# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 loop_ _publ_author_name _publ_author_address A.Cappelli ; Dipartimento Farmaco Chimico Tecnologico Universit\`a degli Studi di Siena via Aldo Moro I-53100 Siena Italy ; G.Giorgi ; Dipartimento di Chimica Universit\`a degli Studi di Siena Via Aldo Moro I-53100 Siena Italy ; S.Vomero ; Dipartimento Farmaco Chimico Tecnologico Universit\`a degli Studi di Siena via Aldo Moro I-53100 Siena Italy ; _publ_contact_author_address ; Dipartimento di Chimica Universit\`a degli Studi di Siena Via Aldo Moro I-53100 Siena Italy ; _publ_contact_author_email gianluca.giorgi@unisi.it _publ_contact_author_fax '+39 0577 234241' _publ_contact_author_phone '+39 0577 234233' _publ_contact_author_name 'Giorgi, Gianluca' data_vc1381 _database_code_depnum_ccdc_archive 'CCDC 844780' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Ethyl 4,6-Dimethoxy-3-phenyl-1H-indene-2-carboxylate ; _chemical_formula_moiety 'C20 H20 O4' _chemical_formula_sum 'C20 H20 O4' _chemical_formula_weight 324.36 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4451(4) _cell_length_b 20.3610(6) _cell_length_c 7.0378(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.380(4) _cell_angle_gamma 90.00 _cell_volume 1748.28(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3185 _cell_measurement_theta_min 2.6005 _cell_measurement_theta_max 29.0725 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_T_min 0.99731 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.0827 _diffrn_reflns_number 16411 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.1083 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 29.14 _reflns_number_total 4187 _reflns_number_gt 1543 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0406P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 4187 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1526 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 0.744 _refine_ls_restrained_S_all 0.744 _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 0.17418(14) 0.27016(9) 0.8628(3) 0.0423(5) Uani 1 1 d . . . H1A H 0.1861(12) 0.2985(7) 0.756(2) 0.052(5) Uiso 1 1 d . . . H1B H 0.1815(13) 0.2987(7) 0.976(2) 0.058(5) Uiso 1 1 d . . . C2 C 0.25564(13) 0.21533(8) 0.9009(2) 0.0421(4) Uani 1 1 d . . . C3 C 0.20466(13) 0.15653(8) 0.8740(2) 0.0401(4) Uani 1 1 d . . . C4 C 0.08654(13) 0.16801(8) 0.8158(2) 0.0401(4) Uani 1 1 d . . . C5 C -0.00322(15) 0.12503(8) 0.7735(3) 0.0493(5) Uani 1 1 d . . . C6 C -0.10752(16) 0.15088(10) 0.7237(3) 0.0571(5) Uani 1 1 d . . . H6 H -0.1688(15) 0.1233(8) 0.698(2) 0.073(6) Uiso 1 1 d . . . C7 C -0.12396(15) 0.21882(10) 0.7155(3) 0.0518(5) Uani 1 1 d . . . C8 C -0.03703(15) 0.26146(10) 0.7588(2) 0.0467(5) Uani 1 1 d . . . H8 H -0.0464(12) 0.3065(7) 0.752(2) 0.041(5) Uiso 1 1 d . . . C9 C 0.06682(15) 0.23524(8) 0.8085(2) 0.0406(4) Uani 1 1 d . . . C10 C 0.37452(16) 0.22608(9) 0.9556(2) 0.0470(5) Uani 1 1 d . . . C11 C 0.51190(18) 0.30801(12) 1.0224(5) 0.0747(7) Uani 1 1 d . . . H11A H 0.551(2) 0.2892(11) 0.925(4) 0.119(10) Uiso 1 1 d . . . H11B H 0.546(2) 0.2878(13) 1.153(4) 0.160(13) Uiso 1 1 d . . . C12 C 0.5203(3) 0.37872(17) 1.0327(10) 0.1230(14) Uani 1 1 d . . . H12A H 0.593(2) 0.3891(10) 1.078(3) 0.098(7) Uiso 1 1 d . . . H12B H 0.497(3) 0.3943(18) 0.902(6) 0.23(2) Uiso 1 1 d . . . H12C H 0.479(3) 0.3980(17) 1.095(6) 0.20(2) Uiso 1 1 d . . . C13 C -0.0699(3) 0.01436(14) 0.7443(7) 0.1087(12) Uani 1 1 d . . . H13A H -0.105(2) 0.0192(11) 0.601(4) 0.114(11) Uiso 1 1 d . . . H13B H -0.125(2) 0.0220(11) 0.829(4) 0.129(12) Uiso 1 1 d . . . H13C H -0.0367(19) -0.0296(12) 0.768(3) 0.120(9) Uiso 1 1 d . . . C14 C -0.2560(2) 0.30557(12) 0.6558(5) 0.0733(7) Uani 1 1 d . . . H14A H -0.2187(16) 0.3266(9) 0.565(3) 0.078(7) Uiso 1 1 d . . . H14B H -0.2307(18) 0.3278(11) 0.787(3) 0.112(9) Uiso 1 1 d . . . H14C H -0.339(2) 0.3078(9) 0.612(3) 0.099(7) Uiso 1 1 d . . . O1 O 0.44569(11) 0.18516(6) 0.9880(2) 0.0733(4) Uani 1 1 d . . . O2 O 0.39625(10) 0.29082(6) 0.96640(19) 0.0622(4) Uani 1 1 d . . . O3 O 0.01959(10) 0.05939(6) 0.7857(2) 0.0722(4) Uani 1 1 d . . . O4 O -0.23154(10) 0.23689(6) 0.6627(2) 0.0727(4) Uani 1 1 d . . . C1' C 0.25757(14) 0.09078(8) 0.8998(3) 0.0507(5) Uani 1 1 d . . . C2' C 0.30290(18) 0.06840(11) 1.0817(4) 0.0708(6) Uani 1 1 d . . . H2' H 0.2996(18) 0.0969(11) 1.197(3) 0.115(9) Uiso 1 1 d . . . C3' C 0.3544(2) 0.00828(13) 1.1084(6) 0.0979(9) Uani 1 1 d . . . H3' H 0.385(2) -0.0072(11) 1.249(4) 0.129(10) Uiso 1 1 d . . . C4' C 0.3595(2) -0.03005(14) 0.9497(7) 0.1074(12) Uani 1 1 d . . . H4' H 0.395(2) -0.0696(12) 0.974(3) 0.113(9) Uiso 1 1 d . . . C5' C 0.3151(3) -0.00869(15) 0.7710(7) 0.1153(11) Uani 1 1 d . . . H5' H 0.316(2) -0.0312(12) 0.652(3) 0.128(10) Uiso 1 1 d . . . C6' C 0.2628(2) 0.05231(12) 0.7433(4) 0.0856(8) Uani 1 1 d . . . H6' H 0.2308(18) 0.0655(10) 0.612(3) 0.096(9) Uiso 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 0.0393(12) 0.0477(11) 0.0396(13) -0.0021(10) 0.0068(9) -0.0086(10) C2 0.0343(11) 0.0514(11) 0.0402(11) -0.0030(9) 0.0066(8) -0.0037(10) C3 0.0363(10) 0.0470(10) 0.0368(11) -0.0020(8) 0.0065(8) -0.0044(10) C4 0.0331(11) 0.0451(10) 0.0414(11) -0.0007(8) 0.0055(8) -0.0038(9) C5 0.0426(13) 0.0445(12) 0.0594(13) -0.0002(9) 0.0064(10) -0.0064(10) C6 0.0337(12) 0.0639(15) 0.0706(14) -0.0019(11) 0.0030(10) -0.0116(12) C7 0.0358(12) 0.0597(13) 0.0576(13) -0.0003(10) 0.0038(9) 0.0010(11) C8 0.0420(13) 0.0479(12) 0.0493(13) 0.0006(10) 0.0073(9) 0.0013(11) C9 0.0379(11) 0.0496(11) 0.0345(10) -0.0010(9) 0.0078(8) -0.0040(10) C10 0.0427(13) 0.0520(12) 0.0463(13) -0.0020(10) 0.0093(10) -0.0093(11) C11 0.0388(14) 0.0768(17) 0.104(2) -0.0146(17) 0.0043(15) -0.0230(12) C12 0.061(2) 0.083(2) 0.209(5) -0.007(3) -0.011(3) -0.0356(18) C13 0.072(2) 0.0566(17) 0.183(4) 0.002(2) -0.010(3) -0.0218(16) C14 0.0452(16) 0.0735(17) 0.100(2) 0.0065(16) 0.0104(16) 0.0118(13) O1 0.0378(9) 0.0647(9) 0.1133(12) -0.0007(8) 0.0045(8) 0.0001(8) O2 0.0371(9) 0.0564(9) 0.0891(11) -0.0044(7) 0.0029(7) -0.0131(7) O3 0.0457(9) 0.0480(8) 0.1165(12) 0.0010(7) 0.0004(8) -0.0125(7) O4 0.0324(9) 0.0724(10) 0.1079(11) 0.0028(8) 0.0002(7) 0.0039(7) C1' 0.0313(11) 0.0467(11) 0.0709(15) -0.0014(11) 0.0023(10) -0.0022(9) C2' 0.0602(15) 0.0578(14) 0.0903(19) 0.0136(14) 0.0047(13) 0.0115(12) C3' 0.081(2) 0.0675(18) 0.136(3) 0.019(2) 0.000(2) 0.0092(15) C4' 0.0599(19) 0.0481(18) 0.203(4) 0.000(2) -0.002(2) 0.0022(15) C5' 0.100(2) 0.083(2) 0.155(3) -0.047(2) 0.008(2) 0.0199(18) C6' 0.089(2) 0.0736(17) 0.088(2) -0.0275(16) 0.0025(16) 0.0208(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C9 1.495(2) . ? C1 C2 1.496(2) . ? C1 H1A 0.983(15) . ? C1 H1B 0.977(16) . ? C2 C3 1.351(2) . ? C2 C10 1.470(2) . ? C3 C4 1.465(2) . ? C3 C1' 1.487(2) . ? C4 C9 1.390(2) . ? C4 C5 1.404(2) . ? C5 O3 1.3655(19) . ? C5 C6 1.380(2) . ? C6 C7 1.398(2) . ? C6 H6 0.936(18) . ? C7 O4 1.367(2) . ? C7 C8 1.374(2) . ? C8 C9 1.378(2) . ? C8 H8 0.925(14) . ? C10 O1 1.2046(19) . ? C10 O2 1.3448(19) . ? C11 C12 1.444(4) . ? C11 O2 1.458(2) . ? C11 H11A 0.99(2) . ? C11 H11B 1.02(3) . ? C12 H12A 0.93(2) . ? C12 H12B 0.96(4) . ? C12 H12C 0.84(3) . ? C13 O3 1.427(3) . ? C13 H13A 1.02(2) . ? C13 H13B 1.01(2) . ? C13 H13C 0.99(2) . ? C14 O4 1.430(2) . ? C14 H14A 0.959(19) . ? C14 H14B 1.02(2) . ? C14 H14C 1.02(2) . ? C1' C6' 1.364(3) . ? C1' C2' 1.371(3) . ? C2' C3' 1.377(3) . ? C2' H2' 1.01(2) . ? C3' C4' 1.374(4) . ? C3' H3' 1.04(3) . ? C4' C5' 1.343(4) . ? C4' H4' 0.92(2) . ? C5' C6' 1.398(4) . ? C5' H5' 0.96(2) . ? C6' H6' 0.97(2) . ? 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 C9 C1 C2 103.33(14) . . ? C9 C1 H1A 110.2(9) . . ? C2 C1 H1A 112.1(8) . . ? C9 C1 H1B 115.2(9) . . ? C2 C1 H1B 110.3(9) . . ? H1A C1 H1B 105.8(13) . . ? C3 C2 C10 126.12(16) . . ? C3 C2 C1 110.69(15) . . ? C10 C2 C1 123.18(15) . . ? C2 C3 C4 108.39(14) . . ? C2 C3 C1' 126.61(15) . . ? C4 C3 C1' 125.00(14) . . ? C9 C4 C5 118.60(16) . . ? C9 C4 C3 109.12(14) . . ? C5 C4 C3 132.26(15) . . ? O3 C5 C6 124.24(17) . . ? O3 C5 C4 116.73(16) . . ? C6 C5 C4 119.03(17) . . ? C5 C6 C7 120.70(18) . . ? C5 C6 H6 120.6(11) . . ? C7 C6 H6 118.7(11) . . ? O4 C7 C8 125.18(17) . . ? O4 C7 C6 113.90(17) . . ? C8 C7 C6 120.92(18) . . ? C7 C8 C9 118.01(18) . . ? C7 C8 H8 122.0(10) . . ? C9 C8 H8 120.0(10) . . ? C8 C9 C4 122.74(16) . . ? C8 C9 C1 128.80(15) . . ? C4 C9 C1 108.46(16) . . ? O1 C10 O2 122.35(16) . . ? O1 C10 C2 127.67(17) . . ? O2 C10 C2 109.98(16) . . ? C12 C11 O2 108.1(2) . . ? C12 C11 H11A 112.3(13) . . ? O2 C11 H11A 108.3(14) . . ? C12 C11 H11B 110.0(16) . . ? O2 C11 H11B 111.1(16) . . ? H11A C11 H11B 107(2) . . ? C11 C12 H12A 107.6(14) . . ? C11 C12 H12B 106(2) . . ? H12A C12 H12B 110(3) . . ? C11 C12 H12C 117(3) . . ? H12A C12 H12C 112(3) . . ? H12B C12 H12C 105(4) . . ? O3 C13 H13A 107.6(14) . . ? O3 C13 H13B 112.1(15) . . ? H13A C13 H13B 111(2) . . ? O3 C13 H13C 105.3(14) . . ? H13A C13 H13C 109.9(19) . . ? H13B C13 H13C 111(2) . . ? O4 C14 H14A 109.3(11) . . ? O4 C14 H14B 112.0(13) . . ? H14A C14 H14B 107.5(18) . . ? O4 C14 H14C 104.6(11) . . ? H14A C14 H14C 111.8(17) . . ? H14B C14 H14C 111.6(17) . . ? C10 O2 C11 115.30(15) . . ? C5 O3 C13 118.15(18) . . ? C7 O4 C14 117.60(17) . . ? C6' C1' C2' 119.1(2) . . ? C6' C1' C3 120.60(19) . . ? C2' C1' C3 120.25(17) . . ? C1' C2' C3' 121.1(3) . . ? C1' C2' H2' 119.2(13) . . ? C3' C2' H2' 119.7(13) . . ? C4' C3' C2' 119.3(3) . . ? C4' C3' H3' 122.4(14) . . ? C2' C3' H3' 118.2(14) . . ? C5' C4' C3' 120.1(3) . . ? C5' C4' H4' 123.6(15) . . ? C3' C4' H4' 116.4(15) . . ? C4' C5' C6' 120.8(3) . . ? C4' C5' H5' 126.4(16) . . ? C6' C5' H5' 112.8(16) . . ? C1' C6' C5' 119.5(3) . . ? C1' C6' H6' 122.3(12) . . ? C5' C6' H6' 118.2(13) . . ? 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 C9 C1 C2 C3 -0.12(19) . . . . ? C9 C1 C2 C10 178.57(14) . . . . ? C10 C2 C3 C4 -178.46(15) . . . . ? C1 C2 C3 C4 0.18(19) . . . . ? C10 C2 C3 C1' 2.0(3) . . . . ? C1 C2 C3 C1' -179.32(16) . . . . ? C2 C3 C4 C9 -0.18(18) . . . . ? C1' C3 C4 C9 179.33(15) . . . . ? C2 C3 C4 C5 -178.69(17) . . . . ? C1' C3 C4 C5 0.8(3) . . . . ? C9 C4 C5 O3 -178.84(14) . . . . ? C3 C4 C5 O3 -0.4(3) . . . . ? C9 C4 C5 C6 0.9(2) . . . . ? C3 C4 C5 C6 179.29(17) . . . . ? O3 C5 C6 C7 179.64(17) . . . . ? C4 C5 C6 C7 -0.1(3) . . . . ? C5 C6 C7 O4 179.54(16) . . . . ? C5 C6 C7 C8 -0.7(3) . . . . ? O4 C7 C8 C9 -179.65(16) . . . . ? C6 C7 C8 C9 0.7(3) . . . . ? C7 C8 C9 C4 0.2(3) . . . . ? C7 C8 C9 C1 -179.59(17) . . . . ? C5 C4 C9 C8 -1.0(2) . . . . ? C3 C4 C9 C8 -179.72(15) . . . . ? C5 C4 C9 C1 178.85(15) . . . . ? C3 C4 C9 C1 0.10(19) . . . . ? C2 C1 C9 C8 179.81(16) . . . . ? C2 C1 C9 C4 0.00(19) . . . . ? C3 C2 C10 O1 -1.2(3) . . . . ? C1 C2 C10 O1 -179.66(17) . . . . ? C3 C2 C10 O2 178.98(15) . . . . ? C1 C2 C10 O2 0.5(2) . . . . ? O1 C10 O2 C11 -0.7(3) . . . . ? C2 C10 O2 C11 179.17(19) . . . . ? C12 C11 O2 C10 -178.3(3) . . . . ? C6 C5 O3 C13 0.0(3) . . . . ? C4 C5 O3 C13 179.8(3) . . . . ? C8 C7 O4 C14 -1.4(3) . . . . ? C6 C7 O4 C14 178.35(19) . . . . ? C2 C3 C1' C6' -108.8(2) . . . . ? C4 C3 C1' C6' 71.7(2) . . . . ? C2 C3 C1' C2' 70.4(2) . . . . ? C4 C3 C1' C2' -109.0(2) . . . . ? C6' C1' C2' C3' 0.7(3) . . . . ? C3 C1' C2' C3' -178.56(19) . . . . ? C1' C2' C3' C4' -0.5(4) . . . . ? C2' C3' C4' C5' 0.3(4) . . . . ? C3' C4' C5' C6' -0.3(5) . . . . ? C2' C1' C6' C5' -0.7(3) . . . . ? C3 C1' C6' C5' 178.6(2) . . . . ? C4' C5' C6' C1' 0.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 0.140 _refine_diff_density_min -0.152 _refine_diff_density_rms 0.031 data_vc1382p2 _database_code_depnum_ccdc_archive 'CCDC 844781' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Ethyl 4,6-Dimethoxy-1-oxo-3-phenyl-1H-indene-2-carboxylate ; _chemical_formula_moiety 'C20 H18 O5' _chemical_formula_sum 'C20 H18 O5' _chemical_formula_weight 338.34 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.466(4) _cell_length_b 19.438(6) _cell_length_c 7.173(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.53(4) _cell_angle_gamma 90.00 _cell_volume 1718.9(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 707 _cell_measurement_theta_min 2.0934 _cell_measurement_theta_max 29.1157 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_colour red-violet _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_T_min 0.78043 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.0827 _diffrn_reflns_number 7919 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.3275 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 29.15 _reflns_number_total 3866 _reflns_number_gt 875 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.1505P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.004(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3866 _refine_ls_number_parameters 250 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.3231 _refine_ls_R_factor_gt 0.1246 _refine_ls_wR_factor_ref 0.3417 _refine_ls_wR_factor_gt 0.3005 _refine_ls_goodness_of_fit_ref 0.838 _refine_ls_restrained_S_all 0.838 _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 0.8499(6) 0.2800(4) 0.1276(10) 0.053(2) Uani 1 1 d . . . O1 O 0.8444(4) 0.3413(2) 0.1233(7) 0.0658(16) Uani 1 1 d . . . C2 C 0.7631(5) 0.2271(4) 0.0814(11) 0.060(2) Uani 1 1 d . . . C3 C 0.8103(5) 0.1630(3) 0.1158(9) 0.0424(17) Uani 1 1 d . . . C4 C 0.9246(5) 0.1690(3) 0.1828(11) 0.050(2) Uani 1 1 d . . . C5 C 1.0069(6) 0.1212(3) 0.2345(11) 0.056(2) Uani 1 1 d . . . C6 C 1.1110(6) 0.1459(4) 0.2984(11) 0.068(2) Uani 1 1 d . . . H6 H 1.1661 0.1144 0.3365 0.082 Uiso 1 1 calc R . . C7 C 1.1354(6) 0.2154(4) 0.3071(11) 0.058(2) Uani 1 1 d . . . C8 C 1.0555(5) 0.2625(3) 0.2629(10) 0.048(2) Uani 1 1 d . . . H8 H 1.0698 0.3092 0.2790 0.058 Uiso 1 1 calc R . . C9 C 0.9521(5) 0.2395(3) 0.1931(11) 0.050(2) Uani 1 1 d . . . C10 C 0.6461(6) 0.2421(5) 0.0255(14) 0.075(3) Uani 1 1 d . A . O2 O 0.5774(5) 0.2000(3) -0.0145(11) 0.101(2) Uani 1 1 d . . . O3 O 0.6245(4) 0.3063(3) 0.0004(11) 0.118(3) Uani 1 1 d D . . C11A C 0.5026(13) 0.3177(16) -0.010(8) 0.081(14) Uani 0.38(3) 1 d PD A 1 H11A H 0.4607 0.2855 -0.0949 0.097 Uiso 0.38(3) 1 calc PR A 1 H11B H 0.4796 0.3155 0.1132 0.097 Uiso 0.38(3) 1 calc PR A 1 C12A C 0.497(4) 0.3894(18) -0.088(5) 0.13(2) Uani 0.38(3) 1 d PD A 1 H12A H 0.5635 0.4131 -0.0433 0.195 Uiso 0.38(3) 1 calc PR A 1 H12B H 0.4375 0.4134 -0.0463 0.195 Uiso 0.38(3) 1 calc PR A 1 H12C H 0.4865 0.3876 -0.2228 0.195 Uiso 0.38(3) 1 calc PR A 1 C11B C 0.5230(16) 0.3307(15) -0.128(3) 0.120(12) Uani 0.62(3) 1 d PD A 2 H11C H 0.5397 0.3579 -0.2333 0.144 Uiso 0.62(3) 1 calc PR A 2 H11D H 0.4747 0.2932 -0.1728 0.144 Uiso 0.62(3) 1 calc PR A 2 C12B C 0.4809(17) 0.3734(17) 0.019(4) 0.113(10) Uani 0.62(3) 1 d PD A 2 H12D H 0.4795 0.3463 0.1307 0.169 Uiso 0.62(3) 1 calc PR A 2 H12E H 0.4088 0.3889 -0.0279 0.169 Uiso 0.62(3) 1 calc PR A 2 H12F H 0.5273 0.4125 0.0491 0.169 Uiso 0.62(3) 1 calc PR A 2 O4 O 0.9804(4) 0.0532(2) 0.2216(8) 0.0719(18) Uani 1 1 d . . . C13 C 1.0601(7) 0.0015(4) 0.2608(13) 0.100(3) Uani 1 1 d . . . H13A H 1.1102 0.0044 0.1715 0.151 Uiso 1 1 calc R . . H13B H 1.0259 -0.0429 0.2514 0.151 Uiso 1 1 calc R . . H13C H 1.0984 0.0078 0.3859 0.151 Uiso 1 1 calc R . . O5 O 1.2405(4) 0.2301(3) 0.3717(9) 0.085(2) Uani 1 1 d . . . C14 C 1.2700(6) 0.2999(5) 0.3775(15) 0.102(4) Uani 1 1 d . . . H14A H 1.2272 0.3239 0.2755 0.152 Uiso 1 1 calc R . . H14B H 1.3454 0.3040 0.3657 0.152 Uiso 1 1 calc R . . H14C H 1.2575 0.3195 0.4952 0.152 Uiso 1 1 calc R . . C1' C 0.7488(5) 0.0947(4) 0.0923(14) 0.060(2) Uani 1 1 d . . . C2' C 0.7413(7) 0.0566(5) 0.2489(16) 0.086(3) Uani 1 1 d . . . H2' H 0.7731 0.0727 0.3662 0.103 Uiso 1 1 calc R . . C3' C 0.6872(7) -0.0054(4) 0.2363(16) 0.093(3) Uani 1 1 d . . . H3' H 0.6808 -0.0312 0.3434 0.111 Uiso 1 1 calc R . . C4' C 0.6412(7) -0.0287(5) 0.0528(19) 0.099(4) Uani 1 1 d . . . H4' H 0.6054 -0.0708 0.0403 0.118 Uiso 1 1 calc R . . C5' C 0.6488(6) 0.0102(5) -0.1078(16) 0.090(3) Uani 1 1 d . . . H5' H 0.6192 -0.0054 -0.2270 0.108 Uiso 1 1 calc R . . C6' C 0.7030(6) 0.0742(4) -0.0834(14) 0.079(3) Uani 1 1 d . . . H6' H 0.7074 0.1022 -0.1870 0.095 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 C1 0.055(5) 0.057(5) 0.047(5) 0.011(4) 0.011(4) 0.001(4) O1 0.067(3) 0.035(3) 0.093(4) 0.006(3) 0.004(3) 0.013(2) C2 0.043(4) 0.058(5) 0.073(6) -0.003(4) -0.008(4) -0.003(4) C3 0.054(4) 0.034(4) 0.038(4) 0.005(3) 0.005(3) -0.004(3) C4 0.035(4) 0.040(4) 0.077(6) -0.012(4) 0.014(4) 0.004(3) C5 0.046(5) 0.041(5) 0.085(6) 0.004(4) 0.018(5) -0.005(3) C6 0.041(5) 0.079(6) 0.080(6) 0.008(5) -0.006(4) 0.016(4) C7 0.042(5) 0.058(5) 0.072(6) 0.004(4) 0.009(4) -0.002(4) C8 0.037(4) 0.052(4) 0.057(5) -0.005(4) 0.011(4) 0.001(4) C9 0.030(4) 0.059(5) 0.063(5) 0.003(4) 0.008(4) 0.006(3) C10 0.031(5) 0.075(6) 0.125(9) 0.009(6) 0.030(5) 0.017(4) O2 0.052(4) 0.067(4) 0.180(7) -0.010(4) 0.006(4) 0.001(3) O3 0.053(4) 0.066(4) 0.222(8) 0.002(4) -0.020(4) 0.035(3) C11A 0.015(11) 0.07(2) 0.16(4) -0.02(2) 0.010(15) 0.022(13) C12A 0.16(4) 0.17(4) 0.07(3) 0.00(3) 0.03(3) 0.10(3) C11B 0.077(13) 0.080(16) 0.21(3) -0.043(18) 0.059(16) -0.016(12) C12B 0.051(11) 0.14(2) 0.15(2) -0.02(2) -0.006(15) 0.018(12) O4 0.046(3) 0.049(3) 0.119(5) 0.000(3) 0.005(3) 0.014(2) C13 0.073(6) 0.083(6) 0.141(10) 0.007(6) 0.003(6) 0.047(5) O5 0.032(3) 0.088(4) 0.132(6) 0.009(4) -0.001(3) -0.015(3) C14 0.045(5) 0.089(7) 0.168(11) -0.016(7) 0.007(6) 0.000(5) C1' 0.034(4) 0.059(5) 0.088(7) -0.007(5) 0.013(5) 0.015(4) C2' 0.088(7) 0.073(6) 0.102(8) 0.011(6) 0.030(6) -0.015(5) C3' 0.083(6) 0.056(6) 0.134(10) 0.022(6) 0.000(7) -0.027(5) C4' 0.051(5) 0.048(5) 0.193(13) 0.002(7) 0.005(7) -0.009(4) C5' 0.059(5) 0.064(6) 0.136(10) -0.007(6) -0.025(6) -0.011(5) C6' 0.061(5) 0.078(6) 0.092(7) -0.003(5) -0.011(5) -0.006(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.193(7) . ? C1 C2 1.494(10) . ? C1 C9 1.512(9) . ? C2 C3 1.384(9) . ? C2 C10 1.483(10) . ? C3 C4 1.439(9) . ? C3 C1' 1.530(10) . ? C4 C5 1.394(9) . ? C4 C9 1.412(9) . ? C5 O4 1.361(7) . ? C5 C6 1.396(9) . ? C6 C7 1.384(9) . ? C6 H6 0.9300 . ? C7 O5 1.353(8) . ? C7 C8 1.355(9) . ? C8 C9 1.387(9) . ? C8 H8 0.9300 . ? C10 O2 1.189(8) . ? C10 O3 1.285(9) . ? O3 C11B 1.525(16) . ? O3 C11A 1.526(15) . ? C11A C12A 1.498(19) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C12A H12A 0.9600 . ? C12A H12B 0.9600 . ? C12A H12C 0.9600 . ? C11B C12B 1.498(17) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C12B H12D 0.9600 . ? C12B H12E 0.9600 . ? C12B H12F 0.9600 . ? O4 C13 1.413(8) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? O5 C14 1.405(9) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C1' C2' 1.360(11) . ? C1' C6' 1.364(11) . ? C2' C3' 1.378(11) . ? C2' H2' 0.9300 . ? C3' C4' 1.429(13) . ? C3' H3' 0.9300 . ? C4' C5' 1.393(13) . ? C4' H4' 0.9300 . ? C5' C6' 1.414(11) . ? C5' H5' 0.9300 . ? C6' H6' 0.9300 . ? 