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  • Title: Adiabatic sweep cross-polarization magic-angle-spinning NMR of half-integer quadrupolar spins.
    Author: Wi S, Kim C, Schurko R, Frydman L.
    Journal: J Magn Reson; 2017 Apr; 277():131-142. PubMed ID: 28285143.
    Abstract:
    The use of frequency-swept radiofrequency (rf) pulses for enhancing signals in the magic-angle spinning (MAS) spectra of half-integer quadrupolar nuclides was explored. The broadband adiabatic inversion cross-polarization magic-angle spinning (BRAIN-CPMAS) method, involving an adiabatic inversion pulse on the S-channel and a simultaneous rectangular spin-lock pulse on the I-channel (1H), was applied to I(1/2)→S(3/2) systems. Optimal BRAIN-CPMAS matching conditions were found to involve low rf pulse strengths for both the I- and S-spin channels. At these low and easily attainable rf field strengths, level-crossing events among the energy levels |3/2〉,|1/2〉,|-1/2〉,|-3/2〉 that are known to complicate the CPMAS of quadrupolar nuclei, are mostly avoided. Zero- and double-quantum polarization transfer modes, akin to those we have observed for I(1/2)→S(1/2) polarization transfers, were evidenced by these analyses even in the presence of the quadrupolar interaction. 1H-23Na and 1H-11B BRAIN-CPMAS conditions were experimentally explored on model compounds by optimizing the width of the adiabatic sweep, as well as the rf pulse powers of the 1H and 23Na/11B channels, for different MAS rates. The experimental data obtained on model compounds containing spin-3/2 nuclides, matched well predictions from numerical simulations and from an average Hamiltonian theory model. Extensions to half-integer spin nuclides with higher spins and potential applications of this BRAIN-CPMAS approach are discussed.
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