data_test _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H26 Cl3 F6 N4 O4' _chemical_formula_weight 871.02 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.310(3) _cell_length_b 13.490(3) _cell_length_c 16.660(3) _cell_angle_alpha 81.15(3) _cell_angle_beta 74.62(3) _cell_angle_gamma 80.74(3) _cell_volume 2827.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.046 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1772 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 5860 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 20.81 _reflns_number_total 5860 _reflns_number_gt 4752 _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^)+(0.1875P)^2^+11.4461P] 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 5860 _refine_ls_number_parameters 736 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1371 _refine_ls_R_factor_gt 0.1171 _refine_ls_wR_factor_ref 0.3282 _refine_ls_wR_factor_gt 0.3123 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.521 _refine_ls_shift/su_mean 0.035 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 C1 C 0.3531(6) 1.7607(6) 0.3446(4) 0.0351(19) Uani 1 1 d . . . C2 C 0.4346(5) 1.8211(6) 0.3252(4) 0.0340(19) Uani 1 1 d . . . C3 C 0.4210(6) 1.9230(6) 0.3404(5) 0.0384(19) Uani 1 1 d . . . H3A H 0.3529 1.9545 0.3649 0.046 Uiso 1 1 calc R . . C4 C 0.5048(6) 1.9774(6) 0.3203(5) 0.045(2) Uani 1 1 d . . . H4A H 0.4943 2.0465 0.3295 0.054 Uiso 1 1 calc R . . C5 C 0.6076(6) 1.9299(7) 0.2856(5) 0.045(2) Uani 1 1 d . . . H5A H 0.6656 1.9672 0.2737 0.054 Uiso 1 1 calc R . . C6 C 0.6241(6) 1.8327(6) 0.2691(5) 0.040(2) Uani 1 1 d . . . H6A H 0.6930 1.8023 0.2455 0.048 Uiso 1 1 calc R . . C7 C 0.5383(6) 1.7769(6) 0.2875(4) 0.0364(19) Uani 1 1 d . . . C8 C 0.4754(6) 1.6220(6) 0.2841(4) 0.0365(19) Uani 1 1 d . . . C9 C 0.4990(7) 1.5228(6) 0.2602(5) 0.050(2) Uani 1 1 d . . . H9A H 0.5687 1.4970 0.2337 0.060 Uiso 1 1 calc R . . C10 C 0.4187(8) 1.4653(7) 0.2764(6) 0.064(3) Uani 1 1 d . . . H10A H 0.4330 1.3985 0.2612 0.077 Uiso 1 1 calc R . . C11 C 0.3148(8) 1.5035(7) 0.3153(6) 0.062(3) Uani 1 1 d . . . H11A H 0.2605 1.4619 0.3256 0.075 Uiso 1 1 calc R . . C12 C 0.2911(7) 1.5981(6) 0.3380(5) 0.048(2) Uani 1 1 d . . . H12A H 0.2205 1.6221 0.3638 0.058 Uiso 1 1 calc R . . C13 C 0.3713(6) 1.6627(6) 0.3238(5) 0.0363(19) Uani 1 1 d . . . C14 C 0.2438(5) 1.8028(6) 0.3888(4) 0.0322(18) Uani 1 1 d . . . C15 C 0.2035(6) 1.7698(6) 0.4734(5) 0.039(2) Uani 1 1 d . . . H15A H 0.2440 1.7225 0.5045 0.047 Uiso 1 1 calc R . . C16 C 0.1015(6) 1.8095(6) 0.5099(5) 0.042(2) Uani 1 1 d . . . H16A H 0.0711 1.7901 0.5675 0.051 Uiso 1 1 calc R . . C17 C 0.0453(6) 1.8759(6) 0.4633(4) 0.0376(19) Uani 1 1 d . . . H17A H -0.0252 1.9018 0.4876 0.045 Uiso 1 1 calc R . . C18 C 0.0928(5) 1.9061(5) 