data_12 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H31 F12 N3 O2 W' _chemical_formula_weight 781.35 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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 21.962(2) _cell_length_b 11.9097(14) _cell_length_c 21.964(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5744.9(11) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7282 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description tablet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3056 _exptl_absorpt_coefficient_mu 4.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6435 _exptl_absorpt_correction_T_max 0.7900 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 SMART 1000 CCD' _diffrn_measurement_method '\w- and \f-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 101815 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7128 _reflns_number_gt 4861 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0180P)^2^+18.7154P] 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 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7128 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.002 _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 W W 0.124670(7) 0.140845(12) 0.348240(6) 0.01788(5) Uani 1 1 d . . . O1 O 0.12265(14) 0.1741(3) 0.26223(12) 0.0277(6) Uani 1 1 d . . . O2 O 0.07017(12) 0.2383(2) 0.39320(12) 0.0229(6) Uani 1 1 d . . . N1 N 0.20294(14) 0.1467(3) 0.37788(15) 0.0227(7) Uani 1 1 d . . . N2 N 0.30068(15) 0.0527(3) 0.37461(17) 0.0265(8) Uani 1 1 d . . . N3 N 0.26547(15) 0.1006(3) 0.46456(17) 0.0272(8) Uani 1 1 d . . . F1 F 0.0488(2) 0.2294(5) 0.12316(18) 0.121(2) Uani 1 1 d . . . F2 F 0.04140(18) 0.3116(4) 0.20880(17) 0.0895(15) Uani 1 1 d . . . F3 F 0.1272(2) 0.3110(4) 0.16314(16) 0.0849(13) Uani 1 1 d . . . F4 F 0.19111(13) 0.1208(3) 0.16316(14) 0.0562(9) Uani 1 1 d . . . F5 F 0.14982(17) -0.0273(3) 0.19882(15) 0.0618(9) Uani 1 1 d . . . F6 F 0.11634(14) 0.0442(3) 0.11600(12) 0.0541(9) Uani 1 1 d . . . F7 F -0.03047(15) 0.3021(4) 0.33271(15) 0.0659(10) Uani 1 1 d . . . F8 F -0.09158(13) 0.2470(4) 0.40234(16) 0.0684(11) Uani 1 1 d . . . F9 F -0.03980(14) 0.1277(3) 0.35083(17) 0.0658(11) Uani 1 1 d . . . F10 F -0.03842(13) 0.3439(3) 0.49765(15) 0.0529(9) Uani 1 1 d . . . F11 F 0.00838(14) 0.4330(2) 0.42580(14) 0.0467(7) Uani 1 1 d . . . F12 F 0.05905(13) 0.3532(3) 0.49659(13) 0.0479(8) Uani 1 1 d . . . C1 C 0.0986(2) 0.0026(4) 0.3582(2) 0.0294(10) Uani 1 1 d . . . C2 C 0.0873(2) -0.1195(4) 0.3688(3) 0.0392(12) Uani 1 1 d . . . H2A H 0.0870 -0.1589 0.3291 0.047 Uiso 1 1 calc R . . H2B H 0.0465 -0.1289 0.3874 0.047 Uiso 1 1 calc R . . C3 C 0.1345(2) -0.1734(4) 0.4097(3) 0.0459(13) Uani 1 1 d . . . H3A H 