data_cu_rxd3_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H54 O4' _chemical_formula_sum 'C34 H54 O4' _chemical_formula_weight 526.77 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 9.3781(2) _cell_length_b 12.6568(3) _cell_length_c 27.0482(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3210.53(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9954 _cell_measurement_theta_min 5.87 _cell_measurement_theta_max 69.17 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.84 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6613 _exptl_absorpt_correction_T_max 0.7942 _exptl_absorpt_process_details 'sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12272 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 5.87 _diffrn_reflns_theta_max 69.38 _reflns_number_total 4892 _reflns_number_gt 4834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1561P)^2^+0.6165P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.026(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(3) _refine_ls_number_reflns 4892 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.2106 _refine_ls_wR_factor_gt 0.2097 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.186 _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 O3 O 0.4077(2) 0.45542(15) 0.79580(7) 0.0276(5) Uani 1 1 d . . . H3 H 0.3809 0.5162 0.8041 0.041 Uiso 1 1 calc R . . O2 O 0.1746(2) 0.53315(15) 0.83505(7) 0.0286(5) Uani 1 1 d . . . O9 O -0.0311(2) 0.29865(16) 0.91004(8) 0.0327(5) Uani 1 1 d . . . O4 O 0.2611(2) 0.21577(15) 0.76894(7) 0.0313(5) Uani 1 1 d . . . C34 C -0.3074(5) 0.1023(4) 0.89809(15) 0.0551(10) Uani 1 1 d . . . H34A H -0.2186 0.1425 0.8949 0.083 Uiso 1 1 calc R . . H34B H -0.2855 0.0299 0.9086 0.083 Uiso 1 1 calc R . . H34C H -0.3689 0.1360 0.9228 0.083 Uiso 1 1 calc R . . C32 C -0.3816(3) 0.0998(2) 0.84981(12) 0.0300(7) Uani 1 1 d . . . C31 C -0.3329(3) 0.1455(2) 0.80885(11) 0.0275(6) Uani 1 1 d . . . H31 H -0.3911 0.1395 0.7803 0.033 Uiso 1 1 calc R . . C30 C -0.1963(3) 0.2054(2) 0.80294(11) 0.0299(6) Uani 1 1 d . . . H30A H -0.1545 0.1887 0.7702 0.036 Uiso 1 1 calc R . . H30B H -0.1280 0.1819 0.8286 0.036 Uiso 1 1 calc R . . C28 C -0.2168(3) 0.3258(2) 0.80715(10) 0.0242(6) Uani 1 1 d . . . H28A H -0.2443 0.3420 0.8417 0.029 Uiso 1 1 calc R . . H28B H -0.2981 0.3459 0.7858 0.029 Uiso 1 1 calc R . . C8 C -0.0887(3) 0.3968(2) 0.79341(9) 0.0217(6) Uani 1 1 d . . . C1 C 0.0330(3) 0.37374(19) 0.83311(9) 0.0223(6) Uani 1 1 d . . . H1 H 0.0622 0.2986 0.8277 0.027 Uiso 1 1 calc R . . C2 C 0.1670(3) 0.4388(2) 0.82633(9) 0.0234(6) Uani 1 1 d . . . C3 C 0.3024(3) 0.3803(2) 0.80989(10) 0.0240(6) Uani 1 1 d . . . C13 C 0.3577(3) 0.3112(2) 0.85273(10) 0.0275(6) Uani 1 1 d . . . H13A