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Tungsten nitride chloride-POCl 3  solvate, [WNCl 3  • POCl 3 ] 4  • 2 POCl 3  is prepared by the reaction of WNCI 3  with excess POCI 3 . With equimolar amounts of POCI 3  in dichloromethane suspension the complex [WNCI 3  • POCl 3 ] 4  • 2 CH 2 CI 2  is formed, which is easily decomposed leaving pure [WNCI 3  • POCl 3 ] 4 . The IR spectra of these complexes were recorded and assigned. A new preparative route to WNCI3 from tungsten hexachloride and iodine azide is described. [WNCI 3  • POCl 3 ] 4  • 2 POCl 3  crystallizes in the triclinic space group P1̅ with two tetrameric units per unit cell. The crystal structure was solved by X-ray diffraction methods (Å = 0,087; 3085 observed reflexions). The structure consists of planar and almost square W 4 N 4 -eight-membered rings with alternating W-N bond lengths. The distorted octahedral environment of the tungsten atoms is completed by three terminal Cl-ligands and by the oxygen atom of a POCI 3  molecule, which is coordinated trans to the W = N triple bond. The two additional POCI 3  molecules are weakly linked to two of the four POCI 3  solvate molecules, giving rise to an increase of the W-O bond lengths to these donor groups

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Darstellung, IR-Spektrum und Kristallstruktur von [WNCI 3  P0Cl 3 ] 4  2 POCI 3  / Preparation, IR Spectra and Crystal Structure of [WNCl 3  • P0Cl 3 ] 4  • 2 P0Cl 3