George L. Clark 3M Materials X-ray Chemistry Laboratory Facility DirectorDanielle L. Gray CrystallographerAmy

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Presentation transcript:

George L. Clark 3M Materials X-ray Chemistry Laboratory Facility DirectorDanielle L. Gray CrystallographerAmy BiocrystallographerYi Gui Business Hours8:30a - 12:00p and 1:00p - 4:30pMonday - Friday Consulting Hours10:00a - 11:00a and 2:00p - 3:00pMonday - Friday Laboratory EntryNortheast Ground Floor Noyes, Room 60 Laboratory Phone

Brief History 1895 Roentgen, Discovers X-rays 1912 Laue, Friedrich, Knipping, Crystals diffract 1914 Bragg and Lawrence, solve atomic positions 1953 Rosalind Franklin, structure of DNA 1915 Both Braggs, win Nobel Prize in Physics 1928 Lonsdale, structure of benzene 1993 Bruker produces first CCD detector 1979 Sheldrick, writes SHELXTL

SHELXTL XPREP XS XP Chemistry P 2 1 /n a = (4) b = (2) c = (1) beta = (1) XL Overview

Organic Chemistry and Crystallography it matters

Absolute structure without a heavy atom Thompson, A.L.; Watkin, D.J. Tetrahedron: Assymetry, 2009, 20, Crystallize the compound with a component of known stereochemistry 2.Bijvoet Pairs (h k l and -h -k -l) need to be examined for anomalous dispersion effects Centrosymmetric vs. Non-centrosymmetric I hkl = I -h-k-l I hkl ≠ I -h-k-l Flack and/or Hooft Analysis Must have Cu radiation with no heavy atoms!

The main pitfall of absolute structures Is the crystal examined a representative of the bulk crystals? –Racemic mixtures can crystallize 1.As a centrosymmetric crystal 2.As a non-centrosymmetric crystal that is twinned 3.Each individually as non-centrosymetric crystals –Circular dichroism or enantioselective chromatography to test if crystal is the same as bulk

Crystal Quality is Essential YES MAYBE NO

The Ideal Sample The ideal sample, like this 40 x 70 x 360 μm crystal mounted on a 300 μm cryo-loop, is attached using an inert oil, frozen in place using a cold gas stream, and recovered after the diffraction experiment is finished. Like many spectroscopic techniques, the overall amplitude of the diffraction pattern is proportional to sample volume. There are no limits on crystal morphology, but the practical range of linear dimensions is 5 to 500 μm. Air, temperature, and light sensitive samples are routinely used.

Growing “good” crystals Solvent Cooling Solvent Evaporation Layering Liquid/Liquid diffusion Vapor Diffusion Sublimation