Journal Sciences News
HIV & AIDS Review
August 2018
Editorial Board
Publication date: August 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 92

August 2018
Backbone amide 15N chemical shift tensors report on hydrogen bonding interactions in proteins: A magic angle spinning NMR study
Publication date: August 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 92 Author(s): Sivakumar Paramasivam, Angela M. Gronenborn, Tatyana Polenova Chemical shift tensors (CSTs) are an exquisite probe of local geometric and electronic structure. 15N CST are very sensitive to hydrogen bonding, yet they have been reported for very few proteins to date. Here we present experimental results and statistical analysis of backbone amide 15N CSTs for 100 residues of four proteins, two E. coli thioredoxin reassemblies (1-73-(U-13C,15N)/74-108-(U-15N) and 1-73-(U-15N)/74-108-(U-13C,15N)), dynein light chain 8 LC8, and CAP-Gly domain of the mammalian dynactin. The 15N CSTs were measured by a symmetry-based CSA recoupling method, ROCSA. Our results show that the principal component
August 2018
Two-dimensional 1H and 1H-detected NMR study of a heterogeneous biocatalyst using fast MAS at high magnetic fields
Publication date: August 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 92 Author(s): Sabu Varghese, Peter J. Halling, Daniel H
August 2018
Foreword: Special issue in honor of Alexander J. (Lex) Vega
Publication date: August 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 92 Author(s): Clare P. Grey, Tatyana Polenova, Shimon Vega
August 2018
Automated detection of broad NMR spectra: 19F NMR of paramagnetic UF4 and 195Pt NMR of supported Pt catalysts
Publication date: August 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 92 Author(s): Christopher A. Klug, Joel B. Miller The automated detection of broad NMR spectra via the controlled stepwise motion of the NMR probe along the field axis of the superconducting solenoid is demonstrated for the detection of 19F NMR of paramagnetic UF4 and 195Pt NMR of supported metal catalysts. The sensitivity advantages of performing these measurements at 2.3
July 2018
Pushing the limit of NMR-based distance measurements – retrieving dipolar couplings to spins with extensively large quadrupolar frequencies
Publication date: August 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 92 Author(s): M. Makrinich, E. Nimerovsky, A. Goldbourt Dipolar recoupling under magic-angle spinning allows to measure accurate inter-nuclear distances provided that the two interacting spins can be efficiently and uniformly excited. Alexander (Lex) Vega has shown that adiabatic transfers of populations in quadrupolar spins during the application of constant-wave (cw) radio-frequency pulses lead to efficient and quantifiable dipolar recoupling curves. Accurate distance determination within and beyond the adiabatic regime using cw pulses is limited by the size of the quadrupolar coupling constant. Here we show that using the approach of long-pulse phase modulation, dipolar recoupling and accurate distances can be obtained for nuclei having extensively large quadrupolar frequencies of 5–10
July 2018
Editorial Board
Publication date: July 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 91

July 2018
Separation of 2H NMR spectra assisted by molecular dynamics in diamagnetic and paramagnetic solids
Publication date: July 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 91 Author(s): Takahiro Iijima, Tadashi Shimizu The relaxation-assisted separation method was applied to overlapping 2H nuclear magnetic resonance (NMR) spectra of diamagnetic and paramagnetic solids to separate them based on the different relaxation behaviors caused by molecular motion. Carr–Purcell–Meiboom–Gill sequences for 2H NMR were adopted to build two-dimensional data sets from one-dimensional NMR experiments. For diamagnetic
July 2018
Description of an rf field-strength controller for solid-state NMR experiments
Publication date: July 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 91 Author(s): Gregory Lusk, Terry Gullion Some MAS NMR experiments are sensitive to fluctuations or drifts in rf field strengths. We examine the simple 1H-13C CPMAS experiment and show that the 13C signal intensities vary over time due to drifts in rf field strengths. The causes of the drifts in rf field strengths are studied. Stabilization of the rf field strengths are obtained by using an rf field-strength controller. The controller is a stand-alone unit, which can be easily incorporated in any spectrometer system. Details of the controller, including circuit design, are provided.

