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We demonstrate that supercycles of previously introduced two-fold symmetry dipolar recoupling schemes may be utilized successfully in homonuclear correlation nuclear magnetic resonance (NMR) spectroscopy for probing proximities among half-integer spin quadrupolar nuclei in network materials undergoing magic-angle-spinning (MAS). These ( S R2 2 1 ) M , ( S R2 4 1 ) M , and ( S R2 8 1 ) M recoupling sequences with M = 3 and M = 4 offer comparably efficient magnetization transfers in single-quantum-single-quantum (1Q-1Q) correlation NMR experiments under moderately fast MAS conditions, as demonstrated at 14.1 T and 24 kHz MAS in the contexts of 11 B NMR on a Na 2 O-CaO-B 2 O 3 -SiO 2 glass and 27 Al NMR on the open framework aluminophosphate AlPO-CJ19 [(NH 4 ) 2 Al 4 (PO 4 ) 4 HPO 4 · H 2 O]. Numerically simulated magnetization transfers in spin-3/2 pairs revealed a progressively enhanced tolerance to resonance offsets and rf-amplitude errors of the recoupling pulses along the series ( S R2 2 1 ) M &lt; ( S R2 4 1 ) M &lt; ( S R2 8 1 ) M for increasing differences in chemical shifts between the two nuclei. Nonetheless, for scenarios of a relatively minor chemical-shift dispersions ( ≲ 3 kHz), the ( S R2 2 1 ) M supercycles perform best both experimentally and in simulations.

molecules/molecules online/molecules annual

Improved Magnetization Transfers among Quadrupolar Nuclei in Two-Dimensional Homonuclear Correlation NMR Experiments Applied to Inorganic Network Structures