1 Y1 Si2 C29 87.4(3) . . . . ? Si4 Y1 Si2 C29 -93.8(2) . . . . ? N3 Y1 Si4 N4 131.7(2) . . . . ? N1 Y1 Si4 N4 -104.8(2) . . . . ? N2 Y1 Si4 N4 -42.9(3) . . . . ? C1 Y1 Si4 N4 -81.0(3) . . . . ? Si2 Y1 Si4 N4 100.1(2) . . . . ? N3 Y1 Si4 C35 37.8(3) . . . . ? N4 Y1 Si4 C35 -93.8(3) . . . . ? N1 Y1 Si4 C35 161.4(3) . . . . ? N2 Y1 Si4 C35 -136.7(3) . . . . ? C1 Y1 Si4 C35 -174.9(3) . . . . ? Si2 Y1 Si4 C35 6.3(3) . . . . ? N3 Y1 Si4 C34 -149.9(3) . . . . ? N4 Y1 Si4 C34 78.4(4) . . . . ? N1 Y1 Si4 C34 -26.4(3) . . . . ? N2 Y1 Si4 C34 35.5(4) . . . . ? C1 Y1 Si4 C34 -2.6(3) . . . . ? Si2 Y1 Si4 C34 178.5(3) . . . . ? N3 Y1 Si4 C33 -59.8(2) . . . . ? N4 Y1 Si4 C33 168.5(3) . . . . ? N1 Y1 Si4 C33 63.7(2) . . . . ? N2 Y1 Si4 C33 125.6(3) . . . . ? C1 Y1 Si4 C33 87.5(3) . . . . ? Si2 Y1 Si4 C33 -91.3(2) . . . . ? N3 Y1 N1 C1 -103.1(3) . . . . ? N4 Y1 N1 C1 107.4(3) . . . . ? N2 Y1 N1 C1 1.5(3) . . . . ? Si2 Y1 N1 C1 -80.7(3) . . . . ? Si4 Y1 N1 C1 139.5(3) . . . . ? N3 Y1 N1 C2 75.6(6) . . . . ? N4 Y1 N1 C2 -73.9(6) . . . . ? N2 Y1 N1 C2 -179.9(6) . . . . ? C1 Y1 N1 C2 178.6(7) . . . . ? Si2 Y1 N1 C2 97.9(5) . . . . ? Si4 Y1 N1 C2 -41.9(6) . . . . ? N3 Y1 N2 C1 102.9(3) . . . . ? N4 Y1 N2 C1 -105.1(3) . . . . ? N1 Y1 N2 C1 -1.5(3) . . . . ? Si2 Y1 N2 C1 136.0(3) . . . . ? Si4 Y1 N2 C1 -82.9(3) . . . . ? N3 Y1 N2 C10 -69.0(7) . . . . ? N4 Y1 N2 C10 83.0(7) . . . . ? N1 Y1 N2 C10 -173.5(8) . . . . ? C1 Y1 N2 C10 -172.0(9) . . . . ? Si2 Y1 N2 C10 -36.0(7) . . . . ? Si4 Y1 N2 C10 105.2(7) . . . . ? C27 Si2 N3 Si1 45.8(4) . . . . ? C28 Si2 N3 Si1 -79.5(4) . . . . ? C29 Si2 N3 Si1 164.0(3) . . . . ? Y1 Si2 N3 Si1 176.3(4) . . . . ? C27 Si2 N3 Y1 -130.5(3) . . . . ? C28 Si2 N3 Y1 104.2(3) . . . . ? C29 Si2 N3 Y1 -12.3(3) . . . . ? C26 Si1 N3 Si2 -83.5(4) . . . . ? C24 Si1 N3 Si2 37.1(4) . . . . ? C25 Si1 N3 Si2 156.4(3) . . . . ? C26 Si1 N3 Y1 91.8(4) . . . . ? C24 Si1 N3 Y1 -147.6(3) . . . . ? C25 Si1 N3 Y1 -28.2(4) . . . . ? N4 Y1 N3 Si2 -61.6(3) . . . . ? N1 Y1 N3 Si2 151.67(18) . . . . ? N2 Y1 N3 Si2 88.2(2) . . . . ? C1 Y1 N3 Si2 120.0(2) . . . . ? Si4 Y1 N3 Si2 -87.96(19) . . . . ? N4 Y1 N3 Si1 122.5(3) . . . . ? N1 Y1 N3 Si1 -24.2(3) . . . . ? N2 Y1 N3 Si1 -87.6(3) . . . . ? C1 Y1 N3 Si1 -55.8(3) . . . . ? Si2 Y1 N3 Si1 -175.8(4) . . . . ? Si4 Y1 N3 Si1 96.2(3) . . . . ? C35 Si4 N4 Si3 -80.2(4) . . . . ? C34 Si4 N4 Si3 44.2(4) . . . . ? C33 Si4 N4 Si3 162.7(3) . . . . ? Y1 Si4 N4 Si3 173.6(4) . . . . ? C35 Si4 N4 Y1 106.2(3) . . . . ? C34 Si4 N4 Y1 -129.4(3) . . . . ? C33 Si4 N4 Y1 -10.8(3) . . . . ? C30 Si3 N4 Si4 35.1(4) . . . . ? C31 Si3 N4 Si4 -85.2(4) . . . . ? C32 Si3 N4 Si4 153.4(3) . . . . ? C30 Si3 N4 Y1 -152.7(3) . . . . ? C31 Si3 N4 Y1 87.0(4) . . . . ? C32 Si3 N4 Y1 -34.4(4) . . . . ? N3 Y1 N4 Si4 -59.2(3) . . . . ? N1 Y1 N4 Si4 87.6(2) . . . . ? N2 Y1 N4 Si4 151.25(19) . . . . ? C1 Y1 N4 Si4 119.1(2) . . . . ? Si2 Y1 N4 Si4 -87.0(2) . . . . ? N3 Y1 N4 Si3 127.8(3) . . . . ? N1 Y1 N4 Si3 -85.5(3) . . . . ? N2 Y1 N4 Si3 -21.8(3) . . . . ? C1 Y1 N4 Si3 -53.9(3) . . . . ? Si2 Y1 N4 Si3 99.9(3) . . . . ? Si4 Y1 N4 Si3 -173.0(5) . . . . ? C2 N1 C1 N2 178.6(4) . . . . ? Y1 N1 C1 N2 -2.3(4) . . . . ? C2 N1 C1 C18 0.0(7) . . . . ? Y1 N1 C1 C18 179.0(4) . . . . ? C2 N1 C1 Y1 -179.0(5) . . . . ? C10 N2 C1 N1 176.3(6) . . . . ? Y1 N2 C1 N1 2.3(4) . . . . ? C10 N2 C1 C18 -5.2(9) . . . . ? Y1 N2 C1 C18 -179.1(4) . . . . ? C10 N2 C1 Y1 174.0(6) . . . . ? N3 Y1 C1 N1 91.2(3) . . . . ? N4 Y1 C1 N1 -87.2(3) . . . . ? N2 Y1 C1 N1 -177.4(5) . . . . ? Si2 Y1 C1 N1 125.9(3) . . . . ? Si4 Y1 C1 N1 -52.6(3) . . . . ? N3 Y1 C1 N2 -91.4(3) . . . . ? N4 Y1 C1 N2 90.2(3) . . . . ? N1 Y1 C1 N2 177.4(5) . . . . ? Si2 Y1 C1 N2 -56.7(3) . . . . ? Si4 Y1 C1 N2 124.8(3) . . . . ? N3 Y1 C1 C18 78(5) . . . . ? N4 Y1 C1 C18 -101(5) . . . . ? N1 Y1 C1 C18 -13(5) . . . . ? N2 Y1 C1 C18 169(5) . . . . ? Si2 Y1 C1 C18 113(5) . . . . ? Si4 Y1 C1 C18 -66(5) . . . . ? C1 N1 C2 C7 77.0(6) . . . . ? Y1 N1 C2 C7 -101.4(6) . . . . ? C1 N1 C2 C3 -105.8(5) . . . . ? Y1 N1 C2 C3 75.7(7) . . . . ? C7 C2 C3 C4 -0.4(7) . . . . ? N1 C2 C3 C4 -177.6(5) . . . . ? C7 C2 C3 C8 179.6(5) . . . . ? N1 C2 C3 C8 2.4(7) . . . . ? C2 C3 C4 C5 -0.1(9) . . . . ? C8 C3 C4 C5 179.8(6) . . . . ? C3 C4 C5 C6 0.6(10) . . . . ? C4 C5 C6 C7 -0.4(10) . . . . ? C5 C6 C7 C2 -0.1(9) . . . . ? C5 C6 C7 C9 -179.7(6) . . . . ? C3 C2 C7 C6 0.5(7) . . . . ? N1 C2 C7 C6 177.6(5) . . . . ? C3 C2 C7 C9 -179.8(5) . . . . ? N1 C2 C7 C9 -2.7(7) . . . . ? C1 N2 C10 C11 87.6(8) . . . . ? Y1 N2 C10 C11 -102.0(8) . . . . ? C1 N2 C10 C15 -96.5(7) . . . . ? Y1 N2 C10 C15 73.9(9) . . . . ? N2 C10 C11 C12 178.7(5) . . . . ? C15 C10 C11 C12 2.7(9) . . . . ? N2 C10 C11 C16 -1.1(10) . . . . ? C15 C10 C11 C16 -177.0(6) . . . . ? C10 C11 C12 C13 -1.2(10) . . . . ? C16 C11 C12 C13 178.5(6) . . . . ? C11 C12 C13 C14 -1.5(10) . . . . ? C12 C13 C14 C15 2.6(10) . . . . ? C13 C14 C15 C10 -0.9(10) . . . . ? C13 C14 C15 C17 177.8(6) . . . . ? C11 C10 C15 C14 -1.7(10) . . . . ? N2 C10 C15 C14 -177.8(5) . . . . ? C11 C10 C15 C17 179.6(6) . . . . ? N2 C10 C15 C17 3.5(9) . . . . ? N1 C1 C18 C23 -138.9(5) . . . . ? N2 C1 C18 C23 42.6(8) . . . . ? Y1 C1 C18 C23 -126(5) . . . . ? N1 C1 C18 C19 88.2(6) . . . . ? N2 C1 C18 C19 -90.2(6) . . . . ? Y1 C1 C18 C19 101(5) . . . . ? C23 C18 C19 C20 57.0(7) . . . . ? C1 C18 C19 C20 -166.6(5) . . . . ? C18 C19 C20 C21 -52.9(8) . . . . ? C19 C20 C21 C22 50.5(8) . . . . ? C20 C21 C22 C23 -51.1(8) . . . . ? C19 C18 C23 C22 -57.7(7) . . . . ? C1 C18 C23 C22 169.0(5) . . . . ? C21 C22 C23 C18 54.6(8) . . . . ? C41 C36 C37 C40 131(21) 2_767 . . 2_767 ? C41 C36 C37 C39 169(18) 2_767 . . 2_767 ? C40 C36 C37 C39 38(5) 2_767 . . 2_767 ? C40 C36 C37 C41 -131(21) 2_767 . . 2_767 ? C41 C36 C37 C38 -179(19) 2_767 . . . ? C40 C36 C37 C38 49(3) 2_767 . . . ? C40 C37 C38 C39 -109(5) 2_767 . . 2_767 ? C36 C37 C38 C39 -166(5) . . . 2_767 ? C41 C37 C38 C39 -166(5) 2_767 . . 2_767 ? C39 C37 C38 C40 109(5) 2_767 . . 2_767 ? C36 C37 C38 C40 -56(4) . . . 2_767 ? C41 C37 C38 C40 -56(4) 2_767 . . 2_767 ? C40 C37 C38 C39 -117(5) 2_767 . . . ? C39 C37 C38 C39 -8(5) 2_767 . . . ? C36 C37 C38 C39 -174(4) . . . . ? C41 C37 C38 C39 -174(4) 2_767 . . . ? C40 C38 C39 C39 -32(7) 2_767 . . 2_767 ? C37 C38 C39 C39 10(6) . . . 2_767 ? C39 C38 C39 C38 0.000(8) 2_767 . . 2_767 ? C40 C38 C39 C38 -32(7) 2_767 . . 2_767 ? C37 C38 C39 C38 10(6) . . . 2_767 ? C39 C38 C39 C37 160(12) 2_767 . . 2_767 ? C40 C38 C39 C37 128(7) 2_767 . . 2_767 ? C37 C38 C39 C37 170(6) . . . 2_767 ? C39 C38 C39 C40 -102(13) 2_767 . . . ? C40 C38 C39 C40 -134(9) 2_767 . . . ? C37 C38 C39 C40 -92(11) . . . . ? C39 C39 C40 C37 151(9) 2_767 . . 2_767 ? C38 C39 C40 C37 112(5) 2_767 . . 2_767 ? C38 C39 C40 C37 -127(11) . . . 2_767 ? C39 C39 C40 C38 39(8) 2_767 . . 2_767 ? C37 C39 C40 C38 -112(5) 2_767 . . 2_767 ? C38 C39 C40 C38 121(11) . . . 2_767 ? C39 C39 C40 C36 103(10) 2_767 . . 2_767 ? C38 C39 C40 C36 64(6) 2_767 . . 2_767 ? C37 C39 C40 C36 -48(5) 2_767 . . 2_767 ? C38 C39 C40 C36 -175(9) . . . 2_767 ? C39 C39 C40 C41 122(9) 2_767 . . . ? C38 C39 C40 C41 84(6) 2_767 . . . ? C37 C39 C40 C41 -28(5) 2_767 . . . ? C38 C39 C40 C41 -156(8) . . . . ? C37 C40 C41 C36 -124(21) 2_767 . . 2_767 ? C38 C40 C41 C36 -44(21) 2_767 . . 2_767 ? C39 C40 C41 C36 -97(20) . . . 2_767 ? C38 C40 C41 C37 80(4) 2_767 . . 2_767 ? C36 C40 C41 C37 124(21) 2_767 . . 2_767 ? C39 C40 C41 C37 27(5) . . . 2_767 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.017 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.073 data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 792826' #TrackingRef 'data.doc' #TrackingRef 'data.doc' #TrackingRef 'data.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H89 Cl Li Lu N4 O3 Si4' _chemical_formula_sum 'C47 H89 Cl Li Lu N4 O3 Si4' _chemical_formula_weight 1087.94 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _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 12.3218(12) _cell_length_b 13.9301(13) _cell_length_c 18.273(2) _cell_angle_alpha 77.021(8) _cell_angle_beta 81.070(8) _cell_angle_gamma 71.718(7) _cell_volume 2889.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8869 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 1.