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X-ray diffraction using focused-ion-beam-prepared single crystals

High-quality single-crystal X-ray diffraction measurements are a prerequisite for obtaining precise and reliable structure data and electron densities. The single crystal should therefore fulfill several conditions, of which a regular defined shape is of particularly high importance for compounds consisting of heavy elements with high X-ray absorption coefficients. The absorption of X-rays passing through a 50 µm-thick LiNbO3 crystal can reduce the transmission of Mo Kα radiation by several tens of percent, which makes an absorption correction of the reflection intensities necessary. In order to reduce ambiguities concerning the shape of a crystal, used for the necessary absorption correction, a method for preparation of regularly shaped single crystals out of large samples is presented and evaluated. This method utilizes a focused ion beam to cut crystals with defined size and shape reproducibly and carefully without splintering. For evaluation, a single-crystal X-ray diffraction study using a laboratory diffractometer is presented, comparing differently prepared LiNbO3 crystals originating from the same macroscopic crystal plate. Results of the data reduction, structure refinement and electron density reconstruction indicate qualitatively similar values for all prepared crystals. Thus, the different preparation techniques have a smaller impact than expected. However, the atomic coordinates, electron densities and atomic charges are supposed to be more reliable since the focused-ion-beam-prepared crystal exhibits the smallest extinction influences. This preparation technique is especially recommended for susceptible samples, for cases where a minimal invasive preparation procedure is needed, and for the preparation of crystals from specific areas, complex material architectures and materials that cannot be prepared with common methods (breaking or grinding).




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The use of local structural similarity of distant homologues for crystallographic model building from a molecular-replacement solution

The performance of automated protein model building usually decreases with resolution, mainly owing to the lower information content of the experimental data. This calls for a more elaborate use of the available structural information about macromolecules. Here, a new method is presented that uses structural homologues to improve the quality of protein models automatically constructed using ARP/wARP. The method uses local structural similarity between deposited models and the model being built, and results in longer main-chain fragments that in turn can be more reliably docked to the protein sequence. The application of the homology-based model extension method to the example of a CFA synthase at 2.7 Å resolution resulted in a more complete model with almost all of the residues correctly built and docked to the sequence. The method was also evaluated on 1493 molecular-replacement solutions at a resolution of 4.0 Å and better that were submitted to the ARP/wARP web service for model building. A significant improvement in the completeness and sequence coverage of the built models has been observed.




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DatView: a graphical user interface for visualizing and querying large data sets in serial femtosecond crystallography

DatView is a new graphical user interface (GUI) for plotting parameters to explore correlations, identify outliers and export subsets of data. It was designed to simplify and expedite analysis of very large unmerged serial femtosecond crystallography (SFX) data sets composed of indexing results from hundreds of thousands of microcrystal diffraction patterns. However, DatView works with any tabulated data, offering its functionality to many applications outside serial crystallography. In DatView's user-friendly GUI, selections are drawn onto plots and synchronized across all other plots, so correlations between multiple parameters in large multi-parameter data sets can be rapidly identified. It also includes an item viewer for displaying images in the current selection alongside the associated metadata. For serial crystallography data processed by indexamajig from CrystFEL [White, Kirian, Martin, Aquila, Nass, Barty & Chapman (2012). J. Appl. Cryst. 45, 335–341], DatView generates a table of parameters and metadata from stream files and, optionally, the associated HDF5 files. By combining the functionality of several commonly needed tools for SFX in a single GUI that operates on tabulated data, the time needed to load and calculate statistics from large data sets is reduced. This paper describes how DatView facilitates (i) efficient feedback during data collection by examining trends in time, sample position or any parameter, (ii) determination of optimal indexing and integration parameters via the comparison mode, (iii) identification of systematic errors in unmerged SFX data sets, and (iv) sorting and highly flexible data filtering (plot selections, Boolean filters and more), including direct export of subset CrystFEL stream files for further processing.




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FXD-CSD-GUI: a graphical user interface for the X-ray-diffraction-based determination of crystallite size distributions

Bragg intensities can be used to analyse crystal size distributions in a method called FXD-CSD, which is based on the fast measurement of many Bragg spots using two-dimensional detectors. This work presents the Python-based software and its graphical user interface FXD-CSD-GUI. The GUI enables user-friendly data handling and processing and provides both graphical and numerical crystal size distribution results.




