data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H24 O3' _chemical_formula_sum 'C29 H24 O3' _chemical_formula_weight 420.48 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 Orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 11.5953(17) _cell_length_b 7.1473(18) _cell_length_c 26.346(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2183.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 562 _cell_measurement_theta_min 2.9060 _cell_measurement_theta_max 21.9200 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9696 _exptl_absorpt_correction_T_max 0.9911 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _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 '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 4894 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2038 _reflns_number_gt 1140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0969P)^2^+13.1750P] 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 0.0092(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2038 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1998 _refine_ls_R_factor_gt 0.1405 _refine_ls_wR_factor_ref 0.3627 _refine_ls_wR_factor_gt 0.3184 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.8276(6) 0.2500 0.5229(3) 0.075(3) Uani 1 2 d S . . O2 O 0.6738(6) 0.2500 0.1783(2) 0.049(2) Uani 1 2 d S . . O3 O 0.6476(6) 0.2500 0.8653(2) 0.067(3) Uani 1 2 d S . . C1 C 0.7246(8) 0.2500 0.5222(4) 0.048(3) Uani 1 2 d S . . C2 C 0.6456(8) 0.2500 0.5674(3) 0.042(3) Uani 1 2 d S . . C3 C 0.6703(8) 0.2500 0.6186(3) 0.045(3) Uani 1 2 d S . . H3 H 0.7462 0.2500 0.6299 0.054 Uiso 1 2 calc SR . . C4 C 0.5780(7) 0.2500 0.6533(3) 0.038(2) Uani 1 2 d S . . C5 C 0.4639(7) 0.2500 0.6343(3) 0.038(2) Uani 1 2 d S . . H5 H 0.4027 0.2500 0.6571 0.045 Uiso 1 2 calc SR . . C6 C 0.4409(8) 0.2500 0.5834(3) 0.040(2) Uani 1 2 d S . . H6 H 0.3651 0.2500 0.5718 0.048 Uiso 1 2 calc SR . . C7 C 0.5311(7) 0.2500 0.5495(3) 0.035(2) Uani 1 2 d S . . C8 C 0.5336(7) 0.2500 0.4930(3) 0.040(2) Uani 1 2 d S . . C9 C 0.4458(8) 0.2500 0.4587(3) 0.047(3) Uani 1 2 d S . . H9 H 0.3695 0.2500 0.4696 0.057 Uiso 1 2 calc SR . . C10 C 0.4714(8) 0.2500 0.4075(3) 0.048(3) Uani 1 2 d S . . H10 H 0.4114 0.2500 0.3841 0.058 Uiso 1 2 calc SR . . C11 C 0.5863(8) 0.2500 0.3896(3) 0.045(3) Uani 1 2 d S . . C12 C 0.6742(8) 0.2500 0.4257(3) 0.043(3) Uani 1 2 d S . . H12 H 0.7510 0.2500 0.4154 0.051 Uiso 1 2 calc SR . . C13 C 0.6473(8) 0.2500 0.4767(3) 0.044(2) Uani 1 2 d S . . C14 C 0.5975(7) 0.2500 0.7089(3) 0.037(2) Uani 1 2 d S . . C15 C 0.6906(10) 0.333(2) 0.7307(4) 0.040(3) Uani 0.50 