H 0.2818 0.2609 0.8624 0.033 Uiso 1 1 calc R . . H13B H 0.4401 0.2695 0.8409 0.033 Uiso 1 1 calc R . . C14 C 0.4023(3) 0.3729(2) 0.89764(10) 0.0277(6) Uani 1 1 d . . . H14 H 0.4503 0.4377 0.8917 0.033 Uiso 1 1 calc R . . C15 C 0.3822(3) 0.3468(2) 0.94441(11) 0.0330(7) Uani 1 1 d . . . C16 C 0.3016(5) 0.2502(3) 0.96197(12) 0.0446(9) Uani 1 1 d . . . H16A H 0.2580 0.2146 0.9336 0.067 Uiso 1 1 calc R . . H16B H 0.2270 0.2717 0.9852 0.067 Uiso 1 1 calc R . . H16C H 0.3677 0.2017 0.9785 0.067 Uiso 1 1 calc R . . C33 C -0.5200(4) 0.0411(2) 0.84977(14) 0.0388(8) Uani 1 1 d . . . H33A H -0.5638 0.0460 0.8170 0.058 Uiso 1 1 calc R . . H33B H -0.5841 0.0722 0.8744 0.058 Uiso 1 1 calc R . . H33C H -0.5028 -0.0332 0.8579 0.058 Uiso 1 1 calc R . . C29 C -0.1385(3) 0.5128(2) 0.79511(10) 0.0277(6) Uani 1 1 d . . . H29A H -0.2063 0.5257 0.7682 0.042 Uiso 1 1 calc R . . H29B H -0.0559 0.5596 0.7913 0.042 Uiso 1 1 calc R . . H29C H -0.1848 0.5269 0.8269 0.042 Uiso 1 1 calc R . . C7 C -0.0328(3) 0.3678(2) 0.74022(10) 0.0240(6) Uani 1 1 d . . . H7 H -0.0042 0.2917 0.7410 0.029 Uiso 1 1 calc R . . C6 C 0.0985(3) 0.4314(2) 0.72221(10) 0.0243(6) Uani 1 1 d . . . H6A H 0.1163 0.4895 0.7459 0.029 Uiso 1 1 calc R . . H6B H 0.0749 0.4640 0.6899 0.029 Uiso 1 1 calc R . . C5 C 0.2384(3) 0.3669(2) 0.71622(10) 0.0255(6) Uani 1 1 d . . . H5 H 0.3180 0.4179 0.7103 0.031 Uiso 1 1 calc R . . C18 C 0.2329(3) 0.2906(2) 0.67236(10) 0.0304(6) Uani 1 1 d . . . H18A H 0.1655 0.2329 0.6803 0.037 Uiso 1 1 calc R . . H18B H 0.1949 0.3289 0.6433 0.037 Uiso 1 1 calc R . . C19 C 0.3735(4) 0.2431(2) 0.65883(11) 0.0319(7) Uani 1 1 d . . . H19 H 0.4248 0.2088 0.6845 0.038 Uiso 1 1 calc R . . C20 C 0.4337(4) 0.2442(2) 0.61442(12) 0.0344(7) Uani 1 1 d . . . C21 C 0.3729(5) 0.2944(3) 0.56892(12) 0.0507(10) Uani 1 1 d . . . H21A H 0.2797 0.3253 0.5767 0.076 Uiso 1 1 calc R . . H21B H 0.3618 0.2408 0.5431 0.076 Uiso 1 1 calc R . . H21C H 0.4375 0.3500 0.5573 0.076 Uiso 1 1 calc R . . C22 C 0.5767(4) 0.1935(3) 0.60652(14) 0.0467(9) Uani 1 1 d . . . H22A H 0.6166 0.1723 0.6385 0.070 Uiso 1 1 calc R . . H22B H 0.6410 0.2441 0.5905 0.070 Uiso 1 1 calc R . . H22C H 0.5657 0.1311 0.5854 0.070 Uiso 1 1 calc R . . C4 C 0.2686(3) 0.3095(2) 0.76465(10) 0.0233(6) Uani 1 1 d . . . C9 C -0.0184(3) 0.3799(2) 0.88694(10) 0.0260(6) Uani 1 1 d . . . C10 C -0.0479(3) 0.4858(2) 0.91249(10) 0.0316(7) Uani 1 1 d . . . H10 H -0.0358 0.5445 0.8881 0.038 Uiso 1 1 calc R . . C11 C -0.2022(4) 0.4868(3) 0.93255(13) 0.0438(8) Uani 1 1 d . . . H11A H -0.2160 0.4267 0.9548 0.066 Uiso 1 1 calc R . . H11B H -0.2693 0.4818 0.9049 0.066 Uiso 1 1 calc R . . H11C H -0.2190 0.5528 0.9506 0.066 Uiso 1 1 calc R . . C12 C 0.0588(4) 0.4998(3) 