Synthesis and characterization of new AMTTO-imine-ligands and their silver(I) complexes: crystal structures of TAMTTO, [Ag-2(TAMMTO)(4)](NO3)(2)center dot 4MeOH,[Ag(TAMTTO)(PPh3)(2)]NO3 center dot 1.5THF, [Ag(FAMTTO)(PPh3)(2)]NO3

摘要

Reaction of 4-amino-6-methyl-1,2,4-triazin-thione-5-one (AMTTO, 1) with 2-thiophenecarboxaldehyde and 2-furaldehyde led to the corresponding iminic compounds 6-methyl-4-[thiophene-2-yl-methylene-amino]-3-thioxo-[1,2,4]-triazin-3,4-dihydro(2H)-5-one (TAMTTO, 2) and 4-[furan-2-yl-methylene-amino]-6-methyl-3-thioxo-[1,2,4]-triazin-3,4-dihydro(2H)-5-one (FAMTTO, 3). Treatment of 2 with AgNO3 gave the complex [Ag-2(TAMMTO)(4)](NO3)(2).4MeOH (4) and of 2 and 3 with [Ag(PPh3)(2)]NO3 gave the complexes [Ag(TAMTTO)(PPh3)(2)]NO3 . 1.5THF (5) and [Ag(FAMTTO)(PPh3)(2)]NO3 (6), respectively. All the compounds have been characterized by elemental analyses, IR spectroscopy and mass spectrometry. Compound 2 and all the complexes have been characterized by X-ray diffraction studies, respectively. In addition, 5 and 6 have been characterized by (31) P NMR spectroscopy. Crystal data for 2 at -80 degreesC: monoclinic, space group C2/c, a = 2319.6(2), b = 609.8(l), c = 1673.6(2) pm, beta = 106.14(l)degrees, Z = 8, R-1 = 0.0523; for 4 at -80 degreesC: triclinic, space group P (1) over bar, a = 877.6(l), b = 1085.2(l), c = 1557.7(2) pm, alpha = 77.14(l)degrees, beta = 80.87(l)degrees, gamma = 78.18(l)degrees, beta = 1, R-1 = 0.0407; for 5 at 20 degreesC: triclinic, space group P (1) over bar, a = 1151.1(2), b = 1225.1(2), c = 1887.4(3) pm, alpha = 78.04(1)degrees, beta = 86.20(l)degrees, gamma = 76.03(l)degrees, Z = 2, R-1 = 0.0662; for 6 at -80 degreesC: triclinic, space group P (1) over bar, a = 1189.7(2), b = 1387.8(2), c = 1410.9(2) pm, alpha = 94.74(2)degrees, beta = 95.12(2)degrees, gamma = 112.41(2)degrees, Z = 2, R-1 = 0.0511. (C) 2004 Elsevier B.V. All rights reserved.