# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1467 data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H15 F3 N2 O2' _chemical_formula_weight 300.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.277(2) _cell_length_b 12.015(2) _cell_length_c 11.056(2) _cell_angle_alpha 97.87(1) _cell_angle_beta 94.66(2) _cell_angle_gamma 71.73(1) _cell_volume 1408.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 35 _cell_measurement_theta_max 45 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 1.056 _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 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'nomal-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R diffractometer' _diffrn_measurement_method ot _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.22 _diffrn_reflns_number 5950 _diffrn_reflns_av_R_equivalents 0.0127 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 65.04 _reflns_number_total 4788 _reflns_number_gt 4029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku/MSC AFC5R software 1992' _computing_cell_refinement 'Rigaku/MSC AFC5R software 1992' _computing_data_reduction 'Rigaku/MSC AFC5R software 1992' _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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0058(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4788 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.2379 _refine_ls_wR_factor_gt 0.2296 _refine_ls_goodness_of_fit_ref 1.941 _refine_ls_restrained_S_all 1.941 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # = = = END 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 F1 F 0.1038(3) 0.2856(5) 1.2146(7) 0.132(2) Uani 0.668(6) 1 d P . . F2 F 0.2830(8) 0.2594(6) 1.2992(4) 0.139(2) Uani 0.668(6) 1 d P . . F3 F 0.2546(6) 0.1545(3) 1.1395(3) 0.1053(14) Uani 0.668(6) 1 d P . . F4 F 0.1746(16) 0.3094(8) 1.2971(10) 0.130(2) Uani 0.332(6) 1 d P . . F5 F 0.3173(10) 0.1883(13) 1.2231(18) 0.1608(19) Uani 0.332(6) 1 d P . . F6 F 0.1441(15) 0.2127(13) 1.1396(7) 0.1238(16) Uani 0.332(6) 1 d P . . F7 F -0.1867(3) 0.4415(4) 0.5383(6) 0.1215(16) Uani 0.808(8) 1 d P . . F8 F -0.0181(7) 0.3416(3) 0.4591(4) 0.1378(19) Uani 0.808(8) 1 d P . . F9 F -0.0205(4) 0.4506(3) 0.6275(3) 0.1061(12) Uani 0.808(8) 1 d P . . F10 F -0.147(3) 0.384(3) 0.468(2) 0.161(5) Uani 0.192(8) 1 d P . . F11 F 0.0360(12) 0.381(3) 0.535(3) 0.157(2) Uani 0.192(8) 1 d P . . F12 F -0.116(4) 0.4646(18) 0.624(3) 0.208(15) Uani 0.192(8) 1 d P . . O1 O 0.2763(3) 