data_q03d _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H50 N2 O4' _chemical_formula_weight 622.82 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1628(3) _cell_length_b 11.2261(4) _cell_length_c 18.4027(6) _cell_angle_alpha 90.6260(10) _cell_angle_beta 100.0740(10) _cell_angle_gamma 93.5530(10) _cell_volume 1656.76(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9930 _cell_measurement_theta_min 4.59 _cell_measurement_theta_max 69.74 _exptl_crystal_description Irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.627 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.916 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Bruker MicroStar microfocus rotating anode' _diffrn_radiation_monochromator 'Helios multilayer optics' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15743 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 69.74 _reflns_number_total 5735 _reflns_number_gt 5656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0338P)^2^+0.6971P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5735 _refine_ls_number_parameters 616 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 0.59724(11) 0.50979(8) 0.38699(5) 0.0287(2) Uani 1 1 d . . . O2 O 0.26241(12) -0.08695(8) 0.46119(5) 0.0279(2) Uani 1 1 d . . . N1 N 0.38615(12) 0.38390(9) 0.40649(5) 0.0174(2) Uani 1 1 d . . . C1 C 0.54594(15) 0.40657(11) 0.39731(6) 0.0205(3) Uani 1 1 d . . . C2 C 0.66180(15) 0.30692(12) 0.39855(8) 0.0256(3) Uani 1 1 d . . . H2A H 0.766(2) 0.3461(14) 0.3916(8) 0.030(4) Uiso 1 1 d . . . H2B H 0.6831(19) 0.2720(14) 0.4478(9) 0.030(4) Uiso 1 1 d . . . C3 C 0.60257(17) 0.21013(12) 0.33938(8) 0.0280(3) Uani 1 1 d . . . H3A H 0.700(2) 0.1659(15) 0.3333(9) 0.035(4) Uiso 1 1 d . . . H3B H 0.5585(19) 0.2475(14) 0.2905(9) 0.030(4) Uiso 1 1 d . . . C4 C 0.46948(16) 0.12186(11) 0.35893(7) 0.0231(3) Uani 1 1 d . . . H4A H 0.5121(18) 0.0886(13) 0.4081(8) 0.023(3) Uiso 1 1 d . . . H4B H 0.4508(18) 0.0562(14) 0.3218(8) 0.027(4) Uiso 1 1 d . . . C5 C 0.29836(14) 0.17017(10) 0.36044(6) 0.0172(2) Uani 1 1 d . . . H5 H 0.2554(17) 0.2036(13) 0.3112(8) 0.021(3) Uiso 1 1 d . . . C6 C 0.17597(15) 0.06399(10) 0.37305(6) 0.0178(2) Uani 1 1 d . . . H6 H 0.0653(18) 0.0954(12) 0.3727(7) 0.020(3) Uiso 1 1 d . . . C7 C 0.23259(14) 0.01673(11) 0.45023(6) 0.0193(2) Uani 1 1 d . . . C8 C 0.25190(16) 0.10870(11) 0.51236(6) 0.0213(3) Uani 1 1 d . . . H8A H 0.3060(19) 0.0721(14) 0.5577(8) 0.027(4) Uiso 1 1 d . . . H8B H 0.1359(19) 0.1274(13) 0.5188(8) 0.024(4) Uiso 1 1 d . . . C9 C 0.35094(15) 0.22401(11) 0.49733(6) 0.0183(2) Uani 1 1 d . . . H9A H 0.3430(17) 0.2873(13) 0.5334(8) 0.020(3) Uiso 1 1 d . . . H9B H 0.4721(19) 0.2082(13) 0.5038(8) 0.022(3) Uiso 1 1 d . . . C10 C 0.29251(14) 0.26948(10) 0.41892(6) 0.0159(2) Uani 1 1 d . . . C11 C 0.11333(14) 0.31174(11) 0.41101(7) 