 
data_s 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C43 H48 O8' 
_chemical_formula_weight          692.81 
 
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 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    10.7525(3) 
_cell_length_b                    13.2311(4) 
_cell_length_c                    15.5424(4) 
_cell_angle_alpha                 105.2250(10) 
_cell_angle_beta                  105.9030(10) 
_cell_angle_gamma                 108.3520(10) 
_cell_volume                      1865.15(9) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     273(2) 
_cell_measurement_reflns_used     9899   
_cell_measurement_theta_min       2.94 
_cell_measurement_theta_max       26.13 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.234 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              740 
_exptl_absorpt_coefficient_mu     0.084 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       273(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'CCD area detector'   
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             11849 
_diffrn_reflns_av_R_equivalents   0.0158 
_diffrn_reflns_av_sigmaI/netI     0.0455 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          2.90 
_diffrn_reflns_theta_max          26.13 
_reflns_number_total              7373 
_reflns_number_gt                 6307 
_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)+(0.0542P)²+0.7220P] 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          7373 
_refine_ls_number_parameters      468 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0503 
_refine_ls_R_factor_gt            0.0426 
_refine_ls_wR_factor_ref          0.1186 
_refine_ls_wR_factor_gt           0.1118 
_refine_ls_goodness_of_fit_ref    1.013 
_refine_ls_restrained_S_all       1.013 
_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 0.45478(13) 0.71364(11) 0.32583(9) 0.0192(3) Uani 1 1 d . . . 
H1A H 0.3953 0.6432 0.3286 0.023 Uiso 1 1 calc R . . 
H1B H 0.4220 0.7721 0.3482 0.023 Uiso 1 1 calc R . . 
C2 C 0.94960(13) 0.65521(11) 0.33257(9) 0.0183(3) Uani 1 1 d . . . 
C3 C 0.67522(14) 0.67840(11) 0.38246(9) 0.0187(3) Uani 1 1 d . . . 
C4 C 0.49988(13) 0.78430(11) 0.19662(9) 0.0187(3) Uani 1 1 d . . . 
C5 C 0.50130(13) 0.77245(11) 0.10535(9) 0.0196(3) Uani 1 1 d . . . 
C6 C 0.81822(14) 0.70922(11) 0.43519(9) 0.0185(3) Uani 1 1 d . . . 
C7 C 0.68858(14) 0.86221(11) 0.46675(9) 0.0190(3) Uani 1 1 d . . . 
C8 C 0.43698(13) 0.69278(11) 0.22142(9) 0.0186(3) Uani 1 1 d . . . 
C9 C 0.83020(14) 0.89522(11) 0.52504(9) 0.0210(3) Uani 1 1 d . . . 
H9 H 0.8818 0.9675 0.5750 0.025 Uiso 1 1 calc R . . 
C10 C 0.79043(14) 0.81265(11) 0.14669(9) 0.0199(3) Uani 1 1 d . . . 
H10 H 0.7262 0.7540 0.1552 0.024 Uiso 1 1 calc R . . 
C11 C 0.36498(13) 0.58346(11) 0.14683(9) 0.0190(3) Uani 1 1 d . . . 
C12 C 0.74206(14) 0.88353(11) 0.10949(9) 0.0199(3) Uani 1 1 d . . . 
C13 C 0.42803(13) 0.66152(11) 0.03384(9) 0.0202(3) Uani 1 1 d . . . 
C14 C 1.02745(13) 0.59629(11) 0.30186(9) 0.0197(3) Uani 1 1 d . . . 
C15 C 0.92405(13) 0.72952(11) 0.28929(9) 0.0187(3) Uani 1 1 d . . . 
H15 H 0.8718 0.7685 0.3085 0.022 Uiso 1 1 calc R . . 
C16 C 0.60767(13) 0.75210(11) 0.39349(9) 0.0181(3) Uani 1 1 d . . . 
C17 C 0.98042(15) 0.98407(13) 0.11951(11) 0.0266(3) Uani 1 1 d . . . 
H17 H 1.0443 1.0416 0.1097 0.032 Uiso 1 1 calc R . . 
C18 C 0.89200(14) 0.63339(11) 0.40821(9) 0.0202(3) Uani 1 1 d . . . 
H18A H 0.8254 0.5533 0.3833 0.024 Uiso 1 1 calc R . . 
H18B H 0.9699 0.6474 0.4658 0.024 Uiso 1 1 calc R . . 
C19 C 0.93128(14) 0.82473(11) 0.17216(9) 0.0206(3) Uani 1 1 d . . . 
C20 C 0.97314(13) 0.74880(11) 0.21792(9) 0.0198(3) Uani 1 1 d . . . 
C21 C 0.59016(14) 0.87190(12) 0.08711(10) 0.0221(3) Uani 1 1 d . . . 
