Abstract: The crystal structures of[NiL]I·0.5H₂O (L=12,14-dimethyl-1,4,8,11-tetraazacyclotetradecane-11,13-diene) and[Cu(2,3,2-tet)I₂] [2,3,2-tet=N,N′-bis(2-aminoethyl)-1,3-propanediamine] have been determined by single-crystal X-ray diffraction analysis[NiL]I·0.5H₂O crystallizes in space group Pbca with Z=16, a=1.806 5(6) nm, b=1.801 7(6) nm, c= 1.972 3(7) nm, R=0.042 6, wR=0.085 7. The asymmetric unit consists of two independent[NiL]⁺ cations, two iodide anions and one water molecule. The nickel(Ⅱ) ion is coordinated by four nitrogen atoms of the macrocyclic ligand with the Ni-N bond distances ranging from 0.184 8(6)-0.193 0(6) nm. Crystal data for [Cu(2,3,2-tet)I₂]: space group P2(1)/n, Z=4, a=0.796 4(2) nm, b=1.114 7(2) nm, c=1.644 2(3) nm, β=91.42(3)°, R=0.034 2, wR=0.085 2. The structure consists of [Cu(2,3,2-tet)I₂] monomers with characteristic N₄I₂ donor sets.

Key words: Tetraaza cycle, Coordination compound, Crystal structure, Nickel, Copper