data_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H27 F3 N6 O3 S' _chemical_formula_weight 752.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'S' 'S' 0.1246 0.1234 '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' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.161 _cell_length_b 13.733 _cell_length_c 14.107 _cell_angle_alpha 67.50 _cell_angle_beta 74.02 _cell_angle_gamma 71.86 _cell_volume 1868.2 _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.150 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12482 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.1707 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.54 _reflns_number_total 8449 _reflns_number_gt 4543 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1000P)^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 8449 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2789 _refine_ls_R_factor_gt 0.1739 _refine_ls_wR_factor_ref 0.3604 _refine_ls_wR_factor_gt 0.3292 _refine_ls_goodness_of_fit_ref 1.697 _refine_ls_restrained_S_all 1.697 _refine_ls_shift/su_max 2.537 _refine_ls_shift/su_mean 0.337 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 0.3219(5) 0.5932(3) 0.0962(4) 0.0373(14) Uani 1 1 d . . . N2 N 0.3171(6) 0.6018(4) 0.2658(4) 0.0446(15) Uani 1 1 d . . . N3 N 0.4081(4) 0.3156(3) 0.1030(3) 0.0256(11) Uani 1 1 d . . . N4 N 0.5558(5) -0.0924(3) 0.1573(3) 0.0254(11) Uani 1 1 d . . . N5 N 0.3675(5) 0.3342(3) 0.4525(3) 0.0294(12) Uani 1 1 d . . . N6 N 0.4050(5) -0.0589(3) 0.6547(3) 0.0274(12) Uani 1 1 d . . . C1 C 0.3478(6) 0.4846(4) 0.1365(4) 0.0292(14) Uani 1 1 d . . . C2 C 0.3058(7) 0.6442(5) 0.1642(5) 0.0473(19) Uani 1 1 d . . . H2B H 0.2832 0.7211 0.1373 0.057 Uiso 1 1 calc R . . C3 C 0.3406(6) 0.4943(4) 0.3046(4) 0.0326(15) Uani 1 1 d . . . C4 C 0.3567(6) 0.4317(4) 0.2413(4) 0.0321(15) Uani 1 1 d . . . H4B H 0.3732 0.3549 0.2695 0.039 Uiso 1 1 calc R . . C5 C 0.3635(6) 0.4230(4) 0.0654(4) 0.0269(13) Uani 1 1 d . . . C6 C 0.3348(6) 0.4773(4) -0.0348(4) 0.0349(15) Uani 1 1 d . . . H6A H 0.3073 0.5540 -0.0598 0.042 Uiso 1 1 calc R . . C7 C 0.3478(6) 0.4161(5) -0.0957(5) 0.0400(16) Uani 1 1 d . . . H7A H 0.3273 0.4502 -0.1637 0.048 Uiso 1 1 calc R . . C8 C 0.3908(6) 0.3046(5) -0.0585(4) 0.0348(15) Uani 1 1 d . . . H8A H 0.3999 0.2615 -0.1002 0.042 Uiso 1 1 calc R . . C9 C 0.4205(5) 0.2569(4) 0.0414(4) 0.0275(14) Uani 1 1 d . . . C10 C 0.4695(6) 0.1370(4) 0.0842(4) 0.0267(14) Uani 1 1 d . . . C11 C 0.3841(6) 0.0678(4) 0.1134(4) 