Mindanao University of Science and Technology

C.M. Recto Ave., Lapasan

Cagayan de Oro City, Philippines
Inorganic Chemistry
Department of Chemistry
College of Arts and Sciences

Preparation and Analysis of a Coordination Compound:

Synthesis of [Co(NH3)5Cl]Cl2
Experiment No. 10

Submitted by:
Group 1
Basa, Marla C.
Baytion, Ana Margarita L.
Tomas, Izza May L.

Date performed:
September 24, 2015
Submitted to:
Sir Glenn D. Ongayo

INTRODUCTION
Coordination compounds are compounds that contain a metal atom or ion bonded to a
froup of molecules ionic compounds consisting of a complex ion (a metal ion with its attached
molecules or ions) and a counter ion or ions to balance the charge. The molecules or ions
attached to the central metal atom are called ligands. A ligand is an ion or molecule that binds to
a central metal atom to form a coordination complex. The electron pairs used to form the bonds
are donated by the ligands, which makes the ligands Lewis bases and the metal ion a Lewis acid.
Cobalt(III) forms some of the most stable and easilyprepared coordination compounds.
The ligand exchange for Co(II) is rapid. The 3+ state is inert with respect to ligand substitution.
Therefore, complexes of Co(III) are easy to handle and can be dissolved in water without a rapid
change in composition. A solution of Co(II) is prepared with a high concentration of the ions or
molecules that we wish to introduce as ligands. The Co(II) is then oxidized with hydrogen
peroxide, to convert the Co(II) to Co(III). This usually results in a compound with five of the six
ligands .
In this experiment we will prepare chloropentaaminecobalt(III) chloride,
[Co(NH3)5Cl]Cl2. The Co(III) in this compound has a coordination number of six: five NH 3
molecules and one Cl- ion, in an octahedral geometry around that Co(III) central metal, to give
an ion with a 2+ charge. The compound has two Cl - anions to balance that charge. The
compound is prepared by dissolving CoCl2 6H2O in water and adding concentrated ammonia
solution.
Co(H2O)62+ + 6 NH3 Co(NH3) 5OH+ + NH4+ + 5H2O

(1)

The Co(II) is then oxidized with hydrogen peroxide.

Co(NH3) 5OH+ + 1/2 H2O2 Co(NH3) 5 OH2+ + OH-

(2)

The solution is acidified and heated to complete the conversion to the desired product.
Co(NH3) 5 OH2+ + H+ Co( NH3) 5 OH23+

(3)

Co( NH3) 5 OH23+ + Cl- Co(NH3) 5 Cl2+ + H2O

(4)

Co(NH3) 5 Cl2+ + 2 Cl- [Co(NH3) 5Cl]Cl2 (solid)

(5)

OBJECTIVES
The objectives of this experiment was to prepare a coordination compound[Co(NH 3 ) 5 Cl]
Cl 2 by dissolving CoCl 2 6H20 in water and adding concentrated ammonia solution- ammonia
mixture, and isolated and synthesized a 6 coordinate Cobalt (III) compound.
MATERIALS
The materials used in this experiment were: 250-mL beakers, 10-mL and 25-mL graduated
cylinder, filter paper, funnel, thermometer, iron stand, stirring rod, hot plate, 400-mL beaker,
wash bottle, 125-mL Erlenmeyer flask and ice.
CHEMICALS
The chemicals used were: CoCl2 6H2O, NH4Cl (solid), concentrated ammonia, 20% H2O2,
concentrated HCl and methanol.
PROCEDURE
A. Synthesis of [Co(NH3)5Cl]Cl2
We weighed approximately 4.0 g of powdered cobalt chloride 6-hydrate in a 125mL
Erlenmeyer flask. While in the hood, we dissolved 2.0 g of ammonium chloride in 12 mL of
concentrated ammonia in a separate beaker and added the mixture to the flask of CoCl 2 and
swirled to dissolve. Some brown and/or purple solid remained in the suspension. We added 4
mL of 30% hydrogen peroxide solution, in 1 mL increments. Swirl the flask between each
addition to stir the mixture and allow the effervescence to cease. When all the hydrogen
peroxide has been added, we allowed 5 minutes for the reaction to be completed. Then slowly,
with swirling, we added 12 mL concentrated hydrochloric acid. We heated the mixture (in the
hood) at 85C for 20 minutes, using a 400 mL beaker on a hotplate as a heating bath. We did not
allow the temperature to rise above 90C. After heating, we cool the mixture to near room
temperature. Once a considerable amount of solid had formed, we speeded the cooling by an ice
bath.
B. Isolation of the compound.
We assembled the filter flask; trap and filter funnel as directed and poured the solution
through the funnel until only a small amount remains. Then swirled the flask to bring the solid
into suspension and quickly poured all of the contents of the flask into the funnel and allowed the

