# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email fraser.white@ed.ac.uk _publ_contact_author_name 'Fraser J. White' loop_ _publ_author_name 'Aakarsh Saxena' 'Hon Wai Lam.' data_hl0008 _database_code_depnum_ccdc_archive 'CCDC 809081' #TrackingRef 'hl0008.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Aakarash Saxena' _exptl_crystal_recrystallization_method 'vapour diffusion of EtOAc and Hexane' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H41 N1 O3 S1 Si1' _chemical_formula_sum 'C30 H41 N O3 S Si' _chemical_formula_weight 523.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.0485(4) _cell_length_b 16.8765(13) _cell_length_c 27.927(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2850.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9473 _cell_measurement_theta_min 2.6160 _cell_measurement_theta_max 73.3999 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.374 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.033 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72060 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 5.1574 _diffrn_reflns_number 25749 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 73.56 _reflns_number_total 5626 _reflns_number_gt 5161 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _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. #============================================================================== The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<< #============================================================================== 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 34 Completeness and resolution meet IUCr standards 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken 791_ALERT_4_G Note: The Model has Chirality at C19 (Verify) S Configuration has been determined by refining the Flack parameter. ; _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^)+(0.0503P)^2^+2.0857P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 5626 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0874(6) 0.65626(19) -0.21360(10) 0.0339(7) Uani 1 1 d . . . H1A H 1.2397 0.6598 -0.2018 0.051 Uiso 1 1 calc R . . H1B H 1.0589 0.6999 -0.2359 0.051 Uiso 1 1 calc R . . H1C H 1.0666 0.6056 -0.2301 0.051 Uiso 1 1 calc R . . C2 C 0.9298(5) 0.66159(16) -0.17218(9) 0.0244(5) Uani 1 1 d . . . C3 C 0.7440(5) 0.61365(17) -0.16997(9) 0.0273(6) Uani 1 1 d . . . H3 H 0.7179 0.5765 -0.1949 0.033 Uiso 1 1 calc R . . C4 C 0.5945(5) 0.61842(16) -0.13215(9) 0.0258(6) Uani 1 1 d . . . H4 H 0.4683 0.5849 -0.1311 0.031 Uiso 1 1 calc R . . C5 C 0.6339(5) 0.67330(15) -0.09590(9) 0.0207(5) Uani 1 1 d . . . C6 C 0.8209(5) 0.72202(17) -0.09741(9) 0.0243(6) Uani 1 1 d . . . H6 H 0.8473 0.7593 -0.0726 0.029 Uiso 1 1 calc R . . C7 C 0.9665(5) 0.71564(17) -0.13510(9) 0.0251(6) Uani 1 1 d . . . H7 H 1.0939 0.7485 -0.1359 0.030 Uiso 1 1 calc R . . C12 C 0.5776(5) 0.56454(15) 0.00764(8) 0.0186(5) Uani 1 1 d . . . C13 C 0.7668(5) 0.52302(16) -0.00452(8) 0.0207(5) Uani 1 1 d . . . H13 H 0.8891 0.5494 -0.0187 0.025 Uiso 1 1 calc R . . C14 C 0.7748(5) 0.44155(16) 0.00453(9) 0.0233(6) Uani 1 1 d . . . H14 H 0.9041 0.4127 -0.0038 0.028 Uiso 1 1 calc R . . C15 C 0.6003(5) 0.40225(15) 0.02515(8) 0.0216(6) Uani 1 1 d . . . C16 C 0.4088(5) 0.44474(16) 0.03630(8) 0.0222(5) Uani 1 1 d . . . H16 H 0.2851 0.4180 0.0496 0.027 Uiso 1 1 calc R . . C17 C 