data_cclk _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H26 N2 O6 S' _chemical_formula_weight 374.45 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' '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, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.5673(13) _cell_length_b 10.510(2) _cell_length_c 57.502(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3968.9(14) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6305 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 22.5 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.195 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9403 _exptl_absorpt_correction_T_max 0.9584 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-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_% 1 _diffrn_reflns_number 22659 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -61 _diffrn_reflns_limit_l_max 61 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5162 _reflns_number_gt 4898 _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, 1997)' _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^)+(0.0500P)^2^+16.0000P] 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 constr. _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(2) _refine_ls_number_reflns 5162 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.2174 _refine_ls_wR_factor_gt 0.2154 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.101 _refine_ls_shift/su_mean 0.013 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 S1A S 0.3287(3) 0.6660(2) 0.75463(4) 0.0398(5) Uani 1 1 d . . . O1A O 0.5442(8) 0.6905(6) 0.75570(12) 0.0566(17) Uani 1 1 d . . . O2A O 0.2571(10) 0.5374(5) 0.75508(11) 0.0524(16) Uani 1 1 d . . . O3A O 0.1761(14) 0.8535(9) 0.84819(15) 0.092(3) Uani 1 1 d . . . O4A O -0.1614(17) 0.8152(12) 0.84716(18) 0.123(4) Uani 1 1 d . . . O5A O 0.0805(10) 0.6300(6) 0.81131(10) 0.0553(17) Uani 1 1 d . . . O6A O -0.0217(10) 0.3764(7) 0.82916(12) 0.063(2) Uani 1 1 d . . . N1A N 0.2256(11) 0.7365(7) 0.77812(12) 0.0421(18) Uani 1 1 d . . . N2A N 0.2971(12) 0.4061(8) 0.84500(13) 0.055(2) Uani 1 1 d . . . H2AB H 0.2796 0.3556 0.8566 0.066 Uiso 1 1 calc R . . C1A C 0.3132(14) 0.8487(8) 0.78722(16) 0.047(2) Uani 1 1 d . . . H1AB H 0.4385 0.8748 0.7814 0.056 Uiso 1 1 calc R . . C2A C 0.2260(16) 0.9187(10) 0.80362(18) 0.058(3) Uani 1 1 d . . . H2AC H 0.2982 0.9860 0.8101 0.070 Uiso 1 1 calc R . . C3A C 0.0126(16) 0.8919(11) 0.81201(18) 0.066(3) Uani 1 1 d . . . H3AA H -0.0599 0.9732 0.8109 0.080 Uiso 1 1 calc R . . C4A C -0.0954(14) 0.8028(9) 