Solid Me3Sn(O2CH): molecular and spin dynamics as viewed by 1H, 13C and 119Sn nuclear magnetic resonance spectroscopy

• Published in: Solid state nuclear magnetic resonance 1994-06, Vol.3 (3), p.137-152
• Main Authors: Kümmerlen, J, Sebald, A
• Format: Article
• Language: English
• Subjects: Anisotropy; Magnetic Resonance Spectroscopy; Temperature; Trimethyltin Compounds - chemistry
• ISSN: 0926-2040
• DOI: 10.1016/0926-2040(94)90009-4

Because of favourable dynamic properties in the solid state, crystalline trimethyltin formate, Me3Sn(O2CH), 1, offers quite unique possibilities to probe questions related to molecular dynamics (2 pi/3 Me3Sn reorientation) and to structural aspects (rigidity of the polymeric backbone, effectively isolated 1H-13C spin pair in the bidentate chain-building formate anion) by 1H, 13C and 119Sn high-resolution solid-state nuclear magnetic resonance (NMR) methods. The combined use of various one- (1D) and two-dimensional (2D) variable-temperature NMR experiments, including consideration of the short-time-cross-polarization (CP) behaviour of the 1H-13C spin pair in 13C-labelled Me3Sn(O2*CH), 1*, yields a fairly comprehensive description of the solid-state structure of 1, also in the absence of the single-crystal X-ray structure determination of 1. Taking advantage of the anisotropic polarization transfer within the formate 1H-13C spin pair allows to relate the orientation of the 1H-13C dipolar interaction, i.e. the C-H bond direction to the principal axes system of the 13C shielding tensor of the formate 13C from static 13C powder patterns of 1*.