Accurate structure models and absolute configuration determination using dynamical effects in continuous-rotation 3D electron diffraction data.
Accurate structure models and absolute configuration determination using dynamical effects in continuous-rotation 3D electron diffraction data.
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DOI：
10.1038/s41557-023-01186-1
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发表时间：
2023-06
期刊：
影响因子：
21.8
通讯作者：
中科院分区：
文献类型：
--
作者：
连续旋转三维电子衍射法在分析非常小的有机分子晶体和结晶无机材料的结构方面越来越受欢迎。动力学绕射效应导致了结构分析中存在的运动强度的非线性偏差。本文提出了一种考虑多重散射效应的连续旋转三维电子衍射数据的结构分析方法。对12种化合物--从小的有机化合物到金属有机骨架再到无机材料--的动力学和运动学修正进行了比较，新方法在精度和可靠性方面产生了显著改善的模型，差分傅里叶图中的噪声水平最多降低了四倍。用动力学衍射对绝对结构的本征灵敏度对9种不同手性化合物的58个晶体进行了归属，表明三维电子衍射是一种可靠的常规绝对结构测定工具。连续旋转三维电子衍射是从纳米晶体中确定结构的一种强有力的技术。现在已经证明，考虑到动态衍射效应的数据处理方法可以产生更准确的结构模型，对微弱信号更敏感，以及可靠地确定绝对构型--即使对于只包含轻原子的材料也是如此。
Continuous-rotation 3D electron diffraction methods are increasingly popular for the structure analysis of very small organic molecular crystals and crystalline inorganic materials. Dynamical diffraction effects cause non-linear deviations from kinematical intensities that present issues in structure analysis. Here, a method for structure analysis of continuous-rotation 3D electron diffraction data is presented that takes multiple scattering effects into account. Dynamical and kinematical refinements of 12 compounds—ranging from small organic compounds to metal–organic frameworks to inorganic materials—are compared, for which the new approach yields significantly improved models in terms of accuracy and reliability with up to fourfold reduction of the noise level in difference Fourier maps. The intrinsic sensitivity of dynamical diffraction to the absolute structure is also used to assign the handedness of 58 crystals of 9 different chiral compounds, showing that 3D electron diffraction is a reliable tool for the routine determination of absolute structures. Continuous-rotation 3D electron diffraction is a powerful technique to determine structures from nanocrystals. A data treatment method that takes into account dynamical diffraction effects has now been shown to lead to more accurate structure models, better sensitivity to weak signals and a reliable determination of absolute configuration—even for materials containing only light atoms.
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影响因子：
64.8
作者：
Nakane T;Kotecha A;Sente A;McMullan G;Masiulis S;Brown PMGE;Grigoras IT;Malinauskaite L;Malinauskas T;Miehling J;Uchański T;Yu L;Karia D;Pechnikova EV;de Jong E;Keizer J;Bischoff M;McCormack J;Tiemeijer P;Hardwick SW;Chirgadze DY;Murshudov G;Aricescu AR;Scheres SHW
通讯作者：
Scheres SHW
影响因子：
2.2
作者：
Oleynikov, P.;Hovmoller, S.;Zou, X. D.
通讯作者：
Zou, X. D.
DOI：
10.1107/s2053273318013918
发表时间：
2019-01-01
影响因子：
1.8
作者：
Clabbers, Max T. B.;Gruene, Tim;Abrahams, Jan Pieter
通讯作者：
Abrahams, Jan Pieter
影响因子：
3.9
作者：
Broadhurst, Edward T.;Xu, Hongyi;Parsons, Simon
通讯作者：
Parsons, Simon
影响因子：
2.7
作者：
Frojdh, Erik;Wennmacher, Julian T. C.;Gruene, Tim
通讯作者：
Gruene, Tim