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 O1 C1 C2 130.1(7) . . ? O1 C1 C9 124.8(6) . . ? C2 C1 C9 105.0(6) . . ? C3 C2 C10 126.9(7) . . ? C3 C2 C1 107.8(6) . . ? C10 C2 C1 125.2(7) . . ? C2 C3 C4 111.1(5) . . ? C2 C3 C1' 124.7(6) . . ? C4 C3 C1' 124.2(6) . . ? C5 C4 C9 118.0(6) . . ? C5 C4 C3 133.6(6) . . ? C9 C4 C3 108.4(5) . . ? O4 C5 C4 117.8(6) . . ? O4 C5 C6 124.1(6) . . ? C4 C5 C6 118.0(6) . . ? C7 C6 C5 122.6(6) . . ? C7 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? O5 C7 C8 125.3(7) . . ? O5 C7 C6 114.6(6) . . ? C8 C7 C6 120.0(6) . . ? C7 C8 C9 118.6(6) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C8 C9 C4 122.6(6) . . ? C8 C9 C1 129.7(6) . . ? C4 C9 C1 107.6(5) . . ? O2 C10 O3 120.4(7) . . ? O2 C10 C2 125.1(7) . . ? O3 C10 C2 114.0(7) . . ? C10 O3 C11B 121.7(12) . . ? C10 O3 C11A 109.6(12) . . ? C11B O3 C11A 36.4(16) . . ? C12A C11A O3 98(3) . . ? C12A C11A H11A 112.1 . . ? O3 C11A H11A 112.1 . . ? C12A C11A H11B 112.1 . . ? O3 C11A H11B 112.1 . . ? H11A C11A H11B 109.7 . . ? C12B C11B O3 95.4(17) . . ? C12B C11B H11C 112.7 . . ? O3 C11B H11C 112.7 . . ? C12B C11B H11D 112.7 . . ? O3 C11B H11D 112.7 . . ? H11C C11B H11D 110.2 . . ? C11B C12B H12D 109.5 . . ? C11B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C11B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C5 O4 C13 121.4(6) . . ? O4 C13 H13A 109.5 . . ? O4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 O5 C14 116.8(6) . . ? O5 C14 H14A 109.5 . . ? O5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2' C1' C6' 122.2(8) . . ? C2' C1' C3 118.4(8) . . ? C6' C1' C3 119.3(8) . . ? C1' C2' C3' 121.0(10) . . ? C1' C2' H2' 119.5 . . ? C3' C2' H2' 119.5 . . ? C2' C3' C4' 117.5(10) . . ? C2' C3' H3' 121.2 . . ? C4' C3' H3' 121.2 . . ? C5' C4' C3' 121.6(8) . . ? C5' C4' H4' 119.2 . . ? C3' C4' H4' 119.2 . . ? C4' C5' C6' 117.7(9) . . ? C4' C5' H5' 121.2 . . ? C6' C5' H5' 121.2 . . ? C1' C6' C5' 119.9(9) . . ? C1' C6' H6' 120.0 . . ? C5' C6' H6' 120.0 . . ? 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 -177.7(8) . . . . ? C9 C1 C2 C3 -0.3(9) . . . . ? O1 C1 C2 C10 -2.7(14) . . . . ? C9 C1 C2 C10 174.8(8) . . . . ? C10 C2 C3 C4 -175.0(8) . . . . ? C1 C2 C3 C4 0.0(9) . . . . ? C10 C2 C3 C1' 3.1(13) . . . . ? C1 C2 C3 C1' 178.0(7) . . . . ? C2 C3 C4 C5 -179.3(9) . . . . ? C1' C3 C4 C5 2.6(13) . . . . ? C2 C3 C4 C9 0.4(9) . . . . ? C1' C3 C4 C9 -177.7(8) . . . . ? C9 C4 C5 O4 -179.0(7) . . . . ? C3 C4 C5 O4 0.6(13) . . . . ? C9 C4 C5 C6 1.7(11) . . . . ? C3 C4 C5 C6 -178.7(8) . . . . ? O4 C5 C6 C7 179.1(8) . . . . ? C4 C5 C6 C7 -1.7(12) . . . . ? C5 C6 C7 O5 -179.7(7) . . . . ? C5 C6 C7 C8 3.8(13) . . . . ? O5 C7 C8 C9 178.2(7) . . . . ? C6 C7 C8 C9 -5.8(12) . . . . ? C7 C8 C9 C4 6.0(12) . . . . ? C7 C8 C9 C1 -177.9(8) . . . . ? C5 C4 C9 C8 -4.0(12) . . . . ? C3 C4 C9 C8 176.3(7) . . . . ? C5 C4 C9 C1 179.2(7) . . . . ? C3 C4 C9 C1 -0.5(8) . . . . ? O1 C1 C9 C8 1.6(14) . . . . ? C2 C1 C9 C8 -176.1(8) . . . . ? O1 C1 C9 C4 178.1(8) . . . . ? C2 C1 C9 C4 0.5(9) . . . . ? C3 C2 C10 O2 -7.4(16) . . . . ? C1 C2 C10 O2 178.5(9) . . . . ? C3 C2 C10 O3 -179.2(8) . . . . ? C1 C2 C10 O3 6.7(13) . . . . ? O2 C10 O3 C11B -17.2(17) . . . . ? C2 C10 O3 C11B 155.0(13) . . . . ? O2 C10 O3 C11A 21(2) . . . . ? C2 C10 O3 C11A -167(2) . . . . ? C10 O3 C11A C12A -166(3) . . . . ? C11B O3 C11A C12A -49(3) . . . . ? C10 O3 C11B C12B 124.5(19) . . . . ? C11A O3 C11B C12B 44(3) . . . . ? C4 C5 O4 C13 176.3(7) . . . . ? C6 C5 O4 C13 -4.6(12) . . . . ? C8 C7 O5 C14 -5.8(12) . . . . ? C6 C7 O5 C14 178.0(8) . . . . ? C2 C3 C1' C2' -113.3(9) . . . . ? C4 C3 C1' C2' 64.5(10) . . . . ? C2 C3 C1' C6' 66.3(10) . . . . ? C4 C3 C1' C6' -115.9(8) . . . . ? C6' C1' C2' C3' 0.6(13) . . . . ? C3 C1' C2' C3' -179.8(7) . . . . ? C1' C2' C3' C4' 1.1(13) . . . . ? C2' C3' C4' C5' -1.1(13) . . . . ? C3' C4' C5' C6' -0.5(13) . . . . ? C2' C1' C6' C5' -2.3(12) . . . . ? C3 C1' C6' C5' 178.1(7) . . . . ? C4' C5' C6' C1' 2.2(12) . . . . ? _diffrn_measured_fraction_theta_max 0.834 _diffrn_reflns_theta_full 29.15 _diffrn_measured_fraction_theta_full 0.834 _refine_diff_density_max 0.449 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.085 data_VC1386-T1 _database_code_depnum_ccdc_archive 'CCDC 844782' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_formula_moiety 'C42 H40 O8' _chemical_formula_sum 'C42 H40 O8' _chemical_formula_weight 672.74 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.289(5) _cell_length_b 8.588(5) _cell_length_c 27.715(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.051(5) _cell_angle_gamma 90.00 _cell_volume 7283(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2195 _cell_measurement_theta_min 2.2014 _cell_measurement_theta_max 28.9477 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_T_min 0.98980 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.0827 _diffrn_reflns_number 15980 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.2881 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 29.01 _reflns_number_total 8241 _reflns_number_gt 2081 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0220P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8241 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2308 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 0.624 _refine_ls_restrained_S_all 0.624 _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 0.64294(8) -0.0022(2) 0.07647(9) 0.0432(7) Uani 1 1 d . . . C2 C 0.60048(9) 0.0086(3) 0.09451(10) 0.0439(7) Uani 1 1 d . . . C3 C 0.56981(9) -0.0915(3) 0.07109(9) 0.0460(7) Uani 1 1 d . . . C4 C 0.58848(9) -0.1756(3) 0.03484(10) 0.0463(7) Uani 1 1 d . . . C5 C 0.57046(10) -0.2857(3) -0.00117(11) 0.0562(8) Uani 1 1 d . . . C6 C 0.59686(11) -0.3578(3) -0.02814(10) 0.0656(9) Uani 1 1 d . . . H6 H 0.5852 -0.4323 -0.0516 0.079 Uiso 1 1 calc R . . C7 C 0.64112(11) -0.3200(3) -0.02065(11) 0.0629(9) Uani 1 1 d . . . C8 C 0.65917(9) -0.2048(3) 0.01262(9) 0.0541(7) Uani 1 1 d . . . H8 H 0.6884 -0.1764 0.0168 0.065 Uiso 1 1 calc R . . C9 C 0.63186(9) -0.1347(2) 0.03912(9) 0.0452(7) Uani 1 1 d . . . C10 C 0.59684(10) 0.1172(3) 0.13404(11) 0.0580(8) Uani 1 1 d . . . O1 O 0.62378(6) 0.21509(19) 0.15004(7) 0.0788(6) Uani 1 1 d . . . O2 O 0.56100(7) 0.0996(2) 0.15183(8) 0.1029(8) Uani 1 1 d . A . C11 C 0.55467(12) 0.2026(7) 0.1914(2) 0.1432(18) Uani 1 1 d . . . H11A H 0.5543 0.1379 0.2200 0.172 Uiso 0.490(16) 1 calc PR A 1 H11B H 0.5804 0.2682 0.1997 0.172 Uiso 0.490(16) 1 calc PR A 1 H11C H 0.5747 0.1776 0.2221 0.172 Uiso 0.510(16) 1 calc PR A 2 H11D H 0.5584 0.3108 0.1832 0.172 Uiso 0.510(16) 1 calc PR A 2 C12A C 0.5221(5) 0.2901(16) 0.1859(4) 0.197(8) Uani 0.490(16) 1 d P A 1 H12A H 0.5183 0.3258 0.2175 0.295 Uiso 0.490(16) 1 calc PR A 1 H12B H 0.4965 0.2338 0.1699 0.295 Uiso 0.490(16) 1 calc PR A 1 H12C H 0.5264 0.3778 0.1659 0.295 Uiso 0.490(16) 1 calc PR A 1 C12B C 0.5105(5) 0.170(2) 0.1941(5) 0.252(9) Uani 0.510(16) 1 d P A 2 H12D H 0.5085 0.1595 0.2281 0.378 Uiso 0.510(16) 1 calc PR A 2 H12E H 0.5012 0.0757 0.1767 0.378 Uiso 0.510(16) 1 calc PR A 2 H12F H 0.4921 0.2546 0.1795 0.378 Uiso 0.510(16) 1 calc PR A 2 O3 O 0.52661(7) -0.31287(18) -0.00683(7) 0.0750(6) Uani 1 1 d . . . C13 C 0.50482(9) -0.3982(3) -0.04985(10) 0.1150(13) Uani 1 1 d . . . H13A H 0.4740 -0.4013 -0.0507 0.172 Uiso 1 1 calc R . . H13B H 0.5161 -0.5025 -0.0484 0.172 Uiso 1 1 calc R . . H13C H 0.5099 -0.3476 -0.0790 0.172 Uiso 1 1 calc R . . O4 O 0.66374(7) -0.40212(19) -0.04966(7) 0.0795(6) Uani 1 1 d . . . C14 C 0.71028(10) -0.3875(3) -0.03941(10) 0.0887(10) Uani 1 1 d . . . H14A H 0.7221 -0.4554 -0.0608 0.133 Uiso 1 1 calc R . . H14B H 0.7219 -0.4155 -0.0057 0.133 Uiso 1 1 calc R . . H14C H 0.7181 -0.2819 -0.0449 0.133 Uiso 1 1 calc R . . C15 C 0.65056(8) 0.1530(2) 0.04871(9) 0.0575(8) Uani 1 1 d . . . H150 H 0.6361 0.1423 0.0143 0.069 Uiso 1 1 calc R . . H150 H 0.6363 0.2375 0.0624 0.069 Uiso 1 1 calc R . . C16 C 0.69830(8) 0.2001(2) 0.05076(9) 0.0566(8) Uani 1 1 d . . . H16A H 0.7127 0.1229 0.0342 0.068 Uiso 1 1 calc R . . H16B H 0.6995 0.2998 0.0347 0.068 Uiso 1 1 calc R . . C17 C 0.72059(8) 0.2108(2) 0.10523(9) 0.0439(7) Uani 1 1 d . . . H17 H 0.7033 0.2842 0.1204 0.053 Uiso 1 1 calc R . . C18 C 0.76766(8) 0.2532(3) 0.12396(9) 0.0443(7) Uani 1 1 d . . . C19 C 0.78717(8) 0.1479(3) 0.15769(9) 0.0434(7) Uani 1 1 d . . . C20 C 0.75617(8) 0.0223(2) 0.16104(9) 0.0390(7) Uani 1 1 d . . . C21 C 0.75901(9) -0.1169(3) 0.18695(9) 0.0465(7) Uani 1 1 d . . . C22 C 0.72348(9) -0.2181(2) 0.17814(9) 0.0488(7) Uani 1 1 d . . . H22 H 0.7249 -0.3108 0.1957 0.059 Uiso 1 1 calc R . . C23 C 0.68581(8) -0.1818(3) 0.14314(9) 0.0451(7) Uani 1 1 d . . . C24 C 0.68155(8) -0.0412(2) 0.11699(9) 0.0397(7) Uani 1 1 d . . . C25 C 0.71706(8) 0.0568(2) 0.12887(9) 0.0367(6) Uani 1 1 d . . . C26 C 0.78423(10) 0.4022(3) 0.10888(11) 0.0601(8) Uani 1 1 d . . . O5 O 0.76368(7) 0.4888(2) 0.07959(8) 0.1052(9) Uani 1 1 d . . . O6 O 0.82484(6) 0.43333(18) 0.13296(7) 0.0769(6) Uani 1 1 d . . . C27 C 0.84369(9) 0.5802(3) 0.12253(11) 0.0868(10) Uani 1 1 d . . . H27A H 0.8229 0.6638 0.1228 0.104 Uiso 1 1 calc R . . H27B H 0.8508 0.5768 0.0901 0.104 Uiso 1 1 calc R . . C28 C 0.88343(9) 0.6088(3) 0.16020(11) 0.1024(11) Uani 1 1 d . . . H28A H 0.8975 0.7017 0.1521 0.154 Uiso 1 1 calc R . . H28B H 0.9030 0.5221 0.1614 0.154 Uiso 1 1 calc R . . H28C H 0.8758 0.6213 0.1918 0.154 Uiso 1 1 calc R . . O7 O 0.79690(6) -0.14739(19) 0.22014(7) 0.0686(6) Uani 1 1 d . . . C29 C 0.79912(8) -0.2839(3) 0.24913(10) 0.0972(11) Uani 1 1 d . . . H29A H 0.8268 -0.2879 0.2719 0.146 Uiso 1 1 calc R . . H29B H 0.7960 -0.3737 0.2281 0.146 Uiso 1 1 calc R . . H29C H 0.7760 -0.2827 0.2671 0.146 Uiso 1 1 calc R . . O8 O 0.65038(5) -0.27756(16) 0.13367(6) 0.0582(5) Uani 1 1 d . . . C30 C 0.65610(8) -0.4396(2) 0.14451(11) 0.1007(12) Uani 1 1 d . . . H30A H 0.6297 -0.4943 0.1306 0.151 Uiso 1 1 calc R . . H30B H 0.6629 -0.4543 0.1796 0.151 Uiso 1 1 calc R . . H30C H 0.6796 -0.4791 0.1306 0.151 Uiso 1 1 calc R . . C1' C 0.52654(9) -0.1269(3) 0.08256(10) 0.0497(7) Uani 1 1 d . . . C2' C 0.52427(10) -0.2442(3) 0.11549(11) 0.0670(9) Uani 1 1 d . . . H2' H 0.5494 -0.2995 0.1295 0.080 Uiso 1 1 calc R . . C3' C 0.48514(12) -0.2811(3) 0.12810(11) 0.0837(10) Uani 1 1 d . . . H3' H 0.4843 -0.3592 0.1511 0.100 Uiso 1 1 calc R . . C4' C 0.44768(11) -0.2043(4) 0.10716(13) 0.0858(10) Uani 1 1 d . . . H4' H 0.4213 -0.2304 0.1156 0.103 Uiso 1 1 calc R . . C5' C 0.44931(10) -0.0887(4) 0.07371(12) 0.0853(10) Uani 1 1 d . . . H5' H 0.4239 -0.0367 0.0589 0.102 Uiso 1 1 calc R . . C6' C 0.48881(11) -0.0486(3) 0.06172(10) 0.0717(9) Uani 1 1 d . . . H6' H 0.4898 0.0317 0.0395 0.086 Uiso 1 1 calc R . . C1" C 0.83265(9) 0.1510(3) 0.18736(10) 0.0470(7) Uani 1 1 d . . . C2" C 0.86414(10) 0.0558(3) 0.17518(11) 0.0692(9) Uani 1 1 d . . . H2" H 0.8569 -0.0100 0.1480 0.083 Uiso 1 1 calc R . . C3" C 0.90624(11) 0.0568(4) 0.20265(14) 0.0910(11) Uani 1 1 d . . . H3" H 0.9271 -0.0091 0.1941 0.109 Uiso 1 1 calc R . . C4" C 0.91757(11) 0.1531(4) 0.24211(14) 0.0959(12) Uani 1 1 d . . . H4" H 0.9461 0.1541 0.2603 0.115 Uiso 1 1 calc R . . C5" C 0.88678(12) 0.2491(4) 0.25511(12) 0.0913(11) Uani 1 1 d . . . H5" H 0.8944 0.3151 0.2821 0.110 Uiso 1 1 calc R . . C6" C 0.84408(10) 0.2469(3) 0.22759(11) 0.0719(9) Uani 1 1 d . . . H6" H 0.8231 0.3112 0.2366 0.086 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 C1 0.0411(19) 0.0424(15) 0.0434(18) -0.0083(14) 0.0027(16) -0.0015(13) C2 0.045(2) 0.0373(15) 0.0453(18) -0.0069(14) 0.0007(16) 0.0044(14) C3 0.047(2) 0.0427(16) 0.047(2) -0.0005(14) 0.0078(17) 0.0009(15) C4 0.050(2) 0.0423(16) 0.0441(19) -0.0060(14) 0.0054(17) -0.0118(15) C5 0.057(2) 0.0575(19) 0.053(2) -0.0050(16) 0.010(2) -0.0168(18) C6 0.085(3) 0.0629(19) 0.050(2) -0.0201(15) 0.017(2) -0.0221(19) C7 0.089(3) 0.0532(19) 0.052(2) -0.0072(16) 0.027(2) 0.0017(19) C8 0.061(2) 0.0487(16) 0.053(2) -0.0094(15) 0.0132(17) -0.0055(16) C9 0.054(2) 0.0401(15) 0.0410(18) -0.0019(14) 0.0076(16) -0.0006(15) C10 0.043(2) 0.066(2) 0.061(2) -0.0138(18) 0.0035(19) 0.0051(17) O1 0.0697(15) 0.0763(13) 0.0883(17) -0.0397(11) 0.0113(13) -0.0104(11) O2 0.0761(18) 0.1307(18) 0.112(2) -0.0737(15) 0.0439(15) -0.0249(14) C11 0.105(4) 0.181(4) 0.156(4) -0.114(4) 0.055(4) -0.012(4) C12A 0.256(16) 0.168(10) 0.117(8) -0.053(7) -0.074(9) 0.153(11) C12B 0.195(14) 0.326(18) 0.305(16) -0.237(13) 0.212(12) -0.097(11) O3 0.0746(16) 0.0793(12) 0.0679(15) -0.0219(10) 0.0078(13) -0.0284(12) C13 0.124(3) 0.136(3) 0.073(3) -0.031(2) -0.004(2) -0.070(2) O4 0.0975(18) 0.0812(13) 0.0648(16) -0.0259(11) 0.0283(15) -0.0011(13) C14 0.098(3) 0.098(2) 0.071(3) -0.0115(18) 0.021(2) 0.037(2) C15 0.059(2) 0.0499(16) 0.055(2) 0.0020(14) -0.0079(16) -0.0013(14) C16 0.065(2) 0.0517(15) 0.048(2) 0.0086(13) -0.0007(18) -0.0067(15) C17 0.0459(19) 0.0387(15) 0.0448(18) -0.0020(13) 0.0041(15) 0.0024(13) C18 0.0463(19) 0.0419(16) 0.0435(18) 0.0042(14) 0.0069(15) -0.0064(14) C19 0.0441(19) 0.0495(16) 0.0366(17) -0.0008(14) 0.0080(15) -0.0020(15) C20 0.046(2) 0.0372(15) 0.0336(17) 0.0050(13) 0.0071(15) 0.0034(15) C21 0.045(2) 0.0578(18) 0.0354(18) 0.0053(15) 0.0056(16) 0.0095(16) C22 0.049(2) 0.0424(15) 0.053(2) 0.0149(14) 0.0073(17) 0.0006(15) C23 0.047(2) 0.0397(16) 0.0490(19) -0.0060(14) 0.0121(16) -0.0049(14) C24 0.0441(19) 0.0301(14) 0.0437(18) -0.0035(13) 0.0062(15) 0.0000(14) C25 0.0439(19) 0.0328(15) 0.0353(17) -0.0017(13) 0.0128(15) 0.0036(13) C26 0.051(2) 0.064(2) 0.059(2) 0.0066(17) -0.0044(18) -0.0177(17) O5 0.0895(18) 0.0790(13) 0.121(2) 0.0530(13) -0.0370(15) -0.0251(12) O6 0.0622(14) 0.0670(12) 0.0908(17) 0.0294(11) -0.0084(13) -0.0213(11) C27 0.074(3) 0.075(2) 0.107(3) 0.0319(19) 0.008(2) -0.0313(18) C28 0.082(3) 0.092(2) 0.128(3) -0.012(2) 0.011(2) -0.0322(19) O7 0.0545(14) 0.0793(12) 0.0652(14) 0.0330(11) -0.0030(12) 0.0001(10) C29 0.072(2) 0.115(2) 0.090(3) 0.061(2) -0.0158(19) 0.0032(19) O8 0.0552(13) 0.0399(10) 0.0767(14) 0.0046(9) 0.0073(10) -0.0126(9) C30 0.091(3) 0.0369(16) 0.167(3) 0.0003(17) 0.012(2) -0.0112(16) C1' 0.057(2) 0.0476(17) 0.044(2) -0.0038(15) 0.0100(17) -0.0075(16) C2' 0.054(2) 0.068(2) 0.077(2) -0.0007(18) 0.0100(19) -0.0013(17) C3' 0.083(3) 0.080(2) 0.094(3) 0.0135(19) 0.034(3) -0.004(2) C4' 0.069(3) 0.107(3) 0.089(3) -0.002(2) 0.034(2) -0.018(2) C5' 0.052(3) 0.125(3) 0.078(3) 0.007(2) 0.013(2) 0.007(2) C6' 0.064(2) 0.082(2) 0.070(2) 0.0160(17) 0.016(2) 0.011(2) C1" 0.047(2) 0.0498(17) 0.043(2) 0.0075(14) 0.0058(17) -0.0019(15) C2" 0.050(2) 0.077(2) 0.076(3) -0.0024(17) 0.002(2) 0.0011(18) C3" 0.061(3) 0.100(3) 0.109(3) 0.012(2) 0.011(3) 0.005(2) C4" 0.055(3) 0.125(3) 0.094(3) 0.021(2) -0.014(2) -0.016(2) C5" 0.090(3) 0.109(3) 0.064(3) -0.002(2) -0.009(3) -0.024(2) C6" 0.060(2) 0.095(2) 0.056(2) -0.0036(19) 0.0024(19) -0.0046(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C24 1.505(3) . ? C1 C2 1.517(3) . ? C1 C9 1.528(3) . ? C1 C15 1.582(3) . ? C2 C3 1.349(3) . ? C2 C10 1.461(3) . ? C3 C4 1.455(3) . ? C3 C1' 1.485(3) . ? C4 C9 1.383(3) . ? C4 C5 1.405(3) . ? C5 O3 1.368(3) . ? C5 C6 1.372(3) . ? C6 C7 1.395(3) . ? C6 H6 0.9300 . ? C7 O4 1.372(3) . ? C7 C8 1.389(3) . ? C8 C9 1.376(3) . ? C8 H8 0.9300 . ? C10 O1 1.207(3) . ? C10 O2 1.325(3) . ? O2 C11 1.454(3) . ? C11 C12A 1.250(10) . ? C11 C12B 1.427(12) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C11 H11D 0.9700 . ? C12A H12A 0.9600 . ? C12A H12B 0.9600 . ? C12A H12C 0.9600 . ? C12B H12D 0.9600 . ? C12B H12E 0.9600 . ? C12B H12F 0.9600 . ? O3 C13 1.444(3) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? O4 C14 1.430(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.537(3) . ? C15 H150 0.9700 . ? C15 H150 0.9700 . ? C16 C17 1.528(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C25 1.490(3) . ? C17 C18 1.501(3) . ? C17 H17 0.9800 . ? C18 C19 1.351(3) . ? C18 C26 1.473(3) . ? C19 C20 1.466(3) . ? C19 C1" 1.488(3) . ? C20 C21 1.388(3) . ? C20 C25 1.387(3) . ? C21 O7 1.365(2) . ? C21 C22 1.392(3) . ? C22 C23 1.397(3) . ? C22 H22 0.9300 . ? C23 O8 1.361(2) . ? C23 C24 1.400(3) . ? C24 C25 1.378(3) . ? C26 O5 1.187(3) . ? C26 O6 1.333(3) . ? O6 C27 1.447(2) . ? C27 C28 1.468(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? O7 C29 1.415(2) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? O8 C30 1.427(2) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C1' C2' 1.371(3) . ? C1' C6' 1.377(3) . ? C2' C3' 1.379(3) . ? C2' H2' 0.9300 . ? C3' C4' 1.364(3) . ? C3' H3' 0.9300 . ? C4' C5' 1.367(3) . ? C4' H4' 0.9300 . ? C5' C6' 1.389(3) . ? C5' H5' 0.9300 . ? C6' H6' 0.9300 . ? C1" C6" 1.373(3) . ? C1" C2" 1.375(3) . ? C2" C3" 1.377(3) . ? C2" H2" 0.9300 . ? C3" C4" 1.358(4) . ? C3" H3" 0.9300 . ? C4" C5" 1.372(4) . ? C4" H4" 0.9300 . ? C5" C6" 1.393(3) . ? C5" H5" 0.9300 . ? C6" H6" 0.9300 . ? 