data_sa2888 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H31 N O4 S2' _chemical_formula_sum 'C37 H31 N O4 S2' _chemical_formula_weight 617.75 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 17.041(5) _cell_length_b 9.345(3) _cell_length_c 19.211(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.886(4) _cell_angle_gamma 90.00 _cell_volume 3004.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6709 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.48 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6046 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18100 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5260 _reflns_number_gt 4327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'Olex2 ver 1.1' _computing_molecular_graphics 'Olex2 ver 1.1' _computing_publication_material 'SHELX97 (Sheldrick, 2008)' _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^)+(0.0566P)^2^+4.6185P] 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_number_reflns 5260 _refine_ls_number_parameters 420 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.1741 _refine_ls_wR_factor_gt 0.1621 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.003 _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 0.98400(19) 0.6251(6) 0.0800(2) 0.0466(8) Uani 0.599(5) 1 d PDU A 1 S2 S 1.33806(6) -0.35585(12) 0.70533(7) 0.0483(3) Uani 1 1 d . . . O1 O 0.73723(15) 0.5621(3) 0.50139(15) 0.0434(7) Uani 1 1 d . . . O2 O 0.79823(16) 0.2165(3) 0.67208(14) 0.0440(7) Uani 1 1 d . . . O3 O 1.14046(14) 0.3541(3) 0.28916(14) 0.0375(7) Uani 1 1 d . . . O4 O 1.24993(15) -0.0318(3) 0.54260(15) 0.0409(7) Uani 1 1 d . . . N1 N 0.75037(18) 0.3964(3) 0.59264(17) 0.0348(8) Uani 1 1 d . . . C1 C 0.7719(2) 0.4627(4) 0.5336(2) 0.0330(9) Uani 1 1 d . . . C2 C 0.8454(2) 0.3864(4) 0.52209(19) 0.0290(8) Uani 1 1 d . . . C3 C 0.8655(2) 0.2861(4) 0.57522(18) 0.0280(8) Uani 1 1 d . . . C4 C 0.8036(2) 0.2894(4) 0.6207(2) 0.0323(9) Uani 1 1 d . . . C5 C 0.89126(19) 0.4040(4) 0.47122(18) 0.0251(8) Uani 1 1 d . . . C6 C 0.96280(19) 0.3224(4) 0.47371(18) 0.0240(8) Uani 1 1 d . . . C7 C 0.99454(19) 0.3657(4) 0.40959(18) 0.0234(7) Uani 1 1 d . . . C8 C 0.9421(2) 0.4656(4) 0.37130(19) 0.0268(8) Uani 1 1 d . . . C9 C 0.8747(2) 0.5007(4) 0.40873(19) 0.0288(8) Uani 1 1 d . . . H9A H 0.8762 0.6024 0.4233 0.035 Uiso 1 1 calc R . . H9B H 0.8222 0.4796 0.3785 0.035 Uiso 1 1 calc R . . C10 C 0.9540(2) 0.5194(4) 0.3072(2) 0.0303(8) Uani 1 1 d . . . H10 H 0.9165 0.5851 0.2821 0.036 Uiso 1 1 calc R . . C11 C 1.0197(2) 0.4795(4) 0.27870(19) 0.0270(8) Uani 1 1 d . . . C12 C 1.0748(2) 0.3839(4) 0.31870(19) 0.0283(8) Uani 1 1 d . . . C13 C 1.0622(2) 0.3262(4) 0.38215(19) 0.0283(8) Uani 1 1 d . . . H13 H 1.0994 0.2597 0.4071 0.034 Uiso 1 1 calc R . . C14 C 1.0279(2) 0.5353(4) 0.2083(2) 0.0320(9) Uani 1 1 d . A . C15 C 0.9621(2) 0.5541(5) 0.1549(2) 0.0417(10) Uani 1 1 d D . . H15 H 0.9093 0.5293 0.1598 0.050 Uiso 0.599(5) 1 calc PR A 1 H15A H 0.9093 0.5267 0.1585 0.050 Uiso 0.401(5) 1 calc PR A 2 C16 C 1.0852(8) 0.640(3) 0.1217(7) 0.033(3) Uani 0.599(5) 1 d PDU A 1 H16 H 1.1256 0.6830 0.1007 0.040 Uiso 0.599(5) 1 calc PR A 1 C17 C 1.0979(2) 0.5814(5) 0.1883(2) 0.0472(11) Uani 1 1 d D . . H17 H 1.1493 0.5732 0.2177 0.057 Uiso 0.599(5) 1 calc PR A 1 H17A H 1.1486 0.5779 0.2191 0.057 Uiso 0.401(5) 1 calc PR A 2 C18 C 1.1957(2) 0.2499(4) 0.3223(2) 0.0367(9) Uani 1 1 d . . . H18A H 1.2172 0.2792 0.3711 0.055 Uiso 1 1 calc R . . H18B H 1.2395 0.2410 0.2961 0.055 Uiso 1 1 calc R . . H18C H 1.1686 0.1575 0.3225 0.055 Uiso 1 1 calc R . . C19 C 0.98509(19) 0.2239(4) 0.52970(18) 0.0235(7) Uani 1 1 d . . . C20 C 0.9335(2) 0.2055(4) 0.57954(18) 0.0264(8) Uani 1 1 d . . . C21 C 0.9641(2) 0.0939(4) 0.63406(19) 0.0311(8) Uani 1 1 d . . . H21A H 0.9746 0.1350 0.6824 0.037 Uiso 1 1 calc R . . H21B H 0.9261 0.0134 0.6322 0.037 Uiso 1 1 calc R . . C22 C 1.0397(2) 0.0476(4) 0.61221(18) 0.0268(8) Uani 1 1 d . . . C23 C 1.0536(2) 0.1249(4) 0.55275(18) 0.0256(8) Uani 1 1 d . . . C24 C 1.1251(2) 0.0991(4) 0.52883(19) 0.0270(8) Uani 1 1 d . . . H24 H 1.1370 0.1511 0.4896 0.032 Uiso 1 1 calc R . . C25 C 1.1786(2) -0.0030(4) 0.56270(19) 0.0294(8) Uani 1 1 d . . . C26 C 1.1641(2) -0.0811(4) 0.62178(19) 0.0274(8) Uani 1 1 d . . . C27 C 1.0929(2) -0.0537(4) 0.64443(19) 0.0287(8) Uani 1 1 d . . . H27 H 1.0806 -0.1064 0.6833 0.034 Uiso 1 1 calc R . . C28 C 1.2232(2) -0.1804(4) 0.6631(2) 0.0311(9) Uani 1 1 d . . . C29 C 1.2227(3) -0.2144(4) 0.7355(2) 0.0445(11) Uani 1 1 d . . . H29 H 1.1847 -0.1757 0.7607 0.053 Uiso 1 1 calc R . . C30 C 1.2811(3) -0.3066(4) 0.7652(2) 0.0491(11) Uani 1 1 d . . . H30 H 1.2890 -0.3392 0.8129 0.059 Uiso 1 1 calc R . . C31 C 1.2838(2) -0.2517(4) 0.6406(2) 0.0368(9) Uani 1 1 d . . . H31 H 1.2946 -0.2442 0.5940 0.044 Uiso 1 1 calc R . . C32 C 1.2713(3) 0.0478(5) 0.4859(2) 0.0533(13) Uani 1 1 d . . . H32A H 1.2728 0.1500 0.4976 0.080 Uiso 1 1 calc R . . H32B H 1.2317 0.0312 0.4425 0.080 Uiso 1 1 calc R . . H32C H 1.3240 0.0172 0.4784 0.080 Uiso 1 1 calc R . . C33 C 0.6803(2) 0.4387(5) 0.6216(2) 0.0392(10) Uani 1 1 d . . . H33A H 0.6703 0.5420 0.6126 0.047 Uiso 1 1 calc R . . H33B H 0.6920 0.4242 0.6736 0.047 Uiso 1 1 calc R . . C34 C 0.6056(2) 0.3560(5) 0.5904(2) 0.0400(10) Uani 1 1 d . . . H34A H 0.6118 0.2559 0.6075 0.048 Uiso 1 1 calc R . . H34B H 0.6000 0.3543 0.5382 0.048 Uiso 1 1 calc R . . C35 C 0.5293(2) 0.4177(5) 0.6092(2) 0.0379(10) Uani 1 1 d . . . H35 H 0.5237 0.5181 0.5909 0.045 Uiso 1 1 calc R . . C36 C 0.4564(2) 0.3343(6) 0.5724(3) 0.0596(13) Uani 1 1 d . . . H36A H 0.4606 0.2348 0.5887 0.089 Uiso 1 1 calc R . . H36B H 0.4538 0.3369 0.5210 0.089 Uiso 1 1 calc R . . H36C H 0.4080 0.3776 0.5837 0.089 Uiso 1 1 calc R . . C37 C 0.5330(3) 0.4238(7) 0.6879(2) 0.0696(17) Uani 1 1 d . . . H37A H 0.5765 0.4874 0.7095 0.104 Uiso 1 1 calc R . . H37B H 0.5426 0.3275 0.7080 0.104 Uiso 1 1 calc R . . H37C H 0.4822 0.4602 0.6976 0.104 Uiso 1 1 calc R . . S1A S 1.0856(4) 0.6434(16) 0.1055(4) 0.0549(18) Uani 0.401(5) 1 d PDU A 2 C16A C 0.9819(8) 0.617(4) 0.0957(9) 0.058(8) Uani 0.401(5) 1 d PDU A 2 H16A H 0.9442 0.6434 0.0546 0.070 Uiso 0.401(5) 1 calc PR A 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 S1 0.0490(15) 0.0563(16) 0.0352(14) 0.0144(12) 0.0097(10) 0.0056(12) S2 0.0398(6) 0.0378(6) 0.0625(8) 0.0107(6) -0.0023(5) 0.0073(5) O1 0.0326(14) 0.0478(17) 0.0513(18) 0.0054(15) 0.0121(13) 0.0117(14) O2 0.0399(16) 0.0577(19) 0.0378(17) 0.0058(15) 0.0162(13) 0.0004(14) O3 0.0279(13) 0.0498(17) 0.0377(16) 0.0112(13) 0.0138(12) 0.0114(13) O4 0.0295(14) 0.0439(16) 0.0514(18) 0.0170(14) 0.0128(13) 0.0110(12) N1 0.0274(16) 0.0430(19) 0.0364(19) -0.0031(15) 0.0124(14) 0.0032(14) C1 0.0270(19) 0.035(2) 0.036(2) -0.0064(19) 0.0047(17) -0.0038(17) C2 0.0230(17) 0.032(2) 0.033(2) -0.0032(17) 0.0065(16) -0.0002(16) C3 0.0260(18) 0.033(2) 0.0257(19) -0.0061(16) 0.0055(15) -0.0036(16) C4 0.0263(19) 0.039(2) 0.032(2) -0.0043(18) 0.0053(17) -0.0025(17) C5 0.0204(17) 0.0260(18) 0.029(2) -0.0033(15) 0.0042(15) -0.0051(14) C6 0.0183(16) 0.0260(18) 0.0274(19) -0.0049(15) 0.0033(14) -0.0047(14) C7 0.0207(16) 0.0229(17) 0.0257(19) -0.0042(15) 0.0018(14) -0.0030(14) C8 0.0235(17) 0.0260(18) 