Abstract
We provide an extensive experimental and numerical evaluation of MQ-phase (S)M supercycles with M={3,4} of three groups of symmetry-based homonuclear dipolar recoupling rf-pulse sequences, S={SR22p1,SR441,SRNNN/2}, for establishing proximities among half-integer spin quadrupolar nuclei under moderately fast magic-angle-spinning (MAS) conditions in single-quantum–single-quantum (1Q–1Q) correlation NMR experiments. The relative merits of the (S)M schemes for variations in resonance offsets and rf-amplitude errors were assessed by numerically simulated magnetization transfers in spin-3/2 pairs with variable isotropic chemical shifts and quadrupolar coupling constants. Experimental demonstrations of 23Na (spin-3/2) NMR on Na2MoO4·2H2O and 27Al (spin-5/2) NMR on AlPO-CJ19 [(NH4)2Al4(PO4)4HPO4·H2O] are presented at 14.1 T and 24 kHz MAS. We recommend using the (SR221)3 or (SR221)4 supercycles for samples that exhibit small chemical-shift dispersions (<3 kHz), and any (SRNNN/2)3 scheme with N⩾10 for larger spreads of isotropic chemical shifts. However, because the (SRNNN/2)3 sequences recouple heteronuclear dipolar interactions, their application to proton-bearing samples requires high-power proton decoupling during the mixing period. Alternatively, the (SR241)3 and (SR241)4 schemes may be employed in the absence of proton decoupling, but with poorer compensation to resonance-offsets and rf-amplitude errors.
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