| Summary: | The solvothermal reactions of LnCl<sub>3</sub>·6H<sub>2</sub>O and MCl<sub>2</sub>·6H<sub>2</sub>O (M = Co, Ni) with 2,2′-diphenol (H<sub>2</sub>L<sup>1</sup>) and 5,7-dichloro-8-hydroxyquinoline (HL<sup>2</sup>) gave three 3d–4f heterometallic wheel-like nano-clusters [Ln<sub>7</sub>M<sub>6</sub>(L<sup>1</sup>)<sub>6</sub>(L<sup>2</sup>)<sub>6</sub>(<i>µ</i><sub>3</sub>-OH)<sub>6</sub>(OCH<sub>3</sub>)<sub>6</sub>Cl(CH<sub>3</sub>CN)<sub>6</sub>]Cl<sub>2</sub>·<i>x</i>H<sub>2</sub>O (Ln = Dy, M = Co, <i>x</i> = 3 for <b>1</b>; Ln = Dy, M = Ni, <i>x</i> = 0 for <b>2</b>; Ln = Tb, M = Ni, <i>x</i> = 0 for <b>3</b>) with similar cluster structure. The innermost Ln(III) ion is encapsulated in a planar Ln<sub>6</sub> ring which is further embedded in a chair-conformation M<sub>6</sub> ring, constructing a Russian doll-like 3d–4f cluster wheel Ln(III)⸦Ln<sub>6</sub>⸦M<sub>6</sub>. <b>2</b> and <b>3</b> show obvious slow magnetic relaxation behavior with negligible opening of the magnetic hysteresis loop. Such a Russian doll-like 3d–4f cluster wheel with the lanthanide disc isolated by transition metallo-ring is rarely reported.
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