The sexa­dentate ligand 1,1,1-tris­[(salicyl­idene­amino)­meth­yl]ethane has been reported numerous times in its triply deprotonated form coordinated to transition metals and lanthanides, yet it has been rarely employed with main-group elements, including in substituted forms. Its structures with gallium and indium are reported as solvates, namely, ({[(2,2-bis­{[(2-oxido­benzyl­idene)amino-κ2N,O]meth­yl}prop­yl)imino]­meth­yl}phenololato-κ2N,O)gallium(III) pyridine monosolvate, [Ga(C26H24N3O3)]·C5H5N, the aceto­nitrile 0.75-solvate, [Ga(C26H24N3O3)]·0.75C2H3N, and ({[(2,2-bis­{[(2-oxido­benzyl­idene)amino-κ2N,O]meth­yl}prop­yl)imino]­meth­yl}phenololato-κ2N,O)indium(III) di­chloro­methane monosolvate, [In(C26H24N3O3)]·CH2Cl2. All three metal complexes are pseudo-octa­hedral and each structure contains multiple weak C—H⋯O and/or C—H⋯N inter­molecular hydrogen-bonding inter­actions. The syntheses and additional characterization in the forms of melting points, high-resolution mass spectra, infra-red (IR) spectra, and 1H and 13C NMR spectra are also reported.

Single crystals of SrFe1.40V0.60O4, strontium tetra­oxidodi[ferrate(III)/vanad­ate(III)], have been obtained as a side product in the course of sinter experiments aimed at the synthesis of double perovskites in the system SrO–Fe2O3–V2O5. The crystal structure can be characterized by layers of six-membered rings of TO4-tetra­hedra (T: FeIII, VIII) perpendicular to [100]. Stacking of the layers along [100] results in a three-dimensional framework enclosing tunnel-like cavities in which SrII cations are incorporated for charge compensation. The sequence of directedness of up (U) and down (D) pointing vertices of neighboring tetra­hedra in a single six-membered ring is UUUDDD. The topology of the tetra­hedral framework belongs to the zeolite-type ABW.

In the title compound, C21H15N2+·C7H5O2−, 2-phenyl-1H-phenanthro[9,10-d]imidazole and benzoic acid form an ion pair complex. The system is consolidated by hydrogen bonds along with π–π inter­actions and N—H⋯π inter­actions between the constituent units. For a better understanding of the crystal structure and inter­molecular inter­actions, a Hirshfeld surface analysis was performed.

A furnace that covers the temperature range from room temperature up to 2000 K has been designed, built and implemented on the D2AM beamline at the ESRF. The QMAX furnace is devoted to the full exploration of the reciprocal hemispace located above the sample surface. It is well suited for symmetric and asymmetric 3D reciprocal space mapping. Owing to the hemispherical design of the furnace, 3D grazing-incidence small- and wide-angle scattering and diffraction measurements are possible. Inert and reactive experiments can be performed at atmospheric pressure under controlled gas flux. It is demonstrated that the QMAX furnace allows monitoring of structural phase transitions as well as microstructural evolution at the nanoscale, such as self-organization processes, crystal growth and strain relaxation. A time-resolved in situ oxidation experiment illustrates the capability to probe the high-temperature reactivity of materials.

The fully automatic processing of crystals of macromolecules has presented a unique opportunity to gather information on the samples that is not usually recorded. This has proved invaluable in improving sample-location, characterization and data-collection algorithms. After operating for four years, MASSIF-1 has now processed over 56 000 samples, gathering information at each stage, from the volume of the crystal to the unit-cell dimensions, the space group, the quality of the data collected and the reasoning behind the decisions made in data collection. This provides an unprecedented opportunity to analyse these data together, providing a detailed landscape of macromolecular crystals, intimate details of their contents and, importantly, how the two are related. The data show that mosaic spread is unrelated to the size or shape of crystals and demonstrate experimentally that diffraction intensities scale in proportion to crystal volume and molecular weight. It is also shown that crystal volume scales inversely with molecular weight. The results set the scene for the development of X-ray crystallography in a changing environment for structural biology.

