Organosilyl Sulfides and Organogermyl Sulfides

Studies of silyl and germyl group VI species. Part VI. Synthesis and vibrational spectra of methylthiosilanes

“…All are, as expected, sharp, polarised bands. The placing of the Si-C stretch at higher wave-number than the S-C is consistent with data on related sulfides (10). In organic sulfides, the S-C stretch typically appears as a strong Raman band with a corresponding rather weak infrared feature (28), and the value of 701 cm-I is close to that in H3SiSCH, where there is no ambiguity.…”

“…3 and 2 respectively. The assignment in Table 7, but for minor details, is essentially in agreement with the earlier partial assignment made along with those of other methylsilylsulfides (10 53 (8)+50 (11)+5 (21)+3 (4) 763 mw, dp 661 ms, p 630 w, dp : ; ; I : , sh 261 m, p 229 s, p 208 ms, dp 150 w, p (CH3),Si group relative to those of CH,S underlines the placing of the latter modes to higher wave-number. The band at 960 cm-I in the Raman (965 cm-' in the ir) can be considered characteristic of the CH3-S rocking motion while the (CH3),-Si rocks can be placed, again characteristically, in the ' range 750-870cm-'.…”

“…In recent years some alkylthiosilanes have been prepared by reaction of appropriate halogenosilanes with CH,SMgI (lo), RSNa (18), and CH3SH in the presence of base (9,10). The use of complex aluminates as synthetic reagents has been studied considerably (8,19).…”

Studies of silyl and germyl Group VI species. Part IV. Dimethyl- and tetramethyl-disilyl chalcogenides and related species

“…Halogeno-silanes (I I) (0.21 g, mmOll 96%) and (H3Si)20 (0.095 g, mmo17 and -germanes were either commercially obtained or prepared 93%, collected at -126OC) and the purity was confirmed by their by literature methods. Lithium telluride, Li2Te, was prepared vibrational (141, 'H nmr (8,151, and mass spectral ( (~~~1 5 -from the elements in liquid NH3 (9). Complex thio-and seleno-Size)+ m/e 147-149, 78.6%; (HnSi20)+ mle 72-80, 73.6%) aluminates were prepared from LiAIH, (12) and hydrogen parameters.…”

Synthesis and NMR Investigation of Selenobutyl Substituted Silanes and Oligosilanes

“…Elemental selenium inserts in THF solution into the carbon-metal bond of organolithium or Grignard compounds, yielding R-Se-Li or R-Se-Mg-X. But attempts to isolate Ph-Se-SiMe 3 by treatment of a Ph-Se-MgBr solution in diethyl ether with Me 3 SiCl yielded only (Me 3 Si) 2 Se [3].…”