_publ_contact_author_name 'Trevor W. Hayton' _publ_contact_author_email 'hayton@chem.ucsb.edu' loop_ _publ_author_name 'Skye Fortier' 'Guang Wu' 'Trevor W. Hayton' _journal_full_name 'Journal of the American Chemical Society' data_Complex_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Lithium bis(tert-butanol) Uranium(V) hexakis(pentafluorophenoxide) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H20 F30 Li O8 U' _chemical_formula_weight 1491.57 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 '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 11.0061(17) _cell_length_b 11.9492(18) _cell_length_c 20.903(3) _cell_angle_alpha 94.746(2) _cell_angle_beta 90.733(2) _cell_angle_gamma 114.593(2) _cell_volume 2487.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular_block _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.008 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1426 _exptl_absorpt_coefficient_mu 3.427 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.388 _exptl_absorpt_correction_T_max 0.482 _exptl_absorpt_process_details 'Psi Scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19511 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.1198 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 26.12 _reflns_number_total 9423 _reflns_number_gt 5872 _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^)+(0.0556P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9423 _refine_ls_number_parameters 763 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 0.901 _refine_ls_restrained_S_all 0.901 _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 U1 U 0.88401(3) 0.33939(3) 0.248803(15) 0.04094(12) Uani 1 1 d . . . O5 O 0.7550(5) 0.2925(5) 0.3255(2) 0.0459(14) Uani 1 1 d . . . O1 O 1.0186(4) 0.2677(4) 0.2931(2) 0.0359(12) Uani 1 1 d . . . O6 O 1.0124(5) 0.3807(4) 0.1720(2) 0.0404(13) Uani 1 1 d . . . F27 F 1.2066(4) 0.3900(4) -0.0307(2) 0.0525(12) Uani 1 1 d . . . O3 O 0.7514(5) 0.3880(5) 0.1995(2) 0.0478(14) Uani 1 1 d . . . F6 F 0.8319(4) 0.1465(4) 0.0800(2) 0.0564(13) Uani 1 1 d . . . F28 F 1.2175(4) 0.6191(4) -0.0415(2) 0.0518(12) Uani 1 1 d . . . F26 F 1.1094(4) 0.2724(4) 0.0758(2) 0.0539(12) Uani 1 1 d . . . F29 F 1.1305(4) 0.7307(4) 0.0543(2) 0.0539(12) Uani 1 1 d . . . O2 O 0.7935(5) 0.1474(5) 0.2094(2) 0.0419(13) Uani 1 1 d . . . F30 F 1.0272(4) 0.6114(4) 0.1588(2) 0.0531(12) Uani 1 1 d . . . O4 O 0.9992(5) 0.5094(5) 0.2984(3) 0.0523(15) Uani 1 1 d . . . F10 F 0.5576(4) -0.0249(5) 0.2496(2) 0.0645(14) Uani 1 1 d . . . C7 C 0.7005(7) 0.0655(7) 0.1675(4) 0.0341(18) Uani 1 1 d . . . F25 F 0.7722(5) 0.3218(5) 0.4572(2) 0.0707(15) Uani 1 1 d . . . F8 F 0.4170(5) -0.1909(5) 0.0356(2) 0.0697(15) Uani 1 1 d . . . F24 F 0.5500(6) 0.2611(6) 0.5240(3) 0.097(2) Uani 1 1 d . . . F5 F 1.2564(4) 0.3472(5) 0.2290(2) 0.0655(14) Uani 1 1 d . . . F9 F 0.3717(4) -0.1896(5) 0.1633(3) 0.0726(15) Uani 1 1 d . . . F21 F 0.5060(5) 0.1946(5) 0.2644(2) 0.0672(14) Uani 1 1 d . . . C32 C 1.1136(7) 0.3864(7) 0.0713(4) 0.0366(18) Uani 1 1 d . . . F15 F 0.7972(5) 0.6277(5) 0.2345(2) 0.0668(14) Uani 1 1 d . . . F7 F 0.6460(5) -0.0212(5) -0.0050(2) 0.0710(15) Uani 1 1 d . . . F4 F 1.4940(4) 0.4709(5) 0.2934(3) 0.0764(16) Uani 1 1 d . . . F1 F 1.0377(4) 0.3292(5) 0.4221(2) 0.0714(15) Uani 1 1 d . . . C34 C 1.1710(6) 0.5617(7) 0.0119(4) 0.0369(19) Uani 1 1 d . . . F11 F 0.5445(5) 0.2503(5) 0.1121(2) 0.0643(14) Uani 1 1 d . . . C19 C 1.0764(9) 0.6148(8) 0.3343(4) 0.052(2) Uani 1 1 d . . . C28 C 0.4167(10) 0.1948(9) 0.4291(5) 0.064(3) Uani 1 1 d . . . F22 F 0.2836(5) 0.1274(5) 0.3308(3) 0.0793(16) Uani 1 1 d . . . F3 F 1.5072(5) 0.5224(5) 0.4222(3) 0.0829(17) Uani 1 1 d . . . C12 C 0.5801(8) -0.0223(7) 0.1864(4) 0.0406(19) Uani 1 1 d . . . C30 C 0.6525(9) 0.2766(8) 0.4260(4) 0.050(2) Uani 1 1 d . . . C33 C 1.1652(7) 0.4460(8) 0.0178(3) 0.0383(19) Uani 1 1 d . . . C31 C 1.0669(7) 0.4420(7) 0.1200(3) 0.0369(18) Uani 1 1 d . . . C11 C 0.4865(8) -0.1055(8) 0.1435(4) 0.046(2) Uani 1 1 d . . . F23 F 0.3034(6) 0.1647(6) 0.4616(3) 0.100(2) Uani 1 1 d . . . C1 C 1.1398(8) 0.3309(7) 0.3241(4) 0.042(2) Uani 1 1 d . . . C13 C 0.6743(7) 0.4380(8) 0.1734(4) 0.0394(19) Uani 1 1 d . . . C8 C 0.7190(7) 0.0627(7) 0.1019(4) 0.043(2) Uani 1 1 d . . . F2 F 1.2772(5) 0.4515(6) 0.4864(3) 0.096(2) Uani 1 1 d . . . F12 F 0.3983(5) 0.3536(6) 0.0578(3) 0.097(2) Uani 1 1 d . . . C2 C 1.1494(8) 0.3612(8) 0.3891(4) 0.047(2) Uani 1 1 d . . . C25 C 0.6448(8) 0.2599(7) 0.3594(4) 0.044(2) Uani 1 1 d . . . C36 C 1.0751(7) 0.5580(7) 0.1132(4) 0.0376(19) Uani 1 1 d . . . C35 C 1.1269(7) 0.6182(7) 0.0598(4) 0.0386(19) Uani 1 1 d . . . C10 C 0.5077(8) -0.1082(8) 0.0792(5) 0.052(2) Uani 1 1 d . . . C9 C 0.6229(8) -0.0226(8) 0.0582(4) 0.047(2) Uani 1 1 d . . . C18 C 0.7010(8) 0.5615(9) 0.1914(4) 0.051(2) Uani 1 1 d . . . C26 C 0.5188(8) 0.2106(8) 0.3295(4) 0.048(2) Uani 1 1 d . . . F16 F 0.9018(7) 0.5979(7) 0.3992(3) 0.101(2) Uani 1 1 d . . . F13 F 0.4488(6) 0.5962(6) 0.0921(4) 0.112(2) Uani 1 1 d . . . C14 C 0.5713(8) 0.3695(8) 0.1288(4) 0.050(2) Uani 1 1 d . . . F14 F 0.6471(6) 0.7312(5) 0.1817(3) 0.094(2) Uani 1 1 d . . . C6 C 1.2595(8) 0.3706(8) 0.2930(4) 0.046(2) Uani 1 1 d . . . C5 C 1.3810(8) 0.4353(8) 0.3262(5) 0.055(2) Uani 1 1 d . . . C27 C 0.4047(8) 0.1774(8) 0.3637(5) 0.057(2) Uani 1 1 d . . . C15 C 0.4965(8) 0.4223(10) 0.1021(4) 0.059(3) Uani 1 1 d . . . C24 C 1.2086(12) 0.6759(11) 0.3226(5) 0.081(3) Uani 1 1 d . . . C4 C 1.3879(8) 0.4635(8) 0.3903(4) 0.056(2) Uani 1 1 d . . . C29 C 0.5403(10) 0.2432(10) 0.4599(4) 0.066(3) Uani 1 1 d . . . C3 C 1.2718(9) 0.4259(8) 0.4226(4) 0.059(2) Uani 1 1 d . . . F19 F 1.4189(8) 0.8417(9) 0.3449(4) 0.186(5) Uani 1 1 d . . . F20 F 1.2568(6) 0.6332(7) 0.2700(3) 0.112(2) Uani 1 1 d . . . C17 C 0.6234(9) 0.6126(9) 0.1640(5) 0.064(3) Uani 1 1 d . . . C16 C 0.5214(10) 0.5432(10) 0.1196(6) 0.070(3) Uani 1 1 d . . . C23 C 1.2925(13) 0.7848(12) 0.3599(7) 0.112(5) Uani 1 1 d . . . C20 C 1.0288(11) 0.6576(9) 0.3854(5) 0.068(3) Uani 1 1 d . . . O7 O 1.0362(6) 0.0844(5) 0.1825(3) 0.075(2) Uani 1 1 d . . . O8 O 0.8254(6) -0.0429(6) 0.2978(3) 0.0709(18) Uani 1 1 d . . . C37 C 0.8189(9) -0.0614(8) 0.3652(4) 0.054(2) Uani 1 1 d . . . C41 C 1.0790(9) -0.0061(9) 0.1526(5) 0.070(3) Uani 1 1 d . . . C43 C 1.2234(10) 0.0559(11) 0.1421(6) 0.101(4) Uani 1 1 d . . . H43A H 1.2383 0.1153 0.1114 0.152 Uiso 1 1 calc R . . H43B H 1.2547 -0.0044 0.1260 0.152 Uiso 1 1 calc R . . H43C H 1.2712 0.0973 0.1820 0.152 Uiso 1 1 calc R . . C38 C 0.7536(11) 0.0135(10) 0.3981(6) 0.101(4) Uani 1 1 d . . . H38A H 0.8071 0.0997 0.3947 0.151 Uiso 1 1 calc R . . H38B H 0.7454 -0.0013 0.4426 0.151 Uiso 1 1 calc R . . H38C H 0.6663 -0.0099 0.3782 0.151 Uiso 1 1 calc R . . C40 C 0.9629(11) -0.0156(11) 0.3915(6) 0.101(4) Uani 1 1 d . . . H40A H 1.0073 -0.0574 0.3668 0.151 Uiso 1 1 calc R . . H40B H 0.9634 -0.0324 0.4357 0.151 Uiso 1 1 calc R . . H40C H 1.0087 0.0718 0.3888 0.151 Uiso 1 1 calc R . . C39 C 0.7418(13) -0.1964(10) 0.3715(5) 0.104(4) Uani 1 1 d . . . H39A H 0.6523 -0.2231 0.3536 0.156 Uiso 1 1 calc R . . H39B H 0.7390 -0.2106 0.4161 0.156 Uiso 1 1 calc R . . H39C H 0.7846 -0.2421 0.3488 0.156 Uiso 1 1 calc R . . C21 C 1.1090(17) 0.7632(15) 0.4226(6) 0.102(4) Uani 1 1 d . . . C22 C 1.2373(19) 0.8252(13) 0.4104(6) 0.118(5) Uani 1 1 d . . . C42 C 1.0629(15) -0.0969(11) 0.2032(7) 0.145(7) Uani 1 1 d . . . H42A H 1.0940 -0.0516 0.2447 0.217 Uiso 1 1 calc R . . H42B H 1.1143 -0.1432 0.1923 0.217 Uiso 1 1 calc R . . H42C H 0.9702 -0.1526 0.2043 0.217 Uiso 1 1 calc R . . C44 C 0.9980(16) -0.0554(14) 0.0929(9) 0.183(9) Uani 1 1 d . . . H44A H 0.9072 -0.1055 0.1023 0.275 Uiso 1 1 calc R . . H44B H 1.0325 -0.1048 0.0672 0.275 Uiso 1 1 calc R . . H44C H 1.0006 0.0117 0.0697 0.275 Uiso 1 1 calc R . . F17 F 1.0605(10) 0.8058(7) 0.4726(3) 0.140(3) Uani 1 1 d . . . F18 F 1.3231(11) 0.9260(7) 0.4466(4) 0.192(5) Uani 1 1 d . . . Li1 Li 0.9362(13) 0.0901(13) 0.2528(6) 0.049(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 U1 0.04022(18) 0.0470(2) 0.03806(19) 0.00429(13) 0.00538(12) 0.02054(14) O5 0.042(3) 0.062(4) 0.037(3) 0.004(3) 0.005(2) 0.024(3) O1 0.031(3) 0.038(3) 0.034(3) -0.001(2) -0.001(2) 0.011(2) O6 0.046(3) 0.035(3) 0.040(3) 0.004(2) 0.001(2) 0.016(3) F27 0.056(3) 0.055(3) 0.045(3) -0.005(2) 0.011(2) 0.024(2) O3 0.046(3) 0.055(4) 0.043(3) 0.007(3) 0.004(3) 0.021(3) F6 0.046(3) 0.067(3) 0.043(3) 0.007(2) 0.007(2) 0.010(3) F28 0.050(3) 0.058(3) 0.042(3) 0.012(2) 0.009(2) 0.016(2) F26 0.055(3) 0.048(3) 0.066(3) 0.007(2) 0.015(2) 0.028(2) F29 0.058(3) 0.043(3) 0.065(3) 0.013(2) 0.010(2) 0.023(2) O2 0.042(3) 0.045(3) 0.033(3) 0.005(3) -0.002(2) 0.012(3) F30 0.063(3) 0.046(3) 0.053(3) -0.002(2) 0.015(2) 0.027(2) O4 0.052(3) 0.052(4) 0.054(4) -0.002(3) 0.000(3) 0.024(3) F10 0.054(3) 0.084(4) 0.042(3) 0.016(3) 0.009(2) 0.014(3) C7 0.036(4) 0.038(5) 0.036(5) 0.008(4) -0.001(4) 0.022(4) F25 0.067(3) 0.101(4) 0.048(3) 0.000(3) -0.001(3) 0.041(3) F8 0.053(3) 0.068(4) 0.063(3) -0.008(3) -0.019(3) 0.004(3) F24 0.116(5) 0.164(6) 0.040(3) 0.022(4) 0.028(3) 0.084(5) F5 0.052(3) 0.083(4) 0.051(3) 0.004(3) 0.016(2) 0.019(3) F9 0.045(3) 0.070(4) 0.078(4) 0.016(3) 0.004(3) -0.002(3) F21 0.056(3) 0.093(4) 0.054(3) 0.004(3) 0.002(2) 0.032(3) C32 0.029(4) 0.032(5) 0.047(5) 0.001(4) 0.000(4) 0.012(4) F15 0.055(3) 0.077(4) 0.063(3) -0.011(3) -0.009(3) 0.025(3) F7 0.069(3) 0.093(4) 0.038(3) -0.004(3) -0.003(2) 0.023(3) F4 0.040(3) 0.090(4) 0.088(4) 0.010(3) 0.018(3) 0.015(3) F1 0.044(3) 0.103(4) 0.048(3) -0.006(3) 0.005(2) 0.013(3) C34 0.020(4) 0.046(5) 0.036(5) 0.000(4) -0.003(3) 0.006(4) F11 0.056(3) 0.057(4) 0.071(4) 0.001(3) 0.004(3) 0.016(3) C19 0.057(6) 0.049(6) 0.047(6) 0.006(5) -0.011(5) 0.019(5) C28 0.072(7) 0.090(8) 0.050(6) 0.026(5) 0.027(5) 0.048(6) F22 0.050(3) 0.098(4) 0.094(4) 0.026(3) 0.010(3) 0.033(3) F3 0.043(3) 0.108(5) 0.076(4) 0.001(3) -0.014(3) 0.012(3) C12 0.040(5) 0.044(5) 0.034(5) 0.007(4) -0.005(4) 0.014(4) C30 0.054(5) 0.067(6) 0.038(5) 0.006(4) 0.005(4) 0.034(5) C33 0.030(4) 0.050(5) 0.029(4) -0.008(4) -0.002(3) 0.014(4) C31 0.030(4) 0.044(5) 0.032(4) 0.001(4) 0.005(3) 0.012(4) C11 0.038(5) 0.046(5) 0.056(6) 0.018(5) 0.011(4) 0.016(4) F23 0.082(4) 0.147(6) 0.097(5) 0.053(4) 0.056(4) 0.064(4) C1 0.047(5) 0.035(5) 0.046(5) -0.001(4) 0.001(4) 0.020(4) C13 0.035(4) 0.055(6) 0.037(5) 0.014(4) 0.010(4) 0.026(4) C8 0.035(4) 0.044(5) 0.049(5) 0.013(4) 0.010(4) 0.013(4) F2 0.065(3) 0.140(6) 0.048(4) -0.019(3) -0.007(3) 0.013(4) F12 0.060(3) 0.103(5) 0.116(5) 0.009(4) -0.033(4) 0.022(3) C2 0.039(5) 0.057(6) 0.039(5) 0.005(4) 0.004(4) 0.013(4) C25 0.044(5) 0.052(5) 0.044(5) 0.007(4) 0.015(4) 0.027(4) C36 0.038(4) 0.033(5) 0.038(5) -0.006(4) 0.005(4) 0.012(4) C35 0.029(4) 0.039(5) 0.043(5) 0.003(4) 0.003(4) 0.010(4) C10 0.035(5) 0.041(5) 0.068(7) -0.007(5) -0.009(5) 0.007(4) C9 0.050(5) 0.053(6) 0.038(5) -0.002(4) -0.007(4) 0.022(5) C18 0.042(5) 0.066(7) 0.054(6) 0.008(5) 0.007(4) 0.031(5) C26 0.052(5) 0.059(6) 0.039(5) 0.005(4) 0.008(4) 0.029(5) F16 0.108(5) 0.123(6) 0.092(5) 0.008(4) 0.018(4) 0.068(5) F13 0.076(4) 0.102(5) 0.174(7) 0.039(5) -0.031(4) 0.050(4) C14 0.037(5) 0.051(6) 0.055(6) 0.008(5) 0.011(4) 0.014(5) F14 0.080(4) 0.056(4) 0.159(6) 0.006(4) -0.002(4) 0.041(3) C6 0.048(5) 0.054(6) 0.033(5) -0.001(4) 0.005(4) 0.019(4) C5 0.038(5) 0.057(6) 0.065(6) 0.009(5) 0.014(5) 0.015(4) C27 0.042(5) 0.061(6) 0.077(7) 0.015(5) 0.010(5) 0.028(5) C15 0.031(5) 0.082(8) 0.059(6) 0.005(5) -0.013(4) 0.019(5) C24 0.092(8) 0.084(9) 0.059(7) 0.014(6) 0.026(6) 0.028(7) C4 0.039(5) 0.059(6) 0.055(6) 0.000(5) -0.005(4) 0.007(4) C29 