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Synthesis, vibrational and NMR spectroscopic characterization of [N(CH3)4][IO2F2] and X-ray crystal structure of [N(CH3)4]2[IO2F2][HF2] |
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| Authors: | Michael Gerken Johnathan P Mack Reijo J Suontamo |
| Institution: | a Department of Chemistry and Biochemistry, University of Lethbridge, Lethbridge, AB T1K 3M4, Canada b Department of Chemistry, McMaster University, Hamilton, ON L8S 4M1, Canada c Department of Chemistry, University of Jyväskylä, P.O. Box 35, FIN-40014 Jyväskylä, Finland |
| Abstract: | The salt, N(CH3)4]IO2F2], was prepared from N(CH3)4]IO3] and 49% aqueous HF, and characterized by Raman, infrared, and 19F NMR spectroscopy. Crystals of N(CH3)4]2IO2F2]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) Å, b = 8.60490(10) Å, c = 13.9572(2) Å, β = 120.2040(10)°, V = 1523.35(3) Å3, Z = 4 and R = 0.0192 at 210 K. The crystal structure consists of two IO2−F2 anions that are symmetrically bridged by two H−F2 anions, forming a F2O2I(FHF)2IO2F2]4− dimer. The symmetric bridging coordination for the H−F2 anion in this structure represents a new bonding modality for the bifluoride anion. |
| Keywords: | Iodine oxide fluorides Difluoroiodate Bifluoride X-ray crystallography Vibrational spectroscopy 19F NMR spectroscopy |
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