0.4337(2) 1.17604(18) 0.0936(8) Uani 1 1 d . . . O2 O 0.50128(17) 0.25400(17) 0.86895(16) 0.0693(5) Uani 1 1 d . . . O3 O -0.1425(2) 0.2180(2) 0.5911(2) 0.0910(7) Uani 1 1 d . . . O4 O 0.2758(3) 0.0362(2) 0.6173(2) 0.0959(8) Uani 1 1 d . . . N1 N 0.22407(17) 0.35167(16) 0.79140(16) 0.0514(5) Uani 1 1 d . . . N2 N 0.22511(18) 0.33170(16) 1.00139(17) 0.0522(5) Uani 1 1 d . . . N3 N 0.15861(19) 0.12913(17) 0.85340(17) 0.0553(5) Uani 1 1 d . . . N4 N 0.02416(17) 0.24312(16) 0.71001(17) 0.0540(5) Uani 1 1 d . . . C1 C 0.2353(2) 0.41121(19) 0.9161(2) 0.0512(5) Uani 1 1 d . . . C2 C 0.1330(2) 0.5294(2) 0.9281(3) 0.0666(7) Uani 1 1 d . . . C3 C 0.1873(3) 0.6078(2) 0.8672(3) 0.0737(7) Uani 1 1 d . . . C4 C 0.3224(3) 0.5732(2) 0.9141(3) 0.0732(8) Uani 1 1 d . . . C5 C 0.3615(2) 0.4410(2) 0.9235(2) 0.0554(6) Uani 1 1 d . . . C6 C 0.4313(2) 0.3602(2) 0.8169(2) 0.0567(6) Uani 1 1 d . . . C7 C 0.5157(3) 0.4012(3) 0.7471(3) 0.0721(7) Uani 1 1 d . . . C8 C 0.5135(3) 0.3848(3) 0.6273(3) 0.0826(9) Uani 1 1 d . . . C9 C 0.4264(3) 0.3331(3) 0.5552(3) 0.0795(8) Uani 1 1 d . . . C10 C 0.3368(3) 0.3053(3) 0.6050(2) 0.0669(7) Uani 1 1 d . . . C11 C 0.3245(2) 0.3352(2) 0.7357(2) 0.0524(5) Uani 1 1 d . . . C12 C 0.2435(2) 0.3527(2) 1.1209(2) 0.0603(6) Uani 1 1 d . . . C13 C 0.2207(3) 0.2632(2) 1.1957(2) 0.0631(6) Uani 1 1 d . . . C14 C 0.5617(4) 0.1541(3) 0.7870(3) 0.1008(11) Uani 1 1 d . . . C15 C 0.0478(2) 0.1362(2) 0.7697(2) 0.0548(6) Uani 1 1 d . . . C16 C -0.0622(3) 0.1377(3) 0.8453(3) 0.0811(8) Uani 1 1 d . . . C17 C -0.0279(19) -0.0025(11) 0.8456(9) 0.095(5) Uani 0.56(3) 1 d P . . C18 C -0.1003(19) 0.0300(11) 0.8101(17) 0.096(5) Uani 0.44(3) 1 d P . . C19 C 0.0165(4) -0.0586(3) 0.7343(6) 0.1136(15) Uani 1 1 d . . . C20 C 0.0822(3) 0.0188(2) 0.6832(2) 0.0689(7) Uani 1 1 d . . . C21 C 0.2243(3) -0.0242(2) 0.6943(2) 0.0633(6) Uani 1 1 d . . . C22 C 0.2918(3) -0.1546(2) 0.6811(3) 0.0784(8) Uani 1 1 d . . . C23 C 0.3849(3) -0.1993(3) 0.7586(3) 0.0842(9) Uani 1 1 d . . . C24 C 0.4214(3) -0.1273(3) 0.8618(3) 0.0853(9) Uani 1 1 d . . . C25 C 0.3600(3) -0.0142(3) 0.8907(3) 0.0771(8) Uani 1 1 d . . . C26 C 0.2462(2) 0.0369(2) 0.8186(2) 0.0586(6) Uani 1 1 d . . . C27 C -0.0671(2) 0.2709(2) 0.6247(2) 0.0627(6) Uani 1 1 d . . . C28 C -0.0713(3) 0.3771(2) 0.5612(3) 0.0701(7) Uani 1 1 d . . . C29 C 0.3144(6) -0.0133(4) 0.5082(5) 0.148(2) Uani 1 1 d . . . # = = = END H1 H 0.0577 0.5234 0.8868 0.081 Uiso 1 1 d . . . H2 H 0.1177 0.5589 1.0114 0.081 Uiso 