data_sa984 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H25 N3 O7' _chemical_formula_sum 'C22 H25 N3 O7' _chemical_formula_weight 443.45 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)/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 6.9086(18) _cell_length_b 12.855(3) _cell_length_c 24.098(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.903(3) _cell_angle_gamma 90.00 _cell_volume 2137.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6553 _cell_measurement_theta_min 1.58 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9499 _exptl_absorpt_correction_T_max 0.9805 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17035 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 27.53 _reflns_number_total 4871 _reflns_number_gt 4575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.0494P)^2^+1.6245P] 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_number_reflns 4871 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1503 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _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 -0.0751(2) 0.70823(13) 0.27921(7) 0.0394(4) Uani 1 1 d . . . O2 O 0.2724(2) 0.57184(13) 0.51330(7) 0.0438(4) Uani 1 1 d . . . O3 O 0.2389(2) 0.74204(13) 0.53036(6) 0.0386(4) Uani 1 1 d . . . O4 O 0.8676(4) 0.96219(18) 0.56229(10) 0.0825(8) Uani 1 1 d . . . O5 O 0.8413(3) 0.81227(18) 0.60127(7) 0.0591(5) Uani 1 1 d . . . O6 O 0.3288(3) 0.43701(15) 0.31455(10) 0.0677(6) Uani 1 1 d . . . O7 O 0.6231(3) 0.50544(14) 0.32021(8) 0.0552(5) Uani 1 1 d . . . N1 N 0.2031(2) 0.77104(13) 0.32202(7) 0.0271(4) Uani 1 1 d . . . N2 N 0.4090(2) 0.77100(13) 0.31769(7) 0.0266(4) Uani 1 1 d . . . N3 N 0.8226(3) 0.87001(19) 0.56097(8) 0.0470(5) Uani 1 1 d . . . C1 C 0.4257(3) 0.74418(19) 0.25775(8) 0.0338(5) Uani 1 1 d . . . H1A H 0.5442 0.7027 0.2526 0.041 Uiso 1 1 calc R . . H1B H 0.4317 0.8082 0.2350 0.041 Uiso 1 1 calc R . . C2 C 0.2449(3) 0.68097(19) 0.24076(9) 0.0350(5) Uani 1 1 d . . . H2A H 0.1995 0.6961 0.2020 0.042 Uiso 1 1 calc R . . H2B H 0.2690 0.6054 0.2448 0.042 Uiso 1 1 calc R . . C3 C 0.1017(3) 0.71879(16) 0.28155(8) 0.0301(4) Uani 1 1 d . . . C4 C 0.1176(3) 0.82828(17) 0.36598(8) 0.0316(4) Uani 1 1 d . . . H4A H -0.0237 0.8334 0.3574 0.038 Uiso 1 1 calc R . . H4B H 0.1705 0.8999 0.3663 0.038 Uiso 1 1 calc R . . C5 C 0.1496(3) 0.78295(16) 0.42293(8) 0.0284(4) Uani 1 1 d . . . H5A H 0.1294 0.8288 0.4530 0.034 Uiso 1 1 calc R . . C6 C 0.2028(3) 0.68640(16) 0.43674(8) 