In the title complex, [Ni(C19H13N5)2](CF3SO3)2·(CH3CH2)2O, the central NiII atom is sixfold coordinated by three nitro­gen atoms of each 2,6-bis­(2-benzimidazol­yl)pyridine ligand in a distorted octa­hedral geometry with two tri­fluoro­methane­sulfonate ions and a mol­ecule of diethyl ether completing the outer coordination sphere of the complex. Hydrogen bonding contributes to the organization of the asymmetric units in columns along the a axis generating a porous supra­molecular structure. The structure was refined as a two-component twin with a refined BASF value of 0.4104 (13).

The structure of the title compound, [C14H18N2)2Ag2](NO3)2, contains subtle differences in ligand, metal, and counter-anion coordination. One quinoxaline ligand uses one of its quinoxaline N atoms to bond to one silver cation. That silver cation is bound to a second quinoxaline which, in turn, is bound to a second silver atom; thereby using both of its quinoxaline N atoms. A nitrate group bonds with one of its O atoms to the first silver and uses the same oxygen to bond to a silver atom (related by symmetry to the second), thereby forming an extended network. The second nitrate group on the other silver bonds via two nitrate O atoms; one silver cation therefore has a coordination number of three whereas the second has a coordination number of four. One of the quinoxaline ligands has a disordered ethyl group.

The title compound, [Ru(C19H13N5)2](PF6)2·3C4H10O, was obtained from the reaction of Ru(bimpy)Cl3 [bimpy is 2,6-bis­(1H-benzimidazol-2-yl)pyridine] and bimpy in refluxing ethanol followed by recrystallization from diethyl ether/aceto­nitrile. At 125 K the complex has ortho­rhom­bic (Pca21) symmetry. It is remarkable that the structure is almost centrosymmetric. However, refinement in space group Pbcn leads to disorder and definitely worse results. It is of inter­est with respect to potential catalytic reduction of CO2. The structure displays N—H⋯O, N—H⋯F hydrogen bonding and significant π–π stacking and C—H⋯π stacking inter­actions.

The title compound, [Ir(C8H12)(C8H15N3)(C18H15P)]BF4, a new triazole-based N-heterocyclic carbene iridium(I) cationic complex with a tetra­fluorido­borate counter-anion, crystallizes with two cations and two anions in the asymmetric unit of space group Pc. The Ir centers of the cations have distorted square-planar conformations, formed by a bidentate (η2 + η2) cyclo­octa-1,5-diene (COD) ligand, an N-heterocyclic carbene and a tri­phenyl­phosphane ligand with the NHC carbon atom and P atom being cis. In the extended structure, non-classical C–H⋯F hydrogen bonds, one of which is notably short (H⋯F = 2.21 Å), link the cations and anions. The carbon atoms of one of the COD ligands are disordered over adjacent sites in a 0.62:0.38 ratio.

A new neutral triazole-based N-heterocyclic carbene rhodium(I) complex [RhCl(C8H12)(C8H15N3)], has been synthesized and structurally characterized. The complex crystallizes with two mol­ecules in the asymmetric unit. The central rhodium(I) atom has a distorted square-planar coordination environment, formed by a cyclo­octa-1,5-diene (COD) ligand, an N-heterocyclic carbene (NHC) ligand, and a chlorido ligand. The bond lengths are unexceptional. A weak inter­molecular non-standard hydrogen-bonding inter­action exists between the chlorido and NHC ligands.

A new, cationic N-heterocyclic carbene RhI complex with a tetra­fluorido­borate counter-anion, [Rh(C8H12)(C8H15N3)(C18H15P)]BF4, has been synthesized and structurally characterized. There are two independent ion pairs in the asymmetric unit. Each complex cation exhibits a distorted square-planar conformation around the RhI atom. Bond lengths and bond angles are as expected for an Rh–NHC complex. There are several close, non-standard C—H⋯F hydrogen-bonding inter­actions between the ions. One of the tetra­fluorido­borate anions shows statistical disorder of the F atoms.

A new triazole-based N-heterocyclic carbene IrI cationic complex with a tetra­fluorido­borate counter-anion and hemi-solvating di­chloro­methane, [Ir(C8H12)(C8H15N3)(C18H15P)]BF4·0.5CH2Cl2, has been synthesized and structurally characterized. There are two independent ion pairs in the asymmetric unit and one di­chloro­methane solvent mol­ecule per two ion pairs. The cationic complex exhibits a distorted square-planar conformation around the IrI atom, formed by a bidentate cyclo­octa-1,5,diene (COD) ligand, a tri­phenyl­phosphane ligand, and an N-heterocyclic carbene (NHC). There are several close non-standard H⋯F hydrogen-bonding inter­actions that orient the tetra­fluorido­borate anions with respect to the IrI complex mol­ecules. The complex shows promising catalytic activity in transfer hydrogenation reactions. The structure was refined as a non-merohedral twin, and one of the COD mol­ecules is statistically disordered.

The crystal structure of a new 1:1 cocrystal of carbamazepine and S-naproxen (C15H12N2O·C14H14O3) was solved from powder X-ray diffraction (PXRD). The PXRD pattern was measured at the high-resolution beamline CRISTAL at synchrotron SOLEIL (France). The structure was solved using Monte Carlo simulated annealing, then refined with Rietveld refinement. The positions of the H atoms were obtained from density functional theory (DFT) ground-state calculations. The symmetry is ortho­rhom­bic with the space group P212121 (No. 19) and the following lattice parameters: a = 33.5486 (9), b = 26.4223 (6), c = 5.3651 (10) Å and V = 4755.83 (19) Å3.