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.315 _exptl_absorpt_correction_T_max 0.521 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27674 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.35 _reflns_number_total 10502 _reflns_number_gt 8932 _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^)+(0.0697P)^2^+3.1846P] 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 10502 _refine_ls_number_parameters 529 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1490 _refine_ls_wR_factor_gt 0.1367 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.79873(2) 0.704938(19) 0.739753(14) 0.04191(11) Uani 1 1 d . . . Cl1 Cl 0.74415(18) 0.89715(13) 0.75218(11) 0.0648(5) Uani 1 1 d . A . Si1 Si 0.6793(2) 0.70854(17) 0.92441(11) 0.0597(5) Uani 1 1 d . . . Si2 Si 0.63982(19) 0.55804(17) 0.84730(12) 0.0600(5) Uani 1 1 d . . . Si3 Si 0.58207(19) 0.82400(17) 0.62695(12) 0.0631(5) Uani 1 1 d . . . Si4 Si 0.7814(2) 0.70022(18) 0.54783(11) 0.0645(6) Uani 1 1 d . . . O1 O 0.7611(13) 1.0894(12) 0.8384(9) 0.086(5) Uiso 0.50 1 d PD A 1 O1' O 0.7517(12) 1.0650(11) 0.8631(9) 0.081(5) Uiso 0.50 1 d PD A 2 O2 O 0.5078(15) 1.1092(13) 0.7970(9) 0.083(3) Uiso 0.50 1 d PD A 1 O2' O 0.5210(15) 1.1312(13) 0.7887(9) 0.083(3) Uiso 0.50 1 d PD A 2 O3 O 0.7404(12) 1.1547(11) 0.6917(8) 0.082(2) Uiso 0.50 1 d PD A 1 O3' O 0.7033(12) 1.1581(11) 0.6739(8) 0.082(2) Uiso 0.50 1 d PD A 2 N1 N 0.9860(5) 0.7116(4) 0.7354(3) 0.0517(14) Uani 1 1 d . . . N2 N 0.9617(4) 0.5569(4) 0.7488(3) 0.0415(12) Uani 1 1 d . . . N3 N 0.7038(4) 0.6521(4) 0.8464(3) 0.0454(12) Uani 1 1 d . . . N4 N 0.7200(5) 0.7407(4) 0.6312(3) 0.0487(13) Uani 1 1 d . . . C1 C 1.0368(6) 0.6115(5) 0.7399(3) 0.0491(16) Uani 1 1 d . . . C2 C 1.0467(6) 0.7860(6) 0.7306(5) 0.063(2) Uani 1 1 d . . . C3 C 1.0420(7) 0.8632(7) 0.6647(7) 0.088(3) Uani 1 1 d . . . C4 C 1.0963(9) 0.9384(8) 0.6611(8) 0.109(4) Uani 1 1 d . . . H4 H 1.0924 0.9899 0.6184 0.131 Uiso 1 1 calc R . . C5 C 1.1539(11) 0.9382(10) 0.7178(10) 0.127(5) Uani 1 1 d . . . H5 H 1.1909 0.9882 0.7135 0.152 Uiso 1 1 calc R . . C6 C 1.1583(8) 0.8656(9) 0.7810(9) 0.113(4) Uani 1 1 d . . . H6 H 1.1983 0.8671 0.8197 0.135 Uiso 1 1 calc R . . C7 C 1.1041(6) 0.7872(7) 0.7906(6) 0.080(3) Uani 1 1 d . . . C8 C 0.9778(9) 0.8656(7) 0.6009(6) 0.093(3) Uani 1 1 d . . . H8A H 0.9785 0.9257 0.5630 0.140 Uiso 1 1 calc R . . H8B H 0.8999 0.8676 0.6192 0.140 Uiso 1 1 calc R . . H8C H 1.0138 0.8051 0.5794 0.140 Uiso 1 1 calc R . . C9 C 1.1081(9) 0.7106(9) 0.8640(6) 0.096(3) Uani 1 1 d . . . H9A H 1.0611 0.6673 0.8634 0.145 Uiso 1 1 calc R . . H9B H 1.0797 0.7468 0.9052 0.145 Uiso 1 1 calc R . . H9C H 1.1858 0.6690 0.8702 0.145 Uiso 1 1 calc R . . C10 C 0.9890(5) 0.4492(5) 0.7761(4) 0.0459(15) Uani 1 1 d . . . C11 C 0.9989(6) 0.4098(5) 0.8530(4) 0.0549(17) Uani 1 1 d . . . C12 C 1.0208(7) 0.3058(6) 0.8803(5) 0.072(2) Uani 1 1 d . . . H12 H 1.0282 0.2808 0.9315 0.086 Uiso 1 1 calc R . . C13 C 1.0319(8) 0.2389(6) 0.8336(6) 0.083(3) Uani 1 1 d . . . H13 H 1.0485 0.1686 0.8525 0.100 Uiso 1 1 calc R . . C14 C 1.0187(7) 0.2754(6) 0.7595(5) 0.069(2) Uani 1 1 d . . . H14 H 1.0242 0.2297 0.7281 0.082 Uiso 1 1 calc R . . C15 C 0.9966(6) 0.3810(5) 0.7288(4) 0.0542(17) Uani 1 1 d . . . C16 C 0.9837(7) 0.4805(6) 0.9070(4) 0.069(2) Uani 1 1 d . . . H16A H 1.0507 0.5037 0.9015 0.103 Uiso 1 1 calc R . . H16B H 0.9731 0.4444 0.9577 0.103 Uiso 1 1 calc R . . H16C H 0.9177 0.5387 0.8965 0.103 Uiso 1 1 calc R . . C17 C 0.9832(8) 0.4161(6) 0.6485(4) 0.073(2) Uani 1 1 d . . . H17A H 0.9162 0.4742 0.6413 0.109 Uiso 1 1 calc R . . H17B H 0.9751 0.3615 0.6278 0.109 Uiso 1 1 calc R . . H17C H 1.0497 0.4358 0.6234 0.109 Uiso 1 1 calc R . . C18 C 1.1669(6) 0.5700(6) 0.7273(4) 0.0595(18) Uani 1 1 d . . . H18 H 1.1968 0.6178 0.7443 0.071 Uiso 1 1 calc R . . C19 C 1.2022(7) 0.5813(8) 0.6429(5) 0.085(3) Uani 1 1 d . . . H19A H 1.1737 0.5362 0.6226 0.101 Uiso 1 1 calc R . . H19B H 1.1669 0.6515 0.6186 0.101 Uiso 1 1 calc R . . C20 C 1.3302(8) 0.5559(9) 0.6247(6) 0.100(3) Uani 1 1 d . . . H20A H 1.3476 0.5543 0.5713 0.120 Uiso 1 1 calc R . . H20B H 1.3558 0.6105 0.6345 0.120 Uiso 1 1 calc R . . C21 C 1.3948(7) 0.4584(8) 0.6670(6) 0.092(3) Uani 1 1 d . . . H21A H 1.4758 0.4535 0.6584 0.110 Uiso 1 1 calc R . . H21B H 1.3837 0.4025 0.6483 0.110 Uiso 1 1 calc R . . C22 C 1.3596(7) 0.4460(8) 0.7503(6) 0.087(3) Uani 1 1 d . . . H22A H 1.3827 0.4942 0.7709 0.104 Uiso 1 1 calc R . . H22B H 1.3985 0.3769 0.7749 0.104 Uiso 1 1 calc R . . C23 C 1.2307(7) 0.4648(7) 0.7665(5) 0.086(3) Uani 1 1 d . . . H23A H 1.2084 0.4131 0.7495 0.103 Uiso 1 1 calc R . . H23B H 1.2102 0.4585 0.8204 0.103 Uiso 1 1 calc R . . C24 C 0.8019(8) 0.7520(7) 0.9345(5) 0.082(3) Uani 1 1 d . . . H24A H 0.8637 0.6936 0.9526 0.123 Uiso 1 1 calc R . . H24B H 0.7790 0.7982 0.9696 0.123 Uiso 1 1 calc R . . H24C H 0.8268 0.7870 0.8864 0.123 Uiso 1 1 calc R . . C25 C 0.6592(11) 0.6210(8) 1.0178(5) 0.107(4) Uani 1 1 d . . . H25A H 0.5950 0.5960 1.0177 0.161 Uiso 1 1 calc R . . H25B H 0.6452 0.6587 1.0579 0.161 Uiso 1 1 calc R . . H25C H 0.7273 0.5639 1.0251 0.161 Uiso 1 1 calc R . . C26 C 0.5490(8) 0.8211(7) 0.9227(5) 0.090(3) Uani 1 1 d . . . H26A H 0.5378 0.8556 0.8715 0.136 Uiso 1 1 calc R . . H26B H 0.5586 0.8679 0.9510 0.136 Uiso 1 1 calc R . . H26C H 0.4834 0.7982 0.9448 0.136 Uiso 1 1 calc R . . C27 C 0.6629(8) 0.5240(7) 0.7520(5) 0.075(2) Uani 1 1 d . . . H27A H 0.6248 0.5826 0.7166 0.113 Uiso 1 1 calc R . . H27B H 0.6321 0.4681 0.7538 0.113 Uiso 1 1 calc R . . H27C H 0.7436 0.5038 0.7364 0.113 Uiso 1 1 calc R . . C28 C 0.6988(9) 0.4327(7) 0.9119(5) 0.090(3) Uani 1 1 d . . . H28A H 0.7762 0.4009 0.8936 0.135 Uiso 1 1 calc R . . H28B H 0.6525 0.3880 0.9135 0.135 Uiso 1 1 calc R . . H28C H 0.6977 0.4450 0.9617 0.135 Uiso 1 1 calc R . . C29 C 0.4805(7) 0.5992(7) 0.8744(5) 0.086(3) Uani 1 1 d . . . H29A H 0.4643 0.6409 0.9123 0.130 Uiso 1 1 calc R . . H29B H 0.4545 0.5395 0.8938 0.130 Uiso 1 1 calc R . . H29C H 0.4416 0.6384 0.8308 0.130 Uiso 1 1 calc R . . C30 C 0.4993(8) 0.8251(8) 0.7217(5) 0.090(3) Uani 1 1 d . . . H30A H 0.4863 0.7592 0.7409 0.136 Uiso 1 1 calc R . . H30B H 0.4269 0.8774 0.7172 0.136 Uiso 1 1 calc R . . H30C H 0.5421 0.8392 0.7555 0.136 Uiso 1 1 calc R . . C31 C 0.4861(8) 0.7901(8) 0.5715(6) 0.097(3) Uani 1 1 d . . . H31A H 0.5178 0.7929 0.5199 0.145 Uiso 1 1 calc R . . H31B H 0.4109 0.8383 0.5738 0.145 Uiso 1 1 calc R . . H31C H 0.4809 0.7219 0.5928 0.145 Uiso 1 1 calc R . . C32 C 0.5830(9) 0.9592(6) 0.5852(5) 0.088(3) Uani 1 1 d . . . H32A H 0.6260 0.9811 0.6145 0.132 Uiso 1 1 calc R . . H32B H 0.5056 1.0036 0.5854 0.132 Uiso 1 1 calc R . . H32C H 0.6180 0.9624 0.5343 0.132 Uiso 1 1 calc R . . C33 C 0.7541(10) 0.8023(9) 0.4604(5) 0.112(4) Uani 1 1 d . . . H33A H 0.6753 0.8192 0.4504 0.169 Uiso 1 1 calc R . . H33B H 0.8033 0.7772 0.4184 0.169 Uiso 1 1 calc R . . H33C H 0.7696 0.8627 0.4677 0.169 Uiso 1 1 calc R . . C34 C 0.7349(9) 0.5928(8) 0.5308(6) 0.098(3) Uani 1 1 d . . . H34A H 0.7628 0.5323 0.5679 0.147 Uiso 1 1 calc R . . H34B H 0.7652 0.5788 0.4814 0.147 Uiso 1 1 calc R . . H34C H 0.6525 0.6118 0.5344 0.147 Uiso 1 1 calc R . . C35 C 0.9413(7) 0.6560(7) 0.5441(4) 0.076(2) Uani 1 1 d . . . H35A H 0.9710 0.7130 0.5218 0.114 Uiso 1 1 calc R . . H35B H 0.9707 0.6031 0.5143 0.114 Uiso 1 1 calc R . . H35C H 0.9643 0.6292 0.5943 0.114 Uiso 1 1 calc R . . C36 C 0.869(2) 1.016(3) 0.8632(15) 0.126(3) Uiso 0.50 1 d PD A 1 C36' C 0.8789(18) 1.029(3) 0.8466(15) 0.126(3) Uiso 0.50 1 d PD A 2 C37 C 0.866(3) 1.020(2) 0.9453(16) 0.126(3) Uiso 0.50 1 d PD A 1 C37' C 0.923(2) 1.004(2) 0.9233(14) 0.126(3) Uiso 0.50 1 d PD A 2 C38 C 0.796(2) 1.128(2) 0.9550(14) 0.126(3) Uiso 0.50 1 d PD A 1 C38' C 0.823(2) 1.067(2) 0.9701(15) 0.126(3) Uiso 0.50 1 d PD A 2 C39 C 0.737(2) 1.1672(18) 0.8856(13) 0.126(3) Uiso 0.50 1 d PD A 1 C39' C 0.715(2) 1.101(2) 0.9316(12) 0.126(3) Uiso 0.50 1 d PD A 2 C40 C 0.456(2) 1.138(2) 0.8683(14) 0.112(3) Uiso 0.50 1 d PD A 1 C40' C 0.448(2) 1.114(2) 0.8604(13) 0.112(3) Uiso 0.50 1 d PD A 2 C41 C 0.3344(19) 1.1542(19) 0.8561(13) 0.112(3) Uiso 0.50 1 d PD A 1 C41' C 0.339(2) 1.095(2) 0.8521(13) 0.112(3) Uiso 0.50 1 d PD A 2 C42 C 0.340(2) 1.0851(19) 0.8019(14) 0.112(3) Uiso 0.50 1 d PD A 1 C42' C 0.3318(19) 1.141(2) 0.7670(12) 0.112(3) Uiso 0.50 1 d PD A 2 C43 C 0.431(2) 1.114(2) 0.7447(13) 0.112(3) Uiso 0.50 1 d PD A 1 C43' C 0.4481(19) 1.148(2) 0.7297(13) 0.112(3) Uiso 0.50 1 d PD A 2 C44 C 0.745(3) 1.2608(18) 0.6669(17) 0.148(4) Uiso 0.50 1 d PD A 1 C44' C 0.687(3) 1.2666(17) 0.6806(16) 0.148(4) Uiso 0.50 1 d PD A 2 C45 C 0.693(3) 1.292(2) 0.5934(16) 0.148(4) Uiso 0.50 1 d PD A 1 C45' C 0.745(3) 1.313(2) 0.6057(16) 0.148(4) Uiso 