0.0279(4) Uani 1 1 d . . . C7 C 0.2363(3) 0.59739(15) 0.39795(8) 0.0283(4) Uani 1 1 d . . . C8 C 0.3887(3) 0.59737(15) 0.36516(8) 0.0256(4) Uani 1 1 d . . . C9 C 0.5107(3) 0.69393(15) 0.35648(8) 0.0244(4) Uani 1 1 d . . . H9A H 0.6264 0.6695 0.3368 0.029 Uiso 1 1 calc R . . C10 C 0.2390(3) 0.65896(17) 0.49680(9) 0.0318(4) Uani 1 1 d . . . C11 C 0.2913(4) 0.7222(2) 0.58877(9) 0.0464(6) Uani 1 1 d . . . H11A H 0.4116 0.6803 0.5923 0.056 Uiso 1 1 calc R . . H11B H 0.1865 0.6832 0.6061 0.056 Uiso 1 1 calc R . . C12 C 0.3212(4) 0.8249(2) 0.61681(10) 0.0496(6) Uani 1 1 d . . . H12A H 0.3534 0.8139 0.6565 0.074 Uiso 1 1 calc R . . H12B H 0.2023 0.8662 0.6123 0.074 Uiso 1 1 calc R . . H12C H 0.4277 0.8619 0.6001 0.074 Uiso 1 1 calc R . . C13 C 0.0867(3) 0.51256(19) 0.40063(11) 0.0413(5) Uani 1 1 d . . . H13A H 0.1429 0.4464 0.3892 0.062 Uiso 1 1 calc R . . H13B H -0.0252 0.5296 0.3757 0.062 Uiso 1 1 calc R . . H13C H 0.0450 0.5064 0.4388 0.062 Uiso 1 1 calc R . . C14 C 0.5906(3) 0.74409(15) 0.41011(8) 0.0245(4) Uani 1 1 d . . . C15 C 0.6087(3) 0.85146(15) 0.41641(8) 0.0283(4) Uani 1 1 d . . . H15A H 0.5671 0.8962 0.3868 0.034 Uiso 1 1 calc R . . C16 C 0.6870(3) 0.89363(17) 0.46569(9) 0.0335(5) Uani 1 1 d . . . H16A H 0.7003 0.9668 0.4701 0.040 Uiso 1 1 calc R . . C17 C 0.7450(3) 0.82686(18) 0.50807(8) 0.0333(5) Uani 1 1 d . . . C18 C 0.7335(3) 0.71997(17) 0.50267(9) 0.0322(4) Uani 1 1 d . . . H18A H 0.7763 0.6756 0.5323 0.039 Uiso 1 1 calc R . . C19 C 0.6586(3) 0.67927(16) 0.45321(8) 0.0286(4) Uani 1 1 d . . . H19A H 0.6531 0.6060 0.4484 0.034 Uiso 1 1 calc R . . C20 C 0.4363(3) 0.50440(16) 0.33101(9) 0.0317(4) Uani 1 1 d . . . C21 C 0.6957(6) 0.4265(2) 0.28328(14) 0.0729(10) Uani 1 1 d . . . H21A H 0.8141 0.3945 0.3007 0.088 Uiso 1 1 calc R . . H21B H 0.5971 0.3712 0.2773 0.088 Uiso 1 1 calc R . . C22 C 0.7394(5) 0.4714(2) 0.23061(12) 0.0644(8) Uani 1 1 d . . . H22A H 0.7995 0.4186 0.2077 0.097 Uiso 1 1 calc R . . H22B H 0.8290 0.5299 0.2367 0.097 Uiso 1 1 calc R . . H22C H 0.6195 0.4962 0.2115 0.097 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 0.0230(7) 0.0483(10) 0.0467(9) 0.0038(7) -0.0019(6) -0.0040(6) O2 0.0486(10) 0.0395(9) 0.0440(9) 0.0157(7) 0.0084(7) 0.0045(7) O3 0.0426(9) 0.0452(9) 0.0277(7) 0.0030(7) 0.0002(6) 0.0076(7) O4 0.121(2) 0.0554(13) 0.0666(14) -0.0266(11) -0.0371(14) 0.0045(13) O5 0.0483(10) 0.0990(16) 0.0295(9) -0.0003(10) -0.0011(7) -0.0052(10) O6 0.0509(11) 0.0455(11) 0.1067(18) -0.0369(11) 