Square-planar tetranuclear clusters [M 4 (L)(AcO) 4 (µ 4 -OH)] -(M = Mn II , Co II , and Ni II ) are synthesized using tetra-anionic p-tert-butylsulfonylcalix [4]arene (L 4-) as a cluster-forming ligand. Three complexes are crystallographically isostructural, being crystallized in the triclinic crystal system with space group P1. The calix[4]arene acts as a tetrakis fac-tridentate ligand through four phenoxo and four sulfonyl oxygen atoms to form square arrangement of four metal ions, which are further bridged by four chelating acetate ions and one hydroxo ion in a µ 4 manner to complete the hexacoordination of each metal center. Although the whole molecule of each complex is crystallographically independent, the molecule is

A coordination polymer [Zn(pyta)(OH)] (pyta = 4-pyridylthioacetate), was synthesized and structurally characterized; it is constructed by an alternating assembly of two types of homo-chiral helices, [Zn-OH] and [Zn-pyta], in which the sulfide moieties are fastened in the latter columns.

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Using p-tert-butylthiacalix[6]arene (H6L) as a clustering ligand, five cluster complexes having CoII5 (2), NiII4 (3) and MIINiII4 (M = CoII (4), MnII (5), and CuII (6)) cores were synthesized. In all the complexes except for 3, a pinched conic L6− acts as a pentanucleating ligand that involves a similar pyramidally arranged cluster core. Each mixed metal complex 4–6 involves four tetragonally arranged NiII ions occupying the basal plane of the pyramid and a MII ion placed at the apex position. In 3, H2L4− is in a cone conformation and the four NiII ions are arranged on the donor surface of H2L4− in a zigzag manner. The mixed metal complexes 4–6 are synthesized by reacting 3 and the appropriate M(AcO)2 in a 1:1 ratio with a novel metal-induced core rearrangement occurring. In this reaction, the insertion of a MII ion at the apex position forces the calixarene to take a cone conformation and the NiII4 array rearranges to form a tetragonal cluster.