Two-Step Mechanochemical Synthesis of Carbene Complexes of Palladium(II) and Platinum(II)

Abstract

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.

Same or different – that is the question: identification of crystal forms from crystal structure data

“…Indeed P21/c and P21/n are alternative representations of the same symmetry and the reduced unit cell for the two structures are nearly identical (ref code ZAZHAL02 and ZAZHAL01 respectively). 36 Finally, two genuine distinct phases could be described by isometric unit cells as exemplified by the above-mentioned forms of aspirin (ACSALA14 and ACSALA13). Both forms have a P21/c symmetry but the cell dimensions of the latter, a 12.095(7) b 6.491(4) c 11.323(6) β 111.509 (9), convert into those of the first one a 11.2776(2) b 6.5517(1) c 11.2741(2) β 95.837 (1) through the transformation matrix [1 0 1 2 0 −1 0 0 0 −1].…”

A Simple and Efficient Mechanochemical Route for the Synthesis of Salophen Ligands and of the Corresponding Zn, Ni, and Pd Complexes

“…A way to approach the problem can be the use of mechanosynthesis, i.e., the use of mechanical energy to trigger chemical reactions between solids [5,6]. This kind of protocol can be a valid tool for ligand preparation, as well as for the synthesis of the corresponding metal complexes [7,8]. The obvious advantages of using such an approach are the relatively large quantity of starting materials that can be used, the shorter reaction times, and the reduction of side reactions [6,9].…”

Expedient synthesis of NOxy-Heterocyclic Carbenes (NOHC) ligands and metal complexes using mechanochemistry

“…Since the discovery of 1,2-bis(adamantan-1-yl)imidazol-2-ylidene as a stable, crystalline compound, [ 8 , 9 ] the poor reputation about nucleophilic carbenes as laboratory curiosities changed dramatically and nowadays nucleophilic carbenes are recognized as useful substrates with diverse applications in catalysis (metallic and organic), [10][11][12][13] in material science [14] and biology [ 15 , 16 ]. In recent years, it has been shown that the mechanosynthesis of ligands and corresponding NHC complexes offers a very efficient approach to the target compounds ( Scheme 1 ) [17][18][19][20][21][22][23][24][25][26][27][28][29][30] . Various types of NHC ligands could be prepared or employed, together with a wide range of metals such as Ag, Cu, Au, Pt, Ru, Pd, to prepare a new collection of organometallics.…”