# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Zhang-Jie Shi' 'Jia Liu' 'Xi Wang' 'Bi-Jie Li' 'Chang-Liang Sun' ; Min Wang ; _publ_contact_author_name 'Zhang-Jie Shi' _publ_contact_author_email zshi@pku.edu.cn data_compound11 _database_code_depnum_ccdc_archive 'CCDC 777559' #TrackingRef '- compound 11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H28 N O7, C7 H8' _chemical_formula_sum 'C38 H36 N O7' _chemical_formula_weight 618.68 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' N N 0.0061 0.0033 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.851(2) _cell_length_b 11.303(2) _cell_length_c 15.868(3) _cell_angle_alpha 82.36(3) _cell_angle_beta 76.88(3) _cell_angle_gamma 64.54(3) _cell_volume 1552.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 325 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 654 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9829 _exptl_absorpt_correction_T_max 0.9910 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16052 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5470 _reflns_number_gt 4872 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (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^)+(0.0653P)^2^+1.2491P] 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 5470 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1767 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_restrained_S_all 1.211 _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 O1 O 0.7776(3) 0.0187(2) 0.30999(14) 0.0377(6) Uani 1 1 d . . . O2 O 0.7860(2) 0.1372(2) 0.18573(14) 0.0338(5) Uani 1 1 d . . . O3 O 0.7449(3) 0.4501(2) -0.06325(14) 0.0410(6) Uani 1 1 d . . . O4 O 1.2339(2) 0.2047(2) -0.19563(14) 0.0390(6) Uani 1 1 d . . . O5 O 1.3678(3) -0.1068(2) 0.02271(15) 0.0468(6) Uani 1 1 d . . . O6 O 1.4272(3) -0.2678(2) 0.12380(16) 0.0450(6) Uani 1 1 d . . . O7 O 1.0789(2) -0.0984(2) 0.15675(14) 0.0351(5) Uani 1 1 d . . . N1 N 0.9792(3) 0.3391(2) -0.14920(15) 0.0276(6) Uani 1 1 d . . . C1 C 1.4321(4) -0.0071(3) 0.35091(19) 0.0299(7) Uani 1 1 d . . . H1A H 1.5339 -0.0480 0.3196 0.036 Uiso 1 1 calc R . . C2 C 1.4031(4) 0.0696(3) 0.4194(2) 0.0334(7) Uani 1 1 d . . . H2A H 1.4840 0.0823 0.4342 0.040 Uiso 1 1 calc R . . C3 C 1.2556(4) 0.1279(3) 0.4664(2) 0.0343(8) Uani 1 1 d . . . H3A H 1.2354 0.1774 0.5152 0.041 Uiso 1 1 calc R . . C4 C 1.1375(4) 0.1132(3) 0.44145(19) 0.0314(7) Uani 1 1 d . . . H4A H 1.0359 0.1560 0.4726 0.038 Uiso 1 1 calc R . . C5 C 1.1638(3) 0.0375(3) 0.37199(19) 0.0260(7) Uani 1 1 d . . . C6 C 1.0316(3) 0.0226(3) 0.34905(19) 0.0275(7) Uani 1 1 d . . . H6A H 0.9717 -0.0145 0.3894 0.033 Uiso 1 1 calc R . . C7 C 0.9977(3) 0.0707(3) 0.25621(18) 0.0246(6) Uani 1 1 d . . . C8 C 0.9914(3) 0.2111(3) 0.23066(19) 0.0270(7) Uani 1 1 d . . . H8A H 0.8858 0.2767 0.2505 0.032 Uiso 1 1 calc R . . H8B H 1.0598 0.2256 0.2612 0.032 Uiso 1 1 calc R . . C9 C 1.0380(3) 0.2333(3) 0.13453(19) 0.0265(7) Uani 1 1 d . . . C10 C 0.9224(3) 0.3247(3) 0.08078(19) 0.0282(7) Uani 1 1 d . . . H10A H 0.9364 0.4073 0.0667 0.034 Uiso 1 1 calc R . . H10B H 0.8176 0.3465 0.1147 0.034 Uiso 1 1 calc R . . C11 C 0.9407(3) 0.2618(3) -0.00339(19) 0.0284(7) Uani 1 1 d . . . H11A H 0.8882 0.2011 0.0099 0.034 Uiso 1 1 calc R . . C12 C 0.8715(4) 0.3619(3) -0.0718(2) 0.0305(7) Uani 1 1 d . . . C13 C 1.1206(3) 0.2380(3) -0.1393(2) 0.0294(7) Uani 1 1 d . . . C14 C 1.1082(3) 0.1839(3) -0.04701(19) 0.0284(7) Uani 1 1 d . . . H14A H 1.1296 0.0890 -0.0465 0.034 Uiso 1 1 calc R . . C15 C 1.2219(4) 0.1993(3) -0.0020(2) 0.0307(7) Uani 1 1 d . . . H15A H 1.3275 0.1369 -0.0254 0.037 Uiso 1 1 calc R . . H15B H 1.2165 0.2893 -0.0132 0.037 Uiso 1 1 calc R . . C16 C 1.1830(3) 0.1726(3) 0.09415(19) 0.0275(7) Uani 1 1 d . . . C17 C 1.3037(3) 0.0790(3) 0.14343(19) 0.0267(7) Uani 1 1 d . . . H17A H 1.2986 0.1221 0.1951 0.032 Uiso 1 1 calc R . . H17B H 1.4059 0.0584 0.1064 0.032 Uiso 1 1 calc R . . C18 C 1.2852(3) -0.0509(3) 0.17273(19) 0.0261(7) Uani 1 1 d . . . C20 C 1.3149(3) -0.0257(3) 0.32672(19) 0.0280(7) Uani 1 1 d . . . C21 C 1.1167(3) -0.0303(3) 0.19065(18) 0.0248(6) Uani 1 1 d . . . C22 C 0.8423(3) 0.0700(3) 0.25534(19) 0.0277(7) Uani 1 1 d . . . C23 C 0.6377(4) 0.1446(4) 0.1799(2) 0.0377(8) Uani 1 1 d . . . H23A H 0.6077 0.1931 0.1264 0.057 Uiso 1 1 calc R . . H23B H 0.5615 0.1900 0.2298 0.057 Uiso 1 1 calc R . . H23C H 0.6437 0.0559 0.1796 0.057 Uiso 1 1 calc R . . C24 C 1.3628(3) -0.1436(3) 0.0977(2) 0.0310(7) Uani 1 1 d . . . C25 C 1.5124(4) -0.3623(4) 0.0564(3) 0.0520(10) Uani 1 1 d . . . H25A H 1.5582 -0.4503 0.0831 0.078 Uiso 1 1 calc R . . H25B H 1.5934 -0.3396 