# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Jun Okuda' 'Waldemar Fegler' 'Thomas P. Spaniol' _publ_contact_author_name 'Jun Okuda' _publ_contact_author_email JUN.OKUDA@AC.RWTH-AACHEN.DE _publ_section_title ; Trimethylsilylmethyl complexes of the rare-earth metals with sterically hindered N-heterocyclic carbene ligands: Adduct formation and C-H bond activation ; # Attachment 'Ln_NHC_Dalton.cif' data_3a _database_code_depnum_ccdc_archive 'CCDC 763325' #TrackingRef 'Ln_NHC_Dalton.cif' # start Validation Reply Form _vrf_PLAT220_3a ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.72 Ratio RESPONSE: The fact that atoms in the periphery of large organometallic molecules are more dislocated is not surprising. The carbon atoms that belong to the methyl group within the isopropyl fragments, noteworthy C12 are affected with larger displacement parameters than the carbon atoms of the aromatic ring systems such as C1. ; _vrf_PLAT222_3a ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.78 Ratio RESPONSE: Displacement parameters of the hydrogen atoms were calculated based on the values of the carbon atoms to which they are bound. ; _vrf_PLAT242_3a ; PROBLEM: Check Low Ueq as Compared to Neighbors for C10 RESPONSE: C10 is directly bound to C11 and C12, which are the carbon atoms from the methyl groups of the isopropyl fragments. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H69 N2 Si3 Y' _chemical_formula_sum 'C39 H69 N2 Si3 Y' _chemical_formula_weight 739.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6036(6) _cell_length_b 18.8246(10) _cell_length_c 19.2411(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.7906(9) _cell_angle_gamma 90.00 _cell_volume 4562.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 8270 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 24.78 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 1.382 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7696 _exptl_absorpt_correction_T_max 0.8196 _exptl_absorpt_process_details 'Platon Mulabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52617 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.1017 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 30.35 _reflns_number_total 13230 _reflns_number_gt 7342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR 97 (Altomare et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _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^)+(0.0414P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13230 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.884 _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 0.408050(16) 0.130350(11) 0.751392(11) 0.02559(6) Uani 1 1 d . . . Si1 Si 0.14184(5) 0.12083(4) 0.66730(3) 0.03374(16) Uani 1 1 d . . . Si2 Si 0.28452(6) 0.13048(4) 0.93319(4) 0.04384(19) Uani 1 1 d . . . Si3 Si 0.43124(5) -0.07362(3) 0.73495(3) 0.02902(15) Uani 1 1 d . . . N1 N 0.62172(13) 0.21556(8) 0.66933(8) 0.0217(4) Uani 1 1 d . . . N2 N 0.66046(13) 0.21551(9) 0.77804(8) 0.0235(4) Uani 1 1 d . . . C1 C 0.58019(15) 0.19821(10) 0.73198(10) 0.0211(5) Uani 1 1 d . . . C2 C 0.72300(17) 0.24273(11) 0.67708(11) 0.0303(5) Uani 1 1 d . . . H2 H 0.7669 0.2585 0.6409 0.036 Uiso 1 1 calc R . . C3 C 0.74773(17) 0.24264(11) 0.74514(11) 0.0310(5) Uani 1 1 d . . . H3 H 0.8125 0.2582 0.7667 0.037 Uiso 1 1 calc R . . C4 C 0.56015(15) 0.21182(11) 0.60445(10) 0.0221(5) Uani 1 1 d . . . C5 C 0.48791(17) 0.26661(11) 0.58980(11) 0.0277(5) Uani 1 1 d . . . C6 C 0.42541(18) 0.26049(12) 0.52961(12) 0.0359(6) Uani 1 1 d . . . H6 H 0.3746 0.2963 0.5185 0.043 Uiso 1 1 calc R . . C7 C 0.43554(19) 0.20353(13) 0.48578(12) 0.0394(6) Uani 1 1 d . . . H7 H 0.3909 0.1999 0.4452 0.047 Uiso 1 1 calc R . . C8 C 0.51006(19) 0.15150(12) 0.50013(12) 0.0357(6) Uani 1 1 d . . . H8 H 0.5173 0.1131 0.4686 0.043 Uiso 1 1 calc R . . C9 C 0.57497(17) 0.15430(11) 0.56018(11) 0.0269(5) Uani 1 1 d . . . C10 C 0.4798(2) 0.33215(13) 0.63610(13) 0.0440(7) Uani 1 1 d . . . H10 H 0.5167 0.3214 0.6817 0.053 Uiso 1 1 calc R . . C11 C 0.3697(3) 0.35456(16) 0.6501(2) 0.1019(15) Uani 1 1 d . . . H11A H 0.3711 0.3905 0.6870 0.153 Uiso 1 1 calc R . . H11B H 0.3287 0.3133 0.6649 0.153 Uiso 1 1 calc R . . H11C H 0.3368 0.3747 0.6077 0.153 Uiso 1 1 calc R . . C12 C 0.5337(3) 0.3946(2) 0.6045(3) 0.162(3) Uani 1 1 d . . . H12A H 0.4924 0.4106 0.5634 0.244 Uiso 1 1 calc R . . H12B H 0.6051 0.3808 0.5908 0.244 Uiso 1 1 calc R . . H12C H 0.5388 0.4333 0.6385 0.244 Uiso 1 1 calc R . . C13 C 0.66126(18) 0.09910(11) 0.57356(11) 0.0323(5) Uani 1 1 d . . . H13 H 0.6787 0.0983 0.6246 0.039 Uiso 1 1 calc R . . C14 C 0.76218(18) 0.11993(13) 0.53560(13) 0.0452(7) Uani 1 1 d . . . H14A H 0.7465 0.1218 0.4854 0.068 Uiso 1 1 calc R . . H14B H 0.8178 0.0846 0.5453 0.068 Uiso 1 1 calc R . . H14C H 0.7866 0.1667 0.5519 0.068 Uiso 1 1 calc R . . C15 C 0.6280(2) 0.02369(12) 0.55128(13) 0.0434(6) Uani 1 1 d . . . H15A H 0.5604 0.0116 0.5721 0.065 Uiso 1 1 calc R . . H15B H 0.6826 -0.0103 0.5670 0.065 Uiso 1 1 calc R . . H15C H 0.6198 0.0217 0.5005 0.065 Uiso 1 1 calc R . . C16 C 0.65432(16) 0.20892(11) 0.85299(10) 0.0250(5) Uani 1 1 d . . . C17 C 0.60971(17) 0.26512(12) 0.88954(11) 0.0304(5) Uani 1 1 d . . . C18 C 0.60413(18) 0.25689(13) 0.96124(12) 0.0399(6) Uani 1 1 d . . . H18 H 0.5746 0.2939 0.9881 0.048 Uiso 1 1 calc R . . C19 C 0.64018(19) 0.19666(15) 0.99389(12) 0.0438(7) Uani 1 1 d . . . H19 H 0.6345 0.1921 1.0428 0.053 Uiso 1 1 calc R . . C20 C 0.68469(19) 0.14255(13) 0.95649(12) 0.0397(6) Uani 1 1 d . . . H20 H 0.7096 0.1011 0.9800 0.048 Uiso 1 1 calc R . . C21 C 0.69382(17) 0.14754(12) 0.88449(11) 0.0299(5) Uani 1 1 d . . . C22 C 0.56956(19) 0.33252(12) 0.85388(13) 0.0402(6) Uani 1 1 d . . . H22 H 0.5631 0.3232 0.8028 0.048 Uiso 1 1 calc R . . C23 C 0.6465(2) 0.39315(15) 0.86570(16) 0.0662(9) Uani 1 1 d . . . H23A H 0.6508 0.4050 0.9153 0.099 Uiso 1 1 calc R . . H23B H 0.6218 0.4347 0.8392 0.099 Uiso 1 1 calc R . . H23C H 0.7169 0.3791 0.8503 0.099 Uiso 1 1 calc R . . C24 C 0.4618(2) 0.35426(17) 0.8787(2) 0.1037(15) Uani 1 1 d . . . H24A H 0.4656 0.3611 0.9292 0.156 Uiso 1 1 calc R . . H24B H 0.4100 0.3170 0.8670 0.156 Uiso 1 1 calc R . . H24C H 0.4400 0.3987 0.8560 0.156 Uiso 1 1 calc R . . C25 C 0.74784(19) 0.08937(12) 0.84395(13) 0.0413(6) Uani 1 1 d . . . H25 H 0.7340 0.0989 0.7933 0.050 Uiso 1 1 calc R . . C26 C 0.7047(2) 0.01584(13) 0.85966(15) 0.0584(8) Uani 1 1 d . . . H26A H 0.7229 0.0033 0.9080 0.088 Uiso 1 1 calc R . . H26B H 0.7359 -0.0190 0.8284 0.088 Uiso 1 1 calc R . . H26C H 0.6273 0.0158 0.8527 0.088 Uiso 1 1 calc R . . C27 C 0.8684(2) 0.09188(17) 0.85768(19) 0.0802(11) Uani 1 1 d . . . H27A H 0.8953 0.1389 0.8453 0.120 Uiso 1 1 calc R . . H27B H 0.9026 0.0556 0.8295 0.120 Uiso 1 1 calc R . . H27C H 0.8844 0.0827 0.9070 0.120 Uiso 1 1 calc R . . C28 C 0.25608(19) 0.17674(13) 0.69236(13) 0.0452(7) Uani 1 1 d . . . H28A H 0.2288 0.2155 0.7216 0.054 Uiso 1 1 calc R . . H28B H 0.2808 0.1992 0.6492 0.054 Uiso 1 1 calc R . . C29 C 0.0160(2) 0.17208(16) 0.65344(15) 0.0596(8) Uani 1 1 d . . . H29A H -0.0023 0.1957 0.6969 0.089 Uiso 1 1 calc R . . H29B H -0.0413 0.1396 0.6390 0.089 Uiso 1 1 calc R . . H29C H 0.0256 0.2079 0.6172 0.089 Uiso 1 1 calc R . . C30 C 0.1683(3) 0.07067(15) 0.58653(14) 0.0679(9) Uani 1 1 d . . . H30A H 0.1920 0.1036 0.5507 0.102 Uiso 1 1 calc R . . H30B H 0.1032 0.0468 0.5701 0.102 Uiso 1 1 calc R . . H30C H 0.2237 0.0352 0.5962 0.102 Uiso 1 1 calc R . . C31 C 0.1152(2) 0.05548(14) 0.73813(12) 0.0464(7) Uani 1 1 d . . . H31A H 0.1789 0.0268 0.7477 0.070 Uiso 1 1 calc R . . H31B H 0.0564 0.0243 0.7234 0.070 Uiso 1 1 calc R . . H31C H 0.0964 0.0811 0.7803 0.070 Uiso 1 1 calc R . . C32 C 0.3898(2) 0.12931(15) 0.87283(13) 0.0529(7) Uani 1 1 d . . . H32A H 0.4309 0.0867 0.8873 0.064 Uiso 1 1 calc R . . H32B H 0.4342 0.1701 0.8883 0.064 Uiso 1 1 calc R . . C33 C 0.1830(3) 0.20153(15) 0.90697(19) 0.0866(11) Uani 1 1 d . . . H33A H 0.2179 0.2480 0.9060 0.130 Uiso 1 1 calc R . . H33B H 0.1264 0.2025 0.9407 0.130 Uiso 1 1 calc R . . H33C H 0.1526 0.1906 0.8607 0.130 Uiso 1 1 calc R . . C34 C 0.3269(3) 0.15425(16) 1.02420(14) 0.0758(11) Uani 1 1 d . . . H34A H 0.3771 0.1186 1.0424 0.114 Uiso 1 1 calc R . . H34B H 0.2646 0.1556 1.0534 0.114 Uiso 1 1 calc R . . H34C H 0.3611 0.2010 1.0245 0.114 Uiso 1 1 calc R . . C35 C 0.2092(2) 0.04549(13) 0.93569(13) 0.0469(7) Uani 1 1 d . . . H35A H 0.1813 0.0341 0.8889 0.070 Uiso 1 1 calc R . . H35B H 0.1502 0.0504 0.9673 0.070 Uiso 1 1 calc R . . H35C H 0.2565 0.0073 0.9522 0.070 Uiso 1 1 calc R . . C36 C 0.4590(2) 0.01847(12) 0.71049(13) 0.0428(6) Uani 1 1 d . . . H36A H 0.4384 0.0201 0.6604 0.051 Uiso 1 1 calc R . . H36B H 0.5375 0.0208 0.7122 0.051 Uiso 1 1 calc R . . C37 C 0.5411(2) -0.13652(13) 0.71454(15) 0.0557(8) Uani 1 1 d . . . H37A H 0.5608 -0.1302 0.6661 0.083 Uiso 1 1 calc R . . H37B H 0.5172 -0.1855 0.7215 0.083 Uiso 1 1 calc R . . H37C H 0.6028 -0.1268 0.7453 0.083 Uiso 1 1 calc R . . C38 C 0.4080(2) -0.08435(15) 0.82963(13) 0.0540(7) Uani 1 1 d . . . H38A H 0.4707 -0.0680 0.8565 0.081 Uiso 1 1 calc R . . H38B H 0.3950 -0.1345 0.8399 0.081 Uiso 1 1 calc R . . H38C H 0.3462 -0.0561 0.8422 0.081 Uiso 1 1 calc R . . C39 C 0.3099(2) -0.10613(14) 0.68615(14) 0.0542(7) Uani 1 1 d . . . H39A H 0.2501 -0.0745 0.6952 0.081 Uiso 1 1 calc R . . H39B H 0.2930 -0.1543 0.7015 0.081 Uiso 1 1 calc R . . H39C H 0.3231 -0.1065 0.6362 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.02162(11) 0.02689(11) 0.02850(12) 0.00017(10) 0.00467(8) -0.00444(10) Si1 0.0275(3) 0.0397(4) 0.0339(4) 0.0052(3) -0.0005(3) 0.0024(3) Si2 0.0587(5) 0.0375(4) 0.0364(4) -0.0083(3) 0.0185(3) -0.0184(4) Si3 0.0289(4) 0.0263(3) 0.0319(4) -0.0009(3) 0.0025(3) 0.0033(3) N1 0.0209(9) 0.0223(9) 0.0220(9) 0.0013(7) 0.0018(7) -0.0004(7) N2 0.0229(10) 0.0247(9) 0.0231(9) 0.0002(7) 0.0009(8) -0.0047(8) C1 0.0240(11) 0.0190(11) 0.0201(11) 0.0001(8) -0.0002(9) 0.0014(9) C2 0.0262(12) 0.0351(13) 0.0299(13) 0.0049(10) 0.0060(10) -0.0095(10) C3 0.0233(12) 0.0361(13) 0.0337(13) 0.0028(11) 0.0009(10) -0.0120(10) C4 0.0195(11) 0.0266(11) 0.0204(11) 0.0050(9) 0.0035(9) -0.0039(9) C5 0.0262(12) 0.0304(12) 0.0269(12) 0.0036(10) 0.0070(10) 0.0028(10) C6 0.0314(13) 0.0426(15) 0.0336(13) 0.0054(11) -0.0012(11) 0.0092(11) C7 0.0378(14) 0.0486(16) 0.0310(13) 0.0003(12) -0.0102(11) 0.0005(12) C8 0.0427(15) 0.0339(13) 0.0302(13) -0.0044(10) -0.0039(11) 0.0026(11) C9 0.0302(12) 0.0265(12) 0.0241(12) 0.0023(9) 0.0009(10) 0.0013(10) C10 0.0498(16) 0.0426(16) 0.0390(15) -0.0065(12) -0.0062(12) 0.0226(13) C11 0.082(3) 0.050(2) 0.178(4) -0.051(2) 0.078(3) -0.0173(18) C12 0.132(4) 0.085(3) 0.279(6) -0.112(4) 0.138(4) -0.073(3) C13 0.0401(14) 0.0301(12) 0.0264(12) -0.0024(10) -0.0039(10) 0.0069(11) C14 0.0341(14) 0.0477(17) 0.0534(17) -0.0038(13) -0.0045(12) 0.0070(12) C15 0.0543(17) 0.0331(14) 0.0428(15) -0.0049(12) 0.0039(13) 0.0071(13) C16 0.0209(11) 0.0318(12) 0.0220(11) 0.0002(9) -0.0027(9) -0.0063(10) C17 0.0256(12) 0.0378(14) 0.0276(12) -0.0063(10) -0.0046(10) -0.0024(10) C18 0.0376(14) 0.0525(16) 0.0291(13) -0.0110(12) -0.0040(11) -0.0004(12) C19 0.0398(15) 0.0700(19) 0.0215(13) 0.0004(13) -0.0011(11) -0.0069(14) C20 0.0369(14) 0.0487(16) 0.0329(14) 0.0126(12) -0.0084(11) -0.0036(12) C21 0.0224(11) 0.0374(14) 0.0298(13) 0.0051(10) -0.0019(10) -0.0038(10) C22 0.0471(16) 0.0348(14) 0.0381(14) -0.0090(11) -0.0088(12) 0.0058(12) C23 0.064(2) 0.0525(18) 0.083(2) 0.0151(17) 0.0007(18) -0.0132(16) C24 0.0382(18) 0.067(2) 0.206(5) 0.046(3) 0.013(2) 0.0157(17) C25 0.0457(16) 0.0340(14) 0.0442(15) 0.0051(12) 0.0008(12) 0.0097(12) C26 0.066(2) 0.0383(16) 0.070(2) -0.0014(14) -0.0039(16) -0.0009(15) C27 0.0389(18) 0.063(2) 0.139(3) -0.016(2) 0.0152(19) 0.0078(16) C28 0.0381(15) 0.0440(15) 0.0538(17) 0.0089(13) 0.0046(13) -0.0011(12) C29 0.0448(17) 0.074(2) 0.060(2) 0.0016(16) -0.0005(15) 0.0159(16) C30 0.095(3) 0.067(2) 0.0412(17) -0.0003(15) 0.0044(16) 0.0195(19) C31 0.0533(17) 0.0454(16) 0.0407(16) -0.0009(12) 0.0073(13) -0.0108(13) C32 0.0572(18) 0.0617(18) 0.0407(15) -0.0136(14) 0.0146(13) -0.0235(15) C33 0.086(3) 0.049(2) 0.127(3) 0.001(2) 0.045(2) 0.0148(18) C34 0.107(3) 0.080(2) 0.0422(17) -0.0299(16) 0.0289(17) -0.049(2) C35 0.0608(18) 0.0446(16) 0.0358(15) -0.0046(12) 0.0123(13) -0.0184(14) C36 0.0397(15) 0.0363(15) 0.0531(17) 0.0009(12) 0.0121(13) -0.0008(12) C37 0.0455(16) 0.0454(17) 0.076(2) -0.0004(15) 0.0065(15) 0.0170(14) C38 0.0567(18) 0.0618(19) 0.0439(16) 0.0102(14) 0.0040(14) -0.0060(15) C39 0.0508(17) 0.0515(17) 0.0597(19) -0.0142(14) -0.0101(14) 0.0034(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 C36 2.345(2) . ? Y1 C32 2.355(2) . ? Y1 C28 2.363(2) . ? Y1 C1 2.555(2) . ? Si1 C28 1.836(3) . ? Si1 C30 1.857(3) . ? Si1 C29 1.869(3) . ? Si1 C31 1.874(2) . ? Si2 C32 1.791(3) . ? Si2 C35 1.862(2) . ? Si2 C34 1.869(3) . ? Si2 C33 1.908(3) . ? Si3 C36 1.833(2) . ? Si3 C38 1.865(3) . ? Si3 C39 1.873(3) . ? Si3 C37 1.873(2) . ? N1 C1 1.369(2) . ? N1 C2 1.379(2) . ? N1 C4 1.451(2) . ? N2 C1 1.363(2) . ? N2 C3 1.384(2) . ? N2 C16 1.452(2) . ? C2 C3 1.337(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C9 1.394(3) . ? C4 C5 1.399(3) . ? C5 C6 1.385(3) . ? C5 C10 1.527(3) . ? C6 C7 1.372(3) . ? C6 H6 0.9500 . ? C7 C8 1.379(3) . ? C7 H7 0.9500 . ? C8 C9 1.396(3) . ? C8 H8 0.9500 . ? C9 C13 1.520(3) . ? C10 C11 1.482(4) . ? C10 C12 1.497(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.537(3) . ? C13 C15 1.537(3) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.390(3) . ? C16 C17 1.398(3) . ? C17 C18 1.392(3) . ? C17 C22 1.521(3) . ? C18 C19 1.367(3) . ? C18 H18 0.9500 . ? C19 C20 1.377(3) . ? C19 H19 0.9500 . ? C20 C21 1.397(3) . ? C20 H20 0.9500 . ? C21 C25 1.518(3) . ? C22 C24 1.510(4) . ? C22 C23 1.511(3) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.521(3) . ? C25 C27 1.535(3) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? 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 C36 Y1 C32 111.21(9) . . ? C36 Y1 C28 113.39(9) . . ? C32 Y1 C28 112.17(10) . . ? C36 Y1 C1 99.04(7) . . ? C32 Y1 C1 104.99(8) . . ? C28 Y1 C1 115.09(7) . . ? C28 Si1 C30 110.57(13) . . ? C28 Si1 C29 113.38(13) . . ? C30 Si1 C29 108.47(13) . . ? C28 Si1 C31 110.01(11) . . ? C30 Si1 C31 108.41(12) . . ? C29 Si1 C31 105.79(13) . . ? C32 Si2 C35 113.27(12) . . ? C32 Si2 C34 114.51(14) . . ? C35 Si2 C34 108.20(12) . . ? C32 Si2 C33 109.98(14) . . ? C35 Si2 C33 105.73(14) . . ? C34 Si2 C33 104.43(16) . . ? C36 Si3 C38 112.98(12) . . ? C36 Si3 C39 109.87(12) . . ? C38 Si3 C39 107.69(13) . . ? C36 Si3 C37 113.31(12) . . ? C38 Si3 C37 106.02(13) . . ? C39 Si3 C37 106.61(13) . . ? C1 N1 C2 111.80(16) . . ? C1 N1 C4 122.49(16) . . ? C2 N1 C4 125.42(17) . . ? C1 N2 C3 112.03(17) . . ? C1 N2 C16 124.31(17) . . ? C3 N2 C16 123.62(17) . . ? N2 C1 N1 102.65(16) . . ? N2 C1 Y1 129.83(13) . . ? N1 C1 Y1 126.72(13) . . ? C3 C2 N1 106.99(18) . . ? C3 C2 H2 126.5 . . ? N1 C2 H2 126.5 . . ? C2 C3 N2 106.52(18) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? C9 C4 C5 123.26(19) . . ? C9 C4 N1 119.03(18) . . ? C5 C4 N1 117.71(18) . . ? C6 C5 C4 117.2(2) . . ? C6 C5 C10 120.6(2) . . ? C4 C5 C10 122.23(19) . . ? C7 C6 C5 121.2(2) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 120.5(2) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C7 C8 C9 121.1(2) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C4 C9 C8 116.68(19) . . ? C4 C9 C13 122.42(19) . . ? C8 C9 C13 120.81(19) . . ? C11 C10 C12 106.8(3) . . ? C11 C10 C5 114.6(2) . . ? C12 C10 C5 111.0(2) . . ? C11 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C5 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 110.08(18) . . ? C9 C13 C15 113.36(19) . . ? C14 C13 C15 108.98(19) . . ? C9 C13 H13 108.1 . . ? C14 C13 H13 108.1 . . ? C15 C13 H13 108.