Synthesis and Characterization of Group 11 1,1,3,3-Tetraalkylguanidinate (TAG) Clusters: [M2(μ-TAG){μ-N(SiMe3)2}]2 (M = Cu, Ag, and Au)

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• 作者：Scott D. Bunge* ; Jennifer L. Steele
• 刊名：Inorganic Chemistry
• 出版年：2009
• 出版时间：March 16, 2009
• 年：2009
• 卷：48
• 期：6
• 页码：2701-2706
• 全文大小：201K
• 年卷期：v.48,no.6(March 16, 2009)
• ISSN：1520-510X

文摘

The addition of diethylcyanamide to a tetrahydrofuran solution of lithium dialkylamide {LiN(CH₃)₂ or LiNCH₂CH₂CH₂CH₂, Li(PYR)} results in the corresponding lithium 1,1,3,3-tetraalkylguanidinate, Li(TAG). Two equivalents of Li(TAG) and 2 equiv of lithium bistrimethylsilylamide, LiN(SiMe₃)₂, were subsequently reacted with 4 equiv of Group 11 halide (CuCl, AgBr, and AuCl) to generate tetranuclear complexes with the general formula [M₂(μ-TAG){μ-N(SiMe₃)₂}]₂ where M and TAG = {Cu, DEDMG, (1)}, {Ag, DEDMG, (2)}, {Au, DEDMG, (3)}, {Cu, DEPYRG, (4)}, {Ag, DEPYRG, (5)}, and {Au, DEPYRG, (6)}. Compounds 1−6 were characterized by single-crystal X-ray diffraction. The bulk powders for all complexes were found to be in agreement with the crystal structures based on elemental analyses, FT-IR spectroscopy, ¹H and ¹³C NMR studies.