# Supplementary Material (ESI) for Perkin Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 188/204
 
data_1a.THF #(1:2) 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C26 H23 O2' 
_chemical_formula_weight          367.44 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'    .0033    .0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'    .0000    .0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'    .0106    .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, -z' 
 
_cell_length_a                    8.9240(10) 
_cell_length_b                    9.1550(10) 
_cell_length_c                    11.963(2) 
_cell_angle_alpha                 90.53(2) 
_cell_angle_beta                  92.119(15) 
_cell_angle_gamma                 96.561(15) 
_cell_volume                      970.2(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.258 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              390 
_exptl_absorpt_coefficient_mu     0.078 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoKa  
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        ? 
_diffrn_measurement_method        ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             7552 
_diffrn_reflns_av_R_equivalents   0.0369 
_diffrn_reflns_av_sigmaI/netI     0.0558 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.24 
_diffrn_reflns_theta_max          25.79 
_reflns_number_total              3477 
_reflns_number_observed           2387 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0560P)^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     ? 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3477 
_refine_ls_number_parameters      276 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0583 
_refine_ls_R_factor_obs           0.0358 
_refine_ls_wR_factor_all          0.0915 
_refine_ls_wR_factor_obs          0.0823 
_refine_ls_goodness_of_fit_all    0.901 
_refine_ls_goodness_of_fit_obs    0.996 
_refine_ls_restrained_S_all       0.901 
_refine_ls_restrained_S_obs       0.996 
_refine_ls_shift/esd_max          0.061 
_refine_ls_shift/esd_mean         0.004 
 
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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
O1 O 0.47049(12) 0.79789(11) 0.16301(8) 0.0214(3) Uani 1 d . . 
H1O H 0.41695(12) 0.84789(11) 0.21990(8) 0.093(9) Uiso 1 d R . 
C1 C 0.9658(2) 0.58984(15) 0.41033(12) 0.0187(3) Uani 1 d . . 
H1 H 0.9427(2) 0.65088(15) 0.34977(12) 0.019(4) Uiso 1 calc R . 
C2 C 0.8618(2) 0.56259(15) 0.49492(12) 0.0170(3) Uani 1 d . . 
C3 C 0.8971(2) 0.47088(15) 0.58683(11) 0.0177(3) Uani 1 d . . 
C4 C 0.7898(2) 0.4425(2) 0.67278(12) 0.0207(4) Uani 1 d . . 
H4 H 0.8111(2) 0.3801(2) 0.73292(12) 0.021(4) Uiso 1 calc R . 
C5 C 0.6577(2) 0.5043(2) 0.66901(12) 0.0210(4) Uani 1 d . . 
H5 H 0.5885(2) 0.4854(2) 0.72704(12) 0.027(4) Uiso 1 calc R . 
C6 C 0.6224(2) 0.5966(2) 0.57944(12) 0.0201(3) Uani 1 d . . 
H6 H 0.5306(2) 0.6400(2) 0.57895(12) 0.022(4) Uiso 1 calc R . 
C7 C 0.7194(2) 0.62418(15) 0.49304(12) 0.0182(3) Uani 1 d . . 
C8 C 0.6793(2) 0.7081(2) 0.39743(12) 0.0184(3) Uani 1 d . . 
C9 C 0.6515(2) 0.7704(2) 0.31244(12) 0.0189(3) Uani 1 d . . 
C10 C 0.6229(2) 0.8401(2) 0.20259(12) 0.0174(3) Uani 1 d . . 
C11 C 0.6559(2) 1.0084(2) 0.21107(12) 0.0177(3) Uani 1 d . . 
C12 C 0.6506(2) 1.0908(2) 0.11317(13) 0.0218(4) Uani 1 d . . 
H12 H 0.6280(2) 1.0420(2) 0.04311(13) 0.024(4) Uiso 1 calc R . 
C13 C 0.6782(2) 1.2433(2) 0.11776(13) 0.0249(4) Uani 1 d . . 
H13 H 0.6740(2) 1.2981(2) 0.05088(13) 0.033(5) Uiso 1 calc R . 
C14 C 0.7118(2) 1.3163(2) 0.21978(14) 0.0270(4) Uani 1 d . . 
H14 H 0.7308(2) 1.4205(2) 0.22262(14) 0.030(5) Uiso 1 calc R . 
C15 C 0.7173(2) 1.2359(2) 0.31726(14) 0.0264(4) Uani 1 d . . 
H15 H 0.7405(2) 1.2850(2) 0.38715(14) 0.027(4) Uiso 1 calc R . 
C16 C 0.6885(2) 1.0828(2) 0.31241(12) 0.0222(4) Uani 1 d . . 
H16 H 0.6913(2) 1.0285(2) 0.37958(12) 0.023(4) Uiso 1 calc R . 
C17 C 0.7262(2) 0.7740(2) 0.11957(12) 0.0184(3) Uani 1 d . . 
C18 C 0.8808(2) 0.8176(2) 0.12456(13) 0.0261(4) Uani 1 d . . 
H18 H 0.9218(2) 0.8895(2) 0.17844(13) 0.028(5) Uiso 1 calc R . 
C19 C 0.9764(2) 0.7576(2) 0.05178(14) 0.0302(4) Uani 1 d . . 
H19 H 1.0818(2) 0.7884(2) 0.05629(14) 0.043(5) Uiso 1 calc R . 
C20 C 0.9174(2) 0.6527(2) -0.02726(13) 0.0267(4) Uani 1 d . . 
H20 H 0.9817(2) 0.6128(2) -0.07808(13) 0.028(4) Uiso 1 calc R . 
C21 C 0.7640(2) 0.6066(2) -0.03151(12) 0.0269(4) Uani 1 d . . 
H21 H 0.7236(2) 0.5335(2) -0.08468(12) 0.039(5) Uiso 1 calc R . 
C22 C 0.6678(2) 0.6665(2) 0.04166(12) 0.0219(4) Uani 1 d . . 
H22 H 0.5628(2) 0.6338(2) 0.03820(12) 0.027(4) Uiso 1 calc R . 
O1T O 0.25725(13) 0.94663(11) 0.25511(9) 0.0276(3) Uani 1 d . . 
C1T C 0.2318(2) 1.0842(2) 0.20308(14) 0.0287(4) Uani 1 d . . 
H1TA H 0.2015(2) 1.0681(2) 0.12309(14) 0.038(5) Uiso 1 calc R . 
H1TB H 0.3247(2) 1.1547(2) 0.20871(14) 0.041(5) Uiso 1 calc R . 
C2T C 0.1046(2) 1.1430(2) 0.26722(13) 0.0240(4) Uani 1 d . . 
H2TA H 0.0082(2) 1.1299(2) 0.22261(13) 0.041(5) Uiso 1 calc R . 
H2TB H 0.1300(2) 1.2486(2) 0.28633(13) 0.035(5) Uiso 1 calc R . 
C3T C 0.0942(2) 1.0492(2) 0.37373(13) 0.0272(4) Uani 1 d . . 
H3TA H 0.0946(2) 1.1120(2) 0.44158(13) 0.034(5) Uiso 1 calc R . 
H3TB H 0.0017(2) 0.9783(2) 0.37088(13) 0.027(4) Uiso 1 calc R . 
C4T C 0.2353(2) 0.9701(2) 0.37218(13) 0.0291(4) Uani 1 d . . 
H4TA H 0.3231(2) 1.0315(2) 0.40765(13) 0.028(4) Uiso 1 calc R . 
H4TB H 0.2198(2) 0.8755(2) 0.41180(13) 0.029(4) Uiso 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 0.0168(6) 0.0250(6) 0.0225(5) -0.0017(4) -0.0002(5) 0.0029(4) 
C1 0.0244(10) 0.0159(7) 0.0157(7) 0.0018(6) 0.0010(7) 0.0022(6) 
C2 0.0198(9) 0.0136(7) 0.0174(7) -0.0014(6) -0.0001(6) 0.0013(6) 
C3 0.0228(10) 0.0148(7) 0.0155(7) -0.0008(6) 0.0022(7) 0.0018(6) 
C4 0.0254(10) 0.0190(8) 0.0177(7) 0.0029(6) 0.0021(7) 0.0019(6) 
C5 0.0215(10) 0.0229(8) 0.0178(7) 0.0006(6) 0.0039(7) -0.0024(6) 
C6 0.0176(9) 0.0234(8) 0.0194(8) -0.0016(6) 0.0004(7) 0.0027(6) 
C7 0.0213(9) 0.0163(7) 0.0166(7) -0.0012(6) 0.0004(7) 0.0009(6) 
C8 0.0163(9) 0.0187(7) 0.0208(8) 0.0001(6) 0.0024(7) 0.0035(6) 
C9 0.0163(9) 0.0184(7) 0.0226(8) -0.0016(6) 0.0040(7) 0.0038(6) 
C10 0.0142(9) 0.0219(8) 0.0164(7) 0.0012(6) -0.0008(7) 0.0036(6) 
C11 0.0129(9) 0.0195(7) 0.0215(8) 0.0017(6) 0.0030(7) 0.0052(6) 
C12 0.0198(10) 0.0260(8) 0.0204(8) 0.0014(6) 0.0022(7) 0.0051(6) 
C13 0.0215(10) 0.0247(8) 0.0299(9) 0.0073(7) 0.0043(7) 0.0068(7) 
C14 0.0249(10) 0.0184(8) 0.0390(10) 0.0009(7) 0.0050(8) 0.0075(6) 
C15 0.0274(11) 0.0255(8) 0.0270(8) -0.0069(7) 0.0021(8) 0.0061(7) 
C16 0.0243(10) 0.0234(8) 0.0199(8) 0.0012(6) 0.0036(7) 0.0065(7) 
C17 0.0218(9) 0.0171(7) 0.0175(7) 0.0039(6) 0.0022(7) 0.0072(6) 
C18 0.0235(10) 0.0260(8) 0.0292(9) -0.0054(7) 0.0046(8) 0.0040(7) 
C19 0.0242(11) 0.0306(9) 0.0376(10) 0.0026(7) 0.0094(8) 0.0085(7) 
C20 0.0356(11) 0.0247(9) 0.0233(8) 0.0061(7) 0.0117(8) 0.0155(7) 
C21 0.0401(12) 0.0238(9) 0.0185(8) -0.0005(6) 0.0035(8) 0.0102(7) 
C22 0.0241(10) 0.0211(8) 0.0214(8) 0.0013(6) 0.0020(7) 0.0050(7) 
O1T 0.0317(7) 0.0275(6) 0.0258(6) 0.0029(5) 0.0053(5) 0.0113(5) 
C1T 0.0318(11) 0.0276(9) 0.0289(9) 0.0080(7) 0.0100(8) 0.0096(7) 
C2T 0.0260(11) 0.0209(8) 0.0255(8) -0.0002(6) 0.0047(8) 0.0031(7) 
C3T 0.0321(11) 0.0249(9) 0.0246(8) -0.0013(7) 0.0075(8) 0.0003(7) 
C4T 0.0366(12) 0.0282(9) 0.0228(8) 0.0041(7) 0.0013(8) 0.0049(8) 
 
