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Issue 17, 2015
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New iron tetrazolate frameworks: synthesis, temperature effect, thermal behaviour, Mössbauer and magnetic studies

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Abstract

The exploration of the FeF3/FeF2-Hamtetraz-HF system in dimethylformamide by solvothermal synthesis evidences two isostructural 3D hybrid fluoroferrates. They are prepared from the same starting mixture at two different synthesis temperatures: 120 °C for [Hdma]·(Fe4IIFeIIIF8(H2O)2(amtetraz)4) (1) and 140 °C for [Hdma]1.5·(Fe4.5IIFe0.5IIIF7(H2O)(HCOO)(amtetraz)4) (2). Both compounds are characterized by single crystal X-ray diffraction, X-ray thermodiffraction, TGA analysis, Mössbauer spectrometry and SQUID magnetometry. They crystallize in the monoclinic system and are built from two distinct chains connected by aminotetrazolate anions. The first chain (FeIIFN4) is common to 1 and 2 and can be found in numerous fluorides. In the second chain (Fe3X12) (X = F, N, O), iron cations adopt both valence states Fe(II)/Fe(III). The hydrolysis of DMF implies the formation of a [Hdma]+ cation and a (HCOO) anion. The presence of Fe3+ in both phases is evidenced by 57Fe Mössbauer spectrometry. The magnetic properties are studied and two transitions from a paramagnetic regime to a long range ordered state below 30 K and 5 K are identified.

Graphical abstract: New iron tetrazolate frameworks: synthesis, temperature effect, thermal behaviour, Mössbauer and magnetic studies

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Supplementary files

Article information


Submitted
20 Jan 2015
Accepted
19 Mar 2015
First published
19 Mar 2015

Dalton Trans., 2015,44, 7951-7959
Article type
Paper

New iron tetrazolate frameworks: synthesis, temperature effect, thermal behaviour, Mössbauer and magnetic studies

V. Pimenta, Q. H. H. Le, L. Clark, J. Lhoste, A. Hémon-Ribaud, M. Leblanc, J. Grenèche, G. Dujardin, P. Lightfoot and V. Maisonneuve, Dalton Trans., 2015, 44, 7951
DOI: 10.1039/C5DT00281H

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