data_global _journal_coden_Cambridge 1048 loop_ _publ_author_name 'Mark Harmer' 'Liane M. Grieco' 'Christopher Junk' 'Robert Miller' 'Vsevolod Rostovtsev' 'Jemma Vickery' 'Stella Work' _publ_contact_author_name 'Mark Harmer' _publ_contact_author_email MARK.A.HARMER@USA.DUPONT.COM _publ_section_title ; Catalytic Reactions Using Superacids in New Types of Ionic Liquids ; # Attachment 'superacid.cif' data_04307 _database_code_depnum_ccdc_archive 'CCDC 715667' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 F4 N2 O3 S' _chemical_formula_weight 292.26 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' F F 0.0171 0.0103 '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)/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 8.770(8) _cell_length_b 9.766(9) _cell_length_c 14.282(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.363(12) _cell_angle_gamma 90.00 _cell_volume 1217.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description iregblok _exptl_crystal_colour colourless _exptl_crystal_size_min 0.440 _exptl_crystal_size_mid 0.480 _exptl_crystal_size_max 0.500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 0.320 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9216 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 28.34 _reflns_number_total 2998 _reflns_number_gt 2547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-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^)+(0.0546P)^2^+0.5848P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.040(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2998 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _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 0.27800(5) -0.29370(4) 0.97758(3) 0.03188(16) Uani 1 1 d . . . F1 F 0.28699(14) -0.17371(12) 1.14132(8) 0.0470(3) Uani 1 1 d . . . C1' C 0.3801(2) -0.24561(17) 1.09038(12) 0.0314(4) Uani 1 1 d . . . O1 O 0.2412(2) -0.16460(15) 0.93255(12) 0.0563(4) Uani 1 1 d . . . F2 F 0.49735(15) -0.16205(14) 1.07328(10) 0.0567(4) Uani 1 1 d . . . O2 O 0.38982(17) -0.37395(15) 0.93468(9) 0.0441(4) Uani 1 1 d . . . C2' C 0.4482(3) -0.3662(2) 1.14725(14) 0.0447(5) Uani 1 1 d . . . H2'A H 0.5064 -0.4255 1.1082 0.054 Uiso 1 1 calc R . . F3 F 0.54003(18) -0.31679(17) 1.22186(10) 0.0698(5) Uani 1 1 d . . . O3 O 0.14971(16) -0.37227(15) 1.00220(12) 0.0507(4) Uani 1 1 d . . . N1 N 0.13816(18) 0.20346(14) 0.93594(10) 0.0330(3) Uani 1 1 d . . . F4 F 0.3360(2) -0.43649(15) 1.18259(10) 0.0687(4) Uani 1 1 d . . . C2 C 0.1251(2) 0.33310(18) 0.90932(13) 0.0333(4) Uani 1 1 d . . . H2A H 0.1365 0.4089 0.9488 0.040 Uiso 1 1 calc R . . N3 N 0.09329(17) 0.33646(15) 0.81721(10) 0.0323(3) Uani 1 1 d . . . C4 C 0.0853(2) 0.20460(18) 0.78371(13) 0.0366(4) Uani 1 1 d . . . H4A H 0.0644 0.1778 0.7213 0.044 Uiso 1 1 calc R . . C5 C 0.1133(2) 0.12151(18) 0.85860(13) 0.0352(4) Uani 1 1 d . . . H5A H 0.1154 0.0263 0.8578 0.042 Uiso 1 1 calc R . . C6 