# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Manfred Scheer' _publ_contact_author_email MANFRED.SCHEER@CHEMIE.UNI-REGENSBURG.DE _publ_section_title ; Mono-, di- and polymetallic Tl(I) complexes stabilized by a 2,5-bis(2-pyridyl)-1-phenyl-phosphole ligand ; loop_ _publ_author_name 'Manfred Scheer' 'Christophe Lescop' 'Regis Reau' 'Stefan Welsch' # Attachment 'sw30c.cif' # CIF-file generated for sw30c Welsch/Lescop R = 0.02 #============================================================================== data_sw30c _database_code_depnum_ccdc_archive 'CCDC 713903' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 Al F36 O4, 2 (C24 H21 N2 P), Tl' _chemical_formula_structural ? _chemical_formula_sum 'C64 H42 Al F36 N4 O4 P2 Tl' _chemical_formula_iupac ? _chemical_formula_weight 1908.32 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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' Al Al 0.0645 0.0514 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.3378(3) _cell_length_b 17.5125(4) _cell_length_c 18.9823(5) _cell_angle_alpha 111.9840(11) _cell_angle_beta 91.1627(12) _cell_angle_gamma 98.9673(10) _cell_volume 3439.48(15) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 27.53 _cell_special_details ; ; _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1868 _exptl_absorpt_coefficient_mu 2.557 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.590 _exptl_absorpt_correction_T_max 0.600 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ccd _diffrn_measurement_method none _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 48350 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 15786 # number of observed reflections (> n sig(I)) _reflns_number_gt 15103 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'KappaCCD software package' _computing_cell_refinement 'KappaCCD software package' _computing_data_reduction 'KappaCCD software package' _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; PLATON (Spek, 2003) and SHELXL-97 (Sheldrick, 1997) ; #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0269P)^2^+2.5106P] 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 refU _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 15786 _refine_ls_number_parameters 1121 _refine_ls_number_restraints 12 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0524 _refine_ls_wR_factor_gt 0.0517 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.970 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.066 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Tl1 Tl 0.470071(5) 0.088497(4) 0.170290(4) 0.01674(3) Uani 1 1 d . . . P1 P 0.32846(4) 0.05949(3) 0.00938(3) 0.01443(8) Uani 1 1 d . . . P2 P 0.36426(4) 0.11041(3) 0.32686(3) 0.01649(9) Uani 1 1 d . . . N1 N 0.24240(13) -0.00398(9) 0.13303(9) 0.0177(3) Uani 1 1 d . . . N3 N 0.35885(14) 0.22361(10) 0.23514(10) 0.0210(3) Uani 1 1 d . . . N2 N 0.41526(15) 0.08567(10) -0.14135(9) 0.0205(3) Uani 1 1 d . . . N4 N 0.42570(15) -0.01160(10) 0.37856(9) 0.0219(3) Uani 1 1 d . . . C1 C 0.30382(16) 0.13286(11) -0.03218(10) 0.0161(3) Uani 1 1 d . . . C2 C 0.21608(16) 0.17490(11) 0.00338(10) 0.0168(3) Uani 1 1 d . . . C3 C 0.18536(18) 0.25286(12) -0.00348(11) 0.0220(4) Uani 1 1 d . . . H3A H 0.1884 0.2473 -0.0572 0.026 Uiso 1 1 calc R . . H3B H 0.2466 0.3015 0.0278 0.026 Uiso 1 1 calc R . . C4 C 0.06153(18) 0.26971(13) 0.02190(13) 0.0261(4) Uani 1 1 d . . . H4A H 0.0519 0.3260 0.0248 0.031 Uiso 1 1 calc R . . H4B H -0.0013 0.2280 -0.0159 0.031 Uiso 1 1 calc R . . C5 C 0.04706(18) 0.26455(12) 0.09959(12) 0.0251(4) Uani 1 1 d . . . H5A H -0.0291 0.2819 0.1184 0.030 Uiso 1 1 calc R . . H5B H 0.1137 0.3029 0.1365 0.030 Uiso 1 1 calc R . . C6 C 0.04707(17) 0.17498(11) 0.09329(11) 0.0209(4) Uani 1 1 d . . . H6A H 0.0500 0.1740 0.1451 0.025 Uiso 1 1 calc R . . H6B H -0.0287 0.1391 0.0650 0.025 Uiso 1 1 calc R . . C7 C 0.15119(15) 0.13923(11) 0.05336(10) 0.0157(3) Uani 1 1 d . . . C8 C 0.19542(15) 0.07362(11) 0.05928(9) 0.0149(3) Uani 1 1 d . . . C9 C 0.15524(15) 0.02198(10) 0.10244(10) 0.0151(3) Uani 1 1 d . . . C10 C 0.03420(16) -0.00429(11) 0.10819(10) 0.0180(3) Uani 1 1 d . . . H10 H -0.0261 0.0145 0.0866 0.022 Uiso 1 1 calc R . . C11 C 0.00283(17) -0.05797(12) 0.14558(11) 0.0211(4) Uani 1 1 d . . . H11 H -0.0791 -0.0761 0.1502 0.025 Uiso 1 1 calc R . . C12 C 0.09255(17) -0.08496(12) 0.17624(11) 0.0214(4) Uani 1 1 d . . . H12 H 0.0736 -0.1223 0.2016 0.026 Uiso 1 1 calc R . . C13 C 0.21017(17) -0.05583(12) 0.16872(11) 0.0210(4) Uani 1 1 d . . . H13 H 0.2717 -0.0737 0.1902 0.025 Uiso 1 1 calc R . . C14 C 0.38617(15) 0.15251(11) -0.08480(10) 0.0165(3) Uani 1 1 d . . . C15 C 0.43277(17) 0.23419(12) -0.07691(11) 0.0215(4) Uani 1 1 d . . . H15 H 0.4120 0.2803 -0.0363 0.026 Uiso 1 1 calc R . . C16 C 0.50949(17) 0.24762(12) -0.12864(12) 0.0228(4) Uani 1 1 d . . . H16 H 0.5434 0.3028 -0.1233 0.027 Uiso 1 1 calc R . . C17 C 0.53588(17) 0.17935(12) -0.18803(11) 0.0219(4) Uani 1 1 d . . . H17 H 0.5865 0.1864 -0.2252 0.026 Uiso 1 1 calc R . . C18 C 0.48657(17) 0.10035(12) -0.19186(11) 0.0223(4) Uani 1 1 d . . . H18 H 0.5045 0.0535 -0.2330 0.027 Uiso 1 1 calc R . . C19 C 0.29838(15) -0.04908(11) -0.05844(10) 0.0164(3) Uani 1 1 d . . . C20 C 0.24215(15) -0.07603(12) -0.13190(11) 0.0189(3) Uani 1 1 d . . . H20 H 0.2159 -0.0370 -0.1497 0.023 Uiso 1 1 calc R . . C21 C 0.22489(17) -0.16046(12) -0.17887(12) 0.0242(4) Uani 1 1 d . . . H21 H 0.1859 -0.1789 -0.2287 0.029 Uiso 1 1 calc R . . C22 C 0.26395(18) -0.21802(12) -0.15390(13) 0.0275(4) Uani 1 1 d . . . H22 H 0.2522 -0.2755 -0.1866 0.033 Uiso 1 1 calc R . . C23 C 0.32009(19) -0.19148(12) -0.08112(12) 0.0260(4) Uani 1 1 d . . . H23 H 0.3466 -0.2308 -0.0638 0.031 Uiso 1 1 calc R . . C24 C 0.33759(17) -0.10743(11) -0.03358(11) 0.0197(4) Uani 1 1 d . . . H24 H 0.3765 -0.0894 0.0162 0.024 Uiso 1 1 calc R . . C25 C 0.26604(16) 0.05825(11) 0.37476(10) 0.0172(3) Uani 1 1 d . . . C26 C 0.15460(16) 0.07885(11) 0.37450(10) 0.0182(3) Uani 1 1 d . . . C27 C 0.04419(17) 0.03875(12) 0.39956(11) 0.0213(4) Uani 1 1 d . . . H27A H 0.0626 0.0421 0.4520 0.026 Uiso 1 1 calc R . . H27B H 0.0251 -0.0212 0.3658 0.026 Uiso 1 1 calc R . . C28 C -0.06643(18) 0.07840(14) 0.39852(12) 0.0272(4) Uani 1 1 d . . . H28A H -0.1391 0.0389 0.3986 0.033 Uiso 1 1 calc R . . H28B H -0.0613 0.1297 0.4451 0.033 Uiso 1 1 calc R . . C29 C -0.07678(18) 0.10037(15) 0.32880(12) 0.0285(4) Uani 1 1 d . . . H29A H -0.1532 0.1205 0.3266 0.034 Uiso 1 1 calc R . . H29B H -0.0766 0.0500 0.2820 0.034 Uiso 1 1 calc R . . C30 C 0.02876(17) 0.16859(14) 0.33305(12) 0.0257(4) Uani 1 1 d . . . H30A H 0.0249 0.1800 0.2859 0.031 Uiso 1 1 calc R . . H30B H 0.0228 0.2208 0.3766 0.031 Uiso 1 1 calc R . . C31 C 0.14719(16) 0.14277(11) 0.34254(10) 0.0192(3) Uani 1 1 d . . . C32 C 0.25311(16) 0.17080(11) 0.32002(10) 0.0183(3) Uani 1 1 d . . . C33 C 0.27961(16) 0.23568(12) 0.28858(11) 0.0197(4) Uani 1 1 d . . . C34 C 0.2317(2) 0.30941(13) 0.31599(13) 0.0278(4) Uani 1 1 d . . . H34 H 0.1764 0.3173 0.3540 0.033 Uiso 1 1 calc R . . C35 C 0.2654(2) 0.37063(13) 0.28733(14) 0.0325(5) Uani 1 1 d . . . H35 H 0.2336 0.4210 0.3055 0.039 Uiso 1 1 calc R . . C36 C 0.3459(2) 0.35794(14) 0.23206(14) 0.0318(5) Uani 1 1 d . . . H36 H 0.3701 0.3988 0.2111 0.038 Uiso 1 1 calc R . . C37 C 0.38994(19) 0.28378(13) 0.20821(13) 0.0280(4) Uani 1 1 d . . . H37 H 0.4456 0.2750 0.1704 0.034 Uiso 1 1 calc R . . C38 C 0.31299(17) -0.00301(11) 0.39800(10) 0.0186(3) Uani 1 1 d . . . C39 C 0.2527(2) -0.04842(12) 0.43707(12) 0.0267(4) Uani 1 1 d . . . H39 H 0.1729 -0.0428 0.4494 0.032 Uiso 1 1 calc R . . C40 C 0.3110(2) -0.10209(13) 0.45768(13) 0.0318(5) Uani 1 1 d . . . H40 H 0.2712 -0.1333 0.4845 0.038 Uiso 1 1 calc R . . C41 C 0.4261(2) -0.10989(13) 0.43920(12) 0.0297(5) Uani 1 1 d . . . H41 H 0.4678 -0.1457 0.4533 0.036 Uiso 1 1 calc R . . C42 C 0.47938(19) -0.06366(12) 0.39916(12) 0.0255(4) Uani 1 1 d . . . H42 H 0.5587 -0.0694 0.3856 0.031 Uiso 1 1 calc R . . C43 C 0.48123(17) 0.18673(11) 0.39621(10) 0.0187(3) Uani 1 1 d . . . C44 C 0.45519(19) 0.25239(13) 0.45853(12) 0.0262(4) Uani 1 1 d . . . H44 H 0.3741 0.2574 0.4676 0.031 Uiso 1 1 calc R . . C45 C 0.5474(2) 0.31118(14) 0.50807(13) 0.0329(5) Uani 1 1 d . . . H45 H 0.5292 0.3558 0.5512 0.040 Uiso 1 1 calc R . . C46 C 0.6654(2) 0.30462(14) 0.49454(13) 0.0320(5) Uani 1 1 d . . . H46 H 0.7282 0.3452 0.5280 0.038 Uiso 1 1 calc R . . C47 C 0.69209(19) 0.23956(14) 0.43279(14) 0.0322(5) Uani 1 1 d . . . H47 H 0.7733 0.2352 0.4237 0.039 Uiso 1 1 calc R . . C48 C 0.60039(18) 0.18008(13) 0.38350(12) 0.0261(4) Uani 1 1 d . . . H48 H 0.6191 0.1348 0.3411 0.031 Uiso 1 1 calc R . . Al1 Al 0.13037(5) 0.41228(3) 0.74399(3) 0.01442(10) Uani 1 1 d . A . O1 O 0.18723(13) 0.47401(9) 0.69605(8) 0.0248(3) Uani 1 1 d . . . O2 O 0.13952(12) 0.30786(8) 0.69864(8) 0.0204(3) Uani 1 1 d . . . O3 O 0.21557(12) 0.44650(8) 0.82954(8) 0.0218(3) Uani 1 1 d . . . O4 O -0.01897(12) 0.41914(9) 0.75351(8) 0.0240(3) Uani 1 1 d . . . C49 C 0.1784(2) 0.49673(13) 0.63608(11) 0.0258(4) Uani 1 1 d . . . C50 C 0.20952(16) 0.24910(11) 0.68250(10) 0.0179(3) Uani 1 1 d . . . C51 C 0.27561(16) 0.51045(11) 0.89027(10) 0.0176(3) Uani 1 1 d . . . C53 C 0.0846(2) 0.55532(14) 0.64806(14) 0.0341(5) Uani 1 1 d . . . C54 C 0.1415(3) 0.41936(16) 0.56061(13) 0.0383(5) Uani 1 1 d . . . C55 C 0.3029(2) 0.54505(15) 0.63081(14) 0.0372(5) Uani 1 1 d . . . C56 C 0.1681(2) 0.18509(12) 0.60029(11) 0.0259(4) Uani 1 1 d . . . C57 C 0.19317(18) 0.20389(12) 0.73892(11) 0.0241(4) Uani 1 1 d . . . C58 C 0.34503(18) 0.28605(12) 0.68669(12) 0.0243(4) Uani 1 1 d . . . C59 C 0.3104(2) 0.47301(14) 0.94861(13) 0.0314(5) Uani 1 1 d . . . C61 C 0.3906(2) 0.55269(13) 0.86749(13) 0.0317(5) Uani 1 1 d . . . C60 C 0.19594(19) 0.57653(12) 0.92741(12) 0.0248(4) Uani 1 1 d . . . F1 F -0.02684(13) 0.51110(10) 0.63070(9) 0.0456(4) Uani 1 1 d . . . F3 F 0.09029(14) 0.60739(9) 0.72035(9) 0.0448(4) Uani 1 1 d . . . F2 F 0.09768(16) 0.60119(10) 0.60536(10) 0.0521(4) Uani 1 1 d . . . F4 F 0.05327(14) 0.36477(9) 0.57049(8) 0.0444(4) Uani 1 1 d . . . F5 F 0.23368(16) 0.37998(10) 0.53774(8) 0.0479(4) Uani 1 1 d . . . F6 F 0.10336(18) 0.43949(11) 0.50404(8) 0.0567(5) Uani 1 1 d . . . F7 F 0.32225(14) 0.62300(9) 0.68365(10) 0.0469(4) Uani 1 1 d . . . F8 F 0.31237(17) 0.55097(11) 0.56290(10) 0.0567(4) Uani 1 1 d . . . F9 F 0.38961(13) 0.50737(10) 0.64235(10) 0.0452(4) Uani 1 1 d . . . F10 F 0.04933(12) 0.16519(8) 0.58989(7) 0.0335(3) Uani 1 1 d . . . F11 F 0.20897(14) 0.11295(8) 0.58437(8) 0.0390(3) Uani 1 1 d . . . F12 F 0.20409(14) 0.21633(8) 0.54899(7) 0.0386(3) Uani 1 1 d . . . F16 F 0.40841(12) 0.22842(8) 0.64809(9) 0.0398(3) Uani 1 1 d . . . F18 F 0.35847(12) 0.34550(8) 0.65836(8) 0.0344(3) Uani 1 1 d . . . F17 F 0.39319(11) 0.32085(8) 0.75829(8) 0.0324(3) Uani 1 1 d . . . F15 F 0.19930(13) 0.25903(8) 0.81028(7) 0.0347(3) Uani 1 1 d . . . F14 F 0.08549(11) 0.15547(8) 0.72529(7) 0.0309(3) Uani 1 1 d . . . F13 F 0.27372(12) 0.15537(8) 0.73481(8) 0.0365(3) Uani 1 1 d . . . F21 F 0.22001(15) 0.42105(8) 0.95701(8) 0.0406(3) Uani 1 1 d . . . F20 F 0.39921(14) 0.43024(9) 0.92482(9) 0.0474(4) Uani 1 1 d . . . F19 F 0.34750(14) 0.53273(9) 1.01782(8) 0.0427(4) Uani 1 1 d . . . F25 F 0.47054(13) 0.59745(10) 0.92658(10) 0.0521(4) Uani 1 1 d . . . F27 F 0.44384(13) 0.49678(9) 0.81731(9) 0.0457(4) Uani 1 1 d . . . F26 F 0.36453(14) 0.60460(8) 0.83493(9) 0.0436(3) Uani 1 1 d . . . F22 F 0.25772(13) 0.64811(8) 0.97787(8) 0.0370(3) Uani 1 1 d . . . F24 F 0.14137(14) 0.59431(9) 0.87438(8) 0.0402(3) Uani 1 1 d . . . F23 F 0.11147(13) 0.54826(8) 0.96323(9) 0.0398(3) Uani 1 1 d . . . C52A C -0.1307(19) 0.3762(9) 0.7647(9) 0.0188(13) Uani 0.413(5) 1 d PD A 1 C62A C -0.2201(5) 0.4353(3) 0.7670(4) 0.0370(15) Uani 0.413(5) 1 d PD A 1 C63A C -0.1166(6) 0.3677(6) 0.8413(4) 0.0423(18) Uani 0.413(5) 1 d PD A 1 C64A C -0.1723(4) 0.2904(3) 0.6998(3) 0.0264(12) Uani 0.413(5) 1 d PD A 1 F28A F -0.3171(5) 0.4173(4) 0.7984(4) 0.0542(15) Uani 0.413(5) 1 d P A 1 F29A F -0.2544(10) 0.4265(7) 0.6947(7) 0.046(2) Uani 0.413(5) 1 d P A 1 F30A F -0.1718(14) 0.5148(9) 0.8089(9) 0.050(3) Uani 0.413(5) 1 d P A 1 F31A F -0.2113(13) 0.3224(11) 0.8520(9) 0.032(2) Uani 0.413(5) 1 d P A 1 F32A F -0.1091(4) 0.4421(4) 0.8982(2) 0.0585(17) Uani 0.413(5) 1 d P A 1 F33A F -0.0306(15) 0.3321(10) 0.8479(12) 0.054(4) Uani 0.413(5) 1 d P A 1 F34A F -0.2905(4) 0.2665(3) 0.6989(3) 0.0369(10) Uani 0.413(5) 1 d P A 1 F35A F -0.1191(4) 0.2322(3) 0.7107(3) 0.0355(10) Uani 0.413(5) 1 d P A 1 F36A F -0.1497(11) 0.3033(9) 0.6381(7) 0.070(4) Uani 0.413(5) 1 d P A 1 C52B C -0.1233(13) 0.3937(5) 0.7708(6) 0.0188(13) Uani 0.587(5) 1 d PD A 2 C62B C -0.1785(3) 0.4666(3) 0.8270(2) 0.0269(9) Uani 0.587(5) 1 d PD A 2 C63B C -0.1209(4) 0.3270(3) 0.8080(3) 0.0336(11) Uani 0.587(5) 1 d PD A 2 C64B C -0.2101(4) 0.3510(2) 0.6966(2) 0.0342(10) Uani 0.587(5) 1 d PD A 2 F28B F -0.2972(3) 0.4485(3) 0.8296(2) 0.0446(9) Uani 0.587(5) 1 d P A 2 F29B F -0.1565(10) 0.5326(6) 0.8060(6) 0.0374(16) Uani 0.587(5) 1 d P A 2 F30B F -0.1281(3) 0.4909(2) 0.89714(15) 0.0405(7) Uani 0.587(5) 1 d P A 2 F31B F -0.2155(11) 0.3124(10) 0.8438(7) 0.060(3) Uani 0.587(5) 1 d P A 2 F32B F -0.0175(8) 0.3522(6) 0.8563(7) 0.0340(13) Uani 0.587(5) 1 d P A 2 F33B F -0.1133(3) 0.2524(2) 0.7557(3) 0.0460(8) Uani 0.587(5) 1 d P A 2 F34B F -0.3105(3) 0.3043(3) 0.7036(2) 0.0514(9) Uani 0.587(5) 1 d P A 2 F35B F -0.1521(5) 0.2949(5) 0.6369(4) 0.0364(16) Uani 0.587(5) 1 d P A 2 F36B F -0.2409(8) 0.4101(6) 0.6753(5) 0.0509(19) Uani 0.587(5) 1 d P A 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 0.01329(4) 0.02017(4) 0.01888(4) 0.00949(3) 0.00276(2) 0.00370(2) P1 0.01296(19) 0.0154(2) 0.0164(2) 0.00738(16) 0.00256(15) 0.00345(16) P2 0.0169(2) 0.0184(2) 0.0170(2) 0.00904(17) 0.00349(16) 0.00534(17) N1 0.0152(7) 0.0194(7) 0.0203(7) 0.0094(6) 0.0029(6) 0.0033(6) N3 0.0186(7) 0.0222(8) 0.0266(8) 0.0135(7) 0.0046(6) 0.0055(6) N2 0.0231(8) 0.0186(7) 0.0250(8) 0.0121(6) 0.0092(6) 0.0076(6) N4 0.0252(8) 0.0193(7) 0.0232(8) 0.0092(6) 0.0041(6) 0.0068(6) C1 0.0167(8) 0.0152(8) 0.0164(8) 0.0066(6) -0.0003(6) 0.0021(6) C2 0.0165(8) 0.0160(8) 0.0174(8) 0.0059(7) -0.0006(6) 0.0032(6) C3 0.0260(10) 0.0191(8) 0.0249(9) 0.0109(7) 0.0052(7) 0.0085(7) C4 0.0254(10) 0.0232(9) 0.0358(11) 0.0148(8) 0.0062(8) 0.0120(8) C5 0.0252(10) 0.0203(9) 0.0314(10) 0.0086(8) 0.0100(8) 0.0104(7) C6 0.0195(9) 0.0203(9) 0.0244(9) 0.0080(7) 0.0065(7) 0.0084(7) C7 0.0150(8) 0.0161(8) 0.0143(8) 0.0040(6) 0.0011(6) 0.0029(6) C8 0.0131(7) 0.0171(8) 0.0133(7) 0.0047(6) 0.0018(6) 0.0023(6) C9 0.0165(8) 0.0147(7) 0.0131(7) 0.0040(6) 0.0023(6) 0.0027(6) C10 0.0149(8) 0.0194(8) 0.0175(8) 0.0050(7) 0.0010(6) 0.0022(6) C11 0.0165(8) 0.0229(9) 0.0214(9) 0.0071(7) 0.0038(7) -0.0005(7) C12 0.0229(9) 0.0205(9) 0.0224(9) 0.0110(7) 0.0048(7) 0.0010(7) C13 0.0194(9) 0.0228(9) 0.0248(9) 0.0133(7) 0.0024(7) 0.0043(7) C14 0.0152(8) 0.0191(8) 0.0177(8) 0.0096(7) 0.0007(6) 0.0035(6) C15 0.0228(9) 0.0180(8) 0.0210(9) 0.0058(7) 0.0024(7) -0.0002(7) C16 0.0210(9) 0.0196(9) 0.0287(10) 0.0123(8) 0.0018(7) -0.0018(7) C17 0.0190(9) 0.0274(9) 0.0256(9) 0.0164(8) 0.0063(7) 0.0050(7) C18 0.0242(9) 0.0217(9) 0.0248(9) 0.0109(7) 0.0093(7) 0.0092(7) C19 0.0124(7) 0.0173(8) 0.0201(8) 0.0070(7) 0.0067(6) 0.0038(6) C20 0.0115(8) 0.0226(9) 0.0226(9) 0.0086(7) 0.0035(6) 0.0033(7) C21 0.0144(8) 0.0265(10) 0.0246(9) 0.0034(8) 0.0018(7) -0.0004(7) C22 0.0242(10) 0.0176(9) 0.0346(11) 0.0047(8) 0.0080(8) -0.0005(7) C23 0.0283(10) 0.0191(9) 0.0347(11) 0.0136(8) 0.0093(8) 0.0065(8) C24 0.0202(9) 0.0202(9) 0.0217(9) 0.0105(7) 0.0071(7) 0.0051(7) C25 0.0213(9) 0.0159(8) 0.0138(8) 0.0053(6) 0.0034(6) 0.0019(7) C26 0.0208(9) 0.0171(8) 0.0140(8) 0.0032(6) 0.0024(6) 0.0023(7) C27 0.0206(9) 0.0216(9) 0.0190(8) 0.0055(7) 0.0041(7) 0.0012(7) C28 0.0204(9) 0.0357(11) 0.0253(10) 0.0117(9) 0.0060(8) 0.0043(8) C29 0.0194(9) 0.0415(12) 0.0255(10) 0.0128(9) 0.0031(8) 0.0075(8) C30 0.0213(9) 0.0357(11) 0.0260(10) 0.0155(8) 0.0054(8) 0.0122(8) C31 0.0196(9) 0.0214(9) 0.0163(8) 0.0057(7) 0.0028(7) 0.0068(7) C32 0.0211(9) 0.0193(8) 0.0171(8) 0.0081(7) 0.0029(7) 0.0079(7) C33 0.0184(8) 0.0221(9) 0.0212(9) 0.0106(7) 0.0008(7) 0.0054(7) C34 0.0314(11) 0.0266(10) 0.0318(11) 0.0144(9) 0.0097(9) 0.0138(8) C35 0.0360(12) 0.0254(10) 0.0447(13) 0.0191(10) 0.0104(10) 0.0149(9) C36 0.0300(11) 0.0269(10) 0.0489(13) 0.0254(10) 0.0068(10) 0.0070(8) C37 0.0245(10) 0.0299(10) 0.0380(11) 0.0210(9) 