Synthesis and Characterization of Chalcogenolato-Bridged Allyl Palladium Complexes: Versatile Precursors for Palladium Chalcogenides
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- 作者：Ninad Ghavale ; Sandip Dey ; Amey Wadawale ; Vimal K. Jain
- 刊名：Organometallics
- 出版年：2008
- 出版时间：July 14, 2008
- 年：2008
- 卷：27
- 期：13
- 页码：3297 - 3302
- 全文大小：171K
- 年卷期：v.27,no.13(July 14, 2008)
- ISSN：1520-6041
文摘
The complexes [Pd(μ-ER)(η3-allyl)]2 (ER = EMes; E = S, Se; allyl = C3H5, C4H7) have been isolated by the reaction of [Pb(ER)2]n with [Pd2(μ-Cl)2(η3-allyl)2]. Similar reactions with [Pb(SeCH2CH2NMe2)2]n resulted in the formation of a trinuclear complex [Pd3Cl2(κ2-Se,N-SeCH2CH2NMe2)(η3-allyl)3]. Treatment of [Pd(μ-SR)(η3-C4H7)]2 with [Pd(SMes)2]n in 1:1 ratio yielded [Pd3(μ-SMes)4(η3-C4H7)2]. These complexes were characterized by elemental analyses and mass, UV−vis, and NMR spectroscopy. The structures of [Pd2(μ-EMes)2(η3-C4H7)2] (E = S, Se) were established by single-crystal X-ray diffraction analysis, which revealed a syn configuration. Two new structural motifs for [Pd3Cl2(κ2-Se,N-SeCH2CH2NMe2)(η3-C3H5)3] and [Pd3(μ-SMes)4(η3-C4H7)2] have also been identified. Pyrolysis of [Pd(μ-ER)(η3-C4H7)]2 yielded palladium chalcogenides, which were characterized by powder XRD and EDAX.