0.0189(2) Uani 1 1 d . . . H11A H 0.0614(17) 0.3071(12) 0.3588(8) 0.018(3) Uiso 1 1 d . . . H11B H 0.0450(19) 0.2622(13) 0.4383(8) 0.024(4) Uiso 1 1 d . . . C12 C 0.13541(15) 0.44049(11) 0.43944(7) 0.0222(3) Uani 1 1 d . . . H12A H 0.1590(18) 0.4431(13) 0.4939(8) 0.022(3) Uiso 1 1 d . . . H12B H 0.036(2) 0.4857(14) 0.4222(8) 0.028(4) Uiso 1 1 d . . . C13 C 0.28704(15) 0.48889(11) 0.40928(7) 0.0208(3) Uani 1 1 d . . . H13B H 0.2558(17) 0.5186(13) 0.3583(8) 0.022(3) Uiso 1 1 d . . . H13A H 0.3542(18) 0.5506(13) 0.4418(8) 0.020(3) Uiso 1 1 d . . . C14 C 0.15239(16) -0.03498(11) 0.31274(7) 0.0223(3) Uani 1 1 d . . . H14A H 0.1492(18) 0.0044(13) 0.2641(8) 0.024(4) Uiso 1 1 d . . . H14B H 0.2481(19) -0.0875(14) 0.3211(8) 0.026(4) Uiso 1 1 d . . . C15 C -0.00697(16) -0.11147(11) 0.31110(6) 0.0206(3) Uani 1 1 d . . . C16 C -0.00548(16) -0.22667(11) 0.33915(6) 0.0226(3) Uani 1 1 d . . . H16 H 0.101(2) -0.2593(14) 0.3583(8) 0.029(4) Uiso 1 1 d . . . C17 C -0.15370(16) -0.29389(11) 0.34058(6) 0.0232(3) Uani 1 1 d . . . H17 H -0.1537(19) -0.3741(14) 0.3605(8) 0.029(4) Uiso 1 1 d . . . C18 C -0.30556(16) -0.24732(11) 0.31446(6) 0.0226(3) Uani 1 1 d . . . H18 H -0.409(2) -0.2944(14) 0.3161(8) 0.028(4) Uiso 1 1 d . . . C19 C -0.30878(16) -0.13364(11) 0.28507(6) 0.0233(3) Uani 1 1 d . . . H19 H -0.416(2) -0.1031(14) 0.2649(8) 0.027(4) Uiso 1 1 d . . . C20 C -0.16063(16) -0.06677(11) 0.28316(6) 0.0222(3) Uani 1 1 d . . . H20 H -0.1654(18) 0.0135(14) 0.2613(8) 0.025(4) Uiso 1 1 d . . . O21 O 0.72040(11) 1.00398(8) 0.09711(5) 0.0264(2) Uani 1 1 d . . . O22 O 0.23803(11) 0.43069(8) 0.03387(5) 0.0249(2) Uani 1 1 d . . . N21 N 0.48208(12) 0.89161(8) 0.09327(5) 0.0181(2) Uani 1 1 d . . . C21 C 0.64455(14) 0.90498(11) 0.08612(6) 0.0190(2) Uani 1 1 d . . . C22 C 0.73263(15) 0.79896(11) 0.06509(7) 0.0205(3) Uani 1 1 d . . . H22A H 0.6795(18) 0.7674(13) 0.0163(8) 0.020(3) Uiso 1 1 d . . . H22B H 0.844(2) 0.8307(14) 0.0608(8) 0.028(4) Uiso 1 1 d . . . C23 C 0.74400(14) 0.69855(11) 0.12092(6) 0.0190(2) Uani 1 1 d . . . H23A H 0.7812(16) 0.7346(12) 0.1713(7) 0.015(3) Uiso 1 1 d . . . H23B H 0.8308(18) 0.6462(13) 0.1114(8) 0.021(3) Uiso 1 1 d . . . C24 C 0.58322(14) 0.61972(10) 0.11570(6) 0.0177(2) Uani 1 1 d . . . H24A H 0.5540(17) 0.5843(12) 0.0654(8) 0.020(3) Uiso 1 1 d . . . H24B H 0.6058(18) 0.5523(13) 0.1498(8) 0.023(3) Uiso 1 1 d . . . C25 C 0.42984(14) 0.67812(10) 0.13452(6) 0.0153(2) Uani 1 1 d . . . H25 H 0.4583(15) 0.7095(11) 0.1860(7) 0.010(3) Uiso 1 1 d . . . C26 C 0.28369(14) 0.58093(10) 0.13035(6) 0.0164(2) Uani 1 1 d . . . H26 H 0.1858(17) 0.6222(12) 0.1405(7) 0.018(3) Uiso 1 1 d . . . C27 C 0.23746(14) 0.53531(11) 0.05078(6) 0.0184(2) Uani 1 1 d . . . C28 C 0.19165(16) 0.62998(12) -0.00588(7) 0.0235(3) Uani 1 1 d . . . H28A H 0.079(2) 0.6533(14) -0.0013(8) 0.029(4) Uiso 1 