A convenient six-step procedure is developed to routinely prepare the hexadentate ligand cis,cis-1,3,5-triaminocyclohexane-N,Nd ' ,N " -tri acetic acid (H(3)tachta) as an HCl salt. Complexes of gallium(III) and indium(III), [Ga(tachta)] and [In(tachta)], are synthesized from the reactions of the ligand and the corresponding metal precursors. Copper(II), palladium(II), and cobalt(II) complexes, [Cu(Htachta)], [Pd(Htachta)], and [Co(Htachta)], are obtained from the reactions of H(3)tachta with the corresponding metal chlorides. The structures of H(3)tachta . 3HCl . 2H(2)O (C12H28C13N3O8) and [Ga(tachta)] (C12H18GaN3O6) are characterized. The crystal of H(3)tachta . 3HCl . 2H(2)O is monoclinic, of the space group P2(1/c), with a = 15.1688 (4) Angstrom, b = 8.4708(2) Angstrom, c = 15.9408(2) Angstrom, P = 108.058(1)degrees, and Z = 4; that of [Ga(tachta)] is cubic, of space group Pa3, with a = 14.0762(1) Angstrom and Z = 8. The gallium atom of [Ga(tachta)] is six-coordinated in the solid state, and the complex assumes a pseudooctahedronal geometry with the completely deprotonated hexadentate ligand encapsulating the metal ion.