0.50 1 d PD A 2 C46 C 0.749(3) 1.205(2) 0.5539(16) 0.148(4) Uiso 0.50 1 d PD A 1 C46' C 0.810(3) 1.222(2) 0.5726(18) 0.148(4) Uiso 0.50 1 d PD A 2 C47 C 0.804(2) 1.130(2) 0.6206(12) 0.148(4) Uiso 0.50 1 d PD A 1 C47' C 0.754(3) 1.134(2) 0.6016(14) 0.148(4) Uiso 0.50 1 d PD A 2 Li1 Li 0.6811(14) 1.0690(11) 0.7705(9) 0.079(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.04385(18) 0.04358(18) 0.03659(16) -0.00683(11) -0.00226(11) -0.01143(13) Cl1 0.0791(13) 0.0436(9) 0.0700(12) -0.0146(8) -0.0071(10) -0.0125(9) Si1 0.0720(14) 0.0625(13) 0.0412(10) -0.0137(9) 0.0028(9) -0.0160(11) Si2 0.0636(13) 0.0606(12) 0.0585(12) -0.0115(10) 0.0089(10) -0.0282(11) Si3 0.0601(13) 0.0643(13) 0.0586(12) -0.0051(10) -0.0196(10) -0.0068(11) Si4 0.0819(15) 0.0695(14) 0.0386(10) -0.0111(9) -0.0134(10) -0.0127(12) N1 0.043(3) 0.047(3) 0.069(4) -0.015(3) -0.002(3) -0.017(3) N2 0.035(3) 0.045(3) 0.042(3) -0.012(2) -0.004(2) -0.005(2) N3 0.042(3) 0.049(3) 0.041(3) -0.007(2) 0.001(2) -0.011(2) N4 0.061(3) 0.051(3) 0.037(3) -0.009(2) -0.011(2) -0.015(3) C1 0.062(4) 0.052(4) 0.033(3) -0.012(3) -0.004(3) -0.014(3) C2 0.048(4) 0.051(4) 0.088(6) -0.021(4) 0.004(4) -0.014(4) C3 0.056(5) 0.056(5) 0.148(9) -0.024(6) 0.021(6) -0.023(4) C4 0.073(7) 0.066(6) 0.185(13) -0.017(7) 0.009(7) -0.028(5) C5 0.100(9) 0.083(8) 0.221(16) -0.032(9) -0.024(10) -0.053(7) C6 0.058(6) 0.093(8) 0.204(14) -0.061(9) -0.009(7) -0.023(6) C7 0.042(4) 0.086(6) 0.129(8) -0.053(6) -0.008(5) -0.021(4) C8 0.100(8) 0.057(5) 0.110(8) 0.001(5) -0.001(6) -0.020(5) C9 0.083(7) 0.114(8) 0.106(8) -0.046(7) -0.016(6) -0.026(6) C10 0.037(3) 0.040(3) 0.058(4) -0.014(3) 0.001(3) -0.007(3) C11 0.046(4) 0.053(4) 0.057(4) 0.001(3) -0.009(3) -0.009(3) C12 0.077(6) 0.065(5) 0.062(5) 0.008(4) -0.024(4) -0.011(4) C13 0.075(6) 0.047(5) 0.116(8) 0.000(5) -0.013(5) -0.011(4) C14 0.065(5) 0.049(4) 0.093(6) -0.020(4) -0.008(4) -0.013(4) C15 0.049(4) 0.055(4) 0.059(4) -0.012(3) -0.005(3) -0.014(3) C16 0.087(6) 0.073(5) 0.040(4) -0.006(4) -0.017(4) -0.012(5) C17 0.085(6) 0.073(5) 0.067(5) -0.034(4) -0.005(4) -0.019(5) C18 0.046(4) 0.060(4) 0.069(5) -0.020(4) 0.000(3) -0.007(4) C19 0.054(5) 0.094(6) 0.075(6) 0.001(5) 0.009(4) 0.003(5) C20 0.055(5) 0.126(9) 0.098(7) -0.016(6) 0.017(5) -0.013(6) C21 0.049(5) 0.097(7) 0.110(8) -0.012(6) 0.003(5) -0.005(5) C22 0.042(4) 0.109(7) 0.101(7) -0.023(6) -0.025(4) 0.001(5) C23 0.052(5) 0.094(7) 0.088(6) 0.000(5) -0.004(4) -0.001(5) C24 0.108(7) 0.085(6) 0.070(5) -0.025(5) -0.031(5) -0.033(6) C25 0.153(11) 0.107(8) 0.051(5) -0.007(5) 0.012(6) -0.040(7) C26 0.092(7) 0.104(7) 0.070(6) -0.042(5) 0.007(5) -0.010(6) C27 0.087(6) 0.086(6) 0.069(5) -0.031(5) 0.006(4) -0.043(5) C28 0.099(7) 0.068(6) 0.093(7) -0.001(5) 0.016(5) -0.030(5) C29 0.072(6) 0.100(7) 0.097(7) -0.019(5) 0.015(5) -0.049(5) C30 0.062(5) 0.108(7) 0.076(6) -0.013(5) -0.002(4) 0.005(5) C31 0.080(6) 0.100(7) 0.115(8) -0.012(6) -0.046(6) -0.021(6) C32 0.115(8) 0.061(5) 0.081(6) -0.012(4) -0.040(6) -0.002(5) C33 0.135(10) 0.125(9) 0.045(5) 0.002(5) -0.004(5) -0.006(7) C34 0.100(7) 0.118(8) 0.097(7) -0.064(6) -0.023(6) -0.023(6) C35 0.075(6) 0.089(6) 0.052(4) -0.010(4) 0.006(4) -0.015(5) Li1 0.093(11) 0.071(9) 0.078(9) -0.035(7) -0.007(8) -0.016(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 N3 2.213(5) . ? Lu1 N4 2.230(5) . ? Lu1 N1 2.328(5) . ? Lu1 N2 2.380(5) . ? Lu1 Cl1 2.6018(17) . ? Lu1 C1 2.812(7) . ? Lu1 Si2 3.376(2) . ? Cl1 Li1 2.358(14) . ? Si1 N3 1.721(5) . ? Si1 C24 1.842(9) . ? Si1 C26 1.858(9) . ? Si1 C25 1.893(9) . ? Si2 N3 1.724(6) . ? Si2 C27 1.864(8) . ? Si2 C28 1.875(9) . ? Si2 C29 1.883(9) . ? Si3 N4 1.733(6) . ? Si3 C30 1.868(9) . ? Si3 C32 1.870(9) . ? Si3 C31 1.894(9) . ? Si4 N4 1.725(5) . ? Si4 C34 1.863(9) . ? Si4 C35 1.865(9) . ? Si4 C33 1.881(9) . ? O1 C39 1.465(17) . ? O1 C36 1.471(18) . ? O1 Li1 1.82(2) . ? O1' C39' 1.412(17) . ? O1' C36' 1.492(18) . ? O1' Li1 2.00(2) . ? O2 C43 1.426(17) . ? O2 C40 1.443(17) . ? O2 Li1 2.04(2) . ? O2' C43' 1.443(17) . ? O2' C40' 1.488(17) . ? O2' Li1 1.90(2) . ? O3 C44 1.461(18) . ? O3 C47 1.460(18) . ? O3 Li1 1.87(2) . ? O3' C47' 1.436(18) . ? O3' C44' 1.490(17) . ? O3' Li1 1.95(2) . ? N1 C1 1.327(8) . ? N1 C2 1.436(9) . ? N2 C1 1.342(8) . ? N2 C10 1.419(8) . ? C1 C18 1.523(10) . ? C2 C7 1.400(12) . ? C2 C3 1.417(13) . ? C3 C4 1.393(13) . ? C3 C8 1.497(14) . ? C4 C5 1.343(17) . ? C4 H4 0.9300 . ? C5 C6 1.348(18) . ? C5 H5 0.9300 . ? C6 C7 1.415(13) . ? C6 H6 0.9300 . ? C7 C9 1.513(14) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C15 1.394(9) . ? C10 C11 1.398(9) . ? C11 C12 1.375(10) . ? C11 C16 1.498(10) . ? C12 C13 1.363(12) . ? C12 H12 0.9300 . ? C13 C14 1.350(12) . ? C13 H13 0.9300 . ? C14 C15 1.406(10) . ? C14 H14 0.9300 . ? C15 C17 1.458(10) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C23 1.502(11) . ? C18 C19 1.522(11) . ? C18 H18 0.9800 . ? C19 C20 1.504(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.454(13) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.503(13) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.519(11) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.508(18) . ? C36' C37' 1.512(18) . ? C37 C38 1.516(18) . ? C37' C38' 1.532(18) . ? C38 C39 1.471(18) . ? C38' C39' 1.493(18) . ? C40 C41 1.493(18) . ? C40' C41' 1.486(18) . ? C41 C42 1.508(17) . ? C41' C42' 1.547(17) . ? C42 C43 1.491(18) . ? C42' C43' 1.512(18) . ? C44 C45 1.492(18) . ? C44' C45' 1.547(18) . ? C45 C46 1.475(18) . ? C45' C46' 1.474(18) . ? C46 C47 1.509(18) . ? C46' C47' 1.547(19) . ? 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 N3 Lu1 N4 119.7(2) . . ? N3 Lu1 N1 121.9(2) . . ? N4 Lu1 N1 118.2(2) . . ? N3 Lu1 N2 96.19(18) . . ? N4 Lu1 N2 112.93(18) . . ? N1 Lu1 N2 56.35(18) . . ? N3 Lu1 Cl1 96.78(14) . . ? N4 Lu1 Cl1 93.75(14) . . ? N1 Lu1 Cl1 83.88(14) . . ? N2 Lu1 Cl1 138.88(13) . . ? N3 Lu1 C1 112.18(19) . . ? N4 Lu1 C1 118.28(19) . . ? N1 Lu1 C1 27.96(19) . . ? N2 Lu1 C1 28.42(18) . . ? Cl1 Lu1 C1 111.50(15) . . ? N3 Lu1 Si2 26.93(14) . . ? N4 Lu1 Si2 99.64(15) . . ? N1 Lu1 Si2 135.45(15) . . ? N2 Lu1 Si2 88.82(13) . . ? Cl1 Lu1 Si2 118.01(6) . . ? C1 Lu1 Si2 113.86(14) . . ? Li1 Cl1 Lu1 175.1(4) . . ? N3 Si1 C24 111.3(4) . . ? N3 Si1 C26 113.5(3) . . ? C24 Si1 C26 107.6(5) . . ? N3 Si1 C25 115.0(4) . . ? C24 Si1 C25 104.1(5) . . ? C26 Si1 C25 104.7(5) . . ? N3 Si2 C27 109.9(3) . . ? N3 Si2 C28 115.1(4) . . ? C27 Si2 C28 104.5(4) . . ? N3 Si2 C29 112.8(3) . . ? C27 Si2 C29 107.8(4) . . ? C28 Si2 C29 106.2(4) . . ? N3 Si2 Lu1 35.55(17) . . ? C27 Si2 Lu1 74.4(3) . . ? C28 Si2 Lu1 125.0(3) . . ? C29 Si2 Lu1 127.0(3) . . ? N4 Si3 C30 112.6(3) . . ? N4 Si3 C32 111.6(4) . . ? C30 Si3 C32 107.6(5) . . ? N4 Si3 C31 115.0(4) . . ? C30 Si3 C31 102.3(5) . . ? C32 Si3 C31 107.1(4) . . ? N4 Si4 C34 113.5(4) . . ? N4 Si4 C35 111.8(3) . . ? C34 Si4 C35 107.2(4) . . ? N4 Si4 C33 115.3(4) . . ? C34 Si4 C33 105.6(5) . . ? C35 Si4 C33 102.7(5) . . ? C39 O1 C36 103(2) . . ? C39 O1 Li1 133.4(15) . . ? C36 O1 Li1 123.0(18) . . ? C39' O1' C36' 114.4(19) . . ? C39' O1' Li1 137.1(14) . . ? C36' O1' Li1 107.5(15) . . ? C43 O2 C40 116.4(19) . . ? C43 O2 Li1 121.6(15) . . ? C40 O2 Li1 122.0(14) . . ? C43' O2' C40' 105.2(17) . . ? C43' O2' Li1 118.7(14) . . ? C40' O2' Li1 127.1(16) . . ? C44 O3 C47 90(2) . . ? C44 O3 Li1 142.2(16) . . ? C47 O3 Li1 128.0(16) . . ? C47' O3' C44' 114.6(19) . . ? C47' O3' Li1 130.8(16) . . ? C44' O3' Li1 113.3(14) . . ? C1 N1 C2 123.8(6) . . ? C1 N1 Lu1 96.8(4) . . ? C2 N1 Lu1 139.4(4) . . ? C1 N2 C10 123.9(5) . . ? C1 N2 Lu1 94.0(4) . . ? C10 N2 Lu1 139.5(4) . . ? Si1 N3 Si2 118.9(3) . . ? Si1 N3 Lu1 123.3(3) . . ? Si2 N3 Lu1 117.5(3) . . ? Si4 N4 Si3 114.5(3) . . ? Si4 N4 Lu1 128.1(3) . . ? Si3 N4 Lu1 117.3(3) . . ? N1 C1 N2 112.8(6) . . ? N1 C1 C18 120.8(6) . . ? N2 C1 C18 126.1(6) . . ? N1 C1 Lu1 55.3(3) . . ? N2 C1 Lu1 57.6(3) . . ? C18 C1 Lu1 171.0(5) . . ? C7 C2 C3 119.7(8) . . ? C7 C2 N1 121.7(8) . . ? C3 C2 N1 118.5(8) . . ? C4 C3 C2 118.8(11) . . ? C4 C3 C8 120.4(10) . . ? C2 C3 C8 120.8(8) . . ? C5 C4 C3 121.6(12) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 120.2(11) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 122.4(12) . . ? C5 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C2 C7 C6 117.3(11) . . ? C2 C7 C9 122.9(8) . . ? C6 C7 C9 119.9(10) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 118.3(6) . . ? C15 C10 N2 121.3(6) . . ? C11 C10 N2 120.2(6) . . ? C12 C11 C10 120.5(7) . . ? C12 