data_06158 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H29 N O5' _chemical_formula_sum 'C28 H29 N O5' _chemical_formula_weight 459.52 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5658(7) _cell_length_b 11.1733(4) _cell_length_c 11.7745(6) _cell_angle_alpha 69.202(3) _cell_angle_beta 75.052(2) _cell_angle_gamma 74.595(3) _cell_volume 1231.95(11) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4979 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9588 _exptl_absorpt_correction_T_max 0.9709 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9841 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4329 _reflns_number_gt 2716 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0787P)^2^+0.1500P] 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 4329 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0979 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.43888(15) 0.28178(13) 0.22726(14) 0.0488(4) Uani 1 1 d . . . N2 N 0.31133(18) 0.37231(15) 0.21891(16) 0.0434(5) Uani 1 1 d . . . C3 C 0.3399(2) 0.50521(18) 0.18440(19) 0.0416(5) Uani 1 1 d . . . H3A H 0.4051 0.5194 0.1071 0.050 Uiso 1 1 calc R . . C4 C 0.4036(2) 0.51478(18) 0.28690(19) 0.0404(5) Uani 1 1 d . . . C5 C 0.5200(2) 0.39629(19) 0.3226(2) 0.0426(5) Uani 1 1 d . . . H5A H 0.5372 0.3915 0.4021 0.051 Uiso 1 1 calc R . . C6 C 0.4760(2) 0.26948(19) 0.3391(2) 0.0441(5) Uani 1 1 d . . . H6A H 0.3983 0.2585 0.4060 0.053 Uiso 1 1 calc R . . C21 C 0.2731(3) 0.3539(2) 0.1153(2) 0.0513(6) Uani 1 1 d . . . H21A H 0.3498 0.3532 0.0490 0.062 Uiso 1 1 calc R . . H21B H 0.2039 0.4267 0.0842 0.062 Uiso 1 1 calc R . . C22 C 0.22317(16) 0.22890(12) 0.15323(15) 0.0490(6) Uani 1 1 d G . . C23 C 0.09656(15) 0.22048(16) 0.22429(17) 0.0674(7) Uani 1 1 d G . . H23A H 0.0448 0.2909 0.2500 0.081 Uiso 1 1 calc R . . C24 C 0.04737(17) 0.1068(2) 0.25699(18) 0.0873(10) Uani 1 1 d G . . H24A H -0.0373 0.1012 0.3045 0.105 Uiso 1 1 calc R . . C25 C 0.1248(2) 0.00152(15) 0.2186(2) 0.0901(10) Uani 1 1 d G . . H25A H 0.0919 -0.0745 0.2405 0.108 Uiso 1 1 calc R . . C26 C 0.2514(2) 0.00994(13) 0.1476(2) 0.0882(10) Uani 1 1 d G . . H26A H 0.3032 -0.0605 0.1219 0.106 Uiso 1 1 calc R . . C27 C 0.30060(15) 0.12363(16) 0.11487(17) 0.0669(7) Uani 1 1 d G . . H27A H 0.3853 0.1293 0.0673 0.080 Uiso 1 1 calc R . . C31 C 0.21164(12) 0.60329(13) 0.16039(13) 0.0456(6) Uani 1 1 d G . . C32 C 0.09152(15) 0.58236(14) 0.23998(12) 0.0579(7) Uani 1 1 d G . . H32A H 0.0905 0.5118 0.3119 0.069 Uiso 1 1 calc R . . C33 C -0.02700(12) 0.66689(18) 0.21204(16) 0.0734(8) Uani 1 1 d G . . H33A H -0.1074 0.6529 0.2653 