Preparation of bis[2,4-bis(trifluoromethyl)phenyl]fluorophosphine and 2,4-bis[trifluoromethyl) phenyl-[2,6-bis(trifluoromethyl)phenyl]-fluorophosphine - two distillable monofluorophosphines. Structure of cis-dichloro-bis[2,4-bis(trifluoromethyl)phenyl)fluorophosphino]platinum(II)
1990; Elsevier BV; Volume: 46; Issue: 2 Linguagem: Inglês
10.1016/s0022-1139(00)80993-8
ISSN1873-3328
AutoresLutz Heuer, Peter G. Jones, Reinhard Schmutzler,
Tópico(s)Coordination Chemistry and Organometallics
ResumoBis[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.
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