data_cd24138 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H22 N2 O6 S' _chemical_formula_weight 430.47 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 20.5357(16) _cell_length_b 11.4427(9) _cell_length_c 20.5964(15) _cell_angle_alpha 90.00 _cell_angle_beta 117.564(2) _cell_angle_gamma 90.00 _cell_volume 4290.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1586 _cell_measurement_theta_min 4.462 _cell_measurement_theta_max 39.510 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.368 _exptl_crystal_size_mid 0.327 _exptl_crystal_size_min 0.163 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.51549 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_% ? _diffrn_reflns_number 25789 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.1489 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 28.32 _reflns_number_total 9877 _reflns_number_gt 3029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0788P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9877 _refine_ls_number_parameters 584 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1798 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1880 _refine_ls_wR_factor_gt 0.1559 _refine_ls_goodness_of_fit_ref 0.740 _refine_ls_restrained_S_all 0.845 _refine_ls_shift/su_max 0.065 _refine_ls_shift/su_mean 0.011 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 0.74465(7) 0.20720(11) 0.70423(6) 0.0576(4) Uani 1 1 d . . . S2 S 0.24176(7) 0.15212(10) 0.70470(6) 0.0537(4) Uani 1 1 d . . . N1 N 0.67120(18) 0.1639(3) 0.63142(17) 0.0490(9) Uani 1 1 d . . . N2 N 0.5862(3) -0.3856(5) 0.5955(3) 0.0849(15) Uani 1 1 d . . . N3 N 0.16774(18) 0.1066(3) 0.63346(17) 0.0471(9) Uani 1 1 d . . . N4 N 0.0819(3) -0.4432(5) 0.5963(3) 0.0885(16) Uani 1 1 d . . . O1 O 0.66683(19) 0.0179(3) 0.43613(17) 0.0802(11) Uani 1 1 d . . . O2 O 0.5841(2) 0.1555(4) 0.38163(19) 0.1100(15) Uani 1 1 d . . . O3 O 0.5450(2) -0.4015(4) 0.6225(3) 0.1105(16) Uani 1 1 d . . . O4 O 0.6077(3) -0.4630(4) 0.5697(3) 0.1245(18) Uani 1 1 d . . . O5 O 0.71843(17) 0.2599(3) 0.75067(15) 0.0735(10) Uani 1 1 d . . . O6 O 0.79332(17) 0.1093(3) 0.72843(16) 0.0735(10) Uani 1 1 d . . . O7 O 0.1609(2) -0.0369(3) 0.43573(18) 0.0840(11) Uani 1 1 d . . . O8 O 0.0740(2) 0.0960(3) 0.38169(19) 0.1073(15) Uani 1 1 d D . . O9 O 0.0429(3) -0.4599(4) 0.6251(3) 0.1283(19) Uani 1 1 d . . . O10 O 0.0999(3) -0.5193(4) 0.5662(3) 0.1290(18) Uani 1 1 d . . . O11 O 0.21707(17) 0.2061(3) 0.75184(15) 0.0685(9) Uani 1 1 d . . . O12 O 0.29049(16) 0.0541(3) 0.72917(16) 0.0678(9) Uani 1 1 d . . . C1 C 0.6149(3) 0.2552(4) 0.5914(3) 0.0543(12) Uani 1 1 d D . . C2 C 0.5990(2) 0.2331(4) 0.5148(2) 0.0516(12) Uani 1 1 d . . . H2 H 0.5685 0.2804 0.4758 0.062 Uiso 1 1 calc R . . C3 C 0.6320(2) 0.1405(4) 0.5075(2) 0.0456(11) Uani 1 1 d . . . C4 C 