Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Lawrence Dahl' _publ_contact_author_address ; Department of Chemistry University of Wisconsin-Madison Madison WI 53706 UNITED STATES OF AMERICA ; _publ_contact_author_email DAHL@CHEM.WISC.EDU _publ_section_title ; Phosphine-ligated induced formation of thallium(I) "full" Pt3TlPt3 sandwich versus "open-face" TlPt3 sandwich with triangular Pt3(\m2-CO)3(PR3)3 units: synthesis and structural / spectroscopic analysis of triphenylphosphine [(\m3-Tl)Pt3(\m2-CO)3(PPh3)3]+ and its (\m3-AuPPh3) analogue. ; loop_ _publ_author_name 'Lawrence Dahl' 'N.de Silva' 'Charles G. Fry' data_dahl218 _database_code_depnum_ccdc_archive 'CCDC 274946' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'TlPt3 triphenylphosphine cluster' _chemical_melting_point ? _chemical_formula_moiety '[TlPt3(CO)3(PPh3)3][PF6].2THF' _chemical_formula_sum 'C65 H61 F6 O5 P4 Pt3 Tl' _chemical_formula_weight 1949.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5297(15) _cell_length_b 14.7786(17) _cell_length_c 16.4101(18) _cell_angle_alpha 89.065(2) _cell_angle_beta 74.643(2) _cell_angle_gamma 84.216(2) _cell_volume 3147.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red/orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 9.365 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20213 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 23.30 _reflns_number_total 9024 _reflns_number_gt 7837 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; " C52 was refined with isotropic thermal parameters " Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+5.1575P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9024 _refine_ls_number_parameters 752 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 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 F3 F 0.1756(5) 0.2133(4) 0.0018(4) 0.0443(17) Uani 1 1 d . . . P4 P 0.2404(2) 0.2705(2) -0.07304(16) 0.0306(7) Uani 1 1 d . . . F4 F 0.2731(5) 0.1815(4) -0.1313(4) 0.0518(18) Uani 1 1 d . . . F2 F 0.2091(5) 0.3591(4) -0.0133(4) 0.0449(17) Uani 1 1 d . . . F6 F 0.1421(5) 0.2938(5) -0.1068(4) 0.0462(17) Uani 1 1 d . . . F5 F 0.3072(5) 0.3282(5) -0.1473(4) 0.0484(18) Uani 1 1 d . . . Pt1 Pt 0.18499(3) 0.10092(2) 0.27701(2) 0.01267(11) Uani 1 1 d . . . Pt3 Pt 0.10751(2) 0.27411(2) 0.31108(2) 0.01165(11) Uani 1 1 d . . . Pt2 Pt 0.28934(3) 0.21260(2) 0.33976(2) 0.01210(11) Uani 1 1 d . . . Tl Tl 0.28331(3) 0.24053(3) 0.15228(2) 0.02427(12) Uani 1 1 d . . . P2 P 0.43465(17) 0.24186(15) 0.37639(14) 0.0137(5) Uani 1 1 d . . . P1 P 0.15998(18) -0.04086(15) 0.24232(15) 0.0154(5) Uani 1 1 d . . . P3 P -0.03035(17) 0.37822(15) 0.31403(14) 0.0126(5) Uani 1 1 d . . . F1 F 0.3411(5) 0.2494(5) -0.0388(4) 0.055(2) Uani 1 1 d . . . C30 C 0.5554(6) 0.1727(6) 0.3250(5) 0.015(2) Uani 1 1 d . . . C41 C 0.5224(7) 0.4009(6) 0.4041(6) 0.017(2) Uani 1 1 d . . . H41 H 0.5338 0.3725 0.4522 0.021 