0.3980(4) 0.52609(16) 0.02800(8) 0.0209(5) Uani 1 1 d . . . H17 H 0.2686 0.5550 0.0362 0.025 Uiso 1 1 calc R . . C18 C 0.6103(6) 0.31386(16) 0.03587(9) 0.0280(6) Uani 1 1 d . . . H18A H 0.7462 0.2918 0.0213 0.034 Uiso 1 1 calc R . . H18B H 0.4823 0.2877 0.0204 0.034 Uiso 1 1 calc R . . C19 C 0.6089(5) 0.29360(15) 0.08963(9) 0.0222(6) Uani 1 1 d . . . H19 H 0.4694 0.3159 0.1033 0.027 Uiso 1 1 calc R . . C20 C 0.5996(5) 0.20431(15) 0.09644(8) 0.0207(5) Uani 1 1 d . . . C21 C 0.7736(5) 0.15544(16) 0.08180(9) 0.0223(5) Uani 1 1 d . . . H21 H 0.9018 0.1786 0.0680 0.027 Uiso 1 1 calc R . . C22 C 0.7624(5) 0.07349(16) 0.08709(9) 0.0249(6) Uani 1 1 d . . . H22 H 0.8822 0.0412 0.0769 0.030 Uiso 1 1 calc R . . C23 C 0.5757(5) 0.03893(15) 0.10734(9) 0.0249(6) Uani 1 1 d . . . H23 H 0.5667 -0.0170 0.1107 0.030 Uiso 1 1 calc R . . C24 C 0.4039(5) 0.08652(16) 0.12244(9) 0.0268(6) Uani 1 1 d . . . H24 H 0.2769 0.0632 0.1367 0.032 Uiso 1 1 calc R . . C25 C 0.4151(5) 0.16885(16) 0.11691(9) 0.0247(6) Uani 1 1 d . . . H25 H 0.2951 0.2009 0.1273 0.030 Uiso 1 1 calc R . . C26 C 0.8011(5) 0.33291(15) 0.11600(9) 0.0244(6) Uani 1 1 d . . . H26A H 0.9420 0.3139 0.1021 0.029 Uiso 1 1 calc R . . H26B H 0.7935 0.3909 0.1110 0.029 Uiso 1 1 calc R . . C27 C 0.8004(6) 0.31591(17) 0.16950(9) 0.0324(7) Uani 1 1 d . . . H27A H 0.6504 0.3262 0.1823 0.039 Uiso 1 1 calc R . . H27B H 0.8334 0.2591 0.1746 0.039 Uiso 1 1 calc R . . C28 C 0.9655(7) 0.36497(16) 0.19739(11) 0.0379(8) Uani 1 1 d . . . H28A H 0.9762 0.3445 0.2305 0.045 Uiso 1 1 calc R . . H28B H 1.1131 0.3603 0.1823 0.045 Uiso 1 1 calc R . . C31 C 1.3324(6) 0.4998(2) 0.16751(11) 0.0358(7) Uani 1 1 d . . . H31A H 1.3379 0.4586 0.1428 0.054 Uiso 1 1 calc R . . H31B H 1.4039 0.4803 0.1967 0.054 Uiso 1 1 calc R . . H31C H 1.4099 0.5472 0.1561 0.054 Uiso 1 1 calc R . . C32 C 0.9113(6) 0.56632(18) 0.12518(9) 0.0312(7) Uani 1 1 d . . . H32A H 0.7574 0.5810 0.1317 0.047 Uiso 1 1 calc R . . H32B H 0.9158 0.5263 0.0998 0.047 Uiso 1 1 calc R . . H32C H 0.9938 0.6134 0.1150 0.047 Uiso 1 1 calc R . . C33 C 1.0207(5) 0.59908(15) 0.23121(8) 0.0219(5) Uani 1 1 d . . . C34 C 1.1396(5) 0.56769(17) 0.27569(9) 0.0270(6) Uani 1 1 d . . . H34A H 1.2973 0.5612 0.2687 0.041 Uiso 1 1 calc R . . H34B H 1.0764 0.5164 0.2848 0.041 Uiso 1 1 calc R . . H34C H 1.1212 0.6053 0.3021 0.041 Uiso 1 1 calc R . . C35 C 0.7794(5) 0.6146(2) 0.24397(11) 0.0322(6) Uani 1 1 d . . . H35A H 0.7076 0.5645 0.2525 0.048 Uiso 1 1 calc R . . H35B H 0.7037 0.6381 0.2164 0.048 Uiso 1 1 calc R . . H35C H 0.7720 0.6511 0.2712 0.048 Uiso 1 1 calc R . . C36 C 1.1292(5) 0.67721(17) 0.21560(10) 0.0286(6) Uani 1 1 d . . . H36A H 1.0534 0.6977 0.1872 0.043 Uiso 1 1 calc R . . H36B H 1.2852 0.6678 0.2081 0.043 Uiso 1 1 calc R . . H36C H 1.1181 0.7160 0.2416 0.043 Uiso 1 1 calc R . . N11 N 0.5649(4) 0.64896(12) 0.00057(7) 0.0211(4) Uani 1 1 d . . . H11 H 0.6195 0.6817 0.0220 0.025 Uiso 1 1 calc R . . O9 O 0.4251(4) 0.76700(11) -0.03975(7) 0.0309(5) Uani 1 1 d . . . O10 O 0.2598(3) 0.63483(12) -0.05760(7) 0.0277(4) Uani 1 1 d . . . O29 O 0.9003(4) 0.44643(11) 0.19849(7) 0.0294(5) Uani 1 1 d . . . S8 S 0.44801(11) 0.68290(4) -0.04776(2) 0.02162(14) Uani 1 1 d . . . Si30 Si 1.03865(13) 0.52505(4) 0.18065(2) 0.02116(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0379(18) 0.0351(16) 0.0287(13) 0.0012(12) 0.0047(13) 0.0100(14) C2 0.0297(14) 0.0214(12) 