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note
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Compound 1 was prepared by laying method, the mixed solution containing 2-[(pyridin-2-ylmethylene)-amino] ethanol (0.1 mmol, 0.0136 g), Cu(ClO4)2 • 6H2O (0.2 mmol, 0.074 g) and pyridine-2-carbaldehyde (0.1 mmol, 0.0107 g) in methanol was carefully layered on the aqueous solution of sodium azide(0.4 mmol, 0.026 g). The single crystals suitable for X-ray diffraction were grown after two weeks. Anal. Calc. for C14H14Cu3.50N27O: H 1.77 C 21.09 N 47.47. Found: H, 1.72; C, 21.65; N, 47.95%. IR (solid KBr pellet, cm-1): 2114.6 (s) and 2050.0 (s), 1280.5(m) 1173.4(w), 1079.9(w), 786.8(m), 676.8(w). Safety note: Azide derivatives are potentially explosive, only a small amount of materials should be prepared, and they should be handled with proper care.
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Crystal data for 1: C14H14Cu3.50N27O, Mr = 798.91; triclinic; space group: P-1; a = 7.5032(15), b = 13.897(3), c = 14.899(3)Å; α = 106.96(3), β = 101.06(3), γ = 105.29(3); V = 1371.2(5) Å3; Z = 2; Dc = 1.935 g/cm3; T = 293(2) K. A total of 4694 reflections were processed to give 3751 unique reflections (Rint = 0.0651). Refinement converged to R = 0.0682, wR(F2) = 0.1552, and S = 1.085 for 3751 reflections with I > 2σ (I), and R = 0.0828, wR(F2) = 0.1607, and S = 1.085 for 4694 unique reflections and 412 parameters.
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