Abstract A series of bimetallic lanthanide complexes was prepared from a bimacrocyclic system in which two DO3A units are linked by a m‐xylyl unit appended with either a NO2 or an NH2 group (DO3A=1,4,7,10‐tetraazacyclododecane‐1,4,7‐triacetic acid). The Nd‐, Eu‐, Tb‐ and Yb‐complexes were all luminescent: time‐resolved studies indicated that the lipophilic xylyl group restricts close approach of H2O to the metal centre.