Solid state nuclear magnetic resonance最新文献

{"title":"Transforming solid-state nuclear magnetic resonance towards a chemistry-ready technique","authors":"Raphaële Coulon ,&nbsp;David Gajan ,&nbsp;Wassilios Papawassiliou ,&nbsp;Andrew J. Pell ,&nbsp;Judith Schlagnitweit ,&nbsp;Franck Fayon ,&nbsp;Pierre Florian ,&nbsp;Dominique Massiot ,&nbsp;Armin Afrough ,&nbsp;Dennis W. Juhl ,&nbsp;Thomas Vosegaard ,&nbsp;Linda Cerofolini ,&nbsp;Moreno Lelli ,&nbsp;Massimo Lucci ,&nbsp;Claudio Luchinat ,&nbsp;Ruud L.E.G. Aspers ,&nbsp;Jennifer S. Gómez ,&nbsp;Arno P.M. Kentgens ,&nbsp;Sander F.H. Lambregts ,&nbsp;Y.T. Angel Wong ,&nbsp;Anne Lesage","doi":"10.1016/j.ssnmr.2025.102048","DOIUrl":"10.1016/j.ssnmr.2025.102048","url":null,"abstract":"<div><div>Solid-state nuclear magnetic resonance (solid-state NMR) is an essential tool for probing local structure and dynamics in complex materials, yet its uptake in the broader chemistry community has remained limited by technical and operational barriers. The PANACEA project established a pan-European infrastructure to transform solid-state NMR into a community-ready analytical technique by combining state-of-the-art instrumentation, coordinated user access, and targeted technological innovation. Over three years, PANACEA enabled over 90 user projects across chemistry and materials science, while driving advances in DNP methods, probe design, ultra-fast MAS, and interoperable software platforms such as EasyNMR and CHEMeDATA. This article presents the main outcomes of the initiative, illustrating how infrastructure-driven research and guided access can broaden the impact of solid-state NMR and integrate it into mainstream chemical workflows.</div></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"140 ","pages":"Article 102048"},"PeriodicalIF":2.4,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145404774","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"In-situ solid-state NMR spectroscopy reveals competing crystallization pathways for a system that forms structurally diverse multicomponent crystalline phases","authors":"Rose Gauttier,&nbsp;Colan E. Hughes,&nbsp;Benson M. Kariuki,&nbsp;Kenneth D.M. Harris","doi":"10.1016/j.ssnmr.2025.102046","DOIUrl":"10.1016/j.ssnmr.2025.102046","url":null,"abstract":"<div><div>The development of NMR strategies for <em>in-situ</em> monitoring of crystallization processes has opened the opportunity to establish new mechanistic insights, including to understand the structural evolution of the solid phase produced in crystallization systems as a function of time. In this paper, we report the results of an <em>in-situ</em> solid-state ¹³C NMR study of crystallization from a solution containing 1,10-dihydroxydecane and urea in methanol, leading to the identification of two structurally diverse multicomponent crystalline phases that are formed at different stages of the crystallization process. The initially produced phase is a urea inclusion compound, in which 1,10-dihydroxydecane guest molecules are included within the well-known urea host tunnel structure. Subsequently, a second crystalline phase is formed, which is identified as a stoichiometric hydrogen-bonded co-crystal 1,10-dihydroxydecane-(urea)₂. The <em>in-situ</em> solid-state ¹³C NMR results suggest that the urea inclusion compound is not an intermediate phase on the crystallization pathway to form the co-crystal, as the urea inclusion compound remains after the formation of the co-crystal phase. However, after the appearance of the co-crystal phase, the subsequent crystallization process is dominated by rapid growth of the co-crystal rather than growth of the urea inclusion compound. The results demonstrate the capability of <em>in-situ</em> solid-state NMR strategies to monitor the structural evolution of multicomponent solid phases during crystallization from solution.