Touchton Alexander J, Wu Guang, Hayton Trevor W
Department of Chemistry and Biochemistry, University of California, Santa Barbara, California 93106, United States.
Inorg Chem. 2021 Dec 6;60(23):17586-17592. doi: 10.1021/acs.inorgchem.1c02184. Epub 2021 Nov 11.
The reaction of [Ni(1,5-COD)] (1.0 equiv), PEt (0.04 equiv), SePEt (0.52 equiv), and [NiCl(PEt)] (0.07 equiv) in a mixture of toluene and THF results in the formation of [NiSeCl(PEt)] (), which can be isolated in moderate yield after workup. Complex was characterized by NMR spectroscopy, ESI-MS, and X-ray crystallography. This open-shell nanocluster features a central [Ni] anticuboctahedral kernel, which is encapsulated by a [Ni(μ-Se)Cl] shell, along with ten PEt ligands and three (μ-Se) ligands. On the basis of our spectroscopic and crystallographic analysis, coupled with spectroscopic monitoring, we believe that the previously reported nanocluster, [NiSe(PEt)], is actually better formulated as [NiSeCl(PEt)].
在甲苯和四氢呋喃的混合溶液中，[Ni(1,5 - 环辛二烯)]（1.0当量）、三乙膦（0.04当量）、二乙硒膦（0.52当量）与[NiCl(三乙膦)]（0.07当量）发生反应，生成了[NiSeCl(三乙膦)]（），经后处理可中等产率分离得到该产物。配合物 通过核磁共振光谱、电喷雾电离质谱和X射线晶体学进行了表征。这个开壳层纳米簇具有一个中心[Ni]反立方八面体核，其被一个[Ni(μ - Se)Cl]壳层所包裹，还有十个三乙膦配体和三个（μ - Se）配体。基于我们的光谱和晶体学分析，以及光谱监测，我们认为先前报道的纳米簇[NiSe(三乙膦)]实际上更应表述为[NiSeCl(三乙膦)]。
