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

来源：

JOURNAL OF FLUORINE CHEMISTRY | 2004年 / 125卷 / 11期

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.

引用

页码：1663 / 1670

页数：8

共 50 条

[31] The reactions of M[BF4] (M= Li, K) and(C2H5)2O•BF3 with (CH3)3SiCN.: Formation of M[BFx(CN)4-x] (M= Li, K; x=1, 2) and (CH3)3SiNCBFx(CN)3-,,9-x, (x=0, 1) [J].

Bernhardt, E ;

Berkei, M ;

Willner, H ;

Schürmann, M .

ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2003, 629 (04) :677-685

[32] Synthesis, crystal structures, and vibrational spectra of trans-[Pt(N3)4X2]2-,X = Cl, Br, I [J].

Schröder, S ;

Preetz, W .

ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2000, 626 (08) :1757-1762

[33] THE X-RAY CRYSTAL-STRUCTURE AND PACKING MODE OF (+/-)-2-THIONO-2-MERCAPTO-A,A'-DINAPHTHO(D,F)(1,3,2)DIOXOPHOSPHEPIN - A CLATHRATE STRUCTURE [J].

GONG, BQ ;

CHEN, WY ;

HU, BF .

PHOSPHORUS SULFUR AND SILICON AND THE RELATED ELEMENTS, 1991, 57 (1-2) :87-94

[34] Synthesis, crystal structure, vibrational spectra, and normal coordinate analysis of cis- and trans-(n-Bu4N2)[PtF2(ox)2] and (n-Bu4N)2[PtF4(ox)] [J].

Uttecht, JG ;

Näther, C ;

Preetz, W .

ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2002, 628 (13) :2847-2854

[35] Second sphere coordination in anion binding: Synthesis, characterization and single crystal X-ray structure determination of tris(1,10-phenanthroline)cobalt(III) chloride dimesitylenesulphonate undecahydrate, [Co(phen)3]Cl[(CH3)3C6H2SO3]2•11H2O [J].

Sharma, Raj Pal ;

Singh, Ajnesh ;

Brandao, Paula ;

Felix, Vitor ;

Venugopalan, Paloth .

JOURNAL OF MOLECULAR STRUCTURE, 2009, 918 (1-3) :1-9

[36] Crystal structure, vibrational spectra, and normal coordinate analysis of (CH2py2)[Ru(NO)FCl4] [J].

Reese, I ;

Preetz, W .

ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2000, 626 (03) :645-648

[37] Crystal structure, vibrational spectra, and normal coordinate analysis of (n-Bu4N)2[{Ru(NO)ClI2}2(μ-I2)] • 2I2 [J].

Reese, I ;

Preetz, W .

ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2000, 626 (04) :911-914

[38] N-H•••S=C hydrogen bond in O-alkyl N-methoxycarbonyl thiocarbamates, ROC(S)N(H)C(O)O)CH3 (R = CH3-, CH3CH2-) [J].

Torrico Vallejos, Sonia ;

Erben, Mauricio F. ;

Piro, Oscar E. ;

Castellano, Eduardo E. ;

Della Vedova, Carlos O. .

POLYHEDRON, 2009, 28 (05) :937-946

[39] The synthesis, NMR (1H, 13C, 119Sn) and IR spectral studies of some di- and tri-organotin(IV) sulfonates:: X-ray crystal structure of [(n-C4H9)2Sn(OSO2C6H4CH3-4)2•2H2O] [J].

Kapoor, R ;

Gupta, A ;

Kapoor, P ;

Venugopalan, P .

APPLIED ORGANOMETALLIC CHEMISTRY, 2003, 17 (08) :607-615

[40] Synthesis, crystal structure, vibrational spectra, and normal coordinate analysis of cis-(n-Bu4N)2[PtX2(ox)2], X = Cl, Br, I [J].

Uttecht, JG ;

Näther, C ;

Preetz, W .

ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2002, 628 (12) :2585-2591

← 1 2 3 4 5 →