The crystal structure of title salt, C14H36N44+·2ClO4−·2Cl−, has been determined using synchrotron radiation at 220 K. The structure determination reveals that protonation has occurred at all four amine N atoms. The asymmetric unit contains one half-cation (completed by crystallographic inversion symmetry), one perchlorate anion and one chloride anion. A distortion of the perchlorate anion is due to its involvement in hydrogen-bonding inter­actions with the cations. The crystal structure is consolidated by inter­molecular hydrogen bonds involving the 1,4,8,11-tetra­methyl-1,4,8,11-tetra­azonia­cyclo­tetra­decane N—H and C—H groups as donor groups, and the O atoms of the perchlorate and chloride anion as acceptor groups, giving rise to a three-dimensional network.

The title compound, [Mn(S4)(C8H20N4)], was accidentally obtained by the hydro­thermal reaction of Mn(ClO4)2·6H2O, cyclen (cyclen = 1,4,7,10-tetra­aza­cyclo­dodeca­ne) and Na3SbS4·9H2O in water at 413 K, indicating that polysulfide anions might represent inter­mediates in the synthesis of thio­metallate compounds using Na3SbS4·9H2O as a reactant. X-ray powder diffraction proves that the sample is slightly contaminated with NaSb(OH)6 and an unknown crystalline phase. The crystal investigated was twinned with a twofold rotation axis as the twin element, and therefore a twin refinement using data in HKLF-5 format was performed. The asymmetric unit of the title compound consists of one MnII cation, one [S4]2− anion and one cyclen ligand in general positions. The MnII cation is sixfold coordinated by two cis-S atoms of the [S4]2− anions, as well as four N atoms of the cyclen ligand within an irregular coordination. The complexes are linked via pairs of N—H⋯S hydrogen bonds into chains, which are further linked into layers by additional N—H⋯S hydrogen bonding. These layers are connected into a three-dimensional network by inter­molecular N—H⋯S and C—H⋯S hydrogen bonding. It is noted that only one similar complex with MnII is reported in the literature.

The crystal structure of title compound, (C14H36N4)[CrO3Cl]2Cl2, has been determined by synchrotron radiation X-ray crystallography at 220 K. The macrocyclic cation lies across a crystallographic inversion center and hence the asymmetric unit contains one half of the organic cation, one chloro­chromate anion and one chloride anion. Both the Cl− anion and chloro­chromate Cl atom are involved in hydrogen bonding. In the crystal, hydrogen bonds involving the 1,4,8,11-tetra­methyl-1,4,8,11-tetra­azonia­cyclo­tetra­decane (TMC) N—H groups and C—H groups as donor groups and three O atoms of the chloro­chromate and the chloride anion as acceptor groups link the components, giving rise to a three-dimensional network.

The structure of the title compound, [CrCl2(C10H24N4)][Cr(HCONH2)2(C10H24N4)][ZnCl4]2 (C10H24N4 = 1,4,8,11-tetra­aza­cyclo­tetra­decane, cyclam; HCONH2 = formamide, fa), has been determined from synchrotron X-ray data. The asymmetric unit contains two independent halves of the [CrCl2(cyclam)]+ and [Cr(fa)(cyclam)]3+ cations, and one tetra­chlorido­zincate anion. In each complex cation, the CrIII ion is coordinated by the four N atoms of the cyclam ligand in the equatorial plane and two Cl ligands or two O-bonded formamide mol­ecules in a trans axial arrangement, displaying a distorted octa­hedral geometry with crystallographic inversion symmetry. The Cr—N(cyclam) bond lengths are in the range 2.061 (2) to 2.074 (2) Å, while the Cr—Cl and Cr—O(fa) bond distances are 2.3194 (7) and 1.9953 (19) Å, respectively. The macrocyclic cyclam moieties adopt the centrosymmetric trans-III conformation with six- and five-membered chelate rings in chair and gauche conformations. The crystal structure is stabilized by inter­molecular hydrogen bonds involving the NH or CH groups of cyclam and the NH2 group of coordinated formamide as donors, and Cl atoms of the ZnCl42− anion as acceptors.

Exact and approximate mathematical formulas of equatorial aberration for powder diffraction data collected with an Si strip X-ray detector in continuous-scan integration mode are presented. An approximate formula is applied to treat the experimental data measured with a commercial powder diffractometer.