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In-house texture measurement using a compact neutron source

In order to improve the instrumental accessibility of neutron diffraction techniques, many emerging compact neutron sources and in-house neutron diffractometers are being developed, even though the precision level of neutron diffraction experiments performed on such instruments was thought to be incomparable with that of large-scale neutron facilities. As a challenging project, the RIKEN accelerator-driven compact neutron source (RANS) was employed here to establish the technical environment for texture measurements, and the recalculated pole figures and orientation distribution functions of an interstitial-free steel sheet obtained from RANS were compared with the results from another two neutron diffractometers well established for texture measurement. These quantitative comparisons revealed that the precise neutron diffraction texture measurement at RANS has been realized successfully, and the fine region division of the neutron detector panel is invaluable for improving the stereographic resolution of texture measurements. Moreover, through selectively using the parts of the obtained neutron diffraction patterns that exhibit good statistics, the Rietveld texture analysis improves the reliability of the texture measurement to a certain extent. These technical research results may accelerate the development of other easily accessible techniques for evaluation of engineering materials using compact neutron sources, and also help to improve the data-collection efficiency for various time-resolved scattering experiments at large-scale neutron facilities.




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Usefulness of oils for cleaning the host matrix and for cryoprotection of lipidic cubic phase crystals

Several oils were examined for use in the cleaning and cryoprotection of crystals in the lipidic cubic phase in terms of their effect on the crystal stability, the background scattering and the facilitation of the experiment.




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X-ray diffraction using focused-ion-beam-prepared single crystals

This study demonstrates a new preparation method for single-crystal X-ray diffraction samples using a focused ion beam. The results of the structure determination and electron density maps with differently prepared samples are discussed, to evaluate this new method.




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EDDIDAT: a graphical user interface for the analysis of energy-dispersive diffraction data

EDDIDAT is a program that provides a graphical user interface (GUI) for the evaluation of energy-dispersive X-ray diffraction data with the focus on the depth-resolved residual stress analysis.




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TAAM: a reliable and user friendly tool for hydrogen-atom location using routine X-ray diffraction data

Hydrogen is present in almost all of the molecules in living things. It is very reactive and forms bonds with most of the elements, terminating their valences and enhancing their chemistry. X-ray diffraction is the most common method for structure determination. It depends on scattering of X-rays from electron density, which means the single electron of hydrogen is difficult to detect. Generally, neutron diffraction data are used to determine the accurate position of hydrogen atoms. However, the requirement for good quality single crystals, costly maintenance and the limited number of neutron diffraction facilities means that these kind of results are rarely available. Here it is shown that the use of Transferable Aspherical Atom Model (TAAM) instead of Independent Atom Model (IAM) in routine structure refinement with X-ray data is another possible solution which largely improves the precision and accuracy of X—H bond lengths and makes them comparable to averaged neutron bond lengths. TAAM, built from a pseudoatom databank, was used to determine the X—H bond lengths on 75 data sets for organic molecule crystals. TAAM parametrizations available in the modified University of Buffalo Databank (UBDB) of pseudoatoms applied through the DiSCaMB software library were used. The averaged bond lengths determined by TAAM refinements with X-ray diffraction data of atomic resolution (dmin ≤ 0.83 Å) showed very good agreement with neutron data, mostly within one single sample standard deviation, much like Hirshfeld atom refinement (HAR). Atomic displacements for both hydrogen and non-hydrogen atoms obtained from the refinements systematically differed from IAM results. Overall TAAM gave better fits to experimental data of standard resolution compared to IAM. The research was accompanied with development of software aimed at providing user-friendly tools to use aspherical atom models in refinement of organic molecules at speeds comparable to routine refinements based on spherical atom model.




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TAAM: a reliable and user friendly tool for hydrogen-atom location using routine X-ray diffraction data

Transferable Aspherical Atom Model (TAAM) instead of Independent Atom Model (IAM) applied through DiSCaMB software library in the structure refinement against X-ray diffraction data largely improves the X—H bond lengths and make them comparable to the averaged neutron bond lengths.




