data_cu_20120226aa_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H23 N O5' _chemical_formula_weight 417.44 _chemical_absolute_configuration 'rm' 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' 'N' 'N' 0.0311 0.0180 '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 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.5226(7) _cell_length_b 7.2796(6) _cell_length_c 14.9337(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.656(3) _cell_angle_gamma 90.00 _cell_volume 1023.42(14) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7094 _cell_measurement_theta_min 5.99 _cell_measurement_theta_max 66.89 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8126 _exptl_absorpt_correction_T_max 0.9062 _exptl_absorpt_process_details 'sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7947 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.99 _diffrn_reflns_theta_max 65.94 _reflns_number_total 2929 _reflns_number_gt 2874 _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^)+(0.0532P)^2^+0.0904P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.12(19) _refine_ls_number_reflns 2929 _refine_ls_number_parameters 283 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.062 _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 1.11332(12) 0.1804(2) 1.07481(7) 0.0565(3) Uani 1 1 d . . . O5 O 0.74757(10) 0.2463(2) 0.61818(6) 0.0535(3) Uani 1 1 d . . . C1 C 1.12322(18) 0.2263(3) 1.23608(10) 0.0518(4) Uani 1 1 d . . . N1 N 0.60049(12) 0.2299(2) 0.72031(8) 0.0488(3) Uani 1 1 d . . . C8 C 0.89522(18) 0.2171(3) 1.13393(10) 0.0502(4) Uani 1 1 d . . . O4 O 0.51025(11) 0.2564(3) 0.57065(7) 0.0609(3) Uani 1 1 d . . . O3 O 0.68898(12) 0.2825(2) 1.02333(7) 0.0565(3) Uani 1 1 d . . . C11 C 0.90196(18) 0.1797(3) 0.96842(10) 0.0524(4) Uani 1 1 d . . . H11A H 0.9415 0.0762 0.9399 0.063 Uiso 1 1 calc R . . H11B H 0.9219 0.2905 0.9365 0.063 Uiso 1 1 calc R . . C20 C 0.71132(16) 0.2068(3) 0.79147(10) 0.0498(4) Uani 1 1 d . . . H20 H 0.8071 0.2036 0.7854 0.060 Uiso 1 1 calc R . . C7 C 0.96902(18) 0.1927(3) 1.06521(10) 0.0487(4) Uani 1 1 d . . . C13 C 0.66056(17) 0.1896(3) 0.87019(10) 0.0489(4) Uani 1 1 d . . . C23 C 0.7358(2) 0.4256(3) 0.47696(14) 0.0622(5) Uani 1 1 d . . . H23A H 0.6338 0.4264 0.4675 0.093 Uiso 1 1 calc R . . H23B H 0.7693 0.4312 0.4195 0.093 Uiso 1 1 calc R . . H23C H 0.7705 0.5300 0.5129 0.093 Uiso 1 1 calc R . . O2 O 0.90301(14) 0.2484(3) 1.29119(8) 0.0820(5) Uani 1 1 d . . . C5 C 1.3365(2) 0.1897(3) 1.16780(12) 0.0642(5) Uani 1 1 d . . . H5 H 1.3796 0.1695 1.1168 0.077 Uiso 1 1 calc