The 12-, 13-and 14-membered tetraphenyl substituted maerocycles Ph4[12JTIM (2,3,8,4,7,3,7,, Ph4[13]TIM (2,3,8,9-tetraphenyl-1,4,7,10-tetra-azacyclotrideca-1,3,7,9-tetraene) and Ph4[14]TIM (2,3,9,10-tetraphenyl-l,4,8,1 ltctradeca-l,3,8,10-tetraene) were prepared and their copper(II) complexes characterised. Magnetic and spectroscopic measurements (i.r. and u.v.-vis.) are discussed. A variety of macrocyclic precursers (KIM = 1,2,8,9-tetraphenyl-3,7-diaza-2,7-dione) and KIM-dioxime were also prepared and characterised.