0.0092(8) 0.0071(8) C38 0.0248(9) 0.0146(8) 0.0146(8) 0.0031(6) 0.0028(7) 0.0042(7) C39 0.0335(11) 0.0225(9) 0.0292(10) 0.0134(8) 0.0133(8) 0.0095(8) C40 0.0489(13) 0.0262(10) 0.0310(11) 0.0190(9) 0.0176(10) 0.0149(9) C41 0.0469(13) 0.0242(10) 0.0251(10) 0.0125(8) 0.0081(9) 0.0182(9) C42 0.0304(10) 0.0241(9) 0.0265(10) 0.0113(8) 0.0061(8) 0.0125(8) C43 0.0205(9) 0.0196(8) 0.0200(8) 0.0125(7) 0.0017(7) 0.0026(7) C44 0.0278(10) 0.0251(10) 0.0254(10) 0.0099(8) 0.0059(8) 0.0028(8) C45 0.0430(13) 0.0246(10) 0.0272(10) 0.0074(8) 0.0025(9) 0.0006(9) C46 0.0352(12) 0.0273(10) 0.0335(11) 0.0170(9) -0.0093(9) -0.0068(9) C47 0.0212(10) 0.0367(12) 0.0431(13) 0.0215(10) -0.0031(9) 0.0021(9) C48 0.0217(9) 0.0285(10) 0.0299(10) 0.0124(8) 0.0018(8) 0.0067(8) Al1 0.0161(2) 0.0142(2) 0.0133(2) 0.00586(19) 0.00072(19) 0.00213(19) O1 0.0285(7) 0.0282(7) 0.0236(7) 0.0169(6) 0.0037(6) 0.0041(6) O2 0.0213(6) 0.0156(6) 0.0216(6) 0.0036(5) 0.0030(5) 0.0040(5) O3 0.0258(7) 0.0182(6) 0.0184(6) 0.0048(5) -0.0042(5) 0.0011(5) O4 0.0194(6) 0.0256(7) 0.0309(7) 0.0141(6) 0.0066(5) 0.0057(5) C49 0.0343(11) 0.0260(10) 0.0223(9) 0.0150(8) 0.0012(8) 0.0056(8) C50 0.0216(9) 0.0150(8) 0.0163(8) 0.0050(7) 0.0032(7) 0.0026(7) C51 0.0203(8) 0.0140(8) 0.0160(8) 0.0040(6) -0.0015(7) 0.0007(6) C53 0.0410(13) 0.0323(11) 0.0339(12) 0.0173(9) -0.0025(10) 0.0091(9) C54 0.0558(15) 0.0378(12) 0.0251(11) 0.0153(10) 0.0013(10) 0.0112(11) C55 0.0447(14) 0.0368(12) 0.0386(13) 0.0236(10) 0.0117(10) 0.0070(10) C56 0.0363(11) 0.0184(9) 0.0203(9) 0.0045(7) 0.0049(8) 0.0049(8) C57 0.0273(10) 0.0217(9) 0.0238(9) 0.0110(8) -0.0004(8) 0.0004(7) C58 0.0241(9) 0.0189(9) 0.0311(10) 0.0098(8) 0.0078(8) 0.0058(7) C59 0.0401(12) 0.0267(10) 0.0268(10) 0.0091(8) -0.0061(9) 0.0084(9) C61 0.0306(11) 0.0197(9) 0.0355(11) 0.0028(8) 0.0063(9) -0.0025(8) C60 0.0301(10) 0.0188(9) 0.0249(10) 0.0069(8) 0.0037(8) 0.0062(8) F1 0.0373(8) 0.0498(9) 0.0517(9) 0.0209(7) -0.0093(7) 0.0118(7) F3 0.0471(8) 0.0424(8) 0.0408(8) 0.0069(6) 0.0003(7) 0.0195(7) F2 0.0655(11) 0.0461(9) 0.0633(10) 0.0389(8) -0.0001(8) 0.0179(8) F4 0.0563(9) 0.0351(7) 0.0337(7) 0.0093(6) -0.0094(7) -0.0034(7) F5 0.0735(11) 0.0429(8) 0.0309(7) 0.0121(6) 0.0134(7) 0.0243(8) F6 0.0898(13) 0.0605(10) 0.0252(7) 0.0207(7) -0.0069(8) 0.0194(9) F7 0.0499(9) 0.0334(7) 0.0592(10) 0.0243(7) 0.0040(7) -0.0040(6) F8 0.0758(12) 0.0624(10) 0.0533(10) 0.0455(9) 0.0250(9) 0.0115(9) F9 0.0346(7) 0.0499(9) 0.0622(10) 0.0330(8) 0.0168(7) 0.0085(6) F10 0.0365(7) 0.0289(6) 0.0248(6) 0.0024(5) -0.0063(5) -0.0023(5) F11 0.0550(9) 0.0196(6) 0.0349(7) -0.0005(5) 0.0045(6) 0.0123(6) F12 0.0590(9) 0.0352(7) 0.0201(6) 0.0103(5) 0.0099(6) 0.0038(6) F16 0.0307(7) 0.0275(6) 0.0589(9) 0.0100(6) 0.0196(6) 0.0130(5) F18 0.0303(7) 0.0309(6) 0.0506(8) 0.0257(6) 0.0121(6) 0.0033(5) F17 0.0238(6) 0.0284(6) 0.0400(7) 0.0090(5) -0.0053(5) 0.0016(5) F15 0.0497(8) 0.0326(7) 0.0200(6) 0.0101(5) 0.0005(5) 0.0025(6) F14 0.0315(6) 0.0274(6) 0.0344(7) 0.0161(5) 0.0044(5) -0.0045(5) F13 0.0388(7) 0.0311(7) 0.0481(8) 0.0231(6) 0.0005(6) 0.0108(6) F21 0.0651(10) 0.0294(7) 0.0300(7) 0.0182(6) -0.0022(6) -0.0007(6) F20 0.0537(9) 0.0455(8) 0.0449(8) 0.0128(7) -0.0117(7) 0.0282(7) F19 0.0587(9) 0.0392(7) 0.0228(6) 0.0056(6) -0.0145(6) 0.0057(7) F25 0.0321(8) 0.0438(8) 0.0547(10) -0.0016(7) -0.0048(7) -0.0144(6) F27 0.0368(8) 0.0302(7) 0.0585(9) 0.0042(7) 0.0245(7) 0.0024(6) F26 0.0580(9) 0.0269(7) 0.0456(8) 0.0170(6) 0.0172(7) -0.0027(6) F22 0.0502(8) 0.0183(6) 0.0321(7) -0.0015(5) 0.0057(6) 0.0043(5) F24 0.0517(9) 0.0342(7) 0.0417(8) 0.0159(6) 0.0002(6) 0.0248(6) F23 0.0383(7) 0.0325(7) 0.0499(8) 0.0147(6) 0.0226(6) 0.0101(6) C52A 0.0154(18) 0.014(4) 0.0246(18) 0.007(2) -0.0013(13) -0.003(3) C62A 0.027(3) 0.030(3) 0.046(4) 0.005(2) 0.003(2) 0.005(2) C63A 0.020(3) 0.070(6) 0.036(4) 0.025(4) 0.003(3) -0.005(4) C64A 0.021(2) 0.027(2) 0.029(3) 0.010(2) -0.0012(19) -0.0009(19) F28A 0.021(2) 0.068(4) 0.065(4) 0.011(3) 0.017(3) 0.017(2) F29A 0.022(2) 0.050(4) 0.082(8) 0.044(5) -0.006(4) 0.007(3) F30A 0.032(3) 0.030(6) 0.076(6) 0.002(4) 0.014(3) 0.015(4) F31A 0.021(4) 0.050(4) 0.031(3) 0.025(3) 0.001(2) -0.001(3) F32A 0.046(2) 0.083(4) 0.0200(18) -0.003(2) 0.0081(16) -0.009(3) F33A 0.041(4) 0.068(8) 0.061(5) 0.048(6) -0.019(3) -0.023(4) F34A 0.0215(18) 0.043(3) 0.044(2) 0.020(2) -0.0028(15) -0.0071(18) F35A 0.0305(18) 0.0242(19) 0.054(3) 0.018(2) 0.004(2) 0.0043(14) F36A 0.119(8) 0.048(5) 0.028(5) -0.005(3) -0.014(4) 0.029(5) C52B 0.0154(18) 0.014(4) 0.0246(18) 0.007(2) -0.0013(13) -0.003(3) C62B 0.0246(18) 0.031(2) 0.0269(19) 0.0104(16) 0.0043(14) 0.0112(15) C63B 0.0212(19) 0.035(2) 0.055(3) 0.029(2) 0.006(2) 0.0031(19) C64B 0.036(2) 0.0289(19) 0.0297(19) 0.0033(15) -0.0070(16) 0.0044(16) F28B 0.0263(16) 0.061(3) 0.046(2) 0.0150(17) 0.0103(15) 0.0189(17) F29B 0.051(4) 0.025(3) 0.041(2) 0.014(2) 0.006(2) 0.018(3) F30B 0.0427(15) 0.0506(18) 0.0216(12) 0.0054(12) 0.0039(10) 0.0109(13) F31B 0.040(4) 0.075(6) 0.075(7) 0.046(5) 0.020(4) -0.009(3) F32B 0.016(2) 0.048(4) 0.053(3) 0.041(3) -0.007(2) -0.006(3) F33B 0.0445(16) 0.0267(15) 0.075(3) 0.0267(17) 0.0132(18) 0.0088(12) F34B 0.0295(16) 0.046(2) 0.065(2) 0.0141(18) -0.0186(13) -0.0117(15) F35B 0.0280(19) 0.038(3) 0.033(3) 0.009(2) -0.0013(18) -0.0105(18) F36B 0.055(4) 0.063(3) 0.036(2) 0.017(2) -0.013(2) 0.022(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _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 Tl1 N3 2.7417(17) . ? Tl1 N1 2.7481(18) . ? Tl1 P2 3.1391(9) . ? Tl1 P1 3.2481(9) . ? P1 C1 1.7925(18) . ? P1 C8 1.7980(19) . ? P1 C19 1.8265(18) . ? P2 C32 1.7986(19) . ? P2 C25 1.8019(19) . ? P2 C43 1.8269(19) . ? N1 C13 1.336(2) . ? N1 C9 1.355(2) . ? N3 C37 1.338(3) . ? N3 C33 1.348(3) . ? N2 C18 1.338(3) . ? N2 C14 1.351(2) . ? N4 C42 1.336(2) . ? N4 C38 1.352(3) . ? C1 C2 1.368(3) . ? C1 C14 1.477(3) . ? C2 C7 1.470(3) . ? C2 C3 1.511(2) . ? C3 C4 1.530(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.521(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.528(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.507(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.363(2) . ? C8 C9 1.462(2) . ? C9 C10 1.398(3) . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 C12 1.389(3) . ? C11 H11 0.9500 . ? C12 C13 1.382(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.396(3) . ? C15 C16 1.386(3) . ? C15 H15 0.9500 . ? C16 C17 1.381(3) . ? C16 H16 0.9500 . ? C17 C18 1.383(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.397(3) . ? C19 C24 1.400(2) . ? C20 C21 1.391(3) . ? C20 H20 0.9500 . ? C21 C22 1.388(3) . ? C21 H21 0.9500 . ? C22 C23 1.386(3) . ? C22 H22 0.9500 . ? C23 C24 1.388(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.367(3) . ? C25 C38 1.467(2) . ? C26 C31 1.471(3) . ? C26 C27 1.512(3) . ? C27 C28 1.529(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.517(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.531(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.510(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.364(3) . ? C32 C33 1.465(3) . ? C33 C34 1.400(3) . ? C34 C35 1.382(3) . ? C34 H34 0.9500 . ? C35 C36 1.382(3) . ? C35 H35 0.9500 . ? C36 C37 1.383(3) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.394(3) . ? C39 C40 1.390(3) . ? C39 H39 0.9500 . ? C40 C41 1.372(3) . ? C40 H40 0.9500 . ? C41 C42 1.388(3) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.382(3) . ? C43 C48 1.392(3) . ? C44 C45 1.392(3) . ? C44 H44 0.9500 . ? C45 C46 1.382(3) . ? C45 H45 0.9500 . ? C46 C47 1.373(3) . ? C46 H46 0.9500 . ? C47 C48 1.391(3) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? Al1 O1 1.7192(15) . ? Al1 O3 1.7195(14) . ? Al1 O4 1.7243(16) . ? Al1 O2 1.7263(14) . ? O1 C49 1.346(2) . ? O2 C50 1.346(2) . ? O3 C51 1.346(2) . ? O4 C52B 1.291(15) . ? O4 C52A 1.43(2) . ? C49 C54 1.552(3) . ? C49 C53 1.552(3) . ? C49 C55 1.554(3) . ? C50 C57 1.551(3) . ? C50 C56 1.552(3) . ? C50 C58 1.560(3) . ? C51 C60 1.547(3) . ? C51 C61 1.548(3) . ? C51 C59 1.555(3) . ? C53 F3 1.327(3) . ? C53 F2 1.334(3) . ? C53 F1 1.339(3) . ? C54 F5 1.332(3) . ? C54 F6 1.333(3) . ? C54 F4 1.339(3) . ? C55 F9 1.324(3) . ? C55 F8 1.337(3) . ? C55 F7 1.338(3) . ? C56 F12 1.327(2) . ? C56 F10 1.328(3) . ? C56 F11 1.344(2) . ? C57 F13 1.326(2) . ? C57 F15 1.330(2) . ? C57 F14 1.333(2) . ? C58 F17 1.328(2) . ? C58 F16 1.329(2) . ? C58 F18 1.330(2) . ? C59 F21 1.315(3) . ? C59 F20 1.334(3) . ? C59 F19 1.345(2) . ? C61 F27 1.319(3) . ? C61 F25 1.331(3) . ? C61 F26 1.339(3) . ? C60 F23 1.325(3) . ? C60 F24 1.327(2) . ? C60 F22 1.334(2) . ? C52A C63A 1.524(16) . ? C52A C62A 1.547(16) . ? C52A C64A 1.539(14) . ? C62A F28A 1.313(9) . ? C62A F30A 1.336(16) . ? C62A F29A 1.364(14) . ? C63A F33A 1.264(19) . ? C63A F31A 1.299(18) . ? C63A F32A 1.334(11) . ? C64A F36A 1.296(14) . ? C64A F35A 1.339(6) . ? C64A F34A 1.339(6) . ? C52B C64B 1.562(10) . ? C52B C63B 1.577(10) . ? C52B C62B 1.555(11) . ? C62B F30B 1.323(4) . ? C62B F28B 1.340(6) . ? C62B F29B 1.349(9) . ? C63B F31B 1.323(14) . ? C63B F33B 1.330(7) . ? C63B F32B 1.379(11) . ? C64B F36B 1.332(11) . ? C64B F34B 1.335(6) . ? C64B F35B 1.442(9) . ? 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 N3 Tl1 N1 85.39(5) . . ? N3 Tl1 P2 63.10(4) . . ? N1 Tl1 P2 74.77(4) . . ? N3 Tl1 P1 87.06(4) . . ? N1 Tl1 P1 60.84(4) . . ? P2 Tl1 P1 128.30(3) . . ? C1 P1 C8 91.71(8) . . ? C1 P1 C19 113.43(8) . . ? C8 P1 C19 104.98(8) . . ? C1 P1 Tl1 130.49(6) . . ? C8 P1 Tl1 87.50(6) . . ? C19 P1 Tl1 114.51(6) . . ? C32 P2 C25 91.07(9) . . ? C32 P2 C43 104.16(9) . . ? C25 P2 C43 109.14(9) . . ? C32 P2 Tl1 97.33(6) . . ? C25 P2 Tl1 143.69(6) . . ? C43 P2 Tl1 102.91(7) . . ? C13 N1 C9 118.47(16) . . ? C13 N1 Tl1 117.19(12) . . ? C9 N1 Tl1 120.38(12) . . ? C37 N3 C33 118.22(17) . . ? C37 N3 Tl1 113.15(13) . . ? C33 N3 Tl1 128.64(12) . . ? C18 N2 C14 117.56(16) . . ? C42 N4 C38 118.31(18) . . ? C2 C1 C14 128.14(16) . . ? C2 C1 P1 109.13(13) . . ? C14 C1 P1 121.62(13) . . ? C1 C2 C7 114.24(15) . . ? C1 C2 C3 125.80(17) . . ? C7 C2 C3 119.94(16) . . ? C2 C3 C4 113.24(16) . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 110.08(16) . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.2 . . ? C4 C5 C6 109.78(16) . . ? C4 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? C4 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? C7 C6 C5 112.77(16) . . ? C7 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? C7 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C2 113.49(16) . . ? C8 C7 C6 125.46(17) . . ? C2 C7 C6 121.04(15) . . ? C7 C8 C9 129.76(16) . . ? C7 C8 P1 109.87(13) . . ? C9 C8 P1 120.22(13) . . ? N1 C9 C10 121.08(16) . . ? N1 C9 C8 116.01(15) . . ? C10 C9 C8 122.78(16) . . ? C11 C10 C9 119.47(17) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 119.19(17) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 117.98(18) . . ? C13 C12 H12 121.0 . . ? C11 C12 H12 121.0 . . ? N1 C13 C12 123.80(17) . . ? N1 C13 H13 118.1 . . ? C12 C13 H13 118.1 . . ? N2 C14 C15 121.57(17) . . ? N2 C14 C1 115.45(16) . . ? C15 C14 C1 122.98(16) . . ? C16 C15 C14 119.62(18) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 118.85(18) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C16 C17 C18 118.12(18) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? N2 C18 C17 124.20(18) . . ? N2 C18 H18 117.9 . . ? C17 C18 H18 117.9 . . ? C20 C19 C24 119.38(17) . . ? C20 C19 P1 124.63(14) . . ? C24 C19 P1 115.97(14) . . ? C21 C20 C19 119.55(18) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C20 120.79(19) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C23 C22 C21 119.82(18) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 119.98(19) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.47(18) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C26 C25 C38 132.42(17) . . ? C26 C25 P2 110.29(14) . . ? C38 C25 P2 116.86(14) . . ? C25 C26 C31 113.64(16) . . ? C25 C26 C27 125.63(17) . . ? C31 C26 C27 120.64(16) . . ? C26 C27 C28 114.37(17) . . ? C26 C27 H27A 108.7 . . ? C28 C27 H27A 108.7 . . ? C26 C27 H27B 108.7 . . ? C28 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? C29 C28 C27 111.28(17) . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C28 C29 C30 109.50(17) . . ? C28 C29 H29A 109.8 . . ? C30 C29 H29A 109.8 . . ? C28 C29 H29B 109.8 . . ? C30 C29 H29B 109.8 . . ? H29A C29 H29B 108.2 . . ? C31 C30 C29 111.35(17) . . ? C31 C30 H30A 109.4 . . ? C29 C30 H30A 109.4 . . ? C31 C30 H30B 109.4 . . ? C29 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? C32 C31 C26 113.79(16) . . ? C32 C31 C30 125.55(17) . . ? C26 C31 C30 120.57(17) . . ? C31 C32 C33 128.60(17) . . ? C31 C32 P2 110.40(14) . . ? C33 C32 P2 120.85(14) . . ? N3 C33 C34 121.18(18) . . ? N3 C33 C32 116.70(16) . . ? C34 C33 C32 121.99(18) . . ? C35 C34 C33 119.5(2) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 119.37(19) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C35 C36 C37 117.8(2) . . ? C35 C36 H36 121.1 . . ? C37 C36 H36 121.1 . . ? N3 C37 C36 123.9(2) . . ? N3 C37 H37 118.0 . . ? C36 C37 H37 118.0 . . ? N4 C38 C39 121.24(17) . . ? N4 C38 C25 112.97(16) . . ? C39 C38 C25 125.79(18) . . ? C40 C39 C38 119.1(2) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C41 C40 C39 119.9(2) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 117.69(19) . . ? C40 C41 H41 121.2 . . ? C42 C41 H41 121.2 . . ? N4 C42 C41 123.8(2) . . ? N4 C42 H42 118.1 . . ? C41 C42 H42 118.1 . . ? C44 C43 C48 119.38(18) . . ? C44 C43 P2 122.16(15) . . ? C48 C43 P2 118.40(15) . . ? C43 C44 C45 120.2(2) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C46 C45 C44 120.0(2) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C47 C46 C45 120.2(2) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C46 C47 C48 120.1(2) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C47 C48 C43 120.1(2) . . ? C47 C48 H48 119.9 . . ? C43 C48 H48 119.9 . . ? O1 Al1 O3 107.45(7) . . ? O1 Al1 O4 108.06(7) . . ? O3 Al1 O4 113.69(8) . . ? O1 Al1 O2 114.31(8) . . ? O3 Al1 O2 105.83(7) . . ? O4 Al1 O2 107.66(7) . . ? C49 O1 Al1 149.21(14) . . ? C50 O2 Al1 146.80(12) . . ? C51 O3 Al1 149.05(12) . . ? C52B O4 Al1 150.8(4) . . ? C52A O4 Al1 143.0(6) . . ? O1 C49 C54 111.39(17) . . ? O1 C49 C53 110.09(18) . . ? C54 C49 C53 109.22(18) . . ? O1 C49 C55 107.89(17) . . ? C54 C49 C55 109.29(19) . . ? C53 C49 C55 108.93(18) . . ? O2 C50 C57 109.92(16) . . ? O2 C50 C56 107.10(15) . . ? C57 C50 C56 109.31(15) . . ? O2 C50 C58 112.65(15) . . ? C57 C50 C58 108.64(15) . . ? C56 C50 C58 109.17(16) . . ? O3 C51 C60 110.98(15) . . ? O3 C51 C61 111.07(16) . . ? C60 C51 C61 109.32(16) . . ? O3 C51 C59 106.83(15) . . ? C60 C51 C59 109.18(16) . . ? C61 C51 C59 109.42(17) . . ? F3 C53 F2 107.71(19) . . ? F3 C53 F1 106.5(2) . . ? F2 C53 F1 106.97(18) . . ? F3 C53 C49 111.21(18) . . ? F2 C53 C49 113.3(2) . . ? F1 C53 C49 110.82(18) . . ? F5 C54 F6 107.5(2) . . ? F5 C54 F4 107.6(2) . . ? F6 C54 F4 107.8(2) . . ? F5 C54 C49 110.7(2) . . ? F6 C54 C49 112.62(19) . . ? F4 C54 C49 110.45(19) . . ? F9 C55 F8 108.2(2) . . ? F9 C55 F7 107.7(2) . . ? F8 C55 F7 107.26(19) . . ? F9 C55 C49 110.63(18) . . ? F8 C55 C49 112.1(2) . . ? F7 C55 C49 110.9(2) . . ? F12 C56 F10 107.27(17) . . ? F12 C56 F11 108.09(17) . . ? F10 C56 F11 106.39(16) . . ? F12 C56 C50 111.08(16) . . ? F10 C56 C50 111.04(16) . . ? F11 C56 C50 112.71(17) . . ? F13 C57 F15 108.42(16) . . ? F13 C57 F14 107.09(16) . . ? F15 C57 F14 106.52(17) . . ? F13 C57 C50 113.06(17) . . ? F15 C57 C50 110.66(16) . . ? F14 C57 C50 110.81(16) . . ? F17 C58 F16 107.54(17) . . ? F17 C58 F18 107.18(16) . . ? F16 C58 F18 108.04(17) . . ? F17 C58 C50 111.22(16) . . ? F16 C58 C50 112.44(16) . . ? F18 C58 C50 110.21(16) . . ? F21 C59 F20 107.29(19) . . ? F21 C59 F19 107.6(2) . . ? F20 C59 F19 107.73(18) . . ? F21 C59 C51 111.77(17) . . ? F20 C59 C51 110.25(19) . . ? F19 C59 C51 111.97(17) . . ? F27 C61 F25 107.57(19) . . ? F27 C61 F26 106.8(2) . . ? F25 C61 F26 107.06(18) . . ? F27 C61 C51 111.24(16) . . ? F25 C61 C51 113.05(19) . . ? F26 C61 C51 110.78(18) . . ? F23 C60 F24 107.34(18) . . ? F23 C60 F22 107.50(17) . . ? F24 C60 F22 107.53(16) . . ? F23 C60 C51 111.07(16) . . ? F24 C60 C51 110.21(16) . . ? F22 C60 C51 112.96(17) . . ? O4 C52A C63A 107.7(11) . . ? O4 C52A C62A 104.0(10) . . ? C63A C52A C62A 110.7(12) . . ? O4 C52A C64A 112.9(13) . . ? C63A C52A C64A 111.2(11) . . ? C62A C52A C64A 110.0(11) . . ? F28A C62A F30A 106.8(8) . . ? F28A