data_yosa _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 N2 O7' _chemical_formula_weight 458.50 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 Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.979(2) _cell_length_b 9.2119(18) _cell_length_c 11.677(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.66(3) _cell_angle_gamma 90.00 _cell_volume 1180.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2879 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 26.59 _exptl_crystal_description Parallalepiped _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9794 _exptl_absorpt_correction_T_max 0.9877 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 '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_% 1 _diffrn_reflns_number 8686 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4105 _reflns_number_gt 3118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0560P)^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 constr _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 -0.3(17) _refine_ls_number_reflns 4105 _refine_ls_number_parameters 304 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1344 _refine_ls_wR_factor_gt 0.1245 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.100 _refine_ls_shift/su_mean 0.008 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 0.7929(2) 0.0965(3) 0.8838(2) 0.0482(7) Uani 1 1 d . . . H1 H 0.8259 0.0180 0.8957 0.058 Uiso 1 1 calc R . . O2 O 0.6473(3) -0.1401(4) 0.8433(3) 0.0748(10) Uani 1 1 d . . . O3 O 0.5205(3) 0.0073(4) 0.7498(3) 0.0794(10) Uani 1 1 d . . . O4 O 0.5821(2) 0.2757(3) 0.8348(2) 0.0555(8) Uani 1 1 d . . . O5 O 0.4476(3) 0.3283(5) 0.6954(3) 0.1029(14) Uani 1 1 d . . . O6 O 1.1292(2) 0.1646(3) 0.8854(2) 0.0604(8) Uani 1 1 d . . . O7 O 1.0826(3) 0.3483(4) 1.0569(2) 0.0677(9) Uani 1 1 d . . . H7 H 1.1228 0.2921 1.0181 0.081 Uiso 1 1 calc R . . N1 N 0.7424(3) 0.0135(3) 0.5744(3) 0.0451(8) Uani 1 1 d . . . N2 N 0.9748(3) 0.3036(3) 0.8095(2) 0.0404(7) Uani 1 1 d . . . C1 C 0.9777(4) 0.2251(5) 0.4439(3) 0.0523(11) Uani 1 1 d . . . H1A H 1.0425 0.2826 0.4687 0.063 Uiso 1 1 calc R . . C2 C 0.9549(4) 0.2060(5) 0.3286(4) 0.0576(12) Uani 1 1 d . . . H2 H 1.0055 0.2496 0.2754 0.069 Uiso 1 1 calc R . . C3 C 0.8588(4) 0.1240(5) 0.2915(3) 0.0549(11) Uani 1 1 d . . . H3 H 0.8436 0.1144 0.2134 0.066 Uiso 1 1 calc R . . C4 C 0.7837(4) 0.0550(5) 0.3687(3) 0.0529(11) Uani 1 1 d . . . H4 H 0.7193 -0.0025 0.3433 0.063 Uiso 1 1 calc R . . C5 C 0.8068(3) 0.0733(4) 0.4850(3) 0.0397(9) Uani 1 1 d . . . C6 C 0.9032(3) 0.1577(4) 0.5223(3) 0.0373(9) Uani 1 1 d . . . C7 C 0.9102(3) 0.1561(4) 