Synthesis and Crystal and Molecular Structure of Tris(dimethylphenylsilyl)antimony

Tris(dimethylphenylsilyl)antimony (1) was prepared in moderate yield from dimetallic “Na₃Sb” (generated in situ) and chlorodimethylphenylsilane in tetrahydrofuran at reflux temperature. The product was identified by standard analytical and spectroscopic techniques, and the crystal structure was determined by single‐crystal X‐ray diffraction (triclinic, space group P1, Z = 2). The SbSi₃ skeleton is pyramidal (average Si‐Sb‐Si angle 100.2°, average Sb‐Si bond length 2.558 Å), and the Me₂PhSi groups are in a staggered conformation.