C62A F29A 107.6(7) . . ? F30A C62A F29A 110.5(9) . . ? F28A C62A C52A 111.0(10) . . ? F30A C62A C52A 110.8(10) . . ? F29A C62A C52A 110.0(8) . . ? F33A C63A F31A 105.0(11) . . ? F33A C63A F32A 111.4(10) . . ? F31A C63A F32A 104.5(10) . . ? F33A C63A C52A 114.1(13) . . ? F31A C63A C52A 111.0(11) . . ? F32A C63A C52A 110.3(9) . . ? F36A C64A F35A 115.6(8) . . ? F36A C64A F34A 109.1(7) . . ? F35A C64A F34A 107.1(4) . . ? F36A C64A C52A 104.5(10) . . ? F35A C64A C52A 110.6(7) . . ? F34A C64A C52A 109.9(9) . . ? O4 C52B C64B 109.0(8) . . ? O4 C52B C63B 112.7(8) . . ? C64B C52B C63B 107.2(7) . . ? O4 C52B C62B 112.4(7) . . ? C64B C52B C62B 107.8(8) . . ? C63B C52B C62B 107.5(8) . . ? F30B C62B F28B 107.6(3) . . ? F30B C62B F29B 107.4(6) . . ? F28B C62B F29B 107.6(6) . . ? F30B C62B C52B 110.8(5) . . ? F28B C62B C52B 114.3(6) . . ? F29B C62B C52B 108.8(7) . . ? F31B C63B F33B 104.3(8) . . ? F31B C63B F32B 110.8(8) . . ? F33B C63B F32B 106.4(5) . . ? F31B C63B C52B 116.6(8) . . ? F33B C63B C52B 111.1(6) . . ? F32B C63B C52B 107.2(7) . . ? F36B C64B F34B 108.0(5) . . ? F36B C64B F35B 110.1(6) . . ? F34B C64B F35B 105.4(4) . . ? F36B C64B C52B 108.9(5) . . ? F34B C64B C52B 114.4(6) . . ? F35B C64B C52B 110.0(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Tl1 P1 C1 43.51(9) . . . . ? N1 Tl1 P1 C1 129.87(9) . . . . ? P2 Tl1 P1 C1 95.35(8) . . . . ? N3 Tl1 P1 C8 -46.61(7) . . . . ? N1 Tl1 P1 C8 39.75(7) . . . . ? P2 Tl1 P1 C8 5.23(6) . . . . ? N3 Tl1 P1 C19 -151.95(7) . . . . ? N1 Tl1 P1 C19 -65.59(7) . . . . ? P2 Tl1 P1 C19 -100.11(6) . . . . ? N3 Tl1 P2 C32 24.28(7) . . . . ? N1 Tl1 P2 C32 -68.28(7) . . . . ? P1 Tl1 P2 C32 -37.43(7) . . . . ? N3 Tl1 P2 C25 126.22(11) . . . . ? N1 Tl1 P2 C25 33.65(11) . . . . ? P1 Tl1 P2 C25 64.51(11) . . . . ? N3 Tl1 P2 C43 -82.13(7) . . . . ? N1 Tl1 P2 C43 -174.70(7) . . . . ? P1 Tl1 P2 C43 -143.84(6) . . . . ? N3 Tl1 N1 C13 -111.45(14) . . . . ? P2 Tl1 N1 C13 -48.09(13) . . . . ? P1 Tl1 N1 C13 159.36(14) . . . . ? N3 Tl1 N1 C9 45.83(13) . . . . ? P2 Tl1 N1 C9 109.19(13) . . . . ? P1 Tl1 N1 C9 -43.37(12) . . . . ? N1 Tl1 N3 C37 -124.54(14) . . . . ? P2 Tl1 N3 C37 160.22(15) . . . . ? P1 Tl1 N3 C37 -63.57(14) . . . . ? N1 Tl1 N3 C33 55.27(15) . . . . ? P2 Tl1 N3 C33 -19.97(14) . . . . ? P1 Tl1 N3 C33 116.24(15) . . . . ? C8 P1 C1 C2 11.73(13) . . . . ? C19 P1 C1 C2 118.87(13) . . . . ? Tl1 P1 C1 C2 -76.45(14) . . . . ? C8 P1 C1 C14 -179.38(14) . . . . ? C19 P1 C1 C14 -72.24(16) . . . . ? Tl1 P1 C1 C14 92.44(15) . . . . ? C14 C1 C2 C7 -179.07(16) . . . . ? P1 C1 C2 C7 -11.11(19) . . . . ? C14 C1 C2 C3 -0.7(3) . . . . ? P1 C1 C2 C3 167.28(14) . . . . ? C1 C2 C3 C4 162.18(18) . . . . ? C7 C2 C3 C4 -19.5(2) . . . . ? C2 C3 C4 C5 49.5(2) . . . . ? C3 C4 C5 C6 -65.9(2) . . . . ? C4 C5 C6 C7 50.2(2) . . . . ? C1 C2 C7 C8 4.1(2) . . . . ? C3 C2 C7 C8 -174.42(16) . . . . ? C1 C2 C7 C6 -176.44(16) . . . . ? C3 C2 C7 C6 5.1(2) . . . . ? C5 C6 C7 C8 158.93(17) . . . . ? C5 C6 C7 C2 -20.5(2) . . . . ? C2 C7 C8 C9 -179.48(16) . . . . ? C6 C7 C8 C9 1.1(3) . . . . ? C2 C7 C8 P1 5.10(18) . . . . ? C6 C7 C8 P1 -174.35(14) . . . . ? C1 P1 C8 C7 -9.58(13) . . . . ? C19 P1 C8 C7 -124.39(13) . . . . ? Tl1 P1 C8 C7 120.89(12) . . . . ? C1 P1 C8 C9 174.50(14) . . . . ? C19 P1 C8 C9 59.68(15) . . . . ? Tl1 P1 C8 C9 -55.04(13) . . . . ? C13 N1 C9 C10 0.3(3) . . . . ? Tl1 N1 C9 C10 -156.69(13) . . . . ? C13 N1 C9 C8 -175.65(16) . . . . ? Tl1 N1 C9 C8 27.36(19) . . . . ? C7 C8 C9 N1 -144.50(18) . . . . ? P1 C8 C9 N1 30.5(2) . . . . ? C7 C8 C9 C10 39.6(3) . . . . ? P1 C8 C9 C10 -145.37(15) . . . . ? N1 C9 C10 C11 -0.2(3) . . . . ? C8 C9 C10 C11 175.47(16) . . . . ? C9 C10 C11 C12 -0.4(3) . . . . ? C10 C11 C12 C13 0.8(3) . . . . ? C9 N1 C13 C12 0.2(3) . . . . ? Tl1 N1 C13 C12 157.90(15) . . . . ? C11 C12 C13 N1 -0.7(3) . . . . ? C18 N2 C14 C15 -2.9(3) . . . . ? C18 N2 C14 C1 177.90(16) . . . . ? C2 C1 C14 N2 -145.23(18) . . . . ? P1 C1 C14 N2 48.2(2) . . . . ? C2 C1 C14 C15 35.5(3) . . . . ? P1 C1 C14 C15 -131.07(16) . . . . ? N2 C14 C15 C16 0.9(3) . . . . ? C1 C14 C15 C16 -179.95(17) . . . . ? C14 C15 C16 C17 1.4(3) . . . . ? C15 C16 C17 C18 -1.7(3) . . . . ? C14 N2 C18 C17 2.7(3) . . . . ? C16 C17 C18 N2 -0.4(3) . . . . ? C1 P1 C19 C20 -10.69(18) . . . . ? C8 P1 C19 C20 87.91(17) . . . . ? Tl1 P1 C19 C20 -177.93(13) . . . . ? C1 P1 C19 C24 168.13(13) . . . . ? C8 P1 C19 C24 -93.26(15) . . . . ? Tl1 P1 C19 C24 0.89(16) . . . . ? C24 C19 C20 C21 0.7(3) . . . . ? P1 C19 C20 C21 179.44(14) . . . . ? C19 C20 C21 C22 -0.7(3) . . . . ? C20 C21 C22 C23 0.5(3) . . . . ? C21 C22 C23 C24 -0.3(3) . . . . ? C22 C23 C24 C19 0.3(3) . . . . ? C20 C19 C24 C23 -0.5(3) . . . . ? P1 C19 C24 C23 -179.38(15) . . . . ? C32 P2 C25 C26 7.71(14) . . . . ? C43 P2 C25 C26 113.11(14) . . . . ? Tl1 P2 C25 C26 -96.23(14) . . . . ? C32 P2 C25 C38 -178.86(14) . . . . ? C43 P2 C25 C38 -73.47(15) . . . . ? Tl1 P2 C25 C38 77.20(17) . . . . ? C38 C25 C26 C31 -177.44(18) . . . . ? P2 C25 C26 C31 -5.39(19) . . . . ? C38 C25 C26 C27 -0.8(3) . . . . ? P2 C25 C26 C27 171.22(14) . . . . ? C25 C26 C27 C28 175.88(17) . . . . ? C31 C26 C27 C28 -7.7(2) . . . . ? C26 C27 C28 C29 40.4(2) . . . . ? C27 C28 C29 C30 -65.2(2) . . . . ? C28 C29 C30 C31 55.1(2) . . . . ? C25 C26 C31 C32 -0.9(2) . . . . ? C27 C26 C31 C32 -177.73(16) . . . . ? C25 C26 C31 C30 175.87(17) . . . . ? C27 C26 C31 C30 -0.9(3) . . . . ? C29 C30 C31 C32 153.55(19) . . . . ? C29 C30 C31 C26 -22.8(2) . . . . ? C26 C31 C32 C33 -177.61(17) . . . . ? C30 C31 C32 C33 5.8(3) . . . . ? C26 C31 C32 P2 6.8(2) . . . . ? C30 C31 C32 P2 -169.81(15) . . . . ? C25 P2 C32 C31 -8.24(14) . . . . ? C43 P2 C32 C31 -118.30(14) . . . . ? Tl1 P2 C32 C31 136.35(12) . . . . ? C25 P2 C32 C33 175.77(15) . . . . ? C43 P2 C32 C33 65.71(16) . . . . ? Tl1 P2 C32 C33 -39.64(15) . . . . ? C37 N3 C33 C34 -0.6(3) . . . . ? Tl1 N3 C33 C34 179.57(14) . . . . ? C37 N3 C33 C32 -176.47(17) . . . . ? Tl1 N3 C33 C32 3.7(2) . . . . ? C31 C32 C33 N3 -144.85(19) . . . . ? P2 C32 C33 N3 30.3(2) . . . . ? C31 C32 C33 C34 39.4(3) . . . . ? P2 C32 C33 C34 -145.46(17) . . . . ? N3 C33 C34 C35 0.5(3) . . . . ? C32 C33 C34 C35 176.15(19) . . . . ? C33 C34 C35 C36 0.0(3) . . . . ? C34 C35 C36 C37 -0.5(3) . . . . ? C33 N3 C37 C36 0.2(3) . . . . ? Tl1 N3 C37 C36 180.00(18) . . . . ? C35 C36 C37 N3 0.4(4) . . . . ? C42 N4 C38 C39 -1.4(3) . . . . ? C42 N4 C38 C25 177.74(16) . . . . ? C26 C25 C38 N4 171.00(18) . . . . ? P2 C25 C38 N4 -0.6(2) . . . . ? C26 C25 C38 C39 -9.9(3) . . . . ? P2 C25 C38 C39 178.43(16) . . . . ? N4 C38 C39 C40 1.4(3) . . . . ? C25 C38 C39 C40 -177.62(19) . . . . ? C38 C39 C40 C41 -0.2(3) . . . . ? C39 C40 C41 C42 -0.8(3) . . . . ? C38 N4 C42 C41 0.3(3) . . . . ? C40 C41 C42 N4 0.8(3) . . . . ? C32 P2 C43 C44 36.04(18) . . . . ? C25 P2 C43 C44 -60.16(18) . . . . ? Tl1 P2 C43 C44 137.15(15) . . . . ? C32 P2 C43 C48 -141.07(15) . . . . ? C25 P2 C43 C48 122.73(16) . . . . ? Tl1 P2 C43 C48 -39.95(16) . . . . ? C48 C43 C44 C45 -0.1(3) . . . . ? P2 C43 C44 C45 -177.16(16) . . . . ? C43 C44 C45 C46 0.8(3) . . . . ? C44 C45 C46 C47 -0.8(3) . . . . ? C45 C46 C47 C48 0.1(3) . . . . ? C46 C47 C48 C43 0.6(3) . . . . ? C44 C43 C48 C47 -0.6(3) . . . . ? P2 C43 C48 C47 176.57(16) . . . . ? O3 Al1 O1 C49 -173.3(3) . . . . ? O4 Al1 O1 C49 -50.2(3) . . . . ? O2 Al1 O1 C49 69.6(3) . . . . ? O1 Al1 O2 C50 78.2(2) . . . . ? O3 Al1 O2 C50 -39.9(2) . . . . ? O4 Al1 O2 C50 -161.8(2) . . . . ? O1 Al1 O3 C51 39.1(3) . . . . ? O4 Al1 O3 C51 -80.4(3) . . . . ? O2 Al1 O3 C51 161.6(2) . . . . ? O1 Al1 O4 C52B 169.0(9) . . . . ? O3 Al1 O4 C52B -71.8(9) . . . . ? O2 Al1 O4 C52B 45.1(9) . . . . ? O1 Al1 O4 C52A 156.7(10) . . . . ? O3 Al1 O4 C52A -84.1(10) . . . . ? O2 Al1 O4 C52A 32.8(10) . . . . ? Al1 O1 C49 C54 -43.0(4) . . . . ? Al1 O1 C49 C53 78.3(3) . . . . ? Al1 O1 C49 C55 -162.9(2) . . . . ? Al1 O2 C50 C57 97.3(2) . . . . ? Al1 O2 C50 C56 -144.0(2) . . . . ? Al1 O2 C50 C58 -24.0(3) . . . . ? Al1 O3 C51 C60 52.0(3) . . . . ? Al1 O3 C51 C61 -69.8(3) . . . . ? Al1 O3 C51 C59 170.9(2) . . . . ? O1 C49 C53 F3 38.2(3) . . . . ? C54 C49 C53 F3 160.8(2) . . . . ? C55 C49 C53 F3 -79.9(2) . . . . ? O1 C49 C53 F2 159.64(18) . . . . ? C54 C49 C53 F2 -77.8(2) . . . . ? C55 C49 C53 F2 41.5(2) . . . . ? O1 C49 C53 F1 -80.1(2) . . . . ? C54 C49 C53 F1 42.4(2) . . . . ? C55 C49 C53 F1 161.74(19) . . . . ? O1 C49 C54 F5 -75.2(2) . . . . ? C53 C49 C54 F5 162.96(19) . . . . ? C55 C49 C54 F5 43.9(2) . . . . ? O1 C49 C54 F6 164.4(2) . . . . ? C53 C49 C54 F6 42.6(3) . . . . ? C55 C49 C54 F6 -76.5(3) . . . . ? O1 C49 C54 F4 43.9(3) . . . . ? C53 C49 C54 F4 -78.0(2) . . . . ? C55 C49 C54 F4 162.97(19) . . . . ? O1 C49 C55 F9 42.7(3) . . . . ? C54 C49 C55 F9 -78.5(2) . . . . ? C53 C49 C55 F9 162.22(19) . . . . ? O1 C49 C55 F8 163.54(19) . . . . ? C54 C49 C55 F8 42.3(3) . . . . ? C53 C49 C55 F8 -77.0(2) . . . . ? O1 C49 C55 F7 -76.6(2) . . . . ? C54 C49 C55 F7 162.11(18) . . . . ? C53 C49 C55 F7 42.9(2) . . . . ? O2 C50 C56 F12 74.5(2) . . . . ? C57 C50 C56 F12 -166.46(17) . . . . ? C58 C50 C56 F12 -47.8(2) . . . . ? O2 C50 C56 F10 -44.8(2) . . . . ? C57 C50 C56 F10 74.3(2) . . . . ? C58 C50 C56 F10 -167.03(15) . . . . ? O2 C50 C56 F11 -164.03(17) . . . . ? C57 C50 C56 F11 -45.0(2) . . . . ? C58 C50 C56 F11 73.7(2) . . . . ? O2 C50 C57 F13 -169.23(15) . . . . ? C56 C50 C57 F13 73.5(2) . . . . ? C58 C50 C57 F13 -45.5(2) . . . . ? O2 C50 C57 F15 -47.4(2) . . . . ? C56 C50 C57 F15 -164.67(16) . . . . ? C58 C50 C57 F15 76.3(2) . . . . ? O2 C50 C57 F14 70.5(2) . . . . ? C56 C50 C57 F14 -46.7(2) . . . . ? C58 C50 C57 F14 -165.78(15) . . . . ? O2 C50 C58 F17 79.81(19) . . . . ? C57 C50 C58 F17 -42.2(2) . . . . ? C56 C50 C58 F17 -161.35(15) . . . . ? O2 C50 C58 F16 -159.52(16) . . . . ? C57 C50 C58 F16 78.5(2) . . . . ? C56 C50 C58 F16 -40.7(2) . . . . ? O2 C50 C58 F18 -38.9(2) . . . . ? C57 C50 C58 F18 -160.94(16) . . . . ? C56 C50 C58 F18 79.93(19) . . . . ? O3 C51 C59 F21 -45.6(2) . . . . ? C60 C51 C59 F21 74.4(2) . . . . ? C61 C51 C59 F21 -165.95(17) . . . . ? O3 C51 C59 F20 73.6(2) . . . . ? C60 C51 C59 F20 -166.32(17) . . . . ? C61 C51 C59 F20 -46.7(2) . . . . ? O3 C51 C59 F19 -166.48(18) . . . . ? C60 C51 C59 F19 -46.4(2) . . . . ? C61 C51 C59 F19 73.2(2) . . . . ? O3 C51 C61 F27 -39.2(2) . . . . ? C60 C51 C61 F27 -162.02(18) . . . . ? C59 C51 C61 F27 78.5(2) . . . . ? O3 C51 C61 F25 -160.39(17) . . . . ? C60 C51 C61 F25 76.8(2) . . . . ? C59 C51 C61 F25 -42.7(2) . . . . ? O3 C51 C61 F26 79.4(2) . . . . ? C60 C51 C61 F26 -43.4(2) . . . . ? C59 C51 C61 F26 -162.87(16) . . . . ? O3 C51 C60 F23 71.6(2) . . . . ? C61 C51 C60 F23 -165.56(17) . . . . ? C59 C51 C60 F23 -45.9(2) . . . . ? O3 C51 C60 F24 -47.2(2) . . . . ? C61 C51 C60 F24 75.6(2) . . . . ? C59 C51 C60 F24 -164.72(17) . . . . ? O3 C51 C60 F22 -167.54(16) . . . . ? C61 C51 C60 F22 -44.7(2) . . . . ? C59 C51 C60 F22 75.0(2) . . . . ? C52B O4 C52A C63A -83(6) . . . . ? Al1 O4 C52A C63A 61.7(14) . . . . ? C52B O4 C52A C62A 35(5) . . . . ? Al1 O4 C52A C62A 179.2(3) . . . . ? C52B O4 C52A C64A 154(6) . . . . ? Al1 O4 C52A C64A -61.5(14) . . . . ? O4 C52A C62A F28A -161.7(7) . . . . ? C63A C52A C62A F28A -46.2(13) . . . . ? C64A C52A C62A F28A 77.1(13) . . . . ? O4 C52A C62A F30A -43.1(12) . . . . ? C63A C52A C62A F30A 72.3(15) . . . . ? C64A C52A C62A F30A -164.3(12) . . . . ? O4 C52A C62A F29A 79.3(10) . . . . ? C63A C52A C62A F29A -165.2(10) . . . . ? C64A C52A C62A F29A -41.8(15) . . . . ? O4 C52A C63A F33A -55.6(13) . . . . ? C62A C52A C63A F33A -168.7(12) . . . . ? C64A C52A C63A F33A 68.6(17) . . . . ? O4 C52A C63A F31A -174.0(11) . . . . ? C62A C52A C63A F31A 72.9(15) . . . . ? C64A C52A C63A F31A -49.8(17) . . . . ? O4 C52A C63A F32A 70.7(11) . . . . ? C62A C52A C63A F32A -42.4(14) . . . . ? C64A C52A C63A F32A -165.1(10) . . . . ? O4 C52A C64A F36A -42.1(12) . . . . ? C63A C52A C64A F36A -163.3(12) . . . . ? C62A C52A C64A F36A 73.6(15) . . . . ? O4 C52A C64A F35A 82.9(10) . . . . ? C63A C52A C64A F35A -38.3(16) . . . . ? C62A C52A C64A F35A -161.4(9) . . . . ? O4 C52A C64A F34A -159.1(8) . . . . ? C63A C52A C64A F34A 79.7(13) . . . . ? C62A C52A C64A F34A -43.4(14) . . . . ? C52A O4 C52B C64B -65(5) . . . . ? Al1 O4 C52B C64B -111.0(8) . . . . ? C52A O4 C52B C63B 54(5) . . . . ? Al1 O4 C52B C63B 7.9(13) . . . . ? C52A O4 C52B C62B 175(6) . . . . ? Al1 O4 C52B C62B 129.5(6) . . . . ? O4 C52B C62B F30B -76.5(8) . . . . ? C64B C52B C62B F30B 163.3(6) . . . . ? C63B C52B C62B F30B 48.0(9) . . . . ? O4 C52B C62B F28B 161.7(6) . . . . ? C64B C52B C62B F28B 41.5(9) . . . . ? C63B C52B C62B F28B -73.8(8) . . . . ? O4 C52B C62B F29B 41.3(9) . . . . ? C64B C52B C62B F29B -78.9(9) . . . . ? C63B C52B C62B F29B 165.8(7) . . . . ? O4 C52B C63B F31B 164.4(9) . . . . ? C64B C52B C63B F31B -75.6(11) . . . . ? C62B C52B C63B F31B 40.1(11) . . . . ? O4 C52B C63B F33B -76.3(7) . . . . ? C64B C52B C63B F33B 43.6(10) . . . . ? C62B C52B C63B F33B 159.3(5) . . . . ? O4 C52B C63B F32B 39.5(9) . . . . ? C64B C52B C63B F32B 159.5(8) . . . . ? C62B C52B C63B F32B -84.8(9) . . . . ? O4 C52B C64B F36B -75.0(8) . . . . ? C63B C52B C64B F36B 162.7(7) . . . . ? C62B C52B C64B F36B 47.3(10) . . . . ? O4 C52B C64B F34B 164.1(5) . . . . ? C63B C52B C64B F34B 41.8(9) . . . . ? C62B C52B C64B F34B -73.6(8) . . . . ? O4 C52B C64B F35B 45.7(7) . . . . ? C63B C52B C64B F35B -76.6(9) . . . . ? C62B C52B C64B F35B 168.0(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C12 H12 F14 0.9500 2.4300 3.193(3) 138.00 2_556 yes C15 H15 F25 0.9500 2.5200 3.256(3) 134.00 2_666 yes C27 H27B F14 0.9900 2.4600 3.408(3) 161.00 2_556 yes C41 H41 F16 0.9500 2.5400 3.056(3) 115.00 2_656 yes # start Validation Reply Form _vrf_PLAT308_sw30c ; PROBLEM: Single Bonded Metal Atom (Unusual !) ........... Tl1 RESPONSE: The rather long coordinative Tl-N, Tl-P and Tl-Ph bonds are not taken into account by the checkCIF routine. ; # end Validation Reply Form #===END # Attachment 'sw139.cif' # CIF-file generated for sw139 Welsch/Scheer R = 0.05 #============================================================================== data_sw139 _database_code_depnum_ccdc_archive 'CCDC 713904' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 Al F36 O4, 2(C24 H21 N2 P), Tl, 2(C7 H8)' _chemical_formula_structural ? _chemical_formula_sum 'C78 H58 Al F36 N4 O4 P2 Tl' _chemical_formula_iupac ? _chemical_formula_weight 2092.58 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Tl Tl -4.1627 8.0900 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 9.6229(1) _cell_length_b 23.3032(2) _cell_length_c 36.1442(2) _cell_angle_alpha 90 _cell_angle_beta 91.045(1) _cell_angle_gamma 90 _cell_volume 8103.79(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 28634 _cell_measurement_theta_min 3.0919 _cell_measurement_theta_max 66.4820 _cell_special_details ; ; _exptl_crystal_description parallelepiped _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.289 _exptl_crystal_size_mid 0.239 _exptl_crystal_size_min 0.187 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 4136 _exptl_absorpt_coefficient_mu 5.541 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_T_min 0.286 _exptl_absorpt_correction_T_max 0.355 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -44.00 12.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -11.6137 71.0000 192.0000 0.0000 0.0000 56 #__ type_ start__ end____ width___ exp.time_ 2 omega -13.00 43.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 11.6137 -77.0000 90.0000 0.0000 0.0000 56 #__ type_ start__ end____ width___ exp.time_ 3 omega -86.00 -33.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -11.6137 -45.0000 210.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 4 omega 11.00 61.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -11.6137 45.0000 120.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 5 omega -166.00 -58.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 -71.0000 242.0000 0.0000 0.0000 108 #__ type_ start__ end____ width___ exp.time_ 6 omega -115.00 -25.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 109.0000 0.0000 0.0000 0.0000 90 #__ type_ start__ end____ width___ exp.time_ 7 omega -114.00 -64.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 -71.0000 347.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 8 omega -167.00 -128.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 -109.0000 179.0000 0.0000 0.0000 39 #__ type_ start__ end____ width___ exp.time_ 9 omega 115.00 171.