Safety note: Some of the materials mentioned here are very dangerous. Ask a qualified chemist for advice before handling them. Qualified chemists should check the relevant safety literature before handling or giving advice about unfamiliar substances. NMR solvents are toxic and most are flammable. Specifically, nickel salts are toxic and Ni(CO)4 is extremely toxic, work in a hood with appropriate gloves.

⁶¹Nickel NMR

⁶¹Nickel (⁶¹Ni) is a low sensitivity nucleus with a low natural abundance that yields somewhat broad lines even in symmetric environments and very broad lines for slightly larger complexes over a very wide chemical shift range. ⁶¹Ni is a spin 3/2 nucleus and is therefore quadrupolar. As a result, the signal width increases with asymmetry of the environment. The most common oxidation state of nickel salts is Ni(II). However, this oxidation state is paramagnetic in the square-planar form so cannot be observed on a high resolution NMR spectrometer but could be observed in principle for complexes that take on the pure diamagnetic tetrahedral form. ⁶¹Ni NMR is most commonly observed for Ni(0) and is usually used for the study of Ni(0) complexes. Each type of nickel compound has its characteristic chemical shift (fig. 1). One bond coupling constants to ³¹P of 400 to 470 Hz are observed and two bond couplings to ¹⁹F in Ni(PF₃)₄ are 28 Hz.

Fig. 1. Chemical shift ranges for nickel NMR

We do not have experience of ⁶¹Ni NMR in our laboratory but could provide the service if given an appropriate sample.

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Properties of ⁶¹Ni

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References

1. N. Hao, M. J. McGlinchey, B. G. Sayer and G. J. Schrobilgen, "A ⁶¹Ni NMR Study of Some d¹⁰ Nickel Complexes", J. Magn. Reson., 46, 158-162 (1982).

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