Phase Transition in the Crystal of Tetramethoxysilane Studied by In Situ X-ray Diffraction Analysis

Single crystals of tetramethoxysilane (I), which is liquid at room temperature, are grown using an original setup for in situ crystallization. The X-ray diffraction analysis of compound I at two temperatures (CIF files CCDC nos. 2006156 and 2006157 for 150 and 200 K, respectively) shows the phase transition accompanied by the disordering of the methoxy groups. The setup developed that is different from commercial analogs by an unusually low cost and a possibility of modifying all components provides wide opportunities for crystal growth directly on a diffractometer for structure determination of various organoelement compounds and, possibly, metal complexes in the liquid or even gaseous state.