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 123.6(2) . . ? C21 C16 N2 118.34(19) . . ? C17 C16 N2 118.02(18) . . ? C18 C17 C16 116.6(2) . . ? C18 C17 C22 120.9(2) . . ? C16 C17 C22 122.5(2) . . ? C19 C18 C17 121.4(2) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 120.6(2) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 121.1(2) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C16 C21 C20 116.7(2) . . ? C16 C21 C25 122.4(2) . . ? C20 C21 C25 120.9(2) . . ? C24 C22 C23 109.1(2) . . ? C24 C22 C17 111.9(2) . . ? C23 C22 C17 111.1(2) . . ? C24 C22 H22 108.2 . . ? C23 C22 H22 108.2 . . ? C17 C22 H22 108.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 112.7(2) . . ? C21 C25 C27 110.3(2) . . ? C26 C25 C27 110.6(2) . . ? C21 C25 H25 107.7 . . ? C26 C25 H25 107.7 . . ? C27 C25 H25 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 Y1 122.11(12) . . ? Si1 C28 H28A 106.8 . . ? Y1 C28 H28A 106.8 . . ? Si1 C28 H28B 106.8 . . ? Y1 C28 H28B 106.8 . . ? H28A C28 H28B 106.6 . . ? Si1 C29 H29A 109.5 . . ? Si1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si2 C32 Y1 137.77(15) . . ? Si2 C32 H32A 102.7 . . ? Y1 C32 H32A 102.7 . . ? Si2 C32 H32B 102.7 . . ? Y1 C32 H32B 102.7 . . ? H32A C32 H32B 105.0 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si3 C36 Y1 134.96(12) . . ? Si3 C36 H36A 103.4 . . ? Y1 C36 H36A 103.4 . . ? Si3 C36 H36B 103.4 . . ? Y1 C36 H36B 103.4 . . ? H36A C36 H36B 105.3 . . ? Si3 C37 H37A 109.5 . . ? Si3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si3 C38 H38A 109.5 . . ? Si3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si3 C39 H39A 109.5 . . ? Si3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N2 C1 N1 0.2(2) . . . . ? C16 N2 C1 N1 178.04(17) . . . . ? C3 N2 C1 Y1 170.37(14) . . . . ? C16 N2 C1 Y1 -11.8(3) . . . . ? C2 N1 C1 N2 -0.3(2) . . . . ? C4 N1 C1 N2 -174.57(17) . . . . ? C2 N1 C1 Y1 -170.92(14) . . . . ? C4 N1 C1 Y1 14.8(3) . . . . ? C36 Y1 C1 N2 -99.61(18) . . . . ? C32 Y1 C1 N2 15.34(19) . . . . ? C28 Y1 C1 N2 139.17(17) . . . . ? C36 Y1 C1 N1 68.39(17) . . . . ? C32 Y1 C1 N1 -176.66(16) . . . . ? C28 Y1 C1 N1 -52.83(18) . . . . ? C1 N1 C2 C3 0.4(2) . . . . ? C4 N1 C2 C3 174.39(19) . . . . ? N1 C2 C3 N2 -0.2(2) . . . . ? C1 N2 C3 C2 0.0(2) . . . . ? C16 N2 C3 C2 -177.84(19) . . . . ? C1 N1 C4 C9 -102.1(2) . . . . ? C2 N1 C4 C9 84.5(3) . . . . ? C1 N1 C4 C5 77.6(2) . . . . ? C2 N1 C4 C5 -95.8(2) . . . . ? C9 C4 C5 C6 3.1(3) . . . . ? N1 C4 C5 C6 -176.52(18) . . . . ? C9 C4 C5 C10 -174.7(2) . . . . ? N1 C4 C5 C10 5.6(3) . . . . ? C4 C5 C6 C7 -1.1(3) . . . . ? C10 C5 C6 C7 176.8(2) . . . . ? C5 C6 C7 C8 -1.2(4) . . . . ? C6 C7 C8 C9 1.7(4) . . . . ? C5 C4 C9 C8 -2.7(3) . . . . ? N1 C4 C9 C8 176.94(18) . . . . ? C5 C4 C9 C13 173.9(2) . . . . ? N1 C4 C9 C13 -6.5(3) . . . . ? C7 C8 C9 C4 0.2(3) . . . . ? C7 C8 C9 C13 -176.4(2) . . . . ? C6 C5 C10 C11 45.7(3) . . . . ? C4 C5 C10 C11 -136.5(3) . . . . ? C6 C5 C10 C12 -75.4(3) . . . . ? C4 C5 C10 C12 102.4(3) . . . . ? C4 C9 C13 C14 -92.7(2) . . . . ? C8 C9 C13 C14 83.8(3) . . . . ? C4 C9 C13 C15 145.0(2) . . . . ? C8 C9 C13 C15 -38.6(3) . . . . ? C1 N2 C16 C21 95.2(2) . . . . ? C3 N2 C16 C21 -87.2(2) . . . . ? C1 N2 C16 C17 -85.4(2) . . . . ? C3 N2 C16 C17 92.2(2) . . . . ? C21 C16 C17 C18 -1.1(3) . . . . ? N2 C16 C17 C18 179.45(18) . . . . ? C21 C16 C17 C22 178.4(2) . . . . ? N2 C16 C17 C22 -1.0(3) . . . . ? C16 C17 C18 C19 -0.3(3) . . . . ? C22 C17 C18 C19 -179.8(2) . . . . ? C17 C18 C19 C20 0.9(4) . . . . ? C18 C19 C20 C21 -0.3(4) . . . . ? C17 C16 C21 C20 1.8(3) . . . . ? N2 C16 C21 C20 -178.82(18) . . . . ? C17 C16 C21 C25 -176.2(2) . . . . ? N2 C16 C21 C25 3.2(3) . . . . ? C19 C20 C21 C16 -1.0(3) . . . . ? C19 C20 C21 C25 177.0(2) . . . . ? C18 C17 C22 C24 -46.4(3) . . . . ? C16 C17 C22 C24 134.0(3) . . . . ? C18 C17 C22 C23 75.7(3) . . . . ? C16 C17 C22 C23 -103.8(3) . . . . ? C16 C21 C25 C26 -131.0(2) . . . . ? C20 C21 C25 C26 51.1(3) . . . . ? C16 C21 C25 C27 104.8(3) . . . . ? C20 C21 C25 C27 -73.0(3) . . . . ? C30 Si1 C28 Y1 -80.09(17) . . . . ? C29 Si1 C28 Y1 157.84(14) . . . . ? C31 Si1 C28 Y1 39.62(18) . . . . ? C36 Y1 C28 Si1 40.26(17) . . . . ? C32 Y1 C28 Si1 -86.73(16) . . . . ? C1 Y1 C28 Si1 153.31(12) . . . . ? C35 Si2 C32 Y1 71.7(2) . . . . ? C34 Si2 C32 Y1 -163.59(19) . . . . ? C33 Si2 C32 Y1 -46.4(3) . . . . ? C36 Y1 C32 Si2 -106.4(2) . . . . ? C28 Y1 C32 Si2 21.7(2) . . . . ? C1 Y1 C32 Si2 147.4(2) . . . . ? C38 Si3 C36 Y1 -30.8(2) . . . . ? C39 Si3 C36 Y1 89.4(2) . . . . ? C37 Si3 C36 Y1 -151.43(17) . . . . ? C32 Y1 C36 Si3 34.5(2) . . . . ? C28 Y1 C36 Si3 -93.0(2) . . . . ? C1 Y1 C36 Si3 144.55(18) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.768 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.061 #===END data_4b _database_code_depnum_ccdc_archive 'CCDC 763326' #TrackingRef 'Ln_NHC_Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H57 Lu N2 Si3' _chemical_formula_sum 'C33 H57 Lu N2 Si3' _chemical_formula_weight 741.05 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' Lu Lu -0.4720 5.8584 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _space_group_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.1968(12) _cell_length_b 10.4002(7) _cell_length_c 43.071(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.0090(10) _cell_angle_gamma 90.00 _cell_volume 7608.2(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9748 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 30.37 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3056 _exptl_absorpt_coefficient_mu 2.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4968 _exptl_absorpt_correction_T_max 0.7732 _exptl_absorpt_process_details 'Platon Mulabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC microsource' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'APEX Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55858 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -61 _diffrn_reflns_limit_l_max 61 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 30.79 _reflns_number_total 11266 _reflns_number_gt 9820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR-92 (Altomare 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _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^)+(0.0423P)^2^+9.2373P] 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 11266 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.164 _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 Lu1 Lu 0.765648(8) 0.401105(14) 0.628438(3) 0.01777(5) Uani 1 1 d . . . N1 N 0.93468(15) 0.5085(3) 0.67994(6) 0.0165(5) Uani 1 1 d . . . N2 N 0.95788(16) 0.5006(3) 0.63274(6) 0.0167(5) Uani 1 1 d . . . Si1 Si 0.61549(6) 0.46748(10) 0.67836(2) 0.0207(2) Uani 1 1 d . . . Si2 Si 0.74236(6) 0.06977(9) 0.59464(2) 