# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 182/1081 data_stud96 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H34 O12' _chemical_formula_weight 502.50 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.425(6) _cell_length_b 23.566(7) _cell_length_c 17.545(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.36(4) _cell_angle_gamma 90.00 _cell_volume 2656(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4309 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1840 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 24.11 _reflns_number_total 4309 _reflns_number_gt 2004 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 SHELXL _refine_ls_extinction_coef 0.110(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 2(4) _refine_ls_number_reflns 4309 _refine_ls_number_parameters 646 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2519 _refine_ls_R_factor_gt 0.1276 _refine_ls_wR_factor_ref 0.2893 _refine_ls_wR_factor_gt 0.2426 _refine_ls_goodness_of_fit_ref 1.340 _refine_ls_restrained_S_all 1.340 _refine_ls_shift/su_max 0.077 _refine_ls_shift/su_mean 0.014 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.2181(17) 0.3407(6) 0.4262(8) 0.076(4) Uani 1 1 d . . . O2 O 0.1186(14) 0.3086(5) 0.4544(6) 0.057(3) Uani 1 1 d . . . O6 O -0.328(3) 0.1577(9) 0.4374(12) 0.150(8) Uani 1 1 d . . . O1' O 0.2475(14) 0.3960(5) 0.4434(7) 0.058(3) Uani 1 1 d . . . O2' O 0.2757(16) 0.2998(5) 0.6032(7) 0.055(3) Uani 1 1 d . . . O3' O 0.6334(16) 0.3743(5) 0.6268(7) 0.056(3) Uani 1 1 d . . . O4' O 0.5417(17) 0.4873(5) 0.5747(7) 0.065(4) Uani 1 1 d . . . O6' O 0.5188(18) 0.4693(6) 0.3730(8) 0.075(4) Uani 1 1 d . . . O7' O 0.582(3) 0.5544(9) 0.3269(11) 0.142(8) Uani 1 1 d . . . O9' O 0.554(3) 0.2427(7) 0.5843(12) 0.128(7) Uani 1 1 d . . . O11' O 0.479(3) 0.3802(10) 0.7417(9) 0.130(7) Uani 1 1 d . . . O13' O 0.845(2) 0.4970(7) 0.5192(10) 0.110(6) Uani 1 1 d . . . C2 C -0.1033(19) 0.2960(8) 0.4561(11) 0.060(5) Uani 1 1 d . . . H2 H -0.1459 0.2891 0.5088 0.071 Uiso 1 1 calc R . . C3 C -0.149(2) 0.2417(8) 0.4067(9) 0.051(5) Uani 1 1 d . . . C4 C -0.347(3) 0.2601(10) 0.3651(12) 0.074(6) Uani 1 1 d . . . H4 H -0.4681 0.2539 0.3980 0.089 Uiso 1 1 calc R . . C5 C -0.311(4) 0.3237(12) 0.3554(14) 0.120(10) Uani 1 1 d . . . H5A H -0.2180 0.3311 0.3132 0.144 Uiso 