3-Dimethylaminopropyl chalcogenolate complexes of palladium(II): Syntheses and characterization, including the crystal structures of [Pd(OAc)(ECH2CH2CH2NMe2)]2·H2O (E=S, Se) and [PdCl(TeCH2CH2CH2NMe2)]2
作者:Sandip Dey、Vimal K. Jain、Babu Varghese、Thilo Schurr、Mark Niemeyer、Wolfgang Kaim、Ray J. Butcher
DOI:10.1016/j.ica.2005.09.019
日期:2006.3
The reactions of the sodium salts of 3-dimethylamino-l-propylchalcogenolates, prepared by sodium borohydride reduction of (Me2NCH2CH2CH2E)(2) in methanol, with Na2PdCl4 yielded homoleptic [Pd(ECH2CH2CH2NMe2)(2)](6) (1) (E=S (1a); Se (1b); Te (1c)). When treated with [Pd(OAc)(2)](3) or Na2PdCl4, compounds 1 readily gave binuclear redistribution products [PdX(ECH2CH2CH2NMe2))(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-l-propylchalcogenolate ligands. On pyrolysis, compound 2b affords Pd17Se15. (c) 2005 Elsevier B.V. All rights reserved.