0.01887(19) Uani 1 1 d . . . Si3 Si 0.65148(6) 0.51293(10) 0.55035(2) 0.0205(2) Uani 1 1 d . . . C1 C 0.89879(18) 0.4846(3) 0.64989(7) 0.0145(6) Uani 1 1 d . . . C2 C 1.01322(19) 0.5387(4) 0.68103(8) 0.0236(8) Uani 1 1 d . . . H2 H 1.0498 0.5591 0.6993 0.028 Uiso 1 1 calc R . . C3 C 1.0279(2) 0.5335(4) 0.65106(8) 0.0231(7) Uani 1 1 d . . . H3 H 1.0768 0.5495 0.6441 0.028 Uiso 1 1 calc R . . C4 C 0.89581(18) 0.5066(3) 0.70717(7) 0.0171(6) Uani 1 1 d . . . C5 C 0.8663(2) 0.6234(3) 0.71686(8) 0.0189(7) Uani 1 1 d . . . C6 C 0.8292(2) 0.6201(3) 0.74348(8) 0.0212(7) Uani 1 1 d . . . H6 H 0.8088 0.6976 0.7507 0.025 Uiso 1 1 calc R . . C7 C 0.8211(2) 0.5057(4) 0.75976(7) 0.0218(7) Uani 1 1 d . . . C8 C 0.8514(2) 0.3931(4) 0.74914(8) 0.0230(7) Uani 1 1 d . . . H8 H 0.8460 0.3152 0.7601 0.028 Uiso 1 1 calc R . . C9 C 0.8896(2) 0.3907(3) 0.72285(8) 0.0203(7) Uani 1 1 d . . . C10 C 0.8734(2) 0.7466(4) 0.69945(9) 0.0263(8) Uani 1 1 d . . . H10A H 0.9267 0.7538 0.6942 0.040 Uiso 1 1 calc R . . H10B H 0.8634 0.8194 0.7127 0.040 Uiso 1 1 calc R . . H10C H 0.8349 0.7472 0.6801 0.040 Uiso 1 1 calc R . . C11 C 0.7803(2) 0.5059(4) 0.78823(8) 0.0287(8) Uani 1 1 d . . . H11A H 0.7233 0.5112 0.7815 0.043 Uiso 1 1 calc R . . H11B H 0.7981 0.5801 0.8015 0.043 Uiso 1 1 calc R . . H11C H 0.7931 0.4265 0.8002 0.043 Uiso 1 1 calc R . . C12 C 0.9218(3) 0.2667(4) 0.71153(9) 0.0300(8) Uani 1 1 d . . . H12A H 0.8896 0.2404 0.6917 0.045 Uiso 1 1 calc R . . H12B H 0.9203 0.1995 0.7274 0.045 Uiso 1 1 calc R . . H12C H 0.9763 0.2800 0.7082 0.045 Uiso 1 1 calc R . . C13 C 0.94833(18) 0.4819(3) 0.59889(7) 0.0159(6) Uani 1 1 d . . . C14 C 0.9176(2) 0.5817(3) 0.57925(8) 0.0180(6) Uani 1 1 d . . . C15 C 0.9076(2) 0.5590(3) 0.54697(8) 0.0199(7) Uani 1 1 d . . . H15 H 0.8862 0.6252 0.5330 0.024 Uiso 1 1 calc R . . C16 C 0.9278(2) 0.4427(4) 0.53462(8) 0.0217(7) Uani 1 1 d . . . C17 C 0.9608(2) 0.3477(4) 0.55529(8) 0.0220(7) Uani 1 1 d . . . H17 H 0.9760 0.2686 0.5470 0.026 Uiso 1 1 calc R . . C18 C 0.97226(19) 0.3646(3) 0.58766(8) 0.0192(7) Uani 1 1 d . . . C19 C 0.8988(2) 0.7120(3) 0.59146(9) 0.0264(8) Uani 1 1 d . . . H19A H 0.8736 0.7014 0.6102 0.040 Uiso 1 1 calc R . . H19B H 0.8630 0.7578 0.5752 0.040 Uiso 1 1 calc R . . H19C H 0.9475 0.7615 0.5969 0.040 Uiso 1 1 calc R . . C20 C 0.9131(2) 0.4176(4) 0.49967(9) 0.0332(9) Uani 1 1 d . . . H20A H 0.9557 0.3646 0.4939 0.050 Uiso 1 1 calc R . . H20B H 0.9111 0.4996 0.4883 0.050 Uiso 1 1 calc R . . H20C H 0.8628 0.3724 0.4940 0.050 Uiso 1 1 calc R . . C21 C 1.0106(2) 0.2619(4) 0.60932(9) 0.0289(8) Uani 1 1 d . . . H21A H 1.0035 0.1782 0.5988 0.043 Uiso 1 1 calc R . . H21B H 0.9863 0.2600 0.6284 0.043 Uiso 1 1 calc R . . H21C H 1.0669 0.2804 0.6149 0.043 Uiso 1 1 calc R . . C22 C 0.6943(2) 0.3602(4) 0.66944(8) 0.0235(7) Uani 1 1 d . . . H22A H 0.6706 0.2738 0.6655 0.028 Uiso 1 1 calc R . . H22B H 0.7332 0.3535 0.6889 0.028 Uiso 1 1 calc R . . C23 C 0.6475(2) 0.6406(4) 0.67823(9) 0.0273(8) Uani 1 1 d . . . H23A H 0.6921 0.6544 0.6951 0.041 Uiso 1 1 calc R . . H23B H 0.6037 0.6964 0.6816 0.041 Uiso 1 1 calc R . . H23C H 0.6635 0.6611 0.6579 0.041 Uiso 1 1 calc R . . C24 C 0.5856(3) 0.4414(5) 0.71831(10) 0.0360(10) Uani 1 1 d . . . H24A H 0.5709 0.3511 0.7204 0.054 Uiso 1 1 calc R . . H24B H 0.5405 0.4966 0.7205 0.054 Uiso 1 1 calc R . . H24C H 0.6298 0.4629 0.7347 0.054 Uiso 1 1 calc R . . C25 C 0.5247(2) 0.4435(4) 0.64854(9) 0.0280(8) Uani 1 1 d . . . H25A H 0.5375 0.4565 0.6274 0.042 Uiso 1 1 calc R . . H25B H 0.4843 0.5055 0.6523 0.042 Uiso 1 1 calc R . . H25C H 0.5048 0.3560 0.6503 0.042 Uiso 1 1 calc R . . C26 C 0.8032(2) 0.2095(4) 0.60823(10) 0.0326(9) Uani 1 1 d . . . H26A H 0.8292 0.2341 0.5902 0.039 Uiso 1 1 calc R . . H26B H 0.8454 0.1755 0.6244 0.039 Uiso 1 1 calc R . . C27 C 0.7508(3) -0.0546(5) 0.62598(10) 0.0432(12) Uani 1 1 d . . . H27A H 0.8063 -0.0770 0.6324 0.065 Uiso 1 1 calc R . . H27B H 0.7214 -0.1315 0.6179 0.065 Uiso 1 1 calc R . . H27C H 0.7292 -0.0210 0.6441 0.065 Uiso 1 1 calc R . . C28 C 0.7724(3) -0.0042(4) 0.55852(9) 0.0366(10) Uani 1 1 d . . . H28A H 0.8288 -0.0241 0.5625 0.055 Uiso 1 1 calc R . . H28B H 0.7617 0.0564 0.5409 0.055 Uiso 1 1 calc R . . H28C H 0.7425 -0.0835 0.5533 0.055 Uiso 1 1 calc R . . C29 C 0.6357(2) 0.1167(4) 0.58422(9) 0.0262(8) Uani 1 1 d . . . H29A H 0.6036 0.0394 0.5791 0.039 Uiso 1 1 calc R . . H29B H 0.6292 0.1743 0.5660 0.039 Uiso 1 1 calc R . . H29C H 0.6186 0.1608 0.6021 0.039 Uiso 1 1 calc R . . C30 C 0.6994(2) 0.5401(4) 0.59121(8) 0.0228(7) Uani 1 1 d . . . H30A H 0.6576 0.5783 0.6017 0.027 Uiso 1 1 calc R . . H30B H 0.7374 0.6103 0.5896 0.027 Uiso 1 1 calc R . . C31 C 0.5484(2) 0.4503(4) 0.54938(10) 0.0285(8) Uani 1 1 d . . . H31A H 0.5157 0.5173 0.5568 0.043 Uiso 1 1 calc R . . H31B H 0.5496 0.3748 0.5630 0.043 Uiso 1 1 calc R . . H31C H 0.5264 0.4262 0.5278 0.043 Uiso 1 1 calc R . . C32 C 0.7077(2) 0.3934(4) 0.52993(9) 0.0298(8) Uani 1 1 d . . . H32A H 0.6797 0.3780 0.5086 0.045 Uiso 1 1 calc R . . H32B H 0.7124 0.3125 0.5417 0.045 Uiso 1 1 calc R . . H32C H 0.7603 0.4273 0.5288 0.045 Uiso 1 1 calc R . . C33 C 0.6443(3) 0.6622(4) 0.52540(10) 0.0373(10) Uani 1 1 d . . . H33A H 0.6127 0.6440 0.5049 0.056 Uiso 1 1 calc R . . H33B H 0.6972 0.6895 0.5225 0.056 Uiso 1 1 calc R . . H33C H 0.6192 0.7309 0.5358 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.01371(7) 0.01889(8) 0.01957(8) -0.00321(6) -0.00098(5) -0.00043(6) N1 0.0121(13) 0.0243(15) 0.0126(12) 0.0015(11) 0.0004(10) -0.0014(11) N2 0.0125(13) 0.0227(14) 0.0140(13) 0.0011(11) -0.0005(10) -0.0012(11) Si1 0.0165(5) 0.0271(5) 0.0174(4) 0.0023(4) -0.0005(4) -0.0023(4) Si2 0.0231(5) 0.0150(4) 0.0190(4) -0.0021(3) 0.0050(4) -0.0013(3) Si3 0.0183(5) 0.0235(5) 0.0189(5) 0.0020(4) 0.0001(4) -0.0028(4) C1 0.0149(15) 0.0161(15) 0.0121(14) -0.0001(11) 0.0012(11) 0.0002(12) C2 0.0103(15) 0.042(2) 0.0168(16) 0.0006(15) -0.0024(12) -0.0056(14) C3 0.0116(15) 0.039(2) 0.0185(16) 0.0015(15) 0.0006(12) -0.0036(14) C4 0.0087(14) 0.0284(18) 0.0130(14) -0.0010(13) -0.0018(11) -0.0034(12) C5 0.0165(16) 0.0222(18) 0.0170(15) -0.0010(12) -0.0003(12) -0.0019(12) C6 0.0170(16) 0.0270(19) 0.0187(16) -0.0030(13) 0.0002(13) -0.0005(13) C7 0.0142(15) 0.039(2) 0.0112(14) -0.0017(14) -0.0005(12) -0.0063(14) C8 0.0249(18) 0.0282(19) 0.0153(15) 0.0047(14) 0.0010(13) -0.0072(15) C9 0.0203(16) 0.0245(18) 0.0147(15) -0.0009(13) -0.0018(12) -0.0015(14) C10 0.032(2) 0.0227(18) 0.0252(18) 0.0013(14) 0.0082(15) 0.0020(15) C11 0.0243(19) 0.045(2) 0.0183(17) -0.0015(16) 0.0066(14) -0.0063(17) C12 0.042(2) 0.0228(19) 0.0254(19) 0.0028(15) 0.0075(17) 0.0039(17) C13 0.0107(14) 0.0222(16) 0.0151(15) -0.0007(12) 0.0030(11) -0.0026(12) C14 0.0169(16) 0.0182(17) 0.0184(15) -0.0007(12) 0.0017(12) -0.0029(12) C15 0.0183(16) 0.0245(17) 0.0159(15) 0.0041(13) -0.0009(13) -0.0028(13) C16 0.0180(17) 0.0318(19) 0.0157(15) -0.0040(14) 0.0036(13) -0.0085(14) C17 0.0184(17) 0.0243(18) 0.0247(18) -0.0069(14) 0.0082(14) -0.0016(14) C18 0.0140(15) 0.0216(16) 0.0221(17) 0.0025(13) 0.0031(13) 0.0012(12) C19 0.032(2) 0.0183(17) 0.0275(19) 0.0021(14) 0.0007(15) -0.0005(15) C20 0.031(2) 0.049(3) 0.0192(17) -0.0068(17) 0.0036(15) -0.0125(18) C21 0.0260(19) 0.026(2) 0.036(2) 0.0058(16) 0.0076(16) 0.0114(15) C22 0.0220(18) 0.0268(18) 0.0210(17) 0.0023(14) 0.0010(14) -0.0019(14) C23 0.0249(19) 0.031(2) 0.0242(18) -0.0011(15) -0.0026(15) -0.0041(15) C24 0.030(2) 0.052(3) 0.027(2) 0.0066(19) 0.0065(17) 0.0023(19) C25 0.0230(19) 0.031(2) 0.0275(19) 0.0056(16) -0.0038(15) -0.0057(15) C26 