0.031(2) 0.0018(16) 0.0046(15) -0.0011(15) C9 0.0242(18) 0.0281(19) 0.034(2) -0.0015(17) 0.0049(16) -0.0015(15) C10 0.0256(18) 0.030(2) 0.033(2) 0.0048(17) -0.0004(16) -0.0020(16) C11 0.0242(17) 0.0287(19) 0.028(2) -0.0007(16) 0.0036(15) -0.0014(15) C12 0.0229(18) 0.031(2) 0.032(2) -0.0039(16) 0.0068(16) -0.0022(15) C13 0.0208(17) 0.032(2) 0.031(2) 0.0006(17) 0.0027(15) 0.0017(15) C14 0.034(2) 0.030(2) 0.033(2) 0.0028(17) 0.0106(17) 0.0009(17) C15 0.037(2) 0.055(3) 0.034(2) 0.008(2) 0.0061(18) 0.006(2) C16 0.038(5) 0.044(6) 0.020(6) 0.012(5) 0.011(4) 0.000(4) C17 0.036(2) 0.064(3) 0.042(3) 0.007(2) 0.0083(19) -0.007(2) C18 0.0273(19) 0.046(2) 0.039(2) 0.0027(19) 0.0116(17) 0.0044(18) C19 0.0220(17) 0.0242(17) 0.0242(19) -0.0032(15) 0.0046(14) -0.0046(14) C20 0.0255(18) 0.0294(19) 0.0232(19) -0.0050(16) 0.0015(15) -0.0037(15) C21 0.0277(19) 0.038(2) 0.029(2) 0.0008(17) 0.0079(16) -0.0047(16) C22 0.0276(18) 0.0268(19) 0.0245(19) -0.0043(16) 0.0013(15) -0.0057(15) C23 0.0242(17) 0.0235(18) 0.0258(19) -0.0038(15) -0.0034(15) -0.0039(14) C24 0.0269(18) 0.0262(18) 0.0275(19) 0.0020(15) 0.0039(15) -0.0011(15) C25 0.0243(18) 0.0295(19) 0.033(2) -0.0013(17) 0.0030(16) 0.0015(15) C26 0.0281(18) 0.0237(18) 0.027(2) -0.0011(16) -0.0036(15) -0.0026(15) C27 0.0299(19) 0.0271(19) 0.027(2) -0.0003(16) -0.0008(16) -0.0071(16) C28 0.034(2) 0.0220(18) 0.034(2) -0.0038(16) -0.0016(17) -0.0056(16) C29 0.054(3) 0.037(2) 0.040(2) 0.012(2) 0.004(2) 0.013(2) C30 0.063(3) 0.036(2) 0.044(3) 0.014(2) 0.002(2) 0.012(2) C31 0.032(2) 0.031(2) 0.044(2) 0.0045(19) -0.0001(18) 0.0007(17) C32 0.038(2) 0.064(3) 0.065(3) 0.026(3) 0.026(2) 0.015(2) C33 0.029(2) 0.054(3) 0.039(2) -0.011(2) 0.0171(18) -0.0001(19) C34 0.033(2) 0.046(2) 0.043(2) -0.005(2) 0.0138(19) -0.0003(19) C35 0.029(2) 0.050(2) 0.036(2) 0.006(2) 0.0093(17) 0.0047(18) C36 0.032(2) 0.072(3) 0.074(4) -0.003(3) 0.010(2) 0.000(2) C37 0.036(2) 0.132(5) 0.044(3) -0.004(3) 0.016(2) 0.018(3) S1A 0.058(3) 0.070(3) 0.040(3) 0.020(3) 0.0155(19) 0.004(2) C16A 0.051(9) 0.067(10) 0.057(11) 0.007(8) 0.011(7) 0.010(7) _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 C15 1.688(5) . ? S1 C16 1.764(10) . ? S2 C30 1.703(5) . ? S2 C31 1.707(4) . ? O1 C1 1.208(5) . ? O2 C4 1.217(4) . ? O3 C12 1.375(4) . ? O3 C18 1.419(4) . ? O4 C25 1.370(4) . ? O4 C32 1.423(5) . ? N1 C4 1.390(5) . ? N1 C1 1.400(5) . ? N1 C33 1.463(4) . ? C1 C2 