# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 188/206 data_cmpd.2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H34 O5' _chemical_formula_weight 498.59 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.703(2) _cell_length_b 12.290(2) _cell_length_c 21.490(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2826.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 22.3 _cell_measurement_theta_max 23.8 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 3000s _diffrn_standards_decay_% 3.54 _diffrn_reflns_number 3276 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 74.11 _reflns_number_total 2416 _reflns_number_gt 2247 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.3624P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0040(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(3) _refine_ls_number_reflns 2416 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.143 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.3742(2) 0.71206(16) 0.33921(9) 0.0565(6) Uani 1 d . . . C1 C 0.2937(3) 0.7845(2) 0.30573(14) 0.0457(7) Uani 1 d . . . H1 H 0.2097 0.7803 0.3238 0.049(8) Uiso 1 calc R . . C2 C 0.3473(3) 0.8969(2) 0.31882(14) 0.0479(7) Uani 1 d . . . H2 H 0.2858 0.9549 0.3124 0.032(6) Uiso 1 calc R . . C3 C 0.3855(3) 0.8860(3) 0.38645(15) 0.0507(7) Uani 1 d . . . H3 H 0.4531 0.9357 0.3983 0.053(9) Uiso 1 calc R . . C4 C 0.4214(3) 0.7671(3) 0.39245(14) 0.0520(8) Uani 1 d . . . H4 H 0.5124 0.7593 0.3950 0.062(9) Uiso 1 calc R . . O2 O 0.2787(2) 0.89582(17) 0.42477(10) 0.0571(6) Uani 1 d . . . O3 O 0.3651(2) 0.73134(18) 0.44719(10) 0.0628(6) Uani 1 d . . . C5 C 0.2842(3) 0.8138(3) 0.47147(15) 0.0556(8) Uani 1 d . . . C6 C 0.1557(4) 0.7678(4) 0.4794(2) 0.0814(12) Uani 1 d . . . H61 H 0.1013 0.8228 0.4960 0.090(14) Uiso 1 calc R . . H62 H 0.1587 0.7073 0.5076 0.13(2) Uiso 1 calc R . . H63 H 0.1245 0.7438 0.4399 0.16(3) Uiso 1 calc R . . C7 C 0.3399(5) 0.8593(4) 0.53056(19) 0.0841(13) Uani 1 d . . . H71 H 0.2855 0.9142 0.5471 0.094(14) Uiso 1 calc R . . H72 H 0.4200 0.8906 0.5217 0.12(2) Uiso 1 calc R . . H73 H 0.3494 0.8018 0.5605 0.105(15) Uiso 1 calc R . . O4 O 0.4567(2) 0.91167(18) 0.28207(11) 0.0580(6) Uani 1 d . . . C8 C 0.4910(4) 1.0192(3) 0.27335(18) 0.0719(11) Uani 1 d . . . H8 H 0.5716 1.0316 0.2589 0.081(12) Uiso 1 calc R . . C9 C 0.4228(4) 1.1037(3) 0.2832(2) 0.0856(13) Uani 1 d . . . C10 C 0.3552(6) 1.1907(4) 0.2915(4) 0.121(2) Uani 1 d . . . C11 C 0.3577(8) 1.2488(7) 0.3514(5) 0.207(5) Uani 1 d . . . H111 H 0.3026 1.3104 0.3495 0.31(6) Uiso 1 calc R . . H112 H 0.4412 1.2732 0.3599 0.38(8) Uiso 