A NEW STRUCTURAL FORM FOR A PENTAOXYPHOSPHORANE. DIEQUATORIAL RING FORMATION IN A TRIGONAL BIPYRAMID

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• Davis , A. R. and Sullivan , A. V. U.S. Patent 2,538,355 . 1951 . To a mixture of P(OCH2CF3)3 (1.487 g, 4.53 mmol) and 2,2′-methylenebis(4-methyl-6-tert-butylphenol) (1.54 g, 4.53 mmol) in diethyl ether at – 75 °C was added (i-Pr)2NCl (0.737 g, 5.44 mmol) in ether. The reaction was brought to room temperature, and the mixture was stirred for 40 h. The removal of (i-Pr)2NH2Cl by filtration followed by slow evaporation of solvent gave 1.81 g of 1 (60% yield); mp 147–150 °C. Colorless crystals were obtained for an X-ray analysis by slow evaporation of a solution of 1 which consisted of a 1:2 mixture of ether and n-hexane. 31P NMR (CDCl3, ppm): – 78.8. 19F, NMR (CDCl3, ppm) – 75.6 (axial OCH2CF 3 groups), – 77.1 (equatorial OCH2CF 3 group). Anal. Calcd for C29H36F9O5P: C, 52.25; H, 5.40. Found: C, 52.17; H, 5.54. 2,2′-Methylenebis(4-methyl-6-tert-butylphenol) was prepared as described previously
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• X-ray study: C29H36F9O5P, orthorhombic space group Pnam (alternate sctting of Pnma, No. 62), a = 19.804 (2) Å, b = 10.237 (2) Å, c = 15.818 (3) Å, Z = 4, and μMoK = 1.670 cm−1. A total of 1923 independent reflections were measured (Enraf-Nonius CAD4 diffractometer, 23 ± 2 °C, graphite-monochromated Mo radiation, δ(K) = 0.71073 Å, 2θmax = 43°). The trifluoroethyl group bonded to O1 is disordered with respect to the mirror plane. Anisotropic refinement of non-hydrogen atoms with all but the two disordered H atoms included as fixed isotropic scatterers in ideal positions gave R = 0.053 and R w = 0.072 for 1223 observed reflections (l ≥ 3 [sgrave]t )
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