0.1751 -0.1631 0.3920 0.069 Uiso 1 1 calc R . . H3B H 0.1258 -0.2538 0.4137 0.069 Uiso 1 1 calc R . . H3C H 0.1332 -0.1381 0.4500 0.069 Uiso 1 1 calc R . . C4 C 0.25224(19) 0.1019(3) 0.40370(19) 0.0242(8) Uani 1 1 d . . . C5 C 0.3428(2) 0.0191(4) 0.4182(2) 0.0351(11) Uani 1 1 d . . . H5 H 0.3802 -0.0183 0.4104 0.042 Uiso 1 1 calc R . . C6 C 0.3216(2) 0.0485(4) 0.4725(2) 0.0335(11) Uani 1 1 d . . . H6 H 0.3414 0.0361 0.5104 0.040 Uiso 1 1 calc R . . C7 C 0.3074(2) 0.0333(4) 0.3075(2) 0.0321(10) Uani 1 1 d . . . C8 C 0.3731(2) -0.0038(5) 0.2944(3) 0.0463(13) Uani 1 1 d . . . H8A H 0.4014 0.0538 0.3091 0.069 Uiso 1 1 calc R . . H8B H 0.3785 -0.0139 0.2505 0.069 Uiso 1 1 calc R . . H8C H 0.3813 -0.0748 0.3154 0.069 Uiso 1 1 calc R . . C9 C 0.2638(2) -0.0612(4) 0.2892(2) 0.0402(12) Uani 1 1 d . . . H9A H 0.2731 -0.1287 0.3130 0.060 Uiso 1 1 calc R . . H9B H 0.2686 -0.0775 0.2458 0.060 Uiso 1 1 calc R . . H9C H 0.2218 -0.0379 0.2973 0.060 Uiso 1 1 calc R . . C10 C 0.2954(2) 0.1423(4) 0.2727(2) 0.0366(11) Uani 1 1 d . . . H10A H 0.2532 0.1659 0.2792 0.055 Uiso 1 1 calc R . . H10B H 0.3024 0.1300 0.2292 0.055 Uiso 1 1 calc R . . H10C H 0.3230 0.2009 0.2875 0.055 Uiso 1 1 calc R . . C11 C 0.2264(2) 0.1459(4) 0.5150(2) 0.0302(9) Uani 1 1 d . . . C12 C 0.2105(2) 0.2676(4) 0.5021(2) 0.0379(11) Uani 1 1 d . . . H12A H 0.2480 0.3108 0.4962 0.057 Uiso 1 1 calc R . . H12B H 0.1877 0.2986 0.5365 0.057 Uiso 1 1 calc R . . H12C H 0.1856 0.2718 0.4652 0.057 Uiso 1 1 calc R . . C13 C 0.2620(2) 0.1402(5) 0.5749(2) 0.0473(13) Uani 1 1 d . . . H13A H 0.2710 0.0616 0.5846 0.071 Uiso 1 1 calc R . . H13B H 0.2375 0.1731 0.6077 0.071 Uiso 1 1 calc R . . H13C H 0.3001 0.1821 0.5707 0.071 Uiso 1 1 calc R . . C14 C 0.1701(2) 0.0717(5) 0.5205(2) 0.0389(11) Uani 1 1 d . . . H14A H 0.1489 0.0694 0.4812 0.058 Uiso 1 1 calc R . . H14B H 0.1428 0.1024 0.5516 0.058 Uiso 1 1 calc R . . H14C H 0.1824 -0.0045 0.5320 0.058 Uiso 1 1 calc R . . C15 C 0.0929(2) 0.1387(5) 0.2093(2) 0.0382(12) Uani 1 1 d . . . C16 C 0.0363(2) 0.0712(7) 0.2201(3) 0.081(3) Uani 1 1 d . . . H16A H 0.0075 0.1154 0.2444 0.121 Uiso 1 1 calc R . . H16B H 0.0467 0.0022 0.2420 0.121 Uiso 1 1 calc R . . H16C H 0.0176 0.0521 0.1809 0.121 Uiso 1 1 calc R . . C17 C 0.0778(3) 0.2520(7) 0.1752(3) 0.068(2) Uani 1 1 d . . . C18 C 0.1381(2) 0.0703(5) 0.1716(2) 0.0416(13) Uani 1 1 d . . . C19 C 0.01431(18) 0.2327(4) 0.42423(19) 0.0261(9) Uani 1 1 d . . . C20 C 0.0098(2) 0.1323(4) 0.4667(2) 0.0446(13) Uani 1 1 d . . . H20A H 0.0211 0.0639 0.4446 0.067 Uiso 1 1 calc R . . H20B H -0.0321 0.1253 0.4816 0.067 Uiso 1 1 calc R . . H20C H 0.0374 0.1429 0.5012 0.067 Uiso 1 1 calc R . . C21 C -0.0369(2) 0.2292(5) 0.3770(3) 0.0464(14) Uani 1 1 d . . . C22 C 0.0104(2) 0.3406(4) 0.4612(2) 0.0345(11) Uani 1 1 d . . . 