Experimental Procedure
All reagents were obtained from commercial sources and were purified further through methods found in literature.[7] All reactions and recrystallizations were performed under aerobic conditions. 1H NMR spectra was taken with a Bruker 400 UltrashieldTM. The IR was taken with a Thermo Scientific Nicolet iS5 spectrophotometer. The UV-Vis was taken with an HP 8453 Diodearray. All measurements were taken during standard conditions.
 |  2-(methylthio)-N-(3-pyridinylmethyl)acetamide (3-HLSMe). A solution of (methylthio)acetic acid (0.9752g; 9.188mmol), EDC·HCl (1.7613g; 9.188mmol), triethylamine(1.8594g; 18.376mmol), and HOBt (1.2416g; 9.188mmol) in 25mL of dichloromethane (CH2Cl2)was cooled to 0 °C and stirred rapidly. 3-aminomethyl pyridine (0.99385g; 9.188mmol) was then added to this solution. The reaction mixturewas stirred for one hour at 0 °C and left to stir overnight andwarm to room temperature. The ligand solution was washed using dichloromethane and a solution of sodium carbonate to eliminate the majority of the urea by-product. Afterwards, the clean ligand solution was placed in a Rota-vapor instrument to remove the dichloromethane. The resulting crude 3-HLSMe was of a waxy consistency and a dark-yellow color. This ligand was then run through a column chromatography to remove the coupling reagents and a TLC indicated that the ligand was in the third (0.19 RF), fourth (0.2 RF), and the fifth (0.2 RF) fractions. These fractions were run through a Rota-vapor and the final purified ligand was of an oily consistency and golden-yellow color. The 3-HLSMe was then run through a 1H NMR and was confirmed to be pure. |
 |  2-(methylthio)-N-(4-pyridinylmethyl)acetamide (4-HLSMe). A solution of (methylthio)acetic acid (0.9752g; 9.188mmol), EDC·HCl (1.7613g; 9.188mmol), triethylamine (1.8594g; 18.376mmol), and HOBt (1.2416g; 9.188mmol) in 25mL of dichloromethane (CH2Cl2) was cooled to 0 °C and stirred rapidly. 4-aminomethyl pyridine (0.99385g; 9.188mmol) was then added to this solution. The reaction mixturewas stirred for one hour at 0 °C and left to stir overnight to warm to room temperature. The ligand solution was washed using dichloromethane and a solution of sodium carbonate to eliminate the majority of the urea by-product. Afterwards, the clean ligand solution was placed in a Rota-vapor instrument to remove the dichloromethane. The resulting 4-HLSMe was of a waxy consistency and a yellow color.This ligand was then run through a column chromatography to remove the coupling reagents however a TLC indicated that the ligand was not present within the solution. After pulling all of the fractions out of the column, the entire flask of solution was dried using a Rota-vapor and the ligand was eventually found. The final purified ligand was of an oily consistency and golden-yellow color. The 4-HLSMe was then run through a 1H NMR and was confirmed to be pure. |
  |  [Ni(C2H3O2)2] ∙ 4H2O. 21.838 grams of the nickel acetate was poured into a 500mL beaker. While the beaker was heated, water was periodically added until the resulting solution was supersaturated and could no longer dissolve any solute. Afterwards, the supersaturated solution was covered with a watch-glass and left to crystallize through slow evaporation. After three days, a sufficient number of crystals had formed on the bottom of the beaker and were harvested. The crystals were left to air dry for an additional day before being crushed to a fine powder (7.2078g) and placed in a vacuumed, round-bottom flask to draw out as much water as possible. The dried powder was 7.1344g and it was found that 33.337% of the original solute crystallized. This powder was then run through an IR spectrophotometer and was confirmed to be pure with peaks at 3354.44cm-1, 2945.22 cm-1, 2832.86 cm-1, 1449.21 cm-1, 1114.95 cm-1, and 1027.97cm-1. A UV-Vis was run at 10mM and the nickel acetate was characterized with peaks at 265nm, 267nm, 269nm, 352nm, and 401nm. |
  |  [Co(C2H3O2)2] ∙ 4H2O. 19.998 grams of the cobalt acetate was poured into a 500mL beaker. While the beaker was heated, water was periodically added until the resulting solution was supersaturated and could no longer dissolve any solute. Afterwards, the supersaturated solution was covered with a watch-glass and left to crystallize through slow evaporation. After five days, a sufficient number of crystals had formed on the bottom of the beaker and were harvested. The crystals were left to air dry for an additional day before being crushed to a fine powder (11.9662g) and placed in a vacuumed, round-bottom flask to draw out as much water as possible. The dried powder was 11.8698g and it was found that 55.464% of the original solute crystallized. This powder was then run through an IR spectrophotometerband confirmed to be pure with peaks at 3404.93cm-1, 2948.31cm-1, 2522.96cm-1, 2225.07cm-1, 2044.30cm-1, 1654.37cm-1, 1449.21cm-1, 1114.65cm-1, and 1032.87cm-1. A UV-Vis was run at 10mM and the cobalt acetate was characterized with peaks at 265nm, 267nm, and 520nm. |
[Ni(C2H3O2)2(3-HLSMe)n] ∙ 4H2O.The nickel acetate (0.0224g) was dissolved in a solution of methanol and3-HLSMe(18.0mM; 5.0mL). This clear, lime-green solution of ligand and acetate was left in a capped vial covered with Parafilm to evaporate the excess methanol. Afterwards, diethyl ether diffusion was prepared for the solution and it was left to crystallize. Due to time constraints, the solution was unable to crystallize and thus, all of the solvent was pulled off using a Rota-vapor leaving an oily, forest-green colored substance. This substance was then run through an IR and a UV-Vis at 2.5mM to confirm that the inorganic synthesis had been successful (See Results and Discussion).
[Ni(C2H3O2)2(4-HLSMe)n] ∙ 4H2O.The nickel acetate (0.04927) was dissolved in methanol (1.0mL) resulting in a clear, lime-green solution. A solution of methanol and 4-HLSMe(9.188mM; 2.0mL) was then mixed with the nickel solution resulting in a more diluted, clear, lime-green color. This solution of ligand and acetate was left in a capped vial covered with Parafilm to crystallize through slow evaporation. Due to time constraints, the solution was unable to crystallize and thus, all of the solvent was pulled off using a Rota-vapor leaving an oily, pastel-green colored substance. This substance was then run through an IR and a UV-Vis at 5mM to confirm that the inorganic synthesis had been successful (See Results and Discussion).
[Co(C2H3O2)2(3-HLSMe)n] ∙ 4H2O.The remaining 3-HLSMe ligand was lost and due to time constraints, it was not purified for further use. Therefore, the inorganic synthesis of the cobalt acetate and the 3-HLSMeligand was not possible.
[Co(C2H3O2)2(4-HLSMe)n] ∙ 4H2O.The cobalt acetate (0.04932) was dissolved in methanol (1.0mL) resulting in a clear, dark-pink solution. A solution of methanol and 4-HLSMe (9.188mM; 2.0mL) was then mixed with the cobalt solution resulting in a salmon color. This solution of ligand and acetate was left in a capped vial covered with Parafilm to crystallize through slow evaporation. Due to time constraints, the solution was unable to crystallize and thus, all of the solvent was pulled off using a Rota-vapor leaving an oily, wine-red colored substance. This substance was then run through an IR and a UV-Vis at 2.5mM to confirm that the inorganic synthesis had been successful (See Results and Discussion). Powered by
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