The two-step mechanochemical preparation of carbene-pyridine complexes of palladium and platinum is reported. The organometallic products, which represent a class of commercially available catalysts, are rapidly formed in excellent yield proving solvent-free synthesis to be a viable synthetic alternative even in the case of NHC-containing compounds.
A mechanochemical
strategy for the synthesis of N-heterocyclic carbene
complexes is described, in which 1,3-dibenzylimidazole
complexes of palladium and platinum are produced in a two-step process
by grinding together the reactants with a mortar and pestle. Crystallographic
characterization reveals that unlike the solution syntheses, which
produce a mixture of products, the solid-state reactions occur under
topochemical conditions affording isomerically and polymorphically
pure products.
In the title compound (C17H17N2)2[Fe2Cl6O], obtained from the solid-state reaction of FeCl2 and N,N′-dibenzylimidazolium chloride, the complex anion has approximate D
3d symmetry with crystallographically imposed inversion symmetry coincident with the bridging μ-O atom. The stereochemistry about each FeCl3O centre is distorted tetrahedral [Fe—Cl = 2.2176 (5)–2.2427 (5) Å and Fe—O = 1.7545 (2) Å]. The Cl atoms are involved in weak anion–cation C—H⋯Cl interactions, giving a network structure.
In the title compound, [Cu(C7H3NO4)(C6H6N2O)(H2O)], the coordination geometry of the CuII atom can be described as distorted square pyramidal. The basal plane is defined by one N atom and two O atoms from the deprotonated pyridine-2,6-dicarboxylate ligand, and a pyridyl N atom from the 4-pyridyl aldoxime ligand. The apical position is occupied by a water molecule. O—H⋯O hydrogen bonds lead to the formation of a two-dimensional network.
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