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

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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.

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About the authors

E. V. Gorbachuk

Arbuzov Institute of Organic and Physical Chemistry, FRC Kazan Scientific Center, Russian Academy of Sciences; Alexander Butlerov Institute of Chemistry, Kazan (Volga Region) Federal University

Email: yakhvar@iopc.ru
Russian Federation, Kazan; Kazan

M. A. Mikhaylov

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Email: yakhvar@iopc.ru
Russian Federation, Novosibirsk

D. G. Sheven

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Email: yakhvar@iopc.ru
Russian Federation, Novosibirsk

M. N. Sokolov

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Email: yakhvar@iopc.ru
Russian Federation, Novosibirsk

D. G. Yakhvarov

Arbuzov Institute of Organic and Physical Chemistry, FRC Kazan Scientific Center, Russian Academy of Sciences; Alexander Butlerov Institute of Chemistry, Kazan (Volga Region) Federal University

Author for correspondence.
Email: yakhvar@iopc.ru
Russian Federation, Kazan; Kazan

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2. Fig. 1. Diffractogram for the obtained powder sample of Re3I9 (shown in black) and theoretically calculated (shown in red) from PCA data for single crystal Re3I9.

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3. Fig. 2. Diffractogram for the obtained powder sample [Re(CO)5I] (shown in black) and theoretically calculated (shown in red) from PCA data for single crystal [Re(CO)5I].

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4. Fig. 3. ESI-MS spectrum of ((n-C4H9)4N)2[Re2Cl8] in CH3CN.

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