# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2003data_global _publ_contact_author_email D.W.YOUNG@SUSSEX.AC.UK _publ_contact_author_name 'Prof Douglas W. Young' _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name D.W.Young P.B.Hitchcock K.Papadopoulos data_mar3800 _database_code_CSD 209161 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H25 N3 O5' _chemical_formula_weight 327.38 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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.2189(3) _cell_length_b 15.3206(5) _cell_length_c 27.7208(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4340.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12547 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 22.986 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 18133 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 4.54 _diffrn_reflns_theta_max 22.99 _reflns_number_total 5957 _reflns_number_gt 5026 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1307P)^2^+2.2895P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.7(18) _refine_ls_number_reflns 5957 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.2092 _refine_ls_wR_factor_gt 0.1961 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.6141(4) 0.6331(2) 0.54746(11) 0.0490(8) Uani 1 1 d . . . O2 O 0.3621(3) 0.5500(2) 0.61254(11) 0.0444(8) Uani 1 1 d . . . O3 O 0.3833(3) 0.4907(2) 0.53811(12) 0.0451(8) Uani 1 1 d . . . O4 O 0.6976(3) 0.3178(2) 0.60274(12) 0.0467(8) Uani 1 1 d . . . O5 O 0.7268(3) 0.32506(19) 0.52109(11) 0.0392(7) Uani 1 1 d . . . N1 N 0.7861(4) 0.6626(2) 0.59461(14) 0.0415(9) Uani 1 1 d . . . H1 H 0.8200 0.6953 0.5717 0.050 Uiso 1 1 calc R . . N2 N 0.8500(4) 0.6620(3) 0.63956(14) 0.0444(10) Uani 1 1 d . . . N3 N 0.6295(3) 0.4343(2) 0.55798(12) 0.0347(8) Uani 1 1 d . . . H3 H 0.6368 0.4610 0.5300 0.042 Uiso 1 1 calc R . . C1 C 0.6779(4) 0.6176(3) 0.58404(16) 0.0350(11) Uani 1 1 d . . . C2 C 0.6352(4) 0.5504(3) 0.62079(16) 0.0382(10) Uani 1 1 d . . . H2 H 0.5764 0.5798 0.6446 0.046 Uiso 1 1 calc R . . C3 C 0.7566(5) 0.5176(3) 0.64777(18) 0.0441(12) Uani 1 1 d . . . H3A H 0.7295 0.4822 0.6760 0.053 Uiso 1 1 calc R . . H3B H 0.8097 0.4802 0.6262 0.053 Uiso 1 1 calc R . . C4 C 0.8350(5) 0.5928(3) 0.66399(18) 0.0446(12) Uani 1 1 d . . . H4 H 0.8767 0.5892 0.6946 0.054 Uiso 1 1 calc R . . C5 C 0.5578(4) 0.4756(3) 0.59671(16) 0.0366(10) Uani 1 1 d . . . H5 H 0.5406 0.4303 0.6219 0.044 Uiso 1 1 calc R . . C6 C 0.4258(4) 0.5067(3) 0.57764(17) 0.0379(11) Uani 1 1 d . . . C7 C 0.2317(5) 0.5906(3) 0.60458(19) 