Supplementary Material (ESI) for Organic & Biomolecular Chemistry This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _audit_creation_date 19-01-00 _publ_contact_author_name 'Claude Bauder' _publ_contact_author_address ; Institut de Chimie LC 03 Universite Louis Pasteur 1 rue Blaise Pascal Strasbourg 67000 FRANCE ; _publ_contact_author_email CBAUDER@CHIMIE.U-STRASBG.FR _publ_section_title ; Synthesis of derivatives of potent antitumor bistramides D and A leading to the first crystal structure of natural bistramide D ; _publ_section_references ; Blessing, R.H. (1987). Crystallogr. Rev. 1, 3-58. Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. A.L. Spek, PLATON 98, Utrecht University, The Netherland, 1998. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; loop_ _publ_author_name 'Claude Bauder' 'Jean-Francois Biard' 'Guy Solladie' data_st529 _database_code_depnum_ccdc_archive 'CCDC 255731' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H88 N2 O10 Si' _chemical_formula_sum 'C50 H88 N2 O10 Si' _chemical_formula_weight 905.31 _chemical_absolute_configuration syn loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0817 0.0704 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.371(2) _cell_length_b 9.5023(10) _cell_length_c 21.501(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.55(5) _cell_angle_gamma 90.00 _cell_volume 2854.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6903 _cell_measurement_theta_min 1.46 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 11544 _diffrn_reflns_av_R_equivalents 0.070 _diffrn_reflns_av_sigmaI/netI 0.1547 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6907 _reflns_number_gt 3551 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0800P)^2^+2.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.3(4) _refine_ls_number_reflns 6903 _refine_ls_number_parameters 568 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1821 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2129 _refine_ls_wR_factor_gt 0.1648 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.002 _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 Si Si 0.4996(2) 0.2480(3) 0.78533(11) 0.0818(8) Uani 1 1 d . . . O1 O 0.4685(4) 0.1956(5) 0.7106(2) 0.0701(15) Uani 1 1 d . . . O2 O 0.5942(3) 0.2410(4) 0.5556(2) 0.0423(10) Uani 1 1 d . . . O3 O 0.8640(3) 0.2661(4) 0.5574(2) 0.0426(10) Uani 1 1 d . . . O4 O 0.9930(2) 0.0301(4) 0.45236(17) 0.0302(8) Uani 1 1 d . . . O5 O 0.9498(6) 0.2207(6) 0.3934(3) 0.134(3) Uani 1 1 d . . . O6 O 1.2019(3) 0.2704(4) 0.4605(2) 0.0551(13) Uani 1 1 d . . . O7 O 1.1258(3) -0.0542(4) 0.18182(17) 0.0391(10) Uani 1 1 d . . . O8 O 0.9927(3) 0.0646(4) 0.12092(18) 0.0432(10) Uani 1 1 d . . . O9 O 0.6423(3) 0.1500(5) 0.0220(2) 0.0495(11) Uani 1 1 d . . . O10 O 0.7581(4) 0.2227(7) -0.0257(3) 0.0840(17) Uani 1 1 d . . . N1 N 0.8930(3) 0.0366(4) 0.5480(2) 0.0379(12) Uani 1 1 d . . . H1 H 0.8677 -0.0472 0.5385 0.045 Uiso 1 1 calc . . . N2 N 1.2014(3) 0.0460(5) 0.4269(2) 0.0361(11) Uani 1 1 d . . . H2 H 1.1853 -0.0413 0.4331 0.043 Uiso 1 1 calc . . . C1 C 0.6084(8) 0.3662(17) 0.8017(6) 0.146(5) Uani 1 1 d . . . H1A H 0.6662 0.3089 0.8056 0.219 Uiso 1 1 calc . . . H1B H 0.6121 0.4179 0.8416 0.219 Uiso 1 1 calc . . . H1C H 0.6034 0.4331 0.7663 0.219 Uiso 1 1 calc . . . C2 C 0.5193(8) 0.0970(11) 0.8408(5) 0.113(4) Uani 1 1 d . . . H2A H 0.4636 0.0345 