data_p21n_all_a _vrf_PLAT088_p21n_all_a ; PROBLEM: Poor Data / Parameter Ratio .................... 4.14 Note RESPONSE: The disorder of the anion requires the parameters used to keep the model stable. ; _vrf_PLAT307_p21n_all_a ; PROBLEM: Isolated Metal Atom found in Structure (Unusual) Ta1B Check RESPONSE: The cation is disordered, but only the position of the tantalum atom can be assigned. ; _vrf_PLAT077_p21n_all_a ; PROBLEM: Unitcell Contains Non-integer Number of Atoms .. Please Check RESPONSE: rounding errors ; _vrf_PLAT029_p21n_all_a ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.814 Why? RESPONSE: Caused by disorder. ; _vrf_PLAT230_p21n_all_a ; PROBLEM: Hirshfeld Test Diff for F2B --C2A . 11.5 s.u. RESPONSE: Caused by disorder. ; _vrf_PLAT911_p21n_all_a ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.597 637 Report RESPONSE: Caused by disorder. ; _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H4 Al F38 O8 Ta1.08' _chemical_formula_weight 1388.70 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' '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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ta' 'Ta' -0.7052 6.5227 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0435(6) _cell_length_b 18.7956(8) _cell_length_c 15.9397(7) _cell_angle_alpha 90 _cell_angle_beta 94.046(2) _cell_angle_gamma 90 _cell_volume 3898.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9990 _cell_measurement_theta_min 4.464 _cell_measurement_theta_max 50.173 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.366 _exptl_crystal_F_000 2631 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_absorpt_coefficient_mu 3.296 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6001 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'INCOATEC Mo Microsource' _diffrn_measurement_device_type 'Bruker Smart Apex II Quazar' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11830 _diffrn_reflns_av_unetI/netI 0.0286 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.678 _diffrn_reflns_theta_max 25.100 _diffrn_reflns_theta_full 25.100 _diffrn_measured_fraction_theta_max 0.814 _diffrn_measured_fraction_theta_full 0.814 _diffrn_reflns_Laue_measured_fraction_max 0.814 _diffrn_reflns_Laue_measured_fraction_full 0.814 _diffrn_reflns_point_group_measured_fraction_max 0.814 _diffrn_reflns_point_group_measured_fraction_full 0.814 _reflns_number_total 5664 _reflns_number_gt 4981 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Apex2 v2013.6-2' _computing_cell_refinement 'SAINT V8.34A' _computing_data_reduction 'SAINT V8.34A' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'OLEX2 v1.2' _computing_publication_material 'ShelXle-915' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+55.5953P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5664 _refine_ls_number_parameters 1368 _refine_ls_number_restraints 16241 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 0.646 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1_12 O 0.242(5) 0.3489(19) 0.633(3) 0.030(7) Uani 0.113(3) 1 d D U P A 3 C1_12 C 0.240(3) 0.3019(13) 0.570(2) 0.034(5) Uani 0.113(3) 1 d D U P A 3 C2_12 C 0.245(3) 0.2246(15) 0.605(2) 0.044(8) Uani 0.113(3) 1 d D U P A 3 F1_12 F 0.339(4) 0.207(3) 0.633(4) 0.061(13) Uani 0.113(3) 1 d D U P A 3 F2_12 F 0.213(5) 0.1790(19) 0.544(3) 0.076(16) Uani 0.113(3) 1 d D U P A 3 F3_12 F 0.183(5) 0.217(3) 0.667(3) 0.053(12) Uani 0.113(3) 1 d D U P A 3 C3_12 C 0.139(3) 0.309(2) 0.513(3) 0.062(9) Uani 0.113(3) 1 d D U P A 3 F4_12 F 0.112(4) 0.376(2) 0.500(4) 0.075(14) Uani 0.113(3) 1 d D U P A 3 F5_12 F 0.065(3) 0.275(4) 0.549(4) 0.087(15) Uani 0.113(3) 1 d D U P A 3 F6_12 F 0.151(5) 0.279(4) 0.439(3) 0.083(15) Uani 0.113(3) 1 d D U P A 3 C4_12 C 0.331(3) 0.313(2) 0.514(2) 0.036(7) Uani 0.113(3) 1 d D U P A 3 F7_12 F 0.314(5) 0.371(3) 0.465(4) 0.054(14) Uani 0.113(3) 1 d D U P A 3 F8_12 F 0.342(5) 0.258(3) 0.463(3) 0.060(14) Uani 0.113(3) 1 d D U P A 3 F9_12 F 0.419(3) 0.323(4) 0.559(3) 0.059(13) Uani 0.113(3) 1 d D U P A 3 O1_11 O 0.3901(19) 0.423(3) 0.727(3) 0.032(10) Uani 0.056(3) 1 d D U P A 3 C1_11 C 0.439(3) 0.410(2) 0.803(3) 0.033(6) Uani 0.056(3) 1 d D U P A 3 C2_11 C 0.547(3) 0.445(3) 0.808(3) 0.042(10) Uani 0.056(3) 1 d D U P A 3 F1_11 F 0.614(4) 0.405(4) 0.772(6) 0.043(13) Uani 0.056(3) 1 d D U P A 3 F2_11 F 0.579(5) 0.456(5) 0.888(4) 0.051(17) Uani 0.056(3) 1 d D U P A 3 F3_11 F 0.542(6) 0.508(3) 0.769(6) 0.047(16) Uani 0.056(3) 1 d D U P A 3 C3_11 C 0.378(4) 0.443(3) 0.873(3) 0.043(10) Uani 0.056(3) 1 d D U P A 3 F4_11 F 0.278(4) 0.442(5) 0.852(5) 0.068(17) Uani 0.056(3) 1 d D U P A 3 F5_11 F 0.407(7) 0.510(3) 0.885(5) 0.043(15) Uani 0.056(3) 1 d D U P A 3 F6_11 F 0.395(7) 0.409(5) 0.946(4) 0.044(17) Uani 0.056(3) 1 d D U P A 3 C4_11 C 0.449(4) 0.328(2) 0.815(3) 0.036(6) Uani 0.056(3) 1 d D U P A 3 F7_11 F 0.360(5) 0.301(3) 0.835(6) 0.050(2) Uani 0.056(3) 1 d D U P A 3 F8_11 F 0.520(6) 0.311(3) 0.875(4) 0.040(12) Uani 0.056(3) 1 d D U P A 3 F9_11 F 0.473(6) 0.297(3) 0.744(4) 0.033(6) Uani 0.056(3) 1 d D U P A 3 O1_10 O 0.275(4) 0.4936(16) 0.618(2) 0.0261(19) Uani 0.135(9) 1 d D U P A 2 C1_10 C 0.269(2) 0.5611(14) 0.5903(15) 0.0220(17) Uani 0.135(9) 1 d D U P A 2 C2_10 C 0.172(2) 0.5675(17) 0.5290(18) 0.036(5) Uani 0.135(9) 1 d D U P A 2 F1_10 F 0.190(4) 0.536(3) 0.457(2) 0.060(11) Uani 0.135(9) 1 d D U P A 2 F2_10 F 0.145(3) 0.6348(17) 0.516(3) 0.049(2) Uani 0.135(9) 1 d D U P A 2 F3_10 F 0.094(3) 0.534(3) 0.562(3) 0.042(11) Uani 0.135(9) 1 d D U P A 2 C3_10 C 0.261(3) 0.6156(18) 0.6621(19) 0.039(7) Uani 0.135(9) 1 d D U P A 2 F4_10 F 0.332(4) 0.603(3) 0.724(2) 0.067(13) Uani 0.135(9) 1 d D U P A 2 F5_10 F 0.168(3) 0.615(3) 0.690(3) 0.054(13) Uani 0.135(9) 1 d D U P A 2 F6_10 F 0.277(5) 0.6814(17) 0.634(3) 0.066(13) Uani 0.135(9) 1 d D U P A 2 C4_10 C 0.366(3) 0.5781(18) 0.543(2) 0.039(7) Uani 0.135(9) 1 d D U P A 2 F7_10 F 0.443(3) 0.597(3) 0.598(3) 0.049(13) Uani 0.135(9) 1 d D U P A 2 F8_10 F 0.350(5) 0.631(3) 0.488(3) 0.049(13) Uani 0.135(9) 1 d D U P A 2 F9_10 F 0.395(4) 0.521(2) 0.502(3) 0.056(13) Uani 0.135(9) 1 d D U P A 2 O1_8 O 0.3047(7) 0.5011(3) 0.6355(5) 0.0261(19) Uani 0.865(9) 1 d D U P A 1 C1_8 C 0.2798(7) 0.5607(4) 0.5900(5) 0.0220(17) Uani 0.865(9) 1 d D U P A 1 C2_8 C 0.3717(8) 0.5770(5) 0.5357(6) 0.035(2) Uani 0.865(9) 1 d D U P A 1 F1_8 F 0.3713(7) 0.5330(4) 0.4704(5) 0.045(2) Uani 0.865(9) 1 d D U P A 1 F2_8 F 0.3688(8) 0.6442(4) 0.5074(6) 0.045(3) Uani 0.865(9) 1 d D U P A 1 F3_8 F 0.4604(7) 0.5703(5) 0.5814(6) 0.043(2) Uani 0.865(9) 1 d D U P A 1 C3_8 C 0.2638(8) 0.6231(5) 0.6504(6) 0.036(2) Uani 0.865(9) 1 d D U P A 1 F4_8 F 0.2034(7) 0.6038(4) 0.7099(5) 0.041(2) Uani 0.865(9) 1 d D U P A 1 F5_8 F 0.3536(6) 0.6445(3) 0.6874(5) 0.0413(19) Uani 0.865(9) 1 d D U P A 1 F6_8 F 0.2203(7) 0.6790(3) 0.6105(5) 0.046(2) Uani 0.865(9) 1 d D U P A 1 C4_8 C 0.1815(8) 0.5506(5) 0.5314(6) 0.034(2) Uani 0.865(9) 1 d D U P A 1 F7_8 F 0.0978(7) 0.5562(5) 0.5745(7) 0.046(3) Uani 0.865(9) 1 d D U P A 1 F8_8 F 0.1727(6) 0.5997(4) 0.4697(4) 0.049(2) Uani 0.865(9) 1 d D U P A 1 F9_8 F 0.1813(6) 0.4872(4) 0.4938(4) 0.049(2) Uani 0.865(9) 1 d D U P A 1 O1_9 O 0.162(2) 0.4467(18) 0.744(2) 0.0325(16) Uani 0.406(7) 1 d D U P A 2 C1_9 C 0.0826(13) 0.4296(8) 0.7892(9) 0.0250(18) Uani 0.406(7) 1 d D U P A 2 C2_9 C 0.0664(14) 0.4909(9) 0.8516(10) 0.037(4) Uani 0.406(7) 1 d D U P A 2 F1_9 F 0.1553(12) 0.5108(9) 0.8899(9) 0.053(2) Uani 0.406(7) 1 d D U P A 2 F2_9 F 0.0061(17) 0.4732(13) 0.9121(12) 0.069(6) Uani 0.406(7) 1 d D U P A 2 F3_9 F 0.0255(18) 0.5468(10) 0.8107(14) 0.058(6) Uani 0.406(7) 1 d D U P A 2 C3_9 C -0.0139(14) 0.4191(9) 0.7283(11) 0.045(4) Uani 0.406(7) 1 d D U P A 2 F4_9 F -0.0089(14) 0.3567(8) 0.6883(10) 0.063(5) Uani 0.406(7) 1 d D U P A 2 F5_9 F -0.0244(18) 0.4716(11) 0.6726(13) 0.065(7) Uani 0.406(7) 1 d D U P A 2 F6_9 F -0.0993(13) 0.4172(11) 0.7677(11) 0.050(3) Uani 0.406(7) 1 d D U P A 2 C4_9 C 0.1033(14) 0.3595(9) 0.8389(10) 0.033(4) Uani 0.406(7) 1 d D U P A 2 F7_9 F 0.1448(18) 0.3120(7) 0.7900(10) 0.063(6) Uani 0.406(7) 1 d D U P A 2 F8_9 F 0.017(2) 0.332(2) 0.865(2) 0.052(9) Uani 0.406(7) 1 d D U P A 2 F9_9 F 0.1672(11) 0.3702(8) 0.9057(8) 0.042(4) Uani 0.406(7) 1 d D U P A 2 O1_7 O 0.373(2) 0.401(2) 0.750(2) 0.030(2) Uani 0.219(3) 1 d D U P A 2 C1_7 C 0.4503(16) 0.4137(11) 0.8092(14) 0.029(4) Uani 0.219(3) 1 d D U P A 2 C2_7 C 0.4304(19) 0.3716(13) 0.8900(14) 0.035(6) Uani 0.219(3) 1 d D U P A 2 F1_7 F 0.357(2) 0.4014(18) 0.9320(16) 0.055(8) Uani 0.219(3) 1 d D U P A 2 F2_7 F 0.512(2) 0.365(2) 0.945(2) 0.042(9) Uani 0.219(3) 1 d D U P A 2 F3_7 F 0.398(3) 0.3067(14) 0.867(2) 0.053(9) Uani 0.219(3) 1 d D U P A 2 C3_7 C 0.5549(16) 0.3906(11) 0.7775(14) 0.033(5) Uani 0.219(3) 1 d D U P A 2 F4_7 F 0.565(3) 0.4135(19) 0.7001(15) 0.033(6) Uani 0.219(3) 1 d D U P A 2 F5_7 F 0.564(2) 0.3200(10) 0.7779(18) 0.038(6) Uani 0.219(3) 1 d D U P A 2 F6_7 F 0.633(2) 0.4167(17) 0.8266(19) 0.035(8) Uani 0.219(3) 1 d D U P A 2 C4_7 C 0.454(2) 0.4944(12) 0.8289(17) 0.041(5) Uani 0.219(3) 1 d D U P A 2 F7_7 F 0.495(2) 0.5294(12) 0.7667(18) 0.037(6) Uani 0.219(3) 1 d D U P A 2 F8_7 F 0.508(5) 0.509(3) 0.900(2) 0.051(11) Uani 0.219(3) 1 d D U P A 2 F9_7 F 0.359(3) 0.520(2) 0.836(4) 0.048(2) Uani 0.219(3) 1 d D U P A 2 O1_6 O 0.235(3) 0.3566(15) 0.621(2) 0.030(5) Uani 0.381(3) 1 d D U P A 2 C1_6 C 0.2621(13) 0.3007(10) 0.5743(10) 0.030(4) Uani 0.381(3) 1 d D U P A 2 C2_6 C 0.1897(16) 0.2977(10) 0.4931(10) 0.045(5) Uani 0.381(3) 1 d D U P