</div></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"140 ","pages":"Article 102046"},"PeriodicalIF":2.4,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145061265","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Through-space NMR correlations between two different half-integer quadrupolar nuclei using T-HMQC sequences","authors":"Yury G. Kolyagin ,&nbsp;Julien Trébosc ,&nbsp;Olivier Lafon ,&nbsp;Jean-Paul Amoureux","doi":"10.1016/j.ssnmr.2025.102044","DOIUrl":"10.1016/j.ssnmr.2025.102044","url":null,"abstract":"<div><div>Proximities between spin-1/2, e.g. ¹H and ¹³C, and quadrupolar nuclei can be analyzed using HMQC (Heteronuclear Multiple-Quantum Correlation) experiments, in which two continuous-wave irradiations similar to those used in TRAPDOR (TRAnsfer of Population in DOuble-Resonance) experiments are applied on the indirectly detected quadrupolar isotope during the defocusing and refocusing delays. Here, we demonstrate that this sequence, called T-HMQC (T stands for TRAPDOR), can be applied to probe proximities between distinct half-integer spin quadrupolar isotopes. We introduce two novel variants of this sequence to reduce the number of resonances along the indirect dimension. These selective variants employ either (i) an echo-antiecho quadrature detection to only retain the single-quantum (1Q) coherences or (ii) two π-pulses selective of the central-transition (CT) to observe only the 1Q-CT coherences. We analyze how the effects of various experimental parameters, including the synchronization of the TRAPDOR recoupling pulses with the sample rotation, and their radio-frequency (rf) field amplitude and frequency offset, affect the efficiency of ¹¹B-²⁷Al T-HMQC experiments on a magnesium aluminoborate glass. The performances of these T-HMQC sequences are compared to those of the D-HMQC scheme employing the SPI-R³ (Synchronous Phase-Inversion Rotary-Resonance-Recoupling) or REDOR (Rotational-Echo DOuble-Resonance) symmetry-based heteronuclear dipolar recouplings built from CT-selective pulses. We demonstrate that the two TRAPDOR pulses in the T-HMQC sequence must be separated by an integer number of rotor periods and must employ the maximum rf field strength compatible with the probe specifications. Furthermore, as the TRAPDOR pulses distribute the populations equally to all possible coherences, the sensitivity of the T-HMQC selective variants is lower than that of the D-HMQC techniques. To limit this sensitivity decrease and the number of cross-peaks, it is preferable to detect indirectly the quadrupolar nucleus <em>I</em> with the lowest spin number, and in the case of <em>I</em> = 3/2, the resolution along the indirect dimension can be enhanced with respect to a MAS spectrum (for instance, by a factor of 27/7, without taking into account the quadrupolar-induced shift (QIS), through the sole indirect detection of triple-quantum (3Q) coherences). Moreover, owing to the use of a high-power TRAPDOR recoupling, the T-HMQC technique benefits from a wider excitation bandwidth than the D-HMQC methods, which is advantageous for broad NMR spectra, especially at high magnetic fields.</div></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"140 ","pages":"Article 102044"},"PeriodicalIF":2.4,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145259306","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"De novo crystal structure determination of L-alaninamide HCl by quadrupolar NMR crystallography guided crystal structure prediction (QNMRX-CSP)","authors":"Carl H. Fleischer III ,&nbsp;Sean T. Holmes ,&nbsp;Xinsong Lin ,&nbsp;Robert W. Schurko","doi":"10.1016/j.ssnmr.2025.102034","DOIUrl":"10.1016/j.ssnmr.2025.102034","url":null,"abstract":"<div><div>Quadrupolar NMR crystallography guided crystal structure prediction (QNMRX-CSP) is a method for determining the crystal structures of organic solids. To date, our two previous QNMRX-CSP studies have relied upon on ³⁵Cl solid-state NMR (SSNMR) spectroscopy, powder X-ray diffraction (PXRD), Monte-Carlo simulated annealing (MC-SA), and dispersion-corrected density functional theory (DFT-D2∗) calculations for the determination of crystal structures for organic HCl salts with known crystal structures, in order to benchmark the method and subject it to blind tests. Herein, we apply QNMRX-CSP for the <em>de novo</em> crystal structure determination of <em>L</em>-alaninamide HCl (<em>L</em>-Ala-NH₂), for which no crystal structure has been reported, using ³⁵Cl SSNMR and PXRD data for structural prediction and refinement, along with ¹³C and ¹⁴N SSNMR data for subsequent structural validation. To further validate our structural models, we determined the crystal structure of <em>L</em>-Ala-NH₂ using single-crystal X-ray diffraction (SCXRD); however, this structure was not obtained until the completion of the QNMRX-CSP analysis and validation. This study highlights the current capabilities of QNMRX-CSP and underscores the benefits of incorporating multinuclear SSNMR data to enhance <em>de novo</em> crystal structure determination across a wide range of organic solids.