TY - JOUR
T1 - Synthesis and structure of [Fe13O4F24(OME)12]5-
T2 - The first open-shell Keggin ion
AU - Bino, Avi
AU - Ardon, Michael
AU - Lee, Dongwhan
AU - Spingler, Bernhard
AU - Lippard, Stephen J.
PY - 2002/5/1
Y1 - 2002/5/1
N2 - The reaction between ferric fluoride trihydrate and pyridine in hot methanol produced yellow-brown crystals of (PyH)5·[Fe13O4F24(OMe)12]·4H2O·CH3OH. The anionic complex [Fe13O4F24(OMe)12]5- (1), which has a full Td symmetry, is the first example of an open-shell Keggin ion consisting of 13 high-spin d5 iron(III) atoms. The central, tetrahedral {FeO4} unit in 1 is surrounded by 12 octahedral iron atoms, which are bridged by methoxide oxygen atoms and fluoride ligands. In addition, each of the 12 iron atoms is coordinated to a terminal fluoride ligand with an Fe-F distance of 1.846(3) Å. Magnetic susceptibility studies indicate strong exchange interactions between the iron atoms, the μeff value of 19.3 μB at 300 K being significantly lower than that expected for thirteen uncoupled S = 5/2 centers.
AB - The reaction between ferric fluoride trihydrate and pyridine in hot methanol produced yellow-brown crystals of (PyH)5·[Fe13O4F24(OMe)12]·4H2O·CH3OH. The anionic complex [Fe13O4F24(OMe)12]5- (1), which has a full Td symmetry, is the first example of an open-shell Keggin ion consisting of 13 high-spin d5 iron(III) atoms. The central, tetrahedral {FeO4} unit in 1 is surrounded by 12 octahedral iron atoms, which are bridged by methoxide oxygen atoms and fluoride ligands. In addition, each of the 12 iron atoms is coordinated to a terminal fluoride ligand with an Fe-F distance of 1.846(3) Å. Magnetic susceptibility studies indicate strong exchange interactions between the iron atoms, the μeff value of 19.3 μB at 300 K being significantly lower than that expected for thirteen uncoupled S = 5/2 centers.
UR - http://www.scopus.com/inward/record.url?scp=0036569676&partnerID=8YFLogxK
U2 - 10.1021/ja025590a
DO - 10.1021/ja025590a
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C2 - 11971702
AN - SCOPUS:0036569676
SN - 0002-7863
VL - 124
SP - 4578
EP - 4579
JO - Journal of the American Chemical Society
JF - Journal of the American Chemical Society
IS - 17
ER -