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We report on the synthesis, structure, and physicochemical characterization of the first three examples of neutral palladium‐oxo clusters (POCs). The 16‐palladium(II)‐oxo cluster [Pd 16 O 24 (OH) 8 ((CH 3 ) 2 As) 8 ] ( Pd 16  ) comprises a cyclic palladium‐oxo unit capped by eight dimethylarsinate groups. The chloro‐derivative [Pd 16 Na 2 O 26 (OH) 3  Cl 3  ((CH 3 ) 2  As) 8 ] ( Pd 16 Cl ) was also prepared, which forms a highly stable 3D supramolecular lattice via strong intermolecular interactions. The 24‐palladium(II)‐oxo cluster [Pd 24 O 44 (OH) 8 ((CH 3 ) 2 As) 16 ] ( Pd 24  ) can be considered as a bicapped derivative of  Pd 16   with a tetra‐palladium‐oxo unit grafted on either side. The three compounds were fully characterized 1) in the solid state by single‐crystal and powder XRD, IR, TGA, and solid‐state  1 H and  13 C NMR spectroscopy, 2) in solution by  1 H,  13 C NMR and  1 H DOSY spectroscopic methods, and 3) in the gas phase by electrospray ionization mass spectrometry (ESI‐MS).

Discovery and Supramolecular Interactions of Neutral Palladium‐Oxo Clusters Pd 16 and Pd 24