1 d . . . H28B H 0.1820(18) 0.5951(13) -0.0544(9) 0.025(4) Uiso 1 1 d . . . C29 C 0.31554(15) 0.74039(11) 0.00398(6) 0.0196(2) Uani 1 1 d . . . H29A H 0.4172(17) 0.7205(12) -0.0147(7) 0.017(3) Uiso 1 1 d . . . H29B H 0.2688(18) 0.8069(13) -0.0259(8) 0.023(3) Uiso 1 1 d . . . C30 C 0.36469(14) 0.78259(10) 0.08525(6) 0.0165(2) Uani 1 1 d . . . C31 C 0.21371(16) 0.83337(11) 0.11291(7) 0.0232(3) Uani 1 1 d . . . H31A H 0.2309(19) 0.8281(14) 0.1673(9) 0.029(4) Uiso 1 1 d . . . H31B H 0.1098(19) 0.7888(13) 0.0918(8) 0.025(4) Uiso 1 1 d . . . C32 C 0.21665(17) 0.96370(12) 0.09068(8) 0.0271(3) Uani 1 1 d . . . H32A H 0.1769(19) 0.9687(13) 0.0386(9) 0.025(4) Uiso 1 1 d . . . H32B H 0.151(2) 1.0116(15) 0.1178(9) 0.033(4) Uiso 1 1 d . . . C33 C 0.40112(16) 1.00109(11) 0.10835(7) 0.0236(3) Uani 1 1 d . . . H33A H 0.4356(19) 1.0655(14) 0.0770(9) 0.030(4) Uiso 1 1 d . . . H33B H 0.4377(18) 1.0264(13) 0.1610(9) 0.026(4) Uiso 1 1 d . . . C34 C 0.31452(14) 0.47928(11) 0.18546(6) 0.0184(2) Uani 1 1 d . . . H34A H 0.3676(17) 0.5150(12) 0.2340(8) 0.018(3) Uiso 1 1 d . . . H34B H 0.3931(18) 0.4239(13) 0.1702(8) 0.024(4) Uiso 1 1 d . . . C35 C 0.15374(14) 0.40836(10) 0.19175(6) 0.0179(2) Uani 1 1 d . . . C36 C 0.12457(15) 0.29006(11) 0.16629(6) 0.0194(2) Uani 1 1 d . . . H36 H 0.2105(18) 0.2512(13) 0.1453(8) 0.021(3) Uiso 1 1 d . . . C37 C -0.02579(15) 0.22647(11) 0.16937(6) 0.0214(3) Uani 1 1 d . . . H37 H -0.0464(18) 0.1455(14) 0.1499(8) 0.025(4) Uiso 1 1 d . . . C38 C -0.14925(15) 0.28032(12) 0.19839(6) 0.0229(3) Uani 1 1 d . . . H38 H -0.256(2) 0.2360(14) 0.1986(8) 0.031(4) Uiso 1 1 d . . . C39 C -0.12205(15) 0.39742(12) 0.22507(6) 0.0225(3) Uani 1 1 d . . . H39 H -0.2066(19) 0.4364(13) 0.2461(8) 0.025(4) Uiso 1 1 d . . . C40 C 0.02844(15) 0.46092(11) 0.22140(6) 0.0202(2) Uani 1 1 d . . . H40 H 0.0444(17) 0.5438(13) 0.2405(8) 0.022(3) Uiso 1 1 d . . . 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(5) 0.0219(5) 0.0371(5) 0.0038(4) 0.0087(4) -0.0071(4) O2 0.0362(5) 0.0172(5) 0.0281(5) 0.0040(3) -0.0006(4) 0.0024(4) N1 0.0175(5) 0.0140(5) 0.0203(5) 0.0017(4) 0.0023(4) -0.0004(4) C1 0.0198(6) 0.0213(7) 0.0193(6) 0.0013(4) 0.0024(4) -0.0040(5) C2 0.0156(6) 0.0267(7) 0.0354(7) 0.0048(5) 0.0072(5) -0.0007(5) C3 0.0240(6) 0.0274(7) 0.0366(7) 0.0008(6) 0.0154(5) 0.0032(6) C4 0.0236(6) 0.0191(6) 0.0284(7) -0.0014(5) 0.0098(5) 0.0017(5) C5 0.0198(6) 0.0158(6) 0.0158(5) 0.0019(4) 0.0035(4) -0.0003(5) C6 0.0198(6) 0.0151(6) 0.0186(6) 0.0007(4) 0.0041(4) 0.0001(5) C7 0.0186(5) 0.0172(6) 0.0225(6) 0.0038(4) 0.0047(4) -0.0010(5) C8 0.0267(6) 0.0203(6) 0.0169(6) 0.0040(5) 0.0042(5) 0.0014(5) C9 0.0197(6) 0.0179(6) 0.0168(5) 0.0009(4) 0.0019(4) 0.0013(5) C10 0.0152(5) 0.0142(6) 0.0183(5) 0.0020(4) 0.0031(4) -0.0008(4) C11 0.0157(5) 0.0179(6) 0.0227(6) 0.0022(4) 0.0024(5) 0.0012(5) C12 