Preparation and Characterisation of (PR3)2>Cl (R = alkyl or aryl); Crystal Structure of >*0.5EtOH*0.3CH2Cl2

Article abstract of DOI:10.1039/DT9950002489

Reaction of NH(PPh2)2 with selenium gives Ph2P(Se)NHP(Se)Ph2 which may be deprotonated with KOBu-t to give K.This can be treated with appropriate Group VIII metal complexes to give (cod)> (cod = cycloocta-1,5-diene), a series of complexes of formula (PR3)2>Cl (PR3 = PMe3, PMe2Ph, PEt3, 1/2NH(PPh2)2 or 1/2Ph2PCH2CH2PPh2) and (PMe2Ph)> (M = Pt or Pd).The new compounds have been characterised by 31P and 195Pt NMR and IR spectroscopy, FAB(1+) mass spectrometry and microanalyses.Furthermore, a small quantity of a mixed-ligand complex >*0.5EtOH*0.3CH2Cl2 has been characterised by X-ray crystallography and 31P NMR spectroscopy.Its structure reveals an approximately planar five-membered PdSeP2N ring and a puckered six-membered PdSe2P2N ring.In the crystal the molecules pack with channels which contain the disordered CH2Cl2 molecules running down the a direction.