Synthesis and characterization of
tris(acetyacetonato)chromium(III)
Prof. Jhon Fredy Pérez-Torres
Inorganic Chemistry Laboratory II – 24733 – School of Chemistry
2025-I
1 Introduction
The tris(acetylacetonato)chromium(III), also known as chromium(III) acetylacetonate, is a coordi-
nation compound fromed by one unit of the transition metal ion Cr3+ and three units of the ligand
acetylacetonate CH3 COCHCOCH3 – (acac – ). Under normal conditions Cr(acac)3 is a red-violet
odorless solid, of density ρ = 1.34 g/mL, melting point T = 214 ◦ C and boiling point T = 340 ◦ C.
The Cr(acac)3 is insoluble in water but soluble in nonpolar organic solvents. Chromium(III) acety-
lacetonate has been employeed as a dietary supplement and pharmaceutical agent1 . Figure 1 shows
the structure of the optical isomer ∆ – Cr(acac)3 .
O
O O
Cr
O O
O
Figure 1: Structure of ∆ – Cr(acac)3
1
Chromium acetylacetonate as a dietary supplement and pharmaceutical agent:
[Link]
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Inorganic Chemistry Laboratory II – 24733 School of Chemistry
2 Objectives
Synthesize and characterize the coordination compound Cr(acac)3 .
Obtain the crystal field parameter Dq and the Racah parameter B of the coordination com-
pound Cr(acac)3 from the UV-Vis espectrum.
3 Reagents 10 mL erlenmeyer
Chromium trichloride hexahydrate, 25 and 50 mL beakers
CrCl3 · 6 H2 O(s)
1 mL pipet, pipet bulb
Acetylacetone (2,4–pentanodione),C5 H8 O2 (l)
Thermometer
Urea, NH2 CONH2 (s)
Microwave synthesis reactor
Ethanol, C2 H5 OH(l)
IR spectrophotometer
4 Materials UV-Vis spectrophotometer
Balance and teflon coated spatula Magnetic susceptibility balance
5 Hazards
Eye protection, laboratory coat and gloves should always be worn. All the experimental procedure
should be done in a fume hood.
6 Synthesis (part I)
We follow the protocol reported by W. C. Fernelius et. al. [3]. Place 1 mmol (266 mg) of
CrCl3 · 6 H2 O(s) and 3 mL of distilled water in a 10 mL erlenmeyer. Add 500 mg of urea in four
steps with gentle stirring during 15 minutes. Add to the system, dropwise, 1 mL of acetylacetone
from a 1 mL pipet. Using a hot plate, heat the mixture in a water bath set to 80 ◦ C during 1 hour,
or transfer the mixture to a 10 mL vessel and heat the mixture in a microwave synthesis reactor
set to 150 ◦ C during 3 minutes. Dark crystals should appear. Allow the reaction system to cool
at room temperature and isolate the crystals using a Hirsch funnel. Wash the crystals with water.
Dry the product in the stove set to T = 60 ◦ C for 10 minutes. Weigh the synthesized compound
and store it in a sterile container.
7 Characterization (part II)
Measure the melting point of the synthesized coordination compound. Record the IR and UV-Vis
spectra. For the UV-Vis spectrum, prepare a 5 mM solution of the coordination compound in
ethanol and measure the absorption from 400 nm to 750 nm.
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Inorganic Chemistry Laboratory II – 24733 School of Chemistry
References
[1] F. Dolati, M. Vakili, A. Ebrahimi, and S. Tayyari. Vibrational spectra of
tris(acetylacetonato)chromium(III). J. Mol. Struct., 1099:340, 2015. doi:[Link]
10.1016/[Link].2015.05.058.
[2] Y.-S. Dou. Equations for calculating Dq and B. J. Chem. Educ., 67:134, 1990. doi:https:
//[Link]/10.1021/ed067p134.
[3] W. C. Fernelius, J. E. Blanch, B. E. Bryant, K. Terada, R. S. Drago, and J. K. Stille. Inorganic
Syntheses. McGraw-Hill, 1957. doi:[Link]
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Inorganic Chemistry Laboratory II – 24733 School of Chemistry
Report
Practice: Date:
Student: Group: Subgroup:
Professor:
1. Write down the corresponding chemical reactions and provide the percentage yield of the
synthesis. How does urea contribute to the synthesis process? Melting point of Cr(acac)3 :
measured , reported: .
2. Generate the IR spectrum of the coordination compound and explain the most relevant (at
least 3) signals [1].
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Inorganic Chemistry Laboratory II – 24733 School of Chemistry
3. Assuming a Oh point group, draw the crystal field splitting diagram inserting the metal d
electrons and indicate if the coordination compound will undergo a geometrical distortion
(Jahn-Teller effect).
4. Plot the UV-Vis-NIR (attenuation coefficient vs. wavelength) spectrum. Indentify the d-d
transitions and obtain the crystal field parameter Dq and the Racah parameter B. Equations
for calculating Dq and B can be found in Ref [2].
5. From the magnetic susceptibility and the recorded room temperature, obtain the effective
magnetic dipole moment µeff of the Cr(acac)3 compound and compare with the value calcu-
lated from the “spin-only” formula.
