SYNTHESIS, SPECTROSCOPIC AND STRUCTURAL CHARACTERIZATION OF METHYL PYRUVATE-HYDRAZINOPYRUVOYLTHIOSEMICARBAZONE AND PYRIDOXAL-HYDRAZINOPYRUVOYLTHIOSEMICARBAZONE

Two new thiosemicarbazones, methyl pyruvate-hydrazinopyruvoylthiosemic arbazone (H2mpipt), pyridoxal-hydrazinopyruvoylthiosemicarbazone (H2pi ript), and their common reaction intermdiate, pyruvic acid thiosemicar bazone hydrazide (Hipt), have been synthesized and characterized using IR and NMR spectroscopic methods. The crystal structures of H2mpipt a nd Hipt.H2O have been determined by X-ray crystallographic methods. Bo th compounds form monoclinic crystals belonging to the space group P2( 1)/c with Z = 4 (a = 11.050(2), b = 10.386(2), c = 11.468(2) angstrom, beta = 114.87(3)-degrees and a = 7.476(1), b = 15.359(3), c = 8.367(1 ) angstrom, beta = 114.43(3)-degrees, respectively). The ligand H2mpip t reacts with [Cu(PPh3)Cl]4 and forms the Cu(I) complex [Cu(PPh3)2(H2m pipt)Cl].CH3OH whose structure has been determined by X-ray crystallog raphic methods. The copper atom has a distorted tetrahedral coordinati on sphere involving a chlorine atom, the phosphorus atoms of the two P Ph3 molecules and a sulfur atom of the H2mpipt moiety. The crystals of the complex are triclinic, space group P1BAR, Z = 2, a = 18.331(2), b = 10.025(2), c = 13.697(2) angstrom, alpha = 72.17(2), beta = 97.77(2 ), gamma = 87.42(2)-degrees. The configuration of H2mpipt in the compl ex is different from that of the free ligand. The H-1, C-13 and N-15 N MR spectra for H2piript are also discussed.