Inorganic chemistry DTU Laboratory Reports

Inorganic chemistry DTU Laboratory Reports

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Inorganic chemistry DTU Laboratory Reports

Khalid Mustapha
Attempt: Final 2
4 Lab reports (30% each) and 1 lab notes (10%) =100%
Using scientific writing style for a masters/phd audience.
1. Introduction (25%) Introduce the experiment and objectives. Must show
evidence of wider reading. Discuss the scientific objectives of this
experiment.
2. Summary of results with structures, balanced equations & yields.
3. Answer a series of discussion questions. All of the equations, structures
& yields requested & answer all questions must be fully completed.
4. Conclusions. Summarise your findings and their wider relevance
5. References. These must include textbooks and/or journals, and must be
in Dalton Transactions format not Harvard.
6. Notes.You will submit laboratory notes and spectra if possible, included.
The 4th submission requires only laboratory notes.
Requirements:
(1) High quality records of laboratory experiments and observations
needed. Good enough for experiments to be repeated by other
chemists.
(2) Isolate & clearly label compounds.
(3) Get good quality analytical data.
(4) Write a concise, properly referenced introduction to an area of
chemistry;
(5) Deduce chemical structures & balanced equations & calculate
yields
(6) Summarise & assign IR spectral data
(7) Write a concise conclusion.
The Experiments:
Lab Report 1 Calculate the number of unpaired electrons in a metal
complex from the magnetic susceptibility; Understand the effect of
temperature on paramagnetism; Understand how ligand sterics affect metal
coordination geometries and properties.
Lab Report 2: Identify chemical environments & assign a simple NMR
spectrum. What is the relationship between CO ligand stretching frequenc
ies and the electron density of the metal centre; what is the relationship
between symmetry & the number of IR stretching modes.
Lab Report 3: To understand the consequences of partial abundance in
NMR spectra, to understand J couplings in metal complexes and use them
to determine a metal coordination geometry.
Lab Report 4 : To be able to: Assign electronic transitions and calculate Δ
from UV-vis spectral data; Understand the spectrochemical series;
Distinguish charge transfer and d-d transitions, Understand UV-vis
selection rules; Understand the reactivity of transition metal complexes.
Lab notes will be marked based on a scan or a photograph appended to
your report.
Laboratory notes: Laboratory notes must be legible, well laid out and
be a perfect record of everything the student did & observed.
Samples and spectra: All the expected samples were present and of an
exemplary standard. Evidence, melting points, spectroscopic data
confirmed the identity and purity of the sample.
Introduction at least 1/2 page roughly: This section should present, in
your own words and style, the background required by the reader to
understand the purpose of the experiment and the methods used for
treating the data. The key point is to place the experiment in its
fundamental academic context and state the aims – what is it intended to
demonstrate, and how. For full marks content, over and above that
contained in this manual, is required showing evidence of background
reading – however the proportion awarded for this is small, and it should
not come at the cost of a correct and clear basic description. Both here and
in the results and discussion please ensure that any literature sources are
cited and that the work is paraphrased and the text is your own. All
chemistry line drawings should be drawn by you with an appropriate
package, not cut and paste from the web.
Marks are separated into three components, each worth a total of two
marks:
Structure and Clarity:Concise, well-structured, written in an appropriate
style (e.g. no use of first person) and free of grammatical, spelling, or
formatting errors.
Understanding: Exceptionally clear grasp of the experiment and its
objectives, free of scientific errors or ambiguities.
Context: Experiment was very well placed in the context of the subject,
with clear evidence of reading beyond the laboratory manual.
Results Summary
Write a short summary of what you did in the real experiment,correct
structures, and correctly calculated yields (stating the amount of starting
materials and product, showing your working). Please calculate yields to 2
sig figs: e.g. 1.5%, or 25%, NOT 1.22% or 86.9%.
2/2 Equations, structures and yields all present, correct and clearly
presented 1.5/2 Minor mistakes, small elements missing or slightly
ambiguous.

Discussion Questions: Inorganic chemistry DTU Laboratory Reports

Several questions will be posed for each experiment, which are relevant to
the lecture material on the course. These breakdown the elements that
would be present in the more freeform discussion of a report or paper. In
many cases, this means your answer will take the form of some sentence(s)
or a short paragraph and may need to reference structures, etc, drawn
elsewhere in the report. It is appreciated & helpful to markers if you
format this section as answers to questions, rather than as a freeform
report. For example:
Q: Assign and explain the 1H-NMR spectrum of cycloheptatrienyl
molybdenum tricarbonyl tetrafluoroborate?
A: The 1H NMR spectrum of cycloheptatrienyl molybdenum tricarbonyl
tetrafluoroborate shows only a single resonance at δ = 6.5 ppm. This
implies that all seven protons are equivalent, and suggests a conjugated
ring system in a high symmetry molecule. This i s consistent with the
“piano stool” structure shown above…
Q: What does the IR spectrum of cycloheptatrienyl molybdenum
tricarbonyl tetrafluoroborate tell you about the bonding in this compound,
compared to the parent molecule cycloheptatriene molybdenum
tricarbonyl?
A: The IR frequencies associated with the carbonyl groups in
cycloheptatrienyl molybdenum tricarbonyl tetrafluoroborate, at 2060 and
1990 cm-1, are at higher frequency than those for the parent molecule,
cycloheptatriene molybdenum tricarbonyl. This implies a stronger carbonoxygen bond and thus a weaker Mo-C bond as expected for a positively
charged metal centre…..”.
Your markers will provide a mark out of 8 that reflects your overall
performance, as they would for a more freestyle discussion: i.e.
8/8 The questions were fully and correctly answered.
6/8 The questions were largely well answered, with some mistakes or
omissions 4/8 Some correct answers were provided, but with many
mistakes or omissions 2/8 Very few answers were correct
0/8 No answers, or completely incorrect answers
Weightings for each question are provided as a guide only.
Conclusion (1/2 page maximum)
Summarise the main outcomes of the experiment and stress the wider
significance of the chemistry explored. A good conclusion will be linked to
the introduction and should avoid raising completely new discussion
points.
1/1 Well-structured, appropriate in length, summarises the main points of
the experiment, and points out its greater significance in chemistry.
References (1/2 page maximum)
Sources must be cited at the point of use and references given at the end of
the report in the formatof DaltonTransactions.
TheDaltonTransactionsformat is as follows:
For journal references:
1. M. Mayr, M. R. Buchmeiser and K. Wurst, Adv. Synth.Catal., 2002, 344,
712.
e.g. NO title, initials THEN surnames of authors in a list with “and” before
the last author, abbreviated journal title in italics, then year, volume in
bold (if the journal has volume numbers), and page numbers.

For book references:

1. N-Heterocyclic Carbenes in Transition Metal Catalysis and
Organocatalysis, ed. C. S. J. Cazin, Springer-Verlag, Heidelberg, 2011
e.g. title in italics, then editor or author, publisher, town of publication and
year. If you want to, you can add a chapter or page number between the
title and the author/editor. All of the information on publisher etc will be
inside the front cover of the book.
References will be marked as follows:
Sufficient, suitable references were presented in the correct format (Dalton
Transactions).
Suitable references include textbooks, journals from recognized academic
publishers (e.g. Royal Society of Chemistry, American Chemical Society,
Wiley, Elsevier, Taylor and Francis), and reputable internet-only resources
(e.g. chemical societies, well known universities). However, you should
avoid exclusively referencing internet resources, & make sure you include
textbooks and/or journals.

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