Developing methods to determine high-resolution structures from micrometre- or even submicrometre-sized protein crystals has become increasingly important in recent years. This applies to both large protein complexes and membrane proteins, where protein production and the subsequent growth of large homogeneous crystals is often challenging, and to samples which yield only micro- or nanocrystals such as amyloid or viral polyhedrin proteins. The versatile macromolecular crystallography microfocus (VMXm) beamline at Diamond Light Source specializes in X-ray diffraction measurements from micro- and nanocrystals. Because of the possibility of measuring data from crystalline samples that approach the resolution limit of visible-light microscopy, the beamline design includes a scanning electron microscope (SEM) to visualize, locate and accurately centre crystals for X-ray diffraction experiments. To ensure that scanning electron microscopy is an appropriate method for sample visualization, tests were carried out to assess the effect of SEM radiation on diffraction quality. Cytoplasmic polyhedrosis virus polyhedrin protein crystals cryocooled on electron-microscopy grids were exposed to SEM radiation before X-ray diffraction data were collected. After processing the data with DIALS, no statistically significant difference in data quality was found between datasets collected from crystals exposed and not exposed to SEM radiation. This study supports the use of an SEM as a tool for the visualization of protein crystals and as an integrated visualization tool on the VMXm beamline.

Apoptosis is a crucial process by which multicellular organisms control tissue growth, removal and inflammation. Disruption of the normal apoptotic function is often observed in cancer, where cell death is avoided by the overexpression of anti-apoptotic proteins of the Bcl-2 (B-cell lymphoma 2) family, including Mcl-1 (myeloid cell leukaemia 1). This makes Mcl-1 a potential target for drug therapy, through which normal apoptosis may be restored by inhibiting the protective function of Mcl-1. Here, the discovery and biophysical properties of an anti-Mcl-1 antibody fragment are described and the utility of both the scFv and Fab are demonstrated in generating an Mcl-1 crystal system amenable to iterative structure-guided drug design.

In recent years, there have been numerous efforts worldwide to develop the synchrotron X-ray scanning tunneling microscopy (SX-STM) technique. Here, the inauguration of XTIP, the world's first beamline fully dedicated to SX-STM, is reported. The XTIP beamline is located at Sector 4 of the Advanced Photon Source at Argonne National Laboratory. It features an insertion device that can provide left- or right-circular as well as horizontal- and vertical-linear polarization. XTIP delivers monochromatic soft X-rays of between 400 and 1900 eV focused into an environmental enclosure that houses the endstation instrument. This article discusses the beamline system design and its performance.

Across all branches of science, medicine and engineering, high-resolution microscopy is required to understand functionality. Although optical methods have been developed to `defeat' the diffraction limit and produce 3D images, and electrons have proven ever more useful in creating pictures of small objects or thin sections, so far there is no substitute for X-ray microscopy in providing multiscale 3D images of objects with a single instrument and minimal labeling and preparation. A powerful technique proven to continuously access length scales from 10 nm to 10 µm is ptychographic X-ray computed tomography, which, on account of the orthogonality of the tomographic rotation axis to the illuminating beam, still has the limitation of necessitating pillar-shaped samples of small (ca 10 µm) diameter. Large-area planar samples are common in science and engineering, and it is therefore highly desirable to create an X-ray microscope that can examine such samples without the extraction of pillars. Computed laminography, where the axis of rotation is not perpendicular to the illumination direction, solves this problem. This entailed the development of a new instrument, LamNI, dedicated to high-resolution 3D scanning X-ray microscopy via hard X-ray ptychographic laminography. Scanning precision is achieved by a dedicated interferometry scheme and the instrument covers a scan range of 12 mm × 12 mm with a position stability of 2 nm and positioning errors below 5 nm. A new feature of LamNI is a pair of counter-rotating stages carrying the sample and interferometric mirrors, respectively.

Whole-mount (WM) platelet preparation followed by transmission electron microscopy (TEM) observation is the standard method currently used to assess dense granule (DG) deficiency (DGD). However, due to the electron-density-based contrast mechanism in TEM, other granules such as α-granules might cause false DG detection. Here, scanning transmission X-ray microscopy (STXM) was used to identify DGs and minimize false DG detection of human platelets. STXM image stacks of human platelets were collected at the calcium (Ca) L2,3 absorption edge and then converted to optical density maps. Ca distribution maps, obtained by subtracting the optical density maps at the pre-edge region from those at the post-edge region, were used to identify DGs based on the Ca richness. DGs were successfully detected using this STXM method without false detection, based on Ca maps for four human platelets. Spectral analysis of granules in human platelets confirmed that DGs contain a richer Ca content than other granules. The Ca distribution maps facilitated more effective DG identification than TEM which might falsely detect DGs. Correct identification of DGs would be important to assess the status of platelets and DG-related diseases. Therefore, this STXM method is proposed as a promising approach for better DG identification and diagnosis, as a complementary tool to the current WM TEM approach.