C 0.1639(3) 0.1533(2) 1.03329(15) 0.0509(5) Uani 1 1 d . . . H6A H 0.2332 0.0758 1.0349 0.061 Uiso 1 1 calc R . . H6B H 0.0673 0.1214 1.0532 0.061 Uiso 1 1 calc R . . C7 C 0.2285(3) 0.2583(3) 1.10081(16) 0.0551(6) Uani 1 1 d . . . H7A H 0.2479 0.2179 1.1621 0.083 Uiso 1 1 calc R . . H7B H 0.1569 0.3322 1.1035 0.083 Uiso 1 1 calc R . . H7C H 0.3226 0.2926 1.0806 0.083 Uiso 1 1 calc R . . C8 C 0.0653(3) 0.4606(2) 0.76051(15) 0.0469(5) Uani 1 1 d . . . H8A H 0.1144 0.5371 0.7929 0.070 Uiso 1 1 calc R . . H8B H -0.0429 0.4771 0.7505 0.070 Uiso 1 1 calc R . . H8C H 0.1061 0.4488 0.7010 0.070 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 0.0387(3) 0.0225(2) 0.0332(2) -0.00285(15) -0.00341(17) 0.00667(15) F1 0.0567(7) 0.0397(6) 0.0449(7) -0.0153(5) 0.0062(5) 0.0153(5) C1' 0.0330(8) 0.0275(8) 0.0338(8) -0.0060(6) 0.0029(6) -0.0003(6) O1 0.0843(12) 0.0306(7) 0.0501(9) 0.0045(6) -0.0143(8) 0.0165(7) F2 0.0507(7) 0.0501(7) 0.0685(9) -0.0063(6) 0.0020(6) -0.0222(6) O2 0.0559(8) 0.0445(8) 0.0322(7) -0.0034(6) 0.0066(6) 0.0159(6) C2' 0.0562(12) 0.0423(10) 0.0338(10) -0.0051(8) -0.0061(8) 0.0147(9) F3 0.0779(10) 0.0784(10) 0.0472(8) -0.0118(7) -0.0262(7) 0.0178(8) O3 0.0377(7) 0.0414(8) 0.0719(10) -0.0143(7) -0.0003(7) -0.0057(6) N1 0.0408(8) 0.0258(7) 0.0326(8) 0.0014(5) 0.0052(6) 0.0004(6) F4 0.1032(12) 0.0476(8) 0.0549(8) 0.0143(6) 0.0056(8) -0.0083(8) C2 0.0405(9) 0.0263(8) 0.0337(9) -0.0015(6) 0.0079(7) -0.0020(7) N3 0.0372(8) 0.0267(7) 0.0333(8) 0.0024(6) 0.0059(6) 0.0020(6) C4 0.0431(10) 0.0315(9) 0.0350(9) -0.0050(7) 0.0020(7) 0.0012(7) C5 0.0406(9) 0.0247(8) 0.0404(10) -0.0031(7) 0.0041(7) 0.0020(7) C6 0.0779(15) 0.0397(10) 0.0344(10) 0.0087(8) 0.0019(10) -0.0036(10) C7 0.0606(14) 0.0665(15) 0.0369(11) -0.0003(10) -0.0029(9) -0.0047(12) C8 0.0589(12) 0.0339(9) 0.0474(11) 0.0141(8) 0.0032(9) 0.0026(9) _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 O3 1.4325(18) . ? S1 O2 1.4366(15) . ? S1 O1 1.4383(17) . ? S1 C1' 1.830(2) . ? F1 C1' 1.342(2) . ? C1' F2 1.353(2) . ? C1' C2' 1.521(3) . ? C2' F4 1.337(3) . ? C2' F3 1.362(3) . ? C2' H2'A 0.9800 . ? N1 C2 1.324(2) . ? N1 C5 1.365(2) . ? N1 C6 1.471(3) . ? C2 N3 1.319(3) . ? C2 H2A 0.9300 . ? N3 C4 1.373(2) . ? N3 C8 1.466(2) . ? C4 C5 1.347(3) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.483(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 O3 S1 O2 113.30(11) . . ? O3 S1 O1 115.51(11) . . ? O2 S1 O1 114.90(11) . . ? O3 S1 C1' 104.62(10) . . ? O2 S1 C1' 102.59(10) . . ? O1 S1 C1' 103.86(10) . . ? F1 C1' F2 107.08(15) . . ? F1 C1' C2' 110.12(16) . . ? F2 C1' C2' 107.26(16) . . ? F1 C1' S1 109.81(13) . . ? F2 C1' S1 108.28(13) . . ? C2' C1' S1 114.01(13) . . ? F4 C2' F3 106.79(18) . . ? F4 C2' C1' 109.48(17) . . ? F3 C2' C1' 108.50(17) . . ? F4 C2' H2'A 110.7 . . ? F3 C2' H2'A 110.7 . . ? C1' C2' H2'A 110.7 . . ? C2 N1 C5 108.98(16) . . ? C2 N1 C6 126.24(16) . . ? C5 N1 C6 124.64(16) . . ? N3 