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A.

TITLE OF EXPERIMENT
Making cis and trans of potassium dioxalatodiaquochromate(III)

B. DATE OF EXPERIMENT
Wednesday, 23rd October 2019 / 09:30 – 12:00 WIB

C. PURPOSE OF EXPERIMENT
1. To learn making complex salt potassium dioxalatodiaquochromate(III)
2. To learn the precipitate of cis and trans complex salt of potassium
dioxalatodiaquochromate(III)

D. BASIC THEORIES
1. Cis and Trans Isomerism
Cis–trans isomerism, also known as geometric isomerism or
configurational isomerism, is a term used in organic chemistry. In the
context of chemistry, cis indicates that the functional groups are on the same
side of the carbon chain while trans conveys that functional groups are on
opposing sides of the carbon chain. Cis-trans isomers are stereoisomers,
that is, pairs of molecules which have the same formula but whose
functional groups are rotated into a different orientation in three-
dimensional space. It is not to be confused with E–Z isomerism, which is an
absolute stereochemical description. In general, stereoisomers contain
double bonds that do not rotate, or they may contain ring structures, where
the rotation of bonds is restricted or prevented. Cis and trans isomers occur
both in organic molecules and in inorganic coordination complexes
(Reusch, 2010).
Physical properties, such as the boiling points of cis and trans
containing compounds. Cis and trans are not structural isomers, because the
order of bonding of atoms and locations of the double bonds is the same.
This isomer pair is included in the stereoisomer category. Cis and trans
isomers in a compound can affect its boiling point, so that cis and trans-
containing compounds can be separated by distillation. Differences between
isomers are generally caused by differences in molecular shape or the
overall dipole moment. The difference is seen at the boiling point of the 2-

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pentene straight chain alkene (boiling point of the trans isomer 36°C and the
cis isomer 37°C). The difference between the cis and trans isomers can also
be very large, as in the case of cycloocene. The cis isomer compound has a
boiling point of 145°C, while the trans isomer is 75°C (Wiberg, Wiberg, &
Holleman, 2001).

2. Stability
Usually for acyclic systems trans isomers are more stable than cis
isomers. This is typically due to the increased unfavorable steric interaction
of the substituents in the cis isomer. Therefore, trans isomers have a less
exothermic heat of combustion, indicating higher thermochemical stability
(March, 1985). In the Benson heat of formation group additivity dataset, cis
isomers suffer a 1.10 kcal/mol stability penalty. Exceptions to this rule exist,
such as 1,2-difluoroethylene, 1,2-difluorodiazene (FN=NF), and several
other halogen- and oxygen-substituted ethylenes. In these cases, the cis
isomer is more stable than the trans isomer. This phenomenon is called the
cis effect (Craig et al., 1997).

3. Cis Effect
Cis effect is defined as the labilization (making unstable) of CO
ligands that are cis to other ligands. CO is a well-known strong pi-accepting
ligand in organometallic chemistry that will labilize in the cis position when
adjacent to ligands due to steric and electronic effects. The system most
often studied for the cis effect is an octahedral complex M(CO)5X where X
is the ligand that will labilize a CO ligand cis to it. The cis effect is observed
in 6-coordinate octahedral transition metal complexes. It has been
determined that ligands that are weak sigma donors and non-pi acceptors
seem to have the strongest cis-labilizing effects. Therefore, the cis effect has
the opposite trend of the trans-effect, which effectively labilizes ligands that
are trans to strong pi accepting and sigma donating ligands (Miessler & Tarr,
2004).
The cis-labilization of 18 e− complexes suggests that dissociation of
ligand X in the cis position creates a square pyramidal transition state, which

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lowers the energy of the M(CO)4X complex, enhancing the rate of reaction
(Coley, Rogers, Green, & Jensen, 2017). The scheme below shows the
dissociation pathway of a CO ligand in the cis and trans position to the X,
followed by the association of ligand Y. This is an example of a dissociative
mechanism, where an 18 e− complex loses a CO ligand, making a 16 e−
intermediate, and a final complex of 18 e− results from an incoming ligand
inserting in place of the CO. This mechanism resembles the SN1 mechanism
in organic chemistry, and applies to coordination compounds as well (Hill
& Fink, 2011).

