TY - JOUR
T1 - Synthesis and structural characterization of silanethiolato complexes having tert-butyldimethylsilyl and trimethylsilyl groups
AU - Komuro, Takashi
AU - Matsuo, Tsukasa
AU - Kawaguchi, Hiroyuki
AU - Tatsumi, Kazuyuki
PY - 2004/5/21
Y1 - 2004/5/21
N2 - Treatment of cyclotrisilathiane (Me2SiS)3 with 3 equiv. of RLi (R = Me, But) in hexane-Et2O afforded the lithium silanethiolates LiSSiMe2R, and the tmeda adduct [(tmeda)LiSSiMe2But]2 1(tmeda = N,N,N′,N′-tetramethylethylenediamine) was isolated in the case of R = But. Reaction of Fe(CH3CN)2(CF 3SO3)2, CoCl2, and [Cu(CH 3CN)4](PF6) with 1 gave rise to the silanethiolato complexes M(SSiMe2But)2(tmeda) (M = Fe 2, Co 3), and [Cu(SSiMe2But)]4 4, respectively. Complexes (C5H5)2Ti(SSiMe 2R)2 (R = Me 5, But 6) and Ni(SSiMe 2R)2(dppe) [R = Me 7, But 8; dppe = 1,2-bis(diphenylphosphino)ethane] were prepared from treatments of (C 5H5)2TiCl2 and NiCl 2(dppe) with the corresponding lithium silanethiolates. Complex 7 readily reacted with (C5H5)TiCl3 to produce the Ti-Ni heterobimetallic compound (C5H5)TiCl(μ-S) 2Ni(dppe) 9, in which silicon-sulfur bond cleavage took place. Characterization of all compounds through spectroscopic techniques and elemental analyses are also described. X-Ray structural data for compounds 1 and 3-9 are reported.
AB - Treatment of cyclotrisilathiane (Me2SiS)3 with 3 equiv. of RLi (R = Me, But) in hexane-Et2O afforded the lithium silanethiolates LiSSiMe2R, and the tmeda adduct [(tmeda)LiSSiMe2But]2 1(tmeda = N,N,N′,N′-tetramethylethylenediamine) was isolated in the case of R = But. Reaction of Fe(CH3CN)2(CF 3SO3)2, CoCl2, and [Cu(CH 3CN)4](PF6) with 1 gave rise to the silanethiolato complexes M(SSiMe2But)2(tmeda) (M = Fe 2, Co 3), and [Cu(SSiMe2But)]4 4, respectively. Complexes (C5H5)2Ti(SSiMe 2R)2 (R = Me 5, But 6) and Ni(SSiMe 2R)2(dppe) [R = Me 7, But 8; dppe = 1,2-bis(diphenylphosphino)ethane] were prepared from treatments of (C 5H5)2TiCl2 and NiCl 2(dppe) with the corresponding lithium silanethiolates. Complex 7 readily reacted with (C5H5)TiCl3 to produce the Ti-Ni heterobimetallic compound (C5H5)TiCl(μ-S) 2Ni(dppe) 9, in which silicon-sulfur bond cleavage took place. Characterization of all compounds through spectroscopic techniques and elemental analyses are also described. X-Ray structural data for compounds 1 and 3-9 are reported.
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U2 - 10.1039/b316567a
DO - 10.1039/b316567a
M3 - Article
AN - SCOPUS:3042724720
SP - 1618
EP - 1625
JO - Dalton Transactions
JF - Dalton Transactions
SN - 1477-9226
IS - 10
ER -