1.493(5) . ? C2 C5 1.372(5) . ? C2 C3 1.380(5) . ? C3 C20 1.371(5) . ? C3 C4 1.492(5) . ? C5 C6 1.431(5) . ? C5 C9 1.487(5) . ? C6 C19 1.413(5) . ? C6 C7 1.492(5) . ? C7 C8 1.401(5) . ? C7 C13 1.405(5) . ? C8 C10 1.379(5) . ? C8 C9 1.502(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.387(5) . ? C10 H10 0.9500 . ? C11 C12 1.413(5) . ? C11 C14 1.480(5) . ? C12 C13 1.387(5) . ? C13 H13 0.9500 . ? C14 C15 1.381(5) . ? C14 C17 1.391(5) . ? C15 C16A 1.379(10) . ? C15 H15 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.370(9) . ? C16 H16 0.9500 . ? C17 S1A 1.669(7) . ? C17 H17 0.9500 . ? C17 H17A 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.427(5) . ? C19 C23 1.489(5) . ? C20 C21 1.500(5) . ? C21 C22 1.491(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.374(5) . ? C22 C23 1.409(5) . ? C23 C24 1.403(5) . ? C24 C25 1.393(5) . ? C24 H24 0.9500 . ? C25 C26 1.410(5) . ? C26 C27 1.388(5) . ? C26 C28 1.485(5) . ? C27 H27 0.9500 . ? C28 C31 1.366(5) . ? C28 C29 1.428(5) . ? C29 C30 1.358(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.513(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.526(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C37 1.503(6) . ? C35 C36 1.523(6) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? S1A C16A 1.758(10) . ? C16A H16A 0.9500 . ? 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 S1 C16 89.9(4) . . ? C30 S2 C31 92.2(2) . . ? C12 O3 C18 118.5(3) . . ? C25 O4 C32 118.8(3) . . ? C4 N1 C1 112.4(3) . . ? C4 N1 C33 124.5(3) . . ? C1 N1 C33 123.1(3) . . ? O1 C1 N1 125.3(3) . . ? O1 C1 C2 129.4(4) . . ? N1 C1 C2 105.3(3) . . ? C5 C2 C3 120.8(3) . . ? C5 C2 C1 130.9(3) . . ? C3 C2 C1 108.2(3) . . ? C20 C3 C2 120.5(3) . . ? C20 C3 C4 131.2(3) . . ? C2 C3 C4 108.4(3) . . ? O2 C4 N1 125.0(3) . . ? O2 C4 C3 129.3(3) . . ? N1 C4 C3 105.6(3) . . ? C2 C5 C6 120.6(3) . . ? C2 C5 C9 127.0(3) . . ? C6 C5 C9 112.4(3) . . ? C19 C6 C5 118.5(3) . . ? C19 C6 C7 135.9(3) . . ? C5 C6 C7 105.5(3) . . ? C8 C7 C13 117.7(3) . . ? C8 C7 C6 108.7(3) . . ? C13 C7 C6 133.6(3) . . ? C10 C8 C7 121.7(3) . . ? C10 C8 C9 127.0(3) . . ? C7 C8 C9 111.3(3) . . ? C5 C9 C8 102.0(3) . . ? C5 C9 H9A 111.4 . . ? C8 C9 H9A 111.4 . . ? C5 C9 H9B 111.4 . . ? C8 C9 H9B 111.4 . . ? H9A C9 H9B 109.2 . . ? C8 C10 C11 121.3(3) . . ? C8 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C12 117.3(3) . . ? C10 C11 C14 