data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H21 N O3' _chemical_formula_weight 383.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 8.3461(7) _cell_length_b 18.8665(17) _cell_length_c 23.936(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3769.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 15370 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.8 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type 'Numerical' _exptl_absorpt_correction_T_min 0.9805 _exptl_absorpt_correction_T_max 0.9936 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63026 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7411 _reflns_number_gt 7314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 3.7.0' _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0499P)^2^+0.8919P] 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 0.0060(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.3(11) _refine_ls_number_reflns 7411 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 1.268 _refine_ls_restrained_S_all 1.268 _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 0.9051(2) 0.16123(10) 0.40454(7) 0.0453(5) Uani 1 1 d . . . O2 O 1.1172(2) 0.13386(12) 0.35343(8) 0.0543(5) Uani 1 1 d . . . O3 O 0.6551(2) 0.30095(9) 0.25543(7) 0.0398(4) Uani 1 1 d . . . O4 O 1.4567(2) 0.04873(10) 0.15816(8) 0.0486(5) Uani 1 1 d . . . O5 O 1.3712(3) 0.10370(11) 0.23432(9) 0.0546(5) Uani 1 1 d . . . O6 O 0.9626(2) -0.08005(10) 0.12900(8) 0.0466(5) Uani 1 1 d . . . N1 N 0.9803(3) 0.17305(12) 0.25602(9) 0.0384(5) Uani 1 1 d . . . N2 N 1.1317(3) 0.00815(12) 0.25418(10) 0.0404(5) Uani 1 1 d . . . C1 C 0.7460(3) 0.18318(14) 0.40865(11) 0.0420(6) Uani 1 1 d . . . C2 C 0.6815(4) 0.18340(16) 0.46209(11) 0.0492(7) Uani 1 1 d . . . H1 H 0.7448 0.1704 0.4934 0.059 Uiso 1 1 calc R . . C3 C 0.5238(4) 0.20283(16) 0.46861(12) 0.0518(7) Uani 1 1 d . . . H2 H 0.4776 0.2039 0.5049 0.062 Uiso 1 1 calc R . . C4 C 0.4312(4) 0.22104(15) 0.42210(12) 0.0502(7) Uani 1 1 d . . . H3 H 0.3218 0.2336 0.4267 0.060 Uiso 1 1 calc R . . C5 C 0.4991(3) 0.22078(14) 0.36923(11) 0.0432(6) Uani 1 1 d . . . H4 H 0.4354 0.2334 0.3379 0.052 Uiso 1 1 calc R . . C6 C 0.6601(3) 0.20225(13) 0.36120(11) 0.0378(6) Uani 1 1 d . . . C7 C 0.7393(3) 0.20149(12) 0.30719(10) 0.0339(5) Uani 1 1 d . . . C8 C 0.8930(3) 0.17863(13) 0.30469(10) 0.0351(5) Uani 1 1 d . . . C9 C 0.9805(3) 0.15565(15) 0.35429(11) 0.0416(6) Uani 1 1 d . . . C10 C 0.6560(3) 0.22462(13) 0.25439(10) 0.0364(5) Uani 1 1 d . . . H5 H 0.5431 0.2069 0.2548 0.044 Uiso 1 1 calc R . . C11 C 0.5736(4) 0.33006(15) 0.20771(12) 0.0483(7) Uani 