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1, 9‐Dihydro‐purine‐6‐thione Derivatives of the d8–d10 Metal Ions (PdII,PtII, and CuI): Synthesis,Spectroscopy, and Structures
Authors:Prof Dr Tarlok S Lobana  Parminderjit Kaur  Geeta Hundal  Ray J Butcher  Chen W Liu
Institution:1. Department of Chemistry, Guru Nanak Dev University, Amritsar‐143005, India;2. Department of Chemistry, Howard University, Washington DC 20059, USA;3. Department of Chemistry, National Dong Hwa University, Hualien 974, Taiwan
Abstract:Reaction of 1, 9‐dihydro‐purine‐6‐thione (puSH2) in presence of aqueous sodium hydroxide with PdCl2(PPh3)2 suspended in ethanol formed Pd(κ2‐N7,S‐puS)(PPh3)2] ( 1 ). Similarly, complexes Pd(κ2‐N7,S‐puS)(κ2‐P, P‐L‐L)] ( 2 – 4 ) {L‐L = dppm (m = 1) ( 2 ), dppp (m = 3) ( 3 ), dppb (m = 4) ( 4 )} were prepared using precursors the PdCl2(L‐L)] {L‐L = Ph2P–(CH2)m–PPh2}. Reaction of puSH2 suspended in benzene with platinic acid, H2PtCl6, in ethanol in the presence of triethylamine followed by the addition of PPh3 yielded the complex Pt(κ2‐N7,S‐puS)(PPh3)2] ( 5 ). Complexes Pt(κ2‐N7,S‐puS)(κ2‐P, P‐L‐L)] ( 6 – 8 ) {L‐L = dppm ( 6 ), dppp ( 7 ), dppb ( 8 )} were prepared similarly. The 1, 9‐dihydro‐purine‐6‐thione acts as N7,S‐chelating dianion in compounds 1 – 8 . The reaction of copper(I) chloride or copper(I) bromide] in acetonitrile with puSH2 and the addition of PPh3 in methanol yielded the same product, Cu(κ2‐N7,S‐puSH)(PPh3)2] ( 9 ), in which the halogen atoms are removed by uninegative N, S‐chelating puSH anion. However, copper(I) iodide did not lose iodide and formed the tetrahedral complex, CuI(κ1‐S‐puSH2)(PPh3)2] ( 10 ), in which the thio ligand is neutral. These complexes were characterized with the help of elemental analysis, NMR spectroscopy (1H, 31P), and single‐crystal X‐ray crystallography ( 3 , 7 , 8 , 9 , and 10 ).
Keywords:Keywords  1  9‐Dihydro‐purine‐6‐thione  Palladium  Platinum  Copper  Triphenyl phosphine
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