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 77.0000 210.0000 0.0000 0.0000 56 #__ type_ start__ end____ width___ exp.time_ 10 omega 115.00 164.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 45.0000 0.0000 0.0000 0.0000 49 #__ type_ start__ end____ width___ exp.time_ 11 omega 92.00 172.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 109.0000 275.0000 0.0000 0.0000 80 #__ type_ start__ end____ width___ exp.time_ 12 omega 15.00 82.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 -109.0000 359.0000 0.0000 0.0000 67 #__ type_ start__ end____ width___ exp.time_ 13 omega 79.00 119.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 -45.0000 90.0000 0.0000 0.0000 40 #__ type_ start__ end____ width___ exp.time_ 14 omega 77.00 126.00 1.0000 11.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 -77.0000 150.0000 0.0000 0.0000 49 ; _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 33548 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 62.38 _diffrn_reflns_theta_full 62.38 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 12511 # number of observed reflections (> n sig(I)) _reflns_number_gt 11802 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXH-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material ; PLATON (Spek, 2003) and SHELXH-97 (Sheldrick, 1997) ; #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0581P)^2^+58.4966P] 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 refU _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 12511 _refine_ls_number_parameters 1566 _refine_ls_number_restraints 885 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 3.228 _refine_diff_density_min -1.491 _refine_diff_density_rms 0.114 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Tl1 Tl -0.07175(2) 0.151738(9) 0.378326(6) 0.02277(9) Uani 1 1 d . . . P1 P -0.06806(15) 0.01441(6) 0.38422(4) 0.0207(3) Uani 1 1 d . . . P2 P 0.21045(14) 0.21474(6) 0.39719(4) 0.0197(3) Uani 1 1 d . . . N1 N 0.0740(6) 0.0893(2) 0.32545(14) 0.0297(12) Uani 1 1 d . . . N2 N -0.2128(5) -0.0134(2) 0.45433(14) 0.0274(11) Uani 1 1 d . . . N3 N 0.0346(5) 0.1505(2) 0.45192(14) 0.0246(11) Uani 1 1 d . . . N4 N 0.3125(5) 0.2527(2) 0.32528(15) 0.0318(12) Uani 1 1 d . . . C1 C -0.2253(6) -0.0269(2) 0.38939(17) 0.0223(12) Uani 1 1 d . . . C2 C -0.2945(6) -0.0305(2) 0.35632(18) 0.0268(13) Uani 1 1 d . . . C3 C -0.4412(7) -0.0523(3) 0.3505(2) 0.0330(15) Uani 1 1 d . . . H3A H -0.4957 -0.0442 0.3729 0.040 Uiso 1 1 calc R . . H3B H -0.4391 -0.0944 0.3469 0.040 Uiso 1 1 calc R . . C4 C -0.5129(8) -0.0243(4) 0.3170(2) 0.050(2) Uani 1 1 d . . . H4A H -0.6052 -0.0421 0.3127 0.060 Uiso 1 1 calc R . . H4B H -0.5267 0.0171 0.3218 0.060 Uiso 1 1 calc R . . C5 C -0.4254(8) -0.0320(4) 0.2831(2) 0.053(2) Uani 1 1 d . . . H5A H -0.4765 -0.0169 0.2612 0.064 Uiso 1 1 calc R . . H5B H -0.4086 -0.0734 0.2791 0.064 Uiso 1 1 calc R . . C6 C -0.2862(9) -0.0010(3) 0.2872(2) 0.0487(19) Uani 1 1 d . . . H6A H -0.2223 -0.0161 0.2683 0.058 Uiso 1 1 calc R . . H6B H -0.3008 0.0403 0.2820 0.058 Uiso 1 1 calc R . . C7 C -0.2177(7) -0.0072(3) 0.32505(17) 0.0289(14) Uani 1 1 d . . . C8 C -0.0900(6) 0.0139(2) 0.33464(16) 0.0253(13) Uani 1 1 d . . . C9 C 0.0145(6) 0.0416(2) 0.31146(16) 0.0259(13) Uani 1 1 d . . . C10 C 0.0544(8) 0.0187(3) 0.27767(18) 0.0360(15) Uani 1 1 d . . . H10 H 0.0125 -0.0156 0.2685 0.043 Uiso 1 1 calc R . . C11 C 0.1551(8) 0.0462(3) 0.25759(19) 0.0423(17) Uani 1 1 d . . . H11 H 0.1833 0.0314 0.2344 0.051 Uiso 1 1 calc R . . C12 C 0.2145(8) 0.0959(3) 0.2720(2) 0.0400(16) Uani 1 1 d . . . H12 H 0.2839 0.1157 0.2587 0.048 Uiso 1 1 calc R . . C13 C 0.1720(7) 0.1159(3) 0.30545(19) 0.0344(15) Uani 1 1 d . . . H13 H 0.2132 0.1500 0.3150 0.041 Uiso 1 1 calc R . . C14 C -0.2650(6) -0.0453(2) 0.42634(17) 0.0232(12) Uani 1 1 d . . . C15 C -0.3458(6) -0.0936(3) 0.43284(19) 0.0284(13) Uani 1 1 d . . . H15 H -0.3779 -0.1167 0.4128 0.034 Uiso 1 1 calc R . . C16 C -0.3791(6) -0.1078(3) 0.4688(2) 0.0340(15) Uani 1 1 d . . . H16 H -0.4354 -0.1404 0.4736 0.041 Uiso 1 1 calc R . . C17 C -0.3297(7) -0.0744(3) 0.49754(19) 0.0351(15) Uani 1 1 d . . . H17 H -0.3525 -0.0826 0.5224 0.042 Uiso 1 1 calc R . . C18 C -0.2453(7) -0.0281(3) 0.48881(19) 0.0335(15) Uani 1 1 d . . . H18 H -0.2086 -0.0055 0.5086 0.040 Uiso 1 1 calc R . . C19 C 0.0738(6) -0.0354(2) 0.39432(16) 0.0221(12) Uani 1 1 d . . . C20 C 0.0683(6) -0.0924(3) 0.38260(17) 0.0274(13) Uani 1 1 d . . . H20 H -0.0091 -0.1058 0.3684 0.033 Uiso 1 1 calc R . . C21 C 0.1762(7) -0.1294(3) 0.3918(2) 0.0360(16) Uani 1 1 d . . . H21 H 0.1724 -0.1683 0.3838 0.043 Uiso 1 1 calc R . . C22 C 0.2891(7) -0.1103(3) 0.4123(2) 0.0395(17) Uani 1 1 d . . . H22 H 0.3622 -0.1360 0.4187 0.047 Uiso 1 1 calc R . . C23 C 0.2960(6) -0.0534(3) 0.4237(2) 0.0353(15) Uani 1 1 d . . . H23 H 0.3740 -0.0402 0.4378 0.042 Uiso 1 1 calc R . . C24 C 0.1887(6) -0.0160(3) 0.41458(17) 0.0263(13) Uani 1 1 d . . . H24 H 0.1937 0.0230 0.4222 0.032 Uiso 1 1 calc R . . C25 C 0.2669(6) 0.2865(2) 0.38554(17) 0.0229(12) Uani 1 1 d . . . C26 C 0.2213(6) 0.3246(2) 0.41146(17) 0.0253(13) Uani 1 1 d . . . C27 C 0.2263(8) 0.3893(3) 0.4076(2) 0.0428(18) Uani 1 1 d . . . H27A H 0.1702 0.4008 0.3856 0.051 Uiso 1 1 calc R . . H27B H 0.3235 0.4012 0.4034 0.051 Uiso 1 1 calc R . . C28 C 0.1726(11) 0.4208(3) 0.4413(3) 0.066(3) Uani 1 1 d . . . H28A H 0.2507 0.4255 0.4592 0.079 Uiso 1 1 calc R . . H28B H 0.1429 0.4597 0.4334 0.079 Uiso 1 1 calc R . . C29 C 0.0603(11) 0.3945(3) 0.4599(3) 0.060(2) Uani 1 1 d . . . H29A H -0.0218 0.3934 0.4430 0.072 Uiso 1 1 calc R . . H29B H 0.0360 0.4185 0.4815 0.072 Uiso 1 1 calc R . . C30 C 0.0920(7) 0.3340(3) 0.47323(18) 0.0302(14) Uani 1 1 d . . . H30A H 0.1572 0.3357 0.4947 0.036 Uiso 1 1 calc R . . H30B H 0.0051 0.3157 0.4815 0.036 Uiso 1 1 calc R . . C31 C 0.1551(6) 0.2978(2) 0.44318(17) 0.0234(12) Uani 1 1 d . . . C32 C 0.1497(6) 0.2395(2) 0.44126(15) 0.0211(12) Uani 1 1 d . . . C33 C 0.0891(6) 0.1986(2) 0.46740(16) 0.0213(12) Uani 1 1 d . . . C34 C 0.0910(6) 0.2072(3) 0.50541(17) 0.0264(13) Uani 1 1 d . . . H34 H 0.1333 0.2406 0.5157 0.032 Uiso 1 1 calc R . . C35 C 0.0309(7) 0.1669(3) 0.52814(18) 0.0336(15) Uani 1 1 d . . . H35 H 0.0303 0.1726 0.5542 0.040 Uiso 1 1 calc R . . C36 C -0.0284(6) 0.1182(3) 0.51252(18) 0.0321(14) Uani 1 1 d . . . H36 H -0.0714 0.0900 0.5275 0.039 Uiso 1 1 calc R . . C37 C -0.0232(6) 0.1117(3) 0.47457(17) 0.0272(13) Uani 1 1 d . . . H37 H -0.0624 0.0780 0.4639 0.033 Uiso 1 1 calc R . . C38 C 0.3306(6) 0.2957(3) 0.34972(18) 0.0268(13) Uani 1 1 d . . . C39 C 0.4108(8) 0.3439(3) 0.3409(2) 0.0423(18) Uani 1 1 d . . . H39 H 0.4261 0.3733 0.3587 0.051 Uiso 1 1 calc R . . C40 C 0.4673(9) 0.3483(3) 0.3063(3) 0.056(2) Uani 1 1 d . . . H40 H 0.5210 0.3809 0.2999 0.067 Uiso 1 1 calc R . . C41 C 0.4452(9) 0.3051(4) 0.2811(2) 0.055(2) Uani 1 1 d . . . H41 H 0.4818 0.3074 0.2569 0.066 Uiso 1 1 calc R . . C42 C 0.3692(8) 0.2586(4) 0.2918(2) 0.0442(18) Uani 1 1 d . . . H42 H 0.3555 0.2285 0.2744 0.053 Uiso 1 1 calc R . . C43 C 0.3688(6) 0.1743(2) 0.40921(16) 0.0219(12) Uani 1 1 d . . . C44 C 0.4658(6) 0.1951(3) 0.43441(19) 0.0310(14) Uani 1 1 d . . . H44 H 0.4517 0.2314 0.4457 0.037 Uiso 1 1 calc R . . C45 C 0.5836(7) 0.1635(3) 0.4435(2) 0.0356(15) Uani 1 1 d . . . H45 H 0.6499 0.1785 0.4607 0.043 Uiso 1 1 calc R . . C46 C 0.6052(7) 0.1103(3) 0.42758(19) 0.0333(15) Uani 1 1 d . . . H46 H 0.6857 0.0885 0.4338 0.040 Uiso 1 1 calc R . . C47 C 0.5078(7) 0.0895(3) 0.4026(2) 0.0370(16) Uani 1 1 d . . . H47 H 0.5218 0.0530 0.3916 0.044 Uiso 1 1 calc R . . C48 C 0.3900(7) 0.1208(3) 0.39313(18) 0.0295(14) Uani 1 1 d . . . H48 H 0.3241 0.1058 0.3758 0.035 Uiso 1 1 calc R . . C49 C -0.2687(11) 0.3034(4) 0.4004(3) 0.074(3) Uani 1 1 d U . . H49A H -0.2219 0.3407 0.4022 0.110 Uiso 1 1 calc R . . H49B H -0.2381 0.2790 0.4211 0.110 Uiso 1 1 calc R . . H49C H -0.3695 0.3091 0.4015 0.110 Uiso 1 1 calc R . . C50 C -0.2332(8) 0.2752(3) 0.3646(3) 0.0527(19) Uani 1 1 d U . . C51 C -0.1074(9) 0.2851(4) 0.3488(3) 0.069(2) Uani 1 1 d U . . H51 H -0.0439 0.3110 0.3603 0.083 Uiso 1 1 calc R . . C52 C -0.0722(10) 0.2589(5) 0.3173(3) 0.081(3) Uani 1 1 d U . . H52 H 0.0158 0.2672 0.3071 0.097 Uiso 1 1 calc R . . C53 C -0.1594(11) 0.2199(6) 0.2989(3) 0.081(3) Uani 1 1 d U . . H53 H -0.1321 0.2015 0.2767 0.098 Uiso 1 1 calc R . . C54 C -0.2877(9) 0.2093(4) 0.3144(3) 0.064(2) Uani 1 1 d U . . H54 H -0.3512 0.1835 0.3027 0.077 Uiso 1 1 calc R . . C55 C -0.3235(7) 0.2367(3) 0.3475(2) 0.0482(18) Uani 1 1 d U . . H55 H -0.4107 0.2288 0.3583 0.058 Uiso 1 1 calc R . . C56 C -0.2639(13) 0.3443(6) 0.2174(4) 0.060(4) Uani 0.666(18) 1 d PU A 1 H56A H -0.2529 0.3551 0.1914 0.090 Uiso 0.666(18) 1 calc PR A 1 H56B H -0.3440 0.3645 0.2275 0.090 Uiso 0.666(18) 1 calc PR A 1 H56C H -0.2788 0.3028 0.2191 0.090 Uiso 0.666(18) 1 calc PR A 1 C57 C -0.131(4) 0.361(3) 0.2397(13) 0.039(5) Uani 0.666(18) 1 d PU A 1 C58 C -0.1423(18) 0.3920(7) 0.2716(6) 0.043(4) Uani 0.666(18) 1 d PU A 1 H58 H -0.2309 0.4047 0.2795 0.052 Uiso 0.666(18) 1 calc PR A 1 C59 C -0.025(2) 0.4050(14) 0.2923(11) 0.045(6) Uani 0.666(18) 1 d PU A 1 H59 H -0.0332 0.4235 0.3156 0.054 Uiso 0.666(18) 1 calc PR A 1 C60 C 0.103(4) 0.3916(13) 0.2795(9) 0.041(6) Uani 0.666(18) 1 d P A 1 H60 H 0.1849 0.4019 0.2931 0.049 Uiso 0.666(18) 1 calc PR A 1 C61 C 0.1116(19) 0.3616(7) 0.2452(5) 0.047(4) Uani 0.666(18) 1 d PU A 1 H61 H 0.2005 0.3522 0.2359 0.056 Uiso 0.666(18) 1 calc PR A 1 C62 C -0.004(2) 0.3460(8) 0.2254(6) 0.046(4) Uani 0.666(18) 1 d PU A 1 H62 H 0.0023 0.3258 0.2026 0.055 Uiso 0.666(18) 1 calc PR A 1 C56B C -0.144(4) 0.3185(12) 0.2024(8) 0.071(10) Uani 0.334(18) 1 d P A 2 H56D H -0.0728 0.3189 0.1834 0.107 Uiso 0.334(18) 1 calc PR A 2 H56E H -0.2314 0.3335 0.1920 0.107 Uiso 0.334(18) 1 calc PR A 2 H56F H -0.1580 0.2791 0.2110 0.107 Uiso 0.334(18) 1 calc PR A 2 C57B C -0.099(4) 0.354(5) 0.233(2) 0.05(2) Uani 0.334(18) 1 d PD A 2 C58B C -0.192(4) 0.3808(15) 0.2568(10) 0.040(8) Uani 0.334(18) 1 d PD A 2 H58B H -0.2882 0.3772 0.2515 0.048 Uiso 0.334(18) 1 calc PR A 2 C59B C -0.151(2) 0.4123(13) 0.2877(8) 0.037(6) Uani 0.334(18) 1 d PD A 2 H59B H -0.2195 0.4295 0.3027 0.045 Uiso 0.334(18) 1 calc PR A 2 C60B C -0.011(4) 0.419(3) 0.297(2) 0.042(13) Uani 0.334(18) 1 d PD A 2 H60B H 0.0201 0.4437 0.3163 0.051 Uiso 0.334(18) 1 calc PR A 2 C61B C 0.079(8) 0.387(3) 0.2755(17) 0.06(3) Uani 0.334(18) 1 d PD A 2 H61B H 0.1747 0.3875 0.2825 0.077 Uiso 0.334(18) 1 calc PR A 2 C62B C 0.039(4) 0.3551(13) 0.2447(11) 0.046(9) Uani 0.334(18) 1 d PD A 2 H62B H 0.1068 0.3340 0.2316 0.056 Uiso 0.334(18) 1 calc PR A 2 Al1 Al 0.48153(17) 0.37094(7) 0.61410(5) 0.0257(4) Uani 1 1 d . B . O1 O 0.5948(5) 0.3871(2) 0.65006(15) 0.0454(13) Uani 1 1 d D . . O2 O 0.3673(5) 0.4275(2) 0.61067(16) 0.0458(13) Uani 1 1 d D . . O3 O 0.3921(5) 0.30959(18) 0.62438(14) 0.0383(11) Uani 1 1 d D . . O4 O 0.5701(7) 0.3614(3) 0.57459(19) 0.0760(18) Uani 1 1 d DU . . C63 C 0.7024(14) 0.3801(5) 0.6746(4) 0.034(3) Uani 0.512(5) 1 d PDU B 1 C67 C 0.6609(15) 0.3690(5) 0.7155(4) 0.034(3) Uani 0.512(5) 1 d PDU B 1 C68 C 0.7936(13) 0.4342(5) 0.6744(3) 0.048(4) Uani 0.512(5) 1 d PDU B 1 C69 C 0.7907(12) 0.3284(5) 0.6627(4) 0.048(4) Uani 0.512(5) 1 d PD B 1 F1 F 0.5598(14) 0.4062(4) 0.7252(3) 0.077(4) Uani 0.512(5) 1 d PDU B 1 F2 F 0.7689(12) 0.3755(4) 0.7406(3) 0.068(3) Uani 0.512(5) 1 d PDU B 1 F3 F 0.6077(10) 0.3161(3) 0.7187(3) 0.0593(16) Uani 0.512(5) 1 d PDU B 1 F4 F 0.7379(12) 0.4768(4) 0.6936(3) 0.069(3) Uani 0.512(5) 1 d PDU B 1 F6 F 0.9257(12) 0.4242(5) 0.6884(4) 0.086(4) Uani 0.512(5) 1 d PDU B 1 F7 F 0.8788(9) 0.3078(5) 0.6889(3) 0.063(3) Uani 0.512(5) 1 d PDU B 1 F5 F 0.8140(15) 0.4548(7) 0.6399(3) 0.048(4) Uani 0.512(5) 1 d PD B 1 F8 F 0.8648(8) 0.3404(4) 0.6330(2) 0.059(3) Uani 0.512(5) 1 d PDU B 1 F9 F 0.7079(8) 0.2842(3) 0.6535(2) 0.048(2) Uani 0.512(5) 1 d PDU B 1 C63B C 0.6744(14) 0.4221(6) 0.6657(4) 0.042(4) Uani 0.488(5) 1 d PDU B 2 C67B C 0.5906(15) 0.4748(6) 0.6789(4) 0.058(5) Uani 0.488(5) 1 d PDU B 2 C68B C 0.7870(19) 0.4452(8) 0.6403(5) 0.051(10) Uani 0.488(5) 1 d PDU B 2 C69B C 0.7438(15) 0.3930(6) 0.6987(4) 0.066(5) Uani 0.488(5) 1 d PDU B 2 F1B F 0.6591(10) 0.5047(3) 0.7049(2) 0.0456(16) Uani 0.488(5) 1 d PDU B 2 F2B F 0.4635(11) 0.4580(5) 0.6930(3) 0.072(2) Uani 0.488(5) 1 d PDU B 2 F3B F 0.5453(9) 0.5138(3) 0.6508(2) 0.0456(16) Uani 0.488(5) 1 d PDU B 2 F4B F 0.8489(12) 0.4941(6) 0.6522(3) 0.083(4) Uani 0.488(5) 1 d PDU B 2 F5B F 0.7312(11) 0.4598(5) 0.6062(3) 0.075(3) Uani 0.488(5) 1 d PDU B 2 F6B F 0.8861(11) 0.4062(6) 0.6337(4) 0.097(5) Uani 0.488(5) 1 d PDU B 2 F7B F 0.8559(10) 0.4260(5) 0.7114(3) 0.071(3) Uani 0.488(5) 1 d PDU B 2 F8B F 0.7978(12) 0.3405(4) 0.6882(4) 0.071(3) Uani 0.488(5) 1 d PDU B 2 F9B F 0.6562(13) 0.3855(5) 0.7282(3) 0.055(3) Uani 0.488(5) 1 d PDU B 2 C64 C 0.2732(15) 0.4631(6) 0.5929(4) 0.0303(13) Uani 0.463(6) 1 d PDU B 1 C70 C 0.1564(12) 0.4245(5) 0.5753(3) 0.037(2) Uani 0.463(6) 1 d PDU B 1 C71 C 0.3295(12) 0.4985(5) 0.5594(3) 0.037(2) Uani 0.463(6) 1 d PDU B 1 C72 C 0.1984(12) 0.5014(5) 0.6190(3) 0.037(2) Uani 0.463(6) 1 d PDU B 1 F10 F 0.0753(10) 0.4510(5) 0.5505(3) 0.071(3) Uani 0.463(6) 1 d PDU B 1 F11 F 0.0736(11) 0.4047(5) 0.6027(3) 0.072(2) Uani 0.463(6) 1 d PDU B 1 F12 F 0.2122(10) 0.3780(4) 0.5597(3) 0.055(3) Uani 0.463(6) 1 d PDU B 1 F13 F 0.2606(16) 0.5450(5) 0.5502(4) 0.093(5) Uani 0.463(6) 1 d PDU B 1 F14 F 0.3583(10) 0.4645(5) 0.5306(3) 0.054(3) Uani 0.463(6) 1 d PDU B 1 F15 F 0.4644(11) 0.5171(5) 0.5715(3) 0.062(3) Uani 0.463(6) 1 d PDU B 1 F16 F 0.1661(16) 0.4801(8) 0.6521(5) 0.0593(16) Uani 0.463(6) 1 d PDU B 1 F17 F 0.0898(12) 0.5286(4) 0.6076(3) 0.0593(16) Uani 0.463(6) 1 d PDU B 1 F18 F 0.2865(12) 0.5498(4) 0.6298(3) 0.0593(16) Uani 0.463(6) 1 d PDU B 1 C64B C 0.3325(15) 0.4760(6) 0.6024(5) 0.071(6) Uani 0.537(6) 1 d PDU B 2 C70B C 0.2103(17) 0.4732(7) 0.5714(5) 0.090(3) Uani 0.537(6) 1 d PDU B 2 C71B C 0.4249(18) 0.5126(7) 0.5812(5) 0.090(3) Uani 0.537(6) 1 d PDU B 2 C72B C 0.2710(17) 0.5065(7) 0.6311(4) 0.090(3) Uani 0.537(6) 1 d PDU B 2 F10B F 0.222(2) 0.4381(9) 0.5399(5) 0.185(8) Uani 0.537(6) 1 d PDU B 2 F11B F 0.1017(10) 0.4539(5) 0.5897(4) 0.087(4) Uani 0.537(6) 1 d PDU B 2 F12B F 0.183(2) 0.5276(7) 0.5565(6) 0.161(8) Uani 0.537(6) 1 d PDU B 2 F13B F 0.5538(12) 0.4957(5) 0.5851(5) 0.116(5) Uani 0.537(6) 1 d PDU B 2 F14B F 0.4128(10) 0.5676(3) 0.5828(3) 0.062(3) Uani 0.537(6) 1 d PDU B 2 F15B F 0.397(3) 0.4980(7) 0.5447(5) 0.192(8) Uani 0.537(6) 1 d PDU B 2 F16B F 0.191(2) 0.4701(7) 0.6525(5) 0.124(8) Uani 0.537(6) 1 d PDU B 2 F17B F 0.1740(19) 0.5477(7) 0.6180(6) 0.175(9) Uani 0.537(6) 1 d PDU B 2 F18B F 0.3721(16) 0.5316(9) 0.6533(4) 0.163(7) Uani 0.537(6) 1 d PDU B 2 C65 C 0.2904(13) 0.2787(5) 0.6409(4) 0.0405(17) Uani 0.629(7) 1 d PDU B 1 C73 C 0.2252(14) 0.3139(6) 0.6728(4) 0.064(4) Uani 0.629(7) 1 d PDU B 1 C74 C 0.3515(13) 0.2224(4) 0.6558(3) 0.057(4) Uani 0.629(7) 1 d PDU B 1 C75 C 0.1784(11) 0.2671(4) 0.6097(3) 0.0405(17) Uani 0.629(7) 1 d PDU B 1 F19 F 0.1338(10) 0.3510(4) 0.6588(3) 0.073(3) Uani 0.629(7) 1 d PDU B 1 F20 F 0.3242(12) 0.3450(5) 0.6914(3) 0.082(3) Uani 0.629(7) 1 d PDU B 1 F21 F 0.1614(16) 0.2811(6) 0.6959(4) 0.129(7) Uani 0.629(7) 1 d PDU B 1 F22 F 0.2516(12) 0.1829(4) 0.6612(4) 0.084(4) Uani 0.629(7) 1 d PDU B 1 F23 F 0.4161(14) 0.2323(6) 0.6888(3) 0.109(5) Uani 0.629(7) 1 d PDU B 1 F24 F 0.4494(14) 0.2003(5) 0.6339(4) 0.056(3) Uani 0.629(7) 1 d PDU B 1 F25 F 0.0794(16) 0.2522(7) 0.6312(4) 0.135(6) Uani 0.629(7) 1 d PDU B 1 F26 F 0.2360(11) 0.2237(4) 0.5906(3) 0.062(3) Uani 0.629(7) 1 d PDU B 1 F27 F 0.1568(11) 0.3114(4) 0.5893(3) 0.100(4) Uani 0.629(7) 1 d PDU B 1 C65B C 0.3392(19) 0.2757(9) 0.6468(6) 0.0405(17) Uani 0.371(7) 1 d PDU B 2 C73B C 0.2837(17) 0.3047(7) 0.6813(5) 0.0405(17) Uani 0.371(7) 1 d PDU B 2 C74B C 0.4604(16) 0.2342(6) 0.6583(4) 0.0405(17) Uani 0.371(7) 1 d PDU B 2 C75B C 0.2211(19) 0.2406(8) 0.6277(6) 0.090(3) Uani 0.371(7) 1 d PDU B 2 F19B F 0.2109(17) 0.3516(5) 0.6717(4) 0.051(4) Uani 0.371(7) 1 d PDU B 2 F20B F 0.3951(15) 0.3220(6) 0.7031(4) 0.058(4) Uani 0.371(7) 1 d PDU B 2 F21B F 0.2055(18) 0.2716(8) 0.7028(5) 0.053(5) Uani 0.371(7) 1 d PDU B 2 F22B F 0.5827(12) 0.2625(5) 0.6653(4) 0.061(4) Uani 0.371(7) 1 d PDU B 2 F23B F 0.499(3) 0.1962(11) 0.6323(7) 0.086(9) Uani 0.371(7) 1 d PDU B 2 F24B F 0.4384(17) 0.2032(6) 0.6884(4) 0.059(4) Uani 0.371(7) 1 d PDU B 