Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email 'Dongmei Cui' _publ_contact_author_name dmcui@ciac.jl.cn loop_ _publ_author_name 'Dongmei Cui' 'Baotong Huang' 'Shihui Li' 'Wei Miao' 'Dun Wang' data_gaowei _database_code_depnum_ccdc_archive 'CCDC 641761' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H56 Lu N O3 S Si' _chemical_formula_weight 749.91 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.1191(14) _cell_length_b 13.0059(11) _cell_length_c 19.0227(16) _cell_angle_alpha 90.00 _cell_angle_beta 97.5610(10) _cell_angle_gamma 90.00 _cell_volume 4198.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blok _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 2.455 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6663 _exptl_absorpt_correction_T_max 0.7571 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22482 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 26.03 _reflns_number_total 8089 _reflns_number_gt 6897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^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 8089 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu Lu 0.713416(7) 0.300290(10) 0.546714(7) 0.02512(6) Uani 1 1 d . . . S S 0.54755(6) 0.30136(7) 0.72769(5) 0.0405(2) Uani 1 1 d . . . Si Si 0.78163(7) 0.06752(8) 0.64905(6) 0.0426(3) Uani 1 1 d . . . O3 O 0.66014(15) 0.18161(18) 0.45366(14) 0.0380(6) Uani 1 1 d . . . C4 C 0.61518(19) 0.3258(3) 0.66782(18) 0.0300(7) Uani 1 1 d . . . O1 O 0.81711(14) 0.36721(18) 0.48752(14) 0.0391(6) Uani 1 1 d . . . O2 O 0.64573(14) 0.40312(19) 0.45373(13) 0.0364(5) Uani 1 1 d . . . N N 0.72962(16) 0.4147(2) 0.63223(15) 0.0308(6) Uani 1 1 d . . . C5 C 0.67993(19) 0.4034(3) 0.68868(18) 0.0333(7) Uani 1 1 d . . . H5A H 0.6563 0.4707 0.6981 0.040 Uiso 1 1 calc R . . H5B H 0.7125 0.3805 0.7328 0.040 Uiso 1 1 calc R . . C2 C 0.5333(2) 0.2064(3) 0.6099(2) 0.0390(9) Uani 1 1 d . . . H2 H 0.5136 0.1613 0.5724 0.047 Uiso 1 1 calc R . . C6 C 0.78263(18) 0.4996(3) 0.64752(17) 0.0307(7) Uani 1 1 d . . . C1 C 0.6015(2) 0.2708(3) 0.60664(18) 0.0310(7) Uani 1 1 d . . . C7 C 0.8609(2) 0.4822(3) 0.68006(19) 0.0357(8) Uani 1 1 d . . . C18 C 0.8025(2) 0.1628(3) 0.5836(2) 0.0377(8) Uani 1 1 d . . . H18A H 0.8108 0.1245 0.5402 0.045 Uiso 1 1 calc R . . H18B H 0.8536 0.1948 0.6019 0.045 Uiso 1 1 calc R . . C11 C 0.7585(2) 0.6009(3) 0.6304(2) 0.0402(8) Uani 1 1 d . . . C26 C 0.5701(2) 0.4495(3) 0.4596(2) 0.0420(9) Uani 1 1 d . . . H26A H 0.5741 0.4966 0.5007 0.050 Uiso 1 1 calc R . . H26B H 0.5305 0.3959 0.4657 0.050 Uiso 1 1 calc R . . C3 C 0.4994(2) 0.2148(3) 0.6699(2) 0.0451(10) Uani 1 1 d . . . H3 H 0.4542 0.1772 0.6789 0.054 Uiso 1 1 calc R . . C12 C 0.8887(2) 0.3768(3) 0.7055(2) 0.0402(9) Uani 1 1 d . . . H12 H 0.8455 0.3270 0.6897 0.048 Uiso 1 1 calc R . . C30 C 0.5761(2) 0.1806(3) 0.4294(2) 0.0417(9) Uani 1 1 d . . . H30A H 0.5639 0.2201 0.3848 0.050 Uiso 1 1 calc R . . H30B H 0.5462 0.2104 0.4656 0.050 Uiso 1 1 calc R . . C8 C 0.9125(2) 0.5661(3) 0.6902(2) 0.0464(10) Uani 1 1 d . . . H8 H 0.9653 0.5545 0.7110 0.056 Uiso 1 1 calc R . . C10 C 0.8125(3) 0.6811(3) 0.6422(3) 0.0505(11) Uani 1 1 d . . . H10 H 0.7959 0.7492 0.6300 0.061 Uiso 1 1 calc R . . C25 C 0.8648(3) 0.3020(3) 0.4470(3) 0.0544(12) Uani 1 1 d . . . H25A H 0.8330 0.2765 0.4033 0.065 Uiso 1 1 calc R . . H25B H 0.8859 0.2422 0.4757 0.065 Uiso 1 1 calc R . . C29 C 0.6628(2) 0.4118(3) 0.3811(2) 0.0456(9) Uani 1 1 d . . . H29A H 0.6716 0.3429 0.3613 0.055 Uiso 1 1 calc R . . H29B H 0.7105 0.4540 0.3790 0.055 Uiso 1 1 calc R . . C22 C 0.8460(2) 0.4726(3) 0.4860(2) 0.0483(10) Uani 1 1 d . . . H22A H 0.8763 0.4915 0.5322 0.058 Uiso 1 1 calc R . . H22B H 0.8017 0.5215 0.4752 0.058 Uiso 1 1 calc R . . C9 C 0.8895(3) 0.6640(3) 0.6713(3) 0.0516(11) Uani 1 1 d . . . H9 H 0.9260 0.7193 0.6780 0.062 Uiso 1 1 calc R . . C15 C 0.6733(2) 0.6269(3) 0.6002(3) 0.0513(11) Uani 1 1 d . . . H15 H 0.6441 0.5605 0.5918 0.062 Uiso 1 1 calc R . . C14 C 0.9614(2) 0.3423(4) 0.6738(3) 0.0551(11) Uani 1 1 d . . . H14A H 0.9503 0.3438 0.6219 0.083 Uiso 1 1 calc R . . H14B H 0.9754 0.2721 0.6895 0.083 Uiso 1 1 calc R . . H14C H 1.0054 0.3887 0.6894 0.083 Uiso 1 1 calc R . . C13 C 0.9036(3) 0.3734(4) 0.7872(2) 0.0573(11) Uani 1 1 d . . . H13A H 0.9464 0.4207 0.8043 0.086 Uiso 1 1 calc R . . H13B H 0.9181 0.3034 0.8028 0.086 Uiso 1 1 calc R . . H13C H 0.8555 0.3940 0.8064 0.086 Uiso 1 1 calc R . . C31 C 0.5566(3) 0.0691(4) 0.4177(3) 0.0612(12) Uani 1 1 d . . . H31A H 0.5094 0.0603 0.3820 0.073 Uiso 1 1 calc R . . H31B H 0.5470 0.0354 0.4624 0.073 Uiso 1 1 calc R . . C32 C 0.6288(3) 0.0256(3) 0.3911(3) 0.0654(13) Uani 1 1 d . . . H32A H 0.6399 -0.0447 0.4097 0.078 Uiso 1 1 calc R . . H32B H 0.6217 0.0231 0.3386 0.078 Uiso 1 1 calc R . . C23 C 0.8979(3) 0.4736(4) 0.4284(3) 0.0687(14) Uani 1 1 d . . . H23A H 0.8671 0.4894 0.3819 0.082 Uiso 1 1 calc R . . H23B H 0.9406 0.5250 0.4384 0.082 Uiso 1 1 calc R . . C33 C 0.6943(3) 0.0975(4) 0.4181(3) 0.0722(15) Uani 1 1 d . . . H33A H 0.7342 0.0613 0.4516 0.087 Uiso 1 1 calc R . . H33B H 0.7203 0.1239 0.3782 0.087 Uiso 1 1 calc R . . C17 C 0.6685(3) 0.6822(4) 0.5295(3) 0.0737(16) Uani 1 1 d . . . H17A H 0.6998 0.7454 0.5353 0.111 Uiso 1 1 calc R . . H17B H 0.6134 0.6995 0.5129 0.111 Uiso 1 1 calc R . . H17C H 0.6890 0.6375 0.4948 0.111 Uiso 1 1 calc R . . C27 C 0.5470(3) 0.5074(5) 0.3922(3) 0.0758(16) Uani 1 1 d . . . H27A H 0.4899 0.5001 0.3763 0.091 Uiso 1 1 calc R . . H27B H 0.5596 0.5814 0.3988 0.091 Uiso 1 1 calc R . . C19 C 0.7652(4) 0.1283(4) 0.7343(3) 0.0735(15) Uani 1 1 d . . . H19A H 0.8131 0.1646 0.7546 0.110 Uiso 1 1 calc R . . H19B H 0.7523 0.0751 0.7675 0.110 Uiso 1 1 calc R . . H19C H 0.7215 0.1773 0.7259 0.110 Uiso 1 1 calc R . . C16 C 0.6332(3) 0.6883(4) 0.6537(4) 0.0741(16) Uani 1 1 d . . . H16A H 0.6618 0.7529 0.6645 0.111 Uiso 1 1 calc R . . H16B H 0.6334 0.6482 0.6973 0.111 Uiso 1 1 calc R . . H16C H 0.5787 0.7035 0.6336 0.111 Uiso 1 1 calc R . . C24 C 0.9303(3) 0.3686(4) 0.4292(3) 0.0735(15) Uani 1 1 d . . . H24A H 0.9771 0.3621 0.4654 0.088 Uiso 1 1 calc R . . H24B H 0.9453 0.3503 0.3823 0.088 Uiso 1 1 calc R . . C21 C 0.6910(3) -0.0080(4) 0.6170(3) 0.0739(15) Uani 1 1 d . . . H21A H 0.6455 0.0384 0.6095 0.111 Uiso 1 1 calc R . . H21B H 0.6822 -0.0599 