1 calc R . . H113 H 0.3308 1.2007 0.3840 0.35(8) Uiso 1 calc R . . C12 C 0.2741(8) 1.2358(7) 0.2390(5) 0.175(4) Uani 1 d . . . H121 H 0.2305 1.2993 0.2534 0.38(8) Uiso 1 calc R . . H122 H 0.2147 1.1816 0.2264 0.44(10) Uiso 1 calc R . . H123 H 0.3261 1.2549 0.2043 1.4(4) Uiso 1 calc R . . C13 C 0.2872(3) 0.7488(2) 0.23861(13) 0.0482(7) Uani 1 d . . . H131 H 0.3662 0.7614 0.2177 0.041(7) Uiso 1 calc R . . H132 H 0.2663 0.6722 0.2356 0.054(9) Uiso 1 calc R . . O5 O 0.19088(18) 0.81448(16) 0.21234(9) 0.0493(5) Uani 1 d . . . C14 C 0.1685(3) 0.8024(2) 0.14620(13) 0.0484(7) Uani 1 d . . . C15 C 0.1456(3) 0.6809(2) 0.13357(14) 0.0501(7) Uani 1 d . . . C16 C 0.0310(4) 0.6345(3) 0.14777(18) 0.0645(9) Uani 1 d . . . H16 H -0.0342 0.6784 0.1615 0.052(9) Uiso 1 calc R . . C17 C 0.0126(5) 0.5239(4) 0.1418(2) 0.0851(13) Uani 1 d . . . H17 H -0.0653 0.4944 0.1508 0.092(14) Uiso 1 calc R . . C18 C 0.1061(5) 0.4579(3) 0.1230(2) 0.0886(14) Uani 1 d . . . H18 H 0.0927 0.3835 0.1192 0.085(13) Uiso 1 calc R . . C19 C 0.2205(5) 0.5011(3) 0.1096(2) 0.0855(13) Uani 1 d . . . H19 H 0.2853 0.4559 0.0968 0.104(16) Uiso 1 calc R . . C20 C 0.2402(4) 0.6119(3) 0.11494(18) 0.0699(10) Uani 1 d . . . H20 H 0.3186 0.6405 0.1059 0.076(12) Uiso 1 calc R . . C21 C 0.2754(3) 0.8531(2) 0.10890(16) 0.0529(7) Uani 1 d . . . C22 C 0.2933(4) 0.8292(3) 0.04638(17) 0.0753(11) Uani 1 d . . . H22 H 0.2429 0.7777 0.0269 0.063(10) Uiso 1 calc R . . C23 C 0.3865(5) 0.8821(4) 0.0127(2) 0.0989(16) Uani 1 d . . . H23 H 0.3966 0.8668 -0.0294 0.122(18) Uiso 1 calc R . . C24 C 0.4628(5) 0.9561(4) 0.0407(3) 0.0980(16) Uani 1 d . . . H24 H 0.5271 0.9888 0.0184 0.112(16) Uiso 1 calc R . . C25 C 0.4441(4) 0.9816(4) 0.1019(3) 0.0870(13) Uani 1 d . . . H25 H 0.4948 1.0331 0.1210 0.13(2) Uiso 1 calc R . . C26 C 0.3506(3) 0.9317(3) 0.13534(18) 0.0642(9) Uani 1 d . . . H26 H 0.3378 0.9513 0.1766 0.081(13) Uiso 1 calc R . . C27 C 0.0512(3) 0.8715(3) 0.13384(16) 0.0540(8) Uani 1 d . . . C28 C -0.0103(4) 0.8656(3) 0.07786(18) 0.0694(10) Uani 1 d . . . H28 H 0.0181 0.8177 0.0475 0.082(13) Uiso 1 calc R . . C29 C -0.1142(4) 0.9298(4) 0.0660(2) 0.0881(13) Uani 1 d . . . H29 H -0.1552 0.9233 0.0280 0.085(13) Uiso 1 calc R . . C30 C -0.1566(4) 1.0013(4) 0.1084(3) 0.0935(15) Uani 1 d . . . H30 H -0.2258 1.0445 0.0999 0.091(13) Uiso 1 calc R . . C31 C -0.0965(5) 1.0092(5) 0.1639(3) 0.1078(17) Uani 1 d . . . H31 H -0.1247 1.0584 0.1936 0.14(2) Uiso 1 calc R . . C32 C 0.0070(4) 0.9443(3) 0.1767(2) 0.0865(13) Uani 1 d . . . H32 H 0.0468 0.9505 0.2150 0.115(17) Uiso 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 