Uiso 1 1 calc R . . C45 C 0.3972(7) 0.2217(6) 0.6643(6) 0.024(2) Uani 1 1 d . . . H45 H 0.3895 0.2197 0.7223 0.029 Uiso 1 1 calc R . . C54 C -0.1401(6) 0.3621(6) 0.4061(5) 0.013(2) Uani 1 1 d . . . C60 C -0.0171(6) 0.5003(6) 0.3182(5) 0.015(2) Uani 1 1 d . . . C43 C 0.4959(7) 0.1816(6) 0.5228(6) 0.022(2) Uani 1 1 d . . . H43 H 0.5549 0.1523 0.4867 0.027 Uiso 1 1 calc R . . C36 C 0.4711(6) 0.3582(6) 0.3548(6) 0.017(2) Uani 1 1 d . . . C31 C 0.6390(7) 0.2115(7) 0.2755(6) 0.023(2) Uani 1 1 d . . . H31 H 0.6355 0.2743 0.2692 0.027 Uiso 1 1 calc R . . C42 C 0.4222(7) 0.2286(6) 0.4900(6) 0.015(2) Uani 1 1 d . . . C24 C 0.2675(7) -0.1297(6) 0.2333(5) 0.016(2) Uani 1 1 d . . . C52 C -0.2234(8) 0.3925(7) 0.1576(6) 0.027(2) Uiso 1 1 d . . . H52 H -0.2935 0.4050 0.1621 0.033 Uiso 1 1 calc R . . C39 C 0.5395(7) 0.5276(6) 0.3101(6) 0.020(2) Uani 1 1 d . . . H39 H 0.5621 0.5844 0.2949 0.024 Uiso 1 1 calc R . . C48 C -0.0833(7) 0.3712(5) 0.2228(5) 0.015(2) Uani 1 1 d . . . C44 C 0.4825(8) 0.1778(7) 0.6099(6) 0.028(2) Uani 1 1 d . . . H44 H 0.5322 0.1451 0.6314 0.033 Uiso 1 1 calc R . . C58 C -0.2766(7) 0.4157(7) 0.5281(6) 0.022(2) Uani 1 1 d . . . H58 H -0.3125 0.4632 0.5637 0.026 Uiso 1 1 calc R . . C46 C 0.3225(8) 0.2690(7) 0.6322(6) 0.028(2) Uani 1 1 d . . . H46 H 0.2641 0.2985 0.6689 0.034 Uiso 1 1 calc R . . C53 C -0.1879(7) 0.3911(6) 0.2293(6) 0.022(2) Uani 1 1 d . . . H53 H -0.2340 0.4035 0.2819 0.027 Uiso 1 1 calc R . . C59 C -0.1946(7) 0.4323(6) 0.4588(6) 0.021(2) Uani 1 1 d . . . H59 H -0.1766 0.4913 0.4482 0.025 Uiso 1 1 calc R . . C12 C 0.1274(7) -0.0570(6) 0.1429(6) 0.018(2) Uani 1 1 d . . . C32 C 0.7285(8) 0.1583(7) 0.2351(7) 0.031(3) Uani 1 1 d . . . H32 H 0.7852 0.1852 0.2030 0.037 Uiso 1 1 calc R . . C23 C 0.0714(8) -0.1030(6) 0.4042(6) 0.025(2) Uani 1 1 d . . . H23 H 0.1384 -0.1093 0.4098 0.030 Uiso 1 1 calc R . . C40 C 0.5564(7) 0.4853(6) 0.3821(6) 0.022(2) Uani 1 1 d . . . H40 H 0.5906 0.5136 0.4154 0.026 Uiso 1 1 calc R . . C35 C 0.5620(7) 0.0774(7) 0.3336(6) 0.024(2) Uani 1 1 d . . . H35 H 0.5065 0.0502 0.3675 0.029 Uiso 1 1 calc R . . C64 C 0.0257(7) 0.6254(6) 0.3912(6) 0.021(2) Uani 1 1 d . . . H64 H 0.0510 0.6470 0.4338 0.025 Uiso 1 1 calc R . . C57 C -0.3035(7) 0.3289(7) 0.5428(6) 0.025(2) Uani 1 1 d . . . H57 H -0.3582 0.3176 0.5885 0.030 Uiso 1 1 calc R . . C49 C -0.0153(7) 0.3544(6) 0.1438(6) 0.022(2) Uani 1 1 d . . . H49 H 0.0547 0.3415 0.1389 0.026 Uiso 1 1 calc R . . C55 C -0.1685(7) 0.2744(6) 0.4216(6) 0.023(2) Uani 1 1 d . . . H55 H -0.1330 0.2268 0.3859 0.027 Uiso 1 1 calc R . . C18 C 0.0530(7) -0.0750(6) 0.3278(5) 0.016(2) Uani 1 1 d . . . C65 C 0.0207(7) 0.5331(6) 0.3830(5) 0.016(2) Uani 1 1 d . . . H65 H 0.0423 0.4927 0.4203 0.019 Uiso 1 1 calc R . . C33 C 0.7326(7) 0.0639(7) 0.2430(6) 0.030(3) Uani 1 1 d . . . H33 H 0.7916 0.0275 0.2149 0.036 Uiso 1 1 calc R . . C51 C -0.1556(8) 0.3755(8) 0.0800(6) 0.033(3) Uani 1 1 d . . . H51 H -0.1799 0.3766 0.0320 0.040 Uiso 1 1 calc R . . O5 O 0.3253(5) 0.4166(4) 0.1418(4) 0.0261(16) Uani 1 1 d . . . O2 O 0.1992(5) 0.3976(4) 0.4143(5) 0.0303(17) Uani 1 1 d . . . O3 O -0.0255(5) 0.1503(4) 0.2443(4) 0.0239(15) Uani 1 1 d . . . O1 O 0.3370(5) 0.0093(4) 0.3675(4) 0.0260(16) Uani 1 1 d . . . O4 O 0.4859(6) 0.2081(5) 0.1275(5) 0.0407(19) Uani 1 1 d . . . C37 C 0.4542(7) 0.4010(6) 0.2829(6) 0.017(2) Uani 1 1 d . . . H37 H 0.4199 0.3732 0.2496 0.020 Uiso 1 1 calc R . . C62 C -0.0412(7) 0.6544(6) 0.2704(6) 0.021(2) Uani 1 1 d . . . H62 H -0.0600 0.6952 0.2321 0.025 Uiso 1 1 calc R . . C8 C 0.2420(7) 0.4801(7) 0.1865(6) 0.030(3) Uani 1 1 d . . . H8A H 0.2614 0.5116 0.2304 0.036 Uiso 1 1 calc R . . H8B H 0.1815 0.4492 0.2121 0.036 Uiso 1 1 calc R . . C61 C -0.0473(7) 0.5613(6) 0.2621(6) 0.017(2) Uani 1 1 d . . . H61 H -0.0717 0.5401 0.2188 0.020 Uiso 1 1 calc R . . C38 C 0.4891(7) 0.4852(6) 0.2614(6) 0.020(2) Uani 1 1 d . . . H38 H 0.4782 0.5137 0.2131 0.024 Uiso 1 1 calc R . . C1 C 0.3033(7) 0.0700(7) 0.3341(6) 0.019(2) Uani 1 1 d . . . C28 C 0.4496(7) -0.1720(7) 0.1808(6) 0.024(2) Uani 1 1 d . . . H28 H 0.5154 -0.1555 0.1564 0.029 Uiso 1 1 calc R . . C47 C 0.3343(7) 0.2727(6) 0.5458(6) 0.025(2) Uani 1 1 d . . . H47 H 0.2838 0.3045 0.5247 0.030 Uiso 1 1 calc R . . C26 C 0.3369(8) -0.2856(6) 0.2378(6) 0.027(2) Uani 1 1 d . . . H26 H 0.3271 -0.3458 0.2519 0.032 Uiso 1 1 calc R . . C11 C 0.3798(8) 0.4569(7) 0.0641(6) 0.032(3) Uani 1 1 d . . . H11A H 0.3743 0.4229 0.0157 0.038 Uiso 1 1 calc R . . H11B H 0.4521 0.4571 0.0620 0.038 Uiso 1 1 calc R . . C27 C 0.4350(8) -0.2626(7) 0.2007(6) 0.026(2) Uani 1 1 d . . . H27 H 0.4907 -0.3070 0.1891 0.031 Uiso 1 1 calc R . . C50 C -0.0512(8) 0.3566(7) 0.0721(6) 0.027(2) Uani 1 1 d . . . H50 H -0.0055 0.3455 0.0191 0.032 Uiso 1 1 calc R . . C29 C 0.3664(7) -0.1073(6) 0.1974(6) 0.022(2) Uani 1 1 d . . . H29 H 0.3768 -0.0469 0.1841 0.027 Uiso 1 1 calc R . . C16 C 0.1386(8) -0.0123(7) 0.0003(6) 0.030(3) Uani 1 1 d . . . H16 H 0.1586 0.0286 -0.0433 0.036 Uiso 1 1 calc R . . C25 C 0.2527(7) -0.2205(6) 0.2543(6) 0.023(2) Uani 1 1 d . . . H25 H 0.1870 -0.2369 0.2792 0.027 Uiso 1 1 calc R . . C2 C 0.2003(7) 0.3357(6) 0.3719(6) 0.019(2) Uani 1 1 d . . . C63 C -0.0067(7) 0.6852(6) 0.3363(6) 0.019(2) Uani 1 1 d . . . H63 H -0.0056 0.7473 0.3435 0.022 Uiso 1 1 calc R . . C17 C 0.1531(8) 0.0047(7) 0.0786(6) 0.025(2) Uani 1 1 d . . . H17 H 0.1802 0.0577 0.0881 0.030 Uiso 1 1 calc R . . C19 C -0.0475(8) -0.0619(6) 0.3204(7) 0.027(2) Uani 1 1 d . . . H19 H -0.0599 -0.0401 0.2702 0.032 Uiso 1 1 calc R . . C56 C -0.2497(7) 0.2576(7) 0.4901(6) 0.026(2) Uani 1 1 d . . . H56 H -0.2681 0.1987 0.5007 0.031 Uiso 1 1 calc R . . C13 C 0.0825(8) -0.1353(7) 0.1290(6) 0.028(2) Uani 1 1 d . . . H13 H 0.0636 -0.1767 0.1722 0.033 Uiso 1 1 calc R . . C3 C 0.0487(7) 0.1659(6) 0.2626(6) 0.016(2) Uani 1 1 d . . . C9 C 0.2212(8) 