Crystal structure of eq-2-p-trifluoromethylphenoxy-2-borane-cis-4,6- dimethyl-1,3,2a3-dioxaphosphorinane, C12H17BF3O3P

Herbert Höpfl, Javier Hernández, Magali Salas-Reyes, Cruz-Sánchez Samuel, Zaira J. Dominiguez
2009 Zeitschrift für Kristallographie - New Crystal Structures  
C12H17BF3O3P, monoclinic, P12i/cl (no. 14) , a = 7.0311(6) Â, b = 23.087(2) Â, c = 9.5486(9) k,ß = 92.612(2)°, V = 1548.4 Â 3 , Ζ = 4, R gt (F) = 0.076, wR^F 2 ) = 0.163, Γ =293 Κ. Source of material The title compound was obtained via a two-step synthetic route. 2-chloro-4,6-dimethyl-l,3,2A 3 -dioxaphosphorinane [1] (1.00 g, 5.9 mmol) was reacted with 4-(trifluoromethyl)phenol (0.96 g, 5.9 mmol) and Et3N (0.82 mL, 5.9 mmol) in dry toluene to obtain eg-2-p-trifluoromethylphenoxy
more » ... -l,3,2A 3 -dioxaphosphorinane as intermediate. The resultant triethylammonium chloride was separated using a filter-tipped cannula. Immediately after filtration, a 1M solution of BH3-THF (7.0 mL) was added to give the desired title compound. The crude product was purified by column chromatography. Crystals suitable for X-ray diffraction were grown from a mixture of hexane and ethyl acetate. Experimental details The structure shows disorder in the trifluoromethyl moiety. The refinement of the disorder converged at the 0.42 : 0.58 ratio. DFIX, SIMU, DELU and ISOR instructions have been used to re-straint C-F bond lengths and the anisotropic displacement parameters [2], The B-Η hydrogen atoms were localized by difference Fourier maps, their coordinates have been refined freely, with i/ iso (H) = 1.5 t/iso(B).
doi:10.1524/ncrs.2009.224.14.259 fatcat:fwzorfy66zcfhdiqe5kianaapi