#------------------------------------------------------------------------------ #$Date: 2026-06-18 23:59:56 +0100 (Thu, 18 Jun 2026) $ #$Revision: 306595 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721143.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7721143 loop_ _publ_author_name 'Leverett, Anthony Richard' 'Martin-Wells, Thomas A' 'Parr, Joseph M.' 'Cole, Marcus Lawford' 'McKay, Alasdair I.' _publ_section_title ; Synthesis, Structure and Reactivity of a Cationic Bis(N-Heterocyclic Carbene) Complex of Thallium ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00924G _journal_year 2026 _chemical_formula_moiety 'C54 H72 N4 Tl, Al C16 F36 O4' _chemical_formula_sum 'C70 H72 Al F36 N4 O4 Tl' _chemical_formula_weight 1948.66 _chemical_name_common '[Tl(IPr)2][Al{OC(CF3)3}4]' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-06-22 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2026-06-10 deposited with the CCDC. 2026-06-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.341(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.2839(5) _cell_length_b 28.9544(10) _cell_length_c 18.4627(7) _cell_measurement_reflns_used 9990 _cell_measurement_temperature 150.15 _cell_measurement_theta_max 25.27 _cell_measurement_theta_min 2.62 _cell_volume 8168.2(5) _computing_cell_refinement 'SAINT V8.32B (?, 2016)' _computing_data_reduction 'SAINT V8.32B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_unetI/netI 0.0333 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 168054 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 27.103 _diffrn_reflns_theta_min 1.308 _diffrn_source_current 0.6 _diffrn_source_power 0.03 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.118 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6168 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0938 before and 0.0553 after correction. The Ratio of minimum to maximum transmission is 0.8267. The \l/2 correction factor is 0.0015.' _exptl_crystal_colour 'light yellow' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.585 _exptl_crystal_description prism _exptl_crystal_F_000 3880 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _refine_diff_density_max 1.866 _refine_diff_density_min -2.042 _refine_diff_density_rms 0.095 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1221 _refine_ls_number_reflns 18002 _refine_ls_number_restraints 709 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0481 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+22.2736P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1137 _refine_ls_wR_factor_ref 0.1225 _reflns_Friedel_coverage 0.000 _reflns_number_gt 14397 _reflns_number_total 18002 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00924g2.cif _cod_data_source_block Compound_1 _cod_database_code 7721143 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_estimated_absorpt_t_max 0.866 _shelx_estimated_absorpt_t_min 0.785 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C39-C37 \\sim C14B-C37 \\sim C37-C71 \\sim C38-C37 with sigma of 0.02 C13-C14A \\sim C14-C13 \\sim C15-C13 \\sim C15A-C13 with sigma of 0.02 C59-C62 \\sim C59-C60 \\sim C59-C61 with sigma of 0.02 F17-C62 \\sim F16-C62 \\sim F18-C62 \\sim F11-C60 \\sim F12-C60 \\sim F10-C60 \\sim F15-C61 \\sim F13-C61 \\sim F14-C61 with sigma of 0.02 C62-C60 \\sim C60-C61 \\sim C62-C61 with sigma of 0.04 O2-C62 \\sim O2-C60 \\sim O2-C61 with sigma of 0.04 F17-F16 \\sim F16-F18 \\sim F18-F17 \\sim F11-F12 \\sim F12-F10 \\sim F10-F11 \\sim F15-F13 \\sim F13-F14 \\sim F14-F15 with sigma of 0.04 F17-C59 \\sim F16-C59 \\sim F18-C59 \\sim F11-C59 \\sim F12-C59 \\sim F10-C59 \\sim F15-C59 \\sim F13-C59 \\sim F14-C59 with sigma of 0.1 C59A-C61A \\sim C59A-C62A \\sim C59A-C60A with sigma of 0.02 F14A-C61A \\sim F15A-C61A \\sim F13A-C61A \\sim F16A-C62A \\sim F17A-C62A \\sim F18A-C62A \\sim F12A- C60A \\sim F10A-C60A \\sim F11A-C60A with sigma of 0.02 C61A-C62A \\sim C62A-C60A \\sim C61A-C60A with sigma of 0.04 O2-C61A \\sim O2-C62A \\sim O2-C60A with sigma of 0.04 F14A-F15A \\sim F15A-F13A \\sim F13A-F14A \\sim F16A-F17A \\sim F17A-F18A \\sim F18A-F16A \\sim F12A- F10A \\sim F10A-F11A \\sim F11A-F12A with sigma of 0.04 F14A-C59A \\sim F15A-C59A \\sim F13A-C59A \\sim F16A-C59A \\sim F17A-C59A \\sim F18A-C59A \\sim F12A- C59A \\sim F10A-C59A \\sim F11A-C59A with sigma of 0.1 O2-C59 \\sim O2-C59A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C71 \\sim C37 \\sim C14B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C38 \\sim C37 \\sim C39: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C15 \\sim C13 \\sim C14: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C15A \\sim C13 \\sim C14A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O2 \\sim C59 \\sim C62 \\sim F17 \\sim F16 \\sim F18 \\sim C60 \\sim F11 \\sim F12 \\sim F10 \\sim C61 \\sim F15 \\sim F13 \\sim F14: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O2 \\sim C59A \\sim C61A \\sim F14A \\sim F15A \\sim F13A \\sim C62A \\sim F16A \\sim F17A \\sim F18A \\sim C60A \\sim F12A \\sim F10A \\sim F11A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 4. Rigid body (RIGU) restrains C71, C37, C14B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C38, C37, C39 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C15, C13, C14 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C15A, C13, C14A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O2, C59, C62, F17, F16, F18, C60, F11, F12, F10, C61, F15, F13, F14 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O2, C59A, C61A, F14A, F15A, F13A, C62A, F16A, F17A, F18A, C60A, F12A, F10A, F11A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(H37A)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C71)=Sof(H71A)= Sof(H71B)=Sof(H71C)=1-FVAR(1) Sof(H37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)= Sof(H39C)=FVAR(1) Sof(H13A)=Sof(C14A)=Sof(H14G)=Sof(H14H)=Sof(H14I)=Sof(C15A)=Sof(H15D)= Sof(H15E)=Sof(H15F)=1-FVAR(2) Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)= Sof(H15C)=FVAR(2) Sof(C59A)=Sof(C61A)=Sof(F14A)=Sof(F15A)=Sof(F13A)=Sof(C62A)=Sof(F16A)= Sof(F17A)=Sof(F18A)=Sof(C60A)=Sof(F12A)=Sof(F10A)=Sof(F11A)=1-FVAR(3) Sof(C59)=Sof(C62)=Sof(F17)=Sof(F16)=Sof(F18)=Sof(C60)=Sof(F11)=Sof(F12)= Sof(F10)=Sof(C61)=Sof(F15)=Sof(F13)=Sof(F14)=FVAR(3) 6.a Ternary CH refined with riding coordinates: C52(H52), C37(H37), C37(H37A), C10(H10), C40(H40), C25(H25), C49(H49), C13(H13), C13(H13A), C22(H22) 6.b Aromatic/amide H refined with riding coordinates: C30(H30), C29(H29), C3(H3), C45(H45), C8(H8), C33(H33), C2(H2), C7(H7), C35(H35), C47(H47), C20(H20), C6(H6), C19(H19), C46(H46), C18(H18), C34(H34) 6.c Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C26(H26A,H26B, H26C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C53(H53A,H53B,H53C), C41(H41A, H41B,H41C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C50(H50A,H50B,H50C), C14(H14A,H14B,H14C), C42(H42A,H42B,H42C), C15(H15A,H15B,H15C), C38(H38A,H38B, H38C), C14B(H14D,H14E,H14F), C71(H71A,H71B,H71C), C39(H39A,H39B,H39C), C14A(H14G,H14H,H14I), C15A(H15D,H15E,H15F) ; _shelx_res_file ; TITL newcom in P2(1)/n newcom.res created by SHELXL-2018/3 at 00:48:53 on 22-Jun-2024 REM newcom in P2(1)/n REM 1045 parameters refined using 0 restraints REM Highest difference peak 1.904, deepest hole -2.256, 1-sigma level 0.157 CELL 0.71073 15.2839 28.9544 18.4627 90 91.341 90 ZERR 4 0.0005 0.001 0.0007 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Al F N O Tl UNIT 280 288 4 144 16 16 4 SADI C39 C37 C14B C37 C37 C71 C38 C37 SADI C13 C14A C14 C13 C15 C13 C15A C13 SADI C59 C62 C59 C60 C59 C61 SADI F17 C62 F16 C62 F18 C62 F11 C60 F12 C60 F10 C60 F15 C61 F13 C61 F14 C61 SADI 0.04 C62 C60 C60 C61 C62 C61 SADI 0.04 O2 C62 O2 C60 O2 C61 SADI 0.04 F17 F16 F16 F18 F18 F17 F11 F12 F12 F10 F10 F11 F15 F13 F13 F14 = F14 F15 SADI 0.1 F17 C59 F16 C59 F18 C59 F11 C59 F12 C59 F10 C59 F15 C59 F13 C59 = F14 C59 SADI C59A C61A C59A C62A C59A C60A SADI F14A C61A F15A C61A F13A C61A F16A C62A F17A C62A F18A C62A F12A C60A = F10A C60A F11A C60A SADI 0.04 C61A C62A C62A C60A C61A C60A SADI 0.04 O2 C61A O2 C62A O2 C60A SADI 0.04 F14A F15A F15A F13A F13A F14A F16A F17A F17A F18A F18A F16A F12A = F10A F10A F11A F11A F12A SADI 0.1 F14A C59A F15A C59A F13A C59A F16A C59A F17A C59A F18A C59A F12A = C59A F10A C59A F11A C59A SADI O2 C59 O2 C59A SIMU C71 C37 C14B SIMU C38 C37 C39 SIMU C15 C13 C14 SIMU C15A C13 C14A SIMU O2 C59 C62 F17 F16 F18 C60 F11 F12 F10 C61 F15 F13 F14 SIMU O2 C59A C61A F14A F15A F13A C62A F16A F17A F18A C60A F12A F10A F11A RIGU C71 C37 C14B RIGU C38 C37 C39 RIGU C15 C13 C14 RIGU C15A C13 C14A RIGU O2 C59 C62 F17 F16 F18 C60 F11 F12 F10 C61 F15 F13 F14 RIGU O2 C59A C61A F14A F15A F13A C62A F16A F17A F18A C60A F12A F10A F11A L.S. 20 PLAN 5 SIZE 0.07 0.09 0.12 TEMP -123 CONF GRID BOND fmap 2 acta 52 MORE -1 BOND $H MERG 2 SHEL 999 0.78 OMIT -1 0 1 OMIT 0 0 2 OMIT 0 2 0 OMIT 0 4 0 OMIT 1 1 0 REM REM REM WGHT 0.050800 22.273602 FVAR 0.05375 0.51050 0.71363 0.69283 TL1 7 0.806528 0.037422 0.783188 11.00000 0.02349 0.04985 = 0.05491 -0.02767 -0.00295 0.00714 AL1 3 0.250065 -0.238315 0.702324 11.00000 0.02678 0.01882 = 0.02316 0.00453 0.00011 -0.00173 N2 5 0.930606 -0.029911 0.671616 11.00000 0.02001 0.02008 = 0.02292 -0.00008 0.00226 0.00175 F25 4 0.162359 -0.327872 0.627590 