A 2 F1_6 F 0.0928(17) 0.308(2) 0.510(2) 0.080(8) Uani 0.381(3) 1 d D U P A 2 F2_6 F 0.196(3) 0.2374(13) 0.4503(16) 0.070(8) Uani 0.381(3) 1 d D U P A 2 F3_6 F 0.2191(19) 0.3472(10) 0.4394(10) 0.063(6) Uani 0.381(3) 1 d D U P A 2 C3_6 C 0.3746(14) 0.3071(11) 0.5503(12) 0.039(4) Uani 0.381(3) 1 d D U P A 2 F4_6 F 0.4406(13) 0.2881(9) 0.6145(11) 0.044(4) Uani 0.381(3) 1 d D U P A 2 F5_6 F 0.394(3) 0.3738(13) 0.5296(19) 0.050(7) Uani 0.381(3) 1 d D U P A 2 F6_6 F 0.391(3) 0.2658(19) 0.4850(18) 0.046(8) Uani 0.381(3) 1 d D U P A 2 C4_6 C 0.2530(16) 0.2305(10) 0.6248(12) 0.047(5) Uani 0.381(3) 1 d D U P A 2 F7_6 F 0.297(2) 0.2391(18) 0.7021(12) 0.050(6) Uani 0.381(3) 1 d D U P A 2 F8_6 F 0.298(3) 0.1769(14) 0.587(3) 0.077(9) Uani 0.381(3) 1 d D U P A 2 F9_6 F 0.1550(15) 0.2127(12) 0.6290(13) 0.054(6) Uani 0.381(3) 1 d D U P A 2 O1_3 O 0.233(2) 0.3561(11) 0.6228(16) 0.028(4) Uani 0.506(3) 1 d D U P A 1 C1_3 C 0.2680(11) 0.3007(8) 0.5782(9) 0.030(3) Uani 0.506(3) 1 d D U P A 1 C2_3 C 0.1729(14) 0.2654(10) 0.5312(12) 0.076(5) Uani 0.506(3) 1 d D U P A 1 F1_3 F 0.1244(15) 0.2258(10) 0.5852(14) 0.101(7) Uani 0.506(3) 1 d D U P A 1 F2_3 F 0.200(2) 0.2225(14) 0.4705(16) 0.107(10) Uani 0.506(3) 1 d D U P A 1 F3_3 F 0.1096(16) 0.3144(13) 0.4964(15) 0.092(7) Uani 0.506(3) 1 d D U P A 1 C3_3 C 0.3446(12) 0.3265(8) 0.5153(9) 0.033(3) Uani 0.506(3) 1 d D U P A 1 F4_3 F 0.4091(18) 0.3730(10) 0.5535(14) 0.037(4) Uani 0.506(3) 1 d D U P A 1 F5_3 F 0.2931(16) 0.3590(11) 0.4515(10) 0.062(6) Uani 0.506(3) 1 d D U P A 1 F6_3 F 0.400(2) 0.2750(13) 0.4843(14) 0.039(5) Uani 0.506(3) 1 d D U P A 1 C4_3 C 0.3209(14) 0.2443(8) 0.6379(11) 0.050(4) Uani 0.506(3) 1 d D U P A 1 F7_3 F 0.4178(11) 0.2618(7) 0.6578(8) 0.055(4) Uani 0.506(3) 1 d D U P A 1 F8_3 F 0.323(2) 0.1801(10) 0.602(2) 0.083(8) Uani 0.506(3) 1 d D U P A 1 F9_3 F 0.270(2) 0.2387(17) 0.7068(13) 0.089(8) Uani 0.506(3) 1 d D U P A 1 O1_2 O 0.1603(14) 0.4460(12) 0.7417(16) 0.0325(16) Uani 0.594(7) 1 d D U P A 1 C1_2 C 0.0745(10) 0.4250(6) 0.7761(7) 0.0250(18) Uani 0.594(7) 1 d D U P A 1 C2_2 C 0.0574(11) 0.4744(7) 0.8513(8) 0.037(3) Uani 0.594(7) 1 d D U P A 1 F1_2 F 0.1200(9) 0.4570(6) 0.9173(6) 0.053(2) Uani 0.594(7) 1 d D U P A 1 F2_2 F -0.0377(9) 0.4701(7) 0.8761(8) 0.045(3) Uani 0.594(7) 1 d D U P A 1 F3_2 F 0.0755(12) 0.5417(6) 0.8318(9) 0.046(3) Uani 0.594(7) 1 d D U P A 1 C3_2 C -0.0158(10) 0.4335(7) 0.7080(8) 0.034(3) Uani 0.594(7) 1 d D U P A 1 F4_2 F 0.0094(9) 0.4065(6) 0.6347(6) 0.050(3) Uani 0.594(7) 1 d D U P A 1 F5_2 F -0.0388(12) 0.5017(5) 0.6948(8) 0.039(3) Uani 0.594(7) 1 d D U P A 1 F6_2 F -0.0998(9) 0.3997(7) 0.7267(8) 0.050(3) Uani 0.594(7) 1 d D U P A 1 C4_2 C 0.0810(11) 0.3464(7) 0.8066(9) 0.035(3) Uani 0.594(7) 1 d D U P A 1 F7_2 F 0.0698(9) 0.3017(5) 0.7424(7) 0.045(3) Uani 0.594(7) 1 d D U P A 1 F8_2 F 0.0097(15) 0.3310(12) 0.8593(14) 0.042(5) Uani 0.594(7) 1 d D U P A 1 F9_2 F 0.1721(8) 0.3332(6) 0.8456(9) 0.052(3) Uani 0.594(7) 1 d D U P A 1 O1_1 O 0.3654(9) 0.4001(8) 0.7570(8) 0.030(2) Uani 0.725(3) 1 d D U P A 1 C1_1 C 0.4461(8) 0.4194(5) 0.8101(6) 0.023(2) Uani 0.725(3) 1 d D U P A 1 C2_1 C 0.4777(10) 0.3543(6) 0.8663(7) 0.041(3) Uani 0.725(3) 1 d D U P A 1 F1_1 F 0.3969(9) 0.3205(6) 0.8919(7) 0.050(2) Uani 0.725(3) 1 d D U P A 1 F2_1 F 0.5359(10) 0.3746(8) 0.9350(8) 0.050(2) Uani 0.725(3) 1 d D U P A 1 F3_1 F 0.5301(9) 0.3081(5) 0.8237(7) 0.059(3) Uani 0.725(3) 1 d D U P A 1 C3_1 C 0.5383(8) 0.4419(6) 0.7602(6) 0.032(2) Uani 0.725(3) 1 d D U P A 1 F4_1 F 0.5241(9) 0.5089(5) 0.7326(6) 0.041(3) Uani 0.725(3) 1 d D U P A 1 F5_1 F 0.5458(13) 0.4016(7) 0.6940(7) 0.057(4) Uani 0.725(3) 1 d D U P A 1 F6_1 F 0.6271(8) 0.4400(6) 0.8071(7) 0.043(3) Uani 0.725(3) 1 d D U P A 1 C4_1 C 0.4170(10) 0.4812(6) 0.8683(7) 0.038(3) Uani 0.725(3) 1 d D U P A 1 F7_1 F 0.3620(11) 0.5302(7) 0.8242(10) 0.048(2) Uani 0.725(3) 1 d D U P A 1 F8_1 F 0.4973(15) 0.5144(9) 0.9055(8) 0.047(4) Uani 0.725(3) 1 d D U P A 1 F9_1 F 0.3601(8) 0.4576(6) 0.9281(5) 0.060(3) Uani 0.725(3) 1 d D U P A 1 Al1 Al 0.2650(2) 0.42627(12) 0.68786(14) 0.0177(6) Uani 1 1 d D . . . . Ta1B Ta 0.2476(5) 0.3200(3) 0.2172(4) 0.0322(15) Uani 0.08 1 d . U P B 2 Ta1 Ta 0.23398(4) 0.35036(3) 0.17632(3) 0.03066(19) Uani 1 1 d . U . C 1 C1A C 0.2981(11) 0.2360(6) 0.2352(7) 0.052(4) Uani 1 1 d . . . C 1 C2A C 0.3734(13) 0.2892(9) 0.2519(10) 0.074(6) Uani 1 1 d . . . C 1 C3A C 0.4154(10) 0.3307(8) 0.1873(9) 0.056(4) Uani 1 1 d . . . C 1 H3A H 0.466291 0.369796 0.199639 0.067 Uiso 1 1 calc R U . C 1 C4A C 0.3882(12) 0.3083(7) 0.1087(9) 0.062(4) Uani 1 1 d . . . C 1 H4A H 0.411798 0.337542 0.061286 0.075 Uiso 1 1 calc R U . C 1 C5A C 0.3084(11) 0.2607(6) 0.0898(7) 0.048(3) Uani 1 1 d . . . C 1 H5A H 0.281013 0.254871 0.029945 0.057 Uiso 1 1 calc R U . C 1 C6A C 0.2605(10) 0.2252(6) 0.1528(8) 0.050(3) Uani 1 1 d . . . C 1 H6A H 0.201178 0.192537 0.138969 0.060 Uiso 1 1 calc R U . C 1 F1B F 0.2633(7) 0.1996(4) 0.2974(5) 0.076(3) Uani 1 1 d . . . C 1 F2B F 0.4221(16) 0.3093(10) 0.3194(12) 0.196(8) Uani 1 1 d . . . C 1 C1B C 0.2381(9) 0.4446(6) 0.1040(6) 0.033(2) Uani 1 1 d . . . C 1 O1B O 0.2409(7) 0.4953(4) 0.0674(4) 0.050(2) Uani 1 1 d . . . C 1 C2B C 0.1018(10) 0.3502(6) 0.0942(6) 0.040(3) Uani 1 1 d . . . C 1 O2B O 0.0310(7) 0.3515(4) 0.0499(5) 0.052(2) Uani 1 1 d . . . C 1 C3B C 0.1077(11) 0.3419(5) 0.2540(7) 0.036(3) Uani 1 1 d . . . C 1 O3B O 0.0433(8) 0.3376(4) 0.2950(6) 0.046(2) Uani 1 1 d . . . C 1 C4B C 0.2503(8) 0.4313(5) 0.2652(5) 0.025(2) Uani 1 1 d . . . C 1 O4B O 0.2606(6) 0.4757(4) 0.3137(4) 0.040(2) Uani 1 1 d . . . C 1 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 O1_12 0.036(14) 0.022(11) 0.034(11) -0.008(11) 0.006(11) -0.007(12) C1_12 0.041(10) 0.025(9) 0.034(10) -0.009(8) -0.002(9) -0.001(9) C2_12 0.068(17) 0.022(10) 0.041(15) -0.011(10) 0.003(13) -0.003(12) F1_12 0.074(19) 0.07(3) 0.04(3) 0.03(3) 0.008(17) 0.006(19) F2_12 0.14(4) 0.030(18) 0.05(2) -0.021(19) -0.01(2) -0.02(3) F3_12 0.08(3) 0.03(2) 0.05(2) -0.002(19) 0.01(2) -0.01(2) C3_12 0.048(13) 0.072(18) 0.062(16) -0.004(14) -0.022(12) -0.008(14) F4_12 0.03(3) 0.08(2) 0.11(4) 0.01(2) -0.04(3) -0.001(18) F5_12 0.043(18) 0.11(3) 0.10(3) 0.03(3) -0.02(2) -0.01(2) F6_12 0.09(4) 0.09(3) 0.066(18) -0.02(2) -0.032(18) -0.04(3) C4_12 0.047(12) 0.032(14) 0.029(13) -0.011(11) 0.001(10) 0.003(12) F7_12 0.06(3) 0.052(19) 0.05(3) 0.010(19) 0.02(2) 0.02(2) F8_12 0.07(3) 0.051(18) 0.06(3) -0.033(19) 0.02(2) 0.00(2) F9_12 0.049(15) 0.08(3) 0.05(2) 0.00(2) -0.005(16) -0.01(2) O1_11 0.04(2) 0.02(2) 0.034(13) 0.010(15) -0.010(15) -0.010(19) C1_11 0.033(12) 0.033(9) 0.033(12) 0.006(10) -0.009(11) -0.003(9) C2_11 0.032(14) 0.036(17) 0.06(2) -0.001(19) -0.008(14) -0.004(13) F1_11 0.03(2) 0.03(2) 0.06(3) 0.00(3) 0.00(2) -0.01(2) F2_11 0.04(4) 0.05(4) 0.06(2) -0.01(2) -0.02(2) 0.01(3) F3_11 0.03(3) 0.04(2) 0.07(3) 0.01(3) 0.00(3) -0.003(18) C3_11 0.039(19) 0.051(18) 0.039(15) 0.009(16) -0.003(16) 0.011(17) F4_11 0.04(2) 0.08(4) 0.08(4) 0.03(4) -0.007(19) 0.01(2) F5_11 0.05(4) 0.052(19) 0.02(3) 0.005(18) 0.00(3) 0.01(2) F6_11 0.04(4) 0.06(3) 0.042(19) 0.01(3) 0.01(2) 0.02(3) C4_11 0.042(10) 0.032(11) 0.031(12) 0.009(11) -0.013(10) -0.004(10) F7_11 0.049(5) 0.049(4) 0.048(4) 0.025(3) -0.015(3) -0.014(4) F8_11 0.047(17) 0.04(3) 0.031(17) 0.01(2) -0.01(2) 0.00(2) F9_11 0.025(14) 0.037(12) 0.035(9) -0.001(8) -0.018(7) -0.010(12) O1_10 0.034(6) 0.017(3) 0.028(4) 0.008(3) 0.000(3) -0.004(3) C1_10 0.027(5) 0.014(3) 0.025(3) 0.004(2) 0.005(3) 0.000(3) C2_10 0.037(10) 0.044(9) 0.028(11) 0.016(8) -0.003(9) -0.012(8) F1_10 0.06(3) 0.09(2) 0.029(13) 0.001(17) -0.009(13) 0.00(2) F2_10 0.051(5) 0.048(4) 0.046(4) 0.023(3) -0.014(4) -0.013(4) F3_10 0.038(13) 0.05(2) 0.03(2) 0.02(2) -0.012(14) -0.025(17) C3_10 0.044(15) 0.032(10) 0.043(11) -0.014(10) 0.005(10) 0.004(12) F4_10 0.06(2) 0.09(3) 0.048(18) -0.022(18) -0.010(17) 0.00(2) F5_10 0.048(18) 0.07(3) 0.05(3) -0.02(2) 0.012(16) 0.006(18) F6_10 0.07(3) 0.025(11) 0.10(3) -0.019(14) 0.01(3) -0.006(18) C4_10 0.033(10) 0.044(13) 0.042(13) 0.018(10) 0.018(9) 0.007(10) F7_10 0.032(17) 0.07(3) 0.05(2) 0.029(19) 0.014(18) -0.01(2) F8_10 0.04(3) 0.06(2) 0.05(2) 0.030(19) 0.030(18) 0.02(2) F9_10 0.06(3) 0.063(17) 0.05(3) 0.013(18) 0.02(2) 0.032(19) O1_8 0.034(6) 0.017(3) 0.028(4) 0.008(3) 0.000(3) -0.004(3) C1_8 0.027(5) 0.014(3) 0.025(3) 0.004(2) 0.005(3) 0.000(3) C2_8 0.035(6) 0.040(5) 0.033(5) 0.010(4) 0.015(4) 0.004(5) F1_8 0.056(7) 0.049(4) 0.032(4) 0.002(3) 0.020(4) 0.004(4) F2_8 0.047(6) 0.036(4) 0.051(5) 0.019(3) 0.006(4) -0.009(3) F3_8 0.033(5) 0.047(5) 0.048(5) 0.014(4) 0.010(3) 0.005(4) C3_8 0.048(7) 0.025(5) 0.037(5) 0.000(4) 0.008(4) 0.005(4) F4_8 0.058(6) 0.026(4) 0.040(4) -0.002(3) 0.019(4) 0.005(4) F5_8 0.054(5) 0.023(3) 0.046(4) -0.005(3) -0.006(3) -0.006(3) F6_8 0.061(7) 0.020(3) 0.058(5) 0.007(3) 0.007(4) 0.015(3) C4_8 0.037(6) 0.028(5) 0.036(5) 0.012(3) 0.002(4) -0.006(4) F7_8 0.023(5) 0.055(6) 0.060(6) 0.014(4) 0.006(4) -0.007(4) F8_8 0.051(5) 0.048(4) 0.046(4) 0.023(3) -0.014(4) -0.013(4) F9_8 0.067(6) 0.038(4) 0.040(4) -0.006(3) -0.015(4) -0.006(3) O1_9 0.033(4) 0.027(3) 0.039(4) 0.000(3) 0.016(3) -0.002(3) C1_9 0.023(5) 0.020(3) 0.032(4) 0.001(3) 0.005(3) -0.001(3) C2_9 0.042(9) 0.031(8) 0.038(8) -0.002(6) 0.017(6) 0.010(7) F1_9 0.064(6) 0.056(6) 0.037(4) -0.008(4) 0.002(4) -0.007(5) F2_9 0.081(14) 0.084(14) 0.048(11) 0.003(10) 0.045(11) 0.016(13) F3_9 0.067(17) 0.042(8) 0.068(13) 0.009(8) 0.028(11) 0.030(10) C3_9 0.036(7) 0.049(9) 0.049(9) 0.019(6) -0.009(6) -0.015(8) F4_9 