vacuum to draw the solution away from the precipitate. We use 10 mL of ice-cold de-ionized
water to transfer any solid remaining in the flask into the funnel.
Note: The washing technique to use is 1) add just enough ice-cold water to the funnel to cover
the precipitate, 2) allow to set a few seconds to wet all of the solid thoroughly, and then 3) draw
the wash solution through into the filter flask. Washing once with ice-cold water is sufficient.
We turned off the vacuum, and added 20 mL of ice cold methanol to the product on the
filter paper and let this set for a few seconds, and applied the vacuum again. When the methanol
has been drawn through the solid product, we turned the vacuum off, and rinsed again with a 20
mL portion of methanol. After this second rinsing with methanol, we left the vacuum on, and
drew air through the solid until it is dry. We placed the solid product in a petri dish and stored it
on a dessicator.
DATA AND DISCUSSIONS
Powdered cobalt chloride hexahydrate, g
Filter paper, g
Filter paper + product, g

4.0467
1.9626
3.5800

Product [(FP + product) (FP)], g = [3.5800 1.9626]

= 1.6174

Theoretical Yield:
1 mol CoCl2 6 H 2O
= 4.0467 g CoCl2 H2O ( 238 g CoCl 2 6 H 2 O

250 g complex
1 mol complex

2 mol complex compound

)(
)(
2 mol CoCl 2 6 H 2 O

= 4.2507 g [Co(NH3)5Cl]Cl2

Percent (%) Yield:

Actual Yield
= Theoretical Yield

* 100 =

1.6174 g
* 100 %
=
4.25 07 g 38.05

Overall equation:

2 CoCl2 6H2O (s) + 2NH4Cl(s) + 8NH3 (aq) + H2O2

2 [Co (NH3)5Cl] Cl2 (s) + H2O (l)

OBSERVATIONS
Heat was generated after addition of concentrated HCl.
Dissolving NH4Cl with conc. NH3 produced a cold (endothermic) reaction.
After storing the product to the dessicator, the filter paper turned blue.

DOCUMENTATIONS:

REVIEW OF RELATED LITERATURE

This experiment serves as an introduction to the area of synthetic chemistry
specifically, inorganic synthesis. The bonds in coordination compounds are two-electron bonds
(like covalent bonds), but both electrons come from the ligand (a Lewis base with an unpaired

electron pair). The metal ion serves as a Lewis acid (an electron-deficient species which can use
its empty orbital for the bond).

CONCLUSION
We conclude that we synthesized a coordination compound; [Co(NH 3)5Cl]Cl2. We also
learned the different techniques in synthesizing. The possible sources of error in this experiment
were: the inability to completely transfer all of the reagents from the weight boats in to
containers. Some of the synthesis precipitate may also have been lost in decanting leaving room
for even more error.

REFERENCES:
Retrieved from:
1.) http://www.macalester.edu/~kuwata/Classes/2004-05/chem%20111/111l%20experiment
%206%20-%20co%20synthesis.pdf
2.) http://www.rexresearch.com/cohex/cocomplex.pdf
3.) http://web.iyte.edu.tr/chemistry/chemlab/inorganic/spring/manual.pdf