Solid state nuclear magnetic resonance最新文献

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Field-stepwise-swept solid-state 127I NMR of 1,4-diiodobenzene 1,4-二碘苯的场逐步扫描固态127I核磁共振。
IF 3.2 3区 化学
Solid state nuclear magnetic resonance Pub Date : 2023-12-01 DOI: 10.1016/j.ssnmr.2023.101905
Kazuhiko Yamada , Tatsuo Kaiho
{"title":"Field-stepwise-swept solid-state 127I NMR of 1,4-diiodobenzene","authors":"Kazuhiko Yamada ,&nbsp;Tatsuo Kaiho","doi":"10.1016/j.ssnmr.2023.101905","DOIUrl":"10.1016/j.ssnmr.2023.101905","url":null,"abstract":"<div><p>Field-stepwise-swept solid-state <sup>127</sup>I NMR experiments of 1,4-diiodobenzene, C<sub>6</sub>H<sub>4</sub>I<sub>2</sub>, applied to a Zeeman-perturbed NQR region, have been presented. A series of QCPMG measurements is performed at <em>T</em><span> = 90 K with resonant frequencies of 271 MHz in the range of magnetic fields from 2.5 T to zero with the interval of 12 mT. The spectral simulation<span>, in which a numerical calculation involves the diagonalization of the combined Zeeman-quadrupolar Hamiltonian, provides quadrupole coupling constant (</span></span><em>C</em><sub>Q</sub>) = 1863(5) MHz and the asymmetry parameter (η<sub>Q</sub>) = 0.04(2). The <sup>127</sup><span>I NQR spectrum is observed at </span><em>T</em> = 90 K, which is consistent in the above experimental results.</p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"128 ","pages":"Article 101905"},"PeriodicalIF":3.2,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138499382","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}
引用次数: 0
Kinetics of 1H →31P NMR cross-polarization and dynamics in a layered crystalline α-Sn(IV) phosphate α-Sn(IV)磷酸层状晶体的1H→31P核磁共振交叉极化动力学及动力学
IF 3.2 3区 化学
Solid state nuclear magnetic resonance Pub Date : 2023-10-01 DOI: 10.1016/j.ssnmr.2023.101898
Vladimir I. Bakhmutov, Douglas W. Elliott, Hong-Cai Zhou
{"title":"Kinetics of 1H →31P NMR cross-polarization and dynamics in a layered crystalline α-Sn(IV) phosphate","authors":"Vladimir I. Bakhmutov,&nbsp;Douglas W. Elliott,&nbsp;Hong-Cai Zhou","doi":"10.1016/j.ssnmr.2023.101898","DOIUrl":"https://doi.org/10.1016/j.ssnmr.2023.101898","url":null,"abstract":"<div><p>The proton-phosphorus (H–P) cross-polarization (CP) is effective in Sn(HPO<sub>4</sub>)<sub>2</sub>·H<sub>2</sub>O despite of the presence of paramagnetic ion impurities. Polarization constants T<sub>H-P</sub> and <sup>1</sup>H T<sub>1ρ</sub> times are measured in static Sn(HPO<sub>4</sub>)<sub>2</sub>·H<sub>2</sub>O by the kinetic variable-temperature H–P CP experiments. The temperature dependence of the <sup>1</sup>H T<sub>1ρ</sub><span> times is interpreted in terms of proton movements in the interlayer space occurring between the phosphate groups<span><span> without participation of the water molecules. The process requires an activation energy of 8.7 ± 0.7 kcal/mol. The </span>MAS effect on the </span></span><sup>1</sup>H T<sub>1ρ</sub> times is shown and discussed.</p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"127 ","pages":"Article 101898"},"PeriodicalIF":3.2,"publicationDate":"2023-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49857793","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}
引用次数: 0
Solid-state NMR of organic molecules: Characterising solid-state form 有机分子的固态核磁共振:表征固态形式
IF 3.2 3区 化学
Solid state nuclear magnetic resonance Pub Date : 2023-08-01 DOI: 10.1016/j.ssnmr.2023.101876
Steven P. Brown, Yongchao Su
{"title":"Solid-state NMR of organic molecules: Characterising solid-state form","authors":"Steven P. Brown,&nbsp;Yongchao Su","doi":"10.1016/j.ssnmr.2023.101876","DOIUrl":"10.1016/j.ssnmr.2023.101876","url":null,"abstract":"","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"126 ","pages":"Article 101876"},"PeriodicalIF":3.2,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9975590","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}
引用次数: 0
High resolution solid-state NMR on the desktop 高分辨率固态核磁共振在桌面上
IF 3.2 3区 化学
Solid state nuclear magnetic resonance Pub Date : 2023-08-01 DOI: 10.1016/j.ssnmr.2023.101884
Ke Xu , Fettah Aldudak , Oliver Pecher , Marco Braun , Andreas Neuberger , Holger Foysi , Jörn Schmedt auf der Günne