C2 N1 108.34(16) . . ? N3 C2 H2A 125.8 . . ? N1 C2 H2A 125.8 . . ? C2 N3 C4 108.86(15) . . ? C2 N3 C8 125.48(16) . . ? C4 N3 C8 125.62(17) . . ? C5 C4 N3 106.78(17) . . ? C5 C4 H4A 126.6 . . ? N3 C4 H4A 126.6 . . ? C4 C5 N1 107.04(17) . . ? C4 C5 H5A 126.5 . . ? N1 C5 H5A 126.5 . . ? N1 C6 C7 113.57(18) . . ? N1 C6 H6A 108.9 . . ? C7 C6 H6A 108.9 . . ? N1 C6 H6B 108.9 . . ? C7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 O3 S1 C1' F1 -58.90(15) . . . . ? O2 S1 C1' F1 -177.40(12) . . . . ? O1 S1 C1' F1 62.63(15) . . . . ? O3 S1 C1' F2 -175.50(12) . . . . ? O2 S1 C1' F2 65.99(15) . . . . ? O1 S1 C1' F2 -53.97(15) . . . . ? O3 S1 C1' C2' 65.21(16) . . . . ? O2 S1 C1' C2' -53.29(16) . . . . ? O1 S1 C1' C2' -173.26(15) . . . . ? F1 C1' C2' F4 51.0(2) . . . . ? F2 C1' C2' F4 167.16(15) . . . . ? S1 C1' C2' F4 -72.98(18) . . . . ? F1 C1' C2' F3 -65.2(2) . . . . ? F2 C1' C2' F3 51.0(2) . . . . ? S1 C1' C2' F3 170.83(14) . . . . ? C5 N1 C2 N3 -0.3(2) . . . . ? C6 N1 C2 N3 -176.08(18) . . . . ? N1 C2 N3 C4 0.2(2) . . . . ? N1 C2 N3 C8 178.02(17) . . . . ? C2 N3 C4 C5 0.0(2) . . . . ? C8 N3 C4 C5 -177.86(17) . . . . ? N3 C4 C5 N1 -0.1(2) . . . . ? C2 N1 C5 C4 0.2(2) . . . . ? C6 N1 C5 C4 176.15(19) . . . . ? C2 N1 C6 C7 -20.4(3) . . . . ? C5 N1 C6 C7 164.43(19) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.411 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.063 #===END data_05219 _database_code_depnum_ccdc_archive 'CCDC 715668' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H11 F9 N2 O3 S' _chemical_formula_weight 410.27 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' F F 0.0171 0.0103 '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 P21/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 9.178(4) _cell_length_b 34.444(13) _cell_length_c 10.022(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.711(7) _cell_angle_gamma 90.00 _cell_volume 3167(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description iregplate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_max 0.400 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.317 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11333 _diffrn_reflns_av_R_equivalents 0.173 _diffrn_reflns_av_sigmaI/netI 0.0954 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.70 _reflns_number_total 7998 _reflns_number_gt 6121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-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^)+(0.1241P)^2^+1.7705P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11349 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1705 _refine_ls_R_factor_gt 0.0916 _refine_ls_wR_factor_ref 0.2580 _refine_ls_wR_factor_gt 0.2183 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 -0.01361(13) 0.07919(3) 0.35514(12) 0.0310(3) Uani 1 1 d . . . F1 F -0.1601(3) 0.11923(8) 0.5246(3) 0.0411(7) Uani 1 1 d . . . F2 F 0.0744(3) 0.12955(9) 