Synthesis and Characterization of Stable Ruthenabenzenes Starting from HCCCH(OH)C
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- 作者：Hong Zhang ; Li Feng ; Lei Gong ; Liqiong Wu ; Guomei He ; Tingbin Wen ; Fangzu Yang ; Haiping Xia
- 刊名：Organometallics
- 出版年：2007
- 出版时间：May 7, 2007
- 年：2007
- 卷：26
- 期：10
- 页码：2705 - 2713
- 全文大小：217K
- 年卷期：v.26,no.10(May 7, 2007)
- ISSN：1520-6041
文摘
Treatment of RuCl2(PPh3)3 with HC
CCH(OH)CCH/PPh3 at room temperature produces the air-stable ruthenabenzene [Ru(CHC(PPh3)CHC(PPh3)CH)Cl2(PPh3)2]Cl (2) in good yield. The ruthenabenzene2 can even be obtained from the one-pot reaction of RuCl3, PPh3, and HCCCH(OH)CCH in themixed solvent of ionic liquid and CH2Cl2 in higher yield. The ruthenabenzene 2 reacts with PMe3, PBu3,tert-butyl isocyanide, 2,2'-dipyridyl (bipy), and 2,2'-dipyridyl/PMe3 to give new stable ruthenabenzenes[Ru(CHC(PPh3)CHC(PPh3)CH)Cl2(PMe3)2]Cl (4), [Ru(CHC(PPh3)CHC(PPh3)CH)Cl2(PBu3)2]Cl (5), [Ru(CHC(PPh3)CHC(PPh3)CH)Cl(tBuNC)(PPh3)2]Cl2 (6), [Ru(CHC(PPh3)CHC(PPh3)CH)Cl(bipy)(PPh3)]Cl2(7), and [Ru(CHC(PPh3)CHC(PPh3)CH)(bipy)(PMe3)2]Cl3 (8), respectively. Reaction of ruthenabenzene2 with AgBF4 gives bisruthenabenzene [Ru(CHC(PPh3)CHC(PPh3)CH)(PPh3)]2(
-Cl)3(BF4)3 (9). Thethermal decomposition reactions of ruthenabenzene 2 and 7 produce a stable Cp- ion derivative, [CHC(PPh3)CHC(PPh3)CH]Cl (10). 2, 4, 7, 8, 9, and 10 have been structurally characterized. 9 is the firstnon-metal-coordinated bismetallabenzene. An electrochemical study shows that the metal centers in thebisruthenabenzene 9 slightly interact with each other through the chloro bridges.
CCH(OH)CCH/PPh3 at room temperature produces the air-stable ruthenabenzene [Ru(CHC(PPh3)CHC(PPh3)CH)Cl2(PPh3)2]Cl (2) in good yield. The ruthenabenzene2 can even be obtained from the one-pot reaction of RuCl3, PPh3, and HCCCH(OH)CCH in themixed solvent of ionic liquid and CH2Cl2 in higher yield. The ruthenabenzene 2 reacts with PMe3, PBu3,tert-butyl isocyanide, 2,2'-dipyridyl (bipy), and 2,2'-dipyridyl/PMe3 to give new stable ruthenabenzenes[Ru(CHC(PPh3)CHC(PPh3)CH)Cl2(PMe3)2]Cl (4), [Ru(CHC(PPh3)CHC(PPh3)CH)Cl2(PBu3)2]Cl (5), [Ru(CHC(PPh3)CHC(PPh3)CH)Cl(tBuNC)(PPh3)2]Cl2 (6), [Ru(CHC(PPh3)CHC(PPh3)CH)Cl(bipy)(PPh3)]Cl2(7), and [Ru(CHC(PPh3)CHC(PPh3)CH)(bipy)(PMe3)2]Cl3 (8), respectively. Reaction of ruthenabenzene2 with AgBF4 gives bisruthenabenzene [Ru(CHC(PPh3)CHC(PPh3)CH)(PPh3)]2(-Cl)3(BF4)3 (9). Thethermal decomposition reactions of ruthenabenzene 2 and 7 produce a stable Cp- ion derivative, [CHC(PPh3)CHC(PPh3)CH]Cl (10). 2, 4, 7, 8, 9, and 10 have been structurally characterized. 9 is the firstnon-metal-coordinated bismetallabenzene. An electrochemical study shows that the metal centers in thebisruthenabenzene 9 slightly interact with each other through the chloro bridges.