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Indirectly detected satellite-transition quadrupolar NMR via progressive saturation of the proton reservoir
Solid State Nuclear Magnetic Resonance ( IF 3.2 ) Pub Date : 2023-03-15 , DOI: 10.1016/j.ssnmr.2023.101862
Tamar Wolf 1 , Anna Eden-Kossoy 2 , Lucio Frydman 1
Affiliation  

Static satellite-transitions (ST) NMR line shapes from half-integer quadrupolar nuclei could be very informative: they can deliver insight about local motions over a wide range of timescales, and can report on small changes in the local electronic environments as reflected by variations in the quadrupolar parameters. Satellite transitions, however, are typically “invisible” for half-integer quadrupolar nuclei due to their sheer breadth, leading to low signal-to-noise ratio –especially for unreceptive low-gamma or dilute quadrupolar nuclei. Very recently we have introduced a method for enhancing the NMR sensitivity of unreceptive X nuclei in static solids dubbed PROgressive Saturation of the Proton Reservoir (PROSPR), which opens the possibility of magnifying the signals from such spins by repeatedly imprinting frequency-selective X-driven depolarizations on the much more sensitive 1H NMR signal. Here, we show that PROSPR's efficacy is high enough for enabling the detection of static ST NMR for challenging species like 35Cl, 33S and even 17O –all at natural-abundance. The ensuing ST-PROSPR NMR experiment thus opens new approaches to probe ultra-wideline (6–8 MHz wide) spectra. These highly pronounced anisotropies can in turn deliver new vistas about dynamic changes in solids, as here illustrated by tracking ST line shapes as a function of temperature during thermally-driven events.



中文翻译:

通过质子库的渐进饱和间接检测到卫星过渡四极核磁共振

来自半整数四极核的静态卫星跃迁 (ST) NMR 线形可能提供非常丰富的信息:它们可以提供有关广泛时间尺度内局部运动的洞察力,并且可以报告局部电子环境的微小变化,如变化所反映的在四极参数中。然而,由于半整数四极核的绝对宽度,卫星跃迁通常是“不可见的”,从而导致低信噪比——尤其是对于不接受的低伽马或稀四极核。最近,我们引入了一种增强静态固体中非接受性 X 核的 NMR 灵敏度的方法,称为质子库渐进饱和 (PROSPR),1 H NMR 信号。在这里,我们表明 PROSPR 的功效足以实现静态 ST NMR 检测具有挑战性的物种,如35 Cl、33 S 甚至17 O——所有这些都是自然丰度。因此,随后的 ST-PROSPR NMR 实验开辟了探测超宽线(6-8 MHz 宽)光谱的新方法。这些高度显着的各向异性反过来可以提供有关固体动态变化的新前景,正如此处通过跟踪 ST 线形状作为热驱动事件期间温度的函数所说明的那样。

更新日期:2023-03-15
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