Coordination complexes with biologically active ligands have a broad application in medicine and biotechnology. Pivalic acid (Hpiv) has found its use as a prodrug in carnitrine homeostasis in human body [1]. In addition, drugs functionalized with pivalic acid increase their oral bioavailability. Moreover, pivalic acid has also been used in antibiotics synthesis [2] and for the preparation of polynuclear clusters as effective catalysts in organic synthesis [3].In continue of our research on preparation of polynuclear coordination clusters of d-f metals with pivalic acid a new heterometallic tetranuclear coordination compound namely [Fe2Dy2(piv)6(thme)2(MeOH)4]·2(MeOH)·2(H2O) was synthesized from the reaction of μ-oxo trinuclear iron pivalate with Dy(NO3)3·6H2O and 1,1,1-tris(hydroxymethyl)ethane (H3thme) ligand in methanol solution. Single-crystal X-ray diffraction analysis showed that the obtained pivalate compound crystallizes in the triclinic P-1 space group with a = 11.2824(9), b = 12.5156(7), c = 14.8596(1) Å, α = 74.089(6), β = 67.987(7), γ = 70.593(6)°, V = 1807.72 Å3 and comprises the neutral cluster [Fe2Dy2(piv)6(thme)2(MeOH)4] and solvent molecules. The cluster (Figure) contains a {Fe2Dy2}12+ core, where two FeIII and two DyIII centers are connected by two thme3- ligands with Fe…Dy distances of 3.427 and 3.434 Å, and a Fe…Fe distance of 3.189 Å. Metal atoms reside in the vertexes of rhombus and are additionally linked by four pivalate ligands. Monodentate pivalate and two MeOH complete the coordination sphere for each of the Dy atoms. In cluster, FeIII atoms are six–coordinated with a distorted octahedral O6 geometry being coordinated by four O atoms from two thme3- and two O atoms from two pivalate bridges (Fe-O, 1.954(4)-2.096(5) Å). The DyIII atoms are eight–coordinated by three O bridging atoms of thme3- ligands (Dy-O, 2.337(4)-2.436(4) Å), three O atoms from three pivalates (Dy-O, 2.306(5) 2.370(4) Å) and two O atoms from two methanol molecules (Dy-O, 2.407(5) and 2.419(7) Å). The coordinated methanol molecules and monodentate pivalates as well as solvent molecules establish a system of intra- and intermolecular hydrogen bonds joining heterometallic clusters into chains. The spectroscopic and thermogravimetric properties of [Fe2Dy2(piv)6(thme)2(MeOH)4] ·2(MeOH)·2(H2O) have also been studied and will be discussed in terms of the known structure.