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Inserting 3d metal-cmplex Cu(acac) 2 into the crystal lattice of paramagnetic Dy(hfac) 3 (H 2 O) 2 leads to the formation of the first true 3d-4f cocrystal made up of only reactants, which exhibits improved magnetic performance with evident SIM behavior. • A genuine 3d-4f complex cocrystal only composed of reactants. • The cocrystal displays evident SIM behavior. • Co-crystallization is a useful tool for improving the magnetic property of LnIII complex. Employing Cu(acac) 2 to react with Dy(hfac) 3 (H 2 O) 2 (where acac− = acetylacetonate and hfac− = 1,1,1,5,5,5-hexafluoroacetylacetonate), the first true 3d-4f metal-complex cocrystal with the composition of [Cu(acac) 2 ·Dy(hfac) 3 (H 2 O) 2 that only consists of reactants, was acquired and structurally characterized. Magnetic investigations revealed that the 4f coformer Dy(hfac) 3 (H 2 O) 2 does not show slow magnetic relaxation behavior even under an applied dc field of 2000 Oe down to 1.9 K, while the obtained 3d-4f cocrystal displays evident slow magnetic relaxation behavior associated with single-ion magnet (SIM) characteristic under the same dc field. This phenomenon is further supported and elucidated by the results of theoretical calculations together with the analyses of their crystal structures. Thus our results first indicate that 3d-4f co-crystallization technique is a useful tool for improving the magnetic performance of lanthanide complexes. [ABSTRACT FROM AUTHOR]