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

IF 1.1 3区化学 Q4 CHEMISTRY, INORGANIC & NUCLEAR Russian Journal of Coordination Chemistry Pub Date : 2024-12-08 DOI:10.1134/S1070328424600463

E. V. Gorbachuk, M. A. Mikhaylov, D. G. Sheven, M. N. Sokolov, D. G. Yakhvarov

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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 [Re₂-Cl₈]^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, 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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[Re(CO)5I]和（(n-C4H9)4N）2[Re2Cl8]合成中的碘化铼簇Re3I9前驱体

在浓HCl和HCOOH存在下，在130℃下，观察到碘化铼簇Re3I9还原为[Re(CO)5I]（收率55%）。在二甲基氯化铵[(CH3)2NH2]Cl熔体中，三角形簇状聚合物Re3I9转化为重阴离子双核簇状配合物[Re2-Cl8]2 -，以46%的产率分离得到四丁基铵盐（(n-C4H9)4N）2[Re2Cl8]。通过粉末x射线衍射、能量色散光谱、红外光谱和拉曼光谱对配合物[Re(CO)5I]的结构进行了证实。（n-C4H9）4N)2[Re2Cl8]采用元素分析、能量色散光谱、红外光谱和拉曼光谱鉴定。用质谱和特征紫外-可见光谱对（(n-C4H9)4N）2[Re2Cl8]乙腈溶液进行了表征。

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来源期刊

Russian Journal of Coordination Chemistry 化学-无机化学与核化学

CiteScore

2.40

自引率

15.80%

发文量

审稿时长

7.2 months

期刊介绍： Russian Journal of Coordination Chemistry is a journal that publishes reviews, original papers, and short communications on all aspects of theoretical and experimental coordination chemistry. Modern coordination chemistry is an interdisciplinary science that makes a bridge between inorganic, organic, physical, analytical, and biological chemistry.