data_mo_jsai_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H27 N O4 S2' _chemical_formula_weight 433.57 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' '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' 'N' 'N' 0.0061 0.0033 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4526(11) _cell_length_b 10.6473(10) _cell_length_c 16.4273(14) _cell_angle_alpha 90.00 _cell_angle_beta 101.465(3) _cell_angle_gamma 90.00 _cell_volume 2134.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6305 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 29.14 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.278 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9465 _exptl_absorpt_correction_T_max 0.9727 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith MicroMount' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Micorfocus source E025 IuS' _diffrn_source_type 'Bruker APEX DUO' _diffrn_source_power 50 _diffrn_source_current 0.6 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_radiation_monochromator 'Quazar MX Multilayer Optics' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'APEX DUO Kappa 4-axis goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 18870 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 29.56 _reflns_number_total 5338 _reflns_number_gt 4008 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2011.4-0' _computing_cell_refinement 'Bruker APEX2 v2011.4-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'Sir2011' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0580P)^2^+0.9358P] 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 5338 _refine_ls_number_parameters 312 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.001 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 N1 N 0.75382(10) 0.62903(12) 1.04234(9) 0.0276(3) Uani 1 1 d . . . O1 O 0.55341(9) 0.65752(12) 0.99738(8) 0.0350(3) Uani 1 1 d . . . O2 O 0.66537(9) 0.83157(11) 1.06945(8) 0.0323(3) Uani 1 1 d . . . O3 O 0.95321(9) 0.58444(11) 1.07504(7) 0.0315(3) Uani 1 1 d . . . O4 O 0.88222(10) 0.76633(11) 1.14202(7) 0.0322(3) Uani 1 1 d . . . S1 S 0.64115(3) 0.70082(4) 1.06083(3) 0.02631(10) Uani 1 1 d . . . S2 S 0.88113(3) 0.68972(4) 1.07071(3) 0.02592(10) Uani 1 1 d . . . C1 C 0.62230(11) 0.64039(15) 1.15613(11) 0.0258(3) Uani 1 1 d . . . C2 C 0.66080(12) 0.70573(15) 1.22923(11) 0.0265(4) Uani 1 1 d . . . H2 H 0.6989 0.7829 1.2283 0.032 Uiso 1 1 calc R . . C3 C 0.64295(12) 0.65704(16) 1.30334(11) 0.0291(4) Uani 1 1 d . . . H3 H 0.6680 0.7024 1.3533 0.035 Uiso 1 1 calc R . . C4 C 0.58913(12) 0.54318(16) 1.30648(11) 0.0300(4) Uani 1 1 d . . . C5 C 0.55333(13) 0.47830(16) 1.23237(12) 0.0336(4) Uani 1 1 d . . . H5 H 0.5180 0.3995 1.2336 0.040 Uiso 1 1 calc R . . C6 C 0.56814(12) 0.52624(16) 1.15698(11) 0.0305(4) Uani 1 1 d . . . H6 H 0.5418 0.4820 1.1068 0.037 Uiso 1 1 calc R . . C7 C 0.56832(15) 0.49246(19) 1.38747(12) 0.0401(5) Uani 1 1 d . . . H7A H 0.6250 0.5234 1.4332 0.060 Uiso 1 1 calc R . . H7B H 0.5703 0.4005 1.3864 0.060 Uiso 1 1 calc R . . H7C H 0.4962 0.5205 1.3955 0.060 Uiso 1 1 calc R . . C8 C 0.89655(12) 0.78303(15) 0.98633(10) 0.0253(3) Uani 1 1 d . . . C9 C 0.87004(12) 0.91005(15) 0.98562(11) 0.0283(4) Uani 1 1 d . . . H9 H 0.8459 0.9471 1.0314 0.034 Uiso 1 1 calc R . . C10 C 0.87939(13) 0.98127(15) 0.91712(11) 0.0296(4) Uani 1 1 d . . . H10 H 0.8621 1.0682 0.9165 0.035 Uiso 1 1 calc R . . C11 C 0.91344(13) 0.92885(16) 0.84901(11) 0.0291(4) Uani 1 1 d . . . C12 C 0.94073(13) 0.80140(16) 0.85181(11) 0.0293(4) Uani 1 1 d . . . H12 H 0.9651 0.7644 0.8061 0.035 Uiso 1 1 calc R . . C13 C 0.93292(12) 0.72823(16) 0.91968(11) 0.0284(4) Uani 1 1 d . . . H13 H 0.9521 0.6418 0.9210 0.034 Uiso 1 1 calc R . . C14 C 0.91679(16) 1.00740(17) 0.77355(12) 0.0378(4) Uani 1 1 d . . . H14A H 0.8427 1.0146 0.7398 0.057 Uiso 1 1 calc R . . H14B H 0.9650 0.9675 0.7407 0.057 Uiso 1 1 calc R . . H14C H 0.9448 1.0913 0.7909 0.057 Uiso 1 1 calc R . . C15 C 0.74496(13) 0.51040(15) 0.99848(11) 0.0303(4) Uani 1 1 d . . . C16 C 0.76135(15) 0.38775(16) 1.04401(12) 0.0362(4) Uani 1 1 d . B . H16A H 0.6976 0.3654 1.0688 0.043 Uiso 0.70 1 calc PR A 1 H16B H 0.8288 0.3877 1.0877 0.043 Uiso 0.70 1 calc PR A 1 H16C H 0.7161 0.3826 1.0848 0.043 Uiso 0.30 1 d PR A 2 H16D H 0.8366 0.3771 1.0710 0.043 Uiso 0.30 1 d PR A 2 C17 C 0.7718(2) 0.2997(3) 0.97004(19) 0.0349(7) Uani 0.70 1 d PU B 1 H17A H 0.8500 0.2850 0.9688 0.042 Uiso 0.70 1 calc PR B 1 H17B H 0.7367 0.2177 0.9760 0.042 Uiso 0.70 1 calc PR B 1 C18 C 0.7141(2) 0.3655(3) 0.88950(18) 0.0330(6) Uani 0.70 1 d PU B 1 H18A H 0.6362 0.3369 0.8753 0.040 Uiso 0.70 1 calc PR B 1 C19 C 0.7171(2) 0.5015(3) 0.9163(2) 0.0297(7) Uani 0.70 1 d PU B 1 H19 H 0.7012 0.5709 0.8796 0.036 Uiso 0.70 1 calc PR B 1 