Allylpalladium (II) complexes with dichalcogenoimidodiphosphinate ligands: Synthesis, structure, spectroscopy and their transformation into palladium chalcogenides |
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Authors: | A Singhal DP Dutta SM Mobin |
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Institution: | a Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400 085, India b National Single-crystal X-ray Diffractometer Facility, Indian Institute of Technology, Powai, Mumbai 400 076, India c Department of Chemistry, Indian Institute of Technology, Powai, Mumbai 400 076, India |
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Abstract: | The synthesis, characterization and thermal behavior of new monomeric allylpalladium (II) complexes with dichalcogenoamidodiphosphinate anions are reported. The complexes R = H, R′ = Pri, E = S (1a); R = H, R′ = Pri, E = Se (1b); R = H, R′ = Ph, E = S (1c); R = H, R′ = Ph, E = Se (1d); R = Me, R′ = Pri, E = S (2a); R = Me, R′ = Pri, E = Se (2b); R = Me, R′ = Ph, E = S (2c); R = Me, R′ = Ph, E = Se (2d)] have been prepared by room temperature reaction of Pd(η3-CH2C(R)CH2)(acac)] (acac = acetylacetonate) with dichalcogenoimidodiphosphinic acids in acetonitrile solution. The complexes have been characterized by multinuclear NMR (1H, 13C{1H}, 31P{1H}, 77Se{1H}), FT-IR and elemental analyses. The crystal structures of complexes 1a, 1d and 2d have been reported and they consist of a six-membered PdE2P2N ring (E = S for 1a and Se for 1d and 2d) and an allyl group, C3H4R(R = H for 1a and 1d and Me for 2d). Thermogravimetric studies have been carried out for few representative complexes. The complexes thermally decompose in argon atmosphere to leave a residue of palladium chalcogenides, which have been characterized by PXRD, SEM and EDS. |
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Keywords: | η3-Allylpalladium complexes Dichalcogenoamidodiphosphinate ligands Multinuclear NMR spectroscopy X-ray crystal structure Thermogravimetric studies Scanning electron microscopy |
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