0.8307 0.169 Uiso 1 1 calc . . . H2B H 0.5285 0.1312 0.8849 0.169 Uiso 1 1 calc . . . H2C H 0.5765 0.0453 0.8365 0.169 Uiso 1 1 calc . . . C3 C 0.3935(7) 0.3425(10) 0.7958(4) 0.086(3) Uani 1 1 d . . . C4 C 0.3042(7) 0.2523(17) 0.7773(5) 0.120(4) Uani 1 1 d . . . H4A H 0.2488 0.3060 0.7835 0.179 Uiso 1 1 calc . . . H4B H 0.3121 0.1678 0.8042 0.179 Uiso 1 1 calc . . . H4C H 0.2939 0.2246 0.7323 0.179 Uiso 1 1 calc . . . C5 C 0.3751(10) 0.4722(13) 0.7524(5) 0.136(5) Uani 1 1 d . . . H5A H 0.3818 0.4466 0.7095 0.204 Uiso 1 1 calc . . . H5B H 0.4217 0.5457 0.7701 0.204 Uiso 1 1 calc . . . H5C H 0.3102 0.5072 0.7499 0.204 Uiso 1 1 calc . . . C6 C 0.4059(10) 0.3956(14) 0.8659(5) 0.137(5) Uani 1 1 d . . . H6A H 0.4688 0.4401 0.8803 0.205 Uiso 1 1 calc . . . H6B H 0.4010 0.3158 0.8938 0.205 Uiso 1 1 calc . . . H6C H 0.3557 0.4643 0.8676 0.205 Uiso 1 1 calc . . . C7 C 0.5307(5) 0.1643(8) 0.6705(4) 0.063(2) Uani 1 1 d . . . H7 H 0.5761 0.2448 0.6725 0.076 Uiso 1 1 calc . . . C8 C 0.5876(7) 0.0353(9) 0.6923(4) 0.085(3) Uani 1 1 d . . . H8 H 0.5539 -0.0504 0.6934 0.102 Uiso 1 1 calc . . . C9 C 0.6828(10) 0.0323(11) 0.7106(6) 0.146(6) Uani 1 1 d . . . H9 H 0.7151 0.1197 0.7111 0.175 Uiso 1 1 calc . . . C10 C 0.7446(13) -0.0968(16) 0.7305(10) 0.255(12) Uani 1 1 d . . . H10A H 0.7615 -0.1039 0.7773 0.382 Uiso 1 1 calc . . . H10B H 0.8032 -0.0888 0.7148 0.382 Uiso 1 1 calc . . . H10C H 0.7092 -0.1811 0.7123 0.382 Uiso 1 1 calc . . . C11 C 0.4728(4) 0.1501(7) 0.6016(3) 0.0447(15) Uani 1 1 d . . . H11A H 0.4271 0.0714 0.5997 0.054 Uiso 1 1 calc . . . H11B H 0.4347 0.2371 0.5901 0.054 Uiso 1 1 calc . . . C12 C 0.5295(4) 0.1248(6) 0.5515(3) 0.0403(15) Uani 1 1 d . . . H12 H 0.5678 0.0367 0.5628 0.048 Uiso 1 1 calc . . . C13 C 0.4677(4) 0.1098(7) 0.4839(3) 0.0484(17) Uani 1 1 d . . . H13A H 0.4260 0.0262 0.4816 0.058 Uiso 1 1 calc . . . H13B H 0.4263 0.1938 0.4730 0.058 Uiso 1 1 calc . . . C14 C 0.5301(6) 0.0943(8) 0.4362(4) 0.070(2) Uani 1 1 d . . . H14A H 0.4897 0.0967 0.3921 0.085 Uiso 1 1 calc . . . H14B H 0.5639 0.0028 0.4427 0.085 Uiso 1 1 calc . . . C15 C 0.6047(6) 0.2170(8) 0.4457(4) 0.070(2) Uani 1 1 d . . . H15 H 0.5683 0.3068 0.4349 0.084 Uiso 1 1 calc . . . C16 C 0.6722(9) 0.2015(13) 0.3993(6) 0.146(6) Uani 1 1 d . . . H16A H 0.7147 0.2834 0.4036 0.220 Uiso 1 1 calc . . . H16B H 0.6339 0.1957 0.3552 0.220 Uiso 1 1 calc . . . H16C H 0.7106 0.1158 0.4098 0.220 Uiso 1 1 calc . . . C17 C 0.6590(4) 0.2260(6) 0.5157(4) 0.0499(17) Uani 1 1 d . . . H17 H 0.6971 0.3149 0.5200 0.060 Uiso 1 1 calc . . . C18 C 0.7303(5) 0.1072(7) 0.5415(5) 0.075(3) Uani 1 1 d . . . H18A H 0.7215 0.0783 0.5840 0.090 Uiso 1 1 calc . . . H18B H 0.7147 0.0251 0.5126 0.090 Uiso 1 1 calc . . . C19 C 0.8358(4) 0.1451(6) 0.5481(3) 0.0393(15) Uani 1 1 d . . . C20 C 0.9961(4) 0.0510(6) 0.5631(3) 0.0339(13) Uani 1 1 d . . . H20A H 1.0251 -0.0426 0.5750 0.041 Uiso 1 1 calc . . . H20B H 1.0157 0.1130 0.6010 0.041 Uiso 1 1 calc . . . C21 C 1.0363(3) 0.1108(5) 0.5090(3) 0.0288(12) Uani 1 1 d . . . H21 H 1.0189 0.2125 0.5022 0.035 Uiso 1 1 calc . . . C22 C 0.9513(5) 0.0971(7) 0.3988(3) 0.0510(17) Uani 1 1 d . . . C23 C 0.9090(5) -0.0019(7) 0.3451(3) 0.0507(17) Uani 1 1 d . . . H23A H 0.8392 0.0076 0.3342 0.076 Uiso 1 1 calc . . . H23B H 0.9264 -0.0989 0.3585 0.076 Uiso 1 1 calc . . . H23C H 0.9339 0.0209 0.3076 0.076 Uiso 1 1 calc . . . C24 C 1.1458(4) 