Synthesis, characterization of a novel 1,2,4-thiotriazine derivative (CAMTTO), and copper(I) and silver(I) complexes thereof (CAMTTO = {(4-[(4-chlorobenzylidene)-amino]-6-methyl-3-thioxo-[1,2,4]-triazin-3,4-dihydro(2H)-5-one)}

摘要

The reaction of 4-amino-6-methyl-1,2,4-triazin-thione-5-one (H(2)AMTTO, 1) with 4-chlorobenzaldhyde led to the corresponding iminic compound {(4-[(4-chloro-benzylidene)-amino]-6-methyl-3-thioxo[1,2,4]-triazin-3,4-dihydro(2H)-5-one), CAMTTO (2). Treatment of 2 with copper(l) chloride in chloroform gave the dimeric complex [{(CAMTTO)(2)CuCl}(2)]center dot 2CHCl(3) (3). Treatment of 2 with copper(I) chloride and silver(I) nitrate in the presence of the co-ligand triphenylphophane gave the complexes [(CAMTTO)CuCl(PPh3)(2)](4) and [(CAMTTO)Ag(PPh3)(2)]NO3 center dot 2CHCl(3) (5). All compounds have been characterized by elemental analyses, H-1 NMR spectroscopy, IR spectroscopy, and partly by mass spectrometry and X-ray diffraction Studies. In addition 4 and 5 have been characterized by P-31{H-1} NMR spectroscopy Crystal data for 2 at -80 degrees C: monoclinic, space group P2(1)/c, a 1370.3(1), b = 767.8(1), c = 1268.7(1) pm, beta = 107.12(1)degrees, Z = 4, R-1 = 0.0379; for 3 at -80 degrees C: monoclinic, space group P2(1)/c, a = 1442.6(2), b = 878.8(1), c = 2558.7(3) pm, beta = 95.31 (1)degrees, Z = 2, R-1 = 0.0746; for 4 at -80 degrees C: triclinic, space group P (1) over bar, a = 1287.9(1), b = 1291.7(1), c = 1359.5(1) pm, alpha = 90.44(1)degrees, beta = 94.81 (1)degrees, gamma = 107.54(1)degrees,Z = 23 R, = 0.0359 and for 5 at -80 degrees C: triclinic, space group P (1) over bar, a = 1060.5(1), b = 1578.2(2), c = 1689.6(2) pm, alpha = 87.70(1)degrees, beta = 86.66(1)degrees, gamma = 76.84(1)degrees, Z = 2, R-1 = 0.0487.