220171-80-2Relevant articles and documents
Synthesis and conformational studies of palladium(II) complexes containing [Ph2P(O)NP(E)Ph2]- (E=S or Se)
Slawin, Alexandra M. Z.,Smith, Martin B.,Woollins, J. Derek
, p. 4465 - 4473 (2008/10/09)
The ligands [Ph2P(O)NP(E)Ph2]- (E=S I; E=Se II) can readily be complexed to a range of palladium(II) starting materials affording new six-membered Pd-O-P-N-P-E palladacycles. Hence ligand substitution reaction of the chloride complexes [PdCl2(bipy)] (bipy=2,2′-bipyridine), [{Pd(μ-Cl)(L-L)}2] (HL-L=C9H13N or C12H13N), [{Pd(μ-Cl)Cl(PMe2Ph)}2] or [PdCl2(PR3)2] [PR3=PPh3; 2PR3=Ph2PCH2CH2PPh2 or cis-Ph2PCH=CHPPh2] with either I (or II) in thf or CH3OH gave [Pd{Ph2P(O)NP(E)Ph2-O,E}(bipy)]PF6, [Pd{Ph2P(O)NP(E)Ph2-O,E}(L-L)], [Pd{Ph2P(O)NP(E)Ph2-O,E}Cl(PMe2Ph)] or [Pd{Ph2P(O)NP(E)Ph2-O,E} (PR3)2]PF6 in good yields. All compounds described have been characterised by a combination of multinuclear NMR [31 P{1 H} and 1 H] and IR spectroscopy and microanalysis. The molecular structures of five complexes containing the selenium ligand II have been determined by single-crystal X-ray crystallography. Three different ring conformations were observed, a pseudo-butterfly, hinge and in the case of all three PR3 complexes, pseudo-boat conformations. Within the Pd-O-P-N-P-Se rings there is evidence for π-electron delocalisation.