0.0926(6) 0.5224(3) 0.0362(14) Uani 1 1 d . . . H24 H 1.1608 -0.0101 0.5280 0.043 Uiso 1 1 calc . . . C25 C 1.1957(5) 0.1689(10) 0.5840(3) 0.070(2) Uani 1 1 d . . . H25A H 1.2639 0.1448 0.5948 0.106 Uiso 1 1 calc . . . H25B H 1.1667 0.1398 0.6190 0.106 Uiso 1 1 calc . . . H25C H 1.1883 0.2708 0.5777 0.106 Uiso 1 1 calc . . . C26 C 1.1844(4) 0.1459(6) 0.4668(3) 0.0341(14) Uani 1 1 d . . . C27 C 1.2455(5) 0.0754(7) 0.3736(3) 0.0514(17) Uani 1 1 d . . . H27A H 1.3001 0.0105 0.3761 0.062 Uiso 1 1 calc . . . H27B H 1.2709 0.1726 0.3779 0.062 Uiso 1 1 calc . . . C28 C 1.1784(5) 0.0600(7) 0.3100(3) 0.0474(16) Uani 1 1 d . . . H28A H 1.2091 0.0981 0.2769 0.057 Uiso 1 1 calc . . . H28B H 1.1203 0.1166 0.3093 0.057 Uiso 1 1 calc . . . C29 C 1.1488(5) -0.0947(6) 0.2935(3) 0.0431(15) Uani 1 1 d . . . H29A H 1.2067 -0.1507 0.2929 0.052 Uiso 1 1 calc . . . H29B H 1.1199 -0.1338 0.3273 0.052 Uiso 1 1 calc . . . C30 C 1.0779(4) -0.1086(6) 0.2292(3) 0.0403(15) Uani 1 1 d . . . H30 H 1.0220 -0.0461 0.2296 0.048 Uiso 1 1 calc . . . C31 C 1.0656(5) -0.0369(7) 0.1191(3) 0.0465(16) Uani 1 1 d . . . C32 C 1.0147(5) -0.1750(7) 0.0952(3) 0.0522(18) Uani 1 1 d . . . H32A H 1.0615 -0.2406 0.0837 0.063 Uiso 1 1 calc . . . H32B H 0.9645 -0.1559 0.0559 0.063 Uiso 1 1 calc . . . C33 C 0.9686(5) -0.2460(7) 0.1446(3) 0.0529(17) Uani 1 1 d . . . H33A H 0.9121 -0.1908 0.1492 0.063 Uiso 1 1 calc . . . H33B H 0.9464 -0.3414 0.1295 0.063 Uiso 1 1 calc . . . C34 C 1.0395(4) -0.2567(6) 0.2095(3) 0.0431(15) Uani 1 1 d . . . H34 H 1.0945 -0.3160 0.2040 0.052 Uiso 1 1 calc . . . C35 C 0.9952(5) -0.3279(7) 0.2595(3) 0.059(2) Uani 1 1 d . . . H35A H 1.0387 -0.3187 0.3018 0.089 Uiso 1 1 calc . . . H35B H 0.9844 -0.4278 0.2489 0.089 Uiso 1 1 calc . . . H35C H 0.9340 -0.2827 0.2598 0.089 Uiso 1 1 calc . . . C36 C 1.0280(5) 0.2041(6) 0.1401(3) 0.0454(16) Uani 1 1 d . . . H36 H 1.0689 0.1986 0.1846 0.054 Uiso 1 1 calc . . . C37 C 1.0893(5) 0.2592(8) 0.0962(3) 0.0594(19) Uani 1 1 d . . . H37A H 1.1160 0.3522 0.1117 0.071 Uiso 1 1 calc . . . H37B H 1.0489 0.2715 0.0524 0.071 Uiso 1 1 calc . . . C38 C 1.1718(6) 0.1567(9) 0.0943(4) 0.067(2) Uani 1 1 d . . . H38A H 1.2065 0.1888 0.0622 0.080 Uiso 1 1 calc . . . H38B H 1.2175 0.1540 0.1366 0.080 Uiso 1 1 calc . . . C39 C 1.1308(6) 0.0123(8) 0.0770(3) 0.064(2) Uani 1 1 d . . . H39A H 1.1840 -0.0556 0.0806 0.076 Uiso 1 1 calc . . . H39B H 1.0941 0.0129 0.0318 0.076 Uiso 1 1 calc . . . C40 C 0.9413(5) 0.2957(6) 0.1412(3) 0.0462(16) Uani 1 1 d . . . H40A H 0.9616 0.3955 0.1438 0.055 Uiso 1 1 calc . . . H40B H 0.8935 0.2831 0.1002 0.055 Uiso 1 1 calc . . . C41 C 0.8935(4) 0.2663(7) 0.1952(3) 0.0439(15) Uani 1 1 d . . . H41A H 0.9394 0.2853 0.2364 0.053 Uiso 1 1 calc . . . H41B H 0.8759 0.1655 0.1944 0.053 Uiso 1 1 calc . . . C42 C 0.8024(5) 0.3567(7) 0.1912(3) 0.0459(16) Uani 1 1 d . . . H42 H 0.8178 0.4574 0.1844 0.055 Uiso 1 1 calc . . . C43 C 0.7690(5) 0.3448(9) 0.2534(3) 0.063(2) Uani 1 1 d . . . H43A H 0.7225 0.4194 0.2550 0.095 Uiso 1 1 calc . . . H43B H 0.8241 0.3546 0.2899 0.095 Uiso 1 1 calc . . . H43C H 0.7390 0.2528 0.2553 0.095 Uiso 1 1 calc . . . C44 C 0.7254(5) 0.3072(7) 0.1346(3) 0.0481(16) Uani 1 1 d . . . H44 H 0.6991 0.2171 0.1392 0.058 Uiso 1 1 calc . . . C45 C 0.6895(4) 0.3717(6) 0.0795(3) 0.0416(15) Uani 1 1 d . . . C46 C 0.7157(6) 0.5184(8) 0.0616(3) 0.062(2) Uani 1 1 d . . . H46A H 0.7662 