data_07090 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 07090 _chemical_melting_point ? _chemical_formula_moiety 'C29 H29 N O4' _chemical_formula_sum 'C29 H29 N O4' _chemical_formula_weight 455.53 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' 'N' 'N' 0.0061 0.0033 '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 P2(1)/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 9.6172(9) _cell_length_b 17.9956(16) _cell_length_c 14.5480(13) _cell_angle_alpha 90.00 _cell_angle_beta 102.988(2) _cell_angle_gamma 90.00 _cell_volume 2453.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3428 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.34 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9603 _exptl_absorpt_correction_T_max 0.9642 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28174 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5609 _reflns_number_gt 4334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _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^)+(0.0558P)^2^+0.7461P] 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_number_reflns 5609 _refine_ls_number_parameters 317 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.023 _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 0.85177(11) 0.06128(6) 0.54702(7) 0.0448(3) Uani 1 1 d . . . O2 O 1.03776(10) 0.17421(5) 0.69440(7) 0.0388(2) Uani 1 1 d . B . O3 O 0.53287(11) 0.17616(6) 0.63060(8) 0.0524(3) Uani 1 1 d . . . O4 O 0.58170(9) 0.10291(5) 0.51585(6) 0.0349(2) Uani 1 1 d . . . N1 N 0.72840(11) 0.10043(6) 0.65883(7) 0.0298(2) Uani 1 1 d . . . C1 C 0.46393(14) 0.13015(8) 0.43842(10) 0.0389(3) Uani 1 1 d . . . C2 C 0.4937(3) 0.21025(10) 0.41837(15) 0.0760(6) Uani 1 1 d . . . H2A H 0.4826 0.2413 0.4716 0.114 Uiso 1 1 calc R . . H2B H 0.4264 0.2266 0.3610 0.114 Uiso 1 1 calc R . . H2C H 0.5914 0.2148 0.4096 0.114 Uiso 1 1 calc R . . C3 C 0.32289(17) 0.11691(14) 0.46435(14) 0.0721(6) Uani 1 1 d . . . H3A H 0.3184 0.0654 0.4855 0.108 Uiso 1 1 calc R . . H3B H 0.2451 0.1259 0.4092 0.108 Uiso 1 1 calc R . . H3C H 0.3134 0.1508 0.5153 0.108 Uiso 1 1 calc R . . C4 C 0.47915(19) 0.08079(10) 0.35723(11) 0.0519(4) Uani 1 1 d . . . H4A H 0.4662 0.0288 0.3734 0.078 Uiso 1 1 calc R . . H4B H 0.5744 0.0873 0.3447 0.078 Uiso 1 1 calc R . . H4C H 0.4067 0.0943 0.3008 0.078 Uiso 1 1 calc R . . C5 C 0.60387(13) 0.13127(7) 0.60112(9) 0.0323(3) Uani 1 1 d . . . C6 C 0.76405(14) 0.10639(7) 0.75919(9) 0.0316(3) Uani 1 1 d . . . C7 C 0.68095(17) 0.13351(8) 0.81780(10) 0.0436(3) Uani 