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Fast magic angle spinning for the characterization of milligram quantities of organic and biological solids at natural isotopic abundance by 13C–13C correlation DNP-enhanced NMR 快速魔角旋转,通过13C–13C相关性DNP增强NMR表征天然同位素丰度下的毫克有机和生物固体
IF 3.2 3区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2023-02-01 DOI: 10.1016/j.ssnmr.2022.101850
Adam N. Smith , Rania Harrabi , Thomas Halbritter , Daniel Lee , Fabien Aussenac , Patrick C.A. van der Wel , Sabine Hediger , Snorri Th. Sigurdsson , Gaël De Paëpe

We show that multidimensional solid-state NMR 13C–13C correlation spectra of biomolecular assemblies and microcrystalline organic molecules can be acquired at natural isotopic abundance with only milligram quantities of sample. These experiments combine fast Magic Angle Spinning of the sample, low-power dipolar recoupling, and dynamic nuclear polarization performed with AsymPol biradicals, a recently introduced family of polarizing agents. Such experiments are essential for structural characterization as they provide short- and long-range distance information. This approach is demonstrated on diverse sample types, including polyglutamine fibrils implicated in Huntington's disease and microcrystalline ampicillin, a small antibiotic molecule.

我们表明,生物分子组件和微晶有机分子的多维固态NMR 13C–13C相关光谱可以在天然同位素丰度下仅用毫克量的样品获得。这些实验结合了样品的快速魔角旋转、低功率偶极重新耦合和用最近引入的偏振剂家族AsymPol双自由基进行的动态核偏振。这样的实验对结构表征至关重要,因为它们提供了短距离和长距离的信息。这种方法在不同的样本类型上得到了证明,包括与亨廷顿舞蹈症有关的聚谷氨酰胺原纤维和微晶氨苄青霉素,一种小的抗生素分子。
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引用次数: 3
A combined solid-state NMR and quantum chemical calculation study of hydrogen bonding in two forms of α-d-glucose α-d-葡萄糖两种形态氢键的固体核磁共振结合量子化学计算研究
IF 3.2 3区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2023-02-01 DOI: 10.1016/j.ssnmr.2022.101848
Darren H. Brouwer, Janelle G. Mikolajewski

Hydrogen bonding plays an important role in the structure and function of a wide range of materials. Solid-state 1H nuclear magnetic resonance (NMR) spectroscopy provides a very sensitive tool to investigate the local structure of hydrogen atoms involved in hydrogen bonding. While there is extensive 1H solid-state NMR data on O–H - - O hydrogen bonding in solid carboxylic acids, there has been no systematic 1H solid-state NMR studies of hydroxyl groups in carbohydrates (and hydroxyl groups in general). With a view to studying the hydrogen bonding in more complex materials such as cellulose polymorphs, we carried out a detailed solid-state 1H NMR investigation of the model compounds α-d-glucose and α-d-glucose monohydrate. Through a combination of fast magic-angle spinning (MAS), combined rotation and multiple pulse spectroscopy (CRAMPS), and two-dimensional (2D) correlation experiments carried out at ultrahigh magnetic fields, it was possible to assign all of the aliphatic (CH), hydroxyl (OH), and water (H2O) 1H chemical shifts in both forms of α-d-glucose. Plane-wave DFT calculations were employed to improve the hydrogen atom positions for α-d-glucose monohydrate and to calculate 1H chemical shifts, providing additional support for the experimentally determined peak assignments. Finally, the relationship between the hydroxyl 1H chemical shifts and their hydrogen bonding geometry was investigated and compared to the well-established relationship for carboxylic acid protons.

