#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2202181.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2202181 loop_ _publ_author_name 'Huang, Xue-Song' 'Jiang, Ren-Wang' 'Ooi, Vincent Eng-Choon' _publ_section_title ; Trilobolide-6-O-isobutyrate, a eudesmanolide from Wedelia trilobata ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o771 _journal_page_last o772 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac 'C23 H32 O9' _chemical_formula_moiety 'C23 H32 O9' _chemical_formula_sum 'C23 H32 O9' _chemical_formula_weight 452.49 _chemical_name_common trilobolide-6-O-isobutyrate _chemical_name_systematic ; ; _space_group_IT_number 170 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P 65' _symmetry_space_group_name_H-M 'P 65' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 _cell_length_a 9.8368(8) _cell_length_b 9.8368(8) _cell_length_c 42.455(5) _cell_measurement_reflns_used 4824 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20.8 _cell_measurement_theta_min 2.44 _cell_volume 3557.7(6) _computing_cell_refinement 'SMART and SAINT (Bruker, 1998)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction 'SHELXS97 (Sheldrick, 1990)' _computing_molecular_graphics 'XP (Bruker, 1998)' _computing_publication_material SHELXTL/PC _computing_structure_refinement SHELXTL/PC _computing_structure_solution 'SHELXTL/PC (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Siemens SMART/CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_av_sigmaI/netI 0.047 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_number 19275 _diffrn_reflns_theta_full 25.0 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 2.4 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1452 _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.29 _refine_diff_density_max 0.30 _refine_diff_density_min -0.31 _refine_ls_abs_structure_Flack unk _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 280 _refine_ls_number_reflns 2119 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.04 _refine_ls_R_factor_all 0.066 _refine_ls_R_factor_gt 0.051 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.105P)^2^+0.2647P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.141 _refine_ls_wR_factor_ref 0.153 _reflns_number_gt 3029 _reflns_number_total 4172 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file tk6094.cif _[local]_cod_data_source_block I _cod_original_cell_volume 3557.6(6) _cod_database_code 2202181 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol O1 1.0229(4) 0.4731(4) 0.15271(7) 0.0534(8) Uani d . 1 O O2 0.7978(6) 0.3943(7) 0.17972(11) 0.0958(16) Uani d . 1 O O3 0.8361(4) 0.5346(4) 0.08709(7) 0.0448(7) Uani d . 