Abstract
Treatment of the thiosemicarbazones 2-ClC 6H 4C(Me) NN(H)C( S)NHR, (R: Me, a; Et, b) and 2-BrC 6H 4C(Me) NN(H)C( S)NHR (R: Me, c; Et, d) with lithium tetrachloropalladate(II) in methanol or palladium(II) acetate in acetic acid gave the tetranuclear cyclometallated complexes [Pd{2-XC 6H 3C(Me) NN C(S)NHR}] 4 (X/R: Cl/Me, 1a; Cl/Et, 1b; Br/Me, 1c; Br/Et, 1d). Reaction of 1a– 1d with bis(diphenylphosphino)methane, Ph 2PCH 2PPh 2, in a 1:4 molar ratio and concentrated hydrochloric acid gave the mononuclear complexes [Pd{2-XC 6H 3C(Me) NN(H)–C( S)NHR}(Ph 2PCH 2PPh 2-P,P)](Cl) ( 2a– 2d). Reaction of 1a– 1d with bis(diphenylphosphino)methane, Ph 2PCH 2PPh 2, in 1:2 and 1:4 molar ratios gave the dinuclear or mononuclear complexes [{Pd[2-XC 6H 3C(Me) NN C(S)NHR]} 2(μ-Ph 2PCH 2PPh 2)] ( 3a– 3d), and [Pd{2-XC 6H 3C(Me) NN C(S)NHR}(Ph 2PCH 2PPh 2-P)] ( 4a– 4d), with bridging and chelating diphosphine, respectively. The molecular structures of complexes 1b, 1d, 4c and 4d have been determined by X-ray diffraction analysis.
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