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Preparation of complexes 1 and 2: A methanolic solution (10 mL) containing copper(II) nitrate trihydrate (48 mg, 0.2 mmol) was mixed with an aqueous solution of sodium azide (130 mg, 2 mmol) dissolved in a minimum of water, R)-phea (11 mg, 0.1 mmol) in 3 mL of water was added to this reaction mixture with continuous stirring. The resulting dark-green solution was filtered and left to stand at 5°C. Brown plate-shaped crystals of 1 suitable for X-ray diffraction were obtained by slow evaporation of the solvents within 2 weeks. Complex 2 was obtained using a method similar to that of 1, except that (S)-phea was used. Yield: 54, Elem anal. Calcd for C16H22-Cu3N20: C, 28.05; H, 3.24; N, 40.89. Found: C, 27.86; H, 3.37; N, 40.63. IR: ν, 2031, 2057, 2089, and 2108 cm-1 (vs) for the azido groups. Crystal data for 1: C16H22Cu3N20
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3, Z = 4, R1 = 0.0651, wR2 = 0.1365 [I > 2σ(I)], Flack χ = 0.09(3). Data for 2: R1 = 0.0634, wR2 = 0.1288 [I > 2σ(I)], Flack χ = 0.07(3).
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