0.0232(19) 0.027(2) 0.046(2) -0.0115(18) -0.0013(17) 0.0012(16) C27 0.044(3) 0.062(3) 0.025(2) 0.019(2) 0.0112(19) 0.020(2) C28 0.051(3) 0.036(2) 0.025(2) 0.0025(17) 0.0112(18) 0.015(2) C29 0.0242(18) 0.029(2) 0.0257(18) -0.0003(15) 0.0058(15) -0.0067(15) C30 0.0169(17) 0.0264(19) 0.0238(18) 0.0011(14) -0.0009(13) 0.0035(14) C31 0.0182(18) 0.033(2) 0.034(2) 0.0005(17) 0.0024(15) -0.0025(15) C32 0.029(2) 0.035(2) 0.0277(19) -0.0049(16) 0.0104(16) -0.0111(17) C33 0.038(2) 0.033(2) 0.038(2) 0.0123(19) -0.0019(19) -0.0061(19) _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 C26 2.307(4) . ? Lu1 C30 2.321(3) . ? Lu1 C22 2.341(4) . ? Lu1 C1 2.488(3) . ? N1 C1 1.367(4) . ? N1 C2 1.380(4) . ? N1 C4 1.438(4) . ? N2 C1 1.357(4) . ? N2 C3 1.376(4) . ? N2 C13 1.455(4) . ? Si1 C22 1.842(4) . ? Si1 C25 1.877(4) . ? Si1 C23 1.883(4) . ? Si1 C24 1.891(4) . ? Si2 C26 1.832(4) . ? Si2 C27 1.859(4) . ? Si2 C28 1.879(4) . ? Si2 C29 1.884(4) . ? Si3 C30 1.844(4) . ? Si3 C32 1.876(4) . ? Si3 C33 1.881(4) . ? Si3 C31 1.882(4) . ? C2 C3 1.355(5) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C9 1.393(5) . ? C4 C5 1.405(5) . ? C5 C6 1.398(5) . ? C5 C10 1.500(5) . ? C6 C7 1.399(5) . ? C6 H6 0.9500 . ? C7 C8 1.388(5) . ? C7 C11 1.505(5) . ? C8 C9 1.396(5) . ? C8 H8 0.9500 . ? C9 C12 1.513(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.390(5) . ? C13 C18 1.398(5) . ? C14 C15 1.394(5) . ? C14 C19 1.507(5) . ? C15 C16 1.387(5) . ? C15 H15 0.9500 . ? C16 C17 1.390(5) . ? C16 C20 1.509(5) . ? C17 C18 1.388(5) . ? C17 H17 0.9500 . ? C18 C21 1.501(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? 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 C26 Lu1 C30 114.43(14) . . ? C26 Lu1 C22 109.76(15) . . ? C30 Lu1 C22 112.07(13) . . ? C26 Lu1 C1 98.42(12) . . ? C30 Lu1 C1 111.28(12) . . ? C22 Lu1 C1 110.10(11) . . ? C1 N1 C2 111.6(3) . . ? C1 N1 C4 124.8(3) . . ? C2 N1 C4 123.5(3) . . ? C1 N2 C3 112.4(3) . . ? C1 N2 C13 123.5(3) . . ? C3 N2 C13 124.0(3) . . ? C22 Si1 C25 109.73(18) . . ? C22 Si1 C23 110.68(18) . . ? C25 Si1 C23 109.73(18) . . ? C22 Si1 C24 114.63(18) . . ? C25 Si1 C24 106.73(19) . . ? C23 Si1 C24 105.1(2) . . ? C26 Si2 C27 110.1(2) . . ? C26 Si2 C28 111.8(2) . . ? C27 Si2 C28 108.4(2) . . ? C26 Si2 C29 110.89(18) . . ? C27 Si2 C29 108.40(19) . . ? C28 Si2 C29 107.02(19) . . ? C30 Si3 C32 111.29(18) . . ? C30 Si3 C33 113.48(19) . . ? C32 Si3 C33 105.8(2) . . ? C30 Si3 C31 110.63(18) . . ? C32 Si3 C31 108.22(18) . . ? C33 Si3 C31 107.18(19) . . ? N2 C1 N1 103.2(3) . . ? N2 C1 Lu1 124.4(2) . . ? N1 C1 Lu1 131.9(2) . . ? C3 C2 N1 106.6(3) . . ? C3 C2 H2 126.7 . . ? N1 C2 H2 126.7 . . ? C2 C3 N2 106.2(3) . . ? C2 C3 H3 126.9 . . ? N2 C3 H3 126.9 . . ? C9 C4 C5 123.1(3) . . ? C9 C4 N1 119.2(3) . . ? C5 C4 N1 117.7(3) . . ? C6 C5 C4 117.1(3) . . ? C6 C5 C10 121.0(3) . . ? C4 C5 C10 121.9(3) . . ? C5 C6 C7 121.7(3) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C8 C7 C6 118.7(3) . . ? C8 C7 C11 121.1(3) . . ? C6 C7 C11 120.2(3) . . ? C7 C8 C9 122.1(3) . . ? C7 C8 H8 118.9 . . ? C9 C8 H8 118.9 . . ? C4 C9 C8 117.3(3) . . ? C4 C9 C12 121.4(3) . . ? C8 C9 C12 121.3(3) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 123.1(3) . . ? C14 C13 N2 118.8(3) . . ? C18 C13 N2 118.1(3) . . ? C13 C14 C15 117.1(3) . . ? C13 C14 C19 122.8(3) . . ? C15 C14 C19 120.1(3) . . ? C16 C15 C14 122.1(3) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 C17 118.4(3) . . ? C15 C16 C20 121.3(3) . . ? C17 C16 C20 120.2(3) . . ? C18 C17 C16 122.2(3) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C13 117.0(3) . . ? C17 C18 C21 120.9(3) . . ? C13 C18 C21 122.0(3) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 Lu1 122.46(18) . . ? Si1 C22 H22A 106.7 . . ? Lu1 C22 H22A 106.7 . . ? Si1 C22 H22B 106.7 . . ? Lu1 C22 H22B 106.7 . . ? H22A C22 H22B 106.6 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? 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 . . ? Si2 C26 Lu1 128.8(2) . . ? Si2 C26 H26A 105.1 . . ? Lu1 C26 H26A 105.1 . . ? Si2 C26 H26B 105.1 . . ? Lu1 C26 H26B 105.1 . . ? H26A C26 H26B 105.9 . . ? 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 Lu1 131.41(19) . . ? Si3 C30 H30A 104.4 . . ? Lu1 C30 H30A 104.4 . . ? Si3 C30 H30B 104.4 . . ? Lu1 C30 H30B 104.4 . . ? H30A C30 H30B 105.6 . . ? 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 . . ? Si3 C33 H33A 109.5 . . ? Si3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N2 C1 N1 -0.2(4) . . . . ? C13 N2 C1 N1 178.4(3) . . . . ? C3 N2 C1 Lu1 -172.7(2) . . . . ? C13 N2 C1 Lu1 5.9(4) . . . . ? C2 N1 C1 N2 0.2(4) . . . . ? C4 N1 C1 N2 178.5(3) . . . . ? C2 N1 C1 Lu1 172.0(3) . . . . ? C4 N1 C1 Lu1 -9.7(5) . . . . ? C26 Lu1 C1 N2 55.7(3) . . . . ? C30 Lu1 C1 N2 -64.7(3) . . . . ? C22 Lu1 C1 N2 170.4(3) . . . . ? C26 Lu1 C1 N1 -114.5(3) . . . . ? C30 Lu1 C1 N1 125.1(3) . . . . ? C22 Lu1 C1 N1 0.2(3) . . . . ? C1 N1 C2 C3 -0.2(4) . . . . ? C4 N1 C2 C3 -178.5(3) . . . . ? N1 C2 C3 N2 0.1(4) . . . . ? C1 N2 C3 C2 0.1(4) . . . . ? C13 N2 C3 C2 -178.5(3) . . . . ? C1 N1 C4 C9 87.2(4) . . . . ? C2 N1 C4 C9 -94.6(4) . . . . ? C1 N1 C4 C5 -93.3(4) . . . . ? C2 N1 C4 C5 84.8(4) . . . . ? C9 C4 C5 C6 -0.2(5) . . . . ? N1 C4 C5 C6 -179.6(3) . . . . ? C9 C4 C5 C10 -179.7(3) . . . . ? N1 C4 C5 C10 0.9(5) . . . . ? C4 C5 C6 C7 -0.3(5) . . . . ? C10 C5 C6 C7 179.1(3) . . . . ? C5 C6 C7 C8 0.4(5) . . . . ? C5 C6 C7 C11 -179.7(3) . . . . ? C6 C7 C8 C9 0.1(5) . . . . ? C11 C7 C8 C9 -179.8(3) . . . . ? C5 C4 C9 C8 0.7(5) . . . . ? N1 C4 C9 C8 -180.0(3) . . . . ? C5 C4 C9 C12 179.6(3) . . . . ? N1 C4 C9 C12 -1.0(5) . . . . ? C7 C8 C9 C4 -0.6(5) . . . . ? C7 C8 C9 C12 -179.6(3) . . . . ? C1 N2 C13 C14 83.0(4) . . . . ? C3 N2 C13 C14 -98.6(4) . . . . ? C1 N2 C13 C18 -98.4(4) . . . . ? C3 N2 C13 C18 80.0(4) . . . . ? C18 C13 C14 C15 3.0(5) . . . . ? N2 C13 C14 C15 -178.5(3) . . . . ? C18 C13 C14 C19 -174.3(3) . . . . ? N2 C13 C14 C19 4.2(5) . . . . ? C13 C14 C15 C16 -0.6(5) . . . . ? C19 C14 C15 C16 176.8(3) . . . . ? C14 C15 C16 C17 -1.6(5) . . . . ? C14 C15 C16 C20 177.2(3) . . . . ? C15 C16 C17 C18 1.6(5) . . . . ? C20 C16 C17 C18 -177.2(3) . . . . ? C16 C17 C18 C13 0.6(5) . . . . ? C16 C17 C18 C21 -177.9(3) . . . . ? C14 C13 C18 C17 -3.0(5) . . . . ? N2 C13 C18 C17 178.5(3) . . . . ? C14 C13 C18 C21 175.5(3) . . . . ? N2 C13 C18 C21 -3.0(5) . . . . ? C25 Si1 C22 Lu1 75.8(2) . . . . ? C23 Si1 C22 Lu1 -45.5(3) . . . . ? C24 Si1 C22 Lu1 -164.2(2) . . . . ? C26 Lu1 C22 Si1 -148.7(2) . . . . ? C30 Lu1 C22 Si1 -20.5(3) . . . . ? C1 Lu1 C22 Si1 104.0(2) . . . . ? C27 Si2 C26 Lu1 -98.3(3) . . . . ? C28 Si2 C26 Lu1 141.0(3) . . . . ? C29 Si2 C26 Lu1 21.7(3) . . . . ? C30 Lu1 C26 Si2 -75.3(3) . . . . ? C22 Lu1 C26 Si2 51.6(3) . . . . ? C1 Lu1 C26 Si2 166.6(3) . . . . ? C32 Si3 C30 Lu1 -36.4(3) . . . . ? C33 Si3 C30 Lu1 -155.6(2) . . . . ? C31 Si3 C30 Lu1 83.9(3) . . . . ? C26 Lu1 C30 Si3 16.0(3) . . . . ? C22 Lu1 C30 Si3 -109.8(2) . . . . ? C1 Lu1 C30 Si3 126.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.360 _refine_diff_density_min -3.668 _refine_diff_density_rms 0.124 #===END data_5a _database_code_depnum_ccdc_archive 'CCDC 763327' #TrackingRef 'Ln_NHC_Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H61 N2 O2 Si2 Y, C4 H8 O' _chemical_formula_sum 'C41 H69 N2 O3 Si2 Y' _chemical_formula_weight 783.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _space_group_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7592(6) _cell_length_b 11.4858(7) _cell_length_c 19.8393(12) _cell_angle_alpha 102.7225(9) _cell_angle_beta 93.1152(9) _cell_angle_gamma 111.7992(9) _cell_volume 2195.