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Available online 17 May 2018
Direct detection and characterization of bioinorganic peroxo moieties in a vanadium complex by 17O solid-state NMR and density functional theory
Publication date: July 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 91 Author(s): Rupal Gupta, John Stringer, Jochem Struppe, Dieter Rehder, Tatyana Polenova Electronic and structural properties of short-lived metal-peroxido complexes, which are key intermediates in many enzymatic reactions, are not fully understood. While detected in various enzymes, their catalytic properties remain elusive because of their transient nature, making them difficult to study spectroscopically. We integrated 17O solid-state NMR and density functional theory (DFT) to directly detect and characterize the peroxido ligand in a bioinorganic V(V) complex mimicking intermediates non-heme vanadium haloperoxidases. 17O chemical shift and quadrupolar tensors, measured by solid-state NMR spectroscopy, probe the electronic structure of the peroxido ligand and its interaction with the metal. DFT analysis reveals the unusually large chemical shift anisotropy arising from the metal orbitals contributing towards the magnetic shielding of the ligand. The results illustrate the power of an integrated approach for studies of oxygen centers in enzyme reaction intermediates.

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Available online 13 April 2018
Acetone mobility in zeolite cages with new features in the deuteron NMR spectra and relaxation
Publication date: Available online 17 May 2018
Source:Solid State Nuclear Magnetic Resonance Author(s): E.E. Ylinen, M. Punkkinen, A. Birczy
April–May 2018
Measurement of proton chemical shift anisotropy in solid-state NMR spectroscopy
Publication date: Available online 13 April 2018
Source:Solid State Nuclear Magnetic Resonance Author(s): Lixin Liang, Guangjin Hou, Xinhe Bao Proton chemical shift anisotropy (CSA) is significantly important as it provides the dynamics and local environment of the proton. The measurement of proton CSA keeps drawing the attention of researchers, and great efforts have been expended. In the early years for solid state NMR, measuring proton CSA was hampered by ineffective ling-narrowing method and the influence from strong H-H dipolar network, and the samples were limited to those with sparse proton sites or single crystals. In the latest decades, the dramatic progress of both pulse sequence and magic-angle spinning (MAS) techniques enables direct detection of proton CSA in complicated powder samples even including proteins, while the indirect detection in solution and liquid crystals (LCs) is accomplished via cross-relaxation experiment and residual CSA respectively. In this review, from the continuous wave (CW) and multiple pulse sequence for detecting static solid samples, to combined rotation and multiple pulse spectroscopy (CRAMPS), then to the latest method such as rotary resonance, CSA amplification and R-symmetry pulse sequences under MAS conditions, a retrospect of the experimental development of proton CSA measurement in solid state NMR is presented, with brief description of the measurement of proton CSA in solution and LCs NMR included.

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April–May 2018
Editorial Board
Publication date: April–May 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 90

April–May 2018
Host-guest interaction of styrene and ethylbenzene in MIL-53 studied by solid-state NMR
Publication date: April–May 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 90 Author(s): Shenhui Li, Jing Li, Jing Tang, Feng Deng Solid-state NMR was utilized to explore the host-guest interaction between adsorbate and adsorbent at atomic level to understand the separation mechanism of styrene (St) and ethylbenzene (EB) in MIL-53(Al). 13C-27Al double-resonance NMR experiments revealed that the host-guest interaction between St and MIL-53 was much stronger than that of EB adsorption. In addition, 13C DIPSHIFT experiments suggested that the adsorbed St was less mobile than EB confined inside the MIL-53 pore. Furthermore, the host-guest interaction model between St, EB and MIL-53 was established on the basis of the spatial proximities information extracted from 2D 1H-1H homo-nuclear correlation NMR experiments. According to the experimental observation from solid-state NMR, it was found that the presence of
April–May 2018
Simultaneous homonuclear and heteronuclear spin decoupling in magic-angle spinning solid-state NMR
Publication date: April–May 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 90 Author(s): Kaustubh R. Mote, Perunthiruthy K. Madhu We show here an effective way of implementing simultaneously homonuclear and heteronuclear dipolar decoupling in magic-angle spinning (MAS) solid-state NMR. Whilst the homonuclear spin decoupling is applied on the 1H channel, heteronuclear spin decoupling is applied on the 13C channel. The 1H spins are observed in a windowed fashion in this case. The resultant 1H spectrum has higher resolution due to the attenuation of broadening arising from both homonuclear 1H-1H and heteronuclear 1H-13C interactions, with the latter normally leading to additional line broadening in 13C labelled samples. The experiments are performed at MAS frequencies of ca. 60
February 2018
Corrigendum to “1H NMR study of water molecules confined in nanochannels of mordenite” [Solid State Nucl. Magn. Reson. 76-77 (2016) 24–28]
Publication date: April–May 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 90 Author(s): A.M. Panich, N.A. Sergeev, M. Paczwa, M. Olszewski
February 2018
Editorial Board
Publication date: February 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 89