1 O O4 0.8481(7) 0.6893(8) 0.12673(14) 0.122(2) Uani d . 1 O O5 0.8084(5) 0.0559(4) 0.05076(10) 0.0687(11) Uani d . 1 O H5A 0.8146 -0.0236 0.0484 0.08(2) Uiso calc R 1 H O6 1.1286(4) 0.3798(4) 0.02784(7) 0.0486(8) Uani d . 1 O O7 1.0525(5) 0.3461(6) -0.02266(8) 0.0718(11) Uani d . 1 O O8 1.0362(5) 0.7789(4) 0.05164(8) 0.0556(9) Uani d . 1 O O9 0.8391(7) 0.7867(5) 0.02710(11) 0.0889(15) Uani d . 1 O C1 0.9351(6) 0.3630(6) 0.12733(11) 0.0501(11) Uani d . 1 C H1A 0.8296 0.3499 0.1265 0.060 Uiso calc R 1 H C2 0.9204(7) 0.2058(6) 0.13451(12) 0.0619(14) Uani d . 1 C H2A 0.8634 0.1644 0.1541 0.074 Uiso calc R 1 H H2B 1.0238 0.2174 0.1368 0.074 Uiso calc R 1 H C3 0.8322(7) 0.0934(6) 0.10729(13) 0.0634(14) Uani d . 1 C H3A 0.8211 -0.0083 0.1119 0.076 Uiso calc R 1 H H3B 0.7277 0.0797 0.1059 0.076 Uiso calc R 1 H C4 0.9140(6) 0.1505(5) 0.07540(11) 0.0519(12) Uani d . 1 C C5 0.9342(5) 0.3163(5) 0.06973(10) 0.0412(10) Uani d . 1 C H5B 0.8265 0.2969 0.0710 0.049 Uiso calc R 1 H C6 0.9848(5) 0.3804(5) 0.03632(10) 0.0409(9) Uani d . 1 C H6A 0.9019 0.3098 0.0218 0.049 Uiso calc R 1 H C7 1.0154(6) 0.5468(5) 0.03049(11) 0.0449(10) Uani d . 1 C H7A 1.0960 0.5926 0.0141 0.054 Uiso calc R 1 H C8 1.0765(6) 0.6583(5) 0.05857(11) 0.0449(10) Uani d . 1 C H8A 1.1908 0.7060 0.0600 0.054 Uiso calc R 1 H C9 1.0026(5) 0.5819(5) 0.08962(10) 0.0412(10) Uani d . 1 C H9A 1.0509 0.6586 0.1067 0.049 Uiso calc R 1 H C10 1.0203(5) 0.4385(5) 0.09645(10) 0.0408(10) Uani d . 1 C C11 0.8805(6) 0.5655(6) 0.01966(11) 0.0540(12) Uani d . 1 C C12 0.9120(7) 0.7198(6) 0.03235(12) 0.0562(13) Uani d . 1 C C13 0.7620(9) 0.4789(9) 0.00149(15) 0.085(2) Uani d . 1 C H13A 0.6921 0.5125 -0.0041 0.102 Uiso calc R 1 H H13B 0.7469 0.3833 -0.0059 0.102 Uiso calc R 1 H C14 1.0630(7) 0.1371(7) 0.07467(14) 0.0659(15) Uani d . 1 C H14A 1.0356 0.0302 0.0785 0.099 Uiso calc R 1 H H14B 1.1345 0.2035 0.0906 0.099 Uiso calc R 1 H H14C 1.1120 0.1692 0.0544 0.099 Uiso calc R 1 H C15 1.1982(6) 0.4990(6) 0.09873(11) 0.0510(11) Uani d . 1 C H15A 1.2420 0.5723 0.1158 0.076 Uiso calc R 1 H H15B 1.2482 0.5501 0.0794 0.076 Uiso calc R 1 H H15C 1.2150 0.4122 0.1024 0.076 Uiso calc R 1 H C16 0.9365(8) 0.4699(8) 0.17795(13) 0.0657(14) Uani d . 1 C C17 1.0411(10) 0.5783(9) 0.20335(16) 0.087(2) Uani d . 1 C H17A 0.9782 0.5753 0.2209 0.131 Uiso calc R 1 H H17B 1.0986 0.6834 0.1953 0.131 Uiso calc R 1 H H17C 1.1133 0.5452 0.2101 0.131 Uiso calc R 1 H C18 0.7774(7) 0.6038(7) 0.10565(13) 0.0645(15) Uani d . 1 C C19 0.6121(8) 0.5561(10) 0.09579(19) 0.089(2) Uani d . 1 C H19A 0.5719 0.6066 0.1092 0.133 Uiso calc R 1 H H19B 0.5468 0.4442 0.0976 0.133 Uiso calc R 1 H H19C 0.6123 0.5870 0.0743 0.133 Uiso calc R 1 H C20 1.1473(6) 0.3604(7) -0.00316(12) 0.0548(12) Uani d . 