 
data_a 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C34 H28 O8' 
_chemical_formula_weight          564.56 
 
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            ? 
_symmetry_space_group_name_H-M    ? 
 
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                    10.4605(8) 
_cell_length_b                    20.3913(13) 
_cell_length_c                    14.1238(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  102.144(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2945.2(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     93(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.40 
_exptl_crystal_size_min           0.40 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.273 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1184 
_exptl_absorpt_coefficient_mu     0.091 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.9646 
_exptl_absorpt_correction_T_max   0.9646 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       93(2) 
_diffrn_radiation_wavelength      0.71075 
_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             13829 
_diffrn_reflns_av_R_equivalents   0.0512 
_diffrn_reflns_av_sigmaI/netI     0.0700 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        26 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          3.12 
_diffrn_reflns_theta_max          27.48 
_reflns_number_total              6223 
_reflns_number_gt                 3453 
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1151P)²+0.9032P] where P=(Fo²+2Fc²)/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          6223 
_refine_ls_number_parameters      383 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1279 
_refine_ls_R_factor_gt            0.0626 
_refine_ls_wR_factor_ref          0.2300 
_refine_ls_wR_factor_gt           0.1630 
_refine_ls_goodness_of_fit_ref    1.078 
_refine_ls_restrained_S_all       1.078 
_refine_ls_shift/su_max           0.024 
_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 0.2913(3) -0.03951(13) 0.52638(18) 0.0256(6) Uani 1 1 d . . . 
C2 C 0.2350(3) 0.01705(13) 0.54746(18) 0.0256(6) Uani 1 1 d . . . 
C3 C 0.3528(3) -0.08632(13) 0.60411(19) 0.0274(6) Uani 1 1 d . . . 
C4 C 0.4357(3) -0.06482(14) 0.68926(19) 0.0289(7) Uani 1 1 d . . . 
H1 H 0.4630 -0.0203 0.6946 0.035 Uiso 1 1 calc R . . 
C5 C 0.4788(3) -0.10712(14) 0.7659(2) 0.0306(7) Uani 1 1 d . . . 
H2 H 0.5352 -0.0919 0.8234 0.037 Uiso 1 1 calc R . . 
C6 C 0.4388(3) -0.17162(14) 0.7577(2) 0.0323(7) Uani 1 1 d . . . 
C7 C 0.3636(4) -0.19569(14) 0.6732(2) 0.0357(8) Uani 1 1 d . . . 
H3 H 0.3403 -0.2408 0.6677 0.043 Uiso 1 1 calc R . . 
C8 C 0.3221(3) -0.15325(13) 0.5962(2) 0.0307(7) Uani 1 1 d . . . 
H4 H 0.2721 -0.1698 0.5370 0.037 Uiso 1 1 calc R . . 
O1 O 0.4655(3) -0.21144(11) 0.84027(15) 0.0423(6) Uani 1 1 d . . . 
C9 C 0.5876(4) -0.23636(15) 0.8686(2) 0.0386(8) Uani 1 1 d . . . 
C10 C 0.6052(5) -0.26604(18) 0.9673(2) 0.0512(11) Uani 1 1 d . . . 
H5 H 0.6804 -0.2958 0.9782 0.077 Uiso 1 1 calc R . . 
H6 H 0.5263 -0.2906 0.9723 0.077 Uiso 1 1 calc R . . 
H7 H 0.6202 -0.2312 1.0162 0.077 Uiso 1 1 calc R . . 
O2 O 0.6670(3) -0.23352(14) 0.8207(2) 0.0609(8) Uani 1 1 d . . . 
C11 C 0.2936(3) -0.06028(13) 0.42535(19) 0.0268(6) Uani 1 1 d . . . 
C12 C 0.4080(3) -0.08594(14) 0.4047(2) 0.0332(7) Uani 1 1 d . . . 
H8 H 0.4833 -0.0903 0.4552 0.040 Uiso 1 1 calc R . . 
C13 C 0.4139(4) -0.10533(14) 0.3115(2) 0.0335(7) Uani 1 1 d . . . 
H9 H 0.4927 -0.1225 0.2981 0.040 Uiso 1 1 calc R . . 
C14 C 0.3043(3) -0.09937(14) 0.23892(19) 0.0304(7) Uani 1 1 d . . . 
C15 C 0.1884(3) -0.07576(14) 0.2570(2) 0.0334(7) Uani 1 1 d . . . 
H10 H 0.1126 -0.0729 0.2065 0.040 Uiso 1 1 calc R . . 
C16 C 0.1845(3) -0.05629(13) 0.35004(19) 0.0290(7) Uani 1 1 d . . . 
H11 H 0.1050 -0.0397 0.3629 0.035 Uiso 1 1 calc R . . 
O3 O 0.3106(3) -0.12079(11) 0.14521(15) 0.0430(6) Uani 1 1 d . . . 
C17 C 0.3449(5) -0.0754(2) 0.0862(3) 0.0565(12) Uani 1 1 d . . . 
C18 C 0.3552(5) -0.1031(2) -0.0091(2) 0.0658(13) Uani 1 1 d . . . 
H12 H 0.3687 -0.0674 -0.0525 0.099 Uiso 1 1 calc R . . 
H13 H 0.2745 -0.1265 -0.0373 0.099 Uiso 1 1 calc R . . 
H14 H 0.4293 -0.1335 -0.0004 0.099 Uiso 1 1 calc R . . 
O4 O 0.3663(6) -0.02033(17) 0.1120(3) 0.124(2) Uani 1 1 d . . . 
C19 C 0.1904(3) 0.06974(13) 0.47478(18) 0.0249(6) Uani 1 1 d . . . 
C20 C 0.2634(3) 0.08909(13) 0.40773(18) 0.0256(6) Uani 1 1 d . . . 
H15 H 0.3432 0.0671 0.4065 0.031 Uiso 1 1 calc R . . 
C21 C 0.2226(3) 0.13945(13) 0.34306(19) 0.0294(7) Uani 1 1 d . . . 
H16 H 0.2735 0.1518 0.2976 0.035 Uiso 1 1 calc R . . 
C22 C 0.1080(4) 0.17138(13) 0.34503(19) 0.0318(7) Uani 1 1 d . . . 
C23 C 0.0333(3) 0.15481(14) 0.4106(2) 0.0334(7) Uani 1 1 d . . . 
H17 H -0.0456 0.1776 0.4115 0.040 Uiso 1 1 calc R . . 
C24 C 0.0750(3) 0.10415(13) 0.4755(2) 0.0299(7) Uani 1 1 d . . . 
H18 H 0.0241 0.0927 0.5213 0.036 Uiso 1 1 calc R . . 
O5 O 0.0705(3) 0.22428(10) 0.28161(15) 0.0390(6) Uani 1 1 d . . . 
C25 C -0.0287(4) 0.21356(16) 0.2054(2) 0.0408(9) Uani 1 1 d . . . 
C26 C -0.0585(6) 0.27259(19) 0.1434(3) 0.0723(15) Uani 1 1 d . . . 
H19 H 0.0210 0.2872 0.1232 0.108 Uiso 1 1 calc R . . 
H20 H -0.0904 0.3076 0.1799 0.108 Uiso 1 1 calc R . . 
H21 H -0.1258 0.2619 0.0859 0.108 Uiso 1 1 calc R . . 
O6 O -0.0844(3) 0.16235(13) 0.19122(17) 0.0597(9) Uani 1 1 d . . . 
C27 C 0.2118(3) 0.03146(13) 0.64611(18) 0.0265(6) Uani 1 1 d . . . 
C28 C 0.2325(3) 0.09372(14) 0.6873(2) 0.0313(7) Uani 1 1 d . . . 
H22 H 0.2641 0.1276 0.6522 0.038 Uiso 1 1 calc R . . 
C29 C 0.2082(3) 0.10772(14) 0.7779(2) 0.0329(7) Uani 1 1 d . . . 
H23 H 0.2241 0.1503 0.8050 0.039 Uiso 1 1 calc R . . 
C30 C 0.1602(4) 0.05820(16) 0.8281(2) 0.0352(8) Uani 1 1 d . . . 
C31 C 0.1359(3) -0.00331(15) 0.7891(2) 0.0338(7) Uani 1 1 d . . . 
H24 H 0.1022 -0.0365 0.8242 0.041 Uiso 1 1 calc R . . 
C32 C 0.1604(3) -0.01688(14) 0.6990(2) 0.0283(7) Uani 1 1 d . . . 
H25 H 0.1424 -0.0594 0.6721 0.034 Uiso 1 1 calc R . . 
O7 O 0.1208(3) 0.06875(13) 0.91578(15) 0.0482(7) Uani 1 1 d . . . 
C33 C 0.2015(5) 0.09632(18) 0.9916(2) 0.0484(9) Uani 1 1 d . . . 
C34 C 0.1422(6) 0.0999(2) 1.0777(3) 0.0719(14) Uani 1 1 d . . . 
H26 H 0.1590 0.0590 1.1145 0.108 Uiso 1 1 calc R . . 
H27 H 0.0476 0.1066 1.0570 0.108 Uiso 1 1 calc R . . 
H28 H 0.1806 0.1367 1.1187 0.108 Uiso 1 1 calc R . . 
O8 O 0.3105(3) 0.11529(14) 0.98806(17) 0.0587(8) Uani 1 1 d . . . 
 
