Spektroskopische und kristallographische Charakterisierung von [Cl3PNPCl3][MoOCl4] und die Kristallstruktur von [Cl3PNPCl3][MoCl6]

Spectroscopic and Crystallographic Characterization of Cl₃PNPCl₃]MoOCl₄] and Crystal Structure of Cl₃PNPCl₃]MoCl₆] Cl₃PNPCl₃]MoCl₆] was obtained by reaction of MoCl₅ with Cl₃PNPCl₃]Cl or Cl₃PNPCl₃]PCl₆]. Its crystal was determined by X-ray diffraction (R = 0.072 for 889 observed reflexions). Lattice parameters: a = 811.9, b = 2086, c = 1016 pm, β = 101.7°, space group P2₁/c, Z = 4. The Cl₃PNPCl₃]⁺ ions have a similar structure as in Cl₃PNPCl₃ PCl₆] with PNP angles of 139°, but the crystal structures of the two compounds are not isotypic. Partial hydrolysis of Cl₃PNPCl₃]MoCl₆] yields Cl₃PNPCl₃]MoOCl₄] which forms green, very moisture sensitive crystals. X-ray diffraction patterns of Cl₃PNPCl₃]MoOCl₄] single crystals exhibit planes of diffuse scattered radiation perpendicular to c^*, which show the presence of a two-dimensional disorder. Additional sharp reflexions correspond to an averaged structure with the lattice parameters a = 1598.4, b = 1141.2 and c = 415.1 pm, Z = 2, space group Pba2. Refinement of the averaged