排序方式: 共有42条查询结果,搜索用时 15 毫秒
1.
2.
K. Dippel U. Klingebiel T. Kottke F. Pauer G. M. Sheldrick D. Stalke 《无机化学与普通化学杂志》1990,584(1):87-104
Fluorosilyl and Fluoroboryl Substituted Cyclotetrasilazanes. Synthesis and Crystal Structures Mono- and dilithiated octamethylcyclotetrasilazanes ( 1, 6 ) react with fluorosilanes and F2BN(SiMe3)2, respectively, under retention of the cyclotetrasilazane structure yielding the mono- and disubstituted compounds 2–5 and 7–13 . In the reaction of the dilithium compound 6 with a fluorsilane in equivalent amounts, the bicyclic compounds 14 and 15 are obtained. Crystallographic investigations of the compounds 2, 3, 8 , and 9 indicate that the monosilylated eight-membered ring has a cradle conformation while the disilylated ring has a chair conformation. The X-ray structure of the bicyclic system 14 indicates that the nitrogen atoms of the Si3N-units have a pyramidal environment. 相似文献
3.
Bis(cyclodisilazane-1-yl) dimethylsilanes — Synthesis and Reactions The monolithium derivate of trisilazan-1-yl-cyclodisilazane 1 reacts with F3SiN (SiMe3)2 with substitution. The silyl-bridged cyclodisilazanes 3–6 are formed in the reaction of the dilithium derivate of 1 with fluoro- and chlorosilanes. Using lithiumamide and lithiummethanolate a controlled exchange of one fluoro atom of 4 occurs ( 7,8 ). 9 and 10 are formed by hydrolysis of 4 . The aminofunctional compounds 11 und 12 are obtained in the reaction of 5 and 6 with NH3. The dispirocyclus 13 is formed in the reaction of 8 with tert.-butyllithium. The reaction of dilithiated 1 with 4 gives the spirocyclus 14 . The crystal structure of 14 is discussed. 相似文献
4.
Synthesis of Functional Carboxylic Acid Silylester Di-tert-butylsilandiol reacts with organic acid chlorides to chlorosilanoles R2Si(OH)Cl 1 (R = t-Bu). The phosphoric acid silylester 2 is obtained from 1 and POCl3. Lithiated halogenosilanoles react with carboxylic acid chlorides to give silylesters ( 3 – 7 ). Lithium (trimethyl-acetoxy)silanolate 8 is obtained in the reaction of the lithiated diol with the chloride of trimethylacetic acid. The analogous reaction with benzoyl chloride lead to the formation of the bis(benzoic acid) silylester 9 . The condensation product 10 is obtained in the reaktion of the lithiated aminosilanol (t-Bu)2Si(NH2)OLi with trimethylacetic acid chlorid and condensation of the formed ester with aminosilanol. 相似文献
5.
Sebastian Scheidel Laurina Östreicher Isabelle Mark Ann-Christin Pöppler 《Magnetic resonance in chemistry : MRC》2022,60(6):572-582
Although solid-state nuclear magnetic resonance (NMR) is a versatile analytical tool to study polymorphs and phase transitions of pharmaceutical molecules and products, this work summarizes examples of spontaneous and unexpected (and unwanted) structural rearrangements and phase transitions (amorphous-to-crystalline and crystalline-to-crystalline) under magic angle spinning (MAS) conditions, some of them clearly being due to the pressure experienced by the samples. It is widely known that such changes can often be detected by X-ray powder diffraction (XRPD); here, the capability of solid-state NMR experiments with a special focus on 1H-13C frequency-switched Lee–Goldburg heteronuclear correlation (FSLG HETCOR)/MAS NMR experiments to detect even subtle changes on a molecular level not observable by conventional 1D NMR experiments or XRPD is presented. Furthermore, it is shown that a polymorphic impurity combined with MAS can induce a crystalline-to-crystalline phase transition. This showcases that solid-state NMR is not always noninvasive and such changes upon MAS should be considered in particular when compounds are studied over longer time spans. 相似文献
6.
B. Fischer B. Ittermann E. Diehl R. Dippel K. H. Ergezinger H.-P. Frank E. Jger W. Seelinger G. Sulzer H. Ackermann H.-J. Stckmann H. G. Bohn 《Annalen der Physik》1990,502(8):659-666
β-radiation detected nuclear magnetic resonance was applied to determine the location of 12B probe nuclei in a Ni3Al single crystal. Combining our results with those of channeling experiments it turned out that more than 90% of the 12B ions occupy the octahedral interstitial site with six Ni ions as nearest neighbours. 相似文献
7.
8.
Granitzka M Pöppler AC Schwarze EK Stern D Schulz T John M Herbst-Irmer R Pandey SK Stalke D 《Journal of the American Chemical Society》2012,134(2):1344-1351
Various 2-thienyllithium derivatives were investigated in the solid state by X-ray diffraction and in solution by 2D NMR experiments. The determined structures of [(Et(2)O)Li(C(4)H(3)S)](4) (1), [(THF)(2)Li(C(4)H(3)S)](2) (2), [(DME)Li(C(4)H(3)S)](2) (3), [(TMEDA)Li(C(4)H(3)S)](2) (4), and [(PMDETA)Li(C(4)H(3)S)] (5) (DME = 1,2-dimethoxyethane, TMEDA = N,N,N',N'-tetramethylethylene-1,2-diamine, and PMDETA = N,N,N',N",N"-pentamethyldiethylenetriamine) were solved in nondonating toluene and provide firm ground for diffusion-ordered NMR spectroscopy as well as heteronuclear Overhauser enhancement NMR spectroscopy. The distance relation of nuclear Overhauser effects with a factor of r(-6) is employed to gain further insight into the aggregation degree of 1-5 in solution. Comparison of the slope provided by the linear region of the buildup curves and of the ∑r(-6) calculated distances from the crystal structures offers a handle to judge the structure retention versus conversion in solution. The structures of 3-5 are maintained in toluene solution. The data of 2, however, indicate a partial dissociation or a rapid exchange between the vertices of a tetrameric core and free THF molecules. Auxiliary exchange spectroscopy investigations showed that the signals of the nitrogen donor base containing compounds 4 and 5 exchange with the signals of nonlithiated thiophene. This is explained by exchange of the deuterium by a hydrogen atom via lithiation of toluene molecules. 相似文献
9.
10.
Photodesorption and photofragmentation of disilane adsorbed on a hydrogen terminated Si(100) surface
The photochemical mechanisms leading to the desorption and fragmentation of Si2H6 adsorbed on a hydrogen terminated Si(100) surface have been explored by recording the time-of-flight distributions of products escaping from the surface and by using electron energy loss spectroscopy to probe possible electronic excitations. Photodesorption of intact Si2H6 involves hot electrons that lose energy and move to the conduction band edge before initiating desorption. When the wavelength of the incident light is 193 nm, Si2H6 fragments give mostly Si, SiH2, H2 and SiH4, but this pathway is quenched at longer wavelengths. This is consistent with direct excitation, but we also show that a negative ion resonance is accessible to substrate electrons that have been excited by 193 nm light. 相似文献