data_wue5659 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H20 N2 O3' _chemical_formula_weight 396.43 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 '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 11.8959(7) _cell_length_b 7.2879(3) _cell_length_c 22.7295(18) _cell_angle_alpha 90.00 _cell_angle_beta 91.218(4) _cell_angle_gamma 90.00 _cell_volume 1970.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3368 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8142 _exptl_absorpt_correction_T_max 0.9789 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14105 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 66.98 _reflns_number_total 3387 _reflns_number_gt 2619 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0490P)^2^+0.7737P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'at N from difmap, others geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3387 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 N1 N 0.50616(15) 0.2003(2) 0.42717(7) 0.0508(4) Uani 1 1 d . . . H1 H 0.5674(19) 0.156(3) 0.4432(10) 0.061 Uiso 1 1 d . . . N2 N 0.41598(15) 0.0995(2) 0.45081(7) 0.0534(4) Uani 1 1 d . . . C3 C 0.3870(2) -0.0808(3) 0.43970(9) 0.0608(6) Uani 1 1 d . . . H3 H 0.4287 -0.1632 0.4170 0.073 Uiso 1 1 calc R . . C4 C 0.2895(2) -0.1207(3) 0.46632(10) 0.0665(6) Uani 1 1 d . . . H4 H 0.2519 -0.2341 0.4657 0.080 Uiso 1 1 calc R . . C5 C 0.25434(18) 0.0437(3) 0.49584(9) 0.0614(6) Uani 1 1 d . . . C6 C 0.1618(2) 0.0894(4) 0.52999(11) 0.0752(7) Uani 1 1 d . . . H6 H 0.1062 0.0019 0.5382 0.090 Uiso 1 1 calc R . . C7 C 0.1544(2) 0.2653(5) 0.55119(11) 0.0846(8) Uani 1 1 d . . . H7 H 0.0918 0.2985 0.5734 0.102 Uiso 1 1 calc R . . C8 C 0.2376(2) 0.3965(4) 0.54069(10) 0.0736(7) Uani 1 1 d . . . H8 H 0.2303 0.5148 0.5566 0.088 Uiso 1 1 calc R . . C9 C 0.3292(2) 0.3563(3) 0.50772(9) 0.0598(6) Uani 1 1 d . . . H9 H 0.3852 0.4441 0.5006 0.072 Uiso 1 1 calc R . . C10 C 0.33571(17) 0.1777(3) 0.48498(8) 0.0517(5) Uani 1 1 d . . . C11 C 0.50941(16) 0.1828(3) 0.36227(8) 0.0454(4) Uani 1 1 d . . . H11 H 0.5062 0.0513 0.3514 0.054 Uiso 1 1 calc R . . C12 C 0.61944(15) 0.2620(3) 0.34334(8) 0.0459(4) Uani 1 1 d . . . C13 C 0.71393(17) 0.1503(3) 0.34079(9) 0.0603(6) Uani 1 1 d . . . H13 H 0.7089 0.0256 0.3510 0.072 Uiso 1 1 calc R . . C14 C 0.81541(19) 0.2228(4) 0.32327(10) 0.0750(7) Uani 1 1 d . . . H14 H 0.8792 0.1470 0.3219 0.090 Uiso 1 1 calc R . . C15 C 0.82374(19) 0.4040(5) 0.30786(10) 0.0756(7) Uani 1 1 d . . . H15 H 0.8928 0.4508 