Alkali Metal Bis(o-anisyl)phosphides: Characterization of MP(C(6)H(4)OMe-o)(2) (M = Li, Na) and Crystal Structure of a Sodium Secondary Organophosphide.
Lithium bis(o-anisyl)phosphide (1)may be prepared by reaction of n-BuLi with bis(o-anisyl)phosphine in THF or toluene; sodium bis(o-anisyl)phosphide (2) is prepared by reaction of sodium with tris(o-anisyl)phosphine in liquid ammonia/THF; both compounds are isolated as unsolvated solids. 1 decomposes quantitatively in THF to give tetrakis(o-anisyl)diphosphine (4); 2 decomposes in THF to give a mixture containing 4 and bis(o-anisyl)phosphine. Addition of diglyme to 2 gives [Na{&mgr;-P(C(6)H(4)OMe-o)(2)}(MeO(CH(2)CH(2)O)(2)Me)](2) (2a), which has been characterized by single-crystal X-ray diffraction. Each Na atom in 2a is 6-coordinate, being bonded to two P atoms, three diglyme O atoms, and one O atom from an o-anisyl group. Crystal data: monoclinic, P2(1)/n, a = 14.549(4) Å, b = 18.555(6) Å, c = 15.846(4) Å, beta = 91.07(2) degrees, Z = 4, final R = 0.041, R(w) = 0.053.
Aspinall
Helen C.
HC
Department of Chemistry, University of Liverpool, P.O. Box 147, Liverpool L69 3BX, U.K.
Tillotson
Martin R.
MR