0.074(7) 0.094(8) 0.046(6) 0.021(5) 0.017(5) 0.048(6) C3 0.050(5) 0.064(6) 0.048(6) -0.009(5) -0.002(5) 0.011(5) F19 0.105(6) 0.188(9) 0.167(8) 0.083(7) -0.009(6) -0.048(6) F20 0.083(4) 0.138(6) 0.109(6) 0.039(5) 0.018(4) 0.036(4) C17 0.049(6) 0.058(7) 0.082(7) 0.010(6) 0.012(5) 0.020(5) C16 0.051(6) 0.065(7) 0.101(9) 0.024(6) 0.000(6) 0.028(6) C23 0.083(9) 0.087(10) 0.099(11) 0.049(9) -0.027(8) -0.036(8) C20 0.086(8) 0.050(6) 0.052(6) -0.012(5) -0.009(6) 0.016(6) O7 0.087(5) 0.045(4) 0.096(5) 0.005(3) 0.049(4) 0.029(3) O8 0.076(4) 0.064(4) 0.053(4) 0.022(3) -0.002(3) 0.007(4) C37 0.064(6) 0.057(6) 0.048(6) 0.020(4) 0.012(4) 0.030(5) C41 0.054(6) 0.058(7) 0.089(8) -0.024(6) 0.017(6) 0.018(5) C43 0.078(8) 0.119(10) 0.117(10) 0.009(8) 0.038(7) 0.051(8) C38 0.085(8) 0.076(8) 0.139(11) -0.022(7) 0.014(8) 0.037(7) C40 0.095(9) 0.129(11) 0.097(9) -0.009(8) -0.020(7) 0.070(8) C39 0.155(12) 0.070(8) 0.082(9) 0.021(6) 0.049(8) 0.039(8) C21 0.151(13) 0.131(13) 0.048(8) 0.015(8) 0.004(8) 0.082(12) C22 0.165(15) 0.093(11) 0.057(9) 0.002(8) 0.020(10) 0.016(11) C42 0.200(16) 0.069(9) 0.207(17) 0.049(10) 0.109(14) 0.088(10) C44 0.159(14) 0.143(14) 0.28(2) -0.109(15) -0.076(15) 0.119(12) F17 0.257(10) 0.121(6) 0.062(4) -0.012(4) 0.006(5) 0.104(7) F18 0.286(12) 0.075(5) 0.111(6) -0.020(5) -0.054(7) -0.019(6) Li1 0.050(8) 0.063(10) 0.034(8) -0.001(7) 0.001(6) 0.026(7) _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 U1 O4 2.069(6) . ? U1 O3 2.072(5) . ? U1 O6 2.103(5) . ? U1 O5 2.108(5) . ? U1 O2 2.168(5) . ? U1 O1 2.222(5) . ? U1 Li1 3.267(14) . ? O5 C25 1.341(8) . ? O1 C1 1.352(9) . ? O1 Li1 2.029(15) . ? O6 C31 1.364(8) . ? F27 C33 1.357(8) . ? O3 C13 1.357(9) . ? F6 C8 1.345(8) . ? F28 C34 1.351(8) . ? F26 C32 1.355(8) . ? F29 C35 1.342(8) . ? O2 C7 1.331(8) . ? O2 Li1 2.172(15) . ? F30 C36 1.337(8) . ? O4 C19 1.345(10) . ? F10 C12 1.347(8) . ? C7 C8 1.390(10) . ? C7 C12 1.392(10) . ? F25 C30 1.334(9) . ? F8 C10 1.345(9) . ? F24 C29 1.334(10) . ? F5 C6 1.341(8) . ? F9 C11 1.343(8) . ? F21 C26 1.356(9) . ? C32 C33 1.375(10) . ? C32 C31 1.389(10) . ? F15 C18 1.312(9) . ? F7 C9 1.349(9) . ? F4 C5 1.352(8) . ? F1 C2 1.344(8) . ? C34 C35 1.367(10) . ? C34 C33 1.373(10) . ? F11 C14 1.343(9) . ? C19 C20 1.350(12) . ? C19 C24 1.366(13) . ? C28 F23 1.355(9) . ? C28 C27 1.363(12) . ? C28 C29 1.364(13) . ? F22 C27 1.361(10) . ? F3 C4 1.339(9) . ? C12 C11 1.352(11) . ? C30 C29 1.359(11) . ? C30 C25 1.387(11) . ? C31 C36 1.372(10) . ? C11 C10 1.368(11) . ? C1 C2 1.369(10) . ? C1 C6 1.391(10) . ? C13 C14 1.378(11) . ? C13 C18 1.396(11) . ? C8 C9 1.384(11) . ? F2 C3 1.339(10) . ? F12 C15 1.346(10) . ? C2 C3 1.385(11) . ? C25 C26 1.377(11) . ? C36 C35 1.377(10) . ? C10 C9 1.363(11) . ? C18 C17 1.381(12) . ? C26 C27 1.378(11) . ? F16 C20 1.327(11) . ? F13 C16 1.357(10) . ? C14 C15 1.366(12) . ? F14 C17 1.347(10) . ? C6 C5 1.377(11) . ? C5 C4 1.348(12) . ? C15 C16 1.370(13) . ? C24 F20 1.377(11) . ? C24 C23 1.403(16) . ? C4 C3 1.372(11) . ? F19 C23 1.325(14) . ? C17 C16 1.371(13) . ? C23 C22 1.375(19) . ? C20 C21 1.368(16) . ? O7 C41 1.450(10) . ? O7 Li1 1.861(13) . ? O8 C37 1.441(9) . ? O8 Li1 1.888(15) . ? C37 C38 1.496(12) . ? C37 C39 1.496(13) . ? C37 C40 1.523(13) . ? C41 C44 1.453(18) . ? C41 C43 1.476(12) . ? C41 C42 1.538(16) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C21 C22 1.333(18) . ? C21 F17 1.338(13) . ? C22 F18 1.342(15) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 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 O4 U1 O3 98.7(2) . . ? O4 U1 O6 91.2(2) . . ? O3 U1 O6 90.72(19) . . ? O4 U1 O5 90.1(2) . . ? O3 U1 O5 90.22(19) . . ? O6 U1 O5 178.3(2) . . ? O4 U1 O2 166.59(19) . . ? O3 U1 O2 94.7(2) . . ? O6 U1 O2 89.25(18) . . ? O5 U1 O2 89.22(19) . . ? O4 U1 O1 87.78(19) . . ? O3 U1 O1 173.13(19) . . ? O6 U1 O1 86.98(18) . . ? O5 U1 O1 91.92(18) . . ? O2 U1 O1 78.85(18) . . ? O4 U1 Li1 125.4(3) . . ? O3 U1 Li1 135.7(3) . . ? O6 U1 Li1 86.2(3) . . ? O5 U1 Li1 92.1(3) . . ? O2 U1 Li1 41.2(3) . . ? O1 U1 Li1 37.7(3) . . ? C25 O5 U1 161.7(5) . . ? C1 O1 Li1 128.5(6) . . ? C1 O1 U1 129.2(4) . . ? Li1 O1 U1 100.3(4) . . ? C31 O6 U1 153.8(5) . . ? C13 O3 U1 170.4(5) . . ? C7 O2 U1 144.5(5) . . ? C7 O2 Li1 117.4(6) . . ? U1 O2 Li1 97.7(4) . . ? C19 O4 U1 175.2(5) . . ? O2 C7 C8 121.4(7) . . ? O2 C7 C12 122.6(7) . . ? C8 C7 C12 116.0(7) . . ? F26 C32 C33 118.8(7) . . ? F26 C32 C31 120.5(7) . . ? C33 C32 C31 120.7(7) . . ? F28 C34 C35 119.7(7) . . ? F28 C34 C33 120.6(6) . . ? C35 C34 C33 119.7(7) . . ? O4 C19 C20 121.4(9) . . ? O4 C19 C24 120.0(9) . . ? C20 C19 C24 118.4(10) . . ? F23 C28 C27 118.0(9) . . ? F23 C28 C29 122.0(9) . . ? C27 C28 C29 120.0(8) . . ? F10 C12 C11 119.3(7) . . ? F10 C12 C7 118.5(7) . . ? C11 C12 C7 122.2(7) . . ? F25 C30 C29 119.6(8) . . ? F25 C30 C25 119.2(7) . . ? C29 C30 C25 121.2(8) . . ? F27 C33 C34 119.0(7) . . ? F27 C33 C32 120.6(7) . . ? C34 C33 C32 120.3(7) . . ? O6 C31 C36 121.9(6) . . ? O6 C31 C32 120.3(7) . . ? C36 C31 C32 117.8(7) . . ? F9 C11 C12 120.7(7) . . ? F9 C11 C10 118.4(8) . . ? C12 C11 C10 120.9(7) . . ? O1 C1 C2 120.3(7) . . ? O1 C1 C6 123.3(7) . . ? C2 C1 C6 116.4(7) . . ? O3 C13 C14 121.0(8) . . ? O3 C13 C18 119.5(7) . . ? C14 C13 C18 119.5(8) . . ? F6 C8 C9 119.1(7) . . ? F6 C8 C7 119.3(7) . . ? C9 C8 C7 121.6(7) . . ? F1 C2 C1 119.7(7) . . ? F1 C2 C3 118.3(7) . . ? C1 C2 C3 121.9(7) . . ? O5 C25 C26 121.5(7) . . ? O5 C25 C30 121.6(7) . . ? C26 C25 C30 116.9(7) . . ? F30 C36 C31 118.5(6) . . ? F30 C36 C35 119.8(7) . . ? C31 C36 C35 121.7(7) . . ? F29 C35 C34 120.4(7) . . ? F29 C35 C36 119.8(6) . . ? C34 C35 C36 119.8(7) . . ? F8 C10 C9 118.6(8) . . ? F8 C10 C11 122.2(7) . . ? C9 C10 C11 119.1(8) . . ? F7 C9 C10 120.7(7) . . ? F7 C9 C8 119.2(7) . . ? C10 C9 C8 120.1(8) . . ? F15 C18 C17 120.4(9) . . ? F15 C18 C13 120.4(8) . . ? C17 C18 C13 119.2(9) . . ? F21 C26 C25 119.2(7) . . ? F21 C26 C27 118.7(8) . . ? C25 C26 C27 122.1(8) . . ? F11 C14 C15 120.3(8) . . ? F11 C14 C13 119.5(8) . . ? C15 C14 C13 120.2(9) . . ? F5 C6 C5 119.1(7) . . ? F5 C6 C1 119.2(7) . . ? C5 C6 C1 121.6(7) . . ? C4 C5 F4 120.2(8) . . ? C4 C5 C6 120.8(7) . . ? F4 C5 C6 119.0(8) . . ? F22 C27 C28 122.2(8) . . ? F22 C27 C26 118.8(8) . . ? C28 C27 C26 119.1(9) . . ? F12 C15 C14 118.8(9) . . ? F12 C15 C16 120.4(9) . . ? C14 C15 C16 120.8(9) . . ? C19 C24 F20 118.4(10) . . ? C19 C24 C23 121.5(11) . . ? F20 C24 C23 119.9(11) . . ? F3 C4 C5 120.1(8) . . ? F3 C4 C3 120.7(8) . . ? C5 C4 C3 119.1(8) . . ? F24 C29 C30 120.2(9) . . ? F24 C29 C28 119.1(8) . . ? C30 C29 C28 120.6(9) . . ? F2 C3 C4 119.8(8) . . ? F2 C3 C2 120.1(7) . . ? C4 C3 C2 120.1(8) . . ? F14 C17 C16 119.7(9) . . ? F14 C17 C18 119.7(9) . . ? C16 C17 C18 120.5(10) . . ? F13 C16 C15 120.7(10) . . ? F13 C16 C17 119.5(10) . . ? C15 C16 C17 119.7(9) . . ? F19 C23 C22 124.2(14) . . ? F19 C23 C24 118.6(15) . . ? C22 C23 C24 117.2(12) . . ? F16 C20 C19 119.8(9) . . ? F16 C20 C21 119.2(11) . . ? C19 C20 C21 120.9(11) . . ? C41 O7 Li1 134.8(7) . . ? C37 O8 Li1 132.2(7) . . ? O8 C37 C38 109.1(8) . . ? O8 C37 C39 108.4(8) . . ? C38 C37 C39 111.4(8) . . ? O8 C37 C40 106.5(8) . . ? C38 C37 C40 110.0(9) . . ? C39 C37 C40 111.3(9) . . ? O7 C41 C44 105.7(9) . . ? O7 C41 C43 108.7(8) . . ? C44 C41 C43 112.7(11) . . ? O7 C41 C42 105.4(8) . . ? C44 C41 C42 117.2(12) . . ? C43 C41 C42 106.7(11) . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C22 C21 F17 118.6(15) . . ? C22 C21 C20 120.9(13) . . ? F17 C21 C20 120.5(14) . . ? C21 C22 F18 124.0(15) . . ? C21 C22 C23 120.9(14) . . ? F18 C22 C23 115.0(15) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O7 Li1 O8 127.7(8) . . ? O7 Li1 O1 106.3(7) . . ? O8 Li1 O1 122.5(7) . . ? O7 Li1 O2 100.6(6) . . ? O8 Li1 O2 102.5(6) . . ? O1 Li1 O2 83.1(5) . . ? O7 Li1 U1 106.7(6) . . ? O8 Li1 U1 121.5(6) . . ? O1 Li1 U1 42.0(3) . . ? O2 Li1 U1 41.1(3) . . ? 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 O4 U1 O5 C25 120.3(16) . . . . ? O3 U1 O5 C25 21.5(16) . . . . ? O6 U1 O5 C25 -101(7) . . . . ? O2 U1 O5 C25 -73.1(16) . . . . ? O1 U1 O5 C25 -151.9(16) . . . . ? Li1 U1 O5 C25 -114.2(16) . . . . ? O4 U1 O1 C1 -14.2(6) . . . . ? O3 U1 O1 C1 147.6(14) . . . . ? O6 U1 O1 C1 77.1(6) . . . . ? O5 U1 O1 C1 -104.3(6) . . . . ? O2 U1 O1 C1 166.9(6) . . . . ? Li1 U1 O1 C1 164.8(7) . . . . ? O4 U1 O1 Li1 -179.0(4) . . . . ? O3 U1 O1 Li1 -17.2(16) . . . . ? O6 U1 O1 Li1 -87.7(4) . . . . ? O5 U1 O1 Li1 90.9(4) . . . . ? O2 U1 O1 Li1 2.1(4) . . . . ? O4 U1 O6 C31 -70.9(10) . . . . ? O3 U1 O6 C31 27.9(10) . . . . ? O5 U1 O6 C31 151(6) . . . . ? O2 U1 O6 C31 122.5(10) . . . . ? O1 U1 O6 C31 -158.6(10) . . . . ? Li1 U1 O6 C31 163.7(11) . . . . ? O4 U1 O3 C13 -8(3) . . . . ? O6 U1 O3 C13 -99(3) . . . . ? O5 U1 O3 C13 82(3) . . . . ? O2 U1 O3 C13 171(3) . . . . ? O1 U1 O3 C13 -170(2) . . . . ? Li1 U1 O3 C13 175(3) . . . . ? O4 U1 O2 C7 -177.3(8) . . . . ? O3 U1 O2 C7 5.3(8) . . . . ? O6 U1 O2 C7 -85.4(8) . . . . ? O5 U1 O2 C7 95.4(8) . . . . ? O1 U1 O2 C7 -172.4(8) . . . . ? Li1 U1 O2 C7 -170.5(9) . . . . ? O4 U1 O2 Li1 -6.8(10) . . . . ? O3 U1 O2 Li1 175.8(4) . . . . ? O6 U1 O2 Li1 85.1(4) . . . . ? O5 U1 O2 Li1 -94.1(4) . . . . ? O1 U1 O2 Li1 -2.0(4) . . . . ? O3 U1 O4 C19 154(7) . . . . ? O6 U1 O4 C19 -115(7) . . . . ? O5 U1 O4 C19 63(7) . . . . ? O2 U1 O4 C19 -24(7) . . . . ? O1 U1 O4 C19 -28(7) . . . . ? Li1 U1 O4 C19 -29(7) . . . . ? U1 O2 C7 C8 75.6(10) . . . . ? Li1 O2 C7 C8 -93.7(8) . . . . ? U1 O2 C7 C12 -104.6(9) . . . . ? Li1 O2 C7 C12 86.0(8) . . . . ? U1 O4 C19 C20 -82(7) . . . . ? U1 O4 C19 C24 93(7) . . . . ? O2 C7 C12 F10 -0.6(11) . . . . ? C8 C7 C12 F10 179.1(7) . . . . ? O2 C7 C12 C11 -179.7(7) . . . . ? C8 C7 C12 C11 0.0(11) . . . . ? F28 C34 C33 F27 -0.1(10) . . . . ? C35 C34 C33 F27 178.6(6) . . . . ? F28 C34 C33 C32 -177.8(6) . . . . ? C35 C34 C33 C32 0.8(11) . . . . ? F26 C32 C33 F27 2.4(10) . . . . ? C31 C32 C33 F27 -177.8(6) . . . . ? F26 C32 C33 C34 -179.9(6) . . . . ? C31 C32 C33 C34 0.0(11) . . . . ? U1 O6 C31 C36 27.3(15) . . . . ? U1 O6 C31 C32 -151.4(8) . . . . ? F26 C32 C31 O6 -2.0(10) . . . . ? C33 C32 C31 O6 178.1(6) . . . . ? F26 C32 C31 C36 179.3(6) . . . . ? C33 C32 C31 C36 -0.6(11) . . . . ? F10 C12 C11 F9 0.4(12) . . . . ? C7 C12 C11 F9 179.5(7) . . . . ? F10 C12 C11 C10 -177.8(7) . . . . ? C7 C12 C11 C10 1.2(13) . . . . ? Li1 O1 C1 C2 -109.5(9) . . . . ? U1 O1 C1 C2 89.8(8) . . . . ? Li1 O1 C1 C6 71.7(10) . . . . ? U1 O1 C1 C6 -89.0(8) . . . . ? U1 O3 C13 C14 -175(2) . . . . ? U1 O3 C13 C18 6(3) . . . . ? O2 C7 C8 F6 -1.6(11) . . . . ? C12 C7 C8 F6 178.6(6) . . . . ? O2 C7 C8 C9 179.7(7) . . . . ? C12 C7 C8 C9 -0.1(11) . . . . ? O1 C1 C2 F1 -0.9(12) . . . . ? C6 C1 C2 F1 178.0(7) . . . . ? O1 C1 C2 C3 180.0(8) . . . . ? C6 C1 C2 C3 -1.1(13) . . . . ? U1 O5 C25 C26 16(2) . . . . ? U1 O5 C25 C30 -162.7(12) . . . . ? F25 C30 C25 O5 -2.5(12) . . . . ? C29 C30 C25 O5 -179.9(8) . . . . ? F25 C30 C25 C26 178.7(8) . . . . ? C29 C30 C25 C26 1.3(13) . . . . ? O6 C31 C36 F30 -0.5(11) . . . . ? C32 C31 C36 F30 178.2(6) . . . . ? O6 C31 C36 C35 -178.2(7) . . . . ? C32 C31 C36 C35 0.5(11) . . . . ? F28 C34 C35 F29 -0.5(10) . . . . ? C33 C34 C35 F29 -179.2(6) . . . . ? F28 C34 C35 C36 177.7(6) . . . . ? C33 C34 C35 C36 -1.0(11) . . . . ? F30 C36 C35 F29 0.8(11) . . . . ? C31 C36 C35 F29 178.5(7) . . . . ? F30 C36 C35 C34 -177.4(6) . . . . ? C31 C36 C35 C34 0.3(11) . . . . ? F9 C11 C10 F8 1.0(12) . . . . ? C12 C11 C10 F8 179.2(7) . . . . ? F9 C11 C10 C9 179.3(7) . . . . ? C12 C11 C10 C9 -2.5(13) . . . . ? F8 C10 C9 F7 -0.4(12) . . . . ? C11 C10 C9 F7 -178.8(7) . . . . ? F8 C10 C9 C8 -179.2(7) . . . . ? C11 C10 C9 C8 2.4(13) . . . . ? F6 C8 C9 F7 1.3(11) . . . . ? C7 C8 C9 F7 180.0(7) . . . . ? F6 C8 C9 C10 -179.9(7) . . . . ? C7 C8 C9 C10 -1.2(12) . . . . ? O3 C13 C18 F15 -2.0(11) . . . . ? C14 C13 C18 F15 178.8(7) . . . . ? O3 C13 C18 C17 179.1(7) . . . . ? C14 C13 C18 C17 -0.1(11) . . . . ? O5 C25 C26 F21 0.1(12) . . . . ? C30 C25 C26 F21 178.8(7) . . . . ? O5 C25 C26 C27 -179.6(8) . . . . ? C30 C25 C26 C27 -0.8(13) . . . . ? O3 C13 C14 F11 1.7(11) . . . . ? C18 C13 C14 F11 -179.1(6) . . . . ? O3 C13 C14 C15 -178.6(7) . . . . ? C18 C13 C14 C15 0.5(11) . . . . ? O1 C1 C6 F5 0.9(12) . . . . ? C2 C1 C6 F5 -177.9(7) . . . . ? O1 C1 C6 C5 179.7(8) . . . . ? C2 C1 C6 C5 0.9(12) . . . . ? F5 C6 C5 C4 178.2(8) . . . . ? C1 C6 C5 C4 -0.6(14) . . . . ? F5 C6 C5 F4 -1.5(13) . . . . ? C1 C6 C5 F4 179.7(7) . . . . ? F23 C28 C27 F22 -2.4(14) . . . . ? C29 C28 C27 F22 178.8(9) . . . . ? F23 C28 C27 C26 178.2(8) . . . . ? C29 C28 C27 C26 -0.7(14) . . . . ? F21 C26 C27 F22 1.4(12) . . . . ? C25 C26 C27 F22 -179.0(8) . . . . ? F21 C26 C27 C28 -179.1(8) . . . . ? C25 C26 C27 C28 0.5(14) . . . . ? F11 C14 C15 F12 -1.6(12) . . . . ? C13 C14 C15 F12 178.7(7) . . . . ? F11 C14 C15 C16 178.8(8) . . . . ? C13 C14 C15 C16 -0.9(13) . . . . ? O4 C19 C24 F20 5.7(14) . . . . ? C20 C19 C24 F20 -179.2(9) . . . . ? O4 C19 C24 C23 -178.8(9) . . . . ? C20 C19 C24 C23 -3.7(16) . . . . ? F4 C5 C4 F3 -2.8(14) . . . . ? C6 C5 C4 F3 177.5(8) . . . . ? F4 C5 C4 C3 -179.7(8) . . . . ? C6 C5 C4 C3 0.6(14) . . . . ? F25 C30 C29 F24 3.3(14) . . . . ? C25 C30 C29 F24 -179.4(8) . . . . ? F25 C30 C29 C28 -178.9(9) . . . . ? C25 C30 C29 C28 -1.5(15) . . . . ? F23 C28 C29 F24 0.3(15) . . . . ? C27 C28 C29 F24 179.0(8) . . . . ? F23 C28 C29 C30 -177.6(9) . . . . ? C27 C28 C29 C30 1.2(15) . . . . ? F3 C4 C3 F2 2.1(14) . . . . ? C5 C4 C3 F2 179.0(8) . . . . ? F3 C4 C3 C2 -177.7(9) . . . . ? C5 C4 C3 C2 -0.8(15) . . . . ? F1 C2 C3 F2 2.2(14) . . . . ? C1 C2 C3 F2 -178.7(8) . . . . ? F1 C2 C3 C4 -178.0(8) . . . . ? C1 C2 C3 C4 1.1(15) . . . . ? F15 C18 C17 F14 0.2(12) . . . . ? C13 C18 C17 F14 179.1(7) . . . . ? F15 C18 C17 C16 -179.0(8) . . . . ? C13 C18 C17 C16 -0.1(13) . . . . ? F12 C15 C16 F13 -0.9(14) . . . . ? C14 C15 C16 F13 178.7(8) . . . . ? F12 C15 C16 C17 -178.8(8) . . . . ? C14 C15 C16 C17 0.7(15) . . . . ? F14 C17 C16 F13 2.6(14) . . . . ? C18 C17 C16 F13 -178.2(8) . . . . ? F14 C17 C16 C15 -179.4(8) . . . . ? C18 C17 C16 C15 -0.2(15) . . . . ? C19 C24 C23 F19 -178.0(10) . . . . ? F20 C24 C23 F19 -2.6(17) . . . . ? C19 C24 C23 C22 2.3(18) . . . . ? F20 C24 C23 C22 177.7(12) . . . . ? O4 C19 C20 F16 -2.9(14) . . . . ? C24 C19 C20 F16 -177.9(9) . . . . ? O4 C19 C20 C21 178.4(9) . . . . ? C24 C19 C20 C21 3.4(16) . . . . ? Li1 O8 C37 C38 75.4(11) . . . . ? Li1 O8 C37 C39 -163.1(9) . . . . ? Li1 O8 C37 C40 -43.3(12) . . . . ? Li1 O7 C41 C44 107.1(14) . . . . ? Li1 O7 C41 C43 -131.7(10) . . . . ? Li1 O7 C41 C42 -17.7(14) . . . . ? F16 C20 C21 C22 179.6(12) . . . . ? C19 C20 C21 C22 -1.6(19) . . . . ? F16 C20 C21 F17 0.3(17) . . . . ? C19 C20 C21 F17 179.1(10) . . . . ? F17 C21 C22 F18 3(2) . . . . ? C20 C21 C22 F18 -176.8(12) . . . . ? F17 C21 C22 C23 179.4(12) . . . . ? C20 C21 C22 C23 0(2) . . . . ? F19 C23 C22 C21 179.8(13) . . . . ? C24 C23 C22 C21 0(2) . . . . ? F19 C23 C22 F18 -3(2) . . . . ? C24 C23 C22 F18 176.7(11) . . . . ? C41 O7 Li1 O8 -14.6(16) . . . . ? C41 O7 Li1 O1 144.6(9) . . . . ? C41 O7 Li1 O2 -129.6(9) . . . . ? C41 O7 Li1 U1 -171.5(8) . . . . ? C37 O8 Li1 O7 128.1(10) . . . . ? C37 O8 Li1 O1 -28.1(13) . . . . ? C37 O8 Li1 O2 -117.8(8) . . . . ? C37 O8 Li1 U1 -78.0(10) . . . . ? C1 O1 Li1 O7 -68.0(10) . . . . ? U1 O1 Li1 O7 96.9(6) . . . . ? C1 O1 Li1 O8 92.6(10) . . . . ? U1 O1 Li1 O8 -102.5(8) . . . . ? C1 O1 Li1 O2 -167.0(6) . . . . ? U1 O1 Li1 O2 -2.1(4) . . . . ? C1 O1 Li1 U1 -164.9(7) . . . . ? C7 O2 Li1 O7 70.5(8) . . . . ? U1 O2 Li1 O7 -103.3(6) . . . . ? C7 O2 Li1 O8 -62.2(8) . . . . ? U1 O2 Li1 O8 124.0(5) . . . . ? C7 O2 Li1 O1 175.9(5) . . . . ? U1 O2 Li1 O1 2.1(4) . . . . ? C7 O2 Li1 U1 173.8(6) . . . . ? O4 U1 Li1 O7 -94.9(6) . . . . ? O3 U1 Li1 O7 81.0(7) . . . . ? O6 U1 Li1 O7 -6.2(6) . . . . ? O5 U1 Li1 O7 173.5(6) . . . . ? O2 U1 Li1 O7 87.0(6) . . . . ? O1 U1 Li1 O7 -96.1(7) . . . . ? O4 U1 Li1 O8 106.5(7) . . . . ? O3 U1 Li1 O8 -77.7(7) . . . . ? O6 U1 Li1 O8 -164.8(7) . . . . ? O5 U1 Li1 O8 14.8(7) . . . . ? O2 U1 Li1 O8 -71.6(7) . . . . ? O1 U1 Li1 O8 105.2(8) . . . . ? O4 U1 Li1 O1 1.2(5) . . . . ? O3 U1 Li1 O1 177.1(3) . . . . ? O6 U1 Li1 O1 90.0(4) . . . . ? O5 U1 Li1 O1 -90.4(4) . . . . ? O2 U1 Li1 O1 -176.9(6) . . . . ? O4 U1 Li1 O2 178.1(3) . . . . ? O3 U1 Li1 O2 -6.0(5) . . . . ? O6 U1 Li1 O2 -93.2(3) . . . . ? O5 U1 Li1 O2 86.4(3) . . . . ? O1 U1 Li1 O2 176.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.596 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.157 #===END=== _publ_contact_author_name 'Trevor W. Hayton' _publ_contact_author_email 'hayton@chem.ucsb.edu' loop_ _publ_author_name 'Skye Fortier' 'Guang Wu' 'Trevor W. Hayton' _journal_full_name 'Journal of the American Chemical Society' data_Complex_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Uranyl bis(pentafluorophenoxide) bis(tert-butanol) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 F10 O6 U' _chemical_formula_weight 784.39 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.6651(13) _cell_length_b 19.3272(19) _cell_length_c 11.1318(11) _cell_angle_alpha 90.00 _cell_angle_beta 112.922(3) _cell_angle_gamma 90.00 _cell_volume 2509.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 6.575 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.360 _exptl_absorpt_correction_T_max 0.520 _exptl_absorpt_process_details 'Psi Scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9661 _diffrn_reflns_av_R_equivalents 0.1030 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.72 _reflns_number_total 2602 _reflns_number_gt 1573 _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^)+(0.0776P)^2^+6.6975P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2602 _refine_ls_number_parameters 167 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.071 _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 U1 U 1.0000 0.0000 1.0000 0.02571(19) Uani 1 2 d S . . O3 O 0.8528(7) 0.0332(4) 1.0737(7) 0.0368(17) Uani 1 1 d . . . F3 F 1.1292(7) 0.3628(4) 0.8607(8) 0.078(3) Uani 1 1 d . . . F5 F 1.1473(7) 0.1220(4) 0.8356(7) 0.065(2) Uani 1 1 d . . . F1 F 1.0175(8) 0.2230(4) 1.1353(8) 0.067(2) Uani 1 1 d . . . F4 F 1.1793(7) 0.2479(4) 0.7549(6) 0.066(2) Uani 1 1 d . . . O2 O 1.0640(8) 0.1061(4) 1.0269(7) 0.046(2) Uani 1 1 d . . . C2 C 1.0549(11) 0.2279(6) 1.0391(12) 0.042(3) Uani 1 1 d . . . F2 F 1.0519(8) 0.3496(4) 1.0551(10) 0.081(2) Uani 1 1 d . . . C5 C 1.1386(10) 0.2422(6) 0.8485(10) 0.041(3) Uani 1 1 d . . . C1 C 1.0786(9) 0.1686(5) 0.9849(10) 0.035(2) Uani 1 1 d . . . C6 C 1.1209(10) 0.1784(6) 0.8897(10) 0.040(3) Uani 1 1 d . . . C4 C 1.1121(11) 0.2996(6) 0.9030(12) 0.050(3) Uani 1 1 d . . . C7 C 0.7520(10) 0.0698(6) 1.0284(10) 0.047(3) Uani 1 1 d D . . C3 C 1.0729(12) 0.2932(6) 0.9998(14) 0.055(3) Uani 1 1 d . . . O1 O 1.0843(6) -0.0146(3) 1.1672(6) 0.0312(18) Uani 1 1 d . . . C8A C 0.764(2) 0.1462(8) 1.033(3) 0.104(6) Uani 0.50 1 d PD . . C9A C 0.736(2) 0.1170(13) 0.916(2) 0.104(6) Uani 0.50 1 d PD . . C10A C 0.6441(17) 0.0299(13) 0.981(3) 0.104(6) Uani 0.50 1 d PD . . C8B C 0.674(2) 0.0596(15) 1.098(2) 0.104(6) Uani 0.50 1 d PD . . C9B C 0.674(2) 0.0595(15) 0.8897(15) 0.104(6) Uani 0.50 1 d PD . . C10B C 0.736(2) 0.1180(13) 1.125(2) 0.104(6) Uani 0.50 1 d PD . . 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 U1 0.0305(3) 0.0228(3) 0.0242(3) 0.0018(2) 0.01114(19) 0.0018(3) O3 0.040(5) 0.035(4) 0.038(4) 0.006(3) 0.018(4) 0.012(4) F3 0.066(6) 0.044(4) 0.109(6) 0.030(4) 0.017(5) -0.007(4) F5 0.086(7) 0.057(5) 0.061(5) -0.026(4) 0.039(5) -0.024(4) F1 0.078(6) 0.053(5) 0.091(6) -0.009(4) 0.056(5) -0.002(4) F4 0.073(6) 0.080(6) 0.049(4) 0.005(4) 0.026(4) -0.028(5) O2 0.052(6) 0.034(5) 0.058(5) -0.004(4) 0.028(4) -0.006(4) C2 0.031(7) 0.033(7) 0.063(7) 0.004(6) 0.022(6) 0.002(5) F2 0.070(6) 0.040(5) 0.138(7) -0.013(5) 0.044(6) 0.003(4) C5 0.041(7) 0.043(7) 0.030(5) 0.002(5) 0.003(5) -0.009(5) C1 0.030(6) 0.028(6) 0.039(6) 0.004(5) 0.005(5) -0.006(5) C6 0.044(7) 0.033(6) 0.033(6) -0.010(5) 0.005(5) -0.010(5) C4 0.036(7) 0.035(7) 0.058(8) 0.019(6) -0.005(6) -0.010(5) C7 0.052(8) 0.037(7) 0.047(7) 0.000(6) 0.014(6) 0.004(6) C3 0.042(8) 0.031(7) 0.082(9) -0.004(6) 0.011(7) 0.009(6) O1 0.023(4) 0.048(5) 0.018(3) 0.006(3) 0.003(3) 0.011(3) C8A 0.095(14) 0.096(13) 0.098(12) -0.001(10) 0.014(11) 0.045(11) C9A 0.095(14) 0.096(13) 0.098(12) -0.001(10) 0.014(11) 0.045(11) C10A 0.095(14) 0.096(13) 0.098(12) -0.001(10) 0.014(11) 0.045(11) C8B 0.095(14) 0.096(13) 0.098(12) -0.001(10) 0.014(11) 0.045(11) C9B 0.095(14) 0.096(13) 0.098(12) -0.001(10) 0.014(11) 0.045(11) C10B 0.095(14) 0.096(13) 0.098(12) -0.001(10) 0.014(11) 0.045(11) _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 U1 O1 1.771(6) . ? U1 O1 1.771(6) 5_757 ? U1 O2 2.183(8) . ? U1 O2 2.183(8) 5_757 ? U1 O3 2.399(7) . ? U1 O3 2.399(7) 5_757 ? O3 C7 1.372(12) . ? F3 C4 1.358(13) . ? F5 C6 1.350(12) . ? F1 C2 1.332(12) . ? F4 C5 1.335(12) . ? O2 C1 1.333(12) . ? C2 C1 1.382(15) . ? C2 C3 1.384(17) . ? F2 C3 1.328(14) . ? C5 C6 1.365(15) . ? C5 C4 1.367(17) . ? C1 C6 1.374(15) . ? C4 C3 1.358(17) . ? C7 C10A 1.478(10) . ? C7 C8B 1.483(10) . ? C7 C8A 1.484(10) . ? C7 C9B 1.488(10) . ? C7 C10B 1.494(10) . ? C7 C9A 1.498(10) . ? C8A C10B 1.329(10) . ? C8A C9A 1.334(10) . ? C9A C9B 1.329(10) . ? C10A C8B 1.334(10) . ? C10A C9B 1.340(10) . ? C8B C10B 1.337(10) . ? 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 O1 U1 O1 180.000(1) . 5_757 ? O1 U1 O2 88.0(3) . . ? O1 U1 O2 92.0(3) 5_757 . ? O1 U1 O2 92.0(3) . 5_757 ? O1 U1 O2 88.0(3) 5_757 5_757 ? O2 U1 O2 180.000(1) . 5_757 ? O1 U1 O3 85.1(3) . . ? O1 U1 O3 94.9(3) 5_757 . ? O2 U1 O3 89.9(3) . . ? O2 U1 O3 90.1(3) 5_757 . ? O1 U1 O3 94.9(3) . 5_757 ? O1 U1 O3 85.1(3) 5_757 5_757 ? O2 U1 O3 90.1(3) . 5_757 ? O2 U1 O3 89.9(3) 5_757 5_757 ? O3 U1 O3 180.000(1) . 5_757 ? C7 O3 U1 138.4(7) . . ? C1 O2 U1 153.8(7) . . ? F1 C2 C1 119.9(10) . . ? F1 C2 C3 118.2(11) . . ? C1 C2 C3 121.9(11) . . ? F4 C5 C6 120.1(11) . . ? F4 C5 C4 121.0(11) . . ? C6 C5 C4 118.9(11) . . ? O2 C1 C6 123.0(10) . . ? O2 C1 C2 121.0(10) . . ? C6 C1 C2 116.0(10) . . ? F5 C6 C5 118.6(10) . . ? F5 C6 C1 118.2(10) . . ? C5 C6 C1 123.3(11) . . ? C3 C4 F3 121.0(13) . . ? C3 C4 C5 120.5(11) . . ? F3 C4 C5 118.5(12) . . ? O3 C7 C10A 117.4(14) . . ? O3 C7 C8B 116.8(13) . . ? C10A C7 C8B 53.6(5) . . ? O3 C7 C8A 115.5(13) . . ? C10A C7 C8A 127.1(13) . . ? C8B C7 C8A 101.4(9) . . ? O3 C7 C9B 117.5(13) . . ? C10A C7 C9B 53.7(5) . . ? C8B C7 C9B 102.2(10) . . ? C8A C7 C9B 100.8(8) . . ? O3 C7 C10B 115.3(13) . . ? C10A C7 C10B 102.4(9) . . ? C8B C7 C10B 53.4(5) . . ? C8A C7 C10B 53.0(5) . . ? C9B C7 C10B 127.2(14) . . ? O3 C7 C9A 115.2(13) . . ? C10A C7 C9A 102.4(10) . . ? C8B C7 C9A 128.0(11) . . ? C8A C7 C9A 53.2(5) . . ? C9B C7 C9A 52.9(5) . . ? C10B C7 C9A 102.1(8) . . ? F2 C3 C4 119.6(13) . . ? F2 C3 C2 121.0(13) . . ? C4 C3 C2 119.3(12) . . ? C10B C8A C9A 121.8(12) . . ? C10B C8A C7 63.9(6) . . ? C9A C8A C7 64.0(6) . . ? C9B C9A C8A 118.6(12) . . ? C9B C9A C7 63.2(6) . . ? C8A C9A C7 62.9(6) . . ? C8B C10A C9B 119.7(13) . . ? C8B C10A C7 63.4(6) . . ? C9B C10A C7 63.5(6) . . ? C10A C8B C10B 120.2(12) . . ? C10A C8B C7 63.0(6) . . ? C10B C8B C7 63.7(6) . . ? C9A C9B C10A 120.6(13) . . ? C9A C9B C7 63.9(6) . . ? C10A C9B C7 62.7(6) . . ? C8A C10B C8B 118.9(13) . . ? C8A C10B C7 63.1(6) . . ? C8B C10B C7 62.9(6) . . ? 