PREPARATION OF BISFLUOROPHOSPHINE AND 2,4-BIS(TRIFLUOROMETHYL)PHENYL>-FLUOROPHOSPHINE - TWO DISTILLABLE MONOFLUOROPHOSPHINES. STRUCTURE OF cis-DICHLORO-BISPLATINUM(II)

Article abstract of DOI:10.1016/S0022-1139(00)80993-8

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 of 1 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-, 119F- and 31P-NMR and mass spectra.The long-range coupling constants ⁴J(PF) and ⁵(J(FF) are discussed.The structure of 3 was cinfirmed 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) deg 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.