0.063(13) 0.068(9) 0.056(10) -0.002(7) -0.013(8) -0.037(8) F5_9 0.050(15) 0.078(12) 0.062(13) 0.040(11) -0.027(9) -0.027(12) F6_9 0.027(5) 0.057(7) 0.063(8) 0.021(6) -0.014(5) -0.017(4) C4_9 0.039(11) 0.023(7) 0.037(8) 0.006(6) -0.002(7) 0.000(7) F7_9 0.117(18) 0.025(7) 0.049(9) 0.003(7) 0.023(11) 0.010(9) F8_9 0.052(12) 0.049(19) 0.055(16) 0.022(13) -0.002(10) -0.019(12) F9_9 0.036(10) 0.047(9) 0.040(7) 0.010(6) -0.004(6) 0.003(7) O1_7 0.028(5) 0.028(3) 0.031(4) 0.011(3) -0.010(3) -0.008(3) C1_7 0.027(8) 0.028(8) 0.030(8) -0.002(7) -0.011(6) 0.000(7) C2_7 0.035(15) 0.037(11) 0.032(10) 0.001(9) -0.006(7) -0.001(10) F1_7 0.061(19) 0.069(18) 0.034(14) 0.009(13) 0.009(12) 0.022(16) F2_7 0.038(17) 0.051(19) 0.037(14) 0.024(12) -0.008(12) -0.012(13) F3_7 0.07(2) 0.039(11) 0.048(19) 0.001(10) 0.003(15) -0.019(12) C3_7 0.029(9) 0.035(10) 0.034(10) -0.004(9) -0.011(7) -0.001(8) F4_7 0.025(14) 0.037(12) 0.035(9) -0.001(8) -0.018(7) -0.010(12) F5_7 0.030(19) 0.033(9) 0.052(17) 0.000(9) 0.007(13) 0.003(9) F6_7 0.027(11) 0.053(18) 0.024(13) -0.004(14) -0.007(10) -0.006(12) C4_7 0.047(10) 0.031(9) 0.045(13) -0.005(8) -0.013(8) 0.002(8) F7_7 0.038(15) 0.018(10) 0.051(14) -0.003(10) -0.016(10) 0.006(10) F8_7 0.052(18) 0.05(2) 0.046(14) -0.021(14) -0.010(14) -0.004(18) F9_7 0.059(5) 0.035(5) 0.048(6) -0.006(4) -0.005(4) 0.015(4) O1_6 0.036(11) 0.025(8) 0.028(9) -0.009(8) 0.001(9) -0.004(9) C1_6 0.037(7) 0.021(7) 0.031(7) -0.009(6) 0.005(6) -0.007(7) C2_6 0.048(10) 0.055(10) 0.031(8) -0.014(6) 0.001(8) -0.013(9) F1_6 0.042(11) 0.111(19) 0.087(18) 0.005(15) 0.001(10) 0.006(12) F2_6 0.08(2) 0.074(11) 0.050(12) -0.038(10) -0.004(11) -0.018(12) F3_6 0.085(17) 0.072(10) 0.030(8) 0.001(7) -0.005(9) -0.024(12) C3_6 0.039(8) 0.034(9) 0.044(10) -0.008(7) 0.009(7) -0.004(8) F4_6 0.032(10) 0.051(10) 0.049(9) -0.014(7) 0.004(7) 0.000(8) F5_6 0.054(17) 0.039(9) 0.060(18) -0.002(9) 0.034(13) -0.010(9) F6_6 0.043(18) 0.050(14) 0.046(12) -0.015(11) 0.004(11) 0.017(13) C4_6 0.061(11) 0.025(8) 0.056(9) 0.000(7) 0.016(8) -0.005(8) F7_6 0.058(15) 0.038(12) 0.056(10) 0.016(8) 0.018(9) -0.005(11) F8_6 0.108(19) 0.020(9) 0.107(18) -0.013(11) 0.038(16) 0.000(11) F9_6 0.069(11) 0.040(10) 0.055(13) 0.008(11) 0.012(9) -0.024(9) O1_3 0.035(9) 0.021(7) 0.028(8) -0.008(6) 0.002(7) 0.000(7) C1_3 0.037(7) 0.019(6) 0.036(7) -0.010(5) 0.006(5) -0.006(5) C2_3 0.048(11) 0.088(13) 0.093(12) -0.061(8) 0.007(8) -0.022(7) F1_3 0.066(14) 0.075(13) 0.170(19) -0.073(10) 0.053(12) -0.047(10) F2_3 0.071(16) 0.126(17) 0.125(18) -0.105(15) 0.007(14) -0.026(13) F3_3 0.045(13) 0.146(15) 0.082(13) -0.070(10) -0.022(9) -0.001(10) C3_3 0.047(9) 0.031(7) 0.021(7) -0.004(5) 0.004(5) 0.003(6) F4_3 0.042(10) 0.029(7) 0.043(10) -0.006(6) 0.016(7) -0.011(6) F5_3 0.069(14) 0.083(12) 0.035(7) 0.005(7) 0.004(7) 0.042(9) F6_3 0.049(13) 0.034(8) 0.035(9) -0.002(6) 0.019(8) 0.002(7) C4_3 0.075(11) 0.020(8) 0.057(10) 0.013(7) 0.033(8) 0.018(8) F7_3 0.075(10) 0.054(8) 0.038(7) 0.000(6) 0.013(7) 0.035(7) F8_3 0.112(17) 0.017(8) 0.124(18) 0.000(9) 0.055(14) 0.008(8) F9_3 0.127(18) 0.055(13) 0.094(12) 0.050(9) 0.076(12) 0.038(13) O1_2 0.033(4) 0.027(3) 0.039(4) 0.000(3) 0.016(3) -0.002(3) C1_2 0.023(5) 0.020(3) 0.032(4) 0.001(3) 0.005(3) -0.001(3) C2_2 0.041(7) 0.033(6) 0.040(6) -0.006(5) 0.017(5) -0.002(6) F1_2 0.064(6) 0.056(6) 0.037(4) -0.008(4) 0.002(4) -0.007(5) F2_2 0.045(7) 0.035(6) 0.059(8) -0.010(6) 0.028(6) -0.001(5) F3_2 0.051(11) 0.030(5) 0.059(8) -0.014(5) 0.018(7) -0.009(6) C3_2 0.027(7) 0.027(6) 0.049(7) 0.008(5) -0.002(5) -0.003(5) F4_2 0.051(8) 0.052(6) 0.046(5) -0.006(5) -0.012(5) 0.000(5) F5_2 0.028(8) 0.033(5) 0.056(7) 0.012(5) 0.009(6) 0.006(5) F6_2 0.027(5) 0.057(7) 0.063(8) 0.021(6) -0.014(5) -0.017(4) C4_2 0.034(9) 0.023(6) 0.049(8) 0.006(5) 0.006(6) 0.004(6) F7_2 0.051(8) 0.021(4) 0.064(6) -0.003(4) 0.015(5) -0.008(4) F8_2 0.046(9) 0.030(10) 0.051(10) 0.009(8) 0.010(7) -0.010(8) F9_2 0.036(7) 0.035(6) 0.084(9) 0.029(6) -0.006(6) 0.000(5) O1_1 0.028(5) 0.028(3) 0.031(4) 0.011(3) -0.010(3) -0.008(3) C1_1 0.018(6) 0.027(5) 0.024(5) 0.001(4) -0.005(4) -0.002(4) C2_1 0.036(8) 0.034(6) 0.050(6) 0.015(5) -0.010(5) 0.001(5) F1_1 0.049(5) 0.049(4) 0.048(4) 0.025(3) -0.015(3) -0.014(4) F2_1 0.049(5) 0.049(4) 0.048(4) 0.025(3) -0.015(3) -0.014(4) F3_1 0.064(8) 0.030(4) 0.081(7) 0.000(5) -0.010(6) 0.010(4) C3_1 0.029(6) 0.038(5) 0.030(6) 0.003(4) 0.003(4) -0.005(5) F4_1 0.038(7) 0.043(5) 0.042(6) 0.014(4) -0.004(5) -0.013(4) F5_1 0.062(11) 0.064(7) 0.049(5) -0.022(5) 0.025(6) -0.018(6) F6_1 0.023(6) 0.053(7) 0.052(7) 0.013(5) 0.004(4) -0.003(4) C4_1 0.043(8) 0.041(6) 0.030(6) -0.005(4) 0.003(4) 0.006(5) F7_1 0.059(5) 0.035(5) 0.048(6) -0.006(4) -0.005(4) 0.015(4) F8_1 0.061(8) 0.040(7) 0.038(6) -0.011(5) -0.008(5) 0.000(6) F9_1 0.066(8) 0.081(7) 0.036(5) 0.000(4) 0.021(4) 0.008(6) Al1 0.0221(19) 0.0129(11) 0.0178(11) 0.0014(9) 0.0002(11) -0.0016(10) Ta1B 0.041(5) 0.024(3) 0.032(3) 0.001(2) 0.005(3) -0.009(2) Ta1 0.0332(4) 0.0274(3) 0.0317(3) -0.0086(2) 0.00499(19) -0.00135(19) C1A 0.068(11) 0.043(6) 0.048(7) 0.003(5) 0.020(7) 0.032(6) C2A 0.067(12) 0.086(11) 0.062(9) -0.042(8) -0.041(9) 0.048(9) C3A 0.023(10) 0.074(9) 0.070(9) -0.039(7) 0.006(7) 0.004(6) C4A 0.063(12) 0.047(7) 0.079(9) -0.017(7) 0.026(8) 0.016(7) C5A 0.065(10) 0.047(7) 0.032(5) -0.019(5) 0.010(6) 0.022(6) C6A 0.047(9) 0.030(6) 0.073(8) -0.020(5) 0.014(7) 0.009(5) F1B 0.089(8) 0.066(5) 0.078(5) 0.015(4) 0.033(5) 0.030(5) F2B 0.23(2) 0.160(15) 0.200(17) 0.010(13) 0.055(15) 0.076(14) C1B 0.027(8) 0.046(6) 0.028(5) -0.004(4) 0.003(4) -0.007(5) O1B 0.058(7) 0.057(5) 0.032(4) 0.011(4) -0.004(4) -0.010(4) C2B 0.045(9) 0.043(6) 0.032(5) -0.012(4) -0.001(5) -0.011(5) O2B 0.046(6) 0.062(5) 0.047(5) -0.007(4) -0.001(4) -0.010(4) C3B 0.047(10) 0.020(5) 0.041(6) -0.005(4) 0.006(6) 0.010(5) O3B 0.047(7) 0.035(4) 0.060(5) 0.006(3) 0.029(5) 0.000(4) C4B 0.021(7) 0.031(5) 0.023(4) 0.001(4) 0.006(4) 0.001(4) O4B 0.061(6) 0.033(4) 0.028(3) -0.008(3) 0.008(3) -0.008(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 O1_12 C1_12 1.341(16) . ? O1_12 Al1 1.710(16) . ? C1_12 C4_12 1.547(15) . ? C1_12 C2_12 1.554(15) . ? C1_12 C3_12 1.557(15) . ? C2_12 F1_12 1.324(15) . ? C2_12 F3_12 1.326(15) . ? C2_12 F2_12 1.331(15) . ? C3_12 F4_12 1.322(15) . ? C3_12 F5_12 1.325(15) . ? C3_12 F6_12 1.330(15) . ? C4_12 F9_12 1.327(15) . ? C4_12 F8_12 1.329(15) . ? C4_12 F7_12 1.331(15) . ? O1_11 C1_11 1.347(17) . ? O1_11 Al1 1.708(17) . ? C1_11 C4_11 1.548(15) . ? C1_11 C3_11 1.550(15) . ? C1_11 C2_11 1.551(15) . ? C2_11 F1_11 1.324(15) . ? C2_11 F3_11 1.331(15) . ? C2_11 F2_11 1.331(15) . ? C3_11 F4_11 1.327(15) . ? C3_11 F6_11 1.327(15) . ? C3_11 F5_11 1.332(15) . ? C4_11 F8_11 1.326(15) . ? C4_11 F7_11 1.330(15) . ? C4_11 F9_11 1.333(15) . ? O1_10 C1_10 1.343(16) . ? O1_10 Al1 1.699(16) . ? C1_10 C3_10 1.544(14) . ? C1_10 C4_10 1.550(15) . ? C1_10 C2_10 1.555(15) . ? C2_10 F2_10 1.324(15) . ? C2_10 F1_10 1.327(15) . ? C2_10 F3_10 1.331(15) . ? C3_10 F4_10 1.325(15) . ? C3_10 F5_10 1.325(15) . ? C3_10 F6_10 1.333(15) . ? C4_10 F9_10 1.328(15) . ? C4_10 F8_10 1.329(15) . ? C4_10 F7_10 1.330(15) . ? O1_8 C1_8 1.362(9) . ? O1_8 Al1 1.732(6) . ? C1_8 C3_8 1.542(10) . ? C1_8 C4_8 1.544(11) . ? C1_8 C2_8 1.557(11) . ? C2_8 F3_8 1.328(11) . ? C2_8 F1_8 1.330(10) . ? C2_8 F2_8 1.340(10) . ? C3_8 F4_8 1.326(11) . ? C3_8 F6_8 1.333(10) . ? C3_8 F5_8 1.337(11) . ? C4_8 F7_8 1.334(11) . ? C4_8 F9_8 1.334(10) . ? C4_8 F8_8 1.348(10) . ? O1_9 C1_9 1.344(14) . ? O1_9 Al1 1.707(13) . ? C1_9 C2_9 1.546(13) . ? C1_9 C3_9 1.547(14) . ? C1_9 C4_9 1.552(13) . ? C2_9 F1_9 1.325(14) . ? C2_9 F3_9 1.328(14) . ? C2_9 F2_9 1.330(14) . ? C3_9 F6_9 1.318(14) . ? C3_9 F5_9 1.327(14) . ? C3_9 F4_9 1.339(14) . ? C4_9 F9_9 1.321(14) . ? C4_9 F7_9 1.325(14) . ? C4_9 F8_9 1.330(14) . ? O1_7 C1_7 1.358(16) . ? O1_7 Al1 1.725(15) . ? C1_7 C2_7 1.549(14) . ? C1_7 C4_7 1.549(14) . ? C1_7 C3_7 1.551(14) . ? C2_7 F2_7 1.330(15) . ? C2_7 F1_7 1.332(15) . ? C2_7 F3_7 1.333(15) . ? C3_7 F4_7 1.323(15) . ? C3_7 F6_7 1.332(15) . ? C3_7 F5_7 1.333(15) . ? C4_7 F8_7 1.327(15) . ? C4_7 F9_7 1.331(15) . ? C4_7 F7_7 1.333(15) . ? O1_6 C1_6 1.354(14) . ? O1_6 Al1 1.714(13) . ? C1_6 C3_6 1.546(14) . ? C1_6 C2_6 1.547(14) . ? C1_6 C4_6 1.555(14) . ? C2_6 F1_6 1.326(15) . ? C2_6 F2_6 1.328(14) . ? C2_6 F3_6 1.338(14) . ? C3_6 F5_6 1.326(14) . ? C3_6 F6_6 1.328(14) . ? C3_6 F4_6 1.338(14) . ? C4_6 F9_6 1.327(14) . ? C4_6 F7_6 1.331(14) . ? C4_6 F8_6 1.331(14) . ? O1_3 C1_3 1.358(13) . ? O1_3 Al1 1.712(11) . ? C1_3 C3_3 1.543(13) . ? C1_3 C2_3 1.552(13) . ? C1_3 C4_3 1.555(13) . ? C2_3 F2_3 1.328(14) . ? C2_3 F1_3 1.330(14) . ? C2_3 F3_3 1.332(14) . ? C3_3 F6_3 1.320(13) . ? C3_3 F5_3 1.327(13) . ? C3_3 F4_3 1.331(14) . ? C4_3 F7_3 1.323(14) . ? C4_3 F9_3 1.326(14) . ? C4_3 F8_3 1.333(14) . ? O1_2 C1_2 1.340(13) . ? O1_2 Al1 1.704(11) . ? C1_2 C2_2 1.544(12) . ? C1_2 C3_2 1.553(12) . ? C1_2 C4_2 1.555(12) . ? C2_2 F1_2 1.326(13) . ? C2_2 F3_2 1.329(12) . ? C2_2 F2_2 1.330(13) . ? C3_2 F6_2 1.319(13) . ? C3_2 F5_2 1.329(12) . ? C3_2 F4_2 1.337(13) . ? C4_2 F7_2 1.324(12) . ? C4_2 F9_2 1.326(12) . ? C4_2 F8_2 1.329(13) . ? O1_1 C1_1 1.354(11) . ? O1_1 Al1 1.722(8) . ? C1_1 C3_1 1.547(12) . ? C1_1 C4_1 1.551(11) . ? C1_1 C2_1 1.554(11) . ? C2_1 F1_1 1.320(12) . ? C2_1 F3_1 1.324(12) . ? C2_1 F2_1 1.343(12) . ? C3_1 F5_1 1.308(12) . ? C3_1 F6_1 1.334(11) . ? C3_1 F4_1 1.342(11) . ? C4_1 F8_1 1.324(12) . ? C4_1 F9_1 1.325(12) . ? C4_1 F7_1 1.335(12) . ? Ta1 