
%0 Journal Article
%A Clark, GR 
%A Greene, TR 
%A Roper, WR 
%T Trifluoromethyl Complexes of Osmium(II) by Halogen Oxidation of an Osmium(0) Difluorocarbene Compound and the Structures of Os(CF<sub>3</sub>)Cl<sub>2</sub>(NO)(PPh<sub>3</sub>)<sub>2</sub>
 and Os(CF<sub>3</sub>)Cl<sub>0.666</sub>I<sub>1.333</sub>(NO)(PPh<sub>3</sub>)<sub>2</sub>
%J Australian Journal of Chemistry
%D 1986/09/01
%V 39
%N 9
%P 1315-1320
%K 
%R https://doi.org/10.1071/CH9861315
%U https://www.publish.csiro.au/paper/CH9861315 
%X Oxidation of Os(=CF2) Cl (NO)(PPh3)2 by the halogens X2(X = Cl , I), unexpectedly yields the trifluoromethyl complexes Os(CF3)CIX(NO)(PPh3)2 in a low yield which is improved by the addition of LiF to the reaction mixture. The crystal structures of both Os(CF3)Cl2(NO)(PPh3)2 and Os(CF3)Cl0.666I1.333(NO)(PPh3)2 have been determined. Crystals of Os(CF3)Cl2(NO)(PPh3)2 are monoclinic, a 24.543(5), b 9.685(1), c 15.951(1) &#506;, &#946; 115.81(1)&#176;, Z 4, space group C2/c. Least-squares refinement has returned a residual, R, of 0.048 for 3371 observed reflections. The molecule lies on a twofold axis, with the CF3-group and one Cl-ligand statistically interchanged. Crystals of Os(CF3)Cl0.666 I1.333(NO)(PPh3)2 are monoclinic, a 24.562(4), b 9.690(1), c 16.385(2) &#506;, &#946; 115.51(1)&#176;, Z 4, space group C2/c. Least-squares refinement has returned a residual of 0.058 for 4087 observed reflections. This crystal structure is best described as a 2 : 1 mixture of Os(CF3) ClI (NO)(PPh3)2 and s(CF3)I2(NO)(PPh3)2, (both with CF3 and I statistically disordered about the diad axis, as above). Both complexes exhibit octahedral coordination geometries. 
