摘要
配体PyCH_2COPh与Ru_3(CO)_(12)在甲苯中加热回流,得到了标题簇合物[PyCH=C(Ph)O]2Ru3(CO)8(1)。通过红外光谱、核磁共振氢谱和碳谱对1的结构进行了表征,用X射线单晶衍射法测定了1的结构。结果表明:3个钌原子呈等腰三角形分布,其中Ru(2)-Ru(1)和Ru(2)-Ru(1)i的键长均为0.280 nm,Ru(1)-Ru(1)i的键长为0.307 nm。同时研究了簇合物1与环戊二烯及茚的反应,分别得到双核钌羰基配合物[(η~5-C_5H_5)Ru(CO)]_2(μ-CO)_2(2)和[(η~5-C_9H_7)Ru(CO)]2(μ-CO)_2(3)。
The title compound, [PyCH=C(Ph)O]_2Ru_3(CO)8(1), was obtained from the reaction of PyCH_2COPh with Ru_3(CO)12in refluxing toluene. Compound 1 was characterized by IR,1H NMR, and13 C NMR spectroscopy as well as by single-crystal X-ray diffraction analysis. X-ray study of the cluster compound 1 shows that the three ruthenium atoms define an isosceles triangle with two distances of 0.280 nm and one of 0.307 nm. When 1 was treated with cyclopentadiene in refluxing toluene, dinuclear metal carbonyl complexes [(η~5-C_5H_5)Ru(CO)]_2( μ-CO)2(2) was obtained. Similar treatment of 1 with indene gave the product [(η5-C9H7)Ru(CO)]_2(μ-CO)_2(3).
引文
[1]Kaim L W,Schwederski B.Bioinorganic Chemistry:Inorganic Elements in the Chemistry of Life.New York:Wiley,1996.
[2]Luo X F,Hu X,Zhao X Y,et al.Polymer,2003,44:5285-5291
[3]Murthy A S N,Reddy A R.J.Chem.Sci.,1981,90:519-526
[4]Ackermann M N,Kiihne S R,Saunders P A,et al.Inorg.Chim.Acta,2002,334:193-203
[5]Royer R E,Deck L M,Vander Jagt T J,et al.J.Med.Chem.,1995,38:2427-2432
[6]Baumgrass R,Weiwad M,Erdmann F,et al.J.Biol.Chem.,2001,276:47914-47921
[7]Brintzinger H,Bercaw J E.J.Am.Chem.Soc.,1971,93:2045-2046
[8]Hay R W,Basak A K.J.Chem.Soc.Dalton Trans.,1982,1819-1823
[9]Bruce M I,Iqbal M Z,Stone F G A.J.Organometal.Chem.,1971,31:275-281
[10]Santini C C,Basset J M,Fontal B,et al.J.Chem.Soc.,Chem.Commun.,1987,7:512-513
[11]Wang Y,Zhao W,Liu D T,et al.Organometallics,2012,31:4182-4190
[12]Koning B,Buter J,Hulst R,et al.Eur.J.Org.Chem.,2000,2735-2743
[13]Sheldrick G M.SHELXL-97,Program for Crystal Structure Renement,University of G觟ttingen,Germany,1997.
[14]van Doorn J A,van Leeuwen P W N M.J.Organomet.Chem.,1981,222:299-309
[15]Mills O S,Nice N P.J.Organomet.Chem.,1967,9:339-344
[16]Sridevi V S,Leong W K.J.Organomet.Chem.,2007,692:4909-4916