氢键在各种材料的结构和功能中起着重要作用。固态1H核磁共振(NMR)光谱为研究氢键中氢原子的局部结构提供了一种非常灵敏的工具。虽然有大量关于固体羧酸中O–H-O氢键的1H固态NMR数据,但还没有对碳水化合物中的羟基(以及一般的羟基)进行系统的1H固体NMR研究。为了研究更复杂材料(如纤维素多晶型物)中的氢键,我们对模型化合物α-d-葡萄糖和α-d-葡糖一水合物进行了详细的固态1H NMR研究。通过快速魔角自旋(MAS)、组合旋转和多脉冲光谱(CRAMPS)以及在超高磁场下进行的二维(2D)相关实验的组合,可以确定两种形式的α-d-葡萄糖中的所有脂族(CH)、羟基(OH)和水(H2O)的1H化学位移。采用平面波DFT计算来改善α-d-葡萄糖一水合物的氢原子位置,并计算1H化学位移,为实验确定的峰分配提供了额外的支持。最后,研究了羟基1H化学位移与其氢键几何结构之间的关系,并将其与羧酸质子的公认关系进行了比较。
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引用次数: 1
Effective Hamiltonian and spin dynamics in fast MAS TRAPDOR-HMQC experiments involving spin-3/2 quadrupolar nuclei 涉及自旋3/2四极核的快速MAS TRAPDOR-HMQC实验中的有效哈密顿量和自旋动力学
IF 3.2 3区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2022-12-01 DOI: 10.1016/j.ssnmr.2022.101821
Sadasivan V. Sajith , Sundaresan Jayanthi , Adonis Lupulescu

We present a theoretical and numerical description of the spin dynamics associated with TRAPDOR-HMQC (T-HMQC) experiment for a 1H (I) – 35Cl (S) spin system under fast magic angle spinning (MAS). Towards this an exact effective Hamiltonian describing the system is numerically evaluated with matrix logarithm approach. The different magnitudes of the heteronuclear and pure S terms in the effective Hamiltonian allow us to suggest a truncation approximation, which is shown to be in excellent agreement with the exact time evolution. Limitations of this approximation, especially at the rotary resonance condition, are discussed. The truncated effective Hamiltonian is further employed to monitor the buildup of various coherences during TRAPDOR irradiation. We observe and explain a functional resemblance between the magnitude of different terms in the truncated effective Hamiltonian and the amplitudes of various coherences during TRAPDOR irradiation, as function of crystallite orientation. Subsequently, the dependence of the sign (phase) of the T-HMQC signal on the coherence type generated is investigated numerically and analytically. We examine the continuous creation and evolution of various coherences at arbitrary times, i.e., at and between avoided level crossings. Behavior between consecutive crossings is described analytically and reveals ‘quadrature’ evolution of pairs of coherences and coherence interconversions. The adiabatic, sudden, and intermediate regimes for T-HMQC experiments are discussed within the approach established by A. J. Vega. Equations as well as numerical simulations suggest the existence of a driving coherence which builds up between consecutive crossings and then gets distributed at crossings among other coherences. In the intermediate regime, redistribution of the driving coherence to other coherences is almost uniform such that coherences involving S-spin double-quantum terms may be efficiently produced.

本文对快速魔角自旋(MAS)下1H (I) - 35Cl (S)自旋体系的trapor - hmqc (T-HMQC)实验的自旋动力学进行了理论和数值描述。为此,用矩阵对数方法对描述系统的精确有效哈密顿量进行了数值计算。有效哈密顿量中异核和纯S项的不同量级使我们能够提出一个截断近似,该近似被证明与精确的时间演化非常吻合。讨论了这种近似的局限性,特别是在旋转共振条件下。截断的有效哈密顿量进一步用于监测TRAPDOR辐照过程中各种相干的积累。我们观察并解释了截断有效哈密顿量中不同项的幅度与TRAPDOR辐照期间各种相干的幅度之间的函数相似性,作为晶体取向的函数。随后,对T-HMQC信号的符号(相位)与相干型的关系进行了数值和解析研究。我们研究了在任意时间,即在避免的平交道口和之间,各种相干性的连续创造和进化。连续交叉点之间的行为被解析地描述,并揭示了相干对和相干相互转换的“正交”演化。在Vega建立的方法中讨论了T-HMQC实验的绝热、突然和中间状态。方程和数值模拟表明,驱动相干存在于连续的交叉点之间,然后分布在其他相干点之间的交叉点。在中间状态下,驱动相干到其他相干的再分配几乎是均匀的,从而可以有效地产生涉及s自旋双量子项的相干。
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引用次数: 1
Hydrates of active pharmaceutical ingredients: A 35Cl and 2H solid-state NMR and DFT study 活性药物成分的水合物:35Cl和2H固态核磁共振和DFT研究
IF 3.2 3区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2022-12-01 DOI: 10.1016/j.ssnmr.2022.101837
Sean T. Holmes , Cameron S. Vojvodin , Natan Veinberg , Emilia M. Iacobelli , David A. Hirsh , Robert W. Schurko

