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The structure of trimethyltin fluoride.

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This study reinvestigated trimethyltin fluoride ((CH3)3SnF) structure using X-ray diffraction and solid-state NMR. Both room-temperature and low-temperature phases exhibit linear chains with symmetric fluorine bridges, clarifying previous structural discrepancies.

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Area of Science:

  • Solid-state chemistry
  • Materials science
  • Organometallic chemistry

Background:

  • Trimethyltin fluoride ((CH3)3SnF) is an organometallic compound with potential applications.
  • Previous structural studies of (CH3)3SnF have yielded conflicting results.
  • Understanding the precise solid-state structure is crucial for predicting its properties and reactivity.

Purpose of the Study:

  • To accurately determine the solid-state structure of trimethyltin fluoride ((CH3)3SnF) using advanced analytical techniques.
  • To resolve discrepancies in previous structural reports of (CH3)3SnF.
  • To elucidate the structural differences between synthesized and recrystallized forms of (CH3)3SnF.

Main Methods:

  • X-ray diffraction (single-crystal and powder) was employed to analyze crystal structures.
  • Multi-nuclear solid-state Magic Angle Spinning (MAS) Nuclear Magnetic Resonance (NMR) spectroscopy was performed on (1)H, (13)C, (19)F, and (119)Sn nuclei.
  • Solid-state NMR experiments, including (119)Sn{(19)F, (1)H} and (19)F{(1)H} cross-polarization, were used to determine shielding tensors.

Main Results:

  • Trimethyltin fluoride ((CH3)3SnF) crystallizes in an orthorhombic Pnma space group at room temperature and transitions to a Cmcm space group below -70 °C.
  • Both crystalline forms feature linear chains with symmetric fluorine bridges, contradicting earlier findings.
  • A poorly crystalline modification forms during synthesis, differing from recrystallized phases primarily in chain packing.
  • (119)Sn NMR data indicates pentacoordination of tin in both non-recrystallized and recrystallized modifications.

Conclusions:

  • The solid-state structure of trimethyltin fluoride ((CH3)3SnF) consists of linear, symmetrically fluorine-bridged chains in both investigated room-temperature phases.
  • The primary difference between synthesized and recrystallized (CH3)3SnF lies in the packing arrangement of these chains.
  • This reinvestigation clarifies the structural ambiguity of (CH3)3SnF, providing a foundation for further studies.