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 C24 C1 C2 112.9(2) . . ? C24 C1 C9 111.92(19) . . ? C2 C1 C9 100.3(2) . . ? C24 C1 C15 111.78(19) . . ? C2 C1 C15 109.87(19) . . ? C9 C1 C15 109.5(2) . . ? C3 C2 C10 127.5(3) . . ? C3 C2 C1 112.7(2) . . ? C10 C2 C1 119.8(2) . . ? C2 C3 C4 107.5(2) . . ? C2 C3 C1' 128.0(2) . . ? C4 C3 C1' 124.1(2) . . ? C9 C4 C5 118.2(3) . . ? C9 C4 C3 110.1(2) . . ? C5 C4 C3 131.7(3) . . ? O3 C5 C6 124.3(3) . . ? O3 C5 C4 116.1(3) . . ? C6 C5 C4 119.5(3) . . ? C5 C6 C7 120.4(3) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? O4 C7 C8 124.5(3) . . ? O4 C7 C6 114.2(3) . . ? C8 C7 C6 121.2(3) . . ? C9 C8 C7 117.0(3) . . ? C9 C8 H8 121.5 . . ? C7 C8 H8 121.5 . . ? C8 C9 C4 123.4(2) . . ? C8 C9 C1 127.5(3) . . ? C4 C9 C1 109.1(2) . . ? O1 C10 O2 121.5(3) . . ? O1 C10 C2 124.2(3) . . ? O2 C10 C2 114.3(3) . . ? C10 O2 C11 118.1(3) . . ? C12A C11 C12B 49.3(7) . . ? C12A C11 O2 120.6(7) . . ? C12B C11 O2 102.0(5) . . ? C12A C11 H11A 107.2 . . ? C12B C11 H11A 70.6 . . ? O2 C11 H11A 107.2 . . ? C12A C11 H11B 107.2 . . ? C12B C11 H11B 149.8 . . ? O2 C11 H11B 107.2 . . ? H11A C11 H11B 106.8 . . ? C12A C11 H11C 126.9 . . ? C12B C11 H11C 111.4 . . ? O2 C11 H11C 111.4 . . ? H11A C11 H11C 43.2 . . ? H11B C11 H11C 64.5 . . ? C12A C11 H11D 62.0 . . ? C12B C11 H11D 111.4 . . ? O2 C11 H11D 111.4 . . ? H11A C11 H11D 139.7 . . ? H11B C11 H11D 50.5 . . ? H11C C11 H11D 109.2 . . ? C11 C12A H12A 109.5 . . ? C11 C12A H12B 109.5 . . ? C11 C12A H12C 109.5 . . ? C11 C12B H12D 109.5 . . ? C11 C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C11 C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C5 O3 C13 118.1(2) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 O4 C14 117.9(2) . . ? O4 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C1 116.60(19) . . ? C16 C15 H150 108.1 . . ? C1 C15 H150 108.1 . . ? C16 C15 H150 108.1 . . ? C1 C15 H150 108.1 . . ? H150 C15 H150 107.3 . . ? C17 C16 C15 107.0(2) . . ? C17 C16 H16A 110.3 . . ? C15 C16 H16A 110.3 . . ? C17 C16 H16B 110.3 . . ? C15 C16 H16B 110.3 . . ? H16A C16 H16B 108.6 . . ? C25 C17 C18 102.75(19) . . ? C25 C17 C16 108.71(18) . . ? C18 C17 C16 124.7(2) . . ? C25 C17 H17 106.5 . . ? C18 C17 H17 106.5 . . ? C16 C17 H17 106.5 . . ? C19 C18 C26 130.0(2) . . ? C19 C18 C17 110.2(2) . . ? C26 C18 C17 119.4(2) . . ? C18 C19 C20 109.1(2) . . ? C18 C19 C1" 127.8(2) . . ? C20 C19 C1" 123.2(2) . . ? C21 C20 C25 118.0(2) . . ? C21 C20 C19 134.0(2) . . ? C25 C20 C19 108.0(2) . . ? O7 C21 C20 117.8(2) . . ? O7 C21 C22 123.2(2) . . ? C20 C21 C22 119.0(2) . . ? C21 C22 C23 120.7(2) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? O8 C23 C22 122.3(2) . . ? O8 C23 C24 115.8(2) . . ? C22 C23 C24 121.8(2) . . ? C25 C24 C23 114.7(2) . . ? C25 C24 C1 121.6(2) . . ? C23 C24 C1 123.5(2) . . ? C24 C25 C20 125.6(2) . . ? C24 C25 C17 124.6(2) . . ? C20 C25 C17 109.6(2) . . ? O5 C26 O6 122.7(3) . . ? O5 C26 C18 124.5(3) . . ? O6 C26 C18 112.8(2) . . ? C26 O6 C27 117.4(2) . . ? O6 C27 C28 108.9(2) . . ? O6 C27 H27A 109.9 . . ? C28 C27 H27A 109.9 . . ? O6 C27 H27B 109.9 . . ? C28 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C21 O7 C29 118.31(19) . . ? O7 C29 H29A 109.5 . . ? O7 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O7 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C23 O8 C30 119.16(19) . . ? O8 C30 H30A 109.5 . . ? O8 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O8 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C2' C1' C6' 118.6(3) . . ? C2' C1' C3 118.0(3) . . ? C6' C1' C3 123.4(3) . . ? C1' C2' C3' 120.6(3) . . ? C1' C2' H2' 119.7 . . ? C3' C2' H2' 119.7 . . ? C4' C3' C2' 120.7(3) . . ? C4' C3' H3' 119.6 . . ? C2' C3' H3' 119.6 . . ? C3' C4' C5' 119.3(3) . . ? C3' C4' H4' 120.4 . . ? C5' C4' H4' 120.4 . . ? C4' C5' C6' 120.3(3) . . ? C4' C5' H5' 119.9 . . ? C6' C5' H5' 119.9 . . ? C1' C6' C5' 120.4(3) . . ? C1' C6' H6' 119.8 . . ? C5' C6' H6' 119.8 . . ? C6" C1" C2" 118.5(3) . . ? C6" C1" C19 121.1(3) . . ? C2" C1" C19 120.4(3) . . ? C1" C2" C3" 120.8(3) . . ? C1" C2" H2" 119.6 . . ? C3" C2" H2" 119.6 . . ? C4" C3" C2" 120.5(3) . . ? C4" C3" H3" 119.7 . . ? C2" C3" H3" 119.7 . . ? C3" C4" C5" 119.9(3) . . ? C3" C4" H4" 120.1 . . ? C5" C4" H4" 120.1 . . ? C4" C5" C6" 119.6(3) . . ? C4" C5" H5" 120.2 . . ? C6" C5" H5" 120.2 . . ? C1" C6" C5" 120.7(3) . . ? C1" C6" H6" 119.7 . . ? C5" C6" H6" 119.7 . . ? 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 C24 C1 C2 C3 -121.7(2) . . . . ? C9 C1 C2 C3 -2.5(3) . . . . ? C15 C1 C2 C3 112.8(2) . . . . ? C24 C1 C2 C10 57.0(3) . . . . ? C9 C1 C2 C10 176.3(2) . . . . ? C15 C1 C2 C10 -68.5(3) . . . . ? C10 C2 C3 C4 -179.7(2) . . . . ? C1 C2 C3 C4 -1.1(3) . . . . ? C10 C2 C3 C1' -6.2(4) . . . . ? C1 C2 C3 C1' 172.4(2) . . . . ? C2 C3 C4 C9 4.7(3) . . . . ? C1' C3 C4 C9 -169.0(2) . . . . ? C2 C3 C4 C5 -175.9(2) . . . . ? C1' C3 C4 C5 10.3(4) . . . . ? C9 C4 C5 O3 -174.7(2) . . . . ? C3 C4 C5 O3 5.9(4) . . . . ? C9 C4 C5 C6 5.0(4) . . . . ? C3 C4 C5 C6 -174.3(2) . . . . ? O3 C5 C6 C7 178.4(2) . . . . ? C4 C5 C6 C7 -1.3(4) . . . . ? C5 C6 C7 O4 179.3(2) . . . . ? C5 C6 C7 C8 -2.6(4) . . . . ? O4 C7 C8 C9 -179.5(2) . . . . ? C6 C7 C8 C9 2.6(4) . . . . ? C7 C8 C9 C4 1.4(4) . . . . ? C7 C8 C9 C1 -177.8(2) . . . . ? C5 C4 C9 C8 -5.2(4) . . . . ? C3 C4 C9 C8 174.3(2) . . . . ? C5 C4 C9 C1 174.1(2) . . . . ? C3 C4 C9 C1 -6.4(3) . . . . ? C24 C1 C9 C8 -55.5(3) . . . . ? C2 C1 C9 C8 -175.4(2) . . . . ? C15 C1 C9 C8 69.0(3) . . . . ? C24 C1 C9 C4 125.2(2) . . . . ? C2 C1 C9 C4 5.3(2) . . . . ? C15 C1 C9 C4 -110.2(2) . . . . ? C3 C2 C10 O1 -172.0(3) . . . . ? C1 C2 C10 O1 9.5(4) . . . . ? C3 C2 C10 O2 8.4(4) . . . . ? C1 C2 C10 O2 -170.1(2) . . . . ? O1 C10 O2 C11 0.3(5) . . . . ? C2 C10 O2 C11 179.9(3) . . . . ? C10 O2 C11 C12A 119.9(12) . . . . ? C10 O2 C11 C12B 169.5(10) . . . . ? C6 C5 O3 C13 -12.8(4) . . . . ? C4 C5 O3 C13 166.9(2) . . . . ? C8 C7 O4 C14 11.0(4) . . . . ? C6 C7 O4 C14 -171.0(2) . . . . ? C24 C1 C15 C16 24.2(3) . . . . ? C2 C1 C15 C16 150.3(2) . . . . ? C9 C1 C15 C16 -100.4(2) . . . . ? C1 C15 C16 C17 -56.1(3) . . . . ? C15 C16 C17 C25 58.6(2) . . . . ? C15 C16 C17 C18 179.80(19) . . . . ? C25 C17 C18 C19 -6.0(3) . . . . ? C16 C17 C18 C19 -129.8(2) . . . . ? C25 C17 C18 C26 -179.4(2) . . . . ? C16 C17 C18 C26 56.8(3) . . . . ? C26 C18 C19 C20 177.0(2) . . . . ? C17 C18 C19 C20 4.5(3) . . . . ? C26 C18 C19 C1" -3.7(4) . . . . ? C17 C18 C19 C1" -176.2(2) . . . . ? C18 C19 C20 C21 176.1(3) . . . . ? C1" C19 C20 C21 -3.3(4) . . . . ? C18 C19 C20 C25 -1.1(3) . . . . ? C1" C19 C20 C25 179.6(2) . . . . ? C25 C20 C21 O7 -177.2(2) . . . . ? C19 C20 C21 O7 5.8(4) . . . . ? C25 C20 C21 C22 2.6(3) . . . . ? C19 C20 C21 C22 -174.3(2) . . . . ? O7 C21 C22 C23 -179.0(2) . . . . ? C20 C21 C22 C23 1.2(4) . . . . ? C21 C22 C23 O8 -179.7(2) . . . . ? C21 C22 C23 C24 -2.3(4) . . . . ? O8 C23 C24 C25 177.15(19) . . . . ? C22 C23 C24 C25 -0.4(3) . . . . ? O8 C23 C24 C1 -7.0(3) . . . . ? C22 C23 C24 C1 175.5(2) . . . . ? C2 C1 C24 C25 -120.5(2) . . . . ? C9 C1 C24 C25 127.3(2) . . . . ? C15 C1 C24 C25 4.0(3) . . . . ? C2 C1 C24 C23 63.9(3) . . . . ? C9 C1 C24 C23 -48.3(3) . . . . ? C15 C1 C24 C23 -171.6(2) . . . . ? C23 C24 C25 C20 4.6(4) . . . . ? C1 C24 C25 C20 -171.4(2) . . . . ? C23 C24 C25 C17 178.5(2) . . . . ? C1 C24 C25 C17 2.5(4) . . . . ? C21 C20 C25 C24 -5.8(4) . . . . ? C19 C20 C25 C24 171.8(2) . . . . ? C21 C20 C25 C17 179.5(2) . . . . ? C19 C20 C25 C17 -2.8(3) . . . . ? C18 C17 C25 C24 -169.5(2) . . . . ? C16 C17 C25 C24 -35.7(3) . . . . ? C18 C17 C25 C20 5.2(3) . . . . ? C16 C17 C25 C20 139.1(2) . . . . ? C19 C18 C26 O5 -177.7(3) . . . . ? C17 C18 C26 O5 -5.8(4) . . . . ? C19 C18 C26 O6 0.2(4) . . . . ? C17 C18 C26 O6 172.1(2) . . . . ? O5 C26 O6 C27 0.5(4) . . . . ? C18 C26 O6 C27 -177.4(2) . . . . ? C26 O6 C27 C28 166.9(2) . . . . ? C20 C21 O7 C29 175.8(2) . . . . ? C22 C21 O7 C29 -4.0(4) . . . . ? C22 C23 O8 C30 -23.9(3) . . . . ? C24 C23 O8 C30 158.6(2) . . . . ? C2 C3 C1' C2' -89.1(3) . . . . ? C4 C3 C1' C2' 83.4(3) . . . . ? C2 C3 C1' C6' 91.1(3) . . . . ? C4 C3 C1' C6' -96.4(3) . . . . ? C6' C1' C2' C3' -1.1(4) . . . . ? C3 C1' C2' C3' 179.1(2) . . . . ? C1' C2' C3' C4' 1.7(5) . . . . ? C2' C3' C4' C5' -0.6(5) . . . . ? C3' C4' C5' C6' -0.9(5) . . . . ? C2' C1' C6' C5' -0.4(4) . . . . ? C3 C1' C6' C5' 179.3(3) . . . . ? C4' C5' C6' C1' 1.4(5) . . . . ? C18 C19 C1" C6" 77.0(4) . . . . ? C20 C19 C1" C6" -103.8(3) . . . . ? C18 C19 C1" C2" -103.7(3) . . . . ? C20 C19 C1" C2" 75.5(3) . . . . ? C6" C1" C2" C3" -0.1(4) . . . . ? C19 C1" C2" C3" -179.4(2) . . . . ? C1" C2" C3" C4" -0.7(5) . . . . ? C2" C3" C4" C5" 0.8(5) . . . . ? C3" C4" C5" C6" -0.1(5) . . . . ? C2" C1" C6" C5" 0.7(4) . . . . ? C19 C1" C6" C5" -179.9(2) . . . . ? C4" C5" C6" C1" -0.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.849 _diffrn_reflns_theta_full 29.01 _diffrn_measured_fraction_theta_full 0.849 _refine_diff_density_max 0.133 _refine_diff_density_min -0.147 _refine_diff_density_rms 0.028 data_vc1386bis _database_code_depnum_ccdc_archive 'CCDC 844783' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C41.59 H38.77 O8, 0.5(C1.18 H4.71 O1.18), 0.41(C H4 O), C0.41 H1.23' _chemical_formula_sum 'C43 H44 O9' _chemical_formula_weight 704.78 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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3555(6) _cell_length_b 13.2852(7) _cell_length_c 15.0996(8) _cell_angle_alpha 114.224(5) _cell_angle_beta 98.647(4) _cell_angle_gamma 107.133(4) _cell_volume 1886.58(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3650 _cell_measurement_theta_min 2.4420 _cell_measurement_theta_max 29.1448 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_T_min 0.99721 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.0827 _diffrn_reflns_number 14407 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.1143 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 29.21 _reflns_number_total 8500 _reflns_number_gt 3250 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0768P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8500 _refine_ls_number_parameters 519 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1482 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1524 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 0.802 _refine_ls_restrained_S_all 0.836 _refine_ls_shift/su_max 0.138 _refine_ls_shift/su_mean 0.018 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 0.8611(2) 0.3210(2) 0.22148(18) 0.0440(6) Uani 1 1 d . . . C2 C 0.9291(3) 0.2749(2) 0.28101(19) 0.0531(7) Uani 1 1 d . A . C3 C 0.8926(3) 0.2885(2) 0.36518(19) 0.0485(7) Uani 1 1 d . . . C4 C 0.7944(2) 0.3398(2) 0.36720(18) 0.0436(6) Uani 1 1 d . . . C5 C 0.7267(2) 0.3731(2) 0.43803(18) 0.0478(6) Uani 1 1 d . . . C6 C 0.6312(3) 0.4108(2) 0.4159(2) 0.0549(7) Uani 1 1 d . . . H6 H 0.5862 0.4337 0.4621 0.066 Uiso 1 1 calc R . . C7 C 0.6008(3) 0.4152(2) 0.3246(2) 0.0520(7) Uani 1 1 d . . . C8 C 0.6700(2) 0.3876(2) 0.25707(18) 0.0473(6) Uani 1 1 d . . . H8 H 0.6514 0.3928 0.1973 0.057 Uiso 1 1 calc R . . C9 C 0.7678(2) 0.3522(2) 0.28050(17) 0.0423(6) Uani 1 1 d . . . C10 C 1.0228(4) 0.2236(3) 0.2474(2) 0.0931(12) Uani 1 1 d . . . O1 O 1.0534(2) 0.2207(2) 0.17190(16) 0.0835(7) Uani 1 1 d . A . O2A O 1.1081(5) 0.2262(5) 0.3219(3) 0.0826(14) Uani 0.589(4) 1 d P A 1 C11A C 1.2157(5) 0.1924(6) 0.3036(4) 0.086(2) Uani 0.589(4) 1 d PD A 1 H11A H 1.2765 0.2488 0.2901 0.103 Uiso 0.589(4) 1 calc PR A 1 H11B H 1.1855 0.1125 0.2459 0.103 Uiso 0.589(4) 1 calc PR A 1 C12A C 1.2782(11) 0.1960(14) 0.4014(8) 0.193(6) Uani 0.589(4) 1 d PD A 1 H12A H 1.2692 0.2577 0.4584 0.289 Uiso 0.589(4) 1 calc PR A 1 H12B H 1.3686 0.2128 0.4097 0.289 Uiso 0.589(4) 1 calc PR A 1 H12C H 1.2366 0.1197 0.3980 0.289 Uiso 0.589(4) 1 calc PR A 1 C1M C 0.3812(16) -0.001(3) 0.446(2) 0.382(13) Uani 0.589(4) 1 d PDU A 1 H1M1 H 0.4012 0.0391 0.4066 0.574 Uiso 0.589(4) 1 calc PR A 1 H1M2 H 0.3437 0.0402 0.4949 0.574 Uiso 0.589(4) 1 calc PR A 1 H1M3 H 0.3207 -0.0823 0.4017 0.574 Uiso 0.589(4) 1 calc PR A 1 O1M O 0.5000 0.0000 0.5000 0.511(11) Uani 0.178(8) 2 d SPDU . 1 H1M H 0.5595 0.0253 0.4839 0.766 Uiso 0.589(4) 1 d PR A 1 O2B O 1.0151(8) 0.1276(7) 0.2678(5) 0.085(2) Uani 0.411(4) 1 d P A 2 C11B C 1.0972(7) 0.1297(7) 0.1100(6) 0.098(3) Uani 0.411(4) 1 d PD A 2 H11C H 1.1324 0.1021 0.1540 0.118 Uiso 0.411(4) 1 d PR A 2 H11D H 1.1696 0.1685 0.0924 0.118 Uiso 0.411(4) 1 d PR A 2 C12B C 1.0000 0.0000 0.0000 0.171(4) Uani 0.822(8) 2 d SPD . 2 H12D H 0.9130 -0.0265 0.0029 0.256 Uiso 0.411(4) 1 d PR A 2 H12E H 1.0326 -0.0612 -0.0082 0.256 Uiso 0.411(4) 1 d PR A 2 H12F H 1.0003 0.0153 -0.0569 0.256 Uiso 0.411(4) 1 d PR A 2 C2M C 1.2899(13) 0.1461(18) 0.4178(11) 0.180(8) Uani 0.411(4) 1 d PDU A 2 H2M1 H 1.3168 0.2314 0.4453 0.270 Uiso 0.411(4) 1 calc PR A 2 H2M2 H 1.2110 0.1142 0.4310 0.270 Uiso 0.411(4) 1 calc PR A 2 H2M3 H 1.2756 0.1094 0.3454 0.270 Uiso 0.411(4) 1 calc PR A 2 O2M O 1.3944(9) 0.1199(6) 0.4676(6) 0.143(3) Uani 0.411(4) 1 d PDU A 2 H2M H 1.3726 0.0470 0.4425 0.215 Uiso 0.411(4) 1 calc PR A 2 O3 O 0.76047(18) 0.36409(17) 0.52432(13) 0.0656(5) Uani 1 1 d . . . C13 C 0.6959(3) 0.3999(3) 0.5980(2) 0.0862(10) Uani 1 1 d . . . H13A H 0.7354 0.3978 0.6578 0.129 Uiso 1 1 calc R . . H13B H 0.6062 0.3460 0.5699 0.129 Uiso 1 1 calc R . . H13C H 0.7026 0.4801 0.6163 0.129 Uiso 1 1 calc R . . O4 O 0.4994(2) 0.44804(19) 0.30980(15) 0.0768(6) Uani 1 1 d . . . C14 C 0.4482(3) 0.4352(3) 0.2124(2) 0.0953(11) Uani 1 1 d . . . H14A H 0.3710 0.4512 0.2098 0.143 Uiso 1 1 calc R . . H14B H 0.4277 0.3547 0.1606 0.143 Uiso 1 1 calc R . . H14C H 0.5112 0.4910 0.2009 0.143 Uiso 1 1 calc R . . C15 C 0.9648(2) 0.4375(2) 0.23416(18) 0.0484(6) Uani 1 1 d . . . H15A H 1.0025 0.4948 0.3065 0.058 Uiso 1 1 calc R . . H15B H 1.0335 0.4177 0.2098 0.058 Uiso 1 1 calc R . . C16 C 0.9167(2) 0.4987(2) 0.17920(17) 0.0475(6) Uani 1 1 d . . . H16A H 0.8645 0.5370 0.2141 0.057 Uiso 1 1 calc R . . H16B H 0.9905 0.5605 0.1814 0.057 Uiso 1 1 calc R . . C17 C 0.8379(2) 0.4102(2) 0.07038(17) 0.0389(6) Uani 1 1 d . . . C18 C 0.8027(2) 0.4213(2) -0.01366(18) 0.0429(6) Uani 1 1 d . . . C19 C 0.7122(2) 0.3014(2) -0.10404(18) 0.0460(6) Uani 1 1 d . . . H19 H 0.7486 0.2818 -0.1608 0.055 Uiso 1 1 calc R . . C20 C 0.7094(2) 0.2172(2) -0.06024(18) 0.0427(6) Uani 1 1 d . . . C21 C 0.6488(3) 0.0954(2) -0.1028(2) 0.0513(7) Uani 1 1 d . . . C22 C 0.6555(3) 0.0411(2) -0.0413(2) 0.0554(7) Uani 1 1 d . . . H22 H 0.6138 -0.0418 -0.0700 0.066 Uiso 1 1 calc R . . C23 C 0.7241(3) 0.1100(2) 0.0625(2) 0.0505(7) Uani 1 1 d . . . C24 C 0.7890(2) 0.2347(2) 0.10814(18) 0.0421(6) Uani 1 1 d . . . C25 C 0.7789(2) 0.2840(2) 0.04267(17) 0.0393(6) Uani 1 1 d . . . C26 C 0.8376(2) 0.5296(2) -0.0254(2) 0.0486(6) Uani 1 1 d . . . O5 O 0.80798(19) 0.52827(17) -0.10609(15) 0.0721(6) Uani 1 1 d . . . O6 O 0.90490(18) 0.63049(16) 0.06302(15) 0.0596(5) Uani 1 1 d . . . C27 C 0.9440(3) 0.7419(3) 0.0582(3) 0.0737(9) Uani 1 1 d . . . H27A H 0.8683 0.7536 0.0327 0.088 Uiso 1 1 calc R . . H27B H 0.9960 0.7396 0.0124 0.088 Uiso 1 1 calc R . . C28 C 1.0205(4) 0.8408(3) 0.1624(3) 0.1119(13) Uani 1 1 d . . . H28A H 1.0646 0.9124 0.1593 0.168 Uiso 1 1 calc R . . H28B H 1.0829 0.8195 0.1929 0.168 Uiso 1 1 calc R . . H28C H 0.9636 0.8549 0.2029 0.168 Uiso 1 1 calc R . . O7 O 0.58265(19) 0.03270(17) -0.20543(14) 0.0735(6) Uani 1 1 d . . . C29 C 0.5048(3) -0.0921(3) -0.2520(2) 0.0940(11) Uani 1 1 d . . . H29A H 0.4616 -0.1213 -0.3227 0.141 Uiso 1 1 calc R . . H29B H 0.4414 -0.1050 -0.2179 0.141 Uiso 1 1 calc R . . H29C H 0.5587 -0.1344 -0.2468 0.141 Uiso 1 1 calc R . . C30 C 0.6799(3) -0.0645(3) 0.0858(3) 0.0900(11) Uani 1 1 d . . . H30A H 0.6929 -0.0837 0.1403 0.135 Uiso 1 1 calc R . . H30B H 0.7237 -0.0980 0.0391 0.135 Uiso 1 1 calc R . . H30C H 0.5888 -0.0976 0.0504 0.135 Uiso 1 1 calc R . . O8 O 0.7304(2) 0.06206(16) 0.12671(14) 0.0707(6) Uani 1 1 d . . . C1' C 0.9354(3) 0.2493(2) 0.43928(19) 0.0500(7) Uani 1 1 d . . . C2' C 1.0491(3) 0.3162(3) 0.5170(2) 0.0631(8) Uani 1 1 d . . . H2' H 1.1010 0.3908 0.5264 0.076 Uiso 1 1 calc R . . C3' C 1.0891(4) 0.2763(3) 0.5820(2) 0.0773(10) Uani 1 1 d . . . H3' H 1.1670 0.3239 0.6349 0.093 Uiso 1 1 calc R . . C4' C 1.0158(4) 0.1690(4) 0.5691(3) 0.1034(13) Uani 1 1 d . . . H4' H 1.0436 0.1408 0.6119 0.124 Uiso 1 1 calc R . . C5' C 0.9013(5) 0.1017(4) 0.4934(4) 0.149(2) Uani 1 1 d . . . H5' H 0.8490 0.0280 0.4854 0.179 Uiso 1 1 calc R . . C6' C 0.8611(4) 0.1421(3) 0.4274(3) 0.1086(14) Uani 1 1 d . . . H6' H 0.7828 0.0948 0.3749 0.130 Uiso 1 1 calc R . . C1" C 0.5758(3) 0.2980(2) -0.1387(2) 0.0542(7) Uani 1 1 d . . . C2" C 0.5078(3) 0.2477(3) -0.2400(2) 0.0808(9) Uani 1 1 d . . . H2" H 0.5454 0.2161 -0.2897 0.097 Uiso 1 1 calc R . . C3" C 0.3841(4) 0.2432(4) -0.2691(3) 0.1033(12) Uani 1 1 d . . . H3" H 0.3390 0.2084 -0.3381 0.124 Uiso 1 1 calc R . . C4" C 0.3277(3) 0.2902(3) -0.1963(3) 0.0922(11) Uani 1 1 d . . . H4" H 0.2449 0.2879 -0.2160 0.111 Uiso 1 1 calc R . . C5" C 0.3929(3) 0.3398(3) -0.0959(3) 0.0754(9) Uani 1 1 d . . . H5" H 0.3544 0.3708 -0.0467 0.090 Uiso 1 1 calc R . . C6" C 0.5162(3) 0.3444(3) -0.0668(2) 0.0652(8) Uani 1 1 d . . . H6" H 0.5605 0.3792 0.0023 0.078 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 C1 0.0519(16) 0.0527(17) 0.0483(15) 0.0336(13) 0.0237(13) 0.0302(14) C2 0.0663(19) 0.0662(19) 0.0546(16) 0.0387(15) 0.0281(15) 0.0434(16) C3 0.0621(18) 0.0468(17) 0.0488(15) 0.0272(13) 0.0206(14) 0.0294(14) C4 0.0493(16) 0.0416(15) 0.0459(15) 0.0240(12) 0.0169(13) 0.0204(13) C5 0.0539(17) 0.0498(17) 0.0438(15) 0.0253(13) 0.0177(14) 0.0205(14) C6 0.0593(18) 0.0577(18) 0.0561(17) 0.0270(14) 0.0301(15) 0.0284(15) C7 0.0540(18) 0.0531(18) 0.0596(18) 0.0290(14) 0.0219(15) 0.0303(15) C8 0.0539(17) 0.0504(17) 0.0523(15) 0.0317(13) 0.0194(14) 0.0279(14) C9 0.0498(16) 0.0379(15) 0.0469(15) 0.0240(12) 0.0186(13) 0.0202(13) C10 0.133(3) 0.149(4) 0.062(2) 0.062(2) 0.046(2) 0.116(3) O1 0.1128(18) 0.1202(19) 0.0797(15) 0.0661(14) 0.0577(14) 0.0864(16) O2A 0.083(3) 0.148(5) 0.079(3) 0.075(3) 0.047(3) 0.086(3) C11A 0.072(4) 0.120(5) 0.130(5) 0.085(4) 0.061(4) 0.070(4) C12A 0.183(9) 0.464(17) 0.232(11) 0.302(12) 0.165(8) 0.272(12) C1M 0.55(3) 0.43(3) 0.49(3) 0.35(3) 0.39(3) 0.31(3) O1M 0.80(4) 0.495(17) 0.324(15) 0.136(13) 0.21(2) 0.44(2) O2B 0.123(6) 0.119(6) 0.084(4) 0.070(4) 0.050(4) 0.099(5) C11B 0.116(7) 0.156(9) 0.162(8) 0.131(8) 0.115(7) 0.120(7) C12B 0.153(8) 0.127(8) 0.271(12) 0.110(8) 0.092(9) 0.071(7) C2M 0.091(10) 0.37(3) 0.118(9) 0.147(14) 0.050(8) 0.097(11) O2M 0.197(8) 0.093(5) 0.127(6) 0.034(5) 0.074(5) 0.058(5) O3 0.0722(13) 0.0933(15) 0.0503(11) 0.0410(11) 0.0297(10) 0.0425(12) C13 0.076(2) 0.138(3) 0.0542(19) 0.049(2) 0.0331(18) 0.045(2) O4 0.0798(15) 0.1113(18) 0.0770(14) 0.0537(13) 0.0368(12) 0.0680(14) C14 0.096(3) 0.147(3) 0.094(3) 0.073(3) 0.038(2) 0.086(3) C15 0.0500(16) 0.0547(17) 0.0441(14) 0.0254(13) 0.0146(13) 0.0228(14) C16 0.0528(16) 0.0409(15) 0.0466(15) 0.0225(13) 0.0143(13) 0.0141(13) C17 0.0414(15) 0.0372(15) 0.0435(15) 0.0233(12) 0.0153(12) 0.0157(12) C18 0.0422(15) 0.0460(16) 0.0512(15) 0.0296(13) 0.0180(13) 0.0204(13) C19 0.0513(17) 0.0490(17) 0.0433(14) 0.0257(13) 0.0165(13) 0.0213(13) C20 0.0436(15) 0.0405(17) 0.0456(15) 0.0216(13) 0.0150(13) 0.0169(13) C21 0.0527(17) 0.0477(19) 0.0472(16) 0.0170(15) 0.0170(14) 0.0196(14) C22 0.0608(18) 0.0355(16) 0.0688(19) 0.0218(15) 0.0265(16) 0.0194(14) C23 0.0640(18) 0.0421(18) 0.0685(19) 0.0361(15) 0.0350(16) 0.0296(15) C24 0.0469(16) 0.0463(17) 0.0491(15) 0.0284(13) 0.0234(13) 0.0269(13) C25 0.0407(14) 0.0375(15) 0.0451(15) 0.0214(12) 0.0170(12) 0.0184(12) C26 0.0429(16) 0.0566(19) 0.0660(19) 0.0407(17) 0.0241(15) 0.0252(14) O5 0.0762(14) 0.0835(15) 0.0765(14) 0.0604(12) 0.0204(12) 0.0271(12) O6 0.0720(13) 0.0435(12) 