NDLI: Reactions with Oleum under Harsh Conditions: Characterization of the Unique $[M(S_{2}O_{7})_{3}]^{2−}$ Ions (M=Si, Ge, Sn) in $A_{2}[M(S_{2}O_{7})_{3}]$ $(A=NH_{4},$ Ag)

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Reactions with Oleum under Harsh Conditions: Characterization of the Unique $[M(S_{2}O_{7})_{3}]^{2−}$ Ions (M=Si, Ge, Sn) in $A_{2}[M(S_{2}O_{7})_{3}]$ $(A=NH_{4},$ Ag)

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Reactions with Oleum under Harsh Conditions: Characterization of the Unique $[M(S_{2}O_{7})_{3}]^{2−}$ Ions (M=Si, Ge, Sn) in $A_{2}[M(S_{2}O_{7})_{3}]$ $(A=NH_{4},$ Ag)

Content Provider	World Health Organization (WHO)-Global Index Medicus
Author	Logemann, Christian Wickleder, Mathias S. Klüner, Thorsten Gunzelmann, Daniel Senker, Jürgen
Description	Author Affiliation: Logemann C ( Carl von Ossietzky University of Oldenburg, Institute of Pure and Applied Chemistry, Carl-von-Ossietzky-Strasse 9-11, 26129 Oldenburg, Germany.)
Abstract	The reactions of group 14 tetrachlorides $MCl_{4}$ (M=Si, Ge, Sn) with oleum (65 % $SO_{3})$ at elevated temperatures lead to the unique complex ions $[M(S_{2}O_{7})_{3}]^{2−},$ which show the central M atoms in coordination with three chelating $S_{2}O_{7}^{2−}$ groups. The mean distances MO within the anions increase from 175.6(2)–177.5(2) pm (M=Si) to 186.4(4)–187.7(4) pm (M=Ge) to 201.9(2)–203.5(2) pm (M=Sn). These distances are reproduced well by DFT calculations. The same calculations show an increasing positive charge for the central M atom in the row Si, Ge, Sn, which can be interpreted as the decreasing covalency of the MO bonds. For the silicon compound $(NH_{4})_{2}[Si(S_{2}O_{7})_{3}],$ $^{29}Si$ solid-state NMR measurements have been performed, with the results showing a signal at −215.5 ppm for $(NH_{4})_{2}[Si(S_{2}O_{7})_{3}],$ which is in very good agreement with theoretical estimations. In addition, the vibrational modes within the $[MO_{6}]$ skeleton have been monitored by Raman spectroscopy for selected examples, and are well reproduced by theory. The charge balance for the $[M(S_{2}O_{7})_{3}]^{2−}$ ions is achieved by monovalent $A^{+}$ counter ions $(A=NH_{4},$ Ag), which are implemented in the syntheses in the form of their sulfates. The sizes of the $A^{+}$ ions, that is, their coordination requirements, cause the crystallographic differences in the crystal structures, although the complex $[M(S_{2}O_{7})_{3}]^{2−}$ ions remain essentially unaffected with the different $A^{+}$ ions. Furthermore, the nature of the $A^{+}$ ions influences the thermal behavior of the compounds, which has been monitored for selected examples by thermogravimetric differential thermal analysis (DTA/TG) and XRD measurements.
ISSN	09476539
e-ISSN	15213765
Journal	Chemistry - A European Journal
Issue Number	48
Volume Number	18
Language	English
Publisher	Wiley-VCH;ChemPubSoc Europe
Publisher Date	2012-11-26
Publisher Place	Germany
Access Restriction	Open
Subject Keyword	Chemistry
Content Type	Text
Resource Type	Article
Subject	Organic Chemistry Catalysis

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