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 O1 U1 O3 C7 161.3(11) . . . . ? O1 U1 O3 C7 -18.7(11) 5_757 . . . ? O2 U1 O3 C7 73.3(11) . . . . ? O2 U1 O3 C7 -106.7(11) 5_757 . . . ? O3 U1 O3 C7 -125(100) 5_757 . . . ? O1 U1 O2 C1 170.4(18) . . . . ? O1 U1 O2 C1 -9.6(18) 5_757 . . . ? O2 U1 O2 C1 -178(100) 5_757 . . . ? O3 U1 O2 C1 -104.6(18) . . . . ? O3 U1 O2 C1 75.4(18) 5_757 . . . ? U1 O2 C1 C6 -52(2) . . . . ? U1 O2 C1 C2 130.4(15) . . . . ? F1 C2 C1 O2 0.4(18) . . . . ? C3 C2 C1 O2 177.9(12) . . . . ? F1 C2 C1 C6 -177.6(11) . . . . ? C3 C2 C1 C6 -0.1(18) . . . . ? F4 C5 C6 F5 1.2(16) . . . . ? C4 C5 C6 F5 -179.9(11) . . . . ? F4 C5 C6 C1 -179.6(10) . . . . ? C4 C5 C6 C1 -0.7(17) . . . . ? O2 C1 C6 F5 0.9(17) . . . . ? C2 C1 C6 F5 178.8(11) . . . . ? O2 C1 C6 C5 -178.4(11) . . . . ? C2 C1 C6 C5 -0.5(17) . . . . ? F4 C5 C4 C3 -178.7(11) . . . . ? C6 C5 C4 C3 2.4(17) . . . . ? F4 C5 C4 F3 -0.6(16) . . . . ? C6 C5 C4 F3 -179.5(11) . . . . ? U1 O3 C7 C10A 102.6(16) . . . . ? U1 O3 C7 C8B 163.4(14) . . . . ? U1 O3 C7 C8A -77.4(16) . . . . ? U1 O3 C7 C9B 41.4(19) . . . . ? U1 O3 C7 C10B -136.7(14) . . . . ? U1 O3 C7 C9A -18.1(18) . . . . ? F3 C4 C3 F2 -0.7(19) . . . . ? C5 C4 C3 F2 177.4(12) . . . . ? F3 C4 C3 C2 179.0(12) . . . . ? C5 C4 C3 C2 -2.9(19) . . . . ? F1 C2 C3 F2 -1(2) . . . . ? C1 C2 C3 F2 -178.5(12) . . . . ? F1 C2 C3 C4 179.3(12) . . . . ? C1 C2 C3 C4 2(2) . . . . ? O3 C7 C8A C10B -103.5(16) . . . . ? C10A C7 C8A C10B 76.5(14) . . . . ? C8B C7 C8A C10B 23.9(15) . . . . ? C9B C7 C8A C10B 128.9(15) . . . . ? C9A C7 C8A C10B 153.2(15) . . . . ? O3 C7 C8A C9A 103.4(14) . . . . ? C10A C7 C8A C9A -76.6(11) . . . . ? C8B C7 C8A C9A -129.3(10) . . . . ? C9B C7 C8A C9A -24.3(11) . . . . ? C10B C7 C8A C9A -153.2(15) . . . . ? C10B C8A C9A C9B 3(2) . . . . ? C7 C8A C9A C9B 31.1(13) . . . . ? C10B C8A C9A C7 -28.5(14) . . . . ? O3 C7 C9A C9B 106.5(17) . . . . ? C10A C7 C9A C9B -22.1(16) . . . . ? C8B C7 C9A C9B -75.2(14) . . . . ? C8A C7 C9A C9B -149.5(15) . . . . ? C10B C7 C9A C9B -127.9(15) . . . . ? O3 C7 C9A C8A -104.0(14) . . . . ? C10A C7 C9A C8A 127.4(12) . . . . ? C8B C7 C9A C8A 74.3(11) . . . . ? C9B C7 C9A C8A 149.5(15) . . . . ? C10B C7 C9A C8A 21.6(12) . . . . ? O3 C7 C10A C8B 104.5(16) . . . . ? C8A C7 C10A C8B -75.5(13) . . . . ? C9B C7 C10A C8B -150(2) . . . . ? C10B C7 C10A C8B -22.8(15) . . . . ? C9A C7 C10A C8B -128.4(12) . . . . ? O3 C7 C10A C9B -105.3(18) . . . . ? C8B C7 C10A C9B 150(2) . . . . ? C8A C7 C10A C9B 74.7(15) . . . . ? C10B C7 C10A C9B 127.4(16) . . . . ? C9A C7 C10A C9B 21.8(16) . . . . ? C9B C10A C8B C10B -1(3) . . . . ? C7 C10A C8B C10B 29.3(17) . . . . ? C9B C10A C8B C7 -30.8(19) . . . . ? O3 C7 C8B C10A -105.5(17) . . . . ? C8A C7 C8B C10A 128.1(14) . . . . ? C9B C7 C8B C10A 24.2(16) . . . . ? C10B C7 C8B C10A 151.8(19) . . . . ? C9A C7 C8B C10A 76.3(14) . . . . ? O3 C7 C8B C10B 102.7(17) . . . . ? C10A C7 C8B C10B -151.8(19) . . . . ? C8A C7 C8B C10B -23.8(15) . . . . ? C9B C7 C8B C10B -127.6(14) . . . . ? C9A C7 C8B C10B -75.6(14) . . . . ? C8A C9A C9B C10A -3(3) . . . . ? C7 C9A C9B C10A 28.1(19) . . . . ? C8A C9A C9B C7 -31.0(13) . . . . ? C8B C10A C9B C9A 2(4) . . . . ? C7 C10A C9B C9A -28(2) . . . . ? C8B C10A C9B C7 30.8(19) . . . . ? O3 C7 C9B C9A -102.0(16) . . . . ? C10A C7 C9B C9A 153(2) . . . . ? C8B C7 C9B C9A 128.7(12) . . . . ? C8A C7 C9B C9A 24.4(11) . . . . ? C10B C7 C9B C9A 75.8(13) . . . . ? O3 C7 C9B C10A 105.1(18) . . . . ? C8B C7 C9B C10A -24.1(16) . . . . ? C8A C7 C9B C10A -128.5(15) . . . . ? C10B C7 C9B C10A -77.1(15) . . . . ? C9A C7 C9B C10A -153(2) . . . . ? C9A C8A C10B C8B -2(3) . . . . ? C7 C8A C10B C8B -30.2(17) . . . . ? C9A C8A C10B C7 28.5(14) . . . . ? C10A C8B C10B C8A 1(3) . . . . ? C7 C8B C10B C8A 30.3(17) . . . . ? C10A C8B C10B C7 -29.1(17) . . . . ? O3 C7 C10B C8A 103.9(17) . . . . ? C10A C7 C10B C8A -127.5(14) . . . . ? C8B C7 C10B C8A -150.3(19) . . . . ? C9B C7 C10B C8A -73.9(13) . . . . ? C9A C7 C10B C8A -21.7(12) . . . . ? O3 C7 C10B C8B -105.8(17) . . . . ? C10A C7 C10B C8B 22.9(15) . . . . ? C8A C7 C10B C8B 150.3(19) . . . . ? C9B C7 C10B C8B 76.4(14) . . . . ? C9A C7 C10B C8B 128.7(13) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.72 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 3.426 _refine_diff_density_min -1.285 _refine_diff_density_rms 0.256 #===END=== _publ_contact_author_name 'Trevor W. Hayton' _publ_contact_author_email 'hayton@chem.ucsb.edu' loop_ _publ_author_name 'Skye Fortier' 'Guang Wu' 'Trevor W. Hayton' _journal_full_name 'Journal of the American Chemical Society' data_Complex_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Uranium(VI) bis(tert-butoxide) tetrakis(pentafluorophenoxide) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H18 F20 O6 U' _chemical_formula_weight 1116.49 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 '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 10.147(5) _cell_length_b 10.565(5) _cell_length_c 10.637(5) _cell_angle_alpha 68.547(7) _cell_angle_beta 63.240(7) _cell_angle_gamma 62.611(6) _cell_volume 885.8(8) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description kite _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 530 _exptl_absorpt_coefficient_mu 4.731 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.466 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details 'Psi Scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5948 _diffrn_reflns_av_R_equivalents 0.0989 _diffrn_reflns_av_sigmaI/netI 0.1108 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3319 _reflns_number_gt 2775 _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^)+(0.0757P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3319 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.006 _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 F8 F 1.0282(8) 0.8450(8) 0.4374(8) 0.079(2) Uani 1 1 d . . . F7 F 0.9576(9) 0.8582(8) 0.2121(8) 0.079(2) Uani 1 1 d . . . C10 C 0.9468(13) 0.7652(12) 0.4551(13) 0.055(3) Uani 1 1 d . . . C9 C 0.9076(13) 0.7757(12) 0.3405(12) 0.056(3) Uani 1 1 d . . . U1 U 0.5000 0.5000 0.5000 0.0428(2) Uani 1 2 d S . . F1 F 0.6943(7) 0.2610(6) 0.8090(7) 0.0587(16) Uani 1 1 d . . . F5 F 0.5112(8) 0.0522(7) 0.6277(7) 0.0595(16) Uani 1 1 d . . . F2 F 0.7757(8) 0.0081(7) 0.9948(7) 0.0644(17) Uani 1 1 d . . . O2 O 0.6812(9) 0.5340(7) 0.5117(8) 0.0508(17) Uani 1 1 d . . . O1 O 0.5677(9) 0.2865(7) 0.6187(8) 0.0548(18) Uani 1 1 d . . . O3 O 0.3411(11) 0.5781(9) 0.6954(8) 0.073(3) Uani 1 1 d . . . C2 C 0.6715(12) 0.1451(11) 0.8086(11) 0.046(2) Uani 1 1 d . . . C1 C 0.6023(11) 0.1649(11) 0.7106(10) 0.042(2) Uani 1 1 d . . . C6 C 0.5777(13) 0.0409(11) 0.7183(11) 0.050(3) Uani 1 1 d . . . C3 C 0.7106(11) 0.0189(11) 0.9034(11) 0.046(2) Uani 1 1 d . . . C13 C 0.2685(14) 0.6609(13) 0.8071(12) 0.058(3) Uani 1 1 d . . . F10 F 0.7683(7) 0.5150(7) 0.7300(6) 0.0531(14) Uani 1 1 d . . . F4 F 0.5860(8) -0.1990(6) 0.8196(7) 0.0607(16) Uani 1 1 d . . . F9 F 0.9387(7) 0.6665(8) 0.6935(7) 0.0657(18) Uani 1 1 d . . . F3 F 0.7235(8) -0.2245(7) 0.9980(7) 0.0667(17) Uani 1 1 d . . . F6 F 0.7904(8) 0.7022(8) 0.2477(7) 0.0678(18) Uani 1 1 d . . . C7 C 0.7708(11) 0.6099(10) 0.4887(10) 0.039(2) Uani 1 1 d . . . C12 C 0.8118(11) 0.6003(10) 0.6015(10) 0.042(2) Uani 1 1 d . . . C8 C 0.8230(12) 0.6953(11) 0.3599(11) 0.046(2) Uani 1 1 d . . . C4 C 0.6845(12) -0.0986(11) 0.9049(11) 0.048(2) Uani 1 1 d . . . C11 C 0.8995(12) 0.6792(12) 0.5827(12) 0.049(3) Uani 1 1 d . . . C5 C 0.6169(12) -0.0852(10) 0.8125(11) 0.047(2) Uani 1 1 d . . . C15 C 0.365(2) 0.586(2) 0.9029(18) 0.111(6) Uani 1 1 d . . . H15A H 0.4712 0.5846 0.8483 0.167 Uiso 1 1 calc R . . H15B H 0.3666 0.4884 0.9430 0.167 Uiso 1 1 calc R . . H15C H 0.3202 0.6378 0.9790 0.167 Uiso 1 1 calc R . . C14 C 0.277(5) 0.800(2) 0.727(2) 0.225(18) Uani 1 1 d . . . H14A H 0.3827 0.7882 0.6613 0.338 Uiso 1 1 calc R . . H14B H 0.2495 0.8587 0.7921 0.338 Uiso 1 1 calc R . . H14C H 0.2050 0.8457 0.6752 0.338 Uiso 1 1 calc R . . C16 C 0.115(2) 0.649(5) 0.897(3) 0.26(2) Uani 1 1 d . . . H16A H 0.0894 0.6614 0.9919 0.388 Uiso 1 1 calc R . . H16B H 0.1181 0.5552 0.9033 0.388 Uiso 1 1 calc R . . H16C H 0.0368 0.7233 0.8568 0.388 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 F8 0.066(5) 0.092(5) 0.096(5) -0.037(4) -0.009(4) -0.046(4) F7 0.078(5) 0.078(5) 0.073(5) 0.001(4) -0.020(4) -0.039(4) C10 0.043(6) 0.057(6) 0.071(8) -0.028(6) -0.009(6) -0.022(5) C9 0.050(7) 0.058(7) 0.047(6) -0.008(5) -0.004(5) -0.022(6) U1 0.0490(4) 0.0381(3) 0.0465(4) -0.0104(2) -0.0223(3) -0.0123(2) F1 0.064(4) 0.056(4) 0.069(4) -0.022(3) -0.026(3) -0.021(3) F5 0.069(4) 0.063(4) 0.064(4) -0.018(3) -0.033(3) -0.023(3) F2 0.067(4) 0.077(4) 0.054(4) -0.011(3) -0.032(3) -0.019(4) O2 0.062(5) 0.052(4) 0.058(4) -0.015(3) -0.030(4) -0.023(4) O1 0.072(5) 0.045(4) 0.057(5) -0.004(4) -0.036(4) -0.020(4) O3 0.113(7) 0.062(5) 0.052(5) -0.025(4) -0.037(5) -0.018(5) C2 0.043(6) 0.043(5) 0.055(6) -0.022(5) -0.012(5) -0.012(5) C1 0.038(5) 0.048(6) 0.037(5) -0.013(5) -0.010(4) -0.013(5) C6 0.058(7) 0.052(6) 0.045(6) -0.015(5) -0.018(5) -0.019(5) C3 0.035(5) 0.052(6) 0.044(6) -0.017(5) -0.014(5) -0.004(5) C13 0.064(8) 0.065(7) 0.047(6) -0.031(6) -0.015(6) -0.014(6) F10 0.052(4) 0.065(4) 0.046(3) -0.016(3) -0.016(3) -0.022(3) F4 0.068(4) 0.049(3) 0.069(4) -0.019(3) -0.014(3) -0.026(3) F9 0.049(4) 0.099(5) 0.071(4) -0.046(4) -0.018(3) -0.024(3) F3 0.073(5) 0.050(4) 0.057(4) 0.004(3) -0.022(3) -0.017(3) F6 0.075(5) 0.087(5) 0.049(4) -0.005(3) -0.033(3) -0.030(4) C7 0.034(5) 0.043(5) 0.038(5) -0.016(4) -0.007(4) -0.010(4) C12 0.036(5) 0.046(5) 0.041(6) -0.019(5) -0.008(4) -0.009(4) C8 0.038(6) 0.052(6) 0.049(6) -0.014(5) -0.016(5) -0.012(5) C4 0.041(6) 0.050(6) 0.038(6) -0.009(5) -0.011(5) -0.005(5) C11 0.040(6) 0.062(7) 0.055(7) -0.035(6) -0.011(5) -0.012(5) C5 0.043(6) 0.037(5) 0.045(6) -0.016(5) 0.000(5) -0.009(5) C15 0.099(12) 0.171(18) 0.091(11) -0.070(12) -0.033(10) -0.036(12) C14 0.46(5) 0.085(14) 0.110(17) -0.032(13) -0.09(3) -0.08(2) C16 0.069(14) 0.60(7) 0.15(2) -0.17(4) 0.015(14) -0.14(3) _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 F8 C10 1.346(12) . ? F7 C9 1.339(13) . ? C10 C11 1.345(16) . ? C10 C9 1.398(16) . ? C9 C8 1.373(15) . ? U1 O2 2.091(6) . ? U1 O2 2.091(6) 2_666 ? U1 O1 2.104(7) 2_666 ? U1 O1 2.104(7) . ? U1 O3 2.148(7) 2_666 ? U1 O3 2.148(7) . ? F1 C2 1.348(11) . ? F5 C6 1.352(11) . ? F2 C3 1.350(10) . ? O2 C7 1.363(11) . ? O1 C1 1.306(12) . ? O3 C13 1.448(11) . ? C2 C3 1.357(15) . ? C2 C1 1.410(13) . ? C1 C6 1.410(14) . ? C6 C5 1.354(15) . ? C3 C4 1.376(15) . ? C13 C14 1.42(2) . ? C13 C16 1.45(2) . ? C13 C15 1.492(18) . ? F10 C12 1.340(12) . ? F4 C5 1.345(11) . ? F9 C11 1.350(11) . ? F3 C4 1.346(12) . ? F6 C8 1.344(11) . ? C7 C8 1.362(14) . ? C7 C12 1.394(12) . ? C12 C11 1.388(14) . ? C4 C5 1.368(14) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 C11 C10 F8 120.6(10) . . ? C11 C10 C9 120.1(9) . . ? F8 C10 C9 119.3(11) . . ? F7 C9 C8 120.6(10) . . ? F7 C9 C10 120.4(10) . . ? C8 C9 C10 118.9(10) . . ? O2 U1 O2 180.0 . 2_666 ? O2 U1 O1 89.5(3) . 2_666 ? O2 U1 O1 90.5(3) 2_666 2_666 ? O2 U1 O1 90.5(3) . . ? O2 U1 O1 89.5(3) 2_666 . ? O1 U1 O1 180.000(1) 2_666 . ? O2 U1 O3 89.6(3) . 2_666 ? O2 U1 O3 90.4(3) 2_666 2_666 ? O1 U1 O3 90.2(3) 2_666 2_666 ? O1 U1 O3 89.8(3) . 