0.5462(7) 0.1195(7) 0.036(3) Uani 1 1 d . . . H9A H 0.1897 0.6048 0.1440 0.043 Uiso 1 1 calc R . . H9B H 0.1777 0.5223 0.0883 0.043 Uiso 1 1 calc R . . C22 C -0.0097(8) -0.1217(7) 0.4721(6) 0.029(2) Uani 1 1 d . . . H22 H 0.0026 -0.1407 0.5232 0.034 Uiso 1 1 calc R . . C14 C 0.0667(8) -0.1502(8) 0.0503(7) 0.034(3) Uani 1 1 d . . . H14 H 0.0368 -0.2017 0.0412 0.041 Uiso 1 1 calc R . . C21 C -0.1108(8) -0.1116(7) 0.4630(6) 0.031(3) Uani 1 1 d . . . H21 H -0.1652 -0.1255 0.5078 0.037 Uiso 1 1 calc R . . C20 C -0.1298(8) -0.0812(6) 0.3880(7) 0.029(3) Uani 1 1 d . . . H20 H -0.1968 -0.0736 0.3826 0.035 Uiso 1 1 calc R . . C15 C 0.0948(8) -0.0893(8) -0.0146(7) 0.039(3) Uani 1 1 d . . . H15 H 0.0845 -0.0998 -0.0673 0.047 Uiso 1 1 calc R . . C7 C 0.5141(9) 0.1105(7) 0.1180(7) 0.043(3) Uani 1 1 d . . . H7A H 0.4532 0.0786 0.1248 0.052 Uiso 1 1 calc R . . H7B H 0.5491 0.0886 0.1601 0.052 Uiso 1 1 calc R . . C4 C 0.5571(9) 0.2524(8) 0.0608(7) 0.042(3) Uani 1 1 d . . . H4A H 0.5863 0.2999 0.0842 0.050 Uiso 1 1 calc R . . H4B H 0.5221 0.2795 0.0205 0.050 Uiso 1 1 calc R . . C6 C 0.5829(10) 0.0955(9) 0.0323(8) 0.054(4) Uani 1 1 d . . . H6A H 0.5443 0.0903 -0.0092 0.064 Uiso 1 1 calc R . . H6B H 0.6309 0.0415 0.0294 0.064 Uiso 1 1 calc R . . C34 C 0.6492(8) 0.0246(7) 0.2926(7) 0.031(3) Uani 1 1 d . . . H34 H 0.6524 -0.0383 0.2981 0.037 Uiso 1 1 calc R . . C10 C 0.3304(8) 0.5525(7) 0.0636(7) 0.034(3) Uani 1 1 d . . . H10A H 0.3295 0.5711 0.0068 0.041 Uiso 1 1 calc R . . H10B H 0.3659 0.5949 0.0872 0.041 Uiso 1 1 calc R . . C5 C 0.6384(10) 0.1816(8) 0.0195(8) 0.051(3) Uani 1 1 d . . . H5A H 0.6948 0.1767 0.0460 0.061 Uiso 1 1 calc R . . H5B H 0.6649 0.1941 -0.0401 0.061 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 F3 0.039(4) 0.057(4) 0.027(3) 0.010(3) 0.007(3) -0.001(3) P4 0.0244(15) 0.0503(19) 0.0149(14) -0.0023(12) -0.0027(12) 0.0005(13) F4 0.059(5) 0.051(4) 0.034(4) -0.011(3) 0.008(3) -0.003(4) F2 0.033(4) 0.059(4) 0.037(4) -0.018(3) 0.002(3) -0.007(3) F6 0.031(4) 0.086(5) 0.022(3) 0.000(3) -0.010(3) -0.001(3) F5 0.039(4) 0.064(5) 0.034(4) 0.003(3) 0.005(3) -0.010(3) Pt1 0.01233(19) 0.01144(19) 0.0148(2) -0.00133(14) -0.00477(15) -0.00063(14) Pt3 0.01080(19) 0.01157(19) 0.01318(19) -0.00100(14) -0.00433(14) -0.00059(14) Pt2 0.01089(19) 0.01314(19) 0.01289(19) -0.00099(14) -0.00434(14) -0.00070(14) Tl 0.0254(2) 0.0311(2) 0.0157(2) 0.00244(16) -0.00185(16) -0.01003(18) P2 0.0128(12) 0.0140(12) 0.0146(12) 0.0003(9) -0.0042(10) -0.0012(10) P1 0.0150(13) 0.0129(12) 0.0185(13) -0.0014(10) -0.0045(10) -0.0022(10) P3 0.0122(12) 0.0121(12) 0.0140(12) -0.0009(9) -0.0049(10) 0.0005(10) F1 0.029(4) 0.105(6) 0.027(4) -0.011(4) -0.008(3) 0.012(4) C30 0.005(5) 0.022(5) 0.018(5) -0.002(4) -0.008(4) 0.004(4) C41 0.016(5) 0.017(5) 0.018(5) -0.002(4) -0.004(4) 0.003(4) C45 0.030(6) 0.029(6) 0.015(5) 0.000(4) -0.007(5) -0.014(5) C54 0.012(5) 0.016(5) 0.017(5) 