G. Laus, K. Wurst, U. E. Horvath
Apr 1, 2004
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Journal
Zeitschrift für Kristallographie - New Crystal Structures
Abstract
C20H21F3N2O5S, monoc l in ic ,P\2 \ \ (no.4) , a = 11.2847(8) A, b = 8.2066(3) A, c = 11.3780(8) A, /S = 101.542(2)°, V = 1032.4 A 3 , Z = 2, R ^ F ) = 0.035, wRnffF) = 0.089, T= 228 K. Source of material The title compound was prepared in analogy to a published procedure [1] f rom 5,6-didehydro-4,14-dihydroxy-3-methoxy-17methylmorphinan-6-carbonitrile and trifluoromethylsulfonic anhydride/pyridine in CH2CI2. Suitable crystals were obtained by slow evaporation of a solution in CDCI3. Discussion The morphinan derivative crystallized in a chiral space group (Flack parameter x = 0.05(9), indicating the correct absolute structure). The hydrogen atom of the hydroxy group at 0 3 was refined isotropically, exhibiting an intramolecular N1—H30 distance of 2.08 A. The double bond length C 5 — C 6 is 1.345(4) A, the single bond C 6 — C I 9 is rather long at 1.440(5) A, and the nitrile triple bond C I 9 — N 2 has a typical value of 1.139(4) A. Only weak intermolecular interactions are observed. Table 1. Data collection and handling.