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Bis(ethylenedithio)tetrathiafulvalene (ET, Strem Chemicals, Inc.) was recrystallized from chloroform (Aldrich) prior to use. Elemental analyses were performed at Galbraith Laboratories (Knoxville, TN) or Midwest Microlab (Indianapolis, IN). 1,1,2- Trichloroethane (TCE, Fluka) was distilled from P2O5 (Aldrich) and filtered through a column containing neutral alumina prior to use. TBA- [Au(C6Cl5)2] was prepared as described previously.1 (Calcd for C28H36N1AuCl10: C, 35.85; H, 3.87; N, 1.49; Au, 21.00; Cl, 37.79. Found: C, 35.79; H, 3.88; N, 1.49; Cl, 37.58. Mp: 180-183 °C.) 1 652 TBA[Au(C6F5)2] was prepared as previously described. (Mp: 113- -13 115 °C.) The Au(C6F5)4 anion was prepared by combining Cd(C6F5)2 with AuCl3 in a molar ratio of 6:1 in diethyl ether at room temperature. A gold(I) compound initially formed which immediately dispropor- tionated into Au(C6F5)4- and elemental gold. PPh4Cl was added, and the yellowish solution was chromatographed over silica. PPh4[Au- (C6F5)4] was isolated as a nearly colorless polycrystalline solid. Yield: 26%. Mp: 175 °C. 19F-NMR: -121.9 (d, o-F), -161.7 (t, p-F), and -164.4 ppm (t, m-F). 发自小木虫IOS客户端 |
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