C11 C16 119.0(7) . . ? C10 C11 C16 120.5(6) . . ? C13 C12 C11 121.1(8) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 C12 119.5(8) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 121.5(8) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C10 C15 C14 119.0(7) . . ? C10 C15 C17 121.8(7) . . ? C14 C15 C17 119.2(7) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 109.4(7) . . ? C23 C18 C1 121.5(7) . . ? C19 C18 C1 109.0(6) . . ? C23 C18 H18 105.2 . . ? C19 C18 H18 105.2 . . ? C1 C18 H18 105.2 . . ? C20 C19 C18 112.8(8) . . ? C20 C19 H19A 109.0 . . ? C18 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? C18 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C21 C20 C19 114.5(8) . . ? C21 C20 H20A 108.6 . . ? C19 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? C19 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C20 C21 C22 112.8(8) . . ? C20 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? C20 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C21 C22 C23 111.2(7) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C18 C23 C22 111.2(8) . . ? C18 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C18 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si3 C30 H30A 109.5 . . ? Si3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si4 C33 H33A 109.5 . . ? Si4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si4 C34 H34A 109.5 . . ? Si4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si4 C35 H35A 109.5 . . ? Si4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O1 C36 C37 105(2) . . ? O1' C36' C37' 104(2) . . ? C36 C37 C38 107(2) . . ? C36' C37' C38' 103(2) . . ? C39 C38 C37 102(2) . . ? C39' C38' C37' 111(2) . . ? O1 C39 C38 112.5(19) . . ? O1' C39' C38' 102.9(19) . . ? O2 C40 C41 97.5(18) . . ? O2' C40' C41' 114.9(19) . . ? C40 C41 C42 105.0(19) . . ? C40' C41' C42' 97.9(19) . . ? C43 C42 C41 99.1(19) . . ? C43' C42' C41' 110.4(19) . . ? O2 C43 C42 96.5(18) . . ? O2' C43' C42' 107.5(18) . . ? O3 C44 C45 103(2) . . ? O3' C44' C45' 104(2) . . ? C46 C45 C44 105(2) . . ? C46' C45' C44' 103(2) . . ? C45 C46 C47 97(2) . . ? C45' C46' C47' 110(2) . . ? O3 C47 C46 111(2) . . ? O3' C47' C46' 99(2) . . ? O1 Li1 O3 92.2(10) . . ? O1 Li1 O2' 111.4(10) . . ? O3 Li1 O2' 108.8(10) . . ? O1 Li1 O3' 108.8(10) . . ? O3 Li1 O3' 17.4(6) . . ? O2' Li1 O3' 96.9(10) . . ? O1 Li1 O1' 14.7(7) . . ? O3 Li1 O1' 106.9(10) . . ? O2' Li1 O1' 106.5(9) . . ? O3' Li1 O1' 123.5(10) . . ? O1 Li1 O2 114.0(10) . . ? O3 Li1 O2 117.9(10) . . ? O2' Li1 O2 10.4(9) . . ? O3' Li1 O2 104.7(10) . . ? O1' Li1 O2 106.6(9) . . ? O1 Li1 Cl1 111.7(9) . . ? O3 Li1 Cl1 111.3(8) . . ? O2' Li1 Cl1 118.4(9) . . ? O3' Li1 Cl1 108.3(7) . . ? O1' Li1 Cl1 104.3(8) . . ? O2 Li1 Cl1 108.9(8) . . ? 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 N3 Lu1 Cl1 Li1 -22(5) . . . . ? N4 Lu1 Cl1 Li1 98(5) . . . . ? N1 Lu1 Cl1 Li1 -144(5) . . . . ? N2 Lu1 Cl1 Li1 -130(5) . . . . ? C1 Lu1 Cl1 Li1 -139(5) . . . . ? Si2 Lu1 Cl1 Li1 -5(5) . . . . ? N4 Lu1 Si2 N3 -140.7(3) . . . . ? N1 Lu1 Si2 N3 70.4(4) . . . . ? N2 Lu1 Si2 N3 106.2(3) . . . . ? Cl1 Lu1 Si2 N3 -41.2(3) . . . . ? C1 Lu1 Si2 N3 92.4(3) . . . . ? N3 Lu1 Si2 C27 178.1(4) . . . . ? N4 Lu1 Si2 C27 37.4(3) . . . . ? N1 Lu1 Si2 C27 -111.5(4) . . . . ? N2 Lu1 Si2 C27 -75.7(3) . . . . ? Cl1 Lu1 Si2 C27 136.9(3) . . . . ? C1 Lu1 Si2 C27 -89.5(3) . . . . ? N3 Lu1 Si2 C28 -84.9(5) . . . . ? N4 Lu1 Si2 C28 134.3(4) . . . . ? N1 Lu1 Si2 C28 -14.5(4) . . . . ? N2 Lu1 Si2 C28 21.3(4) . . . . ? Cl1 Lu1 Si2 C28 -126.1(4) . . . . ? C1 Lu1 Si2 C28 7.4(4) . . . . ? N3 Lu1 Si2 C29 77.3(5) . . . . ? N4 Lu1 Si2 C29 -63.4(4) . . . . ? N1 Lu1 Si2 C29 147.7(4) . . . . ? N2 Lu1 Si2 C29 -176.5(4) . . . . ? Cl1 Lu1 Si2 C29 36.1(4) . . . . ? C1 Lu1 Si2 C29 169.7(4) . . . . ? N3 Lu1 N1 C1 77.0(4) . . . . ? N4 Lu1 N1 C1 -97.8(4) . . . . ? N2 Lu1 N1 C1 2.2(3) . . . . ? Cl1 Lu1 N1 C1 171.2(4) . . . . ? Si2 Lu1 N1 C1 46.8(5) . . . . ? N3 Lu1 N1 C2 -102.3(8) . . . . ? N4 Lu1 N1 C2 82.8(8) . . . . ? N2 Lu1 N1 C2 -177.1(8) . . . . ? Cl1 Lu1 N1 C2 -8.1(7) . . . . ? C1 Lu1 N1 C2 -179.3(10) . . . . ? Si2 Lu1 N1 C2 -132.5(7) . . . . ? N3 Lu1 N2 C1 -126.7(4) . . . . ? N4 Lu1 N2 C1 107.4(4) . . . . ? N1 Lu1 N2 C1 -2.2(3) . . . . ? Cl1 Lu1 N2 C1 -18.9(4) . . . . ? Si2 Lu1 N2 C1 -152.6(3) . . . . ? N3 Lu1 N2 C10 33.8(6) . . . . ? N4 Lu1 N2 C10 -92.2(6) . . . . ? N1 Lu1 N2 C10 158.3(7) . . . . ? Cl1 Lu1 N2 C10 141.5(5) . . . . ? C1 Lu1 N2 C10 160.4(8) . . . . ? Si2 Lu1 N2 C10 7.8(6) . . . . ? C24 Si1 N3 Si2 151.0(4) . . . . ? C26 Si1 N3 Si2 -87.5(5) . . . . ? C25 Si1 N3 Si2 33.0(6) . . . . ? C24 Si1 N3 Lu1 -35.7(5) . . . . ? C26 Si1 N3 Lu1 85.8(5) . . . . ? C25 Si1 N3 Lu1 -153.7(5) . . . . ? C27 Si2 N3 Si1 171.8(4) . . . . ? C28 Si2 N3 Si1 -70.6(5) . . . . ? C29 Si2 N3 Si1 51.4(5) . . . . ? Lu1 Si2 N3 Si1 173.7(5) . . . . ? C27 Si2 N3 Lu1 -1.9(5) . . . . ? C28 Si2 N3 Lu1 115.7(4) . . . . ? C29 Si2 N3 Lu1 -122.3(4) . . . . ? N4 Lu1 N3 Si1 -127.5(3) . . . . ? N1 Lu1 N3 Si1 57.7(4) . . . . ? N2 Lu1 N3 Si1 111.6(3) . . . . ? Cl1 Lu1 N3 Si1 -29.3(3) . . . . ? C1 Lu1 N3 Si1 87.3(3) . . . . ? Si2 Lu1 N3 Si1 -173.4(6) . . . . ? N4 Lu1 N3 Si2 45.9(4) . . . . ? N1 Lu1 N3 Si2 -128.9(3) . . . . ? N2 Lu1 N3 Si2 -75.0(3) . . . . ? Cl1 Lu1 N3 Si2 144.1(3) . . . . ? C1 Lu1 N3 Si2 -99.3(3) . . . . ? C34 Si4 N4 Si3 -81.0(5) . . . . ? C35 Si4 N4 Si3 157.6(4) . . . . ? C33 Si4 N4 Si3 40.8(6) . . . . ? C34 Si4 N4 Lu1 102.1(5) . . . . ? C35 Si4 N4 Lu1 -19.2(5) . . . . ? C33 Si4 N4 Lu1 -136.0(5) . . . . ? C30 Si3 N4 Si4 157.5(4) . . . . ? C32 Si3 N4 Si4 -81.4(4) . . . . ? C31 Si3 N4 Si4 40.9(5) . . . . ? C30 Si3 N4 Lu1 -25.3(5) . . . . ? C32 Si3 N4 Lu1 95.8(4) . . . . ? C31 Si3 N4 Lu1 -141.9(4) . . . . ? N3 Lu1 N4 Si4 -131.6(3) . . . . ? N1 Lu1 N4 Si4 43.3(4) . . . . ? N2 Lu1 N4 Si4 -19.5(4) . . . . ? Cl1 Lu1 N4 Si4 128.4(3) . . . . ? C1 Lu1 N4 Si4 11.5(4) . . . . ? Si2 Lu1 N4 Si4 -112.4(3) . . . . ? N3 Lu1 N4 Si3 51.6(4) . . . . ? N1 Lu1 N4 Si3 -133.4(3) . . . . ? N2 Lu1 N4 Si3 163.7(3) . . . . ? Cl1 Lu1 N4 Si3 -48.4(3) . . . . ? C1 Lu1 N4 Si3 -165.3(3) . . . . ? Si2 Lu1 N4 Si3 70.9(3) . . . . ? C2 N1 C1 N2 176.0(6) . . . . ? Lu1 N1 C1 N2 -3.5(6) . . . . ? C2 N1 C1 C18 -10.2(10) . . . . ? Lu1 N1 C1 C18 170.3(5) . . . . ? C2 N1 C1 Lu1 179.5(8) . . . . ? C10 N2 C1 N1 -161.4(6) . . . . ? Lu1 N2 C1 N1 3.4(5) . . . . ? C10 N2 C1 C18 25.2(9) . . . . ? Lu1 N2 C1 C18 -170.0(6) . . . . ? C10 N2 C1 Lu1 -164.8(6) . . . . ? N3 Lu1 C1 N1 -116.7(4) . . . . ? N4 Lu1 C1 N1 97.5(4) . . . . ? N2 Lu1 C1 N1 -176.2(6) . . . . ? Cl1 Lu1 C1 N1 -9.4(4) . . . . ? Si2 Lu1 C1 N1 -146.0(4) . . . . ? N3 Lu1 C1 N2 59.4(4) . . . . ? N4 Lu1 C1 N2 -86.3(4) . . . . ? N1 Lu1 C1 N2 176.2(6) . . . . ? Cl1 Lu1 C1 N2 166.7(3) . . . . ? Si2 Lu1 C1 N2 30.2(4) . . . . ? N3 Lu1 C1 C18 176(3) . . . . ? N4 Lu1 C1 C18 31(3) . . . . ? N1 Lu1 C1 C18 -67(3) . . . . ? N2 Lu1 C1 C18 117(3) . . . . ? Cl1 Lu1 C1 C18 -76(3) . . . . ? Si2 Lu1 C1 C18 147(3) . . . . ? C1 N1 C2 C7 -66.7(10) . . . . ? Lu1 N1 C2 C7 112.5(8) . . . . ? C1 N1 C2 C3 116.9(8) . . . . ? Lu1 N1 C2 C3 -63.9(10) . . . . ? C7 C2 C3 C4 0.6(12) . . . . ? N1 C2 C3 C4 177.1(7) . . . . ? C7 C2 C3 C8 -178.0(8) . . . . ? N1 C2 C3 C8 -1.5(12) . . . . ? C2 C3 C4 C5 1.1(16) . . . . ? C8 C3 C4 C5 179.7(11) . . . . ? C3 C4 C5 C6 -2(2) . . . . ? C4 C5 C6 C7 0(2) . . . . ? C3 C2 C7 C6 -1.7(12) . . . . ? N1 C2 C7 C6 -178.1(7) . . . . ? C3 C2 C7 C9 177.0(8) . . . . ? N1 C2 C7 C9 0.7(12) . . . . ? C5 C6 C7 C2 1.3(15) . . . . ? C5 C6 C7 C9 -177.5(11) . . . . ? C1 N2 C10 C15 -109.6(7) . . . . ? Lu1 N2 C10 C15 94.1(7) . . . . ? C1 N2 C10 C11 76.1(8) . . . . ? Lu1 N2 C10 C11 -80.2(8) . . . . ? C15 C10 C11 C12 2.9(10) . . . . ? N2 C10 C11 C12 177.4(7) . . . . ? C15 C10 C11 C16 -176.0(7) . . . . ? N2 C10 C11 C16 -1.5(10) . . . . ? C10 C11 C12 C13 -0.9(12) . . . . ? C16 C11 C12 C13 178.1(8) . . . . ? C11 C12 C13 C14 -1.5(14) . . . . ? C12 C13 C14 C15 1.8(13) . . . . ? C11 C10 C15 C14 -2.6(10) . . . . ? N2 C10 C15 C14 -177.1(6) . . . . ? C11 C10 C15 C17 177.8(7) . . . . ? N2 C10 C15 C17 3.4(10) . . . . ? C13 C14 C15 C10 0.3(12) . . . . ? C13 C14 C15 C17 179.9(8) . . . . ? N1 C1 C18 C23 149.5(8) . . . . ? N2 C1 C18 C23 -37.6(11) . . . . ? Lu1 C1 C18 C23 -149(3) . . . . ? N1 C1 C18 C19 -81.9(8) . . . . ? N2 C1 C18 C19 91.0(9) . . . . ? Lu1 C1 C18 C19 -20(3) . . . . ? C23 C18 C19 C20 -52.9(11) . . . . ? C1 C18 C19 C20 172.0(8) . . . . ? C18 C19 C20 C21 49.8(13) . . . . ? C19 