0.3785(4) 0.0325(18) Uani 1 1 d . . . C19 C 0.0382(5) 1.9817(5) 0.3254(4) 0.0319(18) Uani 1 1 d . . . C20 C 0.0885(5) 2.0185(6) 0.2455(5) 0.0364(19) Uani 1 1 d . . . H20A H 0.1589 1.9924 0.2209 0.044 Uiso 1 1 calc R . . C21 C -0.1108(5) 2.0872(6) 0.3114(5) 0.0328(18) Uani 1 1 d . . . C22 C 0.0350(6) 2.0931(6) 0.2026(5) 0.0368(19) Uani 1 1 d . . . C23 C 0.0858(5) 2.1408(6) 0.1174(5) 0.0346(19) Uani 1 1 d . . . C24 C 0.0425(6) 2.2319(6) 0.0839(5) 0.045(2) Uani 1 1 d . . . H24A H -0.0217 2.2654 0.1139 0.054 Uiso 1 1 calc R . . C25 C 0.0944(6) 2.2745(7) 0.0049(5) 0.050(2) Uani 1 1 d . . . H25A H 0.0666 2.3376 -0.0198 0.061 Uiso 1 1 calc R . . C26 C 0.1864(6) 2.2229(6) -0.0359(5) 0.046(2) Uani 1 1 d . . . H26A H 0.2247 2.2505 -0.0891 0.055 Uiso 1 1 calc R . . C27 C 0.2226(6) 2.1304(6) 0.0013(5) 0.038(2) Uani 1 1 d . . . C28 C 0.3203(6) 2.0689(6) -0.0420(4) 0.041(2) Uani 1 1 d . . . C29 C 0.4181(6) 2.1077(6) -0.0661(4) 0.039(2) Uani 1 1 d . . . C30 C 0.4313(6) 2.2036(7) -0.0483(5) 0.047(2) Uani 1 1 d . . . H30A H 0.3726 2.2446 -0.0186 0.056 Uiso 1 1 calc R . . C31 C 0.5270(7) 2.2377(7) -0.0733(5) 0.055(2) Uani 1 1 d . . . H31A H 0.5350 2.3017 -0.0605 0.066 Uiso 1 1 calc R . . C32 C 0.6148(6) 2.1770(8) -0.1186(5) 0.051(2) Uani 1 1 d . . . H32A H 0.6806 2.2027 -0.1376 0.062 Uiso 1 1 calc R . . C33 C 0.6077(6) 2.0841(7) -0.1355(5) 0.046(2) Uani 1 1 d . . . H33A H 0.6676 2.0442 -0.1650 0.055 Uiso 1 1 calc R . . C34 C 0.5079(6) 2.0474(6) -0.1080(4) 0.039(2) Uani 1 1 d . . . C35 C 0.4085(6) 1.9146(6) -0.1042(5) 0.043(2) Uani 1 1 d . . . C36 C 0.4058(7) 1.8202(7) -0.1265(5) 0.058(2) Uani 1 1 d . . . H36A H 0.4685 1.7833 -0.1555 0.069 Uiso 1 1 calc R . . C37 C 0.3140(8) 1.7808(8) -0.1068(6) 0.074(3) Uani 1 1 d . . . H37A H 0.3123 1.7167 -0.1230 0.089 Uiso 1 1 calc R . . C38 C 0.2201(7) 1.8340(8) -0.0624(6) 0.064(3) Uani 1 1 d . . . H38A H 0.1564 1.8049 -0.0485 0.077 Uiso 1 1 calc R . . C39 C 0.2204(7) 1.9257(7) -0.0397(6) 0.055(2) Uani 1 1 d . . . H39A H 0.1571 1.9604 -0.0097 0.066 Uiso 1 1 calc R . . C40 C 0.3159(6) 1.9711(6) -0.0605(5) 0.042(2) Uani 1 1 d . . . C41 C -0.2688(6) 2.2165(7) 0.3181(5) 0.052(2) Uani 1 1 d . . . H41A H -0.2294 2.2558 0.2717 0.062 Uiso 1 1 calc R . . C42 C -0.3707(7) 2.2535(8) 0.3544(6) 0.063(3) Uani 1 1 d . . . H42A H -0.3993 2.3191 0.3348 0.076 Uiso 1 1 calc R . . C43 C -0.4325(6) 2.1946(7) 0.4205(5) 0.050(2) Uani 1 1 d . . . C44 C -0.3857(6) 2.1012(6) 0.4488(5) 0.042(2) Uani 1 1 d . . . H44A H -0.4256 2.0602 0.4935 0.051 Uiso 1 1 calc R . . C45 C -0.2829(5) 2.0665(6) 0.4138(4) 0.0367(19) Uani 1 1 d . . . H45A H -0.2528 2.0026 0.4354 0.044 Uiso 1 1 calc R . . C46 C -0.2222(5) 2.1233(6) 0.3474(4) 0.038(2) Uani 1 1 d . . . C47 C -0.5433(6) 2.2351(8) 0.4627(6) 0.061(3) Uani 1 1 d . . . H47A H -0.5709 2.1855 0.5106 0.073 Uiso 1 1 calc R . . H47B H -0.5876 2.2413 0.4225 0.073 Uiso 1 1 calc R . . C48 C -0.5539(6) 2.3390(7) 0.4949(5) 0.054(2) Uani 1 1 d . . . H48A H -0.5085 2.3336 0.5342 0.064 Uiso 1 1 calc R . . H48B H -0.5286 2.3894 0.4469 0.064 Uiso 1 1 calc R . . C49 C -0.6655(7) 2.3758(8) 0.5388(6) 0.064(3) Uani 1 1 d . . . H49A H -0.6895 2.3279 0.5892 0.076 Uiso 1 1 calc R . . H49B H -0.7120 2.3775 0.5009 0.076 Uiso 1 1 calc R . . C50 C -0.6743(8) 2.4811(8) 0.5649(6) 0.077(3) Uani 1 1 d . . . H50A H -0.7476 2.5031 0.5923 0.115 Uiso 1 1 calc R . . H50B H -0.6507 2.5287 0.5152 0.115 Uiso 1 1 calc R . . H50C H -0.6302 2.4791 0.6040 0.115 Uiso 1 1 calc R . . N1 N 0.5538(5) 1.6807(5) 0.2691(4) 0.0377(16) Uani 1 1 d . . . H1A H 0.6182 1.6546 0.2461 0.045 Uiso 1 1 calc R . . N2 N 0.1920(4) 1.8686(4) 0.3419(4) 0.0334(15) Uani 1 1 d . . . N3 N -0.0631(4) 2.0162(5) 0.3586(4) 0.0342(15) Uani 1 1 d . . . N4 N -0.0657(5) 2.1289(5) 0.2346(4) 0.0380(16) Uani 1 1 d . . . N5 N 0.1745(5) 2.0883(5) 0.0772(4) 0.0390(16) Uani 1 1 d . . . N6 N 0.5001(5) 1.9555(5) -0.1258(4) 0.0381(16) Uani 1 1 d . . . H6B H 0.5572 1.9201 -0.1526 0.046 Uiso 1 1 calc R . . C51 C 0.0921(11) 2.5061(11) -0.1909(10) 0.105(4) Uani 1 1 d . . . C52 C 0.2064(9) 2.4673(11) -0.1994(7) 0.082(3) Uani 1 1 d . . . O1 O 0.2386(5) 2.3832(5) -0.2128(4) 0.0687(19) Uani 1 1 d . . . O2 O 0.2546(8) 2.5400(11) -0.1937(10) 0.189(6) Uani 1 1 d . . . F1 F 0.0451(6) 2.5243(7) -0.1107(7) 0.162(4) Uani 1 1 d . . . F2 F 0.0415(7) 2.4429(7) -0.2053(10) 0.212(7) Uani 1 1 d . . . F3 F 0.0767(7) 2.5943(6) -0.2363(6) 0.131(3) Uani 1 1 d . . . C53 C 0.3163(7) 0.1882(7) 0.2620(7) 0.064(3) Uani 1 1 d . . . C54 C 0.2122(8) 0.2036(9) 0.3285(8) 0.071(3) Uani 1 1 d . . . O3 O 0.3216(5) 0.1291(5) 0.2142(4) 0.0674(19) Uani 1 1 d . . . O4 O 0.3872(6) 0.2296(6) 0.2756(5) 0.094(2) Uani 1 1 d . . . F4 F 0.2107(5) 0.2721(6) 0.3771(5) 0.120(3) Uani 1 1 d . . . F5 F 0.1924(6) 0.1182(6) 0.3778(5) 0.121(3) Uani 1 1 d . . . F6 F 0.1304(5) 0.2275(6) 0.2988(6) 0.127(3) Uani 1 1 d . . . C55 C -0.0318(15) 0.4371(14) 0.448(2) 0.194(11) Uani 1 1 d . . . H55A H -0.0102 0.3895 0.4053 0.233 Uiso 1 1 calc R . . H55B H -0.1092 0.4421 0.4686 0.233 Uiso 1 1 calc R . . C56 C 0.0163(10) 0.3912(7) 0.5219(9) 0.078(4) Uani 1 1 d . . . H56A H 0.0917 0.3680 0.4995 0.093 Uiso 1 1 calc R . . H56B H -0.0181 0.3310 0.5504 0.093 Uiso 1 1 calc R . . C57 C 0.0057(13) 0.468(3) 0.5905(18) 0.29(2) Uani 1 1 d . . . H57A H -0.0674 0.4749 0.6254 0.345 Uiso 1 1 calc R . . H57B H 0.0527 0.4392 0.6278 0.345 Uiso 1 1 calc R . . C58 C -0.0623(9) 0.7860(9) 0.2202(8) 0.091(4) Uani 1 1 d . . . H58A H -0.0899 0.7328 0.1994 0.109 Uiso 1 1 calc R . . Cl1 Cl -0.1006(3) 0.9036(2) 0.1718(2) 0.1006(11) Uani 1 1 d . . . Cl2 Cl -0.1173(3) 