Syntheses, NMR (1H, 31P) spectroscopy and crystal structures of complexes of copper(I) halides with isatin-3-thiosemicarbazones

被引:42
作者
Lobana, TS [1 ]
Rekha
Sidhu, BS
Castineiras, A
Bermejo, E
Nishioka, T
机构
[1] Guru Nanak Dev Univ, Dept Chem, Amritsar 143005, Punjab, India
[2] Univ Santiago, Dept Quim Inorgan, Fac Farm, Santiago 15782, Spain
[3] Osaka City Univ, Dept Mat Sci, Grad Sch Sci, Sumiyoshi Ku, Osaka 5588585, Japan
关键词
copper(I); isatin-3-thiosemicarbazones; halides; phosphine; crystal structures;
D O I
10.1080/00958970500110974
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Isatin-3-thiosemicarbazones (H(2)itsc) react with copper( I) bromide or iodide in a 1 : 1 mol ratio in acetonitrile in the presence of two moles of Ph3P to form tetrahedral monomeric complexes of composition [CuX(eta(1)-S-H(2)itsc)(Ph3P)(2)], X = Br ( 1), I ( 2). These complexes, which have been characterized by single-crystal structure determinations, are unlike the iodo-bridged dinuclear complex of copper( I) iodide of pyrrole-2-carbaldehydethiosemicarbazone (Hptsc), namely [Cu-2(mu- I)(2)(eta(1)-S-Hptsc)(2)(PPh3)(2)] ( 3). In both 1 and 2, the geometry around Cu is distorted tetrahedral with P - Cu - P bond angles being 121.97( 3) ( 1) and 124.09( 5)degrees ( 2). Proton NMR confirms that thiosemicarbazone coordinates to the Cu atom as a neutral ligand, and P-31 NMR shows that there is no dissociation of the complexes in solution; coordination shift values suggest that Ph3P stabilizes the Cu(I) oxidation state.
引用
收藏
页码:803 / 809
页数:7
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