Figure 1 Intermediates in the substitution of M(CO)5X complexes. If


ligands X and Y are neutral donors to the complex:

4. Trans Effect
Kinetic trans effect
The intensity of the trans effect (as measured by the increase in rate of
substitution of the trans ligand) follows this sequence:

F−, H2O, OH− < NH3 < py < Cl− < Br− < I−, SCN−, NO2−, SC(NH2)2,
Ph− < SO32− < PR3, AsR3, SR2, CH3− < H−, NO, CO, CN−, C2H4

The classic example of the trans effect is the synthesis of cisplatin


and its trans isomer. Starting from PtCl42−, the first NH3 ligand is added to
any of the four equivalent positions at random. However, since Cl− has a
greater trans effect than NH3, the second NH3 is added trans to a Cl− and
therefore cis to the first NH3.

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Figure 2 The classic example of the trans effect
If, on the other hand, one starts from Pt(NH3)42+, the trans product is
obtained instead:

Figure 3 Trans product of Pt(NH3)42+


The trans effect in square complexes can be explained in terms of an
addition/elimination mechanism that goes through a trigonal bipyramidal
intermediate. Ligands with a high trans effect are in general those with high
π acidity (as in the case of phosphines) or low-ligand lone-pair–dπ
repulsions (as in the case of hydride), which prefer the more π-basic
equatorial sites in the intermediate. The second equatorial position is
occupied by the incoming ligand; due to the principle of microscopic
reversibility, the departing ligand must also leave from an equatorial
position. The third and final equatorial site is occupied by the trans ligand,
so the net result is that the kinetically favored product is the one in which
the ligand trans to the one with the largest trans effect is eliminated
(Crabtree, 2001).

Structural trans effect


The structural trans effect can be measured experimentally using X-
ray crystallography, and is observed as a stretching of the bonds between
the metal and the ligand trans to a trans-influencing ligand. Stretching by as
much as 0.2 Å occurs with strong trans-influencing ligands such as hydride.
A cis influence can also be observed, but is smaller than the trans influence.
The relative importance of the cis and trans influences depends on the
formal electron configuration of the metal center, and explanations have
been proposed based on the involvement of the atomic orbitals (Anderson
& Orpen, 2001).

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5. Potassium dioxalatodiaquochromate(III)
Complex mixture of cis and trans forms can be done by mixing non-
complex components (complex constituents). Based on the solubility
differences between the cis and trans forms, the two types of isomers can
be separated. For example, trans-dioxalatodiakuochrom(II) chloride can be
crystallized slowly by evaporation of a solution containing a mixture of cis
and trans forms. By evaporation the equilibrium form of cis ↔ trans can be
shifted to the right because the solubility of the trans isomer is lower. In
addition, the separation of cis and trans isomers is different, for example the
cis-dichlorbis (trietilstibin) complex of palladium can be crystallized in
benzene solution even though in the solution there is only 60% cis form.
Chromium is a crystalline metal that is white, not very tough and
cannot be forged with weight. It merges at 1765ºC. This metal is soluble in
dilute or concentrated acid chloride. If not exposed to air, will form ions of
chromium(II)
Cr + H+ → Cr2+ + H2↑
Cr + HCl → Cr2+ + 2Cl- + H2↑
In the presence of oxygen from the atmosphere, chromium is partially or
completely oxidized to the tervalent state:
4Cr2+ + O2 + 4H + → 4Cr3+ + 2H2O
(Hill & Fink, 2011)

E. TOOLS AND SUBSTANCES


Tools
1. Beaker glass 200 mL 1 piece
2. Watch glasses 2 pieces
3. Spiritus heater 1 set
4. Vacuum pump 1 set
5. Evaporation cup 1 piece
6. Measuring cup 25 ml 1 piece
7. Pipette 5 pieces

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Substances
1. Oxalic acid (H2C2O4) sufficiently
2. Potassium dichromate (K2Cr2O7) sufficiently
3. Ethanol sufficiently
4. Dilute ammonium hydroxide solution (0.1 M) sufficiently
5. Aquadest (H2O) sufficiently

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F. LANES WORK
1. Production of Trans Isomer of potassium dioxalatodiaquochromate(III)

