Compound 4

potassium (µ-dinitrido(4-))(µ-oxo)bis[(tris-tert-butoxysiloxouranium(V)]

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)(μ-N2)}]

Compound data: 1H NMR

Compound data: Crystallographic data

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

A dark red solution of complex [K2{[U(OSi(OtBu)3)3]2(μ-O)}], 3 (31.7 mg, 0.015 mmol) in toluene (0.5 mL) was prepared in a Schlenk tube in the glove box under argon. The tube was transferred to the Schlenk line and was degassed by freeze-pump-thawing three times. N2 (1 atm) was added to the solution at room temperature. The solution turned immediately dark brown. 1H NMR shows immediate complete conversion to complex 4. The toluene solution was left standing at -40 °C for 24 h yielding to X-ray suitable crystals of complex [K2{[U(OSi(OtBu)3)3]2(μ-O)(μ-N2)}], 4 (22 mg, 69% yield). The 15N labeled complex 15N-4 was prepared with the same procedure from 15N2. 1H NMR of 4 (400 MHz, tol-d8, 298 K): δ(ppm) = -1.88 (s, CH3 terminal siloxide). Anal. Calcd for 4(toluene)2 C72H162N2O25K2Si6U2(C7H8)2: C, 43.71; H, 7.59; N, 1.19. Found: C, 43.62; H, 7.45; N, 1.10. Magnetic moment at room temperature 1.752 µB.

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