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Exchange reactions of LnCl3 and CymCO2K in aqueous‐organic medium in the presence of diethylene glycol (DEG) bring about isostructural tetranuclear cluster complexes with linear core, [Ln4(CymCO2)12(O(CH2CH2OH)2)2(H2O)4] ⋅ 2THF (Ln=Nd (1), Gd (2), Tb (3), Dy (4), Ho (5); Cym=(η5‐C5H4)Mn(CO)3). The complexes have centrosymmetric structure and contain two types of Ln3+ coordination centers. Thermal decomposition of the complexes under argon and air atmospheres was studied; in the latter case it brings about mixed oxides LnMn2O5 as one of the products. The complexes 1–5 were characterized by dc‐ and ac‐magnetic measurements. Complexes of Nd, Gd, and Dy exhibit the properties of single‐molecule magnets (SMMs) with remagnetization barriers Δeff/kB of 14 K for 1 under 2500 Oe dc‐field, 13 K for 2 under 1500 Oe dc‐field, and with two barriers, 18 and 19 K, for 4 in zero field. The presence of field‐induced slow relaxation of the magnetization detected for the complex 2 is a rare case for Gd complexes. [ABSTRACT FROM AUTHOR]