data_2003789 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1646 _journal_page_last 1648 _publ_section_title ; 16\b-(Acetyloxy)-3\b-[(2,6-dideoxy-3-O-methyl-L-arabino- hexopyranosyl)oxy]-14-hydroxycard-20(22)-enolide Dihydrate ; _chemical_formula_sum 'C32 H52 O11' _chemical_formula_structural 'C32 H48 O9.2H2O' _chemical_formula_weight 612.74 _symmetry_cell_setting orthorhombic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_length_a 9.534(4) _cell_length_b 14.283(4) _cell_length_c 24.020(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3270.9(18) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 30 _exptl_absorpt_coefficient_mu 0.765 _cell_measurement_temperature 293(2) _exptl_crystal_description rectangular _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_colour colourless _chemical_compound_source ? _diffrn_measurement_device 'P4' _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 3221 _reflns_number_total 3031 _reflns_number_observed 2942 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_theta_max 56.74 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.5 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0383 _refine_ls_wR_factor_obs 0.1033 _refine_ls_wR_factor_all 0.1044 _refine_ls_goodness_of_fit_obs 1.117 _refine_ls_goodness_of_fit_all 1.109 _refine_ls_number_reflns 3031 _refine_ls_number_parameters 587 _refine_ls_hydrogen_treatment 'All H atoms are refined isotropically' _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0602P)^2^ + 0.9230P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.039 _refine_diff_density_max 0.18 _refine_diff_density_min -0.22 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0181 0.0091 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.0000 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0492 0.0322 _refine_ls_abs_structure_details 'taken from the sugar substituent' _refine_ls_abs_structure_Flack 0.70(26) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 1 0.6945(5) 1.0205(2) 0.9269(2) 0.0577(10) C2 1 0.7075(5) 0.9425(3) 0.88465(15) 0.0490(8) C3 1 0.6755(3) 0.8464(2) 0.90966(13) 0.0399(7) C4 1 0.5298(4) 0.8407(2) 0.93757(12) 0.0406(7) C5 1 0.5179(5) 0.9245(3) 0.97887(14) 0.0557(9) C6 1 0.5519(5) 1.0190(3) 0.9534(2) 0.0627(11) C7 1 0.5201(5) 0.7510(3) 0.9725(2) 0.0641(11) C8 1 0.4129(3) 0.8427(2) 0.89253(11) 0.0348(7) C9 1 0.4326(3) 0.7636(2) 0.84925(12) 0.0332(6) C10 1 0.5773(3) 0.7685(2) 0.82258(14) 0.0398(7) C11 1 0.6937(4) 0.7684(3) 0.8664(2) 0.0489(9) C12 1 0.2648(4) 0.8391(3) 0.91652(13) 0.0469(8) C13 1 0.1526(4) 0.8416(3) 0.87126(13) 0.0423(7) C14 1 0.1646(3) 0.7592(2) 0.82979(12) 0.0357(7) C15 1 0.3153(3) 0.7592(2) 0.80554(11) 0.0317(6) C16 1 0.3139(3) 0.8404(2) 0.76382(12) 0.0367(7) C17 1 0.1622(3) 0.8528(2) 0.74509(12) 0.0354(7) C18 1 0.0702(3) 0.7837(2) 0.77847(12) 0.0361(7) C19 1 0.1203(4) 0.6674(3) 0.8587(2) 0.0489(8) C20 1 0.0112(3) 0.7048(2) 0.74396(12) 0.0388(7) C21 1 0.0883(4) 0.6266(3) 0.7151(2) 0.0471(8) C22 1 -0.1445(4) 0.6140(2) 0.69534(15) 0.0499(8) C23 1 -0.1239(4) 0.6955(2) 0.73134(14) 0.0460(8) C24 1 0.0452(5) 0.8772(3) 0.6591(2) 0.0613(10) C25 