Paul, S.; Lohmiller, T.; Barrera, J.; Herwig, C.; Cula, B.; Quensel, A.; Limberg, C.: A Doubly Reduced Dipalladium Dibenzylideneacetone Complex. Organometallics 42 (2023), p. 3434–3437
10.1021/acs.organomet.3c00401
Abstract:
Xanthene diiodide reacts with Pd2(dba)3 in the presence of TMEDA via a double insertion of Pd into the C–I bonds, yielding the complex [XanPd2(TMEDA)2I2] (1). Treatment of 1 with potassium naphthalenide in the presence of dba and 18C6 led to [Pd2(dba)2{K(18C6)}2] (2), where two reduced dba ligands span two Pd atoms via olefinic functions. The complex, which can also be readily generated from Pd2(dba)3 through reduction, crystallizes as a dimer composed by the interaction of two neighboring [K(18C6)]+ units with each other, while the second pair of cations coordinate an additional THF molecule each. The electronic structure of 2 was elucidated by SQUID measurements and DFT calculations.