0.0497(13) Uani 1 1 d . . . C8 C 0.1317(5) 0.5194(4) 0.5917(2) 0.0634(15) Uani 1 1 d . . . H8A H 0.0436 0.5446 0.5913 0.095 Uiso 1 1 calc R . . H8B H 0.1356 0.4727 0.6159 0.095 Uiso 1 1 calc R . . H8C H 0.1521 0.4954 0.5598 0.095 Uiso 1 1 calc R . . C9 C 0.2441(6) 0.6599(4) 0.5660(2) 0.0666(16) Uani 1 1 d . . . H9A H 0.3154 0.6999 0.5744 0.100 Uiso 1 1 calc R . . H9B H 0.1619 0.6927 0.5637 0.100 Uiso 1 1 calc R . . H9C H 0.2629 0.6322 0.5349 0.100 Uiso 1 1 calc R . . C10 C 0.2018(6) 0.6292(5) 0.6532(2) 0.0756(19) Uani 1 1 d . . . H10A H 0.1189 0.6612 0.6516 0.113 Uiso 1 1 calc R . . H10B H 0.2722 0.6692 0.6625 0.113 Uiso 1 1 calc R . . H10C H 0.1948 0.5823 0.6771 0.113 Uiso 1 1 calc R . . C11 C 0.6855(4) 0.3549(3) 0.56421(17) 0.0368(10) Uani 1 1 d . . . C12 C 0.8103(5) 0.2466(3) 0.51812(18) 0.0439(12) Uani 1 1 d . . . C13 C 0.7362(6) 0.1663(3) 0.5348(2) 0.0555(14) Uani 1 1 d . . . H13A H 0.7130 0.1726 0.5689 0.083 Uiso 1 1 calc R . . H13B H 0.7914 0.1145 0.5306 0.083 Uiso 1 1 calc R . . H13C H 0.6563 0.1598 0.5155 0.083 Uiso 1 1 calc R . . C14 C 0.9359(6) 0.2608(4) 0.5461(2) 0.0670(16) Uani 1 1 d . . . H14A H 0.9934 0.2102 0.5419 0.100 Uiso 1 1 calc R . . H14B H 0.9155 0.2682 0.5804 0.100 Uiso 1 1 calc R . . H14C H 0.9799 0.3133 0.5341 0.100 Uiso 1 1 calc R . . C15 C 0.8383(5) 0.2414(3) 0.46405(18) 0.0506(13) Uani 1 1 d . . . H15A H 0.7555 0.2376 0.4463 0.076 Uiso 1 1 calc R . . H15B H 0.8913 0.1895 0.4573 0.076 Uiso 1 1 calc R . . H15C H 0.8860 0.2937 0.4538 0.076 Uiso 1 1 calc R . . O1B O -0.1421(3) 0.8307(2) 0.56132(11) 0.0463(8) Uani 1 1 d . . . O2B O -0.3934(3) 0.9418(2) 0.60404(12) 0.0492(8) Uani 1 1 d . . . O3B O -0.3696(3) 0.8116(2) 0.64139(12) 0.0533(9) Uani 1 1 d . . . O4B O -0.0533(4) 0.9433(2) 0.73220(13) 0.0653(11) Uani 1 1 d . . . O5B O -0.0216(4) 0.7940(2) 0.73396(11) 0.0534(9) Uani 1 1 d . . . N1B N 0.0290(4) 0.9169(2) 0.54469(13) 0.0411(9) Uani 1 1 d . . . H1B H 0.0624 0.8757 0.5263 0.049 Uiso 1 1 calc R . . N2B N 0.0938(4) 0.9973(3) 0.54541(14) 0.0440(10) Uani 1 1 d . . . N3B N -0.1276(4) 0.8531(3) 0.67302(12) 0.0414(9) Uani 1 1 d . . . H3B1 H -0.1227 0.8003 0.6606 0.050 Uiso 1 1 calc R . . C1B C -0.0800(5) 0.8970(3) 0.56973(15) 0.0372(11) Uani 1 1 d . . . C2B C -0.1205(4) 0.9636(3) 0.60740(16) 0.0387(10) Uani 1 1 d . . . H2B H -0.1781 1.0074 0.5912 0.046 Uiso 1 1 calc R . . C3B C 0.0007(5) 1.0113(3) 0.62557(17) 0.0496(12) Uani 1 1 d . . . H3B1' H -0.0258 1.0620 0.6455 0.060 Uiso 1 1 calc R . . H3B2 H 0.0538 0.9717 0.6459 0.060 Uiso 1 1 calc R . . C4B C 0.0800(4) 1.0418(3) 0.58352(17) 0.0413(11) Uani 