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Half-sandwich Ru(II), Ir(III) and Rh(III) complexes with bridging or chelating N-heterocyclic bis-carbene ligand: Synthesis and characterization

机译:带有桥接或螯合N-杂环双卡宾配体的半三明治Ru(II),Ir(III)和Rh(III)配合物:合成与表征

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摘要

N-heterocyclic bis-carbene ligand (bis-NHC) which was derived from 1,1′-diisopropyl-3,3′-ethylenediimidazolium dibromide (L·2HBr) via silver carbene transfer method, reacted with [(η~6-p-cymene)RuCl_2]_2 and [Cp ~1MCl_2]_2 (Cp~1 = η~5- C_5Me_5, M = Ir, Rh) respectively, afforded complexes [(η~6-p-cymene)RuCl_2]_2(L) (1), [Cp ~1IrCl_2]_2(L) (2) and [Cp~1RhCl(L)] [Cp~1RhCl_3] (3). When [Cp~1IrCl_2] _2 was treated with 2 equiv AgOTf at first, and then reacted with bis-NHC ligand, [Cp~1IrCl(L)]OTf (4) was obtained. The molecular structures of complexes 1-4 were determined by X-ray single crystal analysis, showing that 1 and 2 adopted bridging coordination mode, 3 and 4 adopted chelating coordination mode. All of these complexes were characterized by ~1H, ~(13)C NMR spectroscopy and element analysis.
机译:由1,1'-二异丙基-3,3'-亚乙基二咪唑二溴化物(L·2HBr)通过银卡宾银转移法得到的N-杂环双卡宾配体(bis-NHC)与[(η〜6-p -cymene)RuCl_2] _2和[Cp〜1MCl_2] _2(Cp〜1 =η〜5- C_5Me_5,M = Ir,Rh),得到配合物[(η〜6-p-cymene)RuCl_2] _2(L) (1),[Cp〜1IrCl_2] _2(L)(2)和[Cp〜1RhCl(L)] [Cp〜1RhCl_3](3)。首先用2当量的AgOTf处理[Cp〜1IrCl_2] _2,然后与bis-NHC配体反应,得到[Cp〜1IrCl(L)] OTf(4)。通过X射线单晶分析确定配合物1-4的分子结构,表明1和2采用桥联配位模式,3和4采用螯合配位模式。所有这些络合物均通过〜1H,〜(13)C NMR光谱和元素分析表征。

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