February 2018
Tin chemical shift anisotropy in tin dioxide: On ambiguity of CSA asymmetry derived from MAS spectra
Publication date: February 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 89 Author(s): Abil E. Aliev, Albert P. Bart
February 2018
NMR interaction tensors of 51V and 207Pb in vanadinite, Pb5(VO4)3Cl, determined from DFT calculations and single-crystal NMR measurements, using only one general rotation axis
Publication date: February 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 89 Author(s): Otto E.O. Zeman, Constantin Hoch, Rupert Hochleitner, Thomas Br
February 2018
Molecular dynamics of palmitic acid and lead palmitate in cross-linked linseed oil films: Implications from deuterium magnetic resonance for lead soap formation in traditional oil paintings
Publication date: February 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 89 Author(s): Jaclyn Catalano, Anna Murphy, Yao Yao, Nicholas Zumbulyadis, Silvia A. Centeno, Cecil Dybowski Many oil paintings, dating from the 15th century to the present, are affected by the formation of heavy-metal carboxylates (soaps) that alter the structural integrity and appearance of the works. Through transport phenomena not yet understood, free fatty acids formed from oils used as binders migrate through the paint film and react with heavy-metal ions that are constituents of pigments and/or driers, forming metal carboxylates. The local molecular dynamics of fatty acids and metal carboxylates are factors influencing material transport in these systems. We report temperature-dependent 2H NMR spectra of palmitic acid and lead palmitate as pure materials, in cross-linked linseed oil films, and in a lead white linseed oil paint film as part of our broader research into metal soap formation. Local dynamics at the
February 2018
Efficient low-power TOBSY sequences for fast MAS
Publication date: February 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 89 Author(s): Kong Ooi Tan, Vipin Agarwal, Nils-Alexander Lakomek, Susanne Penzel, Beat H. Meier, Matthias Ernst Through-bond J-coupling based experiments in solid-state NMR spectroscopy are challenging because the J couplings are typically much smaller than the dipolar couplings. This often leads to a lower transfer efficiency compared to dipolar-coupling based sequences. One of the reasons for the low transfer efficiency are the second-order cross terms involving the strong heteronuclear dipolar couplings leading to fast magnetization decay. Here, we show that by employing a symmetry-based C9 sequence, which was carefully selected to suppress second-order terms, efficient polarization transfers of up to 80% can be achieved without decoupling on fully protonated two-spin model systems at a MAS frequency of 55.5 kHz with rf-field amplitudes of about 25 kHz. In addition, we analyse the effects of rf inhomogeneity and crystallites selection due to the polarization preparation method on the TOBSY transfer efficiency. We demonstrate on small model substances as well as on deuterated and 100% back-exchanged ubiquitin that $C 9 39 1$ and $C 9 48 1$ are efficient and practical TOBSY sequences at experimental conditions ranging from proton Larmor frequencies of 400–850 MHz, and MAS frequencies ranging from 55.5 to 111.1 kHz.

