Synthesis and characterization of complexes of the type [Pt(amine)(4)]I-2 and trans-[Pt(CH3NH2)(2)(H3C-N=C(CH3)2)(2)]I-2 by crystallography and multinuclear magnetic resonance spectroscopy

摘要

Complexes of the type [Pt(amine)(4)]I-2 were synthesized and characterized mainly by multinuclear (Pt-195, H-1 and C-13) magnetic resonance spectroscopy. The compounds were prepared with different primary amines, but not with bulky amines, due to steric hindrance. In Pt-195 NMR, the signals were observed between -2715 and -2769 ppm in D2O. The coupling constant (3)J(Pt-195-H-1) for the MeNH2 Complex is 42 Hz. In C-13 NMR, the average values of the coupling constants (2)J(Pt-195-C-13) and (3)J(Pt-195-C-13) are 18 and 30 Hz, respectively. The crystal structure of [Pt(EtNH2)(4)]I-2 was determined by X-ray diffraction methods. The Pt atom is located on an inversion center. The structure is stabilized by H-bonding between the amines and the iodide ions. The compound with n-BuNH2 was found by crystallographic methods to be [Pt(n-BuNH2)(4)](2)I-3(n-BuNHCOO). The crystal contains two independent [Pt(CH3NH2)(4)](2+) cations, three iodide ions and a carbamate ion formed from the reaction of butylamine with CO2 from the air. When the compound [Pt(CH3NH2)(4)]I-2 was dissolved in acetone, crystals identified as trans-[Pt(CH3NH2)(2)(H3C-N=C(CH3)(2))(2)]I-2 were isolated and characterized by crystallographic methods. Two trans bonded MeNH2 ligands had reacted with acetone to produce the two N-bonded Schiff base Pt(II) compound. (C) 2006 Elsevier B.V. All rights reserved.