 
data_a 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C30 H28 O4' 
_chemical_formula_weight          452.52 
 
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+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
 
_cell_length_a                    9.6317(3) 
_cell_length_b                    15.5277(6) 
_cell_length_c                    16.0905(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  92.4928(12) 
_cell_angle_gamma                 90.00 
_cell_volume                      2404.19(14) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     153(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.50 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.250 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              960 
_exptl_absorpt_coefficient_mu     0.082 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.9602 
_exptl_absorpt_correction_T_max   0.9838 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       153(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             38180 
_diffrn_reflns_av_R_equivalents   0.0369 
_diffrn_reflns_av_sigmaI/netI     0.0213 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -20 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        -20 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          3.37 
_diffrn_reflns_theta_max          27.46 
_reflns_number_total              5479 
_reflns_number_gt                 4529 
_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)+(0.0404P)²+0.9535P] 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          5479 
_refine_ls_number_parameters      311 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0630 
_refine_ls_R_factor_gt            0.0510 
_refine_ls_wR_factor_ref          0.1130 
_refine_ls_wR_factor_gt           0.1073 
_refine_ls_goodness_of_fit_ref    1.055 
_refine_ls_restrained_S_all       1.055 
_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 0.98806(15) 0.28706(9) 0.59399(9) 0.0324(3) Uani 1 1 d . . . 
C2 C 0.90088(15) 0.22579(9) 0.56213(9) 0.0325(3) Uani 1 1 d . . . 
C3 C 1.10811(14) 0.32201(9) 0.54917(9) 0.0308(3) Uani 1 1 d . . . 
C4 C 1.20914(15) 0.26958(10) 0.51691(9) 0.0342(3) Uani 1 1 d . . . 
H1 H 1.2026 0.2090 0.5241 0.041 Uiso 1 1 calc R . . 
C5 C 1.31967(16) 0.30283(10) 0.47437(9) 0.0366(3) Uani 1 1 d . . . 
H2 H 1.3877 0.2655 0.4531 0.044 Uiso 1 1 calc R . . 
C6 C 1.32949(16) 0.39109(10) 0.46326(9) 0.0366(3) Uani 1 1 d . . . 
C7 C 1.23024(17) 0.44514(10) 0.49572(10) 0.0413(4) Uani 1 1 d . . . 
H3 H 1.2366 0.5057 0.4881 0.050 Uiso 1 1 calc R . . 
C8 C 1.12259(16) 0.41103(10) 0.53897(10) 0.0370(3) Uani 1 1 d . . . 
H4 H 1.0570 0.4487 0.5623 0.044 Uiso 1 1 calc R . . 
O1 O 1.43217(13) 0.43137(8) 0.42160(7) 0.0517(3) Uani 1 1 d . . . 
C9 C 1.5429(2) 0.37994(14) 0.39440(13) 0.0611(5) Uani 1 1 d . . . 
H5 H 1.5923 0.3539 0.4427 0.092 Uiso 1 1 calc R . . 
H6 H 1.6073 0.4159 0.3641 0.092 Uiso 1 1 calc R . . 
H7 H 1.5058 0.3344 0.3576 0.092 Uiso 1 1 calc R . . 
C10 C 0.97192(14) 0.32405(9) 0.67884(9) 0.0316(3) Uani 1 1 d . . . 
C11 C 1.08179(15) 0.31884(10) 0.73812(9) 0.0335(3) Uani 1 1 d . . . 
H8 H 1.1675 0.2944 0.7230 0.040 Uiso 1 1 calc R . . 
C12 C 1.06840(15) 0.34852(10) 0.81829(9) 0.0350(3) Uani 1 1 d . . . 
H9 H 1.1440 0.3436 0.8580 0.042 Uiso 1 1 calc R . . 
C13 C 0.94416(15) 0.38556(9) 0.84083(9) 0.0331(3) Uani 1 1 d . . . 
C14 C 0.83455(15) 0.39365(10) 0.78235(10) 0.0362(3) Uani 1 1 d . . . 
H10 H 0.7498 0.4197 0.7970 0.043 Uiso 1 1 calc R . . 
C15 C 0.85049(15) 0.36317(10) 0.70208(10) 0.0368(3) Uani 1 1 d . . . 
