Inorganic-organic hybrid materials:: synthesis and crystal structure determination from powder diffraction data of Pb2(O3PCH2C6H4CH2PO3)

被引:31
作者
Irran, E
Bein, T
Stock, N
机构
[1] Univ Munich, Dept Chem, D-81377 Munich, Germany
[2] Tech Univ Berlin, Inst Chem, D-10623 Berlin, Germany
关键词
lead; phosphonate; hybrid material; hydrothermal synthesis; IR spectroscopy; X-ray diffraction; Rietveld refinement;
D O I
10.1016/S0022-4596(03)00085-9
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
A new lead diphosphonate, Pb-2(O3PCH2C6H4CH2PO3) was hydrothermally synthesized from tetraethyl alpha,alpha'-p-xylenediphosphonate and Pb(NO3)(2). The structure was solved and refined using X-ray powder diffraction data. It crystallizes in the monoclinic space group P2(1)/c, with a = 467.84(2), b = 2007.98(9), c = 639.10(2) pm, beta = 101.020(3)degrees, V = 589.31(4) 10(6) pm, Z = 2 wR(p) = 0.034, R-p = 0.0277 R(F)2 = 0.061, R-F = 0.036. The structure is built from corner-linked [PbO4] polyhedra, containing a lone pair of electrons. These polyhedra are connected to layers by phosphonate groups, RPO32- and through the organic diphosphonic acid to a three-dimensional structure. Thermogravimetric as well as IR spectroscopic studies are also presented. (C) 2003 Elsevier Science (USA). All rights reserved.
引用
收藏
页码:293 / 298
页数:6
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