0.95464(12) 0.0431(8) Uani 1 1 d . . . H12A H 0.0549 0.4380 0.9765 0.065 Uiso 1 1 calc R . . H12B H 0.0349 0.5634 0.9735 0.065 Uiso 1 1 calc R . . H12C H 0.1552 0.5067 0.9410 0.065 Uiso 1 1 calc R . . C17 C 0.4391(4) 0.4142(3) 0.98609(12) 0.0415(8) Uani 1 1 d . . . H17A H 0.4914 0.4744 0.9724 0.062 Uiso 1 1 calc R . . H17B H 0.5032 0.3719 1.0067 0.062 Uiso 1 1 calc R . . H17C H 0.3594 0.4399 1.0062 0.062 Uiso 1 1 calc R . . C23 C -0.1546(3) 0.3784(3) 0.70137(10) 0.0318(7) Uani 1 1 d . . . H23A H -0.2402 0.3412 0.7138 0.038 Uiso 1 1 calc R . . H23B H -0.1793 0.4540 0.6976 0.038 Uiso 1 1 calc R . . C24 C -0.1158(3) 0.3344(3) 0.65183(11) 0.0354(7) Uani 1 1 d . . . H24 H -0.1028 0.2601 0.6502 0.042 Uiso 1 1 calc R . . C25 C -0.0973(4) 0.3872(3) 0.60962(11) 0.0380(8) Uani 1 1 d . . . C26 C -0.1110(4) 0.5037(3) 0.60402(13) 0.0435(8) Uani 1 1 d . . . H26A H -0.1411 0.5347 0.6355 0.065 Uiso 1 1 calc R . . H26B H -0.1822 0.5195 0.5786 0.065 Uiso 1 1 calc R . . H26C H -0.0188 0.5335 0.5943 0.065 Uiso 1 1 calc R . . C27 C -0.0610(5) 0.3319(4) 0.56209(14) 0.0574(11) Uani 1 1 d . . . H27A H -0.0537 0.2557 0.5680 0.086 Uiso 1 1 calc R . . H27B H 0.0303 0.3584 0.5496 0.086 Uiso 1 1 calc R . . H27C H -0.1359 0.3454 0.5376 0.086 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 O3 0.0291(10) 0.0216(9) 0.0320(10) -0.0015(8) 0.0029(8) -0.0047(8) O2 0.0340(11) 0.0164(9) 0.0355(10) -0.0048(8) -0.0021(9) -0.0006(8) O9 0.0419(12) 0.0274(10) 0.0289(10) 0.0061(8) 0.0001(9) -0.0028(9) O4 0.0431(12) 0.0186(10) 0.0323(10) -0.0019(8) -0.0034(9) 0.0014(9) C34 0.065(2) 0.054(2) 0.047(2) 0.0160(17) -0.0069(19) -0.018(2) C32 0.0312(14) 0.0164(12) 0.0423(16) -0.0007(11) 0.0055(12) 0.0014(11) C31 0.0318(14) 0.0174(12) 0.0334(15) -0.0015(10) 0.0020(12) 0.0000(11) C30 0.0324(15) 0.0189(13) 0.0385(15) 0.0008(11) 0.0081(12) -0.0033(11) C28 0.0261(13) 0.0171(12) 0.0294(13) 0.0026(10) 0.0030(11) 0.0013(10) C8 0.0287(13) 0.0143(12) 0.0220(12) 0.0022(9) 0.0001(10) 0.0023(10) C1 0.0273(13) 0.0152(11) 0.0244(12) -0.0012(9) -0.0004(10) 0.0019(10) C2 0.0315(14) 0.0178(13) 0.0208(12) 0.0009(9) -0.0012(11) 0.0018(10) C3 0.0299(14) 0.0172(12) 0.0248(13) 0.0001(10) -0.0001(11) -0.0036(10) C13 0.0324(14) 0.0228(13) 0.0274(14) -0.0007(10) -0.0008(11) -0.0012(11) C14 0.0300(14) 0.0236(13) 0.0295(14) -0.0007(11) -0.0052(11) -0.0011(11) C15 0.0383(16) 0.0316(15) 0.0290(14) -0.0018(12) -0.0075(13) -0.0002(13) C16 0.063(2) 0.0403(18) 0.0302(15) 0.0096(13) -0.0050(16) -0.0075(17) C33 0.0330(16) 0.0229(14) 0.061(2) 0.0083(13) 0.0084(15) -0.0004(12) C29 0.0380(15) 0.0155(12) 0.0295(14) -0.0007(10) 0.0000(12) 0.0037(11) C7 0.0272(13) 0.0212(12) 0.0238(13) 0.0007(10) 0.0003(11) -0.0031(10) C6 0.0352(15) 