0.79515(18) 0.058(3) Uani 1 1 d . . . H4AA H -0.1288 0.8486 0.7810 0.070 Uiso 1 1 calc R . . H4AB H -0.2216 0.7732 0.8021 0.070 Uiso 1 1 calc R . . C5A C 0.0407(13) 0.6876(9) 0.78920(16) 0.049(2) Uani 1 1 d . . . H5AA H -0.0307 0.6283 0.7789 0.058 Uiso 1 1 calc R . . C6A C 0.2252(13) 0.5269(8) 0.81168(16) 0.043(2) Uani 1 1 d . . . H6AA H 0.2374 0.4879 0.7963 0.052 Uiso 1 1 calc R . . C7A C 0.4367(15) 0.5672(9) 0.82102(16) 0.053(3) Uani 1 1 d . . . H7AA H 0.4323 0.6536 0.8269 0.063 Uiso 1 1 calc R . . H7AB H 0.5381 0.5627 0.8088 0.063 Uiso 1 1 calc R . . C8A C 0.4871(18) 0.4737(12) 0.8405(2) 0.085(4) Uani 1 1 d . . . H8AA H 0.5929 0.4150 0.8357 0.102 Uiso 1 1 calc R . . H8AB H 0.5325 0.5185 0.8543 0.102 Uiso 1 1 calc R . . C9A C 0.1543(15) 0.4304(9) 0.82936(15) 0.046(2) Uani 1 1 d . . . C10A C 0.2274(13) 0.7426(9) 0.72840(15) 0.042(2) Uani 1 1 d . . . C11A C -0.0009(14) 0.7145(10) 0.72671(18) 0.057(3) Uani 1 1 d . . . H11A H -0.0503 0.7404 0.7117 0.068 Uiso 1 1 calc R . . H11B H -0.0719 0.7605 0.7386 0.068 Uiso 1 1 calc R . . H11C H -0.0235 0.6249 0.7287 0.068 Uiso 1 1 calc R . . C12A C 0.2700(15) 0.8842(8) 0.72926(17) 0.051(2) Uani 1 1 d . . . H12A H 0.2347 0.9220 0.7146 0.061 Uiso 1 1 calc R . . H12B H 0.4119 0.8980 0.7323 0.061 Uiso 1 1 calc R . . H12C H 0.1902 0.9224 0.7414 0.061 Uiso 1 1 calc R . . C13A C 0.3458(16) 0.6836(9) 0.70781(16) 0.058(3) Uani 1 1 d . . . H13A H 0.3024 0.7226 0.6936 0.070 Uiso 1 1 calc R . . H13B H 0.3196 0.5938 0.7072 0.070 Uiso 1 1 calc R . . H13C H 0.4890 0.6978 0.7099 0.070 Uiso 1 1 calc R . . C14A C -0.004(2) 0.8526(13) 0.8373(2) 0.086(4) Uani 1 1 d . . . C15A C 0.180(3) 0.810(2) 0.8728(2) 0.147(8) Uani 1 1 d . . . H15A H 0.1235 0.8759 0.8826 0.176 Uiso 1 1 calc R . . H15B H 0.0952 0.7349 0.8743 0.176 Uiso 1 1 calc R . . C16A C 0.364(3) 0.783(2) 0.8800(3) 0.176(10) Uani 1 1 d . . . H16A H 0.3582 0.7116 0.8904 0.211 Uiso 1 1 calc R . . H16B H 0.4199 0.8551 0.8879 0.211 Uiso 1 1 calc R . . H16C H 0.4480 0.7619 0.8669 0.211 Uiso 1 1 calc R . . S1B S 0.1350(4) -0.1002(3) 0.95542(4) 0.0525(6) Uani 1 1 d . . . O1B O 0.0004(10) -0.1539(7) 0.97260(13) 0.074(2) Uani 1 1 d . . . O2B O 0.1135(12) -0.1336(7) 0.93095(11) 0.066(2) Uani 1 1 d . . . O3B O -0.013(2) 0.4771(9) 0.9347(2) 0.129(4) Uani 1 1 d . . . O4B O -0.252(2) 0.4008(14) 0.9588(2) 0.144(5) Uani 1 1 d . . . O5B O -0.0500(10) 0.1656(7) 0.92563(10) 0.0578(18) Uani 1 1 d . . . O6B O 0.1990(11) 0.2271(8) 0.88326(13) 0.076(2) Uani 1 1 d . . . N1B N 0.1056(13) 0.0541(8) 0.95653(13) 0.061(2) Uani 1 1 d . . . N2B N -0.1142(13) 0.2019(8) 0.86638(13) 0.064(3) Uani 1 1 d . . . H2BB H -0.0843 0.2413 0.8537 0.077 Uiso 1 1 calc R . . C1B C 0.041(2) 0.1104(14) 0.9775(2) 0.085(4) Uani 1 1 d . . . H1BB H 0.0037 0.0577 0.9898 0.102 Uiso 1 1 calc R . . C2B C 0.032(3) 0.2379(16) 0.9806(2) 0.109(5) Uani 1 1 d . . . H2BC H -0.0198 0.2682 0.9946 0.131 Uiso 1 1 calc R . . C3B C 0.100(2) 0.3328(13) 0.96292(19) 0.084(4) Uani 1 1 d . . . H3BA H 0.1855 0.3959 0.9708 0.100 Uiso 1 1 calc R . . C4B C 0.2368(17) 0.2603(11) 0.94453(19) 0.070(3) Uani 1 1 d . . . H4BA H 0.2590 0.3148 0.9312 0.084 Uiso 1 1 calc R . . H4BB H 0.3683 0.2416 0.9514 0.084 Uiso 1 1 calc R . . C5B C 0.1402(16) 0.1400(9) 0.93682(15) 0.055(3) Uani 1 1 d . . . H5BA H 0.2308 0.0979 0.9257 0.066 Uiso 1 1 calc R . . C6B C -0.0789(15) 0.1131(11) 0.90308(15) 0.057(3) Uani 1 1 d . . . H6BA H -0.0350 0.0240 0.9027 0.069 Uiso 1 1 calc R . . C7B C -0.3117(17) 0.1244(12) 0.89684(17) 0.071(3) Uani 1 1 d . . . H7BA H -0.3840 0.0470 0.9009 0.086 Uiso 1 1 calc R . . H7BB H -0.3739 0.1955 0.9049 0.086 Uiso 1 1 calc R . . C8B C -0.3136(16) 0.1460(12) 0.87041(19) 0.075(3) Uani 1 1 d . . . H8BA H -0.3291 0.0665 0.8620 0.090 Uiso 1 1 calc R . . H8BB H -0.4218 0.2038 0.8659 0.090 Uiso 1 1 calc R . . C9B C 0.0213(15) 0.1876(10) 0.88397(15) 0.051(2) Uani 1 1 d . . . C10B C 0.3940(15) -0.1386(10) 0.96454(17) 0.060(3) Uani 1 1 d . . . C11B C 0.5349(17) -0.0772(15) 0.9467(2) 0.107(5) Uani 1 1 d . . . H11D H 0.6661 -0.1173 0.9473 0.128 Uiso 1 1 calc R . . H11E H 0.5490 0.0118 0.9501 0.128 Uiso 1 1 calc R . . H11F H 0.4783 -0.0875 0.9314 0.128 Uiso 1 1 calc R . . C12B C 0.409(2) -0.2856(12) 0.9641(2) 0.099(5) Uani 1 1 d . . . H12D H 0.5489 -0.3108 0.9651 0.119 Uiso 1 1 calc R . . H12E H 0.3517 -0.3169 0.9498 0.119 Uiso 1 1 calc R . . H12F H 0.3345 -0.3202 0.9770 0.119 Uiso 1 1 calc R . . C13B C 0.431(2) -0.0918(14) 0.9891(2) 0.101(5) Uani 1 1 d . . . H13D H 0.5721 -0.1035 0.9930 0.122 Uiso 1 1 calc R . . H13E H 0.3479 -0.1393 0.9997 0.122 Uiso 1 1 calc R . . H13F H 0.3972 -0.0032 0.9901 0.122 Uiso 1 1 calc R . . C14B C -0.073(3) 0.4003(16) 0.9523(3) 0.103(5) Uani 1 1 d . . . C15B C -0.171(4) 0.5603(18) 0.9235(4) 0.169(10) Uani 1 1 d . . . H15C H -0.2958 0.5570 0.9324 0.202 Uiso 1 1 calc R . . H15D H -0.1234 0.6477 0.9232 0.202 Uiso 1 1 calc R . . C16B C -0.205(5) 0.522(3) 0.9022(5) 0.267(19) Uani 1 1 d . . . H16D H -0.3328 0.5555 0.8969 0.321 Uiso 1 1 calc R . . H16E H -0.2108 0.4303 0.9019 0.321 Uiso 1 1 calc R . . H16F H -0.0978 0.5504 0.8922 0.321 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 