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Crystal structures of (η4-cyclo­octa-1,5-diene)bis(1,3-di­methyl­imidazol-2-yl­idene)iridium(I) iodide and (η4-cyclo­octa-1,5-diene)bis­(1,3-di­ethyl­imidazol-2-yl­idene)iridium(I) iodide

The title complexes, (η4-cyclo­octa-1,5-diene)bis­(1,3-di­methyl­imidazol-2-yl­idene)iridium(I) iodide, [Ir(C5H8N2)2(C8H12)]I, (1) and (η4-cyclo­octa-1,5-di­ene)bis­(1,3-di­ethyl­imidazol-2-yl­idene)iridium(I) iodide, [Ir(C7H12N2)2(C8H12)]I, (2), were prepared using a modified literature method. After carrying out the oxidative addition of the amino acid l-proline to [Ir(COD)(IMe)2]I in water and slowly cooling the reaction to room temperature, a suitable crystal of 1 was obtained and analyzed by single-crystal X-ray diffraction at 100 K. Although this crystal structure has previously been reported in the Pbam space group, it was highly disordered and precise atomic coordinates were not calculated. A single crystal of 2 was also obtained by heating the complex in water and letting it slowly cool to room temperature. Complex 1 was found to crystallize in the monoclinic space group C2/m, while 2 crystallizes in the ortho­rhom­bic space group Pccn, both with Z = 4.




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Crystal structure, Hirshfeld surface analysis and inter­action energy and DFT studies of 2-(2,3-di­hydro-1H-perimidin-2-yl)-6-meth­oxy­phenol

The title compound, C18H16N2O2, consists of perimidine and meth­oxy­phenol units, where the tricyclic perimidine unit contains a naphthalene ring system and a non-planar C4N2 ring adopting an envelope conformation with the NCN group hinged by 47.44 (7)° with respect to the best plane of the other five atoms. In the crystal, O—HPhnl⋯NPrmdn and N—HPrmdn⋯OPhnl (Phnl = phenol and Prmdn = perimidine) hydrogen bonds link the mol­ecules into infinite chains along the b-axis direction. Weak C—H⋯π inter­actions may further stabilize the crystal structure. The Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (49.0%), H⋯C/C⋯H (35.8%) and H⋯O/O⋯H (12.0%) inter­actions. Hydrogen bonding and van der Waals inter­actions are the dominant inter­actions in the crystal packing. Computational chemistry indicates that in the crystal, the O—HPhnl⋯NPrmdn and N—HPrmdn⋯OPhnl hydrogen-bond energies are 58.4 and 38.0 kJ mol−1, respectively. Density functional theory (DFT) optimized structures at the B3LYP/ 6–311 G(d,p) level are compared with the experimentally determined mol­ecular structure in the solid state. The HOMO–LUMO behaviour was elucidated to determine the energy gap.




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Crystal structure, Hirshfeld surface analysis and DFT studies of 6-bromo-3-(12-bromo­dodec­yl)-2-(4-nitro­phen­yl)-4H-imidazo[4,5-b]pyridine

The title compound, C24H30Br2N4O2, consists of a 2-(4-nitro­phen­yl)-4H-imidazo[4,5-b]pyridine entity with a 12-bromo­dodecyl substituent attached to the pyridine N atom. The middle eight-carbon portion of the side chain is planar to within 0.09 (1) Å and makes a dihedral angle of 21.9 (8)° with the mean plane of the imidazolo­pyridine moiety, giving the mol­ecule a V-shape. In the crystal, the imidazolo­pyridine units are associated through slipped π–π stacking inter­actions together with weak C—HPyr⋯ONtr and C—HBrmdc­yl⋯ONtr (Pyr = pyridine, Ntr = nitro and Brmdcyl = bromo­dodec­yl) hydrogen bonds. The 12-bromo­dodecyl chains overlap with each other between the stacks. The terminal –CH2Br group of the side chain shows disorder over two resolved sites in a 0.902 (3):0.098 (3) ratio. Hirshfeld surface analysis indicates that the most important contributions for the crystal packing are from H⋯H (48.1%), H⋯Br/Br⋯H (15.0%) and H⋯O/O⋯H (12.8%) inter­actions. The optimized mol­ecular structure, using density functional theory at the B3LYP/ 6–311 G(d,p) level, is compared with the experimentally determined structure in the solid state. The HOMO–LUMO behaviour was elucidated to determine the energy gap.




