POLYSULFONYLAMINES .38. PREPARATION AND SOLID-STATE STRUCTURE OF BIS(TRIMETHYLTIN)DIMESYLAMIDE HYDROXIDE [ME3SN(MU-(MESO2)2N)ME3SN(MU-OH)]N

The title compound 1 is obtained from equimolar amounts of Me3SnN(SO2Me)2 (2) and Me3SnOH in ethanol or by partial hydrolysis of 2 in CH2Cl2 solution and in presence of a nitrogen base, e.g. pyridine. 1 crystallizes in the triclinic space group P1BAR with (at -95-degrees-C) a = 825.4(3), b = 856.2(3), c = 1341.6(5) pm, alpha = 81.97(3), beta = 74.72(3), gamma = 79.75(3)-degrees, U = 0.8958 nm3, Z = 2. The structure consists of infinite chains, in which Me3Sn groups are bridged by alternating O(H) and (alpha-O, omega-O)-bonded dimesylamide groups. Antiparallel chains are interconnected by O-H ... N hydrogen bonds to form a ''ladder'' structure. There are two independent tin atoms. The Sn-O(H) distances are 211.8(2) and 212.6(2) pm, the Sn-O(S) distances 268.2(2) and 253.3(2) pm, the O(H)-Sn-O(S) angles 174.5(1) and 173.8(1)-degrees, and the Sn-O(H)-Sn angle is 136.9(1)-degrees. In the trigonal-bipyramidal (C3O2) environment of the tin atoms, the C-Sn-C angles are slightly smaller than 120-degrees, the O(H)-Sn-C angles significantly greater than 90-degrees, and the O(S)-Sn-C angles correspondingly smaller than 90-degrees. Thus, the chain structure might reasonably be viewed as consisting of [(Me3Sn)2OH]+ ions alternating with [(MeSO2)2N]- ions.