0.0207(6) 0.0189(6) 0.0275(6) -0.0002(5) 0.0046(5) 0.0050(5) C13 0.0236(6) 0.0150(6) 0.0230(6) 0.0003(5) 0.0017(5) 0.0023(5) C14 0.0295(7) 0.0176(6) 0.0200(6) -0.0005(5) 0.0062(5) -0.0016(5) C15 0.0301(6) 0.0166(6) 0.0147(5) -0.0028(4) 0.0043(5) -0.0013(5) C16 0.0279(6) 0.0190(6) 0.0203(6) -0.0002(5) 0.0023(5) 0.0015(5) C17 0.0326(7) 0.0170(6) 0.0189(6) 0.0016(4) 0.0031(5) -0.0028(5) C18 0.0280(6) 0.0224(6) 0.0164(5) -0.0028(4) 0.0033(5) -0.0044(5) C19 0.0284(7) 0.0227(6) 0.0173(6) -0.0038(5) -0.0002(5) 0.0026(5) C20 0.0337(7) 0.0150(6) 0.0167(5) -0.0012(4) 0.0021(5) 0.0000(5) O21 0.0259(5) 0.0176(5) 0.0324(5) 0.0036(3) -0.0008(4) -0.0069(4) O22 0.0329(5) 0.0192(5) 0.0228(4) -0.0024(3) 0.0077(4) -0.0055(4) N21 0.0201(5) 0.0120(5) 0.0216(5) 0.0008(4) 0.0022(4) 0.0002(4) C21 0.0203(6) 0.0172(6) 0.0177(5) 0.0044(4) -0.0009(4) -0.0029(5) C22 0.0156(6) 0.0207(6) 0.0252(6) 0.0041(5) 0.0038(5) -0.0013(5) C23 0.0157(5) 0.0186(6) 0.0223(6) 0.0017(5) 0.0020(4) 0.0019(5) C24 0.0175(6) 0.0153(6) 0.0202(6) 0.0024(4) 0.0028(4) 0.0011(5) C25 0.0156(5) 0.0141(6) 0.0155(5) 0.0005(4) 0.0016(4) -0.0013(4) C26 0.0155(5) 0.0151(6) 0.0183(5) 0.0013(4) 0.0025(4) -0.0005(5) C27 0.0145(5) 0.0198(6) 0.0202(6) 0.0002(4) 0.0031(4) -0.0052(5) C28 0.0244(6) 0.0242(7) 0.0186(6) 0.0024(5) -0.0028(5) -0.0061(5) C29 0.0196(6) 0.0187(6) 0.0190(6) 0.0040(4) 0.0001(4) -0.0014(5) C30 0.0142(5) 0.0137(6) 0.0209(6) 0.0015(4) 0.0021(4) -0.0009(4) C31 0.0199(6) 0.0205(6) 0.0307(7) 0.0037(5) 0.0074(5) 0.0045(5) C32 0.0279(7) 0.0197(6) 0.0363(8) 0.0044(5) 0.0098(6) 0.0089(5) C33 0.0302(7) 0.0130(6) 0.0279(6) 0.0013(5) 0.0057(5) 0.0036(5) C34 0.0180(5) 0.0176(6) 0.0188(6) 0.0025(4) 0.0010(4) -0.0010(5) C35 0.0190(6) 0.0194(6) 0.0142(5) 0.0052(4) -0.0002(4) -0.0001(5) C36 0.0213(6) 0.0190(6) 0.0176(5) 0.0037(4) 0.0025(4) 0.0010(5) C37 0.0247(6) 0.0185(6) 0.0191(6) 0.0048(4) 0.0003(5) -0.0031(5) C38 0.0204(6) 0.0282(7) 0.0190(6) 0.0080(5) 0.0014(4) -0.0042(5) C39 0.0213(6) 0.0292(7) 0.0179(6) 0.0066(5) 0.0049(5) 0.0042(5) C40 0.0238(6) 0.0203(6) 0.0161(5) 0.0032(4) 0.0018(4) 0.0018(5) _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 C1 1.2356(15) . ? O2 C7 1.2156(15) . ? N1 C1 1.3533(15) . ? N1 C13 1.4757(15) . ? N1 C10 1.4941(15) . ? C1 C2 1.5068(18) . ? C2 C3 1.5248(19) . ? C2 H2A 0.960(17) . ? C2 H2B 0.983(16) . ? C3 C4 1.5175(18) . ? C3 H3A 0.983(17) . ? C3 H3B 1.014(16) . ? C4 C5 1.5340(16) . ? C4 H4A 0.997(15) . ? C4 H4B 0.986(16) . ? C5 C10 1.5498(15) . ? C5 C6 1.5532(16) . ? C5 H5 0.998(14) . ? C6 C7 1.5263(16) . ? C6 C14 1.5412(16) . ? C6 H6 0.989(15) . ? C7 C8 1.5131(17) . ? C8 C9 1.5369(17) . ? C8 H8A 0.980(16) . ? C8 H8B 1.009(15) . ? C9 C10 1.5413(15) . ? C9 H9A 0.980(15) . ? C9 H9B 1.002(15) . ? C10 C11 1.5487(15) . ? C11 C12 1.5210(16) . ? C11 H11A 0.979(14) . ? C11 H11B 0.969(15) . ? C12 