C20 C 0.7674(2) 0.3437(3) 0.81553(17) 0.0389(6) Uani 0.70 1 d P B 1 H20A H 0.8397 0.3861 0.8258 0.047 Uiso 0.70 1 calc PR B 1 H20B H 0.7804 0.2526 0.8106 0.047 Uiso 0.70 1 calc PR B 1 C17' C 0.7295(6) 0.2916(7) 0.9780(5) 0.0427(18) Uani 0.30 1 d PU B 2 H17C H 0.6503 0.2725 0.9694 0.051 Uiso 0.30 1 calc PR B 2 H17D H 0.7715 0.2130 0.9922 0.051 Uiso 0.30 1 calc PR B 2 C18' C 0.7584(6) 0.3537(7) 0.8991(5) 0.0349(15) Uani 0.30 1 d PU B 2 H18' H 0.8372 0.3370 0.8984 0.021(14) Uiso 0.30 1 calc PR B 2 C19' C 0.7454(7) 0.4917(10) 0.9206(7) 0.046(2) Uani 0.30 1 d PU B 2 H19' H 0.7382 0.5574 0.8807 0.055 Uiso 0.30 1 calc PR B 2 C20' C 0.6883(5) 0.3068(6) 0.8180(4) 0.0337(13) Uani 0.30 1 d P B 2 H20C H 0.6105 0.3080 0.8231 0.040 Uiso 0.30 1 calc PR B 2 H20D H 0.7083 0.2185 0.8093 0.040 Uiso 0.30 1 calc PR B 2 C21 C 0.70149(16) 0.3902(2) 0.73501(13) 0.0447(5) Uani 1 1 d . . . H21A H 0.6749 0.4731 0.7428 0.054 Uiso 0.70 1 d PR B 1 H21B H 0.6391 0.3363 0.7185 0.054 Uiso 0.70 1 d PR B 1 H21C H 0.6798 0.4756 0.7410 0.054 Uiso 0.30 1 d PR B 2 H21D H 0.6546 0.3554 0.6868 0.054 Uiso 0.30 1 d PR B 2 C22 C 0.7662(3) 0.3933(3) 0.6642(2) 0.0482(8) Uani 0.70 1 d P B 1 H22A H 0.8294 0.4493 0.6795 0.072 Uiso 0.70 1 calc PR B 1 H22B H 0.7186 0.4241 0.6133 0.072 Uiso 0.70 1 calc PR B 1 H22C H 0.7917 0.3084 0.6548 0.072 Uiso 0.70 1 calc PR B 1 C22' C 0.8107(7) 0.3868(9) 0.7235(6) 0.063(2) Uani 0.30 1 d P B 2 H22D H 0.8589 0.4248 0.7716 0.095 Uiso 0.30 1 calc PR B 2 H22E H 0.8164 0.4340 0.6733 0.095 Uiso 0.30 1 calc PR B 2 H22F H 0.8327 0.2995 0.7175 0.095 Uiso 0.30 1 calc PR B 2 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 N1 0.0222(6) 0.0250(6) 0.0354(8) -0.0080(6) 0.0054(5) 0.0000(5) O1 0.0261(5) 0.0432(7) 0.0323(7) -0.0048(6) -0.0025(5) 0.0040(5) O2 0.0355(6) 0.0252(6) 0.0365(7) -0.0003(5) 0.0080(5) 0.0052(5) O3 0.0257(5) 0.0341(6) 0.0332(7) 0.0017(5) 0.0026(5) 0.0068(5) O4 0.0339(6) 0.0340(6) 0.0274(7) -0.0059(5) 0.0031(5) -0.0014(5) S1 0.02188(17) 0.02662(19) 0.0294(2) -0.00291(16) 0.00255(15) 0.00349(14) S2 0.02217(17) 0.02810(19) 0.0263(2) -0.00268(16) 0.00204(15) 0.00141(14) C1 0.0166(6) 0.0272(8) 0.0328(9) -0.0021(7) 0.0027(6) 0.0030(6) C2 0.0208(6) 0.0239(7) 0.0333(9) -0.0018(7) 0.0022(6) -0.0002(6) C3 0.0246(7) 0.0296(8) 0.0309(9) -0.0035(7) 0.0004(7) -0.0016(6) C4 0.0218(7) 0.0335(9) 0.0336(10) 0.0030(7) 0.0031(7) -0.0003(6) C5 