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Smithsonian Scientist Discovers Two New Bat Species Hiding in Museum Collections for More Than 150 Years

While studying bats recently at the Academy of Natural Sciences in Philadelphia, Smithsonian mammalogist Kristofer Helgen discovered a new species of flying fox bat from […]

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Fossils of tiny cupuladriid colonies reveal extinction can lag more than one million years after its cause

A new Smithsonian study that examines 10 million years of the evolution of tiny coral-like organisms called cupuladriid bryzoans has revealed that some species of this organism lingered on earth for more than one million years after the event that ultimately caused their extinction: the rising of the Isthmus of Panama.

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The Smithsonian’s National Air and Space Museum opens new Public Observatory on the Mall in Washington, D.C.

The Smithsonian’s National Air and Space Museum has opened a new Public Observatory that contains a 16-inch, 3,000-pound Boller and Chivens telescope, on loan from the Smithsonian Astrophysical Observatory. Through this powerful telescope, museum visitors can now observe the sun (with a special filter), the moon and the brighter stars and planets, such as Venus, Jupiter and Saturn, during daylight hours. Funding for the project was provided by the National Science Foundation.

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Hall of Human Origins to open at Smithsonian’s Natural History Museum, March 17, 2010

A major new exhibition hall dedicated to the discovery and understanding of human origins will open next year at the Smithsonian's National Museum of Natural History: The David H. Koch Hall of Human Origins

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For first time, scientists prove locusts use vision to place their legs when walking

In their laboratory, scientists from the University of Cambridge, the University of Southampton and the Smithsonian Tropical Research Institute in Panama, observed as a number of adult locusts walked along a horizontal ladder. After covering the right or left eye of an insect, the scientists observed a significant increase in the error rate of rungs missed by the front leg on the side of the covered eye.

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Ancient star discovered through patience and clever use of technology

Finding this stellar relic wasn’t easy. It is 60,000 times dimmer than the faintest star visible to the unaided eye. The team also had to distinguish it from many surrounding stars that aren’t so old. Just like an archaeological dig, the hunt succeeded through a combination of patience and clever use of technology.

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Eighty-thousand bark beetles enter National Museum of Natural History collections

The Stephen L. Wood collection brings the collection of bark beetles held in the Natural History Museum’s Department of Entomology to an impressive 180,000 specimens, making it one of the most extensive collections in world.

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Killing of methane-producing megafauna may have caused cooling 13,000 years ago

New world megafauna such as mammoths, bison and camelids that were alive at the end of the Pleistocene epoch (some 13,000 years ago) would have produced massive amounts of methane-rich flatulence and belching, thanks to the cellulose-digesting microbes in their guts.

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Kepler spacecraft used by Smithsonian astronomers to find other earths

The Kepler spacecraft was launched in March of 2009 to study extrasolar planets. One of its major goals is the detection of terrestrial planets in habitable zones.

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Coral bleaching event caused by warming ocean waters is documented in Panama

Scientists and local dive operators first noticed coral bleaching in the waters surrounding Isla Colon, in Panama’s Bocas del Toro province in July. Smithsonian staff scientist Nancy Knowlton and colleagues documented an extensive bleaching event in late September.

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Yup’ik mask in “Infinity of Nations” exhibition at the American Indian Museum

This circa 1910 Yup'ik mask from Good News Bay, Alaska--made of driftwood, baleen, feathers, paint and cotton twine--is part of "Infinity of Nations: Art and History in the Collections of the National Museum of the American Indian," an exhibition at the National Museum of the American Indian, opening Saturday, Oct. 23.

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Rutgers glider added to the collections of the National Museum of Natural History

The Scarlet Knight, as the glider is called, made nautical history as the first submersible glider to successfully cross the Atlantic Ocean.

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Narwhal fluke design helps compensate for drag caused by tusk

The male’s fluke design helps it overcome the drag caused by their long tusks, the scientists determined. The female’s fluke design gives them increased speed for diving while foraging.

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Skeletal casts of early hominin ancestor from Africa donated to National Museum of Natural History

A. sediba was discovered in 2008 in the Malapa Cave at the Cradle of Humankind World Heritage Site located outside Johannesburg.

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Space shuttle Discovery to be added to National Air and Space Museum collection

Discovery, the longest-serving orbiter in the space shuttle fleet, will be accepted into the Smithsonian’s National Air and Space Museum collection. The space shuttle has been the icon for American spaceflight for a generation, and Discovery has flown every type of mission during its 27-year career.

