In situ single crystal growth of tris (trimethylsilyl)phosphate, (Me 3 SiO) 3 PO

(Me 3 SiO) 3 PO has been prepared by the reaction of Na[H 2 PO 4 ] and (Me 3 Si)Cl. Crystallization of the liquid was successful using an Optical Heating and Crystallization Device (OHCD) and allow the determination of the crystal structure of the compound (monoclinic, P 2 1 , Z=4), a =1016.67(6) pm, b =1053.70(6) pm, c =1759.2(1) pm, β =91.916(2)°, w R 2 =0.0979). The molecular structure shows the phosphorous atom tetrahedrally coordinated by three (Me 3 SiO) groups and one oxygen atom. The compound can be seen as a missing link between the related cation and anion [(Me 3 SiO) 4 P] + and [(Me 3 SiO) 2 PO 2 ] − , respectively.