期刊
INORGANIC CHEMISTRY
卷 60, 期 23, 页码 17586-17592出版社
AMER CHEMICAL SOC
DOI: 10.1021/acs.inorgchem.1c02184
关键词
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资金
- National Science Foundation [CHE 1764345]
- NSF Major Research Instrumentation (MRI) Award [1920299]
- MRSEC Program of the National Science Foundation [NSF DMR 1720256]
- NSF
- UCSB Eddleman Center for Quantum Innovation
- Division Of Chemistry
- Direct For Mathematical & Physical Scien [1920299] Funding Source: National Science Foundation
In this study, a nano-cluster [Ni23Se12Cl3(PEt3)(10)] was successfully synthesized and characterized using NMR spectroscopy, ESI-MS, and X-ray crystallography. The previously reported nano-cluster [Ni23Se12(PEt3)(13)] was re-evaluated and found to be more accurately formulated as [Ni23Se12Cl3(PEt3)(10)] based on spectroscopic and crystallographic analysis.
The reaction of [Ni(1,5-COD)(2)] (1.0 equiv), PEt3 (0.04 equiv), SePEt3 (0.52 equiv), and [NiCl2(PEt3)(2)] (0.07 equiv) in a mixture of toluene and THF results in the formation of [Ni23Se12Cl3(PEt3)(10)] (1), which can be isolated in moderate yield after workup. Complex 1 was characterized by NMR spectroscopy, ESI-MS, and X-ray crystallography. This open-shell nanocluster features a central [Ni-13](7+) anticuboctahedral kernel, which is encapsulated by a [Ni-10(mu-Se)(9)Cl-3](-) shell, along with ten PEt3 ligands and three (mu(4)-Se)(2-) ligands. On the basis of our spectroscopic and crystallographic analysis, coupled with in situ spectroscopic monitoring, we believe that the previously reported nanocluster, [Ni23Se12(PEt3)(13)], is actually better formulated as [Ni23Se12Cl3(PEt3)(10)].
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