Organic-inorganic hybrids based on polyoxometalates.: 5.: Synthesis and structural characterization of bis(organophosphoryl)decatungtosilicates [γ-SiW10O36((RPO)2]4-

被引：89

作者：

Mayer, CR ^{[1
]}

Herson, P ^{[1
]}

Thouvenot, R ^{[1
]}

机构：

[1] Univ Paris 06, CNRS, U7071, Lab Chim Inorgan & Mat Mol, F-75252 Paris 05, France

来源：

INORGANIC CHEMISTRY | 1999年 / 38卷 / 26期

关键词：

D O I：

10.1021/ic990724f

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

Organophosphoryl polyoxotungstate derivatives [gamma-SiW10O36(RPO)(2)](4-) (R = H (1), Et (2), n-Bu (3), t-Bu (4), C2H4COOH (5), Ph (6)) have been obtained by reaction of the divacant [gamma-SiW10O36](8-) anion with organophosphonic acids RPO(OH)(2) in acetonitrile. These new heteropolyanions have been characterized by elemental analysis, infrared spectroscopy, multinuclear (H-1, Si-29, P-31, and W-183) NMR, and X-ray crystallography. Crystals of (NBu4)(2)(NEt4)H[gamma-SiW10O36(C6H5PO)(2)] (anion 6) are monoclinic, space group P2(1), with lattice constants a = 16.489(4) Angstrom, b = 14.016(3) Angstrom, c = 18.542(8) Angstrom, beta = 91.30(3)degrees and Z = 2. The hybrid anion has a structure of virtual C-2v symmetry with two phenylphosphonate groups grafted to the surface of the divacant tungstosilicate. W-183 and P-31 NMR spectra of NBu4 salts in DMF solution agree with the solid-state structure and the virtual C-2v symmetry.

引用

页码：6152 / 6158

页数：7

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