100 kV is investigated as the operating voltage for single-particle electron cryomicroscopy (cryoEM). Reducing the electron energy from the current standard of 300 or 200 keV offers both cost savings and potentially improved imaging. The latter follows from recent measurements of radiation damage to biological specimens by high-energy electrons, which show that at lower energies there is an increased amount of information available per unit damage. For frozen hydrated specimens around 300 Å in thickness, the predicted optimal electron energy for imaging is 100 keV. Currently available electron cryomicroscopes in the 100–120 keV range are not optimized for cryoEM as they lack both the spatially coherent illumination needed for the high defocus used in cryoEM and imaging detectors optimized for 100 keV electrons. To demonstrate the potential of imaging at 100 kV, the voltage of a standard, commercial 200 kV field-emission gun (FEG) microscope was reduced to 100 kV and a side-entry cryoholder was used. As high-efficiency, large-area cameras are not currently available for 100 keV electrons, a commercial hybrid pixel camera designed for X-ray detection was attached to the camera chamber and was used for low-dose data collection. Using this configuration, five single-particle specimens were imaged: hepatitis B virus capsid, bacterial 70S ribosome, catalase, DNA protection during starvation protein and haemoglobin, ranging in size from 4.5 MDa to 64 kDa with corresponding diameters from 320 to 72 Å. These five data sets were used to reconstruct 3D structures with resolutions between 8.4 and 3.4 Å. Based on this work, the practical advantages and current technological limitations to single-particle cryoEM at 100 keV are considered. These results are also discussed in the context of future microscope development towards the goal of rapid, simple and widely available structure determination of any purified biological specimen.

A series of Co2−xRuxMnSi (x = 0, 0.25, 0.5, 0.75, 1) Heusler compounds were successfully synthesized. The heat-treatment conditions were crucial to make the materials form a single phase with a Heusler structure. With increasing Ru content, the half-metallic gap, lattice parameters and magnetization are continuously adjustable in a wide range. The Co2−xRuxMnSi (x = 0, 0.25) compounds are rigorous half-metals and show a T3 dependence of resistance at low temperature. The Co2−xRuxMnSi (x = 0.5, 0.75, 1) Heusler compounds are the nearly half-metallic materials and show a semiconductive dependence of resistance at low temperature. The experimental magnetization is consistent with that in theory and follows the Slater–Pauling rule. The Curie temperature is higher than 750 K for all Co2−xRuxMnSi Heusler compounds.

Recent improvements in direct electron detectors, microscope technology and software provided the stimulus for a `quantum leap' in the application of cryo-electron microscopy in structural biology, and many national and international centres have since been created in order to exploit this. Here, a new facility for cryo-electron microscopy focused on single-particle reconstruction of biological macromolecules that has been commissioned at the European Synchrotron Radiation Facility (ESRF) is presented. The facility is operated by a consortium of institutes co-located on the European Photon and Neutron Campus and is managed in a similar fashion to a synchrotron X-ray beamline. It has been open to the ESRF structural biology user community since November 2017 and will remain open during the 2019 ESRF–EBS shutdown.

The surface structure of fluoro­apatite (0001) (FAp0001) under quasi-dry and humid conditions has been probed with surface X-ray diffraction (SXRD). Lateral and perpendicular atomic relaxations corresponding to the FAp0001 termination before and after H2O exposure and the location of the adsorbed water molecules have been determined from experimental analysis of the crystal truncation rod (CTR) intensities. The surface under dry conditions exhibits a bulk termination with relaxations in the outermost atomic layers. The hydrated surface is formed by a disordered partially occupied H2O layer containing one water molecule (33% surface coverage) adsorbed at each of the three surface Ca atoms, and is coupled with one OH group randomly bonded to each of the three topmost P atoms with a 33% surface coverage.

ID30A-3 (or MASSIF-3) is a mini-focus (beam size 18 µm × 14 µm) highly intense (2.0 × 1013 photons s−1), fixed-energy (12.81 keV) beamline for macromolecular crystallography (MX) experiments at the European Synchrotron Radiation Facility (ESRF). MASSIF-3 is one of two fixed-energy beamlines sited on the first branch of the canted undulator setup on the ESRF ID30 port and is equipped with a MD2 micro-diffractometer, a Flex HCD sample changer, and an Eiger X 4M fast hybrid photon-counting detector. MASSIF-3 is recommended for collecting diffraction data from single small crystals (≤15 µm in one dimension) or for experiments using serial methods. The end-station has been in full user operation since December 2014, and here its current characteristics and capabilities are described.

