data_notbu1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H44 N2 O2' _chemical_formula_sum 'C30 H44 N2 O2' _chemical_formula_weight 464.67 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.1904(11) _cell_length_b 12.730(3) _cell_length_c 17.528(4) _cell_angle_alpha 85.858(8) _cell_angle_beta 80.307(8) _cell_angle_gamma 83.199(9) _cell_volume 1350.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used 1486 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 21.26 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; 2242 frames x 60 sec. @ 4.959 cm; 0.3 deg steps in omega & phi ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12963 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.1369 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 23.96 _reflns_number_total 4193 _reflns_number_gt 2142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Data at resolution greater than 0.875 Angstroms were supressed in the refinement due to lack of observed reflections. 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^)+(0.0594P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.027(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4193 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1303 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _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 0.7482(4) 0.42061(17) 0.38301(12) 0.0358(6) Uani 1 1 d . . . O2 O -0.2024(4) 0.68574(19) -0.06713(12) 0.0403(7) Uani 1 1 d . . . N1 N 0.5397(4) 0.4279(2) 0.38140(14) 0.0248(7) Uani 1 1 d . . . N2 N 0.0053(4) 0.6719(2) -0.06436(14) 0.0243(7) Uani 1 1 d . . . C1 C 0.4118(5) 0.3426(2) 0.42596(17) 0.0255(8) Uani 1 1 d . . . C2 C 0.2091(5) 0.3934(3) 0.47658(17) 0.0325(9) Uani 1 1 d . . . H2A H 0.2513 0.4481 0.5060 0.0450(15) Uiso 1 1 calc R . . H2B H 0.1422 0.3393 0.5126 0.0450(15) Uiso 1 1 calc R . . H2C H 0.1026 0.4256 0.4439 0.0450(15) Uiso 1 1 calc R . . C3 C 0.5626(6) 0.2797(3) 0.47693(19) 0.0400(10) Uani 1 1 d . . . H3A H 0.6929 0.2461 0.4442 0.0450(15) Uiso 1 1 calc R . . H3B H 0.4835 0.2251 0.5083 0.0450(15) Uiso 1 1 calc R . . H3C H 0.6086 0.3274 0.5111 0.0450(15) Uiso 1 1 calc R . . C4 C 0.3563(6) 0.2691(3) 0.36904(19) 0.0390(10) Uani 1 1 d . . . H4A H 0.2637 0.3095 0.3345 0.0450(15) Uiso 1 1 calc R . . H4B H 0.2768 0.2126 0.3977 0.0450(15) Uiso 1 1 calc R . . H4C H 0.4928 0.2379 0.3383 0.0450(15) Uiso 1 1 calc R . . C5 C 0.4485(5) 0.5199(2) 0.34229(16) 0.0217(8) Uani 1 1 d . . . C6 C 0.5742(5) 0.6054(2) 0.32672(16) 0.0245(8) Uani 1 1 d . . . H6 H 0.7140 0.6011 0.3429 0.0450(15) Uiso 1 1 calc R . . C7 C 0.4952(5) 0.6961(2) 0.28777(16) 0.0233(8) Uani 1 1 d . . . H7 H 0.5828 0.7535 0.2776 0.0450(15) Uiso 1 1 calc R . . C8 C 0.2924(5) 0.7063(2) 0.26297(16) 