1 1 d . . . H7 H 0.5885 0.1532 0.7930 0.052 Uiso 1 1 calc R . . C8 C 0.7377(2) 0.13082(9) 0.91438(11) 0.0490(4) Uani 1 1 d . . . H8 H 0.6832 0.1494 0.9563 0.059 Uiso 1 1 calc R . . C9 C 0.87187(19) 0.10176(8) 0.95075(10) 0.0462(4) Uani 1 1 d . . . H9 H 0.9082 0.1004 1.0171 0.055 Uiso 1 1 calc R . . C10 C 0.95356(16) 0.07454(7) 0.89110(9) 0.0391(3) Uani 1 1 d . . . H10 H 1.0455 0.0543 0.9161 0.047 Uiso 1 1 calc R . . C11 C 0.89955(14) 0.07712(7) 0.79445(9) 0.0311(3) Uani 1 1 d . . . C12 C 0.96317(13) 0.05113(7) 0.71462(9) 0.0301(3) Uani 1 1 d . B . C13 C 0.84373(13) 0.06961(7) 0.62719(9) 0.0307(3) Uani 1 1 d . . . C14 C 0.99599(13) -0.03222(7) 0.71403(9) 0.0313(3) Uani 1 1 d . . . C15 C 0.94787(15) -0.08091(7) 0.77417(10) 0.0362(3) Uani 1 1 d . . . H15 H 0.8983 -0.0621 0.8188 0.043 Uiso 1 1 calc R . . C16 C 0.97146(17) -0.15689(8) 0.76972(11) 0.0443(3) Uani 1 1 d . . . H16 H 0.9384 -0.1896 0.8114 0.053 Uiso 1 1 calc R . . C17 C 1.04275(16) -0.18489(8) 0.70492(12) 0.0459(4) Uani 1 1 d . . . H17 H 1.0599 -0.2368 0.7024 0.055 Uiso 1 1 calc R . . C18 C 1.08900(16) -0.13716(9) 0.64369(12) 0.0461(4) Uani 1 1 d . . . H18 H 1.1369 -0.1564 0.5984 0.055 Uiso 1 1 calc R . . C19 C 1.06588(15) -0.06137(8) 0.64787(11) 0.0401(3) Uani 1 1 d . . . H19 H 1.0979 -0.0290 0.6053 0.048 Uiso 1 1 calc R . . C20 C 1.09119(14) 0.10015(7) 0.70121(10) 0.0378(3) Uani 1 1 d D . . H20 H 1.1099 0.0872 0.6382 0.045 Uiso 1 1 calc R A 1 C21 C 1.2279(2) 0.08691(12) 0.77312(16) 0.0396(5) Uani 0.776(3) 1 d PD B 1 H21A H 1.2766 0.0412 0.7709 0.048 Uiso 0.776(3) 1 calc PR B 1 C22 C 1.2834(2) 0.13496(12) 0.83859(15) 0.0472(5) Uani 0.776(3) 1 d PD B 1 H22A H 1.2369 0.1811 0.8424 0.057 Uiso 0.776(3) 1 calc PR B 1 H22B H 1.3701 0.1238 0.8823 0.057 Uiso 0.776(3) 1 calc PR B 1 C21' C 1.2004(8) 0.1099(5) 0.7985(6) 0.0396(5) Uani 0.224(3) 1 d PD B 2 H21' H 1.1737 0.1274 0.8537 0.048 Uiso 0.224(3) 1 calc PR B 2 C22' C 1.3337(7) 0.0915(4) 0.7965(5) 0.0472(5) Uani 0.224(3) 1 d PD B 2 H22C H 1.3552 0.0743 0.7395 0.057 Uiso 0.224(3) 1 calc PR B 2 H22D H 1.4074 0.0956 0.8520 0.057 Uiso 0.224(3) 1 calc PR B 2 C23 C 1.10238(16) 0.22122(9) 0.63684(13) 0.0488(4) Uani 1 1 d . . . H23A H 1.1018 0.1965 0.5760 0.059 Uiso 1 1 calc R B . H23B H 1.2026 0.2317 0.6689 0.059 Uiso 1 1 calc R . . C24 C 1.01869(15) 0.29269(8) 0.61997(10) 0.0393(3) Uani 1 1 d . B . C25 C 0.87088(17) 0.29084(9) 0.59280(12) 0.0489(4) Uani 1 1 d . . . H25 H 0.8226 0.2444 0.5875 0.059 Uiso 1 1 calc R B . C26 C 0.79321(19) 0.35574(10) 0.57340(13) 0.0545(4) Uani 