Singh Sanjay, Ahn Hans-Jürgen, Stasch Andreas, Jancik Vojtech, Roesky Herbert W, Pal Aritra, Biadene Mariana, Herbst-Irmer Regine, Noltemeyer Mathias, Schmidt Hans-Georg
Institut für Anorganische Chemie der Georg-August-Universität Göttingen, Germany.
Inorg Chem. 2006 Feb 20;45(4):1853-60. doi: 10.1021/ic0517826.
A series of organometallic compounds of group 13 metals supported by the sterically encumbered beta-diketiminate ligand 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 corresponding hydrides. 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 of LGaH(2) (12) has been accomplished by reacting LGaI2 (8) with LiH.BEt3. LAl(Me)Cl (1) and LAlH2 (6) have been converted to LAl(Me)F (5) and LAlF2 (7), respectively. The former was obtained in a reaction of LAl(Me)Cl with Me3SnF while the latter was isolated in a reaction of LAlH2 with BF3.OEt2. Similarly reaction of LGaI2 (8) with Me3SnF affords LGaF2 (9). Compounds reported herein have been characterized by elemental analyses, IR, NMR, EI-MS, and single-crystal X-ray diffraction techniques.
一系列由空间位阻较大的含氢化物、氟化物、氯化物和溴化物的β-二酮亚胺配体支撑的第13族金属有机金属化合物已被合成并进行了结构表征。所采用的合成策略利用卤化物复分解反应以及将金属氯化物还原为相应的氢化物。因此，LLi·OEt₂与MeMCl₂反应生成LM(Me)Cl（M = Al (1)、Ga (2)、In (3)）以及LGaBr₂ (4)与GaBr₃反应。用LiH·BEt₃还原LGa(Me)Cl导致形成LGa(Me)H (10)。通过使LGaI₂ (8)与LiH·BEt₃反应完成了LGaH₂ (12)的合成。LAl(Me)Cl (1)和LAlH₂ (6)分别已被转化为LAl(Me)F (5)和LAlF₂ (7)。前者是在LAl(Me)Cl与Me₃SnF的反应中获得的，而后者是在LAlH₂与BF₃·OEt₂的反应中分离得到的。类似地，LGaI₂ (8)与Me₃SnF反应得到LGaF₂ (9)。本文报道的化合物已通过元素分析、红外光谱、核磁共振、电子轰击质谱和单晶X射线衍射技术进行了表征。