0.0304(14) Uani 1 1 d . . . C12 C 0.2496(6) 0.1084(5) 0.1109(4) 0.0354(15) Uani 1 1 d . . . H12A H 0.2149 0.1843 0.0871 0.042 Uiso 1 1 calc R . . C13 C 0.1726(6) 0.0397(5) 0.1418(4) 0.0365(16) Uani 1 1 d . . . H13A H 0.0840 0.0676 0.1386 0.044 Uiso 1 1 calc R . . C14 C 0.2211(7) -0.0726(5) 0.1788(5) 0.0401(17) Uani 1 1 d . . . H14A H 0.1651 -0.1199 0.2005 0.048 Uiso 1 1 calc R . . C15 C 0.3465(7) -0.1140(5) 0.1839(4) 0.0374(16) Uani 1 1 d . . . H15A H 0.3773 -0.1903 0.2100 0.045 Uiso 1 1 calc R . . C16 C 0.4334(6) -0.0462(4) 0.1513(4) 0.0240(13) Uani 1 1 d . . . C17 C 0.6381(6) -0.0276(4) 0.1279(4) 0.0252(13) Uani 1 1 d . . . C18 C 0.7693(6) -0.0770(5) 0.1329(4) 0.0349(15) Uani 1 1 d . . . H18A H 0.7971 -0.1538 0.1549 0.042 Uiso 1 1 calc R . . C19 C 0.8566(6) -0.0147(5) 0.1060(4) 0.0342(15) Uani 1 1 d . . . H19A H 0.9443 -0.0488 0.1095 0.041 Uiso 1 1 calc R . . C20 C 0.8174(6) 0.0981(4) 0.0736(4) 0.0327(15) Uani 1 1 d . . . H20A H 0.8786 0.1400 0.0559 0.039 Uiso 1 1 calc R . . C21 C 0.6933(6) 0.1487(4) 0.0670(4) 0.0269(14) Uani 1 1 d . . . H21A H 0.6693 0.2256 0.0446 0.032 Uiso 1 1 calc R . . C22 C 0.5975(6) 0.0892(4) 0.0927(4) 0.0255(13) Uani 1 1 d . . . C23 C 0.3524(6) 0.4421(4) 0.4165(4) 0.0306(14) Uani 1 1 d . . . C24 C 0.3426(6) 0.5007(5) 0.4802(5) 0.0392(17) Uani 1 1 d . . . H24A H 0.3274 0.5775 0.4537 0.047 Uiso 1 1 calc R . . C25 C 0.3550(7) 0.4462(5) 0.5819(5) 0.0426(17) Uani 1 1 d . . . H25A H 0.3507 0.4851 0.6263 0.051 Uiso 1 1 calc R . . C26 C 0.3736(7) 0.3366(5) 0.6201(5) 0.0402(16) Uani 1 1 d . . . H26A H 0.3839 0.2978 0.6905 0.048 Uiso 1 1 calc R . . C27 C 0.3773(6) 0.2824(4) 0.5527(4) 0.0278(14) Uani 1 1 d . . . C28 C 0.3876(6) 0.1639(4) 0.5879(4) 0.0258(13) Uani 1 1 d . . . C29 C 0.2776(6) 0.1257(4) 0.6077(4) 0.0289(14) Uani 1 1 d . . . C30 C 0.1563(6) 0.1953(5) 0.5935(4) 0.0371(16) Uani 1 1 d . . . H30A H 0.1472 0.2713 0.5730 0.045 Uiso 1 1 calc R . . C31 C 0.0509(7) 0.1563(6) 0.6084(5) 0.0482(18) Uani 1 1 d . . . H31A H -0.0304 0.2043 0.5991 0.058 Uiso 1 1 calc R . . C32 C 0.0661(7) 0.0439(5) 0.6376(5) 0.0426(17) Uani 1 1 d . . . H32A H -0.0062 0.0173 0.6452 0.051 Uiso 1 1 calc R . . C33 C 0.1782(6) -0.0281(5) 0.6555(4) 0.0339(15) Uani 1 1 d . . . H33A H 0.1833 -0.1036 0.6773 0.041 Uiso 1 1 calc R . . C34 C 0.2886(6) 0.0101(4) 0.6415(4) 0.0276(14) Uani 1 1 d . . . C35 C 0.5155(6) -0.0230(5) 0.6324(4) 0.0311(15) Uani 1 1 d . . . C36 C 0.6362(6) -0.0956(5) 0.6444(4) 0.0315(15) Uani 1 1 d . . . H36A H 0.6430 -0.1716 0.6714 