Solid State Chemistry   (2151H)

Academic year:

2012/2013.

Attendance requirements:

There are no requirements.

ECTS:

9

Study level:

Study program:

Teacher:

Tamara R. Todorović, Ph.D.
full professor, Faculty of Chemistry, Studentski trg 12-16, Beograd

Assistants:

—

Hours of instruction:

Weekly: four hours of lectures + two hours of exercises + three hours of labwork (4+2+3)

Goals:

At this course students will learn to interpret the results of structural analysis of complex molecules. In addition, they should be qualified to solve simple crystal structures and to analyze purity of different inorganic materials.

Outcome:

At this course students learned how to interpret the results of X-ray analysis and solve simple crystal structures.

Teaching methods:

Lectures, experimental exercises and theoretical/calculating exercises.

Extracurricular activities:

Home works; a literature search for the proposed topic.

Coursebooks:

Main coursebooks:

1. Lj. Karanović, D. Poleti, X-ray analysis, Zavod za udžbenike i nastavna sredstva, Belgrade, 2003.
2. B. Prelesnik, Fundamentals of Crystallography and X-ray analysis, script for internal usage
3. B. Prelesnik, K. Anđelković, D. Radanović, T. Todorović, A Collection of Illustrative Problems in Crystallography and X-ray analysis, Faculty of Chemistry, Belgrade 2007.

Supplementary coursebooks:

• A.R. West, Solid State Chemistry and its Applications, John Willey & Sons, 1990

Additional material:

—

Lectures:

5 points (4 hours a week)

Syllabus:

1) Physical conditions of substances, specificities of the solid state.

2) and 3) Geometrical crystallography (the crystal periodicity, the motif arrangement, the motif repetition, crystal lattice representation, crystallographic unit cell, symmetry elements and symmetry operations, symmetry groups, crystal systems and classes, space lattices and the space groups).

4) X-rays and diffraction of X-rays on a crystal lattice.

5) Experimental methods of X-ray diffraction.

6) Diffraction experiment (Bragg’s law, direct and reciprocal space, indexing of reflections, Ewald’s sphere, diffraction intensities, the structure factor).

7) Film-based techniques for single crystal X-ray diffraction (equiinclination Weissenberg).

8) Methods for the preparation of single crystals, choosing a crystal, X-ray diffraction data collection, data reduction.

9) Basic principles of X-ray analysis (the phase problem, Fourier synthesis, Patterson synthesis).

10) Heavy-atom methods, building a structural model, refinement of the parameters for all atoms in the structure and interpretation of the obtained results (atomic coordinates, atomic thermal vibrations, bond lengths and valence angles, ring conformations, absolute configuration).

11) Crysallochemical criteria for accuracy of the structure, descriptive Crystallochemistry.

12) Thermal analysis (principals, application; TG (thermal gravimetry), DSC (differential scanning calorimetry), DTA (differential thermal analysis) with special emphasis on inorganic compounds).

13) Spectroscopic techniques (IR and EPR); basic principals and interpretation of IR spectra of inorganic compounds.

14) Magnetic properties of substances.

15) Examples of magnetic materials, their structure and properties.

Exercises:

0 points (2 hours a week)

Labwork:

15 points (3 hours a week)

Syllabus:

The 1^st, 2^nd and 3^rd week: geometrical crystallography (theoretical-calculating exercises).

The 4^th week: unit-cell determination (crystallographic axes and angles) by film techniques, rotation and oscillation methods (theoretical-calculating exercises).

The 5^th week: Weissenberg method, determination of the space group on the basis of systematic absences of specific reflections, Weissenberg zero-level and upper-level photographs (theoretical-calculating exercises).

The 6^th week: The morphological features of crystals (observing), choosing a suitable crystal for diffraction experiment, measuring a crystal density by flotation method (experimental exercises).

The 7^th week: Structure factors (theoretical-calculating exercises).

The 8^th week: reciprocal lattice (theoretical-calculating exercises).

The 9^th week: Patterson synthesis (theoretical-calculating exercises).

The 10^th week: Packing efficiency in crystal structures (theoretical-calculating exercises).

The 11^th week:  Debye-Scherrer diagrams, indexing of Bragg maxima (theoretical-calculating exercises).

The 12^th week: Crystallographic softwares (presentation) and data base (searching).

The 13^th week: Interpretation of TG, DSC and DTA diagrams (theoretical-calculating exercises).

The 14^th week: Determination of magnetic moment of paramagnetic substances using Evans’s method (experimental exercises).

The 15^th week: Summary of acquired knowledge from Solid State Chemistry.

Semester papers:

5 points

Colloquia:

20 points

Homework:

5 points

Oral exam:

50 points