Synthesis of Oxalate Peroxo-uranyl Complex in situ by Photoreaction

doi:10.13209/j.0479-8023.2020.016

Acta Scientiarum Naturalium Universitatis Pekinensis ›› 2020, Vol. 56 ›› Issue (3): 399-405.DOI: 10.13209/j.0479-8023.2020.016

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Synthesis of Oxalate Peroxo-uranyl Complex in situ by Photoreaction

WEI Wenqi, LIU Chunli^†

Beijing National Laboratory for Molecular Sciences, Fundamental Science Laboratory on Radiochemistry and Radiation Chemistry, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871

Received:2019-03-15 Revised:2019-06-06 Online:2020-05-20 Published:2020-05-20
Contact: LIU Chunli, E-mail: liucl(at)pku.edu.cn

原位光反应法合成过氧桥连草酸铀酰配合物

魏文琦, 刘春立^†

北京分子科学国家研究中心, 放射化学与辐射化学重点学科实验室, 北京大学化学与分子工程学院, 北京 100871

通讯作者: 刘春立, E-mail: liucl(at)pku.edu.cn
基金资助:
国家自然科学基金(11475008, U1530112, U1730245)资助

Abstract

Abstract:

[NH₃(CH₂)₂NH₃]₃[(UO₂)₂O₂(C₂O₄)₄]·4H₂O (1), [NH₃(CH₂)₂NH₂(CH₂)₂NH₃]₂[(UO₂)₂O₂(C₂O₄)₄]·2H₂O (2) and [NH₃(CH₂)₂NH₂(CH₂)₂NH₃]₂[(UO₂)₂O₂(C₂O₄)₄] (3) were synthesized in situ under room temperature and laboratory lamp condition, using 1,2-diaminoethane and 2,2'-diaminodiethylamine separately as templates. Structures and properties were characterized by single-crystal X-ray diffraction, Raman spectra, powder X-ray diffraction (PXRD) and thermogravimetric analysis (TGA). The dihedral angle of U-O₂-U in 1 and 2 is 180°, which deviates from the natural angle of peroxide. The peroxide bond length of 2 and 3 is shorter than that of the reported peroxide, and the bond lenth of 2 is close to superoxide bond length. However, both valence and Raman spectra indicated that 2 and 3 are peroxide bonds.

Key words: uranyl complex, peroxide, in situ, photoreaction, oxalic acid

摘要：

在室温和实验室灯光照射条件下, 通过原位光化学反应, 分别以乙二胺和二亚乙基三胺为模板, 合成3种过氧桥连的草酸铀酰配合物[NH₃(CH₂)₂NH₃]₃[(UO₂)₂O₂(C₂O₄)₄]·4H₂O (1), [NH₃(CH₂)₂NH₂(CH₂)₂NH₃]₂[(UO₂)₂O₂(C₂O₄)₄]·2H₂O (2)和[NH₃(CH₂)₂NH₂(CH₂)₂NH₃]₂[(UO₂)₂O₂(C₂O₄)₄] (3)。借助单晶X射线衍射、拉曼光谱(Raman)、粉末X射线衍射(PXRD)和热重分析(TGA), 对配合物的结构及其性质进行表征和分析。1和2中U-O₂-U二面角为180°, 而通常过氧配合物的过氧二面角小于180°。2和3中过氧键的键长比正常的过氧键长短, 其中2更接近超氧键的键长, 但价态和拉曼图谱都表明其为过氧键。

关键词: 铀酰配合物, 过氧, 原位, 光反应, 草酸

WEI Wenqi, LIU Chunli. Synthesis of Oxalate Peroxo-uranyl Complex in situ by Photoreaction[J]. Acta Scientiarum Naturalium Universitatis Pekinensis, 2020, 56(3): 399-405.

魏文琦, 刘春立. 原位光反应法合成过氧桥连草酸铀酰配合物[J]. 北京大学学报自然科学版, 2020, 56(3): 399-405.

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Synthesis of Oxalate Peroxo-uranyl Complex in situ by Photoreaction

原位光反应法合成过氧桥连草酸铀酰配合物

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