C13 1.5162(17) . ? C12 H12A 0.987(15) . ? C12 H12B 0.990(16) . ? C13 H13B 0.995(15) . ? C13 H13A 0.983(15) . ? C14 C15 1.5092(17) . ? C14 H14A 1.001(15) . ? C14 H14B 0.999(16) . ? C15 C20 1.3955(18) . ? C15 C16 1.3977(17) . ? C16 C17 1.3901(18) . ? C16 H16 0.976(16) . ? C17 C18 1.3851(19) . ? C17 H17 0.976(16) . ? C18 C19 1.3914(18) . ? C18 H18 0.975(16) . ? C19 C20 1.3893(19) . ? C19 H19 0.974(16) . ? C20 H20 0.991(15) . ? O21 C21 1.2350(15) . ? O22 C27 1.2122(15) . ? N21 C21 1.3548(16) . ? N21 C33 1.4771(15) . ? N21 C30 1.4963(15) . ? C21 C22 1.5088(17) . ? C22 C23 1.5296(16) . ? C22 H22A 0.978(14) . ? C22 H22B 0.972(16) . ? C23 C24 1.5247(16) . ? C23 H23A 0.998(14) . ? C23 H23B 0.985(15) . ? C24 C25 1.5381(15) . ? C24 H24A 0.987(14) . ? C24 H24B 0.995(15) . ? C25 C30 1.5532(15) . ? C25 C26 1.5570(15) . ? C25 H25 0.990(13) . ? C26 C27 1.5215(15) . ? C26 C34 1.5381(15) . ? C26 H26 0.992(14) . ? C27 C28 1.5145(16) . ? C28 C29 1.5386(17) . ? C28 H28A 0.990(16) . ? C28 H28B 0.960(15) . ? C29 C30 1.5405(16) . ? C29 H29A 0.989(14) . ? C29 H29B 0.988(15) . ? C30 C31 1.5501(16) . ? C31 C32 1.5234(17) . ? C31 H31A 0.988(16) . ? C31 H31B 0.974(15) . ? C32 C33 1.5155(19) . ? C32 H32A 0.959(16) . ? C32 H32B 0.974(17) . ? C33 H33A 0.988(16) . ? C33 H33B 0.995(15) . ? C34 C35 1.5150(16) . ? C34 H34A 0.991(14) . ? C34 H34B 0.992(15) . ? C35 C36 1.3957(17) . ? C35 C40 1.3983(17) . ? C36 C37 1.3913(17) . ? C36 H36 0.979(15) . ? C37 C38 1.3868(18) . ? C37 H37 0.967(15) . ? C38 C39 1.3892(19) . ? C38 H38 0.975(16) . ? C39 C40 1.3940(18) . ? C39 H39 0.972(15) . ? C40 H40 0.984(15) . ? 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 C1 N1 C13 116.15(10) . . ? C1 N1 C10 130.91(10) . . ? C13 N1 C10 112.83(9) . . ? O1 C1 N1 119.81(11) . . ? O1 C1 C2 119.48(11) . . ? N1 C1 C2 120.70(11) . . ? C1 C2 C3 113.95(11) . . ? C1 C2 H2A 104.2(10) . . ? C3 C2 H2A 111.0(9) . . ? C1 C2 H2B 110.5(9) . . ? C3 C2 H2B 110.7(9) . . ? H2A C2 H2B 106.0(13) . . ? C4 C3 C2 113.52(11) . . ? C4 C3 H3A 108.1(10) . . ? C2 C3 H3A 107.5(10) . . ? C4 C3 H3B 109.0(9) . . ? C2 C3 H3B 110.3(9) . . ? H3A C3 H3B 108.2(13) . . ? C3 C4 C5 116.32(10) . . ? C3 C4 H4A 108.3(8) . . ? C5 C4 H4A 108.8(8) . . ? C3 C4 H4B 108.2(9) . . ? C5 C4 H4B 106.4(9) . . ? H4A C4 H4B 108.5(12) . . ? C4 C5 C10 116.36(10) . . ? C4 C5 C6 108.26(9) . . ? C10 C5 C6 108.52(9) . . ? C4 C5 H5 109.0(8) . . ? C10 C5 H5 106.9(8) . . ? C6 C5 H5 107.5(8) . . ? C7 C6 C14 112.55(10) . . ? C7 C6 C5 108.47(9) . . ? C14 C6 C5 114.12(9) . . ? C7 C6 H6 106.8(8) . . ? C14 C6 H6 106.8(8) . . ? C5 C6 H6 107.8(8) . . ? O2 C7 C8 122.16(11) . . ? O2 C7 C6 122.63(11) . . ? C8 C7 C6 115.21(10) . . ? C7 C8 C9 113.20(10) . . ? C7 C8 H8A 108.0(9) . . ? C9 C8 H8A 110.6(9) . . ? C7 C8 H8B 106.9(8) . . ? C9 C8 H8B 109.8(8) . . ? H8A C8 H8B 108.1(12) . . ? C8 