 
data_a 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C73 H92 Cl O12' 
_chemical_formula_weight          1196.92 
 
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' 
 'O'  'O'   0.0106   0.0060 
 '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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
 
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                    11.607(3) 
_cell_length_b                    12.917(3) 
_cell_length_c                    22.363(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.310(8) 
_cell_angle_gamma                 90.00 
_cell_volume                      3351.9(13) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     6290 
_cell_measurement_theta_min       2.08 
_cell_measurement_theta_max       27.51 
 
_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     1.186 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1286 
_exptl_absorpt_coefficient_mu     0.117 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       296(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             20867 
_diffrn_reflns_av_R_equivalents   0.0667 
_diffrn_reflns_av_sigmaI/netI     0.0709 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          2.00 
_diffrn_reflns_theta_max          25.47 
_reflns_number_total              6147 
_reflns_number_gt                 3177 
_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)+(0.1174P)²+0.5282P] 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          6147 
_refine_ls_number_parameters      394 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1492 
_refine_ls_R_factor_gt            0.0723 
_refine_ls_wR_factor_ref          0.2287 
_refine_ls_wR_factor_gt           0.1851 
_refine_ls_goodness_of_fit_ref    1.017 
_refine_ls_restrained_S_all       1.017 
_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 
O1 O 0.43531(19) 0.26331(17) 0.62432(10) 0.0607(6) Uani 1 1 d . . . 
O2 O 0.2353(2) 0.56941(15) 0.30794(11) 0.0630(7) Uani 1 1 d . . . 
O3 O 0.8593(2) 0.10539(19) 0.56698(10) 0.0697(7) Uani 1 1 d . . . 
O4 O 0.6695(2) 0.44334(17) 0.24771(12) 0.0790(8) Uani 1 1 d . . . 
O5 O 0.8134(2) 0.2204(2) 0.42111(14) 0.0930(9) Uani 1 1 d . . . 
O6 O 0.3758(3) 0.1574(2) 0.33006(13) 0.1038(11) Uani 1 1 d . . . 
C2 C 0.6657(3) 0.1386(2) 0.53903(13) 0.0453(8) Uani 1 1 d . . . 
C3 C 0.6285(3) 0.2324(2) 0.65109(13) 0.0449(8) Uani 1 1 d . . . 
C4 C 0.4246(3) 0.6116(2) 0.28377(13) 0.0457(8) Uani 1 1 d . . . 
C5 C 0.4812(3) 0.4019(2) 0.27252(13) 0.0494(8) Uani 1 1 d . . . 
C6 C 0.3428(3) 0.5352(2) 0.29356(14) 0.0488(8) Uani 1 1 d . . . 
C7 C 0.5397(3) 0.2250(2) 0.60794(14) 0.0456(8) Uani 1 1 d . . . 
C8 C 0.3923(3) 0.7247(2) 0.28744(13) 0.0498(8) Uani 1 1 d . . . 
H8A H 0.3230 0.7353 0.2631 0.060 Uiso 1 1 calc R . . 
H8B H 0.4532 0.7648 0.2697 0.060 Uiso 1 1 calc R . . 
C9 C 0.7553(3) 0.1469(2) 0.58166(14) 0.0485(8) Uani 1 1 d . . . 
C10 C 0.5601(3) 0.1792(2) 0.55332(14) 0.0499(8) Uani 1 1 d . . . 
H10 H 0.5002 0.1756 0.5251 0.060 Uiso 1 1 calc R . . 
C11 C 0.6367(3) 0.1364(2) 0.42626(13) 0.0495(8) Uani 1 1 d . . . 
C12 C 0.5545(3) 0.2374(2) 0.32251(13) 0.0508(8) Uani 1 1 d . . . 
C13 C 0.3722(3) 0.4309(2) 0.28720(14) 0.0530(9) Uani 1 1 d . . . 
H13 H 0.3166 0.3803 0.2931 0.064 Uiso 1 1 calc R . . 
C14 C 0.7349(3) 0.1938(2) 0.63650(14) 0.0514(9) Uani 1 1 d . . . 
H14 H 0.7954 0.1993 0.6643 0.062 Uiso 1 1 calc R . . 
C15 C 0.5270(3) 0.1203(2) 0.40410(14) 0.0562(9) Uani 1 1 d . . . 