0.0722(13) 0.0362(11) 0.0255(11) 0.0207(10) C27 0.079(2) 0.054(2) 0.113(3) 0.056(2) 0.045(2) 0.0284(18) C28 0.133(3) 0.062(3) 0.125(3) 0.042(3) 0.044(3) 0.020(2) O7 0.0787(14) 0.0506(13) 0.0596(13) 0.0128(10) 0.0072(11) 0.0120(11) C29 0.087(2) 0.058(2) 0.077(2) 0.0011(18) 0.0237(19) -0.0028(19) C30 0.107(3) 0.066(2) 0.133(3) 0.071(2) 0.051(2) 0.041(2) O8 0.1006(16) 0.0513(13) 0.0845(14) 0.0496(11) 0.0388(12) 0.0319(11) C1' 0.0651(19) 0.0527(18) 0.0488(16) 0.0313(15) 0.0229(15) 0.0324(15) C2' 0.076(2) 0.0520(19) 0.0557(18) 0.0239(16) 0.0095(17) 0.0270(17) C3' 0.099(3) 0.080(3) 0.0485(17) 0.0221(18) 0.0057(17) 0.050(2) C4' 0.123(4) 0.119(4) 0.096(3) 0.080(3) 0.017(3) 0.051(3) C5' 0.128(4) 0.126(4) 0.189(5) 0.129(4) -0.019(4) 0.002(3) C6' 0.098(3) 0.090(3) 0.123(3) 0.080(3) -0.022(2) 0.004(2) C1" 0.0599(19) 0.0484(17) 0.0532(17) 0.0285(14) 0.0084(15) 0.0187(14) C2" 0.083(3) 0.094(3) 0.057(2) 0.0326(18) 0.0088(18) 0.037(2) C3" 0.079(3) 0.132(4) 0.080(3) 0.050(2) -0.011(2) 0.038(3) C4" 0.067(2) 0.102(3) 0.108(3) 0.060(2) 0.008(3) 0.030(2) C5" 0.055(2) 0.087(2) 0.094(3) 0.048(2) 0.0236(19) 0.0337(18) C6" 0.057(2) 0.080(2) 0.0640(18) 0.0364(17) 0.0188(16) 0.0325(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.517(3) . ? C1 C9 1.526(3) . ? C1 C24 1.526(3) . ? C1 C15 1.559(3) . ? C2 C3 1.354(3) . ? C2 C10 1.469(4) . ? C3 C4 1.466(3) . ? C3 C1' 1.491(3) . ? C4 C9 1.385(3) . ? C4 C5 1.411(3) . ? C5 O3 1.365(3) . ? C5 C6 1.374(3) . ? C6 C7 1.399(3) . ? C6 H6 0.9300 . ? C7 O4 1.366(3) . ? C7 C8 1.377(3) . ? C8 C9 1.381(3) . ? C8 H8 0.9300 . ? C10 O1 1.230(3) . ? C10 O2A 1.351(4) . ? C10 O2B 1.413(6) . ? O1 C11B 1.466(6) . ? O2A C11A 1.447(6) . ? C11A C12A 1.515(7) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C12A H12A 0.9600 . ? C12A H12B 0.9600 . ? C12A H12C 0.9600 . ? C1M O1M 1.461(10) . ? C1M H1M1 0.9600 . ? C1M H1M2 0.9600 . ? C1M H1M3 0.9600 . ? O1M C1M 1.461(10) 2_656 ? O1M H1M 0.7818 . ? C11B C12B 1.711(8) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C12B C11B 1.711(8) 2_755 ? C12B H12D 0.9600 . ? C12B H12E 0.9600 . ? C12B H12F 0.9600 . ? C2M O2M 1.511(9) . ? C2M H2M1 0.9600 . ? C2M H2M2 0.9600 . ? C2M H2M3 0.9600 . ? O2M H2M 0.8208 . ? O3 C13 1.421(3) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? O4 C14 1.417(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.525(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.495(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.352(3) . ? C17 C25 1.455(3) . ? C18 C26 1.467(3) . ? C18 C19 1.512(3) . ? C19 C20 1.511(3) . ? C19 C1" 1.540(4) . ? C19 H19 0.9800 . ? C20 C21 1.365(3) . ? C20 C25 1.383(3) . ? C21 O7 1.371(3) . ? C21 C22 1.396(3) . ? C22 C23 1.392(3) . ? C22 H22 0.9300 . ? C23 O8 1.365(3) . ? C23 C24 1.397(3) . ? C24 C25 1.400(3) . ? C26 O5 1.206(3) . ? C26 O6 1.336(3) . ? O6 C27 1.451(3) . ? C27 C28 1.476(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? O7 C29 1.421(3) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 O8 1.418(3) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C1' C6' 1.345(4) . ? C1' C2' 1.359(4) . ? C2' C3' 1.372(4) . ? C2' H2' 0.9300 . ? C3' C4' 1.338(4) . ? C3' H3' 0.9300 . ? C4' C5' 1.352(5) . ? C4' H4' 0.9300 . ? C5' C6' 1.391(4) . ? C5' H5' 0.9300 . ? C6' H6' 0.9300 . ? C1" C2" 1.372(4) . ? C1" C6" 1.390(3) . ? C2" C3" 1.383(4) . ? C2" H2" 0.9300 . ? C3" C4" 1.376(5) . ? C3" H3" 0.9300 . ? C4" C5" 1.354(4) . ? C4" H4" 0.9300 . ? C5" C6" 1.379(4) . ? C5" H5" 0.9300 . ? C6" H6" 0.9300 . ? 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 C2 C1 C9 101.07(18) . . ? C2 C1 C24 117.0(2) . . ? C9 C1 C24 111.23(19) . . ? C2 C1 C15 107.5(2) . . ? C9 C1 C15 110.21(19) . . ? C24 C1 C15 109.45(19) . . ? C3 C2 C10 126.7(2) . . ? C3 C2 C1 111.6(2) . . ? C10 C2 C1 121.6(2) . . ? C2 C3 C4 108.3(2) . . ? C2 C3 C1' 126.6(2) . . ? C4 C3 C1' 125.0(2) . . ? C9 C4 C5 119.3(2) . . ? C9 C4 C3 109.3(2) . . ? C5 C4 C3 131.4(2) . . ? O3 C5 C6 124.4(2) . . ? O3 C5 C4 117.0(2) . . ? C6 C5 C4 118.6(2) . . ? C5 C6 C7 120.8(2) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? O4 C7 C8 124.4(2) . . ? O4 C7 C6 114.7(2) . . ? C8 C7 C6 120.9(2) . . ? C7 C8 C9 118.2(2) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? C8 C9 C4 122.0(2) . . ? C8 C9 C1 128.8(2) . . ? C4 C9 C1 109.2(2) . . ? O1 C10 O2A 118.7(3) . . ? O1 C10 O2B 118.3(3) . . ? O2A C10 O2B 53.4(3) . . ? O1 C10 C2 121.3(3) . . ? O2A C10 C2 114.9(3) . . ? O2B C10 C2 111.7(4) . . ? C10 O1 C11B 122.5(4) . . ? C10 O2A C11A 121.4(4) . . ? O2A C11A C12A 104.5(5) . . ? O2A C11A H11A 110.9 . . ? C12A C11A H11A 110.8 . . ? O2A C11A H11B 110.8 . . ? C12A C11A H11B 110.8 . . ? H11A C11A H11B 108.9 . . ? C1M O1M C1M 180.0(8) 2_656 . ? C1M O1M H1M 67.5 2_656 . ? C1M O1M H1M 112.5 . . ? O1 C11B C12B 124.8(5) . . ? O1 C11B H11C 106.9 . . ? C12B C11B H11C 103.9 . . ? O1 C11B H11D 108.6 . . ? C12B C11B H11D 105.5 . . ? H11C C11B H11D 105.6 . . ? C11B C12B C11B 180.0(9) . 2_755 ? C11B C12B H12D 109.9 . . ? C11B C12B H12D 70.1 2_755 . ? C11B C12B H12E 109.6 . . ? C11B C12B H12E 70.4 2_755 . ? H12D C12B H12E 109.5 . . ? C11B C12B H12F 108.8 . . ? C11B C12B H12F 71.2 2_755 . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? O2M C2M H2M1 109.6 . . ? O2M C2M H2M2 109.4 . . ? H2M1 C2M H2M2 109.5 . . ? O2M C2M H2M3 109.4 . . ? H2M1 C2M H2M3 109.5 . . ? H2M2 C2M H2M3 109.5 . . ? C2M O2M H2M 109.7 . . ? C5 O3 C13 118.0(2) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 O4 C14 118.2(2) . . ? O4 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C1 116.2(2) . . ? C16 C15 H15A 108.2 . . ? C1 C15 H15A 108.2 . . ? C16 C15 H15B 108.2 . . ? C1 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? C17 C16 C15 111.2(2) . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C25 108.3(2) . . ? C18 C17 C16 133.4(2) . . ? C25 C17 C16 118.3(2) . . ? C17 C18 C26 129.3(2) . . ? C17 C18 C19 111.2(2) . . ? C26 C18 C19 119.5(2) . . ? C18 C19 C20 101.63(18) . . ? C18 C19 C1" 111.97(19) . . ? C20 C19 C1" 111.0(2) . . ? C18 C19 H19 110.7 . . ? C20 C19 H19 110.7 . . ? C1" C19 H19 110.7 . . ? C21 C20 C25 119.1(2) . . ? C21 C20 C19 131.8(2) . . ? C25 C20 C19 109.0(2) . . ? C20 C21 O7 117.1(2) . . ? C20 C21 C22 119.4(2) . . ? O7 C21 C22 123.5(2) . . ? C23 C22 C21 120.6(2) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? O8 C23 C22 123.0(2) . . ? O8 C23 C24 115.6(2) . . ? C22 C23 C24 121.4(2) . . ? C23 C24 C25 115.5(2) . . ? C23 C24 C1 126.6(2) . . ? C25 C24 C1 117.8(2) . . ? C20 C25 C24 124.0(2) . . ? C20 C25 C17 109.6(2) . . ? C24 C25 C17 126.5(2) . . ? O5 C26 O6 123.3(2) . . ? O5 C26 C18 123.8(3) . . ? O6 C26 C18 113.0(2) . . ? C26 O6 C27 116.5(2) . . ? O6 C27 C28 107.8(3) . . ? O6 C27 H27A 110.2 . . ? C28 C27 H27A 110.2 . . ? O6 C27 H27B 110.2 . . ? C28 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C21 O7 C29 119.9(2) . . ? O7 C29 H29A 109.5 . . ? O7 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O7 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O8 C30 H30A 109.5 . . ? O8 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O8 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C23 O8 C30 119.7(2) . . ? C6' C1' C2' 118.3(3) . . ? C6' C1' C3 119.1(3) . . ? C2' C1' C3 122.5(3) . . ? C1' C2' C3' 121.6(3) . . ? C1' C2' H2' 119.2 . . ? C3' C2' H2' 119.2 . . ? C4' C3' C2' 119.9(3) . . ? C4' C3' H3' 120.0 . . ? C2' C3' H3' 120.0 . . ? C3' C4' C5' 119.6(3) . . ? C3' C4' H4' 120.2 . . ? C5' C4' H4' 120.2 . . ? C4' C5' C6' 120.4(4) . . ? C4' C5' H5' 119.8 . . ? C6' C5' H5' 119.8 . . ? C1' C6' C5' 120.2(3) . . ? C1' C6' H6' 119.9 . . ? C5' C6' H6' 119.9 . . ? C2" C1" C6" 117.8(3) . . ? C2" C1" C19 122.1(3) . . ? C6" C1" C19 120.2(2) . . ? C1" C2" C3" 120.9(3) . . ? C1" C2" H2" 119.5 . . ? C3" C2" H2" 119.6 . . ? C4" C3" C2" 120.1(3) . . ? C4" C3" H3" 120.0 . . ? C2" C3" H3" 119.9 . . ? C5" C4" C3" 120.0(3) . . ? C5" C4" H4" 120.0 . . ? C3" C4" H4" 120.0 . . ? C4" C5" C6" 120.0(3) . . ? C4" C5" H5" 120.0 . . ? C6" C5" H5" 120.0 . . ? C5" C6" C1" 121.3(3) . . ? C5" C6" H6" 119.3 . . ? C1" C6" H6" 119.3 . . ? 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 C9 C1 C2 C3 -5.6(3) . . . . ? C24 C1 C2 C3 -126.5(2) . . . . ? C15 C1 C2 C3 109.9(2) . . . . ? C9 C1 C2 C10 174.9(3) . . . . ? C24 C1 C2 C10 53.9(4) . . . . ? C15 C1 C2 C10 -69.6(3) . . . . ? C10 C2 C3 C4 -178.3(3) . . . . ? C1 C2 C3 C4 2.2(3) . . . . ? C10 C2 C3 C1' -2.9(5) . . . . ? C1 C2 C3 C1' 177.5(2) . . . . ? C2 C3 C4 C9 2.6(3) . . . . ? C1' C3 C4 C9 -172.8(2) . . . . ? C2 C3 C4 C5 -178.9(3) . . . . ? C1' C3 C4 C5 5.7(4) . . . . ? C9 C4 C5 O3 -177.2(2) . . . . ? C3 C4 C5 O3 4.4(4) . . . . ? C9 C4 C5 C6 3.5(4) . . . . ? C3 C4 C5 C6 -174.9(2) . . . . ? O3 C5 C6 C7 -178.7(2) . . . . ? C4 C5 C6 C7 0.6(4) . . . . ? C5 C6 C7 O4 176.6(2) . . . . ? C5 C6 C7 C8 -3.3(4) . . . . ? O4 C7 C8 C9 -178.0(2) . . . . ? C6 C7 C8 C9 1.8(4) . . . . ? C7 C8 C9 C4 2.3(4) . . . . ? C7 C8 C9 C1 -177.8(2) . . . . ? C5 C4 C9 C8 -5.0(4) . . . . ? C3 C4 C9 C8 173.7(2) . . . . ? C5 C4 C9 C1 175.1(2) . . . . ? C3 C4 C9 C1 -6.2(3) . . . . ? C2 C1 C9 C8 -172.9(2) . . . . ? C24 C1 C9 C8 -48.0(3) . . . . ? C15 C1 C9 C8 73.6(3) . . . . ? C2 C1 C9 C4 7.0(3) . . . . ? C24 C1 C9 C4 132.0(2) . . . . ? C15 C1 C9 C4 -106.4(2) . . . . ? C3 C2 C10 O1 -176.6(3) . . . . ? C1 C2 C10 O1 2.9(5) . . . . ? C3 C2 C10 O2A -22.2(6) . . . . ? C1 C2 C10 O2A 157.3(4) . . . . ? C3 C2 C10 O2B 36.3(6) . . . . ? C1 C2 C10 O2B -144.2(4) . . . . ? O2A C10 O1 C11B 53.9(6) . . . . ? O2B C10 O1 C11B -7.6(7) . . . . ? C2 C10 O1 C11B -152.7(4) . . . . ? O1 C10 O2A C11A -17.4(8) . . . . ? O2B C10 O2A C11A 88.1(6) . . . . ? C2 C10 O2A C11A -172.5(5) . . . . ? C10 O2A C11A C12A -174.7(8) . . . . ? C10 O1 C11B C12B 96.4(6) . . . . ? O1 C11B C12B C11B -69(100) . . . 2_755 ? C6 C5 O3 C13 -2.2(4) . . . . ? C4 C5 O3 C13 178.4(2) . . . . ? C8 C7 O4 C14 10.4(4) . . . . ? C6 C7 O4 C14 -169.5(3) . . . . ? C2 C1 C15 C16 179.58(19) . . . . ? C9 C1 C15 C16 -71.1(3) . . . . ? C24 C1 C15 C16 51.5(3) . . . . ? C1 C15 C16 C17 -48.6(3) . . . . ? C15 C16 C17 C18 -160.7(2) . . . . ? C15 C16 C17 C25 22.0(3) . . . . ? C25 C17 C18 C26 -179.4(2) . . . . ? C16 C17 C18 C26 3.0(4) . . . . ? C25 C17 C18 C19 2.0(3) . . . . ? C16 C17 C18 C19 -175.5(2) . . . . ? C17 C18 C19 C20 -4.3(2) . . . . ? C26 C18 C19 C20 177.02(19) . . . . ? C17 C18 C19 C1" 114.2(2) . . . . ? C26 C18 C19 C1" -64.5(3) . . . . ? C18 C19 C20 C21 -177.9(2) . . . . ? C1" C19 C20 C21 62.9(3) . . . . ? C18 C19 C20 C25 5.0(2) . . . . ? C1" C19 C20 C25 -114.2(2) . . . . ? C25 C20 C21 O7 -179.1(2) . . . . ? C19 C20 C21 O7 4.1(4) . . . . ? C25 C20 C21 C22 1.6(3) . . . . ? C19 C20 C21 C22 -175.2(2) . . . . ? C20 C21 C22 C23 -0.5(4) . . . . ? O7 C21 C22 C23 -179.8(2) . . . . ? C21 C22 C23 O8 177.9(2) . . . . ? C21 C22 C23 C24 -0.6(4) . . . . ? O8 C23 C24 C25 -178.1(2) . . . . ? C22 C23 C24 C25 0.5(3) . . . . ? O8 C23 C24 C1 -2.2(3) . . . . ? C22 C23 C24 C1 176.5(2) . . . . ? C2 C1 C24 C23 33.6(3) . . . . ? C9 C1 C24 C23 -81.8(3) . . . . ? C15 C1 C24 C23 156.2(2) . . . . ? C2 C1 C24 C25 -150.6(2) . . . . ? C9 C1 C24 C25 94.0(2) . . . . ? C15 C1 C24 C25 -28.0(3) . . . . ? C21 C20 C25 C24 -1.8(3) . . . . ? C19 C20 C25 C24 175.8(2) . . . . ? C21 C20 C25 C17 178.3(2) . . . . ? C19 C20 C25 C17 -4.2(2) . . . . ? C23 C24 C25 C20 0.6(3) . . . . ? C1 C24 C25 C20 -175.6(2) . . . . ? C23 C24 C25 C17 -179.4(2) . . . . ? C1 C24 C25 C17 4.3(3) . . . . ? C18 C17 C25 C20 1.4(3) . . . . ? C16 C17 C25 C20 179.4(2) . . . . ? C18 C17 C25 C24 -178.6(2) . . . . ? C16 C17 C25 C24 -0.6(3) . . . . ? C17 C18 C26 O5 174.5(3) . . . . ? C19 C18 C26 O5 -7.1(3) . . . . ? C17 C18 C26 O6 -6.1(3) . . . . ? C19 C18 C26 O6 172.3(2) . . . . ? O5 C26 O6 C27 -0.9(3) . . . . ? C18 C26 O6 C27 179.7(2) . . . . ? C26 O6 C27 C28 -178.0(3) . . . . ? C20 C21 O7 C29 -172.4(2) . . . . ? C22 C21 O7 C29 6.9(4) . . . . ? C22 C23 O8 C30 8.3(4) . . . . ? C24 C23 O8 C30 -173.1(2) . . . . ? C2 C3 C1' C6' -95.0(4) . . . . ? C4 C3 C1' C6' 79.5(4) . . . . ? C2 C3 C1' C2' 82.8(4) . . . . ? C4 C3 C1' C2' -102.6(3) . . . . ? C6' C1' C2' C3' 0.5(4) . . . . ? C3 C1' C2' C3' -177.4(2) . . . . ? C1' C2' C3' C4' 0.4(5) . . . . ? C2' C3' C4' C5' -1.5(6) . . . . ? C3' C4' C5' C6' 1.8(7) . . . . ? C2' C1' C6' C5' -0.2(6) . . . . ? C3 C1' C6' C5' 177.7(4) . . . . ? C4' C5' C6' C1' -0.9(7) . . . . ? C18 C19 C1" C2" 137.4(3) . . . . ? C20 C19 C1" C2" -109.8(3) . . . . ? C18 C19 C1" C6" -44.1(3) . . . . ? C20 C19 C1" C6" 68.7(3) . . . . ? C6" C1" C2" C3" -0.1(5) . . . . ? C19 C1" C2" C3" 178.4(3) . . . . ? C1" C2" C3" C4" 0.4(5) . . . . ? C2" C3" C4" C5" -0.7(6) . . . . ? C3" C4" C5" C6" 0.7(5) . . . . ? C4" C5" C6" C1" -0.5(5) . . . . ? C2" C1" C6" C5" 0.2(4) . . . . ? C19 C1" C6" C5" -178.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.830 _diffrn_reflns_theta_full 29.21 _diffrn_measured_fraction_theta_full 0.830 _refine_diff_density_max 0.350 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.039 data_vc1409 _database_code_depnum_ccdc_archive 'CCDC 844784' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Ethyl 4,5,6-Trimethoxy-1-oxo-3-phenyl-1H-indene-2-carboxylate ; _chemical_formula_moiety 'C21 H20 O6' _chemical_formula_sum 'C21 H20 O6' _chemical_formula_weight 368.37 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.7773(6) _cell_length_b 11.5001(4) _cell_length_c 20.4105(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.792(3) _cell_angle_gamma 90.00 _cell_volume 3702.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3953 _cell_measurement_theta_min 2.1871 _cell_measurement_theta_max 29.0283 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_T_min 0.95365 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.0827 _diffrn_reflns_number 8222 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 29.09 _reflns_number_total 4238 _reflns_number_gt 2762 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0713P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4238 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.003 _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 0.59705(8) 0.50224(13) -0.05171(7) 0.0379(3) Uani 1 1 d . . . O1 O 0.58162(7) 0.47317(10) -0.10765(5) 0.0534(3) Uani 1 1 d . . . C2 C 0.59382(8) 0.62155(12) -0.02176(7) 0.0373(3) Uani 1 1 d . . . C3 C 0.61802(7) 0.61374(12) 0.04230(7) 0.0344(3) Uani 1 1 d . . . C1' C 0.62914(8) 0.71109(12) 0.08935(7) 0.0369(3) Uani 1 1 d . . . C2' C 0.70836(10) 0.75903(15) 0.09826(9) 0.0552(4) Uani 1 1 d . . . H2' H 0.7540 0.7288 0.0755 0.089(7) Uiso 1 1 calc R . . C3' C 0.72108(13) 0.85099(17) 0.14042(10) 0.0703(5) Uani 1 1 d . . . H3' H 0.7750 0.8823 0.1460 0.091(7) Uiso 1 1 calc R . . C4' C 0.65487(14) 0.89607(17) 0.17398(10) 0.0732(6) Uani 1 1 d . . . H4' H 0.6632 0.9589 0.2020 0.088(6) Uiso 1 1 calc R . . C5' C 0.57627(14) 0.84870(19) 0.16624(11) 0.0810(7) Uani 1 1 d . . . H5' H 0.5311 0.8789 0.1896 0.095(7) Uiso 1 1 calc R . . C6' C 0.56291(11) 0.75586(17) 0.12389(10) 0.0670(5) Uani 1 1 d . . . H6' H 0.5090 0.7241 0.1190 0.093(7) Uiso 1 1 calc R . . C4 C 0.63619(7) 0.49086(12) 0.05891(7) 0.0348(3) Uani 1 1 d . . . C5 C 0.65871(8) 0.43690(12) 0.11755(7) 0.0369(3) Uani 1 1 d . . . C6 C 0.67046(9) 0.31497(13) 0.11739(7) 0.0409(4) Uani 1 1 d . . . C7 C 0.65723(8) 0.24980(12) 0.06036(8) 0.0408(4) Uani 1 1 d . . . C8 C 0.63433(8) 0.30444(12) 0.00196(7) 0.0397(4) Uani 1 1 d . . . H8 H 0.6261 0.2620 -0.0364 0.040(4) Uiso 1 1 calc R . . C9 C 0.62428(8) 0.42330(12) 0.00270(7) 0.0356(3) Uani 1 1 d . . . C10 C 0.56970(9) 0.73075(14) -0.05524(8) 0.0424(4) Uani 1 1 d . . . O2 O 0.56300(9) 0.82271(10) -0.02894(7) 0.0731(4) Uani 1 1 d . . . O3 O 0.55411(8) 0.71512(10) -0.11853(6) 0.0616(3) Uani 1 1 d . . . C11 C 0.52665(13) 0.81712(17) -0.15539(10) 0.0687(5) Uani 1 1 d . . . H11A H 0.4929 0.8666 -0.1274 0.090(7) Uiso 1 1 calc R . . H11B H 0.4912 0.7927 -0.1921 0.136(10) Uiso 1 1 calc R . . C12 C 0.59919(15) 0.8840(2) -0.18007(14) 0.0927(8) Uani 1 1 d . . . H12A H 0.6281 0.9210 -0.1440 0.087(8) Uiso 1 1 calc R . . H12B H 0.5792 0.9420 -0.2104 0.123(9) Uiso 1 1 calc R . . H12C H 0.6375 0.8325 -0.2019 0.149(12) Uiso 1 1 calc R . . O4 O 0.67145(6) 0.49903(9) 0.17352(5) 0.0455(3) Uani 1 1 d . . . C13 C 0.60549(11) 0.48550(19) 0.22059(9) 0.0667(5) Uani 1 1 d . . . H13A H 0.5513 0.4914 0.1989 0.141(10) Uiso 1 1 calc R . . H13B H 0.6105 0.5453 0.2532 0.115(8) Uiso 1 1 calc R . . H13C H 0.6105 0.4107 0.2412 0.145(11) Uiso 1 1 calc R . . O5 O 0.68902(7) 0.26169(10) 0.17566(5) 0.0542(3) Uani 1 1 d . . . C14 C 0.77372(13) 0.2218(2) 0.18343(11) 0.0835(7) Uani 1 1 d . . . H14A H 0.7851 0.1635 0.1510 0.152(12) Uiso 1 1 calc R . . H14B H 0.7813 0.1891 0.2264 0.099(7) Uiso 1 1 calc R . . H14C H 0.8121 0.2858 0.1781 0.147(13) Uiso 1 1 calc R . . O6 O 0.66710(7) 0.13306(9) 0.06739(6) 0.0540(3) Uani 1 1 d . . . C15 C 0.64552(12) 0.06064(15) 0.01284(9) 0.0623(5) Uani 1 1 d . . . H15A H 0.5875 0.0738 0.0002 0.084(6) Uiso 1 1 calc R . . H15B H 0.6530 -0.0194 0.0249 0.092(7) Uiso 1 1 calc R . . H15C H 0.6816 0.0789 -0.0232 0.085(6) 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 C1 0.0355(7) 0.0414(8) 0.0369(8) -0.0031(7) 0.0016(6) -0.0053(6) O1 0.0706(7) 0.0528(7) 0.0367(6) -0.0061(5) -0.0056(5) -0.0011(5) C2 0.0360(7) 0.0364(8) 0.0395(8) 0.0011(6) 0.0019(6) -0.0018(6) C3 0.0286(6) 0.0353(8) 0.0394(8) -0.0014(6) 0.0044(5) -0.0026(5) C1' 0.0432(8) 0.0301(7) 0.0373(8) -0.0007(6) 0.0004(6) 0.0005(6) C2' 0.0520(9) 0.0536(10) 0.0601(11) -0.0173(9) 0.0050(8) -0.0099(8) C3' 0.0789(13) 0.0640(12) 0.0680(13) -0.0195(11) 0.0055(10) -0.0262(10) C4' 0.1099(16) 0.0505(12) 0.0593(13) -0.0231(10) 0.0035(11) -0.0095(11) C5' 0.0850(14) 0.0790(14) 0.0794(15) -0.0352(12) 0.0191(11) 0.0135(12) C6' 0.0528(10) 0.0745(13) 0.0739(13) -0.0293(11) 0.0095(9) -0.0003(9) C4 0.0316(7) 0.0343(8) 0.0385(8) -0.0021(6) 0.0022(5) -0.0007(6) C5 0.0361(7) 0.0386(8) 0.0359(8) -0.0035(7) 0.0016(5) -0.0023(6) C6 0.0415(8) 0.0405(9) 0.0407(9) 0.0030(7) 0.0033(6) 0.0015(6) C7 0.0433(8) 0.0314(8) 0.0479(10) 0.0001(7) 0.0065(6) 0.0001(6) C8 0.0412(8) 0.0363(8) 0.0417(9) -0.0087(7) 0.0041(6) -0.0026(6) C9 0.0338(7) 0.0358(8) 0.0373(8) -0.0028(6) 0.0031(5) -0.0025(6) C10 0.0412(8) 0.0426(9) 0.0434(9) 0.0016(7) 0.0002(6) -0.0020(6) O2 0.1192(11) 0.0391(7) 0.0605(8) -0.0010(7) -0.0158(7) 0.0121(7) O3 0.0922(9) 0.0510(7) 0.0413(7) 0.0062(6) -0.0074(6) 0.0054(6) C11 0.0893(13) 0.0643(12) 0.0522(11) 0.0209(10) -0.0059(10) 0.0062(11) C12 0.0973(16) 0.0916(17) 0.0897(19) 0.0397(16) 0.0235(15) 0.0106(15) O4 0.0537(6) 0.0451(6) 