_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 C10 1.433(2) . ? 
O1 H1O 0.98 . ? 
C1 C3 1.400(2) 2_766 ? 
C1 C2 1.403(2) . ? 
C1 H1 0.95 . ? 
C2 C3 1.437(2) . ? 
C2 C7 1.447(2) . ? 
C3 C1 1.400(2) 2_766 ? 
C3 C4 1.436(2) . ? 
C4 C5 1.365(2) . ? 
C4 H4 0.95 . ? 
C5 C6 1.419(2) . ? 
C5 H5 0.95 . ? 
C6 C7 1.380(2) . ? 
C6 H6 0.95 . ? 
C7 C8 1.441(2) . ? 
C8 C9 1.202(2) . ? 
C9 C10 1.492(2) . ? 
C10 C11 1.537(2) . ? 
C10 C17 1.545(2) . ? 
C11 C16 1.390(2) . ? 
C11 C12 1.401(2) . ? 
C12 C13 1.390(2) . ? 
C12 H12 0.95 . ? 
C13 C14 1.392(2) . ? 
C13 H13 0.95 . ? 
C14 C15 1.387(2) . ? 
C14 H14 0.95 . ? 
C15 C16 1.397(2) . ? 
C15 H15 0.95 . ? 
C16 H16 0.95 . ? 
C17 C22 1.393(2) . ? 
C17 C18 1.390(2) . ? 
C18 C19 1.393(2) . ? 
C18 H18 0.95 . ? 
C19 C20 1.387(3) . ? 
C19 H19 0.95 . ? 
C20 C21 1.385(2) . ? 
C20 H20 0.95 . ? 
C21 C22 1.399(2) . ? 
C21 H21 0.95 . ? 
C22 H22 0.95 . ? 
O1T C4T 1.439(2) . ? 
O1T C1T 1.447(2) . ? 
C1T C2T 1.538(2) . ? 
C1T H1TA 0.99 . ? 
C1T H1TB 0.99 . ? 
C2T C3T 1.543(2) . ? 
C2T H2TA 0.99 . ? 
C2T H2TB 0.99 . ? 
C3T C4T 1.523(2) . ? 
C3T H3TA 0.99 . ? 
C3T H3TB 0.99 . ? 
C4T H4TA 0.99 . ? 
C4T H4TB 0.99 . ? 
 