1 1 d . B . H26 H 0.6920 0.3537 0.5559 0.065 Uiso 1 1 calc R . . C27 C 0.8615(2) 0.42305(9) 0.57924(12) 0.0565(4) Uani 1 1 d . . . H27 H 0.8079 0.4676 0.5652 0.068 Uiso 1 1 calc R B . C28 C 1.0078(2) 0.42565(9) 0.60553(12) 0.0556(4) Uani 1 1 d . B . H28 H 1.0554 0.4722 0.6090 0.067 Uiso 1 1 calc R . . C29 C 1.08666(18) 0.36087(9) 0.62702(10) 0.0454(4) Uani 1 1 d . . . H29 H 1.1877 0.3634 0.6466 0.054 Uiso 1 1 calc R B . 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 0.0413(5) 0.0641(7) 0.0290(5) 0.0026(4) 0.0078(4) 0.0164(5) O2 0.0463(6) 0.0312(5) 0.0413(5) 0.0095(4) 0.0148(4) -0.0011(4) O3 0.0442(6) 0.0563(7) 0.0502(6) -0.0185(5) -0.0034(5) 0.0205(5) O4 0.0328(5) 0.0363(5) 0.0319(5) -0.0017(4) -0.0008(4) 0.0067(4) N1 0.0300(5) 0.0304(5) 0.0279(5) -0.0006(4) 0.0044(4) 0.0024(4) C1 0.0331(7) 0.0410(7) 0.0364(7) 0.0018(6) -0.0055(5) 0.0045(6) C2 0.0992(16) 0.0423(10) 0.0693(13) 0.0140(9) -0.0175(11) 0.0054(10) C3 0.0309(8) 0.1238(18) 0.0566(11) -0.0224(11) -0.0005(7) -0.0009(9) C4 0.0542(9) 0.0627(10) 0.0337(8) -0.0014(7) -0.0007(7) 0.0051(8) C5 0.0289(6) 0.0290(6) 0.0368(7) -0.0030(5) 0.0029(5) 0.0007(5) C6 0.0368(7) 0.0277(6) 0.0301(6) -0.0012(5) 0.0071(5) -0.0032(5) C7 0.0489(8) 0.0437(8) 0.0409(8) -0.0031(6) 0.0158(6) 0.0038(6) C8 0.0709(11) 0.0444(8) 0.0370(8) -0.0069(6) 0.0232(7) -0.0034(8) C9 0.0711(11) 0.0377(8) 0.0279(7) -0.0014(6) 0.0070(7) -0.0117(7) C10 0.0501(8) 0.0321(7) 0.0311(7) 0.0023(5) 0.0006(6) -0.0079(6) C11 0.0362(7) 0.0248(6) 0.0307(6) 0.0016(5) 0.0045(5) -0.0048(5) C12 0.0279(6) 0.0320(6) 0.0290(6) 0.0056(5) 0.0031(5) 0.0000(5) C13 0.0300(6) 0.0307(6) 0.0306(7) 0.0030(5) 0.0053(5) 0.0026(5) C14 0.0262(6) 0.0318(6) 0.0333(6) 0.0035(5) 0.0013(5) 0.0013(5) C15 0.0378(7) 0.0333(7) 0.0370(7) 0.0030(5) 0.0074(6) -0.0001(5) C16 0.0489(8) 0.0329(7) 0.0509(9) 0.0076(6) 0.0105(7) -0.0014(6) C17 0.0407(8) 0.0327(7) 0.0620(10) -0.0004(7) 0.0065(7) 0.0056(6) C18 0.0393(8) 0.0445(8) 0.0559(9) -0.0037(7) 0.0139(7) 0.0061(6) C19 0.0375(7) 0.0399(7) 0.0448(8) 0.0041(6) 0.0134(6) 0.0035(6) C20 0.0322(7) 0.0339(7) 0.0454(8) 0.0112(6) 0.0050(6) -0.0003(5) C21 0.0279(10) 0.0388(12) 0.0515(13) 0.0082(9) 0.0078(8) 0.0015(8) C22 0.0345(10) 0.0558(12) 0.0502(11) 0.0104(9) 0.0072(8) -0.0059(8) C21' 0.0279(10) 0.0388(12) 0.0515(13) 0.0082(9) 0.0078(8) 0.0015(8) C22' 0.0345(10) 0.0558(12) 0.0502(11) 0.0104(9) 0.0072(8) -0.0059(8) C23 0.0395(8) 0.0436(8) 0.0660(10) 0.0239(7) 0.0176(7) 0.0020(6) C24 0.0416(7) 0.0388(7) 0.0388(7) 0.0124(6) 0.0122(6) -0.0004(6) C25 