0.7865(3) 0.3278(3) 0.1229(14) Uani 1 1 d . . . Cl3 Cl 0.0740(3) 0.7576(3) 0.2047(4) 0.177(2) Uani 1 1 d . . . C59 C 0.282(3) 2.486(3) 0.048(2) 0.247(12) Uiso 1 1 d . . . Cl6 Cl 0.2482(9) 2.3776(8) 0.1201(6) 0.138(3) Uiso 0.50 1 d P . . Cl6' Cl 0.3093(13) 2.3820(11) 0.1077(9) 0.196(5) Uiso 0.50 1 d P . . Cl7 Cl 0.2426(15) 2.5767(13) 0.1127(12) 0.136(6) Uiso 0.33 1 d P . . Cl7' Cl 0.2252(10) 2.5975(10) 0.0744(9) 0.116(4) Uiso 0.33 1 d P . . Cl7" Cl 0.2975(11) 2.5828(9) 0.1088(7) 0.105(4) Uiso 0.33 1 d P . . Cl8 Cl 0.4231(13) 2.5112(12) -0.0126(11) 0.220(6) Uiso 0.50 1 d P . . Cl8' Cl 0.4412(15) 2.4652(15) 0.0543(12) 0.253(7) Uiso 0.50 1 d P . . O5 O 0.2961(10) 2.4769(9) -0.0336(8) 0.058(3) Uiso 0.50 1 d P . . O5' O 0.2244(13) 2.5139(11) -0.0140(9) 0.083(4) Uiso 0.50 1 d P . . 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 C1 0.037(5) 0.036(5) 0.033(4) 0.001(4) -0.015(4) 0.000(4) C2 0.028(4) 0.043(5) 0.027(4) -0.004(4) -0.005(3) 0.003(4) C3 0.039(5) 0.040(5) 0.038(5) -0.007(4) -0.012(4) -0.001(4) C4 0.057(6) 0.037(5) 0.045(5) -0.008(4) -0.018(4) -0.006(4) C5 0.035(5) 0.060(6) 0.044(5) -0.005(4) -0.011(4) -0.013(4) C6 0.031(4) 0.047(6) 0.042(5) 0.004(4) -0.014(4) -0.006(4) C7 0.048(5) 0.032(5) 0.033(4) 0.001(4) -0.020(4) -0.003(4) C8 0.043(5) 0.038(5) 0.028(4) -0.008(4) -0.009(4) -0.001(4) C9 0.056(6) 0.043(6) 0.050(5) -0.008(4) -0.012(4) -0.001(5) C10 0.081(8) 0.036(5) 0.075(7) -0.004(5) -0.024(6) -0.003(5) C11 0.061(7) 0.051(7) 0.079(7) -0.010(5) -0.016(5) -0.018(5) C12 0.045(5) 0.045(6) 0.053(5) -0.005(4) -0.009(4) -0.008(4) C13 0.040(5) 0.031(5) 0.037(4) 0.004(4) -0.013(4) -0.001(4) C14 0.027(4) 0.036(5) 0.033(5) -0.006(4) -0.005(4) -0.007(4) C15 0.040(5) 0.040(5) 0.035(5) 0.000(4) -0.009(4) -0.001(4) C16 0.047(5) 0.051(5) 0.026(4) -0.004(4) -0.005(4) -0.004(4) C17 0.037(4) 0.044(5) 0.030(5) -0.008(4) 0.000(4) -0.008(4) C18 0.032(5) 0.032(4) 0.035(5) -0.005(4) -0.007(4) -0.008(4) C19 0.029(5) 0.040(5) 0.027(4) -0.012(4) 0.000(4) -0.009(4) C20 0.022(4) 0.046(5) 0.037(5) -0.003(4) -0.001(4) -0.005(4) C21 0.028(4) 0.038(5) 0.032(5) -0.005(4) -0.010(4) 0.001(4) C22 0.025(4) 0.051(5) 0.033(4) -0.004(4) -0.004(4) -0.008(4) C23 0.026(4) 0.037(5) 0.039(5) 0.001(4) -0.009(4) -0.003(4) C24 0.033(4) 0.055(6) 0.043(5) -0.008(4) -0.001(4) 0.001(4) C25 0.045(5) 0.054(6) 0.039(5) 0.001(4) 0.003(4) 0.001(4) C26 0.046(5) 0.050(6) 0.031(4) 0.003(4) 0.006(4) -0.007(4) C27 0.031(4) 0.046(5) 0.033(5) 0.002(4) -0.001(4) -0.007(4) C28 0.035(5) 0.058(6) 0.023(4) 0.001(4) 0.004(3) -0.009(4) C29 0.037(5) 0.051(5) 0.024(4) 0.003(4) 0.000(4) -0.008(4) C30 0.041(5) 0.062(6) 0.036(5) -0.008(4) -0.007(4) -0.005(4) C31 0.054(6) 0.066(6) 0.050(5) -0.004(5) -0.012(5) -0.024(5) C32 0.036(5) 0.081(7) 0.036(5) 0.007(5) -0.008(4) -0.024(5) C33 