Issue 6, 2012

Mechanochemical interconversion between discrete complexes and coordination networks – formal hydration/dehydration by LAG

Abstract

Using a small planetary ball mill, liquid-assisted grinding (LAG) of metal salts or oxides (ZnO, CdO, CdCO3, Cu(OAc)2·H2O, Co(OAc)2·4H2O, Mn(OAc)2·4H2O, Ni(OAc)2·4H2O, FeSO4·7H2O) with two equivalents of isonicotinic acid (HINA) and small amounts of water (up to 5.6 molar equivalents) gave discrete aquo complexes trans-[M(INA)2(OH2)4] (M = Zn, Cd, Cu, Fe, Co, Ni, Mn) efficiently within 30 min. For M = Zn, Cd and Cu these complexes readily undergo reversible formal dehydration to the extended network structures [M(INA)2] (M = Zn, Cu) or [Cd(INA)2(OH2)]·DMF by further LAG with non-aqueous liquids such as methanol or DMF. Overall, the mechanochemical dehydrations are more effective than heating or immersion in bulk solvents. The work demonstrates a two-step mechanochemical synthesis of coordination networks via discrete aquo complexes which may be preferable to single step reactions or grinding-annealing procedures in some cases. For example, the two step method was the only way to prepare [Cd(INA)2(OH2)]·DMF mechanochemically and the porous network Cu(INA)2 could not be obtained from the aquo complex by heating.

Graphical abstract: Mechanochemical interconversion between discrete complexes and coordination networks – formal hydration/dehydration by LAG

Supplementary files

Article information

Article type
Paper
Submitted
02 Nov 2011
Accepted
04 Jan 2012
First published
19 Jan 2012

CrystEngComm, 2012,14, 1994-1997

Mechanochemical interconversion between discrete complexes and coordination networks – formal hydration/dehydration by LAG

P. Wang, G. Li, Y. Chen, S. Chen, S. L. James and W. Yuan, CrystEngComm, 2012, 14, 1994 DOI: 10.1039/C2CE06469C

To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page.

If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given.

If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page.

Read more about how to correctly acknowledge RSC content.

Social activity

Spotlight

Advertisements