The receptor ability of diethyl N,N'-(1,3-phenyl­ene)dicarbamate (1) to form host–guest com­plexes with theophylline (TEO) and caffeine (CAF) by mechanochemistry was evaluated. The formation of the 1–TEO com­plex (C12H16N2O4·C7H8N4O2) was preferred and involves the conformational change of one of the ethyl carbamate groups of 1 from the endo conformation to the exo conformation to allow the formation of inter­molecular inter­actions. The formation of an N—H⋯O=C hydrogen bond between 1 and TEO triggers the conformational change of 1. CAF mol­ecules are unable to form an N—H⋯O=C hydrogen bond with 1, making the conformational change and, therefore, the formation of the com­plex impossible. Conformational change and selective binding were monitored by IR spectroscopy, solid-state 13C nuclear magnetic resonance and single-crystal X-ray diffraction. The 1–TEO com­plex was characterized by IR spectroscopy, solid-state 13C nuclear magnetic resonance, powder X-ray diffraction and single-crystal X-ray diffraction.

In this study, we report the results of continuous rotation electron diffraction studies of single DyPO4·nH2O (rhabdophane) nanocrystals. The diffraction patterns can be fit to a trigonal lattice (P3121) with lattice parameters a = 7.019 (5) and c = 6.417 (5) Å. However, there is also a set of diffuse background scattering features present that are associated with a disordered superstructure that is double these lattice parameters and fits with an arrangement of water mol­ecules present in the structure pore. Pair distribution function (PDF) maps based on the diffuse background allowed the extent of the water correlation to be estimated, with 2–3 nm correlation along the c axis and ∼5 nm along the a/b axis.

Single-particle cryo-electron microscopy has become a widely adopted method in structural biology due to many recent technological advances in microscopes, detectors and image processing. Before being able to inspect a biological sample in an electron microscope, it needs to be deposited in a thin layer on a grid and rapidly frozen. The VitroJet was designed with this aim, as well as avoiding the delicate manual handling and transfer steps that occur during the conventional grid-preparation process. Since its creation, numerous technical developments have resulted in a device that is now widely utilized in multiple laboratories worldwide. It features plasma treatment, low-volume sample deposition through pin printing, optical ice-thickness measurement and cryofixation of pre-clipped Autogrids through jet vitrification. This paper presents recent technical improvements to the VitroJet and the benefits that it brings to the cryo-EM workflow. A wide variety of applications are shown: membrane proteins, nucleosomes, fatty-acid synthase, Tobacco mosaic virus, lipid nanoparticles, tick-borne encephalitis viruses and bacteriophages. These case studies illustrate the advancement of the VitroJet into an instrument that enables accurate control and reproducibility, demonstrating its suitability for time-efficient cryo-EM structure determination.

The Mycobacterium tuberculosis trifunctional enzyme (MtTFE) is an α2β2 tetrameric enzyme in which the α-chain harbors the 2E-enoyl-CoA hydratase (ECH) and 3S-hydroxyacyl-CoA dehydrogenase (HAD) active sites, and the β-chain provides the 3-ketoacyl-CoA thiolase (KAT) active site. Linear, medium-chain and long-chain 2E-enoyl-CoA molecules are the preferred substrates of MtTFE. Previous crystallographic binding and modeling studies identified binding sites for the acyl-CoA substrates at the three active sites, as well as the NAD binding pocket at the HAD active site. These studies also identified three additional CoA binding sites on the surface of MtTFE that are different from the active sites. It has been proposed that one of these additional sites could be of functional relevance for the substrate channeling (by surface crawling) of reaction intermediates between the three active sites. Here, 226 fragments were screened in a crystallographic fragment-binding study of MtTFE crystals, resulting in the structures of 16 MtTFE–fragment complexes. Analysis of the 121 fragment-binding events shows that the ECH active site is the `binding hotspot' for the tested fragments, with 41 binding events. The mode of binding of the fragments bound at the active sites provides additional insight into how the long-chain acyl moiety of the substrates can be accommodated at their proposed binding pockets. In addition, the 20 fragment-binding events between the active sites identify potential transient binding sites of reaction intermediates relevant to the possible channeling of substrates between these active sites. These results provide a basis for further studies to understand the functional relevance of the latter binding sites and to identify substrates for which channeling is crucial.

β-Glucosidase from the thermophilic bacterium Caldicellulosiruptor saccharo­lyticus (Bgl1) has been denoted as having an attractive catalytic profile for various industrial applications. Bgl1 catalyses the final step of in the decomposition of cellulose, an unbranched glucose polymer that has attracted the attention of researchers in recent years as it is the most abundant renewable source of reduced carbon in the biosphere. With the aim of enhancing the thermostability of Bgl1 for a broad spectrum of biotechnological processes, it has been subjected to structural studies. Crystal structures of Bgl1 and its complex with glucose were determined at 1.47 and 1.95 Å resolution, respectively. Bgl1 is a member of glycosyl hydrolase family 1 (GH1 superfamily, EC 3.2.1.21) and the results showed that the 3D structure of Bgl1 follows the overall architecture of the GH1 family, with a classical (β/α)8 TIM-barrel fold. Comparisons of Bgl1 with sequence or structural homologues of β-glucosidase reveal quite similar structures but also unique structural features in Bgl1 with plausible functional roles.

