Novel Cyclometallated Complexes Derived From a Halogenated Thiosemicarbazone. Crystal and Molecular Structures of 2-FC6H4C(Me)=NN(H)C(=S)NHPh and[(Pd{2-FC6H3C(Me)=NN=C(S)NHPh})2(μ-PPh2(CH2)2PPh2)]

• Published in: Zeitschrift für anorganische und allgemeine Chemie (1950) Vol. 631; no. 11; pp. 2204 - 2209
• Main Authors: Adrio, Luis A., Amoedo, Adriana, Antelo, José M., Fernández, Jesús J., Martínez, Javier, Ortigueira, Juan M., Pereira, M. Teresa, Vila, José M.
• Format: Journal Article
• Language: English
• Published: Weinheim WILEY-VCH Verlag 01.08.2005; WILEY‐VCH Verlag
• Subjects: C-H activation; Cyclometallation; Palladium; Thiosemicarbazones
• ISSN: 0044-2313; 1521-3749
• DOI: 10.1002/zaac.200570044

Treatment of the thiosemicarbazone 2‐FC6H4C(Me)=NN(H)C(=S)NHPh, a, with palladium(II) acetate in acetic acid, or with lithium tetrachloropalladate(II) in methanol, gave the tetranuclear cyclometallated complex [Pd{2‐FC6H3C(Me)=NN=C(S)NHPh}]4 (1a). Reaction of 1a with the diphosphines Ph2P(CH2)2PPh2 (dppe), Ph2PCH=CHPPh2 (trans‐dpe) Ph2P(CH2)3Ph2 (dppp) or Ph2P(CH2)4Ph2 (dppb) in a 1:2 molar ratio gave the dinuclear cyclometallated complexes [(Pd{2‐FC6H3C(Me)=NN=C(S)NHPh})2(μ‐Ph2P(CH2)nPPh2)], (n = 2, 2a; 3, 4a; 4, 5a) and [(Pd{2‐FC6H3C(Me)=NN=C(S)NHPh})2(μ‐Ph2PCH=CHPPh2)], (3a). The X‐ray crystal structure of ligand a and of complex 2a are described. The structure of complex 2a shows the palladium atom is bonded to four different donor atoms: C, N, S and P.