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Issue 18, 2017
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Synthesis and characterization of a series of nickel(II) alkoxide precursors and their utility for Ni(0) nanoparticle production

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Abstract

A series of nickel(II) aryloxide ([Ni(OAr)2(py)x]) precursors was synthesized from an amide-alcohol exchange using [Ni(NR2)2] in the presence of pyridine (py). The H-OAr selected were the mono- and di-ortho-substituted 2-alkyl phenols: alkyl = methyl (H-oMP), iso-propyl (H-oPP), tert-butyl (H-oBP) and 2,6-di-alkyl phenols (alkyl = di-iso-propyl (H-DIP), di-tert-butyl (H-DBP), di-phenyl (H-DPhP)). The crystalline products were solved as solvated monomers and structurally characterized as [Ni(OAr)2(py)x], where x = 4: OAr = oMP (1), oPP (2); x = 3: OAr = oBP (3), DIP (4); x = 2: OAr = DBP (5), DPhP (6). The excited states (singlet or triplet) and various geometries of 1–6 were identified by experimental UV-vis and verified by computational modeling. Magnetic susceptibility of the representative compound 4 was fit to a Curie Weiss model that yielded a magnetic moment of 4.38(3)μB consistent with a Ni2+ center. Compounds 1 and 6 were selected for decomposition studied under solution precipitation routes since they represent the two extremes of coordination. The particle size and crystalline structure were characterized using transmission electron microscopy (TEM) and powder X-ray diffraction (PXRD). The materials isolated from 1 and 6 were found by TEM to form irregular shape nanomaterials (8–15 nm), which by PXRD were found to be Ni0 hcp (PDF: 01-089-7129) and fcc (PDF: 01-070-0989), respectively.

Graphical abstract: Synthesis and characterization of a series of nickel(ii) alkoxide precursors and their utility for Ni(0) nanoparticle production

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Publication details

The article was received on 24 Oct 2016, accepted on 22 Feb 2017 and first published on 22 Feb 2017


Article type: Paper
DOI: 10.1039/C6DT04083G
Citation: Dalton Trans., 2017,46, 5806-5815
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    Synthesis and characterization of a series of nickel(II) alkoxide precursors and their utility for Ni(0) nanoparticle production

    L. J. Treadwell, T. J. Boyle, W. A. Phelan, M. V. Parkes and D. P. Young, Dalton Trans., 2017, 46, 5806
    DOI: 10.1039/C6DT04083G

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