1 1 d . . . H6 H 0.5710 0.3824 0.2108 0.058 Uiso 1 1 calc R . . H7 H 0.4616 0.3128 0.2072 0.058 Uiso 1 1 calc R . . C12 C 0.6555(4) 0.30940(15) 0.15361(11) 0.0463(7) Uani 1 1 d . . . H8 H 0.7647 0.3299 0.1525 0.056 Uiso 1 1 calc R . . H9 H 0.5944 0.3284 0.1215 0.056 Uiso 1 1 calc R . . C13 C 0.6653(3) 0.22891(15) 0.14940(11) 0.0452(6) Uani 1 1 d . . . H10 H 0.7300 0.2158 0.1163 0.054 Uiso 1 1 calc R . . H11 H 0.5563 0.2093 0.1443 0.054 Uiso 1 1 calc R . . C14 C 0.7412(3) 0.19665(13) 0.20196(10) 0.0375(6) Uani 1 1 d . . . H12 H 0.7259 0.1441 0.2005 0.045 Uiso 1 1 calc R . . C15 C 0.9209(3) 0.21164(13) 0.20700(10) 0.0350(5) Uani 1 1 d . . . H13 H 0.9350 0.2635 0.2141 0.042 Uiso 1 1 calc R . . C16 C 1.0204(3) 0.19226(13) 0.15693(10) 0.0369(6) Uani 1 1 d . . . C17 C 1.1183(3) 0.24120(14) 0.13232(10) 0.0369(5) Uani 1 1 d . . . H14 H 1.1225 0.2878 0.1473 0.044 Uiso 1 1 calc R . . C18 C 1.2142(3) 0.22453(14) 0.08484(10) 0.0375(6) Uani 1 1 d . . . C19 C 1.3089(3) 0.27618(15) 0.05798(12) 0.0460(6) Uani 1 1 d . . . H15 H 1.3129 0.3231 0.0724 0.055 Uiso 1 1 calc R . . C20 C 1.3952(4) 0.25918(17) 0.01129(13) 0.0541(8) Uani 1 1 d . . . H16 H 1.4589 0.2943 -0.0064 0.065 Uiso 1 1 calc R . . C21 C 1.3905(4) 0.18999(16) -0.01080(13) 0.0543(8) Uani 1 1 d . . . H17 H 1.4490 0.1789 -0.0437 0.065 Uiso 1 1 calc R . . C22 C 1.3016(3) 0.13873(15) 0.01518(11) 0.0460(6) Uani 1 1 d . . . H18 H 1.3012 0.0919 0.0006 0.055 Uiso 1 1 calc R . . C23 C 1.2102(3) 0.15432(14) 0.06347(10) 0.0379(6) Uani 1 1 d . . . C24 C 1.1098(3) 0.10410(14) 0.08985(11) 0.0414(6) Uani 1 1 d . . . H19 H 1.1065 0.0569 0.0761 0.050 Uiso 1 1 calc R . . C25 C 1.0171(3) 0.12215(13) 0.13489(11) 0.0399(6) Uani 1 1 d . . . H20 H 0.9499 0.0875 0.1516 0.048 Uiso 1 1 calc R . . C26 C 1.4370(3) -0.00218(15) 0.11702(11) 0.0438(6) Uani 1 1 d . . . C27 C 1.5412(4) 0.00132(17) 0.07193(13) 0.0559(8) Uani 1 1 d . . . H21 H 1.6225 0.0365 0.0705 0.067 Uiso 1 1 calc R . . C28 C 1.5245(4) -0.04724(19) 0.02932(13) 0.0594(8) Uani 1 1 d . . . H22 H 1.5942 -0.0453 -0.0020 0.071 Uiso 1 1 calc R . . C29 C 1.4066(4) -0.09895(17) 0.03188(12) 0.0566(8) Uani 1 1 d . . . H23 H 1.3964 -0.1324 0.0024 0.068 Uiso 1 1 calc R . . C30 C 1.3031(4) -0.10217(16) 0.07733(12) 0.0500(7) Uani 1 1 d . . . H24 H 1.2232 -0.1380 0.0788 0.060 Uiso 1 1 calc R . . C31 C 1.3160(3) -0.05277(14) 0.12109(11) 0.0423(6) Uani 1 1 d . . . C32 C 1.2100(3) -0.05086(13) 0.16877(11) 0.0395(6) Uani 1 1 d . . . C33 C 1.2293(3) 0.00078(13) 0.20784(11) 0.0386(6) Uani 1 1 d . . . C34 C 1.3544(3) 0.05412(15) 0.20232(12) 0.0443(6) Uani 1 1 d . . . C35 C 1.0710(3) -0.10133(14) 