0.6797(3) 0.0816(4) 0.5806(2) 0.0484(12) Uani 1 1 d . . . C5 C 0.5475(4) 0.2473(7) 0.6029(4) 0.0770(17) Uani 1 1 d D . . C6 C 0.6298(3) 0.0957(4) 0.4391(3) 0.0590(13) Uani 1 1 d . . . C7 C 0.5828(5) 0.1268(7) 0.3096(4) 0.180(4) Uani 1 1 d D . . H7 H 0.5851 0.1977 0.2849 0.216 Uiso 1 1 calc R . . H8 H 0.6242 0.0776 0.3172 0.216 Uiso 1 1 calc R . . C8 C 0.5153(8) 0.0669(13) 0.2673(9) 0.401(12) Uiso 1 1 d D . . H9 H 0.5081 0.0092 0.2972 0.601 Uiso 1 1 calc R . . H10 H 0.5170 0.0293 0.2264 0.601 Uiso 1 1 calc R . . H11 H 0.4755 0.1218 0.2497 0.601 Uiso 1 1 calc R . . C9 C 0.6563(2) -0.0425(4) 0.5874(2) 0.0467(11) Uani 1 1 d . . . C10 C 0.6833(2) -0.1356(4) 0.5639(2) 0.0598(13) Uani 1 1 d . . . H12 H 0.7166 -0.1221 0.5459 0.072 Uiso 1 1 calc R . . C11 C 0.6608(3) -0.2482(5) 0.5672(3) 0.0679(15) Uani 1 1 d . . . C12 C 0.6123(3) -0.2657(4) 0.5943(3) 0.0601(13) Uani 1 1 d . . . C13 C 0.5861(3) -0.1772(5) 0.6189(2) 0.0636(13) Uani 1 1 d . . . H14 H 0.5535 -0.1919 0.6376 0.076 Uiso 1 1 calc R . . C14 C 0.6086(3) -0.0642(5) 0.6159(3) 0.0581(13) Uani 1 1 d . . . C15 C 0.7845(2) 0.3175(4) 0.6755(2) 0.0511(12) Uani 1 1 d . . . C16 C 0.7736(3) 0.4329(5) 0.6867(3) 0.0565(13) Uani 1 1 d . . . C17 C 0.8008(3) 0.5196(4) 0.6594(3) 0.0694(14) Uani 1 1 d . . . H17 H 0.7928 0.5973 0.6669 0.083 Uiso 1 1 calc R . . C18 C 0.8394(3) 0.4944(5) 0.6213(3) 0.0683(14) Uani 1 1 d . . . C19 C 0.8523(3) 0.3785(5) 0.6140(3) 0.0756(17) Uani 1 1 d . . . C20 C 0.8252(3) 0.2890(4) 0.6407(3) 0.0663(14) Uani 1 1 d . . . H19 H 0.8346 0.2112 0.6349 0.080 Uiso 1 1 calc R . . C21 C 0.8664(3) 0.5905(5) 0.5894(3) 0.111(2) Uani 1 1 d . . . H21 H 0.8857 0.6535 0.6239 0.167 Uiso 1 1 calc R . . H20 H 0.8263 0.6185 0.5449 0.167 Uiso 1 1 calc R . . H22 H 0.9043 0.5604 0.5791 0.167 Uiso 1 1 calc R . . C22 C 0.1105(3) 0.1964(5) 0.5941(3) 0.0560(13) Uani 1 1 d . . . C23 C 0.0933(2) 0.1739(4) 0.5166(2) 0.0556(12) Uani 1 1 d . . . H24 H 0.0621 0.2209 0.4778 0.067 Uiso 1 1 calc R . . C24 C 0.1263(2) 0.0816(4) 0.5083(2) 0.0481(11) Uani 1 1 d . . . C25 C 0.1756(2) 0.0249(4) 0.5814(2) 0.0458(11) Uani 1 1 d D . . C26 C 0.0444(3) 0.1872(5) 0.6086(3) 0.0848(17) Uani 1 1 d . . . H27 H 0.0107 0.2495 0.5838 0.127 Uiso 1 1 calc R . . H26 H 0.0604 0.1929 0.6603 0.127 Uiso 1 1 calc R . . H28 H 0.0204 0.1135 0.5909 0.127 Uiso 1 1 calc R . . C27 C 0.1226(3) 0.0390(5) 0.4394(3) 0.0585(13) Uani 1 1 d . . . C28 C 0.0831(5) 0.0740(8) 0.3117(4) 0.203(5) Uani 1 1 d D . . H29 H 0.1037 0.1419 0.2996 0.244 Uiso 1 1 calc R . . H30 H 0.1144 0.0069 0.3179 0.244 Uiso 1 1 calc R . . C29 C 0.0112(7) 0.0529(12) 0.2580(8) 0.350(9) Uiso 1 1 d D . . H33 H -0.0028 -0.0253 0.2631 0.524 Uiso 1 1 calc R . . H32 H 0.0082 0.0621 0.2104 0.524 Uiso 1 1 calc R . . H31 H -0.0214 0.1075 0.2636 0.524 Uiso 1 1 calc R . . C30 C 0.1532(2) -0.0991(4) 