1 d P . . H15 H 0.7462 0.3877 0.7100 0.048 Uiso 0.50 1 d PR . . C16 C 0.7051(10) 0.347(2) 0.7822(4) 0.043(3) Uani 0.50 1 d P . . H16 H 0.7673 0.4123 0.7959 0.052 Uiso 0.50 1 d PR . . C17 C 0.6249(8) 0.2500 0.8142(3) 0.046(3) Uani 1 2 d S . . C18 C 0.5307(10) 0.170(2) 0.7949(4) 0.045(3) Uani 0.50 1 d P . . H18 H 0.4745 0.1205 0.8162 0.054 Uiso 0.50 1 d PR . . C19 C 0.5180(10) 0.162(2) 0.7422(4) 0.042(3) Uani 0.50 1 d P . . H19 H 0.4571 0.0936 0.7287 0.051 Uiso 0.50 1 d PR . . C20 C 0.5680(10) 0.2500 0.9006(4) 0.076(4) Uani 1 2 d S . . H20A H 0.5197 0.1407 0.8956 0.091 Uiso 0.50 1 calc PR . . H20B H 0.5197 0.3593 0.8956 0.091 Uiso 0.50 1 calc PR . . C21 C 0.6081(12) 0.2500 0.9534(4) 0.095(6) Uani 1 2 d S . . H21A H 0.6621 0.1498 0.9583 0.142 Uiso 0.50 1 calc PR . . H21B H 0.5435 0.2330 0.9757 0.142 Uiso 0.50 1 calc PR . . H21C H 0.6449 0.3672 0.9608 0.142 Uiso 0.50 1 calc PR . . C22 C 0.6086(8) 0.2500 0.3348(3) 0.039(2) Uani 1 2 d S . . C23 C 0.7093(10) 0.166(2) 0.3133(4) 0.041(3) Uani 0.50 1 d P . . H23 H 0.7622 0.1069 0.3344 0.049 Uiso 0.50 1 d PR . . C24 C 0.7281(11) 0.170(2) 0.2612(4) 0.046(3) Uani 0.50 1 d P . . H24 H 0.7955 0.1191 0.2479 0.055 Uiso 0.50 1 d PR . . C25 C 0.6465(8) 0.2500 0.2294(3) 0.039(2) Uani 1 2 d S . . C26 C 0.5476(10) 0.316(2) 0.2487(4) 0.044(4) Uani 0.50 1 d P . . H26 H 0.4909 0.3585 0.2265 0.053 Uiso 0.50 1 d PR . . C27 C 0.5284(10) 0.327(2) 0.3006(4) 0.039(3) Uani 0.50 1 d P . . H27 H 0.4630 0.3869 0.3129 0.047 Uiso 0.50 1 d PR . . C28 C 0.5927(12) 0.2500 0.1438(4) 0.091(5) Uani 1 2 d S . . H28A H 0.5446 0.3594 0.1490 0.109 Uiso 0.50 1 calc PR . . H28B H 0.5446 0.1406 0.1490 0.109 Uiso 0.50 1 calc PR . . C29 C 0.6328(13) 0.2500 0.0907(4) 0.101(6) Uani 1 2 d S . . H29A H 0.6942 0.3390 0.0869 0.152 Uiso 0.50 1 calc PR . . H29B H 0.5701 0.2835 0.0687 0.152 Uiso 0.50 1 calc PR . . H29C H 0.6602 0.1275 0.0819 0.152 Uiso 0.50 1 calc PR . . 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 0.037(4) 0.134(9) 0.054(4) 0.000 -0.001(3) 0.000 O2 0.058(4) 0.057(5) 0.032(3) 0.000 0.005(3) 0.000 O3 0.056(4) 0.111(8) 0.033(4) 0.000 -0.001(3) 0.000 C1 0.037(5) 0.064(7) 0.043(5) 0.000 -0.001(4) 0.000 C2 0.036(5) 0.053(7) 0.038(5) 0.000 -0.005(4) 0.000 C3 0.032(5) 0.059(7) 0.044(5) 0.000 -0.003(4) 0.000 C4 0.033(5) 0.043(6) 0.038(5) 0.000 0.002(4) 0.000 C5 0.033(5) 0.044(6) 0.036(5) 0.000 0.000(4) 0.000 C6 0.034(5) 0.047(6) 0.039(5) 0.000 -0.007(4) 0.000 C7 0.033(5) 0.036(6) 0.036(5) 0.000 -0.001(4) 0.000 C8 0.038(5) 0.044(6) 0.038(5) 0.000 -0.006(4) 0.000 C9 0.036(5) 0.065(8) 0.041(5) 0.000 -0.004(4) 0.000 C10 0.040(5) 0.063(7) 