Configurational stability is conferred on the complex 1 (R=4-MeOC6H4) by the carefully designed tetradentate bis(1,10-phenanthroline) ligand. The resolution and asymmetric synthesis of 1 were readily achieved by using tris(tetrachlorobenzenediolato)phosphate(V) anions (2) as chiral auxiliaries. The picture shows the separation of the enantiomers of 1 by preparative ion-pair thin-layer chromatography.