0.5568 0.0962 0.094 Uiso 1 1 calc . . . H46B H 0.6592 0.5792 0.0548 0.094 Uiso 1 1 calc . . . H46C H 0.7388 0.5139 0.0222 0.094 Uiso 1 1 calc . . . C47 C 0.6159(5) 0.2970(8) 0.0278(3) 0.0579(19) Uani 1 1 d . . . H47 H 0.6122 0.3454 -0.0140 0.069 Uiso 1 1 calc . . . C48 C 0.5161(5) 0.2940(10) 0.0413(4) 0.081(3) Uani 1 1 d . . . H48A H 0.4727 0.2400 0.0078 0.122 Uiso 1 1 calc . . . H48B H 0.4922 0.3904 0.0419 0.122 Uiso 1 1 calc . . . H48C H 0.5196 0.2497 0.0830 0.122 Uiso 1 1 calc . . . C49 C 0.7190(5) 0.1307(9) -0.0044(3) 0.0559(18) Uani 1 1 d . . . C50 C 0.7476(6) -0.0230(10) -0.0004(5) 0.084(3) Uani 1 1 d . . . H50A H 0.7411 -0.0606 -0.0436 0.127 Uiso 1 1 calc . . . H50B H 0.7060 -0.0758 0.0214 0.127 Uiso 1 1 calc . . . H50C H 0.8142 -0.0319 0.0237 0.127 Uiso 1 1 calc . . . 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 Si 0.114(2) 0.0710(15) 0.0541(13) -0.0057(12) 0.0065(13) 0.0074(15) O1 0.087(4) 0.070(3) 0.057(3) -0.005(3) 0.023(3) 0.009(3) O2 0.028(2) 0.030(2) 0.069(3) -0.003(2) 0.010(2) -0.0028(17) O3 0.043(2) 0.019(2) 0.072(3) -0.0050(19) 0.027(2) 0.0017(18) O4 0.024(2) 0.0292(18) 0.034(2) -0.0053(17) 0.0000(17) 0.0001(16) O5 0.247(9) 0.034(3) 0.070(4) 0.007(3) -0.066(5) -0.002(4) O6 0.048(3) 0.023(2) 0.105(4) -0.010(2) 0.039(3) -0.002(2) O7 0.045(2) 0.042(2) 0.032(2) 0.0017(18) 0.0126(19) 0.0027(19) O8 0.054(3) 0.042(2) 0.033(2) -0.0013(18) 0.008(2) 0.008(2) O9 0.051(3) 0.050(2) 0.045(3) -0.004(2) 0.006(2) -0.001(2) O10 0.102(4) 0.088(4) 0.074(4) 0.003(3) 0.045(3) -0.014(4) N1 0.039(3) 0.018(2) 0.065(3) -0.001(2) 0.028(3) -0.001(2) N2 0.043(3) 0.024(2) 0.047(3) 0.000(2) 0.022(2) -0.009(2) C1 0.115(9) 0.187(14) 0.146(10) -0.062(10) 0.050(8) -0.058(10) C2 0.156(10) 0.088(7) 0.086(7) 0.015(6) 0.011(7) 0.027(7) C3 0.114(8) 0.071(5) 0.068(6) 0.007(5) 0.010(5) -0.010(5) C4 0.089(7) 0.187(13) 0.087(7) -0.023(9) 0.029(6) 0.003(9) C5 0.199(13) 0.107(9) 0.097(8) 0.023(7) 0.027(8) 0.079(9) C6 0.184(12) 0.143(11) 0.074(7) -0.027(7) 0.012(7) 0.049(10) C7 0.063(5) 0.048(4) 0.067(5) -0.003(4) -0.006(4) 0.009(4) C8 0.107(7) 0.053(4) 0.075(6) -0.015(5) -0.021(5) 0.019(5) C9 0.148(11) 0.070(6) 0.169(11) -0.047(7) -0.063(9) 0.045(7) C10 0.239(18) 0.127(11) 0.29(2) -0.092(13) -0.162(16) 0.118(12) C11 0.033(3) 0.047(3) 0.051(4) -0.002(3) 0.005(3) 0.005(3) C12 0.022(3) 0.029(3) 0.068(4) -0.008(3) 0.008(3) -0.002(2) C13 0.041(4) 0.048(4) 0.060(4) -0.008(3) 0.020(3) -0.011(3) C14 0.078(5) 0.067(5) 0.079(5) -0.030(4) 0.045(5) -0.031(4) C15 0.096(6) 0.052(4) 0.086(6) -0.021(4) 0.072(5) -0.024(4) C16 0.188(11) 0.130(10) 0.176(11) -0.067(9) 0.154(10) -0.086(9) C17 0.037(4) 0.022(3) 0.098(5) -0.008(3) 0.030(4) -0.004(3) C18 0.045(4) 0.033(3) 0.162(8) 0.000(4) 0.052(5) 0.004(3) C19 0.045(4) 0.020(3) 0.065(4) 0.001(3) 0.037(3) -0.002(3) C20 0.042(4) 0.024(3) 0.036(3) 0.000(2) 0.010(3) 0.005(3) C21 0.024(3) 0.025(3) 0.037(3) -0.003(2) 0.007(3) 0.004(2) C22 0.067(5) 0.037(4) 0.042(4) 0.002(3) -0.002(3) -0.012(3) C23 0.053(4) 0.059(4) 0.038(4) -0.002(3) 0.006(3) -0.013(3) C24 0.024(3) 0.037(3) 0.046(4) -0.005(3) 0.005(3) 0.007(2) C25 0.034(4) 0.111(7) 0.062(5) -0.031(5) 0.003(3) -0.004(4) C26 0.020(3) 0.023(3) 0.060(4) -0.007(3) 0.010(3) -0.003(2) C27 0.058(4) 0.046(4) 0.056(4) -0.007(3) 0.025(4) -0.020(3) C28 0.053(4) 0.041(3) 0.047(4) 0.014(3) 0.010(3) -0.013(3) C29 0.049(4) 0.046(3) 0.033(3) 0.000(3) 0.009(3) -0.010(3) C30 