0.0175(12) 0.0202(12) 0.0030(9) -0.0004(11) -0.0024(11) C5 0.0315(14) 0.0214(13) 0.0236(12) -0.0007(10) 0.0025(11) -0.0026(11) C18 0.0406(16) 0.0278(14) 0.0229(13) -0.0031(11) 0.0031(12) -0.0017(12) C19 0.0458(17) 0.0218(13) 0.0282(14) 0.0017(11) -0.0015(13) 0.0036(12) C20 0.0494(19) 0.0228(14) 0.0310(14) -0.0071(11) 0.0066(14) -0.0034(13) C21 0.068(3) 0.057(2) 0.0273(15) -0.0009(15) 0.0054(16) 0.014(2) C22 0.053(2) 0.0386(18) 0.0486(19) -0.0038(15) 0.0065(17) 0.0079(16) C4 0.0246(12) 0.0199(13) 0.0255(13) -0.0001(10) 0.0015(11) 0.0016(10) C9 0.0273(13) 0.0261(13) 0.0247(13) 0.0008(10) -0.0035(11) 0.0008(11) C10 0.0410(16) 0.0291(14) 0.0247(13) -0.0031(11) 0.0020(13) 0.0009(13) C11 0.050(2) 0.0425(18) 0.0388(17) 0.0011(14) 0.0172(15) 0.0100(16) C12 0.057(2) 0.0382(17) 0.0338(16) -0.0128(13) -0.0020(16) 0.0024(16) C17 0.0478(18) 0.0475(18) 0.0291(14) -0.0022(13) -0.0087(14) -0.0009(16) C23 0.0330(15) 0.0381(16) 0.0243(13) 0.0047(12) -0.0036(12) -0.0037(13) C24 0.0389(16) 0.0348(16) 0.0324(15) -0.0001(12) -0.0090(13) 0.0008(13) C25 0.0382(16) 0.0494(19) 0.0263(14) 0.0012(13) -0.0055(13) 0.0074(15) C26 0.0397(17) 0.055(2) 0.0357(17) 0.0160(15) 0.0071(14) 0.0072(16) C27 0.071(3) 0.071(3) 0.0299(17) -0.0083(17) -0.0095(18) 0.008(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 O3 C3 1.422(3) . ? O3 H3 0.8400 . ? O2 C2 1.219(3) . ? O9 C9 1.209(3) . ? O4 C4 1.194(4) . ? C34 C32 1.480(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C32 C31 1.331(4) . ? C32 C33 1.495(4) . ? C31 C30 1.497(4) . ? C31 H31 0.9500 . ? C30 C28 1.540(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C28 C8 1.546(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C8 C29 1.541(3) . ? C8 C7 1.575(4) . ? C8 C1 1.594(4) . ? C1 C2 1.514(4) . ? C1 C9 1.536(4) . ? C1 H1 1.0000 . ? C2 C3 1.536(4) . ? C3 C13 1.542(4) . ? C3 C4 1.550(4) . ? C13 C14 1.503(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.321(4) . ? C14 H14 0.9500 . ? C15 C17 1.511(4) . ? C15 C16 1.514(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C7 C6 1.550(4) . ? C7 C23 1.557(4) . ? C7 H7 1.0000 . ? C6 C5 1.554(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C5 C4 1.524(4) . ? C5 C18 1.530(4) . ? C5 H5 1.0000 . ? C18 C19 1.495(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.327(5) . ? C19 H19 0.9500 . ? C20 C21 1.498(5) . ? C20 C22 1.501(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C9 C10 1.533(4) . ? C10 C12 1.527(5) . ? C10 C11 1.545(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C23 C24 1.496(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.334(5) . ? C24 H24 0.9500 . ? C25 C26 1.488(5) . ? C25 C27 1.503(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 C3 O3 H3 