# Supplementary Material (ESI) for Green Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1048/2 data_b000825G _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,7,12,-trimethoxy-3,8,13-tri(prop-1-enoxy)-10,15-dihydro-5H-tribenzo [a,d,g]cyclononene ; _chemical_name_common tris-(O-allyl)CTV _chemical_melting_point ? _chemical_formula_moiety 'C33 H36 O6' _chemical_formula_sum 'C33 H36 O6' _chemical_formula_weight 528.62 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 monoclinic _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 14.4429(5) _cell_length_b 8.0609(3) _cell_length_c 24.3908(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.510(2) _cell_angle_gamma 90.00 _cell_volume 2800.62(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _exptl_crystal_description 'needles' _exptl_crystal_colour 'clear, colourless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9749 _exptl_absorpt_correction_T_max 0.9915 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Enraf-nonius Kappa CCD diffractometer' _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 21634 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.82 _reflns_number_total 6441 _reflns_number_gt 3817 _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 'ORTEP-3 for Windows v 1.05' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+2.8101P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6441 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1360 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1946 _refine_ls_wR_factor_gt 0.1581 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 O1 O 0.48371(14) 0.3523(2) 0.04854(8) 0.0246(4) Uani 1 1 d . . . O2 O 0.10886(14) -0.3217(2) 0.25460(8) 0.0269(5) Uani 1 1 d . . . O3 O 0.03486(14) -0.1301(2) 0.16339(8) 0.0278(5) Uani 1 1 d . . . O4 O 0.30112(14) 0.3431(2) 0.02747(9) 0.0288(5) Uani 1 1 d . . . O5 O 0.55816(15) -0.1671(3) 0.33383(8) 0.0312(5) Uani 1 1 d . . . O6 O 0.66718(14) -0.0128(3) 0.27702(8) 0.0290(5) Uani 1 1 d . . . C7 C 0.46371(19) -0.3312(3) 0.19290(11) 0.0203(6) Uani 1 1 d . . . C8 C 0.1571(2) -0.3156(3) 0.21052(11) 0.0222(6) Uani 1 1 d . . . C9 C 0.2995(2) 0.0461(3) 0.04691(10) 0.0213(6) Uani 1 1 d . . . H9 H 0.2330 0.0426 0.0382 0.026 Uiso 1 1 calc R . . C10 C 0.4766(2) -0.3073(3) 0.25079(11) 0.0232(6) Uani 1 1 d . . . H10 H 0.4389 -0.3686 0.2720 0.028 Uiso 1 1 calc