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Synthesis of phosphinogallyliron complexes and their photochemical conversion to a naked gallium-bridged diiron complex
Journal of Organometallic Chemistry ( IF 2.1 ) Pub Date : 2020-11-18 , DOI: 10.1016/j.jorganchem.2020.121625
Takako Muraoka , Tatsuya Yamada , Koichiro Motoyoshi , Keiji Ueno

The dichlorogallyliron complexes Cp’(OC)2FeGaCl2 (Cp’ = Cp* (4a), Cp (4b), Cp*: η5-C5Me5, Cp: η5-C5H5), when treated with LiPPh2 and/or Me3SiPPh2 in Et2O, produce the four-membered Ga2P2 cyclic diiron complexes [Cp’(OC)2FeGa(Cl)PPh2]2 (Cp’ = Cp* (5a), Cp (5b)) in 64% and 47% yields, respectively. Crystal structure analysis using X-ray crystallography revealed that the four-membered Ga2P2 cyclic structure in cis-5a is slightly puckered. The four-membered Ga2P2 cyclic structure remains undisturbed in a solution of complex 5a in C6D6 and C7D8. 5a exists as a mixture of the cis/trans geometric isomers in these solutions. The photochemical reaction with complex 5b in C6D6 produces a complex mixture. However, the photochemical reaction with complex 5a in C6D6 afforded the six-membered Fe-Ga-Fe-P-Ga-P cyclic diiron complex [{Cp*(OC)Fe}2(μ-Ga)(μ-Ph2PGaCl2PPh2)] (6a) in 61% yield (NMR yield). Crystal structure analysis revealed that complex 6a contains the Ga atom-bridged Fe-Ga-Fe fragment with two Fe−Ga multiple bonds.



中文翻译:

膦酰烯丙基铝络合物的合成及其光化学转化为裸镓桥联二铁络合物

所述dichlorogallyliron络合物CP '(OC)2 FeGaCl 2(CP'=的Cp *(图4a)中,Cp(图4b)中,Cp *:η 5 -C 55中,Cp:η 5 -C 5 H ^ 5),经处理的时与LiPPh 2和/或Me 3 SiPPh 2在Et 2 O中,生成四元Ga 2 P 2环状二铁配合物[Cp'(OC)2 FeGa(Cl)PPh 2 ] 2(Cp'= Cp *(5a),Cp(5b))的收益率分别为64%和47%。使用X-射线晶体学晶体结构分析表明,该四元嘎2 P 2在环状结构的顺式-图5a略微起皱。四元Ga 2 P 2环状结构在C 6 D 6和C 7 D 8中的络合物5a的溶液中保持不变。5a在这些溶液中以/几何异构体的混合物形式存在。与络合物5b在C 6 D 6中的光化学反应产生复杂的混合物。然而,与络合物5a在C 6 D 6中的光化学反应提供了六元Fe-Ga-Fe-P-Ga-P环状二铁络合物[{Cp *(OC)Fe} 2(μ-Ga)(μ- Ph 2 PGaCl 2 PPh 2)](6a)的产率为61%(NMR产率)。晶体结构分析表明,配合物6a包含带有两个Fe-Ga多个键的Ga原子桥接的Fe-Ga-Fe片段。

更新日期:2020-11-25
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