Compound 2

tris(di-isopropylphosphinoamidoethyl)amine uranium(IV) chloride

From: Transition-metal-bridged bimetallic clusters with multiple uranium–metal bonds

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Synonyms:
  • [N(CH2CH2NPiPr2)3]UCl

Compound data: 1H NMR

Compound data: 13C NMR

Compound data: 31P NMR

Compound data: UV-Vis

Compound data: Crystallographic data

Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.

A solution of UCl4 (379.8 mg, 1.0 mmol) in THF (10 mL) was added to a pre-cooled solution of N[CH2CH2NLiPiPr2]3 (656.7 mg, 1.0 mmol) in THF (10 mL) at –30 °C. The color of the mixture changed into brown. The mixture was allowed to warm to room temperature and stirred overnight. After removing the solvent in vacuo, the product was extracted with toluene and filtered yielding a brown solution. The filtrate was stored at –30 °C and yielded complex 2 as brown crystals. Yield: 450 mg, 59%. Anal. Calcd (%) for C24H54ClN4P3U: C, 37.68; H, 7.11; N, 7.32. Found: C, 35.35; H, 6.66; N, 7.28. This complex consistently has low carbon content, possibly due to incomplete combustion or the high sensitivity of the compound. 1H NMR (400 MHz, ppm): δ 28.37 (s, 6H), 27.15 (s, 6H), -2.68 (s, 6H), -5.82 (s, 18H), -7.88 (s, 18H). 13C NMR (101 MHz, C6D6, ppm): δ 49.70, 13.63, -2.85, -3.44, -51.05. 31P NMR (162 MHz, C6D6, ppm): δ 739.71.