C9 C10 112.07(9) . . ? C8 C9 H9A 111.4(8) . . ? C10 C9 H9A 109.1(8) . . ? C8 C9 H9B 108.8(8) . . ? C10 C9 H9B 109.5(8) . . ? H9A C9 H9B 105.8(11) . . ? N1 C10 C9 111.13(9) . . ? N1 C10 C11 100.38(9) . . ? C9 C10 C11 110.53(9) . . ? N1 C10 C5 114.01(9) . . ? C9 C10 C5 110.52(9) . . ? C11 C10 C5 109.85(9) . . ? C12 C11 C10 105.00(9) . . ? C12 C11 H11A 110.9(8) . . ? C10 C11 H11A 108.9(8) . . ? C12 C11 H11B 112.1(9) . . ? C10 C11 H11B 111.7(9) . . ? H11A C11 H11B 108.2(12) . . ? C13 C12 C11 102.80(10) . . ? C13 C12 H12A 110.1(8) . . ? C11 C12 H12A 110.2(8) . . ? C13 C12 H12B 112.2(9) . . ? C11 C12 H12B 112.5(9) . . ? H12A C12 H12B 108.9(12) . . ? N1 C13 C12 103.85(9) . . ? N1 C13 H13B 108.6(8) . . ? C12 C13 H13B 111.6(8) . . ? N1 C13 H13A 108.9(8) . . ? C12 C13 H13A 112.7(8) . . ? H13B C13 H13A 110.9(12) . . ? C15 C14 C6 112.06(10) . . ? C15 C14 H14A 109.2(8) . . ? C6 C14 H14A 107.8(8) . . ? C15 C14 H14B 108.5(9) . . ? C6 C14 H14B 110.2(9) . . ? H14A C14 H14B 109.0(12) . . ? C20 C15 C16 118.35(11) . . ? C20 C15 C14 120.27(11) . . ? C16 C15 C14 121.35(11) . . ? C17 C16 C15 120.71(12) . . ? C17 C16 H16 120.1(9) . . ? C15 C16 H16 119.1(9) . . ? C18 C17 C16 120.38(11) . . ? C18 C17 H17 118.4(9) . . ? C16 C17 H17 121.2(9) . . ? C17 C18 C19 119.50(12) . . ? C17 C18 H18 120.1(9) . . ? C19 C18 H18 120.4(9) . . ? C20 C19 C18 120.12(12) . . ? C20 C19 H19 121.0(9) . . ? C18 C19 H19 118.9(9) . . ? C19 C20 C15 120.90(11) . . ? C19 C20 H20 118.9(9) . . ? C15 C20 H20 120.2(9) . . ? C21 N21 C33 116.78(10) . . ? C21 N21 C30 130.44(10) . . ? C33 N21 C30 112.72(9) . . ? O21 C21 N21 119.85(11) . . ? O21 C21 C22 120.15(11) . . ? N21 C21 C22 120.00(10) . . ? C21 C22 C23 114.40(10) . . ? C21 C22 H22A 110.3(8) . . ? C23 C22 H22A 109.7(8) . . ? C21 C22 H22B 105.1(9) . . ? C23 C22 H22B 109.8(9) . . ? H22A C22 H22B 107.2(12) . . ? C24 C23 C22 113.67(9) . . ? C24 C23 H23A 111.9(8) . . ? C22 C23 H23A 108.4(8) . . ? C24 C23 H23B 106.8(8) . . ? C22 C23 H23B 108.6(8) . . ? H23A C23 H23B 107.2(11) . . ? C23 C24 C25 117.33(10) . . ? C23 C24 H24A 108.7(8) . . ? C25 C24 H24A 108.6(8) . . ? C23 C24 H24B 108.0(8) . . ? C25 C24 H24B 107.2(8) . . ? H24A C24 H24B 106.5(11) . . ? C24 C25 C30 116.58(9) . . ? C24 C25 C26 108.90(9) . . ? C30 C25 C26 107.59(9) . . ? C24 C25 H25 108.0(7) . . ? C30 C25 H25 107.3(7) . . ? C26 C25 H25 108.2(7) . . ? C27 C26 C34 112.49(9) . . ? C27 C26 C25 107.93(9) . . ? C34 C26 C25 115.36(9) . . ? C27 C26 H26 105.7(8) . . ? C34 C26 H26 108.1(8) . . ? C25 C26 H26 106.7(8) . . ? O22 C27 C28 122.34(11) . . ? O22 C27 C26 122.41(10) . . ? C28 C27 C26 115.25(10) . . ? C27 C28 C29 113.27(10) . . ? C27 C28 H28A 107.1(9) . . ? C29 C28 H28A 110.2(9) . . ? C27 C28 H28B 109.0(9) . . ? C29 C28 H28B 110.7(9) . . ? H28A C28 H28B 106.3(12) . . ? C28 C29 C30 112.45(10) . . ? C28 C29 H29A 