data_jam04 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H27 Cl F3 N7 O6 S' _chemical_formula_sum 'C33 H27 Cl F3 N7 O6 S' _chemical_formula_weight 742.13 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _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 10.9264(5) _cell_length_b 12.1779(6) _cell_length_c 14.2739(7) _cell_angle_alpha 73.0330(10) _cell_angle_beta 67.6620(10) _cell_angle_gamma 67.3760(10) _cell_volume 1597.82(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16089 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 31.97 _exptl_crystal_description Fragment _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9047 _exptl_absorpt_correction_T_max 0.9667 _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 8 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37699 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 32.63 _reflns_number_total 10400 _reflns_number_gt 7425 _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 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10400 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.637 _refine_ls_restrained_S_all 1.637 _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 0.67425(4) -0.02309(3) 0.08179(2) 0.01556(8) Uani 1 1 d . . . Cl1 Cl 0.09419(4) -0.00993(3) 0.35979(2) 0.01591(8) Uani 1 1 d . . . O1 O 0.58967(10) 0.00287(9) 0.30099(7) 0.0181(2) Uani 1 1 d . . . O2 O 0.60743(10) 0.10342(9) 0.07862(7) 0.0208(2) Uani 1 1 d . . . O3 O 0.69929(10) -0.07715(9) -0.00263(7) 0.0196(2) Uani 1 1 d . . . O4 O 1.02732(12) -0.31168(11) -0.00286(9) 0.0387(3) Uani 1 1 d . . . O5 O 0.82400(12) -0.29491(10) 0.11130(8) 0.0309(3) Uani 1 1 d . . . O6 O 0.07660(11) 0.52703(9) 0.24290(7) 0.0235(2) Uani 1 1 d . . . F1 F 0.37415(8) 0.34046(7) 0.11663(6) 0.0243(2) Uani 1 1 d . . . F2 F 0.29384(9) 0.53401(8) 0.08767(6) 0.0281(2) Uani 1 1 d . . . F3 F 0.23230(9) 0.42887(8) 0.02608(6) 0.0260(2) Uani 1 1 d . . . N1 N 0.69167(15) -0.34991(13) 0.62992(10) 0.0336(4) Uani 1 1 d . . . N2 N 0.68639(13) -0.37014(12) 0.55896(10) 0.0246(3) Uani 1 1 d . . . N3 N 0.68509(14) -0.40890(12) 0.48769(10) 0.0287(3) Uani 1 1 d . . . N4 N 0.29592(12) -0.00974(10) 0.50030(8) 0.0146(2) Uani 1 1 d . . . N5 N 0.09519(12) 0.33315(10) 0.24383(8) 0.0139(2) Uani 1 1 d . . . N6 N 0.57804(12) -0.09328(10) 0.18716(8) 0.0146(2) Uani 1 1 d . . . N7 N 0.92950(14) -0.26493(11) 0.06650(10) 0.0236(3) Uani 1 1 d . . . C1 C 0.63553(16) -0.31601(13) 0.40528(11) 0.0223(3) Uani 1 1 d . . . H1A H 0.6172 -0.3552 0.3624 0.027 Uiso 1 1 calc R . . H1B H 0.7098 -0.2795 0.3607 0.027 Uiso 1 1 calc R . . C2 C 0.50385(15) -0.21652(13) 0.44680(10) 0.0175(3) Uani 1 1 d . . . H2A H 0.5258 -0.1705 0.4818 0.021 Uiso 1 1 calc R . . H2B