0.0254(7) 0.0318(9) 0.0431(11) -0.0023(8) 0.0054(7) -0.0078(6) C6 0.0216(7) 0.0321(8) 0.0366(10) -0.0087(7) 0.0027(7) -0.0043(6) C7 0.0343(9) 0.0448(10) 0.0393(11) 0.0053(9) 0.0030(8) -0.0078(8) C8 0.0188(6) 0.0284(8) 0.0270(9) -0.0031(6) 0.0001(6) -0.0003(6) C9 0.0242(7) 0.0279(8) 0.0314(9) -0.0075(7) 0.0020(6) -0.0013(6) C10 0.0292(7) 0.0227(8) 0.0347(10) -0.0046(7) 0.0013(7) -0.0014(6) C11 0.0239(7) 0.0301(8) 0.0311(9) -0.0026(7) -0.0001(6) -0.0037(6) C12 0.0269(7) 0.0325(8) 0.0284(9) -0.0049(7) 0.0055(7) 0.0000(6) C13 0.0243(7) 0.0275(8) 0.0328(9) -0.0041(7) 0.0043(7) 0.0031(6) C14 0.0435(9) 0.0321(9) 0.0364(10) -0.0006(8) 0.0048(8) -0.0070(8) C15 0.0268(7) 0.0254(8) 0.0387(10) -0.0071(7) 0.0067(7) -0.0005(6) C16 0.0379(9) 0.0284(8) 0.0428(11) -0.0022(8) 0.0097(8) 0.0039(7) C17 0.0374(12) 0.0260(11) 0.0395(14) -0.0044(10) 0.0029(11) 0.0038(10) C18 0.0284(11) 0.0288(11) 0.0395(14) -0.0050(10) 0.0013(11) 0.0041(10) C19 0.0294(12) 0.0227(11) 0.0343(14) -0.0051(10) 0.0001(11) -0.0001(10) C20 0.0376(13) 0.0343(13) 0.0417(16) -0.0131(12) 0.0002(12) 0.0073(11) C17' 0.043(3) 0.038(3) 0.048(3) -0.004(2) 0.012(2) -0.001(2) C18' 0.033(2) 0.034(2) 0.037(3) -0.0057(19) 0.005(2) 0.002(2) C19' 0.043(3) 0.046(3) 0.048(3) 0.001(2) 0.010(2) 0.001(2) C20' 0.028(3) 0.034(3) 0.038(3) -0.013(3) 0.005(2) -0.003(2) C21 0.0414(10) 0.0451(11) 0.0458(12) -0.0087(9) 0.0047(9) 0.0067(8) C22 0.0535(17) 0.0491(17) 0.0421(18) -0.0050(14) 0.0094(14) 0.0068(14) C22' 0.056(4) 0.081(6) 0.055(5) 0.015(4) 0.016(4) 0.001(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 N1 C15 1.447(2) . ? N1 S1 1.6776(13) . ? N1 S2 1.6895(13) . ? O1 S1 1.4283(12) . ? O2 S1 1.4255(12) . ? O3 S2 1.4290(12) . ? O4 S2 1.4253(12) . ? S1 C1 1.7510(18) . ? S2 C8 1.7467(17) . ? C1 C2 1.388(2) . ? C1 C6 1.391(2) . ? C2 C3 1.381(2) . ? C3 C4 1.391(2) . ? C4 C5 1.394(3) . ? C4 C7 1.505(3) . ? C5 C6 1.385(3) . ? C8 C9 1.392(2) . ? C8 C13 1.393(2) . ? C9 C10 1.381(2) . ? C10 C11 1.390(2) . ? C11 C12 1.397(2) . ? C11 C14 1.503(3) . ? C12 C13 1.379(2) . ? C15 C19' 1.296(11) . ? C15 C19 1.328(4) . ? C15 C16 1.499(2) . ? C16 C17' 1.487(8) . ? C16 C17 1.560(3) . ? C17 C18 1.543(4) . ? C18 C19 1.512(4) . ? C18 C20 1.514(4) . ? C20 C21 1.496(3) . ? C17' C18' 1.559(11) . ? C18' C20' 1.525(9) . ? C18' C19' 1.527(13) . ? C20' C21 1.661(7) . ? C21 C22' 1.411(8) . ? C21 C22 1.541(4) . ? 