R . . C12 C 0.74170(19) 0.1555(3) 0.96277(11) 0.0507(4) Uani 1 1 d . . . H12 H 0.7222 0.0301 0.9814 0.061 Uiso 1 1 calc R . . C6 C 1.19031(18) 0.1990(3) 1.16051(10) 0.0515(4) Uani 1 1 d . . . C24 C 0.7345(2) 0.0830(3) 0.47337(14) 0.0620(5) Uani 1 1 d . . . H24A H 0.7666 -0.0247 0.5076 0.093 Uiso 1 1 calc R . . H24B H 0.7697 0.0810 0.4164 0.093 Uiso 1 1 calc R . . H24C H 0.6326 0.0850 0.4628 0.093 Uiso 1 1 calc R . . C19 C 0.47217(16) 0.2287(3) 0.75660(10) 0.0471(4) Uani 1 1 d . . . C9 C 0.96746(18) 0.2312(3) 1.22650(10) 0.0551(4) Uani 1 1 d . . . C14 C 0.50780(17) 0.2040(3) 0.84984(10) 0.0482(4) Uani 1 1 d . . . C3 C 1.3532(2) 0.2403(4) 1.32800(12) 0.0677(5) Uani 1 1 d . . . H3 H 1.4085 0.2560 1.3844 0.081 Uiso 1 1 calc R . . C10 C 0.73689(18) 0.2348(3) 1.11505(10) 0.0560(4) Uani 1 1 d . . . H10A H 0.6940 0.1193 1.1287 0.067 Uiso 1 1 calc R . . H10B H 0.7065 0.3283 1.1543 0.067 Uiso 1 1 calc R . . C22 C 0.78883(16) 0.2516(3) 0.52559(9) 0.0504(4) Uani 1 1 d . . . C21 C 0.61147(15) 0.2455(3) 0.62845(9) 0.0478(4) Uani 1 1 d . . . C2 C 1.20816(19) 0.2460(4) 1.31931(11) 0.0622(5) Uani 1 1 d . . . H2 H 1.1655 0.2637 1.3707 0.075 Uiso 1 1 calc R . . C15 C 0.3998(2) 0.1973(3) 0.90357(11) 0.0604(5) Uani 1 1 d . . . H15 H 0.4212 0.1800 0.9658 0.072 Uiso 1 1 calc R . . C16 C 0.26233(19) 0.2167(4) 0.86300(12) 0.0681(5) Uani 1 1 d . . . H16 H 0.1898 0.2127 0.8983 0.082 Uiso 1 1 calc R . . C4 C 1.4170(2) 0.2106(4) 1.25111(13) 0.0693(6) Uani 1 1 d . . . H4 H 1.5155 0.2050 1.2565 0.083 Uiso 1 1 calc R . . C25 C 0.94934(18) 0.2498(4) 0.54816(12) 0.0717(6) Uani 1 1 d . . . H25A H 0.9805 0.3563 0.5836 0.108 Uiso 1 1 calc R . . H25B H 0.9900 0.2509 0.4931 0.108 Uiso 1 1 calc R . . H25C H 0.9792 0.1410 0.5821 0.108 Uiso 1 1 calc R . . C18 C 0.33256(17) 0.2485(3) 0.71475(11) 0.0551(4) Uani 1 1 d . . . H18 H 0.3101 0.2652 0.6525 0.066 Uiso 1 1 calc R . . C17 C 0.22848(18) 0.2422(4) 0.77022(12) 0.0642(5) Uani 1 1 d . . . H17 H 0.1337 0.2554 0.7447 0.077 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 0.0503(6) 0.0815(10) 0.0387(5) -0.0007(6) 0.0102(4) 0.0066(6) O5 0.0423(5) 0.0817(9) 0.0377(5) 0.0009(6) 0.0093(4) 0.0001(6) C1 0.0583(9) 0.0564(11) 0.0416(7) 0.0013(8) 0.0101(6) -0.0007(9) N1 0.0437(6) 0.0657(9) 0.0382(6) 0.0016(7) 0.0097(5) 0.0015(7) C8 0.0566(8) 0.0553(11) 0.0403(7) 0.0004(8) 0.0122(6) 0.0006(9) O4 0.0457(6) 0.0954(10) 0.0415(5) 0.0039(7) 0.0062(4) 0.0029(7) O3 0.0571(6) 0.0734(9) 0.0400(5) -0.0039(6) 0.0103(5) 0.0110(6) C11 0.0537(9) 0.0663(12) 0.0386(8) -0.0007(7) 0.0116(6) 0.0072(8) C20 0.0446(7) 