1 1 d . . . H3 H 0.1812 0.5919 0.7810 0.089 Uiso 1 1 d . . . H4 H 0.1457 0.6888 0.8915 0.089 Uiso 1 1 d . . . H5 H 0.3734 0.5896 0.8587 0.088 Uiso 1 1 d . . . H6 H 0.3302 0.6155 0.9921 0.088 Uiso 1 1 d . . . H7 H 0.4060 0.4229 0.9990 0.067 Uiso 1 1 d . . . H8 H 0.5718 0.4389 0.7903 0.087 Uiso 1 1 d . . . H9 H 0.5713 0.4080 0.5860 0.099 Uiso 1 1 d . . . H10 H 0.4329 0.3187 0.4690 0.096 Uiso 1 1 d . . . H11 H 0.2841 0.2673 0.5568 0.081 Uiso 1 1 d . . . H12 H 0.2039 0.2624 0.9698 0.063 Uiso 1 1 d . . . H13 H 0.6208 0.1721 0.7436 0.121 Uiso 1 1 d . . . H14 H 0.6032 0.0898 0.8326 0.121 Uiso 1 1 d . . . H15 H 0.5012 0.1330 0.7320 0.121 Uiso 1 1 d . . . H16 H 0.0536 0.0318 0.6015 0.082 Uiso 1 1 d . . . H17 H 0.2676 -0.2052 0.6166 0.095 Uiso 1 1 d . . . H18 H 0.4294 -0.2813 0.7466 0.102 Uiso 1 1 d . . . H19 H 0.4917 -0.1635 0.9121 0.103 Uiso 1 1 d . . . H20 H 0.3889 0.0321 0.9563 0.093 Uiso 1 1 d . . . H21 H 0.0745 0.2935 0.7323 0.065 Uiso 1 1 d . . . H22 H 0.2454 -0.0260 0.4585 0.178 Uiso 1 1 d . . . H23 H 0.3765 -0.0870 0.5147 0.178 Uiso 1 1 d . . . H24 H 0.3476 0.0368 0.4718 0.178 Uiso 1 1 d . . . # = = = END 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 F1 0.0691(19) 0.151(4) 0.197(5) 0.110(4) 0.034(2) -0.019(2) F2 0.213(5) 0.177(4) 0.075(2) 0.058(2) -0.068(3) -0.131(4) F3 0.169(4) 0.0674(17) 0.094(2) 0.0137(14) 0.036(2) -0.048(2) F4 0.197(6) 0.109 0.101 0.016 0.077 -0.050 F5 0.103(5) 0.157 0.227 0.104 0.038 -0.004 F6 0.178(4) 0.162 0.089 0.037 -0.015 -0.130 F7 0.101(2) 0.107(2) 0.155(4) 0.071(2) -0.043(2) -0.0179(18) F8 0.226(5) 0.104(2) 0.102(2) 0.0213(16) 0.064(3) -0.058(2) F9 0.140(3) 0.0782(16) 0.123(2) 0.0535(15) -0.054(2) -0.0641(18) F10 0.201(14) 0.175 0.143 0.089 -0.087 -0.103 F11 0.075(7) 0.177 0.256 0.144 -0.013 -0.047 F12 0.32(4) 0.097 0.177 0.014 0.051 -0.016 O1 0.145(2) 0.1090(16) 0.0592(10) -0.0076(10) 0.0102(12) -0.0916(16) O2 0.0633(10) 0.0777(11) 0.0643(10) 0.0183(9) -0.0047(8) -0.0153(9) O3 0.0886(14) 0.1016(15) 0.1040(16) 0.0424(12) -0.0449(12) -0.0587(13) O4 0.135(2) 0.0741(12) 0.0857(14) 0.0251(11) 0.0319(14) -0.0293(13) N1 0.0548(10) 0.0575(10) 0.0521(10) 0.0147(8) -0.0066(8) -0.0307(8) N2 0.0599(11) 0.0549(10) 0.0533(10) 0.0106(8) -0.0015(8) -0.0331(9) N3 0.0647(11) 0.0553(11) 0.0546(10) 0.0156(8) -0.0151(8) -0.0313(9) N4 0.0581(11) 0.0551(10) 0.0599(11) 0.0178(8) -0.0143(8) -0.0325(9) C1 0.0537(12) 0.0560(12) 0.0541(12) 0.0116(9) -0.0005(9) -0.0299(10) C2 0.0625(14) 0.0627(14) 0.0788(16) 