1 0.0482(7) 0.8570(5) 0.5982(2) 0.096(2) C26 1 0.9189(5) 1.0643(3) 0.9645(2) 0.0605(11) C27 1 1.0370(5) 1.0244(3) 0.9983(2) 0.0648(11) C28 1 1.0235(4) 1.0376(3) 1.0598(2) 0.0542(9) C29 1 0.9832(4) 1.1389(2) 1.07300(15) 0.0513(9) C30 1 0.8562(4) 1.1663(2) 1.03938(14) 0.0507(9) C31 1 1.1538(6) 0.9830(3) 1.1403(2) 0.0815(14) C32 1 0.8039(7) 1.2650(3) 1.0485(2) 0.0791(14) O1 1 0.3358(2) 0.67634(14) 0.77133(8) 0.0370(5) O2 1 -0.0195(3) 0.5748(2) 0.68516(10) 0.0524(6) O3 1 -0.2511(3) 0.5805(2) 0.67625(13) 0.0695(8) O4 1 0.1526(2) 0.8365(2) 0.68553(8) 0.0455(5) O5 1 -0.0389(4) 0.9254(2) 0.6832(2) 0.0885(10) O6 1 0.7995(3) 1.0072(2) 0.97005(10) 0.0575(7) O7 1 0.8869(3) 1.1585(2) 0.98078(9) 0.0623(7) O8 1 1.1560(3) 1.0090(2) 1.0837(2) 0.0811(9) O9 1 0.9554(3) 1.1472(2) 1.13076(10) 0.0608(7) OW1 1 1.0121(4) 1.3232(2) 1.17041(11) 0.0624(7) OW2 1 0.8200(4) 1.0131(2) 1.1962(2) 0.0989(13) H1 1 0.7087(40) 1.0828(28) 0.9063(15) 0.058(10) H2A 1 0.7977(44) 0.9495(26) 0.8705(15) 0.055(11) H2B 1 0.6509(44) 0.9589(28) 0.8524(18) 0.065(11) H3 1 0.7398(33) 0.8348(22) 0.9409(13) 0.036(8) H5A 1 0.5894(46) 0.9121(31) 1.0080(18) 0.073(13) H5B 1 0.4307(46) 0.9197(31) 0.9980(17) 0.066(12) H6A 1 0.4819(45) 1.0296(29) 0.9267(17) 0.068(12) H6B 1 0.5540(44) 1.0675(31) 0.9827(17) 0.069(11) H7A 1 0.4299(53) 0.7598(37) 0.9964(20) 0.082(14) H7B 1 0.5928(52) 0.7495(36) 0.9987(20) 0.077(13) H7C 1 0.5018(58) 0.6973(38) 0.9509(20) 0.099(17) H8 1 0.4169(35) 0.8958(24) 0.8726(13) 0.040(9) H9 1 0.4263(26) 0.6994(19) 0.8713(10) 0.019(6) H10A 1 0.5877(33) 0.7192(23) 0.7938(12) 0.035(8) H10B 1 0.5821(33) 0.8216(24) 0.8013(12) 0.030(8) H11A 1 0.7831(43) 0.7750(28) 0.8493(16) 0.060(11) H11B 1 0.6962(41) 0.7036(29) 0.8902(16) 0.063(11) H12A 1 0.2486(45) 0.8897(30) 0.9432(17) 0.070(12) H12B 1 0.2512(42) 0.7819(29) 0.9383(16) 0.062(11) H13A 1 0.0542(40) 0.8368(25) 0.8892(14) 0.055(10) H13B 1 0.1612(33) 0.9006(22) 0.8500(12) 0.033(8) H16A 1 0.3715(39) 0.8319(25) 0.7279(14) 0.055(10) H16B 1 0.3378(33) 0.9040(22) 0.7842(12) 0.035(8) H17 1 0.1312(32) 0.9116(22) 0.7517(11) 0.031(7) H18 1 -0.0161(37) 0.8167(22) 0.7929(12) 0.038(8) H19A 1 0.0276(50) 0.6784(30) 0.8748(17) 0.070(12) H19B 1 0.1237(49) 0.6202(32) 0.8317(18) 0.072(13) H19C 1 0.1861(51) 0.6531(35) 0.8928(20) 0.089(14) H21A 1 0.1482(44) 0.6522(29) 0.6882(15) 0.056(11) H21B 1 0.1265(42) 0.5841(28) 0.7418(16) 0.060(11) H23 1 -0.2002(42) 0.7351(28) 0.7448(16) 0.061(11) H25A 1 0.1261(50) 0.8167(30) 0.5900(17) 0.197(22) H25B 1 0.0580(49) 0.9145(32) 0.5779(18) 0.252(24) H25C 1 -0.0375(51) 0.8267(35) 0.5875(20) 0.174(21) H26 1 0.9503(33) 1.0666(22) 0.9251(13) 0.039(8) H27A 1 1.1059(51) 1.0554(37) 0.9878(19) 0.078(15) H27B 1 1.0466(66) 0.9513(48) 0.9882(23) 0.123(20) H28 1 0.9433(38) 0.9974(23) 1.0779(13) 0.040(8) H29 1 1.0552(40) 1.1734(27) 1.0624(15) 0.052(10) H30 1 0.7817(41) 1.1192(27) 1.0499(15) 0.056(11) H31A 1 1.2611(63) 0.9577(38) 1.1473(21) 0.103(17) H31B 1 1.0587(70) 0.9392(46) 1.1449(25) 0.138(22) H31C 1 1.1438(66) 1.0447(47) 1.1643(25) 0.126(20) H32A 1 0.7740(51) 1.2822(34) 1.0844(20) 0.084(15) H32B 1 0.7149(65) 1.2737(41) 1.0230(22) 0.114(19) H32C 1 