0.6525 0.111 Uiso 1 1 calc R . . H21C H 0.6977 -0.0421 0.5723 0.111 Uiso 1 1 calc R . . C20 C 0.8641(3) -0.0274(4) 0.6724(3) 0.0797(17) Uani 1 1 d . . . H20A H 0.8704 -0.0692 0.6306 0.120 Uiso 1 1 calc R . . H20B H 0.8515 -0.0721 0.7108 0.120 Uiso 1 1 calc R . . H20C H 0.9131 0.0098 0.6877 0.120 Uiso 1 1 calc R . . C28 C 0.5931(4) 0.4615(5) 0.3407(3) 0.095(2) Uani 1 1 d . . . H28A H 0.6099 0.5151 0.3089 0.113 Uiso 1 1 calc R . . H28B H 0.5610 0.4100 0.3114 0.113 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 Lu 0.02495(9) 0.02456(9) 0.02559(9) 0.00000(5) 0.00243(6) -0.00065(5) S 0.0377(5) 0.0551(6) 0.0298(5) 0.0018(4) 0.0082(4) -0.0074(4) Si 0.0447(6) 0.0320(5) 0.0489(7) 0.0107(5) -0.0020(5) 0.0026(4) O3 0.0374(14) 0.0384(14) 0.0365(14) -0.0088(11) -0.0018(11) 0.0003(10) C4 0.0258(17) 0.0337(18) 0.0298(18) 0.0041(14) 0.0015(14) -0.0007(13) O1 0.0372(14) 0.0367(14) 0.0456(15) -0.0002(11) 0.0143(12) -0.0017(11) O2 0.0346(13) 0.0411(14) 0.0336(13) 0.0049(11) 0.0049(10) 0.0084(11) N 0.0302(14) 0.0312(15) 0.0308(15) -0.0026(12) 0.0032(12) -0.0051(12) C5 0.0327(18) 0.0370(18) 0.0303(18) -0.0040(15) 0.0037(14) -0.0044(15) C2 0.038(2) 0.044(2) 0.034(2) -0.0016(16) 0.0038(16) -0.0146(16) C6 0.0274(17) 0.0357(18) 0.0293(18) -0.0076(14) 0.0048(13) -0.0073(14) C1 0.0294(18) 0.0331(17) 0.0302(18) 0.0027(14) 0.0033(14) -0.0039(14) C7 0.0311(18) 0.041(2) 0.035(2) -0.0028(16) 0.0069(15) -0.0047(15) C18 0.037(2) 0.0357(19) 0.039(2) -0.0022(16) -0.0001(16) 0.0028(16) C11 0.0375(19) 0.0338(19) 0.048(2) -0.0088(17) 0.0025(16) -0.0010(16) C26 0.037(2) 0.044(2) 0.044(2) 0.0012(17) -0.0007(17) 0.0094(16) C3 0.036(2) 0.056(2) 0.043(2) 0.0033(18) 0.0070(17) -0.0149(17) C12 0.0299(18) 0.045(2) 0.043(2) 0.0051(17) -0.0051(15) -0.0086(15) C30 0.039(2) 0.051(2) 0.034(2) -0.0032(16) -0.0023(16) -0.0056(17) C8 0.032(2) 0.055(2) 0.051(2) -0.0041(19) -0.0005(17) -0.0126(17) C10 0.048(3) 0.033(2) 0.070(3) -0.0062(19) 0.008(2) -0.0073(17) C25 0.056(3) 0.049(3) 0.065(3) 0.000(2) 0.033(2) 0.0000(19) C29 0.054(2) 0.053(2) 0.031(2) 0.0093(17) 0.0049(17) 0.0086(19) C22 0.053(2) 0.038(2) 0.056(3) 0.0056(18) 0.016(2) -0.0096(17) C9 0.046(2) 0.044(2) 0.065(3) -0.010(2) 0.007(2) -0.0204(19) C15 0.041(2) 0.032(2) 0.077(3) -0.0044(19) -0.005(2) 0.0020(16) C14 0.040(2) 0.052(2) 0.070(3) -0.001(2) -0.002(2) 0.0041(19) C13 0.053(3) 0.073(3) 0.042(2) 0.010(2) -0.0081(19) -0.011(2) C31 0.062(3) 0.056(3) 0.065(3) -0.007(2) 0.005(2) -0.019(2) C32 0.088(4) 0.041(2) 0.063(3) -0.015(2) -0.004(3) -0.007(2) C23 0.080(3) 0.065(3) 0.066(3) -0.002(2) 0.028(3) -0.029(3) C33 0.058(3) 0.071(3) 0.085(4) -0.048(3) -0.001(3) 0.009(2) C17 0.063(3) 0.051(3) 0.100(5) 0.009(3) -0.016(3) 0.000(2) C27 0.060(3) 0.100(4) 0.068(3) 0.034(3) 0.010(3) 0.030(3) C19 0.107(4) 0.069(3) 0.046(3) 0.018(2) 0.014(3) 0.001(3) C16 0.050(3) 0.057(3) 0.115(5) -0.021(3) 0.011(3) 0.016(2) C24 0.062(3) 0.084(4) 0.083(4) -0.018(3) 0.039(3) -0.022(3) C21 0.073(3) 0.040(2) 0.104(4) 0.017(3) -0.004(3) -0.011(2) C20 0.070(3) 0.057(3) 0.108(5) 0.026(3) -0.007(3) 0.016(3) C28 0.113(5) 0.131(5) 0.039(3) 0.019(3) 0.009(3) 0.074(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 Lu N 2.195(3) . ? Lu C1 2.385(3) . ? Lu O1 2.388(2) . ? Lu O2 2.392(2) . ? Lu C18 2.394(3) . ? Lu O3 2.434(2) . ? S C3 1.708(4) . ? S C4 1.757(4) . ? Si C18 1.825(4) . ? Si C19 1.859(5) . ? Si C21 1.869(5) . ? Si C20 1.883(5) . ? O3 C33 1.450(5) . ? O3 C30 1.452(5) . ? C4 C1 1.360(5) . ? C4 C5 1.512(5) . ? O1 C22 1.459(4) . ? O1 C25 1.465(5) . ? O2 C26 1.446(4) . ? O2 C29 1.454(4) . ? N C6 1.435(4) . ? N C5 1.462(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C2 C3 1.352(6) . ? C2 C1 1.446(5) . ? C2 H2 0.9500 . ? C6 C11 1.407(5) . ? C6 C7 1.418(5) . ? C7 C8 1.401(5) . ? C7 C12 1.510(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C11 C10 1.392(5) . ? C11 C15 1.534(5) . ? C26 C27 1.494(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C3 H3 0.9500 . ? C12 C14 1.521(6) . ? C12 C13 1.541(6) . ? C12 H12 1.0000 . ? C30 C31 1.499(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C8 C9 1.367(6) . ? C8 H8 0.9500 . ? C10 C9 1.379(6) . ? C10 H10 0.9500 . ? C25 C24 1.491(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C29 C28 1.480(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C22 C23 1.499(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C9 H9 0.9500 . ? C15 C17 1.518(7) . ? C15 C16 1.525(7) . ? C15 H15 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C31 C32 1.506(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.499(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C23 C24 1.472(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C27 C28 1.464(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C28 H28A 0.9900 . ? C28 H28B 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 N Lu C1 77.63(11) . . ? N Lu O1 94.20(9) . . ? C1 Lu O1 167.79(10) . . ? N Lu O2 99.84(9) . . ? C1 Lu O2 95.86(10) . . ? O1 Lu O2 76.43(8) . . ? N Lu C18 105.99(12) . . ? C1 Lu C18 105.09(12) . . ? O1 Lu C18 85.76(11) . . ? O2 Lu C18 149.55(11) . . ? N Lu O3 165.39(9) . . ? C1 Lu O3 89.89(10) . . ? O1 Lu O3 96.83(9) . . ? O2 Lu O3 73.62(9) . . ? C18 Lu O3 84.41(11) . . ? C3 S C4 90.35(18) . . ? C18 Si C19 111.9(2) . . ? C18 Si C21 111.3(2) . . ? C19 Si C21 107.0(3) . . ? C18 Si C20 113.5(2) . . ? C19 Si C20 105.6(3) . . ? C21 Si C20 107.3(2) . . ? C33 O3 C30 106.8(3) . . ? C33 O3 Lu 133.0(2) . . ? C30 O3 Lu 119.9(2) . . ? C1 C4 C5 127.8(3) . . ? C1 C4 S 113.9(2) . . ? C5 C4 S 118.3(2) . . ? C22 O1 C25 108.7(3) . . ? C22 O1 Lu 128.8(2) . . ? C25 O1 Lu 122.5(2) . . ? C26 O2 C29 109.6(3) . . ? C26 O2 Lu 121.9(2) . . ? C29 O2 Lu 127.4(2) . . ? C6 N C5 110.0(3) . . ? C6 N Lu 133.4(2) . . ? C5 N Lu 116.6(2) . . ? N C5 C4 110.6(3) . . ? N C5 H5A 109.5 . . ? C4 C5 H5A 109.5 . . ? N C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C3 C2 C1 115.4(3) . . ? C3 C2 H2 122.3 . . ? C1 C2 H2 122.3 . . ? C11 C6 C7 118.8(3) . . ? C11 C6 N 121.0(3) . . ? C7 C6 N 120.1(3) . . ? C4 C1 C2 108.5(3) . . ? C4 C1 Lu 105.4(2) . . ? C2 C1 Lu 144.9(3) . . ? C8 C7 C6 118.6(3) . . ? C8 C7 C12 119.7(3) . . ? C6 C7 C12 121.7(3) . . ? Si C18 Lu 122.21(18) . . ? Si C18 H18A 106.8 . . ? Lu C18 H18A 106.8 . . ? Si C18 H18B 106.8 . . ? Lu C18 H18B 106.8 . . ? H18A C18 H18B 106.6 . . ? C10 C11 C6 119.7(3) . . ? C10 C11 C15 118.3(3) . . ? C6 C11 C15 121.9(3) . . ? O2 C26 C27 106.4(3) . . ? O2 C26 H26A 110.4 . . ? C27 C26 H26A 110.4 . . ? O2 C26 H26B 110.4 . . ? C27 C26 H26B 110.4 . . ? H26A C26 H26B 108.6 . . ? C2 C3 S 111.9(3) . . ? C2 C3 H3 124.1 . . ? S C3 H3 124.1 . . ? C7 C12 C14 112.4(3) . . ? C7 C12 C13 110.7(3) . . ? C14 C12 C13 110.9(3) . . ? C7 C12 H12 107.5 . . ? C14 C12 H12 107.5 . . ? C13 C12 H12 107.5 . . ? O3 C30 C31 104.4(3) . . ? O3 C30 H30A 110.9 . . ? C31 C30 H30A 110.9 . . ? O3 C30 H30B 110.9 . . ? C31 C30 H30B 110.9 . . ? H30A C30 H30B 108.9 . . ? C9 C8 C7 122.3(4) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? C9 C10 C11 121.6(4) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? O1 C25 C24 105.7(3) . . ? O1 C25 H25A 110.6 . . ? C24 C25 H25A 110.6 . . ? O1 C25 H25B 110.6 . . ? C24 C25 H25B 110.6 . . ? H25A C25 H25B 108.7 . . ? O2 C29 C28 106.1(3) . . ? O2 C29 H29A 110.5 . . ? C28 C29 H29A 110.5 . . ? O2 C29 H29B 110.5 . . ? C28 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? O1 C22 C23 104.9(3) . . ? O1 C22 H22A 110.8 . . ? C23 C22 H22A 110.8 . . ? O1 C22 H22B 110.8 . . ? C23 C22 H22B 110.8 . . ? H22A C22 H22B 108.8 . . ? C8 C9 C10 118.8(4) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C17 C15 C16 111.4(4) . . ? C17 C15 C11 112.0(4) . . ? C16 C15 C11 110.7(4) . . ? C17 C15 H15 107.5 . . ? C16 C15 H15 107.5 . . ? C11 C15 H15 107.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C30 C31 C32 103.7(4) . . ? C30 C31 H31A 111.0 . . ? C32 C31 H31A 111.0 . . ? C30 C31 H31B 111.0 . . ? C32 C31 H31B 111.0 . . ? H31A C31 H31B 109.0 . . ? C33 C32 C31 105.1(4) . . ? C33 C32 H32A 110.7 . . ? C31 C32 H32A 110.7 . . ? C33 C32 H32B 110.7 . . ? C31 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? C24 C23 C22 104.1(4) . . ? C24 C23 H23A 110.9 . . ? C22 C23 H23A 110.9 . . ? C24 C23 H23B 110.9 . . ? C22 C23 H23B 110.9 . . ? H23A C23 H23B 109.0 . . ? O3 C33 C32 107.5(4) . . ? O3 C33 H33A 110.2 . . ? C32 C33 H33A 110.2 . . ? O3 C33 H33B 110.2 . . ? C32 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? 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 . . ? C28 C27 C26 105.3(4) . . ? C28 C27 H27A 110.7 . . ? C26 C27 H27A 110.7 . . ? C28 C27 H27B 110.7 . . ? C26 C27 H27B 110.7 . . ? H27A C27 H27B 108.8 . . ? Si C19 H19A 109.5 . . ? Si C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C23 C24 C25 104.4(4) . . ? C23 C24 H24A 110.9 . . ? C25 C24 H24A 110.9 . . ? C23 C24 H24B 110.9 . . ? C25 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? Si C21 H21A 109.5 . . ? Si C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si C20 H20A 109.5 . . ? Si C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C27 C28 C29 107.4(4) . . ? C27 C28 H28A 110.2 . . ? C29 C28 H28A 110.2 . . ? C27 C28 H28B 110.2 . . ? C29 C28 H28B 110.2 . . ? H28A C28 H28B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.095 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.101 # Attachment 'complex 3.cif' data_r117m _database_code_depnum_ccdc_archive 'CCDC 641762' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H65 N2 O S2 Sc' _chemical_formula_weight 747.06 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.1510(11) _cell_length_b 14.9860(11) _cell_length_c 19.3443(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.2400(10) _cell_angle_gamma 90.00 _cell_volume 4385.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blok _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.296 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9487 _exptl_absorpt_correction_T_max 0.9626 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24260 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0841 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 26.04 _reflns_number_total 8659 _reflns_number_gt 5164 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^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 8659 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _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 Sc1 Sc 0.72989(3) 0.28678(3) 0.77844(3) 0.03359(15) Uani 1 1 d . . . S1 S 0.79268(5) 0.44431(5) 0.70208(5) 0.0532(2) Uani 1 1 d . . . S2 S 0.56020(5) 0.19755(5) 0.95382(4) 0.0483(2) Uani 1 1 d . . . O1 O 0.68084(11) 0.21740(11) 0.68670(10) 0.0423(5) Uani 1 1 d . . . N1 N 0.63829(12) 0.37650(13) 0.81099(11) 0.0322(5) Uani 1 1 d . . . N2 N 0.86510(12) 0.28371(12) 0.78126(11) 0.0320(5) Uani 1 1 d . . . C1 C 0.7691(2) 0.4680(2) 0.61620(19) 0.0669(10) Uani 1 1 d . . . H1 H 0.7204 0.5031 0.5993 0.080 Uiso 1 1 calc R . . C2 C 0.8278(2) 0.4309(2) 0.57639(18) 0.0667(10) Uani 1 1 d . . . H2 H 0.8262 0.4386 0.5276 0.080 Uiso 1 1 calc R . . C3 C 0.89358(18) 0.37823(18) 0.61377(14) 0.0431(7) Uani 1 1 d . . . H3 H 0.9392 0.3462 0.5929 0.052 Uiso 1 1 calc R . . C4 C 0.88199(16) 0.38018(16) 0.68299(15) 0.0370(7) Uani 1 1 d . . . C5 C 0.92955(16) 0.33045(17) 0.74100(15) 0.0424(7) Uani 1 1 d . . . H5A H 0.9711 0.2870 0.7221 0.051 Uiso 1 1 calc R . . H5B H 0.9641 0.3727 0.7712 0.051 Uiso 1 1 calc R . . C6 C 0.90668(15) 0.22120(16) 0.82889(14) 0.0350(6) Uani 1 1 d . . . C7 C 0.93418(16) 0.24698(18) 0.89643(14) 0.0389(7) Uani 1 1 d . . . C8 C 0.97425(18) 0.1840(2) 0.94123(16) 0.0489(8) Uani 1 1 d . . . H8 H 0.9931 0.2013 0.9870 0.059 Uiso 1 1 calc R . . C9 C 0.98697(19) 0.0976(2) 0.92044(18) 0.0549(8) Uani 1 1 d . . . H9 H 1.0140 0.0555 0.9517 0.066 Uiso 1 1 calc R . . C10 C 0.96046(18) 0.07216(19) 0.85410(18) 0.0535(8) Uani 1 1 d . . . H10 H 0.9695 0.0123 0.8400 0.064 Uiso 1 1 calc R . . C11 C 0.92069(16) 0.13229(17) 0.80729(16) 0.0424(7) Uani 1 1 d . . . C12 C 0.8959(2) 0.10197(19) 0.73414(17) 0.0565(9) Uani 1 1 d . . . H12 H 0.8626 0.1517 0.7101 0.068 Uiso 1 1 calc R . . C13 C 0.8361(2) 0.0198(2) 0.7319(2) 0.0871(12) Uani 1 1 d . . . H13A H 0.8675 -0.0303 0.7547 0.131 Uiso 1 1 calc R . . H13B H 0.8200 0.0043 0.6836 0.131 Uiso 1 1 calc R . . H13C H 0.7824 0.0328 0.7561 0.131 Uiso 1 1 calc R . . C14 C 0.9787(2) 0.0836(2) 0.69407(18) 0.0763(11) Uani 1 1 d . . . H14A H 1.0162 0.1370 0.6950 0.114 Uiso 1 1 calc R . . H14B H 0.9610 0.0685 0.6460 0.114 Uiso 1 1 calc R . . H14C H 1.0117 0.0337 0.7156 0.114 Uiso 1 1 calc R . . C15 C 1.0106(2) 0.3870(2) 0.94103(18) 