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INTRODUCTION

In this multi-week experiment, you will synthesize a compound and then analyze
it to determine its empirical formula. The substance you will prepare is a vividly
colored coordination compound of copper. Based on the reagents used in the
synthesis procedure, you can assume that the final compound contains copper,
ammonia, sulfate, and water. In your analysis, you goal is to figure outthe mole
ratio of each component in the final compound. In other words, you will solve for
x, y, z and a in the formula Cu x (NH3) y (SO4) z. a H2O
Based on the way the formula is written you can assume that ammonia and
sulfate are acting as ligands and counter-ions, respectively. The water, in
contrast, is water of hydration. That is, it is incorporated into the crystal lattice of
the solid compound in a non covalent manner, usually by hydrogen bonds, and
with a specific stoichiometry.
Synthesis
To prepare your own sample of the coordination compound, youll start with solid
copper(II) sulfate pentahydrate, CuSO4.5H2O. Once dissolved in water, the
copper ions take on water molecules as neutral ligands :copper(II) ions exist as
the hexaquacopper(ii) complex ion in aqueous solution. After adding
concentrated ammonia, NH3 ligands displace the water molecules covalently
bound in the original copper complex, and a dramatic color change occurs. The
copper(II) ammonia complex is a water-soluble ioN, in order to precipitate and
isolate the final product, an ionic compound, you need to decrease the solubility
of the compound. A convenient way of doing this is to add a large amount of
ethanol, CH3CH2OH, to the aqueous solution. EThanol is miscible with water but
is much less polar, and, as the amount of ethanol in the mixture increases, the
solubility of ionic compounds decreases. After the addition of ethanol, your
coordination compound will appear as a crystalline solid, and the synthesis
procedure ends with filtration, rinsing, and drying of the visually stunning
product. The next several parts of the lab involve analysis of your copper(II)
coordination compound to determine its empirical formula.

Why can we crystallize tetraamminecopper (II) sulfate from water when we add
ethanol?

The easiest way to view this is that ethanol dissolves in water and because of the
lower solubility of the complex in the new solvent, an ethanol-water mixture, the
complex then crystallizes. It is indirectly due to polarity, but directly due to
solubility.

Tetraamminecopper(II) sulfate is the inorganic compound with the formula


[Cu(NH3)4(H2O)n]SO4. This dark blue solid is a metal complex. This compound
can be prepared by adding concentrated solution of ammonia to a saturated
aqueous solution of copper sulfate followed by precipitation of the product with
ethanol. The deep blue crystalline solid tends to hydrolyse and evolve (release)
ammonia upon standing in air.[1] The correct concentrations of ammonia and
copper sulfate solution can be determined by colorimetry. The combination of the
correct concentrations will

produce the highest absorbance read out on the colorimeter and as a result the
formula of the complex can be verified.

This compound can be prepared by treating concentrated ammonia solution,


NH3, to a saturated aqueous solution of copper sulfate [Cu(H2O)6]SO4 until all
the copper(II) hydroxide that is initially formed redissolves into a deep blue
solution. The deep blue crystalline solid tends to hydrolyse and lose ammonia
ligands upon standing in air. In the solid state, the salt consists of the
[Cu(NH3)4H2O]2+ cation, which has a square pyramidal molecular geometry.
The Cu-N and Cu-O distances are about 210 and 233 pm.

What is tetraamminecopper (II) sulfate monohydrate [Cu(NH3)4]SO4H2O?


The name tetraamminecopper(II) indicates that four ammonia molecules
(called
ammine in coordination compound ligo) molecules are covalently bonded to the
copper(II) ion. The formula is written [Cu(NH3)4]2+. The square brackets signify
that the four ammonia molecules and the Cu2+ ion act as a group, with a +2
charge. This ion will combine with sulfate (SO4 2- ) to make a neutral ionic
compound [Cu(NH3)4]SO4. This group will form part of the solid crystal
[Cu(NH3)4]SO4H2O, in which there is one molecule of water forming a hydrated
In part A of the lab, we will synthesis the coordination compound
tetraamminecopper (II) sulfate
monohydrate [Cu(NH3)4]SO4H2O. This will be accomplished by adding
concentrated ammonia
(NH3) to copper (II) sulfate pentahydrate which will displace the water molecules
bound in the
original copper complex, and a dramatic color change occurs.

The reaction of ammonia with the copper(II) sulfate pentahydrate is a two-step


process. In the
first step, solid copper (II) hydroxide is formed which is light blue in color. The
Cu(OH)2(s)
dissolves as additional quantities of ammonia are added in the second step to
form the dark blue
[Cu(NH3)4]2+
complex. The equations for the process are below
Reaction 1:
[Cu(H2O)4]SO4H2O (aq) + 2NH3 (aq) Cu (H2O)2(OH)2]SO4 H2O (s) +2
NH4
+
(aq)
Reaction 2:
Cu (H2O)2(OH)2]SO4 H2O (s) + 2 NH4
+
(aq) + 2 NH3 (aq) [Cu(NH3)4] SO4H2O (aq) + 4 H2O (l)
The overall net equation for the reaction is
Cu(H2O)4]SO4H2O (aq) + 4 NH3 (aq) [Cu(NH3)4]SO4H2O + +4 H2O (l)
The copper(II) ammonia complex is water-soluble. In order to precipitate and
isolate the final
product, you need to decrease the solubility of the ionic compound. A convenient
way of doing
this is to add a large amount of ethanol, CH3CH2OH, to the aqueous solution.
Ethanol is much
less polar than water, and as the amount of ethanol in the mixture increases, the
solubility of ionic
compounds decreases. After the addition of ethanol, your coordination compound
will appear as
a crystalline solid. The synthesis procedure ends with filtration, rinsing, and
drying of the product.