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 
C10 O1 H1O 99.43(7) . . ? 
C3 C1 C2 121.49(13) 2_766 . ? 
C3 C1 H1 119.26(8) 2_766 . ? 
C2 C1 H1 119.26(9) . . ? 
C1 C2 C3 119.26(14) . . ? 
C1 C2 C7 122.16(13) . . ? 
C3 C2 C7 118.58(12) . . ? 
C1 C3 C2 119.25(13) 2_766 . ? 
C1 C3 C4 121.71(13) 2_766 . ? 
C2 C3 C4 119.04(14) . . ? 
C5 C4 C3 120.70(13) . . ? 
C5 C4 H4 119.65(8) . . ? 
C3 C4 H4 119.65(9) . . ? 
C4 C5 C6 120.77(13) . . ? 
C4 C5 H5 119.61(8) . . ? 
C6 C5 H5 119.61(9) . . ? 
C7 C6 C5 120.94(14) . . ? 
C7 C6 H6 119.53(9) . . ? 
C5 C6 H6 119.53(9) . . ? 
C6 C7 C8 121.33(14) . . ? 
C6 C7 C2 119.93(13) . . ? 
C8 C7 C2 118.68(12) . . ? 
C9 C8 C7 174.68(15) . . ? 
C8 C9 C10 175.90(15) . . ? 
O1 C10 C9 110.17(11) . . ? 
O1 C10 C11 110.59(11) . . ? 
C9 C10 C11 111.27(12) . . ? 
O1 C10 C17 106.89(12) . . ? 
C9 C10 C17 105.95(11) . . ? 
C11 C10 C17 111.80(11) . . ? 
C16 C11 C12 118.48(13) . . ? 
C16 C11 C10 122.61(12) . . ? 
C12 C11 C10 118.90(13) . . ? 
C13 C12 C11 120.50(15) . . ? 
C13 C12 H12 119.75(9) . . ? 
C11 C12 H12 119.75(9) . . ? 
C12 C13 C14 120.39(14) . . ? 
C12 C13 H13 119.81(9) . . ? 
C14 C13 H13 119.81(9) . . ? 
C15 C14 C13 119.64(14) . . ? 
C15 C14 H14 120.18(10) . . ? 
C13 C14 H14 120.18(9) . . ? 
C14 C15 C16 119.8(2) . . ? 
C14 C15 H15 120.09(10) . . ? 
C16 C15 H15 120.09(9) . . ? 
C11 C16 C15 121.18(14) . . ? 
C11 C16 H16 119.41(8) . . ? 
C15 C16 H16 119.41(9) . . ? 
C22 C17 C18 118.90(13) . . ? 
C22 C17 C10 120.96(14) . . ? 
C18 C17 C10 120.09(13) . . ? 
C19 C18 C17 121.1(2) . . ? 
C19 C18 H18 119.47(11) . . ? 
C17 C18 H18 119.47(9) . . ? 
C18 C19 C20 119.9(2) . . ? 
C18 C19 H19 120.06(11) . . ? 
C20 C19 H19 120.06(10) . . ? 
C21 C20 C19 119.48(14) . . ? 
C21 C20 H20 120.26(9) . . ? 
C19 C20 H20 120.26(10) . . ? 
C20 C21 C22 120.7(2) . . ? 
C20 C21 H21 119.64(9) . . ? 
C22 C21 H21 119.64(10) . . ? 
C17 C22 C21 119.9(2) . . ? 
C17 C22 H22 120.04(9) . . ? 
C21 C22 H22 120.04(10) . . ? 
C4T O1T C1T 104.75(11) . . ? 
O1T C1T C2T 105.91(11) . . ? 
O1T C1T H1TA 110.55(8) . . ? 
C2T C1T H1TA 110.55(10) . . ? 
O1T C1T H1TB 110.55(9) . . ? 
C2T C1T H1TB 110.55(9) . . ? 
H1TA C1T H1TB 108.7 . . ? 
C1T C2T C3T 103.90(12) . . ? 
C1T C2T H2TA 110.98(10) . . ? 
C3T C2T H2TA 110.98(9) . . ? 
C1T C2T H2TB 110.98(9) . . ? 
C3T C2T H2TB 110.98(9) . . ? 
H2TA C2T H2TB 109.0 . . ? 
C4T C3T C2T 103.46(12) . . ? 
C4T C3T H3TA 111.07(9) . . ? 
C2T C3T H3TA 111.07(8) . . ? 
C4T C3T H3TB 111.07(9) . . ? 
C2T C3T H3TB 111.07(9) . . ? 
H3TA C3T H3TB 109.0 . . ? 
O1T C4T C3T 104.05(13) . . ? 
O1T C4T H4TA 110.95(9) . . ? 
C3T C4T H4TA 110.95(9) . . ? 
O1T C4T H4TB 110.95(8) . . ? 
C3T C4T H4TB 110.95(8) . . ? 
H4TA C4T H4TB 109.0 . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
 C3 C1 C2 C3 0.3(2) 2_766 . . . ? 
 C3 C1 C2 C7 -179.82(14) 2_766 . . . ? 
 C1 C2 C3 C1 -0.3(2) . . . 2_766 ? 
 C7 C2 C3 C1 179.82(14) . . . 2_766 ? 
 C1 C2 C3 C4 -179.59(14) . . . . ? 
 C7 C2 C3 C4 0.5(2) . . . . ? 
 C1 C3 C4 C5 179.20(15) 2_766 . . . ? 
 C2 C3 C4 C5 -1.5(2) . . . . ? 
 C3 C4 C5 C6 0.8(2) . . . . ? 
 C4 C5 C6 C7 1.1(2) . . . . ? 
 C5 C6 C7 C8 175.06(15) . . . . ? 
 C5 C6 C7 C2 -2.1(2) . . . . ? 
 C1 C2 C7 C6 -178.64(14) . . . . ? 
 C3 C2 C7 C6 1.2(2) . . . . ? 
 C1 C2 C7 C8 4.2(2) . . . . ? 
 C3 C2 C7 C8 -175.97(13) . . . . ? 
 C6 C7 C8 C9 -141.5(18) . . . . ? 
 C2 C7 C8 C9 35.7(19) . . . . ? 
 C7 C8 C9 C10 -2.6(39) . . . . ? 
 C8 C9 C10 O1 103.9(23) . . . . ? 
 C8 C9 C10 C11 -133.1(23) . . . . ? 
 C8 C9 C10 C17 -11.4(24) . . . . ? 
 O1 C10 C11 C16 115.0(2) . . . . ? 
 C9 C10 C11 C16 -7.8(2) . . . . ? 
 C17 C10 C11 C16 -126.0(2) . . . . ? 
 O1 C10 C11 C12 -63.9(2) . . . . ? 
 C9 C10 C11 C12 173.30(13) . . . . ? 
 C17 C10 C11 C12 55.1(2) . . . . ? 
 C16 C11 C12 C13 0.3(2) . . . . ? 
 C10 C11 C12 C13 179.29(14) . . . . ? 
 C11 C12 C13 C14 0.2(2) . . . . ? 
 C12 C13 C14 C15 -0.2(3) . . . . ? 
 C13 C14 C15 C16 -0.2(2) . . . . ? 
 C12 C11 C16 C15 -0.7(2) . . . . ? 
 C10 C11 C16 C15 -179.69(14) . . . . ? 
 C14 C15 C16 C11 0.7(2) . . . . ? 
 O1 C10 C17 C22 -13.9(2) . . . . ? 
 C9 C10 C17 C22 103.6(2) . . . . ? 
 C11 C10 C17 C22 -135.00(14) . . . . ? 
 O1 C10 C17 C18 168.58(12) . . . . ? 
 C9 C10 C17 C18 -73.9(2) . . . . ? 
 C11 C10 C17 C18 47.4(2) . . . . ? 
 C22 C17 C18 C19 1.3(2) . . . . ? 
 C10 C17 C18 C19 178.88(14) . . . . ? 
 C17 C18 C19 C20 0.1(2) . . . . ? 
 C18 C19 C20 C21 -1.3(2) . . . . ? 
 C19 C20 C21 C22 1.1(2) . . . . ? 
 C18 C17 C22 C21 -1.4(2) . . . . ? 
 C10 C17 C22 C21 -178.99(13) . . . . ? 
 C20 C21 C22 C17 0.2(2) . . . . ? 
 C4T O1T C1T C2T -36.1(2) . . . . ? 
 O1T C1T C2T C3T 14.2(2) . . . . ? 
 C1T C2T C3T C4T 11.4(2) . . . . ? 
 C1T O1T C4T C3T 43.6(2) . . . . ? 
 C2T C3T C4T O1T -33.4(2) . . . . ? 
 
_refine_diff_density_max     .160 
_refine_diff_density_min    -.192 
_refine_diff_density_rms     .045 

 
data_1a.acetone #(1:2) 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C50 H42 O4' 
_chemical_formula_weight          706.84 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'    .0181    .0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'    .0000    .0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'    .0492    .0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            'monoclinic (b unique)' 
_symmetry_space_group_name_H-M    P21/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                    11.5927(3) 
_cell_length_b                    12.8758(5) 
_cell_length_c                    14.0251(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  105.162(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2020.59(11) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     291(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.162 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              748 
_exptl_absorpt_coefficient_mu     0.568 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       291(2) 
_diffrn_radiation_wavelength      1.54180 
_diffrn_radiation_type            CuKa  
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        ? 
_diffrn_measurement_method        ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             3302 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0199 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          4.42 
_diffrn_reflns_theta_max          64.99 
_reflns_number_total              3302 
_reflns_number_observed           2366 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 12 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0947P)^2^+0.5215P] 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     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0190(14) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^' 
_refine_ls_number_reflns          3290 
_refine_ls_number_parameters      268 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0784 
_refine_ls_R_factor_obs           0.0583 
_refine_ls_wR_factor_all          0.1919 
_refine_ls_wR_factor_obs          0.1590 
_refine_ls_goodness_of_fit_all    1.059 
_refine_ls_goodness_of_fit_obs    1.156 
_refine_ls_restrained_S_all       1.169 
_refine_ls_restrained_S_obs       1.156 
_refine_ls_shift/esd_max          -0.089 
_refine_ls_shift/esd_mean         0.009 
 