119.2(3) . . ? C12 C11 C14 123.5(3) . . ? O3 C12 C13 123.9(3) . . ? O3 C12 C11 114.4(3) . . ? C13 C12 C11 121.8(3) . . ? C12 C13 C7 120.1(3) . . ? C12 C13 H13 119.9 . . ? C7 C13 H13 119.9 . . ? C15 C14 C17 112.0(3) . . ? C15 C14 C11 121.4(3) . . ? C17 C14 C11 126.6(3) . . ? C16A C15 C14 112.1(7) . . ? C16A C15 S1 2.7(14) . . ? C14 C15 S1 113.8(3) . . ? C16A C15 H15 124.7 . . ? C14 C15 H15 123.1 . . ? S1 C15 H15 123.1 . . ? C16A C15 H15A 123.9 . . ? C14 C15 H15A 123.9 . . ? S1 C15 H15A 122.2 . . ? H15 C15 H15A 2.1 . . ? C17 C16 S1 111.2(8) . . ? C17 C16 H16 124.4 . . ? S1 C16 H16 124.4 . . ? C16 C17 C14 112.9(6) . . ? C16 C17 S1A 3.8(18) . . ? C14 C17 S1A 114.3(4) . . ? C16 C17 H17 123.6 . . ? C14 C17 H17 123.6 . . ? S1A C17 H17 122.0 . . ? C16 C17 H17A 124.1 . . ? C14 C17 H17A 122.9 . . ? S1A C17 H17A 122.9 . . ? H17 C17 H17A 3.3 . . ? O3 C18 H18A 109.5 . . ? O3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C6 C19 C20 118.6(3) . . ? C6 C19 C23 135.6(3) . . ? C20 C19 C23 105.9(3) . . ? C3 C20 C19 120.9(3) . . ? C3 C20 C21 127.1(3) . . ? C19 C20 C21 112.0(3) . . ? C22 C21 C20 102.1(3) . . ? C22 C21 H21A 111.3 . . ? C20 C21 H21A 111.3 . . ? C22 C21 H21B 111.3 . . ? C20 C21 H21B 111.3 . . ? H21A C21 H21B 109.2 . . ? C27 C22 C23 121.4(3) . . ? C27 C22 C21 127.2(3) . . ? C23 C22 C21 111.4(3) . . ? C24 C23 C22 117.8(3) . . ? C24 C23 C19 133.7(3) . . ? C22 C23 C19 108.5(3) . . ? C25 C24 C23 119.8(3) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? O4 C25 C24 122.7(3) . . ? O4 C25 C26 115.1(3) . . ? C24 C25 C26 122.1(3) . . ? C27 C26 C25 116.9(3) . . ? C27 C26 C28 119.5(3) . . ? C25 C26 C28 123.3(3) . . ? C22 C27 C26 121.8(3) . . ? C22 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C31 C28 C29 110.1(4) . . ? C31 C28 C26 127.8(4) . . ? C29 C28 C26 122.1(3) . . ? C30 C29 C28 114.3(4) . . ? C30 C29 H29 122.8 . . ? C28 C29 H29 122.8 . . ? C29 C30 S2 110.7(3) . . ? C29 C30 H30 124.7 . . ? S2 C30 H30 124.7 . . ? C28 C31 S2 112.6(3) . . ? C28 C31 H31 123.7 . . ? S2 C31 H31 123.7 . . ? O4 C32 H32A 109.5 . . ? O4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N1 C33 C34 113.5(3) . . ? N1 C33 H33A 108.9 . . ? C34 C33 H33A 108.9 . . ? N1 C33 H33B 108.9 . . ? C34 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C33 C34 C35 113.9(3) . . ? C33 C34 H34A 108.8 . . ? C35 C34 H34A 108.8 . . ? C33 C34 H34B 108.8 . . ? C35 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C37 C35 C36 111.2(4) . . ? C37 C35 C34 112.1(3) . . ? C36 C35 C34 110.7(4) . . ? C37 C35 H35 107.5 . . ? C36 C35 H35 107.5 . . ? C34 C35 H35 107.