White crystals of Fe((OPPh(2))(2)N)(3) were obtained from the reaction
of a solution of Fe-2(CO)(9) and excess (PPh(2))(2)NH, under an air a
tmosphere. This product does not form if the solvents are rigorously d
egassed and the reaction is performed under argon. The structure of th
e complex, as determined by single crystal X-ray crystallography, is a
n octahedral tris-chelate arrangement of the oxidized anionic ligand,
[(O=PPh(2))(2)N](-) coordinated to an Fe(III) center. The asymmetric u
nit of the unit cell also contains a disordered THF solvent molecule.
The complex crystallizes in the triclinic space group P (1) over bar,
with Z=2, a=13.581(3), b=13.886(8), c=18.781(7) Angstrom, alpha=95.48(
4), beta=98.73(2), gamma=97.82(3)degrees, V=3444(2) Angstrom(3), M(r)=
1377, D-x= 1.33 Mg m(-3), F(000)=1434, T=298 K and R=0.086 for 5959 ob
served reflections. The magnetic moment of the compound Fe((OPPh(2))(2
)N)(3) was found to be 5.4 BM, using the Gouy method. Reaction of the
oxidized ligand, (OPPh(2))(2)NH, with Fe(III) salts, such as Fe(NO3)(3
), produces Fe((OPPh(2))(2)N)(3) in high yields.