- Preparation and characterization of an (iodobutoxy)uranium complex
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During the reaction of a uranium pellet with freshly sublimed elemental iodine in THF, ring opening of the THF was observed and a U(IV) species was obtained.Further reaction of the solution with Na in THF at room temperature gave, after recrystallization, a green crystalline solid 2 formulated as > on the basis of various analyses.This complex has also been prepared by reaction of UI4 in THF with the potassium salt of the polypyrazolylborate.The mechanism of the ring-opening of THF is discussed.
- Collin, Jacqueline,Matos, Antonio Pires de,Santos, Isabel
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- Facile Syntheses of pure Uranium(III) Halides: UF3, UCl3, UBr3, and UI3
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Herein we describe a convenient lab scale synthesis for pure and solvent-free binary uranium(III) halides UCl3, UBr3, and UI3. This is achieved by the reduction of the respective uranium(IV) halides with elemental silicon in borosilicate ampoules at moderate temperature. The silicon tetrahalides SiX4 formed as a side product are utilized for the removal of excess starting material via a chemical vapor transport reaction. The syntheses introduced herein avoid the need for pure metallic uranium and are based on uranium(IV) halides synthesized from UO2 and the respective aluminum halides and purified by chemical vapor transport. These uranium(III) halides are obtained in single crystalline form. A similar reaction yields UF3 as a microcrystalline powder. However, no beneficial transport reaction occurs with this halide. Also, a higher temperature has to be applied and steel ampoules have to be used. The identities and purity of the products were checked by powder X-ray diffraction as well as IR spectroscopy. The synthesis of UI3 enabled its crystal structure determination on single crystals for the first time. UI3 crystallizes in the PuBr3 structure type with space group type Cmcm and a = 4.3208(9), b = 13.923(3), c = 9.923(2) ?, V = 596.9(2) ?3, and Z = 4 at T = 100 K.
- Rudel, Stefan S.,Deubner, H. Lars,Scheibe, Benjamin,Conrad, Matthias,Kraus, Florian
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p. 323 - 329
(2018/04/05)
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