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Crystal structure and DFT computational studies of (E)-2,4-di-tert-butyl-6-{[3-(tri­fluoro­meth­yl)benz­yl]imino­meth­yl}phenol

The title compound, C23H28F3NO, is an ortho-hy­droxy Schiff base compound, which adopts the enol–imine tautomeric form in the solid state. The mol­ecular structure is not planar and the dihedral angle between the planes of the aromatic rings is 85.52 (10)°. The tri­fluoro­methyl group shows rotational disorder over two sites, with occupancies of 0.798 (6) and 0.202 (6). An intra­molecular O—H⋯N hydrogen bonding generates an S(6) ring motif. The crystal structure is consolidated by C—H⋯π inter­actions. The mol­ecular structure was optimized via density functional theory (DFT) methods with the B3LYP functional and LanL2DZ basis set. The theoretical structure is in good agreement with the experimental data. The frontier orbitals and mol­ecular electrostatic potential map were also examined by DFT computations.




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A thermal-gradient approach to variable-temperature measurements resolved in space

Temperature is a ubiquitous environmental variable used to explore materials structure, properties and reactivity. This article reports a new paradigm for variable-temperature measurements that varies the temperature continuously across a sample such that temperature is measured as a function of sample position and not time. The gradient approach offers advantages over conventional variable-temperature studies, in which temperature is scanned during a series measurement, in that it improves the efficiency with which a series of temperatures can be probed and it allows the sample evolution at multiple temperatures to be measured in parallel to resolve kinetic and thermodynamic effects. Applied to treat samples at a continuum of temperatures prior to measurements at ambient temperature, the gradient approach enables parametric studies of recovered systems, eliminating temperature-dependent structural and chemical variations to simplify interpretation of the data. The implementation of spatially resolved variable-temperature measurements presented here is based on a gradient-heater design that uses a 3D-printed ceramic template to guide the variable pitch of the wire in a resistively heated wire-wound heater element. The configuration of the gradient heater was refined on the basis of thermal modelling. Applications of the gradient heater to quantify thermal-expansion behaviour, to map metastable polymorphs recovered to ambient temperature, and to monitor the time- and temperature-dependent phase evolution in a complex solid-state reaction are demonstrated.




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On-chip crystallization for serial crystallography experiments and on-chip ligand-binding studies

Efficient and reliable sample delivery has remained one of the bottlenecks for serial crystallography experiments. Compared with other methods, fixed-target sample delivery offers the advantage of significantly reduced sample consumption and shorter data collection times owing to higher hit rates. Here, a new method of on-chip crystallization is reported which allows the efficient and reproducible growth of large numbers of protein crystals directly on micro-patterned silicon chips for in-situ serial crystallography experiments. Crystals are grown by sitting-drop vapor diffusion and previously established crystallization conditions can be directly applied. By reducing the number of crystal-handling steps, the method is particularly well suited for sensitive crystal systems. Excessive mother liquor can be efficiently removed from the crystals by blotting, and no sealing of the fixed-target sample holders is required to prevent the crystals from dehydrating. As a consequence, `naked' crystals are obtained on the chip, resulting in very low background scattering levels and making the crystals highly accessible for external manipulation such as the application of ligand solutions. Serial diffraction experiments carried out at cryogenic temperatures at a synchrotron and at room temperature at an X-ray free-electron laser yielded high-quality X-ray structures of the human membrane protein aquaporin 2 and two new ligand-bound structures of thermolysin and the human kinase DRAK2. The results highlight the applicability of the method for future high-throughput on-chip screening of pharmaceutical compounds.




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A cryo-EM grid preparation device for time-resolved structural studies

Structural biology generally provides static snapshots of protein conformations that can provide information on the functional mechanisms of biological systems. Time-resolved structural biology provides a means to visualize, at near-atomic resolution, the dynamic conformational changes that macromolecules undergo as they function. X-ray free-electron-laser technology has provided a powerful tool to study enzyme mechanisms at atomic resolution, typically in the femtosecond to picosecond timeframe. Complementary to this, recent advances in the resolution obtainable by electron microscopy and the broad range of samples that can be studied make it ideally suited to time-resolved approaches in the microsecond to millisecond timeframe to study large loop and domain motions in biomolecules. Here we describe a cryo-EM grid preparation device that permits rapid mixing, voltage-assisted spraying and vitrification of samples. It is shown that the device produces grids of sufficient ice quality to enable data collection from single grids that results in a sub-4 Å reconstruction. Rapid mixing can be achieved by blot-and-spray or mix-and-spray approaches with a delay of ∼10 ms, providing greater temporal resolution than previously reported mix-and-spray approaches.




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Polymorph evolution during crystal growth studied by 3D electron diffraction

3D electron diffraction (3DED) has been used to follow polymorph evolution in the crystallization of glycine from aqueous solution. The three polymorphs of glycine which exist under ambient conditions follow the stability order β < α < γ. The least stable β polymorph forms within the first 3 min, but this begins to yield the α-form after only 1 min more. Both structures could be determined from continuous rotation electron diffraction data collected in less than 20 s on crystals of thickness ∼100 nm. Even though the γ-form is thermodynamically the most stable polymorph, kinetics favour the α-form, which dominates after prolonged standing. In the same sample, some β and one crystallite of the γ polymorph were also observed.




