data_jam06 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H33 F3 N6 O10 S2, C3 H6 O' _chemical_formula_sum 'C42 H39 F3 N6 O11 S2' _chemical_formula_weight 924.91 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' 'F' 'F' 0.0171 0.0103 '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 17.6754(7) _cell_length_b 11.5184(5) _cell_length_c 22.3282(9) _cell_angle_alpha 90.00 _cell_angle_beta 110.488(2) _cell_angle_gamma 90.00 _cell_volume 4258.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5619 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 22.18 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9145 _exptl_absorpt_correction_T_max 0.9918 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 3 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22570 _diffrn_reflns_av_R_equivalents 0.1110 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 22.54 _reflns_number_total 5566 _reflns_number_gt 3657 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.630' _computing_cell_refinement 'Bruker SAINT v6.45A' _computing_data_reduction 'Bruker SAINT v6.45A' _computing_structure_solution 'Bruker XS v6.12' _computing_structure_refinement 'Bruker XL v6.12' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF v6.12' _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 matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5566 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0994 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1220 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 1.647 _refine_ls_restrained_S_all 1.647 _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 S1 S 0.07961(7) 0.11539(11) 0.22983(6) 0.0233(3) Uani 1 1 d . . . S2 S 0.18365(7) 0.24356(11) 0.50098(6) 0.0246(3) Uani 1 1 d . . . F1 F -0.24256(18) 0.3645(3) 0.32442(14) 0.0464(8) Uani 1 1 d . . . F2 F -0.29158(18) 0.3349(3) 0.39892(15) 0.0512(9) Uani 1 1 d . . . F3 F -0.36702(18) 0.3148(3) 0.29998(15) 0.0560(10) Uani 1 1 d . . . O1 O -0.3290(2) 0.1016(3) 0.31114(19) 0.0474(11) Uani 1 1 d . . . O2 O 0.09712(18) 0.2303(3) 0.21478(14) 0.0246(8) Uani 1 1 d . . . O3 O 0.05153(18) 0.0295(3) 0.18112(14) 0.0268(9) Uani 1 1 d . . . O4 O 0.0726(2) -0.1502(3) 0.27138(15) 0.0332(9) Uani 1 1 d . . . O5 O 0.1637(2) -0.2205(3) 0.23590(17) 0.0434(10) Uani 1 1 d . . . O6 O 0.0893(2) 0.5526(3) 0.49402(17) 0.0302(9) Uani 1 1 d . . . O7 O 0.17903(18) 0.1760(3) 0.44614(14) 0.0272(9) Uani 1 1 d . . . O8 O 0.12563(18) 0.2273(3) 0.53210(14) 0.0249(8) Uani 1 1 d . . . O9 O 0.2232(2) 0.3906(3) 0.62403(17) 0.0409(10) Uani 1 1 d . . . O10 O 0.2447(2) 0.2664(3) 0.70112(17) 