0.0204 0.078 Uiso 1 1 calc R . . H25C H 1.4430 -0.3608 0.0204 0.078 Uiso 1 1 calc R . . C26 C 0.9425(3) 0.4045(3) -0.22986(19) 0.0264(7) Uani 1 1 d . . . C27 C 0.8636(4) 0.5399(3) -0.2346(2) 0.0317(7) Uani 1 1 d . . . H27A H 0.8373 0.5899 -0.1851 0.038 Uiso 1 1 calc R . . C28 C 0.8234(4) 0.6015(3) -0.3126(2) 0.0362(8) Uani 1 1 d . . . H28A H 0.7689 0.6941 -0.3165 0.043 Uiso 1 1 calc R . . C19 C 1.3559(4) -0.1160(3) 0.25473(19) 0.0297(7) Uani 1 1 d . . . H19A H 1.3229 -0.1872 0.2776 0.036 Uiso 1 1 calc R . . H19B H 1.4688 -0.1567 0.2369 0.036 Uiso 1 1 calc R . . C29 C 0.8619(4) 0.5295(3) -0.3841(2) 0.0359(8) Uani 1 1 d . . . H29A H 0.8340 0.5723 -0.4372 0.043 Uiso 1 1 calc R . . C30 C 0.9417(4) 0.3940(3) -0.3792(2) 0.0363(8) Uani 1 1 d . . . H30A H 0.9686 0.3444 -0.4289 0.044 Uiso 1 1 calc R . . C31 C 0.9820(4) 0.3312(3) -0.3018(2) 0.0309(7) Uani 1 1 d . . . H31A H 1.0363 0.2385 -0.2981 0.037 Uiso 1 1 calc R . . C32 C 1.6437(4) -0.6364(3) 0.4275(2) 0.0380(8) Uani 1 1 d . . . C33 C 1.5538(4) -0.6209(4) 0.3676(3) 0.0456(9) Uani 1 1 d . . . H33A H 1.4944 -0.6705 0.3755 0.055 Uiso 1 1 calc R . . C34 C 1.5488(4) -0.5354(4) 0.2971(3) 0.0512(10) Uani 1 1 d . . . H34A H 1.4867 -0.5270 0.2568 0.061 Uiso 1 1 calc R . . C35 C 1.6326(4) -0.4623(3) 0.2844(2) 0.0469(9) Uani 1 1 d . . . H35A H 1.6281 -0.4024 0.2360 0.056 Uiso 1 1 calc R . . C36 C 1.7236(4) -0.4766(3) 0.3428(2) 0.0458(9) Uani 1 1 d . . . H36A H 1.7830 -0.4270 0.3343 0.055 Uiso 1 1 calc R . . C37 C 1.7286(4) -0.5622(4) 0.4133(2) 0.0429(9) Uani 1 1 d . . . H37A H 1.7915 -0.5708 0.4531 0.052 Uiso 1 1 calc R . . C38 C 1.6455(5) -0.7280(4) 0.5058(3) 0.0615(12) Uani 1 1 d . . . H38A H 1.7161 -0.7270 0.5401 0.092 Uiso 1 1 calc R . . H38B H 1.6793 -0.8172 0.4871 0.092 Uiso 1 1 calc R . . H38C H 1.5422 -0.6995 0.5412 0.092 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 O1 0.0356(13) 0.0472(14) 0.0338(13) 0.0062(11) -0.0055(10) -0.0232(11) O2 0.0283(12) 0.0418(13) 0.0327(12) 0.0031(10) -0.0082(10) -0.0160(10) O3 0.0291(13) 0.0444(14) 0.0326(13) -0.0019(10) -0.0029(10) -0.0009(11) O4 0.0294(12) 0.0458(14) 0.0283(12) -0.0007(10) -0.0007(10) -0.0057(11) O5 0.0608(17) 0.0462(15) 0.0272(14) -0.0090(11) -0.0022(11) -0.0171(13) O6 0.0519(15) 0.0283(13) 0.0431(15) -0.0134(10) -0.0096(12) -0.0021(11) O7 0.0334(12) 0.0334(12) 0.0401(13) -0.0110(10) -0.0037(10) -0.0144(10) N1 0.0273(14) 0.0298(14) 0.0221(13) 0.0008(10) -0.0028(10) -0.0100(11) C1 0.0289(17) 0.0333(17) 0.0257(16) 0.0054(13) -0.0071(13) -0.0121(14) C2 0.0376(19) 0.0361(18) 0.0313(18) 0.0081(14) -0.0151(15) -0.0183(15) C3 0.048(2) 0.0304(17) 0.0260(17) 0.0015(13) -0.0142(15) -0.0152(15) C4 0.0351(18) 0.0296(17) 0.0247(16) 0.0007(13) -0.0051(13) -0.0096(14) C5 0.0283(16) 0.0231(15) 0.0233(16) 0.0037(12) -0.0058(12) -0.0085(13) C6 0.0262(16) 0.0342(17) 0.0226(15) 0.0023(13) -0.0029(12) -0.0147(14) C7 0.0217(15) 0.0258(15) 0.0245(16) -0.0025(12) -0.0008(12) -0.0095(12) C8 0.0259(16) 0.0239(15) 0.0284(16) -0.0031(12) -0.0038(13) -0.0078(13) C9 0.0330(17) 0.0247(15) 0.0225(15) -0.0021(12) -0.0047(13) -0.0125(13) C10 0.0285(16) 0.0265(16) 0.0241(16) 0.0015(12) -0.0027(13) -0.0082(13) C11 0.0280(16) 0.0271(16) 0.0280(16) -0.0013(13) -0.0021(13) -0.0109(13) C12 0.0296(18) 0.0323(17) 0.0271(17) -0.0048(13) -0.0018(13) -0.0114(15) C13 0.0262(17) 0.0282(16) 0.0293(17) -0.0039(13) -0.0005(14) -0.0087(13) C14 0.0280(16) 0.0262(16) 0.0283(16) -0.0003(12) -0.0019(13) -0.0107(13) C15 0.0282(17) 0.0342(17) 0.0281(17) 0.0022(13) -0.0032(13) -0.0135(14) C16 0.0281(17) 0.0283(16) 0.0264(16) -0.0005(12) -0.0026(13) -0.0136(14) C17 0.0277(16) 0.0288(16) 0.0242(16) -0.0013(12) -0.0037(12) -0.0126(13) C18 0.0247(16) 0.0265(16) 0.0240(15) -0.0031(12) -0.0021(12) -0.0082(13) C20 0.0311(17) 0.0256(16) 0.0253(16) 0.0047(12) -0.0073(13) -0.0107(13) C21 0.0287(16) 0.0214(15) 0.0228(15) 0.0016(12) -0.0058(12) -0.0093(13) C22 0.0294(17) 0.0256(16) 0.0251(16) -0.0017(13) -0.0028(13) -0.0094(14) C23 0.0255(17) 0.047(2) 0.040(2) -0.0019(16) -0.0099(14) -0.0127(15) C24 0.0245(16) 0.0337(18) 0.0343(19) -0.0076(14) -0.0043(13) -0.0104(14) C25 0.044(2) 0.042(2) 0.060(3) -0.0321(19) 0.0019(18) -0.0060(17) C26 0.0266(16) 0.0298(16) 0.0250(16) -0.0008(12) -0.0037(12) -0.0144(13) C27 0.0363(18) 0.0285(17) 0.0313(18) -0.0016(13) -0.0074(14) -0.0137(14) C28 0.041(2) 0.0296(17) 0.0380(19) 0.0047(14) -0.0117(15) -0.0146(15) C19 0.0288(17) 0.0292(16) 0.0252(16) -0.0003(13) -0.0053(13) -0.0067(13) C29 0.0410(19) 0.0368(19) 0.0293(18) 0.0064(14) -0.0114(15) -0.0155(16) C30 0.043(2) 0.042(2) 0.0250(17) -0.0077(14) -0.0054(14) -0.0184(16) C31 