# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ofm27p-1Compound_1 _audit_creation_method SHELXL-97 _chemical_name_common 'Tki(Me3(PriPh)3)Tl BArF, Compound 1 ' _chemical_formula_moiety '(C32 H12 B F24)2,(C34 H43 N3 Tl)2, C6H14' _chemical_formula_sum 'C138 H124 B2 F48 N6 Tl2' _chemical_melting_point 436(2) _exptl_crystal_description rhomb _exptl_crystal_colour colorless _diffrn_ambient_temperature 120(2) _chemical_formula_weight 3208.82 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8319(4) _cell_length_b 16.0697(5) _cell_length_c 17.3854(6) _cell_angle_alpha 98.692(3) _cell_angle_beta 105.005(3) _cell_angle_gamma 90.030(2) _cell_volume 3419.99(19) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11719 _cell_measurement_theta_min 2.5593 _cell_measurement_theta_max 28.6464 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1598 _exptl_absorpt_coefficient_mu 2.479 _exptl_absorpt_correction_T_min 0.64180 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis RED,Empirical,spherical harmonics' _exptl_special_details ? _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, Sapphire2' _diffrn_detector_area_resol_mean 8.3367 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24638 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0900 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 26.37 _reflns_number_total 13958 _reflns_number_gt 10498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13958 _refine_ls_number_parameters 966 _refine_ls_number_restraints 542 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.8504(3) 0.3717(3) 0.7014(2) 0.0172(9) Uani 1 1 d . . . C1 C 0.2345(3) 0.8173(2) 0.80485(19) 0.0182(8) Uani 1 1 d U . . H1 H 0.1816 0.7712 0.7778 0.022 Uiso 1 1 calc R . . C2 C 0.2571(3) 0.8177(2) 0.8955(2) 0.0178(8) Uani 1 1 d U . . C3 C 0.1670(3) 0.7824(2) 0.9222(2) 0.0315(10) Uani 1 1 d U . . H3A H 0.1871 0.7869 0.9799 0.047 Uiso 1 1 calc R . . H3B H 0.1527 0.7242 0.8985 0.047 Uiso 1 1 calc R . . H3C H 0.1033 0.8134 0.9055 0.047 Uiso 1 1 calc R . . C4 C 0.3719(3) 0.8578(2) 1.0257(2) 0.0158(8) Uani 1 1 d U . . C5 C 0.4516(3) 0.8098(2) 1.0668(2) 0.0196(8) Uani 1 1 d . . . C6 C 0.4801(3) 0.8274(2) 1.1509(2) 0.0258(9) Uani 1 1 d . . . H6 H 0.5321 0.7958 1.1801 0.031 Uiso 1 1 calc R . . C7 C 0.4326(3) 0.8910(2) 1.1921(2) 0.0279(9) Uani 1 1 d . . . H7 H 0.4536 0.9017 1.2481 0.033 Uiso 1 1 calc R . . C8 C 0.3548(3) 0.9384(2) 1.1503(2) 0.0241(9) Uani 1 1 d . . . H8 H 0.3229 0.9810 1.1776 0.029 Uiso 1 1 calc R . . C9 C 0.3249(3) 0.9213(2) 1.0668(2) 0.0185(8) Uani 1 1 d . . . H9 H 0.2725 0.9529 1.0379 0.022 Uiso 1 1 calc R . . C10 C 0.5013(3) 0.7389(2) 1.0229(2) 0.0235(9) Uani 1 1 d . . . H10 H 0.4809 0.7445 0.9656 0.028 Uiso 1 1 calc R . . C11 C 0.4557(4) 0.6548(3) 1.0302(3) 0.0644(16) Uani 1 1 d . . . H11A H 0.4760 0.6467 1.0856 0.097 Uiso 1 1 calc R . . H11B H 0.4836 0.6107 0.9983 0.097 Uiso 1 1 calc R . . H11C H 0.3783 0.6535 1.0112 0.097 Uiso 1 1 calc R . . C12 C 0.6221(3) 0.7414(3) 1.0498(3) 0.0632(16) Uani 1 1 d . . . H12A H 0.6501 0.7943 1.0426 0.095 Uiso 1 1 calc R . . H12B H 0.6488 0.6962 1.0184 0.095 Uiso 1 1 calc R . . H12C H 0.6449 0.7354 1.1058 0.095 Uiso 1 1 calc R . . C13 C 0.1865(3) 0.8985(2) 0.7794(2) 0.0196(8) Uani 1 1 d U . . C14 C 0.1138(3) 0.8896(2) 0.6965(2) 0.0316(10) Uani 1 1 d U . . H14A H 0.0887 0.9439 0.6853 0.047 Uiso 1 1 calc R . . H14B H 0.0532 0.8526 0.6924 0.047 Uiso 1 1 calc R . . H14C H 0.1526 0.8666 0.6584 0.047 Uiso 1 1 calc R . . C15 C 0.1832(3) 1.0468(2) 0.8064(2) 0.0252(8) Uani 1 1 d U . . C16 C 0.1188(3) 1.0964(2) 0.8473(2) 0.0338(9) Uani 1 1 d U . . C17 C 0.1001(4) 1.1764(3) 0.8265(3) 0.0472(11) Uani 1 1 d U . . H17 H 0.0566 1.2111 0.8515 0.057 Uiso 1 1 calc R . . C18 C 0.1418(4) 1.2059(3) 0.7718(3) 0.0505(12) Uani 1 1 d U . . H18 H 0.1264 1.2599 0.7601 0.061 Uiso 1 1 calc R . . C19 C 0.2073(4) 1.1570(3) 0.7328(3) 0.0439(11) Uani 1 1 d U . . H19 H 0.2370 1.1776 0.6956 0.053 Uiso 1 1 calc R . . C20 C 0.2272(3) 1.0765(2) 0.7508(2) 0.0302(9) Uani 1 1 d U . . H20 H 0.2706 1.0422 0.7252 0.036 Uiso 1 1 calc R . . C21 C 0.0791(3) 1.0664(3) 0.9130(3) 0.0446(11) Uani 1 1 d U . . H21 H 0.0857 1.0052 0.9082 0.054 Uiso 1 1 calc R . . C22 C -0.0389(4) 1.0858(4) 0.9086(3) 0.083(2) Uani 1 1 d . . . H22A H -0.0486 1.1449 0.9074 0.125 Uiso 1 1 calc R . . H22B H -0.0573 1.0708 0.9549 0.125 Uiso 1 1 calc R . . H22C H -0.0847 1.0540 0.8605 0.125 Uiso 1 1 calc R . . C23 C 0.1506(4) 1.1067(3) 0.9952(3) 0.0508(13) Uani 1 1 d . . . H23A H 0.2241 1.0921 0.9992 0.076 Uiso 1 1 calc R . . H23B H 0.1266 1.0865 1.0372 0.076 Uiso 1 1 calc R . . H23C H 0.1459 1.1668 1.0008 0.076 Uiso 1 1 calc R . . C24 C 0.3367(3) 0.7995(2) 0.77732(19) 0.0173(8) Uani 1 1 d U . . C25 C 0.3587(3) 0.7085(2) 0.7578(2) 0.0295(9) Uani 1 1 d U . . H25A H 0.4216 0.7036 0.7375 0.044 Uiso 1 1 calc R . . H25B H 0.2978 0.6805 0.7176 0.044 Uiso 1 1 calc R . . H25C H 0.3707 0.6829 0.8056 0.044 Uiso 1 1 calc R . . C26 C 0.4970(3) 0.8529(2) 0.7556(2) 0.0188(8) Uani 1 1 d U . . C27 C 0.5079(3) 0.8768(2) 0.6840(2) 0.0247(8) Uani 1 1 d U . . C28 C 0.6109(3) 0.8755(2) 0.6720(3) 0.0339(9) Uani 1 1 d U . . H28 H 0.6209 0.8908 0.6248 0.041 Uiso 1 1 calc R . . C29 C 0.6981(3) 0.8524(2) 0.7276(3) 0.0358(10) Uani 1 1 d U . . H29 H 0.7662 0.8534 0.7183 0.043 Uiso 1 1 calc R . . C30 C 0.6859(3) 0.8278(2) 0.7973(3) 0.0338(9) Uani 1 1 d U . . H30 H 0.7451 0.8110 0.8344 0.041 Uiso 1 1 calc R . . C31 C 0.5849(3) 0.8282(2) 0.8117(2) 0.0260(9) Uani 1 1 d U . . H31 H 0.5759 0.8120 0.8588 0.031 Uiso 1 1 calc R . . C32 C 0.4097(3) 0.8999(2) 0.6228(2) 0.0323(9) Uani 1 1 d U . . H32 H 0.3603 0.9271 0.6525 0.039 Uiso 1 1 calc R . . C33 C 0.3511(4) 0.8211(3) 0.5696(2) 0.0455(12) Uani 1 1 d . . . H33A H 0.3973 0.7933 0.5391 0.068 Uiso 1 1 calc R . . H33B H 0.2866 0.8365 0.5333 0.068 Uiso 1 1 calc R . . H33C H 0.3326 0.7838 0.6026 0.068 Uiso 1 1 calc R . . C34 C 0.4351(4) 0.9619(3) 0.5704(3) 0.0617(15) Uani 1 1 d . . . H34A H 0.4789 1.0086 0.6043 0.093 Uiso 1 1 calc R . . H34B H 0.3690 0.9820 0.5402 0.093 Uiso 1 1 calc R . . H34C H 0.4734 0.9338 0.5339 0.093 Uiso 1 1 calc R . . C35 C 0.8749(3) 0.2788(2) 0.6584(2) 0.0171(8) Uani 1 1 d U . . C36 C 0.8360(3) 0.2035(2) 0.6739(2) 0.0174(8) Uani 1 1 d . . . H36 H 0.7905 0.2063 0.7080 0.021 Uiso 1 1 calc R . . C37 C 0.8619(3) 0.1251(2) 0.6410(2) 0.0179(8) Uani 1 1 d . A . C38 C 0.9303(3) 0.1180(2) 0.5909(2) 0.0196(8) Uani 1 1 d . . . H38 H 0.9474 0.0654 0.5680 0.024 Uiso 1 1 calc R . . C39 C 0.9729(3) 0.1908(2) 0.5755(2) 0.0196(8) Uani 1 1 d . A . C40 C 0.9452(3) 0.2694(2) 0.60855(19) 0.0171(8) Uani 1 1 d U . . H40 H 0.9746 0.3174 0.5970 0.021 Uiso 1 1 calc R . . C41 C 0.8176(3) 0.0470(2) 0.6584(2) 0.0262(9) Uani 1 1 d D . . C42 C 1.0464(3) 0.1878(2) 0.5218(2) 0.0292(10) Uani 1 1 d D . . C43 C 0.7293(3) 0.3770(2) 0.7168(2) 0.0194(8) Uani 1 1 d . . . C44 C 0.7066(3) 0.4410(2) 0.7729(2) 0.0187(8) Uani 1 1 d . . . H44 H 0.7633 0.4758 0.8065 0.022 Uiso 1 1 calc R . . C45 C 0.6028(3) 0.4551(2) 0.7810(2) 0.0195(8) Uani 1 1 d . . . C46 C 0.5171(3) 0.4034(2) 0.7332(2) 0.0209(8) Uani 1 1 d . . . H46 H 0.4476 0.4116 0.7390 0.025 Uiso 1 1 calc R . . C47 C 0.5363(3) 0.3399(2) 0.6771(2) 0.0208(8) Uani 1 1 d . A . C48 C 0.6403(3) 0.3269(2) 0.6681(2) 0.0202(8) Uani 1 1 d . . . H48 H 0.6508 0.2840 0.6288 0.024 Uiso 1 1 calc R . . C49 C 0.5863(3) 0.5264(2) 0.8404(2) 