S1A 0.0336(11) 0.0345(11) 0.0513(13) 0.0067(10) -0.0008(10) 0.0015(10) O1A 0.028(3) 0.064(4) 0.078(4) 0.006(4) 0.005(3) 0.011(3) O2A 0.059(4) 0.038(3) 0.060(4) 0.003(3) -0.009(3) -0.001(3) O3A 0.076(6) 0.111(7) 0.091(6) -0.004(5) 0.013(5) 0.031(6) O4A 0.090(7) 0.165(10) 0.114(7) 0.010(7) 0.037(7) 0.023(8) O5A 0.055(4) 0.050(4) 0.061(4) 0.016(3) 0.015(3) 0.010(3) O6A 0.053(5) 0.063(5) 0.073(5) 0.031(4) -0.005(3) -0.013(4) N1A 0.034(4) 0.037(4) 0.055(5) 0.005(3) -0.003(3) -0.014(3) N2A 0.046(5) 0.067(5) 0.051(5) 0.018(4) -0.013(4) -0.003(4) C1A 0.036(5) 0.037(5) 0.067(6) 0.010(5) -0.009(5) -0.002(4) C2A 0.059(7) 0.045(6) 0.070(7) -0.007(5) -0.011(5) -0.004(5) C3A 0.056(7) 0.062(7) 0.080(7) 0.008(6) 0.000(6) 0.026(6) C4A 0.033(5) 0.059(6) 0.081(7) 0.010(5) 0.008(5) -0.001(5) C5A 0.036(5) 0.049(6) 0.061(6) 0.018(5) 0.002(4) -0.002(5) C6A 0.043(5) 0.036(5) 0.050(5) 0.003(4) -0.002(4) -0.001(4) C7A 0.048(6) 0.055(6) 0.055(6) 0.008(5) 0.001(5) -0.004(5) C8A 0.056(7) 0.086(9) 0.113(10) 0.030(8) -0.013(7) -0.025(7) C9A 0.040(5) 0.054(6) 0.043(5) 0.007(4) 0.004(5) -0.003(5) C10A 0.028(5) 0.054(6) 0.044(5) -0.001(4) 0.007(4) -0.012(4) C11A 0.040(6) 0.058(6) 0.071(7) -0.002(5) -0.008(5) -0.007(5) C12A 0.063(6) 0.021(4) 0.069(6) 0.009(4) -0.001(5) 0.003(4) C13A 0.062(6) 0.046(6) 0.067(6) 0.008(5) 0.003(5) -0.009(5) C14A 0.082(10) 0.089(10) 0.085(9) 0.022(7) 0.024(8) 0.042(8) C15A 0.146(16) 0.24(2) 0.049(8) 0.021(11) 0.005(10) 0.084(17) C16A 0.154(18) 0.31(3) 0.059(9) -0.003(13) 0.005(11) 0.07(2) S1B 0.0370(13) 0.0666(16) 0.0539(14) 0.0209(13) -0.0028(11) 0.0010(13) O1B 0.055(5) 0.074(5) 0.094(6) 0.042(4) 0.010(4) -0.005(4) O2B 0.074(5) 0.068(5) 0.056(4) 0.011(3) -0.013(4) 0.004(4) O3B 0.180(12) 0.083(7) 0.126(8) 0.035(6) 0.010(8) 0.047(7) O4B 0.133(10) 0.171(12) 0.127(9) 0.018(9) 0.014(8) 0.077(10) O5B 0.048(4) 0.080(5) 0.046(4) 0.019(3) -0.005(3) 0.016(4) O6B 0.041(5) 0.112(6) 0.075(5) 0.047(4) -0.017(4) -0.019(4) N1B 0.068(6) 0.067(5) 0.047(4) 0.018(4) 0.008(5) 0.014(5) N2B 0.056(5) 0.088(7) 0.048(5) 0.034(4) 0.010(4) -0.011(5) C1B 0.098(10) 0.092(10) 0.066(7) 0.000(7) 0.030(7) 0.011(9) C2B 0.138(15) 0.122(13) 0.068(8) -0.025(9) 0.026(9) 0.018(11) C3B 0.108(11) 0.086(9) 0.056(7) -0.013(6) -0.019(7) -0.007(9) C4B 0.063(7) 0.079(8) 0.067(7) 0.019(6) -0.002(6) 0.003(6) C5B 0.063(7) 0.050(6) 0.051(5) 0.006(4) 0.023(5) -0.005(5) C6B 0.056(6) 0.080(7) 0.037(5) 0.032(5) -0.003(4) 0.004(6) C7B 0.062(7) 0.090(8) 0.063(7) 0.020(6) -0.014(6) -0.022(7) C8B 0.049(6) 0.086(8) 0.090(8) 0.033(7) 