C4B 2.079(9) . ? Ta1 C2B 2.090(12) . ? Ta1 C1B 2.116(11) . ? Ta1 C3B 2.135(14) . ? Ta1 C3A 2.389(13) . ? Ta1 C2A 2.402(12) . ? Ta1 C6A 2.411(10) . ? Ta1 C5A 2.424(10) . ? Ta1 C1A 2.469(11) . ? Ta1 C4A 2.478(13) . ? C1A F1B 1.311(14) . ? C1A C6A 1.385(17) . ? C1A C2A 1.41(2) . ? C2A F2B 1.27(2) . ? C2A C3A 1.43(2) . ? C3A C4A 1.346(18) . ? C4A C5A 1.390(19) . ? C5A C6A 1.390(17) . ? C1B O1B 1.119(12) . ? C2B O2B 1.122(13) . ? C3B O3B 1.103(13) . ? C4B O4B 1.140(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1_12 O1_12 Al1 159(4) . . ? O1_12 C1_12 C4_12 112(2) . . ? O1_12 C1_12 C2_12 110.5(19) . . ? C4_12 C1_12 C2_12 109.1(17) . . ? O1_12 C1_12 C3_12 110(2) . . ? C4_12 C1_12 C3_12 107.3(17) . . ? C2_12 C1_12 C3_12 107.0(16) . . ? F1_12 C2_12 F3_12 108(2) . . ? F1_12 C2_12 F2_12 109(2) . . ? F3_12 C2_12 F2_12 108(2) . . ? F1_12 C2_12 C1_12 111(2) . . ? F3_12 C2_12 C1_12 111(2) . . ? F2_12 C2_12 C1_12 110(2) . . ? F4_12 C3_12 F5_12 109(2) . . ? F4_12 C3_12 F6_12 109(2) . . ? F5_12 C3_12 F6_12 108(2) . . ? F4_12 C3_12 C1_12 112(2) . . ? F5_12 C3_12 C1_12 109(2) . . ? F6_12 C3_12 C1_12 110(2) . . ? F9_12 C4_12 F8_12 108(2) . . ? F9_12 C4_12 F7_12 107(2) . . ? F8_12 C4_12 F7_12 108(2) . . ? F9_12 C4_12 C1_12 111(2) . . ? F8_12 C4_12 C1_12 111(2) . . ? F7_12 C4_12 C1_12 110(2) . . ? C1_11 O1_11 Al1 136(3) . . ? O1_11 C1_11 C4_11 109(2) . . ? O1_11 C1_11 C3_11 110(2) . . ? C4_11 C1_11 C3_11 110.3(19) . . ? O1_11 C1_11 C2_11 110(2) . . ? C4_11 C1_11 C2_11 110.1(18) . . ? C3_11 C1_11 C2_11 107.3(18) . . ? F1_11 C2_11 F3_11 108(2) . . ? F1_11 C2_11 F2_11 110(2) . . ? F3_11 C2_11 F2_11 108(2) . . ? F1_11 C2_11 C1_11 111(2) . . ? F3_11 C2_11 C1_11 110(2) . . ? F2_11 C2_11 C1_11 110(2) . . ? F4_11 C3_11 F6_11 108(2) . . ? F4_11 C3_11 F5_11 108(2) . . ? F6_11 C3_11 F5_11 108(2) . . ? F4_11 C3_11 C1_11 111(2) . . ? F6_11 C3_11 C1_11 112(2) . . ? F5_11 C3_11 C1_11 109(2) . . ? F8_11 C4_11 F7_11 108(2) . . ? F8_11 C4_11 F9_11 108(2) . . ? F7_11 C4_11 F9_11 107(2) . . ? F8_11 C4_11 C1_11 113(2) . . ? F7_11 C4_11 C1_11 110(2) . . ? F9_11 C4_11 C1_11 110(2) . . ? C1_10 O1_10 Al1 156(3) . . ? O1_10 C1_10 C3_10 113(2) . . ? O1_10 C1_10 C4_10 109.1(19) . . ? C3_10 C1_10 C4_10 108.9(16) . . ? O1_10 C1_10 C2_10 107.5(18) . . ? C3_10 C1_10 C2_10 108.6(16) . . ? C4_10 C1_10 C2_10 109.8(16) . . ? F2_10 C2_10 F1_10 111(2) . . ? F2_10 C2_10 F3_10 109(2) . . ? F1_10 C2_10 F3_10 108(2) . . ? F2_10 C2_10 C1_10 111.3(19) . . ? F1_10 C2_10 C1_10 108.6(19) . . ? F3_10 C2_10 C1_10 109(2) . . ? F4_10 C3_10 F5_10 110(2) . . ? F4_10 C3_10 F6_10 108(2) . . ? F5_10 C3_10 F6_10 107(2) . . ? F4_10 C3_10 C1_10 111.1(19) . . ? F5_10 C3_10 C1_10 111(2) . . ? F6_10 C3_10 C1_10 110(2) . . ? F9_10 C4_10 F8_10 109(2) . . ? F9_10 C4_10 F7_10 108(2) . . ? F8_10 C4_10 F7_10 108(2) . . ? F9_10 C4_10 C1_10 110(2) . . ? F8_10 C4_10 C1_10 112(2) . . ? F7_10 C4_10 C1_10 110(2) . . ? C1_8 O1_8 Al1 148.9(7) . . ? O1_8 C1_8 C3_8 109.3(7) . . ? O1_8 C1_8 C4_8 112.2(7) . . ? C3_8 C1_8 C4_8 109.0(7) . . ? O1_8 C1_8 C2_8 107.2(7) . . ? C3_8 C1_8 C2_8 109.9(7) . . ? C4_8 C1_8 C2_8 109.2(7) . . ? F3_8 C2_8 F1_8 109.0(9) . . ? F3_8 C2_8 F2_8 106.1(9) . . ? F1_8 C2_8 F2_8 108.9(8) . . ? F3_8 C2_8 C1_8 110.6(8) . . ? F1_8 C2_8 C1_8 110.6(8) . . ? F2_8 C2_8 C1_8 111.6(8) . . ? F4_8 C3_8 F6_8 107.6(9) . . ? F4_8 C3_8 F5_8 108.2(9) . . ? F6_8 C3_8 F5_8 107.7(8) . . ? F4_8 C3_8 C1_8 110.6(8) . . ? F6_8 C3_8 C1_8 112.0(8) . . ? F5_8 C3_8 C1_8 110.5(8) . . ? F7_8 C4_8 F9_8 109.0(9) . . ? F7_8 C4_8 F8_8 107.0(9) . . ? F9_8 C4_8 F8_8 106.6(8) . . ? F7_8 C4_8 C1_8 110.8(8) . . ? F9_8 C4_8 C1_8 110.8(8) . . ? F8_8 C4_8 C1_8 112.5(8) . . ? C1_9 O1_9 Al1 153(2) . . ? O1_9 C1_9 C2_9 108.4(14) . . ? O1_9 C1_9 C3_9 108.2(17) . . ? C2_9 C1_9 C3_9 110.9(11) . . ? O1_9 C1_9 C4_9 111.5(17) . . ? C2_9 C1_9 C4_9 109.4(11) . . ? C3_9 C1_9 C4_9 108.4(11) . . ? F1_9 C2_9 F3_9 108.2(16) . . ? F1_9 C2_9 F2_9 106.2(16) . . ? F3_9 C2_9 F2_9 108.5(17) . . ? F1_9 C2_9 C1_9 110.5(13) . . ? F3_9 C2_9 C1_9 110.0(14) . . ? F2_9 C2_9 C1_9 113.2(15) . . ? F6_9 C3_9 F5_9 106.7(16) . . ? F6_9 C3_9 F4_9 105.9(16) . . ? F5_9 C3_9 F4_9 109.8(16) . . ? F6_9 C3_9 C1_9 112.4(14) . . ? F5_9 C3_9 C1_9 111.5(14) . . ? F4_9 C3_9 C1_9 110.3(13) . . ? F9_9 C4_9 F7_9 108.4(16) . . ? F9_9 C4_9 F8_9 107.8(19) . . ? F7_9 C4_9 F8_9 107.8(19) . . ? F9_9 C4_9 C1_9 111.0(12) . . ? F7_9 C4_9 C1_9 109.7(13) . . ? F8_9 C4_9 C1_9 112.0(18) . . ? C1_7 O1_7 Al1 153(3) . . ? O1_7 C1_7 C2_7 109.4(19) . . ? O1_7 C1_7 C4_7 108.7(19) . . ? C2_7 C1_7 C4_7 109.6(14) . . ? O1_7 C1_7 C3_7 110.6(18) . . ? C2_7 C1_7 C3_7 109.3(13) . . ? C4_7 C1_7 C3_7 109.1(14) . . ? F2_7 C2_7 F1_7 106(2) . . ? F2_7 C2_7 F3_7 108(2) . . ? F1_7 C2_7 F3_7 107(2) . . ? F2_7 C2_7 C1_7 114.9(17) . . ? F1_7 C2_7 C1_7 111.8(17) . . ? F3_7 C2_7 C1_7 107.8(18) . . ? F4_7 C3_7 F6_7 107.8(19) . . ? F4_7 C3_7 F5_7 108.3(19) . . ? F6_7 C3_7 F5_7 107.3(19) . . ? F4_7 C3_7 C1_7 111.2(19) . . ? F6_7 C3_7 C1_7 111.0(18) . . ? F5_7 C3_7 C1_7 111.1(17) . . ? F8_7 C4_7 F9_7 107(2) . . ? F8_7 C4_7 F7_7 109(2) . . ? F9_7 C4_7 F7_7 108(2) . . ? F8_7 C4_7 C1_7 112(2) . . ? F9_7 C4_7 C1_7 111(2) . . ? F7_7 C4_7 C1_7 109.8(16) . . ? C1_6 O1_6 Al1 151(2) . . ? O1_6 C1_6 C3_6 111.8(17) . . ? O1_6 C1_6 C2_6 108.7(15) . . ? C3_6 C1_6 C2_6 109.3(13) . . ? O1_6 C1_6 C4_6 109.7(18) . . ? C3_6 C1_6 C4_6 107.6(13) . . ? C2_6 C1_6 C4_6 109.7(12) . . ? F1_6 C2_6 F2_6 109(2) . . ? F1_6 C2_6 F3_6 110.3(18) . . ? F2_6 C2_6 F3_6 103.5(17) . . ? F1_6 C2_6 C1_6 111.1(17) . . ? F2_6 C2_6 C1_6 114.0(17) . . ? F3_6 C2_6 C1_6 108.9(14) . . ? F5_6 C3_6 F6_6 108.2(19) . . ? F5_6 C3_6 F4_6 108.5(17) . . ? F6_6 C3_6 F4_6 108.1(19) . . ? F5_6 C3_6 C1_6 109.7(17) . . ? F6_6 C3_6 C1_6 111.1(17) . . ? F4_6 C3_6 C1_6 111.2(14) . . ? F9_6 C4_6 F7_6 109.5(17) . . ? F9_6 C4_6 F8_6 106.9(19) . . ? F7_6 C4_6 F8_6 109.6(19) . . ? F9_6 C4_6 C1_6 110.5(14) . . ? F7_6 C4_6 C1_6 109.5(16) . . ? F8_6 C4_6 C1_6 110.9(18) . . ? C1_3 O1_3 Al1 146.1(18) . . ? O1_3 C1_3 C3_3 111.0(15) . . ? O1_3 C1_3 C2_3 107.0(12) . . ? C3_3 C1_3 C2_3 110.7(11) . . ? O1_3 C1_3 C4_3 110.7(15) . . ? C3_3 C1_3 C4_3 109.4(11) . . ? C2_3 C1_3 C4_3 107.9(12) . . ? F2_3 C2_3 F1_3 107.3(17) . . ? F2_3 C2_3 F3_3 107.9(17) . . ? F1_3 C2_3 F3_3 110.3(18) . . ? F2_3 C2_3 C1_3 111.3(15) . . ? F1_3 C2_3 C1_3 109.2(13) . . ? F3_3 C2_3 C1_3 110.8(14) . . ? F6_3 C3_3 F5_3 108.1(15) . . ? F6_3 C3_3 F4_3 108.1(15) . . ? F5_3 C3_3 F4_3 108.5(15) . . ? F6_3 C3_3 C1_3 114.0(14) . . ? F5_3 C3_3 C1_3 109.0(13) . . ? F4_3 C3_3 C1_3 109.1(13) . . ? F7_3 C4_3 F9_3 110.3(17) . . ? F7_3 C4_3 F8_3 106.4(16) . . ? F9_3 C4_3 F8_3 107.8(17) . . ? F7_3 C4_3 C1_3 110.6(12) . . ? F9_3 C4_3 C1_3 109.6(14) . . ? F8_3 C4_3 C1_3 112.2(15) . . ? C1_2 O1_2 Al1 149.8(17) . . ? O1_2 C1_2 C2_2 108.1(12) . . ? O1_2 C1_2 C3_2 107.4(13) . . ? C2_2 C1_2 C3_2 109.7(9) . . ? O1_2 C1_2 C4_2 112.3(13) . . ? C2_2 C1_2 C4_2 109.6(9) . . ? C3_2 C1_2 C4_2 109.8(9) . . ? F1_2 C2_2 F3_2 108.1(12) . . ? F1_2 C2_2 F2_2 106.5(12) . . ? F3_2 C2_2 F2_2 108.1(12) . . ? F1_2 C2_2 C1_2 110.7(10) . . ? F3_2 C2_2 C1_2 110.6(11) . . ? F2_2 C2_2 C1_2 112.6(11) . . ? F6_2 C3_2 F5_2 108.7(12) . . ? F6_2 C3_2 F4_2 105.9(11) . . ? F5_2 C3_2 F4_2 107.1(11) . . ? F6_2 C3_2 C1_2 113.2(11) . . ? F5_2 C3_2 C1_2 111.2(11) . . ? F4_2 C3_2 C1_2 110.5(10) . . ? F7_2 C4_2 F9_2 106.8(12) . . ? F7_2 C4_2 F8_2 107.8(14) . . ? F9_2 C4_2 F8_2 107.8(14) . . ? F7_2 C4_2 C1_2 111.2(10) . . ? F9_2 C4_2 C1_2 110.7(10) . . ? F8_2 C4_2 C1_2 112.3(13) . . ? C1_1 O1_1 Al1 147.9(11) . . ? O1_1 C1_1 C3_1 110.5(9) . . ? O1_1 C1_1 C4_1 111.2(10) . . ? C3_1 C1_1 C4_1 109.6(8) . . ? O1_1 C1_1 C2_1 108.2(9) . . ? C3_1 C1_1 C2_1 109.2(8) . . ? C4_1 C1_1 C2_1 108.1(8) . . ? F1_1 C2_1 F3_1 107.1(11) . . ? F1_1 C2_1 F2_1 107.6(10) . . ? F3_1 C2_1 F2_1 108.8(12) . . ? F1_1 C2_1 C1_1 111.9(9) . . ? F3_1 C2_1 C1_1 110.3(9) . . ? F2_1 C2_1 C1_1 111.1(9) . . ? F5_1 C3_1 F6_1 109.0(12) . . ? F5_1 C3_1 F4_1 107.3(10) . . ? F6_1 C3_1 F4_1 107.7(10) . . ? F5_1 C3_1 C1_1 111.1(10) . . ? F6_1 C3_1 C1_1 112.3(9) . . ? F4_1 C3_1 C1_1 109.3(9) . . ? F8_1 C4_1 F9_1 107.5(12) . . ? F8_1 C4_1 F7_1 106.9(11) . . ? F9_1 C4_1 F7_1 107.6(11) . . ? F8_1 C4_1 C1_1 113.7(11) . . ? F9_1 C4_1 C1_1 110.6(9) . . ? F7_1 C4_1 C1_1 110.3(10) . . ? O1_10 Al1 O1_9 106(2) . . ? O1_11 Al1 O1_12 107(3) . . ? O1_2 Al1 O1_3 107.6(12) . . ? O1_10 Al1 O1_6 101(2) . . ? O1_9 Al1 O1_6 109.7(17) . . ? O1_2 Al1 O1_1 109.9(11) . . ? O1_3 Al1 O1_1 108.1(10) . . ? O1_10 Al1 O1_7 119(2) . . ? O1_9 Al1 O1_7 114(2) . . ? O1_6 Al1 O1_7 106.7(19) . . ? O1_2 Al1 O1_8 110.1(9) . . ? O1_3 Al1 O1_8 113.7(11) . . ? O1_1 Al1 O1_8 107.5(6) . . ? C4B Ta1 C2B 117.9(4) . . ? C4B Ta1 C1B 75.7(3) . . ? C2B Ta1 C1B 73.3(4) . . ? C4B Ta1 C3B 72.9(4) . . ? C2B Ta1 C3B 74.1(4) . . ? C1B Ta1 C3B 115.4(4) . . ? C4B Ta1 C3A 90.6(4) . . ? C2B Ta1 C3A 144.5(4) . . ? C1B Ta1 C3A 96.1(5) . . ? C3B Ta1 C3A 138.3(5) . . ? C4B Ta1 C2A 88.4(4) . . ? C2B Ta1 C2A 151.1(5) . . ? C1B Ta1 C2A 128.8(6) . . ? C3B Ta1 C2A 105.2(6) . . ? C3A Ta1 C2A 34.8(6) . . ? C4B Ta1 C6A 144.2(4) . . ? C2B Ta1 C6A 91.3(4) . . ? C1B Ta1 C6A 136.3(4) . . ? C3B Ta1 C6A 98.2(4) . . ? C3A Ta1 C6A 73.0(5) . . ? C2A Ta1 C6A 59.9(5) . . ? C4B Ta1 C5A 150.5(4) . . ? C2B Ta1 C5A 89.3(4) . . ? C1B Ta1 C5A 104.2(4) . . ? C3B Ta1 C5A 129.4(4) . . ? C3A Ta1 C5A 60.0(4) . . ? C2A Ta1 C5A 68.5(4) . . ? C6A Ta1 C5A 33.4(4) . . ? C4B Ta1 C1A 111.3(4) . . ? C2B Ta1 C1A 118.6(5) . . ? C1B Ta1 C1A 156.2(5) . . ? C3B Ta1 C1A 88.2(4) . . ? C3A Ta1 C1A 62.0(5) . . ? C2A Ta1 C1A 33.7(5) . . ? C6A Ta1 C1A 32.9(4) . . ? C5A Ta1 C1A 58.1(4) . . ? C4B Ta1 C4A 118.9(4) . . ? C2B Ta1 C4A 112.7(5) . . ? C1B Ta1 C4A 88.7(5) . . ? C3B Ta1 C4A 155.7(4) . . ? C3A Ta1 C4A 32.0(4) . . ? C2A Ta1 C4A 57.1(6) . . ? C6A Ta1 C4A 59.4(5) . . ? C5A Ta1 C4A 32.9(4) . . ? C1A Ta1 C4A 67.9(5) . . ? F1B C1A C6A 121.5(14) . . ? F1B C1A C2A 120.0(13) . . ? C6A C1A C2A 118.5(13) . . ? F1B C1A Ta1 128.0(8) . . ? C6A C1A Ta1 71.3(6) . . ? C2A C1A Ta1 70.6(7) . . ? F2B C2A C1A 132(2) . . ? F2B C2A C3A 104.6(18) . . ? C1A C2A C3A 123.2(11) . . ? F2B C2A Ta1 126.8(11) . . ? C1A C2A Ta1 75.7(7) . . ? C3A C2A Ta1 72.1(8) . . ? C4A C3A C2A 114.2(13) . . ? C4A C3A Ta1 77.6(8) . . ? C2A C3A Ta1 73.1(8) . . ? C3A C4A C5A 123.2(14) . . ? C3A C4A Ta1 70.3(8) . . ? C5A C4A Ta1 71.4(7) . . ? C4A C5A C6A 121.3(11) . . ? C4A C5A Ta1 75.7(7) . . ? C6A C5A Ta1 72.8(6) . . ? C1A C6A C5A 117.9(12) . . ? C1A C6A Ta1 75.8(6) . . ? C5A C6A Ta1 73.8(6) . . ? O1B C1B Ta1 178.4(8) . . ? O2B C2B Ta1 178.6(10) . . ? O3B C3B Ta1 179.0(10) . . ? O4B C4B Ta1 179.1(9) . . ? 