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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
Author(s) -
Daran Jean-Claude,
Gimeno Nicolas,
Gouygou Maryse,
Volkman Jérôme
Publication year - 2019
Publication title -
acta crystallographica section c
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.304
H-Index - 17
ISSN - 2053-2296
DOI - 10.1107/s2053229619004212
Subject(s) - palladium , chemistry , acetonitrile , supramolecular chemistry , molecule , crystal structure , ligand (biochemistry) , crystallography , intramolecular force , benzene , diethyl ether , coordination complex , stereochemistry , medicinal chemistry , metal , organic chemistry , biochemistry , receptor , catalysis
The self‐assembly of ditopic bis(1 H ‐imidazol‐1‐yl)benzene ligands ( L H ) and the complex (2,2′‐bipyridyl‐κ 2 N , N ′)bis(nitrato‐κ O )palladium(II) affords the supramolecular coordination complex tris[μ‐bis(1 H ‐imidazol‐1‐yl)benzene‐κ 2 N 3 : N 3′ ]‐ triangulo ‐tris[(2,2′‐bipyridyl‐κ 2 N , N ′)palladium(II)] hexakis(hexafluoridophosphate) acetonitrile heptasolvate, [Pd 3 (C 10 H 8 N 2 ) 3 (C 12 H 10 N 4 ) 3 ](PF 6 ) 6 ·7CH 3 CN, 2 . The structure of 2 was characterized in acetonitrile‐ d 3 by 1 H/ 13 C 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 PF 6 − 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 L H 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 ‐ L H and syn / anti ‐[Pd] are a priori possible and expected to be in rapid equilibrium.