Reactions of title ylide, {(C 6 H 5 ) 3 PCHCOC 6 H 4 C 6 H 5 )} (BPPPY), with mercury(II) halides in equimolar ratios in methanol yielded dinuclear complexes [(BPPPY)HgCl 2 ] 2 (1), [(BPPPY) HgBr 2 ] 2 (2), and [(BPPPY)HgI 2 ] 2 (3). Reactions of BPPPY with CdCl 2 in equimolar ratios gave [(BPPPY)CdCl 2 ] 2 (4). Reaction of PdCl 2 with BPPPY (1/2) in acetonitrile at room temperature gave cis/trans [PdCl 2 {CH(PPh 3 )COC 6 H 4 C 6 H 5 } 2 ] (5). The same reaction at reflux gave the orthopalladated complex [Pd{CH{P(2-C 6 H 4 )Ph}(COC 6 H 4 C 6 H 5 )}(-Cl)] 2 (6) along with the phosphonium salt [Ph 3 PCHCOC 6 H 4 C 6 H 5 ]Br. The compounds were characterized by elemental analysis, IR-, 1 H-, 13 C-, and 31 P-NMR spectroscopy. Single crystal X-ray analysis of 3 reveals the centrosymmetric dimeric structure containing the ylide and HgI 2 . Crystallographic data for 3 are: crystal system, monoclinic; space group, P 2 1 /n, a ¼ 15.7744(7), b ¼ 23.0288(9), c ¼ 20.2867(9) Å , ¼ 112.237(3) , V ¼ 6821.4(5) Å 3 , and Z ¼ 1.