data_960GuillotICMMO _publ_requested_journal J.Org.Chem. _publ_contact_author_name ;Vincent Gandon ; _publ_contact_author_address ;Universit\'e Paris-sud 11 Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay (ICMMO) B\^atiment 420 91405 Orsay cedex - France ; _publ_contact_author_email 'vincent.gandon@u-psud.fr ' _publ_contact_author_phone '01.69.15.39.31 ' loop_ _publ_author_name _publ_author_address 'Li, Hui-Jing ' ;Universit\'e Paris-sud 11 Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay (ICMMO) B\^atiment 420 91405 Orsay cedex - France ; "Guillot, R\'egis" ;Universit\'e Paris-sud 11 Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay (ICMMO) B\^atiment 420 91405 Orsay cedex - France ; 'Gandon, Vincent' ;Universit\'e Paris-sud 11 Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay (ICMMO) B\^atiment 420 91405 Orsay cedex - France ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C25 H30 O6' _chemical_formula_sum 'C25 H30 O6' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colorless _diffrn_ambient_temperature 100(1) _chemical_formula_weight 426.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration . loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2634(4) _cell_length_b 11.5796(6) _cell_length_c 13.9766(7) _cell_angle_alpha 109.3720(10) _cell_angle_beta 94.3440(10) _cell_angle_gamma 99.4750(10) _cell_volume 1083.07(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 5781 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 31.83 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.180 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.975 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'kappa X8APEX II Bruker ICMMO' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16938 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 32.34 _reflns_number_total 6207 _reflns_number_gt 5458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+0.3382P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6207 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1094 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.88550(12) 0.68498(8) 0.22755(6) 0.01076(15) Uani 1 1 d . . . C2 C 0.81699(12) 0.57118(8) 0.12885(6) 0.01150(16) Uani 1 1 d . . . H2A H 0.8959 0.5105 0.1259 0.014 Uiso 1 1 calc R . . H2B H 0.6892 0.5325 0.1311 0.014 Uiso 1 1 calc R . . C3 C 0.82069(12) 0.60355(8) 0.03299(6) 0.01094(15) Uani 1 1 d . . . C4 C 0.92986(12) 0.71381(8) 0.03020(6) 0.01105(15) Uani 1 1 d . . . C5 C 1.06974(12) 0.76107(8) 