1 1 calc R . . H5B H -0.4410 0.3436 0.3466 0.144 Uiso 1 1 calc R . . C6 C -0.192(3) 0.1903(10) 0.4581(13) 0.084(7) Uani 1 1 d . . . C7 C -0.040(3) 0.1772(10) 0.5189(14) 0.094(7) Uani 1 1 d . . . H7A H -0.0344 0.2087 0.5545 0.113 Uiso 1 1 calc R . . H7B H 0.0971 0.1731 0.4966 0.113 Uiso 1 1 calc R . . C8 C -0.096(5) 0.1220(11) 0.5628(16) 0.130(10) Uani 1 1 d . . . H8A H 0.0294 0.1042 0.5811 0.195 Uiso 1 1 calc R . . H8B H -0.1683 0.0964 0.5293 0.195 Uiso 1 1 calc R . . H8C H -0.1833 0.1312 0.6053 0.195 Uiso 1 1 calc R . . C9 C 0.035(2) 0.2285(8) 0.3535(10) 0.060(5) Uani 1 1 d . . . H9A H 0.1549 0.2184 0.3836 0.090 Uiso 1 1 calc R . . H9B H 0.0663 0.2614 0.3234 0.090 Uiso 1 1 calc R . . H9C H -0.0012 0.1975 0.3205 0.090 Uiso 1 1 calc R . . C10 C -0.386(4) 0.2310(12) 0.2857(14) 0.115(9) Uani 1 1 d . . . H10A H -0.2803 0.2427 0.2506 0.172 Uiso 1 1 calc R . . H10B H -0.5203 0.2421 0.2662 0.172 Uiso 1 1 calc R . . H10C H -0.3817 0.1906 0.2916 0.172 Uiso 1 1 calc R . . C1' C 0.173(2) 0.3558(7) 0.4966(10) 0.048(5) Uani 1 1 d . . . H1' H 0.0566 0.3704 0.5264 0.057 Uiso 1 1 calc R . . C2' C 0.355(2) 0.3385(7) 0.5465(9) 0.042(4) Uani 1 1 d . . . H2' H 0.4631 0.3201 0.5160 0.050 Uiso 1 1 calc R . . C3' C 0.4437(19) 0.3902(7) 0.5881(9) 0.045(4) Uani 1 1 d . . . H3' H 0.3423 0.4049 0.6247 0.054 Uiso 1 1 calc R . . C4' C 0.498(2) 0.4361(8) 0.5294(11) 0.060(5) Uani 1 1 d . . . H4' H 0.6183 0.4250 0.4989 0.072 Uiso 1 1 calc R . . C5' C 0.310(2) 0.4472(7) 0.4796(10) 0.049(5) Uani 1 1 d . . . H5' H 0.1955 0.4610 0.5114 0.059 Uiso 1 1 calc R . . C6' C 0.356(2) 0.4914(8) 0.4179(11) 0.065(5) Uani 1 1 d . . . H6'1 H 0.2331 0.4980 0.3867 0.077 Uiso 1 1 calc R . . H6'2 H 0.3978 0.5270 0.4410 0.077 Uiso 1 1 calc R . . C7' C 0.634(4) 0.5049(11) 0.3306(13) 0.082(7) Uani 1 1 d . . . C8' C 0.800(4) 0.4789(14) 0.2862(15) 0.140(12) Uani 1 1 d . . . H8'1 H 0.8316 0.4422 0.3068 0.210 Uiso 1 1 calc R . . H8'2 H 0.9214 0.5025 0.2885 0.210 Uiso 1 1 calc R . . H8'3 H 0.7550 0.4750 0.2342 0.210 Uiso 1 1 calc R . . C9' C 0.397(3) 0.2548(10) 0.6201(14) 0.081(7) Uani 1 1 d . . . C10' C 0.302(4) 0.2167(11) 0.6750(16) 0.118(10) Uani 1 1 d . . . H10D H 0.1668 0.2309 0.6886 0.177 Uiso 1 1 calc R . . H10E H 0.3879 0.2144 0.7198 0.177 Uiso 1 1 calc R . . H10F H 0.2874 0.1796 0.6529 0.177 Uiso 1 1 calc