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[Co(CO) 2 (R 2 PCH 2 ) 3 CCH 3 ][Co(CO) 4 ] (R  C 6 H 5 ) reacts with NaBH 4 , depending on the reaction conditions, to give CoH(CO) 2 (R 2 PCH 2 ) 2 C(CH 3 )CH 2 PR 2 · BH 3 and CoH(CO)(R 2 PCH 2 ) 3 CCH 3 . The hydride CoH(CO)(R 2 PCH 2 ) 3 CCH 3 is also formed by the reaction of [Co(CO) 2 (R 2 PCH 2 ) 3 CCH 3 ][Co(CO) 4 ] with LiOH, NaOH and NaNH 2 . The reaction with LiOH primarily gives (acetone) 3 -LiCo(CO)(R 2 PCH 2 ) 3 CCH 3 , which is also formed by reduction of [Co(CO) 2 (R 2 PCH 2 ) 2 C(CH 3 )CH 2 PR 2 ] 2 with lithium in THF/acetone solution. In liquid ammonia [Co(CO) 2 (R 2 PCH 2 ) 3 CCH 3 ][Co(CO) 4 ] at 20°C yields Co(CONH 2 )(CO)(R 2 PCH 2 ) 3 CCH 3 . This compound reacts in the same solvent at 60°C to yield the hydride CoH(CO)(R 2 PCH 2 ) 3 CCH 3 . CH 3 I and HClO 4 react with CoH(CO)(R 2 PCH 2 ) 3 CCH 3 yielding CoI(R 2 PCH 2 ) 3 CCH 3 and the unstable [Co(H) 2 (CO)(R 2 PCH 2 ) 3 CCH 3 ]ClO 4 , respectively. The deutero complex CoD(CO)(R 2 PCH 2 ) 3 CCH 3 was also synthesized. The new compounds were characterized, as much as possible, by their IR, 1 H NMR and 31 P NMR data.