Abstract
Single crystals of [H
3
dien]·(FeF
6)·H
2O (
I) and [H
3
dien]·(CrF
6)·H
2O (
II) are obtained by solvothermal synthesis under microwave heating.
I is orthorhombic (
Pna2
1) with
a=11.530(2)
Å,
b=6.6446(8)
Å,
c=13.787(3)
Å,
V=1056.3(2)
Å
3 and
Z=4.
II is monoclinic (
P2
1
/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)
Å
3 and
Z=4. The structure determinations, performed from single crystal X-ray diffraction data, lead to the
R
1/w
R
2 reliability 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 FeF
6 or CrF
6 octahedra, 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 by
57Fe Mössbauer spectrometry: the hyperfine structure confirms the presence of Fe
3+ in octahedral coordination and reveals the existence of paramagnetic spin fluctuations.
Mössbauer spectra of [H
3
dien]·(FeF
6)·H
2O.