0.5897(2) 0.0458(11) Uani 1 1 d . . . C31 C 0.1762(3) -0.1930(5) 0.5620(2) 0.0640(14) Uani 1 1 d . . . H34 H 0.2071 -0.1790 0.5411 0.077 Uiso 1 1 calc R . . C32 C 0.1545(3) -0.3044(5) 0.5648(3) 0.0666(14) Uani 1 1 d . . . H35 H 0.1702 -0.3662 0.5463 0.080 Uiso 1 1 calc R . . C33 C 0.1091(3) -0.3234(5) 0.5956(3) 0.0619(14) Uani 1 1 d . . . C34 C 0.0872(2) -0.2349(5) 0.6255(2) 0.0613(13) Uani 1 1 d . . . H36 H 0.0578 -0.2503 0.6478 0.074 Uiso 1 1 calc R . . C35 C 0.1092(2) -0.1231(4) 0.6221(2) 0.0558(13) Uani 1 1 d . . . H37 H 0.0942 -0.0624 0.6420 0.067 Uiso 1 1 calc R . . C36 C 0.2811(2) 0.2618(4) 0.6741(2) 0.0487(11) Uani 1 1 d . . . C37 C 0.2692(2) 0.3773(5) 0.6829(2) 0.0600(13) Uani 1 1 d . . . H38 H 0.2426 0.3983 0.7074 0.072 Uiso 1 1 calc R . . C38 C 0.2972(3) 0.4622(5) 0.6550(3) 0.0670(15) Uani 1 1 d . . . C39 C 0.3372(3) 0.4353(5) 0.6189(3) 0.0728(15) Uani 1 1 d . . . C40 C 0.3498(3) 0.3180(5) 0.6127(3) 0.0804(17) Uani 1 1 d . . . H40 H 0.3772 0.2970 0.5890 0.096 Uiso 1 1 calc R . . C41 C 0.3229(3) 0.2308(4) 0.6407(3) 0.0663(14) Uani 1 1 d . . . H41 H 0.3331 0.1526 0.6368 0.080 Uiso 1 1 calc R . . C42 C 0.3649(3) 0.5283(5) 0.5863(3) 0.108(2) Uani 1 1 d . . . H42 H 0.3276 0.5461 0.5376 0.162 Uiso 1 1 calc R . . H44 H 0.4081 0.5008 0.5844 0.162 Uiso 1 1 calc R . . H43 H 0.3765 0.5975 0.6160 0.162 Uiso 1 1 calc R . . H1 H 0.638(2) 0.329(2) 0.614(2) 0.067(14) Uiso 1 1 d D . . H3 H 0.728(2) 0.079(3) 0.590(2) 0.056(14) Uiso 1 1 d . . . H4 H 0.563(2) 0.244(4) 0.655(2) 0.074(16) Uiso 1 1 d . . . H5 H 0.523(2) 0.322(4) 0.589(2) 0.077(17) Uiso 1 1 d . . . H6 H 0.523(2) 0.177(3) 0.585(2) 0.08(2) Uiso 1 1 d D . . H13 H 0.678(2) -0.317(4) 0.554(2) 0.065(14) Uiso 1 1 d . . . H15 H 0.594(2) -0.001(4) 0.637(2) 0.065(14) Uiso 1 1 d . . . H16 H 0.744(2) 0.451(4) 0.711(2) 0.081(16) Uiso 1 1 d . . . H18 H 0.880(2) 0.361(3) 0.589(2) 0.056(13) Uiso 1 1 d . . . H23 H 0.128(2) 0.271(3) 0.6068(19) 0.047(13) Uiso 1 1 d . . . H25 H 0.2276(12) 0.025(3) 0.5922(18) 0.049(12) Uiso 1 1 d D . . H39 H 0.287(2) 0.541(4) 0.659(2) 0.070(16) Uiso 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 S1 0.0679(9) 0.0557(9) 0.0425(7) 0.0009(6) 0.0199(7) -0.0064(7) S2 0.0620(8) 0.0527(9) 0.0418(7) 0.0014(6) 0.0202(6) -0.0055(7) N1 0.056(2) 0.041(2) 0.047(2) -0.0053(18) 0.021(2) -0.0028(18) N2 0.069(4) 0.054(4) 0.096(4) 0.017(3) 0.008(3) -0.003(3) N3 0.047(2) 0.046(2) 0.045(2) -0.0016(18) 0.0190(19) 0.0021(18) N4 0.080(4) 0.057(4) 0.097(4) 0.011(3) 0.014(3) -0.007(3) O1 0.098(3) 0.082(3) 0.068(2) 0.0043(19) 0.045(2) 0.029(2) O2 0.153(4) 0.130(4) 0.053(2) 0.023(2) 0.053(3) 0.075(3) O3 0.087(3) 0.079(3) 0.159(4) 0.035(3) 0.052(3) -0.013(2) O4 0.154(4) 0.041(3) 0.177(5) -0.002(3) 0.075(4) -0.005(3) O5 0.101(3) 0.081(3) 0.0449(19) -0.0117(17) 0.0387(19) -0.017(2) O6 0.072(2) 