Synthesis and Pyrolytical Studies of New Oxorhenium(V) Complexes with a Tetraaza Macrocyclic Ligand
Titel:
Synthesis and Pyrolytical Studies of New Oxorhenium(V) Complexes with a Tetraaza Macrocyclic Ligand
Auteur:
Mashaly, Mahmoud
Verschenen in:
Journal of coordination chemistry
Paginering:
Jaargang 55 (2002) nr. 10 pagina's 1171-1182
Jaar:
2002
Inhoud:
5,12-dioxa-7,14-dimethyl-1,4,8,11-tetraazacyclotetradeca-1,8-diene (N4L) reacts with the starting oxorhenium(V) complex, H2[ReOCl5], to yield either mononuclear [ReO(N4L)(OH2)]Cl3, or dinuclear [Re2O3(N4L)2]Cl4·2H2O depending on the concentration of hydrochloric acid in rhenium complex. The reaction of (N4L) mixed with KSCN or PPh3 with the oxorhenium(V) complex in 6N HCl, yielded the mononuclear complexes [ReO(N4L)(SCN)]Cl2·H2O and [ReO(N4L)(PPh3)]Cl3·H2O respectively. Both complexes have an octahedral configuration. These complexes decompose through several isolable, as well as non-isolable, intermediates during heating. [Re2O3(N4L\)2] (N4L\ = dianionic tetradentate ions), [ReO(N4L)Cl]Cl2 and [ReO(N4L\)(SCN)], were synthesized pyrolytically in the solid state from the corresponding rhenium(V) complexes. All have octahedral configurations. The ligand (N4L) behaves in these complexes either as a neutral tetradentate or dianionic tetradentate ligand towards the oxorhenium ions. All complexes and the corresponding thermal products were isolated and their structures were elucidated by elemental analyses, conductance, IR and electronic absorption spectra, magnetic moments, 1H NMR and TG-DSC measurements as well as by mass spectroscopy.
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