data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H24 N3 O7 V' _chemical_formula_weight 553.43 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' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.4721(13) _cell_length_b 7.0490(6) _cell_length_c 26.159(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.395(2) _cell_angle_gamma 90.00 _cell_volume 2606.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9806 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 25.6 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8961 _exptl_absorpt_correction_T_max 0.9264 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24271 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4847 _reflns_number_gt 3702 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0629P)^2^+3.6694P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4847 _refine_ls_number_parameters 349 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1753 _refine_ls_wR_factor_gt 0.1622 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.001 _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 H3 H 0.353(3) 0.603(3) 1.0716(17) 0.080 Uiso 1 1 d D . . V1 V 0.17150(4) 0.24282(10) 1.04612(3) 0.0545(2) Uani 1 1 d . . . N1 N 0.13274(19) -0.0358(4) 1.02318(12) 0.0493(7) Uani 1 1 d . . . N2 N 0.1222(2) -0.0719(5) 0.97016(12) 0.0513(8) Uani 1 1 d . . . N3 N 0.32793(19) 0.4880(4) 1.06280(13) 0.0498(8) Uani 1 1 d D . . O1 O 0.1990(2) 0.1389(5) 1.11216(12) 0.0713(8) Uani 1 1 d . . . O2 O 0.16995(18) 0.2377(4) 0.97246(11) 0.0576(7) Uani 1 1 d . . . O3 O 0.0788(2) -0.2506(4) 0.87976(12) 0.0745(9) Uani 1 1 d . . . H3A H 0.0882 -0.2388 0.9116 0.112 Uiso 1 1 calc R . . O4 O 0.32630(16) 0.1801(4) 1.04966(10) 0.0533(7) Uani 1 1 d . . . O5 O 0.23290(16) 0.4754(4) 1.05873(11) 0.0552(7) Uani 1 1 d . . . O6 O 0.06854(19) 0.3241(5) 1.04324(13) 0.0739(9) Uani 1 1 d . . . O7 O 0.3804(2) 0.8383(4) 0.10023(13) 0.0712(8) Uani 1 1 d . . . H7 H 0.3610 0.9355 0.0842 0.107 Uiso 1 1 calc R . . C1 C 0.1175(2) -0.1584(6) 1.10654(16) 0.0568(10) Uani 1 1 d . . . C2 C 0.1603(3) -0.0015(7) 1.13535(17) 0.0624(11) Uani 1 1 d . . . C3 C 0.1681(3) 0.0043(8) 1.18941(19) 0.0786(14) Uani 1 1 d . . . H3B H 0.1955 0.1085 1.2087 0.094 Uiso 1 1 calc R . . C4 C 0.1345(4) -0.1474(9) 1.2142(2) 0.0879(15) Uani 1 1 d . . . H4 H 0.1399 -0.1431 1.2502 0.106 Uiso 1 1 calc R . . C5 C 0.0932(4) -0.3049(8) 1.1866(2) 0.0838(15) Uani 1 1 d . . . H5 H 0.0715 -0.4056 1.2038 0.101 Uiso 1 1 calc R . . C6 C 0.0850(3) -0.3087(7) 1.1331(2) 0.0707(12) Uani 1 1 d . . . H6 H 0.0573 -0.4134 1.1142 0.085 Uiso 1 1 calc R . . C7 C 0.1100(2) -0.1700(6) 1.05134(16) 0.0537(10) Uani 1 1 d . . . H7A H 0.0871 -0.2822 1.0346 0.064 Uiso 1 1 calc R . . C8 C 0.1416(2) 0.0797(5) 0.94666(15) 0.0480(9) Uani 1 1 d . . . C9 C 0.1329(2) 0.0776(6) 0.88962(15) 0.0500(9) Uani 1 1 d . . . C10 C 0.1017(3) -0.0870(6) 0.85828(17) 0.0567(10) Uani 1 1 d . . . C11 C 