Publication date: 1 October 2017
Source:Journal of Organometallic Chemistry, Volume 846
Author(s): Petr Štěpnička, Martin Zábranský, Ivana Císařová
Two phosphinoferrocene carboxylic acids differing in the two-carbon spacer separating the phosphinoferrocene moiety and the carboxyl group, Ph2PfcCH=CHCO2H (1a) and Ph2PfcCH2CH2CO2H (1b; fc = ferrocene-1,1′-diyl), were prepared from aldehyde Ph2PfcCHO by Horner-Wadsworth-Emmons olefination, reduction and hydrolysis. These acids reacted with [(L
NC)Pd(acac)] (L
NC = 2-[(dimethylamino-κN)methyl]phenyl-κC
1, acac = pentane-2,5-dionate) under protonation and elimination of the Pd-bound acetylacetonate ligand to afford the respective phosphinocarboxylate complexes, namely, the P,O-bridged dimer [(L
NC)Pd{μ(P,O)-Ph2PfcCH=CHCO2}]2 (6a) and the coordination polymer [(L
NC)Pd{μ(P,O)-Ph2PfcCH2CH2CO2}] n (6a). The crystal structures of P-sulfides prepared from acids 1a and 1b, compounds Ph2P(S)fcCH=CH2CO2H and Ph2P(S)fcCH2CH2CO2H, and the phosphinocarboxylate complexes 6a and 6b (in solvated form) were determined by single-crystal X-ray diffraction analysis.
Graphical abstract