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 W 0.01415(7) 0.01964(8) 0.01984(7) -0.00195(6) -0.00055(6) 0.00192(7) O1 0.0229(14) 0.0414(17) 0.0189(13) -0.0050(12) -0.0033(14) 0.0014(15) O2 0.0186(13) 0.0256(16) 0.0245(15) 0.0011(12) 0.0056(11) 0.0054(12) N1 0.0177(15) 0.0232(18) 0.0272(17) -0.0029(15) -0.0001(13) 0.0030(15) N2 0.0154(16) 0.0223(19) 0.042(2) 0.0013(16) -0.0013(15) -0.0005(14) N3 0.0202(17) 0.0242(19) 0.037(2) 0.0009(16) -0.0089(14) 0.0017(14) F1 0.158(4) 0.155(5) 0.051(2) -0.050(3) -0.064(3) 0.111(4) F2 0.085(3) 0.122(4) 0.062(2) -0.046(2) -0.038(2) 0.070(3) F3 0.126(4) 0.084(3) 0.045(2) 0.0206(19) 0.008(2) 0.033(3) F4 0.0329(16) 0.088(3) 0.0480(19) -0.0162(17) 0.0102(13) -0.0011(16) F5 0.081(2) 0.054(2) 0.051(2) -0.0091(17) -0.0104(18) 0.0176(19) F6 0.0517(19) 0.083(2) 0.0275(14) -0.0233(15) -0.0049(13) 0.0149(17) F7 0.053(2) 0.099(3) 0.0454(19) 0.014(2) -0.0147(16) 0.015(2) F8 0.0216(14) 0.110(3) 0.074(2) -0.021(2) 0.0021(15) 0.0136(18) F9 0.0371(17) 0.080(3) 0.080(3) -0.038(2) -0.0010(17) -0.0049(17) F10 0.0416(17) 0.060(2) 0.0572(19) -0.0164(16) 0.0296(15) 0.0002(15) F11 0.0486(18) 0.0315(16) 0.0601(19) 0.0010(14) 0.0097(15) 0.0091(14) F12 0.0397(16) 0.071(2) 0.0327(15) -0.0150(15) 0.0024(12) 0.0015(16) C1 0.024(2) 0.028(2) 0.036(3) -0.0066(19) -0.0028(18) 0.0009(18) C2 0.033(2) 0.025(3) 0.060(3) -0.006(2) 0.003(2) -0.006(2) C3 0.052(3) 0.024(2) 0.061(3) 0.004(2) 0.009(3) 0.006(2) C4 0.0194(18) 0.0165(19) 0.037(2) 0.0009(17) 0.0002(18) -0.0012(16) C5 0.022(2) 0.029(3) 0.055(3) 0.009(2) -0.006(2) 0.0046(19) C6 0.025(2) 0.030(3) 0.046(3) 0.011(2) -0.008(2) 0.0034(19) C7 0.023(2) 0.030(3) 0.043(3) -0.006(2) 0.0059(19) 0.0039(19) C8 0.024(2) 0.053(3) 0.062(3) -0.002(3) 0.007(3) 0.007(3) C9 0.031(2) 0.036(3) 0.053(3) -0.015(2) 0.005(2) -0.001(2) C10 0.034(2) 0.039(3) 0.037(3) 0.002(2) 0.006(2) 0.000(2) C11 0.030(2) 0.029(2) 0.031(2) -0.001(2) -0.0067(18) 0.005(2) C12 0.046(3) 0.031(3) 0.037(3) -0.007(2) -0.006(2) 0.007(2) C13 0.042(3) 0.063(4) 0.036(3) -0.004(3) -0.014(2) 0.008(3) C14 0.036(3) 0.047(3) 0.034(2) 0.001(2) -0.001(2) -0.002(2) C15 0.028(2) 0.065(4) 0.022(2) -0.015(2) -0.0045(17) 0.005(2) C16 0.034(3) 0.159(8) 0.048(4) -0.054(4) 0.003(3) -0.033(4) C17 0.062(4) 0.112(6) 0.030(3) -0.024(4) -0.022(3) 0.045(4) C18 0.033(3) 0.060(4) 0.031(2) -0.019(2) -0.0019(19) 0.006(2) C19 0.0197(19) 0.032(2) 0.027(2) 0.0011(18) 0.0057(16) 0.0031(18) C20 0.042(3) 0.038(3) 0.054(3) 0.014(3) 0.019(2) 0.006(2) C21 0.020(2) 0.067(4) 0.053(3) -0.013(3) 0.002(2) 0.004(2) C22 0.029(2) 0.039(3) 0.036(3) -0.002(2) 0.014(2) 0.005(2) _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 W C1 