0.2952 0.091 Uiso 1 1 calc R . . C16 C 0.73164(18) 0.5180(4) 0.31081(9) 0.0634(6) Uani 1 1 d . . . H16 H 0.7381 0.6427 0.3008 0.076 Uiso 1 1 calc R . . C17 C 0.62840(16) 0.4476(3) 0.32879(8) 0.0484(5) Uani 1 1 d . . . C18 C 0.52955(18) 0.5702(3) 0.33237(8) 0.0518(5) Uani 1 1 d . . . O1 O 0.53831(15) 0.7351(2) 0.32433(8) 0.0776(5) Uani 1 1 d . . . C19 C 0.41849(17) 0.4873(3) 0.34766(9) 0.0518(5) Uani 1 1 d . . . H19A H 0.3587 0.5530 0.3261 0.062 Uiso 1 1 calc R . . H19B H 0.4064 0.5052 0.3898 0.062 Uiso 1 1 calc R . . C20 C 0.40858(16) 0.2830(3) 0.33368(8) 0.0465(5) Uani 1 1 d . . . H20 H 0.3397 0.2369 0.3524 0.056 Uiso 1 1 calc R . . C21 C 0.39904(15) 0.2382(3) 0.26832(8) 0.0453(4) Uani 1 1 d . . . C22 C 0.38708(15) 0.0525(3) 0.25180(8) 0.0487(5) Uani 1 1 d . . . H22 H 0.3808 -0.0405 0.2802 0.058 Uiso 1 1 calc R . . C23 C 0.38498(15) 0.0126(3) 0.19330(9) 0.0487(5) Uani 1 1 d . . . O24 O 0.37625(13) -0.1581(2) 0.16694(6) 0.0635(4) Uani 1 1 d . . . C25 C 0.3976(2) -0.1252(3) 0.10608(10) 0.0686(6) Uani 1 1 d . . . H25A H 0.4743 -0.1631 0.0969 0.082 Uiso 1 1 calc R . . H25B H 0.3450 -0.1957 0.0812 0.082 Uiso 1 1 calc R . . O26 O 0.38381(14) 0.0661(2) 0.09528(6) 0.0675(4) Uani 1 1 d . . . C27 C 0.39016(17) 0.1461(3) 0.15063(8) 0.0532(5) Uani 1 1 d . . . C28 C 0.3975(2) 0.3266(3) 0.16483(9) 0.0623(6) Uani 1 1 d . . . H28 H 0.3990 0.4180 0.1357 0.075 Uiso 1 1 calc R . . C29 C 0.40272(17) 0.3708(3) 0.22472(9) 0.0541(5) Uani 1 1 d . . . H29 H 0.4089 0.4948 0.2358 0.065 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 N1 0.0514(9) 0.0597(10) 0.0414(9) 0.0035(7) 0.0014(7) -0.0025(8) N2 0.0637(11) 0.0520(10) 0.0448(9) 0.0016(8) 0.0042(8) -0.0068(8) C3 0.0837(16) 0.0491(12) 0.0491(11) 0.0030(9) -0.0077(11) -0.0067(11) C4 0.0798(16) 0.0631(14) 0.0561(13) 0.0124(11) -0.0136(12) -0.0117(12) C5 0.0589(13) 0.0747(15) 0.0502(12) 0.0184(11) -0.0053(10) -0.0079(11) C6 0.0605(14) 0.099(2) 0.0663(15) 0.0266(15) 0.0032(12) -0.0096(14) C7 0.0720(17) 0.114(2) 0.0682(16) 0.0161(16) 0.0180(13) 0.0166(17) C8 0.0829(17) 0.0859(17) 0.0523(13) 0.0002(12) 0.0089(12) 0.0098(14) C9 0.0713(14) 0.0656(14) 0.0424(11) -0.0033(10) -0.0013(10) 0.0046(11) C10 0.0548(11) 0.0643(13) 0.0357(9) 0.0075(9) -0.0028(8) 0.0000(10) C11 0.0500(11) 0.0451(10) 0.0409(10) -0.0001(8) -0.0002(8) 0.0019(8) C12 0.0463(10) 0.0548(12) 0.0364(9) -0.0041(8) -0.0006(8) 0.0029(9) C13 0.0518(12) 0.0724(14) 0.0565(12) -0.0108(11) -0.0056(10) 0.0128(11) C14 0.0483(13) 0.114(2) 0.0622(14) -0.0174(15) -0.0002(11) 