0.21410(6) 0.01134(15) Uani 1 1 d . . . H5A H 1.1625 0.7083 0.2009 0.014 Uiso 1 1 calc R . . H5B H 1.1173 0.8302 0.2777 0.014 Uiso 1 1 calc R . . C6 C 1.04833(12) 0.81353(8) 0.12622(6) 0.01076(15) Uani 1 1 d . . . C7 C 1.24987(12) 0.85052(9) 0.10232(7) 0.01444(17) Uani 1 1 d . . . H7A H 1.2989 0.7765 0.0723 0.022 Uiso 1 1 calc R . . H7B H 1.3299 0.9032 0.1646 0.022 Uiso 1 1 calc R . . H7C H 1.2457 0.8948 0.0553 0.022 Uiso 1 1 calc R . . C8 C 0.92835(12) 0.73282(8) -0.06377(7) 0.01413(17) Uani 1 1 d . . . H8 H 0.9996 0.8059 -0.0664 0.017 Uiso 1 1 calc R . . C9 C 0.82322(13) 0.64541(9) -0.15308(7) 0.01501(17) Uani 1 1 d . . . H9 H 0.8259 0.6595 -0.2148 0.018 Uiso 1 1 calc R . . C10 C 0.71360(13) 0.53633(8) -0.14965(7) 0.01423(17) Uani 1 1 d . . . H10 H 0.6417 0.4775 -0.2088 0.017 Uiso 1 1 calc R . . C11 C 0.71296(12) 0.51660(8) -0.05747(7) 0.01249(16) Uani 1 1 d . . . H11 H 0.6394 0.4440 -0.0553 0.015 Uiso 1 1 calc R . . C12 C 0.96288(12) 0.93173(8) 0.16008(7) 0.01160(16) Uani 1 1 d . . . C13 C 1.06178(12) 1.03617(8) 0.24346(7) 0.01324(16) Uani 1 1 d . . . H13 H 1.1760 1.0317 0.2755 0.016 Uiso 1 1 calc R . . C14 C 0.99323(13) 1.14487(8) 0.27874(7) 0.01353(16) Uani 1 1 d . . . C15 C 0.82183(13) 1.15434(8) 0.23006(7) 0.01404(17) Uani 1 1 d . . . C16 C 0.72380(12) 1.05250(8) 0.14797(7) 0.01416(17) Uani 1 1 d . . . H16 H 0.6107 1.0575 0.1151 0.017 Uiso 1 1 calc R . . C17 C 0.79343(12) 0.94177(8) 0.11387(7) 0.01319(16) Uani 1 1 d . . . H17 H 0.7246 0.8739 0.0593 0.016 Uiso 1 1 calc R . . C18 C 1.25172(14) 1.24283(9) 0.41283(8) 0.01986(19) Uani 1 1 d . . . H18A H 1.2308 1.1741 0.4373 0.030 Uiso 1 1 calc R . . H18B H 1.2961 1.3194 0.4698 0.030 Uiso 1 1 calc R . . H18C H 1.3443 1.2310 0.3668 0.030 Uiso 1 1 calc R . . C19 C 0.60951(15) 1.28456(10) 0.21348(9) 0.0221(2) Uani 1 1 d . . . H19A H 0.6347 1.2746 0.1451 0.033 Uiso 1 1 calc R . . H19B H 0.5879 1.3673 0.2464 0.033 Uiso 1 1 calc R . . H19C H 0.4998 1.2242 0.2111 0.033 Uiso 1 1 calc R . . C20 C 0.73267(12) 0.76250(8) 0.25375(7) 0.01219(16) Uani 1 1 d . . . C21 C 0.66160(14) 0.94238(9) 0.37276(8) 0.01978(19) Uani 1 1 d . . . H21A H 0.5487 0.8975 0.3875 0.024 Uiso 1 1 calc R . . H21B H 0.6260 0.9729 0.3187 0.024 Uiso 1 1 calc R . . C22 C 0.75796(17) 1.05011(10) 0.46758(8) 0.0253(2) Uani 1 1 d . . . H22A H 0.7950 1.0187 0.5200 0.038 Uiso 1 1 calc R . . H22B H 0.6726 1.1051 0.4914 0.038 Uiso 1 1 calc R . . H22C H 0.8675 1.0951 0.4516 0.038 Uiso 1 1 calc R . . C23 C 0.90522(12) 0.63272(8) 0.31412(7) 