0.038 Uiso 1 1 calc R . . C37 C 0.7419(7) -0.0558(5) 0.6169(5) 0.0406(16) Uani 1 1 d . . . H37A H 0.8228 -0.1053 0.6234 0.049 Uiso 1 1 calc R . . C38 C 0.7370(6) 0.0555(5) 0.5791(5) 0.0406(16) Uani 1 1 d . . . H38A H 0.8132 0.0807 0.5603 0.049 Uiso 1 1 calc R . . C39 C 0.6224(6) 0.1263(5) 0.5698(4) 0.0303(15) Uani 1 1 d . . . H39A H 0.6195 0.2017 0.5436 0.036 Uiso 1 1 calc R . . C40 C 0.5048(6) 0.0921(4) 0.5981(4) 0.0269(14) Uani 1 1 d . . . C41 C 0.4162(6) -0.1787(4) 0.6941(5) 0.0362(16) Uani 1 1 d . . . H41A H 0.3316 -0.1930 0.7067 0.054 Uiso 1 1 calc R . . H41B H 0.4500 -0.2107 0.7593 0.054 Uiso 1 1 calc R . . H41C H 0.4745 -0.2107 0.6421 0.054 Uiso 1 1 calc R . . O1 O 1.0142(18) 0.4531(14) 0.6223(14) 0.149(6) Uiso 0.50 1 d P . . S S 0.8855(2) 0.29961(15) 0.33962(16) 0.0554(6) Uiso 1 1 d . . . O2 O 0.9514(7) 0.1899(5) 0.3706(5) 0.095(2) Uiso 1 1 d . . . O3 O 0.8270(15) 0.3066(11) 0.4387(11) 0.114(5) Uiso 0.50 1 d P . . O6 O 0.9132(12) 0.3743(9) 0.3814(9) 0.087(4) Uiso 0.50 1 d P . . O5 O 0.7701(9) 0.3329(7) 0.3048(7) 0.147(3) Uiso 1 1 d . . . C42 C 0.9692(18) 0.3344(14) 0.2000(13) 0.072(5) Uiso 0.50 1 d P . . F1 F 0.9311(12) 0.4343(9) 0.1537(9) 0.109(4) Uiso 0.50 1 d P . . F2 F 1.0894(9) 0.3354(7) 0.2032(6) 0.161(3) Uiso 1 1 d . . . F3 F 0.9566(12) 0.2711(10) 0.1551(10) 0.119(4) Uiso 0.50 1 d P . . F4 F 1.0721(19) 0.3509(14) 0.3486(15) 0.181(7) Uiso 0.50 1 d P . . F5 F 0.9340(18) 0.4772(14) 0.2758(13) 0.168(6) Uiso 0.50 1 d P . . C43 C 1.023(4) 0.394(3) 0.249(3) 0.177(12) Uiso 0.50 1 d P . . O7 O 0.9908(14) 0.2892(11) 0.8204(11) 0.108(4) Uiso 0.50 1 d P . . C44 C 1.024(3) 0.334(3) 0.906(3) 0.189(13) Uiso 0.50 1 d P . . C45 C 1.0000 0.5000 0.5000 0.242(13) Uiso 1 2 d S . . 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 0.067(4) 0.020(3) 0.027(3) -0.002(2) -0.019(3) -0.012(2) N2 0.087(5) 0.018(3) 0.030(3) 0.001(2) -0.020(3) -0.017(3) N3 0.033(3) 0.023(3) 0.021(3) -0.008(2) -0.002(2) -0.010(2) N4 0.039(3) 0.025(2) 0.019(2) -0.0085(19) -0.002(2) -0.016(2) N5 0.044(3) 0.018(2) 0.022(3) -0.001(2) -0.009(2) -0.006(2) N6 0.036(3) 0.023(3) 0.021(3) -0.005(2) -0.008(2) -0.005(2) C1 0.042(4) 0.027(3) 0.014(3) -0.001(2) -0.006(3) -0.009(3) C2 0.091(6) 0.018(3) 0.037(4) -0.004(3) -0.023(4) -0.016(3) C3 0.049(4) 0.024(3) 0.024(3) -0.005(3) -0.005(3) -0.011(3) C4 0.051(4) 0.018(3) 0.028(3) -0.004(3) -0.009(3) -0.012(3) C5 0.036(4) 0.024(3) 0.023(3) -0.009(2) -0.004(3) -0.010(3) C6 0.051(4) 0.018(3) 0.030(3) -0.001(3) -0.014(3) -0.002(3) C7 0.058(5) 