Side-On Bound Dinitrogen Complex of Zirconium Supported by a P2N2 Macrocyclic Ligand

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• 作者：Lara Morello ; Maria Joã ; o Ferreira ; Brian O. Patrick ; Michael D. Fryzuk
• 刊名：Inorganic Chemistry
• 出版年：2008
• 出版时间：February 18, 2008
• 年：2008
• 卷：47
• 期：4
• 页码：1319 - 1323
• 全文大小：706K
• 年卷期：v.47,no.4(February 18, 2008)
• ISSN：1520-510X

文摘

Reduction of [P₂N₂]ZrCl₂ (where P₂N₂ = PhP(CH₂SiMe₂NSiMe₂CH₂)₂PPh) by KC₈ under N₂ generates the dinuclear dinitrogen complex ([P₂N₂]Zr)₂(μ-η²:η²-N₂) and impurities in varying yields depending on the solvent and temperature. The toluene complex [P₂N₂]Zr(η⁶-C₇H₈) along with a dinuclear species with bridging PC₆H₅ groups is observable. Also observable in the crude reaction mixtures is the μ-oxodiazenido derivative, ([P₂N₂]Zr)₂(μ-η²:η²-N₂H₂)(μ-O), due to reaction with trace H₂O. This paper reports the full details of the preparation of ([P₂N₂]Zr)₂(μ-η²:η²-N₂) including an improved method that involves reduction at low temperatures in a tetrahydrofuran solvent. Also reported is a reproducible synthesis of the oxodiazenido complex along with the X-ray structures of the dinitrogen complex and the oxodiazenido derivative.