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Pentaphenylphosphorus crystallizes from tetrahydrofuran (THF) as P(C 6 H 5 ) 5 ・0.5 THF (triclinic space group: P1̅, a = 10.095(4), b = 10.252(3), c = 12.725(3) A° , α = 71.21(1), β = 76.98(3), γ = 87.12(1)°, Z = 2). Its molecular structure is an almost perfect trigonal bipyramid with significantly longer axial than equatorial P-CPh bonds (P-C ax  1.982(2)/1.979(2), P-C eq  1.853(2)/1.845(2)/1.847(2) Å). It differs from the well established structure of solvent-free P(C 6 H 5 ) 5  (P. J. Wheatley, J. Chem. Soc. 2206 (1964)) in the relative orientation of the phenyl rings with respect to each other (axial rings) and with respect to the equatorial PC 3  plane (equatorial rings) but not in the trigonal-bipyramidal (tbp) geometry at phosphorus. Differences in the geometry around the central atom had been found previously for Sb(C 6 H 5 ) 5  (square pyramid) and Sb(C 6 H 5 ) 5  · 0.5C 6 H 12  (tbp) but not in As(C 6 H 5 ) 5  and As(C 6 H 5 ) 5  · 0.5 C 6 H 12  (both tbp).

Crystal and Molecular Structure of P(C 6 H 5 ) 5 · 0.5 THF