 
_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 
C1 C2 1.357(4) . ? 
C1 C11 1.493(4) . ? 
C1 C3 1.494(4) . ? 
C2 C19 1.491(4) . ? 
C2 C27 1.493(4) . ? 
C3 C4 1.397(4) . ? 
C3 C8 1.401(4) . ? 
C4 C5 1.384(4) . ? 
C5 C6 1.378(4) . ? 
C6 C7 1.375(4) . ? 
C6 O1 1.400(3) . ? 
C7 C8 1.387(4) . ? 
O1 C9 1.354(4) . ? 
C9 O2 1.178(5) . ? 
C9 C10 1.495(4) . ? 
C11 C16 1.389(4) . ? 
C11 C12 1.392(5) . ? 
C12 C13 1.388(4) . ? 
C13 C14 1.373(4) . ? 
C14 C15 1.378(5) . ? 
C14 O3 1.409(3) . ? 
C15 C16 1.381(4) . ? 
O3 C17 1.343(5) . ? 
C17 O4 1.188(5) . ? 
C17 C18 1.484(5) . ? 
C19 C20 1.393(4) . ? 
C19 C24 1.398(5) . ? 
C20 C21 1.381(4) . ? 
C21 C22 1.370(5) . ? 
C22 C23 1.373(5) . ? 
C22 O5 1.404(3) . ? 
C23 C24 1.389(4) . ? 
O5 C25 1.346(4) . ? 
C25 O6 1.192(4) . ? 
C25 C26 1.483(5) . ? 
C27 C28 1.394(4) . ? 
C27 C32 1.409(4) . ? 
C28 C29 1.385(4) . ? 
C29 C30 1.388(5) . ? 
C30 C31 1.372(4) . ? 
C30 O7 1.401(4) . ? 
C31 C32 1.379(4) . ? 
O7 C33 1.340(4) . ? 
C33 O8 1.215(5) . ? 
C33 C34 1.479(6) . ? 
 