0.0635(11) 0.0417(7) -0.0002(8) 0.0079(6) 0.0035(8) C7 0.0504(8) 0.0556(11) 0.0409(7) 0.0007(7) 0.0093(6) 0.0037(7) C13 0.0509(8) 0.0554(10) 0.0406(8) -0.0009(7) 0.0074(6) 0.0014(8) C23 0.0679(14) 0.0683(13) 0.0528(11) 0.0048(9) 0.0167(10) 0.0000(9) O2 0.0685(7) 0.1401(15) 0.0406(6) -0.0062(10) 0.0188(5) 0.0014(11) C5 0.0578(10) 0.0878(16) 0.0487(9) 0.0067(10) 0.0133(7) 0.0072(10) C12 0.0556(9) 0.0581(11) 0.0397(8) -0.0004(7) 0.0118(7) 0.0035(7) C6 0.0567(9) 0.0581(11) 0.0397(7) 0.0034(7) 0.0074(6) 0.0009(8) C24 0.0668(14) 0.0699(14) 0.0510(11) -0.0025(9) 0.0145(10) 0.0000(9) C19 0.0464(7) 0.0518(10) 0.0452(7) -0.0003(8) 0.0137(6) -0.0009(8) C9 0.0618(9) 0.0672(12) 0.0381(7) -0.0010(9) 0.0128(6) 0.0002(10) C14 0.0508(8) 0.0524(10) 0.0434(7) 0.0003(7) 0.0130(6) -0.0008(8) C3 0.0658(10) 0.0869(15) 0.0476(8) 0.0027(11) -0.0010(7) -0.0016(12) C10 0.0565(8) 0.0740(12) 0.0395(7) -0.0031(9) 0.0132(6) 0.0032(10) C22 0.0454(8) 0.0703(11) 0.0372(7) -0.0004(8) 0.0121(6) 0.0001(9) C21 0.0456(7) 0.0596(10) 0.0393(7) -0.0006(8) 0.0104(6) 0.0013(8) C2 0.0663(10) 0.0788(13) 0.0411(8) -0.0013(10) 0.0068(7) -0.0012(11) C15 0.0588(10) 0.0793(14) 0.0463(8) 0.0012(9) 0.0188(7) -0.0038(10) C16 0.0553(9) 0.0914(16) 0.0625(10) -0.0060(12) 0.0250(8) -0.0096(11) C4 0.0561(9) 0.0900(17) 0.0608(10) 0.0079(12) 0.0052(8) 0.0039(11) C25 0.0476(9) 0.1126(18) 0.0578(9) 0.0010(13) 0.0171(7) 0.0007(12) C18 0.0499(8) 0.0681(11) 0.0477(8) -0.0002(9) 0.0085(6) -0.0004(9) C17 0.0455(8) 0.0845(14) 0.0634(9) -0.0044(12) 0.0112(7) -0.0016(10) _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 1.363(2) . ? O1 C6 1.3826(19) . ? O5 C21 1.3278(18) . ? O5 C22 1.4938(16) . ? C1 C2 1.385(2) . ? C1 C6 1.392(2) . ? C1 C9 1.469(2) . ? N1 C20 1.3907(19) . ? N1 C21 1.3959(18) . ? N1 C19 1.4093(19) . ? C8 C7 1.340(2) . ? C8 C9 1.452(2) . ? C8 C10 1.497(2) . ? O4 C21 1.1958(18) . ? O3 C10 1.4201(19) . ? O3 C12 1.436(2) . ? C11 C7 1.493(2) . ? C11 C12 1.526(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C20 C13 1.342(2) . ? C20 H20 0.9300 . ? C13 C14 1.444(2) . ? C13 C12 1.500(2) . ? C23 C22 1.509(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? O2 C9 1.227(2) . ? C5 C4 1.368(3) . ? C5 C6 1.382(2) . ? C5 H5 0.9300 . ? C12 H12 0.9800 . ? C24 C22 1.503(3) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C19 C18 1.389(2) . ? C19 C14 1.394(2) . ? C14 C15 1.398(2) . ? C3 C2 1.369(3) . ? C3 C4 1.394(3) . ? C3 H3 0.9300 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C22 C25 1.515(2) . ? C2 H2 0.9300 . ? C15 C16 1.364(3) . ? C15 H15 0.9300 . ? C16 C17 1.387(3) . ? C16 H16 0.9300 . ? C4 H4 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C18 C17 1.385(2) . ? C18 H18 0.9300 . ? C17 H17 0.9300 . ? 