0.0944(3) -0.0776(7) 0.80536(17) 0.0671(12) Uani 1 1 d . . . H11 H 0.0747 -0.1849 0.7853 0.080 Uiso 1 1 calc R . . C12 C 0.1154(3) 0.0856(7) 0.78032(17) 0.0633(11) Uani 1 1 d . . . C13 C 0.1077(3) 0.0985(9) 0.72559(19) 0.0814(14) Uani 1 1 d . . . H13 H 0.0881 -0.0069 0.7047 0.098 Uiso 1 1 calc R . . C14 C 0.1285(4) 0.2609(10) 0.7032(2) 0.0908(17) Uani 1 1 d . . . H14 H 0.1224 0.2653 0.6671 0.109 Uiso 1 1 calc R . . C15 C 0.1587(3) 0.4223(9) 0.7328(2) 0.0877(16) Uani 1 1 d . . . H15 H 0.1732 0.5327 0.7167 0.105 Uiso 1 1 calc R . . C16 C 0.1669(3) 0.4166(8) 0.78537(19) 0.0740(13) Uani 1 1 d . . . H16 H 0.1866 0.5245 0.8052 0.089 Uiso 1 1 calc R . . C17 C 0.1459(3) 0.2506(6) 0.81057(17) 0.0591(10) Uani 1 1 d . . . C18 C 0.1530(2) 0.2394(6) 0.86495(16) 0.0541(10) Uani 1 1 d . . . H18 H 0.1721 0.3467 0.8851 0.065 Uiso 1 1 calc R . . C19 C 0.4774(2) 0.3377(5) 1.06050(13) 0.0455(8) Uani 1 1 d . . . C20 C 0.5285(3) 0.5053(6) 1.06991(16) 0.0589(10) Uani 1 1 d . . . H20 H 0.4987 0.6172 1.0761 0.071 Uiso 1 1 calc R . . C21 C 0.6243(3) 0.5049(7) 1.07002(18) 0.0708(12) Uani 1 1 d . . . H21 H 0.6586 0.6173 1.0764 0.085 Uiso 1 1 calc R . . C22 C 0.6689(3) 0.3426(8) 1.06099(18) 0.0727(13) Uani 1 1 d . . . H22 H 0.7332 0.3443 1.0611 0.087 Uiso 1 1 calc R . . C23 C 0.6193(3) 0.1771(7) 1.05181(18) 0.0715(12) Uani 1 1 d . . . H23 H 0.6499 0.0663 1.0455 0.086 Uiso 1 1 calc R . . C24 C 0.5229(3) 0.1729(6) 1.05178(16) 0.0577(10) Uani 1 1 d . . . H24 H 0.4895 0.0595 1.0459 0.069 Uiso 1 1 calc R . . C25 C 0.3740(2) 0.3291(5) 1.05792(13) 0.0429(8) Uani 1 1 d . . . C26 C 0.3880(6) 0.7356(16) 0.1840(3) 0.179(4) Uani 1 1 d . . . H26A H 0.3219 0.7064 0.1735 0.269 Uiso 1 1 calc R . . H26B H 0.4023 0.7734 0.2201 0.269 Uiso 1 1 calc R . . H26C H 0.4246 0.6255 0.1796 0.269 Uiso 1 1 calc R . . C27 C 0.4097(5) 0.8796(12) 0.1540(3) 0.129(2) Uani 1 1 d . . . H27A H 0.4775 0.9008 0.1624 0.154 Uiso 1 1 calc R . . H27B H 0.3790 0.9951 0.1618 0.154 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 V1 0.0388(3) 0.0543(4) 0.0701(5) -0.0197(3) 0.0109(3) -0.0105(3) N1 0.0327(14) 0.0499(18) 0.064(2) -0.0037(16) 0.0076(13) -0.0059(13) N2 0.0387(16) 0.0523(19) 0.061(2) -0.0124(16) 0.0075(14) -0.0062(14) N3 0.0346(15) 0.0430(17) 0.071(2) -0.0090(15) 0.0093(14) -0.0073(13) O1 0.0626(17) 0.078(2) 0.0730(19) -0.0205(16) 0.0144(14) -0.0221(16) O2 0.0484(14) 0.0516(15) 0.0706(17) -0.0087(13) 0.0080(12) -0.0136(12) O3 0.091(2) 0.0551(18) 0.075(2) -0.0174(16) 0.0129(18) -0.0149(16) O4 0.0392(13) 0.0452(14) 0.0756(18) -0.0135(13) 0.0122(12) -0.0062(11) O5 0.0341(12) 0.0496(15) 0.0798(18) -0.0185(13) 0.0073(12) -0.0036(11) O6 0.0435(15) 0.075(2) 0.103(2) -0.0311(18) 0.0153(15) -0.0089(14) O7 0.082(2) 0.0472(16) 0.081(2) -0.0083(15) 0.0101(17) -0.0079(16) C1 0.0342(18) 0.067(3) 0.071(3) 0.000(2) 0.0153(17) 0.0017(18) C2 0.044(2) 0.077(3) 0.068(3) -0.005(2) 0.0168(19) 0.000(2) C3 0.068(3) 0.096(4) 0.074(3) -0.013(3) 