Inelastic X-ray scattering is a powerful and versatile technique for studying lattice dynamics in materials of scientific and technological importance. In this article, the design and capabilities of the momentum-resolved high-energy-resolution inelastic X-ray spectrometer (HERIX) at beamline 30-ID of the Advanced Photon Source are reported. The instrument operates at 23.724 keV and has an energy resolution of 1.3–1.7 meV. It can accommodate momentum transfers of up to 72  nm−1, at a typical X-ray flux of 4.5 × 109 photons s−1 meV−1 at the sample. A suite of in situ sample environments are provided, including high pressure, static magnetic fields and uniaxial strains, all at high or cryogenic temperatures.

A tandem-double-slit optical system was constructed to evaluate the practical beam emittance of undulator radiation. The optical system was a combination of an upstream slit (S1) and downstream slit (S2) aligned on the optical axis with an appropriate separation. The intensity distribution after the double slits, I(x1, x2), was measured by scanning S1 and S2 in the horizontal direction. Coordinates having 1/sqrt e intensity were extracted from I(x1, x2), whose contour provided the standard deviation ellipse in the x1–x2 space. I(x1, x2) was converted to the corresponding distribution in the phase space, I(x1, x1'). The horizontal beam emittance was evaluated to be 3.1 nm rad, which was larger than the value of 2.4 nm rad estimated by using ray-tracing. It was found that the increase was mainly due to an increase in beam divergence rather than size.

A gas- and vapour-pressure control system synchronized with the continuous data acquisition of millisecond high-resolution powder diffraction measurements was developed to study structural change processes in gas storage and reaction materials such as metal organic framework compounds, zeolite and layered double hydroxide. The apparatus, which can be set up on beamline BL02B2 at SPring-8, mainly comprises a pressure control system of gases and vapour, a gas cell for a capillary sample, and six one-dimensional solid-state (MYTHEN) detectors. The pressure control system can be remotely controlled via developed software connected to a diffraction measurement system and can be operated in the closed gas and vapour line system. By using the temperature-control system on the sample, high-resolution powder diffraction data can be obtained under gas and vapour pressures ranging from 1 Pa to 130 kPa in temperatures ranging from 30 to 1473 K. This system enables one to perform automatic and high-throughput in situ X-ray powder diffraction experiments even at extremely low pressures. Furthermore, this developed system is useful for studying crystal structures during the adsorption/desorption processes, as acquired by millisecond and continuous powder diffraction measurements. The acquisition of diffraction data can be synchronized with the control of the pressure with a high frame rate of up to 100 Hz. In situ and time-resolved powder diffraction measurements are demonstrated for nanoporous Cu coordination polymer in various gas and vapour atmospheres.

The ePix10ka2M (ePix10k) is a new large area detector specifically developed for X-ray free-electron laser (XFEL) applications. The hybrid pixel detector was developed at SLAC to provide a hard X-ray area detector with a high dynamic range, running at the 120 Hz repetition rate of the Linac Coherent Light Source (LCLS). The ePix10k consists of 16 modules, each with 352 × 384 pixels of 100 µm × 100 µm distributed on four ASICs, resulting in a 2.16 megapixel detector, with a 16.5 cm × 16.5 cm active area and ∼80% coverage. The high dynamic range is achieved with three distinct gain settings (low, medium, high) as well as two auto-ranging modes (high-to-low and medium-to-low). Here the three fixed gain modes are evaluated. The resulting dynamic range (from single photon counting to 10000 photons pixel−1 pulse−1 at 8 keV) makes it suitable for a large number of different XFEL experiments. The ePix10k replaces the large CSPAD in operation since 2011. The dimensions of the two detectors are similar, making the upgrade from CSPAD to ePix10k straightforward for most setups, with the ePix10k improving on experimental performance. The SLAC-developed ePix cameras all utilize a similar platform, are tailored to target different experimental conditions and are designed to provide an upgrade path for future high-repetition-rate XFELs. Here the first measurements on this new ePix10k detector are presented and the performance under typical XFEL conditions evaluated during an LCLS X-ray diffuse scattering experiment measuring the 9.5 keV X-ray photons scattered from a thin liquid jet.

