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Syntheses and Crystal Structures of [(AMTTO)Pd(PPh3)Cl]Cl · MeOH and [(AMTTO)Pd(SCN)2] · MeCN

✍ Scribed by Bernhard Neumüller; Majid M. Heravi; Mitra Ghassemzadeh


Publisher
John Wiley and Sons
Year
1999
Tongue
German
Weight
115 KB
Volume
625
Category
Article
ISSN
0372-7874

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✦ Synopsis


The reaction of [(AMTTO)PdCl 2 ] (1) (AMT-TO = 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(PPh 3 )Cl]Cl ḾeOH (2) and [(AMTTO)Pd(SCN) 2 ] ´MeCN (3) in excellent yields. 2 and 3 have been characterized by IR and 31 P NMR spectroscopy, elemental analyses as well as X-ray diffraction studies. Crystal data for 2 at ±83 °C: monoclinic, space group P2 1 /n, with a = 974.4(1), b = 988.6(1), c = 2750.7(2) pm, b = 98.16(1)°, Z = 4, R 1 = 0.0241 and for 3 at ±80 °C: orthorhombic, space group P2 1 2 1 2 1 , with a = 972.0(3), b = 1168.1(4), c = 1316.6(1) pm, Z = 4, R 1 = 0.0817.


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## Reactions of [(AMTTO)PdCl 2 ]•MeOH (1) with sodium bromide and sodium iodide led to the palladacycles [(AMTTO)PdBr 2 ] 2 •3.5THF (2) and [(AMTTO)PdI 2 ] 2 •3MeOH (3) in excellent yields. Treatment of 2 and 3 with triphenylphosphane gave the complexes [(AMTTO)Pd(PPh 3 )Br]-Br•MeOH (4) and [(AMTT