This study uses 35Cl and 2H solid-state NMR (SSNMR) spectroscopy and dispersion-corrected plane-wave density functional theory (DFT) calculations to characterize the molecular-level structures and dynamics of hydrates of active pharmaceutical ingredients (APIs). We use 35Cl SSNMR to measure the EFG tensors of the chloride ions to characterize hydrated forms of hydrochloride salts of APIs, along with two corresponding anhydrous forms. DFT calculations are used to refine the crystal structures of the APIs and determine relationships between the 35Cl EFG tensors and the spatial arrangements of proximate hydrogen bonds, which are particularly influenced by interactions with water molecules. We find that the relationship between 35Cl EFG tensors and local hydrogen bonding geometries is complex, but meaningful structure/property relationships can be garnered through use of DFT calculations. Specifically, for every case in which such a comparison could be made, we find that the hydrate has a smaller magnitude of CQ than the corresponding anhydrous form, indicating a chloride ion environment with a ground-state electron density of higher spherical symmetry in the former. Finally, variable-temperature 35Cl and 2H SSNMR experiments on a deuterium-exchanged sample of the API cimetidine hydrochloride monohydrate are used to monitor temperature-dependent influences on the spectra that may arise from motional influences on the 35Cl and 2H EFG tensors. From the 2H SSNMR spectra, we determine that the motions of water molecules are characterized by jump-like motions about their C2 rotational axes that occur on timescales that are unlikely to influence the 35Cl central-transition (+1/2 ↔︎ −1/2) powder patterns (this is confirmed by 35Cl SSNMR). Together, these methods show great promise for the future study of APIs in their bulk and dosage forms, especially variable hydrates in which crystallographic water content varies with external conditions such as humidity.

本研究采用35Cl和2H固体核磁共振(SSNMR)光谱和色散校正平面波密度泛函理论(DFT)计算来表征活性药物成分(api)水合物的分子水平结构和动力学。我们使用35Cl SSNMR测量氯离子的EFG张量来表征原料药盐酸盐的水合形式,以及两种相应的无水形式。DFT计算用于改进原料药的晶体结构,并确定35Cl EFG张量与近似氢键的空间排列之间的关系,这种关系特别受与水分子相互作用的影响。我们发现35Cl EFG张量与局部氢键几何形状之间的关系是复杂的,但通过使用DFT计算可以获得有意义的结构/性质关系。具体来说,对于每一种可以进行这种比较的情况,我们发现水合物的CQ值比相应的无水形式的CQ值要小,这表明前者是一个具有更高球对称性基态电子密度的氯离子环境。最后,在API盐酸西米替丁一水合物氘交换样品上进行了35Cl和2H变温SSNMR实验,以监测35Cl和2H EFG张量的运动影响对光谱的温度依赖性影响。从2H SSNMR光谱中,我们确定水分子的运动是以围绕其C2自转轴的跳状运动为特征的,这种运动发生在不太可能影响35Cl中心转移(+1/2↔︎−1/2)粉末模式的时间尺度上(35Cl SSNMR证实了这一点)。总之,这些方法在原料药的散装和剂型的未来研究中显示出巨大的希望,特别是在可变水合物中,晶体水含量随外部条件(如湿度)而变化。
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引用次数: 1
Room temperature DNP of diamond powder using frequency modulation 室温下金刚石粉末DNP采用调频法
IF 3.2 3区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2022-12-01 DOI: 10.1016/j.ssnmr.2022.101833
Daphna Shimon , Kelly Cantwell , Linta Joseph , Chandrasekhar Ramanathan