1.757(5) . ? W N1 1.839(3) . ? W O1 1.931(3) . ? W O2 1.938(3) . ? O1 C15 1.399(5) . ? O2 C19 1.405(5) . ? N1 C4 1.334(5) . ? N2 C4 1.373(5) . ? N2 C5 1.389(5) . ? N2 C7 1.499(6) . ? N3 C4 1.368(5) . ? N3 C6 1.390(5) . ? N3 C11 1.503(6) . ? F1 C17 1.337(6) . ? F2 C17 1.299(7) . ? F3 C17 1.319(9) . ? F4 C18 1.324(6) . ? F5 C18 1.333(7) . ? F6 C18 1.347(5) . ? F7 C21 1.311(7) . ? F8 C21 1.340(5) . ? F9 C21 1.340(6) . ? F10 C22 1.338(5) . ? F11 C22 1.348(6) . ? F12 C22 1.330(6) . ? C1 C2 1.494(6) . ? C2 C3 1.515(7) . ? C5 C6 1.328(7) . ? C7 C10 1.528(7) . ? C7 C9 1.531(6) . ? C7 C8 1.536(6) . ? C11 C12 1.517(7) . ? C11 C14 1.525(7) . ? C11 C13 1.531(6) . ? C15 C16 1.500(7) . ? C15 C18 1.527(6) . ? C15 C17 1.579(9) . ? C19 C20 1.520(6) . ? C19 C22 1.522(6) . ? C19 C21 1.531(7) . ? 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 C1 W N1 107.25(18) . . ? C1 W O1 107.84(17) . . ? N1 W O1 111.10(14) . . ? C1 W O2 107.23(16) . . ? N1 W O2 111.98(13) . . ? O1 W O2 111.20(12) . . ? C15 O1 W 139.7(3) . . ? C19 O2 W 139.3(3) . . ? C4 N1 W 153.4(3) . . ? C4 N2 C5 108.6(4) . . ? C4 N2 C7 126.8(3) . . ? C5 N2 C7 124.6(4) . . ? C4 N3 C6 108.4(4) . . ? C4 N3 C11 126.5(3) . . ? C6 N3 C11 125.0(4) . . ? C2 C1 W 170.4(4) . . ? C1 C2 C3 113.0(4) . . ? N1 C4 N3 126.4(4) . . ? N1 C4 N2 127.0(4) . . ? N3 C4 N2 106.6(4) . . ? C6 C5 N2 108.0(4) . . ? C5 C6 N3 108.4(4) . . ? N2 C7 C10 110.1(4) . . ? N2 C7 C9 108.0(4) . . ? C10 C7 C9 112.7(4) . . ? N2 C7 C8 108.6(4) . . ? C10 C7 C8 108.2(4) . . ? C9 C7 C8 109.1(4) . . ? N3 C11 C12 109.6(4) . . ? N3 C11 C14 108.2(4) . . ? C12 C11 C14 112.5(4) . . ? N3 C11 C13 109.0(4) . . ? C12 C11 C13 108.7(4) . . ? C14 C11 C13 108.7(4) . . ? O1 C15 C16 114.7(4) . . ? O1 C15 C18 108.0(4) . . ? C16 C15 C18 109.8(5) . . ? O1 C15 C17 103.5(4) . . ? C16 C15 C17 111.0(5) . . ? C18 C15 C17 109.6(4) . . ? F2 C17 F3 109.2(7) . . ? F2 C17 F1 107.6(5) . . ? F3 C17 F1 109.1(7) . . ? F2 C17 C15 109.1(6) . . ? F3 C17 C15 112.2(5) . . ? F1 C17 C15 109.5(6) . . ? F4 C18 F5 106.7(4) . . ? F4 C18 F6 106.9(4) . . ? F5 C18 F6 105.9(4) . . ? F4 C18 C15 113.9(5) . . ? F5 C18 C15 110.3(4) . . ? F6 C18 C15 112.6(4) . . ? O2 C19 C20 113.1(4) . . ? O2 C19 C22 105.6(3) . . ? C20 C19 C22 109.4(4) . . ? O2 C19 C21 108.3(4) . . ? C20 C19 C21 110.3(4) . . ? C22 C19 C21 110.1(4) . . ? F7 C21 F9 106.5(5) . . ? F7 C21 F8 107.5(5) . . ? F9 C21 F8 106.2(4) . . ? F7 C21 C19 113.9(4) . . ? F9 C21 C19 110.5(5) . . ? F8 C21 C19 111.9(4) . . ? F12 C22 F10 106.9(4) . . ? F12 C22 F11 105.7(4) . . ? F10 C22 F11 107.1(4) . . ? F12 C22 C19 111.2(4) . . ? F10 C22 C19 112.9(4) . . ? F11 C22 C19 112.5(4) . . ? 