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Gérard Bricogne

Publications and source records attributed to Gérard Bricogne.

8 recordsLinked to original sources

Automated structure solution with autoSHARP.

We present here the automated structure solution pipeline "autoSHARP." It is built around the heavy-atom refinement and phasing program SHARP, the density modification program SOLOMON, and the ARP/wARP package for automated model building and refinement (using REFMAC). It allows fully automated structure solution, from merged reflection data to an initial model, without any user intervention. We describe and discuss the preparation of the user input, the data flow through the pipeline, and the various results obtained throughout the procedure.

Algorithms↗

On the interpretation and use of <|E|2>(d*) profiles.

Profiles of squared normalized structure factors, <|E|(2)>(d*), have been computed for a large number of proteins and nucleic acids. These are interpreted in terms of their underlying structural features. It is also shown that the 'solvent dip' at around 6.3 A resolution is to a large extent a protein secondary-structure effect that is enhanced by the water structure. A hierarchical classification of protein structures based on their <|E|(2)>(d*) profiles is briefly outlined, together with the use of <|E|(2)>(d*) profiles as an improvement over Wilson absolute scale estimation and as a novel solvent-modelling method.

Cluster Analysis↗

Triiodide derivatization in protein crystallography.

Methods for producing protein derivatives using cryosoak techniques with triiodide solutions are described. The methods have been tested using six different proteins. SAD/SIRAS phasing was attempted for each protein using data measured with conventional Cu Kalpha X-ray equipment and synchrotron radiation. Refinement of all six derivative structures showed that iodine is able to bind as I(-) (as observed with standard halide soaks) and also as the polyiodide anions I(3)(-) and I(5)(-). The various species are able to bind through hydrogen-bond interactions and to more hydrophobic regions of the protein at surface pockets and in intermolecular and intramolecular cavities. On the whole, the derivative agent behaves promiscuously in terms of its binding to proteins and is capable of generating sufficient phasing power from in-house Cu Kalpha data to permit structure solution by SAD. The results of the phasing experiments and structure refinements are presented.

Animals↗

SAD phasing with triiodide, softer X-rays and some help from radiation damage.

SAD data on a triiodide derivative of porcine pancreatic elastase have been recorded from a single sample using 2.0 A wavelength X-rays. The large anomalous signal of iodine at this wavelength allowed the detection of heavy-atom sites and subsequent structure determination using low-redundancy data. Substantial radiation damage was observed during the measurements and this prevented the merging together of all data. However, a straightforward treatment of the radiation effects on the heavy-atom model during parameter refinement resulted in additional phase information being gleaned from the observed reduction in iodine occupancy factors, which in turn produced a significant improvement in the quality of the electron-density map.

Animals↗

Sheldrick's 1.2 A rule and beyond.

An average profile of squared normalized structure factors as a function of resolution, /E/2>(d*), calculated from a large ensemble of high-resolution protein models, is presented. An interpretation is given that provides a structural explanation for Sheldrick's 1.2 A rule for the applicability of direct methods. The implications for the potential effectiveness of extended direct methods, incorporating stereochemical knowledge, are discussed.

Algorithms↗

Interconversion of ATP binding and conformational free energies by tryptophanyl-tRNA synthetase: structures of ATP bound to open and closed, pre-transition-state conformations.