0.0269(9) Uani 1 1 d . . . C50 C 0.4456(3) 0.2812(3) 0.6260(2) 0.0289(10) Uani 1 1 d D . . C51 C 0.9469(3) 0.3907(2) 0.7860(2) 0.0164(8) Uani 1 1 d . . . C52 C 1.0479(3) 0.4225(2) 0.7854(2) 0.0186(8) Uani 1 1 d . . . H52 H 1.0584 0.4343 0.7371 0.022 Uiso 1 1 calc R . . C53 C 1.1324(3) 0.4370(2) 0.8537(2) 0.0184(8) Uani 1 1 d . . . C54 C 1.1200(3) 0.4207(2) 0.9268(2) 0.0201(8) Uani 1 1 d . . . H54 H 1.1769 0.4309 0.9732 0.024 Uiso 1 1 calc R . . C55 C 1.0218(3) 0.3890(2) 0.9294(2) 0.0180(8) Uani 1 1 d . . . C56 C 0.9366(3) 0.3740(2) 0.8598(2) 0.0183(8) Uani 1 1 d U . . H56 H 0.8709 0.3521 0.8628 0.022 Uiso 1 1 calc R . . C57 C 1.2365(3) 0.4732(3) 0.8481(2) 0.0290(10) Uani 1 1 d . . . C58 C 1.0061(3) 0.3711(2) 1.0073(2) 0.0261(9) Uani 1 1 d . . . C59 C 0.8543(3) 0.4458(2) 0.6468(2) 0.0162(8) Uani 1 1 d U . . C60 C 0.8271(3) 0.4339(2) 0.5626(2) 0.0206(8) Uani 1 1 d . . . H60 H 0.8066 0.3800 0.5344 0.025 Uiso 1 1 calc R . . C61 C 0.8298(3) 0.4992(2) 0.5198(2) 0.0216(8) Uani 1 1 d . . . C62 C 0.8564(3) 0.5811(2) 0.5583(2) 0.0240(9) Uani 1 1 d . . . H62 H 0.8586 0.6251 0.5296 0.029 Uiso 1 1 calc R . . C63 C 0.8796(3) 0.5946(2) 0.6416(2) 0.0201(8) Uani 1 1 d . . . C64 C 0.8795(3) 0.5291(2) 0.6841(2) 0.0202(8) Uani 1 1 d . . . H64 H 0.8970 0.5409 0.7401 0.024 Uiso 1 1 calc R . . C65 C 0.8055(4) 0.4812(3) 0.4299(2) 0.0369(11) Uani 1 1 d . . . C66 C 0.9134(3) 0.6810(2) 0.6870(3) 0.0309(10) Uani 1 1 d . . . C67 C 0.6005(3) 0.6503(2) 0.6381(3) 0.0392(11) Uani 1 1 d . . . H67A H 0.6516 0.6703 0.6127 0.059 Uiso 1 1 calc R . . H67B H 0.6325 0.6552 0.6951 0.059 Uiso 1 1 calc R . . H67C H 0.5375 0.6835 0.6286 0.059 Uiso 1 1 calc R . . C68 C 0.5696(4) 0.5616(3) 0.6043(3) 0.0582(14) Uani 1 1 d . . . H68A H 0.5212 0.5417 0.6329 0.070 Uiso 1 1 calc R . . H68B H 0.6340 0.5291 0.6151 0.070 Uiso 1 1 calc R . . C69 C 0.5155(4) 0.5434(3) 0.5152(3) 0.0480(12) Uani 1 1 d . . . H69A H 0.4517 0.5764 0.5040 0.058 Uiso 1 1 calc R . . H69B H 0.5643 0.5617 0.4863 0.058 Uiso 1 1 calc R . . F1 F 0.7463(3) 0.05920(19) 0.7006(2) 0.0489(10) Uani 0.837(4) 1 d PDU A 1 F2 F 0.8947(2) 0.00123(19) 0.6994(2) 0.0472(10) Uani 0.837(4) 1 d PDU A 1 F3 F 0.7716(3) -0.0063(2) 0.59084(18) 0.0416(10) Uani 0.837(4) 1 d PDU A 1 F4 F 1.0572(3) 0.11212(18) 0.4844(2) 0.0409(9) Uani 0.837(4) 1 d PDU A 1 F5 F 1.0039(3) 0.2331(2) 0.45956(17) 0.0339(9) Uani 0.837(4) 1 d PDU A 1 F6 F 1.14125(17) 0.22756(15) 0.55701(13) 0.0406(6) Uani 1 1 d DU A . F7 F 0.48500(19) 0.53828(17) 0.83976(17) 0.0658(9) Uani 1 1 d . . . F8 F 0.6370(2) 0.51953(16) 0.91580(14) 0.0629(8) Uani 1 1 d . . . F9 F 0.6233(2) 0.59970(15) 0.83024(17) 0.0709(9) Uani 1 1 d . . . F10 F 0.3521(2) 0.3177(2) 0.6113(3) 0.0637(12) Uani 0.837(4) 1 d PDU A 1 F11 F 0.4337(3) 0.2142(2) 0.6574(2) 0.0653(13) Uani 0.837(4) 1 d PDU A 1 F12 F 0.4579(2) 0.2528(2) 0.55283(17) 0.0511(10) Uani 0.837(4) 1 d PDU A 1 F13 F 1.27338(19) 0.42909(19) 0.79040(16) 0.0687(9) Uani 1 1 d . . . F14 F 1.2285(2) 0.55039(17) 0.83008(19) 0.0697(9) Uani 1 1 d . . . F15 F 1.31616(18) 0.47732(17) 0.91462(14) 0.0503(7) Uani 1 1 d . . . F16 F 1.0228(2) 0.28965(14) 1.01615(14) 0.0442(6) Uani 1 1 d . . . F17 F 0.90641(17) 0.38377(14) 1.01465(13) 0.0361(6) Uani 1 1 d . . . F18 F 1.07233(19) 0.41639(15) 1.07179(12) 0.0436(6) Uani 1 1 d . . . F19 F 0.8483(2) 0.41235(19) 0.40297(14) 0.0652(9) Uani 1 1 d . . . F20 F 0.7028(2) 0.4714(2) 0.39399(15) 0.0948(13) Uani 1 1 d . . . F21 F 0.8430(3) 0.5402(2) 0.39821(16) 0.1057(14) Uani 1 1 d . . . F22 F 0.87224(18) 0.74240(13) 0.64634(13) 0.0358(6) Uani 1 1 d . . . F23 F 1.02146(19) 0.69416(14) 0.70554(17) 0.0552(8) Uani 1 1 d . . . F24 F 0.8866(2) 0.69539(13) 0.75714(13) 0.0471(7) Uani 1 1 d . . . F1A F 0.8163(14) -0.0219(10) 0.6087(9) 0.037(5) Uani 0.163(4) 1 d PDU A 2 F2A F 0.7089(9) 0.0592(9) 0.6533(10) 0.034(4) Uani 0.163(4) 1 d PDU A 2 F3A F 0.8565(13) 0.0320(10) 0.7315(7) 0.048(4) Uani 0.163(4) 1 d PDU A 2 F4A F 1.1046(12) 0.1122(8) 0.5295(10) 0.033(4) Uani 0.163(4) 1 d PDU A 2 F5A F 1.0123(18) 0.1951(13) 0.4490(9) 0.049(5) Uani 0.163(4) 1 d PDU A 2 F10A F 0.4736(13) 0.2020(8) 0.6143(12) 0.057(5) Uani 0.163(4) 1 d PDU A 2 F11A F 0.4001(15) 0.3003(11) 0.5579(9) 0.062(5) Uani 0.163(4) 1 d PDU A 2 F12A F 0.3673(12) 0.2766(11) 0.6632(9) 0.048(4) Uani 0.163(4) 1 d PDU A 2 N1 N 0.3468(2) 0.84920(17) 0.93963(16) 0.0151(6) Uani 1 1 d U . . N2 N 0.2140(2) 0.96657(17) 0.82906(16) 0.0172(7) Uani 1 1 d . . . N3 N 0.3952(2) 0.86172(17) 0.77471(16) 0.0168(7) Uani 1 1 d . . . Tl1 Tl 0.423043(12) 0.988936(10) 0.894612(9) 0.02002(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.015(2) 0.018(2) 0.017(2) -0.0029(18) 0.0051(19) -0.0022(18) C1 0.0189(19) 0.0185(18) 0.0143(16) 0.0018(14) -0.0001(15) -0.0065(14) C2 0.021(2) 0.0158(18) 0.0171(17) 0.0030(15) 0.0067(16) -0.0026(15) C3 0.028(2) 0.040(2) 0.026(2) 0.0072(18) 0.0057(17) -0.0129(18) C4 0.0179(15) 0.0159(15) 0.0152(14) 0.0046(12) 0.0057(13) -0.0033(13) C5 0.021(2) 0.020(2) 0.0173(19) 0.0040(16) 0.0034(17) -0.0060(16) C6 0.031(2) 0.027(2) 0.0170(19) 0.0052(17) 0.0021(19) 0.0064(18) C7 0.039(3) 0.030(2) 0.0154(19) 0.0010(18) 0.0094(19) -0.005(2) C8 0.030(2) 0.019(2) 0.026(2) -0.0005(17) 0.015(2) 0.0013(17) C9 0.016(2) 0.0194(19) 0.0212(19) 0.0057(16) 0.0049(17) 0.0009(15) C10 0.028(2) 0.025(2) 0.0157(19) 0.0035(16) 0.0015(18) 0.0057(17) C11 0.079(4) 0.024(3) 0.093(4) -0.016(3) 0.044(3) -0.008(3) C12 0.037(3) 0.055(3) 0.085(4) -0.024(3) 0.015(3) 0.005(2) C13 0.0127(18) 0.0254(19) 0.0189(17) 0.0043(15) 0.0004(15) -0.0022(14) C14 0.030(2) 0.029(2) 0.0256(19) 0.0042(17) -0.0097(17) -0.0018(18) C15 0.0186(19) 0.0239(18) 0.0254(18) 0.0007(15) -0.0064(15) 0.0023(15) C16 0.021(2) 0.0301(19) 0.038(2) -0.0100(16) -0.0051(16) 0.0067(16) C17 0.033(2) 0.033(2) 0.057(2) -0.0101(19) -0.0122(19) 0.0119(19) C18 0.048(3) 0.027(2) 0.054(3) 0.0035(19) -0.025(2) 0.0078(19) C19 0.047(2) 0.032(2) 0.040(2) 0.0120(18) -0.0146(19) -0.0030(19) C20 0.028(2) 0.0274(19) 0.0290(19) 0.0062(16) -0.0045(16) 0.0016(16) C21 0.030(2) 0.051(2) 0.046(2) -0.0137(19) 0.010(2) 0.007(2) C22 0.031(3) 0.138(6) 0.062(4) -0.036(4) 0.006(3) 0.011(3) C23 0.040(3) 0.051(3) 0.054(3) -0.003(2) 0.004(3) 0.013(2) C24 0.0199(15) 0.0184(14) 0.0110(13) 0.0026(12) -0.0006(12) -0.0015(12) C25 0.035(2) 0.021(2) 0.032(2) -0.0010(18) 0.012(2) -0.0007(17) C26 0.0191(19) 0.0147(18) 0.0210(18) -0.0028(15) 0.0058(15) -0.0016(15) C27 0.033(2) 0.0214(19) 0.0207(18) -0.0018(15) 0.0115(17) 0.0005(17) C28 0.042(2) 0.029(2) 0.036(2) -0.0026(17) 0.0225(17) -0.0037(18) C29 0.029(2) 0.028(2) 0.053(2) -0.0050(18) 0.0212(18) 0.0009(17) C30 0.0266(19) 0.028(2) 0.042(2) -0.0039(18) 0.0059(18) 0.0036(17) C31 0.029(2) 0.024(2) 0.0244(19) 0.0013(16) 0.0075(17) 0.0038(17) C32 0.042(2) 0.035(2) 0.0242(19) 0.0106(17) 0.0142(17) 0.0051(19) C33 0.046(3) 0.058(3) 0.030(2) 0.009(2) 0.004(2) -0.002(2) C34 0.077(4) 0.064(4) 0.048(3) 0.032(3) 0.008(3) -0.012(3) C35 0.0135(19) 0.0216(19) 0.0138(17) 0.0022(15) -0.0005(15) -0.0005(15) C36 0.014(2) 0.023(2) 0.0152(18) 0.0027(16) 0.0051(16) -0.0018(16) C37 0.017(2) 0.019(2) 0.0150(18) 0.0024(16) 0.0002(16) -0.0031(16) C38 0.020(2) 0.017(2) 0.0191(19) -0.0030(16) 0.0034(17) 0.0010(16) C39 0.017(2) 0.022(2) 0.0183(19) -0.0001(16) 0.0042(17) -0.0032(16) C40 0.0157(19) 0.0172(19) 0.0175(18) 0.0029(15) 0.0028(16) -0.0051(15) C41 0.028(2) 0.026(2) 0.023(2) 0.0049(18) 