Issue 23, 2007

Layered microporous tin(iv) bisphosphonates


This article reports the hydrothermal synthesis and characterization of two new series of porous tin(IV) phosphonophenoxyphenylphosphonates with controlled pore size distributions, using as precursor the 4-(4′-phosphonophenoxy)phenyl phosphonic acid, [H2O3P–C6H4]2–O. Supermicroporous solids (SBET, 300–400 m2 g−1) were obtained employing n-alcohol (C1-C6)–water mixtures (solvents ratio 1 : 1), in the presence of hydrofluoric acid. X-Ray powder diffraction shows that these compounds are semi-crystalline and the local environments around the phosphorus and tin elements have been studied by 31P and 119Sn MAS-NMR spectroscopy, respectively. The microstructure (particle sizes and shapes) of these phosphonates has been analyzed by scanning and transmission electron microscopy. This study shows that the microstructures of single-ligand (for instance tin(IV) phenylphosphonate) and cross-linked tin(IV) bisphosphonates are different. Tin(IV) phenylphosphonate crystallizes as micron-sized spheres, ∅ ∼ 1–2 µm, formed by the aggregation of nanospheres, whereas tin(IV) bisphosphonates crystallize as microparticles larger than 20 µm. The textural properties of these porous solids were characterized by N2 and CO2 sorption isotherms. The key result of this work is that maxima of pore size distributions smoothly shift from 12 to 16 Å upon increasing the chain length of the alcohol. The microporosity of tin(IV) bisphosphonates is compatible with a double role played by the phosphonate groups acting as a pillar between adjacent layers and as a component of the hybrid organic–inorganic layers.

Graphical abstract: Layered microporous tin(iv) bisphosphonates

Supplementary files

Article information

Article type
22 Dec 2006
12 Mar 2007
First published
03 Apr 2007

Dalton Trans., 2007, 2394-2404

Layered microporous tin(IV) bisphosphonates

M. D. M. Gómez-Alcántara, A. Cabeza, P. Olivera-Pastor, F. Fernández-Moreno, I. Sobrados, J. Sanz, R. E. Morris, A. Clearfield and M. A. G. Aranda, Dalton Trans., 2007, 2394 DOI: 10.1039/B618762E

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