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February 2018
Protein dynamics in the solid-state from 2H NMR lineshape analysis. III. MOMD in the presence of Magic Angle Spinning
Publication date: February 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 89 Author(s): Eva Meirovitch, Zhichun Liang, Jack H. Freed We report on a new approach to the analysis of dynamic NMR lineshapes from polycrystalline (i.e., macroscopically disordered) samples in the presence of Magic Angle Spinning (MAS). This is an application of the Stochastic Liouville Equation developed by Freed and co-workers for treating restricted (i.e., microscopically ordered) motions. The 2H nucleus in an internally-mobile C–CD3 moiety serves as a prototype probe. The acronym is 2H/MOMD/MAS, where MOMD stands for “microscopic-order-macroscopic-disorder.” The key elements describing internal motions – their type, the local spatial restrictions, and related features of local geometry – are treated in MOMD generally, within their rigorous three-dimensional tensorial requirements. Based on this representation a single physically well-defined model of local motion has the capability of reproducing experimental spectra. There exist other methods for analyzing dynamic 2H/MAS spectra which advocate simple motional modes. Yet, to reproduce satisfactorily the experimental lineshapes, one has either to use unusual parameter values, or combine several simple motional modes. The multi-simple-mode reasoning assumes independence of the constituent modes, features ambiguity as different simple modes may be used, renders inter-system comparison difficult as the overall models differ, and makes possible model-improvement only by adding yet another simple mode, i.e., changing the overall model. 2H/MOMD/MAS is free of such limitations and inherently provides a clear physical interpretation. These features are illustrated. The advantage of 2H/MOMD/MAS in dealing with sensitive but hardly investigated slow-motional lineshapes is demonstrated by applying it to actual experimental data. The results differ from those obtained previously with a two-site exchange scheme that yielded unusual parameters.

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November 2017
Selective observation of charge storing ions in supercapacitor electrode materials
Publication date: February 2018
Source:Solid State Nuclear Magnetic Resonance, Volume 89 Author(s): Alexander C. Forse, John M. Griffin, Clare P. Grey Nuclear magnetic resonance (NMR) spectroscopy has emerged as a useful technique for probing the structure and dynamics of the electrode-electrolyte interface in supercapacitors, as ions inside the pores of the carbon electrodes can be studied separately from bulk electrolyte. However, in some cases spectral resolution can limit the information that can be obtained. In this study we address this issue by showing how cross polarisation (CP) NMR experiments can be used to selectively observe the in-pore ions in supercapacitor electrode materials. We do this by transferring magnetisation from 13C nuclei in porous carbons to nearby nuclei in the cations (1H) or anions (19F) of an ionic liquid. Two-dimensional NMR experiments and CP kinetics measurements confirm that in-pore ions are located within
November 2017
Editorial Board
Publication date: November 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 88

November 2017
Insights into protein misfolding and aggregation enabled by solid-state NMR spectroscopy
Publication date: November 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 88 Author(s): Patrick C.A. van der Wel The aggregation of proteins and peptides into a variety of insoluble, and often non-native, aggregated states plays a central role in many devastating diseases. Analogous processes undermine the efficacy of polypeptide-based biological pharmaceuticals, but are also being leveraged in the design of biologically inspired self-assembling materials. This Trends article surveys the essential contributions made by recent solid-state NMR (ssNMR) studies to our understanding of the structural features of polypeptide aggregates, and how such findings are informing our thinking about the molecular mechanisms of misfolding and aggregation. A central focus is on disease-related amyloid fibrils and oligomers involved in neurodegenerative diseases such as Alzheimer's, Parkinson's and Huntington's disease. SSNMR-enabled structural and dynamics-based findings are surveyed, along with a number of resulting emerging themes that appear common to different amyloidogenic proteins, such as their compact alternating short-
November 2017
Spin diffusion and 1H spin-lattice relaxation in Cs2(HSO4)(H2PO4) containing a small amount of ammonium ions
Publication date: November 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 88 Author(s): Shigenobu Hayashi, Keiko Jimura Inorganic solid acid salts with hydrogen bond networks frequently show very long spin-lattice relaxation times even for 1H because the hydrogen bonds suppress motions. In the present work, the 1H spin-lattice relaxation in Cs2(HSO4)(H2PO4) containing a small amount of ammonium ions were studied in detail by use of the effect of magic angle spinning (MAS) on the relaxation. The 1H spin-lattice relaxation times of the acid protons decrease with increase in the content of ammonium ions. Reorientation of the NH4 group fluctuates the dipole-dipole interaction and relaxes the ammonium protons as well as the acid protons. The 1H relaxation times of the acid protons are a little bit longer than those of the ammonium protons at the MAS rate of 8 kHz. The spinning at 50 kHz makes the relaxation times of the acid protons longer and those of the ammonium protons shorter. Spin diffusion between the acid and the ammonium protons averages partially the 1H relaxation of the acid and the ammonium protons at the MAS rate of 8 kHz. The spin diffusion is suppressed completely at the MAS rate of 50 kHz. Spin diffusion between the acid protons is not suppressed at the MAS rate of 50 kHz. The acid protons always show the same relaxation times. The intrinsic relaxation times not affected by spin diffusion are evaluated quantitatively for both the acid and the ammonium protons. Those values are independent of the ammonium content. Contribution of the spin diffusion between the acid and the ammonium protons to the relaxation is estimated quantitatively. Using those parameters, the effect of ammonium ions on the 1H spin-lattice relaxation can be predicted. The 1H spin-lattice relaxation is a sensitive tool to study the distribution of ammonium ions in solids.