R . . C11' C 0.622(3) 0.3701(9) 0.7003(12) 0.071(6) Uani 1 1 d . . . C12' C 0.842(4) 0.3486(13) 0.7316(15) 0.131(11) Uani 1 1 d . . . H12A H 0.9267 0.3808 0.7449 0.196 Uiso 1 1 calc R . . H12B H 0.9103 0.3269 0.6928 0.196 Uiso 1 1 calc R . . H12C H 0.8218 0.3254 0.7758 0.196 Uiso 1 1 calc R . . C13' C 0.723(3) 0.5106(10) 0.5684(15) 0.093(8) Uani 1 1 d . . . C14' C 0.731(4) 0.5646(10) 0.6105(16) 0.108(8) Uani 1 1 d . . . H14A H 0.7507 0.5571 0.6639 0.162 Uiso 1 1 calc R . . H14B H 0.6033 0.5849 0.6029 0.162 Uiso 1 1 calc R . . H14C H 0.8453 0.5871 0.5922 0.162 Uiso 1 1 calc R . . O21 O 0.7197(17) 0.0251(5) 0.9266(7) 0.066(4) Uani 1 1 d . . . O22 O 0.3865(14) 0.0571(5) 0.9545(7) 0.050(3) Uani 1 1 d . . . O26 O 0.831(3) 0.2066(8) 0.9375(11) 0.142(8) Uani 1 1 d . . . O21' O 0.2550(14) -0.0314(5) 0.9420(6) 0.051(3) Uani 1 1 d . . . O22' O 0.2230(16) 0.0668(5) 1.1022(7) 0.058(3) Uani 1 1 d . . . O23' O -0.1310(15) -0.0088(5) 1.1287(7) 0.061(3) Uani 1 1 d . . . O24' O -0.0433(15) -0.1212(5) 1.0749(6) 0.055(3) Uani 1 1 d . . . O26' O -0.0247(19) -0.1044(6) 0.8731(8) 0.074(4) Uani 1 1 d . . . O27' O -0.080(4) -0.1874(10) 0.8281(12) 0.151(8) Uani 1 1 d . . . O29' O -0.055(2) 0.1218(7) 1.0845(12) 0.121(7) Uani 1 1 d . . . O31' O 0.021(3) -0.0100(9) 1.2412(10) 0.121(6) Uani 1 1 d . . . O33' O -0.3547(18) -0.1284(7) 1.0229(11) 0.118(7) Uani 1 1 d . . . C22 C 0.595(2) 0.0699(7) 0.9572(11) 0.054(5) Uani 1 1 d . . . H22 H 0.6367 0.0769 1.0102 0.065 Uiso 1 1 calc R . . C23 C 0.651(2) 0.1235(9) 0.9075(11) 0.065(6) Uani 1 1 d . . . C24 C 0.843(3) 0.1021(10) 0.8615(11) 0.076(6) Uani 1 1 d . . . H24 H 0.9662 0.1077 0.8938 0.091 Uiso 1 1 calc R . . C25 C 0.807(2) 0.0407(9) 0.8563(10) 0.063(5) Uani 1 1 d . . . H25A H 0.7121 0.0320 0.8147 0.075 Uiso 1 1 calc R . . H25B H 0.9368 0.0207 0.8480 0.075 Uiso 1 1 calc R . . C26 C 0.685(3) 0.1765(8) 0.9551(12) 0.070(6) Uani 1 1 d . . . C27 C 0.542(4) 0.1870(10) 1.0218(13) 0.095(7) Uani 1 1 d . . . H27A H 0.3998 0.1870 1.0032 0.114 Uiso 1 1 calc R . . H27B H 0.5565 0.1556 1.0572 0.114 Uiso 1 1 calc R . . C28 C 0.579(5) 0.2411(12) 1.0647(18) 0.145(12) Uani 1 1 d . . . H28A H 0.4757 0.2452 1.1035 0.217 Uiso 1 1 calc R . . H28B H 0.5710 0.2726 1.0301 0.217 Uiso 1 1 calc R . . H28C H 0.7150 0.2401 1.0879 0.217 Uiso 1 1 calc R . . C29 C 0.461(3) 