Structural studies of ReO(V) mixed ligand [SNS][Cl] and [SNS][S] complexes

The synthesis, characterization and spectroscopic properties of four oxorhe nium complexes, ReO[C2H5SCH2CH2N(CH2CH2S)(2)]Cl (1), ReO[C2H5SCH2CH2N(CH2CH 2S)(2)][p-CH3OC6H4S] (2), ReO[(C2H5)(2)NCH2CH2N(CH2CH2S)(2)][p-CH3C6H4S] (3 ), and ReO[C5H10NCH2CH2N(CH2C(CH3)(2)S)(2)][C6H5CH2S] (4) are reported. The se neutral and lipophilic complexes are designed according to the '3 + 1' m ixed ligand concept. X-ray crystallographic studies show that the coordinat ion geometry around rhenium is distorted trigonal bipyramidal in complexes 2 and 3 and trigonally distorted square pyramidal in complex 4 (C15H24NO2S4 Re (2), triclirzic P (1) over bar, a=9.610(2), b=9.628(2), c=11.791(2) Angs trom, alpha=108.307(8), beta=67.735(6), gamma=90.166(8)degrees, V = 950.04 Angstrom(3), Z = 2; C17H29N2OS3Re (3), monoclinic P2(t)/c, a = 13.188(1), b = 7.542(1), c = 21.193(1) Angstrom, beta = 103.260(2)degrees, V = 2051.74 Angstrom(3), Z = 4; C22H37N2OS3Re . 0.5C(2)H(5)OH (4), monoclinic P2(t)/c, a = 16.720(6), b = 11.013(3), c = 16.747(5) Angstrom, beta = 113.44(1)degre es, V = 2829.08 Angstrom(3), Z = 4. Complete assignments of H-1 and C-13 NM R resonances were made for all complexes and compared to those of analogous technetium complexes. Complex 3 was also prepared at the tracer Re-186 lev el. (C) 1999 Elsevier Science S.A. All rights reserved.