C20 C21 C22 -49.1(13) . . . . ? C20 C21 C22 C23 52.4(12) . . . . ? C19 C18 C23 C22 57.0(10) . . . . ? C1 C18 C23 C22 -174.5(7) . . . . ? C21 C22 C23 C18 -57.3(11) . . . . ? C39 O1 C36 C37 31(3) . . . . ? Li1 O1 C36 C37 -144(2) . . . . ? C39' O1' C36' C37' 22(3) . . . . ? Li1 O1' C36' C37' -167(2) . . . . ? O1 C36 C37 C38 -30(3) . . . . ? O1' C36' C37' C38' -21(3) . . . . ? C36 C37 C38 C39 17(3) . . . . ? C36' C37' C38' C39' 15(3) . . . . ? C36 O1 C39 C38 -22(3) . . . . ? Li1 O1 C39 C38 152(2) . . . . ? C37 C38 C39 O1 3(3) . . . . ? C36' O1' C39' C38' -12(3) . . . . ? Li1 O1' C39' C38' -179.2(18) . . . . ? C37' C38' C39' O1' -3(3) . . . . ? C43 O2 C40 C41 4(3) . . . . ? Li1 O2 C40 C41 -178.1(15) . . . . ? C43' O2' C40' C41' 14(3) . . . . ? Li1 O2' C40' C41' -132(2) . . . . ? O2 C40 C41 C42 27(3) . . . . ? O2' C40' C41' C42' -20(3) . . . . ? C40 C41 C42 C43 -48(3) . . . . ? C40' C41' C42' C43' 19(3) . . . . ? C40 O2 C43 C42 -33(3) . . . . ? Li1 O2 C43 C42 149.1(15) . . . . ? C41 C42 C43 O2 46(2) . . . . ? C40' O2' C43' C42' 0(3) . . . . ? Li1 O2' C43' C42' 149.3(16) . . . . ? C41' C42' C43' O2' -12(3) . . . . ? C47 O3 C44 C45 55(3) . . . . ? Li1 O3 C44 C45 -121(2) . . . . ? C47' O3' C44' C45' -6(3) . . . . ? Li1 O3' C44' C45' 162.3(19) . . . . ? O3 C44 C45 C46 -46(3) . . . . ? O3' C44' C45' C46' -12(3) . . . . ? C44 C45 C46 C47 12(3) . . . . ? C44' C45' C46' C47' 26(4) . . . . ? C44 O3 C47 C46 -51(3) . . . . ? Li1 O3 C47 C46 126(3) . . . . ? C45 C46 C47 O3 26(4) . . . . ? C44' O3' C47' C46' 21(3) . . . . ? Li1 O3' C47' C46' -145.4(19) . . . . ? C45' C46' C47' O3' -29(4) . . . . ? C39 O1 Li1 O3 87(2) . . . . ? C36 O1 Li1 O3 -99(2) . . . . ? C39 O1 Li1 O2' -24(3) . . . . ? C36 O1 Li1 O2' 149(2) . . . . ? C39 O1 Li1 O3' 82(2) . . . . ? C36 O1 Li1 O3' -105(2) . . . . ? C39 O1 Li1 O1' -97(4) . . . . ? C36 O1 Li1 O1' 76(3) . . . . ? C39 O1 Li1 O2 -35(3) . . . . ? C36 O1 Li1 O2 139(2) . . . . ? C39 O1 Li1 Cl1 -159(2) . . . . ? C36 O1 Li1 Cl1 15(2) . . . . ? C44 O3 Li1 O1 -61(3) . . . . ? C47 O3 Li1 O1 123.2(19) . . . . ? C44 O3 Li1 O2' 52(3) . . . . ? C47 O3 Li1 O2' -123.3(19) . . . . ? C44 O3 Li1 O3' 101(4) . . . . ? C47 O3 Li1 O3' -75(3) . . . . ? C44 O3 Li1 O1' -62(3) . . . . ? C47 O3 Li1 O1' 122.1(19) . . . . ? C44 O3 Li1 O2 57(3) . . . . ? C47 O3 Li1 O2 -118(2) . . . . ? C44 O3 Li1 Cl1 -176(2) . . . . ? C47 O3 Li1 Cl1 9(2) . . . . ? C43' O2' Li1 O1 163.0(16) . . . . ? C40' O2' Li1 O1 -55(2) . . . . ? C43' O2' Li1 O3 62.8(18) . . . . ? C40' O2' Li1 O3 -155.1(16) . . . . ? C43' O2' Li1 O3' 49.7(18) . . . . ? C40' O2' Li1 O3' -168.2(17) . . . . ? C43' O2' Li1 O1' 177.6(16) . . . . ? C40' O2' Li1 O1' -40(2) . . . . ? C43' O2' Li1 O2 -90(5) . . . . ? C40' O2' Li1 O2 52(5) . . . . ? C43' O2' Li1 Cl1 -65.5(18) . . . . ? C40' O2' Li1 Cl1 76.6(19) . . . . ? C47' O3' Li1 O1 118(2) . . . . ? C44' O3' Li1 O1 -47.9(19) . . . . ? C47' O3' Li1 O3 100(3) . . . . ? C44' O3' Li1 O3 -67(3) . . . . ? C47' O3' Li1 O2' -126(2) . . . . ? C44' O3' Li1 O2' 67.5(17) . . . . ? C47' O3' Li1 O1' 119(2) . . . . ? C44' O3' Li1 O1' -47(2) . . . . ? C47' O3' Li1 O2 -119(2) . . . . ? C44' O3' Li1 O2 74.4(17) . . . . ? C47' O3' Li1 Cl1 -3(2) . . . . ? C44' O3' Li1 Cl1 -169.5(15) . . . . ? C39' O1' Li1 O1 106(4) . . . . ? C36' O1' Li1 O1 -61(3) . . . . ? C39' O1' Li1 O3 111(2) . . . . ? C36' O1' Li1 O3 -57(2) . . . . ? C39' O1' Li1 O2' -5(3) . . . . ? C36' O1' Li1 O2' -173.1(19) . . . . ? C39' O1' Li1 O3' 105(2) . . . . ? C36' O1' Li1 O3' -63(2) . . . . ? C39' O1' Li1 O2 -16(3) . . . . ? C36' O1' Li1 O2 176.1(19) . . . . ? C39' O1' Li1 Cl1 -131(2) . . . . ? C36' O1' Li1 Cl1 61.0(19) . . . . ? C43 O2 Li1 O1 169.8(17) . . . . ? C40 O2 Li1 O1 -8(2) . . . . ? C43 O2 Li1 O3 63(2) . . . . ? C40 O2 Li1 O3 -114.2(19) . . . . ? C43 O2 Li1 O2' 93(5) . . . . ? C40 O2 Li1 O2' -85(5) . . . . ? C43 O2 Li1 O3' 51.0(19) . . . . ? C40 O2 Li1 O3' -126.4(18) . . . . ? C43 O2 Li1 O1' -176.6(16) . . . . ? C40 O2 Li1 O1' 6(2) . . . . ? C43 O2 Li1 Cl1 -64.6(18) . . . . ? C40 O2 Li1 Cl1 117.9(18) . . . . ? Lu1 Cl1 Li1 O1 100(5) . . . . ? Lu1 Cl1 Li1 O3 -158(4) . . . . ? Lu1 Cl1 Li1 O2' -31(5) . . . . ? Lu1 Cl1 Li1 O3' -140(4) . . . . ? Lu1 Cl1 Li1 O1' 87(5) . . . . ? Lu1 Cl1 Li1 O2 -27(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.558 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.113 data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 792827' #TrackingRef 'data.doc' #TrackingRef 'data.doc' #TrackingRef 'data.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H59 N4 Si4 Y, 0.5(C7 H8)' _chemical_formula_sum 'C38.50 H63 N4 Si4 Y' _chemical_formula_weight 783.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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 12.388(5) _cell_length_b 13.303(5) _cell_length_c 15.584(6) _cell_angle_alpha 105.451(6) _cell_angle_beta 109.870(6) _cell_angle_gamma 98.761(6) _cell_volume 2243.0(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9456 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 834 _exptl_absorpt_coefficient_mu 1.436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.395 _exptl_absorpt_correction_T_max 0.650 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21779 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8151 _reflns_number_gt 6279 _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^)+(0.1085P)^2^+0.3582P] 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 8151 _refine_ls_number_parameters 436 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0903 _refine_ls_wR_factor_ref 0.2297 _refine_ls_wR_factor_gt 0.2126 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 0.96912(4) 0.75809(4) 0.72615(4) 0.0426(2) Uani 1 1 d . . . Si1 Si 1.20795(15) 0.99755(14) 0.81289(13) 0.0536(5) Uani 1 1 d . . . Si2 Si 1.23175(15) 0.77427(14) 0.73167(13) 0.0530(5) Uani 1 1 d . . . Si3 Si 0.99190(16) 0.67994(14) 0.90814(12) 0.0505(4) Uani 1 1 d . . . Si4 Si 0.85244(16) 0.49341(13) 0.72156(13) 0.0541(5) Uani 1 1 d . . . N1 N 0.8152(4) 0.8432(4) 0.6994(3) 0.0485(12) Uani 1 1 d . . . N2 N 0.8370(4) 0.7381(4) 0.5700(3) 0.0485(12) Uani 1 1 d . . . N3 N 1.1509(4) 0.8592(4) 0.7652(3) 0.0427(11) Uani 1 1 d . . . N4 N 0.9332(4) 0.6267(4) 0.7841(3) 0.0452(11) Uani 1 1 d . . . C1 C 0.7751(5) 0.8022(4) 0.6029(4) 0.0437(13) Uani 1 1 d . . . C2 C 0.7670(5) 0.9195(5) 0.7465(4) 0.0466(14) Uani 1 1 d . . . C3 C 0.7014(5) 0.8871(5) 0.7975(4) 0.0535(15) Uani 1 1 d . . . C4 C 0.6593(6) 0.9638(7) 0.8485(5) 0.0678(19) Uani 1 1 d . . . H4 H 0.6175 0.9441 0.8836 0.081 Uiso 1 1 calc R . . C5 C 0.6786(6) 1.0672(7) 0.8475(5) 0.074(2) Uani 1 1 d . . . H5 H 0.6469 1.1160 0.8797 0.089 Uiso 1 1 calc R . . C6 C 0.7445(6) 1.1003(5) 0.7994(5) 0.0638(18) Uani 1 1 d . . . H6 H 0.7601 1.1719 0.8020 0.077 Uiso 1 1 calc R . . C7 C 0.7881(5) 1.0263(5) 0.7464(5) 0.0556(16) Uani 1 1 d . . . C8 C 0.6745(6) 0.7724(6) 0.7968(5) 0.0667(18) Uani 1 1 d . . . H8A H 0.7477 0.7528 0.8203 0.100 Uiso 1 1 calc R . . H8B H 0.6260 0.7244 0.7317 0.100 Uiso 1 1 calc R . . H8C H 0.6328 0.7669 0.8379 0.100 Uiso 1 1 calc R . . C9 C 0.8595(7) 1.0646(6) 0.6946(5) 0.0706(19) Uani 1 1 d . . . H9A H 0.9193 1.0263 0.6955 0.106 Uiso 1 1 calc R . . H9B H 0.8970 1.1408 0.7265 0.106 Uiso 1 1 calc R . . H9C H 0.8076 1.0512 0.6285 0.106 Uiso 1 1 calc R . . C10 C 0.8007(5) 0.6810(5) 0.4686(4) 0.0508(15) Uani 1 1 d . . . C11 C 0.6981(6) 0.5933(6) 0.4181(5) 0.0654(18) Uani 1 1 d . . . C12 C 0.6660(9) 0.5427(7) 0.3187(6) 0.091(3) Uani 1 1 d . . . H12 H 0.5967 0.4865 0.2826 0.110 Uiso 1 1 calc R . . C13 C 0.7344(12) 0.5746(9) 0.2749(6) 0.109(4) Uani 1 1 d . . . H13 H 0.7109 0.5391 0.2087 0.131 Uiso 1 1 calc R . . C14 C 0.8368(10) 0.6568(9) 0.3231(6) 0.096(3) Uani 1 1 d . . . H14 H 0.8829 0.6754 0.2905 0.115 Uiso 1 1 calc R . . C15 C 0.8719(6) 0.7129(6) 0.4221(5) 0.0622(17) Uani 1 1 d . . . C16 C 0.6228(7) 0.5563(6) 0.4667(6) 0.088(2) Uani 1 1 d . . . H16A H 0.6654 0.5880 0.5359 0.132 Uiso 1 1 calc R . . H16B H 0.6040 0.4788 0.4481 0.132 Uiso 1 1 calc R . . H16C H 0.5504 0.5782 0.4476 0.132 Uiso 1 1 calc R . . C17 C 0.9799(7) 0.8065(7) 0.4762(6) 0.083(2) Uani 1 1 d . . . H17A H 0.9568 0.8714 0.4969 0.124 Uiso 1 1 calc R . . H17B H 1.0205 0.8139 0.4347 0.124 Uiso 1 1 calc R . . H17C H 1.0321 0.7945 0.5320 0.124 Uiso 1 1 calc R . . C18 C 0.6704(5) 0.8251(5) 0.5356(4) 0.0456(13) Uani 1 1 d . . . C19 C 0.5633(5) 0.8110(5) 0.5482(4) 0.0567(16) Uani 1 1 d . . . H19 H 0.5579 0.7869 0.5978 0.068 Uiso 1 1 