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NMR spectroscopy of paramagnetic complexes. Part 39—natural abundance 2H NMR of paramagnetic sandwich compounds

✍ Scribed by Janet Blümel; Peter Hofmann; Frank H. Köhler

Publisher
John Wiley and Sons
Year
1993
Tongue
English
Weight
446 KB
Volume
31
Category
Article
ISSN
0749-1581

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✦ Synopsis

Abstract

The methylated metallocenes (MeCp)~2~M with M = V, Cr, Mn, Co, Ni (1–5) were investigated by ^1^H and ^2^H NMR spectroscopy at natural abundance. The ^2^H NMR signals are narrower by a factor of up to 30 compared with the corresponding ^1^H NMR signals, thus establishing an inexpensive method and a general improvement of the NMR spectra of paramagnetic π‐complexes. This has allowed the resolution of the signal splitting of Cp deuterons of 1 and 5 which could not be observed earlier in the ^1^H NMR spectra. The origin of the small (1 and 5) and large (2–4) signal splittings is discussed and related to an extended Hückel calculation. The relative magnitude of the signal splitting is reproduced, but the signal assignment had to be deduced from ^13^C NMR results. Primary isotope shifts of up to 4.0 ppm were found for 1, 2, 4 and 5. The much higher values for 3 (up to 16.6 ppm) reflect the combined influence of the intrinsic isotope shift and the isotope effect on the spin crossover.

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