NATURAL-ABUNDANCE HIGH-RESOLUTION SOLID-STATE H-2 NMR-SPECTROSCOPY

We report for the first time an approach for natural abundance solid state H-2 NMR spectroscopy involving magic angle sample spinning (MAS), high-power H-1 decoupling (HPPD) and H-1-H-2 cross polarization (CP). Taking tetrakis (trimethylsilyl)silane (TTMSS), adamantane, 1-chloroadamantane, hexamethylbenzene (HMB), 2,2-dimethyl-1,3-propanediol (DMPD) and 2-hydroxymethyl-2-methyl-1,3-propanediol (HMPD) as examples, it has been shown that the combination of HPPD and MAS can be applied readily to study rotator phase solids, allowing isotropic peaks arising from chemically inequivalent H-2 nuclei to be resolved. For natural abundance samples of TTMSS and chloroadamantane, it has been shown that H-2 CP/HPPD/MAS NMR experiments, involving polarization transfer from H-1 to H-2, may provide considerable sensitivity enhancement in comparison with single pulse experiments.