Time-resolved X-ray absorption spectroscopy (XAS) offers the possibility to monitor the state of materials during chemical reactions. While this technique has been established for transmission measurements for a number of years, XAS measurements in fluorescence mode are challenging because of limitations in signal collection as well as detectors. Nevertheless, measurements in fluorescence mode are often the only option to study complex materials containing heavy matrices or in samples where the element of interest is in low concentration. Here, it has been demonstrated that high-quality quick-scanning full extended X-ray absorption fine-structure data can be readily obtained with sub-second time resolution in fluorescence mode, even for highly diluted samples. It has also been demonstrated that in challenging samples, where transmission measurements are not feasible, quick fluorescence can yield significant insight in reaction kinetics. By studying the fast high-temperature oxidation of a reduced LaFe0.8Ni0.8O3 perovskite type, an example where the perovskite matrix elements prevent measurements in fluorescence, it is shown that it is now possible to follow the state of Ni in situ at a 3 s time resolution.

A scanning soft X-ray spectromicroscope was recently developed based mainly on the photon-in/photon-out measurement scheme for the investigation of local electronic structures on the surfaces and interfaces of advanced materials under conditions ranging from low vacuum to helium atmosphere. The apparatus was installed at the soft X-ray beamline (BL17SU) at SPring-8. The characteristic features of the apparatus are described in detail. The feasibility of this spectromicroscope was demonstrated using soft X-ray undulator radiation. Here, based on these results, element-specific two-dimensional mapping and micro-XAFS (X-ray absorption fine structure) measurements are reported, as well as the observation of magnetic domain structures from using a reference sample of permalloy micro-dot patterns fabricated on a silicon substrate, with modest spatial resolution (e.g. ∼500 nm). Then, the X-ray radiation dose for Nafion® near the fluorine K-edge is discussed as a typical example of material that is not radiation hardened against a focused X-ray beam, for near future experiments.

Two methods for reconstructing intragranular strain fields are developed for scanning three-dimensional X-ray diffraction (3DXRD). The methods are compared with a third approach where voxels are reconstructed independently of their neighbours [Hayashi, Setoyama & Seno (2017). Mater. Sci. Forum, 905, 157–164]. The 3D strain field of a tin grain, located within a sample of approximately 70 grains, is analysed and compared across reconstruction methods. Implicit assumptions of sub-problem independence, made in the independent voxel reconstruction method, are demonstrated to introduce bias and reduce reconstruction accuracy. It is verified that the two proposed methods remedy these problems by taking the spatial properties of the inverse problem into account. Improvements in reconstruction quality achieved by the two proposed methods are further supported by reconstructions using synthetic diffraction data.

Single-crystalline-like thin films composed of crystallographically aligned grains are a new prototype of 2D materials developed recently for low-cost and high-performance flexible electronics as well as second-generation high-temperature superconductors. In this work, significant texture improvement in single-crystalline-like materials is achieved through growth of a 330 nm-thick silver layer.

The distribution of plastic relaxation defects is studied using a nondestructive sub-micrometre X-ray diffraction scanning technique.

An attempt has been made to combine small-angle scattering of X-rays or neutrons with scanning electron microscopy in reciprocal space, in order to establish a structural analysis method covering a wide range of sizes from micro- to macro-scales.

Exact and approximate formulas for equatorial aberration of a continuous-scan Si strip detector are compared.

A detailed study on chiral compound structures found in the Cambridge Structural Database (CSD) is presented. Solvates, salts and co-crystals have intentionally been excluded, in order to focus on the most basic structures of single enantiomers, scalemates and racemates. Similarity between the latter and structures of achiral monomolecular compounds has been established and utilized to arrive at important conclusions about crystallization of chiral compounds. For example, the fundamental phenomenon of conglomerate formation and, in particular, their frequency of occurrence is addressed. In addition, rarely occurring kryptoracemates and scalemic compounds (anomalous racemates) are discussed. Finally, an extended search of enantiomer solid solutions in the CSD is performed to show that there are up to 1800 instances most probably hiding among the deposited crystal structures, while only a couple of dozen have been previously known and studied.

A study on chiral monomolecular compound structures found in the Cambridge Structural Database is presented.

The fossil teeth of a 15- to 18-million-year-old three-toed browsing horse, Anchitherium clarencei, were recently discovered by scientists from the Smithsonian Tropical Research Institute and the […]

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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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A Smithsonian Institution biologist, working with the Natural History Unit of the British Broadcasting Corp., has discovered a new species of giant rat on a film-making expedition to a remote rainforest in New Guinea.