0.0319(17) 0.0278(16) 0.0320(18) -0.0010(13) -0.0057(14) -0.0115(14) C32 0.0361(19) 0.0294(17) 0.0358(19) -0.0030(14) 0.0020(15) -0.0055(15) C33 0.040(2) 0.044(2) 0.055(2) -0.0042(18) -0.0047(18) -0.0214(17) C34 0.049(2) 0.050(2) 0.051(2) -0.0008(19) -0.0169(19) -0.0143(19) C35 0.050(2) 0.0315(19) 0.041(2) 0.0036(16) -0.0008(17) -0.0053(17) C36 0.043(2) 0.037(2) 0.053(2) -0.0069(17) 0.0063(18) -0.0188(17) C37 0.037(2) 0.046(2) 0.041(2) -0.0086(17) -0.0075(16) -0.0112(17) C38 0.061(3) 0.049(2) 0.049(2) 0.0096(19) 0.007(2) -0.012(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 C22 1.195(4) . ? O2 C22 1.341(4) . ? O2 C23 1.451(4) . ? O3 C12 1.208(4) . ? O4 C13 1.209(4) . ? O5 C24 1.204(4) . ? O6 C24 1.321(4) . ? O6 C25 1.454(4) . ? O7 C21 1.212(3) . ? N1 C13 1.398(4) . ? N1 C12 1.399(4) . ? N1 C26 1.430(4) . ? C1 C2 1.382(4) . ? C1 C20 1.399(4) . ? C1 H1A 0.9500 . ? C2 C3 1.384(5) . ? C2 H2A 0.9500 . ? C3 C4 1.390(4) . ? C3 H3A 0.9500 . ? C4 C5 1.394(4) . ? C4 H4A 0.9500 . ? C5 C20 1.407(4) . ? C5 C6 1.510(4) . ? C6 C7 1.559(4) . ? C6 H6A 0.9500 . ? C7 C22 1.537(4) . ? C7 C21 1.540(4) . ? C7 C8 1.563(4) . ? C8 C9 1.510(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C16 1.334(4) . ? C9 C10 1.512(4) . ? C10 C11 1.535(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.506(4) . ? C11 C14 1.540(4) . ? C11 H11A 1.0000 . ? C13 C14 1.509(4) . ? C14 C15 1.535(4) . ? C14 H14A 1.0000 . ? C15 C16 1.509(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.505(4) . ? C17 C18 1.554(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C24 1.527(4) . ? C18 C21 1.537(4) . ? C18 C19 1.561(4) . ? C20 C19 1.502(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C31 1.384(4) . ? C26 C27 1.387(4) . ? C27 C28 1.390(4) . ? C27 H27A 0.9500 . ? C28 C29 1.370(5) . ? C28 H28A 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C29 C30 1.390(5) . ? C29 H29A 0.9500 . ? C30 C31 1.384(4) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C37 1.386(5) . ? C32 C33 1.386(5) . ? C32 C38 1.507(5) . ? C33 C34 1.373(5) . ? C33 H33A 0.9500 . ? C34 C35 1.369(6) . ? C34 H34A 0.9500 . ? C35 C36 1.378(5) . ? C35 H35A 0.9500 . ? C36 C37 1.373(5) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 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 C22 O2 C23 115.4(2) . . ? C24 O6 C25 116.5(3) . . ? C13 N1 C12 112.0(2) . . ? C13 N1 C26 124.7(2) . . ? C12 N1 C26 123.1(2) . . ? C2 C1 C20 121.4(3) . . ? C2 C1 H1A 119.3 . . ? C20 C1 H1A 119.3 . . ? C1 C2 C3 119.7(3) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C3 C4 C5 121.9(3) . . ? C3 C4 H4A 119.1 . . ? C5 C4 H4A 119.1 . . ? C4 C5 C20 118.4(3) . . ? C4 C5 C6 119.6(3) . . ? C20 C5 C6 122.0(3) . . ? C5 C6 C7 117.0(2) . . ? C5 C6 H6A 121.5 . . ? C7 C6 H6A 121.5 . . ? C22 C7 C21 106.3(2) . . ? C22 C7 C6 106.6(2) . . ? C21 C7 C6 109.3(2) . . ? C22 C7 C8 109.9(2) . . ? C21 C7 C8 111.5(2) . . ? C6 C7 C8 113.0(2) . . ? C9 C8 C7 113.4(2) . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C16 C9 C8 121.0(3) . . ? C16 C9 C10 117.7(3) . . ? C8 C9 C10 121.3(3) . . ? C9 C10 C11 111.0(2) . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 112.4(2) . . ? C12 C11 C14 104.6(2) . . ? C10 C11 C14 114.2(3) . . ? C12 C11 H11A 108.5 . . ? C10 C11 H11A 108.5 . . ? C14 C11 H11A 108.5 . . ? O3 C12 N1 123.8(3) . . ? O3 C12 C11 127.0(3) . . ? N1 C12 C11 109.1(3) . . ? O4 C13 N1 124.4(3) . . ? O4 C13 C14 126.8(3) . . ? N1 C13 C14 108.7(2) . . ? C13 C14 C15 110.9(2) . . ? C13 C14 C11 105.3(2) . . ? C15 C14 C11 112.2(3) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C11 C14 H14A 109.5 . . ? C16 C15 C14 109.3(2) . . ? C16 C15 H15A 109.8 . . ? C14 C15 H15A 109.8 . . ? C16 C15 H15B 109.8 . . ? C14 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? C9 C16 C17 120.6(3) . . ? C9 C16 C15 118.3(3) . . ? C17 C16 C15 121.1(3) . . ? C16 C17 C18 112.9(2) . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? C16 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C24 C18 C21 104.9(2) . . ? C24 C18 C17 108.2(2) . . ? C21 C18 C17 112.0(2) . . ? C24 C18 C19 110.4(2) . . ? C21 C18 C19 109.4(2) . . ? C17 C18 C19 111.7(2) . . ? C1 C20 C5 119.1(3) . . ? C1 C20 C19 118.6(3) . . ? C5 C20 C19 122.3(3) . . ? O7 C21 C18 120.0(3) . . ? O7 C21 C7 119.9(3) . . ? C18 C21 C7 120.0(2) . . ? O1 C22 O2 123.8(3) . . ? O1 C22 C7 125.0(3) . . ? O2 C22 C7 111.2(2) . . ? O2 C23 H23A 109.5 . . ? O2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O5 C24 O6 123.8(3) . . ? O5 C24 C18 123.5(3) . . ? O6 C24 C18 112.7(3) . . ? O6 C25 H25A 109.5 . . ? O6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C31 