Organotin(IV) scorpionates – X-ray structure and crystal packing of TpSn(Cl) ₂( n-Bu) [Tp=hydrotris(pyrazol-1-yl)borate]

摘要

Reaction of potassium hydrotris(pyrazol-1-yl)borate ( KTp ) and n -BuSnCl_(3)at room temperature led to the quantitative formation of TpSn(Cl)_(2)( n -Bu) ( 1 ). Colorless single crystals were obtained from a mixture of toluene/dichloromethane and were characterized as TpSn(Cl)_(2)( n -Bu)·? toluene. Complex 1 crystallizes in the triclinic P 1? space group, with Z =2, a =8.0496(8) ?, b =9.4867(9) ?, c =14.2710(14) ?, α =90.365(3)°, β =104.479(3)°, γ =95.066(3)°, and V =1050.60(18) ?~(3). Its structure exhibits a piano stool conformation involving a distorted octahedral geometry around the central Sn(IV) atom. In the crystal and from a supramolecular point of view, 1 is organized in pairs according to a V-shaped arrangement implicating pyrazolyl rings and through weak intermolecular interactions ( π-π , C-H··· π , and C-H···Cl). The structural analysis of 1 was completed by infrared and solution NMR spectroscopy measurements as well as elemental analysis, which confirm the X-ray elucidation.