H 0.4340 -0.2540 0.4987 0.021 Uiso 1 1 calc R . . C3 C 0.43939(14) -0.12763(12) 0.36266(10) 0.0147(3) Uani 1 1 d . . . C4 C 0.31420(14) -0.02743(12) 0.41099(9) 0.0129(3) Uani 1 1 d . . . C5 C 0.20965(14) 0.06825(12) 0.35688(10) 0.0132(3) Uani 1 1 d . . . C6 C 0.27057(14) 0.12484(12) 0.24612(9) 0.0138(3) Uani 1 1 d . . . H6A H 0.3396 0.1600 0.2444 0.017 Uiso 1 1 calc R . . H6B H 0.3206 0.0603 0.2036 0.017 Uiso 1 1 calc R . . C7 C 0.16302(15) 0.22295(12) 0.19804(10) 0.0147(3) Uani 1 1 d . . . H7A H 0.2093 0.2449 0.1239 0.018 Uiso 1 1 calc R . . H7B H 0.0905 0.1892 0.2042 0.018 Uiso 1 1 calc R . . C8 C 0.13342(15) 0.43418(13) 0.20687(10) 0.0160(3) Uani 1 1 d . . . C9 C 0.25997(16) 0.43317(13) 0.10835(11) 0.0202(3) Uani 1 1 d . . . C10 C -0.02401(14) 0.33252(13) 0.34152(9) 0.0152(3) Uani 1 1 d . . . H10 H -0.0734 0.4184 0.3515 0.018 Uiso 1 1 calc R . . C11 C -0.12887(14) 0.28424(13) 0.33537(10) 0.0171(3) Uani 1 1 d . . . H11 H -0.1331 0.2068 0.3736 0.021 Uiso 1 1 calc R . . C12 C -0.21600(15) 0.34440(13) 0.27908(10) 0.0188(3) Uani 1 1 d . . . C13 C -0.21706(17) 0.46632(14) 0.21417(11) 0.0268(4) Uani 1 1 d . . . H13A H -0.1694 0.5030 0.2364 0.040 Uiso 1 1 calc R . . H13B H -0.3134 0.5181 0.2218 0.040 Uiso 1 1 calc R . . H13C H -0.1691 0.4574 0.1419 0.040 Uiso 1 1 calc R . . C14 C -0.31789(16) 0.29312(15) 0.27463(11) 0.0260(4) Uani 1 1 d . . . H14A H -0.3033 0.2105 0.3133 0.039 Uiso 1 1 calc R . . H14B H -0.3041 0.2922 0.2029 0.039 Uiso 1 1 calc R . . H14C H -0.4129 0.3431 0.3049 0.039 Uiso 1 1 calc R . . C15 C 0.03252(14) 0.26650(12) 0.43187(10) 0.0141(3) Uani 1 1 d . . . C16 C -0.01356(14) 0.32287(13) 0.51719(10) 0.0162(3) Uani 1 1 d . . . H16 H -0.0817 0.4002 0.5180 0.019 Uiso 1 1 calc R . . C17 C 0.03769(15) 0.26877(13) 0.60068(10) 0.0171(3) Uani 1 1 d . . . H17 H 0.0031 0.3089 0.6578 0.020 Uiso 1 1 calc R . . C18 C 0.13900(14) 0.15658(13) 0.60141(10) 0.0159(3) Uani 1 1 d . . . H18 H 0.1750 0.1193 0.6579 0.019 Uiso 1 1 calc R . . C19 C 0.18566(14) 0.10104(12) 0.51694(9) 0.0137(3) Uani 1 1 d . . . C20 C 0.13193(14) 0.15357(12) 0.43386(9) 0.0133(3) Uani 1 1 d . . . C21 C 0.54417(14) -0.06251(12) 0.28426(10) 0.0144(3) Uani 1 1 d . . . C22 C 0.42097(14) -0.19310(12) 0.29594(10) 0.0148(3) Uani 1 1 d . . . C23 C 0.34461(15) -0.27189(12) 0.32373(10) 0.0177(3) Uani 1 1 d . . . H23 H 0.2884 -0.2871 0.3927 0.021 Uiso 1 1 calc R . . C24 C 0.35105(15) -0.32836(13) 0.24967(11) 0.0198(3) Uani 1 1 d . . . H24 H 0.2996 -0.3831 0.2681 0.024 Uiso 1 1 calc R . . C25 C 0.43302(15) -0.30494(13) 0.14810(11) 0.0198(3) Uani 1 1 d . . . H25 H 0.4355 -0.3434 0.0980 0.024 Uiso 1 1 calc R . . C26 C 0.51095(15) -0.22673(13) 0.11887(10) 0.0168(3) Uani 1 1 d . . . H26 H 0.5661 -0.2106 0.0497 0.020 Uiso 1 1 calc R . . C27 C 0.50516(14) -0.17323(12) 0.19429(10) 0.0144(3) Uani 1 1 d . . . C28 C 0.83180(14) -0.05772(13) 0.10943(9) 0.0150(3) Uani 1 1 d . . . C29 C 0.85050(16) 0.03452(13) 0.13598(10) 0.0183(3) Uani 1 1 d . . . H29 H 0.7792 0.1100 0.1413 0.022 Uiso 1 1 calc R . . C30 C 0.97299(16) 0.01683(14) 0.15471(10) 0.0208(3) Uani 1 1 d . . . H30 H 0.9846 0.0799 0.1737 0.025 Uiso 1 1 calc R . . C31 C 1.07843(16) -0.09231(14) 0.14586(10) 0.0212(3) Uani 1 1 d . . . H31 H 1.1612 -0.1045 0.1602 0.025 Uiso 1 1 calc R . . C32 C 1.06333(15) -0.18352(14) 0.11619(10) 0.0201(3) Uani 1 1 d . . . H32 H 1.1365 -0.2576 0.1080 0.024 Uiso 1 1 calc R . . C33 C 0.94045(15) -0.16578(13) 0.09860(10) 0.0174(3) 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 S1 0.01542(19) 0.01669(19) 0.01392(16) -0.00196(14) -0.00470(13) -0.00453(15) Cl1 0.01570(18) 0.01642(18) 0.01734(16) -0.00252(13) -0.00616(13) -0.00590(14) O1 0.0168(5) 0.0204(6) 0.0195(5) -0.0065(4) -0.0052(4) -0.0062(5) O2 0.0209(6) 0.0166(5) 0.0231(5) -0.0016(4) -0.0092(4) -0.0027(5) O3 0.0217(6) 0.0249(6) 0.0137(5) -0.0050(4) -0.0039(4) -0.0090(5) O4 0.0295(7) 0.0393(7) 0.0454(7) -0.0285(6) -0.0037(6) -0.0007(6) O5 0.0266(7) 0.0224(6) 0.0451(7) -0.0063(5) -0.0091(5) -0.0105(5) O6 0.0272(6) 0.0160(5) 0.0247(5) -0.0075(4) -0.0028(5) -0.0058(5) F1 0.0175(5) 0.0206(5) 0.0271(4) -0.0033(4) -0.0026(4) -0.0027(4) F2 0.0280(5) 0.0193(5) 0.0329(5) -0.0046(4) 0.0002(4) -0.0123(4) F3 0.0344(5) 0.0256(5) 0.0147(4) -0.0010(4) -0.0066(4) -0.0085(4) N1 0.0325(9) 0.0461(10) 0.0254(7) 0.0036(7) -0.0141(6) -0.0174(7) N2 0.0176(7) 0.0239(7) 0.0282(7) 0.0041(6) -0.0099(6) -0.0055(6) N3 0.0322(8) 0.0195(7) 0.0330(7) -0.0045(6) -0.0198(6) 0.0030(6) N4 0.0134(6) 0.0149(6) 0.0137(5) -0.0021(5) -0.0036(5) -0.0034(5) N5 0.0135(6) 0.0137(6) 0.0120(5) -0.0028(5) -0.0038(4) -0.0014(5) N6 0.0145(6) 0.0174(6) 0.0118(5) -0.0038(5) -0.0029(5) -0.0050(5) N7 0.0223(7) 0.0183(7) 0.0293(7) -0.0054(6) -0.0111(6) -0.0012(6) C1 0.0213(8) 0.0209(8) 0.0228(7) -0.0049(6) -0.0111(6) 0.0006(7) C2 0.0178(8) 0.0164(7) 0.0154(7) -0.0022(6) -0.0072(6) -0.0005(6) C3 0.0137(7) 0.0151(7) 0.0142(6) -0.0028(5) -0.0049(5) -0.0025(6) C4 0.0121(7) 0.0130(7) 0.0138(6) -0.0006(5) -0.0043(5) -0.0048(6) C5 0.0125(7) 0.0137(7) 0.0138(6) -0.0028(5) -0.0040(5) -0.0043(6) C6 0.0133(7) 0.0132(7) 0.0131(6) -0.0031(5) -0.0031(5) -0.0023(6) C7 0.0170(7) 0.0130(7) 0.0136(6) -0.0034(5) -0.0045(5) -0.0033(6) C8 0.0167(8) 0.0166(7) 0.0149(6) -0.0024(6) -0.0070(6) -0.0034(6) C9 0.0223(8) 0.0160(8) 0.0199(7) -0.0021(6) -0.0052(6) -0.0053(7) C10 0.0135(7) 0.0153(7) 0.0130(6) -0.0028(5) -0.0031(5) -0.0013(6) C11 0.0166(8) 0.0164(7) 