期刊
INORGANIC CHEMISTRY
卷 57, 期 11, 页码 6571-6583出版社
AMER CHEMICAL SOC
DOI: 10.1021/acs.inorgchem.8b00715
关键词
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资金
- EPSRC [EP/M027015/1, EP/P001386/1, EP/G004846/1, EP/K039547/1]
- ERC [CoG612724]
- Royal Society [UF110005]
- Leverhulme Trust [RL-2012-072]
- University of Manchester
- EPSRC [EP/P001386/1, EP/K039547/1, EP/M027015/1, EP/G004846/1] Funding Source: UKRI
We report the preparation of a range of alkali metal uranyl(VI) tri-bis(silyl)amide complexes [{M(THF)(x)}{(mu-O)U(O)(N)(3)}] (1M) (N = {N(SiMe3)(2)}(-), M = Li, Na, x = 2; M = K, x = 3; M = K, Rb, Cs, x = 0) containing electrostatic alkali metal uranyl-oxo interactions. Reaction of 1M with 2,2,2-cryptand or 2 equiv of the appropriate crown ether resulted in the isolation of the separated ion pair species [U(O)(2)(N)(3)][M(2,2,2-cryptand)] (3M, M = Li-Cs) and [U(O)(2)(N)(3)][M(crown)(2)] (4M, M = Li, crown = 12-crown-4 ether; M = Na Cs, crown = 15-crown-5 ether). A combination of crystallographic studies and IR, Raman and UV-vis spectroscopies has revealed that the 1M series adopts contact ion pair motifs in the solid state where the alkali metal caps one of the uranyl-oxo groups. Upon dissolution in THF solution, this contact is lost, and instead, separated ion pair motifs are observed, which is confirmed by the isolation of [U(O)(2)(N)(3)][M(THF),] (2M) (M = Li, n = 4; M = Na, K, n = 6). The compounds have been characterized by single crystal X-ray diffraction, multinuclear NMR spectroscopy, IR, Raman, and UV-vis spectroscopies, and elemental analyses.
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