Synthesis and Interconversions of Several Tri- and Tetranuclear Ruthenium Isocyanato Carbonyl Clusters. Crystal and Molecular Structure of H3Ru4(NCO)(CO)12

Douglas E. Fjare, James A. Jensen, Wayne L. Gladfelter

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Abstract

The reaction of Ru3(CO)12 with PPN(N3) was found to lead through several intermediates to PPN[Ru4(NCO)(CO)13]. The structure of this product is proposed to be analogous to [Ru4Cl(CO)13]- with the μ-NCO replacing the chloride. Spectroscopic characterization of the intermediates suggests that their formulations are [Ru3(NCO)(CO)11]- and [Ru3-(NCO)(CO)10]-. Protonation of the initial reaction solution containing these trimers allows the isolation of HRu3(NCO)(CO)10 in low yield. The tetranuclear cluster reacts with CO at room temperature to give [Ru3(NCO)(CO)11]-, and it reacts with H2 under the same conditions to give [H2Ru4(NCO)(CO)12]-. This anion reacts with CF3SO3H to give H3Ru4(NCO)(CO)12, which was characterized by a single-crystal X-ray crystallographic study [P21/n space group; a = 9.836 (2), b = 22.063 (5), c = 10.056 (2) Å; β = 97.93 (1)°; V= 2161 (1) Å3; Z = 4; final R = 0.024; final Rw = 0.028]. The structure contains a butterfly arrangement of ruthenium tricarbonyl groups with the isocyanate bridging the open edge. The hydrogen atoms were located and refined.

Original languageEnglish (US)
Pages (from-to)1774-1780
Number of pages7
JournalInorganic Chemistry
Volume22
Issue number12
DOIs
StatePublished - Jun 1983

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