SYNTHESES OF SOME 10-ATOM, 11-ATOM, AND 12-ATOM PHOSPHABORANES - CRYSTAL-STRUCTURE OF 2-(TRIMETHYLAMINE)-1-PB11H10

The heteroboranes 1,2-PAsB10H10 and 1,2-PSbB10H10 were prepared in low yield by reaction of B10H14 with triethylamine and mixtures Of PCl3 a nd AsCl3 Or PCl3 and SbI3, respectively. From the product mixture in t he related synthesis of 1,2-P2B10H10, the phosphaborane anion 2-PB9H9 has been isolated. Treatment of 1,2-P2B10H10 with excess piperidine fo rmed the 7,8-P2B9H10- ion in good yield. Treatment of Me3NH[B11H14] wi th excess n-butyllithium and PCl3 formed both B11H11P- and 2-NMe3-1-PB 11H10 in moderate yield. The compound 2-NMe3-1-PB11H10 has been charac terized by a single-crystal X-ray structure determination (space group P2(1)/m, a 6.910(1) angstrom, b = 10.603(1) angstrom, c = 8.821(1) an gstrom, beta = 108.27(1)-degrees, Z = 2).