</div></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"140 ","pages":"Article 102034"},"PeriodicalIF":2.4,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144899465","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Direct polarization transfer to remote nuclei: Expanding the reach of cross-effect Dynamic Nuclear Polarization","authors":"Amaria Javed ,&nbsp;Ribal Jabbour ,&nbsp;Waqqas Zia ,&nbsp;Asif Equbal","doi":"10.1016/j.ssnmr.2025.102049","DOIUrl":"10.1016/j.ssnmr.2025.102049","url":null,"abstract":"<div><div>Dynamic Nuclear Polarization (DNP) has revolutionized the field of solid-state NMR spectroscopy by significantly improving the sensitivity of nuclear magnetic resonance experiments. Conventionally, cross-effect DNP relies on biradicals to transfer polarization from coupled electron spins to nearby nuclear spins and subsequent relay to target nuclei via a spin diffusion mechanism. However, direct transfer of electron spin polarization to distant nuclei remains a significant challenge due to the small magnitude of effective Hamiltonian, limiting applicability of DNP in various contexts. In this work, we investigate a biradical design concept that involves a very strong electron–electron coupling, with a magnitude of hundreds of MHz, which could enable direct polarization transfer from coupled electron spins to nuclear spins over much longer distances, exceeding 2.0 nm. The concept is experimentally supported using a 14.1 T MAS DNP setup for various nuclei. The use of ASYMPOL-POK, a strongly coupled biradical, results in up to a four-fold increase in long-range <span><math><msup><mrow></mrow><mrow><mn>1</mn></mrow></msup></math></span>H DNP enhancement compared to AMUPOL, a commonly used standard polarizing agent in traditional MAS DNP.</div><div>We also discuss the potential of tailored biradicals in scenarios where conventional spin diffusion mechanisms are inefficient or where direct nuclear spin polarization enhancement or sensing through electron spin interactions is desired. Our study presents an avenue for expanding the scope of cross-effect DNP in solid-state NMR spectroscopy of <span><math><msup><mrow></mrow><mrow><mn>1</mn></mrow></msup></math></span>H, ¹⁹F and ³¹P nuclei, commonly found in various biological and material systems.</div></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"140 ","pages":"Article 102049"},"PeriodicalIF":2.4,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145461884","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Solid-state NMR spectroscopy for unraveling structure and dynamics in biomaterials","authors":"Rahul Yadav ,&nbsp;Bijaylaxmi Patra ,&nbsp;Ratan Rai ,&nbsp;Neeraj Sinha ,&nbsp;Chandan Singh","doi":"10.1016/j.ssnmr.2025.102045","DOIUrl":"10.1016/j.ssnmr.2025.102045","url":null,"abstract":"<div><div>Biomaterials have emerged as essential components in tissue engineering, drug delivery, and regenerative medicine. Bio-composites, cell walls, plant tissues, hybrid materials, and inorganic systems including calcium phosphate and calcium silicate mimic bone's hierarchical architecture and bioactivity. Hydrogels and engineered scaffolds further enhance biomimetic designs by replicating extracellular matrix (ECM) functions. In this regard, solid-state Nuclear Magnetic Resonance (ssNMR) spectroscopy provides details of biomaterials at atomic scale in their intact form, without extraction, purification or perturbing its surrounding components and interfaces. This non-destructive method has been instrumental in obtaining key structural and functional insights in bones, hydrogels, inorganic