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 C15 N1 S1 120.27(10) . . ? C15 N1 S2 116.46(10) . . ? S1 N1 S2 123.26(8) . . ? O2 S1 O1 120.25(7) . . ? O2 S1 N1 107.15(7) . . ? O1 S1 N1 105.47(7) . . ? O2 S1 C1 109.47(8) . . ? O1 S1 C1 108.35(8) . . ? N1 S1 C1 105.07(7) . . ? O4 S2 O3 120.31(7) . . ? O4 S2 N1 107.50(7) . . ? O3 S2 N1 105.03(7) . . ? O4 S2 C8 110.00(8) . . ? O3 S2 C8 108.58(7) . . ? N1 S2 C8 104.11(7) . . ? C2 C1 C6 120.92(16) . . ? C2 C1 S1 120.31(12) . . ? C6 C1 S1 118.77(13) . . ? C3 C2 C1 119.08(15) . . ? C2 C3 C4 121.52(16) . . ? C3 C4 C5 118.19(16) . . ? C3 C4 C7 120.94(16) . . ? C5 C4 C7 120.86(16) . . ? C6 C5 C4 121.47(16) . . ? C5 C6 C1 118.80(16) . . ? C9 C8 C13 120.93(16) . . ? C9 C8 S2 119.75(13) . . ? C13 C8 S2 119.31(13) . . ? C10 C9 C8 118.84(16) . . ? C9 C10 C11 121.60(15) . . ? C10 C11 C12 118.34(16) . . ? C10 C11 C14 120.23(15) . . ? C12 C11 C14 121.40(16) . . ? C13 C12 C11 121.28(16) . . ? C12 C13 C8 119.00(15) . . ? C19' C15 C19 15.7(4) . . ? C19' C15 N1 127.6(5) . . ? C19 C15 N1 123.14(19) . . ? C19' C15 C16 109.4(5) . . ? C19 C15 C16 115.27(19) . . ? N1 C15 C16 121.51(16) . . ? C17' C16 C15 104.2(3) . . ? C17' C16 C17 21.5(3) . . ? C15 C16 C17 99.14(17) . . ? C18 C17 C16 107.4(2) . . ? C19 C18 C20 113.1(3) . . ? C19 C18 C17 101.8(2) . . ? C20 C18 C17 114.5(2) . . ? C15 C19 C18 110.6(3) . . ? C21 C20 C18 114.1(2) . . ? C16 C17' C18' 104.0(5) . . ? C20' C18' C19' 116.6(6) . . ? C20' C18' C17' 113.6(6) . . ? C19' C18' C17' 99.4(7) . . ? C15 C19' C18' 113.4(8) . . ? C18' C20' C21 114.2(5) . . ? C22' C21 C20 74.7(4) . . ? C22' C21 C22 40.2(4) . . ? C20 C21 C22 113.4(2) . . ? C22' C21 C20' 110.6(4) . . ? C20 C21 C20' 39.1(2) . . ? C22 C21 C20' 141.4(3) . . ? 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 C15 N1 S1 O2 -154.79(13) . . . . ? S2 N1 S1 O2 23.79(12) . . . . ? C15 N1 S1 O1 -25.56(15) . . . . ? S2 N1 S1 O1 153.02(10) . . . . ? C15 N1 S1 C1 88.82(14) . . . . ? S2 N1 S1 C1 -92.59(11) . . . . ? C15 N1 S2 O4 -153.16(12) . . . . ? S1 N1 S2 O4 28.20(12) . . . . ? C15 N1 S2 O3 -23.91(14) . . . . ? S1 N1 S2 O3 157.45(10) . . . . ? C15 N1 S2 C8 90.15(14) . . . . ? S1 N1 S2 C8 -88.49(11) . . . . ? O2 S1 C1 C2 -18.14(14) . . . . ? O1 S1 C1 C2 -151.01(12) . . . . ? N1 S1 C1 C2 96.64(13) . . . . ? O2 S1 C1 C6 161.79(12) . . . . ? O1 S1 C1 C6 28.93(14) . . . . ? N1 S1 C1 C6 -83.43(13) . . . . ? C6 