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.

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The XRD studies were carried out using the scientific equipment of the Center for Molecular Composition Studies of the Nesmeyanov Institute of Organoelement Compounds (Russian Academy of Sciences) supported by the Ministry of Science and Higher Education of the Russian Federation. The authors are grateful to A.N. Bilyachenko for the kindly presented tetramethoxysilane sample.


This work was supported by the Russian Science Foundation, project no. 18-73-00257.

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Correspondence to Yu. V. Nelyubina.

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Translated by E. Yablonskaya

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Smol’yakov, A.F., Nelyubina, Y.V. Phase Transition in the Crystal of Tetramethoxysilane Studied by In Situ X-ray Diffraction Analysis. Russ J Coord Chem 47, 26–31 (2021).

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  • viscous liquids
  • zone smelting
  • organosilanes
  • X-ray diffraction analysis
  • crystal growth
  • phase transition
  • organoelement compounds
  • in situ crystallization