Trihydrido tricyclohexylphosphine gallium

A solution of tricyclohexylphosphine (4.65 g, 16.58 mmol) dissolved in diethyl ether (120 mL) is added to a freshly prepared solution of Li[GaH4]16 (16.30 mmol) in diethyl ether (100 mL), cooled in a liquid nitrogen-chloroform slush bath. The mixture is stirred for 30 min and warmed to ambient temperature as it stirs overnight. 

The reaction mixture is filtered by filter-tipped cannula into a 250-mL Schlenk flask and the filtrate is reduced to half volume in vacuo and cooled to about ca. — 30°C overnight. The supernatant liquid is decanted from the small colorless crystals that form and reduced to half volume and again cooled overnight. The preceding procedure is repeated once more. Overall yield 4.73 g (82%). 

Wiberg and E. Amberger, Hydrides of the Elements of Main Groups I-IV, Elsevier, London, 1971. 

McNally, V. S. Leong, and N. J. Cooper, Experimental Organometallic Chemistry. A Practicum in Synthesis and Characterization, A. L. Wayda and M. Y. Darensbourg (eds.), Symposium Series 357, American Chemical Society, Washington, DC, 1987, p. 6. 

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