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 9904 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 29.98 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5258 _exptl_absorpt_correction_T_max 0.7645 _exptl_absorpt_process_details 'Platon Mulabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC microsource' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'APEX Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33156 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 30.84 _reflns_number_total 12610 _reflns_number_gt 9399 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR-92 (Altomare 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _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^)+(0.0298P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12610 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0797 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _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 0.324381(15) 0.708229(15) 0.235616(8) 0.01721(5) Uani 1 1 d . . . Si1 Si 0.35967(5) 0.54400(5) 0.37932(3) 0.02166(11) Uani 1 1 d . . . Si2 Si 0.31175(5) 0.40427(5) 0.08960(3) 0.02808(12) Uani 1 1 d . . . O1 O 0.28311(11) 0.77882(11) 0.13032(6) 0.0234(3) Uani 1 1 d . . . O2 O 0.07875(11) 0.63860(11) 0.20699(6) 0.0243(3) Uani 1 1 d . . . O3 O 0.82725(12) 0.36941(12) 0.32051(7) 0.0337(3) Uani 1 1 d . . . N1 N 0.48007(13) 1.04257(12) 0.28041(7) 0.0171(3) Uani 1 1 d . . . N2 N 0.31237(13) 1.02440(13) 0.33561(7) 0.0176(3) Uani 1 1 d . . . C1 C 0.35925(15) 0.95253(15) 0.28765(8) 0.0163(3) Uani 1 1 d . . . C2 C 0.50748(16) 1.16454(16) 0.32338(9) 0.0219(4) Uani 1 1 d . . . H2 H 0.5860 1.2411 0.3275 0.026 Uiso 1 1 calc R . . C3 C 0.40194(16) 1.15379(16) 0.35807(9) 0.0229(4) Uani 1 1 d . . . H3 H 0.3906 1.2211 0.3914 0.027 Uiso 1 1 calc R . . C4 C 0.57045(15) 1.01185(15) 0.23516(8) 0.0170(3) Uani 1 1 d . . . C5 C 0.61402(15) 0.91374(15) 0.24514(8) 0.0176(3) Uani 1 1 d . . . C6 C 0.70297(16) 0.88861(16) 0.19960(9) 0.0213(4) Uani 1 1 d . . . H6 H 0.7328 0.8217 0.2030 0.026 Uiso 1 1 calc R . . C7 C 0.74852(16) 0.95649(17) 0.15044(9) 0.0225(4) Uani 1 1 d . . . C8 C 0.70210(16) 1.05176(17) 0.14308(9) 0.0241(4) Uani 1 1 d . . . H8 H 0.7326 1.0983 0.1090 0.029 Uiso 1 1 calc R . . C9 C 0.61151(16) 1.08023(16) 0.18484(9) 0.0207(4) Uani 1 1 d . . . C10 C 0.85009(18) 0.92994(19) 0.10572(10) 0.0330(5) Uani 1 1 d . . . H10A H 0.8655 0.8553 0.1145 0.049 Uiso 1 1 calc R . . H10B H 0.9357 1.0064 0.1176 0.049 Uiso 1 1 calc R . . H10C H 0.8145 0.9109 0.0562 0.049 Uiso 1 1 calc R . . C11 C 0.56176(18) 1.18295(17) 0.17505(10) 0.0289(4) Uani 1 1 d . . . H11A H 0.4668 1.1566 0.1822 0.043 Uiso 1 1 calc R . . H11B H 0.5695 1.1935 0.1276 0.043 Uiso 1 1 calc R . . H11C H 0.6166 1.2655 0.2090 0.043 Uiso 1 1 calc R . . C12 C 0.56322(15) 0.83777(15) 0.29440(9) 0.0199(4) Uani 1 1 d . . . H12A H 0.5677 0.8934 0.3411 0.024 Uiso 1 1 calc R . . H12B H 0.6125 0.7815 0.2989 0.024 Uiso 1 1 calc R . . C13 C 0.18727(15) 0.97326(15) 0.36301(8) 0.0176(3) Uani 1 1 d . . . C14 C 0.07269(16) 0.98552(16) 0.33451(9) 0.0199(4) Uani 1 1 d . . . C15 C -0.04624(16) 0.93383(16) 0.36202(9) 0.0236(4) Uani 1 1 d . . . H15 H -0.1257 0.9412 0.3438 0.028 Uiso 1 1 calc R . . C16 C -0.05237(17) 0.87225(16) 0.41496(9) 0.0238(4) Uani 1 1 d . . . C17 C 0.06548(17) 0.86572(16) 0.44299(9) 0.0243(4) Uani 1 1 d . . . H17 H 0.0626 0.8251 0.4801 0.029 Uiso 1 1 calc R . . C18 C 0.18735(16) 0.91694(16) 0.41823(9) 0.0209(4) Uani 1 1 d . . . C19 C -0.18287(18) 0.81435(19) 0.44280(10) 0.0342(5) Uani 1 1 d . . . H19A H -0.2308 0.7231 0.4169 0.051 Uiso 1 1 calc R . . H19B H -0.2397 0.8623 0.4371 0.051 Uiso 1 1 calc R . . H19C H -0.1629 0.8200 0.4925 0.051 Uiso 1 1 calc R . . C20 C 0.31576(17) 0.91506(18) 0.45114(10) 0.0288(4) Uani 1 1 d . . . H20A H 0.3453 0.8576 0.4178 0.043 Uiso 1 1 calc R . . H20B H 0.2992 0.8832 0.4931 0.043 Uiso 1 1 calc R . . H20C H 0.3864 1.0031 0.4640 0.043 Uiso 1 1 calc R . . C21 C 0.07612(17) 1.05033(17) 0.27610(9) 0.0274(4) Uani 1 1 d . . . H21A H -0.0135 1.0499 0.2637 0.041 Uiso 1 1 calc R . . H21B H 0.1011 1.0032 0.2353 0.041 Uiso 1 1 calc R . . H21C H 0.1430 1.1401 0.2913 0.041 Uiso 1 1 calc R . . C22 C 0.25285(16) 0.58472(16) 0.32142(9) 0.0224(4) Uani 1 1 d . . . H22A H 0.2073 0.6305 0.3526 0.027 Uiso 1 1 calc R . . H22B H 0.1810 0.5007 0.2952 0.027 Uiso 1 1 calc R . . C23 C 0.47876(18) 0.48226(17) 0.33176(10) 0.0297(4) Uani 1 1 d . . . H23A H 0.4265 0.4053 0.2936 0.045 Uiso 1 1 calc R . . H23B H 0.5319 0.4594 0.3644 0.045 Uiso 1 1 calc R . . H23C H 0.5399 0.5500 0.3126 0.045 Uiso 1 1 calc R . . C24 C 0.46701(17) 0.68705(17) 0.45283(9) 0.0274(4) Uani 1 1 d . . . H24A H 0.5133 0.7615 0.4341 0.041 Uiso 1 1 calc R . . H24B H 0.5343 0.6656 0.4769 0.041 Uiso 1 1 calc R . . H24C H 0.4095 0.7088 0.4858 0.041 Uiso 1 1 calc R . . C25 C 0.26155(18) 0.41656(18) 0.42431(10) 0.0307(4) Uani 1 1 d . . . H25A H 0.1966 0.4439 0.4491 0.046 Uiso 1 1 calc R . . H25B H 0.3244 0.4061 0.4578 0.046 Uiso 1 1 calc R . . H25C H 0.2128 0.3337 0.3894 0.046 Uiso 1 1 calc R . . C26 C 0.39374(18) 0.56008(17) 0.15495(9) 0.0259(4) Uani 1 1 d . . . H26A H 0.4518 0.6166 0.1282 0.031 Uiso 1 1 calc R . . H26B H 0.4572 0.5436 0.1859 0.031 Uiso 1 1 calc R . . C27 C 0.20507(19) 0.41129(19) 0.01306(10) 0.0377(5) Uani 1 1 d . . . H27A H 0.1515 0.4615 0.0301 0.057 Uiso 1 1 calc R . . H27B H 0.1442 0.3230 -0.0127 0.057 Uiso 1 1 calc R . . H27C H 0.2641 0.4530 -0.0180 0.057 Uiso 1 1 calc R . . C28 C 0.4347(2) 0.33813(19) 0.04864(11) 0.0389(5) Uani 1 1 d . . . H28A H 0.4822 0.3914 0.0183 0.058 Uiso 1 1 calc R . . H28B H 0.3850 0.2484 0.0209 0.058 Uiso 1 1 calc R . . H28C H 0.5007 0.3404 0.0855 0.058 Uiso 1 1 calc R . . C29 C 0.2000(2) 0.2775(2) 0.13011(13) 0.0539(6) Uani 1 1 d . . . H29A H 0.2545 0.2676 0.1679 0.081 Uiso 1 1 calc R . . H29B H 0.1575 0.1945 0.0945 0.081 Uiso 1 1 calc R . . H29C H 0.1297 0.3043 0.1490 0.081 Uiso 1 1 calc R . . C30 C 0.36687(18) 0.77967(18) 0.07463(9) 0.0273(4) Uani 1 1 d . . . H30A H 0.3433 0.6904 0.0455 0.033 Uiso 1 1 calc R . . H30B H 0.4640 0.8171 0.0946 0.033 Uiso 1 1 calc R . . C31 C 0.3375(2) 0.8619(2) 0.03186(11) 0.0470(6) Uani 1 1 d . . . H31A H 0.3368 0.8263 -0.0184 0.056 Uiso 1 1 calc R . . H31B H 0.4057 0.9523 0.0469 0.056 Uiso 1 1 calc R . . C32 C 0.1992(2) 0.8559(2) 0.04582(11) 0.0446(6) Uani 1 1 d . . . H32A H 0.1266 0.7759 0.0161 0.054 Uiso 1 1 calc R . . H32B H 0.1848 0.9325 0.0382 0.054 Uiso 1 1 calc R . . C33 C 0.20529(19) 0.85534(19) 0.12194(10) 0.0322(4) Uani 1 1 d . . . H33A H 0.2505 0.9448 0.1524 0.039 Uiso 1 1 calc R . . H33B H 0.1132 0.8154 0.1336 0.039 Uiso 1 1 calc R . . C34 C -0.02009(17) 0.64108(18) 0.25401(10) 0.0323(4) Uani 1 1 d . . . H34A H -0.0071 0.7315 0.2766 0.039 Uiso 1 1 calc R . . H34B H -0.0120 0.5973 0.2908 0.039 Uiso 1 1 calc R . . C35 C -0.15626(18) 0.5693(2) 0.20812(11) 0.0383(5) Uani 1 1 d . . . H35A H -0.1806 0.6264 0.1840 0.046 Uiso 1 1 calc R . . H35B H -0.2286 0.5318 0.2353 0.046 Uiso 1 1 calc R . . C36 C -0.13109(19) 0.4643(2) 0.15699(11) 0.0402(5) Uani 1 1 d . . . H36A H -0.1970 0.4296 0.1134 0.048 Uiso 1 1 calc R . . H36B H -0.1359 0.3921 0.1777 0.048 Uiso 1 1 calc R . . C37 C 0.01114(18) 0.53619(19) 0.14359(10) 0.0347(5) Uani 1 1 d . . . H37A H 0.0589 0.4768 0.1336 0.042 Uiso 1 1 calc R . . H37B H 0.0087 0.5734 0.1033 0.042 Uiso 1 1 calc R . . C38 C 0.8592(2) 0.43947(19) 0.39210(11) 0.0393(5) Uani 1 1 d . . . H38A H 0.7900 