S- 2,2-bipyridine palladium II

Solutions of 0.42 g. (0.0010 mole) of K2[Pd(SCN)4],27 dissolved in 10 ml. of absolute ethanol and 5 drops of water, and 0.16 g. (0.0010 mole) of 2,2 -bipyridine, dissolved in 10 ml. of absolute ethanol and 5 drops of ethyl ether, are precooled to — 78°C. in a Dry Ice-acetone bath and then mixed in a beaker fitted with a magnetic stirrer and surrounded by a Dry Ice-acetone bath. The solution is stirred for 1 minute, then removed from the bath, and allowed to stand for 20 minutes at room temperature. The unidentified orange solid which precipitates is removed by filtration, whereupon the desired orange-yellow S-bonded isomer 

The S-bonded isomer can be quantitatively converted to the light yellow AT-bonded isomer by heating the former in vacuo at 156°C. for 30 minutes. Anal. Found C, 38.56 H, 2.43 N, 14.81. 

Alternatively, the pure AT-bonded isomer may also be prepared by mixing, at 25°C., solutions of 0.42 g. (0.0010 mole) of K2[Pd(SCN)J,27 dissolved in 5 ml. of water, and 0.16 g. (0.0010 mole) of 2,2-bipyridine, dissolved in 5 ml. of absolute ethanol. The resulting mixture is stirred for 10 minutes, after which the product is isolated by filtration, washed with 50 ml. each of water, absolute ethanol, and ethyl ether, and dried in vacuo over magnesium perchlorate. Yield is 0.36 g. (94%) m.p. 270°C. (decomp.). Anal. Found C, 38.01 H, 2.34 N, 14.86. 

The linkage isomers may be conveniently distinguished from each other by comparing their infrared spectra. The AT-bonded isomers (Secs. B and D) exhibit strong, broad C—N stretching 

Kuroda and P. S. Gentile, Inorg. Nucl. Chem. Letters, 8, 151 (1967). 

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CycIooctadiene)-Astetra-fluoroborate, 13 59 [Pd(C8H12)(C5H702)][BF4] (1,5-CycIooctadiene)(2,4-pentane-dionato)palladium(II) tetrafluoroborate, 13 56 [Pd(C9HlsO)2(CsHs)] (8-methoxy-4-cycIoocten-l-yl)cycIopenta-dienyl palladium(II), 13 60 [Pd(C10H8N2)(SCN)2] Dithio-cyanato-S-(2,2 -bipyridine) palladium(II), 12 222 (NCS), isomer, 12 223... 

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