Dynamic nuclear polarization (DNP) is a method of enhancing NMR signals via the transfer of polarization from electron spins to nuclear spins using microwave (MW) irradiation. In most cases, monochromatic continuous-wave (MCW) MW irradiation is used. Recently, several groups have shown that frequency modulation of the MW irradiation can result in an additional increase in DNP enhancement above that obtained with MCW. The effect of frequency modulation on the solid effect (SE) and the cross effect (CE) has previously been studied using the stable organic radical 4-hydroxy TEMPO (TEMPOL) at temperatures under 20 K. Here, in addition to the SE and CE, we discuss the effect of frequency modulation on the Overhauser effect (OE) and the truncated CE (tCE) in the room-temperature 13C-DNP of diamond powders. We recently showed that diamond powders can exhibit multiple DNP mechanisms simultaneously due to the heterogeneity of P1 (substitutional nitrogen) environments within diamond crystallites. We explore how the two parameters that define the frequency modulation: (i) the Modulation frequency, fm (how fast the microwave frequency is varied) and (ii) the Modulation amplitude, Δω (the magnitude of the change in microwave frequency) influence the enhancement obtained via each mechanism. Frequency modulation during DNP not only allows us to improve DNP enhancement, but also gives us a way to control which DNP mechanism is most active. By choosing the appropriate modulation parameters, we can selectively enhance some mechanisms while simultaneously suppressing others.

动态核极化(DNP)是利用微波辐照将电子自旋的极化转移到核自旋,从而增强核磁共振信号的一种方法。在大多数情况下,使用单色连续波(MCW)毫瓦辐照。最近,一些研究小组已经表明,毫瓦辐射的频率调制可以导致DNP增强的额外增加,而不是MCW获得的。频率调制对固体效应(SE)和交叉效应(CE)的影响已经在20 K以下的温度下用稳定的有机自由基4-羟基TEMPO (TEMPOL)进行了研究。在此,除了SE和CE外,我们还讨论了调频对室温13C-DNP下金刚石粉末的Overhauser效应(OE)和截断CE (tCE)的影响。我们最近发现,由于金刚石晶体内P1(取代氮)环境的非均质性,金刚石粉末可以同时表现出多种DNP机制。我们探讨了定义频率调制的两个参数:(i)调制频率,fm(微波频率变化的速度)和(ii)调制幅度,Δω(微波频率变化的幅度)如何影响通过每种机制获得的增强。在DNP过程中进行频率调制不仅可以提高DNP的增强效果,而且还提供了一种控制哪一种DNP机制最活跃的方法。通过选择适当的调制参数,我们可以选择性地增强某些机制,同时抑制其他机制。
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引用次数: 1
MAS-DNP enables NMR studies of insect wings MAS-DNP使昆虫翅膀的核磁共振研究
IF 3.2 3区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2022-12-01 DOI: 10.1016/j.ssnmr.2022.101838
Frédéric Mentink-Vigier , Samuel Eddy , Terry Gullion

NMR is a valuable tool for studying insects. Solid-state NMR has been used to obtain the chemical composition and gain insight into the sclerotization process of exoskeletons. There is typically little difficulty in obtaining sufficient sample quantity for exoskeletons. However, obtaining enough sample of other insect components for solid-state NMR experiments can be problematic while isotopically enriching them is near impossible. This is especially the case for insect wing membranes which is of interest to us. Issues with obtaining sufficient sample are the thickness of wing membranes is on the order of microns, each membrane region is surrounded by veins and occupies a small area, and the membranes are separated from the wing by physical dissection. Accordingly, NMR signal enhancement methods are needed. MAS-DNP has a track record of providing significant signal enhancements for a wide variety of materials. Here we demonstrate that MAS-DNP is useful for providing high quality one-dimensional and two-dimensional solid-state NMR spectra on cicada wing membrane at natural isotopic abundance.