O1 0.0735(15) 0.0469(11) 0.0491(11) -0.0028(9) -0.0120(11) 0.0123(11) C1 0.0447(16) 0.0427(15) 0.0497(16) 0.0014(13) -0.0006(13) -0.0002(14) C2 0.0432(16) 0.0445(15) 0.0560(17) 0.0005(14) 0.0068(14) 0.0007(14) C3 0.0449(16) 0.0512(17) 0.0559(18) -0.0115(15) 0.0032(15) -0.0040(14) C4 0.0432(16) 0.0603(19) 0.0524(17) -0.0060(16) -0.0049(14) 0.0089(15) O2 0.0595(13) 0.0550(13) 0.0567(12) -0.0022(10) 0.0083(11) 0.0114(11) O3 0.0785(15) 0.0578(13) 0.0520(12) 0.0024(11) 0.0060(12) 0.0172(13) C5 0.064(2) 0.0513(17) 0.0512(17) -0.0028(15) 0.0049(16) 0.0067(17) C6 0.073(3) 0.081(3) 0.090(3) 0.002(2) 0.025(2) -0.003(2) C7 0.105(4) 0.084(3) 0.064(2) -0.018(2) -0.016(2) 0.024(3) O4 0.0503(12) 0.0566(13) 0.0672(13) -0.0029(11) 0.0134(11) -0.0049(10) C8 0.064(2) 0.067(2) 0.085(3) -0.010(2) 0.021(2) -0.027(2) C9 0.086(3) 0.053(2) 0.118(3) -0.007(2) 0.034(3) -0.024(2) C10 0.100(4) 0.060(3) 0.205(6) -0.019(4) 0.066(4) -0.034(3) C11 0.144(7) 0.127(5) 0.350(14) -0.135(8) 0.108(8) -0.051(5) C12 0.130(5) 0.107(5) 0.289(11) 0.073(6) 0.022(7) 0.020(5) C13 0.0499(16) 0.0435(16) 0.0512(16) 0.0009(13) -0.0019(14) 0.0034(15) O5 0.0503(12) 0.0518(12) 0.0460(11) -0.0036(10) -0.0040(9) 0.0089(10) C14 0.0539(18) 0.0481(16) 0.0433(16) -0.0032(13) -0.0029(14) 0.0019(14) C15 0.0581(18) 0.0473(16) 0.0448(15) -0.0018(14) -0.0068(15) 0.0006(16) C16 0.058(2) 0.060(2) 0.076(2) 0.0072(19) -0.0051(19) -0.0033(18) C17 0.081(3) 0.065(2) 0.109(3) 0.015(2) -0.014(3) -0.023(2) C18 0.108(4) 0.051(2) 0.107(3) -0.004(2) -0.024(3) -0.011(3) C19 0.103(3) 0.056(2) 0.098(3) -0.014(2) -0.007(3) 0.010(3) C20 0.073(2) 0.057(2) 0.080(2) -0.0121(19) 0.003(2) 0.0008(19) C21 0.0569(18) 0.0441(16) 0.0577(18) 0.0028(14) 0.0015(17) 0.0063(15) C22 0.095(3) 0.068(2) 0.062(2) -0.0033(19) 0.017(2) 0.001(2) C23 0.119(4) 0.095(3) 0.083(3) 0.017(3) 0.042(3) 0.021(3) C24 0.081(3) 0.089(3) 0.124(4) 0.046(3) 0.034(3) 0.004(3) C25 0.073(3) 0.066(3) 0.121(4) 0.037(3) -0.005(3) -0.011(2) C26 0.066(2) 0.0522(18) 0.075(2) 0.0149(17) -0.0045(19) -0.0055(18) C27 0.0517(17) 0.0484(17) 0.0619(19) 0.0025(15) -0.0037(16) 0.0005(15) C28 0.071(2) 0.067(2) 0.069(2) 0.005(2) -0.014(2) 0.007(2) C29 0.076(3) 0.083(3) 0.105(3) 0.029(3) -0.033(3) -0.006(3) C30 0.067(3) 0.067(3) 0.146(5) 0.029(3) -0.015(3) 0.014(2) C31 0.091(3) 0.101(4) 0.131(4) -0.016(4) -0.005(3) 0.045(3) C32 0.083(3) 0.088(3) 0.089(3) -0.015(2) -0.012(3) 0.032(2) _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 O1 C4 1.422(4) . ? O1 C1 1.433(3) . ? C1 C13 1.509(4) . ? C1 C2 1.522(4) . ? C2 O4 1.424(4) . ? C2 C3 1.516(4) . ? C3 O2 1.414(4) . ? C3 