11.00000 0.06525 0.04216 = 0.06511 -0.00621 -0.00102 0.01488 N3 5 0.574490 0.087508 0.748794 11.00000 0.01999 0.02103 = 0.01612 -0.00002 0.00247 -0.00125 C43 1 0.648379 0.038269 0.913928 11.00000 0.02127 0.03767 = 0.01429 -0.00343 -0.00055 0.00486 N4 5 0.604292 0.059962 0.853257 11.00000 0.02131 0.02371 = 0.01576 -0.00253 -0.00065 0.00142 C1 1 0.864444 -0.041383 0.716599 11.00000 0.02331 0.02551 = 0.01785 0.00090 0.00095 0.00175 F22 4 0.026689 -0.289449 0.690011 11.00000 0.06472 0.04822 = 0.08883 0.00031 0.03534 -0.00551 F33 4 0.159694 -0.125610 0.631630 11.00000 0.06266 0.06169 = 0.06150 0.00272 -0.02735 0.01959 N1 5 0.870651 -0.088129 0.719477 11.00000 0.02274 0.02191 = 0.02185 0.00243 0.00384 0.00159 C4 1 0.815472 -0.117810 0.761918 11.00000 0.02768 0.01994 = 0.03024 0.00390 0.00463 0.00468 O3 6 0.171196 -0.235117 0.634376 11.00000 0.04407 0.04121 = 0.03901 0.01033 -0.01197 -0.01430 O4 6 0.284159 -0.183024 0.718441 11.00000 0.05656 0.01902 = 0.04256 0.00066 -0.01326 0.00176 C21 1 0.896316 0.036662 0.596090 11.00000 0.02791 0.03255 = 0.03385 0.00759 0.00186 0.00225 C52 1 0.561357 -0.034492 0.884381 11.00000 0.03593 0.02649 = 0.02548 0.00129 0.00190 0.00269 AFIX 13 H52 2 0.520676 -0.011735 0.860647 11.00000 -1.20000 AFIX 0 C37 1 0.473888 0.031599 0.648856 11.00000 0.03345 0.04055 = 0.02453 -0.00599 0.00181 -0.01116 PART 1 AFIX 13 H37 2 0.497315 0.024122 0.698506 21.00000 -1.20000 AFIX 13 PART 2 H37A 2 0.460450 0.035717 0.701210 -21.00000 -1.20000 AFIX 0 PART 0 O1 6 0.336793 -0.271650 0.683251 11.00000 0.04653 0.05687 = 0.06672 -0.00693 0.00974 0.02099 F27 4 0.057284 -0.327783 0.548387 11.00000 0.06914 0.05798 = 0.07940 -0.02780 -0.00749 -0.01798 C30 1 0.527064 0.084417 0.859321 11.00000 0.02580 0.02958 = 0.02232 -0.00366 0.00371 0.00424 AFIX 43 H30 2 0.493826 0.088133 0.901769 11.00000 -1.20000 AFIX 0 C17 1 1.018972 0.040265 0.684554 11.00000 0.02784 0.02662 = 0.04350 -0.00234 0.00083 0.00018 F8 4 0.371754 -0.356986 0.673124 11.00000 0.10066 0.06128 = 0.11275 0.02028 0.01523 -0.02145 C32 1 0.523786 0.073955 0.625128 11.00000 0.02391 0.03167 = 0.02121 -0.00112 0.00134 0.00051 C28 1 0.635338 0.061195 0.784537 11.00000 0.02032 0.02616 = 0.01910 -0.00235 -0.00049 -0.00423 C29 1 0.508354 0.101851 0.793441 11.00000 0.02367 0.02787 = 0.02275 -0.00074 0.00169 0.00486 AFIX 43 H29 2 0.459314 0.120403 0.780083 11.00000 -1.20000 AFIX 0 F26 4 0.184671 -0.304160 0.520006 11.00000 0.07945 0.13448 = 0.05653 -0.02851 0.02930 -0.00792 F36 4 0.133187 -0.154380 0.765983 11.00000 0.05709 0.11461 = 0.08451 -0.01533 0.03266 -0.00258 F29 4 0.396645 -0.139013 0.799158 11.00000 0.08527 0.06471 = 0.11546 0.00567 -0.06851 -0.00771 C3 1 0.974950 -0.068056 0.646911 11.00000 0.02610 0.02846 = 0.03483 -0.00260 0.01076 0.00359 AFIX 43 H3 2 1.022511 -0.068279 0.614693 11.00000 -1.20000 AFIX 0 C9 1 0.746166 -0.140851 0.727369 11.00000 0.03170 0.02397 = 0.03594 -0.00262 0.00587 0.00245 C16 1 0.948918 0.016801 0.650379 11.00000 0.02339 0.02215 = 0.03150 0.00190 0.00785 0.00189 C31 1 0.575612 0.100039 0.672919 11.00000 0.02372 0.02542 = 0.01744 0.00355 0.00107 0.00041 C48 1 0.626842 -0.007247 0.930697 11.00000 0.03243 0.03317 = 0.01986 -0.00269 -0.00004 0.00810 F32 4 0.286078 -0.139567 0.593550 11.00000 0.09211 0.16245 = 0.04325 0.02902 0.02489 0.00615 F24 4 0.012741 -0.217172 0.679951 11.00000 0.08050 0.04571 = 0.12551 -0.02035 0.01564 0.01266 C45 1 0.747324 0.043509 1.014722 11.00000 0.04443 0.06742 = 0.03101 -0.01168 -0.01721 0.00670 AFIX 43 H45 2 0.788553 0.060210 1.043759 11.00000 -1.20000 AFIX 0 C8 1 0.695841 -0.170003 0.769542 11.00000 0.04418 0.03047 = 0.05231 -0.00398 0.01214 -0.00964 AFIX 43 H8 2 0.648099 -0.186279 0.747762 11.00000 -1.20000 AFIX 0 C67 1 0.273098 -0.137801 0.719804 11.00000 0.03530 0.01789 = 0.03874 0.00442 -0.00441 -0.00204 C44 1 0.708344 0.064765 0.954749 11.00000 0.02958 0.04794 = 0.02117 -0.00889 -0.00243 0.00043 C24 1 1.172924 0.033122 0.737584 11.00000 0.03024 0.06298 = 0.06124 -0.00561 -0.00328 0.00158 AFIX 137 H24A 2 1.192573 0.031038 0.687543 11.00000 -1.50000 H24B 2 1.210027 0.013539 0.768823 11.00000 -1.50000 H24C 2 1.177042 0.065226 0.754126 11.00000 -1.50000 AFIX 0 F5 4 0.567213 -0.273624 0.674809 11.00000 0.03532 0.12099 = 0.10270 0.01541 0.00214 -0.00937 F34 4 0.171020 -0.084004 0.770804 11.00000 0.13573 0.07304 = 0.11402 -0.02752 -0.00928 0.05995 F31 4 0.257939 -0.073513 0.640454 11.00000 0.20455 0.06466 = 0.12240 0.06763 -0.07788 -0.05667 F6 4 0.491821 -0.310025 0.751796 11.00000 0.07833 0.12430 = 0.07895 0.04994 -0.01549 -0.00585 C33 1 0.520304 0.088431 0.553188 11.00000 0.03698 0.04709 = 0.02046 -0.00280 -0.00485 0.00458 AFIX 43 H33 2 0.484957 0.071944 0.518987 11.00000 -1.20000 AFIX 0 C51 1 0.670054 0.146952 0.981573 11.00000 0.04426 0.04459 = 0.05576 -0.00694 -0.00907 -0.00321 AFIX 137 H51A 2 0.608323 0.138805 0.973725 11.00000 -1.50000 H51B 2 0.679501 0.178973 0.966440 11.00000 -1.50000 H51C 2 0.685753 0.143696 1.033088 11.00000 -1.50000 AFIX 0 C10 1 0.915543 -0.100258 0.870947 11.00000 0.03643 0.07544 = 0.02947 0.01046 -0.00505 -0.00534 AFIX 13 H10 2 0.945060 -0.081678 0.832946 11.00000 -1.20000 AFIX 0 F35 4 0.234425 -0.130008 0.842643 11.00000 0.15765 0.12539 = 0.03690 -0.02428 -0.00989 0.04976 C40 1 0.677162 0.167471 0.705176 11.00000 0.06296 0.04300 = 0.03900 -0.00251 0.00602 -0.03112 AFIX 13 H40 2 0.664232 0.156524 0.755169 11.00000 -1.20000 AFIX 0 C55 1 0.413991 -0.279989 0.649699 11.00000 0.03887 0.03572 = 0.03885 0.00585 0.01012 0.00718 C2 1 0.937242 -0.104806 0.677645 11.00000 0.03030 0.02273 = 0.03554 -0.00132 0.00751 0.00571 AFIX 43 H2 2 0.953324 -0.136249 0.671724 11.00000 -1.20000 AFIX 0 C63 1 0.105639 -0.254448 0.595122 11.00000 0.04147 0.03812 = 0.03901 0.00693 -0.01263 -0.01134 C54 1 0.505927 -0.067553 0.928134 11.00000 0.06779 0.04769 = 0.03497 0.00094 0.01210 -0.01517 AFIX 137 H54A 2 0.543411 -0.091719 0.949325 11.00000 -1.50000 H54B 2 0.461256 -0.081706 0.896316 11.00000 -1.50000 H54C 2 0.477439 -0.050512 0.966920 11.00000 -1.50000 AFIX 0 C5 1 0.837159 -0.123486 0.835523 11.00000 0.03393 0.03978 = 0.02918 0.01028 0.00292 0.00607 F23 4 -0.050403 -0.261166 0.602444 11.00000 0.04385 0.09940 = 0.15998 -0.02275 -0.02463 0.00549 C7 1 0.714304 -0.175580 0.842419 11.00000 0.05881 0.03518 = 0.05285 0.01511 0.02074 -0.00496 AFIX 43 H7 2 0.678653 -0.195235 0.870485 11.00000 -1.20000 AFIX 0 C25 1 0.825211 0.009575 0.556769 11.00000 0.03112 0.04601 = 0.03086 0.00789 -0.00024 -0.00253 AFIX 13 H25 2 0.817255 -0.020135 0.583436 11.00000 -1.20000 AFIX 0 C49 1 0.727377 0.114646 0.936861 11.00000 0.03875 0.05329 = 0.03233 -0.00807 -0.00517 -0.01482 AFIX 13 H49 2 0.711414 0.119554 0.884591 11.00000 -1.20000 AFIX 0 C36 1 0.622791 0.138754 0.652220 11.00000 0.04099 0.02786 = 0.02983 0.00319 0.00498 -0.00833 F19 4 0.160587 -0.211713 0.498162 11.00000 0.16494 0.18417 = 0.05515 0.06784 -0.03832 -0.10540 C35 1 0.617842 0.150679 0.579211 11.00000 0.05730 0.03827 = 0.03564 0.01385 0.01271 -0.00759 AFIX 43 H35 2 0.650400 0.176398 0.562674 11.00000 -1.20000 AFIX 0 C47 1 0.668204 -0.026799 0.991461 11.00000 0.05941 0.04370 = 0.03044 0.00576 -0.00988 0.01567 AFIX 43 H47 2 0.655729 -0.057803 1.004522 11.00000 -1.20000 AFIX 0 C26 1 0.851969 -0.002143 0.480359 11.00000 0.04032 0.09777 = 0.04876 -0.01396 0.00353 -0.00311 AFIX 137 H26A 2 0.857735 0.026369 0.452271 11.00000 -1.50000 H26B 2 0.807305 -0.021917 0.457370 11.00000 -1.50000 H26C 2 0.908162 -0.018456 0.482056 11.00000 -1.50000 AFIX 0 F21 4 0.039830 -0.245872 0.477252 11.00000 0.16267 0.11702 = 0.08175 0.02607 -0.08685 -0.04329 C27 1 0.737819 0.034782 0.555376 11.00000 0.02966 0.09749 = 0.07493 -0.01829 -0.00021 0.00641 AFIX 137 H27A 2 0.720899 0.041727 0.605076 11.00000 -1.50000 H27B 2 0.693073 0.015212 0.532053 11.00000 -1.50000 H27C 2 0.743205 0.063639 0.528102 11.00000 -1.50000 AFIX 0 C23 1 1.044678 0.022558 0.816773 11.00000 0.03540 0.07979 = 0.05683 0.01844 -0.00739 -0.00301 AFIX 137 H23A 2 1.041561 0.055494 0.828665 11.00000 -1.50000 H23B 2 1.084517 0.007037 0.851278 11.00000 -1.50000 H23C 2 0.986232 0.008846 0.819558 11.00000 -1.50000 AFIX 0 F30 4 0.415888 -0.115832 0.689722 11.00000 0.04741 0.15706 = 0.20579 0.05714 0.01160 -0.04032 F7 4 0.484658 -0.347837 0.608211 11.00000 0.07125 0.08412 = 0.16513 -0.04635 0.02240 0.03561 C13 1 0.726969 -0.135611 0.646990 11.00000 0.03897 0.04946 = 0.03056 -0.01047 0.00143 -0.00667 PART 1 AFIX 13 H13 2 0.764572 -0.110388 0.627705 31.00000 -1.20000 AFIX 13 PART 2 H13A 2 0.781987 -0.123247 0.626047 -31.00000 -1.20000 AFIX 0 PART 0 C22 1 1.078102 0.016862 0.741106 11.00000 0.03239 0.03129 = 0.05149 -0.00347 -0.00895 -0.00010 AFIX 13 H22 2 1.077674 -0.016952 0.730080 11.00000 -1.20000 AFIX 0 F9 4 0.357176 -0.334558 0.565356 11.00000 0.09055 0.13547 = 0.07302 -0.04798 0.01092 -0.01796 C70 1 0.201160 -0.125679 0.775546 11.00000 0.08902 0.04733 = 0.05602 -0.01222 0.00073 0.01484 C53 1 0.608658 -0.059691 0.824501 11.00000 0.04933 0.04919 = 0.03529 -0.01342 0.00835 -0.00228 AFIX 137 H53A 2 0.640262 -0.037286 0.795133 11.00000 -1.50000 H53B 2 0.565918 -0.076218 0.793764 11.00000 -1.50000 H53C 2 0.650263 -0.081801 0.846035 11.00000 -1.50000 AFIX 0 C66 1 0.127061 -0.304660 0.572719 11.00000 0.04517 0.05919 = 0.04025 -0.00952 0.00616 -0.01007 C20 1 0.914241 0.082445 0.577439 11.00000 0.04526 0.03706 = 0.05418 0.01949 -0.00099 0.00444 AFIX 43 H20 2 0.879801 