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 C6 118.47(12) . . ? C21 O5 C22 120.29(11) . . ? C2 C1 C6 117.72(15) . . ? C2 C1 C9 122.00(14) . . ? C6 C1 C9 120.28(14) . . ? C20 N1 C21 126.89(12) . . ? C20 N1 C19 107.91(12) . . ? C21 N1 C19 125.16(12) . . ? C7 C8 C9 120.70(15) . . ? C7 C8 C10 119.78(14) . . ? C9 C8 C10 119.51(13) . . ? C10 O3 C12 111.00(14) . . ? C7 C11 C12 109.84(13) . . ? C7 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? C7 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C13 C20 N1 110.40(13) . . ? C13 C20 H20 124.8 . . ? N1 C20 H20 124.8 . . ? C8 C7 O1 124.40(14) . . ? C8 C7 C11 123.55(15) . . ? O1 C7 C11 112.04(13) . . ? C20 C13 C14 107.04(13) . . ? C20 C13 C12 128.26(15) . . ? C14 C13 C12 124.67(14) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C4 C5 C6 119.09(16) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? O3 C12 C13 107.07(14) . . ? O3 C12 C11 109.40(14) . . ? C13 C12 C11 113.83(14) . . ? O3 C12 H12 108.8 . . ? C13 C12 H12 108.8 . . ? C11 C12 H12 108.8 . . ? C5 C6 O1 117.11(14) . . ? C5 C6 C1 121.53(15) . . ? O1 C6 C1 121.35(15) . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C18 C19 C14 122.37(14) . . ? C18 C19 N1 130.76(14) . . ? C14 C19 N1 106.87(13) . . ? O2 C9 C8 122.38(16) . . ? O2 C9 C1 122.91(15) . . ? C8 C9 C1 114.70(13) . . ? C19 C14 C15 119.24(15) . . ? C19 C14 C13 107.78(13) . . ? C15 C14 C13 132.98(15) . . ? C2 C3 C4 119.02(16) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? O3 C10 C8 111.77(12) . . ? O3 C10 H10A 109.3 . . ? C8 C10 H10A 109.3 . . ? O3 C10 H10B 109.3 . . ? C8 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? O5 C22 C24 109.96(15) . . ? O5 C22 C23 110.57(15) . . ? C24 C22 C23 111.82(13) . . ? O5 C22 C25 101.01(11) . . ? C24 C22 C25 111.41(18) . . ? C23 C22 C25 111.58(18) . . ? O4 C21 O5 127.66(13) . . ? O4 C21 N1 122.91(13) . . ? O5 C21 N1 109.43(12) . . ? C3 C2 C1 121.81(16) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C16 C15 C14 118.77(16) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 121.38(16) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C5 C4 C3 120.82(17) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C17 C18 C19 116.76(15) . . ? C17 C18 H18 121.6 . . ? C19 C18 H18 121.6 . . ? C18 C17 C16 121.49(16) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? 