Single-crystal X-ray diffraction analysis of small molecule active pharmaceutical ingredients is a key technique in the confirmation of molecular connectivity, including absolute stereochemistry, as well as the solid-state form. However, accessing single crystals suitable for X-ray diffraction analysis of an active pharmaceutical ingredient can be experimentally laborious, especially considering the potential for multiple solid-state forms (solvates, hydrates and polymorphs). In recent years, methods for the exploration of experimental crystallization space of small molecules have undergone a `step-change', resulting in new high-throughput techniques becoming available. Here, the application of high-throughput encapsulated nanodroplet crystallization to a series of six di­hydro­pyridines, calcium channel blockers used in the treatment of hypertension related diseases, is described. This approach allowed 288 individual crystallization experiments to be performed in parallel on each molecule, resulting in rapid access to crystals and subsequent crystal structures for all six di­hydro­pyridines, as well as revealing a new solvate polymorph of nifedipine (1,4-dioxane solvate) and the first known solvate of nimodipine (DMSO solvate). This work further demonstrates the power of modern high-throughput crystallization methods in the exploration of the solid-state landscape of active pharmaceutical ingredients to facilitate crystal form discovery and structural analysis by single-crystal X-ray diffraction.

In the title compound, C18H22O7, two hexane rings and an oxane ring are fused together. The two hexane rings tend toward a distorted boat conformation, while the tetra­hydro­furan and di­hydro­furan rings adopt envelope conformations. The oxane ring is puckered. The crystal structure features C—H⋯O hydrogen bonds, which link the mol­ecules into a three-dimensional network. According to a Hirshfeld surface study, H⋯H (60.3%) and O⋯H/H⋯O (35.3%) inter­actions are the most significant contributors to the crystal packing.

In the title benzyl­ideneaniline Schiff base, C18H22N2O, the aromatic rings are inclined to each other by 46.01 (6)°, while the Car—N= C—Car torsion angle is 176.9 (1)°. In the crystal, the only identifiable directional inter­action is a weak C—H⋯π hydrogen bond, which generates inversion dimers that stack along the a-axis direction.

The asymmetric unit of the title compound, 2C31H28N2O4S·C2H6O, contains a parent mol­ecule and a half mol­ecule of ethanol solvent. The main compound stabilizes its mol­ecular conformation by forming a ring with an R12(7) motif with the ethanol solvent mol­ecule. In the crystal, mol­ecules are connected by C—H⋯O and O—H⋯O hydrogen bonds, forming a three-dimensional network. In addition, C—H⋯π inter­actions also strengthen the mol­ecular packing.

The asymmetric unit of the title compound, C25H18N6·H2O, comproses two mol­ecules (I and II), together with a water mol­ecule. The terminal phenyl groups attached to the methyl groups of the mol­ecules I and II do not overlap completely, but are approximately perpendicular. In the crystal, the mol­ecules are connected by N—H⋯N, C—H⋯N, O—H⋯N and N—H⋯O hydrogen bonds with each other directly and through water mol­ecules, forming layers parallel to the (001) plane. C—H⋯π inter­actions between these layers ensure the cohesion of the crystal structure. A Hirshfeld surface analysis indicates that H⋯H (39.1% for mol­ecule I; 40.0% for mol­ecule II), C⋯H/H⋯C (26.6% for mol­ecule I and 25.8% for mol­ecule II) and N⋯H/H⋯N (24.3% for mol­ecules I and II) inter­actions are the most important contributors to the crystal packing.

The title compound, C12H10N2O3, was obtained by the de­acetyl­ation reaction of 1-(6-amino-5-nitro­naphthalen-2-yl)ethanone in a concentrated sulfuric acid methanol solution. The mol­ecule comprises a naphthalene ring system bearing an acetyl group (C-3), an amino group (C-7), and a nitro group (C-8). In the crystal, the mol­ecules are assembled into a two-dimensional network by N⋯H/H⋯N and O⋯H/H⋯O hydrogen-bonding inter­actions. n–π and π–π stacking inter­actions are the dominant inter­actions in the three-dimensional crystal packing. Hirshfeld surface analysis indicates that the most important contributions are from O⋯H/H⋯O (34.9%), H⋯H (33.7%), and C⋯H/H⋯C (11.0%) contacts. The energies of the frontier mol­ecular orbitals were computed using density functional theory (DFT) calculations at the B3LYP-D3BJ/def2-TZVP level of theory and the LUMO–HOMO energy gap of the mol­ecule is 3.765 eV.

The synthesis, crystal structure, and a Hirshfeld surface analysis of tris­{N,N-diethyl-N'-[(4-nitro­phen­yl)(oxo)meth­yl]carbamimido­thio­ato}cobalt(III) conducted at 180 K are presented. The complex consists of three N,N-diethyl-N'-[(4-nitro­benzene)(oxo)meth­yl]carbamimido­thio­ato ligands, threefold sym­metric­ally bonded about the CoIII ion, in approximately octa­hedral coordination, which generates a triple of individually near planar metallacyclic (Co—S—C—N—C—O) rings. The overall geometry of the complex is determined by the mutual orientation of each metallacycle about the crystallographically imposed threefold axis [dihedral angles = 81.70 (2)°] and by the dihedral angles between the various planar groups within each asymmetric unit [metallacycle to benzene ring = 13.83 (7)°; benzene ring to nitro group = 17.494 (8)°]. The complexes stack in anti-parallel columns about the overline{3} axis of the space group (Poverline{3}), generating solvent-accessible channels along [001]. These channels contain ill-defined, multiply disordered, partial-occupancy solvent. Atom–atom contacts in the crystal packing predominantly (∼96%) involve hydrogen, the most abundant types being H⋯H (36.6%), H⋯O (31.0%), H⋯C (19.2%), H⋯N (4.8%), and H⋯S (4.4%).