0.0209(8) Uani 1 1 d . . . C9 C 0.1751(5) 0.6179(3) 0.27545(17) 0.0264(8) Uani 1 1 d . . . H9 H 0.0412 0.6203 0.2553 0.0450(15) Uiso 1 1 calc R . . C10 C 0.2470(5) 0.5267(2) 0.31611(16) 0.0235(8) Uani 1 1 d . . . H10 H 0.1594 0.4693 0.3261 0.0450(15) Uiso 1 1 calc R . . C11 C 0.2151(5) 0.8036(2) 0.21684(16) 0.0201(7) Uani 1 1 d . . . C12 C 0.1711(5) 0.7728(2) 0.14103(16) 0.0199(8) Uani 1 1 d . . . C13 C -0.0357(5) 0.7996(2) 0.11939(17) 0.0219(8) Uani 1 1 d . . . H13 H -0.1458 0.8409 0.1524 0.0450(15) Uiso 1 1 calc R . . C14 C -0.0848(5) 0.7679(2) 0.05173(17) 0.0232(8) Uani 1 1 d . . . H14 H -0.2271 0.7881 0.0385 0.0450(15) Uiso 1 1 calc R . . C15 C 0.0725(5) 0.7061(2) 0.00207(16) 0.0206(8) Uani 1 1 d . . . C16 C 0.2790(5) 0.6767(2) 0.02350(17) 0.0241(8) Uani 1 1 d . . . H16 H 0.3881 0.6342 -0.0091 0.0450(15) Uiso 1 1 calc R . . C17 C 0.3253(5) 0.7089(2) 0.09168(17) 0.0243(8) Uani 1 1 d . . . H17 H 0.4661 0.6871 0.1057 0.0450(15) Uiso 1 1 calc R . . C18 C 0.1516(5) 0.6167(2) -0.13046(17) 0.0226(8) Uani 1 1 d . . . C19 C 0.2140(6) 0.5019(3) -0.1055(2) 0.0427(10) Uani 1 1 d . . . H19A H 0.2952 0.4991 -0.0618 0.0450(15) Uiso 1 1 calc R . . H19B H 0.3071 0.4659 -0.1489 0.0450(15) Uiso 1 1 calc R . . H19C H 0.0801 0.4665 -0.0896 0.0450(15) Uiso 1 1 calc R . . C20 C 0.0176(5) 0.6200(3) -0.19609(18) 0.0403(10) Uani 1 1 d . . . H20A H -0.1073 0.5784 -0.1800 0.0450(15) Uiso 1 1 calc R . . H20B H 0.1112 0.5903 -0.2420 0.0450(15) Uiso 1 1 calc R . . H20C H -0.0373 0.6936 -0.2085 0.0450(15) Uiso 1 1 calc R . . C21 C 0.3549(5) 0.6749(3) -0.15977(18) 0.0317(9) Uani 1 1 d . . . H21A H 0.3082 0.7498 -0.1713 0.0450(15) Uiso 1 1 calc R . . H21B H 0.4368 0.6433 -0.2069 0.0450(15) Uiso 1 1 calc R . . H21C H 0.4497 0.6690 -0.1198 0.0450(15) Uiso 1 1 calc R . . C22 C 0.1897(5) 0.9044(3) 0.24079(17) 0.0219(8) Uani 1 1 d . . . C23 C 0.2111(5) 1.0001(2) 0.17973(17) 0.0248(8) Uani 1 1 d . . . C24 C 0.3507(5) 0.9696(3) 0.10093(17) 0.0325(9) Uani 1 1 d . . . H24A H 0.2673 0.9279 0.0737 0.0450(15) Uiso 1 1 calc R . . H24B H 0.4881 0.9275 0.1099 0.0450(15) Uiso 1 1 calc R . . H24C H 0.3848 1.0340 0.0694 0.0450(15) Uiso 1 1 calc R . . C25 C -0.0066(5) 1.0575(3) 0.16070(19) 0.0347(9) Uani 1 1 d . . . H25A H -0.0863 1.0080 0.1388 0.0450(15) Uiso 1 1 calc R . . H25B H 0.0238 1.1168 0.1230 0.0450(15) Uiso 1 1 calc R . . H25C H -0.0967 1.0845 0.2081 0.0450(15) Uiso 1 1 calc R . . C26 C 0.3434(5) 1.0839(2) 0.20527(19) 0.0341(9) Uani 1 1 d . . . H26A H 0.3535 1.1428 0.1661 0.0450(15) Uiso 1 1 calc R . . H26B H 0.4919 1.0513 0.2108 0.0450(15) Uiso 1 1 calc R . . H26C H 0.2682 1.1104 0.2551 0.0450(15) Uiso 1 1 calc R . . C27 C 0.1351(5) 0.9264(2) 0.32902(17) 0.0254(8) Uani 1 1 d . . . C28 C 0.0320(5) 0.8336(3) 0.37899(17) 