Satellite-Transition MAS NMR of Spin I=3/2, 5/2, 7/2 and 9/2 Nuclei: Sensitivity, Resolution and Practical Implementation

Abstract
         The satellite-transition MAS (STMAS) experiment offers an alternative approach to established methods such as dynamic angle spinning (DAS), double rotation (DOR) and multiple-quantum MAS (MQMAS) for obtaining high-resolution NMR spectra of half-integer quadrupolar nuclei. Unlike the multiple-quantum experiment, STMAS involves two-dimensional correlation of purely single-quantum coherences; satellite transitions in t1 (or F1) and the central transition in t2 (or F2). To date, STMAS has primarily been demonstrated for nuclei with spin quantum numbers I = 3/2 and, to a lesser extent, I = 5/2. However, many chemically relevant nuclei possess I > 3/2, such as 17O and 27Al (both I = 5/2), 59Co (I = 7/2) and 93Nb (I = 9/2). Here, we discuss the application of STMAS to nuclei with spin quantum numbers from I = 3/2 to 9/2. First, we consider the practical implementation of the STMAS experiment using 87Rb (I = 3/2) NMR as an example. We then extend the discussion to include nuclei with higher spin quantum numbers, demonstrating 27Al, 45Sc (I = 7/2), 59Co and 93Nb STMAS experiments on both crystalline and amorphous samples. We also consider the possibility of experiments involving satellite transitions other than mI = ±1/2 to ±3/2 and, using 93Nb NMR, demonstrate the correlation of all single-quantum satellite transitions up to and including mI = ±7/2 to ±9/2. The absolute chemical shift scaling factors in these experiments are discussed, as are the implications for isotropic resolution.