Crystal Structure, Vibrational Spectra. Mass Spectra. Diethyltin Bis(diphenylphosphinate) Et2S n (0 2PPh2)2 has been synthesized by the reaction of (Et2ClSn)20 with Ph2POCl in toluene and by the treatment of (Et2ClSn)20 or Et2SnCl2 with H 0 2PPh2 in methanol. The reaction of Et2SnO with H 0 2PM e2 in toluene was used to prepare Et2S n (0 2PM e2)2. An Xray diffraction study of Et2S n (0 2PPh2)2 (space group P i, Z = 1, a = 559,9( 1), b = 983,7(1), c = 1262,4(l)pm , a = 81,85( 1 )°,/3 = 79,79( 1)°,7 = 75,00(1)°; structure refinement with 2662 independent reflections, R = 0.055) shows that the structure is polymeric and the 0 2PPh2 ligands function as double bridges between the tin atoms leading to the formation of centrosymmetric Sn20 4P2 eight-membered rings. The ethyl groups are in /ra«s-position in the resulting octahedral environment around tin. The I. R. and Raman spectra of Et2S n (0 2PR2)2 (R = Ph, Me) have been discussed and assigned. The mass spectra of Et2S n (0 2PR2)2 show S n (0 2PR2)+ as the base peak.