CRYSTAL-STRUCTURE OF [LI(TMEN)2][LI(C(SIME3)3)2] - A MULTINUCLEAR MAGNETIC-RESONANCE STUDY OF TRIS(TRIMETHYLSILYL)METHYLLITHIUM TETRAHYDROFURAN(1/2) AND -N,N,N',N'-TETRAMETHYLETHYLENEDIAMINE (1/1) (TMEN)

被引：44

作者：

AVENT, AG ^{[1
]}

EABORN, C ^{[1
]}

HITCHCOCK, PB ^{[1
]}

LAWLESS, GA ^{[1
]}

LICKISS, PD ^{[1
]}

MALLIEN, M ^{[1
]}

SMITH, JD ^{[1
]}

WEBB, AD ^{[1
]}

WRACKMEYER, B ^{[1
]}

机构：

[1] UNIV BAYREUTH,ANORGAN CHEM LAB,W-8580 BAYREUTH,GERMANY

来源：

JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS | 1993年 / 21期

关键词：

D O I：

10.1039/dt9930003259

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

A single-crystal X-ray study of (Me3Si)3CLi.tmen (tmen = N,N,N',N'-tetramethylethylenediamine) shows that it crystallises with the ionic structure [Li(tmen)2][Li{C(SiMe3)3}2] but that the anions pack with different orientations from those in crystalline [Li(thf)4][Li{C(SiMe3)3}2] (thf = tetrahydrofuran). The H-1, Li-7, C-13 and Si-29 NMR spectra of (MeSi)3CLi.2thf and (Me3Si)3CLi-tmen in thf and toluene, and Li-7, C-13 and Si-29 NMR spectra of the solids are described. Spectra obtained from solutions below ca. 25-degrees-C show the presence of ion pairs [Li(thf)4][Li{C(SiMe3)3}2] or [Li(tmen)2] [Li{C(SiMe3)3}2], together with further species which appear to be different in thf and toluene. Spectra from solutions at higher temperatures show inter-species exchange on the NMR timescale.

引用

页码：3259 / 3264

页数：6

共 26 条

[1] IMPROVEMENTS IN THE PREPARATION AND USE OF "[TRIS(TRIMETHYLSILYL)METHYL]LITHIUM [J].

AIUBE, ZH ;

EABORN, C .

JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1984, 269 (03) :217-218

[2]

ALHASHIMI S, UNPUB

[3] REACTIONS OF STERICALLY HINDERED ORGANOZINC AND ORGANOCADMIUM COMPOUNDS CONTAINING FUNCTIONAL SILICON CENTERS - CRYSTAL-STRUCTURES OF ZN[C(SIME3)2(SIME2OCOCF3)]2 AND CD[C(SIME3)2(SIME2OME)]2 [J].

ALJUAID, SS ;

EABORN, C ;

HABTEMARIAM, A ;

HITCHCOCK, PB ;

SMITH, JD .

JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1992, 437 (1-2) :41-55

[4] THE CRYSTAL-STRUCTURE OF BIS(TRIS(TRIMETHYLSILYL)METHYL)MAGNESIUM - AN EXAMPLE OF 2-COORDINATE MAGNESIUM IN THE SOLID-STATE [J].

ALJUAID, SS ;

EABORN, C ;

HITCHCOCK, PB ;

MCGEARY, CA ;

SMITH, JD .

JOURNAL OF THE CHEMICAL SOCIETY-CHEMICAL COMMUNICATIONS, 1989, (05) :273-274

[5]

[Anonymous], 1974, INT TABLES XRAY CRYS, VIV

[6] STRUCTURE AND DYNAMICS OF HINDERED ORGANOSILICON COMPOUNDS - THE CONFORMATIONS OF SYMMETRICAL (ME3SI)3C AND (PHME2SI)3C DERIVATIVES [J].

AVENT, AG ;

BOTT, SG ;

LADD, JA ;

LICKISS, PD ;

PIDCOCK, A .

JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1992, 427 (01) :9-21

[7]

BAUR W, 1987, ORGANOMETALLICS, V6, P2371

[8] [BIS(TRIMETHYLSILYL)METHYLENE](DIISOPROPYLAMINO)BORANE - AN ALLENE-TYPE N=B=C-SYSTEM [J].

BOESE, R ;

PAETZOLD, P ;

TAPPER, A .

CHEMISCHE BERICHTE-RECUEIL, 1987, 120 (06) :1069-1071

[9] SOME STERICALLY HINDERED LITHIUM ALKYLBROMO-MAGNESATE AND ALKYLCHLORO-MAGNESATE, CADMATES, AND MANGANATES - CRYSTAL AND MOLECULAR-STRUCTURES OF [LI(THF)2(MU-BR)2MG(C(SIME3)3)(THF)], [LI(THF)4][(CD[C(SIME3)3])3(MU-BR)3(MU-3-BR)].0.5C6H12' [(LI(THF))3(MU-3-BR)3(MU-3-OSIME3)CD(C(SIME3)3)], AND [LI(THF)4][(MN[C(SIME3)3])3-(MU-CL)4(THF)] (THF = TETRAHYDROFURAN)H [J].

BUTTRUS, NH ;

EABORN, C ;

ELKHELI, MNA ;

HITCHCOCK, PB ;

SMITH, JD ;

SULLIVAN, AC ;

TAVAKKOLI, K .

JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1988, (02) :381-391

[10] TRIS(TRIMETHYLSILYL)METHYL!LITHIUM - AN ALKYLLITHIUM COMPOUND OF UNUSUAL STABILITY [J].

COOK, MA ;

EABORN, C ;

JUKES, AE ;

WALTON, DRM .

JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1970, 24 (03) :529-&

← 1 2 3 →