# Electronic Supplementary Material (ESI) for Organic and Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _publ_contact_author_name 'Fengjuan Shen' _publ_contact_author_email shenfjliu@126.com loop_ _publ_author_name 'FengJuan Shen' 'Xiaoliu Li' data_lxl2_0m _database_code_depnum_ccdc_archive 'CCDC 786926' #TrackingRef 'Shen,F.J.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H35 N5 O11 S' _chemical_formula_weight 625.65 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' S S 0.1246 0.1234 '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+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 8.5748(6) _cell_length_b 14.9184(10) _cell_length_c 23.0172(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2944.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.178 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8881 _exptl_absorpt_correction_T_max 0.9731 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18695 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.38 _reflns_number_total 7269 _reflns_number_gt 4391 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0976P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0039(11) _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 0.13(13) _refine_ls_number_reflns 7269 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1144 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1773 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 S1 S 0.35586(15) 0.21285(9) 0.99534(4) 0.0679(4) Uani 1 1 d . . . N1 N 1.2024(4) -0.0542(2) 0.83436(14) 0.0540(8) Uani 1 1 d . . . N2 N 0.9691(3) 0.02139(19) 0.82017(12) 0.0410(7) Uani 1 1 d . . . N3 N 0.5143(3) 0.16126(19) 0.90360(12) 0.0412(7) Uani 1 1 d . . . N4 N 0.2111(3) 0.33970(18) 0.75888(11) 0.0383(6) Uani 1 1 d . . . N5 N -0.0115(4) 0.2665(2) 0.72589(15) 0.0530(8) Uani 1 1 d . . . O1 O 1.3690(3) -0.0809(2) 0.76110(13) 0.0690(8) Uani 1 1 d . . . O2 O 1.0315(4) -0.0362(2) 0.90836(12) 0.0734(9) Uani 1 1 d . . . O3 O 0.7165(3) 0.05060(17) 0.79209(11) 0.0526(7) Uani 1 1 d . . . O4 O 0.6725(4) 0.2289(2) 0.73935(12) 0.0635(8) Uani 1 1 d . . . H4 H 0.7207 0.2377 0.7696 0.095 Uiso 1 1 calc R . . O5 O 0.5183(4) 0.00965(18) 0.91305(13) 0.0636(8) Uani 1 1 d . . . O6 O 0.3973(3) 0.30717(17) 0.83187(10) 0.0477(6) Uani 1 1 d . . . O7 O 0.3392(4) 0.41405(17) 0.94600(10) 0.0542(7) Uani 1 1 d . . . O8 O 0.3262(3) 0.50216(17) 0.86708(10) 0.0536(7) Uani 1 1 d . . . O9 O 0.0132(3) 0.3014(2) 0.82107(12) 0.0619(7) Uani 1 1 d . . . O10 O -0.0424(4) 0.2237(2) 0.63285(14) 0.0791(9) Uani 1 1 d . . . O11 O 0.6654(5) 0.3014(3) 0.60198(15) 0.0938(11) Uani 1 1 d . . . H11 H 0.7408 0.3250 0.6177 0.141 Uiso 1 1 calc R . . C1 C 1.2494(4) -0.0446(3) 0.77706(17) 0.0479(9) Uani 1 1 d . . . C2 C 1.1493(4) 0.0091(3) 0.74089(16) 0.0498(9) Uani 1 1 d . . . C3 C 1.0136(4) 0.0379(2) 0.76380(16) 0.0472(9) Uani 1 1 d . . . H3 H 0.9465 0.0706 0.7402 0.057 Uiso 1 1 calc R . . C4 C 1.0652(4) -0.0240(3) 0.85816(17) 0.0498(9) Uani 1 1 d . . . C5 C 1.1953(6) 0.0240(4) 0.67981(19) 0.0765(14) Uani 1 1 d . . . H5A H 1.1182 0.0603 0.6609 0.115 Uiso 1 1 calc R . . H5B H 1.2032 -0.0327 0.6603 0.115 Uiso 1 1 calc R . . H5C H 1.2943 0.0539 0.6786 0.115 Uiso 1 1 calc R . . C6 C 0.8101(4) 0.0416(2) 0.84174(15) 0.0404(8) Uani 1 1 d . . . H6 H 0.7721 -0.0084 0.8655 0.048 Uiso 1 1 calc R . . C7 C 0.7948(4) 0.1290(2) 0.87560(15) 0.0406(8) Uani 1 1 d . . . H7A H 0.8768 0.1707 0.8650 0.049 Uiso 1 1 calc R . . H7B H 0.7994 0.1182 0.9171 0.049 Uiso 1 1 calc R . . C8 C 0.6346(4) 0.1651(2) 0.85788(14) 0.0371(7) Uani 1 1 d . . . H8 H 0.6470 0.2278 0.8459 0.045 Uiso 1 1 calc R . . C9 C 0.5885(4) 0.1097(2) 0.80391(14) 0.0402(8) Uani 1 1 d . . . H9 H 0.4961 0.0738 0.8132 0.048 Uiso 1 1 calc R . . C10 C 0.5578(4) 0.1623(3) 0.74872(16) 0.0479(9) Uani 1 1 d . . . H10A H 0.5564 0.1216 0.7159 0.057 Uiso 1 1 calc R . . H10B H 0.4561 0.1906 0.7513 0.057 Uiso 1 1 calc R . . C11 C 0.4701(5) 0.0841(3) 0.92804(16) 0.0491(9) Uani 1 1 d . . . C12 C 0.3494(6) 0.0977(3) 0.97470(19) 0.0712(13) Uani 1 1 d . . . H12A H 0.3719 0.0598 1.0079 0.085 Uiso 1 1 calc R . . H12B H 0.2466 0.0825 0.9601 0.085 Uiso 1 1 calc R . . C13 C 0.4436(4) 0.2433(2) 0.92578(14) 0.0429(8) Uani 1 1 d . . . H13 H 0.5255 0.2880 0.9324 0.052 Uiso 1 1 calc R . . C14 C 0.3217(4) 0.2822(3) 0.88537(14) 0.0435(8) Uani 1 1 d . . . H14 H 0.2430 0.2363 0.8771 0.052 Uiso 1 1 calc R . . C15 C 0.2405(4) 0.3663(2) 0.90691(15) 0.0436(8) Uani 1 1 d . . . H15 H 0.1378 0.3536 0.9237 0.052 Uiso 1 1 calc R . . C16 C 0.2303(4) 0.4276(2) 0.85311(14) 0.0409(8) Uani 1 1 d . . . H16 H 0.1231 0.4447 0.8433 0.049 Uiso 1 1 calc R . . C17 C 0.3114(4) 0.3759(2) 0.80462(14) 0.0389(7) Uani 1 1 d . . . H17 H 0.3862 0.4166 0.7862 0.047 Uiso 1 1 calc R . . C18 C 0.3385(5) 0.5062(3) 0.92897(15) 0.0521(9) Uani 1 1 d . . . C19 C 0.4911(7) 0.5484(4) 0.9446(2) 0.0872(16) Uani 1 1 d . . . H19A H 0.4945 0.5589 0.9857 0.131 Uiso 1 1 calc R . . H19B H 0.5019 0.6043 0.9244 0.131 Uiso 1 1 calc R . . H19C H 0.5747 0.5090 0.9338 0.131 Uiso 1 1 calc R . . C20 C 0.1987(6) 0.5529(3) 0.9546(2) 0.0717(13) Uani 1 1 d . . . H20A H 0.1067 0.5180 0.9472 0.108 Uiso 1 1 calc R . . H20B H 0.1875 0.6110 0.9372 0.108 Uiso 1 1 calc R . . H20C H 0.2127 0.5594 0.9958 0.108 Uiso 1 1 calc R . . C21 C 0.2711(4) 0.3332(2) 0.70327(14) 0.0408(8) Uani 1 1 d . . . H21 H 0.3697 0.3570 0.6965 0.049 Uiso 1 1 calc R . . C22 C 0.1973(4) 0.2954(3) 0.65890(15) 0.0470(8) Uani 1 1 d . . . C23 C 0.0422(5) 0.2597(3) 