Recently we have report the μ3-OXO homotrinuclear iron(III) complex based on otoluilate ligands with composition [Fe3O(tol)6(CH3OH)1,5(H2O)1,5] NO3(DMAA) (H2O)(CH3OH) (I) [1]. It was found that the formation of a crystalline product is well reproducible only in the presence of a small amount of N, N-dimethylacetamide (DMAA). In order to obtain a similar heterometallic complex, we carry out the synthesis using iron nitrate, chromium nitrate and NH4tol (1:1:1 ratio of the reactants) in methanol medium without DMAA. However, elemental analysis has shown that there is no chromium in the composition of obtained complex (II). Crystals of II with composition [Fe3O(tol)6(CH3OH)2H2O]NO3 crystallizes in the monoclinic space group C2/c, a=11.3503(4), b=21.0676(9), c=22.0423(11)Å, β=95.574(4)°. V= 5245.9(4) Å3. Complex resides on two fold axis, thus having C2 molecular symmetry. The Fe3+ ions occupy the vertices of about equilateral triangle, Fe1 …Fe2 distances are equal 3.275 Å, while Fe2 …Fe2 distance is 3.286 Å. The center of the triangle is occupied by the μ3-O atom, which is coplanar with the metal core. Two trans-positions to μ3-O atom occupy methanol molecules and third one water molecule (Fig.1). The μ3-oxo trinuclear complexes with composition [Fe3O(tol)6Py(H2O)2]NO3·Py (III) and [Cr3O(tol)6Py(H2O)2]NO3 (IV) were prepared by interaction iron nitrate with o-toluic acid, and chromium nitrate with NH4tol in the presence of pyridine. Trinuclear structure of complex III was confirmed by parameters of Mossbauer spectra. Their parameters δNa +=0,66 mm/c and ΔEQ= 0,58 mm/c (RT) are consistent with the data for high-spin (S=5/2) iron complexes I and II. Trinuclear structure of complexes III and IV was confirmed on the basis of the identity of their infrared spectra, data of GR spectrum for II and III, and elemental analysis.