A triangular palladium(II) supramolecular coordination complex based on 1,4-bis(1 H -imidazol-1-yl)benzene and (2,2′-bipyridyl)palladium(II) nitrate: synthesis and crystal structure - Archive ouverte HAL Accéder directement au contenu
Article Dans Une Revue Acta Crystallographica Section C : Structural Chemistry [2014-...] Année : 2019

A triangular palladium(II) supramolecular coordination complex based on 1,4-bis(1 H -imidazol-1-yl)benzene and (2,2′-bipyridyl)palladium(II) nitrate: synthesis and crystal structure

Résumé

The self-assembly of ditopic bis(1H-imidazol-1-yl)benzene ligands (LH) and the complex (2,2'-bipyridyl-[kappa]2N,N')bis(nitrato-[kappa]O)palladium(II) affords the supramolecular coordination complex tris[[mu]-bis(1H-imidazol-1-yl)benzene-[kappa]2N3:N3']-triangulo-tris[(2,2'-bipyridyl-[kappa]2N,N')palladium(II)] hexakis(hexafluoridophosphate) acetonitrile heptasolvate, [Pd3(C10H8N2)3(C12H10N4)3](PF6)6.7CH3CN, 2. The structure of 2 was characterized in acetonitrile-d3 by 1H/13C NMR spectroscopy and a DOSY experiment. The trimeric nature of supramolecular coordination complex 2 in solution was ascertained by cold spray ionization mass spectrometry (CSI-MS) and confirmed in the solid state by X-ray structure analysis. The asymmetric unit of 2 comprises the trimetallic Pd complex, six PF6- counter-ions and seven acetonitrile solvent molecules. Moreover, there is one cavity within the unit cell which could contain diethyl ether solvent molecules, as suggested by the crystallization process. The packing is stabilized by weak inter- and intramolecular C-H...N and C-H...F interactions. Interestingly, the crystal structure displays two distinct conformations for the LH ligand (i.e. syn and anti), with an all-syn-[Pd] coordination mode. This result is in contrast to the solution behaviour, where multiple structures with syn/anti-LH and syn/anti-[Pd] are a priori possible and expected to be in rapid equilibrium.
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hal-02332780 , version 1 (25-10-2019)

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Jean-Claude Daran, Nicolas Gimeno, Maryse Gouygou, Jérôme Volkman. A triangular palladium(II) supramolecular coordination complex based on 1,4-bis(1 H -imidazol-1-yl)benzene and (2,2′-bipyridyl)palladium(II) nitrate: synthesis and crystal structure. Acta Crystallographica Section C : Structural Chemistry [2014-..], 2019, 75 (5), pp.523-528. ⟨10.1107/S2053229619004212⟩. ⟨hal-02332780⟩
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