0.5329(3) 0.0515(8) Uani 1 1 d . . . F3 F -0.1537(4) 0.15466(9) 0.2612(3) 0.0559(9) Uani 1 1 d . . . F4 F 0.0625(4) 0.17319(10) 0.3224(4) 0.0747(12) Uani 1 1 d . . . F5 F -0.2773(4) 0.18891(10) 0.4522(4) 0.0714(11) Uani 1 1 d . . . F6 F -0.0774(5) 0.19711(11) 0.5679(4) 0.0854(14) Uani 1 1 d . . . F7 F -0.1553(8) 0.23441(12) 0.2548(6) 0.119(2) Uani 1 1 d . . . F8 F 0.0123(6) 0.24855(14) 0.3922(8) 0.149(3) Uani 1 1 d . . . F9 F -0.2036(6) 0.26050(11) 0.4407(6) 0.1133(18) Uani 1 1 d . . . O1 O 0.0234(4) 0.05204(10) 0.4594(3) 0.0438(9) Uani 1 1 d . . . O2 O -0.1516(4) 0.07173(10) 0.2883(4) 0.0448(9) Uani 1 1 d . . . O3 O 0.1026(4) 0.08838(10) 0.2689(3) 0.0409(9) Uani 1 1 d . . . C7 C -0.0419(5) 0.12433(14) 0.4490(5) 0.0324(11) Uani 1 1 d . . . C8 C -0.0651(6) 0.16158(13) 0.3676(5) 0.0352(11) Uani 1 1 d . . . C9 C -0.1317(7) 0.19592(16) 0.4431(7) 0.0550(16) Uani 1 1 d . . . C10 C -0.1200(10) 0.23520(19) 0.3802(10) 0.083(3) Uani 1 1 d . . . S2 S 0.49818(14) 0.08233(3) 0.81277(11) 0.0319(3) Uani 1 1 d . . . F10 F 0.3353(4) 0.13283(10) 0.9292(3) 0.0573(9) Uani 1 1 d . . . F11 F 0.5661(4) 0.14605(9) 0.9415(3) 0.0597(10) Uani 1 1 d . . . F12 F 0.3589(5) 0.14483(9) 0.6450(3) 0.0676(11) Uani 1 1 d . . . F13 F 0.5699(4) 0.16869(10) 0.6939(4) 0.0675(10) Uani 1 1 d . . . F14 F 0.2264(5) 0.19487(13) 0.7872(6) 0.120(2) Uani 1 1 d . . . F15 F 0.4250(7) 0.21432(12) 0.8849(5) 0.117(2) Uani 1 1 d . . . F16 F 0.3432(8) 0.21855(13) 0.5479(6) 0.128(2) Uani 1 1 d . . . F17 F 0.5112(6) 0.24502(14) 0.6588(7) 0.131(2) Uani 1 1 d . . . F18 F 0.2998(7) 0.26146(11) 0.6946(6) 0.1219(19) Uani 1 1 d . . . O4 O 0.5432(5) 0.06463(11) 0.9375(3) 0.0495(10) Uani 1 1 d . . . O5 O 0.3617(4) 0.06786(9) 0.7573(3) 0.0392(8) Uani 1 1 d . . . O6 O 0.6099(4) 0.08597(10) 0.7189(3) 0.0400(9) Uani 1 1 d . . . C17 C 0.4573(5) 0.13280(15) 0.8595(5) 0.0350(11) Uani 1 1 d . . . C18 C 0.4383(6) 0.16147(14) 0.7427(5) 0.0388(12) Uani 1 1 d . . . C19 C 0.3702(8) 0.20038(17) 0.7731(7) 0.0622(18) Uani 1 1 d . . . C20 C 0.3766(11) 0.2319(2) 0.6638(10) 0.083(2) Uani 1 1 d . . . N1 N 0.3511(4) 0.02164(10) 0.4098(4) 0.0291(8) Uani 1 1 d . . . N2 N 0.4516(4) 0.07452(11) 0.3468(4) 0.0320(9) Uani 1 1 d . . . C1 C 0.3889(5) 0.05719(13) 0.4472(5) 0.0315(11) Uani 1 1 d . . . H1A H 0.3737 0.0681 0.5306 0.038 Uiso 1 1 calc R . . C2 C 0.4481(6) 0.05009(15) 0.2397(5) 0.0384(12) Uani 1 1 d . . . H2A H 0.4817 0.0554 0.1550 0.046 Uiso 1 1 calc R . . C3 C 0.3866(6) 0.01676(15) 0.2798(5) 0.0389(12) Uani 1 1 d . . . H3A H 0.3713 -0.0054 0.2285 0.047 Uiso 1 1 calc R . . C4 C 0.2809(5) -0.00695(15) 0.4927(5) 0.0420(13) Uani 1 1 d . . . H4A H 0.3064 -0.0021 0.5848 0.063 Uiso 1 1 calc R . . H4B H 0.3128 -0.0325 0.4686 0.063 Uiso 1 1 calc R . . H4C H 0.1771 -0.0052 0.4795 0.063 Uiso 1 1 calc R . . C5 C 0.5143(6) 0.11404(16) 0.3485(7) 0.0535(15) Uani 1 1 d . . . H5A H 0.6040 0.1139 0.2997 0.064 Uiso 1 1 calc R . . H5B H 0.5384 0.1213 