Abstract: | The reaction of (AMTTO)PdCl2] ( 1 ) (AMTTO = 4-Amino-6-methyl-1,2,4-triazine-3(2H)-thione-5-one) with triphenylphosphane and sodium thiocyanate led to the air-stable crystalline complexes (AMTTO)Pd(PPh3)Cl]Cl · MeOH ( 2 ) and (AMTTO)Pd(SCN)2] · MeCN ( 3 ) in excellent yields. 2 and 3 have been characterized by IR and 31P NMR spectroscopy, elemental analyses as well as X-ray diffraction studies. Crystal data for 2 at –83 °C: monoclinic, space group P21/n, with a = 974.4(1), b = 988.6(1), c = 2750.7(2) pm, β = 98.16(1)°, Z = 4, R1 = 0.0241 and for 3 at –80 °C: orthorhombic, space group P212121, with a = 972.0(3), b = 1168.1(4), c = 1316.6(1) pm, Z = 4, R1 = 0.0817. |