Synthesis of Halogenated Polyhedral Phosphaboranes. Crystal Structure of closo-1,7-P2B10Cl10
- Publication Type
- Journal contribution
- Authors
- Keller, W.; Sawitzki, G.; Haubold, W.
- Year of publication
- 2000
- Published in
- Inorg. Chem.
- Band/Volume
- 39/6
- DOI
- 10.1021/ic990112v
- Page (from - to)
- 1282-1287
The 12-vertex closo-phosphaborane 1,7-P2B10Cl10 (1) was prepd. in low yield from the pyrolysis reaction of B2Cl4 with PCl3 at temps. >400.degree.. A single-crystal x-ray structure detn. of 1 (monoclinic space group P21/n with a 9.239(2), b 16.786(3), c 15.739(3) .ANG., .beta.93.25(3).degree., and Z = 4) confirmed that, consistent with its 26 skeletal electron count, the phosphaborane adopts a distorted icosahedral structure with the P atoms in the 1,7-positions. Crystals of 1 contain toluene in a 1:1 molar ratio embedded between each P atom of neighboring cluster mols. Alteration of the pyrolytic conditions gave the phosphaboranes P4B8Cl6 (2) and P2B8Cl8 (3), which were characterized spectroscopically. Copyrolysis of B2Cl4 with a mixt. of PCl3 and AsCl3 at 450.degree. generated the six-vertex arsaphosphaborane AsPB4Cl4 (4) and traces of the icosahedral arsaphosphaborane AsPB10Cl10. These compds. are examples of heteroboranes which contain two different group-15 atoms within a single mol.