0.029(5) 0.070(7) 0.036(5) -0.006(4) -0.004(4) -0.007(4) C34 0.034(5) 0.048(6) 0.031(4) 0.000(4) -0.006(4) -0.003(4) C35 0.043(5) 0.048(6) 0.032(5) 0.000(4) -0.004(4) -0.003(4) C36 0.056(6) 0.057(7) 0.054(6) -0.011(5) -0.003(5) -0.004(5) C37 0.070(7) 0.072(7) 0.078(7) -0.021(6) -0.001(6) -0.020(6) C38 0.045(6) 0.068(7) 0.078(7) -0.012(6) 0.000(5) -0.024(5) C39 0.046(6) 0.053(6) 0.061(6) -0.008(5) -0.003(4) -0.005(4) C40 0.037(5) 0.054(6) 0.029(4) -0.001(4) -0.002(4) -0.007(4) C41 0.026(5) 0.077(7) 0.038(5) 0.010(5) 0.003(4) -0.002(4) C42 0.042(6) 0.074(7) 0.055(6) 0.014(5) -0.003(5) 0.013(5) C43 0.025(4) 0.084(7) 0.035(5) -0.009(5) -0.003(4) 0.006(5) C44 0.034(5) 0.058(6) 0.032(4) -0.005(4) 0.001(4) -0.013(4) C45 0.028(5) 0.044(5) 0.035(5) -0.006(4) -0.003(4) -0.002(4) C46 0.022(4) 0.059(6) 0.028(4) -0.001(4) -0.004(4) -0.002(4) C47 0.032(5) 0.091(8) 0.050(5) 0.000(5) -0.006(4) 0.007(5) C48 0.048(5) 0.064(6) 0.041(5) -0.003(4) -0.006(4) 0.001(4) C49 0.044(5) 0.083(8) 0.049(5) -0.001(5) -0.006(4) 0.017(5) C50 0.068(7) 0.083(8) 0.067(7) -0.005(6) -0.011(5) 0.011(6) N1 0.031(4) 0.045(5) 0.035(4) -0.001(3) -0.008(3) 0.001(3) N2 0.026(4) 0.038(4) 0.034(4) -0.004(3) -0.006(3) 0.000(3) N3 0.030(4) 0.040(4) 0.031(3) -0.009(3) 0.001(3) -0.008(3) N4 0.037(4) 0.044(4) 0.027(4) -0.001(3) 0.001(3) -0.007(3) N5 0.029(4) 0.049(4) 0.036(4) -0.003(3) -0.004(3) -0.003(3) N6 0.029(4) 0.045(4) 0.032(4) -0.002(3) 0.002(3) 0.002(3) C51 0.087(10) 0.065(9) 0.136(12) -0.044(9) 0.023(9) 0.014(8) C52 0.061(7) 0.088(10) 0.095(9) -0.037(7) 0.003(6) -0.012(7) O1 0.072(4) 0.039(4) 0.076(5) 0.001(3) 0.000(3) 0.014(3) O2 0.079(7) 0.184(12) 0.322(18) -0.131(12) -0.025(9) -0.011(7) F1 0.107(6) 0.124(7) 0.180(9) 0.004(6) 0.049(6) 0.036(5) F2 0.083(6) 0.103(7) 0.47(2) -0.098(10) -0.081(9) 0.013(5) F3 0.147(7) 0.065(5) 0.174(8) -0.007(5) -0.050(6) 0.015(4) C53 0.048(6) 0.040(6) 0.095(8) -0.010(6) 0.002(6) -0.015(5) C54 0.053(7) 0.064(7) 0.095(8) -0.043(7) 0.003(6) -0.010(5) O3 0.051(4) 0.075(5) 0.079(5) -0.046(4) 0.002(3) -0.016(3) O4 0.070(5) 0.099(6) 0.110(6) -0.036(5) 0.005(4) -0.027(5) F4 0.091(5) 0.122(6) 0.155(7) -0.098(6) 0.009(4) -0.025(4) F5 0.114(6) 0.116(6) 0.107(5) -0.034(5) 0.042(4) -0.035(5) F6 0.047(4) 0.162(7) 0.182(8) -0.085(6) -0.017(4) 0.003(4) C55 0.140(16) 0.087(12) 0.40(4) -0.089(18) -0.12(2) 0.005(11) C56 0.083(8) 0.018(5) 0.134(11) -0.012(6) -0.038(8) 0.008(5) C57 0.078(12) 0.46(5) 0.25(3) 0.27(3) -0.069(15) -0.07(2) C58 0.086(8) 0.082(8) 0.128(10) -0.017(7) -0.056(8) -0.023(6) Cl1 0.113(2) 0.074(2) 0.136(3) -0.0073(18) -0.062(2) -0.0236(17) Cl2 0.134(3) 0.099(3) 0.163(4) 0.001(2) -0.074(3) -0.046(2) Cl3 0.071(2) 0.117(3) 0.346(8) -0.082(4) -0.037(3) 0.004(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 