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National Museum of Natural History’s coral collection used in Caribbean agricultural and sewage pollution study

A study published in the journal Global Change Biology finds that while fertilizer has been the dominant source of nitrogen pollution in Caribbean coastal ecosystems for the past 50 years, such pollution is on the decline, thanks in part to the introduction of more advanced, environmentally responsible agricultural practices during the last decade.

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American Indian Museum to host public broadcasts focusing on the Inka Road

The Smithsonian’s National Museum of the American Indian is hosting a series of public satellite broadcasts featuring a multinational team of researchers, engineers and archaeologists who are working in Peru on the origins and engineering of the Inka Road of South America.

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Earthquake causes minor damage to Smithsonian natural history collections

The 5.8-magnitude earthquake that shook the eastern United States on the afternoon of Tuesday, Aug. 23, caused minor damage to some of the Smithsonian's natural history collections. All public Smithsonian museums are open and have been determined safe for visitors and staff.

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New dinosaur species named from hatchling fossil donated to National Museum of Natural History

The fossil represents the youngest nodosaur ever discovered, and the only known specimen of a new genus and species of dinosaur that lived approximately 110 million years ago during the Early Cretaceous Era.

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Ability to raft with flotsam and use non-reef habitats helps tropical fish journey to new places, study finds

Depending on where the fish disperse from, the use of ‘stepping stones', flotsam or simply being an adult can help in the journey to find a new home.

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$35-million donation will build new dinosaur hall at National Museum of Natural History

The National Museum of Natural History will construct a new dinosaur exhibition hall made possible by a $35 million donation from David H. Koch, executive vice president of Koch Industries and philanthropist.

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Common tropical bat uses echolocation with precision previously considered impossible, new experiments reveal

Using echolocation alone the bats found, identified and captured insects perched motionless and silent on the leaves of plants.

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Gray whale specimen an important addition to Natural History Museum collections

Rope, golf balls, sweat pants, bottles and aluminum cans are a few of the discarded items biologist Matt Klope says he has found inside the […]

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Air and Space Museum receives $6 million donation for Public Observatory Program

The Smithsonian’s National Air and Space Museum announced that it will receive a $6 million donation from the Thomas W. Haas Foundation to establish an […]

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Smithsonian secretary on the future of museums, libraries and archives

To download the free e-book Best of Both Worlds: Museums, Libraries, and Archives in a Digital Age, by G. Wayne Clough, Secretary of the Smithsonian, […]

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Package-delivering drones? Q&A with Roger Connor of the National Air and Space Museum

Santa Claus and his sleigh full of gifts has been upstaged early this holiday season by news of autonomous drones possibly delivering packages to your […]

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Sprawl threatens water quality, climate protection, and land conservation in Massachusetts

A groundbreaking study by Harvard University’s Harvard Forest and the Smithsonian Conservation Biology Institute reveals that, if left unchecked, recent trends in the loss of […]

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Arthur C. Clarke papers come to Air and Space Museum Archives

The Smithsonian’s National Air and Space Museum has acquired a large collection from the Sir Arthur C. Clarke Trust. The collection consists of 87 cubic […]

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Video from Solar Dynamics Observatory wows museum visitors

Tucked in the shadow of the towering Skylab exhibit at the Smithsonian’s National Air and Space Museum, there’s an inferno raging. Lucky for all of […]

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Study reveals Agriculture and Fishing Cause Coral Reef Decline

Since researchers began surveys in the 1980s, coral reefs in the Caribbean have undergone widespread change following bleaching and disease epidemics that have reduced the […]

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Did mystery worms cause world’s first mass extinction?

Contrary to popular imagery, massive volcanic eruptions or an asteroid impact may not have been the cause of the world’s first mass extinction. Rather, some […]

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Bats Use Second Sense to Hunt Prey in Noisy Environments

Like many predators, the fringe-lipped bat primarily uses its hearing to find its prey, but with human-generated noise on the rise, scientists are examining how […]

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Trusted Sources: Why Museums and Libraries Are More Relevant Than Ever

Washington, D.C. is a city of symbols. The rites, rituals, and places that define Washington capture the aspirations of our nation and its citizens. Just […]

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Tool use by sea otters has little to do with genetic ties: Smithsonian study

Tool use by sea otters to break open well-armored food is not necessarily a family matter, according to a new study published this week by […]

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