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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
O1 O 0.1982(2) -0.15152(13) 0.59939(13) 0.0618(5) Uani 1 d . . 
H1O H 0.1716(2) -0.19959(13) 0.55543(13) 0.097(11) Uiso 1 d R . 
C1 C 0.5891(2) -0.5673(2) 0.4869(2) 0.0485(6) Uani 1 d . . 
H1 H 0.6485(2) -0.6122(2) 0.4784(2) 0.068(8) Uiso 1 calc R . 
C2 C 0.4743(2) -0.6056(2) 0.4770(2) 0.0451(5) Uani 1 d . . 
C3 C 0.6174(2) -0.4629(2) 0.5095(2) 0.0474(6) Uani 1 d . . 
C4 C 0.7342(2) -0.4231(2) 0.5208(2) 0.0586(7) Uani 1 d . . 
H4 H 0.7941(2) -0.4670(2) 0.5115(2) 0.079(9) Uiso 1 calc R . 
C5 C 0.7602(2) -0.3221(2) 0.5449(2) 0.0664(7) Uani 1 d . . 
H5 H 0.8375(2) -0.2977(2) 0.5524(2) 0.081(9) Uiso 1 calc R . 
C6 C 0.6706(2) -0.2538(2) 0.5588(2) 0.0622(7) Uani 1 d . . 
H6 H 0.6900(2) -0.1851(2) 0.5763(2) 0.078(9) Uiso 1 calc R . 
C7 C 0.5566(2) -0.2872(2) 0.5469(2) 0.0495(6) Uani 1 d . . 
C8 C 0.4635(2) -0.2167(2) 0.5561(2) 0.0519(6) Uani 1 d . . 
C9 C 0.3848(2) -0.1595(2) 0.5606(2) 0.0517(6) Uani 1 d . . 
C10 C 0.2830(2) -0.0921(2) 0.5647(2) 0.0462(6) Uani 1 d . . 
C11 C 0.2229(2) -0.0464(2) 0.4630(2) 0.0454(5) Uani 1 d . . 
C12 C 0.1293(2) 0.0232(2) 0.4542(2) 0.0580(7) Uani 1 d . . 
H12 H 0.1072(2) 0.0441(2) 0.5104(2) 0.075(8) Uiso 1 calc R . 
C13 C 0.0687(3) 0.0616(2) 0.3631(2) 0.0695(8) Uani 1 d . . 
H13 H 0.0054(3) 0.1074(2) 0.3583(2) 0.142(15) Uiso 1 calc R . 
C14 C 0.1013(3) 0.0327(3) 0.2794(2) 0.0780(9) Uani 1 d . . 
H14 H 0.0608(3) 0.0591(3) 0.2181(2) 0.094(10) Uiso 1 calc R . 
C15 C 0.1938(3) -0.0352(3) 0.2874(2) 0.0842(9) Uani 1 d . . 
H15 H 0.2165(3) -0.0552(3) 0.2312(2) 0.107(12) Uiso 1 calc R . 
C16 C 0.2539(3) -0.0745(2) 0.3785(2) 0.0651(7) Uani 1 d . . 
H16 H 0.3166(3) -0.1209(2) 0.3828(2) 0.108(12) Uiso 1 calc R . 
C17 C 0.3273(2) -0.0057(2) 0.6408(2) 0.0486(6) Uani 1 d . . 
C18 C 0.4137(2) 0.0622(2) 0.6284(2) 0.0625(7) Uani 1 d . . 
H18 H 0.4456(2) 0.0544(2) 0.5745(2) 0.067(8) Uiso 1 calc R . 
C19 C 0.4539(3) 0.1416(2) 0.6949(3) 0.0799(9) Uani 1 d . . 
H19 H 0.5113(3) 0.1879(2) 0.6850(3) 0.094(11) Uiso 1 calc R . 
C20 C 0.4090(3) 0.1523(3) 0.7756(3) 0.0883(10) Uani 1 d . . 
H20 H 0.4367(3) 0.2049(3) 0.8212(3) 0.105(11) Uiso 1 calc R . 
C21 C 0.3236(3) 0.0852(3) 0.7884(3) 0.0985(12) Uani 1 d . . 
H21 H 0.2927(3) 0.0927(3) 0.8428(3) 0.123(13) Uiso 1 calc R . 
C22 C 0.2820(3) 0.0059(2) 0.7213(2) 0.0770(9) Uani 1 d . . 
H22 H 0.2235(3) -0.0394(2) 0.7309(2) 0.093(11) Uiso 1 calc R . 
O1A O 0.1065(3) -0.3094(2) 0.4675(2) 0.1354(12) Uani 1 d . . 
C1A C 0.0560(4) -0.3090(3) 0.3795(3) 0.1036(12) Uani 1 d . . 
C2A C 0.1090(6) -0.3575(5) 0.3083(4) 0.140(2) Uani 1 d . . 
H2AA H 0.1882(16) -0.3809(31) 0.3408(7) 0.176(22) Uiso 1 calc R . 
H2AB H 0.1130(35) -0.3082(11) 0.2579(18) 0.231(33) Uiso 1 calc R . 
H2AC H 0.0611(22) -0.4158(21) 0.2787(23) 0.272(43) Uiso 1 calc R . 
C3A C -0.0458(6) -0.2411(5) 0.3405(5) 0.143(2) Uani 1 d . . 
H3AA H -0.0613(25) -0.2007(24) 0.3933(7) 0.281(40) Uiso 1 calc R . 
H3AB H -0.1148(10) -0.2824(5) 0.3107(28) 0.167(23) Uiso 1 calc R . 
H3AC H -0.0284(15) -0.1956(22) 0.2919(23) 0.232(34) Uiso 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 0.0815(12) 0.0508(10) 0.0624(11) -0.0039(8) 0.0355(9) -0.0156(9) 
C1 0.0544(13) 0.0381(11) 0.0550(13) -0.0036(10) 0.0180(11) 0.0096(10) 
C2 0.0519(13) 0.0367(11) 0.0475(12) -0.0012(9) 0.0143(10) 0.0070(10) 
C3 0.0508(13) 0.0407(11) 0.0520(13) -0.0005(10) 0.0159(10) 0.0062(10) 
C4 0.0533(14) 0.0505(14) 0.075(2) 0.0008(12) 0.0227(13) 0.0071(11) 
C5 0.054(2) 0.055(2) 0.091(2) 0.0007(14) 0.0215(14) -0.0042(12) 
C6 0.067(2) 0.0410(13) 0.078(2) -0.0011(12) 0.0176(14) -0.0026(12) 
C7 0.0583(14) 0.0372(11) 0.0522(13) -0.0006(10) 0.0133(11) 0.0048(10) 
C8 0.0645(15) 0.0372(12) 0.0541(14) -0.0034(10) 0.0155(12) 0.0058(11) 
C9 0.069(2) 0.0373(12) 0.0504(13) -0.0041(9) 0.0177(12) 0.0038(11) 
C10 0.0571(13) 0.0357(11) 0.0517(13) -0.0030(9) 0.0246(11) -0.0003(10) 
C11 0.0487(12) 0.0384(11) 0.0529(13) -0.0023(9) 0.0198(10) -0.0026(9) 
C12 0.0580(14) 0.0492(14) 0.071(2) -0.0009(12) 0.0242(13) 0.0067(11) 
C13 0.060(2) 0.058(2) 0.087(2) 0.0071(14) 0.0127(14) 0.0077(13) 
C14 0.076(2) 0.086(2) 0.065(2) 0.015(2) 0.007(2) 0.006(2) 
C15 0.091(2) 0.109(3) 0.056(2) 0.005(2) 0.024(2) 0.020(2) 
C16 0.071(2) 0.077(2) 0.0513(15) 0.0019(13) 0.0241(13) 0.0174(15) 
C17 0.0592(14) 0.0386(11) 0.0506(13) -0.0050(9) 0.0193(11) 0.0041(10) 
C18 0.078(2) 0.0479(14) 0.069(2) -0.0151(12) 0.0338(14) -0.0089(12) 
C19 0.086(2) 0.061(2) 0.098(2) -0.030(2) 0.035(2) -0.020(2) 
C20 0.094(2) 0.083(2) 0.092(2) -0.047(2) 0.032(2) -0.014(2) 
C21 0.117(3) 0.109(3) 0.085(2) -0.051(2) 0.055(2) -0.028(2) 
C22 0.090(2) 0.081(2) 0.073(2) -0.027(2) 0.044(2) -0.020(2) 
O1A 0.220(3) 0.099(2) 0.072(2) -0.0070(14) 0.011(2) -0.050(2) 
C1A 0.137(3) 0.094(3) 0.062(2) -0.013(2) -0.005(2) 0.010(3) 
C2A 0.156(5) 0.168(5) 0.083(3) -0.002(3) 0.007(3) 0.046(4) 
C3A 0.182(6) 0.103(3) 0.158(5) -0.033(4) 0.069(5) -0.004(4) 
 