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Small-angle neutron scattering studies suggest the mechanism of BinAB protein internalization

Small-angle neutron scattering (SANS) is one of the most widely used neutron-based approaches to study the solution structure of biological macromolecular systems. The selective deuterium labelling of different protein components of a complex provides a means to probe conformational changes in multiprotein complexes. The Lysinibacillus sphaericus mosquito-larvicidal BinAB proteins exert toxicity through interaction with the receptor Cqm1 protein; however, the nature of the complex is not known. Rationally engineered deuterated BinB (dBinB) protein from the L. sphaericus ISPC-8 species was synthesized using an Escherichia coli-based protein-expression system in M9 medium in D2O for `contrast-matched' SANS experiments. SANS data were independently analysed by ab initio indirect Fourier transform-based modelling and using crystal structures. These studies confirm the dimeric status of Cqm1 in 100% D2O with a longest intramolecular vector (Dmax) of ∼94 Å and a radius of gyration (Rg) of ∼31 Å. Notably, BinB binds to Cqm1, forming a heterodimeric complex (Dmax of ∼129 Å and Rg of ∼40 Å) and alters its oligomeric status from a dimer to a monomer, as confirmed by matched-out Cqm1–dBinB (Dmax of ∼70 Å and Rg of ∼22 Å). The present study thus provides the first insight into the events involved in the internalization of larvicidal proteins, likely by raft-dependent endocytosis.




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Li-ion half-cells studied operando during cycling by small-angle neutron scattering

Small-angle neutron scattering (SANS) was recently applied to the in situ and operando study of the charge/discharge process in Li-ion battery full-cells based on a pouch cell design. Here, this work is continued in a half-cell with a graphite electrode cycled versus a metallic lithium counter electrode, in a study conducted on the SANS-1 instrument of the neutron source FRM II at the Heinz Maier-Leibnitz Zentrum in Garching, Germany. It is confirmed that the SANS integrated intensity signal varies as a function of graphite lithiation, and this variation can be explained by changes in the squared difference in scattering length density between graphite and the electrolyte. The scattering contrast change upon graphite lithiation/delithiation calculated from a multi-phase neutron scattering model is in good agreement with the experimentally measured values. Due to the finite coherence length, the observed SANS contrast, which mostly stems from scattering between the (lithiated) graphite and the electrolyte phase, contains local information on the mesoscopic scale, which allows the development of lithiated phases in the graphite to be followed. The shape of the SANS signal curve can be explained by a core–shell model with step-wise (de)lithiation from the surface. Here, for the first time, X-ray diffraction, SANS and theory are combined to give a full picture of graphite lithiation in a half-cell. The goal of this contribution is to confirm the correlation between the integrated SANS data obtained during operando measurements of an Li-ion half-cell and the electrochemical processes of lithiation/delithiation in micro-scaled graphite particles. For a deeper understanding of this correlation, modelling and experimental data for SANS and results from X-ray diffraction were taken into account.




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A thermal-gradient approach to variable-temperature measurements resolved in space

A new approach to variable-temperature measurements is presented, where the sample temperature changes continuously as a function of position.




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At 1,500,000 mph, twin stars in the constellation Cancer win speediest orbit award

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.




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Ancient gray whales may have been homebodies

A new study suggests that the annual long-distance migration of gray whales may be a relatively recent phenomenon, and that only a few thousand years ago, these marine mammals stayed much closer to home.

The post Ancient gray whales may have been homebodies appeared first on Smithsonian Insider.




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JoGayle Howard, National Zoological Park pioneer in reproductive biology, dies

For more than three decades JoGayle Howard dedicated her life and work to reproducing endangered species.

The post JoGayle Howard, National Zoological Park pioneer in reproductive biology, dies appeared first on Smithsonian Insider.




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Varied diet has allowed gray whales to survive millions of years, study reveals

Gray whales survived many cycles of global cooling and warming over the past few million years, likely by exploiting a more varied diet than they do today, according to a new study by University of California, Berkeley, and Smithsonian Institution paleontologists.

The post Varied diet has allowed gray whales to survive millions of years, study reveals appeared first on Smithsonian Insider.




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Urban songbirds adjust melodies to adapt to life in the big city, Smithsonian scientists find

For the first time, researchers from the Smithsonian Conservation Biology Institute’s Migratory Bird Center analyzed how songbirds are affected by both general noise and the acoustics of hard human-made surfaces in urban areas.

The post Urban songbirds adjust melodies to adapt to life in the big city, Smithsonian scientists find appeared first on Smithsonian Insider.