1 1 d . . . H4B H 0.1219 1.0971 0.5855 0.050 Uiso 1 1 calc R . . C5B C -0.2006(5) 0.9202(3) 0.64794(17) 0.0417(11) Uani 1 1 d . . . H5B H -0.2212 0.9667 0.6721 0.050 Uiso 1 1 calc R . . C6B C -0.3307(5) 0.8830(3) 0.63063(17) 0.0430(12) Uani 1 1 d . . . C7B C -0.5208(5) 0.9216(3) 0.5808(2) 0.0528(13) Uani 1 1 d . . . C8B C -0.6216(6) 0.9028(4) 0.6189(2) 0.0657(16) Uani 1 1 d . . . H8B1 H -0.5955 0.8510 0.6373 0.099 Uiso 1 1 calc R . . H8B2 H -0.7066 0.8923 0.6036 0.099 Uiso 1 1 calc R . . H8B3 H -0.6285 0.9529 0.6407 0.099 Uiso 1 1 calc R . . C9B C -0.5000(6) 0.8477(4) 0.5450(2) 0.0674(15) Uani 1 1 d . . . H9B1 H -0.5821 0.8356 0.5281 0.101 Uiso 1 1 calc R . . H9B2 H -0.4716 0.7952 0.5624 0.101 Uiso 1 1 calc R . . H9B3 H -0.4327 0.8645 0.5216 0.101 Uiso 1 1 calc R . . C10B C -0.5489(6) 1.0066(4) 0.5538(3) 0.0758(19) Uani 1 1 d . . . H10D H -0.5492 1.0553 0.5767 0.114 Uiso 1 1 calc R . . H10E H -0.6345 1.0027 0.5380 0.114 Uiso 1 1 calc R . . H10F H -0.4810 1.0163 0.5294 0.114 Uiso 1 1 calc R . . C11B C -0.0675(6) 0.8702(4) 0.71479(17) 0.0500(13) Uani 1 1 d . . . C12B C 0.0716(6) 0.7967(4) 0.77450(17) 0.0550(14) Uani 1 1 d . . . C13B C 0.0126(7) 0.8391(5) 0.81802(17) 0.0779(19) Uani 1 1 d . . . H13D H -0.0086 0.9000 0.8106 0.117 Uiso 1 1 calc R . . H13E H 0.0751 0.8370 0.8448 0.117 Uiso 1 1 calc R . . H13F H -0.0675 0.8080 0.8271 0.117 Uiso 1 1 calc R . . C14B C 0.1983(6) 0.8405(5) 0.7581(2) 0.0711(17) Uani 1 1 d . . . H14D H 0.2625 0.8384 0.7844 0.107 Uiso 1 1 calc R . . H14E H 0.1805 0.9015 0.7497 0.107 Uiso 1 1 calc R . . H14F H 0.2331 0.8098 0.7299 0.107 Uiso 1 1 calc R . . C15B C 0.0943(8) 0.7004(4) 0.7834(2) 0.081(2) Uani 1 1 d . . . H15D H 0.0105 0.6718 0.7903 0.121 Uiso 1 1 calc R . . H15E H 0.1532 0.6931 0.8110 0.121 Uiso 1 1 calc R . . H15F H 0.1338 0.6740 0.7547 0.121 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 0.064(2) 0.0360(17) 0.0471(18) 0.0033(15) -0.0196(17) -0.0053(16) O2 0.0327(17) 0.054(2) 0.0464(18) -0.0119(16) 0.0009(14) 0.0100(16) O3 0.0374(17) 0.0466(19) 0.051(2) -0.0138(15) -0.0016(15) -0.0039(15) O4 0.057(2) 0.0400(18) 0.0431(18) 0.0065(15) 0.0037(15) 0.0098(16) O5 0.0450(18) 0.0299(16) 0.0427(17) -0.0015(13) 0.0004(14) 0.0086(14) N1 0.041(2) 0.040(2) 0.043(2) 0.0002(18) -0.0063(17) -0.0042(19) N2 0.041(2) 0.043(2) 0.049(2) -0.003(2) -0.0091(18) 0.0011(19) N3 0.039(2) 0.0278(19) 0.0374(18) 0.0024(15) 0.0069(15) 0.0053(17) C1 0.038(3) 0.025(2) 0.043(3) -0.0062(19) -0.005(2) 0.003(2) C2 0.036(2) 0.037(3) 0.042(2) -0.003(2) -0.0017(19) 0.000(2) C3 0.040(3) 0.042(3) 0.050(3) 