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39749131584
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Salt 2: To a solution of 1 (0.08 g 0.32 mmol) in CH2Cl2 (20 mL) was added HOTf (28 μL, 0.32 mmol) in CH2Cl2 (20 mL, After stirring for 20 min at room temperature, the solvent was evaporated under reduced pressure to afford a dark residue in quantitative yield. Dark-red crystals were grown by slow diffusion of diethyl ether vapor into a CHCl3 solution of the compound. 1H NMR (300 MHz, acetone-d6, δ 7.00 (br s, 2H, 7.89 (d, J, 8.4 Hz, 2H, 8.06 (d, J, 8.5 Hz, 2H, 8.30 (br s, 2H, 13C NMR (75 MHz, CDCl3, δ 110.7, 116.0, 117.7, 119.7, 126.7, 129.3, 132.3, 132.6, 133.9, 143.9, 149.9. 19F NMR (280 MHz, acetone-d6, δ -79.3. IR (KBr/cm -1, νCN 2242, b) Complex 4: A 1.75 mM solution of 1 in benzene (0.5 mL) was combined with a 1.75 mM solution of AgBF4 in
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2: C, 42.00; H, 3.01; N, 8.64. Found: C, 39.92; H, 2.96; N, 8.33.
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24
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39749172323
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Crystal data for 2 (C17H12F 3N3O3S, MW, 395.36, monoclinic, P21/c, a, 10.0624(6) Å, b, 10.3247(6) Å, c, 16.6996(9) Å, β, 91.463(2)°, V, 1734.2(2) Å3, Z, 4, Dcalc, 1.514, T, 173(2) K, μ, 0.241 mm-1, 15 368 reflns measd, 3972 unique refins (Rint, 0.0344, R, 0.0431 [I > 2σ(I, Rw, 0.1279 (for all data, b) Crystal data for 4 (C32H 22Ag2B2F8N6, MW, 879.92, triclinic, P1, a, 9.9210(6) Å, b, 10.0826(4) Å, c, 10.1108(4) Å, α, 118.576(2)°, β, 100.160(3)°, γ, 108.078(3)°, V, 777.79(6) Å3
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2 using SHELXL-97. The H atoms were introduced at calculated positions and not refined (riding model).
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