0.0377(6) -0.0055(5) -0.0003(4) -0.0056(5) C13 0.0767(13) 0.0793(14) 0.0445(10) -0.0144(10) 0.0169(9) -0.0064(10) O5 0.0661(7) 0.0520(7) 0.0445(7) 0.0112(5) 0.0024(5) 0.0112(5) C14 0.0750(14) 0.1109(19) 0.0642(14) 0.0110(14) -0.0125(10) 0.0324(14) O6 0.0728(7) 0.0317(6) 0.0576(8) -0.0005(5) 0.0012(6) 0.0019(5) C15 0.0765(13) 0.0373(10) 0.0731(13) -0.0112(9) 0.0012(10) 0.0005(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.2112(17) . ? C1 C9 1.493(2) . ? C1 C2 1.503(2) . ? C2 C3 1.360(2) . ? C2 C10 1.477(2) . ? C3 C4 1.4804(19) . ? C3 C1' 1.4836(19) . ? C1' C6' 1.369(2) . ? C1' C2' 1.376(2) . ? C2' C3' 1.376(2) . ? C2' H2' 0.9300 . ? C3' C4' 1.360(3) . ? C3' H3' 0.9300 . ? C4' C5' 1.362(3) . ? C4' H4' 0.9300 . ? C5' C6' 1.388(3) . ? C5' H5' 0.9300 . ? C6' H6' 0.9300 . ? C4 C5 1.3900(19) . ? C4 C9 1.3960(19) . ? C5 O4 1.3599(17) . ? C5 C6 1.414(2) . ? C6 O5 1.3660(18) . ? C6 C7 1.398(2) . ? C7 O6 1.3589(17) . ? C7 C8 1.391(2) . ? C8 C9 1.376(2) . ? C8 H8 0.9300 . ? C10 O2 1.1913(18) . ? C10 O3 1.3239(19) . ? O3 C11 1.456(2) . ? C11 C12 1.473(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? O4 C13 1.4346(18) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? O5 C14 1.420(2) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? O6 C15 1.428(2) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 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 O1 C1 C9 125.83(14) . . ? O1 C1 C2 128.89(14) . . ? C9 C1 C2 105.28(12) . . ? C3 C2 C10 124.61(14) . . ? C3 C2 C1 108.67(12) . . ? C10 C2 C1 126.72(13) . . ? C2 C3 C4 109.51(12) . . ? C2 C3 C1' 126.98(13) . . ? C4 C3 C1' 123.46(12) . . ? C6' C1' C2' 118.66(15) . . ? C6' C1' C3 122.20(13) . . ? C2' C1' C3 119.14(13) . . ? C1' C2' C3' 120.99(16) . . ? C1' C2' H2' 119.5 . . ? C3' C2' H2' 119.5 . . ? C4' C3' C2' 120.10(17) . . ? C4' C3' H3' 120.0 . . ? C2' C3' H3' 120.0 . . ? C5' C4' C3' 119.60(18) . . ? C5' C4' H4' 120.2 . . ? C3' C4' H4' 120.2 . . ? C4' C5' C6' 120.67(18) . . ? C4' C5' H5' 119.7 . . ? C6' C5' H5' 119.7 . . ? C1' C6' C5' 119.98(17) . . ? C1' C6' H6' 120.0 . . ? C5' C6' H6' 120.0 . . ? C5 C4 C9 119.28(13) . . ? C5 C4 C3 132.04(13) . . ? C9 C4 C3 108.65(12) . . ? O4 C5 C4 121.46(13) . . ? O4 C5 C6 120.32(13) . . ? C4 C5 C6 118.20(13) . . ? O5 C6 C7 120.82(13) . . ? O5 C6 C5 117.98(13) . . ? C7 C6 C5 121.03(14) . . ? O6 C7 C8 124.39(14) . . ? O6 C7 C6 115.24(14) . . ? C8 C7 C6 120.36(13) . . ? C9 C8 C7 117.90(14) . . ? C9 C8 H8 121.1 . . ? C7 C8 H8 121.1 . . ? C8 C9 C4 123.21(14) . . ? C8 C9 C1 128.89(13) . . ? C4 C9 C1 107.87(12) . . ? O2 C10 O3 122.93(15) . . ? O2 C10 C2 124.77(15) . . ? O3 C10 C2 112.28(14) . . ? C10 O3 C11 116.41(15) . . ? O3 C11 C12 111.72(17) . . ? O3 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? O3 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 O4 C13 113.92(11) . . ? O4 C13 H13A 109.5 . . ? O4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C6 O5 C14 115.62(13) . . ? O5 C14 H14A 109.5 . . ? O5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 O6 C15 117.92(13) . . ? O6 C15 H15A 109.5 . . ? O6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 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 -178.66(13) . . . . ? C9 C1 C2 C3 1.12(14) . . . . ? O1 C1 C2 C10 0.6(2) . . . . ? C9 C1 C2 C10 -179.58(12) . . . . ? C10 C2 C3 C4 179.20(12) . . . . ? C1 C2 C3 C4 -1.48(14) . . . . ? C10 C2 C3 C1' -3.3(2) . . . . ? C1 C2 C3 C1' 175.97(12) . . . . ? C2 C3 C1' C6' 85.2(2) . . . . ? C4 C3 C1' C6' -97.67(18) . . . . ? C2 C3 C1' C2' -94.13(18) . . . . ? C4 C3 C1' C2' 82.99(18) . . . . ? C6' C1' C2' C3' -0.7(3) . . . . ? C3 C1' C2' C3' 178.66(17) . . . . ? C1' C2' C3' C4' -0.1(3) . . . . ? C2' C3' C4' C5' 0.9(3) . . . . ? C3' C4' C5' C6' -0.8(3) . . . . ? C2' C1' C6' C5' 0.8(3) . . . . ? C3 C1' C6' C5' -178.57(18) . . . . ? C4' C5' C6' C1' 0.0(3) . . . . ? C2 C3 C4 C5 -176.43(13) . . . . ? C1' C3 C4 C5 6.0(2) . . . . ? C2 C3 C4 C9 1.31(14) . . . . ? C1' C3 C4 C9 -176.25(12) . . . . ? C9 C4 C5 O4 179.65(11) . . . . ? C3 C4 C5 O4 -2.8(2) . . . . ? C9 C4 C5 C6 1.35(18) . . . . ? C3 C4 C5 C6 178.90(12) . . . . ? O4 C5 C6 O5 4.43(18) . . . . ? C4 C5 C6 O5 -177.25(11) . . . . ? O4 C5 C6 C7 179.69(12) . . . . ? C4 C5 C6 C7 -1.99(19) . . . . ? O5 C6 C7 O6 -2.15(19) . . . . ? C5 C6 C7 O6 -177.28(12) . . . . ? O5 C6 C7 C8 176.86(12) . . . . ? C5 C6 C7 C8 1.7(2) . . . . ? O6 C7 C8 C9 178.11(12) . . . . ? C6 C7 C8 C9 -0.81(19) . . . . ? C7 C8 C9 C4 0.19(19) . . . . ? C7 C8 C9 C1 -177.38(12) . . . . ? C5 C4 C9 C8 -0.49(19) . . . . ? C3 C4 C9 C8 -178.57(11) . . . . ? C5 C4 C9 C1 177.53(11) . . . . ? C3 C4 C9 C1 -0.55(13) . . . . ? O1 C1 C9 C8 -2.6(2) . . . . ? C2 C1 C9 C8 177.56(12) . . . . ? O1 C1 C9 C4 179.49(13) . . . . ? C2 C1 C9 C4 -0.30(13) . . . . ? C3 C2 C10 O2 -5.5(2) . . . . ? C1 C2 C10 O2 175.28(14) . . . . ? C3 C2 C10 O3 175.92(12) . . . . ? C1 C2 C10 O3 -3.3(2) . . . . ? O2 C10 O3 C11 -0.8(2) . . . . ? C2 C10 O3 C11 177.75(13) . . . . ? C10 O3 C11 C12 87.5(2) . . . . ? C4 C5 O4 C13 107.50(16) . . . . ? C6 C5 O4 C13 -74.24(17) . . . . ? C7 C6 O5 C14 77.1(2) . . . . ? C5 C6 O5 C14 -107.59(18) . . . . ? C8 C7 O6 C15 -5.7(2) . . . . ? C6 C7 O6 C15 173.30(13) . . . . ? _diffrn_measured_fraction_theta_max 0.854 _diffrn_reflns_theta_full 29.09 _diffrn_measured_fraction_theta_full 0.854 _refine_diff_density_max 0.181 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.043 data_vc1423-T1 _database_code_depnum_ccdc_archive 'CCDC 844785' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C44 H44 O10' _chemical_formula_sum 'C44 H44 O10' _chemical_formula_weight 732.79 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 Pnca _symmetry_space_group_name_Hall '-P 2a 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 19.246(3) _cell_length_b 23.211(5) _cell_length_c 17.018(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7602(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1603 _cell_measurement_theta_min 2.2869 _cell_measurement_theta_max 29.2031 _exptl_crystal_description prism _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_T_min 0.56081 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.0827 _diffrn_reflns_number 24447 _diffrn_reflns_av_R_equivalents 0.1977 _diffrn_reflns_av_sigmaI/netI 0.6142 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 29.27 _reflns_number_total 8903 _reflns_number_gt 1431 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0159P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8903 _refine_ls_number_parameters 495 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3901 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 0.652 _refine_ls_restrained_S_all 0.652 _refine_ls_shift/su_max 0.000 _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 0.4663(3) 0.3608(3) 0.3564(3) 0.0419(16) Uani 1 1 d . . . C2' C 0.4354(3) 0.3179(2) 0.3998(3) 0.0512(18) Uani 1 1 d . . . H2' H 0.3989 0.2972 0.3778 0.061 Uiso 1 1 calc R . . C3' C 0.4568(3) 0.3050(3) 0.4749(3) 0.066(2) Uani 1 1 d . . . H3' H 0.4359 0.2749 0.5020 0.079 Uiso 1 1 calc R . . C4' C 0.5092(3) 0.3364(3) 0.5101(3) 0.068(2) Uani 1 1 d . . . H4' H 0.5233 0.3286 0.5613 0.082 Uiso 1 1 calc R . . C5' C 0.5400(3) 0.3800(3) 0.4668(3) 0.084(2) Uani 1 1 d . . . H5' H 0.5760 0.4012 0.4890 0.100 Uiso 1 1 calc R . . C6' C 0.5184(3) 0.3928(2) 0.3912(3) 0.067(2) Uani 1 1 d . . . H6' H 0.5390 0.4230 0.3638 0.080 Uiso 1 1 calc R . . C1" C 0.2746(3) 0.3690(3) -0.1624(3) 0.0399(16) Uani 1 1 d . . . C2" C 0.2459(3) 0.4172(3) -0.1280(3) 0.0565(19) Uani 1 1 d . . . H2" H 0.2697 0.4365 -0.0884 0.068 Uiso 1 1 calc R . . C3" C 0.1809(4) 0.4370(3) -0.1530(4) 0.081(2) Uani 1 1 d . . . H3" H 0.1605 0.4693 -0.1303 0.097 Uiso 1 1 calc R . . C4" C 0.1484(3) 0.4071(3) -0.2121(4) 0.075(3) Uani 1 1 d . . . H4" H 0.1049 0.4194 -0.2290 0.089 Uiso 1 1 calc R . . C5" C 0.1778(4) 0.3595(3) -0.2475(3) 0.080(2) Uani 1 1 d . . . H5" H 0.1545 0.3405 -0.2877 0.096 Uiso 1 1 calc R . . C6" C 0.2428(3) 0.3403(2) -0.2222(3) 0.064(2) Uani 1 1 d . . . H6" H 0.2638 0.3086 -0.2457 0.076 Uiso 1 1 calc R . . C1 C 0.4285(3) 0.3751(2) 0.1361(3) 0.0370(15) Uani 1 1 d . . . C2 C 0.4557(3) 0.3450(3) 0.2097(3) 0.0363(15) Uani 1 1 d . . . C3 C 0.4439(3) 0.3750(3) 0.2749(3) 0.0396(16) Uani 1 1 d . . . C4 C 0.4052(3) 0.4274(3) 0.2527(3) 0.0350(15) Uani 1 1 d . . . C5 C 0.3789(3) 0.4709(3) 0.2995(3) 0.0443(17) Uani 1 1 d . . . C6 C 0.3444(3) 0.5163(3) 0.2628(3) 0.0429(17) Uani 1 1 d . . . C7 C 0.3384(3) 0.5175(3) 0.1825(3) 0.0384(15) Uani 1 1 d . . . C8 C 0.3617(3) 0.4733(3) 0.1355(3) 0.0409(16) Uani 1 1 d . . . H8 H 0.3550 0.4734 0.0814 0.049 Uiso 1 1 calc R . . C9 C 0.3955(3) 0.4286(3) 0.1733(3) 0.0380(16) Uani 1 1 d . . . C10 C 0.4915(3) 0.2893(3) 0.2014(3) 0.0472(18) Uani 1 1 d . . . O1 O 0.4988(2) 0.26372(17) 0.1401(2) 0.0719(14) Uani 1 1 d . . . O2 O 0.5153(2) 0.26956(17) 0.2694(2) 0.0688(13) Uani 1 1 d . . . C11 C 0.5494(3) 0.2141(3) 0.2673(3) 0.080(2) Uani 1 1 d . . . H11A H 0.5903 0.2158 0.2340 0.096 Uiso 1 1 calc R . . H11B H 0.5182 0.1851 0.2465 0.096 Uiso 1 1 calc R . . C12 C 0.5697(3) 0.1994(2) 0.3499(3) 0.093(2) Uani 1 1 d . . . H12A H 0.5865 0.1605 0.3518 0.139 Uiso 1 1 calc R . . H12B H 0.5299 0.2032 0.3836 0.139 Uiso 1 1 calc R . . H12C H 0.6056 0.2252 0.3671 0.139 Uiso 1 1 calc R . . O3 O 0.3873(2) 0.47268(16) 0.3788(2) 0.0641(13) Uani 1 1 d . . . C13 C 0.3344(3) 0.4470(3) 0.4238(3) 0.102(3) Uani 1 1 d . . . H13A H 0.3527 0.4358 0.4740 0.152 Uiso 1 1 calc R . . H13B H 0.3170 0.4136 0.3969 0.152 Uiso 1 1 calc R . . H13C H 0.2973 0.4741 0.4312 0.152 Uiso 1 1 calc R . . O4 O 0.31399(19) 0.55832(18) 0.3079(2) 0.0616(13) Uani 1 1 d . . . C14 C 0.3579(3) 0.6013(2) 0.3382(3) 0.106(3) Uani 1 1 d . . . H14A H 0.3311 0.6279 0.3691 0.159 Uiso 1 1 calc R . . H14B H 0.3797 0.6216 0.2957 0.159 Uiso 1 1 calc R . . H14C H 0.3929 0.5839 0.3706 0.159 Uiso 1 1 calc R . . O5 O 0.30660(17) 0.56673(17) 0.1534(2) 0.0548(12) Uani 1 1 d . . . C15 C 0.3057(3) 0.5750(2) 0.0713(3) 0.067(2) Uani 1 1 d . . . H15A H 0.2923 0.6140 0.0599 0.100 Uiso 1 1 calc R . . H15B H 0.2730 0.5490 0.0479 0.100 Uiso 1 1 calc R . . H15C H 0.3512 0.5678 0.0503 0.100 Uiso 1 1 calc R . . C16 C 0.4916(2) 0.3933(2) 0.0840(3) 0.0481(16) Uani 1 1 d . . . H16A H 0.5210 0.4188 0.1146 0.058 Uiso 1 1 calc R . . H16B H 0.5187 0.3591 0.0720 0.058 Uiso 1 1 calc R . . C17 C 0.4736(3) 0.4235(2) 0.0066(3) 0.0516(17) Uani 1 1 d . . . H17A H 0.4564 0.4620 0.0174 0.062 Uiso 1 1 calc R . . H17B H 0.5150 0.4269 -0.0255 0.062 Uiso 1 1 calc R . . C18 C 0.4195(3) 0.3901(2) -0.0371(3) 0.0409(16) Uani 1 1 d . . . C19 C 0.4008(3) 0.3906(2) -0.1118(3) 0.0390(16) Uani 1 1 d . . . C20 C 0.3425(3) 0.3461(2) -0.1268(3) 0.0393(16) Uani 1 1 d . . . H20 H 0.3606 0.3154 -0.1607 0.047 Uiso 1 1 calc R . . C21 C 0.3321(3) 0.3224(2) -0.0455(3) 0.0330(15) Uani 1 1 d . . . C22 C 0.2862(3) 0.2823(2) -0.0172(3) 0.0394(16) Uani 1 1 d . . . C23 C 0.2868(3) 0.2699(2) 0.0616(3) 0.0326(15) Uani 1 1 d . . . C24 C 0.3308(3) 0.2995(3) 0.1143(3) 0.0406(16) Uani 1 1 d . . . C25 C 0.3766(3) 0.3402(2) 0.0856(3) 0.0341(16) Uani 1 1 d . . . C26 C 0.3767(3) 0.3501(2) 0.0081(3) 0.0351(15) Uani 1 1 d . . . C27 C 0.4315(3) 0.4256(3) -0.1733(4) 0.059(2) Uani 1 1 d . . . O6 O 0.4703(2) 0.4657(2) -0.1621(3) 0.102(2) Uani 1 1 d . . . O7 O 0.41206(19) 0.40931(17) -0.2452(2) 0.0775(15) Uani 1 1 d . . . C28 C 0.4366(4) 0.4422(3) -0.3117(3) 0.125(3) Uani 1 1 d . . . H28A H 0.4623 0.4756 -0.2934 0.150 Uiso 1 1 calc R . . H28B H 0.4677 0.4187 -0.3431 0.150 Uiso 1 1 calc R . . C29 C 0.3800(4) 0.4603(3) -0.3581(4) 0.223(6) Uani 1 1 d . . . H29A H 0.3969 0.4767 -0.4062 0.334 Uiso 1 1 calc R . . H29B H 0.3537 0.4887 -0.3299 0.334 Uiso 1 1 calc R . . H29C H 0.3508 0.4279 -0.3697 0.334 Uiso 1 1 calc R . . O8 O 0.24362(19) 0.25238(15) -0.06827(18) 0.0523(11) Uani 1 1 d . . . C30 C 0.1709(3) 0.2639(2) -0.0602(3) 0.080(2) Uani 1 1 d . . . H30A H 0.1458 0.2444 -0.1011 0.119 Uiso 1 1 calc R . . H30B H 0.1629 0.3046 -0.0640 0.119 Uiso 1 1 calc R . . H30C H 0.1551 0.2504 -0.0099 0.119 Uiso 1 1 calc R . . O9 O 0.24416(18) 0.22799(18) 0.09311(18) 0.0519(12) Uani 1 1 d . . . C31 C 0.2638(3) 0.1720(2) 0.0723(3) 0.096(3) Uani 1 1 d . . . H31A H 0.2321 0.1449 0.0954 0.143 Uiso 1 1 calc R . . H31B H 0.3099 0.1645 0.0910 0.143 Uiso 1 1 calc R . . H31C H 0.2627 0.1681 0.0161 0.143 Uiso 1 1 calc R . . O10 O 0.32882(17) 0.28486(14) 0.19239(18) 0.0452(11) Uani 1 1 d . . . C32 C 0.2752(3) 0.3132(2) 0.2362(2) 0.067(2) Uani 1 1 d . . . H32A H 0.2799 0.3039 0.2909 0.101 Uiso 1 1 calc R . . H32B H 0.2306 0.3007 0.2176 0.101 Uiso 1 1 calc R . . H32C H 0.2793 0.3542 0.2293 0.101 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 C1' 0.029(4) 0.041(5) 0.055(4) 0.010(4) -0.011(3) 0.013(3) C2' 0.036(4) 0.055(5) 0.062(4) -0.003(4) -0.007(3) -0.013(4) C3' 0.072(6) 0.066(6) 0.059(4) 0.024(4) 0.005(4) 0.007(4) C4' 0.059(5) 0.091(7) 0.055(4) 0.007(4) -0.025(4) -0.007(4) C5' 0.067(6) 0.108(7) 0.077(5) 0.019(5) -0.031(4) -0.040(5) C6' 0.060(5) 0.078(6) 0.063(4) 0.021(4) -0.016(4) -0.028(4) C1" 0.035(4) 0.037(5) 0.048(4) 0.006(3) 0.003(3) 0.000(4) C2" 0.027(4) 0.068(6) 0.074(4) -0.014(4) 0.000(4) 0.005(4) C3" 0.059(6) 0.083(7) 0.099(5) -0.010(5) 0.002(4) 0.002(5) C4" 0.037(5) 0.099(8) 0.088(6) 0.023(5) -0.002(4) 0.009(5) C5" 0.062(6) 0.097(8) 0.080(5) 0.001(5) -0.030(5) -0.031(5) C6" 0.072(6) 0.061(6) 0.058(4) -0.008(4) -0.013(4) 0.007(4) C1 0.041(4) 0.034(5) 0.035(3) -0.001(3) -0.002(3) -0.010(3) C2 0.022(4) 0.028(4) 0.060(4) -0.004(4) -0.012(3) -0.006(3) C3 0.028(4) 0.038(5) 0.052(4) -0.006(4) -0.010(3) -0.003(3) C4 0.030(4) 0.028(4) 0.047(4) -0.011(3) -0.005(3) -0.005(3) C5 0.052(4) 0.055(5) 0.026(4) -0.004(4) -0.010(3) -0.014(4) C6 0.031(4) 0.048(6) 0.050(4) -0.011(4) 0.001(3) -0.002(4) C7 0.021(4) 0.040(5) 0.055(4) 0.012(4) -0.005(3) -0.007(3) C8 0.029(4) 0.043(5) 0.050(4) -0.008(4) -0.007(3) -0.004(3) C9 0.029(4) 0.051(5) 0.034(4) -0.012(3) -0.009(3) -0.012(4) C10 0.030(4) 0.058(6) 0.053(4) 0.004(4) -0.017(4) -0.011(4) O1 0.064(3) 0.081(4) 0.070(3) -0.021(3) -0.012(2) 0.019(3) O2 0.079(3) 0.060(4) 0.067(3) 0.002(2) -0.016(2) 0.033(3) C11 0.079(6) 0.069(6) 0.091(5) 0.008(5) -0.013(4) 0.032(4) C12 0.069(5) 0.099(7) 0.110(5) 0.030(5) 0.005(4) 0.034(4) O3 0.084(4) 0.057(3) 0.051(3) -0.001(2) -0.007(2) 0.006(3) C13 0.094(6) 0.146(8) 0.064(4) 0.020(4) 0.019(4) 0.025(5) O4 0.057(3) 0.059(4) 0.069(3) -0.014(3) -0.006(2) 0.005(3) C14 0.092(6) 0.075(6) 0.150(6) -0.061(5) -0.013(5) 0.002(5) O5 0.046(3) 0.052(3) 0.066(3) 0.016(2) -0.005(2) 0.012(2) C15 0.060(5) 0.068(6) 0.072(4) 0.037(4) -0.004(3) 0.007(4) C16 0.018(4) 0.054(5) 0.073(4) -0.015(3) -0.009(3) 0.001(3) C17 0.029(4) 0.060(5) 0.066(4) -0.001(4) 0.004(3) -0.009(4) C18 0.038(4) 0.033(5) 0.052(4) 0.002(4) 0.004(3) 0.004(3) C19 0.021(4) 0.053(5) 0.043(3) 0.004(4) 0.010(3) 0.004(3) C20 0.032(4) 0.045(5) 0.041(3) -0.001(3) 0.000(3) 0.000(4) C21 0.019(3) 0.042(5) 0.038(3) 0.011(3) 0.005(3) 0.008(3) C22 0.041(4) 0.041(5) 0.036(3) -0.001(3) -0.011(3) -0.005(4) C23 0.028(4) 0.024(4) 0.046(4) 0.004(3) 0.002(3) 0.000(3) C24 0.038(4) 0.060(5) 0.024(3) 0.009(3) 0.004(3) 0.015(4) C25 0.024(4) 0.046(5) 0.032(3) 0.003(3) -0.005(3) 0.011(3) C26 0.032(4) 0.035(5) 0.039(3) -0.001(3) -0.009(3) -0.003(3) C27 0.032(5) 0.096(8) 0.051(4) -0.007(5) 0.012(4) 0.019(4) O6 0.087(4) 0.117(5) 0.102(3) 0.018(3) 0.005(3) -0.052(3) O7 0.069(3) 0.100(5) 0.064(3) 0.029(3) 0.017(3) -0.008(3) C28 0.124(8) 0.167(9) 0.082(5) 0.068(6) 0.027(5) -0.008(6) C29 0.339(14) 0.188(11) 0.141(7) 0.114(7) -0.131(8) -0.168(10) O8 0.036(3) 0.062(3) 0.059(2) -0.011(2) -0.007(2) -0.021(3) C30 0.042(5) 0.102(7) 0.094(4) 0.004(4) -0.028(4) -0.027(5) O9 0.042(3) 0.047(3) 0.066(2) 0.007(3) 0.007(2) -0.019(3) C31 0.125(7) 0.050(6) 0.111(5) -0.004(5) 0.032(5) -0.034(5) O10 0.028(2) 0.063(3) 0.044(2) -0.001(2) -0.0013(18) -0.002(2) C32 0.062(5) 0.082(6) 0.058(4) -0.009(4) 0.008(3) 0.007(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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' C2' 1.375(6) . ? C1' C6' 1.381(6) . ? C1' C3 1.490(6) . ? C2' C3' 1.375(6) . ? C2' H2' 0.9300 . ? C3' C4' 1.382(7) . ? C3' H3' 0.9300 . ? C4' C5' 1.385(6) . ? C4' H4' 0.9300 . ? C5' C6' 1.384(6) . ? C5' H5' 0.9300 . ? C6' H6' 0.9300 . ? C1" C6" 1.362(6) . ? C1" C2" 1.377(6) . ? C1" C20 1.536(6) . ? C2" C3" 1.398(7) . ? C2" H2" 0.9300 . ? C3" C4" 1.374(7) . ? C3" H3" 0.9300 . ? C4" C5" 1.378(7) . ? C4" H4" 0.9300 . ? C5" C6" 1.396(7) . ? C5" H5" 0.9300 . ? C6" H6" 0.9300 . ? C1 C2 1.525(6) . ? C1 C9 1.531(6) . ? C1 C25 1.547(6) . ? C1 C16 1.563(6) . ? C2 C3 1.330(6) . ? C2 C10 1.473(7) . ? C3 C4 1.475(6) . ? C4 C9 1.365(5) . ? C4 C5 1.381(6) . ? C5 O3 1.360(5) . ? C5 C6 1.395(7) . ? C6 C7 1.371(6) . ? C6 O4 1.371(5) . ? C7 C8 1.377(6) . ? C7 O5 1.387(6) . ? C8 C9 1.384(6) . ? C8 H8 0.9300 . ? C10 O1 1.208(5) . ? C10 O2 1.326(5) . ? O2 C11 1.446(5) . ? C11 C12 1.498(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? O3 C13 1.407(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? O4 C14 1.406(5) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? O5 C15 1.411(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.533(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.496(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.321(6) . ? C18 C26 1.460(6) . ? C19 C27 1.450(7) . ? C19 C20 1.548(6) . ? C20 C21 1.501(5) . ? C20 H20 0.9800 . ? C21 C22 1.371(6) . ? C21 C26 1.408(6) . ? C22 C23 1.372(6) . ? C22 O8 1.382(5) . ? C23 O9 1.382(5) . ? C23 C24 1.411(6) . ? C24 O10 1.373(5) . ? C24 C25 1.379(6) . ? C25 C26 1.339(5) . ? C27 O6 1.208(7) . ? C27 O7 1.334(6) . ? O7 C28 1.446(6) . ? C28 C29 1.410(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? O8 C30 1.432(5) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? O9 C31 1.400(5) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? O10 C32 1.433(5) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 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 C2' C1' C6' 118.2(5) . . ? C2' C1' C3 122.3(6) . . ? C6' C1' C3 119.4(6) . . ? C3' C2' C1' 121.8(5) . . ? C3' C2' H2' 119.1 . . ? C1' C2' H2' 119.1 . . ? C2' C3' C4' 120.4(6) . . ? C2' C3' H3' 119.8 . . ? C4' C3' H3' 119.8 . . ? C3' C4' C5' 117.9(5) . . ? C3' C4' H4' 121.1 . . ? C5' C4' H4' 121.1 . . ? C6' C5' C4' 121.5(6) . . ? C6' C5' H5' 119.3 . . ? C4' C5' H5' 119.3 . . ? C1' C6' C5' 120.1(5) . . ? C1' C6' H6' 120.0 . . ? C5' C6' H6' 120.0 . . ? C6" C1" C2" 122.4(6) . . ? C6" C1" C20 120.5(6) . . ? C2" C1" C20 117.0(6) . . ? C1" C2" C3" 119.7(6) . . ? C1" C2" H2" 120.2 . . ? C3" C2" H2" 120.2 . . ? C4" C3" C2" 117.6(7) . . ? C4" C3" H3" 121.2 . . ? C2" C3" H3" 121.2 . . ? C3" C4" C5" 122.5(7) . . ? C3" C4" H4" 118.7 . . ? C5" C4" H4" 118.7 . . ? C4" C5" C6" 119.3(6) . . ? C4" C5" H5" 120.3 . . ? C6" C5" H5" 120.3 . . ? C1" C6" C5" 118.4(6) . . ? C1" C6" H6" 120.8 . . ? C5" C6" H6" 120.8 . . ? C2 C1 C9 100.0(4) . . ? C2 C1 C25 116.0(4) . . ? C9 C1 C25 112.7(4) . . ? C2 C1 C16 108.8(4) . . ? C9 C1 C16 109.7(4) . . ? C25 C1 C16 109.2(4) . . ? C3 C2 C10 128.2(5) . . ? C3 C2 C1 112.8(5) . . ? C10 C2 C1 119.0(5) . . ? C2 C3 C4 107.7(5) . . ? C2 C3 C1' 127.7(5) . . ? C4 C3 C1' 124.6(5) . . ? C9 C4 C5 120.4(6) . . ? C9 C4 C3 109.8(5) . . ? C5 C4 C3 129.8(5) . . ? O3 C5 C4 123.4(6) . . ? O3 C5 C6 118.6(6) . . ? C4 C5 C6 118.0(5) . . ? C7 C6 O4 120.6(6) . . ? C7 C6 C5 120.1(6) . . ? O4 C6 C5 119.3(5) . . ? C6 C7 C8 122.5(6) . . ? C6 C7 O5 114.1(6) . . ? C8 C7 O5 123.4(5) . . ? C7 C8 C9 116.2(5) . . ? C7 C8 H8 121.9 . . ? C9 C8 H8 121.9 . . ? C4 C9 C8 122.6(6) . . ? C4 C9 C1 109.7(5) . . ? C8 C9 C1 127.7(5) . . ? O1 C10 O2 122.9(6) . . ? O1 C10 C2 124.6(6) . . ? O2 C10 C2 112.5(5) . . ? C10 O2 C11 116.3(4) . . ? O2 C11 C12 107.2(5) . . ? O2 C11 H11A 110.3 . . ? C12 C11 H11A 110.3 . . ? O2 C11 H11B 110.3 . . ? C12 C11 H11B 110.3 . . ? H11A C11 H11B 108.