Powder and single-crystal diffraction of small molecules

Small molecules such as drugs and enzymatic cofactors have been subjected to structural analysis using neutron powder and single-crystal diffraction to provide information on ionization and hydration states and bonding networks. Neutron experiments represent a valid analysis additional to X-ray diffraction studies since they are able to provide hydrogen atom anisotropic temperature factors and thus a more complete picture of the molecular characteristics. A complete model of the thermal motional properties of the molecule's constituent atoms permits the deconvolution of the thermal motion in the molecule from the static electron density determined using X-rays.
 

Case study: the structure of creatine monohydrate, (NH2)CN(CH3)CH2CO2.H2O
Creatine phosphate acts as an energy reservoir in vertebrate muscle. Refinement of data from a single-crystal neutron diffraction experiment using the diffractometer SXD at RAL revealed the locations and thermal properties of all atoms in the molecule. This permitted good definition of the extensive network of hydrogen bonds present in the crystal. The thermal parameter analysis revealed significant torsional motion of the methyl group even at 20 K. J. Chem. Soc. Faraday Trans. (1997) 93, 1875-1879.

Case study: the structures of ibufrofen, acetylcholine and dopamine
Single-crystal analysis of the analgesic ibuprofen and the neurotransmitter acetylcholine were carried out using station SXD. A powder diffraction structure determination for dopamine, another neurotransmitter, using HPRD (the highest resolution neutron powder diffractometer in the world) at RAL was also completed.

Case study: the structure of paracetomol
The structure of the analgesic paracetomol, which is structurally related to ibuprofen, was determined using single crystal neutron diffraction. Anisotropic thermal parameters for all atoms were determined, revealing gross positional variation due to thermal motion for the methyl group hydrogens. J. Mol. Struct. (1997) 405, 207-217.

Case study: the structures and interactions of Buckminsterfullerenes
Neutron experiments have contributed to a better understanding of the structure and interactions of spherical carbon (Nobel Prize in Chemistry, 1996), for which a broad range of potential applications including pharmaceutical products and industrial catalysts have been proposed.

The web page to the instruments relevant to small-molecule structure determination at RAL give some further examples, as does the D19 web page at the ILL.
 
 


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