0.097175 0.540695 11.00000 -1.20000 AFIX 0 C6 1 0.783872 -0.152941 0.874843 11.00000 0.05551 0.04831 = 0.03505 0.01884 0.00787 0.00399 AFIX 43 H6 2 0.795910 -0.157446 0.925061 11.00000 -1.20000 AFIX 0 C69 1 0.244137 -0.118412 0.645359 11.00000 0.07322 0.04636 = 0.05047 0.02377 -0.00345 -0.00357 C58 1 0.407725 -0.331163 0.626289 11.00000 0.05937 0.05364 = 0.06533 -0.00547 0.01913 0.01039 F4 4 0.481227 -0.237169 0.743588 11.00000 0.09251 0.11149 = 0.11340 -0.05098 -0.01181 -0.02139 C19 1 0.980960 0.106425 0.611506 11.00000 0.04928 0.02845 = 0.07907 0.01330 -0.00081 -0.00460 AFIX 43 H19 2 0.991129 0.137710 0.598683 11.00000 -1.20000 AFIX 0 F28 4 0.351382 -0.071651 0.765277 11.00000 0.13826 0.03621 = 0.14686 0.00560 -0.06772 -0.03607 F20 4 0.044104 -0.184890 0.546861 11.00000 0.14032 0.06642 = 0.13502 0.04459 -0.08092 -0.01510 C46 1 0.727355 -0.001223 1.032822 11.00000 0.06233 0.07154 = 0.02874 0.00062 -0.02152 0.02141 AFIX 43 H46 2 0.754578 -0.014828 1.074397 11.00000 -1.20000 AFIX 0 C41 1 0.654023 0.218679 0.700993 11.00000 0.08585 0.04840 = 0.09200 -0.02217 0.02027 -0.02204 AFIX 137 H41A 2 0.668495 0.230682 0.653111 11.00000 -1.50000 H41B 2 0.687440 0.235584 0.738380 11.00000 -1.50000 H41C 2 0.591271 0.222660 0.708803 11.00000 -1.50000 AFIX 0 C11 1 0.888837 -0.067244 0.930465 11.00000 0.06240 0.09965 = 0.05937 -0.01715 -0.00791 -0.01207 AFIX 137 H11A 2 0.846388 -0.044910 0.910759 11.00000 -1.50000 H11B 2 0.940616 -0.050812 0.949276 11.00000 -1.50000 H11C 2 0.862282 -0.084716 0.969746 11.00000 -1.50000 AFIX 0 C18 1 1.033000 0.085984 0.663600 11.00000 0.04221 0.02855 = 0.06833 0.00169 -0.00457 -0.00613 AFIX 43 H18 2 1.079325 0.103123 0.685836 11.00000 -1.20000 AFIX 0 C68 1 0.360901 -0.115703 0.744901 11.00000 0.07212 0.04920 = 0.11288 0.01141 -0.03838 -0.01628 C12 1 0.981110 -0.136457 0.898891 11.00000 0.04234 0.13239 = 0.05840 0.03115 -0.00059 0.02317 AFIX 137 H12A 2 0.953754 -0.155462 0.935998 11.00000 -1.50000 H12B 2 1.032696 -0.120918 0.919916 11.00000 -1.50000 H12C 2 0.998842 -0.156156 0.858643 11.00000 -1.50000 AFIX 0 C57 1 0.489738 -0.274125 0.704930 11.00000 0.05627 0.06520 = 0.06652 0.00421 0.00382 -0.00669 C50 1 0.823607 0.127412 0.947513 11.00000 0.04594 0.08745 = 0.08402 -0.03672 0.00980 -0.02489 AFIX 137 H50A 2 0.839948 0.125311 0.999052 11.00000 -1.50000 H50B 2 0.833000 0.159047 0.930499 11.00000 -1.50000 H50C 2 0.859722 0.106083 0.919835 11.00000 -1.50000 AFIX 0 PART 1 C14 1 0.631096 -0.123342 0.631954 31.00000 0.04323 0.07274 = 0.05444 -0.00110 -0.00885 0.00907 AFIX 137 H14A 2 0.594061 -0.149650 0.644501 31.00000 -1.50000 H14B 2 0.622496 -0.115976 0.580471 31.00000 -1.50000 H14C 2 0.615196 -0.096526 0.661239 31.00000 -1.50000 AFIX 0 PART 0 C42 1 0.773703 0.159992 0.693191 11.00000 0.06158 0.08244 = 0.10330 -0.01822 -0.02545 -0.01354 AFIX 137 H42A 2 0.787559 0.127108 0.698613 11.00000 -1.50000 H42B 2 0.807944 0.177856 0.728919 11.00000 -1.50000 H42C 2 0.788149 0.170165 0.644277 11.00000 -1.50000 AFIX 0 C64 1 0.089556 -0.224168 0.527389 11.00000 0.12570 0.07721 = 0.06297 0.02924 -0.05955 -0.03314 C65 1 0.022442 -0.255765 0.642360 11.00000 0.04361 0.04206 = 0.08779 -0.01189 -0.00285 0.00236 PART 1 C15 1 0.749411 -0.180590 0.608881 31.00000 0.09000 0.09801 = 0.05825 -0.04336 -0.01225 0.03590 AFIX 137 H15A 2 0.810621 -0.188630 0.619679 31.00000 -1.50000 H15B 2 0.740789 -0.176776 0.556457 31.00000 -1.50000 H15C 2 0.711262 -0.205304 0.625988 31.00000 -1.50000 AFIX 0 PART 0 C34 1 0.567182 0.126216 0.530755 11.00000 0.05802 0.04856 = 0.02199 0.01313 0.00559 0.00827 AFIX 43 H34 2 0.564310 0.135338 0.481330 11.00000 -1.20000 AFIX 0 PART 1 C38 1 0.492662 -0.011962 0.601795 21.00000 0.04619 0.03495 = 0.05212 -0.00422 0.01392 -0.00034 AFIX 137 H38A 2 0.466516 -0.007812 0.553258 21.00000 -1.50000 H38B 2 0.467222 -0.039272 0.624536 21.00000 -1.50000 H38C 2 0.556028 -0.016134 0.598063 21.00000 -1.50000 AFIX 0 PART 2 C14B 1 0.385259 0.029362 0.606158 -21.00000 0.03009 0.05092 = 0.05423 -0.00133 -0.00705 -0.01307 AFIX 137 H14D 2 0.354941 0.059043 0.610187 -21.00000 -1.50000 H14E 2 0.348911 0.004840 0.626278 -21.00000 -1.50000 H14F 2 0.395981 0.022792 0.555057 -21.00000 -1.50000 AFIX 0 PART 0 F1 4 0.486621 -0.264408 0.541037 11.00000 0.12436 0.19092 = 0.06595 0.02486 0.04731 -0.05313 F2 4 0.354389 -0.240720 0.549669 11.00000 0.11227 0.21056 = 0.10140 0.10910 -0.02252 -0.01190 F3 4 0.457391 -0.207810 0.608057 11.00000 0.16026 0.08177 = 0.18963 0.07912 -0.02568 -0.04401 C56 1 0.428931 -0.250350 0.583888 11.00000 0.10313 0.09683 = 0.07200 0.05071 -0.00005 -0.02240 PART 2 C71 1 0.526542 -0.009126 0.643013 -21.00000 0.04664 0.03381 = 0.05632 0.00988 -0.01000 -0.00254 AFIX 137 H71A 2 0.537762 -0.015278 0.591867 -21.00000 -1.50000 H71B 2 0.495605 -0.035444 0.663823 -21.00000 -1.50000 H71C 2 0.582267 -0.004504 0.669352 -21.00000 -1.50000 AFIX 0 PART 1 C39 1 0.379291 0.037276 0.656530 21.00000 0.03156 0.03428 = 0.10774 -0.00517 0.02154 -0.00863 AFIX 137 H39A 2 0.368041 0.062898 0.689721 21.00000 -1.50000 H39B 2 0.354397 0.008780 0.675946 21.00000 -1.50000 H39C 2 0.352166 0.043946 0.609056 21.00000 -1.50000 AFIX 0 PART 2 C14A 1 0.657799 -0.099052 0.632207 -31.00000 0.05443 0.08295 = 0.03119 -0.00436 -0.01106 0.00735 AFIX 137 H14G 2 0.603842 -0.107518 0.656600 -31.00000 -1.50000 H14H 2 0.646115 -0.096833 0.579905 -31.00000 -1.50000 H14I 2 0.678735 -0.069177 0.650561 -31.00000 -1.50000 AFIX 0 C15A 1 0.708466 -0.180826 0.607234 -31.00000 0.13543 0.06316 = 0.05415 -0.02518 0.00512 -0.03025 AFIX 137 H15D 2 0.753689 -0.203494 0.620474 -31.00000 -1.50000 H15E 2 0.708773 -0.175431 0.554839 -31.00000 -1.50000 H15F 2 0.651038 -0.192625 0.620826 -31.00000 -1.50000 AFIX 0 PART 0 O2 6 0.202493 -0.261618 0.777476 11.00000 0.06791 0.05684 = 0.03419 0.02168 -0.00665 -0.02667 PART 1 C59 1 0.213599 -0.279068 0.844372 41.00000 0.03541 0.02035 = 0.02517 0.00541 0.00458 -0.00318 C62 1 0.192043 -0.331197 0.843170 41.00000 0.06875 0.02861 = 0.03797 0.00519 -0.00047 -0.01289 F17 4 0.106340 -0.337725 0.831012 41.00000 0.07851 0.05929 = 0.04913 0.00860 -0.01412 -0.04303 F16 4 0.213117 -0.350821 0.905803 41.00000 0.17237 0.04948 = 0.07721 0.04181 -0.05169 -0.04881 F18 4 0.232672 -0.352925 0.792316 41.00000 0.11940 0.05253 = 0.08356 -0.03765 -0.01333 0.02656 C60 1 0.305279 -0.271638 0.880133 41.00000 0.04227 0.04251 = 0.03152 0.00655 -0.00171 -0.00389 F11 4 0.333244 -0.228227 0.867484 41.00000 0.07438 0.05043 = 0.05269 0.00873 -0.01836 -0.03666 F12 4 0.361895 -0.301580 0.854108 41.00000 0.04419 0.08696 = 0.07601 0.00570 0.00336 0.01822 F10 4 0.306661 -0.276051 0.951060 41.00000 0.05507 0.07807 = 0.03275 0.01518 -0.00914 -0.00886 C61 1 0.144182 -0.256030 0.895858 41.00000 0.04813 0.05497 = 0.06037 -0.01593 -0.00628 0.00994 F15 4 0.173728 -0.214908 0.919157 41.00000 0.10693 0.05260 = 0.06412 -0.02601 0.00764 0.00777 F13 4 0.128718 -0.285420 0.953484 41.00000 0.06686 0.14800 = 0.04954 0.04256 0.03156 0.03473 F14 4 0.063820 -0.251972 0.863835 41.00000 0.03533 0.07693 = 0.05308 0.00314 0.01810 0.01317 PART 2 C59A 1 0.202730 -0.281441 0.843407 -41.00000 0.04221 0.03230 = 0.02670 0.00744 0.00367 -0.01028 C61A 1 0.104645 -0.281832 0.862655 -41.00000 0.05147 0.07833 = 0.08135 -0.02901 0.02142 -0.01589 F14A 4 0.086506 -0.240073 0.827677 -41.00000 0.04908 0.07931 = 0.18192 -0.02045 -0.00543 0.01688 F15A 4 0.103976 -0.273117 0.934243 -41.00000 0.11777 0.31390 = 0.08500 -0.06263 0.04467 0.07032 F13A 4 0.065381 -0.318782 0.832425 -41.00000 0.05778 0.07602 = 0.09957 -0.00557 0.00407 -0.03043 C62A 1 0.242991 -0.329031 0.838564 -41.00000 0.07660 0.04724 = 0.05507 0.00844 0.00962 0.00724 F16A 4 0.332195 -0.325009 0.836295 -41.00000 0.06697 0.07175 = 0.17182 0.02229 0.02354 0.02732 F17A 4 0.216866 -0.349066 0.775216 -41.00000 0.12663 0.03539 = 0.04384 0.00817 0.01231 0.01892 F18A 4 0.224810 -0.357142 0.894971 -41.00000 0.07908 0.03133 = 0.05295 0.01092 0.00619 0.02705 C60A 1 0.256039 -0.247773 0.890796 -41.00000 0.07615 0.05920 = 0.03679 0.00475 -0.00414 -0.02611 F12A 4 0.333871 -0.239998 0.854999 -41.00000 0.06995 0.05989 = 0.04993 0.00143 -0.01882 -0.04781 F10A 4 0.276229 -0.268331 0.954798 -41.00000 0.14216 0.08659 = 0.03228 0.01000 -0.02176 -0.06265 F11A 4 0.206850 -0.207711 0.890293 -41.00000 0.10461 0.04029 = 0.09910 -0.04095 0.03818 -0.03107 HKLF 4 REM newcom in P2(1)/n REM wR2 = 0.1225, GooF = S = 1.043, Restrained GooF = 1.048 for all data REM R1 = 0.0481 for 14397 Fo > 4sig(Fo) and 0.0651 for all 18002 data REM 1221 parameters refined using 709 restraints END WGHT 0.0508 22.2740 REM Highest difference peak 1.866, deepest hole -2.042, 1-sigma level 0.095 Q1 1 0.7860 0.0151 0.8046 11.00000 0.05 1.87 Q2 1 0.7975 0.0423 0.7413 11.00000 0.05 1.58 Q3 1 0.3347 -0.2571 0.6377 11.00000 0.05 1.02 Q4 1 0.4015 -0.2630 0.5152 11.00000 0.05 1.01 Q5 1 0.2421 -0.2799 0.7663 11.00000 0.05 0.98 ; _shelx_res_checksum 57712 _olex2_submission_special_instructions 'No special instructions were received' 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' 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 Tl1 Tl 0.80653(2) 0.03742(2) 0.78319(2) 0.04281(7) Uani 1 1 d . . . . . Al1 Al 0.25007(7) -0.23832(4) 0.70232(6) 0.0229(2) Uani 1 1 d . . . . . N2 N 0.93061(19) -0.02991(10) 0.67162(16) 0.0210(6) Uani 1 1 d . . . . . F25 F 0.1624(2) -0.32787(10) 0.62759(17) 0.0575(8) Uani 1 1 d . . . . . N3 N 0.57449(18) 