Transition Metal Synthesis

Report Rubric
Purpose The purpose of this lab is to synthesize two transition metal complexes, determine their percent
yield and percent composition, as well as understand the difference between kinetic and thermodynamic
products.
Data
Part A:
Table 1. Summary of synthesis data and results.
Desired Product u!"py #u!$
%
"py
Mass of u! #&$ .%'( .%)*
Mass of "py #&$ .'+, .+-(
.xperimental /ield #&$ .'*0 .*,,
olor red yellow
Theoretical /ield #&$ .')) .%1',
2 /ield (*.- ,+.+0
Part B:
Table 2. Absorbance data for the standards.
Solution 3bs onc. #M$
3 .-%, .+*
" .'(0 .++,
.1-0 .++-
D .%1% .++'
. .**1 .++%
Table 3. Concentrations and Mass % of Copper(II in samples.
Product
Mass of
Sample
tested (g)
Abs
Cu
2+
(mol/L)
Cu
2+
in
sample
(moles)
Cu
2+
in
sample
(grams)
Mass % Cu
in Sample
Teoretical
% Cu
%
!rror
Cu"#p$ %&'& %2'( %&&)* %&&&22* %&+)2( +,%', +'%-- 2%*
(Cu")2#p$ %&'+ %-** %&&**+ %&&&2,** %&+,* 2+%. 2-%.. '%,
Calculations
Mass of "py alc4
Theoretical /ield alc4
Theoretical 2 Mass u alc4
"eer56ambert 6aw alc4
Grams of Cu
+2
and Experimental % Cu Calc:
% Yield Calc:
% Error Calc:
Discussion:
!n this experiment we synthesized two transition metal compounds from the same set of reactants
by manipulatin& the limitin& rea&ent to dri7e the reaction toward one product or the other. 8urthermore,
we had to calculate the percent yield and percent copper composition of both.
8rom our experiment we obtained percent yields of ,+.+02 and (*.-2 for #u!$
%
"py and u!"py
respecti7ely. !f comparin& our percent yield to the standards in 9o&el:s textbook of practical or&anic
chemistry they would be considered excellent for the (*.-2 and 7ery &ood for the ,+.+02. Some
possible sources could be loss of product throu&h the 7arious transfers from flask to beaker or throu&h
filtration. 3lso, another source of error could be that there was still some moisture in the final product
when we measured it thus throwin& off the percent accuracy as well. 8inally, one last source of error is
product impurity. There could be some traces of the kinetic product in the thermodynamic sample or
thermodynamic product in the kinetic sample, and thus throw off our percent yield.
!n terms of 2 copper composition we obtained experimental 7alues of *0.,02 and %*.-2 for
u!"py and #u!$
%
"py respecti7ely. These experimental 7alues when compared to the theoretical 7alues
ha7e a acceptable mar&inal percent error of %.)2 and ,.02 respecti7ely. There are se7eral sources of
error that could ha7e caused the discrepancies between our experimental and actual 7alues. 8irst, because
we did not test for purity of the product, there could be contamination from traces of kinetic product in the
thermodynamic sample or contamination from traces of thermodynamic product in the kinetic sample.
This will throw our results off because each has a different percent copper composition. Second, because
the readin& on the spectrophotometer had to be read by humans there is a certain de&ree of uncertainty
whether the absorbance read .1% or say .11 and that can affect the concentration that we calculate.
8urthermore, any fin&erprints or residue on the cu7ettes could also affect the spectrophotometer readin&
and thus our percei7ed concentration that was used to calculate 2 copper composition.
The other important concept in coordination chemistry is the color of the compound. The two
products that we obtains were yellow and red. The specific colors of each product maes sense chemically
speain! for se"eral reasons. #irst$ color results from the electrons absorbin! li!ht of certain fre%uencies
to excite their electrons to a hi!her ener!y le"el$ and reflectin! li!ht of fre%uencies it can&t use. The
different colors we see results is due to the ma!nitude of splittin! between the d orbitals. The ma!nitude
of splittin! is caused by the types of fields produced by the li!ands attached to the metals. 'ea field
li!ands such as the halo!ens cause a small amount of splittin! while stron! field such as compounds
containin! nitro!en ha"e stron! amounts of splittin!. This is why Cu()*py is red and +Cu(,
2
*py is yellow.
(n Cu()*py each copper is surrounded by - iodine and only one nitro!en from *py$ while +Cu(,2 *py is
surrounded by 2 iodines and 2 nitro!ens from *py. Therefore$ +Cu(,
2
*py should ha"e a hi!er splittin! of
d orbitals and thus absorb li!ht of a hi!her fre%uency than Cu()*py. This is in fact what we see as Cu(*py
is red which means that the compound absorbed li!ht of the complementary wa"elen!th !reen. .n the
other hand +Cu(,
2
*py is yellow$ which means that it absorbed purple li!ht. /urple li!ht has a hi!her
fre%uency than !reen li!ht which a!rees with our conclusion that +Cu(,
2
*py has !reater field splittin! than
Cu(*py. #urthermore$ the fact that the splittin! in +Cu(,
2
*py is !reater than the splittin! of Cu(*py
mirrors the fact that +Cu(,
2
*py is the inetic product and Cu(bpy is the thermodynamic product. *ecause
Cu(*py is the thermodynamic product$ it is more stable$ which is reflected in its weaer field splittin!$
lower free ener!y. 'hile on the hand$ since +Cu(,
2
*py is the inetic product$ it is more unstable$ and
therefore has a stron!er field splittin!$ hi!her free ener!y.