0.005(2) -0.0050(19) C42 0.029(3) 0.024(2) 0.033(2) -0.005(2) 0.013(2) -0.0014(19) C43 0.017(2) 0.022(2) 0.0178(19) 0.0027(16) 0.0015(17) 0.0012(16) C44 0.020(2) 0.0175(19) 0.0168(18) 0.0015(16) 0.0022(17) -0.0008(16) C45 0.019(2) 0.023(2) 0.0189(19) 0.0063(16) 0.0073(17) 0.0047(16) C46 0.013(2) 0.027(2) 0.024(2) 0.0077(17) 0.0056(17) 0.0019(16) C47 0.013(2) 0.025(2) 0.023(2) 0.0066(17) 0.0010(17) -0.0029(16) C48 0.022(2) 0.019(2) 0.0168(18) -0.0001(16) 0.0024(17) -0.0020(16) C49 0.025(2) 0.029(2) 0.030(2) 0.0060(19) 0.011(2) 0.0012(18) C50 0.021(2) 0.035(2) 0.030(2) 0.005(2) 0.005(2) -0.0023(19) C51 0.014(2) 0.0123(18) 0.0217(19) -0.0016(15) 0.0059(17) 0.0004(15) C52 0.021(2) 0.0190(19) 0.0158(18) 0.0007(15) 0.0062(17) 0.0015(16) C53 0.011(2) 0.019(2) 0.023(2) 0.0015(16) 0.0018(17) 0.0011(15) C54 0.018(2) 0.020(2) 0.0180(19) 0.0007(16) -0.0013(17) 0.0009(16) C55 0.021(2) 0.0150(19) 0.0180(19) 0.0014(15) 0.0067(17) 0.0031(16) C56 0.0159(19) 0.0143(18) 0.0247(19) 0.0023(15) 0.0055(16) -0.0024(15) C57 0.020(2) 0.043(3) 0.021(2) 0.005(2) -0.0008(19) -0.0036(19) C58 0.029(2) 0.024(2) 0.024(2) 0.0062(18) 0.004(2) -0.0028(18) C59 0.0115(15) 0.0169(15) 0.0196(15) 0.0009(12) 0.0037(13) 0.0003(12) C60 0.018(2) 0.0169(19) 0.022(2) -0.0021(16) -0.0004(17) -0.0025(16) C61 0.019(2) 0.026(2) 0.0174(19) 0.0042(17) 0.0003(17) 0.0014(17) C62 0.019(2) 0.022(2) 0.029(2) 0.0120(17) -0.0013(18) -0.0007(17) C63 0.012(2) 0.019(2) 0.027(2) 0.0004(17) 0.0035(17) -0.0026(15) C64 0.0114(19) 0.026(2) 0.0213(19) 0.0022(17) 0.0021(16) -0.0015(16) C65 0.049(3) 0.031(3) 0.025(2) 0.004(2) -0.001(2) -0.002(2) C66 0.030(3) 0.025(2) 0.037(2) 0.004(2) 0.009(2) -0.0016(19) C67 0.039(3) 0.030(2) 0.047(3) -0.009(2) 0.019(2) 0.003(2) C68 0.045(3) 0.069(4) 0.058(3) 0.016(3) 0.005(3) -0.005(3) C69 0.057(3) 0.050(3) 0.044(3) 0.002(2) 0.028(3) -0.008(3) F1 0.069(2) 0.0300(16) 0.069(2) 0.0090(17) 0.055(2) -0.0014(16) F2 0.0443(19) 0.0338(18) 0.067(2) 0.0292(17) 0.0079(17) 0.0038(15) F3 0.054(2) 0.0328(18) 0.0338(17) 0.0039(15) 0.0053(17) -0.0233(17) F4 0.053(2) 0.0338(17) 0.045(2) -0.0062(15) 0.0345(18) -0.0008(15) F5 0.0460(19) 0.040(2) 0.0171(14) 0.0005(14) 0.0138(14) 0.0008(17) F6 0.0227(13) 0.0644(16) 0.0343(13) 0.0020(12) 0.0103(11) -0.0115(12) F7 0.0295(16) 0.077(2) 0.077(2) -0.0399(16) 0.0196(15) 0.0066(14) F8 0.092(2) 0.0615(18) 0.0237(14) -0.0091(13) 0.0030(15) 0.0321(16) F9 0.119(3) 0.0283(15) 0.087(2) -0.0063(14) 0.076(2) -0.0043(15) F10 0.0206(17) 0.056(2) 0.091(3) -0.022(2) -0.0091(18) 0.0028(15) F11 0.080(3) 0.056(2) 0.046(2) 0.0267(17) -0.0190(19) -0.0461(19) F12 0.0351(19) 0.076(2) 0.0325(17) -0.0163(16) 0.0054(14) -0.0256(17) F13 0.0318(15) 0.113(2) 0.0563(18) -0.0313(17) 0.0277(14) -0.0264(15) F14 0.0326(16) 0.0619(19) 0.125(3) 0.0583(19) 0.0150(17) -0.0080(14) F15 0.0190(14) 0.092(2) 0.0342(14) 0.0185(14) -0.0084(12) -0.0210(13) F16 0.0708(18) 0.0287(13) 0.0486(15) 0.0224(12) 0.0336(14) 0.0164(12) F17 0.0379(15) 0.0466(15) 0.0328(13) 0.0117(11) 0.0221(12) 0.0086(12) F18 0.0537(17) 0.0560(16) 0.0188(12) 0.0042(11) 0.0062(12) -0.0163(13) F19 0.084(2) 0.084(2) 0.0262(14) 0.0030(14) 0.0148(15) 0.0362(18) F20 0.0422(19) 0.192(4) 0.0282(15) -0.017(2) -0.0103(15) 0.030(2) F21 0.204(4) 0.080(2) 0.0276(15) 0.0067(15) 0.022(2) -0.059(3) F22 0.0482(16) 0.0184(12) 0.0453(14) 0.0051(11) 0.0204(13) 0.0019(11) F23 0.0277(15) 0.0293(14) 0.093(2) -0.0087(14) -0.0020(14) -0.0111(11) F24 0.085(2) 0.0230(13) 0.0326(14) -0.0043(11) 0.0187(14) -0.0073(13) F1A 0.040(6) 0.031(6) 0.043(6) 0.000(4) 0.018(5) 0.001(4) F2A 0.035(6) 0.028(6) 0.044(6) 0.013(5) 0.014(4) -0.002(4) F3A 0.054(6) 0.046(6) 0.043(6) 0.016(4) 0.007(4) -0.005(4) F4A 0.036(6) 0.035(6) 0.035(6) -0.002(4) 0.026(4) -0.003(4) F5A 0.049(6) 0.053(7) 0.040(6) -0.008(5) 0.013(4) 0.001(5) F10A 0.051(6) 0.047(6) 0.067(6) 0.000(5) 0.010(5) 0.001(4) F11A 0.062(6) 0.062(6) 0.057(6) 0.014(5) 0.004(5) -0.012(5) F12A 0.039(6) 0.056(6) 0.048(6) -0.003(4) 0.015(4) -0.011(4) N1 0.0168(13) 0.0179(13) 0.0123(12) 0.0057(11) 0.0046(11) 0.0003(11) N2 0.0127(16) 0.0217(17) 0.0170(15) 0.0033(13) 0.0032(13) 0.0040(13) N3 0.0201(17) 0.0168(16) 0.0120(15) 0.0015(12) 0.0018(13) -0.0020(13) Tl1 0.01854(8) 0.02177(8) 0.01674(7) 0.00087(5) 0.00049(6) -0.00311(5) _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 B1 C35 1.635(5) . ? B1 C59 1.639(5) . ? B1 C43 1.644(5) . ? B1 C51 1.646(5) . ? C1 C13 1.521(5) . ? C1 C24 1.521(5) . ? C1 C2 1.526(4) . ? C1 H1 0.9800 . ? C2 N1 1.263(4) . ? C2 C3 1.493(5) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C9 1.385(5) . ? C4 C5 1.393(5) . ? C4 N1 1.432(4) . ? C5 C6 1.397(5) . ? C5 C10 1.510(5) . ? C6 C7 1.390(5) . ? C6 H6 0.9300 . ? C7 C8 1.377(5) . ? C7 H7 0.9300 . ? C8 C9 1.386(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C12 1.497(5) . ? C10 C11 1.508(5) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N2 1.274(4) . ? C13 C14 1.486(5) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.379(5) . ? C15 C16 1.398(5) . ? C15 N2 1.432(4) . ? C16 C17 1.393(6) . ? C16 C21 1.504(6) . ? C17 C18 1.347(6) . ? C17 H17 0.9300 . ? C18 C19 1.386(6) . ? C18 H18 0.9300 . ? C19 C20 1.386(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.530(6) . ? C21 C23 1.531(6) . ? C21 H21 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N3 1.264(4) . ? C24 C25 1.494(5) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C31 1.389(5) . ? C26 C27 1.398(5) . ? C26 N3 1.431(4) . ? C27 C28 1.390(5) . ? C27 C32 1.511(5) . ? C28 C29 1.369(5) . ? C28 H28 0.9300 . ? C29 C30 1.375(5) . ? C29 H29 0.9300 . ? C30 C31 1.382(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.519(5) . ? C32 C34 1.535(5) . ? C32 H32 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C40 1.398(4) . ? C35 C36 1.398(5) . ? C36 C37 1.381(5) . ? C36 H36 0.9300 . ? C37 C38 1.382(5) . ? C37 C41 1.481(5) . ? C38 C39 1.382(5) . ? C38 H38 0.9300 . ? C39 C40 1.392(5) . ? C39 C42 1.484(5) . ? C40 H40 0.9300 . ? C41 F1A 1.296(11) . ? C41 F3A 1.299(10) . ? C41 F1 1.311(4) . ? C41 F3 1.341(4) . ? C41 F2 1.350(4) . ? C41 F2A 1.390(11) . ? C42 F5A 1.251(14) . ? C42 F4 1.314(4) . ? C42 F6 1.327(4) . ? C42 F5 1.390(5) . ? C42 F4A 1.432(12) . ? C43 C44 1.392(4) . ? C43 C48 1.400(4) . ? C44 C45 1.390(5) . ? C44 H44 0.9300 . ? C45 C46 1.380(5) . ? C45 C49 1.477(5) . ? C46 C47 1.371(5) . ? C46 H46 0.9300 . ? C47 C48 1.395(5) . ? C47 C50 1.498(5) . ? C48 H48 0.9300 . ? C49 F7 1.312(4) . ? C49 F9 1.323(4) . ? C49 F8 1.325(4) . ? C50 F11A 1.261(11) . ? C50 F11 1.305(4) . ? C50 F10 1.319(4) . ? C50 F10A 1.323(11) . ? C50 F12 1.333(4) . ? C50 F12A 1.337(11) . ? C51 C56 1.389(5) . ? C51 C52 1.396(5) . ? C52 C53 1.375(4) . ? C52 H52 0.9300 . ? C53 C54 1.384(5) . ? C53 C57 1.489(5) . ? C54 C55 1.373(5) . ? C54 H54 0.9300 . ? C55 C56 1.395(5) . ? C55 C58 1.488(5) . ? C56 H56 0.9300 . ? C57 F14 1.322(4) . ? C57 F15 1.323(4) . ? C57 F13 1.328(4) . ? C58 F18 1.330(4) . ? C58 F17 1.331(4) . ? C58 F16 1.352(4) . ? C59 C64 1.395(4) . ? C59 C60 1.398(5) . ? C60 C61 1.382(5) . ? C60 H60 0.9300 . ? C61 C62 1.382(5) . ? C61 C65 1.494(5) . ? C62 C63 1.384(5) . ? C62 H62 0.9300 . ? C63 C64 1.374(5) . ? C63 C66 1.494(5) . ? C64 H64 0.9300 . ? C65 F20 1.302(5) . ? C65 F19 1.312(5) . ? C65 F21 1.314(5) . ? C66 F22 1.331(4) . ? C66 F24 1.338(4) . ? C66 F23 1.348(4) . ? C67 C68 1.470(6) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 C69 1.508(6) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C69 1.431(8) 2_666 ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? N1 Tl1 2.745(3) . ? N2 Tl1 2.629(3) . ? N3 Tl1 2.642(3) . ? Tl1 Tl1 3.6487(3) 2_677 ? 