Synthesis and crystal structure of a new supermolecular compound: [C 12 H 24 O 6 ][H 3 PMo 12 O 40 ]·22H 2 O (C 12 H 24 O 6 =18-crown-6)
2000; Elsevier BV; Volume: 524; Issue: 1-3 Linguagem: Inglês
10.1016/s0022-2860(99)00447-0
ISSN1872-8014
AutoresWan‐Sheng You, Enbo Wang, Qinglin He, Lin Xu, Xingbin Yan, Heng‐Qing Jia,
Tópico(s)Vanadium and Halogenation Chemistry
ResumoThe title compound, [C12H24O6][H3PMo12O40]·22H2O, was synthesized by the self-assembly of 18-crown-6 (abbreviated as C12H24O6 or 18C6) and H3PMo12O40 in the mixed solvent of CH3OH and CH3CN, and was characterized by IR, 1H NMR and X-ray diffraction for the first time. Crystal data: Triclinic, P1̄,a=13.428(3)Å,b=13.557(3)Å,c=14.642(3)Å,α=105.39(3)°, β=90.06(3)°, γ=119.56(5)°, V=2207.5(8)Å3,Z=1, R1=0.0719, wR2=0.1990. It has a disordered α-Keggin PMo12O403− anion, which contains the strong alternating short (mean 1.844 Å) and long (mean 1.958 Å) Mo–O–Mo bonds. In the unit cell, crown ethers and molybdophosphates are alternatively arranged 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 hydrogen bonds (mean 2.7771 Å), which are electrostatic or resonant. The observations show the existence of [H3O(C12H24O6)]+.
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