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 C11 123.1(2) . . ? 
C2 C1 C3 121.4(2) . . ? 
C11 C1 C3 115.5(2) . . ? 
C1 C2 C19 123.3(2) . . ? 
C1 C2 C27 122.4(2) . . ? 
C19 C2 C27 114.3(2) . . ? 
C4 C3 C8 117.7(2) . . ? 
C4 C3 C1 121.7(2) . . ? 
C8 C3 C1 120.5(2) . . ? 
C5 C4 C3 121.3(3) . . ? 
C6 C5 C4 119.1(3) . . ? 
C7 C6 C5 121.5(3) . . ? 
C7 C6 O1 119.6(3) . . ? 
C5 C6 O1 118.7(3) . . ? 
C6 C7 C8 119.1(3) . . ? 
C7 C8 C3 121.1(3) . . ? 
C9 O1 C6 118.3(3) . . ? 
O2 C9 O1 123.2(3) . . ? 
O2 C9 C10 126.3(4) . . ? 
O1 C9 C10 110.5(3) . . ? 
C16 C11 C12 117.7(3) . . ? 
C16 C11 C1 122.6(3) . . ? 
C12 C11 C1 119.6(3) . . ? 
C13 C12 C11 121.2(3) . . ? 
C14 C13 C12 119.1(3) . . ? 
C13 C14 C15 121.5(3) . . ? 
C13 C14 O3 118.5(3) . . ? 
C15 C14 O3 120.0(3) . . ? 
C14 C15 C16 118.7(3) . . ? 
C15 C16 C11 121.9(3) . . ? 
C17 O3 C14 116.2(3) . . ? 
O4 C17 O3 121.3(3) . . ? 
O4 C17 C18 126.3(4) . . ? 
O3 C17 C18 112.4(4) . . ? 
C20 C19 C24 117.4(2) . . ? 
C20 C19 C2 122.4(3) . . ? 
C24 C19 C2 120.1(3) . . ? 
C21 C20 C19 121.5(3) . . ? 
C22 C21 C20 119.4(3) . . ? 
C21 C22 C23 121.4(3) . . ? 
C21 C22 O5 118.7(3) . . ? 
C23 C22 O5 119.8(3) . . ? 
C22 C23 C24 118.9(3) . . ? 
C23 C24 C19 121.3(3) . . ? 
C25 O5 C22 116.8(2) . . ? 
O6 C25 O5 122.9(3) . . ? 
O6 C25 C26 125.3(3) . . ? 
O5 C25 C26 111.8(3) . . ? 
C28 C27 C32 117.3(3) . . ? 
C28 C27 C2 121.8(3) . . ? 
C32 C27 C2 120.8(2) . . ? 
C29 C28 C27 122.1(3) . . ? 
C28 C29 C30 118.6(3) . . ? 
C31 C30 C29 121.1(3) . . ? 
C31 C30 O7 115.5(3) . . ? 
C29 C30 O7 123.1(3) . . ? 
C30 C31 C32 120.0(3) . . ? 
C31 C32 C27 121.0(3) . . ? 
C33 O7 C30 121.2(3) . . ? 
O8 C33 O7 122.7(3) . . ? 
O8 C33 C34 125.3(3) . . ? 
O7 C33 C34 112.1(4) . . ? 
 
_diffrn_measured_fraction_theta_max    0.921 
_diffrn_reflns_theta_full              27.48 
_diffrn_measured_fraction_theta_full   0.921 
_refine_diff_density_max    0.337 
_refine_diff_density_min   -0.339 
_refine_diff_density_rms    0.075 