calc R . . C20 C 0.4649(6) 0.8326(6) 0.4874(5) 0.070(2) Uani 1 1 d . . . H20 H 0.3936 0.8221 0.4957 0.084 Uiso 1 1 calc R . . C21 C 0.4737(6) 0.8695(7) 0.4149(5) 0.077(2) Uani 1 1 d . . . H21 H 0.4085 0.8849 0.3745 0.093 Uiso 1 1 calc R . . C22 C 0.5780(7) 0.8837(7) 0.4020(5) 0.077(2) Uani 1 1 d . . . H22 H 0.5836 0.9087 0.3529 0.092 Uiso 1 1 calc R . . C23 C 0.6756(6) 0.8608(5) 0.4619(5) 0.0608(17) Uani 1 1 d . . . H23 H 0.7458 0.8698 0.4519 0.073 Uiso 1 1 calc R . . C24 C 1.3703(6) 1.0415(6) 0.8948(6) 0.084(2) Uani 1 1 d . . . H24A H 1.3827 1.0107 0.9454 0.126 Uiso 1 1 calc R . . H24B H 1.3958 1.1190 0.9232 0.126 Uiso 1 1 calc R . . H24C H 1.4154 1.0174 0.8579 0.126 Uiso 1 1 calc R . . C25 C 1.1306(7) 1.0629(5) 0.8879(5) 0.0684(19) Uani 1 1 d . . . H25A H 1.0462 1.0311 0.8545 0.103 Uiso 1 1 calc R . . H25B H 1.1478 1.1391 0.8983 0.103 Uiso 1 1 calc R . . H25C H 1.1581 1.0520 0.9494 0.103 Uiso 1 1 calc R . . C26 C 1.1890(7) 1.0558(6) 0.7139(6) 0.084(2) Uani 1 1 d . . . H26A H 1.2335 1.0284 0.6774 0.126 Uiso 1 1 calc R . . H26B H 1.2177 1.1332 0.7416 0.126 Uiso 1 1 calc R . . H26C H 1.1062 1.0357 0.6716 0.126 Uiso 1 1 calc R . . C27 C 1.3108(6) 0.8147(6) 0.6580(5) 0.075(2) Uani 1 1 d . . . H27A H 1.2558 0.8283 0.6047 0.113 Uiso 1 1 calc R . . H27B H 1.3427 0.7574 0.6336 0.113 Uiso 1 1 calc R . . H27C H 1.3745 0.8791 0.6981 0.113 Uiso 1 1 calc R . . C28 C 1.1211(6) 0.6403(5) 0.6528(5) 0.0619(17) Uani 1 1 d . . . H28A H 1.0862 0.6116 0.6905 0.093 Uiso 1 1 calc R . . H28B H 1.1607 0.5910 0.6270 0.093 Uiso 1 1 calc R . . H28C H 1.0598 0.6496 0.6003 0.093 Uiso 1 1 calc R . . C29 C 1.3437(6) 0.7521(6) 0.8364(5) 0.075(2) Uani 1 1 d . . . H29A H 1.4096 0.8158 0.8716 0.113 Uiso 1 1 calc R . . H29B H 1.3719 0.6917 0.8124 0.113 Uiso 1 1 calc R . . H29C H 1.3072 0.7376 0.8786 0.113 Uiso 1 1 calc R . . C30 C 1.0300(6) 0.8312(5) 0.9395(4) 0.0584(16) Uani 1 1 d . . . H30A H 1.0931 0.8536 0.9204 0.088 Uiso 1 1 calc R . . H30B H 1.0553 0.8654 1.0082 0.088 Uiso 1 1 calc R . . H30C H 0.9610 0.8516 0.9058 0.088 Uiso 1 1 calc R . . C31 C 1.1325(6) 0.6444(6) 0.9665(5) 0.0715(19) Uani 1 1 d . . . H31A H 1.1201 0.5675 0.9411 0.107 Uiso 1 1 calc R . . H31B H 1.1548 0.6670 1.0354 0.107 Uiso 1 1 calc R . . H31C H 1.1947 0.6804 0.9529 0.107 Uiso 1 1 calc R . . C32 C 0.8893(7) 0.6449(6) 0.9662(5) 0.0691(19) Uani 1 1 d . . . H32A H 0.8147 0.6591 0.9355 0.104 Uiso 1 1 calc R . . H32B H 0.9243 0.6879 1.0340 0.104 Uiso 1 1 calc R . . H32C H 0.8763 0.5696 0.9591 0.104 Uiso 1 1 calc R . . C33 C 0.9116(9) 0.3975(6) 0.7814(6) 0.091(3) Uani 1 1 d . . . H33A H 0.9953 0.4100 0.7962 0.137 Uiso 1 1 calc R . . H33B H 0.8709 0.3244 0.7384 0.137 Uiso 1 1 calc R . . H33C H 0.8989 0.4088 0.8403 0.137 Uiso 1 1 calc R . . C34 C 0.6926(7) 0.4733(7) 0.7068(7) 0.094(3) Uani 1 1 d . . . H34A H 0.6898 0.5057 0.7687 0.140 Uiso 1 1 calc R . . H34B H 0.6537 0.3972 0.6821 0.140 Uiso 1 1 calc R . . H34C H 0.6528 0.5067 0.6622 0.140 Uiso 1 1 calc R . . C35 C 0.8530(7) 0.4458(6) 0.5969(5) 0.078(2) Uani 1 1 d . . . H35A H 0.8307 0.4963 0.5647 0.117 Uiso 1 1 calc R . . H35B H 0.7973 0.3759 0.5600 0.117 Uiso 1 1 calc R . . H35C H 0.9314 0.4409 0.6023 0.117 Uiso 1 1 calc R . . C36 C 0.483(3) 0.572(2) 0.053(2) 0.162(4) Uiso 0.50 1 d PD . . C37 C 0.435(3) 0.466(2) 0.043(2) 0.162(4) Uiso 0.50 1 d PD . . C38 C 0.436(3) 0.366(2) -0.019(2) 0.162(4) Uiso 0.50 1 d PD . . C39 C 0.510(3) 0.373(3) -0.068(2) 0.162(4) Uiso 0.50 1 d PD . . C40 C 0.573(3) 0.480(3) -0.052(2) 0.162(4) Uiso 0.50 1 d PD . . C41 C 0.568(3) 0.572(3) 0.012(2) 0.162(4) Uiso 0.50 1 d PD . . C42 C 0.471(3) 0.666(2) 0.126(2) 0.162(4) 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 Y1 0.0363(3) 0.0513(4) 0.0485(4) 0.0276(3) 0.0191(3) 0.0107(2) Si1 0.0464(9) 0.0556(10) 0.0630(11) 0.0256(9) 0.0254(9) 0.0078(8) Si2 0.0413(9) 0.0641(11) 0.0600(11) 0.0220(9) 0.0276(8) 0.0133(8) Si3 0.0558(10) 0.0564(10) 0.0475(10) 0.0281(8) 0.0229(8) 0.0133(8) Si4 0.0582(11) 0.0464(9) 0.0599(11) 0.0201(8) 0.0279(9) 0.0067(8) N1 0.054(3) 0.058(3) 0.047(3) 0.027(2) 0.026(2) 0.022(2) N2 0.041(3) 0.067(3) 0.043(3) 0.025(2) 0.018(2) 0.015(2) N3 0.041(2) 0.049(3) 0.045(3) 0.019(2) 0.023(2) 0.014(2) N4 0.053(3) 0.046(3) 0.039(3) 0.017(2) 0.021(2) 0.008(2) C1 0.034(3) 0.046(3) 0.057(4) 0.026(3) 0.022(3) 0.006(3) C2 0.037(3) 0.063(4) 0.038(3) 0.018(3) 0.012(3) 0.016(3) C3 0.043(3) 0.066(4) 0.055(4) 0.030(3) 0.018(3) 0.013(3) C4 0.065(4) 0.094(6) 0.049(4) 0.020(4) 0.029(3) 0.025(4) C5 0.053(4) 0.095(6) 0.062(5) 0.007(4) 0.019(4) 0.033(4) C6 0.056(4) 0.054(4) 0.069(5) 0.010(3) 0.015(4) 0.019(3) C7 0.048(3) 0.061(4) 0.057(4) 0.027(3) 0.014(3) 0.016(3) C8 0.059(4) 0.085(5) 0.073(5) 0.039(4) 0.038(4) 0.019(4) C9 0.073(5) 0.075(5) 0.082(5) 0.047(4) 0.037(4) 0.020(4) C10 0.049(3) 0.064(4) 0.047(4) 0.023(3) 0.020(3) 0.029(3) C11 0.062(4) 0.068(4) 0.059(4) 0.021(4) 0.014(4) 0.023(4) C12 0.097(7) 0.090(6) 0.060(5) 0.003(4) 0.012(5) 0.038(5) C13 0.155(10) 0.123(8) 0.052(5) 0.014(5) 0.035(6) 0.087(8) C14 0.127(8) 0.138(8) 0.068(6) 0.054(6) 0.060(6) 0.083(7) C15 0.068(4) 0.075(4) 0.067(5) 0.036(4) 0.038(4) 0.037(4) C16 0.061(5) 0.079(5) 0.100(6) 0.023(5) 0.016(4) 0.007(4) C17 0.070(5) 0.120(7) 0.087(6) 0.058(5) 0.045(4) 0.035(5) C18 0.039(3) 0.054(3) 0.049(3) 0.024(3) 0.018(3) 0.019(3) C19 0.044(3) 0.081(4) 0.050(4) 0.032(3) 0.018(3) 0.014(3) C20 0.048(4) 0.107(6) 0.067(5) 0.041(4) 0.026(4) 0.026(4) C21 0.060(4) 0.112(6) 0.070(5) 0.044(4) 0.019(4) 0.046(4) C22 0.086(5) 0.110(6) 0.068(5) 0.061(5) 0.040(4) 0.046(5) C23 0.058(4) 0.082(5) 0.059(4) 0.040(4) 0.028(3) 0.027(4) C24 0.052(4) 0.073(5) 0.102(6) 0.014(4) 0.020(4) -0.003(4) C25 0.082(5) 0.049(4) 0.082(5) 0.021(3) 0.040(4) 0.021(4) C26 0.090(6) 0.084(5) 0.110(7) 0.061(5) 0.056(5) 0.022(5) C27 0.053(4) 0.092(5) 0.088(5) 0.024(4) 0.043(4) 0.014(4) C28 0.056(4) 0.061(4) 0.067(4) 0.009(3) 0.033(3) 0.014(3) C29 0.061(4) 0.091(5) 0.081(5) 0.034(4) 0.029(4) 0.028(4) C30 0.072(4) 0.053(4) 0.043(3) 0.011(3) 0.022(3) 0.007(3) C31 0.073(5) 0.079(5) 0.060(4) 0.029(4) 0.019(4) 0.021(4) C32 0.088(5) 0.072(4) 0.068(5) 0.039(4) 0.046(4) 0.020(4) C33 0.138(8) 0.054(4) 0.096(6) 0.038(4) 0.056(6) 0.024(5) C34 0.072(5) 0.085(6) 0.107(7) 0.014(5) 0.042(5) -0.007(4) C35 0.087(5) 0.066(4) 0.061(4) 0.006(4) 0.030(4) -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 Y1 N4 2.225(5) . ? Y1 N3 2.228(5) . ? Y1 N1 2.337(5) . ? Y1 N2 2.343(5) . ? Y1 C1 2.775(6) . ? Y1 Si2 3.198(2) . ? Y1 Si3 3.212(2) . ? Si1 N3 1.719(5) . ? Si1 C26 1.867(7) . ? Si1 C24 1.875(7) . ? Si1 C25 1.875(7) . ? Si2 N3 1.714(5) . ? Si2 C27 1.870(7) . ? Si2 C28 1.874(6) . ? Si2 C29 1.875(7) . ? Si3 N4 1.710(5) . ? Si3 C32 1.865(7) . ? Si3 C31 1.867(7) . ? Si3 C30 1.881(6) . ? Si4 N4 1.723(5) . ? Si4 C33 1.867(8) . ? Si4 C35 1.879(7) . ? Si4 C34 1.882(8) . ? N1 C1 1.334(7) . ? N1 C2 1.418(7) . ? N2 C1 1.346(7) . ? N2 C10 1.432(7) . ? C1 C18 1.497(8) . ? C2 C7 1.405(8) . ? C2 C3 1.412(8) . ? C3 C4 1.398(9) . ? C3 C8 1.508(9) . ? C4 C5 1.365(11) . ? C4 H4 0.9300 . ? C5 C6 1.380(10) . ? C5 H5 0.9300 . ? C6 C7 1.406(9) . ? C6 H6 0.9300 . ? C7 C9 1.504(9) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C15 1.402(9) . ? C10 C11 1.405(9) . ? C11 C12 1.399(10) . ? C11 C16 1.492(11) . ? C12 C13 1.342(14) . ? C12 H12 0.9300 . ? C13 C14 1.365(14) . ? C13 H13 0.9300 . ? C14 C15 1.400(11) . ? C14 H14 0.9300 . ? C15 C17 1.489(10) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C23 1.371(8) . ? C18 C19 1.399(8) . ? C19 C20 1.390(9) . ? C19 H19 0.9300 . ? C20 C21 1.377(10) . ? C20 H20 0.9300 . ? C21 C22 1.367(10) . ? C21 H21 0.9300 . ? C22 C23 1.387(9) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C39 0.68(4) 2_665 ? C36 C40 0.90(4) 2_665 ? C36 C37 1.396(18) . ? C36 C41 1.407(18) . ? C36 C42 1.511(18) . ? C36 C38 1.52(5) 2_665 ? C36 C41 1.82(4) 2_665 ? C37 C40 0.73(4) 2_665 ? C37 C41 0.86(4) 2_665 ? C37 C38 1.419(18) . ? C37 C39 2.03(4) 2_665 ? C38 C41 0.80(4) 2_665 ? C38 C39 1.387(18) . ? C38 C36 1.52(5) 2_665 ? C39 C36 0.68(4) 2_665 ? C39 C42 1.04(4) 2_665 ? C39 C40 1.421(18) . ? C39 C41 1.63(5) 2_665 ? C39 C37 2.03(4) 2_665 ? C40 C37 0.73(4) 2_665 ? C40 C36 0.90(4) 2_665 ? C40 C41 1.384(18) . ? C40 C42 1.86(4) 2_665 ? C41 C38 0.80(4) 2_665 ? C41 C37 0.86(4) 2_665 ? C41 C39 1.63(5) 2_665 ? C41 C36 1.82(4) 2_665 ? C42 C39 1.04(4) 2_665 ? C42 C40 1.86(4) 2_665 ? 