2 F25B F 0.200(2) 0.1900(8) 0.6461(5) 0.083(7) Uani 0.371(7) 1 d PDU B 2 F26B F 0.270(3) 0.2174(14) 0.5947(7) 0.135(6) Uani 0.371(7) 1 d PDU B 2 F27B F 0.081(2) 0.2481(10) 0.6137(7) 0.097(7) Uani 0.371(7) 1 d PDU B 2 C66 C 0.618(2) 0.3362(9) 0.5457(7) 0.0303(13) Uani 0.537(7) 1 d PDU B 1 C76 C 0.4971(14) 0.3503(6) 0.5194(4) 0.079(6) Uani 0.537(7) 1 d PDU B 1 C77 C 0.6428(16) 0.2721(6) 0.5476(4) 0.078(6) Uani 0.537(7) 1 d PDU B 1 C78 C 0.7495(14) 0.3670(6) 0.5326(4) 0.060(4) Uani 0.537(7) 1 d PDU B 1 F28 F 0.5032(12) 0.4065(5) 0.5090(3) 0.082(4) Uani 0.537(7) 1 d PDU B 1 F29 F 0.3740(11) 0.3455(7) 0.5372(4) 0.106(5) Uani 0.537(7) 1 d PDU B 1 F30 F 0.4943(15) 0.3194(5) 0.4891(3) 0.110(5) Uani 0.537(7) 1 d PDU B 1 F31 F 0.7093(16) 0.2519(5) 0.5175(3) 0.111(6) Uani 0.537(7) 1 d PD B 1 F32 F 0.515(2) 0.2462(9) 0.5463(5) 0.198(15) Uani 0.537(7) 1 d PD B 1 F33 F 0.7079(16) 0.2547(4) 0.5772(3) 0.109(5) Uani 0.537(7) 1 d PDU B 1 F34 F 0.7585(17) 0.3613(8) 0.4951(4) 0.086(5) Uani 0.537(7) 1 d PDU B 1 F35 F 0.8595(18) 0.3404(7) 0.5487(4) 0.085(5) Uani 0.537(7) 1 d PDU B 1 F36 F 0.7487(13) 0.4210(4) 0.5416(4) 0.098(4) Uani 0.537(7) 1 d PDU B 1 C66B C 0.617(2) 0.3339(10) 0.5453(8) 0.0303(13) Uani 0.463(7) 1 d PDU B 2 C76B C 0.6352(15) 0.3681(7) 0.5094(4) 0.068(6) Uani 0.463(7) 1 d PDU B 2 C77B C 0.5336(15) 0.2801(6) 0.5360(4) 0.058(5) Uani 0.463(7) 1 d PDU B 2 C78B C 0.7610(15) 0.3153(6) 0.5598(4) 0.059(5) Uani 0.463(7) 1 d PDU B 2 F28B F 0.728(2) 0.3426(9) 0.4875(6) 0.107(9) Uani 0.463(7) 1 d PDU B 2 F29B F 0.6752(14) 0.4215(5) 0.5169(4) 0.076(4) Uani 0.463(7) 1 d PDU B 2 F30B F 0.5125(12) 0.3710(7) 0.4897(3) 0.084(5) Uani 0.463(7) 1 d PDU B 2 F31B F 0.5746(14) 0.2529(6) 0.5049(3) 0.083(4) Uani 0.463(7) 1 d PDU B 2 F32B F 0.3991(9) 0.2925(5) 0.5304(3) 0.060(3) Uani 0.463(7) 1 d PDU B 2 F33B F 0.5395(15) 0.2401(5) 0.5626(3) 0.055(3) Uani 0.463(7) 1 d PDU B 2 F34B F 0.8155(12) 0.2716(5) 0.5419(3) 0.075(4) Uani 0.463(7) 1 d PDU B 2 F35B F 0.7532(11) 0.2992(5) 0.5956(3) 0.063(3) Uani 0.463(7) 1 d PDU B 2 F36B F 0.8519(19) 0.3598(6) 0.5595(5) 0.077(6) Uani 0.463(7) 1 d PDU B 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 0.02401(14) 0.01941(14) 0.02491(14) 0.00132(9) 0.00064(9) 0.00035(9) P1 0.0258(7) 0.0165(7) 0.0199(7) 0.0008(5) 0.0023(6) -0.0011(6) P2 0.0193(7) 0.0176(7) 0.0223(7) 0.0016(5) 0.0046(5) -0.0012(5) N1 0.039(3) 0.026(3) 0.024(3) 0.002(2) 0.006(2) 0.000(2) N2 0.033(3) 0.023(3) 0.026(3) 0.000(2) 0.005(2) -0.004(2) N3 0.022(2) 0.025(3) 0.027(3) 0.004(2) 0.003(2) -0.001(2) N4 0.031(3) 0.037(3) 0.028(3) 0.004(2) 0.008(2) 0.003(2) C1 0.025(3) 0.013(3) 0.029(3) -0.001(2) 0.001(2) 0.003(2) C2 0.030(3) 0.016(3) 0.034(4) 0.000(2) -0.005(3) 0.000(2) C3 0.030(3) 0.025(3) 0.044(4) -0.003(3) -0.006(3) 0.002(3) C4 0.043(4) 0.050(5) 0.057(5) -0.002(4) -0.021(4) 0.003(4) C5 0.053(5) 0.056(5) 0.049(5) 0.000(4) -0.025(4) -0.008(4) C6 0.066(5) 0.045(4) 0.034(4) 0.005(3) -0.017(4) -0.010(4) C7 0.042(4) 0.020(3) 0.025(3) 0.001(2) -0.006(3) 0.003(3) C8 0.037(3) 0.018(3) 0.021(3) 0.000(2) 0.000(2) 0.002(2) C9 0.038(3) 0.019(3) 0.021(3) 0.002(2) 0.001(2) 0.002(3) C10 0.055(4) 0.030(3) 0.023(3) -0.006(3) 0.004(3) 0.003(3) C11 0.059(5) 0.045(4) 0.023(3) -0.003(3) 0.013(3) 0.009(4) C12 0.047(4) 0.039(4) 0.035(4) 0.009(3) 0.014(3) 0.000(3) C13 0.038(4) 0.032(3) 0.033(4) 0.005(3) 0.011(3) -0.004(3) C14 0.019(3) 0.021(3) 0.029(3) 0.001(2) 0.003(2) 0.005(2) C15 0.023(3) 0.022(3) 0.041(4) 0.000(3) -0.001(3) 0.000(2) C16 0.026(3) 0.028(3) 0.048(4) 0.010(3) 0.006(3) -0.005(3) C17 0.038(4) 0.033(4) 0.035(4) 0.009(3) 0.011(3) -0.001(3) C18 0.042(4) 0.028(3) 0.031(4) 0.000(3) 0.005(3) -0.005(3) C19 0.023(3) 0.023(3) 0.021(3) 0.005(2) 0.008(2) -0.001(2) C20 0.027(3) 0.023(3) 0.032(3) 0.000(3) 0.006(3) -0.003(2) C21 0.037(4) 0.021(3) 0.050(4) 0.001(3) 0.012(3) 0.001(3) C22 0.023(3) 0.032(4) 0.063(5) 0.010(3) 0.006(3) 0.002(3) C23 0.016(3) 0.043(4) 0.047(4) 0.004(3) 0.002(3) -0.002(3) C24 0.026(3) 0.026(3) 0.027(3) 0.002(2) 0.008(2) -0.003(2) C25 0.018(3) 0.021(3) 0.030(3) 0.003(2) 0.004(2) -0.001(2) C26 0.024(3) 0.018(3) 0.033(3) 0.002(2) 0.002(2) -0.002(2) C27 0.055(5) 0.021(3) 0.053(5) 0.004(3) 0.013(4) -0.002(3) C28 0.101(7) 0.018(4) 0.081(7) 0.001(4) 0.032(6) 0.009(4) C29 0.091(7) 0.026(4) 0.062(6) 0.001(4) 0.022(5) 0.022(4) C30 0.036(3) 0.025(3) 0.030(3) -0.002(3) 0.005(3) 0.008(3) C31 0.021(3) 0.022(3) 0.027(3) 0.002(2) -0.001(2) 0.003(2) C32 0.020(3) 0.024(3) 0.020(3) 0.000(2) 0.002(2) 0.002(2) C33 0.016(3) 0.021(3) 0.027(3) 0.004(2) 0.002(2) 0.002(2) C34 0.027(3) 0.029(3) 0.024(3) 0.000(2) 0.001(2) -0.002(3) C35 0.032(3) 0.046(4) 0.023(3) 0.004(3) 0.005(3) -0.004(3) C36 0.026(3) 0.040(4) 0.030(3) 0.013(3) 0.003(3) -0.009(3) C37 0.022(3) 0.028(3) 0.032(3) 0.004(3) 0.001(2) -0.006(2) C38 0.022(3) 0.026(3) 0.033(3) 0.011(3) 0.006(2) 0.002(2) C39 0.044(4) 0.028(4) 0.056(5) 0.008(3) 0.022(4) -0.003(3) C40 0.053(5) 0.045(5) 0.071(6) 0.027(4) 0.037(4) 0.005(4) C41 0.057(5) 0.063(5) 0.046(5) 0.027(4) 0.028(4) 0.017(4) C42 0.046(4) 0.058(5) 0.029(4) 0.006(3) 0.013(3) 0.007(4) C43 0.020(3) 0.018(3) 0.028(3) 0.004(2) 0.009(2) 0.001(2) C44 0.027(3) 0.027(3) 0.038(4) -0.005(3) 0.002(3) 0.002(3) C45 0.025(3) 0.033(4) 0.048(4) -0.002(3) 0.000(3) 0.000(3) C46 0.025(3) 0.031(3) 0.044(4) 0.008(3) 0.007(3) 0.004(3) C47 0.040(4) 0.022(3) 0.049(4) -0.003(3) 0.008(3) 0.007(3) C48 0.030(3) 0.022(3) 0.036(4) 0.000(3) 0.003(3) -0.002(3) C49 0.070(6) 0.039(5) 0.111(8) -0.014(5) -0.014(5) 0.008(4) C50 0.041(4) 0.034(4) 0.083(6) 0.014(4) -0.013(4) 0.005(3) C51 0.048(5) 0.045(5) 0.113(7) 0.050(5) -0.002(5) 0.000(4) C52 0.052(5) 0.099(8) 0.092(7) 0.074(6) 0.011(5) 0.016(4) C53 0.079(6) 0.119(9) 0.047(5) 0.041(5) 0.008(4) 0.044(6) C54 0.053(5) 0.082(6) 0.057(5) 0.005(4) -0.017(4) 0.024(4) C55 0.027(3) 0.048(4) 0.069(5) 0.004(4) -0.005(3) 0.008(3) C56 0.043(6) 0.080(10) 0.057(9) 0.008(7) 0.005(5) 0.002(6) C57 0.037(7) 0.041(17) 0.038(19) 0.008(11) 0.019(8) -0.001(7) C58 0.050(10) 0.025(9) 0.054(12) 0.004(8) 0.025(7) 0.000(7) C59 0.077(13) 0.016(16) 0.043(10) 0.001(9) 0.019(7) -0.009(8) C60 0.034(8) 0.028(9) 0.060(17) 0.010(8) 0.000(9) -0.001(7) C61 0.037(8) 0.040(7) 0.064(10) 0.007(6) 0.015(8) 0.000(7) C62 0.040(8) 0.038(8) 0.060(11) 0.001(7) 0.018(8) 0.007(7) C56B 0.10(2) 0.049(16) 0.06(2) -0.015(14) 0.010(16) -0.020(16) C57B 0.09(6) 0.03(3) 0.02(3) -0.002(16) 0.01(4) -0.02(5) C58B 0.039(17) 0.038(17) 0.044(19) -0.001(14) 0.017(15) -0.013(14) C59B 0.027(14) 0.040(17) 0.045(17) 0.000(12) 0.001(11) -0.003(11) C60B 0.07(2) 0.01(3) 0.04(3) 0.009(16) -0.006(15) -0.013(14) C61B 0.09(6) 0.07(4) 0.03(2) 0.009(19) -0.02(3) -0.03(3) C62B 0.04(2) 0.028(14) 0.07(2) 0.010(16) 0.03(2) -0.004(16) Al1 0.0212(8) 0.0188(8) 0.0374(10) -0.0046(7) 0.0079(7) -0.0021(7) O1 0.029(2) 0.037(3) 0.069(4) -0.005(2) -0.011(2) -0.006(2) O2 0.028(2) 0.035(3) 0.074(4) 0.002(2) -0.005(2) 0.006(2) O3 0.034(2) 0.028(2) 0.054(3) 0.005(2) 0.006(2) -0.0102(19) O4 0.083(3) 0.073(3) 0.073(3) -0.012(2) 0.038(2) -0.003(2) C63 0.052(6) 0.031(6) 0.020(6) -0.011(4) 0.014(5) -0.012(5) C67 0.052(6) 0.031(6) 0.020(6) -0.011(4) 0.014(5) -0.012(5) C68 0.058(9) 0.059(9) 0.027(7) 0.006(7) -0.007(6) -0.030(7) C69 0.028(7) 0.077(12) 0.038(9) 0.003(8) 0.007(7) 0.018(8) F1 0.100(8) 0.054(6) 0.079(8) -0.007(5) 0.067(7) -0.003(6) F2 0.097(8) 0.068(6) 0.039(5) -0.008(4) -0.009(5) -0.015(6) F3 0.083(4) 0.031(3) 0.064(4) 0.004(2) 0.018(3) 0.019(2) F4 0.122(9) 0.036(5) 0.051(6) -0.019(4) 0.032(6) -0.029(5) F6 0.076(8) 0.091(8) 0.089(9) 0.014(7) -0.038(7) -0.037(7) F7 0.045(5) 0.080(7) 0.062(6) 0.007(5) -0.016(4) 0.009(5) F5 0.040(6) 0.064(8) 0.042(7) 0.008(5) 0.014(5) -0.031(6) F8 0.037(5) 0.090(7) 0.050(5) 0.006(5) 0.018(4) 0.020(4) F9 0.048(5) 0.043(5) 0.052(5) -0.023(4) 0.000(4) 0.003(4) C63B 0.037(8) 0.056(10) 0.032(8) -0.007(7) -0.005(6) -0.011(7) C67B 0.087(12) 0.042(9) 0.046(9) -0.006(7) 0.002(8) 0.000(8) C68B 0.040(13) 0.050(13) 0.064(15) 0.014(9) 0.013(9) -0.019(9) C69B 0.063(11) 0.051(10) 0.083(13) -0.016(10) -0.018(10) 0.008(9) F1B 0.069(4) 0.022(3) 0.045(3) -0.007(2) -0.011(3) -0.013(3) F2B 0.074(5) 0.079(5) 0.063(5) -0.026(4) 0.032(4) -0.026(4) F3B 0.069(4) 0.022(3) 0.045(3) -0.007(2) -0.011(3) -0.013(3) F4B 0.078(8) 0.090(9) 0.080(8) -0.004(7) -0.004(6) -0.038(7) F5B 0.083(7) 0.085(7) 0.056(6) 0.012(5) 0.003(5) -0.040(6) F6B 0.047(6) 0.148(12) 0.097(9) -0.035(8) 0.019(6) -0.013(7) F7B 0.044(6) 0.094(8) 0.072(8) -0.037(6) -0.032(5) 0.000(5) F8B 0.083(8) 0.057(6) 0.072(8) -0.001(6) -0.027(7) 0.007(6) F9B 0.084(8) 0.044(6) 0.036(6) -0.009(5) -0.006(6) -0.019(6) C64 0.028(3) 0.036(3) 0.027(3) 0.001(3) 0.001(2) 0.007(3) C70 0.022(4) 0.049(5) 0.039(5) 0.024(4) 0.013(3) 0.025(4) C71 0.022(4) 0.049(5) 0.039(5) 0.024(4) 0.013(3) 0.025(4) C72 0.022(4) 0.049(5) 0.039(5) 0.024(4) 0.013(3) 0.025(4) F10 0.040(5) 0.108(9) 0.064(7) -0.002(6) -0.017(5) 0.021(6) F11 0.074(5) 0.079(5) 0.063(5) -0.026(4) 0.032(4) -0.026(4) F12 0.047(5) 0.064(6) 0.054(6) -0.015(5) -0.004(4) 0.001(5) F13 0.119(12) 0.074(8) 0.088(9) 0.044(7) 0.035(9) 0.038(8) F14 0.052(6) 0.070(7) 0.040(5) 0.008(5) 0.005(4) 0.002(5) F15 0.057(7) 0.074(8) 0.054(7) 0.015(6) 0.001(5) -0.032(6) F16 0.083(4) 0.031(3) 0.064(4) 0.004(2) 0.018(3) 0.019(2) F17 0.083(4) 0.031(3) 0.064(4) 0.004(2) 0.018(3) 0.019(2) F18 0.083(4) 0.031(3) 0.064(4) 0.004(2) 0.018(3) 0.019(2) C64B 0.029(8) 0.027(8) 0.157(16) 0.011(9) 0.007(9) -0.001(6) C70B 0.104(7) 0.064(5) 0.103(7) 0.007(5) 0.029(6) 0.019(6) C71B 0.104(7) 0.064(5) 0.103(7) 0.007(5) 0.029(6) 0.019(6) C72B 0.104(7) 0.064(5) 0.103(7) 0.007(5) 0.029(6) 0.019(6) F10B 0.193(16) 0.200(14) 0.163(14) -0.063(12) 0.042(12) -0.015(13) F11B 0.041(5) 0.095(8) 0.125(9) -0.002(7) 0.004(5) -0.008(5) F12B 0.167(15) 0.133(10) 0.184(16) 0.078(9) 0.001(12) 0.035(11) F13B 0.088(7) 0.058(6) 0.205(12) 0.038(8) 0.086(7) 0.019(6) F14B 0.100(7) 0.020(4) 0.068(6) 0.010(4) 0.026(5) 0.006(4) F15B 0.35(2) 0.076(9) 0.145(12) -0.025(9) -0.031(13) 0.023(13) F16B 0.244(18) 0.067(11) 0.063(8) 0.017(7) 0.071(10) 0.002(11) F17B 0.208(17) 0.102(11) 0.220(17) 0.046(11) 0.118(14) 0.086(12) F18B 0.143(11) 0.285(17) 0.060(8) 0.053(9) -0.031(7) -0.150(12) C65 0.050(5) 0.027(3) 0.045(4) -0.006(3) -0.002(3) -0.022(3) C73 0.056(9) 0.057(9) 0.080(11) 0.016(9) 0.020(8) 0.008(8) C74 0.087(10) 0.035(6) 0.050(8) 0.001(6) 0.027(7) -0.008(7) C75 0.050(5) 0.027(3) 0.045(4) -0.006(3) -0.002(3) -0.022(3) F19 0.050(5) 0.060(5) 0.111(9) -0.008(5) 0.033(5) 0.007(5) F20 0.093(8) 0.103(8) 0.052(6) -0.034(5) 0.015(5) 0.009(6) F21 0.191(14) 0.081(8) 0.118(12) 0.037(7) 0.122(11) 0.029(9) F22 0.099(8) 0.033(4) 0.122(10) 0.014(6) 0.055(8) -0.005(5) F23 0.148(11) 0.115(10) 0.063(7) 0.015(7) 0.007(6) 0.069(9) F24 0.075(8) 0.031(5) 0.063(6) 0.002(4) 0.010(5) 0.004(5) F25 0.103(8) 0.165(11) 0.137(10) -0.078(9) 0.019(7) 0.039(7) F26 0.069(6) 0.042(4) 0.076(6) -0.027(4) -0.010(4) -0.007(4) F27 0.089(7) 0.091(7) 0.119(9) -0.008(6) -0.056(6) 0.010(5) C65B 0.050(5) 0.027(3) 0.045(4) -0.006(3) -0.002(3) -0.022(3) C73B 0.050(5) 0.027(3) 0.045(4) -0.006(3) -0.002(3) -0.022(3) C74B 0.050(5) 0.027(3) 0.045(4) -0.006(3) -0.002(3) -0.022(3) C75B 0.104(7) 0.064(5) 0.103(7) 0.007(5) 0.029(6) 0.019(6) F19B 0.068(10) 0.028(7) 0.059(9) -0.008(6) 0.016(8) 0.012(8) F20B 0.073(9) 0.050(8) 0.051(8) -0.006(6) 0.016(7) -0.009(7) F21B 0.071(8) 0.052(8) 0.035(7) 0.007(6) 0.007(6) -0.016(7) F22B 0.059(8) 0.050(7) 0.074(9) 0.005(6) -0.009(6) 0.009(6) F23B 0.084(16) 0.081(14) 0.092(14) 0.034(11) -0.006(11) 0.008(11) F24B 0.075(9) 0.057(9) 0.046(8) 0.013(7) 0.012(6) 0.019(8) F25B 0.111(13) 0.062(11) 0.076(11) 0.027(8) -0.030(9) -0.063(10) F26B 0.103(8) 0.165(11) 0.137(10) -0.078(9) 0.019(7) 0.039(7) F27B 0.077(10) 0.094(10) 0.120(12) 0.003(9) -0.004(8) 0.024(8) C66 0.028(3) 0.036(3) 0.027(3) 0.001(3) 0.001(2) 0.007(3) C76 0.065(11) 0.105(14) 0.065(12) 0.023(10) -0.012(9) -0.021(10) C77 0.127(15) 0.048(9) 0.059(11) -0.007(8) -0.029(11) 0.007(10) C78 0.056(9) 0.063(10) 0.060(10) 0.000(8) -0.005(8) 0.003(8) F28 0.110(9) 0.087(7) 0.047(6) 0.016(6) 0.000(6) 0.049(7) F29 0.052(6) 0.175(14) 0.089(9) 0.006(8) -0.007(6) -0.025(7) F30 0.184(12) 0.062(7) 0.082(8) -0.009(6) -0.086(8) -0.009(7) F31 0.198(16) 0.054(6) 0.080(9) -0.033(6) -0.038(9) 0.064(8) F32 0.33(4) 0.127(16) 0.13(2) 0.020(14) -0.019(19) -0.17(2) F33 0.210(13) 0.038(5) 0.076(8) 0.009(5) -0.053(8) 0.032(7) F34 0.075(8) 0.100(10) 0.085(12) 0.032(8) 0.062(8) 0.028(7) F35 0.046(7) 0.128(13) 0.082(9) -0.013(9) 0.007(6) 0.012(9) F36 0.104(9) 0.059(7) 0.128(11) -0.002(7) -0.033(8) -0.045(6) C66B 0.028(3) 0.036(3) 0.027(3) 0.001(3) 0.001(2) 0.007(3) C76B 0.064(11) 0.098(14) 0.042(10) 0.013(10) 0.027(9) 0.033(10) C77B 0.070(12) 0.050(10) 0.056(11) -0.017(9) 0.007(9) -0.006(9) C78B 0.050(10) 0.088(13) 0.039(9) 0.010(9) 0.008(8) 0.002(9) F28B 0.141(17) 0.130(16) 0.051(9) 0.019(9) 0.049(9) 0.070(13) F29B 0.093(9) 0.068(7) 0.069(8) 0.026(6) 0.049(7) -0.002(7) F30B 0.075(8) 0.145(12) 0.032(6) 0.012(7) 0.007(5) 0.059(8) F31B 0.095(8) 0.089(8) 0.066(7) -0.044(6) 0.000(6) 0.023(7) F32B 0.033(5) 0.069(7) 0.078(7) -0.033(6) -0.015(4) 0.005(5) F33B 0.090(8) 0.023(5) 0.051(7) -0.013(5) 0.020(6) 0.004(5) F34B 0.069(7) 0.089(8) 0.066(7) 0.009(6) 0.015(6) 0.061(6) F35B 0.064(6) 0.084(8) 0.040(6) 0.000(5) -0.015(5) 0.034(6) F36B 0.036(7) 0.079(9) 0.117(14) -0.029(9) -0.017(8) 0.001(6) #=============================================================================== # 10. MOLECULAR GEOMETRY _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 Tl1 N1 2.799(5) . ? Tl1 N3 2.833(5) . ? Tl1 P2 3.1508(14) . ? Tl1 P1 3.2075(14) . ? P1 C8 1.801(6) . ? P1 C1 1.805(6) . ? P1 C19 1.824(6) . ? P2 C32 1.802(6) . ? P2 C25 1.810(6) . ? P2 C43 1.836(6) . ? N1 C9 1.345(8) . ? N1 C13 1.349(8) . ? N2 C18 1.335(8) . ? N2 C14 1.345(8) . ? N3 C37 1.348(8) . ? N3 C33 1.353(8) . ? N4 C42 1.343(8) . ? N4 C38 1.346(9) . ? C1 C2 1.360(9) . ? C1 C14 1.461(8) . ? C2 C7 1.466(9) . ? C2 C3 1.512(9) . ? C3 C4 1.528(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.507(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.527(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.516(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.362(9) . ? C8 C9 1.470(9) . ? C9 C10 1.393(9) . ? C10 C11 1.379(10) . ? C10 H10 0.9500 . ? C11 C12 1.389(11) . ? C11 H11 0.9500 . ? C12 C13 1.365(10) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.390(8) . ? C15 C16 1.385(9) . ? C15 H15 0.9500 . ? C16 C17 1.377(10) . ? C16 H16 0.9500 . ? C17 C18 1.390(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.391(9) . ? C19 C20 1.395(8) . ? C20 C21 1.385(9) . ? C20 H20 0.9500 . ? C21 C22 1.379(10) . ? C21 H21 0.9500 . ? C22 C23 1.388(10) . ? C22 H22 0.9500 . ? C23 C24 1.387(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.369(9) . ? C25 C38 1.458(8) . ? C26 C31 1.462(8) . ? C26 C27 1.515(9) . ? C27 C28 1.520(11) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.422(13) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.520(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.511(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.362(8) . ? C32 C33 1.470(8) . ? C33 C34 1.388(8) . ? C34 C35 1.381(9) . ? C34 H34 0.9500 . ? C35 C36 1.387(10) . ? C35 H35 0.9500 . ? C36 C37 1.382(9) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.401(9) . ? C39 C40 1.378(11) . ? C39 H39 0.9500 . ? C40 C41 1.371(13) . ? C40 H40 0.9500 . ? C41 C42 1.367(11) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.380(9) . ? C43 C48 1.393(9) . ? C44 C45 1.385(9) . ? C44 H44 0.9500 . ? C45 C46 1.384(10) . ? C45 H45 0.9500 . ? C46 C47 1.378(10) . ? C46 H46 0.9500 . ? C47 C48 1.385(9) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.498(14) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.369(12) . ? C50 C55 1.386(11) . ? C51 C52 1.339(16) . ? C51 H51 0.9500 . ? C52 C53 1.398(17) . ? C52 H52 0.9500 . ? C53 C54 1.388(14) . ? C53 H53 0.9500 . ? C54 C55 1.404(12) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C57 1.55(4) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.37(4) . ? C57 C62 1.38(3) . ? C58 C59 1.38(3) . ? C58 H58 0.9500 . ? C59 C60 1.36(3) . ? C59 H59 0.9500 . ? C60 C61 1.43(3) . ? C60 H60 0.9500 . ? C61 C62 1.36(2) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C56B C57B 1.45(6) . ? C56B H56D 0.9800 . ? C56B H56E 0.9800 . ? C56B H56F 0.9800 . ? C57B C62B 1.39(3) . ? C57B C58B 1.39(2) . ? C58B C59B 1.39(2) . ? C58B H58B 0.9500 . ? C59B C60B 1.39(2) . ? C59B