I have provided the information for the lab below. I want to see the chemical reactions that take place during each step of the experiment. So in the procedures when a chemical was added i would like to see what the products and byproducts that were formed. I also want to see one over all reaction for this experiment to just get an overview of what exactly is happening during the experiment. Thank you:)
Part B: Synthesis of [Co(NH3)5Cl]Cl2
Objective:
To prepare and isolate a Co(III)-based coordination compound
starting from the product of
Experiment 4a. The solid is also to be used in additional
experiments involving conductivity, UVVis,
and infrared spectroscopy.
Pre-Lab Study:
You should include equations (3), (4), and (5) of the introduction
in your Pre-lab for Exp.
4b. Also, remember to save some of you intermediate product for
conductivity, UV-vis and
IR studies to be performed in Exp. 4c & 4d.
Background:
Of particular importance to the development of coordination
chemistry are metal
complexes of the type to be synthesized and characterized in this
experiment. Prior to 1950,
research in this area was almost exclusively concerned with the
investigation of complexes of
transition metal ions with such monodentate ligands as Cl-, Br-,
I-, NH3, pyridine, CN-, and NO2
-
and bidentate ligands as ethylenediamine (H2NCH2CH2NH2), oxalate
(-O2CCO2
-), glycinate
(H2NCH2CO2
-), and CO3
2-. These complexes form the basis of a vast amount of research
today,
despite the more recent discoveries of the ligand properties of H,
CH3, CO, H2C=CH2, and
benzene, to mention a few.
Coordination compounds of Co(III) and Cr(III) have been of
particular interest because
their complexes undergo ligand exchange very slowly compared with
complexes of many other
transition metal ions. For example, Ni(NH3)6
2+ reacts instantaneously with H2O to form
Ni(OH2)6
2+. Under the same conditions, the analogous reactions of
Co(NH3)6
3+ and Cr(NH3)6
3+
occur very slowly. This difference in behavior of complexes of
different metal ions has been
qualitatively accounted for by ligand field theory and molecular
orbital theory.
The slow reactivity of Co(III) complexes has made them suitable for
extensive
investigations. The structures of the octahedral Co(III) complexes
that you will prepare are given
below.
NH3
Co
NH3
O
O
H3N
NH3
O
n
NO3
NH3
Co
NH3
Cl
NH3
H3N
NH3
n
Cl2
One important method of characterizing ionic substances is the
determination of the ability of their solutions to conduct an
electric current. Those substances whose solutions have the highest
conductivity consist of the greatest number of ions. Thus, a one
molar solution of [Co(NH3)4CO3]NO3 will have a lower conductance
than a solution of [Co(NH3)5Cl]Cl2 of the same concentration. By
measuring the conductivity of a solution of a compound, it is
possible to determine whether a formula unit of that compound
consists of 2, 3, 4 or more ions. Although measurements will be
done on water solutions of the complexes, the same information can
be frequently obtained using organic solvents such as nitrobenzene
or acetonitrile for ionic compounds that are either not very
soluble in water or react with water.
Another very powerful method for establishing the identity of a
complex is infrared spectroscopy. This technique examines the
frequencies of the vibrational modes of a molecule. Thus, the
infrared spectra of both of the preceding complexes exhibit
absorptions at frequencies (commonly expressed in wave numbers,
cm-1, i.e. reciprocal wavelength 1/) characteristic of stretching
and bending modes of the NH3 group. While the Co-N stretching modes
are in principle also measurable, they sometimes occur at
frequencies too low (below 600 cm-1) to be observed in most
infrared spectrophotometers. More specialized and expensive
infrared instruments are, however, available for studying these
vibrations. The complex [Co(NH3)4CO3]NO3 also exhibits absorptions
characteristic of the carbonate group. Because of its coordination
to the metal ion, the CO32- group has a somewhat different spectrum
in this complex than it has as the ion, as in Na2CO3. The spectrum
should also contain absorptions bands resulting from vibrational
modes of the NO3- ion, very similar to those observed in NaNO3. In
contrast the spectrum of [Co(NH3)5Cl]Cl2 would be largely dominated
by absorptions attributable to the NH3 groups.