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 C35 B1 C59 113.0(3) . . ? C35 B1 C43 113.5(3) . . ? C59 B1 C43 104.0(3) . . ? C35 B1 C51 104.6(3) . . ? C59 B1 C51 109.6(3) . . ? C43 B1 C51 112.4(3) . . ? C13 C1 C24 110.8(3) . . ? C13 C1 C2 112.6(3) . . ? C24 C1 C2 110.3(3) . . ? C13 C1 H1 107.6 . . ? C24 C1 H1 107.6 . . ? C2 C1 H1 107.6 . . ? N1 C2 C3 127.2(3) . . ? N1 C2 C1 117.7(3) . . ? C3 C2 C1 115.1(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C9 C4 C5 121.2(3) . . ? C9 C4 N1 118.5(3) . . ? C5 C4 N1 119.9(3) . . ? C4 C5 C6 117.1(3) . . ? C4 C5 C10 121.7(3) . . ? C6 C5 C10 121.1(3) . . ? C7 C6 C5 121.6(4) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 C7 C6 120.4(3) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 118.7(3) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C4 C9 C8 121.0(3) . . ? C4 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C12 C10 C11 110.4(4) . . ? C12 C10 C5 113.5(3) . . ? C11 C10 C5 110.6(3) . . ? C12 C10 H10 107.4 . . ? C11 C10 H10 107.4 . . ? C5 C10 H10 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 126.7(3) . . ? N2 C13 C1 118.0(3) . . ? C14 C13 C1 115.2(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 122.0(4) . . ? C20 C15 N2 118.6(3) . . ? C16 C15 N2 119.0(4) . . ? C17 C16 C15 115.5(4) . . ? C17 C16 C21 122.8(4) . . ? C15 C16 C21 121.6(4) . . ? C18 C17 C16 123.2(4) . . ? C18 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? C17 C18 C19 120.9(4) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 C18 118.1(5) . . ? C20 C19 H19 121.0 . . ? C18 C19 H19 121.0 . . ? C15 C20 C19 120.4(4) . . ? C15 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C16 C21 C22 113.3(4) . . ? C16 C21 C23 109.3(4) . . ? C22 C21 C23 109.4(4) . . ? C16 C21 H21 108.2 . . ? C22 C21 H21 108.2 . . ? C23 C21 H21 108.2 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N3 C24 C25 126.5(3) . . ? N3 C24 C1 117.8(3) . . ? C25 C24 C1 115.6(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C31 C26 C27 121.4(3) . . ? C31 C26 N3 119.4(3) . . ? C27 C26 N3 118.9(3) . . ? C28 C27 C26 116.9(4) . . ? C28 C27 C32 123.1(4) . . ? C26 C27 C32 120.0(3) . . ? C29 C28 C27 121.9(4) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C28 C29 C30 120.5(4) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C31 119.4(4) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C30 C31 C26 119.8(4) . . ? C30 C31 H31 120.1 . . ? C26 C31 H31 120.1 . . ? C27 C32 C33 110.4(3) . . ? C27 C32 C34 113.7(3) . . ? C33 C32 C34 110.0(3) . . ? C27 C32 H32 107.5 . . ? C33 C32 H32 107.5 . . ? C34 C32 H32 107.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 115.1(3) . . ? C40 C35 B1 121.4(3) . . ? C36 C35 B1 123.2(3) . . ? C37 C36 C35 123.0(3) . . ? C37 C36 H36 118.5 . . ? C35 C36 H36 118.5 . . ? C36 C37 C38 120.4(3) . . ? C36 C37 C41 121.1(3) . . ? C38 C37 C41 118.5(3) . . ? C39 C38 C37 118.5(3) . . ? C39 C38 H38 120.7 . . ? C37 C38 H38 120.7 . . ? C38 C39 C40 120.4(3) . . ? C38 C39 C42 121.3(3) . . ? C40 C39 C42 118.3(3) . . ? C39 C40 C35 122.6(3) . . ? C39 C40 H40 118.7 . . ? C35 C40 H40 118.7 . . ? F1A C41 F3A 108.8(10) . . ? F1A C41 F1 121.6(9) . . ? F3A C41 F1 68.5(8) . . ? F1A C41 F3 28.3(7) . . ? F3A C41 F3 129.7(8) . . ? F1 C41 F3 107.4(3) . . ? F1A C41 F2 75.8(8) . . ? F3A C41 F2 40.8(8) . . ? F1 C41 F2 106.0(3) . . ? F3 C41 F2 103.4(3) . . ? F1A C41 F2A 103.4(9) . . ? F3A C41 F2A 103.7(9) . . ? F1 C41 F2A 36.0(6) . . ? F3 C41 F2A 79.3(7) . . ? F2 C41 F2A 135.5(7) . . ? F1A C41 C37 117.9(9) . . ? F3A C41 C37 114.8(8) . . ? F1 C41 C37 114.5(3) . . ? F3 C41 C37 112.0(3) . . ? F2 C41 C37 112.8(3) . . ? F2A C41 C37 106.6(7) . . ? F5A C42 F4 77.1(9) . . ? F5A C42 F6 113.1(11) . . ? F4 C42 F6 111.8(3) . . ? F5A C42 F5 26.8(9) . . ? F4 C42 F5 103.9(3) . . ? F6 C42 F5 102.4(3) . . ? F5A C42 F4A 110.1(11) . . ? F4 C42 F4A 36.1(6) . . ? F6 C42 F4A 85.3(7) . . ? F5 C42 F4A 135.7(7) . . ? F5A C42 C39 121.6(11) . . ? F4 C42 C39 114.7(3) . . ? F6 C42 C39 113.5(3) . . ? F5 C42 C39 109.4(3) . . ? F4A C42 C39 106.9(7) . . ? C44 C43 C48 115.7(3) . . ? C44 C43 B1 120.5(3) . . ? C48 C43 B1 123.2(3) . . ? C45 C44 C43 122.9(3) . . ? C45 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? C46 C45 C44 120.0(3) . . ? C46 C45 C49 121.1(3) . . ? C44 C45 C49 118.9(3) . . ? C47 C46 C45 118.8(3) . . ? C47 C46 H46 120.6 . . ? C45 C46 H46 120.6 . . ? C46 C47 C48 121.1(3) . . ? C46 C47 C50 120.1(3) . . ? C48 C47 C50 118.8(3) . . ? C47 C48 C43 121.5(3) . . ? C47 C48 H48 119.2 . . ? C43 C48 H48 119.2 . . ? F7 C49 F9 104.7(3) . . ? F7 C49 F8 105.9(3) . . ? F9 C49 F8 103.9(3) . . ? F7 C49 C45 114.5(3) . . ? F9 C49 C45 113.4(3) . . ? F8 C49 C45 113.4(3) . . ? F11A C50 F11 130.6(8) . . ? F11A C50 F10 57.4(9) . . ? F11 C50 F10 107.5(4) . . ? F11A C50 F10A 107.4(10) . . ? F11 C50 F10A 45.1(8) . . ? F10 C50 F10A 133.3(8) . . ? F11A C50 F12 48.8(9) . . ? F11 C50 F12 105.7(4) . . ? F10 C50 F12 103.9(3) . . ? F10A C50 F12 64.4(8) . . ? F11A C50 F12A 105.7(10) . . ? F11 C50 F12A 60.2(8) . . ? F10 C50 F12A 52.5(8) . . ? F10A C50 F12A 102.7(9) . . ? F12 C50 F12A 135.7(7) . . ? F11A C50 C47 115.9(9) . . ? F11 C50 C47 113.2(3) . . ? F10 C50 C47 112.6(3) . . ? F10A C50 C47 113.3(8) . . ? F12 C50 C47 113.2(3) . . ? F12A C50 C47 110.8(7) . . ? C56 C51 C52 116.1(3) . . ? C56 C51 B1 124.0(3) . . ? C52 C51 B1 119.8(3) . . ? C53 C52 C51 122.2(3) . . ? C53 C52 H52 118.9 . . ? C51 C52 H52 118.9 . . ? C52 C53 C54 120.7(3) . . ? C52 C53 C57 118.7(3) . . ? C54 C53 C57 120.6(3) . . ? C55 C54 C53 118.5(3) . . ? C55 C54 H54 120.7 . . ? C53 C54 H54 120.7 . . ? C54 C55 C56 120.5(3) . . ? C54 C55 C58 119.7(3) . . ? C56 C55 C58 119.9(3) . . ? C51 C56 C55 122.0(3) . . ? C51 C56 H56 119.0 . . ? C55 C56 H56 119.0 . . ? F14 C57 F15 106.1(3) . . ? F14 C57 F13 104.8(3) . . ? F15 C57 F13 105.3(3) . . ? F14 C57 C53 112.8(3) . . ? F15 C57 C53 114.5(3) . . ? F13 C57 C53 112.4(3) . . ? F18 C58 F17 106.4(3) . . ? F18 C58 F16 105.8(3) . . ? F17 C58 F16 104.7(3) . . ? F18 C58 C55 113.8(3) . . ? F17 C58 C55 113.5(3) . . ? F16 C58 C55 111.9(3) . . ? C64 C59 C60 115.0(3) . . ? C64 C59 B1 119.9(3) . . ? C60 C59 B1 125.0(3) . . ? C61 C60 C59 122.4(3) . . ? C61 C60 H60 118.8 . . ? C59 C60 H60 118.8 . . ? C60 C61 C62 121.4(3) . . ? C60 C61 C65 119.5(3) . . ? C62 C61 C65 119.0(3) . . ? C61 C62 C63 117.0(3) . . ? C61 C62 H62 121.5 . . ? C63 C62 H62 121.5 . . ? C64 C63 C62 121.5(3) . . ? C64 C63 C66 118.8(3) . . ? C62 C63 C66 119.6(3) . . ? C63 C64 C59 122.7(3) . . ? C63 C64 H64 118.6 . . ? C59 C64 H64 118.6 . . ? F20 C65 F19 105.1(3) . . ? F20 C65 F21 106.1(4) . . ? F19 C65 F21 103.9(4) . . ? F20 C65 C61 113.7(4) . . ? F19 C65 C61 113.5(4) . . ? F21 C65 C61 113.6(3) . . ? F22 C66 F24 106.5(3) . . ? F22 C66 F23 105.5(3) . . ? F24 C66 F23 105.9(3) . . ? F22 C66 C63 113.7(3) . . ? F24 C66 C63 113.1(3) . . ? F23 C66 C63 111.4(3) . . ? C68 C67 H67A 109.5 . . ? C68 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C68 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C67 C68 C69 116.2(4) . . ? C67 C68 H68A 108.2 . . ? C69 C68 H68A 108.2 . . ? C67 C68 H68B 108.2 . . ? C69 C68 H68B 108.2 . . ? H68A C68 H68B 107.4 . . ? C69 C69 C68 114.7(5) 2_666 . ? C69 C69 H69A 108.6 2_666 . ? C68 C69 H69A 108.6 . . ? C69 C69 H69B 108.6 2_666 . ? C68 C69 H69B 108.6 . . ? H69A C69 H69B 107.6 . . ? C2 N1 C4 121.6(3) . . ? C2 N1 Tl1 115.7(2) . . ? C4 N1 Tl1 110.10(19) . . ? C13 N2 C15 121.5(3) . . ? C13 N2 Tl1 114.4(2) . . ? C15 N2 Tl1 103.2(2) . . ? C24 N3 C26 122.9(3) . . ? C24 N3 Tl1 117.0(2) . . ? C26 N3 Tl1 105.99(19) . . ? N2 Tl1 N3 72.85(8) . . ? N2 Tl1 N1 70.19(8) . . ? N3 Tl1 N1 70.79(8) . . ? N2 Tl1 Tl1 130.36(6) . 