A NOVEL 2/3 CONDENSATION COMPLEX OF SALICYLALDOXIME AND DI-N-BUTYLTIN(IV) OXIDE

被引:50
作者
KAYSER, F
BIESEMANS, M
BOUALAM, M
TIEKINK, ERT
ELKHLOUFI, A
MEUNIERPIRET, J
BOUHDID, A
JURKSCHAT, K
GIELEN, M
WILLEM, R
机构
[1] VRIJE UNIV BRUSSELS,CTR HIGH RESOLUT NMR,B-1050 BRUSSELS,BELGIUM
[2] VRIJE UNIV BRUSSELS,FAC ENGN,DEPT GEN & INORGAN CHEM,B-1050 BRUSSELS,BELGIUM
[3] UNIV LIBRE BRUXELLES,DEPT ORGAN CHEM,B-1050 BRUSSELS,BELGIUM
[4] UNIV ADELAIDE,DEPT CHEM,ADELAIDE,SA 5001,AUSTRALIA
[5] UNIV CATHOLIQUE LOUVAIN,PHYS CHEM & CRYSTALLOG LAB,B-1348 LOUVAIN,BELGIUM
[6] MARTIN LUTHER UNIV HALLE WITTENBERG,DEPT CHEM,O-4010 HALLE,GERMANY
关键词
D O I
10.1021/om00016a014
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The crystal structure of the reaction product of the 2:3 condensation of salicylaldoxime with di-n-butyltin(IV) oxide, [(Bu2Sn)(Bu2SnO)(Bu2SnOH)(HONZO)(ONZO)], where HONZOH represents HON=CHC6H4OH (salicylaldoxime), was determined by single-crystal X-ray diffraction; it belongs to the monoclinic system, space group P2(1)/c, with a = 20.995(3) angstrom, b = 17.394(4) angstrom, c = 12.254(2) angstrom, beta = 94.43(2)degrees, and Z = 4. The compound contains two five-coordinate trigonal-bipyramidal tin atoms with the two butyl groups in equatorial positions; the third tin atom has a seven-coordinate pentagonal-bipyramidal geometry with the two butyl groups in apical positions. The bonds of the salicylaldoxime ligands to the metal atoms are inequivalent. Both ligands are bound to the seven-coordinate tin atom through the oxygen atom originating from the phenolic function and through the nitrogen atom of the aldoxime function. In the ligand that binds as HONZO, the phenolate oxygen atom further coordinates a five-coordinate tin atom. In the ligand that coordinates as ONZO, the NO oxygen is bonded to the other five-coordinate atom. The H-1, C-13, and Sn-119 NMR data are in agreement with such a structure existing as a major species M in solution. However, the NMR spectra also reveal the presence of three other minor species in solution, m1, m2, and m3. These species could not be isolated as pure compounds, as crystallization from any solution of this compound led systematically to crystals of M. The H-1 and Sn-119 spectra, the (n)j(Sn-119-Sn-119/Sn-117) coupling satellite patterns observed in Sn-119 spectra, and the two-dimensional proton detected H-1-Sn-119 heteronuclear multiple bond correlation (2D H-1-Sn-119 HMBC) maps allow us to propose a structure for each species.
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页码:1098 / 1113
页数:16
相关论文
共 46 条
[1]   ISOTOPE EFFECTS IN THE NUCLEAR MAGNETIC-RESONANCE SPECTRA OF MIXED AQUA COMPLEXES OF AL-III [J].
AKITT, JW ;
HOWARTH, OW .
JOURNAL OF THE CHEMICAL SOCIETY-FARADAY TRANSACTIONS I, 1989, 85 :121-125
[2]   HOMONUCLEAR HARTMANN-HAHN EFFECTS IN BROAD-BAND DECOUPLING [J].
BARKER, PB ;
SHAKA, AJ ;
FREEMAN, R .
JOURNAL OF MAGNETIC RESONANCE, 1985, 65 (03) :535-539
[3]   H-1 AND C-13 ASSIGNMENTS FROM SENSITIVITY-ENHANCED DETECTION OF HETERONUCLEAR MULTIPLE-BOND CONNECTIVITY BY 2D MULTIPLE QUANTUM NMR [J].
BAX, A ;
SUMMERS, MF .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1986, 108 (08) :2093-2094
[4]   AN IMPROVED METHOD FOR HETERONUCLEAR CHEMICAL-SHIFT CORRELATION BY TWO-DIMENSIONAL NMR [J].
BAX, A ;
MORRIS, GA .
JOURNAL OF MAGNETIC RESONANCE, 1981, 42 (03) :501-505
[5]  
BOUALAM M, 1992, APPL ORGANOMET CHEM, V6, P197
[6]  
BOUALAM M, 1991, MAIN GROUP MET CHEM, V14, P41
[7]  
BOULAM M, 1991, APPL ORGANOMET CHEM, V5, P497
[8]   PENTA-COORDINATED MOLECULES .72. MONONUCLEAR AND TETRANUCLEAR DIORGANOTIN(IV) CARBOXYLATES FROM THE REACTION OF DIMETHYLTIN OXIDE WITH ANTHRANILIC ACID AND ITS PARA-AMINO ISOMER [J].
CHANDRASEKHAR, V ;
DAY, RO ;
HOLMES, JM ;
HOLMES, RR .
INORGANIC CHEMISTRY, 1988, 27 (05) :958-964
[9]   INTRAMOLECULAR HYDROGEN-BONDING IN 1'-SUCROSE DERIVATIVES DETERMINED BY SIMPLE H-1-NMR SPECTROSCOPY [J].
CHRISTOFIDES, JC ;
DAVIES, DB ;
MARTIN, JA ;
RATHBONE, EB .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1986, 108 (19) :5738-5743
[10]   SECONDARY ISOTOPE MULTIPLET NMR-SPECTROSCOPY OF PARTIALLY LABELED ENTITIES - C-13 SIMPLE NMR OF CARBOHYDRATES [J].
CHRISTOFIDES, JC ;
DAVIES, DB .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1983, 105 (15) :5099-5105