0.049(4) 0.041(3) 0.035(3) 0.003(3) 0.016(3) 0.005(3) C31 0.069(5) 0.051(4) 0.023(3) 0.000(3) 0.018(3) 0.010(3) C32 0.074(5) 0.044(4) 0.035(4) -0.010(3) 0.005(3) 0.013(3) C33 0.065(4) 0.043(4) 0.045(4) -0.017(3) 0.004(3) -0.004(3) C34 0.055(4) 0.033(3) 0.041(4) -0.007(3) 0.011(3) -0.001(3) C35 0.083(5) 0.043(4) 0.051(4) -0.007(3) 0.014(4) -0.031(4) C36 0.064(4) 0.036(3) 0.038(3) 0.004(3) 0.016(3) 0.004(3) C37 0.080(5) 0.059(4) 0.044(4) 0.015(4) 0.022(4) -0.004(4) C38 0.078(5) 0.072(5) 0.062(5) 0.019(4) 0.040(4) 0.010(5) C39 0.085(6) 0.066(5) 0.047(4) 0.004(4) 0.029(4) 0.015(4) C40 0.063(4) 0.038(3) 0.036(4) 0.009(3) 0.008(3) 0.011(3) C41 0.051(4) 0.043(3) 0.035(3) -0.004(3) 0.004(3) 0.006(3) C42 0.055(4) 0.046(3) 0.034(3) -0.002(3) 0.003(3) 0.003(3) C43 0.059(5) 0.082(5) 0.047(4) -0.001(4) 0.008(4) 0.011(4) C44 0.048(4) 0.042(3) 0.052(4) 0.003(3) 0.008(3) -0.005(3) C45 0.039(4) 0.040(3) 0.046(4) 0.004(3) 0.011(3) 0.006(3) C46 0.085(5) 0.054(4) 0.045(4) 0.007(3) 0.010(4) 0.003(4) C47 0.055(5) 0.061(4) 0.050(4) -0.001(4) -0.005(3) 0.002(4) C48 0.054(5) 0.082(6) 0.097(6) -0.021(5) -0.005(4) 0.008(5) C49 0.053(5) 0.072(5) 0.042(4) -0.010(4) 0.010(4) 0.003(4) C50 0.072(6) 0.078(6) 0.108(7) -0.027(5) 0.032(5) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si O1 1.642(5) . ? Si C3 1.828(11) . ? Si C2 1.845(10) . ? Si C1 1.891(12) . ? O1 C7 1.411(9) . ? O2 C17 1.414(7) . ? O2 C12 1.433(6) . ? O3 C19 1.220(6) . ? O4 C22 1.330(7) . ? O4 C21 1.451(6) . ? O5 C22 1.180(8) . ? O6 C26 1.224(7) . ? O7 C31 1.431(7) . ? O7 C30 1.451(7) . ? O8 C31 1.431(7) . ? O8 C36 1.444(7) . ? O9 C49 1.366(8) . ? O9 C47 1.460(8) . ? O10 C49 1.188(9) . ? N1 C19 1.320(7) . ? N1 C20 1.447(7) . ? N1 H1 0.8800 . ? N2 C26 1.340(7) . ? N2 C27 1.460(7) . ? N2 H2 0.8800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.518(14) . ? C3 C5 1.531(13) . ? C3 C6 1.558(13) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.487(11) . ? C7 C11 1.525(9) . ? C7 H7 1.0000 . ? C8 C9 1.332(14) . ? C8 H8 0.9500 . ? C9 C10 1.517(15) . ? C9 H9 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.515(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.521(9) . ? C12 H12 1.0000 . ? C13 C14 1.520(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.564(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C17 1.525(10) . ? C15 C16 1.553(10) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.538(9) . ? C17 H17 1.0000 . ? C18 C19 1.531(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C20 C21 1.525(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C24 1.543(7) . ? C21 H21 1.0000 . ? C22 C23 1.502(9) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.518(8) . ? C24 C25 1.533(9) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9801 . ? C27 C28 1.483(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.549(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.519(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C34 1.535(8) . ? C30 H30 1.0000 . ? C31 C39 1.521(10) . ? C31 C32 1.532(10) . ? C32 C33 1.535(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.527(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.529(9) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C40 1.525(9) . ? C36 C37 1.527(9) . ? C36 H36 1.0000 . ? C37 C38 