H15 H 0.4798 0.0735 0.4235 0.067 Uiso 1 1 calc R . . 
C16 C 0.6818(3) 0.0812(2) 0.48130(13) 0.0528(9) Uani 1 1 d . . . 
H16A H 0.7634 0.0680 0.4767 0.063 Uiso 1 1 calc R . . 
H16B H 0.6435 0.0146 0.4839 0.063 Uiso 1 1 calc R . . 
C17 C 0.7059(3) 0.2058(2) 0.39624(15) 0.0553(9) Uani 1 1 d . . . 
C18 C 0.5624(3) 0.4782(2) 0.26284(14) 0.0543(9) Uani 1 1 d . . . 
C19 C 0.5330(3) 0.5814(2) 0.26832(14) 0.0534(9) Uani 1 1 d . . . 
H19 H 0.5884 0.6318 0.2613 0.064 Uiso 1 1 calc R . . 
C20 C 0.6650(3) 0.2536(2) 0.34441(15) 0.0580(9) Uani 1 1 d . . . 
H20 H 0.7134 0.2979 0.3239 0.070 Uiso 1 1 calc R . . 
C21 C 0.5112(3) 0.2881(2) 0.26523(14) 0.0594(10) Uani 1 1 d . . . 
H21A H 0.4432 0.2513 0.2507 0.071 Uiso 1 1 calc R . . 
H21B H 0.5698 0.2816 0.2352 0.071 Uiso 1 1 calc R . . 
C22 C 0.4842(3) 0.1710(2) 0.35388(15) 0.0594(10) Uani 1 1 d . . . 
C23 C 0.7539(3) 0.5136(3) 0.22862(18) 0.0727(11) Uani 1 1 d . . . 
H23A H 0.7754 0.5606 0.2608 0.087 Uiso 1 1 calc R . . 
H23B H 0.7246 0.5539 0.1950 0.087 Uiso 1 1 calc R . . 
C24 C 0.3463(3) 0.2711(3) 0.58007(18) 0.0804(12) Uani 1 1 d . . . 
H24A H 0.3230 0.2027 0.5665 0.097 Uiso 1 1 calc R . . 
H24B H 0.3728 0.3100 0.5459 0.097 Uiso 1 1 calc R . . 
C25 C 0.9542(3) 0.1155(3) 0.60675(19) 0.0822(12) Uani 1 1 d . . . 
H25A H 0.9375 0.0827 0.6446 0.099 Uiso 1 1 calc R . . 
H25B H 0.9702 0.1881 0.6142 0.099 Uiso 1 1 calc R . . 
C26 C 0.1469(3) 0.4963(3) 0.3161(2) 0.0814(12) Uani 1 1 d . . . 
H26A H 0.1711 0.4451 0.3455 0.098 Uiso 1 1 calc R . . 
H26B H 0.1292 0.4610 0.2787 0.098 Uiso 1 1 calc R . . 
C27 C 0.2486(5) 0.5596(4) 0.47169(19) 0.237(2) Uani 0.50 1 d P . . 
Cl1 Cl 0.2486(5) 0.5596(4) 0.47169(19) 0.237(2) Uani 0.50 1 d P . . 
H27A H 0.2010 0.4992 0.4750 0.356 Uiso 1 1 calc R . . 
H27B H 0.2416 0.5869 0.4318 0.356 Uiso 1 1 calc R . . 
H27C H 0.2243 0.6110 0.4997 0.356 Uiso 1 1 calc R . . 
C28 C 0.0434(4) 0.5527(3) 0.3370(3) 0.1062(17) Uani 1 1 d . . . 
H28A H 0.0628 0.5903 0.3729 0.159 Uiso 1 1 calc R . . 
H28B H -0.0168 0.5040 0.3450 0.159 Uiso 1 1 calc R . . 
H28C H 0.0174 0.6003 0.3066 0.159 Uiso 1 1 calc R . . 
C29 C 0.8551(4) 0.4510(3) 0.2108(2) 0.1007(15) Uani 1 1 d . . . 
H29A H 0.8837 0.4122 0.2446 0.151 Uiso 1 1 calc R . . 
H29B H 0.9145 0.4962 0.1969 0.151 Uiso 1 1 calc R . . 
H29C H 0.8323 0.4042 0.1793 0.151 Uiso 1 1 calc R . . 