0.4743 0.4054 0.047 Uiso 1 1 calc R . . H38B H 0.9486 0.5129 0.4010 0.047 Uiso 1 1 calc R . . C39 C 0.8617(2) 0.34370(19) 0.43369(11) 0.0375(5) Uani 1 1 d . . . H39A H 0.7776 0.3134 0.4545 0.045 Uiso 1 1 calc R . . H39B H 0.9403 0.3837 0.4715 0.045 Uiso 1 1 calc R . . C40 C 0.87301(18) 0.23176(18) 0.37999(10) 0.0306(4) Uani 1 1 d . . . H40A H 0.9505 0.2125 0.3958 0.037 Uiso 1 1 calc R . . H40B H 0.7890 0.1523 0.3713 0.037 Uiso 1 1 calc R . . C41 C 0.89498(18) 0.28157(19) 0.31491(10) 0.0309(4) Uani 1 1 d . . . H41A H 0.9927 0.3273 0.3138 0.037 Uiso 1 1 calc R . . H41B H 0.8551 0.2092 0.2721 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.01499(8) 0.01849(8) 0.01711(8) 0.00605(6) 0.00254(6) 0.00462(6) Si1 0.0195(2) 0.0249(3) 0.0236(3) 0.0112(2) 0.0049(2) 0.0091(2) Si2 0.0302(3) 0.0248(3) 0.0289(3) 0.0046(2) 0.0071(2) 0.0115(2) O1 0.0233(6) 0.0323(7) 0.0202(6) 0.0116(5) 0.0075(5) 0.0139(5) O2 0.0152(6) 0.0298(7) 0.0231(7) 0.0071(5) 0.0028(5) 0.0034(5) O3 0.0297(7) 0.0351(8) 0.0339(8) 0.0147(6) -0.0003(6) 0.0076(6) N1 0.0142(7) 0.0182(7) 0.0189(7) 0.0065(6) 0.0047(6) 0.0051(6) N2 0.0130(7) 0.0190(7) 0.0202(7) 0.0056(6) 0.0040(6) 0.0052(6) C1 0.0137(8) 0.0206(8) 0.0166(8) 0.0081(7) 0.0027(6) 0.0070(7) C2 0.0177(8) 0.0167(8) 0.0273(10) 0.0048(7) 0.0032(7) 0.0030(7) C3 0.0205(9) 0.0164(8) 0.0272(10) 0.0017(7) 0.0026(7) 0.0046(7) C4 0.0127(8) 0.0188(8) 0.0168(8) 0.0039(7) 0.0032(6) 0.0034(7) C5 0.0103(7) 0.0186(8) 0.0184(8) 0.0027(7) -0.0018(6) 0.0014(6) C6 0.0153(8) 0.0211(9) 0.0257(9) 0.0037(7) 0.0012(7) 0.0067(7) C7 0.0153(8) 0.0278(9) 0.0185(9) 0.0019(7) 0.0032(7) 0.0042(7) C8 0.0200(9) 0.0311(10) 0.0194(9) 0.0114(8) 0.0061(7) 0.0048(8) C9 0.0168(8) 0.0226(9) 0.0215(9) 0.0085(7) 0.0034(7) 0.0049(7) C10 0.0264(10) 0.0438(12) 0.0283(11) 0.0068(9) 0.0103(8) 0.0141(9) C11 0.0305(10) 0.0307(10) 0.0324(11) 0.0194(9) 0.0105(8) 0.0124(8) C12 0.0159(8) 0.0207(8) 0.0234(9) 0.0085(7) 0.0014(7) 0.0061(7) C13 0.0140(8) 0.0173(8) 0.0189(8) 0.0029(7) 0.0047(6) 0.0041(7) C14 0.0176(8) 0.0219(9) 0.0188(9) 0.0035(7) 0.0027(7) 0.0072(7) C15 0.0147(8) 0.0271(9) 0.0263(10) 0.0029(8) 0.0020(7) 0.0076(7) C16 0.0188(9) 0.0245(9) 0.0248(10) 0.0048(8) 0.0079(7) 0.0052(7) C17 0.0256(9) 0.0258(9) 0.0233(9) 0.0108(8) 0.0077(8) 0.0090(8) C18 0.0200(9) 0.0216(8) 0.0211(9) 0.0045(7) 0.0028(7) 0.0086(7) C19 0.0232(10) 0.0387(11) 0.0383(12) 0.0124(9) 0.0144(9) 0.0067(9) C20 0.0238(9) 0.0373(11) 0.0315(11) 0.0163(9) 0.0042(8) 0.0146(8) C21 0.0233(9) 0.0368(11) 0.0259(10) 0.0126(8) 0.0040(8) 0.0136(8) C22 0.0160(8) 0.0246(9) 0.0256(9) 0.0101(8) 0.0034(7) 0.0048(7) C23 0.0298(10) 0.0313(10) 0.0337(11) 0.0119(9) 0.0090(8) 0.0158(9) C24 0.0228(9) 0.0355(10) 0.0273(10) 0.0093(8) 0.0019(8) 0.0147(8) C25 0.0275(10) 0.0369(11) 0.0346(11) 0.0200(9) 0.0075(8) 0.0140(9) C26 0.0315(10) 0.0277(10) 0.0215(9) 0.0056(8) 0.0039(8) 0.0153(8) C27 0.0329(11) 0.0383(12) 0.0349(12) -0.0055(9) -0.0016(9) 0.0156(9) C28 0.0416(12) 0.0375(12) 0.0406(13) 0.0027(10) 0.0048(10) 0.0234(10) C29 0.0600(16) 0.0334(12) 0.0634(17) 0.0160(12) 0.0220(13) 0.0093(11) C30 0.0272(10) 0.0361(10) 0.0189(9) 0.0094(8) 0.0085(8) 0.0108(8) C31 0.0545(14) 0.0721(16) 0.0314(12) 0.0294(12) 0.0175(11) 0.0334(13) C32 0.0432(13) 0.0686(16) 0.0352(12) 0.0286(12) 0.0049(10) 0.0282(12) C33 0.0349(11) 0.0419(12) 0.0310(11) 0.0174(9) 0.0089(9) 0.0225(9) C34 0.0242(10) 0.0317(10) 0.0361(11) 0.0036(9) 0.0120(9) 0.0074(8) C35 0.0187(10) 0.0475(13) 0.0519(14) 0.0212(11) 0.0086(9) 0.0113(9) C36 0.0269(11) 0.0385(12) 0.0394(12) 0.0062(10) 0.0001(9) -0.0017(9) C37 0.0275(10) 0.0393(11) 0.0289(11) 0.0012(9) 0.0009(9) 0.0087(9) C38 0.0449(13) 0.0320(11) 0.0386(13) 0.0097(10) 0.0018(10) 0.0128(10) C39 0.0441(12) 0.0389(12) 0.0341(12) 0.0163(10) 0.0150(10) 0.0162(10) C40 0.0256(10) 0.0317(10) 0.0335(11) 0.0122(9) 0.0044(8) 0.0080(8) C41 0.0219(9) 0.0373(11) 0.0287(10) 0.0082(9) 0.0033(8) 0.0065(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 Y1 C26 2.4263(17) . ? Y1 C22 2.4285(16) . ? Y1 O2 2.4522(11) . ? Y1 O1 2.4761(11) . ? Y1 C12 2.4995(16) . ? Y1 C1 2.6420(16) . ? Si1 C22 1.8306(17) . ? Si1 C24 1.8742(18) . ? Si1 C23 1.8832(18) . ? Si1 C25 1.8931(17) . ? Si2 C26 1.8284(18) . ? Si2 C29 1.879(2) . ? Si2 C27 1.888(2) . ? Si2 C28 1.8921(19) . ? O1 C33 1.448(2) . ? O1 C30 1.4626(19) . ? O2 C37 1.452(2) . ? O2 C34 1.456(2) . ? O3 C38 1.422(2) . ? O3 C41 1.438(2) . ? N1 C1 1.3665(19) . ? N1 C2 1.384(2) . ? N1 C4 1.444(2) . ? N2 C1 1.363(2) . ? N2 C3 1.391(2) . ? N2 C13 1.4440(19) . ? C2 C3 1.340(2) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C9 1.394(2) . ? C4 C5 1.418(2) . ? C5 C6 1.414(2) . ? C5 C12 1.447(2) . ? C6 C7 1.379(2) . ? C6 H6 0.9500 . ? C7 C8 1.392(2) . ? C7 C10 1.519(2) . ? C8 C9 1.396(2) . ? C8 H8 0.9500 . ? C9 C11 1.508(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.390(2) . ? C13 C14 1.396(2) . ? C14 C15 1.394(2) . ? C14 C21 1.504(2) . ? C15 C16 1.381(2) . ? C15 H15 0.9500 . ? C16 C17 1.391(2) . ? C16 C19 1.507(2) . ? C17 C18 1.390(2) . ? C17 H17 0.9500 . ? C18 C20 1.505(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.502(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.508(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.509(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.511(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.513(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.515(2) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.520(3) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.527(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.519(2) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? 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 C26 Y1 C22 99.54(6) . . ? C26 Y1 O2 108.14(5) . . ? C22 Y1 O2 81.07(5) . . ? C26 Y1 O1 83.54(5) . . ? C22 Y1 O1 153.25(5) . . ? O2 Y1 O1 72.81(4) . . ? C26 Y1 C12 91.24(6) . . ? C22 Y1 C12 96.69(5) . . ? O2 Y1 C12 160.61(5) . . ? O1 Y1 C12 109.87(5) . . ? C26 Y1 C1 146.10(5) . . ? C22 Y1 C1 110.37(5) . . ? O2 Y1 C1 92.34(4) . . ? O1 Y1 C1 76.97(4) . . ? C12 Y1 C1 70.25(5) . . ? C22 Si1 C24 112.35(8) . . ? C22 Si1 C23 112.28(8) . . ? C24 Si1 C23 106.66(8) . . ? C22 Si1 C25 114.01(8) . . ? C24 Si1 C25 104.29(8) . . ? C23 Si1 C25 106.61(8) . . ? C26 Si2 C29 110.50(10) . . ? C26 Si2 C27 113.41(9) . . ? C29 Si2 C27 107.93(11) . . ? C26 Si2 C28 113.75(9) . . ? C29 Si2 C28 106.32(10) . . ? C27 Si2 C28 104.44(9) . . ? C33 O1 C30 108.76(12) . . ? C33 O1 Y1 127.11(10) . . ? C30 O1 Y1 122.08(9) . . ? C37 O2 C34 108.65(13) . . ? C37 O2 Y1 117.34(10) . . ? C34 O2 Y1 128.83(10) . . ? C38 O3 C41 104.94(14) . . ? C1 N1 C2 112.12(13) . . ? C1 N1 C4 123.50(13) . . ? C2 N1 C4 124.33(13) . . ? C1 N2 C3 112.25(13) . . ? C1 N2 C13 124.79(13) . . ? C3 N2 C13 122.91(14) . . ? N2 C1 N1 102.57(13) . . ? N2 C1 Y1 139.89(11) . . ? N1 C1 Y1 115.01(10) . . ? C3 C2 N1 106.78(14) . . ? C3 C2 H2 126.6 . . ? N1 C2 H2 126.6 . . ? C2 C3 N2 106.26(15) . . ? C2 C3 H3 126.9 . . ? N2 C3 H3 126.9 . . ? C9 C4 C5 123.42(15) . . ? C9 C4 N1 118.95(14) . . ? C5 C4 N1 117.62(13) . . ? C6 C5 C4 114.99(14) . . ? C6 C5 C12 122.24(15) . . ? C4 C5 C12 122.59(15) . . ? C7 C6 C5 123.22(16) . . ? C7 C6 H6 118.4 . . ? C5 C6 H6 118.4 . . ? C6 C7 C8 119.12(16) . . ? C6 C7 C10 120.72(16) . . ? C8 C7 C10 120.15(16) . . ? C7 C8 C9 121.18(15) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C4 C9 C8 118.02(15) . . ? C4 C9 C11 122.03(15) . . ? C8 C9 C11 119.95(15) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 Y1 99.97(10) . . ? C5 C12 H12A 111.8 . . ? Y1 C12 H12A 111.8 . . ? C5 C12 H12B 111.8 . . ? Y1 C12 H12B 111.8 . . ? H12A C12 H12B 109.5 . . ? C18 C13 C14 122.74(15) . . ? C18 C13 N2 118.27(14) . . ? C14 C13 N2 118.96(14) . . ? C15 C14 C13 117.13(15) . . ? C15 C14 C21 121.09(15) . . ? C13 C14 C21 121.78(15) . . ? C16 C15 C14 122.14(16) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C17 118.55(15) . . ? C15 C16 C19 121.25(16) . . ? C17 C16 C19 120.19(16) . . ? C18 C17 C16 121.81(16) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C13 C18 C17 117.53(15) . . ? C13 C18 C20 121.03(15) . . ? C17 C18 C20 121.42(15) . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C21 H21A 109.5 . . ? C14 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C14 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 Y1 127.10(8) . . ? Si1 C22 H22A 105.5 . . ? Y1 C22 H22A 105.5 . . ? Si1 C22 H22B 105.5 . . ? Y1 C22 H22B 105.5 . . ? H22A C22 H22B 106.1 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? 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 . . ? Si2 C26 Y1 137.29(9) . . ? Si2 C26 H26A 102.8 . . ? Y1 C26 H26A 102.8 . . ? Si2 C26 H26B 102.8 . . ? Y1 C26 H26B 102.8 . . ? H26A C26 H26B 105.0 . . ? 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 . . ? O1 C30 C31 105.89(14) . . ? O1 C30 H30A 110.6 . . ? C31 C30 H30A 110.6 . . ? O1 C30 H30B 110.6 . . ? C31 C30 H30B 110.6 . . ? H30A C30 H30B 108.7 . . ? C30 C31 C32 104.04(16) . . ? C30 C31 H31A 110.9 . . ? C32 C31 H31A 110.9 . . ? C30 C31 H31B 110.9 . . ? C32 C31 H31B 110.9 . . ? H31A C31 H31B 109.0 . . ? C31 C32 C33 101.75(16) . . ? C31 C32 H32A 111.4 . . ? C33 C32 H32A 111.4 . . ? C31 C32 H32B 111.4 . . ? C33 C32 H32B 111.4 . . ? H32A C32 H32B 109.3 . . ? O1 C33 C32 104.79(15) . . ? O1 C33 H33A 110.8 . . ? C32 C33 H33A 110.8 . . ? O1 C33 H33B 110.8 . . ? C32 C33 H33B 110.8 . . ? H33A C33 H33B 108.9 . . ? O2 C34 C35 105.06(15) . . ? O2 C34 H34A 110.7 . . ? C35 C34 H34A 110.7 . . ? O2 C34 H34B 110.7 . . ? C35 C34 H34B 110.7 . . ? H34A C34 H34B 108.8 . . ? C34 C35 C36 101.48(15) . . ? C34 C35 H35A 111.5 . . ? C36 C35 H35A 111.5 . . ? C34 C35 H35B 111.5 . . ? C36 C35 H35B 111.5 . . ? H35A C35 H35B 109.3 . . ? C35 C36 C37 102.42(16) . . ? C35 C36 H36A 111.3 . . ? C37 C36 H36A 111.3 . . ? C35 C36 H36B 111.3 . . ? C37 C36 H36B 111.3 . . ? H36A C36 H36B 109.2 . . ? O2 C37 C36 105.95(15) . . ? O2 C37 H37A 110.5 . . ? C36 C37 H37A 110.5 . . ? O2 C37 H37B 110.5 . . ? C36 C37 H37B 110.5 . . ? H37A C37 H37B 108.7 . . ? O3 C38 C39 106.37(16) . . ? O3 C38 H38A 110.5 . . ? C39 C38 H38A 110.5 . . ? O3 C38 H38B 110.5 . . ? C39 C38 H38B 110.5 . . ? H38A C38 H38B 108.6 . . ? C38 C39 C40 104.28(16) . . ? C38 C39 H39A 110.9 . . ? C40 C39 H39A 110.9 . . ? C38 C39 H39B 110.9 . . ? C40 C39 H39B 110.9 . . ? H39A C39 H39B 108.9 . . ? C41 C40 C39 103.64(15) . . ? C41 C40 H40A 111.0 . . ? C39 C40 H40A 111.0 . . ? C41 C40 H40B 111.0 . . ? C39 C40 H40B 111.0 . . ? H40A C40 H40B 109.0 . . ? O3 C41 C40 104.53(15) . . ? O3 C41 H41A 110.8 . . ? C40 C41 H41A 110.8 . . ? O3 C41 H41B 110.8 . . ? C40 C41 H41B 110.8 . . ? H41A C41 H41B 108.9 . . ? 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 C26 Y1 O1 C33 164.61(14) . . . . ? C22 Y1 O1 C33 66.24(18) . . . . ? O2 Y1 O1 C33 53.33(13) . . . . ? C12 Y1 O1 C33 -106.40(13) . . . . ? C1 Y1 O1 C33 -43.30(13) . . . . ? C26 Y1 O1 C30 -33.51(12) . . . . ? C22 Y1 O1 C30 -131.89(14) . . . . ? O2 Y1 O1 C30 -144.80(12) . . . . ? C12 Y1 O1 C30 55.47(12) . . . . ? C1 Y1 O1 C30 118.58(12) . . . . ? C26 Y1 O2 C37 -8.19(13) . . . . ? C22 Y1 O2 C37 -105.37(12) . . . . ? O1 Y1 O2 C37 68.78(11) . . . . ? C12 Y1 O2 C37 169.87(14) . . . . ? C1 Y1 O2 C37 144.37(12) . . . . ? C26 Y1 O2 C34 143.25(13) . . . . ? C22 Y1 O2 C34 46.07(13) . . . . ? O1 Y1 O2 C34 -139.77(14) . . . . ? C12 Y1 O2 C34 -38.7(2) . . . . ? C1 Y1 O2 C34 -64.19(13) . . . . ? C3 N2 C1 N1 -0.95(17) . . . . ? C13 N2 C1 N1 -178.41(13) . . . . ? C3 N2 C1 Y1 158.61(13) . . . . ? C13 N2 C1 Y1 -18.9(3) . . . . ? C2 N1 C1 N2 1.19(17) . . . . ? C4 N1 C1 N2 178.79(13) . . . . ? C2 N1 C1 Y1 -164.44(10) . . . . ? C4 N1 C1 Y1 13.17(18) . . . . ? C26 Y1 C1 N2 -178.55(15) . . . . ? C22 Y1 C1 N2 -28.16(18) . . . . ? O2 Y1 C1 N2 53.18(17) . . . . ? O1 Y1 C1 N2 124.93(17) . . . . ? C12 Y1 C1 N2 -118.08(17) . . . . ? C26 Y1 C1 N1 -20.65(16) . . . . ? C22 Y1 C1 N1 129.74(11) . . . . ? O2 Y1 C1 N1 -148.92(11) . . . . ? O1 Y1 C1 N1 -77.16(11) . . . . ? C12 Y1 C1 N1 39.82(11) . . . . ? C1 N1 C2 C3 -1.01(19) . . . . ? C4 N1 C2 C3 -178.60(14) . . . . ? N1 C2 C3 N2 0.37(18) . . . . ? C1 N2 C3 C2 0.38(19) . . . . ? C13 N2 C3 C2 177.90(14) . . . . ? C1 N1 C4 C9 125.05(17) . . . . ? C2 N1 C4 C9 -57.6(2) . . . . ? C1 N1 C4 C5 -55.7(2) . . . . ? C2 N1 C4 C5 121.66(17) . . . . ? C9 C4 C5 C6 -0.4(2) . . . . ? N1 C4 C5 C6 -179.62(13) . . . . ? C9 C4 C5 C12 -175.71(16) . . . . ? N1 C4 C5 C12 5.0(2) . . . . ? C4 C5 C6 C7 2.1(2) . . . . ? C12 C5 C6 C7 177.45(15) . . . . ? C5 C6 C7 C8 -2.2(3) . . . . ? C5 C6 C7 C10 176.63(15) . . . . ? C6 C7 C8 C9 0.5(3) . . . . ? C10 C7 C8 C9 -178.31(16) . . . . ? C5 C4 C9 C8 -1.2(2) . . . . ? N1 C4 C9 C8 178.09(14) . . . . ? C5 C4 C9 C11 179.22(15) . . . . ? N1 C4 C9 C11 -1.5(2) . . . . ? C7 C8 C9 C4 1.1(3) . . . . ? C7 C8 C9 C11 -179.29(16) . . . . ? C6 C5 C12 Y1 -106.42(14) . . . . ? C4 C5 C12 Y1 68.60(16) . . . . ? C26 Y1 C12 C5 79.46(11) . . . . ? C22 Y1 C12 C5 179.21(11) . . . . ? O2 Y1 C12 C5 -98.70(16) . . . . ? O1 Y1 C12 C5 -4.12(12) . . . . ? C1 Y1 C12 C5 -71.51(10) . . . . ? C1 N2 C13 C18 83.3(2) . . . . ? C3 N2 C13 C18 -93.87(19) . . . . ? C1 N2 C13 C14 -98.45(19) . . . . ? C3 N2 C13 C14 84.3(2) . . . . ? C18 C13 C14 C15 -2.4(2) . . . . ? N2 C13 C14 C15 179.44(14) . . . . ? C18 C13 C14 C21 178.20(16) . . . . ? N2 C13 C14 C21 0.1(2) . . . . ? C13 C14 C15 C16 -0.3(3) . . . . ? C21 C14 C15 C16 179.05(16) . . . . ? C14 C15 C16 C17 2.1(3) . . . . ? C14 C15 C16 C19 -178.58(16) . . . . ? C15 C16 C17 C18 -1.3(3) . . . . ? C19 C16 C17 C18 179.40(16) . . . . ? C14 C13 C18 C17 3.2(3) . . . . ? N2 C13 C18 C17 -178.66(14) . . . . ? C14 C13 C18 C20 -175.13(16) . . . . ? N2 C13 C18 C20 3.0(2) . . . . ? C16 C17 C18 C13 -1.3(3) . . . . ? C16 C17 C18 C20 177.06(17) . . . . ? C24 Si1 C22 Y1 74.28(12) . . . . ? C23 Si1 C22 Y1 -45.95(13) . . . . ? C25 Si1 C22 Y1 -167.34(10) . . . . ? C26 Y1 C22 Si1 65.77(11) . . . . ? O2 Y1 C22 Si1 172.82(11) . . . . ? O1 Y1 C22 Si1 160.34(7) . . . . ? C12 Y1 C22 Si1 -26.63(11) . . . . ? C1 Y1 C22 Si1 -98.00(11) . . . . ? C29 Si2 C26 Y1 -56.83(16) . . . . ? C27 Si2 C26 Y1 64.51(15) . . . . ? C28 Si2 C26 Y1 -176.32(12) . . . . ? C22 Y1 C26 Si2 73.00(14) . . . . ? O2 Y1 C26 Si2 -10.65(14) . . . . ? O1 Y1 C26 Si2 -80.15(13) . . . . ? C12 Y1 C26 Si2 169.99(13) . . . . ? C1 Y1 C26 Si2 -135.02(11) . . . . ? C33 O1 C30 C31 0.5(2) . . . . ? Y1 O1 C30 C31 -164.29(12) . . . . ? O1 C30 C31 C32 -23.6(2) . . . . ? C30 C31 C32 C33 36.6(2) . . . . ? C30 O1 C33 C32 22.78(19) . . . . ? Y1 O1 C33 C32 -173.38(11) . . . . ? C31 C32 C33 O1 -36.5(2) . . . . ? C37 O2 C34 C35 -18.76(19) . . . . ? Y1 O2 C34 C35 -172.14(11) . . . . ? O2 C34 C35 C36 36.32(19) . . . . ? C34 C35 C36 C37 -39.6(2) . . . . ? C34 O2 C37 C36 -6.7(2) . . . . ? Y1 O2 C37 C36 150.20(12) . . . . ? C35 C36 C37 O2 29.2(2) . . . . ? C41 O3 C38 C39 -36.55(19) . . . . ? O3 C38 C39 C40 17.2(2) . . . . ? C38 C39 C40 C41 7.3(2) . . . . ? C38 O3 C41 C40 41.21(17) . . . . ? C39 C40 C41 O3 -29.17(18) . . . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.856 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.065 #===END