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C17 S1A C16A 89.9(6) . . ? C15 C16A S1A 111.7(9) . . ? C15 C16A H16A 124.2 . . ? S1A C16A H16A 124.2 . . ? 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 C4 N1 C1 O1 -177.1(4) . . . . ? C33 N1 C1 O1 1.7(6) . . . . ? C4 N1 C1 C2 1.8(4) . . . . ? C33 N1 C1 C2 -179.5(3) . . . . ? O1 C1 C2 C5 -2.7(7) . . . . ? N1 C1 C2 C5 178.5(4) . . . . ? O1 C1 C2 C3 176.0(4) . . . . ? N1 C1 C2 C3 -2.8(4) . . . . ? C5 C2 C3 C20 2.3(5) . . . . ? C1 C2 C3 C20 -176.6(3) . . . . ? C5 C2 C3 C4 -178.4(3) . . . . ? C1 C2 C3 C4 2.7(4) . . . . ? C1 N1 C4 O2 179.8(4) . . . . ? C33 N1 C4 O2 1.0(6) . . . . ? C1 N1 C4 C3 -0.2(4) . . . . ? C33 N1 C4 C3 -178.9(3) . . . . ? C20 C3 C4 O2 -2.4(7) . . . . ? C2 C3 C4 O2 178.4(4) . . . . ? C20 C3 C4 N1 177.5(4) . . . . ? C2 C3 C4 N1 -1.6(4) . . . . ? C3 C2 C5 C6 -2.4(5) . . . . ? C1 C2 C5 C6 176.1(3) . . . . ? C3 C2 C5 C9 176.1(3) . . . . ? C1 C2 C5 C9 -5.4(6) . . . . ? C2 C5 C6 C19 -0.1(5) . . . . ? C9 C5 C6 C19 -178.8(3) . . . . ? C2 C5 C6 C7 178.0(3) . . . . ? C9 C5 C6 C7 -0.7(4) . . . . ? C19 C6 C7 C8 176.4(4) . . . . ? C5 C6 C7 C8 -1.3(4) . . . . ? C19 C6 C7 C13 -2.8(7) . . . . ? C5 C6 C7 C13 179.5(4) . . . . ? C13 C7 C8 C10 2.8(5) . . . . ? C6 C7 C8 C10 -176.6(3) . . . . ? C13 C7 C8 C9 -177.9(3) . . . . ? C6 C7 C8 C9 2.7(4) . . . . ? C2 C5 C9 C8 -176.4(3) . . . . ? C6 C5 C9 C8 2.2(4) . . . . ? C10 C8 C9 C5 176.3(3) . . . . ? C7 C8 C9 C5 -3.0(4) . . . . ? C7 C8 C10 C11 -1.7(5) . . . . ? C9 C8 C10 C11 179.1(3) . . . . ? C8 C10 C11 C12 -1.3(5) . . . . ? C8 C10 C11 C14 177.3(3) . . . . ? C18 O3 C12 C13 5.1(5) . . . . ? C18 O3 C12 C11 -174.7(3) . . . . ? C10 C11 C12 O3 -177.0(3) . . . . ? C14 C11 C12 O3 4.4(5) . . . . ? C10 C11 C12 C13 3.2(5) . . . . ? C14 C11 C12 C13 -175.4(3) . . . . ? O3 C12 C13 C7 178.1(3) . . . . ? C11 C12 C13 C7 -2.1(5) . . . . ? C8 C7 C13 C12 -0.9(5) . . . . ? C6 C7 C13 C12 178.3(3) . . . . ? C10 C11 C14 C15 -36.7(5) . . . . ? C12 C11 C14 C15 141.9(4) . . . . ? C10 C11 C14 C17 139.7(4) . . . . ? C12 C11 C14 C17 -41.7(6) . . . . ? C17 C14 C15 C16A -1.6(17) . . . . ? C11 C14 C15 C16A 175.3(17) . . . . ? C17 C14 C15 S1 0.7(5) . . . . ? C11 C14 C15 S1 177.6(4) . . . . ? C16 S1 C15 C16A 