C1 C13 1.386(10) . ? C1 C2 1.401(10) . ? C1 C14 1.509(10) . ? C2 C3 1.411(11) . ? C2 C7 1.429(11) . ? C3 C4 1.373(11) . ? C4 C5 1.424(11) . ? C5 C6 1.351(11) . ? C6 C7 1.409(11) . ? C7 N1 1.351(9) . ? C8 N1 1.358(10) . ? C8 C9 1.418(11) . ? C8 C13 1.428(11) . ? C9 C10 1.366(13) . ? C10 C11 1.412(13) . ? C11 C12 1.353(12) . ? C12 C13 1.433(11) . ? C14 N2 1.323(9) . ? C14 C15 1.398(10) . ? C15 C16 1.388(11) . ? C16 C17 1.358(11) . ? C17 C18 1.412(10) . ? C18 N2 1.352(9) . ? C18 C19 1.475(10) . ? C19 N3 1.350(9) . ? C19 C20 1.378(10) . ? C20 C22 1.359(10) . ? C21 N3 1.333(9) . ? C21 N4 1.339(9) . ? C21 C46 1.477(10) . ? C22 N4 1.345(9) . ? C22 C23 1.495(10) . ? C23 N5 1.342(9) . ? C23 C24 1.373(11) . ? C24 C25 1.397(11) . ? C25 C26 1.370(11) . ? C26 C27 1.378(11) . ? C27 N5 1.342(9) . ? C27 C28 1.496(11) . ? C28 C40 1.413(11) . ? C28 C29 1.416(11) . ? C29 C34 1.413(11) . ? C29 C30 1.419(12) . ? C30 C31 1.361(12) . ? C31 C32 1.422(13) . ? C32 C33 1.349(12) . ? C33 C34 1.428(11) . ? C34 N6 1.343(10) . ? C35 N6 1.358(10) . ? C35 C36 1.389(12) . ? C35 C40 1.422(11) . ? C36 C37 1.352(13) . ? C37 C38 1.417(14) . ? C38 C39 1.348(13) . ? C39 C40 1.436(12) . ? C41 C42 1.376(11) . ? C41 C46 1.387(11) . ? C42 C43 1.408(12) . ? C43 C44 1.385(12) . ? C43 C47 1.509(11) . ? C44 C45 1.373(11) . ? C45 C46 1.389(10) . ? C47 C48 1.549(13) . ? C48 C49 1.512(12) . ? C49 C50 1.526(14) . ? C51 F2 1.254(16) . ? C51 F3 1.325(15) . ? C51 F1 1.359(15) . ? C51 C52 1.503(18) . ? C52 O1 1.181(13) . ? C52 O2 1.282(15) . ? C53 O3 1.193(11) . ? C53 O4 1.255(12) . ? C53 C54 1.534(14) . ? C54 F6 1.286(13) . ? C54 F4 1.314(11) . ? C54 F5 1.328(13) . ? C55 C57 1.40(3) 2_566 ? C55 C56 1.53(3) . ? C56 C57 1.62(5) . ? C57 C55 1.40(3) 2_566 ? C58 Cl1 1.730(12) . ? C58 Cl2 1.747(14) . ? C58 Cl3 1.750(12) . ? C59 O5 1.34(3) . ? C59 O5' 1.41(3) . ? C59 Cl7' 1.63(3) . ? C59 Cl6' 1.65(3) . ? C59 Cl7 1.68(4) . ? C59 Cl6 1.79(3) . ? C59 Cl7" 1.84(4) . ? C59 Cl8 1.94(3) . ? C59 Cl8' 2.13(4) . ? Cl6 Cl6' 0.794(16) . ? Cl6' Cl8' 2.15(3) . ? Cl7 Cl7' 0.736(19) . ? Cl7 Cl7" 0.734(18) . ? Cl7' Cl7" 1.22(2) . ? Cl7' O5' 1.99(2) . ? Cl7" Cl8' 2.35(2) . ? Cl7" Cl8 2.47(2) . ? Cl8 Cl8' 1.25(2) . ? Cl8 Cl8' 1.82(2) 2_6:5 ? Cl8 O5 1.95(2) . ? Cl8 Cl8 2.16(3) 2_6:5 ? Cl8' Cl8 1.82(2) 2_6:5 ? Cl8' Cl8' 2.25(4) 2_6:5 ? O5 O5' 1.000(16) . ? 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 C13 C1 C2 121.0(7) . . ? C13 C1 C14 119.4(7) . . ? C2 C1 C14 119.6(7) . . ? C1 C2 C3 124.2(7) . . ? C1 C2 C7 118.1(7) . . ? C3 C2 C7 117.7(7) . . ? C4 C3 C2 121.0(7) . . ? C3 C4 C5 119.7(8) . . ? C6 C5 C4 121.3(7) . . ? C5 C6 C7 119.4(7) . . ? N1 C7 C6 119.8(7) . . ? N1 C7 C2 119.5(7) . . ? C6 C7 C2 120.8(7) . . ? N1 C8 C9 119.4(7) . . ? N1 C8 C13 118.6(7) . . ? C9 C8 C13 