0.020(2) -0.005(3) C4 0.084(3) 0.108(4) 0.078(3) -0.001(3) 0.031(3) 0.013(3) C5 0.075(3) 0.085(4) 0.098(4) 0.015(3) 0.033(3) 0.011(3) C6 0.057(3) 0.067(3) 0.090(3) 0.001(2) 0.021(2) 0.006(2) C7 0.0302(17) 0.054(2) 0.074(3) -0.011(2) 0.0051(17) -0.0004(16) C8 0.0262(16) 0.044(2) 0.072(2) -0.0102(18) 0.0058(15) -0.0042(15) C9 0.0278(16) 0.057(2) 0.064(2) -0.0122(19) 0.0064(15) -0.0012(16) C10 0.042(2) 0.052(2) 0.074(3) -0.013(2) 0.0086(18) -0.0019(17) C11 0.058(2) 0.068(3) 0.069(3) -0.024(2) 0.002(2) 0.004(2) C12 0.041(2) 0.080(3) 0.068(3) -0.010(2) 0.0098(18) 0.007(2) C13 0.072(3) 0.104(4) 0.065(3) -0.012(3) 0.008(2) 0.006(3) C14 0.078(3) 0.130(5) 0.065(3) 0.001(4) 0.016(3) 0.009(3) C15 0.069(3) 0.114(5) 0.080(4) 0.018(3) 0.017(3) -0.005(3) C16 0.055(2) 0.083(3) 0.083(3) 0.000(3) 0.013(2) -0.007(2) C17 0.0364(19) 0.074(3) 0.067(3) -0.003(2) 0.0102(17) 0.0030(19) C18 0.0351(18) 0.054(2) 0.072(3) -0.014(2) 0.0079(17) -0.0050(17) C19 0.0356(17) 0.056(2) 0.0433(19) 0.0000(17) 0.0056(14) -0.0040(16) C20 0.042(2) 0.058(2) 0.075(3) -0.001(2) 0.0073(18) -0.0036(18) C21 0.038(2) 0.078(3) 0.092(3) 0.005(3) 0.007(2) -0.013(2) C22 0.034(2) 0.104(4) 0.080(3) 0.005(3) 0.0126(19) -0.004(2) C23 0.051(2) 0.083(3) 0.083(3) -0.015(3) 0.021(2) 0.009(2) C24 0.045(2) 0.061(2) 0.067(3) -0.012(2) 0.0139(18) -0.0013(19) C25 0.0357(17) 0.0439(19) 0.048(2) -0.0040(16) 0.0072(14) -0.0048(15) C26 0.153(8) 0.252(13) 0.133(7) 0.043(8) 0.033(6) 0.069(8) C27 0.123(6) 0.126(6) 0.127(6) 0.020(5) 0.004(5) 0.013(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 V1 O6 1.583(3) . ? V1 O1 1.840(3) . ? V1 O5 1.860(3) . ? V1 O2 1.922(3) . ? V1 N1 2.095(3) . ? V1 O4 2.266(2) . ? N1 C7 1.284(5) . ? N1 N2 1.386(4) . ? N2 C8 1.293(5) . ? N3 C25 1.324(5) . ? N3 O5 1.359(4) . ? N3 H3 0.898(10) . ? O1 C2 1.344(5) . ? O2 C8 1.321(4) . ? O3 C10 1.355(5) . ? O3 H3A 0.8200 . ? O4 C25 1.250(4) . ? O7 C27 1.409(8) . ? O7 H7 0.8200 . ? C1 C6 1.402(6) . ? C1 C2 1.406(6) . ? C1 C7 1.427(6) . ? C2 C3 1.395(6) . ? C3 C4 1.391(7) . ? C3 H3B 0.9300 . ? C4 C5 1.388(8) . ? C4 H4 0.9300 . ? C5 C6 1.379(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.470(5) . ? C9 C18 1.372(6) . ? C9 C10 1.436(5) . ? C10 C11 1.367(6) . ? C11 C12 1.389(6) . ? C11 H11 0.9300 . ? C12 C13 1.415(6) . ? C12 C17 1.423(6) . ? C13 C14 1.349(8) . ? C13 H13 0.9300 . ? C14 C15 1.393(8) . ? C14 H14 0.9300 . ? C15 C16 1.355(6) . ? C15 H15 0.9300 . ? C16 C17 1.408(6) . ? C16 H16 0.9300 . ? C17 C18 1.406(6) . ? C18 H18 0.9300 . ? C19 C24 1.378(5) . ? C19 C20 1.388(5) . ? C19 C25 1.484(5) . ? C20 C21 1.386(5) . ? C20 H20 0.9300 . ? C21 C22 1.359(7) . ? C21 H21 0.9300 . ? C22 C23 1.363(7) . ? C22 H22 0.9300 . ? C23 C24 1.396(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C26 C27 1.361(10) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? 