(CR (Acac) 3) ....

EXP. NO.
0 1
St. Name: Qamar Issa Hammad

Reg. No: 2 2 0 0 2 3 5
Date of the experiment: 3/ 3 / 2024 Date of submission: 31 / 3 / 2024
Synthesis and characterization of [Cr(acac)3] and [Cr (Br-acac)3]
Abstract (100-500) words:

In this experiment I prepared two complexes first, I prepared a Tris(acetylacetonato)
chromium (III) and Tris (bromo-acetylacetonato) chromium (III) The Chromium complex was
synthesized with the use of chromium (III) chloride hexahydrate CrCl3.6H2O , urea,
N-bromosuccinimide , chloroform , ethanol, NaHSO3 and acetylacetone acting as a ligand. then I
measured the physical properties of them like melting point, molecular wight, conductivity,
magnetism, and UV/VIS spectra.
Introduction (1000-3000) words:
In our experiment the ligand is acetylacetone (acac-) which will be prepared by removing the
acidic proton from the acacH is provided by ammonia, the ammonia is generated slowly by the
hydrolysis of urea to produce OH - in aqueous solution, which removes the acidic hydrogen in
acetylacetone in the presence of the chromium ion
The bromo derivative of tris(acetylacetonato)chromium(III), Cr(Br-acac)3 is prepared by the

bromination of tris(acetylacetonato)chromium(III) using N-bromosuccinimide (NBS)
Acetylacetone CrCl3·6H2O Urea
N-Bromosuccinimide
[Cr(acac)3]
Preparation:
1) [ Cr(acac)3 ]
Reaction scheme:
Balanced chemical reactions:
CrCl3·6H2O + 3C5H8O2 → Cr(C5H8O2)3 + 6H2O + 3Cl
Notes:
The room temp was 16C °
1- I added 100 ml distilled water in 250 Erlenmeyer flask then 5.357 g of CrCl3·6H2O (Source
of Cr+3) after chromium salt has dissolved.
2- Add 20.041 g of urea (hydrolysis of urea in H2O produce NH3 to deprotonation of acidic H
in acac) and 11.8 ml of acetylacetone (Source of acac) in Erlenmeyer flask.
(Warning: Acetylacetone is flammable, highly toxic, and an irritant liquid. Do not expose it
to fire)
3- I heated the mixture using a water bath (add boiling stones to the beaker) until
the water boil then keep it boiling mildly for 2 hours (to increase the rate of rxn).
4- After a while a deep maroon crystal will begin to form as the urea releases ammonia and
solution becomes basic.
5- Cool the reaction flask to room temperature then placing the flask in a beaker containing
cold water.
6- then collected the product by suction filtration and washed the crystals with several
small amounts of distilled water.
7- I Transferred the crystalline product to a watch glass and dry in oven at temperature less
than 100C °
Deep maroon crystal forms The first few minutes of heating

Preparation:
2) [ Cr(Br-acac)3]
Reaction scheme:
Balanced chemical reactions:
3NBS+Cr(C5H8O2)3→ [Cr (Br-C5H8O2)3] + 3NHS
Notes:
1- 2.041g of NBS (source of Br) 2.011 g of [Cr(acac)3] (that was prepared
from the previous section) in 70 ml of chloroform the heating on the
hotplate for 5 min. The solution turns green, and a brown precipitate form.
2- Then cool to room temp then in ice bath.
3- after cooling, I collected the brown solid by suction filtration and washed
with 5ml 95% ethanol, two 5ml pf 5% NaHSO3 (to remove Br which didn’t
react.), 5ml of water and two 5 ml of hot 95% ethanol.
4- Finally, Air dry the product.
Product morphology, state, and colour (add image):
1. [ Cr(acac)3 ]
Limiting reagent: CrCl3.6H2O
Theoretical mass (product): 7.0213
Experimental mass: 3.996 g
Yield (%): 56.9%
Literature yield:
Ref.:
Deep maroon
Product morphology, state, and colour (add image):
2. [ Cr(Br-acac) ]
Limiting reagent: NBS
Theoretical mass (product): 2.263
Experimental mass: 2.136 g
Yield (%): 94%
Literature yield:
Ref.:
Brown
1- Melting point measurement
[Cr(acac)3]
Literature value: 216 C °
Ref.: https://www.americanelements.com/chromium-acetylacetonate-21679-31-2
Experimental value: 216 C ° or decomposed.
2- Melting point measurement
[Cr(Br-acac)3]
Literature value: 225 C °
Ref.: https://jns.kashanu.ac.ir/article_43175_db4a9aacce6bffea266e0c130b3429e5.pdf
Experimental value: 219 C °
Cr(acac)3
Cr (Br-acac)3
1- Molecular weight measurement
[ Cr(acac)3 ]
Molecular weight (periodic table): 349.32 g/mol
Mass of test tube and biphenyl: _____________
Mass of empty test tube: ______________
Mass of biphenyl used: 1.674g +/- 0.0001
Time (s) 30 60 90 120 150 180 210 240 270 300 330
Temp. (C) 63
Molecular weight (experimental): 335.48 g/mol
2- Molecular weight measurement
[ Cr(Br-acac) ]
Molecular weight (periodic table): 592.0556 g/mol
Mass of test tube and biphenyl: _____________
Mass of empty test tube: ______________
Mass of biphenyl used: 1.599 +/- 0.0001
Time (s) 30 60 90 120 150 180 210 240 270 300 330
Temp. (C) 67 65 64
Molecular weight (experimental): 290.18 g/mol
Conductivity
1. [ Cr(acac)3 ]
Theoretical number of ions (expected) 4

