Ammonolysis of 1,2‐Bis[dichloro(methyl)silyl]ethane. On the Structure of 1,3,6,8‐Tetramethyl‐2,7,11,12‐tetraaza‐1,3,6,8‐tetrasila‐tricyclo[6.2.1.1^3,6]‐dodecane 

Abstract

Ammonolysis of 1,2‐bis[dichloro(methyl)silyl]ethane afforded a crystalline tricyclic silazane along with polymeric material. The crystalline material could be isolated in pure state. It was analyzed by 1H, 13C, 15N and 29Si NMR spectroscopy in solution, by 13C, 15N and 29Si MAS NMR spectroscopy in the solid state, as well as by single‐crystal and powder X‐ray diffraction. The title compound exists as a single isomer in solution, whereas in the solid state the presence of several modifications is indicated, in particular by the solid‐state MAS NMR spectra.

Insights into the Catalytic Activity of Nitridated Fibrous Silica (KCC‐1) Nanocatalysts from 15N and 29Si NMR Spectroscopy Enhanced by Dynamic Nuclear Polarization

“…15 N CPMAS spectrum without microwave irradiation, with a similar S/N ratio as that in Figure 3 and 25 ppm and can be assigned to NH 2 Si and NHSi 2 sites, respectively. [19,20] The deconvolution of the KCC-1-15 N700 spectrum indicates the presence of an additional site near d = 0 ppm, which can be assigned to ammonium ions. [21] In none of the samples could we detect any signals for 15 NH 3 near d = À32 ppm.…”

Insights into the Catalytic Activity of Nitridated Fibrous Silica (KCC‐1) Nanocatalysts from 15N and 29Si NMR Spectroscopy Enhanced by Dynamic Nuclear Polarization

“…The 15 N spectra of KCC-1-N600 and KCC-1-15 N700 are dominated by two resolved peaks near d = 10 and 25 ppm and can be assigned to NH 2 Si and NHSi 2 sites, respectively. [19,20] The deconvolution of the KCC-1-15 N700 spectrum indicates the presence of an additional site near d = 0 ppm, which can be assigned to ammonium ions. [21] In none of the samples could we detect any signals for 15 NH 3 near d = À32 ppm.…”