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The reactions of methyl(2-pyridyl)ketone oxime, (py)C(Me)NOH, with zinc chloride have been investigated. An excess of the ligand in EtOH/MeCN affords the mononuclear complex [ZnCl 2 {(py)C(Me)NOH} 2 ] (1) in moderate yield. The metal ion is coordinated by two chloro ligands and two N,N′- chelating (py)C(Me)NOH molecules. The six-coordinate molecule is the ciscis- trans isomer considering the positions of the coordinated chlorine, pyridyl and oxime nitrogen atoms, respectively. The reaction between equimolar quantities of ZnCl 2 , (py)C(Me)NOH and LiOH·H 2 O in EtOH/MeCN leads to the tetranuclear cluster [Zn 4 (OH) 2 Cl 2 {(py)C(Me)NO} 4 ] (2) in high yield. The molecule lies on a crystallographic inversion center and has an inverse 12-metallacrown- 4 topology. Two triply bridging hydroxides are accommodated within the metallacrown ring. Each (py)C(Me)NO− ligand adopts the 2.111 coordination mode (Harris notation), chelating one ZnII ion and bridging a Zn II  2 pair. Two metal ions are in a distorted O 2 N 4  octahedral environment, whereas the other two are in a severely distorted tetrahedral O 3 Cl environment. Complex 2 joins a small family of structurally characterized zinc(II) metallacrown complexes. The IR data are discussed in terms of the nature of bonding and the structures of the two complexes.

Investigation of the Zinc Chloride / Methyl(2-pyridyl)ketone Oxime Reaction System: A Mononuclear Complex and an Inverse 12-Metallacrown-4 Cluster