Multi-receiver solid-state NMR using polarization optimized experiments (POE) at ultrafast magic angle spinning

Simultaneous MQMAS NMR Experiments for Two Half-Integer Quadrupolar Nuclei

“…The experiments presented here are a demonstration of the power of multiple receivers in solid-state NMR of materials [1] , [2] , [3] , [4] , [5] , [6] , [7] , [8] , [9] , [10] , [11] , [12] , [13] , [14] , [15] , [16] , [17] , [18] , [19] , [20] , [21] , [22] , [23] , [24] , [25] , [26] , [27] with applications to biological samples also possible [12] , [13] , [65] , [66] . Embedded looping was previously presented for solution and solid-state NMR multiple receiver experiments and is a powerful tool to collect full NMR datasets for small molecules in a short time [49] , [50] , [51] , [52] , [53] , [54] . The core concept of these experiments should be adaptable to many different experiments in materials solid-state NMR such as mixed HETCOR + MQMAS, mixed dimension experiments, (2D + 1D), and more sophisticated MQMAS experiments.…”

“…It is now the standard for commercial spectrometers supplied by Bruker to have a receiver for every channel, lowering the barrier for utilizing multiple receivers so such experiments should become more commonplace. However, it is not yet clear how to best exploit this capability efficiently for solids, although some examples are starting to emerge using spin ½ nuclei for MAS NMR of proteins [52] , [53] , [54] and on a 5-frequency ( 1 H, 19 F, 31 P, 27 Al, and 13 C) probe where 3 receivers are used to measure CP experiments simultaneously using parallel acquisitions [55] .…”

PHRONESIS: A One‐Shot Approach for Sequential Assignment of Protein Resonances by Ultrafast MAS Solid‐State NMR Spectroscopy

“…[1][2][3][4][5][6] The past few years have witnessed a significant effort to speed up the ssNMR experiments using ultrafast magic angle spinning (MAS), dynamic nuclear polarization (DNP), paramagnetic relaxation enhancement (PRE), ultra-high-field magnets, and 1 H detected experiments. [7][8][9][10][11][12][13][14][15][16][17][18] Additionally, the introduction of multi-acquisition polarization optimized experiments (POE) has further boosted data acquisition [19][20][21][22][23] for both solution-and ssNMR spectroscopy. [19][20][21][22][23][24][25][26][27][28][29][30][31][32] Indeed, 1 H detection has significantly improved the sensitivity of fast and ultrafast MAS experiments for fully protonated protein samples; however, the broad line widths of the 1 H resonances reduce the spectral resolution.…”

“…[7][8][9][10][11][12][13][14][15][16][17][18] Additionally, the introduction of multi-acquisition polarization optimized experiments (POE) has further boosted data acquisition [19][20][21][22][23] for both solution-and ssNMR spectroscopy. [19][20][21][22][23][24][25][26][27][28][29][30][31][32] Indeed, 1 H detection has significantly improved the sensitivity of fast and ultrafast MAS experiments for fully protonated protein samples; however, the broad line widths of the 1 H resonances reduce the spectral resolution. [8,14,15,33,34] The latter is often exacerbated by conformational heterogeneity, restricting the range of applications of ssNMR spectroscopy.…”

Rapid structural analysis of minute quantities of organic solids by exhausting 1H polarization in solid-state NMR spectroscopy at fast MAS

“…On one hand, the experimental time of multidimensional solid-state NMR experiments can be substantially reduced by accelerating 1 H spin-lattice relaxation (T1) time, via recycling residual 1 H polarization after low- nuclei signal acquisition, [36][37][38] or selective excitation to accelerate the re-polarization of 1 H that are correlated to the heteronuclear spins of interest. [39][40] On the other hand, multiple acquisition can be implemented in a single scan via multiple detector/receivers [41][42][43] or pulse sequence development by utilizing different magnetization reservoirs and creating multiple polarization transfer pathways. [44][45][46][47] Such strategy is also named as parallel NMR spectroscopy, [48][49] which enables obtaining multiple multidimensional solid-state NMR spectra in a single experiment.…”