3 grams H2C2O4 1 gram K2Cr2O7


- Added into beaker glass - Added into beaker glass
- Diluted it into a little of - Diluted it into a little of
boiled distilled water boiled distilled water

Solution Solution

- Mixed it into beaker glass 50 mL


- Closed it with watch glass
- Let it for a while
- Evaporated the solution using water boiling

A half solution

- Let it in the room temperature

One-third of solution

- Filtered the solution

Filtrate Residue

- Washed the residue with cool


distilled water the ethanol
- Drive it
- Written the result and started
in the percent form

Percent of residue

Reactions:
H2C2O4.2H2O(s) + H2O(l) → H2C2O4.2H2O(aq)
K2Cr2O7(s) + H2O(l) → K2Cr2O7(aq)
7H2C2O4.2H2O(aq) + K2Cr2O7(aq) → 2K[Cr(Cr2O4)2(H2O)2)](s) +
17H2O(l) + 6CO2(g)

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2. Making as isomer of potassium dioxalatodiaquochromate(III)

1 gram K2Cr2O7

- Entered into beaker glass


- Added 3 grams of H2C2O4.2H2O
- Added 1 drop of aquadest
- Covered with watch glass
- Shaken

Release water vapor and formed CO2 gas


- Added 5 mL of ethanol
- Stirred until produce precipitate (in the same direction →)
- Decanted

Residue Filtrate

- Added 5 mL of ethanol until produce crystal


- Filtered

Residue Filtrate

- Dried with oven at temperature 40℃ until the


weight is constant

Percent of residue

Reaction:
7H2C2O4.2H2O(aq) + K2Cr2O7(aq) → 2K[Cr(C2O4)2(H2O)2](s) + 17H2O(l)
+ 6CO2(g)

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3. Isomer Purity Test

Crystal
- Placed on top of filter paper
- Added a little of ammonium solution

The dark green color is The brown color is spread


spread on a filter paper (cis) on a filter paper (trans)

Reactions:
2K[Cr(C2O4)2(H2O)2] + 2NH3 → 2K[Cr(NH3)2(H2O)2]
Cis structure

Trans structure

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G. OBSERVATION RESULT
A. Trans Potassium dioxalate diaquochromium (III) (K[Cr(C2O4)(H2O)2]
making
No. Treatment Observation Reaction
(colour/precipitate/gas)
1. Oxalic acid dihydrate White crystal (3,0020 g) H2C2O4.2H2O(s)
2. Oxalic acid dihydrate White crystal wet H2C2O4.2H2O(s) + H2O(l)
+ distilled water → H2C2O4.2H2O(aq)
3. Potassium dichromate Orange crystal (1,0006 K2Cr2O7(s)
g)
4. Potassium dichromate Orange crystal wet Cr2O72- + 14H+ + 6e- →
+ distilled water 2Cr3+ + 7H2O
5. Oxalic acid Black melt, bubble, 7H2C2O4.2H2O(aq) +
dihydrate(aq) + warm K2Cr2O7(aq) →
potassium 2K[Cr(C2O4)2(H2O)2](s) +
dichromate(aq) 17H2O(l) + 6CO2(g)
6. After the mixture Blackish green 2K[Cr(C2O4)2(H2O)2](s) +
evaporated precipitate, bubbles, ½ heat →
volume solution 2K[Cr(C2O4)2(H2O)2](s) +
H2O(l)
7. After the crystal Residue: blackish green 2K[Cr(C2O4)2(H2O)2](s)
filtered precipitate
Filtrate: blackish green
solution
8. After washed by Black precipitate
distilled water

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9. After washed by Black precipitate
ethanol

10. After dried (at 40⁰C) 1st weight = 1,0563 g %weight = 39%
and constant weight 2nd weight = 0,8136 g
3rd weight = 0,8074 g
11. Purity isomer test: Blue solution K[Cr(C2O4)2(H2O)2](s) +
filtered paper + crystal 6NH4OH(aq) →
+ ammonium 2K[Cr(NH3)2(H2O)2](s) +
H2C2O4(aq) + H2O(l)