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Steady diet of binary star partners makes black holes grow “supermassive”

A new study by astrophysicists at the University of Utah and the Smithsonian Astrophysical Observatory in Cambridge, Mass., has found a new explanation for the growth of supermassive black holes: they repeatedly capture and swallow single stars from pairs of stars that get too close.

The post Steady diet of binary star partners makes black holes grow “supermassive” appeared first on Smithsonian Insider.




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As robins disperse, West Nile mosquitoes switch diet to humans: Q&A with Smithsonian ornithologist Peter Marra

A rising spike in West Nile virus is taking health officials across the country by surprise as this year more than 2,600 people in 45 states and the District of Columbia, have been stricken with severe symptoms of this mosquito-transmitted disease.

The post As robins disperse, West Nile mosquitoes switch diet to humans: Q&A with Smithsonian ornithologist Peter Marra appeared first on Smithsonian Insider.






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Yellow pigment in penguin feathers is chemically distinct, spectroscopic studies reveal

Recent spectroscopic analysis of macaroni penguin (Eudyptes chrysolophus) crest feathers and king penguin (Aptenodytes patagonicus) neck feathers have shown they contain a yellow pigment that […]

The post Yellow pigment in penguin feathers is chemically distinct, spectroscopic studies reveal appeared first on Smithsonian Insider.




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Scientists shine light on world’s least-studied bat: Mortlock Islands flying fox

The Mortlock Islands flying fox, a large, breadfruit-eating bat native to a few remote and tiny Pacific islands, has long been regarded as one of […]

The post Scientists shine light on world’s least-studied bat: Mortlock Islands flying fox appeared first on Smithsonian Insider.




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Discovery: Australia’s invasive cane toads modify their bodies to conquer new territory faster

In 1935, 101 cane toads from Hawaii were set loose in Australia to help control beetles that were decimating the Australian sugar crop. But instead […]

The post Discovery: Australia’s invasive cane toads modify their bodies to conquer new territory faster appeared first on Smithsonian Insider.




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What does candied, microwaved sperm have to do with saving endangered species?

Today’s cutting-edge laboratories rely on ultra-cold refrigeration to keep delicate cells like sperm viable for use in the future. But a new technique using microwaves […]

The post What does candied, microwaved sperm have to do with saving endangered species? appeared first on Smithsonian Insider.



  • Animals
  • Research News
  • Science & Nature
  • Smithsonian Conservation Biology Institute
  • Smithsonian's National Zoo

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Study of bacteria inside guts of wild Canada geese shows greater danger than earlier studies exposed

In the early 20th century, Canada geese were considered endangered in the U.S. So in the 1950s and 1960s, birds from the Midwest were released […]

The post Study of bacteria inside guts of wild Canada geese shows greater danger than earlier studies exposed appeared first on Smithsonian Insider.




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XGANDALF – extended gradient descent algorithm for lattice finding

Serial crystallography records still diffraction patterns from single, randomly oriented crystals, then merges data from hundreds or thousands of them to form a complete data set. To process the data, the diffraction patterns must first be indexed, equivalent to determining the orientation of each crystal. A novel automatic indexing algorithm is presented, which in tests usually gives significantly higher indexing rates than alternative programs currently available for this task. The algorithm does not require prior knowledge of the lattice parameters but can make use of that information if provided, and also allows indexing of diffraction patterns generated by several crystals in the beam. Cases with a small number of Bragg spots per pattern appear to particularly benefit from the new approach. The algorithm has been implemented and optimized for fast execution, making it suitable for real-time feedback during serial crystallography experiments. It is implemented in an open-source C++ library and distributed under the LGPLv3 licence. An interface to it has been added to the CrystFEL software suite.




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X-ray interference fringes from a weakly bent plane-parallel crystal with negative strain gradient

Under the anomalous transmission condition in the Bragg mode, X-ray interference fringes were observed between two beams with different hyperbolic trajectories in a very weakly bent plane-parallel perfect crystal with negative strain gradient. The origin of the fringes was analysed based on the dynamical theory of diffraction for a distorted crystal. In the reflected beam from the entrance surface, the interference fringes were observed between once- and twice-reflected beams from the back surface. In the transmitted beam from the back surface, the interference fringes were observed between the direct beam and once-reflected beam from the entrance surface. In the emitted beam from the lateral surface, the interference fringes were observed between the beams after different numbers of reflections in the crystal. The multiply reflected beams were formed by a combined result of long propagation length along the beam direction with large divergence of the refracted beams when the strain gradient was negative. The period of these interference fringes was sensitive to very weak strain, of the order of 10−7.







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Conrad Labandiera, Smithsonian palentologist, studies fossils to learn how insects got along before flowering plants arrived

The post Conrad Labandiera, Smithsonian palentologist, studies fossils to learn how insects got along before flowering plants arrived appeared first on Smithsonian Insider.