0.08751(10) 0.74879(14) 0.0190(6) Uani 1 1 d . . . . . C43 C 0.6484(2) 0.03827(13) 0.91393(18) 0.0244(7) Uani 1 1 d . . . . . N4 N 0.60429(18) 0.05996(10) 0.85326(15) 0.0203(6) Uani 1 1 d . . . . . C1 C 0.8644(2) -0.04138(12) 0.71660(18) 0.0222(7) Uani 1 1 d . . . . . F22 F 0.0267(2) -0.28945(11) 0.69001(19) 0.0667(9) Uani 1 1 d . . . . . F33 F 0.1597(2) -0.12561(11) 0.63163(17) 0.0624(8) Uani 1 1 d . . . . . N1 N 0.87065(19) -0.08813(10) 0.71948(15) 0.0221(6) Uani 1 1 d . . . . . C4 C 0.8155(2) -0.11781(13) 0.7619(2) 0.0259(8) Uani 1 1 d . . . . . O3 O 0.1712(2) -0.23512(11) 0.63438(16) 0.0416(7) Uani 1 1 d . . . . . O4 O 0.2842(2) -0.18302(9) 0.71844(16) 0.0396(7) Uani 1 1 d . . . . . C21 C 0.8963(3) 0.03666(14) 0.5961(2) 0.0314(8) Uani 1 1 d . . . . . C52 C 0.5614(3) -0.03449(13) 0.8844(2) 0.0293(8) Uani 1 1 d . . . . . H52 H 0.520676 -0.011735 0.860647 0.035 Uiso 1 1 calc R U . . . C37 C 0.4739(3) 0.03160(14) 0.6489(2) 0.0328(9) Uani 1 1 d D U . . . H37 H 0.497315 0.024122 0.698506 0.039 Uiso 0.510(16) 1 calc R U P A 1 H37A H 0.460450 0.035717 0.701210 0.039 Uiso 0.490(16) 1 calc R U P A 2 O1 O 0.3368(2) -0.27165(13) 0.6833(2) 0.0566(9) Uani 1 1 d . . . . . F27 F 0.0573(2) -0.32778(11) 0.54839(19) 0.0690(9) Uani 1 1 d . . . . . C30 C 0.5271(2) 0.08442(13) 0.85932(19) 0.0259(8) Uani 1 1 d . . . . . H30 H 0.493826 0.088133 0.901769 0.031 Uiso 1 1 calc R U . . . C17 C 1.0190(3) 0.04027(14) 0.6846(2) 0.0327(9) Uani 1 1 d . . . . . F8 F 0.3718(3) -0.35699(13) 0.6731(2) 0.0914(12) Uani 1 1 d . . . . . C32 C 0.5238(2) 0.07395(13) 0.62513(19) 0.0256(8) Uani 1 1 d . . . . . C28 C 0.6353(2) 0.06119(12) 0.78454(18) 0.0219(7) Uani 1 1 d . . . . . C29 C 0.5084(2) 0.10185(13) 0.79344(19) 0.0247(7) Uani 1 1 d . . . . . H29 H 0.459314 0.120403 0.780083 0.030 Uiso 1 1 calc R U . . . F26 F 0.1847(3) -0.30416(16) 0.52001(19) 0.0897(13) Uani 1 1 d . . . . . F36 F 0.1332(2) -0.15438(15) 0.7660(2) 0.0849(12) Uani 1 1 d . . . . . F29 F 0.3966(3) -0.13901(12) 0.7992(2) 0.0896(13) Uani 1 1 d . . . . . C3 C 0.9749(2) -0.06806(13) 0.6469(2) 0.0296(8) Uani 1 1 d . . . . . H3 H 1.022511 -0.068279 0.614693 0.036 Uiso 1 1 calc R U . . . C9 C 0.7462(3) -0.14085(13) 0.7274(2) 0.0305(8) Uani 1 1 d . . . . . C16 C 0.9489(2) 0.01680(13) 0.6504(2) 0.0256(8) Uani 1 1 d . . . . . C31 C 0.5756(2) 0.10004(12) 0.67292(18) 0.0222(7) Uani 1 1 d . . . . . C48 C 0.6268(3) -0.00725(14) 0.93070(19) 0.0285(8) Uani 1 1 d . . . . . F32 F 0.2861(3) -0.13957(18) 0.59355(19) 0.0989(14) Uani 1 1 d . . . . . F24 F 0.0127(3) -0.21717(12) 0.6800(2) 0.0837(11) Uani 1 1 d . . . . . C45 C 0.7473(3) 0.04351(19) 1.0147(2) 0.0479(12) Uani 1 1 d . . . . . H45 H 0.788553 0.060210 1.043759 0.057 Uiso 1 1 calc R U . . . C8 C 0.6958(3) -0.17000(15) 0.7695(3) 0.0421(11) Uani 1 1 d . . . . . H8 H 0.648099 -0.186279 0.747762 0.051 Uiso 1 1 calc R U . . . C67 C 0.2731(3) -0.13780(13) 0.7198(2) 0.0307(8) Uani 1 1 d . . . . . C44 C 0.7083(3) 0.06477(15) 0.9547(2) 0.0329(9) Uani 1 1 d . . . . . C24 C 1.1729(3) 0.03312(19) 0.7376(3) 0.0516(12) Uani 1 1 d . . . . . H24A H 1.192573 0.031038 0.687543 0.077 Uiso 1 1 calc R U . . . H24B H 1.210027 0.013539 0.768823 0.077 Uiso 1 1 calc R U . . . H24C H 1.177042 0.065226 0.754126 0.077 Uiso 1 1 calc R U . . . F5 F 0.5672(2) -0.27362(15) 0.6748(2) 0.0863(12) Uani 1 1 d . . . . . F34 F 0.1710(3) -0.08400(14) 0.7708(3) 0.1078(16) Uani 1 1 d . . . . . F31 F 0.2579(4) -0.07351(14) 0.6405(3) 0.132(2) Uani 1 1 d . . . . . F6 F 0.4918(3) -0.31002(16) 0.7518(2) 0.0941(13) Uani 1 1 d . . . . . C33 C 0.5203(3) 0.08843(16) 0.5532(2) 0.0349(9) Uani 1 1 d . . . . . H33 H 0.484957 0.071944 0.518987 0.042 Uiso 1 1 calc R U . . . C51 C 0.6701(3) 0.14695(17) 0.9816(3) 0.0484(12) Uani 1 1 d . . . . . H51A H 0.608323 0.138805 0.973725 0.073 Uiso 1 1 calc R U . . . H51B H 0.679501 0.178973 0.966440 0.073 Uiso 1 1 calc R U . . . H51C H 0.685753 0.143696 1.033088 0.073 Uiso 1 1 calc R U . . . C10 C 0.9155(3) -0.10026(19) 0.8709(2) 0.0472(12) Uani 1 1 d . . . . . H10 H 0.945060 -0.081678 0.832946 0.057 Uiso 1 1 calc R U . . . F35 F 0.2344(3) -0.13001(17) 0.84264(18) 0.1068(16) Uani 1 1 d . . . . . C40 C 0.6772(3) 0.16747(17) 0.7052(3) 0.0482(12) Uani 1 1 d . . . . . H40 H 0.664232 0.156524 0.755169 0.058 Uiso 1 1 calc R U . . . C55 C 0.4140(3) -0.27999(15) 0.6497(2) 0.0377(10) Uani 1 1 d . . . . . C2 C 0.9372(2) -0.10481(13) 0.6776(2) 0.0294(8) Uani 1 1 d . . . . . H2 H 0.953324 -0.136249 0.671724 0.035 Uiso 1 1 calc R U . . . C63 C 0.1056(3) -0.25445(16) 0.5951(2) 0.0397(10) Uani 1 1 d . . . . . C54 C 0.5059(4) -0.06755(18) 0.9281(3) 0.0500(12) Uani 1 1 d . . . . . H54A H 0.543411 -0.091719 0.949325 0.075 Uiso 1 1 calc R U . . . H54B H 0.461256 -0.081706 0.896316 0.075 Uiso 1 1 calc R U . . . H54C H 0.477439 -0.050512 0.966920 0.075 Uiso 1 1 calc R U . . . C5 C 0.8372(3) -0.12349(15) 0.8355(2) 0.0343(9) Uani 1 1 d . . . . . F23 F -0.0504(2) -0.26117(15) 0.6024(3) 0.1015(15) Uani 1 1 d . . . . . C7 C 0.7143(3) -0.17558(16) 0.8424(3) 0.0486(12) Uani 1 1 d . . . . . H7 H 0.678653 -0.195235 0.870485 0.058 Uiso 1 1 calc R U . . . C25 C 0.8252(3) 0.00958(16) 0.5568(2) 0.0360(9) Uani 1 1 d . . . . . H25 H 0.817255 -0.020135 0.583436 0.043 Uiso 1 1 calc R U . . . C49 C 0.7274(3) 0.11465(17) 0.9369(2) 0.0415(10) Uani 1 1 d . . . . . H49 H 0.711414 0.119554 0.884591 0.050 Uiso 1 1 calc R U . . . C36 C 0.6228(3) 0.13875(14) 0.6522(2) 0.0328(9) Uani 1 1 d . . . . . F19 F 0.1606(4) -0.2117(2) 0.4982(2) 0.135(2) Uani 1 1 d . . . . . C35 C 0.6178(3) 0.15068(16) 0.5792(2) 0.0436(11) Uani 1 1 d . . . . . H35 H 0.650400 0.176398 0.562674 0.052 Uiso 1 1 calc R U . . . C47 C 0.6682(3) -0.02680(17) 0.9915(2) 0.0447(11) Uani 1 1 d . . . . . H47 H 0.655729 -0.057803 1.004522 0.054 Uiso 1 1 calc R U . . . C26 C 0.8520(3) -0.0021(2) 0.4804(3) 0.0622(15) Uani 1 1 d . . . . . H26A H 0.857735 0.026369 0.452271 0.093 Uiso 1 1 calc R U . . . H26B H 0.807305 -0.021917 0.457370 0.093 Uiso 1 1 calc R U . . . H26C H 0.908162 -0.018456 0.482056 0.093 Uiso 1 1 calc R U . . . F21 F 0.0398(4) -0.24587(17) 0.4773(2) 0.1219(19) Uani 1 1 d . . . . . C27 C 0.7378(3) 0.0348(2) 0.5554(4) 0.0674(17) Uani 1 1 d . . . . . H27A H 0.720899 0.041727 0.605076 0.101 Uiso 1 1 calc R U . . . H27B H 0.693073 0.015212 0.532053 0.101 Uiso 1 1 calc R U . . . H27C H 0.743205 0.063639 0.528102 0.101 Uiso 1 1 calc R U . . . C23 C 1.0447(3) 0.0226(2) 0.8168(3) 0.0575(14) Uani 1 1 d . . . . . H23A H 1.041561 0.055494 0.828665 0.086 Uiso 1 1 calc R U . . . H23B H 1.084517 0.007037 0.851278 0.086 Uiso 1 1 calc R U . . . H23C H 0.986232 0.008846 0.819558 0.086 Uiso 1 1 calc R U . . . F30 F 0.4159(3) -0.1158(2) 0.6897(4) 0.137(2) Uani 1 1 d . . . . . F7 F 0.4847(3) -0.34784(15) 0.6082(3) 0.1065(16) Uani 1 1 d . . . . . C13 C 0.7270(3) -0.13561(16) 0.6470(2) 0.0397(10) Uani 1 1 d D U . . . H13 H 0.764572 -0.110388 0.627705 0.048 Uiso 0.71(3) 1 calc R U P B 1 H13A H 0.781987 -0.123247 0.626047 0.048 Uiso 0.29(3) 1 calc R U P B 2 C22 C 1.0781(3) 0.01686(15) 0.7411(3) 0.0385(10) Uani 1 1 d . . . . . H22 H 1.077674 -0.016952 0.730080 0.046 Uiso 1 1 calc R U . . . F9 F 0.3572(3) -0.33456(17) 0.5654(2) 0.0995(14) Uani 1 1 d . . . . . C70 C 0.2012(5) -0.1257(2) 0.7755(3) 0.0641(16) Uani 1 1 d . . . . . C53 C 0.6087(3) -0.05969(17) 0.8245(2) 0.0445(11) Uani 1 1 d . . . . . H53A H 0.640262 -0.037286 0.795133 0.067 Uiso 1 1 calc R U . . . H53B H 0.565918 -0.076218 0.793764 0.067 Uiso 1 1 calc R U . . . H53C H 0.650263 -0.081801 0.846035 0.067 Uiso 1 1 calc R U . . . C66 C 0.1271(3) -0.30466(19) 0.5727(3) 0.0481(12) Uani 1 1 d . . . . . C20 C 0.9142(3) 0.08245(16) 0.5774(3) 0.0455(11) Uani 1 1 d . . . . . H20 H 0.879801 0.097175 0.540695 0.055 Uiso 1 1 calc R U . . . C6 C 0.7839(3) -0.15294(17) 0.8748(3) 0.0462(11) Uani 1 1 d . . . . . H6 H 0.795910 -0.157446 0.925061 0.055 Uiso 1 1 calc R U . . . C69 C 0.2441(4) -0.11841(19) 0.6454(3) 0.0568(14) Uani 1 1 d . . . . . C58 C 0.4077(4) -0.3312(2) 0.6263(3) 0.0592(14) Uani 1 1 d . . . . . F4 F 0.4812(3) -0.23717(17) 0.7436(3) 0.1060(15) Uani 1 1 d . . . . . C19 C 0.9810(3) 0.10642(17) 0.6115(3) 0.0523(13) Uani 1 1 d . . . . . H19 H 0.991129 0.137710 0.598683 0.063 Uiso 1 1 calc R U . . . F28 F 0.3514(3) -0.07165(12) 0.7653(3) 0.1082(17) Uani 1 1 d . . . . . F20 F 0.0441(3) -0.18489(15) 0.5469(3) 0.1152(19) Uani 1 1 d . . . . . C46 C 0.7274(4) -0.0012(2) 1.0328(2) 0.0546(14) Uani 1 1 d . . . . . H46 H 0.754578 -0.014828 1.074397 0.065 Uiso 1 1 calc R U . . . C41 C 0.6540(5) 0.2187(2) 0.7010(4) 0.0751(19) Uani 1 1 d . . . . . H41A H 0.668495 0.230682 0.653111 0.113 Uiso 1 1 calc R U . . . H41B H 0.687440 0.235584 0.738380 0.113 Uiso 1 1 calc R U . . . H41C H 0.591271 0.222660 0.708803 0.113 Uiso 1 1 calc R U . . . C11 C 0.8888(4) -0.0672(3) 0.9305(3) 0.0740(18) Uani 1 1 d . . . . . H11A H 0.846388 -0.044910 0.910759 0.111 Uiso 1 1 calc R U . . . H11B H 0.940616 -0.050812 0.949276 0.111 Uiso 1 1 calc R U . . . H11C H 0.862282 -0.084716 0.969746 0.111 Uiso 1 1 calc R U . . . C18 C 1.0330(3) 0.08598(16) 0.6636(3) 0.0465(11) Uani 1 1 d . . . . . H18 H 1.079325 0.103123 0.685836 0.056 Uiso 1 1 calc R U . . . C68 C 0.3609(5) -0.1157(2) 0.7449(4) 0.079(2) Uani 1 1 d . . . . . C12 C 0.9811(4) -0.1365(3) 0.8989(3) 0.078(2) Uani 1 1 d . . . . . H12A H 0.953754 -0.155462 0.935998 0.117 Uiso 1 1 calc R U . . . H12B H 1.032696 -0.120918 0.919916 0.117 Uiso 1 1 calc R U . . . H12C H 0.998842 -0.156156 0.858643 0.117 Uiso 1 1 calc R U . . . C57 C 0.4897(4) -0.2741(2) 0.7049(3) 0.0626(15) Uani 1 1 d . . . . . C50 C 0.8236(4) 0.1274(2) 0.9475(4) 0.0723(19) Uani 1 1 d . . . . . H50A H 0.839948 0.125311 0.999052 0.109 Uiso 1 1 calc R U . . . H50B H 0.833000 0.159047 0.930499 0.109 Uiso 1 1 calc R U . . . H50C H 0.859722 0.106083 0.919835 0.109 Uiso 1 1 calc R U . . . C14 C 0.6311(6) -0.1233(6) 0.6320(5) 0.057(3) Uani 0.71(3) 1 d D U P B 1 H14A H 0.594061 -0.149650 0.644501 0.085 Uiso 0.71(3) 1 calc R U P B 1 H14B H 0.622496 -0.115976 0.580471 0.085 Uiso 0.71(3) 1 calc R U P B 1 H14C H 0.615196 -0.096526 0.661239 0.085 Uiso 0.71(3) 1 calc R U P B 1 C42 C 0.7737(4) 0.1600(3) 0.6932(4) 0.083(2) Uani 1 1 d . . . . . H42A H 0.787559 0.127108 0.698613 0.124 Uiso 1 1 calc R U . . . H42B H 0.807944 0.177856 0.728919 0.124 Uiso 1 1 calc R U . . . H42C H 0.788149 0.170165 0.644277 0.124 Uiso 1 1 calc R U . . . C64 C 0.0896(6) -0.2242(3) 0.5274(4) 0.090(3) Uani 1 1 d . . . . . C65 C 0.0224(3) -0.25577(19) 0.6424(4) 0.0579(14) Uani 1 1 d . . . . . C15 C 0.7494(11) -0.1806(5) 0.6089(11) 0.082(5) Uani 0.71(3) 1 d D U P B 1 H15A H 0.810621 -0.188630 0.619679 0.123 Uiso 0.71(3) 1 calc R U P B 1 H15B H 0.740789 -0.176776 0.556457 0.123 Uiso 0.71(3) 1 calc R U P B 1 H15C H 0.711262 -0.205304 0.625988 0.123 Uiso 0.71(3) 1 calc R U P B 1 C34 C 0.5672(3) 0.12622(17) 0.5308(2) 0.0428(11) Uani 1 1 d . . . . . H34 H 0.564310 0.135338 0.481330 0.051 Uiso 1 1 calc R U . . . C38 C 0.4927(8) -0.0120(3) 0.6018(7) 0.044(3) Uani 0.510(16) 1 d D U P A 1 H38A H 0.466516 -0.007812 0.553258 0.066 Uiso 0.510(16) 1 calc R U P A 1 H38B H 0.467222 -0.039272 0.624536 0.066 Uiso 0.510(16) 1 calc R U P A 1 H38C H 0.556028 -0.016134 0.598063 0.066 Uiso 0.510(16) 1 calc R U P A 1 C14B C 0.3853(6) 0.0294(4) 0.6062(7) 0.045(3) Uani 0.490(16) 1 d D U P A 2 H14D H 0.354941 0.059043 0.610187 0.068 Uiso 0.490(16) 1 calc R U P A 2 H14E H 0.348911 0.004840 0.626278 0.068 Uiso 0.490(16) 1 calc R U P A 2 H14F H 0.395981 0.022792 0.555057 0.068 Uiso 0.490(16) 1 calc R U P A 2 F1 F 0.4866(3) -0.2644(2) 0.5410(2) 0.126(2) Uani 1 1 d . . . . . F2 F 0.3544(3) -0.2407(2) 0.5497(3) 0.142(2) Uani 1 1 d . . . . . F3 F 0.4574(4) -0.20781(17) 0.6081(3) 0.144(2) Uani 1 1 d . . . . . C56 C 0.4289(6) -0.2504(3) 0.5839(4) 0.091(2) Uani 1 1 d . . . . . C71 C 0.5265(7) -0.0091(3) 0.6430(8) 0.046(3) Uani 0.490(16) 1 d D U P A 2 H71A H 0.537762 -0.015278 0.591867 0.069 Uiso 0.490(16) 1 calc R U P A 2 H71B H 0.495605 -0.035444 0.663823 0.069 Uiso 0.490(16) 1 calc R U P A 2 H71C H 0.582267 -0.004504 0.669352 0.069 Uiso 0.490(16) 1 calc R U P A 2 C39 C 0.3793(6) 0.0373(4) 0.6565(10) 0.058(4) Uani 0.510(16) 1 d D U P A 1 H39A H 0.368041 0.062898 0.689721 0.086 Uiso 0.510(16) 1 calc R U P A 1 H39B H 0.354397 0.008780 0.675946 0.086 Uiso 0.510(16) 1 calc R U P A 1 H39C H 0.352166 0.043946 0.609056 0.086 Uiso 0.510(16) 1 calc R U P A 1 C14A C 0.658(2) -0.0991(12) 0.6322(11) 0.056(8) Uani 0.29(3) 1 d D U P B 2 H14G H 0.603842 -0.107518 0.656600 0.085 Uiso 0.29(3) 1 calc R U P B 2 H14H H 0.646115 -0.096833 0.579905 0.085 Uiso 0.29(3) 1 calc R U P B 2 H14I H 0.678735 -0.069177 0.650561 0.085 Uiso 0.29(3) 1 calc R U P B 2 C15A C 0.708(4) -0.1808(10) 0.607(2) 0.084(12) Uani 0.29(3) 1 d D U P B 2 H15D H 0.753689 -0.203494 0.620474 0.126 Uiso 0.29(3) 1 calc R U P B 2 H15E H 0.708773 -0.175431 0.554839 0.126 Uiso 0.29(3) 1 calc R U P B 2 H15F H 0.651038 -0.192625 0.620826 0.126 Uiso 0.29(3) 1 calc R U P B 2 O2 O 0.2025(2) -0.26162(12) 0.77748(17) 0.0531(9) Uani 1 1 d D U . . . C59 C 0.2136(5) -0.2791(2) 0.8444(4) 0.0269(15) Uani 0.693(7) 1 d D U P C 1 C62 C 0.1920(5) -0.3312(2) 0.8432(4) 0.0451(16) Uani 0.693(7) 1 d D U P C 1 F17 F 0.1063(4) -0.3377(2) 0.8310(3) 0.0626(16) Uani 0.693(7) 1 d D U P C 1 F16 F 0.2131(8) -0.3508(4) 0.9058(5) 0.101(4) Uani 0.693(7) 1 d D U P C 1 F18 F 0.2327(8) -0.3529(4) 0.7923(5) 0.085(3) Uani 0.693(7) 1 d D U P C 1 C60 C 0.3053(4) -0.2716(2) 0.8801(3) 0.0388(15) Uani 0.693(7) 1 d D U P C 1 F11 F 0.3332(7) -0.2282(3) 0.8675(7) 0.059(2) Uani 0.693(7) 1 d D U P C 1 F12 F 0.3619(4) -0.3016(2) 0.8541(3) 0.0690(16) Uani 0.693(7) 1 d D U P C 1 F10 F 0.3067(6) -0.2761(4) 0.9511(4) 0.0555(18) Uani 0.693(7) 1 d D U P C 1 C61 C 0.1442(5) -0.2560(2) 0.8959(4) 0.0546(18) Uani 0.693(7) 1 d D U P C 1 F15 F 0.1737(5) -0.2149(2) 0.9192(3) 0.0745(18) Uani 0.693(7) 1 d D U P C 1 F13 F 0.1287(5) -0.2854(3) 0.9535(3) 0.088(2) Uani 0.693(7) 1 d D U P C 1 F14 F 0.0638(3) -0.2520(2) 0.8638(3) 0.0548(14) Uani 0.693(7) 1 d D U P C 1 C59A C 0.2027(10) -0.2814(5) 0.8434(8) 0.034(3) Uani 0.307(7) 1 d D U P C 2 C61A C 0.1046(11) -0.2818(5) 0.8627(8) 0.070(4) Uani 0.307(7) 1 d D U P C 2 F14A F 0.0865(9) -0.2401(5) 0.8277(11) 0.104(5) Uani 0.307(7) 1 d D U P C 2 F15A F 0.1040(17) -0.2731(11) 0.9342(10) 0.172(11) Uani 0.307(7) 1 d D U P C 2 F13A F 0.0654(10) -0.3188(5) 0.8324(9) 0.078(4) Uani 0.307(7) 1 d D U P C 2 C62A C 0.2430(10) -0.3290(6) 0.8386(8) 0.060(4) Uani 0.307(7) 1 d D U P C 2 F16A F 0.3322(9) -0.3250(6) 0.8363(11) 0.103(6) Uani 0.307(7) 1 d D U P C 2 F17A F 0.2169(17) -0.3491(9) 0.7752(9) 0.068(5) Uani 0.307(7) 1 d D U P C 2 F18A F 0.2248(14) -0.3571(7) 0.8950(10) 0.054(4) Uani 0.307(7) 1 d D U P C 2 C60A C 0.2560(10) -0.2478(5) 0.8908(7) 0.057(3) Uani 0.307(7) 1 d D U P C 2 F12A F 0.3339(15) -0.2400(8) 0.8550(15) 0.060(5) Uani 0.307(7) 1 d D U P C 2 F10A F 0.2762(16) -0.2683(8) 0.9548(9) 0.087(7) Uani 0.307(7) 1 d D U P C 2 F11A F 0.2068(10) -0.2077(4) 0.8903(9) 0.081(4) Uani 0.307(7) 1 d D U P C 2 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 Tl1 0.02349(9) 0.04985(12) 0.05491(12) -0.02767(8) -0.00295(7) 0.00714(7) Al1 0.0268(5) 0.0188(5) 0.0232(5) 0.0045(4) 0.0001(4) -0.0017(4) N2 0.0200(14) 0.0201(15) 0.0229(15) -0.0001(11) 0.0023(11) 0.0017(11) F25 0.0653(19) 0.0422(16) 0.0651(19) -0.0062(14) -0.0010(15) 0.0149(14) N3 0.0200(14) 0.0210(15) 0.0161(13) 0.0000(11) 0.0025(11) -0.0013(11) C43 0.0213(17) 0.038(2) 0.0143(16) -0.0034(14) -0.0005(13) 0.0049(15) N4 0.0213(14) 0.0237(16) 0.0158(13) -0.0025(11) -0.0007(11) 0.0014(12) C1 0.0233(17) 0.0255(19) 0.0178(16) 0.0009(13) 0.0009(13) 0.0018(14) F22 0.065(2) 0.0482(18) 0.089(2) 0.0003(17) 0.0353(18) -0.0055(15) F33 0.063(2) 0.0617(19) 0.0615(19) 0.0027(15) -0.0274(15) 0.0196(15) N1 0.0227(15) 0.0219(16) 0.0218(15) 0.0024(11) 0.0038(11) 0.0016(12) C4 0.0277(19) 0.0199(18) 0.0302(19) 0.0039(14) 0.0046(15) 0.0047(14) O3 0.0441(17) 0.0412(18) 0.0390(17) 0.0103(13) -0.0120(13) -0.0143(14) O4 0.0566(19) 0.0190(14) 0.0426(17) 0.0007(12) -0.0133(14) 0.0018(13) C21 0.0279(19) 0.033(2) 0.034(2) 0.0076(16) 0.0019(16) 0.0022(16) C52 0.036(2) 0.026(2) 0.0255(19) 0.0013(15) 0.0019(15) 0.0027(16) C37 0.033(2) 0.041(2) 0.0245(19) -0.0060(16) 0.0018(15) -0.0112(17) O1 0.047(2) 0.057(2) 0.067(2) -0.0069(18) 0.0097(17) 0.0210(17) F27 0.069(2) 0.058(2) 0.079(2) -0.0278(17) -0.0075(17) -0.0180(16) C30 0.0258(18) 0.030(2) 0.0223(18) -0.0037(14) 0.0037(14) 0.0042(15) C17 0.028(2) 0.027(2) 0.044(2) -0.0023(17) 0.0008(17) 0.0002(16) F8 0.101(3) 0.061(2) 0.113(3) 0.020(2) 0.015(2) -0.021(2) C32 0.0239(18) 0.032(2) 0.0212(17) -0.0011(14) 0.0013(14) 0.0005(15) C28 0.0203(17) 0.0262(19) 0.0191(16) -0.0023(13) -0.0005(13) -0.0042(14) C29 0.0237(18) 0.028(2) 0.0227(17) -0.0007(14) 0.0017(14) 0.0049(14) F26 0.079(2) 0.134(4) 0.057(2) -0.029(2) 0.0293(18) -0.008(2) F36 0.057(2) 0.115(3) 0.085(3) -0.015(2) 0.0327(19) -0.003(2) F29 0.085(3) 0.065(2) 0.115(3) 0.006(2) -0.069(2) -0.0077(19) C3 0.0261(19) 0.028(2) 0.035(2) -0.0026(16) 0.0108(16) 0.0036(15) C9 0.032(2) 0.024(2) 0.036(2) -0.0026(16) 0.0059(16) 0.0025(16) C16 0.0234(18) 0.0221(19) 0.0315(19) 0.0019(15) 0.0079(15) 0.0019(14) C31 0.0237(17) 0.0254(19) 0.0174(16) 0.0035(13) 0.0011(13) 0.0004(14) C48 0.032(2) 0.033(2) 0.0199(17) -0.0027(15) 0.0000(15) 0.0081(16) F32 0.092(3) 0.162(4) 0.0433(19) 0.029(2) 0.0249(19) 0.006(3) F24 0.081(2) 0.0457(19) 0.126(3) -0.020(2) 0.016(2) 0.0127(17) C45 0.044(3) 0.067(4) 0.031(2) -0.012(2) -0.017(2) 0.007(2) C8 0.044(3) 0.030(2) 0.052(3) -0.0040(19) 0.012(2) -0.0096(19) C67 0.035(2) 0.0179(19) 0.039(2) 0.0044(15) -0.0044(17) -0.0020(15) C44 0.030(2) 0.048(3) 0.0212(18) -0.0089(17) -0.0024(15) 0.0004(18) C24 0.030(2) 0.063(3) 0.061(3) -0.006(3) -0.003(2) 0.002(2) F5 0.0353(17) 0.121(3) 0.103(3) 0.015(2) 0.0021(17) -0.0094(19) F34 0.136(4) 0.073(3) 0.114(3) -0.028(2) -0.009(3) 0.060(3) F31 0.205(5) 0.065(3) 0.122(4) 0.068(3) -0.078(4) -0.057(3) F6 0.078(3) 0.124(3) 0.079(3) 0.050(2) -0.015(2) -0.006(2) C33 0.037(2) 0.047(3) 0.0205(18) -0.0028(17) -0.0049(16) 0.0046(19) C51 0.044(3) 0.045(3) 0.056(3) -0.007(2) -0.009(2) -0.003(2) C10 0.036(2) 0.075(4) 0.029(2) 0.010(2) -0.0051(18) -0.005(2) F35 0.158(4) 0.125(4) 0.0369(18) -0.024(2) -0.010(2) 0.050(3) C40 0.063(3) 0.043(3) 0.039(2) -0.003(2) 0.006(2) -0.031(2) C55 0.039(2) 0.036(2) 0.039(2) 0.0058(18) 0.0101(18) 0.0072(18) C2 0.030(2) 0.023(2) 0.036(2) -0.0013(15) 0.0075(16) 0.0057(15) C63 0.041(2) 0.038(2) 0.039(2) 0.0069(19) -0.0126(19) -0.0113(19) C54 0.068(3) 0.048(3) 0.035(2) 0.001(2) 0.012(2) -0.015(2) C5 0.034(2) 0.040(2) 0.029(2) 0.0103(17) 0.0029(16) 0.0061(18) F23 0.044(2) 0.099(3) 0.160(4) -0.023(3) -0.025(2) 0.0055(19) C7 0.059(3) 0.035(3) 0.053(3) 0.015(2) 