1.542(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.505(11) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.508(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.551(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C44 1.515(9) . ? C42 C43 1.528(10) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.326(8) . ? C44 H44 0.9500 . ? C45 C46 1.517(9) . ? C45 C47 1.519(9) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.529(11) . ? C47 H47 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.513(12) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 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 O1 Si C3 103.1(4) . . ? O1 Si C2 111.3(4) . . ? C3 Si C2 108.0(5) . . ? O1 Si C1 112.7(4) . . ? C3 Si C1 111.2(5) . . ? C2 Si C1 110.3(7) . . ? C7 O1 Si 126.6(5) . . ? C17 O2 C12 113.2(4) . . ? C22 O4 C21 119.5(4) . . ? C31 O7 C30 114.9(4) . . ? C31 O8 C36 114.6(5) . . ? C49 O9 C47 114.5(6) . . ? C19 N1 C20 122.1(5) . . ? C19 N1 H1 118.9 . . ? C20 N1 H1 118.9 . . ? C26 N2 C27 123.0(5) . . ? C26 N2 H2 118.5 . . ? C27 N2 H2 118.5 . . ? Si C1 H1A 109.5 . . ? Si C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si C2 H2A 109.5 . . ? Si C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C5 106.3(10) . . ? C4 C3 C6 109.6(9) . . ? C5 C3 C6 107.0(9) . . ? C4 C3 Si 111.6(7) . . ? C5 C3 Si 110.5(7) . . ? C6 C3 Si 111.6(7) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 C8 111.2(7) . . ? O1 C7 C11 109.4(6) . . ? C8 C7 C11 111.6(6) . . ? O1 C7 H7 108.2 . . ? C8 C7 H7 108.2 . . ? C11 C7 H7 108.2 . . ? C9 C8 C7 124.1(9) . . ? C9 C8 H8 117.9 . . ? C7 C8 H8 117.9 . . ? C8 C9 C10 126.4(13) . . ? C8 C9 H9 116.8 . . ? C10 C9 H9 116.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C7 116.3(5) . . ? C12 C11 H11A 108.2 . . ? C7 C11 H11A 108.2 . . ? C12 C11 H11B 108.2 . . ? C7 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? O2 C12 C11 106.5(5) . . ? O2 C12 C13 110.9(5) . . ? C11 C12 C13 113.8(5) . . ? O2 C12 H12 108.5 . . ? C11 C12 H12 108.5 . . ? C13 C12 H12 108.5 . . ? C14 C13 C12 110.4(5) . . ? C14 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? C14 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 109.5(5) . . ? C13 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? C13 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? C17 C15 C16 112.7(8) . . ? C17 C15 C14 110.3(6) . . ? C16 C15 C14 111.0(6) . . ? C17 C15 H15 107.5 . . ? C16 C15 H15 107.5 . . ? C14 C15 H15 107.5 . . ? 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 . . ? O2 C17 C15 110.3(5) . . ? O2 C17 C18 109.5(6) . . ? C15 C17 C18 117.3(6) . . ? O2 C17 H17 106.4 . . ? C15 C17 H17 106.4 . . ? C18 C17 H17 106.4 . . ? C19 C18 C17 115.0(5) . . ? C19 C18 H18A 108.5 . . ? C17 C18 H18A 108.5 . . ? C19 C18 H18B 108.5 . . ? C17 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? O3 C19 N1 123.6(5) . . ? O3 C19 C18 121.4(5) . . ? N1 C19 C18 114.8(5) . . ? N1 C20 C21 114.5(5) . . ? N1 C20 H20A 108.6 . . ? C21 C20 H20A 108.6 . . ? N1 C20 H20B 108.6 . . ? C21 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? O4 C21 C20 106.2(4) . . ? O4 C21 C24 108.4(4) . . ? C20 C21 C24 111.6(4) . . ? O4 C21 H21 110.2 . . ? C20 C21 H21 110.2 . . ? C24 C21 H21 110.2 . . ? O5 C22 O4 123.8(6) . . ? O5 C22 C23 123.6(7) . . ? O4 C22 C23 112.6(5) . . ? 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 . . ? C26 C24 C25 109.9(5) . . ? C26 C24 C21 111.1(4) . . ? C25 C24 C21 111.0(5) . . ? C26 C24 H24 108.3 . . ? C25 C24 H24 108.3 . . ? C21 C24 H24 108.