0.0389(10) Uani 1 1 d . . . N1 N 0.0110(2) 0.1260(3) 0.26371(18) 0.0226(10) Uani 1 1 d . . . N2 N -0.1954(2) 0.1372(3) 0.37234(18) 0.0227(10) Uani 1 1 d . . . N3 N 0.1385(3) -0.1474(4) 0.2645(2) 0.0299(11) Uani 1 1 d . . . N4 N -0.0182(3) 0.6301(4) 0.4131(2) 0.0311(11) Uani 1 1 d . . . H4 H -0.0382 0.6704 0.4375 0.037 Uiso 1 1 calc R . . N5 N 0.1821(2) 0.3784(3) 0.48399(17) 0.0256(10) Uani 1 1 d . . . H5 H 0.1624 0.4257 0.5058 0.031 Uiso 1 1 calc R . . N6 N 0.2525(3) 0.3010(4) 0.6515(2) 0.0300(11) Uani 1 1 d . . . C1 C -0.0471(3) 0.0406(4) 0.2606(2) 0.0227(12) Uani 1 1 d . . . H1 H -0.0557 -0.0274 0.2350 0.027 Uiso 1 1 calc R . . C2 C -0.0889(3) 0.0679(4) 0.2987(2) 0.0218(12) Uani 1 1 d . . . C3 C -0.1587(3) -0.0031(4) 0.3036(2) 0.0257(12) Uani 1 1 d . . . H3A H -0.2078 0.0159 0.2667 0.031 Uiso 1 1 calc R . . H3B H -0.1468 -0.0864 0.3004 0.031 Uiso 1 1 calc R . . C4 C -0.1767(3) 0.0156(4) 0.3647(2) 0.0253(12) Uani 1 1 d . . . H4A H -0.2230 -0.0335 0.3638 0.030 Uiso 1 1 calc R . . H4B H -0.1293 -0.0085 0.4019 0.030 Uiso 1 1 calc R . . C5 C -0.1282(3) 0.2126(4) 0.4115(2) 0.0205(12) Uani 1 1 d . . . H5A H -0.1523 0.2853 0.4216 0.025 Uiso 1 1 calc R . . C6 C -0.0728(3) 0.2468(4) 0.3754(2) 0.0200(12) Uani 1 1 d . . . C7 C -0.0305(3) 0.3503(4) 0.3923(2) 0.0229(12) Uani 1 1 d . . . H7 H -0.0408 0.3983 0.4232 0.028 Uiso 1 1 calc R . . C8 C 0.0262(3) 0.3874(4) 0.3661(2) 0.0224(12) Uani 1 1 d . . . C9 C 0.0459(3) 0.3170(4) 0.3233(2) 0.0242(12) Uani 1 1 d . . . H9 H 0.0857 0.3392 0.3058 0.029 Uiso 1 1 calc R . . C10 C 0.0046(3) 0.2125(4) 0.3071(2) 0.0199(12) Uani 1 1 d . . . C11 C -0.0556(3) 0.1763(4) 0.3307(2) 0.0199(12) Uani 1 1 d . . . C12 C -0.2718(4) 0.1699(5) 0.3416(2) 0.0341(14) Uani 1 1 d . . . C13 C -0.2897(3) 0.2987(5) 0.3422(2) 0.0278(13) Uani 1 1 d . . . C14 C -0.0807(3) 0.1539(4) 0.4743(2) 0.0214(12) Uani 1 1 d . . . H14 H -0.0278 0.1279 0.4794 0.026 Uiso 1 1 calc R . . C15 C -0.1064(3) 0.1359(4) 0.5226(2) 0.0233(12) Uani 1 1 d . . . C16 C -0.1879(3) 0.1699(5) 0.5233(3) 0.0477(17) Uani 1 1 d . . . H16A H -0.2187 0.2078 0.4828 0.072 Uiso 1 1 calc R . . H16B H -0.1815 0.2237 0.5587 0.072 Uiso 1 1 calc R . . H16C H -0.2168 0.1005 0.5288 0.072 Uiso 1 1 calc R . . C17 C -0.0527(3) 0.0795(4) 0.5829(2) 0.0313(14) Uani 1 1 d . . . H17A H -0.0012 0.0588 0.5784 0.047 Uiso 1 1 calc R . . H17B H -0.0789 0.0093 0.5911 0.047 Uiso 1 1 calc R . . H17C H -0.0429 0.1336 0.6187 0.047 Uiso 1 1 calc R . . C18 C 0.1699(3) 0.0641(4) 0.2892(2) 0.0216(12) Uani 1 1 d . . . C19 C 0.2257(3) 0.1460(4) 0.3232(2) 0.0258(13) Uani 1 1 d . . . H19 H 0.2118 0.2260 0.3186 0.031 Uiso 1 1 calc R . . C20 C 0.3012(3) 0.1131(5) 0.3636(2) 0.0307(13) Uani 1 1 d . . . H20 H 0.3382 0.1705 0.3873 0.037 Uiso 1 1 calc R . . C21 C 0.3239(3) -0.0013(5) 0.3702(2) 0.0359(14) Uani 1 1 d . . . H21 H 0.3763 -0.0229 0.3980 0.043 Uiso 1 1 calc R . . C22 C 0.2691(3) -0.0866(5) 0.3354(2) 0.0339(14) Uani 1 1 d . . . H22 H 0.2843 -0.1661 0.3387 0.041 Uiso 1 1 calc R . . C23 C 0.1936(3) -0.0528(4) 0.2969(2) 0.0239(12) Uani 1 1 d . . . C24 C 0.0662(3) 0.5096(4) 0.3802(2) 0.0257(13) Uani 1 1 d . . . C25 C 0.0168(3) 0.5916(4) 0.3246(2) 0.0296(13) Uani 1 1 d . . . H25A H 0.0492 0.6600 0.3215 0.036 Uiso 1 1 calc R . . H25B H -0.0014 0.5501 0.2831 0.036 Uiso 1 1 calc R . . C26 C -0.0551(3) 0.6277(5) 0.3434(2) 0.0320(13) Uani 1 1 d . . . H26A H -0.0759 0.7051 0.3260 0.038 Uiso 1 1 calc R . . H26B H -0.0994 0.5702 0.3289 0.038 Uiso 1 1 calc R . . C27 C 0.0487(3) 0.5657(4) 0.4365(3) 0.0277(13) Uani 1 1 d . . . C28 C 0.1556(3) 0.5005(4) 0.3882(2) 0.0231(12) Uani 1 1 d . . . C29 C 0.1867(3) 0.5513(4) 0.3458(2) 0.0273(13) Uani 1 1 d . . . H29 H 0.1528 0.6007 0.3134 0.033 Uiso 1 1 calc R . . C30 C 0.2645(3) 0.5333(5) 0.3485(3) 0.0352(15) Uani 1 1 d . . . H30 H 0.2830 0.5691 0.3178 0.042 Uiso 1 1 calc R . . C31 C 0.3166(3) 0.4630(5) 0.3957(3) 0.0353(15) Uani 1 1 d . . . H31 H 0.3706 0.4503 0.3978 0.042 Uiso 1 1 calc R . . C32 C 0.2877(3) 0.4122(4) 0.4394(2) 0.0307(14) Uani 1 1 d . . . H32 H 0.3223 0.3635 0.4718 0.037 Uiso 1 1 calc R . . C33 C 0.2094(3) 0.4307(4) 0.4368(2) 0.0267(13) Uani 1 1 d . . . C34 C 0.2805(3) 0.2082(4) 0.5594(2) 0.0229(12) Uani 1 1 d . . . C35 C 0.3027(3) 0.2303(4) 0.6255(2) 0.0249(13) Uani 1 1 d . . . C36 C 0.3726(3) 0.1881(5) 0.6679(3) 0.0355(14) Uani 1 1 d . . . H36 H 0.3855 0.2011 0.7124 0.043 Uiso 1 1 calc R . . C37 C 0.4252(3) 0.1260(5) 0.6463(3) 0.0381(15) Uani 1 1 d . . . H37 H 0.4745 0.0980 0.6761 0.046 Uiso 1 1 calc R . . C38 C 0.4066(3) 0.1045(5) 0.5820(3) 0.0351(14) Uani 1 1 d . . . H38 H 0.4433 0.0633 0.5672 0.042 Uiso 1 1 calc R . . C39 C 0.3332(3) 0.1441(4) 0.5390(2) 0.0294(13) Uani 1 1 d . . . H39 H 0.3191 0.1268 0.4948 0.035 Uiso 1 1 calc R . . O11 O 0.4894(3) 0.1449(7) 0.4720(2) 0.135(3) Uani 1 1 d . . . C41 C 0.5216(4) 0.2230(7) 0.3884(4) 0.093(3) Uani 1 1 d . . . H41A H 0.5667 0.1795 0.3835 0.140 Uiso 1 1 calc R . . H41B H 0.5241 0.3040 0.3758 0.140 Uiso 1 1 calc R . . H41C H 0.4704 0.1884 0.3613 0.140 Uiso 1 1 calc R . . C42 C 0.5270(4) 0.2185(8) 0.4564(4) 0.077(2) Uani 1 1 d . . . C43 C 0.5851(6) 0.2895(10) 0.5031(5) 0.161(5) Uani 1 1 d . . . H43A H 0.5700 0.2964 0.5411 0.241 Uiso 1 1 calc R . . H43B H 0.5863 0.3668 0.4851 0.241 Uiso 1 1 