data_pxk2s _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H27 N O7 S2' _chemical_formula_sum 'C23 H27 N O7 S2' _chemical_formula_weight 493.58 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 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 15.327(5) _cell_length_b 7.905(3) _cell_length_c 19.504(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.912(10) _cell_angle_gamma 90.00 _cell_volume 2346.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1412 _cell_measurement_theta_min 2.681 _cell_measurement_theta_max 18.641 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.272 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9707 _exptl_absorpt_correction_T_max 0.9839 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 17246 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5772 _reflns_number_gt 3178 _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, 1990)' _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^)+(0.0693P)^2^+0.6209P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5772 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1509 _refine_ls_R_factor_gt 0.0804 _refine_ls_wR_factor_ref 0.1868 _refine_ls_wR_factor_gt 0.1587 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 C1 C 0.5782(2) 1.1889(5) 0.0705(2) 0.0596(11) Uani 1 1 d . . . H1 H 0.5472 1.1263 0.0352 0.071 Uiso 1 1 calc R . . C2 C 0.6024(3) 1.3540(5) 0.0588(2) 0.0709(12) Uani 1 1 d . . . H2 H 0.5879 1.4028 0.0155 0.085 Uiso 1 1 calc R . . C3 C 0.6481(3) 1.4462(5) 0.1115(3) 0.0729(13) Uani 1 1 d . . . H3 H 0.6642 1.5573 0.1037 0.087 Uiso 1 1 calc R . . C4 C 0.6698(3) 1.3743(6) 0.1755(3) 0.0714(13) Uani 1 1 d . . . H4 H 0.7008 1.4371 0.2106 0.086 Uiso 1 1 calc R . . C5 C 0.6460(2) 1.2105(5) 0.1880(2) 0.0578(10) Uani 1 1 d . . . H5 H 0.6604 1.1624 0.2314 0.069 Uiso 1 1 calc R . . C6 C 0.6001(2) 1.1178(4) 0.13451(19) 0.0443(8) Uani 1 1 d . . . C7 C 0.4165(2) 1.0530(5) 0.1607(2) 0.0468(9) Uani 1 1 d . . . C8 C 0.3371(3) 1.1757(6) 0.0624(2) 0.0831(15) Uani 1 1 d . . . H8A H 0.2825 1.1830 0.0818 0.125 Uiso 1 1 calc R . . H8B H 0.3255 1.1567 0.0135 0.125 Uiso 1 1 calc R . . H8C H 0.3691 1.2796 0.0708 0.125 Uiso 1 1 calc R . . C9 C 0.4707(2) 0.9004(4) 0.18882(17) 0.0398(8) Uani 1 1 d . . . C10 C 0.4882(2) 0.8963(5) 0.26910(18) 0.0518(9) Uani 1 1 d . . . H10A H 0.5503 0.9109 0.2845 0.062 Uiso 1 1 calc R . . H10B H 0.4558 0.9855 0.2890 0.062 Uiso 1 1 calc R . . C11 C 0.4566(3) 0.7212(5) 0.29036(19) 0.0571(10) Uani 1 1 d . . . H11 H 0.4937 0.6799 0.3314 0.069 Uiso 1 1 calc R . . C12 C 0.3602(3) 0.7210(5) 0.30271(19) 0.0602(11) Uani 1 1 d . . . H12A H 0.3533 0.7918 0.3423 0.072 Uiso 1 1 calc R . . H12B H 0.3432 0.6068 