Direct Electrochemical Synthesis and Crystal Structure of Copper(I) Complex with 2′‐hydroxy‐5′‐methyl‐acetophenone and Triphenylphosphine Ligands

Abstract

A new complex of Cu with 2′‐hydroxy‐5′‐methyl‐acetophenone (HMAP) and triphenylphosphine (PPh3) was prepared by the electrochemical oxidation of Cu in acetonitrile solutions. The final product, (MAP)Cu(PPh3)2, was crystallized from bulk solution and characterized by microanalysis, IR, Raman, 1H NMR together with x‐ray crystallographic determinations. The results showed that the complex was a chelate structure in which Cu(I) ion was coordinated with two oxygen atoms of the deprotonated ligand of MAP anion to form a six member ring, and two PPh3 molecules participated in the coordination. The parameters of the complex were monoclinic, space group of P21/n, a=9.048(2) Å, b=26.405(6) Å, c=15.606(4) Å, β=95.990(5)°, Z=4, R=0.057 for 8428 unique reflections. The details of synthesis, reaction mechanism on the electrode and the effect of PPh3 on the coordinating processes are discussed.