0.0221(11) 0.0051(9) -0.0033(11) 0.0086(12) C3 0.0392(17) 0.0189(13) 0.0239(12) -0.0019(10) -0.0016(12) 0.0036(13) C4 0.0337(16) 0.0173(12) 0.0266(12) 0.0014(10) -0.0038(11) 0.0009(12) C5 0.0245(13) 0.0166(12) 0.0211(11) 0.0046(9) -0.0036(10) 0.0049(11) C6 0.0269(15) 0.0251(14) 0.0210(12) 0.0004(10) -0.0057(10) 0.0008(12) C7 0.0248(13) 0.0263(13) 0.0244(12) 0.0048(10) -0.0054(11) 0.0006(12) C12 0.0237(14) 0.0171(11) 0.0151(10) -0.0001(8) -0.0029(10) -0.0001(11) C13 0.0220(13) 0.0225(13) 0.0178(11) 0.0002(9) -0.0007(10) 0.0017(11) C14 0.0287(15) 0.0219(13) 0.0194(11) -0.0008(10) -0.0014(10) 0.0073(12) C15 0.0321(16) 0.0177(12) 0.0151(10) 0.0004(9) -0.0062(10) 0.0012(11) C16 0.0270(15) 0.0201(12) 0.0196(11) 0.0023(9) -0.0007(10) -0.0038(11) C17 0.0201(13) 0.0231(12) 0.0196(10) 0.0007(10) -0.0002(9) 0.0011(11) C18 0.0480(19) 0.0160(12) 0.0201(11) -0.0015(10) -0.0045(11) -0.0009(12) C19 0.0306(15) 0.0159(12) 0.0200(11) 0.0001(9) -0.0018(10) 0.0006(11) C20 0.0300(15) 0.0167(12) 0.0153(10) -0.0003(8) -0.0027(10) -0.0021(11) C21 0.0274(14) 0.0190(13) 0.0204(11) 0.0017(9) 0.0007(10) -0.0011(11) C22 0.0335(16) 0.0208(14) 0.0205(11) -0.0014(10) 0.0002(11) 0.0023(12) C23 0.0386(16) 0.0151(12) 0.0209(11) 0.0005(9) -0.0037(11) -0.0015(12) C24 0.0331(17) 0.0214(13) 0.0260(12) 0.0018(10) -0.0004(11) -0.0049(12) C25 0.0310(15) 0.0199(13) 0.0231(11) -0.0018(10) 0.0009(11) 0.0008(12) C26 0.0346(15) 0.0148(12) 0.0238(12) -0.0001(10) -0.0036(11) -0.0022(12) C27 0.056(2) 0.0166(13) 0.0246(13) 0.0026(10) -0.0126(13) -0.0068(14) C28 0.064(2) 0.0169(13) 0.0326(13) 0.0031(11) -0.0201(16) -0.0068(15) C31 0.0368(18) 0.0377(17) 0.0329(15) -0.0056(13) 0.0038(13) 0.0040(14) C32 0.0402(18) 0.0318(15) 0.0216(11) 0.0040(11) -0.0020(12) -0.0062(14) C33 0.0279(15) 0.0170(12) 0.0208(10) -0.0011(9) 0.0005(10) -0.0022(11) C34 0.0350(16) 0.0252(14) 0.0209(12) -0.0005(10) -0.0020(11) -0.0036(12) C35 0.0348(17) 0.0301(15) 0.0317(14) -0.0001(12) 0.0049(12) 0.0049(14) C36 0.0380(16) 0.0193(13) 0.0286(13) 0.0000(10) -0.0007(12) -0.0079(13) N11 0.0281(12) 0.0162(10) 0.0190(9) -0.0016(8) 0.0001(9) 0.0041(10) O9 0.0402(12) 0.0159(9) 0.0366(10) 0.0047(7) 0.0081(9) 0.0101(9) O10 0.0216(10) 0.0313(11) 0.0304(9) 0.0060(8) -0.0051(8) 0.0009(8) O29 0.0418(13) 0.0169(9) 0.0296(9) -0.0027(7) -0.0019(9) -0.0062(9) S8 0.0246(3) 0.0174(3) 0.0229(3) 0.0028(2) 0.0004(3) 0.0044(3) Si30 0.0273(4) 0.0178(3) 0.0184(3) -0.0012(2) -0.0007(3) -0.0023(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 C1 C2 1.502(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.386(4) . ? C2 C7 1.398(4) . ? C3 C4 1.393(4) . ? C3 H3 0.9500 . ? C4 C5 1.393(4) . ? C4 H4 0.9500 . ? C5 C6 1.399(4) . ? C5 S8 1.760(3) . ? C6 C7 1.377(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C12 C13 1.385(4) . ? C12 C17 1.387(4) . ? C12 N11 1.440(3) . ? C13 C14 1.399(4) . ? C13 H13 0.9500 . ? C14 C15 1.373(4) . ? C14 H14 0.9500 . ? C15 C16 1.397(4) . ? C15 C18 1.523(4) . ? C16 C17 1.394(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.540(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.520(3) . ? C19 C26 1.527(4) . ? C19 H19 1.0000 . ? C20 C25 1.389(4) . ? C20 C21 1.398(4) . ? C21 C22 1.393(4) . ? C21 H21 0.9500 . ? C22 C23 1.391(4) . ? C22 H22 0.9500 . ? C23 C24 1.380(4) . ? C23 H23 0.9500 . ? C24 C25 1.400(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.522(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.513(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O29 1.430(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C31 Si30 1.864(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 Si30 1.865(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.525(4) . ? C33 C34 1.530(4) . ? C33 C36 1.536(4) . ? C33 Si30 1.889(3) . ? 