H21A H 0.5918 0.9427 0.1269 0.026 Uiso 1 1 calc R . . 
H21B H 0.5466 0.8607 0.0198 0.026 Uiso 1 1 calc R . . 
C22 C 0.35829(13) 0.56750(11) 0.05326(9) 0.0207(3) Uani 1 1 d . . . 
H22 H 0.3076 0.4946 0.0041 0.025 Uiso 1 1 calc R . . 
C23 C 0.34209(18) 0.54363(13) -0.13350(10) 0.0333(3) Uani 1 1 d . . . 
H23A H 0.3765 0.4872 -0.1234 0.050 Uiso 1 1 calc R . . 
H23B H 0.3436 0.5506 -0.1932 0.050 Uiso 1 1 calc R . . 
H23C H 0.2464 0.5200 -0.1365 0.050 Uiso 1 1 calc R . . 
C24 C 0.89373(13) 0.81926(11) 0.50791(9) 0.0194(3) Uani 1 1 d . . . 
C25 C 1.08018(14) 0.61547(12) 0.23265(10) 0.0223(3) Uani 1 1 d . . . 
H25 H 1.1334 0.5773 0.2139 0.027 Uiso 1 1 calc R . . 
C26 C 1.02538(15) 0.91098(12) 0.15699(10) 0.0251(3) Uani 1 1 d . . . 
H26 H 1.1191 0.9201 0.1719 0.030 Uiso 1 1 calc R . . 
C27 C 1.05328(14) 0.69198(12) 0.19133(10) 0.0226(3) Uani 1 1 d . . . 
H27 H 1.0895 0.7050 0.1454 0.027 Uiso 1 1 calc R . . 
C28 C 1.10900(17) 0.44867(13) 0.30722(11) 0.0281(3) Uani 1 1 d . . . 
H28A H 1.2041 0.4959 0.3149 0.034 Uiso 1 1 calc R . . 
H28B H 1.0530 0.4027 0.2388 0.034 Uiso 1 1 calc R . . 
C29 C 0.84047(14) 0.97145(12) 0.09675(10) 0.0230(3) Uani 1 1 d . . . 
C30 C 0.24900(18) 0.37987(12) 0.10220(11) 0.0341(4) Uani 1 1 d . . . 
H30A H 0.1704 0.3661 0.0462 0.051 Uiso 1 1 calc R . . 
H30B H 0.2184 0.3257 0.1309 0.051 Uiso 1 1 calc R . . 
H30C H 0.3240 0.3708 0.0834 0.051 Uiso 1 1 calc R . . 
C31 C 0.48095(19) 0.95136(13) 0.27540(12) 0.0354(4) Uani 1 1 d . . . 
H31A H 0.4482 0.9633 0.2165 0.053 Uiso 1 1 calc R . . 
H31B H 0.5329 1.0244 0.3289 0.053 Uiso 1 1 calc R . . 
H31C H 0.4008 0.9055 0.2850 0.053 Uiso 1 1 calc R . . 
C32 C 1.10639(15) 0.94714(13) 0.64670(11) 0.0320(3) Uani 1 1 d . . . 
H32A H 1.1225 1.0145 0.6311 0.048 Uiso 1 1 calc R . . 
H32B H 1.1960 0.9491 0.6825 0.048 Uiso 1 1 calc R . . 
H32C H 1.0500 0.9456 0.6851 0.048 Uiso 1 1 calc R . . 
C33 C 0.70387(16) 1.05071(12) 0.54129(11) 0.0309(3) Uani 1 1 d . . . 
H33A H 0.7464 1.0562 0.6063 0.046 Uiso 1 1 calc R . . 
H33B H 0.6444 1.0917 0.5395 0.046 Uiso 1 1 calc R . . 
H33C H 0.7772 1.0837 0.5201 0.046 Uiso 1 1 calc R . . 
C34 C 0.52821(17) 0.48986(13) 0.35028(13) 0.0359(4) Uani 1 1 d . . . 
H34A H 0.5994 0.4861 0.4009 0.054 Uiso 1 1 calc R . . 
H34B H 0.4727 0.4147 0.2997 0.054 Uiso 1 1 calc R . . 
H34C H 0.4673 0.5160 0.3760 0.054 Uiso 1 1 calc R . . 
C35 C 0.88942(16) 1.14699(13) 0.06915(12) 0.0290(3) Uani 1 1 d . . . 
H35A H 0.9406 1.1313 0.0284 0.035 Uiso 1 1 calc R . . 
H35B H 0.9577 1.1913 0.1354 0.035 Uiso 1 1 calc R . . 
C36 C 1.1155(2) 0.37176(16) 0.36236(14) 0.0430(4) Uani 1 1 d . . . 
H36A H 1.1688 0.4180 0.4301 0.064 Uiso 1 1 calc R . . 
