SYNTHESIS, STRUCTURE, AND PROPERTIES OF TETRAETHYLAMMONIUM BIS[BIS(2-OXYPHENYL)-DISULFIDE-O,O',S]MANGANESE(III)

The title compound (Et4N)[Mn(MP-MP)2] (1) was obtained by air oxidation of an acetonitrile solution of MnCl2.4H2O and Na2MP. The structure of 1 was determined by single crystal X-ray diffraction methods. Crystal data: C32H36MnNO4S4, monoclinic, P21/c, a = 9.598(3), b = 16.845(3), c = 10.702(3) Å, β = 111.20(1)°, V= 1613.1 Å3, Z = 2; Mr = 681.84; dx= 1.40gem-3; F(000) = 712; p = 6.8cm-1, crystal dimensions 0.40 x 0.20 x 0.20 mm3. The Mn atom is octahedrally and symmetrically coordinated by two MP-MP2-ligands, each providing two phenolateoxygen and one disulfide-sulfur atoms to form a terdentate. The presence of an S-S bond is revealed by the distance of 2.093 A, which constitutes the first disulphide chelated to the Mn(III) ion. The paramagnetic nature of the high spin Mn(d4) ion is reflected in a value of μcffof 4.83 μBand broad 1H NMR absorptions at 23 ∼ 25 ppm and —12 ~ —17 ppm. © 1990, Taylor & Francis Group, LLC. All rights reserved.