0.042(5) 0.000 -0.012(4) 0.000 C11 0.042(5) 0.051(6) 0.041(5) 0.000 -0.008(4) 0.000 C12 0.036(5) 0.055(7) 0.038(5) 0.000 -0.003(4) 0.000 C13 0.035(5) 0.058(7) 0.038(5) 0.000 -0.005(4) 0.000 C14 0.032(5) 0.043(6) 0.036(5) 0.000 -0.001(4) 0.000 C15 0.039(6) 0.045(7) 0.035(6) 0.002(6) -0.001(5) 0.003(7) C16 0.039(6) 0.050(8) 0.041(7) -0.006(7) -0.002(5) 0.006(7) C17 0.042(5) 0.060(7) 0.036(5) 0.000 -0.008(4) 0.000 C18 0.040(7) 0.056(9) 0.039(6) -0.006(7) 0.002(5) -0.003(7) C19 0.037(6) 0.048(8) 0.042(7) 0.001(7) -0.002(5) -0.004(7) C20 0.054(6) 0.129(14) 0.045(6) 0.000 0.002(5) 0.000 C21 0.069(8) 0.167(18) 0.049(7) 0.000 -0.003(6) 0.000 C22 0.039(5) 0.045(6) 0.033(5) 0.000 0.001(4) 0.000 C23 0.043(6) 0.041(7) 0.040(6) -0.001(6) -0.003(5) 0.010(7) C24 0.045(7) 0.048(8) 0.044(7) -0.009(7) 0.003(6) 0.004(7) C25 0.043(5) 0.038(6) 0.036(5) 0.000 0.004(4) 0.000 C26 0.046(7) 0.048(9) 0.040(6) 0.008(6) 0.000(5) 0.008(7) C27 0.044(7) 0.035(7) 0.039(6) 0.002(6) 0.002(5) 0.005(6) C28 0.078(9) 0.134(16) 0.060(8) 0.000 0.005(7) 0.000 C29 0.094(10) 0.167(19) 0.043(7) 0.000 0.011(7) 0.000 _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 C1 1.195(11) . ? O2 C28 1.308(13) . ? O2 C25 1.383(10) . ? O3 C20 1.309(12) . ? O3 C17 1.373(11) . ? C1 C13 1.498(12) . ? C1 C2 1.501(13) . ? C2 C3 1.379(12) . ? C2 C7 1.408(12) . ? C3 C4 1.408(12) . ? C3 H3 0.9300 . ? C4 C5 1.414(12) . ? C4 C14 1.481(12) . ? C5 C6 1.368(12) . ? C5 H5 0.9300 . ? C6 C7 1.376(12) . ? C6 H6 0.9300 . ? C7 C8 1.487(12) . ? C8 C9 1.361(13) . ? C8 C13 1.388(13) . ? C9 C10 1.383(13) . ? C9 H9 0.9300 . ? C10 C11 1.412(14) . ? C10 H10 0.9300 . ? C11 C12 1.395(12) . ? C11 C22 1.468(12) . ? C12 C13 1.378(12) . ? C12 H12 0.9300 . ? C14 C15 1.360(14) . ? C14 C15 1.360(14) 8_565 ? C14 C19 1.421(14) 8_565 ? C14 C19 1.421(14) . ? C15 C15 1.19(3) 8_565 ? C15 C16 1.371(15) . ? C15 C16 1.880(18) 8_565 ? C15 C19 2.025(17) 8_565 ? C15 H15 0.9300 . ? C16 C16 1.39(3) 8_565 ? C16 C17 1.436(15) . ? C16 C15 1.880(19) 8_565 ? C16 H16 0.9300 . ? C17 C18 1.334(15) . ? C17 C18 1.334(15) 8_565 ? C17 C16 1.436(15) 8_565 ? C18 C18 1.14(3) 8_565 ? C18 C19 1.396(15) . ? C18 C19 1.840(19) 8_565 ? C18 H18 0.9300 . ? C19 C19 1.26(3) 8_565 ? C19 C18 1.840(19) 8_565 ? C19 C15 2.025(17) 8_565 ? C19 H19 0.9300 . ? C20 C21 1.468(14) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C27 1.406(14) . ? C22 C27 1.406(14) 8_565 ? C22 C23 1.430(14) 8_565 ? C22 C23 1.430(14) . ? C23 C23 1.20(3) 8_565 ? C23 C24 1.391(15) . ? C23 C24 1.820(18) 8_565 ? C23 H23 0.9300 . ? C24 C24 1.15(3) 8_565 ? C24 C25 1.389(15) . ? C24 C23 1.820(18) 8_565 ? C24 