0.060(2) 0.065(2) 0.0139(17) 0.0115(18) 0.0031(19) O7 0.101(3) 0.092(3) 0.071(3) 0.005(2) 0.049(2) 0.026(2) O8 0.155(4) 0.117(3) 0.046(2) 0.017(2) 0.043(3) 0.062(3) O9 0.120(4) 0.088(4) 0.182(5) 0.020(3) 0.074(4) -0.033(3) O10 0.161(5) 0.051(3) 0.175(5) 0.004(3) 0.077(4) 0.002(3) O11 0.090(2) 0.078(2) 0.0462(19) -0.0089(16) 0.0382(18) -0.0101(19) O12 0.067(2) 0.058(2) 0.060(2) 0.0159(16) 0.0134(17) 0.0038(18) C1 0.059(3) 0.045(3) 0.059(3) -0.005(3) 0.027(3) 0.005(3) C2 0.053(3) 0.048(3) 0.054(3) 0.013(2) 0.025(2) 0.006(2) C3 0.048(3) 0.046(3) 0.049(3) 0.004(2) 0.027(2) 0.005(2) C4 0.047(3) 0.049(3) 0.049(3) -0.002(2) 0.022(3) -0.001(2) C5 0.079(5) 0.089(6) 0.074(5) -0.001(4) 0.045(4) 0.013(4) C6 0.065(3) 0.058(4) 0.056(3) 0.009(3) 0.029(3) 0.020(3) C7 0.272(11) 0.204(9) 0.108(6) 0.026(6) 0.125(7) 0.129(9) C9 0.051(3) 0.045(3) 0.038(3) 0.001(2) 0.016(2) 0.001(2) C10 0.069(3) 0.048(3) 0.070(3) 0.009(3) 0.039(3) 0.010(3) C11 0.077(4) 0.037(4) 0.079(4) 0.006(3) 0.028(3) 0.011(3) C12 0.057(3) 0.043(3) 0.061(3) 0.013(3) 0.011(3) -0.004(3) C13 0.061(3) 0.056(4) 0.075(4) 0.007(3) 0.032(3) -0.004(3) C14 0.066(4) 0.050(4) 0.064(3) -0.001(3) 0.036(3) -0.003(3) C15 0.053(3) 0.051(3) 0.045(3) -0.009(2) 0.018(2) -0.006(2) C16 0.065(3) 0.051(4) 0.057(3) -0.010(3) 0.031(3) -0.009(3) C17 0.079(4) 0.051(4) 0.080(4) -0.010(3) 0.039(3) -0.003(3) C18 0.076(4) 0.060(4) 0.071(4) -0.008(3) 0.036(3) -0.018(3) C19 0.085(4) 0.077(5) 0.085(4) -0.019(3) 0.056(4) -0.013(3) C20 0.074(4) 0.051(4) 0.082(4) -0.011(3) 0.043(3) -0.008(3) C21 0.120(5) 0.093(5) 0.143(6) 0.004(4) 0.080(5) -0.028(4) C22 0.057(3) 0.051(4) 0.058(3) -0.002(3) 0.024(3) 0.002(3) C23 0.054(3) 0.055(3) 0.053(3) 0.006(2) 0.021(3) 0.003(3) C24 0.048(3) 0.051(3) 0.047(3) 0.003(2) 0.024(2) 0.000(2) C25 0.046(3) 0.045(3) 0.046(3) 0.000(2) 0.021(2) -0.001(2) C26 0.072(4) 0.105(5) 0.094(4) 0.004(3) 0.052(3) 0.020(3) C27 0.071(4) 0.060(4) 0.048(3) 0.001(3) 0.031(3) -0.001(3) C28 0.268(11) 0.214(10) 0.084(6) -0.017(6) 0.044(7) 0.149(8) C30 0.044(3) 0.045(3) 0.039(3) 0.002(2) 0.011(2) 0.003(2) C31 0.075(4) 0.055(4) 0.069(3) 0.011(3) 0.039(3) 0.015(3) C32 0.081(4) 0.044(3) 0.069(3) 0.003(3) 0.030(3) 0.013(3) C33 0.054(3) 0.048(4) 0.061(3) 0.014(3) 0.007(3) 0.000(3) C34 0.052(3) 0.058(4) 0.071(3) 0.009(3) 0.026(3) -0.002(3) C35 0.055(3) 0.055(4) 0.057(3) 0.003(2) 0.026(3) -0.001(3) C36 0.052(3) 0.050(3) 0.040(3) -0.005(2) 0.018(2) -0.005(2) C37 0.068(3) 0.058(4) 0.062(3) -0.005(3) 0.037(3) -0.002(3) C38 0.077(4) 0.049(4) 0.075(4) -0.007(3) 0.035(3) -0.006(3) C39 0.082(4) 0.060(4) 0.081(4) -0.010(3) 0.042(3) -0.014(3) C40 0.088(4) 0.084(5) 0.092(4) -0.022(4) 0.061(4) -0.018(4) C41 0.073(4) 0.054(4) 0.084(4) -0.013(3) 0.047(3) -0.011(3) C42 0.136(5) 0.086(5) 0.130(5) -0.005(4) 