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C32 C34 124.3(3) . . ? C31 C32 C33 120.9(3) . . ? C34 C32 C33 114.8(3) . . ? C32 C31 C30 127.1(3) . . ? C32 C31 H31 116.5 . . ? C30 C31 H31 116.5 . . ? C31 C30 C28 112.7(2) . . ? C31 C30 H30A 109.0 . . ? C28 C30 H30A 109.0 . . ? C31 C30 H30B 109.0 . . ? C28 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? C30 C28 C8 117.4(2) . . ? C30 C28 H28A 107.9 . . ? C8 C28 H28A 107.9 . . ? C30 C28 H28B 107.9 . . ? C8 C28 H28B 107.9 . . ? H28A C28 H28B 107.2 . . ? C29 C8 C28 108.2(2) . . ? C29 C8 C7 110.5(2) . . ? C28 C8 C7 110.0(2) . . ? C29 C8 C1 111.8(2) . . ? C28 C8 C1 106.7(2) . . ? C7 C8 C1 109.6(2) . . ? C2 C1 C9 110.3(2) . . ? C2 C1 C8 114.4(2) . . ? C9 C1 C8 113.9(2) . . ? C2 C1 H1 105.8 . . ? C9 C1 H1 105.8 . . ? C8 C1 H1 105.8 . . ? O2 C2 C1 123.9(3) . . ? O2 C2 C3 118.7(3) . . ? C1 C2 C3 117.3(2) . . ? O3 C3 C2 109.2(2) . . ? O3 C3 C13 110.3(2) . . ? C2 C3 C13 109.5(2) . . ? O3 C3 C4 108.5(2) . . ? C2 C3 C4 109.8(2) . . ? C13 C3 C4 109.5(2) . . ? C14 C13 C3 114.0(2) . . ? C14 C13 H13A 108.8 . . ? C3 C13 H13A 108.8 . . ? C14 C13 H13B 108.8 . . ? C3 C13 H13B 108.8 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C13 127.2(3) . . ? C15 C14 H14 116.4 . . ? C13 C14 H14 116.4 . . ? C14 C15 C17 121.6(3) . . ? C14 C15 C16 125.0(3) . . ? C17 C15 C16 113.4(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C8 C29 H29A 109.5 . . ? C8 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C8 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C6 C7 C23 109.0(2) . . ? C6 C7 C8 115.5(2) . . ? C23 C7 C8 110.6(2) . . ? C6 C7 H7 107.1 . . ? C23 C7 H7 107.1 . . ? C8 C7 H7 107.1 . . ? C7 C6 C5 115.5(2) . . ? C7 C6 H6A 108.4 . . ? C5 C6 H6A 108.4 . . ? C7 C6 H6B 108.4 . . ? C5 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C4 C5 C18 111.8(2) . . ? C4 C5 C6 108.5(2) . . ? C18 C5 C6 112.6(2) . . ? C4 C5 H5 107.9 . . ? C18 C5 H5 107.9 . . ? C6 C5 H5 107.9 . . ? C19 C18 C5 114.5(3) . . ? C19 C18 H18A 108.6 . . ? C5 C18 H18A 108.6 . . ? C19 C18 H18B 108.6 . . ? C5 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C20 C19 C18 126.4(3) . . ? C20 C19 H19 116.8 . . ? C18 C19 H19 116.8 . . ? C19 C20 C21 125.9(3) . . ? C19 C20 C22 120.3(3) . . ? C21 C20 C22 113.9(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O4 C4 C5 123.1(2) . . ? O4 C4 C3 120.7(2) . . ? C5 C4 C3 116.1(2) . . ? O9 C9 C10 119.5(2) . . ? O9 C9 C1 118.5(2) . . ? C10 C9 C1 121.9(2) . . ? C12 C10 C9 108.6(3) . . ? C12 C10 C11 110.5(3) . . ? C9 C10 C11 109.5(3) . . ? C12 C10 H10 109.4 . . ? C9 C10 H10 109.4 . . ? C11 C10 H10 109.