B. Cis Potassium dioxalate diaquochromium (III) making


No. Treatment Observation Reaction
(colour/precipitate/gas)
1. Oxalic acid dihydrate White crystal (3,0023 g) H2C2O4.2H2O(s)
powder
2. Potassium dichromate Orange crystal (1,0009 K2Cr2O7(s)
powder g)
3. Oxalic acid dihydrate Heterogenous mixture H2C2O4.2H2O(s) +
powder + potassium K2Cr2O7(s) →
dichromate powder
4. Oxalic acid dihydrate Black metlt, warm, 7H2C2O4.2H2O(aq) +
powder + potassium bubble K2C2O4(aq) →

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dichromate powder + 2K[Cr(C2O4)2(H2O)2](s) +
distilled water drop by 17H2O(l) + 6CO2(g)
drop
5. Mixture solution + Stirring time until form
ethanol + stirred (one way) precipitate = 5
mins
6. After decantated + Black residue, greenish
more ethanol black precipitate

7. The crystal after Residue: black


filtered precipitate
Filtrate: greenish black
solution

8. After dried (40⁰C) and 1st weight = 2,7663 g %weight = 74,12%


constant weight 2nd weight = 1,618 g
3rd weight = 1,527 g
9. Purity isomer test: Dark green solution K[Cr(C2O4)2(H2O)2](s) +
filtered paper + crystal NH4OH(aq) →
+ ammonium 2K[Cr(NH3)2(H2O)2](s) +
H2C2O4(aq) + H2O(l)

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H. ANALYSIS
1. Making of trans isomer of potassium dioxalatodiaquochromate(III)
The first experiment was aimed at making a compound which is a
trans isomer of potassium dioxalatodiaquochromate(III) by reacting oxalic
acid dihydrate (H2C2O4.2H2O) with potassium dichromate (K2Cr2O4). The
first step is to take 3,0002 grams of oxalic acid dihydrate (H2C2O4.2H2O),
in the form of white crystals, into a 50 mL beaker. Then dissolve the oxalic
acid with 5 drops of boiling distilled water, resulting in a wet crystal.
Furthermore, it was added with a solution of 1,0006 grams of potassium
dichromate (K2Cr2O7) in the form of orange crystals, dissolved with 5
drops of hot distilled water which produced a wet crystal. The function of
distilled water is to dissolve and accelerate complex formation reactions.
The addition of water as a little as possible with the aim of water that can
also be a ligand, if added too much can replace oxalate as a ligand, so that
what is formed is not the desired complex. Furthermore, it is covered with
a watch glass, with the aim that the reaction that occurs goes in a closed
system to prevent the release of heat, because the reaction that takes place
is an exothermic reaction. The reactions that occur are:
4H2C2O4.2H2O + K2Cr2O7 → 2K[Cr(C2O4)2(H2O)2] + 6CO2 + 7H2O
After the two solutions are mixed homogeneously, the evaporation is
carried out at the mixture of the solution on a water bath until only half of
the original volume of the solution. Furthermore, it is allowed to evaporate
by itself at room temperature until only a third of the volume of the original
solution is left. The purpose of evaporation is to remove undesirable
distilled water levels, so that it does not affect the expected formation of
complex salts, namely potassium dioxalatodiaquochromate(III) complexes,
because these complex compounds contain only 2H2O molecules and
2C2O42- molecules as ligands and in solution it still contains a lot of H2O,
H2O ligand is likely to increase in number which is more than what is chilled
so as to avoid it is evaporated.
After the volume is one third of the initial volume, the crystals are
filtered and the resulting filtrate is a blackish-green solution and the

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residue is a blackish green crystal. Then the blackish green crystals are
washed with cold distilled water and then with alcohol to produce black
precipitate. The black precipitate from the washing process is a trans-
potassium dioxalatodiaquochromate(III) isomer. The resulting black
precipitate is dried in the oven and weighed 3 times to a constant weight.
The weight obtained was 1.0563 gram, 0.8136 gram and 0.8074 gram
respectively and the average weight was 0.8923 gram. So that the results of
the calculation of the levels of trans-potassium
dioxalatodiaquochromate(III) of 39% (calculations attached). The function
of adding ethanol is to remove semi-polar impurities, heated at temperatures
of 40-50℃ to evaporate the remnants of ethanol.
The following is an illustration of the molecular structure of the trans-
potassium bisoksalatodiakuochromat (III) isomer.

