The (C
2H
10N
2)
0.5[M(HPO
3)
2] (M = V, Fe) inorganic-organic hybrid compounds have beensynthesized under mild hydrothermal conditions. The crystal structure determination ofthe vanadium phase has been carried out from X-ray powder diffraction data by using theab initio method. A Rietveld full-profile refinement has been performed on the isostructuraliron compound. The unit-cell parameters are
a = 9.243(1),
b = 8.817(1),
c = 9.684(1) Å, and
![](/images/gifchars/beta2.gif)
= 120.92(2)
![](/images/entities/deg.gif)
and
a = 9.247(1),
b = 8.824(1),
c = 9.693(1) Å, and
![](/images/gifchars/beta2.gif)
= 120.72(1)
![](/images/entities/deg.gif)
for thevanadium and iron compounds, respectively. Both compounds are monoclinic,
P2/
c with
Z = 4. The crystal structure consists of a three-dimensional framework with channels alongthe
c axis where the ethylenediammonium cations are located. The metallic ions areinterconnected by the pseudopyramidal (HPO
3)
2- phosphite anions and adopt a tetrahedral-like-diamond distribution. The IR and Raman spectra of both phases show the bandscorresponding to the phosphite oxoanions and ethylenediammonium cations. The diffusereflectance spectra in the visible region are consistent with the existence of vanadium(III)and high-spin iron(III) cations in slightly distorted octahedral coordination. Magneticmeasurements indicate the existence of antiferromagnetic interactions being stronger inthe iron compound.