0.4400 0.064 Uiso 1 1 calc R . . C6 C 0.4144(8) 0.14359(17) 0.2889(7) 0.0627(18) Uani 1 1 d . . . H6A H 0.4605 0.1686 0.2926 0.094 Uiso 1 1 calc R . . H6B H 0.3262 0.1444 0.3379 0.094 Uiso 1 1 calc R . . H6C H 0.3918 0.1369 0.1976 0.094 Uiso 1 1 calc R . . N3 N 0.1214(4) 0.02591(10) 0.8999(4) 0.0272(8) Uani 1 1 d . . . N4 N -0.0175(4) 0.07549(11) 0.9125(4) 0.0321(9) Uani 1 1 d . . . C11 C 0.0842(5) 0.05496(13) 0.9769(5) 0.0296(10) Uani 1 1 d . . . H11A H 0.1227 0.0602 1.0619 0.036 Uiso 1 1 calc R . . C12 C -0.0470(6) 0.05860(14) 0.7921(5) 0.0374(12) Uani 1 1 d . . . H12A H -0.1153 0.0670 0.7280 0.045 Uiso 1 1 calc R . . C13 C 0.0402(5) 0.02773(14) 0.7829(4) 0.0339(11) Uani 1 1 d . . . H13A H 0.0450 0.0107 0.7110 0.041 Uiso 1 1 calc R . . C14 C 0.2339(5) -0.00283(15) 0.9324(5) 0.0376(12) Uani 1 1 d . . . H14A H 0.2159 -0.0141 1.0179 0.056 Uiso 1 1 calc R . . H14B H 0.3277 0.0095 0.9350 0.056 Uiso 1 1 calc R . . H14C H 0.2322 -0.0228 0.8655 0.056 Uiso 1 1 calc R . . C15 C -0.0917(7) 0.10984(15) 0.9677(6) 0.0472(14) Uani 1 1 d . . . H15A H -0.1955 0.1047 0.9705 0.057 Uiso 1 1 calc R . . H15B H -0.0558 0.1143 1.0584 0.057 Uiso 1 1 calc R . . C16 C -0.0678(11) 0.1443(2) 0.8888(10) 0.107(3) Uani 1 1 d . . . H16A H -0.1470 0.1621 0.8999 0.161 Uiso 1 1 calc R . . H16B H -0.0624 0.1373 0.7964 0.161 Uiso 1 1 calc R . . H16C H 0.0219 0.1564 0.9178 0.161 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 0.0329(7) 0.0241(6) 0.0359(7) -0.0042(5) 0.0000(5) 0.0015(5) F1 0.0473(18) 0.0363(16) 0.0407(17) 0.0003(12) 0.0158(14) 0.0021(13) F2 0.0492(19) 0.0476(19) 0.056(2) -0.0170(15) -0.0186(16) 0.0005(15) F3 0.079(3) 0.0396(18) 0.0482(19) 0.0079(14) -0.0089(18) 0.0109(17) F4 0.055(2) 0.046(2) 0.126(3) 0.029(2) 0.043(2) 0.0059(17) F5 0.060(2) 0.046(2) 0.110(3) -0.0046(19) 0.034(2) 0.0071(17) F6 0.134(4) 0.048(2) 0.074(3) -0.0268(19) -0.014(3) 0.015(2) F7 0.204(7) 0.053(3) 0.102(4) 0.034(3) 0.039(4) 0.026(3) F8 0.094(4) 0.049(3) 0.307(8) 0.009(4) 0.042(5) -0.026(3) F9 0.141(4) 0.033(2) 0.168(5) -0.008(2) 0.045(4) 0.014(2) O1 0.047(2) 0.0333(19) 0.051(2) 0.0051(16) 0.0018(18) 0.0082(17) O2 0.043(2) 0.0293(19) 0.061(2) -0.0142(16) -0.0143(18) -0.0022(15) O3 0.041(2) 0.043(2) 0.039(2) -0.0098(15) 0.0118(16) 0.0007(17) C7 0.026(3) 0.035(3) 0.037(3) -0.003(2) 0.001(2) -0.003(2) C8 0.037(3) 0.025(3) 0.043(3) 0.000(2) 0.007(2) -0.002(2) C9 0.064(4) 0.032(3) 0.069(4) -0.006(3) 0.012(3) -0.001(3) C10 0.103(7) 0.028(4) 0.122(7) 0.002(4) 0.040(6) 0.003(4) S2 0.0391(7) 0.0279(6) 0.0288(6) 0.0007(5) 0.0013(5) 0.0030(5) F10 0.057(2) 0.058(2) 0.059(2) -0.0012(16) 0.0311(17) 0.0110(17) F11 0.072(2) 0.048(2) 0.057(2) -0.0218(15) -0.0222(18) 0.0046(17) F12 0.097(3) 0.0376(19) 0.066(2) 0.0107(16) -0.034(2) -0.0034(18) F13 0.067(2) 0.049(2) 0.089(3) 0.0175(18) 0.034(2) 0.0047(18) F14 0.075(3) 0.064(3) 0.224(6) 0.041(3) 0.067(4) 0.029(2) F15 0.213(6) 0.053(3) 0.084(3) -0.030(2) -0.016(4) 