0.003(6) -0.017(6) C9B 0.047(6) 0.063(6) 0.043(5) 0.015(5) -0.003(5) 0.007(5) C10B 0.050(6) 0.068(7) 0.062(6) 0.032(5) -0.002(5) -0.001(5) C11B 0.041(6) 0.166(15) 0.115(11) 0.070(10) 0.002(7) 0.017(8) C12B 0.101(11) 0.104(11) 0.092(9) 0.032(8) -0.002(8) 0.021(9) C13B 0.101(10) 0.107(11) 0.097(10) 0.026(8) -0.053(8) -0.014(9) C14B 0.128(13) 0.106(12) 0.074(9) -0.020(9) -0.032(10) 0.017(12) C15B 0.22(2) 0.115(14) 0.168(18) -0.026(13) -0.080(19) 0.086(16) C16B 0.31(4) 0.21(3) 0.28(3) -0.05(2) -0.16(3) 0.15(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 S1A O2A 1.431(6) . ? S1A O1A 1.440(6) . ? S1A N1A 1.682(8) . ? S1A C10A 1.835(9) . ? O3A C14A 1.338(16) . ? O3A C15A 1.487(15) . ? O4A C14A 1.240(16) . ? O5A C5A 1.432(10) . ? O5A C6A 1.442(10) . ? O6A C9A 1.288(11) . ? N1A C1A 1.412(11) . ? N1A C5A 1.465(11) . ? N2A C9A 1.324(11) . ? N2A C8A 1.459(13) . ? C1A C2A 1.326(13) . ? C2A C3A 1.509(15) . ? C3A C4A 1.523(15) . ? C3A C14A 1.519(15) . ? C4A C5A 1.544(13) . ? C6A C9A 1.509(12) . ? C6A C7A 1.548(12) . ? C7A C8A 1.526(14) . ? C10A C12A 1.516(12) . ? C10A C13A 1.546(13) . ? C10A C11A 1.531(12) . ? C15A C16A 1.30(2) . ? S1B O1B 1.441(7) . ? S1B O2B 1.457(7) . ? S1B N1B 1.634(9) . ? S1B C10B 1.825(10) . ? O3B C14B 1.354(19) . ? O3B C15B 1.50(2) . ? O4B C14B 1.238(19) . ? O5B C6B 1.422(11) . ? O5B C5B 1.430(12) . ? O6B C9B 1.239(12) . ? N1B C1B 1.409(13) . ? N1B C5B 1.467(11) . ? N2B C9B 1.355(12) . ? N2B C8B 1.454(14) . ? C1B C2B 1.353(18) . ? C2B C3B 1.494(19) . ? C3B C14B 1.47(2) . ? C3B C4B 1.584(16) . ? C4B C5B 1.482(15) . ? C6B C9B 1.501(13) . ? C6B C7B 1.575(15) . ? C7B C8B 1.537(14) . ? C10B C13B 1.512(15) . ? C10B C11B 1.525(14) . ? C10B C12B 1.549(16) . ? C15B C16B 1.31(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 O2A S1A O1A 119.4(4) . . ? O2A S1A N1A 105.6(4) . . ? O1A S1A N1A 106.4(4) . . ? O2A S1A C10A 108.0(4) . . ? O1A S1A C10A 108.2(4) . . ? N1A S1A C10A 108.7(4) . . ? C14A O3A C15A 117.2(12) . . ? C5A O5A C6A 116.8(7) . . ? C1A N1A C5A 118.0(8) . . ? C1A N1A S1A 120.1(6) . . ? C5A N1A S1A 121.9(6) . . ? C9A N2A C8A 113.0(8) . . ? C2A C1A N1A 123.4(9) . . ? C1A C2A C3A 121.7(10) . . ? C4A C3A C2A 110.1(9) . . ? C4A C3A C14A 114.2(11) . . ? C2A C3A C14A 115.1(10) . . ? C3A C4A C5A 110.7(8) . . ? O5A C5A N1A 112.5(7) . . ? O5A C5A C4A 103.9(7) . . ? N1A C5A C4A 107.5(7) . . ? O5A C6A C9A 108.2(7) . . ? O5A C6A C7A 113.0(7) . . ? C9A C6A C7A 103.1(7) . . ? C6A C7A C8A 105.8(8) . . ? N2A C8A C7A 105.0(8) . . ? O6A C9A N2A 123.8(8) . . ? O6A C9A C6A 124.5(8) . . ? N2A