C4 1.516(4) . ? C4 O3 1.393(4) . ? O2 C5 1.423(4) . ? O3 C5 1.431(4) . ? C5 C6 1.498(5) . ? C5 C7 1.510(5) . ? O4 C8 1.384(4) . ? C8 C9 1.287(6) . ? C9 C10 1.303(7) . ? C10 C11 1.473(9) . ? C10 C12 1.528(10) . ? C13 O5 1.425(3) . ? O5 C14 1.449(3) . ? C14 C21 1.529(5) . ? C14 C15 1.538(4) . ? C14 C27 1.539(4) . ? C15 C20 1.380(5) . ? C15 C16 1.387(5) . ? C16 C17 1.379(6) . ? C17 C18 1.350(7) . ? C18 C19 1.365(7) . ? C19 C20 1.383(6) . ? C21 C26 1.379(5) . ? C21 C22 1.389(5) . ? C22 C23 1.393(6) . ? C23 C24 1.362(7) . ? C24 C25 1.366(7) . ? C25 C26 1.377(5) . ? C27 C32 1.368(5) . ? C27 C28 1.374(5) . ? C28 C29 1.387(6) . ? C29 C30 1.345(7) . ? C30 C31 1.359(7) . ? C31 C32 1.393(6) . ? 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 C4 O1 C1 108.8(2) . . ? O1 C1 C13 109.1(2) . . ? O1 C1 C2 104.1(2) . . ? C13 C1 C2 117.2(3) . . ? O4 C2 C3 108.7(2) . . ? O4 C2 C1 108.9(2) . . ? C3 C2 C1 101.5(2) . . ? O2 C3 C2 109.4(2) . . ? O2 C3 C4 103.7(3) . . ? C2 C3 C4 103.6(2) . . ? O3 C4 O1 112.1(3) . . ? O3 C4 C3 105.4(3) . . ? O1 C4 C3 107.5(2) . . ? C3 O2 C5 108.4(2) . . ? C4 O3 C5 110.2(2) . . ? O2 C5 O3 105.6(2) . . ? O2 C5 C6 108.0(3) . . ? O3 C5 C6 109.2(3) . . ? O2 C5 C7 110.4(3) . . ? O3 C5 C7 109.3(3) . . ? C6 C5 C7 113.9(4) . . ? C8 O4 C2 114.5(3) . . ? C9 C8 O4 126.7(3) . . ? C8 C9 C10 178.1(5) . . ? C9 C10 C11 120.5(8) . . ? C9 C10 C12 120.9(7) . . ? C11 C10 C12 118.6(7) . . ? O5 C13 C1 104.3(2) . . ? C13 O5 C14 116.7(2) . . ? O5 C14 C21 110.4(2) . . ? O5 C14 C15 107.4(2) . . ? C21 C14 C15 115.0(3) . . ? O5 C14 C27 104.3(2) . . ? C21 C14 C27 107.2(2) . . ? C15 C14 C27 112.0(3) . . ? C20 C15 C16 117.5(3) . . ? C20 C15 C14 122.0(3) . . ? C16 C15 C14 120.1(3) . . ? C17 C16 C15 120.7(4) . . ? C18 C17 C16 121.0(4) . . ? C17 C18 C19 119.7(4) . . ? C18 C19 C20 120.1(5) . . ? C15 C20 C19 121.1(4) . . ? C26 C21 C22 117.8(4) . . ? C26 C21 C14 120.4(3) . . ? C22 C21 C14 121.6(3) . . ? C21 C22 C23 120.1(4) . . ? C24 C23 C22 120.8(5) . . ? C23 C24 C25 119.3(5) . . ? C24 C25 C26 120.5(5) . . ? C25 C26 C21 121.4(4) . . ? C32 C27 C28 117.3(4) . . ? C32 C27 C14 121.8(3) . . ? C28 C27 C14 120.9(3) . . ? C27 C28 C29 121.0(4) . . ? C30 C29 C28 121.1(4) . . ? C29 C30 C31 118.8(4) . . ? C30 C31 C32 120.6(5) . . ? C27 C32 C31 121.1(4) . . ? 