136033-83-5Relevant academic research and scientific papers
Halogeno(phenyl)-, Diphenyl-, Amino(phenyl)carben- und Phenylimido-Osmiumkomplexe durch Reaktion von mit Phenyllithium und Phenyl-Grignardreagenzien
Werner, Helmut,Wecker, Ulrich,Peters, Karl,Schnering, Hans Georg von
, p. 205 - 212 (2007/10/02)
On treatment of (2: R=t-Bu; 4: R=Cy; 5: R=Xyl)* with C6H5MgBr, the diphenyl- and the bromo(phenyl)osmium(II) compounds (7-9) and (10-12) are formed.As a minor product in the reaction of 4 with C6H5MgBr, the aminocarbene complex > (6) is obtained.From (3) and C6H5MgBr, besides (14) the five-membered ring compound (13) has been prepared; it reacts with CHCl3 to yield the chloro derivative (15).While the reactions of 2 and 3 with C6H5MgI lead to the compounds (16, 17) and (18, 19), from 3 and C6H5Li the metallaheterocycle 13 and the carbene complex (20) are formed.The reaction of 4 and C6H5Li yields (8).The structure of 20 has been determined by an X-ray structural analysis.Key words: Osmium; Mesitylene; Isocyanide; Aminocarbene; Metallaheterocycle; X-ray diffraction
Preparation of [(mes)Os(CNR)Cl2] and reactions of the methyl isocyanide complex with organolithium and Grignard reagents. X-ray crystal structure of [(mes)Os(=C(NHCH3)C6H5)(C6H 5)2]
Werner, Helmut,Wecker, Ulrich,Schulz, Michael,Stahl, Stefan
, p. 3278 - 3282 (2008/10/08)
The isocyanide complexes [(mes)Os(CNR)Cl2] (2-4) are prepared almost quantitatively from [(mes)OsCl2]n (1) and CNR in dichloromethane. Reactions of 2 (R = CH3) with CH3Li and C6H5Li in hydrocarbon-ether give the dimethyl and diphenyl derivates [(mes)OsR2(CNCH3)] (5, 6) in excellent yields. Treatment of 2 with CH3MgI leads to the formation of a mixture of [(mes)OsCH3(CNCH3)I] (7) and [(mes)Os(CNCH3)I2] (9), which can be separated by column chromatography. Analogously, from 2 and C6H5MgI, both [(mes)OsC6H5(CNCH3)I] (8) and 9 have been obtained. In contrast, reaction of 2 with C6H5MgBr gives, besides [(mes)OsC6H5(CNCH3)Br] (11), the carbene complex [(mes)Os(=C(NHCH3)C6H5)(C6H 5)2] (10) as the main product. The X-ray crystal structure of 10 has been determined (monoclinic space group P21/n with a = 12.402 (3) ?, b = 14.237 (2) ?, c = 13.622 (2) ?, β = 91.54 (1)°). The molecule possesses a piano-stool configuration with an Os-C(carbene) distance of 1.992 (5) ?.
