The reaction of di-2-pyridyl ketone with antimony(III) fluoride. Preparation, properties, Mössbauer spectrum and crystal structure of difluoro(methoxydi-2-pyridylmethoxo-NN′O)antimony(III)

Abstract

Di-2-pyridyl ketone (dpk) reacts with SbF₃ in methanol undergoing nucleophilic addition from the solvent. The resultant antimony(III) complex SbF₂[OC(OMe)(NC₅H₄)₂], involving the carbinol form of dpk as a fac-terdentate N,N,O ligand, has been characterized by Mössbauer spectroscopy and single-crystal X-ray analysis. It crystallizes in the orthorhombic system, space group Pnma, with a= 7586(1), b= 14.322(1), c= 11.924(1)Å, and Z= 4. Least-squares refinement based on 710 observed reflections converged to R= 0.036 and R′= 0.033. The co-ordination polyhedron around Sb is a square pyramid [Sb–F 1.967(4), Sb–N 2.580(7), and Sb–O(1) 1.993(8)Å]. The molecule lies on a crystallographic mirror plane.