0.0155(7) -0.0031(6) -0.0028(6) -0.0039(6) C12 0.0156(8) 0.0214(8) 0.0163(7) -0.0069(6) -0.0040(6) -0.0005(6) C13 0.0304(10) 0.0250(9) 0.0243(8) -0.0032(7) -0.0156(7) -0.0013(7) C14 0.0209(9) 0.0344(9) 0.0242(8) -0.0088(7) -0.0093(6) -0.0049(7) C15 0.0111(7) 0.0165(7) 0.0140(6) -0.0017(5) -0.0024(5) -0.0055(6) C16 0.0124(7) 0.0162(7) 0.0176(7) -0.0049(6) -0.0016(5) -0.0033(6) C17 0.0164(8) 0.0203(8) 0.0136(6) -0.0072(6) -0.0010(6) -0.0051(6) C18 0.0167(8) 0.0194(8) 0.0121(6) -0.0016(6) -0.0044(5) -0.0069(6) C19 0.0116(7) 0.0144(7) 0.0138(6) -0.0018(5) -0.0024(5) -0.0046(6) C20 0.0121(7) 0.0147(7) 0.0117(6) -0.0025(5) -0.0015(5) -0.0048(6) C21 0.0121(7) 0.0142(7) 0.0144(6) -0.0028(6) -0.0062(5) 0.0010(6) C22 0.0145(7) 0.0139(7) 0.0140(6) -0.0034(5) -0.0059(5) -0.0001(6) C23 0.0163(8) 0.0157(7) 0.0177(7) -0.0021(6) -0.0037(6) -0.0033(6) C24 0.0160(8) 0.0158(7) 0.0286(8) -0.0043(6) -0.0077(6) -0.0049(6) C25 0.0184(8) 0.0203(8) 0.0233(7) -0.0085(6) -0.0083(6) -0.0032(7) C26 0.0142(7) 0.0192(8) 0.0157(7) -0.0054(6) -0.0050(6) -0.0018(6) C27 0.0118(7) 0.0126(7) 0.0182(7) -0.0030(6) -0.0052(5) -0.0022(6) C28 0.0134(7) 0.0181(7) 0.0116(6) -0.0008(5) -0.0028(5) -0.0050(6) C29 0.0205(8) 0.0163(7) 0.0155(7) -0.0003(6) -0.0044(6) -0.0057(6) C30 0.0257(9) 0.0233(8) 0.0176(7) 0.0002(6) -0.0080(6) -0.0131(7) C31 0.0175(8) 0.0282(9) 0.0179(7) 0.0023(6) -0.0066(6) -0.0105(7) C32 0.0162(8) 0.0207(8) 0.0179(7) -0.0002(6) -0.0043(6) -0.0030(6) C33 0.0186(8) 0.0172(8) 0.0143(6) -0.0013(6) -0.0033(6) -0.0061(6) _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 1.4240(10) . ? S1 O3 1.4262(10) . ? S1 N6 1.6843(11) . ? S1 C28 1.7770(15) . ? Cl1 C5 1.8334(14) . ? O1 C21 1.2015(16) . ? O4 N7 1.2260(16) . ? O5 N7 1.2240(16) . ? O6 C8 1.2187(16) . ? F1 C9 1.3400(16) . ? F2 C9 1.3369(16) . ? F3 C9 1.3384(16) . ? N1 N2 1.1362(18) . ? N2 N3 1.2467(18) . ? N3 C1 1.4808(18) . ? N4 C4 1.2826(16) . ? N4 C19 1.4307(17) . ? N5 C8 1.3475(18) . ? N5 C7 1.4683(17) . ? N5 C10 1.5039(16) . ? N6 C21 1.4160(16) . ? N6 C27 1.4384(18) . ? N7 C33 1.4689(19) . ? C1 C2 1.5229(19) . ? C2 C3 1.5518(18) . ? C3 C22 1.5151(19) . ? C3 C4 1.5250(19) . ? C3 C21 1.5487(19) . ? C4 C5 1.5429(19) . ? C5 C20 1.5120(18) . ? C5 C6 1.5279(17) . ? C6 C7 1.5276(18) . ? C8 C9 1.5519(19) . ? C10 C11 1.514(2) . ? C10 C15 1.5196(18) . ? C11 C12 1.3378(19) . ? C12 C14 1.498(2) . ? C12 C13 1.502(2) . ? C15 C20 1.3869(18) . ? C15 C16 1.4014(18) . ? C16 C17 1.3904(19) . ? C17 C18 1.3888(19) . ? C18 C19 1.3837(18) . ? C19 C20 1.3991(18) . ? C22 C23 1.384(2) . ? C22 C27 1.4007(18) . ? C23 C24 1.388(2) . ? C24 C25 1.3977(19) . ? C25 C26 1.389(2) . ? C26 C27 1.3833(19) . ? C28 C29 1.390(2) . ? C28 C33 1.3936(19) . ? C29 C30 1.388(2) . ? C30 C31 1.385(2) . ? C31 C32 1.382(2) . ? C32 C33 1.383(2) . ? 