2_677 ? N3 Tl1 Tl1 131.77(6) . 2_677 ? N1 Tl1 Tl1 79.25(6) . 2_677 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.860 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.100 _database_code_depnum_ccdc_archive 'CCDC 899511' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ofm61p-1Compound_2 #TrackingRef 'Tl_Tki_Angew_Final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 442(2) _chemical_formula_moiety 'C32 H12 B F24, C37 H49 N3 Tl' _chemical_formula_sum 'C69 H61 B F24 N3 Tl' _chemical_formula_weight 1603.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.8168(4) _cell_length_b 16.3174(7) _cell_length_c 16.4832(6) _cell_angle_alpha 73.129(4) _cell_angle_beta 79.390(3) _cell_angle_gamma 63.442(3) _cell_volume 3404.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 38437 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 30.51 _exptl_crystal_description rhomb _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 2.481 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.784 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrysAlis RED,Empirical,spherical harmonics' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, Sapphire2' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38437 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0855 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 30.51 _reflns_number_total 20729 _reflns_number_gt 15407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20729 _refine_ls_number_parameters 922 _refine_ls_number_restraints 162 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.904 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.8422(2) 0.3371(2) 0.91162(18) 0.0140(6) Uani 1 1 d . . . C1 C 0.63426(17) 0.00004(17) 0.74582(15) 0.0124(5) Uani 1 1 d . . . H1 H 0.6669 -0.0241 0.7996 0.015 Uiso 1 1 calc R . . C2 C 0.54796(17) 0.09848(17) 0.74820(15) 0.0129(5) Uani 1 1 d . . . C3 C 0.54759(18) 0.13940(19) 0.82100(16) 0.0173(5) Uani 1 1 d . . . C4 C 0.6469(2) 0.1504(2) 0.81226(18) 0.0260(6) Uani 1 1 d . . . H4A H 0.7029 0.0896 0.8170 0.039 Uiso 1 1 calc R . . H4B H 0.6471 0.1778 0.8564 0.039 Uiso 1 1 calc R . . H4C H 0.6526 0.1906 0.7579 0.039 Uiso 1 1 calc R . . C5 C 0.5402(2) 0.0706(2) 0.90587(16) 0.0269(7) Uani 1 1 d . . . H5A H 0.4804 0.0606 0.9090 0.040 Uiso 1 1 calc R . . H5B H 0.5369 0.0967 0.9521 0.040 Uiso 1 1 calc R . . H5C H 0.5986 0.0115 0.9094 0.040 Uiso 1 1 calc R . . C6 C 0.4590(2) 0.2348(2) 0.82489(18) 0.0263(7) Uani 1 1 d . . . H6A H 0.4632 0.2816 0.7750 0.039 Uiso 1 1 calc R . . H6B H 0.4618 0.2529 0.8745 0.039 Uiso 1 1 calc R . . H6C H 0.3964 0.2297 0.8276 0.039 Uiso 1 1 calc R . . C7 C 0.41338(18) 0.22756(18) 0.66611(15) 0.0147(5) Uani 1 1 d . . . C8 C 0.31050(18) 0.24796(19) 0.68412(16) 0.0180(6) Uani 1 1 d . . . C9 C 0.2430(2) 0.3418(2) 0.65657(18) 0.0265(7) Uani 1 1 d . . . H9 H 0.1741 0.3579 0.6679 0.032 Uiso 1 1 calc R . . C10 C 0.2740(2) 0.4112(2) 0.61359(19) 0.0299(7) Uani 1 1 d . . . H10 H 0.2267 0.4733 0.5978 0.036 Uiso 1 1 calc R . . C11 C 0.3751(2) 0.3891(2) 0.59384(18) 0.0283(7) Uani 1 1 d . . . H11 H 0.3965 0.4358 0.5637 0.034 Uiso 1 1 calc R . . C12 C 0.4448(2) 0.2967(2) 0.61916(17) 0.0221(6) Uani 1 1 d . . . H12 H 0.5132 0.2809 0.6045 0.027 Uiso 1 1 calc R . . C13 C 0.27577(18) 0.1714(2) 0.73020(17) 0.0225(6) Uani 1 1 d . . . H13 H 0.3322 0.1191 0.7616 0.027 Uiso 1 1 calc R . . C14 C 0.1867(2) 0.2041(2) 0.79403(19) 0.0378(8) Uani 1 1 d . . . H14A H 0.2027 0.2307 0.8312 0.057 Uiso 1 1 calc R . . H14B H 0.1729 0.1513 0.8268 0.057 Uiso 1 1 calc R . . H14C H 0.1282 0.2509 0.7643 0.057 Uiso 1 1 calc R . . C15 C 0.2485(2) 0.1341(2) 0.6683(2) 0.0326(7) Uani 1 1 d . . . H15A H 0.1916 0.1834 0.6381 0.049 Uiso 1 1 calc R . . H15B H 0.2317 0.0825 0.6990 0.049 Uiso 1 1 calc R . . H15C H 0.3051 0.1127 0.6286 0.049 Uiso 1 1 calc R . . C16 C 0.71621(17) 0.00239(18) 0.67464(15) 0.0140(5) Uani 1 1 d . . . C17 C 0.82146(18) -0.0679(2) 0.69807(17) 0.0240(6) Uani 1 1 d . . . H17A H 0.8688 -0.0604 0.6515 0.036 Uiso 1 1 calc R . . H17B H 0.8254 -0.1306 0.7106 0.036 Uiso 1 1 calc R . . H17C H 0.8373 -0.0576 0.7471 0.036 Uiso 1 1 calc R . . C18 C 0.76634(17) 0.05663(19) 0.53224(15) 0.0161(5) Uani 1 1 d . . . C19 C 0.79044(18) 0.13407(19) 0.50119(16) 0.0179(6) Uani 1 1 d . . . C20 C 0.8560(2) 0.1326(2) 0.42870(18) 0.0299(7) Uani 1 1 d . . . H20 H 0.8745 0.1826 0.4067 0.036 Uiso 1 1 calc R . . C21 C 0.8942(2) 0.0594(3) 0.38855(19) 0.0355(8) Uani 1 1 d . . . H21 H 0.9375 0.0609 0.3400 0.043 Uiso 1 1 calc R . . C22 C 0.8688(2) -0.0154(2) 0.41990(19) 0.0317(7) Uani 1 1 d . . . H22 H 0.8949 -0.0649 0.3930 0.038 Uiso 1 1 calc R . . C23 C 0.80391(19) -0.0170(2) 0.49186(17) 0.0228(6) Uani 1 1 d . . . H23 H 0.7856 -0.0672 0.5131 0.027 Uiso 1 1 calc R . . C24 C 0.7520(2) 0.2124(2) 0.54708(17) 0.0224(6) Uani 1 1 d . . . H24 H 0.6901 0.2124 0.5807 0.027 Uiso 1 1 calc R . . C25 C 0.8280(2) 0.1931(2) 0.6093(2) 0.0382(8) Uani 1 1 d . . . H25A H 0.8422 0.1325 0.6477 0.057 Uiso 1 1 calc R . . H25B H 0.8000 0.2410 0.6409 0.057 Uiso 1 1 calc R . . H25C H 0.8893 0.1937 0.5784 0.057 Uiso 1 1 calc R . . C26 C 0.7246(3) 0.3105(2) 0.4878(2) 0.0378(8) Uani 1 1 d . . . H26A H 0.7852 0.3159 0.4597 0.057 Uiso 1 1 calc R . . H26B H 0.6903 0.3575 0.5203 0.057 Uiso 1 1 calc R . . H26C H 0.6812 0.3198 0.4462 0.057 Uiso 1 1 calc R . . C27 C 0.59295(17) -0.06912(17) 0.74196(15) 0.0130(5) Uani 1 1 d . . . C28 C 0.5526(2) -0.1126(2) 0.82449(16) 0.0205(6) Uani 1 1 d . . . H28A H 0.4920 -0.0651 0.8437 0.031 Uiso 1 1 calc R . . H28B H 0.6022 -0.1392 0.8659 0.031 Uiso 1 1 calc R . . H28C H 0.5377 -0.1613 0.8169 0.031 Uiso 1 1 calc R . . C29 C 0.55239(18) -0.14313(18) 0.66015(15) 0.0146(5) Uani 1 1 d . . . C30 C 0.61449(19) -0.22595(18) 0.63220(16) 0.0172(5) Uani 1 1 d . . . C31 C 0.5686(2) -0.27604(19) 0.61512(17) 0.0220(6) Uani 1 1 d . . . H31 H 0.6088 -0.3311 0.5968 0.026 Uiso 1 1 calc R . . C32 C 0.4644(2) -0.2468(2) 0.62448(17) 0.0264(7) Uani 1 1 d . . . H32 H 0.4355 -0.2815 0.6120 0.032 Uiso 1 1 calc R . . C33 C 0.4038(2) -0.1653(2) 0.65262(17) 0.0227(6) Uani 1 1 d . . . H33 H 0.3340 -0.1455 0.6595 0.027 Uiso 1 1 calc R . . C34 C 0.44725(18) -0.11338(19) 0.67045(15) 0.0176(5) Uani 1 1 d . . . H34 H 0.4066 -0.0588 0.6893 0.021 Uiso 1 1 calc R . . C35 C 0.72817(19) -0.2609(2) 0.62736(17) 0.0225(6) Uani 1 1 d . . . H35 H 0.7435 -0.2058 0.6149 0.027 Uiso 1 1 calc R . . C36 C 0.7690(2) -0.3229(3) 0.7134(2) 0.0452(10) Uani 1 1 d . . . H36A H 0.7368 -0.2879 0.7563 0.068 Uiso 1 1 calc R . . H36B H 0.8406 -0.3420 0.7108 0.068 Uiso 1 1 calc R . . H36C H 0.7551 -0.3776 0.7271 0.068 Uiso 1 1 calc R . . C37 C 0.7820(2) -0.3139(2) 0.5581(2) 0.0364(8) Uani 1 1 d . . . H37A H 0.7777 -0.3736 0.5736 0.055 Uiso 1 1 calc R . . H37B H 0.8517 -0.3241 0.5513 0.055 Uiso 1 1 calc R . . H37C H 0.7505 -0.2775 0.5056 0.055 Uiso 1 1 calc