Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Andrea Vasella' 'Ai-Guo Hu' 'Chepuri Venkata Ramana' 'Axel Zimmermann' _publ_contact_author_name 'Prof Andrea Vasella' _publ_contact_author_address ; ETH-Z HCI H317 ETH-Hönggerberg CH-8093 Zürich CH 8093 SWITZERLAND ; _publ_contact_author_email VASELLA@ORG.CHEM.ETHZ.CH _publ_section_title ; Cyclopentanes from N-amino-glyconolactams. A synthesis of Mannostatin A ; data_v230501 _database_code_CSD 202048 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1R-(1,2,3,4/5)-1,5-di-O-benzoyl-4-O-tert- Butyldimethylsilyl-2,3-O- isopropylidene-cyclopentane-1,2,3,4,5-pentol ; _chemical_name_common ; 1R-(1,2,3,4/5)-1,5-di-O-benzoyl-4-O-tert-Butyldimethylsilyl- 2,3-O-isopropylidene-cyclopentane-1,2,3,4,5-pentol ; _chemical_melting_point 434.5–436 _chemical_formula_moiety ? _chemical_formula_sum 'C28 H36 O7 Si' _chemical_formula_weight 512.66 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.3780(10) _cell_length_b 19.449(5) _cell_length_c 11.752(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.00(2) _cell_angle_gamma 90.00 _cell_volume 1420.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14 _cell_measurement_theta_min 19.7 _cell_measurement_theta_max 23.5 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 1.076 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _diffrn_measurement_method \o/2\p _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 10000s _diffrn_standards_decay_% ? _diffrn_reflns_number 2283 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 68.93 _reflns_number_total 2627 _reflns_number_gt 1842 _reflns_threshold_expression >3sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction MolEN _computing_structure_solution 'SIR97 (Altomare, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep, Pluto' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ with reflections >3sigma. 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^. 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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _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 -0.10(7) _refine_ls_number_reflns 1842 _refine_ls_number_parameters 332 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1632 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.285 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.006 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 Si1 Si 0.1995(3) 0.96663(10) 0.55013(16) 0.0695(5) Uani 1 1 d . . . O6 O 0.1024(6) 0.68376(19) 0.7961(3) 0.0532(8) Uani 1 1 d . . . O7 O 0.3837(10) 0.6117(3) 0.8247(6) 0.0994(17) Uani 1 1 d . . . O8 O 0.3870(7) 0.7665(2) 0.9347(3) 0.0612(10) Uani 1 1 d . . . O9 O 0.2457(7) 0.8689(2) 0.8574(3) 0.0675(11) Uani 1 1 d . . . O10 O 0.1098(6) 0.9022(2) 0.6189(3) 0.0651(11) Uani 1 1 d . . . O11 O -0.0448(5) 0.7587(2) 