The mol­ecular structure of tricarbon­yl[η4-6-exo-(tri­phenyl­phosphino)cyclo­hepta-2,4-dien-1-one]iron(0) tetra­fluoro­borate di­chloro­methane hemisolvate, [Fe(C28H22O4)(CO)3]BF4·0.5CH2Cl2, as determined by single-crystal X-ray diffraction is reported. The two independent tricarbon­yl[η4-6-exo-(tri­phenyl­phosphino)cyclo­hepta-2,4-dien-1-one] iron(0) cations and their corresponding anions form dimers, which constitute the asymmetric unit of the structure parallel to the (100) plane. Solid-state stability within that asymmetric unit as well as between neighboring dimeric units is afforded by C—H⋯O and C—H⋯F hydrogen bonds and C—H⋯π and Y—X⋯π (Y = B, C; X = F, O) inter­actions, which yield diperiodic sheets and a three-dimensional extended network.

Reaction of thorium(IV) nitrate with 2-[(4-phenyl-1H-1,2,3-triazol-1-yl)meth­yl]pyridine (L) yielded (LH)2[Th(NO3)6] or (C14H13N4)2[Th(NO3)6] (1), instead of the expected mixed-ligand complex [Th(NO3)4L2], which was detected in the mass spectrum of 1. In the structure, the [Th(NO3)6]2− anions display an icosa­hedral coordination geometry and are connected by LH+ cations through C—H⋯O hydrogen bonds. The LH+ cations inter­act via N—H⋯N hydrogen bonds. Hirshfeld surface analysis indicates that the most important inter­actions are O⋯H/H⋯O hydrogen-bonding inter­actions, which represent a 55.2% contribution.

The crystal structures of two inter­mediates, 4-amino-3,5-di­fluoro­benzo­nitrile, C7H4F2N2 (I), and ethyl 4-amino-3,5-di­fluoro­benzoate, C9H9F2NO2 (II), along with a visible-light-responsive azo­benzene derivative, diethyl 4,4'-(diazene-1,2-di­yl)bis­(3,5-di­fluoro­benzoate), C18H14F4N2O4 (III), obtained by four-step synthetic procedure, were studied using single-crystal X-ray diffraction. The mol­ecules of I and II demonstrate the quinoid character of phenyl rings accompanied by the distortion of bond angles related to the presence of fluorine substituents in the 3 and 5 (ortho) positions. In the crystals of I and II, the mol­ecules are connected by N—H⋯N, N—H⋯F and N—H⋯O hydrogen bonds, C—H⋯F short contacts, and π-stacking inter­actions. In crystal of III, only stacking inter­actions between the mol­ecules are found.

The dinuclear mol­ecule of the title compound, [Mo2(C9H13)2(CO)6] or [Mo(tBuCp)(CO)3]2 where tBu and Cp are tert-butyl and cyclo­penta­dienyl, is centrosymmetric and is characterized by an Mo—Mo bond length of 3.2323 (3) Å. Imposed by inversion symmetry, the tBuCp and the carbonyl ligands are in a transoid arrangement to each other. In the crystal, inter­molecular C—H⋯O contacts lead to the formation of layers parallel to the bc plane.

The title compound, bis­[μ-2,2'-(4H-1,2,4-triazole-3,5-di­yl)di­acetato]­bis­[di­aqua­copper(II)] dihydrate, [Cu2(C6H5N3O4)2(H2O)4]·2H2O, is a dinuclear octa­hedral CuII triazole-based complex. The central copper atoms are hexa-coordinated by two nitro­gen atoms in the equatorial positions, two equatorial oxygen atoms of two carboxyl­ate substituents in position 3 and 5 of the 1,2,4-triazole ring, and two axial oxygen atoms of two water mol­ecules. Two additional solvent water mol­ecules are linked to the title mol­ecule by O—H⋯N and O⋯H—O hydrogen bonds. The crystal structure is built up from the parallel packing of discrete supra­molecular chains running along the a-axis direction. Hirshfeld surface analysis suggests that the most important contributions to the surface contacts are from H⋯O/O⋯H (53.5%), H⋯H (28.1%), O⋯O (6.3%) and H⋯C/C⋯H (6.2%) inter­actions. The crystal studied was twinned by a twofold rotation around [100].

In the title compound, C33H29ClN2O2, the two piperidine rings of the di­aza­bicyclo moiety adopt distorted-chair conformations. Inter­molecular C—H⋯π inter­actions are mainly responsible for the crystal packing. The inter­molecular inter­actions were qu­anti­fied and analysed using Hirshfeld surface analysis, revealing that H⋯H inter­actions contribute most to the crystal packing (52.3%). The mol­ecular structure was further optimized by density functional theory (DFT) at the B3LYP/6–31 G(d,p) level and is compared with the experimentally determined mol­ecular structure in the solid state.