0.1390(10) 0.8543(12) 0.086(7) Uani 1 1 d . . . H29A H 0.4262 0.1069 0.8231 0.128 Uiso 1 1 calc R . . H29B H 0.4986 0.1704 0.8223 0.128 Uiso 1 1 calc R . . H29C H 0.3441 0.1493 0.8849 0.128 Uiso 1 1 calc R . . C30 C 0.885(4) 0.1311(13) 0.7871(15) 0.146(13) Uani 1 1 d . . . H30A H 0.9084 0.1708 0.7959 0.218 Uiso 1 1 calc R . . H30B H 0.7667 0.1264 0.7538 0.218 Uiso 1 1 calc R . . H30C H 1.0053 0.1146 0.7640 0.218 Uiso 1 1 calc R . . C21' C 0.327(2) 0.0104(7) 0.9948(10) 0.050(4) Uani 1 1 d . . . H21' H 0.4442 -0.0043 1.0250 0.060 Uiso 1 1 calc R . . C22' C 0.143(2) 0.0267(8) 1.0475(9) 0.052(5) Uani 1 1 d . . . H22' H 0.0331 0.0448 1.0170 0.062 Uiso 1 1 calc R . . C23' C 0.055(2) -0.0245(7) 1.0881(9) 0.050(4) Uani 1 1 d . . . H23' H 0.1586 -0.0386 1.1248 0.060 Uiso 1 1 calc R . . C24' C 0.007(2) -0.0706(7) 1.0319(9) 0.044(4) Uani 1 1 d . . . H24' H -0.1157 -0.0594 1.0019 0.053 Uiso 1 1 calc R . . C25' C 0.188(2) -0.0823(8) 0.9770(10) 0.057(5) Uani 1 1 d . . . H25' H 0.3048 -0.0965 1.0078 0.069 Uiso 1 1 calc R . . C26' C 0.147(3) -0.1245(9) 0.9180(12) 0.076(6) Uani 1 1 d . . . H26A H 0.2684 -0.1295 0.8863 0.091 Uiso 1 1 calc R . . H26B H 0.1124 -0.1607 0.9410 0.091 Uiso 1 1 calc R . . C27' C -0.138(4) -0.1384(14) 0.8298(15) 0.096(8) Uani 1 1 d . . . C28' C -0.311(4) -0.1127(12) 0.7907(13) 0.114(9) Uani 1 1 d . . . H28D H -0.2596 -0.0864 0.7535 0.170 Uiso 1 1 calc R . . H28E H -0.3964 -0.0930 0.8266 0.170 Uiso 1 1 calc R . . H28F H -0.3913 -0.1416 0.7656 0.170 Uiso 1 1 calc R . . C29' C 0.100(4) 0.1139(9) 1.1162(11) 0.067(6) Uani 1 1 d . . . C30' C 0.215(4) 0.1472(11) 1.1779(13) 0.107(8) Uani 1 1 d . . . H30D H 0.3610 0.1393 1.1751 0.160 Uiso 1 1 calc R . . H30E H 0.1636 0.1362 1.2271 0.160 Uiso 1 1 calc R . . H30F H 0.1915 0.1870 1.1704 0.160 Uiso 1 1 calc R . . C31' C -0.140(4) -0.0030(10) 1.2026(12) 0.080(7) Uani 1 1 d . . . C32' C -0.329(4) 0.0194(12) 1.2322(14) 0.146(12) Uani 1 1 d . . . H32A H -0.4445 -0.0024 1.2132 0.219 Uiso 1 1 calc R . . H32B H -0.3443 0.0582 1.2164 0.219 Uiso 1 1 calc R . . H32C H -0.3258 0.0175 1.2868 0.219 Uiso 1 1 calc R . . C33' C -0.224(3) -0.1498(8) 1.0660(14) 0.072(6) Uani 1 1 d . . . C34' C -0.239(3) -0.1972(11) 1.1142(13) 0.092(7) Uani 1 1 d . . . H34A H -0.1923 -0.1872 1.1644 0.138 Uiso 1 1 calc R . . H34B H -0.1544 -0.2274 