0.5551(3) 0.0554(9) Uani 1 1 d . . . O12 O -0.3529(7) 0.7502(4) 0.6136(4) 0.0924(17) Uani 1 1 d . . . C1 C 0.2188(9) 0.7276(3) 0.7347(4) 0.0498(12) Uani 1 1 d . . . H1 H 0.2781 0.7002 0.6793 0.060 Uiso 1 1 calc R . . C2 C 0.4022(9) 0.7676(3) 0.8161(4) 0.0543(13) Uani 1 1 d . . . H2 H 0.5435 0.7516 0.8077 0.065 Uiso 1 1 calc R . . C3 C 0.3648(9) 0.8426(3) 0.7786(5) 0.0597(14) Uani 1 1 d . . . H3 H 0.4991 0.8677 0.7817 0.072 Uiso 1 1 calc R . . C4 C 0.2208(8) 0.8401(3) 0.6565(5) 0.0521(12) Uani 1 1 d . . . H4 H 0.3064 0.8267 0.6006 0.063 Uiso 1 1 calc R . . C5 C 0.0677(9) 0.7825(3) 0.6684(4) 0.0479(12) Uani 1 1 d . . . H5 H -0.0344 0.7977 0.7142 0.057 Uiso 1 1 calc R . . C14 C 0.2122(10) 0.6275(3) 0.8443(5) 0.0603(14) Uani 1 1 d . . . C15 C 0.1067(10) 0.5910(3) 0.9267(5) 0.0563(13) Uani 1 1 d . . . C16 C 0.2077(13) 0.5341(4) 0.9853(7) 0.082(2) Uani 1 1 d . . . H16 H 0.3360 0.5187 0.9691 0.099 Uiso 1 1 calc R . . C17 C 0.1240(19) 0.5002(4) 1.0655(8) 0.103(3) Uani 1 1 d . . . H17 H 0.1957 0.4629 1.1059 0.124 Uiso 1 1 calc R . . C18 C -0.072(2) 0.5225(5) 1.0863(8) 0.111(3) Uani 1 1 d . . . H18 H -0.1307 0.5000 1.1417 0.134 Uiso 1 1 calc R . . C19 C -0.1777(15) 0.5759(5) 1.0275(7) 0.092(2) Uani 1 1 d . . . H19 H -0.3109 0.5890 1.0403 0.111 Uiso 1 1 calc R . . C20 C -0.0880(11) 0.6121(4) 0.9470(5) 0.0682(16) Uani 1 1 d . . . H20 H -0.1590 0.6499 0.9077 0.082 Uiso 1 1 calc R . . C21 C 0.3028(10) 0.8301(3) 0.9632(5) 0.0598(13) Uani 1 1 d . . . C22 C 0.1019(12) 0.8175(5) 1.0069(7) 0.087(2) Uani 1 1 d . . . H22A H -0.0001 0.7927 0.9490 0.131 Uiso 1 1 calc R . . H22B H 0.0408 0.8608 1.0219 0.131 Uiso 1 1 calc R . . H22C H 0.1369 0.7912 1.0777 0.131 Uiso 1 1 calc R . . C23 C 0.4751(12) 0.8671(4) 1.0531(6) 0.0816(19) Uani 1 1 d . . . H23A H 0.5128 0.8398 1.1228 0.122 Uiso 1 1 calc R . . H23B H 0.4209 0.9108 1.0713 0.122 Uiso 1 1 calc R . . H23C H 0.6003 0.8740 1.0219 0.122 Uiso 1 1 calc R . . C24 C 0.1594(14) 0.9456(4) 0.3912(7) 0.090(2) Uani 1 1 d . . . C25 C 0.286(2) 0.8794(6) 0.3742(8) 0.135(4) Uani 1 1 d . . . H25A H 0.2666 0.8699 0.2924 0.203 Uiso 1 1 calc R . . H25B H 0.2336 0.8413 0.4119 0.203 Uiso 1 1 calc R . . H25C H 0.4364 0.8861 0.4080 0.203 Uiso 1 1 calc R . . C26 C -0.0776(18) 0.9326(7) 0.3365(9) 0.137(4) Uani 1 1 d . . . H26A H -0.0916 0.9142 0.2594 0.205 Uiso 1 1 calc R . . H26B H -0.1558 0.9751 0.3320 0.205 Uiso 1 1 calc R . . H26C H -0.1346 0.9004 0.3836 0.205 Uiso 1 1 calc R . . C27 C 0.2489(19) 1.0092(7) 0.3328(11) 0.149(5) Uani 1 1 d . . . H27A H 0.4019 1.0124 0.3617 0.224 Uiso 1 1 calc R . . H27B H 0.1821 1.0506 0.3517 0.224 Uiso 1 1 calc R . . H27C H 0.2171 1.0033 0.2496 0.224 Uiso 1 1 calc R . . C28 C 0.0315(18) 1.0430(4) 0.5653(10) 0.112(3) Uani 1 1 d . . . H28A H -0.1165 1.0294 0.5535 0.168 Uiso 1 1 calc R . . H28B H 0.0457 1.0769 0.5081 0.168 Uiso 1 1 calc