Solid-State NMR at 1.0 GHz: A World-Leading UK Facility to Deliver Advances in Chemistry, Biology and Materials Science

1.0 GHz 固态核磁共振：世界领先的英国设施，推动化学、生物学和材料科学领域的进步

• 批准号: EP/R029946/1
• 负责人: Steven Brown
• 金额: $ 1005.23万
• 依托单位: University of Warwick
• 依托单位国家: 英国
• 项目类别: Research Grant
• 财政年份: 2018
• 资助国家: 英国
• 起止时间: 2018 至 无数据
• 项目状态: 已结题
• 来源: https://gtr.ukri.org/projects?ref=EP%2FR029946%2F1
• 关键词: Solid; State; NMR; 1.0; GHz

It is the structural arrangement and motion of molecules and ions that determine, e.g., the bulk properties of a material or the function of biomolecules. Therefore, the availability of state-of-the-art analytical infrastructure for probing atomic-level structure and dynamics is essential to enable advances across science. The power of solid-state Nuclear Magnetic Resonance (NMR) spectroscopy as such a probe is being increasingly demonstrated by applications to, e.g., materials for use as batteries or for radioactive waste encapsulation or capture of emitted carbon dioxide, pharmaceutical formulations, and protein complexes relevant to illness. Solid-state NMR is most sensitive to the local chemical structure (usually up to a few bond lengths) around a particular nucleus and is thus well suited to characterising the many important systems that lack periodic order, making it complementary to well-established diffraction techniques.To extend the applicability of NMR, two key limiting factors must be addressed: sensitivity, i.e., the relative intensity of spectral peaks as compared to the noise level, and resolution, i.e., the linewidths of individual peaks that determine whether two close-together signals can be separately observed. Both sensitivity and resolution are much improved by performing NMR experiments at higher magnetic field; this proposal is to provide UK researchers with new solid-state NMR capability at a world-leading magnetic field strength of 23.5 Tesla, corresponding to a frequency for the 1H nucleus of 1.0 GHz. This builds on the very successful and well-established UK 850 MHz Solid-State NMR Facility, so as to create a combined 850 MHz and 1.0 GHz Facility whose sustainable ongoing and future operation will be based on the key factors that have enabled the success of the existing 850 MHz Facility: dedicated Facility Manager support and genuine nationwide buy-in achieved through oversight by a national executive and an independent time allocation procedure.The resonance frequencies of different nuclear isotopes are well separated such that an NMR spectrum is specific to a particular chosen isotope. NMR experiments at 23.5 Tesla will make use of as much of the Periodic Table as possible. In solid-state NMR, the experiment is usually performed by physically rotating the sample around an axis inclined at the so-called magic angle of 54.7 degrees to the magnetic field. Nuclei are classified according to their so-called spin quantum number, I. For the two most important I = 1/2 nuclei, 1H and 13C, 1.0 GHz will much benefit so-called inverse (i.e., 1H) detection experiments, e.g., for pharmaceuticals and protein complexes, as well as 13C-13C correlation experiments, e.g., for investigating structure and dynamics in plant cell walls. High magnetic field is particularly important for the study of the over two thirds of NMR-active isotopes that possess an electric quadrupole moment, i.e., a non-spherical distribution of electric charge (I of 1 and above). The residual broadening (in the usual NMR scale of ppm) that remains in the magic-angle spinning experiment is inversely proportional to the magnetic field squared; as well as improving resolution, the concentration of the signal intensity into a narrower lineshape means a still greater sensitivity dependence on the magnetic field strength. Application examples include 14N and 35,37Cl for pharmaceuticals, and 25Mg, 45Sc and 71Ga in materials science.A test of a powerful technique is its applicability to a wide range of problems. The new 1.0 GHz ultra-high magnetic field solid-state NMR facility will make possible experiments that provide unique information for applications across science, ranging from materials for catalysis, radioactive waste encapsulation, batteries, drug delivery, through gaining new understanding of geological processes, to the life sciences, e.g., plant cell walls, protein complexes, membrane proteins and bone structure.