1.0947 0.138 Uiso 1 1 calc R . . H34C H -0.3816 -0.2095 1.1162 0.138 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.040(7) 0.082(10) 0.107(11) -0.006(8) -0.031(7) 0.026(7) O2 0.028(6) 0.077(9) 0.065(8) -0.008(7) -0.005(5) -0.022(6) O6 0.162(17) 0.127(16) 0.161(19) -0.015(14) -0.035(14) -0.081(15) O1' 0.033(6) 0.060(9) 0.080(9) 0.023(7) -0.003(6) -0.002(6) O2' 0.049(7) 0.049(8) 0.067(8) 0.012(6) 0.005(6) -0.008(6) O3' 0.047(6) 0.061(8) 0.060(8) -0.001(7) 0.006(6) 0.012(6) O4' 0.051(7) 0.068(9) 0.077(9) -0.010(7) 0.017(6) -0.014(6) O6' 0.057(7) 0.063(9) 0.103(10) 0.015(8) 0.005(7) -0.010(7) O7' 0.162(17) 0.100(15) 0.163(19) 0.063(14) 0.005(14) -0.059(13) O9' 0.107(13) 0.083(12) 0.196(19) 0.052(12) 0.067(13) 0.048(10) O11' 0.153(15) 0.191(19) 0.048(10) 0.018(11) 0.012(10) 0.005(15) O13' 0.079(10) 0.101(12) 0.151(15) -0.035(11) 0.044(10) -0.023(9) C2 0.002(7) 0.089(14) 0.088(14) -0.010(12) 0.014(7) -0.013(8) C3 0.034(9) 0.071(13) 0.049(11) -0.016(10) 0.004(8) -0.013(8) C4 0.032(10) 0.12(2) 0.075(15) -0.028(13) -0.014(9) -0.009(11) C5 0.13(2) 0.12(2) 0.11(2) -0.018(17) -0.098(17) 0.027(17) C6 0.067(13) 0.110(19) 0.075(16) -0.034(14) 0.022(12) -0.048(14) C7 0.097(16) 0.077(16) 0.108(19) 0.022(14) -0.006(15) -0.051(13) C8 0.19(3) 0.070(17) 0.13(2) 0.028(17) -0.01(2) -0.024(18) C9 0.044(9) 0.075(13) 0.062(12) -0.017(10) 0.007(8) 0.019(9) C10 0.083(15) 0.15(2) 0.11(2) -0.004(18) -0.051(14) -0.023(16) C1' 0.023(8) 0.058(12) 0.062(12) -0.013(10) -0.007(8) -0.024(8) C2' 0.015(7) 0.045(10) 0.066(11) 0.019(9) 0.001(7) -0.010(7) C3' 0.015(7) 0.062(12) 0.059(11) 0.021(10) -0.003(7) 0.004(8) C4' 0.024(9) 0.072(13) 0.084(15) -0.005(12) -0.004(9) -0.007(8) C5' 0.033(9) 0.040(11) 0.074(13) 0.004(10) 0.023(8) 0.001(8) C6' 0.038(9) 0.051(12) 0.104(15) 0.013(11) -0.004(10) 0.011(9) C7' 0.098(17) 0.062(15) 0.087(17) 0.022(14) -0.007(13) -0.049(14) C8' 0.14(2) 0.18(3) 0.099(19) -0.02(2) 0.062(18) -0.05(2) C9' 0.054(13) 0.073(16) 0.117(19) 0.022(15) 0.008(13) -0.025(12) C10' 0.112(18) 0.088(18) 0.15(2) 0.041(18) -0.041(17) -0.038(15) C11' 0.099(16) 0.068(14) 0.046(14) 0.001(11) 0.003(11) -0.030(12) C12' 0.090(16) 0.15(3) 0.15(2) -0.03(2) -0.085(16) 0.018(17) C13' 0.054(13) 0.086(18) 0.14(2) -0.065(16) 0.028(14) -0.014(12) C14' 0.104(17) 0.064(16) 0.15(2) 0.007(16) 