Binding ATP to tryptophanyl-tRNA synthetase (TrpRS) in a catalytically competent configuration for amino acid activation destabilizes the enzyme structure prior to forming the transition state. This conclusion follows from monitoring the titration of TrpRS with ATP by small angle solution X-ray scattering, enzyme activity, and crystal structures. ATP induces a significantly smaller radius of gyration at pH=7 with a transition midpoint at approximately 8mM. A non-reciprocal dependence of Trp and ATP dissociation constants on concentrations of the second substrate show that Trp binding enhances affinity for ATP, while the affinity for Trp falls with the square of the [ATP] over the same concentration range ( approximately 5mM) that induces the more compact conformation. Two distinct TrpRS:ATP structures have been solved, a high-affinity complex grown with 1mM ATP and a low-affinity complex grown at 10mM ATP. The former is isomorphous with unliganded TrpRS and the Trp complex from monoclinic crystals. Reacting groups of the two individually-bound substrates are separated by 6.7A. Although it lacks tryptophan, the low-affinity complex has a closed conformation similar to that observed in the presence of both ATP and Trp analogs such as indolmycin, and resembles a complex previously postulated to form in the closely-related TyrRS upon induced-fit active-site assembly, just prior to catalysis. Titration of TrpRS with ATP therefore successively produces structurally distinct high- and low-affinity ATP-bound states. The higher quality X-ray data for the closed ATP complex (2.2A) provide new structural details likely related to catalysis, including an extension of the KMSKS loop that engages the second lysine and serine residues, K195 and S196, with the alpha and gamma-phosphates; interactions of the K111 side-chain with the gamma-phosphate; and a water molecule bridging the consensus sequence residue T15 to the beta-phosphate. Induced-fit therefore strengthens active-site interactions with ATP, substantially intensifying the interaction of the KMSKS loop with the leaving PP(i) group. Formation of this conformation in the absence of a Trp analog implies that ATP is a key allosteric effector for TrpRS. The paradoxical requirement for high [ATP] implies that Gibbs binding free energy is stored in an unfavorable protein conformation and can then be recovered for useful purposes, including catalysis in the case of TrpRS.

Adenosine Triphosphate↗

Structure of bacterial 3beta/17beta-hydroxysteroid dehydrogenase at 1.2 A resolution: a model for multiple steroid recognition.

The enzyme 3beta/17beta-hydroxysteroid dehydrogenase (3beta/17beta-HSD) is a steroid-inducible component of the Gram-negative bacterium Comamonas testosteroni. It catalyzes the reversible reduction/dehydrogenation of the oxo/beta-hydroxy groups at positions 3 and 17 of steroid compounds, including hormones and isobile acids. Crystallographic analysis at 1.2 A resolution reveals the enzyme to have nearly identical subunits that form a tetramer with 222 symmetry. This is one of the largest oligomeric structures refined at this resolution. The subunit consists of a monomer with a single-domain structure built around a seven-stranded beta-sheet flanked by six alpha-helices. The active site contains a Ser-Tyr-Lys triad, typical for short-chain dehydrogenases/reductases (SDR). Despite their highly diverse substrate specificities, SDR members show a close to identical folding pattern architectures and a common catalytic mechanism. In contrast to other SDR apostructures determined, the substrate binding loop is well-defined. Analysis of structure-activity relationships of catalytic cleft residues, docking analysis of substrates and inhibitors, and accessible surface analysis explains how 3beta/17beta-HSD accommodates steroid substrates of different conformations.

17-Hydroxysteroid Dehydrogenases↗

Triiodide derivatization and combinatorial counter-ion replacement: two methods for enhancing phasing signal using laboratory Cu Kalpha X-ray equipment.

A series of experiments performed at Cu Kalpha wavelength on in-house X-ray equipment are presented which investigate two possibilities for enhancing the experimental phasing signal by means of (i) triiodide/iodide soaks using KI/I(2) and (ii) combinations of counter-ions introduced using the short cryosoak method. Triiodide-derivative crystal structures for five test proteins have been refined and reveal that iodine can bind as polyiodide and single iodide ions through hydrophobic and hydrogen-bonding interactions both at the molecular surface and in intramolecular and intermolecular cavities. In three cases, the structures could be automatically determined with autoSHARP using in-house SAD and SIRAS data. The investigation of combinatorial counter-ion replacement using multiple salts with Na(+) and Cs(+) as cations and I(-) and Cl(-) as anions reveals that, for the case of hen egg-white lysozyme, significant improvement in phasing signal is obtained by the combined use of salts compared with SIRAS methods using native and single short-soak derivative data sets.

Animals↗