C30 C 1.0553(4) 0.0654(4) 0.5796(2) 0.1042(16) Uani 1 1 d . . . 
H30A H 1.0416 -0.0076 0.5758 0.156 Uiso 1 1 calc R . . 
H30B H 1.1224 0.0768 0.6047 0.156 Uiso 1 1 calc R . . 
H30C H 1.0675 0.0946 0.5408 0.156 Uiso 1 1 calc R . . 
C31 C 0.2470(4) 0.3254(4) 0.6081(2) 0.1136(18) Uani 1 1 d . . . 
H31A H 0.2190 0.2844 0.6404 0.170 Uiso 1 1 calc R . . 
H31B H 0.1865 0.3352 0.5787 0.170 Uiso 1 1 calc R . . 
H31C H 0.2721 0.3915 0.6231 0.170 Uiso 1 1 calc R . . 
C32 C 0.2951(5) 0.1016(5) 0.3636(3) 0.139(3) Uani 1 1 d . . . 
H32A H 0.2365 0.0742 0.3363 0.167 Uiso 1 1 calc R . . 
H32B H 0.3342 0.0432 0.3822 0.167 Uiso 1 1 calc R . . 
C33 C 0.8847(4) 0.2991(4) 0.3993(3) 0.1195(19) Uani 1 1 d . . . 
H33A H 0.8421 0.3634 0.3951 0.143 Uiso 1 1 calc R . . 
H33B H 0.9141 0.2802 0.3605 0.143 Uiso 1 1 calc R . . 
C34 C 0.3874(6) 0.5277(4) 0.4866(3) 0.122(2) Uani 1 1 d . . . 
C35 C 0.5491(8) 0.5323(5) 0.5517(2) 0.143(3) Uani 1 1 d . . . 
H35 H 0.5829 0.5551 0.5874 0.172 Uiso 1 1 calc R . . 
C36 C 0.4401(8) 0.5583(4) 0.5384(3) 0.141(3) Uani 1 1 d . . . 
H36 H 0.3994 0.5983 0.5653 0.169 Uiso 1 1 calc R . . 
C37 C 0.9834(5) 0.3113(5) 0.4448(3) 0.174(3) Uani 1 1 d . . . 
H37A H 0.9526 0.3197 0.4840 0.261 Uiso 1 1 calc R . . 
H37B H 1.0282 0.3711 0.4350 0.261 Uiso 1 1 calc R . . 
H37C H 1.0313 0.2508 0.4442 0.261 Uiso 1 1 calc R . . 
C38 C 0.2445(9) 0.1543(7) 0.4049(5) 0.237(6) Uani 1 1 d . . . 
H38A H 0.2624 0.2238 0.4107 0.284 Uiso 1 1 calc R . . 
H38B H 0.1902 0.1225 0.4288 0.284 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 
O1 C7 1.366(4) . ? 
O1 C24 1.418(4) . ? 
O2 C6 1.369(4) . ? 
O2 C26 1.409(4) . ? 
O3 C9 1.368(4) . ? 
O3 C25 1.406(4) . ? 
O4 C18 1.373(4) . ? 
O4 C23 1.408(4) . ? 
O5 C17 1.368(4) . ? 
O5 C33 1.406(5) . ? 
O6 C22 1.366(4) . ? 
O6 C32 1.412(6) . ? 
C2 C10 1.377(4) . ? 
C2 C9 1.399(4) . ? 
C2 C16 1.504(4) . ? 
C3 C14 1.378(4) . ? 
C3 C7 1.399(4) . ? 
C3 C8 1.507(4) 3_666 ? 
C4 C19 1.369(4) . ? 
C4 C6 1.389(4) . ? 
C4 C8 1.511(4) . ? 
C5 C13 1.367(5) . ? 
C5 C18 1.384(4) . ? 
C5 C21 1.520(4) . ? 
C6 C13 1.398(4) . ? 
C7 C10 1.383(4) . ? 
C8 C3 1.507(4) 3_666 ? 
C9 C14 1.393(4) . ? 
C11 C15 1.372(4) . ? 
C11 C17 1.387(4) . ? 
C11 C16 1.507(4) . ? 
C12 C20 1.378(4) . ? 
C12 C22 1.385(5) . ? 