0.0432(8) 0.0400(8) 0.0636(10) 0.0142(7) 0.0124(7) 0.0000(6) C26 0.0484(9) 0.0542(10) 0.0619(10) 0.0143(8) 0.0142(8) 0.0122(7) C27 0.0767(12) 0.0411(9) 0.0517(10) 0.0052(7) 0.0146(9) 0.0171(8) C28 0.0811(13) 0.0344(8) 0.0483(9) -0.0011(7) 0.0085(8) -0.0069(8) C29 0.0515(9) 0.0453(8) 0.0380(8) 0.0066(6) 0.0072(6) -0.0082(7) _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 C13 1.1955(15) . ? O2 C20 1.4238(16) . ? O2 C23 1.4273(16) . ? O3 C5 1.1977(16) . ? O4 C5 1.3138(15) . ? O4 C1 1.4895(15) . ? N1 C13 1.4069(16) . ? N1 C5 1.4125(16) . ? N1 C6 1.4267(16) . ? C1 C3 1.506(2) . ? C1 C2 1.511(2) . ? C1 C4 1.511(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 C7 1.3820(19) . ? C6 C11 1.3923(18) . ? C7 C8 1.389(2) . ? C7 H7 0.9500 . ? C8 C9 1.382(2) . ? C8 H8 0.9500 . ? C9 C10 1.384(2) . ? C9 H9 0.9500 . ? C10 C11 1.3859(18) . ? C10 H10 0.9500 . ? C11 C12 1.5037(18) . ? C12 C14 1.5333(18) . ? C12 C13 1.5464(17) . ? C12 C20 1.5621(18) . ? C14 C15 1.3890(18) . ? C14 C19 1.3942(19) . ? C15 C16 1.390(2) . ? C15 H15 0.9500 . ? C16 C17 1.380(2) . ? C16 H16 0.9500 . ? C17 C18 1.381(2) . ? C17 H17 0.9500 . ? C18 C19 1.386(2) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.504(2) . ? C20 C21' 1.572(8) . ? C20 H20 1.0000 . ? C21 C22 1.308(3) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C22 H22B 0.9500 . ? C21' C22' 1.332(9) . ? C21' H21' 0.9500 . ? C22' H22C 0.9500 . ? C22' H22D 0.9500 . ? C23 C24 1.508(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.383(2) . ? C24 C25 1.388(2) . ? C25 C26 1.381(2) . ? C25 H25 0.9500 . ? C26 C27 1.371(2) . ? C26 H26 0.9500 . ? C27 C28 1.374(3) . ? C27 H27 0.9500 . ? C28 C29 1.387(2) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? 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 C20 O2 C23 113.44(11) . . ? C5 O4 C1 121.38(10) . . ? C13 N1 C5 125.86(11) . . ? C13 N1 C6 109.80(10) . . ? C5 N1 C6 123.73(11) . . ? O4 C1 C3 109.45(13) . . ? O4 C1 C2 108.37(12) . . ? C3 C1 C2 114.82(16) . . ? O4 C1 C4 101.94(11) . . ? C3 C1 C4 110.71(14) . . ? C2 C1 C4 110.73(15) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 O4 127.99(12) . . ? O3 C5 N1 121.85(12) . . ? O4 C5 N1 110.16(10) . . ? C7 C6 C11 121.96(12) . . ? C7 C6 N1 128.21(12) . . ? C11 C6 N1 109.78(11) . . ? C6 C7 C8 117.47(14) . . ? C6 C7 H7 121.3 . . ? C8 C7 H7 121.3 . . ? C9 C8 C7 121.42(14) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C10 120.41(13) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C11 119.21(14) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C10 