49(25) . . . . ? C16 S1 C15 C14 -2.8(11) . . . . ? C15 S1 C16 C17 4.2(18) . . . . ? S1 C16 C17 C14 -5(2) . . . . ? S1 C16 C17 S1A 108(15) . . . . ? C15 C14 C17 C16 2.6(15) . . . . ? C11 C14 C17 C16 -174.1(14) . . . . ? C15 C14 C17 S1A -1.3(8) . . . . ? C11 C14 C17 S1A -178.0(7) . . . . ? C5 C6 C19 C20 2.7(5) . . . . ? C7 C6 C19 C20 -174.7(3) . . . . ? C5 C6 C19 C23 -177.6(4) . . . . ? C7 C6 C19 C23 5.0(7) . . . . ? C2 C3 C20 C19 0.4(5) . . . . ? C4 C3 C20 C19 -178.7(3) . . . . ? C2 C3 C20 C21 179.3(3) . . . . ? C4 C3 C20 C21 0.2(6) . . . . ? C6 C19 C20 C3 -2.9(5) . . . . ? C23 C19 C20 C3 177.3(3) . . . . ? C6 C19 C20 C21 178.1(3) . . . . ? C23 C19 C20 C21 -1.7(4) . . . . ? C3 C20 C21 C22 -178.7(3) . . . . ? C19 C20 C21 C22 0.3(4) . . . . ? C20 C21 C22 C27 179.7(3) . . . . ? C20 C21 C22 C23 1.4(4) . . . . ? C27 C22 C23 C24 -2.3(5) . . . . ? C21 C22 C23 C24 176.1(3) . . . . ? C27 C22 C23 C19 179.1(3) . . . . ? C21 C22 C23 C19 -2.5(4) . . . . ? C6 C19 C23 C24 4.5(7) . . . . ? C20 C19 C23 C24 -175.8(4) . . . . ? C6 C19 C23 C22 -177.2(4) . . . . ? C20 C19 C23 C22 2.5(4) . . . . ? C22 C23 C24 C25 1.6(5) . . . . ? C19 C23 C24 C25 179.7(3) . . . . ? C32 O4 C25 C24 1.5(5) . . . . ? C32 O4 C25 C26 -176.6(4) . . . . ? C23 C24 C25 O4 -179.1(3) . . . . ? C23 C24 C25 C26 -1.0(5) . . . . ? O4 C25 C26 C27 179.2(3) . . . . ? C24 C25 C26 C27 1.1(5) . . . . ? O4 C25 C26 C28 4.1(5) . . . . ? C24 C25 C26 C28 -174.0(3) . . . . ? C23 C22 C27 C26 2.4(5) . . . . ? C21 C22 C27 C26 -175.7(3) . . . . ? C25 C26 C27 C22 -1.7(5) . . . . ? C28 C26 C27 C22 173.6(3) . . . . ? C27 C26 C28 C31 159.7(4) . . . . ? C25 C26 C28 C31 -25.3(6) . . . . ? C27 C26 C28 C29 -20.0(5) . . . . ? C25 C26 C28 C29 155.0(4) . . . . ? C31 C28 C29 C30 0.4(5) . . . . ? C26 C28 C29 C30 -179.8(4) . . . . ? C28 C29 C30 S2 -0.5(5) . . . . ? C31 S2 C30 C29 0.3(4) . . . . ? C29 C28 C31 S2 -0.1(4) . . . . ? C26 C28 C31 S2 -179.9(3) . . . . ? C30 S2 C31 C28 -0.1(3) . . . . ? C4 N1 C33 C34 -90.0(5) . . . . ? C1 N1 C33 C34 91.4(5) . . . . ? N1 C33 C34 C35 -168.8(3) . . . . ? C33 C34 C35 C37 -58.6(5) . . . . ? C33 C34 C35 C36 176.6(4) . . . . ? C16 C17 S1A C16A -66(13) . . . . ? C14 C17 S1A C16A 2.8(14) . . . . ? C14 C15 C16A S1A 4(3) . . . . ? S1 C15 C16A S1A -126(26) . . . . ? C17 S1A C16A C15 -4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.255 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.055