0.0123(12) 0.0056(12) -0.0226(12) C3 0.0885(19) 0.0576(14) 0.0818(18) 0.0196(12) 0.0032(14) -0.0273(13) C4 0.0884(19) 0.0699(16) 0.0803(17) 0.0079(13) 0.0034(14) -0.0517(15) C5 0.0593(13) 0.0682(14) 0.0524(12) 0.0116(10) -0.0061(10) -0.0396(11) C6 0.0506(12) 0.0717(14) 0.0577(13) 0.0169(11) -0.0038(10) -0.0306(11) C7 0.0619(14) 0.098(2) 0.0730(17) 0.0213(14) 0.0022(12) -0.0438(14) C8 0.0727(17) 0.115(2) 0.0768(18) 0.0267(17) 0.0105(14) -0.0443(17) C9 0.0862(19) 0.104(2) 0.0532(14) 0.0143(14) 0.0076(13) -0.0330(17) C10 0.0774(16) 0.0792(16) 0.0502(13) 0.0086(11) -0.0056(11) -0.0344(13) C11 0.0586(12) 0.0571(12) 0.0504(12) 0.0122(9) -0.0047(9) -0.0295(10) C12 0.0700(14) 0.0694(14) 0.0545(13) 0.0032(11) 0.0035(10) -0.0413(12) C13 0.0707(15) 0.0712(15) 0.0549(13) 0.0147(11) -0.0027(11) -0.0305(13) C14 0.098(2) 0.091(2) 0.094(2) 0.0204(19) 0.0107(19) 0.0035(19) C15 0.0602(13) 0.0594(13) 0.0565(13) 0.0189(10) -0.0140(10) -0.0341(11) C16 0.0747(17) 0.091(2) 0.097(2) 0.0387(17) 0.0006(15) -0.0424(15) C17 0.106(11) 0.101(6) 0.112(6) 0.044(4) -0.004(5) -0.070(7) C18 0.079(9) 0.085(6) 0.141(9) 0.023(5) 0.001(7) -0.046(6) C19 0.093(2) 0.076(2) 0.194(5) 0.032(3) -0.011(3) -0.056(2) C20 0.0879(18) 0.0578(14) 0.0711(16) 0.0157(12) -0.0258(13) -0.0406(13) C21 0.0815(17) 0.0549(13) 0.0612(14) 0.0152(11) -0.0037(12) -0.0299(12) C22 0.106(2) 0.0591(15) 0.0750(18) 0.0109(13) 0.0040(16) -0.0315(15) C23 0.095(2) 0.0650(16) 0.093(2) 0.0314(15) 0.0084(17) -0.0148(15) C24 0.0725(17) 0.087(2) 0.095(2) 0.0363(17) -0.0108(15) -0.0163(15) C25 0.0696(16) 0.0833(19) 0.0815(19) 0.0213(15) -0.0186(14) -0.0285(14) C26 0.0654(14) 0.0558(13) 0.0645(14) 0.0195(10) -0.0081(11) -0.0301(11) C27 0.0625(14) 0.0664(14) 0.0680(15) 0.0201(12) -0.0163(11) -0.0317(12) C28 0.0800(17) 0.0645(15) 0.0691(16) 0.0220(13) -0.0152(13) -0.0255(13) C29 0.229(6) 0.109(3) 0.125(4) 0.004(3) 0.084(4) -0.066(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. ; # = = = END 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 F1 F6 1.129(11) . ? F1 F4 1.228(14) . ? F1 C13 1.289(4) . ? F2 F5 1.112(15) . ? F2 F4 1.180(12) . ? F2 C13 1.292(4) . ? F3 F5 1.221(19) . ? F3 F6 1.222(14) . ? F3 C13 1.320(4) . ? F4 C13 1.256(7) . ? F5 C13 1.223(9) . ? F6 C13 1.280(7) . ? F7 F10 1.00(3) . ? F7 F12 1.25(4) . ? F7 C28 1.314(4) . ? F8 F11 1.14(3) . ? F8 C28 1.278(4) . ? F8 F10 1.39(3) . ? F9 F12 1.03(5) . ? F9 F11 1.30(4) . ? F9 C28 1.311(4) . ? F10 C28 1.282(16) . ? F11 C28 1.284(13) . ? F12 