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首页> 美国卫生研究院文献>Scientific Reports >In-situ X-ray diffraction snapshotting: Determination of the kinetics of a photodimerization within a single crystal
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In-situ X-ray diffraction snapshotting: Determination of the kinetics of a photodimerization within a single crystal

机译：原位X射线衍射快照：单晶内光二聚化动力学的测定

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摘要

In a single-crystal-to-single-crystal (SCSC) transformation, a preformed three-dimensional coordination polymer,[Ni3(oba)2(bpe)2(SO4)(H2O)4]·H2O (H2oba = 4,4′-oxydibenzoic acid; bpe = (E)-1,2-di(pyridin-4-yl)ethane) (1), was shown to undergo a [2+2] cycloaddition reaction upon exposure to UV irradiation. The kinetics of this reaction were followed by taking “snapshots” of the solid state transformation using in situ single crystal X-ray crystallography; a first order process was indicated. The reaction rate was influenced by many factors such as the separation of the sample from the UV light source, the heat produced by the UV irradiation, the light flux of the UV lamp used, the size of the single-crystal and the powder samples. The investigation of the kinetics was complemented by 1H NMR studies. The results clearly demonstrate that in situ single-crystal X-ray diffraction is able to provide useful insights into the gradual formation of the photoproducts and the reaction processes. The work also offers a clear indication that it is possible to use the technique to study the kinetics of other photocycloaddition reactions and SCSC processes in general.
机译：在单晶至单晶（SCSC）转换中，预制的三维配位聚合物[Ni3（oba）2（bpe）2（SO4）（H2O）4]·H2O（H2oba = 4,4 ′-氧二苯甲酸； bpe =（E）-1,2-二（吡啶-4-基）乙烷）（1），经暴露于紫外线照射后，发生[2 + 2]环加成反应。通过原位单晶X射线晶体学拍摄固态转变的快照，跟踪该反应的动力学。指示了一级处理。反应速率受许多因素的影响，例如样品与紫外光源的分离，紫外辐射产生的热量，所用紫外灯的光通量，单晶和粉末样品的尺寸。动力学研究辅以 1 H NMR研究。结果清楚地表明，原位单晶X射线衍射能够为光产物的逐步形成和反应过程提供有用的见解。这项工作还清楚地表明，有可能使用该技术来研究一般而言其他光环加成反应和SCSC过程的动力学。

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