0.17279(11) 0.0399(6) Uani 1 1 d . . . H25 H 1.1097 -0.1505 0.1650 0.048 Uiso 1 1 calc R . . C36 C 0.8239(4) -0.12523(16) 0.12696(13) 0.0539(7) Uani 1 1 d . . . H26 H 0.8580 -0.1750 0.1214 0.065 Uiso 1 1 calc R . . H27 H 0.7555 -0.1115 0.0950 0.065 Uiso 1 1 calc R . . C37 C 0.7293(3) -0.11935(15) 0.18032(13) 0.0508(7) Uani 1 1 d . . . H28 H 0.6334 -0.1502 0.1783 0.061 Uiso 1 1 calc R . . H29 H 0.6930 -0.0698 0.1856 0.061 Uiso 1 1 calc R . . C38 C 0.8343(3) -0.14183(14) 0.22932(12) 0.0457(7) Uani 1 1 d . . . H30 H 0.8584 -0.1931 0.2263 0.055 Uiso 1 1 calc R . . H31 H 0.7756 -0.1339 0.2647 0.055 Uiso 1 1 calc R . . C39 C 0.9915(3) -0.09968(13) 0.23023(11) 0.0388(6) Uani 1 1 d . . . H32 H 1.0654 -0.1240 0.2570 0.047 Uiso 1 1 calc R . . C40 C 0.9711(3) -0.02259(13) 0.25046(11) 0.0375(5) Uani 1 1 d . . . H33 H 0.9081 0.0043 0.2219 0.045 Uiso 1 1 calc R . . C41 C 0.8852(3) -0.01836(13) 0.30582(11) 0.0373(6) Uani 1 1 d . . . C42 C 0.7315(3) 0.00752(13) 0.30844(11) 0.0402(6) Uani 1 1 d . . . H34 H 0.6835 0.0261 0.2756 0.048 Uiso 1 1 calc R . . C43 C 0.6426(3) 0.00721(13) 0.35883(11) 0.0386(6) Uani 1 1 d . . . C44 C 0.4843(3) 0.03396(14) 0.36226(12) 0.0449(6) Uani 1 1 d . . . H35 H 0.4344 0.0523 0.3297 0.054 Uiso 1 1 calc R . . C45 C 0.4023(4) 0.03382(16) 0.41162(12) 0.0505(7) Uani 1 1 d . . . H36 H 0.2969 0.0528 0.4132 0.061 Uiso 1 1 calc R . . C46 C 0.4729(4) 0.00585(16) 0.45982(13) 0.0516(7) Uani 1 1 d . . . H37 H 0.4149 0.0061 0.4940 0.062 Uiso 1 1 calc R . . C47 C 0.6246(4) -0.02185(15) 0.45843(12) 0.0486(7) Uani 1 1 d . . . H38 H 0.6701 -0.0416 0.4913 0.058 Uiso 1 1 calc R . . C48 C 0.7143(3) -0.02100(14) 0.40773(11) 0.0416(6) Uani 1 1 d . . . C49 C 0.8737(3) -0.04636(14) 0.40423(11) 0.0434(6) Uani 1 1 d . . . H39 H 0.9236 -0.0650 0.4367 0.052 Uiso 1 1 calc R . . C50 C 0.9570(3) -0.04466(14) 0.35533(11) 0.0424(6) Uani 1 1 d . . . H40 H 1.0644 -0.0613 0.3544 0.051 Uiso 1 1 calc R . . H41 H 1.087(4) 0.1705(14) 0.2608(11) 0.041(8) Uiso 1 1 d . . . H42 H 1.143(4) 0.0490(17) 0.2744(12) 0.055(9) 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 0.0440(11) 0.0563(12) 0.0358(9) 0.0044(8) -0.0027(8) 0.0088(9) O2 0.0413(11) 0.0745(14) 0.0471(11) 0.0076(10) -0.0037(9) 0.0105(10) O3 0.0419(10) 0.0349(9) 0.0426(10) 0.0026(7) -0.0038(8) 0.0034(7) O4 0.0446(11) 0.0503(11) 0.0508(11) 0.0053(9) 0.0057(9) -0.0044(9) O5 0.0574(12) 0.0502(11) 0.0561(12) -0.0058(10) 0.0024(10) -0.0200(10) O6 0.0491(11) 0.0440(10) 0.0467(10) 0.0004(8) -0.0089(9) 0.0002(9) N1 0.0331(11) 0.0433(12) 0.0387(11) 0.0026(9) -0.0009(10) 0.0041(9) N2 0.0385(11) 0.0372(12) 0.0456(12) -0.0025(10) 