The two intermediate spin, five-coordinated complexes [Fe(nia)2Br3](H2O) and [Fe(nia)3(H2O)2](ClO4)3 were synthesized. Their spectroscopic, thermal and magnetic properties were characterized. The magnetic properties of both compounds are consistent with S = 3/2 ground state. Magnetic measurements over the temperature range 1.8–300 K re vealed antiferromagnetic interaction between Fe(III) magnetic centers in the crystal lattice and the presence of Neel temperature for both compounds [Fe(nia)2Br3](H2O) at 4.7 K and [Fe(nia)3(H2O)2](ClO4)3 at 3.0 K.
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