| Summary: | Three new 1D cyanido-bridged 3d-4f coordination polymers, {[Gd(L)(H<sub>2</sub>O)<sub>2</sub>Fe(CN)<sub>6</sub>]·H<sub>2</sub>O}<sub>n</sub> (<b>1</b><sub>GdFe</sub>), {[Dy(L)(H<sub>2</sub>O)<sub>2</sub>Fe(CN)<sub>6</sub>]·3H<sub>2</sub>O}<sub>n</sub> (<b>2</b><sub>DyFe</sub>), and {[Dy(L)(H<sub>2</sub>O)<sub>2</sub>Co(CN)<sub>6</sub>]·H<sub>2</sub>O}<sub>n</sub> (<b>3</b><sub>DyCo</sub>), were assembled following the building-block approach (L = pentadentate <i>bis</i>-semicarbazone ligand resulting from the condensation reaction between 2,6-diacetyl-pyridine and semicarbazide). The crystal structures consist of crenel-like Ln<sup>III</sup>-M<sup>III</sup> alternate chains, with the Ln<sup>III</sup> ions connected by the hexacyanido metalloligands through two <i>cis</i> cyanido groups. The magnetic properties of the three complexes have been investigated. Field-induced slow relaxation of the magnetization was observed for compounds <b>2</b><sub>DyFe</sub> and <b>3</b><sub>DyCo</sub>. Compound <b>3</b><sub>DyCo</sub> is a new example of chain of Single Ion Magnets.
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