The two mol­ecules in the asymmetric unit of the title compound, C23H24N2O2S, have a structural overlap with an r.m.s. deviation of 0.82 Å. The piperidine rings adopt a distorted boat conformation. Intra- and inter­molecular C—H⋯O hydrogen bonds are responsible for the cohesion of the crystal packing. The inter­molecular inter­actions were qu­anti­fied and analysed using Hirshfeld surface analysis. The mol­ecular structure optimized by density functional theory (DFT) at the B3LYP/6–311++G(d,p)level is compared with the experimentally determined mol­ecular structure in the solid state.

When reacted in dry, degassed toluene, [Ir(COD)Cl]2 (COD = cyclo­octa-1,5-diene) and 2 equivalents of 2-(di-tert-butyl­phosphinito)anthra­quinone (tBuPOAQH) were found to form a unique tri-iridium compound consisting of one monoanionic dinuclear tri-μ-chlorido complex bearing one bidentate tBuPOAQ ligand per iridium, which was charge-balanced by an outer sphere [Ir(toluene)(COD)]+ ion, the structure of which has not previously been reported. This product, which is a toluene solvate, namely, (η2:η2-cyclo­octa-1,5-diene)(η6-toluene)­iridium(I) tri-μ-chlorido-bis­({3-[(di-tert-butyl­phosphan­yl)­oxy]-9,10-dioxoanthracen-2-yl}hydridoiridium(III)) toluene monosolvate, [Ir(C7H8)(C8H12)][Ir2H2(C22H24O3P)2Cl3]·C7H8 or [Ir(toluene)(COD)][Ir(κ-P,C-tBuPOAQ)(H)]2(μ-Cl)3]·toluene, formed as small orange platelets at room temperature, crystallizing in the triclinic space group Poverline{1}. The cation and anion are linked via weak C—H⋯O inter­actions. The stronger inter­molecular attractions are likely the offset parallel π–π inter­actions, which occur between the toluene ligands of pairs of inverted cations and between pairs of inverted anthra­quinone moieties, the latter of which are capped by toluene solvate mol­ecules, making for π-stacks of four mol­ecules each. The related ligand, 2-(di-tert-butyl­phosphinometh­yl)-anthra­quinone (tBuPCAQH), did not form crystals suitable for X-ray diffraction under analogous reaction conditions. However, when the reaction was conducted in chloro­form, yellow needles readily formed following addition of 1 atm of carbon monoxide. Diffraction studies revealed a neutral, dinuclear, di-μ-chlorido complex, di-μ-chlorido-bis­(carbon­yl{3-[(di-tert-butyl­phosphan­yl)­oxy]-9,10-dioxoanthracen-2-yl}hydridoiridium(I)), [Ir2H2(C23H26O2P)2Cl2(CO)2] or [Ir(κ-P,C-tBuPCAQ)(H)(CO)(μ-Cl)]2, Ir2C48H54Cl2O6P2, again crystallizing in space group Poverline{1}. Offset parallel π–π inter­actions between anthra­quinone groups of adjacent mol­ecules link the mol­ecules in one dimension.

In the title compound, C25H17NO3, the torsion angle associated with the phenyl benzoate group is −173.7 (2)° and that for the benz­yloxy group is −174.8 (2)° establishing an anti-type conformation. The dihedral angles between the ten-membered cyanona­phthalene ring and the aromatic ring of the phenyl benzoate and the benz­yloxy fragments are 40.70 (10) and 87.51 (11)°, respectively, whereas the dihedral angle between the aromatic phenyl benzoate and the benz­yloxy fragments is 72.30 (13)°. In the crystal, the mol­ecules are linked by weak C—H⋯O inter­actions forming S(4) chains propagating parallel to [010]. The packing is consolidated by three C—H⋯π inter­actions and two π–π stacking inter­actions between the aromatic rings of naphthalene and phenyl benzoate with centroid-to-centroid distances of 3.9698 (15) and 3.8568 (15) Å, respectively. Inter­molecular inter­actions were qu­anti­fied using Hirshfeld surface analysis. The mol­ecular structure was further optimized by density functional theory (DFT) at the B3LYP/6–311+ G(d,p) level, revealing that the energy gap between HOMO and LUMO is 3.17 eV. Mol­ecular docking studies were carried out for the title compound as a ligand and SARS-Covid-2(PDB ID:7QF0) protein as a receptor giving a binding affinity of −9.5 kcal mol−1.

Time-resolved high-energy X-ray diffraction was used during growth of ultrathin NixFe3−xO4 films with varying Ni content (0 ≤ x ≤ 1.5) deposited on MgO(001) substrates by reactive molecular beam epitaxy, providing an insight into the growth dynamics of these films. In order to obtain structural information, reciprocal-space maps were recorded and the temporal evolution of the Bragg peaks specific to the octahedral and tetrahedral lattice sites of the inverse spinel structure of NixFe3−xO4 was observed during growth of the films. A time delay, corresponding to a coverage of 1.2–1.8 nm, between the appearance of the Bragg reflections originating from octahedral sites and reflections originating exclusively from tetrahedral sites indicates that the ferrite films grow in two stages. In the initial growth phase, a rock salt interface layer is formed. Afterwards, a structural transition occurs and the films grow in an inverse spinel structure. The thickness of the initial rock salt phase was found to increase with Ni content and to be responsible for atypical strain in the thin films. Films with Ni contents x > 1 do not show a structural transition. These films remain in a (deficient) rock salt structure consisting of a mixed Ni–Fe oxide and do not form a spinel structure at all. They show an increased number of NiO clusters as detected by X-ray photoelectron spectroscopy of the valence band, accompanied by a significant roughening of the films.