{"title":"High resolution solid-state NMR on the desktop","authors":"Ke Xu ,&nbsp;Fettah Aldudak ,&nbsp;Oliver Pecher ,&nbsp;Marco Braun ,&nbsp;Andreas Neuberger ,&nbsp;Holger Foysi ,&nbsp;Jörn Schmedt auf der Günne","doi":"10.1016/j.ssnmr.2023.101884","DOIUrl":"10.1016/j.ssnmr.2023.101884","url":null,"abstract":"<div><p><span>High-resolution low-field nuclear magnetic resonance (NMR) spectroscopy has found wide application for characterization of liquid compounds because of the low maintenance cost of modern permanent magnets. Solid-state NMR so far is limited to low-resolution measurements of static powders, because of the limited space available in this type of magnet. Magic-angle sample spinning and low-magnetic fields are an attractive combination to achieve high spectral resolution especially for paramagnetic solids. Here we show that magic angle spinning<span> modules can be miniaturized using 3D printing techniques so that high-resolution solid-state NMR in permanent magnets becomes possible. The suggested conical rotor design was developed using </span></span>finite element<span><span> calculations and provides sample spinning frequencies higher than 20 kHz. The setup was tested on various diamagnetic and paramagnetic compounds including paramagnetic battery materials. The only comparable experiments in low-cost magnets known so far, had been done in the early times of magic angle spinning using electromagnets at much lower sample spinning frequency. Our results demonstrate that high-resolution low-field magic-angle-spinning NMR does not require expensive </span>superconducting magnets and that high-resolution solid-state NMR spectra of paramagnetic compounds are feasible. Generally, this could introduce low-field solid-state NMR for abundant nuclei standard as a routine analytical tool.</span></p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"126 ","pages":"Article 101884"},"PeriodicalIF":3.2,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9982675","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}
引用次数: 0
Remembering Shimon Vega: Special issue on solid-state and DNP NMR 纪念Shimon Vega:固态和DNP NMR特刊
IF 3.2 3区 化学
Solid state nuclear magnetic resonance Pub Date : 2023-08-01 DOI: 10.1016/j.ssnmr.2023.101885
G. Goobes, P.K. Madhu, A. Goldbourt
{"title":"Remembering Shimon Vega: Special issue on solid-state and DNP NMR","authors":"G. Goobes,&nbsp;P.K. Madhu,&nbsp;A. Goldbourt","doi":"10.1016/j.ssnmr.2023.101885","DOIUrl":"10.1016/j.ssnmr.2023.101885","url":null,"abstract":"","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"126 ","pages":"Article 101885"},"PeriodicalIF":3.2,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9988512","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}
引用次数: 0
Spin diffusion in the Phosphorus-31 NMR relaxation in a layered crystalline α-Sn(IV) phosphate contaminated by paramagnetic impurities 顺磁杂质污染层状α-Sn(IV)磷酸盐中磷-31核磁共振弛豫的自旋扩散
IF 3.2 3区 化学
Solid state nuclear magnetic resonance Pub Date : 2023-08-01 DOI: 10.1016/j.ssnmr.2023.101875
Vladimir I. Bakhmutov , Douglas W. Elliott , Nattamai Bhuvanesh , Hong-Cai Zhou
{"title":"Spin diffusion in the Phosphorus-31 NMR relaxation in a layered crystalline α-Sn(IV) phosphate contaminated by paramagnetic impurities","authors":"Vladimir I. Bakhmutov ,&nbsp;Douglas W. Elliott ,&nbsp;Nattamai Bhuvanesh ,&nbsp;Hong-Cai Zhou","doi":"10.1016/j.ssnmr.2023.101875","DOIUrl":"10.1016/j.ssnmr.2023.101875","url":null,"abstract":"<div><p>The study of a layered crystalline Sn(IV) phosphate by solid-state NMR has demonstrated that the <sup>31</sup>P T<sub>1</sub><span><span> relaxation of phosphate groups, dependent on spinning rate is completely controlled by the limited </span>spin diffusion<span> to paramagnetic ions found by EPR. The spin-diffusion constant, D(SD), was estimated as 2.04 10</span></span><sup>−14</sup> cm<sup>2</sup>s<sup>−1</sup>. The conclusion was supported by the <sup>31</sup>P T<sub>1</sub><span> time measurements in zirconium phosphate </span><strong>1</strong>–<strong>1</strong><span>, also showing paramagnetic ions and in diamagnetic compound (NH</span><sub>4</sub>)<sub>2</sub>HPO<sub>4</sub>.</p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"126 ","pages":"Article 101875"},"PeriodicalIF":3.2,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10038540","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}
引用次数: 1
Corrigendum to “Implanted-ion β NMR: A new probe for nanoscience” [Solid State Nucl. Magn. Reson. 68-69 (2015) 1–12] “植入离子βNMR:纳米科学的新探针”勘误表[Solid State Nucl.Magn.Reson.68-69(2015)1-12]
