Akademik Veri Yönetim Sistemi
JOURNAL OF MOLECULAR STRUCTURE, cilt.1336, 2025 (SCI-Expanded)
This study aims to optimize the synthesis process of a nickel (II) dicationic precatalyst supported by alpha-iminopyridine ligands (ImPy) to improve yield and efficiency. A Taguchi optimization approach was used to systematically evaluate and optimize key factors-reaction time, temperature, and stirring speed-in the synthesis of bis(alpha-iminopyridine)diaquanickel (II) complex. The synthetic procedure involves the oxidative addition of methoxyphosphonium salts with non-coordinating anions, and an orthogonal Taguchi design was employed to determine the optimal conditions. The optimal synthesis conditions were identified as a reaction time of 3 h, a temperature of 0 degrees C, and a stirring speed of 350 rpm, resulting in a 90% yield. The synthesized dicationic nickel (II) complexes with aryl-ortho substituted bis(alpha-iminopyridine) ligands were thoroughly characterized by FTIR, UV-Vis, and NMR spectroscopy. Single crystals of [Ni(H2O)2(Me)2ImPy(Me)][(PF6)2] were successfully grown by antisolvent crystallization and analyzed by single-crystal X-ray diffraction, revealing a monoclinic structure with space group P21/n and specific lattice parameters. The Taguchi optimization method effectively improved the yield of the nickel (II) dicationic precatalyst synthesis. The characterization confirmed the paramagnetic octahedral nickel (II) nature and provided insights into the crystal structure and supramolecular interactions. DFT calculations were performed to validate the complex geometry, and the results supported the crystallographic data by confirming the optimized coordination environment and electronic properties of the complexes.