K. Chryssou et al., SYNTHESIS AND STRUCTURAL CHARACTERIZATION OF THE ETHYL-4,7-DIAZA-2,9-DECANEDITHIOLATO]OXORHENIUM(V) COMPLEX, Inorganica Chimica Acta, 268(2), 1998, pp. 169-175
The neutral and lipophilic complex -dimethyl-4,7-diaza-2,9-decanedithi
o]oxorhenium(V) was synthesized and characterized by FT-IR, UV, mass a
nd NMR spectroscopies, X-ray crystallographic analysis of the complex
(C10H21N2OS2Re) showed that the complex crystallizes in the monoclinic
space group C2/c with a=21.357(2), b=13.615(1), c=20.778(2) Angstrom,
beta=98.648(3)degrees, V=5973.0(9) Angstrom(3), z=16. Detailed NMR st
udies revealed that in CDCl3 and CD3OD solutions the amine proton of t
he complex is labile and undergoes exchange between the two nitrogens
of the complex, Evidence is presented that the nature of the exchange
is intermolecular. In the presence of DCl, both in CD3OD and D2O solut
ions, the complex is protonated on both nitrogens while in the presenc
e of NaOD the complex is completely deprotonated. Protonation/deproton
ation of the complex are completely reversible processes as evidenced
by NMR. (C) 1998 Elsevier Science S.A.