Transition Metal Post Lab Questions
0. 1ow many bonds would each of the followin! chelates form with a metal ion2
a. 3iethylenetriamine) Two
41
2
5 C1
2
5 C1
2
5 41 5 C1
2
5 C1
2
5 41
2
b. 6alen)four
c. 7cetylacetone) two
d. Glutamic 7cid$ an amino acid side chain found in proteins) one
2.
a. 1ow many d electrons does Cu
+
ha"e2 Cu
2+
2
Cu
+
has 08 d electrons and Cu
+2
has 9 d electrons.
b. 3raw the d orbital splittin! for the metal centers in the compounds you made$ with the
correct oxidation state for copper. :emember$ your compounds were 4.T octahedral. 6ee
pp!. 9;8)9;< in =umbdahl for help drawin! the correct d orbital dia!ram.
c. 7ccordin! to the dia!ram from part b.$ should your compound be colored2 'hy or why
not2
Yes our compounds should be colored because they do not ha"e a full d electron set.
Therefore$ electrons can absorb li!ht of a certain wa"elen!th to excite themsel"es and
reflect the rest which results in the colors we see.
d. .b"iously it has a "ery stron! color. 'hy is this the case2
The stron! color results from the electrons absorbin! li!ht of certain fre%uencies to excite
their electrons to a hi!her ener!y le"el$ and reflectin! li!ht of fre%uencies it can&t use. The
u!5"py
#u!$
%
"py
different colors we see results is due to the ma!nitude of splittin! between the d orbitals.
The ma!nitude of splittin! is caused by the types of fields produced by the li!ands attached
to the metals. 'ea field li!ands such as the halo!ens cause a small amount of splittin!
while stron! field such as compounds containin! nitro!en ha"e stron! amounts of splittin!.
This is why Cu()*py is red and +Cu(,
2
*py is yellow. (n Cu()*py each copper is
surrounded by - iodine and only one nitro!en from *py$ while +Cu(,2 *py is surrounded
by 2 iodines and 2 nitro!ens from *py. Therefore$ +Cu(,
2
*py should ha"e a hi!er splittin!
of d orbitals and thus absorb li!ht of a hi!her fre%uency than Cu()*py. This is in fact what
we see as Cu(*py is red which means that the compound absorbed li!ht of the
complementary wa"elen!th !reen. .n the other hand +Cu(,
2
*py is yellow$ which means
that it absorbed purple li!ht. /urple li!ht has a hi!her fre%uency than !reen li!ht which
a!rees with our conclusion that +Cu(,
2
*py has !reater field splittin! than Cu(*py.
-. 3raw an ener!y dia!ram comparin! the thermodynamic and inetic products. >abel the followin!:
reactant$ thermodynamic and inetic product$ acti"ation ener!y +E
a
,$ chan!e in enthalpy +?1,.
@*ecause this is a dia!ram of free ener!y$ but the %uestion ass for labelin! of ?1$ we assume that
?G
Reaction oordinate
8
r
e
e

.
n
e
r
&
y
Reactants
Products Products
atalyzed Reaction
;ncatalyzed Reaction
the ?1 is proportional to ?G.
a. 'hat can you do to mae the inetic product instead of the thermodynamic product2 The
thermodynamic product instead of the inetic product2
.ther than chan!in! the ratio of the reactants and picin! a limitin! rea!ent that forces the
formation of the thermodynamic or inetic product$ if we wanted to mae the inetic product
instead of the thermodynamic product$ we can do se"eral other thin!s. #irst$ we can run the
reaction at lower temperatures so that there is not enou!h ener!y to o"ercome the hi!her acti"ation
ener!y re%uired for the thermodynamic product. 7lso by allowin! the reaction to run for only brief
periods of time$ you will be able to pre"ent your inetic product from spontaneously turnin! into
the thermodynamic one. (f you wanted to mae your thermodynamic product instead of the inetic
product$ you should run the reaction at hi!her temperatures so that the acti"ation ener!y for the
thermodynamic product can be surpassed. #urthermore$ allowin! the reaction to run for extended
periods of time will cause any inetic product that does form to turn into the thermodynamic
product spontaneous because it is more stable.
A. Figure 1 shows the different B. dia!rams for your two complexes. >abel each dia!ram as
belon!in! to the thermodynamic or inetic product$ based on the color of the product.
C. >etDs say you wanted to mae a networ similar to what you did in lab$ but you donDt want to use
iodine. The other options you ha"e a"ailable in your lab that could be used as li!ands are the
followin!:
<inetic Product Thermodynamic Product
'hich one could you use as a "iable substitute for (
)
2
1ydroxide would probably be the next best thin! as a substitute for (odine because it most closely
resembles the number of lone pairs of iodine and therefore can chelate more than once to lin metals in a
networ. The other two only ha"e one lone pair free and therefore cannot form networ metals because
they can only bind to one metal atom.