H24 0.9300 . ? C25 C26 1.341(14) 8_565 ? C25 C26 1.341(14) . ? C25 C24 1.389(15) 8_565 ? C26 C26 0.95(3) 8_565 ? C26 C27 1.387(15) . ? C26 C27 1.722(17) 8_565 ? C26 H26 0.9300 . ? C27 C27 1.10(3) 8_565 ? C27 C26 1.722(17) 8_565 ? C27 H27 0.9300 . ? C28 C29 1.474(14) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 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 C28 O2 C25 120.8(8) . . ? C20 O3 C17 124.1(8) . . ? O1 C1 C13 127.5(9) . . ? O1 C1 C2 126.9(9) . . ? C13 C1 C2 105.6(8) . . ? C3 C2 C7 121.5(8) . . ? C3 C2 C1 130.4(8) . . ? C7 C2 C1 108.1(8) . . ? C2 C3 C4 118.6(8) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C5 118.7(8) . . ? C3 C4 C14 121.7(8) . . ? C5 C4 C14 119.6(8) . . ? C6 C5 C4 122.0(8) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 119.3(8) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C6 C7 C2 119.9(8) . . ? C6 C7 C8 131.6(8) . . ? C2 C7 C8 108.5(8) . . ? C9 C8 C13 120.3(9) . . ? C9 C8 C7 130.5(8) . . ? C13 C8 C7 109.2(8) . . ? C8 C9 C10 119.2(9) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C9 C10 C11 121.8(9) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C12 C11 C10 117.6(8) . . ? C12 C11 C22 122.9(9) . . ? C10 C11 C22 119.6(8) . . ? C13 C12 C11 119.9(8) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 121.2(8) . . ? C12 C13 C1 130.2(8) . . ? C8 C13 C1 108.6(8) . . ? C15 C14 C15 51.8(12) . 8_565 ? C15 C14 C19 93.4(8) . 8_565 ? C15 C14 C19 116.5(9) 8_565 8_565 ? C15 C14 C19 116.5(9) . . ? C15 C14 C19 93.4(8) 8_565 . ? C19 C14 C19 52.5(12) 8_565 . ? C15 C14 C4 122.7(8) . . ? C15 C14 C4 122.7(8) 8_565 . ? C19 C14 C4 120.8(8) 8_565 . ? C19 C14 C4 120.8(8) . . ? C15 C15 C14 64.1(6) 8_565 . ? C15 C15 C16 94.3(9) 8_565 . ? C14 C15 C16 123.3(11) . . ? C15 C15 C16 46.7(6) 8_565 8_565 ? C14 C15 C16 94.4(9) . 8_565 ? C16 C15 C16 47.6(11) . 8_565 ? C15 C15 C19 91.0(7) 8_565 8_565 ? C14 C15 C19 44.5(6) . 8_565 ? C16 C15 C19 88.4(8) . 8_565 ? C16 C15 C19 89.5(8) 8_565 8_565 ? C15 C15 H15 114.8 8_565 . ? C14 C15 H15 119.0 . . ? C16 C15 H15 117.7 . . ? C16 C15 H15 130.5 8_565 . ? C19 C15 H15 139.9 8_565 . ? C15 C16 C16 85.7(9) . 8_565 ? C15 C16 C17 117.7(12) . . ? C16 C16 C17 61.0(6) 8_565 . ? C15 C16 C15 39.0(10) . 8_565 ? C16 C16 C15 46.7(6) 8_565 8_565 ? C17 C16 C15 91.9(9) . 8_565 ? C15 C16 H16 121.0 . . ? C16 C16 H16 119.9 8_565 . ? C17 C16 H16 121.2 . . ? C15 C16 H16 133.7 8_565 . ? C18 C17 C18 50.8(14) . 8_565 ? C18 C17 O3 122.1(9) . . ? C18 C17 O3 122.1(9) 8_565 . ? C18 C17 C16 121.0(9) . . ? C18 C17 C16 95.7(8) 8_565 . ? O3 C17 C16 116.8(8) . . ? C18 C17 C16 95.7(8) . 