0.3135 0.072 Uiso 1 1 calc R . . C13 C 0.2990(2) 0.7852(5) 0.24039(17) 0.0504(9) Uani 1 1 d . . . H13A H 0.2400 0.7436 0.2431 0.061 Uiso 1 1 calc R . . H13B H 0.2972 0.9078 0.2414 0.061 Uiso 1 1 calc R . . C14 C 0.3290(2) 0.7284(4) 0.17418(17) 0.0412(8) Uani 1 1 d . . . C15 C 0.4267(2) 0.7242(4) 0.16913(18) 0.0438(8) Uani 1 1 d . . . H15 H 0.4397 0.6842 0.1239 0.053 Uiso 1 1 calc R . . C16 C 0.4681(2) 0.6110(5) 0.2281(2) 0.0563(10) Uani 1 1 d . . . H16A H 0.4370 0.5045 0.2296 0.068 Uiso 1 1 calc R . . H16B H 0.5297 0.5890 0.2245 0.068 Uiso 1 1 calc R . . C17 C 0.1362(2) 0.7817(5) 0.00719(19) 0.0470(9) Uani 1 1 d . . . C18 C 0.1631(2) 0.7633(5) -0.0567(2) 0.0635(11) Uani 1 1 d . . . H18 H 0.1805 0.6578 -0.0711 0.076 Uiso 1 1 calc R . . C19 C 0.1643(3) 0.9016(6) -0.0997(2) 0.0704(12) Uani 1 1 d . . . H19 H 0.1826 0.8879 -0.1432 0.085 Uiso 1 1 calc R . . C20 C 0.1391(2) 1.0592(6) -0.0797(2) 0.0596(11) Uani 1 1 d . . . C21 C 0.1122(3) 1.0756(5) -0.0152(2) 0.0638(11) Uani 1 1 d . . . H21 H 0.0950 1.1811 -0.0005 0.077 Uiso 1 1 calc R . . C22 C 0.1102(3) 0.9376(5) 0.0277(2) 0.0622(11) Uani 1 1 d . . . H22 H 0.0912 0.9504 0.0710 0.075 Uiso 1 1 calc R . . C23 C 0.1406(3) 1.2105(7) -0.1271(2) 0.0937(16) Uani 1 1 d . . . H23A H 0.1926 1.2067 -0.1499 0.141 Uiso 1 1 calc R . . H23B H 0.1404 1.3126 -0.1005 0.141 Uiso 1 1 calc R . . H23C H 0.0896 1.2080 -0.1609 0.141 Uiso 1 1 calc R . . N1 N 0.28229(19) 0.6723(4) 0.12103(15) 0.0540(8) Uani 1 1 d . . . H1A H 0.3012 0.5683 0.1111 0.065 Uiso 1 1 calc R . . H1B H 0.2885 0.7401 0.0849 0.065 Uiso 1 1 calc R . . O1 O 0.55817(15) 0.8238(3) 0.08208(12) 0.0539(7) Uani 1 1 d . . . O2 O 0.64291(15) 0.8338(3) 0.19768(13) 0.0609(7) Uani 1 1 d . . . O3 O 0.38880(16) 1.0367(3) 0.09430(14) 0.0579(7) Uani 1 1 d . . . O4 O 0.40089(19) 1.1722(3) 0.19518(14) 0.0717(8) Uani 1 1 d . . . O5 O 0.18982(16) 0.6637(3) 0.13111(13) 0.0598(7) Uani 1 1 d . . . O6 O 0.1695(2) 0.4639(4) 0.03199(17) 0.0854(10) Uani 1 1 d . . . O7 O 0.04624(18) 0.5945(4) 0.08327(16) 0.0888(11) Uani 1 1 d . . . S1 S 0.57480(6) 0.90312(11) 0.14846(5) 0.0449(3) Uani 1 1 d . . . S2 S 0.13100(7) 0.60650(14) 0.06103(6) 0.0639(3) Uani 1 1 d . . . 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 C1 0.054(2) 0.062(3) 0.061(3) -0.004(2) 0.000(2) -0.010(2) C2 0.067(3) 0.062(3) 0.085(3) 0.017(2) 0.013(3) 0.002(2) C3 0.063(3) 0.050(2) 0.109(4) -0.014(3) 0.026(3) -0.002(2) C4 0.061(3) 0.064(3) 0.090(4) -0.034(3) 0.011(3) -0.008(2) C5 0.050(2) 0.066(3) 0.058(3) -0.016(2) 0.008(2) 0.002(2) C6 0.0356(18) 0.049(2) 0.049(2) -0.0079(18) 0.0085(16) 0.0001(16) C7 0.042(2) 0.047(2) 0.054(2) 0.0023(18) 0.0160(18) -0.0014(16) C8 0.071(3) 0.097(4) 0.080(3) 