0.086(5) -0.042(4) _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 O6 1.429(3) . ? S1 O5 1.430(3) . ? S1 N1 1.636(3) . ? S1 C15 1.749(5) . ? S2 O11 1.427(3) . ? S2 O12 1.431(3) . ? S2 N3 1.634(3) . ? S2 C36 1.759(4) . ? N1 C4 1.477(5) . ? N1 C1 1.491(5) . ? N2 O4 1.217(6) . ? N2 O3 1.221(5) . ? N2 C12 1.477(6) . ? N3 C25 1.486(5) . ? N3 C22 1.487(5) . ? N4 O9 1.213(6) . ? N4 O10 1.221(6) . ? N4 C33 1.482(6) . ? O1 C6 1.191(5) . ? O2 C6 1.312(5) . ? O2 C7 1.509(6) . ? O7 C27 1.197(5) . ? O8 C27 1.318(5) . ? O8 C28 1.558(7) . ? C1 C2 1.477(6) . ? C1 C5 1.511(7) . ? C1 H1 0.97(2) . ? C2 C3 1.305(5) . ? C2 H2 0.9300 . ? C3 C6 1.479(6) . ? C3 C4 1.521(6) . ? C4 C9 1.527(6) . ? C4 H3 0.91(4) . ? C5 H4 0.97(4) . ? C5 H5 0.97(4) . ? C5 H6 0.94(2) . ? C7 C8 1.425(14) . ? C7 H7 0.9700 . ? C7 H8 0.9700 . ? C8 H9 0.9600 . ? C8 H10 0.9600 . ? C8 H11 0.9600 . ? C9 C14 1.377(6) . ? C9 C10 1.387(5) . ? C10 C11 1.381(6) . ? C10 H12 0.9300 . ? C11 C12 1.365(7) . ? C11 H13 0.96(4) . ? C12 C13 1.350(6) . ? C13 C14 1.384(6) . ? C13 H14 0.9300 . ? C14 H15 0.96(4) . ? C15 C20 1.370(5) . ? C15 C16 1.376(6) . ? C16 C17 1.380(6) . ? C16 H16 0.96(4) . ? C17 C18 1.380(6) . ? C17 H17 0.9300 . ? C18 C19 1.373(7) . ? C18 C21 1.512(6) . ? C19 C20 1.394(6) . ? C19 H18 0.94(4) . ? C20 H19 0.9300 . ? C21 H21 0.9600 . ? C21 H20 0.9600 . ? C21 H22 0.9600 . ? C22 C23 1.489(6) . ? C22 C26 1.523(6) . ? C22 H23 0.91(4) . ? C23 C24 1.308(5) . ? C23 H24 0.9300 . ? C24 C27 1.469(6) . ? C24 C25 1.518(6) . ? C25 C30 1.526(6) . ? C25 H25 0.986(19) . ? C26 H27 0.9600 . ? C26 H26 0.9600 . ? C26 H28 0.9600 . ? C28 C29 1.398(12) . ? C28 H29 0.9700 . ? C28 H30 0.9700 . ? C29 H33 0.9600 . ? C29 H32 0.9600 . ? C29 H31 0.9600 . ? C30 C35 1.377(5) . ? C30 C31 1.397(6) . ? C31 C32 1.361(6) . ? C31 H34 0.9300 . ? C32 C33 1.366(6) . ? C32 H35 0.9300 . ? C33 C34 1.364(6) . ? C34 C35 1.369(6) . ? C34 H36 0.9300 . ? C35 H37 0.9300 . ? C36 C37 1.371(6) . ? C36 C41 1.374(5) . ? C37 C38 1.381(6) . ? C37 H38 0.9300 . ? C38 C39 1.374(7) . ? C38 H39 0.94(4) . ? C39 C40 1.384(7) . ? C39 C42 1.504(6) . ? C40 C41 1.389(6) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 H42 0.9600 . ? C42 H44 0.9600 . ? C42 H43 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 O6 S1 O5 121.1(2) . . ? O6 S1 N1 106.36(19) . . ? O5 S1 N1 105.55(19) . . ? O6 S1 C15 108.8(2) . . ? O5 S1 C15 107.6(2) . . ? N1 S1 C15 106.59(18) . . ? O11 S2 O12 120.70(19) . . ? O11 S2 N3 105.85(18) . . ? O12 S2 N3 105.96(19) . . ? O11 S2 C36 107.5(2) . . ? O12 S2 C36 108.9(2) . . ? N3 S2 C36 107.21(18) . . ? C4 N1 C1 111.7(3) . . ? C4 N1 S1 118.8(3) . . ? C1 N1 S1 116.4(3) . . ? O4 N2 O3 123.9(6) . . ? O4 N2 C12 117.4(6) . . ? O3 N2 C12 118.6(6) . . ? C25 N3 C22 111.3(3) . . ? C25 N3 S2 118.8(3) . . ? C22 N3 S2 116.2(3) . . ? O9 N4 O10 124.0(6) . . ? O9 N4 C33 