0.0027(11) -0.0131(9) O7 0.0528(11) 0.0396(9) 0.0765(13) -0.0254(9) 0.0343(9) -0.0055(8) N1 0.0216(8) 0.0312(9) 0.0288(8) 0.0018(7) 0.0029(6) 0.0027(6) N2 0.0213(8) 0.0304(9) 0.0282(8) 0.0034(7) 0.0040(6) -0.0014(6) N3 0.0395(11) 0.0649(15) 0.0362(11) -0.0148(10) -0.0029(8) 0.0048(10) C1 0.0285(10) 0.0468(13) 0.0267(10) 0.0033(9) 0.0060(8) -0.0009(9) C2 0.0319(10) 0.0448(13) 0.0282(10) -0.0031(9) 0.0005(8) 0.0009(9) C3 0.0283(10) 0.0320(11) 0.0298(10) 0.0053(8) -0.0009(8) -0.0009(8) C4 0.0337(10) 0.0311(11) 0.0304(10) 0.0020(8) 0.0050(8) 0.0085(8) C5 0.0244(9) 0.0324(10) 0.0291(10) 0.0015(8) 0.0064(7) 0.0032(8) C6 0.0195(9) 0.0331(10) 0.0318(10) 0.0054(8) 0.0075(7) -0.0010(7) C7 0.0246(9) 0.0264(10) 0.0336(10) 0.0049(8) 0.0005(7) -0.0017(7) C8 0.0240(9) 0.0233(9) 0.0292(9) 0.0004(7) -0.0010(7) -0.0016(7) C9 0.0204(8) 0.0249(9) 0.0282(9) -0.0011(7) 0.0039(7) -0.0001(7) C10 0.0241(9) 0.0375(12) 0.0346(11) 0.0084(9) 0.0088(8) 0.0026(8) C11 0.0488(14) 0.0606(16) 0.0295(11) 0.0088(11) -0.0018(10) 0.0059(12) C12 0.0424(13) 0.0703(18) 0.0354(12) -0.0036(12) -0.0039(10) 0.0044(12) C13 0.0327(11) 0.0389(13) 0.0526(14) 0.0068(11) 0.0046(10) -0.0104(9) C14 0.0189(8) 0.0274(10) 0.0275(9) -0.0004(7) 0.0051(7) -0.0018(7) C15 0.0267(9) 0.0273(10) 0.0310(10) 0.0017(8) 0.0029(7) -0.0011(8) C16 0.0327(10) 0.0306(11) 0.0372(11) -0.0062(9) 0.0024(8) -0.0017(8) C17 0.0254(9) 0.0461(13) 0.0286(10) -0.0072(9) 0.0024(8) -0.0007(9) C18 0.0242(9) 0.0401(12) 0.0324(10) 0.0067(9) 0.0009(8) 0.0013(8) C19 0.0227(9) 0.0278(10) 0.0355(10) 0.0026(8) 0.0013(7) 0.0004(7) C20 0.0358(11) 0.0265(10) 0.0327(10) -0.0012(8) -0.0002(8) -0.0005(8) C21 0.105(3) 0.0382(15) 0.081(2) -0.0197(14) 0.055(2) 0.0038(15) C22 0.101(2) 0.0476(16) 0.0463(15) -0.0122(13) 0.0179(15) 0.0023(16) _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 C3 1.227(2) . ? O2 C10 1.207(3) . ? O3 C10 1.340(3) . ? O3 C11 1.458(3) . ? O4 N3 1.225(3) . ? O5 N3 1.224(3) . ? O6 C20 1.195(3) . ? O7 C20 1.330(3) . ? O7 C21 1.455(3) . ? N1 C3 1.350(3) . ? N1 N2 1.431(2) . ? N1 C4 1.441(3) . ? N2 C1 1.495(3) . ? N2 C9 1.511(2) . ? N3 C17 1.467(3) . ? C1 C2 1.528(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.510(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C4 C5 1.497(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.332(3) . ? C5 H5A 0.9500 . ? C6 C10 1.498(3) . ? C6 C7 1.503(3) . ? C7 C8 1.348(3) . ? C7 C13 1.506(3) . ? C8 C20 1.497(3) . ? C8 C9 1.521(3) . ? C9 C14 1.523(3) . ? C9 