| Abstract: | The reactions of dl‐proline with chiral macrocyclic NiII complex Ni(SS‐L)](ClO4)2 in acetonitrile/water gave a six‐coordinate enantiomer formulated as Ni(SS‐L)(l‐Pro)](ClO4)2 · H2O ( 1 ). Another enantiomer of Ni(RR‐L)(d‐Pro)](ClO4)2 · H2O ( 2 ) was obtained when Ni(RR‐L)](ClO4)2 was used (L = 5,5,7,12,12,14‐hexamethyl‐1,4,8,11‐tetraazacyclotetradecane, Pro = proline). Single‐crystal X‐ray diffraction analyses of complexes 1 and 2 revealed that the NiII atom has a distorted octahedral coordination arrangement, being coordinated by four nitrogen atoms of L in a folded configuration, plus two carboxylate oxygen atoms of proline in mutually cis positions. Complexes 1 and 2 are supramolecular stereoisomers, which are constructed with hydrogen bonding linking of Ni(SS‐L)(l‐Pro)]2+ and Ni(RR‐L)(d‐Pro)]2+ monomers to form one‐dimensional zigzag chains. The homochiral natures of complexes 1 and 2 were confirmed by solid CD spectroscopy. |