R . . C11 C 0.29201(19) -0.2589(3) 0.06555(10) 0.0196(6) Uani 1 1 d . . . H11A H 0.2413 -0.2606 0.0328 0.023 Uiso 1 1 calc R . . H11B H 0.3334 -0.3550 0.0622 0.023 Uiso 1 1 calc R . . C12 C 0.2900(2) -0.3753(3) 0.16342(11) 0.0205(6) Uani 1 1 d . . . C13 C 0.49228(19) 0.0556(3) 0.07046(10) 0.0200(6) Uani 1 1 d . . . H13 H 0.5589 0.0587 0.0780 0.024 Uiso 1 1 calc R . . C14 C 0.34513(19) 0.1955(3) 0.04309(10) 0.0207(6) Uani 1 1 d . . . C15 C 0.51958(19) -0.2415(3) 0.16215(11) 0.0195(6) Uani 1 1 d . . . C16 C 0.2422(2) -0.3919(3) 0.20849(11) 0.0221(6) Uani 1 1 d . . . H16 H 0.2694 -0.4585 0.2391 0.026 Uiso 1 1 calc R . . C17 C 0.16204(19) -0.2069(3) 0.11945(11) 0.0208(6) Uani 1 1 d . . . H17 H 0.1334 -0.1438 0.0883 0.025 Uiso 1 1 calc R . . C18 C 0.24832(19) -0.2814(3) 0.11728(10) 0.0196(6) Uani 1 1 d . . . C19 C 0.5061(2) -0.2424(3) 0.09881(11) 0.0211(6) Uani 1 1 d . . . H19A H 0.5680 -0.2367 0.0865 0.025 Uiso 1 1 calc R . . H19B H 0.4749 -0.3467 0.0844 0.025 Uiso 1 1 calc R . . C20 C 0.60045(19) -0.1117(3) 0.24673(11) 0.0230(6) Uani 1 1 d . . . C21 C 0.34900(19) -0.1006(3) 0.06334(10) 0.0187(6) Uani 1 1 d . . . C22 C 0.1161(2) -0.2201(3) 0.16462(11) 0.0223(6) Uani 1 1 d . . . C23 C 0.44641(19) -0.0946(3) 0.07593(10) 0.0189(6) Uani 1 1 d . . . C24 C 0.5418(2) -0.1987(3) 0.27758(11) 0.0242(6) Uani 1 1 d . . . C25 C 0.38682(19) -0.4516(3) 0.16774(11) 0.0226(6) Uani 1 1 d . . . H25A H 0.3976 -0.4849 0.1302 0.027 Uiso 1 1 calc R . . H25B H 0.3901 -0.5526 0.1911 0.027 Uiso 1 1 calc R . . C26 C 0.4435(2) 0.2000(3) 0.05443(10) 0.0208(6) Uani 1 1 d . . . C27 C 0.58795(19) -0.1335(3) 0.18972(11) 0.0221(6) Uani 1 1 d . . . H27 H 0.6267 -0.0737 0.1687 0.026 Uiso 1 1 calc R . . C28 C 0.2025(2) 0.3478(4) 0.02698(15) 0.0348(7) Uani 1 1 d . . . H28A H 0.1710 0.2741 -0.0022 0.052 Uiso 1 1 calc R . . H28B H 0.1796 0.4614 0.0197 0.052 Uiso 1 1 calc R . . H28C H 0.1889 0.3111 0.0631 0.052 Uiso 1 1 calc R . . C29 C 0.5820(2) 0.3582(4) 0.04713(12) 0.0271(6) Uani 1 1 d . . . H29A H 0.5955 0.4589 0.0266 0.033 Uiso 1 1 calc R . . H29B H 0.5991 0.2608 0.0262 0.033 Uiso 1 1 calc R . . C30 C -0.1302(2) -0.1379(5) 0.14194(14) 0.0371(8) Uani 1 1 d . . . H30 H -0.1333 -0.0203 0.1398 0.044 Uiso 1 1 calc R . . C31 C 0.6420(2) 0.3597(4) 0.10277(14) 0.0310(7) Uani 1 1 d . . . H31 H 0.6228 0.4164 0.1332 0.037 Uiso 1 1 calc R . . C32 C 0.1504(2) -0.4146(4) 