Synthesis of hydrido- and deuterio-carbonyl cluster complexes of ruthenium, iron--ruthenium, and osmium from metal carbonyls and hydrogen at atmospheric pressure

Ru4H4(CO)12 and Os3H2(CO)10 are obtained in high yield and purity by reaction of H2 at atmospheric pressure at 1200 in hydrocarbon solutions of Ru3(CO)12 and Os3(CO)12, respectively. Further treatment of Os3H2(CO)10 with H2 leads to Os4H4(CO)12. Ru4D4(CO)12 is obtained from Ru3(CO)12 and D2 in hydrocarbon solvent; however, extensive hydrogen exchange with solvent is observed in the osmium system. Ru4H2D2(CO)12 is obtained in the reaction of D2 with Ru4H2(CO)13 and the new mixed metal complex FeRu3H4(CO)12 is obtained from FeRu3H2(CO)13 and H2. Substances are characterized by ir, NMR, Raman, and mass spectrometry. (U.S.)