@article{TackeLopezMrasSperlichetal.1993, author = {Tacke, Reinhold and Lopez-Mras, A. and Sperlich, J. and Strohmann, C. and Kuhs, W. F. and Mattern, G. and Sebald, A.}, title = {Neue zwitterionische \(\lambda_5\)-Spirosilicate: Synthesen, Einkristall-R{\"o}ntgenstrukturanalysen und Festk{\"o}rper-NMR-Untersuchungen}, url = {http://nbn-resolving.de/urn:nbn:de:bvb:20-opus-64251}, year = {1993}, abstract = {The zwitterionic spirocyclic \(\lambda_5\) -Silicates bis(3,4,5,6-tetrabromo- 1,2-benzenediolato(2- ))[2-(pyrrolidinio)ethyl]silicate (5; and its monohydrate 5 · H\(_2\)O) and bis[1,2-benzenediolato(2- )][( dimethylammonio)methyl]silicate (6) were synthesized by various methods including Si-C bond cleavage reactions. The crystal structures of 5, 5 · H\(_2\)O, and 6 were investigated by Xray d{\"u}fraction. Furthermore, 5, 5 · H\(_2\)O, 6, and the related zwitterionic \(\lambda_5\)-spirosilicates 1 · 1/4 CH\(_3\)CN, 2 · CH\(_3\)CN, 3 · CH\(_3\)CN, and 4 were characterized by solid-state NMR spectroscopy (\(^{29}\)Si and \(^{15}\)N CP/MAS). The pentacoordinate silicon atoms of 5, 5 · H\(_2\)O (two crystallographically independent ZWitterions and two crystallographically independent water molecules), and 6 (two crystallographically independent zwitterions) are surrounded by four oxygen atoms and one carbon atom. The coordination polyhedrons around the silicon atoms of 5 and 6 can be described as distorted (5) or nearly ideal (6) trigonal bipyramids, the carbon atoms being in equatorial positions. 5 forms intramolecular and 6 intermolecular (--+ formation of dimeric units) N- H···O hydrogen bonds. The coordination polyhedrons around the two crystallographically independent silicon atoms of 5 · H\(_2\)O can be described as a nearly ideal and slightly distorted square pyramid, respectively, the carbon atoms being in the apical positions. In the crystal lattice of 5 · H\(_2\)O, intermolecular N-H···O and 0-H···O hydrogen bonds between the zwitterions and water molecules are observed. The results obtained by X-ray diffraction and solid-state NMR spectroscopy are consistent for each compound studied.}, subject = {Anorganische Chemie}, language = {de} } @article{TackeBechtMatternetal.1992, author = {Tacke, Reinhold and Becht, J. and Mattern, G. and Kuhs, W. F.}, title = {Zur Existenz zwitterionischer \(\lambda_5\)-(Ammonioorganyl)tetrafluorosilicate: Synthese sowie Kristall- und Molek{\"u}lstruktur von Tetrafluoro(pyrrolidiniomethyl)silicat}, url = {http://nbn-resolving.de/urn:nbn:de:bvb:20-opus-64217}, year = {1992}, abstract = {The zwitterionic tetrafluoro(pyrrolidiniomethyl)silicate (6) was synthesized by the reaction of trimethoxy(pyrrolidinomethyl) silane (7) with hydrogen fluoride in ethanol/hydrofluoric acid (yield 83\%). 6 crystallizes in the space group P2\(_1\)fc with two crystallographically distinct molecules in the asymmetric unit. In both molecules the pentacoordinate silicon atom is surrounded by four fluorine atoms and one carbon atom, the latter being in an equatorial position. The coordination polyhedron of the silicon atoms can be described as a slightly distorted trigonal bipyramid. The zwitterionic structure was also proved for dissolved 6 (solution in CD\(_3\)CN, NMRspectroscopic studies).}, subject = {Anorganische Chemie}, language = {de} }