0.037(3) 0.006(3) 0.033(3) C9 0.0402(18) 0.0422(18) 0.0368(19) -0.0048(15) 0.0040(15) 0.0023(15) C10 0.052(2) 0.059(2) 0.044(2) -0.0103(18) 0.0020(18) -0.0079(18) C11 0.059(2) 0.063(3) 0.045(2) 0.0111(19) -0.0104(19) -0.004(2) C12 0.070(3) 0.069(3) 0.041(2) 0.0062(19) 0.007(2) -0.013(2) C13 0.050(2) 0.055(2) 0.048(2) 0.0000(18) 0.0137(18) -0.0016(18) C14 0.045(2) 0.0402(18) 0.0362(19) 0.0015(15) -0.0044(16) -0.0044(15) C15 0.046(2) 0.0416(19) 0.044(2) -0.0099(16) 0.0059(17) 0.0029(16) C16 0.050(2) 0.047(2) 0.069(3) 0.002(2) -0.001(2) 0.0026(18) C17 0.040(2) 0.055(2) 0.044(2) 0.0025(17) -0.0053(17) -0.0031(16) C18 0.053(2) 0.070(3) 0.069(3) 0.002(2) 0.012(2) 0.016(2) C19 0.059(3) 0.095(4) 0.060(3) 0.016(3) 0.018(2) 0.013(3) C20 0.043(2) 0.076(3) 0.058(3) 0.020(2) -0.0015(19) -0.005(2) C21 0.079(3) 0.051(2) 0.060(3) -0.004(2) 0.003(2) -0.007(2) C22 0.079(3) 0.067(3) 0.041(2) -0.003(2) 0.009(2) -0.013(2) C23 0.097(4) 0.098(4) 0.088(4) 0.042(3) 0.018(3) -0.005(3) N1 0.056(2) 0.0552(19) 0.0494(19) 0.0114(16) 0.0023(16) -0.0028(15) O1 0.0565(15) 0.0528(15) 0.0537(15) -0.0141(13) 0.0123(12) 0.0005(12) O2 0.0449(15) 0.0658(17) 0.0704(18) 0.0087(14) 0.0006(13) 0.0147(13) O3 0.0547(16) 0.0626(17) 0.0552(17) 0.0095(14) 0.0023(13) 0.0142(13) O4 0.092(2) 0.0527(17) 0.074(2) -0.0052(15) 0.0256(17) 0.0219(15) O5 0.0439(14) 0.0807(19) 0.0520(16) 0.0142(14) -0.0049(12) -0.0115(13) O6 0.101(2) 0.0492(17) 0.095(2) 0.0011(16) -0.0322(19) -0.0039(16) O7 0.0541(18) 0.119(3) 0.088(2) 0.044(2) -0.0132(16) -0.0323(17) S1 0.0401(5) 0.0471(5) 0.0476(6) -0.0045(4) 0.0054(4) 0.0042(4) S2 0.0575(7) 0.0656(7) 0.0627(7) 0.0180(6) -0.0172(5) -0.0180(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 C1 C6 1.374(5) . ? C1 C2 1.384(5) . ? C1 H1 0.9300 . ? C2 C3 1.381(6) . ? C2 H2 0.9300 . ? C3 C4 1.375(6) . ? C3 H3 0.9300 . ? C4 C5 1.374(6) . ? C4 H4 0.9300 . ? C5 C6 1.394(5) . ? C5 H5 0.9300 . ? C6 S1 1.769(4) . ? C7 O4 1.198(4) . ? C7 O3 1.320(4) . ? C7 C9 1.529(5) . ? C8 O3 1.451(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.557(5) . ? C9 C15 1.575(4) . ? C9 S1 1.862(3) . ? C10 C11 1.540(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.522(5) . ? C11 C12 1.525(5) . ? C11 H11 0.9800 . ? C12 C13 1.530(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.491(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N1 1.267(4) . ? C14 C15 1.512(5) . ? C15 C16 1.533(5) . ? C15 H15 0.9800 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.366(5) . ? C17 C22 1.370(5) . ? C17 S2 1.746(4) . ? C18 C19 1.380(6) . ? C18 H18 0.9300 . ? C19 C20 1.376(6) . ? C19 H19 0.9300 . ? C20 C21 1.375(6) . ? C20 C23 1.513(6) . ? C21 C22 1.378(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? N1 O5 1.456(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? O1 S1 1.434(2) . ? O2 S1 1.439(2) . ? O5 S2 1.609(3) . ? O6 S2 1.421(3) . ? O7 S2 1.421(3) . ? 