108.8(8) . . ? C30 C29 H29A 108.9(8) . . ? C28 C29 H29B 110.8(8) . . ? C30 C29 H29B 109.1(8) . . ? H29A C29 H29B 106.7(11) . . ? N21 C30 C29 111.50(9) . . ? N21 C30 C31 100.18(9) . . ? C29 C30 C31 110.43(9) . . ? N21 C30 C25 113.82(9) . . ? C29 C30 C25 110.52(9) . . ? C31 C30 C25 109.96(9) . . ? C32 C31 C30 105.00(10) . . ? C32 C31 H31A 110.0(9) . . ? C30 C31 H31A 108.7(9) . . ? C32 C31 H31B 112.6(9) . . ? C30 C31 H31B 111.4(9) . . ? H31A C31 H31B 109.0(12) . . ? C33 C32 C31 102.08(10) . . ? C33 C32 H32A 110.0(9) . . ? C31 C32 H32A 109.6(9) . . ? C33 C32 H32B 112.3(9) . . ? C31 C32 H32B 112.7(9) . . ? H32A C32 H32B 109.9(13) . . ? N21 C33 C32 103.63(10) . . ? N21 C33 H33A 109.0(9) . . ? C32 C33 H33A 113.7(9) . . ? N21 C33 H33B 109.6(9) . . ? C32 C33 H33B 112.3(9) . . ? H33A C33 H33B 108.4(12) . . ? C35 C34 C26 111.48(9) . . ? C35 C34 H34A 110.5(8) . . ? C26 C34 H34A 108.0(8) . . ? C35 C34 H34B 108.5(8) . . ? C26 C34 H34B 110.9(8) . . ? H34A C34 H34B 107.3(11) . . ? C36 C35 C40 118.17(11) . . ? C36 C35 C34 121.05(11) . . ? C40 C35 C34 120.75(11) . . ? C37 C36 C35 121.03(11) . . ? C37 C36 H36 119.2(8) . . ? C35 C36 H36 119.7(8) . . ? C38 C37 C36 120.02(11) . . ? C38 C37 H37 119.5(9) . . ? C36 C37 H37 120.4(9) . . ? C37 C38 C39 119.95(11) . . ? C37 C38 H38 119.4(9) . . ? C39 C38 H38 120.7(9) . . ? C38 C39 C40 119.76(11) . . ? C38 C39 H39 121.1(9) . . ? C40 C39 H39 119.1(9) . . ? C39 C40 C35 121.05(11) . . ? C39 C40 H40 118.2(8) . . ? C35 C40 H40 120.8(8) . . ? 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 C13 N1 C1 O1 -4.73(16) . . . . ? C10 N1 C1 O1 179.36(10) . . . . ? C13 N1 C1 C2 176.06(10) . . . . ? C10 N1 C1 C2 0.15(18) . . . . ? O1 C1 C2 C3 -119.59(13) . . . . ? N1 C1 C2 C3 59.62(15) . . . . ? C1 C2 C3 C4 -79.51(15) . . . . ? C2 C3 C4 C5 68.88(15) . . . . ? C3 C4 C5 C10 -63.53(14) . . . . ? C3 C4 C5 C6 174.00(10) . . . . ? C4 C5 C6 C7 66.19(11) . . . . ? C10 C5 C6 C7 -60.94(11) . . . . ? C4 C5 C6 C14 -60.14(12) . . . . ? C10 C5 C6 C14 172.73(9) . . . . ? C14 C6 C7 O2 3.14(16) . . . . ? C5 C6 C7 O2 -124.09(12) . . . . ? C14 C6 C7 C8 -177.82(10) . . . . ? C5 C6 C7 C8 54.94(13) . . . . ? O2 C7 C8 C9 131.24(12) . . . . ? C6 C7 C8 C9 -47.80(14) . . . . ? C7 C8 C9 C10 46.29(14) . . . . ? C1 N1 C10 C9 71.99(14) . . . . ? C13 N1 C10 C9 -104.03(11) . . . . ? C1 N1 C10 C11 -171.07(11) . . . . ? C13 N1 C10 C11 12.91(11) . . . . ? C1 N1 C10 C5 -53.72(15) . . . . ? C13 N1 C10 C5 130.26(10) . . . . ? C8 C9 C10 N1 177.93(9) . . . . ? C8 C9 C10 C11 67.38(12) . . . . ? C8 C9 C10 C5 -54.44(12) . . . . ? C4 C5 C10 N1 65.95(13) . . . . ? C6 C5 C10 N1 -171.73(9) . . . . ? C4 C5 C10 C9 -60.08(13) . . . . ? C6 C5 C10 C9 62.24(12) . . . . ? C4 C5 C10 C11 177.70(10) . . . . ? C6 C5 C10 C11 -59.98(12) . . . . ? N1 C10 C11 C12 -31.98(11) . . . . ? C9 C10 C11 C12 85.40(11) . . . . ? C5 