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Meet our Scientist Rachel Page. She studies frog-eating bats, and other animals, in Panama

Meet Rachel Page, a Smithsonian scientist in Panama who studies frog-eating bats (fringe-lipped bats), among other topics. Her current research focuses on learning and memory in neotropical bats, combining field studies with laboratory experiments to learn about predator cognition and its effects on the evolution of their prey.

The post Meet our Scientist Rachel Page. She studies frog-eating bats, and other animals, in Panama appeared first on Smithsonian Insider.




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Beautiful Japan: Benten Festival 1917-1918, from the Smithsonian’s Human Studies Film Archive

This film is from the collections of the Human Studies Film Archives, Smithsonian Institution. Clip from silent film, Beautiful Japan (1917-18), by travel-lecturer Benjamin Brodsky. Benten Festival is celebrated on Shiraishi Island. Benten (Benzaiten) is the Goddess of the Sea and one of the Seven Lucky Gods of Japan.

The post Beautiful Japan: Benten Festival 1917-1918, from the Smithsonian’s Human Studies Film Archive appeared first on Smithsonian Insider.




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Construction of Mount Rushmore National Memorial from the Smithsonian’s Human Studies Film Archives

Clip from silent edited film "Bryson Jones Travelogue: Lure of the West" (ca. 1927) shows Mount Rushmore National Memorial under construction, including blasting off cliff face, scaffolding, men working, and the completed monument.

The post Construction of Mount Rushmore National Memorial from the Smithsonian’s Human Studies Film Archives appeared first on Smithsonian Insider.




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Geisha Hairstyling, ca. 1927, a silent black & white archival film clip from the Smithsonian’s Human Studies Film Archives

Silent black & white archival film clip from "Japan: Promotional and Theatrical Footage, ca. 1927". The full film, which is 17 minutes long, includes segments from what are believed to be a theatrical film, a promotional film and, possibly, amateur film - all of unknown origin.

The post Geisha Hairstyling, ca. 1927, a silent black & white archival film clip from the Smithsonian’s Human Studies Film Archives appeared first on Smithsonian Insider.




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Quarry carvings by American WWI soldiers

The French-German border is littered with as many as 500 underground sites used during World War I. Researcher Jeff Gusky explores them and finds a […]

The post Quarry carvings by American WWI soldiers appeared first on Smithsonian Insider.



  • Art
  • History & Culture
  • Video
  • National Air and Space Museum

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Medieval book is important resource for how plants were once collected, treated and used

Latinus 9333 is the Latin translation of the so-called Tacuinum sanitatis, a medieval handbook on wellness written in Arabic by the 11th-century physician ibn Butlan. It deals with factors influencing human health: from the air, the environment and food, to physical exercise and sexual activity.

The post Medieval book is important resource for how plants were once collected, treated and used appeared first on Smithsonian Insider.




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Starch grains found on Neandertal teeth debunks theory that dietary deficiencies caused their extinction

The discovery of starch granules in the calculus on Neandertal teeth provides direct evidence that they made sophisticated, thoughtful food choices and ate more nutrient-rich plants, for example date palms, legumes and grains such as barley.

The post Starch grains found on Neandertal teeth debunks theory that dietary deficiencies caused their extinction appeared first on Smithsonian Insider.




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Sugar is key ingredient to evolutionary success of ants, researchers find

One way to avoid a cold or the flu, doctors say, is to stay away from crowded places. Viruses spread fast in places where people […]

The post Sugar is key ingredient to evolutionary success of ants, researchers find appeared first on Smithsonian Insider.




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3D study of teeth in modern mammals opens window to extinct animal diets

By charting the slopes and crags on animals’ teeth as if they were mountain ranges, scientists at the Smithsonian’s National Museum of Natural History have […]

The post 3D study of teeth in modern mammals opens window to extinct animal diets appeared first on Smithsonian Insider.




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Crystal structure, Hirshfeld surface analysis and DFT studies of 2-(2,3-di­hydro-1H-perimidin-2-yl)phenol

The asymmetric unit of the title compound contains two independent mol­ecules, consisting of perimidine and phenol units, which are linked through an N—H⋯O hydrogen bond. Intra­molecular O—H⋯N hydrogen bonds are observed in both independent mol­ecules.




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Crystal structure and Hirshfeld surface analysis of 1,3-diethynyladamantane

The title compound exhibits exceptionally weak inter­molecular C—H⋯π hydrogen bonding of the ethynyl groups, with the corresponding H⋯π separations [2.91 (2) and 3.12 (2) Å] exceeding normal vdW distances. This bonding compliments distal contacts of the CH (aliphatic)⋯π type [H⋯π = 3.12 (2)–3.14 (2) Å] to sustain supra­molecular layers.