0.088 Uiso 1 1 calc R . . C34 C -0.02541(14) 0.77236(16) 0.10450(18) 0.0793(9) Uani 1 1 d G . . H34A H -0.1047 0.8289 0.0858 0.095 Uiso 1 1 calc R . . C35 C 0.09470(18) 0.79329(13) 0.02491(14) 0.0706(8) Uani 1 1 d G . . H35A H 0.0958 0.8639 -0.0470 0.085 Uiso 1 1 calc R . . C36 C 0.21322(14) 0.70876(14) 0.05285(12) 0.0539(6) Uani 1 1 d G . . H36A H 0.2936 0.7228 -0.0004 0.065 Uiso 1 1 calc R . . C41 C 0.4626(2) 0.6380(2) 0.2341(2) 0.0439(6) Uani 1 1 d . . . O42 O 0.46826(16) 0.70877(14) 0.12944(15) 0.0556(5) Uani 1 1 d . . . O43 O 0.51562(16) 0.65393(14) 0.31750(14) 0.0544(4) Uani 1 1 d . . . C44 C 0.5868(3) 0.7606(2) 0.2728(3) 0.0680(8) Uani 1 1 d . . . H44A H 0.6203 0.7652 0.3392 0.102 Uiso 1 1 calc R . . H44B H 0.5274 0.8409 0.2413 0.102 Uiso 1 1 calc R . . H44C H 0.6601 0.7464 0.2080 0.102 Uiso 1 1 calc R . . C45 C 0.2985(2) 0.5243(2) 0.4016(2) 0.0467(6) Uani 1 1 d . . . O46 O 0.26657(18) 0.43410(16) 0.48681(15) 0.0665(5) Uani 1 1 d . . . O47 O 0.24241(16) 0.64854(14) 0.39347(14) 0.0578(5) Uani 1 1 d . . . C48 C 0.1380(3) 0.6711(3) 0.4947(3) 0.0804(9) Uani 1 1 d . . . H48A H 0.1058 0.7632 0.4795 0.121 Uiso 1 1 calc R . . H48B H 0.1728 0.6350 0.5701 0.121 Uiso 1 1 calc R . . H48C H 0.0659 0.6301 0.5018 0.121 Uiso 1 1 calc R . . C51 C 0.6495(2) 0.4106(2) 0.2278(2) 0.0557(6) Uani 1 1 d . . . H51A H 0.7180 0.3362 0.2538 0.084 Uiso 1 1 calc R . . H51B H 0.6770 0.4884 0.2213 0.084 Uiso 1 1 calc R . . H51C H 0.6348 0.4162 0.1488 0.084 Uiso 1 1 calc R . . C61 C 0.58406(14) 0.14994(12) 0.36778(14) 0.0481(6) Uani 1 1 d G . . C62 C 0.64217(17) 0.07937(15) 0.28486(14) 0.0600(7) Uani 1 1 d G . . H62A H 0.6163 0.1070 0.2084 0.072 Uiso 1 1 calc R . . C63 C 0.73896(17) -0.03248(15) 0.31619(19) 0.0776(9) Uani 1 1 d G . . H63A H 0.7778 -0.0797 0.2607 0.093 Uiso 1 1 calc R . . C64 C 0.77764(15) -0.07378(13) 0.4304(2) 0.0846(10) Uani 1 1 d G . . H64A H 0.8424 -0.1486 0.4514 0.102 Uiso 1 1 calc R . . C65 C 0.7195(2) -0.00321(18) 0.51335(16) 0.0877(10) Uani 1 1 d G . . H65A H 0.7454 -0.0308 0.5898 0.105 Uiso 1 1 calc R . . C66 C 0.62274(18) 0.10865(17) 0.48203(14) 0.0724(8) Uani 1 1 d G . . H66A H 0.5839 0.1559 0.5375 0.087 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 0.0489(10) 0.0421(8) 0.0562(10) -0.0181(7) -0.0137(7) -0.0019(7) N2 0.0438(11) 0.0369(10) 0.0506(11) -0.0124(8) -0.0134(9) -0.0066(8) C3 0.0442(13) 0.0381(11) 0.0419(12) -0.0114(9) -0.0052(10) -0.0105(10) C4 0.0408(13) 0.0367(11) 0.0419(12) -0.0116(9) -0.0034(10) -0.0090(9) C5 0.0396(13) 0.0424(12) 0.0448(13) -0.0132(10) -0.0088(10) -0.0057(10) C6 0.0446(14) 0.0401(12) 