The influence of various combinations of residual stress, composition and grain interaction gradients in polycrystalline materials with cubic symmetry on energy-dispersive X-ray stress analysis is theoretically investigated. For the evaluation of the simulated sin2ψ distributions, two different strategies are compared with regard to their suitability for separating the individual gradients. It is shown that the separation of depth gradients of the strain-free lattice parameter a0(z) from residual stress gradients σ(z) is only possible if the data analysis is carried out in section planes parallel to the surface. The impact of a surface layer z* that is characterized by a direction-dependent grain interaction model in contrast to the volume of the material is quantified by comparing a ferritic and an austenitic steel, which feature different elastic anisotropy. It is shown to be of minor influence on the resulting residual stress depth profiles if the data evaluation is restricted to reflections hkl with orientation factors Γhkl close to the model-independent orientation Γ*. Finally, a method is proposed that allows the thickness of the anisotropic surface layer z* to be estimated on the basis of an optimization procedure.

Portland cements (PCs) and cement blends are multiphase materials of different fineness, and quantitatively analysing their hydration pathways is very challenging. The dissolution (hydration) of the initial crystalline and amorphous phases must be determined, as well as the formation of labile (such as ettringite), reactive (such as portlandite) and amorphous (such as calcium silicate hydrate gel) components. The microstructural changes with hydration time must also be mapped out. To address this robustly and accurately, an innovative approach is being developed based on in situ measurements of pastes without any sample conditioning. Data are sequentially acquired by Mo Kα1 laboratory X-ray powder diffraction (LXRPD) and microtomography (µCT), where the same volume is scanned with time to reduce variability. Wide capillaries (2 mm in diameter) are key to avoid artefacts, e.g. self-desiccation, and to have excellent particle averaging. This methodology is tested in three cement paste samples: (i) a commercial PC 52.5 R, (ii) a blend of 80 wt% of this PC and 20 wt% quartz, to simulate an addition of supplementary cementitious materials, and (iii) a blend of 80 wt% PC and 20 wt% limestone, to simulate a limestone Portland cement. LXRPD data are acquired at 3 h and 1, 3, 7 and 28 days, and µCT data are collected at 12 h and 1, 3, 7 and 28 days. Later age data can also be easily acquired. In this methodology, the amounts of the crystalline phases are directly obtained from Rietveld analysis and the amorphous phase contents are obtained from mass-balance calculations. From the µCT study, and within the attained spatial resolution, three components (porosity, hydrated products and unhydrated cement particles) are determined. The analyses quantitatively demonstrate the filler effect of quartz and limestone in the hydration of alite and the calcium aluminate phases. Further hydration details are discussed.

X-ray ptychography is a lensless imaging technique that visualizes the nano­structure of a thick specimen which cannot be observed with an electron microscope. It reconstructs a complex-valued refractive index of the specimen from observed diffraction patterns. This reconstruction problem is called phase retrieval (PR). For further improvement in the imaging capability, including expansion of the depth of field, various PR algorithms have been proposed. Since a high-quality PR method is built upon a base PR algorithm such as ePIE, developing a well performing base PR algorithm is important. This paper proposes an improved iterative algorithm named CRISP. It exploits subgradient projection which allows adaptive step size and can be expected to avoid yielding a poor image. The proposed algorithm was compared with ePIE, which is a simple and fast-convergence algorithm, and its modified algorithm, rPIE. The experiments confirmed that the proposed method improved the reconstruction performance for both simulation and real data.

Moderna says recently completed studies have found its vaccine to have a neutralizing effect against all COVID-19 variants tested, including the delta variant.; Credit: Fred Tanneau/AFP via Getty Images

Studies have found that Moderna's COVID-19 vaccine is effective against several variants of concern, including the delta variant, the biotech company announced.

Moderna said Tuesday that recently completed studies have found the vaccine to have a neutralizing effect against all COVID-19 variants tested, including the beta, delta, eta and kappa variants.

While still highly effective against the delta variant, the study showed the vaccine was less effective against it and certain other variants than against the original strain of the virus.

The antibody response against the delta variant was about two times weaker than against the ancestral strain of the virus.

The news echoes other findings that the Moderna and Pfizer vaccines are highly effective against the delta variant. A study published this month in Nature found that Pfizer's vaccine was able to neutralize variants including delta, though at somewhat reduced strength.

"These new data are encouraging and reinforce our belief that the Moderna COVID-19 Vaccine should remain protective against newly detected variants," Stéphane Bancel, Moderna's chief executive officer, said in a statement. "These findings highlight the importance of continuing to vaccinate populations with an effective primary series vaccine."

The company also said it is developing a booster candidate: a 50-50 mix of its currently authorized COVID-19 vaccine and another messenger RNA vaccine it has developed.

The delta variant is spreading fast

The delta variant is the fast-moving form of the coronavirus that is now found in 96 countries, including the United States.

Last week, Dr. Anthony Fauci of the National Institutes of Health said the delta variant is "currently the greatest threat in the U.S. to our attempt to eliminate COVID-19," noting that the proportion of infections being caused by the variant is doubling every two weeks.

The delta variant is now infecting at least 1 out of every 5 people who get the virus in the United States. In some sections of the country, the variant is already far more common, particularly in parts of the Midwest and West. At its current pace, the delta variant is expected to be the dominant virus in the U.S. within weeks.

Dr. Maria Van Kerkhove, an infectious disease expert at the World Health Organization, called the delta variant "incredibly transmissible."