119.1(6) . . ? O10 N4 C33 116.8(6) . . ? C6 O2 C7 117.0(4) . . ? C27 O8 C28 112.9(4) . . ? C2 C1 N1 101.7(3) . . ? C2 C1 C5 113.0(4) . . ? N1 C1 C5 113.8(5) . . ? C2 C1 H1 118(2) . . ? N1 C1 H1 105(2) . . ? C5 C1 H1 105(2) . . ? C3 C2 C1 113.1(4) . . ? C3 C2 H2 123.4 . . ? C1 C2 H2 123.4 . . ? C2 C3 C6 127.1(4) . . ? C2 C3 C4 112.1(4) . . ? C6 C3 C4 120.8(4) . . ? N1 C4 C3 100.8(4) . . ? N1 C4 C9 112.5(4) . . ? C3 C4 C9 114.7(4) . . ? N1 C4 H3 110(2) . . ? C3 C4 H3 112(2) . . ? C9 C4 H3 107(2) . . ? C1 C5 H4 109(3) . . ? C1 C5 H5 107(3) . . ? H4 C5 H5 102(4) . . ? C1 C5 H6 111(3) . . ? H4 C5 H6 104(4) . . ? H5 C5 H6 123(4) . . ? O1 C6 O2 123.4(5) . . ? O1 C6 C3 124.6(4) . . ? O2 C6 C3 111.9(4) . . ? C8 C7 O2 106.0(10) . . ? C8 C7 H7 110.5 . . ? O2 C7 H7 110.5 . . ? C8 C7 H8 110.5 . . ? O2 C7 H8 110.5 . . ? H7 C7 H8 108.7 . . ? C7 C8 H9 109.4 . . ? C7 C8 H10 109.5 . . ? H9 C8 H10 109.5 . . ? C7 C8 H11 109.5 . . ? H9 C8 H11 109.5 . . ? H10 C8 H11 109.5 . . ? C14 C9 C10 119.2(5) . . ? C14 C9 C4 121.5(4) . . ? C10 C9 C4 119.3(4) . . ? C11 C10 C9 120.3(5) . . ? C11 C10 H12 119.9 . . ? C9 C10 H12 119.9 . . ? C12 C11 C10 118.6(5) . . ? C12 C11 H13 115(3) . . ? C10 C11 H13 126(3) . . ? C13 C12 C11 122.5(5) . . ? C13 C12 N2 118.7(5) . . ? C11 C12 N2 118.8(5) . . ? C12 C13 C14 119.0(5) . . ? C12 C13 H14 120.5 . . ? C14 C13 H14 120.5 . . ? C9 C14 C13 120.3(5) . . ? C9 C14 H15 119(3) . . ? C13 C14 H15 120(3) . . ? C20 C15 C16 120.2(4) . . ? C20 C15 S1 120.0(4) . . ? C16 C15 S1 119.8(4) . . ? C15 C16 C17 119.5(5) . . ? C15 C16 H16 119(3) . . ? C17 C16 H16 122(3) . . ? C16 C17 C18 122.0(5) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C19 C18 C17 117.0(5) . . ? C19 C18 C21 121.8(5) . . ? C17 C18 C21 121.2(5) . . ? C18 C19 C20 122.3(5) . . ? C18 C19 H18 118(3) . . ? C20 C19 H18 120(3) . . ? C15 C20 C19 118.9(5) . . ? C15 C20 H19 120.6 . . ? C19 C20 H19 120.6 . . ? C18 C21 H21 109.5 . . ? C18 C21 H20 109.5 . . ? H21 C21 H20 109.5 . . ? C18 C21 H22 109.5 . . ? H21 C21 H22 109.5 . . ? H20 C21 H22 109.5 . . ? N3 C22 C23 101.5(4) . . ? N3 C22 C26 113.4(4) . . ? C23 C22 C26 114.0(4) . . ? N3 C22 H23 112(2) . . ? C23 C22 H23 109(2) . . ? C26 C22 H23 106(2) . . ? C24 C23 C22 113.6(4) . . ? C24 C23 H24 123.2 . . ? C22 C23 H24 123.2 . . ? C23 C24 C27 126.7(4) . . ? C23 C24 C25 111.3(4) . . ? C27 C24 C25 122.0(4) . . ? N3 C25 C24 101.6(3) . . ? N3 C25 C30 111.5(3) . . ? C24 C25 C30 114.3(4) . . ? N3 C25 H25 108(2) . . ? C24 C25 H25 112(2) . . ? C30 C25 H25 109(2) . . ? C22 C26 H27 109.5 . . ? C22 C26 H26 109.5 . . ? H27 C26 H26 109.5 . . ? C22 C26 H28 109.5 . . ? H27 C26 H28 109.5 . . ? H26 C26 H28 109.5 . . ? O7 C27 O8 123.3(5) . . ? O7 C27 C24 124.1(5) . . ? O8 C27 C24 112.6(5) . . ? C29 C28 O8 103.0(10) . . ? C29 C28 H29 111.1 . . ? O8 C28 H29 111.2 . . ? C29 