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 O3 C13 116.2(4) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C6 O4 C14 117.0(4) . . ? O4 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 O5 C15 118.1(4) . . ? O5 C15 H15A 109.5 . . ? O5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C1 115.8(4) . . ? C17 C16 H16A 108.3 . . ? C1 C16 H16A 108.3 . . ? C17 C16 H16B 108.3 . . ? C1 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C18 C17 C16 110.4(4) . . ? C18 C17 H17A 109.6 . . ? C16 C17 H17A 109.6 . . ? C18 C17 H17B 109.6 . . ? C16 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C19 C18 C26 111.1(5) . . ? C19 C18 C17 131.5(6) . . ? C26 C18 C17 117.4(4) . . ? C18 C19 C27 126.1(6) . . ? C18 C19 C20 110.5(5) . . ? C27 C19 C20 123.4(5) . . ? C21 C20 C1" 112.2(4) . . ? C21 C20 C19 100.8(4) . . ? C1" C20 C19 116.8(5) . . ? C21 C20 H20 108.9 . . ? C1" C20 H20 108.9 . . ? C19 C20 H20 108.9 . . ? C22 C21 C26 118.3(5) . . ? C22 C21 C20 131.1(5) . . ? C26 C21 C20 110.5(5) . . ? C21 C22 C23 118.7(5) . . ? C21 C22 O8 120.2(5) . . ? C23 C22 O8 120.9(5) . . ? C22 C23 O9 121.5(5) . . ? C22 C23 C24 121.6(5) . . ? O9 C23 C24 117.0(5) . . ? O10 C24 C25 122.0(5) . . ? O10 C24 C23 118.5(5) . . ? C25 C24 C23 119.5(5) . . ? C26 C25 C24 117.9(5) . . ? C26 C25 C1 117.1(5) . . ? C24 C25 C1 125.0(4) . . ? C25 C26 C21 124.0(5) . . ? C25 C26 C18 129.0(5) . . ? C21 C26 C18 107.0(4) . . ? O6 C27 O7 122.4(7) . . ? O6 C27 C19 124.7(6) . . ? O7 C27 C19 112.9(6) . . ? C27 O7 C28 118.5(5) . . ? C29 C28 O7 110.1(6) . . ? C29 C28 H28A 109.6 . . ? O7 C28 H28A 109.6 . . ? C29 C28 H28B 109.6 . . ? O7 C28 H28B 109.6 . . ? H28A C28 H28B 108.2 . . ? 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 . . ? C22 O8 C30 115.2(4) . . ? O8 C30 H30A 109.5 . . ? O8 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O8 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C23 O9 C31 113.3(4) . . ? O9 C31 H31A 109.5 . . ? O9 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O9 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C24 O10 C32 114.1(4) . . ? O10 C32 H32A 109.5 . . ? O10 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O10 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 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 C6' C1' C2' C3' -2.7(9) . . . . ? C3 C1' C2' C3' 179.7(5) . . . . ? C1' C2' C3' C4' 2.2(9) . . . . ? C2' C3' C4' C5' -1.5(10) . . . . ? C3' C4' C5' C6' 1.4(10) . . . . ? C2' C1' C6' C5' 2.5(9) . . . . ? C3 C1' C6' C5' -179.8(5) . . . . ? C4' C5' C6' C1' -1.9(10) . . . . ? C6" C1" C2" C3" 2.0(9) . . . . ? C20 C1" C2" C3" -174.0(5) . . . . ? C1" C2" C3" C4" -0.5(9) . . . . ? C2" C3" C4" C5" -0.7(10) . . . . ? C3" C4" C5" C6" 0.6(11) . . . . ? C2" C1" C6" C5" -2.1(9) . . . . ? C20 C1" C6" C5" 173.8(5) . . . . ? C4" C5" C6" C1" 0.8(9) . . . . ? C9 C1 C2 C3 -2.0(6) . . . . ? C25 C1 C2 C3 -123.5(5) . . . . ? C16 C1 C2 C3 112.9(5) . . . . ? C9 C1 C2 C10 179.0(5) . . . . ? C25 C1 C2 C10 57.5(7) . . . . ? C16 C1 C2 C10 -66.1(6) . . . . ? C10 C2 C3 C4 -179.1(5) . . . . ? C1 C2 C3 C4 2.0(6) . . . . ? C10 C2 C3 C1' 2.6(10) . . . . ? C1 C2 C3 C1' -176.3(5) . . . . ? C2' C1' C3 C2 -74.1(8) . . . . ? C6' C1' C3 C2 108.2(7) . . . . ? C2' C1' C3 C4 107.8(7) . . . . ? C6' C1' C3 C4 -69.8(7) . . . . ? C2 C3 C4 C9 -1.1(6) . . . . ? C1' C3 C4 C9 177.3(5) . . . . ? C2 C3 C4 C5 177.4(5) . . . . ? C1' C3 C4 C5 -4.2(9) . . . . ? C9 C4 C5 O3 -179.4(5) . . . . ? C3 C4 C5 O3 2.3(9) . . . . ? C9 C4 C5 C6 -2.0(8) . . . . ? C3 C4 C5 C6 179.7(5) . . . . ? O3 C5 C6 C7 176.3(4) . . . . ? C4 C5 C6 C7 -1.2(8) . . . . ? O3 C5 C6 O4 -6.4(8) . . . . ? C4 C5 C6 O4 176.1(5) . . . . ? O4 C6 C7 C8 -173.0(5) . . . . ? C5 C6 C7 C8 4.3(8) . . . . ? O4 C6 C7 O5 6.4(7) . . . . ? C5 C6 C7 O5 -176.3(5) . . . . ? C6 C7 C8 C9 -3.9(8) . . . . ? O5 C7 C8 C9 176.8(4) . . . . ? C5 C4 C9 C8 2.3(8) . . . . ? C3 C4 C9 C8 -179.0(5) . . . . ? C5 C4 C9 C1 -178.9(5) . . . . ? C3 C4 C9 C1 -0.2(6) . . . . ? C7 C8 C9 C4 0.6(8) . . . . ? C7 C8 C9 C1 -178.0(5) . . . . ? C2 C1 C9 C4 1.3(6) . . . . ? C25 C1 C9 C4 125.1(5) . . . . ? C16 C1 C9 C4 -113.0(5) . . . . ? C2 C1 C9 C8 180.0(5) . . . . ? C25 C1 C9 C8 -56.2(7) . . . . ? C16 C1 C9 C8 65.7(7) . . . . ? C3 C2 C10 O1 178.0(6) . . . . ? C1 C2 C10 O1 -3.1(9) . . . . ? C3 C2 C10 O2 -2.0(8) . . . . ? C1 C2 C10 O2 176.8(4) . . . . ? O1 C10 O2 C11 -1.9(8) . . . . ? C2 C10 O2 C11 178.2(5) . . . . ? C10 O2 C11 C12 -178.0(5) . . . . ? C4 C5 O3 C13 -92.1(6) . . . . ? C6 C5 O3 C13 90.6(7) . . . . ? C7 C6 O4 C14 -102.8(6) . . . . ? C5 C6 O4 C14 79.9(7) . . . . ? C6 C7 O5 C15 172.5(4) . . . . ? C8 C7 O5 C15 -8.1(7) . . . . ? C2 C1 C16 C17 179.1(4) . . . . ? C9 C1 C16 C17 -72.4(5) . . . . ? C25 C1 C16 C17 51.6(6) . . . . ? C1 C16 C17 C18 -49.2(6) . . . . ? C16 C17 C18 C19 -160.7(6) . . . . ? C16 C17 C18 C26 21.2(7) . . . . ? C26 C18 C19 C27 179.4(5) . . . . ? C17 C18 C19 C27 1.1(10) . . . . ? C26 C18 C19 C20 -3.1(7) . . . . ? C17 C18 C19 C20 178.7(5) . . . . ? C6" C1" C20 C21 -108.9(6) . . . . ? C2" C1" C20 C21 67.2(6) . . . . ? C6" C1" C20 C19 135.4(5) . . . . ? C2" C1" C20 C19 -48.5(7) . . . . ? C18 C19 C20 C21 1.2(6) . . . . ? C27 C19 C20 C21 178.8(5) . . . . ? C18 C19 C20 C1" 123.1(5) . . . . ? C27 C19 C20 C1" -59.3(7) . . . . ? C1" C20 C21 C22 52.8(8) . . . . ? C19 C20 C21 C22 177.8(6) . . . . ? C1" C20 C21 C26 -123.9(5) . . . . ? C19 C20 C21 C26 1.1(6) . . . . ? C26 C21 C22 C23 -1.5(8) . . . . ? C20 C21 C22 C23 -178.0(5) . . . . ? C26 C21 C22 O8 -177.3(5) . . . . ? C20 C21 C22 O8 6.3(9) . . . . ? C21 C22 C23 O9 -176.9(5) . . . . ? O8 C22 C23 O9 -1.2(8) . . . . ? C21 C22 C23 C24 3.4(8) . . . . ? O8 C22 C23 C24 179.1(5) . . . . ? C22 C23 C24 O10 -179.9(4) . . . . ? O9 C23 C24 O10 0.4(7) . . . . ? C22 C23 C24 C25 -3.0(8) . . . . ? O9 C23 C24 C25 177.3(5) . . . . ? O10 C24 C25 C26 177.4(4) . . . . ? C23 C24 C25 C26 0.6(8) . . . . ? O10 C24 C25 C1 -2.1(8) . . . . ? C23 C24 C25 C1 -178.9(5) . . . . ? C2 C1 C25 C26 -149.1(5) . . . . ? C9 C1 C25 C26 96.4(5) . . . . ? C16 C1 C25 C26 -25.8(7) . . . . ? C2 C1 C25 C24 30.4(8) . . . . ? C9 C1 C25 C24 -84.1(6) . . . . ? C16 C1 C25 C24 153.7(5) . . . . ? C24 C25 C26 C21 1.2(8) . . . . ? C1 C25 C26 C21 -179.2(5) . . . . ? C24 C25 C26 C18 -179.7(5) . . . . ? C1 C25 C26 C18 -0.2(8) . . . . ? C22 C21 C26 C25 -0.8(8) . . . . ? C20 C21 C26 C25 176.4(5) . . . . ? C22 C21 C26 C18 180.0(5) . . . . ? C20 C21 C26 C18 -2.9(6) . . . . ? C19 C18 C26 C25 -175.4(5) . . . . ? C17 C18 C26 C25 3.1(8) . . . . ? C19 C18 C26 C21 3.8(6) . . . . ? C17 C18 C26 C21 -177.7(5) . . . . ? C18 C19 C27 O6 -13.0(11) . . . . ? C20 C19 C27 O6 169.8(7) . . . . ? C18 C19 C27 O7 167.6(5) . . . . ? C20 C19 C27 O7 -9.7(8) . . . . ? O6 C27 O7 C28 -2.1(10) . . . . ? C19 C27 O7 C28 177.4(5) . . . . ? C27 O7 C28 C29 -125.7(7) . . . . ? C21 C22 O8 C30 -114.4(6) . . . . ? C23 C22 O8 C30 70.0(6) . . . . ? C22 C23 O9 C31 70.8(6) . . . . ? C24 C23 O9 C31 -109.5(5) . . . . ? C25 C24 O10 C32 98.4(6) . . . . ? C23 C24 O10 C32 -84.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 29.27 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 0.174 _refine_diff_density_min -0.161 _refine_diff_density_rms 0.040 data_vc1423-T2 _database_code_depnum_ccdc_archive 'CCDC 844786' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C44 H44 O10' _chemical_formula_sum 'C44 H44 O10' _chemical_formula_weight 732.79 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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.914 _cell_length_b 18.910 _cell_length_c 20.176 _cell_angle_alpha 63.59 _cell_angle_beta 82.53 _cell_angle_gamma 74.28 _cell_volume 3918.6 _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7040 _cell_measurement_theta_min 2.2341 _cell_measurement_theta_max 29.0480 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_T_min 0.99489 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.0827 _diffrn_reflns_number 30528 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.1007 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 29.11 _reflns_number_total 17688 _reflns_number_gt 7033 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0628P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17688 _refine_ls_number_parameters 989 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1392 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.799 _refine_ls_shift/su_max 0.000 _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 C1A C -0.14748(18) 0.34927(12) 0.29769(11) 0.0476(5) Uani 1 1 d . . . C2A C -0.07313(19) 0.40274(13) 0.23923(12) 0.0517(6) Uani 1 1 d . . . C3A C -0.00716(18) 0.36415(13) 0.19928(12) 0.0490(5) Uani 1 1 d . . . C1'A C 0.0885(2) 0.39097(13) 0.14650(13) 0.0565(6) Uani 1 1 d . . . C2'A C 0.0842(2) 0.40944(15) 0.07244(15) 0.0757(7) Uani 1 1 d . . . H2'A H 0.0191 0.4056 0.0544 0.091 Uiso 1 1 calc R . . C3'A C 0.1743(3) 0.43340(18) 0.02474(17) 0.0978(9) Uani 1 1 d . . . H3'A H 0.1696 0.4464 -0.0252 0.117 Uiso 1 1 calc R . . C4'A C 0.2717(3) 0.43799(19) 0.0513(2) 0.1087(11) Uani 1 1 d . . . H4'A H 0.3331 0.4538 0.0193 0.130 Uiso 1 1 calc R . . C5'A C 0.2783(3) 0.4193(2) 0.1245(2) 0.1061(11) Uani 1 1 d . . . H5'A H 0.3441 0.4223 0.1425 0.127 Uiso 1 1 calc R . . C6'A C 0.1874(2) 0.39613(16) 0.17147(16) 0.0784(8) Uani 1 1 d . . . H6'A H 0.1925 0.3836 0.2213 0.094 Uiso 1 1 calc R . . C4A C -0.04029(18) 0.28774(12) 0.22030(11) 0.0466(5) Uani 1 1 d . . . C5A C 0.00268(18) 0.22463(13) 0.19841(11) 0.0472(5) Uani 1 1 d . . . C6A C -0.04743(18) 0.15848(13) 0.22757(12) 0.0505(6) Uani 1 1 d . . . C7A C -0.13982(18) 0.15413(13) 0.27823(12) 0.0499(6) Uani 1 1 d . . . C8A C -0.18095(18) 0.21565(13) 0.30211(11) 0.0504(6) Uani 1 1 d . . . H8A H -0.2417 0.2128 0.3365 0.060 Uiso 1 1 calc R . . C9A C -0.12983(18) 0.28068(12) 0.27379(11) 0.0454(5) Uani 1 1 d . . . C10A C -0.0746(2) 0.48215(16) 0.23589(17) 0.0673(7) Uani 1 1 d . . . O1A O -0.10683(19) 0.50147(11) 0.28565(12) 0.1035(7) Uani 1 1 d . . . O2A O -0.03963(16) 0.53207(10) 0.17023(11) 0.0908(6) Uani 1 1 d . . . C11A C -0.0347(3) 0.61184(18) 0.1616(2) 0.1266(13) Uani 1 1 d . . . H11A H -0.1131 0.6461 0.1570 0.152 Uiso 1 1 calc R . . H11B H 0.0001 0.6063 0.2051 0.152 Uiso 1 1 calc R . . C12A C 0.0315(4) 0.6483(2) 0.0984(3) 0.224(3) Uani 1 1 d . . . H12A H 0.1119 0.6193 0.1066 0.336 Uiso 1 1 calc R . . H12B H 0.0243 0.7038 0.0889 0.336 Uiso 1 1 calc R . . H12C H 0.0036 0.6468 0.0567 0.336 Uiso 1 1 calc R . . O3A O 0.09267(14) 0.22747(9) 0.14754(8) 0.0637(4) Uani 1 1 d . . . C13A C 0.2040(2) 0.18429(18) 0.18091(17) 0.0966(9) Uani 1 1 d . . . H13A H 0.2219 0.2092 0.2093 0.145 Uiso 1 1 calc R . . H13B H 0.2624 0.1858 0.1431 0.145 Uiso 1 1 calc R . . H13C H 0.2026 0.1288 0.2128 0.145 Uiso 1 1 calc R . . O4A O 0.00090(13) 0.09397(9) 0.20944(9) 0.0635(4) Uani 1 1 d . . . C14A C -0.0683(2) 0.08428(18) 0.16292(16) 0.0952(9) Uani 1 1 d . . . H14A H -0.1439 0.0801 0.1852 0.143 Uiso 1 1 calc R . . H14B H -0.0311 0.0358 0.1567 0.143 Uiso 1 1 calc R . . H14C H -0.0765 0.1305 0.1155 0.143 Uiso 1 1 calc R . . O5A O -0.17921(14) 0.08554(9) 0.30324(10) 0.0729(5) Uani 1 1 d . . . C15A C -0.2864(2) 0.08185(15) 0.34167(15) 0.0828(8) Uani 1 1 d . . . H15A H -0.2784 0.0788 0.3897 0.124 Uiso 1 1 calc R . . H15B H -0.3091 0.0345 0.3471 0.124 Uiso 1 1 calc R . . H15C H -0.3448 0.1297 0.3144 0.124 Uiso 1 1 calc R . . C16A C -0.08309(19) 0.31283(13) 0.37289(12) 0.0565(6) Uani 1 1 d . . . H16A H -0.0162 0.2697 0.3737 0.068 Uiso 1 1 calc R . . H16B H -0.0539 0.3549 0.3751 0.068 Uiso 1 1 calc R . . C17A C -0.1574(2) 0.27881(13) 0.44212(12) 0.0600(6) Uani 1 1 d . . . H17A H -0.1876 0.2363 0.4415 0.072 Uiso 1 1 calc R . . H17B H -0.1110 0.2560 0.4862 0.072 Uiso 1 1 calc R . . C18A C -0.25668(19) 0.34883(12) 0.44156(11) 0.0509(6) Uani 1 1 d . . . H18A H -0.2203 0.3900 0.4405 0.061 Uiso 1 1 calc R . . C19A C -0.3520(2) 0.34198(12) 0.49863(12) 0.0509(6) Uani 1 1 d . . . C20A C -0.4581(2) 0.38046(12) 0.46568(12) 0.0516(6) Uani 1 1 d . . . C1'B C -0.5728(2) 0.38865(13) 0.50367(12) 0.0506(6) Uani 1 1 d . . . C2'B C -0.6471(2) 0.46413(14) 0.48840(13) 0.0651(7) Uani 1 1 d . . . H2'B H -0.6253 0.5108 0.4535 0.078 Uiso 1 1 calc R . . C3'B C -0.7535(3) 0.47070(18) 0.52469(17) 0.0812(8) Uani 1 1 d . . . H3'B H -0.8028 0.5218 0.5141 0.097 Uiso 1 1 calc R . . C4'B C -0.7869(3) 0.4021(2) 0.57635(18) 0.0903(9) Uani 1 1 d . . . H4'B H -0.8583 0.4068 0.6008 0.108 Uiso 1 1 calc R . . C5'B C -0.7141(3) 0.32689(19) 0.59151(15) 0.0830(8) Uani 1 1 d . . . H5'B H -0.7364 0.2803 0.6260 0.100 Uiso 1 1 calc R . . C6'B C -0.6078(2) 0.32050(14) 0.55551(13) 0.0642(7) Uani 1 1 d . . . H6'B H -0.5587 0.2693 0.5664 0.077 Uiso 1 1 calc R . . C21A C -0.44125(19) 0.41062(11) 0.38467(11) 0.0457(5) Uani 1 1 d . . . C22A C -0.51678(19) 0.44840(12) 0.32523(12) 0.0493(5) Uani 1 1 d . . . C23A C -0.4705(2) 0.45782(12) 0.25553(12) 0.0497(6) Uani 1 1 d . . . C24A C -0.3527(2) 0.42699(12) 0.24509(12) 0.0486(5) Uani 1 1 d . . . C25A C -0.27467(18) 0.39015(11) 0.30354(11) 0.0440(5) Uani 1 1 d . . . C26A C -0.32259(19) 0.38716(11) 0.37082(12) 0.0446(5) Uani 1 1 d . . . C27A C -0.3288(2) 0.31301(14) 0.57709(14) 0.0625(6) Uani 1 1 d . . . O6A O -0.39301(19) 0.28963(14) 0.62863(11) 0.1176(8) Uani 1 1 d . . . O7A O -0.22357(17) 0.31818(12) 0.58649(9) 0.0908(6) Uani 1 1 d . . . C28A C -0.1936(3) 0.2982(3) 0.66187(16) 0.1281(13) Uani 1 1 d . . . H28A H -0.2643 0.3044 0.6907 0.154 Uiso 1 1 calc R . . H28B H -0.1495 0.2421 0.6853 0.154 Uiso 1 1 calc R . . C29A C -0.1276(5) 0.3498(2) 0.6597(2) 0.232(3) Uani 1 1 d . . . H29A H -0.0464 0.3261 0.6554 0.348 Uiso 1 1 calc R . . H29B H -0.1409 0.3573 0.7044 0.348 Uiso 1 1 calc R . . H29C H -0.1501 0.4014 0.6179 0.348 Uiso 1 1 calc R . . O8A O -0.63328(14) 0.47990(10) 0.33365(9) 0.0693(5) Uani 1 1 d . . . C30A C -0.7145(2) 0.43987(18) 0.32839(18) 0.1036(10) Uani 1 1 d . . . H30A H -0.7129 0.4443 0.2790 0.155 Uiso 1 1 calc R . . H30B H -0.7913 0.4647 0.3399 0.155 Uiso 1 1 calc R . . H30C H -0.6941 0.3835 0.3627 0.155 Uiso 1 1 calc R . . O9A O -0.54474(14) 0.49480(10) 0.19527(9) 0.0727(5) Uani 1 1 d . . . C31A C -0.5679(4) 0.5798(2) 0.1603(2) 0.182(2) Uani 1 1 d . . . H31A H -0.5892 0.6009 0.1967 0.273 Uiso 1 1 calc R . . H31B H -0.6308 0.6007 0.1262 0.273 Uiso 1 1 calc R . . H31C H -0.4995 0.5962 0.1338 0.273 Uiso 1 1 calc R . . O10A O -0.30845(13) 0.43667(9) 0.17550(8) 0.0642(4) Uani 1 1 d . . . C32A C -0.3451(2) 0.39342(18) 0.14316(14) 0.0924(9) Uani 1 1 d . . . H32A H -0.3411 0.3385 0.1793 0.139 Uiso 1 1 calc R . . H32B H -0.2951 0.3932 0.1019 0.139 Uiso 1 1 calc R . . H32C H -0.4239 0.4194 0.1265 0.139 Uiso 1 1 calc R . . C1B C -0.42659(17) -0.04655(11) 0.19373(10) 0.0410(5) Uani 1 1 d . . . C2B C -0.38881(18) 0.02588(12) 0.13082(11) 0.0461(5) Uani 1 1 d . . . C3B C -0.34551(17) 0.00902(13) 0.07249(11) 0.0460(5) Uani 1 1 d . . . C1'C C -0.29434(19) 0.06257(13) 0.00295(11) 0.0512(6) Uani 1 1 d . . . C2'C C -0.1808(2) 0.06702(18) 0.00203(14) 0.0879(9) Uani 1 1 d . . . H2'C H -0.1369 0.0362 0.0449 0.106 Uiso 1 1 calc R . . C3'C C -0.1312(3) 0.1161(2) -0.06105(17) 0.1228(13) Uani 1 1 d . . . H3'C H -0.0540 0.1181 -0.0611 0.147 Uiso 1 1 calc R . . C4'C C -0.1966(3) 0.1625(2) -0.12442(16) 0.1195(13) Uani 1 1 d . . . H4'C H -0.1642 0.1972 -0.1669 0.143 Uiso 1 1 calc R . . C5'C C -0.3081(3) 0.15761(18) -0.12514(14) 0.0963(10) Uani 1 1 d . . . H5'C H -0.3516 0.1880 -0.1682 0.116 Uiso 1 1 calc R . . C6'C C -0.3564(2) 0.10742(15) -0.06158(13) 0.0684(7) Uani 1 1 d . . . H6'C H -0.4324 0.1038 -0.0623 0.082 Uiso 1 1 calc R . . C4B C -0.34824(17) -0.07471(12) 0.09085(11) 0.0435(5) Uani 1 1 d . . . C5B C -0.31596(18) -0.12058(14) 0.05038(12) 0.0516(6) Uani 1 1 d . . . C6B C -0.32186(19) -0.20129(15) 0.08357(13) 0.0565(6) Uani 1 1 d . . . C7B C -0.35993(19) -0.23692(14) 0.15742(13) 0.0526(6) Uani 1 1 d . . . C8B C -0.39524(17) -0.19017(13) 0.19733(11) 0.0472(5) Uani 1 1 d . . . H8B H -0.4219 -0.2127 0.2459 0.057 Uiso 1 1 calc R . . C9B C -0.38964(16) -0.10989(12) 0.16290(11) 0.0412(5) Uani 1 1 d . . . C10B C -0.4038(2) 0.10088(14) 0.13979(14) 0.0585(6) Uani 1 1 d . . . O1B O -0.45559(17) 0.11284(10) 0.19066(10) 0.0874(6) Uani 1 1 d . . . O2B O -0.35355(16) 0.15591(10) 0.08557(9) 0.0806(5) Uani 1 1 d . . . C11B C -0.3643(3) 0.23122(16) 0.09065(16) 0.1063(11) Uani 1 1 d . . . H11C H -0.3297 0.2208 0.1360 0.128 Uiso 1 1 calc R . . H11D H -0.4457 0.2592 0.0902 0.128 Uiso 1 1 calc R . . C12B C -0.3016(4) 0.2812(2) 0.02517(19) 0.179(2) Uani 1 1 d . . . H12D H -0.2200 0.2661 0.0358 0.268 Uiso 1 1 calc R . . H12E H -0.3322 0.3377 0.0140 0.268 Uiso 1 1 calc R . . H12F H -0.3121 0.2721 -0.0166 0.268 Uiso 1 1 calc R . . O3B O -0.28856(15) -0.08408(10) -0.02389(9) 0.0716(5) Uani 1 1 d . . . C13B C -0.1707(3) -0.1059(2) -0.04298(17) 0.1107(11) Uani 1 1 d . . . H13D H -0.1227 -0.0974 -0.0137 0.166 Uiso 1 1 calc R . . H13E H -0.1588 -0.0729 -0.0945 0.166 Uiso 1 1 calc R . . H13F H -0.1500 -0.1621 -0.0338 0.166 Uiso 1 1 calc R . . O4B O -0.28686(15) -0.24804(10) 0.04430(9) 0.0787(5) Uani 1 1 d . . . C14B C -0.3804(3) -0.2529(2) 0.01026(17) 0.1155(11) Uani 1 1 d . . . H14D H -0.4409 -0.2683 0.0462 0.173 Uiso 1 1 calc R . . H14E H -0.3523 -0.2927 -0.0091 0.173 Uiso 1 1 calc R . . H14F