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 120.01(6) . . ? O2 S1 N6 107.28(6) . . ? O3 S1 N6 107.23(6) . . ? O2 S1 C28 107.05(6) . . ? O3 S1 C28 110.36(6) . . ? N6 S1 C28 103.69(6) . . ? N1 N2 N3 171.19(15) . . ? N2 N3 C1 115.84(13) . . ? C4 N4 C19 107.30(11) . . ? C8 N5 C7 125.26(11) . . ? C8 N5 C10 117.08(11) . . ? C7 N5 C10 117.64(11) . . ? C21 N6 C27 110.75(11) . . ? C21 N6 S1 119.57(9) . . ? C27 N6 S1 129.14(9) . . ? O5 N7 O4 125.07(14) . . ? O5 N7 C33 117.60(12) . . ? O4 N7 C33 117.33(13) . . ? N3 C1 C2 112.83(12) . . ? C1 C2 C3 113.61(11) . . ? C22 C3 C4 118.06(12) . . ? C22 C3 C21 102.26(10) . . ? C4 C3 C21 104.90(11) . . ? C22 C3 C2 111.98(11) . . ? C4 C3 C2 109.39(11) . . ? C21 C3 C2 109.53(11) . . ? N4 C4 C3 120.43(12) . . ? N4 C4 C5 113.83(12) . . ? C3 C4 C5 125.42(11) . . ? C20 C5 C6 116.08(11) . . ? C20 C5 C4 100.03(10) . . ? C6 C5 C4 116.65(11) . . ? C20 C5 Cl1 108.91(9) . . ? C6 C5 Cl1 109.25(9) . . ? C4 C5 Cl1 105.03(9) . . ? C7 C6 C5 114.39(11) . . ? N5 C7 C6 114.75(11) . . ? O6 C8 N5 125.99(12) . . ? O6 C8 C9 116.88(12) . . ? N5 C8 C9 117.12(12) . . ? F2 C9 F3 107.14(11) . . ? F2 C9 F1 106.70(12) . . ? F3 C9 F1 107.39(11) . . ? F2 C9 C8 109.93(12) . . ? F3 C9 C8 111.99(12) . . ? F1 C9 C8 113.36(11) . . ? N5 C10 C11 112.45(11) . . ? N5 C10 C15 109.42(11) . . ? C11 C10 C15 113.48(11) . . ? C12 C11 C10 123.71(13) . . ? C11 C12 C14 122.06(14) . . ? C11 C12 C13 122.82(14) . . ? C14 C12 C13 115.11(13) . . ? C20 C15 C16 117.22(12) . . ? C20 C15 C10 123.57(12) . . ? C16 C15 C10 119.18(12) . . ? C17 C16 C15 121.85(13) . . ? C18 C17 C16 120.64(13) . . ? C19 C18 C17 117.71(12) . . ? C18 C19 C20 121.94(13) . . ? C18 C19 N4 125.82(12) . . ? C20 C19 N4 112.16(11) . . ? C15 C20 C19 120.61(12) . . ? C15 C20 C5 132.79(12) . . ? C19 C20 C5 106.49(11) . . ? O1 C21 N6 125.18(12) . . ? O1 C21 C3 127.13(12) . . ? N6 C21 C3 107.69(12) . . ? C23 C22 C27 119.66(13) . . ? C23 C22 C3 129.41(12) . . ? C27 C22 C3 110.73(12) . . ? C22 C23 C24 119.25(13) . . ? C23 C24 C25 120.17(14) . . ? C26 C25 C24 121.41(14) . . ? C27 C26 C25 117.48(13) . . ? C26 C27 C22 121.99(13) . . ? C26 C27 N6 129.48(12) . . ? C22 C27 N6 108.53(12) . . ? C29 C28 C33 118.43(14) . . ? C29 C28 S1 116.44(11) . . ? C33 C28 S1 124.93(11) . . ? C28 C29 C30 120.25(14) . . ? C31 C30 C29 120.37(14) . . ? C32 C31 C30 120.09(14) . . ? C31 C32 C33 119.26(14) . . ? C32 C33 C28 121.55(14) . . ? C32 C33 N7 117.33(13) . . ? C28 C33 N7 121.11(13) . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 32.63 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 0.887 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.074