biomaterials and polysaccharide and oligosaccharide-based biomaterials. This review emphasizes the critical applications of ssNMR in advancing biomaterials, providing key insights into structure-function relationships that are essential for developing innovative therapeutic and biomedical solutions. Specifically, herein demonstrated how ssNMR provides atomic-level insights into molecular organization, dynamics, and interfaces in biomaterials, driving the development of next-generation bio-composites and functional scaffolds. In addition, perspectives of how ssNMR will expand in cell wall research, integrating with imaging and modeling to reveal molecular architecture, advancing biomaterials design, drug delivery, and disease understanding through improved resolution and labeling strategies are discussed.</div></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"140 ","pages":"Article 102045"},"PeriodicalIF":2.4,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145047582","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"In-situ two-dimensional MAS NMR spectroscopy for heterogeneous catalysis","authors":"Lixin Liang ,&nbsp;Daoning Wu ,&nbsp;Guangjin Hou","doi":"10.1016/j.ssnmr.2025.102050","DOIUrl":"10.1016/j.ssnmr.2025.102050","url":null,"abstract":"<div><div><em>In-situ</em> magic-angle spinning (MAS) NMR has emerged as a pivotal technique for elucidating catalytic reaction mechanisms and dynamic structural evolution of catalysts at the atomic level under working conditions. This review summarizes the applications of <em>in-situ</em> MAS NMR in the investigation of catalytic reactions and crystallization processes of catalysts, highlighting its unique capability in real-time monitoring of transient species and structural transformations. Recent advances in specialized NMR hardware (e.g., high-temperature and high-pressure (HTHP) rotors) and pulse sequences (e.g., fast 2D acquisition) have significantly enhanced the sensitivity and acquisition efficiency, enabling unprecedented mechanistic insights via <em>in-situ</em> charactorization. We showcase the latest breakthroughs in catalysis research utilizing <em>in-situ</em> MAS NMR spectroscopy, including methanol conversion, zeolite synthesis, and surface reaction dynamics. This review also emphasizes the transformative integration of HTHP <em>in-situ</em> MAS NMR with fast 2D correlation spectroscopy particularly for quadrupolar nuclei. The importance of combining the hardware (HTHP rotors) and software (pulse sequences) methods is highlighted in developing <em>in-situ</em> MAS NMR, and the key directions for future methodological innovations are discussed.</div></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"140 ","pages":"Article 102050"},"PeriodicalIF":2.4,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145462303","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Hyperfine interactions and magnetic order in oxyborate Co3BO5 according to 10,11B and 59Co NMR data","authors":"A.G. Smolnikov ,&nbsp;M.E. Kashnikova ,&nbsp;N.A. Utkin ,&nbsp;A.F. Sadykov ,&nbsp;Yu.V. Piskunov ,&nbsp;V.V. Ogloblichev ,&nbsp;A.P. Gerashenko ,&nbsp;L.A. Stashkova ,&nbsp;N.V. Kazak","doi":"10.1016/j.ssnmr.2025.102047","DOIUrl":"10.1016/j.ssnmr.2025.102047","url":null,"abstract":"<div><div>Information on the local charge and magnetic environment of ^10,11B and ⁵⁹Co nuclei in homometallic oxyborate Co₃BO₅ has been obtained using NMR spectroscopy. The data were obtained over a wide range of temperatures, in both paramagnetic and magnetically ordered states of the sample, as well as in various magnetic fields. The parameters of the electric field gradient tensor and the values hyperfine fields at the positions of the studied nuclei have been experimentally determined, which is possible only by NMR methods. The data indicate the presence of super-superexchange Co – O – B – O – Co interactions, which presumably occur with the participation of <em>sp</em>²-hybridized orbitals of the B³⁺ ion. A model of super-superexchange involving orbitals of the Co³⁺ ion in the low-spin (LS) 3 d⁶ state is proposed. The ⁵⁹Co NMR data in the magnetically ordered phase most likely relate to cobalt ions in the LS state with local fields of 31.5 (3) kOe induced on the nuclei. Based on NMR data from ^10,11B and ⁵⁹Co, a magnetic order model is proposed in which the magnetic moments of cobalt ions are directed predominantly along the b axis of the crystal.