0.0347(9) Uani 1 1 d . . . H28A H 0.1462 0.7741 0.3831 0.0450(15) Uiso 1 1 calc R . . H28B H -0.0848 0.8110 0.3546 0.0450(15) Uiso 1 1 calc R . . H28C H -0.0304 0.8572 0.4309 0.0450(15) Uiso 1 1 calc R . . C29 C -0.0464(5) 1.0206(3) 0.34482(18) 0.0347(9) Uani 1 1 d . . . H29A H -0.0806 1.0306 0.4007 0.0450(15) Uiso 1 1 calc R . . H29B H -0.1795 1.0057 0.3260 0.0450(15) Uiso 1 1 calc R . . H29C H 0.0060 1.0852 0.3178 0.0450(15) Uiso 1 1 calc R . . C30 C 0.3351(5) 0.9468(3) 0.36564(18) 0.0346(9) Uani 1 1 d . . . H30A H 0.2885 0.9564 0.4212 0.0450(15) Uiso 1 1 calc R . . H30B H 0.3956 1.0107 0.3407 0.0450(15) Uiso 1 1 calc R . . H30C H 0.4483 0.8861 0.3583 0.0450(15) 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 0.0272(16) 0.0363(15) 0.0446(15) 0.0034(12) -0.0135(12) 0.0014(12) O2 0.0176(15) 0.0665(19) 0.0389(14) -0.0183(13) -0.0091(11) 0.0019(12) N1 0.0249(18) 0.0265(17) 0.0240(15) -0.0011(13) -0.0090(13) 0.0003(14) N2 0.0176(17) 0.0303(17) 0.0254(15) -0.0042(13) -0.0042(13) -0.0014(13) C1 0.030(2) 0.023(2) 0.0228(18) 0.0018(15) -0.0031(16) -0.0030(16) C2 0.033(2) 0.039(2) 0.0245(18) 0.0043(17) -0.0036(16) -0.0019(18) C3 0.042(2) 0.036(2) 0.038(2) 0.0109(18) -0.0060(18) 0.0029(19) C4 0.055(3) 0.023(2) 0.039(2) 0.0026(17) -0.0072(19) -0.0101(19) C5 0.026(2) 0.022(2) 0.0163(17) -0.0024(15) -0.0039(15) 0.0022(16) C6 0.022(2) 0.029(2) 0.0228(17) -0.0018(16) -0.0067(15) -0.0031(17) C7 0.024(2) 0.023(2) 0.0228(17) -0.0021(15) -0.0021(15) -0.0049(16) C8 0.022(2) 0.020(2) 0.0210(17) -0.0036(15) -0.0043(15) 0.0005(16) C9 0.026(2) 0.029(2) 0.0272(18) -0.0067(16) -0.0068(16) -0.0053(17) C10 0.025(2) 0.024(2) 0.0237(17) -0.0010(16) -0.0070(15) -0.0063(16) C11 0.0129(18) 0.025(2) 0.0222(17) 0.0010(15) -0.0022(14) -0.0029(15) C12 0.024(2) 0.0166(18) 0.0189(17) 0.0002(14) -0.0037(15) -0.0006(15) C13 0.019(2) 0.0216(19) 0.0236(18) 0.0034(15) -0.0002(15) -0.0022(15) C14 0.0188(19) 0.0227(19) 0.0287(19) 0.0014(16) -0.0061(16) -0.0028(15) C15 0.020(2) 0.0210(19) 0.0203(17) 0.0013(15) -0.0027(15) -0.0033(15) C16 0.025(2) 0.024(2) 0.0238(18) -0.0032(15) -0.0055(15) 0.0027(16) C17 0.018(2) 0.028(2) 0.0276(19) 0.0026(16) -0.0068(16) -0.0017(16) C18 0.023(2) 0.022(2) 0.0235(18) -0.0046(15) -0.0031(15) -0.0004(15) C19 0.049(3) 0.027(2) 0.047(2) -0.0013(18) 0.0007(19) 0.0005(19) C20 0.027(2) 0.063(3) 0.032(2) -0.0212(19) -0.0032(17) 0.0002(19) C21 0.029(2) 0.037(2) 0.0284(19) 0.0011(16) 0.0003(16) -0.0058(17) C22 0.0124(18) 0.026(2) 0.0269(18) 0.0000(15) -0.0034(14) -0.0026(15) C23 0.025(2) 0.0197(19) 0.0294(18) 0.0002(15) -0.0041(15) -0.0011(15) C24 0.035(2) 0.029(2) 0.0325(19) 0.0039(16) -0.0027(17) -0.0087(17) C25 0.033(2) 0.032(2) 0.039(2) 0.0057(17) -0.0096(17) -0.0013(17) C26 0.033(2) 0.024(2) 0.045(2) 