8_565 ? C18 C17 C16 121.0(9) 8_565 8_565 ? O3 C17 C16 116.8(8) . 8_565 ? C16 C17 C16 58.0(12) . 8_565 ? C18 C18 C17 64.6(7) 8_565 . ? C18 C18 C19 92.3(9) 8_565 . ? C17 C18 C19 118.8(11) . . ? C18 C18 C19 49.3(6) 8_565 8_565 ? C17 C18 C19 94.2(10) . 8_565 ? C19 C18 C19 43.1(11) . 8_565 ? C18 C18 H18 112.4 8_565 . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.8 . . ? C19 C18 H18 130.4 8_565 . ? C19 C19 C18 87.7(9) 8_565 . ? C19 C19 C14 63.7(6) 8_565 . ? C18 C19 C14 121.9(11) . . ? C19 C19 C18 49.3(6) 8_565 8_565 ? C18 C19 C18 38.4(11) . 8_565 ? C14 C19 C18 97.2(10) . 8_565 ? C19 C19 C15 89.0(7) 8_565 8_565 ? C18 C19 C15 92.5(8) . 8_565 ? C14 C19 C15 42.1(6) . 8_565 ? C18 C19 C15 91.3(8) 8_565 8_565 ? C19 C19 H19 121.7 8_565 . ? C18 C19 H19 118.9 . . ? C14 C19 H19 119.2 . . ? C18 C19 H19 133.9 8_565 . ? C15 C19 H19 134.6 8_565 . ? O3 C20 C21 116.7(10) . . ? O3 C20 H20A 108.1 . . ? C21 C20 H20A 108.1 . . ? O3 C20 H20B 108.1 . . ? C21 C20 H20B 108.1 . . ? H20A C20 H20B 107.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C27 46.0(12) . 8_565 ? C27 C22 C23 97.1(8) . 8_565 ? C27 C22 C23 116.8(9) 8_565 8_565 ? C27 C22 C23 116.8(9) . . ? C27 C22 C23 97.1(8) 8_565 . ? C23 C22 C23 49.6(12) 8_565 . ? C27 C22 C11 120.9(8) . . ? C27 C22 C11 120.9(8) 8_565 . ? C23 C22 C11 122.2(8) 8_565 . ? C23 C22 C11 122.2(8) . . ? C23 C23 C24 89.0(9) 8_565 . ? C23 C23 C22 65.2(6) 8_565 . ? C24 C23 C22 120.7(11) . . ? C23 C23 C24 49.8(6) 8_565 8_565 ? C24 C23 C24 39.2(11) . 8_565 ? C22 C23 C24 97.2(9) . 8_565 ? C23 C23 H23 117.1 8_565 . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 131.8 8_565 . ? C24 C24 C25 65.6(6) 8_565 . ? C24 C24 C23 91.0(9) 8_565 . ? C25 C24 C23 119.8(11) . . ? C24 C24 C23 49.8(6) 8_565 8_565 ? C25 C24 C23 96.2(10) . 8_565 ? C23 C24 C23 41.2(10) . 8_565 ? C24 C24 H24 112.9 8_565 . ? C25 C24 H24 120.4 . . ? C23 C24 H24 119.8 . . ? C23 C24 H24 129.5 8_565 . ? C26 C25 C26 41.4(12) 8_565 . ? C26 C25 O2 124.4(9) 8_565 . ? C26 C25 O2 124.4(9) . . ? C26 C25 C24 120.0(10) 8_565 8_565 ? C26 C25 C24 101.9(9) . 8_565 ? O2 C25 C24 115.6(8) . 8_565 ? C26 C25 C24 101.9(9) 8_565 . ? C26 C25 C24 120.0(10) . . ? O2 C25 C24 115.6(8) . . ? C24 C25 C24 48.9(13) 8_565 . ? C26 C26 C25 69.3(6) 8_565 . ? C26 C26 C27 93.1(8) 8_565 . ? C25 C26 C27 122.1(11) . . ? C26 C26 C27 53.5(6) 8_565 8_565 ? C25 C26 C27 101.7(10) . 8_565 ? C27 C26 C27 39.6(10) . 8_565 ? C26 C26 H26 108.9 8_565 . ? C25 C26 H26 118.8 . . ? C27 C26 H26 119.2 . . ? C27 C26 H26 126.8 8_565 . ? C27 C27 C26 86.9(8) 8_565 . ? C27 C27 C22 67.0(6) 8_565 . ? C26 C27 C22 120.2(11) . . ? C27 C27 C26 53.5(6) 8_565 8_565 ? C26 C27 C26 33.3(10) . 