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Synthesis and multinuclear NMR study of Hg(II), Cd(II), and Pd(II) complexes with biphenylmethylenetriphenylphosphorane: X-ray crystal structure of \C6H5C6H4CO\(C6H5)(3)P\CH\HgI2(2)

, , and . JOURNAL OF COORDINATION CHEMISTRY, 63 (7): 1165-1175 (2010)
DOI: {10.1080/00958971003728320}

Abstract

Reactions of title ylide, \(C6H5)(3)PCHCOC6H4C6H5)\ (BPPPY), with mercury(II) halides in equimolar ratios in methanol yielded dinuclear complexes (BPPPY)HgCl2(2) (1), (BPPPY) HgBr2(2) (2), and (BPPPY)HgI2(2) (3). Reactions of BPPPY with CdCl2 in equimolar ratios gave (BPPPY)CdCl2(2) (4). Reaction of PdCl2 with BPPPY (1/2) in acetonitrile at room temperature gave cis/trans PdCl2\CH(PPh3)COC6H4C6H5\(2) (5). The same reaction at reflux gave the orthopalladated complex Pd\CH\P(2-C6H4)Ph\(COC6H4C6H5)\(mu-Cl)(2) (6) along with the phosphonium salt Ph3PCHCOC6H4C6H5Br. The compounds were characterized by elemental analysis, IR-, H-1-, C-13-, and P-31-NMR spectroscopy. Single crystal X-ray analysis of 3 reveals the centrosymmetric dimeric structure containing the ylide and HgI2. Crystallographic data for 3 are: crystal system, monoclinic; space group, P 2(1)/n, a = 15.7744(7), b = 23.0288(9), c = 20.2867(9) angstrom, beta = 112.237(3)degrees, V = 6821.4(5) angstrom(3), and Z = 1.

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