0.0002(10) -0.0076(9) C1 0.0439(15) 0.0362(14) 0.0459(15) 0.0009(12) -0.0011(12) 0.0000(11) C2 0.0582(19) 0.0530(17) 0.0363(14) 0.0020(12) -0.0017(13) 0.0029(14) C3 0.062(2) 0.0510(17) 0.0419(15) 0.0011(12) 0.0116(14) 0.0059(14) C4 0.0492(17) 0.0495(16) 0.0520(16) 0.0037(13) 0.0115(14) 0.0083(13) C5 0.0468(15) 0.0387(14) 0.0442(14) 0.0022(11) -0.0003(12) 0.0052(12) C6 0.0407(14) 0.0314(12) 0.0414(14) -0.0005(10) 0.0005(12) 0.0009(10) C7 0.0346(13) 0.0314(12) 0.0357(12) -0.0004(10) -0.0016(11) -0.0016(10) C8 0.0375(13) 0.0335(12) 0.0343(12) 0.0003(10) -0.0032(11) -0.0028(11) C9 0.0402(15) 0.0454(14) 0.0391(14) 0.0008(11) -0.0029(12) 0.0036(12) C10 0.0333(12) 0.0351(13) 0.0409(13) 0.0032(11) 0.0002(11) -0.0008(10) C11 0.0490(16) 0.0459(15) 0.0499(16) 0.0102(13) -0.0056(13) 0.0089(13) C12 0.0474(16) 0.0471(15) 0.0443(15) 0.0120(12) -0.0049(13) 0.0007(13) C13 0.0389(14) 0.0573(17) 0.0394(14) 0.0014(13) -0.0033(12) -0.0012(13) C14 0.0386(14) 0.0346(13) 0.0394(13) 0.0005(11) 0.0016(11) -0.0034(10) C15 0.0367(14) 0.0325(12) 0.0357(12) 0.0023(10) 0.0008(11) 0.0017(10) C16 0.0371(13) 0.0361(13) 0.0374(13) 0.0016(10) -0.0011(11) 0.0035(11) C17 0.0343(13) 0.0376(13) 0.0389(13) -0.0001(10) -0.0005(11) 0.0011(10) C18 0.0300(12) 0.0418(14) 0.0408(13) 0.0069(11) -0.0034(11) 0.0030(11) C19 0.0390(15) 0.0418(15) 0.0573(16) 0.0033(13) 0.0037(13) -0.0034(12) C20 0.0446(16) 0.0558(18) 0.0619(18) 0.0052(15) 0.0161(15) -0.0029(14) C21 0.0508(17) 0.0557(18) 0.0565(17) 0.0027(14) 0.0152(15) 0.0041(14) C22 0.0450(15) 0.0456(15) 0.0475(15) -0.0009(12) 0.0074(13) 0.0067(13) C23 0.0372(14) 0.0376(13) 0.0388(13) 0.0037(11) -0.0018(11) 0.0048(11) C24 0.0509(16) 0.0321(12) 0.0413(14) 0.0025(11) -0.0027(12) 0.0019(12) C25 0.0445(15) 0.0358(13) 0.0392(13) 0.0018(11) 0.0000(12) -0.0002(11) C26 0.0419(15) 0.0455(15) 0.0439(14) 0.0019(12) -0.0003(12) 0.0088(12) C27 0.0536(17) 0.0548(17) 0.0594(18) 0.0153(15) 0.0097(15) 0.0066(15) C28 0.062(2) 0.065(2) 0.0509(17) 0.0110(15) 0.0130(15) 0.0203(17) C29 0.071(2) 0.0540(18) 0.0449(16) -0.0010(14) 0.0048(15) 0.0212(16) C30 0.0581(18) 0.0451(15) 0.0469(15) 0.0003(13) -0.0022(14) 0.0090(14) C31 0.0428(15) 0.0407(14) 0.0434(14) 0.0048(11) -0.0005(12) 0.0106(12) C32 0.0389(14) 0.0341(13) 0.0454(14) 0.0036(11) -0.0032(12) 0.0039(11) C33 0.0357(13) 0.0355(13) 0.0447(14) 0.0047(11) -0.0008(11) 0.0010(10) C34 0.0386(15) 0.0469(15) 0.0473(15) 0.0068(13) -0.0015(13) -0.0033(12) C35 0.0406(15) 0.0365(13) 0.0425(13) 0.0001(11) -0.0059(12) 0.0027(11) C36 0.0485(17) 0.0483(16) 0.0650(18) -0.0086(14) -0.0182(15) 0.0009(13) C37 0.0399(15) 0.0429(16) 