0.0672(10) Uani 1 1 d . . . H15A H 1.0397 0.3564 0.9809 0.101 Uiso 1 1 calc R . . H15B H 1.0006 0.4496 0.9529 0.101 Uiso 1 1 calc R . . H15C H 1.0482 0.3838 0.9015 0.101 Uiso 1 1 calc R . . C16 C 0.92167(18) 0.34191(18) 0.92199(15) 0.0475(7) Uani 1 1 d . . . H16 H 0.8922 0.3766 0.8830 0.057 Uiso 1 1 calc R . . C17 C 0.8610(2) 0.3443(2) 0.98206(17) 0.0716(10) Uani 1 1 d . . . H17A H 0.8035 0.3187 0.9673 0.107 Uiso 1 1 calc R . . H17B H 0.8530 0.4063 0.9967 0.107 Uiso 1 1 calc R . . H17C H 0.8875 0.3096 1.0209 0.107 Uiso 1 1 calc R . . C18 C 0.63193(19) 0.10938(18) 0.94909(16) 0.0491(8) Uani 1 1 d . . . H18 H 0.6307 0.0580 0.9778 0.059 Uiso 1 1 calc R . . C19 C 0.68981(18) 0.12162(17) 0.90009(15) 0.0459(7) Uani 1 1 d . . . H19 H 0.7342 0.0791 0.8910 0.055 Uiso 1 1 calc R . . C20 C 0.67981(16) 0.20430(17) 0.86199(14) 0.0383(7) Uani 1 1 d . . . C21 C 0.61161(16) 0.25153(17) 0.88717(13) 0.0338(6) Uani 1 1 d . . . C22 C 0.58161(17) 0.34330(16) 0.86426(14) 0.0388(7) Uani 1 1 d . . . H22A H 0.5195 0.3408 0.8455 0.047 Uiso 1 1 calc R . . H22B H 0.5846 0.3844 0.9044 0.047 Uiso 1 1 calc R . . C23 C 0.61677(15) 0.46549(16) 0.78938(14) 0.0325(6) Uani 1 1 d . . . C24 C 0.55744(16) 0.48040(17) 0.73178(14) 0.0363(6) Uani 1 1 d . . . C25 C 0.54582(17) 0.56664(18) 0.70601(15) 0.0445(7) Uani 1 1 d . . . H25 H 0.5080 0.5766 0.6659 0.053 Uiso 1 1 calc R . . C26 C 0.58891(18) 0.63789(19) 0.73829(17) 0.0497(8) Uani 1 1 d . . . H26 H 0.5811 0.6964 0.7200 0.060 Uiso 1 1 calc R . . C27 C 0.64281(17) 0.62438(18) 0.79663(16) 0.0467(8) Uani 1 1 d . . . H27 H 0.6711 0.6741 0.8189 0.056 Uiso 1 1 calc R . . C28 C 0.65712(16) 0.53907(17) 0.82409(15) 0.0389(7) Uani 1 1 d . . . C29 C 0.71572(18) 0.52704(18) 0.88937(16) 0.0505(8) Uani 1 1 d . . . H29 H 0.7238 0.4615 0.8972 0.061 Uiso 1 1 calc R . . C30 C 0.8081(2) 0.5688(2) 0.88278(19) 0.0729(10) Uani 1 1 d . . . H30A H 0.8364 0.5415 0.8436 0.109 Uiso 1 1 calc R . . H30B H 0.8445 0.5580 0.9255 0.109 Uiso 1 1 calc R . . H30C H 0.8021 0.6331 0.8751 0.109 Uiso 1 1 calc R . . C31 C 0.6725(2) 0.5657(2) 0.95239(17) 0.0688(10) Uani 1 1 d . . . H31A H 0.6619 0.6297 0.9453 0.103 Uiso 1 1 calc R . . H31B H 0.7118 0.5569 0.9938 0.103 Uiso 1 1 calc R . . H31C H 0.6162 0.5353 0.9584 0.103 Uiso 1 1 calc R . . C32 C 0.50531(17) 0.40422(19) 0.69812(14) 0.0438(7) Uani 1 1 d . . . H32 H 0.5271 0.3476 0.7205 0.053 Uiso 1 1 calc R . . C33 C 0.5180(2) 0.3961(2) 0.62057(16) 0.0675(10) Uani 1 1 d . . . H33A H 0.4957 0.4500 0.5969 0.101 Uiso 1 1 calc R . . H33B H 0.4855 0.3440 0.6021 0.101 Uiso 1 1 calc R . . H33C H 0.5810 0.3890 0.6130 0.101 Uiso 1 1 calc R . . C34 C 0.40617(18) 0.4126(2) 0.71090(17) 0.0561(8) Uani 1 1 d . . . H34A H 0.3984 0.4145 0.7608 0.084 Uiso 1 1 calc R . . H34B H 0.3743 0.3612 0.6906 0.084 Uiso 1 1 calc R . . H34C H 0.3828 0.4676 0.6894 0.084 Uiso 1 1 calc R . . C35 C 0.60392(19) 0.1591(2) 0.69069(18) 0.0614(9) Uani 1 1 d . . . H35A H 0.5521 0.1935 0.7048 0.074 Uiso 1 1 calc R . . H35B H 0.6163 0.1108 0.7248 0.074 Uiso 1 1 calc R . . C36 C 0.5872(3) 0.1221(3) 0.6212(2) 0.1061(16) Uani 1 1 d . . . H36A H 0.5723 0.0579 0.6239 0.127 Uiso 1 1 calc R . . H36B H 0.5373 0.1536 0.5966 0.127 Uiso 1 1 calc R . . C37 C 0.6684(2) 0.1344(2) 0.58480(18) 0.0690(10) Uani 1 1 d . . . H37A H 0.6548 0.1441 0.5347 0.083 Uiso 1 1 calc R . . H37B H 0.7074 0.0816 0.5908 0.083 Uiso 1 1 calc R . . C38 C 0.71123(18) 0.21450(19) 0.61696(15) 0.0482(7) Uani 1 1 d . . . H38A H 0.7764 0.2092 0.6179 0.058 Uiso 1 1 calc R . . H38B H 0.6932 0.2691 0.5910 0.058 Uiso 1 1 calc R . . C39 C 0.8199(3) 0.7408(3) 0.6874(2) 0.1004(14) Uani 1 1 d . . . H39A H 0.7956 0.6853 0.7052 0.151 Uiso 1 1 calc R . . H39B H 0.8381 0.7800 0.7262 0.151 Uiso 1 1 calc R . . H39C H 0.8713 0.7271 0.6607 0.151 Uiso 1 1 calc R . . C40 C 0.7494(3) 0.7878(3) 0.6407(2) 0.0948(14) Uani 1 1 d . . . H40A H 0.7754 0.8427 0.6219 0.114 Uiso 1 1 calc R . . H40B H 0.7003 0.8061 0.6692 0.114 Uiso 1 1 calc R . . C41 C 0.7115(2) 0.7311(2) 0.5801(2) 0.0757(11) Uani 1 1 d . . . H41A H 0.6863 0.6756 0.5986 0.091 Uiso 1 1 calc R . . H41B H 0.6627 0.7644 0.5555 0.091 Uiso 1 1 calc R . . C42 C 0.7403(2) 0.6567(2) 0.4663(2) 0.0811(11) Uani 1 1 d . . . H42A H 0.6938 0.6937 0.4425 0.097 Uiso 1 1 calc R . . H42B H 0.7123 0.6010 0.4817 0.097 Uiso 1 1 calc R . . C43 C 0.7788(2) 0.7068(2) 0.52920(19) 0.0709(10) Uani 1 1 d . . . H43A H 0.8251 0.6695 0.5530 0.085 Uiso 1 1 calc R . . H43B H 0.8073 0.7621 0.5135 0.085 Uiso 1 1 calc R . . C44 C 0.8108(3) 0.6334(3) 0.4149(2) 0.1048(14) Uani 1 1 d . . . H44A H 0.8386 0.6884 0.3993 0.157 Uiso 1 1 calc R . . H44B H 0.7829 0.6021 0.3749 0.157 Uiso 1 1 calc R . . H44C H 0.8559 0.5949 0.4377 0.157 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.0311(3) 0.0310(3) 0.0390(3) -0.0004(2) 0.0044(2) 0.0035(2) S1 0.0514(5) 0.0461(4) 0.0628(6) 0.0098(4) 0.0079(4) 0.0102(4) S2 0.0576(5) 0.0493(5) 0.0387(5) 0.0057(4) 0.0087(4) -0.0056(4) O1 0.0386(10) 0.0461(11) 0.0431(12) -0.0075(10) 0.0095(9) -0.0098(8) N1 0.0322(11) 0.0321(12) 0.0328(13) 0.0033(10) 0.0054(10) 0.0031(9) N2 0.0329(11) 0.0281(11) 0.0353(13) 0.0031(10) 0.0042(10) 0.0045(9) C1 0.056(2) 0.071(2) 0.072(3) 0.039(2) -0.013(2) -0.0048(17) C2 0.069(2) 0.089(3) 0.041(2) 0.017(2) -0.0020(19) -0.032(2) C3 0.0465(17) 0.0491(17) 0.0340(18) -0.0014(15) 0.0042(14) -0.0141(14) C4 0.0379(15) 0.0292(14) 0.0441(18) 0.0012(13) 0.0056(13) -0.0060(11) C5 0.0379(15) 0.0373(15) 0.0523(19) 0.0024(15) 0.0043(14) -0.0006(12) C6 0.0272(13) 0.0345(15) 0.0438(17) 0.0037(14) 0.0064(12) 0.0040(11) C7 0.0351(15) 0.0444(16) 0.0377(17) 0.0056(14) 0.0069(13) 0.0053(12) C8 0.0502(18) 0.0568(19) 0.0399(18) 0.0110(16) 0.0044(15) 0.0077(15) C9 0.0508(18) 0.050(2) 0.064(2) 0.0237(18) 0.0026(18) 0.0093(15) C10 0.0514(18) 0.0367(17) 0.072(2) 0.0088(17) 0.0040(18) 0.0100(14) C11 0.0364(15) 0.0357(16) 0.055(2) 0.0027(15) 0.0015(14) 0.0077(12) C12 0.066(2) 0.0361(17) 0.066(2) -0.0078(16) -0.0075(18) 0.0173(15) C13 0.082(3) 0.068(2) 0.109(3) -0.028(2) -0.014(2) -0.004(2) C14 0.100(3) 0.060(2) 0.070(3) -0.010(2) 0.015(2) 0.015(2) C15 0.077(2) 0.053(2) 0.070(2) -0.0144(19) -0.006(2) 0.0008(17) C16 0.0553(18) 0.0501(18) 0.0368(18) -0.0042(15) 0.0010(15) 0.0096(14) C17 0.077(2) 0.080(2) 0.059(2) -0.008(2) 0.016(2) 0.0199(19) C18 0.0606(19) 