0.036(4) 0.024(3) 0.001(3) -0.019(3) -0.010(3) C8 0.044(4) 0.039(4) 0.022(3) -0.011(3) -0.012(3) -0.002(3) C9 0.032(4) 0.024(3) 0.027(3) -0.005(3) -0.008(3) -0.008(3) C10 0.043(4) 0.026(3) 0.021(3) -0.011(2) -0.008(3) -0.014(3) C11 0.038(4) 0.036(3) 0.020(3) -0.008(3) -0.006(3) -0.013(3) C12 0.034(4) 0.045(4) 0.026(3) -0.011(3) 0.000(3) -0.012(3) C13 0.032(4) 0.053(4) 0.033(4) -0.017(3) -0.011(3) -0.013(3) C14 0.050(5) 0.051(4) 0.038(4) -0.020(3) -0.008(3) -0.029(4) C15 0.059(5) 0.031(3) 0.031(4) -0.011(3) -0.010(3) -0.018(3) C16 0.032(4) 0.023(3) 0.019(3) -0.009(2) -0.006(3) -0.005(3) C17 0.032(4) 0.029(3) 0.013(3) -0.007(2) -0.003(3) -0.005(3) C18 0.046(4) 0.028(3) 0.026(3) -0.006(3) -0.011(3) -0.003(3) C19 0.033(4) 0.051(4) 0.020(3) -0.015(3) -0.004(3) -0.006(3) C20 0.038(4) 0.032(3) 0.026(3) -0.005(3) 0.001(3) -0.016(3) C21 0.041(4) 0.026(3) 0.019(3) -0.006(2) -0.006(3) -0.017(3) C22 0.035(4) 0.033(3) 0.013(3) -0.010(2) -0.005(3) -0.009(3) C23 0.041(4) 0.029(3) 0.025(3) -0.011(3) -0.011(3) -0.006(3) C24 0.055(5) 0.033(4) 0.031(4) -0.019(3) -0.007(3) -0.003(3) C25 0.066(5) 0.038(4) 0.044(4) -0.026(3) -0.027(4) -0.008(3) C26 0.064(5) 0.039(4) 0.020(3) -0.009(3) -0.010(3) -0.014(3) C27 0.032(4) 0.026(3) 0.024(3) -0.009(3) -0.003(3) -0.005(3) C28 0.039(4) 0.024(3) 0.018(3) -0.011(2) -0.010(3) -0.003(3) C29 0.039(4) 0.033(3) 0.016(3) -0.008(2) -0.007(3) -0.008(3) C30 0.041(4) 0.031(3) 0.023(3) -0.003(3) -0.004(3) 0.004(3) C31 0.035(4) 0.051(4) 0.044(4) -0.010(3) -0.011(3) 0.005(3) C32 0.038(4) 0.066(5) 0.033(4) -0.017(3) -0.006(3) -0.025(4) C33 0.033(4) 0.040(4) 0.031(3) -0.011(3) -0.005(3) -0.014(3) C34 0.044(4) 0.028(3) 0.012(3) -0.003(2) -0.009(3) -0.012(3) C35 0.042(4) 0.036(3) 0.016(3) -0.010(3) -0.005(3) -0.008(3) C36 0.031(4) 0.032(3) 0.027(3) -0.010(3) -0.008(3) 0.003(3) C37 0.033(4) 0.052(4) 0.031(4) -0.015(3) -0.010(3) 0.003(3) C38 0.039(4) 0.054(4) 0.035(4) -0.010(3) -0.011(3) -0.019(3) C39 0.036(4) 0.032(3) 0.024(3) -0.013(3) -0.004(3) -0.006(3) C40 0.038(4) 0.032(3) 0.013(3) -0.010(2) -0.001(3) -0.010(3) C41 0.046(4) 0.020(3) 0.042(4) -0.008(3) -0.012(3) -0.005(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 N1 C2 1.335(7) . ? N1 C1 1.343(7) . ? N2 C3 1.330(7) . ? N2 C2 1.350(7) . ? N3 C5 1.339(6) . ? N3 C9 1.351(7) . ? N4 C16 1.326(7) . ? N4 C17 1.352(7) . ? N5 C27 1.335(7) . ? N5 C23 1.341(7) . ? N6 C34 1.361(7) . ? N6 C35 1.382(7) . ? N6 C41 1.497(6) . ? C1 C4 1.392(7) . ? C1 C5 1.488(8) . ? C3 C4 1.404(8) . ? C3 