Beiträge zur Chemie der Silicium‐Schwefel‐Verbindungen. 50 [1] Bis(triorganoxysilyl)polysulfide und die Struktur des Bis(tri‐t‐butoxysilyl)disulfids

Abstract

Disilylierte Polysulfide (RO)3SiSnSi(OR)3, R = i‐Pr, t‐Bu, 2,6‐Me2C6H3, n = 2–5, wurden durch Reaktion von (RO)3SiSNa mit I2 bzw. SnCl2 dargestellt. Die Umsetzung von [(t‐BuO)3Si]2S2 mit Ph3SiH liefert ein gemischtes Sulfid (t‐BuO)3SiSSiPh3 und mit Ph3P oder Bu3P, durch Abbau eines S‐Atoms, [(t‐BuO)3Si]2S. Die Kristall‐Struktur von [(t‐BuO)3Si]2S2 wurde bestimmt. Die SS‐Bindungslänge beträgt 209,2 pm, SiS 213,2 pm. Der Mittelwert für den SiSS‐Winkel beträgt 100,7°, der Torsionswinkel SiSSSi −127,6°.

The first manganese trialkoxysilanethiolates: Formation, properties and structure of solvent ligated complexes – [Mn{SSi(OBut)3}2(MeCN)] and [Mn{SSi(OBut)3}2(MeOH)4]

“…Crystals of 3 subjected to the stream of oxygen gave dark-brown oily residue from which (Bu t O) 3 SiSH was separated by column chromatography. Corresponding disulfide [(Bu t O) 3 SiS] 2 [27] was not found.…”

Tri(mesityloxy)silanethiol – The First Structurally Characterized Organoxysilanethiol (Contributions to the Chemistry of Silicon–Sulfur Compounds. 77 [1])

“…As usual, the non‐bonding lone pair electrons occupy a well‐defined volume, exerting a steric effect, which leaves asulfur atom half‐uncovered (see Figure 1S, Electronic Supporting Information). The structural parameters of TMST are compared with those calculated for tri‐ tert ‐butoxysilanethiol 20 and measured for bis(tri‐ tert ‐butoxysilyl) disulfide 21 in Table 1S (Electronic Supporting Information).…”

“…Supporting Information (see footnote on the first page of this article) : Crystal packing and the spacefill model of the molecule in color, FT‐IR spectrum of TMST, comparison of the geometrical parameters of TMST with those calculated for tri‐ tert ‐butoxysilanethiol 20 and measured for bis(tri‐ tert ‐butoxysilyl) disulfide 21, the atom coordinates, displacement parameters, full tables of bond lengths, and bond angles.…”

Synthesis of tetraphenylporphyrinate manganese(III) siloxides by silyl group transfer from silanethiols

“…In a modified literature procedure [52], a vial was charged with 115 μL (536 μmol) of HSSi i Pr 3 , 75 µL (540 μmol) of Et 3 N, and 1 mL of toluene. After briefly stirring the contents of the solution, 63.8 mg (503 μmol) of I 2 was added as solid in one portion.…”