Synthesis and characterization of cobalt complexes (Day 3)

Part 1. Synthesis

[1.6] Resolution of [Co(en)3]Cl3 as [(+)-Co(en)3][(+)-tartrate]Cl5H2O

Add [Co(en)3]Cl3 (1.2 g, 3.5 mmol) and L-(+)-tartaric acid (0.65 g, 4.4 mmol) in 5 mL water. Add sodium hydroxide
(0.35 g, 8.75 mmol) and cover solution. Gently stir the mixture and heat without boiling until the solids completely
dissolve. Add more water, if needed. Let the solution cool at room temperature. Cover and store in the locker (make
sure the container is sealed at the very least with Parafilm) for 2 days. Then, collect the dark orange crystals via
filtration. Set aside the filtrate! Wash the crystals with cold 1:1 acetone:water, then cold acetone. Air dry the [(+)Co(en)3][(+)-tartate]Cl5H2O crystals.
[1.7] Preparation of [(+)-Co(en)3]I3H2O
In a beaker, add 0.5 g [(+)-Co(en)3][(+)-tartate]Cl5H2O and break the crystal into smaller pieces. Prepare an NaOH
solution (concentration ~ 1 pellet/15 mL water). Then, add ~3.3 mL of this NaOH solution to the [(+)-Co(en) 3][(+)tartate]Cl5H2O crystals. With stirring, heat the crystals gently until all solids dissolved. DO NOT heat the Co
complex for more than 5 minutes. Add 0.9 g sodium iodide. Continue heating and stirring for 1 minute. Then, cool in
an ice bath. Filter off the crystals, and wash the crystals with an ice cold solution of 0.75 g sodium iodide in 2.5 mL
water. Then, wash with cold ethanol, then cold acetone.
[1.8] Preparation of [()-Co(en)3]I3H2O
Dilute the filtrate from part [1.6], Day 2 to 7.5 mL with water. Add 1/4 pellet of sodium hydroxide. Heat the solution
gently until NaOH dissolves, and add with stirring 2.1 g sodium iodide. Cool the solution in ice bath. Wash the
precipitate with an ice cold solution of 0.75 g sodium iodide in 2.5 mL water. Then, redissolve the precipitate, with
stirring in 8.7 mL water at 50oC. Filter off the undissolved racemate. To the filtrate, add 1.25 g sodium iodide. Cool the
filtrate in an ice bath. Filter off crystals. Wash with cold ethanol, then cold acetone.
Part 2. Characterization
[2.1]

UV-Vis spectroscopy

Prepare ~1 mM solutions of complexes with the minimum amount of required solvent. Choose a solvent (water,
ethanol, acetone, or toluene) where the complex is soluble. Obtain the UV-Vis spectra of the complex solutions.
[2.2]

FTIR spectroscopy

Prepare a minimum amount of complex and grind with KBr in an agate mortar in 1 1:10 ratio. Obtain the IR diffuse
reflectance spectrum (DRS) of the complex.
[2.3]

Magnetic susceptibility balance

Warm up the balance for at least 30 min.

Choose a range (x1 or x10) by adjusting the RANGE knob.
Adjust the ZERO knob until the display reads 000. The zero should be readjusted if the range is changed.

Place an empty tube of known weight into the tube guide and take the reading R0. Rezero the instrument before each
measurement.
Fill the sample tube with the sample and tap the bottom of the tube gently to pack the sample. You must have at least
1.5 cm of solid to obtain a stable reading. Measure the height L of the sample in cm. Obtain the sample mass m, in
grams.
Rezero, place the packed sample tube into the tube guide, and take the reading R.
Empty the sample tube and rinse it with a suitable solvent.