C23 1.487(8) . ? C5 C6 1.396(7) . ? C6 C7 1.369(8) . ? C7 C8 1.384(8) . ? C8 C9 1.393(7) . ? C9 C10 1.496(7) . ? C10 C22 1.391(8) . ? C10 C11 1.425(8) . ? C11 C16 1.424(7) . ? C11 C12 1.434(8) . ? C12 C13 1.342(8) . ? C13 C14 1.401(8) . ? C14 C15 1.347(9) . ? C15 C16 1.417(8) . ? C17 C18 1.418(8) . ? C17 C22 1.444(7) . ? C18 C19 1.376(8) . ? C19 C20 1.396(8) . ? C20 C21 1.353(8) . ? C21 C22 1.431(8) . ? C23 C24 1.382(8) . ? C24 C25 1.364(8) . ? C25 C26 1.358(8) . ? C26 C27 1.401(8) . ? C27 C28 1.484(7) . ? C28 C40 1.377(8) . ? C28 C29 1.400(8) . ? C29 C30 1.408(8) . ? C29 C34 1.447(7) . ? C30 C31 1.373(9) . ? C31 C32 1.403(9) . ? C32 C33 1.349(8) . ? C33 C34 1.423(8) . ? C35 C36 1.413(8) . ? C35 C40 1.440(8) . ? C36 C37 1.352(9) . ? C37 C38 1.401(9) . ? C38 C39 1.349(8) . ? C39 C40 1.433(8) . ? O1 C45 1.629(18) . ? S O3 1.397(15) . ? S O5 1.385(9) . ? S O2 1.409(6) . ? S O6 1.503(12) . ? S C42 1.877(17) . ? S C43 2.14(3) . ? O3 O6 1.414(17) . ? O6 F5 1.635(18) . ? O6 F4 1.66(2) . ? O6 C43 1.91(4) . ? C42 F1 1.262(17) . ? C42 F3 1.313(19) . ? C42 F2 1.359(18) . ? C42 C43 1.57(4) . ? F1 C43 1.73(4) . ? F2 C43 1.17(4) . ? F4 C43 1.49(3) . ? F5 C43 1.36(4) . ? O7 C44 1.71(4) . ? C45 O1 1.629(18) 2_766 ? 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 C2 N1 C1 114.8(5) . . ? C3 N2 C2 115.1(5) . . ? C5 N3 C9 117.5(4) . . ? C16 N4 C17 118.2(5) . . ? C27 N5 C23 118.1(5) . . ? C34 N6 C35 122.5(5) . . ? C34 N6 C41 119.7(5) . . ? C35 N6 C41 117.8(5) . . ? N1 C1 C4 121.4(5) . . ? N1 C1 C5 117.4(5) . . ? C4 C1 C5 121.2(5) . . ? N1 C2 N2 129.1(5) . . ? N2 C3 C4 121.0(5) . . ? N2 C3 C23 118.1(5) . . ? C4 C3 C23 120.9(5) . . ? C1 C4 C3 118.5(5) . . ? N3 C5 C6 123.7(5) . . ? N3 C5 C1 116.0(5) . . ? C6 C5 C1 120.3(5) . . ? C7 C6 C5 117.6(5) . . ? C6 C7 C8 120.2(5) . . ? C9 C8 C7 118.6(5) . . ? N3 C9 C8 122.3(5) . . ? N3 C9 C10 117.2(5) . . ? C8 C9 C10 120.5(5) . . ? C22 C10 C11 118.1(5) . . ? C22 C10 C9 122.5(5) . . ? C11 C10 C9 119.3(5) . . ? C10 C11 C16 118.4(6) . . ? C10 C11 C12 122.8(5) . . ? C16 C11 C12 118.7(5) . . ? C13 C12 C11 120.4(6) . . ? C12 C13 C14 120.9(6) . . ? C15 C14 C13 120.6(6) . . ? C14 C15 C16 121.5(6) . . ? N4 C16 C11 123.8(5) . . ? N4 C16 C15 118.4(5) . . ? C11 C16 C15 117.9(6) . . ? N4 C17 C18 118.2(5) . . ? N4 C17 C22 122.6(5) . . ? C18 C17 C22 119.2(5) . . ? C19 C18 C17 120.5(5) . . ? C18 C19 C20 120.5(6) . . ? C21 C20 C19 121.0(6) . . ? C20 C21 C22 121.7(5) . . ? C10 C22 C17 118.7(5) . . ? C10 C22 C21 124.1(5) . . ? C17 C22 