0.041(3) F16 0.217(7) 0.050(3) 0.117(4) 0.032(3) -0.027(4) 0.008(3) F17 0.117(4) 0.059(3) 0.218(6) 0.047(3) 0.029(4) -0.011(3) F18 0.148(5) 0.034(2) 0.185(5) 0.018(3) 0.028(4) 0.026(3) O4 0.071(3) 0.046(2) 0.031(2) 0.0063(16) -0.0065(18) 0.010(2) O5 0.044(2) 0.0282(18) 0.045(2) 0.0012(15) -0.0048(16) -0.0053(15) O6 0.040(2) 0.034(2) 0.046(2) -0.0028(15) 0.0143(17) 0.0028(16) C17 0.031(3) 0.041(3) 0.034(3) -0.011(2) 0.006(2) -0.002(2) C18 0.041(3) 0.030(3) 0.046(3) -0.002(2) 0.002(2) -0.003(2) C19 0.071(5) 0.033(3) 0.085(5) 0.002(3) 0.024(4) 0.005(3) C20 0.105(7) 0.027(4) 0.117(7) 0.009(4) 0.001(6) 0.007(4) N1 0.026(2) 0.026(2) 0.035(2) 0.0016(16) -0.0013(17) 0.0027(16) N2 0.031(2) 0.028(2) 0.037(2) 0.0006(17) 0.0025(18) 0.0011(17) C1 0.036(3) 0.031(3) 0.027(2) -0.0044(19) -0.001(2) 0.004(2) C2 0.045(3) 0.044(3) 0.027(3) 0.001(2) 0.009(2) 0.013(2) C3 0.052(3) 0.035(3) 0.030(3) -0.005(2) -0.002(2) 0.014(2) C4 0.030(3) 0.041(3) 0.055(3) 0.016(2) 0.002(2) 0.001(2) C5 0.043(3) 0.043(3) 0.075(4) 0.002(3) 0.003(3) -0.003(3) C6 0.059(4) 0.036(3) 0.092(5) 0.016(3) -0.011(4) -0.005(3) N3 0.0212(19) 0.028(2) 0.032(2) 0.0000(16) -0.0002(16) -0.0024(15) N4 0.035(2) 0.028(2) 0.033(2) -0.0008(16) 0.0017(18) -0.0008(18) C11 0.034(3) 0.026(2) 0.028(2) -0.0035(18) -0.003(2) 0.000(2) C12 0.041(3) 0.039(3) 0.032(3) 0.001(2) -0.006(2) 0.003(2) C13 0.036(3) 0.039(3) 0.026(2) -0.004(2) -0.003(2) 0.002(2) C14 0.037(3) 0.037(3) 0.039(3) 0.004(2) 0.000(2) 0.000(2) C15 0.054(4) 0.039(3) 0.049(3) -0.008(2) 0.002(3) 0.013(3) C16 0.118(7) 0.036(4) 0.170(9) 0.013(5) 0.073(7) 0.014(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 S1 O3 1.428(4) . ? S1 O1 1.435(4) . ? S1 O2 1.438(4) . ? S1 C7 1.840(5) . ? F1 C7 1.353(5) . ? F2 C7 1.351(5) . ? F3 C8 1.342(6) . ? F4 C8 1.330(6) . ? F5 C9 1.364(7) . ? F6 C9 1.333(7) . ? F7 C10 1.289(10) . ? F8 C10 1.301(9) . ? F9 C10 1.320(8) . ? C7 C8 1.532(7) . ? C8 C9 1.540(8) . ? C9 C10 1.498(9) . ? S2 O6 1.417(3) . ? S2 O4 1.440(3) . ? S2 O5 1.444(4) . ? S2 C17 1.842(5) . ? F10 C17 1.338(6) . ? F11 C17 1.353(6) . ? F12 C18 1.332(6) . ? F13 C18 1.340(6) . ? F14 C19 1.345(8) . ? F15 C19 1.306(8) . ? F16 C20 1.278(9) . ? F17 C20 1.319(10) . ? F18 C20 1.282(8) . ? C17 C18 1.538(7) . ? C18 C19 1.514(8) . ? C19 C20 1.543(10) . ? N1 C1 1.324(6) . ? N1 C3 1.362(6) . ? N1 C4 1.452(6) . ? N2 C1 1.317(6) . ? N2 C2 1.364(6) . ? N2 C5 1.478(7) . ? C1 H1A 0.9300 . ? C2 C3 1.346(7) . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.483(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? N3 C11 1.315(6) . ? N3 C13 1.372(6) . ? N3 C14 1.460(6) . ? N4 C11 1.324(6) . ? N4 C12 1.359(6) . ? N4 C15 1.481(6) . ? C11 H11A 0.9300 . ? C12 C13 1.336(7) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.447(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 O3 S1 O1 114.8(2) . . ? O3 S1 O2 114.9(2) . . ? O1 S1 O2 114.1(2) . . ? O3 S1 C7 104.0(2) . . ? O1 