Synthesis and structure of [Bi-2(N(t)Bu)(4)]Li-2(2)center dot 2THF; A bimetallic cubane fragment containing a [Bi-2(N(t)Bu)(4)](2-) anion

被引:21
作者
Edwards, AJ [1 ]
Beswick, MA [1 ]
Galsworthy, JR [1 ]
Paver, MA [1 ]
Raithby, PR [1 ]
Rennie, MA [1 ]
Russell, CA [1 ]
Verhorevoort, KL [1 ]
Wright, DS [1 ]
机构
[1] UNIV CAMBRIDGE,CHEM LAB,CAMBRIDGE CB2 1EW,ENGLAND
关键词
crystal structures; bismuth complexes; imido complexes; cubane complexes;
D O I
10.1016/0020-1693(95)04974-6
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The imido-Bi complex [Bi-2(N(t)Bu)(4)]Li-2 . 2THF (1) has been prepared by the in situ reaction of [(Me(2)N)Bi(mu-N(t)Bu)](2) with [(t)BuNHLi] in toluene/THF solution. The complex has been characterised by elemental analysis, solid-state IR spectroscopy, H-1 NMR spectroscopy in solution, and by a low-temperature (153 K) X-ray diffraction study. The complex crystallises in the monoclinic space group P2(1)/n, with cell dimensions a = 11.158(2), b = 16.777(3), c = 17.239(3) Angstrom, beta = 92.45(3)degrees, V = 3224.2(10) Angstrom(3) and Z = 4. Molecules of 1 consist of discrete [Bi2Li2N4] cubane units in the solid state. Further association of these units into a structure akin to the previously characterised complex [Sb-2(NCy)(4)]Li-2(4) (2), consisting of a cage of two interlocked 'broken cubes', is prevented by Lewis base solvation of Li. Solution NMR and cryoscopic studies of 2 show that the complex is involved in a dissociative equilibrium in which separate cubane units, similar to those identified in 1, are formed.
引用
收藏
页码:9 / 14
页数:6
相关论文
共 39 条
[1]   SYNTHESIS AND STRUCTURE OF [SB2LI2(N(C6H11))4]2 - A CAGE COMPLEX CONTAINING A CORE OF 2 INTERLOCKED BROKEN CUBES [J].
ALTON, RA ;
BARR, D ;
EDWARDS, AJ ;
PAVER, MA ;
RAITHBY, PR ;
RENNIE, MA ;
RUSSELL, CA ;
WRIGHT, DS .
JOURNAL OF THE CHEMICAL SOCIETY-CHEMICAL COMMUNICATIONS, 1994, (12) :1481-1482
[2]   COMPLEXES OF ORGANOALUMINUM COMPOUNDS .10. CRYSTAL AND MOLECULAR-STRUCTURES OF THE CAGE COMPOUNDS BIS-MU-METHYLAMIDO-HEXA-MU-3-METHYLIMIDO-BIS(DIMETHYLALUMINIUM)-HEXAKIS(METHYLALUMINIUM) AND BIS-MU-METHYLAMIDO-HEXA-MU-3-METHYLIMIDO-BIS(DIMETHYLGALLIUM)-HEXAKIS-(METHYLGALLIUM) [J].
AMIRKHALILI, S ;
HITCHCOCK, PB ;
SMITH, JD .
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1979, (07) :1206-1212
[3]   PREPARATIONS AND REACTIONS OF TRIS(DIALKYLAMINO)BISMUTHINE [J].
ANDO, F ;
HAYASHI, T ;
OHASHI, K ;
KOKETSU, J .
JOURNAL OF INORGANIC & NUCLEAR CHEMISTRY, 1975, 37 (09) :2011-2013
[4]  
BARR D, 1994, ANGEW CHEM INT EDIT, V33, P1875, DOI 10.1002/anie.199418751
[5]   CAGE EXPANSION OF [((CYNLI)(3)SB)(2)] - SYNTHESIS AND STRUCTURE OF THE TRIMETALLIC COMPLEX [((CYNLI)(3)SB)(2)(TBUOK)(3)-CENTER-DOT-X-C6H5CH3] [J].
BARR, D ;
EDWARDS, AJ ;
PAVER, MA ;
RAITHBY, PR ;
RENNIE, MA ;
RUSSELL, CA ;
WRIGHT, DS .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION IN ENGLISH, 1995, 34 (09) :1012-1013
[6]  
BARR D, 1995, ANGEW CHEM, V107, P1088
[7]  
Barr D., 1994, ANGEW CHEM, V106, P1960
[8]   SYNTHESIS AND STRUCTURE OF SESB2CL2(NCME3)4 - A COMPOUND WITH A SELENIUM ATOM COORDINATED BY 3 NITROGEN-ATOMS [J].
BJORGVINSSON, M ;
ROESKY, HW ;
PAUER, F ;
SHELDRICK, GM .
CHEMISCHE BERICHTE-RECUEIL, 1992, 125 (04) :767-769
[9]   TRIS(TRIMETHYLSILYLAMINO)SILANES RSI(NHSIME3)3 - SYNTHESIS, CRYSTAL AND MOLECULAR-STRUCTURE OF 3 DIMERIC TRILITHIO DERIVATIVES [J].
BRAUER, DJ ;
BURGER, H ;
LIEWALD, GR ;
WILKE, J .
JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1985, 287 (03) :305-320
[10]   SYNTHESES AND CRYSTAL-STRUCTURES OF THE DIMERS OF A BIS(LITHIOAMINO)-SILANE AND A TRIS(LITHIOAMINO)-SILANE CONTAINING ELECTRON-DEFICIENT LI4N4 AND LI6N6 CLUSTERS [J].
BRAUER, DJ ;
BURGER, H ;
LIEWALD, GR .
JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1986, 308 (02) :119-130