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Co-crystal structure, Hirshfeld surface analysis and DFT studies of 3,4-ethyl­ene­dioxy­thio­phene solvated bis­[1,3-bis­(penta­fluoro­phen­yl)propane-1,3-dionato]copper(II)

The title complex, Cu(L)2 or [Cu(C15HF10O2)2], comprising one copper ion and two fully fluorinated ligands (L−), was crystallized with 3,4-ethyl­ene­dioxy­thio­phene (EDOT, C6H6O2S) as a guest mol­ecule to give in a di­chloro­methane solution a unique co-crystal, Cu(L)2·3C6H6O2S.




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Crystal structure and Hirshfeld surface analysis of 1,3-diethynyladamantane

The title compound, C14H16, exhibits exceptionally weak intermolecular C—H...π hydrogen bonding of the ethynyl groups, with the corresponding H...π separations [2.91 (2) and 3.12 (2) Å] exceeding normal vdW distances. This bonding complements distal contacts of the CH (aliphatic)...π type [H...π = 3.12 (2)–3.14 (2) Å] to sustain supramolecular layers. Hirshfeld surface analysis of the title compound suggests a relatively limited significance of the C...H/H...C contacts to the crystal packing (24.6%) and a major contribution from H...H contacts accounting 74.9% to the entire surface.




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Crystal structure, Hirshfeld surface analysis and DFT studies of 2-(2,3-dihydro-1H-perimidin-2-yl)phenol

The asymmetric unit of the title compound, C17H14N2O, contains two independent molecules each consisting of perimidine and phenol units. The tricyclic perimidine units contain naphthalene ring systems and non-planar C4N2 rings adopting envelope conformations with the C atoms of the NCN groups hinged by 44.11 (7) and 48.50 (6)° with respect to the best planes of the other five atoms. Intramolecular O—H...N hydrogen bonds may help to consolidate the molecular conformations. The two independent molecules are linked through an N—H...O hydrogen bond. The Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H...H (52.9%) and H...C/C...H (39.5%) interactions. Hydrogen bonding and van der Waals interactions are the dominant interactions in the crystal packing. Density functional theory (DFT) optimized structures at the B3LYP/ 6–311 G(d,p) level are compared with the experimentally determined molecular structure in the solid state. The HOMO–LUMO behaviour was elucidated to determine the energy gap.




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Synthesis, decom­position studies and crystal structure of a three-dimensional CuCN network structure with protonated N-methyl­ethano­lamine as the guest cation

The com­pound poly[2-hy­droxy-N-methyl­ethan-1-aminium [μ3-cyanido-κ3C:C:N-di-μ-cyanido-κ4C:N-dicuprate(I)]], {(C3H10NO)[Cu2(CN)3]}n or [meoenH]Cu2(CN)3, crystallizes in the tetra­gonal space group P43. The structure consists of a three-dimensional (3D) anionic CuICN network with noncoordinated protonated N-methyl­ethano­lamine cations providing charge neutrality. Pairs of cuprophilic Cu atoms are bridged by the C atoms of μ3-cyanide ligands, which link these units into a 43 spiral along the c axis. The spirals are linked together into a 3D anionic network by the two other cyanide groups. The cationic moieties are linked into their own 43 spiral via N—H⋯O and O—H⋯O hydrogen bonds, and the cations inter­act with the 3D network via an unusual pair of N—H⋯N hydrogen bonds to one of the μ2-cyanide groups. Thermogravimetric analysis indicates an initial loss of the base cation and one cyanide as HCN at temperatures in the range 130–250 °C to form CuCN. We show how loss of a specific cyanide group from the 3D CuCN structure could form the linear CuCN structure. Further heating leaves a residue of elemental copper, isolated as the oxide.




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'Lost in Space' robot designer Robert Kinoshita dies at 100

Video of the B9 robot from "Lost In Space" and his most famous catchphrases.; Credit: timtomp (via YouTube)

Mike Roe

Robert Kinoshita, the Los Angeles native who designed the iconic robots from "Lost in Space" and "Forbidden Planet," has passed away. He was 100 years old.

Konishita died Dec. 9 at a Torrance nursing home, according to the Hollywood Reporter, citing family friend Mike Clark. His creations included "Forbidden Planet's" Robby the Robot, the B9 robot from "Lost in Space," Tobor from "Tobor the Great" and more. Kinoshita also created "Lost in Space's" iconic flying-saucer-shaped Jupiter 2 spaceship.

Kinoshita built the original miniature prototype of Robby the Robot out of wood and plastic by combining several different concepts, according to the Reporter; the Rafu Shimpo reported that he struggled with the design.

