BaBa-xy16: Robust and broadband homonuclear DQ recoupling for applications in rigid and soft solids up to the highest MAS frequencies

被引:132
作者
Saalwaechter, Kay [1 ]
Lange, Frank [1 ]
Matyjaszewski, Krzysztof [2 ]
Huang, Chih-Feng [2 ]
Graf, Robert [3 ]
机构
[1] Univ Halle Wittenberg, Inst Phys, NMR, D-06120 Halle, Germany
[2] Carnegie Mellon Univ, Dept Chem, Pittsburgh, PA 15213 USA
[3] Max Planck Inst Polymer Res, D-55128 Mainz, Germany
关键词
Multiple-quantum NMR; Double-quantum NMR; Recoupling; (31)P NMR; Phosphates; Polymers; Elastomers; Networks; Biomolecular solid-state NMR; NUCLEAR-MAGNETIC-RESONANCE; QUANTUM NMR-SPECTROSCOPY; TRANSFER RADICAL POLYMERIZATION; CROSS-LINK DENSITY; STATE NMR; ROTATING SOLIDS; CHAIN DYNAMICS; DISTANCE MEASUREMENTS; PULSE SEQUENCE; ORDER;
D O I
10.1016/j.jmr.2011.07.001
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
We here present a substantially improved version of the popular Back-to-Back (BaBa) homonuclear double-quantum (DQ) MAS recoupling pulse sequence. By combining the original pulse sequence with a virtual pi pulse train with xy-16 phase cycling along with time-reversed DQ reconversion, a truly broadband and exceptionally robust pulse sequence is obtained. The sequence has moderate radio-frequency power requirements, amounting to only one 360 degrees nutation per rotor cycle, it is robust with respect to rf power and tune-up errors, and its broadband performance increases with increasing spinning frequency, here tested up to 63 kHz. The experiment can be applied to many spin-1/2 nuclei in rigid solids with substantial frequency offsets and CSAs, which is demonstrated on the example of (31)P NMR of a magnesium ultra-phosphate, comparing experimental data with multi-spin simulations, and we also show simulations addressing the performance in (13)C NMR of bio(macro)molecules. (1)H-based studies of polymer dynamics are highlighted for the example of a rigid solid with strongly anisotropic mobility, represented by a polymer inclusion compound, and for the example of soft materials with weak residual dipole-dipole couplings, represented by homogeneous and inhomogeneous elastomers. We advocate the use of normalized (relaxation-corrected) DQ build-up curves for a quantitative assessment of weak average dipole-dipole couplings and even distributions thereof. (C) 2011 Elsevier Inc. All rights reserved.
引用
收藏
页码:204 / 215
页数:12
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