IF 3.2 3区 化学
Solid state nuclear magnetic resonance Pub Date : 2023-08-01 DOI: 10.1016/j.ssnmr.2023.101886
W.A. MacFarlane
{"title":"Corrigendum to “Implanted-ion β NMR: A new probe for nanoscience” [Solid State Nucl. Magn. Reson. 68-69 (2015) 1–12]","authors":"W.A. MacFarlane","doi":"10.1016/j.ssnmr.2023.101886","DOIUrl":"10.1016/j.ssnmr.2023.101886","url":null,"abstract":"","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"126 ","pages":"Article 101886"},"PeriodicalIF":3.2,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9983841","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}
引用次数: 0
Investigating particle size effects on NMR spectra of ions diffusing in porous carbons through a mesoscopic model 通过介观模型研究离子在多孔碳中扩散的粒度对核磁共振谱的影响
IF 3.2 3区 化学
Solid state nuclear magnetic resonance Pub Date : 2023-08-01 DOI: 10.1016/j.ssnmr.2023.101883
Anagha Sasikumar , Céline Merlet
{"title":"Investigating particle size effects on NMR spectra of ions diffusing in porous carbons through a mesoscopic model","authors":"Anagha Sasikumar ,&nbsp;Céline Merlet","doi":"10.1016/j.ssnmr.2023.101883","DOIUrl":"10.1016/j.ssnmr.2023.101883","url":null,"abstract":"<div><p><span><span>Characterizing ion adsorption and diffusion in porous carbons is essential to understand the performance of such materials in a range of key technologies such as energy storage and capacitive deionisation. Nuclear Magnetic Resonance (NMR) spectroscopy is a powerful technique to get insights in these systems thanks to its ability to distinguish between bulk and adsorbed species and to its sensitivity to dynamic phenomena. Nevertheless, a clear interpretation of the experimental results is sometimes rendered difficult by the various factors affecting </span>NMR spectra<span>. A mesoscopic model to predict NMR spectra of ions diffusing in carbon particles is adapted to include dynamic exchange between the intra-particle space and the bulk electrolyte surrounding the particle. A systematic study of the particle size effect on the NMR spectra for different distributions of magnetic environments in the porous carbons is conducted. The model demonstrates the importance of considering a range of magnetic environments, instead of a single chemical shift value corresponding to adsorbed species, and of including a range of exchange rates (between in and out of the particle), instead of a single timescale, to predict realistic NMR spectra. Depending on the </span></span>pore size distribution<span> of the carbon particle and the ratio between bulk and adsorbed species, both the NMR linewidth and peak positions can be largely influenced by the particle size.</span></p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"126 ","pages":"Article 101883"},"PeriodicalIF":3.2,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9984738","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}
引用次数: 0
Determination of the mutual orientation between proton CSA tensors mediated through band-selective 1H–1H recoupling under fast MAS 快速MAS下带选择性1H-1H重耦合介导的质子CSA张量相互取向的测定
IF 3.2 3区 化学
Solid state nuclear magnetic resonance Pub Date : 2023-06-01 DOI: 10.1016/j.ssnmr.2023.101874
Takeshi Kobayashi , Yusuke Nishiyama , Manoj Kumar Pandey
{"title":"Determination of the mutual orientation between proton CSA tensors mediated through band-selective 1H–1H recoupling under fast MAS","authors":"Takeshi Kobayashi ,&nbsp;Yusuke Nishiyama ,&nbsp;Manoj Kumar Pandey","doi":"10.1016/j.ssnmr.2023.101874","DOIUrl":"https://doi.org/10.1016/j.ssnmr.2023.101874","url":null,"abstract":"<div><p><span>The mutual orientation of nuclear spin interaction tensors provides critical information on the conformation and arrangement of molecules in chemicals, materials, and biological systems at an atomic level. Proton is a ubiquitous and important element in a variety of substances, and its NMR is highly sensitive due to their virtually 100% natural abundance and large gyromagnetic ratio. Nevertheless, the measurement of mutual orientation between the </span><sup>1</sup><span>H CSA tensors has remained largely untouched in the past due to strong </span><sup>1</sup>H–<sup>1</sup><span>H homonuclear interactions in a dense network of protons. In this study, we have developed a proton-detected 