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-BuSnCl3 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)(nBu)(center dot 1/2) toluene. Complex 1 crystallizes in the triclinic P (1) over bar space group, with Z = 2, a = 8.0496(8) angstrom, b = 9.4867(9) angstrom, c = 14.2710(14) angstrom, alpha = 90.365(3)degrees, beta = 104.479(3)degrees, gamma = 95.066(3)degrees, and V = 1050.60(18)angstrom(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 (pi-pi, C-H center dot center dot center dot pi, and C-H center dot center dot center dot 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.