0.30255(12) 0.0326(7) Uani 1 1 d . . . H32A H 0.1607 -0.5293 0.2916 0.049 Uiso 1 1 calc R . . H32B H 0.1082 -0.4137 0.3302 0.049 Uiso 1 1 calc R . . H32C H 0.2106 -0.3644 0.3186 0.049 Uiso 1 1 calc R . . C33 C 0.4861(2) -0.2131(4) 0.36497(11) 0.0279(6) Uani 1 1 d . . . H33A H 0.4787 -0.3352 0.3652 0.033 Uiso 1 1 calc R . . H33B H 0.4254 -0.1629 0.3483 0.033 Uiso 1 1 calc R . . C34 C -0.0474(2) -0.2130(4) 0.17724(13) 0.0306(7) Uani 1 1 d . . . H34A H -0.0511 -0.1971 0.2171 0.037 Uiso 1 1 calc R . . H34B H -0.0445 -0.3334 0.1698 0.037 Uiso 1 1 calc R . . C35 C 0.5161(2) -0.1505(4) 0.42241(12) 0.0349(7) Uani 1 1 d . . . H35 H 0.5276 -0.0350 0.4273 0.042 Uiso 1 1 calc R . . C36 C 0.7274(3) 0.0755(5) 0.24742(14) 0.0546(11) Uani 1 1 d . . . H36A H 0.7604 -0.0026 0.2267 0.082 Uiso 1 1 calc R . . H36B H 0.7733 0.1381 0.2736 0.082 Uiso 1 1 calc R . . H36C H 0.6904 0.1525 0.2215 0.082 Uiso 1 1 calc R . . C37 C -0.1993(3) -0.2221(6) 0.11359(16) 0.0534(10) Uani 1 1 d . . . H37A H -0.1985 -0.3399 0.1148 0.064 Uiso 1 1 calc R . . H37B H -0.2502 -0.1656 0.0918 0.064 Uiso 1 1 calc R . . C38 C 0.5275(2) -0.2443(5) 0.46664(14) 0.0496(10) Uani 1 1 d . . . H38A H 0.5165 -0.3603 0.4631 0.059 Uiso 1 1 calc R . . H38B H 0.5469 -0.1966 0.5023 0.059 Uiso 1 1 calc R . . C39 C 0.7221(3) 0.2807(6) 0.10867(18) 0.0599(11) Uani 1 1 d . . . H39A H 0.7403 0.2247 0.0779 0.072 Uiso 1 1 calc R . . H39B H 0.7621 0.2794 0.1437 0.072 Uiso 1 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 0.0283(10) 0.0153(10) 0.0304(10) 0.0026(8) 0.0055(9) -0.0052(8) O2 0.0338(11) 0.0293(11) 0.0193(9) 0.0034(8) 0.0099(8) -0.0010(9) O3 0.0269(11) 0.0228(11) 0.0364(11) 0.0030(9) 0.0130(9) 0.0010(8) O4 0.0285(11) 0.0175(10) 0.0396(12) 0.0050(8) 0.0037(9) 0.0012(8) O5 0.0329(12) 0.0422(13) 0.0194(10) 0.0000(9) 0.0067(9) -0.0099(10) O6 0.0285(11) 0.0327(12) 0.0260(10) -0.0015(9) 0.0052(9) -0.0101(9) C7 0.0227(14) 0.0153(13) 0.0233(13) 0.0016(10) 0.0053(11) 0.0029(11) C8 0.0306(15) 0.0185(13) 0.0197(13) -0.0023(10) 0.0109(11) -0.0067(11) C9 0.0253(14) 0.0202(14) 0.0186(12) -0.0001(10) 0.0044(11) -0.0013(11) C10 0.0263(14) 0.0225(14) 0.0213(13) 0.0069(11) 0.0057(11) -0.0017(11) C11 0.0248(14) 0.0175(13) 0.0166(12) -0.0006(10) 0.0042(11) -0.0013(11) C12 0.0286(15) 0.0127(13) 0.0205(13) -0.0013(10) 0.0047(11) -0.0054(11) C13 0.0244(14) 0.0196(14) 0.0169(12) -0.0012(10) 