0.6511(3) 0.0392(9) Uani 1 1 d . . . C8 C 0.8104(3) 0.0415(4) 0.6825(3) 0.0414(9) Uani 1 1 d . . . H8 H 0.8514 -0.0485 0.7056 0.050 Uiso 1 1 calc R . . C9 C 0.7247(3) 0.0893(5) 0.7815(3) 0.0435(10) Uani 1 1 d . . . C10 C 0.6748(3) 0.2397(4) 0.7530(3) 0.0441(10) Uani 1 1 d . . . H10 H 0.6366 0.2356 0.6768 0.053 Uiso 1 1 calc R . . C11 C 0.7702(3) 0.3617(4) 0.7528(3) 0.0420(9) Uani 1 1 d . . . C12 C 0.8951(3) 0.3087(4) 0.7080(3) 0.0405(9) Uani 1 1 d . . . H12 H 0.9268 0.3822 0.6555 0.049 Uiso 1 1 calc R . . C13 C 1.0387(3) 0.1135(4) 0.6991(3) 0.0462(10) Uani 1 1 d . . . H13A H 1.0433 0.0097 0.7123 0.055 Uiso 1 1 calc R . . H13B H 1.1016 0.1406 0.6455 0.055 Uiso 1 1 calc R . . C14 C 1.0549(3) 0.1949(4) 0.8099(3) 0.0432(10) Uani 1 1 d . . . C15 C 0.9357(4) 0.4013(4) 0.9000(3) 0.0491(10) Uani 1 1 d . . . H15 H 0.9753 0.4959 0.8908 0.059 Uiso 1 1 calc R . . C16 C 0.7987(4) 0.4164(5) 0.8759(3) 0.0533(11) Uani 1 1 d . . . H16A H 0.7745 0.5172 0.8832 0.064 Uiso 1 1 calc R . . H16B H 0.7534 0.3597 0.9310 0.064 Uiso 1 1 calc R . . C17 C 0.6856(4) -0.1280(5) 0.5570(4) 0.0605(12) Uani 1 1 d . . . H17A H 0.6023 -0.1151 0.5333 0.073 Uiso 1 1 calc R . . H17B H 0.6885 -0.1819 0.6273 0.073 Uiso 1 1 calc R . . H17C H 0.7286 -0.1803 0.4989 0.073 Uiso 1 1 calc R . . C18 C 0.6261(4) -0.0271(5) 0.7961(4) 0.0540(11) Uani 1 1 d . . . C19 C 0.4233(5) -0.0985(8) 0.7637(6) 0.121(3) Uani 1 1 d . . . H19A H 0.4352 -0.1778 0.7117 0.146 Uiso 1 1 calc R . . H19B H 0.3462 -0.0533 0.7476 0.146 Uiso 1 1 calc R . . H19C H 0.4244 -0.1342 0.8409 0.146 Uiso 1 1 calc R . . C20 C 0.4732(4) 0.3184(7) 0.7940(4) 0.0772(16) Uani 1 1 d . . . C21 C 0.3906(4) 0.3583(9) 0.8900(4) 0.114(3) Uani 1 1 d . . . H21A H 0.4241 0.4398 0.9309 0.137 Uiso 1 1 calc R . . H21B H 0.3830 0.2774 0.9412 0.137 Uiso 1 1 calc R . . H21C H 0.3118 0.3835 0.8595 0.137 Uiso 1 1 calc R . . C22 C 0.7231(4) 0.4892(5) 0.6791(4) 0.0599(12) Uani 1 1 d . . . H22A H 0.6470 0.5228 0.7111 0.072 Uiso 1 1 calc R . . H22B H 0.7812 0.5682 0.6857 0.072 Uiso 1 1 calc R . . C23 C 0.7017(5) 0.4581(5) 0.5517(4) 0.0689(14) Uani 1 1 d . . . H23A H 0.7780 0.4359 0.5163 0.083 Uiso 1 1 calc R . . H23B H 0.6662 0.5419 0.5156 0.083 Uiso 1 1 calc R . . H23C H 0.6475 0.3769 0.5433 0.083 Uiso 1 1 calc R . . C24 C 0.9599(3) 0.3442(5) 1.0199(3) 0.0541(11) Uani 1 1 d . . . H24A H 0.9117 0.4003 1.0731 0.065 Uiso 1 1 calc R . . H24B H 0.9318 0.2445 1.0235 0.065 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 0.0498(17) 0.0532(17) 0.0413(16) 0.0050(13) -0.0124(12) 0.0026(14) O2 0.079(2) 0.083(2) 0.062(2) 0.0363(19) -0.0097(16) -0.0311(19) O3 0.0475(19) 0.108(3) 