Synthesis of the tris-cyclometalated complex fac-[Rh(ptpy)₃] and X-ray crystal structure of [Rh(acac)(ptpy)₂]

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• 作者：Hans-Christian Bö ; ttcher^a ; Marion Graf^a ; Karlheinz S&#xfc ; nkel^a ; ^{karlheinz.suenkel@cup.uni-muenchen.de} ; Beatrice Salert^b ; Hartmut Kr&#xfc ; ger^b
• 关键词：Rhodium complexes ; Cyclometalation ; Crystal structure ; Phosphorescence
• 刊名：Inorganic Chemistry Communications
• 出版年：2011
• 出版时间：February 2011
• 年：2011
• 卷：14
• 期：2
• 页码：377-379
• 全文大小：459 K

文摘

New convenient syntheses of the cyclometalated complexes [Rh(acac)(ptpy)₂] (3, ptpy = 2-(p-tolyl)pyridinato) and fac-[Rh(ptpy)₃] (4) are described. The compounds were prepared in a kind of one-pot synthesis starting from in situ prepared [Rh(acac)(coe)₂] (2) (coe = cis-cyclooctene) followed by reaction with Hptpy in refluxing toluene. Under these conditions oxidative addition occurred and the new complex 3 was obtained in good yields. Compound 4 was prepared in good yields by reaction of 3 with Hptpy in excess. The complex 3 crystallized from dichloromethane/iso-hexane in the space group P − 1 and its molecular structure was confirmed by a single-crystal X-ray diffraction study. The absorption and emission spectra exhibit the new compounds as red-emitting phosphorescent complexes.