PREPARATION OF BIS[2,4-BIS(TRIFLUOROMETHYL)PHENYL]FLUOROPHOSPHINE AND 2,4-BIS(TRIFLUOROMETHYL) PHENYL-[2,6-BIS(TRIFLUOROMETHYL)PHENYL]-FLUOROPHOSPHINE - 2 DISTILLABLE MONOFLUOROPHOSPHINES - STRUCTURE OF CIS-DICHLORO-BIS[BIS(2,4-BIS(TRIFLUOROMETHYL)PHENYL)FLUOROPHOSPHINO]-PLATINUM(II)

Bis[2,4-bis(trifluoromethyl)phenyl]fluorophosphine, 1, and 2,4-bis(trifluoromethyl)phenyl-[2,6-bis(trifluoromethyl)phenyl]fluorophosphine, 2, were found amongst the products of the reaction of 1,3-bis(trifluoromethyl)benzene with n-butyllithium, followed by chlorodifluorophosphine. The mixture of1 and 2 was a stable, distillable oily liquid, which crystallized on standing. The reaction of the mixture of 1 and 2 with dichloro-(η4-1.5-cyclooctadiene)platinum(II) led to the formation of cis-dichloro-bis(bis(2,4-bis(trifluoromethyl)phenyl)fluorophosphino)platinum(II), 3. The products 1, 2 and 3 were characterized by their 1H-.19F- and 31P-NMR and mass spectra. The long-range coupling constants 4J(PF) and 5J(FF) are discussed. The structure of 3 was confirmed by a single crystal X-ray investigation. 3 crystallizes in the monoclinic space group C2/c with cell constants a = 1331.8(3). b = 2392.5(4), c = 1263.1(2) pm, β = 93.75(2)° and Z = 4 (the complex possesses crystallographic twofold symmetry). The bond lengths Pt-P 221.7, Pt-Cl 232.6, P-F 155.9 pm all lie in the expected range for platinum fluorophosphine complexes. © 1999.