C28 1.17(2) . ? O1 C12 1.218(3) . ? O2 C14 1.420(4) . ? O2 C6 1.441(3) . ? O3 C27 1.220(3) . ? O4 C29 1.313(5) . ? O4 C21 1.450(3) . ? N1 C11 1.280(3) . ? N1 C1 1.478(3) . ? N2 C12 1.322(3) . ? N2 C1 1.466(3) . ? N3 C26 1.269(3) . ? N3 C15 1.481(3) . ? N4 C27 1.332(3) . ? N4 C15 1.465(3) . ? C1 C2 1.520(3) . ? C1 C5 1.566(3) . ? C2 C3 1.523(4) . ? C3 C4 1.515(4) . ? C4 C5 1.526(4) . ? C5 C6 1.520(3) . ? C6 C7 1.504(3) . ? C6 C11 1.524(3) . ? C7 C8 1.312(4) . ? C8 C9 1.451(5) . ? C9 C10 1.337(4) . ? C10 C11 1.448(3) . ? C12 C13 1.535(3) . ? C15 C16 1.546(4) . ? C15 C20 1.550(4) . ? C16 C18 1.481(10) . ? C16 C17 1.606(12) . ? C17 C18 0.874(11) . ? C17 C19 1.372(10) . ? C18 C19 1.621(14) . ? C19 C20 1.541(4) . ? C20 C21 1.521(4) . ? C21 C22 1.505(4) . ? C21 C26 1.506(3) . ? C22 C23 1.323(5) . ? C23 C24 1.448(5) . ? C24 C25 1.325(5) . ? C25 C26 1.461(4) . ? C27 C28 1.524(3) . ? 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 F6 F1 F4 118.4(8) . . ? F6 F1 C13 63.5(5) . . ? F4 F1 C13 59.8(4) . . ? F5 F2 F4 116.4(9) . . ? F5 F2 C13 60.6(7) . . ? F4 F2 C13 60.9(5) . . ? F5 F3 F6 113.5(7) . . ? F5 F3 C13 57.4(5) . . ? F6 F3 C13 60.3(4) . . ? F2 F4 F1 122.0(7) . . ? F2 F4 C13 63.9(5) . . ? F1 F4 C13 62.5(5) . . ? F2 F5 F3 127.0(10) . . ? F2 F5 C13 67.0(6) . . ? F3 F5 C13 65.4(8) . . ? F1 F6 F3 122.6(8) . . ? F1 F6 C13 64.4(4) . . ? F3 F6 C13 63.6(6) . . ? F10 F7 F12 117.4(19) . . ? F10 F7 C28 65.6(12) . . ? F12 F7 C28 54.2(12) . . ? F11 F8 C28 63.9(12) . . ? F11 F8 F10 114.6(16) . . ? C28 F8 F10 57.3(10) . . ? F12 F9 F11 113.8(17) . . ? F12 F9 C28 58.5(14) . . ? F11 F9 C28 59.0(9) . . ? F7 F10 C28 69.0(13) . . ? F7 F10 F8 121.1(16) . . ? C28 F10 F8 57.0(10) . . ? F8 F11 C28 63.4(9) . . ? F8 F11 F9 121.0(12) . . ? C28 F11 F9 61.0(12) . . ? F9 F12 C28 72.8(19) . . ? F9 F12 F7 130(2) . . ? C28 F12 F7 65.7(17) . . ? C14 O2 C6 117.4(2) . . ? C29 O4 C21 120.9(3) . . ? C11 N1 C1 109.21(17) . . ? C12 N2 C1 122.68(18) . . ? C26 N3 C15 109.04(19) . . ? C27 N4 C15 120.99(18) . . ? N2 C1 N1 106.89(16) . . ? N2 C1 C2 113.28(19) . . ? N1 C1 C2 108.11(19) . . ? N2 C1 C5 116.12(19) . . ? N1 C1 C5 106.21(17) . . ? C2 C1 C5 105.80(18) . . ? C1 C2 C3 102.9(2) . . ? C4 C3 C2 102.9(2) . . ? C3 C4 C5 106.5(2) . . ? C6 C5 C4 116.5(2) . . ? C6 C5 C1 102.91(17) . . ? C4 C5 C1 104.4(2) . . ? O2 C6 C7 110.2(2) . . ? O2 C6 C5 104.17(18) . . ? C7 C6 C5 119.6(2) . . ? O2 C6 C11 108.50(18) . . ? C7 C6 C11 111.9(2) . . ? C5 C6 C11 101.61(18) . . ? C8 C7 C6 