0.006(2) -0.011(2) 0.004(2) C4 0.037(3) 0.049(3) 0.048(3) -0.006(2) -0.008(2) 0.006(2) C5 0.037(2) 0.029(2) 0.044(2) -0.0003(19) 0.0033(19) 0.0010(19) C6 0.032(2) 0.034(2) 0.048(3) -0.003(2) 0.004(2) -0.004(2) C7 0.034(3) 0.054(3) 0.060(3) -0.015(3) 0.006(2) 0.005(2) C8 0.032(3) 0.077(4) 0.081(4) -0.016(3) 0.006(3) -0.009(3) C9 0.048(3) 0.055(3) 0.097(4) -0.002(3) -0.001(3) 0.012(3) C10 0.047(3) 0.101(5) 0.078(4) -0.041(4) -0.001(3) 0.022(3) C11 0.032(2) 0.035(3) 0.044(3) -0.001(2) -0.0006(19) -0.002(2) C12 0.044(3) 0.035(3) 0.053(3) -0.001(2) 0.001(2) 0.014(2) C13 0.070(4) 0.031(3) 0.065(3) 0.005(2) 0.007(3) 0.006(3) C14 0.052(3) 0.076(4) 0.073(4) -0.010(3) -0.006(3) 0.018(3) C15 0.060(3) 0.039(3) 0.053(3) -0.007(2) 0.012(2) 0.012(2) O1B 0.056(2) 0.0419(19) 0.0408(17) 0.0006(14) 0.0020(15) -0.0168(18) O2B 0.0343(18) 0.0438(19) 0.069(2) 0.0126(17) 0.0040(16) 0.0027(15) O3B 0.0414(19) 0.053(2) 0.066(2) 0.0128(18) 0.0044(17) 0.0019(18) O4B 0.103(3) 0.044(2) 0.049(2) -0.0145(18) -0.009(2) 0.000(2) O5B 0.076(3) 0.048(2) 0.0363(17) 0.0004(16) -0.0127(17) -0.0079(19) N1B 0.044(2) 0.034(2) 0.044(2) -0.0005(17) 0.0074(18) -0.0057(18) N2B 0.038(2) 0.043(2) 0.052(2) 0.008(2) -0.0045(18) -0.0097(18) N3B 0.051(2) 0.038(2) 0.035(2) -0.0025(17) -0.0009(17) 0.0014(19) C1B 0.040(3) 0.036(3) 0.035(2) 0.006(2) -0.007(2) -0.003(2) C2B 0.035(2) 0.036(2) 0.045(2) 0.003(2) 0.001(2) 0.000(2) C3B 0.055(3) 0.042(3) 0.052(3) -0.011(2) 0.003(2) -0.002(2) C4B 0.036(3) 0.037(3) 0.051(3) 0.000(2) -0.006(2) -0.008(2) C5B 0.044(3) 0.039(3) 0.042(2) 0.002(2) 0.003(2) 0.009(2) C6B 0.039(3) 0.039(3) 0.051(3) 0.005(2) 0.012(2) 0.003(2) C7B 0.030(3) 0.048(3) 0.080(4) 0.011(3) -0.004(2) -0.002(2) C8B 0.041(3) 0.074(4) 0.082(4) 0.015(3) 0.011(3) 0.002(3) C9B 0.052(3) 0.073(4) 0.077(4) -0.002(3) -0.004(3) -0.002(3) C10B 0.056(4) 0.065(4) 0.107(5) 0.037(4) -0.013(3) -0.002(3) C11B 0.066(3) 0.051(3) 0.034(2) -0.002(2) -0.001(2) 0.000(3) C12B 0.069(4) 0.059(3) 0.037(3) 0.003(2) -0.015(2) -0.001(3) C13B 0.094(5) 0.107(5) 0.032(3) -0.003(3) -0.008(3) -0.022(4) C14B 0.065(4) 0.084(5) 0.063(3) -0.011(3) -0.007(3) 0.000(4) C15B 0.102(5) 0.072(4) 0.068(4) 0.018(3) -0.032(4) -0.006(4) _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 1.229(5) . ? O2 C6 1.341(5) . ? O2 C7 1.487(6) . ? O3 C6 1.204(5) . ? O4 C11 1.216(5) . ? O5 C11 1.348(5) . ? O5 C12 1.476(5) . ? N1 C1 1.336(6) . ? N1 N2 1.407(5) . ? N2 C4 1.267(6) . ? N3 C11 1.354(6) . ? N3 C5 1.446(6) . ? C1 C2 1.512(6) . ? C2 C3 1.533(6) . ? C2 C5 1.545(6) . ? C3 C4 1.474(7) . ? C5 C6 1.525(7) . ? C7 C10 