Iron, nickel and cobalt tri-osmium carbonyl hydrides and their preparation
AssigneeThe Ohio State University Research Foundation
InventorsSheldon G. Shore, Jeffrey S. Plotkin
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Abstract
H.sub.2 Os.sub.3 (CO).sub.10 has apparent Lewis base character and can be made to react with electron deficient iron, cobalt and nickel carbonyls, including salts of [Fe(CO).sub.4 ].sup.2-, Fe.sub.2 (CO).sub.9, (.eta..sup.5 -C.sub.5 H.sub.5)Co(CO).sub.2, Co.sub.2 (CO).sub.8 and [(.eta..sup.5 -C.sub.5 H.sub.5)Ni(CO)].sub.2, to give heteronuclear tri-osmium carbonyl hydrides, some of which are new compounds. New compounds disclosed include H.sub.2 Fe.sub.2 Os.sub.3 (CO).sub.16,H.sub.2 Fe.sub.2 Os.sub.3 (CO).sub.15, H.sub.2 (.eta..sup.5 -C.sub.5 H.sub.5)CoOs.sub.3 (CO).sub.10 and H.sub.3 (.eta..sup.5 -C.sub.5 H.sub.5)NiOs.sub.3 (CO).sub.9.
Claims63
A method for making a tri-osmium heteronuclear metal carbonyl compound, which comprises:
- (a) establishing a reaction mixture comprising an electron deficient cobalt, nickel or iron carbonyl or carbonyl anion, H.sub.2 Os.sub.3 (CO).sub.10, and a solvent which at least partially solubilizes at least one of said electron deficient carbonyl compound and said H.sub.2 Os.sub.3 (CO).sub.10, said H.sub.2 Os.sub.3 (CO).sub.10 reacting with said electron deficient carbonyl compound as a Lewis base;
- and
- (b) recovering said tri-osmium heteronuclear metal carbonyl compound from said reaction mixture.
H.sub.2 Fe.sub.2 Os.sub.3 (CO).sub.16
The compound H.sub.2 Fe.sub.2 Os.sub.3 (CO).sub.15, characterized by being red in color, having a mass spectral m/e value of about 1108 (P-2), and infrared absorption peaks (cyclohexane solvent at room temperature) at about the following wave numbers [(CO), cm.sup.-1 ] 2110, 2100, 2082, 2070, 2045, 2038, 2020, 2002, 1990, and 1985.
The compound H.sub.2 Fe.sub.2 Os.sub.3 (CO).sub.15, characterized as being capable of being made by the reaction of Fe.sub.2 (CO).sub.9 and H.sub.2 Os.sub.3 (CO).sub.10 in a molar ratio of about 2:1 in benzene solvent under substantially anhydrous conditions at a temperature of about 25.degree. C.
H.sub.2 (.eta..sup.5 -C.sub.5 H.sub.5)CoOs.sub.3 (CO).sub.10.
H.sub.3 (.eta..sup.5 -C.sub.5 H.sub.5)NiOs.sub.3 (CO).sub.9.
A nickel carbonyl compound characterized as being capable of being made by the reaction of (.eta..sup.5 -C.sub.5 H.sub.5)Ni(CO).sub.2 and H.sub.2 Os.sub.3 (CO).sub.10, as displaying no protons in the hydride region of its proton nuclear magnetic resonance spectrum and showing infrared bands at about 2058, 2036, 2020, 2010, 1987, 1975, 1966 and 1955 cm.sup.-1.
Dependencies are inferred from the claim text.