H -0.4109 -0.2008 -0.0293 0.173 Uiso 1 1 calc R . . O5B O -0.36146(15) -0.31656(10) 0.18390(9) 0.0744(5) Uani 1 1 d . . . C15B C -0.3875(3) -0.35889(15) 0.26005(15) 0.0894(9) Uani 1 1 d . . . H15D H -0.3350 -0.3543 0.2894 0.134 Uiso 1 1 calc R . . H15E H -0.3788 -0.4152 0.2720 0.134 Uiso 1 1 calc R . . H15F H -0.4663 -0.3358 0.2703 0.134 Uiso 1 1 calc R . . C16B C -0.56263(17) -0.02571(13) 0.20207(11) 0.0518(6) Uani 1 1 d . . . H16C H -0.5898 0.0322 0.1882 0.062 Uiso 1 1 calc R . . H16D H -0.5952 -0.0372 0.1673 0.062 Uiso 1 1 calc R . . C17B C -0.61050(18) -0.07121(13) 0.27919(11) 0.0508(6) Uani 1 1 d . . . H17C H -0.5876 -0.1294 0.2939 0.061 Uiso 1 1 calc R . . H17D H -0.6950 -0.0543 0.2799 0.061 Uiso 1 1 calc R . . C18B C -0.55871(17) -0.04990(12) 0.33147(10) 0.0417(5) Uani 1 1 d . . . H18B H -0.5795 0.0095 0.3120 0.050 Uiso 1 1 calc R . . C19B C -0.58303(18) -0.08307(12) 0.41343(11) 0.0420(5) Uani 1 1 d . . . C20B C -0.48147(17) -0.11371(11) 0.45197(11) 0.0403(5) Uani 1 1 d . . . C1'D C -0.46622(17) -0.14664(12) 0.53274(11) 0.0408(5) Uani 1 1 d . . . C2'D C -0.50409(19) -0.21507(12) 0.58191(12) 0.0505(6) Uani 1 1 d . . . H2'D H -0.5432 -0.2396 0.5644 0.061 Uiso 1 1 calc R . . C3'D C -0.4840(2) -0.24707(13) 0.65696(12) 0.0613(6) Uani 1 1 d . . . H3'D H -0.5100 -0.2929 0.6896 0.074 Uiso 1 1 calc R . . C4'D C -0.4257(2) -0.21145(15) 0.68371(13) 0.0644(7) Uani 1 1 d . . . H4'D H -0.4119 -0.2334 0.7341 0.077 Uiso 1 1 calc R . . C5'D C -0.3882(2) -0.14331(15) 0.63548(13) 0.0602(6) Uani 1 1 d . . . H5'D H -0.3494 -0.1189 0.6534 0.072 Uiso 1 1 calc R . . C6'D C -0.40805(19) -0.11113(13) 0.56067(12) 0.0521(6) Uani 1 1 d . . . H6'D H -0.3822 -0.0651 0.5284 0.063 Uiso 1 1 calc R . . C21B C -0.38285(17) -0.10989(11) 0.39895(10) 0.0381(5) Uani 1 1 d . . . C22B C -0.26276(18) -0.13769(11) 0.40697(11) 0.0422(5) Uani 1 1 d . . . C23B C -0.19351(17) -0.13266(12) 0.34420(12) 0.0444(5) Uani 1 1 d . . . C24B C -0.24417(18) -0.10323(12) 0.27509(11) 0.0431(5) Uani 1 1 d . . . C25B C -0.36457(17) -0.07450(11) 0.26622(10) 0.0379(5) Uani 1 1 d . . . C26B C -0.42918(16) -0.07570(11) 0.32834(11) 0.0377(5) Uani 1 1 d . . . C27B C -0.70154(19) -0.06875(14) 0.44305(13) 0.0491(5) Uani 1 1 d . . . O6B O -0.77402(13) -0.00899(9) 0.38961(8) 0.0659(4) Uani 1 1 d . . . O7B O -0.73417(14) -0.10371(11) 0.50511(9) 0.0805(5) Uani 1 1 d . . . C28B C -0.89520(19) 0.01604(16) 0.40908(15) 0.0750(7) Uani 1 1 d . . . H28C H -0.9160 -0.0279 0.4532 0.090 Uiso 1 1 calc R . . H28D H -0.9449 0.0277 0.3692 0.090 Uiso 1 1 calc R . . C29B C -0.9144(2) 0.08834(17) 0.42247(16) 0.0949(9) Uani 1 1 d . . . H29D H -0.8712 0.0752 0.4651 0.142 Uiso 1 1 calc R . . H29E H -0.9960 0.1067 0.4310 0.142 Uiso 1 1 calc R . . H29F H -0.8885 0.1306 0.3801 0.142 Uiso 1 1 calc R . . O8B O -0.20990(12) -0.16584(9) 0.47377(8) 0.0587(4) Uani 1 1 d . . . C30B C -0.1759(2) -0.25180(16) 0.51384(14) 0.0896(9) Uani 1 1 d . . . H30D H -0.2411 -0.2745 0.5185 0.134 Uiso 1 1 calc R . . H30E H -0.1503 -0.2655 0.5622 0.134 Uiso 1 1 calc R . . H30F H -0.1133 -0.2735 0.4879 0.134 Uiso 1 1 calc R . . O9B O -0.07366(12) -0.16152(9) 0.35108(8) 0.0558(4) Uani 1 1 d . . . C31B C -0.0144(2) -0.10828(16) 0.35503(17) 0.0941(9) Uani 1 1 d . . . H31D H -0.0221 -0.0604 0.3089 0.141 Uiso 1 1 calc R . . H31E H 0.0666 -0.1350 0.3645 0.141 Uiso 1 1 calc R . . H31F H -0.0475 -0.0933 0.3943 0.141 Uiso 1 1 calc R . . O10B O -0.17512(12) -0.09884(9) 0.21356(7) 0.0562(4) Uani 1 1 d . . . C32B C -0.1091(2) -0.17503(16) 0.21503(14) 0.0779(8) Uani 1 1 d . . . H32D H -0.0362 -0.1907 0.2392 0.117 Uiso 1 1 calc R . . H32E H -0.0945 -0.1697 0.1653 0.117 Uiso 1 1 calc R . . H32F H -0.1522 -0.2158 0.2416 0.117 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 C1A 0.0539(14) 0.0453(13) 0.0470(14) -0.0200(11) 0.0004(11) -0.0174(11) C2A 0.0558(14) 0.0493(14) 0.0557(15) -0.0238(12) 0.0000(12) -0.0194(12) C3A 0.0476(13) 0.0490(14) 0.0503(14) -0.0186(11) -0.0026(11) -0.0152(11) C1'A 0.0537(15) 0.0496(14) 0.0621(17) -0.0197(12) 0.0059(13) -0.0168(12) C2'A 0.0717(18) 0.0821(19) 0.0595(18) -0.0159(14) 0.0045(15) -0.0250(15) C3'A 0.101(3) 0.097(2) 0.069(2) -0.0171(16) 0.0231(19) -0.025(2) C4'A 0.083(3) 0.100(3) 0.125(3) -0.033(2) 0.040(2) -0.041(2) C5'A 0.068(2) 0.127(3) 0.137(3) -0.057(3) 0.017(2) -0.051(2) C6'A 0.0650(18) 0.095(2) 0.088(2) -0.0426(17) 0.0040(16) -0.0357(16) C4A 0.0476(13) 0.0481(14) 0.0465(14) -0.0193(11) -0.0011(11) -0.0164(11) C5A 0.0438(13) 0.0543(15) 0.0448(13) -0.0237(11) 0.0031(11) -0.0112(12) C6A 0.0468(14) 0.0510(15) 0.0605(15) -0.0305(12) 0.0007(12) -0.0112(12) C7A 0.0491(14) 0.0445(14) 0.0602(15) -0.0250(12) 0.0033(12) -0.0149(11) C8A 0.0469(13) 0.0502(14) 0.0542(14) -0.0240(11) 0.0082(11) -0.0130(11) C9A 0.0499(14) 0.0418(13) 0.0455(13) -0.0184(10) 0.0001(11) -0.0135(11) C10A 0.0681(17) 0.0630(18) 0.080(2) -0.0347(16) 0.0078(15) -0.0271(14) O1A 0.1498(19) 0.0810(14) 0.1084(16) -0.0618(13) 0.0243(14) -0.0467(13) O2A 0.1076(15) 0.0515(11) 0.1109(16) -0.0319(11) 0.0289(12) -0.0348(10) C11A 0.151(3) 0.059(2) 0.170(4) -0.048(2) 0.035(3) -0.045(2) C12A 0.246(6) 0.111(3) 0.305(7) -0.075(4) 0.136(5) -0.116(4) O3A 0.0592(11) 0.0720(11) 0.0636(11) -0.0345(9) 0.0159(9) -0.0195(9) C13A 0.0514(18) 0.117(2) 0.117(3) -0.055(2) 0.0128(17) -0.0103(17) O4A 0.0599(10) 0.0660(11) 0.0828(12) -0.0495(9) 0.0045(9) -0.0148(8) C14A 0.094(2) 0.124(3) 0.112(2) -0.086(2) 0.0081(18) -0.0362(19) O5A 0.0694(11) 0.0562(11) 0.1072(14) -0.0474(10) 0.0285(10) -0.0287(9) C15A 0.089(2) 0.0699(18) 0.109(2) -0.0514(16) 0.0418(17) -0.0459(16) C16A 0.0587(15) 0.0557(15) 0.0561(15) -0.0261(12) -0.0074(12) -0.0087(12) C17A 0.0668(16) 0.0536(15) 0.0517(15) -0.0187(11) -0.0124(13) -0.0036(13) C18A 0.0658(16) 0.0423(13) 0.0432(14) -0.0178(10) -0.0091(12) -0.0077(11) C19A 0.0634(16) 0.0432(13) 0.0429(14) -0.0183(10) -0.0037(12) -0.0065(12) C20A 0.0630(16) 0.0443(13) 0.0496(15) -0.0236(11) 0.0025(13) -0.0116(12) C1'B 0.0653(16) 0.0445(14) 0.0488(14) -0.0251(11) 0.0017(12) -0.0154(12) C2'B 0.0803(19) 0.0476(15) 0.0701(17) -0.0288(13) 0.0004(15) -0.0139(14) C3'B 0.076(2) 0.082(2) 0.100(2) -0.0621(19) 0.0064(18) -0.0044(17) C4'B 0.080(2) 0.120(3) 0.102(2) -0.074(2) 0.0333(18) -0.044(2) C5'B 0.107(2) 0.086(2) 0.075(2) -0.0431(17) 0.0292(18) -0.052(2) C6'B 0.087(2) 0.0532(16) 0.0598(16) -0.0291(13) 0.0048(15) -0.0221(14) C21A 0.0569(15) 0.0346(12) 0.0449(14) -0.0173(10) -0.0032(11) -0.0081(11) C22A 0.0484(15) 0.0443(13) 0.0535(16) -0.0210(11) -0.0054(12) -0.0066(11) C23A 0.0573(16) 0.0452(13) 0.0448(14) -0.0138(11) -0.0114(12) -0.0141(12) C24A 0.0639(16) 0.0471(13) 0.0383(14) -0.0170(10) 0.0008(12) -0.0215(12) C25A 0.0560(14) 0.0360(12) 0.0421(13) -0.0155(10) -0.0031(11) -0.0152(11) C26A 0.0551(15) 0.0314(12) 0.0473(14) -0.0162(10) -0.0064(11) -0.0085(10) C27A 0.0691(18) 0.0645(16) 0.0444(16) -0.0170(12) 0.0008(14) -0.0133(14) O6A 0.1120(17) 0.177(2) 0.0518(13) -0.0322(13) 0.0068(12) -0.0495(16) O7A 0.0891(14) 0.1293(17) 0.0520(12) -0.0354(11) -0.0112(10) -0.0243(12) C28A 0.133(3) 0.200(4) 0.053(2) -0.043(2) -0.0284(19) -0.050(3) C29A 0.409(8) 0.104(3) 0.192(5) -0.052(3) -0.208(5) 0.000(4) O8A 0.0596(11) 0.0741(11) 0.0726(12) -0.0340(9) -0.0049(9) -0.0068(9) C30A 0.0656(19) 0.112(2) 0.156(3) -0.075(2) 0.0001(19) -0.0272(18) O9A 0.0748(11) 0.0811(13) 0.0549(11) -0.0197(9) -0.0221(9) -0.0145(9) C31A 0.259(5) 0.079(3) 0.153(4) 0.035(2) -0.137(4) -0.041(3) O10A 0.0760(11) 0.0803(11) 0.0424(10) -0.0264(8) 0.0015(8) -0.0293(9) C32A 0.113(2) 0.118(2) 0.0699(19) -0.0546(18) -0.0011(17) -0.0390(19) C1B 0.0462(13) 0.0436(12) 0.0335(12) -0.0191(10) 0.0020(10) -0.0080(10) C2B 0.0532(14) 0.0461(13) 0.0353(13) -0.0150(10) -0.0039(10) -0.0090(11) C3B 0.0459(13) 0.0537(14) 0.0366(13) -0.0173(10) -0.0030(10) -0.0118(11) C1'C 0.0549(15) 0.0613(15) 0.0386(14) -0.0189(11) 0.0013(11) -0.0210(12) C2'C 0.0705(19) 0.129(3) 0.0497(17) -0.0119(16) -0.0059(14) -0.0449(18) C3'C 0.084(2) 0.192(4) 0.067(2) -0.007(2) 0.0008(18) -0.082(2) C4'C 0.100(3) 0.165(3) 0.060(2) 0.0058(19) 0.0064(18) -0.078(2) C5'C 0.079(2) 0.126(3) 0.0488(17) 0.0046(16) -0.0064(15) -0.0421(19) C6'C 0.0602(16) 0.0894(19) 0.0487(16) -0.0164(13) -0.0008(13) -0.0306(14) C4B 0.0445(13) 0.0537(14) 0.0363(12) -0.0228(11) 0.0047(10) -0.0142(11) C5B 0.0533(14) 0.0676(17) 0.0387(14) -0.0297(12) 0.0071(11) -0.0132(12) C6B 0.0601(15) 0.0641(17) 0.0565(16) -0.0408(14) 0.0072(12) -0.0096(13) C7B 0.0588(15) 0.0473(15) 0.0562(15) -0.0282(12) -0.0025(12) -0.0086(12) C8B 0.0523(14) 0.0515(14) 0.0393(13) -0.0212(11) 0.0056(10) -0.0145(11) C9B 0.0393(12) 0.0474(14) 0.0391(13) -0.0211(10) 0.0006(10) -0.0099(10) C10B 0.0816(18) 0.0474(15) 0.0432(15) -0.0151(12) -0.0088(13) -0.0141(13) O1B 0.1421(17) 0.0647(11) 0.0637(12) -0.0393(10) 0.0134(12) -0.0236(11) O2B 0.1283(16) 0.0564(11) 0.0647(12) -0.0222(9) 0.0001(11) -0.0408(11) C11B 0.179(3) 0.0563(19) 0.089(2) -0.0221(16) -0.030(2) -0.041(2) C12B 0.347(7) 0.100(3) 0.095(3) -0.001(2) -0.022(3) -0.125(4) O3B 0.0806(13) 0.0877(12) 0.0511(11) -0.0361(9) 0.0176(9) -0.0246(10) C13B 0.091(2) 0.153(3) 0.097(2) -0.066(2) 0.0440(19) -0.041(2) O4B 0.0917(13) 0.0844(12) 0.0785(12) -0.0590(11) 0.0075(10) -0.0111(10) C14B 0.136(3) 0.153(3) 0.111(3) -0.095(2) 0.003(2) -0.052(2) O5B 0.1075(14) 0.0559(11) 0.0670(12) -0.0325(9) 0.0032(10) -0.0218(10) C15B 0.141(3) 0.0559(17) 0.074(2) -0.0239(14) 0.0029(18) -0.0360(17) C16B 0.0496(14) 0.0666(15) 0.0397(13) -0.0282(11) -0.0046(11) -0.0030(12) C17B 0.0425(13) 0.0673(15) 0.0501(14) -0.0333(12) -0.0004(11) -0.0108(11) C18B 0.0446(13) 0.0416(12) 0.0406(13) -0.0196(10) 0.0030(10) -0.0108(10) C19B 0.0479(14) 0.0445(13) 0.0387(13) -0.0214(10) 0.0074(11) -0.0166(11) C20B 0.0500(14) 0.0381(12) 0.0373(13) -0.0194(9) 0.0049(11) -0.0139(10) C1'D 0.0475(13) 0.0424(13) 0.0358(12) -0.0207(10) 0.0021(10) -0.0103(10) C2'D 0.0670(15) 0.0452(14) 0.0436(14) -0.0207(11) 0.0050(11) -0.0196(12) C3'D 0.0841(18) 0.0451(14) 0.0438(15) -0.0107(11) 0.0079(13) -0.0174(13) C4'D 0.0798(18) 0.0677(18) 0.0376(14) -0.0204(13) -0.0052(13) -0.0070(14) C5'D 0.0735(17) 0.0665(17) 0.0505(16) -0.0331(13) -0.0062(13) -0.0156(14) C6'D 0.0691(16) 0.0508(14) 0.0431(14) -0.0231(11) 0.0018(12) -0.0206(12) C21B 0.0453(13) 0.0380(12) 0.0357(12) -0.0173(9) 0.0003(10) -0.0150(10) C22B 0.0494(14) 0.0429(13) 0.0375(13) -0.0167(10) -0.0068(11) -0.0141(11) C23B 0.0383(13) 0.0438(13) 0.0514(15) -0.0213(10) -0.0012(11) -0.0082(10) C24B 0.0445(14) 0.0458(13) 0.0392(13) -0.0192(10) 0.0066(11) -0.0127(10) C25B 0.0417(13) 0.0365(12) 0.0356(12) -0.0160(9) 0.0006(10) -0.0094(10) C26B 0.0412(13) 0.0367(12) 0.0372(13) -0.0171(9) 0.0017(10) -0.0112(10) C27B 0.0519(15) 0.0571(15) 0.0451(15) -0.0255(12) 0.0083(12) -0.0212(12) O6B 0.0474(10) 0.0726(11) 0.0591(11) -0.0206(9) 0.0101(8) -0.0042(8) O7B 0.0630(11) 0.1056(14) 0.0512(11) -0.0192(10) 0.0170(9) -0.0206(10) C28B 0.0452(16) 0.085(2) 0.085(2) -0.0330(16) 0.0120(13) -0.0128(14) C29B 0.0700(19) 0.097(2) 0.125(3) -0.065(2) 0.0198(18) -0.0118(17) O8B 0.0589(10) 0.0701(11) 0.0484(10) -0.0243(8) -0.0129(8) -0.0138(8) C30B 0.101(2) 0.080(2) 0.0703(19) -0.0105(15) -0.0380(17) -0.0166(17) O9B 0.0402(9) 0.0629(10) 0.0680(11) -0.0315(8) -0.0027(7) -0.0110(8) C31B 0.0573(17) 0.083(2) 0.142(3) -0.0401(19) -0.0087(17) -0.0272(16) O10B 0.0482(9) 0.0683(11) 0.0461(9) -0.0241(8) 0.0112(7) -0.0111(8) C32B 0.0568(16) 0.101(2) 0.0761(19) -0.0539(16) 0.0067(14) 0.0052(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1A C25A 1.519(3) . ? C1A C9A 1.530(3) . ? C1A C2A 1.533(3) . ? C1A C16A 1.566(3) . ? C2A C3A 1.359(3) . ? C2A C10A 1.468(3) . ? C3A C4A 1.464(3) . ? C3A C1'A 1.486(3) . ? C1'A C2'A 1.380(3) . ? C1'A C6'A 1.383(3) . ? C2'A C3'A 1.376(4) . ? C2'A H2'A 0.9300 . ? C3'A C4'A 1.378(4) . ? C3'A H3'A 0.9300 . ? C4'A C5'A 1.365(4) . ? C4'A H4'A 0.9300 . ? C5'A C6'A 1.372(4) . ? C5'A H5'A 0.9300 . ? C6'A H6'A 0.9300 . ? C4A C5A 1.400(3) . ? C4A C9A 1.404(3) . ? C5A O3A 1.379(2) . ? C5A C6A 1.388(3) . ? C6A O4A 1.384(2) . ? C6A C7A 1.395(3) . ? C7A O5A 1.358(2) . ? C7A C8A 1.398(3) . ? C8A C9A 1.378(3) . ? C8A H8A 0.9300 . ? C10A O1A 1.199(3) . ? C10A O2A 1.333(3) . ? O2A C11A 1.456(3) . ? C11A C12A 1.406(4) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C12A H12A 0.9600 . ? C12A H12B 0.9600 . ? C12A H12C 0.9600 . ? O3A C13A 1.426(3) . ? C13A H13A 0.9600 . ? C13A H13B 0.9600 . ? C13A H13C 0.9600 . ? O4A C14A 1.425(3) . ? C14A H14A 0.9600 . ? C14A H14B 0.9600 . ? C14A H14C 0.9600 . ? O5A C15A 1.407(3) . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C16A C17A 1.528(3) . ? C16A H16A 0.9700 . ? C16A H16B 0.9700 . ? C17A C18A 1.515(3) . ? C17A H17A 0.9700 . ? C17A H17B 0.9700 . ? C18A C19A 1.496(3) . ? C18A C26A 1.497(3) . ? C18A H18A 0.9800 . ? C19A C20A 1.364(3) . ? C19A C27A 1.464(3) . ? C20A C21A 1.478(3) . ? C20A C1'B 1.483(3) . ? C1'B C6'B 1.381(3) . ? C1'B C2'B 1.382(3) . ? C2'B C3'B 1.384(3) . ? C2'B H2'B 0.9300 . ? C3'B C4'B 1.377(4) . ? C3'B H3'B 0.9300 . ? C4'B C5'B 1.373(4) . ? C4'B H4'B 0.9300 . ? C5'B C6'B 1.379(3) . ? C5'B H5'B 0.9300 . ? C6'B H6'B 0.9300 . ? C21A C22A 1.389(3) . ? C21A C26A 1.393(3) . ? C22A O8A 1.375(2) . ? C22A C23A 1.394(3) . ? C23A O9A 1.392(2) . ? C23A C24A 1.393(3) . ? C24A O10A 1.384(2) . ? C24A C25A 1.394(3) . ? C25A C26A 1.386(3) . ? C27A O6A 1.196(3) . ? C27A O7A 1.328(3) . ? O7A C28A 1.463(3) . ? C28A C29A 1.393(5) . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C29A H29A 0.9600 . ? C29A H29B 0.9600 . ? C29A H29C 0.9600 . ? O8A C30A 1.419(3) . ? C30A H30A 0.9600 . ? C30A H30B 0.9600 . ? C30A H30C 0.9600 . ? O9A C31A 1.400(3) . ? C31A H31A 0.9600 . ? C31A H31B 0.9600 . ? C31A H31C 0.9600 . ? O10A C32A 1.424(3) . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C1B C9B 1.524(3) . ? C1B C2B 1.526(3) . ? C1B C25B 1.532(3) . ? C1B C16B 1.566(3) . ? C2B C3B 1.356(3) . ? C2B C10B 1.469(3) . ? C3B C4B 1.466(3) . ? C3B C1'C 1.488(3) . ? C1'C C6'C 1.374(3) . ? C1'C C2'C 1.376(3) . ? C2'C C3'C 1.372(3) . ? C2'C H2'C 0.9300 . ? C3'C C4'C 1.379(4) . ? C3'C H3'C 0.9300 . ? C4'C C5'C 1.359(4) . ? C4'C H4'C 0.9300 . ? C5'C C6'C 1.377(3) . ? C5'C H5'C 0.9300 . ? C6'C H6'C 0.9300 . ? C4B C9B 1.389(3) . ? C4B C5B 1.391(3) . ? C5B O3B 1.380(2) . ? C5B C6B 1.385(3) . ? C6B O4B 1.386(2) . ? C6B C7B 1.406(3) . ? C7B O5B 1.360(2) . ? C7B C8B 1.397(3) . ? C8B C9B 1.377(3) . ? C8B H8B 0.9300 . ? C10B O1B 1.205(3) . ? C10B O2B 1.339(3) . ? O2B C11B 1.443(3) . ? C11B C12B 1.487(4) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C12B H12D 0.9600 . ? C12B H12E 0.9600 . ? C12B H12F 0.9600 . ? O3B C13B 1.406(3) . ? C13B H13D 0.9600 . ? C13B H13E 0.9600 . ? C13B H13F 0.9600 . ? O4B C14B 1.425(3) . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? O5B C15B 1.419(3) . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16B C17B 1.527(3) . ? C16B H16C 0.9700 . ? C16B H16D 0.9700 . ? C17B C18B 1.529(3) . ? C17B H17C 0.9700 . ? C17B H17D 0.9700 . ? C18B C26B 1.489(3) . ? C18B C19B 1.504(3) . ? C18B H18B 0.9800 . ? C19B C20B 1.367(3) . ? C19B C27B 1.463(3) . ? C20B C21B 1.477(3) . ? C20B C1'D 1.480(3) . ? C1'D C2'D 1.386(3) . ? C1'D C6'D 1.393(3) . ? C2'D C3'D 1.385(3) . ? C2'D H2'D 0.9300 . ? C3'D C4'D 1.379(3) . ? C3'D H3'D 0.9300 . ? C4'D C5'D 1.375(3) . ? C4'D H4'D 0.9300 . ? C5'D C6'D 1.379(3) . ? C5'D H5'D 0.9300 . ? C6'D H6'D 0.9300 . ? C21B C22B 1.388(3) . ? C21B C26B 1.394(2) . ? C22B O8B 1.377(2) . ? C22B C23B 1.399(3) . ? C23B O9B 1.385(2) . ? C23B C24B 1.402(3) . ? C24B O10B 1.380(2) . ? C24B C25B 1.394(3) . ? C25B C26B 1.378(2) . ? C27B O7B 1.197(2) . ? C27B O6B 1.347(2) . ? O6B C28B 1.453(2) . ? C28B C29B 1.462(3) . ? C28B H28C 0.9700 . ? C28B H28D 0.9700 . ? C29B H29D 0.9600 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? O8B C30B 1.421(3) . ? C30B H30D 0.9600 . ? C30B H30E 0.9600 . ? C30B H30F 0.9600 . ? O9B C31B 1.410(3) . ? C31B H31D 0.9600 . ? C31B H31E 0.9600 . ? C31B H31F 0.9600 . ? O10B C32B 1.432(2) . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 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 C25A C1A C9A 113.77(16) . . ? C25A C1A C2A 116.41(17) . . ? C9A C1A C2A 100.66(16) . . ? C25A C1A C16A 111.56(17) . . ? C9A C1A C16A 107.48(16) . . ? C2A C1A C16A 105.99(17) . . ? C3A C2A C10A 128.9(2) . . ? C3A C2A C1A 111.28(19) . . ? C10A C2A C1A 119.7(2) . . ? C2A C3A C4A 108.7(2) . . ? C2A C3A C1'A 126.5(2) . . ? C4A C3A C1'A 124.66(19) . . ? C2'A C1'A C6'A 117.7(2) . . ? C2'A C1'A C3A 122.2(2) . . ? C6'A C1'A C3A 120.0(2) . . ? C3'A C2'A C1'A 121.2(3) . . ? C3'A C2'A H2'A 119.4 . . ? C1'A C2'A H2'A 119.4 . . ? C2'A C3'A C4'A 119.6(3) . . ? C2'A C3'A H3'A 120.2 . . ? C4'A C3'A H3'A 120.2 . . ? C5'A C4'A C3'A 120.1(3) . . ? C5'A C4'A H4'A 119.9 . . ? C3'A C4'A H4'A 119.9 . . ? C4'A C5'A C6'A 119.7(3) . . ? C4'A C5'A H5'A 120.1 . . ? C6'A C5'A H5'A 120.1 . . ? C5'A C6'A C1'A 121.6(3) . . ? C5'A C6'A H6'A 119.2 . . ? C1'A C6'A H6'A 119.2 . . ? C5A C4A C9A 118.93(19) . . ? C5A C4A C3A 132.0(2) . . ? C9A C4A C3A 109.04(18) . . ? O3A C5A C6A 119.29(18) . . ? O3A C5A C4A 121.31(19) . . ? C6A C5A C4A 119.39(19) . . ? O4A C6A C5A 118.82(19) . . ? O4A C6A C7A 120.1(2) . . ? C5A C6A C7A 120.91(19) . . ? O5A C7A C6A 114.79(18) . . ? O5A C7A C8A 125.1(2) . . ? C6A C7A C8A 120.1(2) . . ? C9A C8A C7A 118.8(2) . . ? C9A C8A H8A 120.6 . . ? C7A C8A H8A 120.6 . . ? C8A C9A C4A 121.79(18) . . ? C8A C9A C1A 128.86(19) . . ? C4A C9A C1A 109.07(17) . . ? O1A C10A O2A 123.2(2) . . ? O1A C10A C2A 124.2(3) . . ? O2A C10A C2A 112.6(2) . . ? C10A O2A C11A 117.0(2) . . ? C12A C11A O2A 110.1(3) . . ? C12A C11A H11A 109.6 . . ? O2A C11A H11A 109.6 . . ? C12A C11A H11B 109.6 . . ? O2A C11A H11B 109.6 . . ? H11A C11A H11B 108.1 . . ? C11A C12A H12A 109.5 . . ? C11A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? C11A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? C5A O3A C13A 113.19(18) . . ? O3A C13A H13A 109.5 . . ? O3A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? O3A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? C6A O4A C14A 115.35(17) . . ? O4A C14A H14A 109.5 . . ? O4A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? O4A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C7A O5A C15A 119.64(17) . . ? O5A C15A H15A 109.5 . . ? O5A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? O5A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C17A C16A C1A 115.17(18) . . ? C17A C16A H16A 108.5 . . ? C1A C16A H16A 108.5 . . ? C17A C16A H16B 108.5 . . ? C1A C16A H16B 108.5 . . ? H16A C16A H16B 107.5 . . ? C18A C17A C16A 107.10(18) . . ? C18A C17A H17A 110.3 . . ? C16A C17A H17A 110.3 . . ? C18A C17A H17B 110.3 . . ? C16A C17A H17B 110.3 . . ? H17A C17A H17B 108.6 . . ? C19A C18A C26A 102.75(18) . . ? C19A C18A C17A 124.89(18) . . ? C26A C18A C17A 109.77(17) . . ? C19A C18A H18A 106.0 . . ? C26A C18A H18A 106.0 . . ? C17A C18A H18A 106.0 . . ? C20A C19A C27A 125.8(2) . . ? C20A C19A C18A 110.55(19) . . ? C27A C19A C18A 122.4(2) . . ? C19A C20A C21A 108.68(19) . . ? C19A C20A C1'B 126.5(2) . . ? C21A C20A C1'B 124.76(19) . . ? C6'B C1'B C2'B 118.4(2) . . ? C6'B C1'B C20A 120.4(2) . . ? C2'B C1'B C20A 121.2(2) . . ? C1'B C2'B C3'B 120.4(2) . . ? C1'B C2'B H2'B 119.8 . . ? C3'B C2'B H2'B 119.8 . . ? C4'B C3'B C2'B 120.4(3) . . ? C4'B C3'B H3'B 119.8 . . ? C2'B C3'B H3'B 119.8 . . ? C5'B C4'B C3'B 119.6(3) . . ? C5'B C4'B H4'B 120.2 . . ? C3'B C4'B H4'B 120.2 . . ? C4'B C5'B C6'B 119.9(3) . . ? C4'B C5'B H5'B 120.1 . . ? C6'B C5'B H5'B 120.1 . . ? C5'B C6'B C1'B 121.3(2) . . ? C5'B C6'B H6'B 119.4 . . ? C1'B C6'B H6'B 119.4 . . ? C22A C21A C26A 118.1(2) . . ? C22A C21A C20A 133.9(2) . . ? C26A C21A C20A 107.69(18) . . ? O8A C22A C21A 121.2(2) . . ? O8A C22A C23A 120.40(19) . . ? C21A C22A C23A 118.3(2) . . ? O9A C23A C24A 118.8(2) . . ? O9A C23A C22A 119.3(2) . . ? C24A C23A C22A 121.81(19) . . ? O10A C24A C23A 120.97(19) . . ? O10A C24A C25A 117.9(2) . . ? C23A C24A C25A 120.96(19) . . ? C26A C25A C24A 115.42(19) . . ? C26A C25A C1A 120.64(18) . . ? C24A C25A C1A 123.76(19) . . ? C25A C26A C21A 124.92(19) . . ? C25A C26A C18A 125.0(2) . . ? C21A C26A C18A 109.69(19) . . ? O6A C27A O7A 121.0(2) . . ? O6A C27A C19A 127.8(3) . . ? O7A C27A C19A 111.2(2) . . ? C27A O7A C28A 116.6(2) . . ? C29A C28A O7A 109.5(3) . . ? C29A C28A H28A 109.8 . . ? O7A C28A H28A 109.8 . . ? C29A C28A H28B 109.8 . . ? O7A C28A H28B 109.8 . . ? H28A C28A H28B 108.2 . . ? C28A C29A H29A 109.5 . . ? C28A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C28A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C22A O8A C30A 117.94(18) . . ? O8A C30A H30A 109.5 . . ? O8A C30A H30B 109.5 . . ? H30A C30A H30B 109.5 . . ? O8A C30A H30C 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C23A O9A C31A 115.05(19) . . ? O9A C31A H31A 109.5 . . ? O9A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? O9A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? C24A O10A C32A 116.85(18) . . ? O10A C32A H32A 109.5 . . ? O10A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? O10A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C9B C1B C2B 101.09(15) . . ? C9B C1B C25B 111.71(15) . . ? C2B C1B C25B 112.25(16) . . ? C9B C1B C16B 108.96(15) . . ? C2B C1B C16B 109.55(16) . . ? C25B C1B C16B 112.66(16) . . ? C3B C2B C10B 129.7(2) . . ? C3B C2B C1B 111.28(18) . . ? C10B C2B C1B 119.05(18) . . ? C2B C3B C4B 108.77(18) . . ? C2B C3B C1'C 127.0(2) . . ? C4B C3B C1'C 124.12(18) . . ? C6'C C1'C C2'C 118.2(2) . . ? C6'C C1'C C3B 122.2(2) . . ? C2'C C1'C C3B 119.6(2) . . ? C3'C C2'C C1'C 121.1(2) . . ? C3'C C2'C H2'C 119.4 . . ? C1'C C2'C H2'C 119.4 . . ? C2'C C3'C C4'C 119.5(3) . . ? C2'C C3'C H3'C 120.3 . . ? C4'C C3'C H3'C 120.3 . . ? C5'C C4'C C3'C 120.3(3) . . ? C5'C C4'C H4'C 119.8 . . ? C3'C C4'C H4'C 119.8 . . ? C4'C C5'C C6'C 119.5(2) . . ? C4'C C5'C H5'C 120.3 . . ? C6'C C5'C H5'C 120.3 . . ? C1'C C6'C C5'C 121.4(2) . . ? C1'C C6'C H6'C 119.3 . . ? C5'C C6'C H6'C 119.3 . . ? C9B C4B C5B 119.4(2) . . ? C9B C4B C3B 108.98(17) . . ? C5B C4B C3B 131.7(2) . . ? O3B C5B C6B 120.26(19) . . ? O3B C5B C4B 120.1(2) . . ? C6B C5B C4B 119.3(2) . . ? C5B C6B O4B 119.7(2) . . ? C5B C6B C7B 120.65(19) . . ? O4B C6B C7B 119.6(2) . . ? O5B C7B C8B 124.9(2) . . ? O5B C7B C6B 115.20(19) . . ? C8B C7B C6B 119.9(2) . . ? C9B C8B C7B 118.3(2) . . ? C9B C8B H8B 120.8 . . ? C7B C8B H8B 120.8 . . ? C8B C9B C4B 122.33(18) . . ? C8B C9B C1B 128.03(18) . . ? C4B C9B C1B 109.63(18) . . ? O1B C10B O2B 122.3(2) . . ? O1B C10B C2B 124.2(2) . . ? O2B C10B C2B 113.5(2) . . ? C10B O2B C11B 116.7(2) . . ? O2B C11B C12B 106.5(3) . . ? O2B C11B H11C 110.4 . . ? C12B C11B H11C 110.4 . . ? O2B C11B H11D 110.4 . . ? C12B C11B H11D 110.4 . . ? H11C C11B H11D 108.6 . . ? C11B C12B H12D 109.5 . . ? C11B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C11B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C5B O3B C13B 115.78(19) . . ? O3B C13B H13D 109.5 . . ? O3B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? O3B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C6B O4B C14B 113.78(19) . . ? O4B C14B H14D 109.5 . . ? O4B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? O4B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C7B O5B C15B 118.39(17) . . ? O5B C15B H15D 109.5 . . ? O5B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? O5B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C17B C16B C1B 115.58(16) . . ? C17B C16B H16C 108.4 . . ? C1B C16B H16C 108.4 . . ? C17B C16B H16D 108.4 . . ? C1B C16B H16D 108.4 . . ? H16C C16B H16D 107.4 . . ? C16B C17B C18B 106.38(17) . . ? C16B C17B H17C 110.5 . . ? C18B C17B H17C 110.5 . . ? C16B C17B H17D 110.5 . . ? C18B C17B H17D 110.5 . . ? H17C C17B H17D 108.6 . . ? C26B C18B C19B 102.29(15) . . ? C26B C18B C17B 109.03(15) . . ? C19B C18B C17B 123.55(17) . . ? C26B C18B H18B 107.0 . . ? C19B C18B H18B 107.0 . . ? C17B C18B H18B 107.0 . . ? C20B C19B C27B 126.83(18) . . ? C20B C19B C18B 110.68(17) . . ? C27B C19B C18B 121.58(18) . . ? C19B C20B C21B 108.44(17) . . ? C19B C20B C1'D 128.33(18) . . ? C21B C20B C1'D 123.23(17) . . ? C2'D C1'D C6'D 118.45(19) . . ? C2'D C1'D C20B 121.39(18) . . ? C6'D C1'D C20B 120.09(18) . . ? C3'D C2'D C1'D 120.4(2) . . ? C3'D C2'D H2'D 119.8 . . ? C1'D C2'D H2'D 119.8 . . ? C4'D C3'D C2'D 120.4(2) . . ? C4'D C3'D H3'D 119.8 . . ? C2'D C3'D H3'D 119.8 . . ? C5'D C4'D C3'D 119.7(2) . . ? C5'D C4'D H4'D 120.2 . . ? C3'D C4'D H4'D 120.2 . . ? C4'D C5'D C6'D 120.2(2) . . ? C4'D C5'D H5'D 119.9 . . ? C6'D C5'D H5'D 119.9 . . ? C5'D C6'D C1'D 120.9(2) . . ? C5'D C6'D H6'D 119.6 . . ? C1'D C6'D H6'D 119.6 . . ? C22B C21B C26B 118.64(18) . . ? C22B C21B C20B 133.54(18) . . ? C26B C21B C20B 107.61(17) . . ? O8B C22B C21B 122.00(18) . . ? O8B C22B C23B 119.30(18) . . ? C21B C22B C23B 118.61(18) . . ? O9B C23B C22B 119.64(18) . . ? O9B C23B C24B 119.35(19) . . ? C22B C23B C24B 120.89(19) . . ? O10B C24B C25B 118.52(18) . . ? O10B C24B C23B 120.45(18) . . ? C25B C24B C23B 120.97(18) . . ? C26B C25B C24B 116.34(17) . . ? C26B C25B C1B 119.74(17) . . ? C24B C25B C1B 123.84(17) . . ? C25B C26B C21B 124.20(18) . . ? C25B C26B C18B 125.02(17) . . ? C21B C26B C18B 110.42(17) . . ? O7B C27B O6B 122.5(2) . . ? O7B C27B C19B 127.2(2) . . ? O6B C27B C19B 110.38(19) . . ? C27B O6B C28B 118.50(18) . . ? O6B C28B C29B 110.7(2) . . ? O6B C28B H28C 109.5 . . ? C29B C28B H28C 109.5 . . ? O6B C28B H28D 109.5 . . ? C29B C28B H28D 109.5 . . ? H28C C28B H28D 108.1 . . ? C28B C29B H29D 109.5 . . ? C28B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C28B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C22B O8B C30B 115.59(16) . . ? O8B C30B H30D 109.5 . . ? O8B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? O8B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C23B O9B C31B 114.98(16) . . ? O9B C31B H31D 109.5 . . ? O9B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? O9B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? C24B O10B C32B 115.82(16) . . ? O10B C32B H32D 109.5 . . ? O10B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? O10B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 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 C25A C1A C2A C3A -134.01(19) . . . . ? C9A C1A C2A C3A -10.5(2) . . . . ? C16A C1A C2A C3A 101.3(2) . . . . ? C25A C1A C2A C10A 49.8(3) . . . . ? C9A C1A C2A C10A 173.32(19) . . . . ? C16A C1A C2A C10A -74.8(2) . . . . ? C10A C2A C3A C4A -177.7(2) . . . . ? C1A C2A C3A C4A 6.6(2) . . . . ? C10A C2A C3A C1'A 6.0(4) . . . . ? C1A C2A C3A C1'A -169.65(19) . . . . ? C2A C3A C1'A C2'A -118.6(3) . . . . ? C4A C3A C1'A C2'A 65.7(3) . . . . ? C2A C3A C1'A C6'A 63.0(3) . . . . ? C4A C3A C1'A C6'A -112.6(2) . . . . ? C6'A C1'A C2'A C3'A -1.0(4) . . . . ? C3A C1'A C2'A C3'A -179.4(2) . . . . ? C1'A C2'A C3'A C4'A 1.0(4) . . . . ? C2'A C3'A C4'A C5'A -0.4(5) . . . . ? C3'A C4'A C5'A C6'A -0.1(5) . . . . ? C4'A C5'A C6'A C1'A 0.1(5) . . . . ? C2'A C1'A C6'A C5'A 0.5(4) . . . . ? C3A C1'A C6'A C5'A 178.9(2) . . . . ? C2A C3A C4A C5A -177.3(2) . . . . ? C1'A C3A C4A C5A -1.0(4) . . . . ? C2A C3A C4A C9A 0.7(2) . . . . ? C1'A C3A C4A C9A 177.07(19) . . . . ? C9A C4A C5A O3A -178.26(18) . . . . ? C3A C4A C5A O3A -0.4(3) . . . . ? C9A C4A C5A C6A 2.8(3) . . . . ? C3A C4A C5A C6A -179.3(2) . . . . ? O3A C5A C6A O4A 5.4(3) . . . . ? C4A C5A C6A O4A -175.62(18) . . . . ? O3A C5A C6A C7A -178.96(19) . . . . ? C4A C5A C6A C7A 0.0(3) . . . . ? O4A C6A C7A O5A -3.3(3) . . . . ? C5A C6A C7A O5A -178.93(18) . . . . ? O4A C6A C7A C8A 173.62(18) . . . . ? C5A C6A C7A C8A -2.0(3) . . . . ? O5A C7A C8A C9A 177.65(19) . . . . ? C6A C7A C8A C9A 1.0(3) . . . . ? C7A C8A C9A C4A 1.8(3) . . . . ? C7A C8A C9A C1A -171.37(19) . . . . ? C5A C4A C9A C8A -3.8(3) . . . . ? C3A C4A C9A C8A 177.89(18) . . . . ? C5A C4A C9A C1A 170.64(17) . . . . ? C3A C4A C9A C1A -7.7(2) . . . . ? C25A C1A C9A C8A -50.1(3) . . . . ? C2A C1A C9A C8A -175.4(2) . . . . ? C16A C1A C9A C8A 73.9(3) . . . . ? C25A C1A C9A C4A 135.99(18) . . . . ? C2A C1A C9A C4A 10.7(2) . . . . ? C16A C1A C9A C4A -100.0(2) . . . . ? C3A C2A C10A O1A -156.5(3) . . . . ? C1A C2A C10A O1A 18.9(4) . . . . ? C3A C2A C10A O2A 25.6(3) . . . . ? C1A C2A C10A O2A -159.0(2) . . . . ? O1A C10A O2A C11A 3.7(4) . . . . ? C2A C10A O2A C11A -178.3(2) . . . . ? C10A O2A C11A C12A 164.4(3) . . . . ? C6A C5A O3A C13A -84.6(2) . . . . ? C4A C5A O3A C13A 96.5(2) . . . . ? C5A C6A O4A C14A -110.7(2) . . . . ? C7A C6A O4A C14A 73.6(3) . . . . ? C6A C7A O5A C15A -166.5(2) . . . . ? C8A C7A O5A C15A 16.7(3) . . . . ? C25A C1A C16A C17A 34.6(2) . . . . ? C9A C1A C16A C17A -90.7(2) . . . . ? C2A C1A C16A C17A 162.28(18) . . . . ? C1A C16A C17A C18A -61.6(2) . . . . ? C16A C17A C18A C19A 178.51(19) . . . . ? C16A C17A C18A C26A 56.1(2) . . . . ? C26A C18A C19A C20A -7.1(2) . . . . ? C17A C18A C19A C20A -132.6(2) . . . . ? C26A C18A C19A C27A -175.23(19) . . . . ? C17A C18A C19A C27A 59.3(3) . . . . ? C27A C19A C20A C21A 171.4(2) . . . . ? C18A C19A C20A C21A 3.8(2) . . . . ? C27A C19A C20A C1'B -10.8(4) . . . . ? C18A C19A C20A C1'B -178.40(19) . . . . ? C19A C20A C1'B C6'B -55.9(3) . . . . ? C21A C20A C1'B C6'B 121.5(2) . . . . ? C19A C20A C1'B C2'B 123.9(2) . . . . ? C21A C20A C1'B C2'B -58.6(3) . . . . ? C6'B C1'B C2'B C3'B 0.3(3) . . . . ? C20A C1'B C2'B C3'B -179.6(2) . . . . ? C1'B C2'B C3'B C4'B -0.1(4) . . . . ? C2'B C3'B C4'B C5'B -0.3(4) . . . . ? C3'B C4'B C5'B C6'B 0.6(4) . . . . ? C4'B C5'B C6'B C1'B -0.5(4) . . . . ? C2'B C1'B C6'B C5'B 0.0(3) . . . . ? C20A C1'B C6'B C5'B 179.9(2) . . . . ? C19A C20A C21A C22A 174.9(2) . . . . ? C1'B C20A C21A C22A -2.9(3) . . . . ? C19A C20A C21A C26A 1.4(2) . . . . ? C1'B C20A C21A C26A -176.41(18) . . . . ? C26A C21A C22A O8A -173.89(18) . . . . ? C20A C21A C22A O8A 13.2(3) . . . . ? C26A C21A C22A C23A 2.5(3) . . . . ? C20A C21A C22A C23A -170.4(2) . . . . ? O8A C22A C23A O9A -4.2(3) . . . . ? C21A C22A C23A O9A 179.37(18) . . . . ? O8A C22A C23A C24A 179.69(19) . . . . ? C21A C22A C23A C24A 3.2(3) . . . . ? O9A C23A C24A O10A 3.6(3) . . . . ? C22A C23A C24A O10A 179.74(18) . . . . ? O9A C23A C24A C25A 179.35(17) . . . . ? C22A C23A C24A C25A -4.5(3) . . . . ? O10A C24A C25A C26A 175.69(17) . . . . ? C23A C24A C25A C26A -0.2(3) . . . . ? O10A C24A C25A C1A -9.2(3) . . . . ? C23A C24A C25A C1A 174.90(19) . . . . ? C9A C1A C25A C26A 117.3(2) . . . . ? C2A C1A C25A C26A -126.3(2) . . . . ? C16A C1A C25A C26A -4.5(3) . . . . ? C9A C1A C25A C24A -57.5(3) . . . . ? C2A C1A C25A C24A 58.9(3) . . . . ? C16A C1A C25A C24A -179.34(17) . . . . ? C24A C25A C26A C21A 6.4(3) . . . . ? C1A C25A C26A C21A -168.88(18) . . . . ? C24A C25A C26A C18A 178.38(18) . . . . ? C1A C25A C26A C18A 3.1(3) . . . . ? C22A C21A C26A C25A -7.7(3) . . . . ? C20A C21A C26A C25A 166.97(18) . . . . ? C22A C21A C26A C18A 179.28(17) . . . . ? C20A C21A C26A C18A -6.1(2) . . . . ? C19A C18A C26A C25A -165.07(18) . . . . ? C17A C18A C26A C25A -30.3(3) . . . . ? C19A C18A C26A C21A 8.0(2) . . . . ? C17A C18A C26A C21A 142.75(19) . . . . ? C20A C19A C27A O6A 30.3(4) . . . . ? C18A C19A C27A O6A -163.5(3) . . . . ? C20A C19A C27A O7A -147.2(2) . . . . ? C18A C19A C27A O7A 19.0(3) . . . . ? O6A C27A O7A C28A -3.2(4) . . . . ? C19A C27A O7A C28A 174.5(2) . . . . ? C27A O7A C28A C29A -142.8(4) . . . . ? C21A C22A O8A C30A -110.0(2) . . . . ? C23A C22A O8A C30A 73.7(3) . . . . ? C24A C23A O9A C31A -97.9(3) . . . . ? C22A C23A O9A C31A 85.9(3) . . . . ? C23A C24A O10A C32A -68.3(3) . . . . ? C25A C24A O10A C32A 115.8(2) . . . . ? C9B C1B C2B C3B 3.6(2) . . . . ? C25B C1B C2B C3B 122.76(18) . . . . ? C16B C1B C2B C3B -111.31(18) . . . . ? C9B C1B C2B C10B -176.98(17) . . . . ? C25B C1B C2B C10B -57.8(2) . . . . ? C16B C1B C2B C10B 68.1(2) . . . . ? C10B C2B C3B C4B 179.7(2) . . . . ? C1B C2B C3B C4B -0.9(2) . . . . ? C10B C2B C3B C1'C 4.2(4) . . . . ? C1B C2B C3B C1'C -176.48(19) . . . . ? C2B C3B C1'C C6'C -100.6(3) . . . . ? C4B C3B C1'C C6'C 84.5(3) . . . . ? C2B C3B C1'C C2'C 80.4(3) . . . . ? C4B C3B C1'C C2'C -94.5(3) . . . . ? C6'C C1'C C2'C C3'C 1.3(4) . . . . ? C3B C1'C C2'C C3'C -179.7(3) . . . . ? C1'C C2'C C3'C C4'C 0.7(5) . . . . ? C2'C C3'C C4'C C5'C -2.2(6) . . . . ? C3'C C4'C C5'C C6'C 1.5(6) . . . . ? C2'C C1'C C6'C C5'C -2.0(4) . . . . ? C3B C1'C C6'C C5'C 179.0(2) . . . . ? C4'C C5'C C6'C C1'C 0.6(5) . . . . ? C2B C3B C4B C9B -2.5(2) . . . . ? C1'C C3B C4B C9B 173.23(18) . . . . ? C2B C3B C4B C5B 178.8(2) . . . . ? C1'C C3B C4B C5B -5.5(3) . . . . ? C9B C4B C5B O3B 171.91(18) . . . . ? C3B C4B C5B O3B -9.5(3) . . . . ? C9B C4B C5B C6B -2.2(3) . . . . ? C3B C4B C5B C6B 176.3(2) . . . . ? O3B C5B C6B O4B 7.6(3) . . . . ? C4B C5B C6B O4B -178.25(19) . . . . ? O3B C5B C6B C7B -174.20(19) . . . . ? C4B C5B C6B C7B 0.0(3) . . . . ? C5B C6B C7B O5B -179.71(19) . . . . ? O4B C6B C7B O5B -1.5(3) . . . . ? C5B C6B C7B C8B 1.7(3) . . . . ? O4B C6B C7B C8B 179.95(19) . . . . ? O5B C7B C8B C9B -179.48(19) . . . . ? C6B C7B C8B C9B -1.1(3) . . . . ? C7B C8B C9B C4B -1.3(3) . . . . ? C7B C8B C9B C1B 177.83(18) . . . . ? C5B C4B C9B C8B 3.0(3) . . . . ? C3B C4B C9B C8B -175.93(17) . . . . ? C5B C4B C9B C1B -176.28(17) . . . . ? C3B C4B C9B C1B 4.8(2) . . . . ? C2B C1B C9B C8B 175.77(19) . . . . ? C25B C1B C9B C8B 56.2(3) . . . . ? C16B C1B C9B C8B -68.9(2) . . . . ? C2B C1B C9B C4B -5.0(2) . . . . ? C25B C1B C9B C4B -124.60(18) . . . . ? C16B C1B C9B C4B 110.29(18) . . . . ? C3B C2B C10B O1B 171.1(2) . . . . ? C1B C2B C10B O1B -8.3(3) . . . . ? C3B C2B C10B O2B -9.2(3) . . . . ? C1B C2B C10B O2B 171.53(18) . . . . ? O1B C10B O2B C11B -0.1(3) . . . . ? C2B C10B O2B C11B -179.8(2) . . . . ? C10B O2B C11B C12B 179.7(3) . . . . ? C6B C5B O3B C13B -75.1(3) . . . . ? C4B C5B O3B C13B 110.8(2) . . . . ? C5B C6B O4B C14B -96.4(3) . . . . ? C7B C6B O4B C14B 85.4(3) . . . . ? C8B C7B O5B C15B -7.8(3) . . . . ? C6B C7B O5B C15B 173.7(2) . . . . ? C9B C1B C16B C17B 96.8(2) . . . . ? C2B C1B C16B C17B -153.45(17) . . . . ? C25B C1B C16B C17B -27.7(2) . . . . ? C1B C16B C17B C18B 59.2(2) . . . . ? C16B C17B C18B C26B -59.4(2) . . . . ? C16B C17B C18B C19B -179.35(17) . . . . ? C26B C18B C19B C20B 7.4(2) . . . . ? C17B C18B C19B C20B 130.42(19) . . . . ? C26B C18B C19B C27B 177.20(17) . . . . ? C17B C18B C19B C27B -59.8(3) . . . . ? C27B C19B C20B C21B -174.24(18) . . . . ? C18B C19B C20B C21B -5.1(2) . . . . ? C27B C19B C20B C1'D 6.2(3) . . . . ? C18B C19B C20B C1'D 175.36(17) . . . . ? C19B C20B C1'D C2'D 62.6(3) . . . . ? C21B C20B C1'D C2'D -116.8(2) . . . . ? C19B C20B C1'D C6'D -120.4(2) . . . . ? C21B C20B C1'D C6'D 60.2(3) . . . . ? C6'D C1'D C2'D C3'D -0.1(3) . . . . ? C20B C1'D C2'D C3'D 176.94(18) . . . . ? C1'D C2'D C3'D C4'D -0.2(3) . . . . ? C2'D C3'D C4'D C5'D 0.5(4) . . . . ? C3'D C4'D C5'D C6'D -0.5(3) . . . . ? C4'D C5'D C6'D C1'D 0.2(3) . . . . ? C2'D C1'D C6'D C5'D 0.1(3) . . . . ? C20B C1'D C6'D C5'D -176.95(18) . . . . ? C19B C20B C21B C22B -174.1(2) . . . . ? C1'D C20B C21B C22B 5.5(3) . . . . ? C19B C20B C21B C26B 0.4(2) . . . . ? C1'D C20B C21B C26B 180.00(17) . . . . ? C26B C21B C22B O8B 174.41(16) . . . . ? C20B C21B C22B O8B -11.5(3) . . . . ? C26B C21B C22B C23B -2.1(3) . . . . ? C20B C21B C22B C23B 171.98(19) . . . . ? O8B C22B C23B O9B 4.7(3) . . . . ? C21B C22B C23B O9B -178.70(16) . . . . ? O8B C22B C23B C24B -179.09(17) . . . . ? C21B C22B C23B C24B -2.5(3) . . . . ? O9B C23B C24B O10B -3.5(3) . . . . ? C22B C23B C24B O10B -179.71(17) . . . . ? O9B C23B C24B C25B 179.32(17) . . . . ? C22B C23B C24B C25B 3.1(3) . . . . ? O10B C24B C25B C26B -176.26(16) . . . . ? C23B C24B C25B C26B 1.0(3) . . . . ? O10B C24B C25B C1B 6.8(3) . . . . ? C23B C24B C25B C1B -175.96(17) . . . . ? C9B C1B C25B C26B -125.65(19) . . . . ? C2B C1B C25B C26B 121.61(19) . . . . ? C16B C1B C25B C26B -2.6(2) . . . . ? C9B C1B C25B C24B 51.2(2) . . . . ? C2B C1B C25B C24B -61.6(2) . . . . ? C16B C1B C25B C24B 174.21(18) . . . . ? C24B C25B C26B C21B -5.9(3) . . . . ? C1B C25B C26B C21B 171.17(17) . . . . ? C24B C25B C26B C18B -178.31(17) . . . . ? C1B C25B C26B C18B -1.2(3) . . . . ? C22B C21B C26B C25B 6.5(3) . . . . ? C20B C21B C26B C25B -168.93(17) . . . . ? C22B C21B C26B C18B 179.93(16) . . . . ? C20B C21B C26B C18B 4.4(2) . . . . ? C19B C18B C26B C25B 166.23(17) . . . . ? C17B C18B C26B C25B 33.9(3) . . . . ? C19B C18B C26B C21B -7.1(2) . . . . ? C17B C18B C26B C21B -139.41(17) . . . . ? C20B C19B C27B O7B -27.1(3) . . . . ? C18B C19B C27B O7B 164.9(2) . . . . ? C20B C19B C27B O6B 153.44(19) . . . . ? C18B C19B C27B O6B -14.6(3) . . . . ? O7B C27B O6B C28B 2.7(3) . . . . ? C19B C27B O6B C28B -177.84(18) . . . . ? C27B O6B C28B C29B 97.5(3) . . . . ? C21B C22B O8B C30B 100.6(2) . . . . ? C23B C22B O8B C30B -82.9(2) . . . . ? C22B C23B O9B C31B -80.3(2) . . . . ? C24B C23B O9B C31B 103.5(2) . . . . ? C25B C24B O10B C32B -117.5(2) . . . . ? C23B C24B O10B C32B 65.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 0.839 _refine_diff_density_max 0.233 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.033