R . . H28C H 0.0787 1.0621 0.6421 0.168 Uiso 1 1 calc R . . C29 C 0.4832(16) 0.9844(6) 0.6186(10) 0.141(5) Uani 1 1 d . . . H29A H 0.5001 0.9882 0.7016 0.212 Uiso 1 1 calc R . . H29B H 0.5261 1.0267 0.5885 0.212 Uiso 1 1 calc R . . H29C H 0.5715 0.9476 0.6015 0.212 Uiso 1 1 calc R . . C30 C -0.2540(9) 0.7443(3) 0.5394(5) 0.0581(14) Uani 1 1 d . . . C31 C -0.3521(9) 0.7214(3) 0.4189(5) 0.0549(12) Uani 1 1 d . . . C32 C -0.2421(11) 0.7276(4) 0.3295(5) 0.0655(15) Uani 1 1 d . . . H32 H -0.1033 0.7453 0.3442 0.079 Uiso 1 1 calc R . . C33 C -0.3443(14) 0.7066(4) 0.2180(6) 0.084(2) Uani 1 1 d . . . H33 H -0.2733 0.7105 0.1574 0.101 Uiso 1 1 calc R . . C34 C -0.5458(15) 0.6806(5) 0.1964(7) 0.095(3) Uani 1 1 d . . . H34 H -0.6124 0.6675 0.1208 0.114 Uiso 1 1 calc R . . C35 C -0.6543(13) 0.6730(5) 0.2850(8) 0.095(3) Uani 1 1 d . . . H35 H -0.7911 0.6536 0.2696 0.114 Uiso 1 1 calc R . . C36 C -0.5583(10) 0.6944(4) 0.3961(6) 0.0728(17) Uani 1 1 d . . . H36 H -0.6318 0.6908 0.4558 0.087 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 Si1 0.0746(11) 0.0646(10) 0.0686(10) 0.0110(9) 0.0145(8) -0.0087(9) O6 0.056(2) 0.0506(19) 0.0540(18) 0.0141(16) 0.0139(15) 0.0018(17) O7 0.084(3) 0.092(3) 0.135(5) 0.032(3) 0.051(3) 0.035(3) O8 0.082(3) 0.062(2) 0.0386(17) 0.0037(16) 0.0105(16) 0.003(2) O9 0.094(3) 0.060(2) 0.047(2) -0.0011(18) 0.013(2) 0.009(2) O10 0.060(2) 0.071(3) 0.064(2) 0.023(2) 0.0142(19) -0.003(2) O11 0.051(2) 0.080(3) 0.0374(16) -0.0030(16) 0.0141(14) -0.0028(19) O12 0.059(2) 0.162(5) 0.062(2) -0.024(3) 0.027(2) -0.017(3) C1 0.057(3) 0.052(3) 0.044(3) 0.001(2) 0.018(2) 0.005(2) C2 0.050(3) 0.072(4) 0.041(2) 0.010(2) 0.010(2) 0.004(3) C3 0.058(3) 0.065(3) 0.054(3) 0.009(3) 0.010(2) -0.009(3) C4 0.050(3) 0.059(3) 0.048(3) 0.011(2) 0.012(2) 0.000(2) C5 0.051(3) 0.056(3) 0.038(2) 0.005(2) 0.0133(19) 0.002(2) C14 0.068(4) 0.048(3) 0.064(3) 0.003(2) 0.013(3) 0.000(3) C15 0.068(3) 0.044(3) 0.052(3) 0.004(2) 0.002(2) -0.008(2) C16 0.090(5) 0.057(4) 0.091(5) 0.017(4) 0.001(4) -0.004(3) C17 0.135(8) 0.071(5) 0.088(6) 0.038(4) -0.007(5) -0.025(5) C18 0.175(10) 0.089(6) 0.075(5) 0.007(5) 0.038(6) -0.053(7) C19 0.116(6) 0.086(5) 0.088(5) 0.000(4) 0.051(5) -0.029(5) C20 0.081(4) 0.063(4) 0.061(3) 0.002(3) 0.017(3) -0.010(3) C21 0.073(4) 0.060(3) 0.045(3) -0.001(2) 0.011(2) -0.001(3) C22 0.081(5) 0.106(6) 0.080(4) 0.003(4) 0.030(4) 0.008(4) C23 0.094(5) 0.089(5) 0.059(4) -0.010(4) 0.010(3) -0.014(4) C24 0.103(6) 0.085(5) 0.088(5) 0.012(4) 0.031(4) 0.008(4) C25 0.230(12) 0.112(7) 0.087(6) 0.015(5) 0.084(7) 0.058(8) C26 0.133(9) 0.160(10) 0.093(6) 0.004(6) -0.025(6) -0.013(8) C27 0.150(9) 0.172(11) 0.141(9) 0.104(9) 0.065(8) 0.017(8) C28 0.147(8) 0.066(5) 0.138(8) -0.001(5) 0.064(7) 0.019(5) C29 0.100(6) 0.145(10) 0.153(9) 0.054(8) -0.022(6) -0.062(7) C30 0.052(3) 0.069(4) 0.054(3) 