TY - JOUR
T1 - New iron tetrazolate frameworks
T2 - synthesis, temperature effect, thermal behaviour, Mössbauer and magnetic studies
AU - Pimenta, Vanessa
AU - Le, Quang Hoang Hanh
AU - Clark, Lucy
AU - Lhoste, Jerome
AU - Hemon-Ribaud, Annie
AU - Leblanc, Marc
AU - Greneche, Jean-Marc
AU - Dujardin, G.
AU - Lightfoot, Philip
AU - Maisonneuve, Vincent
PY - 2015/5/7
Y1 - 2015/5/7
N2 - 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.
AB - 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.
UR - http://pubs.rsc.org/is/content/articlehtml/2015/dt/c5dt00281h
U2 - 10.1039/C5DT00281H
DO - 10.1039/C5DT00281H
M3 - Article
SN - 1477-9234
VL - 44
SP - 7951
EP - 7959
JO - Dalton Transactions
JF - Dalton Transactions
IS - 17
ER -