Line-narrowing in proton-detected nitrogen-14 NMR

作者: Simone Cavadini , Veronika Vitzthum , Simone Ulzega , Anuji Abraham , Geoffrey Bodenhausen

DOI: 10.1016/J.JMR.2009.09.018

关键词: Magic angleNuclear magnetic resonanceHeteronuclear moleculeChemistryHeteronuclear single quantum coherence spectroscopyCrystallographySolid-state nuclear magnetic resonanceHomonuclear moleculeProtonNuclear magnetic resonance spectroscopyAsymmetry

摘要: In solids spinning at the magic angle, indirect detection of single-quantum (SQ) and double-quantum (DQ) (14)N spectra (I=1) via spy nuclei S=1/2 such as protons can be achieved in manner heteronuclear single- or multiple-quantum correlation (HSQC HMQC) spectroscopy. The HMQC method relies on excitation two-spin coherences type T(11)(I)T(11)(S) T(21)(I)T(11)(S) beginning evolution interval t(1). obtained by Fourier transformation from t(1) to omega(1) may broadened homogenous decay transverse terms S. This broadening is mostly due homonuclear dipolar S-S' interactions between proton nuclei. this work we have investigated possibility inserting rotor-synchronized symmetry-based C R sequences decoupling schemes Phase-Modulated Lee-Goldburg (PMLG) period. These reduce proton-proton lead an enhancement resolution both SQ DQ proton-detected spectra. addition, combination HSQC with PMLG shown that highest dimension using R-type. We show improvements samples l-alanine tripeptide ala-ala-gly (AAG). particular, for width peak reduced 2 1.2 kHz, agreement simulations. report accurate measurements quadrupolar coupling constants asymmetry parameters amide AAG peptide bonds.

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