In the present study the interaction of Fe(II) and Ni(II) with the related expanded quaterpyridines, 1,2-, 1,3-and 1,4-bis-(5¢-methyl-[2,2¢]bipyridinyl-5-ylmethoxy)benzene ligands (4-6 respectively), incorporating flexible, bis-aryl/methylene ether linkages in the bridges between the dipyridyl domains, was shown to predominantly result in the assembly of [M 2 L 3 ] 4+ complexes; although with 4 and 6 there was also evidence for the (minor) formation of the corresponding [M 4 L 6 ] 8+ species. Overall, this result contrasts with the behaviour of the essentially rigid 'parent' quaterpyridine 1 for which only tetrahedral [M 4 L 6 ] 8+ cage species were observed when reacted with various Fe(II) salts. It also contrasts with that observed for 2 and 3 incorporating essentially rigid substituted phenylene and biphenylene bridges between the dipyridyl domains where reaction with Fe(II) and Ni(II) yielded both [M 2 L 3 ] 4+ and [M 4 L 6 ] 8+ complex types, but in this case it was the latter species that was assigned as the thermodynamically favoured product type. The X-ray structures of the triple helicate complexes [