C26 C27 120.7(3) . . ? C31 C26 N1 119.3(3) . . ? C27 C26 N1 119.9(3) . . ? C26 C27 C28 119.2(3) . . ? C26 C27 H27A 120.4 . . ? C28 C27 H27A 120.4 . . ? C29 C28 C27 120.4(3) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C20 C19 C18 115.6(2) . . ? C20 C19 H19A 108.4 . . ? C18 C19 H19A 108.4 . . ? C20 C19 H19B 108.4 . . ? C18 C19 H19B 108.4 . . ? H19A C19 H19B 107.4 . . ? C28 C29 C30 120.2(3) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C31 C30 C29 120.0(3) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C26 C31 C30 119.4(3) . . ? C26 C31 H31A 120.3 . . ? C30 C31 H31A 120.3 . . ? C37 C32 C33 117.4(3) . . ? C37 C32 C38 121.6(4) . . ? C33 C32 C38 121.0(4) . . ? C34 C33 C32 121.4(4) . . ? C34 C33 H33A 119.3 . . ? C32 C33 H33A 119.3 . . ? C35 C34 C33 120.4(4) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C36 119.2(3) . . ? C34 C35 H35A 120.4 . . ? C36 C35 H35A 120.4 . . ? C37 C36 C35 120.3(3) . . ? C37 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C36 C37 C32 121.2(3) . . ? C36 C37 H37A 119.4 . . ? C32 C37 H37A 119.4 . . ? C32 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 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 C20 C1 C2 C3 1.1(5) . . . . ? C1 C2 C3 C4 -2.9(4) . . . . ? C2 C3 C4 C5 2.2(5) . . . . ? C3 C4 C5 C20 0.3(4) . . . . ? C3 C4 C5 C6 178.6(3) . . . . ? C4 C5 C6 C7 120.4(3) . . . . ? C20 C5 C6 C7 -61.4(4) . . . . ? C5 C6 C7 C22 -169.2(2) . . . . ? C5 C6 C7 C21 76.4(3) . . . . ? C5 C6 C7 C8 -48.4(3) . . . . ? C22 C7 C8 C9 -90.2(3) . . . . ? C21 C7 C8 C9 27.4(3) . . . . ? C6 C7 C8 C9 151.0(2) . . . . ? C7 C8 C9 C16 -69.7(4) . . . . ? C7 C8 C9 C10 110.4(3) . . . . ? C16 C9 C10 C11 45.9(4) . . . . ? C8 C9 C10 C11 -134.1(3) . . . . ? C9 C10 C11 C12 -159.3(3) . . . . ? C9 C10 C11 C14 -40.3(3) . . . . ? C13 N1 C12 O3 174.8(3) . . . . ? C26 N1 C12 O3 -10.4(5) . . . . ? C13 N1 C12 C11 -4.2(3) . . . . ? C26 N1 C12 C11 170.6(3) . . . . ? C10 C11 C12 O3 -49.5(4) . . . . ? C14 C11 C12 O3 -173.9(3) . . . . ? C10 C11 C12 N1 129.5(3) . . . . ? C14 C11 C12 N1 5.0(3) . . . . ? C12 N1 C13 O4 -176.0(3) . . . . ? C26 N1 C13 O4 9.3(5) . . . . ? C12 N1 C13 C14 1.5(3) . . . . ? C26 N1 C13 C14 -173.3(3) . . . . ? O4 C13 C14 C15 57.6(4) . . . . ? N1 C13 C14 C15 -119.8(3) . . . . ? O4 C13 C14 C11 179.2(3) . . . . ? N1 C13 C14 C11 1.8(3) . . . . ? C12 C11 C14 C13 -4.0(3) . . . . ? C10 C11 C14 C13 -127.3(3) . . . . ? C12 C11 C14 C15 116.7(3) . . . . ? C10 C11 C14 C15 -6.6(4) . . . . ? C13 C14 C15 C16 167.5(2) . . . . ? C11 C14 C15 C16 50.1(3) . . . . ? C8 C9 C16 C17 0.8(4) . . . . ? C10 C9 C16 C17 -179.3(3) . . . . ? C8 C9 C16 C15 -179.9(3) . . . . ? C10 C9 C16 C15 0.0(4) . . . . ? C14 C15 C16 C9 -49.3(4) . . . . ? C14 C15 C16 C17 130.0(3) . . . . ? C9 C16 C17 C18 70.5(4) . . . . ? C15 C16 C17 C18 -108.8(3) . . . . ? C16 C17 C18 C24 84.2(3) . . . . ? C16 C17 C18 C21 -31.0(3) . . . . ? C16 C17 C18 C19 -154.1(2) . . . . ? C2 C1 C20 C5 1.5(4) . . . . ? C2 C1 C20 C19 -176.8(3) . . . . ? C4 C5 C20 C1 -2.2(4) . . . . ? C6 C5 C20 C1 179.6(3) . . . . ? C4 C5 C20 C19 176.1(3) . . . . ? C6 C5 C20 C19 -2.2(4) . . . . ? C24 C18 C21 O7 10.8(4) . . . . ? C17 C18 C21 O7 128.0(3) . . . . ? C19 C18 C21 O7 -107.6(3) . . . . ? C24 C18 C21 C7 -173.2(2) . . . . ? C17 C18 C21 C7 -56.0(3) . . . . ? C19 C18 C21 C7 68.4(3) . . . . ? C22 C7 C21 O7 -6.3(4) . . . . ? C6 C7 C21 O7 108.4(3) . . . . ? C8 C7 C21 O7 -126.0(3) . . . . ? C22 C7 C21 C18 177.7(2) . . . . ? C6 C7 C21 C18 -67.6(3) . . . . ? C8 C7 C21 C18 58.0(3) . . . . ? C23 O2 C22 O1 0.0(4) . . . . ? C23 O2 C22 C7 -178.7(2) . . . . ? C21 C7 C22 O1 103.7(3) . . . . ? C6 C7 C22 O1 -12.8(4) . . . . ? C8 C7 C22 O1 -135.5(3) . . . . ? C21 C7 C22 O2 -77.6(3) . . . . ? C6 C7 C22 O2 165.9(2) . . . . ? C8 C7 C22 O2 43.2(3) . . . . ? C25 O6 C24 O5 2.2(5) . . . . ? C25 O6 C24 C18 -176.1(3) . . . . ? C21 C18 C24 O5 87.0(4) . . . . ? C17 C18 C24 O5 -32.7(4) . . . . ? C19 C18 C24 O5 -155.3(3) . . . . ? C21 C18 C24 O6 -94.7(3) . . . . ? C17 C18 C24 O6 145.6(3) . . . . ? C19 C18 C24 O6 23.0(4) . . . . ? C13 N1 C26 C31 45.6(4) . . . . ? C12 N1 C26 C31 -128.5(3) . . . . ? C13 N1 C26 C27 -136.5(3) . . . . ? C12 N1 C26 C27 49.3(4) . . . . ? C31 C26 C27 C28 0.4(5) . . . . ? N1 C26 C27 C28 -177.4(3) . . . . ? C26 C27 C28 C29 -0.3(5) . . . . ? C1 C20 C19 C18 -117.4(3) . . . . ? C5 C20 C19 C18 64.4(4) . . . . ? C24 C18 C19 C20 167.2(3) . . . . ? C21 C18 C19 C20 -77.8(3) . . . . ? C17 C18 C19 C20 46.7(3) . . . . ? C27 C28 C29 C30 0.0(5) . . . . ? C28 C29 C30 C31 0.3(5) . . . . ? C27 C26 C31 C30 -0.1(5) . . . . ? N1 C26 C31 C30 177.7(3) . . . . ? C29 C30 C31 C26 -0.2(5) . . . . ? C37 C32 C33 C34 -0.1(5) . . . . ? C38 C32 C33 C34 178.5(3) . . . . ? C32 C33 C34 C35 -0.4(6) . . . . ? C33 C34 C35 C36 0.8(6) . . . . ? C34 C35 C36 C37 -0.7(5) . . . . ? C35 C36 C37 C32 0.3(5) . . . . ? C33 C32 C37 C36 0.1(5) . . . . ? C38 C32 C37 C36 -178.