POLYSULFONYLAMINES .43. TRIMETHYLGERMANIU M(IV) AND TRIMETHYLLEAD(IV)DIMESYLAMIDE - SYNTHESIS AND SOLID-STATE STRUCTURES

The new compounds Me3GeN(SO2Me)2 (3) and Me3PbN(SO2Me)2 (4) were prepa red from the corresponding chlorides Me3ECl and AgN(SO2Me)2 in MeCN so lution. The crystallographic data at -95-degrees-C are for 3: triclini c, space group P1BAR. a 771.7(2), b 1204.1(4), c 1388.4(5) pm, alpha 6 6.75(3), beta 84.12(3), gamma 74.15(2)-degrees, V 1.1401 nm3. Z = 4; f or 4: monoclinic, space group P2(1)/c, a 751.1(3), b 1065.5(4), c 1493 .9(5) pm, beta 100.99(3)-degrees, V 1.1738 nm3, Z = 4. The crystal str ucture of 3 consists of two crystallographically independent, monomeri c molecules with tetrahedral Ge atoms and trigonal-planar N atoms (ave rage angle values: C-Ge-C 112.7, C-Ge-N 106.0, Ge-N-S 121.1, S-N-S 117 .3-degrees). The most striking features of the molecular structure are the extremely long Ge-N bond distances of 198.2(2) and 198.5(2) pm, w hich are equal to the uncorrected sum of the covalent single bond radi i. In the crystal structure of 4, Me3PbN(SO2Me)2 units are linked by a n intermolecular Pb-O interaction (265.3(6) pm) to form infinite paral lel chains. The Pb atom has a distorted trigonal-bipyramidal arrangeme nt (N-Pb-O 169.3: average values: C-Pb-C 119.2, C-Pb-N 95.5, C-Pb-0 84 .8-degrees), in which the N atom is trigonal-planar (S-N-S 119.2, mean Pb-N-S 119.8-degrees). The Pb-N distance is 248.4(6) pm, i.e. 30 pm l onger than the sum of the covalent radii, suggesting a mainly ionic bo nd character. In both structures secondary intramolecular 1,4-interact ions with Ge...O distances of 295.8 and Pb...O of 328 pm, respectively , are observed.