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O6 C26 N2 122.7(6) . . ? O6 C26 C24 122.2(5) . . ? N2 C26 C24 115.0(5) . . ? N2 C27 C28 113.4(5) . . ? N2 C27 H27A 108.9 . . ? C28 C27 H27A 108.9 . . ? N2 C27 H27B 108.9 . . ? C28 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C27 C28 C29 112.9(5) . . ? C27 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? C27 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C28 112.4(5) . . ? C30 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C30 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.9 . . ? O7 C30 C29 106.3(5) . . ? O7 C30 C34 109.4(5) . . ? C29 C30 C34 116.8(5) . . ? O7 C30 H30 108.0 . . ? C29 C30 H30 108.0 . . ? C34 C30 H30 108.0 . . ? O7 C31 O8 109.7(4) . . ? O7 C31 C39 106.0(6) . . ? O8 C31 C39 111.5(5) . . ? O7 C31 C32 110.7(5) . . ? O8 C31 C32 106.9(5) . . ? C39 C31 C32 112.0(5) . . ? C31 C32 C33 113.2(5) . . ? C31 C32 H32A 108.9 . . ? C33 C32 H32A 108.9 . . ? C31 C32 H32B 108.9 . . ? C33 C32 H32B 108.9 . . ? H32A C32 H32B 107.8 . . ? C34 C33 C32 111.0(5) . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C33 C34 C35 111.9(5) . . ? C33 C34 C30 108.1(5) . . ? C35 C34 C30 113.2(5) . . ? C33 C34 H34 107.8 . . ? C35 C34 H34 107.8 . . ? C30 C34 H34 107.8 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O8 C36 C40 107.2(5) . . ? O8 C36 C37 110.7(5) . . ? C40 C36 C37 113.9(5) . . ? O8 C36 H36 108.3 . . ? C40 C36 H36 108.3 . . ? C37 C36 H36 108.3 . . ? C36 C37 C38 111.0(6) . . ? C36 C37 H37A 109.4 . . ? C38 C37 H37A 109.4 . . ? C36 C37 H37B 109.4 . . ? C38 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? C39 C38 C37 108.9(6) . . ? C39 C38 H38A 109.9 . . ? C37 C38 H38A 109.9 . . ? C39 C38 H38B 109.9 . . ? C37 C38 H38B 109.9 . . ? H38A C38 H38B 108.3 . . ? C38 C39 C31 113.1(6) . . ? C38 C39 H39A 109.0 . . ? C31 C39 H39A 109.0 . . ? C38 C39 H39B 109.0 . . ? C31 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C41 C40 C36 115.3(5) . . ? C41 C40 H40A 108.4 . . ? C36 C40 H40A 108.4 . . ? C41 C40 H40B 108.4 . . ? C36 C40 H40B 108.4 . . ? H40A C40 H40B 107.5 . . ? C40 C41 C42 112.7(5) . . ? C40 C41 H41A 109.1 . . ? C42 C41 H41A 109.1 . . ? C40 C41 H41B 109.1 . . ? C42 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C44 C42 C43 111.1(6) . . ? C44 C42 C41 108.7(5) . . ? C43 C42 C41 110.1(5) . . ? C44 C42 H42 109.0 . . ? C43 C42 H42 109.0 . . ? C41 C42 H42 109.0 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C42 129.2(6) . . ? C45 C44 H44 115.4 . . ? C42 C44 H44 115.4 . . ? C44 C45 C46 125.7(6) . . ? C44 C45 C47 119.8(6) . . ? C46 C45 C47 114.6(6) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O9 C47 C45 111.0(5) . . ? O9 C47 C48 105.8(6) . . ? C45 C47 C48 113.1(6) . . ? O9 C47 H47 108.9 . . ? C45 C47 H47 108.9 . . ? C48 C47 H47 108.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O10 C49 O9 124.2(7) . . ? O10 C49 C50 125.8(7) . . ? O9 C49 C50 109.9(7) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 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 Si O1 C7 155.2(6) . . . . ? C2 Si O1 C7 -89.3(7) . . . . ? C1 Si O1 C7 35.1(8) . . . . ? O1 Si C3 C4 54.1(7) . . . . ? C2 Si C3 C4 -63.8(8) . . . . ? C1 Si C3 C4 175.1(7) . . . . ? O1 Si C3 C5 -63.9(8) . . . . ? C2 Si C3 C5 178.2(8) . . . . ? C1 Si C3 C5 57.1(9) . . . . ? O1 Si C3 C6 177.1(8) . . . . ? C2 Si C3 