Preparation of trihydridostannyl complexes of rhenium stabilised by isocyanide ligands |
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| Authors: | Gabriele Albertin Stefano Antoniutti Gianluigi Zanardo |
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| Affiliation: | a Dipartimento di Chimica, Università Ca’ Foscari Venezia, Dorsoduro 2137, 30123 Venezia, Italy
b Departamento de Química Inorgánica, Universidade de Vigo, Facultade de Química, Edificio de Ciencias Experimentais, 36310 Vigo (Galicia), Spain |
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| Abstract: | Mixed-ligand complexes [ReBr(CO)2(CNR)nL3−n] (1-4) [R = 4-CH3OC6H4, 4-CH3C6H4, C(CH3)3; L = P(OEt)3, PPh(OEt)2; n = 1, 2] were prepared by allowing carbonyl compounds [ReBr(CO)4L] and [ReBr(CO)3L2] to react with an excess of isocyanide. Treatment of these bromocomplexes [ReBr(CO)2(CNR)nL3−n] with SnCl2 · 2H2O yielded the trichlorostannyl derivatives [Re(SnCl3)(CO)2(CNR)nL3−n] (5-8). Trihydridestannyl complexes [Re(SnH3)(CO)2(CNR)nL3−n] (9-12) were prepared by allowing trichlorostannyl compounds 5-8 to react with NaBH4 in ethanol. The trimethylstannyl derivative [Re(SnMe3)(CO)2(CNC6H4-4-CH3){PPh(OEt)2}2] (13b) was also prepared by treating [Re(SnCl3)(CO)2(CNC6H4-4-CH3){PPh(OEt)2}2] with an excess of MgBrMe in diethylether. Reaction of the tin trihydride complexes [Re(SnH3)(CO)2(CNR)nL3−n] (9-12) with CO2 (1 atm) led to dinuclear OH-bridging bis(formate) derivatives [Re{Sn(OC(H) O)2(μ-OH)}(CO)2(CNR)nL3−n]2 (14, 15). The complexes were characterised spectroscopically (IR, 1H, 31P, 13C, 119Sn NMR) and by X-ray crystal structure determination of [Re(SnH3)(CO)2{CNC(CH3)3}{PPh(OEt)2}2] (10b). |
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| Keywords: | Stannyl complexes Rhenium Phosphite ligands Isocyanide ligands Synthesis |
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