Rhenium Iodide Cluster Re₃I₉ as a Precursor in the Synthesis of [Re(CO)₅I] and ((н-C₄H₉)₄N)2[Re₂Cl₈]

Abstract

The reduction of rhenium iodide cluster Re3I9 to [Re(CO)5I] (55% yield) was observed in the presence of concentrated HCl and HCOOH at 130°C. In a dimethylammonium chloride [(CH3)2NH2]Cl melt, the triangular cluster polymer Re3I9 is transformed into the dianionic binuclear cluster complex [Re2Cl8]2–, which was isolated as the tetrabutylammonium salt ((n-C4H9)4N)2[Re2Cl8] in 46% yield. The structure of the complex [Re(CO)5I] was confirmed by powder X-ray diffraction, energy dispersive spectroscopy, IR spectroscopy, and Raman spectroscopy. ((n-C4H9)4N)2[Re2Cl8] was identified using elemental analysis, energy dispersive spectroscopy, and IR and Raman spectroscopy. An acetonitrile solution of ((n-C4H9)4N)2[Re2Cl8] was characterized by the mass spectrum and characteristic UV-Vis spectrum.