The program Mercury, developed at the Cambridge Crystallographic Data Centre, was originally designed primarily as a crystal structure visualization tool. Over the years the fields and scientific communities of chemical crystallography and crystal engineering have developed to require more advanced structural analysis software. Mercury has evolved alongside these scientific communities and is now a powerful analysis, design and prediction platform which goes a lot further than simple structure visualization.

Silicon nanowire-based sensors find many applications in micro- and nano-electromechanical systems, thanks to their unique characteristics of flexibility and strength that emerge at the nanoscale. This work is the first study of this class of micro- and nano-fabricated silicon-based structures adopting the scanning X-ray diffraction microscopy technique for mapping the in-plane crystalline strain (∊044) and tilt of a device which includes pillars with suspended nanowires on a substrate. It is shown how the micro- and nanostructures of this new type of nanowire system are influenced by critical steps of the fabrication process, such as electron-beam lithography and deep reactive ion etching. X-ray analysis performed on the 044 reflection shows a very low level of lattice strain (<0.00025 Δd/d) but a significant degree of lattice tilt (up to 0.214°). This work imparts new insights into the crystal structure of micro- and nanomaterial-based sensors, and their relationship with critical steps of the fabrication process.

Book review

Book review

Book review

This article presents the capability of the QMAX furnace, devoted to reciprocal space mapping through X-ray scattering at high temperature up to 2000 K.

The structure of the Pseudomonas aeruginosa T6SS PldB immunity protein PA5086 is reported at 1.9 Å resolution. Comparison of PA5086 with its homologs PA5087 and PA5088 showed great similarities in sequence and structure, but vast divergences in electrostatic potential surfaces.

The true identity of the protein found in the crystals reported by Bondoc et al. [(2019), Acta Cryst. F75, 646–651] is given.

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 […]

The post Smithsonian Scientist Discovers Two New Bat Species Hiding in Museum Collections for More Than 150 Years appeared first on Smithsonian Insider.

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

The post Hall of Human Origins to open at Smithsonian’s Natural History Museum, March 17, 2010 appeared first on Smithsonian Insider.

The stars move quickly because they are very close to each other, separated by only about one-fourth the distance from the Earth to the Moon. As a result, they share strong gravitational forces. They were once farther apart but have spiraled closer together over time. Billions of years from now, they will crash together and merge.

The post At 1,500,000 mph, twin stars in the constellation Cancer win speediest orbit award appeared first on Smithsonian Insider.

Long before dawn on a recent morning, Katie Milton and a group of stalwart volunteers, each armed with flashlight and compass, spread out into the jungle to take up positions at 35 listening stations marked on maps of the island.

The post Census reveals 1,200 howler monkeys living on Barro Colorado Island appeared first on Smithsonian Insider.

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.

The post Killing of methane-producing megafauna may have caused cooling 13,000 years ago appeared first on Smithsonian Insider.

Data from a recent study of wild takins in the high-altitude forests of the Tangjiahe National Nature Reserve in southeast China has shown that the […]

The post Great Sichuan earthquake of 2008 had little impact on of China’s wild takins appeared first on Smithsonian Insider.

Using the ancient magnetic field recorded in these rocks, a Smithsonian research group revealed Santa Marta’s 2,200-kilometer journey from northern Peru to its modern position on the Caribbean coast of Colombia during the past 170 million years.

The post Earth’s highest coastal mountain range moved 1,367 miles in 170 million years appeared first on Smithsonian Insider.

Snowflake Study through Photomicrography, 1890 Wilson A. Bentley became fascinated with the crystalline structure of individual snowflakes on his parent’s Vermont farm. By adapting a […]

The post Snowflake Study through Photomicrography, 1890 appeared first on Smithsonian Insider.

Tiny Antarctic marine creatures collected 100 years ago by British Royal Navy explorer Robert Falcon Scott are giving scientists new clues about polar environmental change.

The post Tiny creatures collected 100 years ago confirm accelerating carbon uptake in Antarctic Ocean appeared first on Smithsonian Insider.

Faced with insufficient time and inadequate library resources to tackle the problem on their own, they instead posted a catalog of specimen images to Facebook and turned to their network of colleagues for help.

The post Facebook friends help scientists quickly identify nearly 5,000 fish specimens collected in Guyana appeared first on Smithsonian Insider.