calc R . . H43C H 0.6386 0.2537 0.5148 0.241 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 S1 0.0281(8) 0.0239(8) 0.0214(8) -0.0007(6) 0.0131(6) 0.0002(6) S2 0.0272(8) 0.0267(8) 0.0216(8) -0.0007(6) 0.0105(6) -0.0021(6) F1 0.054(2) 0.042(2) 0.041(2) 0.0058(16) 0.0130(17) 0.0042(17) F2 0.059(2) 0.054(2) 0.043(2) 0.0068(17) 0.0198(17) 0.0180(18) F3 0.046(2) 0.069(3) 0.048(2) 0.0152(18) 0.0106(18) 0.0235(18) O1 0.025(2) 0.052(3) 0.061(3) 0.021(2) 0.010(2) -0.007(2) O2 0.036(2) 0.017(2) 0.025(2) 0.0016(15) 0.0167(16) -0.0023(16) O3 0.033(2) 0.029(2) 0.021(2) -0.0057(16) 0.0131(16) -0.0022(17) O4 0.041(2) 0.033(2) 0.031(2) 0.0018(17) 0.0193(19) -0.0044(18) O5 0.051(3) 0.038(3) 0.045(3) -0.015(2) 0.022(2) 0.010(2) O6 0.045(2) 0.028(2) 0.024(2) -0.0025(18) 0.0196(19) -0.0010(18) O7 0.032(2) 0.030(2) 0.021(2) -0.0061(16) 0.0106(16) -0.0017(17) O8 0.0264(19) 0.026(2) 0.025(2) 0.0020(16) 0.0116(16) -0.0003(16) O9 0.069(3) 0.028(2) 0.037(2) -0.004(2) 0.033(2) -0.001(2) O10 0.049(2) 0.050(3) 0.023(2) -0.0041(19) 0.0182(18) -0.010(2) N1 0.027(2) 0.023(3) 0.023(2) -0.001(2) 0.0148(19) 0.001(2) N2 0.019(2) 0.030(3) 0.018(2) 0.002(2) 0.0063(19) 0.002(2) N3 0.039(3) 0.027(3) 0.027(3) 0.005(2) 0.016(2) 0.003(2) N4 0.043(3) 0.022(3) 0.038(3) -0.001(2) 0.026(2) 0.007(2) N5 0.033(3) 0.027(3) 0.021(2) -0.003(2) 0.014(2) -0.001(2) N6 0.042(3) 0.026(3) 0.024(3) -0.010(2) 0.015(2) -0.011(2) C1 0.026(3) 0.019(3) 0.023(3) 0.000(2) 0.009(2) -0.002(2) C2 0.023(3) 0.024(3) 0.018(3) 0.002(2) 0.007(2) -0.003(2) C3 0.025(3) 0.034(3) 0.019(3) -0.003(2) 0.009(2) -0.004(2) C4 0.024(3) 0.030(3) 0.022(3) 0.002(2) 0.009(2) -0.004(2) C5 0.023(3) 0.019(3) 0.020(3) 0.000(2) 0.008(2) 0.002(2) C6 0.020(3) 0.025(3) 0.016(3) 0.007(2) 0.008(2) 0.003(2) C7 0.033(3) 0.024(3) 0.016(3) 0.004(2) 0.014(2) 0.008(3) C8 0.023(3) 0.023(3) 0.020(3) 0.005(2) 0.007(2) 0.007(3) C9 0.027(3) 0.026(3) 0.024(3) 0.006(2) 0.014(2) 0.007(3) C10 0.021(3) 0.021(3) 0.018(3) 0.004(2) 0.008(2) 0.005(2) C11 0.018(3) 0.026(3) 0.016(3) 0.007(2) 0.006(2) 0.007(2) C12 0.041(4) 0.050(4) 0.021(3) 0.012(3) 0.023(3) 0.015(3) C13 0.021(3) 0.054(4) 0.008(3) 0.011(3) 0.005(2) 0.004(3) C14 0.017(3) 0.026(3) 0.021(3) 0.002(2) 0.006(2) -0.001(2) C15 0.025(3) 0.025(3) 0.020(3) -0.002(2) 0.009(2) -0.002(2) C16 0.047(4) 0.075(5) 0.029(4) 0.008(3) 0.024(3) 0.006(3) C17 0.036(3) 0.036(4) 0.019(3) 0.002(3) 0.007(3) -0.004(3) C18 0.025(3) 0.030(3) 0.015(3) 0.000(2) 0.012(2) -0.001(3) C19 0.030(3) 0.026(3) 0.028(3) 0.000(3) 0.019(3) 0.002(3) C20 0.034(3) 0.034(4) 0.027(3) -0.006(3) 0.014(3) -0.006(3) C21 0.027(3) 0.049(4) 0.028(3) -0.001(3) 