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 C21 N1 C20 C13 -177.51(18) . . . . ? C19 N1 C20 C13 0.5(2) . . . . ? C9 C8 C7 O1 -0.4(3) . . . . ? C10 C8 C7 O1 178.02(18) . . . . ? C9 C8 C7 C11 -179.10(19) . . . . ? C10 C8 C7 C11 -0.7(3) . . . . ? C6 O1 C7 C8 -1.9(3) . . . . ? C6 O1 C7 C11 176.95(16) . . . . ? C12 C11 C7 C8 -12.5(3) . . . . ? C12 C11 C7 O1 168.67(15) . . . . ? N1 C20 C13 C14 -0.5(2) . . . . ? N1 C20 C13 C12 177.49(19) . . . . ? C10 O3 C12 C13 167.34(15) . . . . ? C10 O3 C12 C11 -68.86(18) . . . . ? C20 C13 C12 O3 133.4(2) . . . . ? C14 C13 C12 O3 -48.8(2) . . . . ? C20 C13 C12 C11 12.4(3) . . . . ? C14 C13 C12 C11 -169.86(16) . . . . ? C7 C11 C12 O3 45.27(19) . . . . ? C7 C11 C12 C13 165.00(16) . . . . ? C4 C5 C6 O1 178.9(2) . . . . ? C4 C5 C6 C1 -1.0(3) . . . . ? C7 O1 C6 C5 -178.68(18) . . . . ? C7 O1 C6 C1 1.3(3) . . . . ? C2 C1 C6 C5 0.7(3) . . . . ? C9 C1 C6 C5 -178.5(2) . . . . ? C2 C1 C6 O1 -179.2(2) . . . . ? C9 C1 C6 O1 1.5(3) . . . . ? C20 N1 C19 C18 179.2(2) . . . . ? C21 N1 C19 C18 -2.7(3) . . . . ? C20 N1 C19 C14 -0.2(2) . . . . ? C21 N1 C19 C14 177.84(19) . . . . ? C7 C8 C9 O2 -177.9(2) . . . . ? C10 C8 C9 O2 3.6(3) . . . . ? C7 C8 C9 C1 3.0(3) . . . . ? C10 C8 C9 C1 -175.40(18) . . . . ? C2 C1 C9 O2 -1.8(4) . . . . ? C6 C1 C9 O2 177.4(2) . . . . ? C2 C1 C9 C8 177.2(2) . . . . ? C6 C1 C9 C8 -3.6(3) . . . . ? C18 C19 C14 C15 0.5(3) . . . . ? N1 C19 C14 C15 -179.99(18) . . . . ? C18 C19 C14 C13 -179.60(19) . . . . ? N1 C19 C14 C13 -0.1(2) . . . . ? C20 C13 C14 C19 0.4(2) . . . . ? C12 C13 C14 C19 -177.72(19) . . . . ? C20 C13 C14 C15 -179.7(2) . . . . ? C12 C13 C14 C15 2.1(3) . . . . ? C12 O3 C10 C8 54.2(2) . . . . ? C7 C8 C10 O3 -19.2(3) . . . . ? C9 C8 C10 O3 159.24(18) . . . . ? C21 O5 C22 C24 -62.0(2) . . . . ? C21 O5 C22 C23 62.0(2) . . . . ? C21 O5 C22 C25 -179.8(2) . . . . ? C22 O5 C21 O4 -3.4(3) . . . . ? C22 O5 C21 N1 176.68(16) . . . . ? C20 N1 C21 O4 176.3(2) . . . . ? C19 N1 C21 O4 -1.4(3) . . . . ? C20 N1 C21 O5 -3.8(3) . . . . ? C19 N1 C21 O5 178.52(17) . . . . ? C4 C3 C2 C1 -1.1(4) . . . . ? C6 C1 C2 C3 0.3(4) . . . . ? C9 C1 C2 C3 179.6(2) . . . . ? C19 C14 C15 C16 -0.5(3) . . . . ? C13 C14 C15 C16 179.7(2) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? C6 C5 C4 C3 0.3(4) . . . . ? C2 C3 C4 C5 0.8(4) . . . . ? C14 C19 C18 C17 -0.2(3) . . . . ? N1 C19 C18 C17 -179.5(2) . . . . ? C19 C18 C17 C16 -0.2(4) . . . . ? C15 C16 C17 C18 0.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 65.94 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.159 _refine_diff_density_min -0.151 _refine_diff_density_rms 0.028