0.0169(14) C15 0.0447(13) 0.128(2) 0.0539(13) -0.0042(15) 0.0061(10) -0.0128(14) C16 0.0605(13) 0.0830(16) 0.0467(11) 0.0032(11) -0.0002(10) -0.0195(12) C17 0.0475(11) 0.0592(12) 0.0386(10) -0.0012(9) 0.0005(8) -0.0045(9) C18 0.0624(12) 0.0490(12) 0.0441(10) -0.0015(9) -0.0019(9) -0.0009(10) O1 0.0910(12) 0.0468(9) 0.0948(12) 0.0057(8) 0.0001(9) -0.0021(8) C19 0.0548(11) 0.0538(12) 0.0469(11) -0.0021(9) 0.0044(9) 0.0116(9) C20 0.0429(10) 0.0521(11) 0.0448(10) 0.0005(9) 0.0047(8) 0.0002(9) C21 0.0377(9) 0.0520(11) 0.0463(10) 0.0013(9) -0.0002(8) 0.0008(8) C22 0.0432(10) 0.0530(11) 0.0498(11) 0.0039(9) -0.0013(8) -0.0026(9) C23 0.0405(10) 0.0523(12) 0.0531(11) -0.0058(9) -0.0045(8) -0.0010(9) O24 0.0732(10) 0.0583(9) 0.0587(9) -0.0092(7) -0.0090(7) -0.0040(7) C25 0.0726(15) 0.0746(16) 0.0580(13) -0.0141(12) -0.0087(11) 0.0032(12) O26 0.0814(10) 0.0736(10) 0.0472(8) -0.0060(7) -0.0065(7) -0.0001(8) C27 0.0532(12) 0.0637(14) 0.0425(10) -0.0023(10) -0.0053(9) -0.0003(10) C28 0.0765(15) 0.0616(14) 0.0486(12) 0.0080(10) -0.0050(10) -0.0015(11) C29 0.0612(13) 0.0513(12) 0.0497(11) 0.0013(9) -0.0041(9) -0.0003(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 N1 N2 1.416(2) . ? N1 C11 1.482(2) . ? N1 H1 0.87(2) . ? N2 C10 1.368(3) . ? N2 C3 1.381(3) . ? C3 C4 1.351(3) . ? C3 H3 0.9400 . ? C4 C5 1.440(3) . ? C4 H4 0.9400 . ? C5 C6 1.400(3) . ? C5 C10 1.400(3) . ? C6 C7 1.373(4) . ? C6 H6 0.9400 . ? C7 C8 1.400(4) . ? C7 H7 0.9400 . ? C8 C9 1.368(3) . ? C8 H8 0.9400 . ? C9 C10 1.403(3) . ? C9 H9 0.9400 . ? C11 C12 1.502(3) . ? C11 C20 1.537(3) . ? C11 H11 0.9900 . ? C12 C13 1.390(3) . ? C12 C17 1.397(3) . ? C13 C14 1.384(3) . ? C13 H13 0.9400 . ? C14 C15 1.370(4) . ? C14 H14 0.9400 . ? C15 C16 1.378(4) . ? C15 H15 0.9400 . ? C16 C17 1.400(3) . ? C16 H16 0.9400 . ? C17 C18 1.480(3) . ? C18 O1 1.221(2) . ? C18 C19 1.500(3) . ? C19 C20 1.526(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.523(3) . ? C20 H20 0.9900 . ? C21 C29 1.386(3) . ? C21 C22 1.411(3) . ? C22 C23 1.361(3) . ? C22 H22 0.9400 . ? C23 C27 1.376(3) . ? C23 O24 1.383(2) . ? O24 C25 1.432(3) . ? C25 O26 1.424(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? O26 C27 1.388(2) . ? C27 C28 1.357(3) . ? C28 C29 1.399(3) . ? C28 H28 0.9400 . ? C29 H29 0.9400 . ? 