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 Al1 O1_12 C1_12 C4_12 28(12) . . . . ? Al1 O1_12 C1_12 C2_12 150(11) . . . . ? Al1 O1_12 C1_12 C3_12 -92(12) . . . . ? O1_12 C1_12 C2_12 F1_12 -78(4) . . . . ? C4_12 C1_12 C2_12 F1_12 46(3) . . . . ? C3_12 C1_12 C2_12 F1_12 162(3) . . . . ? O1_12 C1_12 C2_12 F3_12 42(4) . . . . ? C4_12 C1_12 C2_12 F3_12 166(3) . . . . ? C3_12 C1_12 C2_12 F3_12 -78(3) . . . . ? O1_12 C1_12 C2_12 F2_12 162(4) . . . . ? C4_12 C1_12 C2_12 F2_12 -74(3) . . . . ? C3_12 C1_12 C2_12 F2_12 41(3) . . . . ? O1_12 C1_12 C3_12 F4_12 41(4) . . . . ? C4_12 C1_12 C3_12 F4_12 -82(3) . . . . ? C2_12 C1_12 C3_12 F4_12 161(3) . . . . ? O1_12 C1_12 C3_12 F5_12 -80(4) . . . . ? C4_12 C1_12 C3_12 F5_12 157(3) . . . . ? C2_12 C1_12 C3_12 F5_12 40(3) . . . . ? O1_12 C1_12 C3_12 F6_12 162(4) . . . . ? C4_12 C1_12 C3_12 F6_12 39(3) . . . . ? C2_12 C1_12 C3_12 F6_12 -78(3) . . . . ? O1_12 C1_12 C4_12 F9_12 45(4) . . . . ? C2_12 C1_12 C4_12 F9_12 -78(4) . . . . ? C3_12 C1_12 C4_12 F9_12 167(4) . . . . ? O1_12 C1_12 C4_12 F8_12 166(4) . . . . ? C2_12 C1_12 C4_12 F8_12 43(4) . . . . ? C3_12 C1_12 C4_12 F8_12 -72(4) . . . . ? O1_12 C1_12 C4_12 F7_12 -74(4) . . . . ? C2_12 C1_12 C4_12 F7_12 163(4) . . . . ? C3_12 C1_12 C4_12 F7_12 48(4) . . . . ? Al1 O1_11 C1_11 C4_11 82(6) . . . . ? Al1 O1_11 C1_11 C3_11 -39(6) . . . . ? Al1 O1_11 C1_11 C2_11 -157(5) . . . . ? O1_11 C1_11 C2_11 F1_11 -82(5) . . . . ? C4_11 C1_11 C2_11 F1_11 38(4) . . . . ? C3_11 C1_11 C2_11 F1_11 158(4) . . . . ? O1_11 C1_11 C2_11 F3_11 37(5) . . . . ? C4_11 C1_11 C2_11 F3_11 158(4) . . . . ? C3_11 C1_11 C2_11 F3_11 -82(5) . . . . ? O1_11 C1_11 C2_11 F2_11 156(5) . . . . ? C4_11 C1_11 C2_11 F2_11 -83(4) . . . . ? C3_11 C1_11 C2_11 F2_11 37(4) . . . . ? O1_11 C1_11 C3_11 F4_11 33(5) . . . . ? C4_11 C1_11 C3_11 F4_11 -88(4) . . . . ? C2_11 C1_11 C3_11 F4_11 152(5) . . . . ? O1_11 C1_11 C3_11 F6_11 154(5) . . . . ? C4_11 C1_11 C3_11 F6_11 34(5) . . . . ? C2_11 C1_11 C3_11 F6_11 -87(5) . . . . ? O1_11 C1_11 C3_11 F5_11 -86(5) . . . . ? C4_11 C1_11 C3_11 F5_11 153(4) . . . . ? C2_11 C1_11 C3_11 F5_11 33(5) . . . . ? O1_11 C1_11 C4_11 F8_11 162(4) . . . . ? C3_11 C1_11 C4_11 F8_11 -77(4) . . . . ? C2_11 C1_11 C4_11 F8_11 41(4) . . . . ? O1_11 C1_11 C4_11 F7_11 -77(4) . . . . ? C3_11 C1_11 C4_11 F7_11 43(4) . . . . ? C2_11 C1_11 C4_11 F7_11 162(4) . . . . ? O1_11 C1_11 C4_11 F9_11 40(4) . . . . ? C3_11 C1_11 C4_11 F9_11 161(4) . . . . ? C2_11 C1_11 C4_11 F9_11 -80(4) . . . . ? Al1 O1_10 C1_10 C3_10 15(8) . . . . ? Al1 O1_10 C1_10 C4_10 136(7) . . . . ? Al1 O1_10 C1_10 C2_10 -105(8) . . . . ? O1_10 C1_10 C2_10 F2_10 163(3) . . . . ? C3_10 C1_10 C2_10 F2_10 41(3) . . . . ? C4_10 C1_10 C2_10 F2_10 -78(3) . . . . ? O1_10 C1_10 C2_10 F1_10 -74(3) . . . . ? C3_10 C1_10 C2_10 F1_10 164(3) . . . . ? C4_10 C1_10 C2_10 F1_10 45(3) . . . . ? O1_10 C1_10 C2_10 F3_10 43(3) . . . . ? C3_10 C1_10 C2_10 F3_10 -79(3) . . . . ? C4_10 C1_10 C2_10 F3_10 162(3) . . . . ? O1_10 C1_10 C3_10 F4_10 48(3) . . . . ? C4_10 C1_10 C3_10 F4_10 -73(3) . . . . ? C2_10 C1_10 C3_10 F4_10 168(3) . . . . ? O1_10 C1_10 C3_10 F5_10 -74(3) . . . . ? C4_10 C1_10 C3_10 F5_10 164(3) . . . . ? C2_10 C1_10 C3_10 F5_10 45(3) . . . . ? O1_10 C1_10 C3_10 F6_10 168(3) . . . . ? C4_10 C1_10 C3_10 F6_10 46(3) . . . . ? C2_10 C1_10 C3_10 F6_10 -73(3) . . . . ? O1_10 C1_10 C4_10 F9_10 35(3) . . . . ? C3_10 C1_10 C4_10 F9_10 158(3) . . . . ? C2_10 C1_10 C4_10 F9_10 -83(3) . . . . ? O1_10 C1_10 C4_10 F8_10 156(3) . . . . ? C3_10 C1_10 C4_10 F8_10 -80(3) . . . . ? C2_10 C1_10 C4_10 F8_10 38(3) . . . . ? O1_10 C1_10 C4_10 F7_10 -84(3) . . . . ? C3_10 C1_10 C4_10 F7_10 40(3) . . . . ? C2_10 C1_10 C4_10 F7_10 158(3) . . . . ? Al1 O1_8 C1_8 C3_8 87.1(13) . . . . ? Al1 O1_8 C1_8 C4_8 -34.0(15) . . . . ? Al1 O1_8 C1_8 C2_8 -153.9(11) . . . . ? O1_8 C1_8 C2_8 F3_8 -44.4(10) . . . . ? C3_8 C1_8 C2_8 F3_8 74.3(10) . . . . ? C4_8 C1_8 C2_8 F3_8 -166.1(8) . . . . ? O1_8 C1_8 C2_8 F1_8 76.4(10) . . . . ? C3_8 C1_8 C2_8 F1_8 -164.9(8) . . . . ? C4_8 C1_8 C2_8 F1_8 -45.3(10) . . . . ? O1_8 C1_8 C2_8 F2_8 -162.2(8) . . . . ? C3_8 C1_8 C2_8 F2_8 -43.5(10) . . . . ? C4_8 C1_8 C2_8 F2_8 76.0(10) . . . . ? O1_8 C1_8 C3_8 F4_8 -47.8(11) . . . . ? C4_8 C1_8 C3_8 F4_8 75.2(10) . . . . ? C2_8 C1_8 C3_8 F4_8 -165.2(8) . . . . ? O1_8 C1_8 C3_8 F6_8 -167.9(9) . . . . ? C4_8 C1_8 C3_8 F6_8 -44.8(11) . . . . ? C2_8 C1_8 C3_8 F6_8 74.8(10) . . . . ? O1_8 C1_8 C3_8 F5_8 72.0(10) . . . . ? C4_8 C1_8 C3_8 F5_8 -165.0(8) . . . . ? C2_8 C1_8 C3_8 F5_8 -45.4(10) . . . . ? O1_8 C1_8 C4_8 F7_8 78.5(10) . . . . ? C3_8 C1_8 C4_8 F7_8 -42.8(10) . . . . ? C2_8 C1_8 C4_8 F7_8 -162.8(8) . . . . ? O1_8 C1_8 C4_8 F9_8 -42.6(11) . . . . ? C3_8 C1_8 C4_8 F9_8 -163.9(8) . . . . ? C2_8 C1_8 C4_8 F9_8 76.0(9) . . . . ? O1_8 C1_8 C4_8 F8_8 -161.8(8) . . . . ? C3_8 C1_8 C4_8 F8_8 76.9(10) . . . . ? C2_8 C1_8 C4_8 F8_8 -43.1(10) . . . . ? Al1 O1_9 C1_9 C2_9 149(6) . . . . ? Al1 O1_9 C1_9 C3_9 -90(6) . . . . ? Al1 O1_9 C1_9 C4_9 29(7) . . . . ? O1_9 C1_9 C2_9 F1_9 -47(2) . . . . ? C3_9 C1_9 C2_9 F1_9 -165.4(15) . . . . ? C4_9 C1_9 C2_9 F1_9 75.1(17) . . . . ? O1_9 C1_9 C2_9 F3_9 73(2) . . . . ? C3_9 C1_9 C2_9 F3_9 -46(2) . . . . ? C4_9 C1_9 C2_9 F3_9 -165.6(16) . . . . ? O1_9 C1_9 C2_9 F2_9 -166(2) . . . . ? C3_9 C1_9 C2_9 F2_9 75.5(18) . . . . ? C4_9 C1_9 C2_9 F2_9 -44.0(19) . . . . ? O1_9 C1_9 C3_9 F6_9 -166.5(19) . . . . ? C2_9 C1_9 C3_9 F6_9 -47.7(19) . . . . ? C4_9 C1_9 C3_9 F6_9 72.4(17) . . . . ? O1_9 C1_9 C3_9 F5_9 -47(2) . . . . ? C2_9 C1_9 C3_9 F5_9 72(2) . . . . ? C4_9 C1_9 C3_9 F5_9 -167.7(17) . . . . ? O1_9 C1_9 C3_9 F4_9 76(2) . . . . ? C2_9 C1_9 C3_9 F4_9 -165.6(15) . . . . ? C4_9 C1_9 C3_9 F4_9 -45.5(17) . . . . ? O1_9 C1_9 C4_9 F9_9 77(2) . . . . ? C2_9 C1_9 C4_9 F9_9 -43.0(18) . . . . ? C3_9 C1_9 C4_9 F9_9 -164.0(15) . . . . ? O1_9 C1_9 C4_9 F7_9 -43(2) . . . . ? C2_9 C1_9 C4_9 F7_9 -162.7(17) . . . . ? C3_9 C1_9 C4_9 F7_9 76.2(18) . . . . ? O1_9 C1_9 C4_9 F8_9 -162(3) . . . . ? C2_9 C1_9 C4_9 F8_9 78(2) . . . . ? C3_9 C1_9 C4_9 F8_9 -43(2) . . . . ? Al1 O1_7 C1_7 C2_7 109(7) . . . . ? Al1 O1_7 C1_7 C4_7 -11(8) . . . . ? Al1 O1_7 C1_7 C3_7 -130(7) . . . . ? O1_7 C1_7 C2_7 F2_7 164(3) . . . . ? C4_7 C1_7 C2_7 F2_7 -77(3) . . . . ? C3_7 C1_7 C2_7 F2_7 42(3) . . . . ? O1_7 C1_7 C2_7 F1_7 -75(3) . . . . ? C4_7 C1_7 C2_7 F1_7 44(3) . . . . ? C3_7 C1_7 C2_7 F1_7 164(2) . . . . ? O1_7 C1_7 C2_7 F3_7 43(3) . . . . ? C4_7 C1_7 C2_7 F3_7 162(2) . . . . ? C3_7 C1_7 C2_7 F3_7 -78(3) . . . . ? O1_7 C1_7 C3_7 F4_7 46(3) . . . . ? C2_7 C1_7 C3_7 F4_7 167(2) . . . . ? C4_7 C1_7 C3_7 F4_7 -73(2) . . . . ? O1_7 C1_7 C3_7 F6_7 166(3) . . . . ? C2_7 C1_7 C3_7 F6_7 -73(2) . . . . ? C4_7 C1_7 C3_7 F6_7 47(2) . . . . ? O1_7 C1_7 C3_7 F5_7 -74(3) . . . . ? C2_7 C1_7 C3_7 F5_7 46(2) . . . . ? C4_7 C1_7 C3_7 F5_7 165.9(19) . . . . ? O1_7 C1_7 C4_7 F8_7 164(3) . . . . ? C2_7 C1_7 C4_7 F8_7 44(3) . . . . ? C3_7 C1_7 C4_7 F8_7 -76(3) . . . . ? O1_7 C1_7 C4_7 F9_7 44(3) . . . . ? C2_7 C1_7 C4_7 F9_7 -76(3) . . . . ? C3_7 C1_7 C4_7 F9_7 164(3) . . . . ? O1_7 C1_7 C4_7 F7_7 -75(3) . . . . ? C2_7 C1_7 C4_7 F7_7 165(2) . . . . ? C3_7 C1_7 C4_7 F7_7 45(2) . . . . ? Al1 O1_6 C1_6 C3_6 -22(6) . . . . ? Al1 O1_6 C1_6 C2_6 -143(6) . . . . ? Al1 O1_6 C1_6 C4_6 97(6) . . . . ? O1_6 C1_6 C2_6 F1_6 -44(3) . . . . ? C3_6 C1_6 C2_6 F1_6 -166(2) . . . . ? C4_6 C1_6 C2_6 F1_6 76(2) . . . . ? O1_6 C1_6 C2_6 F2_6 -167(2) . . . . ? C3_6 C1_6 C2_6 F2_6 71(2) . . . . ? C4_6 C1_6 C2_6 F2_6 -47(2) . . . . ? O1_6 C1_6 C2_6 F3_6 78(2) . . . . ? C3_6 C1_6 C2_6 F3_6 -44(2) . . . . ? C4_6 C1_6 C2_6 F3_6 -162.1(17) . . . . ? O1_6 C1_6 C3_6 F5_6 -41(2) . . . . ? C2_6 C1_6 C3_6 F5_6 79.1(19) . . . . ? C4_6 C1_6 C3_6 F5_6 -161.8(18) . . . . ? O1_6 C1_6 C3_6 F6_6 -161(2) . . . . ? C2_6 C1_6 C3_6 F6_6 -40(2) . . . . ? C4_6 C1_6 C3_6 F6_6 79(2) . . . . ? O1_6 C1_6 C3_6 F4_6 79(2) . . . . ? C2_6 C1_6 C3_6 F4_6 -160.9(16) . . . . ? C4_6 C1_6 C3_6 F4_6 -41.9(18) . . . . ? O1_6 C1_6 C4_6 F9_6 74(2) . . . . ? C3_6 C1_6 C4_6 F9_6 -164.3(17) . . . . ? C2_6 C1_6 C4_6 F9_6 -46(2) . . . . ? O1_6 C1_6 C4_6 F7_6 -47(2) . . . . ? C3_6 C1_6 C4_6 F7_6 75.0(19) . . . . ? C2_6 C1_6 C4_6 F7_6 -166.2(19) . . . . ? O1_6 C1_6 C4_6 F8_6 -168(2) . . . . ? C3_6 C1_6 C4_6 F8_6 -46(2) . . . . ? C2_6 C1_6 C4_6 F8_6 73(2) . . . . ? Al1 O1_3 C1_3 C3_3 -56(4) . . . . ? Al1 O1_3 C1_3 C2_3 -177(3) . . . . ? Al1 O1_3 C1_3 C4_3 65(4) . . . . ? O1_3 C1_3 C2_3 F2_3 165(2) . . . . ? C3_3 C1_3 C2_3 F2_3 43(2) . . . . ? C4_3 C1_3 C2_3 F2_3 -76(2) . . . . ? O1_3 C1_3 C2_3 F1_3 -77(2) . . . . ? C3_3 C1_3 C2_3 F1_3 161.7(15) . . . . ? C4_3 C1_3 C2_3 F1_3 42.0(18) . . . . ? O1_3 C1_3 C2_3 F3_3 44(2) . . . . ? C3_3 C1_3 C2_3 F3_3 -76.6(18) . . . . ? C4_3 C1_3 C2_3 F3_3 163.7(16) . . . . ? O1_3 C1_3 C3_3 F6_3 164.9(19) . . . . ? C2_3 C1_3 C3_3 F6_3 -76.4(19) . . . . ? C4_3 C1_3 C3_3 F6_3 42.4(18) . . . . ? O1_3 C1_3 C3_3 F5_3 -74.3(18) . . . . ? C2_3 C1_3 C3_3 F5_3 44.4(17) . . . . ? C4_3 C1_3 C3_3 F5_3 163.3(14) . . . . ? O1_3 C1_3 C3_3 F4_3 44.0(19) . . . . ? C2_3 C1_3 C3_3 F4_3 162.7(16) . . . . ? C4_3 C1_3 C3_3 F4_3 -78.4(16) . . . . ? O1_3 C1_3 C4_3 F7_3 -84.2(17) . . . . ? C3_3 C1_3 C4_3 F7_3 38.4(16) . . . . ? C2_3 C1_3 C4_3 F7_3 159.0(14) . . . . ? O1_3 C1_3 C4_3 F9_3 38(2) . . . . ? C3_3 C1_3 C4_3 F9_3 160.2(18) . . . . ? C2_3 C1_3 C4_3 F9_3 -79.3(19) . . . . ? O1_3 C1_3 C4_3 F8_3 157.2(19) . . . . ? C3_3 C1_3 C4_3 F8_3 -80.2(19) . . . . ? C2_3 C1_3 C4_3 F8_3 40(2) . . . . ? Al1 O1_2 C1_2 C2_2 151(4) . . . . ? Al1 O1_2 C1_2 C3_2 -91(4) . . . . ? Al1 O1_2 C1_2 C4_2 30(4) . . . . ? O1_2 C1_2 C2_2 F1_2 -77.1(17) . . . . ? C3_2 C1_2 C2_2 F1_2 166.2(11) . . . . ? C4_2 C1_2 C2_2 F1_2 45.6(14) . . . . ? O1_2 C1_2 C2_2 F3_2 42.7(17) . . . . ? C3_2 C1_2 C2_2 F3_2 -74.1(15) . . . . ? C4_2 C1_2 C2_2 F3_2 165.4(12) . . . . ? O1_2 C1_2 C2_2 F2_2 163.8(15) . . . . ? C3_2 C1_2 C2_2 F2_2 47.1(14) . . . . ? C4_2 C1_2 C2_2 F2_2 -73.5(14) . . . . ? O1_2 C1_2 C3_2 F6_2 165.1(14) . . . . ? C2_2 C1_2 C3_2 F6_2 -77.6(14) . . . . ? C4_2 C1_2 C3_2 F6_2 42.9(14) . . . . ? O1_2 C1_2 C3_2 F5_2 -72.2(15) . . . . ? C2_2 C1_2 C3_2 F5_2 45.0(15) . . . . ? C4_2 C1_2 C3_2 F5_2 165.5(12) . . . . ? O1_2 C1_2 C3_2 F4_2 46.6(15) . . . . ? C2_2 C1_2 C3_2 F4_2 163.8(11) . . . . ? C4_2 C1_2 C3_2 F4_2 -75.7(13) . . . . ? O1_2 C1_2 C4_2 F7_2 -75.5(17) . . . . ? C2_2 C1_2 C4_2 F7_2 164.3(12) . . . . ? C3_2 C1_2 C4_2 F7_2 43.8(14) . . . . ? O1_2 C1_2 C4_2 F9_2 43.0(18) . . . . ? C2_2 C1_2 C4_2 F9_2 -77.2(14) . . . . ? C3_2 C1_2 C4_2 F9_2 162.3(12) . . . . ? O1_2 C1_2 C4_2 F8_2 163.6(18) . . . . ? C2_2 C1_2 C4_2 F8_2 43.4(17) . . . . ? C3_2 C1_2 C4_2 F8_2 -77.1(17) . . . . ? Al1 O1_1 C1_1 C3_1 -76(2) . . . . ? Al1 O1_1 C1_1 C4_1 46(2) . . . . ? Al1 O1_1 C1_1 C2_1 164(2) . . . . ? O1_1 C1_1 C2_1 F1_1 -41.9(14) . . . . ? C3_1 C1_1 C2_1 F1_1 -162.3(10) . . . . ? C4_1 C1_1 C2_1 F1_1 78.6(12) . . . . ? O1_1 C1_1 C2_1 F3_1 77.2(13) . . . . ? C3_1 C1_1 C2_1 F3_1 -43.2(12) . . . . ? C4_1 C1_1 C2_1 F3_1 -162.3(10) . . . . ? O1_1 C1_1 C2_1 F2_1 -162.2(13) . . . . ? C3_1 C1_1 C2_1 F2_1 77.5(13) . . . . ? C4_1 C1_1 C2_1 F2_1 -41.6(14) . . . . ? O1_1 C1_1 C3_1 F5_1 -38.2(14) . . . . ? C4_1 C1_1 C3_1 F5_1 -161.0(11) . . . . ? C2_1 C1_1 C3_1 F5_1 80.8(12) . . . . ? O1_1 C1_1 C3_1 F6_1 -160.6(11) . . . . ? C4_1 C1_1 C3_1 F6_1 76.6(12) . . . . ? C2_1 C1_1 C3_1 F6_1 -41.6(12) . . . . ? O1_1 C1_1 C3_1 F4_1 80.0(11) . . . . ? C4_1 C1_1 C3_1 F4_1 -42.8(11) . . . . ? C2_1 C1_1 C3_1 F4_1 -161.0(9) . . . . ? O1_1 C1_1 C4_1 F8_1 -163.3(12) . . . . ? C3_1 C1_1 C4_1 F8_1 -40.9(13) . . . . ? C2_1 C1_1 C4_1 F8_1 78.0(13) . . . . ? O1_1 C1_1 C4_1 F9_1 75.6(12) . . . . ? C3_1 C1_1 C4_1 F9_1 -162.0(10) . . . . ? C2_1 C1_1 C4_1 F9_1 -43.1(13) . . . . ? O1_1 C1_1 C4_1 F7_1 -43.3(14) . . . . ? C3_1 C1_1 C4_1 F7_1 79.1(12) . . . . ? C2_1 C1_1 C4_1 F7_1 -162.0(11) . . . . ? C1_10 O1_10 Al1 O1_9 36(8) . . . . ? C1_10 O1_10 Al1 O1_6 150(8) . . . . ? C1_10 O1_10 Al1 O1_7 -94(8) . . . . ? C1_2 O1_2 Al1 O1_3 30(4) . . . . ? C1_2 O1_2 Al1 O1_1 -88(4) . . . . ? C1_2 O1_2 Al1 O1_8 154(4) . . . . ? C1_9 O1_9 Al1 O1_10 153(6) . . . . ? C1_9 O1_9 Al1 O1_6 45(7) . . . . ? C1_9 O1_9 Al1 O1_7 -75(7) . . . . ? C1_11 O1_11 Al1 O1_12 -102(6) . . . . ? C1_12 O1_12 Al1 O1_11 -81(12) . . . . ? C1_3 O1_3 Al1 O1_2 -158(4) . . . . ? C1_3 O1_3 Al1 O1_1 -39(4) . . . . ? C1_3 O1_3 Al1 O1_8 80(4) . . . . ? C1_6 O1_6 Al1 O1_10 92(6) . . . . ? C1_6 O1_6 Al1 O1_9 -157(6) . . . . ? C1_6 O1_6 Al1 O1_7 -33(6) . . . . ? C1_1 O1_1 Al1 O1_2 -85(2) . . . . ? C1_1 O1_1 Al1 O1_3 158(2) . . . . ? C1_1 O1_1 Al1 O1_8 35(2) . . . . ? C1_7 O1_7 Al1 O1_10 62(8) . . . . ? C1_7 O1_7 Al1 O1_9 -63(8) . . . . ? C1_7 O1_7 Al1 O1_6 175(7) . . . . ? C1_8 O1_8 Al1 O1_2 -39.7(16) . . . . ? C1_8 O1_8 Al1 O1_3 81.1(16) . . . . ? C1_8 O1_8 Al1 O1_1 -159.3(13) . . . . ? F1B C1A C2A F2B 4(2) . . . . ? C6A C1A C2A F2B -178.3(16) . . . . ? Ta1 C1A C2A F2B 127.0(19) . . . . ? F1B C1A C2A C3A 179.6(11) . . . . ? C6A C1A C2A C3A -2.3(19) . . . . ? Ta1 C1A C2A C3A -57.0(12) . . . . ? F1B C1A C2A Ta1 -123.4(10) . . . . ? C6A C1A C2A Ta1 54.6(10) . . . . ? F2B C2A C3A C4A 168.0(13) . . . . ? C1A C2A C3A C4A -9(2) . . . . ? Ta1 C2A C3A C4A -67.6(11) . . . . ? F2B C2A C3A Ta1 -124.4(12) . . . . ? C1A C2A C3A Ta1 58.6(12) . . . . ? C2A C3A C4A C5A 14.6(19) . . . . ? Ta1 C3A C4A C5A -50.3(12) . . . . ? C2A C3A C4A Ta1 64.9(10) . . . . ? C3A C4A C5A C6A -9(2) . . . . ? Ta1 C4A C5A C6A -59.2(10) . . . . ? C3A C4A C5A Ta1 49.9(12) . . . . ? F1B C1A C6A C5A -173.7(10) . . . . ? C2A C1A C6A C5A 8.3(16) . . . . ? Ta1 C1A C6A C5A 62.6(9) . . . . ? F1B C1A C6A Ta1 123.7(11) . . . . ? C2A C1A C6A Ta1 -54.3(10) . . . . ? C4A C5A C6A C1A -3.1(17) . . . . ? Ta1 C5A C6A C1A -63.7(9) . . . . ? C4A C5A C6A Ta1 60.5(10) . . . . ? _refine_diff_density_max 1.422 _refine_diff_density_min -1.738 _refine_diff_density_rms 0.146 _shelx_res_file ; TITL p21n_all_a.res in P2(1)/n p21n_all_a.res created by SHELXL-2018/3 at 09:58:14 on 12-Feb-2019 REM Old TITL p21n_all in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.185, Rweak 0.011, Alpha 0.066, Orientation as input REM Formula found by SHELXT: C40 O12 F27 Al Ta CELL 0.71073 13.0435 18.7956 15.9397 90.000 94.046 90.000 ZERR 4.000 0.0006 0.0008 0.0007 0.000 0.002 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C O F AL TA H UNIT 104 32.0001 152.001 4 4.32 16 EADP F6_9 F6_2 EADP F2_10 F8_8 EADP F1_1 F7_11 EADP F9_11 F4_7 EADP F9_7 F7_1 EADP C1_8 C1_10 EADP O1_8 O1_10 EADP F1_9 F1_2 EADP C1_9 C1_2 EADP O1_9 O1_2 EADP F1_1 F2_1 EADP O1_7 O1_1 TEMP -173.150 L.S. 10 LIST 4 ACTA CONF BOND FMAP 2 PLAN 60 OMIT 6 4 1 OMIT -6 5 3 REM Restraints for Fragment oc(cf3)3, Nonafluoro-tert-butoxy, [(CF3)3CO]- REM from: TURBOMOLE V6.0 B-P86/def-SV(P). Please cite REM doi:10.1107/S1600576715005580 SADI_CCF3 0.02 C1 C2 C1 C3 C1 C4 SADI_CCF3 0.02 F1 C2 F2 C2 F3 C2 F4 C3 F5 C3 F6 C3 F7 C4 F8 C4 F9 C4 SADI_CCF3 0.04 C2 C3 C3 C4 C2 C4 SADI_CCF3 0.04 O1 C2 O1 C3 O1 C4 SADI_CCF3 0.04 F1 F2 F2 F3 F3 F1 F4 F5 F5 F6 F6 F4 F7 F8 F8 F9 F9 F7 SADI_CCF3 0.1 F1 C1 F2 C1 F3 C1 F4 C1 F5 C1 F6 C1 F7 C1 F8 C1 F9 C1 SIMU_CCF3 O1 > F9 RIGU_CCF3 O1 > F9 SADI_CCF3 0.02 O1 C1 SAME_CCF3 O1 > F9 SIMU 0.04 0.08 1 SIMU 0.02 0.05 0.55 SADI Al1 O1_3 Al1 O1_6 Al1 O1_9 Al1 O1_2 Al1 O1_7 Al1 O1_1 Al1 O1_8 = AL1 O1_10 AL1 O1_11 AL1 O1_12 SUMP 1 0.0001 1 2 1 9 1 5 SUMP 1 0.0001 1 4 1 6 1 7 REM Restraints for Fragment dimof, Ta fragment from: ShelXle DSR GUI. REM Please cite https://doi.org/10.1107/S1600576718004508 REM RESI TAFR 13 WGHT 0.052700 55.595306 FVAR 0.22146 0.72480 0.59429 0.50620 0.05586 0.38090 0.11291 FVAR 0.86529 0.21934 RESI CCF3 12 PART 3 71 O1 2 0.241598 0.348889 0.633420 71.00000 0.03551 0.02165 = 0.03411 -0.00783 0.00639 -0.00660 C1 1 0.240434 0.301945 0.570031 71.00000 0.04130 0.02506 = 0.03382 -0.00942 -0.00190 -0.00108 C2 1 0.244511 0.224626 0.604561 71.00000 0.06849 0.02235 = 0.04073 -0.01137 0.00291 -0.00301 F1 3 0.338772 0.206928 0.633317 71.00000 0.07375 0.06549 = 0.04316 0.03326 0.00767 0.00587 F2 3 0.213293 0.179022 0.544191 71.00000 0.14291 0.03047 = 0.05291 -0.02093 -0.00688 -0.01595 F3 3 0.183174 0.217355 0.666932 71.00000 0.07810 0.02775 = 0.05387 -0.00173 0.01308 -0.00595 C3 1 0.139129 0.308854 0.512876 71.00000 0.04782 0.07232 = 0.06209 -0.00433 -0.02187 -0.00752 F4 3 0.111872 0.375961 0.500356 71.00000 0.03081 0.07933 = 0.10730 0.00780 -0.03965 -0.00126 F5 3 0.065009 0.274552 0.548821 71.00000 0.04321 0.10924 = 0.10367 0.03324 -0.02266 -0.00675 F6 3 0.150662 0.278708 0.438609 71.00000 0.08876 0.09040 = 0.06572 -0.02210 -0.03167 -0.03991 C4 1 0.330738 0.313259 0.513515 71.00000 0.04744 0.03214 = 0.02905 -0.01106 0.00141 0.00326 F7 3 0.314370 0.370616 0.465454 71.00000 0.06055 0.05241 = 0.05191 0.01027 0.01846 0.01974 F8 3 0.341822 0.257668 0.463394 71.00000 0.07230 0.05087 = 0.05838 -0.03267 0.01653 0.00434 F9 3 0.418610 0.323198 0.559159 71.00000 0.04945 0.07956 = 0.04812 -0.00139 -0.00531 -0.01467 PART 0 RESI 0 REM REM DSR PUT OC(CF3)3 WITH O1 C1 F4 ON O1_6B Q67 Q8 PART 3 OCC 121 RESI REM !CCF3 RESI CCF3 11 PART 3 51 O1 2 0.390115 0.423340 0.727277 51.00000 0.03770 0.02344 = 0.03431 0.00987 -0.00953 -0.00951 C1 1 0.438912 0.409727 0.802894 51.00000 0.03304 0.03251 = 0.03284 0.00634 -0.00854 -0.00304 C2 1 0.546751 0.444916 0.808333 51.00000 0.03166 0.03569 = 0.05661 -0.00102 -0.00795 -0.00384 F1 3 0.614144 0.404631 0.771970 51.00000 0.03212 0.03077 = 0.06381 -0.00416 -0.00274 -0.00978 F2 3 0.578958 0.456367 0.888287 51.00000 0.03538 0.05070 = 0.06448 -0.01252 -0.01806 0.00797 F3 3 0.542156 0.507533 0.769280 51.00000 0.02796 0.03747 = 0.07418 0.00509 -0.00167 -0.00347 C3 1 0.378048 0.442710 0.873396 51.00000 0.03878 0.05107 = 0.03858 0.00909 -0.00324 0.01101 F4 3 0.277786 0.441757 0.852463 51.00000 0.03601 0.08192 = 0.08302 0.03161 -0.00713 0.00846 F5 3 0.406939 0.510173 0.885001 51.00000 0.05376 