0.01221(16) Uani 1 1 d . . . C24 C 1.10348(14) 0.57461(9) 0.42316(7) 0.01702(18) Uani 1 1 d . . . H24A H 1.0412 0.4872 0.3954 0.020 Uiso 1 1 calc R . . H24B H 1.0474 0.6161 0.4828 0.020 Uiso 1 1 calc R . . C25 C 1.31106(15) 0.58646(11) 0.45221(9) 0.0246(2) Uani 1 1 d . . . H25A H 1.3627 0.5388 0.3941 0.037 Uiso 1 1 calc R . . H25B H 1.3303 0.5555 0.5072 0.037 Uiso 1 1 calc R . . H25C H 1.3727 0.6727 0.4739 0.037 Uiso 1 1 calc R . . O1 O 1.07978(10) 1.24882(6) 0.36035(5) 0.01710(14) Uani 1 1 d . . . O2 O 0.76724(10) 1.26614(6) 0.26984(6) 0.01927(15) Uani 1 1 d . . . O3 O 0.79384(9) 0.86067(6) 0.34128(5) 0.01506(14) Uani 1 1 d . . . O4 O 0.57858(9) 0.73899(6) 0.20571(5) 0.01731(14) Uani 1 1 d . . . O5 O 0.76926(9) 0.59105(7) 0.34635(5) 0.01723(14) Uani 1 1 d . . . O6 O 1.08249(9) 0.63328(6) 0.34622(5) 0.01475(14) 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 0.0108(4) 0.0110(4) 0.0105(3) 0.0037(3) 0.0011(3) 0.0025(3) C2 0.0122(4) 0.0102(4) 0.0112(4) 0.0031(3) 0.0011(3) 0.0014(3) C3 0.0103(4) 0.0116(4) 0.0112(4) 0.0035(3) 0.0020(3) 0.0037(3) C4 0.0099(4) 0.0116(4) 0.0111(4) 0.0030(3) 0.0012(3) 0.0025(3) C5 0.0099(4) 0.0117(4) 0.0121(4) 0.0041(3) 0.0006(3) 0.0017(3) C6 0.0100(4) 0.0102(3) 0.0113(3) 0.0035(3) 0.0005(3) 0.0010(3) C7 0.0107(4) 0.0162(4) 0.0160(4) 0.0059(3) 0.0021(3) 0.0007(3) C8 0.0142(4) 0.0142(4) 0.0140(4) 0.0055(3) 0.0022(3) 0.0014(3) C9 0.0161(4) 0.0174(4) 0.0119(4) 0.0056(3) 0.0016(3) 0.0037(3) C10 0.0137(4) 0.0146(4) 0.0118(4) 0.0018(3) 0.0002(3) 0.0026(3) C11 0.0111(4) 0.0112(4) 0.0136(4) 0.0024(3) 0.0015(3) 0.0019(3) C12 0.0117(4) 0.0107(4) 0.0123(4) 0.0047(3) 0.0014(3) 0.0009(3) C13 0.0133(4) 0.0123(4) 0.0135(4) 0.0045(3) -0.0002(3) 0.0017(3) C14 0.0154(4) 0.0113(4) 0.0124(4) 0.0037(3) 0.0008(3) 0.0002(3) C15 0.0155(4) 0.0121(4) 0.0158(4) 0.0057(3) 0.0037(3) 0.0039(3) C16 0.0119(4) 0.0143(4) 0.0167(4) 0.0062(3) 0.0010(3) 0.0026(3) C17 0.0122(4) 0.0117(4) 0.0145(4) 0.0042(3) 0.0002(3) 0.0009(3) C18 0.0189(4) 0.0186(4) 0.0165(4) 0.0010(4) -0.0028(3) 0.0015(3) C19 0.0203(5) 0.0179(4) 0.0289(5) 0.0075(4) 0.0012(4) 0.0088(4) C20 0.0124(4) 0.0115(4) 0.0135(4) 0.0051(3) 0.0034(3) 0.0023(3) C21 0.0202(5) 0.0173(4) 0.0234(5) 0.0055(4) 0.0099(4) 0.0087(4) C22 0.0369(6) 0.0169(4) 0.0216(5) 0.0028(4) 0.0132(4) 0.0081(4) C23 0.0145(4) 0.0108(4) 0.0102(3) 0.0023(3) 0.0009(3) 0.0031(3) C24 0.0206(4) 0.0194(4) 0.0150(4) 0.0102(4) 0.0016(3) 0.0066(3) C25 0.0222(5) 0.0283(5) 0.0266(5) 0.0145(4) -0.0036(4) 0.0071(4) O1 0.0198(3) 0.0119(3) 0.0150(3) 