_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 C10 1.428(3) . ? 
O1 H1O 0.87 . ? 
C1 C2 1.391(3) . ? 
C1 C3 1.401(3) . ? 
C1 H1 0.93 . ? 
C2 C3 1.432(3) 3_646 ? 
C2 C7 1.443(3) 3_646 ? 
C3 C4 1.417(3) . ? 
C3 C2 1.432(3) 3_646 ? 
C4 C5 1.358(4) . ? 
C4 H4 0.93 . ? 
C5 C6 1.412(4) . ? 
C5 H5 0.93 . ? 
C6 C7 1.358(3) . ? 
C6 H6 0.93 . ? 
C7 C8 1.442(3) . ? 
C7 C2 1.443(3) 3_646 ? 
C8 C9 1.187(3) . ? 
C9 C10 1.478(3) . ? 
C10 C11 1.532(3) . ? 
C10 C17 1.534(3) . ? 
C11 C16 1.373(3) . ? 
C11 C12 1.388(3) . ? 
C12 C13 1.378(4) . ? 
C12 H12 0.93 . ? 
C13 C14 1.375(4) . ? 
C13 H13 0.93 . ? 
C14 C15 1.366(4) . ? 
C14 H14 0.93 . ? 
C15 C16 1.382(4) . ? 
C15 H15 0.93 . ? 
C16 H16 0.93 . ? 
C17 C22 1.372(3) . ? 
C17 C18 1.374(3) . ? 
C18 C19 1.381(4) . ? 
C18 H18 0.93 . ? 
C19 C20 1.370(4) . ? 
C19 H19 0.93 . ? 
C20 C21 1.360(5) . ? 
C20 H20 0.93 . ? 
C21 C22 1.388(4) . ? 
C21 H21 0.93 . ? 
C22 H22 0.93 . ? 
O1A C1A 1.220(4) . ? 
C1A C2A 1.445(6) . ? 
C1A C3A 1.455(6) . ? 
C2A H2AA 0.96 . ? 
C2A H2AB 0.96 . ? 
C2A H2AC 0.96 . ? 
C3A H3AA 0.96 . ? 
C3A H3AB 0.96 . ? 
C3A H3AC 0.96 . ? 
 
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 
C10 O1 H1O 106.72(11) . . ? 
C2 C1 C3 121.6(2) . . ? 
C2 C1 H1 119.18(12) . . ? 
C3 C1 H1 119.18(13) . . ? 
C1 C2 C3 119.5(2) . 3_646 ? 
C1 C2 C7 122.4(2) . 3_646 ? 
C3 C2 C7 118.2(2) 3_646 3_646 ? 
C1 C3 C4 122.2(2) . . ? 
C1 C3 C2 118.9(2) . 3_646 ? 
C4 C3 C2 118.9(2) . 3_646 ? 
C5 C4 C3 121.1(2) . . ? 
C5 C4 H4 119.4(2) . . ? 
C3 C4 H4 119.44(13) . . ? 
C4 C5 C6 120.5(2) . . ? 
C4 C5 H5 119.8(2) . . ? 
C6 C5 H5 119.75(15) . . ? 
C7 C6 C5 120.9(2) . . ? 
C7 C6 H6 119.56(14) . . ? 
C5 C6 H6 119.56(15) . . ? 
C6 C7 C8 121.1(2) . . ? 
C6 C7 C2 120.4(2) . 3_646 ? 
C8 C7 C2 118.5(2) . 3_646 ? 
C9 C8 C7 177.8(3) . . ? 
C8 C9 C10 177.5(3) . . ? 
O1 C10 C9 109.0(2) . . ? 
O1 C10 C11 109.7(2) . . ? 
C9 C10 C11 111.2(2) . . ? 
O1 C10 C17 106.6(2) . . ? 
C9 C10 C17 109.2(2) . . ? 
C11 C10 C17 110.9(2) . . ? 
C16 C11 C12 117.9(2) . . ? 
C16 C11 C10 123.0(2) . . ? 
C12 C11 C10 119.0(2) . . ? 
C13 C12 C11 120.8(2) . . ? 
C13 C12 H12 119.6(2) . . ? 
C11 C12 H12 119.61(15) . . ? 
C14 C13 C12 120.4(3) . . ? 
C14 C13 H13 119.8(2) . . ? 
C12 C13 H13 119.8(2) . . ? 
C15 C14 C13 119.3(3) . . ? 
C15 C14 H14 120.4(2) . . ? 
C13 C14 H14 120.4(2) . . ? 
C14 C15 C16 120.4(3) . . ? 
C14 C15 H15 119.8(2) . . ? 
C16 C15 H15 119.8(2) . . ? 
C11 C16 C15 121.2(3) . . ? 
C11 C16 H16 119.38(15) . . ? 
C15 C16 H16 119.4(2) . . ? 
C22 C17 C18 119.0(2) . . ? 
C22 C17 C10 121.4(2) . . ? 
C18 C17 C10 119.7(2) . . ? 
C17 C18 C19 120.9(3) . . ? 
C17 C18 H18 119.54(14) . . ? 
C19 C18 H18 119.5(2) . . ? 
C20 C19 C18 119.9(3) . . ? 
C20 C19 H19 120.1(2) . . ? 
C18 C19 H19 120.1(2) . . ? 
C21 C20 C19 119.5(3) . . ? 
C21 C20 H20 120.3(2) . . ? 
C19 C20 H20 120.3(2) . . ? 
C20 C21 C22 120.9(3) . . ? 
C20 C21 H21 119.5(2) . . ? 
C22 C21 H21 119.5(2) . . ? 
C17 C22 C21 119.8(3) . . ? 
C17 C22 H22 120.1(2) . . ? 
C21 C22 H22 120.1(2) . . ? 
O1A C1A C2A 121.3(5) . . ? 
O1A C1A C3A 120.7(4) . . ? 
C2A C1A C3A 116.7(4) . . ? 
C1A C2A H2AA 109.5(3) . . ? 
C1A C2A H2AB 109.5(3) . . ? 
H2AA C2A H2AB 109.5 . . ? 
C1A C2A H2AC 109.5(3) . . ? 
H2AA C2A H2AC 109.5 . . ? 
H2AB C2A H2AC 109.5 . . ? 
C1A C3A H3AA 109.5(3) . . ? 
C1A C3A H3AB 109.5(3) . . ? 
H3AA C3A H3AB 109.5 . . ? 
C1A C3A H3AC 109.5(3) . . ? 
H3AA C3A H3AC 109.5 . . ? 
H3AB C3A H3AC 109.5 . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
 C3 C1 C2 C3 -0.3(4) . . . 3_646 ? 
 C3 C1 C2 C7 179.5(2) . . . 3_646 ? 
 C2 C1 C3 C4 179.3(2) . . . . ? 
 C2 C1 C3 C2 0.3(4) . . . 3_646 ? 
 C1 C3 C4 C5 -178.4(3) . . . . ? 
 C2 C3 C4 C5 0.6(4) 3_646 . . . ? 
 C3 C4 C5 C6 -0.4(4) . . . . ? 
 C4 C5 C6 C7 -1.0(4) . . . . ? 
 C5 C6 C7 C8 -176.9(2) . . . . ? 
 C5 C6 C7 C2 2.1(4) . . . 3_646 ? 
 C6 C7 C8 C9 121.5(63) . . . . ? 
 C2 C7 C8 C9 -57.5(65) 3_646 . . . ? 
 C7 C8 C9 C10 52.8(102) . . . . ? 
 C8 C9 C10 O1 36.4(57) . . . . ? 
 C8 C9 C10 C11 -84.7(56) . . . . ? 
 C8 C9 C10 C17 152.6(55) . . . . ? 
 O1 C10 C11 C16 -114.5(2) . . . . ? 
 C9 C10 C11 C16 6.2(3) . . . . ? 
 C17 C10 C11 C16 127.9(2) . . . . ? 
 O1 C10 C11 C12 62.5(3) . . . . ? 
 C9 C10 C11 C12 -176.7(2) . . . . ? 
 C17 C10 C11 C12 -55.0(3) . . . . ? 
 C16 C11 C12 C13 0.8(4) . . . . ? 
 C10 C11 C12 C13 -176.4(2) . . . . ? 
 C11 C12 C13 C14 -1.0(4) . . . . ? 
 C12 C13 C14 C15 0.5(5) . . . . ? 
 C13 C14 C15 C16 0.1(5) . . . . ? 
 C12 C11 C16 C15 -0.2(4) . . . . ? 
 C10 C11 C16 C15 176.9(3) . . . . ? 
 C14 C15 C16 C11 -0.2(5) . . . . ? 
 O1 C10 C17 C22 -2.5(3) . . . . ? 
 C9 C10 C17 C22 -120.2(3) . . . . ? 
 C11 C10 C17 C22 116.9(3) . . . . ? 
 O1 C10 C17 C18 177.7(2) . . . . ? 
 C9 C10 C17 C18 60.0(3) . . . . ? 
 C11 C10 C17 C18 -62.9(3) . . . . ? 
 C22 C17 C18 C19 -0.8(4) . . . . ? 
 C10 C17 C18 C19 179.0(3) . . . . ? 
 C17 C18 C19 C20 1.3(5) . . . . ? 
 C18 C19 C20 C21 -1.1(6) . . . . ? 
 C19 C20 C21 C22 0.5(6) . . . . ? 
 C18 C17 C22 C21 0.1(5) . . . . ? 
 C10 C17 C22 C21 -179.7(3) . . . . ? 
 C20 C21 C22 C17 0.0(6) . . . . ? 
 
