SYNTHESIS AND CRYSTAL-STRUCTURE OF THE NITRIDO OXALATO OSMATE PPH4(NA(15-CROWN-5)[OSNCL3(C2O4)])

被引：2
作者：
BUTH, S [1 ]
HARMS, K [1 ]
DEHNICKE, K [1 ]
机构：
[1] PHILIPPS UNIV MARBURG,FACHBEREICH CHEM,HANS MEERWEIN STR,D-35043 MARBURG,GERMANY
来源：
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE | 1993年 / 619卷 / 08期
关键词：
NITRIDO OXALATO COMPLEX OF OSMIUM; SYNTHESIS; NMR SPECTRA; CRYSTAL STRUCTURE;
D O I：
10.1002/zaac.19936190815
中图分类号：
O61 [无机化学];
学科分类号：
070301 ; 081704 ;
摘要：
The title compound has been prepared by slow reaction of PPh4[OsNCl4] with sodium oxalate in boiling dichloromethane in the presence of 15-crown-5, forming violet crystals, which were characterized by an X-ray structure determination. Space group P2(1)/c, Z = 4, 4769 observed unique reflections, R = 0.035. Lattice dimensions at -80-degrees-C: a = 1931.4, b = 1178.7, c = 1764.1 pm, beta = 99.39-degrees. The structure consists of PPh4+ ions and ion pairs {Na(15-crown-5)[OsNCl3(C2O4)]}-, in which the osmium atom is distortedly octahedrally coordinated by the nitrido ligand, by three chlorine atoms, and by two oxygen atoms of the oxalato group. The remaining oxygen atoms of the oxalato ligand are coordinated to the sodium atom, which, together with the five oxygen atoms of the crown ether molecule, gets coordination number seven.
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页码：1409 / 1413
页数：5
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