STRUCTURE OF [HTMPP]3W2CL9 [HTMPP = TRIS(2,4,6-TRIMETHOXYPHENYL)-PHOSPHONIUM]

Tris(2,4,6-trimethoxyphenyl)phosphonium nonachloroditungstate(III)-pyridine-tetrahydrofuran (1/2/1), 3C27H34O9P+.W2Cl9(3-).2C5H5N.C4H4O (1), M(r) = 2513.7, triclinic, P1BAR, a = 16.993 (5), b = 24.746 (9), c = 14.094 (4) angstrom, alpha = 95.170 (2), beta = 111.690 (2), gamma = 87.630 (3)-degrees, V = 5484 (3) angstrom 3, Z = 2, D(x) = 1.522 g cm-3, gamma(Mo K-alpha) = 0.71073 angstrom, mu = 24.7 cm-1, F(000) = 2540, T = 295 K, R = 0.057 for 9260 unique reflections total with F(o)2 > 3-sigma(F(o)2). The asymmetric unit is composed of one triply bonded confacial bioctahedral [W2Cl9]3- dimer with three crystallographically independent protonated phosphine counterions, HTMPP+, and three interstitial solvent molecules (two pyridines and one tetrahydrofuran). The W-W distance is 2.4329 (6) angstrom, the average W-Cl bridging distance is 2.490 (6) angstrom, and the average W-Cl terminal distance is 2.414 (6) angstrom.