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A neutral four-coordinate CuIIN3O complex with Shiff base ligand, product of template assembling of two S-methylisothiosemicarbazide units with benzoylacetone and nitromalondialdehyde, was synthesized by two steps procedure via CuIIN2O2 chelate precursor and was fully characterized by elemental analysis, IR, UV–Vis, ESR spectra and magnetochemistry. X-ray analysis confirms its structural assignment. The assembling ligand assumes an acyclic structure of ‘4+1’ type where a non-bonding interaction between the metal and the amino group of one S-methylisothiosemicarbazide unit takes place.

Synthesis, structure and physico-chemical investigation of four new nickel(II) complexes with [N 3 O] chelate tetradentate ligands are described. They were obtained by template condensation of mono-S-methylisothiosemicarbazone of acetylacetone or 1-phenyl-butane1,3-dione with bifunctional carbonyl compounds such as anthranil aldehyde or 4-amino-3-penten-2-one. Square–planar complexes were obtained as only products with good yield and were fully characterised by EI MS, NMR ( 1 H, 13 C) spectroscopy, elemental analysis, and, in the case of three complexes, by X-ray investigation. A Cambridge Structural Database surveys on related square–planar Ni(II) complexes was also included, showing a small but significant correlation between NiO distances and ONiN angles.