Details of CH4204 (Spring 2020)

Level: 4 Type: Theory Credits: 4.0

Course CodeCourse NameInstructor(s)
CH4204 Physical Methods of Structural Elucidation Rahul Banerjee,
Supratim Banerjee

Preamble
In this course, three physical techniques namely NMR Spectroscopy, Mass Spectrometry and X-ray Crystallography will be discussed. These techniques have become indispensable for the structural determination of organic and inorganic compounds. Basic theory of the techniques as well as their application in the elucidation of unknown structures will be discussed.

Syllabus
Syllabus: lecture wise (40 Lectures)

1. What is NMR? Basic principles and history. Nuclear spins and nuclear magnetic moment, nuclear spins in a magnetic field and NMR signal. (2 lectures)
2. 1H NMR spectroscopy and Pulse NMR technique. Spin-lattice and spin-spin relaxation times.(2 lectures)
3. Chemical shifts and discussion on chemical shifts of protons in organic compounds.(2 lectures)
4. Spin-spin coupling, chemical and magnetic equivalence, spin system notation.Discussion on NMR spectra of different kinds of organic compounds. (2 lectures)
5. 13C NMR spectroscopy and proton decoupled spectra. An introduction to DEPT and APT techniques.(2 lectures)
6. Nuclear Overhauser Effect (NOE) and NOE difference spectra in the identification of stereochemistry.(2 lectures)
7. Dynamic NMR spectroscopy. (2 lectures)
8. 2D NMR spectroscopy, COSY, HETCOR and NOESY and their applications in the determination of structures of organic compounds.(3 lectures)
9. A brief introduction to solid state NMR and Magic angle spinning (MAS). (1 lecture)
10. Introduction to Mass Spectrometry, ionization methods and mass analysers. Identification of molecular ion and analysis based on ion-molecule chemistry. (4 lectures)
11. Crystal Lattices, Crystal Symmetry, Close Packed Structures, Miller Indices and Reciprocal Lattice. (3 lectures)
12. Physical Properties of Crystals, X-rays: Origin and Properties. X-ray Diffraction & Braggs Law, Ewald Sphere. (3 lectures)
13. X-ray Diffraction Techniques, Single Crystal Techniques, Fourier Transforms (real vs reciprocal space).(3 lectures)
14. Scattering of X-rays by Crystals, The atomic structure factor, The structure factor (X-ray diffraction, electron diffraction and neutron diffraction). (3 lectures)
15. The Friedels Law, Systematic Absences, Practical determination of space groups, Data reduction.(2 lectures)
16. Crystal Growing Methods, Crystal selection to structure refinement.(2 lectures)
17. Mssbauer effect; Hyperfine Interactions between Nuclei and Electrons and Mssbauer Parameters (Isomer shift, quadrupole splitting, Magnetic splitting); examples related to iron based coordination complexes and organometallic complexes (2 lectures)

Prerequisite
None

References
1. Introduction to Spectroscopy: Donald L. Pavia, Gary M. Lampman, George S. Kriz and James R. Vyvyan.
2. Solving Problems with NMR Spectroscopy: Atta-Ur-Rahman, Muhammad Iqbal Choudhary and Atia-Tul-Wahab.
3. Crystal Structure Analysis for Chemist and Biologists: J. P. Glusker, M. Lewis and M. Rossi.
4. Crystal Structure Analysis: Principle and Practice: W. Clegg, A. J. Blake, J. M. Cole, J. S. O. Evans and P. Main.
NMR Spectroscopy: What is NMR? Basic principles and history. Nuclear spins and nuclear magnetic moment, nuclear spins in a magnetic field and NMR signal. 1H NMR spectroscopy and Pulse NMR technique. Spin-lattice and spin-spin relaxation times. Chemical shifts and discussion on chemical shifts of protons in organic compounds. Spin-spin coupling, chemical and magnetic equivalence, spin system notation. Discussion on NMR spectra of different kinds of organic compounds. 13C NMR spectroscopy and proton decoupled spectra. An introduction to DEPT and APT techniques. Nuclear Overhauser Effect (NOE) and NOE difference spectra in the identification of stereochemistry. Dynamic NMR spectroscopy. 2D NMR spectroscopy, COSY, HETCOR and NOESY and their applications in the determination of structures of organic compounds. A brief introduction to solid state NMR and Magic angle spinning (MAS).
Mass Spectrometry: Introduction to Mass Spectrometry, ionization methods and mass analysers. Identification of molecular ion and analysis based on ion-molecule chemistry.
X-ray Crystallography: Crystal Lattices, Crystal Symmetry, Close Packed Structures, Miller Indices and Reciprocal Lattice. Physical Properties of Crystals, X-rays: Origin and Properties. X-ray Diffraction & Braggs Law, Ewald Sphere. X-ray Diffraction Techniques, Single Crystal Techniques, Fourier Transforms (real vs reciprocal space). Scattering of X-rays by Crystals, the atomic structure factor and the structure factor (X-ray diffraction, electron diffraction, neutron diffraction). The Friedels Law, Systematic Absences, Practical determination of space groups, Data reduction. Crystal Growing Methods, Crystal selection to structure refinement.
Mssbauer spectroscopy: Mssbauer effect; Hyperfine Interactions between Nuclei and Electrons and Mssbauer Parameters (Isomer shift, quadrupole splitting, Magnetic splitting); examples related to iron based coordination complexes and organometallic complexes

Course Credit Options

Sl. No.ProgrammeSemester NoCourse Choice
1 IP 2 Not Allowed
2 IP 4 Elective
3 IP 6 Not Allowed
4 MR 2 Not Allowed
5 MR 4 Not Allowed
6 MS 8 Core
7 RS 1 Elective
8 RS 2 Elective