Over the past decade there has been an extraordinary interest in the synthesis, investigation and possible applications of heterometallic 3d-4f coordination clusters. A new heterometallic tetranuclear cluster [Mn2Gd2O2(piv)8(Hpiv)2(EtOH)2] (1) (where Hpiv = pivalic acid) has been prepared by the reaction of Mn(piv)2 with Gd(NO3)3 6H2O in the presence of triethanolamine in a mixture of ethanol and acetonitrile. The complex was characterized by IR spectroscopy and the X-ray study. The IR spectrum of 1 contains strong and broad bands in the 1672 - 1545 and 1406 cm^-1 regions, resulting from asymmetric and symmetrical stretching vibrations of the coordinated carboxylate groups, respectively. The C–H asymmetric and symmetrical stretching vibrations for methyl and ethyl groups of carboxylates and EtOH are observed between 2962 and 2872 cm^-1, while asymmetric and symmetrical bending vibrations for these groups produce a band at 1482 cm^-1 and a doublet (1373 - 1357 cm^-1), respectively. The uncoordinated OH groups of HPiv and the coordinated OH of EtOH molecules result in a broad band of 3275 cm^-1. Compound 1 crystallizes in the monoclinic space group C2/c, a = 27.883(2), b = 13.369(4), c = 24.212(2) Å, beta = 128.04(11)°, V = 7107.9(11) Å3. Single crystal X-ray analysis showed that the complex possesses a centrosymmetric tetranuclear unit [Mn2Gd2O2(piv)8(Hpiv)2(EtOH)2] (Figure). The structure of the {Mn2Gd2} core of the compound consists of two manganese(III) ions and two gadolinium(III) ions, connected by two m3-oxo groups. The metal atoms of the MnGd edges (3.475Å) in the {Mn2Gd2} rhomb are additionally connected via bridge linkages formed by the entrainment of two pivalate ligands. Each of the MnIII ions is six-coordinated and adopts an octahedral O6 configuration, and the GdIII ions receive the nine coordinate number. The central MnIII atoms are coordinated by two m3-oxo atoms (Mn–m3-O, 1.897(5) Å), four oxygen atoms from different pivalate ligands (Mn–O, 1.960(5) – 2.196(4) Å). The Mn…Mn separation is 2.846Å. The terminal Gd^III atoms are surrounded by the m3-oxygen atom (Gd–m3-O, 2.571(6) Å), the seven oxygen atoms of the different pivalate ligands (Gd–O, 2.505(4) – 2.571(4) Å) and the oxygen atom belonging to the EtOH molecule with a Gd–O distance of 2.395(4) Å. Two coordinated pivalic acids form strong O–H…O hydrogen bonds of 2.550(6) Å with m3-O.