Synthesis and Structural Characterization of Alkaline-Earth-Metal Bis(amido)silane and Lithium Oxobis(aminolato)silane Complexes
详细信息 查看全文
- 作者：Dongming Yang ; Yuqiang Ding ; Haishun Wu ; Wenjun Zheng
- 刊名：Inorganic Chemistry
- 出版年：2011
- 出版时间：August 15, 2011
- 年：2011
- 卷：50
- 期：16
- 页码：7698-7706
- 全文大小：1101K
- 年卷期：v.50,no.16(August 15, 2011)
- ISSN：1520-510X
文摘
Several of alkaline-earth-metal complexes [(畏2:畏2:渭(N):渭(N)-Li)+]2[{畏2-Me2Si(DippN)2}2Mg]2鈥?/sup> (4), [畏2(N,N)-Me2Si(DippN)2Ca路3THF] (5), [畏2(N,N)-Me2Si(DippN)2Sr路THF] (6), and [畏2(N,N)-Me2Si(DippN)2Ba路4THF] (7) of a bulky bis(amido)silane ligand were readily prepared by the metathesis reaction of alkali-metal bis(amido)silane [Me2Si(DippNLi)2] (Dipp = 2,6-i-Pr2C6H3) and alkaline-earth-metal halides MX2 (M = Mg, X = Br; M = Ca, Sr, Ba, X = I). Alternatively, compounds 5鈥?b>7 were synthesized either by transamination of M[N(SiMe3)2]2路2THF (M = Ca, Sr, Ba) and [Me2Si(DippNH)2] or by transmetalation of Sn[N(SiMe3)2]2, [Me2Si(DippNH)2], and metallic calcium, strontium, and barium in situ. The metathesis reaction of dilithium bis(amido)silane [Me2Si(DippNLi)2] and magnesium bromide in the presence of oxygen afforded, however, an unusual lithium oxo polyhedral complex {[(DippN(Me2Si)2)(渭-O)(Me2Si)]2(渭-Br)2[(渭3-Li)路THF]4(渭4-O)4(渭3-Li)2} (8) with a square-basket-shaped core Li6Br2O4 bearing a bis(aminolato)silane ligand. All complexes were characterized using 1H, 13C, and 7Li NMR and IR spectroscopy, in addition to X-ray crystallography.