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 O6 V1 O1 101.54(16) . . ? O6 V1 O5 95.64(14) . . ? O1 V1 O5 100.71(13) . . ? O6 V1 O2 98.67(15) . . ? O1 V1 O2 152.55(13) . . ? O5 V1 O2 95.55(12) . . ? O6 V1 N1 97.72(14) . . ? O1 V1 N1 83.46(13) . . ? O5 V1 N1 164.91(11) . . ? O2 V1 N1 75.55(12) . . ? O6 V1 O4 170.02(14) . . ? O1 V1 O4 82.62(12) . . ? O5 V1 O4 74.59(10) . . ? O2 V1 O4 80.57(10) . . ? N1 V1 O4 91.74(10) . . ? C7 N1 N2 116.9(3) . . ? C7 N1 V1 127.7(3) . . ? N2 N1 V1 115.1(2) . . ? C8 N2 N1 109.6(3) . . ? C25 N3 O5 117.3(3) . . ? C25 N3 H3 127(3) . . ? O5 N3 H3 115(3) . . ? C2 O1 V1 133.7(3) . . ? C8 O2 V1 117.6(2) . . ? C10 O3 H3A 109.5 . . ? C25 O4 V1 110.3(2) . . ? N3 O5 V1 120.5(2) . . ? C27 O7 H7 109.5 . . ? C6 C1 C2 119.0(4) . . ? C6 C1 C7 119.8(4) . . ? C2 C1 C7 121.1(4) . . ? O1 C2 C3 119.0(4) . . ? O1 C2 C1 121.0(4) . . ? C3 C2 C1 119.8(4) . . ? C4 C3 C2 119.3(5) . . ? C4 C3 H3B 120.3 . . ? C2 C3 H3B 120.3 . . ? C5 C4 C3 121.8(5) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C6 C5 C4 118.5(5) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 C1 121.6(5) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? N1 C7 C1 124.4(4) . . ? N1 C7 H7A 117.8 . . ? C1 C7 H7A 117.8 . . ? N2 C8 O2 121.9(3) . . ? N2 C8 C9 119.6(3) . . ? O2 C8 C9 118.5(3) . . ? C18 C9 C10 118.4(4) . . ? C18 C9 C8 119.2(3) . . ? C10 C9 C8 122.4(4) . . ? O3 C10 C11 119.2(4) . . ? O3 C10 C9 121.7(4) . . ? C11 C10 C9 119.0(4) . . ? C10 C11 C12 122.7(4) . . ? C10 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C11 C12 C13 123.6(5) . . ? C11 C12 C17 119.2(4) . . ? C13 C12 C17 117.2(5) . . ? C14 C13 C12 121.2(5) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 121.5(5) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C16 C15 C14 119.3(5) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 121.3(5) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 122.9(4) . . ? C18 C17 C12 117.6(4) . . ? C16 C17 C12 119.4(4) . . ? C9 C18 C17 123.1(4) . . ? C9 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? C24 C19 C20 119.4(3) . . ? C24 C19 C25 118.1(3) . . ? C20 C19 C25 122.5(3) . . ? C21 C20 C19 119.6(4) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C20 120.9(4) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 120.0(4) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 120.4(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 119.7(4) . . ? C19 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? O4 C25 N3 117.2(3) . . ? O4 C25 C19 123.8(3) . . ? N3 C25 C19 119.0(3) . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C26 C27 O7 111.4(7) . . ? C26 C27 H27A 109.3 . . ? O7 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? O7 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? 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 O3 H3A N2 0.82 1.91 2.634(4) 146.7 . O7 H7 O4 0.82 1.96 2.779(4) 174.3 1_564 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.700 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.057