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C24 C23 C7 113.2(3) . . ? C24 C23 H23A 108.9 . . ? C7 C23 H23A 108.9 . . ? C24 C23 H23B 108.9 . . ? C7 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C25 C24 C23 127.7(3) . . ? C25 C24 H24 116.1 . . ? C23 C24 H24 116.1 . . ? C24 C25 C26 124.9(3) . . ? C24 C25 C27 121.9(3) . . ? C26 C25 C27 113.2(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 C34 C32 C31 C30 1.1(5) . . . . ? C33 C32 C31 C30 -179.2(3) . . . . ? C32 C31 C30 C28 -97.2(4) . . . . ? C31 C30 C28 C8 -170.4(2) . . . . ? C30 C28 C8 C29 174.1(2) . . . . ? C30 C28 C8 C7 53.3(3) . . . . ? C30 C28 C8 C1 -65.5(3) . . . . ? C29 C8 C1 C2 -60.5(3) . . . . ? C28 C8 C1 C2 -178.5(2) . . . . ? C7 C8 C1 C2 62.4(3) . . . . ? C29 C8 C1 C9 67.7(3) . . . . ? C28 C8 C1 C9 -50.3(3) . . . . ? C7 C8 C1 C9 -169.5(2) . . . . ? C9 C1 C2 O2 -58.3(3) . . . . ? C8 C1 C2 O2 71.7(3) . . . . ? C9 C1 C2 C3 118.6(2) . . . . ? C8 C1 C2 C3 -111.4(2) . . . . ? O2 C2 C3 O3 -14.7(3) . . . . ? C1 C2 C3 O3 168.2(2) . . . . ? O2 C2 C3 C13 106.2(3) . . . . ? C1 C2 C3 C13 -70.9(3) . . . . ? O2 C2 C3 C4 -133.6(3) . . . . ? C1 C2 C3 C4 49.3(3) . . . . ? O3 C3 C13 C14 57.2(3) . . . . ? C2 C3 C13 C14 -63.1(3) . . . . ? C4 C3 C13 C14 176.5(2) . . . . ? C3 C13 C14 C15 141.3(3) . . . . ? C13 C14 C15 C17 177.1(3) . . . . ? C13 C14 C15 C16 -3.4(5) . . . . ? C29 C8 C7 C6 62.1(3) . . . . ? C28 C8 C7 C6 -178.5(2) . . . . ? C1 C8 C7 C6 -61.5(3) . . . . ? C29 C8 C7 C23 -62.3(3) . . . . ? C28 C8 C7 C23 57.1(3) . . . . ? C1 C8 C7 C23 174.1(2) . . . . ? C23 C7 C6 C5 -122.1(2) . . . . ? C8 C7 C6 C5 112.6(3) . . . . ? C7 C6 C5 C4 -53.7(3) . . . . ? C7 C6 C5 C18 70.7(3) . . . . ? C4 C5 C18 C19 -69.3(3) . . . . ? C6 C5 C18 C19 168.2(2) . . . . ? C5 C18 C19 C20 -126.5(3) . . . . ? C18 C19 C20 C21 0.7(5) . . . . ? C18 C19 C20 C22 179.6(3) . . . . ? C18 C5 C4 O4 -13.5(4) . . . . ? C6 C5 C4 O4 111.3(3) . . . . ? C18 C5 C4 C3 169.8(2) . . . . ? C6 C5 C4 C3 -65.4(3) . . . . ? O3 C3 C4 O4 134.3(3) . . . . ? C2 C3 C4 O4 -106.4(3) . . . . ? C13 C3 C4 O4 13.8(4) . . . . ? O3 C3 C4 C5 -48.9(3) . . . . ? C2 C3 C4 C5 70.4(3) . . . . ? C13 C3 C4 C5 -169.4(2) . . . . ? C2 C1 C9 O9 -122.4(3) . . . . ? C8 C1 C9 O9 107.4(3) . . . . ? C2 C1 C9 C10 55.1(3) . . . . ? C8 C1 C9 C10 -75.1(3) . . . . ? O9 C9 C10 C12 62.6(4) . . . . ? C1 C9 C10 C12 -114.9(3) . . . . ? O9 C9 C10 C11 -58.2(4) . . . . ? C1 C9 C10 C11 124.3(3) . . . . ? C6 C7 C23 C24 61.9(3) . . . . ? C8 C7 C23 C24 -170.1(2) . . . . ? C7 C23 C24 C25 -113.0(4) . . . . ? C23 C24 C25 C26 0.7(6) . . . . ? C23 C24 C25 C27 -178.8(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.84 2.12 2.622(3) 118.1 . _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 69.38 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.806 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.197