在魔角自旋固体核磁共振中,采用异步五重对称序列实现更好的同核极化转移

IF 1.8 3区 化学 Q4 CHEMISTRY, PHYSICAL Solid state nuclear magnetic resonance Pub Date : 2023-04-01 DOI:10.1016/j.ssnmr.2023.101858
Vaishali Arunachalam, Kshama Sharma, Kaustubh R. Mote, P.K. Madhu
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引用次数: 0

摘要

魔角自旋(MAS)固态NMR中的重耦合、解耦和多维关联实验可以通过利用内部自旋相互作用的对称性来设计。一种这样的方案,即C521及其超循环版本SPC521,记为五重对称序列,被广泛用于双量子偶极-偶极重耦合。这种方案通常通过设计实现转子同步。我们展示了SPC521序列的异步实现,与正常同步实现相比,该序列具有更高的双量子同核极化转移效率。转子同步以两种不同的方式中断:延长其中一个脉冲的持续时间,表示为脉冲宽度变化(PWV),以及失配MAS频率,表示为MAS变化(MASV)。该异步序列在三种不同的样品上的应用,即U–13C-丙氨酸和1,4-13C-标记的邻苯二甲酸铵,包括13Cα-13Cβ、13Cα-13 Co和13Co–13Co自旋系统,以及腺苷5′-三磷酸二钠盐三水合物(ATP·3H2O)。我们表明,异步版本对于具有小偶极-偶极耦合和大化学位移各向异性的自旋对(例如13Co–13Co)表现更好。仿真和实验证实了这一结果。
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Asynchronising five-fold symmetry sequence for better homonuclear polarisation transfer in magic-angle-spinning solid-state NMR

Recoupling, decoupling, and multidimensional correlation experiments in magic-angle-spinning (MAS) solid-state NMR can be designed by exploiting the symmetry of internal spin interactions. One such scheme, namely, C521, and its supercycled version SPC521, notated as a five-fold symmetry sequence, is widely used for double-quantum dipole-dipole recoupling. Such schemes are generally rotor synchronised by design. We demonstrate an asynchronous implementation of the SPC521 sequence leading to higher double-quantum homonuclear polarisation transfer efficiency compared to the normal synchronous implementation. Rotor-synchronisation is broken in two different ways: lengthening the duration of one of the pulses, denoted as pulse-width variation (PWV), and mismatching the MAS frequency denoted as MAS variation (MASV). The application of this asynchronous sequence is shown on three different samples, namely, U–13C-alanine and 1,4-13C-labelled ammonium phthalate which include 13Cα-13Cβ, 13Cα-13Co, and 13Co13Co spin systems, and adenosine 5′- triphosphate disodium salt trihydrate (ATP⋅3H2O). We show that the asynchronous version performs better for spin pairs with small dipole-dipole couplings and large chemical-shift anisotropies, for example, 13Co13Co. Simulations and experiments are shown to corroborate the results.

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来源期刊
CiteScore
5.30
自引率
9.40%
发文量
42
审稿时长
72 days
期刊介绍: The journal Solid State Nuclear Magnetic Resonance publishes original manuscripts of high scientific quality dealing with all experimental and theoretical aspects of solid state NMR. This includes advances in instrumentation, development of new experimental techniques and methodology, new theoretical insights, new data processing and simulation methods, and original applications of established or novel methods to scientific problems.
期刊最新文献
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