Bifunctional Zniiln
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- Preparation of complexes
- Physical measurements
EXPERIMENTAL SECTIONGeneral Procedures: Unless stated otherwise, all reactions were conducted in oven-dried glassware in aerobic conditions, with the reagents purchased commercially and used without further purification. The ligand H2L was prepared as previously described.12a Preparation of complexes[Zn(-L)(-OAc)Ln(NO3)2] (LnIII = Tb (1), Dy (2), Er (3), Yb(4)). A general procedure was used for the preparation of these complexes: To a solution of H2L (56 mg, 0.125 mmol) in 5 mL of MeOH were subsequently added with continuous stirring 27 mg (0.125 mmol) of Zn(OAc)2·2H2O and 0.125 mmol of Ln(NO3)3·nH2O. The resulting colourless solution was filtered and allowed to stand at room temperature. After two days, well formed prismatic colourless crystals of compounds 1 and 2, pink crystals for 3 and yellow crystals for 4, were obtained with yields in the range 40-55%, based on Zn. [Zn(-L)(-NO3)Er(NO3)2] (5) and [Zn(H2O)(-L)Nd(NO3)3]·2CH3OH (6). These compounds were prepared in a 60 % yield as pink and violet crystals, respectively, following the procedure for 1-4, except that Zn(NO3)2·6H2O (37 mg, 0.125 mmol) was used instead of Zn(OAc)2·2H2O. [Zn(-L)(-9-An)Ln(NO3)2]·2CH3CN (LnIII = Tb (7), Dy (8), Er (9), Yb(10); 9-An = 9-anthracenecarboxylate) To a solution of H2L (56 mg, 0.125 mmol) in 5 mL de CH3CN were subsequently added with continuous stirring 37 mg (0.125 mmol) of Zn(NO3)2·6H2O and (0.125 mmol) of Ln(NO3)3·nH2O. To this solution was added dropwise another solution containing 28 mg of 9-anthracene-carboxylic acid (0.125 mmol) and 0.125 mmol of triethylamine. The resulting solution was filtered and the filtrate allowed to stand at room temperature for two days, whereupon colourless crystals of compounds 7 and 8, and pink for 9, and yellow for 10 were obtained with yields in the range 40-50% based on Zn. [Zn(-L)(-9-An)Yb(9-An)(NO3)2]·3CH3CN (11) To a solution of H2L (56 mg, 0.125 mmol) in 5 mL of MeOH were subsequently added with continuous stirring 37 mg (0.125 mmol) of Zn(NO3)2·6H2O and 56 mg (0.125 mmol) of Yb(NO3)3·5H2O. To this solution was added dropwise another methanolic solution containing 28 mg of 9-anthracene-carboxylic acid (0.125 mmol) and 0.125 mmol of triethylamine and immediately a yellow precipitate was obtained. The precipitate was dissolved in acetonitrile and the resulting solution filtered to eliminate any insoluble material. The filtrate was kept at room temperature for a week affording yellow crystals of compound 11 in 32 % yield based on Zn. [Zn(-L)(-9-An)Nd(9-An)(NO3)2]·2CH3CN·3H2O (12). To a solution of H2L (56 mg, 0.125 mmol) in 5 mL de CH3CN were subsequently added with continuous stirring 37 mg (0.125 mmol) of Zn(NO3)2·6H2O and 55 mg (0.125 mmol) of Nd(NO3)3·6H2O. To this solution was added dropwise another solution containing 28 mg of 9-anthracene-carboxylic acid (0.125 mmol) and 0.125 mmol of triethylamine. The resulting solution was filtered and allowed to stand at room temperature for two days, whereupon violet crystals of 12 were obtained with a yield of 41 % based on Zn. [Zn(-L)(-9-An)Nd(CH3OH)2(NO3)](ClO4)·2CH3OH (13) To a solution of H2L (56 mg, 0.125 mmol) in 5 mL of MeOH were subsequently added with continuous stirring 46 mg (0.125 mmol) of Zn(ClO4)2·6H2O and 56 mg (0.125 mmol) of Nd(NO3)3·5H2O. To this solution was added dropwise another methanolic solution containing 28 mg of 9-anthracene-carboxylic acid (0.125 mmol) and 0.125 mmol of triethylamine. The resulting solution was filtered and allowed to stand at room temperature. After one week, well formed prismatic violet crystals of 13, were obtained with a yield of 38% based on Zn. The purity of the complexes was checked by elemental analysis (see Table S1).
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