0.05202 = 0.02398 0.00466 0.00431 0.00988 F6 3 0.395186 0.408930 0.946142 51.00000 0.03522 0.05609 = 0.04169 0.01441 0.00612 0.01903 C4 1 0.449193 0.328311 0.815270 51.00000 0.04207 0.03186 = 0.03052 0.00912 -0.01320 -0.00371 F7 3 0.359900 0.301274 0.835216 51.00000 0.04871 0.04929 = 0.04794 0.02458 -0.01544 -0.01446 F8 3 0.520461 0.310744 0.875151 51.00000 0.04704 0.03832 = 0.03142 0.00783 -0.01418 0.00403 F9 3 0.472516 0.297102 0.743998 51.00000 0.02545 0.03705 = 0.03491 -0.00109 -0.01836 -0.00967 PART 0 RESI 0 REM REM DSR PUT OC(CF3)3 WITH O1 C1 C4 ON Q64 C1_7B Q18 PART 3 OCC 101 RESI REM !CCF3 RESI CCF3 10 PART 2 -81 O1 2 0.274750 0.493622 0.617791 -81.00000 0.03387 0.01650 = 0.02760 0.00775 0.00028 -0.00362 C1 1 0.269325 0.561128 0.590299 -81.00000 0.02744 0.01445 = 0.02450 0.00448 0.00535 -0.00034 C2 1 0.171621 0.567503 0.529030 -81.00000 0.03711 0.04364 = 0.02764 0.01636 -0.00321 -0.01210 F1 3 0.189570 0.535534 0.457324 -81.00000 0.06169 0.08699 = 0.02929 0.00115 -0.00883 0.00493 F2 3 0.144902 0.634819 0.516482 -81.00000 0.05068 0.04820 = 0.04628 0.02317 -0.01446 -0.01283 F3 3 0.094238 0.533646 0.561824 -81.00000 0.03825 0.05299 = 0.03296 0.01602 -0.01177 -0.02536 C3 1 0.261304 0.615602 0.662061 -81.00000 0.04379 0.03197 = 0.04296 -0.01406 0.00486 0.00362 F4 3 0.331530 0.603161 0.724468 -81.00000 0.05781 0.09270 = 0.04805 -0.02184 -0.01004 0.00402 F5 3 0.168099 0.614537 0.690142 -81.00000 0.04754 0.06861 = 0.04800 -0.02028 0.01242 0.00643 F6 3 0.276719 0.681365 0.634234 -81.00000 0.07296 0.02537 = 0.10091 -0.01868 0.01254 -0.00567 C4 1 0.366271 0.578123 0.543005 -81.00000 0.03261 0.04358 = 0.04205 0.01779 0.01763 0.00729 F7 3 0.443238 0.597147 0.597598 -81.00000 0.03160 0.06653 = 0.05064 0.02935 0.01419 -0.00617 F8 3 0.349588 0.630948 0.488341 -81.00000 0.04194 0.06108 = 0.04637 0.02994 0.03016 0.02070 F9 3 0.395341 0.520808 0.502188 -81.00000 0.05517 0.06303 = 0.05326 0.01322 0.02260 0.03249 PART 0 RESI 0 REM REM DSR PUT OC(CF3)3 WITH O1 C1 F2 ON O1_8A Q113 Q4 PART 2 OCC -81 RESI REM !CCF3 RESI CCF3 8 PART 1 81 O1 2 0.304679 0.501051 0.635530 81.00000 0.03387 0.01650 = 0.02760 0.00775 0.00028 -0.00362 C1 1 0.279849 0.560662 0.589958 81.00000 0.02744 0.01445 = 0.02450 0.00448 0.00535 -0.00034 C2 1 0.371730 0.577010 0.535736 81.00000 0.03465 0.03965 = 0.03314 0.00972 0.01548 0.00401 F1 3 0.371329 0.532994 0.470398 81.00000 0.05619 0.04897 = 0.03191 0.00193 0.01956 0.00359 F2 3 0.368844 0.644173 0.507399 81.00000 0.04733 0.03594 = 0.05093 0.01941 0.00611 -0.00898 F3 3 0.460359 0.570283 0.581385 81.00000 0.03336 0.04693 = 0.04843 0.01411 0.00970 0.00513 C3 1 0.263765 0.623135 0.650355 81.00000 0.04812 0.02543 = 0.03653 0.00047 0.00785 0.00543 F4 3 0.203392 0.603776 0.709898 81.00000 0.05838 0.02569 = 0.04032 -0.00190 0.01935 0.00463 F5 3 0.353639 0.644465 0.687419 81.00000 0.05444 0.02256 = 0.04561 -0.00535 -0.00637 -0.00607 F6 3 0.220291 0.679019 0.610548 81.00000 0.06130 0.02004 = 0.05774 0.00659 0.00658 0.01476 C4 1 0.181456 0.550639 0.531435 81.00000 0.03732 0.02836 = 0.03561 0.01170 0.00225 -0.00625 F7 3 0.097778 0.556156 0.574500 81.00000 0.02322 0.05454 = 0.05959 0.01434 0.00564 -0.00741 F8 3 0.172675 0.599670 0.469656 81.00000 0.05068 0.04820 = 0.04628 0.02317 -0.01446 -0.01283 F9 3 0.181342 0.487205 0.493833 81.00000 0.06699 0.03783 = 0.04032 -0.00552 -0.01494 -0.00557 PART 0 RESI 0 REM REM DSR REPLACE OC(CF3)3 WITH O1 C1 C4 ON O1_4 C1_4 C2_4 PART 1 OCC 81 REM !RESI CCF3 RESI 9 CCF3 PART 2 -31 O1 2 0.161855 0.446690 0.743541 -31.00000 0.03308 0.02684 = 0.03934 0.00026 0.01581 -0.00153 C1 1 0.082617 0.429648 0.789222 -31.00000 0.02315 0.02026 = 0.03193 0.00072 0.00454 -0.00124 C2 1 0.066426 0.490941 0.851603 -31.00000 0.04246 0.03092 = 0.03846 -0.00216 0.01692 0.00973 F1 3 0.155315 0.510756 0.889881 -31.00000 0.06409 0.05631 = 0.03690 -0.00846 0.00208 -0.00666 F2 3 0.006100 0.473199 0.912142 -31.00000 0.08054 0.08369 = 0.04776 0.00343 0.04476 0.01610 F3 3 0.025541 0.546836 0.810696 -31.00000 0.06673 0.04177 = 0.06839 0.00863 0.02752 0.03012 C3 1 -0.013866 0.419096 0.728294 -31.00000 0.03642 0.04926 = 0.04888 0.01926 -0.00919 -0.01517 F4 3 -0.008930 0.356667 0.688303 -31.00000 0.06269 0.06779 = 0.05553 -0.00238 -0.01295 -0.03728 F5 3 -0.024414 0.471552 0.672634 -31.00000 0.05020 0.07802 = 0.06171 0.03972 -0.02750 -0.02745 F6 3 -0.099283 0.417164 0.767730 -31.00000 0.02654 0.05692 = 0.06267 0.02113 -0.01442 -0.01707 C4 1 0.103329 0.359497 0.838865 -31.00000 0.03899 0.02284 = 0.03720 0.00608 -0.00153 -0.00002 F7 3 0.144831 0.312008 0.790020 -31.00000 0.11701 0.02454 = 0.04853 0.00335 0.02277 0.01007 F8 3 0.017454 0.331546 0.864952 -31.00000 0.05190 0.04929 = 0.05467 0.02240 -0.00189 -0.01882 F9 3 0.167223 0.370217 0.905669 -31.00000 0.03620 0.04688 = 0.04047 0.01029 -0.00442 0.00284 PART 0 RESI 0 REM REM DSR PUT OC(CF3)3 WITH O1 C1 C4 ON O1_2A C1_2A Q14 PART 2 OCC -31 REM !RESI CCF3 REM REM DSR PUT 12-DIFLUOROBENZ WITH C2 C1 F1 ON Q42 C1_5A Q24 PART 2 OCC REM !-61 RESI FBEN RESI 7 CCF3 PART 2 91 O1 2 0.372821 0.401125 0.749627 91.00000 0.02842 0.02807 = 0.03105 0.01119 -0.01038 -0.00838 C1 1 0.450285 0.413714 0.809223 91.00000 0.02703 0.02837 = 0.03049 -0.00157 -0.01094 -0.00037 C2 1 0.430424 0.371582 0.889987 91.00000 0.03513 0.03682 = 0.03245 0.00082 -0.00626 -0.00141 F1 3 0.356811 0.401355 0.931954 91.00000 0.06126 0.06928 = 0.03382 0.00924 0.00862 0.02202 F2 3 0.511765 0.364646 0.944549 91.00000 0.03788 0.05054 = 0.03746 0.02357 -0.00796 -0.01167 F3 3 0.398221 0.306742 0.866852 91.00000 0.07093 0.03904 = 0.04770 0.00057 0.00333 -0.01868 C3 1 0.554947 0.390606 0.777545 91.00000 0.02850 0.03540 = 0.03428 -0.00398 -0.01076 -0.00130 F4 3 0.565152 0.413532 0.700134 91.00000 0.02545 0.03705 = 0.03491 -0.00109 -0.01836 -0.00967 F5 3 0.564254 0.319994 0.777942 91.00000 0.03028 0.03318 = 0.05177 -0.00042 0.00722 0.00320 F6 3 0.632922 0.416690 0.826640 91.00000 0.02731 0.05280 = 0.02412 -0.00388 -0.00690 -0.00564 C4 1 0.453604 0.494424 0.828911 91.00000 0.04660 0.03060 = 0.04464 -0.00514 -0.01337 0.00181 F7 3 0.494707 0.529406 0.766732 91.00000 0.03834 0.01800 = 0.05091 -0.00326 -0.01604 0.00648 F8 3 0.508112 0.508594 0.900443 91.00000 0.05208 0.05183 = 0.04601 -0.02114 -0.01050 -0.00411 F9 3 0.359359 0.520006 0.835682 91.00000 0.05907 0.03547 = 0.04833 -0.00556 -0.00506 0.01538 PART 0 RESI 0 REM REM DSR PUT OC(CF3)3 WITH O1 C1 C4 ON O1_1A C1_1A Q33 PART 2 OCC -21 REM !RESI CCF3 RESI 6 CCF3 PART 2 61 O1 2 0.234559 0.356597 0.621369 61.00000 0.03572 0.02497 = 0.02787 -0.00915 0.00121 -0.00371 C1 1 0.262121 0.300722 0.574257 61.00000 0.03654 0.02145 = 0.03118 -0.00916 0.00452 -0.00723 C2 1 0.189697 0.297725 0.493149 61.00000 0.04775 0.05495 = 0.03063 -0.01407 0.00134 -0.01340 F1 3 0.092776 0.308234 0.510039 61.00000 0.04166 0.11072 = 0.08656 0.00546 0.00086 0.00582 F2 3 0.195638 0.237415 0.450308 61.00000 0.08326 0.07385 = 0.05032 -0.03833 -0.00353 -0.01796 F3 3 0.219055 0.347174 0.439415 61.00000 0.08476 0.07232 = 0.02955 0.00066 -0.00464 -0.02358 C3 1 0.374573 0.307059 0.550275 61.00000 0.03899 0.03378 = 0.04374 -0.00846 0.00862 -0.00372 F4 3 0.440594 0.288147 0.614468 61.00000 0.03249 0.05054 = 0.04920 -0.01428 0.00436 0.00021 F5 3 0.394167 0.373753 0.529568 61.00000 0.05420 0.03869 = 0.05988 -0.00174 0.03401 -0.00975 F6 3 0.391354 0.265815 0.485033 61.00000 0.04332 0.04979 = 0.04645 -0.01501 0.00428 0.01715 C4 1 0.252972 0.230520 0.624780 61.00000 0.06126 0.02527 = 0.05596 0.00006 0.01619 -0.00475 F7 3 0.296660 0.239120 0.702097 61.00000 0.05761 0.03792 = 0.05552 0.01592 0.01825 -0.00536 F8 3 0.298138 0.176885 0.587179 61.00000 0.10784 0.01996 = 0.10737 -0.01294 0.03818 -0.00004 F9 3 0.155032 0.212737 0.629034 61.00000 0.06914 0.03999 = 0.05507 0.00845 0.01209 -0.02427 PART 0 RESI 0 REM REM DSR PUT OC(CF3)3 WITH O1 C1 C4 ON O1_3A C1_3A Q14 PART 2 OCC -41 REM !RESI CCF3 REM REM DSR REPLACE OC(CF3)3 WITH O1 C1 C4 ON O2 C019 C01H PART 1 OCC 51 REM !RESI CCF3 RESI 3 CCF3 PART 1 41 O1 2 0.232803 0.356093 0.622813 41.00000 0.03472 0.02146 = 0.02756 -0.00756 0.00219 -0.00011 C1 1 0.267965 0.300747 0.578165 41.00000 0.03657 0.01924 = 0.03562 -0.00990 0.00604 -0.00554 C2 1 0.172891 0.265389 0.531222 41.00000 0.04802 0.08837 = 0.09258 -0.06102 0.00694 -0.02222 F1 3 0.124368 0.225843 0.585171 41.00000 0.06554 0.07471 = 0.16999 -0.07320 0.05276 -0.04726 F2 3 0.200482 0.222500 0.470519 41.00000 0.07058 0.12612 = 0.12525 -0.10533 0.00730 -0.02647 F3 3 0.109595 0.314417 0.496401 41.00000 0.04498 0.14563 = 0.08155 -0.07031 -0.02202 -0.00061 C3 1 0.344617 0.326505 0.515285 41.00000 0.04725 0.03122 = 0.02059 -0.00391 0.00353 0.00291 F4 3 0.409081 0.373046 0.553493 41.00000 0.04216 0.02875 = 0.04283 -0.00641 0.01560 -0.01050 F5 3 0.293090 0.358999 0.451512 41.00000 0.06946 0.08331 = 0.03455 0.00480 0.00355 0.04243 F6 3 0.399567 0.275025 0.484348 41.00000 0.04906 0.03425 = 0.03516 -0.00248 0.01937 0.00200 C4 1 0.320863 0.244269 0.637903 41.00000 0.07529 0.02044 = 0.05726 0.01319 0.03338 0.01778 F7 3 0.417789 0.261833 0.657779 41.00000 0.07514 0.05375 = 0.03759 0.00028 0.01273 0.03492 F8 3 0.322683 0.180114 0.602399 41.00000 0.11248 0.01747 = 0.12425 -0.00035 0.05507 0.00804 F9 3 0.270051 0.238692 0.706761 41.00000 0.12701 0.05549 = 0.09378 0.04971 0.07575 0.03817 PART 0 RESI 0 REM REM DSR REPLACE OC(CF3)3 WITH O1 C1 C4 ON O1 C015 C028 PART 1 OCC 41 REM !RESI CCF3 RESI 2 CCF3 PART 1 31 O1 2 0.160311 0.446017 0.741736 31.00000 0.03308 0.02684 = 0.03934 0.00026 0.01581 -0.00153 