Synthesis, crystal structure and NMR of [Na(DB18C6)(CH3CN)]3[α-PW12O40]

被引:14
作者
Lu, XM [1 ]
Liu, B
Sarula
Wang, J
Ye, CH
机构
[1] Capital Normal Univ, Dept Chem, Beijing 100037, Peoples R China
[2] SINOPEC, Res Inst Petr Proc, Beijing 100083, Peoples R China
[3] Wuhan Inst Phys, Wuhan 430071, Peoples R China
关键词
crown ether; polytungatate; NMR; crystal structure;
D O I
10.1016/j.poly.2005.03.019
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
A novel super-molecular complex [Na(DB18C6)(CH3CN)](3) [alpha-PW12O40] was obtained by solvothernial reaction and characterized by IR, X-ray, H-1, C-13 and P-31 NMR. The result reveals that the complex consists of all [alpha-PW12O40](3-) anion with alpha-Keggin structure and three complex [Na(DB18C6)(CH3OH)](+) cations in which every sodium ion located in the cavity of dibelizo-18-crown-6 with six Na-O bonds and coordinated with one of the terminal O atom of [alpha-PW12O40](3-) and the N atom of CH3CN from two sides of the distorted DB18C6 plane, respectively. The three terminal 0 atoms linked with sodium ion are from a single W3O3 triplet of the alpha-Keggin tungstophosphate anion. The C-13 resonance (119.27 ppm) bonded to N atom in CH3CN has been clarified by gUMBC spectrum (see Fig. 1), which is too weak to be observed in 13 C NMR spectrum due to its too low relaxation rate. (c) 2005 Elsevier Ltd. All rights reserved.
引用
收藏
页码:2889 / 2893
页数:5
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