C11 C6 119.53(13) . . ? C10 C11 C12 130.42(12) . . ? C6 C11 C12 110.04(11) . . ? C11 C12 C14 115.38(10) . . ? C11 C12 C13 102.27(10) . . ? C14 C12 C13 108.75(10) . . ? C11 C12 C20 112.94(11) . . ? C14 C12 C20 112.50(10) . . ? C13 C12 C20 103.68(10) . . ? O1 C13 N1 126.68(12) . . ? O1 C13 C12 125.21(12) . . ? N1 C13 C12 108.06(10) . . ? C15 C14 C19 118.57(12) . . ? C15 C14 C12 121.02(12) . . ? C19 C14 C12 120.24(12) . . ? C16 C15 C14 120.68(13) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 120.17(14) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 119.68(14) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C19 120.39(14) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C14 120.50(13) . . ? C18 C19 H19 119.7 . . ? C14 C19 H19 119.7 . . ? O2 C20 C21 116.24(14) . . ? O2 C20 C12 104.78(10) . . ? C21 C20 C12 114.47(12) . . ? O2 C20 C21' 96.6(3) . . ? C21 C20 C21' 24.3(3) . . ? C12 C20 C21' 109.7(3) . . ? O2 C20 H20 106.9 . . ? C21 C20 H20 106.9 . . ? C12 C20 H20 106.9 . . ? C21' C20 H20 129.1 . . ? C22 C21 C20 123.5(2) . . ? C22 C21 H21A 118.3 . . ? C20 C21 H21A 118.3 . . ? C21 C22 H22A 120.0 . . ? C21 C22 H22B 120.0 . . ? H22A C22 H22B 120.0 . . ? C22' C21' C20 113.8(7) . . ? C22' C21' H21' 123.1 . . ? C20 C21' H21' 123.1 . . ? C21' C22' H22C 120.0 . . ? C21' C22' H22D 120.0 . . ? H22C C22' H22D 120.0 . . ? O2 C23 C24 108.31(12) . . ? O2 C23 H23A 110.0 . . ? C24 C23 H23A 110.0 . . ? O2 C23 H23B 110.0 . . ? C24 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? C29 C24 C25 118.64(14) . . ? C29 C24 C23 121.23(14) . . ? C25 C24 C23 120.07(14) . . ? C26 C25 C24 120.69(15) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 C25 120.34(16) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 119.57(15) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C27 C28 C29 120.53(15) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C24 C29 C28 120.22(15) . . ? C24 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? 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 C5 O4 C1 C3 -61.49(17) . . . . ? C5 O4 C1 C2 64.41(18) . . . . ? C5 O4 C1 C4 -178.75(12) . . . . ? C1 O4 C5 O3 5.7(2) . . . . ? C1 O4 C5 N1 -175.02(11) . . . . ? C13 N1 C5 O3 -155.99(14) . . . . ? C6 N1 C5 O3 14.2(2) . . . . ? C13 N1 C5 O4 24.64(17) . . . . ? C6 N1 C5 O4 -165.20(11) . . . . ? C13 N1 C6 C7 -179.89(13) . . . . ? C5 N1 C6 C7 8.6(2) . . . . ? C13 N1 C6 C11 -2.34(14) . . . . ? C5 N1 C6 C11 -173.88(11) . . . . ? C11 C6 C7 C8 0.2(2) . . . . ? N1 C6 C7 C8 