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November 2017
Comparing the efficacy of solid and magic-echo refocusing sequences: Applications to 1H NMR echo spectroscopy of shale rock
Publication date: November 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 88 Author(s): Gregory S. Boutis, Ravinath Kausik Quantitative evaluation of the solid and viscous components of unconventional shale rock, namely kerogen and bitumen, is important for understanding reservoir quality. Short transverse coherence times, due to strong 1H-1H dipolar interactions, motivates the application of solid state refocusing pulse sequences that allow for investigating components of the free-induction decay that are otherwise obscured by instrumental effects such as probe ringdown. This work reports on static, wide-line 1H spectroscopy of shale rock and their extracted components, which include kerogen and bitumen, by the application of solid echo and magic echo pulse sequences. We characterize the efficiency of these cycles as a function of the radio frequency power and inter-pulse spacing. Magic echos are shown to provide superior refocusing in comparison to solid echo based experiments, as can be understood from the truncation of the Magnus expansion and ability to also refocus any $I z$ Hamiltonians (e.g. static field inhomogeneity). We characterize the optimal echo spacing and RF power for two shale samples of different maturity, motivating routine core and cuttings analysis and applications.

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October 2017
TOC
Publication date: November 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 88

October 2017
Editorial Board
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87

October 2017
Identification of double four-ring units in germanosilicate ITQ-13 zeolite by solid-state NMR spectroscopy
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Xiaolong Liu, Yueying Chu, Qiang Wang, Weiyu Wang, Chao Wang, Jun Xu, Feng Deng Well-crystallized Ge-free and Ge-ITQ-13 were successfully obtained by solid state synthesis method. The Ge/Si ratio and the water content that are the two important factors in the synthesis of germanosilicate zeolites were explored for the formation of ITQ-13. The effect of the mineralizing agents (NH4F and NH4Cl) on the ITQ-13 synthesis was investigated as well. The obtained pure silica ITQ-13 and Ge-ITQ-13 were characterized by one- and two-dimensional solid- state NMR techniques. One-dimensional (1D) 19F MAS, 1H
October 2017
Energy efficiency increase of NQR spectrometer transmitter at pulse resonance excitation with noise signals
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): A. Samila, V. Khandozhko, L. Politansky The specific feature of NQR is expansion of spectral lines which is caused not only by dipole-dipole interaction of nuclei, but also by local field nonuniformity caused by the defects and deformation in crystal matrix. Considerable line expansion, which is typical of crystals, requires in pulsed NQR method the optimization of pulse shape and the reserve of transmitter power output. Parametric computer identification was used to study a dependence of parameters of the energy spectra of the output signal of pulsed NQR spectrometer transmitter on the duration of excitation pulses with sine and noise occupation. The energy efficiency of a linear amplifier was calculated and experimental investigations of its temperature conditions were carried out. The energy-efficient broadband transmitter was proposed that can be used in portable setups for the pursuance of research in the field of pulsed NQR spectroscopy, for instance when studying isotopes with quadrupole moments 14N, 35Cl, 63Cu, 69Ga, 71Ga, 113In, 115In and others.