_refine_diff_density_max     .471 
_refine_diff_density_min    -.382 
_refine_diff_density_rms     .042 
 


data_1b.acetone #(1:2) 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C25 H19 O2' 
_chemical_formula_weight          351.40 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'    .0033    .0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'    .0000    .0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'    .0106    .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                    8.4000(10) 
_cell_length_b                    8.8800(10) 
_cell_length_c                    13.450(2) 
_cell_angle_alpha                 82.33(2) 
_cell_angle_beta                  71.63(2) 
_cell_angle_gamma                 76.64(2) 
_cell_volume                      924.4(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     102(2) 
_cell_measurement_reflns_used     5000
_cell_measurement_theta_min       4.7
_cell_measurement_theta_max       51.8
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             yellow
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.32
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.263 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              370 
_exptl_absorpt_coefficient_mu     0.079 
_exptl_absorpt_correction_type    'no abs corr'
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoKa  
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'STOE IDPS (Stoe &Cie, GmbH)'
_diffrn_measurement_method        'image plate'
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5935 
_diffrn_reflns_av_R_equivalents   0.0222 
_diffrn_reflns_av_sigmaI/netI     0.0318 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          2.61 
_diffrn_reflns_theta_max          26.09 
_reflns_number_total              3331 
_reflns_number_observed           2689 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0660P)^2^+0.0470P] 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     ? 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3328 
_refine_ls_number_parameters      265 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0462 
_refine_ls_R_factor_obs           0.0348 
_refine_ls_wR_factor_all          0.1002 
_refine_ls_wR_factor_obs          0.0923 
_refine_ls_goodness_of_fit_all    1.052 
_refine_ls_goodness_of_fit_obs    1.097 
_refine_ls_restrained_S_all       1.060 
_refine_ls_restrained_S_obs       1.097 
_refine_ls_shift/esd_max          0.048 
_refine_ls_shift/esd_mean         0.003 
 