Giant squid eye, 2008 Giant squid have the largest eyes in the animal kingdom—at up to 10 inches in diameter, they are the size of […]

The post Giant squid eye, 2008 appeared first on Smithsonian Insider.

A remarkable 5,000-year-old deposit of bones representing an entire herd of Persian gazelles recently discovered in northeastern Syria is firm evidence, scientists say, of an ancient hunting practice largely responsible for the near extinction of gazelles in this region today.

The post Archaeological evidence confirms mass hunting of gazelles 5,000 years ago appeared first on Smithsonian Insider.

Collecting trips for Charles Doolittle Walcott (1850-1927), paleontologist and fourth Secretary of the Smithsonian Institution, were often a family affair. This 1910 photograph shows their […]

The post Charles Doolittle Walcott (1850-1927) family campsite in the Canadian Rockies appeared first on Smithsonian Insider.

Astronomers have discovered a new comet that they expect will be visible to the naked eye in early 2013.A preliminary orbit computed by the Minor Planet Center at the Smithsonian Astrophysical Observatory in Cambridge, Mass., shows that the comet will come within about 30 million miles of the sun in early 2013, about the same distance as Mercury. The comet will pose no danger to Earth.

The post New comet may be visible to the naked eye in 2013 appeared first on Smithsonian Insider.

Astronomers using NASA's Chandra X-ray Observatory discovered the first pair of supermassive black holes in a spiral galaxy similar to the Milky Way. Approximately 160 million light years from Earth, the pair is the nearest known such phenomenon.

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University of Florida and Smithsonian Tropical Research Institute scientists describe a new 20-foot extinct species of crocodile discovered in the same Colombian coal mine with Titanoboa, the world’s largest snake.

The post New 20-foot extinct species of crocodile discovered in Colombian coal mine appeared first on Smithsonian Insider.

In 2011, scholars from three institutions—National Museum of American History Curators Carlene Stephens and Shari Stout, Library of Congress Digital Conversion Specialist Peter Alyea and Lawrence Berkeley National Laboratory Scientists Carl Haber and Earl Cornell—came together in a newly designed preservation laboratory at the Library of Congress to recover sound from those recordings made more than 100 years ago.

The post Digital technology allows Alexander Graham Bell’s 1880s disc recordings to be played again appeared first on Smithsonian Insider.

An excavation at a site in South Africa has unearthed the 190-million-year-old dinosaur nesting site of the prosauropod dinosaur Massospondylus–revealing significant clues about the evolution of complex reproductive behavior in early dinosaurs.

The post 190-million-year-old dinosaur nesting site discovered in South Africa appeared first on Smithsonian Insider.

The fastest wind ever discovered blowing off a disk around a stellar-mass black hole has been observed by a team of astronomers using NASA’s Chandra X-ray Observatory.

The post Chandra X-ray Observatory clocks stellar wind at 20 million mph appeared first on Smithsonian Insider.

This composite image from the Chandra X-ray Observatory (operated for NASA by the Smithsonian Astrophysical Observatory) shows the distribution of dark matter, galaxies, and hot […]

The post Chandra image of the core of the merging galaxy cluster Abell 520 appeared first on Smithsonian Insider.

For the last 1,000 days the Infrared Array Camera, aboard NASA’s Spitzer Space Telescope, has been operating continuously to probe the universe from its most distant regions to our local solar neighborhood.

The post Top 10 gallery celebrates the Infrared Array Camera aboard the Spitzer Space Telescope appeared first on Smithsonian Insider.

To celebrate its 22nd anniversary in orbit, the Hubble Space Telescope has released a dramatic new image of the star-forming region 30 Doradus, also known […]

The post New image of the star-forming region 30 Doradus, also known as the Tarantula Nebula appeared first on Smithsonian Insider.

Scientists have discovered several specimens of tiny insects covered with pollen grains in two pieces of amber, revealing the first record of pollen transport and social behavior in this group of animals.

The post First ever record of insect pollination captured in 100 million-year-old amber appeared first on Smithsonian Insider.

To celebrate the 10th anniversary of researchers producing the first complete human genome sequence — the genetic blueprint of the human body — the Smithsonian’s National Museum of Natural History, will open a new high-tech, high-intensity exhibition in 2013.

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“The Age of Plastic: Ingenuity + Responsibility” a public Smithsonian Symposium that will take an uncommon look at the most common of materials. On Thursday, June […]

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