The complex [Ph 2 Si(OSnf-Bu 2 ) 2 Of-Bu 2 Sn(OH) 2 ] (2) was obtained in high yield by reaction of Ph 2 Si(OH) 2 with (f-Bu 2 SnO) 3 (1). Reaction of f-Bu 2 Si(OH) 2 with 1 gave [t-Bu 2 Si(0Snf-Bu 2 ) 2 0] (4a) instead. The compounds were investigated by means of NMR, IR, MOssbauer spectroscopy, and in case of 2 by X-ray analysis. In solution, 2 is in equilibrium with [Ph 2 Si(0Snf-Bu 2 ) 2 0] (2a), 1, and water. i-Bu 2 Sn(OH) 2 (3) was prepared by controlled hydrolysis of f-Bu 2 Sn(OMe) 2 and was shown to undergo condensation with formation of 1. Mössbauer studies as well as 11 ®Sn CP MAS NMR including side band analysis suggest 3 to exhibit a dimeric structure with pentacoordinate tin. Similar studies on 1 suggest fast rotation of the molecule in the crystal lattice. Abstract (f-Bu 2 SnO) 3 + Ph 2 Si(OH) 2 1 toluene, 60° C, 1d [Ph 2 Si(0Snf-Bu2)2Of-Bu 2 Sn(0H)2] (1) 2 113 Brought to you by | Purdue University Libraries Authenticated Download Date | 6/11/15 12:28 AMThe 119 Sn CP MAS NMR spectrum of 2 shows two signals at -265.7 and -273.7 ppm, respectively, with an integral ratio of 1:2 which is in line with the structure established by the X-ray measurement. The IR spectrum shows the presence of the OH groups by a (OH) of 3644 cm" 1 .