H9A 1.0000 . ? C11 C12 1.493(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.393(3) . ? C14 C19 1.394(3) . ? C15 C16 1.390(3) . ? C15 H15A 0.9500 . ? C16 C17 1.378(3) . ? C16 H16A 0.9500 . ? C17 C18 1.382(3) . ? C18 C19 1.378(3) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C21 C22 1.440(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 C10 O3 C11 115.82(18) . . ? C20 O7 C21 118.7(2) . . ? C3 N1 N2 115.36(16) . . ? C3 N1 C4 124.60(17) . . ? N2 N1 C4 119.98(16) . . ? N1 N2 C1 101.30(14) . . ? N1 N2 C9 112.82(14) . . ? C1 N2 C9 112.97(16) . . ? O5 N3 O4 123.3(2) . . ? O5 N3 C17 118.7(2) . . ? O4 N3 C17 118.0(2) . . ? N2 C1 C2 106.23(16) . . ? N2 C1 H1A 110.5 . . ? C2 C1 H1A 110.5 . . ? N2 C1 H1B 110.5 . . ? C2 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? C3 C2 C1 101.99(17) . . ? C3 C2 H2A 111.4 . . ? C1 C2 H2A 111.4 . . ? C3 C2 H2B 111.4 . . ? C1 C2 H2B 111.4 . . ? H2A C2 H2B 109.2 . . ? O1 C3 N1 124.5(2) . . ? O1 C3 C2 128.15(19) . . ? N1 C3 C2 107.30(17) . . ? N1 C4 C5 115.35(17) . . ? N1 C4 H4A 108.4 . . ? C5 C4 H4A 108.4 . . ? N1 C4 H4B 108.4 . . ? C5 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? C6 C5 C4 128.16(19) . . ? C6 C5 H5A 115.9 . . ? C4 C5 H5A 115.9 . . ? C5 C6 C10 119.42(19) . . ? C5 C6 C7 127.11(19) . . ? C10 C6 C7 113.46(17) . . ? C8 C7 C6 120.97(17) . . ? C8 C7 C13 125.7(2) . . ? C6 C7 C13 113.37(18) . . ? C7 C8 C20 121.47(18) . . ? C7 C8 C9 122.35(17) . . ? C20 C8 C9 115.95(16) . . ? N2 C9 C8 112.14(15) . . ? N2 C9 C14 112.62(15) . . ? C8 C9 C14 114.12(16) . . ? N2 C9 H9A 105.7 . . ? C8 C9 H9A 105.7 . . ? C14 C9 H9A 105.7 . . ? O2 C10 O3 123.2(2) . . ? O2 C10 C6 123.8(2) . . ? O3 C10 C6 112.97(18) . . ? O3 C11 C12 107.7(2) . . ? O3 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? O3 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 C13 H13A 109.5 . . ? C7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 119.06(18) . . ? C15 C14 C9 122.59(17) . . ? C19 C14 C9 118.24(17) . . ? C16 C15 C14 120.55(19) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C17 C16 C15 118.4(2) . . ? C17 C16 H16A 120.8 . . ? C15 C16 H16A 120.8 . . ? C16 C17 C18 122.44(19) . . ? C16 C17 N3 119.2(2) . . ? C18 C17 N3 118.3(2) . . ? C19 C18 C17 118.42(19) . . ? C19 C18 H18A 120.8 . . ? C17 C18 H18A 120.8 . . ? C18 C19 C14 120.99(19) . . ? C18 C19 H19A 119.5 . . ? C14 C19 H19A 119.5 . . ? O6 C20 O7 122.3(2) . . ? O6 C20 C8 127.7(2) . . ? O7 C20 C8 109.98(17) . . ? C22 C21 O7 110.7(2) . . ? C22 C21 H21A 109.5 . . ? O7 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? O7 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? 