Synthesis and crystal structure of a new supermolecular compound: [C12H24O6][H3PMo12O40]center dot 22H(2)O (C12H24O6=18-crown-6)

The title compound, [C12H24O6][H3PMo12O40]. 22H(2)O, was synthesized by the self-assembly of 18-crown-6 (abbreviated as C12H24O6 or 18C6) and H3PMo12O 40 in the mixed solvent of CH3OH and CH3CN, and was characterized by IR, H- 1 NMR and Xray diffraction for the first time. Crystal data: Triclinic, P ( 1) over bar, a = 13.428(3) Angstrom, b = 13.557(3)A, c = 14.642(3) Angstrom , a = 105.39(3)degrees, beta = 90.06(3)degrees, gamma = 119.56(5)degrees, V = 2207.5(8) Angstrom(3), Z = 1, R1 = 0.0719, wR2 = 0.1990. It has a disord ered alpha-Keggin PMo12O403- anion, which contains the strong alternating s hort (mean 1.844 Angstrom) and long (mean 1.958 Angstrom) Mo-O-Mo bonds. In the unit cell, crown ethers and molybdophosphates are alternatively arrang ed in good order along c-axis. An oxonium ion is located at the center of a crown ether molecule., Oxonium ion interacts with 18C6 by the means of hyd rogen bonds (mean 2.7771 Angstrom), which are electrostatic or resonant. Th e observations show the existence of [H3O(C12H24O6)](+) (C) 2000 Elsevier S cience B.V. All rights reserved.