Obtaining accurate chemical shifts for all magnetic nuclei (1H, 13C, 17O, and 27Al) in tris(2,4-pentanedionato-O,O′)aluminium(III) — A solid-state NMR case study

Wong, Alan and Smith, Mark E. and Terskikh, Victor and Wu, Gang (2011) Obtaining accurate chemical shifts for all magnetic nuclei (1H, 13C, 17O, and 27Al) in tris(2,4-pentanedionato-O,O′)aluminium(III) — A solid-state NMR case study. Canadian Journal of Chemistry, 89 (9). pp. 1087-1094. ISSN 1480-3291

Abstract

We report a complete set of high-resolution solid-state NMR spectra for all magnetic nuclei (1H, 13C, 17O, and 27Al) in the α-form of tris(2,4-pentanedionato-O,O′)aluminium(III), α-Al(acac)3. These high-resolution NMR spectra were obtained by using a host of solid-state NMR techniques: standard cross-polarization under the magic-angle spinning (CPMAS) method for 13C, 1-D homonuclear decoupling using the windowed DUMBO sequence for 1H, double-rotation (DOR) for 17O and 27Al, and multiple-quantum MAS for 27Al. Some experiments were performed at multiple magnetic fields. We show that the isotropic chemical shifts obtained for 1H, 13C, 17O, and 27Al nuclei in α-Al(acac)3 are highly resolved and accurate, regardless of the nature of the targeted nuclear spins (i.e., spin-1/2 or quadrupolar) and, as such, can be treated equally in comparison with computational chemical shifts obtained from a gauge-including projector-augmented wave (GIPAW) plane-wave pseudopotential DFT method.