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October 2017
A model to describe the inhomogeneous broadening of NQR lines in chlorohalobenzenes with orientational or substitutional disorder
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Silvina C. P
October 2017
Detailed mechanisms of 1H spin-lattice relaxation in ammonium dihydrogen phosphate confirmed by magic angle spinning
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Shigenobu Hayashi, Keiko Jimura Mechanisms of the 1H spin-lattice relaxation in NH4H2PO4 were studied in detail by use of the effect of magic angle spinning on the relaxation. The acid and the ammonium protons have different relaxation times at the spinning rates higher than 10 kHz due to suppression of spin diffusion between the two kinds of protons. The intrinsic relaxation times not affected by the spin diffusion and the spin-diffusion assisted relaxation times were evaluated separately, taking into consideration temperature dependence. Both mechanisms contribute to the 1H relaxation of the acid protons comparatively. The spin-diffusion assisted relaxation mechanism was suppressed to the level lower than the experimental errors at the spinning rate of 30 kHz.

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October 2017
Assignment of solid-state 13C and 1H NMR spectra of paramagnetic Ni(II) acetylacetonate complexes aided by first-principles computations
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Syed Awais Rouf, Vibe Boel Jakobsen, Ji
October 2017
Improved strategies for DNP-enhanced 2D 1H-X heteronuclear correlation spectroscopy of surfaces
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Takeshi Kobayashi, Fr
October 2017
Solid-state NMR spectroscopic trends for supramolecular assemblies and protein aggregates
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Rasmus Linser Solid-state NMR is able to generate structural data on sample preparations that are explicitly non-crystalline. In particular, for amyloid fibril samples, which can comprise significant degrees of sample disorder, solid-state NMR has been used very successfully. But also solid-state NMR studies of other supramolecular assemblies that have resisted assessment by more standard methods are being performed with increasing ease and biological impact, many of which are briefly reviewed here. New technical trends with respect to structure calculation, protein dynamics and smaller sample amounts have reshaped the field of solid-state NMR recently. In particular, proton-detected approaches based on fast Magic-Angle Spinning (MAS) were demonstrated for crystalline systems initially. Currently, such approaches are being expanded to the above-mentioned non-crystalline targets, the characterization of which can now be pursued with sample amounts on the order of a milligram. In this Trends article, I am giving a brief overview about achievements of the last years as well as the directions that the field has been heading into and delineate some satisfactory perspectives for solid-state NMR's future striving.

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October 2017
Investigation of zeolitic imidazolate frameworks using 13C and 15N solid-state NMR spectroscopy
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Scott Sneddon, J
October 2017
Preface: Ultrafast magic-angle spinning NMR
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Marek J. Potrzebowski
October 2017
1H CSA parameters by ultrafast MAS NMR: Measurement and applications to structure refinement
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Habeeba K. Miah, Rosalie Cresswell, Dinu Iuga, Jeremy J. Titman A 1H anisotropic-isotropic chemical shift correlation experiment which employs symmetry-based recoupling sequences to reintroduce the chemical shift anisotropy in
October 2017
Probing intermolecular interactions in a diethylcarbamazine citrate salt by fast MAS 1H solid-state NMR spectroscopy and GIPAW calculations
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Tiago Ven
October 2017
Hydrogen bond strength in membrane proteins probed by time-resolved 1H-detected solid-state NMR and MD simulations
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Jo
October 2017
1H-31P CPVC NMR method under Very Fast Magic Angle Spinning for analysis of dipolar interactions and dynamics processes in the crystalline phosphonium tetrafluoroborate salts
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Piotr Paluch, Julien Tr
October 2017
Resolution enhancement in proton double quantum magic-angle spinning spectra by constant-time acquisition
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Henri Colaux, Yusuke Nishiyama Although very fast MAS rate (>60 kHz) paves a way to obtain a sufficient resolution in the 1H double-quantum magic-angle spinning (DQMAS) experiments to probe 1H proximities, the 1H resolution still limits wider applications below its potential use. Here, the combination of the DQMAS experiment with the constant-time (CT) acquisition approach is demonstrated, giving an increased peak-separation power in the DQ dimension. The advantages and disadvantages in terms of sensitivity and resolution of the conventional and CT approaches are discussed.

