Structural Chemistry

Overview

Staff:
Dr. Nockemann Contribution: 7 lectures, 2 seminars and 2 workshops in crystal chemistry, X-ray diffraction and crystallography

Dr. Lagunas Contribution: 7 lectures, 2 seminars and 2 workshops in symmetry, vibrational spectroscopy and mass spectrometry.

Dr. James Contribution: 7 lectures, 2 seminars and 2 workshops in NMR spectroscopy: Basic concepts and application to inorganic chemistry

Dr. Stevenson Contribution: 7 lectures, 2 seminars and 2 workshops in NMR spectroscopy: Application to organic chemistry

Summary of Lecture Content if applicable:

1. SYMMETRY, VIBRATIONAL SPECTROSCOPY AND MASS SPECTROMETRY
Lecturer: Dr. Cristina Lagunas E-mail address: c.lagunas@qub.ac.uk
7 Lectures, 2 seminars and 2 workshops.

Detailed synopsis:

Basic concepts of symmetry
Molecular shape. Symmetry operations and elements. Stereochemistry.
Introduction to spectroscopic techniques

Vibrational spectroscopy
Basic concepts. Interpretation of spectra. Characteristic organic groups frequencies. Characteristic frequencies of common ligands in metal complexes.

Mass Spectrometry
Introduction to mass spectrometry. Instrumentation and ionisation techniques. Base peaks, fragmentations, molecular ion and molecular formula determination.

Recommended text books:
Shriver & Atkins, Inorganic Chemistry, 4th Ed., Chapters 6 and 7, Oxford University Press.
Duckett and Gilbert, Foundations of Spectroscopy, Oxford Chemistry Primer, O.U.P., 2000.
Brisdon, Inorganic Spectroscopic Methods, Oxford Chemistry Primer 62, O.U.P., 1998.

2. NMR SPECTROSCOPY: BASIC CONCEPTS AND APPLICATION TO INORGANIC CHEMISTRY
Lecturer: Dr. S. James E-mail address: s.james@qub.ac.uk
7 Lectures, 2 seminars and 2 workshops.

Detailed synopsis:

Revision of Magnetism
Spin, the Electromagnetic Spectrum and Boltzmann Distribution.
Chemical Shift and factors that affect it; Shielding Constant.
Continuous Wave and Fourier Transform NMR Spectroscopy.
Relaxation. Coupling. Satellites.
Examples of NMR Spectroscopy applied to Inorganic Chemistry: 19F, 31P, 195Pt., etc.

Recommended text books:
Shriver & Atkins, Inorganic Chemistry, 4th Ed., Chapter 6, Oxford University Press.
Brisdon, Inorganic Spectroscopic Methods, Oxford Chemistry Primer 62, O.U.P., 1998.
Iggo, NMR Spectroscopy in Inorganic Chemistry, Oxford Chemistry Primer 83, O.U.P., 1999.
Macomber, A Complete Introduction to Modern NMR Spectroscopy, Wiley-Interscience, 1998.

3. NMR SPECTROSCOPY: APPLICATION TO ORGANIC CHEMISTRY
Lecturer: Dr. P. Stevenson E-mail address: p.stevenson@qub.ac.uk
7 Lectures, 2 seminars and 2 workshops.

Detailed synopsis:

1H NMR Spectroscopy.
Variation of proton chemical shift with molecular environment. Effect of electronegativity and magnetic anisotropy on chemical shift. 1H chemical shifts of common functional groups and integration. Scalar coupling, and its effect on proton NMR spectra. Magnetic equivalence and the n+1 rule. Use of Pascal’s Triangle to predict intensities of multiplets. Angular dependence of coupling constants and the Karplus equation. Analysis of simple multiplets and of multiplets containing more than one coupling constant. Brief introduction to second order systems AB and ABX. Use of coupling constants to determine connectivity patterns and hence molecular structure. Decoupling.

13C NMR Spectroscopy.
13C chemical shifts of common functional groups. Prediction of 13C chemical shifts using empirical formulae. Relative intensity of 13C signals. DEPT and APT will be introduced for assigning methyl, methylene, methine and quaternary carbons.

Recommended text books:
Shriver & Atkins, Inorganic Chemistry, 4th Ed., Chapter 6, Oxford University Press.
Williams and Fleming, Spectroscopic Methods in Organic Chemistry, McGraw Hill.

4. CRYSTAL CHEMISTRY, X-RAY DIFFRACTION AND CRYSTALLOGRAPHY
Lecturer: Dr. P. Nockemann E-mail address: p.nockemann@qub.ac.uk
7 Lectures, 2 seminars and 2 workshops.

Detailed synopsis:

Crystal Chemistry
Classification of solids. Structures of molecular, ionic, covalent and metallic crystals. Lattices, lattice points, unit cells and cell dimensions. Crystal systems and Bravais lattices. Crystal symmetry and symmetry elements. Point groups and space groups. Miller indices.
Diffraction of X-Rays by Crystals
Production and diffraction of X-rays. The Bragg equation. Scattering of X rays by atoms and by unit cells. Variation in diffraction intensity. Electron density. The phase problem. Structural factors. Solution and refinement of crystal structures. Experimental methods.

Powder Diffraction (XRD)
Microcrystalline aggregates. The Debye-Scherrer Method. Uses of XRD – advantages and limitations. Ab initio structure determination from powder data – the Rietveld method.
Neutron, Synchrotron and Electron Diffraction
Uses and limitations.
Taught by external lecturer Tristan Youngs from the ISIS Neutron Source in Oxfordshire.

Learning Objectives

By the end of this course students should be able to:
i) Know the principles of molecular symmetry and be able to classify molecules according to their symmetry. Know the structures of simple solids.
ii) Know the principles of mass spectrometry, IR and NMR spectroscopy, and X-ray diffraction, and understand what information each technique provides.
iii) Be able to derive the structures of organic and inorganic compounds by a combination of analytical and spectroscopic techniques.

Skills

Subject specific problem-solving skills in exams and seminars (includes team working).
Working with numbers, including data handling and calculation.

Assessment

Assessment:
Workshops 60 %
Course work 40 %

Both the workshops and total coursework elements must be passed at 40%.

Course Requirements:
Practical attendance at 80 %
Practical report submission 80 %