Synthesis and characterization of cyclometallated complexes of benzalazines. Crystal and molecular structure of [{Pd(p-ClC6H3CHN–)Cl(PEt3)2}2]
- 1 January 1983
- journal article
- research article
- Published by Royal Society of Chemistry (RSC) in J. Chem. Soc., Dalton Trans.
- No. 11,p. 2441-2446
- https://doi.org/10.1039/dt9830002441
Abstract
The reaction of benzalazines, (p-RC6H4CHN–)2(R = H, Cl, NO2, or NMe2), with PdCl2 leads in the the first two cases to the formation of cyclometallated polymeric species that react with phosphines to yield dimetallated compounds [{Pd(p-RC6H3CHN–)Cl(PR′3)2}2](R′= Et or Ph) and/or [{[graphic omitted]–)Cl(PPh3)}2]. Phosphine exchange reactions give the complex [{Pd(p-RC6H3CHN–)Cl(PEt3)(PPh3)}2]. The molecular structure of [{Pd(p-ClC6H3CHN–)Cl(PEt3)2}2] has been determined by a single-crystal X-ray analysis. The crystals are monoclinic, space group P21/n, a= 11.124(3), b= 10.062(2), c= 22.566(5)Å, β= 102.95(3)°, and Z= 2; R= 0.052 for 3 306 reflections. Palladium atoms are five-co-ordinated, the Pd–N distance being 2.743 Å. However, n.m.r. spectra show that, in solution, free rotation around the C(aromatic)–C(azomethine) bonds does occur even at –100 °C.Keywords
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