分子和离子的结构排列和运动决定了材料的大量特性或生物分子的功能。因此，最先进的分析基础架构用于探测原子水平的结构和动力学对于能够在科学跨越的进步至关重要。固态核磁共振（NMR）光谱的功能越来越多地证明了用作电池或放射性废物封装或捕获发射二氧化碳，药物配方和与疾病相关的蛋白质复合物的材料。固态NMR对特定核周围的局部化学结构（通常长达几个键长）最敏感，因此非常适合表征缺乏周期性顺序的许多重要系统，从而使其互补地与良好的衍射技术互补。即，单个峰的线宽决定了是否可以单独观察到两个近距离信号。通过在较高的磁场上进行NMR实验，灵敏度和分辨率都大大提高。该提议是为英国研究人员提供新的固态NMR能力，在世界领先的磁场强度为23.5特斯拉，对应于1.0 GHz的1H核的频率。 This builds on the very successful and well-established UK 850 MHz Solid-State NMR Facility, so as to create a combined 850 MHz and 1.0 GHz Facility whose sustainable ongoing and future operation will be based on the key factors that have enabled the success of the existing 850 MHz Facility: dedicated Facility Manager support and genuine nationwide buy-in achieved through oversight by a national executive and an independent time allocation procedure.The resonance frequencies不同的核同位素是很好的分离，因此NMR光谱特定于特定选择的同位素。 23.5特斯拉的NMR实验将尽可能多地使用元素周期表。在固态NMR中，通常是通过将样品物理旋转在与磁场的所谓魔法角度倾斜的轴上进行物理旋转的轴进行。根据其所谓的自旋量子数对核进行分类。对于两个最重要的I = 1/2核，1H和13C，1.0 GHz，将有很大的好处，例如，所谓的逆（1H）检测实验，例如，对于药物和蛋白质复合物以及13C Corelation corlerations corlerations，E.G.，以及用于植物的构造和蛋白质复合物，以及用于E.G. g。高磁场对于研究具有电力四极力矩的NMR活性同位素的三分之二尤其重要，即电荷的非球形分布（I为1及以上）。在魔法旋转实验中保留的残留拓宽（在PPM的通常NMR量表中）与磁场平方成反比。除了改善分辨率外，信号强度的浓度还指向较窄的线形，这意味着对磁场强度的敏感性依赖性仍然更大。申请示例包括用于药物的14N和35,37CL，材料科学中的25mg，45SC和71GA。强大的技术测试是其适用于广泛问题的适用性。新的1.0 GHz超高磁场固态NMR设施将进行可能的实验，从而为跨科学的应用提供独特的信息，从催化，放射性废物封装的材料，电池，药物输送，通过对地质过程的新理解，对生命科学的新理解，等等，植物细胞，植物细胞，蛋白质复合物，蛋白质复合物，骨骼蛋白质，骨膜蛋白和骨骼结构。

项目成果

Revealing carbon capture chemistry with 17-oxygen NMR spectroscopy.

• DOI: 10.1038/s41467-022-35254-w
• 发表时间: 2022-12-15
• 期刊: NATURE COMMUNICATIONS
• 影响因子: 16.6
• 作者: Berge, Astrid H.;Pugh, Suzi M.;Short, Marion I. M.;Kaur, Chanjot;Lu, Ziheng;Lee, Jung-Hoon;Pickard, Chris J.;Sayari, Abdelhamid;Forse, Alexander C.
• 通讯作者: Forse, Alexander C.

Understanding the Degradation of Methylenediammonium and Its Role in Phase-Stabilizing Formamidinium Lead Triiodide.

• DOI: 10.1021/jacs.3c01531
• 发表时间: 2023-05-10
• 期刊: JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
• 影响因子: 15
• 作者: Duijnstee, Elisabeth A.;Gallant, Benjamin M.;Holzhey, Philippe;Kubicki, Dominik J.;Collavini, Silvia;Sturdza, Bernd K.;Sansom, Harry C.;Smith, Joel;Gutmann, Matthias J.;Saha, Santanu;Gedda, Murali;Nugraha, Mohamad I.;Kober-Czerny, Manuel;Xia, Chelsea;Wright, Adam D.;Lin, Yen-Hung;Ramadan, Alexandra J.;Matzen, Andrew;Hung, Esther Y. -H.;Seo, Seongrok;Zhou, Suer;Lim, Jongchul;Anthopoulos, Thomas D.;Filip, Marina R.;Johnston, Michael B.;Nicholas, Robin J.;Delgado, Juan Luis;Snaith, Henry J.
• 通讯作者: Snaith, Henry J.

Discovering the Solid-State Secrets of Lorlatinib by NMR Crystallography: To Hydrogen Bond or not to Hydrogen Bond

通过 NMR 晶体学发现 Lorlatinib 的固态秘密：氢键或非氢键

• DOI: 10.1016/j.xphs.2023.02.022
• 发表时间: 2023
• 期刊: Journal of Pharmaceutical Sciences
• 影响因子: 3.8
• 作者: Rehman Z

Revealing Carbon Capture Chemistry with 17-Oxygen NMR Spectroscopy

利用 17-氧 NMR 光谱揭示碳捕获化学

• DOI: 10.33774/chemrxiv-2021-09vcw
• 发表时间: 2021
• 作者: Berge A