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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
O1 O 0.39740(11) 0.47969(10) 0.69211(6) 0.0138(2) Uani 1 d . . 
H1O H 0.47974(11) 0.50091(10) 0.64029(6) 0.037(5) Uiso 1 d R . 
C1 C 0.8621(2) 0.12610(14) 0.52783(9) 0.0118(3) Uani 1 d . . 
H1 H 0.7689(2) 0.21138(14) 0.54659(9) 0.020(4) Uiso 1 calc R . 
C2 C 0.94751(15) 0.05688(14) 0.60160(9) 0.0107(3) Uani 1 d . . 
C3 C 0.9109(2) 0.07255(13) 0.42662(9) 0.0115(3) Uani 1 d . . 
C4 C 0.8223(2) 0.14195(14) 0.35115(10) 0.0140(3) Uani 1 d . . 
H4 H 0.7308(2) 0.22889(14) 0.36863(10) 0.019(4) Uiso 1 calc R . 
C5 C 1.1323(2) -0.08469(15) 0.74543(10) 0.0151(3) Uani 1 d . . 
H5 H 1.1943(2) -0.13038(15) 0.79369(10) 0.017(4) Uiso 1 calc R . 
C6 C 0.9925(2) 0.04304(14) 0.77434(9) 0.0140(3) Uani 1 d . . 
H6 H 0.9628(2) 0.08177(14) 0.84171(9) 0.020(4) Uiso 1 calc R . 
C7 C 0.89979(15) 0.11129(14) 0.70620(9) 0.0116(3) Uani 1 d . . 
C8 C 0.7518(2) 0.23542(14) 0.73703(9) 0.0114(3) Uani 1 d . . 
C9 C 0.6268(2) 0.33715(14) 0.75727(9) 0.0119(3) Uani 1 d . . 
C10 C 0.46703(15) 0.45785(14) 0.77905(9) 0.0114(3) Uani 1 d . . 
C11 C 0.3358(2) 0.41093(14) 0.87966(9) 0.0125(3) Uani 1 d . . 
C12 C 0.2603(2) 0.28305(15) 0.89975(10) 0.0157(3) Uani 1 d . . 
H12 H 0.2836(2) 0.21325(15) 0.84686(10) 0.024(4) Uiso 1 calc R . 
C13 C 0.1485(2) 0.2587(2) 1.00013(10) 0.0199(3) Uani 1 d . . 
H13 H 0.0947(2) 0.1717(2) 1.01560(10) 0.024(4) Uiso 1 calc R . 
C14 C 0.1157(2) 0.3619(2) 1.07757(10) 0.0203(3) Uani 1 d . . 
H14 H 0.0412(2) 0.3431(2) 1.14554(10) 0.028(4) Uiso 1 calc R . 
C15 C 0.1903(2) 0.4914(2) 1.05679(10) 0.0174(3) Uani 1 d . . 
H15 H 0.1666(2) 0.5613(2) 1.10965(10) 0.029(4) Uiso 1 calc R . 
C16 C 0.3008(2) 0.51691(14) 0.95659(9) 0.0134(3) Uani 1 d . . 
C17 C 0.3955(2) 0.64233(15) 0.91085(9) 0.0135(3) Uani 1 d . . 
C18 C 0.3984(2) 0.77866(15) 0.95136(10) 0.0168(3) Uani 1 d . . 
H18 H 0.3346(2) 0.80102(15) 1.02169(10) 0.024(4) Uiso 1 calc R . 
C19 C 0.4962(2) 0.8807(2) 0.88695(11) 0.0194(3) Uani 1 d . . 
H19 H 0.4978(2) 0.9740(2) 0.91367(11) 0.022(4) Uiso 1 calc R . 
C20 C 0.5924(2) 0.8489(2) 0.78360(11) 0.0197(3) Uani 1 d . . 
H20 H 0.6576(2) 0.9206(2) 0.74072(11) 0.030(4) Uiso 1 calc R . 
C21 C 0.5925(2) 0.71123(15) 0.74326(10) 0.0161(3) Uani 1 d . . 
H21 H 0.6589(2) 0.68770(15) 0.67355(10) 0.023(4) Uiso 1 calc R . 
C22 C 0.4940(2) 0.61043(14) 0.80696(9) 0.0116(3) Uani 1 d . . 
O1A O 0.68274(12) 0.50648(11) 0.51733(7) 0.0194(2) Uani 1 d . . 
C1A C 0.7528(2) 0.5950(2) 0.44865(10) 0.0161(3) Uani 1 d . . 
C2A C 0.9263(2) 0.5391(2) 0.37285(11) 0.0239(3) Uani 1 d . . 
H2AA H 1.0125(3) 0.5817(10) 0.3889(5) 0.032(4) Uiso 1 calc R . 
H2AB H 0.9237(4) 0.5739(11) 0.30098(13) 0.039(5) Uiso 1 calc R . 
H2AC H 0.9554(6) 0.4256(2) 0.3794(6) 0.043(5) Uiso 1 calc R . 
C3A C 0.6729(2) 0.7642(2) 0.43870(11) 0.0243(3) Uani 1 d . . 
H3AA H 0.6677(15) 0.7926(4) 0.3667(3) 0.061(6) Uiso 1 calc R . 
H3AB H 0.7421(9) 0.8266(2) 0.4554(10) 0.064(7) Uiso 1 calc R . 
H3AC H 0.5568(6) 0.7836(3) 0.4875(7) 0.054(6) Uiso 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 0.0142(4) 0.0175(4) 0.0097(4) -0.0014(3) -0.0044(4) -0.0020(4) 
C1 0.0095(6) 0.0083(6) 0.0152(6) -0.0006(5) -0.0009(5) -0.0013(5) 
C2 0.0093(6) 0.0086(6) 0.0127(6) -0.0001(5) 0.0002(5) -0.0039(5) 
C3 0.0101(6) 0.0076(6) 0.0152(6) 0.0000(5) -0.0014(5) -0.0027(5) 
C4 0.0112(6) 0.0105(6) 0.0172(6) 0.0001(5) -0.0019(5) -0.0003(5) 
C5 0.0151(6) 0.0151(6) 0.0142(6) 0.0020(5) -0.0048(5) -0.0023(5) 
C6 0.0148(6) 0.0146(6) 0.0110(6) -0.0012(5) -0.0013(5) -0.0033(5) 
C7 0.0101(6) 0.0084(6) 0.0137(6) -0.0005(5) 0.0010(5) -0.0037(5) 
C8 0.0128(6) 0.0120(6) 0.0096(5) -0.0003(5) -0.0021(5) -0.0052(5) 
C9 0.0142(6) 0.0129(6) 0.0090(5) -0.0009(5) -0.0021(5) -0.0051(5) 
C10 0.0115(6) 0.0124(6) 0.0095(6) -0.0015(5) -0.0035(5) 0.0000(5) 
C11 0.0100(6) 0.0131(6) 0.0113(6) -0.0001(5) -0.0027(5) 0.0026(5) 
C12 0.0144(6) 0.0151(6) 0.0164(6) 0.0004(5) -0.0044(5) -0.0014(5) 
C13 0.0170(7) 0.0203(7) 0.0203(7) 0.0061(5) -0.0041(5) -0.0056(6) 
C14 0.0147(6) 0.0277(8) 0.0123(6) 0.0041(5) 0.0000(5) -0.0004(6) 
C15 0.0146(6) 0.0225(7) 0.0111(6) -0.0014(5) -0.0026(5) 0.0026(6) 
C16 0.0103(6) 0.0153(6) 0.0117(6) -0.0012(5) -0.0037(5) 0.0036(5) 
C17 0.0113(6) 0.0151(6) 0.0122(6) -0.0020(5) -0.0048(5) 0.0033(5) 
C18 0.0194(7) 0.0170(6) 0.0138(6) -0.0063(5) -0.0077(5) 0.0038(6) 
C19 0.0250(7) 0.0140(6) 0.0228(7) -0.0060(5) -0.0129(6) 0.0000(6) 
C20 0.0230(7) 0.0164(7) 0.0225(7) -0.0002(5) -0.0092(6) -0.0065(6) 
C21 0.0160(6) 0.0168(6) 0.0149(6) -0.0019(5) -0.0036(5) -0.0031(6) 
C22 0.0108(6) 0.0112(6) 0.0125(6) -0.0021(5) -0.0051(5) 0.0015(5) 
O1A 0.0219(5) 0.0207(5) 0.0134(4) 0.0010(4) -0.0015(4) -0.0067(4) 
C1A 0.0174(6) 0.0205(7) 0.0134(6) -0.0027(5) -0.0053(5) -0.0079(6) 
C2A 0.0180(7) 0.0267(8) 0.0249(7) -0.0037(6) 0.0007(6) -0.0090(6) 
C3A 0.0275(8) 0.0184(7) 0.0248(7) -0.0010(6) -0.0018(6) -0.0088(6) 
 
_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 C10 1.4371(14) . ? 
O1 H1O 0.85 . ? 
C1 C2 1.400(2) . ? 
C1 C3 1.407(2) . ? 
C1 H1 0.95 . ? 
C2 C3 1.442(2) 2_756 ? 
C2 C7 1.453(2) . ? 
C3 C4 1.436(2) . ? 
C3 C2 1.442(2) 2_756 ? 
C4 C5 1.366(2) 2_756 ? 
C4 H4 0.95 . ? 
C5 C4 1.366(2) 2_756 ? 
C5 C6 1.425(2) . ? 
C5 H5 0.95 . ? 
C6 C7 1.378(2) . ? 
C6 H6 0.95 . ? 
C7 C8 1.448(2) . ? 
C8 C9 1.200(2) . ? 
C9 C10 1.485(2) . ? 
C10 C11 1.530(2) . ? 
C10 C22 1.536(2) . ? 
C11 C12 1.381(2) . ? 
C11 C16 1.408(2) . ? 
C12 C13 1.403(2) . ? 
C12 H12 0.95 . ? 
C13 C14 1.399(2) . ? 
C13 H13 0.95 . ? 
C14 C15 1.389(2) . ? 
C14 H14 0.95 . ? 
C15 C16 1.399(2) . ? 
C15 H15 0.95 . ? 
C16 C17 1.473(2) . ? 
C17 C18 1.400(2) . ? 
C17 C22 1.409(2) . ? 
C18 C19 1.390(2) . ? 
C18 H18 0.95 . ? 
C19 C20 1.399(2) . ? 
C19 H19 0.95 . ? 
C20 C21 1.401(2) . ? 
C20 H20 0.95 . ? 
C21 C22 1.382(2) . ? 
C21 H21 0.95 . ? 
O1A C1A 1.222(2) . ? 
C1A C3A 1.505(2) . ? 
C1A C2A 1.508(2) . ? 
C2A H2AA 0.98 . ? 
C2A H2AB 0.98 . ? 
C2A H2AC 0.98 . ? 
C3A H3AA 0.98 . ? 
C3A H3AB 0.98 . ? 
C3A H3AC 0.98 . ? 
 
