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Two 3 d ‐4 f  hetero‐metal pentanuclear complexes with the formula {[Cr III  2 Ln III  3 L 10 (OH) 6 (H 2 O) 2 ]Et 3 NH} [Ln=Tb ( 1 ), Dy ( 2 ); HL=pivalic acid, Et 3 N=triethylamine] have been produced. The metal core of each cluster is made up of a trigonal bipyramid with three Ln III  ions (plane) and two Cr III  ions (above and below) held together by six  μ  3 ‐OH bridges. Also reported with this series is the diamagnetic Cr III –Y III  analogue ( 3 ). Fortunately, we successfully prepared Al III –Ln III  analogues with the formula {[Al III  2 Ln III  3 L 10 (OH) 6 (H 2 O) 2 ]Et 3 NH⋅H 2 O} [Ln=Tb ( 4 ), Dy ( 5 )], containing diamagnetic Al III  ions, which can be used to evaluate the Cr III –Ln III  magnetic nature through a diamagnetic substitution method. Subsequently, static (dc) magnetic susceptibility studies reveal dominant ferromagnetic interactions between Cr III  and Ln III  ions. Dynamic (ac) magnetic susceptibility studies show frequency‐dependent out‐of‐phase ( χ ′′) signals for [Cr III  2 Tb III  3 ] ( 1 ), [Cr III  2 Dy III  3 ] ( 2 ), and [Al III  2 Dy III  3 ] ( 5 ), which are derived from the single‐ion behavior of Ln III  ions and/or the Cr III –Ln III  ferromagnetic interactions.

Magnetic Nature of the Cr III –Ln III Interactions in [Cr III 2 Ln III 3 ] Clusters with Slow Magnetic Relaxation