8_565 ? C22 C27 C26 101.0(10) . 8_565 ? C27 C27 H27 117.5 8_565 . ? C26 C27 H27 120.1 . . ? C22 C27 H27 119.7 . . ? C26 C27 H27 131.1 8_565 . ? O2 C28 C29 115.6(11) . . ? O2 C28 H28A 108.4 . . ? C29 C28 H28A 108.4 . . ? O2 C28 H28B 108.4 . . ? C29 C28 H28B 108.4 . . ? H28A C28 H28B 107.4 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 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 O1 C1 C2 C3 0.000(4) . . . . ? C13 C1 C2 C3 180.000(3) . . . . ? O1 C1 C2 C7 180.000(3) . . . . ? C13 C1 C2 C7 0.000(2) . . . . ? C7 C2 C3 C4 0.000(4) . . . . ? C1 C2 C3 C4 180.000(3) . . . . ? C2 C3 C4 C5 0.000(4) . . . . ? C2 C3 C4 C14 180.000(3) . . . . ? C3 C4 C5 C6 0.000(4) . . . . ? C14 C4 C5 C6 180.000(3) . . . . ? C4 C5 C6 C7 0.000(4) . . . . ? C5 C6 C7 C2 0.000(4) . . . . ? C5 C6 C7 C8 180.000(3) . . . . ? C3 C2 C7 C6 0.000(4) . . . . ? C1 C2 C7 C6 180.000(3) . . . . ? C3 C2 C7 C8 180.000(3) . . . . ? C1 C2 C7 C8 0.000(2) . . . . ? C6 C7 C8 C9 0.000(4) . . . . ? C2 C7 C8 C9 180.000(3) . . . . ? C6 C7 C8 C13 180.000(3) . . . . ? C2 C7 C8 C13 0.000(3) . . . . ? C13 C8 C9 C10 0.000(3) . . . . ? C7 C8 C9 C10 180.000(3) . . . . ? C8 C9 C10 C11 0.000(3) . . . . ? C9 C10 C11 C12 0.000(3) . . . . ? C9 C10 C11 C22 180.000(2) . . . . ? C10 C11 C12 C13 0.000(3) . . . . ? C22 C11 C12 C13 180.000(2) . . . . ? C11 C12 C13 C8 0.000(3) . . . . ? C11 C12 C13 C1 180.000(3) . . . . ? C9 C8 C13 C12 0.000(3) . . . . ? C7 C8 C13 C12 180.000(2) . . . . ? C9 C8 C13 C1 180.000(2) . . . . ? C7 C8 C13 C1 0.000(2) . . . . ? O1 C1 C13 C12 0.000(4) . . . . ? C2 C1 C13 C12 180.000(3) . . . . ? O1 C1 C13 C8 180.000(3) . . . . ? C2 C1 C13 C8 0.000(3) . . . . ? C3 C4 C14 C15 31.2(8) . . . . ? C5 C4 C14 C15 -148.8(8) . . . . ? C3 C4 C14 C15 -31.2(8) . . . 8_565 ? C5 C4 C14 C15 148.8(8) . . . 8_565 ? C3 C4 C14 C19 149.0(8) . . . 8_565 ? C5 C4 C14 C19 -31.0(8) . . . 8_565 ? C3 C4 C14 C19 -149.0(8) . . . . ? C5 C4 C14 C19 31.0(8) . . . . ? C19 C14 C15 C15 121.5(7) 8_565 . . 8_565 ? C19 C14 C15 C15 72.1(8) . . . 8_565 ? C4 C14 C15 C15 -108.1(7) . . . 8_565 ? C15 C14 C15 C16 -77.4(14) 8_565 . . . ? C19 C14 C15 C16 44.1(14) 8_565 . . . ? C19 C14 C15 C16 -5.3(18) . . . . ? C4 C14 C15 C16 174.5(11) . . . . ? C15 C14 C15 C16 -36.6(8) 8_565 . . 8_565 ? C19 C14 C15 C16 84.8(8) 8_565 . . 8_565 ? C19 C14 C15 C16 35.5(11) . . . 8_565 ? C4 C14 C15 C16 -144.8(6) . . . 8_565 ? C15 C14 C15 C19 -121.5(7) 8_565 . . 8_565 ? C19 C14 C15 C19 -49.4(13) . . . 8_565 ? C4 C14 C15 C19 130.4(8) . . . 8_565 ? C15 C15 C16 C16 0.000(11) 8_565 . . 8_565 ? C14 C15 C16 C16 61.7(12) . . . 