"I thought, what the hell. We’re wasting so much time designing and drawing one sketch after another. I said to myself, I’m going to make a model," Kinoshita told the Rafu Shimpo in a 2004 interview. "Then one day, the art director sees the model. He says, ‘Give me that thing.’ He grabbed it and ran. ... Ten minutes later, he comes running back and puts the model back on my desk and says, ‘Draw it!’"

Watch Kinoshita and his colleagues talking about the construction of Robby the Robot:

Robby the Robot's construction

The 1956 classic sci-fi movie "Forbidden Planet" — based on Shakespeare's "The Tempest" — went on to be nominated for a special effects Oscar.

Kinoshita later served as art director on the 1960s sci-fi TV series "Lost in Space," creating the arm-flailing robot — named B9 — who delivered the classic line "Danger! Danger, Will Robinson!" That robot received as much fan mail as the actual humans on the show, according to the Reporter.

Watch the robot's feud with "Lost in Space's" Dr. Smith:

The robot vs. Dr. Smith

The "Lost in Space" robot even inspired a B9 Robot Builders Club, featured in Forbes. Kinoshita sent a message in 2000 to the club, thanking them for their support for the robot he originally nicknamed "Blinky."

"I'm truly flabbergasted and honored by your support for 'Blinky!' It's a well-designed little beauty," Kinoshita wrote. "Your thoughtful remembrance is something we designers seldom are lucky enough to receive."

Kinoshita described the thought process behind its design in a 1998 interview.

"You're laying in bed, and something comes to you," he said. "Until, finally, you get to a point where you say, 'This could work,' 'OK, let's see what the boss man says.' And you present it to him."

He told the Rafu Shimpo that he tried to create his robots to disguise the fact that there was a person inside. "I tried to camouflage it enough so you’d wonder where the hell the human was," he said.

Both the Japanese-American Kinoshita and his wife, Lillian, were sent to an Arizona internment camp during World War II, though they were able to get out before the end of the war and moved to Wisconsin, according to the Reporter.

While in Wisconsin, Kinoshita learned industrial design and plastic fabrication, designing washing machines for the Army and Air Force before returning to California, according to the Rafu Shimpo.

Kinoshita said that he had to overcome racial prejudice to break into working in Hollywood.

Kinoshita attributed his long life to clean living — along with daily doses of apple cider vinegar, family friend Clark told the Reporter.

Kinoshita also worked as a designer and art director on numerous classic TV shows, including "Kojak," "Barnaby Jones," "Hawaii Five-O," "Bat Masterson," "Sea Hunt," "Tombstone Territory," "Star Trek" creator Gene Roddenberry's "Planet Earth" and more, according to his IMDB. His last TV show was 1984's "Cover Up."

Kinoshita grew up in Boyle Heights, according to the Reporter, attending Maryknoll Japanese Catholic School, Roosevelt High School and USC's School of Architecture. His career began with work on 1937's "100 Men and a Girl." Kinoshita graduated cum laude from USC, according to the Rafu Shimpo.

Watch Kinoshita speak at his 95th birthday gathering with the B9 Robot Builders Club. He said he hoped to make it to 100, and he ended up doing so.

Kinoshita's 95th birthday speech

This content is from Southern California Public Radio. View the original story at SCPR.org.




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Los Angeles comedian, 'Parks & Recreation' writer Harris Wittels, 30, dies in possible drug overdose

File: (L-R) "The Sarah Silverman Program" writer Harris Wittels, comedian Sarah Silverman, executive producer/head writer Dan Sterling and actress Laura Silverman, arrive at Comedy Central's Emmy Awards party at the STK restaurant Sept. 21, 2008 in Los Angeles.; Credit: Ethan Miller/Getty Images

Mike Roe with Jennifer Velez

Harris Wittels, a comedy writer who worked on "Parks & Recreation," has died at 30, the Los Angeles Police Department's Jane Kim tells KPCC.

Wittels was discovered by his assistant around 12 p.m., Kim said, and was already dead. Kim said that Wittels' death was a possible overdose, but that the Coroner's Office would determine the cause of death. Wittels had attended drug rehab twice.

Comedy Central, where Wittels worked on "The Sarah Silverman Program" and "Secret Girlfriend," confirmed Wittels' death, as did the comedy show he appeared at Wednesday night.

Comedy Central tweet

Meltdown Show tweet

Wittels was also well known for his @Humblebrag Twitter account and later book, helping to popularize the idea online of the false modesty of bragging while trying not to look like you're bragging.

Wittels had spoken about his struggles with addiction in places including Pete Holmes's podcast "You Made It Weird" in a November episode.

"I just really stopped caring about my life," Wittels said on "You Made It Weird," explaining how he got into doing drugs. "I just really started to think, well, if I'm only here for 80 years, then who cares if I spend it high or not?"

Wittels received his first big break when Sarah Silverman saw him performing comedy and gave him a job writing for her Comedy Central show.