H59B 0.9500 . ? C60B C61B 1.39(3) . ? C60B H60B 0.9500 . ? C61B C62B 1.39(3) . ? C61B H61B 0.9500 . ? C62B H62B 0.9500 . ? Al1 O4 1.691(6) . ? Al1 O3 1.713(4) . ? Al1 O2 1.720(5) . ? Al1 O1 1.723(5) . ? O1 C63B 1.247(15) . ? O1 C63 1.361(16) . ? O2 C64B 1.213(16) . ? O2 C64 1.378(16) . ? O3 C65B 1.25(2) . ? O3 C65 1.362(14) . ? O4 C66B 1.32(4) . ? O4 C66 1.29(3) . ? C63 C68 1.535(14) . ? C63 C69 1.541(15) . ? C63 C67 1.560(14) . ? C67 F3 1.341(14) . ? C67 F1 1.353(15) . ? C67 F2 1.374(15) . ? C68 F4 1.331(14) . ? C68 F5 1.353(14) . ? C68 F6 1.379(15) . ? C69 F8 1.328(13) . ? C69 F9 1.341(14) . ? C69 F7 1.348(14) . ? C63B C69B 1.517(16) . ? C63B C68B 1.529(17) . ? C63B C67B 1.549(16) . ? C67B F1B 1.334(14) . ? C67B F2B 1.389(15) . ? C67B F3B 1.425(14) . ? C68B F6B 1.343(17) . ? C68B F4B 1.352(19) . ? C68B F5B 1.378(18) . ? C69B F8B 1.384(15) . ? C69B F9B 1.385(15) . ? C69B F7B 1.397(15) . ? F3B F18B 1.72(2) . ? C64 C72 1.494(15) . ? C64 C70 1.565(16) . ? C64 C71 1.568(15) . ? C70 F10 1.331(13) . ? C70 F12 1.339(14) . ? C70 F11 1.362(13) . ? C71 F13 1.309(14) . ? C71 F14 1.340(14) . ? C71 F15 1.429(14) . ? C72 F17 1.284(14) . ? C72 F16 1.337(16) . ? C72 F18 1.459(14) . ? C64B C72B 1.397(17) . ? C64B C71B 1.461(17) . ? C64B C70B 1.612(18) . ? C70B F11B 1.325(15) . ? C70B F12B 1.400(17) . ? C70B F10B 1.409(17) . ? C71B F14B 1.289(17) . ? C71B F13B 1.307(17) . ? C71B F15B 1.385(18) . ? C72B F18B 1.379(16) . ? C72B F16B 1.390(17) . ? C72B F17B 1.416(17) . ? C65 C74 1.531(14) . ? C65 C73 1.556(15) . ? C65 C75 1.569(13) . ? C73 F21 1.294(14) . ? C73 F19 1.327(14) . ? C73 F20 1.363(14) . ? C74 F24 1.344(14) . ? C74 F22 1.349(13) . ? C74 F23 1.355(14) . ? C75 F27 1.283(12) . ? C75 F25 1.288(14) . ? C75 F26 1.351(12) . ? C65B C73B 1.525(18) . ? C65B C75B 1.552(18) . ? C65B C74B 1.565(18) . ? C73B F21B 1.337(17) . ? C73B F19B 1.340(16) . ? C73B F20B 1.379(16) . ? C74B F24B 1.326(17) . ? C74B F23B 1.348(18) . ? C74B F22B 1.368(16) . ? C75B F25B 1.372(19) . ? C75B F27B 1.443(18) . ? C75B F26B 1.400(19) . ? C66 C77 1.514(19) . ? C66 C76 1.528(17) . ? C66 C78 1.533(18) . ? C76 F30 1.313(16) . ? C76 F29 1.362(15) . ? C76 F28 1.364(15) . ? C77 F33 1.295(15) . ? C77 F31 1.356(16) . ? C77 F32 1.368(17) . ? C78 F36 1.302(15) . ? C78 F35 1.350(16) . ? C78 F34 1.363(17) . ? C66B C78B 1.531(19) . ? C66B C77B 1.527(19) . ? C66B C76B 1.54(2) . ? C76B F29B 1.329(16) . ? C76B F28B 1.344(17) . ? C76B F30B 1.369(15) . ? C77B F33B 1.338(16) . ? C77B F32B 1.338(15) . ? C77B F31B 1.354(15) . ? C78B F34B 1.321(16) . ? C78B F35B 1.351(14) . ? C78B F36B 1.357(17) . ? 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 N1 Tl1 N3 117.34(15) . . ? N1 Tl1 P2 87.09(11) . . ? N3 Tl1 P2 60.41(10) . . ? N1 Tl1 P1 61.43(11) . . ? N3 Tl1 P1 85.67(10) . . ? P2 Tl1 P1 116.24(4) . . ? C8 P1 C1 90.9(3) . . ? C8 P1 C19 105.6(3) . . ? C1 P1 C19 105.4(3) . . ? C8 P1 Tl1 86.52(19) . . ? C1 P1 Tl1 122.01(18) . . ? C19 P1 Tl1 130.97(19) . . ? C32 P2 C25 90.8(3) . . ? C32 P2 C43 103.6(3) . . ? C25 P2 C43 106.1(3) . . ? C32 P2 Tl1 92.74(19) . . ? C25 P2 Tl1 129.90(19) . . ? C43 P2 Tl1 121.34(19) . . ? C9 N1 C13 118.3(6) . . ? C9 N1 Tl1 118.1(4) . . ? C13 N1 Tl1 119.4(4) . . ? C18 N2 C14 118.0(5) . . ? C37 N3 C33 117.8(5) . . ? C37 N3 Tl1 115.5(4) . . ? C33 N3 Tl1 120.7(4) . . ? C42 N4 C38 117.7(6) . . ? C2 C1 C14 130.7(5) . . ? C2 C1 P1 109.9(4) . . ? C14 C1 P1 119.0(4) . . ? C1 C2 C7 114.1(5) . . ? C1 C2 C3 125.8(6) . . ? C7 C2 C3 120.0(6) . . ? C2 C3 C4 112.0(6) . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 110.0(6) . . ? C5 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? C5 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 C5 C6 111.6(7) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C5 114.0(6) . . ? C7 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C2 113.7(5) . . ? C8 C7 C6 124.8(6) . . ? C2 C7 C6 121.0(6) . . ? C7 C8 C9 129.5(6) . . ? C7 C8 P1 110.1(5) . . ? C9 C8 P1 119.7(4) . . ? N1 C9 C10 121.7(6) . . ? N1 C9 C8 116.1(5) . . ? C10 C9 C8 122.2(6) . . ? C11 C10 C9 119.4(6) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 118.6(6) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C13 C12 C11 119.3(6) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? N1 C13 C12 122.7(6) . . ? N1 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? N2 C14 C15 121.5(6) . . ? N2 C14 C1 115.1(5) . . ? C15 C14 C1 123.3(6) . . ? C16 C15 C14 119.5(6) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 119.3(6) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 117.6(6) . . ? C16 C17 H17 121.2 . . ? C18 C17 H17 121.2 . . ? N2 C18 C17 124.0(6) . . ? N2 C18 H18 118.0 . . ? C17 C18 H18 118.0 . . ? C24 C19 C20 119.7(5) . . ? C24 C19 P1 118.9(4) . . ? C20 C19 P1 121.4(5) . . ? C21 C20 C19 119.8(6) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 120.4(6) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.2(6) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.8(6) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 120.2(6) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? C26 C25 C38 131.0(5) . . ? C26 C25 P2 109.8(4) . . ? C38 C25 P2 118.4(4) . . ? C25 C26 C31 114.1(5) . . ? C25 C26 C27 124.9(6) . . ? C31 C26 C27 120.8(5) . . ? C26 C27 C28 113.3(6) . . ? C26 C27 H27A 108.9 . . ? C28 C27 H27A 108.9 . . ? C26 C27 H27B 108.9 . . ? C28 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C29 C28 C27 116.4(7) . . ? C29 C28 H28A 108.2 . . ? C27 C28 H28A 108.2 . . ? C29 C28 H28B 108.2 . . ? C27 C28 H28B 108.2 . . ? H28A C28 H28B 107.3 . . ? C28 C29 C30 113.5(7) . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C31 C30 C29 111.9(6) . . ? C31 C30 H30A 109.2 . . ? C29 C30 H30A 109.2 . . ? C31 C30 H30B 109.2 . . ? C29 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C32 C31 C26 113.8(5) . . ? C32 C31 C30 125.3(5) . . ? C26 C31 C30 120.8(5) . . ? C31 C32 C33 129.0(5) . . ? C31 C32 P2 110.6(4) . . ? C33 C32 P2 120.0(4) . . ? N3 C33 C34 121.8(5) . . ? N3 C33 C32 115.2(5) . . ? C34 C33 C32 122.9(5) . . ? C35 C34 C33 119.5(6) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 119.2(6) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C37 C36 C35 118.1(6) . . ? C37 C36 H36 120.9 . . ? C35 C36 H36 120.9 . . ? N3 C37 C36 123.5(6) . . ? N3 C37 H37 118.3 . . ? C36 C37 H37 118.3 . . ? N4 C38 C39 120.9(6) . . ? N4 C38 C25 114.9(5) . . ? C39 C38 C25 124.2(6) . . ? C40 C39 C38 119.6(7) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C41 C40 C39 119.3(7) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C42 C41 C40 118.1(7) . . ? C42 C41 H41 120.9 . . ? C40 C41 H41 120.9 . . ? N4 C42 C41 124.4(8) . . ? N4 C42 H42 117.8 . . ? C41 C42 H42 117.8 . . ? C44 C43 C48 119.1(6) . . ? C44 C43 P2 121.7(4) . . ? C48 C43 P2 119.2(5) . . ? C43 C44 C45 120.8(6) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C46 C45 C44 120.4(6) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C47 C46 C45 118.9(6) . . ? C47 C46 H46 120.6 . . ? C45 C46 H46 120.6 . . ? C46 C47 C48 121.3(6) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.3 . . ? C47 C48 C43 119.6(6) . . ? C47 C48 H48 120.2 . . ? C43 C48 H48 120.2 . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 C55 118.3(10) . . ? C51 C50 C49 120.3(9) . . ? C55 C50 C49 121.3(8) . . ? C52 C51 C50 121.2(10) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C51 C52 C53 122.8(9) . . ? C51 C52 H52 118.6 . . ? C53 C52 H52 118.6 . . ? C54 C53 C52 117.0(11) . . ? C54 C53 H53 121.5 . . ? C52 C53 H53 121.5 . . ? C53 C54 C55 119.8(10) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C50 C55 C54 120.9(8) . . ? C50 C55 H55 119.6 . . ? C54 C55 H55 119.6 . . ? C58 C57 C62 122(3) . . ? C58 C57 C56 120(3) . . ? C62 C57 C56 118(3) . . ? C57 C58 C59 120(2) . . ? C57 C58 H58 120.1 . . ? C59 C58 H58 120.1 . . ? C60 C59 C58 120(3) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C59 C60 C61 118(3) . . ? C59 C60 H60 120.8 . . ? C61 C60 H60 120.8 . . ? C62 C61 C60 122(2) . . ? C62 C61 H61 119.0 . . ? C60 C61 H61 119.0 . . ? C61 C62 C57 117(2) . . ? C61 C62 H62 121.4 . . ? C57 C62 H62 121.4 . . ? C57B C56B H56D 109.5 . . ? C57B C56B H56E 109.5 . . ? H56D C56B H56E 109.5 . . ? C57B C56B H56F 109.5 . . ? H56D C56B H56F 109.5 . . ? H56E C56B H56F 109.5 . . ? C62B C57B C58B 116(4) . . ? C62B C57B C56B 121(5) . . ? C58B C57B C56B 123(4) . . ? C59B C58B C57B 124(3) . . ? C59B C58B H58B 118.1 . . ? C57B C58B H58B 118.1 . . ? C58B C59B C60B 121(3) . . ? C58B C59B H59B 119.6 . . ? C60B C59B H59B 119.6 . . ? C61B C60B C59B 115(5) . . ? C61B C60B H60B 122.6 . . ? C59B C60B H60B 122.6 . . ? C60B C61B C62B 125(6) . . ? C60B C61B H61B 117.7 . . ? C62B C61B H61B 117.7 . . ? C57B C62B C61B 120(5) . . ? C57B C62B H62B 120.1 . . ? C61B C62B H62B 120.1 . . ? O4 Al1 O3 109.7(3) . . ? O4 Al1 O2 111.8(3) . . ? O3 Al1 O2 109.4(2) . . ? O4 Al1 O1 110.1(3) . . ? O3 Al1 O1 109.4(3) . . ? O2 Al1 O1 106.3(3) . . ? C63B O1 Al1 149.3(8) . . ? C63 O1 Al1 158.3(6) . . ? C64B O2 Al1 154.7(8) . . ? C64 O2 Al1 155.3(7) . . ? C65B O3 Al1 152.0(9) . . ? C65 O3 Al1 154.7(6) . . ? C66B O4 Al1 157.5(10) . . ? C66 O4 Al1 159.4(9) . . ? O1 C63 C68 109.1(10) . . ? O1 C63 C69 109.2(10) . . ? C68 C63 C69 108.8(10) . . ? O1 C63 C67 115.7(10) . . ? C68 C63 C67 107.3(9) . . ? C69 C63 C67 106.7(10) . . ? F3 C67 F1 106.7(10) . . ? F3 C67 F2 109.2(11) . . ? F1 C67 F2 107.4(12) . . ? F3 C67 C63 109.8(10) . . ? F1 C67 C63 109.7(11) . . ? F2 C67 C63 113.8(11) . . ? F4 C68 F5 106.4(10) . . ? F4 C68 F6 108.2(11) . . ? F5 C68 F6 104.4(11) . . ? F4 C68 C63 112.0(10) . . ? F5 C68 C63 112.9(12) . . ? F6 C68 C63 112.5(11) . . ? F8 C69 F9 106.6(11) . . ? F8 C69 F7 107.6(9) . . ? F9 C69 F7 105.3(10) . . ? F8 C69 C63 111.6(10) . . ? F9 C69 C63 110.0(9) . . ? F7 C69 C63 115.2(12) . . ? O1 C63B C69B 108.8(12) . . ? O1 C63B C68B 113.3(13) . . ? C69B C63B C68B 108.7(11) . . ? O1 C63B C67B 109.8(11) . . ? C69B C63B C67B 109.7(10) . . ? C68B C63B C67B 106.5(11) . . ? F1B C67B F2B 108.4(11) . . ? F1B C67B F3B 108.0(10) . . ? F2B C67B F3B 100.4(10) . . ? F1B C67B C63B 112.2(12) . . ? F2B C67B C63B 110.9(11) . . ? F3B C67B C63B 116.1(10) . . ? F6B C68B F4B 108.4(15) . . ? F6B C68B F5B 105.8(14) . . ? F4B C68B F5B 103.8(13) . . ? F6B C68B C63B 112.5(14) . . ? F4B C68B C63B 114.8(15) . . ? F5B C68B C63B 110.7(14) . . ? F8B C69B F9B 109.7(12) . . ? F8B C69B F7B 106.6(11) . . ? F9B C69B F7B 106.9(12) . . ? F8B C69B C63B 110.0(12) . . ? F9B C69B C63B 113.4(11) . . ? F7B C69B C63B 109.9(12) . . ? C67B F3B F18B 113.6(9) . . ? O2 C64 C72 112.6(10) . . ? O2 C64 C70 107.7(10) . . ? C72 C64 C70 104.4(10) . . ? O2 C64 C71 116.3(10) . . ? C72 C64 C71 110.5(10) . . ? C70 C64 C71 104.2(10) . . ? F10 C70 F12 109.0(11) . . ? F10 C70 F11 107.6(10) . . ? F12 C70 F11 106.1(10) . . ? F10 C70 C64 114.5(11) . . ? F12 C70 C64 110.3(10) . . ? F11 C70 C64 109.0(10) . . ? F13 C71 F14 113.8(11) . . ? F13 C71 F15 106.2(12) . . ? F14 C71 F15 102.6(9) . . ? F13 C71 C64 116.7(11) . . ? F14 C71 C64 111.5(10) . . ? F15 C71 C64 104.3(10) . . ? F17 C72 F16 105.6(11) . . ? F17 C72 F18 99.8(10) . . ? F16 C72 F18 101.1(11) . . ? F17 C72 C64 119.4(12) . . ? F16 C72 C64 117.8(13) . . ? F18 C72 C64 110.2(10) . . ? O2 C64B C72B 114.2(16) . . ? O2 C64B C71B 120.3(13) . . ? C72B C64B C71B 111.3(12) . . ? O2 C64B C70B 109.1(13) . . ? C72B C64B C70B 102.9(11) . . ? C71B C64B C70B 95.8(12) . . ? F11B C70B F12B 110.8(14) . . ? F11B C70B F10B 106.5(14) . . ? F12B C70B F10B 103.4(14) . . ? F11B C70B C64B 103.8(12) . . ? F12B C70B C64B 111.1(16) . . ? F10B C70B C64B 121.1(16) . . ? F14B C71B F13B 112.4(13) . . ? F14B C71B F15B 105.8(14) . . ? F13B C71B F15B 101.2(15) . . ? F14B C71B C64B 120.1(14) . . ? F13B C71B C64B 110.6(14) . . ? F15B C71B C64B 104.4(17) . . ? F18B C72B F16B 109.2(14) . . ? F18B C72B C64B 110.0(15) . . ? F16B C72B C64B 110.5(15) . . ? F18B C72B F17B 111.1(15) . . ? F16B C72B F17B 103.4(13) . . ? C64B C72B F17B 112.4(15) . . ? C72B F18B F3B 122.8(16) . . ? O3 C65 C74 109.4(9) . . ? O3 C65 C73 110.5(9) . . ? C74 C65 C73 110.4(9) . . ? O3 C65 C75 105.4(9) . . ? C74 C65 C75 111.0(9) . . ? C73 C65 C75 110.0(9) . . ? F21 C73 F19 108.2(11) . . ? F21 C73 F20 109.4(12) . . ? F19 C73 F20 107.1(11) . . ? F21 C73 C65 111.7(13) . . ? F19 C73 C65 109.4(10) . . ? F20 C73 C65 110.9(10) . . ? F24 C74 F22 109.4(9) . . ? F24 C74 F23 105.6(11) . . ? F22 C74 F23 107.8(11) . . ? F24 C74 C65 113.0(11) . . ? F22 C74 C65 111.5(11) . . ? F23 C74 C65 109.3(10) . . ? F27 C75 F25 116.8(12) . . ? F27 C75 F26 111.7(10) . . ? F25 C75 F26 115.0(10) . . ? F27 C75 C65 112.2(9) . . ? F25 C75 C65 96.8(12) . . ? F26 C75 C65 102.4(9) . . ? O3 C65B C73B 113.8(15) . . ? O3 C65B C75B 110.5(16) . . ? C73B C65B C75B 109.4(13) . . ? O3 C65B C74B 104.7(14) . . ? C73B C65B C74B 109.0(14) . . ? C75B C65B C74B 109.2(13) . . ? F21B C73B F19B 108.9(14) . . ? F21B C73B F20B 106.0(13) . . ? F19B C73B F20B 107.9(13) . . ? F21B C73B C65B 115.4(17) . . ? F19B C73B C65B 109.9(14) . . ? F20B C73B C65B 108.5(13) . . ? F24B C74B F23B 105.3(15) . . ? F24B C74B F22B 105.2(13) . . ? F23B C74B F22B 101.5(14) . . ? F24B C74B C65B 115.2(16) . . ? F23B C74B C65B 115.5(18) . . ? F22B C74B C65B 112.7(12) . . ? F25B C75B F27B 97.4(15) . . ? F25B C75B F26B 97.9(17) . . ? F27B C75B F26B 94.5(15) . . ? F25B C75B C65B 110.5(18) . . ? F27B C75B C65B 139.9(18) . . ? F26B C75B C65B 109(2) . . ? O4 C66 C77 118.1(16) . . ? O4 C66 C76 97.0(16) . . ? C77 C66 C76 110.9(15) . . ? O4 C66 C78 110.3(16) . . ? C77 C66 C78 110.4(16) . . ? C76 C66 C78 109.3(13) . . ? F30 C76 F29 110.2(12) . . ? F30 C76 F28 107.3(12) . . ? F29 C76 F28 104.5(12) . . ? F30 C76 C66 113.9(17) . . ? F29 C76 C66 110.5(14) . . ? F28 C76 C66 109.9(12) . . ? F33 C77 F31 109.0(13) . . ? F33 C77 F32 108.0(14) . . ? F31 C77 F32 104.9(13) . . ? F33 C77 C66 114.7(13) . . ? F31 C77 C66 112.4(16) . . ? F32 C77 C66 107.2(15) . . ? F36 C78 F35 110.0(12) . . ? F36 C78 F34 110.1(13) . . ? F35 C78 F34 108.8(12) . . ? F36 C78 C66 111.5(14) . . ? F35 C78 C66 107.1(13) . . ? F34 C78 C66 109.2(16) . . ? O4 C66B C78B 100.7(17) . . ? O4 C66B C77B 112.8(18) . . ? C78B C66B C77B 108.2(16) . . ? O4 C66B C76B 118.0(18) . . ? C78B C66B C76B 108.7(17) . . ? C77B C66B C76B 107.8(18) . . ? F29B C76B F28B 110.0(14) . . ? F29B C76B F30B 107.7(13) . . ? F28B C76B F30B 107.0(14) . . ? F29B C76B C66B 110.4(14) . . ? F28B C76B C66B 111(2) . . ? F30B C76B C66B 110.9(13) . . ? F33B C77B F32B 106.6(12) . . ? F33B C77B F31B 105.2(12) . . ? F32B C77B F31B 105.8(12) . . ? F33B C77B C66B 113.4(13) . . ? F32B C77B C66B 111.2(13) . . ? F31B C77B C66B 114.0(19) . . ? F34B C78B F35B 106.5(11) . . ? F34B C78B F36B 109.0(13) . . ? F35B C78B F36B 105.4(13) . . ? F34B C78B C66B 114.5(18) . . ? F35B C78B C66B 109.9(14) . . ? F36B C78B C66B 111.0(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C13 H13 N4 0.9500 2.6000 3.531(8) 166.00 . yes C29 H29A F12B 0.9900 2.4100 3.01(2) 119.00 3_566 yes C37 H37 N2 0.9500 2.5900 3.509(8) 162.00 . yes C53 H53 F2 0.9500 2.4100 3.131(16) 133.00 4_454 yes # start Validation Reply Form _vrf_PLAT308_sw139 ; PROBLEM: Single Bonded Metal Atom (Unusual !) ........... Tl1 RESPONSE: There are rather long coordinative bonds between P1, P2, N1, N3 and the Tl(I) cation. Additionally, the thallium cation is pi-coordinated by one of the toluene solvent molecules. ; _vrf_PLAT083_sw139 ; PROBLEM: SHELXL Second Parameter in WGHT unusually Large. 58.00 RESPONSE: Possibly a result of the weak diffraction at high theta angles and/or a strong disorder of the counterion. ; # end Validation Reply Form #===END # Attachment 'sw141.cif' # CIF-file generated for sw141 R = 0.04 #============================================================================== data_sw141 _database_code_depnum_ccdc_archive 'CCDC 713905' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H21 N2 P)2, Tl2, (F6 P)2' _chemical_formula_structural ? _chemical_formula_sum 'C48 H42 F12 N4 P4 Tl2' _chemical_formula_iupac ? _chemical_formula_weight 1435.50 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Tl Tl -4.1627 8.0900 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 10.8581(2) _cell_length_b 12.5163(2) _cell_length_c 18.3704(3) _cell_angle_alpha 91.335(2) _cell_angle_beta 91.937(2) _cell_angle_gamma 102.785(2) _cell_volume 2432.10(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 26549 _cell_measurement_theta_min 2.4046 _cell_measurement_theta_max 66.5006 _cell_special_details ; ; _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 14.583 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.00248 _exptl_absorpt_correction_T_max 0.41700 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 10.00 63.