0.0021(17) -0.0061(17) -0.0072(17) C27 0.024(2) 0.026(2) 0.0264(18) -0.0049(16) -0.0010(15) -0.0035(16) C28 0.038(2) 0.036(2) 0.0273(19) -0.0060(17) 0.0038(17) -0.0017(18) C29 0.032(2) 0.035(2) 0.035(2) -0.0087(17) 0.0011(17) 0.0004(18) C30 0.039(2) 0.034(2) 0.0320(19) -0.0072(17) -0.0107(17) 0.0009(18) _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 N1 1.288(3) . ? O2 N2 1.285(3) . ? N1 C5 1.421(4) . ? N1 C1 1.513(4) . ? N2 C15 1.413(4) . ? N2 C18 1.506(4) . ? C1 C2 1.515(4) . ? C1 C3 1.520(4) . ? C1 C4 1.522(4) . ? C5 C10 1.391(4) . ? C5 C6 1.396(4) . ? C6 C7 1.380(4) . ? C7 C8 1.385(4) . ? C8 C9 1.395(4) . ? C8 C11 1.504(4) . ? C9 C10 1.384(4) . ? C11 C22 1.361(4) . ? C11 C12 1.488(4) . ? C12 C13 1.393(4) . ? C12 C17 1.401(4) . ? C13 C14 1.372(4) . ? C14 C15 1.399(4) . ? C15 C16 1.394(4) . ? C16 C17 1.376(4) . ? C18 C19 1.519(4) . ? C18 C20 1.523(4) . ? C18 C21 1.532(4) . ? C22 C23 1.566(4) . ? C22 C27 1.565(4) . ? C23 C25 1.531(4) . ? C23 C24 1.550(4) . ? C23 C26 1.552(4) . ? C27 C30 1.543(4) . ? C27 C29 1.549(4) . ? C27 C28 1.553(4) . ? 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 O1 N1 C5 116.5(2) . . ? O1 N1 C1 117.4(2) . . ? C5 N1 C1 125.9(3) . . ? O2 N2 C15 116.6(2) . . ? O2 N2 C18 116.9(2) . . ? C15 N2 C18 126.5(3) . . ? N1 C1 C2 109.6(3) . . ? N1 C1 C3 107.0(3) . . ? C2 C1 C3 109.4(3) . . ? N1 C1 C4 109.1(2) . . ? C2 C1 C4 112.8(3) . . ? C3 C1 C4 108.8(3) . . ? C10 C5 C6 119.1(3) . . ? C10 C5 N1 123.3(3) . . ? C6 C5 N1 117.5(3) . . ? C7 C6 C5 120.0(3) . . ? C6 C7 C8 122.2(3) . . ? C7 C8 C9 116.8(3) . . ? C7 C8 C11 121.2(3) . . ? C9 C8 C11 121.6(3) . . ? C10 C9 C8 122.3(3) . . ? C9 C10 C5 119.5(3) . . ? C22 C11 C12 125.3(3) . . ? C22 C11 C8 125.2(3) . . ? C12 C11 C8 109.6(3) . . ? C13 C12 C17 116.9(3) . . ? C13 C12 C11 120.4(3) . . ? C17 C12 C11 122.5(3) . . ? C14 C13 C12 121.8(3) . . ? C13 C14 C15 120.7(3) . . ? C16 C15 C14 118.4(3) . . ? C16 C15 N2 124.3(3) . . ? C14 C15 N2 117.2(3) . . ? C17 C16 C15 120.2(3) . . ? C16 C17 C12 122.0(3) . . ? N2 C18 C19 109.7(3) . . ? N2 C18 C20 106.9(2) . . ? C19 C18 C20 109.0(3) . . ? N2 C18 C21 111.0(2) . . ? C19 C18 C21 111.9(3) . . ? C20 C18 C21 108.0(2) . . ? C11 C22 C23 120.0(3) . . ? C11 C22 C27 120.9(3) . . ? C23 C22 C27 119.1(3) . . ? C25 C23 C24 105.9(3) . . ? C25 C23 C26 107.7(3) . . ? C24 C23 C26 102.0(3) . . ? C25 C23 C22 115.6(3) . . ? C24 C23 C22 113.3(2) . . ? C26 C23 C22 111.3(3) . . ? C30 C27 C29 108.7(3) . . ? C30 C27 C28 105.8(3) . . ? C29 C27 C28 102.8(2) . . ? C30 C27 C22 114.6(2) . . ? C29 C27 C22 111.6(2) . . ? C28 C27 C22 112.6(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.96 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.195 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.054