C6 59.2(9) . . . . ? C1 Si C3 C6 -61.9(9) . . . . ? Si O1 C7 C8 68.2(8) . . . . ? Si O1 C7 C11 -168.0(5) . . . . ? O1 C7 C8 C9 -119.2(11) . . . . ? C11 C7 C8 C9 118.4(10) . . . . ? C7 C8 C9 C10 -177.2(14) . . . . ? O1 C7 C11 C12 176.6(5) . . . . ? C8 C7 C11 C12 -60.0(9) . . . . ? C17 O2 C12 C11 174.3(5) . . . . ? C17 O2 C12 C13 -61.5(6) . . . . ? C7 C11 C12 O2 -58.3(7) . . . . ? C7 C11 C12 C13 179.3(5) . . . . ? O2 C12 C13 C14 56.3(6) . . . . ? C11 C12 C13 C14 176.3(5) . . . . ? C12 C13 C14 C15 -52.3(8) . . . . ? C13 C14 C15 C17 52.3(8) . . . . ? C13 C14 C15 C16 178.0(9) . . . . ? C12 O2 C17 C15 61.2(6) . . . . ? C12 O2 C17 C18 -69.3(6) . . . . ? C16 C15 C17 O2 179.5(7) . . . . ? C14 C15 C17 O2 -55.8(7) . . . . ? C16 C15 C17 C18 -54.3(9) . . . . ? C14 C15 C17 C18 70.3(7) . . . . ? O2 C17 C18 C19 -130.7(6) . . . . ? C15 C17 C18 C19 102.7(7) . . . . ? C20 N1 C19 O3 4.0(9) . . . . ? C20 N1 C19 C18 -170.7(6) . . . . ? C17 C18 C19 O3 27.9(11) . . . . ? C17 C18 C19 N1 -157.3(6) . . . . ? C19 N1 C20 C21 -77.8(7) . . . . ? C22 O4 C21 C20 129.2(5) . . . . ? C22 O4 C21 C24 -110.8(5) . . . . ? N1 C20 C21 O4 -49.3(5) . . . . ? N1 C20 C21 C24 -167.3(4) . . . . ? C21 O4 C22 O5 2.6(12) . . . . ? C21 O4 C22 C23 -179.2(5) . . . . ? O4 C21 C24 C26 60.6(5) . . . . ? C20 C21 C24 C26 177.2(4) . . . . ? O4 C21 C24 C25 -176.8(5) . . . . ? C20 C21 C24 C25 -60.2(6) . . . . ? C27 N2 C26 O6 2.2(9) . . . . ? C27 N2 C26 C24 -175.1(5) . . . . ? C25 C24 C26 O6 -40.0(8) . . . . ? C21 C24 C26 O6 83.2(7) . . . . ? C25 C24 C26 N2 137.3(5) . . . . ? C21 C24 C26 N2 -99.5(5) . . . . ? C26 N2 C27 C28 -110.2(6) . . . . ? N2 C27 C28 C29 -69.1(7) . . . . ? C27 C28 C29 C30 178.3(5) . . . . ? C31 O7 C30 C29 -170.3(5) . . . . ? C31 O7 C30 C34 62.7(6) . . . . ? C28 C29 C30 O7 60.8(6) . . . . ? C28 C29 C30 C34 -176.9(5) . . . . ? C30 O7 C31 O8 62.7(6) . . . . ? C30 O7 C31 C39 -176.8(5) . . . . ? C30 O7 C31 C32 -55.1(6) . . . . ? C36 O8 C31 O7 62.4(6) . . . . ? C36 O8 C31 C39 -54.8(7) . . . . ? C36 O8 C31 C32 -177.6(5) . . . . ? O7 C31 C32 C33 47.7(7) . . . . ? O8 C31 C32 C33 -71.7(6) . . . . ? C39 C31 C32 C33 165.8(6) . . . . ? C31 C32 C33 C34 -49.7(7) . . . . ? C32 C33 C34 C35 -179.7(5) . . . . ? C32 C33 C34 C30 55.0(6) . . . . ? O7 C30 C34 C33 -60.4(6) . . . . ? C29 C30 C34 C33 178.9(5) . . . . ? O7 C30 C34 C35 175.1(5) . . . . ? C29 C30 C34 C35 54.4(7) . . . . ? C31 O8 C36 C40 -178.3(4) . . . . ? C31 O8 C36 C37 56.9(6) . . . . ? O8 C36 C37 C38 -55.6(7) . . . . ? C40 C36 C37 C38 -176.5(6) . . . . ? C36 C37 C38 C39 53.5(8) . . . . ? C37 C38 C39 C31 -52.2(8) . . . . ? O7 C31 C39 C38 -66.6(7) . . . . ? O8 C31 C39 C38 52.7(8) . . . . ? C32 C31 C39 C38 172.5(6) . . . . ? O8 C36 C40 C41 71.8(6) . . . . ? C37 C36 C40 C41 -165.4(5) . . . . ? C36 C40 C41 C42 -176.5(5) . . . . ? C40 C41 C42 C44 69.5(7) . . . . ? C40 C41 C42 C43 -168.5(6) . . . . ? C43 C42 C44 C45 128.8(8) . . . . ? C41 C42 C44 C45 -109.9(7) . . . . ? C42 C44 C45 C46 -3.1(11) . . . . ? C42 C44 C45 C47 176.5(6) . . . . ? C49 O9 C47 C45 -71.3(7) . . . . ? C49 O9 C47 C48 165.6(5) . . . . ? C44 C45 C47 O9 -42.3(8) . . . . ? C46 C45 C47 O9 137.3(6) . . . . ? C44 C45 C47 C48 76.4(8) . . . . ? C46 C45 C47 C48 -104.0(7) . . . . ? C47 O9 C49 O10 -5.3(10) . . . . ? C47 O9 C49 C50 172.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.595 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.080