1 C C21 1.2954(8) 0.3593(9) -0.00938(14) 0.0805(19) Uani d . 1 C H21A 1.3739 0.4137 0.0071 0.097 Uiso calc R 1 H C22 1.2545(19) 0.194(2) -0.0127(5) 0.221(8) Uiso d . 1 C H22A 1.2169 0.1408 0.0071 0.331 Uiso calc R 1 H H22B 1.3459 0.1892 -0.0190 0.331 Uiso calc R 1 H H22C 1.1741 0.1437 -0.0284 0.331 Uiso calc R 1 H C23 1.3581(19) 0.4185(17) -0.0409(4) 0.182(6) Uiso d . 1 C H23A 1.3908 0.5281 -0.0422 0.273 Uiso calc R 1 H H23B 1.2781 0.3617 -0.0564 0.273 Uiso calc R 1 H H23C 1.4463 0.4043 -0.0449 0.273 Uiso calc R 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.069(2) 0.063(2) 0.0340(16) 0.0379(18) -0.0070(15) -0.0044(14) O2 0.082(3) 0.132(4) 0.076(3) 0.055(3) 0.012(2) -0.018(3) O3 0.0487(17) 0.0510(18) 0.0449(16) 0.0325(15) -0.0010(13) -0.0038(13) O4 0.121(4) 0.164(6) 0.123(5) 0.102(4) -0.031(4) -0.086(4) O5 0.090(3) 0.0450(19) 0.078(3) 0.039(2) -0.025(2) -0.0193(18) O6 0.0532(18) 0.0615(19) 0.0426(17) 0.0373(16) -0.0063(14) -0.0113(14) O7 0.073(3) 0.110(3) 0.0447(19) 0.055(3) -0.0066(18) -0.014(2) O8 0.078(2) 0.0415(18) 0.0532(19) 0.0340(17) -0.0072(17) 0.0003(14) O9 0.141(4) 0.091(3) 0.078(3) 0.091(3) -0.034(3) -0.016(2) C1 0.065(3) 0.047(3) 0.039(2) 0.028(2) -0.005(2) -0.0015(19) C2 0.088(4) 0.054(3) 0.052(3) 0.041(3) 0.001(3) 0.011(2) C3 0.076(4) 0.044(3) 0.067(3) 0.027(3) -0.003(3) 0.008(2) C4 0.065(3) 0.040(2) 0.055(3) 0.029(2) -0.011(2) -0.007(2) C5 0.046(2) 0.039(2) 0.046(2) 0.027(2) -0.0029(18) -0.0043(18) C6 0.042(2) 0.044(2) 0.041(2) 0.025(2) -0.0068(18) -0.0043(17) C7 0.057(3) 0.044(2) 0.041(2) 0.031(2) 0.004(2) 0.0014(19) C8 0.048(2) 0.039(2) 0.050(2) 0.023(2) -0.0058(19) -0.0022(19) C9 0.047(2) 0.037(2) 0.041(2) 0.022(2) -0.0097(18) -0.0086(17) C10 0.050(3) 0.040(2) 0.036(2) 0.025(2) -0.0054(18) -0.0039(17) C11 0.075(3) 0.062(3) 0.043(2) 0.048(3) -0.012(2) -0.008(2) C12 0.084(4) 0.060(3) 0.047(3) 0.052(3) -0.007(2) 0.003(2) C13 0.119(6) 0.102(5) 0.072(4) 0.083(5) -0.052(4) -0.036(4) C14 0.095(4) 0.060(3) 0.067(3) 0.057(3) -0.014(3) -0.010(3) C15 0.059(3) 0.056(3) 0.047(2) 0.036(3) -0.012(2) -0.009(2) C16 0.082(4) 0.086(4) 0.047(3) 0.056(4) 0.003(3) -0.005(3) C17 0.114(5) 0.107(5) 0.059(4) 0.070(5) -0.017(3) -0.029(4) C18 0.077(4) 0.077(4) 0.059(3) 0.053(3) -0.002(3) -0.007(3) C19 0.077(4) 0.118(6) 0.095(5) 0.067(4) 0.014(4) 0.004(4) C20 0.059(3) 0.066(3) 0.047(3) 0.037(3) -0.002(2) -0.011(2) C21 0.080(4) 0.122(6) 0.061(3) 0.067(4) 0.001(3) -0.015(3) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C16 O1 C1 115.6(4) ? C18 O3 C9 119.4(4) ? C4 O5 H5A 109.5 ? C20 O6 C6 116.0(3) ? C12 O8 C8 109.3(3) ? O1 C1 C2 109.1(4) ? O1 C1 C10 107.1(4) ? C2 C1 C10 114.7(4) ? O1 C1 H1A 108.6 ? C2 C1 H1A 108.6 ? C10 C1 