C1 1 0.074503 0.425016 0.776103 31.00000 0.02315 0.02026 = 0.03193 0.00072 0.00454 -0.00124 C2 1 0.057367 0.474359 0.851319 31.00000 0.04133 0.03251 = 0.04005 -0.00610 0.01667 -0.00162 F1 3 0.120003 0.457038 0.917301 31.00000 0.06409 0.05631 = 0.03690 -0.00846 0.00208 -0.00666 F2 3 -0.037694 0.470147 0.876148 31.00000 0.04520 0.03467 = 0.05897 -0.00956 0.02837 -0.00070 F3 3 0.075463 0.541747 0.831777 31.00000 0.05066 0.03024 = 0.05927 -0.01396 0.01826 -0.00855 C3 1 -0.015833 0.433542 0.708007 31.00000 0.02656 0.02674 = 0.04897 0.00832 -0.00206 -0.00264 F4 3 0.009426 0.406495 0.634671 31.00000 0.05121 0.05166 = 0.04576 -0.00605 -0.01185 0.00002 F5 3 -0.038759 0.501693 0.694761 31.00000 0.02762 0.03257 = 0.05635 0.01193 0.00909 0.00639 F6 3 -0.099814 0.399658 0.726722 31.00000 0.02654 0.05692 = 0.06267 0.02113 -0.01442 -0.01707 C4 1 0.080998 0.346444 0.806556 31.00000 0.03357 0.02304 = 0.04913 0.00590 0.00550 0.00405 F7 3 0.069765 0.301682 0.742424 31.00000 0.05054 0.02143 = 0.06423 -0.00302 0.01543 -0.00798 F8 3 0.009664 0.331009 0.859285 31.00000 0.04579 0.03037 = 0.05094 0.00905 0.01042 -0.00964 F9 3 0.172134 0.333151 0.845593 31.00000 0.03618 0.03499 = 0.08432 0.02858 -0.00595 -0.00026 PART 0 RESI 0 REM REM DSR REPLACE OC(CF3)3 WITH O1 C1 C4 ON O3 C013 C01Z PART 1 OCC 31 REM !RESI CCF3 RESI 1 CCF3 PART 1 21 O1 2 0.365382 0.400130 0.756969 21.00000 0.02842 0.02807 = 0.03105 0.01119 -0.01038 -0.00838 C1 1 0.446149 0.419388 0.810102 21.00000 0.01804 0.02719 = 0.02404 0.00077 -0.00505 -0.00216 C2 1 0.477683 0.354340 0.866326 21.00000 0.03639 0.03447 = 0.04959 0.01478 -0.00950 0.00088 F1 3 0.396918 0.320485 0.891894 21.00000 0.04871 0.04929 = 0.04794 0.02458 -0.01544 -0.01446 F2 3 0.535862 0.374555 0.935045 21.00000 0.04871 0.04929 = 0.04794 0.02458 -0.01544 -0.01446 F3 3 0.530101 0.308052 0.823669 21.00000 0.06358 0.02954 = 0.08113 0.00039 -0.00999 0.01023 C3 1 0.538324 0.441922 0.760178 21.00000 0.02874 0.03796 = 0.02998 0.00285 0.00293 -0.00490 F4 3 0.524074 0.508886 0.732639 21.00000 0.03768 0.04298 = 0.04245 0.01434 -0.00372 -0.01311 F5 3 0.545798 0.401563 0.694016 21.00000 0.06249 0.06369 = 0.04889 -0.02202 0.02466 -0.01830 F6 3 0.627061 0.440019 0.807140 21.00000 0.02312 0.05263 = 0.05200 0.01324 0.00372 -0.00330 C4 1 0.416976 0.481220 0.868263 21.00000 0.04258 0.04147 = 0.02972 -0.00517 0.00292 0.00567 F7 3 0.361959 0.530158 0.824191 21.00000 0.05907 0.03547 = 0.04833 -0.00556 -0.00506 0.01538 F8 3 0.497317 0.514414 0.905503 21.00000 0.06058 0.04048 = 0.03787 -0.01062 -0.00847 0.00010 F9 3 0.360086 0.457588 0.928074 21.00000 0.06599 0.08051 = 0.03626 -0.00024 0.02054 0.00773 PART 0 RESI 0 AL1 4 0.264994 0.426270 0.687862 11.00000 0.02210 0.01290 = 0.01783 0.00141 0.00016 -0.00165 PART 2 TA1B 5 0.247569 0.320046 0.217183 10.08000 0.04067 0.02412 = 0.03214 0.00081 0.00528 -0.00927 PART 0 PART 1 11 TA1 5 0.233978 0.350361 0.176324 11.00000 0.03324 0.02743 = 0.03168 -0.00858 0.00499 -0.00135 C1A 1 0.298116 0.235961 0.235216 11.00000 0.06847 0.04305 = 0.04783 0.00297 0.01971 0.03151 C2A 1 0.373376 0.289155 0.251874 11.00000 0.06668 0.08638 = 0.06214 -0.04235 -0.04148 0.04795 C3A 1 0.415400 0.330735 0.187274 11.00000 0.02293 0.07411 = 0.06988 -0.03862 0.00604 0.00392 AFIX 13 H3A 6 0.466291 0.369796 0.199639 11.00000 -1.20000 AFIX 0 C4A 1 0.388196 0.308301 0.108666 11.00000 0.06315 0.04718 = 0.07889 -0.01723 0.02573 0.01600 AFIX 13 H4A 6 0.411798 0.337542 0.061286 11.00000 -1.20000 AFIX 0 C5A 1 0.308361 0.260680 0.089754 11.00000 0.06488 0.04748 = 0.03172 -0.01927 0.00981 0.02212 AFIX 13 H5A 6 0.281013 0.254871 0.029945 11.00000 -1.20000 AFIX 0 C6A 1 0.260524 0.225178 0.152776 11.00000 0.04744 0.03024 = 0.07284 -0.02022 0.01388 0.00868 AFIX 13 H6A 6 0.201178 0.192537 0.138969 11.00000 -1.20000 AFIX 0 F1B 3 0.263287 0.199551 0.297363 11.00000 0.08910 0.06571 = 0.07828 0.01548 0.03284 0.03000 F2B 3 0.422091 0.309311 0.319392 11.00000 0.23291 0.15982 = 0.19997 0.01027 0.05535 0.07600 C1B 1 0.238142 0.444612 0.104046 11.00000 0.02740 0.04561 = 0.02755 -0.00359 0.00258 -0.00720 O1B 2 0.240910 0.495295 0.067431 11.00000 0.05837 0.05684 = 0.03229 0.01115 -0.00439 -0.00959 C2B 1 0.101811 0.350190 0.094208 11.00000 0.04526 0.04273 = 0.03248 -0.01180 -0.00052 -0.01075 O2B 2 0.030998 0.351546 0.049942 11.00000 0.04644 0.06214 = 0.04655 -0.00675 -0.00087 -0.01048 C3B 1 0.107689 0.341880 0.253953 11.00000 0.04667 0.01952 = 0.04104 -0.00505 0.00624 0.01043 O3B 2 0.043339 0.337649 0.294987 11.00000 0.04741 0.03518 = 0.06008 0.00592 0.02865 -0.00022 C4B 1 0.250295 0.431290 0.265154 11.00000 0.02146 0.03110 = 0.02284 0.00052 0.00558 0.00117 O4B 2 0.260619 0.475740 0.313692 11.00000 0.06117 0.03331 = 0.02752 -0.00814 0.00794 -0.00833 PART 0 HKLF 4 REM p21n_all_a.res in P2(1)/n REM wR2 = 0.1381, GooF = S = 1.146, Restrained GooF = 0.646 for all data REM R1 = 0.0510 for 4981 Fo > 4sig(Fo) and 0.0566 for all 5664 data REM 1368 parameters refined using 16241 restraints END WGHT 0.0524 55.6529 REM Highest difference peak 1.422, deepest hole -1.738, 1-sigma level 0.146 Q1 1 0.1970 0.3531 0.1181 11.00000 0.05 1.42 Q2 1 0.0761 0.3496 0.1759 11.00000 0.05 1.32 Q3 1 -0.1020 0.4531 0.8049 11.00000 0.05 1.02 Q4 1 0.1667 0.4488 0.3233 11.00000 0.05 0.86 Q5 1 0.2670 0.3514 0.2426 11.00000 0.05 0.81 Q6 1 0.3467 0.4505 0.3239 11.00000 0.05 0.78 Q7 1 0.3143 0.4270 0.7833 11.00000 0.05 0.72 Q8 1 0.0923 0.1484 0.6740 11.00000 0.05 0.68 Q9 1 0.4574 0.4164 0.6738 11.00000 0.05 0.68 Q10 1 0.3428 0.3506 0.1798 11.00000 0.05 0.66 Q11 1 0.4493 0.3253 0.0635 11.00000 0.05 0.63 Q12 1 0.1865 0.5158 0.8618 11.00000 0.05 0.59 Q13 1 0.5517 0.4442 0.9230 11.00000 0.05 0.58 Q14 1 0.1652 0.3334 0.2207 11.00000 0.05 0.56 Q15 1 0.3362 0.3580 0.0993 11.00000 0.05 0.54 Q16 1 0.0880 0.3506 0.4780 11.00000 0.05 0.53 Q17 1 0.1337 0.5107 0.9051 11.00000 0.05 0.52 Q18 1 0.1645 0.4560 0.0439 11.00000 0.05 0.52 Q19 1 0.3327 0.4489 1.0244 11.00000 0.05 0.52 Q20 1 0.0724 0.3858 0.5437 11.00000 0.05 0.52 Q21 1 0.2309 0.4350 0.6855 11.00000 0.05 0.51 Q22 1 0.1873 0.4078 0.7689 11.00000 0.05 0.51 Q23 1 0.1615 0.2718 0.6866 11.00000 0.05 0.50 Q24 1 0.1533 0.2637 0.0928 11.00000 0.05 0.49 Q25 1 0.3414 0.4881 0.5058 11.00000 0.05 0.49 Q26 1 0.2408 0.5589 0.5738 11.00000 0.05 0.48 Q27 1 -0.0076 0.5463 0.6767 11.00000 0.05 0.48 Q28 1 0.4205 0.3504 0.1759 11.00000 0.05 0.48 Q29 1 0.2084 0.3777 0.5478 11.00000 0.05 0.48 Q30 1 0.2616 0.1974 0.6398 11.00000 0.05 0.47 Q31 1 0.1087 0.4292 0.6950 11.00000 0.05 0.47 Q32 1 0.3518 0.2478 0.6608 11.00000 0.05 0.47 Q33 1 0.1711 0.6438 0.6734 11.00000 0.05 0.47 Q34 1 0.4114 0.3028 0.8142 11.00000 0.05 0.46 Q35 1 0.0843 0.2905 0.6125 11.00000 0.05 0.46 Q36 1 0.2293 0.2885 0.2436 11.00000 0.05 0.46 Q37 1 0.3175 0.4291 0.7253 11.00000 0.05 0.46 Q38 1 0.2557 0.1754 0.3423 11.00000 0.05 0.46 Q39 1 -0.0132 0.5136 0.8935 11.00000 0.05 0.45 Q40 1 0.2390 0.3389 0.2943 11.00000 0.05 0.44 Q41 1 0.0788 0.3252 0.3421 11.00000 0.05 0.44 Q42 1 0.3304 0.3141 0.0867 11.00000 0.05 0.44 Q43 1 0.4730 0.4187 0.7843 11.00000 0.05 0.44 Q44 1 0.3981 0.3003 0.7626 11.00000 0.05 0.44 Q45 1 0.1685 0.3374 0.0661 11.00000 0.05 0.43 Q46 1 0.2748 0.3042 0.5078 11.00000 0.05 0.43 Q47 1 0.3166 0.6924 0.5735 11.00000 0.05 0.43 Q48 1 0.3062 0.5870 0.4594 11.00000 0.05 0.43 Q49 1 0.3982 0.1450 0.6625 11.00000 0.05 0.42 Q50 1 0.2555 0.2379 0.3191 11.00000 0.05 0.42 Q51 1 0.3456 0.3693 0.4307 11.00000 0.05 0.42 Q52 1 0.1651 0.6418 0.5436 11.00000 0.05 0.42 Q53 1 0.3118 0.5139 0.9024 11.00000 0.05 0.41 Q54 1 0.0698 0.3067 0.8026 11.00000 0.05 0.41 Q55 1 0.1008 0.5649 0.6162 11.00000 0.05 0.41 Q56 1 0.3940 0.3189 0.5052 11.00000 0.05 0.40 Q57 1 0.0616 0.4541 0.8039 11.00000 0.05 0.40 Q58 1 0.0990 0.4392 0.7362 11.00000 0.05 0.40 Q59 1 0.4634 0.3909 0.8305 11.00000 0.05 0.40 Q60 1 0.5816 0.4081 0.7145 11.00000 0.05 0.40 ; _shelx_res_checksum 74126 _shelx_hkl_file ; -2 0 0 5100.69 95.49 2 0 0 4951.20 95.59 -3 0 0 1.00 0.50 3 0 0 -0.30 0.40 4 0 0 2997.90 57.79 -4 0 0 3032.80 57.79 -4 0 0 3093.09 57.89 -6 0 0 2828.32 54.19 -8 0 0 2346.27 45.30 -9 0 0 1.10 1.00 0 -1 0 0.40 0.20 0 1 0 0.50 0.20 1 -1 0 16.10 0.80 -1 -1 0 15.80 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0 65.29 2.40 -6 3 0 54.79 3.00 6 3 0 63.89 2.40 -7 -3 0 520.05 11.00 -7 3 0 510.45 12.00 -8 -3 0 17.70 1.60 -8 3 0 16.80 2.10 -9 3 0 1064.69 22.50 0 4 0 1644.34 32.80 1 4 0 3166.78 61.19 -1 4 0 3161.48 61.39 2 4 0 471.05 10.80 -2 4 0 507.75 11.40 -3 4 0 2946.81 57.19 3 4 0 2908.31 56.59 4 4 0 637.74 13.70 -4 4 0 655.93 14.50 -5 4 0 775.02 17.30 5 4 0 796.32 16.40 6 4 0 982.60 20.60 -6 4 0 1041.00 21.70 -7 -4 0 300.97 7.00 7 4 0 292.07 7.00 -7 4 0 265.47 7.90 -8 -4 0 505.15 11.10 8 4 0 522.55 11.30 -8 4 0 521.45 12.50 -9 4 0 36.20 3.10 0 5 0 1.30 1.10 1 5 0 9.60 1.60 -1 5 0 8.80 1.60 2 5 0 944.11 19.90 -2 5 0 943.81 20.30 -3 5 0 19.50 2.20 3 5 0 19.50 1.90 -4 5 0 94.69 4.10 4 5 0 92.89 3.50 5 5 0 49.50 2.60 -5 5 0 37.60 3.20 6 5 0 1420.66 29.00 -6 5 0 1453.15 30.10 7 5 0 43.30 2.50 -7 5 0 47.30 3.40 -8 -5 0 695.83 15.10 8 5 0 688.83 15.20 -8 5 0 732.63 16.60 9 5 0 50.39 2.70 -9 5 0 46.60 3.60 0 6 0 7807.52 149.49 1 6 0 857.61 19.30 -1 6 0 901.51 19.60 2 6 0 467.65 11.40 -2 6 0 466.55 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5.60 1 -7 -18 162.78 11.90 -1 7 18 156.08 11.60 1 7 -18 147.49 11.80 0 -7 -18 9.90 5.80 0 7 18 9.30 5.60 0 7 -18 12.40 6.40 1 0 -19 196.88 13.10 1 -1 -19 34.50 7.50 1 1 -19 29.90 7.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 11606