122.1(7) . . ? C10 C9 C8 118.1(8) . . ? C9 C10 C11 121.2(9) . . ? C12 C11 C10 121.4(9) . . ? C11 C12 C13 120.7(8) . . ? C1 C13 C12 124.2(7) . . ? C1 C13 C8 119.2(7) . . ? C12 C13 C8 116.6(7) . . ? N2 C14 C15 124.7(7) . . ? N2 C14 C1 115.5(6) . . ? C15 C14 C1 119.8(7) . . ? C16 C15 C14 117.0(7) . . ? C17 C16 C15 120.0(7) . . ? C16 C17 C18 119.3(7) . . ? N2 C18 C17 121.6(7) . . ? N2 C18 C19 116.2(6) . . ? C17 C18 C19 122.2(7) . . ? N3 C19 C20 120.5(7) . . ? N3 C19 C18 117.6(6) . . ? C20 C19 C18 121.9(6) . . ? C22 C20 C19 118.3(7) . . ? N3 C21 N4 125.4(6) . . ? N3 C21 C46 117.0(6) . . ? N4 C21 C46 117.6(6) . . ? N4 C22 C20 122.1(7) . . ? N4 C22 C23 116.3(6) . . ? C20 C22 C23 121.6(7) . . ? N5 C23 C24 123.5(7) . . ? N5 C23 C22 115.4(6) . . ? C24 C23 C22 121.1(7) . . ? C23 C24 C25 118.9(7) . . ? C26 C25 C24 118.3(8) . . ? C25 C26 C27 119.0(7) . . ? N5 C27 C26 123.8(7) . . ? N5 C27 C28 114.9(7) . . ? C26 C27 C28 121.3(7) . . ? C40 C28 C29 118.9(7) . . ? C40 C28 C27 120.2(7) . . ? C29 C28 C27 120.9(8) . . ? C28 C29 C34 118.9(8) . . ? C28 C29 C30 123.2(7) . . ? C34 C29 C30 117.9(7) . . ? C31 C30 C29 120.9(8) . . ? C30 C31 C32 119.8(9) . . ? C33 C32 C31 122.0(8) . . ? C32 C33 C34 118.3(8) . . ? N6 C34 C29 120.4(7) . . ? N6 C34 C33 118.5(7) . . ? C29 C34 C33 121.0(8) . . ? N6 C35 C36 120.0(7) . . ? N6 C35 C40 118.8(8) . . ? C36 C35 C40 121.2(8) . . ? C37 C36 C35 119.8(9) . . ? C36 C37 C38 120.8(10) . . ? C39 C38 C37 120.6(9) . . ? C38 C39 C40 120.5(8) . . ? C28 C40 C35 119.8(7) . . ? C28 C40 C39 123.1(7) . . ? C35 C40 C39 117.1(8) . . ? C42 C41 C46 121.8(7) . . ? C41 C42 C43 120.2(8) . . ? C44 C43 C42 117.6(7) . . ? C44 C43 C47 121.4(8) . . ? C42 C43 C47 120.9(8) . . ? C45 C44 C43 121.6(7) . . ? C44 C45 C46 121.1(7) . . ? C45 C46 C41 117.7(7) . . ? C45 C46 C21 121.0(7) . . ? C41 C46 C21 121.2(7) . . ? C43 C47 C48 114.4(8) . . ? C49 C48 C47 112.9(8) . . ? C48 C49 C50 111.6(9) . . ? C8 N1 C7 123.5(6) . . ? C14 N2 C18 117.4(6) . . ? C21 N3 C19 117.3(6) . . ? C22 N4 C21 116.3(6) . . ? C23 N5 C27 116.5(6) . . ? C34 N6 C35 123.2(7) . . ? F2 C51 F3 110.9(15) . . ? F2 C51 F1 104.7(13) . . ? F3 C51 F1 104.4(9) . . ? F2 C51 C52 112.8(11) . . ? F3 C51 C52 113.2(12) . . ? F1 C51 C52 110.2(13) . . ? O1 C52 O2 130.7(11) . . ? O1 C52 C51 120.5(12) . . ? O2 C52 C51 108.8(12) . . ? O3 C53 O4 130.1(9) . . ? O3 C53 C54 116.4(9) . . ? O4 C53 C54 112.5(10) . . ? F6 C54 F4 107.4(9) . . ? F6 C54 F5 102.7(9) . . ? F4 C54 F5 107.2(10) . . ? F6 C54 C53 114.5(10) . . ? F4 C54 C53 113.1(9) . . ? F5 C54 C53 111.2(8) . . ? C57 C55 C56 116.6(18) 2_566 . ? C55 C56 C57 114.4(12) . . ? C55 C57 C56 111(2) 2_566 . ? Cl1 C58 Cl2 107.3(7) . . ? Cl1 C58 Cl3 113.3(7) . . ? Cl2 C58 Cl3 107.9(6) . . ? O5 C59 O5' 42.6(13) . . ? O5 C59 Cl7' 114(2) . . ? O5' C59 