Jul 042012
 

Picture of Emmanuel Marfo-Owusu
Following his degree in Tokyo studying supramolecular complexes of achiral surfactant molecules with racemic and chiral aromatic guest molecules, Emmanuel travelled extensively.  He has worked at the Ghana Atomic Energy Commission as Senior Scientific officer; at the Department of Chemistry in University of Ghana as Senior Lecturer; at the Department of Chemistry in Mississippi State University, Starkville;  at the Department of Chemistry in University of Washington, Seattle; at the Chemistry Department in Sultan Qaboos University in the Sultanate of Oman; at the University of Nizwa, in Oman as an Assistant Professor of Chemistry, as well as studying at the Department of Crystallography in University of Pittsburgh and the Structural Chemistry Laboratory in University of Witwatersrand, South-Africa.

Since 2010, Emmanuel has been working at the Chemistry Department at the University of Cape Coast in Ghana as an Associate Professor and he is working hard to establish the first crystallography laboratory in Ghana to serve Ghana Scientific Institutions and those in the West-Africa sub-region.  Emmanuel’s current research is centred on structural studies of self assembly structures that aggregate through O-H…N, N-H…O and O-H…O inter/intramolecular interactions, with special emphasis on those that possess functional molecular properties.

May 012012
 

Presented by: Nicholas G. White
Research Leader: Prof. Paul D. Beer
Published: Chemical Communications

Pyridinium-3,5-bis(triazole) can bind anions through polarised C-H···anion hydrogen bonds.  We have incorporated this motif into pseudorotaxanes, catenanes and rotaxanes (in conjunction with an isophthalamide macrocycle), and the resulting interlocked architectures are formed in high yields and display interesting and unusual anion selectivities.  Despite the difficulties of crystallising such systems, single crystals of a pseudorotaxane, rotaxane and catenane have all been isolated (as chloride salts).  Data were collected using a Nonius Kappa-CCD, synchrotron radiation on I19 at Diamond and Cu Kα radiation with an Oxford Diffraction (Agilent) SuperNova (respectively).  All three datasets are of unusually high quality for such systems (final R1 [I > 2σ(I)] = 6.9-8.0%).

Structure of the Month – May 2012

Structure of the Month – May 2012

Apr 302012
 

J Appl. Cryst. (2012), 45, 417-429. [ doi:10.1107/S0021889812015191 ]

Leverages measure the influence that observations (intensity data and restraints) have on the fit obtained in crystal structure refinement. Further analysis enables the influence that observations have on specific parameters to be measured. The results of leverage analyses are discussed in the context of the amino acid alanine and an incomplete high-pressure data set of the complex bis(salicylaldoximato)copper(II). Leverage analysis can reveal situations where weak data are influential and allows an assessment of the influence of restraints. Analysis of the high-pressure refinement of the copper complex shows that the influence of the highest-leverage intensity observations increases when completeness is reduced, but low leverages stay low. The influence of restraints, notably those applying the Hirshfeld rigid-bond criterion, also increases dramatically. In alanine the precision of the Flack parameter is determined by medium-resolution data with moderate intensities. The results of a leverage analysis can be incorporated into a weighting scheme designed to optimize the precision of a selected parameter. This was applied to absolute structure refinement of light-atom crystal structures. The standard uncertainty of the Flack parameter could be reduced to around 0.1 even for a hydrocarbon.

Electronic reprints

Publisher’s copy

Apr 202012
 

The 2012 Meeting of the British Crystallographic Association was held at Warwick University.  Oxford was very well represented this year with Kirsten Christensen chairing the Programme Committee and prizes being awarded to Joe Paddison, Nick Funnell and Emma McKinley.

Other contributions from Oxford include:

Karim J. Sutton, Kirsten E. Christensen, Amber L. Thompson & Richard I. Cooper
Exploiting the Tunable Wavelength Capabilities of I19 (Poster & Oral Presentation)

Callum A. Young & Andrew L. Goodwin
An Examination of the Low Temperature Structure of Fe3O4 Using Reverse Monte Carlo Refinements (Oral Presentation)

Andrew L. Goodwin
Frameworks, Flexibility and Frustration (Oral Presentation)

Kirsten E. Christensen, Amber L. Thompson & Arwen R Pearson
Discussion Forum:  From Small Molecules to Proteins:  Bridging the Gap

Emma J. McKinley, Kirsten E. Christensen & Amber L. Thompson
Investigation of the Transient Modulated Phase of Barluenga’s Reagent (Poster)

Andrew B. Cairns, Amber L. Thompson, Andrew L, Goodwin, Matthew G. Tucker & Julien Haines
Anomalous Compression of Cyanide Frameworks:  Mechanisms for Extreme Negative Response (Poster)

Callum A. Young, Edward Dixon, Michael A. Hayward & Andrew L. Goodwin
Apical Oxygen Bonding in YBCO – A Reverse Monte Carlo Approach (Poster)

Ines E. Collings, Andrew B. Cairns, Amber L. Thompson, Andrew L, Goodwin, Philip Pattison, Julien Haines, Matthew G. Tucker, Julia E. Parker & Chiu C. Tang
Transferable Mechanics in Molecular Framework Materials (Poster)

Joseph A. M. Paddison, Andrew L. Goodwin, Ross Stewart, Pascal Manuel, Matthias J. Gutmann, David A. Keen, Matthew G. Tucker, Andrew Wildes & Brian Rainford
Frustration and Magnetic Diffuse Scattering in β-Mn0.8Co0.2 and MnO:  A Reverse Monte Carlo Study (Poster)

Matthew Cliffe & Andrew L. Goodwin
Disorder and Defects in Zirconium MOFs (Poster)

Nicholas P. Funnell, Martin T. Dove Andrew L. Goodwin Simon Parsons & Matthew G. Tucker
How Molecules Prepare to Undergo a Transition:  The Onset of Disorder in Solid Cyclohexane (Poster).