"These viruses are becoming more fit. The virus is evolving, and this is natural," she told NPR's Morning Edition. "It's more transmissible than the alpha variant, so we need to just do all we can to prevent as many infections as we can and do what we can do to reduce the spread."

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

Former Alaska Sen. Mike Gravel, who read the Pentagon Papers into the Congressional Record and confronted Barack Obama about nuclear weapons during a later presidential run, has died. He was 91.; Credit: Charles Dharapak/AP

SEASIDE, Calif. — Mike Gravel, a former U.S. senator from Alaska who read the Pentagon Papers into the Congressional Record and confronted Barack Obama about nuclear weapons during a later presidential run, has died. He was 91.

Gravel, who represented Alaska as a Democrat in the Senate from 1969 to 1981, died Saturday, according to his daughter, Lynne Mosier. Gravel had been living in Seaside, California, and was in failing health, said Theodore W. Johnson, a former aide.

Gravel's two terms came during tumultuous years for Alaska when construction of the trans-Alaska oil pipeline was authorized and when Congress was deciding how to settle Alaska Native land claims and whether to classify enormous amounts of federal land as parks, preserves and monuments.

He had the unenviable position of being an Alaska Democrat when some residents were burning President Jimmy Carter in effigy for his measures to place large sections of public lands in the state under protection from development.

Gravel feuded with Alaska's other senator, Republican Ted Stevens, on the land matter, preferring to fight Carter's actions and rejecting Stevens' advocacy for a compromise.

In the end, Congress passed the Alaska National Interest Lands Conservation Act of 1980, a compromise that set aside millions of acres for national parks, wildlife refuges and other protected areas. It was one of the last bills Carter signed before leaving office.

Gravel's Senate tenure also was notable for his anti-war activity. In 1971, he led a one-man filibuster to protest the Vietnam-era draft and he read into the Congressional Record 4,100 pages of the 7,000-page leaked document known as the Pentagon Papers, the Defense Department's history of the country's early involvement in Vietnam.

Gravel reentered national politics decades after his time in the Senate to twice run for president. Gravel, then 75, and his wife, Whitney, took public transportation in 2006 to announce he was running for president as a Democrat in the 2008 election ultimately won by Obama.

He launched his quest for the 2008 Democratic presidential nomination as a critic of the Iraq war.

"I believe America is doing harm every day our troops remain in Iraq — harm to ourselves and to the prospects for peace in the world," Gravel said in 2006. He hitched his campaign to an effort that would give all policy decisions to the people through a direct vote, including health care reform and declarations of war.

Gravel garnered attention for his fiery comments at Democratic forums.

In one 2007 debate, the issue of the possibility of using nuclear weapons against Iran came up, and Gravel confronted then-Sen. Obama. "Tell me, Barack, who do you want to nuke?" Gravel said. Obama replied: "I'm not planning to nuke anybody right now, Mike."

Gravel then ran as a Libertarian candidate after he was excluded from later Democratic debates.

In an email to supporters, he said the Democratic Party "no longer represents my vision for our great country." "It is a party that continues to sustain war, the military-industrial complex and imperialism — all of which I find anathema to my views," he said.

He failed to get the Libertarian nomination.

Gravel briefly ran for the Democratic nomination for president in 2020. He again criticized American wars and vowed to slash military spending. His last campaign was notable in that both his campaign manager and chief of staff were just 18 at the time of his short-lived candidacy.

"There was never any ... plan that he would do anything more than participate in the debates. He didn't plan to campaign, but he wanted to get his ideas before a larger audience," Johnson said.

Gravel failed to qualify for the debates. He endorsed Vermont Sen. Bernie Sanders in the contest eventually won by now-President Joe Biden.

Gravel was born Maurice Robert Gravel in Springfield, Massachusetts, on May 13, 1930.

In Alaska, he served as a state representative, including a stint as House speaker, in the mid-1960s.

He won his first Senate term after defeating incumbent Sen. Ernest Gruening, a former territorial governor, in the 1968 Democratic primary.

Gravel served two terms until he was defeated in the 1980 Democratic primary by Gruening's grandson, Clark Gruening, who lost the election to Republican Frank Murkowski.

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

President Barack Obama presents novelist, essayist and screenwriter Larry McMurtry with a National Humanities Medal in September 2015.; Credit: Leigh Vogel/WireImage/Getty Images

Larry McMurtry, a prolific, Pulitzer Prize-winning author and Oscar-winning screenwriter, has died at age 84. He was beloved for riveting and yet unsentimental depictions of the American West in books like Lonesome Dove, as well as for tales of family drama including Terms of Endearment.

In a statement, his representative Amanda Lundberg said McMurtry "passed away last night, on March 25 of heart failure at 84 years old surrounded by his loved ones who he lived with including long time writing partner Diana Ossana, his wife Norma Faye and their 3 dogs."

In all, McMurtry wrote more than 30 novels as well as over a dozen non-fiction works that spanned memoir, history and essays. He also wrote over 20 screenplays and television scripts.

McMurtry was also famous for his bookstore, Booked Up in Archer City, Texas. Even after selling off more than half of his holdings in 2012, he still had about 200,000 books between his private collection and the store.

When he won an Oscar in 2006 for the screenplay adaption of E. Annie Proulx' short story Brokeback Mountain, which he co-wrote with longtime writing partner Diana Ossana, he thanked booksellers.

"From the humblest paperback exchange to the masters of the great bookshops of the world," he said, "all are contributors to the survival of the culture of the book, a wonderful culture, which we mustn't lose."