R . . C38 C 0.80962(17) 0.37958(17) 0.81348(15) 0.0125(5) Uani 1 1 d . . . C39 C 0.88032(17) 0.37970(18) 0.74442(15) 0.0155(5) Uani 1 1 d . . . H39 H 0.9471 0.3606 0.7552 0.019 Uiso 1 1 calc R . . C40 C 0.85585(17) 0.40676(18) 0.66088(15) 0.0154(5) Uani 1 1 d . . . C41 C 0.75723(18) 0.43838(18) 0.64076(16) 0.0164(5) Uani 1 1 d . . . H41 H 0.7400 0.4586 0.5846 0.020 Uiso 1 1 calc R . . C42 C 0.68498(17) 0.43875(18) 0.70781(16) 0.0153(5) Uani 1 1 d . . . C43 C 0.71090(17) 0.40896(17) 0.79159(15) 0.0146(5) Uani 1 1 d . . . H43 H 0.6609 0.4085 0.8348 0.017 Uiso 1 1 calc R . . C44 C 0.9384(2) 0.3992(2) 0.59228(17) 0.0282(7) Uani 1 1 d . . . C45 C 0.57879(19) 0.4688(2) 0.69019(17) 0.0235(6) Uani 1 1 d . . . C46 C 0.94777(17) 0.34037(17) 0.92177(15) 0.0140(5) Uani 1 1 d . . . C47 C 1.02297(17) 0.26946(18) 0.97475(15) 0.0144(5) Uani 1 1 d . . . H47 H 1.0175 0.2130 1.0010 0.017 Uiso 1 1 calc R . . C48 C 1.10526(18) 0.28094(18) 0.98925(15) 0.0167(5) Uani 1 1 d . . . C49 C 1.11821(19) 0.3623(2) 0.94999(17) 0.0217(6) Uani 1 1 d . . . H49 H 1.1743 0.3692 0.9591 0.026 Uiso 1 1 calc R . . C50 C 1.04582(19) 0.43311(19) 0.89684(17) 0.0218(6) Uani 1 1 d . A . C51 C 0.96224(18) 0.42257(19) 0.88372(16) 0.0186(6) Uani 1 1 d . . . H51 H 0.9140 0.4719 0.8483 0.022 Uiso 1 1 calc R . . C52 C 1.1847(2) 0.2045(2) 1.04641(18) 0.0243(6) Uani 1 1 d . . . C53 C 1.0594(2) 0.5205(2) 0.8515(2) 0.0371(8) Uani 1 1 d DU . . C54 C 0.76299(17) 0.39717(17) 0.97863(15) 0.0141(5) Uani 1 1 d . . . C55 C 0.77720(18) 0.35959(19) 1.06610(16) 0.0165(5) Uani 1 1 d . . . H55 H 0.8279 0.2995 1.0837 0.020 Uiso 1 1 calc R . . C56 C 0.71924(18) 0.40803(19) 1.12674(15) 0.0164(5) Uani 1 1 d . . . C57 C 0.64217(18) 0.49752(19) 1.10348(16) 0.0191(6) Uani 1 1 d . . . H57 H 0.6028 0.5306 1.1441 0.023 Uiso 1 1 calc R . . C58 C 0.62574(18) 0.53585(19) 1.01814(17) 0.0187(6) Uani 1 1 d . . . C59 C 0.68568(18) 0.48745(18) 0.95715(16) 0.0179(6) Uani 1 1 d . . . H59 H 0.6739 0.5162 0.9001 0.021 Uiso 1 1 calc R . . C60 C 0.7389(2) 0.3623(2) 1.21823(16) 0.0222(6) Uani 1 1 d . . . C61 C 0.5463(2) 0.6334(2) 0.99098(18) 0.0281(7) Uani 1 1 d . . . C62 C 0.84909(17) 0.22984(17) 0.93470(15) 0.0129(5) Uani 1 1 d . . . C63 C 0.92061(17) 0.16360(18) 0.89035(15) 0.0146(5) Uani 1 1 d . . . H63 H 0.9673 0.1803 0.8516 0.018 Uiso 1 1 calc R . . C64 C 0.92464(17) 0.07488(17) 0.90172(15) 0.0140(5) Uani 1 1 d . . . C65 C 0.85780(17) 0.04592(18) 0.96124(15) 0.0156(5) Uani 1 1 d . . . H65 H 0.8614 -0.0145 0.9710 0.019 Uiso 1 1 calc R . . C66 C 0.78651(17) 0.11003(18) 1.00482(15) 0.0147(5) Uani 1 1 d . . . C67 C 0.78188(17) 0.20000(18) 0.99160(15) 0.0147(5) Uani 1 1 d . . . H67 H 0.7322 0.2415 1.0218 0.018 Uiso 1 1 calc R . . C68 C 0.99407(19) 0.01098(19) 0.84688(16) 0.0195(6) Uani 1 1 d . . . C69 C 0.71068(19) 0.08490(19) 1.06696(17) 0.0207(6) Uani 1 1 d . . . F1 F 0.99156(14) 0.44562(17) 0.59722(12) 0.0550(6) Uani 1 1 d . . . F2 F 0.90653(12) 0.43247(16) 0.51497(10) 0.0503(6) Uani 1 1 d . . . F3 F 1.00599(14) 0.31032(15) 0.59739(12) 0.0575(7) Uani 1 1 d . . . F4 F 0.51321(12) 0.53206(16) 0.73442(12) 0.0503(6) Uani 1 1 d . . . F5 F 0.55014(15) 0.39985(15) 0.71214(17) 0.0747(8) Uani 1 1 d U . . F6 F 0.55727(11) 0.51324(14) 0.60980(10) 0.0392(5) Uani 1 1 d . . . F7 F 1.19920(13) 0.23401(13) 1.10870(11) 0.0409(5) Uani 1 1 d . . . F8 F 1.27578(12) 0.17081(14) 1.00537(12) 0.0526(6) Uani 1 1 d . . . F9 F 1.16494(13) 0.13014(12) 1.08484(12) 0.0419(5) Uani 1 1 d . . . F10 F 0.9690(2) 0.59753(19) 0.8370(2) 0.0548(11) Uani 0.700(5) 1 d PDU A 1 F11 F 1.0944(3) 0.5496(2) 0.9036(2) 0.0548(11) Uani 0.700(5) 1 d PDU A 1 F12 F 1.1117(4) 0.5165(3) 0.7849(3) 0.0950(19) Uani 0.700(5) 1 d PDU A 1 F13 F 0.70367(12) 0.42408(13) 1.26751(10) 0.0353(4) Uani 1 1 d . . . F14 F 0.83752(11) 0.31148(12) 1.23125(9) 0.0308(4) Uani 1 1 d . . . F15 F 0.69539(14) 0.30245(14) 1.25079(10) 0.0430(5) Uani 1 1 d . . . F16 F 0.58268(13) 0.69878(12) 0.97446(12) 0.0428(5) Uani 1 1 d . . . F17 F 0.50439(15) 0.64644(14) 0.92060(13) 0.0626(7) Uani 1 1 d U . . F18 F 0.47083(12) 0.65723(12) 1.05000(11) 0.0347(4) Uani 1 1 d . . . F19 F 1.07237(13) 0.03089(13) 0.81157(12) 0.0417(5) Uani 1 1 d . . . F20 F 1.03280(12) -0.07971(11) 0.88738(10) 0.0298(4) Uani 1 1 d . . . F21 F 0.94649(12) 0.01566(13) 0.78278(11) 0.0416(5) Uani 1 1 d . . . F22 F 0.61627(10) 0.14706(12) 1.04924(10) 0.0320(4) Uani 1 1 d . . . F23 F 0.72013(13) 0.08228(16) 1.14630(10) 0.0491(6) Uani 1 1 d . . . F24 F 0.71414(13) 0.00133(12) 1.06750(12) 0.0447(5) Uani 1 1 d . . . F10A F 1.1645(4) 0.4940(5) 0.8262(5) 0.047(2) Uani 0.300(5) 1 d PDU A 2 F11A F 1.0309(7) 0.5523(6) 0.7692(5) 0.066(3) Uani 0.300(5) 1 d PDU A 2 F12A F 1.0350(9) 0.5828(6) 0.8841(6) 0.083(3) Uani 0.300(5) 1 d PDU A 2 N1 N 0.48873(14) 0.13278(15) 0.68820(12) 0.0137(4) Uani 1 1 d . . . N2 N 0.69232(14) 0.05845(15) 0.60256(13) 0.0147(4) Uani 1 1 d . . . N3 N 0.59419(14) -0.08375(15) 0.66991(13) 0.0149(4) Uani 1 1 d . . . Tl1 Tl 0.526693(8) 0.081083(8) 0.544517(6) 0.01679(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0120(13) 0.0138(14) 0.0164(14) -0.0012(12) -0.0011(10) -0.0068(11) C1 0.0118(11) 0.0150(13) 0.0108(12) -0.0014(10) -0.0014(9) -0.0066(10) C2 0.0120(11) 0.0153(13) 0.0125(12) -0.0006(10) 0.0013(9) -0.0091(10) C3 0.0180(13) 0.0204(14) 0.0155(13) -0.0040(11) -0.0042(10) -0.0087(11) C4 0.0267(15) 0.0328(17) 0.0283(16) -0.0106(13) -0.0066(12) -0.0170(13) C5 0.0358(16) 0.0284(16) 0.0166(14) -0.0048(12) -0.0028(12) -0.0134(14) C6 0.0315(15) 0.0276(16) 0.0230(15) -0.0117(13) -0.0060(12) -0.0101(13) C7 0.0162(12) 0.0143(13) 0.0137(12) -0.0018(10) -0.0052(9) -0.0058(10) C8 0.0165(12) 0.0218(14) 0.0148(13) -0.0042(11) -0.0039(10) -0.0064(11) C9 0.0186(14) 0.0250(16) 0.0287(16) -0.0041(13) -0.0089(11) -0.0013(12) C10 0.0307(16) 0.0159(15) 0.0336(17) 0.0001(13) -0.0171(13) 0.0004(13) C11 0.0394(17) 0.0207(15) 0.0249(16) 0.0047(12) -0.0105(13) -0.0156(14) C12 0.0214(14) 0.0229(15) 0.0233(15) -0.0017(12) -0.0021(11) -0.0123(12) C13 0.0098(12) 0.0232(15) 0.0276(15) 0.0010(12) -0.0038(10) -0.0043(11) C14 0.0293(17) 0.051(2) 0.0336(18) -0.0099(16) 0.0093(13) -0.0209(16) C15 0.0321(17) 0.0315(18) 0.0407(19) -0.0107(15) 0.0009(13) -0.0189(14) C16 0.0112(11) 0.0157(13) 0.0192(13) -0.0049(11) -0.0013(9) -0.0086(10) C17 0.0140(13) 0.0311(16) 0.0225(14) -0.0016(12) -0.0038(10) -0.0076(12) C18 0.0105(11) 0.0233(14) 0.0141(13) -0.0017(11) -0.0018(9) -0.0081(11) C19 0.0149(12) 0.0236(14) 0.0163(13) -0.0017(11) -0.0010(10) -0.0109(11) C20 0.0284(16) 0.0430(19) 0.0275(16) -0.0068(14) 0.0071(12) -0.0271(15) C21 0.0290(16) 0.057(2) 0.0265(16) -0.0159(16) 0.0128(12) -0.0254(16) C22 0.0225(15) 0.044(2) 0.0345(18) -0.0229(15) 0.0075(12) -0.0141(14) C23 0.0191(13) 0.0271(16) 0.0273(15) -0.0102(13) 0.0005(11) -0.0124(12) C24 0.0214(14) 0.0260(15) 0.0248(15) -0.0051(12) -0.0002(11) -0.0153(12) C25 0.051(2) 0.0335(19) 0.0316(18) -0.0020(15) -0.0175(15) -0.0173(17) C26 0.054(2) 0.0292(18) 0.0357(19) -0.0012(15) -0.0176(15) -0.0202(16) C27 0.0086(11) 0.0118(12) 0.0159(12) 0.0006(10) -0.0028(9) -0.0034(10) C28 0.0254(14) 0.0242(15) 0.0156(13) 0.0018(11) -0.0021(10) -0.0172(12) C29 0.0180(12) 0.0169(13) 0.0113(12) 0.0032(10) -0.0037(9) -0.0123(11) C30 0.0216(13) 0.0138(13) 0.0164(13) 0.0015(10) -0.0038(10) -0.0096(11) C31 0.0283(15) 0.0146(14) 0.0236(15) -0.0013(11) -0.0042(11) -0.0104(12) C32 