1.503(7) . ? C7 C9 1.513(8) . ? C7 C8 1.537(7) . ? C12 C14 1.515(8) . ? C12 C13 1.517(7) . ? C12 C15 1.528(7) . ? O1B C1B 1.221(5) . ? O2B C6B 1.329(6) . ? O2B C7B 1.486(6) . ? O3B C6B 1.202(6) . ? O4B C11B 1.227(6) . ? O5B C11B 1.367(6) . ? O5B C12B 1.474(6) . ? N1B C1B 1.347(6) . ? N1B N2B 1.399(5) . ? N2B C4B 1.265(6) . ? N3B C11B 1.337(6) . ? N3B C5B 1.448(6) . ? C1B C2B 1.517(6) . ? C2B C3B 1.524(7) . ? C2B C5B 1.540(7) . ? C3B C4B 1.495(7) . ? C5B C6B 1.524(7) . ? C7B C8B 1.504(8) . ? C7B C9B 1.519(8) . ? C7B C10B 1.528(8) . ? C12B C13B 1.497(8) . ? C12B C15B 1.513(9) . ? C12B C14B 1.527(9) . ? 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 O2 C7 122.3(4) . . ? C11 O5 C12 120.5(3) . . ? C1 N1 N2 125.1(4) . . ? C4 N2 N1 115.0(4) . . ? C11 N3 C5 120.8(4) . . ? O1 C1 N1 121.3(4) . . ? O1 C1 C2 122.3(4) . . ? N1 C1 C2 116.3(4) . . ? C1 C2 C3 108.6(4) . . ? C1 C2 C5 111.2(4) . . ? C3 C2 C5 112.4(4) . . ? C4 C3 C2 109.4(4) . . ? N2 C4 C3 123.8(4) . . ? N3 C5 C6 109.1(4) . . ? N3 C5 C2 112.7(3) . . ? C6 C5 C2 111.8(4) . . ? O3 C6 O2 125.6(4) . . ? O3 C6 C5 124.8(4) . . ? O2 C6 C5 109.5(4) . . ? O2 C7 C10 102.3(4) . . ? O2 C7 C9 108.9(4) . . ? C10 C7 C9 112.0(5) . . ? O2 C7 C8 109.5(4) . . ? C10 C7 C8 110.6(5) . . ? C9 C7 C8 113.0(5) . . ? O4 C11 O5 126.0(4) . . ? O4 C11 N3 125.1(4) . . ? O5 C11 N3 108.9(4) . . ? O5 C12 C14 110.1(4) . . ? O5 C12 C13 110.8(4) . . ? C14 C12 C13 112.6(5) . . ? O5 C12 C15 101.9(4) . . ? C14 C12 C15 110.6(5) . . ? C13 C12 C15 110.4(4) . . ? C6B O2B C7B 121.5(4) . . ? C11B O5B C12B 119.6(4) . . ? C1B N1B N2B 125.6(4) . . ? C4B N2B N1B 115.7(4) . . ? C11B N3B C5B 120.8(4) . . ? O1B C1B N1B 121.3(4) . . ? O1B C1B C2B 123.3(4) . . ? N1B C1B C2B 115.4(4) . . ? C1B C2B C3B 109.2(4) . . ? C1B C2B C5B 110.9(4) . . ? C3B C2B C5B 113.4(4) . . ? C4B C3B C2B 109.4(4) . . ? N2B C4B C3B 122.9(4) . . ? N3B C5B C6B 109.5(4) . . ? N3B C5B C2B 112.5(4) . . ? C6B C5B C2B 113.3(4) . . ? O3B C6B O2B 126.5(5) . . ? O3B C6B C5B 123.5(4) . . ? O2B C6B C5B 110.0(4) . . ? O2B C7B C8B 109.5(4) . . ? O2B C7B C9B 108.4(4) . . ? C8B C7B C9B 114.3(5) . . ? O2B C7B C10B 101.5(4) . . ? C8B C7B C10B 112.2(5) . . ? C9B C7B C10B 110.1(5) . . ? O4B C11B N3B 125.1(5) . . ? O4B C11B O5B 125.9(4) . . ? N3B C11B O5B 109.0(4) . . ? O5B C12B C13B 111.5(5) . . ? O5B C12B C15B 101.3(4) . . ? C13B C12B C15B 110.7(5) . . ? O5B C12B C14B 109.5(4) . . ? C13B C12B C14B 112.9(5) . . ? C15B C12B C14B 110.3(6) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.656 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.069 #===END