0.021(2) -0.005(2) C25 0.031(2) 0.046(3) 0.031(2) 0.0079(18) -0.0002(16) -0.0025(18) C49 0.039(2) 0.053(3) 0.032(2) -0.0081(19) -0.0052(18) -0.015(2) C36 0.041(2) 0.028(2) 0.030(2) 0.0032(16) 0.0050(17) -0.0083(17) F19 0.165(5) 0.184(5) 0.055(2) 0.068(3) -0.038(3) -0.105(4) C35 0.057(3) 0.038(3) 0.036(2) 0.0139(19) 0.013(2) -0.008(2) C47 0.059(3) 0.044(3) 0.030(2) 0.0058(19) -0.010(2) 0.016(2) C26 0.040(3) 0.098(5) 0.049(3) -0.014(3) 0.004(2) -0.003(3) F21 0.163(5) 0.117(4) 0.082(3) 0.026(2) -0.087(3) -0.043(3) C27 0.030(3) 0.097(5) 0.075(4) -0.018(3) 0.000(2) 0.006(3) C23 0.035(3) 0.080(4) 0.057(3) 0.018(3) -0.007(2) -0.003(2) F30 0.047(2) 0.157(5) 0.206(6) 0.057(4) 0.012(3) -0.040(3) F7 0.071(2) 0.084(3) 0.165(4) -0.046(3) 0.022(3) 0.036(2) C13 0.039(2) 0.049(3) 0.031(2) -0.0105(18) 0.0014(17) -0.0067(19) C22 0.032(2) 0.031(2) 0.051(3) -0.0035(19) -0.0089(19) -0.0001(18) F9 0.091(3) 0.135(4) 0.073(3) -0.048(3) 0.011(2) -0.018(3) C70 0.089(5) 0.047(3) 0.056(3) -0.012(3) 0.001(3) 0.015(3) C53 0.049(3) 0.049(3) 0.035(2) -0.013(2) 0.008(2) -0.002(2) C66 0.045(3) 0.059(3) 0.040(3) -0.010(2) 0.006(2) -0.010(2) C20 0.045(3) 0.037(3) 0.054(3) 0.019(2) -0.001(2) 0.004(2) C6 0.056(3) 0.048(3) 0.035(2) 0.019(2) 0.008(2) 0.004(2) C69 0.073(4) 0.046(3) 0.050(3) 0.024(2) -0.003(3) -0.004(3) C58 0.059(3) 0.054(3) 0.065(4) -0.005(3) 0.019(3) 0.010(3) F4 0.093(3) 0.111(4) 0.113(3) -0.051(3) -0.012(3) -0.021(3) C19 0.049(3) 0.028(2) 0.079(4) 0.013(2) -0.001(3) -0.005(2) F28 0.138(4) 0.0362(19) 0.147(4) 0.006(2) -0.068(3) -0.036(2) F20 0.140(4) 0.066(3) 0.135(4) 0.045(3) -0.081(3) -0.015(3) C46 0.062(3) 0.072(4) 0.029(2) 0.001(2) -0.022(2) 0.021(3) C41 0.086(5) 0.048(3) 0.092(5) -0.022(3) 0.020(4) -0.022(3) C11 0.062(4) 0.100(5) 0.059(4) -0.017(3) -0.008(3) -0.012(3) C18 0.042(3) 0.029(2) 0.068(3) 0.002(2) -0.005(2) -0.0061(19) C68 0.072(4) 0.049(4) 0.113(6) 0.011(4) -0.038(4) -0.016(3) C12 0.042(3) 0.132(6) 0.058(4) 0.031(4) -0.001(3) 0.023(3) C57 0.056(3) 0.065(4) 0.067(4) 0.004(3) 0.004(3) -0.007(3) C50 0.046(3) 0.087(5) 0.084(4) -0.037(4) 0.010(3) -0.025(3) C14 0.043(4) 0.073(8) 0.054(5) -0.001(5) -0.009(4) 0.009(4) C42 0.062(4) 0.082(5) 0.103(5) -0.018(4) -0.025(4) -0.014(3) C64 0.126(7) 0.077(5) 0.063(4) 0.029(4) -0.060(4) -0.033(5) C65 0.044(3) 0.042(3) 0.088(4) -0.012(3) -0.003(3) 0.002(2) C15 0.090(10) 0.098(8) 0.058(7) -0.043(7) -0.012(8) 0.036(8) C34 0.058(3) 0.049(3) 0.022(2) 0.0131(18) 0.0056(19) 0.008(2) C38 0.046(6) 0.035(5) 0.052(7) -0.004(4) 0.014(5) 0.000(4) C14B 0.030(5) 0.051(7) 0.054(7) -0.001(5) -0.007(4) -0.013(4) F1 0.124(4) 0.191(6) 0.066(3) 0.025(3) 0.047(3) -0.053(4) F2 0.112(4) 0.211(6) 0.101(3) 0.109(4) -0.023(3) -0.012(4) F3 0.160(5) 0.082(3) 0.190(6) 0.079(4) -0.026(4) -0.044(3) C56 0.103(6) 0.097(6) 0.072(5) 0.051(4) 0.000(4) -0.022(5) C71 0.047(6) 0.034(5) 0.056(8) 0.010(5) -0.010(5) -0.003(4) C39 0.032(4) 0.034(5) 0.108(13) -0.005(6) 0.022(6) -0.009(4) C14A 0.054(13) 0.083(15) 0.031(9) -0.004(10) -0.011(9) 0.007(12) C15A 0.14(3) 0.063(13) 0.054(16) -0.025(12) 0.01(2) -0.030(15) O2 0.068(2) 0.057(2) 0.0342(16) 0.0217(15) -0.0067(15) -0.0267(18) C59 0.035(3) 0.020(3) 0.025(3) 0.005(3) 0.005(3) -0.003(2) C62 0.069(4) 0.029(3) 0.038(3) 0.005(2) 0.000(3) -0.013(3) F17 0.079(4) 0.059(4) 0.049(3) 0.009(2) -0.014(3) -0.043(3) F16 0.172(10) 0.049(5) 0.077(5) 0.042(4) -0.052(5) -0.049(6) F18 0.119(6) 0.053(6) 0.084(6) -0.038(5) -0.013(5) 0.027(4) C60 0.042(3) 0.043(4) 0.032(3) 0.007(3) -0.002(2) -0.004(3) F11 0.074(4) 0.050(4) 0.053(5) 0.009(4) -0.018(3) -0.037(3) F12 0.044(3) 0.087(4) 0.076(3) 0.006(3) 0.003(2) 0.018(3) F10 0.055(3) 0.078(4) 0.033(2) 0.015(2) -0.009(2) -0.009(3) C61 0.048(4) 0.055(4) 0.060(4) -0.016(3) -0.006(3) 0.010(3) F15 0.107(5) 0.053(3) 0.064(4) -0.026(3) 0.008(3) 0.008(3) F13 0.067(4) 0.148(5) 0.050(3) 0.043(3) 0.032(3) 0.035(4) F14 0.035(2) 0.077(4) 0.053(3) 0.003(2) 0.0181(19) 0.013(2) C59A 0.042(6) 0.032(6) 0.027(6) 0.007(5) 0.004(5) -0.010(5) C61A 0.051(7) 0.078(9) 0.081(10) -0.029(7) 0.021(7) -0.016(6) F14A 0.049(8) 0.079(8) 0.182(17) -0.020(9) -0.005(10) 0.017(6) F15A 0.118(17) 0.31(3) 0.085(10) -0.063(12) 0.045(11) 0.070(17) F13A 0.058(8) 0.076(9) 0.100(10) -0.006(8) 0.004(8) -0.030(6) C62A 0.077(8) 0.047(7) 0.055(8) 0.008(5) 0.010(7) 0.007(7) F16A 0.067(7) 0.072(11) 0.172(16) 0.022(10) 0.024(8) 0.027(7) F17A 0.127(14) 0.035(7) 0.044(6) 0.008(5) 0.012(7) 0.019(9) F18A 0.079(9) 0.031(7) 0.053(7) 0.011(5) 0.006(7) 0.027(7) C60A 0.076(8) 0.059(7) 0.037(6) 0.005(6) -0.004(6) -0.026(6) F12A 0.070(7) 0.060(12) 0.050(9) 0.001(8) -0.019(5) -0.048(7) F10A 0.14(2) 0.087(13) 0.032(6) 0.010(7) -0.022(8) -0.063(12) F11A 0.105(10) 0.040(6) 0.099(11) -0.041(6) 0.038(7) -0.031(5) 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' Al Al 0.0645 0.0514 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C28 Tl1 C1 122.47(10) . . ? O4 Al1 O3 106.39(15) . . ? O4 Al1 O2 111.12(17) . . ? O1 Al1 O3 114.81(19) . . ? O1 Al1 O4 109.60(18) . . ? O1 Al1 O2 107.1(2) . . ? O2 Al1 O3 107.88(16) . . ? C1 N2 C3 112.5(3) . . ? C1 N2 C16 123.1(3) . . ? C3 N2 C16 124.3(3) . . ? C28 N3 C29 112.3(3) . . ? C28 N3 C31 125.9(3) . . ? C29 N3 C31 121.8(3) . . ? C48 C43 N4 118.5(3) . . ? C48 C43 C44 123.5(3) . . ? C44 C43 N4 117.9(3) . . ? C30 N4 C43 123.1(3) . . ? C28 N4 C43 124.6(3) . . ? C28 N4 C30 112.2(3) . . ? N2 C1 Tl1 108.7(2) . . ? N1 C1 Tl1 146.4(2) . . ? N1 C1 N2 102.4(3) . . ? C1 N1 C4 124.9(3) . . ? C1 N1 C2 112.3(3) . . ? C2 N1 C4 122.8(3) . . ? C9 C4 N1 118.9(3) . . ? C9 C4 C5 123.2(4) . . ? C5 C4 N1 117.9(3) . . ? C63 O3 Al1 150.5(3) . . ? C67 O4 Al1 153.4(3) . . ? C16 C21 C25 121.8(4) . . ? C16 C21 C20 117.1(4) . . ? C20 C21 C25 121.1(4) . . ? C48 C52 H52 107.4 . . ? C48 C52 C54 113.2(3) . . ? C54 C52 H52 107.4 . . ? C53 C52 H52 107.4 . . ? C53 C52 C48 109.8(3) . . ? C53 C52 C54 111.3(4) . . ? C32 C37 H37 105.6 . . ? C32 C37 H37A 107.4 . . ? C32 C37 C38 113.1(4) . . ? C32 C37 C14B 109.0(5) . . ? C38 C37 H37 105.6 . . ? C14B C37 H37A 107.4 . . ? C71 C37 H37A 107.4 . . ? C71 C37 C32 110.9(5) . . ? C71 C37 C14B 114.3(7) . . ? C39 C37 H37 105.6 . . ? C39 C37 C32 116.2(5) . . ? C39 C37 C38 109.8(7) . . ? C55 O1 Al1 152.7(3) . . ? N4 C30 H30 126.8 . . ? C29 C30 N4 106.5(3) . . ? C29 C30 H30 126.8 . . ? C16 C17 C22 121.7(4) . . ? C18 C17 C16 117.0(4) . . ? C18 C17 C22 121.2(4) . . ? C31 C32 C37 122.6(3) . . ? C33 C32 C37 120.8(3) . . ? C33 C32 C31 116.7(4) . . ? N3 C28 Tl1 142.0(2) . . ? N3 C28 N4 102.5(3) . . ? N4 C28 Tl1 111.0(2) . . ? N3 C29 H29 126.7 . . ? C30 C29 N3 106.5(3) . . ? C30 C29 H29 126.7 . . ? N2 C3 H3 127.0 . . ? C2 C3 N2 106.0(3) . . ? C2 C3 H3 127.0 . . ? C4 C9 C13 121.9(4) . . ? C8 C9 C4 117.3(4) . . ? C8 C9 C13 120.8(4) . . ? C21 C16 N2 118.1(3) . . ? C21 C16 C17 122.9(4) . . ? C17 C16 N2 118.9(3) . . ? C32 C31 N3 117.2(3) . . ? C36 C31 N3 119.1(3) . . ? C36 C31 C32 123.6(3) . . ? C43 C48 C52 121.4(3) . . ? C47 C48 C43 117.2(4) . . ? C47 C48 C52 121.4(4) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C46 C45 C44 121.2(4) . . ? C9 C8 H8 119.5 . . ? C7 C8 C9 120.9(4) . . ? C7 C8 H8 119.5 . . ? O4 C67 C70 109.1(4) . . ? O4 C67 C69 112.3(4) . . ? O4 C67 C68 107.8(4) . . ? C69 C67 C70 108.3(4) . . ? C69 C67 C68 110.2(4) . . ? C68 C67 C70 109.2(5) . . ? C43 C44 C49 122.2(4) . . ? C45 C44 C43 116.7(4) . . ? C45 C44 C49 121.1(4) . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? C32 C33 H33 119.4 . . ? C34 C33 C32 121.2(4) . . ? C34 C33 H33 119.4 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? C5 C10 H10 107.6 . . ? C5 C10 C11 111.7(4) . . ? C5 C10 C12 110.3(5) . . ? C11 C10 H10 107.6 . . ? C11 C10 C12 111.8(5) . . ? C12 C10 H10 107.6 . . ? C36 C40 H40 107.7 . . ? C36 C40 C41 112.2(5) . . ? C41 C40 H40 107.7 . . ? C42 C40 H40 107.7 . . ? C42 C40 C36 110.4(4) . . ? C42 C40 C41 110.9(5) . . ? O1 C55 C58 104.3(4) . . ? O1 C55 C57 109.0(4) . . ? O1 C55 C56 114.4(5) . . ? C57 C55 C58 109.4(4) . . ? C56 C55 C58 109.2(5) . . ? C56 C55 C57 110.3(5) . . ? N1 C2 H2 126.6 . . ? C3 C2 N1 106.8(3) . . ? C3 C2 H2 126.6 . . ? O3 C63 C66 112.0(4) . . ? O3 C63 C64 107.6(4) . . ? O3 C63 C65 108.4(4) . . ? C66 C63 C65 107.9(4) . . ? C64 C63 C66 110.4(5) . . ? C64 C63 C65 110.5(5) . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C4 C5 C10 122.4(4) . . ? C6 C5 C4 116.7(4) . . ? C6 C5 C10 120.9(4) . . ? C8 C7 H7 119.7 . . ? C6 C7 C8 120.5(4) . . ? C6 C7 H7 119.7 . . ? C21 C25 H25 107.7 . . ? C21 C25 C26 110.9(4) . . ? C21 C25 C27 112.3(4) . . ? C26 C25 H25 107.7 . . ? C26 C25 C27 110.3(4) . . ? C27 C25 H25 107.7 . . ? C44 C49 C51 110.5(4) . . ? C44 C49 H49 107.6 . . ? C44 C49 C50 113.2(5) . . ? C51 C49 H49 107.6 . . ? C50 C49 C51 110.1(4) . . ? C50 C49 H49 107.6 . . ? C31 C36 C40 123.0(4) . . ? C31 C36 C35 116.7(4) . . ? C35 C36 C40 120.3(4) . . ? C36 C35 H35 119.3 . . ? C34 C35 C36 121.5(4) . . ? C34 C35 H35 119.3 . . ? C48 C47 H47 119.9 . . ? C46 C47 C48 120.3(5) . . ? C46 C47 H47 119.