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Prepared from the corresponding (1S,3aR,4S,6aR)-octahydropentalene-1,4- diol using the method reported in ref 8.
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Prepared from the corresponding (1S,3aR,4S,6aR)-octahydropentalene-1,4- diol using the method reported in ref 8.
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40
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61349198499
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2O.
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2O.
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41
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61349145915
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Crystallographic data for (R,R)-5 (C12H 14O2, T, 293 (2) K; wavelength: 0.71073 Å; crystal system: orthorhombic, space group: mdit > P212 121; unit cell dimensions: a, 6.1336(7) Å, b, 11.7280(14) Å, c, 14.5571(17) Å, α, 90°, β, 90°, γ, 90°; V, 1047.2 (2) Å3; Z, 4; ρcalc, 1.410 Mg/m3; F(000, 472; final R indices [I > 2σ(I, R 1, 0.0392, wR2, 0.0616; R indices (all data, R1, 0.0564, wR2, 0.0655; 6189 reflections mesured, 1337 were unique (Rint, 0.0711
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int) = 0.0711).
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42
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61349194723
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The rhodium complex was obtained by treatment of (R,R)-5 with [RhCl(C2H4)2]2 in THF at room temperature for 48 h. 1H NMR (300 MHz, CDCl3, δ 1.76 (s, 2H, 3.74-3.79 (m, 2H, 3.89 (dd, J, 6.5, 14.0 Hz, 2H, 4.01-4.17 (m, 4H, 4.19-4.30 (m, 4H, 13C NMR (75 MHz, CDCl3, δ 48.1, 65.4, 65.6, 68.0, 68.1, 82.3, 82.4, 119.6. Crystallographic data for [RhCl(R,R)-5]2 (C24H 28Cl2O8Rh2, T, 293(2) K; wavelength: 0.71073 Å; crystal system: orthorhombic, space group: P212121; unit cell dimensions: a, 9.7534(10) Å, b, 9.9312(10) Å, c, 28.882(3) Å, α, 90°, β, 90°, γ, 90°; V, 2797.6(5) Å3; Z, 4; ρcalc, 1.848 Mg/m 3; F000, 1572; f
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int) = 0.0938).
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