The structure of trimethyltin fluoride
Date
2015
Authors
Chaudhary, Praveen
Bieringer, Mario
Hazendonk, Paul
Gerken, Michael
Journal Title
Journal ISSN
Volume Title
Publisher
Royal Society of Chemistry
Abstract
The solid-state structure of (CH3)3SnF was reinvestigated by X-ray diffraction techniques as well as by multi-nuclear solid-state NMR spectroscopy. Trimethyltin fluoride crystallizes from hot ethanol in the orthorhombic space group Pnma at room temperature and changes to a low-temperature orthorhombic phase (space group: Cmcm) below −70 °C. In both modifications, trimethyltin fluoride adopts a linear chain structure with symmetric fluorine bridges, in contrast to previous reports. During its synthesis, (CH3)3SnF precipitates in another, poorly crystalline modification, as shown by powder X-ray diffraction. Solid-state MAS NMR experiments of both room-temperature phases of (CH3)3SnF (non-recrystallized and recrystallized) were carried out for the 1H, 13C, 19F, and 119Sn nuclei. The 119Sn{19F, 1H} and 19F{1H} NMR spectra offer unambiguous determination for the 19F and 119Sn shielding tensors. The 119Sn{1H} solid-state NMR spectra are in agreement with pentacoordination of Sn in this compound for the non-recrystallized and the recrystallized modifications. Based on the solid-state NMR results, the non-recrystallized modification of (CH3)3SnF also consists of linear, symmetrically fluorine-bridged chains, and differs from the recrystallized orthorhombic phase only in packing of the chains.
Description
Accepted author manuscript
Keywords
Trimethyltin fluoride , NMR spectroscopy
Citation
Chaudhary, P., Bieringer, M., Hazendon, P., & Gerken, M. (2015). The structure of trimethyltin fluoride. Dalton Transactions, 44, 19651-19658. https://doi.org/10.1039/C5DT01994J