0.0697(19) -0.0038(14) -0.0121(14) -0.0002(12) C38 0.0410(14) 0.0375(14) 0.0585(17) 0.0019(12) -0.0046(13) -0.0042(12) C39 0.0372(14) 0.0323(13) 0.0469(14) 0.0031(11) -0.0040(11) 0.0002(10) C40 0.0369(13) 0.0338(13) 0.0419(13) 0.0023(11) -0.0014(12) -0.0039(10) C41 0.0372(13) 0.0337(12) 0.0412(13) 0.0013(10) 0.0011(11) -0.0024(11) C42 0.0412(14) 0.0362(13) 0.0433(14) 0.0061(11) -0.0011(12) -0.0002(11) C43 0.0401(14) 0.0326(12) 0.0429(14) 0.0030(11) -0.0029(11) -0.0020(11) C44 0.0387(14) 0.0474(15) 0.0485(15) 0.0097(12) -0.0029(12) 0.0010(12) C45 0.0443(16) 0.0531(17) 0.0542(16) 0.0057(14) 0.0028(14) 0.0038(13) C46 0.0507(17) 0.0549(17) 0.0491(16) 0.0089(14) 0.0091(14) 0.0030(14) C47 0.0543(17) 0.0498(16) 0.0416(15) 0.0072(12) -0.0009(13) 0.0033(14) C48 0.0401(14) 0.0373(14) 0.0473(15) 0.0012(11) -0.0018(12) 0.0007(11) C49 0.0475(15) 0.0430(14) 0.0398(14) 0.0042(12) -0.0039(12) 0.0057(12) C50 0.0399(14) 0.0427(14) 0.0446(14) -0.0008(12) -0.0053(12) 0.0049(11) _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 C9 1.362(3) . ? O1 C1 1.395(3) . ? O2 C9 1.213(3) . ? O3 C11 1.438(3) . ? O3 C10 1.440(3) . ? O4 C34 1.363(3) . ? O4 C26 1.385(3) . ? O5 C34 1.217(3) . ? O6 C36 1.439(4) . ? O6 C35 1.441(3) . ? N1 C8 1.378(3) . ? N1 C15 1.467(3) . ? N2 C33 1.383(3) . ? N2 C40 1.463(3) . ? C1 C2 1.388(4) . ? C1 C6 1.390(4) . ? C2 C3 1.375(4) . ? C3 C4 1.398(4) . ? C4 C5 1.387(4) . ? C5 C6 1.401(4) . ? C6 C7 1.452(3) . ? C7 C8 1.355(4) . ? C7 C10 1.507(3) . ? C8 C9 1.460(3) . ? C10 C14 1.536(3) . ? C11 C12 1.516(4) . ? C12 C13 1.524(4) . ? C13 C14 1.534(4) . ? C14 C15 1.532(4) . ? C15 C16 1.503(3) . ? C16 C17 1.366(4) . ? C16 C25 1.424(3) . ? C17 C18 1.425(4) . ? C18 C19 1.410(4) . ? C18 C23 1.420(4) . ? C19 C20 1.368(4) . ? C20 C21 1.409(4) . ? C21 C22 1.368(4) . ? C22 C23 1.416(4) . ? C23 C24 1.414(4) . ? C24 C25 1.370(4) . ? C26 C27 1.388(4) . ? C26 C31 1.393(4) . ? C27 C28 1.378(5) . ? C28 C29 1.387(5) . ? C29 C30 1.390(4) . ? C30 C31 1.406(4) . ? C31 C32 1.444(4) . ? C32 C33 1.360(4) . ? C32 C35 1.504(4) . ? C33 C34 1.456(4) . ? C35 C39 1.527(4) . ? C36 C37 1.506(4) . ? C37 C38 1.524(4) . ? C38 C39 1.535(4) . ? C39 C40 1.542(3) . ? C40 C41 1.509(4) . ? C41 C42 1.374(4) . ? C41 C50 1.418(4) . ? C42 C43 1.416(4) . ? C43 C44 1.417(4) . ? C43 C48 1.418(4) . ? C44 C45 1.365(4) . ? C45 C46 1.399(4) . ? C46 C47 1.370(4) . ? C47 C48 1.426(4) . ? C48 C49 1.416(4) . ? C49 C50 1.362(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 C9 O1 C1 121.7(2) . . ? C11 O3 C10 111.75(19) . . ? C34 O4 C26 121.9(2) . . ? C36 O6 C35 111.4(2) . . ? C8 N1 C15 117.3(2) . . ? C33 N2 