Blues et al. (1977) have reported the preparation, characterization, and crystal structure of tetrakis acetatotriphenyl phosphine silver(I). Tetrakis acetatotriphenyl phosphine silver(I) is reported to have monoclinic symmetry.I now report the preparation of silver(I) acetate bis-triphenyl phosphine complex from silver(I) ketenide and the preliminary elucidation of its crystal structure by X-ray diffraction techniques. Crystals of AgOAC · 2 PPh 3 were prepared by the reaction of tetragonal silver(I) ketenide (Ag 2 C 2 0) with an excess amount of triphenyl phosphine and refluxed for 15 h in toluene. The toluene phase was filtered from unreacted silver(I) ketenide, evaporated to dryness, and the resulting solid was recrystallized from toluene to give white crystals, m.p. 148 -150°C. The complex was characterized as CH 3 COOAg-2PPh 3 by elemental, infrared, mass spectra, and X-ray crystallographic analysis. The elemental analysis found C66.0 %, Η 4.73%, Ρ 8.12%, Ag 16.2%; Ag(0 2 CCH 3 ) (PPh 3 ) 2 requires C 66.0%, Η 4.78%, Ρ 8.97 %, Ag 15.6 %. The infrared spectrum showed acetate absorption bands at 1540 and 650 cm" 1 and phosphine absorption bands at 1587, 1195, 850, 720, and 690cm" 1 , respectively. Its mass spectrum showed the highest molecular ion peak at m/e = 692.The X-ray powder diffraction pattern of this material showed it to be highly crystalline, and so the X-ray single crystal analysis was carried out. A single crystal was mounted with a* axis parallel to the instrument axis of a General Electric XRD 5 apparatus which was used to measure diffraction intensities and cell dimensions.The preliminary investigations have shown the crystal to have a triclinic unit cell.The crystal data are as follows:= 691, triclinic, a = 10.06 Ä, b = 24.34 A, c = 13.83 A, α = 92.0°, β = 99.9°, y = 89.7°, U = 3334 A 3 , Ζ = 4, D m = 1.36, D c = 1.36 g cm" 3 , Motfoc radiation λ = 0.7107 A.