Identification of AlFx(OR)y Species in Strongly Disordered Aluminum Isopropoxide Fluoride Solids: A Field-Dependent MAS NMR Study
Identification of AlFx(OR)y Species in Strongly Disordered Aluminum Isopropoxide Fluoride Solids: A Field-Dependent MAS NMR Study
复制标题
强无序氟化异丙醇铝固体中 AlFx(OR)y 形态的鉴定：场相关 MAS NMR 研究
DOI：
10.1021/jp9066795
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发表时间：
2009
影响因子：
3.7
通讯作者：
E. Kemnitz
中科院分区：
文献类型：
--
作者：
R. König;G. Scholz;A. Pawlik;C. Jäger;B. Rossum;E. Kemnitz
高度无序和X-射线无定形氟化异丙氧基铝可以被看作是在高表面AlF 3的合成过程中形成的中间体。在高达21.1T的不同磁场下记录了它们的~（27）Al MAS NMR谱。在B 0 = 14.1 T下得到的27 Al 3QMAS实验数据使得能够模拟27 Al MAS NMR谱。除了6重配位物种外，该系统首次明确确定了4重和5重配位AlFx（OiPr）CN−x（配位数CN为4或5）的存在。观察到的氟和异丙氧基铝氟化物与不同的F含量的化学位移的比较允许一个简单的相关性为适当的物种。作为一个主要的结果，相应的F-物种连接到4倍和5倍协调的铝物种的暗示得到证实。此外，这是第一次，固体中存在的AlFxO 4 −x和AlFxO 5 −x单元可以基于全面的图形解释进行分配（27 Al化学...
Highly disordered and X-ray amorphous aluminum isopropoxide fluorides can be seen as intermediates formed during the synthesis of high-surface AlF3. Their 27Al MAS NMR spectra were recorded at different magnetic fields of up to 21.1 T. The 27Al 3QMAS experimental data derived at B0 = 14.1 T enabled the simulation of the 27Al MAS NMR spectrum. In addition to 6-fold coordinated species, the presence of four- and 5-fold coordinated AlFx(OiPr)CN−x (coordination number, CN, of 4 or 5) was unambiguously established for the first time for this system. A comparison of the chemical shifts observed for fluorine and aluminum isopropoxide fluorides with different F contents allows for a simple correlation for the appropriate species. As a main outcome, hints of corresponding F-species connected to 4-fold and 5-fold coordinated Al species were corroborated. Moreover, for the first time, AlFxO4−x and AlFxO5−x units present in the solids could be assigned based on a comprehensive graphical interpretation (27Al chemical ...