Einfache Trithio- und Perthiocarbonatokomplexe mit interessanter Koordinationschemie: [E(CS3)2]2− (E = Sn,Zn, Cd), [E(CS3)3]3− (E = As,Sb, Bi,Co), {Cu(CS3)−}∞ und [Zn(CS4)2]2− |
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Authors: | A Müller E Krickemeyer F El-Katri D Rehder A Stammler H Bgge F Hellweg |
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Institution: | A. Müller,E. Krickemeyer,F. El-Katri,D. Rehder,A. Stammler,H. Bögge,F. Hellweg |
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Abstract: | Simple Trithio- and Perthiocarbonato Complexes with Interesting Bond Properties: E(CS3)2]2? (E = Sn, Zn, Cd), E(CS3)3]3? (E = As, Sb, Bi, Co), {Cu(CS3)?}∞ and Zn(CS4)2]2? By reactions of potassium trithiocarbonate ( 1 ) with solutions of zinc(II)- acetylacetonate, cadmium(II)-chloride, tin(II)-chloride, arsenic(III)-sulfide (suspension), antimony(III)-chloride, bismuth(III)-chloride and copper(II)-chloride in dimethyl sulfoxide, as well as of trisodium hexanitrito cobaltate(III) in water, and the precipitation of the complexes with an aqueous solution of tetraphenylphosphonium chloride the compounds (PPh4)2Zn(CS3)2] ( 2 ), (PPh4)2Cd(CS3)2] ( 3 ), (PPh4)2Sn(CS3)2] ( 4 ), (PPh4)3As(CS3)3] ( 5 ), (PPh4)3Sb(CS3)3] ( 6 ), (PPh4)3Bi(CS3)3] ( 7 ), (PPh4)3Co(CS3)3] ( 8 ) and (PPh4)Cu(CS3) ( 9 ) have been isolated. (PPh4)2Zn(CS4)2] · CH3NO2 ( 10 ) has been prepared by heating a solution of 2 in nitromethane to 60--70°C in presence of air. The reaction of 1 in dimethyl sulfoxide with an aqueous tetraphenylphosphonium chloride solution in presence of oxygen leads to (PPh4)2C2S6] ( 11 ). The compounds have been characterized by spectroscopical studies (IR, Raman, UV/Vis, 113Cd/59Co-NMR), magnetic susceptibility measurements, powder diffractometry, elemental analyses and single crystal X-ray structure analysis ( 4 – 7 , 10 and 11 ). The difficult growing of single crystals has been reported in detail. For crystal data see Inhaltsübersicht. |
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Keywords: | zinc cadmium tin arsenic antimony bismuth cobalt copper trithio complexes perthio complexes perthiodicarbonate synthesis crystal structure IR spectroscopy Raman spectroscopy 113Cd and 59Co NMR spectroscopy |
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