Bunge Scott D, Bertke Jeffrey A, Cleland Travis L
Kent State University, Department of Chemistry, Kent, Ohio 44242, USA.
Inorg Chem. 2009 Aug 17;48(16):8037-43. doi: 10.1021/ic9007153.
Diethylcyanamide is added to a hexanes solution of lithium diethylamide [LiN(CH(2)CH(3))(2)] resulting in the formation of lithium 1,1,3,3-tetraethylguanidinate, Li(mu-TEG) (1). Upon successful isolation of 1, the metathesis reaction of MX(2) (MX(2) = MnBr(2), FeBr(2), CoBr(2), and ZnCl(2)) with Li(mu-TEG) and lithium bistrimethylsilylamide, LiN(SiMe(3))(2), was performed to generate dinuclear tetraethylguanidinate (TEG) complexes with the general formula M(mu-TEG){N(SiMe(3))(2)} {M = Mn (2), Fe (3), Co (4), Zn (5)}. Further reaction of 2 with 2 equiv of ethanol (EtOH) and 2 equiv of 2,6-ditert-butylphenol (H-DBP) results in the formation of the manganese alkoxide, Mn(mu-OEt)(DBP)(H-TEG) (6). Elemental analysis, FT-IR spectroscopy, UV-vis spectroscopy, and single crystal X-ray diffraction were utilized to characterize the six compounds.
将二乙基氰胺加入到二乙胺锂[LiN(CH(2)CH(3))(2)]的己烷溶液中，生成1,1,3,3 - 四乙基胍基锂Li(μ - TEG) (1)。成功分离出1后，使MX(2)（MX(2) = MnBr(2)、FeBr(2)、CoBr(2)和ZnCl(2)）与Li(μ - TEG)以及双(三甲基硅基)氨基锂LiN(SiMe(3))(2)发生复分解反应，生成通式为M(μ - TEG){N(SiMe(3))(2)}的双核四乙基胍基（TEG）配合物{M = Mn (2)、Fe (3)、Co (4)、Zn (5)}。2与2当量的乙醇（EtOH）和2当量的2,6 - 二叔丁基苯酚（H - DBP）进一步反应，生成锰醇盐Mn(μ - OEt)(DBP)(H - TEG) (6)。利用元素分析、傅里叶变换红外光谱、紫外 - 可见光谱和单晶X射线衍射对这六种化合物进行了表征。
