Thompson Niklas B, Mulfort Karen L, Tiede David M
Division of Chemical Sciences and Engineering, Argonne National Laboratory, 9700 South Cass Avenue, Lemont, Illinois 60439 USA.
IUCrJ. 2024 May 1;11(Pt 3):423-433. doi: 10.1107/S2052252524003282.
Appreciating that the role of the solute-solvent and other outer-sphere interactions is essential for understanding chemistry and chemical dynamics in solution, experimental approaches are needed to address the structural consequences of these interactions, complementing condensed-matter simulations and coarse-grained theories. High-energy X-ray scattering (HEXS) combined with pair distribution function analysis presents the opportunity to probe these structures directly and to develop quantitative, atomistic models of molecular systems in situ in the solution phase. However, at concentrations relevant to solution-phase chemistry, the total scattering signal is dominated by the bulk solvent, prompting researchers to adopt a differential approach to eliminate this unwanted background. Though similar approaches are well established in quantitative structural studies of macromolecules in solution by small- and wide-angle X-ray scattering (SAXS/WAXS), analogous studies in the HEXS regime-where sub-ångström spatial resolution is achieved-remain underdeveloped, in part due to the lack of a rigorous theoretical description of the experiment. To address this, herein we develop a framework for differential solution scattering experiments conducted at high energies, which includes concepts of the solvent-excluded volume introduced to describe SAXS/WAXS data, as well as concepts from the time-resolved X-ray scattering community. Our theory is supported by numerical simulations and experiment and paves the way for establishing quantitative methods to determine the atomic structures of small molecules in solution with resolution approaching that of crystallography.
认识到溶质 - 溶剂以及其他外层球相互作用的作用对于理解溶液中的化学和化学动力学至关重要,需要实验方法来研究这些相互作用的结构后果,以补充凝聚态模拟和粗粒度理论。高能X射线散射(HEXS)结合对分布函数分析为直接探测这些结构以及在溶液相中原位开发分子系统的定量原子模型提供了机会。然而,在与溶液相化学相关的浓度下,总散射信号由大量溶剂主导,这促使研究人员采用差分方法来消除这种不需要的背景。尽管类似的方法在通过小角和广角X射线散射(SAXS / WAXS)对溶液中的大分子进行定量结构研究中已经很成熟,但在实现亚埃空间分辨率的HEXS领域的类似研究仍未充分发展,部分原因是缺乏对该实验的严格理论描述。为了解决这个问题,我们在此开发了一个用于高能差分溶液散射实验的框架,其中包括用于描述SAXS / WAXS数据的溶剂排除体积概念,以及来自时间分辨X射线散射领域的概念。我们的理论得到了数值模拟和实验的支持,为建立定量方法以确定溶液中小分子的原子结构铺平了道路,其分辨率接近晶体学分辨率。