8_565 ? C19 C15 C16 C16 90.9(7) 8_565 . . 8_565 ? C15 C15 C16 C17 -53.9(10) 8_565 . . . ? C14 C15 C16 C17 8(2) . . . . ? C16 C15 C16 C17 -53.9(11) 8_565 . . . ? C19 C15 C16 C17 37.0(13) 8_565 . . . ? C14 C15 C16 C15 61.7(12) . . . 8_565 ? C16 C15 C16 C15 0.000(15) 8_565 . . 8_565 ? C19 C15 C16 C15 90.9(7) 8_565 . . 8_565 ? C20 O3 C17 C18 -30.4(9) . . . . ? C20 O3 C17 C18 30.4(9) . . . 8_565 ? C20 O3 C17 C16 147.1(7) . . . . ? C20 O3 C17 C16 -147.1(7) . . . 8_565 ? C15 C16 C17 C18 -9.0(18) . . . . ? C16 C16 C17 C18 -76.2(9) 8_565 . . . ? C15 C16 C17 C18 -39.7(12) 8_565 . . . ? C15 C16 C17 C18 -56.1(14) . . . 8_565 ? C16 C16 C17 C18 -123.2(8) 8_565 . . 8_565 ? C15 C16 C17 C18 -86.7(9) 8_565 . . 8_565 ? C15 C16 C17 O3 173.5(10) . . . . ? C16 C16 C17 O3 106.3(7) 8_565 . . . ? C15 C16 C17 O3 142.8(6) 8_565 . . . ? C15 C16 C17 C16 67.2(13) . . . 8_565 ? C15 C16 C17 C16 36.5(8) 8_565 . . 8_565 ? O3 C17 C18 C18 107.3(7) . . . 8_565 ? C16 C17 C18 C18 -70.0(9) . . . 8_565 ? C16 C17 C18 C18 -125.9(8) 8_565 . . 8_565 ? C18 C17 C18 C19 77.9(13) 8_565 . . . ? O3 C17 C18 C19 -174.8(10) . . . . ? C16 C17 C18 C19 7.8(18) . . . . ? C16 C17 C18 C19 -48.1(14) 8_565 . . . ? C18 C17 C18 C19 40.6(8) 8_565 . . 8_565 ? O3 C17 C18 C19 148.0(6) . . . 8_565 ? C16 C17 C18 C19 -29.4(13) . . . 8_565 ? C16 C17 C18 C19 -85.3(8) 8_565 . . 8_565 ? C18 C18 C19 C19 0.000(14) 8_565 . . 8_565 ? C17 C18 C19 C19 -62.1(11) . . . 8_565 ? C18 C18 C19 C14 56.8(11) 8_565 . . . ? C17 C18 C19 C14 -5(2) . . . . ? C19 C18 C19 C14 56.8(11) 8_565 . . . ? C17 C18 C19 C18 -62.1(11) . . . 8_565 ? C19 C18 C19 C18 0.00(3) 8_565 . . 8_565 ? C18 C18 C19 C15 88.9(7) 8_565 . . 8_565 ? C17 C18 C19 C15 26.8(14) . . . 8_565 ? C19 C18 C19 C15 88.9(7) 8_565 . . 8_565 ? C15 C14 C19 C19 72.7(8) . . . 8_565 ? C15 C14 C19 C19 121.2(7) 8_565 . . 8_565 ? C4 C14 C19 C19 -107.1(7) . . . 8_565 ? C15 C14 C19 C18 3.8(17) . . . . ? C15 C14 C19 C18 52.3(14) 8_565 . . . ? C19 C14 C19 C18 -68.8(13) 8_565 . . . ? C4 C14 C19 C18 -176.0(10) . . . . ? C15 C14 C19 C18 35.4(12) . . . 8_565 ? C15 C14 C19 C18 83.9(8) 8_565 . . 8_565 ? C19 C14 C19 C18 -37.3(8) 8_565 . . 8_565 ? C4 C14 C19 C18 -144.4(6) . . . 8_565 ? C15 C14 C19 C15 -48.5(13) . . . 8_565 ? C19 C14 C19 C15 -121.2(7) 8_565 . . 8_565 ? C4 C14 C19 C15 131.7(8) . . . 8_565 ? C17 O3 C20 C21 180.000(5) . . . . ? C12 C11 C22 C27 -152.9(7) . . . . ? C10 C11 C22 C27 27.1(7) . . . . ? C12 C11 C22 C27 152.9(7) . . . 8_565 ? C10 C11 C22 C27 -27.1(7) . . . 8_565 ? C12 C11 C22 C23 -29.7(8) . . . 8_565 ? C10 C11 C22 C23 150.3(8) . . . 