A binucleating ligand, xylylene-bridged biscyclam α,α′-bis(1,4,8,11-tetraazacyclotetradecan-6-yl)- p-xylene ((cyclam) 2- p-xyl) was prepared from α,α′-dichloro- p-xylene, diethylmalonate and 1,4,8,11-tetraazaundecane in three steps. The second step, aminolytic condensation of the tetraamine was critical. The ligand yielded a dinickel(II) complex (Ni 2(cyclam) 2- p-xyl](ClO 4) 4 · 4H 2O. X-ray crystal analysis of the complex disclosed opposite and almost perpendicular occupation of the macrocycles to the bridging benzene ring through equatorial connection at the 6-carbons. Crystal data: tetragonal space group P4 2, a = 15.251(2), c = 9.821(2) A ̊ V = 2284.3(6) A ̊ 3 Z = 2 . It is anticipated that conformational change in solution due to free rotation around the methylene carbon at the junction puts the macrocycles into face-to-face location with NiNi distance of ∼ 7.7 Å.