Syntheses, Characterization, and X-ray Crystal Structures of -Diketiminate Group 13 Hydrides, Chlorides, and Fluoride
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- 作者：Sanjay Singh ; Hans-Jü ; rgen Ahn ; Andreas Stasch ; Vojtech Jancik ; Herbert W. Roesky ; Aritra Pal ; Mariana Biadene ; Regine Herbst-Irmer ; Mathias Noltemeyer ; and Hans-Georg Schmidt
- 刊名：Inorganic Chemistry
- 出版年：2006
- 出版时间：February 20, 2006
- 年：2006
- 卷：45
- 期：4
- 页码：1853 - 1860
- 全文大小：210K
- 年卷期：v.45,no.4(February 20, 2006)
- ISSN：1520-510X
文摘
A series of organometallic compounds of group 13 metals supported by the sterically encumbered 
-diketiminateligand containing hydrides, fluorides, chlorides, and bromide have been synthesized and structurally characterized.The synthetic strategy applied utilizes halide metathesis and reduction of metal chlorides to the correspondinghydrides. Thus, the reaction of LLi·OEt2 with MeMCl2 affords LM(Me)Cl (M = Al (1), Ga (2), In (3)) and LGaBr2(4) with GaBr3. Reduction of LGa(Me)Cl with LiH·BEt3 leads to the formation of LGa(Me)H (10). Synthesis ofLGaH2 (12) has been accomplished by reacting LGaI2 (8) with LiH·BEt3. LAl(Me)Cl (1) and LAlH2 (6) have beenconverted to LAl(Me)F (5) and LAlF2 (7), respectively. The former was obtained in a reaction of LAl(Me)Cl withMe3SnF while the latter was isolated in a reaction of LAlH2 with BF3·OEt2. Similarly reaction of LGaI2 (8) withMe3SnF affords LGaF2 (9). Compounds reported herein have been characterized by elemental analyses, IR, NMR,EI-MS, and single-crystal X-ray diffraction techniques.
-diketiminateligand containing hydrides, fluorides, chlorides, and bromide have been synthesized and structurally characterized.The synthetic strategy applied utilizes halide metathesis and reduction of metal chlorides to the correspondinghydrides. Thus, the reaction of LLi·OEt2 with MeMCl2 affords LM(Me)Cl (M = Al (1), Ga (2), In (3)) and LGaBr2(4) with GaBr3. Reduction of LGa(Me)Cl with LiH·BEt3 leads to the formation of LGa(Me)H (10). Synthesis ofLGaH2 (12) has been accomplished by reacting LGaI2 (8) with LiH·BEt3. LAl(Me)Cl (1) and LAlH2 (6) have beenconverted to LAl(Me)F (5) and LAlF2 (7), respectively. The former was obtained in a reaction of LAl(Me)Cl withMe3SnF while the latter was isolated in a reaction of LAlH2 with BF3·OEt2. Similarly reaction of LGaI2 (8) withMe3SnF affords LGaF2 (9). Compounds reported herein have been characterized by elemental analyses, IR, NMR,EI-MS, and single-crystal X-ray diffraction techniques.