0.000(3) 0.012(2) 0.000(3) C31 0.057(3) 0.055(3) 0.050(3) -0.001(2) 0.006(2) 0.007(2) C32 0.072(4) 0.075(4) 0.049(3) -0.006(3) 0.012(3) 0.002(3) C33 0.112(6) 0.089(5) 0.048(3) -0.013(3) 0.013(3) -0.010(4) C34 0.107(6) 0.094(5) 0.066(4) -0.024(4) -0.020(4) 0.010(5) C35 0.078(5) 0.105(6) 0.090(5) -0.027(5) -0.008(4) -0.005(4) C36 0.059(4) 0.084(5) 0.073(4) -0.009(3) 0.008(3) 0.000(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 Si1 O10 1.661(4) . ? Si1 C29 1.840(9) . ? Si1 C28 1.864(8) . ? Si1 C24 1.872(9) . ? O6 C14 1.353(7) . ? O6 C1 1.428(6) . ? O7 C14 1.208(8) . ? O8 C21 1.418(8) . ? O8 C2 1.418(6) . ? O9 C3 1.419(7) . ? O9 C21 1.430(7) . ? O10 C4 1.419(7) . ? O11 C30 1.335(7) . ? O11 C5 1.439(6) . ? O12 C30 1.191(7) . ? C1 C5 1.530(7) . ? C1 C2 1.545(8) . ? C2 C3 1.526(9) . ? C3 C4 1.520(8) . ? C4 C5 1.513(8) . ? C14 C15 1.479(8) . ? C15 C20 1.378(9) . ? C15 C16 1.384(9) . ? C16 C17 1.354(12) . ? C17 C18 1.398(15) . ? C18 C19 1.341(15) . ? C19 C20 1.400(9) . ? C21 C22 1.504(9) . ? C21 C23 1.523(9) . ? C24 C26 1.525(13) . ? C24 C25 1.558(13) . ? C24 C27 1.582(12) . ? C30 C31 1.482(8) . ? C31 C36 1.385(9) . ? C31 C32 1.394(8) . ? C32 C33 1.387(9) . ? C33 C34 1.351(12) . ? C34 C35 1.381(13) . ? C35 C36 1.377(10) . ? 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 O10 Si1 C29 110.0(4) . . ? O10 Si1 C28 106.6(4) . . ? C29 Si1 C28 109.8(6) . . ? O10 Si1 C24 109.6(3) . . ? C29 Si1 C24 112.2(5) . . ? C28 Si1 C24 108.5(5) . . ? C14 O6 C1 114.5(4) . . ? C21 O8 C2 109.4(4) . . ? C3 O9 C21 107.9(4) . . ? C4 O10 Si1 126.2(4) . . ? C30 O11 C5 118.1(4) . . ? O6 C1 C5 109.6(4) . . ? O6 C1 C2 113.3(4) . . ? C5 C1 C2 105.4(4) . . ? O8 C2 C3 104.9(5) . . ? O8 C2 C1 113.0(4) . . ? C3 C2 C1 104.8(4) . . ? O9 C3 C4 109.2(5) . . ? O9 C3 C2 103.1(4) . . ? C4 C3 C2 105.3(5) . . ? O10 C4 C5 111.8(4) . . ? O10 C4 C3 114.9(5) . . ? C5 C4 C3 101.7(4) . . ? O11 C5 C4 110.6(4) . . ? O11 C5 C1 111.8(4) . . ? C4 C5 C1 102.6(4) . . ? O7 C14 O6 122.1(5) . . ? O7 C14 C15 124.6(6) . . ? O6 C14 C15 113.2(5) . . ? C20 C15 C16 119.3(6) . . ? C20 C15 C14 122.0(5) . . ? C16 C15 C14 118.7(6) . . ? C17 C16 C15 121.5(8) . . ? C16 C17 C18 118.7(8) . . ? C19 C18 C17 121.0(8) . . ? C18 C19 C20 120.2(9) . . ? C15 C20 C19 119.2(7) . . ? O8 C21 O9 106.9(4) . . ? O8 C21 C22 109.7(6) . . ? O9 C21 C22 108.2(5) . . ? O8 C21 C23 108.9(5) . . ? O9 C21 C23 110.9(5) . . ? C22 C21 C23 112.2(5) . . ? C26 C24 C25 107.6(9) . . ? C26 C24 C27 111.5(8) . . ? C25 C24 C27 110.0(7) . . ? C26 C24 Si1 110.9(7) . . ? C25 C24 Si1 110.5(6) . . ? C27 C24 Si1 106.3(7) . . ? O12 C30 O11 123.7(5) . . ? O12 C30 C31 123.3(5) . . ? O11 C30 C31 112.9(5) . . ? C36 C31 C32 120.3(5) . . ? C36 C31 C30 118.5(5) . . ? C32 C31 C30 121.2(5) . . ? C33 C32 C31 118.5(6) . . ? C34 C33 C32 120.9(7) . . ? C33 C34 C35 121.0(7) . . ? C36 C35 C34 119.4(8) . . ? C35 C36 C31 119.9(7) . . ? 