0.002(4) -0.013(4) -0.001(4) C60 0.008(5) 0.022(5) 0.016(5) -0.001(4) -0.003(4) -0.005(4) C43 0.021(5) 0.027(6) 0.020(5) 0.001(4) -0.007(4) 0.004(4) C36 0.008(5) 0.021(5) 0.021(5) 0.001(4) -0.003(4) 0.000(4) C31 0.014(5) 0.025(5) 0.029(6) 0.002(4) -0.006(4) -0.001(4) C42 0.021(5) 0.008(4) 0.020(5) -0.002(4) -0.010(4) -0.008(4) C24 0.016(5) 0.018(5) 0.015(5) -0.003(4) -0.005(4) 0.000(4) C39 0.015(5) 0.011(5) 0.032(6) 0.000(4) -0.003(4) 0.000(4) C48 0.022(5) 0.006(4) 0.015(5) 0.004(4) -0.004(4) -0.003(4) C44 0.040(7) 0.030(6) 0.018(6) 0.008(4) -0.016(5) -0.001(5) C58 0.014(5) 0.032(6) 0.020(5) -0.010(4) -0.005(4) -0.001(4) C46 0.025(6) 0.042(6) 0.016(5) -0.006(5) -0.004(5) -0.004(5) C53 0.011(5) 0.034(6) 0.022(5) -0.003(4) -0.007(4) -0.001(4) C59 0.026(6) 0.016(5) 0.022(5) -0.006(4) -0.010(5) -0.002(4) C12 0.019(5) 0.015(5) 0.019(5) -0.006(4) -0.004(4) 0.000(4) C32 0.022(6) 0.032(6) 0.035(6) 0.005(5) -0.002(5) -0.004(5) C23 0.027(6) 0.023(6) 0.028(6) -0.004(4) -0.011(5) -0.003(5) C40 0.011(5) 0.024(5) 0.028(6) -0.005(4) 0.000(4) -0.005(4) C35 0.013(5) 0.030(6) 0.034(6) 0.002(5) -0.013(5) -0.003(4) C64 0.021(5) 0.021(5) 0.024(5) -0.004(4) -0.010(4) -0.004(4) C57 0.012(5) 0.039(6) 0.019(5) 0.006(5) 0.002(4) -0.002(5) C49 0.018(5) 0.028(6) 0.020(5) -0.001(4) -0.009(4) 0.002(4) C55 0.020(5) 0.024(6) 0.022(5) -0.001(4) -0.003(4) 0.002(4) C18 0.013(5) 0.015(5) 0.016(5) -0.007(4) 0.000(4) -0.001(4) C65 0.016(5) 0.015(5) 0.017(5) -0.003(4) -0.005(4) 0.002(4) C33 0.013(5) 0.042(7) 0.029(6) -0.005(5) -0.001(5) 0.011(5) C51 0.031(6) 0.055(7) 0.020(6) 0.004(5) -0.017(5) -0.003(5) O5 0.022(4) 0.033(4) 0.023(4) 0.008(3) -0.006(3) -0.006(3) O2 0.028(4) 0.022(4) 0.046(5) -0.018(4) -0.022(4) 0.012(3) O3 0.021(4) 0.021(4) 0.034(4) -0.004(3) -0.013(3) -0.006(3) O1 0.031(4) 0.020(4) 0.036(4) 0.004(3) -0.025(3) 0.000(3) O4 0.041(5) 0.036(5) 0.037(5) 0.005(4) 0.002(4) -0.002(4) C37 0.017(5) 0.019(5) 0.018(5) 0.001(4) -0.011(4) -0.002(4) C62 0.020(5) 0.016(5) 0.024(5) 0.007(4) -0.004(4) 0.001(4) C8 0.020(6) 0.031(6) 0.030(6) -0.002(5) 0.010(5) -0.004(5) C61 0.012(5) 0.020(5) 0.020(5) 0.003(4) -0.007(4) 0.001(4) C38 0.014(5) 0.021(5) 0.024(5) 0.003(4) -0.002(4) -0.003(4) C1 0.012(5) 0.025(6) 0.023(5) -0.005(4) -0.011(4) 0.004(4) C28 0.016(5) 0.028(6) 0.027(6) -0.003(4) -0.003(4) 0.002(5) C47 0.024(6) 0.027(6) 0.026(6) -0.001(4) -0.010(5) 0.002(5) C26 0.030(6) 0.013(5) 0.038(6) 0.001(4) -0.012(5) 0.002(5) C11 0.025(6) 0.047(7) 0.022(6) 0.000(5) -0.002(5) -0.010(5) C27 0.022(6) 0.024(6) 0.029(6) 0.000(4) -0.006(5) 0.006(5) C50 0.029(6) 0.036(6) 0.016(5) -0.005(4) -0.009(5) 0.001(5) C29 0.020(5) 0.022(5) 0.024(5) 0.001(4) -0.005(4) -0.001(4) C16 0.032(6) 0.041(7) 0.019(6) 0.004(5) -0.009(5) -0.006(5) C25 0.021(5) 0.019(5) 0.027(6) -0.008(4) -0.003(4) -0.002(4) C2 0.015(5) 0.012(5) 0.027(5) -0.001(4) -0.003(4) 0.004(4) C63 0.012(5) 0.013(5) 0.031(6) -0.005(4) -0.004(4) -0.005(4) C17 