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.585 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.080 # Attachment '- compound 17.cif' data_compound_17 _database_code_depnum_ccdc_archive 'CCDC 777560' #TrackingRef '- compound 17.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H34 O13' _chemical_formula_weight 614.58 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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.624(3) _cell_length_b 10.895(2) _cell_length_c 21.852(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.90(3) _cell_angle_gamma 90.00 _cell_volume 2904.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12532 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9572 _exptl_absorpt_correction_T_max 0.9677 _exptl_absorpt_process_details ; HIGASHI, T. (1995). Abscor-Empirical Absorption Correction based on Fourier Series Approximation. Rigaku Corporation,Tokyo,Japan. ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method \W _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12532 _diffrn_reflns_av_R_equivalents 0.0903 _diffrn_reflns_av_sigmaI/netI 0.2371 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6634 _reflns_number_gt 2441 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid-AUTO (Rigaku,2000)' _computing_cell_refinement Rapid-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC,2000)' _computing_structure_solution SHELXS-97,(Sheldrick,1997) _computing_structure_refinement SHELXL-97,(Sheldrick,1997) _computing_molecular_graphics 'Siemens SHELXTL V4.2,(Sheldrick,1990)' _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^)+(0.0000P)^2^+0.0000P] 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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6634 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1659 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 0.0939(3) 0.5949(3) 0.90893(14) 0.0175(9) Uani 1 1 d . . . C2 C 0.1781(3) 0.5301(3) 0.96401(14) 0.0193(9) Uani 1 1 d . . . H2A H 0.1973 0.5855 0.9999 0.023 Uiso 1 1 calc R . . H2B H 0.1437 0.4584 0.9769 0.023 Uiso 1 1 calc R . . C3 C 0.2825(3) 0.4904(3) 0.94720(14) 0.0164(9) Uani 1 1 d . . . C4 C 0.3531(3) 0.5725(3) 0.93602(15) 0.0166(9) Uani 1 1 d . . . C5 C 0.3298(3) 0.7102(3) 0.94116(15) 0.0214(10) Uani 1 1 d . . . H5A H 0.3961 0.7562 0.9425 0.026 Uiso 1 1 calc R . . H5B H 0.3098 0.7251 0.9805 0.026 Uiso 1 1 calc R . . C6 C 0.2372(3) 0.7575(3) 0.88560(14) 0.0153(9) Uani 1 1 d . . . C7 C 0.1748(3) 0.8725(3) 0.90321(14) 0.0193(9) Uani 1 1 d . . . H7A H 0.2193 0.9448 0.9024 0.023 Uiso 1 1 calc R . . H7B H 0.1071 0.8827 0.8705 0.023 Uiso 1 1 calc R . . C8 C 0.1470(3) 0.8682(3) 0.96706(15) 0.0181(9) Uani 1 1 d . . . C9 C 0.0830(3) 0.7836(3) 0.98226(15) 0.0188(9) Uani 1 1 d . . . C10 C 0.0229(3) 0.6891(3) 0.93518(15) 0.0212(9) Uani 1 1 d . . . H10A H -0.0234 0.7326 0.8994 0.025 Uiso 1 1 calc R . . H10B H -0.0251 0.6432 0.9550 0.025 Uiso 1 1 calc R . . C11 C 0.1515(3) 0.6560(3) 0.86151(16) 0.0158(9) Uani 1 1 d . . . C12 C 0.4576(3) 0.5370(3) 0.91825(15) 0.0193(9) Uani 1 1 d . . . H12A H 0.4607 0.5815 0.8803 0.023 Uiso 1 1 calc R . . H12B H 0.5198 0.5628 0.9519 0.023 Uiso 1 1 calc R . . C13 C 0.4685(3) 0.4026(3) 0.90675(15) 0.0198(9) Uani 1 1 d . . . C14 C 0.3984(3) 0.3201(3) 0.92034(15) 0.0200(9) Uani 1 1 d . . . C15 C 0.3009(3) 0.3535(3) 0.94414(15) 0.0211(9) Uani 1 1 d . . . H15A H 0.3104 0.3191 0.9861 0.025 Uiso 1 1 calc R . . H15B H 0.2361 0.3165 0.9167 0.025 Uiso 1 1 calc R . . C16 C 0.0643(3) 0.7768(4) 1.04638(15) 0.0260(10) Uani 1 1 d . . . H16A H 0.0985 0.7026 1.0668 0.031 Uiso 1 1 calc R . . H16B H -0.0139 0.7699 1.0421 0.031 Uiso 1 1 calc R . . C17 C 0.1073(3) 0.8840(3) 1.08871(14) 0.0179(9) Uani 1 1 d . . . C18 C 0.1635(3) 0.9750(3) 1.07176(15) 0.0202(9) Uani 1 1 d . . . C19 C 0.1941(3) 0.9733(3) 1.01055(15) 0.0268(10) Uani 1 1 d . . . H19A H 0.2734 0.9701 1.0193 0.032 Uiso 1 1 calc R . . H19B H 0.1703 1.0497 0.9885 0.032 Uiso 1 1 calc R . . C20 C 0.0191(3) 0.5002(4) 0.86781(16) 0.0218(10) Uani 1 1 d . . . C21 C 0.2836(3) 0.7915(3) 0.82989(16) 0.0203(9) Uani 1 1 d . . . C22 C 0.4049(4) 0.1846(4) 0.9054(2) 0.0330(11) Uani 1 1 d . . . C23 C 0.5582(3) 0.3726(4) 0.87566(17) 0.0230(9) Uani 1 1 d . . . C24 C 0.0848(3) 0.8748(3) 1.15159(17) 0.0197(9) Uani 1 1 d . . . C25 C 0.1951(3) 1.0838(3) 