0.082(2) 0.018(2) -0.0170(17) -0.0213(19) O4 0.0458(16) 0.088(2) 0.0329(14) 0.0015(15) 0.0005(12) 0.0099(16) O5 0.069(2) 0.181(4) 0.059(2) 0.013(3) -0.0051(17) 0.052(3) O6 0.0483(17) 0.067(2) 0.0651(19) -0.0062(16) -0.0243(14) 0.0020(14) O7 0.0630(19) 0.079(2) 0.060(2) -0.0128(17) -0.0273(16) -0.0086(17) N1 0.0491(19) 0.048(2) 0.0386(19) 0.0000(16) 0.0021(15) -0.0169(16) N2 0.0448(17) 0.0356(17) 0.0406(18) -0.0020(16) -0.0095(14) -0.0032(15) C1 0.057(3) 0.051(3) 0.049(3) -0.006(2) 0.011(2) -0.017(2) C2 0.077(3) 0.054(3) 0.042(3) 0.001(2) 0.015(2) -0.009(2) C3 0.070(3) 0.062(3) 0.033(2) 0.001(2) 0.003(2) -0.010(2) C4 0.054(3) 0.059(3) 0.045(2) -0.006(2) -0.004(2) -0.011(2) C5 0.043(2) 0.041(2) 0.036(2) -0.0030(18) -0.0023(17) 0.0023(18) C6 0.041(2) 0.0307(19) 0.040(2) -0.0025(18) -0.0016(17) 0.0002(17) C7 0.038(2) 0.038(2) 0.042(2) -0.0012(18) 0.0002(17) -0.0029(17) C8 0.045(2) 0.041(2) 0.038(2) 0.0057(18) -0.0087(18) 0.0037(17) C9 0.043(2) 0.055(3) 0.033(2) 0.0080(19) -0.0057(17) -0.003(2) C10 0.042(2) 0.065(3) 0.026(2) 0.0067(19) -0.0043(17) 0.010(2) C11 0.051(2) 0.038(2) 0.036(2) -0.0008(18) -0.0068(17) 0.0060(19) C12 0.047(2) 0.040(2) 0.034(2) 0.0024(18) -0.0053(16) -0.0081(18) C13 0.041(2) 0.048(2) 0.050(2) -0.001(2) -0.0044(18) -0.0039(19) C14 0.039(2) 0.044(2) 0.046(2) -0.0014(19) -0.0095(19) -0.0069(19) C15 0.060(3) 0.040(2) 0.047(3) -0.009(2) 0.000(2) -0.004(2) C16 0.057(3) 0.059(3) 0.043(3) -0.011(2) -0.0081(19) 0.012(2) C17 0.071(3) 0.060(3) 0.051(3) -0.002(2) 0.001(2) -0.025(2) C18 0.056(3) 0.073(3) 0.034(2) 0.010(2) 0.001(2) -0.008(2) C19 0.071(4) 0.165(7) 0.128(5) 0.021(5) -0.018(3) -0.055(4) C20 0.053(3) 0.124(5) 0.054(3) 0.001(3) -0.003(2) 0.025(3) C21 0.065(3) 0.208(8) 0.070(3) -0.009(4) 0.017(3) 0.034(4) C22 0.067(3) 0.050(3) 0.063(3) 0.006(2) -0.003(2) 0.014(2) C23 0.090(4) 0.065(3) 0.051(3) 0.027(2) -0.005(2) 0.011(3) C24 0.063(3) 0.062(3) 0.037(2) -0.011(2) -0.0043(19) -0.003(2) _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 1.404(4) . ? O2 C18 1.199(5) . ? O3 C18 1.313(5) . ? O3 C19 1.455(6) . ? O4 C20 1.341(5) . ? O4 C10 1.442(4) . ? O5 C20 1.186(5) . ? O6 C14 1.227(4) . ? O7 C24 1.410(4) . ? N1 C5 1.381(5) . ? N1 C17 1.458(5) . ? N1 C8 1.482(4) . ? N2 C14 1.332(5) . ? N2 C15 1.456(4) . ? N2 C12 1.466(4) . ? C1 C2 1.379(5) . ? C1 C6 1.382(5) . ? C2 C3 1.363(6) . ? C3 C4 1.383(5) . ? C4 C5 1.389(5) . ? C5 C6 1.380(5) . ? C6 C7 1.505(5) . ? C7 C13 1.562(5) . ? C7 C12 1.565(5) . ? C7 C8 1.568(5) . ? C8 C9 1.562(5) . ? C9 C10 1.525(5) . ? C9 C18 1.535(6) . ? C10 C11 1.536(5) . ? C11 C22 1.542(5) . ? C11 C12 1.552(5) . ? C11 C16 1.551(5) . ? C13 C14 1.504(5) . ? C15 C24 1.517(5) . ? C15 C16 1.533(5) . ? C20 C21 1.496(7) . ? C22 C23 1.530(6) . ? 