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1
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33746504855
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note
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xx. 0.5 Hz); EI-MS: ml: 690 (M), 675 (M Me), 613 (M - Ph)+, 505 (M - PPhj). Found: C, 76.36; H, 5.85. Cale, for CH38P4: C, 76.52; H, 5.55%. [Au{(AP,Rp-TPP4}]PF6: [NBu4][AuIJ (0.11 g, 0.14 mmol) was added to a solution of (RP,Rr)-TPPt (0.11 g, 0.14 mmol) in ethanol (20 cm') and thé mixture heated briefly on a steam bath. The volume of the solution was reduced by fa. 50% to give [Au{(#P,/?P)-TPP4}]I (0.14 g, 97%). The iodide salt was redissolved in acetone (20 cm5) and a solution of NH4PF6 (0.11 g, 0.880 mmol) in water (10 cm3) was added. The volume of the solution was reduced to ca. 10 cmto give a white solid that was subsequently recrystallised from acetonitrile by the addition of diethyl ether (0.11 g, 93%). mp 288 "C. 'H NMR data [300 MHz, (CD3)2CO at 20 °C]: S 1.97 (bs, 6H, PMe), 7.59-8.55 (m, 32 H, aromatic); 31P-{'H} NMR data [121.5 MHz, (CD3)2CO at 20 °C]: <5A 3.69 (internal P; AA'), <5X 23.57 (terminal P; XX'), (XAA'X', J. 41 Hz, /AX 131 Hz, JA.X 75 Hz, J. 7 Hz). Found: C, 49.14; H, 3.60. Calc. for CHAuFtPs H2O: C, 49.45; H, 3.96%. t Crystal data for [Au{(KP,V)-TPP4}]PF6-CHjCl2: C45H40AuClr FPS, M= 1117.54, triclinic, a = 9.7019(3), 6=14.5445(4), c = 16.3041(4) A, a = 86.957, B= 76.013(2), y = 87.492(2)°, U= 2228.2(1) A3, T= 200.0 K, space group PI (no. 2), Z = 2, /i(Mo-Ka) = 36.7 cirT1, 48690 reflections measured, 10205 unique (RM = 0.092), 7069 with / > 2
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2
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0034400421
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