In general, metal-Cl stretching frequencies are lower than can be
observed on usual infrared instruments, and the ionic Cl- groups,
of course, are not, in the solid state, strongly bonded to any
other single atoms; thus, no absorptions are expected in the
infrared spectrum to indicate their presence in the compound. While
infrared spectroscopy and other instrumental methods of compound
characterization are emphasized in this and in other experiments in
this book, it should be stressed that a quantitative elemental
analysis is an absolutely essential step in determining the
composition and structure of a new compound.
The synthesis of [Co(NH3)4CO3]NO3 will be carried out according to
the unbalanced equation,
Co(NO3)2 + NH3 (aq) + (NH4)2CO3 + H2O2
[Co(NH3)4CO3]NO3 + NH4NO3 + H2O (1)
The Co(NO3)2 that is available commercially has the formula
Co(NO3)2 • 6 H2O and very probably is a coordination compound
having the ionic formulation [Co(OH2)6](NO3)2. Since Co(II)
complexes, like those of Ni(II), react very rapidly by ligand
exchange, the first step in the reaction might be expected to
be,
Co(OH2)62+ + 4 NH3 + CO32- Co(NH3)4CO3 + 6 H2O (2)
This Co(II) complex could then be oxidized by the transfer of an
electron to H2O2 to give the relatively non-reactive Co(III) ion,
[Co(NH3)4CO3]+. The preparation of [Co(NH3)5Cl]2+ is accomplished
from the carbonato complex according to the following series of
equations:
[Co(NH3)4CO3]+ + 2 HCl [Co(NH3)4(OH2)Cl]2+ + CO2 (g) + Cl-
(3)
[Co(NH3)4(OH2)Cl]2+ + NH3 (aq) [Co(NH3)5(OH2)]3+ + Cl- (4)
[Co(NH3)5(OH2)]3+ + 3HCl [Co(NH3)5Cl]Cl2 (s) + H2O + 3H+
(5)
On the basis of mechanistic studies of reactions of [Co(NH3)4CO3]+
with acids, the first
reaction in the preceding sequence probably involves the following
mechanism:
Co
O
O
(NH O 3)4
n
Co
Cl
O
O O
(NH3)4
Cl H
+
Co
Cl
OH2
(NH3)4
n
CO2
2
+
2+
+
Chemicals Used:
Product from Exp. 3a – [Co(NH3)4CO3]NO3
Concentrated Hydrochloric acid – HCl
Ammonium Hydroxide – NH4OH
Procedure:
You are encouraged to make observations of color changes and
precipitate formations
during the course of each part of this experiment.
Chloropentaamminecobalt(III) Chloride, [Co(NH3)5Cl]Cl2: dissolve
3.0 g of
[Co(NH3)4CO3]NO3 in 30 mL of H2O and add 3 to 6 mL of concentrated
HCl until all of the CO2
is expelled. The 3-6 mL of the concentrated, 12 Molar HCl(aq) can
be added slowly until no
further gas is evolved and all of the intermediate has gone into
the solution. Record the amount of
acid utilized. Neutralize with concentrated aqueous NH3 and then
add about 3 mL excess. It is
important that any excess acid has been neutralized and then that
the required excess of the 15
Molar, ammonia has been added. If you cannot be sure whether the
solution has been neutralized
by directly testing of the liquid with full-range litmus paper,
hold a moistened litmus above the
solution in the beaker. Once the first sign that the gas over the
solution is basic, you can assume
neutralization has been achieved. Then heat the solution to between
80-90 C on a hot plate for 15
minutes until the [Co(NH3)5H2O]3+ complex has formed. Avoid
boiling. Note the solution color.
Sometimes a slight precipitate of the hydroxo-complex is observed
at this point. Cool the solution
to below 40 C in an ice bath and then add the 50 mL of conc. HCl.
Note the color of the precipitate
that should form at this point. Reheat the solution to between
75-85°C for 15-20 minutes and
observe the color changes. Wash the compound with small amount (1-2
mL) of ice-cold distilled
water; then filter under a water aspirator vacuum with a glass
fritted funnel. The final solid present
should be purple in color. Calculate the percent yield. (Do not
discard the compound because
part of it will be needed in Experiment 4c & 4d).
Waste:
Cobalt filtrate from the synthesis should be deposited in the
appropriately labeled waste container.
This is the overall reaction of the si thesis .
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