Formation and Chemistry of the Homologous Series of Nitrido Clusters: [Ru4N(CO)12]-, [Ru5N(CO)14]-, and [Ru6N(CO)16]-

Margaret L. Blohm; Wayne L. Gladfelter

doi:10.1021/om00120a009

Formation and Chemistry of the Homologous Series of Nitrido Clusters: [Ru₄N(CO)₁₂]^-, [Ru₅N(CO)₁₄]^-, and [Ru₆N(CO)₁₆]^-

Margaret L. Blohm, Wayne L. Gladfelter

Chemistry (Twin Cities)

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Abstract

The reaction of coordinated isocyanate ligands to give new nitrido clusters is explored. The thermolysis of [ru₄(NCO)(CO)₁₃]^-gives [Ru₄N(CO)₁₂]^-in 78% recrystallized yield after 24 h. When the trinuclear isocyanate clusters [Ru₃(NCO)(CO)₁₀]^-and [Ru3(NCO)(CO)_u]^-are heated with 1 equiv of Ru₃(CO)₁₂, the hexanuclear nitrido cluster [Ru₆N(CO)₁₆]^-can be isolated in 82% yield. [Ru_€N(CO)₁₆]^-reacts rapidly with CO at room temperature to give [Ru5N(CO)₁₄]^-in quantitative yield. A single-crystal X-ray crystallographic study of (PhCH₂Et₃N)[Ru₅N(CO)₁₄] [P1 space group, a = 12.123 (6) Å, b = 14.263 (5) Å, c = 10.642 (3) Å, a = 104.74 (3)°, β = 93.28 (3)°, γ = 80.25 (4)°, Z = 2] revealed a square-based pyramid of metal atoms with the nitrogen positioned slightly below the square face. Other interconversions among the nitrido clusters are also discussed. At high CO pressure, the isocyanate ligand can be reformed from the nitrido clusters.

Original language	English (US)
Pages (from-to)	45-52
Number of pages	8
Journal	Organometallics
Volume	4
Issue number	1
DOIs	https://doi.org/10.1021/om00120a009
State	Published - Feb 21 1985

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title = "Formation and Chemistry of the Homologous Series of Nitrido Clusters: [Ru4N(CO)12]-, [Ru5N(CO)14]-, and [Ru6N(CO)16]-",

abstract = "The reaction of coordinated isocyanate ligands to give new nitrido clusters is explored. The thermolysis of [ru4(NCO)(CO)13]-gives [Ru4N(CO)12]-in 78% recrystallized yield after 24 h. When the trinuclear isocyanate clusters [Ru3(NCO)(CO)10]-and [Ru3(NCO)(CO)u]-are heated with 1 equiv of Ru3(CO)12, the hexanuclear nitrido cluster [Ru6N(CO)16]-can be isolated in 82% yield. [Ru€N(CO)16]-reacts rapidly with CO at room temperature to give [Ru5N(CO)14]-in quantitative yield. A single-crystal X-ray crystallographic study of (PhCH2Et3N)[Ru5N(CO)14] [P1 space group, a = 12.123 (6) {\AA}, b = 14.263 (5) {\AA}, c = 10.642 (3) {\AA}, a = 104.74 (3)°, β = 93.28 (3)°, γ = 80.25 (4)°, Z = 2] revealed a square-based pyramid of metal atoms with the nitrogen positioned slightly below the square face. Other interconversions among the nitrido clusters are also discussed. At high CO pressure, the isocyanate ligand can be reformed from the nitrido clusters.",

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AU - Gladfelter, Wayne L.

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N2 - The reaction of coordinated isocyanate ligands to give new nitrido clusters is explored. The thermolysis of [ru4(NCO)(CO)13]-gives [Ru4N(CO)12]-in 78% recrystallized yield after 24 h. When the trinuclear isocyanate clusters [Ru3(NCO)(CO)10]-and [Ru3(NCO)(CO)u]-are heated with 1 equiv of Ru3(CO)12, the hexanuclear nitrido cluster [Ru6N(CO)16]-can be isolated in 82% yield. [Ru€N(CO)16]-reacts rapidly with CO at room temperature to give [Ru5N(CO)14]-in quantitative yield. A single-crystal X-ray crystallographic study of (PhCH2Et3N)[Ru5N(CO)14] [P1 space group, a = 12.123 (6) Å, b = 14.263 (5) Å, c = 10.642 (3) Å, a = 104.74 (3)°, β = 93.28 (3)°, γ = 80.25 (4)°, Z = 2] revealed a square-based pyramid of metal atoms with the nitrogen positioned slightly below the square face. Other interconversions among the nitrido clusters are also discussed. At high CO pressure, the isocyanate ligand can be reformed from the nitrido clusters.

AB - The reaction of coordinated isocyanate ligands to give new nitrido clusters is explored. The thermolysis of [ru4(NCO)(CO)13]-gives [Ru4N(CO)12]-in 78% recrystallized yield after 24 h. When the trinuclear isocyanate clusters [Ru3(NCO)(CO)10]-and [Ru3(NCO)(CO)u]-are heated with 1 equiv of Ru3(CO)12, the hexanuclear nitrido cluster [Ru6N(CO)16]-can be isolated in 82% yield. [Ru€N(CO)16]-reacts rapidly with CO at room temperature to give [Ru5N(CO)14]-in quantitative yield. A single-crystal X-ray crystallographic study of (PhCH2Et3N)[Ru5N(CO)14] [P1 space group, a = 12.123 (6) Å, b = 14.263 (5) Å, c = 10.642 (3) Å, a = 104.74 (3)°, β = 93.28 (3)°, γ = 80.25 (4)°, Z = 2] revealed a square-based pyramid of metal atoms with the nitrogen positioned slightly below the square face. Other interconversions among the nitrido clusters are also discussed. At high CO pressure, the isocyanate ligand can be reformed from the nitrido clusters.

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Formation and Chemistry of the Homologous Series of Nitrido Clusters: [Ru₄N(CO)₁₂]^-, [Ru₅N(CO)₁₄]^-, and [Ru₆N(CO)₁₆]^-

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