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 C4 O1 C1 C13 156.1(2) . . . . ? C4 O1 C1 C2 30.2(3) . . . . ? O1 C1 C2 O4 76.4(3) . . . . ? C13 C1 C2 O4 -44.2(3) . . . . ? O1 C1 C2 C3 -38.2(3) . . . . ? C13 C1 C2 C3 -158.8(3) . . . . ? O4 C2 C3 O2 166.9(2) . . . . ? C1 C2 C3 O2 -78.4(3) . . . . ? O4 C2 C3 C4 -82.9(3) . . . . ? C1 C2 C3 C4 31.8(3) . . . . ? C1 O1 C4 O3 105.8(3) . . . . ? C1 O1 C4 C3 -9.6(3) . . . . ? O2 C3 C4 O3 -20.3(3) . . . . ? C2 C3 C4 O3 -134.6(3) . . . . ? O2 C3 C4 O1 99.4(3) . . . . ? C2 C3 C4 O1 -14.9(3) . . . . ? C2 C3 O2 C5 136.1(3) . . . . ? C4 C3 O2 C5 26.0(3) . . . . ? O1 C4 O3 C5 -109.2(3) . . . . ? C3 C4 O3 C5 7.4(3) . . . . ? C3 O2 C5 O3 -22.0(3) . . . . ? C3 O2 C5 C6 -138.9(3) . . . . ? C3 O2 C5 C7 96.0(3) . . . . ? C4 O3 C5 O2 8.3(3) . . . . ? C4 O3 C5 C6 124.3(3) . . . . ? C4 O3 C5 C7 -110.4(3) . . . . ? C3 C2 O4 C8 -90.6(3) . . . . ? C1 C2 O4 C8 159.6(3) . . . . ? C2 O4 C8 C9 -15.5(6) . . . . ? O4 C8 C9 C10 -138(15) . . . . ? C8 C9 C10 C11 -130(15) . . . . ? C8 C9 C10 C12 48(15) . . . . ? O1 C1 C13 O5 171.1(2) . . . . ? C2 C1 C13 O5 -71.0(3) . . . . ? C1 C13 O5 C14 176.4(2) . . . . ? C13 O5 C14 C21 -71.9(3) . . . . ? C13 O5 C14 C15 54.2(3) . . . . ? C13 O5 C14 C27 173.2(2) . . . . ? O5 C14 C15 C20 -94.8(4) . . . . ? C21 C14 C15 C20 28.5(4) . . . . ? C27 C14 C15 C20 151.2(3) . . . . ? O5 C14 C15 C16 77.6(4) . . . . ? C21 C14 C15 C16 -159.1(3) . . . . ? C27 C14 C15 C16 -36.4(4) . . . . ? C20 C15 C16 C17 -1.6(6) . . . . ? C14 C15 C16 C17 -174.3(3) . . . . ? C15 C16 C17 C18 1.1(7) . . . . ? C16 C17 C18 C19 -0.1(8) . . . . ? C17 C18 C19 C20 -0.3(7) . . . . ? C16 C15 C20 C19 1.2(6) . . . . ? C14 C15 C20 C19 173.8(4) . . . . ? C18 C19 C20 C15 -0.3(7) . . . . ? O5 C14 C21 C26 -22.2(4) . . . . ? C15 C14 C21 C26 -143.9(3) . . . . ? C27 C14 C21 C26 90.8(3) . . . . ? O5 C14 C21 C22 163.4(3) . . . . ? C15 C14 C21 C22 41.7(4) . . . . ? C27 C14 C21 C22 -83.5(4) . . . . ? C26 C21 C22 C23 1.3(5) . . . . ? C14 C21 C22 C23 175.8(3) . . . . ? C21 C22 C23 C24 1.4(7) . . . . ? C22 C23 C24 C25 -2.7(7) . . . . ? C23 C24 C25 C26 1.3(7) . . . . ? C24 C25 C26 C21 1.5(6) . . . . ? C22 C21 C26 C25 -2.8(5) . . . . ? C14 C21 C26 C25 -177.3(3) . . . . ? O5 C14 C27 C32 13.6(4) . . . . ? C21 C14 C27 C32 -103.5(4) . . . . ? C15 C14 C27 C32 129.5(4) . . . . ? O5 C14 C27 C28 -169.2(3) . . . . ? C21 C14 C27 C28 73.7(4) . . . . ? C15 C14 C27 C28 -53.3(4) . . . . ? C32 C27 C28 C29 -1.0(6) . . . . ? C14 C27 C28 C29 -178.3(3) . . . . ? C27 C28 C29 C30 1.2(6) . . . . ? C28 C29 C30 C31 -0.6(7) . . . . ? C29 C30 C31 C32 -0.1(8) . . . . ? C28 C27 C32 C31 0.2(6) . . . . ? C14 C27 C32 C31 177.5(4) . . . . ? C30 C31 C32 C27 0.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.744 _diffrn_reflns_theta_full 74.11 _diffrn_measured_fraction_theta_full 0.744 _refine_diff_density_max 0.142 _refine_diff_density_min -0.117 _refine_diff_density_rms 0.027