2. Making of cis isomer of potassium dioxalatodiaquochromate(III)


The second experiment was aimed at making a compound which is a
cis isomer of potassium dioxalatodiaquochromate (III) by reacting oxalic
acid dihydrate (H2C2O4.2H2O) with potassium dichromate (K2Cr2O4). The
production of a cis isomer of the potassium dioxalato diachochromate(III)
compound is carried out by reacting 3,0023 grams of oxalic acid dihydrate
(white crystals) with 1,0009 gram of potassium dichromate (orange
crystals) in a beaker glass 50 mL. Then 1 drop of distilled water is added to
speed up the reaction of the two substances and immediately after adding
the distilled water the evaporating cup is covered with a watch glass. Such
a procedure is carried out because the reaction between potassium
dichromate and oxalic acid dihydrate is an exothermic reaction (releasing
heat) so that during the reaction it must be covered with a watch glass to
prevent heat release. Both types of hygroscopic crystals that are given a drop

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of distilled water melt and slowly turn into a black melt solution. Let the
two crystals react but do not become a solution. The color change from
orange and white to brown is due to the formation of potassium
dioxalatodiaquochromate complex compounds, where in the complex
compound are two kinds of ligands and one central atom of transition metal.
The reaction of the formation of the cis isomer of the potassium
dioxalatodiaquochromate compound is shown as follows:
4H2C2O4.2H2O + K2Cr2O4 → 2KCr(C2O4)2(H2O)2 + 6CO2 + 7H2O
From this reaction it can be seen that the complex compound
K[Cr(C2O4)(H2O)2] is formed where in the complex compound there are
two kinds of ligands, namely ligands (C2O4)2- and ligands (H2O), and
accompanied by side products in the form of CO2 and H2O gas.
Then the precipitate is decanted and added with a few drops of
ethanol to produce a filtrate in the form of a black solution and a residue in
the form of a black precipitate. The addition of ethanol is intended to
condense all the precipitate (specificly semi polar precipitate) formed to
form a black solid precipitate. Then the precipitate was filtered and
produced a black precipitate that was thicker than the precipitate on the
trans isomer. The resulting black paste was dried in an oven at 50℃ and
weighed to a constant weight and obtained the weight of the precipitate was
2,7663 gram, 1,6180 gram, and 1,5270 gram, by the average 1,970 gram.
So that the results of the calculation (calculations attached) of the levels of
cis potassium dioxalatodiakuochromat (III) of 74,12%.

3. Isomer Purity Test


In this third experiment, the purity test aims to differentiate between
the trans-potassium dioxalatodiaquochromate(III) isomer and the cis-
potassium dioxalatodiaquochromate(III) isomer. Complex crystals obtained
from the experiment were placed in test tubes. Then the crystal test is carried
out using ammonium solution in the form of a colorless solution.
Ammonium (NH4OH), like oxalate or water, is also a ligand. Addition of
ammonium can substitute for oxalate or water ligands. Trans isomer crystals
added with ammonium solution produce a blue solution. Cis isomer crystals

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added with a few drops of ammonium solution produce a green solution.
The reactions that occur in the purity test are as follows:
2K[Cr(C2O4)2(H2O)2] + 2NH3 → 2K[Cr(NH3)2(H2O)2]
This difference can be explained by the order of influence of the
strength of the trans ligand effect: H2O < OH < NH3 < Cl < Br < I = NO2 =
PR3 << CO = C2H4 = CN.
In trans crystal NH3 can not substitute oxalate ligand because the
strength of NH3 ligand under oxalate ligand is based on the strength of the
trans effect formed. However, the trans effect is overcome H2O, resulting in
a change in H2O ligand which results in a change in the color of the crystal
to blue where the color should be brown.
In cis crystals the effect is reversed. NH3 has a greater cis effect
strength than oxalic acid, so it is able to substitute oxalate ligands from
complex crystals. As a result, the complex dissolves and ligand changes
causing the solution to turn green.

