(a) 1H NMR spectrum from a mixture containing d6-ethanol solvent, the PVP polymer comb catalyst
particles (PVPCs), and the (fully protonated) pyridine substrate thermally
polarized at 9.4 T following activation with pH2 bubbling.
(b) 1H NMR spectrum of the sample in (a) obtained after
PVPC activation but with pH2 bubbling occurring at high
field, acquired immediately after cessation of pH2 gas
bubbling; for the most part, no high-field (in situ) SABRE effect was observed. (c) 1H (ex situ) HET-SABRE NMR spectrum obtained from the same sample, acquired
immediately after 30 s of pH2 bubbling at low field (∼100
G) and rapid transfer of the sample into the NMR magnet. All spectra
shown were acquired with a single scan (90° pulse). Peaks at
about δ ≈1.1, ≈3.6, and ≈5.2 ppm are from
residual protons from the deuterated ethanol solvent. The peak at
≈4.5 ppm is from (ortho-)hydrogen (oH2) gas. The
inset shows the expected hexacoordinate structure of the activated
catalytic moiety, exchanging with pH2 and the substrate
pyridine (Py).