C40 116.8(2) . . ? C2 C1 C6 123.5(3) . . ? C2 C1 O1 115.8(2) . . ? C6 C1 O1 120.7(2) . . ? C3 C2 C1 118.5(3) . . ? C2 C3 C4 120.3(3) . . ? C5 C4 C3 120.0(3) . . ? C4 C5 C6 121.2(3) . . ? C1 C6 C5 116.5(2) . . ? C1 C6 C7 119.4(2) . . ? C5 C6 C7 124.1(2) . . ? C8 C7 C6 118.3(2) . . ? C8 C7 C10 119.5(2) . . ? C6 C7 C10 122.3(2) . . ? C7 C8 N1 124.2(2) . . ? C7 C8 C9 122.2(2) . . ? N1 C8 C9 113.6(2) . . ? O2 C9 O1 118.4(2) . . ? O2 C9 C8 123.9(2) . . ? O1 C9 C8 117.6(2) . . ? O3 C10 C7 106.11(19) . . ? O3 C10 C14 111.1(2) . . ? C7 C10 C14 111.8(2) . . ? O3 C11 C12 111.5(2) . . ? C11 C12 C13 109.7(2) . . ? C12 C13 C14 111.3(2) . . ? C15 C14 C13 113.3(2) . . ? C15 C14 C10 109.0(2) . . ? C13 C14 C10 110.0(2) . . ? N1 C15 C16 109.29(19) . . ? N1 C15 C14 107.6(2) . . ? C16 C15 C14 115.7(2) . . ? C17 C16 C25 118.6(2) . . ? C17 C16 C15 120.6(2) . . ? C25 C16 C15 120.7(2) . . ? C16 C17 C18 122.0(2) . . ? C19 C18 C23 119.6(2) . . ? C19 C18 C17 121.7(2) . . ? C23 C18 C17 118.7(2) . . ? C20 C19 C18 120.4(3) . . ? C19 C20 C21 120.6(3) . . ? C22 C21 C20 120.0(3) . . ? C21 C22 C23 121.1(3) . . ? C24 C23 C22 123.0(2) . . ? C24 C23 C18 118.6(2) . . ? C22 C23 C18 118.4(2) . . ? C25 C24 C23 121.3(2) . . ? C24 C25 C16 120.8(2) . . ? O4 C26 C27 116.4(3) . . ? O4 C26 C31 120.8(2) . . ? C27 C26 C31 122.8(3) . . ? C28 C27 C26 118.7(3) . . ? C27 C28 C29 120.4(3) . . ? C28 C29 C30 120.4(3) . . ? C29 C30 C31 120.4(3) . . ? C26 C31 C30 117.2(3) . . ? C26 C31 C32 118.8(2) . . ? C30 C31 C32 123.9(3) . . ? C33 C32 C31 119.3(2) . . ? C33 C32 C35 120.0(2) . . ? C31 C32 C35 120.5(2) . . ? C32 C33 N2 123.6(2) . . ? C32 C33 C34 121.2(2) . . ? N2 C33 C34 115.2(2) . . ? O5 C34 O4 118.2(2) . . ? O5 C34 C33 123.8(3) . . ? O4 C34 C33 117.9(2) . . ? O6 C35 C32 105.1(2) . . ? O6 C35 C39 112.1(2) . . ? C32 C35 C39 112.3(2) . . ? O6 C36 C37 110.5(2) . . ? C36 C37 C38 109.3(2) . . ? C37 C38 C39 111.0(2) . . ? C35 C39 C38 110.4(2) . . ? C35 C39 C40 110.5(2) . . ? C38 C39 C40 113.5(2) . . ? N2 C40 C41 111.2(2) . . ? N2 C40 C39 107.0(2) . . ? C41 C40 C39 112.2(2) . . ? C42 C41 C50 118.8(2) . . ? C42 C41 C40 120.2(2) . . ? C50 C41 C40 121.0(2) . . ? C41 C42 C43 121.8(2) . . ? C42 C43 C44 122.4(2) . . ? C42 C43 C48 118.9(2) . . ? C44 C43 C48 118.6(2) . . ? C45 C44 C43 121.1(3) . . ? C44 C45 C46 120.2(3) . . ? C47 C46 C45 120.9(3) . . ? C46 C47 C48 120.1(3) . . ? C49 C48 C43 118.3(2) . . ? C49 C48 C47 122.7(2) . . ? C43 C48 C47 119.0(2) . . ? C50 C49 C48 121.5(3) . . ? C49 C50 C41 120.7(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.195 _refine_diff_density_min -0.181 _refine_diff_density_rms 0.042