Crystal structure of µI, µII, µIII-tris(dithioacetato)-µ3-trithio-orthoacetato-triangulo-trinickel(II) in two crystalline forms

Abstract

The title compound crystallizes in two orthorhombic forms: form (I) with a= 8.999(5), b= 14.311(5), c= 14.116(5)Å, and form (II) with a= 7.562(10), b= 17.283(10), c= 14.130(10)Å, both in space group Pna2₁. The complex units in the two structures are similar, and consist of a trigonal pyramid-like molecule, which is an example of a transition-metal cluster. The structures were solved from X-ray data by the heavy-atom technique and refined by least squares to R 0.063 (I) and 0.077 (II) for 1 041 and 1 076, respectively, visually estimated independent reflections. Three nickel atoms (forming a regular triangle with presumably non-bonded Ni ⋯ Ni 3.0 Å), and two different kinds of ligands [three molecules of the dithioacetate ligand and one of the sulphur-substituted ortho-form of acetic acid (MeCS₃^3–)] are present. The co-ordination of the nickel atoms is essentially square planar: two have short distances (3.2 Å) to sulphur atoms of neighbouring molecules, to give a one-dimensional polymeric system.