S1 C7 102.3(2) . . ? O2 S1 C7 104.7(2) . . ? F2 C7 F1 107.5(4) . . ? F2 C7 C8 108.4(4) . . ? F1 C7 C8 107.8(4) . . ? F2 C7 S1 108.0(3) . . ? F1 C7 S1 107.7(3) . . ? C8 C7 S1 117.1(3) . . ? F4 C8 F3 107.5(4) . . ? F4 C8 C7 108.9(4) . . ? F3 C8 C7 110.2(4) . . ? F4 C8 C9 107.6(4) . . ? F3 C8 C9 106.7(4) . . ? C7 C8 C9 115.6(4) . . ? F6 C9 F5 106.4(5) . . ? F6 C9 C10 109.7(6) . . ? F5 C9 C10 105.7(6) . . ? F6 C9 C8 110.0(5) . . ? F5 C9 C8 107.5(5) . . ? C10 C9 C8 116.9(6) . . ? F7 C10 F8 107.7(8) . . ? F7 C10 F9 109.2(8) . . ? F8 C10 F9 106.2(7) . . ? F7 C10 C9 111.8(7) . . ? F8 C10 C9 111.0(8) . . ? F9 C10 C9 110.7(7) . . ? O6 S2 O4 114.8(2) . . ? O6 S2 O5 114.3(2) . . ? O4 S2 O5 114.3(2) . . ? O6 S2 C17 104.0(2) . . ? O4 S2 C17 103.5(2) . . ? O5 S2 C17 104.0(2) . . ? F10 C17 F11 107.3(4) . . ? F10 C17 C18 108.6(4) . . ? F11 C17 C18 108.1(4) . . ? F10 C17 S2 108.3(3) . . ? F11 C17 S2 108.7(3) . . ? C18 C17 S2 115.6(3) . . ? F12 C18 F13 106.9(4) . . ? F12 C18 C19 108.0(5) . . ? F13 C18 C19 106.9(4) . . ? F12 C18 C17 109.3(4) . . ? F13 C18 C17 108.3(4) . . ? C19 C18 C17 117.0(5) . . ? F15 C19 F14 108.4(6) . . ? F15 C19 C18 110.3(6) . . ? F14 C19 C18 107.9(5) . . ? F15 C19 C20 109.2(6) . . ? F14 C19 C20 103.4(6) . . ? C18 C19 C20 117.1(6) . . ? F16 C20 F18 112.7(8) . . ? F16 C20 F17 106.7(8) . . ? F18 C20 F17 105.0(7) . . ? F16 C20 C19 112.3(6) . . ? F18 C20 C19 110.8(8) . . ? F17 C20 C19 108.9(7) . . ? C1 N1 C3 108.5(4) . . ? C1 N1 C4 125.6(4) . . ? C3 N1 C4 125.9(4) . . ? C1 N2 C2 108.7(4) . . ? C1 N2 C5 126.0(4) . . ? C2 N2 C5 125.2(4) . . ? N2 C1 N1 108.6(4) . . ? N2 C1 H1A 125.7 . . ? N1 C1 H1A 125.7 . . ? C3 C2 N2 106.9(4) . . ? C3 C2 H2A 126.5 . . ? N2 C2 H2A 126.5 . . ? C2 C3 N1 107.1(4) . . ? C2 C3 H3A 126.4 . . ? N1 C3 H3A 126.4 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 113.1(5) . . ? N2 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? N2 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C11 N3 C13 108.9(4) . . ? C11 N3 C14 125.4(4) . . ? C13 N3 C14 125.7(4) . . ? C11 N4 C12 108.9(4) . . ? C11 N4 C15 124.8(4) . . ? C12 N4 C15 126.3(4) . . ? N3 C11 N4 108.1(4) . . ? N3 C11 H11A 125.9 . . ? N4 C11 H11A 125.9 . . ? C13 C12 N4 107.3(4) . . ? C13 C12 H12A 126.3 . . ? N4 C12 H12A 126.3 . . ? C12 C13 N3 106.8(4) . . ? C12 C13 H13A 126.6 . . ? N3 C13 H13A 126.6 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 N4 111.9(5) . . ? C16 C15 H15A 109.2 . . ? N4 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? N4 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? 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 . . ? 