0.66900(18) 0.0549(10) Uani 1 1 d . . . C24 C 0.0679(4) 0.3029(2) 0.77168(17) 0.0465(8) Uani 1 1 d . . . C25 C 0.2619(6) 0.2900(4) 0.59896(18) 0.0729(13) Uani 1 1 d . . . H25A H 0.1953 0.3223 0.5728 0.109 Uiso 1 1 calc R . . H25B H 0.2678 0.2284 0.5872 0.109 Uiso 1 1 calc R . . H25C H 0.3644 0.3159 0.5983 0.109 Uiso 1 1 calc R . . C26 C 0.6761(7) 0.3126(4) 0.5426(2) 0.0885(16) Uani 1 1 d . . . H26A H 0.5799 0.2945 0.5247 0.133 Uiso 1 1 calc R . . H26B H 0.7599 0.2765 0.5278 0.133 Uiso 1 1 calc R . . H26C H 0.6960 0.3745 0.5340 0.133 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 S1 0.0779(8) 0.0820(8) 0.0439(5) 0.0072(5) 0.0162(5) 0.0252(6) N1 0.0414(16) 0.064(2) 0.0568(19) 0.0011(15) 0.0026(15) 0.0141(16) N2 0.0396(15) 0.0429(16) 0.0405(15) -0.0044(12) 0.0002(12) 0.0106(13) N3 0.0393(15) 0.0421(16) 0.0423(15) 0.0016(13) 0.0067(12) 0.0076(13) N4 0.0339(14) 0.0410(15) 0.0401(15) 0.0019(12) -0.0030(11) -0.0051(12) N5 0.0464(17) 0.0506(18) 0.062(2) 0.0019(15) -0.0130(15) -0.0086(15) O1 0.0470(15) 0.076(2) 0.084(2) -0.0091(16) 0.0183(15) 0.0147(15) O2 0.0639(18) 0.111(3) 0.0450(16) 0.0035(15) 0.0005(14) 0.0228(19) O3 0.0468(14) 0.0578(16) 0.0534(15) -0.0199(12) -0.0103(12) 0.0193(13) O4 0.0585(17) 0.0735(19) 0.0586(17) 0.0112(15) 0.0021(14) -0.0139(15) O5 0.0726(19) 0.0412(16) 0.0771(19) 0.0121(14) 0.0165(15) 0.0041(14) O6 0.0449(13) 0.0609(16) 0.0372(12) 0.0013(11) 0.0039(10) 0.0186(12) O7 0.0796(19) 0.0446(14) 0.0384(13) -0.0047(11) -0.0042(13) 0.0141(14) O8 0.0728(19) 0.0493(15) 0.0387(13) -0.0004(11) 0.0005(12) -0.0082(14) O9 0.0494(15) 0.082(2) 0.0544(17) 0.0063(14) 0.0031(13) -0.0171(14) O10 0.073(2) 0.085(2) 0.079(2) -0.0272(18) -0.0222(17) -0.0090(18) O11 0.086(3) 0.116(3) 0.080(2) -0.029(2) -0.0024(19) -0.019(2) C1 0.0358(18) 0.049(2) 0.059(2) -0.0063(17) 0.0073(16) -0.0003(16) C2 0.046(2) 0.051(2) 0.053(2) -0.0005(17) 0.0058(17) -0.0018(18) C3 0.047(2) 0.0421(19) 0.052(2) 0.0002(16) 0.0001(17) 0.0020(16) C4 0.0408(19) 0.062(2) 0.046(2) -0.0067(18) -0.0007(16) 0.0137(18) C5 0.068(3) 0.100(4) 0.061(3) 0.013(2) 0.019(2) -0.003(3) C6 0.0348(17) 0.0403(18) 0.0460(19) -0.0058(14) -0.0029(14) 0.0038(15) C7 0.0341(17) 0.0411(19) 0.0465(19) -0.0069(15) 0.0003(15) 0.0031(15) C8 0.0342(17) 0.0345(17) 0.0425(18) 0.0014(14) 0.0040(14) 0.0040(14) C9 0.0326(17) 0.0400(19) 0.048(2) -0.0052(15) -0.0008(14) 0.0064(14) C10 0.0421(19) 0.054(2) 0.047(2) -0.0058(17) -0.0039(16) 0.0029(18) C11 0.051(2) 0.045(2) 0.050(2) 0.0151(17) 0.0044(17) 0.0000(18) C12 0.072(3) 0.079(3) 0.063(3) 0.023(2) 0.024(2) 0.011(3) C13 0.045(2) 0.042(2) 0.0422(18) -0.0050(15) 0.0022(15) 0.0087(15) C14 0.0421(19) 0.0454(19) 0.0430(18) -0.0016(15) 0.0055(15) 0.0037(16) C15 0.0440(19) 0.0424(19) 0.0442(19) 