8_565 ? C12 C11 C22 C23 29.7(8) . . . . ? C10 C11 C22 C23 -150.3(8) . . . . ? C27 C22 C23 C23 75.6(8) . . . 8_565 ? C27 C22 C23 C23 119.4(7) 8_565 . . 8_565 ? C11 C22 C23 C23 -106.9(7) . . . 8_565 ? C27 C22 C23 C24 2.9(17) . . . . ? C27 C22 C23 C24 46.7(14) 8_565 . . . ? C23 C22 C23 C24 -72.7(13) 8_565 . . . ? C11 C22 C23 C24 -179.6(10) . . . . ? C27 C22 C23 C24 36.4(12) . . . 8_565 ? C27 C22 C23 C24 80.2(8) 8_565 . . 8_565 ? C23 C22 C23 C24 -39.2(8) 8_565 . . 8_565 ? C11 C22 C23 C24 -146.1(6) . . . 8_565 ? C23 C23 C24 C24 0.000(6) 8_565 . . 8_565 ? C22 C23 C24 C24 60.1(11) . . . 8_565 ? C23 C23 C24 C25 -62.2(11) 8_565 . . . ? C22 C23 C24 C25 -2.1(19) . . . . ? C24 C23 C24 C25 -62.2(11) 8_565 . . . ? C22 C23 C24 C23 60.1(11) . . . 8_565 ? C24 C23 C24 C23 0.000(7) 8_565 . . 8_565 ? C28 O2 C25 C26 25.4(8) . . . 8_565 ? C28 O2 C25 C26 -25.4(8) . . . . ? C28 O2 C25 C24 -152.7(7) . . . 8_565 ? C28 O2 C25 C24 152.7(7) . . . . ? C24 C24 C25 C26 -119.5(8) 8_565 . . 8_565 ? C23 C24 C25 C26 -43.3(14) . . . 8_565 ? C23 C24 C25 C26 -79.2(9) 8_565 . . 8_565 ? C24 C24 C25 C26 -79.3(9) 8_565 . . . ? C23 C24 C25 C26 -3.0(18) . . . . ? C23 C24 C25 C26 -38.9(13) 8_565 . . . ? C24 C24 C25 O2 102.6(6) 8_565 . . . ? C23 C24 C25 O2 178.8(10) . . . . ? C23 C24 C25 O2 142.9(6) 8_565 . . . ? C23 C24 C25 C24 76.2(13) . . . 8_565 ? C23 C24 C25 C24 40.4(8) 8_565 . . 8_565 ? O2 C25 C26 C26 105.0(7) . . . 8_565 ? C24 C25 C26 C26 -122.1(8) 8_565 . . 8_565 ? C24 C25 C26 C26 -73.0(9) . . . 8_565 ? C26 C25 C26 C27 80.3(13) 8_565 . . . ? O2 C25 C26 C27 -174.7(9) . . . . ? C24 C25 C26 C27 -41.8(14) 8_565 . . . ? C24 C25 C26 C27 7.3(18) . . . . ? C26 C25 C26 C27 43.4(9) 8_565 . . 8_565 ? O2 C25 C26 C27 148.4(6) . . . 8_565 ? C24 C25 C26 C27 -78.8(9) 8_565 . . 8_565 ? C24 C25 C26 C27 -29.6(14) . . . 8_565 ? C26 C26 C27 C27 0.000(5) 8_565 . . 8_565 ? C25 C26 C27 C27 -67.4(11) . . . 8_565 ? C26 C26 C27 C22 61.0(11) 8_565 . . . ? C25 C26 C27 C22 -6.4(19) . . . . ? C27 C26 C27 C22 61.0(11) 8_565 . . . ? C25 C26 C27 C26 -67.4(11) . . . 8_565 ? C27 C26 C27 C26 0.000(11) 8_565 . . 8_565 ? C23 C22 C27 C27 120.8(7) 8_565 . . 8_565 ? C23 C22 C27 C27 72.8(8) . . . 8_565 ? C11 C22 C27 C27 -104.7(6) . . . 8_565 ? C27 C22 C27 C26 -71.6(12) 8_565 . . . ? C23 C22 C27 C26 49.2(13) 8_565 . . . ? C23 C22 C27 C26 1.2(16) . . . . ? C11 C22 C27 C26 -176.3(9) . . . . ? C27 C22 C27 C26 -42.3(8) 8_565 . . 8_565 ? C23 C22 C27 C26 78.5(9) 8_565 . . 8_565 ? C23 C22 C27 C26 30.5(12) . . . 8_565 ? C11 C22 C27 C26 -147.0(6) . . . 8_565 ? C25 O2 C28 C29 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.456 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.082