138900-10-4Relevant articles and documents
Reactions of the polyhydride complex ReH7(PPH3)2 with quinoline, 2-hydroxyquinoline, and 2-mercaptoquinoline. Preparation and characterization of hydrido complexes of rhenium(V) and chloro complexes of rhenium(III)
Leeaphon, Malee,Rohl, Kymberly,Thomas, Robert J.,Fanwick, Phillip E.,Walton, Richard A.
, p. 5562 - 5568 (2008/10/08)
The thermal reactions of the heptahydride complex ReH7(PPh3)2 with quinoline (qn), 2-hydroxyquinoline (Hhq), and 2-mercaptoquinoline (Hmq) afford the hydridorhenium(V) complexes ReH5(PPh3)2(qn), ReH4(Hq)(PPh3)2, and ReH4(mq)(PPh3)2, respectively, when refluxing tetrahydrofuran or ethanol is used as the reaction solvent, whereas the paramagnetic chlororhenium(III) species ReCl3(qn)2(PPh3), ReCl2(Hq)(PPh3)2, and ReCl2(mq)(PPh3)2 are formed in refluxing 1,2-dichloroethane solutions. The diamagnetic polyhydride complexes are fluxional at room temperature (by 1H and 31P{1H} NMR spectroscopy) and show cyclic voltammetric properties that are similar to those of other hydridorhenium(V) species. The structure of ReH4(hq)(PPh3)2 (1) has been determined by X-ray crystallography and shown to be that of a distorted dodecahedron. The chlororhenium(III) species display very characteristic, well-defined, Knight-shifted 1H NMR spectra. The crystal structure determination of ReCl2(mq)-(PPh3)2 (2) shows that the PPh3 ligands are in a trans disposition relative to one another and confirms the presence of a chelating mq ligand. Crystal data for 1 (+20°C): monoclinic space group F21/c (No. 14), a = 9.6655(8) A?, b = 16.095(1) A?, c = 24.562(2) A?, β = 100.279(6)°, V = 3759.7(9) A?3, Z = 4. The structure was refined to R = 0.024 (Rw = 0.029) for 3646 data with I > 3.0σ(I). Crystal data for 2 (+20°C): monoclinic space group P21, (No. 4), a = 11.908(3) A?, b = 16.779(8) A?, c = 12.061(3) A?, β = 99.73(2)°, V= 2374(2) A?3, Z = 2. The structure was refined to R = 0.054 (Rw = 0.070) for 2774 data with I > 3.0σ(I).