0.0401(17) 0.0457(19) 0.0107(15) -0.0060(16) -0.0049(14) C19 0.0478(17) 0.0384(16) 0.051(2) 0.0062(15) -0.0031(15) 0.0037(13) C20 0.0359(14) 0.0390(15) 0.0397(17) 0.0006(14) 0.0000(13) -0.0005(12) C21 0.0362(14) 0.0343(14) 0.0307(16) 0.0008(12) -0.0005(12) -0.0042(11) C22 0.0394(15) 0.0413(16) 0.0359(17) -0.0023(14) 0.0044(13) 0.0020(12) C23 0.0313(13) 0.0318(14) 0.0353(16) 0.0003(13) 0.0102(12) 0.0048(11) C24 0.0334(14) 0.0404(16) 0.0358(16) 0.0015(14) 0.0079(13) 0.0081(12) C25 0.0407(16) 0.0476(18) 0.0457(19) 0.0095(15) 0.0055(14) 0.0135(14) C26 0.0450(17) 0.0402(17) 0.066(2) 0.0177(17) 0.0182(17) 0.0116(14) C27 0.0414(16) 0.0329(16) 0.066(2) -0.0026(16) 0.0071(16) 0.0001(13) C28 0.0332(14) 0.0381(16) 0.0462(18) 0.0025(14) 0.0081(13) 0.0062(12) C29 0.0540(18) 0.0352(16) 0.061(2) -0.0051(16) -0.0093(17) -0.0008(14) C30 0.054(2) 0.074(2) 0.089(3) -0.008(2) -0.0168(19) -0.0070(17) C31 0.089(3) 0.064(2) 0.053(2) -0.0066(19) -0.005(2) 0.0038(19) C32 0.0441(16) 0.0466(17) 0.0397(18) -0.0040(15) -0.0060(14) 0.0115(13) C33 0.066(2) 0.089(3) 0.047(2) -0.0186(19) -0.0034(17) 0.0155(19) C34 0.0505(18) 0.0558(19) 0.062(2) -0.0030(17) 0.0017(17) -0.0013(15) C35 0.0510(19) 0.065(2) 0.069(2) -0.0062(19) 0.0104(18) -0.0255(16) C36 0.091(3) 0.135(4) 0.094(3) -0.038(3) 0.020(3) -0.069(3) C37 0.088(3) 0.063(2) 0.055(2) -0.0105(19) -0.002(2) -0.0121(19) C38 0.0454(17) 0.0583(19) 0.0414(18) -0.0035(16) 0.0066(14) -0.0050(14) C39 0.093(3) 0.117(3) 0.092(3) 0.008(3) 0.015(3) -0.015(3) C40 0.094(3) 0.080(3) 0.114(4) -0.012(3) 0.042(3) -0.015(2) C41 0.063(2) 0.068(2) 0.097(3) 0.014(2) 0.017(2) -0.0020(19) C42 0.082(3) 0.063(2) 0.095(3) 0.002(2) -0.023(2) -0.006(2) C43 0.064(2) 0.063(2) 0.085(3) 0.006(2) -0.004(2) -0.0047(18) C44 0.121(4) 0.098(3) 0.092(3) -0.019(3) -0.018(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 N2 2.0468(19) . ? Sc1 N1 2.0564(19) . ? Sc1 O1 2.1526(19) . ? Sc1 C20 2.203(3) . ? Sc1 S1 2.9697(9) . ? S1 C1 1.716(3) . ? S1 C4 1.717(3) . ? S2 C18 1.717(3) . ? S2 C21 1.743(3) . ? O1 C38 1.451(3) . ? O1 C35 1.462(3) . ? N1 C23 1.430(3) . ? N1 C22 1.465(3) . ? N2 C6 1.434(3) . ? N2 C5 1.462(3) . ? C1 C2 1.330(4) . ? C1 H1 0.9500 . ? C2 C3 1.435(4) . ? C2 H2 0.9500 . ? C3 C4 1.361(4) . ? C3 H3 0.9500 . ? C4 C5 1.497(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.403(4) . ? C6 C11 1.416(3) . ? C7 C8 1.397(4) . ? C7 C16 1.521(4) . ? C8 C9 1.372(4) . ? C8 H8 0.9500 . ? C9 C10 1.377(4) . ? C9 H9 0.9500 . ? C10 C11 1.390(4) . ? C10 H10 0.9500 . ? C11 C12 1.513(4) . ? C12 C13 1.528(4) . ? C12 C14 1.536(4) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.533(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.522(4) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.340(4) . ? C18 H18 0.9500 . ? C19 C20 1.445(3) . ? C19 H19 0.9500 . ? C20 C21 1.365(3) . ? C21 C22 1.507(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.409(4) . ? C23 C28 1.412(3) . ? C24 C25 1.393(3) . ? C24 C32 1.514(4) . ? C25 C26 1.382(4) . ? C25 H25 0.9500 . ? C26 C27 1.370(4) . ? C26 H26 0.9500 . ? C27 C28 1.397(3) . ? C27 H27 0.9500 . ? C28 C29 1.513(4) . ? C29 C31 1.530(4) . ? C29 C30 1.545(4) . ? C29 H29 1.0000 . ? 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 C33 1.528(4) . ? C32 C34 1.541(3) . ? C32 H32 1.0000 . ? 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 C36 1.463(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.464(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.484(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.532(5) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.533(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C43 1.501(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.518(5) . ? C42 C44 1.541(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 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 N2 Sc1 N1 134.29(8) . . ? N2 Sc1 O1 108.03(7) . . ? N1 Sc1 O1 111.14(8) . . ? N2 Sc1 C20 110.70(9) . . ? N1 Sc1 C20 82.87(9) . . ? O1 Sc1 C20 102.51(8) . . ? N2 Sc1 S1 71.51(6) . . ? N1 Sc1 S1 82.72(6) . . ? O1 Sc1 S1 94.54(5) . . ? C20 Sc1 S1 160.76(7) . . ? C1 S1 C4 91.76(16) . . ? C1 S1 Sc1 126.21(11) . . ? C4 S1 Sc1 86.59(9) . . ? C18 S2 C21 90.41(13) . . ? C38 O1 C35 109.1(2) . . ? C38 O1 Sc1 131.93(15) . . ? C35 O1 Sc1 118.96(17) . . ? C23 N1 C22 112.91(18) . . ? C23 N1 Sc1 131.84(15) . . ? C22 N1 Sc1 115.20(15) . . ? C6 N2 C5 111.89(19) . . ? C6 N2 Sc1 115.75(14) . . ? C5 N2 Sc1 132.28(16) . . ? C2 C1 S1 111.4(3) . . ? C2 C1 H1 124.3 . . ? S1 C1 H1 124.3 . . ? C1 C2 C3 113.9(3) . . ? C1 C2 H2 123.0 . . ? C3 C2 H2 123.0 . . ? C4 C3 C2 111.1(3) . . ? C4 C3 H3 124.5 . . ? C2 C3 H3 124.5 . . ? C3 C4 C5 130.1(3) . . ? C3 C4 S1 111.8(2) . . ? C5 C4 S1 118.0(2) . . ? N2 C5 C4 109.3(2) . . ? N2 C5 H5A 109.8 . . ? C4 C5 H5A 109.8 . . ? N2 C5 H5B 109.8 . . ? C4 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? C7 C6 C11 119.5(3) . . ? C7 C6 N2 121.0(2) . . ? C11 C6 N2 119.5(2) . . ? C8 C7 C6 119.2(3) . . ? C8 C7 C16 119.2(3) . . ? C6 C7 C16 121.6(2) . . ? C9 C8 C7 121.3(3) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.7(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 121.4(3) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 119.0(3) . . ? C10 C11 C12 119.3(3) . . ? C6 C11 C12 121.7(3) . . ? C11 C12 C13 112.6(3) . . ? C11 C12 C14 111.1(3) . . ? C13 C12 C14 110.0(3) . . ? C11 C12 H12 107.7 . . ? C13 C12 H12 107.7 . . ? C14 C12 H12 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C7 C16 C17 111.2(2) . . ? C7 C16 C15 111.5(2) . . ? C17 C16 C15 111.5(3) . . ? C7 C16 H16 107.5 . . ? C17 C16 H16 107.5 . . ? C15 C16 H16 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 S2 112.0(2) . . ? C19 C18 H18 124.0 . . ? S2 C18 H18 124.0 . . ? C18 C19 C20 115.1(2) . . ? C18 C19 H19 122.5 . . ? C20 C19 H19 122.5 . . ? C21 C20 C19 108.8(2) . . ? C21 C20 Sc1 105.66(18) . . ? C19 C20 Sc1 145.5(2) . . ? C20 C21 C22 126.2(2) . . ? C20 C21 S2 113.7(2) . . ? C22 C21 S2 120.08(18) . . ? N1 C22 C21 109.74(19) . . ? N1 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? N1 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C24 C23 C28 119.5(2) . . ? C24 C23 N1 120.2(2) . . ? C28 C23 N1 120.3(2) . . ? C25 C24 C23 119.5(3) . . ? C25 C24 C32 119.6(3) . . ? C23 C24 C32 121.0(2) . . ? C26 C25 C24 120.5(3) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 C25 120.2(3) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 121.4(3) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C27 C28 C23 118.7(3) . . ? C27 C28 C29 119.9(3) . . ? C23 C28 C29 121.4(2) . . ? C28 C29 C31 111.3(2) . . ? C28 C29 C30 112.0(3) . . ? C31 C29 C30 110.1(3) . . ? C28 C29 H29 107.8 . . ? C31 C29 H29 107.8 . . ? C30 C29 H29 107.