TITLE:
A Facile Route to Phosphanylborohydrides:Synthesis, Crystal Structure and Spectroscopic Properties of 1,2-Bis(Diphenylphosphinoborane)Ethane
AUTHORS:
Leyla Tatar Yildirim, Mehdi Masjedi, Saim Özkar
KEYWORDS:
Crystal Structure, Synthesis, Phosphinoborane, Sodium Borohydride, Phosphanylborohydride, X-Ray Diffraction
JOURNAL NAME:
Journal of Crystallization Process and Technology,
Vol.1 No.1,
March
16,
2011
ABSTRACT: A novel and simple synthetic way using NaBH4 in the mixure of H2O-THF was applied to prepare 1,2-bis(diphenylphosphinoborane)ethane, dppe(BH3)2, in high yield and purity. The phosphanylborohydride compound dppe(BH3)2 was isolated in the form of colorless crystals and characterized by single crystal X-ray diffraction, 1H, 13C, 31P and 11B NMR spectroscopy. Prismatic colorless crystals of dppe(BH3)2 were obtained in monoclinic crystal system and space group P21 with two asymmetric units in the unit cell. Lattice parameters were: a = 11.657(2), b = 17.237(2), c = 12.764(2) Å, β = 98.735(14)°, 2535.0(7) Å3