核磁共振是研究昆虫的重要工具。固态核磁共振已被用于获得化学成分和深入了解外骨骼的硬化过程。一般来说,获得足够数量的外骨骼样本没有什么困难。然而,为固体核磁共振实验获得足够的其他昆虫成分样本可能会有问题,而同位素富集它们几乎是不可能的。这对我们感兴趣的昆虫翅膀膜来说尤其如此。获得足够样品的问题是,机翼膜的厚度在微米量级,每个膜区域被静脉包围并占据很小的面积,并且膜通过物理解剖与机翼分离。因此,需要核磁共振信号增强方法。MAS-DNP具有为各种材料提供显著信号增强的记录。本研究表明,MAS-DNP可用于在自然同位素丰度下提供高质量的蝉翅膜一维和二维固体核磁共振光谱。
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引用次数: 1
New salts of teriflunomide (TFM) – Single crystal X-ray and solid state NMR investigation 新型特氟米特盐(TFM) -单晶x射线和固态核磁共振研究
IF 3.2 3区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2022-12-01 DOI: 10.1016/j.ssnmr.2022.101820
Tomasz Pawlak , Piotr Paluch , Rafał Dolot , Grzegorz Bujacz , Marek J. Potrzebowski

New salts of teriflunomide TFM (drug approved for Multiple Sclerosis treatment) with inorganic counterions: lithium (TFM_Li), sodium (TFM_Na), potassium (TFM_K), rubidium (TFM_Rb), caesium (TFM_Cs) and ammonium (TFM_NH4) were prepared and investigated employing solid state NMR Spectroscopy, Powder X-ray Diffraction PXRD and Single Crystal X-ray Diffraction (SC XRD). Crystal and molecular structures of three salts: TFM_Na (CCDC: 2173257), TFM_Cs (CCDC: 2165288) and TFM_NH4 (CCDC: 2165281) were determined and deposited. Compared to the native TFM, for all crystalline salt structures, a conformational change of the teriflunomide molecule involving about 180-degree rotation of the end group, forming an intramolecular hydrogen bond N–H⋯O is observed. By applying a complementary multi-technique approach, employing 1D and 2D solid state MAS NMR techniques, single and powder X-ray diffraction measurements, as well as the DFT-based GIPAW calculations of NMR chemical shifts for TFM_Na and TFM_Cs allowed to propose structural features of TFM_Li for which it was not possible to obtain adequate material for single crystal X-Ray measurement.

采用固体核磁共振波谱、粉末x射线衍射(PXRD)和单晶x射线衍射(SC XRD)对特立氟米特TFM(批准用于多发性硬化症治疗的药物)的无机反离子锂(TFM_Li)、钠(TFM_Na)、钾(TFM_K)、铷(TFM_Rb)、铯(TFM_Cs)和铵(TFM_NH4)盐进行了研究。测定并沉积了TFM_Na (CCDC: 2173257)、TFM_Cs (CCDC: 2165288)和TFM_NH4 (CCDC: 2165281)三种盐的晶体结构和分子结构。与天然TFM相比,对于所有结晶盐结构,观察到teri氟米特分子的构象变化涉及端基约180度旋转,形成分子内氢键N-H⋯O。通过采用互补的多技术方法,采用1D和2D固态MAS核磁共振技术,单晶和粉末x射线衍射测量,以及基于dft的TFM_Na和TFM_Cs核磁共振化学位移的GIPAW计算,可以提出TFM_Li的结构特征,而单晶x射线测量无法获得足够的材料。
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引用次数: 0
Interaction frames in solid-state NMR: A case study for chemical-shift-selective irradiation schemes 固态核磁共振中的相互作用框架:化学偏移选择性辐照方案的案例研究
IF 3.2 3区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2022-12-01 DOI: 10.1016/j.ssnmr.2022.101834
Matías Chávez, Matthias Ernst

Interaction frames play an important role in describing and understanding experimental schemes in magnetic resonance. They are often used to eliminate dominating parts of the spin Hamiltonian, e.g., the Zeeman Hamiltonian in the usual (Zeeman) rotating frame, or the radio-frequency-field (rf) Hamiltonian to describe the efficiency of decoupling or recoupling sequences. Going into an interaction frame can also make parts of a time-dependent Hamiltonian time independent like the rf-field Hamiltonian in the usual (Zeeman) rotating frame. Eliminating the dominant term often allows a better understanding of the details of the spin dynamics. Going into an interaction frame can also reduces the energy-level splitting in the Hamiltonian leading to a faster convergence of perturbation expansions, average Hamiltonian, or Floquet theory. Often, there is no obvious choice of the interaction frame to use but some can be more convenient than others. Using the example of frequency-selective dipolar recoupling, we discuss the differences, advantages, and disadvantages of different choices of interaction frames. They always include the complete radio-frequency Hamiltonian but can also contain the chemical shifts of the spins and may or may not contain the effective fields over one cycle of the pulse sequence.

