[Li(tmeda)2][cyclo-(P5But4)]: An unusual ion-separated lithium oligophosphanide
摘要:
The reaction of lithium with (BuPCl2)-P-t and PCl3 in the ratio 12:4:1 in THF gave a product mixture comprising cyclo-(P4Bu4t), Li-2(P4Bu4t), and lithium tetra-tert-butylcyclopentaphosphanide Li[cyclo-(P5Bu4t)] (1) among other phosphanides and phosphanes. Optimization of the reaction conditions and recrystallization from THF/TMEDA (TMEDA: Me2NCH2CH2NMe2) gave [Li(tmeda)(2)][cyclo-(P5Bu4t)] (1b) which was characterized by multinuclear NMR spectroscopy, mass spectrometry. IR spectroscopy, and elemental analysis. Single-crystal X-ray diffraction studies showed the presence of separated [Li(tmeda)(2)](+) cations and [cyclo-(P5Bu4t)](-) anions. 1b represents the first structure of a "naked" [cyclo-(P5Bu4t)](-) anion. (C) 2010 Academie des sciences. Published by Elsevier Masson SAS. All rights reserved.