0.0444(13) -0.0113(10) -0.0092(10) -0.0045(10) C21 0.0589(16) 0.0474(13) 0.0507(14) -0.0111(11) -0.0151(12) -0.0159(11) C22 0.0548(16) 0.0472(13) 0.0504(14) -0.0120(10) -0.0212(12) -0.0117(11) C23 0.0631(19) 0.0700(17) 0.0739(18) -0.0193(14) -0.0117(14) -0.0255(14) C24 0.088(2) 0.095(2) 0.088(2) -0.0136(18) -0.0206(18) -0.049(2) C25 0.121(3) 0.066(2) 0.099(2) -0.0034(17) -0.049(2) -0.047(2) C26 0.121(3) 0.0473(16) 0.114(3) -0.0264(16) -0.059(2) -0.0071(17) C27 0.0729(19) 0.0541(15) 0.0794(19) -0.0238(13) -0.0222(15) -0.0086(13) C31 0.0461(14) 0.0435(12) 0.0486(13) -0.0159(10) -0.0134(11) -0.0040(10) C32 0.0468(16) 0.0619(15) 0.0582(16) -0.0129(12) -0.0108(12) -0.0059(12) C33 0.0486(17) 0.088(2) 0.079(2) -0.0291(16) -0.0142(14) 0.0009(14) C34 0.065(2) 0.081(2) 0.092(2) -0.0330(17) -0.0363(18) 0.0152(16) C35 0.085(2) 0.0546(16) 0.0678(18) -0.0113(13) -0.0329(17) 0.0014(14) C36 0.0619(17) 0.0481(14) 0.0519(15) -0.0126(11) -0.0181(12) -0.0075(12) C41 0.0393(13) 0.0441(13) 0.0474(14) -0.0186(11) -0.0020(11) -0.0063(10) O42 0.0605(11) 0.0495(9) 0.0557(11) -0.0114(8) -0.0082(8) -0.0176(8) O43 0.0592(11) 0.0530(9) 0.0586(10) -0.0191(8) -0.0109(8) -0.0203(8) C44 0.0672(18) 0.0615(16) 0.085(2) -0.0246(14) -0.0091(15) -0.0302(14) C45 0.0449(14) 0.0467(13) 0.0475(14) -0.0165(11) -0.0069(11) -0.0058(11) O46 0.0697(12) 0.0547(10) 0.0531(10) -0.0072(8) 0.0072(9) -0.0067(9) O47 0.0565(11) 0.0518(10) 0.0574(10) -0.0238(8) 0.0043(8) -0.0026(8) C48 0.073(2) 0.0834(19) 0.0742(19) -0.0404(15) 0.0111(16) 0.0017(15) C51 0.0429(15) 0.0510(14) 0.0688(17) -0.0181(12) -0.0055(12) -0.0066(11) C61 0.0416(14) 0.0381(12) 0.0584(15) -0.0098(10) -0.0038(11) -0.0095(10) C62 0.0572(16) 0.0426(13) 0.0812(18) -0.0221(12) -0.0117(14) -0.0080(12) C63 0.0544(18) 0.0503(16) 0.132(3) -0.0388(17) -0.0101(18) -0.0072(13) C64 0.0482(18) 0.0492(16) 0.140(3) -0.0071(18) -0.0231(19) -0.0069(13) C65 0.070(2) 0.076(2) 0.091(2) 0.0027(17) -0.0283(18) 0.0020(16) C66 0.0686(19) 0.0688(17) 0.0635(18) -0.0108(13) -0.0185(15) 0.0068(14) _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 C6 1.420(3) . ? O1 N2 1.457(2) . ? N2 C21 1.473(3) . ? N2 C3 1.486(2) . ? C3 C31 1.518(2) . ? C3 C4 1.572(3) . ? C3 H3A 0.9800 . ? C4 C41 1.523(3) . ? C4 C45 1.527(3) . ? C4 C5 1.565(3) . ? C5 C51 1.531(3) . ? C5 C6 1.540(3) . ? C5 H5A 0.9800 . ? C6 C61 1.507(2) . ? C6 H6A 0.9800 . ? C21 C22 1.502(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C23 H23A 0.9300 . ? C24 C25 1.3900 . ? C24 H24A 0.9300 . ? C25 C26 1.3900 . ? C25 H25A 0.9300 . ? C26 C27 1.3900 . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C32 H32A 0.9300 . ? C33 C34 1.3900 . ? C33 H33A 0.9300 . ? C34 C35 1.3900 . ? C34 H34A 0.9300 . ? C35 C36 1.3900 . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C41 O42 1.201(2) . ? C41 O43 1.331(3) . ? O43 C44 1.445(3) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 O46 1.193(2) . ? C45 O47 1.337(3) . ? O47 C48 1.445(3) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C62 H62A 0.9300 . ? C63 C64 1.3900 . ? C63 H63A 0.9300 . ? C64 C65 1.3900 . ? C64 H64A 0.9300 . ? C65 C66 1.3900 . ? C65 H65A 0.9300 . ? C66 H66A 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 C6 O1 N2 107.80(14) . . ? O1 N2 C21 101.41(15) . . ? O1 N2 C3 106.67(15) . . ? C21 N2 C3 110.70(16) . . ? N2 C3 C31 108.08(16) . . ? N2 C3 C4 109.77(16) . . ? C31 C3 C4 114.53(16) . . ? N2 C3 H3A 108.1 . . ? C31 C3 H3A 108.1 . . ? C4 C3 H3A 108.1 . . ? C41 C4 C45 108.65(16) . . ? C41 C4 C5 107.53(17) . . ? C45 C4 C5 110.19(17) . . ? C41 C4 C3 107.83(17) . . ? C45 C4 C3 111.13(18) . . ? C5 C4 C3 111.38(16) . . ? C51 C5 C6 110.88(17) . . ? C51 C5 C4 112.47(17) . . ? C6 C5 C4 109.24(17) . . ? C51 C5 H5A 108.0 . . ? C6 C5 H5A 108.0 . . ? C4 C5 H5A 108.0 . . ? O1 C6 C61 108.42(16) . . ? O1 C6 C5 107.91(16) . . ? C61 C6 C5 113.27(17) . . ? O1 C6 H6A 109.1 . . ? C61 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N2 C21 C22 111.93(17) . . ? N2 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? N2 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C27 120.0 . . ? C23 C22 C21 119.33(14) . . ? C27 C22 C21 120.64(14) . . ? C24 C23 C22 120.0 . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C22 120.0 . . ? C26 C27 H27A 120.0 . . ? C22 C27 H27A 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 C3 120.34(12) . . ? C36 C31 C3 119.46(12) . . ? C33 C32 C31 120.0 . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36A 120.0 . . ? C31 C36 H36A 120.0 . . ? O42 C41 O43 123.4(2) . . ? O42 C41 C4 125.4(2) . . ? O43 C41 C4 111.02(19) . . ? C41 O43 C44 115.42(18) . . ? O43 C44 H44A 109.5 . . ? O43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O46 C45 O47 123.3(2) . . ? O46 C45 C4 125.59(19) . . ? O47 C45 C4 111.04(18) . . ? C45 O47 C48 116.69(18) . . ? O47 C48 H48A 109.5 . . ? O47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C62 C61 C66 120.0 . . ? C62 C61 C6 121.75(13) . . ? C66 C61 C6 118.23(13) . . ? C63 C62 C61 120.0 . . ? C63 C62 H62A 120.0 . . ? C61 C62 H62A 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63A 120.0 . . ? C64 C63 H63A 120.0 . . ? C63 C64 C65 120.0 . . ? C63 C64 H64A 120.0 . . ? C65 C64 H64A 120.0 . . ? C66 C65 C64 120.0 . . ? C66 C65 H65A 120.0 . . ? C64 C65 H65A 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66A 120.0 . . ? C61 C66 H66A 120.0 . . ? 