2_666 ? O2 U1 O3 90.4(3) . . ? O2 U1 O3 89.6(3) 2_666 . ? O1 U1 O3 89.8(3) 2_666 . ? O1 U1 O3 90.2(3) . . ? O3 U1 O3 180.000(1) 2_666 . ? C7 O2 U1 156.4(6) . . ? C1 O1 U1 170.1(6) . . ? C13 O3 U1 159.9(8) . . ? F1 C2 C3 119.4(8) . . ? F1 C2 C1 116.9(9) . . ? C3 C2 C1 123.6(9) . . ? O1 C1 C6 123.3(8) . . ? O1 C1 C2 122.6(8) . . ? C6 C1 C2 114.1(9) . . ? F5 C6 C5 120.3(9) . . ? F5 C6 C1 117.3(9) . . ? C5 C6 C1 122.5(9) . . ? F2 C3 C2 120.4(9) . . ? F2 C3 C4 120.2(9) . . ? C2 C3 C4 119.4(9) . . ? C14 C13 O3 102.5(11) . . ? C14 C13 C16 119(3) . . ? O3 C13 C16 109.5(15) . . ? C14 C13 C15 113.5(19) . . ? O3 C13 C15 106.9(10) . . ? C16 C13 C15 104.9(15) . . ? C8 C7 O2 123.0(8) . . ? C8 C7 C12 118.0(9) . . ? O2 C7 C12 119.0(9) . . ? F10 C12 C11 118.4(8) . . ? F10 C12 C7 121.1(8) . . ? C11 C12 C7 120.4(10) . . ? F6 C8 C7 119.3(9) . . ? F6 C8 C9 118.6(10) . . ? C7 C8 C9 122.1(9) . . ? F3 C4 C5 120.6(9) . . ? F3 C4 C3 120.0(9) . . ? C5 C4 C3 119.4(9) . . ? C10 C11 F9 120.6(9) . . ? C10 C11 C12 120.4(9) . . ? F9 C11 C12 119.0(10) . . ? F4 C5 C6 120.3(9) . . ? F4 C5 C4 118.7(9) . . ? C6 C5 C4 121.0(9) . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 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 C11 C10 C9 F7 -178.3(10) . . . . ? F8 C10 C9 F7 3.6(16) . . . . ? C11 C10 C9 C8 -1.1(16) . . . . ? F8 C10 C9 C8 -179.3(9) . . . . ? O2 U1 O2 C7 -48(100) 2_666 . . . ? O1 U1 O2 C7 0.9(15) 2_666 . . . ? O1 U1 O2 C7 -179.1(15) . . . . ? O3 U1 O2 C7 91.1(15) 2_666 . . . ? O3 U1 O2 C7 -88.9(15) . . . . ? O2 U1 O1 C1 65(4) . . . . ? O2 U1 O1 C1 -115(4) 2_666 . . . ? O1 U1 O1 C1 -16(100) 2_666 . . . ? O3 U1 O1 C1 155(4) 2_666 . . . ? O3 U1 O1 C1 -25(4) . . . . ? O2 U1 O3 C13 32(2) . . . . ? O2 U1 O3 C13 -148(2) 2_666 . . . ? O1 U1 O3 C13 -58(2) 2_666 . . . ? O1 U1 O3 C13 122(2) . . . . ? O3 U1 O3 C13 -46(100) 2_666 . . . ? U1 O1 C1 C6 143(4) . . . . ? U1 O1 C1 C2 -39(5) . . . . ? F1 C2 C1 O1 3.2(14) . . . . ? C3 C2 C1 O1 -178.9(10) . . . . ? F1 C2 C1 C6 -178.3(9) . . . . ? C3 C2 C1 C6 -0.5(14) . . . . ? O1 C1 C6 F5 -1.7(15) . . . . ? C2 C1 C6 F5 179.8(9) . . . . ? O1 C1 C6 C5 178.7(10) . . . . ? C2 C1 C6 C5 0.3(15) . . . . ? F1 C2 C3 F2 -1.8(14) . . . . ? C1 C2 C3 F2 -179.6(9) . . . . ? F1 C2 C3 C4 178.8(9) . . . . ? C1 C2 C3 C4 0.9(15) . . . . ? U1 O3 C13 C14 38(3) . . . . ? U1 O3 C13 C16 165(2) . . . . ? U1 O3 C13 C15 -82(2) . . . . ? U1 O2 C7 C8 -44.0(19) . . . . ? U1 O2 C7 C12 136.1(12) . . . . ? C8 C7 C12 F10 -178.0(8) . . . . ? O2 C7 C12 F10 1.9(13) . . . . ? C8 C7 C12 C11 1.7(14) . . . . ? O2 C7 C12 C11 -178.3(8) . . . . ? O2 C7 C8 F6 -2.5(14) . . . . ? C12 C7 C8 F6 177.5(8) . . . . ? O2 C7 C8 C9 177.2(9) . . . . ? C12 C7 C8 C9 -2.9(15) . . . . ? F7 C9 C8 F6 -0.6(15) . . . . ? C10 C9 C8 F6 -177.7(9) . . . . ? F7 C9 C8 C7 179.7(9) . . . . ? C10 C9 C8 C7 2.6(16) . . . . ? F2 C3 C4 F3 0.2(15) . . . . ? C2 C3 C4 F3 179.7(9) . . . . ? F2 C3 C4 C5 179.3(9) . . . . ? C2 C3 C4 C5 -1.2(15) . . . . ? F8 C10 C11 F9 -2.9(15) . . . . ? C9 C10 C11 F9 179.0(9) . . . . ? F8 C10 C11 C12 178.2(9) . . . . ? C9 C10 C11 C12 0.1(16) . . . . ? F10 C12 C11 C10 179.4(9) . . . . ? C7 C12 C11 C10 -0.4(15) . . . . ? F10 C12 C11 F9 0.5(13) . . . . ? C7 C12 C11 F9 -179.3(8) . . . . ? F5 C6 C5 F4 -1.9(15) . . . . ? C1 C6 C5 F4 177.6(9) . . . . ? F5 C6 C5 C4 179.9(9) . . . . ? C1 C6 C5 C4 -0.6(16) . . . . ? F3 C4 C5 F4 1.9(14) . . . . ? C3 C4 C5 F4 -177.1(8) . . . . ? F3 C4 C5 C6 -179.9(9) . . . . ? C3 C4 C5 C6 1.0(15) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 4.218 _refine_diff_density_min -1.690 _refine_diff_density_rms 0.216 #===END=== _publ_contact_author_name 'Trevor W. Hayton' _publ_contact_author_email 'hayton@chem.ucsb.edu' loop_ _publ_author_name 'Skye Fortier' 'Guang Wu' 'Trevor W. Hayton' _journal_full_name 'Journal of the American Chemical Society' data_Complex_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Lithium 1,2-dimethoxyethane Uranium(IV) hexakis(pentafluorophenoxide) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H60 F30 Li2 O18 U' _chemical_formula_weight 1890.99 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' 'Li' 'Li' -0.0003 0.0001 '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' 'U' 'U' -9.6767 9.6646 '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' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 15.738(2) _cell_length_b 15.738(2) _cell_length_c 25.227(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5411.1(19) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour clear _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2796 _exptl_absorpt_coefficient_mu 2.393 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.485 _exptl_absorpt_correction_T_max 0.579 _exptl_absorpt_process_details 'Psi Scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9817 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.73 _reflns_number_total 2500 _reflns_number_gt 2102 _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^)+(0.0356P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2500 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _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 U1 U 0.6667 0.3333 0.3333 0.04439(14) Uani 1 6 d S . . O1 O 0.53510(17) 0.29404(18) 0.38241(10) 0.0557(7) Uani 1 1 d . . . F3 F 0.15768(15) 0.10944(17) 0.45694(10) 0.0731(7) Uani 1 1 d . . . C2 C 0.3905(2) 0.1491(2) 0.40880(13) 0.0428(8) Uani 1 1 d . . . C3 C 0.2971(3) 0.1027(2) 0.42853(14) 0.0445(8) Uani 1 1 d . . . C4 C 0.2501(2) 0.1548(3) 0.43818(14) 0.0494(9) Uani 1 1 d . . . F1 F 0.43357(15) 0.09445(15) 0.39888(9) 0.0573(5) Uani 1 1 d . . . F2 F 0.25120(15) 0.00553(15) 0.43873(9) 0.0623(6) Uani 1 1 d . . . C1 C 0.4434(2) 0.2494(2) 0.39856(13) 0.0415(8) Uani 1 1 d . . . F4 F 0.43742(16) 0.39607(15) 0.39801(10) 0.0690(6) Uani 1 1 d . . . F5 F 0.25346(16) 0.30582(17) 0.43642(11) 0.0754(7) Uani 1 1 d . . . C5 C 0.2985(3) 0.2532(3) 0.42765(15) 0.0504(9) Uani 1 1 d . . . C6 C 0.3926(3) 0.2995(2) 0.40799(14) 0.0462(9) Uani 1 1 d . . . O2 O 0.2494(2) 0.5357(2) 0.36576(13) 0.0794(9) Uani 1 1 d . . . Li1 Li 0.3333 0.6667 0.4119(4) 0.040(2) Uani 1 3 d S . . O3 O 0.4165(2) 0.6194(2) 0.45566(12) 0.0774(9) Uani 1 1 d . . . C9 C 0.3831(3) 0.5530(3) 0.49838(16) 0.0667(11) Uani 1 1 d . . . H9A H 0.3592 0.4876 0.4853 0.100 Uiso 1 1 calc R . . H9B H 0.3311 0.5564 0.5163 0.100 Uiso 1 1 calc R . . H9C H 0.4362 0.5697 0.5226 0.100 Uiso 1 1 calc R . . C7 C 0.2843(3) 0.5015(3) 0.32481(19) 0.0783(14) Uani 1 1 d . . . H7A H 0.3063 0.4593 0.3392 0.117 Uiso 1 1 calc R . . H7B H 0.3380 0.5561 0.3073 0.117 Uiso 1 1 calc R . . H7C H 0.2326 0.4655 0.2998 0.117 Uiso 1 1 calc R . . C8 C 0.1676(3) 0.4650(3) 0.38939(19) 0.0744(13) Uani 1 1 d . . . H8A H 0.1808 0.4151 0.4031 0.089 Uiso 1 1 calc R . . H8B H 0.1161 0.4343 0.3631 0.089 Uiso 1 1 calc R . . C10 C 0.4981(3) 0.6306(4) 0.4333(2) 0.0800(14) Uani 1 1 d . . . H10A H 0.4855 0.5677 0.4199 0.096 Uiso 1 1 calc R . . H10B H 0.5487 0.6515 0.4602 0.096 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 U1 0.03984(15) 0.03984(15) 0.0535(2) 0.000 0.000 0.01992(8) O1 0.0442(14) 0.0551(15) 0.0649(18) 0.0020(13) 0.0063(12) 0.0227(12) F3 0.0455(13) 0.0786(16) 0.0881(18) 0.0021(13) 0.0169(12) 0.0257(12) C2 0.043(2) 0.046(2) 0.043(2) -0.0060(16) -0.0057(16) 0.0253(17) C3 0.048(2) 0.042(2) 0.040(2) -0.0023(16) -0.0067(16) 0.0194(17) C4 0.0350(19) 0.056(2) 0.051(2) -0.0040(18) 0.0019(16) 0.0178(18) F1 0.0602(13) 0.0544(12) 0.0696(15) -0.0069(11) -0.0035(11) 0.0379(11) F2 0.0594(13) 0.0445(12) 0.0711(15) 0.0076(10) -0.0010(11) 0.0171(10) C1 0.0395(19) 0.047(2) 0.037(2) -0.0030(16) -0.0014(15) 0.0204(17) F4 0.0637(14) 0.0433(12) 0.1005(18) 0.0062(12) -0.0009(13) 0.0270(11) F5 0.0648(14) 0.0736(15) 0.1082(19) -0.0116(14) 0.0013(13) 0.0499(13) C5 0.048(2) 0.057(2) 0.056(2) -0.0094(18) -0.0022(18) 0.0337(19) C6 0.048(2) 0.040(2) 0.051(2) -0.0017(16) -0.0058(17) 0.0221(17) O2 0.0637(18) 0.0619(18) 0.093(2) -0.0250(16) 0.0229(17) 0.0170(15) Li1 0.037(3) 0.037(3) 0.048(6) 0.000 0.000 0.0183(15) O3 0.0615(18) 0.099(2) 0.086(2) 0.0424(18) 0.0208(16) 0.0514(17) C9 0.075(3) 0.066(3) 0.061(3) 0.022(2) 0.003(2) 0.037(2) C7 0.075(3) 0.075(3) 0.082(3) -0.030(3) 0.005(2) 0.036(3) C8 0.059(3) 0.053(3) 0.089(3) -0.015(2) 0.005(2) 0.011(2) C10 0.060(3) 0.087(3) 0.107(4) 0.028(3) 0.015(3) 0.048(3) _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 U1 O1 2.218(2) 17 ? U1 O1 2.218(2) 2_655 ? U1 O1 2.218(2) 3_665 ? U1 O1 2.218(2) . ? U1 O1 2.219(2) 18_545 ? U1 O1 2.219(2) 16_655 ? O1 C1 1.315(4) . ? F3 C4 1.345(4) . ? C2 F1 1.358(4) . ? C2 C3 1.367(5) . ? C2 C1 1.392(5) . ? C3 F2 1.349(4) . ? C3 C4 1.374(5) . ? C4 C5 1.366(5) . ? C1 C6 1.395(5) . ? F4 C6 1.342(4) . ? F5 C5 1.351(4) . ? C5 C6 1.375(5) . ? O2 C8 1.348(5) . ? O2 C7 1.398(5) . ? O2 Li1 2.151(6) . ? Li1 O3 2.112(6) 2_665 ? Li1 O3 2.112(6) 3_565 ? Li1 O3 2.112(6) . ? Li1 O2 2.151(6) 3_565 ? Li1 O2 2.151(6) 2_665 ? O3 C10 1.330(5) . ? O3 C9 1.407(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C10 1.480(6) 3_565 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 C8 1.480(6) 2_665 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? 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 O1 U1 O1 179.998(1) 17 2_655 ? O1 U1 O1 88.12(9) 17 3_665 ? O1 U1 O1 91.89(9) 2_655 3_665 ? O1 U1 O1 88.12(9) 17 . ? O1 U1 O1 91.89(9) 2_655 . ? O1 U1 O1 91.89(9) 3_665 . ? O1 U1 O1 91.88(9) 17 18_545 ? O1 U1 O1 88.11(9) 2_655 18_545 ? O1 U1 O1 180.0 3_665 18_545 ? O1 U1 O1 88.12(9) . 18_545 ? O1 U1 O1 91.88(9) 17 16_655 ? O1 U1 O1 88.11(9) 2_655 16_655 ? O1 U1 O1 88.12(9) 3_665 16_655 ? O1 U1 O1 180.0 . 16_655 ? O1 U1 O1 91.88(9) 18_545 16_655 ? C1 O1 U1 160.7(2) . . ? F1 C2 C3 118.2(3) . . ? F1 C2 C1 118.6(3) . . ? C3 C2 C1 123.1(3) . . ? F2 C3 C2 119.8(3) . . ? F2 C3 C4 120.0(3) . . ? C2 C3 C4 120.1(3) . . ? F3 C4 C5 120.9(3) . . ? F3 C4 C3 120.4(3) . . ? C5 C4 C3 118.7(3) . . ? O1 C1 C2 122.5(3) . . ? O1 C1 C6 122.4(3) . . ? C2 C1 C6 115.0(3) . . ? F5 C5 C4 119.7(3) . . ? F5 C5 C6 119.4(3) . . ? C4 C5 C6 120.9(3) . . ? F4 C6 C5 119.0(3) . . ? F4 C6 C1 118.9(3) . . ? C5 C6 C1 122.1(3) . . ? C8 O2 C7 113.9(3) . . ? C8 O2 Li1 115.3(3) . . ? C7 O2 Li1 126.7(3) . . ? O3 Li1 O3 95.2(3) 2_665 3_565 ? O3 Li1 O3 95.2(3) 2_665 . ? O3 Li1 O3 95.2(3) 3_565 . ? O3 Li1 O2 75.39(11) 2_665 3_565 ? O3 Li1 O2 97.90(13) 3_565 3_565 ? O3 Li1 O2 164.48(12) . 3_565 ? O3 Li1 O2 164.48(12) 2_665 . ? O3 Li1 O2 75.39(11) 3_565 . ? O3 Li1 O2 97.90(13) . . ? O2 Li1 O2 93.5(3) 3_565 . ? O3 Li1 O2 97.90(13) 2_665 2_665 ? O3 Li1 O2 164.48(12) 3_565 2_665 ? O3 Li1 O2 75.39(11) . 2_665 ? O2 Li1 O2 93.5(3) 3_565 2_665 ? O2 Li1 O2 93.5(3) . 2_665 ? C10 O3 C9 113.7(3) . . ? C10 O3 Li1 117.3(3) . . ? C9 O3 Li1 126.4(3) . . ? O3 C9 H9A 109.5 . . ? O3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O2 C8 C10 113.4(3) . 3_565 ? O2 C8 H8A 108.9 . . ? C10 C8 H8A 108.9 3_565 . ? O2 C8 H8B 108.9 . . ? C10 C8 H8B 108.9 3_565 . ? H8A C8 H8B 107.7 . . ? O3 C10 C8 113.7(3) . 2_665 ? O3 C10 H10A 108.8 . . ? C8 C10 H10A 108.8 2_665 . ? O3 C10 H10B 108.8 . . ? C8 C10 H10B 108.8 2_665 . ? H10A C10 H10B 107.7 . . ? 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 O1 U1 O1 C1 83.6(7) 17 . . . ? O1 U1 O1 C1 -96.4(7) 2_655 . . . ? O1 U1 O1 C1 171.6(7) 3_665 . . . ? O1 U1 O1 C1 -8.4(7) 18_545 . . . ? O1 U1 O1 C1 -24(14) 16_655 . . . ? F1 C2 C3 F2 1.5(5) . . . . ? C1 C2 C3 F2 -178.3(3) . . . . ? F1 C2 C3 C4 -178.8(3) . . . . ? C1 C2 C3 C4 1.4(5) . . . . ? F2 C3 C4 F3 -1.2(5) . . . . ? C2 C3 C4 F3 179.1(3) . . . . ? F2 C3 C4 C5 179.8(3) . . . . ? C2 C3 C4 C5 0.0(5) . . . . ? U1 O1 C1 C2 59.2(8) . . . . ? U1 O1 C1 C6 -122.5(6) . . . . ? F1 C2 C1 O1 -3.8(5) . . . . ? C3 C2 C1 O1 176.1(3) . . . . ? F1 C2 C1 C6 177.8(3) . . . . ? C3 C2 C1 C6 -2.4(5) . . . . ? F3 C4 C5 F5 0.4(5) . . . . ? C3 C4 C5 F5 179.5(3) . . . . ? F3 C4 C5 C6 -179.4(3) . . . . ? C3 C4 C5 C6 -0.3(6) . . . . ? F5 C5 C6 F4 0.0(5) . . . . ? C4 C5 C6 F4 179.7(3) . . . . ? F5 C5 C6 C1 179.4(3) . . . . ? C4 C5 C6 C1 -0.8(6) . . . . ? O1 C1 C6 F4 3.0(5) . . . . ? C2 C1 C6 F4 -178.5(3) . . . . ? O1 C1 C6 C5 -176.4(3) . . . . ? C2 C1 C6 C5 2.1(5) . . . . ? C8 O2 Li1 O3 -62.1(18) . . . 