H36B H 1.1612 0.3247 0.3400 0.064 Uiso 1 1 calc R . . 
H36C H 1.0208 0.3233 0.3523 0.064 Uiso 1 1 calc R . . 
C37 C 0.80848(19) 1.21280(16) 0.03645(15) 0.0452(4) Uani 1 1 d . . . 
H37A H 0.7420 1.1685 -0.0294 0.068 Uiso 1 1 calc R . . 
H37B H 0.8736 1.2847 0.0407 0.068 Uiso 1 1 calc R . . 
H37C H 0.7579 1.2274 0.0771 0.068 Uiso 1 1 calc R . . 
C38 C 0.5328(5) 0.2445(2) 0.4040(2) 0.0895(11) Uani 1 1 d . . . 
H38 H 0.5293 0.2545 0.4647 0.107 Uiso 1 1 calc R . . 
C39 C 0.6599(4) 0.2796(2) 0.3968(2) 0.0810(9) Uani 1 1 d . . . 
H39 H 0.7437 0.3133 0.4517 0.097 Uiso 1 1 calc R . . 
C40 C 0.4136(4) 0.1963(2) 0.3270(4) 0.0902(12) Uani 1 1 d . . . 
H40 H 0.3268 0.1726 0.3336 0.108 Uiso 1 1 calc R . . 
C41 C 0.6639(3) 0.2649(2) 0.3064(3) 0.0763(8) Uani 1 1 d . . . 
H41 H 0.7508 0.2889 0.2999 0.092 Uiso 1 1 calc R . . 
C42 C 0.5404(4) 0.2152(2) 0.22721(19) 0.0727(8) Uani 1 1 d . . . 
H42 H 0.5419 0.2052 0.1661 0.087 Uiso 1 1 calc R . . 
C43 C 0.4165(3) 0.1808(2) 0.2376(3) 0.0835(10) Uani 1 1 d . . . 
H43 H 0.3316 0.1460 0.1834 0.100 Uiso 1 1 calc R . . 
O1 O 1.04517(11) 0.52006(9) 0.34419(7) 0.0254(2) Uani 1 1 d . . . 
O2 O 0.78871(10) 1.04151(9) 0.06237(8) 0.0298(2) Uani 1 1 d . . . 
O3 O 0.57123(10) 0.89327(8) 0.26919(7) 0.0243(2) Uani 1 1 d . . . 
O4 O 0.43084(11) 0.65222(8) -0.05533(7) 0.0269(2) Uani 1 1 d . . . 
O5 O 0.29972(10) 0.49383(8) 0.17047(7) 0.0231(2) Uani 1 1 d . . . 
O6 O 0.62019(10) 0.93271(8) 0.47891(7) 0.0240(2) Uani 1 1 d . . . 
O7 O 0.59522(10) 0.56801(8) 0.31214(7) 0.0243(2) Uani 1 1 d . . . 
O8 O 1.03306(10) 0.84655(8) 0.55962(7) 0.0255(2) 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 C8 1.5190(17) . ? 
C1 C16 1.5205(17) . ? 
C2 C15 1.3824(18) . ? 
C2 C14 1.4038(18) . ? 
C2 C18 1.5211(17) . ? 
C3 O7 1.3867(15) . ? 
C3 C16 1.3908(18) . ? 
C3 C6 1.3933(18) . ? 
C4 O3 1.3837(15) . ? 
C4 C5 1.3906(18) . ? 
C4 C8 1.3944(18) . ? 
C5 C13 1.3947(18) . ? 
C5 C21 1.5091(18) . ? 
C6 C24 1.3947(18) . ? 
C6 C18 1.5080(17) . ? 
C7 O6 1.3646(16) . ? 
C7 C9 1.3956(18) . ? 
C7 C16 1.4012(18) . ? 
C8 C11 1.3993(18) . ? 
C9 C24 1.3924(19) . ? 
C10 C12 1.3826(18) . ? 
C10 C19 1.4006(18) . ? 
C11 O5 1.3711(15) . ? 
C11 C22 1.3916(18) . ? 
C12 C29 1.4046(19) . ? 
C12 C21 1.5213(18) . ? 
C13 O4 1.3684(16) . ? 
C13 C22 1.3910(19) . ? 
C14 O1 1.3739(15) . ? 
C14 C25 1.3892(18) . ? 
C15 C20 1.3996(18) . ? 
C17 C26 1.3945(19) . ? 
C17 C29 1.391(2) . ? 
C19 C26 1.3880(19) . ? 
C19 C20 1.4840(18) . ? 
C20 C27 1.3850(19) . ? 
C23 O4 1.4267(17) . ? 
C24 O8 1.3667(16) . ? 
C25 C27 1.3947(19) . ? 
C28 O1 1.4257(16) . ? 
C28 C36 1.498(2) . ? 
C29 O2 1.3701(16) . ? 