Melting Point Test


The melting point test is also carried out as a proof of the purity of the
formed cis crystals. Melting point test is carried out using melting bock. Cis
crystals are filled into the capillary tubes, then inserted into the melting
block. After that, the melting block and thermometer are arranged in such a
way on three legs. The melting block is heated until the crystals in the
capillary tube all melt, the temperature at which it is formed is observed
from the attached thermometer.
Theoretically, the melting point of cis and trans isomers is more than
300℃. Based on observations of the melting point of cis potassium
dioxalatodiakuochromate crystal is 220℃. In theory, the trans isomer has a
lower melting point than the cis isomer. Polarity is a key factor that
determines the relative boiling point of a compound because it will increase
the intermolecular force, while symmetry is a key factor that determines the
relative melting point because it allows the arrangement of the key factors
that determine the relative melting point because it allows better
arrangement of molecules in the shape solid.

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I. CONCLUSION
From these experiments, it can conclude that:
1. Cis and trans complexes can be made by mixing non-complex components
(complex constituents), namely H2C2O4.2H2O with K2Cr2O4 with the
addition of 3-5 drops of aquadest.
2. From the manufacture of cis and trans from 1 gram of potassium dichromate
and 3 grams of oxalato dihydric acid obtained black crystals with an average
constant weight of 0.8923 grams for the trans-potassium
dioxalatodiaquochromate(III) isomer and 1,970 grams for the cis-potassium
dioxalatodiaquochromate(III). In order to obtain a solution of 39% for the
trans-potassium dioxalatodiaquochromate(III) isomer and 74.12% for the
cis-potassium dioxalatodiaquochromate(III).
3. In trans crystal NH3 can not substitute oxalate ligand because the strength
of NH3 ligand under oxalate ligand, while in cis complex, NH3 has a greater
cis effect strength than oxalic acid, so it is able to substitute oxalate ligands.
Melting point of cis-potassium disoksalatodiaquokromate(III) of 220℃.

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REFERENCES

Anderson, K. M., & Orpen, A. G. (2001). On the relative magnitudes of cis and
trans influences in metal complexes. Chemical Communications, 1(24), 2682–
2683. https://doi.org/10.1039/b108517b
Coley, C. W., Rogers, L., Green, W. H., & Jensen, K. F. (2017). Computer-Assisted
Retrosynthesis Based on Molecular Similarity. ACS Central Science, 3(12),
1237–1245. https://doi.org/10.1021/acscentsci.7b00355
Crabtree, R. H. (2001). The organometallic chemistry of the transition metals. John
Wiley.
Craig, N. C., Chen, A., Ki Hwan Suh, Klee, S., Mellau, G. C., Winnewisser, B. P.,
& Winnewisser, M. (1997). Contribution to the study of the Gauche effect.
The complete structure of the anti rotamer of 1,2-difluoroethane. Journal of
the American Chemical Society, 119(20), 4789–4790.
https://doi.org/10.1021/ja963819e
Hill, A. F., & Fink, M. J. (2011). Advances in organometallic chemistry. Vol. 59.
Academic.
March, J. (1985). Advanced organic chemistry : reactions, mechanisms, and
structure. Wiley.
Miessler, G. L., & Tarr, D. A. (Donald A. (2004). Inorganic chemistry. Pearson
Education.
Reusch, W. (2010). Stereoisomers Part I. Virtual Textbook of Organic Chemistry.
Retrieved from
http://www2.chemistry.msu.edu/faculty/reusch/VirtTxtJml/sterisom.htm#star
Wiberg, E., Wiberg, N., & Holleman, A. F. (Arnold F. (2001). Inorganic chemistry.
Academic Press.

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ATTACHMENTS

A. Calculations
Trans isomer of potassium dioxalatodiaquo chromate (III)
Mass of H2C2O4 = 3,0029 gram
Mass of K2Cr2O7 = 1,0006 gram
Mr H2C2O4.2H2O = 126 g/mol
Mr K2Cr2O7 = 294 g/mol
Mass of K[Cr(C2O4)2(H2O)2] = 0,8074 gram

3,0029 𝑔
Mole of H2C2O4 = 126 𝑔/𝑚𝑜𝑙 = 0,0238 mol
1,0006 𝑔
Mole of K2Cr2O7 = 294 𝑔/𝑚𝑜𝑙 = 0,0034 mol

Reaction
4H2SO4.2H2O(aq) + K2Cr2O7(aq) → 2K[Cr(C2O4)2(H2O)2](s)
I: 0,0238 mol 0,0034 mol
R: 0,0136 mol 0,0034 mol 0,0068 mol
E: 0,0102 mol 0 mol 0,0068 mol