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 C18 O3 C19 116.0(4) . . ? C20 O4 C10 117.7(3) . . ? C5 N1 C17 118.2(3) . . ? C5 N1 C8 108.5(3) . . ? C17 N1 C8 119.0(3) . . ? C14 N2 C15 131.5(3) . . ? C14 N2 C12 114.5(3) . . ? C15 N2 C12 112.9(3) . . ? C2 C1 C6 119.2(4) . . ? C3 C2 C1 120.8(4) . . ? C2 C3 C4 120.8(4) . . ? C3 C4 C5 118.6(4) . . ? C6 C5 N1 112.6(3) . . ? C6 C5 C4 120.5(4) . . ? N1 C5 C4 127.0(4) . . ? C1 C6 C5 120.2(3) . . ? C1 C6 C7 129.9(3) . . ? C5 C6 C7 109.9(3) . . ? C6 C7 C13 113.4(3) . . ? C6 C7 C12 114.3(3) . . ? C13 C7 C12 100.0(3) . . ? C6 C7 C8 102.2(3) . . ? C13 C7 C8 112.2(3) . . ? C12 C7 C8 115.3(3) . . ? N1 C8 C9 112.2(3) . . ? N1 C8 C7 105.4(3) . . ? C9 C8 C7 114.3(3) . . ? O1 C9 C10 109.2(3) . . ? O1 C9 C18 107.9(3) . . ? C10 C9 C18 114.0(3) . . ? O1 C9 C8 108.9(3) . . ? C10 C9 C8 108.2(3) . . ? C18 C9 C8 108.4(3) . . ? O4 C10 C9 108.6(3) . . ? O4 C10 C11 108.6(3) . . ? C9 C10 C11 114.9(3) . . ? C10 C11 C22 109.5(3) . . ? C10 C11 C12 112.0(3) . . ? C22 C11 C12 110.1(3) . . ? C10 C11 C16 111.5(3) . . ? C22 C11 C16 109.5(3) . . ? C12 C11 C16 104.2(3) . . ? N2 C12 C11 105.0(3) . . ? N2 C12 C7 104.5(3) . . ? C11 C12 C7 121.7(3) . . ? C14 C13 C7 106.3(3) . . ? O6 C14 N2 127.4(3) . . ? O6 C14 C13 125.2(4) . . ? N2 C14 C13 107.5(3) . . ? N2 C15 C24 113.9(3) . . ? N2 C15 C16 102.7(3) . . ? C24 C15 C16 111.2(3) . . ? C15 C16 C11 109.1(3) . . ? O2 C18 O3 124.3(4) . . ? O2 C18 C9 121.7(4) . . ? O3 C18 C9 114.0(4) . . ? O5 C20 O4 124.6(4) . . ? O5 C20 C21 124.7(4) . . ? O4 C20 C21 110.6(4) . . ? C23 C22 C11 116.6(4) . . ? O7 C24 C15 115.5(3) . . ? 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 C1 C2 C3 1.2(6) . . . . ? C1 C2 C3 C4 -1.7(7) . . . . ? C2 C3 C4 C5 1.3(6) . . . . ? C17 N1 C5 C6 -148.2(3) . . . . ? C8 N1 C5 C6 -8.8(4) . . . . ? C17 N1 C5 C4 31.3(6) . . . . ? C8 N1 C5 C4 170.7(4) . . . . ? C3 C4 C5 C6 -0.5(6) . . . . ? C3 C4 C5 N1 -180.0(4) . . . . ? C2 C1 C6 C5 -0.4(6) . . . . ? C2 C1 C6 C7 177.6(4) . . . . ? N1 C5 C6 C1 179.6(4) . . . . ? C4 C5 C6 C1 0.1(6) . . . . ? N1 C5 C6 C7 1.2(4) . . . . ? C4 C5 C6 C7 -178.3(3) . . . . ? C1 C6 C7 C13 -50.9(5) . . . . ? C5 C6 C7 C13 127.3(3) . . . . ? C1 C6 C7 C12 62.8(5) . . . . ? C5 C6 C7 C12 -119.0(3) . . . . ? C1 C6 C7 C8 -171.9(4) . . . . ? C5 C6 C7 C8 6.2(4) . . . . ? C5 N1 C8 C9 137.2(3) . . . . ? C17 N1 C8 C9 -83.7(4) . . . . ? C5 N1 C8 C7 12.2(4) . . . . ? C17 N1 C8 C7 151.3(3) . . . . ? C6 C7 C8 N1 -10.9(4) . . . . ? C13 C7 C8 N1 -132.7(3) . . . . ? C12 C7 