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Original Articles

Characterization of the Crystalline Nature of the Racemates of Novel Chiral Five-Membered Cyclic Nitroxides

, , , , , , & show all
Pages 23-35 | Published online: 31 Aug 2006

REFERENCES

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  • The X-ray data were collected at 298 K on an Enraf-Nonius Kappa CCD diffractometer. The crystal structures were solved by the direct methods and refined by full-matrix least squares. All non-hydrogen atoms were refined anisotropically. All of the crystallographic calculations were performed by using maXus software package. Crystal data for (±)-4: C13H18NO2, Mr = 220.29, 0.29 × 0.25 × 0.20 mm, monoclinic, space group P21/c, a = 8.1217(5), b = 20.2165(7), c = 8.0943(5) Å, β = 110.403(2)°, V = 1245.65(12) Å3, Z = 4, ρcalcd = 1.175 g cm−3, 2Θmax = 53.5°, MoKα (λ = 0.71073 Å), μ = 0.79 cm−1, Φ–ωscans, T = 298 K, 2655 independent reflections, 1605 observed reflections (I > 2.0σ(I)), 149 refined parameters, R = 0.051, R w = 0.126, Δρmax = 0.187eÅ−3, Δρmin = − 0.281 eÅ−3. Crystal data for trans-(±)-5: C18H20NO3, Mr = 298.36, 0.26 × 0.16 × 0.06 mm, orthorhombic, space group Pbcn, a = 19.178(2), b = 8.9422(8), c = 9.0107(4) Å, V = 1545.3(2) Å3, Z = 4, ρcalcd = 1.282 g cm−3, 2Θmax = 54.2°, MoKα (λ = 0.71073 Å), μ = 0.87 cm−1, Φ–ωscans, T = 298 K, 1717 independent reflections, 887 observed reflections (I > 2.0σ(I)), 103 refined parameters, R = 0.052, R w = 0.128, Δρmax = 0.241 eÅ−3, Δρmin = − 0.328 eÅ−3. Crystal data for trans-(±)-6: C18H20NO, Mr = 266.36, 0.30 × 0.24 × 0.20 mm, orthorhombic, space group Pbcn, a = 19.3353(6), b = 9.2424(6), c = 8.5632(5) Å, V = 1530.3(1) Å3, Z = 4, ρcalcd = 1.156 g cm−3, 2Θmax = 58.3°, MoKα (λ = 0.71073 Å), μ = 0.71 cm−1, Φ–ωscans, T = 298 K, 2063 independent reflections, 1284 observed reflections (I > 2.0σ(I)), 103 refined parameters, R = 0.055, R w = 0.156, Δρmax = 0.251 eÅ−3, Δρmin = − 0.452 eÅ−3. CCDC-217527-217529 contains the supplementary crystallographic data for this paper. These data can be obtained online free of charge (or from the Cambridge Crystallographic Data Centre, 12, Union Road, Cambridge CB2 1EZ, UK; fax: (+ 44) 1223-336-033; or [email protected]) .

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