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 C6 O1 N2 C21 -168.64(15) . . . . ? C6 O1 N2 C3 75.46(18) . . . . ? O1 N2 C3 C31 173.57(14) . . . . ? C21 N2 C3 C31 64.1(2) . . . . ? O1 N2 C3 C4 -60.89(19) . . . . ? C21 N2 C3 C4 -170.39(17) . . . . ? N2 C3 C4 C41 166.00(16) . . . . ? C31 C3 C4 C41 -72.2(2) . . . . ? N2 C3 C4 C45 -75.0(2) . . . . ? C31 C3 C4 C45 46.7(2) . . . . ? N2 C3 C4 C5 48.2(2) . . . . ? C31 C3 C4 C5 170.02(14) . . . . ? C41 C4 C5 C51 -39.6(2) . . . . ? C45 C4 C5 C51 -157.85(18) . . . . ? C3 C4 C5 C51 78.3(2) . . . . ? C41 C4 C5 C6 -163.17(17) . . . . ? C45 C4 C5 C6 78.6(2) . . . . ? C3 C4 C5 C6 -45.2(2) . . . . ? N2 O1 C6 C61 163.84(14) . . . . ? N2 O1 C6 C5 -73.12(19) . . . . ? C51 C5 C6 O1 -67.3(2) . . . . ? C4 C5 C6 O1 57.2(2) . . . . ? C51 C5 C6 C61 52.7(2) . . . . ? C4 C5 C6 C61 177.25(16) . . . . ? O1 N2 C21 C22 76.0(2) . . . . ? C3 N2 C21 C22 -171.11(17) . . . . ? N2 C21 C22 C23 74.6(2) . . . . ? N2 C21 C22 C27 -107.32(18) . . . . ? C27 C22 C23 C24 0.0 . . . . ? C21 C22 C23 C24 178.07(17) . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C22 0.0 . . . . ? C23 C22 C27 C26 0.0 . . . . ? C21 C22 C27 C26 -178.05(17) . . . . ? N2 C3 C31 C32 43.94(19) . . . . ? C4 C3 C31 C32 -78.74(18) . . . . ? N2 C3 C31 C36 -130.82(14) . . . . ? C4 C3 C31 C36 106.50(16) . . . . ? C36 C31 C32 C33 0.0 . . . . ? C3 C31 C32 C33 -174.73(16) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? C3 C31 C36 C35 174.78(16) . . . . ? C45 C4 C41 O42 -125.9(2) . . . . ? C5 C4 C41 O42 114.8(2) . . . . ? C3 C4 C41 O42 -5.4(3) . . . . ? C45 C4 C41 O43 57.9(2) . . . . ? C5 C4 C41 O43 -61.3(2) . . . . ? C3 C4 C41 O43 178.45(16) . . . . ? O42 C41 O43 C44 -2.5(3) . . . . ? C4 C41 O43 C44 173.76(18) . . . . ? C41 C4 C45 O46 -152.7(2) . . . . ? C5 C4 C45 O46 -35.2(3) . . . . ? C3 C4 C45 O46 88.8(3) . . . . ? C41 C4 C45 O47 28.9(3) . . . . ? C5 C4 C45 O47 146.51(18) . . . . ? C3 C4 C45 O47 -89.5(2) . . . . ? O46 C45 O47 C48 -0.2(4) . . . . ? C4 C45 O47 C48 178.2(2) . . . . ? O1 C6 C61 C62 7.0(2) . . . . ? C5 C6 C61 C62 -112.79(17) . . . . ? O1 C6 C61 C66 -171.27(12) . . . . ? C5 C6 C61 C66 68.99(19) . . . . ? C66 C61 C62 C63 0.0 . . . . ? C6 C61 C62 C63 -178.19(15) . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C66 0.0 . . . . ? C64 C65 C66 C61 0.0 . . . . ? C62 C61 C66 C65 0.0 . . . . ? C6 C61 C66 C65 178.25(15) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.225 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.041