C30 O5 1.4218(17) . ? 
C31 O3 1.4229(18) . ? 
C32 O8 1.4259(17) . ? 
C33 O6 1.4245(16) . ? 
C34 O7 1.4236(19) . ? 
C35 O2 1.4282(17) . ? 
C35 C37 1.497(2) . ? 
C38 C40 1.314(5) . ? 
C38 C39 1.344(5) . ? 
C39 C41 1.381(4) . ? 
C40 C43 1.360(5) . ? 
C41 C42 1.357(4) . ? 
C42 C43 1.335(4) . ? 
 
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 
C8 C1 C16 113.17(10) . . ? 
C15 C2 C14 117.56(11) . . ? 
C15 C2 C18 122.12(11) . . ? 
C14 C2 C18 120.29(11) . . ? 
O7 C3 C16 117.42(11) . . ? 
O7 C3 C6 118.14(11) . . ? 
C16 C3 C6 124.40(12) . . ? 
O3 C4 C5 118.10(11) . . ? 
O3 C4 C8 117.46(11) . . ? 
C5 C4 C8 124.37(12) . . ? 
C4 C5 C13 116.61(12) . . ? 
C4 C5 C21 121.69(11) . . ? 
C13 C5 C21 121.40(12) . . ? 
C3 C6 C24 116.47(11) . . ? 
C3 C6 C18 121.90(11) . . ? 
C24 C6 C18 121.29(12) . . ? 
O6 C7 C9 122.64(11) . . ? 
O6 C7 C16 116.37(11) . . ? 
C9 C7 C16 120.97(12) . . ? 
C4 C8 C11 116.47(11) . . ? 
C4 C8 C1 120.10(11) . . ? 
C11 C8 C1 123.35(11) . . ? 
C24 C9 C7 119.57(12) . . ? 
C12 C10 C19 123.35(12) . . ? 
O5 C11 C22 122.03(11) . . ? 
O5 C11 C8 116.56(11) . . ? 
C22 C11 C8 121.41(12) . . ? 
C10 C12 C29 117.54(12) . . ? 
C10 C12 C21 122.09(12) . . ? 
C29 C12 C21 120.31(12) . . ? 
O4 C13 C22 122.96(12) . . ? 
O4 C13 C5 115.46(11) . . ? 
C22 C13 C5 121.58(12) . . ? 
O1 C14 C25 123.94(12) . . ? 
O1 C14 C2 115.38(11) . . ? 
C25 C14 C2 120.68(12) . . ? 
C2 C15 C20 123.08(12) . . ? 
C3 C16 C7 116.79(11) . . ? 
C3 C16 C1 120.27(11) . . ? 
C7 C16 C1 122.91(11) . . ? 
C26 C17 C29 120.40(12) . . ? 
C6 C18 C2 112.21(10) . . ? 
C26 C19 C10 117.77(12) . . ? 
C26 C19 C20 123.73(12) . . ? 
C10 C19 C20 118.43(11) . . ? 
C27 C20 C15 117.92(12) . . ? 
C27 C20 C19 123.78(11) . . ? 
C15 C20 C19 118.25(11) . . ? 
C5 C21 C12 112.23(11) . . ? 
C13 C22 C11 119.45(12) . . ? 
O8 C24 C9 123.10(12) . . ? 
O8 C24 C6 115.28(11) . . ? 
C9 C24 C6 121.62(12) . . ? 
C14 C25 C27 120.02(12) . . ? 
C19 C26 C17 120.49(13) . . ? 
C20 C27 C25 120.69(12) . . ? 
O1 C28 C36 108.19(12) . . ? 
O2 C29 C17 124.14(12) . . ? 
O2 C29 C12 115.43(12) . . ? 
C17 C29 C12 120.42(12) . . ? 
O2 C35 C37 107.49(12) . . ? 
C40 C38 C39 121.2(3) . . ? 
C38 C39 C41 118.9(3) . . ? 
C38 C40 C43 120.3(3) . . ? 
C42 C41 C39 119.6(2) . . ? 
C43 C42 C41 119.6(3) . . ? 
C42 C43 C40 120.4(3) . . ? 
C14 O1 C28 117.27(10) . . ? 
C29 O2 C35 117.65(11) . . ? 
C4 O3 C31 112.17(10) . . ? 
C13 O4 C23 117.25(11) . . ? 
C11 O5 C30 117.83(10) . . ? 
C7 O6 C33 117.88(10) . . ? 
C3 O7 C34 111.55(10) . . ? 
C24 O8 C32 117.29(11) . . ? 
 
_diffrn_measured_fraction_theta_max    0.991 
_diffrn_reflns_theta_full              26.13 
_diffrn_measured_fraction_theta_full   0.991 
_refine_diff_density_max    0.414 
_refine_diff_density_min   -0.341 
_refine_diff_density_rms    0.041 