C1 C2 C3 -1.2(2) . . . . ? S1 C1 C2 C3 178.77(11) . . . . ? C1 C2 C3 C4 1.2(2) . . . . ? C2 C3 C4 C5 0.1(2) . . . . ? C2 C3 C4 C7 -178.81(15) . . . . ? C3 C4 C5 C6 -1.5(2) . . . . ? C7 C4 C5 C6 177.45(16) . . . . ? C4 C5 C6 C1 1.5(2) . . . . ? C2 C1 C6 C5 -0.1(2) . . . . ? S1 C1 C6 C5 179.92(12) . . . . ? O4 S2 C8 C9 -22.18(14) . . . . ? O3 S2 C8 C9 -155.74(12) . . . . ? N1 S2 C8 C9 92.75(13) . . . . ? O4 S2 C8 C13 159.31(12) . . . . ? O3 S2 C8 C13 25.75(14) . . . . ? N1 S2 C8 C13 -85.76(13) . . . . ? C13 C8 C9 C10 0.6(2) . . . . ? S2 C8 C9 C10 -177.89(12) . . . . ? C8 C9 C10 C11 0.6(2) . . . . ? C9 C10 C11 C12 -1.4(2) . . . . ? C9 C10 C11 C14 176.62(15) . . . . ? C10 C11 C12 C13 0.9(2) . . . . ? C14 C11 C12 C13 -177.09(15) . . . . ? C11 C12 C13 C8 0.3(2) . . . . ? C9 C8 C13 C12 -1.1(2) . . . . ? S2 C8 C13 C12 177.43(12) . . . . ? S1 N1 C15 C19' 99.1(5) . . . . ? S2 N1 C15 C19' -79.6(5) . . . . ? S1 N1 C15 C19 80.6(2) . . . . ? S2 N1 C15 C19 -98.1(2) . . . . ? S1 N1 C15 C16 -96.17(17) . . . . ? S2 N1 C15 C16 85.15(18) . . . . ? C19' C15 C16 C17' -20.8(6) . . . . ? C19 C15 C16 C17' -5.0(4) . . . . ? N1 C15 C16 C17' 172.0(3) . . . . ? C19' C15 C16 C17 0.6(5) . . . . ? C19 C15 C16 C17 16.4(2) . . . . ? N1 C15 C16 C17 -166.61(17) . . . . ? C17' C16 C17 C18 82.4(10) . . . . ? C15 C16 C17 C18 -23.3(2) . . . . ? C16 C17 C18 C19 22.6(3) . . . . ? C16 C17 C18 C20 145.0(2) . . . . ? C19' C15 C19 C18 69(2) . . . . ? N1 C15 C19 C18 -179.56(18) . . . . ? C16 C15 C19 C18 -2.6(3) . . . . ? C20 C18 C19 C15 -136.1(2) . . . . ? C17 C18 C19 C15 -12.8(3) . . . . ? C19 C18 C20 C21 -73.3(3) . . . . ? C17 C18 C20 C21 170.7(2) . . . . ? C15 C16 C17' C18' 30.2(5) . . . . ? C17 C16 C17' C18' -48.5(8) . . . . ? C16 C17' C18' C20' -152.7(5) . . . . ? C16 C17' C18' C19' -28.0(7) . . . . ? C19 C15 C19' C18' -113(2) . . . . ? N1 C15 C19' C18' 168.0(4) . . . . ? C16 C15 C19' C18' 1.8(8) . . . . ? C20' C18' C19' C15 139.3(7) . . . . ? C17' C18' C19' C15 16.7(8) . . . . ? C19' C18' C20' C21 54.3(8) . . . . ? C17' C18' C20' C21 169.1(5) . . . . ? C18 C20 C21 C22' 156.6(5) . . . . ? C18 C20 C21 C22 167.7(2) . . . . ? C18 C20 C21 C20' -47.4(4) . . . . ? C18' C20' C21 C22' 60.7(7) . . . . ? C18' C20' C21 C20 36.1(4) . . . . ? C18' C20' C21 C22 93.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.407 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.057