Compound 6

potassium bis(µ-oxo)-bis[tris-tert-butoxysiloxouranium(IV)]

From: The role of bridging ligands in dinitrogen reduction and functionalization by uranium multimetallic complexes

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Synonyms:
  • [K2{[U(OSi(OtBu)3)3]2(μ-O)2}]

Compound data: 1H NMR

Compound data: Crystallographic data

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

Excess KC8 (27.5 mg, 0.203 mmol, 5 eq) was added to a cold solution (-80°C) of [{U(OSi(OtBu)3)3}2(μ-O)], 2 (84.2 mg, 0.041 mmol, 1 eq) in THF (3 mL). The suspension was stirred at -80°C for 15 minutes. The reaction mixture was then filtered on cooled glassware in order to remove graphite and unreacted KC8. The solid was washed with cold THF. The resulting dark red solution was concentrated to 3 mL and connected to a Schlenk line. The solution was degassed by freeze-pump-thawing and 1 equivalent of N2O was added. The color turned immediately green. The solution was then brought to dryness and the resulting solid was dissolved in 1.5 mL of toluene. The solution was left standing at -40°C overnight affording the formation of [K2{[U(OSi(OtBu)3)3]2(μ-O)2}] as a green crystalline solid (51.1 mg, 58% yield). 1H NMR of 6 (400 MHz, tol-d8, 298 K): δ(ppm) = -1.38 (s, CH3 terminal siloxide) Anal. Calcd for 6(toluene)1.7 C72H162O26K2Si6U2(C7H8)1.7: C, 43.37; H, 7.62; N, 0.00. Found: C, 43.13; H, 8.04; N, 0.00.

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