0.8889(50) 1.3004(32) 1.0387(18) 0.069(13) HO1 1 0.3405(46) 0.6288(30) 0.7929(15) 0.059(12) HO9 1 0.9684(51) 1.1973(35) 1.1441(18) 0.077(14) H1W1 1 0.9426(52) 1.3536(33) 1.1772(19) 0.072(15) H2W1 1 1.0627(63) 1.3366(40) 1.2087(23) 0.122(19) H1W2 1 0.8740(80) 1.0630(55) 1.1781(29) 0.155(27) H2W2 1 0.7165(73) 1.0274(45) 1.1850(24) 0.121(21) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C1 0.090(3) -0.003(2) -0.013(2) 0.035(2) -0.002(2) 0.049(2) C2 0.060(2) -0.010(2) -0.001(2) 0.045(2) -0.003(2) 0.043(2) C3 0.043(2) 0.002(2) -0.0062(15) 0.036(2) -0.0038(14) 0.041(2) C4 0.046(2) 0.002(2) -0.0010(14) 0.041(2) 0.0028(14) 0.0348(14) C5 0.059(2) 0.001(2) -0.004(2) 0.074(2) -0.011(2) 0.034(2) C6 0.086(3) 0.021(2) -0.013(2) 0.050(2) -0.022(2) 0.053(2) C7 0.069(3) -0.014(2) -0.020(2) 0.071(3) 0.025(2) 0.052(2) C8 0.040(2) 0.003(2) 0.0013(13) 0.036(2) -0.0007(14) 0.0285(13) C9 0.0339(15) 0.0008(13) 0.0006(13) 0.0299(14) 0.0028(13) 0.0357(15) C10 0.036(2) 0.002(2) 0.0026(14) 0.037(2) -0.011(2) 0.046(2) C11 0.036(2) 0.003(2) -0.001(2) 0.048(2) -0.017(2) 0.062(2) C12 0.043(2) 0.003(2) 0.0040(14) 0.062(2) -0.010(2) 0.036(2) C13 0.037(2) 0.007(2) 0.0034(14) 0.050(2) -0.007(2) 0.040(2) C14 0.038(2) -0.0010(15) 0.0042(13) 0.0350(15) 0.0028(13) 0.0337(14) C15 0.0357(15) 0.0007(13) 0.0020(12) 0.0279(14) -0.0027(12) 0.0314(14) C16 0.042(2) 0.0009(14) 0.0003(14) 0.0304(15) 0.0020(13) 0.038(2) C17 0.043(2) 0.0058(15) -0.0048(14) 0.0274(15) 0.0009(13) 0.0362(15) C18 0.036(2) 0.0057(14) -0.0001(14) 0.0325(15) -0.0054(13) 0.0396(15) C19 0.050(2) -0.006(2) 0.006(2) 0.051(2) 0.012(2) 0.046(2) C20 0.043(2) -0.0007(15) -0.0004(14) 0.0344(15) 0.0012(13) 0.0394(15) C21 0.043(2) 0.000(2) -0.006(2) 0.039(2) -0.012(2) 0.060(2) C22 0.050(2) 0.000(2) -0.005(2) 0.038(2) -0.004(2) 0.062(2) C23 0.040(2) -0.002(2) -0.001(2) 0.044(2) -0.009(2) 0.054(2) C24 0.066(2) -0.013(2) -0.022(2) 0.054(2) 0.020(2) 0.065(2) C25 0.099(4) -0.029(4) -0.031(3) 0.136(5) 0.017(3) 0.054(2) C26 0.086(3) -0.017(2) 0.010(2) 0.045(2) -0.011(2) 0.050(2) C27 0.062(2) -0.011(2) 0.011(2) 0.056(2) -0.019(2) 0.076(3) C28 0.045(2) -0.001(2) -0.003(2) 0.046(2) -0.008(2) 0.072(2) C29 0.060(2) -0.016(2) 0.000(2) 0.039(2) -0.004(2) 0.056(2) C30 0.062(2) -0.007(2) -0.004(2) 0.033(2) -0.005(2) 0.057(2) C31 0.088(3) 0.002(3) -0.032(3) 0.054(2) -0.010(2) 0.103(4) C32 0.103(4) 0.008(3) -0.016(3) 0.046(2) -0.017(2) 0.087(3) O1 0.0427(11) 0.0011(10) 0.0014(10) 0.0286(10) -0.0047(9) 0.0395(11) O2 0.0512(14) 0.0001(12) -0.0080(12) 0.0395(12) -0.0142(11) 0.0665(14) O3 0.0512(15) -0.0076(13) -0.018(2) 0.057(2) -0.016(2) 0.100(2) O4 0.0544(12) -0.0007(12) -0.0056(10) 0.0441(12) 0.0043(10) 0.0379(10) O5 0.078(2) 0.029(2) -0.032(2) 0.079(2) 0.005(2) 0.108(2) O6 0.079(2) -0.0198(14) -0.0129(13) 0.0424(13) -0.0031(11) 0.0510(13) O7 0.095(2) -0.0216(14) -0.0018(14) 0.0397(12) -0.0011(11) 0.0521(12) O8 0.057(2) 0.001(2) -0.012(2) 0.074(2) -0.017(2) 0.112(2) O9 0.088(2) -0.0069(14) -0.0016(14) 0.0408(13) -0.0075(12) 0.0536(13) OW1 0.076(2) 0.010(2) -0.0148(15) 0.0544(15) -0.0086(12) 0.0568(15) OW2 0.082(2) 0.003(2) 0.015(2) 0.056(2) 0.038(2) 0.159(4)