 

Karim speaks to the Young Crystallographers

Karim speaks to the Young Crystallographers

 

Emma, Richard and Ines go to the conference dinner

Emma, Richard and Ines go to the conference dinner

Ines and Emma

Ines and Emma

This time Karim brought his Dad...

This time Karim brought his Dad…

Callum and Emma at Dinner

Callum and Emma at Dinner

Kirsten presents Nick with his prize

Kirsten presents Nick with his prize

Emma receives her prize

Emma receives her prize

<no comment />

<no comment />

Contemplating Fourier Transforms...

Contemplating Fourier Transforms…

Apr 202012
 

My poster is all about Barluenga’s Reagent,
A cool iodinating and oxidising agent.
It is known to have a solid-state transition,
But we didn’t know at what temperature position.

Variable temperature X-ray diffraction
Let us investigate the transition action.
In addition, we found something a little surprising,
Extra reflections in precession images were arising.

After some thinking we came to the conclusion,
A transient modulated phase must be the solution.
So if this poem has got you excited,
Come and see my poster…

…You are all invited!

E. J. McKinley
BCA 2012.

Emma receives her prize

Emma receives her prize

Mar 192012
 

Acta Cryst.  (2012), C68, o152-o155.    [ doi:10.1107/S0108270112009377 ]

Tetraisohexylammonium bromide [systematic name: tetrakis(4-methylpentyl)azanium bromide], C24H52N+·Br, is a powerful structure II clathrate hydrate crystal-growth inhibitor. The crystal structure, in the space group P3221, contains one ammonium cation and one bromide anion in the asymmetric unit, both on general positions. At 100 K, the ammonium cation exhibits one ordered isohexyl chain and three disordered isohexyl chains. At 250 K, all four isohexyl chains are disordered. In an effort to reduce the disorder in the alkyl chains, the crystal was thermally cycled, but the disorder remained, indicating that it is dynamic in nature.

Tetraisohexylammonium Bromide

Tetraisohexylammonium Bromide

Electronic reprints

  • Oxford University Research Archive [direct pdf]

Publisher’s copy

Mar 072012
 

Dave is the Principal Beamline Scientist on the small-molecule single-crystal diffraction beamline, I19. Before his appointment at Diamond in 2006, Dave was a lecturer in The School of Physics at The University of Edinburgh and he laterally held an EPSRC Advanced Research Fellowship within The School of Chemistry. Apart from developing the beamline to improve its capabilities for the ever increasing user base, his main research interests involve the high-pressure and low-temperature polymorphism of small-molecule systems and the development of in situ crystal growth techniques. Dave can occasionally been seen around the department, usually on Tuesdays, when he gets the chance to attend the Chem. Cryst. group meetings.

Mar 072012
 

Chiralabs are long-term collaborators and world-leading experts in a wide range of spectroscopic, physicochemical and theoretical approaches including in chirality, circular dichroism, optical spectroscopies, crystallization and biopharmaceutical analysis. Specialist areas of investigation include:

  • Molecular chirality & enantiomeric composition
  • Crystal growth, polymorphism & solubility
  • Biomacromolecular structure, folding and properties
  • Biopharmaceutical development & spectroscopic fingerprinting
  • Spectroscopic & physicochemical characterisation

Chiralabs is also the home of CrystalGEM, the internationally award winning rational crystallisation screening technology that has revolutionised the screening of pharmaceutical polymorphism, morphology and crystal growth.

Feb 192012
 

Dalton Trans. (2012), 41, 1951-1960.    [ doi:10.1039/C1DT11758K ]

Uranium complexes of bis(p-tert-butyl-salicylidene)-1,2-diphenylethylenediamine (1) and bis(salicylidene)-1,2-diphenylethylenediamine (2) have been synthesized and investigated by X-ray single crystal diffraction and MD calculations in Periodic Boundary Conditions. Both compounds form crystals which are densely packed and do not provide voids accessible to solvent molecules. The configurations adopted by 1 and 2 are determined by well defined T-shaped and π-stacking non covalent interactions between phenyl groups of adjacent molecules as well as by a network of hydrogen bonds. These interactions and the relative arrangements of the molecules, explain the packing in the crystal structures. Each uranyl moiety shows a penta-coordination in the equatorial plane perpendicular to the trans oxygens giving rise, in both compounds, to a bypiramidal geometry. As usual for this class of compounds, the 5th position is characterized by the presence of the coordinated solvent. The in silico simulations confirm this hypothesis in very fine details. Moreover, in 1, even the partial occupancy of the solvent molecule determined from the crystal structure refinement, was shown to be due to a constrained freedom of motion of the solvent molecule that can be reproduced by molecular dynamics. This suggests that the reported disorder is not due to a poor quality of the harvested crystals but to a structural feature. In further agreement with the above mentioned results, DFT calculations demonstrated that the molecular orbital configuration and energies suit the described properties of complexes 1 and 2 suggesting a potential enantioselective activity as already shown by molecules belonging to this class of compounds.

Electronic reprints

  • Oxford University Research Archive [direct pdf]

Publisher’s copy