0.004(3) -0.002(3) C22 0.036(4) 0.037(4) 0.033(4) 0.008(3) 0.018(3) 0.012(3) C23 0.027(3) 0.029(3) 0.017(3) -0.002(2) 0.009(2) -0.004(3) C24 0.036(3) 0.022(3) 0.026(3) 0.002(2) 0.020(3) 0.001(3) C25 0.039(3) 0.023(3) 0.035(3) 0.006(3) 0.024(3) 0.002(3) C26 0.045(4) 0.025(3) 0.031(4) 0.006(3) 0.019(3) 0.006(3) C27 0.043(4) 0.017(3) 0.033(4) -0.002(3) 0.026(3) -0.008(3) C28 0.030(3) 0.020(3) 0.024(3) -0.004(2) 0.015(3) -0.004(3) C29 0.036(3) 0.024(3) 0.026(3) -0.007(2) 0.016(3) -0.006(3) C30 0.052(4) 0.034(4) 0.036(4) -0.002(3) 0.037(3) -0.011(3) C31 0.036(4) 0.034(4) 0.044(4) -0.005(3) 0.026(3) -0.007(3) C32 0.034(3) 0.031(4) 0.032(3) 0.000(3) 0.019(3) -0.004(3) C33 0.035(3) 0.022(3) 0.032(3) -0.008(3) 0.023(3) -0.012(3) C34 0.027(3) 0.023(3) 0.018(3) 0.002(2) 0.007(2) -0.006(2) C35 0.029(3) 0.024(3) 0.023(3) -0.004(3) 0.011(3) -0.011(3) C36 0.038(4) 0.041(4) 0.023(3) -0.007(3) 0.006(3) -0.017(3) C37 0.030(3) 0.045(4) 0.032(4) 0.002(3) 0.002(3) -0.003(3) C38 0.031(3) 0.040(4) 0.034(4) 0.004(3) 0.011(3) 0.005(3) C39 0.031(3) 0.038(4) 0.023(3) -0.002(3) 0.014(3) -0.006(3) O11 0.108(5) 0.253(8) 0.047(4) -0.027(4) 0.032(3) -0.099(5) C41 0.065(5) 0.126(8) 0.093(7) 0.047(5) 0.034(5) 0.015(5) C42 0.037(4) 0.126(8) 0.068(6) 0.010(5) 0.017(4) -0.021(5) C43 0.122(9) 0.172(12) 0.155(11) -0.074(8) 0.008(8) -0.058(8) _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 O2 1.426(3) . ? S1 O3 1.425(3) . ? S1 N1 1.644(4) . ? S1 C18 1.781(5) . ? S2 O7 1.429(3) . ? S2 O8 1.438(3) . ? S2 N5 1.597(4) . ? S2 C34 1.798(5) . ? F1 C13 1.287(5) . ? F2 C13 1.344(5) . ? F3 C13 1.375(5) . ? O1 C12 1.272(6) . ? O4 N3 1.227(5) . ? O5 N3 1.231(5) . ? O6 C27 1.241(6) . ? O9 N6 1.220(5) . ? O10 N6 1.230(5) . ? N1 C1 1.406(5) . ? N1 C10 1.422(6) . ? N2 C12 1.338(6) . ? N2 C4 1.462(6) . ? N2 C5 1.484(6) . ? N3 C23 1.472(6) . ? N4 C27 1.337(6) . ? N4 C26 1.462(6) . ? N4 H4 0.8800 . ? N5 C33 1.437(6) . ? N5 H5 0.8800 . ? N6 C35 1.465(6) . ? C1 C2 1.344(6) . ? C1 H1 0.9500 . ? C2 C11 1.457(6) . ? C2 C3 1.517(6) . ? C3 C4 1.520(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C14 1.518(6) . ? C5 C6 1.522(6) . ? C5 H5A 1.0000 . ? C6 C7 1.388(6) . ? C6 C11 1.401(6) . ? C7 C8 1.393(6) . ? C7 H7 0.9500 . ? C8 C9 1.388(6) . ? C8 C24 1.557(6) . ? C9 C10 1.389(6) . ? C9 H9 0.9500 . ? C10 C11 1.404(6) . ? C12 C13 1.519(7) . ? C14 C15 1.326(6) . ? C14 H14 0.9500 . ? C15 C17 1.496(6) . ? C15 C16 1.498(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.385(6) . ? C18 C23 1.403(6) . ? C19 C20 1.377(7) . ? C19 H19 0.9500 . ? C20 C21 1.370(7) . ? C20 H20 0.9500 . ? C21 C22 1.406(7) . ? C21 H21 0.9500 . ? C22 C23 1.367(6) . ? C22 H22 0.9500 . ? C24 C28 1.531(6) . ? C24 C27 1.538(7) . ? C24 C25 1.561(7) . ? C25 C26 1.528(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C28 C29 1.379(6) . ? C28 C33 1.416(7) . ? C29 C30 1.372(6) . ? C29 H29 0.9500 . ? C30 C31 1.392(7) . ? C30 H30 0.9500 . ? C31 C32 1.380(6) . ? C31 H31 0.9500 . ? C32 C33 1.381(6) . ? C32 H32 0.9500 . ? C34 C39 1.386(6) . ? C34 C35 1.412(6) . ? C35 C36 1.356(7) . ? C36 C37 1.387(7) . ? C36 H36 0.9500 . ? C37 C38 1.379(7) . ? C37 H37 0.9500 . ? C38 C39 1.393(7) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? O11 C42 1.201(8) . ? C41 C42 1.487(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.436(10) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? 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 O2 S1 O3 120.74(19) . . ? O2 S1 N1 107.17(19) . . ? O3 S1 N1 106.7(2) . . ? O2 S1 C18 105.8(2) . . ? O3 S1 C18 108.6(2) . . ? N1 S1 C18 107.2(2) . . ? O7 S2 O8 120.4(2) . . ? O7 S2 N5 109.6(2) . . ? O8 S2 N5 106.59(19) . . ? O7 S2 C34 104.6(2) . . ? O8 S2 C34 106.2(2) . . ? N5 S2 C34 109.0(2) . . ? C1 N1 C10 107.0(3) . . ? C1 N1 S1 124.7(3) . . ? C10 N1 S1 127.9(3) . . ? C12 N2 C4 116.0(4) . . ? C12 N2 C5 126.4(4) . . ? C4 N2 C5 117.5(4) . . ? O4 N3 O5 125.4(4) . . ? O4 N3 C23 116.9(4) . . ? O5 N3 C23 117.6(4) . . ? C27 N4 C26 114.2(4) . . ? C27 N4 H4 122.9 . . ? C26 N4 H4 122.9 . . ? C33 N5 S2 126.8(3) . . ? C33 N5 H5 116.6 . . ? S2 N5 H5 116.6 . . ? O9 N6 O10 124.5(4) . . ? O9 N6 C35 118.8(4) . . ? O10 N6 C35 116.7(4) . . ? C2 C1 N1 111.0(4) . . ? C2 C1 H1 124.5 . . ? N1 C1 H1 124.5 . . ? C1 C2 C11 107.1(4) . . ? C1 C2 C3 124.1(4) . . ? C11 C2 C3 128.8(4) . . ? C4 C3 C2 114.8(4) . . ? C4 C3 H3A 108.6 . . ? C2 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? C2 C3 H3B 108.6 . . ? H3A C3 H3B 107.5 . . ? N2 C4 C3 111.5(4) . . ? N2 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N2 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? N2 C5 C14 110.7(4) . . ? N2 C5 C6 111.7(4) . . ? C14 C5 C6 110.7(4) . . ? N2 C5 H5A 107.9 . . ? C14 C5 H5A 107.9 . . ? C6 C5 H5A 107.9 . . ? C7 C6 C11 117.4(4) . . ? C7 C6 C5 117.6(4) . . ? C11 C6 C5 124.7(4) . . ? C6 C7 C8 123.2(4) . . ? C6 C7 H7 118.4 . . ? C8 C7 H7 118.4 . . ? C9 C8 C7 120.1(5) . . ? C9 C8 C24 117.5(4) . . ? C7 C8 C24 122.3(4) . . ? C8 C9 C10 116.7(4) . . ? C8 C9 H9 121.7 . . ? C10 C9 H9 121.7 . . ? C9 C10 C11 124.0(4) . . ? C9 C10 N1 128.6(4) . . ? C11 C10 N1 107.4(4) . . ? C6 C11 C10 118.5(4) . . ? C6 C11 C2 134.0(4) . . ? C10 C11 C2 107.4(4) . . ? O1 C12 N2 124.8(5) . . ? O1 C12 C13 118.7(5) . . ? N2 C12 C13 