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 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? N11 S8 1.628(2) . ? N11 H11 0.8800 . ? O9 S8 1.4436(19) . ? O10 S8 1.425(2) . ? O29 Si30 1.646(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 118.5(3) . . ? C3 C2 C1 120.9(3) . . ? C7 C2 C1 120.6(3) . . ? C2 C3 C4 121.8(3) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C3 C4 C5 118.6(3) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 S8 120.5(2) . . ? C6 C5 S8 119.0(2) . . ? C7 C6 C5 119.6(3) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C2 121.1(3) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C13 C12 C17 120.7(2) . . ? C13 C12 N11 120.7(2) . . ? C17 C12 N11 118.5(2) . . ? C12 C13 C14 118.8(3) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C15 C14 C13 121.6(3) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C16 118.9(2) . . ? C14 C15 C18 121.7(3) . . ? C16 C15 C18 119.5(3) . . ? C17 C16 C15 120.5(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C12 C17 C16 119.5(3) . . ? C12 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C15 C18 C19 114.1(2) . . ? C15 C18 H18A 108.7 . . ? C19 C18 H18A 108.7 . . ? C15 C18 H18B 108.7 . . ? C19 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C20 C19 C26 113.5(2) . . ? C20 C19 C18 110.0(2) . . ? C26 C19 C18 111.7(2) . . ? C20 C19 H19 107.1 . . ? C26 C19 H19 107.1 . . ? C18 C19 H19 107.1 . . ? C25 C20 C21 118.1(2) . . ? C25 C20 C19 120.6(2) . . ? C21 C20 C19 121.3(2) . . ? C22 C21 C20 121.2(3) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C23 C22 C21 119.9(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 119.5(2) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 120.5(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C20 C25 C24 120.8(3) . . ? C20 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C27 C26 C19 112.9(2) . . ? C27 C26 H26A 109.0 . . ? C19 C26 H26A 109.0 . . ? C27 C26 H26B 109.0 . . ? C19 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? C28 C27 C26 113.6(3) . . ? C28 C27 H27A 108.8 . . ? C26 C27 H27A 108.8 . . ? C28 C27 H27B 108.8 . . ? C26 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? O29 C28 C27 110.8(3) . . ? O29 C28 H28A 109.5 . . ? C27 C28 H28A 109.5 . . ? O29 C28 H28B 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? Si30 C31 H31A 109.5 . . ? Si30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si30 C32 H32A 109.5 . . ? Si30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C33 C34 108.6(2) . . ? C35 C33 C36 109.2(2) . . ? C34 C33 C36 109.1(2) . . ? C35 C33 Si30 110.08(19) . . ? C34 C33 Si30 110.54(18) . . ? C36 C33 Si30 109.33(17) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C12 N11 S8 119.01(17) . . ? C12 N11 H11 120.5 . . ? S8 N11 H11 120.5 . . ? C28 O29 Si30 128.9(2) . . ? O10 S8 O9 120.86(14) . . ? O10 S8 N11 107.86(12) . . ? O9 S8 N11 105.02(12) . . ? O10 S8 C5 108.10(12) . . ? O9 S8 C5 105.68(12) . . ? N11 S8 C5 108.87(12) . . ? O29 Si30 C31 111.10(14) . . ? O29 Si30 C32 110.03(13) . . ? C31 