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 C1 C2 119.7(4) . . ? C6 C1 H1 120.2 . . ? C2 C1 H1 120.2 . . ? C3 C2 C1 119.8(4) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 120.7(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 118.9(4) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C1 C6 C5 120.7(4) . . ? C1 C6 S1 119.9(3) . . ? C5 C6 S1 119.3(3) . . ? O4 C7 O3 124.4(3) . . ? O4 C7 C9 123.8(4) . . ? O3 C7 C9 111.8(3) . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 C10 113.4(3) . . ? C7 C9 C15 114.3(3) . . ? C10 C9 C15 104.1(3) . . ? C7 C9 S1 107.2(2) . . ? C10 C9 S1 111.9(2) . . ? C15 C9 S1 105.7(2) . . ? C11 C10 C9 105.5(3) . . ? C11 C10 H10A 110.6 . . ? C9 C10 H10A 110.6 . . ? C11 C10 H10B 110.6 . . ? C9 C10 H10B 110.6 . . ? H10A C10 H10B 108.8 . . ? C16 C11 C12 109.5(3) . . ? C16 C11 C10 103.2(3) . . ? C12 C11 C10 112.7(3) . . ? C16 C11 H11 110.4 . . ? C12 C11 H11 110.4 . . ? C10 C11 H11 110.4 . . ? C11 C12 C13 112.8(3) . . ? C11 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? C11 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C14 C13 C12 111.4(3) . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N1 C14 C13 127.7(3) . . ? N1 C14 C15 113.9(3) . . ? C13 C14 C15 118.3(3) . . ? C14 C15 C16 106.7(3) . . ? C14 C15 C9 111.3(3) . . ? C16 C15 C9 101.9(3) . . ? C14 C15 H15 112.1 . . ? C16 C15 H15 112.1 . . ? C9 C15 H15 112.1 . . ? C11 C16 C15 100.8(3) . . ? C11 C16 H16A 111.6 . . ? C15 C16 H16A 111.6 . . ? C11 C16 H16B 111.6 . . ? C15 C16 H16B 111.6 . . ? H16A C16 H16B 109.4 . . ? C18 C17 C22 119.5(4) . . ? C18 C17 S2 120.3(3) . . ? C22 C17 S2 120.1(3) . . ? C17 C18 C19 119.9(4) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 121.3(4) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C21 C20 C19 118.1(4) . . ? C21 C20 C23 120.8(4) . . ? C19 C20 C23 121.1(4) . . ? C20 C21 C22 120.8(4) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C17 C22 C21 120.4(4) . . ? C17 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C14 N1 O5 111.7(3) . . ? C14 N1 H1A 109.3 . . ? O5 N1 H1A 109.3 . . ? C14 N1 H1B 109.3 . . ? O5 N1 H1B 109.3 . . ? H1A N1 H1B 107.9 . . ? C7 O3 C8 116.2(3) . . ? N1 O5 S2 110.7(2) . . ? O1 S1 O2 118.14(16) . . ? O1 S1 C6 107.41(16) . . ? O2 S1 C6 108.24(16) . . ? O1 S1 C9 107.97(15) . . ? O2 S1 C9 107.65(15) . . ? C6 S1 C9 106.93(15) . . ? O6 S2 O7 120.5(2) . . ? O6 S2 O5 110.14(16) . . ? O7 S2 O5 101.46(17) . . ? O6 S2 C17 109.8(2) . . ? O7 S2 C17 110.24(18) . . ? O5 S2 C17 103.11(16) . . ? 