Cl7' 81.4(19) . . ? O5 C59 Cl6' 116(2) . . ? O5' C59 Cl6' 136(3) . . ? Cl7' C59 Cl6' 129(2) . . ? O5 C59 Cl7 139(3) . . ? O5' C59 Cl7 106(2) . . ? Cl7' C59 Cl7 25.6(8) . . ? Cl6' C59 Cl7 105(2) . . ? O5 C59 Cl6 116(2) . . ? O5' C59 Cl6 116(2) . . ? Cl7' C59 Cl6 118(2) . . ? Cl6' C59 Cl6 26.3(8) . . ? Cl7 C59 Cl6 100.0(19) . . ? O5 C59 Cl7" 136(2) . . ? O5' C59 Cl7" 120(2) . . ? Cl7' C59 Cl7" 40.6(10) . . ? Cl6' C59 Cl7" 100.9(19) . . ? Cl7 C59 Cl7" 23.5(8) . . ? Cl6 C59 Cl7" 106.9(18) . . ? O5 C59 Cl8 70.4(17) . . ? O5' C59 Cl8 103(2) . . ? Cl7' C59 Cl8 103.4(18) . . ? Cl6' C59 Cl8 99.4(18) . . ? Cl7 C59 Cl8 103.7(19) . . ? Cl6 C59 Cl8 125(2) . . ? Cl7" C59 Cl8 81.7(15) . . ? O5 C59 Cl8' 99(2) . . ? O5' C59 Cl8' 138(2) . . ? Cl7' C59 Cl8' 110.2(19) . . ? Cl6' C59 Cl8' 68.2(14) . . ? Cl7 C59 Cl8' 95.3(18) . . ? Cl6 C59 Cl8' 94.3(17) . . ? Cl7" C59 Cl8' 72.5(13) . . ? Cl8 C59 Cl8' 35.5(8) . . ? Cl6' Cl6 C59 67.0(17) . . ? Cl6 Cl6' C59 86.7(19) . . ? Cl6 Cl6' Cl8' 152(2) . . ? C59 Cl6' Cl8' 66.5(14) . . ? Cl7' Cl7 Cl7" 112(3) . . ? Cl7' Cl7 C59 74(2) . . ? Cl7" Cl7 C59 90(2) . . ? Cl7 Cl7' Cl7" 33.8(18) . . ? Cl7 Cl7' C59 81(2) . . ? Cl7" Cl7' C59 78.7(15) . . ? Cl7 Cl7' O5' 123(2) . . ? Cl7" Cl7' O5' 120.6(11) . . ? C59 Cl7' O5' 44.4(13) . . ? Cl7 Cl7" Cl7' 33.9(18) . . ? Cl7 Cl7" C59 66(2) . . ? Cl7' Cl7" C59 60.7(13) . . ? Cl7 Cl7" Cl8' 124(2) . . ? Cl7' Cl7" Cl8' 116.3(10) . . ? C59 Cl7" Cl8' 59.4(12) . . ? Cl7 Cl7" Cl8 114(2) . . ? Cl7' Cl7" Cl8 92.9(10) . . ? C59 Cl7" Cl8 50.9(11) . . ? Cl8' Cl7" Cl8 29.9(5) . . ? Cl8' Cl8 Cl8' 92.4(17) . 2_6:5 ? Cl8' Cl8 O5 112.3(16) . . ? Cl8' Cl8 O5 147.9(14) 2_6:5 . ? Cl8' Cl8 C59 80.5(17) . . ? Cl8' Cl8 C59 171.7(18) 2_6:5 . ? O5 Cl8 C59 40.3(11) . . ? Cl8' Cl8 Cl8 57.0(13) . 2_6:5 ? Cl8' Cl8 Cl8 35.3(8) 2_6:5 2_6:5 ? O5 Cl8 Cl8 158.6(13) . 2_6:5 ? C59 Cl8 Cl8 137.3(17) . 2_6:5 ? Cl8' Cl8 Cl7" 69.9(13) . . ? Cl8' Cl8 Cl7" 126.2(10) 2_6:5 . ? O5 Cl8 Cl7" 83.1(7) . . ? C59 Cl8 Cl7" 47.4(11) . . ? Cl8 Cl8 Cl7" 107.3(11) 2_6:5 . ? Cl8 Cl8' Cl8 87.6(17) . 2_6:5 ? Cl8 Cl8' C59 64.0(15) . . ? Cl8 Cl8' C59 151.4(18) 2_6:5 . ? Cl8 Cl8' Cl6' 104.1(16) . . ? Cl8 Cl8' Cl6' 159.0(13) 2_6:5 . ? C59 Cl8' Cl6' 45.3(10) . . ? Cl8 Cl8' Cl8' 53.8(12) . 2_6:5 ? Cl8 Cl8' Cl8' 33.8(7) 2_6:5 2_6:5 ? C59 Cl8' Cl8' 117.7(17) . 2_6:5 ? Cl6' Cl8' Cl8' 152.9(16) . 2_6:5 ? Cl8 Cl8' Cl7" 80.2(13) . . ? Cl8 Cl8' Cl7" 126.7(11) 2_6:5 . ? C59 Cl8' Cl7" 48.1(10) . . ? Cl6' Cl8' Cl7" 73.2(8) . . ? Cl8' Cl8' Cl7" 112.8(13) 2_6:5 . ? O5' O5 C59 72.4(17) . . ? O5' O5 Cl8 124.3(14) . . ? C59 O5 Cl8 69.3(16) . . ? O5 O5' C59 65.0(17) . . ? O5 O5' Cl7' 109.3(14) . . ? C59 O5' Cl7' 54.2(15) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.732 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.084