Ru3(CO)12in Acidic Media. Intermediates of the Acid-Cocatalyzed Water-Gas Shift Reaction (WGSR)

Abstract
The elucidation of the WGSR promoted by ruthenium carbonyls in acidic media started with the detection of the Ru(0), Ru(I), and Ru(II) intermediate complexes, namely Ru3(CO)12, Ru2[μ-η2-OC(CF3)O]2(CO)6, and fac-[Ru(CF3COO)3(CO)3]-, which accumulate when CF3COOH is employed as an acid cocatalyst. Under catalytic conditions, the three were found to interconvert through elementary steps which produce CO2 and H2. In fact, Ru(0) is oxidized by H+ to Ru(I) and half the hydrogen of the catalytic cycle is supplied by this reaction. On the other hand, Ru(I) disproportionates to Ru(0) and Ru(II), and this latter species undergoes nucleophilic attack by H2O. The decomposition of the metallacarboxylic acid intermediate gives back Ru(I), while H2 and CO2 are produced in a 1/2 molar ratio. The two alternating pathways for dihydrogen formation, namely Ru(0) oxidation by H+ and the decomposition of a metallacarboxylic acid intermediate, involve H2 reductive elimination from the same RuHCF3COO(CO)2L2 intermediate (L = H2O, ethers). These findings define an acid-cocatalyzed WGSR whose distinctive features are (i) the intervention of a disproportionation reaction to generate a Ru(II) electron poor complex, whose CO ligands can undergo nucleophilic attack by water, (ii) the generation of the hydrido intermediate for dihydrogen production through two distinct reaction patways, and (iii) the reductive elimination of H2 from the hydrido intermediate without involving H+ from the medium.

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