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2.1 Synthesis and structure characterization of complex 2
General procedure: [Ru(bpy)3]Cl2·6H2O (1.0110 g, 1.350 mmol) was purchased from Adamas Reagent. Ltd. and dissolved in ethylene glycol. An aqueous solution of excess Na[BF4] (2.0124 g, 18.330 mmol) was slowly added into the reaction mixture under stirring, resulting in a red suspension. The suspension was then filtrated and the resulting precipitate was washed with deionized water and dried under vacuum at 70 °C overnight. The crude product was purified by column chromatography on silica gel (200-300 mesh) with dichloromethane/methanol (v/v = 10:1) as the eluent, yielding a red powder (0.5311 g, 0.715 mmol). Yield: 53%.
61%
In lithium hydroxide monohydrate Cooling with ice; Inert atmosphere;
In lithium hydroxide monohydrate excess NaClO4; crystn.;
In lithium hydroxide monohydrate with excess of NaClO4; recrystd. three times from H2O-ethanol mixture (4:1) and dried under vac. at 60°C for 48 h;
In lithium hydroxide monohydrate with excess of NaClO4; the crystals were washed with H2O, recrystd. once from ethanol and twice from acetonitrile and dried under vac. at 90°C for 24 h;
With Ag2SO4 In lithium hydroxide monohydrate byproducts: AgCl; Ag2SO4 was added to aq. soln. of chloride complex, filtered, satd. NaClO4 soln. was added;; recrystd. from water;;
In lithium hydroxide monohydrate sample metathesis in excess Na-salt soln.; crystals washing (H2O) recrystn. (EtOH, MeCN), vac. drying at 90°C for 24 h;
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