1.11382(16) 0.0218(9) Uani 1 1 d . . . C26 C -0.1444(3) 0.4679(4) 0.78930(16) 0.0429(12) Uani 1 1 d . . . H26A H -0.1726 0.4041 0.8109 0.064 Uiso 1 1 calc R . . H26B H -0.1025 0.4321 0.7629 0.064 Uiso 1 1 calc R . . H26C H -0.2041 0.5142 0.7636 0.064 Uiso 1 1 calc R . . C27 C 0.2547(3) 0.9002(3) 0.73422(13) 0.0327(11) Uani 1 1 d . . . H27A H 0.2497 0.8300 0.7071 0.049 Uiso 1 1 calc R . . H27B H 0.3294 0.9276 0.7471 0.049 Uiso 1 1 calc R . . H27C H 0.2094 0.9650 0.7117 0.049 Uiso 1 1 calc R . . C28 C 0.5145(4) 0.0236(5) 0.8827(3) 0.111(3) Uani 1 1 d . . . H28A H 0.4651 0.0184 0.8413 0.167 Uiso 1 1 calc R . . H28B H 0.4955 -0.0377 0.9096 0.167 Uiso 1 1 calc R . . H28C H 0.5882 0.0100 0.8797 0.167 Uiso 1 1 calc R . . C29 C 0.5960(4) 0.2912(5) 0.78395(17) 0.0663(18) Uani 1 1 d . . . H29A H 0.6480 0.2345 0.8086 0.099 Uiso 1 1 calc R . . H29B H 0.6337 0.3633 0.7755 0.099 Uiso 1 1 calc R . . H29C H 0.5586 0.2534 0.7447 0.099 Uiso 1 1 calc R . . C30 C 0.2978(3) 1.2670(4) 1.13451(16) 0.0445(13) Uani 1 1 d . . . H30A H 0.3182 1.2426 1.1782 0.067 Uiso 1 1 calc R . . H30B H 0.2386 1.3249 1.1278 0.067 Uiso 1 1 calc R . . H30C H 0.3595 1.3043 1.1237 0.067 Uiso 1 1 calc R . . C31 C -0.0538(3) 0.8780(4) 1.20703(14) 0.0297(10) Uani 1 1 d . . . H31A H -0.0071 0.9250 1.2405 0.045 Uiso 1 1 calc R . . H31B H -0.0469 0.7924 1.2177 0.045 Uiso 1 1 calc R . . H31C H -0.1285 0.9033 1.2016 0.045 Uiso 1 1 calc R . . O1 O 0.1272(2) 0.6267(2) 0.80687(10) 0.0224(6) Uani 1 1 d . . . O2 O 0.0453(2) 0.3927(2) 0.86430(11) 0.0279(7) Uani 1 1 d . . . O3 O -0.0745(2) 0.5487(2) 0.83542(10) 0.0249(7) Uani 1 1 d . . . O4 O 0.2178(2) 0.8670(2) 0.78986(10) 0.0243(7) Uani 1 1 d . . . O5 O 0.3693(2) 0.7523(3) 0.82276(11) 0.0348(8) Uani 1 1 d . . . O6 O 0.3260(3) 0.1209(3) 0.88952(16) 0.0696(11) Uani 1 1 d . . . O7 O 0.5065(2) 0.1459(3) 0.90942(14) 0.0575(10) Uani 1 1 d . . . O8 O 0.6521(2) 0.3977(3) 0.89652(11) 0.0415(8) Uani 1 1 d . . . O9 O 0.5167(2) 0.3254(3) 0.81893(12) 0.0485(9) Uani 1 1 d . . . O10 O 0.1628(2) 1.1020(2) 1.16003(10) 0.0283(7) Uani 1 1 d . . . O11 O 0.2628(2) 1.1590(2) 1.09452(11) 0.0308(7) Uani 1 1 d . . . O12 O -0.0218(2) 0.8985(2) 1.14821(10) 0.0247(7) Uani 1 1 d . . . O13 O 0.1507(2) 0.8419(2) 1.19927(11) 0.0264(7) 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 0.023(2) 0.011(2) 0.0170(19) -0.0031(17) 0.0026(17) -0.0023(18) C2 0.021(2) 0.016(2) 0.019(2) 0.0075(17) 0.0013(17) -0.0002(18) C3 0.017(2) 0.015(2) 0.0153(19) 0.0005(17) 0.0013(17) 0.0030(17) C4 0.022(2) 0.010(2) 0.0162(19) 0.0006(17) 0.0017(17) 0.0011(18) C5 0.025(2) 0.021(2) 0.022(2) -0.0064(18) 0.0126(18) -0.0073(19) C6 0.021(2) 0.013(2) 0.0128(18) 0.0039(17) 0.0068(17) 0.0002(18) C7 0.027(2) 0.009(2) 0.025(2) 0.0013(17) 0.0107(18) -0.0002(18) C8 0.024(2) 0.012(2) 0.0179(19) -0.0041(17) 0.0048(17) 0.0067(18) C9 0.023(2) 0.013(2) 0.022(2) -0.0028(17) 0.0079(18) -0.0003(18) C10 0.020(2) 0.017(2) 0.028(2) -0.0019(18) 0.0089(18) -0.0025(18) C11 0.016(2) 0.011(2) 0.021(2) 0.0067(17) 0.0059(17) 0.0100(17) C12 0.019(2) 0.019(2) 0.020(2) 0.0015(18) 0.0052(17) -0.0033(19) C13 0.016(2) 0.018(2) 0.024(2) -0.0044(19) 0.0031(18) 0.0024(18) C14 0.018(2) 0.013(2) 0.024(2) 0.0006(18) -0.0018(18) 0.0016(18) C15 0.024(2) 0.018(2) 0.021(2) 0.0038(17) 0.0061(18) 0.0001(19) C16 0.026(3) 0.023(3) 0.033(2) -0.005(2) 0.0141(19) -0.007(2) C17 0.025(2) 0.014(2) 0.0174(19) -0.0025(17) 0.0105(18) 0.0014(18) C18 0.028(3) 0.022(2) 0.0120(19) -0.0047(18) 0.0083(18) -0.001(2) C19 0.034(3) 0.021(2) 0.028(2) -0.003(2) 0.012(2) -0.003(2) C20 0.024(2) 0.023(3) 0.019(2) -0.0012(19) 0.0080(18) -0.005(2) C21 0.027(3) 0.016(2) 0.019(2) -0.0048(18) 0.0080(19) -0.010(2) C22 0.030(3) 0.018(3) 0.053(3) -0.001(2) 0.014(2) 0.008(2) C23 0.023(2) 0.020(2) 0.024(2) -0.0040(19) 0.0031(19) -0.001(2) C24 0.024(2) 0.006(2) 0.030(2) -0.0026(19) 0.0068(19) -0.0029(19) C25 0.025(2) 0.018(2) 0.024(2) -0.0038(19) 0.0115(19) 0.0043(19) C26 0.030(3) 0.035(3) 0.049(3) -0.009(2) -0.016(2) -0.005(2) C27 0.041(3) 0.039(3) 0.018(2) 0.015(2) 0.0073(19) -0.003(2) C28 0.060(5) 0.054(4) 0.193(6) -0.079(4) -0.015(4) 0.022(3) C29 0.033(3) 0.116(5) 0.054(3) -0.054(3) 0.019(2) -0.003(3) C30 0.045(3) 0.042(3) 0.055(3) -0.030(2) 0.027(3) -0.029(3) C31 0.033(3) 0.027(3) 0.036(2) 0.005(2) 0.022(2) 0.004(2) O1 0.0320(17) 0.0161(16) 0.0209(13) -0.0014(13) 0.0101(12) -0.0057(13) O2 0.0243(17) 0.0116(17) 0.0432(16) -0.0031(14) 0.0005(13) 0.0005(13) O3 0.0192(16) 0.0155(16) 0.0318(14) -0.0052(13) -0.0083(12) -0.0015(13) O4 0.0308(17) 0.0202(17) 0.0228(14) 0.0060(13) 0.0085(12) 0.0002(14) O5 0.037(2) 0.038(2) 0.0367(16) 