C9A C6A 111.6(8) . . ? C12A C10A C13A 109.0(7) . . ? C12A C10A C11A 111.9(8) . . ? C13A C10A C11A 111.5(8) . . ? C12A C10A S1A 109.7(6) . . ? C13A C10A S1A 105.7(6) . . ? C11A C10A S1A 108.8(7) . . ? O4A C14A O3A 121.8(12) . . ? O4A C14A C3A 125.6(14) . . ? O3A C14A C3A 112.4(11) . . ? C16A C15A O3A 112.7(16) . . ? O1B S1B O2B 120.5(5) . . ? O1B S1B N1B 106.8(5) . . ? O2B S1B N1B 105.4(4) . . ? O1B S1B C10B 106.8(4) . . ? O2B S1B C10B 108.3(5) . . ? N1B S1B C10B 108.6(5) . . ? C14B O3B C15B 117.9(17) . . ? C6B O5B C5B 117.0(7) . . ? C1B N1B C5B 116.7(9) . . ? C1B N1B S1B 119.1(8) . . ? C5B N1B S1B 124.3(6) . . ? C9B N2B C8B 115.3(8) . . ? C2B C1B N1B 122.9(12) . . ? C1B C2B C3B 123.9(12) . . ? C14B C3B C2B 112.0(14) . . ? C14B C3B C4B 113.1(10) . . ? C2B C3B C4B 107.7(11) . . ? C5B C4B C3B 111.6(10) . . ? O5B C5B N1B 109.1(8) . . ? O5B C5B C4B 110.4(8) . . ? N1B C5B C4B 111.1(8) . . ? O5B C6B C9B 114.0(9) . . ? O5B C6B C7B 107.9(8) . . ? C9B C6B C7B 102.7(7) . . ? C8B C7B C6B 104.1(9) . . ? N2B C8B C7B 102.1(9) . . ? O6B C9B N2B 123.8(9) . . ? O6B C9B C6B 127.7(9) . . ? N2B C9B C6B 108.4(8) . . ? C13B C10B C11B 113.1(11) . . ? C13B C10B C12B 109.3(9) . . ? C11B C10B C12B 111.9(11) . . ? C13B C10B S1B 110.3(8) . . ? C11B C10B S1B 106.2(7) . . ? C12B C10B S1B 105.9(8) . . ? O4B C14B O3B 120.1(16) . . ? O4B C14B C3B 127.6(17) . . ? O3B C14B C3B 112.0(17) . . ? C16B C15B O3B 109.8(17) . . ? 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 O2A S1A N1A C1A 159.5(6) . . . . ? O1A S1A N1A C1A 31.6(7) . . . . ? C10A S1A N1A C1A -84.8(7) . . . . ? O2A S1A N1A C5A -22.8(7) . . . . ? O1A S1A N1A C5A -150.7(6) . . . . ? C10A S1A N1A C5A 92.9(7) . . . . ? C5A N1A C1A C2A -7.1(12) . . . . ? S1A N1A C1A C2A 170.7(8) . . . . ? N1A C1A C2A C3A -7.2(15) . . . . ? C1A C2A C3A C4A -14.7(13) . . . . ? C1A C2A C3A C14A 116.1(12) . . . . ? C2A C3A C4A C5A 48.3(11) . . . . ? C14A C3A C4A C5A -83.0(11) . . . . ? C6A O5A C5A N1A -57.0(10) . . . . ? C6A O5A C5A C4A -173.0(7) . . . . ? C1A N1A C5A O5A -73.6(10) . . . . ? S1A N1A C5A O5A 108.6(8) . . . . ? C1A N1A C5A C4A 40.2(10) . . . . ? S1A N1A C5A C4A -137.5(7) . . . . ? C3A C4A C5A O5A 58.4(10) . . . . ? C3A C4A C5A N1A -61.0(10) . . . . ? C5A O5A C6A C9A -143.9(8) . . . . ? C5A O5A C6A C7A 102.6(9) . . . . ? O5A C6A C7A C8A 126.9(9) . . . . ? C9A C6A C7A C8A 10.4(10) . . . . ? C9A N2A C8A C7A 9.4(14) . . . . ? C6A C7A C8A N2A -11.9(12) . . . . ? C8A N2A C9A O6A 176.3(10) . . . . ? C8A N2A C9A C6A -2.6(12) . . . . ? O5A C6A C9A O6A 56.0(12) . . . . ? C7A C6A