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -11.6137 45.0000 210.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 2 omega 33.00 86.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 11.6137 45.0000 210.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 3 omega -45.00 13.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -11.6137 77.0000 90.0000 0.0000 0.0000 58 #__ type_ start__ end____ width___ exp.time_ 4 omega -39.00 14.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -11.6137 45.0000 30.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 5 omega -16.00 37.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 11.6137 45.0000 150.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 6 omega -37.00 16.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -11.6137 -45.0000 210.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 7 omega -112.00 -58.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 101.0000 54.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 8 omega -115.00 -62.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 -45.0000 300.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 9 omega -116.00 -12.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 113.0000 172.0000 0.0000 0.0000 104 #__ type_ start__ end____ width___ exp.time_ 10 omega -124.00 -65.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 77.0000 210.0000 0.0000 0.0000 59 #__ type_ start__ end____ width___ exp.time_ 11 omega -114.00 -60.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 108.0000 298.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 12 omega -165.00 -111.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 -45.0000 120.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 13 omega -119.00 -64.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 119.0000 227.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 14 omega -165.00 -111.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 -45.0000 30.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 15 omega -114.00 -56.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 -77.0000 60.0000 0.0000 0.0000 58 #__ type_ start__ end____ width___ exp.time_ 16 omega -115.00 -61.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 112.0000 114.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 17 omega -165.00 -111.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 -45.0000 270.0000 0.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 18 omega 69.00 127.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 -77.0000 240.0000 0.0000 0.0000 58 #__ type_ start__ end____ width___ exp.time_ 19 omega 19.00 72.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 -45.0000 180.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 20 omega 19.00 72.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 -45.0000 210.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 21 omega 60.00 118.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 77.0000 120.0000 0.0000 0.0000 58 #__ type_ start__ end____ width___ exp.time_ 22 omega 69.00 127.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 -77.0000 300.0000 0.0000 0.0000 58 #__ type_ start__ end____ width___ exp.time_ 23 omega 66.00 119.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 45.0000 330.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 24 omega 66.00 119.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 45.0000 180.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 25 omega 114.00 172.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 77.0000 150.0000 0.0000 0.0000 58 #__ type_ start__ end____ width___ exp.time_ 26 omega 69.00 127.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 -77.0000 180.0000 0.0000 0.0000 58 #__ type_ start__ end____ width___ exp.time_ 27 omega 114.00 172.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 93.5000 77.0000 240.0000 0.0000 0.0000 58 #__ type_ start__ end____ width___ exp.time_ 28 omega -178.00 -1.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 0.0000 330.0000 0.0000 0.0000 177 #__ type_ start__ end____ width___ exp.time_ 29 omega -178.00 -1.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 0.0000 150.0000 0.0000 0.0000 177 #__ type_ start__ end____ width___ exp.time_ 30 omega -178.00 -1.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 0.0000 180.0000 0.0000 0.0000 177 #__ type_ start__ end____ width___ exp.time_ 31 omega -178.00 -1.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 0.0000 210.0000 0.0000 0.0000 177 #__ type_ start__ end____ width___ exp.time_ 32 omega -178.00 -1.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 0.0000 0.0000 0.0000 0.0000 177 #__ type_ start__ end____ width___ exp.time_ 33 omega -178.00 -90.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -90.0000 0.0000 30.0000 0.0000 0.0000 88 ; _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 37915 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 66.64 _diffrn_reflns_theta_full 66.64 _diffrn_measured_fraction_theta_max 0.970 _diffrn_measured_fraction_theta_full 0.970 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 8341 # number of observed reflections (> n sig(I)) _reflns_number_gt 7663 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material ; PLATON (Spek, 2003) and SHELXL-97 (Sheldrick, 1997) ; #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0624P)^2^+6.8836P] 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 refU _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 8341 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0963 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.985 _refine_diff_density_min -2.117 _refine_diff_density_rms 0.142 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Tl1 Tl 0.638405(16) 0.895722(14) 0.258180(10) 0.02339(8) Uani 1 1 d . . . Tl2 Tl 0.83545(2) 1.60058(2) 0.251097(14) 0.04282(9) Uani 1 1 d . . . P1 P 0.35974(10) 0.79426(9) 0.21456(6) 0.0163(2) Uani 1 1 d . . . P2 P 0.70878(11) 1.15697(9) 0.29381(6) 0.0186(2) Uani 1 1 d . . . P3 P 0.84912(17) 0.75927(18) 0.07497(10) 0.0545(5) Uani 1 1 d . . . P4 P 0.67067(13) 0.66011(12) 0.42679(8) 0.0348(3) Uani 1 1 d . . . N1 N 0.0748(4) 0.5872(3) 0.3039(2) 0.0235(8) Uani 1 1 d . . . N2 N 0.5203(4) 0.9888(3) 0.1469(2) 0.0199(8) Uani 1 1 d . . . N3 N 0.8759(4) 1.4167(3) 0.1819(2) 0.0266(9) Uani 1 1 d . . . N4 N 0.4998(4) 0.9810(3) 0.3583(2) 0.0216(8) Uani 1 1 d . . . F1 F 0.9281(4) 0.7755(4) 0.1517(2) 0.0733(13) Uani 1 1 d . . . F2 F 0.9615(6) 0.8385(5) 0.0400(3) 0.0953(18) Uani 1 1 d . . . F3 F 0.7702(5) 0.7395(5) -0.0009(2) 0.0821(16) Uani 1 1 d . . . F4 F 0.7375(4) 0.6687(6) 0.1115(3) 0.0957(19) Uani 1 1 d . . . F5 F 0.9099(4) 0.6597(4) 0.0548(2) 0.0643(11) Uani 1 1 d . . . F6 F 0.7795(8) 0.8482(7) 0.0980(4) 0.141(3) Uani 1 1 d . . . F7 F 0.8032(4) 0.6370(5) 0.4030(2) 0.0852(17) Uani 1 1 d . . . F8 F 0.6212(4) 0.6483(4) 0.3431(2) 0.0693(13) Uani 1 1 d . . . F9 F 0.5394(4) 0.6819(3) 0.4499(2) 0.0517(9) Uani 1 1 d . . . F10 F 0.7226(4) 0.6788(4) 0.5089(2) 0.0706(13) Uani 1 1 d . . . F11 F 0.7220(6) 0.7876(4) 0.4152(3) 0.0962(19) Uani 1 1 d . . . F12 F 0.6207(5) 0.5353(4) 0.4369(4) 0.0940(18) Uani 1 1 d . . . C1 C 0.3150(4) 0.9188(4) 0.1904(2) 0.0187(9) Uani 1 1 d . . . C2 C 0.2096(4) 0.9286(4) 0.2250(2) 0.0183(9) Uani 1 1 d . . . C3 C 0.1426(5) 1.0229(4) 0.2185(3) 0.0251(10) Uani 1 1 d . . . H3A H 0.0829 1.0088 0.1757 0.030 Uiso 1 1 calc R . . H3B H 0.2058 1.0915 0.2106 0.030 Uiso 1 1 calc R . . C4 C 0.0707(5) 1.0373(4) 0.2866(3) 0.0296(11) Uani 1 1 d . . . H4A H 0.1314 1.0636 0.3280 0.036 Uiso 1 1 calc R . . H4B H 0.0201 1.0930 0.2783 0.036 Uiso 1 1 calc R . . C5 C -0.0165(5) 0.9291(4) 0.3053(3) 0.0274(11) Uani 1 1 d . . . H5A H -0.0742 0.9006 0.2629 0.033 Uiso 1 1 calc R . . H5B H -0.0685 0.9411 0.3466 0.033 Uiso 1 1 calc R . . C6 C 0.0611(4) 0.8454(4) 0.3256(3) 0.0231(10) Uani 1 1 d . . . H6A H 0.1046 0.8669 0.3736 0.028 Uiso 1 1 calc R . . H6B H 0.0034 0.7728 0.3300 0.028 Uiso 1 1 calc R . . C7 C 0.1585(4) 0.8360(3) 0.2700(2) 0.0175(9) Uani 1 1 d . . . C8 C 0.2188(4) 0.7513(3) 0.2651(2) 0.0176(9) Uani 1 1 d . . . C9 C 0.1942(4) 0.6461(3) 0.3020(2) 0.0183(9) Uani 1 1 d . . . C10 C 0.2961(4) 0.6075(4) 0.3331(3) 0.0223(10) Uani 1 1 d . . . H10 H 0.3802 0.6492 0.3305 0.027 Uiso 1 1 calc R . . C11 C 0.2723(5) 0.5088(4) 0.3674(3) 0.0258(10) Uani 1 1 d . . . H11 H 0.3398 0.4831 0.3900 0.031 Uiso 1 1 calc R . . C12 C 0.1504(5) 0.4476(4) 0.3688(3) 0.0309(11) Uani 1 1 d . . . H12 H 0.1319 0.3785 0.3912 0.037 Uiso 1 1 calc R . . C13 C 0.0560(5) 0.4905(4) 0.3365(3) 0.0304(12) Uani 1 1 d . . . H13 H -0.0283 0.4485 0.3375 0.037 Uiso 1 1 calc R . . C14 C 0.3965(4) 0.9932(3) 0.1425(2) 0.0171(9) Uani 1 1 d . . . C15 C 0.3528(5) 1.0598(4) 0.0924(3) 0.0231(10) Uani 1 1 d . . . H15 H 0.2655 1.0603 0.0885 0.028 Uiso 1 1 calc R . . C16 C 0.4381(5) 1.1255(4) 0.0482(3) 0.0257(10) Uani 1 1 d . . . H16 H 0.4100 1.1723 0.0145 0.031 Uiso 1 1 calc R . . C17 C 0.5643(5) 1.1218(4) 0.0541(3) 0.0272(11) Uani 1 1 d . . . H17 H 0.6244 1.1665 0.0249 0.033 Uiso 1 1 calc R . . C18 C 0.6017(4) 1.0518(4) 0.1033(3) 0.0233(10) Uani 1 1 d . . . H18 H 0.6881 1.0480 0.1064 0.028 Uiso 1 1 calc R . . C19 C 0.3362(4) 0.7132(3) 0.1295(2) 0.0184(9) Uani 1 1 d . . . C20 C 0.2185(5) 0.6892(4) 0.0917(3) 0.0279(11) Uani 1 1 d . . . H20 H 0.1503 0.7172 0.1093 0.033 Uiso 1 1 calc R . . C21 C 0.2027(6) 0.6250(5) 0.0291(3) 0.0387(13) Uani 1 1 d . . . H21 H 0.1226 0.6074 0.0038 0.046 Uiso 1 1 calc R . . C22 C 0.3023(6) 0.5856(4) 0.0022(3) 0.0389(14) Uani 1 1 d . . . H22 H 0.2896 0.5390 -0.0402 0.047 Uiso 1 1 calc R . . C23 C 0.4194(6) 0.6139(4) 0.0370(3) 0.0356(13) Uani 1 1 d . . . H23 H 0.4889 0.5905 0.0170 0.043 Uiso 1 1 calc R . . C24 C 0.4365(5) 0.6763(4) 0.1011(3) 0.0258(10) Uani 1 1 d . . . H24 H 0.5171 0.6939 0.1257 0.031 Uiso 1 1 calc R . . C25 C 0.5483(4) 1.1623(3) 0.3138(2) 0.0189(9) Uani 1 1 d . . . C26 C 0.5122(4) 1.2437(4) 0.2773(2) 0.0196(9) Uani 1 1 d . . . C27 C 0.3864(4) 1.2741(4) 0.2832(3) 0.0237(10) Uani 1 1 d . . . H27A H 0.3891 1.3218 0.3272 0.028 Uiso 1 1 calc R . . H27B H 0.3206 1.2066 0.2895 0.028 Uiso 1 1 calc R . . C28 C 0.3495(5) 1.3333(4) 0.2169(3) 0.0301(11) Uani 1 1 d . . . H28A H 0.2749 1.3635 0.2277 0.036 Uiso 1 1 calc R . . H28B H 0.3264 1.2807 0.1750 0.036 Uiso 1 1 calc R . . C29 C 0.4596(5) 1.4264(4) 0.1975(3) 0.0317(12) Uani 1 1 d . . . H29A H 0.4326 1.4678 0.1570 0.038 Uiso 1 1 calc R . . H29B H 0.4846 1.4776 0.2401 0.038 Uiso 1 1 calc R . . C30 C 0.5719(5) 1.3810(4) 0.1753(3) 0.0251(10) Uani 1 1 d . . . H30A H 0.5517 1.3424 0.1272 0.030 Uiso 1 1 calc R . . H30B H 0.6454 1.4428 0.1698 0.030 Uiso 1 1 calc R . . C31 C 0.6081(4) 1.3025(4) 0.2294(2) 0.0212(9) Uani 1 1 d . . . C32 C 0.7201(4) 1.2727(4) 0.2347(2) 0.0203(9) Uani 1 1 d . . . C33 C 0.8361(4) 1.3095(4) 0.1933(2) 0.0222(10) Uani 1 1 d . . . C34 C 0.9041(5) 1.2339(4) 0.1692(3) 0.0275(11) Uani 1 1 d . . . H34 H 0.8754 1.1582 0.1784 0.033 Uiso 1 1 calc R . . C35 C 1.0137(5) 1.2696(5) 0.1316(3) 0.0333(12) Uani 1 1 d . . . H35 H 1.0602 1.2189 0.1142 0.040 Uiso 1 1 calc R . . C36 C 1.0537(5) 1.3796(5) 0.1200(3) 0.0305(11) Uani 1 1 d . . . H36 H 1.1287 1.4066 0.0948 0.037 Uiso 1 1 calc R . . C37 C 0.9830(5) 1.4498(4) 0.1456(3) 0.0294(11) Uani 1 1 d . . . H37 H 1.0110 1.5258 0.1373 0.035 Uiso 1 1 calc R . . C38 C 0.4782(4) 1.0831(4) 0.3638(3) 0.0197(9) Uani 1 1 d . . . C39 C 0.3967(5) 1.1101(4) 0.4145(3) 0.0262(10) Uani 1 1 d . . . H39 H 0.3839 1.1827 0.4182 0.031 Uiso 1 1 calc R . . C40 C 0.3344(5) 1.0301(5) 0.4594(3) 0.0303(11) Uani 1 1 d . . . H40 H 0.2789 1.0475 0.4945 0.036 Uiso 1 1 calc R . . C41 C 0.3536(5) 0.9247(4) 0.4529(3) 0.0300(12) Uani 1 1 d . . . H41 H 0.3101 0.8679 0.4821 0.036 Uiso 1 1 calc R . . C42 C 0.4378(5) 0.9048(4) 0.4029(3) 0.0273(11) Uani 1 1 d . . . H42 H 0.4533 0.8331 0.3995 0.033 Uiso 1 1 calc R . . C43 C 0.7934(4) 1.2199(4) 0.3778(2) 0.0192(9) Uani 1 1 d . . . C44 C 0.7664(4) 1.3132(4) 0.4098(3) 0.0223(10) Uani 1 1 d . . . H44 H 0.7017 1.3440 0.3887 0.027 Uiso 1 1 calc R . . C45 C 0.8328(5) 1.3619(4) 0.4722(3) 0.0286(11) Uani 1 1 d . . . H45 H 0.8142 1.4261 0.4936 0.034 Uiso 1 1 calc R . . C46 C 0.9268(5) 1.3161(4) 0.5033(3) 0.0317(11) Uani 1 1 d . . . H46 H 0.9728 1.3491 0.5461 0.038 Uiso 1 1 calc R . . C47 C 0.9534(5) 1.2228(5) 0.4722(3) 0.0325(12) Uani 1 1 d . . . H47 H 1.0178 1.1917 0.4935 0.039 Uiso 1 1 calc R . . C48 C 0.8865(4) 1.1740(4) 0.4098(3) 0.0241(10) Uani 1 1 d . . . H48 H 0.9045 1.1093 0.3889 0.029 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl1 0.01635(11) 0.02133(12) 0.03250(13) 0.00155(8) -0.00208(8) 0.00457(7) Tl2 0.03145(14) 0.05269(17) 0.04542(16) -0.02088(11) -0.00929(10) 0.01562(11) P1 0.0138(5) 0.0147(5) 0.0201(6) 0.0035(4) 0.0013(4) 0.0025(4) P2 0.0199(6) 0.0157(5) 0.0195(6) 0.0020(4) 0.0022(4) 0.0021(4) P3 0.0441(9) 0.0858(14) 0.0423(10) -0.0087(9) -0.0019(7) 0.0346(9) P4 0.0247(7) 0.0428(8) 0.0377(8) 0.0116(6) -0.0028(6) 0.0084(6) N1 0.022(2) 0.021(2) 0.026(2) 0.0021(16) 0.0042(16) 0.0007(16) N2 0.0189(19) 0.0175(18) 0.022(2) 0.0029(15) 0.0025(16) 0.0004(15) N3 0.028(2) 0.027(2) 0.021(2) 0.0018(16) 0.0033(17) -0.0012(17) N4 0.022(2) 0.0200(19) 0.020(2) 0.0035(15) -0.0024(16) -0.0012(15) F1 0.049(2) 0.119(4) 0.047(2) -0.024(2) -0.0089(19) 0.012(2) F2 0.118(5) 0.079(4) 0.082(4) 0.022(3) 0.009(3) 0.003(3) F3 0.076(3) 0.143(5) 0.048(3) -0.005(3) -0.013(2) 0.073(3) F4 0.035(2) 0.178(6) 0.063(3) 0.004(3) -0.005(2) 0.002(3) F5 0.055(2) 0.066(3) 0.076(3) -0.010(2) -0.019(2) 0.025(2) F6 0.165(7) 0.186(7) 0.112(5) -0.059(5) -0.017(5) 0.135(6) F7 0.032(2) 0.179(6) 0.053(3) 0.012(3) -0.0009(18) 0.043(3) F8 0.040(2) 0.127(4) 0.046(2) -0.008(2) -0.0116(18) 0.032(2) F9 0.041(2) 0.070(3) 0.051(2) -0.0034(18) -0.0008(17) 0.0286(18) F10 0.055(2) 0.124(4) 0.039(2) 0.017(2) -0.0093(18) 0.034(3) F11 0.113(4) 0.060(3) 0.094(4) 0.032(3) -0.018(3) -0.025(3) F12 0.095(4) 0.038(2) 0.155(5) 0.015(3) 0.033(4) 0.022(2) C1 0.015(2) 0.020(2) 0.021(2) 0.0021(17) -0.0027(18) 0.0038(17) C2 0.017(2) 0.020(2) 0.018(2) -0.0021(17) -0.0018(17) 0.0054(17) C3 0.025(2) 0.020(2) 0.033(3) 0.0051(19) 0.000(2) 0.0091(19) C4 0.031(3) 0.027(3) 0.035(3) 0.004(2) 0.008(2) 0.015(2) C5 0.019(2) 0.030(3) 0.036(3) -0.002(2) 0.007(2) 0.009(2) C6 0.019(2) 0.023(2) 0.026(3) 0.0008(18) 0.0046(19) 0.0025(18) C7 0.013(2) 0.018(2) 0.020(2) -0.0009(17) -0.0018(17) 0.0018(16) C8 0.015(2) 0.020(2) 0.017(2) -0.0023(17) 0.0000(17) 0.0013(17) C9 0.019(2) 0.015(2) 0.020(2) -0.0023(17) 0.0034(18) 0.0018(17) C10 0.023(2) 0.020(2) 0.024(2) -0.0002(18) 0.0027(19) 0.0032(18) C11 0.035(3) 0.021(2) 0.023(3) 0.0040(18) 0.004(2) 0.010(2) C12 0.044(3) 0.021(2) 0.027(3) 0.007(2) 0.008(2) 0.005(2) C13 0.033(3) 0.024(3) 0.028(3) 0.003(2) 0.005(2) -0.009(2) C14 0.018(2) 0.013(2) 0.021(2) -0.0003(16) 0.0011(18) 0.0043(16) C15 0.022(2) 0.020(2) 0.028(3) 0.0032(19) 0.001(2) 0.0047(18) C16 0.036(3) 0.019(2) 0.024(3) 0.0070(18) 0.003(2) 0.009(2) C17 0.031(3) 0.021(2) 0.027(3) 0.0035(19) 0.008(2) -0.003(2) C18 0.019(2) 0.024(2) 0.024(3) 0.0033(19) 0.0001(19) -0.0009(18) C19 0.023(2) 0.013(2) 0.019(2) 0.0036(16) 0.0053(18) 0.0014(17) C20 0.023(2) 0.032(3) 0.024(3) 0.005(2) 0.004(2) -0.003(2) C21 0.039(3) 0.041(3) 0.026(3) 0.002(2) 0.001(2) -0.012(2) C22 0.063(4) 0.021(2) 0.025(3) -0.002(2) 0.015(3) -0.010(2) C23 0.055(4) 0.025(3) 0.032(3) 0.005(2) 0.020(3) 0.015(2) C24 0.032(3) 0.019(2) 0.029(3) 0.0066(19) 0.009(2) 0.010(2) C25 0.019(2) 0.016(2) 0.020(2) 0.0000(17) -0.0007(18) 0.0004(17) C26 0.018(2) 0.017(2) 0.021(2) -0.0011(17) -0.0026(18) 0.0001(17) C27 0.017(2) 0.024(2) 0.031(3) 0.0038(19) 0.0037(19) 0.0057(18) C28 0.026(3) 0.031(3) 0.034(3) 0.003(2) -0.004(2) 0.009(2) C29 0.039(3) 0.025(3) 0.032(3) 0.009(2) -0.001(2) 0.010(2) C30 0.029(3) 0.021(2) 0.023(3) 0.0086(18) -0.001(2) -0.0003(19) C31 0.023(2) 0.018(2) 0.020(2) 0.0012(17) -0.0011(18) -0.0004(18) C32 0.022(2) 0.019(2) 0.018(2) 0.0017(17) -0.0005(18) -0.0007(18) C33 0.021(2) 0.025(2) 0.018(2) 0.0022(18) -0.0038(18) -0.0006(18) C34 0.026(3) 0.026(2) 0.030(3) 0.005(2) 0.003(2) 0.004(2) C35 0.028(3) 0.040(3) 0.033(3) 0.007(2) 0.006(2) 0.010(2) C36 0.021(2) 0.046(3) 0.024(3) 0.007(2) 0.003(2) 0.004(2) C37 0.025(3) 0.032(3) 0.026(3) 0.009(2) 