Mass of 2K[Cr(C2O4)2(H2O)2] = mol × Mr


= 0,0068 mol × 303,154 g/mol
= 2,06 gram
0,8074 𝑔
%mass trans K[Cr(C2O4)2(H2O)2] = × 100%
2,06 𝑔

= 39,19%

Cis isomer of potassium dioxalatodiaquo chromate (III)


Mass of H2C2O4.2H2O = 3,0023 gram
Mass of K2Cr2O7 = 1,0009 gram
Mass of K[Cr(C2O4)2(H2O)2] = 1,527 gram
3,0023 𝑔
Mole of H2C2O4.2H2O = 126 𝑔/𝑚𝑜𝑙 = 0,0238 mol
1,0009 𝑔
Mole of K2Cr2O7 = 294 𝑔/𝑚𝑜𝑙 = 0,0034 mol

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Reaction
4H2SO4.2H2O(aq) + K2Cr2O7(aq) → 2K[Cr(C2O4)2(H2O)2](s)
I: 0,0238 mol 0,0034 mol
R: 0,0136 mol 0,0034 mol 0,0068 mol
E: 0,0102 mol 0 mol 0,0068 mol

Mass of 2K[Cr(C2O4)2(H2O)2] = mol × Mr


= 0,0068 mol × 303,154 g/mol
= 2,06 gram
1,527 𝑔
%mass trans K[Cr(C2O4)2(H2O)2] = × 100%
2,06 𝑔

= 74,12%

B. Documentations
trans-potassium dioxatalatodiaquochromate (III) making

3,0029 gram white 1,0006 gram orange K2Cr2O7 added 5 drops


crystal H2C2O4.2H2O crystal K2Cr2O7 hot distilled water

H2C2O4.2H2O added 5 Mixed K2Cr2O7 + Evaporated using water


drops boiled distilled H2C2O4.2H2O = black boiling = blackish green
water melt, bubble and warm precipitate, bubble

20 | (C i s a n d T r a n s )
Washed using distilled Black precipitate trans Purity test : Blue
water and ethanol = potassium bis oxalate solution
black precipitate diaquochromium (III)

cis-potassium dioxatalatodiaquochromate (III) making

3,0023 gram white 1,0009 gram orange K2Cr2O7 added


crystal H2C2O4.2H2O crystal K2Cr2O7 H2C2O4.2H2O and mixed
until homogen

Mixed K2Cr2O7 + Decantaned + ethanol : Filtered = residu black


H2C2O4.2H2O + a drops black redisu and precipitate, filtrate
distilled water = black blackish green solution greenish black solution
melt, bubble and warm

21 | (C i s a n d T r a n s )
Black precipitate cis Purity test : Drak green Melting point test
potassium bis oxalate solution
diaquochromium (III)

C. Question Answers
1) In which part of the oxalate ion acts as bidentate in complex formation
reactions?
Answer:
In oxalate ions which act as bidentates in complex formation reactions in O
atoms originating from ligands (C2O4)2

2) Write down the reactions that occur in the cis and trans complex formation
process!
Answer:
(1) Production of Trans Isomer of potassium
biooxalatodiaquochromate(III)
H2C2O4.2H2O(s) + H2O(l) → H2C2O4.2H2O(aq)
K2Cr2O7(s) + H2O(l) → K2Cr2O7(aq)
7H2C2O4.2H2O(aq) + K2Cr2O7(aq) → 2K[Cr(Cr2O4)2(H2O)2)](s) +
17H2O(l) + 6CO2(g)
(2) Making as isomer of potassium biooxalatodiaquochromate(III)
7H2C2O4.2H2O(aq) + K2Cr2O7(aq) → 2K[Cr(C2O4)2(H2O)2](s) +
17H2O(l) + 6CO2(g)
(3) Isomer Purity Test
2K[Cr(C2O4)2(H2O)2] + 2NH3 → 2K[Cr(NH3)2(H2O)2]
Cis structure

22 | (C i s a n d T r a n s )
Trans structure

3) Write down the reaction that occurred in the cis and trans purity test
process!
Answer:
2K2[Cr(C2O4)2(H2O)2] + 2NH3 → 2K[Cr(NH3)2(H2O)2]

23 | (C i s a n d T r a n s )

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