0.0006(3) -0.0028(2) 0.0017(2) O2 0.0209(3) 0.0138(3) 0.0220(3) 0.0034(3) 0.0009(3) 0.0075(3) O3 0.0153(3) 0.0138(3) 0.0146(3) 0.0014(3) 0.0033(2) 0.0055(2) O4 0.0117(3) 0.0172(3) 0.0222(3) 0.0061(3) 0.0000(2) 0.0034(2) O5 0.0159(3) 0.0207(3) 0.0168(3) 0.0090(3) 0.0038(2) 0.0023(3) O6 0.0143(3) 0.0184(3) 0.0148(3) 0.0096(3) 0.0010(2) 0.0045(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 C1 C23 1.5293(12) . ? C1 C20 1.5309(12) . ? C1 C2 1.5367(11) . ? C1 C5 1.5370(12) . ? C2 C3 1.5071(12) . ? C3 C4 1.4018(12) . ? C3 C11 1.4038(12) . ? C4 C8 1.4014(12) . ? C4 C6 1.5313(11) . ? C5 C6 1.5488(12) . ? C6 C12 1.5418(12) . ? C6 C7 1.5494(12) . ? C8 C9 1.3888(12) . ? C9 C10 1.3951(13) . ? C10 C11 1.3814(13) . ? C12 C17 1.3863(12) . ? C12 C13 1.4103(12) . ? C13 C14 1.3811(12) . ? C14 O1 1.3699(11) . ? C14 C15 1.4110(13) . ? C15 O2 1.3665(11) . ? C15 C16 1.3843(12) . ? C16 C17 1.4042(12) . ? C18 O1 1.4234(12) . ? C19 O2 1.4261(12) . ? C20 O4 1.2009(11) . ? C20 O3 1.3472(11) . ? C21 O3 1.4485(11) . ? C21 C22 1.5092(15) . ? C23 O5 1.2106(11) . ? C23 O6 1.3293(11) . ? C24 O6 1.4612(11) . ? C24 C25 1.5030(14) . ? 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 C23 C1 C20 104.34(7) . . ? C23 C1 C2 106.03(7) . . ? C20 C1 C2 110.77(7) . . ? C23 C1 C5 114.34(7) . . ? C20 C1 C5 112.59(7) . . ? C2 C1 C5 108.55(7) . . ? C3 C2 C1 113.29(7) . . ? C4 C3 C11 119.36(8) . . ? C4 C3 C2 122.99(8) . . ? C11 C3 C2 117.63(7) . . ? C8 C4 C3 118.42(8) . . ? C8 C4 C6 119.46(8) . . ? C3 C4 C6 122.12(7) . . ? C1 C5 C6 113.94(7) . . ? C4 C6 C12 111.03(7) . . ? C4 C6 C5 110.78(7) . . ? C12 C6 C5 110.95(7) . . ? C4 C6 C7 109.12(7) . . ? C12 C6 C7 108.31(7) . . ? C5 C6 C7 106.50(7) . . ? C9 C8 C4 121.75(8) . . ? C8 C9 C10 119.56(8) . . ? C11 C10 C9 119.34(8) . . ? C10 C11 C3 121.57(8) . . ? C17 C12 C13 117.64(8) . . ? C17 C12 C6 124.00(8) . . ? C13 C12 C6 118.35(7) . . ? C14 C13 C12 121.66(8) . . ? O1 C14 C13 124.79(8) . . ? O1 C14 C15 115.14(8) . . ? C13 C14 C15 120.07(8) . . ? O2 C15 C16 125.62(8) . . ? O2 C15 C14 115.62(8) . . ? C16 C15 C14 118.76(8) . . ? C15 C16 C17 120.63(8) . . ? C12 C17 C16 121.23(8) . . ? O4 C20 O3 124.17(8) . . ? O4 C20 C1 125.80(8) . . ? O3 C20 C1 110.00(7) . . ? O3 C21 C22 107.42(8) . . ? O5 C23 O6 124.38(8) . . ? O5 C23 C1 121.90(8) . . ? O6 C23 C1 113.67(7) . . ? O6 C24 C25 107.31(8) . . ? C14 O1 C18 117.11(7) . . ? C15 O2 C19 116.65(8) . . ? C20 O3 C21 114.91(7) . . ? C23 O6 C24 114.55(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 