0.002(2) -0.005(2) C38 0.017(2) 0.020(2) 0.020(2) 0.0020(17) -0.0018(18) 0.0019(17) C39 0.025(2) 0.026(2) 0.027(3) 0.006(2) 0.000(2) 0.005(2) C40 0.021(2) 0.044(3) 0.025(3) 0.007(2) 0.006(2) 0.004(2) C41 0.025(3) 0.035(3) 0.022(3) 0.010(2) -0.003(2) -0.012(2) C42 0.027(3) 0.022(2) 0.029(3) 0.008(2) -0.001(2) -0.0027(19) C43 0.019(2) 0.018(2) 0.019(2) 0.0047(17) 0.0034(18) -0.0015(17) C44 0.023(2) 0.020(2) 0.023(2) 0.0027(18) 0.0000(19) 0.0036(18) C45 0.034(3) 0.025(2) 0.024(3) -0.0050(19) 0.006(2) 0.001(2) C46 0.028(3) 0.040(3) 0.022(3) 0.000(2) -0.003(2) -0.004(2) C47 0.024(3) 0.047(3) 0.026(3) 0.009(2) -0.001(2) 0.006(2) C48 0.023(2) 0.026(2) 0.023(2) 0.0039(19) 0.0046(19) 0.0043(19) #=============================================================================== # 10. MOLECULAR GEOMETRY _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 Tl1 N4 2.755(4) . ? Tl1 N2 2.790(4) . ? Tl1 P1 3.0819(11) . ? Tl1 P2 3.2349(11) . ? Tl2 N3 2.731(4) . ? Tl2 N1 2.785(4) 1_665 ? Tl2 N1 13.594(4) . ? P1 C1 1.793(4) . ? P1 C8 1.802(4) . ? P1 C19 1.821(5) . ? P2 C25 1.808(5) . ? P2 C32 1.816(4) . ? P2 C43 1.837(5) . ? P3 F6 1.537(5) . ? P3 F2 1.560(6) . ? P3 F5 1.577(4) . ? P3 F3 1.596(5) . ? P3 F1 1.609(4) . ? P3 F4 1.640(6) . ? P4 F12 1.554(5) . ? P4 F9 1.580(4) . ? P4 F10 1.587(4) . ? P4 F11 1.591(5) . ? P4 F7 1.602(4) . ? P4 F8 1.603(4) . ? N1 C13 1.341(6) . ? N1 C9 1.344(6) . ? N1 Tl2 2.785(4) 1_445 ? N2 C18 1.346(6) . ? N2 C14 1.356(6) . ? N3 C33 1.339(6) . ? N3 C37 1.349(6) . ? N4 C42 1.350(6) . ? N4 C38 1.352(6) . ? C1 C2 1.356(6) . ? C1 C14 1.467(6) . ? C2 C7 1.458(6) . ? C2 C3 1.522(6) . ? C3 C4 1.525(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.525(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.527(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.515(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.368(6) . ? C8 C9 1.470(6) . ? C9 C10 1.411(7) . ? C10 C11 1.377(6) . ? C10 H10 0.9500 . ? C11 C12 1.377(8) . ? C11 H11 0.9500 . ? C12 C13 1.382(8) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.395(6) . ? C15 C16 1.392(7) . ? C15 H15 0.9500 . ? C16 C17 1.382(7) . ? C16 H16 0.9500 . ? C17 C18 1.385(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.386(6) . ? C19 C20 1.403(7) . ? C20 C21 1.372(8) . ? C20 H20 0.9500 . ? C21 C22 1.384(9) . ? C21 H21 0.9500 . ? C22 C23 1.374(9) . ? C22 H22 0.9500 . ? C23 C24 1.382(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.354(6) . ? C25 C38 1.471(6) . ? C26 C31 1.468(6) . ? C26 C27 1.503(6) . ? C27 C28 1.528(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.533(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.519(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.515(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.350(7) . ? C32 C33 1.484(6) . ? C33 C34 1.397(7) . ? C34 C35 1.388(7) . ? C34 H34 0.9500 . ? C35 C36 1.373(8) . ? C35 H35 0.9500 . ? C36 C37 1.374(8) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.391(7) . ? C39 C40 1.386(7) . ? C39 H39 0.9500 . ? C40 C41 1.384(8) . ? C40 H40 0.9500 . ? C41 C42 1.374(8) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.388(7) . ? C43 C48 1.389(7) . ? C44 C45 1.387(7) . ? C44 H44 0.9500 . ? C45 C46 1.390(8) . ? C45 H45 0.9500 . ? C46 C47 1.380(8) . ? C46 H46 0.9500 . ? C47 C48 1.389(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? 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 N4 Tl1 N2 89.40(11) . . ? N4 Tl1 P1 74.72(8) . . ? N2 Tl1 P1 60.93(8) . . ? N4 Tl1 P2 61.30(8) . . ? N2 Tl1 P2 74.30(8) . . ? P1 Tl1 P2 116.30(3) . . ? N3 Tl2 N1 76.48(12) . 1_665 ? N3 Tl2 N1 56.18(9) . . ? N1 Tl2 N1 106.79(9) 1_665 . ? C1 P1 C8 91.5(2) . . ? C1 P1 C19 103.6(2) . . ? C8 P1 C19 107.0(2) . . ? C1 P1 Tl1 97.39(15) . . ? C8 P1 Tl1 133.89(15) . . ? C19 P1 Tl1 114.51(15) . . ? C25 P2 C32 90.6(2) . . ? C25 P2 C43 100.8(2) . . ? C32 P2 C43 102.9(2) . . ? C25 P2 Tl1 93.68(14) . . ? C32 P2 Tl1 131.25(15) . . ? C43 P2 Tl1 123.72(14) . . ? F6 P3 F2 96.0(5) . . ? F6 P3 F5 174.4(5) . . ? F2 P3 F5 89.6(3) . . ? F6 P3 F3 90.8(3) . . ? F2 P3 F3 91.7(3) . . ? F5 P3 F3 89.2(2) . . ? F6 P3 F1 90.4(3) . . ? F2 P3 F1 89.3(3) . . ? F5 P3 F1 89.5(2) . . ? F3 P3 F1 178.4(3) . . ? F6 P3 F4 88.3(5) . . ? F2 P3 F4 175.6(4) . . ? F5 P3 F4 86.1(3) . . ? F3 P3 F4 89.3(3) . . ? F1 P3 F4 89.6(3) . . ? F12 P4 F9 90.1(3) . . ? F12 P4 F10 92.1(3) . . ? F9 P4 F10 90.2(2) . . ? F12 P4 F11 179.1(3) . . ? F9 P4 F11 90.3(3) . . ? F10 P4 F11 88.7(3) . . ? F12 P4 F7 89.5(3) . . ? F9 P4 F7 179.5(3) . . ? F10 P4 F7 90.2(2) . . ? F11 P4 F7 90.1(3) . . ? F12 P4 F8 91.1(3) . . ? F9 P4 F8 89.9(2) . . ? F10 P4 F8 176.8(3) . . ? F11 P4 F8 88.2(3) . . ? F7 P4 F8 89.8(2) . . ? C13 N1 C9 117.6(4) . . ? C13 N1 Tl2 104.3(3) . 1_445 ? C9 N1 Tl2 137.9(3) . 1_445 ? C13 N1 Tl2 146.6(3) . . ? C9 N1 Tl2 33.8(2) . . ? Tl2 N1 Tl2 106.79(8) 1_445 . ? C18 N2 C14 119.1(4) . . ? C18 N2 Tl1 113.6(3) . . ? C14 N2 Tl1 126.0(3) . . ? C33 N3 C37 118.2(4) . . ? C33 N3 Tl2 132.9(3) . . ? C37 N3 Tl2 105.6(3) . . ? C42 N4 C38 117.8(4) . . ? C42 N4 Tl1 112.9(3) . . ? C38 N4 Tl1 129.1(3) . . ? C2 C1 C14 131.2(4) . . ? C2 C1 P1 110.3(3) . . ? C14 C1 P1 118.3(3) . . ? C1 C2 C7 113.8(4) . . ? C1 C2 C3 126.1(4) . . ? C7 C2 C3 120.1(4) . . ? C2 C3 C4 111.7(4) . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 110.6(4) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 110.2(4) . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C7 C6 C5 112.7(4) . . ? C7 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? C7 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C2 114.5(4) . . ? C8 C7 C6 124.6(4) . . ? C2 C7 C6 120.2(4) . . ? C7 C8 C9 129.8(4) . . ? C7 C8 P1 108.9(3) . . ? C9 C8 P1 120.6(3) . . ? N1 C9 C10 121.2(4) . . ? N1 C9 C8 119.2(4) . . ? C10 C9 C8 119.6(4) . . ? C11 C10 C9 119.3(4) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 119.7(5) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 117.5(4) . . ? C11 C12 H12 121.3 . . ? C13 C12 H12 121.3 . . ? N1 C13 C12 124.6(5) . . ? N1 C13 H13 117.7 . . ? C12 C13 H13 117.7 . . ? N2 C14 C15 120.8(4) . . ? N2 C14 C1 114.8(4) . . ? C15 C14 C1 124.2(4) . . ? C16 C15 C14 119.6(4) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 119.0(4) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 C18 118.9(4) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? N2 C18 C17 122.5(4) . . ? N2 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C24 C19 C20 119.4(4) . . ? C24 C19 P1 119.6(4) . . ? C20 C19 P1 120.9(4) . . ? C21 C20 C19 119.5(5) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 120.7(5) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 119.9(5) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.2(5) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 120.1(5) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? C26 C25 C38 130.2(4) . . ? C26 C25 P2 110.6(3) . . ? C38 C25 P2 119.2(3) . . ? C25 C26 C31 113.9(4) . . ? C25 C26 C27 124.9(4) . . ? C31 C26 C27 121.1(4) . . ? C26 C27 C28 113.3(4) . . ? C26 C27 H27A 108.9 . . ? C28 C27 H27A 108.9 . . ? C26 C27 H27B 108.9 . . ? C28 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C27 C28 C29 110.2(4) . . ? C27 C28 H28A 109.6 . . ? C29 C28 H28A 109.6 . . ? C27 C28 H28B 109.6 . . ? C29 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C30 C29 C28 110.5(4) . . ? C30 C29 H29A 109.6 . . ? C28 C29 H29A 109.6 . . ? C30 C29 H29B 109.6 . . ? C28 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C31 C30 C29 113.4(4) . . ? C31 C30 H30A 108.9 . . ? C29 C30 H30A 108.9 . . ? C31 C30 H30B 108.9 . . ? C29 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C32 C31 C26 114.3(4) . . ? C32 C31 C30 126.1(4) . . ? C26 C31 C30 119.3(4) . . ? C31 C32 C33 129.9(4) . . ? C31 C32 P2 110.2(3) . . ? C33 C32 P2 119.3(3) . . ? N3 C33 C34 121.1(4) . . ? N3 C33 C32 118.6(4) . . ? C34 C33 C32 120.3(4) . . ? C35 C34 C33 119.7(5) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C36 C35 C34 118.8(5) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C35 C36 C37 118.6(5) . . ? C35 C36 H36 120.7 . . ? C37 C36 H36 120.7 . . ? N3 C37 C36 123.6(5) . . ? N3 C37 H37 118.2 . . ? C36 C37 H37 118.2 . . ? N4 C38 C39 121.5(4) . . ? N4 C38 C25 115.2(4) . . ? C39 C38 C25 123.3(4) . . ? C40 C39 C38 119.3(5) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C41 C40 C39 119.5(5) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 120.3 . . ? C42 C41 C40 117.8(4) . . ? C42 C41 H41 121.1 . . ? C40 C41 H41 121.1 . . ? N4 C42 C41 124.0(5) . . ? N4 C42 H42 118.0 . . ? C41 C42 H42 118.0 . . ? C44 C43 C48 119.3(4) . . ? C44 C43 P2 121.0(4) . . ? C48 C43 P2 119.7(4) . . ? C45 C44 C43 120.8(4) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C46 119.5(5) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C47 C46 C45 120.0(5) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.3(5) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C43 C48 C47 120.1(5) . . ? C43 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? 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 N4 Tl1 P1 C1 65.03(17) . . . . ? N2 Tl1 P1 C1 -32.98(17) . . . . ? P2 Tl1 P1 C1 18.69(16) . . . . ? N4 Tl1 P1 C8 -34.3(2) . . . . ? N2 Tl1 P1 C8 -132.3(2) . . . . ? P2 Tl1 P1 C8 -80.6(2) . . . . ? N4 Tl1 P1 C19 173.66(17) . . . . ? N2 Tl1 P1 C19 75.64(17) . . . . ? P2 Tl1 P1 C19 127.32(15) . . . . ? N4 Tl1 P2 C25 -30.34(17) . . . . ? N2 Tl1 P2 C25 67.79(17) . . . . ? P1 Tl1 P2 C25 22.37(15) . . . . ? N4 Tl1 P2 C32 -124.4(2) . . . . ? N2 Tl1 P2 C32 -26.3(2) . . . . ? P1 Tl1 P2 C32 -71.7(2) . . . . ? N4 Tl1 P2 C43 75.23(19) . . . . ? N2 Tl1 P2 C43 173.36(19) . . . . ? P1 Tl1 P2 C43 127.94(17) . . . . ? N3 Tl2 N1 C13 82.3(5) . . . . ? N1 Tl2 N1 C13 22.1(6) 1_665 . . . ? N3 Tl2 N1 C9 41.0(5) . . . . ? N1 Tl2 N1 C9 -19.2(5) 1_665 . . . ? N3 Tl2 N1 Tl2 -119.75(14) . . . 1_445 ? N1 Tl2 N1 Tl2 180.0 1_665 . . 1_445 ? N4 Tl1 N2 C18 126.8(3) . . . . ? P1 Tl1 N2 C18 -160.4(3) . . . . ? P2 Tl1 N2 C18 66.5(3) . . . . ? N4 Tl1 N2 C14 -39.8(3) . . . . ? P1 Tl1 N2 C14 33.0(3) . . . . ? P2 Tl1 N2 C14 -100.1(3) . . . . ? N1 Tl2 N3 C33 101.0(4) 1_665 . . . ? N1 Tl2 N3 C33 -20.2(4) . . . . ? N1 Tl2 N3 C37 -57.6(3) 1_665 . . . ? N1 Tl2 N3 C37 -178.9(4) . . . . ? N2 Tl1 N4 C42 127.5(3) . . . . ? P1 Tl1 N4 C42 67.6(3) . . . . ? P2 Tl1 N4 C42 -160.1(3) . . . . ? N2 Tl1 N4 C38 -46.1(4) . . . . ? P1 Tl1 N4 C38 -106.1(4) . . . . ? P2 Tl1 N4 C38 26.2(3) . . . . ? C8 P1 C1 C2 6.0(4) . . . . ? C19 P1 C1 C2 113.8(4) . . . . ? Tl1 P1 C1 C2 -128.7(3) . . . . ? C8 P1 C1 C14 -177.2(4) . . . . ? C19 P1 C1 C14 -69.4(4) . . . . ? Tl1 P1 C1 C14 48.1(4) . . . . ? C14 C1 C2 C7 -178.1(5) . . . . ? P1 C1 C2 C7 -1.9(5) . . . . ? C14 C1 C2 C3 3.7(8) . . . . ? P1 C1 C2 C3 180.0(4) . . . . ? C1 C2 C3 C4 -153.4(5) . . . . ? C7 C2 C3 C4 28.6(6) . . . . ? C2 C3 C4 C5 -52.4(6) . . . . ? C3 C4 C5 C6 64.7(6) . . . . ? C4 C5 C6 C7 -50.1(6) . . . . ? C1 C2 C7 C8 -5.1(6) . . . . ? C3 C2 C7 C8 173.1(4) . . . . ? C1 C2 C7 C6 165.5(4) . . . . ? C3 C2 C7 C6 -16.2(6) . . . . ? C5 C6 C7 C8 -163.7(4) . . . . ? C5 C6 C7 C2 26.6(6) . . . . ? C2 C7 C8 C9 179.9(4) . . . . ? C6 C7 C8 C9 9.6(8) . . . . ? C2 C7 C8 P1 9.4(5) . . . . ? C6 C7 C8 P1 -160.9(4) . . . . ? C1 P1 C8 C7 -8.7(3) . . . . ? C19 P1 C8 C7 -113.4(3) . . . . ? Tl1 P1 C8 C7 93.1(3) . . . . ? C1 P1 C8 C9 179.8(4) . . . . ? C19 P1 C8 C9 75.1(4) . . . . ? Tl1 P1 C8 C9 -78.5(4) . . . . ? C13 N1 C9 C10 0.1(7) . . . . ? Tl2 N1 C9 C10 -176.0(3) 1_445 . . . ? Tl2 N1 C9 C10 155.9(7) . . . . ? C13 N1 C9 C8 178.5(4) . . . . ? Tl2 N1 C9 C8 2.3(7) 1_445 . . . ? Tl2 N1 C9 C8 -25.8(3) . . . . ? C7 C8 C9 N1 46.8(7) . . . . ? P1 C8 C9 N1 -143.7(4) . . . . ? C7 C8 C9 C10 -134.8(5) . . . . ? P1 C8 C9 C10 34.7(6) . . . . ? N1 C9 C10 C11 -1.4(7) . . . . ? C8 C9 C10 C11 -179.8(4) . . . . ? C9 C10 C11 C12 2.1(7) . . . . ? C10 C11 C12 C13 -1.4(7) . . . . ? C9 N1 C13 C12 0.5(8) . . . . ? Tl2 N1 C13 C12 177.9(4) 1_445 . . . ? Tl2 N1 C13 C12 -23.9(9) . . . . ? C11 C12 C13 N1 0.1(8) . . . . ? C18 N2 C14 C15 1.5(7) . . . . ? Tl1 N2 C14 C15 167.4(3) . . . . ? C18 N2 C14 C1 178.0(4) . . . . ? Tl1 N2 C14 C1 -16.1(5) . . . . ? C2 C1 C14 N2 147.6(5) . . . . ? P1 C1 C14 N2 -28.4(5) . . . . ? C2 C1 C14 C15 -36.0(8) . . . . ? P1 C1 C14 C15 148.0(4) . . . . ? N2 C14 C15 C16 -2.3(7) . . . . ? C1 C14 C15 C16 -178.4(4) . . . . ? C14 C15 C16 C17 1.1(7) . . . . ? C15 C16 C17 C18 0.7(7) . . . . ? C14 N2 C18 C17 0.4(7) . . . . ? Tl1 N2 C18 C17 -167.2(4) . . . . ? C16 C17 C18 N2 -1.5(8) . . . . ? C1 P1 C19 C24 122.6(4) . . . . ? C8 P1 C19 C24 -141.5(3) . . . . ? Tl1 P1 C19 C24 17.8(4) . . . . ? C1 P1 C19 C20 -56.3(4) . . . . ? C8 P1 C19 C20 39.6(4) . . . . ? Tl1 P1 C19 C20 -161.1(3) . . . . ? C24 C19 C20 C21 3.2(7) . . . . ? P1 C19 C20 C21 -177.9(4) . . . . ? C19 C20 C21 C22 -1.3(7) . . . . ? C20 C21 C22 C23 -2.3(8) . . . . ? C21 C22 C23 C24 3.8(8) . . . . ? C22 C23 C24 C19 -1.8(7) . . . . ? C20 C19 C24 C23 -1.7(6) . . . . ? P1 C19 C24 C23 179.4(3) . . . . ? C32 P2 C25 C26 0.7(4) . . . . ? C43 P2 C25 C26 104.0(4) . . . . ? Tl1 P2 C25 C26 -130.7(3) . . . . ? C32 P2 C25 C38 -179.5(4) . . . . ? C43 P2 C25 C38 -76.3(4) . . . . ? Tl1 P2 C25 C38 49.1(4) . . . . ? C38 C25 C26 C31 -177.3(4) . . . . ? P2 C25 C26 C31 2.5(5) . . . . ? C38 C25 C26 C27 2.6(8) . . . . ? P2 C25 C26 C27 -177.7(4) . . . . ? C25 C26 C27 C28 -156.7(5) . . . . ? C31 C26 C27 C28 23.1(6) . . . . ? C26 C27 C28 C29 -48.6(6) . . . . ? C27 C28 C29 C30 63.5(6) . . . . ? C28 C29 C30 C31 -50.7(6) . . . . ? C25 C26 C31 C32 -5.8(6) . . . . ? C27 C26 C31 C32 174.3(4) . . . . ? C25 C26 C31 C30 168.9(4) . . . . ? C27 C26 C31 C30 -11.0(7) . . . . ? C29 C30 C31 C32 -161.3(5) . . . . ? C29 C30 C31 C26 24.7(6) . . . . ? C26 C31 C32 C33 176.9(4) . . . . ? C30 C31 C32 C33 2.6(8) . . . . ? C26 C31 C32 P2 6.1(5) . . . . ? C30 C31 C32 P2 -168.2(4) . . . . ? C25 P2 C32 C31 -3.9(4) . . . . ? C43 P2 C32 C31 -105.1(4) . . . . ? Tl1 P2 C32 C31 91.5(4) . . . . ? C25 P2 C32 C33 -175.8(4) . . . . ? C43 P2 C32 C33 83.0(4) . . . . ? Tl1 P2 C32 C33 -80.4(4) . . . . ? C37 N3 C33 C34 0.8(7) . . . . ? Tl2 N3 C33 C34 -155.8(4) . . . . ? C37 N3 C33 C32 178.5(4) . . . . ? Tl2 N3 C33 C32 21.9(6) . . . . ? C31 C32 C33 N3 44.2(7) . . . . ? P2 C32 C33 N3 -145.7(4) . . . . ? C31 C32 C33 C34 -138.0(5) . . . . ? P2 C32 C33 C34 32.1(6) . . . . ? N3 C33 C34 C35 -1.1(7) . . . . ? C32 C33 C34 C35 -178.8(5) . . . . ? C33 C34 C35 C36 1.0(8) . . . . ? C34 C35 C36 C37 -0.5(8) . . . . ? C33 N3 C37 C36 -0.3(8) . . . . ? Tl2 N3 C37 C36 162.1(4) . . . . ? C35 C36 C37 N3 0.1(8) . . . . ? C42 N4 C38 C39 1.1(7) . . . . ? Tl1 N4 C38 C39 174.6(3) . . . . ? C42 N4 C38 C25 -180.0(4) . . . . ? Tl1 N4 C38 C25 -6.5(6) . . . . ? C26 C25 C38 N4 142.3(5) . . . . ? P2 C25 C38 N4 -37.4(5) . . . . ? C26 C25 C38 C39 -38.8(8) . . . . ? P2 C25 C38 C39 141.5(4) . . . . ? N4 C38 C39 C40 -1.2(7) . . . . ? C25 C38 C39 C40 180.0(5) . . . . ? C38 C39 C40 C41 -0.4(8) . . . . ? C39 C40 C41 C42 1.9(7) . . . . ? C38 N4 C42 C41 0.5(7) . . . . ? Tl1 N4 C42 C41 -173.9(4) . . . . ? C40 C41 C42 N4 -2.1(8) . . . . ? C25 P2 C43 C44 -43.7(4) . . . . ? C32 P2 C43 C44 49.5(4) . . . . ? Tl1 P2 C43 C44 -145.5(3) . . . . ? C25 P2 C43 C48 136.8(4) . . . . ? C32 P2 C43 C48 -130.1(4) . . . . ? Tl1 P2 C43 C48 34.9(4) . . . . ? C48 C43 C44 C45 1.2(7) . . . . ? P2 C43 C44 C45 -178.4(4) . . . . ? C43 C44 C45 C46 -0.5(7) . . . . ? C44 C45 C46 C47 -0.1(7) . . . . ? C45 C46 C47 C48 -0.1(8) . . . . ? C44 C43 C48 C47 -1.3(7) . . . . ? P2 C43 C48 C47 178.2(4) . . . . ? C46 C47 C48 C43 0.8(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C5 H5A F1 0.9900 2.5500 3.338(7) 136.00 1_455 yes C16 H16 F3 0.9500 2.4600 3.218(8) 137.00 2_675 yes C24 H24 F4 0.9500 2.5000 3.290(7) 140.00 . yes C30 H30B N3 0.9900 2.6000 3.229(7) 122.00 . yes C34 H34 P2 0.9500 2.8300 3.193(6) 104.00 . yes C42 H42 F9 0.9500 2.4700 3.340(6) 152.00 . yes C46 H46 F7 0.9500 2.5400 3.279(7) 134.00 2_776 yes # start Validation Reply Form _vrf_PLAT307_sw141 ; PROBLEM: Isolated Metal Atom (Unusual !) ................ Tl2 RESPONSE: The Tl2 ions are part of a coordination polymer and show in the polymeric strands two long coordinative bonds to the neighbouring phosphole ligands accompanied by weak contacts to the PF6- counter ions. ; _vrf_PLAT780_sw141 ; PROBLEM: Coordinates do not Form a Properly Connected Set ? RESPONSE: A consequence of the orientation of the repeating units in the unit cell of the polymeric structure. ; # end Validation Reply Form #===END