2_665 ? C7 O2 Li1 O3 142.2(15) . . . 2_665 ? C8 O2 Li1 O3 -8.2(3) . . . 3_565 ? C7 O2 Li1 O3 -163.9(4) . . . 3_565 ? C8 O2 Li1 O3 85.1(4) . . . . ? C7 O2 Li1 O3 -70.6(5) . . . . ? C8 O2 Li1 O2 -105.5(4) . . . 3_565 ? C7 O2 Li1 O2 98.8(3) . . . 3_565 ? C8 O2 Li1 O2 160.8(3) . . . 2_665 ? C7 O2 Li1 O2 5.1(5) . . . 2_665 ? O3 Li1 O3 C10 -103.3(5) 2_665 . . . ? O3 Li1 O3 C10 161.0(4) 3_565 . . . ? O2 Li1 O3 C10 -51.6(18) 3_565 . . . ? O2 Li1 O3 C10 85.1(4) . . . . ? O2 Li1 O3 C10 -6.5(4) 2_665 . . . ? O3 Li1 O3 C9 96.3(3) 2_665 . . . ? O3 Li1 O3 C9 0.5(5) 3_565 . . . ? O2 Li1 O3 C9 147.9(15) 3_565 . . . ? O2 Li1 O3 C9 -75.4(5) . . . . ? O2 Li1 O3 C9 -166.9(4) 2_665 . . . ? C7 O2 C8 C10 178.9(4) . . . 3_565 ? Li1 O2 C8 C10 20.1(5) . . . 3_565 ? C9 O3 C10 C8 -178.3(4) . . . 2_665 ? Li1 O3 C10 C8 18.8(6) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.711 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.075 #===END=== _publ_contact_author_name 'Trevor W. Hayton' _publ_contact_author_email 'hayton@chem.ucsb.edu' loop_ _publ_author_name 'Skye Fortier' 'Guang Wu' 'Trevor W. Hayton' _journal_full_name 'Journal of the American Chemical Society' data_Complex_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver 1,2-dimethoxyethane bistoluene Uranium(V) hexakis(pentafluorophenoxide) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H26 Ag F30 O8 U' _chemical_formula_weight 1718.65 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 '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 11.808(3) _cell_length_b 12.910(3) _cell_length_c 19.626(4) _cell_angle_alpha 82.199(3) _cell_angle_beta 79.196(3) _cell_angle_gamma 73.259(3) _cell_volume 2803.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular_block _exptl_crystal_colour red _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1646 _exptl_absorpt_coefficient_mu 3.389 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.281 _exptl_absorpt_correction_T_max 0.412 _exptl_absorpt_process_details 'Psi Scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23446 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 26.73 _reflns_number_total 11227 _reflns_number_gt 7081 _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^)+(0.0646P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11227 _refine_ls_number_parameters 824 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.934 _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 F2 F 0.4147(3) 1.2169(3) -0.00359(18) 0.0658(10) Uani 1 1 d . . . F13 F 1.2324(4) 1.0847(3) 0.3025(2) 0.0776(12) Uani 1 1 d . . . C15 C 1.1946(5) 0.9678(5) 0.2332(3) 0.0488(15) Uani 1 1 d . . . U1 U 1.0000 1.0000 0.0000 0.04484(11) Uani 1 2 d S . . U2 U 0.0000 0.0000 0.5000 0.05681(13) Uani 1 2 d S . . Ag Ag 0.40498(8) 0.60746(5) 0.76309(4) 0.0984(3) Uani 1 1 d . . . O3 O 0.9901(4) 1.0191(4) 0.1075(2) 0.0610(12) Uani 1 1 d . . . F12 F 1.2757(3) 0.8830(3) 0.26030(17) 0.0651(10) Uani 1 1 d . . . F27 F 0.4230(4) 0.2356(4) 0.4900(2) 0.0923(14) Uani 1 1 d . . . O4 O 0.0259(4) -0.0550(4) 0.4001(3) 0.0782(15) Uani 1 1 d . . . F16 F -0.1534(4) 0.0748(3) 0.3300(3) 0.0985(16) Uani 1 1 d . . . O6 O 0.1804(4) 0.0028(4) 0.4888(3) 0.0666(13) Uani 1 1 d . . . F6 F 0.8504(3) 0.7849(3) -0.0322(2) 0.0663(10) Uani 1 1 d . . . C14 C 1.1362(5) 0.9502(5) 0.1835(3) 0.0460(14) Uani 1 1 d . . . O1 O 0.8139(3) 1.0203(4) 0.0126(2) 0.0605(12) Uani 1 1 d . . . F14 F 1.0688(4) 1.2528(3) 0.2475(2) 0.0892(14) Uani 1 1 d . . . F1 F 0.6509(3) 1.1876(3) -0.0464(2) 0.0729(11) Uani 1 1 d . . . F21 F 0.1179(4) 0.2770(3) 0.3979(2) 0.0761(11) Uani 1 1 d . . . F5 F 0.7298(3) 0.8812(3) 0.1138(2) 0.0740(11) Uani 1 1 d . . . F11 F 1.1578(3) 0.8504(3) 0.16462(18) 0.0629(10) Uani 1 1 d . . . F15 F 0.9479(4) 1.2209(3) 0.1527(2) 0.0762(12) Uani 1 1 d . . . F30 F 0.3545(4) -0.1105(3) 0.3932(2) 0.0798(12) Uani 1 1 d . . . F4 F 0.4928(4) 0.9149(4) 0.1592(2) 0.0876(13) Uani 1 1 d . . . O2 O 1.0276(4) 0.8300(3) 0.0217(2) 0.0607(12) Uani 1 1 d . . . F20 F 0.1121(4) -0.2683(3) 0.37177(19) 0.0728(11) Uani 1 1 d . . . C5 C 0.5330(6) 0.9828(5) 0.1086(3) 0.0529(16) Uani 1 1 d . . . C36 C 0.3709(6) -0.0252(5) 0.4178(3) 0.0514(16) Uani 1 1 d . . . C6 C 0.6519(6) 0.9672(5) 0.0864(3) 0.0496(15) Uani 1 1 d . . . C35 C 0.4741(6) 0.0061(6) 0.3937(3) 0.0606(18) Uani 1 1 d . . . O5 O -0.0420(4) 0.1626(3) 0.4579(3) 0.0806(15) Uani 1 1 d . . . F18 F -0.1540(5) -0.2213(4) 0.2139(2) 0.1108(18) Uani 1 1 d . . . F28 F 0.5940(4) 0.1230(4) 0.3947(3) 0.1078(17) Uani 1 1 d . . . F3 F 0.3343(3) 1.0812(4) 0.1006(2) 0.0818(12) Uani 1 1 d . . . F26 F 0.2191(4) 0.1767(3) 0.5365(2) 0.0835(13) Uani 1 1 d . . . F25 F -0.2655(4) 0.2744(4) 0.5177(2) 0.0953(14) Uani 1 1 d . . . F8 F 0.9037(5) 0.4484(3) 0.1007(2) 0.0971(15) Uani 1 1 d . . . F24 F -0.3230(4) 0.4912(4) 0.5193(3) 0.1122(18) Uani 1 1 d . . . F22 F 0.0577(6) 0.4939(4) 0.3996(4) 0.133(2) Uani 1 1 d . . . C2 C 0.6140(5) 1.1195(5) 0.0052(3) 0.0446(14) Uani 1 1 d . . . F19 F 0.0225(5) -0.3467(3) 0.2793(2) 0.0962(16) Uani 1 1 d . . . C13 C 1.0494(5) 1.0363(5) 0.1548(3) 0.0479(15) Uani 1 1 d . . . C10 C 0.9343(7) 0.5418(6) 0.0811(4) 0.068(2) Uani 1 1 d . . . F17 F -0.2434(4) -0.0065(4) 0.2388(2) 0.1014(16) Uani 1 1 d . . . C34 C 0.4913(6) 0.0947(6) 0.4180(4) 0.066(2) Uani 1 1 d . . . F7 F 0.7919(4) 0.5961(3) 0.0055(2) 0.0831(13) Uani 1 1 d . . . C4 C 0.4507(5) 1.0680(5) 0.0790(3) 0.0508(15) Uani 1 1 d . . . C18 C 1.0301(5) 1.1357(5) 0.1785(3) 0.0535(16) Uani 1 1 d . . . O8 O 0.4759(5) 0.4229(4) 0.8011(3) 0.0906(17) Uani 1 1 d . . . F9 F 1.0835(5) 0.4893(3) 0.1531(2) 0.1078(17) Uani 1 1 d . . . C32 C 0.3021(6) 0.1195(5) 0.4898(3) 0.0501(15) Uani 1 1 d . . . C16 C 1.1730(6) 1.0678(5) 0.2557(3) 0.0545(16) Uani 1 1 d . . . F10 F 1.1475(4) 0.6741(3) 0.1124(3) 0.0940(15) Uani 1 1 d . . . F29 F 0.5579(5) -0.0497(4) 0.3462(3) 0.1128(18) Uani 1 1 d . . . C3 C 0.4931(5) 1.1342(5) 0.0269(3) 0.0484(15) Uani 1 1 d . . . C37 C 0.2781(16) 0.6483(8) 0.6720(8) 0.151(8) Uani 1 1 d . . . H37 H 0.2574 0.7230 0.6745 0.181 Uiso 1 1 calc R . . C7 C 0.9979(6) 0.7364(5) 0.0401(3) 0.0524(16) Uani 1 1 d . . . C47 C 0.5380(10) 0.6329(9) 0.9015(6) 0.173(3) Uani 1 1 d D . . H47 H 0.6000 0.5879 0.9235 0.208 Uiso 1 1 calc R . . C26 C 0.0081(6) 0.3280(5) 0.4268(3) 0.0575(17) Uani 1 1 d . . . C11 C 1.0235(8) 0.5627(5) 0.1073(4) 0.069(2) Uani 1 1 d . . . C23 C -0.0210(7) -0.2430(5) 0.2933(3) 0.066(2) Uani 1 1 d . . . C49 C 0.4608(9) 0.7714(7) 0.8126(6) 0.173(3) Uani 1 1 d D . . H49 H 0.4740 0.8186 0.7736 0.208 Uiso 1 1 calc R . . C33 C 0.4058(6) 0.1497(6) 0.4662(3) 0.0579(17) Uani 1 1 d . . . C24 C 0.0252(6) -0.2027(5) 0.3399(3) 0.0523(16) Uani 1 1 d . . . C1 C 0.6970(5) 1.0351(5) 0.0337(3) 0.0430(14) Uani 1 1 d . . . C25 C -0.0727(6) 0.2691(5) 0.4579(3) 0.0512(15) Uani 1 1 d . . . F23 F -0.1635(6) 0.6011(3) 0.4592(4) 0.163(3) Uani 1 1 d . . . C31 C 0.2812(5) 0.0315(5) 0.4666(3) 0.0458(14) Uani 1 1 d . . . C17 C 1.0905(6) 1.1534(5) 0.2267(3) 0.0576(17) Uani 1 1 d . . . C41 C 0.2427(8) 0.4745(8) 0.7057(5) 0.097(3) Uani 1 1 d . . . H41 H 0.1958 0.4317 0.7314 0.117 Uiso 1 1 calc R . . C29 C -0.2142(7) 0.4373(6) 0.4893(4) 0.071(2) Uani 1 1 d . . . C20 C -0.1105(7) -0.0310(5) 0.3185(4) 0.067(2) Uani 1 1 d . . . C8 C 0.9090(6) 0.7125(5) 0.0141(3) 0.0520(15) Uani 1 1 d . . . C44 C 0.3496(10) 0.7582(9) 0.8400(7) 0.173(3) Uani 1 1 d D . . H44 H 0.2865 0.8011 0.8180 0.208 Uiso 1 1 calc R . . C40 C 0.3410(9) 0.4283(7) 0.6640(5) 0.084(3) Uani 1 1 d . . . C30 C -0.1848(6) 0.3279(6) 0.4885(3) 0.0598(17) Uani 1 1 d . . . C19 C -0.0200(6) -0.0941(6) 0.3545(3) 0.0574(17) Uani 1 1 d . . . C9 C 0.8767(6) 0.6170(6) 0.0335(4) 0.0608(17) Uani 1 1 d . . . C39 C 0.4069(9) 0.4863(11) 0.6272(5) 0.103(3) Uani 1 1 d . . . H39 H 0.4761 0.4526 0.5984 0.123 Uiso 1 1 calc R . . C28 C -0.1367(9) 0.4934(6) 0.4595(5) 0.090(3) Uani 1 1 d . . . C42 C 0.2093(9) 0.5817(10) 0.7117(6) 0.120(4) Uani 1 1 d . . . H42 H 0.1406 0.6121 0.7420 0.144 Uiso 1 1 calc R . . C12 C 1.0567(7) 0.6567(5) 0.0873(4) 0.0624(18) Uani 1 1 d . . . C46 C 0.4201(10) 0.6302(8) 0.9196(6) 0.173(3) Uani 1 1 d D . . H46 H 0.4097 0.5765 0.9550 0.208 Uiso 1 1 calc R . . C38 C 0.3775(15) 0.5946(13) 0.6297(7) 0.143(6) Uani 1 1 d . . . H38 H 0.4261 0.6341 0.6017 0.171 Uiso 1 1 calc R . . C27 C -0.0234(8) 0.4387(6) 0.4280(5) 0.083(3) Uani 1 1 d . . . C43 C 0.3822(14) 0.3041(9) 0.6563(8) 0.220(9) Uani 1 1 d . . . H43A H 0.3566 0.2897 0.6157 0.330 Uiso 1 1 calc R . . H43B H 0.3475 0.2667 0.6968 0.330 Uiso 1 1 calc R . . H43C H 0.4679 0.2793 0.6515 0.330 Uiso 1 1 calc R . . C45 C 0.3189(11) 0.6864(8) 0.8983(7) 0.173(3) Uani 1 1 d D . . H45 H 0.2425 0.6806 0.9173 0.208 Uiso 1 1 calc R . . C22 C -0.1102(7) -0.1778(6) 0.2597(4) 0.072(2) Uani 1 1 d . . . C21 C -0.1561(7) -0.0725(6) 0.2724(4) 0.066(2) Uani 1 1 d . . . C54 C 0.4097(15) 0.3688(10) 0.8516(6) 0.195(8) Uani 1 1 d . . . H54A H 0.4321 0.2932 0.8437 0.293 Uiso 1 1 calc R . . H54B H 0.3260 0.3993 0.8493 0.293 Uiso 1 1 calc R . . H54C H 0.4251 0.3762 0.8968 0.293 Uiso 1 1 calc R . . C53 C 0.6072(13) 0.3873(9) 0.7919(8) 0.181(8) Uani 1 1 d . . . H53A H 0.6351 0.3089 0.7918 0.217 Uiso 1 1 calc R . . H53B H 0.6359 0.4087 0.8296 0.217 Uiso 1 1 calc R . . O7 O 0.6140(8) 0.5382(11) 0.7288(4) 0.171(5) Uani 1 1 d . . . C52 C 0.6541(15) 0.442(2) 0.7209(10) 0.33(2) Uani 1 1 d . . . H52A H 0.7409 0.4223 0.7118 0.401 Uiso 1 1 calc R . . H52B H 0.6244 0.4231 0.6829 0.401 Uiso 1 1 calc R . . C51 C 0.674(2) 0.604(2) 0.6692(7) 0.348(19) Uani 1 1 d . . . H51A H 0.6499 0.6794 0.6785 0.522 Uiso 1 1 calc R . . H51B H 0.6503 0.5977 0.6262 0.522 Uiso 1 1 calc R . . H51C H 0.7595 0.5774 0.6656 0.522 Uiso 1 1 calc R . . C48 C 0.5532(11) 0.7077(8) 0.8484(6) 0.173(3) Uani 1 1 d D . . C50 C 0.6711(10) 0.7177(13) 0.8216(8) 0.273(11) Uani 1 1 d D . . H50A H 0.6963 0.7539 0.8532 0.410 Uiso 1 1 calc R . . H50B H 0.6709 0.7590 0.7771 0.410 Uiso 1 1 calc R . . H50C H 0.7253 0.6467 0.8165 0.410 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 F2 0.040(2) 0.075(3) 0.066(2) 0.0053(19) -0.0150(17) 0.0081(18) F13 0.087(3) 0.072(3) 0.078(3) -0.016(2) -0.039(2) -0.006(2) C15 0.042(4) 0.054(4) 0.044(3) 0.001(3) 0.002(3) -0.011(3) U1 0.02670(18) 0.04234(19) 0.0657(2) 0.00581(15) -0.01459(14) -0.00974(14) U2 0.0355(2) 0.03698(19) 0.0993(3) -0.02331(18) 0.00680(18) -0.01509(15) Ag 0.1417(7) 0.0602(4) 0.1093(5) -0.0022(3) -0.0848(5) -0.0132(4) O3 0.045(3) 0.072(3) 0.070(3) -0.001(2) -0.013(2) -0.022(2) F12 0.066(3) 0.059(2) 0.059(2) 0.0025(18) -0.0192(18) 0.0037(19) F27 0.106(4) 0.094(3) 0.102(3) -0.016(3) -0.004(3) -0.070(3) O4 0.053(3) 0.072(3) 0.114(4) -0.045(3) 0.014(3) -0.025(3) F16 0.068(3) 0.055(3) 0.147(4) -0.016(3) 0.027(3) -0.002(2) O6 0.037(3) 0.056(3) 0.110(4) -0.020(3) 0.006(2) -0.022(2) F6 0.051(2) 0.058(2) 0.089(3) 0.007(2) -0.0222(19) -0.0125(18) C14 0.042(3) 0.049(4) 0.047(3) 0.004(3) -0.002(3) -0.019(3) O1 0.026(2) 0.067(3) 0.091(3) -0.008(2) -0.013(2) -0.013(2) F14 0.094(3) 0.058(3) 0.111(3) -0.029(2) -0.035(3) 0.008(2) F1 0.054(2) 0.065(2) 0.087(3) 0.019(2) 0.0032(19) -0.0160(19) F21 0.062(3) 0.082(3) 0.081(3) 0.003(2) -0.006(2) -0.020(2) F5 