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 N2 N1 C11 111.66(15) . . ? N2 N1 H1 106.2(15) . . ? C11 N1 H1 110.3(15) . . ? C10 N2 C3 108.99(18) . . ? C10 N2 N1 122.90(17) . . ? C3 N2 N1 127.82(18) . . ? C4 C3 N2 109.7(2) . . ? C4 C3 H3 125.2 . . ? N2 C3 H3 125.2 . . ? C3 C4 C5 106.9(2) . . ? C3 C4 H4 126.6 . . ? C5 C4 H4 126.6 . . ? C6 C5 C10 119.1(2) . . ? C6 C5 C4 134.1(2) . . ? C10 C5 C4 106.8(2) . . ? C7 C6 C5 118.3(2) . . ? C7 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? C6 C7 C8 121.8(2) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? C9 C8 C7 121.4(3) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C10 116.9(2) . . ? C8 C9 H9 121.6 . . ? C10 C9 H9 121.6 . . ? N2 C10 C5 107.67(19) . . ? N2 C10 C9 129.8(2) . . ? C5 C10 C9 122.5(2) . . ? N1 C11 C12 107.06(14) . . ? N1 C11 C20 110.08(15) . . ? C12 C11 C20 111.93(15) . . ? N1 C11 H11 109.2 . . ? C12 C11 H11 109.2 . . ? C20 C11 H11 109.2 . . ? C13 C12 C17 119.41(19) . . ? C13 C12 C11 119.84(19) . . ? C17 C12 C11 120.75(17) . . ? C14 C13 C12 120.0(2) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.6(2) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.4(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 119.8(2) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C12 C17 C16 119.7(2) . . ? C12 C17 C18 120.42(17) . . ? C16 C17 C18 119.8(2) . . ? O1 C18 C17 121.0(2) . . ? O1 C18 C19 120.64(19) . . ? C17 C18 C19 118.32(17) . . ? C18 C19 C20 114.14(16) . . ? C18 C19 H19A 108.7 . . ? C20 C19 H19A 108.7 . . ? C18 C19 H19B 108.7 . . ? C20 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C21 C20 C19 114.58(16) . . ? C21 C20 C11 110.61(15) . . ? C19 C20 C11 108.62(16) . . ? C21 C20 H20 107.6 . . ? C19 C20 H20 107.6 . . ? C11 C20 H20 107.6 . . ? C29 C21 C22 118.90(18) . . ? C29 C21 C20 123.04(17) . . ? C22 C21 C20 118.05(17) . . ? C23 C22 C21 117.68(18) . . ? C23 C22 H22 121.2 . . ? C21 C22 H22 121.2 . . ? C22 C23 C27 122.51(19) . . ? C22 C23 O24 127.93(19) . . ? C27 C23 O24 109.55(17) . . ? C23 O24 C25 104.75(16) . . ? O26 C25 O24 107.93(17) . . ? O26 C25 H25A 110.1 . . ? O24 C25 H25A 110.1 . . ? O26 C25 H25B 110.1 . . ? O24 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? C27 O26 C25 104.56(16) . . ? C28 C27 C23 121.43(19) . . ? C28 C27 O26 128.71(19) . . ? C23 C27 O26 109.84(18) . . ? C27 C28 C29 117.1(2) . . ? C27 C28 H28 121.4 . . ? C29 C28 H28 121.4 . . ? C21 C29 C28 122.2(2) . . ? C21 C29 H29 118.9 . . ? C28 C29 H29 118.9 . . ? 