SYNTHESIS AND CHARACTERIZATION OF ISOCYANIDE CONTAINING RHENIUM(III) COMPLEXES TRANS-[RECL3(CNR)(PPH(3))(2)] AND CRYSTAL-STRUCTURE OF TRANS-[RECL3(CN-T-C4H9)(PPH(3))(2)]

被引:18
作者
SPIES, H
GLASER, M
HAHN, FE
LUGGER, T
SCHELLER, D
机构
[1] FREE UNIV BERLIN,INST ANORGAN & ANALYT CHEM,D-14195 BERLIN,GERMANY
[2] TECH UNIV DRESDEN,INST ANALYT CHEM,D-01062 DRESDEN,GERMANY
关键词
CRYSTAL STRUCTURES; RHENIUM COMPLEXES; ISOCYANIDE COMPLEXES;
D O I
10.1016/0020-1693(94)04373-4
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Isocyanide containing complexes trans-[ReCl3(CNR)(PPh(3))(3)] (3) (R = tert-C4H9 (3a), c-C6H11 (3b), C6H5 (3c), CH2C(O)OCH3 (3d), CH2CH2-(N-morpholinyl) (3e)) were obtained by reduction of trans-[Re(O)Cl-3(PPh(3))(2)] with an excess of triphenylphosphane in the presence of the isocyanide or by substitution of the acetonitrile ligand in trans-[ReCl3(NCCH3)(PPh(3))(2)] by the isocyanide ligand. Generally, the substitution reaction starting with Re(III) gives a higher yield. The crystal structure of 3a has been determined by X-ray diffraction methods. 3a crystallizes with one molecule of CH2Cl2 per formula unit. Crystals of 3a.CH2Cl2 are monoclinic, space group P2(1)/c with a = 12.868(3), b = 20.454(7), c = 16.378(9) Angstrom, beta = 104.71(4)degrees, Z = 4 and D-o = 1.58 g cm(-3). The structure was solved from 6190 diffraction data (F-0(2) greater than or equal to 3 sigma(F-0(2))] collected at -100(2) degrees C and refined to R = 0.0429 (R(w) = 0.0727).
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页码:235 / 239
页数:5
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