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 C29 Si1 O10 C4 -43.4(7) . . . . ? C28 Si1 O10 C4 -162.4(5) . . . . ? C24 Si1 O10 C4 80.4(5) . . . . ? C14 O6 C1 C5 171.1(4) . . . . ? C14 O6 C1 C2 -71.6(6) . . . . ? C21 O8 C2 C3 11.5(6) . . . . ? C21 O8 C2 C1 -102.1(5) . . . . ? O6 C1 C2 O8 -14.5(6) . . . . ? C5 C1 C2 O8 105.2(5) . . . . ? O6 C1 C2 C3 -128.3(5) . . . . ? C5 C1 C2 C3 -8.5(5) . . . . ? C21 O9 C3 C4 139.6(5) . . . . ? C21 O9 C3 C2 28.0(6) . . . . ? O8 C2 C3 O9 -24.1(5) . . . . ? C1 C2 C3 O9 95.2(5) . . . . ? O8 C2 C3 C4 -138.5(5) . . . . ? C1 C2 C3 C4 -19.2(6) . . . . ? Si1 O10 C4 C5 -156.0(4) . . . . ? Si1 O10 C4 C3 88.9(5) . . . . ? O9 C3 C4 O10 50.5(6) . . . . ? C2 C3 C4 O10 160.7(4) . . . . ? O9 C3 C4 C5 -70.4(5) . . . . ? C2 C3 C4 C5 39.8(6) . . . . ? C30 O11 C5 C4 -139.0(5) . . . . ? C30 O11 C5 C1 107.3(5) . . . . ? O10 C4 C5 O11 73.0(5) . . . . ? C3 C4 C5 O11 -164.0(5) . . . . ? O10 C4 C5 C1 -167.6(4) . . . . ? C3 C4 C5 C1 -44.6(5) . . . . ? O6 C1 C5 O11 -86.2(5) . . . . ? C2 C1 C5 O11 151.6(4) . . . . ? O6 C1 C5 C4 155.2(4) . . . . ? C2 C1 C5 C4 33.0(5) . . . . ? C1 O6 C14 O7 -8.6(8) . . . . ? C1 O6 C14 C15 168.2(4) . . . . ? O7 C14 C15 C20 179.0(7) . . . . ? O6 C14 C15 C20 2.2(8) . . . . ? O7 C14 C15 C16 -0.8(10) . . . . ? O6 C14 C15 C16 -177.6(6) . . . . ? C20 C15 C16 C17 -2.7(11) . . . . ? C14 C15 C16 C17 177.1(7) . . . . ? C15 C16 C17 C18 2.0(13) . . . . ? C16 C17 C18 C19 0.6(14) . . . . ? C17 C18 C19 C20 -2.5(14) . . . . ? C16 C15 C20 C19 0.8(9) . . . . ? C14 C15 C20 C19 -179.0(6) . . . . ? C18 C19 C20 C15 1.7(12) . . . . ? C2 O8 C21 O9 5.5(6) . . . . ? C2 O8 C21 C22 122.6(5) . . . . ? C2 O8 C21 C23 -114.4(5) . . . . ? C3 O9 C21 O8 -21.8(6) . . . . ? C3 O9 C21 C22 -139.8(6) . . . . ? C3 O9 C21 C23 96.7(6) . . . . ? O10 Si1 C24 C26 58.7(8) . . . . ? C29 Si1 C24 C26 -178.9(8) . . . . ? C28 Si1 C24 C26 -57.4(8) . . . . ? O10 Si1 C24 C25 -60.6(7) . . . . ? C29 Si1 C24 C25 61.9(8) . . . . ? C28 Si1 C24 C25 -176.6(7) . . . . ? O10 Si1 C24 C27 -179.9(5) . . . . ? C29 Si1 C24 C27 -57.4(7) . . . . ? C28 Si1 C24 C27 64.0(7) . . . . ? C5 O11 C30 O12 0.3(9) . . . . ? C5 O11 C30 C31 179.0(5) . . . . ? O12 C30 C31 C36 -11.4(10) . . . . ? O11 C30 C31 C36 169.8(5) . . . . ? O12 C30 C31 C32 167.6(7) . . . . ? O11 C30 C31 C32 -11.2(8) . . . . ? C36 C31 C32 C33 0.4(10) . . . . ? C30 C31 C32 C33 -178.6(6) . . . . ? C31 C32 C33 C34 -0.2(11) . . . . ? C32 C33 C34 C35 -1.1(13) . . . . ? C33 C34 C35 C36 2.2(14) . . . . ? C34 C35 C36 C31 -1.9(13) . . . . ? C32 C31 C36 C35 0.7(11) . . . . ? C30 C31 C36 C35 179.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.676 _diffrn_reflns_theta_full 68.93 _diffrn_measured_fraction_theta_full 0.676 _refine_diff_density_max 0.670 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.047