0.031(6) 0.021(5) 0.022(6) -0.007(4) -0.007(5) -0.002(5) C19 0.027(6) 0.017(5) 0.032(6) 0.007(4) 0.000(5) -0.001(4) C56 0.019(5) 0.021(5) 0.033(6) 0.005(5) 0.000(5) 0.001(4) C13 0.029(6) 0.026(6) 0.029(6) -0.003(5) -0.009(5) -0.006(5) C3 0.018(5) 0.009(5) 0.023(5) 0.003(4) -0.010(4) 0.004(4) C9 0.018(6) 0.039(7) 0.049(7) 0.013(6) -0.009(5) 0.004(5) C22 0.034(6) 0.036(6) 0.014(5) 0.004(4) -0.001(5) -0.011(5) C14 0.026(6) 0.041(7) 0.039(7) -0.014(6) -0.011(5) -0.005(5) C21 0.030(6) 0.025(6) 0.025(6) 0.000(5) 0.015(5) -0.003(5) C20 0.018(6) 0.020(5) 0.045(7) 0.010(5) -0.002(5) 0.004(4) C15 0.030(6) 0.062(8) 0.025(6) -0.019(6) -0.011(5) 0.005(6) C7 0.051(8) 0.018(6) 0.046(7) 0.010(5) 0.009(6) 0.001(5) C4 0.035(7) 0.042(7) 0.043(7) 0.010(6) 0.001(6) -0.011(6) C6 0.053(8) 0.049(8) 0.049(8) -0.010(6) 0.003(7) -0.003(7) C34 0.027(6) 0.023(6) 0.041(7) -0.006(5) -0.009(5) 0.008(5) C10 0.023(6) 0.044(7) 0.033(6) 0.020(5) -0.005(5) -0.005(5) C5 0.048(8) 0.042(8) 0.051(8) -0.002(6) 0.004(6) -0.003(6) _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 F3 P4 1.593(6) . ? F3 Tl 3.232(7) . ? P4 F6 1.578(7) . ? P4 F4 1.593(7) . ? P4 F2 1.602(6) . ? P4 F5 1.602(7) . ? P4 F1 1.607(7) . ? F2 Tl 3.521(7) . ? Pt1 C3 2.061(9) . ? Pt1 C1 2.069(9) . ? Pt1 P1 2.261(2) . ? Pt1 Pt2 2.6596(5) . ? Pt1 Pt3 2.6755(5) . ? Pt1 Tl 3.0314(5) . ? Pt3 C2 2.080(10) . ? Pt3 C3 2.111(9) . ? Pt3 P3 2.286(2) . ? Pt3 Pt2 2.6924(5) . ? Pt3 Tl 3.0357(5) . ? Pt2 C2 2.072(9) . ? Pt2 C1 2.099(10) . ? Pt2 P2 2.285(2) . ? Pt2 Tl 3.1189(6) . ? Tl O4 2.657(8) . ? Tl O5 2.712(6) . ? Tl F1 3.028(6) . ? P2 C42 1.837(9) . ? P2 C36 1.840(9) . ? P2 C30 1.840(9) . ? P1 C12 1.825(9) . ? P1 C24 1.835(9) . ? P1 C18 1.835(9) . ? P3 C48 1.832(9) . ? P3 C60 1.836(9) . ? P3 C54 1.849(9) . ? C30 C31 1.377(13) . ? C30 C35 1.410(13) . ? C41 C40 1.382(12) . ? C41 C36 1.392(13) . ? C45 C44 1.368(14) . ? C45 C46 1.383(14) . ? C54 C59 1.380(12) . ? C54 C55 1.389(12) . ? C60 C61 1.386(12) . ? C60 C65 1.408(12) . ? C43 C42 1.378(13) . ? C43 C44 1.393(13) . ? C36 C37 1.390(12) . ? C31 C32 1.387(13) . ? C42 C47 1.400(13) . ? C24 C29 1.383(12) . ? C24 C25 1.401(13) . ? C52 C51 1.368(14) . ? C52 C53 1.382(14) . ? C39 C38 1.374(13) . ? C39 C40 1.391(13) . ? C48 C49 1.386(13) . ? C48 C53 1.393(12) . ? C58 C57 1.368(13) . ? C58 C59 1.401(13) . ? C46 C47 1.386(13) . ? C12 C17 1.378(13) . ? C12 C13 1.409(13) . ? C32 C33 1.395(14) . ? C23 C22 1.388(13) . ? C23 C18 1.389(13) . ? C35 C34 1.366(14) . ? C64 C63 1.374(13) . ? C64 C65 1.383(12) . ? C57 C56 1.389(13) . ? C49 C50 1.386(13) . ? C55 C56 1.387(13) . ? C18 C19 1.390(13) . ? C33 C34 1.380(14) . ? C51 C50 1.383(14) . ? O5 C8 1.435(11) . ? O5 C11 1.445(11) . ? O2 C2 1.155(10) . ? O3 C3 1.166(10) . ? O1 C1 1.160(11) . ? O4 C4 1.449(12) . ? O4 C7 1.454(12) . ? C37 C38 1.382(12) . ? C62 C63 1.385(13) . ? C62 C61 1.397(12) . ? C8 C9 1.522(14) . ? C28 C29 1.373(13) . ? C28 C27 1.394(13) . ? C26 C27 1.379(14) . ? C26 C25 1.386(14) . ? C11 C10 1.502(15) . ? C16 C17 1.382(14) . ? C16 C15 1.389(15) . ? C19 C20 1.397(14) . ? C13 C14 1.387(14) . ? C9 C10 1.529(14) . ? C22 C21 1.408(15) . ? C14 C15 1.383(16) . ? C21 C20 1.381(15) . ? C7 C6 1.474(16) . ? C4 C5 1.470(16) . ? C6 C5 1.525(16) . ? 