Wittels also wrote for HBO's "Eastbound & Down," several MTV awards shows and the American Music Awards. He had a recurring role on "Parks & Recreation" and was a regular guest on the "Comedy Bang Bang" podcast.

Comedians, actors and fans mourned Wittels' death online.

Harris Wittels Storify

See Wittels in a scene from "Parks & Recreation":

Wittels on Parks & Recreation

Listen to Wittels on "Comedy Bang Bang":

Wittels on Comedy Bang Bang

This story has been updated.

This content is from Southern California Public Radio. View the original story at SCPR.org.




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WWE looks to springboard from Wrestlemania 31 into new audiences

Brock Lesnar after losing his championship in the main event of Wrestlemania 31.; Credit: WWE

Mike Roe

World Wrestling Entertainment held their annual Wrestlemania show last weekend in Northern California, the culmination of another year's worth of spectacle. According to the company, it was their highest grossing event of all-time, drawing $12.6 million, with an official attendance placing it fifth on their list of all-time crowds for the event. The show was headlined by former UFC Heavyweight Champion Brock Lesnar going up against up-and-coming star (and a relative of Dwayne "The Rock" Johnson) Roman Reigns.

WWE Network

It comes at a time when the company has embarked on a new way of making money: their over-the-top online programming provider, the WWE Network, where fans can pay $9.99 a month to see programming including what formerly used to cost $45 for most shows and $60 for Wrestlemania. They're one year in now on gambling that enough fans will want the Network that it will ultimately make them more money in the long-term, despite losing that pay-per-view revenue. Wall Street doesn't appear to be buying it — after announcing the day after Wrestlemania that they'd hit 1.3 million subscribers, WWE's stock took a significant loss.

"The point is not whether it's real or if it's staged. The point is, are you entertained by it, or not?" former WWE announcer Jim Ross told KPCC in an interview. WWE is looking for more fans to be entertained enough to plunk down $9.99 for all the pro wrestling content they want.

NXT

They're also in a transitional period with their audiences. They've launched a new show that's only on the Network called "NXT," turning their minor league into a program targeting hardcore pro wrestling fans with a different style of show than the more family-targeted "Raw" and "Smackdown." It's also where they groom potential future stars, many of whom seem to break the mold of some of the traditional stars on WWE's main roster.

They're signing up talent that's been getting buzz on the independent circuits, trying to create their own underground movement that hopefully spells money, and taking the NXT brand on tour for the first time. On the Raw after Wrestlemania, several NXT stars made their debut on the main roster. That follows a sell-out crowd (albeit at a smaller 5,000 seat venue) on the Friday night before Wrestlemania for a non-televised NXT show.

Give Divas a chance

WWE also faces cultural forces pushing them in new directions, including a difference in how society deals with gender. When WWE executive Stephanie McMahon, daughter of the famed Vince McMahon, tweeted in support of Patricia Arquette's speech calling for greater equality for women at the Academy Awards, one of their own wrestlers, AJ Lee, responded by publicly calling Stephanie McMahon out on Twitter for not promoting the women in her own company equally and paying them less than the male stars.

AJ tweet 1

AJ tweet 2

Of course, the women in the company aren't given the same prominence as the men in part because it's felt that they won't make the company as much money. Still, it forced WWE's hand and Stephanie McMahon and the company as a whole publicly embraced the idea of giving the women (who WWE brands as "divas") a chance with the Give Divas A Chance movement (and accompanying trending hashtag).

What's next

The women have been promoted nearly equal to the men in that underground NXT league, but only time will tell if it continues to trickle upward. Wrestlemania didn't seem to show huge promise of that happening, with the one women's match of the show only getting a few minutes in the ring. However, the show also included a high-profile storyline with UFC female fighter and champion Ronda Rousey alongside the Rock, going up against Stephanie McMahon and Triple H, so there appears to be the room for women in prominent positions when they have the right storyline.

Whether WWE is able to wade through these forces of change to make more money — and perhaps regain some of the cultural currency that they've lost since becoming a monopoly and purchasing their top competition in 2001 — remains to be seen. They've stayed relatively steady despite a challenge from UFC, which many see as being what pro wrestling would be like if WWE didn't present fictional  They'll have to hope that giving new stars, including "divas," a chance will take them to another level.

This content is from Southern California Public Radio. View the original story at SCPR.org.




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#Chemsafety at #ACSSanDiego

Here’s what’s planned for chemical and laboratory safety at the ACS National Meeting in San Diego, which starts on Sunday. You can also take advantage of the Division of Chemical Health & Safety’s printer-friendly CHAS-At-A-Glance. Sunday, Aug. 25 Committee on Chemical Safety Open and Executive Subcommittee Meeting, 7:00–10:00 am, Marriott Marquis San Diego Marina, Marina […]

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