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 C11 N1 N2 C10 -123.78(18) . . . . ? C11 N1 N2 C3 49.3(3) . . . . ? C10 N2 C3 C4 -0.3(2) . . . . ? N1 N2 C3 C4 -174.12(18) . . . . ? N2 C3 C4 C5 0.2(2) . . . . ? C3 C4 C5 C6 179.5(2) . . . . ? C3 C4 C5 C10 -0.1(2) . . . . ? C10 C5 C6 C7 0.4(3) . . . . ? C4 C5 C6 C7 -179.2(2) . . . . ? C5 C6 C7 C8 -1.5(4) . . . . ? C6 C7 C8 C9 1.3(4) . . . . ? C7 C8 C9 C10 0.0(3) . . . . ? C3 N2 C10 C5 0.2(2) . . . . ? N1 N2 C10 C5 174.39(16) . . . . ? C3 N2 C10 C9 179.4(2) . . . . ? N1 N2 C10 C9 -6.4(3) . . . . ? C6 C5 C10 N2 -179.76(18) . . . . ? C4 C5 C10 N2 0.0(2) . . . . ? C6 C5 C10 C9 0.9(3) . . . . ? C4 C5 C10 C9 -179.34(18) . . . . ? C8 C9 C10 N2 179.7(2) . . . . ? C8 C9 C10 C5 -1.2(3) . . . . ? N2 N1 C11 C12 -168.96(15) . . . . ? N2 N1 C11 C20 69.2(2) . . . . ? N1 C11 C12 C13 88.9(2) . . . . ? C20 C11 C12 C13 -150.38(17) . . . . ? N1 C11 C12 C17 -90.40(19) . . . . ? C20 C11 C12 C17 30.3(2) . . . . ? C17 C12 C13 C14 -0.8(3) . . . . ? C11 C12 C13 C14 179.90(18) . . . . ? C12 C13 C14 C15 -0.5(3) . . . . ? C13 C14 C15 C16 1.4(4) . . . . ? C14 C15 C16 C17 -1.0(3) . . . . ? C13 C12 C17 C16 1.2(3) . . . . ? C11 C12 C17 C16 -179.50(17) . . . . ? C13 C12 C17 C18 -178.70(17) . . . . ? C11 C12 C17 C18 0.6(3) . . . . ? C15 C16 C17 C12 -0.3(3) . . . . ? C15 C16 C17 C18 179.59(19) . . . . ? C12 C17 C18 O1 174.13(19) . . . . ? C16 C17 C18 O1 -5.8(3) . . . . ? C12 C17 C18 C19 -4.4(3) . . . . ? C16 C17 C18 C19 175.74(17) . . . . ? O1 C18 C19 C20 157.88(19) . . . . ? C17 C18 C19 C20 -23.6(2) . . . . ? C18 C19 C20 C21 -71.6(2) . . . . ? C18 C19 C20 C11 52.6(2) . . . . ? N1 C11 C20 C21 -169.96(15) . . . . ? C12 C11 C20 C21 71.1(2) . . . . ? N1 C11 C20 C19 63.48(19) . . . . ? C12 C11 C20 C19 -55.5(2) . . . . ? C19 C20 C21 C29 2.0(3) . . . . ? C11 C20 C21 C29 -121.14(19) . . . . ? C19 C20 C21 C22 -178.63(16) . . . . ? C11 C20 C21 C22 58.2(2) . . . . ? C29 C21 C22 C23 3.0(3) . . . . ? C20 C21 C22 C23 -176.38(16) . . . . ? C21 C22 C23 C27 -2.3(3) . . . . ? C21 C22 C23 O24 178.65(18) . . . . ? C22 C23 O24 C25 -170.2(2) . . . . ? C27 C23 O24 C25 10.6(2) . . . . ? C23 O24 C25 O26 -17.7(2) . . . . ? O24 C25 O26 C27 18.0(2) . . . . ? C22 C23 C27 C28 -0.1(3) . . . . ? O24 C23 C27 C28 179.1(2) . . . . ? C22 C23 C27 O26 -178.64(17) . . . . ? O24 C23 C27 O26 0.6(2) . . . . ? C25 O26 C27 C28 170.1(2) . . . . ? C25 O26 C27 C23 -11.5(2) . . . . ? C23 C27 C28 C29 1.7(3) . . . . ? O26 C27 C28 C29 179.9(2) . . . . ? C22 C21 C29 C28 -1.5(3) . . . . ? C20 C21 C29 C28 177.88(19) . . . . ? C27 C28 C29 C21 -0.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 66.98 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.250 _refine_diff_density_min -0.156 _refine_diff_density_rms 0.035