Synthesis, reactivity and

spectra of
Tris(Acetylacetonato)Cobalt(I
II)
Experiment 3

Introduction:
The aim of the experiment is to synthesisze ()() [()3 ]. The
copper complex was then nitrated with () to form[( 2 )3 ],
the complexes were both analyzed in infrared, electronic spectra and NMR. The melting points for the
complexes were measured.
Method:
The method was done as in the inorganic chemistry third year practical guide.
Results:
Table1: The table illustrating the percentage yield, structure of the complex and melting points
C Yield (g)
o
m
p
o
u
n
d
f
o
r
m
u
l
a
e
[()
2.33 3 ]

[(
0.55
2 )3 ]

Perc
enta
ge
yield
(%)

Melting
pointd()

31.1
0

204-210

39.9
0

196-200

Structure of complex

Calculation protocol for percentage yield:

 = 3 ()()3
23 + 6 + 2 2 2[()3 ] + 22 + 42
(3 ) =

2.5
118.941

= 0.02013

(1: 1) (23 : 2[()3 ])

The ([()3 ]) = 0.0201
([()3 ]) = = 0.0201 359.281 = 7.552
% =

2.33

100% = 7552 100% = 30.85%

For nitrated complex

[( 2 ]
(3 )2 + 32 + 2(3 )2 (3 ) 32 + 23 2 + 2
[()3 ] + 33 2 2 [( 2 )3 ] + 33 2

(()3 ) = = 359.281 = 0.002783

(1: 1) ()3 : [( 2 )3 ]
Then ([( 2 )3 ]) = 0.00278
So ([( 2 )3 ]) = = 0.00278 494.2729 = 1.376
% =

0.55

100%0 = 1.376 100% = 40%

Table 2: Table illustrating UV/visible spectra for two complexes formed.

Complex formed

Color of complex
Absorbed color
Wavelength peak(nm)
Dark green
520,18
Green
[Co(acac)3]
Dark green
520,18
Green
[Co(acac-NO2)3]
The peaks are not visible; the use of literature values was used for the completion of the results.
Table 3: The IR data and the observed peaks
Peaks , Possible Function
groups
C-H
C=O
Discussion

1
2966.37
1569.10

The experiment involves the synthesis of Tris(Acetylacetonato)cobalt(III), ()2 and the nitration of
the complex to form the nitrated compound (( 2 )3 ), below is the balanced chemical
reaction
23 + 6 + 2 2 2[()3 ] + 22 + 42
The experiment procedure resulted in small yield of the products which is 38%, the most products got
lost in the addition of the oxidizing agent the hydrogen peroxide which coursed the bubbling and the
splitting of the reagent at the beginning of the practical.
The color of the complex is dark green color with the literature absorbance wavelength which shows
that the absorbed color of the complex is purple which a complementary color of the green color at that
is given wavelength number. The melting point of the complex is at 204 210 and the literature
melting point for the complex is at 201 213 these results shows that the complex has an impurity
thats why it has low melting point.
The nitration of [()3 ] to form(( 2 )3 ), below is a balance equation
(3 )2 32 + 2(3 )2 (3 ) 32 + 23 2 2
The yield of the products was 40% which is a low yield, this was brought by the process of
recrystallization and the products were lost in the process, the use of chloroform to was going to help
crystalize most of the products but it was not used. The color of the complex is green with the
wavelength of 520nm from the literature and purple is the absorbed complementary color of the
complex.
The melting point of the complex is at 196 200, with the literature melting point at 197
198 so which this indicate that the product has impurities since it was not washed with ethanol to
make them pure.
Assignment
Question 1: discussed above
Question 2
Free ligands

[Co(acac)3]

[Co(acac-NO2)3]

Question 3
Chelation is a process which involves ligands with more two or more binding sides to bond to a metal.
This process allows ligands with bi-dentate characters to bind to a central metal atom to form a ring like
structure.
Question 4
The spectrum bands and possible functional groups is indicated at table 3, the IR spectrum for nitrated
compound [Co(acac-NO2)3] the spectrum is not included the analyses was not done for that

reason. The functional groups for [Co(acac)3] C-H is at 2966.37cm-1 and C=O is at
1569.10cm-1. The bands are not the same due to transmittance which is different, the NO2
band is not available in the spectrum but is at 822.16 according to literature books
Shalhoub(1980) and this could have been nicely observed in IR spectrum of the nitrated
complex which is not available.
Question5
The HNMR show only for peaks which are proton based peaks. The peak at 1.90 shows a water
molecule and it has two hydrogen atoms in it. The peak at 5.38 represents the solvent
molecules containing the hydrogens atoms in it. There are two peaks up field which are
2.099m and 3.49pm and the show hydrogens from acac-ligands and methyl groups
respectively.
Question 6

Comments

The practical was centered on the analyses of the spectrums which is still new at level but
gaining experience and the preparation of the crystals was success but the analyses took much
of the time.

Bibliography
Atkins, A., T, O., Rourke, J., M, W., & F, A. (2010). Shriver And Atkin's inorganic chemistry. New York:
Oxford university press.
Shalhoub. (1980). synthesis reaction and spectr. chemistry education, 525-526.
Smith. (2011). Organic chermistry. New York: McGraw-Hill.