Mass of complex (g) 0.0336 g
Volume of solution (mL) 100 ml
Concentration of complex ions (mol)/L 9.62x10-4
Conductance of pure solvent, C (s(ohm-1)) 4x10-7
Conductance of solution, C (s(ohm-1)) 1.2x10-6
Cell constant, k 1.2
C, (s(ohm-1)) 8x10-7
Specific conductance of solution, L(kC) 9.6x10-7
Molar conductivity 0.9979
Experimental number of ions
2. [ Cr (Br-acac)3 ]
Theoretical number of ions (expected) 4

Mass of complex (g) 0.0589g
Volume of solution (mL) 100 ml
Concentration of complex ions (mol)/L 9.95x10-4
Conductance of pure solvent, C (s(ohm-1)) 4x10-7
Conductance of solution, C (s(ohm-1)) 6x10-7
Cell constant, k 1.2
C, (s(ohm-1)) 2x10-7
Specific conductance of solution, L(kC) 2.4x10-6
Molar conductivity 2.412
Experimental number of ions
Magnetism
1- [ Cr(acac)3 ]
Theoretical number of unpaired electrons: Cr+3 has d3 = 3 unpaired electrons
F 15.9 F(sample) 19
F` 15.8983 F`(sample) 18.9983
W 0.4639
T 294.15 k
106 5.88  (sample) 1.457x10-5
W 0.9627 Molar Weight 349.32

m 5.090x10-3
 0.02295 m` 2.254x10-3
ß 0.3546 µ 3.516
∑ 1.7x10-3 n 2.7≈3
2- [ Cr(Br-acac)3 ]
Theoretical number of unpaired electrons: Cr+3 has d3 = 3 unpaired electrons
F 15.9 F(sample) 11.7
F` 15.8983 F`(sample) 11.6983
W 0.5238
T 294.15 k
106 5.88  (sample) 7.9x10-6
W 0.9627 Molar Weight 592.0556

m 4.714x10-3
 0.02295 m` 4.883x10-3
ß 0.3546 µ 3.389
∑ 1.7x10-3 n 2.5≈3
UV-visible spectroscopy analysis
Assign peaks and calculate splitting energy.
FT-IR spectroscopy analysis
Ligand FTIR
Complex FTIR
Assign bands and compare differences.
Summary
Discuss the reaction features.
Discuss the electronic structure based on spectroscopy techniques.

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EXP. NO.

St. Name: Qamar Issa Hammad

Date of the experiment: 3/ 3 / 2024 Date of submission: 31 / 3 / 2024

Synthesis and characterization of [Cr(acac)3] and [Cr (Br-acac)3]

Abstract (100-500) words:

Introduction (1000-3000) words:

The bromo derivative of tris(acetylacetonato)chromium(III), Cr(Br-acac)3 is prepared by the

Deep maroon crystal forms The first few minutes of heating

Limiting reagent: CrCl3.6H2O

Theoretical mass (product): 7.0213

Experimental mass: 3.996 g

Yield (%): 56.9%

Limiting reagent: NBS

Theoretical mass (product): 2.263

Experimental mass: 2.136 g

Yield (%): 94%

Theoretical number of ions (expected) 4

Theoretical number of ions (expected) 4

W 0.9627 Molar Weight 349.32

W 0.9627 Molar Weight 592.0556

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