Reaction of (bpy)Pd(PF 6 ) 2 (bpy=2,2′-bipyridine) with new tridentate ligand 1,3,5-tris(nicotinoyloxyethyl)cyanurate (L) followed by slow evaporation of solvents allows to form amorphous microspheres consisting of [(bpy)Pd(L)] 2 (PF 6 ) 4 without any template or additive. Recrystallization of amorphous microspheres yields, after three weeks, single crystals consisting of [(bpy) 3 Pd 3 (μ 3 -HPO 4 )(L)](PF 3 (OH) 3 )·3F. Formation of the crystalline product can be induced from the decomposition of the PF 6 − anions. Alternatively, direct reactions of (bpy)Pd(PF 6 ) 2 with L in the presence of Na 2 HPO 4 or Na 2 HAsO 4 under reflux conditions produce the same single crystals in the form of cage molecules, [(bpy) 3 Pd 3 (μ 3 -HPO 4 )(L)](PF 3 (OH) 3 )·3F and [(bpy) 3 Pd 3 (μ 3 -HAsO 4 )(L)](PF 3 (OH) 3 )·3F, respectively.