177.46(13) . . . . ? C6 C7 C8 C9 -0.4(2) . . . . ? C7 C8 C9 C10 0.1(2) . . . . ? C8 C9 C10 C11 0.3(2) . . . . ? C9 C10 C11 C6 -0.51(19) . . . . ? C9 C10 C11 C12 -179.17(13) . . . . ? C7 C6 C11 C10 0.27(19) . . . . ? N1 C6 C11 C10 -177.46(11) . . . . ? C7 C6 C11 C12 179.18(12) . . . . ? N1 C6 C11 C12 1.45(14) . . . . ? C10 C11 C12 C14 60.79(18) . . . . ? C6 C11 C12 C14 -117.96(12) . . . . ? C10 C11 C12 C13 178.66(13) . . . . ? C6 C11 C12 C13 -0.10(13) . . . . ? C10 C11 C12 C20 -70.56(17) . . . . ? C6 C11 C12 C20 110.68(12) . . . . ? C5 N1 C13 O1 -4.0(2) . . . . ? C6 N1 C13 O1 -175.28(13) . . . . ? C5 N1 C13 C12 173.54(11) . . . . ? C6 N1 C13 C12 2.23(13) . . . . ? C11 C12 C13 O1 176.26(13) . . . . ? C14 C12 C13 O1 -61.25(17) . . . . ? C20 C12 C13 O1 58.65(17) . . . . ? C11 C12 C13 N1 -1.29(13) . . . . ? C14 C12 C13 N1 121.20(11) . . . . ? C20 C12 C13 N1 -118.90(11) . . . . ? C11 C12 C14 C15 10.12(17) . . . . ? C13 C12 C14 C15 -104.06(13) . . . . ? C20 C12 C14 C15 141.68(12) . . . . ? C11 C12 C14 C19 -174.71(11) . . . . ? C13 C12 C14 C19 71.12(15) . . . . ? C20 C12 C14 C19 -43.14(16) . . . . ? C19 C14 C15 C16 1.3(2) . . . . ? C12 C14 C15 C16 176.53(13) . . . . ? C14 C15 C16 C17 -0.3(2) . . . . ? C15 C16 C17 C18 -0.8(2) . . . . ? C16 C17 C18 C19 0.9(2) . . . . ? C17 C18 C19 C14 0.2(2) . . . . ? C15 C14 C19 C18 -1.2(2) . . . . ? C12 C14 C19 C18 -176.51(13) . . . . ? C23 O2 C20 C21 82.89(17) . . . . ? C23 O2 C20 C12 -149.70(12) . . . . ? C23 O2 C20 C21' 97.9(3) . . . . ? C11 C12 C20 O2 -52.68(13) . . . . ? C14 C12 C20 O2 174.55(10) . . . . ? C13 C12 C20 O2 57.23(13) . . . . ? C11 C12 C20 C21 75.82(17) . . . . ? C14 C12 C20 C21 -56.96(18) . . . . ? C13 C12 C20 C21 -174.28(14) . . . . ? C11 C12 C20 C21' 50.1(3) . . . . ? C14 C12 C20 C21' -82.7(3) . . . . ? C13 C12 C20 C21' 160.0(3) . . . . ? O2 C20 C21 C22 12.6(3) . . . . ? C12 C20 C21 C22 -109.8(2) . . . . ? C21' C20 C21 C22 -26.1(7) . . . . ? O2 C20 C21' C22' -124.9(6) . . . . ? C21 C20 C21' C22' 20.7(5) . . . . ? C12 C20 C21' C22' 126.8(6) . . . . ? C20 O2 C23 C24 169.30(12) . . . . ? O2 C23 C24 C29 135.62(14) . . . . ? O2 C23 C24 C25 -47.2(2) . . . . ? C29 C24 C25 C26 -0.1(2) . . . . ? C23 C24 C25 C26 -177.36(15) . . . . ? C24 C25 C26 C27 1.1(3) . . . . ? C25 C26 C27 C28 -0.7(3) . . . . ? C26 C27 C28 C29 -0.6(3) . . . . ? C25 C24 C29 C28 -1.2(2) . . . . ? C23 C24 C29 C28 176.02(15) . . . . ? C27 C28 C29 C24 1.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.282 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.036