H11 H 0.7758 0.3694 0.6620 0.044 Uiso 1 1 calc R . . 
O2 O 0.94127(12) 0.41269(8) 0.92172(7) 0.0460(3) Uani 1 1 d . . . 
C16 C 0.81818(18) 0.45441(11) 0.94662(10) 0.0453(4) Uani 1 1 d . . . 
H12 H 0.7985 0.5041 0.9105 0.068 Uiso 1 1 calc R . . 
H13 H 0.8312 0.4739 1.0044 0.068 Uiso 1 1 calc R . . 
H14 H 0.7401 0.4139 0.9422 0.068 Uiso 1 1 calc R . . 
C17 C 0.91178(14) 0.18971(9) 0.47652(8) 0.0302(3) Uani 1 1 d . . . 
C18 C 0.91043(15) 0.10029(9) 0.46566(9) 0.0318(3) Uani 1 1 d . . . 
H15 H 0.8988 0.0643 0.5126 0.038 Uiso 1 1 calc R . . 
C19 C 0.92554(15) 0.06292(10) 0.38882(9) 0.0338(3) Uani 1 1 d . . . 
H16 H 0.9257 0.0020 0.3835 0.041 Uiso 1 1 calc R . . 
C20 C 0.94063(14) 0.11460(10) 0.31901(8) 0.0314(3) Uani 1 1 d . . . 
C21 C 0.93950(15) 0.20324(10) 0.32754(9) 0.0328(3) Uani 1 1 d . . . 
H17 H 0.9484 0.2390 0.2801 0.039 Uiso 1 1 calc R . . 
C22 C 0.92530(15) 0.24010(10) 0.40565(9) 0.0336(3) Uani 1 1 d . . . 
H18 H 0.9248 0.3011 0.4107 0.040 Uiso 1 1 calc R . . 
O3 O 0.95628(12) 0.07122(7) 0.24584(6) 0.0417(3) Uani 1 1 d . . . 
C23 C 0.96688(17) 0.12141(12) 0.17221(9) 0.0436(4) Uani 1 1 d . . . 
H19 H 0.8789 0.1516 0.1602 0.065 Uiso 1 1 calc R . . 
H20 H 0.9870 0.0836 0.1255 0.065 Uiso 1 1 calc R . . 
H21 H 1.0420 0.1636 0.1803 0.065 Uiso 1 1 calc R . . 
C24 C 0.78872(15) 0.18720(9) 0.61180(9) 0.0316(3) Uani 1 1 d . . . 
C25 C 0.65236(16) 0.18429(10) 0.58007(10) 0.0363(3) Uani 1 1 d . . . 
H22 H 0.6314 0.2056 0.5256 0.044 Uiso 1 1 calc R . . 
C26 C 0.54552(17) 0.15088(10) 0.62614(11) 0.0425(4) Uani 1 1 d . . . 
H23 H 0.4527 0.1505 0.6035 0.051 Uiso 1 1 calc R . . 
C27 C 0.57538(18) 0.11839(10) 0.70490(10) 0.0418(4) Uani 1 1 d . . . 
C28 C 0.71138(19) 0.11863(11) 0.73692(10) 0.0451(4) Uani 1 1 d . . . 
H24 H 0.7325 0.0956 0.7907 0.054 Uiso 1 1 calc R . . 
C29 C 0.81611(17) 0.15215(11) 0.69095(9) 0.0403(4) Uani 1 1 d . . . 
H25 H 0.9089 0.1515 0.7135 0.048 Uiso 1 1 calc R . . 
O4 O 0.47887(14) 0.08435(9) 0.75641(8) 0.0600(4) Uani 1 1 d . . . 
C30 C 0.3435(2) 0.06981(14) 0.72263(16) 0.0708(6) Uani 1 1 d . . . 
H26 H 0.2984 0.1252 0.7102 0.106 Uiso 1 1 calc R . . 
H27 H 0.2897 0.0380 0.7628 0.106 Uiso 1 1 calc R . . 
H28 H 0.3484 0.0362 0.6713 0.106 Uiso 1 1 calc R . . 
 
 
_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 1.355(2) . ? 
C1 C3 1.491(2) . ? 
C1 C10 1.496(2) . ? 