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C24 C32 C33 113.0(2) . . ? C24 C32 C34 111.0(2) . . ? C33 C32 C34 110.0(2) . . ? C24 C32 H32 107.5 . . ? C33 C32 H32 107.5 . . ? C34 C32 H32 107.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O1 C35 C36 106.0(2) . . ? O1 C35 H35A 110.5 . . ? C36 C35 H35A 110.5 . . ? O1 C35 H35B 110.5 . . ? C36 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? C37 C36 C35 106.7(3) . . ? C37 C36 H36A 110.4 . . ? C35 C36 H36A 110.4 . . ? C37 C36 H36B 110.4 . . ? C35 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? C36 C37 C38 105.0(3) . . ? C36 C37 H37A 110.7 . . ? C38 C37 H37A 110.7 . . ? C36 C37 H37B 110.7 . . ? C38 C37 H37B 110.7 . . ? H37A C37 H37B 108.8 . . ? O1 C38 C37 105.1(2) . . ? O1 C38 H38A 110.7 . . ? C37 C38 H38A 110.7 . . ? O1 C38 H38B 110.7 . . ? C37 C38 H38B 110.7 . . ? H38A C38 H38B 108.8 . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C39 C40 C41 114.5(3) . . ? C39 C40 H40A 108.6 . . ? C41 C40 H40A 108.6 . . ? C39 C40 H40B 108.6 . . ? C41 C40 H40B 108.6 . . ? H40A C40 H40B 107.6 . . ? C43 C41 C40 113.4(3) . . ? C43 C41 H41A 108.9 . . ? C40 C41 H41A 108.9 . . ? C43 C41 H41B 108.9 . . ? C40 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? C43 C42 C44 112.4(3) . . ? C43 C42 H42A 109.1 . . ? C44 C42 H42A 109.1 . . ? C43 C42 H42B 109.1 . . ? C44 C42 H42B 109.1 . . ? H42A C42 H42B 107.9 . . ? C41 C43 C42 113.6(3) . . ? C41 C43 H43A 108.8 . . ? C42 C43 H43A 108.8 . . ? C41 C43 H43B 108.8 . . ? C42 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.414 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.052 # Attachment 'complex 2.cif' data_r125m _database_code_depnum_ccdc_archive 'CCDC 641965' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H56 N O3 S Si Y' _chemical_formula_weight 663.85 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' S S 0.1246 0.1234 '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 P21/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 10.1278(7) _cell_length_b 18.1189(12) _cell_length_c 19.4029(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.2550(10) _cell_angle_gamma 90.00 _cell_volume 3550.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blok _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 1.766 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7654 _exptl_absorpt_correction_T_max 0.8029 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19754 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.05 _reflns_number_total 7006 _reflns_number_gt 4958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^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 7006 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 Y Y 0.14708(3) 0.657541(14) 0.284460(14) 0.02658(10) Uani 1 1 d . . . S S -0.12272(8) 0.87401(4) 0.29330(5) 0.0403(2) Uani 1 1 d . . . N N 0.0633(2) 0.71414(12) 0.18834(11) 0.0274(6) Uani 1 1 d . . . Si Si -0.12304(10) 0.53823(5) 0.34760(5) 0.0414(2) Uani 1 1 d . . . O1 O 0.3050(2) 0.57749(11) 0.22985(12) 0.0425(6) Uani 1 1 d . . . O2 O 0.3450(2) 0.73373(10) 0.29711(11) 0.0366(5) Uani 1 1 d . . . O3 O 0.2534(2) 0.63277(11) 0.39930(11) 0.0419(6) Uani 1 1 d . . . C1 C 0.0227(3) 0.75867(16) 0.32942(16) 0.0340(7) Uani 1 1 d . . . C2 C -0.0112(3) 0.79788(17) 0.39077(16) 0.0410(8) Uani 1 1 d . . . H2 H 0.0173 0.7816 0.4360 0.049 Uiso 1 1 calc R . . C3 C -0.0858(3) 0.85914(17) 0.37942(18) 0.0426(9) Uani 1 1 d . . . H1 H -0.1142 0.8901 0.4150 0.051 Uiso 1 1 calc R . . C4 C -0.0344(3) 0.79389(15) 0.27282(15) 0.0297(7) Uani 1 1 d . . . C5 C -0.0331(3) 0.77259(17) 0.19808(15) 0.0357(8) Uani 1 1 d . . . H5A H -0.1224 0.7554 0.1810 0.043 Uiso 1 1 calc R . . H5B H -0.0111 0.8164 0.1707 0.043 Uiso 1 1 calc R . . C6 C 0.0715(3) 0.69721(15) 0.11677(14) 0.0266(6) Uani 1 1 d . . . C7 C 0.1722(3) 0.72863(15) 0.07910(14) 0.0287(7) Uani 1 1 d . . . C8 C 0.1808(3) 0.71031(17) 0.00991(15) 0.0367(8) Uani 1 1 d . . . H8 H 0.2481 0.7319 -0.0151 0.044 Uiso 1 1 calc R . . C9 C 0.0931(3) 0.66134(18) -0.02285(16) 0.0411(8) Uani 1 1 d . . . H9 H 0.1013 0.6484 -0.0698 0.049 Uiso 1 1 calc R . . C10 C -0.0063(3) 0.63127(17) 0.01266(17) 0.0407(8) Uani 1 1 d . . . H10 H -0.0675 0.5983 -0.0105 0.049 Uiso 1 1 calc R . . C11 C -0.0193(3) 0.64800(16) 0.08183(16) 0.0320(7) Uani 1 1 d . . . C12 C 0.2729(3) 0.78295(16) 0.11279(15) 0.0345(7) Uani 1 1 d . . . H15 H 0.2819 0.7720 0.1634 0.041 Uiso 1 1 calc R . . C13 C 0.2254(4) 0.86262(18) 0.1040(2) 0.0525(10) Uani 1 1 d . . . H17A H 0.2107 0.8741 0.0547 0.079 Uiso 1 1 calc R . . H17B H 0.2926 0.8960 0.1255 0.079 Uiso 1 1 calc R . . H17C H 0.1424 0.8688 0.1263 0.079 Uiso 1 1 calc R . . C14 C 0.4108(3) 0.77611(19) 0.08571(17) 0.0459(9) Uani 1 1 d . . . H16A H 0.4381 0.7242 0.0867 0.069 Uiso 1 1 calc R . . H16B H 0.4743 0.8053 0.1150 0.069 Uiso 1 1 calc R . . H16C H 0.4081 0.7945 0.0381 0.069 Uiso 1 1 calc R . . C15 C -0.1322(3) 0.61281(17) 0.11738(17) 0.0401(8) Uani 1 1 d . . . H12 H -0.1201 0.6255 0.1676 0.048 Uiso 1 1 calc R . . C16 C -0.1320(4) 0.52871(19) 0.11114(19) 0.0578(10) Uani 1 1 d . . . H14A H -0.1525 0.5147 0.0627 0.087 Uiso 1 1 calc R . . H14B H -0.1990 0.5079 0.1395 0.087 Uiso 1 1 calc R . . H14C H -0.0446 0.5096 0.1271 0.087 Uiso 1 1 calc R . . C17 C -0.2663(3) 0.6443(2) 0.0889(2) 0.0620(11) Uani 1 1 d . . . H13A H -0.2656 0.6981 0.0941 0.093 Uiso 1 1 calc R . . H13B H -0.3371 0.6234 0.1147 0.093 Uiso 1 1 calc R . . H13C H -0.2817 0.6315 0.0399 0.093 Uiso 1 1 calc R . . C18 C 0.0276(3) 0.54292(16) 0.30183(15) 0.0314(7) Uani 1 1 d . . . H30A H 0.0055 0.5218 0.2553 0.038 Uiso 1 1 calc R . . H30B H 0.0918 0.5087 0.3259 0.038 Uiso 1 1 calc R . . C19 C -0.2676(4) 0.5784(3) 0.2942(3) 0.0883(16) Uani 1 1 d . . . H32A H -0.2539 0.6315 0.2883 0.132 Uiso 1 1 calc R . . H32B H -0.3489 0.5702 0.3176 0.132 Uiso 1 1 calc R . . H32C H -0.2756 0.5544 0.2488 0.132 Uiso 1 1 calc R . . C20 C -0.1039(5) 0.5890(2) 0.4305(2) 0.0932(17) Uani 1 1 d . . . H33A H -0.0314 0.5673 0.4600 0.140 Uiso 1 1 calc R . . H33B H -0.1863 0.5858 0.4538 0.140 Uiso 1 1 calc R . . H33C H -0.0839 0.6409 0.4216 0.140 Uiso 1 1 calc R . . C21 C -0.1775(4) 0.44314(19) 0.3700(2) 0.0571(10) Uani 1 1 d . . . H31A H -0.1871 0.4130 0.3280 0.086 Uiso 1 1 calc R . . H31B H -0.2627 0.4458 0.3908 0.086 Uiso 1 1 calc R . . H31C H -0.1112 0.4208 0.4030 0.086 Uiso 1 1 calc R . . C22 C 0.3094(4) 0.49848(18) 0.2245(2) 0.0648(12) Uani 1 1 d . . . H25A H 0.2360 0.4756 0.2479 0.078 Uiso 1 1 calc R . . H25B H 0.3945 0.4791 0.2455 0.078 Uiso 1 1 calc R . . C23 C 0.2953(4) 0.4831(2) 0.1483(2) 0.0708(13) Uani 1 1 d . . . H24A H 0.2010 0.4788 0.1315 0.085 Uiso 1 1 calc R . . H24B H 0.3420 0.4371 0.1372 0.085 Uiso 1 1 calc R . . C24 C 0.3590(5) 0.5499(2) 0.1169(2) 0.0727(13) Uani 1 1 d . . . H23A H 0.4430 0.5361 0.0972 0.087 Uiso 1 1 calc R . . H23B H 0.2988 0.5721 0.0801 0.087 Uiso 1 1 calc R . . C25 C 0.3840(3) 0.60264(19) 0.17634(17) 0.0454(9) Uani 1 1 d . . . H22A H 0.4790 0.6026 0.1927 0.054 Uiso 1 1 calc R . . H22B H 0.3583 0.6534 0.1620 0.054 Uiso 1 1 calc R . . C26 C 0.3439(3) 0.81392(16) 0.29948(18) 0.0417(8) Uani 1 1 d . . . H18A H 0.3302 0.8315 0.3467 0.050 Uiso 1 1 calc R . . H18B H 0.2724 0.8339 0.2672 0.050 Uiso 1 1 calc R . . C27 C 0.4782(4) 0.83767(17) 0.27809(19) 0.0477(9) Uani 1 1 d . . . H19A H 0.5168 0.8765 0.3094 0.057 Uiso 1 1 calc R . . H19B H 0.4714 0.8568 0.2302 0.057 Uiso 1 1 calc R . . C28 C 0.5619(4) 0.76793(19) 0.2835(2) 0.0526(10) Uani 1 1 d . . . H20A H 0.5805 0.7497 0.2371 0.063 Uiso 1 1 calc R . . H20B H 0.6468 0.7769 0.3108 0.063 Uiso 1 1 calc R . . C29 C 0.4780(3) 0.71361(17) 0.31951(19) 0.0446(9) Uani 1 1 d . . . H21A H 0.4974 0.6624 0.3057 0.054 Uiso 1 1 calc R . . H21B H 0.4935 0.7180 0.3703 0.054 Uiso 1 1 calc R . . C30 C 0.3116(4) 0.56532(18) 0.42757(19) 0.0559(10) Uani 1 1 d . . . H29A H 0.3489 0.5354 0.3910 0.067 Uiso 1 1 calc R . . H29B H 0.2450 0.5354 0.4499 0.067 Uiso 1 1 calc R . . C31 C 0.4194(4) 0.5910(2) 0.47992(19) 0.0587(11) Uani 1 1 d . . . H28A H 0.5047 0.5956 0.4585 0.070 Uiso 1 1 calc R . . H28B H 0.4306 0.5559 0.5190 0.070 Uiso 1 1 calc R . . C32 C 0.3735(4) 0.66513(18) 0.50415(18) 0.0486(9) Uani 1 1 d . . . H27A H 0.3490 0.6622 0.5525 0.058 Uiso 1 1 calc R . . H27B H 0.4441 0.7026 0.5013 0.058 Uiso 1 1 calc R . . C33 C 0.2549(4) 0.68453(19) 0.45634(17) 0.0483(9) Uani 1 1 d . . . H26A H 0.1726 0.6801 0.4806 0.058 Uiso 1 1 calc R . . H26B H 0.2621 0.7358 0.4393 0.058 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 Y 0.03073(17) 0.02334(15) 0.02574(16) 0.00026(13) 0.00255(11) 0.00253(13) S 0.0379(5) 0.0309(4) 0.0529(6) -0.0037(4) 0.0089(4) 0.0080(4) N 0.0277(14) 0.0309(13) 0.0237(13) 0.0019(11) 0.0033(11) 0.0052(11) Si 0.0447(6) 0.0366(5) 0.0450(6) 0.0032(4) 0.0175(5) 0.0024(4) O1 0.0436(13) 0.0267(11) 0.0598(15) -0.0001(11) 0.0216(12) 0.0031(10) O2 0.0343(12) 0.0261(11) 0.0484(14) 0.0028(10) -0.0034(10) -0.0007(9) O3 0.0585(15) 0.0319(11) 0.0333(13) 0.0018(10) -0.0107(11) -0.0027(11) C1 0.0381(19) 0.0318(16) 0.0330(18) -0.0024(14) 0.0084(15) 0.0032(14) C2 0.054(2) 0.0404(19) 0.0307(18) 0.0002(15) 0.0132(16) 0.0028(17) C3 0.048(2) 0.0349(18) 0.047(2) -0.0114(16) 0.0182(17) 0.0008(15) C4 0.0277(16) 0.0271(15) 0.0357(18) -0.0022(14) 0.0111(14) 0.0004(13) C5 0.0366(19) 0.0354(17) 0.0354(18) 0.0040(15) 0.0043(15) 0.0081(14) C6 0.0292(16) 0.0264(15) 0.0238(16) 0.0016(13) -0.0004(13) 0.0053(13) C7 0.0333(17) 0.0286(16) 0.0242(16) 0.0036(13) 0.0016(13) 0.0023(13) C8 0.040(2) 0.0413(18) 0.0296(18) -0.0001(15) 0.0068(15) 0.0018(15) C9 0.052(2) 0.047(2) 0.0245(17) -0.0029(16) 0.0044(16) 0.0075(18) C10 0.049(2) 0.0365(17) 0.0347(19) -0.0061(15) -0.0076(17) -0.0027(16) C11 0.0330(17) 0.0291(16) 0.0338(18) -0.0001(14) 0.0008(14) 0.0001(13) C12 0.0395(19) 0.0383(17) 0.0261(16) 0.0030(14) 0.0047(14) -0.0083(15) C13 0.054(2) 0.0386(19) 0.065(3) -0.0067(18) 0.006(2) -0.0081(17) C14 0.040(2) 0.054(2) 0.043(2) 0.0062(17) 0.0062(17) -0.0108(17) C15 0.040(2) 0.0404(19) 0.040(2) 0.0011(16) 0.0002(16) -0.0111(15) C16 0.073(3) 0.044(2) 0.056(2) -0.0005(19) 0.008(2) -0.021(2) C17 0.039(2) 0.074(3) 0.072(3) 0.010(2) 0.001(2) -0.012(2) C18 0.0324(17) 0.0311(16) 0.0306(17) 0.0004(14) 0.0018(14) 0.0013(13) C19 0.052(3) 0.097(3) 0.120(4) 0.046(3) 0.032(3) 0.032(2) C20 0.133(4) 0.080(3) 0.075(3) -0.030(3) 0.060(3) -0.035(3) C21 0.052(2) 0.055(2) 0.066(3) 0.005(2) 0.018(2) -0.0086(19) C22 0.079(3) 0.0280(18) 0.095(3) 0.005(2) 0.052(3) 0.0128(18) C23 0.053(3) 0.047(2) 0.115(4) -0.032(2) 0.025(3) -0.0073(19) C24 0.106(4) 0.056(3) 0.058(3) -0.005(2) 0.021(3) 0.003(2) C25 0.045(2) 0.0418(19) 0.052(2) 0.0016(17) 0.0184(18) -0.0001(16) C26 0.058(2) 0.0242(15) 0.043(2) -0.0031(15) 0.0018(17) 0.0020(16) C27 0.061(2) 0.0363(18) 0.044(2) 0.0046(17) -0.0029(18) -0.0152(18) C28 0.044(2) 0.050(2) 0.065(3) 0.0005(19) 0.0050(19) -0.0097(18) C29 0.039(2) 0.0356(18) 0.058(2) 0.0025(17) -0.0044(17) -0.0002(15) C30 0.084(3) 0.0319(18) 0.049(2) 0.0046(17) -0.017(2) 0.0068(19) C31 0.066(3) 0.058(2) 0.049(2) 0.0055(19) -0.013(2) 0.012(2) C32 0.062(2) 0.045(2) 0.038(2) 0.0049(17) -0.0066(18) -0.0110(18) C33 0.065(3) 0.0417(19) 0.037(2) -0.0056(16) -0.0045(18) 0.0030(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y N 2.239(2) . ? Y C1 2.423(3) . ? Y O2 2.431(2) . ? Y C18 2.439(3) . ? Y O3 2.444(2) . ? Y O1 2.457(2) . ? S C3 1.706(4) . ? S C4 1.766(3) . ? N C6 1.430(3) . ? N C5 1.462(3) . ? Si C18 1.824(3) . ? Si C20 1.851(4) . ? Si C21 1.870(3) . ? Si C19 1.877(4) . ? O1 C25 1.432(4) . ? O1 C22 1.436(4) . ? O2 C29 1.432(4) . ? O2 C26 1.454(3) . ? O3 C30 1.447(4) . ? O3 C33 1.450(4) . ? C1 C4 1.362(4) . ? C1 C2 1.449(4) . ? C2 C3 1.352(4) . ? C2 H2 0.9500 . ? C3 H1 0.9500 . ? C4 C5 1.502(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C11 1.417(4) . ? C6 C7 1.418(4) . ? C7 C8 1.392(4) . ? C7 C12 1.529(4) . ? C8 C9 1.377(4) . ? C8 H8 0.9500 . ? C9 C10 1.374(5) . ? C9 H9 0.9500 . ? C10 C11 1.392(4) . ? C10 H10 0.9500 . ? C11 C15 1.518(4) . ? C12 C13 1.527(4) . ? C12 C14 1.533(4) . ? C12 H15 1.0000 . ? C13 H17A 0.9800 . ? C13 H17B 0.9800 . ? C13 H17C 0.9800 . ? C14 H16A 0.9800 . ? C14 H16B 