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 O3 S1 C7 F2 -69.8(4) . . . . ? O1 S1 C7 F2 50.0(4) . . . . ? O2 S1 C7 F2 169.3(3) . . . . ? O3 S1 C7 F1 174.3(3) . . . . ? O1 S1 C7 F1 -65.9(4) . . . . ? O2 S1 C7 F1 53.4(4) . . . . ? O3 S1 C7 C8 52.7(4) . . . . ? O1 S1 C7 C8 172.6(4) . . . . ? O2 S1 C7 C8 -68.2(4) . . . . ? F2 C7 C8 F4 46.6(5) . . . . ? F1 C7 C8 F4 162.6(4) . . . . ? S1 C7 C8 F4 -75.8(5) . . . . ? F2 C7 C8 F3 164.3(4) . . . . ? F1 C7 C8 F3 -79.6(5) . . . . ? S1 C7 C8 F3 41.9(5) . . . . ? F2 C7 C8 C9 -74.7(5) . . . . ? F1 C7 C8 C9 41.4(6) . . . . ? S1 C7 C8 C9 162.9(4) . . . . ? F4 C8 C9 F6 -83.5(6) . . . . ? F3 C8 C9 F6 161.3(5) . . . . ? C7 C8 C9 F6 38.4(7) . . . . ? F4 C8 C9 F5 161.1(5) . . . . ? F3 C8 C9 F5 45.9(6) . . . . ? C7 C8 C9 F5 -77.0(6) . . . . ? F4 C8 C9 C10 42.5(8) . . . . ? F3 C8 C9 C10 -72.7(7) . . . . ? C7 C8 C9 C10 164.4(6) . . . . ? F6 C9 C10 F7 172.4(6) . . . . ? F5 C9 C10 F7 -73.3(8) . . . . ? C8 C9 C10 F7 46.3(10) . . . . ? F6 C9 C10 F8 52.1(9) . . . . ? F5 C9 C10 F8 166.4(7) . . . . ? C8 C9 C10 F8 -74.1(10) . . . . ? F6 C9 C10 F9 -65.6(9) . . . . ? F5 C9 C10 F9 48.8(9) . . . . ? C8 C9 C10 F9 168.3(7) . . . . ? O6 S2 C17 F10 168.9(3) . . . . ? O4 S2 C17 F10 -70.8(4) . . . . ? O5 S2 C17 F10 48.9(4) . . . . ? O6 S2 C17 F11 -74.9(4) . . . . ? O4 S2 C17 F11 45.4(4) . . . . ? O5 S2 C17 F11 165.2(3) . . . . ? O6 S2 C17 C18 46.8(4) . . . . ? O4 S2 C17 C18 167.1(4) . . . . ? O5 S2 C17 C18 -73.1(4) . . . . ? F10 C17 C18 F12 -79.1(5) . . . . ? F11 C17 C18 F12 164.8(4) . . . . ? S2 C17 C18 F12 42.8(5) . . . . ? F10 C17 C18 F13 164.8(4) . . . . ? F11 C17 C18 F13 48.7(5) . . . . ? S2 C17 C18 F13 -73.3(5) . . . . ? F10 C17 C18 C19 44.0(6) . . . . ? F11 C17 C18 C19 -72.1(6) . . . . ? S2 C17 C18 C19 165.9(4) . . . . ? F12 C18 C19 F15 167.1(5) . . . . ? F13 C18 C19 F15 -78.1(6) . . . . ? C17 C18 C19 F15 43.4(7) . . . . ? F12 C18 C19 F14 48.9(7) . . . . ? F13 C18 C19 F14 163.6(5) . . . . ? C17 C18 C19 F14 -74.9(7) . . . . ? F12 C18 C19 C20 -67.2(8) . . . . ? F13 C18 C19 C20 47.5(8) . . . . ? C17 C18 C19 C20 169.1(6) . . . . ? F15 C19 C20 F16 171.0(7) . . . . ? F14 C19 C20 F16 -73.7(9) . . . . ? C18 C19 C20 F16 44.8(11) . . . . ? F15 C19 C20 F18 -61.9(9) . . . . ? F14 C19 C20 F18 53.3(9) . . . . ? C18 C19 C20 F18 171.9(7) . . . . ? F15 C19 C20 F17 53.0(9) . . . . ? F14 C19 C20 F17 168.3(7) . . . . ? C18 C19 C20 F17 -73.2(9) . . . . ? C2 N2 C1 N1 2.9(5) . . . . ? C5 N2 C1 N1 -177.8(4) . . . . ? C3 N1 C1 N2 -2.1(5) . . . . ? C4 N1 C1 N2 179.1(4) . . . . ? C1 N2 C2 C3 -2.5(6) . . . . ? C5 N2 C2 C3 178.2(5) . . . . ? N2 C2 C3 N1 1.2(6) . . . . ? C1 N1 C3 C2 0.6(5) . . . . ? C4 N1 C3 C2 179.4(4) . . . . ? C1 N2 C5 C6 -98.4(6) . . . . ? C2 N2 C5 C6 80.8(7) . . . . ? C13 N3 C11 N4 -0.4(5) . . . . ? C14 N3 C11 N4 177.8(4) . . . . ? C12 N4 C11 N3 0.9(5) . . . . ? C15 N4 C11 N3 177.7(4) . . . . ? C11 N4 C12 C13 -1.1(6) . . . . ? C15 N4 C12 C13 -177.7(5) . . . . ? N4 C12 C13 N3 0.8(6) . . . . ? C11 N3 C13 C12 -0.2(5) . . . . ? C14 N3 C13 C12 -178.5(4) . . . . ? C11 N4 C15 C16 119.6(7) . . . . ? C12 N4 C15 C16 -64.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.578 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.107 #===END