Novel cyclopalladated ferrocenyl Schiff base compounds with bridging and chelating diphosphines. Crystal and molecular structure of [{Pd[(η 5-C 5H 5)Fe(η 5-C 5H 3)C(H)N-2,4,6-Me 3C 6H 2]}{Ph 2P(CH 2) nPPh 2 P, P}][PF 6] ( n=1, 2)

• Published in: Journal of organometallic chemistry 2001-12, Vol.637, p.577-585
• Main Authors: Vila, José M, Gayoso, Eduardo, Pereira, Teresa, Mariño, Marta, Martı́nez, Javier, Fernández, Jesús J, Fernández, Alberto, López-Torres, Margarita
• Format: Article
• Language: English
• Subjects: Cyclometallation; Imine; Palladium
• ISSN: 0022-328X; 1872-8561
• DOI: 10.1016/S0022-328X(01)00976-7

The reaction of the ferrocenylimine (η 5-C 5H 5)Fe(η 5-C 5H 4)C(H)NR (R=2,4,6-Me 3C 6H 2) ( a), with Pd(AcO) 2 or with Li 2[PdCl 4] leads to the heterotetrametallic compounds [Pd{(η 5-C 5H 5)Fe(η 5-C 5H 3)C(H)NR}(μ-O 2CMe)] 2 ( 1) and [Pd{(η 5-C 5H 5)Fe(η 5-C 5H 3)C(H)NR}(μ-Cl)] 2 ( 2), respectively. Compound 2 may also be obtained by treatment of 1 with aqueous sodium chloride. Compound 2 reacts with tertiary diphosphines in 1:1 or 1:2 molar ratio to give [{Pd[(η 5-C 5H 5)Fe(η 5-C 5H 3)C(H)NR]Cl} 2{μ-Ph 2P(CH 2) n PPh 2}] ( n=1, 3; n=2, 4; n=3, 5; n=4, 6), [{Pd[(η 5-C 5H 5)Fe(η 5-C 5H 3)C(H)NR]Cl} 2(μ-Ph 2PC 5H 4FeC 5H 4PPh 2)] ( 7), and [Pd{(η 5-C 5H 5)Fe(η 5-C 5H 3)C(H)NR}{Ph 2P(CH 2) n PPh 2 P, P}][PF 6] ( n=1, 8; n=2, 9; n=3, 10; n=4, 11), [Pd{(η 5-C 5H 5)Fe(η 5-C 5H 3)C(H)NR}(Ph 2PC 5H 4FeC 5H 4PPh 2 P, P)][PF 6] ( 12), respectively. The crystal structures of compounds 8 and 9 have been determined by X-ray crystallography. New cyclopalladated ferrocenylimine compounds with bridging and chelating diphosphines are synthesized and full spectroscopic data given. The first crystal structures of two such compounds [{Pd[(η 5-C 5H 5)Fe(η 5-C 5H 3)C(H)N-2,4,6-Me 3C 6H 2]}{Ph 2P(CH 2) n PPh 2 P, P}][PF 6] ( n=1, 2) are also reported.