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? C9 C13 H13 108.8 . . ? C9 C13 H13A 105.6 . . ? C9 C13 C14 111.4(5) . . ? C9 C13 C15 109.1(8) . . ? C9 C13 C14A 111.4(9) . . ? C9 C13 C15A 115(2) . . ? C14 C13 H13 108.8 . . ? C15 C13 H13 108.8 . . ? C15 C13 C14 109.9(7) . . ? C14A C13 H13A 105.6 . . ? C14A C13 C15A 113.1(19) . . ? C15A C13 H13A 105.6 . . ? C17 C22 C24 112.5(4) . . ? C17 C22 H22 107.2 . . ? C24 C22 H22 107.2 . . ? C23 C22 C17 112.2(4) . . ? C23 C22 C24 110.4(4) . . ? C23 C22 H22 107.2 . . ? F36 C70 C67 109.2(4) . . ? F34 C70 F36 107.2(6) . . ? F34 C70 C67 114.8(5) . . ? F34 C70 F35 106.1(5) . . ? F35 C70 F36 110.0(6) . . ? F35 C70 C67 109.4(5) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? F25 C66 F27 108.3(4) . . ? F25 C66 F26 107.6(4) . . ? F25 C66 C63 111.0(4) . . ? F27 C66 C63 113.0(4) . . ? F26 C66 F27 107.4(4) . . ? F26 C66 C63 109.5(4) . . ? C21 C20 H20 119.5 . . ? C19 C20 C21 120.9(4) . . ? C19 C20 H20 119.5 . . ? C5 C6 H6 119.3 . . ? C7 C6 C5 121.3(4) . . ? C7 C6 H6 119.3 . . ? F33 C69 C67 111.8(4) . . ? F32 C69 F33 106.1(5) . . ? F32 C69 C67 110.2(4) . . ? F32 C69 F31 109.1(5) . . ? F31 C69 F33 107.3(5) . . ? F31 C69 C67 112.2(5) . . ? F8 C58 C55 113.4(5) . . ? F8 C58 F7 110.9(5) . . ? F8 C58 F9 105.9(5) . . ? F7 C58 C55 111.8(5) . . ? F7 C58 F9 104.9(5) . . ? F9 C58 C55 109.4(5) . . ? C20 C19 H19 119.5 . . ? C18 C19 C20 121.1(4) . . ? C18 C19 H19 119.5 . . ? C45 C46 C47 121.1(4) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C18 H18 119.5 . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18 119.5 . . ? F29 C68 C67 110.9(5) . . ? F29 C68 F30 108.8(6) . . ? F29 C68 F28 108.7(6) . . ? F30 C68 C67 109.1(6) . . ? F30 C68 F28 106.9(6) . . ? F28 C68 C67 112.3(5) . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? F5 C57 F6 105.7(5) . . ? F5 C57 C55 113.1(5) . . ? F6 C57 C55 110.3(5) . . ? F4 C57 F5 109.0(5) . . ? F4 C57 F6 106.5(5) . . ? F4 C57 C55 112.0(5) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? F19 C64 C63 112.5(6) . . ? F19 C64 F21 108.4(7) . . ? F19 C64 F20 108.3(6) . . ? F21 C64 C63 111.7(5) . . ? F21 C64 F20 106.5(6) . . ? F20 C64 C63 109.1(6) . . ? F22 C65 F24 106.2(5) . . ? F22 C65 C63 111.4(4) . . ? F22 C65 F23 108.1(5) . . ? F24 C65 C63 112.0(4) . . ? F24 C65 F23 106.7(5) . . ? F23 C65 C63 112.1(5) . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C33 C34 H34 119.8 . . ? C35 C34 C33 120.4(4) . . ? C35 C34 H34 119.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C14B H14D 109.5 . . ? C37 C14B H14E 109.5 . . ? C37 C14B H14F 109.5 . . ? H14D C14B H14E 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? F1 C56 C55 116.2(7) . . ? F1 C56 F2 112.0(7) . . ? F1 C56 F3 105.7(7) . . ? F2 C56 C55 111.1(6) . . ? F2 C56 F3 103.2(7) . . ? F3 C56 C55 107.5(6) . . ? C37 C71 H71A 109.5 . . ? C37 C71 H71B 109.5 . . ? C37 C71 H71C 109.5 . . ? H71A C71 H71B 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C13 C14A H14G 109.5 . . ? C13 C14A H14H 109.5 . . ? C13 C14A H14I 109.5 . . ? H14G C14A H14H 109.5 . . ? H14G C14A H14I 109.5 . . ? H14H C14A H14I 109.5 . . ? C13 C15A H15D 109.5 . . ? C13 C15A H15E 109.5 . . ? C13 C15A H15F 109.5 . . ? H15D C15A H15E 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? C59 O2 Al1 147.6(4) . . ? C59A O2 Al1 154.8(7) . . ? O2 C59 C62 109.4(5) . . ? O2 C59 C60 115.7(5) . . ? O2 C59 C61 108.7(5) . . ? C62 C59 C60 109.4(5) . . ? C62 C59 C61 105.9(6) . . ? C60 C59 C61 107.3(5) . . ? F17 C62 C59 110.4(6) . . ? F16 C62 C59 111.1(7) . . ? F16 C62 F17 107.7(7) . . ? F18 C62 C59 112.2(8) . . ? F18 C62 F17 107.0(8) . . ? F18 C62 F16 108.2(9) . . ? F11 C60 C59 110.0(7) . . ? F12 C60 C59 110.3(6) . . ? F12 C60 F11 109.6(7) . . ? F10 C60 C59 113.8(6) . . ? F10 C60 F11 105.4(8) . . ? F10 C60 F12 107.6(6) . . ? F15 C61 C59 109.9(6) . . ? F15 C61 F13 111.2(7) . . ? F15 C61 F14 111.0(6) . . ? F13 C61 C59 109.3(6) . . ? F14 C61 C59 112.7(6) . . ? F14 C61 F13 102.6(6) . . ? O2 C59A C61A 103.2(10) . . ? O2 C59A C62A 109.1(11) . . ? O2 C59A C60A 103.6(10) . . ? C62A C59A C61A 113.8(12) . . ? C62A C59A C60A 113.7(11) . . ? C60A C59A C61A 112.2(11) . . ? F14A C61A C59A 94.0(11) . . ? F15A C61A C59A 104.7(15) . . ? F15A C61A F14A 106.6(15) . . ? F13A C61A C59A 109.6(13) . . ? F13A C61A F14A 114.6(14) . . ? F13A C61A F15A 123.0(17) . . ? F16A C62A C59A 109.3(13) . . ? F17A C62A C59A 109.2(16) . . ? F17A C62A F16A 106.4(15) . . ? F18A C62A C59A 114.2(14) . . ? F18A C62A F16A 107.3(14) . . ? F18A C62A F17A 110.1(15) . . ? F12A C60A C59A 106.3(14) . . ? F10A C60A C59A 109.1(15) . . ? F10A C60A F12A 107.8(16) . . ? F10A C60A F11A 119.2(15) . . ? F11A C60A C59A 104.4(11) . . ? F11A C60A F12A 109.4(14) . . ? 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 Tl1 C1 2.748(3) . ? Tl1 C28 2.706(3) . ? Al1 O3 1.722(3) . ? Al1 O4 1.708(3) . ? Al1 O1 1.684(3) . ? Al1 O2 1.719(3) . ? N2 C1 1.365(4) . ? N2 C3 1.379(5) . ? N2 C16 1.438(5) . ? F25 C66 1.320(6) . ? N3 C28 1.361(5) . ? N3 C29 1.383(4) . ? N3 C31 1.448(4) . ? C43 N4 1.438(4) . ? C43 C48 1.395(6) . ? C43 C44 1.401(5) . ? N4 C30 1.383(5) . ? N4 C28 1.365(4) . ? C1 N1 1.358(5) . ? F22 C65 1.314(7) . ? F33 C69 1.326(7) . ? N1 C4 1.447(5) . ? N1 C2 1.379(5) . ? C4 C9 1.394(6) . ? C4 C5 1.401(5) . ? O3 C63 1.345(5) . ? O4 C67 1.321(5) . ? C21 C16 1.394(5) . ? C21 C25 1.512(6) . ? C21 C20 1.398(6) . ? C52 H52 1.0000 . ? C52 C48 1.522(6) . ? C52 C54 1.523(6) . ? C52 C53 1.521(6) . ? C37 H37 1.0000 . ? C37 H37A 1.0000 . ? C37 C32 1.514(5) . ? C37 C38 1.562(9) . ? C37 C14B 1.553(9) . ? C37 C71 1.433(9) . ? C37 C39 1.465(9) . ? O1 C55 1.367(5) . ? F27 C66 1.329(6) . ? C30 H30 0.9500 . ? C30 C29 1.342(5) . ? C17 C16 1.405(6) . ? C17 C22 1.524(6) . ? C17 C18 1.397(6) . ? F8 C58 1.277(7) . ? C32 C31 1.394(5) . ? C32 C33 1.393(5) . ? C29 H29 0.9500 . ? F26 C66 1.328(6) . ? F36 C70 1.339(7) . ? F29 C68 1.316(7) . ? C3 H3 0.9500 . ? C3 C2 1.342(5) . ? C9 C8 1.392(6) . ? C9 C13 1.514(6) . ? C31 C36 1.391(5) . ? C48 C47 1.395(6) . ? F32 C69 1.315(7) . ? F24 C65 1.326(6) . ? C45 H45 0.9500 . ? C45 C44 1.389(6) . ? C45 C46 1.374(8) . ? C8 H8 0.9500 . ? C8 C7 1.378(7) . ? C67 C70 1.563(7) . ? C67 C69 1.540(6) . ? C67 C68 1.548(7) . ? C44 C49 1.511(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24 C22 1.527(6) . ? F5 C57 1.320(7) . ? F34 C70 1.294(7) . ? F31 C69 1.320(6) . ? F6 C57 1.352(7) . ? C33 H33 0.9500 . ? C33 C34 1.377(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C51 C49 1.536(7) . ? C10 H10 1.0000 . ? C10 C5 1.510(6) . ? C10 C11 1.520(8) . ? C10 C12 1.531(7) . ? F35 C70 1.334(7) . ? C40 H40 1.0000 . ? C40 C36 1.516(6) . ? C40 C41 1.526(8) . ? C40 C42 1.513(8) . ? C55 C58 1.546(7) . ? C55 C57 1.534(8) . ? C55 C56 1.509(7) . ? C2 H2 0.9500 . ? C63 C66 1.549(7) . ? C63 C64 1.542(7) . ? C63 C65 1.559(7) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C5 C6 1.395(6) . ? F23 C65 1.330(7) . ? C7 H7 0.9500 . ? C7 C6 1.374(7) . ? C25 H25 1.0000 . ? C25 C26 1.516(6) . ? C25 C27 1.522(7) . ? C49 H49 1.0000 . ? C49 C50 1.525(7) . ? C36 C35 1.392(6) . ? F19 C64 1.276(10) . ? C35 H35 0.9500 . ? C35 C34 1.367(7) . ? C47 H47 0.9500 . ? C47 C46 1.384(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? F21 C64 1.340(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23 C22 1.508(7) . ? F30 C68 1.336(10) . ? F7 C58 1.321(6) . ? C13 H13 1.0000 . ? C13 H13A 1.0000 . ? C13 C14 1.527(8) . ? C13 C15 1.523(9) . ? C13 C14A 1.516(14) . ? C13 C15A 1.524(15) . ? C22 H22 1.0000 . ? F9 C58 1.353(7) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C20 H20 0.9500 . ? C20 C19 1.374(7) . ? C6 H6 0.9500 . ? F4 C57 1.294(7) . ? C19 H19 0.9500 . ? C19 C18 1.368(7) . ? F28 C68 1.339(8) . ? F20 C64 1.385(10) . ? C46 H46 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C18 H18 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C34 H34 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? F1 C56 1.266(10) . ? F2 C56 1.320(9) . ? F3 C56 1.377(10) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C14A H14G 0.9800 . ? C14A H14H 0.9800 . ? C14A H14I 0.9800 . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? O2 C59 1.342(8) . ? O2 C59A 1.346(15) . ? C59 C62 1.545(8) . ? C59 C60 1.550(9) . ? C59 C61 1.588(9) . ? C62 F17 1.337(9) . ? C62 F16 1.322(9) . ? C62 F18 1.300(10) . ? C60 F11 1.350(9) . ? C60 F12 1.323(8) . ? C60 F10 1.315(8) . ? C61 F15 1.341(8) . ? C61 F13 1.387(9) . ? C61 F14 1.356(8) . ? C59A C61A 1.549(16) . ? C59A C62A 1.513(16) . ? C59A C60A 1.532(16) . ? C61A F14A 1.396(14) . ? C61A F15A 1.346(14) . ? C61A F13A 1.342(13) . ? C62A F16A 1.370(14) . ? C62A F17A 1.357(15) . ? C62A F18A 1.356(14) . ? C60A F12A 1.393(15) . ? C60A F10A 1.352(14) . ? C60A F11A 1.382(14) . ? 