0.0058(11) -0.0025(11) C14 0.0287(15) 0.0149(13) 0.0185(12) 0.0018(10) 0.0043(11) 0.0010(11) C15 0.0221(13) 0.0152(13) 0.0211(13) 0.0018(10) 0.0032(11) 0.0039(11) C16 0.0307(15) 0.0173(14) 0.0180(12) 0.0001(10) 0.0034(11) -0.0027(11) C17 0.0268(14) 0.0167(13) 0.0188(12) 0.0020(10) 0.0037(11) -0.0045(11) C18 0.0258(14) 0.0140(13) 0.0193(12) -0.0015(10) 0.0046(11) -0.0038(11) C19 0.0263(14) 0.0156(13) 0.0232(13) -0.0008(10) 0.0088(11) -0.0007(11) C20 0.0238(14) 0.0207(14) 0.0246(14) 0.0003(11) 0.0047(12) -0.0008(11) C21 0.0285(14) 0.0151(13) 0.0140(12) -0.0002(9) 0.0075(11) -0.0037(11) C22 0.0269(15) 0.0158(13) 0.0247(14) -0.0028(10) 0.0060(12) -0.0008(11) C23 0.0280(15) 0.0167(13) 0.0139(11) -0.0019(10) 0.0089(11) -0.0008(11) C24 0.0283(15) 0.0252(15) 0.0192(13) 0.0017(11) 0.0041(11) 0.0022(12) C25 0.0316(15) 0.0147(13) 0.0222(13) 0.0036(10) 0.0063(12) -0.0013(11) C26 0.0301(15) 0.0164(13) 0.0166(12) -0.0002(10) 0.0062(11) -0.0041(11) C27 0.0238(14) 0.0199(14) 0.0230(13) 0.0040(11) 0.0054(11) 0.0009(11) C28 0.0277(16) 0.0226(16) 0.053(2) 0.0021(14) 0.0016(15) 0.0019(13) C29 0.0329(16) 0.0185(14) 0.0344(15) 0.0003(12) 0.0183(13) -0.0038(12) C30 0.0288(17) 0.045(2) 0.0395(17) 0.0023(15) 0.0123(14) 0.0030(15) C31 0.0245(15) 0.0217(15) 0.0466(18) -0.0004(13) 0.0049(14) -0.0018(12) C32 0.0443(19) 0.0335(17) 0.0211(14) 0.0064(12) 0.0092(13) -0.0018(14) C33 0.0288(15) 0.0327(16) 0.0229(14) 0.0016(12) 0.0065(12) -0.0037(13) C34 0.0287(16) 0.0331(17) 0.0332(16) 0.0023(13) 0.0145(13) -0.0038(13) C35 0.0347(18) 0.0441(19) 0.0275(15) -0.0035(14) 0.0101(14) -0.0041(15) C36 0.061(3) 0.071(3) 0.0342(18) -0.0099(18) 0.0136(18) -0.045(2) C37 0.036(2) 0.076(3) 0.049(2) 0.005(2) 0.0088(17) -0.0069(19) C38 0.039(2) 0.080(3) 0.0286(17) 0.0058(18) 0.0041(15) -0.0025(19) C39 0.048(2) 0.077(3) 0.053(2) 0.006(2) 0.003(2) -0.004(2) _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 C26 1.376(3) . ? O1 C29 1.426(3) . ? O2 C8 1.375(3) . ? O2 C32 1.434(3) . ? O3 C22 1.375(3) . ? O3 C34 1.450(4) . ? O4 C14 1.373(3) . ? O4 C28 1.423(4) . ? O5 C24 1.377(3) . ? O5 C33 1.435(4) . ? O6 C20 1.369(3) . ? O6 C36 1.412(4) . ? C7 C15 1.392(4) . ? C7 C10 1.407(4) . ? C7 C25 1.525(4) . ? C8 C16 1.383(4) . ? C8 C22 1.406(4) . ? C9 C14 1.383(4) . ? C9 C21 1.405(4) . ? C10 C24 1.370(4) . ? C11 C18 1.512(4) . ? C11 C21 1.524(4) . ? C12 C16 1.397(4) . ? C12 C18 