0.015(16) -0.033(13) O21 0.055(7) 0.053(8) 0.089(9) 0.017(7) 0.042(7) -0.003(6) O22 0.021(5) 0.048(7) 0.081(8) 0.004(7) -0.001(5) -0.009(5) O26 0.146(15) 0.119(15) 0.161(18) 0.001(13) 0.037(13) -0.093(14) O21' 0.031(6) 0.052(7) 0.071(8) -0.001(7) 0.009(5) -0.013(5) O22' 0.051(7) 0.054(8) 0.070(8) -0.001(7) 0.000(6) -0.007(6) O23' 0.041(6) 0.074(9) 0.069(9) 0.011(7) 0.013(6) 0.003(6) O24' 0.042(6) 0.041(7) 0.082(9) 0.005(6) -0.007(6) -0.011(5) O26' 0.059(8) 0.074(9) 0.088(10) 0.001(8) -0.022(7) -0.008(7) O27' 0.19(2) 0.096(15) 0.17(2) -0.031(15) -0.072(15) -0.026(15) O29' 0.058(9) 0.099(13) 0.205(19) -0.035(13) -0.053(11) 0.033(9) O31' 0.132(14) 0.141(16) 0.092(12) 0.005(12) 0.007(11) 0.018(13) O33' 0.033(7) 0.104(12) 0.216(18) 0.079(12) -0.054(9) -0.031(7) C22 0.010(7) 0.056(11) 0.097(15) -0.006(11) 0.004(8) -0.013(8) C23 0.031(9) 0.089(16) 0.074(13) -0.004(12) 0.004(9) -0.019(9) C24 0.048(11) 0.102(19) 0.077(15) 0.035(13) -0.011(10) -0.028(11) C25 0.037(9) 0.104(18) 0.047(11) 0.010(11) 0.014(8) -0.001(10) C26 0.067(12) 0.047(12) 0.096(17) 0.009(12) -0.028(11) -0.028(10) C27 0.126(19) 0.071(16) 0.087(17) -0.003(13) 0.033(15) 0.025(14) C28 0.21(3) 0.073(18) 0.15(3) -0.028(19) 0.06(2) -0.005(19) C29 0.072(13) 0.108(19) 0.077(15) 0.043(13) -0.009(11) 0.000(12) C30 0.14(2) 0.17(3) 0.13(2) 0.09(2) 0.098(19) 0.04(2) C21' 0.043(9) 0.047(12) 0.061(11) 0.004(10) -0.010(8) -0.013(9) C22' 0.039(9) 0.071(13) 0.045(11) 0.004(10) -0.001(8) -0.011(9) C23' 0.035(9) 0.061(12) 0.056(11) 0.002(10) -0.006(8) -0.020(8) C24' 0.025(8) 0.050(11) 0.058(12) -0.012(9) 0.006(8) 0.002(7) C25' 0.041(10) 0.068(14) 0.063(13) 0.006(11) -0.005(9) -0.019(9) C26' 0.064(12) 0.068(14) 0.097(16) -0.028(13) 0.040(12) 0.015(11) C27' 0.085(17) 0.11(2) 0.10(2) -0.021(19) 0.021(15) -0.015(18) C28' 0.115(18) 0.13(2) 0.097(18) -0.004(17) -0.064(16) -0.017(18) C29' 0.083(15) 0.066(15) 0.051(12) -0.024(11) 0.009(11) -0.021(13) C30' 0.124(19) 0.11(2) 0.086(17) -0.037(15) 0.006(15) 0.023(16) C31' 0.094(16) 0.106(18) 0.040(14) 0.004(13) 0.039(12) -0.016(15) C32' 0.19(3) 0.13(2) 0.12(2) -0.050(19) 0.13(2) 0.01(2) C33' 0.046(11) 0.047(12) 0.123(18) 0.000(13) -0.003(12) -0.035(10) C34' 0.064(13) 0.11(2) 0.101(17) 0.032(15) 0.021(12) -0.033(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.39(2) . ? O1 C5 1.43(2) . ? O2 