3-Dimethylaminopropyl chalcogenolate complexes of palladium(II): Syntheses and characterization, including the crystal structures of [Pd(OAc)(ECH 2CH 2CH 2NMe 2)] 2 · H 2O (E = S, Se) and [PdCl(TeCH 2CH 2CH 2NMe 2)] 2

Abstract

The reactions of the sodium salts of 3-dimethylamino-1-propylchalcogenolates, prepared by sodium borohydride reduction of (Me 2NCH 2CH 2CH 2E) 2 in methanol, with Na 2PdCl 4 yielded homoleptic [Pd(ECH 2CH 2CH 2NMe 2) 2] 6 ( 1) (E = S ( 1a); Se ( 1b); Te ( 1c)). When treated with [Pd(OAc) 2] 3 or Na 2PdCl 4, compounds 1 readily gave binuclear redistribution products [PdX(ECH 2CH 2CH 2NMe 2)] 2 where X = OAc ( 2) (E = S ( 2a); Se ( 2b); or Cl ( 3)) (E = S ( 3a); Se ( 3b); Te ( 3c)), respectively. The terminal acetate/chloride ligands in 2b/ 3b can be substituted by other ionic ligands like PhSe −. The complexes were characterized by elemental analysis, UV–Vis, IR and NMR spectroscopy. The structures of 2a, 2b and 3c were established by X-ray crystallography. Each molecule has a dimeric structure in which there are two chalcogenolate bridges from the chelating 3-dimethylamino-1-propylchalcogenolate ligands. On pyrolysis, compound 2b affords Pd 17Se 15.