C23 C1 C2 C3 -170.33(7) . . . . ? C20 C1 C2 C3 77.05(9) . . . . ? C5 C1 C2 C3 -47.05(9) . . . . ? C1 C2 C3 C4 19.74(11) . . . . ? C1 C2 C3 C11 -162.02(7) . . . . ? C11 C3 C4 C8 -0.45(12) . . . . ? C2 C3 C4 C8 177.75(8) . . . . ? C11 C3 C4 C6 179.07(8) . . . . ? C2 C3 C4 C6 -2.73(13) . . . . ? C23 C1 C5 C6 179.97(7) . . . . ? C20 C1 C5 C6 -61.17(9) . . . . ? C2 C1 C5 C6 61.84(9) . . . . ? C8 C4 C6 C12 70.26(10) . . . . ? C3 C4 C6 C12 -109.25(9) . . . . ? C8 C4 C6 C5 -165.99(8) . . . . ? C3 C4 C6 C5 14.50(11) . . . . ? C8 C4 C6 C7 -49.04(10) . . . . ? C3 C4 C6 C7 131.44(8) . . . . ? C1 C5 C6 C4 -44.59(9) . . . . ? C1 C5 C6 C12 79.21(9) . . . . ? C1 C5 C6 C7 -163.13(7) . . . . ? C3 C4 C8 C9 -0.41(13) . . . . ? C6 C4 C8 C9 -179.94(8) . . . . ? C4 C8 C9 C10 0.96(14) . . . . ? C8 C9 C10 C11 -0.62(13) . . . . ? C9 C10 C11 C3 -0.25(13) . . . . ? C4 C3 C11 C10 0.79(13) . . . . ? C2 C3 C11 C10 -177.51(8) . . . . ? C4 C6 C12 C17 4.60(11) . . . . ? C5 C6 C12 C17 -119.05(9) . . . . ? C7 C6 C12 C17 124.39(9) . . . . ? C4 C6 C12 C13 -175.77(7) . . . . ? C5 C6 C12 C13 60.58(10) . . . . ? C7 C6 C12 C13 -55.98(10) . . . . ? C17 C12 C13 C14 0.26(13) . . . . ? C6 C12 C13 C14 -179.39(8) . . . . ? C12 C13 C14 O1 178.70(8) . . . . ? C12 C13 C14 C15 -1.13(14) . . . . ? O1 C14 C15 O2 0.95(12) . . . . ? C13 C14 C15 O2 -179.20(8) . . . . ? O1 C14 C15 C16 -178.91(8) . . . . ? C13 C14 C15 C16 0.94(13) . . . . ? O2 C15 C16 C17 -179.74(9) . . . . ? C14 C15 C16 C17 0.10(13) . . . . ? C13 C12 C17 C16 0.80(13) . . . . ? C6 C12 C17 C16 -179.57(8) . . . . ? C15 C16 C17 C12 -0.99(14) . . . . ? C23 C1 C20 O4 -112.94(10) . . . . ? C2 C1 C20 O4 0.75(12) . . . . ? C5 C1 C20 O4 122.51(9) . . . . ? C23 C1 C20 O3 65.32(8) . . . . ? C2 C1 C20 O3 179.01(7) . . . . ? C5 C1 C20 O3 -59.23(9) . . . . ? C20 C1 C23 O5 42.82(10) . . . . ? C2 C1 C23 O5 -74.20(10) . . . . ? C5 C1 C23 O5 166.24(8) . . . . ? C20 C1 C23 O6 -139.75(7) . . . . ? C2 C1 C23 O6 103.23(8) . . . . ? C5 C1 C23 O6 -16.32(10) . . . . ? C13 C14 O1 C18 -0.79(13) . . . . ? C15 C14 O1 C18 179.05(8) . . . . ? C16 C15 O2 C19 -8.80(14) . . . . ? C14 C15 O2 C19 171.35(8) . . . . ? O4 C20 O3 C21 -2.80(13) . . . . ? C1 C20 O3 C21 178.90(7) . . . . ? C22 C21 O3 C20 -176.57(8) . . . . ? O5 C23 O6 C24 2.02(12) . . . . ? C1 C23 O6 C24 -175.34(7) . . . . ? C25 C24 O6 C23 -178.63(8) . . . . ? _diffrn_measured_fraction_theta_max 0.804 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.446 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.051