C10 C11 C12 -152.38(10) . . . . ? C10 C11 C12 C13 39.76(12) . . . . ? C1 N1 C13 C12 -165.62(10) . . . . ? C10 N1 C13 C12 11.02(12) . . . . ? C11 C12 C13 N1 -30.68(12) . . . . ? C7 C6 C14 C15 76.39(13) . . . . ? C5 C6 C14 C15 -159.44(10) . . . . ? C6 C14 C15 C20 73.33(14) . . . . ? C6 C14 C15 C16 -104.83(13) . . . . ? C20 C15 C16 C17 -1.37(17) . . . . ? C14 C15 C16 C17 176.82(11) . . . . ? C15 C16 C17 C18 -0.30(18) . . . . ? C16 C17 C18 C19 1.54(17) . . . . ? C17 C18 C19 C20 -1.08(17) . . . . ? C18 C19 C20 C15 -0.63(17) . . . . ? C16 C15 C20 C19 1.83(17) . . . . ? C14 C15 C20 C19 -176.38(10) . . . . ? C33 N21 C21 O21 4.81(16) . . . . ? C30 N21 C21 O21 -178.13(10) . . . . ? C33 N21 C21 C22 -175.46(10) . . . . ? C30 N21 C21 C22 1.61(17) . . . . ? O21 C21 C22 C23 117.33(12) . . . . ? N21 C21 C22 C23 -62.40(14) . . . . ? C21 C22 C23 C24 78.76(13) . . . . ? C22 C23 C24 C25 -65.03(13) . . . . ? C23 C24 C25 C30 61.50(13) . . . . ? C23 C24 C25 C26 -176.59(9) . . . . ? C24 C25 C26 C27 -64.29(11) . . . . ? C30 C25 C26 C27 62.92(11) . . . . ? C24 C25 C26 C34 62.47(12) . . . . ? C30 C25 C26 C34 -170.32(9) . . . . ? C34 C26 C27 O22 -5.12(15) . . . . ? C25 C26 C27 O22 123.29(11) . . . . ? C34 C26 C27 C28 175.23(10) . . . . ? C25 C26 C27 C28 -56.36(12) . . . . ? O22 C27 C28 C29 -132.53(12) . . . . ? C26 C27 C28 C29 47.12(14) . . . . ? C27 C28 C29 C30 -44.45(14) . . . . ? C21 N21 C30 C29 -71.38(14) . . . . ? C33 N21 C30 C29 105.78(11) . . . . ? C21 N21 C30 C31 171.75(11) . . . . ? C33 N21 C30 C31 -11.09(12) . . . . ? C21 N21 C30 C25 54.47(15) . . . . ? C33 N21 C30 C25 -128.37(10) . . . . ? C28 C29 C30 N21 -178.70(9) . . . . ? C28 C29 C30 C31 -68.25(13) . . . . ? C28 C29 C30 C25 53.65(13) . . . . ? C24 C25 C30 N21 -66.94(12) . . . . ? C26 C25 C30 N21 170.47(9) . . . . ? C24 C25 C30 C29 59.43(12) . . . . ? C26 C25 C30 C29 -63.16(11) . . . . ? C24 C25 C30 C31 -178.39(10) . . . . ? C26 C25 C30 C31 59.01(11) . . . . ? N21 C30 C31 C32 31.90(12) . . . . ? C29 C30 C31 C32 -85.76(12) . . . . ? C25 C30 C31 C32 152.01(10) . . . . ? C30 C31 C32 C33 -41.27(13) . . . . ? C21 N21 C33 C32 163.73(10) . . . . ? C30 N21 C33 C32 -13.85(13) . . . . ? C31 C32 C33 N21 33.14(13) . . . . ? C27 C26 C34 C35 -70.68(12) . . . . ? C25 C26 C34 C35 164.91(9) . . . . ? C26 C34 C35 C36 112.34(12) . . . . ? C26 C34 C35 C40 -65.84(13) . . . . ? C40 C35 C36 C37 0.83(16) . . . . ? C34 C35 C36 C37 -177.39(10) . . . . ? C35 C36 C37 C38 -0.31(17) . . . . ? C36 C37 C38 C39 -0.65(17) . . . . ? C37 C38 C39 C40 1.06(17) . . . . ? C38 C39 C40 C35 -0.53(17) . . . . ? C36 C35 C40 C39 -0.41(16) . . . . ? C34 C35 C40 C39 177.82(10) . . . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 66.00 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.286 _refine_diff_density_min -0.168 _refine_diff_density_rms 0.033