0.0341(16) 0.0275(16) 0.0275(16) 0.0032(13) -0.0100(12) -0.0243(14) C33 0.0186(13) 0.0268(16) 0.0265(15) 0.0006(12) -0.0026(11) -0.0165(12) C34 0.0179(13) 0.0192(14) 0.0169(13) -0.0026(11) 0.0013(10) -0.0108(11) C35 0.0194(13) 0.0181(14) 0.0301(16) -0.0058(12) -0.0025(11) -0.0076(12) C36 0.0237(16) 0.059(2) 0.0368(19) -0.0106(18) -0.0098(14) -0.0012(16) C37 0.0297(17) 0.0388(19) 0.0392(19) -0.0134(16) 0.0081(14) -0.0143(15) C38 0.0105(11) 0.0107(12) 0.0172(12) -0.0025(10) -0.0012(9) -0.0056(10) C39 0.0096(11) 0.0176(13) 0.0187(13) -0.0006(11) -0.0018(9) -0.0070(10) C40 0.0126(12) 0.0159(13) 0.0160(13) 0.0003(10) -0.0008(9) -0.0069(10) C41 0.0161(12) 0.0183(13) 0.0143(12) -0.0002(10) -0.0033(9) -0.0082(11) C42 0.0102(11) 0.0161(13) 0.0211(13) -0.0011(11) -0.0040(9) -0.0078(10) C43 0.0122(11) 0.0155(13) 0.0177(13) -0.0011(10) 0.0006(9) -0.0095(10) C44 0.0157(13) 0.0433(19) 0.0192(15) 0.0008(14) -0.0015(11) -0.0114(14) C45 0.0155(13) 0.0323(17) 0.0227(15) 0.0040(13) -0.0041(11) -0.0153(13) C46 0.0114(11) 0.0168(13) 0.0153(12) -0.0037(10) 0.0007(9) -0.0078(10) C47 0.0159(12) 0.0155(13) 0.0143(12) -0.0031(10) -0.0001(9) -0.0094(11) C48 0.0153(12) 0.0187(14) 0.0167(13) -0.0035(11) -0.0038(10) -0.0070(11) C49 0.0179(13) 0.0280(16) 0.0273(15) -0.0073(12) -0.0053(11) -0.0148(12) C50 0.0222(14) 0.0210(15) 0.0273(15) -0.0009(12) -0.0056(11) -0.0148(12) C51 0.0169(12) 0.0185(14) 0.0207(14) 0.0004(11) -0.0064(10) -0.0088(11) C52 0.0226(14) 0.0248(16) 0.0269(15) -0.0005(13) -0.0101(11) -0.0113(13) C53 0.0396(17) 0.0343(18) 0.0463(19) 0.0045(15) -0.0142(14) -0.0273(15) C54 0.0126(11) 0.0150(13) 0.0170(13) -0.0011(10) -0.0021(9) -0.0090(10) C55 0.0131(12) 0.0161(13) 0.0212(14) 0.0000(11) -0.0041(10) -0.0083(11) C56 0.0156(12) 0.0219(14) 0.0157(13) -0.0005(11) -0.0009(10) -0.0138(11) C57 0.0174(13) 0.0219(14) 0.0211(14) -0.0078(11) 0.0031(10) -0.0107(11) C58 0.0179(13) 0.0155(13) 0.0234(14) -0.0059(11) -0.0030(10) -0.0062(11) C59 0.0201(13) 0.0174(13) 0.0175(13) -0.0004(11) -0.0048(10) -0.0099(11) C60 0.0223(14) 0.0275(16) 0.0182(14) 0.0007(12) 0.0000(11) -0.0157(12) C61 0.0307(16) 0.0227(16) 0.0251(16) -0.0088(13) -0.0030(12) -0.0039(13) C62 0.0109(11) 0.0158(13) 0.0119(12) 0.0012(10) -0.0050(9) -0.0065(10) C63 0.0113(11) 0.0195(13) 0.0134(12) 0.0011(10) -0.0035(9) -0.0087(10) C64 0.0127(11) 0.0143(13) 0.0147(12) -0.0013(10) -0.0058(9) -0.0048(10) C65 0.0145(12) 0.0137(13) 0.0212(13) -0.0006(11) -0.0055(10) -0.0087(10) C66 0.0127(12) 0.0170(13) 0.0145(12) 0.0021(10) -0.0033(9) -0.0088(10) C67 0.0100(11) 0.0170(13) 0.0154(12) -0.0015(10) -0.0009(9) -0.0055(10) C68 0.0183(13) 0.0190(14) 0.0196(14) -0.0022(11) -0.0022(10) -0.0076(11) C69 0.0174(13) 0.0202(14) 0.0241(15) -0.0001(12) 0.0004(10) -0.0111(12) F1 0.0427(11) 0.0995(18) 0.0408(12) -0.0098(12) 0.0110(9) -0.0546(12) F2 0.0233(9) 0.0975(17) 0.0149(9) 0.0011(10) 0.0007(7) -0.0214(10) F3 0.0326(10) 0.0538(13) 0.0447(12) -0.0046(10) 0.0190(9) 0.0057(10) F4 0.0142(8) 0.0792(16) 0.0443(12) -0.0191(11) -0.0022(8) -0.0053(9) F5 0.0486(12) 0.0467(13) 0.134(2) 0.0343(14) -0.0561(13) -0.0389(11) F6 0.0204(8) 0.0622(13) 0.0270(9) 0.0035(9) -0.0110(7) -0.0153(9) F7 0.0502(11) 0.0342(11) 0.0429(11) -0.0059(9) -0.0330(9) -0.0124(9) F8 0.0201(9) 0.0571(14) 0.0473(12) -0.0019(10) -0.0061(8) 0.0080(9) F9 0.0488(11) 0.0272(10) 0.0537(12) 0.0148(9) -0.0354(9) -0.0223(9) F10 0.0473(18) 0.0235(15) 0.094(3) 0.0193(16) -0.0349(17) -0.0240(13) F11 0.072(2) 0.0354(19) 0.078(2) 0.0126(16) -0.0441(19) -0.0415(18) F12 0.153(5) 0.052(3) 0.077(3) -0.023(2) 0.075(3) -0.067(3) F13 0.0373(10) 0.0443(11) 0.0205(9) -0.0115(8) -0.0038(7) -0.0108(9) F14 0.0222(8) 0.0384(10) 0.0213(9) 0.0043(8) -0.0056(6) -0.0089(8) F15 0.0564(12) 0.0594(13) 0.0266(10) 0.0108(9) -0.0041(8) -0.0481(11) F16 0.0412(11) 0.0188(9) 0.0516(12) 0.0019(9) 0.0098(9) -0.0090(8) F17 0.0652(13) 0.0418(12) 0.0529(13) -0.0267(10) -0.0396(11) 0.0247(11) F18 0.0240(9) 0.0248(9) 0.0446(11) -0.0079(8) 0.0052(8) -0.0038(8) F19 0.0344(10) 0.0374(11) 0.0599(13) -0.0271(10) 0.0295(9) -0.0236(9) F20 0.0315(9) 0.0185(9) 0.0313(9) -0.0046(7) -0.0015(7) -0.0043(7) F21 0.0353(10) 0.0509(12) 0.0312(10) -0.0233(9) -0.0156(8) 0.0018(9) F22 0.0136(8) 0.0316(10) 0.0414(10) 0.0050(8) 0.0021(7) -0.0111(7) F23 0.0463(11) 0.0942(17) 0.0193(9) -0.0006(10) 0.0033(8) -0.0502(12) F24 0.0387(10) 0.0227(9) 0.0714(14) -0.0104(9) 0.0236(9) -0.0224(8) F10A 0.034(3) 0.036(4) 0.071(5) 0.022(3) -0.012(3) -0.031(3) F11A 0.076(5) 0.070(5) 0.064(4) 0.051(3) -0.047(4) -0.065(4) F12A 0.113(6) 0.047(5) 0.081(5) -0.017(4) 0.045(5) -0.044(4) N1 0.0107(10) 0.0158(11) 0.0145(10) -0.0001(9) -0.0014(8) -0.0074(9) N2 0.0135(10) 0.0185(11) 0.0148(11) -0.0010(9) -0.0019(8) -0.0103(9) N3 0.0143(10) 0.0152(11) 0.0168(11) -0.0010(9) -0.0017(8) -0.0090(9) Tl1 0.01769(5) 0.02008(5) 0.01551(5) -0.00137(4) -0.00353(3) -0.01122(4) _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 B1 C46 1.628(4) . ? B1 C38 1.633(4) . ? B1 C54 1.637(4) . ? B1 C62 1.640(4) . ? C1 C27 1.525(4) . ? C1 C16 1.531(3) . ? C1 C2 1.549(3) . ? C1 H1 0.9800 . ? C2 N1 1.273(3) . ? C2 C3 1.531(3) . ? C3 C6 1.534(4) . ? C3 C4 1.536(4) . ? C3 C5 1.540(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C12 1.385(4) . ? C7 C8 1.400(3) . ? C7 N1 1.432(3) . ? C8 C9 1.395(4) . ? C8 C13 1.511(4) . ? C9 C10 1.370(4) . ? C9 H9 0.9300 . ? C10 C11 1.372(4) . ? C10 H10 0.9300 . ? C11 C12 1.385(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C15 1.519(4) . ? C13 C14 1.523(4) . ? C13 H13 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N2 1.268(3) . ? C16 C17 1.504(3) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C23 1.387(4) . ? C18 C19 1.395(4) . ? C18 N2 1.439(3) . ? C19 C20 1.393(3) . ? C19 C24 1.510(4) . ? C20 C21 1.378(4) . ? C20 H20 0.9300 . ? C21 C22 1.370(4) . ? C21 H21 0.9300 . ? C22 C23 1.384(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.530(4) . ? C24 C26 1.530(4) . ? C24 H24 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 N3 1.273(3) . ? C27 C28 1.493(3) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.402(3) . ? C29 C30 1.407(4) . ? C29 N3 1.418(3) . ? C30 C31 1.382(4) . ? C30 C35 1.512(3) . ? C31 C32 1.391(4) . ? C31 H31 0.9300 . ? C32 C33 1.388(4) . ? C32 H32 0.9300 . ? C33 C34 1.386(4) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C37 1.520(4) . ? C35 C36 1.528(4) . ? C35 H35 0.9800 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.398(3) . ? C38 C43 1.402(3) . ? C39 C40 1.382(3) . ? C39 H39 0.9300 . ? C40 C41 1.384(3) . ? C40 C44 1.492(3) . ? C41 C42 1.389(3) . ? C41 H41 0.9300 . ? C42 C43 1.389(3) . ? C42 C45 1.482(3) . ? C43 H43 0.9300 . ? C44 F2 1.316(3) . ? C44 F3 1.332(3) . ? C44 F1 1.339(4) . ? C45 F5 1.308(3) . ? C45 F6 1.332(3) . ? C45 F4 1.349(3) . ? C46 C51 1.399(4) . ? C46 C47 1.401(3) . ? C47 C48 1.384(3) . ? C47 H47 0.9300 . ? C48 C49 1.378(4) . ? C48 C52 1.498(3) . ? C49 C50 1.380(4) . ? C49 H49 0.9300 . ? C50 C51 1.386(3) . ? C50 C53 1.489(4) . ? C51 H51 0.9300 . ? C52 F9 1.328(3) . ? C52 F7 1.339(3) . ? C52 F8 1.340(3) . ? C53 F12A 1.170(8) . ? C53 F12 1.223(4) . ? C53 F11 1.361(4) . ? C53 F10 1.367(4) . ? C53 F11A 1.377(7) . ? C53 F10A 1.432(7) . ? C54 C59 1.395(3) . ? C54 C55 1.408(3) . ? C55 C56 1.377(4) . ? C55 H55 0.9300 . ? C56 C57 1.389(3) . ? C56 C60 1.493(3) . ? C57 C58 1.381(3) . ? C57 H57 0.9300 . ? C58 