Filmmakers were drawn to McMurtry's work; his books Hud, The Last Picture Show and Terms of Endearment were all made into films. Lonesome Dove, which earned him the Pulitzer in 1985, became a successful TV miniseries in 1989, starring Robert Duvall and Tommy Lee Jones.

Born in 1936 on a Texas ranch, McMurtry came to his love of the West through his family. His grandfather broke horses, and his father raised cattle.

"The West is mostly a very beautiful place," he told All Things Considered in 2014. "There are all those lovely spaces. There are all those running horses. It's a poetic imagery and it's been there for a long time."

But he wanted to scour that landscape of sentimental nostalgia for cowboys, he added. "To me it was hollow and I think it was hollow for my father, although he might not have ever brought that to his conscious mind. He totally loved cowboys and so did most of the cowboys we worked with and that got him through his life. But he knew perfectly well, so did we, that it wouldn't last another generation, it just was not going to last."

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

Rescue workers move a stretcher containing recovered remains at the site of the collapsed Champlain Towers South condo building in Surfside, Fla., on Monday. Rescuers have recovered three more bodies and officials say the demolition of the building will accelerate search efforts.; Credit: Lynne Sladky/AP

Miami-Dade County mayor Daniella Levine Cava said on Monday morning that three more victims have been recovered from the ruins of the collapsed condo tower in Surfside, Fl., bringing the total death toll so far to 27.

Cava added that the demolition of the rest of Champlain Towers South "was executed exactly as planned" the previous evening, and that it would now allow rescue teams to work on a section of the collapsed building that was previously inaccessible. She noted that 118 individuals remain unaccounted for.

"Truly, we could not continue without bringing this building down," Cava said. "The area closest to the building was not accessible, due to the enormous risk to the team of first responders, because of the instability of the building."

According to Florida Governor Ron DeSantis, the newly accessible section of rubble is also from a part of the building where many bedrooms were located, and may contain the remains of many victims. The building collapsed in the middle of the night.

Authorities had been concerned that an approaching tropical storm might topple the standing part of the building onto the section that had already collapsed. That would have been a massive setback in the search for victims and for clues to the cause of the disaster.

Tropical Storm Elsa now appears to be tracking further to the west, and is more likely to hit the west coast of Florida, rather than the site of the disaster. But officials at the National Weather Service say the storm's course still could change.

Cava acknowledged that demolishing people's homes "is a devastating decision" and said that "our teams are doing everything possible to help those who lost their home begin to rebuild."

She said that authorities are working with insurance companies and the Federal Emergency Management Agency to streamline claims and help those who've lost homes and property.

One animal rescue volunteer had gone to court to stop the demolition of the rest of the tower, asking the court to allow more time to rescue pets that might still be trapped inside. The judge denied the motion.

Cava said in her Monday briefing that Miami-Dade rescue teams had already gone through parts of the building that were still accessible, "searching in closets and under beds" to find missing pets.

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

The facility is now testing biodiesel fuel being produced by several companies in the region and from the harvest of crops growing around the landfill to test which ones grow best in the local climate while producing the best oils for biodiesel.

Evidence exists linking three cancers and two other health problems with chemicals used in herbicides in the Vietnam War, a committee of the Institute of Medicine (IOM) has concluded.

Cancer-causing chemicals that occur naturally in foods are far more numerous in the human diet than synthetic carcinogens, yet both types are consumed at levels so low that they currently appear to pose little threat to human health, a committee of the National Research Council said in a report released today.

The federal government should not increase the maximum level of copper allowed in drinking water, because higher levels could lead to liver poisoning in infants and children with certain genetic disorders.

Recent strides in biotechnology offer the promise of new and innovative applications -- from edible vaccines to protein-based electronics components.

One out of every four dogs and cats in the western world is now obese. Like humans, dogs and cats that are obese run a higher risk of developing diabetes, heart disease, or other health problems.

The vast majority of healthy people adequately meet their daily hydration needs by letting thirst be their guide, says the newest report on nutrient recommendations from the Institute of Medicine of the National Academies.

A limited body of evidence suggests an association between military service and later development of amyotrophic lateral sclerosis (ALS), a rare but fatal neurodegenerative disorder, says a new report from the Institute of Medicine.

Most Americans and Canadians up to age 70 need no more than 600 international units (IUs) of vitamin D per day to maintain health, and those 71 and older may need as much as 800 IUs, says a new report from the Institute of Medicine.

The U.S. Environmental Protection Agency (EPA) carries out experiments in which volunteer participants agree to be intentionally exposed by inhalation to specific pollutants at restricted concentrations over short periods to obtain important information about the effects of outdoor air pollution on human health.

A new report from the National Academies of Sciences, Engineering, and Medicine outlines how to examine whether specific levels of nutrients or other food substances (NOFSs) can ameliorate the risk of chronic disease and recommends ways to develop dietary reference intakes (DRI) based on chronic disease outcomes.

Although the process used to develop the Dietary Guidelines for Americans (DGA) has become more evidence-based since its inception more than 30 years ago, it is not currently positioned to effectively adapt to changes such as food diversity and chronic disease prevalence, while also ensuring the integrity of the process, says a new congressionally mandated report from the National Academies of Sciences, Engineering, and Medicine.

A new congressionally mandated report from the National Academies of Sciences, Engineering, and Medicine takes a comprehensive look at evidence on the human health effects of e-cigarettes.