H1A 108.6 ? C1 C2 C3 108.5(4) ? C1 C2 H2A 110.0 ? C3 C2 H2A 110.0 ? C1 C2 H2B 110.0 ? C3 C2 H2B 110.0 ? H2A C2 H2B 108.4 ? C4 C3 C2 113.4(4) ? C4 C3 H3A 108.9 ? C2 C3 H3A 108.9 ? C4 C3 H3B 108.9 ? C2 C3 H3B 108.9 ? H3A C3 H3B 107.7 ? O5 C4 C3 109.2(4) ? O5 C4 C14 109.9(4) ? C3 C4 C14 109.6(4) ? O5 C4 C5 103.7(4) ? C3 C4 C5 106.8(4) ? C14 C4 C5 117.3(4) ? C6 C5 C10 114.6(3) ? C6 C5 C4 114.8(4) ? C10 C5 C4 115.5(3) ? C6 C5 H5B 103.2 ? C10 C5 H5B 103.2 ? C4 C5 H5B 103.2 ? O6 C6 C7 106.9(4) ? O6 C6 C5 110.0(3) ? C7 C6 C5 116.2(4) ? O6 C6 H6A 107.8 ? C7 C6 H6A 107.8 ? C5 C6 H6A 107.8 ? C11 C7 C8 101.9(3) ? C11 C7 C6 117.9(4) ? C8 C7 C6 116.1(4) ? C11 C7 H7A 106.7 ? C8 C7 H7A 106.7 ? C6 C7 H7A 106.7 ? O8 C8 C9 108.8(4) ? O8 C8 C7 104.9(3) ? C9 C8 C7 113.9(4) ? O8 C8 H8A 109.7 ? C9 C8 H8A 109.7 ? C7 C8 H8A 109.7 ? O3 C9 C8 106.1(3) ? O3 C9 C10 110.2(4) ? C8 C9 C10 112.0(4) ? O3 C9 H9A 109.5 ? C8 C9 H9A 109.5 ? C10 C9 H9A 109.5 ? C1 C10 C9 108.7(4) ? C1 C10 C15 111.9(4) ? C9 C10 C15 106.6(4) ? C1 C10 C5 107.1(4) ? C9 C10 C5 107.7(3) ? C15 C10 C5 114.6(4) ? C13 C11 C12 123.0(5) yes C13 C11 C7 131.4(5) yes C12 C11 C7 105.5(4) yes O9 C12 O8 122.4(5) ? O9 C12 C11 127.5(5) ? O8 C12 C11 110.1(4) ? C11 C13 H13A 120.0 ? C11 C13 H13B 120.0 ? H13A C13 H13B 120.0 ? C4 C14 H14A 109.5 ? C4 C14 H14B 109.5 ? H14A C14 H14B 109.5 ? C4 C14 H14C 109.5 ? H14A C14 H14C 109.5 ? H14B C14 H14C 109.5 ? C10 C15 H15A 109.5 ? C10 C15 H15B 109.5 ? H15A C15 H15B 109.5 ? C10 C15 H15C 109.5 ? H15A C15 H15C 109.5 ? H15B C15 H15C 109.5 ? O2 C16 O1 125.1(6) ? O2 C16 C17 124.4(6) ? O1 C16 C17 110.5(6) ? C16 C17 H17A 109.5 ? C16 C17 H17B 109.5 ? H17A C17 H17B 109.5 ? C16 C17 H17C 109.5 ? H17A C17 H17C 109.5 ? H17B C17 H17C 109.5 ? O4 C18 O3 123.5(6) ? O4 C18 C19 126.0(6) ? O3 C18 C19 110.4(5) ? C18 C19 H19A 109.5 ? C18 C19 H19B 109.5 ? H19A C19 H19B 109.5 ? C18 C19 H19C 109.5 ? H19A C19 H19C 109.5 ? H19B C19 H19C 109.5 ? O7 C20 O6 122.3(5) ? O7 C20 C21 125.7(5) ? O6 C20 C21 112.0(4) ? C23 C21 C22 100.3(11) ? C23 C21 C20 112.2(8) ? C22 C21 C20 107.3(9) ? C23 C21 H21A 112.1 ? C22 C21 H21A 112.1 ? C20 C21 H21A 112.1 ? C21 C22 H22A 109.5 ? C21 C22 H22B 109.5 ? H22A C22 H22B 109.5 ? C21 C22 H22C 109.5 ? H22A C22 H22C 109.5 ? H22B C22 H22C 109.5 ? C21 C23 H23A 109.5 ? C21 C23 H23B 109.5 ? H23A C23 H23B 109.5 ? C21 C23 H23C 109.5 ? H23A C23 H23C 109.5 ? H23B C23 H23C 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 C16 1.359(7) yes O1 C1 1.464(6) yes O2 C16 1.185(8) yes O3 C18 1.346(6) yes O3 C9 1.465(6) yes O4 C18 1.186(7) yes O5 C4 1.439(6) yes O5 H5A 0.8200 ? O6 C20 1.355(6) yes O6 C6 1.463(5) yes O7 C20 1.201(6) yes O8 C12 1.338(6) yes O8 C8 1.456(5) yes O9 C12 1.211(6) yes C1 C2 