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 N3 123.76(16) . . ? N4 Y1 N1 111.22(17) . . ? N3 Y1 N1 116.76(17) . . ? N4 Y1 N2 117.37(17) . . ? N3 Y1 N2 112.30(17) . . ? N1 Y1 N2 57.59(16) . . ? N4 Y1 C1 117.82(17) . . ? N3 Y1 C1 118.39(16) . . ? N1 Y1 C1 28.65(16) . . ? N2 Y1 C1 28.94(16) . . ? N4 Y1 Si2 105.18(13) . . ? N3 Y1 Si2 30.71(12) . . ? N1 Y1 Si2 143.17(12) . . ? N2 Y1 Si2 109.67(12) . . ? C1 Y1 Si2 130.63(12) . . ? N4 Y1 Si3 30.26(12) . . ? N3 Y1 Si3 104.71(12) . . ? N1 Y1 Si3 108.15(12) . . ? N2 Y1 Si3 142.85(12) . . ? C1 Y1 Si3 129.04(12) . . ? Si2 Y1 Si3 100.31(5) . . ? N3 Si1 C26 110.6(3) . . ? N3 Si1 C24 113.1(3) . . ? C26 Si1 C24 107.8(4) . . ? N3 Si1 C25 111.5(3) . . ? C26 Si1 C25 107.6(4) . . ? C24 Si1 C25 106.0(4) . . ? N3 Si2 C27 114.9(3) . . ? N3 Si2 C28 105.9(3) . . ? C27 Si2 C28 106.7(3) . . ? N3 Si2 C29 113.8(3) . . ? C27 Si2 C29 107.7(3) . . ? C28 Si2 C29 107.4(3) . . ? N3 Si2 Y1 41.58(15) . . ? C27 Si2 Y1 134.6(3) . . ? C28 Si2 Y1 65.2(2) . . ? C29 Si2 Y1 117.4(2) . . ? N4 Si3 C32 115.3(3) . . ? N4 Si3 C31 113.2(3) . . ? C32 Si3 C31 107.6(3) . . ? N4 Si3 C30 105.9(3) . . ? C32 Si3 C30 107.1(3) . . ? C31 Si3 C30 107.3(3) . . ? N4 Si3 Y1 40.97(16) . . ? C32 Si3 Y1 135.2(2) . . ? C31 Si3 Y1 116.8(2) . . ? C30 Si3 Y1 65.86(19) . . ? N4 Si4 C33 113.7(3) . . ? N4 Si4 C35 111.3(3) . . ? C33 Si4 C35 105.7(4) . . ? N4 Si4 C34 111.6(3) . . ? C33 Si4 C34 106.6(4) . . ? C35 Si4 C34 107.7(4) . . ? C1 N1 C2 122.0(5) . . ? C1 N1 Y1 94.2(3) . . ? C2 N1 Y1 143.5(4) . . ? C1 N2 C10 121.8(5) . . ? C1 N2 Y1 93.7(3) . . ? C10 N2 Y1 144.2(4) . . ? Si2 N3 Si1 122.1(3) . . ? Si2 N3 Y1 107.7(2) . . ? Si1 N3 Y1 130.0(2) . . ? Si3 N4 Si4 122.2(3) . . ? Si3 N4 Y1 108.8(2) . . ? Si4 N4 Y1 128.9(2) . . ? N1 C1 N2 114.5(5) . . ? N1 C1 C18 123.4(5) . . ? N2 C1 C18 122.0(5) . . ? N1 C1 Y1 57.1(3) . . ? N2 C1 Y1 57.4(3) . . ? C18 C1 Y1 179.4(4) . . ? C7 C2 C3 120.5(6) . . ? C7 C2 N1 121.2(5) . . ? C3 C2 N1 118.3(5) . . ? C4 C3 C2 118.5(6) . . ? C4 C3 C8 119.9(6) . . ? C2 C3 C8 121.7(6) . . ? C5 C4 C3 121.1(7) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 120.8(7) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C7 120.3(7) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C2 C7 C6 118.7(6) . . ? C2 C7 C9 122.1(6) . . ? C6 C7 C9 119.1(6) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 121.2(6) . . ? C15 C10 N2 118.3(6) . . ? C11 C10 N2 120.5(6) . . ? C12 C11 C10 117.6(8) . . ? C12 C11 C16 120.3(8) . . ? C10 C11 C16 122.1(6) . . ? C13 C12 C11 120.6(9) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 122.9(9) . . ? C12 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C13 C14 C15 119.3(9) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C10 118.4(8) . . ? C14 C15 C17 120.9(8) . . ? C10 C15 C17 120.7(6) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 118.3(5) . . ? C23 C18 C1 122.4(5) . . ? C19 C18 C1 119.4(5) . . ? C20 C19 C18 120.7(6) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 119.5(6) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C22 C21 C20 120.3(6) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.1(7) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C18 C23 C22 121.1(6) . . ? C18 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si3 C30 H30A 109.5 . . ? Si3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si4 C33 H33A 109.5 . . ? Si4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si4 C34 H34A 109.5 . . ? Si4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si4 C35 H35A 109.5 . . ? Si4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C39 C36 C40 129(6) 2_665 2_665 ? C39 C36 C37 155(5) 2_665 . ? C40 C36 C37 27(3) 2_665 . ? C39 C36 C41 97(4) 2_665 . ? C40 C36 C41 134(3) 2_665 . ? C37 C36 C41 109(2) . . ? C39 C36 C42 36(3) 2_665 . ? C40 C36 C42 98(4) 2_665 . ? C37 C36 C42 120(3) . . ? C41 C36 C42 128(3) . . ? C39 C36 C38 66(4) 2_665 2_665 ? C40 C36 C38 159(4) 2_665 2_665 ? C37 C36 C38 139(2) . 2_665 ? C41 C36 C38 31.6(16) . 2_665 ? C42 C36 C38 100(3) . 2_665 ? C39 C36 C41 165(7) 2_665 2_665 ? C40 C36 C41 48(2) 2_665 2_665 ? C37 C36 C41 27.2(18) . 2_665 ? C41 C36 C41 86(2) . 2_665 ? C42 C36 C41 145(3) . 2_665 ? C38 C36 C41 114(3) 2_665 2_665 ? C40 C37 C41 122(6) 2_665 2_665 ? C40 C37 C36 34(4) 2_665 . ? C41 C37 C36 105(4) 2_665 . ? C40 C37 C38 152(6) 2_665 . ? C41 C37 C38 30(3) 2_665 . ? C36 C37 C38 130(3) . . ? C40 C37 C39 27(4) 2_665 2_665 ? C41 C37 C39 112(4) 2_665 2_665 ? C36 C37 C39 8.2(16) . 2_665 ? C38 C37 C39 138(2) . 2_665 ? C41 C38 C39 92(4) 2_665 . ? C41 C38 C37 33(3) 2_665 . ? C39 C38 C37 116(3) . . ? C41 C38 C36 67(3) 2_665 2_665 ? C39 C38 C36 26.5(17) . 2_665 ? C37 C38 C36 90(2) . 2_665 ? C36 C39 C42 122(5) 2_665 2_665 ? C36 C39 C38 88(5) 2_665 . ? C42 C39 C38 146(4) 2_665 . ? C36 C39 C40 30(4) 2_665 . ? C42 C39 C40 97(3) 2_665 . ? C38 C39 C40 116(3) . . ? C36 C39 C41 59(3) 2_665 2_665 ? C42 C39 C41 158(4) 2_665 2_665 ? C38 C39 C41 29.5(19) . 2_665 ? C40 C39 C41 88(2) . 2_665 ? C36 C39 C37 17(3) 2_665 2_665 ? C42 C39 C37 106(3) 2_665 2_665 ? C38 C39 C37 105(2) . 2_665 ? C40 C39 C37 13(2) . 2_665 ? C41 C39 C37 76.0(16) 2_665 2_665 ? C37 C40 C36 118(6) 2_665 2_665 ? C37 C40 C41 32(4) 2_665 . ? C36 C40 C41 103(4) 2_665 . ? C37 C40 C39 140(6) 2_665 . ? C36 C40 C39 22(3) 2_665 . ? C41 C40 C39 124(3) . . ? C37 C40 C42 152(6) 2_665 2_665 ? C36 C40 C42 54(3) 2_665 2_665 ? C41 C40 C42 157(3) . 2_665 ? C39 C40 C42 33.8(16) . 2_665 ? C38 C41 C37 117(6) 2_665 2_665 ? C38 C41 C40 144(5) 2_665 . ? C37 C41 C40 27(3) 2_665 . ? C38 C41 C36 82(3) 2_665 . ? C37 C41 C36 132(5) 2_665 . ? C40 C41 C36 123(3) . . ? C38 C41 C39 58(3) 2_665 2_665 ? C37 C41 C39 144(5) 2_665 2_665 ? C40 C41 C39 145(3) . 2_665 ? C36 C41 C39 24.4(15) . 2_665 ? C38 C41 C36 153(5) 2_665 2_665 ? C37 C41 C36 48(3) 2_665 2_665 ? C40 C41 C36 28.7(18) . 2_665 ? C36 C41 C36 94(2) . 2_665 ? C39 C41 C36 117(3) 2_665 2_665 ? C39 C42 C36 22(2) 2_665 . ? C39 C42 C40 49(2) 2_665 2_665 ? C36 C42 C40 28.6(18) . 2_665 ? 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 Y1 Si2 N3 -132.1(3) . . . . ? N1 Y1 Si2 N3 39.0(3) . . . . ? N2 Y1 Si2 N3 100.8(3) . . . . ? C1 Y1 Si2 N3 77.4(3) . . . . ? Si3 Y1 Si2 N3 -101.5(2) . . . . ? N4 Y1 Si2 C27 150.5(4) . . . . ? N3 Y1 Si2 C27 -77.4(4) . . . . ? N1 Y1 Si2 C27 -38.4(4) . . . . ? N2 Y1 Si2 C27 23.4(4) . . . . ? C1 Y1 Si2 C27 0.0(4) . . . . ? Si3 Y1 Si2 C27 -178.8(3) . . . . ? N4 Y1 Si2 C28 61.1(3) . . . . ? N3 Y1 Si2 C28 -166.7(4) . . . . ? N1 Y1 Si2 C28 -127.8(3) . . . . ? N2 Y1 Si2 C28 -65.9(3) . . . . ? C1 Y1 Si2 C28 -89.3(3) . . . . ? Si3 Y1 Si2 C28 91.8(3) . . . . ? N4 Y1 Si2 C29 -36.4(3) . . . . ? N3 Y1 Si2 C29 95.7(4) . . . . ? N1 Y1 Si2 C29 134.7(3) . . . . ? N2 Y1 Si2 C29 -163.5(3) . . . . ? C1 Y1 Si2 C29 173.1(3) . . . . ? Si3 Y1 Si2 C29 -5.8(3) . . . . ? N3 Y1 Si3 N4 -133.7(3) . . . . ? N1 Y1 Si3 N4 101.2(3) . . . . ? N2 Y1 Si3 N4 41.3(3) . . . . ? C1 Y1 Si3 N4 78.6(3) . . . . ? Si2 Y1 Si3 N4 -102.5(3) . . . . ? N4 Y1 Si3 C32 -76.4(4) . . . . ? N3 Y1 Si3 C32 149.9(4) . . . . ? N1 Y1 Si3 C32 24.7(4) . . . . ? N2 Y1 Si3 C32 -35.2(4) . . . . ? C1 Y1 Si3 C32 2.2(4) . . . . ? Si2 Y1 Si3 C32 -178.9(3) . . . . ? N4 Y1 Si3 C31 95.2(4) . . . . ? N3 Y1 Si3 C31 -38.4(3) . . . . ? N1 Y1 Si3 C31 -163.6(3) . . . . ? N2 Y1 Si3 C31 136.5(3) . . . . ? C1 Y1 Si3 C31 173.8(3) . . . . ? Si2 Y1 Si3 C31 -7.3(3) . . . . ? N4 Y1 Si3 C30 -166.7(4) . . . . ? N3 Y1 Si3 C30 59.6(3) . . . . ? N1 Y1 Si3 C30 -65.6(3) . . . . ? N2 Y1 Si3 C30 -125.5(3) . . . . ? C1 Y1 Si3 C30 -88.2(3) . . . . ? Si2 Y1 Si3 C30 90.8(2) . . . . ? N4 Y1 N1 C1 -109.5(3) . . . . ? N3 Y1 N1 C1 100.8(3) . . . . ? N2 Y1 N1 C1 0.2(3) . . . . ? Si2 Y1 N1 C1 79.7(4) . . . . ? Si3 Y1 N1 C1 -141.5(3) . . . . ? N4 Y1 N1 C2 77.7(7) . . . . ? N3 Y1 N1 C2 -72.0(7) . . . . ? N2 Y1 N1 C2 -172.5(7) . . . . ? C1 Y1 N1 C2 -172.8(9) . . . . ? Si2 Y1 N1 C2 -93.1(7) . . . . ? Si3 Y1 N1 C2 45.7(7) . . . . ? N4 Y1 N2 C1 98.6(3) . . . . ? N3 Y1 N2 C1 -108.7(3) . . . . ? N1 Y1 N2 C1 -0.2(3) . . . . ? Si2 Y1 N2 C1 -141.5(3) . . . . ? Si3 Y1 N2 C1 76.6(4) . . . . ? N4 Y1 N2 C10 -73.7(7) . . . . ? N3 Y1 N2 C10 79.0(7) . . . . ? N1 Y1 N2 C10 -172.6(7) . . . . ? C1 Y1 N2 C10 -172.4(9) . . . . ? Si2 Y1 N2 C10 46.1(7) . . . . ? Si3 Y1 N2 C10 -95.7(7) . . . . ? C27 Si2 N3 Si1 -46.4(4) . . . . ? C28 Si2 N3 Si1 -163.9(3) . . . . ? C29 Si2 N3 Si1 78.4(4) . . . . ? Y1 Si2 N3 Si1 -176.4(4) . . . . ? C27 Si2 N3 Y1 130.0(3) . . . . ? C28 Si2 N3 Y1 12.5(3) . . . . ? C29 Si2 N3 Y1 -105.2(3) . . . . ? C26 Si1 N3 Si2 84.1(4) . . . . ? C24 Si1 N3 Si2 -37.0(4) . . . . ? C25 Si1 N3 Si2 -156.3(3) . . . . ? C26 Si1 N3 Y1 -91.5(4) . . . . ? C24 Si1 N3 Y1 147.5(4) . . . . ? C25 Si1 N3 Y1 28.2(4) . . . . ? N4 Y1 N3 Si2 59.4(3) . . . . ? N1 Y1 N3 Si2 -155.0(2) . . . . ? N2 Y1 N3 Si2 -91.3(2) . . . . ? C1 Y1 N3 Si2 -122.7(2) . . . . ? Si3 Y1 N3 Si2 85.4(2) . . . . ? N4 Y1 N3 Si1 -124.6(3) . . . . ? N1 Y1 N3 Si1 21.0(4) . . . . ? N2 Y1 N3 Si1 84.8(3) . . . . ? C1 Y1 N3 Si1 53.4(4) . . . . ? Si2 Y1 N3 Si1 176.0(5) . . . . ? Si3 Y1 N3 Si1 -98.5(3) . . . . ? C32 Si3 N4 Si4 -45.4(4) . . . . ? C31 Si3 N4 Si4 79.1(4) . . . . ? C30 Si3 N4 Si4 -163.6(3) . . . . ? Y1 Si3 N4 Si4 -176.2(5) . . . . ? C32 Si3 N4 Y1 130.8(3) . . . . ? C31 Si3 N4 Y1 -104.7(3) . . . . ? C30 Si3 N4 Y1 12.6(3) . . . . ? C33 Si4 N4 Si3 -38.3(5) . . . . ? C35 Si4 N4 Si3 -157.4(4) . . . . ? C34 Si4 N4 Si3 82.3(5) . . . . ? C33 Si4 N4 Y1 146.4(4) . . . . ? C35 Si4 N4 Y1 27.2(5) . . . . ? C34 Si4 N4 Y1 -93.0(4) . . . . ? N3 Y1 N4 Si3 57.3(3) . . . . ? N1 Y1 N4 Si3 -89.9(3) . . . . ? N2 Y1 N4 Si3 -153.3(2) . . . . ? C1 Y1 N4 Si3 -120.6(2) . . . . ? Si2 Y1 N4 Si3 84.4(2) . . . . ? N3 Y1 N4 Si4 -126.8(3) . . . . ? N1 Y1 N4 Si4 86.0(3) . . . . ? N2 Y1 N4 Si4 22.5(4) . . . . ? C1 Y1 N4 Si4 55.3(4) . . . . ? Si2 Y1 N4 Si4 -99.7(3) . . . . ? Si3 Y1 N4 Si4 175.8(5) . . . . ? C2 N1 C1 N2 174.5(5) . . . . ? Y1 N1 C1 N2 -0.4(5) . . . . ? C2 N1 C1 C18 -5.2(8) . . . . ? Y1 N1 C1 C18 179.8(5) . . . . ? C2 N1 C1 Y1 174.9(6) . . . . ? C10 N2 C1 N1 175.2(5) . . . . ? Y1 N2 C1 N1 0.4(5) . . . . ? C10 N2 C1 C18 -5.1(8) . . . . ? Y1 N2 C1 C18 -179.8(4) . . . . ? C10 N2 C1 Y1 174.8(6) . . . . ? N4 Y1 C1 N1 83.6(4) . . . . ? N3 Y1 C1 N1 -94.5(3) . . . . ? N2 Y1 C1 N1 -179.6(5) . . . . ? Si2 Y1 C1 N1 -129.0(3) . . . . ? Si3 Y1 C1 N1 49.6(4) . . . . ? N4 Y1 C1 N2 -96.9(3) . . . . ? N3 Y1 C1 N2 85.1(4) . . . . ? N1 Y1 C1 N2 179.6(5) . . . . ? Si2 Y1 C1 N2 50.6(4) . . . . ? Si3 Y1 C1 N2 -130.8(3) . . . . ? N4 Y1 C1 C18 -83(44) . . . . ? N3 Y1 C1 C18 99(44) . . . . ? N1 Y1 C1 C18 -167(100) . . . . ? N2 Y1 C1 C18 14(43) . . . . ? Si2 Y1 C1 C18 64(44) . . . . ? Si3 Y1 C1 C18 -117(44) . . . . ? C1 N1 C2 C7 -71.0(7) . . . . ? Y1 N1 C2 C7 100.5(7) . . . . ? C1 N1 C2 C3 111.9(6) . . . . ? Y1 N1 C2 C3 -76.6(8) . . . . ? C7 C2 C3 C4 -0.6(9) . . . . ? N1 C2 C3 C4 176.5(5) . . . . ? C7 C2 C3 C8 178.4(6) . . . . ? N1 C2 C3 C8 -4.4(8) . . . . ? C2 C3 C4 C5 1.4(10) . . . . ? C8 C3 C4 C5 -177.6(6) . . . . ? C3 C4 C5 C6 -2.6(11) . . . . ? C4 C5 C6 C7 3.1(10) . . . . ? C3 C2 C7 C6 1.1(9) . . . . ? N1 C2 C7 C6 -176.0(5) . . . . ? C3 C2 C7 C9 178.9(6) . . . . ? N1 C2 C7 C9 1.8(9) . . . . ? C5 C6 C7 C2 -2.3(9) . . . . ? C5 C6 C7 C9 179.9(6) . . . . ? C1 N2 C10 C15 111.4(6) . . . . ? Y1 N2 C10 C15 -77.6(8) . . . . ? C1 N2 C10 C11 -70.4(8) . . . . ? Y1 N2 C10 C11 100.6(7) . . . . ? C15 C10 C11 C12 -3.3(9) . . . . ? N2 C10 C11 C12 178.5(6) . . . . ? C15 C10 C11 C16 178.4(6) . . . . ? N2 C10 C11 C16 0.3(9) . . . . ? C10 C11 C12 C13 2.8(12) . . . . ? C16 C11 C12 C13 -179.0(8) . . . . ? C11 C12 C13 C14 -0.4(14) . . . . ? C12 C13 C14 C15 -1.6(14) . . . . ? C13 C14 C15 C10 1.0(11) . . . . ? C13 C14 C15 C17 -177.1(7) . . . . ? C11 C10 C15 C14 1.5(9) . . . . ? N2 C10 C15 C14 179.7(6) . . . . ? C11 C10 C15 C17 179.6(6) . . . . ? N2 C10 C15 C17 -2.2(9) . . . . ? N1 C1 C18 C23 128.4(7) . . . . ? N2 C1 C18 C23 -51.3(8) . . . . ? Y1 C1 C18 C23 -65(44) . . . . ? N1 C1 C18 C19 -50.9(8) . . . . ? N2 C1 C18 C19 129.4(6) . . . . ? Y1 C1 C18 C19 116(44) . . . . ? C23 C18 C19 C20 0.1(10) . . . . ? C1 C18 C19 C20 179.4(6) . . . . ? C18 C19 C20 C21 -0.9(11) . . . . ? C19 C20 C21 C22 0.8(12) . . . . ? C20 C21 C22 C23 0.0(12) . . . . ? C19 C18 C23 C22 0.8(10) . . . . ? C1 C18 C23 C22 -178.5(6) . . . . ? C21 C22 C23 C18 -0.9(12) . . . . ? C39 C36 C37 C40 22(15) 2_665 . . 2_665 ? C41 C36 C37 C40 -161(9) . . . 2_665 ? C42 C36 C37 C40 37(7) . . . 2_665 ? C38 C36 C37 C40 -151(10) 2_665 . . 2_665 ? C41 C36 C37 C40 -125(10) 2_665 . . 2_665 ? C39 C36 C37 C41 147(16) 2_665 . . 2_665 ? C40 C36 C37 C41 125(10) 2_665 . . 2_665 ? C41 C36 C37 C41 -36(7) . . . 2_665 ? C42 C36 C37 C41 162(5) . . . 2_665 ? C38 C36 C37 C41 -26(7) 2_665 . . 2_665 ? C39 C36 C37 C38 165(15) 2_665 . . . ? C40 C36 C37 C38 143(9) 2_665 . . . ? C41 C36 C37 C38 -17(6) . . . . ? C42 C36 C37 C38 -180(3) . . . . ? C38 C36 C37 C38 -8(8) 2_665 . . . ? C41 C36 C37 C38 18(4) 2_665 . . . ? C40 C36 C37 C39 -22(15) 2_665 . . 2_665 ? C41 C36 C37 C39 178(19) . . . 2_665 ? C42 C36 C37 C39 16(14) . . . 2_665 ? C38 C36 C37 C39 -173(21) 2_665 . . 2_665 ? C41 C36 C37 C39 -147(16) 2_665 . . 2_665 ? C40 C37 C38 C41 8(11) 2_665 . . 2_665 ? C36 C37 C38 C41 -37(7) . . . 2_665 ? C39 C37 C38 C41 -34(7) 2_665 . . 2_665 ? C40 C37 C38 C39 55(13) 2_665 . . . ? C41 C37 C38 C39 47(7) 2_665 . . . ? C36 C37 C38 C39 10(5) . . . . ? C39 C37 C38 C39 13(6) 2_665 . . . ? C40 C37 C38 C36 50(12) 2_665 . . 2_665 ? C41 C37 C38 C36 42(6) 2_665 . . 2_665 ? C36 C37 C38 C36 5(5) . . . 2_665 ? C39 C37 C38 C36 8(4) 2_665 . . 2_665 ? C41 C38 C39 C36 13(7) 2_665 . . 2_665 ? C37 C38 C39 C36 -11(7) . . . 2_665 ? C41 C38 C39 C42 -139(8) 2_665 . . 2_665 ? C37 C38 C39 C42 -162(7) . . . 2_665 ? C36 C38 C39 C42 -151(13) 2_665 . . 2_665 ? C41 C38 C39 C40 22(5) 2_665 . . . ? C37 C38 C39 C40 -1(5) . . . . ? C36 C38 C39 C40 9(5) 2_665 . . . ? C37 C38 C39 C41 -23(4) . . . 2_665 ? C36 C38 C39 C41 -13(7) 2_665 . . 2_665 ? C41 C38 C39 C37 14(5) 2_665 . . 2_665 ? C37 C38 C39 C37 -9(4) . . . 2_665 ? C36 C38 C39 C37 2(4) 2_665 . . 2_665 ? C36 C39 C40 C37 -16(11) 2_665 . . 2_665 ? C42 C39 C40 C37 134(9) 2_665 . . 2_665 ? C38 C39 C40 C37 -35(10) . . . 2_665 ? C41 C39 C40 C37 -25(8) 2_665 . . 2_665 ? C42 C39 C40 C36 150(12) 2_665 . . 2_665 ? C38 C39 C40 C36 -19(9) . . . 2_665 ? C41 C39 C40 C36 -9(9) 2_665 . . 2_665 ? C37 C39 C40 C36 16(11) 2_665 . . 2_665 ? C36 C39 C40 C41 22(10) 2_665 . . . ? C42 C39 C40 C41 172(4) 2_665 . . . ? C38 C39 C40 C41 3(5) . . . . ? C41 C39 C40 C41 14(4) 2_665 . . . ? C37 C39 C40 C41 38(7) 2_665 . . . ? C36 C39 C40 C42 -150(12) 2_665 . . 2_665 ? C38 C39 C40 C42 -169(6) . . . 2_665 ? C41 C39 C40 C42 -159(4) 2_665 . . 2_665 ? C37 C39 C40 C42 -134(9) 2_665 . . 2_665 ? C37 C40 C41 C38 -7(9) 2_665 . . 2_665 ? C36 C40 C41 C38 -130(9) 2_665 . . 2_665 ? C39 C40 C41 C38 -138(8) . . . 2_665 ? C42 C40 C41 C38 -127(9) 2_665 . . 2_665 ? C36 C40 C41 C37 -123(10) 2_665 . . 2_665 ? C39 C40 C41 C37 -131(10) . . . 2_665 ? C42 C40 C41 C37 -120(12) 2_665 . . 2_665 ? C37 C40 C41 C36 119(9) 2_665 . . . ? C36 C40 C41 C36 -4(7) 2_665 . . . ? C39 C40 C41 C36 -12(6) . . . . ? C42 C40 C41 C36 -1(11) 2_665 . . . ? C37 C40 C41 C39 107(10) 2_665 . . 2_665 ? C36 C40 C41 C39 -16(7) 2_665 . . 2_665 ? C39 C40 C41 C39 -24(7) . . . 2_665 ? C42 C40 C41 C39 -13(11) 2_665 . . 2_665 ? C37 C40 C41 C36 123(10) 2_665 . . 2_665 ? C39 C40 C41 C36 -8(4) . . . 2_665 ? C42 C40 C41 C36 3(5) 2_665 . . 2_665 ? C39 C36 C41 C38 -13(7) 2_665 . . 2_665 ? C40 C36 C41 C38 156(8) 2_665 . . 2_665 ? C37 C36 C41 C38 168(4) . . . 2_665 ? C42 C36 C41 C38 -32(6) . . . 2_665 ? C41 C36 C41 C38 153(5) 2_665 . . 2_665 ? C39 C36 C41 C37 -132(7) 2_665 . . 2_665 ? C40 C36 C41 C37 37(10) 2_665 . . 2_665 ? C37 C36 C41 C37 49(8) . . . 2_665 ? C42 C36 C41 C37 -151(5) . . . 2_665 ? C38 C36 C41 C37 -119(8) 2_665 . . 2_665 ? C41 C36 C41 C37 33(5) 2_665 . . 2_665 ? C39 C36 C41 C40 -164(5) 2_665 . . . ? C40 C36 C41 C40 5(10) 2_665 . . . ? C37 C36 C41 C40 17(6) . . . . ? C42 C36 C41 C40 178(3) . . . . ? C38 C36 C41 C40 -151(6) 2_665 . . . ? C41 C36 C41 C40 2(4) 2_665 . . . ? C40 C36 C41 C39 169(12) 2_665 . . 2_665 ? C37 C36 C41 C39 -179(8) . . . 2_665 ? C42 C36 C41 C39 -19(4) . . . 2_665 ? C38 C36 C41 C39 13(7) 2_665 . . 2_665 ? C41 C36 C41 C39 165(7) 2_665 . . 2_665 ? C39 C36 C41 C36 -165(7) 2_665 . . 2_665 ? C40 C36 C41 C36 4(7) 2_665 . . 2_665 ? C37 C36 C41 C36 16(3) . . . 2_665 ? C42 C36 C41 C36 176(4) . . . 2_665 ? C38 C36 C41 C36 -153(5) 2_665 . . 2_665 ? C41 C36 C41 C36 0.000(2) 2_665 . . 2_665 ? C40 C36 C42 C39 -152(11) 2_665 . . 2_665 ? C37 C36 C42 C39 -169(10) . . . 2_665 ? C41 C36 C42 C39 33(7) . . . 2_665 ? C38 C36 C42 C39 17(7) 2_665 . . 2_665 ? C41 C36 C42 C39 -154(12) 2_665 . . 2_665 ? C39 C36 C42 C40 152(11) 2_665 . . 2_665 ? C37 C36 C42 C40 -16(4) . . . 2_665 ? C41 C36 C42 C40 -174(7) . . . 2_665 ? C38 C36 C42 C40 169(6) 2_665 . . 2_665 ? C41 C36 C42 C40 -2(3) 2_665 . . 2_665 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.958 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.085