A series of dinuclear Zn(II), Cu(II) and Ni(II) complexes of two new bis-tripodal ligands with aromatic (H 2 -4a) and aliphatic (H 2 -4b) diamide spacers has been synthesized and structurally characterized. Each of the two tripodal entities of the neutral dinucleating ligands coordinates to one metal ion via three amine functions and a carbonyl oxygen atom of the amide groups. Either trifluoroacetate counterions or solvent molecules complete the trigonal-bipyramidal (Zn, 5a), square-pyramidal (Cu, 6a and 6b), and octahedral (Ni, 7a and 7b) coordination environment at the metal centers. Complexes 5a, 6a, and 7a with the phenylene-bridged diamide ligand are readily deprotonated by potassium tert-butoxide effecting a rearrangement of the dinuclear complexes. In the resulting zinc and copper complexes 8 and 9, one of the metal centers is coordinated by three amine functions of a tripodal subunit and the two amidate nitrogen atoms of the deprotonated ligand 4a 2-while the coordination geometry of