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 
C10 O1 H1O 103.20(6) . . ? 
C2 C1 C3 121.64(11) . . ? 
C2 C1 H1 119.18(7) . . ? 
C3 C1 H1 119.18(7) . . ? 
C1 C2 C3 119.34(11) . 2_756 ? 
C1 C2 C7 122.41(10) . . ? 
C3 C2 C7 118.25(11) 2_756 . ? 
C1 C3 C4 121.82(10) . . ? 
C1 C3 C2 119.02(11) . 2_756 ? 
C4 C3 C2 119.15(11) . 2_756 ? 
C5 C4 C3 120.91(11) 2_756 . ? 
C5 C4 H4 119.54(7) 2_756 . ? 
C3 C4 H4 119.55(7) . . ? 
C4 C5 C6 120.50(11) 2_756 . ? 
C4 C5 H5 119.75(7) 2_756 . ? 
C6 C5 H5 119.75(7) . . ? 
C7 C6 C5 121.07(11) . . ? 
C7 C6 H6 119.46(7) . . ? 
C5 C6 H6 119.46(7) . . ? 
C6 C7 C8 121.43(11) . . ? 
C6 C7 C2 120.06(10) . . ? 
C8 C7 C2 118.50(10) . . ? 
C9 C8 C7 176.06(12) . . ? 
C8 C9 C10 176.46(13) . . ? 
O1 C10 C9 109.89(9) . . ? 
O1 C10 C11 110.08(10) . . ? 
C9 C10 C11 110.29(10) . . ? 
O1 C10 C22 112.26(10) . . ? 
C9 C10 C22 112.21(10) . . ? 
C11 C10 C22 101.86(9) . . ? 
C12 C11 C16 121.56(12) . . ? 
C12 C11 C10 128.09(11) . . ? 
C16 C11 C10 110.33(11) . . ? 
C11 C12 C13 118.43(12) . . ? 
C11 C12 H12 120.79(7) . . ? 
C13 C12 H12 120.79(8) . . ? 
C12 C13 C14 120.29(13) . . ? 
C12 C13 H13 119.85(8) . . ? 
C14 C13 H13 119.85(8) . . ? 
C15 C14 C13 121.16(12) . . ? 
C15 C14 H14 119.42(8) . . ? 
C13 C14 H14 119.42(8) . . ? 
C14 C15 C16 118.77(12) . . ? 
C14 C15 H15 120.61(8) . . ? 
C16 C15 H15 120.61(8) . . ? 
C15 C16 C11 119.78(13) . . ? 
C15 C16 C17 131.44(12) . . ? 
C11 C16 C17 108.78(11) . . ? 
C18 C17 C22 119.41(13) . . ? 
C18 C17 C16 131.79(11) . . ? 
C22 C17 C16 108.78(11) . . ? 
C19 C18 C17 118.88(12) . . ? 
C19 C18 H18 120.56(7) . . ? 
C17 C18 H18 120.56(8) . . ? 
C18 C19 C20 121.32(12) . . ? 
C18 C19 H19 119.34(7) . . ? 
C20 C19 H19 119.34(9) . . ? 
C21 C20 C19 120.05(14) . . ? 
C21 C20 H20 119.98(8) . . ? 
C19 C20 H20 119.98(9) . . ? 
C22 C21 C20 118.64(12) . . ? 
C22 C21 H21 120.68(7) . . ? 
C20 C21 H21 120.68(8) . . ? 
C21 C22 C17 121.68(12) . . ? 
C21 C22 C10 128.14(11) . . ? 
C17 C22 C10 110.13(11) . . ? 
O1A C1A C3A 121.59(12) . . ? 
O1A C1A C2A 120.93(12) . . ? 
C3A C1A C2A 117.44(13) . . ? 
C1A C2A H2AA 109.47(8) . . ? 
C1A C2A H2AB 109.47(8) . . ? 
H2AA C2A H2AB 109.5 . . ? 
C1A C2A H2AC 109.47(8) . . ? 
H2AA C2A H2AC 109.5 . . ? 
H2AB C2A H2AC 109.5 . . ? 
C1A C3A H3AA 109.47(7) . . ? 
C1A C3A H3AB 109.47(8) . . ? 
H3AA C3A H3AB 109.5 . . ? 
C1A C3A H3AC 109.47(8) . . ? 
H3AA C3A H3AC 109.5 . . ? 
H3AB C3A H3AC 109.5 . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
 C3 C1 C2 C3 0.0(2) . . . 2_756 ? 
 C3 C1 C2 C7 179.54(12) . . . . ? 
 C2 C1 C3 C4 179.20(12) . . . . ? 
 C2 C1 C3 C2 0.0(2) . . . 2_756 ? 
 C1 C3 C4 C5 -177.64(13) . . . 2_756 ? 
 C2 C3 C4 C5 1.6(2) 2_756 . . 2_756 ? 
 C4 C5 C6 C7 0.3(2) 2_756 . . . ? 
 C5 C6 C7 C8 176.52(12) . . . . ? 
 C5 C6 C7 C2 -2.2(2) . . . . ? 
 C1 C2 C7 C6 -177.35(12) . . . . ? 
 C3 C2 C7 C6 2.2(2) 2_756 . . . ? 
 C1 C2 C7 C8 3.9(2) . . . . ? 
 C3 C2 C7 C8 -176.57(11) 2_756 . . . ? 
 C6 C7 C8 C9 -167.7(19) . . . . ? 
 C2 C7 C8 C9 11.1(20) . . . . ? 
 C7 C8 C9 C10 30.9(36) . . . . ? 
 C8 C9 C10 O1 -36.7(20) . . . . ? 
 C8 C9 C10 C11 84.9(20) . . . . ? 
 C8 C9 C10 C22 -162.3(20) . . . . ? 
 O1 C10 C11 C12 59.34(15) . . . . ? 
 C9 C10 C11 C12 -62.1(2) . . . . ? 
 C22 C10 C11 C12 178.62(11) . . . . ? 
 O1 C10 C11 C16 -122.46(10) . . . . ? 
 C9 C10 C11 C16 116.12(11) . . . . ? 
 C22 C10 C11 C16 -3.18(12) . . . . ? 
 C16 C11 C12 C13 -1.0(2) . . . . ? 
 C10 C11 C12 C13 177.01(11) . . . . ? 
 C11 C12 C13 C14 -0.3(2) . . . . ? 
 C12 C13 C14 C15 1.0(2) . . . . ? 
 C13 C14 C15 C16 -0.5(2) . . . . ? 
 C14 C15 C16 C11 -0.8(2) . . . . ? 
 C14 C15 C16 C17 178.95(12) . . . . ? 
 C12 C11 C16 C15 1.5(2) . . . . ? 
 C10 C11 C16 C15 -176.79(10) . . . . ? 
 C12 C11 C16 C17 -178.23(10) . . . . ? 
 C10 C11 C16 C17 3.44(13) . . . . ? 
 C15 C16 C17 C18 -3.6(2) . . . . ? 
 C11 C16 C17 C18 176.17(12) . . . . ? 
 C15 C16 C17 C22 178.04(12) . . . . ? 
 C11 C16 C17 C22 -2.22(13) . . . . ? 
 C22 C17 C18 C19 1.3(2) . . . . ? 
 C16 C17 C18 C19 -176.97(12) . . . . ? 
 C17 C18 C19 C20 -0.7(2) . . . . ? 
 C18 C19 C20 C21 -0.5(2) . . . . ? 
 C19 C20 C21 C22 1.1(2) . . . . ? 
 C20 C21 C22 C17 -0.5(2) . . . . ? 
 C20 C21 C22 C10 176.88(11) . . . . ? 
 C18 C17 C22 C21 -0.7(2) . . . . ? 
 C16 C17 C22 C21 177.91(10) . . . . ? 
 C18 C17 C22 C10 -178.50(10) . . . . ? 
 C16 C17 C22 C10 0.13(13) . . . . ? 
 O1 C10 C22 C21 -58.1(2) . . . . ? 
 C9 C10 C22 C21 66.3(2) . . . . ? 
 C11 C10 C22 C21 -175.81(11) . . . . ? 
 O1 C10 C22 C17 119.51(10) . . . . ? 
 C9 C10 C22 C17 -116.15(11) . . . . ? 
 C11 C10 C22 C17 1.79(12) . . . . ? 
 
_refine_diff_density_max     .208 
_refine_diff_density_min    -.204 
_refine_diff_density_rms     .043