120.8(2) . . ? C7 C8 C9 122.6(3) . . ? C10 C9 C8 122.8(2) . . ? C9 C10 C11 117.0(2) . . ? N1 C11 C10 124.6(2) . . ? N1 C11 C6 114.58(19) . . ? C10 C11 C6 120.6(2) . . ? O1 C12 N2 127.2(2) . . ? O1 C12 C13 117.8(2) . . ? N2 C12 C13 115.0(2) . . ? F5 C13 F4 103.6(9) . . ? F5 C13 F6 109.4(10) . . ? F4 C13 F6 106.0(8) . . ? F5 C13 F1 135.4(5) . . ? F4 C13 F1 57.6(7) . . ? F6 C13 F1 52.1(6) . . ? F5 C13 F2 52.4(8) . . ? F4 C13 F2 55.2(6) . . ? F6 C13 F2 136.7(4) . . ? F1 C13 F2 109.3(4) . . ? F5 C13 F3 57.3(9) . . ? F4 C13 F3 134.1(4) . . ? F6 C13 F3 56.1(7) . . ? F1 C13 F3 104.4(4) . . ? F2 C13 F3 106.2(4) . . ? F5 C13 C12 112.7(5) . . ? F4 C13 C12 113.0(4) . . ? F6 C13 C12 111.6(4) . . ? F1 C13 C12 111.9(3) . . ? F2 C13 C12 111.7(3) . . ? F3 C13 C12 112.9(2) . . ? N4 C15 N3 106.79(16) . . ? N4 C15 C16 113.3(2) . . ? N3 C15 C16 108.4(2) . . ? N4 C15 C20 115.28(19) . . ? N3 C15 C20 105.3(2) . . ? C16 C15 C20 107.3(2) . . ? C18 C16 C15 111.1(5) . . ? C18 C16 C17 32.6(5) . . ? C15 C16 C17 97.3(5) . . ? C18 C17 C19 89.6(12) . . ? C18 C17 C16 65.9(11) . . ? C19 C17 C16 109.5(5) . . ? C17 C18 C16 81.6(13) . . ? C17 C18 C19 57.8(10) . . ? C16 C18 C19 103.3(8) . . ? C17 C19 C20 107.4(4) . . ? C17 C19 C18 32.6(4) . . ? C20 C19 C18 107.1(4) . . ? C21 C20 C19 115.1(2) . . ? C21 C20 C15 103.22(19) . . ? C19 C20 C15 104.8(3) . . ? O4 C21 C22 111.2(2) . . ? O4 C21 C26 100.6(2) . . ? C22 C21 C26 112.9(2) . . ? O4 C21 C20 110.0(2) . . ? C22 C21 C20 119.5(2) . . ? C26 C21 C20 100.5(2) . . ? C23 C22 C21 120.3(3) . . ? C22 C23 C24 122.1(3) . . ? C25 C24 C23 123.0(3) . . ? C24 C25 C26 117.6(3) . . ? N3 C26 C25 125.2(2) . . ? N3 C26 C21 115.1(2) . . ? C25 C26 C21 119.6(2) . . ? O3 C27 N4 126.5(2) . . ? O3 C27 C28 118.5(2) . . ? N4 C27 C28 114.9(2) . . ? F12 C28 F8 140.1(13) . . ? F12 C28 F10 104(2) . . ? F8 C28 F10 65.7(16) . . ? F12 C28 F11 106(2) . . ? F8 C28 F11 52.8(16) . . ? F10 C28 F11 112.3(16) . . ? F12 C28 F9 49(2) . . ? F8 C28 F9 110.1(4) . . ? F10 C28 F9 134.8(11) . . ? F11 C28 F9 60.0(17) . . ? F12 C28 F7 60(2) . . ? F8 C28 F7 107.6(4) . . ? F10 C28 F7 45.4(17) . . ? F11 C28 F7 133.6(7) . . ? F9 C28 F7 104.3(3) . . ? F12 C28 C27 110.1(12) . . ? F8 C28 C27 109.6(3) . . ? F10 C28 C27 109.7(9) . . ? F11 C28 C27 114.6(7) . . ? F9 C28 C27 113.4(2) . . ? F7 C28 C27 111.6(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 65.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.515 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.060