3D </span><sup>1</sup>H CSA/<sup>1</sup>H CSA/<sup>1</sup>H CS correlation method that utilizes three techniques to manage homonuclear interactions, namely fast magic-angle spinning, windowless <em>C</em>-symmetry-based CSA recoupling (windowless-ROCSA), and a band-selective <sup>1</sup>H–<sup>1</sup><span>H polarization transfer. The asymmetric </span><sup>1</sup>H CSA/<sup>1</sup>H CSA correlated powder patterns produced by the C-symmetry-based methods are highly sensitive to the sign and asymmetry parameter of the <sup>1</sup>H CSA, and the Euler angle <em>β</em> as compared to the symmetric pattern obtained by the existing <em>γ</em>-encoded <em>R</em>-symmetry-based CSA/CSA correlation methods and allows a larger spectral area for data fitting. These features are beneficial for determining the mutual orientation between the nuclear spin interaction tensors with improved accuracy.</p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"125 ","pages":"Article 101874"},"PeriodicalIF":3.2,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49866177","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}
引用次数: 0
Site-specific protein backbone deuterium 2Hα quadrupolar patterns by proton-detected quadruple-resonance 3D 2HαcαNH MAS NMR spectroscopy 质子检测四共振3D 2Hαcα nh MAS核磁共振谱图的位点特异性蛋白主干氘2Hα四极性图谱
IF 3.2 3区 化学
Solid state nuclear magnetic resonance Pub Date : 2023-06-01 DOI: 10.1016/j.ssnmr.2023.101861
Ümit Akbey
{"title":"Site-specific protein backbone deuterium 2Hα quadrupolar patterns by proton-detected quadruple-resonance 3D 2HαcαNH MAS NMR spectroscopy","authors":"Ümit Akbey","doi":"10.1016/j.ssnmr.2023.101861","DOIUrl":"https://doi.org/10.1016/j.ssnmr.2023.101861","url":null,"abstract":"<div><p>A novel deuterium-excited and proton-detected quadruple-resonance three-dimensional (3D) <sup>2</sup>H<sub>α</sub>c<sub>α</sub><span><span>NH MAS </span>nuclear magnetic resonance (NMR) method is presented to obtain site-specific </span><sup>2</sup>H<sub>α</sub><span> deuterium quadrupolar couplings from protein backbone, as an extension to the 2D version of the experiment reported earlier. Proton-detection results in high sensitivity compared to the heteronuclei detection methods. Utilizing four independent radiofrequency (RF) channels (quadruple-resonance), we managed to excite the </span><sup>2</sup>H<sub>α</sub>, then transfer deuterium polarization to its attached C<sub>α</sub><span>, followed by polarization transfers to the neighboring backbone nitrogen and then to the amide proton for detection. This experiment results in an easy to interpret HSQC-like 2D </span><sup>1</sup>H–<sup>15</sup><span>N fingerprint NMR spectrum, which contains site-specific deuterium quadrupolar patterns in the indirect third dimension. Provided that four-channel NMR probe technology is available, the setup of the </span><sup>2</sup>H<sub>α</sub>c<sub>α</sub>NH experiment is relatively straightforward, by using low power deuterium excitation and polarization transfer schemes we have been developing. To our knowledge, this is the first demonstration of a quadruple-resonance MAS NMR experiment to link <sup>2</sup>H<sub>α</sub> quadrupolar couplings to proton-detection, extending our previous triple-resonance demonstrations. Distortion-free excitation and polarization transfer of ∼160–170 kHz <sup>2</sup>H<sub>α</sub><span> quadrupolar coupling were presented by using a deuterium RF strength of ∼20 kHz. From these </span><sup>2</sup>H<sub>α</sub> patterns, an average backbone order parameter of S = 0.92 was determined on a deuterated SH3 sample, with an average η = 0.22. These indicate that SH3 backbone represents sizable dynamics in the microsecond timescale where the <sup>2</sup>H<sub>α</sub> lineshape is sensitive. Moreover, site-specific <sup>2</sup>H<sub>α</sub> T<sub>1</sub> relaxation times were obtained for a proof of concept. This 3D <sup>2</sup>H<sub>α</sub>c<sub>α</sub>NH NMR experiment has the potential to determine structure and dynamics of perdeuterated proteins by utilizing deuterium as a novel reporter.</p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"125 ","pages":"Article 101861"},"PeriodicalIF":3.2,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49858070","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}
引用次数: 1
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