0.071(3) 0.067(2) 0.076(2) 0.008(2) -0.034(2) 0.004(2) F11 0.075(3) 0.051(2) 0.062(2) -0.0005(18) -0.0124(19) -0.0173(19) F15 0.060(3) 0.062(2) 0.096(3) -0.007(2) -0.022(2) 0.007(2) F30 0.090(3) 0.065(3) 0.085(3) -0.029(2) -0.008(2) -0.017(2) F4 0.094(3) 0.083(3) 0.074(3) 0.022(2) 0.006(2) -0.030(3) O2 0.049(3) 0.042(2) 0.093(3) 0.007(2) -0.021(2) -0.016(2) F20 0.088(3) 0.062(2) 0.069(2) -0.0064(19) -0.033(2) -0.007(2) C5 0.055(4) 0.061(4) 0.042(3) 0.003(3) -0.004(3) -0.021(3) C36 0.056(4) 0.046(4) 0.053(4) -0.004(3) -0.011(3) -0.012(3) C6 0.048(4) 0.051(4) 0.049(4) -0.004(3) -0.019(3) -0.005(3) C35 0.047(4) 0.058(4) 0.060(4) 0.001(3) 0.015(3) -0.004(3) O5 0.066(3) 0.038(3) 0.136(5) -0.019(3) 0.002(3) -0.016(2) F18 0.149(5) 0.096(3) 0.091(3) 0.000(3) -0.075(3) -0.007(3) F28 0.058(3) 0.107(4) 0.153(4) 0.018(3) 0.013(3) -0.045(3) F3 0.035(2) 0.116(4) 0.085(3) 0.004(2) 0.0071(19) -0.020(2) F26 0.099(3) 0.064(3) 0.090(3) -0.031(2) 0.032(3) -0.044(2) F25 0.061(3) 0.100(3) 0.113(4) -0.002(3) 0.008(2) -0.019(3) F8 0.128(4) 0.045(2) 0.112(4) -0.001(2) 0.003(3) -0.030(3) F24 0.093(4) 0.107(4) 0.113(4) -0.050(3) -0.033(3) 0.039(3) F22 0.127(5) 0.081(4) 0.209(6) 0.058(4) -0.068(4) -0.060(3) C2 0.036(3) 0.046(3) 0.052(3) 0.005(3) -0.006(3) -0.016(3) F19 0.150(5) 0.053(3) 0.092(3) -0.007(2) -0.067(3) -0.006(3) C13 0.030(3) 0.062(4) 0.048(3) 0.003(3) -0.001(3) -0.015(3) C10 0.079(6) 0.044(4) 0.079(5) -0.010(4) 0.005(4) -0.022(4) F17 0.091(4) 0.089(3) 0.091(3) 0.030(3) -0.015(3) 0.012(3) C34 0.044(4) 0.070(5) 0.082(5) 0.020(4) -0.005(4) -0.029(4) F7 0.069(3) 0.062(3) 0.126(4) -0.017(2) -0.012(3) -0.027(2) C4 0.029(3) 0.074(4) 0.048(3) -0.007(3) -0.001(3) -0.015(3) C18 0.033(3) 0.049(4) 0.069(4) 0.003(3) -0.006(3) -0.001(3) O8 0.088(4) 0.079(4) 0.090(4) 0.017(3) -0.017(3) -0.009(3) F9 0.166(5) 0.050(2) 0.098(3) 0.015(2) -0.048(3) -0.007(3) C32 0.050(4) 0.043(3) 0.057(4) -0.008(3) 0.006(3) -0.017(3) C16 0.052(4) 0.059(4) 0.051(4) -0.005(3) -0.006(3) -0.013(3) F10 0.111(4) 0.054(2) 0.128(4) 0.003(2) -0.077(3) -0.008(2) F29 0.103(4) 0.086(3) 0.113(4) -0.014(3) 0.054(3) -0.010(3) C3 0.035(3) 0.052(4) 0.053(4) 0.001(3) -0.013(3) -0.003(3) C37 0.253(19) 0.040(5) 0.196(15) -0.019(7) -0.190(15) 0.007(8) C7 0.051(4) 0.036(3) 0.064(4) 0.001(3) -0.006(3) -0.006(3) C47 0.201(7) 0.091(4) 0.261(8) -0.075(4) -0.143(7) 0.004(4) C26 0.062(5) 0.046(4) 0.064(4) -0.001(3) -0.021(3) -0.007(3) C11 0.098(6) 0.030(4) 0.063(4) 0.004(3) -0.009(4) 0.002(4) C23 0.093(6) 0.048(4) 0.051(4) 0.009(3) -0.024(4) -0.005(4) C49 0.201(7) 0.091(4) 0.261(8) -0.075(4) -0.143(7) 0.004(4) C33 0.055(4) 0.061(4) 0.064(4) -0.001(3) -0.008(3) -0.028(3) C24 0.063(4) 0.045(4) 0.047(4) -0.005(3) 0.002(3) -0.019(3) C1 0.022(3) 0.053(4) 0.056(4) -0.014(3) -0.008(3) -0.008(3) C25 0.059(4) 0.037(3) 0.061(4) -0.010(3) -0.017(3) -0.012(3) F23 0.179(6) 0.028(2) 0.299(9) -0.017(4) -0.127(6) 0.002(3) C31 0.034(3) 0.051(4) 0.053(4) -0.001(3) -0.007(3) -0.014(3) C17 0.048(4) 0.051(4) 0.068(4) -0.009(3) -0.002(3) -0.008(3) C41 0.067(6) 0.094(7) 0.138(8) -0.015(6) -0.018(6) -0.029(5) C29 0.067(5) 0.060(5) 0.082(5) -0.024(4) -0.034(4) 0.008(4) C20 0.060(5) 0.037(4) 0.082(5) -0.006(3) 0.034(4) -0.010(3) C8 0.046(4) 0.037(3) 0.067(4) -0.005(3) -0.007(3) -0.002(3) C44 0.201(7) 0.091(4) 0.261(8) -0.075(4) -0.143(7) 0.004(4) C40 0.073(6) 0.074(6) 0.106(7) -0.039(5) -0.031(5) 0.001(5) C30 0.058(5) 0.056(4) 0.063(4) -0.010(3) -0.008(3) -0.010(3) C19 0.045(4) 0.061(4) 0.061(4) -0.013(3) 0.016(3) -0.018(3) C9 0.052(4) 0.054(4) 0.079(5) -0.015(4) -0.002(3) -0.019(3) C39 0.086(7) 0.145(11) 0.078(6) -0.024(7) -0.027(5) -0.016(7) C28 0.098(7) 0.038(4) 0.137(8) -0.012(5) -0.063(6) 0.009(5) C42 0.097(8) 0.118(9) 0.132(9) -0.065(8) -0.060(7) 0.043(7) C12 0.072(5) 0.043(4) 0.071(4) -0.007(3) -0.021(4) -0.006(3) C46 0.201(7) 0.091(4) 0.261(8) -0.075(4) -0.143(7) 0.004(4) C38 0.218(17) 0.134(11) 0.130(11) 0.068(9) -0.114(11) -0.113(12) C27 0.100(7) 0.055(5) 0.109(6) 0.025(4) -0.051(5) -0.037(5) C43 0.271(19) 0.102(9) 0.290(19) -0.113(11) -0.167(16) 0.070(10) C45 0.201(7) 0.091(4) 0.261(8) -0.075(4) -0.143(7) 0.004(4) C22 0.091(6) 0.071(5) 0.053(4) 0.009(4) -0.026(4) -0.017(4) C21 0.062(5) 0.054(5) 0.064(5) 0.019(4) 0.005(4) -0.006(4) C54 0.35(2) 0.117(10) 0.103(8) 0.030(7) 0.032(11) -0.104(12) C53 0.213(16) 0.101(8) 0.211(14) -0.069(9) -0.153(13) 0.088(9) O7 0.129(7) 0.331(14) 0.102(5) -0.082(8) 0.048(5) -0.154(9) C52 0.169(16) 0.52(4) 0.207(19) -0.27(3) -0.067(15) 0.20(2) C51 0.44(3) 0.67(5) 0.099(10) -0.084(18) 0.083(15) -0.46(4) C48 0.201(7) 0.091(4) 0.261(8) -0.075(4) -0.143(7) 0.004(4) C50 0.185(19) 0.33(3) 0.31(2) -0.21(2) -0.028(17) -0.001(17) _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 F2 C3 1.349(6) . ? F13 C16 1.329(7) . ? C15 F12 1.352(6) . ? C15 C16 1.360(9) . ? C15 C14 1.372(8) . ? U1 O1 2.107(4) 2_775 ? U1 O1 2.107(4) . ? U1 O2 2.118(4) 2_775 ? U1 O2 2.118(4) . ? U1 O3 2.134(4) . ? U1 O3 2.134(4) 2_775 ? U2 O5 2.102(5) . ? U2 O5 2.102(5) 2_556 ? U2 O6 2.110(4) 2_556 ? U2 O6 2.110(4) . ? U2 O4 2.114(5) 2_556 ? U2 O4 2.114(5) . ? Ag O8 2.353(5) . ? Ag O7 2.370(10) . ? Ag C37 2.452(9) . ? Ag C44 2.488(10) . ? Ag C38 2.731(12) . ? Ag C49 2.732(9) . ? O3 C13 1.338(7) . ? F27 C33 1.340(7) . ? O4 C19 1.346(8) . ? F16 C20 1.346(7) . ? O6 C31 1.326(7) . ? F6 C8 1.346(7) . ? C14 F11 1.329(7) . ? C14 C13 1.412(8) . ? O1 C1 1.330(6) . ? F14 C17 1.339(7) . ? F1 C2 1.342(6) . ? F21 C26 1.331(7) . ? F5 C6 1.343(6) . ? F15 C18 1.352(7) . ? F30 C36 1.337(7) . ? F4 C5 1.344(7) . ? O2 C7 1.339(7) . ? F20 C24 1.326(7) . ? C5 C6 1.354(9) . ? C5 C4 1.384(8) . ? C36 C35 1.373(9) . ? C36 C31 1.393(8) . ? C6 C1 1.393(8) . ? C35 F29 1.340(7) . ? C35 C34 1.377(10) . ? O5 C25 1.317(7) . ? F18 C22 1.367(8) . ? F28 C34 1.348(7) . ? F3 C4 1.328(6) . ? F26 C32 1.333(7) . ? F25 C30 1.335(8) . ? F8 C10 1.344(8) . ? F24 C29 1.339(8) . ? F22 C27 1.350(9) . ? C2 C1 1.373(8) . ? C2 C3 1.375(8) . ? F19 C23 1.336(7) . ? C13 C18 1.367(9) . ? C10 C11 1.360(11) . ? C10 C9 1.374(10) . ? F17 C21 1.350(8) . ? C34 C33 1.353(10) . ? F7 C9 1.334(8) . ? C4 C3 1.358(8) . ? C18 C17 1.364(9) . ? O8 C54 1.385(11) . ? O8 C53 1.468(14) . ? F9 C11 1.352(8) . ? C32 C33 1.370(8) . ? C32 C31 1.380(8) . ? C16 C17 1.383(9) . ? F10 C12 1.346(8) . ? C37 C38 1.368(19) . ? C37 C42 1.410(17) . ? C37 H37 0.9300 . ? C7 C8 1.374(9) . ? C7 C12 1.404(9) . ? C47 C48 1.345(9) . ? C47 C46 1.379(9) . ? C47 H47 0.9300 . ? C26 C27 1.372(10) . ? C26 C25 1.390(9) . ? C11 C12 1.367(10) . ? C23 C22 1.361(9) . ? C23 C24 1.372(9) . ? C49 C44 1.372(9) . ? C49 C48 1.404(8) . ? C49 H49 0.9300 . ? C24 C19 1.398(9) . ? C25 C30 1.391(9) . ? F23 C28 1.333(8) . ? C41 C40 1.323(12) . ? C41 C42 1.339(13) . ? C41 H41 0.9300 . ? C29 C28 1.331(11) . ? C29 C30 1.355(10) . ? C20 C21 1.370(10) . ? C20 C19 1.389(10) . ? C8 C9 1.377(9) . ? C44 C45 1.431(9) . ? C44 H44 0.9300 . ? C40 C39 1.290(13) . ? C40 C43 1.556(13) . ? C39 C38 1.346(15) . ? C39 H39 0.9300 . ? C28 C27 1.391(12) . ? C42 H42 0.9300 . ? C46 C45 1.317(8) . ? C46 H46 0.9300 . ? C38 H38 0.9300 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C45 H45 0.9300 . ? C22 C21 1.349(10) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C53 C52 1.56(3) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? O7 C52 1.21(2) . ? O7 C51 1.539(17) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C48 C50 1.429(9) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 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 F12 C15 C16 119.5(6) . . ? F12 C15 C14 118.7(6) . . ? C16 C15 C14 121.8(6) . . ? O1 U1 O1 180.0(3) 2_775 . ? O1 U1 O2 89.90(16) 2_775 2_775 ? O1 U1 O2 90.10(16) . 2_775 ? O1 U1 O2 90.10(16) 2_775 . ? O1 U1 O2 89.90(16) . . ? O2 U1 O2 180.0(3) 2_775 . ? O1 U1 O3 88.58(17) 2_775 . ? O1 U1 O3 91.42(17) . . ? O2 U1 O3 88.99(18) 2_775 . ? O2 U1 O3 91.01(18) . . ? O1 U1 O3 91.42(17) 2_775 2_775 ? O1 U1 O3 88.58(17) . 2_775 ? O2 U1 O3 91.01(18) 2_775 2_775 ? O2 U1 O3 88.99(18) . 2_775 ? O3 U1 O3 180.0 . 2_775 ? O5 U2 O5 180.000(1) . 2_556 ? O5 U2 O6 91.42(18) . 2_556 ? O5 U2 O6 88.58(18) 2_556 2_556 ? O5 U2 O6 88.58(18) . . ? O5 U2 O6 91.42(18) 2_556 . ? O6 U2 O6 180.0 2_556 . ? O5 U2 O4 89.0(2) . 2_556 ? O5 U2 O4 91.0(2) 2_556 2_556 ? O6 U2 O4 92.04(18) 2_556 2_556 ? O6 U2 O4 87.96(18) . 2_556 ? O5 U2 O4 91.0(2) . . ? O5 U2 O4 89.0(2) 2_556 . ? O6 U2 O4 87.96(18) 2_556 . ? O6 U2 O4 92.04(18) . . ? O4 U2 O4 180.0 2_556 . ? O8 Ag O7 67.3(3) . . ? O8 Ag C37 116.2(3) . . ? O7 Ag C37 117.4(5) . . ? O8 Ag C44 124.2(3) . . ? O7 Ag C44 114.0(3) . . ? C37 Ag C44 111.1(4) . . ? O8 Ag C38 101.4(4) . . ? O7 Ag C38 87.9(4) . . ? C37 Ag C38 30.0(4) . . ? C44 Ag C38 133.9(5) . . ? O8 Ag C49 123.7(2) . . ? O7 Ag C49 85.8(3) . . ? C37 Ag C49 120.1(3) . . ? C44 Ag C49 30.0(2) . . ? C38 Ag C49 127.1(3) . . ? C13 O3 U1 144.5(4) . . ? C19 O4 U2 146.8(4) . . ? C31 O6 U2 161.1(4) . . ? F11 C14 C15 119.6(5) . . ? F11 C14 C13 119.9(5) . . ? C15 C14 C13 120.4(6) . . ? C1 O1 U1 168.7(4) . . ? C7 O2 U1 157.2(4) . . ? F4 C5 C6 120.5(6) . . ? F4 C5 C4 118.8(6) . . ? C6 C5 C4 120.7(6) . . ? F30 C36 C35 119.8(6) . . ? F30 C36 C31 118.8(6) . . ? C35 C36 C31 121.4(6) . . ? F5 C6 C5 119.6(6) . . ? F5 C6 C1 118.2(6) . . ? C5 C6 C1 122.2(5) . . ? F29 C35 C36 119.7(7) . . ? F29 C35 C34 120.0(7) . . ? C36 C35 C34 120.3(6) . . ? C25 O5 U2 157.3(5) . . ? F1 C2 C1 119.5(5) . . ? F1 C2 C3 118.9(5) . . ? C1 C2 C3 121.5(5) . . ? O3 C13 C18 123.1(6) . . ? O3 C13 C14 120.7(6) . . ? C18 C13 C14 116.2(6) . . ? F8 C10 C11 120.6(7) . . ? F8 C10 C9 120.3(7) . . ? C11 C10 C9 119.1(7) . . ? F28 C34 C33 121.4(7) . . ? F28 C34 C35 119.4(7) . . ? C33 C34 C35 119.1(6) . . ? F3 C4 C3 122.3(6) . . ? F3 C4 C5 119.9(6) . . ? C3 C4 C5 117.8(6) . . ? F15 C18 C17 118.3(6) . . ? F15 C18 C13 118.5(6) . . ? C17 C18 C13 123.2(6) . . ? C54 O8 C53 119.7(10) . . ? C54 O8 Ag 123.0(7) . . ? C53 O8 Ag 111.8(6) . . ? F26 C32 C33 119.1(6) . . ? F26 C32 C31 119.0(5) . . ? C33 C32 C31 121.9(6) . . ? F13 C16 C15 121.4(6) . . ? F13 C16 C17 120.2(6) . . ? C15 C16 C17 118.4(6) . . ? F2 C3 C4 119.1(5) . . ? F2 C3 C2 119.5(5) . . ? C4 C3 C2 121.5(5) . . ? C38 C37 C42 114.9(10) . . ? C38 C37 Ag 86.4(8) . . ? C42 C37 Ag 89.0(7) . . ? C38 C37 H37 122.6 . . ? C42 C37 H37 122.6 . . ? Ag C37 H37 94.3 . . ? O2 C7 C8 122.4(5) . . ? O2 C7 C12 121.4(6) . . ? C8 C7 C12 116.2(6) . . ? C48 C47 C46 112.4(11) . . ? C48 C47 H47 123.8 . . ? C46 C47 H47 123.8 . . ? F21 C26 C27 119.5(7) . . ? F21 C26 C25 120.2(6) . . ? C27 C26 C25 120.2(7) . . ? F9 C11 C10 120.5(7) . . ? F9 C11 C12 118.2(8) . . ? C10 C11 C12 121.3(6) . . ? F19 C23 C22 118.8(7) . . ? F19 C23 C24 120.4(6) . . ? C22 C23 C24 120.8(7) . . ? C44 C49 C48 114.4(11) . . ? C44 C49 Ag 65.1(6) . . ? C48 C49 Ag 98.2(6) . . ? C44 C49 H49 122.8 . . ? C48 C49 H49 122.8 . . ? Ag C49 H49 104.9 . . ? F27 C33 C34 119.0(6) . . ? F27 C33 C32 120.2(6) . . ? C34 C33 C32 120.8(6) . . ? F20 C24 C23 119.4(6) . . ? F20 C24 C19 120.2(6) . . ? C23 C24 C19 120.5(6) . . ? O1 C1 C2 121.7(6) . . ? O1 C1 C6 122.1(5) . . ? C2 C1 C6 116.2(5) . . ? O5 C25 C26 120.4(6) . . ? O5 C25 C30 122.7(6) . . ? C26 C25 C30 116.9(6) . . ? O6 C31 C32 122.0(6) . . ? O6 C31 C36 121.5(6) . . ? C32 C31 C36 116.5(6) . . ? F14 C17 C18 120.6(6) . . ? F14 C17 C16 119.4(6) . . ? C18 C17 C16 120.0(6) . . ? C40 C41 C42 121.5(10) . . ? C40 C41 H41 119.3 . . ? C42 C41 H41 119.3 . . ? C28 C29 F24 118.7(8) . . ? C28 C29 C30 120.9(7) . . ? F24 C29 C30 120.4(8) . . ? F16 C20 C21 119.8(7) . . ? F16 C20 C19 117.8(8) . . ? C21 C20 C19 122.4(6) . . ? F6 C8 C7 119.0(5) . . ? F6 C8 C9 118.2(6) . . ? C7 C8 C9 122.7(6) . . ? C49 C44 C45 127.8(13) . . ? C49 C44 Ag 84.9(7) . . ? C45 C44 Ag 90.0(7) . . ? C49 C44 H44 116.1 . . ? C45 C44 H44 116.1 . . ? Ag C44 H44 95.8 . . ? C39 C40 C41 120.4(9) . . ? C39 C40 C43 117.1(12) . . ? C41 C40 C43 122.6(12) . . ? F25 C30 C29 119.3(7) . . ? F25 C30 C25 118.7(6) . . ? C29 C30 C25 122.0(7) . . ? O4 C19 C20 123.4(7) . . ? O4 C19 C24 120.2(6) . . ? C20 C19 C24 116.4(7) . . ? F7 C9 C10 119.8(6) . . ? F7 C9 C8 120.6(6) . . ? C10 C9 C8 119.6(7) . . ? C40 C39 C38 121.3(12) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C29 C28 F23 122.2(9) . . ? C29 C28 C27 119.4(7) . . ? F23 C28 C27 118.4(10) . . ? C41 C42 C37 120.1(11) . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? F10 C12 C11 120.3(6) . . ? F10 C12 C7 118.7(6) . . ? C11 C12 C7 121.0(7) . . ? C45 C46 C47 134.6(11) . . ? C45 C46 H46 112.7 . . ? C47 C46 H46 112.7 . . ? C39 C38 C37 121.9(13) . . ? C39 C38 Ag 100.8(6) . . ? C37 C38 Ag 63.6(7) . . ? C39 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? Ag C38 H38 105.3 . . ? F22 C27 C26 119.2(9) . . ? F22 C27 C28 120.3(8) . . ? C26 C27 C28 120.5(8) . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C46 C45 C44 106.6(13) . . ? C46 C45 H45 126.7 . . ? C44 C45 H45 126.7 . . ? C21 C22 C23 120.5(7) . . ? C21 C22 F18 120.6(7) . . ? C23 C22 F18 118.9(7) . . ? C22 C21 F17 121.1(8) . . ? C22 C21 C20 119.4(7) . . ? F17 C21 C20 119.4(7) . . ? O8 C54 H54A 109.5 . . ? O8 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O8 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O8 C53 C52 107.1(9) . . ? O8 C53 H53A 110.3 . . ? C52 C53 H53A 110.3 . . ? O8 C53 H53B 110.3 . . ? C52 C53 H53B 110.3 . . ? H53A C53 H53B 108.5 . . ? C52 O7 C51 109.5(15) . . ? C52 O7 Ag 118.7(13) . . ? C51 O7 Ag 116.6(14) . . ? O7 C52 C53 103.0(10) . . ? O7 C52 H52A 111.2 . . ? C53 C52 H52A 111.2 . . ? O7 C52 H52B 111.2 . . ? C53 C52 H52B 111.2 . . ? H52A C52 H52B 109.1 . . ? O7 C51 H51A 109.5 . . ? O7 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O7 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C47 C48 C49 123.8(11) . . ? C47 C48 C50 119.2(8) . . ? C49 C48 C50 116.7(9) . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 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 O1 U1 O3 C13 13.9(7) 2_775 . . . ? O1 U1 O3 C13 -166.1(7) . . . . ? O2 U1 O3 C13 -76.1(7) 2_775 . . . ? O2 U1 O3 C13 103.9(7) . . . . ? O3 U1 O3 C13 114(100) 2_775 . . . ? O5 U2 O4 C19 -101.0(9) . . . . ? O5 U2 O4 C19 79.0(9) 2_556 . . . ? O6 U2 O4 C19 -9.6(9) 2_556 . . . ? O6 U2 O4 C19 170.4(9) . . . . ? O4 U2 O4 C19 -116(100) 2_556 . . . ? O5 U2 O6 C31 -21.8(13) . . . . ? O5 U2 O6 C31 158.2(13) 2_556 . . . ? O6 U2 O6 C31 52(68) 2_556 . . . ? O4 U2 O6 C31 -110.8(13) 2_556 . . . ? O4 U2 O6 C31 69.2(13) . . . . ? F12 C15 C14 F11 1.9(8) . . . . ? C16 C15 C14 F11 -178.0(5) . . . . ? F12 C15 C14 C13 178.9(5) . . . . ? C16 C15 C14 C13 -1.0(9) . . . . ? O1 U1 O1 C1 -171(100) 2_775 . . . ? O2 U1 O1 C1 -89(2) 2_775 . . . ? O2 U1 O1 C1 91(2) . . . . ? O3 U1 O1 C1 -1(2) . . . . ? O3 U1 O1 C1 179(100) 2_775 . . . ? O1 U1 O2 C7 174.1(11) 2_775 . . . ? O1 U1 O2 C7 -5.9(11) . . . . ? O2 U1 O2 C7 -83(100) 2_775 . . . ? O3 U1 O2 C7 85.5(11) . . . . ? O3 U1 O2 C7 -94.5(11) 2_775 . . . ? F4 C5 C6 F5 2.1(9) . . . . ? C4 C5 C6 F5 -177.0(6) . . . . ? F4 C5 C6 C1 179.3(6) . . . . ? C4 C5 C6 C1 0.2(10) . . . . ? F30 C36 C35 F29 -0.6(9) . . . . ? C31 C36 C35 F29 -179.3(6) . . . . ? F30 C36 C35 C34 179.2(6) . . . . ? C31 C36 C35 C34 0.5(10) . . . . ? O5 U2 O5 C25 -90(100) 2_556 . . . ? O6 U2 O5 C25 91.5(12) 2_556 . . . ? O6 U2 O5 C25 -88.5(12) . . . . ? O4 U2 O5 C25 -0.5(12) 2_556 . . . ? O4 U2 O5 C25 179.5(12) . . . . ? U1 O3 C13 C18 100.2(8) . . . . ? U1 O3 C13 C14 -80.3(8) . . . . ? F11 C14 C13 O3 -1.4(8) . . . . ? C15 C14 C13 O3 -178.5(5) . . . . ? F11 C14 C13 C18 178.1(5) . . . . ? C15 C14 C13 C18 1.1(8) . . . . ? F29 C35 C34 F28 -1.4(10) . . . . ? C36 C35 C34 F28 178.8(6) . . . . ? F29 C35 C34 C33 -179.7(6) . . . . ? C36 C35 C34 C33 0.5(10) . . . . ? F4 C5 C4 F3 -0.2(9) . . . . ? C6 C5 C4 F3 178.9(6) . . . . ? F4 C5 C4 C3 -178.6(6) . . . . ? C6 C5 C4 C3 0.6(10) . . . . ? O3 C13 C18 F15 -0.5(9) . . . . ? C14 C13 C18 F15 180.0(5) . . . . ? O3 C13 C18 C17 -179.9(6) . . . . ? C14 C13 C18 C17 0.6(9) . . . . ? O7 Ag O8 C54 165.2(9) . . . . ? C37 Ag O8 C54 -84.3(10) . . . . ? C44 Ag O8 C54 60.8(9) . . . . ? C38 Ag O8 C54 -112.0(9) . . . . ? C49 Ag O8 C54 97.1(9) . . . . ? O7 Ag O8 C53 11.5(6) . . . . ? C37 Ag O8 C53 122.0(8) . . . . ? C44 Ag O8 C53 -93.0(7) . . . . ? C38 Ag O8 C53 94.3(7) . . . . ? C49 Ag O8 C53 -56.6(7) . . . . ? F12 C15 C16 F13 1.9(9) . . . . ? C14 C15 C16 F13 -178.2(6) . . . . ? F12 C15 C16 C17 179.4(6) . . . . ? C14 C15 C16 C17 -0.7(9) . . . . ? F3 C4 C3 F2 0.7(9) . . . . ? C5 C4 C3 F2 179.0(6) . . . . ? F3 C4 C3 C2 179.9(6) . . . . ? C5 C4 C3 C2 -1.8(10) . . . . ? F1 C2 C3 F2 -0.6(9) . . . . ? C1 C2 C3 F2 -178.5(5) . . . . ? F1 C2 C3 C4 -179.8(6) . . . . ? C1 C2 C3 C4 2.3(10) . . . . ? O8 Ag C37 C38 -65.8(11) . . . . ? O7 Ag C37 C38 11.0(11) . . . . ? C44 Ag C37 C38 144.8(9) . . . . ? C49 Ag C37 C38 112.9(8) . . . . ? O8 Ag C37 C42 49.2(10) . . . . ? O7 Ag C37 C42 126.0(9) . . . . ? C44 Ag C37 C42 -100.2(7) . . . . ? C38 Ag C37 C42 115.0(10) . . . . ? C49 Ag C37 C42 -132.1(6) . . . . ? U1 O2 C7 C8 45.5(14) . . . . ? U1 O2 C7 C12 -134.6(9) . . . . ? F8 C10 C11 F9 0.6(11) . . . . ? C9 C10 C11 F9 -178.6(6) . . . . ? F8 C10 C11 C12 179.2(6) . . . . ? C9 C10 C11 C12 0.0(11) . . . . ? O8 Ag C49 C44 -101.3(8) . . . . ? O7 Ag C49 C44 -160.4(8) . . . . ? C37 Ag C49 C44 80.2(10) . . . . ? C38 Ag C49 C44 115.4(9) . . . . ? O8 Ag C49 C48 11.9(8) . . . . ? O7 Ag C49 C48 -47.2(8) . . . . ? C37 Ag C49 C48 -166.6(9) . . . . ? C44 Ag C49 C48 113.2(11) . . . . ? C38 Ag C49 C48 -131.4(8) . . . . ? F28 C34 C33 F27 1.5(10) . . . . ? C35 C34 C33 F27 179.7(6) . . . . ? F28 C34 C33 C32 -179.5(6) . . . . ? C35 C34 C33 C32 -1.3(10) . . . . ? F26 C32 C33 F27 0.1(9) . . . . ? C31 C32 C33 F27 -179.9(6) . . . . ? F26 C32 C33 C34 -178.9(6) . . . . ? C31 C32 C33 C34 1.1(10) . . . . ? F19 C23 C24 F20 -1.1(10) . . . . ? C22 C23 C24 F20 -179.9(7) . . . . ? F19 C23 C24 C19 179.9(6) . . . . ? C22 C23 C24 C19 1.0(11) . . . . ? U1 O1 C1 C2 121.0(19) . . . . ? U1 O1 C1 C6 -58(2) . . . . ? F1 C2 C1 O1 1.8(9) . . . . ? C3 C2 C1 O1 179.7(5) . . . . ? F1 C2 C1 C6 -179.3(5) . . . . ? C3 C2 C1 C6 -1.4(9) . . . . ? F5 C6 C1 O1 -3.6(9) . . . . ? C5 C6 C1 O1 179.1(6) . . . . ? F5 C6 C1 C2 177.5(5) . . . . ? C5 C6 C1 C2 0.2(9) . . . . ? U2 O5 C25 C26 113.1(11) . . . . ? U2 O5 C25 C30 -66.5(14) . . . . ? F21 C26 C25 O5 -1.1(9) . . . . ? C27 C26 C25 O5 -178.7(6) . . . . ? F21 C26 C25 C30 178.5(6) . . . . ? C27 C26 C25 C30 0.9(9) . . . . ? U2 O6 C31 C32 79.2(14) . . . . ? U2 O6 C31 C36 -100.0(13) . . . . ? F26 C32 C31 O6 0.7(9) . . . . ? C33 C32 C31 O6 -179.3(6) . . . . ? F26 C32 C31 C36 180.0(5) . . . . ? C33 C32 C31 C36 -0.1(9) . . . . ? F30 C36 C31 O6 -0.2(9) . . . . ? C35 C36 C31 O6 178.5(6) . . . . ? F30 C36 C31 C32 -179.4(5) . . . . ? C35 C36 C31 C32 -0.7(9) . . . . ? F15 C18 C17 F14 -0.1(10) . . . . ? C13 C18 C17 F14 179.3(6) . . . . ? F15 C18 C17 C16 178.3(6) . . . . ? C13 C18 C17 C16 -2.3(10) . . . . ? F13 C16 C17 F14 -1.8(10) . . . . ? C15 C16 C17 F14 -179.3(6) . . . . ? F13 C16 C17 C18 179.8(6) . . . . ? C15 C16 C17 C18 2.3(10) . . . . ? O2 C7 C8 F6 0.8(10) . . . . ? C12 C7 C8 F6 -179.0(6) . . . . ? O2 C7 C8 C9 -179.1(6) . . . . ? C12 C7 C8 C9 1.1(10) . . . . ? C48 C49 C44 C45 -1.8(17) . . . . ? Ag C49 C44 C45 86.0(11) . . . . ? C48 C49 C44 Ag -87.8(9) . . . . ? O8 Ag C44 C49 99.5(7) . . . . ? O7 Ag C44 C49 21.5(9) . . . . ? C37 Ag C44 C49 -114.0(9) . . . . ? C38 Ag C44 C49 -90.4(9) . . . . ? O8 Ag C44 C45 -28.5(9) . . . . ? O7 Ag C44 C45 -106.5(7) . . . . ? C37 Ag C44 C45 118.0(9) . . . . ? C38 Ag C44 C45 141.6(7) . . . . ? C49 Ag C44 C45 -128.0(12) . . . . ? C42 C41 C40 C39 -0.7(14) . . . . ? C42 C41 C40 C43 179.7(9) . . . . ? C28 C29 C30 F25 -178.7(7) . . . . ? F24 C29 C30 F25 0.1(10) . . . . ? C28 C29 C30 C25 1.2(11) . . . . ? F24 C29 C30 C25 -180.0(6) . . . . ? O5 C25 C30 F25 -1.6(10) . . . . ? C26 C25 C30 F25 178.8(6) . . . . ? O5 C25 C30 C29 178.5(6) . . . . ? C26 C25 C30 C29 -1.1(9) . . . . ? U2 O4 C19 C20 73.6(11) . . . . ? U2 O4 C19 C24 -108.1(8) . . . . ? F16 C20 C19 O4 0.3(9) . . . . ? C21 C20 C19 O4 -179.9(6) . . . . ? F16 C20 C19 C24 -178.1(5) . . . . ? C21 C20 C19 C24 1.7(9) . . . . ? F20 C24 C19 O4 1.2(9) . . . . ? C23 C24 C19 O4 -179.8(6) . . . . ? F20 C24 C19 C20 179.6(6) . . . . ? C23 C24 C19 C20 -1.3(9) . . . . ? F8 C10 C9 F7 -1.5(10) . . . . ? C11 C10 C9 F7 177.7(7) . . . . ? F8 C10 C9 C8 179.8(6) . . . . ? C11 C10 C9 C8 -0.9(11) . . . . ? F6 C8 C9 F7 1.8(10) . . . . ? C7 C8 C9 F7 -178.3(6) . . . . ? F6 C8 C9 C10 -179.5(6) . . . . ? C7 C8 C9 C10 0.4(11) . . . . ? C41 C40 C39 C38 -0.6(14) . . . . ? C43 C40 C39 C38 179.0(9) . . . . ? F24 C29 C28 F23 0.8(12) . . . . ? C30 C29 C28 F23 179.6(7) . . . . ? F24 C29 C28 C27 -179.9(7) . . . . ? C30 C29 C28 C27 -1.0(12) . . . . ? C40 C41 C42 C37 1.2(15) . . . . ? C38 C37 C42 C41 -0.5(15) . . . . ? Ag C37 C42 C41 -86.0(9) . . . . ? F9 C11 C12 F10 0.6(11) . . . . ? C10 C11 C12 F10 -178.0(7) . . . . ? F9 C11 C12 C7 -179.8(6) . . . . ? C10 C11 C12 C7 1.6(11) . . . . ? O2 C7 C12 F10 -2.3(10) . . . . ? C8 C7 C12 F10 177.6(6) . . . . ? O2 C7 C12 C11 178.1(6) . . . . ? C8 C7 C12 C11 -2.0(10) . . . . ? C48 C47 C46 C45 -2.6(19) . . . . ? C40 C39 C38 C37 1.3(16) . . . . ? C40 C39 C38 Ag 66.9(11) . . . . ? C42 C37 C38 C39 -0.7(16) . . . . ? Ag C37 C38 C39 86.5(10) . . . . ? C42 C37 C38 Ag -87.2(9) . . . . ? O8 Ag C38 C39 3.1(11) . . . . ? O7 Ag C38 C39 69.4(10) . . . . ? C37 Ag C38 C39 -120.4(14) . . . . ? C44 Ag C38 C39 -168.6(8) . . . . ? C49 Ag C38 C39 152.6(8) . . . . ? O8 Ag C38 C37 123.4(10) . . . . ? O7 Ag C38 C37 -170.3(10) . . . . ? C44 Ag C38 C37 -48.3(11) . . . . ? C49 Ag C38 C37 -87.1(10) . . . . ? F21 C26 C27 F22 0.2(10) . . . . ? C25 C26 C27 F22 177.8(6) . . . . ? F21 C26 C27 C28 -178.4(7) . . . . ? C25 C26 C27 C28 -0.8(11) . . . . ? C29 C28 C27 F22 -177.8(7) . . . . ? F23 C28 C27 F22 1.6(12) . . . . ? C29 C28 C27 C26 0.8(12) . . . . ? F23 C28 C27 C26 -179.8(7) . . . . ? C47 C46 C45 C44 5.4(18) . . . . ? C49 C44 C45 C46 -2.8(16) . . . . ? Ag C44 C45 C46 80.7(8) . . . . ? F19 C23 C22 C21 -179.8(7) . . . . ? C24 C23 C22 C21 -0.9(12) . . . . ? F19 C23 C22 F18 1.4(11) . . . . ? C24 C23 C22 F18 -179.7(7) . . . . ? C23 C22 C21 F17 179.1(7) . . . . ? F18 C22 C21 F17 -2.2(11) . . . . ? C23 C22 C21 C20 1.3(11) . . . . ? F18 C22 C21 C20 180.0(6) . . . . ? F16 C20 C21 C22 178.1(6) . . . . ? C19 C20 C21 C22 -1.7(11) . . . . ? F16 C20 C21 F17 0.2(10) . . . . ? C19 C20 C21 F17 -179.6(6) . . . . ? C54 O8 C53 C52 165.6(12) . . . . ? Ag O8 C53 C52 -39.7(13) . . . . ? O8 Ag O7 C52 27.6(13) . . . . ? C37 Ag O7 C52 -81.2(14) . . . . ? C44 Ag O7 C52 146.2(13) . . . . ? C38 Ag O7 C52 -75.8(14) . . . . ? C49 Ag O7 C52 156.8(13) . . . . ? O8 Ag O7 C51 162.0(9) . . . . ? C37 Ag O7 C51 53.2(9) . . . . ? C44 Ag O7 C51 -79.4(9) . . . . ? C38 Ag O7 C51 58.6(8) . . . . ? C49 Ag O7 C51 -68.8(8) . . . . ? C51 O7 C52 C53 167.9(13) . . . . ? Ag O7 C52 C53 -54.8(16) . . . . ? O8 C53 C52 O7 60.6(18) . . . . ? C46 C47 C48 C49 -3.6(17) . . . . ? C46 C47 C48 C50 -177.6(11) . . . . ? C44 C49 C48 C47 5.4(17) . . . . ? Ag C49 C48 C47 -60.9(12) . . . . ? C44 C49 C48 C50 179.4(11) . . . . ? Ag C49 C48 C50 113.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.534 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.115