Polysulfonylamine: XLIII. Trimethylgermanium(IV)- und Trimethylblei(IV)-dimesylamid: Synthese und Festkörperstrukturen

Abstract

The new compounds Me 3GeN(SO 2Me) 2 ( 3) and Me 3PbN(SO 2Me) 2 ( 4) were prepared from the corresponding chlorides Me 3ECl and AgN(SO 2Me) 2 in MeCN solution. The crystallographic data at −95°C are for 3: triclinic, space group P 1 , a 771.7(2), b 1204.1(4), c 1388.4(5) pm, α 66.75(3), β 84.12(3), γ 74.15(2)°, V 1.1401 nm 3, Z = 4; for 4: monoclinic, space group P2 1/ c, a 751.1(3), b 1065.5(4), c 1493.9(5) pm, β 100.99(3)°, V 1.1738 nm 3, Z = 4. The crystal structure of 3 consists of two crystallographically independent, monomeric molecules with tetrahedral Ge atoms and trigonal- planar N atoms (average angle values: CGeC 112.7, CGeN 106.0, GeNS 121.1, SNS 117.3 °). 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, which are equal to the uncorrected sum of the covalent single bond radii. In the crystal structure of 4, Me 3PbN(SO 2Me) 2 units are linked by an intermolecular PbO interaction (265.3(6) pm) to form infinite parallel chains. The Pb atom has a distorted trigonal-bipyramidal arrangement (NPbO 169.3; average values: CPbC 119.2, CPbN 95.5, CPbO 84.8°), in which the N atom is trigonal-planar (SNS 119.2, mean PbNS 119.8°). The PbN distance is 248.4(6) pm, i.e. 30 pm longer than the sum of the covalent radii, suggesting a mainly ionic bond character. In both structures secondary intramolecular 1,4-interactions with Ge ⋯ O distances of 295.8 and Pb ⋯ O of 328 pm, respectively, are observed.