Substitution reactions of tetrahydrofuran in [Cr(thf)3Cl3] with mono and bidentate N-donor ligands: X-ray crystal structures of [Cr(bipy)(OH2)Cl3] and [HpyNH2][Cr(bipy)Cl4]
摘要:
Substitution of thf ligands in [Cr(thf)(3)Cl-3] and [Cr(thf)(2)(OH2)Cl-3] was investigated. 2,2'-Bipyridine (bipy) was reacted with [Cr(thf)(3)Cl-3] to form [Cr( bipy)(thf)Cl-3] (1), which was subsequently reacted with water to give [Cr(bipy)(OH2)Cl-3] (2). Reaction of 1 with acetonitrile (CH3CN), pyridine (py) and pyridine derivatives to form [Cr(bipy)(L)Cl-3] (L= CH3CN3, py 4 and 4-pyR with R = NH(2)5, Bu-t 6 and Ph7). In addition, the substitution of bipy in [Cr(thf)Cl-3(3)] was followed by H-1 NMR spectroscopy at room temperature, which showed completion of the reaction in ca. 100 min. Complex 2 was characterised by single crystal X-ray diffraction. The theoretical powder diffraction pattern of 2 was compared to the experimentally obtained powder X-ray diffraction pattern, and shows excellent agreement. The dimer [Cr-2(bipy)(2)Cl-4(mu-Cl)(2)] was cleaved asymmetrically to give the anionic complex [Cr(bipy)Cl-4](-) (8) and [Cr(bipy)(2)Cl-2](+) (9). Complexes 8 and 9 were characterised by single crystal X-ray diffraction. (c) 2008 Elsevier B.V. All rights reserved.