Dimethylantimonazid: Synthese, Spektren und Kristallstruktur Dimethylbismutazid: Synthese und Kristallstruktur Trimethylbleiazid: Verfeinerung der Kristallstruktur / Dimethyl Antimony Azide: Preparation, Spectra and Crystal Structure Dimethyl Bismut Azide: Synthesis and Crystal Structure Trimethyl Lead Azide: Refinem ent of the Crystal Structure

Abstract

Reaction of Me2SbBr or Et2SbBr with AgN3 in ether affords Me2SbN3 and Et:SbN3. respectively. Me2SbN3 can also be obtained from Me2SbNMe2 and HN3 in ether. Me2BiN3 from Me2BiN(SiMe3)3 and HN3 in ether. Me2SbN3 and Et2SbN3 dissolve as monomers in benzene; 1H, 13C, iaN and 15N NMR spectra of the solutions are reported. IR and Raman spectra of solid Me2SbN3 and Et2SbN, as well as the mass spectrum of Me2SbN3 are assigned. The crystal structures of Me2SbN3 and Me2BiN3 were determined by X-ray diffraction data collected at -67 °C (888 and 439 reflexions, R = 0.024 and 0.076. respectively). Both compounds are isotypic, space group Pnma. Z = 4. Crystal data: Me2SbN3, a = 843.6. b = 919.3, c = 744.1 pm: Me2BiN3, a - 870.8. b = 911.3, c = 738.4 pm. In the crystals, the metal atoms are linked via the aN atoms of the azido groups to form endless zig-zag chains. Whereas the Bi -N distances are equal. Sb-N bonds alternate with two different lengths (232 and 243 pm). Including the lone pair of electrons, the metal coordination can be described as distorted trigonal bipyramidal, with nitrogen atoms occupying the apical positions. With new X-ray diffraction data collected at -100 °C, the crystal structure of Me3PbN3 was refined (1692 reflexions, R = 0.036). Crystal data: a = 656.3, c = 1377 pm. space group P3221, Z = 3. It consists of endless metal-nitrogen chains of helical symmetry. the Pb atoms having trigonal bipyramidal coordination.