A new macrocyclic compound, [Ni(L)](ClO4)2(1) (L = 1,3,10,12,15,18-hexaazatetracyclo [16,2,1,112.15,04.9]docosane) was synthesized by condensation reactions involving amines and formaldehyde in the present of nickel anion. Compound 1 crystallizes in monoclinic, space groupCc, witha= 13.802(11) Å,b= 12.975(10) Å,c= 13.322(11) Å,α= 90°,β= 99.439(9)°,γ= 90°,V= 2353(3) Å3,Z= 4,F(000) = 1184,Dc= 1.598 Mg/m3,Mr= 566.09,μ= 1.106 mm−1,λ= 0.71073 Å, the finalR= 0.0425 andωR= 0.1235 for 2,030 observed reflections withI>2σ(I). X-ray crystallographic analysis shows simultaneous presence of two conformers of the same macrocyclic compound [Ni(L)]2+in the crystal. [ABSTRACT FROM AUTHOR]