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 P4 F3 Tl 102.7(3) . . ? F6 P4 F3 90.2(4) . . ? F6 P4 F4 90.9(4) . . ? F3 P4 F4 90.4(4) . . ? F6 P4 F2 90.2(4) . . ? F3 P4 F2 89.2(3) . . ? F4 P4 F2 178.8(4) . . ? F6 P4 F5 90.8(4) . . ? F3 P4 F5 178.9(4) . . ? F4 P4 F5 90.0(4) . . ? F2 P4 F5 90.4(4) . . ? F6 P4 F1 178.6(5) . . ? F3 P4 F1 90.7(4) . . ? F4 P4 F1 90.1(4) . . ? F2 P4 F1 88.7(4) . . ? F5 P4 F1 88.2(4) . . ? P4 F2 Tl 91.4(3) . . ? C3 Pt1 C1 156.6(4) . . ? C3 Pt1 P1 97.4(3) . . ? C1 Pt1 P1 99.7(3) . . ? C3 Pt1 Pt2 111.5(2) . . ? C1 Pt1 Pt2 50.8(3) . . ? P1 Pt1 Pt2 150.47(6) . . ? C3 Pt1 Pt3 50.9(2) . . ? C1 Pt1 Pt3 109.5(3) . . ? P1 Pt1 Pt3 147.95(6) . . ? Pt2 Pt1 Pt3 60.616(14) . . ? C3 Pt1 Tl 84.2(2) . . ? C1 Pt1 Tl 98.7(3) . . ? P1 Pt1 Tl 124.94(6) . . ? Pt2 Pt1 Tl 66.090(14) . . ? Pt3 Pt1 Tl 63.917(14) . . ? C2 Pt3 C3 156.8(3) . . ? C2 Pt3 P3 106.1(2) . . ? C3 Pt3 P3 95.7(2) . . ? C2 Pt3 Pt1 108.4(2) . . ? C3 Pt3 Pt1 49.3(2) . . ? P3 Pt3 Pt1 144.90(6) . . ? C2 Pt3 Pt2 49.4(2) . . ? C3 Pt3 Pt2 108.7(2) . . ? P3 Pt3 Pt2 155.55(6) . . ? Pt1 Pt3 Pt2 59.400(12) . . ? C2 Pt3 Tl 91.8(2) . . ? C3 Pt3 Tl 83.3(2) . . ? P3 Pt3 Tl 121.37(6) . . ? Pt1 Pt3 Tl 63.750(13) . . ? Pt2 Pt3 Tl 65.660(14) . . ? C2 Pt2 C1 150.5(4) . . ? C2 Pt2 P2 100.4(3) . . ? C1 Pt2 P2 102.6(2) . . ? C2 Pt2 Pt1 109.3(3) . . ? C1 Pt2 Pt1 49.8(2) . . ? P2 Pt2 Pt1 150.37(6) . . ? C2 Pt2 Pt3 49.7(3) . . ? C1 Pt2 Pt3 108.0(2) . . ? P2 Pt2 Pt3 149.22(6) . . ? Pt1 Pt2 Pt3 59.984(14) . . ? C2 Pt2 Tl 89.6(3) . . ? C1 Pt2 Tl 95.4(3) . . ? P2 Pt2 Tl 118.37(6) . . ? Pt1 Pt2 Tl 62.690(12) . . ? Pt3 Pt2 Tl 62.478(12) . . ? O4 Tl O5 83.1(2) . . ? O4 Tl F1 82.7(2) . . ? O5 Tl F1 83.7(2) . . ? O4 Tl Pt1 107.11(15) . . ? O5 Tl Pt1 142.06(14) . . ? F1 Tl Pt1 133.09(15) . . ? O4 Tl Pt3 132.43(16) . . ? O5 Tl Pt3 93.44(14) . . ? F1 Tl Pt3 144.29(12) . . ? Pt1 Tl Pt3 52.333(11) . . ? O4 Tl Pt2 81.30(16) . . ? O5 Tl Pt2 96.59(14) . . ? F1 Tl Pt2 163.85(12) . . ? Pt1 Tl Pt2 51.220(11) . . ? Pt3 Tl Pt2 51.862(12) . . ? O4 Tl F3 121.23(19) . . ? O5 Tl F3 104.94(18) . . ? F1 Tl F3 42.51(16) . . ? Pt1 Tl F3 100.47(11) . . ? Pt3 Tl F3 105.56(10) . . ? Pt2 Tl F3 150.11(10) . . ? O4 Tl F2 114.01(18) . . ? O5 Tl F2 66.45(17) . . ? F1 Tl F2 39.18(16) . . ? Pt1 Tl F2 133.19(10) . . ? Pt3 Tl F2 107.55(9) . . ? Pt2 Tl F2 154.11(10) . . ? F3 Tl F2 38.49(15) . . ? C42 P2 C36 103.8(4) . . ? C42 P2 C30 104.5(4) . . ? C36 P2 C30 102.0(4) . . ? C42 P2 Pt2 112.6(3) . . ? C36 P2 Pt2 114.9(3) . . ? C30 P2 Pt2 117.4(3) . . ? C12 P1 C24 101.0(4) . . ? C12 P1 C18 107.5(4) . . ? C24 P1 