C59 1.388(4) . ? C58 C61 1.491(4) . ? C59 H59 0.9300 . ? C60 F15 1.338(3) . ? C60 F14 1.340(3) . ? C60 F13 1.340(3) . ? C61 F18 1.334(3) . ? C61 F17 1.334(3) . ? C61 F16 1.340(4) . ? C62 C67 1.390(3) . ? C62 C63 1.405(3) . ? C63 C64 1.380(4) . ? C63 H63 0.9300 . ? C64 C65 1.399(3) . ? C64 C68 1.486(4) . ? C65 C66 1.377(3) . ? C65 H65 0.9300 . ? C66 C67 1.392(4) . ? C66 C69 1.491(3) . ? C67 H67 0.9300 . ? C68 F19 1.330(3) . ? C68 F20 1.332(3) . ? C68 F21 1.341(3) . ? C69 F23 1.327(3) . ? C69 F22 1.334(3) . ? C69 F24 1.339(3) . ? N1 Tl1 2.623(2) . ? N2 Tl1 2.6312(19) . ? N3 Tl1 2.763(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C46 B1 C38 111.8(2) . . ? C46 B1 C54 102.9(2) . . ? C38 B1 C54 114.36(19) . . ? C46 B1 C62 113.3(2) . . ? C38 B1 C62 103.7(2) . . ? C54 B1 C62 111.1(2) . . ? C27 C1 C16 110.9(2) . . ? C27 C1 C2 111.33(19) . . ? C16 C1 C2 113.6(2) . . ? C27 C1 H1 106.9 . . ? C16 C1 H1 106.9 . . ? C2 C1 H1 106.9 . . ? N1 C2 C3 130.3(2) . . ? N1 C2 C1 114.1(2) . . ? C3 C2 C1 115.62(19) . . ? C2 C3 C6 115.0(2) . . ? C2 C3 C4 108.3(2) . . ? C6 C3 C4 108.6(2) . . ? C2 C3 C5 108.6(2) . . ? C6 C3 C5 106.2(2) . . ? C4 C3 C5 110.0(2) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 C8 121.0(2) . . ? C12 C7 N1 117.9(2) . . ? C8 C7 N1 120.8(2) . . ? C9 C8 C7 116.4(3) . . ? C9 C8 C13 122.5(2) . . ? C7 C8 C13 121.1(2) . . ? C10 C9 C8 122.7(3) . . ? C10 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? C9 C10 C11 120.0(3) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 119.3(3) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C12 C7 120.5(3) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C8 C13 C15 111.3(2) . . ? C8 C13 C14 112.4(2) . . ? C15 C13 C14 109.6(2) . . ? C8 C13 H13 107.7 . . ? C15 C13 H13 107.7 . . ? C14 C13 H13 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C17 125.6(2) . . ? N2 C16 C1 120.2(2) . . ? C17 C16 C1 114.2(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 121.7(2) . . ? C23 C18 N2 119.3(2) . . ? C19 C18 N2 118.6(2) . . ? C20 C19 C18 116.5(3) . . ? C20 C19 C24 122.0(3) . . ? C18 C19 C24 121.4(2) . . ? C21 C20 C19 122.1(3) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C22 C21 C20 120.2(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 119.6(3) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C18 C23 C22 119.8(3) . . ? C18 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C19 C24 C25 110.7(2) . . ? C19 C24 C26 113.8(2) . . ? C25 C24 C26 110.3(3) . . ? C19 C24 H24 107.2 . . ? C25 C24 H24 107.2 . . ? C26 C24 H24 107.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 C28 125.9(2) . . ? N3 C27 C1 118.2(2) . . ? C28 C27 C1 115.9(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 120.4(2) . . ? C34 C29 N3 119.0(2) . . ? C30 C29 N3 120.3(2) . . ? C31 C30 C29 118.0(2) . . ? C31 C30 C35 122.1(2) . . ? C29 C30 C35 119.8(2) . . ? C30 C31 C32 122.1(3) . . ? C30 C31 H31 119.0 . . ? C32 C31 H31 119.0 . . ? C33 C32 C31 119.5(3) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C34 120.0(2) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C29 120.1(2) . . ? C33 C34 H34 120.0 . . ? C29 C34 H34 120.0 . . ? C30 C35 C37 113.5(2) . . ? C30 C35 C36 109.9(2) . . ? C37 C35 C36 110.1(2) . . ? C30 C35 H35 107.7 . . ? C37 C35 H35 107.7 . . ? C36 C35 H35 107.7 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C43 114.7(2) . . ? C39 C38 B1 122.3(2) . . ? C43 C38 B1 122.7(2) . . ? C40 C39 C38 123.2(2) . . ? C40 C39 H39 118.4 . . ? C38 C39 H39 118.4 . . ? C41 C40 C39 121.0(2) . . ? C41 C40 C44 120.3(2) . . ? C39 C40 C44 118.7(2) . . ? C40 C41 C42 117.3(2) . . ? C40 C41 H41 121.3 . . ? C42 C41 H41 121.3 . . ? C41 C42 C43 121.1(2) . . ? C41 C42 C45 119.7(2) . . ? C43 C42 C45 119.1(2) . . ? C42 C43 C38 122.5(2) . . ? C42 C43 H43 118.7 . . ? C38 C43 H43 118.7 . . ? F2 C44 F3 106.9(3) . . ? F2 C44 F1 106.2(2) . . ? F3 C44 F1 105.1(2) . . ? F2 C44 C40 114.0(2) . . ? F3 C44 C40 111.9(2) . . ? F1 C44 C40 112.1(3) . . ? F5 C45 F6 108.3(2) . . ? F5 C45 F4 104.6(2) . . ? F6 C45 F4 103.5(2) . . ? F5 C45 C42 113.5(2) . . ? F6 C45 C42 114.3(2) . . ? F4 C45 C42 111.7(2) . . ? C51 C46 C47 115.6(2) . . ? C51 C46 B1 119.6(2) . . ? C47 C46 B1 124.4(2) . . ? C48 C47 C46 121.9(2) . . ? C48 C47 H47 119.0 . . ? C46 C47 H47 119.0 . . ? C49 C48 C47 121.2(2) . . ? C49 C48 C52 117.6(2) . . ? C47 C48 C52 121.2(2) . . ? C48 C49 C50 118.3(2) . . ? C48 C49 H49 120.9 . . ? C50 C49 H49 120.9 . . ? C49 C50 C51 120.7(3) . . ? C49 C50 C53 119.4(2) . . ? C51 C50 C53 119.9(2) . . ? C50 C51 C46 122.4(2) . . ? C50 C51 H51 118.8 . . ? C46 C51 H51 118.8 . . ? F9 C52 F7 105.7(2) . . ? F9 C52 F8 105.8(2) . . ? F7 C52 F8 104.9(2) . . ? F9 C52 C48 114.2(2) . . ? F7 C52 C48 112.7(2) . . ? F8 C52 C48 112.8(2) . . ? F12A C53 F12 122.1(6) . . ? F12A C53 F11 39.1(6) . . ? F12 C53 F11 110.1(4) . . ? F12A C53 F10 58.8(6) . . ? F12 C53 F10 108.9(4) . . ? F11 C53 F10 97.8(3) . . ? F12A C53 F11A 111.7(6) . . ? F12 C53 F11A 50.4(4) . . ? F11 C53 F11A 136.6(4) . . ? F10 C53 F11A 64.2(4) . . ? F12A C53 F10A 105.9(6) . . ? F12 C53 F10A 43.5(4) . . ? F11 C53 F10A 74.6(4) . . ? F10 C53 F10A 139.3(4) . . ? F11A C53 F10A 93.6(5) . . ? F12A C53 C50 121.4(5) . . ? F12 C53 C50 115.5(3) . . ? F11 C53 C50 111.1(3) . . ? F10 C53 C50 112.1(3) . . ? F11A C53 C50 112.3(4) . . ? F10A C53 C50 107.8(4) . . ? C59 C54 C55 115.3(2) . . ? C59 C54 B1 125.8(2) . . ? C55 C54 B1 118.6(2) . . ? C56 C55 C54 122.8(2) . . ? C56 C55 H55 118.6 . . ? C54 C55 H55 118.6 . . ? C55 C56 C57 120.6(2) . . ? C55 C56 C60 119.1(2) . . ? C57 C56 C60 120.3(2) . . ? C58 C57 C56 118.0(2) . . ? C58 C57 H57 121.0 . . ? C56 C57 H57 121.0 . . ? C57 C58 C59 121.2(2) . . ? C57 C58 C61 119.1(2) . . ? C59 C58 C61 119.6(2) . . ? C58 C59 C54 122.1(2) . . ? C58 C59 H59 118.9 . . ? C54 C59 H59 118.9 . . ? F15 C60 F14 105.7(2) . . ? F15 C60 F13 106.0(2) . . ? F14 C60 F13 106.4(2) . . ? F15 C60 C56 111.9(2) . . ? F14 C60 C56 113.0(2) . . ? F13 C60 C56 113.3(2) . . ? F18 C61 F17 106.6(2) . . ? F18 C61 F16 105.2(2) . . ? F17 C61 F16 106.1(3) . . ? F18 C61 C58 113.1(2) . . ? F17 C61 C58 112.9(2) . . ? F16 C61 C58 112.3(2) . . ? C67 C62 C63 115.4(2) . . ? C67 C62 B1 124.2(2) . . ? C63 C62 B1 120.1(2) . . ? C64 C63 C62 122.9(2) . . ? C64 C63 H63 118.6 . . ? C62 C63 H63 118.6 . . ? C63 C64 C65 120.4(2) . . ? C63 C64 C68 121.0(2) . . ? C65 C64 C68 118.5(2) . . ? C66 C65 C64 117.7(2) . . ? C66 C65 H65 121.2 . . ? C64 C65 H65 121.2 . . ? C65 C66 C67 121.4(2) . . ? C65 C66 C69 120.4(2) . . ? C67 C66 C69 118.1(2) . . ? C62 C67 C66 122.2(2) . . ? C62 C67 H67 118.9 . . ? C66 C67 H67 118.9 . . ? F19 C68 F20 106.2(2) . . ? F19 C68 F21 106.4(2) . . ? F20 C68 F21 105.1(2) . . ? F19 C68 C64 113.2(2) . . ? F20 C68 C64 113.8(2) . . ? F21 C68 C64 111.5(2) . . ? F23 C69 F22 106.0(2) . . ? F23 C69 F24 106.8(2) . . ? F22 C69 F24 105.2(2) . . ? F23 C69 C66 113.3(2) . . ? F22 C69 C66 111.7(2) . . ? F24 C69 C66 113.2(2) . . ? C2 N1 C7 126.3(2) . . ? C2 N1 Tl1 126.49(16) . . ? C7 N1 Tl1 102.06(14) . . ? C16 N2 C18 121.5(2) . . ? C16 N2 Tl1 116.69(16) . . ? C18 N2 Tl1 107.93(14) . . ? C27 N3 C29 121.7(2) . . ? C27 N3 Tl1 112.58(17) . . ? C29 N3 Tl1 108.52(14) . . ? N1 Tl1 N2 68.38(6) . . ? N1 Tl1 N3 74.01(6) . . ? N2 Tl1 N3 70.30(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.413 _refine_diff_density_min -1.909 _database_code_depnum_ccdc_archive 'CCDC 899512'