相互作用框架在描述和理解磁共振实验方案中起着重要作用。它们通常用于消除自旋哈密顿量的主要部分,例如,通常(塞曼)旋转框架中的塞曼哈密顿量,或射频场(rf)哈密顿量来描述解耦或重耦合序列的效率。进入一个相互作用的坐标系也可以使部分依赖于时间的哈密顿量与时间无关,就像通常(塞曼)旋转坐标系中的rf场哈密顿量。消除占主导地位的术语通常可以更好地理解自旋动力学的细节。进入一个相互作用的框架也可以减少哈密顿量中的能级分裂,从而导致扰动扩展,平均哈密顿量或Floquet理论的更快收敛。通常,没有明显的选择要使用的交互框架,但有些可能比其他更方便。以频率选择性偶极重耦合为例,讨论了不同选择的相互作用框架的差异、优缺点。它们总是包含完整的射频哈密顿量,但也可以包含自旋的化学位移,也可以包含或不包含脉冲序列一个周期内的有效场。
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引用次数: 1
Monitoring the influence of additives on the crystallization processes of glycine with dynamic nuclear polarization solid-state NMR 动态核极化固体核磁共振监测添加剂对甘氨酸结晶过程的影响
IF 3.2 3区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2022-12-01 DOI: 10.1016/j.ssnmr.2022.101836
Marie Juramy , Paolo Cerreia Vioglio , Fabio Ziarelli , Stéphane Viel , Pierre Thureau , Giulia Mollica

Crystallization is fundamental in many domains, and the investigation of the sequence of solid phases produced as a function of crystallization time is thus key to understand and control crystallization processes. Here, we used a solid-state nuclear magnetic resonance strategy to monitor the crystallization process of glycine, which is a model compound in polymorphism, under the influence of crystallizing additives, such as methanol or sodium chloride. More specifically, our strategy is based on a combination of low-temperatures and dynamic nuclear polarization (DNP) to trap and detect transient crystallizing forms, which may be present only in low quantities. Interestingly, our results show that these additives yield valuable DNP signal enhancements even in the absence of glycerol within the crystallizing solution.

结晶是许多领域的基础,研究结晶时间对固相序列的影响是理解和控制结晶过程的关键。在此,我们使用固态核磁共振策略来监测甘氨酸的结晶过程,甘氨酸是一种多态模型化合物,在结晶添加剂(如甲醇或氯化钠)的影响下。更具体地说,我们的策略是基于低温和动态核极化(DNP)的结合来捕获和检测瞬态结晶形式,这可能只存在于少量。有趣的是,我们的结果表明,即使在结晶溶液中没有甘油,这些添加剂也能产生有价值的DNP信号增强。
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引用次数: 1
Teaching product operators using the Vega diagram 教产品操作员使用织女星图
IF 3.2 3区 化学 Q4 CHEMISTRY, PHYSICAL Pub Date : 2022-12-01 DOI: 10.1016/j.ssnmr.2022.101830
Jörg Matysik , Chen Song , Pavlo Bielytskyi , A. Alia

We all will remember Shimon Vega (1942–2021) as wonderful human and scientist. Paramount examples of his scientific work are quoted in this special issue dedicated to his memory. This article is dedicated to remember Shimon Vega as a fantastic teacher. To introduce to the world of product operators, Shimon created a simple scheme that we now call the Vega diagram. It allows for fast analysis of pulse sequences for AX spin systems. Here, we want to document this scheme for future generations.

我们都会记得西蒙·维加(1942-2021)是一位出色的人类和科学家。在这期纪念他的特刊中引用了他科学工作中最重要的例子。这篇文章是为了纪念西蒙·维加这位出色的老师。为了向产品操作员的世界介绍,Shimon创建了一个简单的方案,我们现在称之为Vega图。它允许快速分析AX自旋系统的脉冲序列。在这里,我们想为后代记录下这个计划。
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引用次数: 0
期刊
Solid state nuclear magnetic resonance
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