C18 106.7(4) . . ? C12 P1 Pt1 118.2(3) . . ? C24 P1 Pt1 117.1(3) . . ? C18 P1 Pt1 105.7(3) . . ? C48 P3 C60 101.6(4) . . ? C48 P3 C54 104.3(4) . . ? C60 P3 C54 103.3(4) . . ? C48 P3 Pt3 114.0(3) . . ? C60 P3 Pt3 120.1(3) . . ? C54 P3 Pt3 111.7(3) . . ? P4 F1 Tl 111.0(3) . . ? C31 C30 C35 118.7(8) . . ? C31 C30 P2 121.6(7) . . ? C35 C30 P2 119.6(7) . . ? C40 C41 C36 120.5(9) . . ? C44 C45 C46 119.4(9) . . ? C59 C54 C55 119.3(8) . . ? C59 C54 P3 123.3(7) . . ? C55 C54 P3 117.3(7) . . ? C61 C60 C65 119.3(8) . . ? C61 C60 P3 122.2(7) . . ? C65 C60 P3 118.5(7) . . ? C42 C43 C44 120.3(9) . . ? C37 C36 C41 119.5(8) . . ? C37 C36 P2 118.4(7) . . ? C41 C36 P2 121.9(7) . . ? C30 C31 C32 120.9(9) . . ? C43 C42 C47 118.8(9) . . ? C43 C42 P2 123.8(7) . . ? C47 C42 P2 117.3(7) . . ? C29 C24 C25 118.9(8) . . ? C29 C24 P1 118.3(7) . . ? C25 C24 P1 122.6(7) . . ? C51 C52 C53 120.0(10) . . ? C38 C39 C40 119.7(8) . . ? C49 C48 C53 119.3(8) . . ? C49 C48 P3 118.3(7) . . ? C53 C48 P3 122.0(7) . . ? C45 C44 C43 120.9(9) . . ? C57 C58 C59 119.4(9) . . ? C45 C46 C47 120.4(9) . . ? C52 C53 C48 120.1(9) . . ? C54 C59 C58 120.7(9) . . ? C17 C12 C13 119.5(9) . . ? C17 C12 P1 119.9(7) . . ? C13 C12 P1 120.4(7) . . ? C31 C32 C33 119.4(9) . . ? C22 C23 C18 120.3(9) . . ? C41 C40 C39 119.7(9) . . ? C34 C35 C30 120.5(9) . . ? C63 C64 C65 120.0(9) . . ? C58 C57 C56 120.6(9) . . ? C48 C49 C50 120.3(9) . . ? C56 C55 C54 120.2(9) . . ? C23 C18 C19 120.0(8) . . ? C23 C18 P1 119.3(7) . . ? C19 C18 P1 120.3(7) . . ? C64 C65 C60 120.0(9) . . ? C34 C33 C32 120.0(9) . . ? C52 C51 C50 120.8(9) . . ? C8 O5 C11 109.6(7) . . ? C8 O5 Tl 114.6(5) . . ? C11 O5 Tl 123.0(6) . . ? C4 O4 C7 108.0(8) . . ? C4 O4 Tl 121.5(6) . . ? C7 O4 Tl 108.7(6) . . ? C38 C37 C36 119.4(8) . . ? C63 C62 C61 119.2(9) . . ? O5 C8 C9 104.7(8) . . ? C60 C61 C62 120.3(9) . . ? C39 C38 C37 121.2(9) . . ? O1 C1 Pt1 139.2(7) . . ? O1 C1 Pt2 138.0(7) . . ? Pt1 C1 Pt2 79.3(3) . . ? C29 C28 C27 119.7(9) . . ? C46 C47 C42 120.2(9) . . ? C27 C26 C25 121.2(9) . . ? O5 C11 C10 106.5(8) . . ? C26 C27 C28 119.3(9) . . ? C51 C50 C49 119.4(9) . . ? C28 C29 C24 121.6(9) . . ? C17 C16 C15 121.1(10) . . ? C26 C25 C24 119.4(9) . . ? O2 C2 Pt2 136.7(7) . . ? O2 C2 Pt3 141.3(7) . . ? Pt2 C2 Pt3 80.9(3) . . ? C64 C63 C62 121.1(8) . . ? C12 C17 C16 120.1(9) . . ? C18 C19 C20 120.3(10) . . ? C55 C56 C57 119.8(9) . . ? C14 C13 C12 119.5(10) . . ? O3 C3 Pt1 140.4(7) . . ? O3 C3 Pt3 139.5(7) . . ? Pt1 C3 Pt3 79.8(3) . . ? C8 C9 C10 101.1(8) . . ? C23 C22 C21 119.3(9) . . ? C15 C14 C13 120.8(10) . . ? C20 C21 C22 120.6(9) . . ? C21 C20 C19 119.5(10) . . ? C14 C15 C16 118.9(10) . . ? O4 C7 C6 106.3(9) . . ? O4 C4 C5 106.6(9) . . ? C7 C6 C5 101.7(10) . . ? C35 C34 C33 120.5(10) . . ? C11 C10 C9 102.8(8) . . ? C4 C5 C6 103.1(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.798 _refine_diff_density_min -2.149 _refine_diff_density_rms 0.291