Two new hetero-tetranuclear complexes, [Sm-2(o-phen)(2)(DMF)(6)(H2O)2(mu-CN)(4)Fe-2 (CN)(8)]center dot 5H(2)O center dot CH3OH (1) and [Sm-2(o-phen)(2)(DMF)(6)(H2O)(2)(mu-CN)(4)Co-2(CN)(8)]center dot 5H(2)O (2), have been prepared from reaction of SmCl3 center dot 6H(2)O, K-3[Fe(CN)(6)]center dot 3H(2)O or K-3[Co(CN)(6)], and o-phen in methanol/DMF, and characterized. The structure of I consists of a cyano-bridged discrete cyclic tetranuclear complex in which the Sm(III) and Fe(III) centers are linked by four CN groups. Mossbauer spectrum of 57 Fe indicates that both Fe(III) atoms in I have the same low-spin (S=1/2) electronic ground state. From comparison of the magnetic data of I and 2, at low temperature for I indicates weak ferromagnetic coupling between Sm(III) and Fe(III).