was performed with a JEOL JNM-ECX400 spectrometer (9.4 T) with a 4
mm MAS probe. The 31P MAS NMR spectra were collected at
a spinning frequency of 15 kHz with a π/2 excitation pulse of
3.11 μs. A total of 32 scans with a 60 s recycle delay were
used to ensure good quantitative peak intensities. The chemical shifts
of the 31P MAS NMR spectra were referenced to an 85% H3PO4 solution (0 ppm).
7Li MAS
NMR spectroscopy was performed by using a JEOL JNM-ECZ-600R spectrometer
(14.1 T) with a 3.2 mm MAS probe. The 7Li MAS NMR experiments
were performed with a 20 kHz spinning speed and a 2.90 μs excitation
pulse. The delay time between each of the eight scans was set to 60
s to ensure good quantitative peak intensities. A 1 M LiCl solution
was used for the chemical shift reference (0 ppm).
For the solid-state 31P and 7Li NMR measurements,
the samples were packed into ZrO2 sample tubes in a glovebox.
No spectral changes were observed during the NMR measurements, meaning
that the use of airtight sample tubes prevented reactions with oxygen
and water in the air.