C1' 1.381(18) . ? O2 C2 1.457(15) . ? O6 C6 1.22(2) . ? O1' C1' 1.415(18) . ? O1' C5' 1.420(19) . ? O2' C9' 1.35(2) . ? O2' C2' 1.445(18) . ? O3' C11' 1.30(2) . ? O3' C3' 1.441(16) . ? O4' C13' 1.30(2) . ? O4' C4' 1.47(2) . ? O6' C7' 1.35(2) . ? O6' C6' 1.41(2) . ? O7' C7' 1.21(3) . ? O9' C9' 1.23(2) . ? O11' C11' 1.19(2) . ? O13' C13' 1.21(2) . ? C2 C3 1.57(2) . ? C3 C4 1.53(2) . ? C3 C6 1.53(3) . ? C3 C9 1.54(2) . ? C4 C5 1.53(3) . ? C4 C10 1.57(3) . ? C6 C7 1.47(3) . ? C7 C8 1.56(3) . ? C1' C2' 1.51(2) . ? C2' C3' 1.53(2) . ? C3' C4' 1.53(2) . ? C4' C5' 1.51(2) . ? C5' C6' 1.53(2) . ? C7' C8' 1.46(3) . ? C9' C10' 1.45(3) . ? C11' C12' 1.60(3) . ? C13' C14' 1.47(3) . ? O21 C25 1.406(18) . ? O21 C22 1.432(19) . ? O22 C21' 1.363(18) . ? O22 C22 1.374(15) . ? O26 C26 1.22(2) . ? O21' C25' 1.42(2) . ? O21' C21' 1.428(18) . ? O22' C29' 1.38(2) . ? O22' C22' 1.44(2) . ? O23' C31' 1.30(2) . ? O23' C23' 1.443(18) . ? O24' C33' 1.349(18) . ? O24' C24' 1.448(19) . ? O26' C27' 1.32(3) . ? O26' C26' 1.43(2) . ? O27' C27' 1.21(3) . ? O29' C29' 1.15(2) . ? O31' C31' 1.25(2) . ? O33' C33' 1.23(2) . ? C22 C23 1.58(3) . ? C23 C26 1.52(3) . ? C23 C24 1.56(3) . ? C23 C29 1.57(2) . ? C24 C25 1.47(3) . ? C24 C30 1.50(3) . ? C26 C27 1.51(3) . ? C27 C28 1.50(3) . ? C21' C22' 1.55(2) . ? C22' C23' 1.51(2) . ? C23' C24' 1.50(2) . ? C24' C25' 1.54(2) . ? C25' C26' 1.46(3) . ? C27' C28' 1.43(3) . ? C29' C30' 1.52(3) . ? C31' C32' 1.43(3) . ? C33' C34' 1.40(3) . ? 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 O1 C5 109.4(16) . . ? C1' O2 C2 113.5(12) . . ? C1' O1' C5' 111.7(13) . . ? C9' O2' C2' 116.3(13) . . ? C11' O3' C3' 115.7(14) . . ? C13' O4' C4' 118.1(14) . . ? C7' O6' C6' 119.3(17) . . ? O1 C2 O2 110.8(14) . . ? O1 C2 C3 108.2(14) . . ? O2 C2 C3 109.6(12) . . ? C4 C3 C6 110.8(16) . . ? C4 C3 C9 114.2(15) . . ? C6 C3 C9 109.6(15) . . ? C4 C3 C2 100.6(15) . . ? C6 C3 C2 110.6(14) . . ? C9 C3 C2 110.8(13) . . ? C3 C4 C5 101.8(15) . . ? C3 C4 C10 115.2(17) . . ? C5 C4 C10 111(2) . . ? O1 C5 C4 104.1(18) . . ? O6 C6 C7 124(2) . . ? O6 C6 C3 117(2) . . ? C7 C6 C3 118.0(16) . . ? C6 C7 C8 112(2) . . ? O2 C1' O1' 105.7(13) . . ? O2 C1' C2' 106.7(13) . . ? O1' C1' C2' 107.5(10) . . ? O2' C2' C1' 107.1(11) . . ? O2' C2' C3' 107.9(13) . . ? C1' C2' C3' 110.2(12) . . ? O3' C3' C2' 