C2 C17 1.4950(19) . ? 
C2 C24 1.497(2) . ? 
C3 C4 1.387(2) . ? 
C3 C8 1.400(2) . ? 
C4 C5 1.390(2) . ? 
C5 C6 1.386(2) . ? 
C6 O1 1.3699(18) . ? 
C6 C7 1.391(2) . ? 
C7 C8 1.379(2) . ? 
O1 C9 1.417(2) . ? 
C10 C15 1.384(2) . ? 
C10 C11 1.396(2) . ? 
C11 C12 1.381(2) . ? 
C12 C13 1.390(2) . ? 
C13 O2 1.3695(17) . ? 
C13 C14 1.389(2) . ? 
C14 C15 1.390(2) . ? 
O2 C16 1.4238(19) . ? 
C17 C22 1.394(2) . ? 
C17 C18 1.399(2) . ? 
C18 C19 1.379(2) . ? 
C19 C20 1.393(2) . ? 
C20 O3 1.3705(17) . ? 
C20 C21 1.383(2) . ? 
C21 C22 1.393(2) . ? 
O3 C23 1.4255(18) . ? 
C24 C25 1.389(2) . ? 
C24 C29 1.400(2) . ? 
C25 C26 1.394(2) . ? 
C26 C27 1.383(2) . ? 
C27 O4 1.3775(19) . ? 
C27 C28 1.387(2) . ? 
C28 C29 1.379(2) . ? 
O4 C30 1.408(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 C1 C3 123.60(13) . . ? 
C2 C1 C10 121.86(13) . . ? 
C3 C1 C10 114.54(12) . . ? 
C1 C2 C17 123.00(13) . . ? 
C1 C2 C24 121.94(13) . . ? 
C17 C2 C24 115.04(12) . . ? 
C4 C3 C8 117.43(13) . . ? 
C4 C3 C1 122.61(13) . . ? 
C8 C3 C1 119.96(13) . . ? 
C3 C4 C5 122.09(14) . . ? 
C6 C5 C4 119.27(14) . . ? 
O1 C6 C5 124.71(15) . . ? 
O1 C6 C7 115.52(14) . . ? 
C5 C6 C7 119.77(14) . . ? 
C8 C7 C6 120.11(15) . . ? 
C7 C8 C3 121.29(14) . . ? 
C6 O1 C9 117.58(14) . . ? 
C15 C10 C11 117.74(13) . . ? 
C15 C10 C1 122.54(13) . . ? 
C11 C10 C1 119.72(13) . . ? 
C12 C11 C10 121.33(13) . . ? 
C11 C12 C13 119.89(14) . . ? 
O2 C13 C14 124.73(13) . . ? 
O2 C13 C12 115.38(13) . . ? 
C14 C13 C12 119.88(13) . . ? 
C13 C14 C15 119.15(13) . . ? 
C10 C15 C14 121.95(14) . . ? 
C13 O2 C16 117.32(12) . . ? 
C22 C17 C18 117.10(13) . . ? 
C22 C17 C2 123.80(13) . . ? 
C18 C17 C2 119.09(12) . . ? 
C19 C18 C17 121.91(13) . . ? 
C18 C19 C20 119.95(14) . . ? 
O3 C20 C21 125.16(13) . . ? 
O3 C20 C19 115.39(13) . . ? 
C21 C20 C19 119.45(13) . . ? 
C20 C21 C22 119.98(13) . . ? 
C21 C22 C17 121.59(14) . . ? 
C20 O3 C23 117.38(12) . . ? 
C25 C24 C29 117.36(14) . . ? 
C25 C24 C2 120.65(13) . . ? 
C29 C24 C2 121.99(13) . . ? 
C24 C25 C26 121.65(15) . . ? 
C27 C26 C25 119.61(15) . . ? 
O4 C27 C26 124.93(16) . . ? 
O4 C27 C28 115.39(16) . . ? 
C26 C27 C28 119.68(15) . . ? 
C29 C28 C27 120.21(16) . . ? 
C28 C29 C24 121.45(15) . . ? 
C27 O4 C30 117.82(16) . . ? 
 
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              27.46 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    0.259 
_refine_diff_density_min   -0.200 
_refine_diff_density_rms    0.035 
