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A new 14-membered hexazamacrocyclic copper(II) complex [Cu(H2L1)](ClO4)4(L1=1,8-bis(2-aminoethyl)-1,3,6,8,10,13-hexaazacyclotetradecane) has been prepared by the one-pot reaction of ethylenediamine and formaldehyde in the presence of the Cu(II) ion. The crystal structure of [Cu(H2L1)](ClO4)4 was determined by X-ray diffraction. It crystallizes in the triclinic space group P−1 with a=12.118(2) A˚, b=12.438(2) A˚, c=12.466(2) A˚, α=102.26(1)°, β=112.82(1)°, γ=111.51(1)°, and Z=2. The coordination geometry around the copper(II) ions is axially elongated octahedral with four nitrogen atoms of the macrocycle [Cu–N 2.012(7) A˚ for Cu(1) and 2.013(6) A˚ for Cu(2), average value] and two oxygen atoms of two ClO4− anions [Cu–O=2.550 A˚ for Cu(1) and 2.601(6) A˚ for Cu(2)]. [CuL2](ClO4)2(L2=3,7-bis(2-aminoethyl)-1,3,5,7-tetraazabicyclo[3,3,2]decane) with a novel tetraazabicyclic ligand was obtained from the same reaction system as an additional product. Crystal structure of [CuL2](ClO4)2: monoclinic space group Cc, a=16.393(3) A˚, b=8.8640(18) A˚, c= 13.085(3) A˚, β=105.01(3)°, and Z=4. [Copyright &y& Elsevier]