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 nexr t 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 twostep 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.