0.9800 . ? C14 H16C 0.9800 . ? C15 C16 1.529(4) . ? C15 C17 1.537(5) . ? C15 H12 1.0000 . ? C16 H14A 0.9800 . ? C16 H14B 0.9800 . ? C16 H14C 0.9800 . ? C17 H13A 0.9800 . ? C17 H13B 0.9800 . ? C17 H13C 0.9800 . ? C18 H30A 0.9900 . ? C18 H30B 0.9900 . ? C19 H32A 0.9800 . ? C19 H32B 0.9800 . ? C19 H32C 0.9800 . ? C20 H33A 0.9800 . ? C20 H33B 0.9800 . ? C20 H33C 0.9800 . ? C21 H31A 0.9800 . ? C21 H31B 0.9800 . ? C21 H31C 0.9800 . ? C22 C23 1.500(5) . ? C22 H25A 0.9900 . ? C22 H25B 0.9900 . ? C23 C24 1.520(5) . ? C23 H24A 0.9900 . ? C23 H24B 0.9900 . ? C24 C25 1.504(5) . ? C24 H23A 0.9900 . ? C24 H23B 0.9900 . ? C25 H22A 0.9900 . ? C25 H22B 0.9900 . ? C26 C27 1.514(5) . ? C26 H18A 0.9900 . ? C26 H18B 0.9900 . ? C27 C28 1.521(5) . ? C27 H19A 0.9900 . ? C27 H19B 0.9900 . ? C28 C29 1.506(5) . ? C28 H20A 0.9900 . ? C28 H20B 0.9900 . ? C29 H21A 0.9900 . ? C29 H21B 0.9900 . ? C30 C31 1.508(5) . ? C30 H29A 0.9900 . ? C30 H29B 0.9900 . ? C31 C32 1.508(5) . ? C31 H28A 0.9900 . ? C31 H28B 0.9900 . ? C32 C33 1.504(4) . ? C32 H27A 0.9900 . ? C32 H27B 0.9900 . ? C33 H26A 0.9900 . ? C33 H26B 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 N Y C1 77.20(9) . . ? N Y O2 94.74(8) . . ? C1 Y O2 88.91(9) . . ? N Y C18 110.11(9) . . ? C1 Y C18 108.52(10) . . ? O2 Y C18 152.02(8) . . ? N Y O3 163.28(8) . . ? C1 Y O3 90.94(9) . . ? O2 Y O3 73.02(7) . . ? C18 Y O3 84.68(9) . . ? N Y O1 97.45(8) . . ? C1 Y O1 167.01(9) . . ? O2 Y O1 79.66(7) . . ? C18 Y O1 84.40(8) . . ? O3 Y O1 91.59(8) . . ? C3 S C4 90.73(15) . . ? C6 N C5 111.6(2) . . ? C6 N Y 131.65(17) . . ? C5 N Y 116.07(17) . . ? C18 Si C20 111.27(18) . . ? C18 Si C21 115.34(15) . . ? C20 Si C21 105.64(19) . . ? C18 Si C19 111.10(17) . . ? C20 Si C19 108.3(2) . . ? C21 Si C19 104.71(19) . . ? C25 O1 C22 104.1(3) . . ? C25 O1 Y 122.80(18) . . ? C22 O1 Y 130.1(2) . . ? C29 O2 C26 104.7(2) . . ? C29 O2 Y 129.52(17) . . ? C26 O2 Y 124.24(18) . . ? C30 O3 C33 106.0(2) . . ? C30 O3 Y 129.82(19) . . ? C33 O3 Y 123.78(18) . . ? C4 C1 C2 108.7(3) . . ? C4 C1 Y 105.4(2) . . ? C2 C1 Y 145.9(2) . . ? C3 C2 C1 115.6(3) . . ? C3 C2 H2 122.2 . . ? C1 C2 H2 122.2 . . ? C2 C3 S 111.6(3) . . ? C2 C3 H1 124.2 . . ? S C3 H1 124.2 . . ? C1 C4 C5 128.7(3) . . ? C1 C4 S 113.3(2) . . ? C5 C4 S 118.0(2) . . ? N C5 C4 111.4(2) . . ? N C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? N C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C11 C6 C7 118.2(3) . . ? C11 C6 N 121.1(3) . . ? C7 C6 N 120.7(2) . . ? C8 C7 C6 120.0(3) . . ? C8 C7 C12 118.6(3) . . ? C6 C7 C12 121.4(3) . . ? C9 C8 C7 121.0(3) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 119.7(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 121.5(3) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 119.6(3) . . ? C10 C11 C15 118.4(3) . . ? C6 C11 C15 122.0(3) . . ? C13 C12 C7 111.5(3) . . ? C13 C12 C14 109.0(3) . . ? C7 C12 C14 113.4(3) . . ? C13 C12 H15 107.6 . . ? C7 C12 H15 107.6 . . ? C14 C12 H15 107.6 . . ? C12 C13 H17A 109.5 . . ? C12 C13 H17B 109.5 . . ? H17A C13 H17B 109.5 . . ? C12 C13 H17C 109.5 . . ? H17A C13 H17C 109.5 . . ? H17B C13 H17C 109.5 . . ? C12 C14 H16A 109.5 . . ? C12 C14 H16B 109.5 . . ? H16A C14 H16B 109.5 . . ? C12 C14 H16C 109.5 . . ? H16A C14 H16C 109.5 . . ? H16B C14 H16C 109.5 . . ? C11 C15 C16 112.2(3) . . ? C11 C15 C17 110.8(3) . . ? C16 C15 C17 110.3(3) . . ? C11 C15 H12 107.8 . . ? C16 C15 H12 107.8 . . ? C17 C15 H12 107.8 . . ? C15 C16 H14A 109.5 . . ? C15 C16 H14B 109.5 . . ? H14A C16 H14B 109.5 . . ? C15 C16 H14C 109.5 . . ? H14A C16 H14C 109.5 . . ? H14B C16 H14C 109.5 . . ? C15 C17 H13A 109.5 . . ? C15 C17 H13B 109.5 . . ? H13A C17 H13B 109.5 . . ? C15 C17 H13C 109.5 . . ? H13A C17 H13C 109.5 . . ? H13B C17 H13C 109.5 . . ? Si C18 Y 123.25(14) . . ? Si C18 H30A 106.5 . . ? Y C18 H30A 106.5 . . ? Si C18 H30B 106.5 . . ? Y C18 H30B 106.5 . . ? H30A C18 H30B 106.5 . . ? Si C19 H32A 109.5 . . ? Si C19 H32B 109.5 . . ? H32A C19 H32B 109.5 . . ? Si C19 H32C 109.5 . . ? H32A C19 H32C 109.5 . . ? H32B C19 H32C 109.5 . . ? Si C20 H33A 109.5 . . ? Si C20 H33B 109.5 . . ? H33A C20 H33B 109.5 . . ? Si C20 H33C 109.5 . . ? H33A C20 H33C 109.5 . . ? H33B C20 H33C 109.5 . . ? Si C21 H31A 109.5 . . ? Si C21 H31B 109.5 . . ? H31A C21 H31B 109.5 . . ? Si C21 H31C 109.5 . . ? H31A C21 H31C 109.5 . . ? H31B C21 H31C 109.5 . . ? O1 C22 C23 104.8(3) . . ? O1 C22 H25A 110.8 . . ? C23 C22 H25A 110.8 . . ? O1 C22 H25B 110.8 . . ? C23 C22 H25B 110.8 . . ? H25A C22 H25B 108.9 . . ? C22 C23 C24 103.6(3) . . ? C22 C23 H24A 111.0 . . ? C24 C23 H24A 111.0 . . ? C22 C23 H24B 111.0 . . ? C24 C23 H24B 111.0 . . ? H24A C23 H24B 109.0 . . ? C25 C24 C23 104.5(3) . . ? C25 C24 H23A 110.8 . . ? C23 C24 H23A 110.8 . . ? C25 C24 H23B 110.8 . . ? C23 C24 H23B 110.8 . . ? H23A C24 H23B 108.9 . . ? O1 C25 C24 106.4(3) . . ? O1 C25 H22A 110.5 . . ? C24 C25 H22A 110.5 . . ? O1 C25 H22B 110.5 . . ? C24 C25 H22B 110.5 . . ? H22A C25 H22B 108.6 . . ? O2 C26 C27 105.4(3) . . ? O2 C26 H18A 110.7 . . ? C27 C26 H18A 110.7 . . ? O2 C26 H18B 110.7 . . ? C27 C26 H18B 110.7 . . ? H18A C26 H18B 108.8 . . ? C26 C27 C28 104.6(3) . . ? C26 C27 H19A 110.8 . . ? C28 C27 H19A 110.8 . . ? C26 C27 H19B 110.8 . . ? C28 C27 H19B 110.8 . . ? H19A C27 H19B 108.9 . . ? C29 C28 C27 104.2(3) . . ? C29 C28 H20A 110.9 . . ? C27 C28 H20A 110.9 . . ? C29 C28 H20B 110.9 . . ? C27 C28 H20B 110.9 . . ? H20A C28 H20B 108.9 . . ? O2 C29 C28 104.1(3) . . ? O2 C29 H21A 110.9 . . ? C28 C29 H21A 110.9 . . ? O2 C29 H21B 110.9 . . ? C28 C29 H21B 110.9 . . ? H21A C29 H21B 109.0 . . ? O3 C30 C31 104.4(3) . . ? O3 C30 H29A 110.9 . . ? C31 C30 H29A 110.9 . . ? O3 C30 H29B 110.9 . . ? C31 C30 H29B 110.9 . . ? H29A C30 H29B 108.9 . . ? C30 C31 C32 105.1(3) . . ? C30 C31 H28A 110.7 . . ? C32 C31 H28A 110.7 . . ? C30 C31 H28B 110.7 . . ? C32 C31 H28B 110.7 . . ? H28A C31 H28B 108.8 . . ? C33 C32 C31 105.4(3) . . ? C33 C32 H27A 110.7 . . ? C31 C32 H27A 110.7 . . ? C33 C32 H27B 110.7 . . ? C31 C32 H27B 110.7 . . ? H27A C32 H27B 108.8 . . ? O3 C33 C32 106.4(3) . . ? O3 C33 H26A 110.5 . . ? C32 C33 H26A 110.5 . . ? O3 C33 H26B 110.5 . . ? C32 C33 H26B 110.5 . . ? H26A C33 H26B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.537 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.069