C12 C21 1.514(4) . ? 
C15 C22 1.383(4) . ? 
C17 C20 1.388(4) . ? 
C18 C19 1.383(4) . ? 
C23 C29 1.488(5) . ? 
C24 C31 1.498(6) . ? 
C25 C30 1.482(5) . ? 
C26 C28 1.490(5) . ? 
C27 C34 1.688(8) . ? 
C32 C38 1.299(9) . ? 
C33 C37 1.523(7) . ? 
C34 C36 1.356(8) . ? 
C34 C35 1.381(8) 3_666 ? 
C35 C36 1.336(9) . ? 
C35 C34 1.381(8) 3_666 ? 
 
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 
C7 O1 C24 118.4(3) . . ? 
C6 O2 C26 119.0(3) . . ? 
C9 O3 C25 119.7(3) . . ? 
C18 O4 C23 120.2(3) . . ? 
C17 O5 C33 119.8(3) . . ? 
C22 O6 C32 118.4(3) . . ? 
C10 C2 C9 117.6(3) . . ? 
C10 C2 C16 121.1(3) . . ? 
C9 C2 C16 121.2(3) . . ? 
C14 C3 C7 117.5(3) . . ? 
C14 C3 C8 120.8(3) . 3_666 ? 
C7 C3 C8 121.6(3) . 3_666 ? 
C19 C4 C6 118.2(3) . . ? 
C19 C4 C8 121.3(3) . . ? 
C6 C4 C8 120.4(3) . . ? 
C13 C5 C18 118.6(3) . . ? 
C13 C5 C21 120.4(3) . . ? 
C18 C5 C21 120.9(3) . . ? 
O2 C6 C13 124.1(3) . . ? 
O2 C6 C4 116.0(3) . . ? 
C13 C6 C4 119.9(3) . . ? 
O1 C7 C10 124.3(3) . . ? 
O1 C7 C3 115.8(3) . . ? 
C10 C7 C3 120.0(3) . . ? 
C4 C8 C3 116.8(2) . 3_666 ? 
O3 C9 C14 123.4(3) . . ? 
O3 C9 C2 116.9(3) . . ? 
C14 C9 C2 119.7(3) . . ? 
C7 C10 C2 122.7(3) . . ? 
C15 C11 C17 117.8(3) . . ? 
C15 C11 C16 121.7(3) . . ? 
C17 C11 C16 120.5(3) . . ? 
C20 C12 C22 117.9(3) . . ? 
C20 C12 C21 121.5(3) . . ? 
C22 C12 C21 120.5(3) . . ? 
C5 C13 C6 121.2(3) . . ? 
C3 C14 C9 122.5(3) . . ? 
C11 C15 C22 122.3(3) . . ? 
C11 C16 C2 114.8(2) . . ? 
O5 C17 C20 124.8(3) . . ? 
O5 C17 C11 115.2(3) . . ? 
C20 C17 C11 120.1(3) . . ? 
O4 C18 C5 115.4(3) . . ? 
O4 C18 C19 124.4(3) . . ? 
C5 C18 C19 120.2(3) . . ? 
C4 C19 C18 121.8(3) . . ? 
C12 C20 C17 121.8(3) . . ? 
C12 C21 C5 113.6(2) . . ? 
O6 C22 C12 115.4(3) . . ? 
O6 C22 C15 124.5(3) . . ? 
C12 C22 C15 120.0(3) . . ? 
O4 C23 C29 106.8(3) . . ? 
O1 C24 C31 107.2(3) . . ? 
O3 C25 C30 108.5(3) . . ? 
O2 C26 C28 107.9(3) . . ? 
C38 C32 O6 115.3(7) . . ? 
O5 C33 C37 106.4(4) . . ? 
C36 C34 C35 117.1(6) . 3_666 ? 
C36 C34 C27 120.5(6) . . ? 
C35 C34 C27 122.4(6) 3_666 . ? 
C36 C35 C34 121.3(5) . 3_666 ? 
C35 C36 C34 121.6(6) . . ? 
 
_diffrn_measured_fraction_theta_max    0.989 
_diffrn_reflns_theta_full              25.47 
_diffrn_measured_fraction_theta_full   0.989 
_refine_diff_density_max    0.458 
_refine_diff_density_min   -0.375 
_refine_diff_density_rms    0.047 