C9A O6A 176.0(9) . . . . ? O5A C6A C9A N2A -125.1(8) . . . . ? C7A C6A C9A N2A -5.1(10) . . . . ? O2A S1A C10A C12A 170.6(6) . . . . ? O1A S1A C10A C12A -58.7(7) . . . . ? N1A S1A C10A C12A 56.5(7) . . . . ? O2A S1A C10A C13A -72.0(7) . . . . ? O1A S1A C10A C13A 58.7(7) . . . . ? N1A S1A C10A C13A 173.9(6) . . . . ? O2A S1A C10A C11A 47.9(8) . . . . ? O1A S1A C10A C11A 178.6(7) . . . . ? N1A S1A C10A C11A -66.2(7) . . . . ? C15A O3A C14A O4A -1(2) . . . . ? C15A O3A C14A C3A -176.8(12) . . . . ? C4A C3A C14A O4A -44.2(17) . . . . ? C2A C3A C14A O4A -173.0(13) . . . . ? C4A C3A C14A O3A 131.3(11) . . . . ? C2A C3A C14A O3A 2.5(16) . . . . ? C14A O3A C15A C16A 163(2) . . . . ? O1B S1B N1B C1B 26.8(10) . . . . ? O2B S1B N1B C1B 156.1(9) . . . . ? C10B S1B N1B C1B -88.0(10) . . . . ? O1B S1B N1B C5B -152.7(8) . . . . ? O2B S1B N1B C5B -23.4(10) . . . . ? C10B S1B N1B C5B 92.5(9) . . . . ? C5B N1B C1B C2B -7(2) . . . . ? S1B N1B C1B C2B 173.4(13) . . . . ? N1B C1B C2B C3B -4(3) . . . . ? C1B C2B C3B C14B 108.8(18) . . . . ? C1B C2B C3B C4B -16(2) . . . . ? C14B C3B C4B C5B -77.4(15) . . . . ? C2B C3B C4B C5B 47.0(13) . . . . ? C6B O5B C5B N1B -110.6(8) . . . . ? C6B O5B C5B C4B 127.0(9) . . . . ? C1B N1B C5B O5B -83.0(11) . . . . ? S1B N1B C5B O5B 96.5(9) . . . . ? C1B N1B C5B C4B 38.9(13) . . . . ? S1B N1B C5B C4B -141.6(8) . . . . ? C3B C4B C5B O5B 61.7(10) . . . . ? C3B C4B C5B N1B -59.5(12) . . . . ? C5B O5B C6B C9B -80.1(10) . . . . ? C5B O5B C6B C7B 166.5(8) . . . . ? O5B C6B C7B C8B 146.6(9) . . . . ? C9B C6B C7B C8B 25.9(12) . . . . ? C9B N2B C8B C7B 16.0(13) . . . . ? C6B C7B C8B N2B -25.0(12) . . . . ? C8B N2B C9B O6B 178.5(11) . . . . ? C8B N2B C9B C6B 0.9(13) . . . . ? O5B C6B C9B O6B 49.0(15) . . . . ? C7B C6B C9B O6B 165.5(12) . . . . ? O5B C6B C9B N2B -133.5(9) . . . . ? C7B C6B C9B N2B -17.0(12) . . . . ? O1B S1B C10B C13B -55.2(9) . . . . ? O2B S1B C10B C13B 173.6(8) . . . . ? N1B S1B C10B C13B 59.6(9) . . . . ? O1B S1B C10B C11B -178.1(9) . . . . ? O2B S1B C10B C11B 50.7(10) . . . . ? N1B S1B C10B C11B -63.2(10) . . . . ? O1B S1B C10B C12B 62.9(8) . . . . ? O2B S1B C10B C12B -68.3(8) . . . . ? N1B S1B C10B C12B 177.7(7) . . . . ? C15B O3B C14B O4B 0(2) . . . . ? C15B O3B C14B C3B -174.9(13) . . . . ? C2B C3B C14B O4B 12(2) . . . . ? C4B C3B C14B O4B 134.0(18) . . . . ? C2B C3B C14B O3B -173.9(11) . . . . ? C4B C3B C14B O3B -52.0(17) . . . . ? C14B O3B C15B C16B -112(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.524 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.095