</div></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"140 ","pages":"Article 102047"},"PeriodicalIF":2.4,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145318656","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Measurement of C-H distances in solids at natural abundance via proton-detected fast MAS NMR spectroscopy.","authors":"Yayatika Bhardwaj, Ketan Kumar Rohilla, Yusuke Nishiyama, Manoj Kumar Pandey","doi":"10.1016/j.ssnmr.2025.102031","DOIUrl":"10.1016/j.ssnmr.2025.102031","url":null,"abstract":"<p><p>Measurement of heteronuclear distances from the radio-frequency (rf) pulse-based recoupling of NMR experiments is vital for structural refinement and dynamics studies at the atomic level. Despite advancements in the design and development of recoupling methods, the extraction of the directly-bonded heteronuclear XH distances in samples with XH₂ moieties remains challenging. This is primarily due to the interference effects from the neighboring spins/local fields leading to distorted dipolar coupling powder lineshapes. In this regard, we present a proton-detected 3D ¹³C chemical shift (CS)/¹³C-¹H dipolar coupling/¹H chemical shift (CS) correlation experiment under fast magic angle spinning (MAS), which has the potential to measure the directly-bonded CH distances in naturally abundant samples with CH₂ groups. We have implemented the windowless ROCSA-based ¹³C-¹H dipolar interaction recoupling scheme under ¹H evolution to achieve undistorted ¹³C-¹H dipolar coupling powder lineshapes in contrast to our previously reported windowless ROCSA-DIPSHIFT method under X-nuclei evolution, wherein extraction of the directly-bonded CH distances in samples with CH₂ groups is shown to be sensitive to the presence of the local fields due to neighboring spins. ¹³C-¹H distances reported from the method presented in this work are also validated from the results emerging from the quantum chemical calculations.</p>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"139 ","pages":"102031"},"PeriodicalIF":2.4,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144812414","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"High-quality 13C-detected structural analysis of mass-limited amyloid samples using a CPMAS CryoProbe and moderate magnetic fields","authors":"Sara Andrés-Campos ,&nbsp;Gustavo A. Titaux-Delgado ,&nbsp;Fátima C. Escobedo-González,&nbsp;Miguel Mompeán","doi":"10.1016/j.ssnmr.2025.102028","DOIUrl":"10.1016/j.ssnmr.2025.102028","url":null,"abstract":"<div><div>Solid-state NMR (SSNMR) of biomolecules typically requires several milligrams of sample to achieve sufficient sensitivity for multidimensional experiments, especially when relying on ¹³C detection. Recent developments in fast magic-angle spinning (MAS) and ¹H-detected methods have enabled the use of submilligram samples in reduced-diameter rotors, but these approaches demand advanced hardware and often suffer from limited ¹H chemical shift dispersion. Here, we demonstrate that a CPMAS CryoProbe enables the acquisition of high-quality ¹³C-detected 2D and 3D spectra from just ∼1.5 mg of uniformly labeled amyloid fibrils packed in a standard 3.2 mm rotor. As a proof of concept, we apply this approach to RIPK3, a key protein in immune signaling that forms functional amyloid assemblies. Using standard 3D experiments (NCACX and NCOCX), we obtain ¹³C and ¹⁵N backbone assignments and secondary structure information, despite the limited sample quantity and the use of only moderate magnetic fields. These findings highlight the potential of CPMAS CryoProbes to shift the paradigm in mass-limited SSNMR studies, from relying exclusively on ¹H-detection and fast MAS to reembracing ¹³C-detected strategies.</div></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"139 ","pages":"Article 102028"},"PeriodicalIF":1.8,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144656609","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}