Abstract

High-resolution solid-state 13C and 29Si NMR spectroscopy have been used to investigate the dynamic properties of tetrakis(trimethylsilyl)silane (TTMSS) as a function of temperature; from the temperature dependence of the spectra, it is clear that TTMSS is not useful as a chemical shift reference material below ca. 238K, but the spectral changes associated with the phase transition at this temperature nevertheless provide a precise method for controlling temperature calibration in low-temperature solid-state 13C NMR studies.

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