0.0144(15) 0.0229(15) 0.0108(16) O6 0.036(2) 0.021(2) 0.157(3) -0.021(2) 0.035(2) -0.0101(17) O7 0.030(2) 0.022(2) 0.108(3) -0.0212(19) -0.0039(19) 0.0065(16) O8 0.0240(18) 0.059(2) 0.0424(17) -0.0185(17) 0.0099(15) -0.0082(17) O9 0.0252(19) 0.082(3) 0.0404(17) -0.0306(18) 0.0131(14) -0.0077(17) O10 0.0417(19) 0.0188(17) 0.0260(14) -0.0069(13) 0.0117(14) -0.0026(14) O11 0.0385(19) 0.0202(16) 0.0410(17) -0.0167(13) 0.0235(15) -0.0145(14) O12 0.0295(17) 0.0182(16) 0.0304(15) 0.0055(13) 0.0149(13) 0.0077(13) O13 0.0271(17) 0.0217(17) 0.0286(14) -0.0008(13) 0.0037(13) -0.0038(14) _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 C20 1.526(5) . ? C1 C2 1.555(4) . ? C1 C11 1.560(4) . ? C1 C10 1.566(5) . ? C2 C3 1.519(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.329(5) . ? C3 C15 1.513(5) . ? C4 C12 1.518(5) . ? C4 C5 1.539(4) . ? C5 C6 1.541(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C21 1.526(4) . ? C6 C11 1.542(5) . ? C6 C7 1.579(4) . ? C7 C8 1.525(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.323(5) . ? C8 C19 1.509(5) . ? C9 C16 1.481(4) . ? C9 C10 1.514(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O1 1.197(3) . ? C12 C13 1.498(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.347(5) . ? C13 C23 1.498(5) . ? C14 C15 1.499(5) . ? C14 C22 1.519(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.502(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.327(5) . ? C17 C24 1.476(4) . ? C18 C19 1.485(4) . ? C18 C25 1.491(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O2 1.226(4) . ? C20 O3 1.321(4) . ? C21 O5 1.210(4) . ? C21 O4 1.326(4) . ? C22 O6 1.190(5) . ? C22 O7 1.332(5) . ? C23 O8 1.188(4) . ? C23 O9 1.320(4) . ? C24 O13 1.209(4) . ? C24 O12 1.353(4) . ? C25 O10 1.199(4) . ? C25 O11 1.328(4) . ? C26 O3 1.452(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 O4 1.455(3) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 O7 1.469(5) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O9 1.455(4) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 O11 1.465(4) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 O12 1.460(3) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 C20 C1 C2 110.2(3) . . ? C20 C1 C11 102.8(3) . . ? C2 C1 C11 111.4(3) . . ? C20 C1 C10 109.4(3) . . ? C2 C1 C10 110.8(3) . . ? C11 C1 C10 111.8(3) . . ? C3 C2 C1 113.9(3) . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C15 122.5(3) . . ? C4 C3 C2 121.1(3) . . ? C15 C3 C2 116.4(3) . . ? C3 C4 C12 122.9(3) . . ? C3 C4 C5 119.5(3) . . ? C12 C4 C5 117.6(3) . . ? C4 C5 C6 112.9(3) . . ? C4 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C21 C6 C5 110.0(3) . . ? C21 C6 C11 106.3(3) . . ? C5 C6 C11 110.6(3) . . ? C21 C6 C7 108.6(3) . . ? C5 C6 C7 113.4(3) . . ? C11 C6 C7 107.5(3) . . ? C8 C7 C6 116.5(3) . . ? C8 C7 H7A 108.2 . . ? C6 C7 H7A 108.2 . . ? C8 C7 H7B 108.2 . . ? C6 C7 H7B 108.2 . . ? H7A C7 H7B 107.3 . . ? C9 C8 C19 122.5(3) . . ? C9 C8 C7 123.4(3) . . ? C19 C8 C7 114.0(3) . . ? C8 C9 C16 121.9(3) . . ? C8 C9 C10 122.3(3) . . ? C16 C9 C10 115.8(3) . . ? C9 C10 C1 117.4(3) . . ? C9 C10 H10A 107.9 . . ? C1 C10 H10A 107.9 . . ? C9 C10 H10B 107.9 . . ? C1 C10 H10B 107.9 . . ? H10A C10 H10B 107.2 . . ? O1 C11 C6 120.6(3) . . ? O1 C11 C1 120.3(3) . . ? C6 C11 C1 119.0(3) . . ? C13 C12 C4 114.5(3) . . ? C13 C12 H12A 108.6 . . ? C4 C12 H12A 108.6 . . ? C13 C12 H12B 108.6 . . ? C4 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? C14 C13 C12 121.4(3) . . ? C14 C13 C23 124.8(4) . . ? C12 C13 C23 113.7(3) . . ? C13 C14 C15 124.0(3) . . ? C13 C14 C22 121.7(4) . . ? C15 C14 C22 113.9(3) . . ? C14 C15 C3 113.8(3) . . ? C14 C15 H15A 108.8 . . ? C3 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? C3 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C9 C16 C17 115.1(3) . . ? C9 C16 H16A 108.5 . . ? C17 C16 H16A 108.5 . . ? C9 C16 H16B 108.5 . . ? C17 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? C18 C17 C24 123.7(3) . . ? C18 C17 C16 122.9(3) . . ? C24 C17 C16 113.3(3) . . ? C17 C18 C19 121.6(3) . . ? C17 C18 C25 120.0(3) . . ? C19 C18 C25 118.4(3) . . ? C18 C19 C8 115.2(3) . . ? C18 C19 H19A 108.5 . . ? C8 C19 H19A 108.5 . . ? C18 C19 H19B 108.5 . . ? C8 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? O2 C20 O3 124.6(3) . . ? O2 C20 C1 123.2(4) . . ? O3 C20 C1 112.3(3) . . ? O5 C21 O4 124.3(3) . . ? O5 C21 C6 123.8(4) . . ? O4 C21 C6 111.9(3) . . ? O6 C22 O7 123.7(4) . . ? O6 C22 C14 122.8(4) . . ? O7 C22 C14 113.4(4) . . ? O8 C23 O9 124.5(4) . . ? O8 C23 C13 124.9(4) . . ? O9 C23 C13 110.3(3) . . ? O13 C24 O12 124.0(3) . . ? O13 