Single crystals of [H3dien]·(FeF6)·H2O (I) and [H3dien]·(CrF6)·H2O (II) are obtained by solvothermal synthesis under microwave heating. I is orthorhombic (Pna21) with a=11.530(2) Å, b=6.6446(8) Å, c=13.787(3) Å, V=1056.3(2) Å3and Z=4. II is monoclinic (P21/c) with a=13.706(1) Å, b=6.7606(6) Å, c=11.3181(9) Å, β=99.38(1)°, V=1034.7(1) Å3and Z=4. The structure determinations, performed from single crystal X-ray diffraction data, lead to the R1/wR2reliability factors 0.028/0.066 for I and 0.035/0.102 for II. The structures of I and II are built up from isolated FeF6or CrF6octahedra, water molecules and triprotonated amines. In both structures, each octahedron is connected by hydrogen bonds to six organic cations and two water molecules. The iron-based compound is also characterized by57Fe Mössbauer spectrometry: the hyperfine structure confirms the presence of Fe3+in octahedral coordination and reveals the existence of paramagnetic spin fluctuations. © 2007 Elsevier Inc. All rights reserved.
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