The reaction of pentaphenylantimony with triphenylantimony dinitrate in toluene gives tetraphenylantimony nitrate in 99% yield. The X-ray diffraction data show that the antimony atom in the molecule of tetraphenyl antimony nitrate has a distorted trigonal-bipyramidal coordination with axial location of the oxygen atom of the nitrate group. The Sb-O, Sb-ax, and Sb-C-eq bond lengths in two independent molecules of tetraphenylantimony nitrate are 2.498(3), 2.548(2); 2.134(3), 2.138(3); and 2.101(3)-2.112 Angstrom.