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The spread of Africanized honey bees across Central America has had a much smaller impact on native tropical bee species than scientists previously predicted...

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In a series of ongoing experiments on Barro Colorado Island in the Panama Canal, Kays and other researchers are using camera traps, radio collars and palm nuts with tracking transmitters attached to them to take a closer look at the nut-hoarding strategies of the agouti.

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Recently, researchers from Boston University and the Smithsonian Tropical Research Institute in Panama have been taking a closer look at the vibrations that red-eyed treefrog embryos use as cues to trigger early hatching. They discovered that treefrog embryos can evaluate different features of vibrations.

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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.

Eric Silver of SAO is pursuing innovative and interdisciplinary uses of his technique for chemical imaging at the cellular level.

The post Technology developed for X-ray astronomy is being adapted to study cancer cells appeared first on Smithsonian Insider.

The Caddo people of Arkansas, Louisiana, Texas and Oklahoma have maintained many of their traditional ways and actively work to preserve their unique tribal cultural today. One example is the pottery of Jeri Redcorn.

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Now that astronomers are finding rocky worlds orbiting distant stars, they're asking the next logical questions: Do any of those worlds have volcanoes? And if so, could we detect them? Work by theorists at the Harvard-Smithsonian Center for Astrophysics suggests that the answer to the latter is a qualified "Yes."

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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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For two weeks the team recorded and documented the community’s elders, families and llamas along a pilgrimage of remembrance in Pisaq, Peru.

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Bats living in the dense urban area of Panama City, the scientists learned, represent just a small fraction of the roughly 25 species of high-flying insectivorous bats found in Panama’s rainforests.

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There is a new candidate for coldest known star: a brown dwarf with about the same temperature as a hot cup of coffee. That’s cool enough to begin crossing the blurry line between small cold stars and big hot planets.

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The new research reveals that from the period between 1100-1600 small agricultural settlements up and down the Delaware River Valley caused a 50-percent increase in sediment runoff into the Delaware River.

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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 […]

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A new genetic study by a team of Cuban and American researchers confirms that American crocodiles are hybridizing with wild populations of critically endangered Cuban crocodiles, which may cause a population decline of this species found only in the Cuban Archipelago.

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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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In a new paper appearing this week in Science, a group of biologists have shown that females themselves can also limit the evolution of increased elaboration.

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Using 2-dimensional and 3-dimensional CT scans, Natural History Museum anthropologists found that the brain and major organs were removed and rolls of linen filled out the abdominal cavity. This mummification method is evidence of superior embalming, indicating a person of higher status.

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A new study by a team of scientists from the Smithsonian’s National Museum of Natural History, the National University of Singapore and the Slovenian Academy of Sciences and Arts have unlocked the secret to mate binding in orb web spiders, and revealed just how it calms the cannibalistic female spider.

The post Suitor’s gentle massage soothes aggressive, cannibalistic female spiders, researchers find appeared first on Smithsonian Insider.

Halocoryza acapulcana Whitehead (Acapulco Saline Catarrh Beetle), described in 1966 by Donald R. Whitehead. This image is from a recent paper by Terry L. Erwin, […]

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Viewed from inside the SOMATOM Emotion 6CT scanner used at the Smithsonian’s National Museum of Natural History, the skeleton and internal organs of this well-preserved […]

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Smithsonian Secretary Wayne Clough, left, talks with Carlos Jaramillo, scientist at the Smithsonian Tropical Research Institute in Panama, at a research site near the Panama […]

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The discovery of two new extinct camel species by scientists from the University of Florida and the Smithsonian is casting new light on the history of the tropics, a region containing more than half the world's biodiversity and some of its most important ecosystems.

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A new video to help aviators identify the cause of bird strikes has been posted on YouTube by the U.S. Department of Agriculture's Wildlife Services Airport Wildlife Hazard Program and the Smithsonian's National Museum of Natural History.

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This image shows a 3-D scan of the type specimen of Odobenocetops, the walrus whale, in the Smithsonian’s National Museum of Natural History. The skull […]

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Hew research by astronomers at the Harvard-Smithsonian Center for Astrophysics shows that planets still can form in the cosmic maelstrom of Milky Way's center.

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The Smithsonian Astrophysical Observatory has been awarded a NASA project to build the Tropospheric Emissions: Monitoring of Pollution (TEMPO) instrument. TEMPO will measure North American air pollution, from Mexico City to the Canadian tar/oil sands, and from the Atlantic to the Pacific, hourly and at high spatial resolution.

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Frontispiece illustration of “flies” from the 1882 book American game fishes, their habits, habitat, and peculiarities; how, when, and where to angle for them, featuring […]

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