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 -0.3(6) . . . . ? C1 C2 C3 C4 0.2(7) . . . . ? C2 C3 C4 C5 -0.3(7) . . . . ? C3 C4 C5 C6 0.5(6) . . . . ? C2 C1 C6 C5 0.4(6) . . . . ? C2 C1 C6 S1 -176.5(3) . . . . ? C4 C5 C6 C1 -0.6(5) . . . . ? C4 C5 C6 S1 176.4(3) . . . . ? O4 C7 C9 C10 11.7(5) . . . . ? O3 C7 C9 C10 -168.0(3) . . . . ? O4 C7 C9 C15 130.8(4) . . . . ? O3 C7 C9 C15 -48.9(4) . . . . ? O4 C7 C9 S1 -112.3(4) . . . . ? O3 C7 C9 S1 67.9(3) . . . . ? C7 C9 C10 C11 126.3(3) . . . . ? C15 C9 C10 C11 1.5(4) . . . . ? S1 C9 C10 C11 -112.2(3) . . . . ? C9 C10 C11 C16 27.8(4) . . . . ? C9 C10 C11 C12 -90.2(4) . . . . ? C16 C11 C12 C13 -58.5(4) . . . . ? C10 C11 C12 C13 55.8(4) . . . . ? C11 C12 C13 C14 37.3(4) . . . . ? C12 C13 C14 N1 137.5(4) . . . . ? C12 C13 C14 C15 -38.1(4) . . . . ? N1 C14 C15 C16 -119.8(3) . . . . ? C13 C14 C15 C16 56.4(4) . . . . ? N1 C14 C15 C9 129.8(3) . . . . ? C13 C14 C15 C9 -54.0(4) . . . . ? C7 C9 C15 C14 -40.7(4) . . . . ? C10 C9 C15 C14 83.5(3) . . . . ? S1 C9 C15 C14 -158.4(2) . . . . ? C7 C9 C15 C16 -154.2(3) . . . . ? C10 C9 C15 C16 -29.9(3) . . . . ? S1 C9 C15 C16 88.1(3) . . . . ? C12 C11 C16 C15 73.4(3) . . . . ? C10 C11 C16 C15 -46.9(3) . . . . ? C14 C15 C16 C11 -69.5(3) . . . . ? C9 C15 C16 C11 47.3(3) . . . . ? C22 C17 C18 C19 0.4(6) . . . . ? S2 C17 C18 C19 178.0(3) . . . . ? C17 C18 C19 C20 0.1(6) . . . . ? C18 C19 C20 C21 -0.2(6) . . . . ? C18 C19 C20 C23 -180.0(4) . . . . ? C19 C20 C21 C22 -0.3(6) . . . . ? C23 C20 C21 C22 179.5(4) . . . . ? C18 C17 C22 C21 -0.8(6) . . . . ? S2 C17 C22 C21 -178.4(3) . . . . ? C20 C21 C22 C17 0.8(6) . . . . ? C13 C14 N1 O5 -1.3(5) . . . . ? C15 C14 N1 O5 174.4(3) . . . . ? O4 C7 O3 C8 0.8(5) . . . . ? C9 C7 O3 C8 -179.5(3) . . . . ? C14 N1 O5 S2 175.4(2) . . . . ? C1 C6 S1 O1 17.7(3) . . . . ? C5 C6 S1 O1 -159.3(3) . . . . ? C1 C6 S1 O2 146.3(3) . . . . ? C5 C6 S1 O2 -30.7(3) . . . . ? C1 C6 S1 C9 -98.0(3) . . . . ? C5 C6 S1 C9 85.1(3) . . . . ? C7 C9 S1 O1 -83.7(3) . . . . ? C10 C9 S1 O1 151.4(2) . . . . ? C15 C9 S1 O1 38.7(3) . . . . ? C7 C9 S1 O2 147.7(2) . . . . ? C10 C9 S1 O2 22.8(3) . . . . ? C15 C9 S1 O2 -89.9(2) . . . . ? C7 C9 S1 C6 31.6(3) . . . . ? C10 C9 S1 C6 -93.3(3) . . . . ? C15 C9 S1 C6 154.0(2) . . . . ? N1 O5 S2 O6 47.3(3) . . . . ? N1 O5 S2 O7 176.0(2) . . . . ? N1 O5 S2 C17 -69.8(3) . . . . ? C18 C17 S2 O6 8.4(4) . . . . ? C22 C17 S2 O6 -174.1(3) . . . . ? C18 C17 S2 O7 -126.6(3) . . . . ? C22 C17 S2 O7 50.9(4) . . . . ? C18 C17 S2 O5 125.7(3) . . . . ? C22 C17 S2 O5 -56.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.270 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.055