C28 H30 111.3 . . ? O8 C28 H30 111.2 . . ? H29 C28 H30 109.1 . . ? C28 C29 H33 109.3 . . ? C28 C29 H32 109.5 . . ? H33 C29 H32 109.5 . . ? C28 C29 H31 109.5 . . ? H33 C29 H31 109.5 . . ? H32 C29 H31 109.5 . . ? C35 C30 C31 117.8(4) . . ? C35 C30 C25 122.6(4) . . ? C31 C30 C25 119.6(4) . . ? C32 C31 C30 121.5(5) . . ? C32 C31 H34 119.2 . . ? C30 C31 H34 119.2 . . ? C31 C32 C33 118.5(5) . . ? C31 C32 H35 120.8 . . ? C33 C32 H35 120.8 . . ? C34 C33 C32 121.9(5) . . ? C34 C33 N4 118.6(5) . . ? C32 C33 N4 119.5(5) . . ? C33 C34 C35 119.0(5) . . ? C33 C34 H36 120.5 . . ? C35 C34 H36 120.5 . . ? C34 C35 C30 121.2(5) . . ? C34 C35 H37 119.4 . . ? C30 C35 H37 119.4 . . ? C37 C36 C41 120.4(4) . . ? C37 C36 S2 120.1(4) . . ? C41 C36 S2 119.5(4) . . ? C36 C37 C38 119.3(5) . . ? C36 C37 H38 120.4 . . ? C38 C37 H38 120.4 . . ? C39 C38 C37 122.4(5) . . ? C39 C38 H39 119(3) . . ? C37 C38 H39 119(3) . . ? C38 C39 C40 116.9(5) . . ? C38 C39 C42 121.8(5) . . ? C40 C39 C42 121.3(5) . . ? C39 C40 C41 122.1(5) . . ? C39 C40 H40 119.0 . . ? C41 C40 H40 119.0 . . ? C36 C41 C40 118.9(5) . . ? C36 C41 H41 120.5 . . ? C40 C41 H41 120.5 . . ? C39 C42 H42 109.5 . . ? C39 C42 H44 109.5 . . ? H42 C42 H44 109.5 . . ? C39 C42 H43 109.5 . . ? H42 C42 H43 109.5 . . ? H44 C42 H43 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 O6 S1 N1 C4 -35.9(4) . . . . ? O5 S1 N1 C4 -165.7(3) . . . . ? C15 S1 N1 C4 80.1(4) . . . . ? O6 S1 N1 C1 -174.0(3) . . . . ? O5 S1 N1 C1 56.2(3) . . . . ? C15 S1 N1 C1 -58.0(3) . . . . ? O11 S2 N3 C25 -167.4(3) . . . . ? O12 S2 N3 C25 -38.1(3) . . . . ? C36 S2 N3 C25 78.1(3) . . . . ? O11 S2 N3 C22 55.5(3) . . . . ? O12 S2 N3 C22 -175.2(3) . . . . ? C36 S2 N3 C22 -59.0(3) . . . . ? C4 N1 C1 C2 -8.2(5) . . . . ? S1 N1 C1 C2 132.8(3) . . . . ? C4 N1 C1 C5 113.6(5) . . . . ? S1 N1 C1 C5 -105.4(5) . . . . ? N1 C1 C2 C3 5.7(5) . . . . ? C5 C1 C2 C3 -116.7(5) . . . . ? C1 C2 C3 C6 -178.1(4) . . . . ? C1 C2 C3 C4 -1.3(5) . . . . ? C1 N1 C4 C3 7.5(4) . . . . ? S1 N1 C4 C3 -132.4(3) . . . . ? C1 N1 C4 C9 -115.1(4) . . . . ? S1 N1 C4 C9 105.0(4) . . . . ? C2 C3 C4 N1 -3.8(5) . . . . ? C6 C3 C4 N1 173.2(4) . . . . ? C2 C3 C4 C9 117.2(4) . . . . ? C6 C3 C4 C9 -65.7(6) . . . . ? C7 O2 C6 O1 -3.7(9) . . . . ? C7 O2 C6 C3 173.6(6) . . . . ? C2 C3 C6 O1 171.8(5) . . . . ? C4 C3 C6 O1 -4.7(8) . . . . ? C2 C3 C6 O2 -5.4(7) . . . . ? C4 C3 C6 O2 178.0(4) . . . . ? C6 O2 C7 C8 107.9(10) . . . . ? N1 C4 C9 C14 22.5(6) . . . . ? C3 C4 C9 C14 -91.9(5) . . . . ? N1 C4 C9 C10 -157.9(4) . . . . ? C3 C4 C9 C10 87.7(5) . . . . ? C14 C9 C10 C11 1.9(7) . . . . ? C4 C9 C10 C11 -177.7(4) . . . . ? C9 C10 C11 C12 -0.5(7) . . . . ? C10 C11 C12 C13 -0.8(8) . . . . ? C10 C11 C12 N2 177.9(4) . . . . ? O4 N2 C12 C13 176.4(5) . . . . ? O3 N2 C12 C13 -4.0(7) . . . . ? O4 N2 C12 C11 -2.4(7) . . . . ? O3 N2 C12 C11 177.2(5) . . . . ? C11 C12 C13 C14 0.7(7) . . . . ? N2 C12 C13 C14 -178.1(4) . . . . ? C10 C9 C14 C13 -2.1(7) . . . . ? C4 C9 C14 C13 177.5(4) . . . . ? C12 C13 C14 C9 0.8(7) . . . . ? O6 S1 C15 C20 36.0(4) . . . . ? O5 S1 C15 C20 168.8(4) . . . . ? N1 S1 C15 C20 -78.4(4) . . . . ? O6 S1 C15 C16 -145.3(4) . . . . ? O5 S1 C15 C16 -12.4(4) . . . . ? N1 S1 C15 C16 100.4(4) . . . . ? C20 C15 C16 C17 3.3(7) . . . . ? S1 C15 C16 C17 -175.5(4) . . . . ? C15 C16 C17 C18 -0.5(7) . . . . ? C16 C17 C18 C19 -2.6(8) . . . . ? C16 C17 C18 C21 177.8(5) . . . . ? C17 C18 C19 C20 2.9(8) . . . . ? C21 C18 C19 C20 -177.4(5) . . . . ? C16 C15 C20 C19 -2.9(7) . . . . ? S1 C15 C20 C19 175.8(4) . . . . ? C18 C19 C20 C15 -0.3(8) . . . . ? C25 N3 C22 C23 -8.0(5) . . . . ? S2 N3 C22 C23 132.2(3) . . . . ? C25 N3 C22 C26 114.7(4) . . . . ? S2 N3 C22 C26 -105.1(4) . . . . ? N3 C22 C23 C24 6.1(5) . . . . ? C26 C22 C23 C24 -116.2(5) . . . . ? C22 C23 C24 C27 -177.7(4) . . . . ? C22 C23 C24 C25 -1.9(6) . . . . ? C22 N3 C25 C24 7.1(4) . . . . ? S2 N3 C25 C24 -131.9(3) . . . . ? C22 N3 C25 C30 -115.1(4) . . . . ? S2 N3 C25 C30 105.9(4) . . . . ? C23 C24 C25 N3 -3.2(5) . . . . ? C27 C24 C25 N3 172.8(4) . . . . ? C23 C24 C25 C30 117.0(4) . . . . ? C27 C24 C25 C30 -66.9(5) . . . . ? C28 O8 C27 O7 -12.4(8) . . . . ? C28 O8 C27 C24 165.5(5) . . . . ? C23 C24 C27 O7 170.1(5) . . . . ? C25 C24 C27 O7 -5.3(7) . . . . ? C23 C24 C27 O8 -7.8(7) . . . . ? C25 C24 C27 O8 176.8(4) . . . . ? C27 O8 C28 C29 134.0(8) . . . . ? N3 C25 C30 C35 20.1(5) . . . . ? C24 C25 C30 C35 -94.5(5) . . . . ? N3 C25 C30 C31 -161.5(4) . . . . ? C24 C25 C30 C31 83.9(5) . . . . ? C35 C30 C31 C32 1.8(6) . . . . ? C25 C30 C31 C32 -176.7(4) . . . . ? C30 C31 C32 C33 0.1(7) . . . . ? C31 C32 C33 C34 -2.2(7) . . . . ? C31 C32 C33 N4 177.2(4) . . . . ? O9 N4 C33 C34 -2.1(7) . . . . ? O10 N4 C33 C34 176.8(5) . . . . ? O9 N4 C33 C32 178.4(5) . . . . ? O10 N4 C33 C32 -2.7(7) . . . . ? C32 C33 C34 C35 2.4(7) . . . . ? N4 C33 C34 C35 -177.0(4) . . . . ? C33 C34 C35 C30 -0.4(7) . . . . ? C31 C30 C35 C34 -1.6(6) . . . . ? C25 C30 C35 C34 176.8(4) . . . . ? O11 S2 C36 C37 -14.4(4) . . . . ? O12 S2 C36 C37 -146.8(4) . . . . ? N3 S2 C36 C37 99.0(4) . . . . ? O11 S2 C36 C41 166.3(3) . . . . ? O12 S2 C36 C41 33.9(4) . . . . ? N3 S2 C36 C41 -80.3(4) . . . . ? C41 C36 C37 C38 2.8(7) . . . . ? S2 C36 C37 C38 -176.5(4) . . . . ? C36 C37 C38 C39 -0.5(8) . . . . ? C37 C38 C39 C40 -1.1(8) . . . . ? C37 C38 C39 C42 177.6(5) . . . . ? C38 C39 C40 C41 0.6(8) . . . . ? C42 C39 C40 C41 -178.2(5) . . . . ? C37 C36 C41 C40 -3.3(7) . . . . ? S2 C36 C41 C40 176.0(4) . . . . ? C39 C40 C41 C36 1.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.669 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.057