Abstract: | The title bimetallic compound, [Yb4(μ3‐OH)4(C6H13NO2)7(H2O)7][ZnCl4][ZnCl3(OH)]Cl4·8H2O, was synthesized at near physiological pH (6.0). The compound exhibits some novel structural features, including an asymmetric [Yb4(μ3‐OH)4(l ‐leucine)7(H2O)7]8+ complex cation in which four OH groups act as bridging ligands, linking four Yb3+ cations into a Yb4O4 structural unit. Each pair of adjacent Yb3+ ions is further bridged by one carboxy group from a leucine ligand. Water molecules and a monodentate leucine ligand also coordinate to Yb3+ ions, completing their eight‐coordinate square‐antiprismatic coordination. The Yb4(μ3‐OH)4(l ‐leucine)7(H2O)7]8+ cation, the [ZnCl4]2−, [ZnCl3OH]2− and Cl− anions, and the lattice water molecules are linked via hydrogen bonds. |