New heteroleptic oxovanadium(V) chloro oximato complexes of the type [VO{Cl} 3-n {ON=C(CH 3 )(Ar)} n ] (where Ar = C 4 H 3 O-2, C 4 H 3 S-2, C 5 H 4 N-2 and n = 1 or 2) have been synthesized in excellent yields by the reaction of VOCl 3 with the sodium salts of corresponding internally functionallized oximes in refluxing anhydrous benzene. The complexes are characterized by elemental analyses and spectroscopic techniques (FT-IR, 1 H-, 1 3C{ 1 H}-and 51 V-NMR). FAB mass spectral analysis of one of the derivatives, [VOCl{ON=C(CH 3 )C 4 H 3 S} 2 ] indicates the monomeric nature of the complex. 51 V-NMR spectral studies of these complexes suggest tetra-coordination around the vanadium atom in solution. However, the single crystal X-ray diffraction study of a redistribution product [VOCl{ON=C(CH 3 )(C 4 H 3 S-2)} 2 ] AE CH 3 OH obtained on recrystallization of [VOCl 2 {ON=C(CH 3 )(C 4 H 3 S-2)}] from a methanol-hexane mixture shows the vanadium(V) atom is hepta-coordinated with distorted pentagonal bipyramidal geometry. The oxo-atom occupies the axial position while the weakly coordinated CH 3 OH group is trans to the V=O atom. The two oximato ligands in the approximate pentagonal plane are bonded to the central vanadium atom in dihapto (g 2 -N, O) manner with the formation of three-membered rings. The V-Cl bond occupies the fifth position in the approximate plane.
Some new adducts of the type [R 2 NH 2 ] + [SbCl 5 S 2 CNR 2 ]" (where R=C 2 H 5 , C 3 H 7 n , C 3 H 7 \ C 4 H 9 " and NR 2 ) have been prepared by the reaction of antimony pentachloride with ammonium salts of dithiocarbamates in 1:1 molar ratio in chloroform under strictly anhydrous conditions. These moisture sensitive, thermally unstable complexes have been characterized by elemental analyses, molar conductivity, IR, 'H and "C NMR spectral studies. Molar conductivity measurements in DMSO suggest a predominant ionic bonding between dialkyl ammonium cation and dialkyldithiocarbamato pentachloroantimonate anion. IR and NMR spectral studies suggest hepta-coordination around antimony(V).
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