C24 C17 124.6(4) . . ? O12 C24 C17 111.3(3) . . ? O10 C25 O11 123.5(4) . . ? O10 C25 C18 123.8(4) . . ? O11 C25 C18 112.8(3) . . ? O3 C26 H26A 109.5 . . ? O3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O4 C27 H27A 109.5 . . ? O4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O7 C28 H28A 109.5 . . ? O7 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O7 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O9 C29 H29A 109.5 . . ? O9 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O9 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O11 C30 H30A 109.5 . . ? O11 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O11 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O12 C31 H31A 109.5 . . ? O12 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O12 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C20 O3 C26 115.4(3) . . ? C21 O4 C27 115.1(3) . . ? C22 O7 C28 115.1(4) . . ? C23 O9 C29 115.7(3) . . ? C25 O11 C30 115.2(3) . . ? C24 O12 C31 114.8(3) . . ? 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 C20 C1 C2 C3 88.0(4) . . . . ? C11 C1 C2 C3 -25.5(4) . . . . ? C10 C1 C2 C3 -150.7(3) . . . . ? C1 C2 C3 C4 67.5(4) . . . . ? C1 C2 C3 C15 -112.6(3) . . . . ? C15 C3 C4 C12 0.9(5) . . . . ? C2 C3 C4 C12 -179.2(3) . . . . ? C15 C3 C4 C5 -178.9(3) . . . . ? C2 C3 C4 C5 0.9(5) . . . . ? C3 C4 C5 C6 -73.3(4) . . . . ? C12 C4 C5 C6 106.8(3) . . . . ? C4 C5 C6 C21 -85.1(4) . . . . ? C4 C5 C6 C11 32.1(4) . . . . ? C4 C5 C6 C7 153.0(3) . . . . ? C21 C6 C7 C8 -165.5(3) . . . . ? C5 C6 C7 C8 -42.9(4) . . . . ? C11 C6 C7 C8 79.8(4) . . . . ? C6 C7 C8 C9 -61.1(5) . . . . ? C6 C7 C8 C19 122.0(4) . . . . ? C19 C8 C9 C16 -7.9(6) . . . . ? C7 C8 C9 C16 175.4(3) . . . . ? C19 C8 C9 C10 171.1(3) . . . . ? C7 C8 C9 C10 -5.6(6) . . . . ? C8 C9 C10 C1 64.3(5) . . . . ? C16 C9 C10 C1 -116.7(4) . . . . ? C20 C1 C10 C9 174.3(3) . . . . ? C2 C1 C10 C9 52.5(4) . . . . ? C11 C1 C10 C9 -72.5(4) . . . . ? C21 C6 C11 O1 -5.9(5) . . . . ? C5 C6 C11 O1 -125.3(3) . . . . ? C7 C6 C11 O1 110.3(3) . . . . ? C21 C6 C11 C1 176.1(3) . . . . ? C5 C6 C11 C1 56.7(4) . . . . ? C7 C6 C11 C1 -67.7(4) . . . . ? C20 C1 C11 O1 3.1(4) . . . . ? C2 C1 C11 O1 121.1(4) . . . . ? C10 C1 C11 O1 -114.2(4) . . . . ? C20 C1 C11 C6 -178.9(3) . . . . ? C2 C1 C11 C6 -60.9(4) . . . . ? C10 C1 C11 C6 63.8(4) . . . . ? C3 C4 C12 C13 6.9(5) . . . . ? C5 C4 C12 C13 -173.2(3) . . . . ? C4 C12 C13 C14 -9.1(5) . . . . ? C4 C12 C13 C23 167.2(3) . . . . ? C12 C13 C14 C15 3.7(5) . . . . ? C23 C13 C14 C15 -172.2(3) . . . . ? C12 C13 C14 C22 176.4(3) . . . . ? C23 C13 C14 C22 0.5(6) . . . . ? C13 C14 C15 C3 4.3(5) . . . . ? C22 C14 C15 C3 -169.0(3) . . . . ? C4 C3 C15 C14 -6.6(5) . . . . ? C2 C3 C15 C14 173.5(3) . . . . ? C8 C9 C16 C17 9.8(5) . . . . ? C10 C9 C16 C17 -169.3(3) . . . . ? C9 C16 C17 C18 -3.8(6) . . . . ? C9 C16 C17 C24 178.7(3) . . . . ? C24 C17 C18 C19 173.3(3) . . . . ? C16 C17 C18 C19 -3.9(6) . . . . ? C24 C17 C18 C25 -8.2(6) . . . . ? C16 C17 C18 C25 174.6(3) . . . . ? C17 C18 C19 C8 6.0(5) . . . . ? C25 C18 C19 C8 -172.5(3) . . . . ? C9 C8 C19 C18 0.0(5) . . . . ? C7 C8 C19 C18 176.9(3) . . . . ? C2 C1 C20 O2 -24.2(5) . . . . ? C11 C1 C20 O2 94.7(4) . . . . ? C10 C1 C20 O2 -146.4(3) . . . . ? C2 C1 C20 O3 157.8(3) . . . . ? C11 C1 C20 O3 -83.3(3) . . . . ? C10 C1 C20 O3 35.7(4) . . . . ? C5 C6 C21 O5 21.2(5) . . . . ? C11 C6 C21 O5 -98.6(4) . . . . ? C7 C6 C21 O5 145.9(4) . . . . ? C5 C6 C21 O4 -159.9(3) . . . . ? C11 C6 C21 O4 80.3(4) . . . . ? C7 C6 C21 O4 -35.2(4) . . . . ? C13 C14 C22 O6 -145.4(5) . . . . ? C15 C14 C22 O6 28.1(6) . . . . ? C13 C14 C22 O7 32.3(6) . . . . ? C15 C14 C22 O7 -154.3(3) . . . . ? C14 C13 C23 O8 -125.4(5) . . . . ? C12 C13 C23 O8 58.4(5) . . . . ? C14 C13 C23 O9 60.8(5) . . . . ? C12 C13 C23 O9 -115.3(3) . . . . ? C18 C17 C24 O13 -77.1(6) . . . . ? C16 C17 C24 O13 100.3(4) . . . . ? C18 C17 C24 O12 107.8(4) . . . . ? C16 C17 C24 O12 -74.8(4) . . . . ? C17 C18 C25 O10 -8.4(6) . . . . ? C19 C18 C25 O10 170.1(4) . . . . ? C17 C18 C25 O11 171.8(4) . . . . ? C19 C18 C25 O11 -9.7(5) . . . . ? O2 C20 O3 C26 -5.3(5) . . . . ? C1 C20 O3 C26 172.6(3) . . . . ? O5 C21 O4 C27 0.9(5) . . . . ? C6 C21 O4 C27 -177.9(3) . . . . ? O6 C22 O7 C28 9.9(7) . . . . ? C14 C22 O7 C28 -167.7(4) . . . . ? O8 C23 O9 C29 6.8(6) . . . . ? C13 C23 O9 C29 -179.4(3) . . . . ? O10 C25 O11 C30 0.9(5) . . . . ? C18 C25 O11 C30 -179.3(3) . . . . ? O13 C24 O12 C31 -1.7(5) . . . . ? C17 C24 O12 C31 173.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.471 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.080