116.5(5) . . ? F1 C13 F2 109.9(4) . . ? F1 C13 F3 107.7(4) . . ? F2 C13 F3 105.0(4) . . ? F1 C13 C12 114.4(4) . . ? F2 C13 C12 112.7(4) . . ? F3 C13 C12 106.6(4) . . ? C15 C14 C5 125.8(4) . . ? C15 C14 H14 117.1 . . ? C5 C14 H14 117.1 . . ? C14 C15 C17 120.6(4) . . ? C14 C15 C16 124.9(4) . . ? C17 C15 C16 114.5(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 117.5(4) . . ? C19 C18 S1 117.6(4) . . ? C23 C18 S1 124.1(4) . . ? C20 C19 C18 120.9(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 121.0(5) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 119.6(5) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 118.7(5) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C18 122.3(5) . . ? C22 C23 N3 115.6(5) . . ? C18 C23 N3 122.1(4) . . ? C28 C24 C27 115.3(4) . . ? C28 C24 C8 109.8(4) . . ? C27 C24 C8 109.7(4) . . ? C28 C24 C25 113.7(4) . . ? C27 C24 C25 100.3(4) . . ? C8 C24 C25 107.4(4) . . ? C26 C25 C24 103.5(4) . . ? C26 C25 H25A 111.1 . . ? C24 C25 H25A 111.1 . . ? C26 C25 H25B 111.1 . . ? C24 C25 H25B 111.1 . . ? H25A C25 H25B 109.0 . . ? N4 C26 C25 101.1(4) . . ? N4 C26 H26A 111.5 . . ? C25 C26 H26A 111.5 . . ? N4 C26 H26B 111.5 . . ? C25 C26 H26B 111.5 . . ? H26A C26 H26B 109.4 . . ? O6 C27 N4 125.7(5) . . ? O6 C27 C24 125.9(5) . . ? N4 C27 C24 108.4(5) . . ? C29 C28 C33 116.4(4) . . ? C29 C28 C24 122.2(4) . . ? C33 C28 C24 121.1(4) . . ? C30 C29 C28 122.7(5) . . ? C30 C29 H29 118.7 . . ? C28 C29 H29 118.7 . . ? C29 C30 C31 120.6(5) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C32 C31 C30 118.1(5) . . ? C32 C31 H31 120.9 . . ? C30 C31 H31 120.9 . . ? C31 C32 C33 121.2(5) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C32 C33 C28 121.0(4) . . ? C32 C33 N5 119.6(5) . . ? C28 C33 N5 119.5(4) . . ? C39 C34 C35 117.9(5) . . ? C39 C34 S2 117.5(4) . . ? C35 C34 S2 124.3(4) . . ? C36 C35 C34 121.2(5) . . ? C36 C35 N6 116.9(5) . . ? C34 C35 N6 121.9(5) . . ? C35 C36 C37 119.9(5) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.8(5) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 118.9(5) . . ? C37 C38 H38 120.5 . . ? C39 C38 H38 120.5 . . ? C34 C39 C38 121.3(5) . . ? C34 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O11 C42 C43 121.3(8) . . ? O11 C42 C41 118.4(7) . . ? C43 C42 C41 119.7(7) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4 O8 0.88 2.23 3.072(5) 160.1 3_566 N5 H5 O6 0.88 1.91 2.651(5) 141.0 . N5 H5 O9 0.88 2.51 2.955(5) 112.1 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 22.54 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.089 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.084