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 C1 W O1 C15 23.4(5) . . . . ? N1 W O1 C15 140.7(4) . . . . ? O2 W O1 C15 -93.8(4) . . . . ? C1 W O2 C19 -9.4(4) . . . . ? N1 W O2 C19 -126.8(4) . . . . ? O1 W O2 C19 108.2(4) . . . . ? C1 W N1 C4 -0.2(7) . . . . ? O1 W N1 C4 -117.8(7) . . . . ? O2 W N1 C4 117.2(7) . . . . ? N1 W C1 C2 -13(2) . . . . ? O1 W C1 C2 107(2) . . . . ? O2 W C1 C2 -133(2) . . . . ? W C1 C2 C3 26(3) . . . . ? W N1 C4 N3 -92.2(8) . . . . ? W N1 C4 N2 90.8(8) . . . . ? C6 N3 C4 N1 -178.6(4) . . . . ? C11 N3 C4 N1 2.1(7) . . . . ? C6 N3 C4 N2 -1.1(5) . . . . ? C11 N3 C4 N2 179.6(4) . . . . ? C5 N2 C4 N1 178.8(4) . . . . ? C7 N2 C4 N1 -3.2(7) . . . . ? C5 N2 C4 N3 1.3(5) . . . . ? C7 N2 C4 N3 179.3(4) . . . . ? C4 N2 C5 C6 -1.1(5) . . . . ? C7 N2 C5 C6 -179.1(4) . . . . ? N2 C5 C6 N3 0.4(5) . . . . ? C4 N3 C6 C5 0.4(5) . . . . ? C11 N3 C6 C5 179.8(4) . . . . ? C4 N2 C7 C10 51.3(6) . . . . ? C5 N2 C7 C10 -131.0(4) . . . . ? C4 N2 C7 C9 -72.1(5) . . . . ? C5 N2 C7 C9 105.5(5) . . . . ? C4 N2 C7 C8 169.7(4) . . . . ? C5 N2 C7 C8 -12.7(6) . . . . ? C4 N3 C11 C12 -54.1(6) . . . . ? C6 N3 C11 C12 126.6(4) . . . . ? C4 N3 C11 C14 68.9(5) . . . . ? C6 N3 C11 C14 -110.4(5) . . . . ? C4 N3 C11 C13 -173.0(4) . . . . ? C6 N3 C11 C13 7.7(6) . . . . ? W O1 C15 C16 16.6(8) . . . . ? W O1 C15 C18 -106.1(5) . . . . ? W O1 C15 C17 137.7(4) . . . . ? O1 C15 C17 F2 -62.3(6) . . . . ? C16 C15 C17 F2 61.2(6) . . . . ? C18 C15 C17 F2 -177.4(5) . . . . ? O1 C15 C17 F3 58.8(5) . . . . ? C16 C15 C17 F3 -177.6(5) . . . . ? C18 C15 C17 F3 -56.2(6) . . . . ? O1 C15 C17 F1 -179.8(5) . . . . ? C16 C15 C17 F1 -56.3(6) . . . . ? C18 C15 C17 F1 65.1(7) . . . . ? O1 C15 C18 F4 -50.2(6) . . . . ? C16 C15 C18 F4 -175.9(5) . . . . ? C17 C15 C18 F4 62.0(6) . . . . ? O1 C15 C18 F5 69.8(5) . . . . ? C16 C15 C18 F5 -55.9(6) . . . . ? C17 C15 C18 F5 -178.0(4) . . . . ? O1 C15 C18 F6 -172.1(4) . . . . ? C16 C15 C18 F6 62.2(6) . . . . ? C17 C15 C18 F6 -60.0(6) . . . . ? W O2 C19 C20 46.1(6) . . . . ? W O2 C19 C22 165.8(3) . . . . ? W O2 C19 C21 -76.3(5) . . . . ? O2 C19 C21 F7 -45.1(6) . . . . ? C20 C19 C21 F7 -169.3(4) . . . . ? C22 C19 C21 F7 69.8(5) . . . . ? O2 C19 C21 F9 74.7(5) . . . . ? C20 C19 C21 F9 -49.5(5) . . . . ? C22 C19 C21 F9 -170.3(4) . . . . ? O2 C19 C21 F8 -167.2(4) . . . . ? C20 C19 C21 F8 68.6(6) . . . . ? C22 C19 C21 F8 -52.3(6) . . . . ? O2 C19 C22 F12 -54.6(5) . . . . ? C20 C19 C22 F12 67.4(5) . . . . ? C21 C19 C22 F12 -171.2(4) . . . . ? O2 C19 C22 F10 -174.8(4) . . . . ? C20 C19 C22 F10 -52.8(5) . . . . ? C21 C19 C22 F10 68.6(5) . . . . ? O2 C19 C22 F11 63.8(5) . . . . ? C20 C19 C22 F11 -174.2(4) . . . . ? C21 C19 C22 F11 -52.8(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.924 _refine_diff_density_min -1.239 _refine_diff_density_rms 0.124