1.407(4) . ? C12 C25 1.516(4) . ? C13 C26 1.383(4) . ? C13 C23 1.397(4) . ? C14 C26 1.402(4) . ? C15 C27 1.402(4) . ? C15 C19 1.525(4) . ? C17 C22 1.381(4) . ? C17 C18 1.392(4) . ? C19 C23 1.522(4) . ? C20 C27 1.384(4) . ? C20 C24 1.410(4) . ? C21 C23 1.390(4) . ? C29 C31 1.485(4) . ? C30 C37 1.306(5) . ? C30 C34 1.483(4) . ? C31 C39 1.307(5) . ? C33 C35 1.485(4) . ? C35 C38 1.306(5) . ? 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 C26 O1 C29 118.1(2) . . ? C8 O2 C32 117.3(2) . . ? C22 O3 C34 118.7(2) . . ? C14 O4 C28 116.2(2) . . ? C24 O5 C33 117.3(2) . . ? C20 O6 C36 117.1(2) . . ? C15 C7 C10 118.5(2) . . ? C15 C7 C25 124.2(2) . . ? C10 C7 C25 117.3(2) . . ? O2 C8 C16 125.5(2) . . ? O2 C8 C22 116.2(2) . . ? C16 C8 C22 118.4(2) . . ? C14 C9 C21 121.8(3) . . ? C24 C10 C7 122.2(3) . . ? C18 C11 C21 115.6(2) . . ? C16 C12 C18 118.7(3) . . ? C16 C12 C25 118.5(2) . . ? C18 C12 C25 122.8(2) . . ? C26 C13 C23 121.9(3) . . ? O4 C14 C9 124.7(3) . . ? O4 C14 C26 116.1(2) . . ? C9 C14 C26 119.2(2) . . ? C7 C15 C27 119.3(2) . . ? C7 C15 C19 123.7(2) . . ? C27 C15 C19 116.8(2) . . ? C8 C16 C12 122.9(2) . . ? C22 C17 C18 123.3(2) . . ? C17 C18 C12 118.0(2) . . ? C17 C18 C11 118.7(2) . . ? C12 C18 C11 123.4(2) . . ? C23 C19 C15 109.7(2) . . ? O6 C20 C27 125.4(3) . . ? O6 C20 C24 115.7(2) . . ? C27 C20 C24 118.9(2) . . ? C23 C21 C9 118.8(2) . . ? C23 C21 C11 123.6(2) . . ? C9 C21 C11 117.5(2) . . ? O3 C22 C17 117.5(2) . . ? O3 C22 C8 123.5(2) . . ? C17 C22 C8 118.8(2) . . ? C21 C23 C13 119.2(2) . . ? C21 C23 C19 123.0(2) . . ? C13 C23 C19 117.7(2) . . ? C10 C24 O5 125.8(3) . . ? C10 C24 C20 119.3(2) . . ? O5 C24 C20 114.8(2) . . ? C12 C25 C7 111.9(2) . . ? O1 C26 C13 125.1(3) . . ? O1 C26 C14 115.7(2) . . ? C13 C26 C14 119.1(2) . . ? C20 C27 C15 121.7(3) . . ? O1 C29 C31 114.3(2) . . ? C37 C30 C34 124.6(4) . . ? C39 C31 C29 118.0(3) . . ? O5 C33 C35 106.7(2) . . ? O3 C34 C30 106.9(2) . . ? C38 C35 C33 124.1(3) . . ? 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 C32 O2 C8 C16 0.2(4) . . . . ? C32 O2 C8 C22 -178.4(2) . . . . ? C15 C7 C10 C24 0.3(4) . . . . ? C25 C7 C10 C24 -178.1(3) . . . . ? C28 O4 C14 C9 14.0(4) . . . . ? C28 O4 C14 C26 -167.6(3) . . . . ? C21 C9 C14 O4 -179.8(2) . . . . ? C21 C9 C14 C26 1.8(4) . . . . ? C10 C7 C15 C27 1.4(4) . . . . ? C25 C7 C15 C27 179.6(2) . . . . ? C10 C7 C15 C19 -173.5(2) . . . . ? C25 