C8 N1 113.7(3) . . . . ? C6 C7 C8 C9 -134.5(3) . . . . ? C13 C7 C8 C9 103.6(3) . . . . ? C12 C7 C8 C9 -10.0(4) . . . . ? N1 C8 C9 O1 172.8(3) . . . . ? C7 C8 C9 O1 -67.3(4) . . . . ? N1 C8 C9 C10 -68.5(4) . . . . ? C7 C8 C9 C10 51.4(4) . . . . ? N1 C8 C9 C18 55.7(4) . . . . ? C7 C8 C9 C18 175.5(3) . . . . ? C20 O4 C10 C9 -127.6(4) . . . . ? C20 O4 C10 C11 106.8(4) . . . . ? O1 C9 C10 O4 -70.0(4) . . . . ? C18 C9 C10 O4 50.8(4) . . . . ? C8 C9 C10 O4 171.6(3) . . . . ? O1 C9 C10 C11 51.8(4) . . . . ? C18 C9 C10 C11 172.7(3) . . . . ? C8 C9 C10 C11 -66.6(4) . . . . ? O4 C10 C11 C22 -80.6(4) . . . . ? C9 C10 C11 C22 157.6(3) . . . . ? O4 C10 C11 C12 157.0(3) . . . . ? C9 C10 C11 C12 35.2(4) . . . . ? O4 C10 C11 C16 40.7(4) . . . . ? C9 C10 C11 C16 -81.2(4) . . . . ? C14 N2 C12 C11 144.3(3) . . . . ? C15 N2 C12 C11 -24.7(4) . . . . ? C14 N2 C12 C7 15.2(4) . . . . ? C15 N2 C12 C7 -153.7(3) . . . . ? C10 C11 C12 N2 -108.2(3) . . . . ? C22 C11 C12 N2 129.7(3) . . . . ? C16 C11 C12 N2 12.5(4) . . . . ? C10 C11 C12 C7 9.8(4) . . . . ? C22 C11 C12 C7 -112.3(4) . . . . ? C16 C11 C12 C7 130.4(3) . . . . ? C6 C7 C12 N2 -145.7(3) . . . . ? C13 C7 C12 N2 -24.2(3) . . . . ? C8 C7 C12 N2 96.3(3) . . . . ? C6 C7 C12 C11 96.1(4) . . . . ? C13 C7 C12 C11 -142.5(3) . . . . ? C8 C7 C12 C11 -21.9(4) . . . . ? C6 C7 C13 C14 148.0(3) . . . . ? C12 C7 C13 C14 26.0(4) . . . . ? C8 C7 C13 C14 -96.7(4) . . . . ? C15 N2 C14 O6 -11.7(7) . . . . ? C12 N2 C14 O6 -178.1(4) . . . . ? C15 N2 C14 C13 168.4(4) . . . . ? C12 N2 C14 C13 2.1(4) . . . . ? C7 C13 C14 O6 161.5(4) . . . . ? C7 C13 C14 N2 -18.7(4) . . . . ? C14 N2 C15 C24 -20.7(6) . . . . ? C12 N2 C15 C24 145.8(3) . . . . ? C14 N2 C15 C16 -141.1(4) . . . . ? C12 N2 C15 C16 25.4(4) . . . . ? N2 C15 C16 C11 -15.9(4) . . . . ? C24 C15 C16 C11 -138.1(4) . . . . ? C10 C11 C16 C15 123.2(4) . . . . ? C22 C11 C16 C15 -115.5(4) . . . . ? C12 C11 C16 C15 2.2(4) . . . . ? C19 O3 C18 O2 3.4(7) . . . . ? C19 O3 C18 C9 -178.7(4) . . . . ? O1 C9 C18 O2 -41.1(5) . . . . ? C10 C9 C18 O2 -162.7(4) . . . . ? C8 C9 C18 O2 76.7(5) . . . . ? O1 C9 C18 O3 140.8(4) . . . . ? C10 C9 C18 O3 19.3(5) . . . . ? C8 C9 C18 O3 -101.4(4) . . . . ? C10 O4 C20 O5 0.1(9) . . . . ? C10 O4 C20 C21 -177.2(5) . . . . ? C10 C11 C22 C23 -63.0(5) . . . . ? C12 C11 C22 C23 60.5(5) . . . . ? C16 C11 C22 C23 174.5(4) . . . . ? N2 C15 C24 O7 74.2(5) . . . . ? C16 C15 C24 O7 -170.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O7 0.82 1.94 2.749(4) 171.0 2_747 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.156 _refine_diff_density_min -0.156 _refine_diff_density_rms 0.037