Si30 C32 108.40(15) . . ? O29 Si30 C33 106.13(11) . . ? C31 Si30 C33 110.69(14) . . ? C32 Si30 C33 110.49(13) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 73.56 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.494 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.055 _chemical_absolute_configuration ad _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -64.00 28.00 1.0000 8.0100 omega____ theta____ kappa____ phi______ frames - -41.5664 38.0000 -150.0000 92 #__ type_ start__ end____ width___ exp.time_ 2 omega -90.00 -9.00 1.0000 8.0100 omega____ theta____ kappa____ phi______ frames - -41.5664 125.0000 -150.0000 81 #__ type_ start__ end____ width___ exp.time_ 3 omega 88.00 115.00 1.0000 8.0100 omega____ theta____ kappa____ phi______ frames - 41.5664 38.0000 -90.0000 27 #__ type_ start__ end____ width___ exp.time_ 4 omega 51.00 77.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 -45.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 5 omega 92.00 149.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 162.0000 3.0000 57 #__ type_ start__ end____ width___ exp.time_ 6 omega 43.00 123.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 -128.0000 42.0000 80 #__ type_ start__ end____ width___ exp.time_ 7 omega 99.00 178.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 117.0000 53.0000 79 #__ type_ start__ end____ width___ exp.time_ 8 omega 38.00 72.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 -45.0000 -90.0000 34 #__ type_ start__ end____ width___ exp.time_ 9 omega 48.00 178.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 15.0000 60.0000 130 #__ type_ start__ end____ width___ exp.time_ 10 omega -120.00 -8.00 1.0000 8.0100 omega____ theta____ kappa____ phi______ frames - -41.5664 -77.0000 -150.0000 112 #__ type_ start__ end____ width___ exp.time_ 11 omega -117.00 -15.00 1.0000 8.0100 omega____ theta____ kappa____ phi______ frames - -41.5664 -38.0000 60.0000 102 #__ type_ start__ end____ width___ exp.time_ 12 omega 79.00 178.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 45.0000 -120.0000 99 #__ type_ start__ end____ width___ exp.time_ 13 omega 32.00 77.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 -45.0000 90.0000 45 #__ type_ start__ end____ width___ exp.time_ 14 omega 32.00 77.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 -45.0000 150.0000 45 #__ type_ start__ end____ width___ exp.time_ 15 omega 79.00 178.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 45.0000 150.0000 99 #__ type_ start__ end____ width___ exp.time_ 16 omega -120.00 -8.00 1.0000 8.0100 omega____ theta____ kappa____ phi______ frames - -41.5664 -77.0000 -30.0000 112 #__ type_ start__ end____ width___ exp.time_ 17 omega 23.00 99.00 1.0000 8.0100 omega____ theta____ kappa____ phi______ frames - 41.5664 -125.0000 60.0000 76 #__ type_ start__ end____ width___ exp.time_ 18 omega 79.00 178.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 45.0000 -60.0000 99 #__ type_ start__ end____ width___ exp.time_ 19 omega 79.00 178.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 45.0000 90.0000 99 #__ type_ start__ end____ width___ exp.time_ 20 omega 73.00 98.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 77.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 21 omega 30.00 118.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.5417 -117.0000 126.0000 88 ;