C21 117.2(5) . . ? N5 C23 C24 122.2(5) . . ? N5 C23 C3 115.1(5) . . ? C24 C23 C3 122.7(5) . . ? C25 C24 C23 118.8(6) . . ? C26 C25 C24 120.4(6) . . ? C25 C26 C27 118.1(5) . . ? N5 C27 C26 122.3(5) . . ? N5 C27 C28 115.0(5) . . ? C26 C27 C28 122.7(5) . . ? C40 C28 C29 120.1(5) . . ? C40 C28 C27 120.5(5) . . ? C29 C28 C27 119.4(5) . . ? C28 C29 C30 122.8(5) . . ? C28 C29 C34 119.1(5) . . ? C30 C29 C34 118.1(6) . . ? C31 C30 C29 121.8(6) . . ? C30 C31 C32 118.4(6) . . ? C33 C32 C31 123.3(6) . . ? C32 C33 C34 119.4(6) . . ? N6 C34 C33 121.7(5) . . ? N6 C34 C29 119.3(5) . . ? C33 C34 C29 118.9(5) . . ? N6 C35 C36 121.9(5) . . ? N6 C35 C40 118.1(5) . . ? C36 C35 C40 120.0(6) . . ? C37 C36 C35 119.3(6) . . ? C36 C37 C38 122.7(6) . . ? C39 C38 C37 119.0(6) . . ? C38 C39 C40 122.5(6) . . ? C28 C40 C35 120.8(5) . . ? C28 C40 C39 122.8(5) . . ? C35 C40 C39 116.4(5) . . ? O3 S O5 93.4(7) . . ? O3 S O2 97.9(6) . . ? O5 S O2 122.1(5) . . ? O3 S O6 58.2(7) . . ? O5 S O6 116.4(6) . . ? O2 S O6 117.7(6) . . ? O3 S C42 161.7(8) . . ? O5 S C42 88.7(7) . . ? O2 S C42 96.3(6) . . ? O6 S C42 104.8(8) . . ? O3 S C43 118.4(12) . . ? O5 S C43 115.6(11) . . ? O2 S C43 107.9(12) . . ? O6 S C43 60.2(12) . . ? C42 S C43 45.6(11) . . ? S O3 O6 64.6(8) . . ? O3 O6 S 57.1(7) . . ? O3 O6 F5 141.9(12) . . ? S O6 F5 101.7(9) . . ? O3 O6 F4 133.4(12) . . ? S O6 F4 100.9(9) . . ? F5 O6 F4 77.7(11) . . ? O3 O6 C43 133.8(15) . . ? S O6 C43 76.7(12) . . ? F5 O6 C43 44.4(11) . . ? F4 O6 C43 48.7(12) . . ? F1 C42 F3 114.1(16) . . ? F1 C42 F2 97.9(13) . . ? F3 C42 F2 118.3(16) . . ? F1 C42 C43 74.4(17) . . ? F3 C42 C43 165(2) . . ? F2 C42 C43 46.4(15) . . ? F1 C42 S 109.5(13) . . ? F3 C42 S 110.9(12) . . ? F2 C42 S 105.0(11) . . ? C43 C42 S 76.1(15) . . ? C42 F1 C43 61.0(15) . . ? C43 F2 C42 76.5(19) . . ? C43 F4 O6 74.2(18) . . ? C43 F5 O6 78.5(18) . . ? F2 C43 F5 164(4) . . ? F2 C43 F4 103(3) . . ? F5 C43 F4 93(3) . . ? F2 C43 C42 57.1(18) . . ? F5 C43 C42 113(3) . . ? F4 C43 C42 129(3) . . ? F2 C43 F1 83(2) . . ? F5 C43 F1 81(2) . . ? F4 C43 F1 165(3) . . ? C42 C43 F1 44.6(12) . . ? F2 C43 O6 134(3) . . ? F5 C43 O6 57.1(17) . . ? F4 C43 O6 57.1(15) . . ? C42 C43 O6 101(2) . . ? F1 C43 O6 109(2) . . ? F2 C43 S 98(2) . . ? F5 C43 S 85(2) . . ? F4 C43 S 82.6(17) . . ? C42 C43 S 58.4(13) . . ? F1 C43 S 83.2(15) . . ? O6 C43 S 43.1(8) . . ? O1 C45 O1 180.000(2) 2_766 . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.342 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.112