Synthesis of the tris-cyclometalated complex fac-[Rh(ptpy)3] and X-ray crystal structure of [Rh(acac)(ptpy)2]
Synthesis of the tris-cyclometalated complex fac-[Rh(ptpy)3] and X-ray crystal structure of [Rh(acac)(ptpy)2]
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DOI：
10.1016/j.inoche.2010.12.005
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发表时间：
2011-02-01
影响因子：
3.8
通讯作者：
Krueger, Hartmut
中科院分区：
文献类型：
--
作者：
Boettcher, Hans-Christian;Graf, Marion;Krueger, Hartmut
报道了环金属配合物[Rh(Acac)(Ptpy)(2)](3，ptpy=2-(对甲苯基)吡啶)和fac-[Rh(Ptpy)(3)](4)的新的简便合成方法。以原位合成的[Rh(Acac)(CoE)(2)](2)(CoE=顺式环辛烯)为原料，与Hptpy在甲苯中回流反应，一锅法合成了这些化合物。在此条件下发生氧化加成反应，以较高的产率得到了新的络合物3。通过3与过量的Hptpy反应，以较高的产率合成了化合物4。配合物3由二氯甲烷/异正己烷在P-1空间群结晶而成，其分子结构经单晶X-射线衍射法确证。吸收光谱和发射光谱表明新化合物为红色磷光配合物。(C)2010爱思唯尔B.V.保留所有权利。
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. (C) 2010 Elsevier B.V. All rights reserved.