25463-79-0Relevant articles and documents
[NBu4][ReNCl4]: Facile synthesis, structure, electron paramagnetic resonance spectroscopy and reactions
Abram, Ulrich,Braun, Martin,Abram, Sonja,Kirmse, Reinhard,Voigt, Andreas
, p. 231 - 238 (1998)
The compound [NBu4][ReNCl4] has been found to be easily accessible by the reaction of [NBu4][ReO4] with sodium azide and HCl gas in ethanol and represents an excellent precursor for the synthesis of further rhenium nitrido complexes. It has been studied by X-ray crystallography. Rhenium(VI) compounds of the general formula [ReNX4(5)]-,2- (X = Br or NCS) were obtained when [NBu4][ReNCl4] reacts with HBr or KSCN. The products as well as mixed-ligand intermediates which are formed during the ligand exchange have been studied by EPR spectroscopy. The EPR parameters of the individual mixed-ligand compounds are clearly correlated to the composition of the co-ordination sphere and can be used to characterize the mixed-ligand species unambiguously. This is shown by a nearly linear dependence of g0, g∥, a0Re and A∥Re on the spin-orbit coupling constants of the equatorial donors. Reactions of [NBu4][ReNCl4] with most organic ligands yielded rhenium(V) compounds. A number of phosphine complexes and chelates with sulfur-containing ligands have been prepared and spectroscopically characterized. A crystallographic study on [ReN(Hdetcb)2] (Hdetcb- = N2-diethylthiocarbamoylbenzamidinate) shows cis co-ordination for the chelating S,N-donor ligands. Weak intermolecular hydrogen bridges have been found between the co-ordinated nitrogen atoms and the lone pair of the nitrido nitrogen. A comparison between the crystal structural data of [NBu4]2[ReN(mnt)2] (mnt2- = 1,2-dicyanoethene-1,2-dithiolate), prepared from [NBu4][ReNCl4] and Na2mnt, and [NBu4][ReO(mnt)2] shows longer Re-S bonds in the nitrido anion but markedly higher O-Re-S bond angles indicating higher steric requirements of the oxo ligand compared with 'N3-'.
Dichlorotrisnitridorhenium(V),ReNCl2(Me2PhP)3
Forsellini, E.,Casellato, U.,Graziani, R.,Magon, L.
, p. 3081 - 3083 (2007/10/02)
, C24H33Cl2NP3Re, Mr = 686, orthorhombic, space group Pcab, a = 16.673 (5), b = 16.754 (5), c = 19.200 (6) Angstroem, V = 5364 (3) Angstroem3, Dx = 1.70 Mg m-3 for Z = 8, μ = 4.7 mm-1 (MoKα).The structure was solved by standard methods from X-ray diffractometer intensities and refined by full-matrix least squares to a final R of 0.034 for 2816 observed reflexions.The Re atom is in a distorted octahedral-coordination geometry and the Re-N bond length is 1.660 (8) Angstroem.