109.2(12) . . ? O3' C3' C4' 107.8(11) . . ? C2' C3' C4' 109.1(13) . . ? O4' C4' C5' 108.7(14) . . ? O4' C4' C3' 105.0(14) . . ? C5' C4' C3' 109.1(12) . . ? O1' C5' C4' 109.4(13) . . ? O1' C5' C6' 108.5(14) . . ? C4' C5' C6' 111.7(13) . . ? O6' C6' C5' 106.9(13) . . ? O7' C7' O6' 118(2) . . ? O7' C7' C8' 125(2) . . ? O6' C7' C8' 116(2) . . ? O9' C9' O2' 123.1(19) . . ? O9' C9' C10' 123(2) . . ? O2' C9' C10' 112.8(19) . . ? O11' C11' O3' 130(2) . . ? O11' C11' C12' 122(2) . . ? O3' C11' C12' 107.9(19) . . ? O13' C13' O4' 122.3(19) . . ? O13' C13' C14' 124(2) . . ? O4' C13' C14' 110.6(18) . . ? C25 O21 C22 111.3(14) . . ? C21' O22 C22 115.8(13) . . ? C25' O21' C21' 113.7(13) . . ? C29' O22' C22' 116.3(13) . . ? C31' O23' C23' 124.0(15) . . ? C33' O24' C24' 123.0(14) . . ? C27' O26' C26' 122.5(19) . . ? O22 C22 O21 111.9(13) . . ? O22 C22 C23 112.5(13) . . ? O21 C22 C23 104.6(13) . . ? C26 C23 C24 115.9(15) . . ? C26 C23 C29 104.1(17) . . ? C24 C23 C29 112.2(15) . . ? C26 C23 C22 112.9(15) . . ? C24 C23 C22 102.2(15) . . ? C29 C23 C22 109.7(13) . . ? C25 C24 C30 115(2) . . ? C25 C24 C23 103.0(14) . . ? C30 C24 C23 116.7(19) . . ? O21 C25 C24 105.5(15) . . ? O26 C26 C27 125(2) . . ? O26 C26 C23 117(2) . . ? C27 C26 C23 118.2(16) . . ? C28 C27 C26 116(2) . . ? O22 C21' O21' 108.1(13) . . ? O22 C21' C22' 109.0(13) . . ? O21' C21' C22' 108.1(12) . . ? O22' C22' C23' 110.0(13) . . ? O22' C22' C21' 106.8(12) . . ? C23' C22' C21' 111.8(15) . . ? O23' C23' C24' 110.0(11) . . ? O23' C23' C22' 109.9(14) . . ? C24' C23' C22' 110.1(14) . . ? O24' C24' C23' 107.5(13) . . ? O24' C24' C25' 110.4(12) . . ? C23' C24' C25' 112.8(12) . . ? O21' C25' C26' 108.9(15) . . ? O21' C25' C24' 110.6(14) . . ? C26' C25' C24' 115.5(13) . . ? O26' C26' C25' 107.7(15) . . ? O27' C27' O26' 115(3) . . ? O27' C27' C28' 129(3) . . ? O26' C27' C28' 116(3) . . ? O29' C29' O22' 122.4(17) . . ? O29' C29' C30' 132(2) . . ? O22' C29' C30' 105.4(18) . . ? O31' C31' O23' 119.0(18) . . ? O31' C31' C32' 124(2) . . ? O23' C31' C32' 116(2) . . ? O33' C33' O24' 116.6(17) . . ? O33' C33' C34' 129.9(16) . . ? O24' C33' C34' 113.1(19) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.11 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.651 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.128