Synthesis, vibrational and NMR spectroscopic characterization of [N(CH3)4][[IO2F2] and X-ray crystal structure of [N(CH3)4]2[IO2F2][HF2]

被引:9
|
作者
Gerken, M [1 ]
Mack, JP
Schrobilgen, GJ
Suontamo, RJ
机构
[1] Univ Lethbridge, Dept Chem & Biochem, Lethbridge, AB T1K 3M4, Canada
[2] McMaster Univ, Dept Chem, Hamilton, ON L8S 4M1, Canada
[3] Univ Jyvaskyla, Dept Chem, FIN-40014 Jyvaskyla, Finland
关键词
iodine oxide fluorides; difluoroiodate; bifluoride; x-ray crystallography; vibrational spectroscopy; F-19 NMR spectroscopy;
D O I
10.1016/j.jfluchem.2004.09.005
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The salt, [N(CH3)(4)][IO2F2], was prepared from [N(CH3)(4)][IO3] and 49% aqueous HF, and characterized by Raman, infrared, and F-19 NMR spectroscopy. Crystals of [N(CH3)(4)](2)[IO2F2][HF2] were obtained by reduction of [N(CH3)(4)][cis-IO2F4] in the presence of [N(CH3)(4)][F] in CH3CN solvent and were characterized by Raman spectroscopy and single-crystal X-ray diffraction: C2/m, a = 14.6765(2) Angstrom, b = 8.60490(10) Angstrom, c = 13.9572(2) Angstrom, beta = 120.2040(10)degrees, V = 1523.35(3) Angstrom(3), Z = 4 and R = 0.0192 at 210 K. The crystal structure consists of two IO2F2- anions that are symmetrically bridged by two HF2- anions, forming a [F2O2I(FHF)(2)IO2F2](4-) dimer. The symmetric bridging coordination for the HF2- anion in this structure represents a new bonding modality for the bifluoride anion. (C) 2004 Elsevier B.V. All rights reserved.
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页码:1663 / 1670
页数:8
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