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 C3 N1 N2 C1 19.8(2) . . . . ? C4 N1 N2 C1 -157.48(17) . . . . ? C3 N1 N2 C9 -101.25(19) . . . . ? C4 N1 N2 C9 81.5(2) . . . . ? N1 N2 C1 C2 -27.3(2) . . . . ? C9 N2 C1 C2 93.63(19) . . . . ? N2 C1 C2 C3 25.7(2) . . . . ? N2 N1 C3 O1 178.09(19) . . . . ? C4 N1 C3 O1 -4.8(3) . . . . ? N2 N1 C3 C2 -3.7(2) . . . . ? C4 N1 C3 C2 173.49(18) . . . . ? C1 C2 C3 O1 164.3(2) . . . . ? C1 C2 C3 N1 -13.9(2) . . . . ? C3 N1 C4 C5 111.5(2) . . . . ? N2 N1 C4 C5 -71.5(2) . . . . ? N1 C4 C5 C6 -18.2(3) . . . . ? C4 C5 C6 C10 176.11(19) . . . . ? C4 C5 C6 C7 -2.6(3) . . . . ? C5 C6 C7 C8 69.2(3) . . . . ? C10 C6 C7 C8 -109.6(2) . . . . ? C5 C6 C7 C13 -111.2(2) . . . . ? C10 C6 C7 C13 70.0(2) . . . . ? C6 C7 C8 C20 173.20(17) . . . . ? C13 C7 C8 C20 -6.4(3) . . . . ? C6 C7 C8 C9 -12.5(3) . . . . ? C13 C7 C8 C9 167.93(19) . . . . ? N1 N2 C9 C8 33.1(2) . . . . ? C1 N2 C9 C8 -81.09(19) . . . . ? N1 N2 C9 C14 -97.29(18) . . . . ? C1 N2 C9 C14 148.56(16) . . . . ? C7 C8 C9 N2 -75.8(2) . . . . ? C20 C8 C9 N2 98.76(19) . . . . ? C7 C8 C9 C14 53.7(2) . . . . ? C20 C8 C9 C14 -131.67(18) . . . . ? C11 O3 C10 O2 2.8(3) . . . . ? C11 O3 C10 C6 -174.46(18) . . . . ? C5 C6 C10 O2 173.9(2) . . . . ? C7 C6 C10 O2 -7.2(3) . . . . ? C5 C6 C10 O3 -8.9(3) . . . . ? C7 C6 C10 O3 170.02(16) . . . . ? C10 O3 C11 C12 168.94(19) . . . . ? N2 C9 C14 C15 -14.5(2) . . . . ? C8 C9 C14 C15 -143.80(18) . . . . ? N2 C9 C14 C19 169.38(16) . . . . ? C8 C9 C14 C19 40.0(2) . . . . ? C19 C14 C15 C16 -2.3(3) . . . . ? C9 C14 C15 C16 -178.38(17) . . . . ? C14 C15 C16 C17 -0.4(3) . . . . ? C15 C16 C17 C18 2.1(3) . . . . ? C15 C16 C17 N3 -178.19(19) . . . . ? O5 N3 C17 C16 167.2(2) . . . . ? O4 N3 C17 C16 -13.7(3) . . . . ? O5 N3 C17 C18 -13.0(3) . . . . ? O4 N3 C17 C18 166.1(2) . . . . ? C16 C17 C18 C19 -1.0(3) . . . . ? N3 C17 C18 C19 179.27(18) . . . . ? C17 C18 C19 C14 -1.8(3) . . . . ? C15 C14 C19 C18 3.4(3) . . . . ? C9 C14 C19 C18 179.67(17) . . . . ? C21 O7 C20 O6 5.2(4) . . . . ? C21 O7 C20 C8 -174.6(2) . . . . ? C7 C8 C20 O6 24.4(4) . . . . ? C9 C8 C20 O6 -150.2(2) . . . . ? C7 C8 C20 O7 -155.8(2) . . . . ? C9 C8 C20 O7 29.6(2) . . . . ? C20 O7 C21 C22 108.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.511 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.049