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October 2017
Minimizing the t1-noise when using an indirect 1H high-resolution detection of unlabeled samples
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): M. Shen, S. Wegner, J. Tr
October 2017
Expanding the horizons for structural analysis of fully protonated protein assemblies by NMR spectroscopy at MAS frequencies above 100 kHz
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Jochem Struppe, Caitlin M. Quinn, Manman Lu, Mingzhang Wang, Guangjin Hou, Xingyu Lu, Jodi Kraus, Loren B. Andreas, Jan Stanek, Daniela Lalli, Anne Lesage, Guido Pintacuda, Werner Maas, Angela M. Gronenborn, Tatyana Polenova The recent breakthroughs in NMR probe technologies resulted in the development of MAS NMR probes with rotation frequencies exceeding 100 kHz. Herein, we explore dramatic increases in sensitivity and resolution observed at MAS frequencies of 110–111 kHz in a novel 0.7 mm HCND probe that enable structural analysis of fully protonated biological systems. Proton- detected 2D and 3D correlation spectroscopy under such conditions requires only 0.1–0.5 mg of sample and a fraction of time compared to conventional 13C-detected experiments. We discuss the performance of several proton- and heteronuclear- (13C-,15N-) based correlation experiments in terms of sensitivity and resolution, using a model microcrystalline fMLF tripeptide. We demonstrate the applications of ultrafast MAS to a large, fully protonated protein assembly of the 231-residue HIV-1 CA capsid protein. Resonance assignments of protons and heteronuclei, as well as 1H-15N dipolar and 1HN CSA tensors are readily obtained from the high sensitivity and resolution proton-detected 3D experiments. The approach demonstrated here is expected to enable the determination of atomic-resolution structures of large protein assemblies, inaccessible by current methodologies.

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October 2017
Is protein deuteration beneficial for proton detected solid-state NMR at and above 100 kHz magic-angle spinning?
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Diane Cala-De Paepe, Jan Stanek, Kristaps Jaudzems, Kaspars Tars, Loren B. Andreas, Guido Pintacuda 1H-detection in solid-state NMR of proteins has been traditionally combined with deuteration for both resolution and sensitivity reasons, with the optimal level of proton dilution being dependent on MAS rate. Here we present 1H-detected 15N and 13C CP-HSQC spectra on two microcrystalline samples acquired at 60 and 111 kHz MAS and at ultra-high field. We critically compare the benefits of three labeling schemes yielding different levels of proton content in terms of resolution, coherence lifetimes and feasibility of scalar-based 2D correlations under these experimental conditions. We observe unexpectedly high resolution and sensitivity of aromatic resonances in 2D 13C-1H correlation spectra of protonated samples. Ultrafast MAS reduces or even removes the necessity of 1H dilution for high-resolution 1H-detection in biomolecular solid-state NMR. It yields 15N,1H and 13C,1H fingerprint spectra of exceptional resolution for fully protonated samples, with notably superior 1H and 13C lineshapes for side-chain resonances.

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October 2017
Imaging the spatial distribution of radiofrequency field, sample and temperature in MAS NMR rotor
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Hiroki Nagashima, Julien Tr

Corrigendum to “Accurate NMR determination of C–H or N–H distances for unlabeled molecules” [Solid State Nuclear Magnetic Resonance 73 (2016) 15–21]
Publication date: October 2017
Source:Solid State Nuclear Magnetic Resonance, Volume 87 Author(s): Y. Nishiyama, M. Malon, M.J. Potrzebowski, P. Paluch, J.P. Amoureux
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