C7 C15 C19 4.7(4) . . . . ? O2 C8 C16 C12 -177.1(2) . . . . ? C22 C8 C16 C12 1.4(4) . . . . ? C18 C12 C16 C8 -2.1(4) . . . . ? C25 C12 C16 C8 174.6(2) . . . . ? C22 C17 C18 C12 0.4(4) . . . . ? C22 C17 C18 C11 179.8(2) . . . . ? C16 C12 C18 C17 1.2(4) . . . . ? C25 C12 C18 C17 -175.3(2) . . . . ? C16 C12 C18 C11 -178.2(2) . . . . ? C25 C12 C18 C11 5.3(4) . . . . ? C21 C11 C18 C17 84.6(3) . . . . ? C21 C11 C18 C12 -96.0(3) . . . . ? C7 C15 C19 C23 95.4(3) . . . . ? C27 C15 C19 C23 -79.6(3) . . . . ? C36 O6 C20 C27 0.7(4) . . . . ? C36 O6 C20 C24 179.7(3) . . . . ? C14 C9 C21 C23 -0.1(4) . . . . ? C14 C9 C21 C11 -179.3(2) . . . . ? C18 C11 C21 C23 99.7(3) . . . . ? C18 C11 C21 C9 -81.1(3) . . . . ? C34 O3 C22 C17 131.9(3) . . . . ? C34 O3 C22 C8 -52.2(4) . . . . ? C18 C17 C22 O3 175.0(2) . . . . ? C18 C17 C22 C8 -1.1(4) . . . . ? O2 C8 C22 O3 3.0(4) . . . . ? C16 C8 C22 O3 -175.7(2) . . . . ? O2 C8 C22 C17 178.9(2) . . . . ? C16 C8 C22 C17 0.2(4) . . . . ? C9 C21 C23 C13 -1.7(4) . . . . ? C11 C21 C23 C13 177.4(2) . . . . ? C9 C21 C23 C19 174.6(2) . . . . ? C11 C21 C23 C19 -6.2(4) . . . . ? C26 C13 C23 C21 1.9(4) . . . . ? C26 C13 C23 C19 -174.6(2) . . . . ? C15 C19 C23 C21 -89.6(3) . . . . ? C15 C19 C23 C13 86.7(3) . . . . ? C7 C10 C24 O5 179.4(3) . . . . ? C7 C10 C24 C20 -2.3(4) . . . . ? C33 O5 C24 C10 -18.6(4) . . . . ? C33 O5 C24 C20 163.0(3) . . . . ? O6 C20 C24 C10 -176.4(2) . . . . ? C27 C20 C24 C10 2.6(4) . . . . ? O6 C20 C24 O5 2.1(4) . . . . ? C27 C20 C24 O5 -178.9(2) . . . . ? C16 C12 C25 C7 -89.2(3) . . . . ? C18 C12 C25 C7 87.4(3) . . . . ? C15 C7 C25 C12 -101.5(3) . . . . ? C10 C7 C25 C12 76.8(3) . . . . ? C29 O1 C26 C13 14.1(4) . . . . ? C29 O1 C26 C14 -166.1(2) . . . . ? C23 C13 C26 O1 179.5(2) . . . . ? C23 C13 C26 C14 -0.3(4) . . . . ? O4 C14 C26 O1 0.1(3) . . . . ? C9 C14 C26 O1 178.6(2) . . . . ? O4 C14 C26 C13 179.9(2) . . . . ? C9 C14 C26 C13 -1.5(4) . . . . ? O6 C20 C27 C15 177.9(3) . . . . ? C24 C20 C27 C15 -1.0(4) . . . . ? C7 C15 C27 C20 -1.0(4) . . . . ? C19 C15 C27 C20 174.2(2) . . . . ? C26 O1 C29 C31 -83.6(3) . . . . ? O1 C29 C31 C39 144.3(3) . . . . ? C24 O5 C33 C35 -174.1(2) . . . . ? C22 O3 C34 C30 -145.5(3) . . . . ? C37 C30 C34 O3 132.7(4) . . . . ? O5 C33 C35 C38 -122.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.693 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.071