Synthesis and spectroscopic characterization of the heterosilylated anions [PW9O34(tBuSiO)3(SiR)]3- (R = -CH3, -CH=CH2, -CH2-CH=CH2, -(CH2)4-CH=CH2) -: X-ray crystal structure of [nBu4N]3[PW9O34(tBuSiO)3(SiCH2-CH=CH2)]

被引:28
作者
Agustin, D [1 ]
Coelho, C [1 ]
Mazeaud, A [1 ]
Herson, P [1 ]
Proust, A [1 ]
Thouvenot, R [1 ]
机构
[1] Univ Paris 06, UMR CNRS 7071, Lab Chim Inorgan & Mat Mol, F-75252 Paris 05, France
来源
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE | 2004年 / 630卷 / 12期
关键词
polyoxometalates; tungsten; silicon; organic-inorganic hybrids; NMR (multinuclear);
D O I
10.1002/zaac.200400276
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The reaction of the open-structure anion [PW9O34((BuSiOH)-Bu-t)(3)](3-) with RSiCl3 (R = (CH2)(n)CH=CH2 (n = 0, 1, 4)) affords [PW9O34((BuSiO)-Bu-t)(3)(SiR)](3-) heterosilylated capped hybrid compounds. These complexes were characterized by infrared spectroscopy and in solution by multinuclear (H-1, Si-29, P-31 and W-183) NMR. Crystals of [(Bu4N)-Bu-n](3)[PW9O34((BuSiO)-Bu-t)(3)Si(CH2-CH=CH2)] are orthorhombic, space group P2(1)2(1)2(1) (Ndegrees 19), with lattice constants a = 15.599(2) Angstrom, b = 23.963(5) Angstrom, c = 26.886(1) Angstrom, V = 10.050(3) Angstrom(3), and Z = 4.
引用
收藏
页码:2049 / 2053
页数:5
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