Preparation and crystal structure of [PHBu3][MoHCl4(PBu3)2]
Abstract
The preparation of the series of anionic, paramagnetic, hydrido complexes [PHR3][MoHCl4(PR3)2](R = Et, X = Cl or Br; R = Bu, X = Cl; R3= Me2Ph, X = Br) from the reactions of anhydrous HX with [MoH4(PR3)4] in tetrahydrofuran is described. The structure of one example, [PHBu3][MoHCl4(PBu3)2], has been determined by X-ray crystallography. The co-ordination geometry of the anion is best described as a distorted pentagonal bipyramid, with apical chloro-groups [(Mo–Clax)av 2.423(10)Å]. The hydride was located in the structure [Mo–H 1.83(4)Å] and is displaced 0.31 Å out of the equatorial plane towards one of the axial sites. The remaining ligands in the equatorial positions have bond lengths (Mo–Cleq)av 2.485(1) and (Mo–P)av 2.511 (5)Å.