Five-coordinate nickel(II) complexes with carboxylate anions and derivatives of 1,5,9-triazacyclododec-1-ene: structural and 1H NMR spectroscopic studies.
The hydroxo complexes [Ni2(mcN3)2(mu-OH)2]2(PF6)2[mcN3 = 2,4,4-trimethyl-1,5,9-triazacyclododec-1-ene (Me3-mcN3) or 2,4,4,9-tetramethyl-1,5,9-triazacyclododec-1-ene (Me4-mcN3)] react with the corresponding carboxylic acid [HA = benzoic (Hbz), salicylic (Hsal) or acetylsalicylic (Hacsal) acid] to give five-coordinate nickel(II) complexes of the type [Ni(mcN3)(A)](PF6). The complexes have been studied by spectroscopic methods (IR, UV-Vis and 1H NMR). In acetone solution they exhibit isotropically shifted 1H NMR resonances. The full assignment of these resonances has been made using one- and two-dimensional 1H NMR techniques. The single-crystal structures of [Ni(Me4-mcN3)(bz)](PF6), [Ni(Me4-mcN3)(sal)](PF6) and[Ni(Me4-mcN3)(acsal)](PF6) have been established by X-ray diffraction.
Santana
M Dolores
MD
Departamento de Química Inorgánica, Universidad de Murcia, 30071 Murcia, Spain. dsl@um.es
Lozano
A Abel
AA
Garcia
Gabriel
G
Lopez
Gregorio
G
Perez
Jose
J