1.510(7) ? C1 C10 1.533(7) ? C1 H1A 0.9800 ? C2 C3 1.534(8) ? C2 H2A 0.9700 ? C2 H2B 0.9700 ? C3 C4 1.531(8) ? C3 H3A 0.9700 ? C3 H3B 0.9700 ? C4 C14 1.536(8) ? C4 C5 1.560(6) ? C5 C6 1.531(6) ? C5 C10 1.559(6) ? C5 H5B 0.9800 ? C6 C7 1.529(6) ? C6 H6A 0.9800 ? C7 C11 1.500(7) ? C7 C8 1.525(6) ? C7 H7A 0.9800 ? C8 C9 1.512(7) ? C8 H8A 0.9800 ? C9 C10 1.534(6) ? C9 H9A 0.9800 ? C10 C15 1.544(7) ? C11 C13 1.299(8) yes C11 C12 1.490(7) ? C13 H13A 0.9300 ? C13 H13B 0.9300 ? C14 H14A 0.9600 ? C14 H14B 0.9600 ? C14 H14C 0.9600 ? C15 H15A 0.9600 ? C15 H15B 0.9600 ? C15 H15C 0.9600 ? C16 C17 1.504(9) ? C17 H17A 0.9600 ? C17 H17B 0.9600 ? C17 H17C 0.9600 ? C18 C19 1.509(9) ? C19 H19A 0.9600 ? C19 H19B 0.9600 ? C19 H19C 0.9600 ? C20 C21 1.487(8) ? C21 C23 1.468(18) ? C21 C22 1.48(2) ? C21 H21A 0.9800 ? C22 H22A 0.9600 ? C22 H22B 0.9600 ? C22 H22C 0.9600 ? C23 H23A 0.9600 ? C23 H23B 0.9600 ? C23 H23C 0.9600 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O5 H5A O9 1_545 0.82 2.19 2.986(3) 163 yes 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 C16 O1 C1 C2 -85.8(5) C16 O1 C1 C10 149.6(4) O1 C1 C2 C3 -178.4(4) C10 C1 C2 C3 -58.4(6) C1 C2 C3 C4 59.3(6) C2 C3 C4 O5 -168.2(4) C2 C3 C4 C14 71.4(6) C2 C3 C4 C5 -56.6(6) O5 C4 C5 C6 -53.4(5) C3 C4 C5 C6 -168.7(4) C14 C4 C5 C6 68.0(5) O5 C4 C5 C10 169.8(4) C3 C4 C5 C10 54.5(5) C14 C4 C5 C10 -68.8(5) C20 O6 C6 C7 -83.2(5) C20 O6 C6 C5 149.9(4) C10 C5 C6 O6 82.3(4) C4 C5 C6 O6 -54.8(5) C10 C5 C6 C7 -39.3(5) C4 C5 C6 C7 -176.4(4) O6 C6 C7 C11 146.6(4) C5 C6 C7 C11 -90.2(5) O6 C6 C7 C8 -92.2(4) C5 C6 C7 C8 31.0(6) C12 O8 C8 C9 -96.6(4) C12 O8 C8 C7 25.6(5) C11 C7 C8 O8 -28.3(5) C6 C7 C8 O8 -157.7(4) C11 C7 C8 C9 90.6(5) C6 C7 C8 C9 -38.8(6) C18 O3 C9 C8 -114.3(4) C18 O3 C9 C10 124.3(4) O8 C8 C9 O3 51.9(4) C7 C8 C9 O3 -64.8(4) O8 C8 C9 C10 172.1(3) C7 C8 C9 C10 55.5(5) O1 C1 C10 C9 -68.0(4) C2 C1 C10 C9 170.8(4) O1 C1 C10 C15 49.4(5) C2 C1 C10 C15 -71.8(5) O1 C1 C10 C5 175.9(3) C2 C1 C10 C5 54.7(5) O3 C9 C10 C1 -59.2(4) C8 C9 C10 C1 -177.0(4) O3 C9 C10 C15 -180.0(3) C8 C9 C10 C15 62.2(4) O3 C9 C10 C5 56.6(4) C8 C9 C10 C5 -61.3(5) C6 C5 C10 C1 170.0(4) C4 C5 C10 C1 -53.2(5) C6 C5 C10 C9 53.2(5) C4 C5 C10 C9 -169.9(4) C6 C5 C10 C15 -65.2(5) C4 C5 C10 C15 71.7(5) C8 C7 C11 C13 -162.7(7) C6 C7 C11 C13 -34.5(9) C8 C7 C11 C12 21.5(5) C6 C7 C11 C12 149.8(4) C8 O8 C12 O9 167.6(5) C8 O8 C12 C11 -11.7(6) C13 C11 C12 O9 -2.6(10) C7 C11 C12 O9 173.6(6) C13 C11 C12 O8 176.7(6) C7 C11 C12 O8 -7.2(6) C1 O1 C16 O2 -5.4(8) C1 O1 C16 C17 175.5(5) C9 O3 C18 O4 -8.9(9) C9 O3 C18 C19 171.4(5) C6 O6 C20 O7 0.7(7) C6 O6 C20 C21 -179.2(5) O7 C20 C21 C23 29.4(11) O6 C20 C21 C23 -150.7(8) O7 C20 C21 C22 -79.8(12) O6 C20 C21 C22 100.1(11)