0.0029(15) 0.0093(16) 0.0073(15) C16 0.0367(17) 0.043(2) 0.0431(18) 0.0009(15) 0.0013(14) 0.0010(15) C17 0.0326(16) 0.0437(19) 0.0406(18) 0.0010(14) 0.0010(14) -0.0010(15) C18 0.067(3) 0.052(2) 0.0366(18) -0.0068(16) 0.0045(17) 0.000(2) C19 0.091(4) 0.106(4) 0.065(3) -0.018(3) -0.006(3) -0.022(3) C20 0.095(4) 0.049(2) 0.071(3) -0.008(2) 0.021(3) 0.016(2) C21 0.0410(19) 0.0390(18) 0.0423(19) 0.0044(15) 0.0010(14) -0.0004(15) C22 0.050(2) 0.048(2) 0.0430(19) -0.0028(16) -0.0071(16) 0.0029(18) C23 0.056(2) 0.053(2) 0.056(2) -0.0090(18) -0.014(2) 0.0023(19) C24 0.0451(19) 0.043(2) 0.052(2) 0.0050(16) -0.0082(17) -0.0039(16) C25 0.065(3) 0.098(4) 0.055(2) -0.019(2) -0.002(2) -0.003(3) C26 0.102(4) 0.096(4) 0.068(3) -0.014(3) 0.001(3) -0.004(3) _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 S1 C12 1.783(5) . ? S1 C13 1.827(4) . ? N1 C4 1.373(5) . ? N1 C1 1.387(5) . ? N2 C3 1.375(4) . ? N2 C4 1.379(5) . ? N2 C6 1.482(4) . ? N3 C11 1.337(5) . ? N3 C13 1.458(4) . ? N3 C8 1.475(4) . ? N4 C24 1.377(5) . ? N4 C21 1.383(4) . ? N4 C17 1.463(4) . ? N5 C24 1.367(5) . ? N5 C23 1.392(5) . ? O1 C1 1.216(4) . ? O2 C4 1.205(5) . ? O3 C6 1.403(4) . ? O3 C9 1.433(4) . ? O4 C10 1.414(5) . ? O4 H4 0.8200 . ? O5 C11 1.234(5) . ? O6 C17 1.410(4) . ? O6 C14 1.441(4) . ? O7 C15 1.426(5) . ? O7 C18 1.429(5) . ? O8 C16 1.420(4) . ? O8 C18 1.430(4) . ? O9 C24 1.230(4) . ? O10 C23 1.228(5) . ? O11 C26 1.380(6) . ? O11 H11 0.8200 . ? C1 C2 1.440(5) . ? C2 C3 1.348(5) . ? C2 C5 1.477(5) . ? C3 H3 0.9300 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.526(5) . ? C6 H6 0.9800 . ? C7 C8 1.531(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.544(5) . ? C8 H8 0.9800 . ? C9 C10 1.517(5) . ? C9 H9 0.9800 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.505(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.515(5) . ? C13 H13 0.9800 . ? C14 C15 1.517(5) . ? C14 H14 0.9800 . ? C15 C16 1.542(5) . ? C15 H15 0.9800 . ? C16 C17 1.525(5) . ? C16 H16 0.9800 . ? C17 H17 0.9800 . ? C18 C19 1.496(7) . ? C18 C20 1.508(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.327(5) . ? C21 H21 0.9300 . ? C22 C23 1.452(6) . ? C22 C25 1.489(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? 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 C12 S1 C13 91.09(17) . . ? C4 N1 C1 126.5(3) . . ? C3 N2 C4 121.4(3) . . ? C3 N2 C6 122.4(3) . . ? C4 N2 C6 115.9(3) . . ? C11 N3 C13 117.2(3) . . ? C11 N3 C8 122.2(3) . . ? C13 N3 C8 120.5(3) . . ? C24 N4 C21 120.1(3) . . ? C24 N4 C17 121.2(3) . . ? C21 N4 C17 118.3(3) . . ? C24 N5 C23 126.1(3) . . ? C6 O3 C9 110.0(2) . . ? C10 O4 H4 109.5 . . ? C17 O6 C14 109.4(2) . . ? C15 O7 C18 107.8(3) . . ? C16 O8 C18 107.5(3) . . ? C26 O11 H11 109.5 . . ? O1 C1 N1 119.1(4) . . ? O1 C1 C2 125.2(4) . . ? N1 C1 C2 115.7(3) . . ? C3 C2 C1 117.8(3) . . ? C3 C2 C5 123.7(4) . . ? C1 C2 C5 118.3(4) . . ? C2 C3 N2 123.5(3) . . ? C2 C3 H3 118.2 . . ? N2 C3 H3 118.2 . . ? O2 C4 N1 122.5(4) . . ? O2 C4 N2 122.7(3) . . ? N1 C4 N2 114.8(3) . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 N2 105.9(3) . . ? O3 C6 C7 106.6(3) . . ? N2 C6 C7 115.1(3) . . ? O3 C6 H6 109.7 . . ? N2 C6 H6 109.7 . . ? C7 C6 H6 109.7 . . ? C6 C7 C8 104.0(3) . . ? C6 C7 H7A 111.0 . . ? C8 C7 H7A 111.0 . . ? C6 C7 H7B 111.0 . . ? C8 C7 H7B 111.0 . . ? H7A C7 H7B 109.0 . . ? N3 C8 C7 115.1(3) . . ? N3 C8 C9 112.0(3) . . ? C7 C8 C9 104.8(3) . . ? N3 C8 H8 108.2 . . ? C7 C8 H8 108.2 . . ? C9 C8 H8 108.2 . . ? O3 C9 C10 107.0(3) . . ? O3 C9 C8 106.6(3) . . ? C10 C9 C8 116.1(3) . . ? O3 C9 H9 109.0 . . ? C10 C9 H9 109.0 . . ? C8 C9 H9 109.0 . . ? O4 C10 C9 111.8(3) . . ? O4 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? O4 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? O5 C11 N3 124.2(3) . . ? O5 C11 C12 123.5(4) . . ? N3 C11 C12 112.3(3) . . ? C11 C12 S1 107.4(3) . . ? C11 C12 H12A 110.2 . . ? S1 C12 H12A 110.2 . . ? C11 C12 H12B 110.2 . . ? S1 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? N3 C13 C14 113.2(3) . . ? N3 C13 S1 105.6(2) . . ? C14 C13 S1 110.4(2) . . ? N3 C13 H13 109.2 . . ? C14 C13 H13 109.2 . . ? S1 C13 H13 109.2 . . ? O6 C14 C13 108.2(3) . . ? O6 C14 C15 105.8(3) . . ? C13 C14 C15 115.6(3) . . ? O6 C14 H14 109.0 . . ? C13 C14 H14 109.0 . . ? C15 C14 H14 109.0 . . ? O7 C15 C14 110.3(3) . . ? O7 C15 C16 104.1(3) . . ? C14 C15 C16 104.7(3) . . ? O7 C15 H15 112.4 . . ? C14 C15 H15 112.4 . . ? C16 C15 H15 112.4 . . ? O8 C16 C17 107.4(3) . . ? O8 C16 C15 104.5(3) . . ? C17 C16 C15 105.2(3) . . ? O8 C16 H16 113.0 . . ? C17 C16 H16 113.0 . . ? C15 C16 H16 113.0 . . ? O6 C17 N4 111.1(3) . . ? O6 C17 C16 106.3(3) . . ? N4 C17 C16 116.5(3) . . ? O6 C17 H17 107.6 . . ? N4 C17 H17 107.6 . . ? C16 C17 H17 107.6 . . ? O7 C18 O8 103.5(3) . . ? O7 C18 C19 109.6(4) . . ? O8 C18 C19 108.8(3) . . ? O7 C18 C20 109.9(3) . . ? O8 C18 C20 110.5(3) . . ? C19 C18 C20 114.0(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N4 124.4(3) . . ? C22 C21 H21 117.8 . . ? N4 C21 H21 117.8 . . ? C21 C22 C23 118.0(3) . . ? C21 C22 C25 124.0(4) . . ? C23 C22 C25 118.0(3) . . ? O10 C23 N5 118.3(4) . . ? O10 C23 C22 126.4(4) . . ? N5 C23 C22 115.3(3) . . ? O9 C24 N5 121.0(3) . . ? O9 C24 N4 123.1(3) . . ? N5 C24 N4 115.9(3) . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O11 C26 H26A 109.5 . . ? O11 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O11 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.882 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.054