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Structure Determination

The document discusses several techniques for analyzing inorganic structures including circular dichroism, electron paramagnetic resonance, nuclear magnetic resonance, and X-ray spectroscopy. It provides examples of using cobalt ions with ethylenediamine in circular dichroism, the hyperfine structure of the silyl radical seen by electron paramagnetic resonance, and Bloch and Purcell winning the Nobel Prize in 1952 for their work developing nuclear magnetic resonance. It also describes using powder patterns in X-ray diffraction for qualitative analysis and determining if structures are isostructural.

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Sheena Gagarin
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53 views19 pages

Structure Determination

The document discusses several techniques for analyzing inorganic structures including circular dichroism, electron paramagnetic resonance, nuclear magnetic resonance, and X-ray spectroscopy. It provides examples of using cobalt ions with ethylenediamine in circular dichroism, the hyperfine structure of the silyl radical seen by electron paramagnetic resonance, and Bloch and Purcell winning the Nobel Prize in 1952 for their work developing nuclear magnetic resonance. It also describes using powder patterns in X-ray diffraction for qualitative analysis and determining if structures are isostructural.

Uploaded by

Sheena Gagarin
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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Inorganic Structure

Techniques
Circular Dichroism
Cobalt ions with Ethylenediamine

purple cis-enantiomer pair green trans isomer


Cobalt ions with Ethylenediamine
[Co(en)3]+

absorption spectrum

CD spectra of the 2
optical isomers
[Co(ala)3]+
Electron Paramagnetic Resonance

Hyperfine Structure of
the EPR spectrum of
the silyl radical, SiH3
Electron Paramagnetic Resonance

The copper is pure Cu-63.


Nuclear Magnetic Resonance
• Bloch and Purcell won the Nobel Prize in
Physics- 1952
• most common nuclei studied using NMR
are H-1, C-13, F-19 and P-31
Nuclear Magnetic Resonance
• other spin 1/2 nuclei: N-15, Fe-57, Ag-107,
Ag-109, Sn-117, Sn-119, W-183, Pt-195,
Hg-199, and Pb-207
• Other nuclei: N-14 spin of 1, Li-7 spin of
3/2, B-10 a spin of 3, O-17 a spin of 5/2,
Co-59 a spin of 7/2, and In-115 a spin of 9/2
Anasazi 60Mhz NMR

With broadband
probe, capable of
studying H-1, C-13,
F-19, Si 29, and P-31.
X-Ray Spectroscopy
• Emission
• Absorption
• Diffraction
Diffraction
Powder Pattern
– qualitative analysis => ASTM database
– isostructural
Diffraction of X-Rays
Bragg's Law "Diffraction of X-rays by a crystal."
Powder Diffractometer
Goniometer Head for Single Crystal
Automatic Diffractometer
Automatic Diffractometer
X-ray Diffraction
Information provided by X-ray diffraction:
1. Declare that structures are isostructural.
2. Identify unknowns
3. Determine crystal structure

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