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 Tl1 C1 N1 C4 21.0(6) . . . . ? Tl1 C1 N1 C2 -158.2(4) . . . . ? Al1 O3 C63 C66 -43.5(8) . . . . ? Al1 O3 C63 C64 -165.0(6) . . . . ? Al1 O3 C63 C65 75.4(8) . . . . ? Al1 O4 C67 C70 64.2(8) . . . . ? Al1 O4 C67 C69 -55.8(8) . . . . ? Al1 O4 C67 C68 -177.4(6) . . . . ? Al1 O1 C55 C58 -140.7(7) . . . . ? Al1 O1 C55 C57 102.5(8) . . . . ? Al1 O1 C55 C56 -21.4(10) . . . . ? Al1 O2 C59 C62 -111.5(8) . . . . ? Al1 O2 C59 C60 12.6(11) . . . . ? Al1 O2 C59 C61 133.3(6) . . . . ? Al1 O2 C59A C61A 173.2(10) . . . . ? Al1 O2 C59A C62A -65(2) . . . . ? Al1 O2 C59A C60A 56(2) . . . . ? N2 C1 N1 C4 178.7(3) . . . . ? N2 C1 N1 C2 -0.5(4) . . . . ? N2 C3 C2 N1 0.6(4) . . . . ? N3 C31 C36 C40 3.0(6) . . . . ? N3 C31 C36 C35 -176.6(4) . . . . ? C43 N4 C30 C29 176.3(3) . . . . ? C43 N4 C28 Tl1 -14.4(4) . . . . ? C43 N4 C28 N3 -176.3(3) . . . . ? C43 C48 C47 C46 0.5(7) . . . . ? C43 C44 C49 C51 94.5(5) . . . . ? C43 C44 C49 C50 -141.5(4) . . . . ? N4 C43 C48 C52 2.7(5) . . . . ? N4 C43 C48 C47 -177.6(3) . . . . ? N4 C43 C44 C45 177.5(4) . . . . ? N4 C43 C44 C49 0.0(5) . . . . ? N4 C30 C29 N3 0.1(4) . . . . ? C1 N2 C3 C2 -1.0(4) . . . . ? C1 N2 C16 C21 -78.8(5) . . . . ? C1 N2 C16 C17 101.6(4) . . . . ? C1 N1 C4 C9 100.5(4) . . . . ? C1 N1 C4 C5 -82.3(5) . . . . ? C1 N1 C2 C3 -0.1(4) . . . . ? N1 C4 C9 C8 178.4(3) . . . . ? N1 C4 C9 C13 -0.1(5) . . . . ? N1 C4 C5 C10 -0.6(6) . . . . ? N1 C4 C5 C6 -178.8(4) . . . . ? C4 N1 C2 C3 -179.2(3) . . . . ? C4 C9 C8 C7 0.0(6) . . . . ? C4 C9 C13 C14 -128.8(8) . . . . ? C4 C9 C13 C15 109.7(9) . . . . ? C4 C9 C13 C14A -95.4(19) . . . . ? C4 C9 C13 C15A 135(2) . . . . ? C4 C5 C6 C7 0.8(7) . . . . ? O3 Al1 O4 C67 27.9(7) . . . . ? O3 Al1 O1 C55 76.6(8) . . . . ? O3 Al1 O2 C59 170.3(7) . . . . ? O3 Al1 O2 C59A 165.1(16) . . . . ? O3 C63 C66 F25 44.1(5) . . . . ? O3 C63 C66 F27 165.9(4) . . . . ? O3 C63 C66 F26 -74.5(5) . . . . ? O3 C63 C64 F19 43.7(8) . . . . ? O3 C63 C64 F21 165.9(7) . . . . ? O3 C63 C64 F20 -76.6(6) . . . . ? O3 C63 C65 F22 -77.5(5) . . . . ? O3 C63 C65 F24 41.3(6) . . . . ? O3 C63 C65 F23 161.2(4) . . . . ? O4 Al1 O3 C63 -166.3(6) . . . . ? O4 Al1 O1 C55 -43.0(8) . . . . ? O4 Al1 O2 C59 -73.4(8) . . . . ? O4 Al1 O2 C59A -78.6(16) . . . . ? O4 C67 C70 F36 -45.4(6) . . . . ? O4 C67 C70 F34 -165.8(5) . . . . ? O4 C67 C70 F35 75.0(6) . . . . ? O4 C67 C69 F33 78.2(5) . . . . ? O4 C67 C69 F32 -39.5(6) . . . . ? O4 C67 C69 F31 -161.2(5) . . . . ? O4 C67 C68 F29 -42.7(7) . . . . ? O4 C67 C68 F30 77.1(6) . . . . ? O4 C67 C68 F28 -164.5(5) . . . . ? C21 C20 C19 C18 1.4(8) . . . . ? C52 C48 C47 C46 -179.8(4) . . . . ? C37 C32 C31 N3 -5.2(5) . . . . ? C37 C32 C31 C36 179.3(4) . . . . ? C37 C32 C33 C34 -178.4(4) . . . . ? O1 Al1 O3 C63 72.3(7) . . . . ? O1 Al1 O4 C67 152.6(7) . . . . ? O1 Al1 O2 C59 46.3(8) . . . . ? O1 Al1 O2 C59A 41.0(16) . . . . ? O1 C55 C58 F8 -39.0(6) . . . . ? O1 C55 C58 F7 -165.2(5) . . . . ? O1 C55 C58 F9 79.0(5) . . . . ? O1 C55 C57 F5 -169.0(5) . . . . ? O1 C55 C57 F6 73.0(6) . . . . ? O1 C55 C57 F4 -45.3(6) . . . . ? O1 C55 C56 F1 -162.5(6) . . . . ? O1 C55 C56 F2 -32.8(9) . . . . ? O1 C55 C56 F3 79.4(7) . . . . ? C30 N4 C28 Tl1 162.1(2) . . . . ? C30 N4 C28 N3 0.3(4) . . . . ? C32 C31 C36 C40 178.5(4) . . . . ? C32 C31 C36 C35 -1.2(6) . . . . ? C32 C33 C34 C35 -0.6(7) . . . . ? C28 N3 C29 C30 0.0(4) . . . . ? C28 N3 C31 C32 98.6(4) . . . . ? C28 N3 C31 C36 -85.7(5) . . . . ? C28 N4 C30 C29 -0.3(4) . . . . ? C29 N3 C28 Tl1 -152.0(3) . . . . ? C29 N3 C28 N4 -0.2(4) . . . . ? C29 N3 C31 C32 -81.4(4) . . . . ? C29 N3 C31 C36 94.4(4) . . . . ? C3 N2 C1 Tl1 168.1(2) . . . . ? C3 N2 C1 N1 0.9(4) . . . . ? C3 N2 C16 C21 98.4(4) . . . . ? C3 N2 C16 C17 -81.1(5) . . . . ? C9 C4 C5 C10 176.5(4) . . . . ? C9 C4 C5 C6 -1.8(6) . . . . ? C9 C8 C7 C6 -1.0(7) . . . . ? C16 N2 C1 Tl1 -14.4(4) . . . . ? C16 N2 C1 N1 178.4(3) . . . . ? C16 N2 C3 C2 -178.5(3) . . . . ? C16 C21 C25 C26 -106.5(5) . . . . ? C16 C21 C25 C27 129.6(5) . . . . ? C16 C21 C20 C19 0.0(7) . . . . ? C16 C17 C22 C24 144.9(4) . . . . ? C16 C17 C22 C23 -89.9(5) . . . . ? C16 C17 C18 C19 -0.7(7) . . . . ? C31 N3 C28 Tl1 28.1(6) . . . . ? C31 N3 C28 N4 179.9(3) . . . . ? C31 N3 C29 C30 180.0(3) . . . . ? C31 C32 C33 C34 1.1(6) . . . . ? C31 C36 C35 C34 1.7(7) . . . . ? C48 C43 N4 C30 89.9(4) . . . . ? C48 C43 N4 C28 -93.9(4) . . . . ? C48 C43 C44 C45 0.1(6) . . . . ? C48 C43 C44 C49 -177.4(4) . . . . ? C48 C47 C46 C45 -0.7(8) . . . . ? C45 C44 C49 C51 -82.9(5) . . . . ? C45 C44 C49 C50 41.1(6) . . . . ? C8 C9 C13 C14 52.7(9) . . . . ? C8 C9 C13 C15 -68.8(9) . . . . ? C8 C9 C13 C14A 86.1(19) . . . . ? C8 C9 C13 C15A -44(2) . . . . ? C8 C7 C6 C5 0.6(8) . . . . ? C44 C43 N4 C30 -87.6(4) . . . . ? C44 C43 N4 C28 88.6(4) . . . . ? C44 C43 C48 C52 -179.9(3) . . . . ? C44 C43 C48 C47 -0.2(6) . . . . ? C44 C45 C46 C47 0.6(8) . . . . ? C33 C32 C31 N3 175.4(3) . . . . ? C33 C32 C31 C36 -0.2(6) . . . . ? C10 C5 C6 C7 -177.5(5) . . . . ? C40 C36 C35 C34 -178.0(5) . . . . ? C2 N1 C4 C9 -80.4(5) . . . . ? C2 N1 C4 C5 96.8(4) . . . . ? C54 C52 C48 C43 -145.1(4) . . . . ? C54 C52 C48 C47 35.3(6) . . . . ? C5 C4 C9 C8 1.4(6) . . . . ? C5 C4 C9 C13 -177.2(4) . . . . ? C25 C21 C16 N2 -3.7(5) . . . . ? C25 C21 C16 C17 175.8(4) . . . . ? C25 C21 C20 C19 -177.6(4) . . . . ? C36 C35 C34 C33 -0.9(7) . . . . ? C13 C9 C8 C7 178.6(4) . . . . ? C22 C17 C16 N2 2.6(6) . . . . ? C22 C17 C16 C21 -176.9(4) . . . . ? C22 C17 C18 C19 178.4(5) . . . . ? C70 C67 C69 F33 -42.3(6) . . . . ? C70 C67 C69 F32 -160.0(5) . . . . ? C70 C67 C69 F31 78.3(6) . . . . ? C70 C67 C68 F29 75.7(7) . . . . ? C70 C67 C68 F30 -164.5(5) . . . . ? C70 C67 C68 F28 -46.1(7) . . . . ? C53 C52 C48 C43 89.7(4) . . . . ? C53 C52 C48 C47 -89.9(5) . . . . ? C66 C63 C64 F19 -78.8(7) . . . . ? C66 C63 C64 F21 43.3(9) . . . . ? C66 C63 C64 F20 160.9(5) . . . . ? C66 C63 C65 F22 44.0(5) . . . . ? C66 C63 C65 F24 162.9(4) . . . . ? C66 C63 C65 F23 -77.3(5) . . . . ? C20 C21 C16 N2 178.7(4) . . . . ? C20 C21 C16 C17 -1.8(6) . . . . ? C20 C21 C25 C26 71.1(6) . . . . ? C20 C21 C25 C27 -52.9(6) . . . . ? C20 C19 C18 C17 -1.0(8) . . . . ? C69 C67 C70 F36 77.1(5) . . . . ? C69 C67 C70 F34 -43.4(7) . . . . ? C69 C67 C70 F35 -162.5(5) . . . . ? C69 C67 C68 F29 -165.5(6) . . . . ? C69 C67 C68 F30 -45.7(6) . . . . ? C69 C67 C68 F28 72.7(7) . . . . ? C58 C55 C57 F5 77.5(6) . . . . ? C58 C55 C57 F6 -40.5(6) . . . . ? C58 C55 C57 F4 -158.9(5) . . . . ? C58 C55 C56 F1 -46.0(8) . . . . ? C58 C55 C56 F2 83.7(8) . . . . ? C58 C55 C56 F3 -164.1(6) . . . . ? C46 C45 C44 C43 -0.3(7) . . . . ? C46 C45 C44 C49 177.2(5) . . . . ? C41 C40 C36 C31 -127.3(5) . . . . ? C41 C40 C36 C35 52.4(6) . . . . ? C11 C10 C5 C4 118.0(5) . . . . ? C11 C10 C5 C6 -63.8(6) . . . . ? C18 C17 C16 N2 -178.4(4) . . . . ? C18 C17 C16 C21 2.1(6) . . . . ? C18 C17 C22 C24 -34.1(6) . . . . ? C18 C17 C22 C23 91.0(5) . . . . ? C68 C67 C70 F36 -162.9(5) . . . . ? C68 C67 C70 F34 76.6(6) . . . . ? C68 C67 C70 F35 -42.5(6) . . . . ? C68 C67 C69 F33 -161.7(5) . . . . ? C68 C67 C69 F32 80.7(6) . . . . ? C68 C67 C69 F31 -41.0(7) . . . . ? C12 C10 C5 C4 -117.0(5) . . . . ? C12 C10 C5 C6 61.2(6) . . . . ? C57 C55 C58 F8 77.5(6) . . . . ? C57 C55 C58 F7 -48.7(6) . . . . ? C57 C55 C58 F9 -164.5(4) . . . . ? C57 C55 C56 F1 74.3(8) . . . . ? C57 C55 C56 F2 -156.0(7) . . . . ? C57 C55 C56 F3 -43.8(8) . . . . ? C42 C40 C36 C31 108.4(5) . . . . ? C42 C40 C36 C35 -71.9(6) . . . . ? C64 C63 C66 F25 164.0(5) . . . . ? C64 C63 C66 F27 -74.2(6) . . . . ? C64 C63 C66 F26 45.4(6) . . . . ? C64 C63 C65 F22 164.8(5) . . . . ? C64 C63 C65 F24 -76.4(6) . . . . ? C64 C63 C65 F23 43.5(6) . . . . ? C65 C63 C66 F25 -75.2(5) . . . . ? C65 C63 C66 F27 46.6(5) . . . . ? C65 C63 C66 F26 166.2(4) . . . . ? C65 C63 C64 F19 162.0(6) . . . . ? C65 C63 C64 F21 -75.9(8) . . . . ? C65 C63 C64 F20 41.7(6) . . . . ? C38 C37 C32 C31 -127.2(7) . . . . ? C38 C37 C32 C33 52.2(8) . . . . ? C14B C37 C32 C31 144.0(7) . . . . ? C14B C37 C32 C33 -36.6(8) . . . . ? C56 C55 C58 F8 -161.7(6) . . . . ? C56 C55 C58 F7 72.0(7) . . . . ? C56 C55 C58 F9 -43.7(6) . . . . ? C56 C55 C57 F5 -42.6(7) . . . . ? C56 C55 C57 F6 -160.7(6) . . . . ? C56 C55 C57 F4 81.0(7) . . . . ? C71 C37 C32 C31 -89.2(8) . . . . ? C71 C37 C32 C33 90.2(8) . . . . ? C39 C37 C32 C31 104.4(9) . . . . ? C39 C37 C32 C33 -76.2(9) . . . . ? O2 Al1 O3 C63 -47.0(7) . . . . ? O2 Al1 O4 C67 -89.3(7) . . . . ? O2 Al1 O1 C55 -163.6(7) . . . . ? O2 C59 C62 F17 -68.8(7) . . . . ? O2 C59 C62 F16 171.8(8) . . . . ? O2 C59 C62 F18 50.5(9) . . . . ? O2 C59 C60 F11 42.5(9) . . . . ? O2 C59 C60 F12 -78.5(7) . . . . ? O2 C59 C60 F10 160.4(7) . . . . ? O2 C59 C61 F15 -82.6(7) . . . . ? O2 C59 C61 F13 155.1(6) . . . . ? O2 C59 C61 F14 41.7(8) . . . . ? O2 C59A C61A F14A -34.5(13) . . . . ? O2 C59A C61A F15A -142.8(16) . . . . ? O2 C59A C61A F13A 83.4(14) . . . . ? O2 C59A C62A F16A 77.7(15) . . . . ? O2 C59A C62A F17A -38.4(17) . . . . ? O2 C59A C62A F18A -162.2(15) . . . . ? O2 C59A C60A F12A -51.6(16) . . . . ? O2 C59A C60A F10A -167.5(14) . . . . ? O2 C59A C60A F11A 64.0(13) . . . . ? C62 C59 C60 F11 166.5(7) . . . . ? C62 C59 C60 F12 45.6(7) . . . . ? C62 C59 C60 F10 -75.5(9) . . . . ? C62 C59 C61 F15 159.9(6) . . . . ? C62 C59 C61 F13 37.7(8) . . . . ? C62 C59 C61 F14 -75.8(7) . . . . ? C60 C59 C62 F17 163.5(5) . . . . ? C60 C59 C62 F16 44.1(9) . . . . ? C60 C59 C62 F18 -77.2(9) . . . . ? C60 C59 C61 F15 43.1(7) . . . . ? C60 C59 C61 F13 -79.1(7) . . . . ? C60 C59 C61 F14 167.5(6) . . . . ? C61 C59 C62 F17 48.2(7) . . . . ? C61 C59 C62 F16 -71.2(9) . . . . ? C61 C59 C62 F18 167.5(7) . . . . ? C61 C59 C60 F11 -79.0(8) . . . . ? C61 C59 C60 F12 160.0(6) . . . . ? C61 C59 C60 F10 38.9(9) . . . . ? C61A C59A C62A F16A -167.7(14) . . . . ? C61A C59A C62A F17A 76.3(18) . . . . ? C61A C59A C62A F18A -47(2) . . . . ? C61A C59A C60A F12A -162.2(16) . . . . ? C61A C59A C60A F10A 81.8(16) . . . . ? C61A C59A C60A F11A -46.7(15) . . . . ? C62A C59A C61A F14A -152.6(13) . . . . ? C62A C59A C61A F15A 99.0(18) . . . . ? C62A C59A C61A F13A -34.7(18) . . . . ? C62A C59A C60A F12A 66.8(18) . . . . ? C62A C59A C60A F10A -49.2(18) . . . . ? C62A C59A C60A F11A -177.7(12) . . . . ? C60A C59A C61A F14A 76.4(14) . . . . ? C60A C59A C61A F15A -31.9(18) . . . . ? C60A C59A C61A F13A -165.6(13) . . . . ? C60A C59A C62A F16A -37.4(18) . . . . ? C60A C59A C62A F17A -153.5(15) . . . . ? C60A C59A C62A F18A 82.7(18) . . . . ?