单晶的45Sc-NMR定量四极性相互作用

IF 1.8 3区 化学 Q4 CHEMISTRY, PHYSICAL Solid state nuclear magnetic resonance Pub Date : 2022-02-01 DOI:10.1016/j.ssnmr.2022.101775
Otto E.O. Zeman, Thomas Bräuniger
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引用次数: 0

摘要

采用45Sc-NMR对化合物[{Sc(H2O)5(μ-OH)}2]Cl4·2H2O的单晶进行了研究,并在微扰理论的层次框架下分析了四极耦合相互作用对自旋7/2核谱的影响。Orientation-dependent光谱获得B0 = 17.6  T显示强劲的二阶效应由于较大耦合常数的χ =  | 14.613±0.006 |兆赫,有一个关联的不对称参数Q η= 0.540 9 ±0.000 4。通过分析±3/2卫星在良好近似下只受一阶效应影响的分裂,可以确定完整的四极耦合张量。这个张量引起的二阶效应根据所有方向的理论预测计算,并从卫星的重心和中心过渡中减去。这允许提取完整的化学位移张量,特征值为δ11 =(5.6 ± 0.9)ppm, δ22 =(12.4 ± 0.9)ppm, δ33 =(38.5 ± 0.9)ppm。在较低磁场B0 = 9.4 T下获得的光谱中,可以检测到三阶效应,并使用解析表达式进行类似的量化。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

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Quantifying the quadrupolar interaction by 45Sc-NMR spectroscopy of single crystals

Single crystals of the compound [{Sc(H2O)5(μ-OH)}2]Cl4 ⋅ 2H2O were studied by 45Sc-NMR, with the effect of the quadrupolar coupling interaction on the spectra of the spin-7/2 nucleus analysed in the hierarchical framework of perturbation theory. Orientation-dependent spectra acquired at B0 = 17.6 T showed strong second-order effects due to the comparatively large coupling constant of χ = |14.613 ± 0.006| MHz, with an associated asymmetry parameter of ηQ = 0.540 9 ± 0.000 4. By analysing the splittings of the ±3/2 satellites, which in good approximation are subjected to first-order effects only, the full quadrupolar coupling tensor could be determined. The second-order effects caused by this tensor were calculated according to theoretical predictions for all orientations, and subtracted from both the centres of gravity of the satellites, and the central transitions. This allowed extraction of the full chemical shift tensor, with the eigenvalues being δ11 = (5.6 ± 0.9) ppm, δ22 = (12.4 ± 0.9) ppm, and δ33 = (38.5 ± 0.9) ppm. In spectra acquired at a lower magnetic field of B0 = 9.4 T, third-order effects could be detected, and similarly quantified using analytical expressions.

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来源期刊
CiteScore
5.30
自引率
9.40%
发文量
42
审稿时长
72 days
期刊介绍: The journal Solid State Nuclear Magnetic Resonance publishes original manuscripts of high scientific quality dealing with all experimental and theoretical aspects of solid state NMR. This includes advances in instrumentation, development of new experimental techniques and methodology, new theoretical insights, new data processing and simulation methods, and original applications of established or novel methods to scientific problems.
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