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A Mettler Toledo TGA/SDTA 851E thermogravimetric analyzer (TGA) was used to obtain TGA curves. A 10 mg sample of 1-2 was placed in a 70 mL alumina pan and heated from 25 to 1000 °C at a rate of 5 °C/min in nitrogen atmosphere with a flow rate of 60-90 mL/min.
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A Mettler Toledo TGA/SDTA 851E thermogravimetric analyzer (TGA) was used to obtain TGA curves. A 10 mg sample of 1-2 was placed in a 70 mL alumina pan and heated from 25 to 1000 °C at a rate of 5 °C/min in nitrogen atmosphere with a flow rate of 60-90 mL/min.
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45
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84868977689
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A reaction mixture consisting of V2O5 (0.45 mmol, NiCl2 · 6H2O (0.25 mmol, 1,4-C6H 4(COOH)2 (0.55 mmol, H2O (555.6 mmol, and C5H5N (12.2 mmol) was placed in a 23 mL Teflon-lined Parr autoclave. After the mixture was stirred for 30 seconds, the reaction vessel was closed and heated in a furnace maintained at 145 °C for 6 days. The furnace was then turned off, and the reaction vessel, which was left inside the furnace, was cooled slowly to room temperature over a period of 24 h. Dark green needle-like crystals of 1, which were mixed with a brown powdery impurity, were filtered from the yellow mother liquor. The crystals were separated from the powder mechanically and dried in air at room temperature to give ∼50 mg of 1 yield ∼ 22.5% based on vanadium
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5N (12.2 mmol) was placed in a 23 mL Teflon-lined Parr autoclave. After the mixture was stirred for 30 seconds, the reaction vessel was closed and heated in a furnace maintained at 145 °C for 6 days. The furnace was then turned off, and the reaction vessel, which was left inside the furnace, was cooled slowly to room temperature over a period of 24 h. Dark green needle-like crystals of 1, which were mixed with a brown powdery impurity, were filtered from the yellow mother liquor. The crystals were separated from the powder mechanically and dried in air at room temperature to give ∼50 mg of 1 (yield ∼ 22.5% based on vanadium).
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